# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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#######################################################################

data_ic80-mcn
_database_code_depnum_ccdc_archive 'CCDC 2078647'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2021-04-19 deposited with the CCDC.	2021-06-10 downloaded from the CCDC.
;
_audit_creation_date             2020-07-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis-[N-(2,6-di{pyrazol-1-yl}pyrid-4-yl)acetamide]iron(II)ditetrafluoroborate di-acetonitrile solvate'
_chemical_formula_moiety         'C26 H24 Fe N12 O2, 2(B F4), 2(C2 H3 N)'
_chemical_formula_sum            'C30 H30 B2 F8 Fe N14 O2'
_chemical_formula_weight         848.15
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.05780(18)
_cell_length_b                   12.7729(4)
_cell_length_c                   18.7921(6)
_cell_angle_alpha                96.071(3)
_cell_angle_beta                 102.311(2)
_cell_angle_gamma                101.565(2)
_cell_volume                     1828.85(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8276
_cell_measurement_temperature    120(2)
_cell_measurement_theta_min      4.61
_cell_measurement_theta_max      73.67
_exptl_absorpt_coefficient_mu    4.135
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       lath
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.951
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13810
_diffrn_reflns_point_group_measured_fraction_full 0.951
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.854
_diffrn_reflns_theta_min         3.575
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6579
_reflns_number_total             6908
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2015)'
_refine_diff_density_max         0.813
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         6908
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0422
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0595P)²+1.3319P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1107
_refine_special_details          
;
 One BF₄⁻ ion is disordered over two sites, with refined occupancies of
 0.77:0.23. The bond distance restraints that were applied to the 
 disordered anion are listed below. All non-H atoms except the disordered 
 anion were refined anisotropically, and H atoms were placed in calculated 
 positions and refined using a riding model.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N18-H18 = N38-H38
 0.95 with sigma of 0.02
 B42A-F43A = B42A-F44A = B42A-F45A = B42A-F46A
 1.38081 with sigma of 0.02
 B42B-F43B = B42B-F44B = B42B-F45B = B42B-F46B
 1.38081 with sigma of 0.02
 F43A-F44A = F43A-F45A = F43A-F46A = F44A-F45A = F44A-F46A = F45A-F46A
 2.254863 with sigma of 0.02
 F43B-F44B = F43B-F45B = F43B-F46B = F44B-F45B = F44B-F46B = F45B-F46B
 2.254863 with sigma of 0.02
3. Others
 1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: B42A(0.77) F43A(0.77) F44A(0.77) F45A(0.77) F46A(0.77) B42B(0.23)
 F43B(0.23) F44B(0.23) F45B(0.23) F46B(0.23)
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17),
 N18(H18), C24(H24), C26(H26), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36),
  C37(H37), N38(H38)
4.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C41(H41A,H41B,H41C), C52(H52A,H52B,H52C), C55(H55A,H55B,
 H55C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.74151(4) 0.67581(2) 0.27196(2) 0.01630(10) Uani 1 1 d . . . . .
N2 N 0.7756(2) 0.83554(13) 0.32612(9) 0.0154(3) Uani 1 1 d . . . . .
C3 C 0.7601(3) 0.85514(16) 0.39524(11) 0.0160(4) Uani 1 1 d . . . . .
C4 C 0.7828(3) 0.95652(17) 0.43365(11) 0.0187(4) Uani 1 1 d . . . . .
H4 H 0.772151 0.966677 0.483147 0.022 Uiso 1 1 calc R U . . .
C5 C 0.8227(3) 1.04469(17) 0.39651(11) 0.0191(4) Uani 1 1 d . . . . .
C6 C 0.8402(3) 1.02699(17) 0.32420(11) 0.0192(4) Uani 1 1 d . . . . .
H6 H 0.867684 1.085241 0.298019 0.023 Uiso 1 1 calc R U . . .
C7 C 0.8157(3) 0.92086(17) 0.29255(11) 0.0161(4) Uani 1 1 d . . . . .
N8 N 0.7154(2) 0.76013(14) 0.42552(9) 0.0167(3) Uani 1 1 d . . . . .
N9 N 0.6994(2) 0.66271(14) 0.38368(9) 0.0179(3) Uani 1 1 d . . . . .
C10 C 0.6578(3) 0.58916(17) 0.42557(12) 0.0210(4) Uani 1 1 d . . . . .
H10 H 0.638931 0.513337 0.411116 0.025 Uiso 1 1 calc R U . . .
C11 C 0.6455(3) 0.63832(18) 0.49433(12) 0.0247(5) Uani 1 1 d . . . . .
H11 H 0.617556 0.603364 0.533845 0.030 Uiso 1 1 calc R U . . .
C12 C 0.6821(3) 0.74684(18) 0.49219(12) 0.0225(4) Uani 1 1 d . . . . .
H12 H 0.683995 0.802602 0.530250 0.027 Uiso 1 1 calc R U . . .
N13 N 0.8304(2) 0.89179(14) 0.22017(9) 0.0169(3) Uani 1 1 d . . . . .
N14 N 0.8082(2) 0.78446(14) 0.19380(9) 0.0175(3) Uani 1 1 d . . . . .
C15 C 0.8319(3) 0.78296(18) 0.12572(11) 0.0196(4) Uani 1 1 d . . . . .
H15 H 0.823825 0.718937 0.093181 0.024 Uiso 1 1 calc R U . . .
C16 C 0.8704(3) 0.88776(18) 0.10804(12) 0.0217(4) Uani 1 1 d . . . . .
H16 H 0.893349 0.907658 0.063171 0.026 Uiso 1 1 calc R U . . .
C17 C 0.8679(3) 0.95530(17) 0.16937(11) 0.0204(4) Uani 1 1 d . . . . .
H17 H 0.888334 1.031947 0.175261 0.025 Uiso 1 1 calc R U . . .
N18 N 0.8392(3) 1.14686(15) 0.43486(10) 0.0245(4) Uani 1 1 d D . . . .
H18 H 0.816316 1.148879 0.478672 0.029 Uiso 1 1 calc DR U . . .
C19 C 0.8871(3) 1.24530(18) 0.41238(13) 0.0266(5) Uani 1 1 d . . . . .
O20 O 0.9303(3) 1.25482(14) 0.35521(10) 0.0425(5) Uani 1 1 d . . . . .
C21 C 0.8800(4) 1.34004(18) 0.46586(14) 0.0322(5) Uani 1 1 d . . . . .
H21A H 0.758422 1.337896 0.467050 0.048 Uiso 1 1 calc R U . . .
H21B H 0.930068 1.407615 0.450113 0.048 Uiso 1 1 calc R U . . .
H21C H 0.947096 1.336218 0.515201 0.048 Uiso 1 1 calc R U . . .
N22 N 0.6427(2) 0.51123(14) 0.21905(9) 0.0155(3) Uani 1 1 d . . . . .
C23 C 0.7428(3) 0.43971(17) 0.22486(10) 0.0161(4) Uani 1 1 d . . . . .
C24 C 0.6865(3) 0.33110(16) 0.19656(11) 0.0172(4) Uani 1 1 d . . . . .
H24 H 0.762556 0.282992 0.202814 0.021 Uiso 1 1 calc R U . . .
C25 C 0.5109(3) 0.29545(16) 0.15805(11) 0.0181(4) Uani 1 1 d . . . . .
C26 C 0.4040(3) 0.36958(17) 0.14904(11) 0.0186(4) Uani 1 1 d . . . . .
H26 H 0.285964 0.347708 0.121585 0.022 Uiso 1 1 calc R U . . .
C27 C 0.4764(3) 0.47487(17) 0.18139(11) 0.0164(4) Uani 1 1 d . . . . .
N28 N 0.9157(2) 0.48691(14) 0.26428(9) 0.0161(3) Uani 1 1 d . . . . .
N29 N 0.9570(2) 0.59436(14) 0.29355(9) 0.0186(4) Uani 1 1 d . . . . .
C30 C 1.1242(3) 0.61504(18) 0.32896(12) 0.0230(4) Uani 1 1 d . . . . .
H30 H 1.189873 0.683734 0.355076 0.028 Uiso 1 1 calc R U . . .
C31 C 1.1910(3) 0.52228(18) 0.32270(12) 0.0234(4) Uani 1 1 d . . . . .
H31 H 1.306496 0.516317 0.343213 0.028 Uiso 1 1 calc R U . . .
C32 C 1.0559(3) 0.44207(18) 0.28103(11) 0.0201(4) Uani 1 1 d . . . . .
H32 H 1.059309 0.369133 0.266551 0.024 Uiso 1 1 calc R U . . .
N33 N 0.3810(2) 0.55592(14) 0.17912(9) 0.0177(3) Uani 1 1 d . . . . .
N34 N 0.4606(2) 0.65589(14) 0.21932(10) 0.0195(4) Uani 1 1 d . . . . .
C35 C 0.3400(3) 0.71351(19) 0.20851(13) 0.0252(5) Uani 1 1 d . . . . .
H35 H 0.357262 0.786920 0.229729 0.030 Uiso 1 1 calc R U . . .
C36 C 0.1838(3) 0.6516(2) 0.16160(13) 0.0286(5) Uani 1 1 d . . . . .
H36 H 0.078977 0.674756 0.145450 0.034 Uiso 1 1 calc R U . . .
C37 C 0.2125(3) 0.55169(19) 0.14385(12) 0.0231(4) Uani 1 1 d . . . . .
H37 H 0.131440 0.491081 0.113047 0.028 Uiso 1 1 calc R U . . .
N38 N 0.4353(2) 0.18838(15) 0.12658(10) 0.0220(4) Uani 1 1 d D . . . .
H38 H 0.339837 0.176764 0.090992 0.026 Uiso 1 1 calc DR U . . .
C39 C 0.4946(3) 0.09794(18) 0.14544(12) 0.0236(5) Uani 1 1 d . . . . .
O40 O 0.6232(2) 0.10375(13) 0.19420(9) 0.0266(3) Uani 1 1 d . . . . .
C41 C 0.3834(4) -0.0071(2) 0.10132(17) 0.0407(7) Uani 1 1 d . . . . .
H41A H 0.271043 -0.022329 0.114889 0.061 Uiso 1 1 calc R U . . .
H41B H 0.442848 -0.065581 0.111630 0.061 Uiso 1 1 calc R U . . .
H41C H 0.363647 -0.001821 0.048659 0.061 Uiso 1 1 calc R U . . .
B42A B 0.7253(6) 1.0937(3) 0.6221(2) 0.0233(8) Uiso 0.77 1 d D . P A 1
F43A F 0.6586(3) 0.98660(18) 0.58797(12) 0.0384(5) Uiso 0.77 1 d D . P A 1
F44A F 0.8050(3) 1.09975(16) 0.69515(11) 0.0370(4) Uiso 0.77 1 d D . P A 1
F45A F 0.5974(3) 1.15207(18) 0.61506(12) 0.0424(5) Uiso 0.77 1 d D . P A 1
F46A F 0.8521(3) 1.14130(16) 0.58579(11) 0.0352(4) Uiso 0.77 1 d D . P A 1
B42B B 0.6721(14) 1.0764(8) 0.6054(5) 0.014(2) Uiso 0.23 1 d D . P B 2
F43B F 0.5833(8) 0.9727(4) 0.5752(3) 0.0178(11) Uiso 0.23 1 d D . P B 2
F44B F 0.8488(10) 1.0790(7) 0.6192(5) 0.056(2) Uiso 0.23 1 d D . P B 2
F45B F 0.6153(8) 1.0984(5) 0.6676(3) 0.0311(13) Uiso 0.23 1 d D . P B 2
F46B F 0.6369(7) 1.1462(4) 0.5573(3) 0.0260(12) Uiso 0.23 1 d D . P B 2
B47 B -0.0399(3) 0.2028(2) 0.08400(14) 0.0231(5) Uani 1 1 d . . . . .
F48 F 0.00952(19) 0.22100(13) 0.16062(8) 0.0350(3) Uani 1 1 d . . . . .
F49 F -0.0131(2) 0.30055(15) 0.05836(12) 0.0618(6) Uani 1 1 d . . . . .
F50 F -0.21203(17) 0.14799(11) 0.05966(8) 0.0283(3) Uani 1 1 d . . . . .
F51 F 0.06712(19) 0.13996(15) 0.05956(8) 0.0414(4) Uani 1 1 d . . . . .
C52 C 0.7130(4) 0.8561(2) 0.71489(15) 0.0404(6) Uani 1 1 d . . . . .
H52A H 0.636458 0.905932 0.719068 0.061 Uiso 1 1 calc R U . . .
H52B H 0.790580 0.881034 0.683396 0.061 Uiso 1 1 calc R U . . .
H52C H 0.783013 0.853734 0.763980 0.061 Uiso 1 1 calc R U . . .
C53 C 0.6080(3) 0.7487(2) 0.68268(13) 0.0297(5) Uani 1 1 d . . . . .
N54 N 0.5263(4) 0.6649(2) 0.65746(13) 0.0440(6) Uani 1 1 d . . . . .
C55 C 0.5923(4) 0.3277(2) -0.01396(13) 0.0318(5) Uani 1 1 d . . . . .
H55A H 0.485567 0.303691 0.002670 0.048 Uiso 1 1 calc R U . . .
H55B H 0.669274 0.278132 -0.002880 0.048 Uiso 1 1 calc R U . . .
H55C H 0.562102 0.328349 -0.067248 0.048 Uiso 1 1 calc R U . . .
C56 C 0.6812(3) 0.4362(2) 0.02399(13) 0.0290(5) Uani 1 1 d . . . . .
N57 N 0.7486(4) 0.52116(19) 0.05395(14) 0.0429(6) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.1191(17) . ?
Fe1 N9 2.2151(17) . ?
Fe1 N14 2.2003(18) . ?
Fe1 N22 2.1427(17) . ?
Fe1 N29 2.1850(18) . ?
Fe1 N34 2.2200(19) . ?
N2 C3 1.334(3) . ?
N2 C7 1.335(3) . ?
C3 C4 1.372(3) . ?
C3 N8 1.409(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.405(3) . ?
C5 C6 1.395(3) . ?
C5 N18 1.390(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.379(3) . ?
C7 N13 1.408(3) . ?
N8 N9 1.367(2) . ?
N8 C12 1.357(3) . ?
N9 C10 1.326(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.408(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.365(3) . ?
C12 H12 0.9500 . ?
N13 N14 1.370(2) . ?
N13 C17 1.360(3) . ?
N14 C15 1.332(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.404(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.371(3) . ?
C17 H17 0.9500 . ?
N18 H18 0.8800 . ?
N18 C19 1.377(3) . ?
C19 O20 1.208(3) . ?
C19 C21 1.507(3) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
N22 C23 1.333(3) . ?
N22 C27 1.337(3) . ?
C23 C24 1.379(3) . ?
C23 N28 1.408(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.403(3) . ?
C25 C26 1.402(3) . ?
C25 N38 1.390(3) . ?
C26 H26 0.9500 . ?
C26 C27 1.371(3) . ?
C27 N33 1.407(3) . ?
N28 N29 1.370(2) . ?
N28 C32 1.360(3) . ?
N29 C30 1.329(3) . ?
C30 H30 0.9500 . ?
C30 C31 1.400(3) . ?
C31 H31 0.9500 . ?
C31 C32 1.366(3) . ?
C32 H32 0.9500 . ?
N33 N34 1.369(2) . ?
N33 C37 1.365(3) . ?
N34 C35 1.327(3) . ?
C35 H35 0.9500 . ?
C35 C36 1.403(4) . ?
C36 H36 0.9500 . ?
C36 C37 1.362(3) . ?
C37 H37 0.9500 . ?
N38 H38 0.8800 . ?
N38 C39 1.387(3) . ?
C39 O40 1.212(3) . ?
C39 C41 1.502(3) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
B42A F43A 1.394(5) . ?
B42A F44A 1.372(5) . ?
B42A F45A 1.381(4) . ?
B42A F46A 1.420(4) . ?
B42B F43B 1.369(11) . ?
B42B F44B 1.385(12) . ?
B42B F45B 1.367(10) . ?
B42B F46B 1.361(10) . ?
B47 F48 1.390(3) . ?
B47 F49 1.379(3) . ?
B47 F50 1.377(3) . ?
B47 F51 1.402(3) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C52 C53 1.451(4) . ?
C53 N54 1.131(4) . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C55 C56 1.455(3) . ?
C56 N57 1.137(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N9 73.08(6) . . ?
N2 Fe1 N14 73.50(6) . . ?
N2 Fe1 N22 166.04(7) . . ?
N2 Fe1 N29 119.23(7) . . ?
N2 Fe1 N34 95.10(6) . . ?
N9 Fe1 N34 94.41(7) . . ?
N14 Fe1 N9 146.57(6) . . ?
N14 Fe1 N34 89.41(7) . . ?
N22 Fe1 N9 100.95(6) . . ?
N22 Fe1 N14 111.83(6) . . ?
N22 Fe1 N29 72.80(6) . . ?
N22 Fe1 N34 72.48(6) . . ?
N29 Fe1 N9 91.01(6) . . ?
N29 Fe1 N14 104.47(7) . . ?
N29 Fe1 N34 145.26(7) . . ?
C3 N2 Fe1 121.57(14) . . ?
C3 N2 C7 117.25(17) . . ?
C7 N2 Fe1 121.17(13) . . ?
N2 C3 C4 124.4(2) . . ?
N2 C3 N8 113.02(17) . . ?
C4 C3 N8 122.59(18) . . ?
C3 C4 H4 121.5 . . ?
C3 C4 C5 117.02(19) . . ?
C5 C4 H4 121.5 . . ?
C6 C5 C4 120.02(19) . . ?
N18 C5 C4 116.65(19) . . ?
N18 C5 C6 123.3(2) . . ?
C5 C6 H6 121.6 . . ?
C7 C6 C5 116.80(19) . . ?
C7 C6 H6 121.6 . . ?
N2 C7 C6 124.50(18) . . ?
N2 C7 N13 112.91(17) . . ?
C6 C7 N13 122.59(19) . . ?
N9 N8 C3 118.44(16) . . ?
C12 N8 C3 130.37(18) . . ?
C12 N8 N9 111.19(17) . . ?
N8 N9 Fe1 113.85(12) . . ?
C10 N9 Fe1 140.88(14) . . ?
C10 N9 N8 105.24(16) . . ?
N9 C10 H10 124.5 . . ?
N9 C10 C11 111.01(19) . . ?
C11 C10 H10 124.5 . . ?
C10 C11 H11 127.3 . . ?
C12 C11 C10 105.41(19) . . ?
C12 C11 H11 127.3 . . ?
N8 C12 C11 107.15(19) . . ?
N8 C12 H12 126.4 . . ?
C11 C12 H12 126.4 . . ?
N14 N13 C7 118.66(17) . . ?
C17 N13 C7 129.86(18) . . ?
C17 N13 N14 111.46(16) . . ?
N13 N14 Fe1 113.72(12) . . ?
C15 N14 Fe1 141.56(15) . . ?
C15 N14 N13 104.69(17) . . ?
N14 C15 H15 124.2 . . ?
N14 C15 C16 111.56(18) . . ?
C16 C15 H15 124.2 . . ?
C15 C16 H16 127.4 . . ?
C17 C16 C15 105.27(18) . . ?
C17 C16 H16 127.4 . . ?
N13 C17 C16 107.02(19) . . ?
N13 C17 H17 126.5 . . ?
C16 C17 H17 126.5 . . ?
C5 N18 H18 116.2 . . ?
C19 N18 C5 127.63(19) . . ?
C19 N18 H18 116.2 . . ?
N18 C19 C21 113.5(2) . . ?
O20 C19 N18 123.2(2) . . ?
O20 C19 C21 123.2(2) . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 N22 Fe1 121.25(14) . . ?
C23 N22 C27 117.18(17) . . ?
C27 N22 Fe1 121.51(13) . . ?
N22 C23 C24 124.90(19) . . ?
N22 C23 N28 112.44(17) . . ?
C24 C23 N28 122.66(18) . . ?
C23 C24 H24 121.8 . . ?
C23 C24 C25 116.42(18) . . ?
C25 C24 H24 121.8 . . ?
C26 C25 C24 119.89(19) . . ?
N38 C25 C24 123.05(19) . . ?
N38 C25 C26 117.06(19) . . ?
C25 C26 H26 121.3 . . ?
C27 C26 C25 117.42(19) . . ?
C27 C26 H26 121.3 . . ?
N22 C27 C26 124.13(18) . . ?
N22 C27 N33 112.94(18) . . ?
C26 C27 N33 122.92(19) . . ?
N29 N28 C23 118.39(16) . . ?
C32 N28 C23 130.30(18) . . ?
C32 N28 N29 111.29(17) . . ?
N28 N29 Fe1 115.02(13) . . ?
C30 N29 Fe1 139.95(15) . . ?
C30 N29 N28 105.01(17) . . ?
N29 C30 H30 124.5 . . ?
N29 C30 C31 111.08(19) . . ?
C31 C30 H30 124.5 . . ?
C30 C31 H31 127.0 . . ?
C32 C31 C30 105.91(19) . . ?
C32 C31 H31 127.0 . . ?
N28 C32 C31 106.70(19) . . ?
N28 C32 H32 126.6 . . ?
C31 C32 H32 126.6 . . ?
N34 N33 C27 118.31(17) . . ?
C37 N33 C27 130.24(19) . . ?
C37 N33 N34 111.42(17) . . ?
N33 N34 Fe1 114.45(12) . . ?
C35 N34 Fe1 140.28(16) . . ?
C35 N34 N33 105.01(18) . . ?
N34 C35 H35 124.5 . . ?
N34 C35 C36 111.0(2) . . ?
C36 C35 H35 124.5 . . ?
C35 C36 H36 126.9 . . ?
C37 C36 C35 106.2(2) . . ?
C37 C36 H36 126.9 . . ?
N33 C37 H37 126.8 . . ?
C36 C37 N33 106.4(2) . . ?
C36 C37 H37 126.8 . . ?
C25 N38 H38 116.6 . . ?
C39 N38 C25 126.77(19) . . ?
C39 N38 H38 116.6 . . ?
N38 C39 C41 114.1(2) . . ?
O40 C39 N38 122.6(2) . . ?
O40 C39 C41 123.4(2) . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
F43A B42A F46A 107.4(3) . . ?
F44A B42A F43A 111.4(3) . . ?
F44A B42A F45A 110.2(3) . . ?
F44A B42A F46A 108.4(3) . . ?
F45A B42A F43A 111.6(3) . . ?
F45A B42A F46A 107.6(3) . . ?
F43B B42B F44B 107.7(7) . . ?
F45B B42B F43B 105.1(7) . . ?
F45B B42B F44B 113.6(9) . . ?
F46B B42B F43B 110.7(8) . . ?
F46B B42B F44B 108.4(8) . . ?
F46B B42B F45B 111.4(7) . . ?
F48 B47 F51 107.10(19) . . ?
F49 B47 F48 109.2(2) . . ?
F49 B47 F51 109.5(2) . . ?
F50 B47 F48 110.5(2) . . ?
F50 B47 F49 110.72(19) . . ?
F50 B47 F51 109.7(2) . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C53 C52 H52A 109.5 . . ?
C53 C52 H52B 109.5 . . ?
C53 C52 H52C 109.5 . . ?
N54 C53 C52 179.9(3) . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C56 C55 H55A 109.5 . . ?
C56 C55 H55B 109.5 . . ?
C56 C55 H55C 109.5 . . ?
N57 C56 C55 179.1(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N18 H18 F46A 0.88 1.99 2.825(3) 158.6 . yes
N18 H18 F46B 0.88 2.28 3.091(6) 154.0 . yes
N38 H38 F51 0.88 2.09 2.877(2) 148.2 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N2 C3 C4 179.08(16) . . . . ?
Fe1 N2 C3 N8 -1.6(2) . . . . ?
Fe1 N2 C7 C6 -179.87(16) . . . . ?
Fe1 N2 C7 N13 0.3(2) . . . . ?
Fe1 N9 C10 C11 -177.40(17) . . . . ?
Fe1 N14 C15 C16 178.23(16) . . . . ?
Fe1 N22 C23 C24 175.69(15) . . . . ?
Fe1 N22 C23 N28 -3.8(2) . . . . ?
Fe1 N22 C27 C26 -177.17(15) . . . . ?
Fe1 N22 C27 N33 1.9(2) . . . . ?
Fe1 N29 C30 C31 178.41(17) . . . . ?
Fe1 N34 C35 C36 173.19(17) . . . . ?
N2 C3 C4 C5 1.0(3) . . . . ?
N2 C3 N8 N9 2.1(3) . . . . ?
N2 C3 N8 C12 -177.3(2) . . . . ?
N2 C7 N13 N14 -1.8(3) . . . . ?
N2 C7 N13 C17 179.5(2) . . . . ?
C3 N2 C7 C6 -0.6(3) . . . . ?
C3 N2 C7 N13 179.52(17) . . . . ?
C3 C4 C5 C6 -1.0(3) . . . . ?
C3 C4 C5 N18 177.69(19) . . . . ?
C3 N8 N9 Fe1 -1.7(2) . . . . ?
C3 N8 N9 C10 179.78(17) . . . . ?
C3 N8 C12 C11 -179.9(2) . . . . ?
C4 C3 N8 N9 -178.51(19) . . . . ?
C4 C3 N8 C12 2.1(3) . . . . ?
C4 C5 C6 C7 0.3(3) . . . . ?
C4 C5 N18 C19 175.9(2) . . . . ?
C5 C6 C7 N2 0.5(3) . . . . ?
C5 C6 C7 N13 -179.64(19) . . . . ?
C5 N18 C19 O20 -3.7(4) . . . . ?
C5 N18 C19 C21 176.2(2) . . . . ?
C6 C5 N18 C19 -5.4(4) . . . . ?
C6 C7 N13 N14 178.37(19) . . . . ?
C6 C7 N13 C17 -0.3(3) . . . . ?
C7 N2 C3 C4 -0.2(3) . . . . ?
C7 N2 C3 N8 179.19(17) . . . . ?
C7 N13 N14 Fe1 2.3(2) . . . . ?
C7 N13 N14 C15 -179.18(17) . . . . ?
C7 N13 C17 C16 178.7(2) . . . . ?
N8 C3 C4 C5 -178.33(18) . . . . ?
N8 N9 C10 C11 0.4(2) . . . . ?
N9 N8 C12 C11 0.7(3) . . . . ?
N9 C10 C11 C12 0.0(3) . . . . ?
C10 C11 C12 N8 -0.4(3) . . . . ?
C12 N8 N9 Fe1 177.81(14) . . . . ?
C12 N8 N9 C10 -0.7(2) . . . . ?
N13 N14 C15 C16 0.5(2) . . . . ?
N14 N13 C17 C16 -0.1(2) . . . . ?
N14 C15 C16 C17 -0.5(2) . . . . ?
C15 C16 C17 N13 0.3(2) . . . . ?
C17 N13 N14 Fe1 -178.73(13) . . . . ?
C17 N13 N14 C15 -0.3(2) . . . . ?
N18 C5 C6 C7 -178.3(2) . . . . ?
N22 C23 C24 C25 1.0(3) . . . . ?
N22 C23 N28 N29 2.8(2) . . . . ?
N22 C23 N28 C32 -179.07(19) . . . . ?
N22 C27 N33 N34 -5.5(3) . . . . ?
N22 C27 N33 C37 176.8(2) . . . . ?
C23 N22 C27 C26 0.2(3) . . . . ?
C23 N22 C27 N33 179.25(17) . . . . ?
C23 C24 C25 C26 1.1(3) . . . . ?
C23 C24 C25 N38 -179.85(19) . . . . ?
C23 N28 N29 Fe1 -0.7(2) . . . . ?
C23 N28 N29 C30 178.07(17) . . . . ?
C23 N28 C32 C31 -177.7(2) . . . . ?
C24 C23 N28 N29 -176.65(18) . . . . ?
C24 C23 N28 C32 1.5(3) . . . . ?
C24 C25 C26 C27 -2.4(3) . . . . ?
C24 C25 N38 C39 21.4(3) . . . . ?
C25 C26 C27 N22 1.8(3) . . . . ?
C25 C26 C27 N33 -177.18(18) . . . . ?
C25 N38 C39 O40 1.0(4) . . . . ?
C25 N38 C39 C41 179.7(2) . . . . ?
C26 C25 N38 C39 -159.6(2) . . . . ?
C26 C27 N33 N34 173.54(18) . . . . ?
C26 C27 N33 C37 -4.2(3) . . . . ?
C27 N22 C23 C24 -1.7(3) . . . . ?
C27 N22 C23 N28 178.88(16) . . . . ?
C27 N33 N34 Fe1 6.5(2) . . . . ?
C27 N33 N34 C35 -178.22(18) . . . . ?
C27 N33 C37 C36 178.1(2) . . . . ?
N28 C23 C24 C25 -179.59(18) . . . . ?
N28 N29 C30 C31 0.1(2) . . . . ?
N29 N28 C32 C31 0.5(2) . . . . ?
N29 C30 C31 C32 0.2(3) . . . . ?
C30 C31 C32 N28 -0.4(2) . . . . ?
C32 N28 N29 Fe1 -179.18(13) . . . . ?
C32 N28 N29 C30 -0.4(2) . . . . ?
N33 N34 C35 C36 -0.1(2) . . . . ?
N34 N33 C37 C36 0.3(2) . . . . ?
N34 C35 C36 C37 0.3(3) . . . . ?
C35 C36 C37 N33 -0.4(3) . . . . ?
C37 N33 N34 Fe1 -175.44(13) . . . . ?
C37 N33 N34 C35 -0.1(2) . . . . ?
N38 C25 C26 C27 178.50(18) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile/diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_80-acnhs
_database_code_depnum_ccdc_archive 'CCDC 2078648'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2021-04-19 deposited with the CCDC.	2021-06-10 downloaded from the CCDC.
;
_audit_creation_date             2020-07-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis-[N-(2,6-di{pyrazol-1-yl}pyrid-4-yl)acetamide]iron(II)ditetrafluoroborate acetonitrile solvate'
_chemical_formula_moiety         'C26 H24 Fe N12 O2, 2(B F4), C2 H3 N'
_chemical_formula_sum            'C28 H27 B2 F8 Fe N13 O2'
_chemical_formula_weight         807.09
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2279(3)
_cell_length_b                   12.5396(6)
_cell_length_c                   17.5742(11)
_cell_angle_alpha                83.354(5)
_cell_angle_beta                 79.986(4)
_cell_angle_gamma                80.831(4)
_cell_volume                     1755.54(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6502
_cell_measurement_temperature    200(2)
_cell_measurement_theta_min      4.19
_cell_measurement_theta_max      73.47
_exptl_absorpt_coefficient_mu    4.268
_exptl_absorpt_correction_T_min  0.837
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.948
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6607
_diffrn_reflns_point_group_measured_fraction_full 0.948
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.574
_diffrn_reflns_theta_min         3.585
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5861
_reflns_number_total             6607
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2015)'
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         6607
_refine_ls_number_restraints     64
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0702
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0916P)²+2.4776P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2060
_refine_ls_wR_factor_ref         0.2112
_refine_special_details          
;The data were resolved into two non-superimposable twin domains, in a 
 ratio of 0.60:0.40.

 The C atoms of one pyrazole ring in the complex cation were modelled as 
 disordered over two half-occupied sites, to resolve an intermolecular
 steric clash. Both BF₄⁻ ions are also disordered over two sites 
 sharing a common wholly occupied B atom; and, over three orientations, 
 two of which also share a common B atom. The acetonitrile molecule is
 also disordered over two sites. The bond distance restraints that were 
 applied to the disordered residues are listed below.

 All crystallographically ordered non-H atoms were refined anisotropically,
 and H atoms were placed in calculated positions and refined using a 
 riding model.,Twin
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.603(4)
 0.397(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N14-C15A = N14-C15B
 1.32 with sigma of 0.01
 C15A-C16A = C15B-C16B
 1.39 with sigma of 0.01
 C16A-C17A = C16B-C17B
 1.37 with sigma of 0.01
 N13-C17A = N13-C17B
 1.36 with sigma of 0.01
 B42-F43A = B42-F44A = B42-F45A = B42-F46A
 1.39265 with sigma of 0.02
 B42-F43B = B42-F44B = B42-F45B = B42-F46B
 1.39265 with sigma of 0.02
 F43A-F44A = F43A-F45A = F43A-F46A = F44A-F45A = F44A-F46A = F45A-F46A
 2.274197 with sigma of 0.02
 F43B-F44B = F43B-F45B = F43B-F46B = F44B-F45B = F44B-F46B = F45B-F46B
 2.274197 with sigma of 0.02
 B47A-F48A = B47A-F49A = B47A-F50A = B47A-F51A
 1.39265 with sigma of 0.02
 B47B-F48B = B47B-F49B = B47B-F50B = B47B-F51B
 1.39265 with sigma of 0.02
 B47B-F48C = B47B-F49C = B47B-F50C = B47B-F51C
 1.39265 with sigma of 0.02
 F48A-F49A = F48A-F50A = F48A-F51A = F49A-F50A = F49A-F51A = F50A-F51A
 2.274197 with sigma of 0.02
 F48B-F49B = F48B-F50B = F48B-F51B = F49B-F50B = F49B-F51B = F50B-F51B
 2.274197 with sigma of 0.02
 F48C-F49C = F48C-F50C = F48C-F51C = F49C-F50C = F49C-F51C = F50C-F51C
 2.274197 with sigma of 0.02
 C52A-C53A = C52B-C53B
 1.48 with sigma of 0.02
 C53A-N54A = C53B-N54B
 1.15 with sigma of 0.02
 C52A-N54A = C52B-N54B
 2.63 with sigma of 0.02
4. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: C15A(0.5) H15A(0.5) C16A(0.5) H16A(0.5) C17A(0.5) H17A(0.5)
 C15B(0.5) H15B(0.5) C16B(0.5) H16B(0.5) C17B(0.5) H17B(0.5) F43A(0.67)
 F44A(0.67) F45A(0.67) F46A(0.67) F43B(0.33) F44B(0.33) F45B(0.33) F46B(0.33)
 B47A(0.5) F48A(0.5) F49A(0.5) F50A(0.5) F51A(0.5) B47B(0.5) F48B(0.2)
 F49B(0.2) F50B(0.2) F51B(0.2) F48C(0.3) F49C(0.3) F50C(0.3) F51C(0.3)
 C52A(0.5) H52A(0.5) H52B(0.5) H52C(0.5) C53A(0.5) N54A(0.5) C52B(0.5)
 H52D(0.5) H52E(0.5) H52F(0.5) C53B(0.5) N54B(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C15A(H15A), C16A(H16A),
 C17A(H17A), C15B(H15B), C16B(H16B), C17B(H17B), N18(H18), C24(H24), C26(H26),
 C30(H30), C31(H31), C32(H32), C35(H35), C36(H36), C37(H37), N38(H38)
5.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C41(H41A,H41B,H41C), C52A(H52A,H52B,H52C), C52B(H52D,
 H52E,H52F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.78354(9) 0.26215(6) 0.73252(4) 0.0356(2) Uani 1 1 d . . . . .
N2 N 0.8170(4) 0.1156(3) 0.67983(19) 0.0301(7) Uani 1 1 d . . . . .
C3 C 0.7890(5) 0.1133(3) 0.6075(2) 0.0296(8) Uani 1 1 d . . . . .
C4 C 0.8076(6) 0.0208(3) 0.5709(2) 0.0345(9) Uani 1 1 d . . . . .
H4 H 0.789283 0.023373 0.518802 0.041 Uiso 1 1 calc R U . . .
C5 C 0.8543(6) -0.0776(3) 0.6126(3) 0.0363(9) Uani 1 1 d . . . . .
C6 C 0.8845(6) -0.0780(4) 0.6890(3) 0.0390(10) Uani 1 1 d . . . . .
H6 H 0.917709 -0.143467 0.718817 0.047 Uiso 1 1 calc R U . . .
C7 C 0.8635(5) 0.0207(4) 0.7181(2) 0.0345(9) Uani 1 1 d . . . . .
N8 N 0.7363(5) 0.2175(3) 0.5727(2) 0.0323(7) Uani 1 1 d . . . . .
N9 N 0.7227(5) 0.3047(3) 0.6151(2) 0.0364(8) Uani 1 1 d . . . . .
C10 C 0.6661(6) 0.3888(4) 0.5698(3) 0.0442(11) Uani 1 1 d . . . . .
H10 H 0.644673 0.461444 0.583394 0.053 Uiso 1 1 calc R U . . .
C11 C 0.6417(7) 0.3573(4) 0.4991(3) 0.0519(13) Uani 1 1 d . . . . .
H11 H 0.601976 0.402944 0.457238 0.062 Uiso 1 1 calc R U . . .
C12 C 0.6868(7) 0.2482(4) 0.5030(3) 0.0439(11) Uani 1 1 d . . . . .
H12 H 0.684123 0.202056 0.464077 0.053 Uiso 1 1 calc R U . . .
N13 N 0.8876(5) 0.0320(3) 0.7940(2) 0.0423(9) Uani 1 1 d D . . . .
N14 N 0.8577(5) 0.1335(4) 0.8194(2) 0.0443(9) Uani 1 1 d D . . . .
C15A C 0.8558(14) 0.1321(8) 0.8948(4) 0.038(2) Uiso 0.5 1 d D . P A 1
H15A H 0.840042 0.192852 0.924339 0.045 Uiso 0.5 1 calc R U P A 1
C16A C 0.8822(14) 0.0218(7) 0.9222(5) 0.045(2) Uiso 0.5 1 d D . P A 1
H16A H 0.889027 -0.007248 0.974138 0.054 Uiso 0.5 1 calc R U P A 1
C17A C 0.8961(14) -0.0354(7) 0.8591(4) 0.040(2) Uiso 0.5 1 d D . P A 1
H17A H 0.909901 -0.112244 0.860938 0.048 Uiso 0.5 1 calc R U P A 1
C15B C 0.9013(15) 0.1033(8) 0.8896(5) 0.047(3) Uiso 0.5 1 d D . P A 2
H15B H 0.892558 0.154617 0.926390 0.056 Uiso 0.5 1 calc R U P A 2
C16B C 0.9596(16) -0.0054(8) 0.9066(6) 0.057(3) Uiso 0.5 1 d D . P A 2
H16B H 0.993758 -0.038989 0.953673 0.068 Uiso 0.5 1 calc R U P A 2
C17B C 0.9571(14) -0.0532(7) 0.8414(5) 0.043(2) Uiso 0.5 1 d D . P A 2
H17B H 0.993816 -0.126548 0.830790 0.051 Uiso 0.5 1 calc R U P A 2
N18 N 0.8673(6) -0.1712(3) 0.5755(2) 0.0458(10) Uani 1 1 d . . . . .
H18 H 0.843805 -0.161791 0.527963 0.055 Uiso 1 1 calc R U . . .
C19 C 0.9123(8) -0.2763(4) 0.6036(4) 0.0536(13) Uani 1 1 d . . . . .
O20 O 0.9536(8) -0.3013(3) 0.6665(3) 0.0853(16) Uani 1 1 d . . . . .
C21 C 0.9048(9) -0.3589(4) 0.5491(4) 0.0674(17) Uani 1 1 d . . . . .
H21A H 0.788851 -0.357933 0.542317 0.101 Uiso 1 1 calc R U . . .
H21B H 0.948670 -0.431172 0.570812 0.101 Uiso 1 1 calc R U . . .
H21C H 0.972002 -0.341369 0.498801 0.101 Uiso 1 1 calc R U . . .
N22 N 0.7121(5) 0.3960(3) 0.8009(2) 0.0342(7) Uani 1 1 d . . . . .
C23 C 0.8155(5) 0.4683(4) 0.8012(2) 0.0347(9) Uani 1 1 d . . . . .
C24 C 0.7759(6) 0.5597(4) 0.8403(3) 0.0386(9) Uani 1 1 d . . . . .
H24 H 0.853376 0.608928 0.838526 0.046 Uiso 1 1 calc R U . . .
C25 C 0.6159(6) 0.5766(4) 0.8830(3) 0.0410(10) Uani 1 1 d . . . . .
C26 C 0.5063(6) 0.5015(4) 0.8861(3) 0.0382(9) Uani 1 1 d . . . . .
H26 H 0.398187 0.510547 0.916230 0.046 Uiso 1 1 calc R U . . .
C27 C 0.5620(5) 0.4137(4) 0.8435(2) 0.0362(9) Uani 1 1 d . . . . .
N28 N 0.9720(5) 0.4406(3) 0.7556(2) 0.0353(8) Uani 1 1 d . . . . .
N29 N 0.9951(5) 0.3521(3) 0.7141(2) 0.0386(8) Uani 1 1 d . . . . .
C30 C 1.1501(6) 0.3462(4) 0.6771(3) 0.0450(11) Uani 1 1 d . . . . .
H30 H 1.202099 0.292057 0.643626 0.054 Uiso 1 1 calc R U . . .
C31 C 1.2277(6) 0.4309(4) 0.6940(3) 0.0455(11) Uani 1 1 d . . . . .
H31 H 1.338467 0.444454 0.674767 0.055 Uiso 1 1 calc R U . . .
C32 C 1.1116(6) 0.4891(4) 0.7434(3) 0.0419(10) Uani 1 1 d . . . . .
H32 H 1.125321 0.552124 0.765450 0.050 Uiso 1 1 calc R U . . .
N33 N 0.4628(5) 0.3333(3) 0.8392(2) 0.0388(8) Uani 1 1 d . . . . .
N34 N 0.5242(5) 0.2567(3) 0.7882(2) 0.0425(9) Uani 1 1 d . . . . .
C35 C 0.4081(7) 0.1930(5) 0.7978(3) 0.0498(12) Uani 1 1 d . . . . .
H35 H 0.415015 0.132008 0.769305 0.060 Uiso 1 1 calc R U . . .
C36 C 0.2740(7) 0.2252(5) 0.8544(3) 0.0582(14) Uani 1 1 d . . . . .
H36 H 0.177422 0.191056 0.871985 0.070 Uiso 1 1 calc R U . . .
C37 C 0.3114(7) 0.3163(5) 0.8792(3) 0.0510(12) Uani 1 1 d . . . . .
H37 H 0.244261 0.359425 0.917087 0.061 Uiso 1 1 calc R U . . .
N38 N 0.5577(6) 0.6682(4) 0.9238(3) 0.0493(10) Uani 1 1 d . . . . .
H38 H 0.482281 0.661178 0.965522 0.059 Uiso 1 1 calc R U . . .
C39 C 0.6093(8) 0.7686(4) 0.9037(3) 0.0563(14) Uani 1 1 d . . . . .
O40 O 0.7154(6) 0.7859(3) 0.8492(3) 0.0698(12) Uani 1 1 d . . . . .
C41 C 0.5181(10) 0.8553(5) 0.9554(5) 0.079(2) Uani 1 1 d . . . . .
H41A H 0.599055 0.894989 0.970575 0.118 Uiso 1 1 calc R U . . .
H41B H 0.455602 0.821055 1.001982 0.118 Uiso 1 1 calc R U . . .
H41C H 0.440808 0.905691 0.927175 0.118 Uiso 1 1 calc R U . . .
B42 B 0.7077(7) -0.0613(5) 0.3760(3) 0.0469(13) Uani 1 1 d D . . . .
F43A F 0.6524(10) 0.0360(4) 0.4098(3) 0.0739(19) Uani 0.67 1 d D . P B 1
F44A F 0.7681(9) -0.0442(6) 0.2990(3) 0.0609(15) Uani 0.67 1 d D . P B 1
F45A F 0.5744(6) -0.1188(5) 0.3855(4) 0.0706(15) Uani 0.67 1 d D . P B 1
F46A F 0.8301(6) -0.1250(4) 0.4160(3) 0.0523(11) Uani 0.67 1 d D . P B 1
F43B F 0.7355(15) 0.0391(9) 0.3953(7) 0.058(3) Uiso 0.33 1 d D . P B 2
F44B F 0.8093(19) -0.0818(12) 0.3044(7) 0.070(5) Uiso 0.33 1 d D . P B 2
F45B F 0.5465(15) -0.0595(14) 0.3661(10) 0.109(6) Uiso 0.33 1 d D . P B 2
F46B F 0.758(2) -0.1406(11) 0.4308(8) 0.095(5) Uiso 0.33 1 d D . P B 2
B47A B 0.1203(15) 0.6940(10) 0.9506(7) 0.048(4) Uiso 0.5 1 d D . P C 1
F48A F -0.0497(11) 0.7075(9) 0.9845(6) 0.078(4) Uiso 0.5 1 d D . P C 1
F49A F 0.1809(10) 0.7855(6) 0.9191(5) 0.081(2) Uiso 0.5 1 d D . P C 1
F50A F 0.1286(10) 0.6212(7) 0.8941(5) 0.073(2) Uiso 0.5 1 d D . P C 1
F51A F 0.2124(16) 0.6376(11) 1.0066(7) 0.089(7) Uiso 0.5 1 d D . P C 1
B47B B 0.0984(13) 0.6700(9) 0.9567(6) 0.044(3) Uiso 0.5 1 d D . P . .
F48B F 0.003(3) 0.7713(16) 0.9771(13) 0.103(10) Uiso 0.2 1 d D . P C 2
F49B F -0.021(3) 0.595(2) 0.9849(15) 0.151(13) Uiso 0.2 1 d D . P C 2
F50B F 0.1321(14) 0.6682(12) 0.8775(5) 0.026(2) Uiso 0.2 1 d D . P C 2
F51B F 0.2234(17) 0.6464(18) 1.0019(8) 0.018(4) Uiso 0.2 1 d D . P C 2
F48C F -0.0392(13) 0.7385(12) 0.9843(6) 0.042(3) Uiso 0.3 1 d D . P C 3
F49C F 0.095(2) 0.5642(10) 0.9511(10) 0.103(5) Uiso 0.3 1 d D . P C 3
F50C F 0.167(2) 0.7157(14) 0.8812(7) 0.100(5) Uiso 0.3 1 d D . P C 3
F51C F 0.2241(15) 0.6809(14) 1.0020(7) 0.064(5) Uiso 0.3 1 d D . P C 3
C52A C 0.555(2) 0.2087(10) 0.2662(8) 0.067(3) Uiso 0.5 1 d D . P D 1
H52A H 0.637842 0.215636 0.219428 0.100 Uiso 0.5 1 calc R U P D 1
H52B H 0.455093 0.186224 0.252815 0.100 Uiso 0.5 1 calc R U P D 1
H52C H 0.600962 0.154297 0.304325 0.100 Uiso 0.5 1 calc R U P D 1
C53A C 0.509(2) 0.3137(11) 0.2994(10) 0.052(5) Uiso 0.5 1 d D . P D 1
N54A N 0.480(2) 0.3987(12) 0.3201(12) 0.065(6) Uiso 0.5 1 d D . P D 1
C52B C 0.630(2) 0.2178(12) 0.2629(10) 0.079(4) Uiso 0.5 1 d D . P E 2
H52D H 0.564981 0.199236 0.225711 0.119 Uiso 0.5 1 calc R U P E 2
H52E H 0.640581 0.157941 0.303658 0.119 Uiso 0.5 1 calc R U P E 2
H52F H 0.740800 0.230124 0.235992 0.119 Uiso 0.5 1 calc R U P E 2
C53B C 0.545(2) 0.3159(13) 0.2976(11) 0.059(6) Uiso 0.5 1 d D . P E 2
N54B N 0.466(3) 0.3860(15) 0.3306(13) 0.082(8) Uiso 0.5 1 d D . P E 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.111(3) . ?
Fe1 N9 2.195(4) . ?
Fe1 N14 2.178(4) . ?
Fe1 N22 2.125(3) . ?
Fe1 N29 2.180(4) . ?
Fe1 N34 2.196(4) . ?
N2 C3 1.336(5) . ?
N2 C7 1.331(6) . ?
C3 C4 1.364(6) . ?
C3 N8 1.412(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.395(6) . ?
C5 C6 1.405(6) . ?
C5 N18 1.388(6) . ?
C6 H6 0.9500 . ?
C6 C7 1.369(6) . ?
C7 N13 1.409(5) . ?
N8 N9 1.372(5) . ?
N8 C12 1.353(6) . ?
N9 C10 1.319(6) . ?
C10 H10 0.9500 . ?
C10 C11 1.402(7) . ?
C11 H11 0.9500 . ?
C11 C12 1.357(7) . ?
C12 H12 0.9500 . ?
N13 N14 1.368(6) . ?
N13 C17A 1.346(7) . ?
N13 C17B 1.388(8) . ?
N14 C15A 1.322(7) . ?
N14 C15B 1.341(8) . ?
C15A H15A 0.9500 . ?
C15A C16A 1.407(9) . ?
C16A H16A 0.9500 . ?
C16A C17A 1.368(9) . ?
C17A H17A 0.9500 . ?
C15B H15B 0.9500 . ?
C15B C16B 1.387(9) . ?
C16B H16B 0.9500 . ?
C16B C17B 1.360(9) . ?
C17B H17B 0.9500 . ?
N18 H18 0.8800 . ?
N18 C19 1.370(7) . ?
C19 O20 1.204(8) . ?
C19 C21 1.504(8) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
N22 C23 1.340(6) . ?
N22 C27 1.328(6) . ?
C23 C24 1.370(6) . ?
C23 N28 1.408(6) . ?
C24 H24 0.9500 . ?
C24 C25 1.395(7) . ?
C25 C26 1.394(7) . ?
C25 N38 1.399(6) . ?
C26 H26 0.9500 . ?
C26 C27 1.376(6) . ?
C27 N33 1.411(6) . ?
N28 N29 1.368(5) . ?
N28 C32 1.357(6) . ?
N29 C30 1.322(6) . ?
C30 H30 0.9500 . ?
C30 C31 1.407(7) . ?
C31 H31 0.9500 . ?
C31 C32 1.355(7) . ?
C32 H32 0.9500 . ?
N33 N34 1.366(5) . ?
N33 C37 1.355(6) . ?
N34 C35 1.318(6) . ?
C35 H35 0.9500 . ?
C35 C36 1.392(8) . ?
C36 H36 0.9500 . ?
C36 C37 1.365(8) . ?
C37 H37 0.9500 . ?
N38 H38 0.8800 . ?
N38 C39 1.381(7) . ?
C39 O40 1.204(7) . ?
C39 C41 1.517(7) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
B42 F43A 1.395(7) . ?
B42 F44A 1.362(7) . ?
B42 F45A 1.382(7) . ?
B42 F46A 1.417(7) . ?
B42 F43B 1.403(11) . ?
B42 F44B 1.410(12) . ?
B42 F45B 1.364(12) . ?
B42 F46B 1.368(12) . ?
B47A F48A 1.413(13) . ?
B47A F49A 1.345(13) . ?
B47A F50A 1.410(12) . ?
B47A F51A 1.404(13) . ?
B47B F48B 1.433(15) . ?
B47B F49B 1.446(15) . ?
B47B F50B 1.373(12) . ?
B47B F51B 1.381(12) . ?
B47B F48C 1.361(12) . ?
B47B F49C 1.346(14) . ?
B47B F50C 1.440(14) . ?
B47B F51C 1.442(13) . ?
C52A H52A 0.9800 . ?
C52A H52B 0.9800 . ?
C52A H52C 0.9800 . ?
C52A C53A 1.469(13) . ?
C53A N54A 1.141(13) . ?
C52B H52D 0.9800 . ?
C52B H52E 0.9800 . ?
C52B H52F 0.9800 . ?
C52B C53B 1.458(14) . ?
C53B N54B 1.155(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N9 73.34(13) . . ?
N2 Fe1 N14 73.65(14) . . ?
N2 Fe1 N22 168.66(14) . . ?
N2 Fe1 N29 117.18(14) . . ?
N2 Fe1 N34 96.89(14) . . ?
N9 Fe1 N34 94.85(15) . . ?
N14 Fe1 N9 146.96(14) . . ?
N14 Fe1 N29 100.98(15) . . ?
N14 Fe1 N34 87.74(16) . . ?
N22 Fe1 N9 111.34(14) . . ?
N22 Fe1 N14 100.89(14) . . ?
N22 Fe1 N29 73.30(14) . . ?
N22 Fe1 N34 72.71(14) . . ?
N29 Fe1 N9 95.14(14) . . ?
N29 Fe1 N34 145.92(14) . . ?
C3 N2 Fe1 121.7(3) . . ?
C7 N2 Fe1 121.3(3) . . ?
C7 N2 C3 116.9(4) . . ?
N2 C3 C4 124.1(4) . . ?
N2 C3 N8 112.5(3) . . ?
C4 C3 N8 123.4(4) . . ?
C3 C4 H4 121.1 . . ?
C3 C4 C5 117.8(4) . . ?
C5 C4 H4 121.1 . . ?
C4 C5 C6 119.5(4) . . ?
N18 C5 C4 117.1(4) . . ?
N18 C5 C6 123.5(4) . . ?
C5 C6 H6 121.7 . . ?
C7 C6 C5 116.6(4) . . ?
C7 C6 H6 121.7 . . ?
N2 C7 C6 125.1(4) . . ?
N2 C7 N13 112.4(4) . . ?
C6 C7 N13 122.5(4) . . ?
N9 N8 C3 118.2(3) . . ?
C12 N8 C3 130.4(4) . . ?
C12 N8 N9 111.3(4) . . ?
N8 N9 Fe1 114.2(3) . . ?
C10 N9 Fe1 141.0(3) . . ?
C10 N9 N8 104.7(4) . . ?
N9 C10 H10 124.3 . . ?
N9 C10 C11 111.4(4) . . ?
C11 C10 H10 124.3 . . ?
C10 C11 H11 127.2 . . ?
C12 C11 C10 105.7(4) . . ?
C12 C11 H11 127.2 . . ?
N8 C12 C11 106.9(4) . . ?
N8 C12 H12 126.5 . . ?
C11 C12 H12 126.5 . . ?
N14 N13 C7 118.5(4) . . ?
N14 N13 C17B 118.2(5) . . ?
C17A N13 C7 135.0(5) . . ?
C17A N13 N14 104.3(5) . . ?
C17B N13 C7 122.9(5) . . ?
N13 N14 Fe1 114.0(2) . . ?
C15A N14 Fe1 132.1(5) . . ?
C15A N14 N13 113.0(5) . . ?
C15B N14 Fe1 149.3(5) . . ?
C15B N14 N13 96.4(6) . . ?
N14 C15A H15A 127.3 . . ?
N14 C15A C16A 105.5(7) . . ?
C16A C15A H15A 127.3 . . ?
C15A C16A H16A 126.9 . . ?
C17A C16A C15A 106.2(8) . . ?
C17A C16A H16A 126.9 . . ?
N13 C17A C16A 110.9(7) . . ?
N13 C17A H17A 124.6 . . ?
C16A C17A H17A 124.6 . . ?
N14 C15B H15B 121.2 . . ?
N14 C15B C16B 117.7(9) . . ?
C16B C15B H15B 121.2 . . ?
C15B C16B H16B 127.5 . . ?
C17B C16B C15B 104.9(9) . . ?
C17B C16B H16B 127.5 . . ?
N13 C17B H17B 128.7 . . ?
C16B C17B N13 102.5(8) . . ?
C16B C17B H17B 128.7 . . ?
C5 N18 H18 116.0 . . ?
C19 N18 C5 128.0(5) . . ?
C19 N18 H18 116.0 . . ?
N18 C19 C21 114.1(5) . . ?
O20 C19 N18 123.4(5) . . ?
O20 C19 C21 122.5(5) . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 N22 Fe1 121.2(3) . . ?
C27 N22 Fe1 121.8(3) . . ?
C27 N22 C23 116.9(4) . . ?
N22 C23 C24 124.8(4) . . ?
N22 C23 N28 112.2(4) . . ?
C24 C23 N28 123.0(4) . . ?
C23 C24 H24 121.7 . . ?
C23 C24 C25 116.5(4) . . ?
C25 C24 H24 121.7 . . ?
C24 C25 N38 122.4(4) . . ?
C26 C25 C24 120.4(4) . . ?
C26 C25 N38 117.2(4) . . ?
C25 C26 H26 121.5 . . ?
C27 C26 C25 116.9(4) . . ?
C27 C26 H26 121.5 . . ?
N22 C27 C26 124.4(4) . . ?
N22 C27 N33 112.5(4) . . ?
C26 C27 N33 123.1(4) . . ?
N29 N28 C23 118.5(4) . . ?
C32 N28 C23 130.6(4) . . ?
C32 N28 N29 110.8(4) . . ?
N28 N29 Fe1 114.6(3) . . ?
C30 N29 Fe1 139.9(3) . . ?
C30 N29 N28 105.3(4) . . ?
N29 C30 H30 124.6 . . ?
N29 C30 C31 110.9(4) . . ?
C31 C30 H30 124.6 . . ?
C30 C31 H31 127.2 . . ?
C32 C31 C30 105.6(4) . . ?
C32 C31 H31 127.2 . . ?
N28 C32 H32 126.3 . . ?
C31 C32 N28 107.3(4) . . ?
C31 C32 H32 126.3 . . ?
N34 N33 C27 117.9(4) . . ?
C37 N33 C27 130.5(4) . . ?
C37 N33 N34 111.6(4) . . ?
N33 N34 Fe1 114.7(3) . . ?
C35 N34 Fe1 140.2(4) . . ?
C35 N34 N33 104.3(4) . . ?
N34 C35 H35 123.9 . . ?
N34 C35 C36 112.3(5) . . ?
C36 C35 H35 123.9 . . ?
C35 C36 H36 127.4 . . ?
C37 C36 C35 105.1(5) . . ?
C37 C36 H36 127.4 . . ?
N33 C37 C36 106.7(5) . . ?
N33 C37 H37 126.6 . . ?
C36 C37 H37 126.6 . . ?
C25 N38 H38 117.4 . . ?
C39 N38 C25 125.1(4) . . ?
C39 N38 H38 117.4 . . ?
N38 C39 C41 114.0(5) . . ?
O40 C39 N38 122.7(5) . . ?
O40 C39 C41 123.2(6) . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
F43A B42 F46A 109.8(5) . . ?
F44A B42 F43A 111.8(6) . . ?
F44A B42 F45A 109.5(5) . . ?
F44A B42 F46A 110.8(5) . . ?
F45A B42 F43A 108.0(6) . . ?
F45A B42 F46A 106.8(5) . . ?
F43B B42 F44B 107.5(8) . . ?
F45B B42 F43B 111.7(9) . . ?
F45B B42 F44B 107.3(10) . . ?
F45B B42 F46B 113.2(10) . . ?
F46B B42 F43B 108.9(9) . . ?
F46B B42 F44B 108.0(9) . . ?
F49A B47A F48A 115.6(10) . . ?
F49A B47A F50A 111.3(10) . . ?
F49A B47A F51A 112.0(11) . . ?
F50A B47A F48A 103.6(9) . . ?
F51A B47A F48A 107.8(10) . . ?
F51A B47A F50A 105.8(10) . . ?
F48B B47B F49B 101.5(13) . . ?
F50B B47B F48B 110.4(12) . . ?
F50B B47B F49B 106.6(12) . . ?
F50B B47B F51B 121.7(10) . . ?
F51B B47B F48B 107.5(12) . . ?
F51B B47B F49B 107.3(13) . . ?
F48C B47B F50C 108.1(10) . . ?
F48C B47B F51C 105.7(10) . . ?
F49C B47B F48C 122.6(12) . . ?
F49C B47B F50C 107.2(11) . . ?
F49C B47B F51C 109.7(11) . . ?
F50C B47B F51C 101.5(10) . . ?
H52A C52A H52B 109.5 . . ?
H52A C52A H52C 109.5 . . ?
H52B C52A H52C 109.5 . . ?
C53A C52A H52A 109.5 . . ?
C53A C52A H52B 109.5 . . ?
C53A C52A H52C 109.5 . . ?
N54A C53A C52A 175(2) . . ?
H52D C52B H52E 109.5 . . ?
H52D C52B H52F 109.5 . . ?
H52E C52B H52F 109.5 . . ?
C53B C52B H52D 109.5 . . ?
C53B C52B H52E 109.5 . . ?
C53B C52B H52F 109.5 . . ?
N54B C53B C52B 172(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N18 H18 F46A 0.88 1.99 2.854(6) 168.5 . yes
N18 H18 F46B 0.88 1.93 2.808(14) 171.4 . yes
N38 H38 F51A 0.88 2.27 3.019(14) 143.3 . yes
N38 H38 F51B 0.88 2.15 2.892(18) 142.2 . yes
N38 H38 F51C 0.88 2.09 2.837(14) 141.7 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N2 C3 C4 -179.5(3) . . . . ?
Fe1 N2 C3 N8 0.0(5) . . . . ?
Fe1 N2 C7 C6 178.5(4) . . . . ?
Fe1 N2 C7 N13 -0.6(5) . . . . ?
Fe1 N9 C10 C11 -174.8(4) . . . . ?
Fe1 N14 C15A C16A 167.0(6) . . . . ?
Fe1 N14 C15B C16B -171.0(7) . . . . ?
Fe1 N22 C23 C24 176.3(4) . . . . ?
Fe1 N22 C23 N28 -3.1(5) . . . . ?
Fe1 N22 C27 C26 -176.9(4) . . . . ?
Fe1 N22 C27 N33 1.7(5) . . . . ?
Fe1 N29 C30 C31 -175.7(4) . . . . ?
Fe1 N34 C35 C36 167.2(4) . . . . ?
N2 C3 C4 C5 1.8(7) . . . . ?
N2 C3 N8 N9 0.7(5) . . . . ?
N2 C3 N8 C12 -175.6(4) . . . . ?
N2 C7 N13 N14 1.6(6) . . . . ?
N2 C7 N13 C17A 161.8(8) . . . . ?
N2 C7 N13 C17B -171.2(7) . . . . ?
C3 N2 C7 C6 0.0(7) . . . . ?
C3 N2 C7 N13 -179.2(4) . . . . ?
C3 C4 C5 C6 -1.6(7) . . . . ?
C3 C4 C5 N18 177.9(4) . . . . ?
C3 N8 N9 Fe1 -1.0(5) . . . . ?
C3 N8 N9 C10 -177.7(4) . . . . ?
C3 N8 C12 C11 177.2(5) . . . . ?
C4 C3 N8 N9 -179.8(4) . . . . ?
C4 C3 N8 C12 3.9(7) . . . . ?
C4 C5 C6 C7 0.7(7) . . . . ?
C4 C5 N18 C19 179.3(5) . . . . ?
C5 C6 C7 N2 0.1(7) . . . . ?
C5 C6 C7 N13 179.2(4) . . . . ?
C5 N18 C19 O20 -2.7(10) . . . . ?
C5 N18 C19 C21 177.0(5) . . . . ?
C6 C5 N18 C19 -1.1(8) . . . . ?
C6 C7 N13 N14 -177.5(4) . . . . ?
C6 C7 N13 C17A -17.4(11) . . . . ?
C6 C7 N13 C17B 9.6(9) . . . . ?
C7 N2 C3 C4 -1.0(6) . . . . ?
C7 N2 C3 N8 178.5(4) . . . . ?
C7 N13 N14 Fe1 -1.8(5) . . . . ?
C7 N13 N14 C15A 168.8(6) . . . . ?
C7 N13 N14 C15B -178.1(6) . . . . ?
C7 N13 C17A C16A -165.7(7) . . . . ?
C7 N13 C17B C16B 178.6(7) . . . . ?
N8 C3 C4 C5 -177.6(4) . . . . ?
N8 N9 C10 C11 0.5(6) . . . . ?
N9 N8 C12 C11 0.7(6) . . . . ?
N9 C10 C11 C12 -0.1(7) . . . . ?
C10 C11 C12 N8 -0.4(6) . . . . ?
C12 N8 N9 Fe1 176.0(3) . . . . ?
C12 N8 N9 C10 -0.7(5) . . . . ?
N13 N14 C15A C16A -1.6(10) . . . . ?
N13 N14 C15B C16B 2.3(11) . . . . ?
N14 N13 C17A C16A -3.6(10) . . . . ?
N14 N13 C17B C16B 5.7(11) . . . . ?
N14 C15A C16A C17A -0.7(12) . . . . ?
N14 C15B C16B C17B 0.8(15) . . . . ?
C15A C16A C17A N13 2.7(12) . . . . ?
C17A N13 N14 Fe1 -167.5(5) . . . . ?
C17A N13 N14 C15A 3.2(8) . . . . ?
C15B C16B C17B N13 -3.5(12) . . . . ?
C17B N13 N14 Fe1 171.4(6) . . . . ?
C17B N13 N14 C15B -4.9(9) . . . . ?
N18 C5 C6 C7 -178.8(4) . . . . ?
N22 C23 C24 C25 0.4(7) . . . . ?
N22 C23 N28 N29 4.4(6) . . . . ?
N22 C23 N28 C32 -176.9(4) . . . . ?
N22 C27 N33 N34 -6.0(6) . . . . ?
N22 C27 N33 C37 172.7(5) . . . . ?
C23 N22 C27 C26 1.3(7) . . . . ?
C23 N22 C27 N33 179.9(4) . . . . ?
C23 C24 C25 C26 1.6(7) . . . . ?
C23 C24 C25 N38 -178.2(4) . . . . ?
C23 N28 N29 Fe1 -3.7(5) . . . . ?
C23 N28 N29 C30 179.6(4) . . . . ?
C23 N28 C32 C31 -179.4(5) . . . . ?
C24 C23 N28 N29 -175.0(4) . . . . ?
C24 C23 N28 C32 3.6(7) . . . . ?
C24 C25 C26 C27 -2.1(7) . . . . ?
C24 C25 N38 C39 29.1(8) . . . . ?
C25 C26 C27 N22 0.6(7) . . . . ?
C25 C26 C27 N33 -177.8(4) . . . . ?
C25 N38 C39 O40 -2.4(10) . . . . ?
C25 N38 C39 C41 176.5(6) . . . . ?
C26 C25 N38 C39 -150.7(5) . . . . ?
C26 C27 N33 N34 172.6(4) . . . . ?
C26 C27 N33 C37 -8.7(8) . . . . ?
C27 N22 C23 C24 -1.9(7) . . . . ?
C27 N22 C23 N28 178.7(4) . . . . ?
C27 N33 N34 Fe1 7.3(5) . . . . ?
C27 N33 N34 C35 179.0(4) . . . . ?
C27 N33 C37 C36 -177.9(5) . . . . ?
N28 C23 C24 C25 179.8(4) . . . . ?
N28 N29 C30 C31 -0.4(6) . . . . ?
N29 N28 C32 C31 -0.7(5) . . . . ?
N29 C30 C31 C32 0.0(6) . . . . ?
C30 C31 C32 N28 0.4(6) . . . . ?
C32 N28 N29 Fe1 177.4(3) . . . . ?
C32 N28 N29 C30 0.7(5) . . . . ?
N33 N34 C35 C36 -0.9(6) . . . . ?
N34 N33 C37 C36 0.9(6) . . . . ?
N34 C35 C36 C37 1.4(7) . . . . ?
C35 C36 C37 N33 -1.3(6) . . . . ?
C37 N33 N34 Fe1 -171.6(3) . . . . ?
C37 N33 N34 C35 0.0(6) . . . . ?
N38 C25 C26 C27 177.7(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.603(4)
2 0.397(4)

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile/diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_80acn125
_database_code_depnum_ccdc_archive 'CCDC 2078649'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2021-04-19 deposited with the CCDC.	2021-06-10 downloaded from the CCDC.
;
_audit_creation_date             2020-07-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis-[N-(2,6-di{pyrazol-1-yl}pyrid-4-yl)acetamide]iron(II)ditetrafluoroborate acetonitrile solvate'
_chemical_formula_moiety         'C26 H24 Fe N12 O2, 2(B F4), C2 H3 N'
_chemical_formula_sum            'C28 H27 B2 F8 Fe N13 O2'
_chemical_formula_weight         807.09
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2204(5)
_cell_length_b                   12.3298(10)
_cell_length_c                   17.2739(14)
_cell_angle_alpha                82.969(7)
_cell_angle_beta                 79.317(6)
_cell_angle_gamma                85.481(6)
_cell_volume                     1704.7(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3160
_cell_measurement_temperature    125(2)
_cell_measurement_theta_min      4.25
_cell_measurement_theta_max      72.88
_exptl_absorpt_coefficient_mu    4.395
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.1020
_diffrn_reflns_Laue_measured_fraction_full 0.939
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6359
_diffrn_reflns_point_group_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.592
_diffrn_reflns_theta_min         3.618
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      125(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4744
_reflns_number_total             6359
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2015)'
_refine_diff_density_max         1.060
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         6359
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1117
_refine_ls_R_factor_gt           0.0862
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0909P)²+5.8415P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2333
_refine_ls_wR_factor_ref         0.2517
_refine_special_details          
;The data were resolved into two non-superimposable twin domains, in a 
 ratio of 0.57:0.43.

