# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_mh453rt
_database_code_depnum_ccdc_archive 'CCDC 2261786'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2023-08-21 deposited with the CCDC.	2023-08-30 downloaded from the CCDC.
;
_audit_creation_date             2023-08-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis[2,6-di(pyrazol-1-yl)pyridine]iron(II) bis[2,6-di(pyrazol-1-yl)pyridine]-zinc(II) ditetrafluoroborate 0.54:0.46 solid solution'
_chemical_formula_moiety         'C22 H18 Fe0.54 N10 Zn0.46, 2(B F4)'
_chemical_formula_sum            'C22 H18 B2 F8 Fe0.54 N10 Zn0.46'
_chemical_formula_weight         656.31
_chemical_absolute_configuration ab
_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 0.0019 0.0015 '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 0.0004 0.0006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0124 0.0097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.2961 0.8007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0037 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2335 1.3591 '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           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   8.5002(1)
_cell_length_b                   8.5263(1)
_cell_length_c                   19.0498(1)
_cell_angle_alpha                90
_cell_angle_beta                 95.740(1)
_cell_angle_gamma                90
_cell_volume                     1373.72(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9064
_cell_measurement_temperature    300.15
_cell_measurement_theta_max      31.98
_cell_measurement_theta_min      1.04
_exptl_absorpt_coefficient_mu    0.735
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.948
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
DIALS 3.12.1-2-g1c07bc2b3-release
Scaling & analysis of unmerged intensities, absorption correction using 
spherical harmonics
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       lath
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_diffrn_reflns_av_R_equivalents  0.0857
_diffrn_reflns_av_unetI/netI     0.0840
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14617
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        24.620
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         1.041
_diffrn_ambient_temperature      300.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_measurement_device       'Fixed χ 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.948
_reflns_Friedel_fraction_max     0.943
_reflns_number_gt                4149
_reflns_number_total             5179
_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       'XIA2 0.4.0.438-g4431aaa (Winter, 2010)'
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction        'XIA2 0.4.0.438-g4431aaa (Winter, 2010)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 
;
 Flack x determined using 1355 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(15)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         5179
_refine_ls_number_restraints     61
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0467
_refine_ls_restrained_S_all      1.102
_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)+(0.0756P)²+0.1121P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1300
_refine_ls_wR_factor_ref         0.1368
_refine_special_details          
;
 Unlike the low temperature structure, separate partial [Fe(bpp)₂]2+
 and [Zn(bpp)₂]2+ molecule sites could not be refined at this temperature.
 Hence, the organic ligand framework was modelled as crystallographically
 ordered. Attempts to distinguish Fe and Zn half-atoms in the Fourier map
 were also unproductive, so a mixed Fe~0.54~/Zn~0.46~ metal site was 
 refined with the same atomic coordinates, but independently refined 
 displacement parameters. The metal occupancies from the 100 K structure
 were used, since these could be accurately refined.

 The F atoms of both anions are also disordered, over three sites with a
 0.50:0.25:0.25 occupancy ratio. These were treated with the refined