 No disorder is present in the model, and no restraints were applied to the
 refinement. All non-H atoms were refined anisotropically and H atoms were 
 placed in calculated positions and refined using a riding model.,Twin
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.567(4)
 0.433(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17),
 N18(H18), C24(H24), C26(H26), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36),
  C37(H37), N38(H38)
3.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C41(H41A,H41B,H41C), C52(H52A,H52B,H52C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.76267(12) 0.76456(8) 0.73233(6) 0.0205(3) Uani 1 1 d . . . . .
N2 N 0.8142(6) 0.6320(4) 0.6848(3) 0.0231(11) Uani 1 1 d . . . . .
C3 C 0.7892(8) 0.6254(5) 0.6119(4) 0.0234(13) Uani 1 1 d . . . . .
C4 C 0.8102(8) 0.5305(5) 0.5764(4) 0.0250(13) Uani 1 1 d . . . . .
H4 H 0.793733 0.529555 0.523539 0.030 Uiso 1 1 calc R U . . .
C5 C 0.8571(8) 0.4348(5) 0.6219(4) 0.0264(14) Uani 1 1 d . . . . .
C6 C 0.8788(8) 0.4386(5) 0.7004(4) 0.0264(14) Uani 1 1 d . . . . .
H6 H 0.907442 0.374320 0.732497 0.032 Uiso 1 1 calc R U . . .
C7 C 0.8568(8) 0.5389(5) 0.7286(4) 0.0223(13) Uani 1 1 d . . . . .
N8 N 0.7338(7) 0.7281(5) 0.5774(3) 0.0255(12) Uani 1 1 d . . . . .
N9 N 0.7134(7) 0.8127(4) 0.6246(3) 0.0234(11) Uani 1 1 d . . . . .
C10 C 0.6576(8) 0.8968(5) 0.5819(5) 0.0324(16) Uani 1 1 d . . . . .
H10 H 0.631710 0.967444 0.599143 0.039 Uiso 1 1 calc R U . . .
C11 C 0.6405(9) 0.8698(6) 0.5067(5) 0.0330(15) Uani 1 1 d . . . . .
H11 H 0.602730 0.916878 0.465052 0.040 Uiso 1 1 calc R U . . .
C12 C 0.6900(9) 0.7609(6) 0.5068(4) 0.0294(14) Uani 1 1 d . . . . .
H12 H 0.692834 0.717140 0.464970 0.035 Uiso 1 1 calc R U . . .
N13 N 0.8667(7) 0.5619(4) 0.8050(3) 0.0257(12) Uani 1 1 d . . . . .
N14 N 0.8306(6) 0.6680(4) 0.8213(3) 0.0201(10) Uani 1 1 d . . . . .
C15 C 0.8348(8) 0.6694(6) 0.8963(4) 0.0282(14) Uani 1 1 d . . . . .
H15 H 0.815430 0.732626 0.923885 0.034 Uiso 1 1 calc R U . . .
C16 C 0.8720(9) 0.5637(6) 0.9298(4) 0.0322(15) Uani 1 1 d . . . . .
H16 H 0.879765 0.542316 0.983748 0.039 Uiso 1 1 calc R U . . .
C17 C 0.8953(8) 0.4964(6) 0.8710(4) 0.0288(14) Uani 1 1 d . . . . .
H17 H 0.925050 0.420188 0.875261 0.035 Uiso 1 1 calc R U . . .
N18 N 0.8721(8) 0.3396(4) 0.5857(3) 0.0293(12) Uani 1 1 d . . . . .
H18 H 0.845476 0.346177 0.538219 0.035 Uiso 1 1 calc R U . . .
C19 C 0.9235(10) 0.2354(6) 0.6145(5) 0.0325(15) Uani 1 1 d . . . . .
O20 O 0.9721(9) 0.2163(4) 0.6766(4) 0.0485(15) Uani 1 1 d . . . . .
C21 C 0.9089(10) 0.1499(6) 0.5613(5) 0.0411(19) Uani 1 1 d . . . . .
H21A H 0.981727 0.085572 0.573098 0.062 Uiso 1 1 calc R U . . .
H21B H 0.941469 0.179835 0.505850 0.062 Uiso 1 1 calc R U . . .
H21C H 0.793856 0.128729 0.570451 0.062 Uiso 1 1 calc R U . . .
N22 N 0.6987(6) 0.8892(4) 0.7877(3) 0.0222(11) Uani 1 1 d . . . . .
C23 C 0.8083(8) 0.9639(5) 0.7890(4) 0.0233(13) Uani 1 1 d . . . . .
C24 C 0.7712(8) 1.0545(5) 0.8298(4) 0.0265(14) Uani 1 1 d . . . . .
H24 H 0.850808 1.106770 0.828640 0.032 Uiso 1 1 calc R U . . .
C25 C 0.6101(8) 1.0656(5) 0.8730(4) 0.0253(13) Uani 1 1 d . . . . .
C26 C 0.4954(8) 0.9858(5) 0.8756(4) 0.0255(13) Uani 1 1 d . . . . .
H26 H 0.387159 0.990962 0.906349 0.031 Uiso 1 1 calc R U . . .
C27 C 0.5471(8) 0.9004(5) 0.8318(4) 0.0265(14) Uani 1 1 d . . . . .
N28 N 0.9621(7) 0.9349(4) 0.7445(3) 0.0243(11) Uani 1 1 d . . . . .
N29 N 0.9747(7) 0.8392(4) 0.7089(3) 0.0229(11) Uani 1 1 d . . . . .
C30 C 1.1297(8) 0.8299(5) 0.6719(4) 0.0235(13) Uani 1 1 d . . . . .
H30 H 1.174865 0.772081 0.641370 0.028 Uiso 1 1 calc R U . . .
C31 C 1.2198(8) 0.9177(6) 0.6839(4) 0.0286(14) Uani 1 1 d . . . . .
H31 H 1.333678 0.929046 0.664134 0.034 Uiso 1 1 calc R U . . .
C32 C 1.1102(8) 0.9826(5) 0.7297(4) 0.0259(13) Uani 1 1 d . . . . .
H32 H 1.132754 1.048651 0.747735 0.031 Uiso 1 1 calc R U . . .
N33 N 0.4539(7) 0.8109(4) 0.8258(3) 0.0251(11) Uani 1 1 d . . . . .
N34 N 0.5308(6) 0.7353(4) 0.7768(3) 0.0225(11) Uani 1 1 d . . . . .
C35 C 0.4220(8) 0.6598(6) 0.7832(4) 0.0280(14) Uani 1 1 d . . . . .
H35 H 0.439260 0.596475 0.755750 0.034 Uiso 1 1 calc R U . . .
C36 C 0.2783(8) 0.6861(6) 0.8359(5) 0.0315(16) Uani 1 1 d . . . . .
H36 H 0.183461 0.643929 0.851270 0.038 Uiso 1 1 calc R U . . .
C37 C 0.2992(8) 0.7833(6) 0.8611(5) 0.0318(15) Uani 1 1 d . . . . .
H37 H 0.221513 0.823551 0.896276 0.038 Uiso 1 1 calc R U . . .
N38 N 0.5543(7) 1.1537(5) 0.9162(4) 0.0294(12) Uani 1 1 d . . . . .
H38 H 0.468039 1.143885 0.954421 0.035 Uiso 1 1 calc R U . . .
C39 C 0.6210(9) 1.2550(6) 0.9050(4) 0.0300(15) Uani 1 1 d . . . . .
O40 O 0.7424(7) 1.2778(4) 0.8546(4) 0.0415(13) Uani 1 1 d . . . . .
C41 C 0.5257(11) 1.3368(6) 0.9561(6) 0.045(2) Uani 1 1 d . . . . .
H41A H 0.510683 1.305574 1.011758 0.068 Uiso 1 1 calc R U . . .
H41B H 0.416977 1.354825 0.940746 0.068 Uiso 1 1 calc R U . . .
H41C H 0.587011 1.403283 0.949227 0.068 Uiso 1 1 calc R U . . .
B42 B 0.7127(10) 0.4530(7) 0.3808(5) 0.0306(17) Uani 1 1 d . . . . .
F43 F 0.7105(10) 0.5551(4) 0.4055(3) 0.0704(19) Uani 1 1 d . . . . .
F44 F 0.5590(7) 0.4166(8) 0.3900(4) 0.093(3) Uani 1 1 d . . . . .
F45 F 0.7874(6) 0.4552(4) 0.3025(3) 0.0431(11) Uani 1 1 d . . . . .
F46 F 0.8077(7) 0.3827(4) 0.4274(3) 0.0547(14) Uani 1 1 d . . . . .
B47 B 0.0989(11) 1.1711(7) 0.9478(5) 0.0359(19) Uani 1 1 d . . . . .
F48 F 0.1298(6) 1.1183(4) 0.8796(3) 0.0456(12) Uani 1 1 d . . . . .
F49 F -0.0562(6) 1.1534(6) 0.9883(4) 0.0682(17) Uani 1 1 d . . . . .
F50 F 0.1208(8) 1.2827(4) 0.9279(4) 0.0615(15) Uani 1 1 d . . . . .
F51 F 0.2180(5) 1.1290(3) 0.9958(3) 0.0366(10) Uani 1 1 d . . . . .
C52 C 0.618(2) 0.7109(9) 0.2548(6) 0.081(4) Uani 1 1 d . . . . .
H52A H 0.719864 0.681182 0.273840 0.121 Uiso 1 1 calc R U . . .
H52B H 0.644069 0.732242 0.197542 0.121 Uiso 1 1 calc R U . . .
H52C H 0.536269 0.655075 0.266104 0.121 Uiso 1 1 calc R U . . .
C53 C 0.5521(11) 0.8063(7) 0.2949(5) 0.0398(18) Uani 1 1 d . . . . .
N54 N 0.4999(10) 0.8797(6) 0.3267(5) 0.0511(19) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.901(5) . ?
Fe1 N9 1.988(6) . ?
Fe1 N14 1.964(5) . ?
Fe1 N22 1.896(5) . ?
Fe1 N29 1.987(5) . ?
Fe1 N34 1.962(5) . ?
N2 C3 1.327(9) . ?
N2 C7 1.355(8) . ?
C3 C4 1.370(9) . ?
C3 N8 1.410(9) . ?
C4 H4 0.9500 . ?
C4 C5 1.404(10) . ?
C5 C6 1.406(10) . ?
C5 N18 1.383(8) . ?
C6 H6 0.9500 . ?
C6 C7 1.372(9) . ?
C7 N13 1.400(9) . ?
N8 N9 1.382(7) . ?
N8 C12 1.341(9) . ?
N9 C10 1.301(10) . ?
C10 H10 0.9500 . ?
C10 C11 1.415(11) . ?
C11 H11 0.9500 . ?
C11 C12 1.372(10) . ?
C12 H12 0.9500 . ?
N13 N14 1.371(7) . ?
N13 C17 1.360(9) . ?
N14 C15 1.305(9) . ?
C15 H15 0.9500 . ?
C15 C16 1.394(10) . ?
C16 H16 0.9500 . ?
C16 C17 1.366(10) . ?
C17 H17 0.9500 . ?
N18 H18 0.8800 . ?
N18 C19 1.383(9) . ?
C19 O20 1.204(10) . ?
C19 C21 1.505(10) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
N22 C23 1.343(8) . ?
N22 C27 1.341(9) . ?
C23 C24 1.378(9) . ?
C23 N28 1.397(9) . ?
C24 H24 0.9500 . ?
C24 C25 1.400(10) . ?
C25 C26 1.407(9) . ?
C25 N38 1.393(8) . ?
C26 H26 0.9500 . ?
C26 C27 1.366(9) . ?
C27 N33 1.416(9) . ?
N28 N29 1.385(7) . ?
N28 C32 1.362(8) . ?
N29 C30 1.318(8) . ?
C30 H30 0.9500 . ?
C30 C31 1.415(9) . ?
C31 H31 0.9500 . ?
C31 C32 1.361(10) . ?
C32 H32 0.9500 . ?
N33 N34 1.374(8) . ?
N33 C37 1.355(9) . ?
N34 C35 1.322(8) . ?
C35 H35 0.9500 . ?
C35 C36 1.393(10) . ?
C36 H36 0.9500 . ?
C36 C37 1.358(10) . ?
C37 H37 0.9500 . ?
N38 H38 0.8800 . ?
N38 C39 1.381(9) . ?
C39 O40 1.222(9) . ?
C39 C41 1.499(10) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
B42 F43 1.376(9) . ?
B42 F44 1.349(10) . ?
B42 F45 1.375(10) . ?
B42 F46 1.402(10) . ?
B47 F48 1.389(9) . ?
B47 F49 1.356(11) . ?
B47 F50 1.394(11) . ?
B47 F51 1.424(10) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C52 C53 1.456(13) . ?
C53 N54 1.131(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N9 79.5(2) . . ?
N2 Fe1 N14 79.9(2) . . ?
N2 Fe1 N29 104.3(2) . . ?
N2 Fe1 N34 95.9(2) . . ?
N14 Fe1 N9 159.4(2) . . ?
N14 Fe1 N29 92.7(2) . . ?
N22 Fe1 N2 174.6(2) . . ?
N22 Fe1 N9 103.8(2) . . ?
N22 Fe1 N14 96.7(2) . . ?
N22 Fe1 N29 79.9(2) . . ?
N22 Fe1 N34 79.9(2) . . ?
N29 Fe1 N9 92.4(2) . . ?
N34 Fe1 N9 93.1(2) . . ?
N34 Fe1 N14 89.0(2) . . ?
N34 Fe1 N29 159.7(2) . . ?
C3 N2 Fe1 120.9(5) . . ?
C3 N2 C7 118.5(6) . . ?
C7 N2 Fe1 120.0(4) . . ?
N2 C3 C4 124.1(6) . . ?
N2 C3 N8 110.7(6) . . ?
C4 C3 N8 125.2(6) . . ?
C3 C4 H4 121.5 . . ?
C3 C4 C5 117.0(6) . . ?
C5 C4 H4 121.5 . . ?
C4 C5 C6 120.2(6) . . ?
N18 C5 C4 115.8(6) . . ?
N18 C5 C6 123.9(6) . . ?
C5 C6 H6 121.4 . . ?
C7 C6 C5 117.2(6) . . ?
C7 C6 H6 121.4 . . ?
N2 C7 C6 123.0(6) . . ?
N2 C7 N13 109.7(5) . . ?
C6 C7 N13 127.3(6) . . ?
N9 N8 C3 116.1(5) . . ?
C12 N8 C3 132.4(6) . . ?
C12 N8 N9 111.4(5) . . ?
N8 N9 Fe1 112.5(4) . . ?
C10 N9 Fe1 142.1(5) . . ?
C10 N9 N8 105.2(5) . . ?
N9 C10 H10 124.3 . . ?
N9 C10 C11 111.4(6) . . ?
C11 C10 H10 124.3 . . ?
C10 C11 H11 127.4 . . ?
C12 C11 C10 105.1(7) . . ?
C12 C11 H11 127.4 . . ?
N8 C12 C11 106.9(6) . . ?
N8 C12 H12 126.6 . . ?
C11 C12 H12 126.6 . . ?
N14 N13 C7 117.1(5) . . ?
C17 N13 C7 132.2(6) . . ?
C17 N13 N14 110.6(5) . . ?
N13 N14 Fe1 113.0(4) . . ?
C15 N14 Fe1 139.4(5) . . ?
C15 N14 N13 106.9(5) . . ?
N14 C15 H15 125.3 . . ?
N14 C15 C16 109.4(6) . . ?
C16 C15 H15 125.3 . . ?
C15 C16 H16 126.1 . . ?
C17 C16 C15 107.7(6) . . ?
C17 C16 H16 126.1 . . ?
N13 C17 C16 105.3(6) . . ?
N13 C17 H17 127.3 . . ?
C16 C17 H17 127.4 . . ?
C5 N18 H18 115.8 . . ?
C5 N18 C19 128.3(6) . . ?
C19 N18 H18 115.8 . . ?
N18 C19 C21 113.2(7) . . ?
O20 C19 N18 122.5(6) . . ?
O20 C19 C21 124.3(7) . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 N22 Fe1 120.8(4) . . ?
C27 N22 Fe1 120.9(4) . . ?
C27 N22 C23 118.2(5) . . ?
N22 C23 C24 123.7(6) . . ?
N22 C23 N28 110.2(5) . . ?
C24 C23 N28 126.1(6) . . ?
C23 C24 H24 121.7 . . ?
C23 C24 C25 116.6(6) . . ?
C25 C24 H24 121.7 . . ?
C24 C25 C26 120.8(6) . . ?
N38 C25 C24 122.9(6) . . ?
N38 C25 C26 116.3(6) . . ?
C25 C26 H26 121.6 . . ?
C27 C26 C25 116.9(6) . . ?
C27 C26 H26 121.6 . . ?
N22 C27 C26 123.8(6) . . ?
N22 C27 N33 109.5(6) . . ?
C26 C27 N33 126.7(6) . . ?
N29 N28 C23 117.2(5) . . ?
C32 N28 C23 132.0(6) . . ?
C32 N28 N29 110.8(5) . . ?
N28 N29 Fe1 111.9(4) . . ?
C30 N29 Fe1 142.7(5) . . ?
C30 N29 N28 105.4(5) . . ?
N29 C30 H30 124.6 . . ?
N29 C30 C31 110.9(6) . . ?
C31 C30 H30 124.6 . . ?
C30 C31 H31 127.0 . . ?
C32 C31 C30 106.0(6) . . ?
C32 C31 H31 127.0 . . ?
N28 C32 H32 126.5 . . ?
C31 C32 N28 107.0(6) . . ?
C31 C32 H32 126.5 . . ?
N34 N33 C27 116.5(5) . . ?
C37 N33 C27 131.7(6) . . ?
C37 N33 N34 111.8(5) . . ?
N33 N34 Fe1 113.1(4) . . ?
C35 N34 Fe1 141.6(5) . . ?
C35 N34 N33 104.8(5) . . ?
N34 C35 H35 124.8 . . ?
N34 C35 C36 110.5(6) . . ?
C36 C35 H35 124.8 . . ?
C35 C36 H36 126.4 . . ?
C37 C36 C35 107.2(6) . . ?
C37 C36 H36 126.4 . . ?
N33 C37 C36 105.6(6) . . ?
N33 C37 H37 127.2 . . ?
C36 C37 H37 127.2 . . ?
C25 N38 H38 116.8 . . ?
C39 N38 C25 126.5(6) . . ?
C39 N38 H38 116.8 . . ?
N38 C39 C41 114.3(7) . . ?
O40 C39 N38 122.7(6) . . ?
O40 C39 C41 122.8(7) . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
F43 B42 F46 106.4(6) . . ?
F44 B42 F43 112.1(8) . . ?
F44 B42 F45 109.5(6) . . ?
F44 B42 F46 109.7(8) . . ?
F45 B42 F43 110.0(7) . . ?
F45 B42 F46 109.1(6) . . ?
F48 B47 F50 109.7(7) . . ?
F48 B47 F51 108.2(6) . . ?
F49 B47 F48 110.5(7) . . ?
F49 B47 F50 111.1(7) . . ?
F49 B47 F51 109.8(7) . . ?
F50 B47 F51 107.5(7) . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C53 C52 H52A 109.5 . . ?
C53 C52 H52B 109.5 . . ?
C53 C52 H52C 109.5 . . ?
N54 C53 C52 179.3(10) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N18 H18 F46 0.88 1.99 2.860(8) 170.5 . yes
N38 H38 F51 0.88 2.06 2.872(8) 152.6 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N2 C3 C4 -174.3(5) . . . . ?
Fe1 N2 C3 N8 4.0(7) . . . . ?
Fe1 N2 C7 C6 173.1(5) . . . . ?
Fe1 N2 C7 N13 -4.5(7) . . . . ?
Fe1 N9 C10 C11 -174.6(6) . . . . ?
Fe1 N14 C15 C16 169.1(5) . . . . ?
Fe1 N22 C23 C24 -178.1(5) . . . . ?
Fe1 N22 C23 N28 1.0(8) . . . . ?
Fe1 N22 C27 C26 177.3(5) . . . . ?
Fe1 N22 C27 N33 -2.2(8) . . . . ?
Fe1 N29 C30 C31 -177.1(6) . . . . ?
Fe1 N34 C35 C36 170.2(6) . . . . ?
N2 C3 C4 C5 1.6(10) . . . . ?
N2 C3 N8 N9 -1.2(8) . . . . ?
N2 C3 N8 C12 -178.5(7) . . . . ?
N2 C7 N13 N14 1.1(7) . . . . ?
N2 C7 N13 C17 175.8(6) . . . . ?
C3 N2 C7 C6 1.5(9) . . . . ?
C3 N2 C7 N13 -176.1(5) . . . . ?
C3 C4 C5 C6 0.7(9) . . . . ?
C3 C4 C5 N18 177.9(6) . . . . ?
C3 N8 N9 Fe1 -1.7(6) . . . . ?
C3 N8 N9 C10 -178.1(5) . . . . ?
C3 N8 C12 C11 177.8(7) . . . . ?
C4 C3 N8 N9 177.0(6) . . . . ?
C4 C3 N8 C12 -0.3(11) . . . . ?
C4 C5 C6 C7 -1.8(9) . . . . ?
C4 C5 N18 C19 176.7(7) . . . . ?
C5 C6 C7 N2 0.7(9) . . . . ?
C5 C6 C7 N13 177.8(6) . . . . ?
C5 N18 C19 O20 -4.3(13) . . . . ?
C5 N18 C19 C21 174.6(6) . . . . ?
C6 C5 N18 C19 -6.2(11) . . . . ?
C6 C7 N13 N14 -176.3(6) . . . . ?
C6 C7 N13 C17 -1.6(11) . . . . ?
C7 N2 C3 C4 -2.7(9) . . . . ?
C7 N2 C3 N8 175.5(5) . . . . ?
C7 N13 N14 Fe1 2.5(7) . . . . ?
C7 N13 N14 C15 175.2(5) . . . . ?
C7 N13 C17 C16 -173.4(7) . . . . ?
N8 C3 C4 C5 -176.4(6) . . . . ?
N8 N9 C10 C11 -0.1(7) . . . . ?
N9 Fe1 N22 C23 -91.1(5) . . . . ?
N9 Fe1 N22 C27 94.4(5) . . . . ?
N9 N8 C12 C11 0.4(8) . . . . ?
N9 C10 C11 C12 0.3(8) . . . . ?
C10 C11 C12 N8 -0.4(8) . . . . ?
C12 N8 N9 Fe1 176.1(4) . . . . ?
C12 N8 N9 C10 -0.2(7) . . . . ?
N13 N14 C15 C16 -0.6(7) . . . . ?
N14 Fe1 N22 C23 90.4(5) . . . . ?
N14 Fe1 N22 C27 -84.1(5) . . . . ?
N14 N13 C17 C16 1.5(7) . . . . ?
N14 C15 C16 C17 1.6(8) . . . . ?
C15 C16 C17 N13 -1.8(8) . . . . ?
C17 N13 N14 Fe1 -173.4(4) . . . . ?
C17 N13 N14 C15 -0.6(7) . . . . ?
N18 C5 C6 C7 -178.8(6) . . . . ?
N22 C23 C24 C25 1.4(10) . . . . ?
N22 C23 N28 N29 -0.2(8) . . . . ?
N22 C23 N28 C32 -178.6(7) . . . . ?
N22 C27 N33 N34 -1.6(8) . . . . ?
N22 C27 N33 C37 177.0(7) . . . . ?
C23 N22 C27 C26 2.7(10) . . . . ?
C23 N22 C27 N33 -176.8(6) . . . . ?
C23 C24 C25 C26 1.7(10) . . . . ?
C23 C24 C25 N38 -179.1(6) . . . . ?
C23 N28 N29 Fe1 -0.7(7) . . . . ?
C23 N28 N29 C30 -179.4(6) . . . . ?
C23 N28 C32 C31 178.6(7) . . . . ?
C24 C23 N28 N29 179.0(6) . . . . ?
C24 C23 N28 C32 0.6(12) . . . . ?
C24 C25 C26 C27 -2.4(10) . . . . ?
C24 C25 N38 C39 21.5(11) . . . . ?
C25 C26 C27 N22 0.2(10) . . . . ?
C25 C26 C27 N33 179.6(6) . . . . ?
C25 N38 C39 O40 -1.2(12) . . . . ?
C25 N38 C39 C41 175.1(7) . . . . ?
C26 C25 N38 C39 -159.3(7) . . . . ?
C26 C27 N33 N34 178.9(6) . . . . ?
C26 C27 N33 C37 -2.5(12) . . . . ?
C27 N22 C23 C24 -3.5(10) . . . . ?
C27 N22 C23 N28 175.7(6) . . . . ?
C27 N33 N34 Fe1 4.4(7) . . . . ?
C27 N33 N34 C35 178.2(6) . . . . ?
C27 N33 C37 C36 -177.0(7) . . . . ?
N28 C23 C24 C25 -177.7(6) . . . . ?
N28 N29 C30 C31 0.9(7) . . . . ?
N29 Fe1 N22 C23 -1.1(5) . . . . ?
N29 Fe1 N22 C27 -175.6(6) . . . . ?
N29 N28 C32 C31 0.1(8) . . . . ?
N29 C30 C31 C32 -0.8(8) . . . . ?
C30 C31 C32 N28 0.4(8) . . . . ?
C32 N28 N29 Fe1 178.1(4) . . . . ?
C32 N28 N29 C30 -0.6(7) . . . . ?
N33 N34 C35 C36 -0.5(8) . . . . ?
N34 Fe1 N22 C23 178.2(6) . . . . ?
N34 Fe1 N22 C27 3.7(5) . . . . ?
N34 N33 C37 C36 1.7(8) . . . . ?
N34 C35 C36 C37 1.5(8) . . . . ?
C35 C36 C37 N33 -1.9(8) . . . . ?
C37 N33 N34 Fe1 -174.5(5) . . . . ?
C37 N33 N34 C35 -0.7(8) . . . . ?
N38 C25 C26 C27 178.3(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.567(4)
2 0.433(4)

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile/diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_80clalt
_database_code_depnum_ccdc_archive 'CCDC 2078651'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2021-04-19 deposited with the CCDC.	2021-06-10 downloaded from the CCDC.
;
_audit_creation_date             2020-07-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis-[N-(2,6-di{pyrazol-1-yl}pyrid-4-yl)acetamide]iron(II)diperchlorate acetonitrile solvate'
_chemical_formula_moiety         'C26 H24 Fe N12 O2, 2(Cl O4), C2 H3 N'
_chemical_formula_sum            'C28 H27 Cl2 Fe N13 O10'
_chemical_formula_weight         832.37
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.3202(8)
_cell_length_b                   12.3819(8)
_cell_length_c                   17.5192(9)
_cell_angle_alpha                81.925(5)
_cell_angle_beta                 78.760(6)
_cell_angle_gamma                85.352(6)
_cell_volume                     1750.0(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5377
_cell_measurement_temperature    160(2)
_cell_measurement_theta_min      4.15
_cell_measurement_theta_max      73.53
_exptl_absorpt_coefficient_mu    5.521
_exptl_absorpt_correction_T_min  0.633
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 0.943
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13173
_diffrn_reflns_point_group_measured_fraction_full 0.943
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.867
_diffrn_reflns_theta_min         3.611
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5614
_reflns_number_total             6578
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2015)'
_refine_diff_density_max         0.968
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.119
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         6578
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0875
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1255P)²+5.8633P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2520
_refine_ls_wR_factor_ref         0.2599
_refine_special_details          
;
 The data were resolved into two non-superimposable twin domains, in a 
 ratio of 0.80:0.20.

 One ClO₄⁻ ion and the acetonitrile molecule are both disordered over 
 two half-occupied orientations. The bond distance restraints that were 
 applied to the disordered residues are listed below.

 All crystallographically ordered non-H atoms were refined anisotropically,
 and H atoms were placed in calculated positions and refined using a 
 riding model.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl2A-O43A = Cl2A-O44A = Cl2A-O45A = Cl2A-O46A
 1.44134 with sigma of 0.02
 Cl2B-O43B = Cl2B-O44B = Cl2B-O45B = Cl2B-O46B
 1.44134 with sigma of 0.02
 O43A-O44A = O43A-O45A = O43A-O46A = O44A-O45A = O44A-O46A = O45A-O46A
 2.353708 with sigma of 0.02
 O43B-O44B = O43B-O45B = O43B-O46B = O44B-O45B = O44B-O46B = O45B-O46B
 2.353708 with sigma of 0.02
 C52A-C53A = C52B-C53B
 1.48 with sigma of 0.02
 C53A-N54A = C53B-N54B
 1.15 with sigma of 0.02
 C52A-N54A = C52B-N54B
 2.63 with sigma of 0.02
3. Others
 1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: Cl2A(0.5) O43A(0.5) O44A(0.5) O45A(0.5) O46A(0.5) Cl2B(0.5)
 O43B(0.5) O44B(0.5) O45B(0.5) O46B(0.5) C52A(0.5) H52A(0.5) H52B(0.5)
 H52C(0.5) C53A(0.5) N54A(0.5) C52B(0.5) H52D(0.5) H52E(0.5) H52F(0.5)
 C53B(0.5) N54B(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17),
 N18(H18), C24(H24), C26(H26), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36),
  C37(H37), N38(H38)
4.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C41(H41A,H41B,H41C), C52A(H52A,H52B,H52C), C52B(H52D,
 H52E,H52F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.76091(11) 0.26287(7) 0.73263(5) 0.0339(3) Uani 1 1 d . . . . .
N2 N 0.8106(6) 0.1301(4) 0.6854(3) 0.0347(10) Uani 1 1 d . . . . .
C3 C 0.7860(7) 0.1263(5) 0.6129(3) 0.0351(11) Uani 1 1 d . . . . .
C4 C 0.8056(7) 0.0318(5) 0.5784(3) 0.0379(12) Uani 1 1 d . . . . .
H4 H 0.788747 0.031799 0.526340 0.046 Uiso 1 1 calc R U . . .
C5 C 0.8514(7) -0.0644(5) 0.6231(3) 0.0388(12) Uani 1 1 d . . . . .
C6 C 0.8730(8) -0.0627(5) 0.7011(3) 0.0407(13) Uani 1 1 d . . . . .
H6 H 0.901511 -0.127135 0.733116 0.049 Uiso 1 1 calc R U . . .
C7 C 0.8503(7) 0.0373(5) 0.7275(3) 0.0378(12) Uani 1 1 d . . . . .
N8 N 0.7339(6) 0.2291(4) 0.5791(3) 0.0371(10) Uani 1 1 d . . . . .
N9 N 0.7115(6) 0.3139(4) 0.6246(3) 0.0387(10) Uani 1 1 d . . . . .
C10 C 0.6575(8) 0.3985(5) 0.5820(4) 0.0441(13) Uani 1 1 d . . . . .
H10 H 0.632581 0.468857 0.598427 0.053 Uiso 1 1 calc R U . . .
C11 C 0.6408(9) 0.3723(5) 0.5086(4) 0.0511(16) Uani 1 1 d . . . . .
H11 H 0.603660 0.419900 0.467318 0.061 Uiso 1 1 calc R U . . .
C12 C 0.6891(8) 0.2638(5) 0.5088(4) 0.0447(14) Uani 1 1 d . . . . .
H12 H 0.690998 0.221068 0.467588 0.054 Uiso 1 1 calc R U . . .
N13 N 0.8626(6) 0.0575(4) 0.8039(3) 0.0395(11) Uani 1 1 d . . . . .
N14 N 0.8269(6) 0.1631(4) 0.8201(3) 0.0364(10) Uani 1 1 d . . . . .
C15 C 0.8357(8) 0.1597(6) 0.8955(3) 0.0466(15) Uani 1 1 d . . . . .
H15 H 0.818642 0.221367 0.923394 0.056 Uiso 1 1 calc R U . . .
C16 C 0.8730(9) 0.0550(6) 0.9274(4) 0.0506(15) Uani 1 1 d . . . . .
H16 H 0.884140 0.031920 0.980222 0.061 Uiso 1 1 calc R U . . .
C17 C 0.8911(9) -0.0100(5) 0.8686(4) 0.0478(15) Uani 1 1 d . . . . .
H17 H 0.918022 -0.086408 0.872383 0.057 Uiso 1 1 calc R U . . .
N18 N 0.8656(7) -0.1586(4) 0.5873(3) 0.0451(12) Uani 1 1 d . . . . .
H18 H 0.838827 -0.151036 0.540559 0.054 Uiso 1 1 calc R U . . .
C19 C 0.9162(10) -0.2622(5) 0.6157(4) 0.0523(16) Uani 1 1 d . . . . .
O20 O 0.9655(9) -0.2841(4) 0.6772(3) 0.0706(16) Uani 1 1 d . . . . .
C21 C 0.9043(10) -0.3465(5) 0.5628(5) 0.0584(18) Uani 1 1 d . . . . .
H21A H 0.790747 -0.368118 0.571611 0.088 Uiso 1 1 calc R U . . .
H21B H 0.976498 -0.410630 0.574677 0.088 Uiso 1 1 calc R U . . .
H21C H 0.937781 -0.315326 0.507935 0.088 Uiso 1 1 calc R U . . .
N22 N 0.6973(6) 0.3874(4) 0.7880(3) 0.0378(10) Uani 1 1 d . . . . .
C23 C 0.8047(7) 0.4608(4) 0.7894(3) 0.0376(12) Uani 1 1 d . . . . .
C24 C 0.7682(8) 0.5502(5) 0.8300(4) 0.0426(13) Uani 1 1 d . . . . .
H24 H 0.846901 0.602155 0.828889 0.051 Uiso 1 1 calc R U . . .
C25 C 0.6083(8) 0.5597(5) 0.8730(3) 0.0436(14) Uani 1 1 d . . . . .
C26 C 0.4949(8) 0.4807(5) 0.8750(4) 0.0436(13) Uani 1 1 d . . . . .
H26 H 0.387496 0.485104 0.905582 0.052 Uiso 1 1 calc R U . . .
C27 C 0.5463(8) 0.3970(5) 0.8309(3) 0.0410(13) Uani 1 1 d . . . . .
N28 N 0.9577(6) 0.4329(4) 0.7455(3) 0.0414(11) Uani 1 1 d . . . . .
N29 N 0.9718(6) 0.3385(4) 0.7093(3) 0.0383(10) Uani 1 1 d . . . . .
C30 C 1.1247(8) 0.3319(5) 0.6724(4) 0.0435(13) Uani 1 1 d . . . . .
H30 H 1.170307 0.275234 0.641995 0.052 Uiso 1 1 calc R U . . .
C31 C 1.2122(9) 0.4183(5) 0.6832(4) 0.0503(15) Uani 1 1 d . . . . .
H31 H 1.324415 0.430715 0.662483 0.060 Uiso 1 1 calc R U . . .
C32 C 1.1037(8) 0.4812(5) 0.7296(4) 0.0432(13) Uani 1 1 d . . . . .
H32 H 1.125937 0.546492 0.747503 0.052 Uiso 1 1 calc R U . . .
N33 N 0.4526(6) 0.3094(4) 0.8252(3) 0.0439(11) Uani 1 1 d . . . . .
N34 N 0.5285(6) 0.2333(4) 0.7784(3) 0.0400(11) Uani 1 1 d . . . . .
C35 C 0.4194(8) 0.1582(6) 0.7842(4) 0.0486(15) Uani 1 1 d . . . . .
H35 H 0.437315 0.095422 0.757353 0.058 Uiso 1 1 calc R U . . .
C36 C 0.2769(9) 0.1842(6) 0.8344(4) 0.0553(17) Uani 1 1 d . . . . .
H36 H 0.181502 0.143178 0.848670 0.066 Uiso 1 1 calc R U . . .
C37 C 0.2986(9) 0.2798(6) 0.8598(4) 0.0535(16) Uani 1 1 d . . . . .
H37 H 0.221233 0.318627 0.894906 0.064 Uiso 1 1 calc R U . . .
N38 N 0.5530(7) 0.6457(4) 0.9167(3) 0.0491(13) Uani 1 1 d . . . . .
H38 H 0.468157 0.634407 0.955072 0.059 Uiso 1 1 calc R U . . .
C39 C 0.6186(9) 0.7463(5) 0.9055(4) 0.0511(16) Uani 1 1 d . . . . .
O40 O 0.7397(7) 0.7709(4) 0.8554(3) 0.0621(13) Uani 1 1 d . . . . .
C41 C 0.5283(12) 0.8240(7) 0.9601(5) 0.074(2) Uani 1 1 d . . . . .
H41A H 0.603071 0.878167 0.966111 0.111 Uiso 1 1 calc R U . . .
H41B H 0.487635 0.783134 1.011444 0.111 Uiso 1 1 calc R U . . .
H41C H 0.435618 0.861221 0.938380 0.111 Uiso 1 1 calc R U . . .
Cl4A Cl 0.7067(5) -0.0566(4) 0.3857(3) 0.0425(14) Uiso 0.5 1 d D . P A 1
O43A O 0.6490(13) 0.0473(7) 0.4154(6) 0.058(2) Uiso 0.5 1 d D . P A 1
O44A O 0.5725(11) -0.1216(8) 0.3942(6) 0.056(2) Uiso 0.5 1 d D . P A 1
O45A O 0.7710(13) -0.0259(9) 0.2994(5) 0.043(2) Uiso 0.5 1 d D . P A 1
O46A O 0.8359(11) -0.1070(7) 0.4210(5) 0.0389(19) Uiso 0.5 1 d D . P A 1
Cl4B Cl 0.7140(5) -0.0371(4) 0.3775(3) 0.0408(13) Uiso 0.5 1 d D . P B 2
O43B O 0.7397(13) 0.0631(7) 0.4019(6) 0.054(2) Uiso 0.5 1 d D . P B 2
O44B O 0.5455(12) -0.0544(11) 0.3848(7) 0.078(3) Uiso 0.5 1 d D . P B 2
O45B O 0.8033(14) -0.0552(10) 0.3021(5) 0.054(3) Uiso 0.5 1 d D . P B 2
O46B O 0.7776(17) -0.1273(9) 0.4339(7) 0.076(4) Uiso 0.5 1 d D . P B 2
Cl47 Cl 0.0947(2) 0.66652(14) 0.95148(10) 0.0555(4) Uani 1 1 d . . . . .
O48 O 0.1329(7) 0.6156(5) 0.8816(3) 0.0718(16) Uani 1 1 d . . . . .
O49 O -0.0661(8) 0.6439(7) 0.9908(4) 0.096(2) Uani 1 1 d . . . . .
O50 O 0.1079(11) 0.7796(5) 0.9327(4) 0.100(3) Uani 1 1 d . . . . .
O51 O 0.2124(6) 0.6262(4) 1.0015(3) 0.0549(12) Uani 1 1 d . . . . .
C52A C 0.563(2) 0.2119(12) 0.2573(10) 0.063(4) Uiso 0.5 1 d D . P C 1
H52A H 0.564778 0.145633 0.295027 0.095 Uiso 0.5 1 calc R U P C 1
H52B H 0.669740 0.217317 0.221920 0.095 Uiso 0.5 1 calc R U P C 1
H52C H 0.477100 0.208621 0.226658 0.095 Uiso 0.5 1 calc R U P C 1
C53A C 0.529(3) 0.3079(13) 0.2995(11) 0.052(6) Uiso 0.5 1 d D . P C 1
N54A N 0.504(3) 0.3788(14) 0.3354(12) 0.063(6) Uiso 0.5 1 d D . P C 1
C52B C 0.643(2) 0.2206(13) 0.2554(10) 0.065(4) Uiso 0.5 1 d D . P D 2
H52D H 0.656164 0.240906 0.198535 0.097 Uiso 0.5 1 calc R U P D 2
H52E H 0.573006 0.158495 0.271612 0.097 Uiso 0.5 1 calc R U P D 2
H52F H 0.751038 0.200350 0.269439 0.097 Uiso 0.5 1 calc R U P D 2
C53B C 0.568(3) 0.3130(14) 0.2951(12) 0.054(6) Uiso 0.5 1 d D . P D 2
N54B N 0.502(3) 0.3911(16) 0.3189(14) 0.079(8) Uiso 0.5 1 d D . P D 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.922(4) . ?
Fe1 N9 2.019(5) . ?
Fe1 N14 1.965(5) . ?
Fe1 N22 1.921(5) . ?
Fe1 N29 2.001(5) . ?
Fe1 N34 1.986(5) . ?
N2 C3 1.333(7) . ?
N2 C7 1.330(7) . ?
C3 C4 1.375(8) . ?
C3 N8 1.399(7) . ?
C4 H4 0.9500 . ?
C4 C5 1.399(8) . ?
C5 C6 1.415(8) . ?
C5 N18 1.387(7) . ?
C6 H6 0.9500 . ?
C6 C7 1.369(8) . ?
C7 N13 1.420(7) . ?
N8 N9 1.384(6) . ?
N8 C12 1.360(8) . ?
N9 C10 1.300(8) . ?
C10 H10 0.9500 . ?
C10 C11 1.406(9) . ?
C11 H11 0.9500 . ?
C11 C12 1.370(9) . ?
C12 H12 0.9500 . ?
N13 N14 1.373(7) . ?
N13 C17 1.359(8) . ?
N14 C15 1.331(7) . ?
C15 H15 0.9500 . ?
C15 C16 1.375(10) . ?
C16 H16 0.9500 . ?
C16 C17 1.372(9) . ?
C17 H17 0.9500 . ?
N18 H18 0.8800 . ?
N18 C19 1.373(8) . ?
C19 O20 1.214(9) . ?
C19 C21 1.511(10) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
N22 C23 1.330(8) . ?
N22 C27 1.338(8) . ?
C23 C24 1.381(8) . ?
C23 N28 1.398(8) . ?
C24 H24 0.9500 . ?
C24 C25 1.399(9) . ?
C25 C26 1.406(9) . ?
C25 N38 1.394(8) . ?
C26 H26 0.9500 . ?
C26 C27 1.370(8) . ?
C27 N33 1.411(8) . ?
N28 N29 1.391(7) . ?
N28 C32 1.361(8) . ?
N29 C30 1.312(8) . ?
C30 H30 0.9500 . ?
C30 C31 1.395(10) . ?
C31 H31 0.9500 . ?
C31 C32 1.365(9) . ?
C32 H32 0.9500 . ?
N33 N34 1.370(7) . ?
N33 C37 1.361(9) . ?
N34 C35 1.332(8) . ?
C35 H35 0.9500 . ?
C35 C36 1.377(10) . ?
C36 H36 0.9500 . ?
C36 C37 1.358(10) . ?
C37 H37 0.9500 . ?
N38 H38 0.8800 . ?
N38 C39 1.374(9) . ?
C39 O40 1.228(9) . ?
C39 C41 1.506(9) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
Cl4A O43A 1.466(9) . ?
Cl4A O44A 1.401(9) . ?
Cl4A O45A 1.507(9) . ?
Cl4A O46A 1.404(8) . ?
Cl4B O43B 1.413(9) . ?
Cl4B O44B 1.414(10) . ?
Cl4B O45B 1.421(9) . ?
Cl4B O46B 1.517(10) . ?
Cl47 O48 1.425(5) . ?
Cl47 O49 1.411(7) . ?
Cl47 O50 1.401(7) . ?
Cl47 O51 1.452(5) . ?
C52A H52A 0.9800 . ?
C52A H52B 0.9800 . ?
C52A H52C 0.9800 . ?
C52A C53A 1.467(14) . ?
C53A N54A 1.132(14) . ?
C52B H52D 0.9800 . ?
C52B H52E 0.9800 . ?
C52B H52F 0.9800 . ?
C52B C53B 1.457(14) . ?
C53B N54B 1.160(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N9 79.44(19) . . ?
N2 Fe1 N14 79.32(19) . . ?
N2 Fe1 N29 105.2(2) . . ?
N2 Fe1 N34 95.7(2) . . ?
N14 Fe1 N9 158.8(2) . . ?
N14 Fe1 N29 92.9(2) . . ?
N14 Fe1 N34 88.7(2) . . ?
N22 Fe1 N2 174.4(2) . . ?
N22 Fe1 N9 103.9(2) . . ?
N22 Fe1 N14 97.3(2) . . ?
N22 Fe1 N29 79.3(2) . . ?
N22 Fe1 N34 79.6(2) . . ?
N29 Fe1 N9 92.8(2) . . ?
N34 Fe1 N9 93.2(2) . . ?
N34 Fe1 N29 158.9(2) . . ?
C3 N2 Fe1 120.5(4) . . ?
C7 N2 Fe1 120.6(4) . . ?
C7 N2 C3 118.4(5) . . ?
N2 C3 C4 123.2(5) . . ?
N2 C3 N8 111.0(5) . . ?
C4 C3 N8 125.7(5) . . ?
C3 C4 H4 121.3 . . ?
C3 C4 C5 117.3(5) . . ?
C5 C4 H4 121.3 . . ?
C4 C5 C6 120.3(5) . . ?
N18 C5 C4 115.7(5) . . ?
N18 C5 C6 123.9(5) . . ?
C5 C6 H6 122.0 . . ?
C7 C6 C5 115.9(5) . . ?
C7 C6 H6 122.0 . . ?
N2 C7 C6 124.7(5) . . ?
N2 C7 N13 109.9(5) . . ?
C6 C7 N13 125.4(5) . . ?
N9 N8 C3 117.7(4) . . ?
C12 N8 C3 132.1(5) . . ?
C12 N8 N9 110.1(5) . . ?
N8 N9 Fe1 111.3(3) . . ?
C10 N9 Fe1 142.4(4) . . ?
C10 N9 N8 106.1(5) . . ?
N9 C10 H10 124.4 . . ?
N9 C10 C11 111.2(6) . . ?
C11 C10 H10 124.4 . . ?
C10 C11 H11 127.1 . . ?
C12 C11 C10 105.7(6) . . ?
C12 C11 H11 127.1 . . ?
N8 C12 C11 106.9(5) . . ?
N8 C12 H12 126.5 . . ?
C11 C12 H12 126.5 . . ?
N14 N13 C7 116.3(5) . . ?
C17 N13 C7 132.2(5) . . ?
C17 N13 N14 111.2(5) . . ?
N13 N14 Fe1 113.6(3) . . ?
C15 N14 Fe1 140.9(4) . . ?
C15 N14 N13 105.1(5) . . ?
N14 C15 H15 124.6 . . ?
N14 C15 C16 110.8(6) . . ?
C16 C15 H15 124.6 . . ?
C15 C16 H16 126.4 . . ?
C17 C16 C15 107.2(6) . . ?
C17 C16 H16 126.4 . . ?
N13 C17 C16 105.7(6) . . ?
N13 C17 H17 127.2 . . ?
C16 C17 H17 127.2 . . ?
C5 N18 H18 116.0 . . ?
C19 N18 C5 128.0(6) . . ?
C19 N18 H18 116.0 . . ?
N18 C19 C21 113.2(6) . . ?
O20 C19 N18 123.5(6) . . ?
O20 C19 C21 123.2(6) . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 N22 Fe1 121.1(4) . . ?
C23 N22 C27 118.9(5) . . ?
C27 N22 Fe1 119.8(4) . . ?
N22 C23 C24 124.0(6) . . ?
N22 C23 N28 110.3(5) . . ?
C24 C23 N28 125.7(6) . . ?
C23 C24 H24 122.0 . . ?
C23 C24 C25 116.0(6) . . ?
C25 C24 H24 122.0 . . ?
C24 C25 C26 121.0(6) . . ?
N38 C25 C24 122.7(6) . . ?
N38 C25 C26 116.3(6) . . ?
C25 C26 H26 121.5 . . ?
C27 C26 C25 117.0(6) . . ?
C27 C26 H26 121.5 . . ?
N22 C27 C26 123.1(6) . . ?
N22 C27 N33 110.9(5) . . ?
C26 C27 N33 126.0(6) . . ?
N29 N28 C23 117.5(5) . . ?
C32 N28 C23 132.2(5) . . ?
C32 N28 N29 110.2(5) . . ?
N28 N29 Fe1 111.7(4) . . ?
C30 N29 Fe1 143.2(4) . . ?
C30 N29 N28 105.1(5) . . ?
N29 C30 H30 124.2 . . ?
N29 C30 C31 111.7(6) . . ?
C31 C30 H30 124.2 . . ?
C30 C31 H31 127.0 . . ?
C32 C31 C30 106.0(6) . . ?
C32 C31 H31 127.0 . . ?
N28 C32 C31 107.0(6) . . ?
N28 C32 H32 126.5 . . ?
C31 C32 H32 126.5 . . ?
N34 N33 C27 116.6(5) . . ?
C37 N33 C27 133.2(6) . . ?
C37 N33 N34 110.1(5) . . ?
N33 N34 Fe1 112.9(4) . . ?
C35 N34 Fe1 141.1(5) . . ?
C35 N34 N33 105.7(5) . . ?
N34 C35 H35 124.8 . . ?
N34 C35 C36 110.4(6) . . ?
C36 C35 H35 124.8 . . ?
C35 C36 H36 126.5 . . ?
C37 C36 C35 106.9(6) . . ?
C37 C36 H36 126.5 . . ?
N33 C37 H37 126.6 . . ?
C36 C37 N33 106.8(6) . . ?
C36 C37 H37 126.6 . . ?
C25 N38 H38 117.0 . . ?
C39 N38 C25 126.1(6) . . ?
C39 N38 H38 117.0 . . ?
N38 C39 C41 113.9(7) . . ?
O40 C39 N38 123.1(6) . . ?
O40 C39 C41 122.9(7) . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O43A Cl4A O45A 104.8(6) . . ?
O44A Cl4A O43A 108.9(6) . . ?
O44A Cl4A O45A 108.6(6) . . ?
O44A Cl4A O46A 114.2(6) . . ?
O46A Cl4A O43A 111.2(6) . . ?
O46A Cl4A O45A 108.7(6) . . ?
O43B Cl4B O44B 112.3(7) . . ?
O43B Cl4B O45B 115.0(7) . . ?
O43B Cl4B O46B 107.0(7) . . ?
O44B Cl4B O45B 111.5(7) . . ?
O44B Cl4B O46B 105.2(8) . . ?
O45B Cl4B O46B 104.9(7) . . ?
O48 Cl47 O51 109.2(3) . . ?
O49 Cl47 O48 109.8(4) . . ?
O49 Cl47 O51 110.4(4) . . ?
O50 Cl47 O48 109.7(4) . . ?
O50 Cl47 O49 109.8(5) . . ?
O50 Cl47 O51 107.8(4) . . ?
H52A C52A H52B 109.5 . . ?
H52A C52A H52C 109.5 . . ?
H52B C52A H52C 109.5 . . ?
C53A C52A H52A 109.5 . . ?
C53A C52A H52B 109.5 . . ?
C53A C52A H52C 109.5 . . ?
N54A C53A C52A 177(2) . . ?
H52D C52B H52E 109.5 . . ?
H52D C52B H52F 109.5 . . ?
H52E C52B H52F 109.5 . . ?
C53B C52B H52D 109.5 . . ?
C53B C52B H52E 109.5 . . ?
C53B C52B H52F 109.5 . . ?
N54B C53B C52B 172(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N18 H18 O46A 0.88 2.09 2.947(9) 163.4 . yes
N18 H18 O46B 0.88 2.01 2.888(12) 177.7 . yes
N38 H38 O51 0.88 2.13 2.943(8) 153.4 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N2 C3 C4 -174.2(4) . . . . ?
Fe1 N2 C3 N8 4.0(7) . . . . ?
Fe1 N2 C7 C6 173.8(5) . . . . ?
Fe1 N2 C7 N13 -5.2(7) . . . . ?
Fe1 N9 C10 C11 -174.8(5) . . . . ?
Fe1 N14 C15 C16 170.9(5) . . . . ?
Fe1 N22 C23 C24 -177.9(4) . . . . ?
Fe1 N22 C23 N28 1.0(6) . . . . ?
Fe1 N22 C27 C26 176.7(5) . . . . ?
Fe1 N22 C27 N33 -2.2(6) . . . . ?
Fe1 N29 C30 C31 -178.4(5) . . . . ?
Fe1 N34 C35 C36 172.8(5) . . . . ?
N2 C3 C4 C5 0.9(9) . . . . ?
N2 C3 N8 N9 -2.1(7) . . . . ?
N2 C3 N8 C12 -177.4(6) . . . . ?
N2 C7 N13 N14 2.2(7) . . . . ?
N2 C7 N13 C17 176.1(6) . . . . ?
C3 N2 C7 C6 2.0(9) . . . . ?
C3 N2 C7 N13 -176.9(5) . . . . ?
C3 C4 C5 C6 1.1(9) . . . . ?
C3 C4 C5 N18 178.3(5) . . . . ?
C3 N8 N9 Fe1 -0.5(6) . . . . ?
C3 N8 N9 C10 -177.5(5) . . . . ?
C3 N8 C12 C11 176.8(6) . . . . ?
C4 C3 N8 N9 176.1(5) . . . . ?
C4 C3 N8 C12 0.7(11) . . . . ?
C4 C5 C6 C7 -1.5(9) . . . . ?
C4 C5 N18 C19 176.4(6) . . . . ?
C5 C6 C7 N2 -0.1(9) . . . . ?
C5 C6 C7 N13 178.7(6) . . . . ?
C5 N18 C19 O20 -4.2(12) . . . . ?
C5 N18 C19 C21 175.7(6) . . . . ?
C6 C5 N18 C19 -6.6(11) . . . . ?
C6 C7 N13 N14 -176.7(5) . . . . ?
C6 C7 N13 C17 -2.8(11) . . . . ?
C7 N2 C3 C4 -2.5(9) . . . . ?
C7 N2 C3 N8 175.7(5) . . . . ?
C7 N13 N14 Fe1 1.4(6) . . . . ?
C7 N13 N14 C15 175.9(5) . . . . ?
C7 N13 C17 C16 -174.2(6) . . . . ?
N8 C3 C4 C5 -177.0(6) . . . . ?
N8 N9 C10 C11 0.8(7) . . . . ?
N9 N8 C12 C11 1.2(7) . . . . ?
N9 C10 C11 C12 0.0(8) . . . . ?
C10 C11 C12 N8 -0.7(8) . . . . ?
C12 N8 N9 Fe1 175.8(4) . . . . ?
C12 N8 N9 C10 -1.2(7) . . . . ?
N13 N14 C15 C16 -1.1(7) . . . . ?
N14 N13 C17 C16 -0.1(7) . . . . ?
N14 C15 C16 C17 1.1(8) . . . . ?
C15 C16 C17 N13 -0.6(8) . . . . ?
C17 N13 N14 Fe1 -173.8(4) . . . . ?
C17 N13 N14 C15 0.7(7) . . . . ?
N18 C5 C6 C7 -178.4(6) . . . . ?
N22 C23 C24 C25 1.5(9) . . . . ?
N22 C23 N28 N29 0.3(7) . . . . ?
N22 C23 N28 C32 -179.9(6) . . . . ?
N22 C27 N33 N34 -0.3(7) . . . . ?
N22 C27 N33 C37 176.4(6) . . . . ?
C23 N22 C27 C26 1.7(9) . . . . ?
C23 N22 C27 N33 -177.2(5) . . . . ?
C23 C24 C25 C26 1.3(9) . . . . ?
C23 C24 C25 N38 -179.7(6) . . . . ?
C23 N28 N29 Fe1 -1.2(6) . . . . ?
C23 N28 N29 C30 179.7(5) . . . . ?
C23 N28 C32 C31 -179.8(6) . . . . ?
C24 C23 N28 N29 179.1(5) . . . . ?
C24 C23 N28 C32 -1.1(10) . . . . ?
C24 C25 C26 C27 -2.4(9) . . . . ?
C24 C25 N38 C39 22.4(10) . . . . ?
C25 C26 C27 N22 0.9(9) . . . . ?
C25 C26 C27 N33 179.6(6) . . . . ?
C25 N38 C39 O40 -2.1(12) . . . . ?
C25 N38 C39 C41 177.8(7) . . . . ?
C26 C25 N38 C39 -158.5(7) . . . . ?
C26 C27 N33 N34 -179.2(6) . . . . ?
C26 C27 N33 C37 -2.4(11) . . . . ?
C27 N22 C23 C24 -3.0(8) . . . . ?
C27 N22 C23 N28 175.9(5) . . . . ?
C27 N33 N34 Fe1 2.5(6) . . . . ?
C27 N33 N34 C35 178.1(5) . . . . ?
C27 N33 C37 C36 -177.1(7) . . . . ?
N28 C23 C24 C25 -177.2(5) . . . . ?
N28 N29 C30 C31 0.3(7) . . . . ?
N29 N28 C32 C31 0.0(7) . . . . ?
N29 C30 C31 C32 -0.3(8) . . . . ?
C30 C31 C32 N28 0.1(7) . . . . ?
C32 N28 N29 Fe1 178.9(4) . . . . ?
C32 N28 N29 C30 -0.2(6) . . . . ?
N33 N34 C35 C36 -0.9(7) . . . . ?
N34 N33 C37 C36 -0.2(8) . . . . ?
N34 C35 C36 C37 0.8(8) . . . . ?
C35 C36 C37 N33 -0.4(8) . . . . ?
C37 N33 N34 Fe1 -175.0(4) . . . . ?
C37 N33 N34 C35 0.6(7) . . . . ?
N38 C25 C26 C27 178.6(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile/diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_80claht
_database_code_depnum_ccdc_archive 'CCDC 2078650'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2021-04-19 deposited with the CCDC.	2021-06-10 downloaded from the CCDC.
;
_audit_creation_date             2020-07-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis-[N-(2,6-di{pyrazol-1-yl}pyrid-4-yl)acetamide]iron(II)diperchlorate acetonitrile solvate'
_chemical_formula_moiety         'C26 H24 Fe N12 O2, 2(Cl O4), C2 H3 N'
_chemical_formula_sum            'C28 H27 Cl2 Fe N13 O10'
_chemical_formula_weight         832.37
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2794(3)
_cell_length_b                   12.6110(5)
_cell_length_c                   17.7349(8)
_cell_angle_alpha                82.848(4)
_cell_angle_beta                 79.767(3)
_cell_angle_gamma                80.613(3)
_cell_volume                     1789.15(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7480
_cell_measurement_temperature    200(2)
_cell_measurement_theta_min      4.13
_cell_measurement_theta_max      73.66
_exptl_absorpt_coefficient_mu    5.400
_exptl_absorpt_correction_T_min  0.719
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.948
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6760
_diffrn_reflns_point_group_measured_fraction_full 0.948
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.728
_diffrn_reflns_theta_min         3.570
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6254
_reflns_number_total             6760
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2015)'
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         6760
_refine_ls_number_restraints     74
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0594
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0590P)²+2.9811P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1523
_refine_ls_wR_factor_ref         0.1551
_refine_special_details          
;The data were resolved into two non-superimposable twin domains, in a 
 ratio of 0.76:0.24.

 The C atoms of one pyrazole ring in the complex cation were modelled as 
 disordered over two half-occupied sites, to resolve an intermolecular
 steric clash. Both ClO₄⁻ ions are also disordered over three equally 
 occupied sites; in one case, two of these sites share a common Cl atom. 
 The acetonitrile molecule is also disordered over two sites. The bond 
 distance restraints that were applied to the disordered residues are 
 listed below.

 All crystallographically ordered non-H atoms were refined anisotropically,
 and H atoms were placed in calculated positions and refined using a 
 riding model.,Twin
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.756(3)
 0.244(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N14-C15A = N14-C15B
 1.32 with sigma of 0.01
 C15A-C16A = C15B-C16B
 1.39 with sigma of 0.01
 C16A-C17A = C16B-C17B
 1.37 with sigma of 0.01
 N13-C17A = N13-C17B
 1.36 with sigma of 0.01
 Cl2A-O43A = Cl2A-O44A = Cl2A-O45A = Cl2A-O46A
 1.43685 with sigma of 0.02
 Cl2B-O43B = Cl2B-O44B = Cl2B-O45B = Cl2B-O46B
 1.43685 with sigma of 0.02
 Cl2C-O43C = Cl2C-O44C = Cl2C-O45C = Cl2C-O46C
 1.43685 with sigma of 0.02
 O43A-O44A = O43A-O45A = O43A-O46A = O44A-O45A = O44A-O46A = O45A-O46A
 2.346376 with sigma of 0.02
 O43B-O44B = O43B-O45B = O43B-O46B = O44B-O45B = O44B-O46B = O45B-O46B
 2.346376 with sigma of 0.02
 O43C-O44C = O43C-O45C = O43C-O46C = O44C-O45C = O44C-O46C = O45C-O46C
 2.346376 with sigma of 0.02
 Cl7A-O48A = Cl7A-O49A = Cl7A-O50A = Cl7A-O51A
 1.43685 with sigma of 0.02
 Cl7B-O48B = Cl7B-O49B = Cl7B-O50B = Cl7B-O51B
 1.43685 with sigma of 0.02
 Cl7B-O48C = Cl7B-O49C = Cl7B-O50C = Cl7B-O51C
 1.43685 with sigma of 0.02
 O48A-O49A = O48A-O50A = O48A-O51A = O49A-O50A = O49A-O51A = O50A-O51A
 2.346376 with sigma of 0.02
 O48B-O49B = O48B-O50B = O48B-O51B = O49B-O50B = O49B-O51B = O50B-O51B
 2.346376 with sigma of 0.02
 O48C-O49C = O48C-O50C = O48C-O51C = O49C-O50C = O49C-O51C = O50C-O51C
 2.346376 with sigma of 0.02
 C52A-C53A = C52B-C53B
 1.48 with sigma of 0.02
 C53A-N54A = C53B-N54B
 1.15 with sigma of 0.02
 C52A-N54A = C52B-N54B
 2.63 with sigma of 0.02
4. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: C15A(0.5) H15A(0.5) C16A(0.5) H16A(0.5) C17A(0.5) H17A(0.5)
 C15B(0.5) H15B(0.5) C16B(0.5) H16B(0.5) C17B(0.5) H17B(0.5) Cl2A(0.34)
 O43A(0.34) O44A(0.34) O45A(0.34) O46A(0.34) Cl2B(0.33) O43B(0.33) O44B(0.33)
 O45B(0.33) O46B(0.33) Cl2C(0.33) O43C(0.33) O44C(0.33) O45C(0.33) O46C(0.33)
 Cl7A(0.34) O48A(0.34) O49A(0.34) O50A(0.34) O51A(0.34) Cl7B(0.66) O48B(0.33)
 O49B(0.33) O50B(0.33) O51B(0.33) O48C(0.33) O49C(0.33) O50C(0.33) O51C(0.33)
 C52A(0.5) H52A(0.5) H52B(0.5) H52C(0.5) C53A(0.5) N54A(0.5) C52B(0.5)
 H52D(0.5) H52E(0.5) H52F(0.5) C53B(0.5) N54B(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C15A(H15A), C16A(H16A),
 C17A(H17A), C15B(H15B), C16B(H16B), C17B(H17B), N18(H18), C24(H24), C26(H26),
 C30(H30), C31(H31), C32(H32), C35(H35), C36(H36), C37(H37), N38(H38)
5.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C41(H41A,H41B,H41C), C52A(H52A,H52B,H52C), C52B(H52D,
 H52E,H52F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.78421(7) 0.26710(5) 0.72931(3) 0.03417(17) Uani 1 1 d . . . . .
N2 N 0.8161(3) 0.1198(2) 0.67897(15) 0.0279(6) Uani 1 1 d . . . . .
C3 C 0.7903(4) 0.1169(3) 0.60765(19) 0.0275(7) Uani 1 1 d . . . . .
C4 C 0.8081(4) 0.0245(3) 0.57212(19) 0.0311(7) Uani 1 1 d . . . . .
H4 H 0.790362 0.026692 0.520438 0.037 Uiso 1 1 calc R U . . .
C5 C 0.8534(5) -0.0734(3) 0.6150(2) 0.0336(7) Uani 1 1 d . . . . .
C6 C 0.8807(5) -0.0728(3) 0.6902(2) 0.0382(8) Uani 1 1 d . . . . .
H6 H 0.911116 -0.137953 0.720831 0.046 Uiso 1 1 calc R U . . .
C7 C 0.8617(4) 0.0257(3) 0.7182(2) 0.0329(7) Uani 1 1 d . . . . .
N8 N 0.7397(4) 0.2207(2) 0.57139(16) 0.0302(6) Uani 1 1 d . . . . .
N9 N 0.7264(4) 0.3078(2) 0.61223(17) 0.0345(6) Uani 1 1 d . . . . .
C10 C 0.6706(5) 0.3919(3) 0.5660(2) 0.0449(9) Uani 1 1 d . . . . .
H10 H 0.650164 0.464524 0.578396 0.054 Uiso 1 1 calc R U . . .
C11 C 0.6460(6) 0.3596(3) 0.4967(3) 0.0501(10) Uani 1 1 d . . . . .
H11 H 0.606681 0.404289 0.454591 0.060 Uiso 1 1 calc R U . . .
C12 C 0.6905(5) 0.2500(3) 0.5026(2) 0.0414(9) Uani 1 1 d . . . . .
H12 H 0.687223 0.203233 0.464996 0.050 Uiso 1 1 calc R U . . .
N13 N 0.8839(4) 0.0379(3) 0.79346(17) 0.0408(8) Uani 1 1 d D . . . .
N14 N 0.8574(4) 0.1396(3) 0.81643(17) 0.0424(8) Uani 1 1 d D . . . .
C15A C 0.8557(11) 0.1398(6) 0.8908(4) 0.0335(18) Uiso 0.5 1 d D . P A 1
H15A H 0.840302 0.200818 0.919191 0.040 Uiso 0.5 1 calc R U P A 1
C16A C 0.8817(11) 0.0296(6) 0.9194(4) 0.0386(17) Uiso 0.5 1 d D . P A 1
H16A H 0.890645 0.001636 0.970983 0.046 Uiso 0.5 1 calc R U P A 1
C17A C 0.8915(10) -0.0288(5) 0.8583(3) 0.0321(15) Uiso 0.5 1 d D . P A 1
H17A H 0.902188 -0.105344 0.861363 0.039 Uiso 0.5 1 calc R U P A 1
C15B C 0.9009(13) 0.1104(7) 0.8868(4) 0.047(2) Uiso 0.5 1 d D . P A 2
H15B H 0.892992 0.162151 0.922334 0.056 Uiso 0.5 1 calc R U P A 2
C16B C 0.9574(15) 0.0025(7) 0.9053(5) 0.061(3) Uiso 0.5 1 d D . P A 2
H16B H 0.990362 -0.030483 0.952358 0.074 Uiso 0.5 1 calc R U P A 2
C17B C 0.9554(12) -0.0462(6) 0.8410(5) 0.046(2) Uiso 0.5 1 d D . P A 2
H17B H 0.993266 -0.119234 0.831203 0.055 Uiso 0.5 1 calc R U P A 2
N18 N 0.8654(5) -0.1668(2) 0.5786(2) 0.0424(8) Uani 1 1 d . . . . .
H18 H 0.842830 -0.157259 0.531344 0.051 Uiso 1 1 calc R U . . .
C19 C 0.9082(6) -0.2717(3) 0.6074(3) 0.0509(10) Uani 1 1 d . . . . .
O20 O 0.9492(6) -0.2961(3) 0.6700(2) 0.0798(12) Uani 1 1 d . . . . .
C21 C 0.9008(7) -0.3532(3) 0.5535(3) 0.0624(13) Uani 1 1 d . . . . .
H21A H 0.784727 -0.356924 0.550739 0.094 Uiso 1 1 calc R U . . .
H21B H 0.954303 -0.424236 0.572404 0.094 Uiso 1 1 calc R U . . .
H21C H 0.958602 -0.331433 0.502073 0.094 Uiso 1 1 calc R U . . .
N22 N 0.7149(4) 0.3996(2) 0.79789(16) 0.0320(6) Uani 1 1 d . . . . .
C23 C 0.8173(4) 0.4701(3) 0.79793(19) 0.0313(7) Uani 1 1 d . . . . .
C24 C 0.7784(5) 0.5606(3) 0.8378(2) 0.0366(8) Uani 1 1 d . . . . .
H24 H 0.855241 0.609692 0.835557 0.044 Uiso 1 1 calc R U . . .
C25 C 0.6205(5) 0.5762(3) 0.8814(2) 0.0380(8) Uani 1 1 d . . . . .
C26 C 0.5121(5) 0.5014(3) 0.8842(2) 0.0371(8) Uani 1 1 d . . . . .
H26 H 0.405396 0.509438 0.914972 0.045 Uiso 1 1 calc R U . . .
C27 C 0.5653(4) 0.4160(3) 0.8408(2) 0.0332(7) Uani 1 1 d . . . . .
N28 N 0.9728(4) 0.4433(2) 0.75213(17) 0.0331(6) Uani 1 1 d . . . . .
N29 N 0.9948(4) 0.3569(3) 0.70993(18) 0.0379(7) Uani 1 1 d . . . . .
C30 C 1.1485(5) 0.3515(3) 0.6728(2) 0.0432(9) Uani 1 1 d . . . . .
H30 H 1.199321 0.298681 0.638754 0.052 Uiso 1 1 calc R U . . .
C31 C 1.2269(5) 0.4336(3) 0.6901(2) 0.0432(9) Uani 1 1 d . . . . .
H31 H 1.337128 0.446779 0.670836 0.052 Uiso 1 1 calc R U . . .
C32 C 1.1123(5) 0.4905(3) 0.7403(2) 0.0388(8) Uani 1 1 d . . . . .
H32 H 1.127051 0.552025 0.762840 0.047 Uiso 1 1 calc R U . . .
N33 N 0.4661(4) 0.3373(3) 0.83606(17) 0.0373(7) Uani 1 1 d . . . . .
N34 N 0.5259(4) 0.2614(3) 0.78522(18) 0.0396(7) Uani 1 1 d . . . . .
C35 C 0.4097(5) 0.1986(4) 0.7944(3) 0.0484(10) Uani 1 1 d . . . . .
H35 H 0.416065 0.138164 0.766342 0.058 Uiso 1 1 calc R U . . .
C36 C 0.2771(6) 0.2317(4) 0.8501(3) 0.0558(12) Uani 1 1 d . . . . .
H36 H 0.179659 0.199015 0.866984 0.067 Uiso 1 1 calc R U . . .
C37 C 0.3147(5) 0.3204(4) 0.8756(2) 0.0484(10) Uani 1 1 d . . . . .
H37 H 0.248237 0.362453 0.913697 0.058 Uiso 1 1 calc R U . . .
N38 N 0.5647(5) 0.6651(3) 0.9235(2) 0.0465(8) Uani 1 1 d . . . . .
H38 H 0.490787 0.656583 0.965260 0.056 Uiso 1 1 calc R U . . .
C39 C 0.6157(6) 0.7653(4) 0.9053(3) 0.0517(11) Uani 1 1 d . . . . .
O40 O 0.7218(5) 0.7840(3) 0.8516(2) 0.0660(9) Uani 1 1 d . . . . .
C41 C 0.5260(8) 0.8491(4) 0.9584(4) 0.0770(17) Uani 1 1 d . . . . .
H41A H 0.576689 0.840388 1.005075 0.116 Uiso 1 1 calc R U . . .
H41B H 0.408970 0.839497 0.972254 0.116 Uiso 1 1 calc R U . . .
H41C H 0.534409 0.921538 0.932055 0.116 Uiso 1 1 calc R U . . .
Cl2A Cl 0.7061(7) -0.0735(3) 0.3841(2) 0.0291(10) Uiso 0.34 1 d D . P B 1
O43A O 0.6500(17) 0.0353(7) 0.4121(6) 0.037(2) Uiso 0.34 1 d D . P B 1
O44A O 0.7623(16) -0.0467(11) 0.2997(4) 0.028(2) Uiso 0.34 1 d D . P B 1
O45A O 0.5735(12) -0.1320(9) 0.3997(7) 0.048(3) Uiso 0.34 1 d D . P B 1
O46A O 0.8407(12) -0.1292(9) 0.4171(5) 0.028(2) Uiso 0.34 1 d D . P B 1
Cl2B Cl 0.6827(6) -0.0520(4) 0.3781(3) 0.0327(13) Uiso 0.33 1 d D . P C 2
O43B O 0.6019(15) 0.0366(8) 0.4166(6) 0.053(4) Uiso 0.33 1 d D . P C 2
O44B O 0.7444(18) -0.0224(11) 0.2967(6) 0.065(6) Uiso 0.33 1 d D . P C 2
O45B O 0.5748(12) -0.1298(8) 0.3795(7) 0.037(3) Uiso 0.33 1 d D . P C 2
O46B O 0.8307(13) -0.1011(9) 0.4133(6) 0.042(3) Uiso 0.33 1 d D . P C 2
Cl2C Cl 0.7162(7) -0.0572(5) 0.3709(3) 0.0328(13) Uiso 0.33 1 d D . P D 3
O43C O 0.7245(15) 0.0439(7) 0.3967(6) 0.061(3) Uiso 0.33 1 d D . P D 3
O44C O 0.8079(15) -0.0757(10) 0.2994(5) 0.062(4) Uiso 0.33 1 d D . P D 3
O45C O 0.5486(14) -0.0763(13) 0.3758(9) 0.093(4) Uiso 0.33 1 d D . P D 3
O46C O 0.7895(18) -0.1412(10) 0.4286(7) 0.078(5) Uiso 0.33 1 d D . P D 3
Cl7A Cl 0.1216(6) 0.6969(4) 0.9487(3) 0.0355(11) Uiso 0.34 1 d D . P E 1
O48A O 0.1353(10) 0.6354(9) 0.8856(5) 0.0378(18) Uiso 0.34 1 d D . P E 1
O49A O -0.0419(14) 0.7044(12) 0.9951(8) 0.068(5) Uiso 0.34 1 d D . P E 1
O50A O 0.1734(14) 0.7963(8) 0.9239(6) 0.062(3) Uiso 0.34 1 d D . P E 1
O51A O 0.2282(15) 0.6381(10) 1.0044(6) 0.028(3) Uiso 0.34 1 d D . P E 1
Cl7B Cl 0.0986(3) 0.6709(2) 0.95806(14) 0.0484(5) Uani 0.66 1 d D . P . .
O48B O 0.1489(14) 0.6886(11) 0.8775(5) 0.067(3) Uiso 0.33 1 d D . P E 2
O49B O -0.0314(11) 0.7560(8) 0.9837(6) 0.048(2) Uiso 0.33 1 d D . P E 2
O50B O 0.040(2) 0.5677(11) 0.9740(11) 0.136(7) Uiso 0.33 1 d D . P E 2
O51B O 0.2282(14) 0.6729(11) 1.0028(6) 0.054(3) Uiso 0.33 1 d D . P E 2
O48C O 0.1142(17) 0.5933(11) 0.9060(8) 0.082(4) Uiso 0.33 1 d D . P E 3
O49C O -0.0635(13) 0.7190(13) 0.9801(8) 0.060(4) Uiso 0.33 1 d D . P E 3
O50C O 0.182(2) 0.7620(13) 0.9046(10) 0.122(7) Uiso 0.33 1 d D . P E 3
O51C O 0.201(2) 0.6363(16) 1.0128(9) 0.079(8) Uiso 0.33 1 d D . P E 3
C52A C 0.5429(15) 0.2173(8) 0.2634(6) 0.058(2) Uiso 0.5 1 d D . P F 1
H52A H 0.627085 0.225044 0.217448 0.087 Uiso 0.5 1 calc R U P F 1
H52B H 0.441736 0.200993 0.248605 0.087 Uiso 0.5 1 calc R U P F 1
H52C H 0.584820 0.158329 0.299564 0.087 Uiso 0.5 1 calc R U P F 1
C53A C 0.5056(18) 0.3182(9) 0.3003(7) 0.047(4) Uiso 0.5 1 d D . P F 1
N54A N 0.466(2) 0.3909(11) 0.3333(9) 0.073(5) Uiso 0.5 1 d D . P F 1
C52B C 0.6204(18) 0.2222(9) 0.2623(8) 0.074(3) Uiso 0.5 1 d D . P G 2
H52D H 0.650082 0.237831 0.206466 0.111 Uiso 0.5 1 calc R U P G 2
H52E H 0.543329 0.168904 0.273225 0.111 Uiso 0.5 1 calc R U P G 2
H52F H 0.720785 0.193323 0.284518 0.111 Uiso 0.5 1 calc R U P G 2
C53B C 0.5414(19) 0.3216(11) 0.2962(9) 0.058(5) Uiso 0.5 1 d D . P G 2
N54B N 0.4839(19) 0.4014(10) 0.3192(9) 0.064(4) Uiso 0.5 1 d D . P G 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.119(3) . ?
Fe1 N9 2.193(3) . ?
Fe1 N14 2.176(3) . ?
Fe1 N22 2.132(3) . ?
Fe1 N29 2.185(3) . ?
Fe1 N34 2.200(3) . ?
N2 C3 1.325(4) . ?
N2 C7 1.332(5) . ?
C3 C4 1.367(5) . ?
C3 N8 1.418(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.400(5) . ?
C5 C6 1.394(5) . ?
C5 N18 1.393(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.370(5) . ?
C7 N13 1.410(4) . ?
N8 N9 1.368(4) . ?
N8 C12 1.344(5) . ?
N9 C10 1.330(5) . ?
C10 H10 0.9500 . ?
C10 C11 1.399(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.367(6) . ?
C12 H12 0.9500 . ?
N13 N14 1.366(5) . ?
N13 C17A 1.343(6) . ?
N13 C17B 1.392(7) . ?
N14 C15A 1.317(6) . ?
N14 C15B 1.350(7) . ?
C15A H15A 0.9500 . ?
C15A C16A 1.414(8) . ?
C16A H16A 0.9500 . ?
C16A C17A 1.368(8) . ?
C17A H17A 0.9500 . ?
C15B H15B 0.9500 . ?
C15B C16B 1.384(9) . ?
C16B H16B 0.9500 . ?
C16B C17B 1.363(8) . ?
C17B H17B 0.9500 . ?
N18 H18 0.8800 . ?
N18 C19 1.372(5) . ?
C19 O20 1.207(6) . ?
C19 C21 1.504(6) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
N22 C23 1.325(5) . ?
N22 C27 1.332(5) . ?
C23 C24 1.381(5) . ?
C23 N28 1.409(5) . ?
C24 H24 0.9500 . ?
C24 C25 1.393(6) . ?
C25 C26 1.395(5) . ?
C25 N38 1.396(5) . ?
C26 H26 0.9500 . ?
C26 C27 1.371(5) . ?
C27 N33 1.406(5) . ?
N28 N29 1.368(4) . ?
N28 C32 1.356(5) . ?
N29 C30 1.321(5) . ?
C30 H30 0.9500 . ?
C30 C31 1.399(6) . ?
C31 H31 0.9500 . ?
C31 C32 1.358(6) . ?
C32 H32 0.9500 . ?
N33 N34 1.370(4) . ?
N33 C37 1.359(5) . ?
N34 C35 1.319(5) . ?
C35 H35 0.9500 . ?
C35 C36 1.387(6) . ?
C36 H36 0.9500 . ?
C36 C37 1.357(6) . ?
C37 H37 0.9500 . ?
N38 H38 0.8800 . ?
N38 C39 1.379(6) . ?
C39 O40 1.204(6) . ?
C39 C41 1.515(6) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
Cl2A O43A 1.492(8) . ?
Cl2A O44A 1.499(8) . ?
Cl2A O45A 1.390(9) . ?
Cl2A O46A 1.397(9) . ?
Cl2B O43B 1.395(10) . ?
Cl2B O44B 1.466(11) . ?
Cl2B O45B 1.425(9) . ?
Cl2B O46B 1.483(10) . ?
Cl2C O43C 1.422(9) . ?
Cl2C O44C 1.383(10) . ?
Cl2C O45C 1.433(11) . ?
Cl2C O46C 1.508(11) . ?
Cl7A O48A 1.417(8) . ?
Cl7A O49A 1.450(11) . ?
Cl7A O50A 1.385(10) . ?
Cl7A O51A 1.491(8) . ?
Cl7B O48B 1.416(9) . ?
Cl7B O49B 1.445(8) . ?
Cl7B O50B 1.440(12) . ?
Cl7B O51B 1.448(9) . ?
Cl7B O48C 1.402(10) . ?
Cl7B O49C 1.389(10) . ?
Cl7B O50C 1.565(12) . ?
Cl7B O51C 1.385(11) . ?
C52A H52A 0.9800 . ?
C52A H52B 0.9800 . ?
C52A H52C 0.9800 . ?
C52A C53A 1.467(11) . ?
C53A N54A 1.122(12) . ?
C52B H52D 0.9800 . ?
C52B H52E 0.9800 . ?
C52B H52F 0.9800 . ?
C52B C53B 1.463(12) . ?
C53B N54B 1.133(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N9 73.19(11) . . ?
N2 Fe1 N14 73.47(11) . . ?
N2 Fe1 N22 167.79(11) . . ?
N2 Fe1 N29 117.76(11) . . ?
N2 Fe1 N34 96.23(11) . . ?
N9 Fe1 N34 95.46(12) . . ?
N14 Fe1 N9 146.65(11) . . ?
N14 Fe1 N29 101.06(12) . . ?
N14 Fe1 N34 87.44(13) . . ?
N22 Fe1 N9 112.89(11) . . ?
N22 Fe1 N14 99.76(12) . . ?
N22 Fe1 N29 73.11(11) . . ?
N22 Fe1 N34 73.03(11) . . ?
N29 Fe1 N9 94.93(12) . . ?
N29 Fe1 N34 146.01(12) . . ?
C3 N2 Fe1 121.7(2) . . ?
C3 N2 C7 117.1(3) . . ?
C7 N2 Fe1 121.2(2) . . ?
N2 C3 C4 124.4(3) . . ?
N2 C3 N8 112.8(3) . . ?
C4 C3 N8 122.8(3) . . ?
C3 C4 H4 121.3 . . ?
C3 C4 C5 117.3(3) . . ?
C5 C4 H4 121.3 . . ?
C6 C5 C4 119.5(3) . . ?
N18 C5 C4 116.4(3) . . ?
N18 C5 C6 124.1(3) . . ?
C5 C6 H6 121.4 . . ?
C7 C6 C5 117.1(3) . . ?
C7 C6 H6 121.4 . . ?
N2 C7 C6 124.5(3) . . ?
N2 C7 N13 112.5(3) . . ?
C6 C7 N13 123.0(3) . . ?
N9 N8 C3 117.9(3) . . ?
C12 N8 C3 130.4(3) . . ?
C12 N8 N9 111.5(3) . . ?
N8 N9 Fe1 114.4(2) . . ?
C10 N9 Fe1 140.8(3) . . ?
C10 N9 N8 104.6(3) . . ?
N9 C10 H10 124.4 . . ?
N9 C10 C11 111.3(3) . . ?
C11 C10 H10 124.4 . . ?
C10 C11 H11 127.4 . . ?
C12 C11 C10 105.2(4) . . ?
C12 C11 H11 127.4 . . ?
N8 C12 C11 107.3(3) . . ?
N8 C12 H12 126.3 . . ?
C11 C12 H12 126.3 . . ?
N14 N13 C7 118.4(3) . . ?
N14 N13 C17B 118.1(4) . . ?
C17A N13 C7 134.6(4) . . ?
C17A N13 N14 105.2(4) . . ?
C17B N13 C7 122.8(5) . . ?
N13 N14 Fe1 114.5(2) . . ?
C15A N14 Fe1 131.7(4) . . ?
C15A N14 N13 112.8(4) . . ?
C15B N14 Fe1 149.1(5) . . ?
C15B N14 N13 96.3(5) . . ?
N14 C15A H15A 127.4 . . ?
N14 C15A C16A 105.1(6) . . ?
C16A C15A H15A 127.4 . . ?
C15A C16A H16A 126.6 . . ?
C17A C16A C15A 106.7(6) . . ?
C17A C16A H16A 126.6 . . ?
N13 C17A C16A 109.9(6) . . ?
N13 C17A H17A 125.0 . . ?
C16A C17A H17A 125.0 . . ?
N14 C15B H15B 121.1 . . ?
N14 C15B C16B 117.8(8) . . ?
C16B C15B H15B 121.1 . . ?
C15B C16B H16B 127.6 . . ?
C17B C16B C15B 104.8(8) . . ?
C17B C16B H16B 127.6 . . ?
N13 C17B H17B 128.7 . . ?
C16B C17B N13 102.5(7) . . ?
C16B C17B H17B 128.7 . . ?
C5 N18 H18 116.1 . . ?
C19 N18 C5 127.9(4) . . ?
C19 N18 H18 116.1 . . ?
N18 C19 C21 113.7(4) . . ?
O20 C19 N18 123.0(4) . . ?
O20 C19 C21 123.3(4) . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 N22 Fe1 121.3(2) . . ?
C23 N22 C27 117.6(3) . . ?
C27 N22 Fe1 121.1(2) . . ?
N22 C23 C24 124.6(3) . . ?
N22 C23 N28 112.6(3) . . ?
C24 C23 N28 122.8(3) . . ?
C23 C24 H24 121.8 . . ?
C23 C24 C25 116.4(3) . . ?
C25 C24 H24 121.8 . . ?
C24 C25 C26 120.1(3) . . ?
C24 C25 N38 122.2(4) . . ?
C26 C25 N38 117.6(4) . . ?
C25 C26 H26 121.3 . . ?
C27 C26 C25 117.5(4) . . ?
C27 C26 H26 121.3 . . ?
N22 C27 C26 123.7(3) . . ?
N22 C27 N33 113.0(3) . . ?
C26 C27 N33 123.3(3) . . ?
N29 N28 C23 118.4(3) . . ?
C32 N28 C23 130.9(3) . . ?
C32 N28 N29 110.7(3) . . ?
N28 N29 Fe1 114.5(2) . . ?
C30 N29 Fe1 140.1(3) . . ?
C30 N29 N28 105.3(3) . . ?
N29 C30 H30 124.4 . . ?
N29 C30 C31 111.1(3) . . ?
C31 C30 H30 124.4 . . ?
C30 C31 H31 127.2 . . ?
C32 C31 C30 105.6(3) . . ?
C32 C31 H31 127.2 . . ?
N28 C32 C31 107.3(3) . . ?
N28 C32 H32 126.4 . . ?
C31 C32 H32 126.4 . . ?
N34 N33 C27 118.3(3) . . ?
C37 N33 C27 130.7(3) . . ?
C37 N33 N34 111.1(3) . . ?
N33 N34 Fe1 114.2(2) . . ?
C35 N34 Fe1 140.3(3) . . ?
C35 N34 N33 104.7(3) . . ?
N34 C35 H35 124.2 . . ?
N34 C35 C36 111.6(4) . . ?
C36 C35 H35 124.2 . . ?
C35 C36 H36 127.0 . . ?
C37 C36 C35 106.1(4) . . ?
C37 C36 H36 127.0 . . ?
N33 C37 H37 126.7 . . ?
C36 C37 N33 106.6(4) . . ?
C36 C37 H37 126.7 . . ?
C25 N38 H38 117.3 . . ?
C39 N38 C25 125.5(4) . . ?
C39 N38 H38 117.3 . . ?
N38 C39 C41 114.2(4) . . ?
O40 C39 N38 122.5(4) . . ?
O40 C39 C41 123.3(4) . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O43A Cl2A O44A 102.6(7) . . ?
O45A Cl2A O43A 109.0(8) . . ?
O45A Cl2A O44A 113.4(7) . . ?
O45A Cl2A O46A 110.8(7) . . ?
O46A Cl2A O43A 112.0(6) . . ?
O46A Cl2A O44A 108.9(8) . . ?
O43B Cl2B O44B 112.7(8) . . ?
O43B Cl2B O45B 111.5(7) . . ?
O43B Cl2B O46B 109.4(7) . . ?
O44B Cl2B O46B 106.0(7) . . ?
O45B Cl2B O44B 106.3(7) . . ?
O45B Cl2B O46B 110.8(7) . . ?
O43C Cl2C O45C 112.1(9) . . ?
O43C Cl2C O46C 105.2(7) . . ?
O44C Cl2C O43C 115.2(7) . . ?
O44C Cl2C O45C 111.4(8) . . ?
O44C Cl2C O46C 106.8(8) . . ?
O45C Cl2C O46C 105.2(8) . . ?
O48A Cl7A O49A 112.4(8) . . ?
O48A Cl7A O51A 109.4(6) . . ?
O49A Cl7A O51A 101.9(8) . . ?
O50A Cl7A O48A 110.6(7) . . ?
O50A Cl7A O49A 113.6(8) . . ?
O50A Cl7A O51A 108.5(7) . . ?
O48B Cl7B O49B 109.9(6) . . ?
O48B Cl7B O50B 107.7(8) . . ?
O48B Cl7B O51B 114.1(7) . . ?
O49B Cl7B O51B 105.0(7) . . ?
O50B Cl7B O49B 110.6(8) . . ?
O50B Cl7B O51B 109.6(8) . . ?
O48C Cl7B O50C 100.4(8) . . ?
O49C Cl7B O48C 113.9(8) . . ?
O49C Cl7B O50C 104.0(9) . . ?
O51C Cl7B O48C 110.8(9) . . ?
O51C Cl7B O49C 120.1(9) . . ?
O51C Cl7B O50C 105.0(9) . . ?
H52A C52A H52B 109.5 . . ?
H52A C52A H52C 109.5 . . ?
H52B C52A H52C 109.5 . . ?
C53A C52A H52A 109.5 . . ?
C53A C52A H52B 109.5 . . ?
C53A C52A H52C 109.5 . . ?
N54A C53A C52A 173.5(17) . . ?
H52D C52B H52E 109.5 . . ?
H52D C52B H52F 109.5 . . ?
H52E C52B H52F 109.5 . . ?
C53B C52B H52D 109.5 . . ?
C53B C52B H52E 109.5 . . ?
C53B C52B H52F 109.5 . . ?
N54B C53B C52B 176.6(18) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N18 H18 O46A 0.88 2.01 2.881(9) 167.9 . yes
N18 H18 O46B 0.88 2.14 2.997(10) 164.4 . yes
N18 H18 O46C 0.88 1.93 2.810(12) 177.9 . yes
N38 H38 O51A 0.88 2.20 2.951(15) 142.6 . yes
N38 H38 O51B 0.88 2.14 2.881(12) 141.3 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N2 C3 C4 -179.7(3) . . . . ?
Fe1 N2 C3 N8 -0.4(4) . . . . ?
Fe1 N2 C7 C6 178.3(3) . . . . ?
Fe1 N2 C7 N13 0.1(4) . . . . ?
Fe1 N9 C10 C11 -174.0(3) . . . . ?
Fe1 N14 C15A C16A 167.2(4) . . . . ?
Fe1 N14 C15B C16B -171.5(7) . . . . ?
Fe1 N22 C23 C24 176.7(3) . . . . ?
Fe1 N22 C23 N28 -3.1(4) . . . . ?
Fe1 N22 C27 C26 -178.0(3) . . . . ?
Fe1 N22 C27 N33 1.1(4) . . . . ?
Fe1 N29 C30 C31 -174.4(3) . . . . ?
Fe1 N34 C35 C36 168.3(4) . . . . ?
N2 C3 C4 C5 1.3(5) . . . . ?
N2 C3 N8 N9 0.9(4) . . . . ?
N2 C3 N8 C12 -174.4(4) . . . . ?
N2 C7 N13 N14 0.1(5) . . . . ?
N2 C7 N13 C17A 162.1(6) . . . . ?
N2 C7 N13 C17B -169.9(6) . . . . ?
C3 N2 C7 C6 -1.1(5) . . . . ?
C3 N2 C7 N13 -179.3(3) . . . . ?
C3 C4 C5 C6 -1.0(5) . . . . ?
C3 C4 C5 N18 177.9(3) . . . . ?
C3 N8 N9 Fe1 -0.9(4) . . . . ?
C3 N8 N9 C10 -177.3(3) . . . . ?
C3 N8 C12 C11 176.6(4) . . . . ?
C4 C3 N8 N9 -179.8(3) . . . . ?
C4 C3 N8 C12 4.9(6) . . . . ?
C4 C5 C6 C7 -0.2(6) . . . . ?
C4 C5 N18 C19 179.5(4) . . . . ?
C5 C6 C7 N2 1.4(6) . . . . ?
C5 C6 C7 N13 179.4(3) . . . . ?
C5 N18 C19 O20 -3.3(8) . . . . ?
C5 N18 C19 C21 177.2(4) . . . . ?
C6 C5 N18 C19 -1.6(7) . . . . ?
C6 C7 N13 N14 -178.2(4) . . . . ?
C6 C7 N13 C17A -16.1(8) . . . . ?
C6 C7 N13 C17B 11.9(7) . . . . ?
C7 N2 C3 C4 -0.3(5) . . . . ?
C7 N2 C3 N8 179.0(3) . . . . ?
C7 N13 N14 Fe1 -0.2(4) . . . . ?
C7 N13 N14 C15A 169.7(5) . . . . ?
C7 N13 N14 C15B -177.0(5) . . . . ?
C7 N13 C17A C16A -167.8(6) . . . . ?
C7 N13 C17B C16B 177.8(6) . . . . ?
N8 C3 C4 C5 -177.9(3) . . . . ?
N8 N9 C10 C11 0.8(5) . . . . ?
N9 N8 C12 C11 1.1(5) . . . . ?
N9 C10 C11 C12 -0.2(5) . . . . ?
C10 C11 C12 N8 -0.5(5) . . . . ?
C12 N8 N9 Fe1 175.2(3) . . . . ?
C12 N8 N9 C10 -1.2(4) . . . . ?
N13 N14 C15A C16A -0.5(8) . . . . ?
N13 N14 C15B C16B 3.0(10) . . . . ?
N14 N13 C17A C16A -4.1(8) . . . . ?
N14 N13 C17B C16B 7.8(9) . . . . ?
N14 C15A C16A C17A -2.0(9) . . . . ?
N14 C15B C16B C17B 1.3(13) . . . . ?
C15A C16A C17A N13 3.9(10) . . . . ?
C17A N13 N14 Fe1 -167.0(4) . . . . ?
C17A N13 N14 C15A 2.9(7) . . . . ?
C15B C16B C17B N13 -4.8(11) . . . . ?
C17B N13 N14 Fe1 170.3(5) . . . . ?
C17B N13 N14 C15B -6.6(7) . . . . ?
N18 C5 C6 C7 -179.1(4) . . . . ?
N22 C23 C24 C25 0.9(6) . . . . ?
N22 C23 N28 N29 5.0(5) . . . . ?
N22 C23 N28 C32 -176.2(4) . . . . ?
N22 C27 N33 N34 -5.3(5) . . . . ?
N22 C27 N33 C37 173.4(4) . . . . ?
C23 N22 C27 C26 0.4(5) . . . . ?
C23 N22 C27 N33 179.4(3) . . . . ?
C23 C24 C25 C26 1.0(6) . . . . ?
C23 C24 C25 N38 -179.1(4) . . . . ?
C23 N28 N29 Fe1 -4.6(4) . . . . ?
C23 N28 N29 C30 179.4(3) . . . . ?
C23 N28 C32 C31 -179.3(4) . . . . ?
C24 C23 N28 N29 -174.7(3) . . . . ?
C24 C23 N28 C32 4.1(6) . . . . ?
C24 C25 C26 C27 -2.2(6) . . . . ?
C24 C25 N38 C39 28.9(6) . . . . ?
C25 C26 C27 N22 1.5(6) . . . . ?
C25 C26 C27 N33 -177.5(3) . . . . ?
C25 N38 C39 O40 -3.6(8) . . . . ?
C25 N38 C39 C41 176.1(4) . . . . ?
C26 C25 N38 C39 -151.2(4) . . . . ?
C26 C27 N33 N34 173.8(3) . . . . ?
C26 C27 N33 C37 -7.5(6) . . . . ?
C27 N22 C23 C24 -1.7(5) . . . . ?
C27 N22 C23 N28 178.6(3) . . . . ?
C27 N33 N34 Fe1 6.8(4) . . . . ?
C27 N33 N34 C35 178.9(3) . . . . ?
C27 N33 C37 C36 -178.4(4) . . . . ?
N28 C23 C24 C25 -179.3(3) . . . . ?
N28 N29 C30 C31 -0.2(5) . . . . ?
N29 N28 C32 C31 -0.4(4) . . . . ?
N29 C30 C31 C32 -0.1(5) . . . . ?
C30 C31 C32 N28 0.3(5) . . . . ?
C32 N28 N29 Fe1 176.3(2) . . . . ?
C32 N28 N29 C30 0.4(4) . . . . ?
N33 N34 C35 C36 -0.3(5) . . . . ?
N34 N33 C37 C36 0.4(5) . . . . ?
N34 C35 C36 C37 0.6(6) . . . . ?
C35 C36 C37 N33 -0.6(5) . . . . ?
C37 N33 N34 Fe1 -172.1(3) . . . . ?
C37 N33 N34 C35 0.0(5) . . . . ?
N38 C25 C26 C27 178.0(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.756(3)
2 0.244(3)

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile/diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_80etcnlt
_database_code_depnum_ccdc_archive 'CCDC 2078654'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2021-04-19 deposited with the CCDC.	2021-06-10 downloaded from the CCDC.
;
_audit_creation_date             2020-07-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis-[N-(2,6-di{pyrazol-1-yl}pyrid-4-yl)acetamide]iron(II)ditetrafluoroborate propionitrile solvate'
_chemical_formula_moiety         'C26 H24 Fe N12 O2, 2(B F4), C3 H5 N'
_chemical_formula_sum            'C29 H29 B2 F8 Fe N13 O2'
_chemical_formula_weight         821.12
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2658(5)
_cell_length_b                   12.3645(10)
_cell_length_c                   17.5585(11)
_cell_angle_alpha                83.555(6)
_cell_angle_beta                 79.079(5)
_cell_angle_gamma                84.390(6)
_cell_volume                     1745.5(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4341
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      72.61
_cell_measurement_theta_min      3.58
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.303
_exptl_absorpt_correction_T_max  0.690
_exptl_absorpt_correction_T_min  0.476
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.931
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10076
_diffrn_reflns_point_group_measured_fraction_full 0.931
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.715
_diffrn_reflns_theta_min         3.609
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7780
_reflns_number_total             10076
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2015)'
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         10076
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0631
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0942P)²+1.3621P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1595
_refine_ls_wR_factor_ref         0.1746
_refine_special_details          
;The data were resolved into two non-superimposable twin domains, in a 
 ratio of 0.52:0.48

 No disorder is present in the model and no restraints were applied to the
 refinement. All non-H atoms were refined anisotropically and H atoms were
 placed in calculated positions and refined using a riding model.,Twin
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.5188(13)
 0.4812(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17),
 N18(H18), C24(H24), C26(H26), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36),
  C37(H37), N38(H38)
3.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C41(H41A,H41B,H41C), C52(H52A,H52B,H52C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.76630(9) 0.77031(6) 0.72971(4) 0.02566(19) Uani 1 1 d . . . . .
N2 N 0.8164(5) 0.6348(3) 0.6846(2) 0.0260(8) Uani 1 1 d . . . . .
C3 C 0.7905(6) 0.6266(3) 0.6128(3) 0.0265(9) Uani 1 1 d . . . . .
C4 C 0.8126(6) 0.5301(4) 0.5791(3) 0.0277(10) Uani 1 1 d . . . . .
H4 H 0.797304 0.527560 0.527115 0.033 Uiso 1 1 calc R U . . .
C5 C 0.8584(6) 0.4355(4) 0.6243(3) 0.0307(10) Uani 1 1 d . . . . .
C6 C 0.8806(6) 0.4417(4) 0.7015(3) 0.0298(10) Uani 1 1 d . . . . .
H6 H 0.909794 0.378800 0.733915 0.036 Uiso 1 1 calc R U . . .
C7 C 0.8573(6) 0.5440(4) 0.7269(3) 0.0283(10) Uani 1 1 d . . . . .
N8 N 0.7367(5) 0.7286(3) 0.5780(2) 0.0283(8) Uani 1 1 d . . . . .
N9 N 0.7170(5) 0.8158(3) 0.6232(2) 0.0293(9) Uani 1 1 d . . . . .
C10 C 0.6610(6) 0.8984(4) 0.5792(3) 0.0338(10) Uani 1 1 d . . . . .
H10 H 0.636504 0.970440 0.594373 0.041 Uiso 1 1 calc R U . . .
C11 C 0.6413(7) 0.8676(4) 0.5071(3) 0.0379(11) Uani 1 1 d . . . . .
H11 H 0.602769 0.912852 0.465746 0.045 Uiso 1 1 calc R U . . .
C12 C 0.6896(7) 0.7587(4) 0.5090(3) 0.0356(11) Uani 1 1 d . . . . .
H12 H 0.689920 0.712739 0.469111 0.043 Uiso 1 1 calc R U . . .
N13 N 0.8694(5) 0.5683(3) 0.8028(2) 0.0279(8) Uani 1 1 d . . . . .
N14 N 0.8313(5) 0.6755(3) 0.8176(2) 0.0279(8) Uani 1 1 d . . . . .
C15 C 0.8411(6) 0.6773(4) 0.8920(3) 0.0330(11) Uani 1 1 d . . . . .
H15 H 0.820064 0.740908 0.919201 0.040 Uiso 1 1 calc R U . . .
C16 C 0.8863(7) 0.5737(4) 0.9248(3) 0.0387(11) Uani 1 1 d . . . . .
H16 H 0.902547 0.554166 0.976891 0.046 Uiso 1 1 calc R U . . .
C17 C 0.9025(6) 0.5055(4) 0.8673(3) 0.0351(11) Uani 1 1 d . . . . .
H17 H 0.931335 0.429077 0.871568 0.042 Uiso 1 1 calc R U . . .
N18 N 0.8733(5) 0.3385(3) 0.5900(2) 0.0330(9) Uani 1 1 d . . . . .
H18 H 0.846217 0.343157 0.543566 0.040 Uiso 1 1 calc R U . . .
C19 C 0.9250(7) 0.2358(4) 0.6196(3) 0.0351(11) Uani 1 1 d . . . . .
O20 O 0.9763(6) 0.2183(3) 0.6799(2) 0.0530(11) Uani 1 1 d . . . . .
C21 C 0.9091(8) 0.1475(4) 0.5686(3) 0.0456(14) Uani 1 1 d . . . . .
H21A H 0.979612 0.082286 0.581672 0.068 Uiso 1 1 calc R U . . .
H21B H 0.943497 0.173901 0.513726 0.068 Uiso 1 1 calc R U . . .
H21C H 0.793777 0.129372 0.577595 0.068 Uiso 1 1 calc R U . . .
N22 N 0.7042(5) 0.8971(3) 0.7847(2) 0.0278(8) Uani 1 1 d . . . . .
C23 C 0.5550(6) 0.9101(4) 0.8281(3) 0.0278(10) Uani 1 1 d . . . . .
C24 C 0.5040(6) 0.9954(4) 0.8733(3) 0.0332(11) Uani 1 1 d . . . . .
H24 H 0.395447 1.002853 0.903015 0.040 Uiso 1 1 calc R U . . .
C25 C 0.6203(6) 1.0710(4) 0.8733(3) 0.0335(11) Uani 1 1 d . . . . .
C26 C 0.7811(7) 1.0573(4) 0.8301(3) 0.0328(11) Uani 1 1 d . . . . .
H26 H 0.862312 1.106569 0.830303 0.039 Uiso 1 1 calc R U . . .
C27 C 0.8138(6) 0.9684(4) 0.7877(3) 0.0283(10) Uani 1 1 d . . . . .
N28 N 0.4574(5) 0.8252(3) 0.8216(2) 0.0307(9) Uani 1 1 d . . . . .
N29 N 0.5327(5) 0.7474(3) 0.7731(2) 0.0295(8) Uani 1 1 d . . . . .
C30 C 0.4203(7) 0.6765(4) 0.7772(3) 0.0372(12) Uani 1 1 d . . . . .
H30 H 0.436340 0.613780 0.749160 0.045 Uiso 1 1 calc R U . . .
C31 C 0.2745(7) 0.7059(5) 0.8284(3) 0.0422(12) Uani 1 1 d . . . . .
H31 H 0.177444 0.667505 0.841644 0.051 Uiso 1 1 calc R U . . .
C32 C 0.3006(7) 0.8003(4) 0.8550(3) 0.0382(12) Uani 1 1 d . . . . .
H32 H 0.224152 0.841418 0.890346 0.046 Uiso 1 1 calc R U . . .
N33 N 0.9684(5) 0.9370(3) 0.7426(2) 0.0304(9) Uani 1 1 d . . . . .
N34 N 0.9770(5) 0.8424(3) 0.7059(2) 0.0302(9) Uani 1 1 d . . . . .
C35 C 1.1308(6) 0.8338(4) 0.6666(3) 0.0352(10) Uani 1 1 d . . . . .
H35 H 1.174951 0.776550 0.634952 0.042 Uiso 1 1 calc R U . . .
C36 C 1.2188(6) 0.9190(4) 0.6776(3) 0.0361(11) Uani 1 1 d . . . . .
H36 H 1.330835 0.930071 0.655653 0.043 Uiso 1 1 calc R U . . .
C37 C 1.1129(6) 0.9841(4) 0.7261(3) 0.0346(11) Uani 1 1 d . . . . .
H37 H 1.136518 1.049272 0.744403 0.041 Uiso 1 1 calc R U . . .
N38 N 0.5691(6) 1.1581(3) 0.9182(3) 0.0380(10) Uani 1 1 d . . . . .
H38 H 0.479628 1.150797 0.953937 0.046 Uiso 1 1 calc R U . . .
C39 C 0.6434(7) 1.2549(4) 0.9128(3) 0.0386(12) Uani 1 1 d . . . . .
O40 O 0.7675(5) 1.2749(3) 0.8667(2) 0.0451(9) Uani 1 1 d . . . . .
C41 C 0.5505(8) 1.3338(5) 0.9683(4) 0.0522(15) Uani 1 1 d . . . . .
H41A H 0.619298 1.393497 0.969783 0.078 Uiso 1 1 calc R U . . .
H41B H 0.523829 1.295595 1.020571 0.078 Uiso 1 1 calc R U . . .
H41C H 0.448156 1.363571 0.950659 0.078 Uiso 1 1 calc R U . . .
B42 B 0.7141(8) 0.4434(5) 0.3885(4) 0.0390(14) Uani 1 1 d . . . . .
F43 F 0.7150(5) 0.5499(3) 0.4082(2) 0.0611(10) Uani 1 1 d . . . . .
F44 F 0.5587(5) 0.4129(4) 0.3967(2) 0.0699(11) Uani 1 1 d . . . . .
F45 F 0.7914(4) 0.4390(3) 0.31099(18) 0.0492(8) Uani 1 1 d . . . . .
F46 F 0.8063(5) 0.3746(3) 0.4355(2) 0.0589(10) Uani 1 1 d . . . . .
B47 B 0.1088(9) 1.1701(6) 0.9532(4) 0.0430(15) Uani 1 1 d . . . . .
F48 F 0.1255(4) 1.1134(3) 0.88813(19) 0.0511(8) Uani 1 1 d . . . . .
F49 F -0.0424(5) 1.1614(4) 0.9998(2) 0.0781(13) Uani 1 1 d . . . . .
F50 F 0.1354(6) 1.2792(3) 0.9294(2) 0.0694(11) Uani 1 1 d . . . . .
F51 F 0.2335(4) 1.1283(3) 0.99606(18) 0.0490(8) Uani 1 1 d . . . . .
C52 C 0.5490(12) 0.6403(6) 0.2465(5) 0.080(3) Uani 1 1 d . . . . .
H52A H 0.501002 0.604717 0.297412 0.119 Uiso 1 1 calc R U . . .
H52B H 0.608437 0.585018 0.213504 0.119 Uiso 1 1 calc R U . . .
H52C H 0.460659 0.679175 0.221660 0.119 Uiso 1 1 calc R U . . .
C53 C 0.6669(9) 0.7200(5) 0.2574(4) 0.0584(17) Uani 1 1 d . . . . .
H53A H 0.750474 0.682236 0.286786 0.070 Uiso 1 1 calc R U . . .
H53B H 0.725149 0.749829 0.205879 0.070 Uiso 1 1 calc R U . . .
C54 C 0.5746(9) 0.8103(5) 0.3005(4) 0.0544(16) Uani 1 1 d . . . . .
N55 N 0.5057(8) 0.8804(5) 0.3312(4) 0.0696(17) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.909(3) . ?
Fe1 N9 1.997(4) . ?
Fe1 N14 1.957(4) . ?
Fe1 N22 1.910(4) . ?
Fe1 N29 1.973(4) . ?
Fe1 N34 1.987(4) . ?
N2 C3 1.334(6) . ?
N2 C7 1.327(6) . ?
C3 C4 1.372(6) . ?
C3 N8 1.407(6) . ?
C4 H4 0.9500 . ?
C4 C5 1.399(7) . ?
C5 C6 1.415(7) . ?
C5 N18 1.386(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.372(6) . ?
C7 N13 1.421(6) . ?
N8 N9 1.388(5) . ?
N8 C12 1.344(6) . ?
N9 C10 1.311(6) . ?
C10 H10 0.9500 . ?
C10 C11 1.406(7) . ?
C11 H11 0.9500 . ?
C11 C12 1.365(7) . ?
C12 H12 0.9500 . ?
N13 N14 1.375(5) . ?
N13 C17 1.356(6) . ?
N14 C15 1.326(6) . ?
C15 H15 0.9500 . ?
C15 C16 1.392(7) . ?
C16 H16 0.9500 . ?
C16 C17 1.367(7) . ?
C17 H17 0.9500 . ?
N18 H18 0.8800 . ?
N18 C19 1.377(6) . ?
C19 O20 1.204(7) . ?
C19 C21 1.517(6) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
N22 C23 1.327(6) . ?
N22 C27 1.336(6) . ?
C23 C24 1.376(6) . ?
C23 N28 1.412(6) . ?
C24 H24 0.9500 . ?
C24 C25 1.405(7) . ?
C25 C26 1.404(7) . ?
C25 N38 1.391(6) . ?
C26 H26 0.9500 . ?
C26 C27 1.373(6) . ?
C27 N33 1.414(6) . ?
N28 N29 1.380(5) . ?
N28 C32 1.367(7) . ?
N29 C30 1.325(6) . ?
C30 H30 0.9500 . ?
C30 C31 1.403(8) . ?
C31 H31 0.9500 . ?
C31 C32 1.355(7) . ?
C32 H32 0.9500 . ?
N33 N34 1.388(5) . ?
N33 C37 1.348(6) . ?
N34 C35 1.327(6) . ?
C35 H35 0.9500 . ?
C35 C36 1.388(7) . ?
C36 H36 0.9500 . ?
C36 C37 1.369(7) . ?
C37 H37 0.9500 . ?
N38 H38 0.8800 . ?
N38 C39 1.384(7) . ?
C39 O40 1.207(7) . ?
C39 C41 1.508(7) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
B42 F43 1.400(6) . ?
B42 F44 1.352(7) . ?
B42 F45 1.394(7) . ?
B42 F46 1.393(7) . ?
B47 F48 1.384(7) . ?
B47 F49 1.365(8) . ?
B47 F50 1.392(8) . ?
B47 F51 1.413(8) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C52 C53 1.502(10) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53 C54 1.486(9) . ?
C54 N55 1.122(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N9 79.78(15) . . ?
N2 Fe1 N14 79.47(15) . . ?
N2 Fe1 N22 173.79(18) . . ?
N2 Fe1 N29 95.99(16) . . ?
N2 Fe1 N34 105.04(16) . . ?
N14 Fe1 N9 159.25(15) . . ?
N14 Fe1 N29 89.38(17) . . ?
N14 Fe1 N34 93.41(17) . . ?
N22 Fe1 N9 104.70(16) . . ?
N22 Fe1 N14 95.96(17) . . ?
N22 Fe1 N29 79.66(17) . . ?
N22 Fe1 N34 79.30(16) . . ?
N29 Fe1 N9 92.35(17) . . ?
N29 Fe1 N34 158.95(15) . . ?
N34 Fe1 N9 92.36(17) . . ?
C3 N2 Fe1 120.4(3) . . ?
C7 N2 Fe1 120.8(3) . . ?
C7 N2 C3 118.2(4) . . ?
N2 C3 C4 123.3(4) . . ?
N2 C3 N8 111.1(4) . . ?
C4 C3 N8 125.6(4) . . ?
C3 C4 H4 121.2 . . ?
C3 C4 C5 117.6(4) . . ?
C5 C4 H4 121.2 . . ?
C4 C5 C6 120.0(4) . . ?
N18 C5 C4 116.4(4) . . ?
N18 C5 C6 123.5(4) . . ?
C5 C6 H6 122.0 . . ?
C7 C6 C5 116.0(4) . . ?
C7 C6 H6 122.0 . . ?
N2 C7 C6 124.8(4) . . ?
N2 C7 N13 109.9(4) . . ?
C6 C7 N13 125.3(4) . . ?
N9 N8 C3 116.5(4) . . ?
C12 N8 C3 132.1(4) . . ?
C12 N8 N9 111.3(4) . . ?
N8 N9 Fe1 112.1(3) . . ?
C10 N9 Fe1 143.3(3) . . ?
C10 N9 N8 104.4(4) . . ?
N9 C10 H10 124.1 . . ?
N9 C10 C11 111.9(4) . . ?
C11 C10 H10 124.1 . . ?
C10 C11 H11 127.4 . . ?
C12 C11 C10 105.2(5) . . ?
C12 C11 H11 127.4 . . ?
N8 C12 C11 107.2(4) . . ?
N8 C12 H12 126.4 . . ?
C11 C12 H12 126.4 . . ?
N14 N13 C7 115.8(4) . . ?
C17 N13 C7 133.0(4) . . ?
C17 N13 N14 111.0(4) . . ?
N13 N14 Fe1 113.8(3) . . ?
C15 N14 Fe1 140.9(3) . . ?
C15 N14 N13 105.1(4) . . ?
N14 C15 H15 124.5 . . ?
N14 C15 C16 111.0(4) . . ?
C16 C15 H15 124.5 . . ?
C15 C16 H16 126.9 . . ?
C17 C16 C15 106.3(4) . . ?
C17 C16 H16 126.9 . . ?
N13 C17 C16 106.6(4) . . ?
N13 C17 H17 126.7 . . ?
C16 C17 H17 126.7 . . ?
C5 N18 H18 115.9 . . ?
C19 N18 C5 128.1(4) . . ?
C19 N18 H18 115.9 . . ?
N18 C19 C21 113.0(5) . . ?
O20 C19 N18 123.2(4) . . ?
O20 C19 C21 123.8(5) . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 N22 Fe1 120.2(3) . . ?
C23 N22 C27 118.0(4) . . ?
C27 N22 Fe1 121.4(3) . . ?
N22 C23 C24 123.9(4) . . ?
N22 C23 N28 111.0(4) . . ?
C24 C23 N28 125.1(4) . . ?
C23 C24 H24 121.7 . . ?
C23 C24 C25 116.7(4) . . ?
C25 C24 H24 121.7 . . ?
C26 C25 C24 120.7(4) . . ?
N38 C25 C24 117.0(4) . . ?
N38 C25 C26 122.2(5) . . ?
C25 C26 H26 122.0 . . ?
C27 C26 C25 115.9(5) . . ?
C27 C26 H26 122.0 . . ?
N22 C27 C26 124.6(4) . . ?
N22 C27 N33 110.0(4) . . ?
C26 C27 N33 125.4(4) . . ?
N29 N28 C23 115.8(4) . . ?
C32 N28 C23 133.6(4) . . ?
C32 N28 N29 110.5(4) . . ?
N28 N29 Fe1 113.1(3) . . ?
C30 N29 Fe1 141.7(3) . . ?
C30 N29 N28 105.0(4) . . ?
N29 C30 H30 124.3 . . ?
N29 C30 C31 111.3(4) . . ?
C31 C30 H30 124.3 . . ?
C30 C31 H31 127.0 . . ?
C32 C31 C30 105.9(5) . . ?
C32 C31 H31 127.0 . . ?
N28 C32 H32 126.4 . . ?
C31 C32 N28 107.2(5) . . ?
C31 C32 H32 126.4 . . ?
N34 N33 C27 116.4(4) . . ?
C37 N33 C27 131.8(4) . . ?
C37 N33 N34 111.8(4) . . ?
N33 N34 Fe1 112.8(3) . . ?
C35 N34 Fe1 143.1(3) . . ?
C35 N34 N33 104.1(4) . . ?
N34 C35 H35 124.4 . . ?
N34 C35 C36 111.3(4) . . ?
C36 C35 H35 124.4 . . ?
C35 C36 H36 126.6 . . ?
C37 C36 C35 106.8(5) . . ?
C37 C36 H36 126.6 . . ?
N33 C37 C36 106.0(4) . . ?
N33 C37 H37 127.0 . . ?
C36 C37 H37 127.0 . . ?
C25 N38 H38 116.4 . . ?
C39 N38 C25 127.2(5) . . ?
C39 N38 H38 116.4 . . ?
N38 C39 C41 113.2(5) . . ?
O40 C39 N38 123.1(4) . . ?
O40 C39 C41 123.7(5) . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
F44 B42 F43 111.7(5) . . ?
F44 B42 F45 108.8(4) . . ?
F44 B42 F46 111.4(5) . . ?
F45 B42 F43 108.5(5) . . ?
F46 B42 F43 107.7(4) . . ?
F46 B42 F45 108.6(5) . . ?
F48 B47 F50 109.2(5) . . ?
F48 B47 F51 108.8(5) . . ?
F49 B47 F48 112.0(5) . . ?
F49 B47 F50 110.6(5) . . ?
F49 B47 F51 109.3(5) . . ?
F50 B47 F51 106.9(5) . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C53 C52 H52A 109.5 . . ?
C53 C52 H52B 109.5 . . ?
C53 C52 H52C 109.5 . . ?
C52 C53 H53A 109.7 . . ?
C52 C53 H53B 109.7 . . ?
H53A C53 H53B 108.2 . . ?
C54 C53 C52 109.8(6) . . ?
C54 C53 H53A 109.7 . . ?
C54 C53 H53B 109.7 . . ?
N55 C54 C53 178.1(7) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N18 H18 F46 0.88 1.98 2.848(5) 170.7 . yes
N38 H38 F51 0.88 2.06 2.890(6) 156.1 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N2 C3 C4 -175.2(4) . . . . ?
Fe1 N2 C3 N8 4.2(5) . . . . ?
Fe1 N2 C7 C6 173.8(4) . . . . ?
Fe1 N2 C7 N13 -4.8(5) . . . . ?
Fe1 N9 C10 C11 -173.1(4) . . . . ?
Fe1 N14 C15 C16 174.3(4) . . . . ?
Fe1 N22 C23 C24 175.9(4) . . . . ?
Fe1 N22 C23 N28 -4.1(5) . . . . ?
Fe1 N22 C27 C26 -175.5(4) . . . . ?
Fe1 N22 C27 N33 2.8(5) . . . . ?
Fe1 N29 C30 C31 172.2(4) . . . . ?
Fe1 N34 C35 C36 -179.2(4) . . . . ?
N2 C3 C4 C5 2.6(7) . . . . ?
N2 C3 N8 N9 -1.4(6) . . . . ?
N2 C3 N8 C12 -176.8(5) . . . . ?
N2 C7 N13 N14 2.5(6) . . . . ?
N2 C7 N13 C17 178.0(5) . . . . ?
C3 N2 C7 C6 2.3(7) . . . . ?
C3 N2 C7 N13 -176.3(4) . . . . ?
C3 C4 C5 C6 -0.1(7) . . . . ?
C3 C4 C5 N18 177.4(4) . . . . ?
C3 N8 N9 Fe1 -1.6(5) . . . . ?
C3 N8 N9 C10 -177.6(4) . . . . ?
C3 N8 C12 C11 176.9(5) . . . . ?
C4 C3 N8 N9 177.9(4) . . . . ?
C4 C3 N8 C12 2.5(9) . . . . ?
C4 C5 C6 C7 -1.1(7) . . . . ?
C4 C5 N18 C19 176.0(5) . . . . ?
C5 C6 C7 N2 0.0(7) . . . . ?
C5 C6 C7 N13 178.4(5) . . . . ?
C5 N18 C19 O20 -5.2(9) . . . . ?
C5 N18 C19 C21 174.3(5) . . . . ?
C6 C5 N18 C19 -6.5(8) . . . . ?
C6 C7 N13 N14 -176.1(4) . . . . ?
C6 C7 N13 C17 -0.6(9) . . . . ?
C7 N2 C3 C4 -3.6(7) . . . . ?
C7 N2 C3 N8 175.7(4) . . . . ?
C7 N13 N14 Fe1 0.6(5) . . . . ?
C7 N13 N14 C15 176.3(4) . . . . ?
C7 N13 C17 C16 -175.9(5) . . . . ?
N8 C3 C4 C5 -176.6(4) . . . . ?
N8 N9 C10 C11 0.7(6) . . . . ?
N9 N8 C12 C11 1.3(6) . . . . ?
N9 C10 C11 C12 0.0(6) . . . . ?
C10 C11 C12 N8 -0.8(6) . . . . ?
C12 N8 N9 Fe1 174.7(3) . . . . ?
C12 N8 N9 C10 -1.3(5) . . . . ?
N13 N14 C15 C16 0.6(5) . . . . ?
N14 N13 C17 C16 -0.3(6) . . . . ?
N14 C15 C16 C17 -0.8(6) . . . . ?
C15 C16 C17 N13 0.6(6) . . . . ?
C17 N13 N14 Fe1 -175.8(3) . . . . ?
C17 N13 N14 C15 -0.2(5) . . . . ?
N18 C5 C6 C7 -178.5(5) . . . . ?
N22 C23 C24 C25 -1.1(7) . . . . ?
N22 C23 N28 N29 0.1(6) . . . . ?
N22 C23 N28 C32 178.2(5) . . . . ?
N22 C27 N33 N34 -0.2(6) . . . . ?
N22 C27 N33 C37 177.6(5) . . . . ?
C23 N22 C27 C26 -2.9(7) . . . . ?
C23 N22 C27 N33 175.5(4) . . . . ?
C23 C24 C25 C26 -1.2(7) . . . . ?
C23 C24 C25 N38 179.3(4) . . . . ?
C23 N28 N29 Fe1 3.6(5) . . . . ?
C23 N28 N29 C30 179.0(4) . . . . ?
C23 N28 C32 C31 -177.9(5) . . . . ?
C24 C23 N28 N29 -179.9(4) . . . . ?
C24 C23 N28 C32 -1.8(8) . . . . ?
C24 C25 C26 C27 1.4(7) . . . . ?
C24 C25 N38 C39 -162.5(5) . . . . ?
C25 C26 C27 N22 0.6(7) . . . . ?
C25 C26 C27 N33 -177.5(4) . . . . ?
C25 N38 C39 O40 -0.6(9) . . . . ?
C25 N38 C39 C41 177.5(5) . . . . ?
C26 C25 N38 C39 18.0(8) . . . . ?
C26 C27 N33 N34 178.1(4) . . . . ?
C26 C27 N33 C37 -4.0(8) . . . . ?
C27 N22 C23 C24 3.1(7) . . . . ?
C27 N22 C23 N28 -176.9(4) . . . . ?
C27 N33 N34 Fe1 -2.2(5) . . . . ?
C27 N33 N34 C35 178.2(4) . . . . ?
C27 N33 C37 C36 -178.0(5) . . . . ?
N28 C23 C24 C25 178.9(4) . . . . ?
N28 N29 C30 C31 -1.0(6) . . . . ?
N29 N28 C32 C31 0.2(6) . . . . ?
N29 C30 C31 C32 1.1(7) . . . . ?
C30 C31 C32 N28 -0.8(6) . . . . ?
C32 N28 N29 Fe1 -174.9(3) . . . . ?
C32 N28 N29 C30 0.5(5) . . . . ?
N33 N34 C35 C36 0.2(5) . . . . ?
N34 N33 C37 C36 -0.1(6) . . . . ?
N34 C35 C36 C37 -0.3(6) . . . . ?
C35 C36 C37 N33 0.2(6) . . . . ?
C37 N33 N34 Fe1 179.6(3) . . . . ?
C37 N33 N34 C35 -0.1(5) . . . . ?
N38 C25 C26 C27 -179.1(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.5312 6057 7077 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000
1.0000
2 0.4688 6088 7077 nmt -0.9978 -0.0046 -0.0022 -0.4660 0.3616 0.6410 -0.4598
1.3524 -0.3635
_oxdiff_twin_integration_method  simultaneous
_twin_special_details            
;
Component 2 rotated by -179.9244° 
 around [-0.00 0.71 0.70] (reciprocal) or [-0.30 0.86 0.41] (direct)
;
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: propionitrile/diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_80etcnht
_database_code_depnum_ccdc_archive 'CCDC 2078652'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2021-04-19 deposited with the CCDC.	2021-06-10 downloaded from the CCDC.
;
_audit_creation_date             2020-07-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis-[N-(2,6-di{pyrazol-1-yl}pyrid-4-yl)acetamide]iron(II)ditetrafluoroborate propionitrile solvate'
_chemical_formula_moiety         'C26 H24 Fe N12 O2, 2(B F4), C3 H5 N'
_chemical_formula_sum            'C29 H29 B2 F8 Fe N13 O2'
_chemical_formula_weight         821.12
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2454(3)
_cell_length_b                   12.6105(6)
_cell_length_c                   17.8210(9)
_cell_angle_alpha                84.191(4)
_cell_angle_beta                 80.215(4)
_cell_angle_gamma                81.291(4)
_cell_volume                     1799.57(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4631
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      73.26
_cell_measurement_theta_min      5.49
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.173
_exptl_absorpt_correction_T_max  0.700
_exptl_absorpt_correction_T_min  0.496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.939
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11551
_diffrn_reflns_point_group_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.885
_diffrn_reflns_theta_min         3.556
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9044
_reflns_number_total             11551
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2015)'
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         11551
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0581
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1089P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1573
_refine_ls_wR_factor_ref         0.1646
_refine_special_details          
;The data were resolved into two non-superimposable twin domains, in a 
 ratio of 0.51:0.49

 The C atoms of one pyrazole ring in the complex cation were modelled as 
 disordered over two half-occupied sites, to resolve an intermolecular
 steric clash. BF₄⁻ ion B47-F51 is disordered over two equally occupied 
 sites. The propionitrile molecule is also disordered over two equally 
 occupied orientations. The bond ldistance restraints that were applied 
 o the disordered residues are listed below. All crystallographically 
 ordered non-H atoms were refined anisotropically, and H atoms were placed 
 in calculated positions and refined using a riding model.,Twin
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.4877(12)
 0.5123(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N14-C15A = N14-C15B
 1.32 with sigma of 0.01
 C15A-C16A = C15B-C16B
 1.39 with sigma of 0.01
 C16A-C17A = C16B-C17B
 1.37 with sigma of 0.01
 N13-C17A = N13-C17B
 1.36 with sigma of 0.01
 B47A-F48A = B47A-F49A = B47A-F50A = B47A-F51A
 1.38708 with sigma of 0.02
 B47B-F48B = B47B-F49B = B47B-F50B = B47B-F51B
 1.38708 with sigma of 0.02
 F48A-F49A = F48A-F50A = F48A-F51A = F49A-F50A = F49A-F51A = F50A-F51A
 2.265102 with sigma of 0.02
 F48B-F49B = F48B-F50B = F48B-F51B = F49B-F50B = F49B-F51B = F50B-F51B
 2.265102 with sigma of 0.02
 C52A-C53A = C52B-C53B
 1.51 with sigma of 0.02
 C53A-C54A = C53B-C54B
 1.48 with sigma of 0.02
 C54A-N55A = C54B-N55B
 1.15 with sigma of 0.02
 C52A-C54A = C52B-C54B
 2.44 with sigma of 0.02
 C53A-N55A = C53B-N55B
 2.63 with sigma of 0.02
4. Others
 1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: C15A(0.5) H15A(0.5) C16A(0.5) H16A(0.5) C17A(0.5) H17A(0.5)
 C15B(0.5) H15B(0.5) C16B(0.5) H16B(0.5) C17B(0.5) H17B(0.5) B47A(0.5)
 F48A(0.5) F49A(0.5) F50A(0.5) F51A(0.5) B47B(0.5) F48B(0.5) F49B(0.5)
 F50B(0.5) F51B(0.5) C52A(0.5) H52A(0.5) H52B(0.5) H52C(0.5) C53A(0.5)
 H53A(0.5) H53B(0.5) C54A(0.5) N55A(0.5) C52B(0.5) H52D(0.5) H52E(0.5)
 H52F(0.5) C53B(0.5) H53C(0.5) H53D(0.5) C54B(0.5) N55B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C53A(H53A,H53B), C53B(H53C,H53D)
5.b Me refined with riding coordinates:
 C52A(H52A,H52B,H52C), C52B(H52D,H52E,H52F)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C15A(H15A), C16A(H16A),
 C17A(H17A), C15B(H15B), C16B(H16B), C17B(H17B), N18(H18), C24(H24), C26(H26),
 C30(H30), C31(H31), C32(H32), C35(H35), C36(H36), C37(H37), N38(H38)
5.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C41(H41A,H41B,H41C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.78135(7) 0.77253(4) 0.72582(3) 0.03412(16) Uani 1 1 d . . . . .
N2 N 0.8143(3) 0.6224(2) 0.67881(15) 0.0290(5) Uani 1 1 d . . . . .
C3 C 0.7904(4) 0.6152(2) 0.60759(18) 0.0282(6) Uani 1 1 d . . . . .
C4 C 0.8102(4) 0.5200(3) 0.57367(19) 0.0336(7) Uani 1 1 d . . . . .
H4 H 0.793016 0.518490 0.522431 0.040 Uiso 1 1 calc R U . . .
C5 C 0.8566(4) 0.4256(3) 0.6175(2) 0.0347(7) Uani 1 1 d . . . . .
C6 C 0.8813(4) 0.4310(3) 0.6931(2) 0.0362(7) Uani 1 1 d . . . . .
H6 H 0.911913 0.368115 0.724489 0.043 Uiso 1 1 calc R U . . .
C7 C 0.8591(4) 0.5311(3) 0.71904(18) 0.0318(7) Uani 1 1 d . . . . .
N8 N 0.7379(4) 0.7162(2) 0.57101(16) 0.0334(6) Uani 1 1 d . . . . .
N9 N 0.7254(4) 0.8057(2) 0.60987(17) 0.0375(6) Uani 1 1 d . . . . .
C10 C 0.6659(5) 0.8859(3) 0.5633(2) 0.0478(9) Uani 1 1 d . . . . .
H10 H 0.643412 0.959072 0.574907 0.057 Uiso 1 1 calc R U . . .
C11 C 0.6407(6) 0.8497(3) 0.4958(2) 0.0528(10) Uani 1 1 d . . . . .
H11 H 0.599645 0.891793 0.453946 0.063 Uiso 1 1 calc R U . . .
C12 C 0.6870(5) 0.7416(3) 0.5020(2) 0.0455(9) Uani 1 1 d . . . . .
H12 H 0.684359 0.692823 0.465048 0.055 Uiso 1 1 calc R U . . .
N13 N 0.8775(4) 0.5495(2) 0.79398(16) 0.0381(6) Uani 1 1 d D . . . .
N14 N 0.8515(4) 0.6524(3) 0.81420(16) 0.0396(7) Uani 1 1 d D . . . .
C15A C 0.8545(10) 0.6590(7) 0.8867(4) 0.0328(18) Uiso 0.5 1 d D . P A 1
H15A H 0.840961 0.722470 0.912985 0.039 Uiso 0.5 1 calc R U P A 1
C16A C 0.8824(11) 0.5511(7) 0.9175(4) 0.0398(18) Uiso 0.5 1 d D . P A 1
H16A H 0.893411 0.527837 0.968991 0.048 Uiso 0.5 1 calc R U P A 1
C17A C 0.8907(11) 0.4860(6) 0.8590(4) 0.0349(18) Uiso 0.5 1 d D . P A 1
H17A H 0.903501 0.409591 0.863654 0.042 Uiso 0.5 1 calc R U P A 1
C15B C 0.8762(12) 0.6287(8) 0.8880(5) 0.046(2) Uiso 0.5 1 d D . P A 2
H15B H 0.865082 0.683190 0.922402 0.055 Uiso 0.5 1 calc R U P A 2
C16B C 0.9182(16) 0.5209(8) 0.9104(6) 0.068(3) Uiso 0.5 1 d D . P A 2
H16B H 0.935713 0.490411 0.959797 0.082 Uiso 0.5 1 calc R U P A 2
C17B C 0.9292(14) 0.4683(8) 0.8466(5) 0.056(3) Uiso 0.5 1 d D . P A 2
H17B H 0.963687 0.394041 0.839788 0.067 Uiso 0.5 1 calc R U P A 2
N18 N 0.8722(4) 0.3302(2) 0.58298(19) 0.0434(7) Uani 1 1 d . . . . .
H18 H 0.849855 0.335675 0.536070 0.052 Uiso 1 1 calc R U . . .
C19 C 0.9190(5) 0.2270(3) 0.6139(3) 0.0508(10) Uani 1 1 d . . . . .
O20 O 0.9599(6) 0.2083(2) 0.6754(2) 0.0798(11) Uani 1 1 d . . . . .
C21 C 0.9130(7) 0.1415(3) 0.5613(3) 0.0662(13) Uani 1 1 d . . . . .
H21A H 0.967157 0.072163 0.581062 0.099 Uiso 1 1 calc R U . . .
H21B H 0.971034 0.160940 0.510175 0.099 Uiso 1 1 calc R U . . .
H21C H 0.797027 0.135818 0.558408 0.099 Uiso 1 1 calc R U . . .
N22 N 0.7122(4) 0.9035(2) 0.79578(16) 0.0336(6) Uani 1 1 d . . . . .
C23 C 0.5615(4) 0.9195(3) 0.83778(19) 0.0341(7) Uani 1 1 d . . . . .
C24 C 0.5084(5) 1.0047(3) 0.8820(2) 0.0397(8) Uani 1 1 d . . . . .
H24 H 0.400549 1.013162 0.911512 0.048 Uiso 1 1 calc R U . . .
C25 C 0.6185(5) 1.0784(3) 0.8820(2) 0.0402(8) Uani 1 1 d . . . . .
C26 C 0.7779(5) 1.0630(3) 0.8397(2) 0.0387(8) Uani 1 1 d . . . . .
H26 H 0.855945 1.111235 0.839772 0.046 Uiso 1 1 calc R U . . .
C27 C 0.8154(4) 0.9741(3) 0.79800(19) 0.0325(7) Uani 1 1 d . . . . .
N28 N 0.4633(4) 0.8402(2) 0.83121(17) 0.0377(6) Uani 1 1 d . . . . .
N29 N 0.5220(4) 0.7662(3) 0.77896(18) 0.0411(7) Uani 1 1 d . . . . .
C30 C 0.4057(5) 0.7023(3) 0.7863(2) 0.0507(9) Uani 1 1 d . . . . .
H30 H 0.411578 0.643107 0.756509 0.061 Uiso 1 1 calc R U . . .
C31 C 0.2736(6) 0.7330(4) 0.8432(3) 0.0583(11) Uani 1 1 d . . . . .
H31 H 0.176887 0.699109 0.859392 0.070 Uiso 1 1 calc R U . . .
C32 C 0.3110(5) 0.8212(4) 0.8709(2) 0.0519(10) Uani 1 1 d . . . . .
H32 H 0.245004 0.861750 0.909962 0.062 Uiso 1 1 calc R U . . .
N33 N 0.9715(3) 0.9480(2) 0.75192(16) 0.0343(6) Uani 1 1 d . . . . .
N34 N 0.9907(4) 0.8633(2) 0.70790(18) 0.0402(7) Uani 1 1 d . . . . .
C35 C 1.1455(5) 0.8592(3) 0.6707(2) 0.0450(9) Uani 1 1 d . . . . .
H35 H 1.195064 0.807902 0.635091 0.054 Uiso 1 1 calc R U . . .
C36 C 1.2257(5) 0.9394(3) 0.6903(2) 0.0466(9) Uani 1 1 d . . . . .
H36 H 1.336314 0.952774 0.671610 0.056 Uiso 1 1 calc R U . . .
C37 C 1.1108(5) 0.9950(3) 0.7423(2) 0.0433(8) Uani 1 1 d . . . . .
H37 H 1.126374 1.055254 0.766912 0.052 Uiso 1 1 calc R U . . .
N38 N 0.5625(4) 1.1668(3) 0.92504(19) 0.0492(8) Uani 1 1 d . . . . .
H38 H 0.482593 1.159105 0.963916 0.059 Uiso 1 1 calc R U . . .
C39 C 0.6201(6) 1.2646(3) 0.9127(3) 0.0576(11) Uani 1 1 d . . . . .
O40 O 0.7331(5) 1.2831(3) 0.8617(2) 0.0784(11) Uani 1 1 d . . . . .
C41 C 0.5272(8) 1.3467(4) 0.9652(3) 0.0793(16) Uani 1 1 d . . . . .
H41A H 0.605509 1.389019 0.979932 0.119 Uiso 1 1 calc R U . . .
H41B H 0.469778 1.310230 1.011007 0.119 Uiso 1 1 calc R U . . .
H41C H 0.445673 1.394534 0.939045 0.119 Uiso 1 1 calc R U . . .
B42 B 0.7212(6) 0.4254(4) 0.3834(3) 0.0489(11) Uani 1 1 d . . . . .
F43 F 0.7201(5) 0.5281(2) 0.40423(17) 0.0897(11) Uani 1 1 d . . . . .
F44 F 0.5699(5) 0.3997(4) 0.3867(3) 0.1174(16) Uani 1 1 d . . . . .
F45 F 0.8016(4) 0.4167(3) 0.30919(15) 0.0733(8) Uani 1 1 d . . . . .
F46 F 0.8177(5) 0.3552(3) 0.42931(18) 0.0905(11) Uani 1 1 d . . . . .
B47A B 0.1020(16) 1.1714(11) 0.9624(7) 0.055(5) Uiso 0.5 1 d D . P B 1
F48A F 0.1278(7) 1.1502(5) 0.8855(3) 0.0591(16) Uiso 0.5 1 d D . P B 1
F49A F -0.0467(10) 1.1536(7) 0.9993(5) 0.102(2) Uiso 0.5 1 d D . P B 1
F50A F 0.0826(12) 1.2898(7) 0.9491(5) 0.104(3) Uiso 0.5 1 d D . P B 1
F51A F 0.2381(10) 1.1531(6) 1.0011(4) 0.059(2) Uiso 0.5 1 d D . P B 1
B47B B 0.1070(13) 1.1922(10) 0.9541(6) 0.040(3) Uiso 0.5 1 d D . P C 2
F48B F 0.1296(7) 1.1153(5) 0.9009(3) 0.0523(14) Uiso 0.5 1 d D . P C 2
F49B F -0.0425(8) 1.2128(6) 0.9950(4) 0.0777(17) Uiso 0.5 1 d D . P C 2
F50B F 0.1622(9) 1.2894(5) 0.9286(4) 0.0718(16) Uiso 0.5 1 d D . P C 2
F51B F 0.2177(10) 1.1346(6) 1.0051(4) 0.058(2) Uiso 0.5 1 d D . P C 2
C52A C 0.5505(18) 0.6427(10) 0.2521(8) 0.092(4) Uiso 0.5 1 d D . P D 1
H52A H 0.618634 0.580529 0.228549 0.139 Uiso 0.5 1 calc R U P D 1
H52B H 0.493835 0.619467 0.302670 0.139 Uiso 0.5 1 calc R U P D 1
H52C H 0.467784 0.674666 0.219898 0.139 Uiso 0.5 1 calc R U P D 1
C53A C 0.6598(15) 0.7248(9) 0.2602(7) 0.076(3) Uiso 0.5 1 d D . P D 1
H53A H 0.744339 0.692633 0.292298 0.091 Uiso 0.5 1 calc R U P D 1
H53B H 0.718229 0.747957 0.209339 0.091 Uiso 0.5 1 calc R U P D 1
C54A C 0.5586(15) 0.8179(8) 0.2954(6) 0.063(3) Uiso 0.5 1 d D . P D 1
N55A N 0.485(2) 0.8875(12) 0.3232(10) 0.085(5) Uiso 0.5 1 d D . P D 1
C52B C 0.6750(15) 0.6795(11) 0.2391(7) 0.084(3) Uiso 0.5 1 d D . P E 2
H52D H 0.690683 0.605165 0.224872 0.126 Uiso 0.5 1 calc R U P E 2
H52E H 0.679476 0.728883 0.192931 0.126 Uiso 0.5 1 calc R U P E 2
H52F H 0.763059 0.689143 0.267441 0.126 Uiso 0.5 1 calc R U P E 2
C53B C 0.5072(13) 0.7032(7) 0.2890(6) 0.063(2) Uiso 0.5 1 d D . P E 2
H53C H 0.418317 0.692304 0.260707 0.076 Uiso 0.5 1 calc R U P E 2
H53D H 0.501999 0.652517 0.335306 0.076 Uiso 0.5 1 calc R U P E 2
C54B C 0.4795(13) 0.8130(7) 0.3113(5) 0.053(2) Uiso 0.5 1 d D . P E 2
N55B N 0.4526(19) 0.9011(10) 0.3284(8) 0.066(4) Uiso 0.5 1 d D . P E 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.109(3) . ?
Fe1 N9 2.179(3) . ?
Fe1 N14 2.161(3) . ?
Fe1 N22 2.121(3) . ?
Fe1 N29 2.197(3) . ?
Fe1 N34 2.175(3) . ?
N2 C3 1.331(4) . ?
N2 C7 1.330(4) . ?
C3 C4 1.374(4) . ?
C3 N8 1.412(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.397(5) . ?
C5 C6 1.406(5) . ?
C5 N18 1.386(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.365(5) . ?
C7 N13 1.415(4) . ?
N8 N9 1.365(4) . ?
N8 C12 1.359(4) . ?
N9 C10 1.331(5) . ?
C10 H10 0.9500 . ?
C10 C11 1.387(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.358(5) . ?
C12 H12 0.9500 . ?
N13 N14 1.358(4) . ?
N13 C17A 1.351(7) . ?
N13 C17B 1.386(9) . ?
N14 C15A 1.308(7) . ?
N14 C15B 1.362(8) . ?
C15A H15A 0.9500 . ?
C15A C16A 1.416(9) . ?
C16A H16A 0.9500 . ?
C16A C17A 1.377(9) . ?
C17A H17A 0.9500 . ?
C15B H15B 0.9500 . ?
C15B C16B 1.386(10) . ?
C16B H16B 0.9500 . ?
C16B C17B 1.356(10) . ?
C17B H17B 0.9500 . ?
N18 H18 0.8800 . ?
N18 C19 1.386(5) . ?
C19 O20 1.190(6) . ?
C19 C21 1.511(6) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
N22 C23 1.336(4) . ?
N22 C27 1.329(4) . ?
C23 C24 1.370(5) . ?
C23 N28 1.404(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.394(5) . ?
C25 C26 1.396(5) . ?
C25 N38 1.393(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.375(4) . ?
C27 N33 1.416(4) . ?
N28 N29 1.363(4) . ?
N28 C32 1.375(5) . ?
N29 C30 1.325(5) . ?
C30 H30 0.9500 . ?
C30 C31 1.393(6) . ?
C31 H31 0.9500 . ?
C31 C32 1.356(6) . ?
C32 H32 0.9500 . ?
N33 N34 1.363(4) . ?
N33 C37 1.349(5) . ?
N34 C35 1.331(5) . ?
C35 H35 0.9500 . ?
C35 C36 1.391(6) . ?
C36 H36 0.9500 . ?
C36 C37 1.372(5) . ?
C37 H37 0.9500 . ?
N38 H38 0.8800 . ?
N38 C39 1.372(6) . ?
C39 O40 1.218(6) . ?
C39 C41 1.499(6) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
B42 F43 1.381(5) . ?
B42 F44 1.326(6) . ?
B42 F45 1.382(6) . ?
B42 F46 1.396(6) . ?
B47A F48A 1.399(13) . ?
B47A F49A 1.329(14) . ?
B47A F50A 1.476(15) . ?
B47A F51A 1.392(14) . ?
B47B F48B 1.395(11) . ?
B47B F49B 1.325(12) . ?
B47B F50B 1.378(13) . ?
B47B F51B 1.461(13) . ?
C52A H52A 0.9800 . ?
C52A H52B 0.9800 . ?
C52A H52C 0.9800 . ?
C52A C53A 1.504(14) . ?
C53A H53A 0.9900 . ?
C53A H53B 0.9900 . ?
C53A C54A 1.464(13) . ?
C54A N55A 1.098(14) . ?
C52B H52D 0.9800 . ?
C52B H52E 0.9800 . ?
C52B H52F 0.9800 . ?
C52B C53B 1.518(13) . ?
C53B H53C 0.9900 . ?
C53B H53D 0.9900 . ?
C53B C54B 1.454(11) . ?
C54B N55B 1.160(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N9 73.64(10) . . ?
N2 Fe1 N14 73.50(10) . . ?
N2 Fe1 N22 165.76(11) . . ?
N2 Fe1 N29 95.44(11) . . ?
N2 Fe1 N34 118.30(11) . . ?
N9 Fe1 N29 94.79(12) . . ?
N14 Fe1 N9 147.12(11) . . ?
N14 Fe1 N29 87.33(12) . . ?
N14 Fe1 N34 100.67(12) . . ?
N22 Fe1 N9 115.16(11) . . ?
N22 Fe1 N14 96.91(11) . . ?
N22 Fe1 N29 73.24(11) . . ?
N22 Fe1 N34 73.25(11) . . ?
N34 Fe1 N9 95.61(12) . . ?
N34 Fe1 N29 146.24(11) . . ?
C3 N2 Fe1 121.2(2) . . ?
C7 N2 Fe1 121.5(2) . . ?
C7 N2 C3 117.3(3) . . ?
N2 C3 C4 124.0(3) . . ?
N2 C3 N8 112.6(3) . . ?
C4 C3 N8 123.4(3) . . ?
C3 C4 H4 121.3 . . ?
C3 C4 C5 117.3(3) . . ?
C5 C4 H4 121.3 . . ?
C4 C5 C6 119.8(3) . . ?
N18 C5 C4 116.5(3) . . ?
N18 C5 C6 123.7(3) . . ?
C5 C6 H6 121.7 . . ?
C7 C6 C5 116.5(3) . . ?
C7 C6 H6 121.7 . . ?
N2 C7 C6 125.0(3) . . ?
N2 C7 N13 111.8(3) . . ?
C6 C7 N13 123.2(3) . . ?
N9 N8 C3 118.2(3) . . ?
C12 N8 C3 130.5(3) . . ?
C12 N8 N9 111.2(3) . . ?
N8 N9 Fe1 114.3(2) . . ?
C10 N9 Fe1 141.0(3) . . ?
C10 N9 N8 104.4(3) . . ?
N9 C10 H10 124.1 . . ?
N9 C10 C11 111.8(3) . . ?
C11 C10 H10 124.1 . . ?
C10 C11 H11 127.2 . . ?
C12 C11 C10 105.5(3) . . ?
C12 C11 H11 127.2 . . ?
N8 C12 H12 126.4 . . ?
C11 C12 N8 107.1(3) . . ?
C11 C12 H12 126.4 . . ?
N14 N13 C7 118.5(3) . . ?
N14 N13 C17B 118.1(5) . . ?
C17A N13 C7 134.5(4) . . ?
C17A N13 N14 106.1(4) . . ?
C17B N13 C7 123.3(5) . . ?
N13 N14 Fe1 114.76(19) . . ?
N13 N14 C15B 96.8(5) . . ?
C15A N14 Fe1 131.5(4) . . ?
C15A N14 N13 113.2(4) . . ?
C15B N14 Fe1 148.3(5) . . ?
N14 C15A H15A 127.5 . . ?
N14 C15A C16A 105.0(6) . . ?
C16A C15A H15A 127.5 . . ?
C15A C16A H16A 126.3 . . ?
C17A C16A C15A 107.4(7) . . ?
C17A C16A H16A 126.3 . . ?
N13 C17A C16A 108.3(6) . . ?
N13 C17A H17A 125.9 . . ?
C16A C17A H17A 125.9 . . ?
N14 C15B H15B 121.8 . . ?
N14 C15B C16B 116.5(8) . . ?
C16B C15B H15B 121.8 . . ?
C15B C16B H16B 127.3 . . ?
C17B C16B C15B 105.3(9) . . ?
C17B C16B H16B 127.3 . . ?
N13 C17B H17B 128.6 . . ?
C16B C17B N13 102.8(8) . . ?
C16B C17B H17B 128.6 . . ?
C5 N18 H18 116.3 . . ?
C19 N18 C5 127.4(3) . . ?
C19 N18 H18 116.3 . . ?
N18 C19 C21 112.8(4) . . ?
O20 C19 N18 123.3(4) . . ?
O20 C19 C21 123.9(4) . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 N22 Fe1 121.1(2) . . ?
C27 N22 Fe1 121.3(2) . . ?
C27 N22 C23 117.6(3) . . ?
N22 C23 C24 123.5(3) . . ?
N22 C23 N28 112.7(3) . . ?
C24 C23 N28 123.8(3) . . ?
C23 C24 H24 121.2 . . ?
C23 C24 C25 117.5(3) . . ?
C25 C24 H24 121.2 . . ?
C24 C25 C26 120.4(3) . . ?
N38 C25 C24 117.5(3) . . ?
N38 C25 C26 122.1(3) . . ?
C25 C26 H26 121.9 . . ?
C27 C26 C25 116.2(3) . . ?
C27 C26 H26 121.9 . . ?
N22 C27 C26 124.8(3) . . ?
N22 C27 N33 112.3(3) . . ?
C26 C27 N33 122.9(3) . . ?
N29 N28 C23 118.6(3) . . ?
N29 N28 C32 110.9(3) . . ?
C32 N28 C23 130.4(3) . . ?
N28 N29 Fe1 113.8(2) . . ?
C30 N29 Fe1 140.1(3) . . ?
C30 N29 N28 105.0(3) . . ?
N29 C30 H30 124.3 . . ?
N29 C30 C31 111.4(4) . . ?
C31 C30 H30 124.3 . . ?
C30 C31 H31 126.9 . . ?
C32 C31 C30 106.1(4) . . ?
C32 C31 H31 126.9 . . ?
N28 C32 H32 126.8 . . ?
C31 C32 N28 106.5(4) . . ?
C31 C32 H32 126.8 . . ?
N34 N33 C27 118.0(3) . . ?
C37 N33 C27 130.5(3) . . ?
C37 N33 N34 111.5(3) . . ?
N33 N34 Fe1 114.8(2) . . ?
C35 N34 Fe1 140.3(3) . . ?
C35 N34 N33 104.6(3) . . ?
N34 C35 H35 124.2 . . ?
N34 C35 C36 111.6(3) . . ?
C36 C35 H35 124.2 . . ?
C35 C36 H36 127.4 . . ?
C37 C36 C35 105.2(3) . . ?
C37 C36 H36 127.4 . . ?
N33 C37 C36 107.1(3) . . ?
N33 C37 H37 126.5 . . ?
C36 C37 H37 126.5 . . ?
C25 N38 H38 116.8 . . ?
C39 N38 C25 126.3(4) . . ?
C39 N38 H38 116.8 . . ?
N38 C39 C41 114.0(4) . . ?
O40 C39 N38 122.3(4) . . ?
O40 C39 C41 123.6(4) . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
F43 B42 F45 109.7(4) . . ?
F43 B42 F46 107.2(3) . . ?
F44 B42 F43 112.9(5) . . ?
F44 B42 F45 107.5(4) . . ?
F44 B42 F46 113.2(5) . . ?
F45 B42 F46 106.2(4) . . ?
F48A B47A F50A 96.2(9) . . ?
F49A B47A F48A 113.3(10) . . ?
F49A B47A F50A 102.7(10) . . ?
F49A B47A F51A 119.7(11) . . ?
F51A B47A F48A 118.2(10) . . ?
F51A B47A F50A 100.7(10) . . ?
F48B B47B F51B 97.9(8) . . ?
F49B B47B F48B 117.7(9) . . ?
F49B B47B F50B 107.7(9) . . ?
F49B B47B F51B 107.7(9) . . ?
F50B B47B F48B 116.7(9) . . ?
F50B B47B F51B 108.0(8) . . ?
H52A C52A H52B 109.5 . . ?
H52A C52A H52C 109.5 . . ?
H52B C52A H52C 109.5 . . ?
C53A C52A H52A 109.5 . . ?
C53A C52A H52B 109.5 . . ?
C53A C52A H52C 109.5 . . ?
C52A C53A H53A 109.7 . . ?
C52A C53A H53B 109.7 . . ?
H53A C53A H53B 108.2 . . ?
C54A C53A C52A 109.7(10) . . ?
C54A C53A H53A 109.7 . . ?
C54A C53A H53B 109.7 . . ?
N55A C54A C53A 178.2(15) . . ?
H52D C52B H52E 109.5 . . ?
H52D C52B H52F 109.5 . . ?
H52E C52B H52F 109.5 . . ?
C53B C52B H52D 109.5 . . ?
C53B C52B H52E 109.5 . . ?
C53B C52B H52F 109.5 . . ?
C52B C53B H53C 109.4 . . ?
C52B C53B H53D 109.4 . . ?
H53C C53B H53D 108.0 . . ?
C54B C53B C52B 111.0(9) . . ?
C54B C53B H53C 109.4 . . ?
C54B C53B H53D 109.4 . . ?
N55B C54B C53B 177.8(12) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N18 H18 F46 0.88 1.95 2.829(4) 174.7 . yes
N38 H38 F51A 0.88 2.02 2.808(9) 148.0 . yes
N38 H38 F51B 0.88 2.24 3.023(9) 148.1 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N2 C3 C4 179.8(3) . . . . ?
Fe1 N2 C3 N8 -1.7(4) . . . . ?
Fe1 N2 C7 C6 179.3(3) . . . . ?
Fe1 N2 C7 N13 0.9(4) . . . . ?
Fe1 N9 C10 C11 -172.0(3) . . . . ?
Fe1 N14 C15A C16A 169.7(4) . . . . ?
Fe1 N14 C15B C16B 176.3(7) . . . . ?
Fe1 N22 C23 C24 -177.8(3) . . . . ?
Fe1 N22 C23 N28 1.8(4) . . . . ?
Fe1 N22 C27 C26 177.6(3) . . . . ?
Fe1 N22 C27 N33 -2.3(4) . . . . ?
Fe1 N29 C30 C31 165.9(3) . . . . ?
Fe1 N34 C35 C36 -172.8(3) . . . . ?
N2 C3 C4 C5 0.7(5) . . . . ?
N2 C3 N8 N9 2.7(4) . . . . ?
N2 C3 N8 C12 -173.4(4) . . . . ?
N2 C7 N13 N14 -1.1(4) . . . . ?
N2 C7 N13 C17A 165.9(6) . . . . ?
N2 C7 N13 C17B -177.6(6) . . . . ?
C3 N2 C7 C6 -0.4(5) . . . . ?
C3 N2 C7 N13 -178.9(3) . . . . ?
C3 C4 C5 C6 -0.1(5) . . . . ?
C3 C4 C5 N18 178.5(3) . . . . ?
C3 N8 N9 Fe1 -2.4(4) . . . . ?
C3 N8 N9 C10 -176.8(3) . . . . ?
C3 N8 C12 C11 176.4(4) . . . . ?
C4 C3 N8 N9 -178.9(3) . . . . ?
C4 C3 N8 C12 5.0(6) . . . . ?
C4 C5 C6 C7 -0.6(5) . . . . ?
C4 C5 N18 C19 178.9(4) . . . . ?
C5 C6 C7 N2 0.9(5) . . . . ?
C5 C6 C7 N13 179.2(3) . . . . ?
C5 N18 C19 O20 -3.5(8) . . . . ?
C5 N18 C19 C21 176.7(4) . . . . ?
C6 C5 N18 C19 -2.5(6) . . . . ?
C6 C7 N13 N14 -179.6(3) . . . . ?
C6 C7 N13 C17A -12.6(8) . . . . ?
C6 C7 N13 C17B 3.9(8) . . . . ?
C7 N2 C3 C4 -0.4(5) . . . . ?
C7 N2 C3 N8 178.0(3) . . . . ?
C7 N13 N14 Fe1 0.9(4) . . . . ?
C7 N13 N14 C15A 173.2(5) . . . . ?
C7 N13 N14 C15B 177.8(5) . . . . ?
C7 N13 C17A C16A -171.6(5) . . . . ?
C7 N13 C17B C16B -176.2(7) . . . . ?
N8 C3 C4 C5 -177.6(3) . . . . ?
N8 N9 C10 C11 -0.2(5) . . . . ?
N9 N8 C12 C11 0.1(5) . . . . ?
N9 C10 C11 C12 0.2(5) . . . . ?
C10 C11 C12 N8 -0.2(5) . . . . ?
C12 N8 N9 Fe1 174.4(3) . . . . ?
C12 N8 N9 C10 0.1(4) . . . . ?
N13 N14 C15A C16A -0.9(8) . . . . ?
N13 N14 C15B C16B 1.7(10) . . . . ?
N14 N13 C17A C16A -3.5(8) . . . . ?
N14 N13 C17B C16B 7.3(11) . . . . ?
N14 C15A C16A C17A -1.3(9) . . . . ?
N14 C15B C16B C17B 2.4(13) . . . . ?
C15A C16A C17A N13 3.0(9) . . . . ?
C17A N13 N14 Fe1 -169.5(4) . . . . ?
C17A N13 N14 C15A 2.8(6) . . . . ?
C15B C16B C17B N13 -5.2(12) . . . . ?
C17B N13 N14 Fe1 177.5(6) . . . . ?
C17B N13 N14 C15B -5.5(8) . . . . ?
N18 C5 C6 C7 -179.2(3) . . . . ?
N22 C23 C24 C25 0.6(5) . . . . ?
N22 C23 N28 N29 -7.0(5) . . . . ?
N22 C23 N28 C32 171.9(4) . . . . ?
N22 C27 N33 N34 5.4(4) . . . . ?
N22 C27 N33 C37 -175.8(3) . . . . ?
C23 N22 C27 C26 -0.7(5) . . . . ?
C23 N22 C27 N33 179.4(3) . . . . ?
C23 C24 C25 C26 -1.7(5) . . . . ?
C23 C24 C25 N38 178.0(3) . . . . ?
C23 N28 N29 Fe1 8.6(4) . . . . ?
C23 N28 N29 C30 179.4(3) . . . . ?
C23 N28 C32 C31 -178.6(4) . . . . ?
C24 C23 N28 N29 172.6(3) . . . . ?
C24 C23 N28 C32 -8.6(6) . . . . ?
C24 C25 C26 C27 1.5(5) . . . . ?
C24 C25 N38 C39 -154.7(4) . . . . ?
C25 C26 C27 N22 -0.3(5) . . . . ?
C25 C26 C27 N33 179.6(3) . . . . ?
C25 N38 C39 O40 -1.8(8) . . . . ?
C25 N38 C39 C41 175.8(4) . . . . ?
C26 C25 N38 C39 25.0(6) . . . . ?
C26 C27 N33 N34 -174.5(3) . . . . ?
C26 C27 N33 C37 4.3(6) . . . . ?
C27 N22 C23 C24 0.6(5) . . . . ?
C27 N22 C23 N28 -179.9(3) . . . . ?
C27 N33 N34 Fe1 -6.0(4) . . . . ?
C27 N33 N34 C35 178.9(3) . . . . ?
C27 N33 C37 C36 -178.9(3) . . . . ?
N28 C23 C24 C25 -178.9(3) . . . . ?
N28 N29 C30 C31 -0.8(5) . . . . ?
N29 N28 C32 C31 0.3(5) . . . . ?
N29 C30 C31 C32 1.0(6) . . . . ?
C30 C31 C32 N28 -0.8(5) . . . . ?
C32 N28 N29 Fe1 -170.4(3) . . . . ?
C32 N28 N29 C30 0.3(4) . . . . ?
N33 N34 C35 C36 0.2(4) . . . . ?
N34 N33 C37 C36 -0.1(4) . . . . ?
N34 C35 C36 C37 -0.3(5) . . . . ?
C35 C36 C37 N33 0.2(4) . . . . ?
C37 N33 N34 Fe1 175.0(2) . . . . ?
C37 N33 N34 C35 -0.1(4) . . . . ?
N38 C25 C26 C27 -178.2(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.4866 8726 5598 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000
1.0000
2 0.5134 8744 5598 nmt -1.0000 0.0003 -0.0002 -0.5507 0.3583 0.6426 -0.5489
1.3564 -0.3584
_oxdiff_twin_integration_method  simultaneous
_twin_special_details            
;
Component 2 rotated by -179.9836° 
 around [0.00 0.71 0.71] (reciprocal) or [-0.34 0.85 0.40] (direct)
;
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: propionitrile/diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_etcnmaht
_database_code_depnum_ccdc_archive 'CCDC 2078658'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2021-04-19 deposited with the CCDC.	2021-06-10 downloaded from the CCDC.
;
_audit_creation_date             2020-07-21
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis-[N-(2,6-di{pyrazol-1-yl}pyrid-4-yl)acetamide]iron(II)tetrafluoroborate(2/0.9) perchlorate(2/1.1) propionitrile solvate'
_chemical_formula_moiety         
'C26 H24 Fe N12 O2, 0.9(B F4), 1.1(Cl O4), C3 H5 N'
_chemical_formula_sum            'C29 H29 B0.90 Cl1.10 F3.60 Fe N13 O6.40'
_chemical_formula_weight         835.02
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2960(2)
_cell_length_b                   12.6295(5)
_cell_length_c                   18.0010(7)
_cell_angle_alpha                84.076(3)
_cell_angle_beta                 80.160(3)
_cell_angle_gamma                81.045(3)
_cell_volume                     1829.95(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7445
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      73.12
_cell_measurement_theta_min      4.17
_exptl_absorpt_coefficient_mu    4.756
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             854
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.947
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14861
_diffrn_reflns_point_group_measured_fraction_full 0.947
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.703
_diffrn_reflns_theta_min         3.554
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      250(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5901
_reflns_number_total             6892
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2015)'
_refine_diff_density_max         0.788
_refine_diff_density_min         -1.376
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         6892
_refine_ls_number_restraints     83
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0727
_refine_ls_restrained_S_all      1.120
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1154P)²+2.1637P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2001
_refine_ls_wR_factor_ref         0.2078
_refine_special_details          
;
 Separate partial BF₄⁻ and ClO₄⁻ ions were modelled on each anion 
 site. The BF₄⁻:ClO₄⁻ occupancy ratio for one anion refined to 
 0.49:0.51, while the other anion refined to 0.42:0.58; the latter was 
 actually refined as 0.41:0.59, for consistency with the lower temperature
 refinements from the same crystal. The F atoms of the latter BF₄⁻ 
 anion population are in turn disordered over two 0.2-occupied sites. The 
 C atoms of one pyrazole ring in the complex cation were modelled as 
 disordered over two half-occupied sites, to resolve an intermolecular
 steric clash. The bond distance restraints that were applied to the
 disordered residues are listed below. 