 distance restraints listed below. An EADP thermal parameter constraint
 between the two partial metal atoms was also required to make the
 refinement converge.

 All crystallographically ordered non-H atoms plus the partial metal sites 
 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
2. Restrained distances
 B34-F35A = B34-F36A = B34-F37A = B34-F38A
 1.38873 with sigma of 0.02
 B34-F35B = B34-F36B = B34-F37B = B34-F38B
 1.38873 with sigma of 0.02
 B34-F35C = B34-F36C = B34-F37C = B34-F38C
 1.38873 with sigma of 0.02
 B39-F40A = B39-F41A = B39-F42A = B39-F43A
 1.38873 with sigma of 0.02
 B39-F40B = B39-F41B = B39-F42B = B39-F43B
 1.38873 with sigma of 0.02
 B39-F40C = B39-F41C = B39-F42C = B39-F43C
 1.38873 with sigma of 0.02
 F35A-F36A = F35A-F37A = F35A-F38A = F36A-F37A = F36A-F38A = F37A-F38A
 2.267796 with sigma of 0.02
 F35B-F36B = F35B-F37B = F35B-F38B = F36B-F37B = F36B-F38B = F37B-F38B
 2.267796 with sigma of 0.02
 F35C-F36C = F35C-F37C = F35C-F38C = F36C-F37C = F36C-F38C = F37C-F38C
 2.267796 with sigma of 0.02
 F40A-F41A = F40A-F42A = F40A-F43A = F41A-F42A = F41A-F43A = F42A-F43A
 2.267796 with sigma of 0.02
 F40B-F41B = F40B-F42B = F40B-F43B = F41B-F42B = F41B-F43B = F42B-F43B
 2.267796 with sigma of 0.02
 F40C-F41C = F40C-F42C = F40C-F43C = F41C-F42C = F41C-F43C = F42C-F43C
 2.267796 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Fe1) = Uanis(Zn1)
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)
 X(Fe1)=X(Zn1)=FVAR(2)
 Y(Fe1)=Y(Zn1)=FVAR(3)
 Z(Fe1)=Z(Zn1)=FVAR(4)
 Fixed Sof: Fe1(0.54) Zn1(0.46) F35A(0.5) F36A(0.5) F37A(0.5) F38A(0.5)
 F35B(0.25) F36B(0.25) F37B(0.25) F38B(0.25) F35C(0.25) F36C(0.25) F37C(0.25)
 F38C(0.25) F40A(0.5) F41A(0.5) F42A(0.5) F43A(0.5) F40B(0.25) F41B(0.25)
 F42B(0.25) F43B(0.25) F40C(0.25) F41C(0.25) F42C(0.25) F43C(0.25)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16),
 C17(H17), C20(H20), C21(H21), C22(H22), C26(H26), C27(H27), C28(H28), C31(H31),
  C32(H32), C33(H33)
;
_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 0.26168(7) 0.18634(12) 0.25242(3) 0.0580(2) Uani 0.54 1 d . . P A 1
Zn1 Zn 0.26168(7) 0.18634(12) 0.25242(3) 0.0580(2) Uani 0.46 1 d . . P A 2
N2 N 0.2781(4) 0.1870(7) 0.3638(2) 0.0531(8) Uani 1 1 d . . . . .
C3 C 0.4054(6) 0.1339(6) 0.4022(3) 0.0577(11) Uani 1 1 d . . . . .
C4 C 0.4184(8) 0.1265(8) 0.4748(3) 0.0730(15) Uani 1 1 d . . . . .
H4 H 0.508577 0.086963 0.500433 0.088 Uiso 1 1 calc R U . . .
C5 C 0.2928(8) 0.1799(10) 0.5076(3) 0.0794(16) Uani 1 1 d . . . . .
H5 H 0.298220 0.177504 0.556608 0.095 Uiso 1 1 calc R U . . .
C6 C 0.1586(8) 0.2371(8) 0.4697(3) 0.0755(18) Uani 1 1 d . . . . .
H6 H 0.072679 0.272419 0.491931 0.091 Uiso 1 1 calc R U . . .
C7 C 0.1575(7) 0.2395(6) 0.3972(3) 0.0596(12) Uani 1 1 d . . . . .
N8 N 0.5247(5) 0.0857(5) 0.3600(2) 0.0576(10) Uani 1 1 d . . . . .
N9 N 0.4974(5) 0.0954(6) 0.2887(2) 0.0600(10) Uani 1 1 d . . . . .
C10 C 0.6289(7) 0.0447(7) 0.2644(4) 0.0721(16) Uani 1 1 d . . . . .
H10 H 0.645173 0.041058 0.216876 0.087 Uiso 1 1 calc R U . . .
C11 C 0.7400(7) -0.0027(8) 0.3192(4) 0.0824(19) Uani 1 1 d . . . . .
H11 H 0.839623 -0.044919 0.315184 0.099 Uiso 1 1 calc R U . . .
C12 C 0.6721(7) 0.0259(7) 0.3798(4) 0.0741(17) Uani 1 1 d . . . . .
H12 H 0.717097 0.008247 0.425607 0.089 Uiso 1 1 calc R U . . .
N13 N 0.0312(5) 0.2963(6) 0.3511(3) 0.0631(11) Uani 1 1 d . . . . .
N14 N 0.0390(5) 0.2804(6) 0.2804(3) 0.0667(12) Uani 1 1 d . . . . .
C15 C -0.0895(7) 0.3518(8) 0.2512(4) 0.0801(17) Uani 1 1 d . . . . .
H15 H -0.116256 0.360970 0.202819 0.096 Uiso 1 1 calc R U . . .
C16 C -0.1777(8) 0.4102(10) 0.3014(5) 0.096(2) Uani 1 1 d . . . . .
H16 H -0.273365 0.463316 0.293510 0.115 Uiso 1 1 calc R U . . .
C17 C -0.0984(8) 0.3757(8) 0.3655(5) 0.084(2) Uani 1 1 d . . . . .
H17 H -0.127897 0.401709 0.409759 0.101 Uiso 1 1 calc R U . . .
N18 N 0.2648(4) 0.2044(7) 0.1418(2) 0.0555(10) Uani 1 1 d . . . . .
C19 C 0.2129(6) 0.0885(7) 0.0994(3) 0.0556(11) Uani 1 1 d . . . . .
C20 C 0.2136(8) 0.0943(8) 0.0274(3) 0.0720(15) Uani 1 1 d . . . . .
H20 H 0.177580 0.011014 -0.001349 0.086 Uiso 1 1 calc R U . . .
C21 C 0.2710(8) 0.2317(9) -0.0002(3) 0.080(2) Uani 1 1 d . . . . .
H21 H 0.273012 0.240734 -0.048768 0.096 Uiso 1 1 calc R U . . .
C22 C 0.3240(7) 0.3526(8) 0.0418(3) 0.0692(15) Uani 1 1 d . . . . .
H22 H 0.362775 0.443648 0.022957 0.083 Uiso 1 1 calc R U . . .
C23 C 0.3185(6) 0.3362(7) 0.1131(3) 0.0575(12) Uani 1 1 d . . . . .
N24 N 0.1555(5) -0.0396(5) 0.1365(2) 0.0579(10) Uani 1 1 d . . . . .
N25 N 0.1623(5) -0.0323(6) 0.2083(2) 0.0611(10) Uani 1 1 d . . . . .
C26 C 0.0948(7) -0.1637(8) 0.2266(4) 0.0707(15) Uani 1 1 d . . . . .
H26 H 0.082618 -0.191912 0.272871 0.085 Uiso 1 1 calc R U . . .
C27 C 0.0445(8) -0.2539(9) 0.1685(4) 0.0832(18) Uani 1 1 d . . . . .
H27 H -0.005672 -0.350867 0.168239 0.100 Uiso 1 1 calc R U . . .
C28 C 0.0835(7) -0.1720(9) 0.1121(4) 0.0768(16) Uani 1 1 d . . . . .
H28 H 0.064197 -0.201659 0.065003 0.092 Uiso 1 1 calc R U . . .
N29 N 0.3686(5) 0.4494(6) 0.1641(3) 0.0653(12) Uani 1 1 d . . . . .
N30 N 0.3515(6) 0.4214(6) 0.2327(3) 0.0663(12) Uani 1 1 d . . . . .
C31 C 0.4043(8) 0.5526(9) 0.2667(4) 0.0813(19) Uani 1 1 d . . . . .
H31 H 0.405309 0.568488 0.315000 0.098 Uiso 1 1 calc R U . . .
C32 C 0.4562(8) 0.6592(8) 0.2206(5) 0.095(2) Uani 1 1 d . . . . .
H32 H 0.498495 0.757684 0.231845 0.113 Uiso 1 1 calc R U . . .
C33 C 0.4340(8) 0.5936(8) 0.1549(5) 0.089(2) Uani 1 1 d . . . . .
H33 H 0.458264 0.637765 0.112671 0.107 Uiso 1 1 calc R U . . .
B34 B 0.2039(9) 0.7417(9) 0.4229(4) 0.0741(18) Uani 1 1 d D . . . .
F35A F 0.3218(14) 0.7948(15) 0.3864(7) 0.076(3) Uiso 0.5 1 d D . P B 1
F36A F 0.2499(12) 0.7987(12) 0.4960(5) 0.079(3) Uiso 0.5 1 d D . P B 1
F37A F 0.1980(13) 0.5889(11) 0.4378(6) 0.104(3) Uiso 0.5 1 d D . P B 1
F38A F 0.0614(13) 0.8032(17) 0.4002(6) 0.106(3) Uiso 0.5 1 d D . P B 1
F35B F 0.281(2) 0.823(2) 0.3746(10) 0.086(7) Uiso 0.25 1 d D . P B 2
F36B F 0.0427(15) 0.729(2) 0.3872(8) 0.078(4) Uiso 0.25 1 d D . P B 2
F37B F 0.199(3) 0.815(2) 0.4843(9) 0.090(6) Uiso 0.25 1 d D . P B 2
F38B F 0.2481(16) 0.5782(13) 0.4209(7) 0.058(3) Uiso 0.25 1 d D . P B 2
F35C F 0.3522(18) 0.775(2) 0.4012(10) 0.072(6) Uiso 0.25 1 d D . P B 3
F36C F 0.101(2) 0.871(2) 0.4065(10) 0.099(6) Uiso 0.25 1 d D . P B 3
F37C F 0.209(2) 0.719(2) 0.4918(7) 0.096(5) Uiso 0.25 1 d D . P B 3
F38C F 0.141(3) 0.614(3) 0.3832(13) 0.157(10) Uiso 0.25 1 d D . P B 3
B39 B 0.2620(9) 0.7203(10) -0.0736(4) 0.088(2) Uani 1 1 d D . . . .