 All crystallographically ordered non-H atoms were refined anisotropically, 
 and H atoms were placed in calculated positions and refined using a riding 
 model. The deepest Fourier hole of -1.4 e.Å⁻³ is associated with the
 partial anion Cl47-O51.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N14-C15A = N14-C15B
 1.32 with sigma of 0.01
 C15A-C16A = C15B-C16B
 1.39 with sigma of 0.01
 C16A-C17A = C16B-C17B
 1.37 with sigma of 0.01
 N13-C17A = N13-C17B
 1.36 with sigma of 0.01
 B42-F43 = B42-F44 = B42-F45 = B42-F46
 1.37 with sigma of 0.02
 B47-F48A = B47-F49A = B47-F50A = B47-F51A
 1.37 with sigma of 0.02
 B47-F48B = B47-F49B = B47-F50B = B47-F51B
 1.37 with sigma of 0.02
 F43-F44 = F43-F45 = F43-F46 = F44-F45 = F44-F46 = F45-F46
 2.24 with sigma of 0.02
 F48A-F49A = F48A-F50A = F48A-F51A = F49A-F50A = F49A-F51A = F50A-F51A
 2.24 with sigma of 0.02
 F48B-F49B = F48B-F50B = F48B-F51B = F49B-F50B = F49B-F51B = F50B-F51B
 2.24 with sigma of 0.02
 Cl42-O43 = Cl42-O44 = Cl42-O45 = Cl42-O46
 1.45 with sigma of 0.02
 Cl47-O48 = Cl47-O49 = Cl47-O50 = Cl47-O51
 1.45 with sigma of 0.02
 O43-O44 = O43-O45 = O43-O46 = O44-O45 = O44-O46 = O45-O46
 2.37 with sigma of 0.02
 O48-O49 = O48-O50 = O48-O51 = O49-O50 = O49-O51 = O50-O51
 2.37 with sigma of 0.02
 C52A-C53A = C52B-C53B
 1.51 with sigma of 0.02
 C53A-C54A = C53B-C54B
 1.48 with sigma of 0.02
 C54A-N55A = C54B-N55B
 1.15 with sigma of 0.02
 C52A-C54A = C52B-C54B
 2.44 with sigma of 0.02
 C53A-N55A = C53B-N55B
 2.63 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
B47 \\sim F48A \\sim F49A \\sim F50A \\sim F51A \\sim F48B \\sim F49B \\sim
F50B \\sim F51B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.002 within 2A
4. Others
 Fixed Sof: C15A(0.5) H15A(0.5) C16A(0.5) H16A(0.5) C17A(0.5) H17A(0.5)
 C15B(0.5) H15B(0.5) C16B(0.5) H16B(0.5) C17B(0.5) H17B(0.5) B42(0.49)
 F43(0.49) F44(0.49) F45(0.49) F46(0.49) Cl42(0.51) O43(0.51) O44(0.51)
 O45(0.51) O46(0.51) B47(0.41) F48A(0.21) F49A(0.21) F50A(0.21) F51A(0.21)
 F48B(0.2) F49B(0.2) F50B(0.2) F51B(0.2) Cl47(0.59) O48(0.59) O49(0.59)
 O50(0.59) O51(0.59) C53A(0.5) H53A(0.5) H53B(0.5) C52A(0.5) H52A(0.5)
 H52B(0.5) H52C(0.5) C54A(0.5) N55A(0.5) C52B(0.5) H52D(0.5) H52E(0.5)
 H52F(0.5) C53B(0.5) H53C(0.5) H53D(0.5) C54B(0.5) N55B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C53A(H53A,H53B), C53B(H53C,H53D)
5.b Me refined with riding coordinates:
 C52A(H52A,H52B,H52C), C52B(H52D,H52E,H52F)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C15A(H15A), C16A(H16A),
 C17A(H17A), C15B(H15B), C16B(H16B), C17B(H17B), N18(H18), C24(H24), C26(H26),
 C30(H30), C31(H31), C32(H32), C35(H35), C36(H36), C37(H37), N38(H38)
5.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C41(H41A,H41B,H41C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.78103(7) 0.77382(4) 0.72545(3) 0.0369(2) Uani 1 1 d . . . . .
N2 N 0.8131(4) 0.6233(2) 0.67866(16) 0.0313(6) Uani 1 1 d . . . . .
C3 C 0.7883(4) 0.6160(3) 0.60815(19) 0.0317(7) Uani 1 1 d . . . . .
C4 C 0.8086(5) 0.5220(3) 0.5748(2) 0.0369(8) Uani 1 1 d . . . . .
H4 H 0.792676 0.520767 0.524432 0.044 Uiso 1 1 calc R U . . .
C5 C 0.8543(5) 0.4270(3) 0.6183(2) 0.0382(8) Uani 1 1 d . . . . .
C6 C 0.8788(5) 0.4319(3) 0.6925(2) 0.0389(8) Uani 1 1 d . . . . .
H6 H 0.908162 0.369460 0.723248 0.047 Uiso 1 1 calc R U . . .
C7 C 0.8579(5) 0.5318(3) 0.71841(19) 0.0338(7) Uani 1 1 d . . . . .
N8 N 0.7375(4) 0.7172(2) 0.57179(17) 0.0353(6) Uani 1 1 d . . . . .
N9 N 0.7251(4) 0.8067(2) 0.60977(19) 0.0412(7) Uani 1 1 d . . . . .
C10 C 0.6677(6) 0.8874(3) 0.5639(3) 0.0518(10) Uani 1 1 d . . . . .
H10 H 0.646825 0.959809 0.575041 0.062 Uiso 1 1 calc R U . . .
C11 C 0.6426(7) 0.8507(4) 0.4970(3) 0.0605(13) Uani 1 1 d . . . . .
H11 H 0.602638 0.892227 0.455844 0.073 Uiso 1 1 calc R U . . .
C12 C 0.6877(6) 0.7426(3) 0.5037(2) 0.0491(10) Uani 1 1 d . . . . .
H12 H 0.684914 0.694343 0.467662 0.059 Uiso 1 1 calc R U . . .
N13 N 0.8775(4) 0.5490(3) 0.79259(17) 0.0393(7) Uani 1 1 d D . . . .
N14 N 0.8532(4) 0.6522(3) 0.81263(17) 0.0414(7) Uani 1 1 d D . . . .
C15A C 0.8565(14) 0.6542(8) 0.8848(4) 0.038(2) Uiso 0.5 1 d D . P A 1
H15A H 0.844619 0.715833 0.911487 0.046 Uiso 0.5 1 calc R U P A 1
C16A C 0.8812(13) 0.5472(7) 0.9150(5) 0.047(2) Uiso 0.5 1 d D . P A 1
H16A H 0.891078 0.523381 0.965478 0.057 Uiso 0.5 1 calc R U P A 1
C17A C 0.8881(12) 0.4839(6) 0.8569(4) 0.039(2) Uiso 0.5 1 d D . P A 1
H17A H 0.898380 0.408463 0.860902 0.047 Uiso 0.5 1 calc R U P A 1
C15B C 0.8855(16) 0.6316(9) 0.8835(5) 0.056(4) Uiso 0.5 1 d D . P A 2
H15B H 0.877303 0.686620 0.915942 0.067 Uiso 0.5 1 calc R U P A 2
C16B C 0.9316(16) 0.5251(8) 0.9062(6) 0.062(3) Uiso 0.5 1 d D . P A 2
H16B H 0.954824 0.495911 0.954012 0.075 Uiso 0.5 1 calc R U P A 2
C17B C 0.9359(14) 0.4718(7) 0.8439(5) 0.052(3) Uiso 0.5 1 d D . P A 2
H17B H 0.971070 0.398404 0.837587 0.062 Uiso 0.5 1 calc R U P A 2
N18 N 0.8693(5) 0.3316(3) 0.5839(2) 0.0493(9) Uani 1 1 d . . . . .
H18 H 0.846189 0.337493 0.538165 0.059 Uiso 1 1 calc R U . . .
C19 C 0.9167(7) 0.2282(3) 0.6139(3) 0.0556(11) Uani 1 1 d . . . . .
O20 O 0.9554(7) 0.2094(3) 0.6751(2) 0.0875(14) Uani 1 1 d . . . . .
C21 C 0.9119(8) 0.1433(4) 0.5616(4) 0.0715(15) Uani 1 1 d . . . . .
H21A H 0.964766 0.074558 0.581119 0.107 Uiso 1 1 calc R U . . .
H21B H 0.969994 0.162636 0.511732 0.107 Uiso 1 1 calc R U . . .
H21C H 0.797982 0.138143 0.558264 0.107 Uiso 1 1 calc R U . . .
N22 N 0.7121(4) 0.9044(2) 0.79525(17) 0.0351(6) Uani 1 1 d . . . . .
C23 C 0.5639(5) 0.9207(3) 0.8373(2) 0.0362(8) Uani 1 1 d . . . . .
C24 C 0.5112(5) 1.0050(3) 0.8816(2) 0.0422(9) Uani 1 1 d . . . . .
H24 H 0.405752 1.012908 0.911213 0.051 Uiso 1 1 calc R U . . .
C25 C 0.6205(5) 1.0787(3) 0.8811(2) 0.0424(9) Uani 1 1 d . . . . .
C26 C 0.7775(5) 1.0635(3) 0.8387(2) 0.0416(9) Uani 1 1 d . . . . .
H26 H 0.853813 1.111404 0.838172 0.050 Uiso 1 1 calc R U . . .
C27 C 0.8154(5) 0.9746(3) 0.7975(2) 0.0342(7) Uani 1 1 d . . . . .
N28 N 0.4645(4) 0.8423(3) 0.83049(18) 0.0406(7) Uani 1 1 d . . . . .
N29 N 0.5219(4) 0.7682(3) 0.7792(2) 0.0439(8) Uani 1 1 d . . . . .
C30 C 0.4073(6) 0.7050(4) 0.7864(3) 0.0541(11) Uani 1 1 d . . . . .
H30 H 0.413093 0.646238 0.757499 0.065 Uiso 1 1 calc R U . . .
C31 C 0.2764(7) 0.7369(5) 0.8425(3) 0.0652(13) Uani 1 1 d . . . . .
H31 H 0.180335 0.704572 0.858325 0.078 Uiso 1 1 calc R U . . .
C32 C 0.3153(6) 0.8238(4) 0.8698(3) 0.0554(11) Uani 1 1 d . . . . .
H32 H 0.251378 0.863811 0.908462 0.067 Uiso 1 1 calc R U . . .
N33 N 0.9689(4) 0.9489(2) 0.75144(18) 0.0364(7) Uani 1 1 d . . . . .
N34 N 0.9886(4) 0.8648(3) 0.70724(19) 0.0419(7) Uani 1 1 d . . . . .
C35 C 1.1418(5) 0.8608(4) 0.6703(3) 0.0493(10) Uani 1 1 d . . . . .
H35 H 1.190663 0.810366 0.635253 0.059 Uiso 1 1 calc R U . . .
C36 C 1.2213(5) 0.9406(4) 0.6898(3) 0.0512(10) Uani 1 1 d . . . . .
H36 H 1.330071 0.953646 0.671562 0.061 Uiso 1 1 calc R U . . .
C37 C 1.1078(5) 0.9958(3) 0.7411(3) 0.0441(9) Uani 1 1 d . . . . .
H37 H 1.123196 1.055437 0.764968 0.053 Uiso 1 1 calc R U . . .
N38 N 0.5643(5) 1.1659(3) 0.9248(2) 0.0538(9) Uani 1 1 d . . . . .
H38 H 0.486046 1.158033 0.962908 0.065 Uiso 1 1 calc R U . . .
C39 C 0.6229(7) 1.2636(4) 0.9123(3) 0.0621(13) Uani 1 1 d . . . . .
O40 O 0.7332(6) 1.2829(3) 0.8617(3) 0.0831(13) Uani 1 1 d . . . . .
C41 C 0.5313(9) 1.3455(5) 0.9657(4) 0.088(2) Uani 1 1 d . . . . .
H41A H 0.601751 1.398725 0.969286 0.131 Uiso 1 1 calc R U . . .
H41B H 0.501383 1.309700 1.015400 0.131 Uiso 1 1 calc R U . . .
H41C H 0.432117 1.380632 0.946855 0.131 Uiso 1 1 calc R U . . .
B42 B 0.7196(10) 0.4356(7) 0.3776(5) 0.014(2) Uiso 0.49 1 d D . P B 1
F43 F 0.7452(8) 0.5277(4) 0.4006(3) 0.0553(13) Uiso 0.49 1 d D . P B 1
F44 F 0.5596(9) 0.4221(8) 0.3780(5) 0.098(3) Uiso 0.49 1 d D . P B 1
F45 F 0.8133(9) 0.4005(6) 0.3136(4) 0.0647(19) Uiso 0.49 1 d D . P B 1
F46 F 0.7754(11) 0.3478(6) 0.4373(5) 0.092(3) Uiso 0.49 1 d D . P B 1
Cl42 Cl 0.7180(5) 0.4220(3) 0.3872(2) 0.0671(13) Uiso 0.51 1 d D . P C 2
O43 O 0.6680(11) 0.5273(6) 0.4142(5) 0.072(2) Uiso 0.51 1 d D . P C 2
O44 O 0.5790(9) 0.3701(7) 0.3952(5) 0.074(2) Uiso 0.51 1 d D . P C 2
O45 O 0.7843(10) 0.4358(7) 0.3054(4) 0.064(2) Uiso 0.51 1 d D . P C 2
O46 O 0.8436(8) 0.3597(5) 0.4252(3) 0.0464(14) Uiso 0.51 1 d D . P C 2
B47 B 0.0823(14) 1.1610(10) 0.9661(6) 0.0579(15) Uiso 0.41 1 d D U P . .
F48A F 0.144(2) 1.1407(14) 0.8887(7) 0.0538(19) Uiso 0.21 1 d D U P D 1
F49A F -0.0673(14) 1.1510(13) 0.9909(8) 0.0627(17) Uiso 0.21 1 d D U P D 1
F50A F 0.0783(19) 1.2840(8) 0.9535(8) 0.0594(17) Uiso 0.21 1 d D U P D 1
F51A F 0.1972(17) 1.1255(12) 1.0089(8) 0.0603(18) Uiso 0.21 1 d D U P D 1
F48B F 0.116(2) 1.1624(13) 0.8865(6) 0.0551(19) Uiso 0.2 1 d D U P D 2
F49B F -0.0201(17) 1.0921(11) 0.9983(8) 0.0654(17) Uiso 0.2 1 d D U P D 2
F50B F -0.0212(17) 1.2614(10) 0.9815(8) 0.0617(17) Uiso 0.2 1 d D U P D 2
F51B F 0.2222(17) 1.1620(15) 0.9962(10) 0.0596(18) Uiso 0.2 1 d D U P D 2
Cl47 Cl 0.1052(3) 1.18317(18) 0.95888(13) 0.0597(5) Uiso 0.59 1 d D . P E 3
O48 O 0.1263(10) 1.1119(6) 0.9020(4) 0.068(2) Uiso 0.59 1 d D . P E 3
O49 O -0.0436(9) 1.1963(7) 1.0038(4) 0.079(2) Uiso 0.59 1 d D . P E 3
O50 O 0.1523(10) 1.2906(5) 0.9305(4) 0.080(2) Uiso 0.59 1 d D . P E 3
O51 O 0.2411(9) 1.1418(6) 1.0058(4) 0.0552(19) Uiso 0.59 1 d D . P E 3
C53A C 0.5113(16) 0.7055(9) 0.2881(7) 0.079(3) Uiso 0.5 1 d D . P F 1
H53A H 0.420776 0.695583 0.262139 0.095 Uiso 0.5 1 calc R U P F 1
H53B H 0.508650 0.654903 0.333257 0.095 Uiso 0.5 1 calc R U P F 1
C52A C 0.670(2) 0.6784(15) 0.2374(10) 0.112(5) Uiso 0.5 1 d D . P F 1
H52A H 0.679795 0.604818 0.224259 0.168 Uiso 0.5 1 calc R U P F 1
H52B H 0.672753 0.726622 0.191823 0.168 Uiso 0.5 1 calc R U P F 1
H52C H 0.760770 0.685876 0.263057 0.168 Uiso 0.5 1 calc R U P F 1
C54A C 0.4824(15) 0.8141(8) 0.3118(6) 0.062(3) Uiso 0.5 1 d D . P F 1
N55A N 0.451(3) 0.9016(11) 0.3285(11) 0.088(6) Uiso 0.5 1 d D . P F 1
C52B C 0.556(2) 0.6453(12) 0.2492(10) 0.112(5) Uiso 0.5 1 d D . P G 2
H52D H 0.623776 0.583380 0.226837 0.168 Uiso 0.5 1 calc R U P G 2
H52E H 0.492351 0.622096 0.296881 0.168 Uiso 0.5 1 calc R U P G 2
H52F H 0.481231 0.679777 0.215129 0.168 Uiso 0.5 1 calc R U P G 2
C53B C 0.6637(18) 0.7228(11) 0.2628(9) 0.094(4) Uiso 0.5 1 d D . P G 2
H53C H 0.740224 0.687933 0.296745 0.113 Uiso 0.5 1 calc R U P G 2
H53D H 0.729080 0.745740 0.214815 0.113 Uiso 0.5 1 calc R U P G 2
C54B C 0.5609(17) 0.8180(9) 0.2971(7) 0.071(3) Uiso 0.5 1 d D . P G 2
N55B N 0.489(2) 0.8906(12) 0.3241(11) 0.087(6) Uiso 0.5 1 d D . P G 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.119(3) . ?
Fe1 N9 2.195(3) . ?
Fe1 N14 2.172(3) . ?
Fe1 N22 2.124(3) . ?
Fe1 N29 2.210(3) . ?
Fe1 N34 2.176(3) . ?
N2 C3 1.335(4) . ?
N2 C7 1.331(5) . ?
C3 C4 1.360(5) . ?
C3 N8 1.412(5) . ?
C4 H4 0.9400 . ?
C4 C5 1.401(5) . ?
C5 C6 1.394(5) . ?
C5 N18 1.390(5) . ?
C6 H6 0.9400 . ?
C6 C7 1.366(5) . ?
C7 N13 1.415(4) . ?
N8 N9 1.362(4) . ?
N8 C12 1.351(5) . ?
N9 C10 1.325(5) . ?
C10 H10 0.9400 . ?
C10 C11 1.392(7) . ?
C11 H11 0.9400 . ?
C11 C12 1.357(6) . ?
C12 H12 0.9400 . ?
N13 N14 1.364(5) . ?
N13 C17A 1.356(7) . ?
N13 C17B 1.362(8) . ?
N14 C15A 1.308(7) . ?
N14 C15B 1.339(8) . ?
C15A H15A 0.9400 . ?
C15A C16A 1.401(8) . ?
C16A H16A 0.9400 . ?
C16A C17A 1.368(8) . ?
C17A H17A 0.9400 . ?
C15B H15B 0.9400 . ?
C15B C16B 1.379(9) . ?
C16B H16B 0.9400 . ?
C16B C17B 1.359(9) . ?
C17B H17B 0.9400 . ?
N18 H18 0.8700 . ?
N18 C19 1.385(6) . ?
C19 O20 1.190(6) . ?
C19 C21 1.507(6) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
N22 C23 1.328(5) . ?
N22 C27 1.334(5) . ?
C23 C24 1.368(5) . ?
C23 N28 1.411(5) . ?
C24 H24 0.9400 . ?
C24 C25 1.395(6) . ?
C25 C26 1.389(6) . ?
C25 N38 1.393(5) . ?
C26 H26 0.9400 . ?
C26 C27 1.375(5) . ?
C27 N33 1.407(5) . ?
N28 N29 1.357(4) . ?
N28 C32 1.358(5) . ?
N29 C30 1.315(5) . ?
C30 H30 0.9400 . ?
C30 C31 1.392(7) . ?
C31 H31 0.9400 . ?
C31 C32 1.350(7) . ?
C32 H32 0.9400 . ?
N33 N34 1.365(4) . ?
N33 C37 1.353(5) . ?
N34 C35 1.327(5) . ?
C35 H35 0.9400 . ?
C35 C36 1.390(6) . ?
C36 H36 0.9400 . ?
C36 C37 1.363(6) . ?
C37 H37 0.9400 . ?
N38 H38 0.8700 . ?
N38 C39 1.380(6) . ?
C39 O40 1.210(7) . ?
C39 C41 1.511(7) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C41 H41C 0.9700 . ?
B42 F43 1.333(9) . ?
B42 F44 1.363(10) . ?
B42 F45 1.348(10) . ?
B42 F46 1.538(11) . ?
Cl42 O43 1.439(8) . ?
Cl42 O44 1.392(8) . ?
Cl42 O45 1.485(7) . ?
Cl42 O46 1.431(7) . ?
B47 F48A 1.434(14) . ?
B47 F49A 1.266(13) . ?
B47 F50A 1.543(14) . ?
B47 F51A 1.323(14) . ?
B47 F48B 1.410(14) . ?
B47 F49B 1.332(14) . ?
B47 F50B 1.440(14) . ?
B47 F51B 1.365(14) . ?
Cl47 O48 1.403(7) . ?
Cl47 O49 1.352(7) . ?
Cl47 O50 1.486(7) . ?
Cl47 O51 1.520(6) . ?
C53A H53A 0.9800 . ?
C53A H53B 0.9800 . ?
C53A C52A 1.481(14) . ?
C53A C54A 1.450(12) . ?
C52A H52A 0.9700 . ?
C52A H52B 0.9700 . ?
C52A H52C 0.9700 . ?
C54A N55A 1.154(13) . ?
C52B H52D 0.9700 . ?
C52B H52E 0.9700 . ?
C52B H52F 0.9700 . ?
C52B C53B 1.489(15) . ?
C53B H53C 0.9800 . ?
C53B H53D 0.9800 . ?
C53B C54B 1.486(13) . ?
C54B N55B 1.121(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N9 73.25(11) . . ?
N2 Fe1 N14 73.23(11) . . ?
N2 Fe1 N22 165.47(12) . . ?
N2 Fe1 N29 95.51(12) . . ?
N2 Fe1 N34 118.63(12) . . ?
N9 Fe1 N29 95.17(13) . . ?
N14 Fe1 N9 146.47(12) . . ?
N14 Fe1 N29 87.54(14) . . ?
N14 Fe1 N34 100.81(13) . . ?
N22 Fe1 N9 115.67(12) . . ?
N22 Fe1 N14 97.10(12) . . ?
N22 Fe1 N29 72.88(12) . . ?
N22 Fe1 N34 73.25(12) . . ?
N34 Fe1 N9 95.51(13) . . ?
N34 Fe1 N29 145.85(12) . . ?
C3 N2 Fe1 121.4(2) . . ?
C7 N2 Fe1 121.5(2) . . ?
C7 N2 C3 117.0(3) . . ?
N2 C3 C4 124.1(3) . . ?
N2 C3 N8 112.4(3) . . ?
C4 C3 N8 123.5(3) . . ?
C3 C4 H4 121.3 . . ?
C3 C4 C5 117.5(3) . . ?
C5 C4 H4 121.3 . . ?
C6 C5 C4 119.7(3) . . ?
N18 C5 C4 116.5(3) . . ?
N18 C5 C6 123.7(3) . . ?
C5 C6 H6 121.6 . . ?
C7 C6 C5 116.8(3) . . ?
C7 C6 H6 121.6 . . ?
N2 C7 C6 124.8(3) . . ?
N2 C7 N13 112.2(3) . . ?
C6 C7 N13 123.0(3) . . ?
N9 N8 C3 118.6(3) . . ?
C12 N8 C3 130.3(3) . . ?
C12 N8 N9 111.0(3) . . ?
N8 N9 Fe1 114.2(2) . . ?
C10 N9 Fe1 140.4(3) . . ?
C10 N9 N8 105.1(3) . . ?
N9 C10 H10 124.5 . . ?
N9 C10 C11 111.1(4) . . ?
C11 C10 H10 124.5 . . ?
C10 C11 H11 127.2 . . ?
C12 C11 C10 105.6(4) . . ?
C12 C11 H11 127.2 . . ?
N8 C12 C11 107.2(4) . . ?
N8 C12 H12 126.4 . . ?
C11 C12 H12 126.4 . . ?
N14 N13 C7 118.1(3) . . ?
C17A N13 C7 133.9(4) . . ?
C17A N13 N14 106.9(4) . . ?
C17B N13 C7 125.3(5) . . ?
C17B N13 N14 116.2(5) . . ?
N13 N14 Fe1 115.0(2) . . ?
C15A N14 Fe1 133.4(5) . . ?
C15A N14 N13 110.8(5) . . ?
C15B N14 Fe1 146.7(5) . . ?
C15B N14 N13 98.3(6) . . ?
N14 C15A H15A 126.4 . . ?
N14 C15A C16A 107.2(7) . . ?
C16A C15A H15A 126.4 . . ?
C15A C16A H16A 126.6 . . ?
C17A C16A C15A 106.8(7) . . ?
C17A C16A H16A 126.6 . . ?
N13 C17A C16A 108.2(7) . . ?
N13 C17A H17A 125.9 . . ?
C16A C17A H17A 125.9 . . ?
N14 C15B H15B 121.9 . . ?
N14 C15B C16B 116.2(9) . . ?
C16B C15B H15B 121.9 . . ?
C15B C16B H16B 127.7 . . ?
C17B C16B C15B 104.5(9) . . ?
C17B C16B H16B 127.7 . . ?
N13 C17B H17B 127.9 . . ?
C16B C17B N13 104.3(8) . . ?
C16B C17B H17B 127.9 . . ?
C5 N18 H18 116.2 . . ?
C19 N18 C5 127.6(4) . . ?
C19 N18 H18 116.2 . . ?
N18 C19 C21 113.1(4) . . ?
O20 C19 N18 122.8(4) . . ?
O20 C19 C21 124.1(4) . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 N22 Fe1 121.6(2) . . ?
C23 N22 C27 117.2(3) . . ?
C27 N22 Fe1 121.2(2) . . ?
N22 C23 C24 124.1(4) . . ?
N22 C23 N28 112.6(3) . . ?
C24 C23 N28 123.3(4) . . ?
C23 C24 H24 121.4 . . ?
C23 C24 C25 117.3(4) . . ?
C25 C24 H24 121.4 . . ?
C26 C25 C24 120.3(3) . . ?
C26 C25 N38 122.8(4) . . ?
N38 C25 C24 116.9(4) . . ?
C25 C26 H26 121.8 . . ?
C27 C26 C25 116.5(4) . . ?
C27 C26 H26 121.8 . . ?
N22 C27 C26 124.6(4) . . ?
N22 C27 N33 112.3(3) . . ?
C26 C27 N33 123.1(3) . . ?
N29 N28 C23 118.7(3) . . ?
N29 N28 C32 110.8(3) . . ?
C32 N28 C23 130.4(4) . . ?
N28 N29 Fe1 113.8(2) . . ?
C30 N29 Fe1 139.7(3) . . ?
C30 N29 N28 105.5(3) . . ?
N29 C30 H30 124.6 . . ?
N29 C30 C31 110.8(4) . . ?
C31 C30 H30 124.6 . . ?
C30 C31 H31 126.9 . . ?
C32 C31 C30 106.2(4) . . ?
C32 C31 H31 126.9 . . ?
N28 C32 H32 126.7 . . ?
C31 C32 N28 106.7(4) . . ?
C31 C32 H32 126.7 . . ?
N34 N33 C27 118.4(3) . . ?
C37 N33 C27 130.6(3) . . ?
C37 N33 N34 110.9(3) . . ?
N33 N34 Fe1 114.6(2) . . ?
C35 N34 Fe1 140.3(3) . . ?
C35 N34 N33 104.8(3) . . ?
N34 C35 H35 124.2 . . ?
N34 C35 C36 111.6(4) . . ?
C36 C35 H35 124.2 . . ?
C35 C36 H36 127.4 . . ?
C37 C36 C35 105.3(4) . . ?
C37 C36 H36 127.4 . . ?
N33 C37 C36 107.4(4) . . ?
N33 C37 H37 126.3 . . ?
C36 C37 H37 126.3 . . ?
C25 N38 H38 117.4 . . ?
C39 N38 C25 125.2(4) . . ?
C39 N38 H38 117.4 . . ?
N38 C39 C41 113.5(5) . . ?
O40 C39 N38 123.1(4) . . ?
O40 C39 C41 123.3(5) . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
F43 B42 F44 117.0(7) . . ?
F43 B42 F45 118.1(8) . . ?
F43 B42 F46 105.4(7) . . ?
F44 B42 F46 102.8(8) . . ?
F45 B42 F44 109.4(7) . . ?
F45 B42 F46 101.6(7) . . ?
O43 Cl42 O45 107.8(5) . . ?
O44 Cl42 O43 108.6(6) . . ?
O44 Cl42 O45 108.1(5) . . ?
O44 Cl42 O46 111.1(5) . . ?
O46 Cl42 O43 112.5(5) . . ?
O46 Cl42 O45 108.6(5) . . ?
F48A B47 F50A 95.3(10) . . ?
F49A B47 F48A 117.7(12) . . ?
F49A B47 F50A 102.9(11) . . ?
F49A B47 F51A 119.9(12) . . ?
F51A B47 F48A 110.4(11) . . ?
F51A B47 F50A 106.4(11) . . ?
F48B B47 F50B 105.0(10) . . ?
F49B B47 F48B 113.8(12) . . ?
F49B B47 F50B 100.2(10) . . ?
F49B B47 F51B 117.9(12) . . ?
F51B B47 F48B 111.7(12) . . ?
F51B B47 F50B 106.4(11) . . ?
O48 Cl47 O50 113.3(4) . . ?
O48 Cl47 O51 105.4(5) . . ?
O49 Cl47 O48 117.3(5) . . ?
O49 Cl47 O50 109.0(5) . . ?
O49 Cl47 O51 110.4(5) . . ?
O50 Cl47 O51 99.9(4) . . ?
H53A C53A H53B 107.6 . . ?
C52A C53A H53A 108.6 . . ?
C52A C53A H53B 108.6 . . ?
C54A C53A H53A 108.6 . . ?
C54A C53A H53B 108.6 . . ?
C54A C53A C52A 114.6(11) . . ?
C53A C52A H52A 109.5 . . ?
C53A C52A H52B 109.5 . . ?
C53A C52A H52C 109.5 . . ?
H52A C52A H52B 109.5 . . ?
H52A C52A H52C 109.5 . . ?
H52B C52A H52C 109.5 . . ?
N55A C54A C53A 176.0(16) . . ?
H52D C52B H52E 109.5 . . ?
H52D C52B H52F 109.5 . . ?
H52E C52B H52F 109.5 . . ?
C53B C52B H52D 109.5 . . ?
C53B C52B H52E 109.5 . . ?
C53B C52B H52F 109.5 . . ?
C52B C53B H53C 109.7 . . ?
C52B C53B H53D 109.7 . . ?
H53C C53B H53D 108.2 . . ?
C54B C53B C52B 109.9(12) . . ?
C54B C53B H53C 109.7 . . ?
C54B C53B H53D 109.7 . . ?
N55B C54B C53B 177.2(18) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N18 H18 F46 0.87 1.99 2.855(9) 175.3 . yes
N18 H18 O46 0.87 2.03 2.883(7) 167.4 . yes
N38 H38 F51B 0.87 2.16 2.915(17) 144.5 . yes
N38 H38 O51 0.87 2.08 2.870(9) 150.5 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N2 C3 C4 179.2(3) . . . . ?
Fe1 N2 C3 N8 -1.0(4) . . . . ?
Fe1 N2 C7 C6 179.1(3) . . . . ?
Fe1 N2 C7 N13 0.8(4) . . . . ?
Fe1 N9 C10 C11 -172.6(4) . . . . ?
Fe1 N14 C15A C16A 167.7(5) . . . . ?
Fe1 N14 C15B C16B -179.3(7) . . . . ?
Fe1 N22 C23 C24 -178.1(3) . . . . ?
Fe1 N22 C23 N28 0.9(4) . . . . ?
Fe1 N22 C27 C26 177.2(3) . . . . ?
Fe1 N22 C27 N33 -1.8(4) . . . . ?
Fe1 N29 C30 C31 166.8(4) . . . . ?
Fe1 N34 C35 C36 -172.4(3) . . . . ?
N2 C3 C4 C5 1.8(6) . . . . ?
N2 C3 N8 N9 2.0(5) . . . . ?
N2 C3 N8 C12 -173.9(4) . . . . ?
N2 C7 N13 N14 -1.5(5) . . . . ?
N2 C7 N13 C17A 164.4(7) . . . . ?
N2 C7 N13 C17B -174.1(7) . . . . ?
C3 N2 C7 C6 -0.6(6) . . . . ?
C3 N2 C7 N13 -178.8(3) . . . . ?
C3 C4 C5 C6 -0.7(6) . . . . ?
C3 C4 C5 N18 178.0(4) . . . . ?
C3 N8 N9 Fe1 -1.9(4) . . . . ?
C3 N8 N9 C10 -176.9(4) . . . . ?
C3 N8 C12 C11 176.3(4) . . . . ?
C4 C3 N8 N9 -178.3(4) . . . . ?
C4 C3 N8 C12 5.8(7) . . . . ?
C4 C5 C6 C7 -0.8(6) . . . . ?
C4 C5 N18 C19 178.1(4) . . . . ?
C5 C6 C7 N2 1.5(6) . . . . ?
C5 C6 C7 N13 179.5(4) . . . . ?
C5 N18 C19 O20 -1.9(9) . . . . ?
C5 N18 C19 C21 177.5(4) . . . . ?
C6 C5 N18 C19 -3.2(7) . . . . ?
C6 C7 N13 N14 -179.8(4) . . . . ?
C6 C7 N13 C17A -13.9(9) . . . . ?
C6 C7 N13 C17B 7.6(8) . . . . ?
C7 N2 C3 C4 -1.1(5) . . . . ?
C7 N2 C3 N8 178.6(3) . . . . ?
C7 N13 N14 Fe1 1.5(4) . . . . ?
C7 N13 N14 C15A 172.5(6) . . . . ?
C7 N13 N14 C15B -179.1(7) . . . . ?
C7 N13 C17A C16A -170.9(6) . . . . ?
C7 N13 C17B C16B -179.6(7) . . . . ?
N8 C3 C4 C5 -177.9(3) . . . . ?
N8 N9 C10 C11 0.2(5) . . . . ?
N9 N8 C12 C11 0.2(5) . . . . ?
N9 C10 C11 C12 -0.1(6) . . . . ?
C10 C11 C12 N8 -0.1(6) . . . . ?
C12 N8 N9 Fe1 174.7(3) . . . . ?
C12 N8 N9 C10 -0.3(5) . . . . ?
N13 N14 C15A C16A -1.1(10) . . . . ?
N13 N14 C15B C16B 1.8(12) . . . . ?
N14 N13 C17A C16A -3.9(9) . . . . ?
N14 N13 C17B C16B 7.6(11) . . . . ?
N14 C15A C16A C17A -1.3(11) . . . . ?
N14 C15B C16B C17B 2.4(15) . . . . ?
C15A C16A C17A N13 3.3(11) . . . . ?
C17A N13 N14 Fe1 -167.9(5) . . . . ?
C17A N13 N14 C15A 3.1(8) . . . . ?
C15B C16B C17B N13 -5.5(13) . . . . ?
C17B N13 N14 Fe1 174.8(6) . . . . ?
C17B N13 N14 C15B -5.8(9) . . . . ?
N18 C5 C6 C7 -179.4(4) . . . . ?
N22 C23 C24 C25 1.0(6) . . . . ?
N22 C23 N28 N29 -5.6(5) . . . . ?
N22 C23 N28 C32 171.7(4) . . . . ?
N22 C27 N33 N34 5.2(5) . . . . ?
N22 C27 N33 C37 -176.2(4) . . . . ?
C23 N22 C27 C26 -1.6(6) . . . . ?
C23 N22 C27 N33 179.4(3) . . . . ?
C23 C24 C25 C26 -1.9(6) . . . . ?
C23 C24 C25 N38 178.3(4) . . . . ?
C23 N28 N29 Fe1 7.4(4) . . . . ?
C23 N28 N29 C30 178.6(4) . . . . ?
C23 N28 C32 C31 -178.1(4) . . . . ?
C24 C23 N28 N29 173.4(4) . . . . ?
C24 C23 N28 C32 -9.3(7) . . . . ?
C24 C25 C26 C27 1.1(6) . . . . ?
C24 C25 N38 C39 -155.5(5) . . . . ?
C25 C26 C27 N22 0.7(6) . . . . ?
C25 C26 C27 N33 179.6(4) . . . . ?
C25 N38 C39 O40 -1.2(9) . . . . ?
C25 N38 C39 C41 176.4(5) . . . . ?
C26 C25 N38 C39 24.7(7) . . . . ?
C26 C27 N33 N34 -173.8(4) . . . . ?
C26 C27 N33 C37 4.7(6) . . . . ?
C27 N22 C23 C24 0.7(6) . . . . ?
C27 N22 C23 N28 179.6(3) . . . . ?
C27 N33 N34 Fe1 -6.1(4) . . . . ?
C27 N33 N34 C35 179.2(3) . . . . ?
C27 N33 C37 C36 -179.3(4) . . . . ?
N28 C23 C24 C25 -177.9(4) . . . . ?
N28 N29 C30 C31 -0.6(6) . . . . ?
N29 N28 C32 C31 -0.5(6) . . . . ?
N29 C30 C31 C32 0.3(7) . . . . ?
C30 C31 C32 N28 0.2(6) . . . . ?
C32 N28 N29 Fe1 -170.4(3) . . . . ?
C32 N28 N29 C30 0.7(5) . . . . ?
N33 N34 C35 C36 0.0(5) . . . . ?
N34 N33 C37 C36 -0.7(5) . . . . ?
N34 C35 C36 C37 -0.5(5) . . . . ?
C35 C36 C37 N33 0.7(5) . . . . ?
C37 N33 N34 Fe1 175.1(3) . . . . ?
C37 N33 N34 C35 0.4(5) . . . . ?
N38 C25 C26 C27 -179.1(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: propionitrile/diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ic80_meo
_database_code_depnum_ccdc_archive 'CCDC 2078663'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2021-04-19 deposited with the CCDC.	2021-06-10 downloaded from the CCDC.
;
_audit_creation_date             2020-07-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            
'Bis-[N-(2,6-di{pyrazol-1-yl}pyrid-4-yl)acetamide]iron(II)ditetrafluoroborate methanol solvate'
_chemical_name_systematic        ?
_chemical_formula_moiety         'C26 H24 Fe N12 O2, C H4 O, 2(B F4)'
_chemical_formula_sum            'C27 H28 B2 F8 Fe N12 O3'
_chemical_formula_weight         798.08
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.2085(2)
_cell_length_b                   38.9652(11)
_cell_length_c                   10.8625(3)
_cell_angle_alpha                90
_cell_angle_beta                 105.691(3)
_cell_angle_gamma                90
_cell_volume                     3344.85(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4985
_cell_measurement_temperature    120(2)
_cell_measurement_theta_min      4.53
_cell_measurement_theta_max      73.33
_exptl_absorpt_coefficient_mu    4.485
_exptl_absorpt_correction_T_min  0.338
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.947
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12628
_diffrn_reflns_point_group_measured_fraction_full 0.947
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.681
_diffrn_reflns_theta_min         4.539
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5910
_reflns_number_total             6289
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2015)'
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         6289
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0615
_refine_ls_restrained_S_all      1.143
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0385P)²+8.1499P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1424
_refine_special_details          
;
 No disorder is present in the model, and all non-H atoms were refined 
 anisotropically. All C- and N-bound H atoms were placed in calculated 
 positions and refined using a riding model. The methanol hydroxyl H atom 
 was located in the Fourier map and allowed to refine with Uiso = 
 1.5xUeq{O}.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, H11 of C11, H12 of C12, H15 of C15, H10 of C10, H16 of C16,
   H6 of C6, H4 of C4, H30 of C30, H37 of C37, H32 of C32, H24 of C24, H26 of
  C26, H31 of C31, H35 of C35, H36 of C36, H17 of C17
 At 1.5 times of:
  All C(H,H,H) groups, H53 of C3
2. Restrained distances
 N18-H18 = N38-H38
 0.95 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17),
 N18(H18), C24(H24), C26(H26), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36),
  C37(H37), N38(H38)
3.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C41(H41A,H41B,H41C), C52(H52A,H52B,H52C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.42438(6) 0.61859(2) 0.69033(5) 0.01824(14) Uani 1 1 d . . . . .
N2 N 0.4297(3) 0.67340(7) 0.6780(3) 0.0179(5) Uani 1 1 d . . . . .
C3 C 0.5752(4) 0.69069(8) 0.7172(3) 0.0177(6) Uani 1 1 d . . . . .
H53 H 0.940(5) 0.7754(11) 0.621(4) 0.027 Uiso 1 1 d . U . . .
C4 C 0.5877(4) 0.72565(8) 0.7136(3) 0.0202(7) Uani 1 1 d . . . . .
H4 H 0.693455 0.736934 0.744397 0.024 Uiso 1 1 calc R U . . .
C5 C 0.4384(4) 0.74417(8) 0.6627(3) 0.0200(7) Uani 1 1 d . . . . .
C6 C 0.2848(4) 0.72667(8) 0.6166(3) 0.0205(7) Uani 1 1 d . . . . .
H6 H 0.181869 0.738488 0.579832 0.025 Uiso 1 1 calc R U . . .
C7 C 0.2907(4) 0.69158(8) 0.6274(3) 0.0190(6) Uani 1 1 d . . . . .
N8 N 0.7161(3) 0.66883(7) 0.7612(3) 0.0198(6) Uani 1 1 d . . . . .
N9 N 0.6910(4) 0.63413(7) 0.7547(3) 0.0220(6) Uani 1 1 d . . . . .
C10 C 0.8432(4) 0.62061(9) 0.8028(4) 0.0268(8) Uani 1 1 d . . . . .
H10 H 0.865944 0.596690 0.810591 0.032 Uiso 1 1 calc R U . . .
C11 C 0.9666(5) 0.64642(10) 0.8409(4) 0.0313(8) Uani 1 1 d . . . . .
H11 H 1.084414 0.643372 0.878377 0.038 Uiso 1 1 calc R U . . .
C12 C 0.8813(4) 0.67675(9) 0.8126(4) 0.0270(8) Uani 1 1 d . . . . .
H12 H 0.928787 0.699125 0.826289 0.032 Uiso 1 1 calc R U . . .
N13 N 0.1452(3) 0.67087(7) 0.5854(3) 0.0200(6) Uani 1 1 d . . . . .
N14 N 0.1645(3) 0.63612(7) 0.5954(3) 0.0206(6) Uani 1 1 d . . . . .
C15 C 0.0112(5) 0.62366(9) 0.5461(4) 0.0263(8) Uani 1 1 d . . . . .
H15 H -0.015891 0.599906 0.540942 0.032 Uiso 1 1 calc R U . . .
C16 C -0.1065(4) 0.64996(9) 0.5023(4) 0.0297(8) Uani 1 1 d . . . . .
H16 H -0.224109 0.647485 0.462389 0.036 Uiso 1 1 calc R U . . .
C17 C -0.0176(4) 0.67984(9) 0.5289(4) 0.0253(7) Uani 1 1 d . . . . .
H17 H -0.060949 0.702445 0.511297 0.030 Uiso 1 1 calc R U . . .
N18 N 0.4501(4) 0.77969(7) 0.6626(3) 0.0254(6) Uani 1 1 d D . . . .
H18 H 0.547278 0.788519 0.706165 0.031 Uiso 1 1 calc DR U . . .
C19 C 0.3270(4) 0.80277(9) 0.6019(3) 0.0242(7) Uani 1 1 d . . . . .
O20 O 0.1937(3) 0.79436(6) 0.5286(3) 0.0288(6) Uani 1 1 d . . . . .
C21 C 0.3716(5) 0.83954(9) 0.6376(4) 0.0340(9) Uani 1 1 d . . . . .
H21A H 0.306936 0.854631 0.569632 0.051 Uiso 1 1 calc R U . . .
H21B H 0.492929 0.843053 0.648518 0.051 Uiso 1 1 calc R U . . .
H21C H 0.344082 0.844893 0.717774 0.051 Uiso 1 1 calc R U . . .
N22 N 0.3340(3) 0.56895(6) 0.7213(3) 0.0174(5) Uani 1 1 d . . . . .
C23 C 0.2865(4) 0.56194(8) 0.8265(3) 0.0193(7) Uani 1 1 d . . . . .
C24 C 0.2122(4) 0.53174(8) 0.8470(3) 0.0208(7) Uani 1 1 d . . . . .
H24 H 0.178993 0.527907 0.923137 0.025 Uiso 1 1 calc R U . . .
C25 C 0.1875(4) 0.50676(8) 0.7508(3) 0.0219(7) Uani 1 1 d . . . . .
C26 C 0.2375(4) 0.51326(8) 0.6407(3) 0.0204(7) Uani 1 1 d . . . . .
H26 H 0.221568 0.496793 0.573973 0.024 Uiso 1 1 calc R U . . .
C27 C 0.3113(4) 0.54467(8) 0.6324(3) 0.0182(6) Uani 1 1 d . . . . .
N28 N 0.3243(4) 0.58850(7) 0.9180(3) 0.0208(6) Uani 1 1 d . . . . .
N29 N 0.3995(3) 0.61755(7) 0.8888(3) 0.0201(6) Uani 1 1 d . . . . .
C30 C 0.4286(4) 0.63666(9) 0.9945(3) 0.0239(7) Uani 1 1 d . . . . .
H30 H 0.480749 0.658618 1.003620 0.029 Uiso 1 1 calc R U . . .
C31 C 0.3726(5) 0.62032(9) 1.0899(4) 0.0327(9) Uani 1 1 d . . . . .
H31 H 0.377946 0.628776 1.172908 0.039 Uiso 1 1 calc R U . . .
C32 C 0.3083(5) 0.58947(9) 1.0382(3) 0.0290(8) Uani 1 1 d . . . . .
H32 H 0.261324 0.572050 1.079378 0.035 Uiso 1 1 calc R U . . .
N33 N 0.3739(3) 0.55413(7) 0.5285(3) 0.0185(6) Uani 1 1 d . . . . .
N34 N 0.4473(3) 0.58574(7) 0.5311(3) 0.0205(6) Uani 1 1 d . . . . .
C35 C 0.5061(4) 0.58652(9) 0.4290(4) 0.0271(8) Uani 1 1 d . . . . .
H35 H 0.563669 0.605509 0.405363 0.033 Uiso 1 1 calc R U . . .
C36 C 0.4721(5) 0.55563(9) 0.3602(4) 0.0267(7) Uani 1 1 d . . . . .
H36 H 0.501861 0.549818 0.284177 0.032 Uiso 1 1 calc R U . . .
C37 C 0.3871(4) 0.53571(9) 0.4259(3) 0.0225(7) Uani 1 1 d . . . . .
H37 H 0.345224 0.513177 0.403747 0.027 Uiso 1 1 calc R U . . .
N38 N 0.1171(4) 0.47600(7) 0.7760(3) 0.0277(7) Uani 1 1 d D . . . .
H38 H 0.107402 0.473276 0.854079 0.033 Uiso 1 1 calc DR U . . .
C39 C 0.0612(5) 0.44948(8) 0.6926(4) 0.0253(7) Uani 1 1 d . . . . .
O40 O 0.0670(4) 0.44988(7) 0.5827(3) 0.0407(7) Uani 1 1 d . . . . .
C41 C -0.0117(5) 0.42003(9) 0.7508(4) 0.0333(9) Uani 1 1 d . . . . .
H41A H -0.130276 0.424891 0.746371 0.050 Uiso 1 1 calc R U . . .
H41B H 0.052788 0.417158 0.840337 0.050 Uiso 1 1 calc R U . . .
H41C H -0.004914 0.398914 0.703403 0.050 Uiso 1 1 calc R U . . .
B42 B 0.9263(6) 0.80638(12) 0.8297(4) 0.0308(9) Uani 1 1 d . . . . .
F43 F 0.9258(3) 0.77265(7) 0.8696(3) 0.0501(7) Uani 1 1 d . . . . .
F44 F 0.9954(4) 0.82804(8) 0.9299(3) 0.0592(8) Uani 1 1 d . . . . .
F45 F 1.0213(4) 0.80929(7) 0.7424(3) 0.0539(7) Uani 1 1 d . . . . .
F46 F 0.7619(3) 0.81580(7) 0.7727(4) 0.0661(10) Uani 1 1 d . . . . .
B47 B 0.2508(5) 0.47678(12) 1.1361(4) 0.0321(10) Uani 1 1 d . . . . .
F48 F 0.1211(3) 0.46015(7) 1.0480(2) 0.0484(7) Uani 1 1 d . . . . .
F49 F 0.2024(4) 0.51122(7) 1.1398(3) 0.0538(7) Uani 1 1 d . . . . .
F50 F 0.3935(4) 0.47504(11) 1.0973(4) 0.0861(13) Uani 1 1 d . . . . .
F51 F 0.2727(4) 0.46247(7) 1.2559(3) 0.0562(8) Uani 1 1 d . . . . .
C52 C 0.7825(6) 0.77153(13) 0.4580(5) 0.0538(13) Uani 1 1 d . . . . .
H52A H 0.714489 0.790123 0.479309 0.081 Uiso 1 1 calc R U . . .
H52B H 0.707648 0.754505 0.404726 0.081 Uiso 1 1 calc R U . . .
H52C H 0.858991 0.780918 0.411051 0.081 Uiso 1 1 calc R U . . .
O53 O 0.8780(4) 0.75582(8) 0.5711(3) 0.0432(7) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.141(3) . ?
Fe1 N9 2.195(3) . ?
Fe1 N14 2.211(3) . ?
Fe1 N22 2.131(3) . ?
Fe1 N29 2.220(3) . ?
Fe1 N34 2.200(3) . ?
N2 C3 1.337(4) . ?
N2 C7 1.329(4) . ?
C3 C4 1.367(5) . ?
C3 N8 1.411(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.401(5) . ?
C5 C6 1.402(5) . ?
C5 N18 1.387(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.372(5) . ?
C7 N13 1.411(4) . ?
N8 N9 1.367(4) . ?
N8 C12 1.355(4) . ?
N9 C10 1.326(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.408(5) . ?
C11 H11 0.9500 . ?
C11 C12 1.366(5) . ?
C12 H12 0.9500 . ?
N13 N14 1.365(4) . ?
N13 C17 1.356(4) . ?
N14 C15 1.320(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.400(5) . ?
C16 H16 0.9500 . ?
C16 C17 1.363(5) . ?
C17 H17 0.9500 . ?
N18 H18 0.8800 . ?
N18 C19 1.380(4) . ?
C19 O20 1.211(4) . ?
C19 C21 1.503(5) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
N22 C23 1.332(4) . ?
N22 C27 1.329(4) . ?
C23 C24 1.371(5) . ?
C23 N28 1.410(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.403(5) . ?
C25 C26 1.389(5) . ?
C25 N38 1.389(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.379(5) . ?
C27 N33 1.409(4) . ?
N28 N29 1.367(4) . ?
N28 C32 1.348(5) . ?
N29 C30 1.334(4) . ?
C30 H30 0.9500 . ?
C30 C31 1.396(6) . ?
C31 H31 0.9500 . ?
C31 C32 1.371(5) . ?
C32 H32 0.9500 . ?
N33 N34 1.368(4) . ?
N33 C37 1.355(4) . ?
N34 C35 1.324(5) . ?
C35 H35 0.9500 . ?
C35 C36 1.404(5) . ?
C36 H36 0.9500 . ?
C36 C37 1.366(5) . ?
C37 H37 0.9500 . ?
N38 H38 0.8800 . ?
N38 C39 1.368(5) . ?
C39 O40 1.208(5) . ?
C39 C41 1.509(5) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
B42 F43 1.384(5) . ?
B42 F44 1.373(5) . ?
B42 F45 1.385(5) . ?
B42 F46 1.374(5) . ?
B47 F48 1.384(5) . ?
B47 F49 1.403(5) . ?
B47 F50 1.350(6) . ?
B47 F51 1.383(5) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C52 O53 1.407(6) . ?
O53 H53 1.00(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N9 73.09(10) . . ?
N2 Fe1 N14 72.32(10) . . ?
N2 Fe1 N29 95.03(10) . . ?
N2 Fe1 N34 121.57(11) . . ?
N9 Fe1 N14 144.71(10) . . ?
N9 Fe1 N29 92.37(11) . . ?
N9 Fe1 N34 96.94(11) . . ?
N14 Fe1 N29 97.36(11) . . ?
N22 Fe1 N2 158.32(11) . . ?
N22 Fe1 N9 124.06(10) . . ?
N22 Fe1 N14 91.19(10) . . ?
N22 Fe1 N29 72.71(10) . . ?
N22 Fe1 N34 72.76(10) . . ?
N34 Fe1 N14 95.16(11) . . ?
N34 Fe1 N29 143.38(10) . . ?
C3 N2 Fe1 121.0(2) . . ?
C7 N2 Fe1 121.8(2) . . ?
C7 N2 C3 117.1(3) . . ?
N2 C3 C4 124.1(3) . . ?
N2 C3 N8 112.5(3) . . ?
C4 C3 N8 123.4(3) . . ?
C3 C4 H4 121.3 . . ?
C3 C4 C5 117.4(3) . . ?
C5 C4 H4 121.3 . . ?
C4 C5 C6 119.8(3) . . ?
N18 C5 C4 117.5(3) . . ?
N18 C5 C6 122.8(3) . . ?
C5 C6 H6 121.7 . . ?
C7 C6 C5 116.5(3) . . ?
C7 C6 H6 121.7 . . ?
N2 C7 C6 125.0(3) . . ?
N2 C7 N13 112.7(3) . . ?
C6 C7 N13 122.3(3) . . ?
N9 N8 C3 118.8(3) . . ?
C12 N8 C3 129.7(3) . . ?
C12 N8 N9 111.5(3) . . ?
N8 N9 Fe1 114.4(2) . . ?
C10 N9 Fe1 140.2(2) . . ?
C10 N9 N8 105.1(3) . . ?
N9 C10 H10 124.5 . . ?
N9 C10 C11 111.0(3) . . ?
C11 C10 H10 124.5 . . ?
C10 C11 H11 127.2 . . ?
C12 C11 C10 105.5(3) . . ?
C12 C11 H11 127.2 . . ?
N8 C12 C11 106.9(3) . . ?
N8 C12 H12 126.6 . . ?
C11 C12 H12 126.6 . . ?
N14 N13 C7 118.1(3) . . ?
C17 N13 C7 130.0(3) . . ?
C17 N13 N14 111.8(3) . . ?
N13 N14 Fe1 114.87(19) . . ?
C15 N14 Fe1 140.3(2) . . ?
C15 N14 N13 104.8(3) . . ?
N14 C15 H15 124.3 . . ?
N14 C15 C16 111.3(3) . . ?
C16 C15 H15 124.3 . . ?
C15 C16 H16 127.1 . . ?
C17 C16 C15 105.8(3) . . ?
C17 C16 H16 127.1 . . ?
N13 C17 C16 106.4(3) . . ?
N13 C17 H17 126.8 . . ?
C16 C17 H17 126.8 . . ?
C5 N18 H18 116.3 . . ?
C19 N18 C5 127.5(3) . . ?
C19 N18 H18 116.3 . . ?
N18 C19 C21 113.7(3) . . ?
O20 C19 N18 123.5(3) . . ?
O20 C19 C21 122.7(3) . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 N22 Fe1 121.1(2) . . ?
C27 N22 Fe1 121.2(2) . . ?
C27 N22 C23 117.5(3) . . ?
N22 C23 C24 124.2(3) . . ?
N22 C23 N28 113.2(3) . . ?
C24 C23 N28 122.5(3) . . ?
C23 C24 H24 121.4 . . ?
C23 C24 C25 117.1(3) . . ?
C25 C24 H24 121.4 . . ?
C26 C25 C24 119.9(3) . . ?
C26 C25 N38 124.2(3) . . ?
N38 C25 C24 115.9(3) . . ?
C25 C26 H26 121.5 . . ?
C27 C26 C25 117.1(3) . . ?
C27 C26 H26 121.5 . . ?
N22 C27 C26 124.2(3) . . ?
N22 C27 N33 112.7(3) . . ?
C26 C27 N33 123.1(3) . . ?
N29 N28 C23 118.1(3) . . ?
C32 N28 C23 130.0(3) . . ?
C32 N28 N29 111.7(3) . . ?
N28 N29 Fe1 114.0(2) . . ?
C30 N29 Fe1 141.6(2) . . ?
C30 N29 N28 104.4(3) . . ?
N29 C30 H30 124.3 . . ?
N29 C30 C31 111.5(3) . . ?
C31 C30 H30 124.3 . . ?
C30 C31 H31 127.4 . . ?
C32 C31 C30 105.3(3) . . ?
C32 C31 H31 127.4 . . ?
N28 C32 C31 107.1(3) . . ?
N28 C32 H32 126.5 . . ?
C31 C32 H32 126.5 . . ?
N34 N33 C27 118.2(3) . . ?
C37 N33 C27 130.4(3) . . ?
C37 N33 N34 111.2(3) . . ?
N33 N34 Fe1 114.1(2) . . ?
C35 N34 Fe1 140.6(2) . . ?
C35 N34 N33 105.2(3) . . ?
N34 C35 H35 124.4 . . ?
N34 C35 C36 111.2(3) . . ?
C36 C35 H35 124.4 . . ?
C35 C36 H36 127.3 . . ?
C37 C36 C35 105.4(3) . . ?
C37 C36 H36 127.3 . . ?
N33 C37 C36 107.1(3) . . ?
N33 C37 H37 126.4 . . ?
C36 C37 H37 126.4 . . ?
C25 N38 H38 116.4 . . ?
C39 N38 C25 127.2(3) . . ?
C39 N38 H38 116.4 . . ?
N38 C39 C41 113.4(3) . . ?
O40 C39 N38 123.2(3) . . ?
O40 C39 C41 123.3(3) . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
F43 B42 F45 110.0(4) . . ?
F44 B42 F43 111.8(4) . . ?
F44 B42 F45 107.7(3) . . ?
F44 B42 F46 109.8(4) . . ?
F46 B42 F43 108.0(3) . . ?
F46 B42 F45 109.6(4) . . ?
F48 B47 F49 107.3(3) . . ?
F50 B47 F48 109.3(4) . . ?
F50 B47 F49 109.5(4) . . ?
F50 B47 F51 111.7(4) . . ?
F51 B47 F48 110.0(3) . . ?
F51 B47 F49 108.9(4) . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O53 C52 H52A 109.5 . . ?
O53 C52 H52B 109.5 . . ?
O53 C52 H52C 109.5 . . ?
C52 O53 H53 103(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N18 H18 F46 0.88 2.02 2.882(4) 167.3 . yes
N38 H38 F48 0.88 2.14 3.010(4) 169.5 . yes
O53 H53 F45 1.00(4) 1.85(4) 2.829(4) 165(4) . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N2 C3 C4 -179.1(3) . . . . ?
Fe1 N2 C3 N8 1.7(4) . . . . ?
Fe1 N2 C7 C6 179.9(3) . . . . ?
Fe1 N2 C7 N13 0.3(4) . . . . ?
Fe1 N9 C10 C11 -171.7(3) . . . . ?
Fe1 N14 C15 C16 177.8(3) . . . . ?
Fe1 N22 C23 C24 173.5(3) . . . . ?
Fe1 N22 C23 N28 -8.2(4) . . . . ?
Fe1 N22 C27 C26 -173.2(2) . . . . ?
Fe1 N22 C27 N33 7.9(4) . . . . ?
Fe1 N29 C30 C31 176.9(3) . . . . ?
Fe1 N34 C35 C36 -177.2(3) . . . . ?
N2 C3 C4 C5 -1.6(5) . . . . ?
N2 C3 N8 N9 2.5(4) . . . . ?
N2 C3 N8 C12 -177.0(3) . . . . ?
N2 C7 N13 N14 -3.0(4) . . . . ?
N2 C7 N13 C17 -179.6(3) . . . . ?
C3 N2 C7 C6 -2.4(5) . . . . ?
C3 N2 C7 N13 178.1(3) . . . . ?
C3 C4 C5 C6 -0.8(5) . . . . ?
C3 C4 C5 N18 178.1(3) . . . . ?
C3 N8 N9 Fe1 -5.3(4) . . . . ?
C3 N8 N9 C10 -179.6(3) . . . . ?
C3 N8 C12 C11 179.3(3) . . . . ?
C4 C3 N8 N9 -176.6(3) . . . . ?
C4 C3 N8 C12 3.9(6) . . . . ?
C4 C5 C6 C7 1.4(5) . . . . ?
C4 C5 N18 C19 170.0(3) . . . . ?
C5 C6 C7 N2 0.2(5) . . . . ?
C5 C6 C7 N13 179.7(3) . . . . ?
C5 N18 C19 O20 -7.5(6) . . . . ?
C5 N18 C19 C21 171.1(4) . . . . ?
C6 C5 N18 C19 -11.2(6) . . . . ?
C6 C7 N13 N14 177.4(3) . . . . ?
C6 C7 N13 C17 0.8(6) . . . . ?
C7 N2 C3 C4 3.1(5) . . . . ?
C7 N2 C3 N8 -176.0(3) . . . . ?
C7 N13 N14 Fe1 4.1(4) . . . . ?
C7 N13 N14 C15 -178.1(3) . . . . ?
C7 N13 C17 C16 177.2(4) . . . . ?
N8 C3 C4 C5 177.4(3) . . . . ?
N8 N9 C10 C11 0.2(4) . . . . ?
N9 N8 C12 C11 -0.2(4) . . . . ?
N9 C10 C11 C12 -0.3(5) . . . . ?
C10 C11 C12 N8 0.3(5) . . . . ?
C12 N8 N9 Fe1 174.3(2) . . . . ?
C12 N8 N9 C10 0.0(4) . . . . ?
N13 N14 C15 C16 1.0(4) . . . . ?
N14 N13 C17 C16 0.4(4) . . . . ?
N14 C15 C16 C17 -0.8(5) . . . . ?
C15 C16 C17 N13 0.2(4) . . . . ?
C17 N13 N14 Fe1 -178.7(2) . . . . ?
C17 N13 N14 C15 -0.9(4) . . . . ?
N18 C5 C6 C7 -177.4(3) . . . . ?
N22 C23 C24 C25 0.8(5) . . . . ?
N22 C23 N28 N29 1.2(4) . . . . ?
N22 C23 N28 C32 -173.9(3) . . . . ?
N22 C27 N33 N34 0.0(4) . . . . ?
N22 C27 N33 C37 173.9(3) . . . . ?
C23 N22 C27 C26 2.0(5) . . . . ?
C23 N22 C27 N33 -176.9(3) . . . . ?
C23 C24 C25 C26 -0.1(5) . . . . ?
C23 C24 C25 N38 178.0(3) . . . . ?
C23 N28 N29 Fe1 5.6(3) . . . . ?
C23 N28 N29 C30 -176.4(3) . . . . ?
C23 N28 C32 C31 176.2(3) . . . . ?
C24 C23 N28 N29 179.5(3) . . . . ?
C24 C23 N28 C32 4.5(6) . . . . ?
C24 C25 C26 C27 0.3(5) . . . . ?
C24 C25 N38 C39 171.2(3) . . . . ?
C25 C26 C27 N22 -1.3(5) . . . . ?
C25 C26 C27 N33 177.4(3) . . . . ?
C25 N38 C39 O40 0.0(6) . . . . ?
C25 N38 C39 C41 -178.9(3) . . . . ?
C26 C25 N38 C39 -10.8(6) . . . . ?
C26 C27 N33 N34 -178.9(3) . . . . ?
C26 C27 N33 C37 -4.9(5) . . . . ?
C27 N22 C23 C24 -1.7(5) . . . . ?
C27 N22 C23 N28 176.6(3) . . . . ?
C27 N33 N34 Fe1 -7.2(3) . . . . ?
C27 N33 N34 C35 175.0(3) . . . . ?
C27 N33 C37 C36 -173.9(3) . . . . ?
N28 C23 C24 C25 -177.4(3) . . . . ?
N28 N29 C30 C31 -0.2(4) . . . . ?
N29 N28 C32 C31 0.9(4) . . . . ?
N29 C30 C31 C32 0.7(4) . . . . ?
C30 C31 C32 N28 -1.0(4) . . . . ?
C32 N28 N29 Fe1 -178.4(2) . . . . ?
C32 N28 N29 C30 -0.4(4) . . . . ?
N33 N34 C35 C36 -0.2(4) . . . . ?
N34 N33 C37 C36 0.4(4) . . . . ?
N34 C35 C36 C37 0.5(4) . . . . ?
C35 C36 C37 N33 -0.5(4) . . . . ?
C37 N33 N34 Fe1 177.8(2) . . . . ?
C37 N33 N34 C35 -0.1(4) . . . . ?
N38 C25 C26 C27 -177.6(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol/diethyl ether'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_80etcnmt
_database_code_depnum_ccdc_archive 'CCDC 2078653'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2021-04-19 deposited with the CCDC.	2021-06-10 downloaded from the CCDC.
;
_audit_creation_date             2020-07-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis-[N-(2,6-di{pyrazol-1-yl}pyrid-4-yl)acetamide]iron(II)ditetrafluoroborate propionitrile solvate'
_chemical_formula_moiety         'C26 H24 Fe N12 O2, 2(B F4), C3 H5 N'
_chemical_formula_sum            'C29 H29 B2 F8 Fe N13 O2'
_chemical_formula_weight         821.12
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2464(3)
_cell_length_b                   12.5340(9)
_cell_length_c                   17.7464(9)
_cell_angle_alpha                83.832(5)
_cell_angle_beta                 79.727(4)
_cell_angle_gamma                82.425(5)
_cell_volume                     1782.48(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5844
_cell_measurement_temperature    187(2)
_cell_measurement_theta_max      72.43
_cell_measurement_theta_min      4.21
_exptl_absorpt_coefficient_mu    4.213
_exptl_absorpt_correction_T_max  0.696
_exptl_absorpt_correction_T_min  0.493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.935
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11206
_diffrn_reflns_point_group_measured_fraction_full 0.935
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.788
_diffrn_reflns_theta_min         3.571
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      187(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8519
_reflns_number_total             11206
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2015)'
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         11206
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0614
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1058P)²+0.0991P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1619
_refine_ls_wR_factor_ref         0.1724
_refine_special_details          
;The data were resolved into two non-superimposable twin domains, in a 
 ratio of 0.52:0.48.