F40A F 0.3408(14) 0.7426(14) 0.0008(5) 0.082(3) Uiso 0.5 1 d D . P C 1
F41A F 0.3222(13) 0.8456(12) -0.1069(5) 0.078(2) Uiso 0.5 1 d D . P C 1
F42A F 0.1129(11) 0.7265(15) -0.0655(6) 0.111(3) Uiso 0.5 1 d D . P C 1
F43A F 0.315(2) 0.5780(15) -0.0967(7) 0.130(4) Uiso 0.5 1 d D . P C 1
F40B F 0.124(2) 0.651(3) -0.1025(13) 0.162(10) Uiso 0.25 1 d D . P C 2
F41B F 0.273(2) 0.717(2) -0.0027(7) 0.087(5) Uiso 0.25 1 d D . P C 2
F42B F 0.275(3) 0.8756(19) -0.0980(11) 0.106(8) Uiso 0.25 1 d D . P C 2
F43B F 0.382(2) 0.621(2) -0.0964(10) 0.107(6) Uiso 0.25 1 d D . P C 2
F40C F 0.3411(15) 0.7838(18) -0.1244(7) 0.065(3) Uiso 0.25 1 d D . P C 3
F41C F 0.211(2) 0.5728(16) -0.1040(8) 0.083(4) Uiso 0.25 1 d D . P C 3
F42C F 0.1056(14) 0.8029(18) -0.0762(8) 0.069(3) Uiso 0.25 1 d D . P C 3
F43C F 0.340(2) 0.703(3) -0.0101(8) 0.082(6) Uiso 0.25 1 d D . P C 3


_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 2.113(4) . ?
Fe1 N9 2.195(5) . ?
Fe1 N14 2.171(5) . ?
Fe1 N18 2.115(4) . ?
Fe1 N25 2.180(5) . ?
Fe1 N30 2.191(5) . ?
Zn1 N2 2.113(4) . ?
Zn1 N9 2.195(5) . ?
Zn1 N14 2.171(5) . ?
Zn1 N18 2.115(4) . ?
Zn1 N25 2.180(5) . ?
Zn1 N30 2.191(5) . ?
N2 C3 1.324(7) . ?
N2 C7 1.337(7) . ?
C3 C4 1.378(8) . ?
C3 N8 1.417(7) . ?
C4 H4 0.9300 . ?
C4 C5 1.367(9) . ?
C5 H5 0.9300 . ?
C5 C6 1.377(10) . ?
C6 H6 0.9300 . ?
C6 C7 1.381(9) . ?
C7 N13 1.403(8) . ?
N8 N9 1.357(7) . ?
N8 C12 1.370(7) . ?
N9 C10 1.325(7) . ?
C10 H10 0.9300 . ?
C10 C11 1.395(10) . ?
C11 H11 0.9300 . ?
C11 C12 1.363(10) . ?
C12 H12 0.9300 . ?
N13 N14 1.361(7) . ?
N13 C17 1.345(8) . ?
N14 C15 1.323(8) . ?
C15 H15 0.9300 . ?
C15 C16 1.368(11) . ?
C16 H16 0.9300 . ?
C16 C17 1.365(12) . ?
C17 H17 0.9300 . ?
N18 C19 1.324(8) . ?
N18 C23 1.350(8) . ?
C19 C20 1.373(8) . ?
C19 N24 1.415(7) . ?
C20 H20 0.9300 . ?
C20 C21 1.393(10) . ?
C21 H21 0.9300 . ?
C21 C22 1.354(10) . ?
C22 H22 0.9300 . ?
C22 C23 1.369(8) . ?
C23 N29 1.406(8) . ?
N24 N25 1.365(6) . ?
N24 C28 1.345(8) . ?
N25 C26 1.321(8) . ?
C26 H26 0.9300 . ?
C26 C27 1.380(10) . ?
C27 H27 0.9300 . ?
C27 C28 1.351(10) . ?
C28 H28 0.9300 . ?
N29 N30 1.350(7) . ?
N29 C33 1.367(8) . ?
N30 C31 1.346(8) . ?
C31 H31 0.9300 . ?
C31 C32 1.367(11) . ?
C32 H32 0.9300 . ?
C32 C33 1.367(11) . ?
C33 H33 0.9300 . ?
B34 F35A 1.354(11) . ?
B34 F36A 1.491(11) . ?
B34 F37A 1.335(12) . ?
B34 F38A 1.350(12) . ?
B34 F35B 1.373(15) . ?
B34 F36B 1.471(14) . ?
B34 F37B 1.330(15) . ?
B34 F38B 1.445(13) . ?
B34 F35C 1.395(14) . ?
B34 F36C 1.418(15) . ?
B34 F37C 1.324(15) . ?
B34 F38C 1.402(17) . ?
B39 F40A 1.518(12) . ?
B39 F41A 1.367(11) . ?
B39 F42A 1.294(11) . ?
B39 F43A 1.380(13) . ?
B39 F40B 1.380(18) . ?
B39 F41B 1.344(15) . ?
B39 F42B 1.412(16) . ?
B39 F43B 1.426(16) . ?
B39 F40C 1.346(12) . ?
B39 F41C 1.433(15) . ?
B39 F42C 1.502(14) . ?
B39 F43C 1.328(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 73.62(16) . . ?
N2 Fe1 N14 73.97(17) . . ?
N2 Fe1 N18 173.8(2) . . ?
N2 Fe1 N25 111.9(2) . . ?
N2 Fe1 N30 100.4(2) . . ?
N14 Fe1 N9 147.58(19) . . ?
N14 Fe1 N25 95.57(18) . . ?
N14 Fe1 N30 91.81(19) . . ?
N18 Fe1 N9 103.74(17) . . ?
N18 Fe1 N14 108.41(18) . . ?
N18 Fe1 N25 73.8(2) . . ?
N18 Fe1 N30 73.9(2) . . ?
N25 Fe1 N9 97.21(18) . . ?
N25 Fe1 N30 147.62(18) . . ?
N30 Fe1 N9 93.12(18) . . ?
N2 Zn1 N9 73.62(16) . . ?
N2 Zn1 N14 73.97(17) . . ?
N2 Zn1 N18 173.8(2) . . ?
N2 Zn1 N25 111.9(2) . . ?
N2 Zn1 N30 100.4(2) . . ?
N14 Zn1 N9 147.58(19) . . ?
N14 Zn1 N25 95.57(18) . . ?
N14 Zn1 N30 91.81(19) . . ?
N18 Zn1 N9 103.74(17) . . ?
N18 Zn1 N14 108.41(18) . . ?
N18 Zn1 N25 73.8(2) . . ?
N18 Zn1 N30 73.9(2) . . ?
N25 Zn1 N9 97.21(18) . . ?
N25 Zn1 N30 147.62(18) . . ?
N30 Zn1 N9 93.12(18) . . ?
C3 N2 Fe1 121.5(3) . . ?
C3 N2 Zn1 121.5(3) . . ?
C3 N2 C7 118.4(4) . . ?
C7 N2 Fe1 120.1(4) . . ?
C7 N2 Zn1 120.1(4) . . ?
N2 C3 C4 123.3(5) . . ?
N2 C3 N8 112.2(5) . . ?
C4 C3 N8 124.6(5) . . ?
C3 C4 H4 121.4 . . ?
C5 C4 C3 117.1(6) . . ?
C5 C4 H4 121.4 . . ?
C4 C5 H5 119.3 . . ?
C4 C5 C6 121.5(5) . . ?
C6 C5 H5 119.3 . . ?
C5 C6 H6 121.6 . . ?
C5 C6 C7 116.9(5) . . ?
C7 C6 H6 121.6 . . ?
N2 C7 C6 122.8(6) . . ?
N2 C7 N13 113.2(5) . . ?
C6 C7 N13 124.0(5) . . ?
N9 N8 C3 119.3(4) . . ?
N9 N8 C12 111.0(5) . . ?
C12 N8 C3 129.7(5) . . ?
N8 N9 Fe1 113.4(3) . . ?
N8 N9 Zn1 113.4(3) . . ?
C10 N9 Fe1 141.4(5) . . ?
C10 N9 Zn1 141.4(5) . . ?
C10 N9 N8 105.3(5) . . ?
N9 C10 H10 124.3 . . ?
N9 C10 C11 111.4(6) . . ?
C11 C10 H10 124.3 . . ?
C10 C11 H11 127.2 . . ?
C12 C11 C10 105.6(5) . . ?
C12 C11 H11 127.2 . . ?
N8 C12 H12 126.7 . . ?
C11 C12 N8 106.7(6) . . ?
C11 C12 H12 126.7 . . ?
N14 N13 C7 118.3(4) . . ?
C17 N13 C7 129.5(6) . . ?
C17 N13 N14 112.0(6) . . ?
N13 N14 Fe1 114.2(3) . . ?
N13 N14 Zn1 114.2(3) . . ?
C15 N14 Fe1 140.3(5) . . ?
C15 N14 Zn1 140.3(5) . . ?
C15 N14 N13 104.5(5) . . ?
N14 C15 H15 124.5 . . ?
N14 C15 C16 111.1(7) . . ?
C16 C15 H15 124.5 . . ?
C15 C16 H16 126.5 . . ?
C17 C16 C15 106.9(6) . . ?
C17 C16 H16 126.5 . . ?
N13 C17 C16 105.5(7) . . ?
N13 C17 H17 127.3 . . ?
C16 C17 H17 127.3 . . ?
C19 N18 Fe1 121.1(4) . . ?