 BF₄⁻ ion B47-F51 is disordered over two equally occupied sites. The 
 propionitrile molecule is also disordered over two orientations, whose 
 occupancies refined to 0.60:0.40. The bond distance restraints that were
 applied to the disordered residues are listed below. All 
 crystallographically ordered non-H atoms were refined anisotropically, 
 and H atoms were placed in calculated positions and refined using a 
 riding model.,Twin
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.4795(12)
 0.5205(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 B47A-F48A = B47A-F49A = B47A-F50A = B47A-F51A
 1.39558 with sigma of 0.02
 B47B-F48B = B47B-F49B = B47B-F50B = B47B-F51B
 1.39558 with sigma of 0.02
 F48A-F49A = F48A-F50A = F48A-F51A = F49A-F50A = F49A-F51A = F50A-F51A
 2.278982 with sigma of 0.02
 F48B-F49B = F48B-F50B = F48B-F51B = F49B-F50B = F49B-F51B = F50B-F51B
 2.278982 with sigma of 0.02
 C52A-C53A = C52B-C53B
 1.51 with sigma of 0.02
 C53A-C54A = C53B-C54B
 1.48 with sigma of 0.02
 C54A-N55A = C54B-N55B
 1.15 with sigma of 0.02
 C52A-C54A = C52B-C54B
 2.44 with sigma of 0.02
 C53A-N55A = C53B-N55B
 2.63 with sigma of 0.02
4. Others
 1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: B47A(0.5) F48A(0.5) F49A(0.5) F50A(0.5) F51A(0.5) B47B(0.5)
 F48B(0.5) F49B(0.5) F50B(0.5) F51B(0.5) C52A(0.6) H52A(0.6) H52B(0.6)
 H52C(0.6) C53A(0.6) H53A(0.6) H53B(0.6) C54A(0.6) N55A(0.6) C52B(0.4)
 H52D(0.4) H52E(0.4) H52F(0.4) C53B(0.4) H53C(0.4) H53D(0.4) C54B(0.4) N55B(0.4)
5.a Secondary CH2 refined with riding coordinates:
 C53A(H53A,H53B), C53B(H53C,H53D)
5.b Me refined with riding coordinates:
 C52A(H52A,H52B,H52C), C52B(H52D,H52E,H52F)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17),
 N18(H18), C24(H24), C26(H26), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36),
  C37(H37), N38(H38)
5.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C41(H41A,H41B,H41C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.77455(8) 0.77249(5) 0.72646(3) 0.03658(18) Uani 1 1 d . . . . .
N2 N 0.8139(4) 0.6271(2) 0.68073(17) 0.0344(7) Uani 1 1 d . . . . .
C3 C 0.7886(5) 0.6190(3) 0.6092(2) 0.0340(8) Uani 1 1 d . . . . .
C4 C 0.8105(5) 0.5238(3) 0.5756(2) 0.0389(8) Uani 1 1 d . . . . .
H4 H 0.794780 0.521750 0.524066 0.047 Uiso 1 1 calc R U . . .
C5 C 0.8568(5) 0.4296(3) 0.6201(2) 0.0411(9) Uani 1 1 d . . . . .
C6 C 0.8797(5) 0.4358(3) 0.6964(2) 0.0420(9) Uani 1 1 d . . . . .
H6 H 0.909673 0.373107 0.728255 0.050 Uiso 1 1 calc R U . . .
C7 C 0.8568(5) 0.5368(3) 0.7222(2) 0.0381(8) Uani 1 1 d . . . . .
N8 N 0.7366(5) 0.7199(3) 0.57312(19) 0.0417(8) Uani 1 1 d . . . . .
N9 N 0.7223(5) 0.8094(3) 0.6137(2) 0.0479(9) Uani 1 1 d . . . . .
C10 C 0.6641(7) 0.8898(4) 0.5679(4) 0.0667(15) Uani 1 1 d . . . . .
H10 H 0.641105 0.962699 0.580384 0.080 Uiso 1 1 calc R U . . .
C11 C 0.6404(8) 0.8551(4) 0.4992(3) 0.0739(17) Uani 1 1 d . . . . .
H11 H 0.600256 0.898198 0.457513 0.089 Uiso 1 1 calc R U . . .
C12 C 0.6869(6) 0.7461(4) 0.5040(3) 0.0564(12) Uani 1 1 d . . . . .
H12 H 0.684837 0.698123 0.466331 0.068 Uiso 1 1 calc R U . . .
N13 N 0.8726(4) 0.5577(3) 0.79708(18) 0.0423(8) Uani 1 1 d . . . . .
N14 N 0.8421(4) 0.6624(3) 0.81502(18) 0.0402(7) Uani 1 1 d . . . . .
C15 C 0.8516(6) 0.6603(4) 0.8889(2) 0.0537(11) Uani 1 1 d . . . . .
H15 H 0.835930 0.722027 0.917219 0.064 Uiso 1 1 calc R U . . .
C16 C 0.8878(7) 0.5551(5) 0.9186(3) 0.0740(16) Uani 1 1 d . . . . .
H16 H 0.900803 0.531919 0.970124 0.089 Uiso 1 1 calc R U . . .
C17 C 0.9013(7) 0.4904(4) 0.8598(3) 0.0642(13) Uani 1 1 d . . . . .
H17 H 0.925875 0.414017 0.862361 0.077 Uiso 1 1 calc R U . . .
N18 N 0.8732(5) 0.3333(3) 0.5861(2) 0.0492(9) Uani 1 1 d . . . . .
H18 H 0.850698 0.338333 0.539098 0.059 Uiso 1 1 calc R U . . .
C19 C 0.9206(7) 0.2306(4) 0.6171(3) 0.0556(11) Uani 1 1 d . . . . .
O20 O 0.9663(6) 0.2126(3) 0.6784(2) 0.0765(12) Uani 1 1 d . . . . .
C21 C 0.9131(8) 0.1439(4) 0.5653(3) 0.0706(15) Uani 1 1 d . . . . .
H21A H 0.989438 0.080199 0.577453 0.106 Uiso 1 1 calc R U . . .
H21B H 0.945035 0.171213 0.511502 0.106 Uiso 1 1 calc R U . . .
H21C H 0.799787 0.124130 0.573186 0.106 Uiso 1 1 calc R U . . .
N22 N 0.7085(4) 0.9023(3) 0.7916(2) 0.0442(8) Uani 1 1 d . . . . .
C23 C 0.5590(5) 0.9171(4) 0.8339(2) 0.0459(10) Uani 1 1 d . . . . .
C24 C 0.5078(6) 1.0018(4) 0.8790(2) 0.0515(11) Uani 1 1 d . . . . .
H24 H 0.400143 1.009532 0.909207 0.062 Uiso 1 1 calc R U . . .
C25 C 0.6195(6) 1.0757(4) 0.8788(2) 0.0532(12) Uani 1 1 d . . . . .
C26 C 0.7790(6) 1.0613(4) 0.8359(2) 0.0511(11) Uani 1 1 d . . . . .
H26 H 0.858291 1.109985 0.835571 0.061 Uiso 1 1 calc R U . . .
C27 C 0.8140(5) 0.9728(3) 0.7942(2) 0.0431(9) Uani 1 1 d . . . . .
N28 N 0.4605(4) 0.8362(3) 0.8276(2) 0.0511(9) Uani 1 1 d . . . . .
N29 N 0.5244(4) 0.7609(3) 0.7763(2) 0.0506(9) Uani 1 1 d . . . . .
C30 C 0.4099(7) 0.6954(5) 0.7825(3) 0.0693(15) Uani 1 1 d . . . . .
H30 H 0.418241 0.635146 0.753277 0.083 Uiso 1 1 calc R U . . .
C31 C 0.2729(7) 0.7272(6) 0.8385(4) 0.083(2) Uani 1 1 d . . . . .
H31 H 0.175041 0.692591 0.853960 0.099 Uiso 1 1 calc R U . . .
C32 C 0.3079(6) 0.8161(6) 0.8659(3) 0.0735(16) Uani 1 1 d . . . . .
H32 H 0.239662 0.856738 0.904339 0.088 Uiso 1 1 calc R U . . .
N33 N 0.9705(5) 0.9452(3) 0.7480(2) 0.0466(8) Uani 1 1 d . . . . .
N34 N 0.9856(5) 0.8571(3) 0.7060(2) 0.0545(10) Uani 1 1 d . . . . .
C35 C 1.1414(6) 0.8522(5) 0.6682(3) 0.0674(16) Uani 1 1 d . . . . .
H35 H 1.189444 0.799465 0.633565 0.081 Uiso 1 1 calc R U . . .
C36 C 1.2245(7) 0.9334(5) 0.6855(3) 0.0657(14) Uani 1 1 d . . . . .
H36 H 1.336085 0.945723 0.665999 0.079 Uiso 1 1 calc R U . . .
C37 C 1.1130(6) 0.9920(4) 0.7365(3) 0.0561(12) Uani 1 1 d . . . . .
H37 H 1.131799 1.053468 0.759389 0.067 Uiso 1 1 calc R U . . .
N38 N 0.5655(5) 1.1638(3) 0.9227(2) 0.0599(11) Uani 1 1 d . . . . .
H38 H 0.481758 1.156064 0.960457 0.072 Uiso 1 1 calc R U . . .
C39 C 0.6292(7) 1.2606(4) 0.9130(3) 0.0657(14) Uani 1 1 d . . . . .
O40 O 0.7459(6) 1.2795(3) 0.8636(2) 0.0812(12) Uani 1 1 d . . . . .
C41 C 0.5381(9) 1.3415(5) 0.9664(4) 0.0846(19) Uani 1 1 d . . . . .
H41A H 0.616332 1.386906 0.978586 0.127 Uiso 1 1 calc R U . . .
H41B H 0.485396 1.303669 1.013798 0.127 Uiso 1 1 calc R U . . .
H41C H 0.452916 1.386887 0.941642 0.127 Uiso 1 1 calc R U . . .
B42 B 0.7201(8) 0.4308(5) 0.3849(3) 0.0593(14) Uani 1 1 d . . . . .
F43 F 0.7204(6) 0.5345(3) 0.40507(19) 0.0943(12) Uani 1 1 d . . . . .
F44 F 0.5694(5) 0.4030(4) 0.3908(2) 0.1100(15) Uani 1 1 d . . . . .
F45 F 0.7998(4) 0.4237(3) 0.30968(17) 0.0810(10) Uani 1 1 d . . . . .
F46 F 0.8150(5) 0.3612(3) 0.43193(19) 0.0912(11) Uani 1 1 d . . . . .
B47A B 0.0976(16) 1.1680(11) 0.9599(7) 0.049(4) Uiso 0.5 1 d D . P A 1
F48A F 0.1280(9) 1.1417(6) 0.8849(4) 0.063(2) Uiso 0.5 1 d D . P A 1
F49A F -0.0510(9) 1.1492(7) 1.0000(4) 0.085(2) Uiso 0.5 1 d D . P A 1
F50A F 0.0886(11) 1.2848(6) 0.9442(5) 0.084(2) Uiso 0.5 1 d D . P A 1
F51A F 0.2426(9) 1.1497(6) 0.9978(4) 0.0521(19) Uiso 0.5 1 d D . P A 1
B47B B 0.1154(15) 1.1904(10) 0.9523(7) 0.045(4) Uiso 0.5 1 d D . P B 2
F48B F 0.1282(8) 1.1124(6) 0.8974(4) 0.0507(17) Uiso 0.5 1 d D . P B 2
F49B F -0.0376(9) 1.2020(6) 0.9965(4) 0.0752(18) Uiso 0.5 1 d D . P B 2
F50B F 0.1640(9) 1.2893(5) 0.9264(4) 0.0665(17) Uiso 0.5 1 d D . P B 2
F51B F 0.2142(9) 1.1278(6) 1.0040(4) 0.059(2) Uiso 0.5 1 d D . P B 2
C52A C 0.5501(14) 0.6394(8) 0.2491(6) 0.082(3) Uiso 0.6 1 d D . P C 1
H52A H 0.616311 0.578072 0.224291 0.124 Uiso 0.6 1 calc R U P C 1
H52B H 0.492080 0.614049 0.299663 0.124 Uiso 0.6 1 calc R U P C 1
H52C H 0.468771 0.673323 0.217170 0.124 Uiso 0.6 1 calc R U P C 1
C53A C 0.6648(12) 0.7224(8) 0.2589(6) 0.072(3) Uiso 0.6 1 d D . P C 1
H53A H 0.748168 0.687189 0.290238 0.086 Uiso 0.6 1 calc R U P C 1
H53B H 0.724866 0.746442 0.207774 0.086 Uiso 0.6 1 calc R U P C 1
C54A C 0.5788(15) 0.8129(8) 0.2942(6) 0.071(3) Uiso 0.6 1 d D . P C 1
N55A N 0.5027(15) 0.8851(9) 0.3188(7) 0.088(4) Uiso 0.6 1 d D . P C 1
C52B C 0.674(2) 0.6744(16) 0.2356(12) 0.106(6) Uiso 0.4 1 d D . P D 2
H52D H 0.683585 0.600849 0.220104 0.159 Uiso 0.4 1 calc R U P D 2
H52E H 0.681480 0.725890 0.189785 0.159 Uiso 0.4 1 calc R U P D 2
H52F H 0.764039 0.680612 0.263662 0.159 Uiso 0.4 1 calc R U P D 2
C53B C 0.509(2) 0.6991(12) 0.2869(10) 0.087(5) Uiso 0.4 1 d D . P D 2
H53C H 0.417306 0.692500 0.259004 0.104 Uiso 0.4 1 calc R U P D 2
H53D H 0.500108 0.647088 0.333100 0.104 Uiso 0.4 1 calc R U P D 2
C54B C 0.4960(18) 0.8118(9) 0.3101(7) 0.054(3) Uiso 0.4 1 d D . P D 2
N55B N 0.453(2) 0.8910(10) 0.3367(9) 0.070(4) Uiso 0.4 1 d D . P D 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.038(3) . ?
Fe1 N9 2.112(4) . ?
Fe1 N14 2.081(3) . ?
Fe1 N22 2.056(3) . ?
Fe1 N29 2.112(4) . ?
Fe1 N34 2.113(5) . ?
N2 C3 1.338(5) . ?
N2 C7 1.325(5) . ?
C3 C4 1.368(5) . ?
C3 N8 1.406(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.396(5) . ?
C5 C6 1.412(5) . ?
C5 N18 1.387(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.370(5) . ?
C7 N13 1.413(5) . ?
N8 N9 1.378(4) . ?
N8 C12 1.355(5) . ?
N9 C10 1.320(6) . ?
C10 H10 0.9500 . ?
C10 C11 1.392(8) . ?
C11 H11 0.9500 . ?
C11 C12 1.367(7) . ?
C12 H12 0.9500 . ?
N13 N14 1.364(5) . ?
N13 C17 1.359(6) . ?
N14 C15 1.324(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.382(8) . ?
C16 H16 0.9500 . ?
C16 C17 1.368(7) . ?
C17 H17 0.9500 . ?
N18 H18 0.8800 . ?
N18 C19 1.380(6) . ?
C19 O20 1.203(6) . ?
C19 C21 1.511(6) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
N22 C23 1.326(5) . ?
N22 C27 1.329(6) . ?
C23 C24 1.376(6) . ?
C23 N28 1.405(6) . ?
C24 H24 0.9500 . ?
C24 C25 1.389(7) . ?
C25 C26 1.397(7) . ?
C25 N38 1.397(5) . ?
C26 H26 0.9500 . ?
C26 C27 1.370(6) . ?
C27 N33 1.422(5) . ?
N28 N29 1.370(5) . ?
N28 C32 1.360(6) . ?
N29 C30 1.313(6) . ?
C30 H30 0.9500 . ?
C30 C31 1.411(9) . ?
C31 H31 0.9500 . ?
C31 C32 1.346(9) . ?
C32 H32 0.9500 . ?
N33 N34 1.377(5) . ?
N33 C37 1.356(6) . ?
N34 C35 1.336(6) . ?
C35 H35 0.9500 . ?
C35 C36 1.389(8) . ?
C36 H36 0.9500 . ?
C36 C37 1.368(7) . ?
C37 H37 0.9500 . ?
N38 H38 0.8800 . ?
N38 C39 1.367(7) . ?
C39 O40 1.210(7) . ?
C39 C41 1.497(7) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
B42 F43 1.384(7) . ?
B42 F44 1.318(7) . ?
B42 F45 1.386(7) . ?
B42 F46 1.402(7) . ?
B47A F48A 1.377(13) . ?
B47A F49A 1.339(14) . ?
B47A F50A 1.455(14) . ?
B47A F51A 1.455(13) . ?
B47B F48B 1.435(12) . ?
B47B F49B 1.361(13) . ?
B47B F50B 1.360(14) . ?
B47B F51B 1.436(13) . ?
C52A H52A 0.9800 . ?
C52A H52B 0.9800 . ?
C52A H52C 0.9800 . ?
C52A C53A 1.537(12) . ?
C53A H53A 0.9900 . ?
C53A H53B 0.9900 . ?
C53A C54A 1.402(12) . ?
C54A N55A 1.114(12) . ?
C52B H52D 0.9800 . ?
C52B H52E 0.9800 . ?
C52B H52F 0.9800 . ?
C52B C53B 1.512(18) . ?
C53B H53C 0.9900 . ?
C53B H53D 0.9900 . ?
C53B C54B 1.498(15) . ?
C54B N55B 1.133(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N9 75.70(12) . . ?
N2 Fe1 N14 75.65(12) . . ?
N2 Fe1 N22 168.26(14) . . ?
N2 Fe1 N29 95.93(14) . . ?
N2 Fe1 N34 113.85(13) . . ?
N9 Fe1 N34 94.18(14) . . ?
N14 Fe1 N9 151.34(13) . . ?
N14 Fe1 N29 87.91(14) . . ?
N14 Fe1 N34 98.11(14) . . ?
N22 Fe1 N9 112.19(13) . . ?
N22 Fe1 N14 96.00(13) . . ?
N22 Fe1 N29 75.26(15) . . ?
N22 Fe1 N34 75.09(14) . . ?
N29 Fe1 N9 94.17(14) . . ?
N29 Fe1 N34 150.20(15) . . ?
C3 N2 Fe1 121.1(2) . . ?
C7 N2 Fe1 121.1(2) . . ?
C7 N2 C3 117.8(3) . . ?
N2 C3 C4 123.9(3) . . ?
N2 C3 N8 111.9(3) . . ?
C4 C3 N8 124.2(3) . . ?
C3 C4 H4 121.3 . . ?
C3 C4 C5 117.4(3) . . ?
C5 C4 H4 121.3 . . ?
C4 C5 C6 119.7(3) . . ?
N18 C5 C4 116.7(3) . . ?
N18 C5 C6 123.6(4) . . ?
C5 C6 H6 121.6 . . ?
C7 C6 C5 116.8(3) . . ?
C7 C6 H6 121.6 . . ?
N2 C7 C6 124.4(3) . . ?
N2 C7 N13 111.3(3) . . ?
C6 C7 N13 124.3(3) . . ?
N9 N8 C3 117.8(3) . . ?
C12 N8 C3 130.7(4) . . ?
C12 N8 N9 111.4(3) . . ?
N8 N9 Fe1 113.5(2) . . ?
C10 N9 Fe1 141.7(3) . . ?
C10 N9 N8 104.4(4) . . ?
N9 C10 H10 124.0 . . ?
N9 C10 C11 111.9(4) . . ?
C11 C10 H10 124.0 . . ?
C10 C11 H11 127.1 . . ?
C12 C11 C10 105.7(4) . . ?
C12 C11 H11 127.1 . . ?
N8 C12 C11 106.5(4) . . ?
N8 C12 H12 126.7 . . ?
C11 C12 H12 126.7 . . ?
N14 N13 C7 117.6(3) . . ?
C17 N13 C7 131.7(4) . . ?
C17 N13 N14 110.6(4) . . ?
N13 N14 Fe1 114.4(2) . . ?
C15 N14 Fe1 138.9(3) . . ?
C15 N14 N13 106.3(4) . . ?
N14 C15 H15 125.0 . . ?
N14 C15 C16 109.9(4) . . ?
C16 C15 H15 125.0 . . ?
C15 C16 H16 126.4 . . ?
C17 C16 C15 107.2(4) . . ?
C17 C16 H16 126.4 . . ?
N13 C17 C16 106.0(5) . . ?
N13 C17 H17 127.0 . . ?
C16 C17 H17 127.0 . . ?
C5 N18 H18 116.1 . . ?
C19 N18 C5 127.8(4) . . ?
C19 N18 H18 116.1 . . ?
N18 C19 C21 113.0(4) . . ?
O20 C19 N18 123.2(4) . . ?
O20 C19 C21 123.8(4) . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 N22 Fe1 120.7(3) . . ?
C23 N22 C27 117.7(4) . . ?
C27 N22 Fe1 121.7(3) . . ?
N22 C23 C24 123.4(5) . . ?
N22 C23 N28 112.3(4) . . ?
C24 C23 N28 124.2(4) . . ?
C23 C24 H24 121.3 . . ?
C23 C24 C25 117.4(4) . . ?
C25 C24 H24 121.3 . . ?
C24 C25 C26 120.5(4) . . ?
C24 C25 N38 117.4(4) . . ?
C26 C25 N38 122.1(5) . . ?
C25 C26 H26 122.0 . . ?
C27 C26 C25 115.9(5) . . ?
C27 C26 H26 122.0 . . ?
N22 C27 C26 125.0(4) . . ?
N22 C27 N33 111.5(4) . . ?
C26 C27 N33 123.5(4) . . ?
N29 N28 C23 117.6(3) . . ?
C32 N28 C23 130.9(5) . . ?
C32 N28 N29 111.5(5) . . ?
N28 N29 Fe1 113.8(3) . . ?
C30 N29 Fe1 140.3(4) . . ?
C30 N29 N28 105.1(4) . . ?
N29 C30 H30 124.8 . . ?
N29 C30 C31 110.5(6) . . ?
C31 C30 H30 124.8 . . ?
C30 C31 H31 126.7 . . ?
C32 C31 C30 106.6(5) . . ?
C32 C31 H31 126.7 . . ?
N28 C32 H32 126.9 . . ?
C31 C32 N28 106.3(5) . . ?
C31 C32 H32 126.9 . . ?
N34 N33 C27 117.3(4) . . ?
C37 N33 C27 130.9(4) . . ?
C37 N33 N34 111.8(4) . . ?
N33 N34 Fe1 114.4(3) . . ?
C35 N34 Fe1 141.6(4) . . ?
C35 N34 N33 103.8(4) . . ?
N34 C35 H35 124.1 . . ?
N34 C35 C36 111.9(5) . . ?
C36 C35 H35 124.1 . . ?
C35 C36 H36 127.0 . . ?
C37 C36 C35 106.0(5) . . ?
C37 C36 H36 127.0 . . ?
N33 C37 C36 106.5(5) . . ?
N33 C37 H37 126.8 . . ?
C36 C37 H37 126.8 . . ?
C25 N38 H38 116.6 . . ?
C39 N38 C25 126.8(4) . . ?
C39 N38 H38 116.6 . . ?
N38 C39 C41 114.2(5) . . ?
O40 C39 N38 122.3(4) . . ?
O40 C39 C41 123.4(6) . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
F43 B42 F45 109.1(5) . . ?
F43 B42 F46 107.0(4) . . ?
F44 B42 F43 112.9(6) . . ?
F44 B42 F45 108.6(4) . . ?
F44 B42 F46 111.8(5) . . ?
F45 B42 F46 107.3(5) . . ?
F48A B47A F50A 97.8(9) . . ?
F48A B47A F51A 114.3(9) . . ?
F49A B47A F48A 115.7(10) . . ?
F49A B47A F50A 105.3(9) . . ?
F49A B47A F51A 119.6(10) . . ?
F51A B47A F50A 99.1(9) . . ?
F48B B47B F51B 98.2(8) . . ?
F49B B47B F48B 112.2(10) . . ?
F49B B47B F51B 102.4(9) . . ?
F50B B47B F48B 118.0(9) . . ?
F50B B47B F49B 109.8(9) . . ?
F50B B47B F51B 114.7(10) . . ?
H52A C52A H52B 109.5 . . ?
H52A C52A H52C 109.5 . . ?
H52B C52A H52C 109.5 . . ?
C53A C52A H52A 109.5 . . ?
C53A C52A H52B 109.5 . . ?
C53A C52A H52C 109.5 . . ?
C52A C53A H53A 109.0 . . ?
C52A C53A H53B 109.0 . . ?
H53A C53A H53B 107.8 . . ?
C54A C53A C52A 112.9(9) . . ?
C54A C53A H53A 109.0 . . ?
C54A C53A H53B 109.0 . . ?
N55A C54A C53A 175.1(14) . . ?
H52D C52B H52E 109.5 . . ?
H52D C52B H52F 109.5 . . ?
H52E C52B H52F 109.5 . . ?
C53B C52B H52D 109.5 . . ?
C53B C52B H52E 109.5 . . ?
C53B C52B H52F 109.5 . . ?
C52B C53B H53C 109.9 . . ?
C52B C53B H53D 109.9 . . ?
H53C C53B H53D 108.3 . . ?
C54B C53B C52B 108.9(13) . . ?
C54B C53B H53C 109.9 . . ?
C54B C53B H53D 109.9 . . ?
N55B C54B C53B 164.5(17) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N18 H18 F46 0.88 1.96 2.838(5) 174.2 . yes
N38 H38 F51A 0.88 1.97 2.776(9) 150.8 . yes
N38 H38 F51B 0.88 2.27 3.065(9) 151.0 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N2 C3 C4 -179.1(3) . . . . ?
Fe1 N2 C3 N8 0.7(5) . . . . ?
Fe1 N2 C7 C6 177.7(3) . . . . ?
Fe1 N2 C7 N13 -1.2(5) . . . . ?
Fe1 N9 C10 C11 -171.8(4) . . . . ?
Fe1 N14 C15 C16 172.3(4) . . . . ?
Fe1 N22 C23 C24 179.6(3) . . . . ?
Fe1 N22 C23 N28 0.0(5) . . . . ?
Fe1 N22 C27 C26 179.7(3) . . . . ?
Fe1 N22 C27 N33 -0.5(5) . . . . ?
Fe1 N29 C30 C31 167.9(4) . . . . ?
Fe1 N34 C35 C36 -174.0(4) . . . . ?
N2 C3 C4 C5 2.1(6) . . . . ?
N2 C3 N8 N9 1.2(5) . . . . ?
N2 C3 N8 C12 -174.6(5) . . . . ?
N2 C7 N13 N14 0.3(5) . . . . ?
N2 C7 N13 C17 174.3(5) . . . . ?
C3 N2 C7 C6 1.2(6) . . . . ?
C3 N2 C7 N13 -177.7(3) . . . . ?
C3 C4 C5 C6 -0.3(6) . . . . ?
C3 C4 C5 N18 178.0(4) . . . . ?
C3 N8 N9 Fe1 -2.4(5) . . . . ?
C3 N8 N9 C10 -176.8(4) . . . . ?
C3 N8 C12 C11 176.4(5) . . . . ?
C4 C3 N8 N9 -179.0(4) . . . . ?
C4 C3 N8 C12 5.1(7) . . . . ?
C4 C5 C6 C7 -0.9(6) . . . . ?
C4 C5 N18 C19 178.5(5) . . . . ?
C5 C6 C7 N2 0.5(7) . . . . ?
C5 C6 C7 N13 179.2(4) . . . . ?
C5 N18 C19 O20 -5.5(9) . . . . ?
C5 N18 C19 C21 175.9(5) . . . . ?
C6 C5 N18 C19 -3.3(8) . . . . ?
C6 C7 N13 N14 -178.5(4) . . . . ?
C6 C7 N13 C17 -4.5(8) . . . . ?
C7 N2 C3 C4 -2.5(6) . . . . ?
C7 N2 C3 N8 177.3(3) . . . . ?
C7 N13 N14 Fe1 0.6(4) . . . . ?
C7 N13 N14 C15 175.1(4) . . . . ?
C7 N13 C17 C16 -174.1(5) . . . . ?
N8 C3 C4 C5 -177.6(4) . . . . ?
N8 N9 C10 C11 0.0(6) . . . . ?
N9 N8 C12 C11 0.4(6) . . . . ?
N9 C10 C11 C12 0.3(7) . . . . ?
C10 C11 C12 N8 -0.4(7) . . . . ?
C12 N8 N9 Fe1 174.2(3) . . . . ?
C12 N8 N9 C10 -0.2(5) . . . . ?
N13 N14 C15 C16 -0.1(5) . . . . ?
N14 N13 C17 C16 0.2(6) . . . . ?
N14 C15 C16 C17 0.2(7) . . . . ?
C15 C16 C17 N13 -0.3(7) . . . . ?
C17 N13 N14 Fe1 -174.6(3) . . . . ?
C17 N13 N14 C15 -0.1(5) . . . . ?
N18 C5 C6 C7 -179.1(4) . . . . ?
N22 C23 C24 C25 0.8(6) . . . . ?
N22 C23 N28 N29 -4.8(5) . . . . ?
N22 C23 N28 C32 173.4(4) . . . . ?
N22 C27 N33 N34 3.5(5) . . . . ?
N22 C27 N33 C37 -177.4(4) . . . . ?
C23 N22 C27 C26 -1.6(6) . . . . ?
C23 N22 C27 N33 178.2(3) . . . . ?
C23 C24 C25 C26 -1.9(6) . . . . ?
C23 C24 C25 N38 177.9(4) . . . . ?
C23 N28 N29 Fe1 7.1(4) . . . . ?
C23 N28 N29 C30 179.3(4) . . . . ?
C23 N28 C32 C31 -178.7(5) . . . . ?
C24 C23 N28 N29 175.6(4) . . . . ?
C24 C23 N28 C32 -6.2(7) . . . . ?
C24 C25 C26 C27 1.3(6) . . . . ?
C24 C25 N38 C39 -157.9(5) . . . . ?
C25 C26 C27 N22 0.6(6) . . . . ?
C25 C26 C27 N33 -179.3(4) . . . . ?
C25 N38 C39 O40 -1.1(9) . . . . ?
C25 N38 C39 C41 176.6(5) . . . . ?
C26 C25 N38 C39 22.0(7) . . . . ?
C26 C27 N33 N34 -176.6(4) . . . . ?
C26 C27 N33 C37 2.5(7) . . . . ?
C27 N22 C23 C24 0.9(6) . . . . ?
C27 N22 C23 N28 -178.7(3) . . . . ?
C27 N33 N34 Fe1 -4.8(4) . . . . ?
C27 N33 N34 C35 178.9(4) . . . . ?
C27 N33 C37 C36 -179.1(4) . . . . ?
N28 C23 C24 C25 -179.6(4) . . . . ?
N28 N29 C30 C31 -0.9(6) . . . . ?
N29 N28 C32 C31 -0.4(6) . . . . ?
N29 C30 C31 C32 0.7(7) . . . . ?
C30 C31 C32 N28 -0.2(6) . . . . ?
C32 N28 N29 Fe1 -171.4(3) . . . . ?
C32 N28 N29 C30 0.8(5) . . . . ?
N33 N34 C35 C36 0.5(5) . . . . ?
N34 N33 C37 C36 0.1(5) . . . . ?
N34 C35 C36 C37 -0.4(6) . . . . ?
C35 C36 C37 N33 0.2(5) . . . . ?
C37 N33 N34 Fe1 175.9(3) . . . . ?
C37 N33 N34 C35 -0.4(5) . . . . ?
N38 C25 C26 C27 -178.6(4) . . . . ?
C52B C53B C54B N55B -178(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.4833 8083 6005 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000
1.0000
2 0.5167 8103 6005 nmt -0.9997 -0.0008 -0.0004 -0.5206 0.3588 0.6431 -0.5156
1.3551 -0.3596
_oxdiff_twin_integration_method  simultaneous
_twin_special_details            
;
Component 2 rotated by -179.9227° 
 around [0.00 0.71 0.71] (reciprocal) or [-0.33 0.85 0.40] (direct)
;
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: propionitrile/diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_etcnclmt
_database_code_depnum_ccdc_archive 'CCDC 2078656'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2021-04-19 deposited with the CCDC.	2021-06-10 downloaded from the CCDC.
;
_audit_creation_date             2020-07-24
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis-[N-(2,6-di{pyrazol-1-yl}pyrid-4-yl)acetamide]iron(II)diperchlorate propionitrile solvate'
_chemical_formula_moiety         'C26 H24 Fe N12 O2, 2(Cl O4), C3 H5 N'
_chemical_formula_sum            'C29 H29 Cl2 Fe N13 O10'
_chemical_formula_weight         846.40
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.3390(2)
_cell_length_b                   20.3671(5)
_cell_length_c                   22.8144(7)
_cell_angle_alpha                108.029(3)
_cell_angle_beta                 98.689(2)
_cell_angle_gamma                95.458(2)
_cell_volume                     3600.56(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11254
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      73.69
_cell_measurement_theta_min      4.01
_exptl_absorpt_coefficient_mu    5.376
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.943
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19056
_diffrn_reflns_point_group_measured_fraction_full 0.943
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.871
_diffrn_reflns_theta_min         3.576
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                14582
_reflns_number_total             19056
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2015)'
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     993
_refine_ls_number_reflns         19056
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0749
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1279P)²+5.4432P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1991
_refine_ls_wR_factor_ref         0.2156
_refine_special_details          
;The data were resolved into two non-superimposable twin domains, in a 
 ratio of 0.61:0.39.

 The asymmetric unit contains two formula units of the compound, with each 
 residue lying on a general crystallographic site. The only disorder in the 
 model is to one propionitrile molecule, which was modelled over two sites 
 whose occupancies refined to 0.83:0.17. The bond distance restraints that 
 were applied to the disordered solvent are listed below. All 
 crystallographically ordered non-H atoms were refined anisotropically, 
 and H atoms were placed in calculated positions and refined using a riding 
 model.,Twin
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.6094(12)
 0.3906(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C66A-C67A = C66B-C67B
 1.51 with sigma of 0.02
 C67A-C68A = C67B-C68B
 1.48 with sigma of 0.02
 C68A-N69A = C68B-N69B
 1.15 with sigma of 0.02
 C66A-C68A = C66B-C68B
 2.44 with sigma of 0.02
 C67A-N69A = C67B-N69B
 2.63 with sigma of 0.02
4. Others
 Fixed Sof: C66A(0.83) H66A(0.83) H66B(0.83) H66C(0.83) C67A(0.83) H67A(0.83)
 H67B(0.83) C68A(0.83) N69A(0.83) C66B(0.17) H66D(0.17) H66E(0.17) H66F(0.17)
 C67B(0.17) H67C(0.17) H67D(0.17) C68B(0.17) N69B(0.17)
5.a Secondary CH2 refined with riding coordinates:
 C63(H63A,H63B), C67A(H67A,H67B), C67B(H67C,H67D)
5.b Me refined with riding coordinates:
 C66A(H66A,H66B,H66C), C66B(H66D,H66E,H66F)
5.c Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C6A(H6A), C10A(H10A), C11A(H11A), C12A(H12A), C15A(H15A),
 C16A(H16A), C17A(H17A), N18A(H18A), C24A(H24A), C26A(H26A), C30A(H30A),
 C31A(H31A), C32A(H32A), C35A(H35A), C36A(H36A), C37A(H37A), N38A(H38A),
 C4B(H4B), C6B(H6B), C10B(H10B), C11B(H11B), C12B(H12B), C15B(H15B), C16B(H16B),
  C17B(H17B), N18B(H18B), C24B(H24B), C26B(H26B), C30B(H30B), C31B(H31B),
 C32B(H32B), C35B(H35B), C36B(H36B), C37B(H37B), N38B(H38B)
5.d Idealised Me refined as rotating group:
 C21A(H21A,H21B,H21C), C41A(H41A,H41B,H41C), C21B(H21D,H21E,H21F), C41B(H41D,
 H41E,H41F), C62(H62A,H62B,H62C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1A Fe -0.01348(10) 0.98194(5) 0.25145(4) 0.0208(2) Uani 1 1 d . . . . .
N2A N -0.0339(6) 0.9491(3) 0.1629(2) 0.0259(10) Uani 1 1 d . . . . .
C3A C 0.0888(7) 0.9649(3) 0.1357(3) 0.0267(12) Uani 1 1 d . . . . .
C4A C 0.0786(8) 0.9468(3) 0.0721(3) 0.0293(13) Uani 1 1 d . . . . .
H4A H 0.168281 0.959255 0.054560 0.035 Uiso 1 1 calc R U . . .
C5A C -0.0702(8) 0.9090(3) 0.0341(3) 0.0286(12) Uani 1 1 d . . . . .
C6A C -0.2042(8) 0.8931(3) 0.0604(3) 0.0300(13) Uani 1 1 d . . . . .
H6A H -0.307119 0.868977 0.035277 0.036 Uiso 1 1 calc R U . . .
C7A C -0.1766(7) 0.9147(3) 0.1249(3) 0.0255(12) Uani 1 1 d . . . . .
N8A N 0.2250(6) 1.0033(3) 0.1818(2) 0.0265(10) Uani 1 1 d . . . . .
N9A N 0.2083(6) 1.0174(3) 0.2437(2) 0.0255(10) Uani 1 1 d . . . . .
C10A C 0.3488(7) 1.0550(4) 0.2779(3) 0.0323(14) Uani 1 1 d . . . . .
H10A H 0.373385 1.071847 0.322522 0.039 Uiso 1 1 calc R U . . .
C11A C 0.4561(8) 1.0665(4) 0.2393(4) 0.0391(16) Uani 1 1 d . . . . .
H11A H 0.563420 1.092553 0.252606 0.047 Uiso 1 1 calc R U . . .
C12A C 0.3770(8) 1.0331(4) 0.1788(3) 0.0352(14) Uani 1 1 d . . . . .
H12A H 0.418799 1.030974 0.141893 0.042 Uiso 1 1 calc R U . . .
N13A N -0.2952(6) 0.9069(3) 0.1614(2) 0.0269(10) Uani 1 1 d . . . . .
N14A N -0.2452(6) 0.9331(3) 0.2262(2) 0.0258(10) Uani 1 1 d . . . . .
C15A C -0.3747(8) 0.9183(3) 0.2493(3) 0.0303(13) Uani 1 1 d . . . . .
H15A H -0.377304 0.929881 0.292796 0.036 Uiso 1 1 calc R U . . .
C16A C -0.5087(8) 0.8829(3) 0.2002(3) 0.0327(14) Uani 1 1 d . . . . .
H16A H -0.615483 0.866520 0.204402 0.039 Uiso 1 1 calc R U . . .
C17A C -0.4546(8) 0.8768(3) 0.1458(3) 0.0328(14) Uani 1 1 d . . . . .
H17A H -0.516841 0.855467 0.104451 0.039 Uiso 1 1 calc R U . . .
N18A N -0.0796(7) 0.8891(3) -0.0304(2) 0.0341(12) Uani 1 1 d . . . . .
H18A H -0.006076 0.911865 -0.043782 0.041 Uiso 1 1 calc R U . . .
C19A C -0.1915(9) 0.8376(4) -0.0755(3) 0.0380(15) Uani 1 1 d . . . . .
O20A O -0.3013(7) 0.8028(3) -0.0635(2) 0.0448(12) Uani 1 1 d . . . . .
C21A C -0.1670(12) 0.8262(4) -0.1423(3) 0.053(2) Uani 1 1 d . . . . .
H21A H -0.265566 0.798139 -0.171746 0.080 Uiso 1 1 calc R U . . .
H21B H -0.072547 0.801730 -0.149539 0.080 Uiso 1 1 calc R U . . .
H21C H -0.147114 0.871512 -0.148649 0.080 Uiso 1 1 calc R U . . .
N22A N 0.0215(6) 1.0245(2) 0.3404(2) 0.0216(9) Uani 1 1 d . . . . .
C23A C 0.0867(7) 0.9924(3) 0.3788(3) 0.0222(11) Uani 1 1 d . . . . .
C24A C 0.1281(7) 1.0223(3) 0.4424(3) 0.0235(11) Uani 1 1 d . . . . .
H24A H 0.173509 0.997504 0.468305 0.028 Uiso 1 1 calc R U . . .
C25A C 0.1006(7) 1.0914(3) 0.4677(3) 0.0261(12) Uani 1 1 d . . . . .
C26A C 0.0389(7) 1.1281(3) 0.4287(3) 0.0270(12) Uani 1 1 d . . . . .
H26A H 0.024748 1.175721 0.444807 0.032 Uiso 1 1 calc R U . . .
C27A C -0.0001(7) 1.0909(3) 0.3654(3) 0.0244(12) Uani 1 1 d . . . . .
N28A N 0.1133(6) 0.9248(3) 0.3439(2) 0.0240(10) Uani 1 1 d . . . . .
N29A N 0.0702(6) 0.9062(3) 0.2796(2) 0.0234(10) Uani 1 1 d . . . . .
C30A C 0.1123(8) 0.8429(3) 0.2578(3) 0.0317(13) Uani 1 1 d . . . . .
H30A H 0.095827 0.815900 0.214622 0.038 Uiso 1 1 calc R U . . .
C31A C 0.1831(9) 0.8217(4) 0.3064(3) 0.0365(15) Uani 1 1 d . . . . .
H31A H 0.222984 0.778690 0.302843 0.044 Uiso 1 1 calc R U . . .
C32A C 0.1844(8) 0.8754(3) 0.3612(3) 0.0329(14) Uani 1 1 d . . . . .
H32A H 0.226961 0.877141 0.402757 0.039 Uiso 1 1 calc R U . . .
N33A N -0.0622(6) 1.1175(3) 0.3177(2) 0.0256(10) Uani 1 1 d . . . . .
N34A N -0.0801(6) 1.0731(3) 0.2568(2) 0.0251(10) Uani 1 1 d . . . . .
C35A C -0.1292(7) 1.1102(3) 0.2208(3) 0.0296(13) Uani 1 1 d . . . . .
H35A H -0.151647 1.093158 0.176244 0.035 Uiso 1 1 calc R U . . .
C36A C -0.1435(8) 1.1776(3) 0.2571(3) 0.0326(13) Uani 1 1 d . . . . .
H36A H -0.176472 1.213944 0.242281 0.039 Uiso 1 1 calc R U . . .
C37A C -0.1004(8) 1.1809(3) 0.3183(3) 0.0316(13) Uani 1 1 d . . . . .
H37A H -0.097755 1.220239 0.354364 0.038 Uiso 1 1 calc R U . . .
N38A N 0.1499(7) 1.1215(3) 0.5330(2) 0.0314(12) Uani 1 1 d . . . . .
H38A H 0.197111 1.095300 0.552606 0.038 Uiso 1 1 calc R U . . .
C39A C 0.1330(8) 1.1876(4) 0.5702(3) 0.0352(14) Uani 1 1 d . . . . .
O40A O 0.0653(8) 1.2273(3) 0.5495(2) 0.0547(15) Uani 1 1 d . . . . .
C41A C 0.2086(9) 1.2044(4) 0.6378(3) 0.0432(17) Uani 1 1 d . . . . .
H41A H 0.154687 1.240193 0.663807 0.065 Uiso 1 1 calc R U . . .
H41B H 0.325801 1.221879 0.644405 0.065 Uiso 1 1 calc R U . . .
H41C H 0.194988 1.162138 0.649624 0.065 Uiso 1 1 calc R U . . .
Fe1B Fe 0.53242(11) 0.52776(5) 0.25026(4) 0.0246(2) Uani 1 1 d . . . . .
N2B N 0.5683(6) 0.5600(3) 0.3497(2) 0.0256(10) Uani 1 1 d . . . . .
C3B C 0.4482(7) 0.5462(3) 0.3787(3) 0.0258(12) Uani 1 1 d . . . . .
C4B C 0.4645(7) 0.5647(3) 0.4429(3) 0.0302(13) Uani 1 1 d . . . . .
H4B H 0.376933 0.553104 0.461886 0.036 Uiso 1 1 calc R U . . .
C5B C 0.6170(7) 0.6017(3) 0.4791(3) 0.0273(12) Uani 1 1 d . . . . .
C6B C 0.7440(7) 0.6165(3) 0.4497(3) 0.0276(12) Uani 1 1 d . . . . .
H6B H 0.847855 0.641383 0.473296 0.033 Uiso 1 1 calc R U . . .
C7B C 0.7126(7) 0.5935(3) 0.3852(3) 0.0266(12) Uani 1 1 d . . . . .
N8B N 0.3029(6) 0.5107(3) 0.3369(2) 0.0292(11) Uani 1 1 d . . . . .
N9B N 0.2976(6) 0.4987(3) 0.2737(2) 0.0301(11) Uani 1 1 d . . . . .
C10B C 0.1483(8) 0.4639(3) 0.2466(3) 0.0354(14) Uani 1 1 d . . . . .
H10B H 0.106921 0.448849 0.202690 0.042 Uiso 1 1 calc R U . . .
C11B C 0.0597(9) 0.4521(4) 0.2903(4) 0.0429(17) Uani 1 1 d . . . . .
H11B H -0.048099 0.427266 0.281980 0.052 Uiso 1 1 calc R U . . .
C12B C 0.1596(8) 0.4838(4) 0.3480(3) 0.0360(15) Uani 1 1 d . . . . .
H12B H 0.133708 0.486346 0.387729 0.043 Uiso 1 1 calc R U . . .
N13B N 0.8296(6) 0.6042(3) 0.3491(2) 0.0252(10) Uani 1 1 d . . . . .
N14B N 0.7800(6) 0.5847(3) 0.2856(2) 0.0290(11) Uani 1 1 d . . . . .
C15B C 0.9122(8) 0.6024(4) 0.2646(3) 0.0350(14) Uani 1 1 d . . . . .
H15B H 0.915295 0.595410 0.221633 0.042 Uiso 1 1 calc R U . . .
C16B C 1.0459(8) 0.6326(3) 0.3139(3) 0.0358(15) Uani 1 1 d . . . . .
H16B H 1.153638 0.649388 0.310963 0.043 Uiso 1 1 calc R U . . .
C17B C 0.9901(8) 0.6329(3) 0.3669(3) 0.0297(13) Uani 1 1 d . . . . .
H17B H 1.051796 0.650029 0.408559 0.036 Uiso 1 1 calc R U . . .
N18B N 0.6305(7) 0.6218(3) 0.5440(2) 0.0337(12) Uani 1 1 d . . . . .
H18B H 0.560045 0.598722 0.558370 0.040 Uiso 1 1 calc R U . . .
C19B C 0.7442(9) 0.6749(4) 0.5883(3) 0.0366(15) Uani 1 1 d . . . . .
O20B O 0.8504(6) 0.7082(3) 0.5742(2) 0.0437(12) Uani 1 1 d . . . . .
C21B C 0.7188(11) 0.6870(5) 0.6546(3) 0.051(2) Uani 1 1 d . . . . .
H21D H 0.817252 0.715153 0.684117 0.077 Uiso 1 1 calc R U . . .
H21E H 0.698069 0.641999 0.661426 0.077 Uiso 1 1 calc R U . . .
H21F H 0.624521 0.711770 0.661442 0.077 Uiso 1 1 calc R U . . .
N22B N 0.4609(6) 0.4731(3) 0.1534(2) 0.0235(10) Uani 1 1 d . . . . .
C23B C 0.4048(7) 0.5046(3) 0.1134(3) 0.0222(11) Uani 1 1 d . . . . .
C24B C 0.3596(7) 0.4725(3) 0.0494(3) 0.0263(12) Uani 1 1 d . . . . .
H24B H 0.320752 0.497402 0.022528 0.032 Uiso 1 1 calc R U . . .
C25B C 0.3732(7) 0.4018(3) 0.0258(3) 0.0257(12) Uani 1 1 d . . . . .
C26B C 0.4319(7) 0.3664(3) 0.0673(3) 0.0279(12) Uani 1 1 d . . . . .
H26B H 0.440675 0.318058 0.052501 0.033 Uiso 1 1 calc R U . . .
C27B C 0.4753(7) 0.4049(3) 0.1295(3) 0.0243(11) Uani 1 1 d . . . . .
N28B N 0.3943(6) 0.5752(3) 0.1437(2) 0.0254(10) Uani 1 1 d . . . . .
N29B N 0.4466(6) 0.6024(3) 0.2070(2) 0.0292(11) Uani 1 1 d . . . . .
C30B C 0.4136(9) 0.6672(3) 0.2221(3) 0.0370(15) Uani 1 1 d . . . . .
H30B H 0.438500 0.699588 0.263591 0.044 Uiso 1 1 calc R U . . .
C31B C 0.3380(9) 0.6822(4) 0.1700(3) 0.0424(17) Uani 1 1 d . . . . .
H31B H 0.302742 0.724918 0.169080 0.051 Uiso 1 1 calc R U . . .
C32B C 0.3257(8) 0.6220(3) 0.1204(3) 0.0326(14) Uani 1 1 d . . . . .
H32B H 0.278204 0.614370 0.077839 0.039 Uiso 1 1 calc R U . . .
N33B N 0.5333(6) 0.3775(3) 0.1769(2) 0.0255(10) Uani 1 1 d . . . . .
N34B N 0.5769(6) 0.4228(3) 0.2376(2) 0.0256(10) Uani 1 1 d . . . . .
C35B C 0.6147(8) 0.3826(4) 0.2719(3) 0.0314(13) Uani 1 1 d . . . . .
H35B H 0.649357 0.399149 0.316230 0.038 Uiso 1 1 calc R U . . .
C36B C 0.5968(9) 0.3123(4) 0.2343(3) 0.0415(16) Uani 1 1 d . . . . .
H36B H 0.616058 0.273795 0.248044 0.050 Uiso 1 1 calc R U . . .
C37B C 0.5461(9) 0.3104(4) 0.1740(3) 0.0384(15) Uani 1 1 d . . . . .
H37B H 0.524201 0.270288 0.137301 0.046 Uiso 1 1 calc R U . . .
N38B N 0.3223(7) 0.3695(3) -0.0385(2) 0.0329(12) Uani 1 1 d . . . . .
H38B H 0.276219 0.394909 -0.059234 0.039 Uiso 1 1 calc R U . . .
C39B C 0.3350(9) 0.3022(4) -0.0737(3) 0.0356(14) Uani 1 1 d . . . . .
O40B O 0.4030(8) 0.2626(3) -0.0521(2) 0.0493(14) Uani 1 1 d . . . . .
C41B C 0.2523(10) 0.2821(4) -0.1419(3) 0.0440(18) Uani 1 1 d . . . . .
H41D H 0.306209 0.246242 -0.167794 0.066 Uiso 1 1 calc R U . . .
H41E H 0.260812 0.323360 -0.155432 0.066 Uiso 1 1 calc R U . . .
H41F H 0.136395 0.263799 -0.146678 0.066 Uiso 1 1 calc R U . . .
Cl42 Cl 0.3534(2) 0.89685(9) -0.05994(7) 0.0367(3) Uani 1 1 d . . . . .
O43 O 0.3005(10) 0.8309(3) -0.1089(3) 0.075(2) Uani 1 1 d . . . . .
O44 O 0.5028(8) 0.9312(4) -0.0676(3) 0.0701(19) Uani 1 1 d . . . . .
O45 O 0.3768(6) 0.8864(3) -0.0001(2) 0.0423(12) Uani 1 1 d . . . . .
O46 O 0.2257(6) 0.9402(3) -0.0627(2) 0.0407(11) Uani 1 1 d . . . . .
Cl47 Cl 0.37142(18) 0.96846(9) 0.58055(7) 0.0324(3) Uani 1 1 d . . . . .
O48 O 0.5419(7) 0.9903(4) 0.5898(4) 0.081(2) Uani 1 1 d . . . . .
O49 O 0.2838(8) 1.0271(3) 0.5947(2) 0.0563(16) Uani 1 1 d . . . . .
O50 O 0.3434(6) 0.9300(3) 0.6217(2) 0.0489(14) Uani 1 1 d . . . . .
O51 O 0.3076(9) 0.9261(3) 0.5167(2) 0.0634(18) Uani 1 1 d . . . . .
Cl52 Cl 0.19282(19) 0.61182(9) 0.56822(7) 0.0347(3) Uani 1 1 d . . . . .
O53 O 0.3171(6) 0.5669(3) 0.5703(2) 0.0380(10) Uani 1 1 d . . . . .
O54 O 0.2652(9) 0.6819(3) 0.6064(3) 0.0646(18) Uani 1 1 d . . . . .
O55 O 0.0599(8) 0.5893(4) 0.5921(4) 0.073(2) Uani 1 1 d . . . . .
O56 O 0.1436(6) 0.6101(3) 0.5053(2) 0.0467(13) Uani 1 1 d . . . . .
Cl57 Cl 0.1306(2) 0.51817(9) -0.09717(7) 0.0354(3) Uani 1 1 d . . . . .
O58 O 0.1706(7) 0.5541(3) -0.1388(3) 0.0561(16) Uani 1 1 d . . . . .
O59 O 0.2141(8) 0.4573(3) -0.1084(3) 0.0599(17) Uani 1 1 d . . . . .
O60 O 0.1896(10) 0.5608(3) -0.0335(3) 0.073(2) Uani 1 1 d . . . . .
O61 O -0.0407(7) 0.4984(5) -0.1099(4) 0.082(2) Uani 1 1 d . . . . .
C62 C 0.5262(13) 0.7959(5) 0.5429(5) 0.076(3) Uani 1 1 d . . . . .
H62A H 0.607441 0.763856 0.536777 0.114 Uiso 1 1 calc R U . . .
H62B H 0.508878 0.808266 0.586332 0.114 Uiso 1 1 calc R U . . .
H62C H 0.566269 0.838307 0.534558 0.114 Uiso 1 1 calc R U . . .
C63 C 0.3711(11) 0.7620(5) 0.4999(5) 0.062(2) Uani 1 1 d . . . . .
H63A H 0.288373 0.794030 0.505958 0.075 Uiso 1 1 calc R U . . .
H63B H 0.329323 0.719396 0.508405 0.075 Uiso 1 1 calc R U . . .
C64 C 0.3996(12) 0.7431(5) 0.4336(4) 0.057(2) Uani 1 1 d . . . . .
N65 N 0.4184(10) 0.7265(5) 0.3833(4) 0.068(2) Uani 1 1 d . . . . .
C66A C 0.0036(15) 0.6944(7) -0.0576(6) 0.074(3) Uiso 0.83 1 d D . P A 1
H66A H 0.019788 0.673345 -0.100735 0.111 Uiso 0.83 1 calc R U P A 1
H66B H -0.046586 0.658089 -0.043260 0.111 Uiso 0.83 1 calc R U P A 1
H66C H -0.068542 0.729858 -0.056262 0.111 Uiso 0.83 1 calc R U P A 1
C67A C 0.1692(12) 0.7284(5) -0.0148(4) 0.053(2) Uiso 0.83 1 d D . P A 1
H67A H 0.242650 0.692612 -0.016707 0.063 Uiso 0.83 1 calc R U P A 1
H67B H 0.220672 0.764453 -0.029722 0.063 Uiso 0.83 1 calc R U P A 1
C68A C 0.1505(14) 0.7604(5) 0.0502(4) 0.045(2) Uiso 0.83 1 d D . P A 1
N69A N 0.1206(17) 0.7838(6) 0.1003(5) 0.058(3) Uiso 0.83 1 d D . P A 1
C66B C 0.096(6) 0.716(2) -0.0600(15) 0.044(10) Uiso 0.17 1 d D . P B 2
H66D H 0.045432 0.681570 -0.101109 0.067 Uiso 0.17 1 calc R U P B 2
H66E H 0.088455 0.763000 -0.061242 0.067 Uiso 0.17 1 calc R U P B 2
H66F H 0.211104 0.710494 -0.049648 0.067 Uiso 0.17 1 calc R U P B 2
C67B C 0.007(5) 0.703(2) -0.0110(15) 0.042(9) Uiso 0.17 1 d D . P B 2
H67C H -0.110378 0.707961 -0.021789 0.050 Uiso 0.17 1 calc R U P B 2
H67D H 0.012432 0.655385 -0.010179 0.050 Uiso 0.17 1 calc R U P B 2
C68B C 0.080(6) 0.754(2) 0.0520(13) 0.043(10) Uiso 0.17 1 d D . P B 2
N69B N 0.164(8) 0.789(3) 0.099(2) 0.07(2) Uiso 0.17 1 d D . P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1A N2A 1.896(5) . ?
Fe1A N9A 1.974(5) . ?
Fe1A N14A 2.000(5) . ?
Fe1A N22A 1.907(5) . ?
Fe1A N29A 1.990(5) . ?
Fe1A N34A 1.962(5) . ?
N2A C3A 1.337(8) . ?
N2A C7A 1.347(8) . ?
C3A C4A 1.368(8) . ?
C3A N8A 1.403(8) . ?
C4A H4A 0.9500 . ?
C4A C5A 1.401(9) . ?
C5A C6A 1.403(9) . ?
C5A N18A 1.388(8) . ?
C6A H6A 0.9500 . ?
C6A C7A 1.376(8) . ?
C7A N13A 1.413(8) . ?
N8A N9A 1.383(7) . ?
N8A C12A 1.373(8) . ?
N9A C10A 1.324(8) . ?
C10A H10A 0.9500 . ?
C10A C11A 1.400(9) . ?
C11A H11A 0.9500 . ?
C11A C12A 1.363(10) . ?
C12A H12A 0.9500 . ?
N13A N14A 1.388(7) . ?
N13A C17A 1.355(8) . ?
N14A C15A 1.320(8) . ?
C15A H15A 0.9500 . ?
C15A C16A 1.411(9) . ?
C16A H16A 0.9500 . ?
C16A C17A 1.359(10) . ?
C17A H17A 0.9500 . ?
N18A H18A 0.8800 . ?
N18A C19A 1.374(9) . ?
C19A O20A 1.219(9) . ?
C19A C21A 1.516(9) . ?
C21A H21A 0.9800 . ?
C21A H21B 0.9800 . ?
C21A H21C 0.9800 . ?
N22A C23A 1.330(8) . ?
N22A C27A 1.336(8) . ?
C23A C24A 1.361(8) . ?
C23A N28A 1.419(7) . ?
C24A H24A 0.9500 . ?
C24A C25A 1.402(8) . ?
C25A C26A 1.402(9) . ?
C25A N38A 1.401(7) . ?
C26A H26A 0.9500 . ?
C26A C27A 1.378(8) . ?
C27A N33A 1.411(8) . ?
N28A N29A 1.376(6) . ?
N28A C32A 1.343(8) . ?
N29A C30A 1.333(8) . ?
C30A H30A 0.9500 . ?
C30A C31A 1.383(10) . ?
C31A H31A 0.9500 . ?
C31A C32A 1.381(9) . ?
C32A H32A 0.9500 . ?
N33A N34A 1.379(7) . ?
N33A C37A 1.358(8) . ?
N34A C35A 1.324(8) . ?
C35A H35A 0.9500 . ?
C35A C36A 1.393(9) . ?
C36A H36A 0.9500 . ?
C36A C37A 1.366(9) . ?
C37A H37A 0.9500 . ?
N38A H38A 0.8800 . ?
N38A C39A 1.386(8) . ?
C39A O40A 1.198(9) . ?
C39A C41A 1.495(9) . ?
C41A H41A 0.9800 . ?
C41A H41B 0.9800 . ?
C41A H41C 0.9800 . ?
Fe1B N2B 2.121(5) . ?
Fe1B N9B 2.183(5) . ?
Fe1B N14B 2.173(5) . ?
Fe1B N22B 2.106(5) . ?
Fe1B N29B 2.173(5) . ?
Fe1B N34B 2.143(5) . ?
N2B C3B 1.335(8) . ?
N2B C7B 1.333(8) . ?
C3B C4B 1.376(8) . ?
C3B N8B 1.399(8) . ?
C4B H4B 0.9500 . ?
C4B C5B 1.408(9) . ?
C5B C6B 1.393(9) . ?
C5B N18B 1.393(8) . ?
C6B H6B 0.9500 . ?
C6B C7B 1.374(8) . ?
C7B N13B 1.412(8) . ?
N8B N9B 1.379(7) . ?
N8B C12B 1.359(8) . ?
N9B C10B 1.327(8) . ?
C10B H10B 0.9500 . ?
C10B C11B 1.391(10) . ?
C11B H11B 0.9500 . ?
C11B C12B 1.372(10) . ?
C12B H12B 0.9500 . ?
N13B N14B 1.363(7) . ?
N13B C17B 1.356(8) . ?
N14B C15B 1.329(8) . ?
C15B H15B 0.9500 . ?
C15B C16B 1.396(10) . ?
C16B H16B 0.9500 . ?
C16B C17B 1.358(9) . ?
C17B H17B 0.9500 . ?
N18B H18B 0.8800 . ?
N18B C19B 1.388(9) . ?
C19B O20B 1.207(9) . ?
C19B C21B 1.507(9) . ?
C21B H21D 0.9800 . ?
C21B H21E 0.9800 . ?
C21B H21F 0.9800 . ?
N22B C23B 1.324(7) . ?
N22B C27B 1.349(8) . ?
C23B C24B 1.377(8) . ?
C23B N28B 1.409(7) . ?
C24B H24B 0.9500 . ?
C24B C25B 1.394(9) . ?
C25B C26B 1.417(9) . ?
C25B N38B 1.387(7) . ?
C26B H26B 0.9500 . ?
C26B C27B 1.365(8) . ?
C27B N33B 1.410(7) . ?
N28B N29B 1.360(7) . ?
N28B C32B 1.357(8) . ?
N29B C30B 1.323(8) . ?
C30B H30B 0.9500 . ?
C30B C31B 1.392(10) . ?
C31B H31B 0.9500 . ?
C31B C32B 1.371(9) . ?
C32B H32B 0.9500 . ?
N33B N34B 1.375(7) . ?
N33B C37B 1.363(8) . ?
N34B C35B 1.325(8) . ?
C35B H35B 0.9500 . ?
C35B C36B 1.402(10) . ?
C36B H36B 0.9500 . ?
C36B C37B 1.363(10) . ?
C37B H37B 0.9500 . ?
N38B H38B 0.8800 . ?
N38B C39B 1.381(8) . ?
C39B O40B 1.212(9) . ?
C39B C41B 1.513(9) . ?
C41B H41D 0.9800 . ?
C41B H41E 0.9800 . ?
C41B H41F 0.9800 . ?
Cl42 O43 1.434(6) . ?
Cl42 O44 1.431(6) . ?
Cl42 O45 1.434(5) . ?
Cl42 O46 1.452(5) . ?
Cl47 O48 1.412(6) . ?
Cl47 O49 1.436(5) . ?
Cl47 O50 1.427(5) . ?
Cl47 O51 1.433(5) . ?
Cl52 O53 1.451(5) . ?
Cl52 O54 1.437(6) . ?
Cl52 O55 1.406(6) . ?
Cl52 O56 1.422(5) . ?
Cl57 O58 1.424(6) . ?
Cl57 O59 1.453(6) . ?
Cl57 O60 1.424(6) . ?
Cl57 O61 1.407(6) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C62 C63 1.463(13) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C63 C64 1.503(14) . ?
C64 N65 1.130(12) . ?
C66A H66A 0.9800 . ?
C66A H66B 0.9800 . ?
C66A H66C 0.9800 . ?
C66A C67A 1.527(13) . ?
C67A H67A 0.9900 . ?
C67A H67B 0.9900 . ?
C67A C68A 1.462(11) . ?
C68A N69A 1.170(11) . ?
C66B H66D 0.9800 . ?
C66B H66E 0.9800 . ?
C66B H66F 0.9800 . ?
C66B C67B 1.50(2) . ?
C67B H67C 0.9900 . ?
C67B H67D 0.9900 . ?
C67B C68B 1.486(19) . ?
C68B N69B 1.16(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2A Fe1A N9A 79.8(2) . . ?
N2A Fe1A N14A 79.8(2) . . ?
N2A Fe1A N22A 173.4(2) . . ?
N2A Fe1A N29A 104.9(2) . . ?
N2A Fe1A N34A 95.9(2) . . ?
N9A Fe1A N14A 159.6(2) . . ?
N9A Fe1A N29A 91.5(2) . . ?
N22A Fe1A N9A 95.1(2) . . ?
N22A Fe1A N14A 105.3(2) . . ?
N22A Fe1A N29A 79.19(19) . . ?
N22A Fe1A N34A 79.9(2) . . ?
N29A Fe1A N14A 93.3(2) . . ?
N34A Fe1A N9A 89.6(2) . . ?
N34A Fe1A N14A 92.9(2) . . ?
N34A Fe1A N29A 159.1(2) . . ?
C3A N2A Fe1A 121.0(4) . . ?
C3A N2A C7A 117.3(5) . . ?
C7A N2A Fe1A 121.4(4) . . ?
N2A C3A C4A 124.0(6) . . ?
N2A C3A N8A 109.9(5) . . ?
C4A C3A N8A 126.1(6) . . ?
C3A C4A H4A 121.5 . . ?
C3A C4A C5A 117.0(6) . . ?
C5A C4A H4A 121.5 . . ?
C4A C5A C6A 121.2(5) . . ?
N18A C5A C4A 117.1(6) . . ?
N18A C5A C6A 121.6(6) . . ?
C5A C6A H6A 122.3 . . ?
C7A C6A C5A 115.5(6) . . ?
C7A C6A H6A 122.3 . . ?
N2A C7A C6A 124.9(6) . . ?
N2A C7A N13A 109.7(5) . . ?
C6A C7A N13A 125.3(6) . . ?
N9A N8A C3A 116.8(5) . . ?
C12A N8A C3A 132.9(5) . . ?
C12A N8A N9A 110.2(5) . . ?
N8A N9A Fe1A 112.4(4) . . ?
C10A N9A Fe1A 141.6(4) . . ?
C10A N9A N8A 105.8(5) . . ?
N9A C10A H10A 124.7 . . ?
N9A C10A C11A 110.6(6) . . ?
C11A C10A H10A 124.7 . . ?
C10A C11A H11A 126.6 . . ?
C12A C11A C10A 106.8(6) . . ?
C12A C11A H11A 126.6 . . ?
N8A C12A H12A 126.7 . . ?
C11A C12A N8A 106.6(6) . . ?
C11A C12A H12A 126.7 . . ?
N14A N13A C7A 117.1(5) . . ?
C17A N13A C7A 132.4(5) . . ?
C17A N13A N14A 110.5(5) . . ?
N13A N14A Fe1A 111.8(4) . . ?
C15A N14A Fe1A 142.5(4) . . ?
C15A N14A N13A 105.6(5) . . ?
N14A C15A H15A 124.9 . . ?
N14A C15A C16A 110.3(6) . . ?
C16A C15A H15A 124.9 . . ?
C15A C16A H16A 126.8 . . ?
C17A C16A C15A 106.4(6) . . ?
C17A C16A H16A 126.8 . . ?
N13A C17A C16A 107.2(6) . . ?
N13A C17A H17A 126.4 . . ?
C16A C17A H17A 126.4 . . ?
C5A N18A H18A 116.6 . . ?
C19A N18A C5A 126.9(6) . . ?
C19A N18A H18A 116.6 . . ?
N18A C19A C21A 114.6(7) . . ?
O20A C19A N18A 123.3(6) . . ?
O20A C19A C21A 122.0(7) . . ?
C19A C21A H21A 109.5 . . ?
C19A C21A H21B 109.5 . . ?
C19A C21A H21C 109.5 . . ?
H21A C21A H21B 109.5 . . ?
H21A C21A H21C 109.5 . . ?
H21B C21A H21C 109.5 . . ?
C23A N22A Fe1A 121.2(4) . . ?
C23A N22A C27A 118.1(5) . . ?
C27A N22A Fe1A 120.2(4) . . ?
N22A C23A C24A 124.1(5) . . ?
N22A C23A N28A 110.3(5) . . ?
C24A C23A N28A 125.6(5) . . ?
C23A C24A H24A 121.6 . . ?
C23A C24A C25A 116.9(5) . . ?
C25A C24A H24A 121.6 . . ?
C26A C25A C24A 120.9(5) . . ?
N38A C25A C24A 115.4(6) . . ?
N38A C25A C26A 123.5(6) . . ?
C25A C26A H26A 122.1 . . ?
C27A C26A C25A 115.8(6) . . ?
C27A C26A H26A 122.1 . . ?
N22A C27A C26A 124.2(6) . . ?
N22A C27A N33A 110.3(5) . . ?
C26A C27A N33A 125.4(5) . . ?
N29A N28A C23A 116.0(5) . . ?
C32A N28A C23A 132.1(5) . . ?
C32A N28A N29A 111.6(5) . . ?
N28A N29A Fe1A 113.1(3) . . ?
C30A N29A Fe1A 142.0(4) . . ?
C30A N29A N28A 104.7(5) . . ?
N29A C30A H30A 124.5 . . ?
N29A C30A C31A 111.1(6) . . ?
C31A C30A H30A 124.5 . . ?
C30A C31A H31A 126.9 . . ?
C32A C31A C30A 106.3(6) . . ?
C32A C31A H31A 126.9 . . ?
N28A C32A C31A 106.3(6) . . ?
N28A C32A H32A 126.9 . . ?
C31A C32A H32A 126.9 . . ?
N34A N33A C27A 116.2(5) . . ?
C37A N33A C27A 133.3(5) . . ?
C37A N33A N34A 110.4(5) . . ?
N33A N34A Fe1A 113.2(4) . . ?
C35A N34A Fe1A 141.2(4) . . ?
C35A N34A N33A 105.4(5) . . ?
N34A C35A H35A 124.5 . . ?
N34A C35A C36A 111.0(6) . . ?
C36A C35A H35A 124.5 . . ?
C35A C36A H36A 126.9 . . ?
C37A C36A C35A 106.1(6) . . ?
C37A C36A H36A 126.9 . . ?
N33A C37A C36A 107.0(6) . . ?
N33A C37A H37A 126.5 . . ?
C36A C37A H37A 126.5 . . ?
C25A N38A H38A 116.2 . . ?
C39A N38A C25A 127.5(6) . . ?
C39A N38A H38A 116.2 . . ?
N38A C39A C41A 113.4(6) . . ?
O40A C39A N38A 122.7(6) . . ?
O40A C39A C41A 123.9(6) . . ?
C39A C41A H41A 109.5 . . ?
C39A C41A H41B 109.5 . . ?
C39A C41A H41C 109.5 . . ?
H41A C41A H41B 109.5 . . ?
H41A C41A H41C 109.5 . . ?
H41B C41A H41C 109.5 . . ?
N2B Fe1B N9B 73.31(19) . . ?
N2B Fe1B N14B 73.30(19) . . ?
N2B Fe1B N29B 116.15(19) . . ?
N2B Fe1B N34B 95.86(19) . . ?
N14B Fe1B N9B 146.17(19) . . ?
N14B Fe1B N29B 94.4(2) . . ?
N22B Fe1B N2B 165.2(2) . . ?
N22B Fe1B N9B 95.25(19) . . ?
N22B Fe1B N14B 118.58(19) . . ?
N22B Fe1B N29B 73.53(19) . . ?
N22B Fe1B N34B 73.88(19) . . ?
N29B Fe1B N9B 95.4(2) . . ?
N34B Fe1B N9B 87.63(19) . . ?
N34B Fe1B N14B 100.97(19) . . ?
N34B Fe1B N29B 147.40(19) . . ?
C3B N2B Fe1B 121.1(4) . . ?
C7B N2B Fe1B 121.1(4) . . ?
C7B N2B C3B 117.8(5) . . ?
N2B C3B C4B 123.9(5) . . ?
N2B C3B N8B 112.9(5) . . ?
C4B C3B N8B 123.2(5) . . ?
C3B C4B H4B 121.6 . . ?
C3B C4B C5B 116.8(5) . . ?
C5B C4B H4B 121.6 . . ?
C6B C5B C4B 120.2(5) . . ?
C6B C5B N18B 123.6(5) . . ?
N18B C5B C4B 116.3(5) . . ?
C5B C6B H6B 121.5 . . ?
C7B C6B C5B 117.0(5) . . ?
C7B C6B H6B 121.5 . . ?
N2B C7B C6B 124.2(6) . . ?
N2B C7B N13B 112.3(5) . . ?
C6B C7B N13B 123.4(5) . . ?
N9B N8B C3B 118.1(5) . . ?
C12B N8B C3B 130.2(6) . . ?
C12B N8B N9B 111.7(5) . . ?
N8B N9B Fe1B 114.2(4) . . ?
C10B N9B Fe1B 140.9(5) . . ?
C10B N9B N8B 104.2(5) . . ?
N9B C10B H10B 124.1 . . ?
N9B C10B C11B 111.8(6) . . ?
C11B C10B H10B 124.1 . . ?
C10B C11B H11B 127.0 . . ?
C12B C11B C10B 106.0(6) . . ?
C12B C11B H11B 127.0 . . ?
N8B C12B C11B 106.2(6) . . ?
N8B C12B H12B 126.9 . . ?
C11B C12B H12B 126.9 . . ?
N14B N13B C7B 118.2(5) . . ?
C17B N13B C7B 130.6(5) . . ?
C17B N13B N14B 111.3(5) . . ?
N13B N14B Fe1B 114.7(4) . . ?
C15B N14B Fe1B 140.0(4) . . ?
C15B N14B N13B 104.9(5) . . ?
N14B C15B H15B 124.5 . . ?
N14B C15B C16B 111.1(6) . . ?
C16B C15B H15B 124.5 . . ?
C15B C16B H16B 127.1 . . ?
C17B C16B C15B 105.8(6) . . ?
C17B C16B H16B 127.1 . . ?
N13B C17B C16B 107.0(6) . . ?
N13B C17B H17B 126.5 . . ?
C16B C17B H17B 126.5 . . ?
C5B N18B H18B 116.8 . . ?
C19B N18B C5B 126.3(6) . . ?
C19B N18B H18B 116.8 . . ?
N18B C19B C21B 113.3(6) . . ?
O20B C19B N18B 122.6(6) . . ?
O20B C19B C21B 124.1(7) . . ?
C19B C21B H21D 109.5 . . ?
C19B C21B H21E 109.5 . . ?
C19B C21B H21F 109.5 . . ?
H21D C21B H21E 109.5 . . ?
H21D C21B H21F 109.5 . . ?
H21E C21B H21F 109.5 . . ?
C23B N22B Fe1B 121.4(4) . . ?
C23B N22B C27B 117.4(5) . . ?
C27B N22B Fe1B 121.1(4) . . ?
N22B C23B C24B 124.5(5) . . ?
N22B C23B N28B 112.3(5) . . ?
C24B C23B N28B 123.2(5) . . ?
C23B C24B H24B 121.4 . . ?
C23B C24B C25B 117.1(5) . . ?
C25B C24B H24B 121.4 . . ?
C24B C25B C26B 119.9(5) . . ?
N38B C25B C24B 116.6(5) . . ?
N38B C25B C26B 123.5(6) . . ?
C25B C26B H26B 121.6 . . ?
C27B C26B C25B 116.8(6) . . ?
C27B C26B H26B 121.6 . . ?
N22B C27B C26B 124.2(5) . . ?
N22B C27B N33B 111.8(5) . . ?
C26B C27B N33B 124.0(6) . . ?
N29B N28B C23B 118.5(5) . . ?
C32B N28B C23B 129.8(5) . . ?
C32B N28B N29B 111.4(5) . . ?
N28B N29B Fe1B 114.1(4) . . ?
C30B N29B Fe1B 140.8(5) . . ?
C30B N29B N28B 104.7(5) . . ?
N29B C30B H30B 124.0 . . ?
N29B C30B C31B 112.0(6) . . ?
C31B C30B H30B 124.0 . . ?
C30B C31B H31B 127.5 . . ?
C32B C31B C30B 105.0(6) . . ?
C32B C31B H31B 127.5 . . ?
N28B C32B C31B 106.8(6) . . ?
N28B C32B H32B 126.6 . . ?
C31B C32B H32B 126.6 . . ?
N34B N33B C27B 117.8(5) . . ?
C37B N33B C27B 130.4(5) . . ?
C37B N33B N34B 111.7(5) . . ?
N33B N34B Fe1B 115.3(4) . . ?
C35B N34B Fe1B 139.2(4) . . ?
C35B N34B N33B 104.6(5) . . ?
N34B C35B H35B 124.4 . . ?
N34B C35B C36B 111.2(6) . . ?
C36B C35B H35B 124.4 . . ?
C35B C36B H36B 126.8 . . ?
C37B C36B C35B 106.3(6) . . ?
C37B C36B H36B 126.8 . . ?
N33B C37B C36B 106.1(6) . . ?
N33B C37B H37B 126.9 . . ?
C36B C37B H37B 126.9 . . ?
C25B N38B H38B 116.1 . . ?
C39B N38B C25B 127.8(6) . . ?
C39B N38B H38B 116.1 . . ?
N38B C39B C41B 113.5(6) . . ?
O40B C39B N38B 123.4(6) . . ?
O40B C39B C41B 123.1(6) . . ?
C39B C41B H41D 109.5 . . ?
C39B C41B H41E 109.5 . . ?
C39B C41B H41F 109.5 . . ?
H41D C41B H41E 109.5 . . ?
H41D C41B H41F 109.5 . . ?
H41E C41B H41F 109.5 . . ?
O43 Cl42 O45 109.7(4) . . ?
O43 Cl42 O46 108.1(4) . . ?
O44 Cl42 O43 111.0(5) . . ?
O44 Cl42 O45 109.7(4) . . ?
O44 Cl42 O46 109.3(4) . . ?
O45 Cl42 O46 109.0(3) . . ?
O48 Cl47 O49 111.4(5) . . ?
O48 Cl47 O50 108.5(4) . . ?
O48 Cl47 O51 110.9(5) . . ?
O50 Cl47 O49 108.2(4) . . ?
O50 Cl47 O51 110.2(4) . . ?
O51 Cl47 O49 107.6(4) . . ?
O54 Cl52 O53 107.9(3) . . ?
O55 Cl52 O53 109.2(4) . . ?
O55 Cl52 O54 110.1(5) . . ?
O55 Cl52 O56 111.7(4) . . ?
O56 Cl52 O53 109.0(3) . . ?
O56 Cl52 O54 108.9(4) . . ?
O58 Cl57 O59 107.9(4) . . ?
O60 Cl57 O58 110.7(4) . . ?
O60 Cl57 O59 107.2(4) . . ?
O61 Cl57 O58 108.2(4) . . ?
O61 Cl57 O59 111.0(5) . . ?
O61 Cl57 O60 111.8(5) . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C63 C62 H62A 109.5 . . ?
C63 C62 H62B 109.5 . . ?
C63 C62 H62C 109.5 . . ?
C62 C63 H63A 109.9 . . ?
C62 C63 H63B 109.9 . . ?
C62 C63 C64 108.9(9) . . ?
H63A C63 H63B 108.3 . . ?
C64 C63 H63A 109.9 . . ?
C64 C63 H63B 109.9 . . ?
N65 C64 C63 177.5(11) . . ?
H66A C66A H66B 109.5 . . ?
H66A C66A H66C 109.5 . . ?
H66B C66A H66C 109.5 . . ?
C67A C66A H66A 109.5 . . ?
C67A C66A H66B 109.5 . . ?
C67A C66A H66C 109.5 . . ?
C66A C67A H67A 109.4 . . ?
C66A C67A H67B 109.4 . . ?
H67A C67A H67B 108.0 . . ?
C68A C67A C66A 111.2(9) . . ?
C68A C67A H67A 109.4 . . ?
C68A C67A H67B 109.4 . . ?
N69A C68A C67A 173.9(13) . . ?
H66D C66B H66E 109.5 . . ?
H66D C66B H66F 109.5 . . ?
H66E C66B H66F 109.5 . . ?
C67B C66B H66D 109.5 . . ?
C67B C66B H66E 109.5 . . ?
C67B C66B H66F 109.5 . . ?
C66B C67B H67C 109.5 . . ?
C66B C67B H67D 109.5 . . ?
H67C C67B H67D 108.1 . . ?
C68B C67B C66B 111(2) . . ?
C68B C67B H67C 109.5 . . ?
C68B C67B H67D 109.5 . . ?
N69B C68B C67B 167(6) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N18A H18A O46 0.88 2.11 2.941(8) 157.2 . yes
N38A H38A O49 0.88 2.05 2.923(8) 173.8 . yes
N18B H18B O53 0.88 2.15 2.963(7) 153.1 . yes
N38B H38B O59 0.88 1.99 2.863(8) 169.3 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1A N2A C3A C4A -175.6(5) . . . . ?
Fe1A N2A C3A N8A 3.2(7) . . . . ?
Fe1A N2A C7A C6A 175.7(5) . . . . ?
Fe1A N2A C7A N13A -1.7(7) . . . . ?
Fe1A N9A C10A C11A -173.4(5) . . . . ?
Fe1A N14A C15A C16A 176.3(5) . . . . ?
Fe1A N22A C23A C24A 174.0(4) . . . . ?
Fe1A N22A C23A N28A -3.4(6) . . . . ?
Fe1A N22A C27A C26A -172.8(5) . . . . ?
Fe1A N22A C27A N33A 5.1(6) . . . . ?
Fe1A N29A C30A C31A 172.5(5) . . . . ?
Fe1A N34A C35A C36A -174.5(5) . . . . ?
N2A C3A C4A C5A -0.4(9) . . . . ?
N2A C3A N8A N9A -0.3(7) . . . . ?
N2A C3A N8A C12A -178.0(6) . . . . ?
N2A C7A N13A N14A -1.5(7) . . . . ?
N2A C7A N13A C17A 179.8(6) . . . . ?
C3A N2A C7A C6A 1.7(9) . . . . ?
C3A N2A C7A N13A -175.7(5) . . . . ?
C3A C4A C5A C6A 2.5(9) . . . . ?
C3A C4A C5A N18A -178.5(6) . . . . ?
C3A N8A N9A Fe1A -2.4(6) . . . . ?
C3A N8A N9A C10A -178.5(5) . . . . ?
C3A N8A C12A C11A 177.5(6) . . . . ?
C4A C3A N8A N9A 178.5(6) . . . . ?
C4A C3A N8A C12A 0.8(11) . . . . ?
C4A C5A C6A C7A -2.3(9) . . . . ?
C4A C5A N18A C19A 161.2(7) . . . . ?
C5A C6A C7A N2A 0.2(9) . . . . ?
C5A C6A C7A N13A 177.2(6) . . . . ?
C5A N18A C19A O20A 1.2(12) . . . . ?
C5A N18A C19A C21A -178.0(7) . . . . ?
C6A C5A N18A C19A -19.7(10) . . . . ?
C6A C7A N13A N14A -178.9(6) . . . . ?
C6A C7A N13A C17A 2.4(11) . . . . ?
C7A N2A C3A C4A -1.6(9) . . . . ?
C7A N2A C3A N8A 177.3(5) . . . . ?
C7A N13A N14A Fe1A 3.7(6) . . . . ?
C7A N13A N14A C15A -178.7(5) . . . . ?
C7A N13A C17A C16A 178.4(6) . . . . ?
N8A C3A C4A C5A -179.1(6) . . . . ?
N8A N9A C10A C11A 0.8(7) . . . . ?
N9A Fe1A N2A C3A -3.7(5) . . . . ?
N9A Fe1A N2A C7A -177.5(5) . . . . ?
N9A N8A C12A C11A -0.3(7) . . . . ?
N9A C10A C11A C12A -1.0(8) . . . . ?
C10A C11A C12A N8A 0.8(8) . . . . ?
C12A N8A N9A Fe1A 175.8(4) . . . . ?
C12A N8A N9A C10A -0.4(7) . . . . ?
N13A N14A C15A C16A -0.1(7) . . . . ?
N14A Fe1A N2A C3A 176.8(5) . . . . ?
N14A Fe1A N2A C7A 3.0(5) . . . . ?
N14A N13A C17A C16A -0.4(7) . . . . ?
N14A C15A C16A C17A -0.1(8) . . . . ?
C15A C16A C17A N13A 0.3(8) . . . . ?
C17A N13A N14A Fe1A -177.3(4) . . . . ?
C17A N13A N14A C15A 0.3(7) . . . . ?
N18A C5A C6A C7A 178.7(6) . . . . ?
N22A C23A C24A C25A -0.7(9) . . . . ?
N22A C23A N28A N29A 0.8(7) . . . . ?
N22A C23A N28A C32A 175.3(6) . . . . ?
N22A C27A N33A N34A -3.2(7) . . . . ?
N22A C27A N33A C37A -178.2(6) . . . . ?
C23A N22A C27A C26A -1.0(9) . . . . ?
C23A N22A C27A N33A 176.9(5) . . . . ?
C23A C24A C25A C26A -2.2(9) . . . . ?
C23A C24A C25A N38A -177.8(5) . . . . ?
C23A N28A N29A Fe1A 1.9(6) . . . . ?
C23A N28A N29A C30A 177.6(5) . . . . ?
C23A N28A C32A C31A -176.7(6) . . . . ?
C24A C23A N28A N29A -176.5(5) . . . . ?
C24A C23A N28A C32A -1.9(10) . . . . ?
C24A C25A C26A C27A 3.3(9) . . . . ?
C24A C25A N38A C39A -177.9(6) . . . . ?
C25A C26A C27A N22A -1.7(9) . . . . ?
C25A C26A C27A N33A -179.3(5) . . . . ?
C25A N38A C39A O40A 2.9(12) . . . . ?
C25A N38A C39A C41A -176.5(6) . . . . ?
C26A C25A N38A C39A 6.6(10) . . . . ?
C26A C27A N33A N34A 174.7(5) . . . . ?
C26A C27A N33A C37A -0.3(10) . . . . ?
C27A N22A C23A C24A 2.2(8) . . . . ?
C27A N22A C23A N28A -175.1(5) . . . . ?
C27A N33A N34A Fe1A 0.1(6) . . . . ?
C27A N33A N34A C35A -176.2(5) . . . . ?
C27A N33A C37A C36A 175.3(6) . . . . ?
N28A C23A C24A C25A 176.2(5) . . . . ?
N28A N29A C30A C31A -1.1(7) . . . . ?
N29A Fe1A N2A C3A -92.5(5) . . . . ?
N29A Fe1A N2A C7A 93.7(5) . . . . ?
N29A N28A C32A C31A -1.9(7) . . . . ?
N29A C30A C31A C32A 0.0(8) . . . . ?
C30A C31A C32A N28A 1.2(8) . . . . ?
C32A N28A N29A Fe1A -173.8(4) . . . . ?
C32A N28A N29A C30A 1.9(7) . . . . ?
N33A N34A C35A C36A 0.0(7) . . . . ?
N34A Fe1A N2A C3A 84.8(5) . . . . ?
N34A Fe1A N2A C7A -89.0(5) . . . . ?
N34A N33A C37A C36A 0.0(7) . . . . ?
N34A C35A C36A C37A 0.0(7) . . . . ?
C35A C36A C37A N33A 0.0(7) . . . . ?
C37A N33A N34A Fe1A 176.2(4) . . . . ?
C37A N33A N34A C35A 0.0(6) . . . . ?
N38A C25A C26A C27A 178.5(5) . . . . ?
Fe1B N2B C3B C4B 179.0(5) . . . . ?
Fe1B N2B C3B N8B -0.9(7) . . . . ?
Fe1B N2B C7B C6B 179.3(5) . . . . ?
Fe1B N2B C7B N13B 0.5(7) . . . . ?
Fe1B N9B C10B C11B 167.6(6) . . . . ?
Fe1B N14B C15B C16B -171.3(5) . . . . ?
Fe1B N22B C23B C24B 178.4(5) . . . . ?
Fe1B N22B C23B N28B -2.3(7) . . . . ?
Fe1B N22B C27B C26B -179.8(5) . . . . ?
Fe1B N22B C27B N33B 3.1(7) . . . . ?
Fe1B N29B C30B C31B -171.6(6) . . . . ?
Fe1B N34B C35B C36B 168.6(5) . . . . ?
N2B C3B C4B C5B 1.5(10) . . . . ?
N2B C3B N8B N9B -4.1(8) . . . . ?
N2B C3B N8B C12B 174.9(6) . . . . ?
N2B C7B N13B N14B 4.7(8) . . . . ?
N2B C7B N13B C17B -176.6(6) . . . . ?
C3B N2B C7B C6B -1.9(9) . . . . ?
C3B N2B C7B N13B 179.4(5) . . . . ?
C3B C4B C5B C6B -1.4(9) . . . . ?
C3B C4B C5B N18B 178.2(6) . . . . ?
C3B N8B N9B Fe1B 6.9(7) . . . . ?
C3B N8B N9B C10B 179.2(6) . . . . ?
C3B N8B C12B C11B -177.8(7) . . . . ?
C4B C3B N8B N9B 176.1(6) . . . . ?
C4B C3B N8B C12B -4.9(11) . . . . ?
C4B C5B C6B C7B -0.1(9) . . . . ?
C4B C5B N18B C19B -159.0(6) . . . . ?
C5B C6B C7B N2B 1.8(10) . . . . ?
C5B C6B C7B N13B -179.5(6) . . . . ?
C5B N18B C19B O20B -2.9(11) . . . . ?
C5B N18B C19B C21B 175.9(6) . . . . ?
C6B C5B N18B C19B 20.6(10) . . . . ?
C6B C7B N13B N14B -174.1(6) . . . . ?
C6B C7B N13B C17B 4.6(10) . . . . ?
C7B N2B C3B C4B 0.1(9) . . . . ?
C7B N2B C3B N8B -179.7(5) . . . . ?
C7B N13B N14B Fe1B -7.4(6) . . . . ?
C7B N13B N14B C15B 178.4(5) . . . . ?
C7B N13B C17B C16B -178.3(6) . . . . ?
N8B C3B C4B C5B -178.7(6) . . . . ?
N8B N9B C10B C11B -1.2(8) . . . . ?
N9B N8B C12B C11B 1.3(8) . . . . ?
N9B C10B C11B C12B 2.0(9) . . . . ?
C10B C11B C12B N8B -1.9(8) . . . . ?
C12B N8B N9B Fe1B -172.3(4) . . . . ?
C12B N8B N9B C10B -0.1(7) . . . . ?
N13B N14B C15B C16B 0.4(7) . . . . ?
N14B N13B C17B C16B 0.5(7) . . . . ?
N14B C15B C16B C17B -0.1(8) . . . . ?
C15B C16B C17B N13B -0.2(7) . . . . ?
C17B N13B N14B Fe1B 173.6(4) . . . . ?
C17B N13B N14B C15B -0.5(7) . . . . ?
N18B C5B C6B C7B -179.7(6) . . . . ?
N22B C23B C24B C25B 0.5(9) . . . . ?
N22B C23B N28B N29B 2.6(7) . . . . ?
N22B C23B N28B C32B -171.3(6) . . . . ?
N22B C27B N33B N34B -4.6(7) . . . . ?
N22B C27B N33B C37B 171.1(6) . . . . ?
C23B N22B C27B C26B -1.8(9) . . . . ?
C23B N22B C27B N33B -178.9(5) . . . . ?
C23B C24B C25B C26B -0.1(9) . . . . ?
C23B C24B C25B N38B 177.9(5) . . . . ?
C23B N28B N29B Fe1B -1.7(6) . . . . ?
C23B N28B N29B C30B -176.7(6) . . . . ?
C23B N28B C32B C31B 175.9(6) . . . . ?
C24B C23B N28B N29B -178.2(5) . . . . ?
C24B C23B N28B C32B 8.0(10) . . . . ?
C24B C25B C26B C27B -1.1(9) . . . . ?
C24B C25B N38B C39B 174.4(7) . . . . ?
C25B C26B C27B N22B 2.1(9) . . . . ?
C25B C26B C27B N33B 178.9(5) . . . . ?
C25B N38B C39B O40B -3.9(12) . . . . ?
C25B N38B C39B C41B 174.7(6) . . . . ?
C26B C25B N38B C39B -7.6(11) . . . . ?
C26B C27B N33B N34B 178.2(6) . . . . ?
C26B C27B N33B C37B -6.0(10) . . . . ?
C27B N22B C23B C24B 0.4(9) . . . . ?
C27B N22B C23B N28B 179.7(5) . . . . ?
C27B N33B N34B Fe1B 4.1(6) . . . . ?
C27B N33B N34B C35B 175.7(5) . . . . ?
C27B N33B C37B C36B -175.0(6) . . . . ?
N28B C23B C24B C25B -178.7(5) . . . . ?
N28B N29B C30B C31B 1.1(8) . . . . ?
N29B N28B C32B C31B 1.7(8) . . . . ?
N29B C30B C31B C32B -0.1(9) . . . . ?
C30B C31B C32B N28B -0.9(8) . . . . ?
C32B N28B N29B Fe1B 173.2(4) . . . . ?
C32B N28B N29B C30B -1.8(7) . . . . ?
N33B N34B C35B C36B 0.3(7) . . . . ?
N34B N33B C37B C36B 0.9(8) . . . . ?
N34B C35B C36B C37B 0.3(8) . . . . ?
C35B C36B C37B N33B -0.7(8) . . . . ?
C37B N33B N34B Fe1B -172.4(4) . . . . ?
C37B N33B N34B C35B -0.8(7) . . . . ?
N38B C25B C26B C27B -179.0(6) . . . . ?
C66B C67B C68B N69B -55(25) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.6094(12)
2 0.3906(12)

_twin_special_details            
;
Component 2 rotated by 179.9209° 
 around [-0.00 0.00 1.00] (reciprocal) or [0.42 0.31 0.85] (direct)
;
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: propionitrile/diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_etcnmamt
_database_code_depnum_ccdc_archive 'CCDC 2078659'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2021-04-19 deposited with the CCDC.	2021-06-10 downloaded from the CCDC.
;
_audit_creation_date             2020-07-24
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis-[N-(2,6-di{pyrazol-1-yl}pyrid-4-yl)acetamide]iron(II)tetrafluoroborate(2/0.9) perchlorate(2/1.1) propionitrile solvate'
_chemical_formula_moiety         
'C26 H24 Fe N12 O2, 0.9(B F4), 1.1(Cl O4), C3 H5 N'
_chemical_formula_sum            'C29 H29 B0.90 Cl1.10 F3.60 Fe N13 O6.40'
_chemical_formula_weight         835.02
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.3169(3)
_cell_length_b                   20.4484(7)
_cell_length_c                   22.6673(8)
_cell_angle_alpha                107.978(3)
_cell_angle_beta                 99.002(3)
_cell_angle_gamma                95.195(3)
_cell_volume                     3581.8(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10156
_cell_measurement_temperature    180.15
_cell_measurement_theta_min      3.57
_cell_measurement_theta_max      73.29
_exptl_absorpt_coefficient_mu    4.860
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       lath
_exptl_crystal_F_000             1707
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 0.946
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            28990
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.529
_diffrn_reflns_theta_min         3.578
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10282
_reflns_number_total             13444
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2015)'
_refine_diff_density_max         0.852
_refine_diff_density_min         -1.207
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     972
_refine_ls_number_reflns         13444
_refine_ls_number_restraints     92
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0676
_refine_ls_restrained_S_all      12.195
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0965P)²+4.9720P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1799
_refine_ls_wR_factor_ref         0.1950
_refine_special_details          
;
 The asymmetric unit contains two formula units of the compound, with each 
 residue lying on a general crystallographic site. Separate partial BF₄⁻
 and ClO₄⁻ ions were modelled on each anion site. The BF₄⁻:ClO₄⁻
 occupancy ratio refined to 0.49:0.51 for two of anion pairs, and to
 0.41:0.59 for the other two. One propionitrile molecule was also modelled over
 two sites whose occupancies refined to 0.74:0.26. The bond distance restraints 
 that were applied to the disordered residues are listed below. 