C19 N18 Zn1 121.1(4) . . ?
C19 N18 C23 118.6(5) . . ?
C23 N18 Fe1 120.2(4) . . ?
C23 N18 Zn1 120.2(4) . . ?
N18 C19 C20 123.3(5) . . ?
N18 C19 N24 112.5(5) . . ?
C20 C19 N24 124.3(5) . . ?
C19 C20 H20 121.8 . . ?
C19 C20 C21 116.4(6) . . ?
C21 C20 H20 121.8 . . ?
C20 C21 H21 119.2 . . ?
C22 C21 C20 121.7(6) . . ?
C22 C21 H21 119.2 . . ?
C21 C22 H22 121.1 . . ?
C21 C22 C23 117.8(6) . . ?
C23 C22 H22 121.1 . . ?
N18 C23 C22 122.3(5) . . ?
N18 C23 N29 112.5(5) . . ?
C22 C23 N29 125.3(5) . . ?
N25 N24 C19 118.9(4) . . ?
C28 N24 C19 130.0(5) . . ?
C28 N24 N25 111.0(5) . . ?
N24 N25 Fe1 113.7(3) . . ?
N24 N25 Zn1 113.7(3) . . ?
C26 N25 Fe1 141.8(4) . . ?
C26 N25 Zn1 141.8(4) . . ?
C26 N25 N24 104.4(5) . . ?
N25 C26 H26 124.1 . . ?
N25 C26 C27 111.7(6) . . ?
C27 C26 H26 124.1 . . ?
C26 C27 H27 127.2 . . ?
C28 C27 C26 105.6(6) . . ?
C28 C27 H27 127.2 . . ?
N24 C28 C27 107.3(6) . . ?
N24 C28 H28 126.3 . . ?
C27 C28 H28 126.3 . . ?
N30 N29 C23 119.6(5) . . ?
N30 N29 C33 111.6(6) . . ?
C33 N29 C23 128.8(6) . . ?
N29 N30 Fe1 113.6(4) . . ?
N29 N30 Zn1 113.6(4) . . ?
C31 N30 Fe1 141.5(5) . . ?
C31 N30 Zn1 141.5(5) . . ?
C31 N30 N29 104.8(6) . . ?
N30 C31 H31 124.5 . . ?
N30 C31 C32 110.9(7) . . ?
C32 C31 H31 124.5 . . ?
C31 C32 H32 126.5 . . ?
C31 C32 C33 107.0(6) . . ?
C33 C32 H32 126.5 . . ?
N29 C33 H33 127.1 . . ?
C32 C33 N29 105.7(7) . . ?
C32 C33 H33 127.1 . . ?
F35A B34 F36A 103.5(8) . . ?
F37A B34 F35A 118.8(10) . . ?
F37A B34 F36A 97.5(8) . . ?
F37A B34 F38A 113.3(10) . . ?
F38A B34 F35A 113.0(10) . . ?
F38A B34 F36A 108.4(8) . . ?
F35B B34 F36B 102.4(11) . . ?
F35B B34 F38B 109.2(11) . . ?
F37B B34 F35B 114.2(13) . . ?
F37B B34 F36B 109.3(11) . . ?
F37B B34 F38B 120.4(11) . . ?
F38B B34 F36B 98.6(9) . . ?
F35C B34 F36C 109.3(12) . . ?
F35C B34 F38C 107.9(13) . . ?
F37C B34 F35C 112.6(12) . . ?
F37C B34 F36C 106.6(11) . . ?
F37C B34 F38C 113.3(14) . . ?
F38C B34 F36C 106.9(13) . . ?
F41A B39 F40A 100.6(8) . . ?
F41A B39 F43A 113.0(9) . . ?
F42A B39 F40A 103.3(8) . . ?
F42A B39 F41A 116.1(9) . . ?
F42A B39 F43A 115.2(10) . . ?
F43A B39 F40A 106.3(10) . . ?
F40B B39 F42B 111.2(15) . . ?
F40B B39 F43B 103.5(14) . . ?
F41B B39 F40B 111.2(13) . . ?
F41B B39 F42B 110.4(13) . . ?
F41B B39 F43B 108.4(12) . . ?
F42B B39 F43B 111.9(13) . . ?
F40C B39 F41C 102.4(10) . . ?
F40C B39 F42C 107.0(9) . . ?
F41C B39 F42C 99.7(10) . . ?
F43C B39 F40C 117.5(12) . . ?
F43C B39 F41C 111.7(13) . . ?
F43C B39 F42C 116.2(11) . . ?

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 -177.4(4) . . . . ?
Fe1 N2 C3 N8 2.4(7) . . . . ?
Fe1 N2 C7 C6 177.3(5) . . . . ?
Fe1 N2 C7 N13 -2.5(7) . . . . ?
Fe1 N9 C10 C11 -178.4(5) . . . . ?
Fe1 N14 C15 C16 -167.7(6) . . . . ?
Fe1 N18 C19 C20 -179.5(4) . . . . ?
Fe1 N18 C19 N24 1.3(6) . . . . ?
Fe1 N18 C23 C22 179.4(4) . . . . ?
Fe1 N18 C23 N29 0.3(6) . . . . ?
Fe1 N25 C26 C27 174.5(5) . . . . ?
Fe1 N30 C31 C32 175.3(5) . . . . ?
Zn1 N2 C3 C4 -177.4(4) . . . . ?
Zn1 N2 C3 N8 2.4(7) . . . . ?
Zn1 N2 C7 C6 177.3(5) . . . . ?
Zn1 N2 C7 N13 -2.5(7) . . . . ?
Zn1 N9 C10 C11 -178.4(5) . . . . ?
Zn1 N14 C15 C16 -167.7(6) . . . . ?
Zn1 N18 C19 C20 -179.5(4) . . . . ?
Zn1 N18 C19 N24 1.3(6) . . . . ?
Zn1 N18 C23 C22 179.4(4) . . . . ?
Zn1 N18 C23 N29 0.3(6) . . . . ?
Zn1 N25 C26 C27 174.5(5) . . . . ?
Zn1 N30 C31 C32 175.3(5) . . . . ?
N2 C3 C4 C5 -1.1(10) . . . . ?
N2 C3 N8 N9 -1.1(7) . . . . ?
N2 C3 N8 C12 179.5(6) . . . . ?
N2 C7 N13 N14 5.2(7) . . . . ?
N2 C7 N13 C17 -170.3(6) . . . . ?
C3 N2 C7 C6 -1.7(9) . . . . ?
C3 N2 C7 N13 178.5(5) . . . . ?
C3 C4 C5 C6 0.6(11) . . . . ?
C3 N8 N9 Fe1 -0.5(6) . . . . ?
C3 N8 N9 Zn1 -0.5(6) . . . . ?
C3 N8 N9 C10 179.3(5) . . . . ?
C3 N8 C12 C11 179.6(5) . . . . ?
C4 C3 N8 N9 178.6(5) . . . . ?
C4 C3 N8 C12 -0.8(9) . . . . ?
C4 C5 C6 C7 -0.7(11) . . . . ?
C5 C6 C7 N2 1.2(10) . . . . ?
C5 C6 C7 N13 -179.0(6) . . . . ?
C6 C7 N13 N14 -174.7(5) . . . . ?
C6 C7 N13 C17 9.9(10) . . . . ?
C7 N2 C3 C4 1.6(9) . . . . ?
C7 N2 C3 N8 -178.6(5) . . . . ?
C7 N13 N14 Fe1 -5.3(6) . . . . ?
C7 N13 N14 Zn1 -5.3(6) . . . . ?
C7 N13 N14 C15 -176.4(5) . . . . ?
C7 N13 C17 C16 176.5(6) . . . . ?
N8 C3 C4 C5 179.1(6) . . . . ?
N8 N9 C10 C11 1.9(7) . . . . ?
N9 N8 C12 C11 0.1(7) . . . . ?
N9 C10 C11 C12 -1.8(8) . . . . ?
C10 C11 C12 N8 1.0(7) . . . . ?
C12 N8 N9 Fe1 179.0(4) . . . . ?
C12 N8 N9 Zn1 179.0(4) . . . . ?
C12 N8 N9 C10 -1.2(6) . . . . ?
N13 N14 C15 C16 -0.6(8) . . . . ?
N14 N13 C17 C16 0.8(8) . . . . ?
N14 C15 C16 C17 1.1(9) . . . . ?
C15 C16 C17 N13 -1.1(8) . . . . ?
C17 N13 N14 Fe1 170.9(4) . . . . ?
C17 N13 N14 Zn1 170.9(4) . . . . ?
C17 N13 N14 C15 -0.2(7) . . . . ?
N18 C19 C20 C21 -0.7(9) . . . . ?
N18 C19 N24 N25 -1.4(6) . . . . ?
N18 C19 N24 C28 174.5(5) . . . . ?
N18 C23 N29 N30 -3.4(7) . . . . ?
N18 C23 N29 C33 177.7(5) . . . . ?
C19 N18 C23 C22 -1.3(7) . . . . ?
C19 N18 C23 N29 179.6(4) . . . . ?
C19 C20 C21 C22 0.3(10) . . . . ?
C19 N24 N25 Fe1 0.9(5) . . . . ?
C19 N24 N25 Zn1 0.9(5) . . . . ?
C19 N24 N25 C26 177.4(5) . . . . ?