 All crystallographically ordered non-H atoms were refined anisotropically, 
 and H atoms were placed in calculated positions and refined using a riding 
 model. The deepest Fourier hole of -1.1 e.Å⁻³ is associated with the
 partial anion Cl57-O61.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B42-F43 = B42-F44 = B42-F45 = B42-F46
 1.37 with sigma of 0.02
 B47-F48 = B47-F49 = B47-F50 = B47-F51
 1.37 with sigma of 0.02
 B52-F53 = B52-F54 = B52-F55 = B52-F56
 1.37 with sigma of 0.02
 B57-F58 = B57-F59 = B57-F60 = B57-F61
 1.37 with sigma of 0.02
 F43-F44 = F43-F45 = F43-F46 = F44-F45 = F44-F46 = F45-F46
 2.24 with sigma of 0.02
 F48-F49 = F48-F50 = F48-F51 = F49-F50 = F49-F51 = F50-F51
 2.24 with sigma of 0.02
 F53-F54 = F53-F55 = F53-F56 = F54-F55 = F54-F56 = F55-F56
 2.24 with sigma of 0.02
 F58-F59 = F58-F60 = F58-F61 = F59-F60 = F59-F61 = F60-F61
 2.24 with sigma of 0.02
 Cl42-O43 = Cl42-O44 = Cl42-O45 = Cl42-O46
 1.45 with sigma of 0.02
 Cl47-O48 = Cl47-O49 = Cl47-O50 = Cl47-O51
 1.45 with sigma of 0.02
 Cl52-O53 = Cl52-O54 = Cl52-O55 = Cl52-O56
 1.45 with sigma of 0.02
 Cl57-O48 = Cl57-O49 = Cl57-O50 = Cl57-O51
 1.45 with sigma of 0.02
 O43-O44 = O43-O45 = O43-O46 = O44-O45 = O44-O46 = O45-O46
 2.37 with sigma of 0.02
 O48-O49 = O48-O50 = O48-O51 = O49-O50 = O49-O51 = O50-O51
 2.37 with sigma of 0.02
 O53-O54 = O53-O55 = O53-O56 = O54-O55 = O54-O56 = O55-O56
 2.37 with sigma of 0.02
 O58-O59 = O58-O60 = O58-O61 = O59-O60 = O59-O61 = O60-O61
 2.37 with sigma of 0.02
 C66A-C67A = C66B-C67B
 1.51 with sigma of 0.02
 C67A-C68A = C67B-C68B
 1.48 with sigma of 0.02
 C68A-N69A = C68B-N69B
 1.15 with sigma of 0.02
 C66A-C68A = C66B-C68B
 2.44 with sigma of 0.02
 C67A-N69A = C67B-N69B
 2.63 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
B57 \\sim Cl57: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
B42 \\sim Cl42: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
4. Others
 Fixed Sof: B42(0.41) F43(0.41) F44(0.41) F45(0.41) F46(0.41) Cl42(0.59)
 O43(0.59) O44(0.59) O45(0.59) O46(0.59) B47(0.49) F48(0.49) F49(0.49)
 F50(0.49) F51(0.49) Cl47(0.51) O48(0.51) O49(0.51) O50(0.51) O51(0.51)
 B52(0.41) F53(0.41) F54(0.41) F55(0.41) F56(0.41) Cl52(0.59) O53(0.59)
 O54(0.59) O55(0.59) O56(0.59) B57(0.49) F58(0.49) F59(0.49) F60(0.49)
 F61(0.49) Cl57(0.51) O58(0.51) O59(0.51) O60(0.51) O61(0.51) C66A(0.74)
 H66A(0.74) H66B(0.74) H66C(0.74) C67A(0.74) H67A(0.74) H67B(0.74) C68A(0.74)
 N69A(0.74) C66B(0.26) H66D(0.26) H66E(0.26) H66F(0.26) C67B(0.26) H67C(0.26)
 H67D(0.26) C68B(0.26) N69B(0.26)
5.a Secondary CH2 refined with riding coordinates:
 C63(H63A,H63B), C67A(H67A,H67B), C67B(H67C,H67D)
5.b Me refined with riding coordinates:
 C66A(H66A,H66B,H66C), C66B(H66D,H66E,H66F)
5.c Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C6A(H6A), C10A(H10A), C11A(H11A), C12A(H12A), C15A(H15A),
 C16A(H16A), C17A(H17A), N18A(H18A), C24A(H24A), C26A(H26A), C30A(H30A),
 C31A(H31A), C32A(H32A), C35A(H35A), C36A(H36A), C37A(H37A), N38A(H38A),
 C4B(H4B), C6B(H6B), C10B(H10B), C11B(H11B), C12B(H12B), C15B(H15B), C16B(H16B),
  C17B(H17B), N18B(H18B), C24B(H24B), C26B(H26B), C30B(H30B), C31B(H31B),
 C32B(H32B), C35B(H35B), C36B(H36B), C37B(H37B), N38B(H38B)
5.d Idealised Me refined as rotating group:
 C21A(H21A,H21B,H21C), C41A(H41A,H41B,H41C), C21B(H21D,H21E,H21F), C41B(H41D,
 H41E,H41F), C62(H62A,H62B,H62C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1A Fe -0.01419(7) 0.98083(3) 0.25133(2) 0.02184(15) Uani 1 1 d . . . . .
N2A N -0.0376(4) 0.94756(15) 0.16100(14) 0.0264(6) Uani 1 1 d . . . . .
C3A C 0.0867(5) 0.96403(19) 0.13403(18) 0.0293(8) Uani 1 1 d . . . . .
C4A C 0.0736(5) 0.9447(2) 0.06961(18) 0.0326(8) Uani 1 1 d . . . . .
H4A H 0.162849 0.956480 0.051457 0.039 Uiso 1 1 calc R U . . .
C5A C -0.0756(5) 0.9070(2) 0.03164(18) 0.0328(8) Uani 1 1 d . . . . .
C6A C -0.2091(5) 0.8915(2) 0.05877(18) 0.0318(8) Uani 1 1 d . . . . .
H6A H -0.312360 0.867040 0.033819 0.038 Uiso 1 1 calc R U . . .
C7A C -0.1803(5) 0.91401(18) 0.12372(17) 0.0271(7) Uani 1 1 d . . . . .
N8A N 0.2239(4) 1.00207(17) 0.17981(16) 0.0319(7) Uani 1 1 d . . . . .
N9A N 0.2091(4) 1.01572(17) 0.24186(15) 0.0309(7) Uani 1 1 d . . . . .
C10A C 0.3510(5) 1.0531(2) 0.2763(2) 0.0405(10) Uani 1 1 d . . . . .
H10A H 0.377646 1.069519 0.321192 0.049 Uiso 1 1 calc R U . . .
C11A C 0.4551(6) 1.0647(3) 0.2368(2) 0.0477(11) Uani 1 1 d . . . . .
H11A H 0.562479 1.090689 0.249746 0.057 Uiso 1 1 calc R U . . .
C12A C 0.3746(5) 1.0320(2) 0.1767(2) 0.0430(10) Uani 1 1 d . . . . .
H12A H 0.415088 1.030119 0.139324 0.052 Uiso 1 1 calc R U . . .
N13A N -0.2977(4) 0.90611(16) 0.16072(14) 0.0279(6) Uani 1 1 d . . . . .
N14A N -0.2464(4) 0.93222(17) 0.22529(14) 0.0294(7) Uani 1 1 d . . . . .
C15A C -0.3766(5) 0.9171(2) 0.24840(19) 0.0352(9) Uani 1 1 d . . . . .
H15A H -0.378671 0.928499 0.292184 0.042 Uiso 1 1 calc R U . . .
C16A C -0.5096(5) 0.8822(2) 0.2000(2) 0.0397(9) Uani 1 1 d . . . . .
H16A H -0.616201 0.866076 0.204595 0.048 Uiso 1 1 calc R U . . .
C17A C -0.4574(5) 0.8757(2) 0.1445(2) 0.0352(9) Uani 1 1 d . . . . .
H17A H -0.520199 0.854177 0.102894 0.042 Uiso 1 1 calc R U . . .
N18A N -0.0858(5) 0.88658(19) -0.03358(15) 0.0399(8) Uani 1 1 d . . . . .
H18A H -0.013395 0.909102 -0.047534 0.048 Uiso 1 1 calc R U . . .
C19A C -0.1979(6) 0.8348(2) -0.07804(19) 0.0424(10) Uani 1 1 d . . . . .
O20A O -0.3049(5) 0.79987(18) -0.06525(14) 0.0528(9) Uani 1 1 d . . . . .
C21A C -0.1731(8) 0.8229(3) -0.1451(2) 0.0612(15) Uani 1 1 d . . . . .
H21A H -0.278422 0.803385 -0.174509 0.092 Uiso 1 1 calc R U . . .
H21B H -0.093822 0.790330 -0.154811 0.092 Uiso 1 1 calc R U . . .
H21C H -0.131076 0.867175 -0.149387 0.092 Uiso 1 1 calc R U . . .
N22A N 0.0240(4) 1.02489(15) 0.34167(13) 0.0226(6) Uani 1 1 d . . . . .
C23A C 0.0907(4) 0.99279(17) 0.38046(16) 0.0226(7) Uani 1 1 d . . . . .
C24A C 0.1317(4) 1.02306(19) 0.44478(16) 0.0261(7) Uani 1 1 d . . . . .
H24A H 0.175546 0.998286 0.471258 0.031 Uiso 1 1 calc R U . . .
C25A C 0.1058(5) 1.09278(19) 0.47004(16) 0.0267(7) Uani 1 1 d . . . . .
C26A C 0.0418(5) 1.12829(18) 0.43004(16) 0.0270(7) Uani 1 1 d . . . . .
H26A H 0.025930 1.175487 0.445991 0.032 Uiso 1 1 calc R U . . .
C27A C 0.0031(4) 1.09125(18) 0.36635(16) 0.0236(7) Uani 1 1 d . . . . .
N28A N 0.1155(4) 0.92547(15) 0.34605(14) 0.0267(6) Uani 1 1 d . . . . .
N29A N 0.0703(4) 0.90520(16) 0.28103(13) 0.0275(6) Uani 1 1 d . . . . .
C30A C 0.1129(5) 0.8423(2) 0.26032(19) 0.0352(9) Uani 1 1 d . . . . .
H30A H 0.096262 0.814701 0.217011 0.042 Uiso 1 1 calc R U . . .
C31A C 0.1848(6) 0.8220(2) 0.3101(2) 0.0419(10) Uani 1 1 d . . . . .
H31A H 0.224727 0.779287 0.307238 0.050 Uiso 1 1 calc R U . . .
C32A C 0.1866(5) 0.8762(2) 0.3642(2) 0.0358(9) Uani 1 1 d . . . . .
H32A H 0.229656 0.878490 0.406300 0.043 Uiso 1 1 calc R U . . .
N33A N -0.0587(4) 1.11741(15) 0.31816(14) 0.0265(6) Uani 1 1 d . . . . .
N34A N -0.0797(4) 1.07309(16) 0.25723(13) 0.0250(6) Uani 1 1 d . . . . .
C35A C -0.1278(5) 1.1098(2) 0.22075(18) 0.0326(8) Uani 1 1 d . . . . .
H35A H -0.152025 1.092435 0.175850 0.039 Uiso 1 1 calc R U . . .
C36A C -0.1383(6) 1.1775(2) 0.2569(2) 0.0406(10) Uani 1 1 d . . . . .
H36A H -0.168956 1.213868 0.241703 0.049 Uiso 1 1 calc R U . . .
C37A C -0.0955(5) 1.1809(2) 0.3189(2) 0.0371(9) Uani 1 1 d . . . . .
H37A H -0.092202 1.220149 0.355220 0.045 Uiso 1 1 calc R U . . .
N38A N 0.1542(4) 1.12291(17) 0.53523(14) 0.0330(7) Uani 1 1 d . . . . .
H38A H 0.200033 1.096757 0.555447 0.040 Uiso 1 1 calc R U . . .
C39A C 0.1390(6) 1.1888(2) 0.57195(18) 0.0377(9) Uani 1 1 d . . . . .
O40A O 0.0723(5) 1.22892(17) 0.55077(15) 0.0568(10) Uani 1 1 d . . . . .
C41A C 0.2145(6) 1.2057(3) 0.64071(19) 0.0478(11) Uani 1 1 d . . . . .
H41A H 0.171381 1.245956 0.666011 0.072 Uiso 1 1 calc R U . . .
H41B H 0.334379 1.216607 0.646669 0.072 Uiso 1 1 calc R U . . .
H41C H 0.186983 1.165688 0.654232 0.072 Uiso 1 1 calc R U . . .
Fe1B Fe 0.52922(7) 0.52623(3) 0.25019(2) 0.02469(15) Uani 1 1 d . . . . .
N2B N 0.5653(4) 0.55863(15) 0.34970(13) 0.0268(6) Uani 1 1 d . . . . .
C3B C 0.4449(5) 0.54486(19) 0.37841(17) 0.0285(8) Uani 1 1 d . . . . .
C4B C 0.4615(5) 0.5645(2) 0.44321(18) 0.0331(8) Uani 1 1 d . . . . .
H4B H 0.373646 0.553288 0.462244 0.040 Uiso 1 1 calc R U . . .
C5B C 0.6117(5) 0.6014(2) 0.47969(17) 0.0318(8) Uani 1 1 d . . . . .
C6B C 0.7416(5) 0.61612(19) 0.45095(17) 0.0301(8) Uani 1 1 d . . . . .
H6B H 0.845724 0.640685 0.474882 0.036 Uiso 1 1 calc R U . . .
C7B C 0.7087(4) 0.59268(18) 0.38563(16) 0.0255(7) Uani 1 1 d . . . . .
N8B N 0.2999(4) 0.50872(17) 0.33602(15) 0.0308(7) Uani 1 1 d . . . . .
N9B N 0.2942(4) 0.49669(18) 0.27309(15) 0.0317(7) Uani 1 1 d . . . . .
C10B C 0.1462(5) 0.4613(2) 0.2449(2) 0.0429(10) Uani 1 1 d . . . . .
H10B H 0.105332 0.445761 0.200614 0.051 Uiso 1 1 calc R U . . .
C11B C 0.0584(6) 0.4501(3) 0.2895(2) 0.0484(11) Uani 1 1 d . . . . .
H11B H -0.049514 0.425346 0.281091 0.058 Uiso 1 1 calc R U . . .
C12B C 0.1558(5) 0.4808(2) 0.3465(2) 0.0416(10) Uani 1 1 d . . . . .
H12B H 0.129693 0.482800 0.386305 0.050 Uiso 1 1 calc R U . . .
N13B N 0.8266(4) 0.60267(16) 0.34918(13) 0.0275(6) Uani 1 1 d . . . . .
N14B N 0.7767(4) 0.58206(18) 0.28526(15) 0.0336(7) Uani 1 1 d . . . . .
C15B C 0.9108(6) 0.5991(2) 0.2644(2) 0.0423(10) Uani 1 1 d . . . . .
H15B H 0.914252 0.591057 0.221074 0.051 Uiso 1 1 calc R U . . .
C16B C 1.0443(5) 0.6300(2) 0.3135(2) 0.0388(9) Uani 1 1 d . . . . .
H16B H 1.152355 0.646209 0.310444 0.047 Uiso 1 1 calc R U . . .
C17B C 0.9871(5) 0.6320(2) 0.3673(2) 0.0342(8) Uani 1 1 d . . . . .
H17B H 1.048185 0.650502 0.409354 0.041 Uiso 1 1 calc R U . . .
N18B N 0.6246(5) 0.62268(19) 0.54507(15) 0.0389(8) Uani 1 1 d . . . . .
H18B H 0.554480 0.599938 0.559767 0.047 Uiso 1 1 calc R U . . .
C19B C 0.7367(6) 0.6760(2) 0.58901(19) 0.0423(10) Uani 1 1 d . . . . .
O20B O 0.8420(5) 0.70938(18) 0.57476(15) 0.0546(9) Uani 1 1 d . . . . .
C21B C 0.7111(8) 0.6891(3) 0.6559(2) 0.0583(14) Uani 1 1 d . . . . .
H21D H 0.813263 0.686084 0.682512 0.087 Uiso 1 1 calc R U . . .
H21E H 0.623024 0.654161 0.656420 0.087 Uiso 1 1 calc R U . . .
H21F H 0.680596 0.735562 0.672323 0.087 Uiso 1 1 calc R U . . .
N22B N 0.4633(4) 0.47268(15) 0.15308(13) 0.0233(6) Uani 1 1 d . . . . .
C23B C 0.4031(4) 0.50443(17) 0.11282(16) 0.0235(7) Uani 1 1 d . . . . .
C24B C 0.3590(5) 0.47277(19) 0.04910(16) 0.0272(7) Uani 1 1 d . . . . .
H24B H 0.318996 0.497452 0.021932 0.033 Uiso 1 1 calc R U . . .
C25B C 0.3749(5) 0.40209(19) 0.02519(16) 0.0269(7) Uani 1 1 d . . . . .
C26B C 0.4357(5) 0.36688(19) 0.06620(16) 0.0279(7) Uani 1 1 d . . . . .
H26B H 0.447287 0.319078 0.051253 0.034 Uiso 1 1 calc R U . . .
C27B C 0.4776(4) 0.40589(18) 0.12956(16) 0.0236(7) Uani 1 1 d . . . . .
N28B N 0.3886(4) 0.57427(15) 0.14384(13) 0.0257(6) Uani 1 1 d . . . . .
N29B N 0.4411(4) 0.60077(17) 0.20772(14) 0.0326(7) Uani 1 1 d . . . . .
C30B C 0.4057(6) 0.6654(2) 0.2234(2) 0.0420(10) Uani 1 1 d . . . . .
H30B H 0.429399 0.697402 0.265284 0.050 Uiso 1 1 calc R U . . .
C31B C 0.3297(6) 0.6802(2) 0.1709(2) 0.0492(12) Uani 1 1 d . . . . .
H31B H 0.292592 0.722599 0.170037 0.059 Uiso 1 1 calc R U . . .
C32B C 0.3195(5) 0.6213(2) 0.1209(2) 0.0375(9) Uani 1 1 d . . . . .
H32B H 0.272846 0.614356 0.078035 0.045 Uiso 1 1 calc R U . . .
N33B N 0.5382(4) 0.37819(15) 0.17688(13) 0.0265(6) Uani 1 1 d . . . . .
N34B N 0.5765(4) 0.42253(16) 0.23788(13) 0.0265(6) Uani 1 1 d . . . . .
C35B C 0.6176(5) 0.3828(2) 0.27285(19) 0.0355(9) Uani 1 1 d . . . . .
H35B H 0.650955 0.399239 0.317573 0.043 Uiso 1 1 calc R U . . .
C36B C 0.6048(6) 0.3136(2) 0.2349(2) 0.0453(11) Uani 1 1 d . . . . .
H36B H 0.626501 0.275255 0.248629 0.054 Uiso 1 1 calc R U . . .
C37B C 0.5551(6) 0.3118(2) 0.1739(2) 0.0411(10) Uani 1 1 d . . . . .
H37B H 0.536053 0.272120 0.136930 0.049 Uiso 1 1 calc R U . . .
N38B N 0.3237(4) 0.36998(17) -0.03976(14) 0.0336(7) Uani 1 1 d . . . . .
H38B H 0.277780 0.395417 -0.060748 0.040 Uiso 1 1 calc R U . . .
C39B C 0.3362(6) 0.3029(2) -0.07522(18) 0.0385(9) Uani 1 1 d . . . . .
O40B O 0.4056(5) 0.26406(17) -0.05367(14) 0.0564(10) Uani 1 1 d . . . . .
C41B C 0.2549(7) 0.2844(3) -0.14406(19) 0.0499(12) Uani 1 1 d . . . . .
H41D H 0.287807 0.241029 -0.168760 0.075 Uiso 1 1 calc R U . . .
H41E H 0.289250 0.321808 -0.159992 0.075 Uiso 1 1 calc R U . . .
H41F H 0.135005 0.278371 -0.147977 0.075 Uiso 1 1 calc R U . . .
B42 B 0.3110(14) 0.8807(5) -0.0693(5) 0.0271(16) Uiso 0.41 1 d D U P A 1
F43 F 0.2542(10) 0.8216(4) -0.1068(3) 0.0529(19) Uiso 0.41 1 d D . P A 1
F44 F 0.4591(10) 0.9102(4) -0.0874(4) 0.064(2) Uiso 0.41 1 d D . P A 1
F45 F 0.3684(10) 0.8768(4) -0.0082(3) 0.039(2) Uiso 0.41 1 d D . P A 1
F46 F 0.2051(11) 0.9294(5) -0.0672(4) 0.046(3) Uiso 0.41 1 d D . P A 1
Cl42 Cl 0.3535(2) 0.89704(10) -0.05987(9) 0.0382(4) Uiso 0.59 1 d D U P B 2
O43 O 0.3143(9) 0.8346(3) -0.1101(3) 0.0503(15) Uiso 0.59 1 d D . P B 2
O44 O 0.5058(7) 0.9340(3) -0.0652(3) 0.0456(13) Uiso 0.59 1 d D . P B 2
O45 O 0.3798(8) 0.8936(4) 0.0023(3) 0.0379(18) Uiso 0.59 1 d D . P B 2
O46 O 0.2279(8) 0.9427(4) -0.0619(3) 0.0343(19) Uiso 0.59 1 d D . P B 2
B47 B 0.3763(10) 0.9825(5) 0.5884(4) 0.016(2) Uiso 0.49 1 d D . P C 1
F48 F 0.5359(7) 1.0002(4) 0.6014(3) 0.0559(18) Uiso 0.49 1 d D . P C 1
F49 F 0.3074(9) 1.0381(3) 0.5973(3) 0.0505(18) Uiso 0.49 1 d D . P C 1
F50 F 0.3351(7) 0.9438(3) 0.6288(3) 0.0365(14) Uiso 0.49 1 d D . P C 1
F51 F 0.2935(8) 0.9297(3) 0.5237(3) 0.0373(15) Uiso 0.49 1 d D . P C 1
Cl47 Cl 0.3702(3) 0.96648(15) 0.58080(13) 0.0389(7) Uiso 0.51 1 d D . P D 2
O48 O 0.5405(8) 0.9789(4) 0.5826(4) 0.0455(17) Uiso 0.51 1 d D . P D 2
O49 O 0.2672(8) 1.0202(3) 0.5931(3) 0.0334(15) Uiso 0.51 1 d D . P D 2
O50 O 0.3427(7) 0.9226(3) 0.6175(3) 0.0307(15) Uiso 0.51 1 d D . P D 2
O51 O 0.3288(12) 0.9266(5) 0.5133(4) 0.063(3) Uiso 0.51 1 d D . P D 2
B52 B 0.1593(12) 0.5972(5) 0.5609(4) 0.015(2) Uiso 0.41 1 d D . P E 1
F53 F 0.2959(9) 0.5620(4) 0.5674(4) 0.037(2) Uiso 0.41 1 d D . P E 1
F54 F 0.2231(12) 0.6703(4) 0.6097(4) 0.071(3) Uiso 0.41 1 d D . P E 1
F55 F 0.0381(11) 0.5748(5) 0.5792(5) 0.073(3) Uiso 0.41 1 d D . P E 1
F56 F 0.1375(9) 0.6027(4) 0.5040(3) 0.0373(19) Uiso 0.41 1 d D . P E 1
Cl52 Cl 0.1903(3) 0.61457(12) 0.56912(10) 0.0393(5) Uiso 0.59 1 d D . P F 2
O53 O 0.3266(8) 0.5746(3) 0.5734(3) 0.0348(18) Uiso 0.59 1 d D . P F 2
O54 O 0.2756(8) 0.6855(3) 0.6077(3) 0.0429(13) Uiso 0.59 1 d D . P F 2
O55 O 0.0662(7) 0.5982(3) 0.5976(3) 0.0478(15) Uiso 0.59 1 d D . P F 2
O56 O 0.1459(8) 0.6225(4) 0.5094(3) 0.0388(17) Uiso 0.59 1 d D . P F 2
B57 B 0.1359(14) 0.5109(5) -0.1033(5) 0.0250(16) Uiso 0.49 1 d D U P G 1
F58 F 0.1658(9) 0.5628(4) -0.1311(3) 0.050(2) Uiso 0.49 1 d D . P G 1
F59 F 0.1812(10) 0.4537(4) -0.1075(4) 0.062(2) Uiso 0.49 1 d D . P G 1
F60 F 0.2137(8) 0.5627(3) -0.0364(3) 0.0405(14) Uiso 0.49 1 d D . P G 1
F61 F -0.0366(8) 0.5139(4) -0.0998(3) 0.0591(19) Uiso 0.49 1 d D . P G 1
Cl57 Cl 0.1290(4) 0.52186(14) -0.09480(13) 0.0410(6) Uiso 0.51 1 d D U P H 2
O58 O 0.1765(8) 0.5462(4) -0.1440(3) 0.0321(16) Uiso 0.51 1 d D . P H 2
O59 O 0.2330(8) 0.4633(3) -0.1070(3) 0.0323(14) Uiso 0.51 1 d D . P H 2
O60 O 0.1574(11) 0.5589(4) -0.0315(3) 0.053(2) Uiso 0.51 1 d D . P H 2
O61 O -0.0371(8) 0.4892(4) -0.1159(3) 0.0466(17) Uiso 0.51 1 d D . P H 2
C62 C 0.5180(10) 0.7999(4) 0.5442(5) 0.110(3) Uani 1 1 d . . . . .
H62A H 0.597357 0.767007 0.541604 0.165 Uiso 1 1 calc R U . . .
H62B H 0.501931 0.818216 0.587916 0.165 Uiso 1 1 calc R U . . .
H62C H 0.559998 0.838356 0.530899 0.165 Uiso 1 1 calc R U . . .
C63 C 0.3656(9) 0.7655(3) 0.5041(4) 0.087(2) Uani 1 1 d . . . . .
H63A H 0.281699 0.797168 0.507977 0.104 Uiso 1 1 calc R U . . .
H63B H 0.325140 0.724337 0.514728 0.104 Uiso 1 1 calc R U . . .
C64 C 0.4031(10) 0.7432(3) 0.4356(3) 0.077(2) Uani 1 1 d . . . . .
N65 N 0.4193(7) 0.7243(3) 0.3850(3) 0.0780(16) Uani 1 1 d . . . . .
C66A C 0.0039(11) 0.6923(5) -0.0590(4) 0.077(2) Uiso 0.74 1 d D . P I 1
H66A H 0.024219 0.671685 -0.101851 0.115 Uiso 0.74 1 calc R U P I 1
H66B H -0.044717 0.655719 -0.044879 0.115 Uiso 0.74 1 calc R U P I 1
H66C H -0.071911 0.726290 -0.059104 0.115 Uiso 0.74 1 calc R U P I 1
C67A C 0.1683(9) 0.7290(4) -0.0136(3) 0.0525(16) Uiso 0.74 1 d D . P I 1
H67A H 0.245373 0.694728 -0.014264 0.063 Uiso 0.74 1 calc R U P I 1
H67B H 0.218163 0.765339 -0.028497 0.063 Uiso 0.74 1 calc R U P I 1
C68A C 0.1454(10) 0.7603(4) 0.0501(3) 0.0492(17) Uiso 0.74 1 d D . P I 1
N69A N 0.1020(12) 0.7793(5) 0.1006(4) 0.074(3) Uiso 0.74 1 d D . P I 1
C66B C 0.114(4) 0.7184(16) -0.0572(10) 0.092(8) Uiso 0.26 1 d D . P J 2
H66D H 0.066526 0.688252 -0.100518 0.137 Uiso 0.26 1 calc R U P J 2
H66E H 0.119267 0.767136 -0.055031 0.137 Uiso 0.26 1 calc R U P J 2
H66F H 0.224798 0.708518 -0.044715 0.137 Uiso 0.26 1 calc R U P J 2
C67B C 0.009(3) 0.7050(13) -0.0138(8) 0.084(8) Uiso 0.26 1 d D . P J 2
H67C H 0.002127 0.655592 -0.016411 0.101 Uiso 0.26 1 calc R U P J 2
H67D H -0.103567 0.714300 -0.026743 0.101 Uiso 0.26 1 calc R U P J 2
C68B C 0.079(3) 0.7505(9) 0.0529(7) 0.046(4) Uiso 0.26 1 d D . P J 2
N69B N 0.142(2) 0.7915(8) 0.1002(7) 0.036(4) Uiso 0.26 1 d D . P J 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1A N2A 1.920(3) . ?
Fe1A N9A 1.995(3) . ?
Fe1A N14A 2.000(3) . ?
Fe1A N22A 1.927(3) . ?
Fe1A N29A 2.008(3) . ?
Fe1A N34A 1.982(3) . ?
N2A C3A 1.348(5) . ?
N2A C7A 1.332(5) . ?
C3A C4A 1.374(5) . ?
C3A N8A 1.398(5) . ?
C4A H4A 0.9500 . ?
C4A C5A 1.399(6) . ?
C5A C6A 1.409(6) . ?
C5A N18A 1.393(5) . ?
C6A H6A 0.9500 . ?
C6A C7A 1.374(5) . ?
C7A N13A 1.413(5) . ?
N8A N9A 1.375(4) . ?
N8A C12A 1.366(5) . ?
N9A C10A 1.330(5) . ?
C10A H10A 0.9500 . ?
C10A C11A 1.394(6) . ?
C11A H11A 0.9500 . ?
C11A C12A 1.350(7) . ?
C12A H12A 0.9500 . ?
N13A N14A 1.375(4) . ?
N13A C17A 1.357(5) . ?
N14A C15A 1.327(5) . ?
C15A H15A 0.9500 . ?
C15A C16A 1.389(6) . ?
C16A H16A 0.9500 . ?
C16A C17A 1.367(6) . ?
C17A H17A 0.9500 . ?
N18A H18A 0.8800 . ?
N18A C19A 1.369(6) . ?
C19A O20A 1.216(6) . ?
C19A C21A 1.514(6) . ?
C21A H21A 0.9800 . ?
C21A H21B 0.9800 . ?
C21A H21C 0.9800 . ?
N22A C23A 1.335(4) . ?
N22A C27A 1.337(4) . ?
C23A C24A 1.369(5) . ?
C23A N28A 1.409(4) . ?
C24A H24A 0.9500 . ?
C24A C25A 1.413(5) . ?
C25A C26A 1.399(5) . ?
C25A N38A 1.390(4) . ?
C26A H26A 0.9500 . ?
C26A C27A 1.377(5) . ?
C27A N33A 1.407(4) . ?
N28A N29A 1.381(4) . ?
N28A C32A 1.351(5) . ?
N29A C30A 1.328(5) . ?
C30A H30A 0.9500 . ?
C30A C31A 1.387(6) . ?
C31A H31A 0.9500 . ?
C31A C32A 1.373(6) . ?
C32A H32A 0.9500 . ?
N33A N34A 1.372(4) . ?
N33A C37A 1.357(5) . ?
N34A C35A 1.320(5) . ?
C35A H35A 0.9500 . ?
C35A C36A 1.391(6) . ?
C36A H36A 0.9500 . ?
C36A C37A 1.373(6) . ?
C37A H37A 0.9500 . ?
N38A H38A 0.8800 . ?
N38A C39A 1.378(5) . ?
C39A O40A 1.205(5) . ?
C39A C41A 1.505(5) . ?
C41A H41A 0.9800 . ?
C41A H41B 0.9800 . ?
C41A H41C 0.9800 . ?
Fe1B N2B 2.108(3) . ?
Fe1B N9B 2.180(3) . ?
Fe1B N14B 2.162(4) . ?
Fe1B N22B 2.091(3) . ?
Fe1B N29B 2.162(3) . ?
Fe1B N34B 2.133(3) . ?
N2B C3B 1.331(5) . ?
N2B C7B 1.329(5) . ?
C3B C4B 1.378(5) . ?
C3B N8B 1.401(5) . ?
C4B H4B 0.9500 . ?
C4B C5B 1.390(6) . ?
C5B C6B 1.402(5) . ?
C5B N18B 1.393(5) . ?
C6B H6B 0.9500 . ?
C6B C7B 1.381(5) . ?
C7B N13B 1.417(5) . ?
N8B N9B 1.363(4) . ?
N8B C12B 1.367(5) . ?
N9B C10B 1.324(5) . ?
C10B H10B 0.9500 . ?
C10B C11B 1.396(7) . ?
C11B H11B 0.9500 . ?
C11B C12B 1.341(7) . ?
C12B H12B 0.9500 . ?
N13B N14B 1.361(4) . ?
N13B C17B 1.357(5) . ?
N14B C15B 1.336(5) . ?
C15B H15B 0.9500 . ?
C15B C16B 1.387(6) . ?
C16B H16B 0.9500 . ?
C16B C17B 1.366(6) . ?
C17B H17B 0.9500 . ?
N18B H18B 0.8800 . ?
N18B C19B 1.381(6) . ?
C19B O20B 1.205(6) . ?
C19B C21B 1.509(6) . ?
C21B H21D 0.9800 . ?
C21B H21E 0.9800 . ?
C21B H21F 0.9800 . ?
N22B C23B 1.336(4) . ?
N22B C27B 1.328(4) . ?
C23B C24B 1.362(5) . ?
C23B N28B 1.409(4) . ?
C24B H24B 0.9500 . ?
C24B C25B 1.405(5) . ?
C25B C26B 1.403(5) . ?
C25B N38B 1.392(4) . ?
C26B H26B 0.9500 . ?
C26B C27B 1.381(5) . ?
C27B N33B 1.408(4) . ?
N28B N29B 1.362(4) . ?
N28B C32B 1.356(5) . ?
N29B C30B 1.332(5) . ?
C30B H30B 0.9500 . ?
C30B C31B 1.390(6) . ?
C31B H31B 0.9500 . ?
C31B C32B 1.361(6) . ?
C32B H32B 0.9500 . ?
N33B N34B 1.368(4) . ?
N33B C37B 1.360(5) . ?
N34B C35B 1.330(5) . ?
C35B H35B 0.9500 . ?
C35B C36B 1.396(6) . ?
C36B H36B 0.9500 . ?
C36B C37B 1.366(6) . ?
C37B H37B 0.9500 . ?
N38B H38B 0.8800 . ?
N38B C39B 1.381(5) . ?
C39B O40B 1.199(5) . ?
C39B C41B 1.515(6) . ?
C41B H41D 0.9800 . ?
C41B H41E 0.9800 . ?
C41B H41F 0.9800 . ?
B42 F43 1.242(12) . ?
B42 F44 1.491(12) . ?
B42 F45 1.421(11) . ?
B42 F46 1.382(12) . ?
Cl42 O43 1.394(6) . ?
Cl42 O44 1.456(6) . ?
Cl42 O45 1.416(6) . ?
Cl42 O46 1.468(6) . ?
B47 F48 1.305(10) . ?
B47 F49 1.295(10) . ?
B47 F50 1.442(9) . ?
B47 F51 1.537(10) . ?
Cl47 O48 1.408(7) . ?
Cl47 O49 1.439(6) . ?
Cl47 O50 1.425(6) . ?
Cl47 O51 1.462(8) . ?
B52 F53 1.411(11) . ?
B52 F54 1.546(11) . ?
B52 F55 1.250(11) . ?
B52 F56 1.316(10) . ?
Cl52 O53 1.464(6) . ?
Cl52 O54 1.486(6) . ?
Cl52 O55 1.369(6) . ?
Cl52 O56 1.408(6) . ?
B57 F58 1.415(11) . ?
B57 F59 1.242(11) . ?
B57 F60 1.555(11) . ?
B57 F61 1.455(12) . ?
Cl57 O58 1.446(6) . ?
Cl57 O59 1.522(6) . ?
Cl57 O60 1.370(7) . ?
Cl57 O61 1.419(7) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C62 C63 1.419(9) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C63 C64 1.566(10) . ?
C64 N65 1.126(8) . ?
C66A H66A 0.9800 . ?
C66A H66B 0.9800 . ?
C66A H66C 0.9800 . ?
C66A C67A 1.545(10) . ?
C67A H67A 0.9900 . ?
C67A H67B 0.9900 . ?
C67A C68A 1.439(8) . ?
C68A N69A 1.214(9) . ?
C66B H66D 0.9800 . ?
C66B H66E 0.9800 . ?
C66B H66F 0.9800 . ?
C66B C67B 1.479(18) . ?
C67B H67C 0.9900 . ?
C67B H67D 0.9900 . ?
C67B C68B 1.500(15) . ?
C68B N69B 1.146(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2A Fe1A N9A 79.27(13) . . ?
N2A Fe1A N14A 78.95(12) . . ?
N2A Fe1A N22A 172.77(13) . . ?
N2A Fe1A N29A 105.62(12) . . ?
N2A Fe1A N34A 96.06(12) . . ?
N9A Fe1A N14A 158.22(13) . . ?
N9A Fe1A N29A 92.16(13) . . ?
N14A Fe1A N29A 93.30(13) . . ?
N22A Fe1A N9A 95.28(13) . . ?
N22A Fe1A N14A 106.46(12) . . ?
N22A Fe1A N29A 79.16(12) . . ?
N22A Fe1A N34A 78.99(12) . . ?
N34A Fe1A N9A 89.11(13) . . ?
N34A Fe1A N14A 93.57(13) . . ?
N34A Fe1A N29A 158.14(12) . . ?
C3A N2A Fe1A 119.8(3) . . ?
C7A N2A Fe1A 121.3(2) . . ?
C7A N2A C3A 118.6(3) . . ?
N2A C3A C4A 122.3(4) . . ?
N2A C3A N8A 111.2(3) . . ?
C4A C3A N8A 126.5(4) . . ?
C3A C4A H4A 121.1 . . ?
C3A C4A C5A 117.7(4) . . ?
C5A C4A H4A 121.1 . . ?
C4A C5A C6A 120.9(3) . . ?
N18A C5A C4A 117.1(4) . . ?
N18A C5A C6A 122.0(4) . . ?
C5A C6A H6A 122.2 . . ?
C7A C6A C5A 115.6(4) . . ?
C7A C6A H6A 122.2 . . ?
N2A C7A C6A 124.8(3) . . ?
N2A C7A N13A 110.0(3) . . ?
C6A C7A N13A 125.2(3) . . ?
N9A N8A C3A 116.5(3) . . ?
C12A N8A C3A 133.3(4) . . ?
C12A N8A N9A 110.1(3) . . ?
N8A N9A Fe1A 113.1(2) . . ?
C10A N9A Fe1A 140.8(3) . . ?
C10A N9A N8A 105.9(3) . . ?
N9A C10A H10A 125.0 . . ?
N9A C10A C11A 110.0(4) . . ?
C11A C10A H10A 125.0 . . ?
C10A C11A H11A 126.4 . . ?
C12A C11A C10A 107.2(4) . . ?
C12A C11A H11A 126.4 . . ?
N8A C12A H12A 126.6 . . ?
C11A C12A N8A 106.9(4) . . ?
C11A C12A H12A 126.6 . . ?
N14A N13A C7A 116.9(3) . . ?
C17A N13A C7A 131.7(3) . . ?
C17A N13A N14A 111.4(3) . . ?
N13A N14A Fe1A 112.7(2) . . ?
C15A N14A Fe1A 142.4(3) . . ?
C15A N14A N13A 104.9(3) . . ?
N14A C15A H15A 124.5 . . ?
N14A C15A C16A 110.9(4) . . ?
C16A C15A H15A 124.5 . . ?
C15A C16A H16A 126.7 . . ?
C17A C16A C15A 106.7(4) . . ?
C17A C16A H16A 126.7 . . ?
N13A C17A C16A 106.1(4) . . ?
N13A C17A H17A 126.9 . . ?
C16A C17A H17A 126.9 . . ?
C5A N18A H18A 116.9 . . ?
C19A N18A C5A 126.2(4) . . ?
C19A N18A H18A 116.9 . . ?
N18A C19A C21A 113.8(4) . . ?
O20A C19A N18A 123.6(4) . . ?
O20A C19A C21A 122.6(5) . . ?
C19A C21A H21A 109.5 . . ?
C19A C21A H21B 109.5 . . ?
C19A C21A H21C 109.5 . . ?
H21A C21A H21B 109.5 . . ?
H21A C21A H21C 109.5 . . ?
H21B C21A H21C 109.5 . . ?
C23A N22A Fe1A 120.6(2) . . ?
C23A N22A C27A 118.5(3) . . ?
C27A N22A Fe1A 120.4(2) . . ?
N22A C23A C24A 123.5(3) . . ?
N22A C23A N28A 110.8(3) . . ?
C24A C23A N28A 125.7(3) . . ?
C23A C24A H24A 121.5 . . ?
C23A C24A C25A 117.0(3) . . ?
C25A C24A H24A 121.5 . . ?
C26A C25A C24A 120.4(3) . . ?
N38A C25A C24A 115.7(3) . . ?
N38A C25A C26A 123.8(3) . . ?
C25A C26A H26A 121.7 . . ?
C27A C26A C25A 116.5(3) . . ?
C27A C26A H26A 121.7 . . ?
N22A C27A C26A 123.9(3) . . ?
N22A C27A N33A 110.4(3) . . ?
C26A C27A N33A 125.7(3) . . ?
N29A N28A C23A 116.9(3) . . ?
C32A N28A C23A 132.0(3) . . ?
C32A N28A N29A 111.0(3) . . ?
N28A N29A Fe1A 112.4(2) . . ?
C30A N29A Fe1A 142.4(3) . . ?
C30A N29A N28A 104.9(3) . . ?
N29A C30A H30A 124.4 . . ?
N29A C30A C31A 111.3(3) . . ?
C31A C30A H30A 124.4 . . ?
C30A C31A H31A 126.9 . . ?
C32A C31A C30A 106.1(4) . . ?
C32A C31A H31A 126.9 . . ?
N28A C32A C31A 106.7(4) . . ?
N28A C32A H32A 126.6 . . ?
C31A C32A H32A 126.6 . . ?
N34A N33A C27A 116.5(3) . . ?
C37A N33A C27A 132.7(3) . . ?
C37A N33A N34A 110.7(3) . . ?
N33A N34A Fe1A 113.6(2) . . ?
C35A N34A Fe1A 140.5(3) . . ?
C35A N34A N33A 105.7(3) . . ?
N34A C35A H35A 124.5 . . ?
N34A C35A C36A 110.9(3) . . ?
C36A C35A H35A 124.5 . . ?
C35A C36A H36A 126.9 . . ?
C37A C36A C35A 106.1(4) . . ?
C37A C36A H36A 126.9 . . ?
N33A C37A C36A 106.5(4) . . ?
N33A C37A H37A 126.7 . . ?
C36A C37A H37A 126.7 . . ?
C25A N38A H38A 116.1 . . ?
C39A N38A C25A 127.7(3) . . ?
C39A N38A H38A 116.1 . . ?
N38A C39A C41A 113.4(4) . . ?
O40A C39A N38A 123.0(4) . . ?
O40A C39A C41A 123.6(4) . . ?
C39A C41A H41A 109.5 . . ?
C39A C41A H41B 109.5 . . ?
C39A C41A H41C 109.5 . . ?
H41A C41A H41B 109.5 . . ?
H41A C41A H41C 109.5 . . ?
H41B C41A H41C 109.5 . . ?
N2B Fe1B N9B 73.61(12) . . ?
N2B Fe1B N14B 73.55(12) . . ?
N2B Fe1B N29B 115.18(12) . . ?
N2B Fe1B N34B 96.06(11) . . ?
N14B Fe1B N9B 146.83(12) . . ?
N22B Fe1B N2B 166.31(12) . . ?
N22B Fe1B N9B 96.25(12) . . ?
N22B Fe1B N14B 116.92(12) . . ?
N22B Fe1B N29B 74.20(11) . . ?
N22B Fe1B N34B 73.98(11) . . ?
N29B Fe1B N9B 95.08(13) . . ?
N29B Fe1B N14B 94.60(13) . . ?
N34B Fe1B N9B 87.74(12) . . ?
N34B Fe1B N14B 100.23(12) . . ?
N34B Fe1B N29B 148.18(11) . . ?
C3B N2B Fe1B 120.7(3) . . ?
C7B N2B Fe1B 121.3(2) . . ?
C7B N2B C3B 118.0(3) . . ?
N2B C3B C4B 123.3(4) . . ?
N2B C3B N8B 113.0(3) . . ?
C4B C3B N8B 123.6(3) . . ?
C3B C4B H4B 121.2 . . ?
C3B C4B C5B 117.5(4) . . ?
C5B C4B H4B 121.2 . . ?
C4B C5B C6B 120.6(3) . . ?
C4B C5B N18B 116.7(4) . . ?
N18B C5B C6B 122.7(4) . . ?
C5B C6B H6B 122.1 . . ?
C7B C6B C5B 115.8(3) . . ?
C7B C6B H6B 122.1 . . ?
N2B C7B C6B 124.8(3) . . ?
N2B C7B N13B 112.2(3) . . ?
C6B C7B N13B 123.1(3) . . ?
N9B N8B C3B 118.3(3) . . ?
N9B N8B C12B 111.1(3) . . ?
C12B N8B C3B 130.6(3) . . ?
N8B N9B Fe1B 113.9(2) . . ?
C10B N9B Fe1B 140.2(3) . . ?
C10B N9B N8B 105.1(3) . . ?
N9B C10B H10B 124.7 . . ?
N9B C10B C11B 110.5(4) . . ?
C11B C10B H10B 124.7 . . ?
C10B C11B H11B 126.6 . . ?
C12B C11B C10B 106.9(4) . . ?
C12B C11B H11B 126.6 . . ?
N8B C12B H12B 126.8 . . ?
C11B C12B N8B 106.4(4) . . ?
C11B C12B H12B 126.8 . . ?
N14B N13B C7B 117.9(3) . . ?
C17B N13B C7B 130.6(3) . . ?
C17B N13B N14B 111.4(3) . . ?
N13B N14B Fe1B 114.8(2) . . ?
C15B N14B Fe1B 140.6(3) . . ?
C15B N14B N13B 104.3(3) . . ?
N14B C15B H15B 124.0 . . ?
N14B C15B C16B 112.0(4) . . ?
C16B C15B H15B 124.0 . . ?
C15B C16B H16B 127.4 . . ?
C17B C16B C15B 105.2(4) . . ?
C17B C16B H16B 127.4 . . ?
N13B C17B C16B 107.1(4) . . ?
N13B C17B H17B 126.4 . . ?
C16B C17B H17B 126.4 . . ?
C5B N18B H18B 116.9 . . ?
C19B N18B C5B 126.3(4) . . ?
C19B N18B H18B 116.9 . . ?
N18B C19B C21B 113.2(4) . . ?
O20B C19B N18B 122.9(4) . . ?
O20B C19B C21B 123.8(4) . . ?
C19B C21B H21D 109.5 . . ?
C19B C21B H21E 109.5 . . ?
C19B C21B H21F 109.5 . . ?
H21D C21B H21E 109.5 . . ?
H21D C21B H21F 109.5 . . ?
H21E C21B H21F 109.5 . . ?
C23B N22B Fe1B 121.0(2) . . ?
C27B N22B Fe1B 121.1(2) . . ?
C27B N22B C23B 117.9(3) . . ?
N22B C23B C24B 123.9(3) . . ?
N22B C23B N28B 112.4(3) . . ?
C24B C23B N28B 123.7(3) . . ?
C23B C24B H24B 121.4 . . ?
C23B C24B C25B 117.2(3) . . ?
C25B C24B H24B 121.4 . . ?
C26B C25B C24B 120.4(3) . . ?
N38B C25B C24B 116.4(3) . . ?
N38B C25B C26B 123.2(3) . . ?
C25B C26B H26B 122.0 . . ?
C27B C26B C25B 116.0(3) . . ?
C27B C26B H26B 122.0 . . ?
N22B C27B C26B 124.6(3) . . ?
N22B C27B N33B 112.4(3) . . ?
C26B C27B N33B 123.1(3) . . ?
N29B N28B C23B 118.4(3) . . ?
C32B N28B C23B 130.3(3) . . ?
C32B N28B N29B 111.2(3) . . ?
N28B N29B Fe1B 114.1(2) . . ?
C30B N29B Fe1B 141.0(3) . . ?
C30B N29B N28B 104.6(3) . . ?
N29B C30B H30B 124.2 . . ?
N29B C30B C31B 111.6(4) . . ?
C31B C30B H30B 124.2 . . ?
C30B C31B H31B 127.3 . . ?
C32B C31B C30B 105.5(4) . . ?
C32B C31B H31B 127.3 . . ?
N28B C32B C31B 107.1(4) . . ?
N28B C32B H32B 126.4 . . ?
C31B C32B H32B 126.4 . . ?
N34B N33B C27B 117.3(3) . . ?
C37B N33B C27B 131.0(3) . . ?
C37B N33B N34B 111.4(3) . . ?
N33B N34B Fe1B 115.2(2) . . ?
C35B N34B Fe1B 139.2(3) . . ?
C35B N34B N33B 105.1(3) . . ?
N34B C35B H35B 124.6 . . ?
N34B C35B C36B 110.7(3) . . ?
C36B C35B H35B 124.6 . . ?
C35B C36B H36B 126.8 . . ?
C37B C36B C35B 106.4(4) . . ?
C37B C36B H36B 126.8 . . ?
N33B C37B C36B 106.3(4) . . ?
N33B C37B H37B 126.9 . . ?
C36B C37B H37B 126.9 . . ?
C25B N38B H38B 116.1 . . ?
C39B N38B C25B 127.8(3) . . ?
C39B N38B H38B 116.1 . . ?
N38B C39B C41B 112.8(4) . . ?
O40B C39B N38B 123.3(4) . . ?
O40B C39B C41B 123.9(4) . . ?
C39B C41B H41D 109.5 . . ?
C39B C41B H41E 109.5 . . ?
C39B C41B H41F 109.5 . . ?
H41D C41B H41E 109.5 . . ?
H41D C41B H41F 109.5 . . ?
H41E C41B H41F 109.5 . . ?
F43 B42 F44 111.0(9) . . ?
F43 B42 F45 109.7(8) . . ?
F43 B42 F46 114.6(10) . . ?
F45 B42 F44 105.0(8) . . ?
F46 B42 F44 104.5(8) . . ?
F46 B42 F45 111.5(8) . . ?
O43 Cl42 O44 108.3(4) . . ?
O43 Cl42 O45 117.8(4) . . ?
O43 Cl42 O46 112.1(4) . . ?
O44 Cl42 O46 106.7(4) . . ?
O45 Cl42 O44 105.7(4) . . ?
O45 Cl42 O46 105.6(4) . . ?
F48 B47 F50 107.6(7) . . ?
F48 B47 F51 119.5(8) . . ?
F49 B47 F48 108.9(8) . . ?
F49 B47 F50 112.1(7) . . ?
F49 B47 F51 108.8(7) . . ?
F50 B47 F51 99.7(6) . . ?
O48 Cl47 O49 124.1(5) . . ?
O48 Cl47 O50 108.4(4) . . ?
O48 Cl47 O51 94.8(5) . . ?
O49 Cl47 O51 108.2(5) . . ?
O50 Cl47 O49 109.6(4) . . ?
O50 Cl47 O51 110.5(5) . . ?
F53 B52 F54 102.2(8) . . ?
F55 B52 F53 113.8(8) . . ?
F55 B52 F54 104.9(8) . . ?
F55 B52 F56 118.7(9) . . ?
F56 B52 F53 107.5(7) . . ?
F56 B52 F54 108.3(8) . . ?
O53 Cl52 O54 100.1(4) . . ?
O55 Cl52 O53 113.5(4) . . ?
O55 Cl52 O54 107.9(4) . . ?
O55 Cl52 O56 117.7(4) . . ?
O56 Cl52 O53 113.7(4) . . ?
O56 Cl52 O54 101.2(4) . . ?
F58 B57 F60 91.1(7) . . ?
F58 B57 F61 100.2(8) . . ?
F59 B57 F58 135.5(10) . . ?
F59 B57 F60 108.4(8) . . ?
F59 B57 F61 115.2(9) . . ?
F61 B57 F60 98.4(7) . . ?
O58 Cl57 O59 93.7(4) . . ?
O60 Cl57 O58 126.3(5) . . ?
O60 Cl57 O59 110.3(4) . . ?
O60 Cl57 O61 110.3(5) . . ?
O61 Cl57 O58 107.8(4) . . ?
O61 Cl57 O59 105.8(4) . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C63 C62 H62A 109.5 . . ?
C63 C62 H62B 109.5 . . ?
C63 C62 H62C 109.5 . . ?
C62 C63 H63A 110.7 . . ?
C62 C63 H63B 110.7 . . ?
C62 C63 C64 105.1(7) . . ?
H63A C63 H63B 108.8 . . ?
C64 C63 H63A 110.7 . . ?
C64 C63 H63B 110.7 . . ?
N65 C64 C63 175.0(8) . . ?
H66A C66A H66B 109.5 . . ?
H66A C66A H66C 109.5 . . ?
H66B C66A H66C 109.5 . . ?
C67A C66A H66A 109.5 . . ?
C67A C66A H66B 109.5 . . ?
C67A C66A H66C 109.5 . . ?
C66A C67A H67A 109.3 . . ?
C66A C67A H67B 109.3 . . ?
H67A C67A H67B 107.9 . . ?
C68A C67A C66A 111.7(7) . . ?
C68A C67A H67A 109.3 . . ?
C68A C67A H67B 109.3 . . ?
N69A C68A C67A 169.3(9) . . ?
H66D C66B H66E 109.5 . . ?
H66D C66B H66F 109.5 . . ?
H66E C66B H66F 109.5 . . ?
C67B C66B H66D 109.5 . . ?
C67B C66B H66E 109.5 . . ?
C67B C66B H66F 109.5 . . ?
C66B C67B H67C 109.5 . . ?
C66B C67B H67D 109.5 . . ?
C66B C67B C68B 110.5(15) . . ?
H67C C67B H67D 108.1 . . ?
C68B C67B H67C 109.5 . . ?
C68B C67B H67D 109.5 . . ?
N69B C68B C67B 170(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N18A H18A F46 0.88 1.98 2.793(10) 154.1 . yes
N18A H18A O46 0.88 2.17 2.995(8) 156.6 . yes
N38A H38A F49 0.88 1.94 2.820(7) 177.5 . yes
N38A H38A O49 0.88 2.08 2.948(7) 168.5 . yes
N18B H18B F53 0.88 2.27 3.078(9) 152.6 . yes
N18B H18B O53 0.88 2.02 2.823(8) 152.0 . yes
N38B H38B F59 0.88 1.97 2.849(8) 178.4 . yes
N38B H38B O59 0.88 2.01 2.869(7) 165.4 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1A N2A C3A C4A -176.6(3) . . . . ?
Fe1A N2A C3A N8A 3.3(4) . . . . ?
Fe1A N2A C7A C6A 176.8(3) . . . . ?
Fe1A N2A C7A N13A -2.2(4) . . . . ?
Fe1A N9A C10A C11A -172.8(4) . . . . ?
Fe1A N14A C15A C16A 176.8(3) . . . . ?
Fe1A N22A C23A C24A 175.3(3) . . . . ?
Fe1A N22A C23A N28A -3.4(4) . . . . ?
Fe1A N22A C27A C26A -174.0(3) . . . . ?
Fe1A N22A C27A N33A 4.4(4) . . . . ?
Fe1A N29A C30A C31A 172.0(3) . . . . ?
Fe1A N34A C35A C36A -173.4(3) . . . . ?
N2A C3A C4A C5A 0.5(6) . . . . ?
N2A C3A N8A N9A -0.1(5) . . . . ?
N2A C3A N8A C12A -177.6(4) . . . . ?
N2A C7A N13A N14A -0.8(4) . . . . ?
N2A C7A N13A C17A -179.7(4) . . . . ?
C3A N2A C7A C6A 3.3(5) . . . . ?
C3A N2A C7A N13A -175.7(3) . . . . ?
C3A C4A C5A C6A 1.9(6) . . . . ?
C3A C4A C5A N18A -178.7(3) . . . . ?
C3A N8A N9A Fe1A -2.9(4) . . . . ?
C3A N8A N9A C10A -178.8(3) . . . . ?
C3A N8A C12A C11A 177.5(4) . . . . ?
C4A C3A N8A N9A 179.8(4) . . . . ?
C4A C3A N8A C12A 2.3(7) . . . . ?
C4A C5A C6A C7A -1.7(5) . . . . ?
C4A C5A N18A C19A 160.7(4) . . . . ?
C5A C6A C7A N2A -1.0(6) . . . . ?
C5A C6A C7A N13A 177.9(3) . . . . ?
C5A N18A C19A O20A 0.4(8) . . . . ?
C5A N18A C19A C21A -177.6(4) . . . . ?
C6A C5A N18A C19A -20.0(6) . . . . ?
C6A C7A N13A N14A -179.8(3) . . . . ?
C6A C7A N13A C17A 1.3(6) . . . . ?
C7A N2A C3A C4A -3.0(5) . . . . ?
C7A N2A C3A N8A 176.9(3) . . . . ?
C7A N13A N14A Fe1A 3.1(4) . . . . ?
C7A N13A N14A C15A -178.8(3) . . . . ?
C7A N13A C17A C16A 178.7(4) . . . . ?
N8A C3A C4A C5A -179.4(4) . . . . ?
N8A N9A C10A C11A 1.2(5) . . . . ?
N9A N8A C12A C11A -0.1(5) . . . . ?
N9A C10A C11A C12A -1.3(6) . . . . ?
C10A C11A C12A N8A 0.8(5) . . . . ?
C12A N8A N9A Fe1A 175.2(3) . . . . ?
C12A N8A N9A C10A -0.7(4) . . . . ?
N13A N14A C15A C16A -0.3(4) . . . . ?
N14A N13A C17A C16A -0.2(4) . . . . ?
N14A C15A C16A C17A 0.2(5) . . . . ?
C15A C16A C17A N13A 0.0(5) . . . . ?
C17A N13A N14A Fe1A -177.8(3) . . . . ?
C17A N13A N14A C15A 0.3(4) . . . . ?
N18A C5A C6A C7A 179.0(4) . . . . ?
N22A C23A C24A C25A -2.2(5) . . . . ?
N22A C23A N28A N29A 0.6(4) . . . . ?
N22A C23A N28A C32A 175.7(4) . . . . ?
N22A C27A N33A N34A -2.3(4) . . . . ?
N22A C27A N33A C37A -178.0(4) . . . . ?
C23A N22A C27A C26A -2.0(5) . . . . ?
C23A N22A C27A N33A 176.3(3) . . . . ?
C23A C24A C25A C26A -0.3(5) . . . . ?
C23A C24A C25A N38A -177.7(3) . . . . ?
C23A N28A N29A Fe1A 2.1(4) . . . . ?
C23A N28A N29A C30A 177.1(3) . . . . ?
C23A N28A C32A C31A -176.6(4) . . . . ?
C24A C23A N28A N29A -178.0(3) . . . . ?
C24A C23A N28A C32A -2.9(7) . . . . ?
C24A C25A C26A C27A 1.5(6) . . . . ?
C24A C25A N38A C39A -178.1(4) . . . . ?
C25A C26A C27A N22A -0.3(6) . . . . ?
C25A C26A C27A N33A -178.4(3) . . . . ?
C25A N38A C39A O40A 3.3(7) . . . . ?
C25A N38A C39A C41A -176.4(4) . . . . ?
C26A C25A N38A C39A 4.7(7) . . . . ?
C26A C27A N33A N34A 176.1(3) . . . . ?
C26A C27A N33A C37A 0.3(7) . . . . ?
C27A N22A C23A C24A 3.3(5) . . . . ?
C27A N22A C23A N28A -175.3(3) . . . . ?
C27A N33A N34A Fe1A -0.6(4) . . . . ?
C27A N33A N34A C35A -176.1(3) . . . . ?
C27A N33A C37A C36A 174.9(4) . . . . ?
N28A C23A C24A C25A 176.3(3) . . . . ?
N28A N29A C30A C31A -0.4(5) . . . . ?
N29A N28A C32A C31A -1.3(5) . . . . ?
N29A C30A C31A C32A -0.3(5) . . . . ?
C30A C31A C32A N28A 1.0(5) . . . . ?
C32A N28A N29A Fe1A -174.0(3) . . . . ?
C32A N28A N29A C30A 1.0(4) . . . . ?
N33A N34A C35A C36A 0.1(4) . . . . ?
N34A N33A C37A C36A -1.0(5) . . . . ?
N34A C35A C36A C37A -0.7(5) . . . . ?
C35A C36A C37A N33A 1.0(5) . . . . ?
C37A N33A N34A Fe1A 176.0(3) . . . . ?
C37A N33A N34A C35A 0.6(4) . . . . ?
N38A C25A C26A C27A 178.6(3) . . . . ?
Fe1B N2B C3B C4B 179.8(3) . . . . ?
Fe1B N2B C3B N8B -0.5(4) . . . . ?
Fe1B N2B C7B C6B 179.4(3) . . . . ?
Fe1B N2B C7B N13B -0.5(4) . . . . ?
Fe1B N9B C10B C11B 167.6(3) . . . . ?
Fe1B N14B C15B C16B -172.0(3) . . . . ?
Fe1B N22B C23B C24B 179.5(3) . . . . ?
Fe1B N22B C23B N28B -1.2(4) . . . . ?
Fe1B N22B C27B C26B 179.5(3) . . . . ?
Fe1B N22B C27B N33B 0.7(4) . . . . ?
Fe1B N29B C30B C31B -171.7(4) . . . . ?
Fe1B N34B C35B C36B 170.5(3) . . . . ?
N2B C3B C4B C5B 0.9(6) . . . . ?
N2B C3B N8B N9B -4.6(5) . . . . ?
N2B C3B N8B C12B 174.3(4) . . . . ?
N2B C7B N13B N14B 4.9(5) . . . . ?
N2B C7B N13B C17B -177.1(4) . . . . ?
C3B N2B C7B C6B -1.2(5) . . . . ?
C3B N2B C7B N13B 178.8(3) . . . . ?
C3B C4B C5B C6B -1.5(6) . . . . ?
C3B C4B C5B N18B 178.1(4) . . . . ?
C3B N8B N9B Fe1B 7.2(4) . . . . ?
C3B N8B N9B C10B 179.1(3) . . . . ?
C3B N8B C12B C11B -178.2(4) . . . . ?
C4B C3B N8B N9B 175.1(4) . . . . ?
C4B C3B N8B C12B -6.0(7) . . . . ?
C4B C5B C6B C7B 0.8(6) . . . . ?
C4B C5B N18B C19B -158.6(4) . . . . ?
C5B C6B C7B N2B 0.6(6) . . . . ?
C5B C6B C7B N13B -179.5(3) . . . . ?
C5B N18B C19B O20B -2.5(8) . . . . ?
C5B N18B C19B C21B 176.2(4) . . . . ?
C6B C5B N18B C19B 21.0(7) . . . . ?
C6B C7B N13B N14B -175.1(3) . . . . ?
C6B C7B N13B C17B 3.0(6) . . . . ?
C7B N2B C3B C4B 0.4(5) . . . . ?
C7B N2B C3B N8B -179.8(3) . . . . ?
C7B N13B N14B Fe1B -6.8(4) . . . . ?
C7B N13B N14B C15B 178.7(3) . . . . ?
C7B N13B C17B C16B -178.7(4) . . . . ?
N8B C3B C4B C5B -178.8(4) . . . . ?
N8B N9B C10B C11B -0.7(5) . . . . ?
N9B N8B C12B C11B 0.7(5) . . . . ?
N9B C10B C11B C12B 1.2(6) . . . . ?
C10B C11B C12B N8B -1.1(5) . . . . ?
C12B N8B N9B Fe1B -171.9(3) . . . . ?
C12B N8B N9B C10B 0.0(5) . . . . ?
N13B N14B C15B C16B 0.0(5) . . . . ?
N14B N13B C17B C16B -0.5(5) . . . . ?
N14B C15B C16B C17B -0.4(5) . . . . ?
C15B C16B C17B N13B 0.5(5) . . . . ?
C17B N13B N14B Fe1B 174.8(3) . . . . ?
C17B N13B N14B C15B 0.3(4) . . . . ?
N18B C5B C6B C7B -178.7(4) . . . . ?
N22B C23B C24B C25B 1.4(6) . . . . ?
N22B C23B N28B N29B 2.5(5) . . . . ?
N22B C23B N28B C32B -173.0(4) . . . . ?
N22B C27B N33B N34B -1.7(5) . . . . ?
N22B C27B N33B C37B 172.5(4) . . . . ?
C23B N22B C27B C26B 0.4(5) . . . . ?
C23B N22B C27B N33B -178.4(3) . . . . ?
C23B C24B C25B C26B -0.6(6) . . . . ?
C23B C24B C25B N38B 177.8(3) . . . . ?
C23B N28B N29B Fe1B -2.6(4) . . . . ?
C23B N28B N29B C30B -177.4(4) . . . . ?
C23B N28B C32B C31B 176.8(4) . . . . ?
C24B C23B N28B N29B -178.2(3) . . . . ?
C24B C23B N28B C32B 6.3(6) . . . . ?
C24B C25B C26B C27B -0.2(6) . . . . ?
C24B C25B N38B C39B 175.4(4) . . . . ?
C25B C26B C27B N22B 0.4(6) . . . . ?
C25B C26B C27B N33B 179.1(3) . . . . ?
C25B N38B C39B O40B -5.2(8) . . . . ?
C25B N38B C39B C41B 175.6(4) . . . . ?
C26B C25B N38B C39B -6.3(7) . . . . ?
C26B C27B N33B N34B 179.5(3) . . . . ?
C26B C27B N33B C37B -6.4(7) . . . . ?
C27B N22B C23B C24B -1.4(5) . . . . ?
C27B N22B C23B N28B 177.9(3) . . . . ?
C27B N33B N34B Fe1B 1.9(4) . . . . ?
C27B N33B N34B C35B 175.3(3) . . . . ?
C27B N33B C37B C36B -174.1(4) . . . . ?
N28B C23B C24B C25B -177.7(3) . . . . ?
N28B N29B C30B C31B 0.8(5) . . . . ?
N29B N28B C32B C31B 1.0(5) . . . . ?
N29B C30B C31B C32B -0.2(6) . . . . ?
C30B C31B C32B N28B -0.5(6) . . . . ?
C32B N28B N29B Fe1B 173.7(3) . . . . ?
C32B N28B N29B C30B -1.1(5) . . . . ?
N33B N34B C35B C36B -0.4(5) . . . . ?
N34B N33B C37B C36B 0.3(5) . . . . ?
N34B C35B C36B C37B 0.6(6) . . . . ?
C35B C36B C37B N33B -0.5(5) . . . . ?
C37B N33B N34B Fe1B -173.4(3) . . . . ?
C37B N33B N34B C35B 0.0(4) . . . . ?
N38B C25B C26B C27B -178.5(4) . . . . ?
C66A C67A C68A N69A 19(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: propionitrile/diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_etcnclht
_database_code_depnum_ccdc_archive 'CCDC 2078655'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2021-04-19 deposited with the CCDC.	2021-06-10 downloaded from the CCDC.
;
_audit_creation_date             2020-07-21
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis-[N-(2,6-di{pyrazol-1-yl}pyrid-4-yl)acetamide]iron(II)diperchlorate propionitrile solvate'
_chemical_formula_moiety         'C26 H24 Fe N12 O2, 2(Cl O4), C3 H5 N'
_chemical_formula_sum            'C29 H29 Cl2 Fe N13 O10'
_chemical_formula_weight         846.40
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.3297(4)
_cell_length_b                   12.6635(8)
_cell_length_c                   18.0861(10)
_cell_angle_alpha                83.662(5)
_cell_angle_beta                 80.003(4)
_cell_angle_gamma                80.933(5)
_cell_volume                     1848.56(18)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5120
_cell_measurement_temperature    240(2)
_cell_measurement_theta_max      73.50
_cell_measurement_theta_min      3.52
_exptl_absorpt_coefficient_mu    5.236
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.943
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11656
_diffrn_reflns_point_group_measured_fraction_full 0.943
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.743
_diffrn_reflns_theta_min         3.547
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      240(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9056
_reflns_number_total             11656
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2015)'
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.920
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         11656
_refine_ls_number_restraints     68
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0760
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1346P)²+0.8521P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2052
_refine_ls_wR_factor_ref         0.2177
_refine_special_details          
;The data were resolved into two non-superimposable twin domains, in a 
 ratio of 0.76:0.24.

 The C atoms of one pyrazole ring in the complex cation were modelled as 
 disordered over two half-occupied sites, to resolve an intermolecular
 steric clash. Both ClO₄⁻ ions are disordered, over two or three 
 equally occupied sites. The propionitrile molecule is also disordered 
 over two half-occupied orientations. The bond distance restraints that 
 were applied to the disordered residues are listed below.

 All crystallographically ordered non-H atoms were refined anisotropically,
 and H atoms were placed in calculated positions and refined using a 
 riding model.,Twin
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.5807(15)
 0.4193(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N14-C15A = N14-C15B
 1.32 with sigma of 0.01
 C15A-C16A = C15B-C16B
 1.39 with sigma of 0.01
 C16A-C17A = C16B-C17B
 1.37 with sigma of 0.01
 N13-C17A = N13-C17B
 1.36 with sigma of 0.01
 Cl2A-O43A = Cl2A-O44A = Cl2A-O45A = Cl2A-O46A
 1.44708 with sigma of 0.02
 Cl2B-O43B = Cl2B-O44B = Cl2B-O45B = Cl2B-O46B
 1.44708 with sigma of 0.02
 O43A-O44A = O43A-O45A = O43A-O46A = O44A-O45A = O44A-O46A = O45A-O46A
 2.363082 with sigma of 0.02
 O43B-O44B = O43B-O45B = O43B-O46B = O44B-O45B = O44B-O46B = O45B-O46B
 2.363082 with sigma of 0.02
 Cl7A-O48A = Cl7A-O49A = Cl7A-O50A = Cl7A-O51A
 1.44708 with sigma of 0.02
 Cl7B-O48B = Cl7B-O49B = Cl7B-O50B = Cl7B-O51B
 1.44708 with sigma of 0.02
 Cl7C-O48C = Cl7C-O49C = Cl7C-O50C = Cl7C-O51C
 1.44708 with sigma of 0.02
 O48A-O49A = O48A-O50A = O48A-O51A = O49A-O50A = O49A-O51A = O50A-O51A
 2.363082 with sigma of 0.02
 O48B-O49B = O48B-O50B = O48B-O51B = O49B-O50B = O49B-O51B = O50B-O51B
 2.363082 with sigma of 0.02
 O48C-O49C = O48C-O50C = O48C-O51C = O49C-O50C = O49C-O51C = O50C-O51C
 2.363082 with sigma of 0.02
 C52A-C53A = C52B-C53B
 1.51 with sigma of 0.02
 C53A-C54A = C53B-C54B
 1.48 with sigma of 0.02
 C54A-N55A = C54B-N55B
 1.15 with sigma of 0.02
 C52A-C54A = C52B-C54B
 2.44 with sigma of 0.02
 C53A-N55A = C53B-N55B
 2.63 with sigma of 0.02
4. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: C15A(0.5) H15A(0.5) C16A(0.5) H16A(0.5) C17A(0.5) H17A(0.5)
 C15B(0.5) H15B(0.5) C16B(0.5) H16B(0.5) C17B(0.5) H17B(0.5) Cl2A(0.5)
 O43A(0.5) O44A(0.5) O45A(0.5) O46A(0.5) Cl2B(0.5) O43B(0.5) O44B(0.5)
 O45B(0.5) O46B(0.5) Cl7A(0.34) O48A(0.34) O49A(0.34) O50A(0.34) O51A(0.34)
 Cl7B(0.33) O48B(0.33) O49B(0.33) O50B(0.33) O51B(0.33) Cl7C(0.33) O48C(0.33)
 O49C(0.33) O50C(0.33) O51C(0.33) C53A(0.5) H53A(0.5) H53B(0.5) C52A(0.5)
 H52A(0.5) H52B(0.5) H52C(0.5) C54A(0.5) N55A(0.5) C52B(0.5) H52D(0.5)
 H52E(0.5) H52F(0.5) C53B(0.5) H53C(0.5) H53D(0.5) C54B(0.5) N55B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C53A(H53A,H53B), C53B(H53C,H53D)
5.b Me refined with riding coordinates:
 C52A(H52A,H52B,H52C), C52B(H52D,H52E,H52F)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C15A(H15A), C16A(H16A),
 C17A(H17A), C15B(H15B), C16B(H16B), C17B(H17B), N18(H18), C24(H24), C26(H26),
 C30(H30), C31(H31), C32(H32), C35(H35), C36(H36), C37(H37), N38(H38)
5.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C41(H41A,H41B,H41C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.78267(10) 0.77550(6) 0.72433(4) 0.0343(2) Uani 1 1 d . . . . .
N2 N 0.8134(5) 0.6253(3) 0.6787(2) 0.0285(8) Uani 1 1 d . . . . .
C3 C 0.7897(6) 0.6184(3) 0.6085(2) 0.0284(9) Uani 1 1 d . . . . .
C4 C 0.8099(6) 0.5241(4) 0.5752(3) 0.0337(10) Uani 1 1 d . . . . .
H4 H 0.794707 0.523099 0.524956 0.040 Uiso 1 1 calc R U . . .
C5 C 0.8544(6) 0.4288(4) 0.6193(3) 0.0357(10) Uani 1 1 d . . . . .
C6 C 0.8778(6) 0.4338(4) 0.6938(3) 0.0370(11) Uani 1 1 d . . . . .
H6 H 0.906393 0.371437 0.724834 0.044 Uiso 1 1 calc R U . . .
C7 C 0.8571(6) 0.5337(4) 0.7191(3) 0.0315(10) Uani 1 1 d . . . . .
N8 N 0.7398(5) 0.7193(3) 0.5714(2) 0.0332(8) Uani 1 1 d . . . . .
N9 N 0.7276(6) 0.8082(3) 0.6097(2) 0.0386(9) Uani 1 1 d . . . . .
C10 C 0.6707(8) 0.8888(4) 0.5626(3) 0.0488(14) Uani 1 1 d . . . . .
H10 H 0.651026 0.961285 0.572886 0.059 Uiso 1 1 calc R U . . .
C11 C 0.6442(9) 0.8526(5) 0.4964(4) 0.0574(16) Uani 1 1 d . . . . .
H11 H 0.603849 0.894030 0.455437 0.069 Uiso 1 1 calc R U . . .
C12 C 0.6894(8) 0.7441(4) 0.5038(3) 0.0461(13) Uani 1 1 d . . . . .
H12 H 0.686031 0.695715 0.468473 0.055 Uiso 1 1 calc R U . . .
N13 N 0.8771(5) 0.5510(3) 0.7926(2) 0.0367(9) Uani 1 1 d D . . . .
N14 N 0.8545(5) 0.6535(3) 0.8119(2) 0.0376(9) Uani 1 1 d D . . . .
C15A C 0.860(2) 0.6550(11) 0.8837(5) 0.038(4) Uiso 0.5 1 d D . P A 1
H15A H 0.853519 0.716426 0.909510 0.046 Uiso 0.5 1 calc R U P A 1
C16A C 0.8781(17) 0.5484(9) 0.9149(6) 0.045(3) Uiso 0.5 1 d D . P A 1
H16A H 0.883016 0.524630 0.965704 0.053 Uiso 0.5 1 calc R U P A 1
C17A C 0.8871(16) 0.4854(8) 0.8569(5) 0.035(3) Uiso 0.5 1 d D . P A 1
H17A H 0.898208 0.410012 0.860899 0.042 Uiso 0.5 1 calc R U P A 1
C15B C 0.883(2) 0.6365(12) 0.8830(6) 0.049(5) Uiso 0.5 1 d D . P A 2
H15B H 0.871749 0.691966 0.914803 0.059 Uiso 0.5 1 calc R U P A 2
C16B C 0.9315(19) 0.5299(10) 0.9054(7) 0.055(4) Uiso 0.5 1 d D . P A 2
H16B H 0.957186 0.501448 0.952888 0.066 Uiso 0.5 1 calc R U P A 2
C17B C 0.9343(18) 0.4746(9) 0.8443(6) 0.049(4) Uiso 0.5 1 d D . P A 2
H17B H 0.967804 0.400958 0.839300 0.059 Uiso 0.5 1 calc R U P A 2
N18 N 0.8695(6) 0.3335(3) 0.5855(3) 0.0465(11) Uani 1 1 d . . . . .
H18 H 0.846464 0.339274 0.539954 0.056 Uiso 1 1 calc R U . . .
C19 C 0.9171(8) 0.2307(4) 0.6160(4) 0.0538(15) Uani 1 1 d . . . . .
O20 O 0.9547(9) 0.2120(3) 0.6766(3) 0.0870(19) Uani 1 1 d . . . . .
C21 C 0.9103(10) 0.1463(5) 0.5645(5) 0.068(2) Uani 1 1 d . . . . .
H21A H 0.972171 0.078995 0.581163 0.103 Uiso 1 1 calc R U . . .
H21B H 0.957820 0.168866 0.513462 0.103 Uiso 1 1 calc R U . . .
H21C H 0.796643 0.136626 0.565704 0.103 Uiso 1 1 calc R U . . .
N22 N 0.7144(5) 0.9058(3) 0.7939(2) 0.0321(8) Uani 1 1 d . . . . .
C23 C 0.5668(6) 0.9213(4) 0.8356(3) 0.0333(10) Uani 1 1 d . . . . .
C24 C 0.5154(6) 1.0048(4) 0.8802(3) 0.0378(11) Uani 1 1 d . . . . .
H24 H 0.410449 1.012340 0.909806 0.045 Uiso 1 1 calc R U . . .
C25 C 0.6230(7) 1.0776(4) 0.8801(3) 0.0392(11) Uani 1 1 d . . . . .
C26 C 0.7806(7) 1.0636(4) 0.8372(3) 0.0400(11) Uani 1 1 d . . . . .
H26 H 0.856431 1.111497 0.836450 0.048 Uiso 1 1 calc R U . . .
C27 C 0.8173(6) 0.9751(4) 0.7963(3) 0.0316(10) Uani 1 1 d . . . . .
N28 N 0.4668(5) 0.8440(3) 0.8288(2) 0.0378(9) Uani 1 1 d . . . . .
N29 N 0.5249(6) 0.7703(3) 0.7778(3) 0.0409(10) Uani 1 1 d . . . . .
C30 C 0.4105(7) 0.7074(5) 0.7848(4) 0.0518(14) Uani 1 1 d . . . . .
H30 H 0.416905 0.648860 0.756072 0.062 Uiso 1 1 calc R U . . .
C31 C 0.2784(8) 0.7391(5) 0.8405(4) 0.0598(16) Uani 1 1 d . . . . .
H31 H 0.182819 0.706540 0.856143 0.072 Uiso 1 1 calc R U . . .
C32 C 0.3158(7) 0.8264(5) 0.8675(4) 0.0520(14) Uani 1 1 d . . . . .
H32 H 0.250953 0.866746 0.905401 0.062 Uiso 1 1 calc R U . . .
N33 N 0.9710(5) 0.9498(3) 0.7500(2) 0.0337(9) Uani 1 1 d . . . . .
N34 N 0.9893(5) 0.8668(3) 0.7055(3) 0.0389(9) Uani 1 1 d . . . . .
C35 C 1.1424(7) 0.8628(4) 0.6686(3) 0.0470(13) Uani 1 1 d . . . . .
H35 H 1.191207 0.812760 0.633649 0.056 Uiso 1 1 calc R U . . .
C36 C 1.2215(7) 0.9426(4) 0.6884(4) 0.0472(13) Uani 1 1 d . . . . .
H36 H 1.329636 0.956167 0.670095 0.057 Uiso 1 1 calc R U . . .
C37 C 1.1082(7) 0.9963(4) 0.7400(3) 0.0413(12) Uani 1 1 d . . . . .
H37 H 1.123350 1.055218 0.764142 0.050 Uiso 1 1 calc R U . . .
N38 N 0.5680(6) 1.1643(4) 0.9241(3) 0.0497(12) Uani 1 1 d . . . . .
H38 H 0.488933 1.156030 0.961642 0.060 Uiso 1 1 calc R U . . .
C39 C 0.6264(9) 1.2607(5) 0.9137(4) 0.0587(16) Uani 1 1 d . . . . .
O40 O 0.7370(7) 1.2809(4) 0.8639(3) 0.0776(15) Uani 1 1 d . . . . .
C41 C 0.5346(12) 1.3419(6) 0.9669(5) 0.083(2) Uani 1 1 d . . . . .
H41A H 0.476200 1.305125 1.010805 0.124 Uiso 1 1 calc R U . . .
H41B H 0.456431 1.391557 0.941481 0.124 Uiso 1 1 calc R U . . .
H41C H 0.612259 1.381204 0.982426 0.124 Uiso 1 1 calc R U . . .
Cl2A Cl 0.7216(5) 0.4316(3) 0.3796(2) 0.0376(10) Uiso 0.5 1 d D . P B 1
O43A O 0.6632(15) 0.5286(8) 0.4143(6) 0.074(3) Uiso 0.5 1 d D . P B 1
O44A O 0.5770(13) 0.3698(10) 0.3964(7) 0.078(3) Uiso 0.5 1 d D . P B 1
O45A O 0.7840(14) 0.4361(9) 0.3040(5) 0.065(3) Uiso 0.5 1 d D . P B 1
O46A O 0.8420(11) 0.3628(7) 0.4250(5) 0.048(2) Uiso 0.5 1 d D . P B 1
Cl2B Cl 0.7127(5) 0.4185(4) 0.3923(3) 0.0499(14) Uiso 0.5 1 d D . P C 2
O43B O 0.7456(12) 0.5298(6) 0.4008(5) 0.0491(19) Uiso 0.5 1 d D . P C 2
O44B O 0.5507(13) 0.4246(11) 0.3822(8) 0.093(4) Uiso 0.5 1 d D . P C 2
O45B O 0.8106(13) 0.4009(9) 0.3128(5) 0.060(3) Uiso 0.5 1 d D . P C 2
O46B O 0.7837(16) 0.3409(9) 0.4400(7) 0.086(4) Uiso 0.5 1 d D . P C 2
Cl7A Cl 0.1171(6) 1.1947(4) 0.9540(2) 0.0294(10) Uiso 0.34 1 d D . P D 1
O48A O 0.1298(19) 1.1280(17) 0.8934(10) 0.036(3) Uiso 0.34 1 d D . P D 1
O49A O -0.0455(16) 1.2193(14) 0.9940(9) 0.070(4) Uiso 0.34 1 d D . P D 1
O50A O 0.174(3) 1.2963(13) 0.9235(11) 0.092(7) Uiso 0.34 1 d D . P D 1
O51A O 0.2398(19) 1.1483(13) 1.0028(8) 0.035(4) Uiso 0.34 1 d D . P D 1
Cl7B Cl 0.1138(9) 1.1685(6) 0.9692(3) 0.0439(18) Uiso 0.33 1 d D . P E 2
O48B O 0.124(2) 1.1007(13) 0.9091(9) 0.062(6) Uiso 0.33 1 d D . P E 2
O49B O -0.0476(15) 1.1746(14) 1.0095(8) 0.056(3) Uiso 0.33 1 d D . P E 2
O50B O 0.125(2) 1.2848(10) 0.9356(9) 0.053(4) Uiso 0.33 1 d D . P E 2
O51B O 0.247(3) 1.142(3) 1.0098(17) 0.120(15) Uiso 0.33 1 d D . P E 2
Cl7C Cl 0.0819(7) 1.1727(5) 0.9600(4) 0.0378(15) Uiso 0.33 1 d D . P F 3
O48C O 0.138(3) 1.1516(16) 0.8834(8) 0.073(8) Uiso 0.33 1 d D . P F 3
O49C O -0.062(2) 1.1273(17) 0.9930(12) 0.104(7) Uiso 0.33 1 d D . P F 3
O50C O 0.051(3) 1.2885(11) 0.9620(12) 0.094(6) Uiso 0.33 1 d D . P F 3
O51C O 0.2109(18) 1.1283(13) 1.0079(8) 0.042(4) Uiso 0.33 1 d D . P F 3
C53A C 0.508(2) 0.7069(12) 0.2872(10) 0.080(4) Uiso 0.5 1 d D . P G 1
H53A H 0.417863 0.697550 0.261279 0.095 Uiso 0.5 1 calc R U P G 1
H53B H 0.506040 0.655512 0.331905 0.095 Uiso 0.5 1 calc R U P G 1
C52A C 0.665(3) 0.683(2) 0.2367(14) 0.117(8) Uiso 0.5 1 d D . P G 1
H52A H 0.677292 0.609748 0.222747 0.176 Uiso 0.5 1 calc R U P G 1
H52B H 0.667364 0.732192 0.191755 0.176 Uiso 0.5 1 calc R U P G 1
H52C H 0.755579 0.690135 0.262412 0.176 Uiso 0.5 1 calc R U P G 1
C54A C 0.480(2) 0.8159(10) 0.3111(8) 0.061(3) Uiso 0.5 1 d D . P G 1
N55A N 0.455(3) 0.8978(12) 0.3331(11) 0.072(5) Uiso 0.5 1 d D . P G 1
C52B C 0.551(3) 0.6513(15) 0.2475(12) 0.103(6) Uiso 0.5 1 d D . P H 2
H52D H 0.615932 0.589968 0.223686 0.155 Uiso 0.5 1 calc R U P H 2
H52E H 0.488131 0.626933 0.294847 0.155 Uiso 0.5 1 calc R U P H 2
H52F H 0.476473 0.688911 0.214524 0.155 Uiso 0.5 1 calc R U P H 2
C53B C 0.664(2) 0.7259(14) 0.2620(12) 0.089(5) Uiso 0.5 1 d D . P H 2
H53C H 0.740261 0.688464 0.295059 0.107 Uiso 0.5 1 calc R U P H 2
H53D H 0.728561 0.750662 0.214451 0.107 Uiso 0.5 1 calc R U P H 2
C54B C 0.562(2) 0.8185(11) 0.2982(9) 0.063(4) Uiso 0.5 1 d D . P H 2
N55B N 0.494(3) 0.8969(15) 0.3193(14) 0.096(8) Uiso 0.5 1 d D . P H 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.117(4) . ?
Fe1 N9 2.181(4) . ?
Fe1 N14 2.179(4) . ?
Fe1 N22 2.131(4) . ?
Fe1 N29 2.204(5) . ?
Fe1 N34 2.180(4) . ?
N2 C3 1.334(6) . ?
N2 C7 1.336(6) . ?
C3 C4 1.370(6) . ?
C3 N8 1.413(6) . ?
C4 H4 0.9400 . ?
C4 C5 1.407(7) . ?
C5 C6 1.405(7) . ?
C5 N18 1.391(6) . ?
C6 H6 0.9400 . ?
C6 C7 1.368(6) . ?
C7 N13 1.413(6) . ?
N8 N9 1.367(5) . ?
N8 C12 1.350(7) . ?
N9 C10 1.338(7) . ?
C10 H10 0.9400 . ?
C10 C11 1.391(8) . ?
C11 H11 0.9400 . ?
C11 C12 1.364(8) . ?
C12 H12 0.9400 . ?
N13 N14 1.357(6) . ?
N13 C17A 1.359(9) . ?
N13 C17B 1.359(10) . ?
N14 C15A 1.310(10) . ?
N14 C15B 1.336(10) . ?
C15A H15A 0.9400 . ?
C15A C16A 1.401(11) . ?
C16A H16A 0.9400 . ?
C16A C17A 1.372(10) . ?
C17A H17A 0.9400 . ?
C15B H15B 0.9400 . ?
C15B C16B 1.383(11) . ?
C16B H16B 0.9400 . ?
C16B C17B 1.367(11) . ?
C17B H17B 0.9400 . ?
N18 H18 0.8700 . ?
N18 C19 1.383(7) . ?
C19 O20 1.181(8) . ?
C19 C21 1.507(8) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
N22 C23 1.325(6) . ?
N22 C27 1.329(6) . ?
C23 C24 1.369(6) . ?
C23 N28 1.410(6) . ?
C24 H24 0.9400 . ?
C24 C25 1.384(7) . ?
C25 C26 1.400(8) . ?
C25 N38 1.398(6) . ?
C26 H26 0.9400 . ?
C26 C27 1.376(6) . ?
C27 N33 1.415(6) . ?
N28 N29 1.360(6) . ?
N28 C32 1.367(7) . ?
N29 C30 1.317(7) . ?
C30 H30 0.9400 . ?
C30 C31 1.398(9) . ?
C31 H31 0.9400 . ?
C31 C32 1.356(9) . ?
C32 H32 0.9400 . ?
N33 N34 1.366(5) . ?
N33 C37 1.343(7) . ?
N34 C35 1.329(7) . ?
C35 H35 0.9400 . ?
C35 C36 1.398(8) . ?
C36 H36 0.9400 . ?
C36 C37 1.362(8) . ?
C37 H37 0.9400 . ?
N38 H38 0.8700 . ?
N38 C39 1.366(8) . ?
C39 O40 1.209(9) . ?
C39 C41 1.512(8) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C41 H41C 0.9700 . ?
Cl2A O43A 1.419(10) . ?
Cl2A O44A 1.508(10) . ?
Cl2A O45A 1.374(10) . ?
Cl2A O46A 1.514(8) . ?
Cl2B O43B 1.506(8) . ?
Cl2B O44B 1.382(11) . ?
Cl2B O45B 1.547(10) . ?
Cl2B O46B 1.366(11) . ?
Cl7A O48A 1.437(11) . ?
Cl7A O49A 1.425(13) . ?
Cl7A O50A 1.457(15) . ?
Cl7A O51A 1.476(12) . ?
Cl7B O48B 1.441(13) . ?
Cl7B O49B 1.409(13) . ?
Cl7B O50B 1.540(14) . ?
Cl7B O51B 1.411(16) . ?
Cl7C O48C 1.423(14) . ?
Cl7C O49C 1.418(15) . ?
Cl7C O50C 1.451(14) . ?
Cl7C O51C 1.499(13) . ?
C53A H53A 0.9800 . ?
C53A H53B 0.9800 . ?
C53A C52A 1.472(19) . ?
C53A C54A 1.463(15) . ?
C52A H52A 0.9700 . ?
C52A H52B 0.9700 . ?
C52A H52C 0.9700 . ?
C54A N55A 1.128(15) . ?
C52B H52D 0.9700 . ?
C52B H52E 0.9700 . ?
C52B H52F 0.9700 . ?
C52B C53B 1.506(19) . ?
C53B H53C 0.9800 . ?
C53B H53D 0.9800 . ?
C53B C54B 1.480(16) . ?
C54B N55B 1.132(16) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N9 73.29(14) . . ?
N2 Fe1 N14 73.15(14) . . ?
N2 Fe1 N22 165.13(16) . . ?
N2 Fe1 N29 95.27(15) . . ?
N2 Fe1 N34 119.07(15) . . ?
N9 Fe1 N29 95.09(17) . . ?
N14 Fe1 N9 146.44(14) . . ?
N14 Fe1 N29 87.65(17) . . ?
N14 Fe1 N34 101.00(17) . . ?
N22 Fe1 N9 115.94(15) . . ?
N22 Fe1 N14 96.88(15) . . ?
N22 Fe1 N29 72.92(15) . . ?
N22 Fe1 N34 73.07(15) . . ?
N34 Fe1 N9 95.42(17) . . ?
N34 Fe1 N29 145.66(15) . . ?
C3 N2 Fe1 121.3(3) . . ?
C3 N2 C7 117.2(4) . . ?
C7 N2 Fe1 121.4(3) . . ?
N2 C3 C4 124.3(4) . . ?
N2 C3 N8 112.7(4) . . ?
C4 C3 N8 123.0(4) . . ?
C3 C4 H4 121.4 . . ?
C3 C4 C5 117.2(4) . . ?
C5 C4 H4 121.4 . . ?
C6 C5 C4 119.7(4) . . ?
N18 C5 C4 116.5(5) . . ?
N18 C5 C6 123.8(4) . . ?
C5 C6 H6 121.6 . . ?
C7 C6 C5 116.8(4) . . ?
C7 C6 H6 121.6 . . ?
N2 C7 C6 124.8(4) . . ?
N2 C7 N13 112.2(4) . . ?
C6 C7 N13 123.0(4) . . ?
N9 N8 C3 117.8(4) . . ?
C12 N8 C3 130.2(4) . . ?
C12 N8 N9 111.9(4) . . ?
N8 N9 Fe1 114.9(3) . . ?
C10 N9 Fe1 141.1(3) . . ?
C10 N9 N8 103.8(4) . . ?
N9 C10 H10 124.0 . . ?
N9 C10 C11 111.9(5) . . ?
C11 C10 H10 124.0 . . ?
C10 C11 H11 127.4 . . ?
C12 C11 C10 105.3(5) . . ?
C12 C11 H11 127.4 . . ?
N8 C12 C11 107.1(5) . . ?
N8 C12 H12 126.4 . . ?
C11 C12 H12 126.4 . . ?
N14 N13 C7 118.3(4) . . ?
N14 N13 C17A 107.2(5) . . ?
N14 N13 C17B 115.7(6) . . ?
C17A N13 C7 133.3(6) . . ?
C17B N13 C7 125.7(6) . . ?
N13 N14 Fe1 114.9(3) . . ?
C15A N14 Fe1 133.8(7) . . ?
C15A N14 N13 110.6(7) . . ?
C15B N14 Fe1 144.6(7) . . ?
C15B N14 N13 100.4(7) . . ?
N14 C15A H15A 126.3 . . ?
N14 C15A C16A 107.5(10) . . ?
C16A C15A H15A 126.3 . . ?
C15A C16A H16A 126.7 . . ?
C17A C16A C15A 106.6(10) . . ?
C17A C16A H16A 126.7 . . ?
N13 C17A C16A 108.0(9) . . ?
N13 C17A H17A 126.0 . . ?
C16A C17A H17A 126.0 . . ?
N14 C15B H15B 123.0 . . ?
N14 C15B C16B 114.0(12) . . ?
C16B C15B H15B 123.0 . . ?
C15B C16B H16B 127.1 . . ?
C17B C16B C15B 105.8(12) . . ?
C17B C16B H16B 127.1 . . ?
N13 C17B C16B 103.8(10) . . ?
N13 C17B H17B 128.1 . . ?
C16B C17B H17B 128.1 . . ?
C5 N18 H18 116.3 . . ?
C19 N18 C5 127.3(5) . . ?
C19 N18 H18 116.3 . . ?
N18 C19 C21 112.5(6) . . ?
O20 C19 N18 123.1(5) . . ?
O20 C19 C21 124.3(6) . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 N22 Fe1 121.1(3) . . ?
C23 N22 C27 117.5(4) . . ?
C27 N22 Fe1 121.3(3) . . ?
N22 C23 C24 123.6(5) . . ?
N22 C23 N28 113.1(4) . . ?
C24 C23 N28 123.3(5) . . ?
C23 C24 H24 121.1 . . ?
C23 C24 C25 117.9(5) . . ?
C25 C24 H24 121.1 . . ?
C24 C25 C26 120.4(4) . . ?
C24 C25 N38 117.5(5) . . ?
N38 C25 C26 122.1(5) . . ?
C25 C26 H26 122.2 . . ?
C27 C26 C25 115.7(5) . . ?
C27 C26 H26 122.2 . . ?
N22 C27 C26 125.0(5) . . ?
N22 C27 N33 112.3(4) . . ?
C26 C27 N33 122.7(5) . . ?
N29 N28 C23 118.3(4) . . ?
N29 N28 C32 111.1(4) . . ?
C32 N28 C23 130.6(4) . . ?
N28 N29 Fe1 114.2(3) . . ?
C30 N29 Fe1 139.5(4) . . ?
C30 N29 N28 105.4(4) . . ?
N29 C30 H30 124.5 . . ?
N29 C30 C31 111.0(5) . . ?
C31 C30 H30 124.5 . . ?
C30 C31 H31 126.9 . . ?
C32 C31 C30 106.2(6) . . ?
C32 C31 H31 126.9 . . ?
N28 C32 H32 126.8 . . ?
C31 C32 N28 106.3(5) . . ?
C31 C32 H32 126.8 . . ?
N34 N33 C27 118.1(4) . . ?
C37 N33 C27 130.4(4) . . ?
C37 N33 N34 111.5(4) . . ?
N33 N34 Fe1 114.8(3) . . ?
C35 N34 Fe1 140.1(4) . . ?
C35 N34 N33 104.6(4) . . ?
N34 C35 H35 124.4 . . ?
N34 C35 C36 111.2(5) . . ?
C36 C35 H35 124.4 . . ?
C35 C36 H36 127.4 . . ?
C37 C36 C35 105.2(5) . . ?
C37 C36 H36 127.4 . . ?
N33 C37 C36 107.4(5) . . ?
N33 C37 H37 126.3 . . ?
C36 C37 H37 126.3 . . ?
C25 N38 H38 116.9 . . ?
C39 N38 C25 126.2(5) . . ?
C39 N38 H38 116.9 . . ?
N38 C39 C41 114.3(7) . . ?
O40 C39 N38 122.8(5) . . ?
O40 C39 C41 122.8(6) . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O43A Cl2A O44A 104.3(7) . . ?
O43A Cl2A O46A 108.7(6) . . ?
O44A Cl2A O46A 101.5(6) . . ?
O45A Cl2A O43A 119.3(7) . . ?
O45A Cl2A O44A 110.6(7) . . ?
O45A Cl2A O46A 110.8(6) . . ?
O43B Cl2B O45B 100.3(6) . . ?
O44B Cl2B O43B 108.4(7) . . ?
O44B Cl2B O45B 103.4(7) . . ?
O46B Cl2B O43B 113.7(7) . . ?
O46B Cl2B O44B 122.3(9) . . ?
O46B Cl2B O45B 105.8(7) . . ?
O48A Cl7A O50A 108.9(12) . . ?
O48A Cl7A O51A 109.2(9) . . ?
O49A Cl7A O48A 114.4(9) . . ?
O49A Cl7A O50A 107.2(10) . . ?
O49A Cl7A O51A 113.9(9) . . ?
O50A Cl7A O51A 102.4(10) . . ?
O48B Cl7B O50B 109.3(10) . . ?
O49B Cl7B O48B 107.4(10) . . ?
O49B Cl7B O50B 103.2(9) . . ?
O49B Cl7B O51B 118.4(14) . . ?
O51B Cl7B O48B 112.9(14) . . ?
O51B Cl7B O50B 104.9(14) . . ?
O48C Cl7C O50C 107.1(11) . . ?
O48C Cl7C O51C 111.0(10) . . ?
O49C Cl7C O48C 113.8(12) . . ?
O49C Cl7C O50C 110.1(11) . . ?
O49C Cl7C O51C 106.2(11) . . ?
O50C Cl7C O51C 108.5(10) . . ?
H53A C53A H53B 107.8 . . ?
C52A C53A H53A 109.0 . . ?
C52A C53A H53B 109.0 . . ?
C54A C53A H53A 109.0 . . ?
C54A C53A H53B 109.0 . . ?
C54A C53A C52A 113.1(15) . . ?
C53A C52A H52A 109.5 . . ?
C53A C52A H52B 109.5 . . ?
C53A C52A H52C 109.5 . . ?
H52A C52A H52B 109.5 . . ?
H52A C52A H52C 109.5 . . ?
H52B C52A H52C 109.5 . . ?
N55A C54A C53A 176.4(19) . . ?
H52D C52B H52E 109.5 . . ?
H52D C52B H52F 109.5 . . ?
H52E C52B H52F 109.5 . . ?
C53B C52B H52D 109.5 . . ?
C53B C52B H52E 109.5 . . ?
C53B C52B H52F 109.5 . . ?
C52B C53B H53C 110.0 . . ?
C52B C53B H53D 110.0 . . ?
H53C C53B H53D 108.4 . . ?
C54B C53B C52B 108.3(15) . . ?
C54B C53B H53C 110.0 . . ?
C54B C53B H53D 110.0 . . ?
N55B C54B C53B 172(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N18 H18 O46A 0.87 2.07 2.930(10) 167.5 . yes
N18 H18 O46B 0.87 1.96 2.832(13) 174.8 . yes
N38 H38 O51A 0.87 2.09 2.881(18) 150.2 . yes
N38 H38 O51B 0.87 2.08 2.89(3) 154.2 . yes
N38 H38 O51C 0.87 2.39 3.172(18) 150.0 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N2 C3 C4 179.0(4) . . . . ?
Fe1 N2 C3 N8 -1.5(5) . . . . ?
Fe1 N2 C7 C6 179.4(4) . . . . ?
Fe1 N2 C7 N13 0.5(6) . . . . ?
Fe1 N9 C10 C11 -172.1(5) . . . . ?
Fe1 N14 C15A C16A 165.9(7) . . . . ?
Fe1 N14 C15B C16B -179.0(8) . . . . ?
Fe1 N22 C23 C24 -178.7(4) . . . . ?
Fe1 N22 C23 N28 0.4(6) . . . . ?
Fe1 N22 C27 C26 177.2(4) . . . . ?
Fe1 N22 C27 N33 -1.2(5) . . . . ?
Fe1 N29 C30 C31 167.2(5) . . . . ?
Fe1 N34 C35 C36 -171.8(4) . . . . ?
N2 C3 C4 C5 1.7(7) . . . . ?
N2 C3 N8 N9 2.0(6) . . . . ?
N2 C3 N8 C12 -172.9(5) . . . . ?
N2 C7 N13 N14 -1.4(6) . . . . ?
N2 C7 N13 C17A 164.5(9) . . . . ?
N2 C7 N13 C17B -174.1(9) . . . . ?
C3 N2 C7 C6 -0.5(7) . . . . ?
C3 N2 C7 N13 -179.4(4) . . . . ?
C3 C4 C5 C6 -0.7(7) . . . . ?
C3 C4 C5 N18 178.1(5) . . . . ?
C3 N8 N9 Fe1 -1.6(5) . . . . ?
C3 N8 N9 C10 -176.9(5) . . . . ?
C3 N8 C12 C11 175.8(5) . . . . ?
C4 C3 N8 N9 -178.4(5) . . . . ?
C4 C3 N8 C12 6.7(8) . . . . ?
C4 C5 C6 C7 -0.7(8) . . . . ?
C4 C5 N18 C19 177.5(6) . . . . ?
C5 C6 C7 N2 1.4(8) . . . . ?
C5 C6 C7 N13 -179.8(5) . . . . ?
C5 N18 C19 O20 -1.5(11) . . . . ?
C5 N18 C19 C21 176.8(6) . . . . ?
C6 C5 N18 C19 -3.7(9) . . . . ?
C6 C7 N13 N14 179.6(5) . . . . ?
C6 C7 N13 C17A -14.5(11) . . . . ?
C6 C7 N13 C17B 7.0(11) . . . . ?
C7 N2 C3 C4 -1.1(7) . . . . ?
C7 N2 C3 N8 178.4(4) . . . . ?
C7 N13 N14 Fe1 1.7(6) . . . . ?
C7 N13 N14 C15A 173.3(9) . . . . ?
C7 N13 N14 C15B 179.9(9) . . . . ?
C7 N13 C17A C16A -169.8(8) . . . . ?
C7 N13 C17B C16B 179.8(8) . . . . ?
N8 C3 C4 C5 -177.8(4) . . . . ?
N8 N9 C10 C11 1.1(7) . . . . ?
N9 N8 C12 C11 0.7(7) . . . . ?
N9 C10 C11 C12 -0.7(8) . . . . ?
C10 C11 C12 N8 0.0(8) . . . . ?
C12 N8 N9 Fe1 174.2(4) . . . . ?
C12 N8 N9 C10 -1.1(6) . . . . ?
N13 N14 C15A C16A -3.5(14) . . . . ?
N13 N14 C15B C16B 3.7(16) . . . . ?
N14 N13 C17A C16A -2.8(11) . . . . ?
N14 N13 C17B C16B 7.0(14) . . . . ?
N14 C15A C16A C17A 1.7(16) . . . . ?
N14 C15B C16B C17B 0(2) . . . . ?
C15A C16A C17A N13 0.7(15) . . . . ?
C17A N13 N14 Fe1 -167.6(6) . . . . ?
C17A N13 N14 C15A 4.0(11) . . . . ?
C15B C16B C17B N13 -4.0(16) . . . . ?
C17B N13 N14 Fe1 175.1(7) . . . . ?
C17B N13 N14 C15B -6.7(12) . . . . ?
N18 C5 C6 C7 -179.5(5) . . . . ?
N22 C23 C24 C25 1.3(8) . . . . ?
N22 C23 N28 N29 -5.0(6) . . . . ?
N22 C23 N28 C32 172.7(5) . . . . ?
N22 C27 N33 N34 5.3(6) . . . . ?
N22 C27 N33 C37 -176.4(5) . . . . ?
C23 N22 C27 C26 -2.0(7) . . . . ?
C23 N22 C27 N33 179.5(4) . . . . ?
C23 C24 C25 C26 -1.7(8) . . . . ?
C23 C24 C25 N38 178.2(5) . . . . ?
C23 N28 N29 Fe1 7.0(6) . . . . ?
C23 N28 N29 C30 178.2(5) . . . . ?
C23 N28 C32 C31 -177.5(6) . . . . ?
C24 C23 N28 N29 174.1(5) . . . . ?
C24 C23 N28 C32 -8.2(9) . . . . ?
C24 C25 C26 C27 0.5(8) . . . . ?
C24 C25 N38 C39 -156.5(6) . . . . ?
C25 C26 C27 N22 1.5(8) . . . . ?
C25 C26 C27 N33 179.8(5) . . . . ?
C25 N38 C39 O40 -0.8(11) . . . . ?
C25 N38 C39 C41 175.9(6) . . . . ?
C26 C25 N38 C39 23.4(9) . . . . ?
C26 C27 N33 N34 -173.2(5) . . . . ?
C26 C27 N33 C37 5.1(8) . . . . ?
C27 N22 C23 C24 0.5(7) . . . . ?
C27 N22 C23 N28 179.6(4) . . . . ?
C27 N33 N34 Fe1 -6.7(5) . . . . ?
C27 N33 N34 C35 179.4(4) . . . . ?
C27 N33 C37 C36 -179.1(5) . . . . ?
N28 C23 C24 C25 -177.8(5) . . . . ?
N28 N29 C30 C31 -0.4(7) . . . . ?
N29 N28 C32 C31 0.3(7) . . . . ?
N29 C30 C31 C32 0.6(8) . . . . ?
C30 C31 C32 N28 -0.5(8) . . . . ?
C32 N28 N29 Fe1 -171.1(4) . . . . ?
C32 N28 N29 C30 0.1(6) . . . . ?
N33 N34 C35 C36 -0.5(6) . . . . ?
N34 N33 C37 C36 -0.7(6) . . . . ?
N34 C35 C36 C37 0.0(7) . . . . ?
C35 C36 C37 N33 0.4(6) . . . . ?
C37 N33 N34 Fe1 174.6(3) . . . . ?
C37 N33 N34 C35 0.7(6) . . . . ?
N38 C25 C26 C27 -179.5(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.5807(15)
2 0.4193(15)

_twin_special_details            
;
Component 2 rotated by 179.8713° 
 around [0.00 0.71 0.71] (reciprocal) or [-0.35 0.85 0.39] (direct)
;
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: propionitrile/diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_etcncllt
_database_code_depnum_ccdc_archive 'CCDC 2078657'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2021-04-19 deposited with the CCDC.	2021-06-10 downloaded from the CCDC.
;
_audit_creation_date             2020-07-21
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis-[N-(2,6-di{pyrazol-1-yl}pyrid-4-yl)acetamide]iron(II)diperchlorate propionitrile solvate'
_chemical_formula_moiety         'C26 H24 Fe N12 O2, 2(Cl O4), C3 H5 N'
_chemical_formula_sum            'C29 H29 Cl2 Fe N13 O10'
_chemical_formula_weight         846.40
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.3410(3)
_cell_length_b                   12.3849(4)
_cell_length_c                   17.6860(5)
_cell_angle_alpha                82.187(3)
_cell_angle_beta                 78.664(3)
_cell_angle_gamma                85.140(3)
_cell_volume                     1771.57(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8032
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.59
_cell_measurement_theta_min      4.13
_exptl_absorpt_coefficient_mu    5.464
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.946
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6668
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.586
_diffrn_reflns_theta_min         3.609
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6198
_reflns_number_total             6668
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 1990)'
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         6668
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0579
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0943P)²+4.5289P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1856
_refine_ls_wR_factor_ref         0.1883
_refine_special_details          
;The data were resolved into two non-superimposable twin domains, in a 
 ratio of 0.80:0.20.

 No disorder is present in the model and no restraints were applied
 to the refinement. All non-H atoms were refined anisotropically and H
 atoms were placed in calculated positions and refined using a riding
 model.,Twin
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.802(4)
 0.198(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17),
 N18(H18), C24(H24), C26(H26), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36),
  C37(H37), N38(H38)
3.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C41(H41A,H41B,H41C), C52(H52A,H52B,H52C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.76616(7) 0.76876(5) 0.73046(4) 0.01815(18) Uani 1 1 d . . . . .
N2 N 0.8166(4) 0.6354(3) 0.6858(2) 0.0194(7) Uani 1 1 d . . . . .
C3 C 0.7932(5) 0.6288(3) 0.6142(2) 0.0204(8) Uani 1 1 d . . . . .
C4 C 0.8145(5) 0.5332(3) 0.5811(3) 0.0229(8) Uani 1 1 d . . . . .
H4 H 0.800060 0.531602 0.529334 0.028 Uiso 1 1 calc R U . . .
C5 C 0.8588(5) 0.4378(3) 0.6273(3) 0.0220(8) Uani 1 1 d . . . . .
C6 C 0.8801(5) 0.4418(4) 0.7041(3) 0.0236(9) Uani 1 1 d . . . . .
H6 H 0.908699 0.378314 0.736408 0.028 Uiso 1 1 calc R U . . .
C7 C 0.8570(5) 0.5435(3) 0.7293(2) 0.0207(8) Uani 1 1 d . . . . .
N8 N 0.7400(4) 0.7310(3) 0.5799(2) 0.0209(7) Uani 1 1 d . . . . .
N9 N 0.7191(4) 0.8166(3) 0.6244(2) 0.0208(7) Uani 1 1 d . . . . .
C10 C 0.6623(5) 0.9010(4) 0.5807(3) 0.0255(9) Uani 1 1 d . . . . .
H10 H 0.636670 0.972032 0.595999 0.031 Uiso 1 1 calc R U . . .
C11 C 0.6449(6) 0.8718(4) 0.5089(3) 0.0292(10) Uani 1 1 d . . . . .
H11 H 0.607566 0.917933 0.467668 0.035 Uiso 1 1 calc R U . . .
C12 C 0.6928(6) 0.7632(4) 0.5105(3) 0.0262(9) Uani 1 1 d . . . . .
H12 H 0.693034 0.718736 0.470734 0.031 Uiso 1 1 calc R U . . .
N13 N 0.8677(4) 0.5662(3) 0.8038(2) 0.0215(7) Uani 1 1 d . . . . .
N14 N 0.8293(4) 0.6729(3) 0.8188(2) 0.0211(7) Uani 1 1 d . . . . .
C15 C 0.8386(5) 0.6734(4) 0.8925(3) 0.0265(9) Uani 1 1 d . . . . .
H15 H 0.820144 0.736357 0.918968 0.032 Uiso 1 1 calc R U . . .
C16 C 0.8796(6) 0.5679(4) 0.9261(3) 0.0281(9) Uani 1 1 d . . . . .
H16 H 0.891900 0.546872 0.978423 0.034 Uiso 1 1 calc R U . . .
C17 C 0.8985(6) 0.5015(4) 0.8690(3) 0.0271(9) Uani 1 1 d . . . . .
H17 H 0.927342 0.425344 0.873707 0.032 Uiso 1 1 calc R U . . .
N18 N 0.8728(5) 0.3419(3) 0.5933(2) 0.0252(8) Uani 1 1 d . . . . .
H18 H 0.844774 0.347628 0.547385 0.030 Uiso 1 1 calc R U . . .
C19 C 0.9250(6) 0.2389(4) 0.6224(3) 0.0289(10) Uani 1 1 d . . . . .
O20 O 0.9794(5) 0.2201(3) 0.6822(2) 0.0393(8) Uani 1 1 d . . . . .
C21 C 0.9090(6) 0.1516(4) 0.5737(3) 0.0347(11) Uani 1 1 d . . . . .
H21A H 0.982316 0.088130 0.585723 0.052 Uiso 1 1 calc R U . . .
H21B H 0.938581 0.179610 0.518586 0.052 Uiso 1 1 calc R U . . .
H21C H 0.795622 0.129865 0.585094 0.052 Uiso 1 1 calc R U . . .
N22 N 0.7049(4) 0.8937(3) 0.7840(2) 0.0199(7) Uani 1 1 d . . . . .
C23 C 0.5530(5) 0.9048(4) 0.8271(2) 0.0228(8) Uani 1 1 d . . . . .
C24 C 0.5046(5) 0.9883(4) 0.8717(3) 0.0236(8) Uani 1 1 d . . . . .
H24 H 0.397030 0.994151 0.901557 0.028 Uiso 1 1 calc R U . . .
C25 C 0.6198(5) 1.0650(4) 0.8716(2) 0.0241(9) Uani 1 1 d . . . . .
C26 C 0.7796(5) 1.0533(3) 0.8290(2) 0.0236(9) Uani 1 1 d . . . . .
H26 H 0.860299 1.103003 0.829071 0.028 Uiso 1 1 calc R U . . .
C27 C 0.8129(5) 0.9653(3) 0.7870(2) 0.0217(8) Uani 1 1 d . . . . .
N28 N 0.4584(4) 0.8196(3) 0.8199(2) 0.0233(7) Uani 1 1 d . . . . .
N29 N 0.5339(4) 0.7425(3) 0.7735(2) 0.0218(7) Uani 1 1 d . . . . .
C30 C 0.4236(5) 0.6707(4) 0.7774(3) 0.0255(9) Uani 1 1 d . . . . .
H30 H 0.441213 0.607607 0.750984 0.031 Uiso 1 1 calc R U . . .
C31 C 0.2768(6) 0.7001(4) 0.8258(3) 0.0304(10) Uani 1 1 d . . . . .
H31 H 0.179196 0.661882 0.837678 0.036 Uiso 1 1 calc R U . . .
C32 C 0.3015(6) 0.7945(4) 0.8524(3) 0.0285(9) Uani 1 1 d . . . . .
H32 H 0.224804 0.834755 0.886789 0.034 Uiso 1 1 calc R U . . .
N33 N 0.9659(4) 0.9362(3) 0.7431(2) 0.0221(7) Uani 1 1 d . . . . .
N34 N 0.9761(4) 0.8429(3) 0.7064(2) 0.0221(7) Uani 1 1 d . . . . .
C35 C 1.1284(5) 0.8356(4) 0.6673(3) 0.0248(9) Uani 1 1 d . . . . .
H35 H 1.171699 0.779696 0.635866 0.030 Uiso 1 1 calc R U . . .
C36 C 1.2171(5) 0.9213(4) 0.6785(3) 0.0273(9) Uani 1 1 d . . . . .
H36 H 1.328593 0.933624 0.656905 0.033 Uiso 1 1 calc R U . . .
C37 C 1.1120(5) 0.9834(4) 0.7262(3) 0.0260(9) Uani 1 1 d . . . . .
H37 H 1.136128 1.047813 0.744470 0.031 Uiso 1 1 calc R U . . .
N38 N 0.5681(5) 1.1493(3) 0.9166(2) 0.0272(8) Uani 1 1 d . . . . .
H38 H 0.477941 1.140111 0.951662 0.033 Uiso 1 1 calc R U . . .
C39 C 0.6425(6) 1.2460(4) 0.9126(3) 0.0277(9) Uani 1 1 d . . . . .
O40 O 0.7672(4) 1.2687(3) 0.8669(2) 0.0325(7) Uani 1 1 d . . . . .
C41 C 0.5488(8) 1.3220(4) 0.9680(3) 0.0412(12) Uani 1 1 d . . . . .
H41A H 0.607216 1.388908 0.962406 0.062 Uiso 1 1 calc R U . . .
H41B H 0.539308 1.286106 1.021471 0.062 Uiso 1 1 calc R U . . .
H41C H 0.439167 1.340398 0.956067 0.062 Uiso 1 1 calc R U . . .
Cl42 Cl 0.71281(13) 0.44585(9) 0.38922(6) 0.0270(2) Uani 1 1 d . . . . .
O43 O 0.7150(6) 0.5527(3) 0.4107(2) 0.0528(11) Uani 1 1 d . . . . .
O44 O 0.5515(5) 0.4131(5) 0.4004(2) 0.0596(13) Uani 1 1 d . . . . .
O45 O 0.7875(4) 0.4440(3) 0.3094(2) 0.0384(8) Uani 1 1 d . . . . .
O46 O 0.8071(6) 0.3723(3) 0.4368(2) 0.0491(11) Uani 1 1 d . . . . .
Cl47 Cl 0.10533(13) 1.16269(9) 0.95461(6) 0.0287(3) Uani 1 1 d . . . . .
O48 O 0.1288(4) 1.1056(3) 0.88772(19) 0.0342(8) Uani 1 1 d . . . . .
O49 O -0.0524(5) 1.1468(4) 1.0003(2) 0.0543(11) Uani 1 1 d . . . . .
O50 O 0.1272(6) 1.2768(3) 0.9305(2) 0.0470(10) Uani 1 1 d . . . . .
O51 O 0.2292(4) 1.1206(3) 1.00053(19) 0.0329(7) Uani 1 1 d . . . . .
C52 C 0.5379(9) 0.6469(5) 0.2481(4) 0.0535(16) Uani 1 1 d . . . . .
H52A H 0.495770 0.605302 0.298284 0.080 Uiso 1 1 calc R U . . .
H52B H 0.592706 0.596640 0.211544 0.080 Uiso 1 1 calc R U . . .
H52C H 0.446902 0.688101 0.227609 0.080 Uiso 1 1 calc R U . . .
C53 C 0.6589(7) 0.7253(4) 0.2588(3) 0.0393(12) Uani 1 1 d . . . . .
H53A H 0.742110 0.684991 0.286563 0.047 Uiso 1 1 calc R U . . .
H53B H 0.716006 0.757684 0.207291 0.047 Uiso 1 1 calc R U . . .
C54 C 0.5763(7) 0.8121(5) 0.3029(3) 0.0389(12) Uani 1 1 d . . . . .
N55 N 0.5112(7) 0.8804(5) 0.3357(3) 0.0535(13) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.906(4) . ?
Fe1 N9 1.992(3) . ?
Fe1 N14 1.960(4) . ?
Fe1 N22 1.904(4) . ?
Fe1 N29 1.974(4) . ?
Fe1 N34 1.991(4) . ?
N2 C3 1.334(5) . ?
N2 C7 1.342(5) . ?
C3 C4 1.373(6) . ?
C3 N8 1.403(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.408(6) . ?
C5 C6 1.412(6) . ?
C5 N18 1.389(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.377(6) . ?
C7 N13 1.406(5) . ?
N8 N9 1.385(5) . ?
N8 C12 1.360(5) . ?
N9 C10 1.324(6) . ?
C10 H10 0.9500 . ?
C10 C11 1.404(7) . ?
C11 H11 0.9500 . ?
C11 C12 1.368(7) . ?
C12 H12 0.9500 . ?
N13 N14 1.381(5) . ?
N13 C17 1.367(5) . ?
N14 C15 1.322(6) . ?
C15 H15 0.9500 . ?
C15 C16 1.403(7) . ?
C16 H16 0.9500 . ?
C16 C17 1.364(7) . ?
C17 H17 0.9500 . ?
N18 H18 0.8800 . ?
N18 C19 1.377(6) . ?
C19 O20 1.219(6) . ?
C19 C21 1.501(6) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
N22 C23 1.351(6) . ?
N22 C27 1.330(5) . ?
C23 C24 1.371(6) . ?
C23 N28 1.402(6) . ?
C24 H24 0.9500 . ?
C24 C25 1.407(6) . ?
C25 C26 1.403(6) . ?
C25 N38 1.387(6) . ?
C26 H26 0.9500 . ?
C26 C27 1.380(6) . ?
C27 N33 1.404(6) . ?
N28 N29 1.376(5) . ?
N28 C32 1.366(6) . ?
N29 C30 1.319(6) . ?
C30 H30 0.9500 . ?
C30 C31 1.400(7) . ?
C31 H31 0.9500 . ?
C31 C32 1.364(7) . ?
C32 H32 0.9500 . ?
N33 N34 1.389(5) . ?
N33 C37 1.359(6) . ?
N34 C35 1.323(6) . ?
C35 H35 0.9500 . ?
C35 C36 1.401(6) . ?
C36 H36 0.9500 . ?
C36 C37 1.358(7) . ?
C37 H37 0.9500 . ?
N38 H38 0.8800 . ?
N38 C39 1.382(6) . ?
C39 O40 1.214(6) . ?
C39 C41 1.511(7) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
Cl42 O43 1.427(4) . ?
Cl42 O44 1.408(4) . ?
Cl42 O45 1.430(4) . ?
Cl42 O46 1.444(4) . ?
Cl47 O48 1.432(3) . ?
Cl47 O49 1.416(4) . ?
Cl47 O50 1.436(4) . ?
Cl47 O51 1.457(3) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C52 C53 1.512(8) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53 C54 1.459(8) . ?
C54 N55 1.131(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N9 79.76(15) . . ?
N2 Fe1 N14 79.85(15) . . ?
N2 Fe1 N29 95.96(15) . . ?
N2 Fe1 N34 104.73(15) . . ?
N14 Fe1 N9 159.60(15) . . ?
N14 Fe1 N29 89.60(14) . . ?
N14 Fe1 N34 93.10(14) . . ?
N22 Fe1 N2 174.36(14) . . ?
N22 Fe1 N9 104.28(15) . . ?
N22 Fe1 N14 96.04(15) . . ?
N22 Fe1 N29 80.08(15) . . ?
N22 Fe1 N34 79.22(15) . . ?
N29 Fe1 N9 92.13(14) . . ?
N29 Fe1 N34 159.29(15) . . ?
N34 Fe1 N9 92.42(14) . . ?
C3 N2 Fe1 120.7(3) . . ?
C3 N2 C7 118.5(4) . . ?
C7 N2 Fe1 120.3(3) . . ?
N2 C3 C4 123.5(4) . . ?
N2 C3 N8 110.5(4) . . ?
C4 C3 N8 126.0(4) . . ?
C3 C4 H4 121.4 . . ?
C3 C4 C5 117.1(4) . . ?
C5 C4 H4 121.4 . . ?
C4 C5 C6 120.6(4) . . ?
N18 C5 C4 115.7(4) . . ?
N18 C5 C6 123.6(4) . . ?
C5 C6 H6 122.0 . . ?
C7 C6 C5 116.0(4) . . ?
C7 C6 H6 122.0 . . ?
N2 C7 C6 124.2(4) . . ?
N2 C7 N13 110.1(4) . . ?
C6 C7 N13 125.7(4) . . ?
N9 N8 C3 117.0(3) . . ?
C12 N8 C3 132.0(4) . . ?
C12 N8 N9 110.8(3) . . ?
N8 N9 Fe1 111.9(2) . . ?
C10 N9 Fe1 142.8(3) . . ?
C10 N9 N8 105.1(3) . . ?
N9 C10 H10 124.4 . . ?
N9 C10 C11 111.2(4) . . ?
C11 C10 H10 124.4 . . ?
C10 C11 H11 127.0 . . ?
C12 C11 C10 106.0(4) . . ?
C12 C11 H11 127.0 . . ?
N8 C12 C11 107.0(4) . . ?
N8 C12 H12 126.5 . . ?
C11 C12 H12 126.5 . . ?
N14 N13 C7 116.4(3) . . ?
C17 N13 C7 132.8(4) . . ?
C17 N13 N14 110.6(4) . . ?
N13 N14 Fe1 113.2(3) . . ?
C15 N14 Fe1 140.9(3) . . ?
C15 N14 N13 105.7(3) . . ?
N14 C15 H15 124.7 . . ?
N14 C15 C16 110.5(4) . . ?
C16 C15 H15 124.7 . . ?
C15 C16 H16 126.6 . . ?
C17 C16 C15 106.7(4) . . ?
C17 C16 H16 126.6 . . ?
N13 C17 H17 126.8 . . ?
C16 C17 N13 106.4(4) . . ?
C16 C17 H17 126.8 . . ?
C5 N18 H18 115.9 . . ?
C19 N18 C5 128.1(4) . . ?
C19 N18 H18 115.9 . . ?
N18 C19 C21 114.0(4) . . ?
O20 C19 N18 123.2(4) . . ?
O20 C19 C21 122.8(4) . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 N22 Fe1 119.7(3) . . ?
C27 N22 Fe1 121.7(3) . . ?
C27 N22 C23 118.2(4) . . ?
N22 C23 C24 122.8(4) . . ?
N22 C23 N28 110.5(4) . . ?
C24 C23 N28 126.7(4) . . ?
C23 C24 H24 121.2 . . ?
C23 C24 C25 117.7(4) . . ?
C25 C24 H24 121.2 . . ?
C26 C25 C24 120.4(4) . . ?
N38 C25 C24 116.8(4) . . ?
N38 C25 C26 122.8(4) . . ?
C25 C26 H26 122.0 . . ?
C27 C26 C25 116.1(4) . . ?
C27 C26 H26 122.0 . . ?
N22 C27 C26 124.7(4) . . ?
N22 C27 N33 109.9(4) . . ?
C26 C27 N33 125.3(4) . . ?
N29 N28 C23 116.8(3) . . ?
C32 N28 C23 132.4(4) . . ?
C32 N28 N29 110.8(4) . . ?
N28 N29 Fe1 112.7(3) . . ?
C30 N29 Fe1 141.5(3) . . ?
C30 N29 N28 105.6(4) . . ?
N29 C30 H30 124.6 . . ?
N29 C30 C31 110.7(4) . . ?
C31 C30 H30 124.6 . . ?
C30 C31 H31 126.7 . . ?
C32 C31 C30 106.5(4) . . ?
C32 C31 H31 126.7 . . ?
N28 C32 H32 126.8 . . ?
C31 C32 N28 106.3(4) . . ?
C31 C32 H32 126.8 . . ?
N34 N33 C27 116.8(3) . . ?
C37 N33 C27 132.7(4) . . ?
C37 N33 N34 110.4(4) . . ?
N33 N34 Fe1 112.2(3) . . ?
C35 N34 Fe1 142.7(3) . . ?
C35 N34 N33 105.1(3) . . ?
N34 C35 H35 124.5 . . ?
N34 C35 C36 111.0(4) . . ?
C36 C35 H35 124.5 . . ?
C35 C36 H36 126.8 . . ?
C37 C36 C35 106.4(4) . . ?
C37 C36 H36 126.8 . . ?
N33 C37 H37 126.4 . . ?
C36 C37 N33 107.1(4) . . ?
C36 C37 H37 126.4 . . ?
C25 N38 H38 116.4 . . ?
C39 N38 C25 127.2(4) . . ?
C39 N38 H38 116.4 . . ?
N38 C39 C41 113.3(4) . . ?
O40 C39 N38 123.0(4) . . ?
O40 C39 C41 123.7(4) . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O43 Cl42 O45 110.0(2) . . ?
O43 Cl42 O46 107.5(2) . . ?
O44 Cl42 O43 111.1(3) . . ?
O44 Cl42 O45 108.9(2) . . ?
O44 Cl42 O46 110.4(3) . . ?
O45 Cl42 O46 108.9(2) . . ?
O48 Cl47 O50 109.7(2) . . ?
O48 Cl47 O51 108.5(2) . . ?
O49 Cl47 O48 110.4(3) . . ?
O49 Cl47 O50 110.7(3) . . ?
O49 Cl47 O51 109.4(2) . . ?
O50 Cl47 O51 108.1(2) . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C53 C52 H52A 109.5 . . ?
C53 C52 H52B 109.5 . . ?
C53 C52 H52C 109.5 . . ?
C52 C53 H53A 109.4 . . ?
C52 C53 H53B 109.4 . . ?
H53A C53 H53B 108.0 . . ?
C54 C53 C52 111.0(5) . . ?
C54 C53 H53A 109.4 . . ?
C54 C53 H53B 109.4 . . ?
N55 C54 C53 178.6(6) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N18 H18 O46 0.88 2.02 2.895(5) 172.4 . yes
N38 H38 O51 0.88 2.11 2.949(5) 160.3 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N2 C3 C4 -174.6(3) . . . . ?
Fe1 N2 C3 N8 3.6(5) . . . . ?
Fe1 N2 C7 C6 173.6(3) . . . . ?
Fe1 N2 C7 N13 -4.9(4) . . . . ?
Fe1 N9 C10 C11 -172.9(4) . . . . ?
Fe1 N14 C15 C16 173.2(4) . . . . ?
Fe1 N22 C23 C24 175.0(3) . . . . ?
Fe1 N22 C23 N28 -4.1(5) . . . . ?
Fe1 N22 C27 C26 -175.4(3) . . . . ?
Fe1 N22 C27 N33 3.0(5) . . . . ?
Fe1 N29 C30 C31 174.5(4) . . . . ?
Fe1 N34 C35 C36 -178.7(4) . . . . ?
N2 C3 C4 C5 1.9(6) . . . . ?
N2 C3 N8 N9 -1.0(5) . . . . ?
N2 C3 N8 C12 -176.0(4) . . . . ?
N2 C7 N13 N14 2.6(5) . . . . ?
N2 C7 N13 C17 177.3(4) . . . . ?
C3 N2 C7 C6 1.6(6) . . . . ?
C3 N2 C7 N13 -176.8(3) . . . . ?
C3 C4 C5 C6 -0.2(6) . . . . ?
C3 C4 C5 N18 177.5(4) . . . . ?
C3 N8 N9 Fe1 -1.7(4) . . . . ?
C3 N8 N9 C10 -177.3(4) . . . . ?
C3 N8 C12 C11 176.9(4) . . . . ?
C4 C3 N8 N9 177.1(4) . . . . ?
C4 C3 N8 C12 2.1(7) . . . . ?
C4 C5 C6 C7 -0.7(6) . . . . ?
C4 C5 N18 C19 174.9(4) . . . . ?
C5 C6 C7 N2 0.0(6) . . . . ?
C5 C6 C7 N13 178.3(4) . . . . ?
C5 N18 C19 O20 -5.8(8) . . . . ?
C5 N18 C19 C21 174.2(4) . . . . ?
C6 C5 N18 C19 -7.5(7) . . . . ?
C6 C7 N13 N14 -175.8(4) . . . . ?
C6 C7 N13 C17 -1.1(7) . . . . ?
C7 N2 C3 C4 -2.6(6) . . . . ?
C7 N2 C3 N8 175.5(3) . . . . ?
C7 N13 N14 Fe1 0.5(4) . . . . ?
C7 N13 N14 C15 176.5(4) . . . . ?
C7 N13 C17 C16 -175.0(4) . . . . ?
N8 C3 C4 C5 -176.0(4) . . . . ?
N8 N9 C10 C11 0.4(5) . . . . ?
N9 N8 C12 C11 1.7(5) . . . . ?
N9 C10 C11 C12 0.6(5) . . . . ?
C10 C11 C12 N8 -1.4(5) . . . . ?
C12 N8 N9 Fe1 174.4(3) . . . . ?
C12 N8 N9 C10 -1.3(5) . . . . ?
N13 N14 C15 C16 -1.1(5) . . . . ?
N14 N13 C17 C16 -0.1(5) . . . . ?
N14 C15 C16 C17 1.1(5) . . . . ?
C15 C16 C17 N13 -0.6(5) . . . . ?
C17 N13 N14 Fe1 -175.4(3) . . . . ?
C17 N13 N14 C15 0.7(5) . . . . ?
N18 C5 C6 C7 -178.2(4) . . . . ?
N22 C23 C24 C25 0.1(6) . . . . ?
N22 C23 N28 N29 1.0(5) . . . . ?
N22 C23 N28 C32 178.8(4) . . . . ?
N22 C27 N33 N34 0.0(5) . . . . ?
N22 C27 N33 C37 177.9(4) . . . . ?
C23 N22 C27 C26 -2.6(6) . . . . ?
C23 N22 C27 N33 175.8(3) . . . . ?
C23 C24 C25 C26 -2.0(6) . . . . ?
C23 C24 C25 N38 179.6(4) . . . . ?
C23 N28 N29 Fe1 2.2(4) . . . . ?
C23 N28 N29 C30 178.5(4) . . . . ?
C23 N28 C32 C31 -178.3(4) . . . . ?
C24 C23 N28 N29 -178.1(4) . . . . ?
C24 C23 N28 C32 -0.3(7) . . . . ?
C24 C25 C26 C27 1.6(6) . . . . ?
C24 C25 N38 C39 -164.0(4) . . . . ?
C25 C26 C27 N22 0.8(6) . . . . ?
C25 C26 C27 N33 -177.4(4) . . . . ?
C25 N38 C39 O40 0.1(7) . . . . ?
C25 N38 C39 C41 177.4(4) . . . . ?
C26 C25 N38 C39 17.6(7) . . . . ?
C26 C27 N33 N34 178.4(4) . . . . ?
C26 C27 N33 C37 -3.7(7) . . . . ?
C27 N22 C23 C24 2.1(6) . . . . ?
C27 N22 C23 N28 -177.0(3) . . . . ?
C27 N33 N34 Fe1 -2.6(4) . . . . ?
C27 N33 N34 C35 177.9(3) . . . . ?
C27 N33 C37 C36 -177.8(4) . . . . ?
N28 C23 C24 C25 179.1(4) . . . . ?
N28 N29 C30 C31 0.1(5) . . . . ?
N29 N28 C32 C31 -0.4(5) . . . . ?
N29 C30 C31 C32 -0.3(5) . . . . ?
C30 C31 C32 N28 0.4(5) . . . . ?
C32 N28 N29 Fe1 -176.1(3) . . . . ?
C32 N28 N29 C30 0.2(4) . . . . ?
N33 N34 C35 C36 0.6(5) . . . . ?
N34 N33 C37 C36 0.2(5) . . . . ?
N34 C35 C36 C37 -0.4(5) . . . . ?
C35 C36 C37 N33 0.1(5) . . . . ?
C37 N33 N34 Fe1 179.0(3) . . . . ?
C37 N33 N34 C35 -0.5(4) . . . . ?
N38 C25 C26 C27 179.9(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.802(4)
2 0.198(4)

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile/diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_etcnmalt
_database_code_depnum_ccdc_archive 'CCDC 2078660'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2021-04-19 deposited with the CCDC.	2021-06-10 downloaded from the CCDC.
;
_audit_creation_date             2020-07-21
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis-[N-(2,6-di{pyrazol-1-yl}pyrid-4-yl)acetamide]iron(II)tetrafluoroborate(2/0.9) perchlorate(2/1.1) propionitrile solvate'
_chemical_formula_moiety         
'C26 H24 Fe N12 O2, 0.9(B F4), 1.1(Cl O4), C3 H5 N'
_chemical_formula_sum            'C29 H29 B0.90 Cl1.10 F3.60 Fe N13 O6.40'
_chemical_formula_weight         835.02
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.3123(5)
_cell_length_b                   12.3617(5)
_cell_length_c                   17.5779(6)
_cell_angle_alpha                82.678(3)
_cell_angle_beta                 78.686(4)
_cell_angle_gamma                85.091(4)
_cell_volume                     1753.24(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5626
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      73.39
_cell_measurement_theta_min      4.15
_exptl_absorpt_coefficient_mu    4.964
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.443
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             854
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.05
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_Laue_measured_fraction_full 0.944
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13546
_diffrn_reflns_point_group_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.588
_diffrn_reflns_theta_min         3.612
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      125(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5375
_reflns_number_total             6565
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2015)'
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         6565
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0495
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0598P)²+0.8511P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1245
_refine_special_details          
;
 Separate partial BF₄⁻ and ClO₄⁻ ions were modelled on each anion 
 site. The BF₄⁻:ClO₄⁻ occupancy ratio for one anion refined to 
 0.48:0.52, while the other anion refined to 0.41:0.59; the former was 
 actually refined as 0.49:0.51, for consistency with the higher temperature
 refinements from the same crystal. The bond distance restraints that
 were applied to the disordered anions are listed below. SIMU displacement
 ellipsoid restraints were also used for the partial BF₄⁻ ions, to 
 keep the B atom thermal parameters at reasonable values.

 All crystallographically ordered non-H atoms were refined anisotropically, 
 and H atoms were placed in calculated positions and refined using a riding 
 model. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B42-F43 = B42-F44 = B42-F45 = B42-F46
 1.37 with sigma of 0.02
 B47-F48 = B47-F49 = B47-F50 = B47-F51
 1.37 with sigma of 0.02
 F43-F44 = F43-F45 = F43-F46 = F44-F45 = F44-F46 = F45-F46
 2.24 with sigma of 0.02
 F48-F49 = F48-F50 = F48-F51 = F49-F50 = F49-F51 = F50-F51
 2.24 with sigma of 0.02
 Cl42-O43 = Cl42-O44 = Cl42-O45 = Cl42-O46
 1.45 with sigma of 0.02
 Cl47-O48 = Cl47-O49 = Cl47-O50 = Cl47-O51
 1.45 with sigma of 0.02
 O43-O44 = O43-O45 = O43-O46 = O44-O45 = O44-O46 = O45-O46
 2.37 with sigma of 0.02
 O48-O49 = O48-O50 = O48-O51 = O49-O50 = O49-O51 = O50-O51
 2.37 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
B42 \\sim F43 \\sim F44 \\sim F45 \\sim F46: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
B47 \\sim F48 \\sim F49 \\sim F50 \\sim F51: within 2A with sigma of 0.002 and
sigma for terminal atoms of 0.004 within 2A
4. Others
 Fixed Sof: B42(0.49) F43(0.49) F44(0.49) F45(0.49) F46(0.49) Cl42(0.51)
 O43(0.51) O44(0.51) O45(0.51) O46(0.51) B47(0.41) F48(0.41) F49(0.41)
 F50(0.41) F51(0.41) Cl47(0.59) O48(0.59) O49(0.59) O50(0.59) O51(0.59)
5.a Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B)
5.b Me refined with riding coordinates:
 C52(H52A,H52B,H52C)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17),
 N18(H18), C24(H24), C26(H26), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36),
  C37(H37), N38(H38)
5.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C41(H41A,H41B,H41C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.76671(5) 0.76940(4) 0.73000(2) 0.01715(12) Uani 1 1 d . . . . .
N2 N 0.8175(3) 0.63545(19) 0.68535(13) 0.0177(5) Uani 1 1 d . . . . .
C3 C 0.7935(3) 0.6279(2) 0.61352(16) 0.0197(6) Uani 1 1 d . . . . .
C4 C 0.8145(4) 0.5316(2) 0.58021(16) 0.0209(6) Uani 1 1 d . . . . .
H4 H 0.799177 0.529205 0.528300 0.025 Uiso 1 1 calc R U . . .
C5 C 0.8596(4) 0.4369(2) 0.62643(17) 0.0212(6) Uani 1 1 d . . . . .
C6 C 0.8815(4) 0.4420(2) 0.70301(17) 0.0209(6) Uani 1 1 d . . . . .
H6 H 0.910369 0.378664 0.735378 0.025 Uiso 1 1 calc R U . . .
C7 C 0.8587(3) 0.5444(2) 0.72877(16) 0.0193(6) Uani 1 1 d . . . . .
N8 N 0.7391(3) 0.72945(19) 0.57872(14) 0.0206(5) Uani 1 1 d . . . . .
N9 N 0.7186(3) 0.8157(2) 0.62349(14) 0.0215(5) Uani 1 1 d . . . . .
C10 C 0.6616(4) 0.9000(2) 0.57982(17) 0.0232(6) Uani 1 1 d . . . . .
H10 H 0.636447 0.971341 0.595182 0.028 Uiso 1 1 calc R U . . .
C11 C 0.6434(4) 0.8697(3) 0.50773(18) 0.0277(7) Uani 1 1 d . . . . .
H11 H 0.604782 0.915228 0.466434 0.033 Uiso 1 1 calc R U . . .
C12 C 0.6927(4) 0.7610(3) 0.50938(17) 0.0245(6) Uani 1 1 d . . . . .
H12 H 0.694127 0.716127 0.469193 0.029 Uiso 1 1 calc R U . . .
N13 N 0.8691(3) 0.5677(2) 0.80376(14) 0.0204(5) Uani 1 1 d . . . . .
N14 N 0.8309(3) 0.67421(19) 0.81847(14) 0.0198(5) Uani 1 1 d . . . . .
C15 C 0.8389(4) 0.6756(3) 0.89298(16) 0.0225(6) Uani 1 1 d . . . . .
H15 H 0.818594 0.738915 0.919764 0.027 Uiso 1 1 calc R U . . .
C16 C 0.8815(4) 0.5709(3) 0.92666(18) 0.0262(6) Uani 1 1 d . . . . .
H16 H 0.894573 0.550524 0.979173 0.031 Uiso 1 1 calc R U . . .
C17 C 0.9006(4) 0.5036(3) 0.86897(17) 0.0243(6) Uani 1 1 d . . . . .
H17 H 0.929910 0.427360 0.873460 0.029 Uiso 1 1 calc R U . . .
N18 N 0.8742(3) 0.3402(2) 0.59205(15) 0.0248(5) Uani 1 1 d . . . . .
H18 H 0.845704 0.345131 0.546019 0.030 Uiso 1 1 calc R U . . .
C19 C 0.9278(4) 0.2377(3) 0.62146(18) 0.0258(6) Uani 1 1 d . . . . .
O20 O 0.9801(3) 0.21958(19) 0.68118(14) 0.0367(6) Uani 1 1 d . . . . .
C21 C 0.9108(4) 0.1499(3) 0.5712(2) 0.0318(7) Uani 1 1 d . . . . .
H21A H 0.975088 0.083285 0.586556 0.048 Uiso 1 1 calc R U . . .
H21B H 0.951459 0.175345 0.516210 0.048 Uiso 1 1 calc R U . . .
H21C H 0.794854 0.134168 0.578370 0.048 Uiso 1 1 calc R U . . .
N22 N 0.7048(3) 0.89534(19) 0.78398(13) 0.0179(5) Uani 1 1 d . . . . .
C23 C 0.5539(4) 0.9064(2) 0.82743(16) 0.0201(6) Uani 1 1 d . . . . .
C24 C 0.5047(4) 0.9906(2) 0.87237(17) 0.0219(6) Uani 1 1 d . . . . .
H24 H 0.396791 0.996954 0.902429 0.026 Uiso 1 1 calc R U . . .
C25 C 0.6208(4) 1.0671(2) 0.87202(16) 0.0222(6) Uani 1 1 d . . . . .
C26 C 0.7806(4) 1.0549(2) 0.82930(17) 0.0211(6) Uani 1 1 d . . . . .
H26 H 0.861393 1.104715 0.829492 0.025 Uiso 1 1 calc R U . . .
C27 C 0.8148(3) 0.9661(2) 0.78669(16) 0.0202(6) Uani 1 1 d . . . . .
N28 N 0.4586(3) 0.8214(2) 0.82015(14) 0.0206(5) Uani 1 1 d . . . . .
N29 N 0.5345(3) 0.74327(19) 0.77314(13) 0.0201(5) Uani 1 1 d . . . . .
C30 C 0.4231(4) 0.6725(2) 0.77658(17) 0.0235(6) Uani 1 1 d . . . . .
H30 H 0.439875 0.609946 0.749025 0.028 Uiso 1 1 calc R U . . .
C31 C 0.2762(4) 0.7016(3) 0.82637(19) 0.0289(7) Uani 1 1 d . . . . .
H31 H 0.178575 0.663056 0.838901 0.035 Uiso 1 1 calc R U . . .
C32 C 0.3021(4) 0.7964(3) 0.85312(18) 0.0264(6) Uani 1 1 d . . . . .
H32 H 0.225631 0.837046 0.887976 0.032 Uiso 1 1 calc R U . . .
N33 N 0.9680(3) 0.93676(19) 0.74250(14) 0.0197(5) Uani 1 1 d . . . . .
N34 N 0.9780(3) 0.8426(2) 0.70558(14) 0.0209(5) Uani 1 1 d . . . . .
C35 C 1.1301(4) 0.8344(2) 0.66657(17) 0.0230(6) Uani 1 1 d . . . . .
H35 H 1.173280 0.777874 0.634980 0.028 Uiso 1 1 calc R U . . .
C36 C 1.2204(4) 0.9204(3) 0.67787(18) 0.0252(6) Uani 1 1 d . . . . .
H36 H 1.332405 0.932119 0.656297 0.030 Uiso 1 1 calc R U . . .
C37 C 1.1144(4) 0.9835(2) 0.72607(17) 0.0231(6) Uani 1 1 d . . . . .
H37 H 1.138533 1.048062 0.744610 0.028 Uiso 1 1 calc R U . . .
N38 N 0.5691(3) 1.1526(2) 0.91739(15) 0.0258(5) Uani 1 1 d . . . . .
H38 H 0.479108 1.143918 0.952952 0.031 Uiso 1 1 calc R U . . .
C39 C 0.6438(4) 1.2494(3) 0.91256(18) 0.0254(6) Uani 1 1 d . . . . .
O40 O 0.7690(3) 1.27136(18) 0.86696(13) 0.0302(5) Uani 1 1 d . . . . .
C41 C 0.5502(5) 1.3273(3) 0.9677(2) 0.0371(8) Uani 1 1 d . . . . .
H41A H 0.594557 1.399573 0.953739 0.056 Uiso 1 1 calc R U . . .
H41B H 0.561559 1.299976 1.021369 0.056 Uiso 1 1 calc R U . . .
H41C H 0.433677 1.332739 0.963821 0.056 Uiso 1 1 calc R U . . .
B42 B 0.7073(14) 0.4368(10) 0.3946(7) 0.022(3) Uiso 0.49 1 d D U P A 1
F43 F 0.7352(6) 0.5523(3) 0.4060(2) 0.0241(10) Uiso 0.49 1 d D U P A 1
F44 F 0.5497(5) 0.4266(4) 0.3986(3) 0.0320(12) Uiso 0.49 1 d D U P A 1
F45 F 0.7936(6) 0.4320(5) 0.3143(3) 0.0272(15) Uiso 0.49 1 d D U P A 1
F46 F 0.7852(6) 0.3663(4) 0.4416(3) 0.0331(13) Uiso 0.49 1 d D U P A 1
Cl42 Cl 0.7142(3) 0.4480(2) 0.38671(15) 0.0254(7) Uiso 0.51 1 d D . P B 2
O43 O 0.6839(8) 0.5500(4) 0.4141(3) 0.0342(15) Uiso 0.51 1 d D . P B 2
O44 O 0.5612(7) 0.3932(5) 0.4009(3) 0.0368(16) Uiso 0.51 1 d D . P B 2
O45 O 0.7849(7) 0.4533(5) 0.3047(3) 0.0236(16) Uiso 0.51 1 d D . P B 2
O46 O 0.8277(6) 0.3802(4) 0.4305(3) 0.0194(11) Uiso 0.51 1 d D . P B 2
B47 B 0.0920(14) 1.1500(10) 0.9559(7) 0.024(2) Uiso 0.41 1 d D U P C 1
F48 F 0.1310(11) 1.1002(7) 0.8909(4) 0.030(2) Uiso 0.41 1 d D U P C 1
F49 F -0.0541(6) 1.1352(5) 0.9991(3) 0.0302(14) Uiso 0.41 1 d D U P C 1
F50 F 0.1073(8) 1.2728(5) 0.9331(4) 0.0339(16) Uiso 0.41 1 d D U P C 1
F51 F 0.2339(10) 1.1306(7) 0.9954(5) 0.028(2) Uiso 0.41 1 d D U P C 1
Cl47 Cl 0.1079(2) 1.16435(16) 0.95327(11) 0.0265(4) Uiso 0.59 1 d D . P D 2
O48 O 0.1251(10) 1.1139(6) 0.8844(4) 0.031(2) Uiso 0.59 1 d D . P D 2
O49 O -0.0415(6) 1.1667(5) 1.0017(3) 0.0394(15) Uiso 0.59 1 d D . P D 2
O50 O 0.1505(7) 1.2799(4) 0.9268(3) 0.0303(13) Uiso 0.59 1 d D . P D 2
O51 O 0.2319(8) 1.1159(6) 1.0011(4) 0.029(2) Uiso 0.59 1 d D . P D 2
C52 C 0.5421(6) 0.6423(3) 0.2478(3) 0.0495(10) Uani 1 1 d . . . . .
H52A H 0.602759 0.584063 0.218979 0.074 Uiso 1 1 calc R U . . .
H52B H 0.485958 0.610608 0.299112 0.074 Uiso 1 1 calc R U . . .
H52C H 0.460684 0.679936 0.218539 0.074 Uiso 1 1 calc R U . . .
C53 C 0.6613(5) 0.7236(3) 0.2584(2) 0.0373(8) Uani 1 1 d . . . . .
H53A H 0.744574 0.685149 0.287152 0.045 Uiso 1 1 calc R U . . .
H53B H 0.719279 0.754533 0.206514 0.045 Uiso 1 1 calc R U . . .
C54 C 0.5764(5) 0.8119(3) 0.3011(2) 0.0346(8) Uani 1 1 d . . . . .
N55 N 0.5078(4) 0.8810(3) 0.3337(2) 0.0484(8) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.902(2) . ?
Fe1 N9 1.993(2) . ?
Fe1 N14 1.960(2) . ?
Fe1 N22 1.907(2) . ?
Fe1 N29 1.969(3) . ?
Fe1 N34 1.991(3) . ?
N2 C3 1.332(4) . ?
N2 C7 1.336(4) . ?
C3 C4 1.376(4) . ?
C3 N8 1.404(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.404(4) . ?
C5 C6 1.403(4) . ?
C5 N18 1.393(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.383(4) . ?
C7 N13 1.405(4) . ?
N8 N9 1.384(3) . ?
N8 C12 1.351(4) . ?
N9 C10 1.324(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.405(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.370(4) . ?
C12 H12 0.9500 . ?
N13 N14 1.373(3) . ?
N13 C17 1.364(4) . ?
N14 C15 1.327(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.400(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.369(4) . ?
C17 H17 0.9500 . ?
N18 H18 0.8800 . ?
N18 C19 1.377(4) . ?
C19 O20 1.201(4) . ?
C19 C21 1.516(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
N22 C23 1.340(4) . ?
N22 C27 1.330(4) . ?
C23 C24 1.373(4) . ?
C23 N28 1.401(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.406(4) . ?
C25 C26 1.398(4) . ?
C25 N38 1.392(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.385(4) . ?
C27 N33 1.400(4) . ?
N28 N29 1.382(3) . ?
N28 C32 1.361(4) . ?
N29 C30 1.315(4) . ?
C30 H30 0.9500 . ?
C30 C31 1.405(4) . ?
C31 H31 0.9500 . ?
C31 C32 1.366(5) . ?
C32 H32 0.9500 . ?
N33 N34 1.392(3) . ?
N33 C37 1.356(4) . ?
N34 C35 1.318(4) . ?
C35 H35 0.9500 . ?
C35 C36 1.408(5) . ?
C36 H36 0.9500 . ?
C36 C37 1.364(4) . ?
C37 H37 0.9500 . ?
N38 H38 0.8800 . ?
N38 C39 1.380(4) . ?
C39 O40 1.210(4) . ?
C39 C41 1.512(4) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
B42 F43 1.509(12) . ?
B42 F44 1.315(11) . ?
B42 F45 1.458(12) . ?
B42 F46 1.338(11) . ?
Cl42 O43 1.392(6) . ?
Cl42 O44 1.455(6) . ?
Cl42 O45 1.441(6) . ?
Cl42 O46 1.474(5) . ?
B47 F48 1.338(12) . ?
B47 F49 1.314(12) . ?
B47 F50 1.529(13) . ?
B47 F51 1.470(12) . ?
Cl47 O48 1.410(6) . ?
Cl47 O49 1.361(5) . ?
Cl47 O50 1.495(5) . ?
Cl47 O51 1.495(6) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C52 C53 1.522(6) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53 C54 1.457(5) . ?
C54 N55 1.138(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N9 79.74(10) . . ?
N2 Fe1 N14 79.62(10) . . ?
N2 Fe1 N22 174.23(10) . . ?
N2 Fe1 N29 95.84(10) . . ?
N2 Fe1 N34 104.40(10) . . ?
N14 Fe1 N9 159.36(10) . . ?
N14 Fe1 N29 89.68(10) . . ?
N14 Fe1 N34 92.88(10) . . ?
N22 Fe1 N9 104.41(10) . . ?
N22 Fe1 N14 96.14(10) . . ?
N22 Fe1 N29 80.14(10) . . ?
N22 Fe1 N34 79.60(10) . . ?
N29 Fe1 N9 91.97(10) . . ?
N29 Fe1 N34 159.73(10) . . ?
N34 Fe1 N9 92.66(10) . . ?
C3 N2 Fe1 120.6(2) . . ?
C3 N2 C7 118.6(2) . . ?
C7 N2 Fe1 120.32(19) . . ?
N2 C3 C4 123.6(3) . . ?
N2 C3 N8 110.9(2) . . ?
C4 C3 N8 125.5(3) . . ?
C3 C4 H4 121.5 . . ?
C3 C4 C5 117.0(3) . . ?
C5 C4 H4 121.5 . . ?
C6 C5 C4 120.7(3) . . ?
N18 C5 C4 115.6(3) . . ?
N18 C5 C6 123.7(3) . . ?
C5 C6 H6 121.8 . . ?
C7 C6 C5 116.3(3) . . ?
C7 C6 H6 121.8 . . ?
N2 C7 C6 123.8(3) . . ?
N2 C7 N13 110.3(2) . . ?
C6 C7 N13 125.9(3) . . ?
N9 N8 C3 116.5(2) . . ?
C12 N8 C3 132.5(3) . . ?
C12 N8 N9 110.8(2) . . ?
N8 N9 Fe1 112.08(17) . . ?
C10 N9 Fe1 142.5(2) . . ?
C10 N9 N8 105.2(2) . . ?
N9 C10 H10 124.5 . . ?
N9 C10 C11 111.0(3) . . ?
C11 C10 H10 124.5 . . ?
C10 C11 H11 127.2 . . ?
C12 C11 C10 105.7(3) . . ?
C12 C11 H11 127.2 . . ?
N8 C12 C11 107.3(3) . . ?
N8 C12 H12 126.4 . . ?
C11 C12 H12 126.4 . . ?
N14 N13 C7 116.1(2) . . ?
C17 N13 C7 132.8(3) . . ?
C17 N13 N14 111.0(2) . . ?
N13 N14 Fe1 113.48(18) . . ?
C15 N14 Fe1 140.6(2) . . ?
C15 N14 N13 105.6(2) . . ?
N14 C15 H15 124.7 . . ?
N14 C15 C16 110.6(3) . . ?
C16 C15 H15 124.7 . . ?
C15 C16 H16 126.8 . . ?
C17 C16 C15 106.4(3) . . ?
C17 C16 H16 126.8 . . ?
N13 C17 C16 106.4(3) . . ?
N13 C17 H17 126.8 . . ?
C16 C17 H17 126.8 . . ?
C5 N18 H18 116.1 . . ?
C19 N18 C5 127.8(3) . . ?
C19 N18 H18 116.1 . . ?
N18 C19 C21 112.8(3) . . ?
O20 C19 N18 123.6(3) . . ?
O20 C19 C21 123.6(3) . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 N22 Fe1 119.7(2) . . ?
C27 N22 Fe1 120.8(2) . . ?
C27 N22 C23 119.0(2) . . ?
N22 C23 C24 123.0(3) . . ?
N22 C23 N28 110.7(2) . . ?
C24 C23 N28 126.3(3) . . ?
C23 C24 H24 121.4 . . ?
C23 C24 C25 117.2(3) . . ?
C25 C24 H24 121.4 . . ?
C26 C25 C24 120.7(3) . . ?
N38 C25 C24 116.6(3) . . ?
N38 C25 C26 122.6(3) . . ?
C25 C26 H26 121.8 . . ?
C27 C26 C25 116.4(3) . . ?
C27 C26 H26 121.8 . . ?
N22 C27 C26 123.7(3) . . ?
N22 C27 N33 110.8(2) . . ?
C26 C27 N33 125.5(3) . . ?
N29 N28 C23 116.6(2) . . ?
C32 N28 C23 132.6(3) . . ?
C32 N28 N29 110.8(2) . . ?
N28 N29 Fe1 112.54(18) . . ?
C30 N29 Fe1 141.9(2) . . ?
C30 N29 N28 105.4(2) . . ?
N29 C30 H30 124.5 . . ?
N29 C30 C31 111.1(3) . . ?
C31 C30 H30 124.5 . . ?
C30 C31 H31 127.0 . . ?
C32 C31 C30 106.0(3) . . ?
C32 C31 H31 127.0 . . ?
N28 C32 C31 106.7(3) . . ?
N28 C32 H32 126.7 . . ?
C31 C32 H32 126.7 . . ?
N34 N33 C27 116.6(2) . . ?
C37 N33 C27 132.7(3) . . ?
C37 N33 N34 110.7(2) . . ?
N33 N34 Fe1 112.02(18) . . ?
C35 N34 Fe1 142.8(2) . . ?
C35 N34 N33 105.1(2) . . ?
N34 C35 H35 124.5 . . ?
N34 C35 C36 111.0(3) . . ?
C36 C35 H35 124.5 . . ?
C35 C36 H36 127.0 . . ?
C37 C36 C35 106.1(3) . . ?
C37 C36 H36 127.0 . . ?
N33 C37 C36 107.0(3) . . ?
N33 C37 H37 126.5 . . ?
C36 C37 H37 126.5 . . ?
C25 N38 H38 116.5 . . ?
C39 N38 C25 127.0(3) . . ?
C39 N38 H38 116.5 . . ?
N38 C39 C41 113.3(3) . . ?
O40 C39 N38 123.5(3) . . ?
O40 C39 C41 123.2(3) . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
F44 B42 F43 109.8(8) . . ?
F44 B42 F45 109.4(8) . . ?
F44 B42 F46 117.6(9) . . ?
F45 B42 F43 100.7(7) . . ?
F46 B42 F43 109.6(8) . . ?
F46 B42 F45 108.5(8) . . ?
O43 Cl42 O44 109.3(4) . . ?
O43 Cl42 O45 113.5(4) . . ?
O43 Cl42 O46 109.4(3) . . ?
O44 Cl42 O46 107.4(4) . . ?
O45 Cl42 O44 108.9(4) . . ?
O45 Cl42 O46 108.2(3) . . ?
F48 B47 F50 108.3(9) . . ?
F48 B47 F51 106.9(9) . . ?
F49 B47 F48 117.2(10) . . ?
F49 B47 F50 108.1(9) . . ?
F49 B47 F51 117.2(9) . . ?
F51 B47 F50 96.9(8) . . ?
O48 Cl47 O50 105.4(4) . . ?
O48 Cl47 O51 111.0(4) . . ?
O49 Cl47 O48 118.4(4) . . ?
O49 Cl47 O50 107.7(3) . . ?
O49 Cl47 O51 107.4(4) . . ?
O50 Cl47 O51 106.1(4) . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C53 C52 H52A 109.5 . . ?
C53 C52 H52B 109.5 . . ?
C53 C52 H52C 109.5 . . ?
C52 C53 H53A 109.3 . . ?
C52 C53 H53B 109.3 . . ?
H53A C53 H53B 108.0 . . ?
C54 C53 C52 111.4(3) . . ?
C54 C53 H53A 109.3 . . ?
C54 C53 H53B 109.3 . . ?
N55 C54 C53 178.7(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N18 H18 F46 0.88 1.98 2.855(5) 176.3 . yes
N18 H18 O46 0.88 2.05 2.915(5) 165.9 . yes
N38 H38 F51 0.88 2.04 2.873(9) 157.0 . yes
N38 H38 O51 0.88 2.10 2.942(8) 159.0 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N2 C3 C4 -174.4(2) . . . . ?
Fe1 N2 C3 N8 3.5(3) . . . . ?
Fe1 N2 C7 C6 173.4(2) . . . . ?
Fe1 N2 C7 N13 -4.5(3) . . . . ?
Fe1 N9 C10 C11 -173.1(3) . . . . ?
Fe1 N14 C15 C16 173.1(2) . . . . ?
Fe1 N22 C23 C24 175.1(2) . . . . ?
Fe1 N22 C23 N28 -4.7(3) . . . . ?
Fe1 N22 C27 C26 -175.3(2) . . . . ?
Fe1 N22 C27 N33 3.3(3) . . . . ?
Fe1 N29 C30 C31 174.2(2) . . . . ?
Fe1 N34 C35 C36 -178.5(3) . . . . ?
N2 C3 C4 C5 1.7(4) . . . . ?
N2 C3 N8 N9 -0.8(3) . . . . ?
N2 C3 N8 C12 -176.8(3) . . . . ?
N2 C7 N13 N14 2.1(3) . . . . ?
N2 C7 N13 C17 177.4(3) . . . . ?
C3 N2 C7 C6 1.4(4) . . . . ?
C3 N2 C7 N13 -176.5(2) . . . . ?
C3 C4 C5 C6 0.0(4) . . . . ?
C3 C4 C5 N18 177.8(3) . . . . ?
C3 N8 N9 Fe1 -1.9(3) . . . . ?
C3 N8 N9 C10 -177.7(2) . . . . ?
C3 N8 C12 C11 177.0(3) . . . . ?
C4 C3 N8 N9 177.0(3) . . . . ?
C4 C3 N8 C12 1.1(5) . . . . ?
C4 C5 C6 C7 -0.9(4) . . . . ?
C4 C5 N18 C19 174.8(3) . . . . ?
C5 C6 C7 N2 0.2(4) . . . . ?
C5 C6 C7 N13 177.8(3) . . . . ?
C5 N18 C19 O20 -4.7(5) . . . . ?
C5 N18 C19 C21 174.2(3) . . . . ?
C6 C5 N18 C19 -7.5(5) . . . . ?
C6 C7 N13 N14 -175.7(3) . . . . ?
C6 C7 N13 C17 -0.5(5) . . . . ?
C7 N2 C3 C4 -2.4(4) . . . . ?
C7 N2 C3 N8 175.5(2) . . . . ?
C7 N13 N14 Fe1 0.9(3) . . . . ?
C7 N13 N14 C15 176.2(2) . . . . ?
C7 N13 C17 C16 -175.2(3) . . . . ?
N8 C3 C4 C5 -175.9(3) . . . . ?
N8 N9 C10 C11 0.5(3) . . . . ?
N9 N8 C12 C11 0.9(3) . . . . ?
N9 C10 C11 C12 0.0(4) . . . . ?
C10 C11 C12 N8 -0.5(4) . . . . ?
C12 N8 N9 Fe1 174.9(2) . . . . ?
C12 N8 N9 C10 -0.9(3) . . . . ?
N13 N14 C15 C16 -0.2(3) . . . . ?
N14 N13 C17 C16 0.2(3) . . . . ?
N14 C15 C16 C17 0.3(4) . . . . ?
C15 C16 C17 N13 -0.3(3) . . . . ?
C17 N13 N14 Fe1 -175.36(19) . . . . ?
C17 N13 N14 C15 0.0(3) . . . . ?
N18 C5 C6 C7 -178.5(3) . . . . ?
N22 C23 C24 C25 -0.4(4) . . . . ?
N22 C23 N28 N29 1.5(3) . . . . ?
N22 C23 N28 C32 178.7(3) . . . . ?
N22 C27 N33 N34 -0.4(3) . . . . ?
N22 C27 N33 C37 178.1(3) . . . . ?
C23 N22 C27 C26 -3.3(4) . . . . ?
C23 N22 C27 N33 175.4(2) . . . . ?
C23 C24 C25 C26 -1.9(4) . . . . ?
C23 C24 C25 N38 179.6(3) . . . . ?
C23 N28 N29 Fe1 2.0(3) . . . . ?
C23 N28 N29 C30 178.9(2) . . . . ?
C23 N28 C32 C31 -178.0(3) . . . . ?
C24 C23 N28 N29 -178.3(3) . . . . ?
C24 C23 N28 C32 -1.1(5) . . . . ?
C24 C25 C26 C27 1.7(4) . . . . ?
C24 C25 N38 C39 -163.5(3) . . . . ?
C25 C26 C27 N22 1.0(4) . . . . ?
C25 C26 C27 N33 -177.5(3) . . . . ?
C25 N38 C39 O40 -0.9(5) . . . . ?
C25 N38 C39 C41 176.9(3) . . . . ?
C26 C25 N38 C39 18.1(5) . . . . ?
C26 C27 N33 N34 178.3(3) . . . . ?
C26 C27 N33 C37 -3.2(5) . . . . ?
C27 N22 C23 C24 3.0(4) . . . . ?
C27 N22 C23 N28 -176.8(2) . . . . ?
C27 N33 N34 Fe1 -2.4(3) . . . . ?
C27 N33 N34 C35 178.2(2) . . . . ?
C27 N33 C37 C36 -178.2(3) . . . . ?
N28 C23 C24 C25 179.4(3) . . . . ?
N28 N29 C30 C31 -1.2(3) . . . . ?
N29 N28 C32 C31 -0.6(3) . . . . ?
N29 C30 C31 C32 0.9(4) . . . . ?
C30 C31 C32 N28 -0.1(4) . . . . ?
C32 N28 N29 Fe1 -175.75(19) . . . . ?
C32 N28 N29 C30 1.2(3) . . . . ?
N33 N34 C35 C36 0.7(3) . . . . ?
N34 N33 C37 C36 0.4(3) . . . . ?
N34 C35 C36 C37 -0.4(4) . . . . ?
C35 C36 C37 N33 0.0(3) . . . . ?
C37 N33 N34 Fe1 178.78(18) . . . . ?
C37 N33 N34 C35 -0.7(3) . . . . ?
N38 C25 C26 C27 -179.9(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: propionitrile/diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ic80-men
_database_code_depnum_ccdc_archive 'CCDC 2078661'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2021-04-19 deposited with the CCDC.	2021-06-10 downloaded from the CCDC.
;
_audit_creation_date             2020-07-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis-[N-(2,6-di{pyrazol-1-yl}pyrid-4-yl)acetamide]iron(II)ditetrafluoroborate bis-nitromethane solvate'
_chemical_formula_moiety         'C26 H24 Fe N12 O2, 2(B F4), 2(C H3 N O2)'
_chemical_formula_sum            'C28 H30 B2 F8 Fe N14 O6'
_chemical_formula_weight         888.13
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'

_cell_length_a                   20.7377(3)
_cell_length_b                   8.8852(2)
_cell_length_c                   19.6895(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3627.96(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4195
_cell_measurement_temperature    120(2)
_cell_measurement_theta_min      4.24
_cell_measurement_theta_max      73.44
_exptl_absorpt_coefficient_mu    4.283
_exptl_absorpt_correction_T_min  0.561
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8233
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_detector                 'CCD plate'
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.795
_diffrn_reflns_theta_min         4.264
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3036
_reflns_number_total             3449
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2015)'
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         3449
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0343
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0455P)²+1.8193P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0874
_refine_special_details          
;
 The asymmetric unit contains half a formula unit, with Fe1 lying on the
 C₂ axis 1/2, y, 1/4. No disorder is present in the model, and all non-H 
 atoms were refined anisotropically. H atoms were placed in calculated 
 positions and refined using a riding model. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N18-H18
 0.95 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17),
 N18(H18)
3.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C27(H27A,H27B,H27C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.500000 0.70128(5) 0.250000 0.01685(12) Uani 1 2 d S T P . .
N2 N 0.39799(7) 0.69395(17) 0.24918(7) 0.0154(3) Uani 1 1 d . . . . .
C3 C 0.36597(8) 0.6101(2) 0.20395(8) 0.0159(3) Uani 1 1 d . . . . .
C4 C 0.29989(8) 0.6045(2) 0.19954(9) 0.0174(4) Uani 1 1 d . . . . .
H4 H 0.278965 0.542907 0.166844 0.021 Uiso 1 1 calc R U . . .
C5 C 0.26451(8) 0.6933(2) 0.24519(8) 0.0166(4) Uani 1 1 d . . . . .
C6 C 0.29679(8) 0.7848(2) 0.29223(9) 0.0169(4) Uani 1 1 d . . . . .
H6 H 0.274112 0.848141 0.322890 0.020 Uiso 1 1 calc R U . . .
C7 C 0.36327(8) 0.7779(2) 0.29158(8) 0.0156(3) Uani 1 1 d . . . . .
N8 N 0.40700(6) 0.52592(17) 0.16107(7) 0.0172(3) Uani 1 1 d . . . . .
N9 N 0.47234(7) 0.54243(18) 0.16896(8) 0.0194(3) Uani 1 1 d . . . . .
C10 C 0.49800(8) 0.4553(2) 0.12128(10) 0.0245(4) Uani 1 1 d . . . . .
H10 H 0.543032 0.444067 0.114021 0.029 Uiso 1 1 calc R U . . .
C11 C 0.45055(9) 0.3823(2) 0.08307(10) 0.0277(4) Uani 1 1 d . . . . .
H11 H 0.456881 0.314451 0.046363 0.033 Uiso 1 1 calc R U . . .
C12 C 0.39309(9) 0.4292(2) 0.10980(9) 0.0227(4) Uani 1 1 d . . . . .
H12 H 0.351301 0.399713 0.095211 0.027 Uiso 1 1 calc R U . . .
N13 N 0.40218(7) 0.86199(17) 0.33686(7) 0.0166(3) Uani 1 1 d . . . . .
N14 N 0.46759(7) 0.85934(18) 0.32732(8) 0.0191(3) Uani 1 1 d . . . . .
C15 C 0.49144(9) 0.9402(2) 0.37822(10) 0.0235(4) Uani 1 1 d . . . . .
H15 H 0.536074 0.959053 0.384966 0.028 Uiso 1 1 calc R U . . .
C16 C 0.44238(8) 0.9940(2) 0.42066(9) 0.0247(4) Uani 1 1 d . . . . .
H16 H 0.447157 1.054336 0.460180 0.030 Uiso 1 1 calc R U . . .
C17 C 0.38614(8) 0.9414(2) 0.39319(9) 0.0211(4) Uani 1 1 d . . . . .
H17 H 0.343873 0.957492 0.410315 0.025 Uiso 1 1 calc R U . . .
N18 N 0.19796(7) 0.68306(19) 0.24037(8) 0.0201(3) Uani 1 1 d D . . . .
H18 H 0.183448 0.619764 0.209583 0.024 Uiso 1 1 calc DR U . . .
C19 C 0.15140(8) 0.7579(2) 0.27695(9) 0.0183(4) Uani 1 1 d . . . . .
O20 O 0.16305(6) 0.85338(16) 0.31923(7) 0.0244(3) Uani 1 1 d . . . . .
C21 C 0.08345(9) 0.7113(2) 0.25885(10) 0.0227(4) Uani 1 1 d . . . . .
H21A H 0.064235 0.656781 0.297108 0.034 Uiso 1 1 calc R U . . .
H21B H 0.084417 0.645770 0.218816 0.034 Uiso 1 1 calc R U . . .
H21C H 0.057630 0.800970 0.248900 0.034 Uiso 1 1 calc R U . . .
B22 B 0.16920(11) 0.4438(3) 0.08443(11) 0.0252(5) Uani 1 1 d . . . . .
F23 F 0.15194(5) 0.45593(14) 0.15347(6) 0.0289(3) Uani 1 1 d . . . . .
F24 F 0.16433(8) 0.58254(19) 0.05510(9) 0.0604(5) Uani 1 1 d . . . . .
F25 F 0.23198(5) 0.39014(15) 0.08023(6) 0.0339(3) Uani 1 1 d . . . . .
F26 F 0.12685(6) 0.3445(2) 0.05438(8) 0.0549(5) Uani 1 1 d . . . . .
C27 C 0.19175(10) 0.8856(2) 0.47244(10) 0.0287(4) Uani 1 1 d . . . . .
H27A H 0.149191 0.872094 0.493187 0.043 Uiso 1 1 calc R U . . .
H27B H 0.224977 0.882298 0.507804 0.043 Uiso 1 1 calc R U . . .
H27C H 0.199477 0.804986 0.439483 0.043 Uiso 1 1 calc R U . . .
N28 N 0.19418(7) 1.03242(19) 0.43761(8) 0.0225(3) Uani 1 1 d . . . . .
O29 O 0.14600(7) 1.11081(19) 0.43773(9) 0.0395(4) Uani 1 1 d . . . . .
O30 O 0.24470(7) 1.06832(17) 0.40967(7) 0.0293(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.1165(15) . ?
Fe1 N9 2.2061(16) . ?
Fe1 N14 2.1776(16) . ?
N2 C3 1.337(2) . ?
N2 C7 1.331(2) . ?
C3 C4 1.374(2) . ?
C3 N8 1.413(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.403(2) . ?
C5 C6 1.402(2) . ?
C5 N18 1.386(2) . ?
C6 H6 0.9500 . ?
C6 C7 1.380(2) . ?
C7 N13 1.416(2) . ?
N8 N9 1.3718(19) . ?
N8 C12 1.357(2) . ?
N9 C10 1.328(2) . ?
C10 H10 0.9500 . ?
C10 C11 1.399(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.368(3) . ?
C12 H12 0.9500 . ?
N13 N14 1.3694(19) . ?
N13 C17 1.356(2) . ?
N14 C15 1.328(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.401(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.368(2) . ?
C17 H17 0.9500 . ?
N18 H18 0.8800 . ?
N18 C19 1.376(2) . ?
C19 O20 1.213(2) . ?
C19 C21 1.511(2) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
B22 F23 1.410(2) . ?
B22 F24 1.365(3) . ?
B22 F25 1.389(2) . ?
B22 F26 1.378(3) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C27 N28 1.474(3) . ?
N28 O29 1.218(2) . ?
N28 O30 1.226(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 176.47(8) . 4_655 ?
N2 Fe1 N9 104.22(5) . 4_655 ?
N2 Fe1 N9 73.44(5) . . ?
N2 Fe1 N14 108.85(5) . 4_655 ?
N2 Fe1 N14 73.54(5) . . ?
N9 Fe1 N9 100.45(8) . 4_655 ?
N14 Fe1 N9 89.27(6) . 4_655 ?
N14 Fe1 N9 146.93(5) . . ?
N14 Fe1 N14 99.68(8) 4_655 . ?
C3 N2 Fe1 121.23(12) . . ?
C7 N2 Fe1 121.24(12) . . ?
C7 N2 C3 117.46(15) . . ?
N2 C3 C4 123.88(16) . . ?
N2 C3 N8 113.19(14) . . ?
C4 C3 N8 122.93(16) . . ?
C3 C4 H4 121.3 . . ?
C3 C4 C5 117.43(16) . . ?
C5 C4 H4 121.3 . . ?
C6 C5 C4 119.96(16) . . ?
N18 C5 C4 116.10(16) . . ?
N18 C5 C6 123.94(16) . . ?
C5 C6 H6 121.8 . . ?
C7 C6 C5 116.41(16) . . ?
C7 C6 H6 121.8 . . ?
N2 C7 C6 124.84(16) . . ?
N2 C7 N13 112.48(14) . . ?
C6 C7 N13 122.68(16) . . ?
N9 N8 C3 118.07(14) . . ?
C12 N8 C3 130.69(15) . . ?
C12 N8 N9 111.22(14) . . ?
N8 N9 Fe1 114.02(11) . . ?
C10 N9 Fe1 141.26(12) . . ?
C10 N9 N8 104.68(14) . . ?
N9 C10 H10 124.2 . . ?
N9 C10 C11 111.65(16) . . ?
C11 C10 H10 124.2 . . ?
C10 C11 H11 127.3 . . ?
C12 C11 C10 105.32(17) . . ?
C12 C11 H11 127.3 . . ?
N8 C12 C11 107.12(16) . . ?
N8 C12 H12 126.4 . . ?
C11 C12 H12 126.4 . . ?
N14 N13 C7 117.98(14) . . ?
C17 N13 C7 130.54(15) . . ?
C17 N13 N14 111.35(14) . . ?
N13 N14 Fe1 114.37(11) . . ?
C15 N14 Fe1 139.56(12) . . ?
C15 N14 N13 104.84(14) . . ?
N14 C15 H15 124.3 . . ?
N14 C15 C16 111.36(16) . . ?
C16 C15 H15 124.3 . . ?
C15 C16 H16 127.3 . . ?
C17 C16 C15 105.46(16) . . ?
C17 C16 H16 127.3 . . ?
N13 C17 C16 106.98(16) . . ?
N13 C17 H17 126.5 . . ?
C16 C17 H17 126.5 . . ?
C5 N18 H18 115.4 . . ?
C19 N18 C5 129.13(16) . . ?
C19 N18 H18 115.4 . . ?
N18 C19 C21 113.47(16) . . ?
O20 C19 N18 123.89(16) . . ?
O20 C19 C21 122.64(16) . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
F24 B22 F23 108.68(18) . . ?
F24 B22 F25 110.75(19) . . ?
F24 B22 F26 110.44(19) . . ?
F25 B22 F23 108.76(16) . . ?
F26 B22 F23 107.51(18) . . ?
F26 B22 F25 110.60(18) . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N28 C27 H27A 109.5 . . ?
N28 C27 H27B 109.5 . . ?
N28 C27 H27C 109.5 . . ?
O29 N28 C27 118.49(17) . . ?
O29 N28 O30 123.59(17) . . ?
O30 N28 C27 117.92(16) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N18 H18 F23 0.88 1.94 2.8127(19) 170.6 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N2 C3 C4 -177.88(13) . . . . ?
Fe1 N2 C3 N8 2.7(2) . . . . ?
Fe1 N2 C7 C6 176.91(13) . . . . ?
Fe1 N2 C7 N13 -2.8(2) . . . . ?
Fe1 N9 C10 C11 -177.90(15) . . . . ?
Fe1 N14 C15 C16 -165.31(15) . . . . ?
N2 C3 C4 C5 0.4(3) . . . . ?
N2 C3 N8 N9 -1.9(2) . . . . ?
N2 C3 N8 C12 179.93(18) . . . . ?
N2 C7 N13 N14 6.5(2) . . . . ?
N2 C7 N13 C17 -168.79(18) . . . . ?
C3 N2 C7 C6 -0.1(3) . . . . ?
C3 N2 C7 N13 -179.77(15) . . . . ?
C3 C4 C5 C6 0.9(3) . . . . ?
C3 C4 C5 N18 -178.82(16) . . . . ?
C3 N8 N9 Fe1 0.33(19) . . . . ?
C3 N8 N9 C10 -177.97(16) . . . . ?
C3 N8 C12 C11 177.76(18) . . . . ?
C4 C3 N8 N9 178.68(16) . . . . ?
C4 C3 N8 C12 0.5(3) . . . . ?
C4 C5 C6 C7 -1.8(2) . . . . ?
C4 C5 N18 C19 -178.57(18) . . . . ?
C5 C6 C7 N2 1.4(3) . . . . ?
C5 C6 C7 N13 -178.96(16) . . . . ?
C5 N18 C19 O20 3.2(3) . . . . ?
C5 N18 C19 C21 -177.53(17) . . . . ?
C6 C5 N18 C19 1.7(3) . . . . ?
C6 C7 N13 N14 -173.21(16) . . . . ?
C6 C7 N13 C17 11.5(3) . . . . ?
C7 N2 C3 C4 -0.9(3) . . . . ?
C7 N2 C3 N8 179.67(15) . . . . ?
C7 N13 N14 Fe1 -7.08(19) . . . . ?
C7 N13 N14 C15 -176.96(16) . . . . ?
C7 N13 C17 C16 176.43(18) . . . . ?
N8 C3 C4 C5 179.83(16) . . . . ?
N8 N9 C10 C11 -0.4(2) . . . . ?
N9 N8 C12 C11 -0.5(2) . . . . ?
N9 C10 C11 C12 0.1(3) . . . . ?
C10 C11 C12 N8 0.3(2) . . . . ?
C12 N8 N9 Fe1 178.86(12) . . . . ?
C12 N8 N9 C10 0.6(2) . . . . ?
N13 N14 C15 C16 0.4(2) . . . . ?
N14 N13 C17 C16 0.9(2) . . . . ?
N14 C15 C16 C17 0.1(2) . . . . ?
C15 C16 C17 N13 -0.6(2) . . . . ?
C17 N13 N14 Fe1 169.07(12) . . . . ?
C17 N13 N14 C15 -0.8(2) . . . . ?
N18 C5 C6 C7 177.97(17) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: nitromethane/diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_80clo4nm
_database_code_depnum_ccdc_archive 'CCDC 2078662'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2021-04-19 deposited with the CCDC.	2021-06-10 downloaded from the CCDC.
;
_audit_creation_date             2020-07-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis-[N-(2,6-di{pyrazol-1-yl}pyrid-4-yl)acetamide]iron(II)diperchlorate bis-nitromethane solvate'
_chemical_formula_moiety         'C26 H24 Fe N12 O2, 2(Cl O4), 2(C H3 N O2)'
_chemical_formula_sum            'C28 H30 Cl2 Fe N14 O14'
_chemical_formula_weight         913.41
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'

_cell_length_a                   20.7926(4)
_cell_length_b                   8.8370(3)
_cell_length_c                   20.0553(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3685.05(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4187
_cell_measurement_temperature    120(2)
_cell_measurement_theta_min      4.23
_cell_measurement_theta_max      73.36
_exptl_absorpt_coefficient_mu    5.394
_exptl_absorpt_correction_T_min  0.662
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9763
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.706
_diffrn_reflns_theta_min         4.253
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3121
_reflns_number_total             3626
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2015)'
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         3626
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0383
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0503P)²+2.2433P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1036
_refine_special_details          
;
 The asymmetric unit contains half a formula unit, with Fe1 lying on the
 C₂ axis 1/2, y, 1/4. No disorder is present in the model, and all non-H 
 atoms were refined anisotropically. H atoms were placed in calculated 
 positions and refined using a riding model. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17),
 N18(H18)
2.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C27(H27A,H27B,H27C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.500000 0.71985(6) 0.250000 0.02304(15) Uani 1 2 d S T P . .
N2 N 0.39790(8) 0.7100(2) 0.24921(9) 0.0207(4) Uani 1 1 d . . . . .
C3 C 0.36640(9) 0.6262(3) 0.20479(11) 0.0225(5) Uani 1 1 d . . . . .
C4 C 0.30055(10) 0.6200(3) 0.20024(11) 0.0236(5) Uani 1 1 d . . . . .
H4 H 0.279783 0.557758 0.168187 0.028 Uiso 1 1 calc R U . . .
C5 C 0.26533(10) 0.7094(3) 0.24488(11) 0.0231(5) Uani 1 1 d . . . . .
C6 C 0.29693(10) 0.8009(3) 0.29146(11) 0.0231(5) Uani 1 1 d . . . . .
H6 H 0.274063 0.863933 0.321643 0.028 Uiso 1 1 calc R U . . .
C7 C 0.36335(10) 0.7943(3) 0.29100(11) 0.0216(5) Uani 1 1 d . . . . .
N8 N 0.40760(8) 0.5427(2) 0.16253(9) 0.0236(4) Uani 1 1 d . . . . .
N9 N 0.47261(8) 0.5591(2) 0.17076(10) 0.0253(4) Uani 1 1 d . . . . .
C10 C 0.49865(10) 0.4730(3) 0.12346(13) 0.0299(5) Uani 1 1 d . . . . .
H10 H 0.543605 0.462401 0.116374 0.036 Uiso 1 1 calc R U . . .
C11 C 0.45139(11) 0.3999(3) 0.08544(13) 0.0330(6) Uani 1 1 d . . . . .
H11 H 0.457828 0.332323 0.049198 0.040 Uiso 1 1 calc R U . . .
C12 C 0.39387(11) 0.4467(3) 0.11175(12) 0.0294(5) Uani 1 1 d . . . . .
H12 H 0.352225 0.417402 0.097153 0.035 Uiso 1 1 calc R U . . .
N13 N 0.40187(8) 0.8786(2) 0.33563(9) 0.0225(4) Uani 1 1 d . . . . .
N14 N 0.46706(8) 0.8782(2) 0.32580(10) 0.0252(4) Uani 1 1 d . . . . .
C15 C 0.49055(10) 0.9598(3) 0.37595(13) 0.0297(5) Uani 1 1 d . . . . .
H15 H 0.534989 0.980072 0.382399 0.036 Uiso 1 1 calc R U . . .
C16 C 0.44161(11) 1.0120(3) 0.41805(12) 0.0312(5) Uani 1 1 d . . . . .
H16 H 0.446176 1.072286 0.456970 0.037 Uiso 1 1 calc R U . . .
C17 C 0.38577(10) 0.9574(3) 0.39104(12) 0.0283(5) Uani 1 1 d . . . . .
H17 H 0.343577 0.971999 0.408037 0.034 Uiso 1 1 calc R U . . .
N18 N 0.19867(9) 0.6995(2) 0.23944(10) 0.0254(4) Uani 1 1 d . . . . .
H18 H 0.184402 0.637095 0.208593 0.031 Uiso 1 1 calc R U . . .
C19 C 0.15201(10) 0.7735(3) 0.27554(12) 0.0241(5) Uani 1 1 d . . . . .
O20 O 0.16361(7) 0.8687(2) 0.31765(9) 0.0298(4) Uani 1 1 d . . . . .
C21 C 0.08436(11) 0.7272(3) 0.25739(12) 0.0279(5) Uani 1 1 d . . . . .
H21A H 0.064279 0.676340 0.295507 0.042 Uiso 1 1 calc R U . . .
H21B H 0.085604 0.657840 0.219269 0.042 Uiso 1 1 calc R U . . .
H21C H 0.059291 0.817177 0.245612 0.042 Uiso 1 1 calc R U . . .
Cl22 Cl 0.16921(2) 0.44368(7) 0.08325(3) 0.02784(15) Uani 1 1 d . . . . .
O23 O 0.15148(8) 0.4703(2) 0.15236(8) 0.0328(4) Uani 1 1 d . . . . .
O24 O 0.16344(10) 0.5815(3) 0.04672(11) 0.0505(5) Uani 1 1 d . . . . .
O25 O 0.23432(8) 0.3892(2) 0.08095(9) 0.0395(5) Uani 1 1 d . . . . .
O26 O 0.12632(8) 0.3319(3) 0.05694(10) 0.0443(5) Uani 1 1 d . . . . .
C27 C 0.18881(13) 0.8970(3) 0.46771(13) 0.0353(6) Uani 1 1 d . . . . .
H27A H 0.146535 0.884898 0.488659 0.053 Uiso 1 1 calc R U . . .
H27B H 0.222426 0.889436 0.501802 0.053 Uiso 1 1 calc R U . . .
H27C H 0.195047 0.817330 0.434332 0.053 Uiso 1 1 calc R U . . .
N28 N 0.19243(9) 1.0459(2) 0.43524(10) 0.0288(4) Uani 1 1 d . . . . .
O29 O 0.14478(9) 1.1258(2) 0.43543(11) 0.0473(5) Uani 1 1 d . . . . .
O30 O 0.24343(8) 1.0820(2) 0.40910(9) 0.0363(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.1247(18) . ?
Fe1 N9 2.206(2) . ?
Fe1 N14 2.177(2) . ?
N2 C3 1.331(3) . ?
N2 C7 1.332(3) . ?
C3 C4 1.373(3) . ?
C3 N8 1.413(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.401(3) . ?
C5 C6 1.399(3) . ?
C5 N18 1.393(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.382(3) . ?
C7 N13 1.413(3) . ?
N8 N9 1.369(2) . ?
N8 C12 1.356(3) . ?
N9 C10 1.331(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.402(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.371(3) . ?
C12 H12 0.9500 . ?
N13 N14 1.370(2) . ?
N13 C17 1.353(3) . ?
N14 C15 1.330(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.400(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.369(3) . ?
C17 H17 0.9500 . ?
N18 H18 0.8800 . ?
N18 C19 1.376(3) . ?
C19 O20 1.216(3) . ?
C19 C21 1.510(3) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
Cl22 O23 1.4533(17) . ?
Cl22 O24 1.426(2) . ?
Cl22 O25 1.4375(17) . ?
Cl22 O26 1.4315(19) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C27 N28 1.470(3) . ?
N28 O29 1.217(3) . ?
N28 O30 1.225(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 175.29(11) 4_655 . ?
N2 Fe1 N9 73.16(7) . . ?
N2 Fe1 N9 103.70(7) . 4_655 ?
N2 Fe1 N14 73.57(7) . . ?
N2 Fe1 N14 109.61(7) . 4_655 ?
N9 Fe1 N9 99.85(11) 4_655 . ?
N14 Fe1 N9 146.69(6) . . ?
N14 Fe1 N9 89.55(7) . 4_655 ?
N14 Fe1 N14 99.98(11) 4_655 . ?
C3 N2 Fe1 121.31(14) . . ?
C3 N2 C7 117.84(18) . . ?
C7 N2 Fe1 120.75(14) . . ?
N2 C3 C4 123.9(2) . . ?
N2 C3 N8 113.19(17) . . ?
C4 C3 N8 122.9(2) . . ?
C3 C4 H4 121.4 . . ?
C3 C4 C5 117.2(2) . . ?
C5 C4 H4 121.4 . . ?
C6 C5 C4 120.5(2) . . ?
N18 C5 C4 115.8(2) . . ?
N18 C5 C6 123.8(2) . . ?
C5 C6 H6 121.9 . . ?
C7 C6 C5 116.1(2) . . ?
C7 C6 H6 121.9 . . ?
N2 C7 C6 124.5(2) . . ?
N2 C7 N13 112.82(17) . . ?
C6 C7 N13 122.6(2) . . ?
N9 N8 C3 118.08(18) . . ?
C12 N8 C3 130.51(18) . . ?
C12 N8 N9 111.39(18) . . ?
N8 N9 Fe1 114.20(14) . . ?
C10 N9 Fe1 140.92(15) . . ?
C10 N9 N8 104.77(18) . . ?
N9 C10 H10 124.3 . . ?
N9 C10 C11 111.47(19) . . ?
C11 C10 H10 124.3 . . ?
C10 C11 H11 127.4 . . ?
C12 C11 C10 105.3(2) . . ?
C12 C11 H11 127.4 . . ?
N8 C12 C11 107.1(2) . . ?
N8 C12 H12 126.4 . . ?
C11 C12 H12 126.4 . . ?
N14 N13 C7 117.92(18) . . ?
C17 N13 C7 130.62(17) . . ?
C17 N13 N14 111.37(18) . . ?
N13 N14 Fe1 114.43(14) . . ?
C15 N14 Fe1 139.53(15) . . ?
C15 N14 N13 104.67(18) . . ?
N14 C15 H15 124.2 . . ?
N14 C15 C16 111.6(2) . . ?
C16 C15 H15 124.2 . . ?
C15 C16 H16 127.4 . . ?
C17 C16 C15 105.2(2) . . ?
C17 C16 H16 127.4 . . ?
N13 C17 C16 107.24(19) . . ?
N13 C17 H17 126.4 . . ?
C16 C17 H17 126.4 . . ?
C5 N18 H18 115.5 . . ?
C19 N18 C5 129.1(2) . . ?
C19 N18 H18 115.5 . . ?
N18 C19 C21 113.6(2) . . ?
O20 C19 N18 123.7(2) . . ?
O20 C19 C21 122.7(2) . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O24 Cl22 O23 109.28(12) . . ?
O24 Cl22 O25 110.39(12) . . ?
O24 Cl22 O26 110.33(13) . . ?
O25 Cl22 O23 108.89(11) . . ?
O26 Cl22 O23 107.77(11) . . ?
O26 Cl22 O25 110.11(12) . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N28 C27 H27A 109.5 . . ?
N28 C27 H27B 109.5 . . ?
N28 C27 H27C 109.5 . . ?
O29 N28 C27 118.5(2) . . ?
O29 N28 O30 123.7(2) . . ?
O30 N28 C27 117.9(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N18 H18 O23 0.88 1.98 2.848(3) 169.8 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N2 C3 C4 -177.39(18) . . . . ?
Fe1 N2 C3 N8 3.0(3) . . . . ?
Fe1 N2 C7 C6 176.39(18) . . . . ?
Fe1 N2 C7 N13 -3.4(3) . . . . ?
Fe1 N9 C10 C11 -176.5(2) . . . . ?
Fe1 N14 C15 C16 -164.6(2) . . . . ?
N2 C3 C4 C5 0.8(4) . . . . ?
N2 C3 N8 N9 -1.3(3) . . . . ?
N2 C3 N8 C12 -179.7(2) . . . . ?
N2 C7 N13 N14 7.6(3) . . . . ?
N2 C7 N13 C17 -168.4(2) . . . . ?
C3 N2 C7 C6 0.0(3) . . . . ?
C3 N2 C7 N13 -179.76(19) . . . . ?
C3 C4 C5 C6 0.4(3) . . . . ?
C3 C4 C5 N18 -179.4(2) . . . . ?
C3 N8 N9 Fe1 -0.7(2) . . . . ?
C3 N8 N9 C10 -177.8(2) . . . . ?
C3 N8 C12 C11 177.8(2) . . . . ?
C4 C3 N8 N9 179.0(2) . . . . ?
C4 C3 N8 C12 0.7(4) . . . . ?
C4 C5 C6 C7 -1.2(3) . . . . ?
C4 C5 N18 C19 -179.5(2) . . . . ?
C5 C6 C7 N2 1.1(4) . . . . ?
C5 C6 C7 N13 -179.2(2) . . . . ?
C5 N18 C19 O20 3.7(4) . . . . ?
C5 N18 C19 C21 -177.1(2) . . . . ?
C6 C5 N18 C19 0.8(4) . . . . ?
C6 C7 N13 N14 -172.2(2) . . . . ?
C6 C7 N13 C17 11.8(4) . . . . ?
C7 N2 C3 C4 -1.0(3) . . . . ?
C7 N2 C3 N8 179.3(2) . . . . ?
C7 N13 N14 Fe1 -8.1(2) . . . . ?
C7 N13 N14 C15 -177.4(2) . . . . ?
C7 N13 C17 C16 176.9(2) . . . . ?
N8 C3 C4 C5 -179.5(2) . . . . ?
N8 N9 C10 C11 -0.7(3) . . . . ?
N9 N8 C12 C11 -0.6(3) . . . . ?
N9 C10 C11 C12 0.4(3) . . . . ?
C10 C11 C12 N8 0.1(3) . . . . ?
C12 N8 N9 Fe1 177.91(16) . . . . ?
C12 N8 N9 C10 0.8(3) . . . . ?
N13 N14 C15 C16 0.3(3) . . . . ?
N14 N13 C17 C16 0.8(3) . . . . ?
N14 C15 C16 C17 0.1(3) . . . . ?
C15 C16 C17 N13 -0.5(3) . . . . ?
C17 N13 N14 Fe1 168.61(16) . . . . ?
C17 N13 N14 C15 -0.7(3) . . . . ?
N18 C5 C6 C7 178.5(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: nitromethane/diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_80-etoh
_database_code_depnum_ccdc_archive 'CCDC 2078664'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2021-04-19 deposited with the CCDC.	2021-06-10 downloaded from the CCDC.
;
_audit_creation_date             2020-07-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis-[N-(2,6-di{pyrazol-1-yl}pyrid-4-yl)acetamide]iron(II)diperchlorate hemi-ethanol solvate'
_chemical_formula_moiety         'C26 H24 Fe N12 O2, 2(Cl O4), 0.5(C2 H6 O)'
_chemical_formula_sum            'C27 H27 Cl2 Fe N12 O10.50'
_chemical_formula_weight         814.35
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2123(7)
_cell_length_b                   10.9318(10)
_cell_length_c                   20.008(2)
_cell_angle_alpha                79.143(9)
_cell_angle_beta                 78.844(9)
_cell_angle_gamma                75.480(8)
_cell_volume                     1687.4(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6098
_cell_measurement_temperature    120(2)
_cell_measurement_theta_min      4.47
_cell_measurement_theta_max      73.41
_exptl_absorpt_coefficient_mu    5.712
_exptl_absorpt_correction_T_min  0.829
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             834
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13392
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.845
_diffrn_reflns_theta_min         4.224
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5519
_reflns_number_total             6407
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2015)'
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         6407
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0472
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0742P)²+0.9623P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1269
_refine_special_details          
;
 The asymmetric unit contains one complex cation and two ClO₄⁻ anions on
 general crystallographic sites, and half an ethanol molecule spanning the
 crystallographic inversion centre. One of the ClO₄⁻ ions is disordered
 over two equally occupied sites. The bond distance restraints that were 
 applied to the disordered anion are listed below. This anion accepts a 
 hydrogen bond from the solvent, and its disorder correlates with the 
 orientation of that solvent about its inversion centre.

 All non-H atoms except the disordered anion O atoms were refined 
 anisotropically, and H atoms were placed in calculated positions and 
 refined using a riding model.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl4A-O48A = Cl4A-O49A = Cl4A-O50A = Cl4A-O51A
 1.43461 with sigma of 0.02
 Cl4B-O48B = Cl4B-O49B = Cl4B-O50B = Cl4B-O51B
 1.43461 with sigma of 0.02
 O48A-O49A = O48A-O50A = O48A-O51A = O49A-O50A = O49A-O51A = O50A-O51A
 2.342718 with sigma of 0.02
 O48B-O49B = O48B-O50B = O48B-O51B = O49B-O50B = O49B-O51B = O50B-O51B
 2.342718 with sigma of 0.02
3. Others
 1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: Cl4A(0.5) O48A(0.5) O49A(0.5) O50A(0.5) O51A(0.5) Cl4B(0.5)
 O48B(0.5) O49B(0.5) O50B(0.5) O51B(0.5) C52(0.5) H52A(0.5) H52B(0.5) H52C(0.5)
 C53(0.5) H53A(0.5) H53B(0.5) O54(0.5) H54(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B)
4.b Me refined with riding coordinates:
 C52(H52A,H52B,H52C)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17),
 N18(H18), C24(H24), C26(H26), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36),
  C37(H37), N38(H38)
4.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C41(H41A,H41B,H41C)
4.e Idealised tetrahedral OH refined as rotating group:
 O54(H54)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.81712(5) 0.75062(4) 0.73894(2) 0.02035(13) Uani 1 1 d . . . . .
N2 N 0.7705(3) 0.7498(2) 0.63810(11) 0.0206(4) Uani 1 1 d . . . . .
C3 C 0.7260(3) 0.6506(2) 0.62272(13) 0.0210(5) Uani 1 1 d . . . . .
C4 C 0.6769(4) 0.6484(3) 0.56148(14) 0.0245(5) Uani 1 1 d . . . . .
H4 H 0.641802 0.576820 0.553252 0.029 Uiso 1 1 calc R U . . .
C5 C 0.6808(4) 0.7570(3) 0.51131(14) 0.0247(6) Uani 1 1 d . . . . .
C6 C 0.7281(4) 0.8626(3) 0.52553(14) 0.0243(6) Uani 1 1 d . . . . .
H6 H 0.729505 0.937628 0.492766 0.029 Uiso 1 1 calc R U . . .
C7 C 0.7726(3) 0.8516(2) 0.58976(13) 0.0207(5) Uani 1 1 d . . . . .
N8 N 0.7377(3) 0.5454(2) 0.67597(11) 0.0222(5) Uani 1 1 d . . . . .
N9 N 0.7856(3) 0.5579(2) 0.73594(11) 0.0215(5) Uani 1 1 d . . . . .
C10 C 0.7943(4) 0.4433(3) 0.77425(14) 0.0246(6) Uani 1 1 d . . . . .
H10 H 0.823755 0.422479 0.819306 0.030 Uiso 1 1 calc R U . . .
C11 C 0.7543(4) 0.3573(3) 0.73929(15) 0.0312(6) Uani 1 1 d . . . . .
H11 H 0.751478 0.270336 0.755562 0.037 Uiso 1 1 calc R U . . .
C12 C 0.7202(4) 0.4252(3) 0.67690(15) 0.0295(6) Uani 1 1 d . . . . .
H12 H 0.689982 0.393823 0.640915 0.035 Uiso 1 1 calc R U . . .
N13 N 0.8282(3) 0.9484(2) 0.61077(11) 0.0225(5) Uani 1 1 d . . . . .
N14 N 0.8688(3) 0.9278(2) 0.67582(11) 0.0241(5) Uani 1 1 d . . . . .
C15 C 0.9258(4) 1.0293(3) 0.67946(15) 0.0284(6) Uani 1 1 d . . . . .
H15 H 0.963390 1.042336 0.719050 0.034 Uiso 1 1 calc R U . . .
C16 C 0.9238(4) 1.1147(3) 0.61786(15) 0.0291(6) Uani 1 1 d . . . . .
H16 H 0.958812 1.193574 0.607853 0.035 Uiso 1 1 calc R U . . .
C17 C 0.8604(4) 1.0601(3) 0.57503(14) 0.0263(6) Uani 1 1 d . . . . .
H17 H 0.842628 1.094122 0.529036 0.032 Uiso 1 1 calc R U . . .
N18 N 0.6396(4) 0.7502(2) 0.44806(13) 0.0309(6) Uani 1 1 d . . . . .
H18 H 0.633541 0.674215 0.441531 0.037 Uiso 1 1 calc R U . . .
C19 C 0.6074(4) 0.8469(3) 0.39484(14) 0.0265(6) Uani 1 1 d . . . . .
O20 O 0.6140(3) 0.9558(2) 0.39595(11) 0.0400(6) Uani 1 1 d . . . . .
C21 C 0.5607(4) 0.8054(3) 0.33477(15) 0.0341(7) Uani 1 1 d . . . . .
H21A H 0.439322 0.804741 0.343630 0.051 Uiso 1 1 calc R U . . .
H21B H 0.628011 0.719464 0.328674 0.051 Uiso 1 1 calc R U . . .
H21C H 0.584455 0.865169 0.292908 0.051 Uiso 1 1 calc R U . . .
N22 N 0.7953(3) 0.7440(2) 0.84759(11) 0.0206(4) Uani 1 1 d . . . . .
C23 C 0.6479(3) 0.7901(2) 0.88549(14) 0.0207(5) Uani 1 1 d . . . . .
C24 C 0.6271(4) 0.7926(3) 0.95471(14) 0.0227(5) Uani 1 1 d . . . . .
H24 H 0.519777 0.827540 0.979506 0.027 Uiso 1 1 calc R U . . .
C25 C 0.7707(4) 0.7414(3) 0.98769(13) 0.0231(5) Uani 1 1 d . . . . .
C26 C 0.9273(4) 0.6919(3) 0.94948(14) 0.0235(5) Uani 1 1 d . . . . .
H26 H 1.026431 0.655916 0.970420 0.028 Uiso 1 1 calc R U . . .
C27 C 0.9300(4) 0.6980(2) 0.87999(13) 0.0219(5) Uani 1 1 d . . . . .
N28 N 0.5127(3) 0.8361(2) 0.84677(11) 0.0227(5) Uani 1 1 d . . . . .
N29 N 0.5483(3) 0.8325(2) 0.77735(11) 0.0237(5) Uani 1 1 d . . . . .
C30 C 0.3997(4) 0.8815(3) 0.75484(15) 0.0287(6) Uani 1 1 d . . . . .
H30 H 0.383729 0.890683 0.708237 0.034 Uiso 1 1 calc R U . . .
C31 C 0.2700(4) 0.9177(3) 0.80889(16) 0.0310(6) Uani 1 1 d . . . . .
H31 H 0.153548 0.955384 0.806036 0.037 Uiso 1 1 calc R U . . .
C32 C 0.3465(4) 0.8874(3) 0.86650(15) 0.0265(6) Uani 1 1 d . . . . .
H32 H 0.292823 0.900001 0.911962 0.032 Uiso 1 1 calc R U . . .
N33 N 1.0800(3) 0.6575(2) 0.83504(11) 0.0219(5) Uani 1 1 d . . . . .
N34 N 1.0743(3) 0.6753(2) 0.76581(11) 0.0252(5) Uani 1 1 d . . . . .
C35 C 1.2316(4) 0.6272(3) 0.73738(15) 0.0311(6) Uani 1 1 d . . . . .
H35 H 1.267061 0.626146 0.689352 0.037 Uiso 1 1 calc R U . . .
C36 C 1.3391(4) 0.5781(3) 0.78739(16) 0.0329(7) Uani 1 1 d . . . . .
H36 H 1.456650 0.538100 0.780040 0.040 Uiso 1 1 calc R U . . .
C37 C 1.2391(4) 0.5998(3) 0.84880(15) 0.0281(6) Uani 1 1 d . . . . .
H37 H 1.274211 0.578438 0.892875 0.034 Uiso 1 1 calc R U . . .
N38 N 0.7486(3) 0.7470(2) 1.05779(11) 0.0266(5) Uani 1 1 d . . . . .
H38 H 0.652229 0.794855 1.075057 0.032 Uiso 1 1 calc R U . . .
C39 C 0.8595(4) 0.6865(3) 1.10333(14) 0.0267(6) Uani 1 1 d . . . . .
O40 O 0.9910(3) 0.6101(2) 1.08811(10) 0.0311(5) Uani 1 1 d . . . . .
C41 C 0.8011(4) 0.7229(3) 1.17417(15) 0.0376(8) Uani 1 1 d . . . . .
H41A H 0.823990 0.646605 1.208603 0.056 Uiso 1 1 calc R U . . .
H41B H 0.678577 0.760669 1.179838 0.056 Uiso 1 1 calc R U . . .
H41C H 0.862450 0.785135 1.180333 0.056 Uiso 1 1 calc R U . . .
Cl42 Cl 0.77538(9) 0.37595(7) 0.45774(4) 0.03047(17) Uani 1 1 d . . . . .
O43 O 0.8099(4) 0.2618(2) 0.42734(13) 0.0476(7) Uani 1 1 d . . . . .
O44 O 0.6808(4) 0.4791(2) 0.41495(13) 0.0500(7) Uani 1 1 d . . . . .
O45 O 0.9281(4) 0.4048(4) 0.4649(2) 0.0803(12) Uani 1 1 d . . . . .
O46 O 0.6721(4) 0.3595(2) 0.52421(12) 0.0460(6) Uani 1 1 d . . . . .
Cl4A Cl 0.2546(8) 0.9031(6) 1.1003(3) 0.050(2) Uani 0.5 1 d D . P A 1
O48A O 0.2514(9) 0.7727(6) 1.1077(3) 0.0522(14) Uiso 0.5 1 d D . P A 1
O49A O 0.2371(9) 0.9591(6) 1.0296(3) 0.035(2) Uiso 0.5 1 d D . P A 1
O50A O 0.1329(10) 0.9657(8) 1.1489(4) 0.064(3) Uiso 0.5 1 d D . P A 1
O51A O 0.4250(6) 0.9079(5) 1.1146(2) 0.0322(11) Uiso 0.5 1 d D . P A 1
Cl4B Cl 0.2507(4) 0.9059(4) 1.1000(2) 0.0187(11) Uani 0.5 1 d D . P B 2
O48B O 0.1715(7) 0.7975(5) 1.1102(3) 0.0402(11) Uiso 0.5 1 d D . P B 2
O49B O 0.2709(9) 0.9632(6) 1.0294(3) 0.0301(19) Uiso 0.5 1 d D . P B 2
O50B O 0.1386(6) 1.0005(5) 1.1399(3) 0.0280(12) Uiso 0.5 1 d D . P B 2
O51B O 0.4077(7) 0.8657(6) 1.1232(3) 0.0461(15) Uiso 0.5 1 d D . P B 2
C52 C 0.573(4) 0.472(3) 0.9701(15) 0.032(4) Uani 0.5 1 d . . P C -1
H52A H 0.658573 0.406546 0.992568 0.047 Uiso 0.5 1 calc R U P C -1
H52B H 0.511184 0.431681 0.946469 0.047 Uiso 0.5 1 calc R U P C -1
H52C H 0.628908 0.532301 0.936596 0.047 Uiso 0.5 1 calc R U P C -1
C53 C 0.450(5) 0.542(3) 1.0231(18) 0.045(7) Uani 0.5 1 d . . P C -1
H53A H 0.395210 0.481387 1.057429 0.055 Uiso 0.5 1 calc R U P C -1
H53B H 0.513043 0.582099 1.047546 0.055 Uiso 0.5 1 calc R U P C -1
O54 O 0.3291(6) 0.6345(5) 0.9941(2) 0.0394(11) Uani 0.5 1 d . . P C -1
H54 H 0.252565 0.663610 1.025129 0.047 Uiso 0.5 1 calc R U P C -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.127(2) . ?
Fe1 N9 2.199(2) . ?
Fe1 N14 2.193(2) . ?
Fe1 N22 2.135(2) . ?
Fe1 N29 2.208(2) . ?
Fe1 N34 2.197(2) . ?
N2 C3 1.331(4) . ?
N2 C7 1.331(3) . ?
C3 C4 1.368(4) . ?
C3 N8 1.410(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.406(4) . ?
C5 C6 1.398(4) . ?
C5 N18 1.391(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.379(4) . ?
C7 N13 1.411(4) . ?
N8 N9 1.373(3) . ?
N8 C12 1.354(4) . ?
N9 C10 1.333(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.404(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.367(4) . ?
C12 H12 0.9500 . ?
N13 N14 1.370(3) . ?
N13 C17 1.353(4) . ?
N14 C15 1.326(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.399(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.373(4) . ?
C17 H17 0.9500 . ?
N18 H18 0.8800 . ?
N18 C19 1.366(4) . ?
C19 O20 1.210(4) . ?
C19 C21 1.506(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
N22 C23 1.333(3) . ?
N22 C27 1.331(4) . ?
C23 C24 1.367(4) . ?
C23 N28 1.412(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.403(4) . ?
C25 C26 1.399(4) . ?
C25 N38 1.390(3) . ?
C26 H26 0.9500 . ?
C26 C27 1.376(4) . ?
C27 N33 1.404(3) . ?
N28 N29 1.369(3) . ?
N28 C32 1.351(4) . ?
N29 C30 1.331(4) . ?
C30 H30 0.9500 . ?
C30 C31 1.402(4) . ?
C31 H31 0.9500 . ?
C31 C32 1.366(4) . ?
C32 H32 0.9500 . ?
N33 N34 1.370(3) . ?
N33 C37 1.357(4) . ?
N34 C35 1.325(4) . ?
C35 H35 0.9500 . ?
C35 C36 1.404(4) . ?
C36 H36 0.9500 . ?
C36 C37 1.364(4) . ?
C37 H37 0.9500 . ?
N38 H38 0.8800 . ?
N38 C39 1.374(4) . ?
C39 O40 1.213(4) . ?
C39 C41 1.500(4) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
Cl42 O43 1.431(2) . ?
Cl42 O44 1.436(3) . ?
Cl42 O45 1.406(3) . ?
Cl42 O46 1.439(3) . ?
Cl4A O48A 1.411(8) . ?
Cl4A O49A 1.452(8) . ?
Cl4A O50A 1.394(9) . ?
Cl4A O51A 1.496(8) . ?
Cl4B O48B 1.454(6) . ?
Cl4B O49B 1.430(6) . ?
Cl4B O50B 1.450(6) . ?
Cl4B O51B 1.392(6) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C52 C53 1.494(13) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53 O54 1.36(4) . ?
O54 H54 0.8400 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N9 73.25(8) . . ?
N2 Fe1 N14 72.86(9) . . ?
N2 Fe1 N22 164.47(9) . . ?
N2 Fe1 N29 94.03(9) . . ?
N2 Fe1 N34 120.39(9) . . ?
N9 Fe1 N29 96.85(9) . . ?
N14 Fe1 N9 144.51(8) . . ?
N14 Fe1 N29 95.71(9) . . ?
N14 Fe1 N34 96.18(9) . . ?
N22 Fe1 N9 99.82(8) . . ?
N22 Fe1 N14 115.60(9) . . ?
N22 Fe1 N29 72.69(8) . . ?
N22 Fe1 N34 72.98(8) . . ?
N34 Fe1 N9 91.93(9) . . ?
N34 Fe1 N29 145.54(8) . . ?
C3 N2 Fe1 120.89(17) . . ?
C3 N2 C7 117.6(2) . . ?
C7 N2 Fe1 121.32(18) . . ?
N2 C3 C4 124.3(3) . . ?
N2 C3 N8 112.9(2) . . ?
C4 C3 N8 122.8(3) . . ?
C3 C4 H4 121.6 . . ?
C3 C4 C5 116.9(3) . . ?
C5 C4 H4 121.6 . . ?
C6 C5 C4 120.4(2) . . ?
N18 C5 C4 116.1(3) . . ?
N18 C5 C6 123.6(3) . . ?
C5 C6 H6 121.9 . . ?
C7 C6 C5 116.3(2) . . ?
C7 C6 H6 121.9 . . ?
N2 C7 C6 124.6(3) . . ?
N2 C7 N13 112.6(2) . . ?
C6 C7 N13 122.8(2) . . ?
N9 N8 C3 118.4(2) . . ?
C12 N8 C3 130.1(2) . . ?
C12 N8 N9 111.3(2) . . ?
N8 N9 Fe1 113.84(16) . . ?
C10 N9 Fe1 141.35(19) . . ?
C10 N9 N8 104.8(2) . . ?
N9 C10 H10 124.4 . . ?
N9 C10 C11 111.1(2) . . ?
C11 C10 H10 124.4 . . ?
C10 C11 H11 127.2 . . ?
C12 C11 C10 105.5(3) . . ?
C12 C11 H11 127.2 . . ?
N8 C12 C11 107.2(3) . . ?
N8 C12 H12 126.4 . . ?
C11 C12 H12 126.4 . . ?
N14 N13 C7 118.0(2) . . ?
C17 N13 C7 130.3(2) . . ?
C17 N13 N14 111.5(2) . . ?
N13 N14 Fe1 114.52(17) . . ?
C15 N14 Fe1 140.83(19) . . ?
C15 N14 N13 104.6(2) . . ?
N14 C15 H15 124.1 . . ?
N14 C15 C16 111.7(3) . . ?
C16 C15 H15 124.1 . . ?
C15 C16 H16 127.4 . . ?
C17 C16 C15 105.1(3) . . ?
C17 C16 H16 127.4 . . ?
N13 C17 C16 106.9(2) . . ?
N13 C17 H17 126.5 . . ?
C16 C17 H17 126.5 . . ?
C5 N18 H18 116.0 . . ?
C19 N18 C5 128.1(3) . . ?
C19 N18 H18 116.0 . . ?
N18 C19 C21 113.6(3) . . ?
O20 C19 N18 123.4(3) . . ?
O20 C19 C21 123.0(3) . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 N22 Fe1 121.56(17) . . ?
C27 N22 Fe1 121.31(18) . . ?
C27 N22 C23 117.1(2) . . ?
N22 C23 C24 124.3(2) . . ?
N22 C23 N28 112.9(2) . . ?
C24 C23 N28 122.7(2) . . ?
C23 C24 H24 121.3 . . ?
C23 C24 C25 117.3(2) . . ?
C25 C24 H24 121.3 . . ?
C26 C25 C24 119.9(2) . . ?
N38 C25 C24 116.7(2) . . ?
N38 C25 C26 123.4(2) . . ?
C25 C26 H26 121.8 . . ?
C27 C26 C25 116.4(2) . . ?
C27 C26 H26 121.8 . . ?
N22 C27 C26 125.0(3) . . ?
N22 C27 N33 112.6(2) . . ?
C26 C27 N33 122.4(2) . . ?
N29 N28 C23 118.0(2) . . ?
C32 N28 C23 130.5(2) . . ?
C32 N28 N29 111.4(2) . . ?
N28 N29 Fe1 114.71(16) . . ?
C30 N29 Fe1 140.52(19) . . ?
C30 N29 N28 104.8(2) . . ?
N29 C30 H30 124.4 . . ?
N29 C30 C31 111.2(2) . . ?
C31 C30 H30 124.4 . . ?
C30 C31 H31 127.3 . . ?
C32 C31 C30 105.4(3) . . ?
C32 C31 H31 127.3 . . ?
N28 C32 C31 107.2(3) . . ?
N28 C32 H32 126.4 . . ?
C31 C32 H32 126.4 . . ?
N34 N33 C27 118.8(2) . . ?
C37 N33 C27 130.0(2) . . ?
C37 N33 N34 111.2(2) . . ?
N33 N34 Fe1 114.06(17) . . ?
C35 N34 Fe1 140.51(19) . . ?
C35 N34 N33 105.0(2) . . ?
N34 C35 H35 124.4 . . ?
N34 C35 C36 111.3(3) . . ?
C36 C35 H35 124.4 . . ?
C35 C36 H36 127.3 . . ?
C37 C36 C35 105.5(3) . . ?
C37 C36 H36 127.3 . . ?
N33 C37 C36 107.1(2) . . ?
N33 C37 H37 126.5 . . ?
C36 C37 H37 126.5 . . ?
C25 N38 H38 116.2 . . ?
C39 N38 C25 127.7(2) . . ?
C39 N38 H38 116.2 . . ?
N38 C39 C41 113.4(2) . . ?
O40 C39 N38 123.5(2) . . ?
O40 C39 C41 123.1(3) . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O43 Cl42 O44 108.94(15) . . ?
O43 Cl42 O46 109.64(16) . . ?
O44 Cl42 O46 107.90(16) . . ?
O45 Cl42 O43 110.47(19) . . ?
O45 Cl42 O44 110.2(2) . . ?
O45 Cl42 O46 109.6(2) . . ?
O48A Cl4A O49A 107.9(5) . . ?
O48A Cl4A O51A 106.7(5) . . ?
O49A Cl4A O51A 109.7(5) . . ?
O50A Cl4A O48A 111.8(6) . . ?
O50A Cl4A O49A 113.7(6) . . ?
O50A Cl4A O51A 106.8(5) . . ?
O49B Cl4B O48B 111.6(4) . . ?
O49B Cl4B O50B 107.9(4) . . ?
O50B Cl4B O48B 107.5(4) . . ?
O51B Cl4B O48B 109.1(4) . . ?
O51B Cl4B O49B 110.5(5) . . ?
O51B Cl4B O50B 110.2(4) . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C53 C52 H52A 109.5 . . ?
C53 C52 H52B 109.5 . . ?
C53 C52 H52C 109.5 . . ?
C52 C53 H53A 109.4 . . ?
C52 C53 H53B 109.4 . . ?
H53A C53 H53B 108.0 . . ?
O54 C53 C52 111.3(16) . . ?
O54 C53 H53A 109.4 . . ?
O54 C53 H53B 109.4 . . ?
C53 O54 H54 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N18 H18 O44 0.88 2.22 3.080(4) 166.8 . yes
N38 H38 O51A 0.88 2.07 2.948(5) 179.4 . yes
N38 H38 O51B 0.88 2.08 2.939(6) 166.1 . yes
O54 H54 O48A 0.84 2.21 2.848(8) 132.5 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N2 C3 C4 172.9(2) . . . . ?
Fe1 N2 C3 N8 -8.2(3) . . . . ?
Fe1 N2 C7 C6 -173.6(2) . . . . ?
Fe1 N2 C7 N13 7.2(3) . . . . ?
Fe1 N9 C10 C11 179.1(2) . . . . ?
Fe1 N14 C15 C16 -178.4(2) . . . . ?
Fe1 N22 C23 C24 -177.7(2) . . . . ?
Fe1 N22 C23 N28 2.7(3) . . . . ?
Fe1 N22 C27 C26 179.1(2) . . . . ?
Fe1 N22 C27 N33 0.4(3) . . . . ?
Fe1 N29 C30 C31 179.9(2) . . . . ?
Fe1 N34 C35 C36 -171.0(2) . . . . ?
N2 C3 C4 C5 2.5(4) . . . . ?
N2 C3 N8 N9 2.2(3) . . . . ?
N2 C3 N8 C12 -172.6(3) . . . . ?
N2 C7 N13 N14 -1.0(3) . . . . ?
N2 C7 N13 C17 174.0(3) . . . . ?
C3 N2 C7 C6 1.6(4) . . . . ?
C3 N2 C7 N13 -177.5(2) . . . . ?
C3 C4 C5 C6 -1.9(4) . . . . ?
C3 C4 C5 N18 176.5(3) . . . . ?
C3 N8 N9 Fe1 4.3(3) . . . . ?
C3 N8 N9 C10 -176.7(2) . . . . ?
C3 N8 C12 C11 176.1(3) . . . . ?
C4 C3 N8 N9 -179.0(2) . . . . ?
C4 C3 N8 C12 6.3(5) . . . . ?
C4 C5 C6 C7 1.3(4) . . . . ?
C4 C5 N18 C19 168.7(3) . . . . ?
C5 C6 C7 N2 -1.1(4) . . . . ?
C5 C6 C7 N13 178.0(2) . . . . ?
C5 N18 C19 O20 1.3(5) . . . . ?
C5 N18 C19 C21 -178.0(3) . . . . ?
C6 C5 N18 C19 -12.9(5) . . . . ?
C6 C7 N13 N14 179.9(2) . . . . ?
C6 C7 N13 C17 -5.1(4) . . . . ?
C7 N2 C3 C4 -2.4(4) . . . . ?
C7 N2 C3 N8 176.5(2) . . . . ?
C7 N13 N14 Fe1 -5.1(3) . . . . ?
C7 N13 N14 C15 176.3(2) . . . . ?
C7 N13 C17 C16 -175.4(3) . . . . ?
N8 C3 C4 C5 -176.2(2) . . . . ?
N8 N9 C10 C11 0.6(3) . . . . ?
N9 N8 C12 C11 1.1(3) . . . . ?
N9 C10 C11 C12 0.1(4) . . . . ?
C10 C11 C12 N8 -0.7(4) . . . . ?
C12 N8 N9 Fe1 179.97(19) . . . . ?
C12 N8 N9 C10 -1.0(3) . . . . ?
N13 N14 C15 C16 -0.4(3) . . . . ?
N14 N13 C17 C16 -0.2(3) . . . . ?
N14 C15 C16 C17 0.3(4) . . . . ?
C15 C16 C17 N13 -0.1(3) . . . . ?
C17 N13 N14 Fe1 178.97(18) . . . . ?
C17 N13 N14 C15 0.3(3) . . . . ?
N18 C5 C6 C7 -177.1(3) . . . . ?
N22 C23 C24 C25 -0.9(4) . . . . ?
N22 C23 N28 N29 -2.2(3) . . . . ?
N22 C23 N28 C32 178.9(3) . . . . ?
N22 C27 N33 N34 3.5(4) . . . . ?
N22 C27 N33 C37 -176.1(3) . . . . ?
C23 N22 C27 C26 1.6(4) . . . . ?
C23 N22 C27 N33 -177.2(2) . . . . ?
C23 C24 C25 C26 0.7(4) . . . . ?
C23 C24 C25 N38 178.7(2) . . . . ?
C23 N28 N29 Fe1 0.8(3) . . . . ?
C23 N28 N29 C30 -179.7(2) . . . . ?
C23 N28 C32 C31 179.3(3) . . . . ?
C24 C23 N28 N29 178.2(2) . . . . ?
C24 C23 N28 C32 -0.7(5) . . . . ?
C24 C25 C26 C27 0.6(4) . . . . ?
C24 C25 N38 C39 168.7(3) . . . . ?
C25 C26 C27 N22 -1.8(4) . . . . ?
C25 C26 C27 N33 176.9(3) . . . . ?
C25 N38 C39 O40 -5.7(5) . . . . ?
C25 N38 C39 C41 175.0(3) . . . . ?
C26 C25 N38 C39 -13.3(5) . . . . ?
C26 C27 N33 N34 -175.3(3) . . . . ?
C26 C27 N33 C37 5.1(5) . . . . ?
C27 N22 C23 C24 -0.2(4) . . . . ?
C27 N22 C23 N28 -179.7(2) . . . . ?
C27 N33 N34 Fe1 -5.4(3) . . . . ?
C27 N33 N34 C35 -179.3(3) . . . . ?
C27 N33 C37 C36 178.9(3) . . . . ?
N28 C23 C24 C25 178.6(2) . . . . ?
N28 N29 C30 C31 0.7(3) . . . . ?
N29 N28 C32 C31 0.4(3) . . . . ?
N29 C30 C31 C32 -0.5(4) . . . . ?
C30 C31 C32 N28 0.0(3) . . . . ?
C32 N28 N29 Fe1 179.88(19) . . . . ?
C32 N28 N29 C30 -0.7(3) . . . . ?
N33 N34 C35 C36 0.2(4) . . . . ?
N34 N33 C37 C36 -0.6(3) . . . . ?
N34 C35 C36 C37 -0.6(4) . . . . ?
C35 C36 C37 N33 0.7(4) . . . . ?
C37 N33 N34 Fe1 174.17(19) . . . . ?
C37 N33 N34 C35 0.3(3) . . . . ?
N38 C25 C26 C27 -177.3(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.452
_oxdiff_exptl_absorpt_empirical_full_min 0.802
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: ethanol/diethyl ether'