C19 N24 C28 C27 -177.0(5) . . . . ?
C20 C19 N24 N25 179.5(5) . . . . ?
C20 C19 N24 C28 -4.6(9) . . . . ?
C20 C21 C22 C23 -0.4(10) . . . . ?
C21 C22 C23 N18 0.9(8) . . . . ?
C21 C22 C23 N29 179.9(5) . . . . ?
C22 C23 N29 N30 177.5(5) . . . . ?
C22 C23 N29 C33 -1.3(9) . . . . ?
C23 N18 C19 C20 1.2(8) . . . . ?
C23 N18 C19 N24 -178.0(4) . . . . ?
C23 N29 N30 Fe1 4.7(6) . . . . ?
C23 N29 N30 Zn1 4.7(6) . . . . ?
C23 N29 N30 C31 -177.7(5) . . . . ?
C23 N29 C33 C32 177.9(5) . . . . ?
N24 C19 C20 C21 178.4(5) . . . . ?
N24 N25 C26 C27 -0.3(6) . . . . ?
N25 N24 C28 C27 -0.9(7) . . . . ?
N25 C26 C27 C28 -0.2(8) . . . . ?
C26 C27 C28 N24 0.6(8) . . . . ?
C28 N24 N25 Fe1 -175.8(4) . . . . ?
C28 N24 N25 Zn1 -175.8(4) . . . . ?
C28 N24 N25 C26 0.7(6) . . . . ?
N29 N30 C31 C32 -1.2(7) . . . . ?
N30 N29 C33 C32 -1.0(7) . . . . ?
N30 C31 C32 C33 0.6(8) . . . . ?
C31 C32 C33 N29 0.2(8) . . . . ?
C33 N29 N30 Fe1 -176.3(4) . . . . ?
C33 N29 N30 Zn1 -176.3(4) . . . . ?
C33 N29 N30 C31 1.3(6) . . . . ?

_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_mh453ltd
_database_code_depnum_ccdc_archive 'CCDC 2261788'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2023-08-21 deposited with the CCDC.	2023-08-30 downloaded from the CCDC.
;
_audit_creation_date             2023-03-06
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis[2,6-di(pyrazol-1-yl)pyridine]iron(II) bis[2,6-di(pyrazol-1-yl)pyridine]-zinc(II) ditetrafluoroborate 0.54:0.46 solid solution (disordered refinement)'
_chemical_formula_moiety         
'0.54(C22 H18 Fe N10), 0.46(C22 H18 N10 Zn), 2(B F4)'
_chemical_formula_sum            'C22 H18 B2 F8 Fe0.54 N10 Zn0.46'
_chemical_formula_weight         656.31
_chemical_absolute_configuration ab
_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 0.0019 0.0015 '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 0.0004 0.0006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0124 0.0097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.2961 0.8007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0037 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2335 1.3591 '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           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   8.4486(1)
_cell_length_b                   8.4867(1)
_cell_length_c                   18.5535(1)
_cell_angle_alpha                90
_cell_angle_beta                 97.618(1)
_cell_angle_gamma                90
_cell_volume                     1318.56(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    13086
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      35.15
_cell_measurement_theta_min      2.14
_exptl_absorpt_coefficient_mu    0.766
_exptl_absorpt_correction_T_min  0.897
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
DIALS 3.12.1-2-g1c07bc2b3-release
Scaling & analysis of unmerged intensities, absorption correction using 
spherical harmonics
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       lath
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0724
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            29979
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        24.620
_diffrn_reflns_theta_max         36.109
_diffrn_reflns_theta_min         1.073
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.930
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_measurement_device       'Fixed χ 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.979
_reflns_Friedel_fraction_max     0.844
_reflns_number_gt                9617
_reflns_number_total             12312
_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       'XIA2 0.4.0.438-g4431aaa (Winter, 2010)'
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction        'XIA2 0.4.0.438-g4431aaa (Winter, 2010)'
_computing_molecular_graphics    'XSEED (Barbour, 2020)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details 
;
 Flack x determined using 3006 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.006(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         12312
_refine_ls_number_restraints     44
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0377
_refine_ls_restrained_S_all      1.022
_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)+(0.0299P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0753
_refine_special_details          
;
 Following an initial structure solution, discrete partial (low-spin) 
 [Fe(bpp)₂]2+ and [Zn(bpp)₂]2+ molecule sites were constructed and 
 refined without restraints. The Fe:Zn occupancy ratio refined to 0.54:0.46, 
 so those occupancies were used for those disorder sites in the final least 
 squares cycles. The F atoms of one BF₄⁻ ion were also disordered over 
 two orientations, with refined occupancies of 0.67:0.33. The refined 
 distance restraints listed below were applied to that moiety.

 The Fe and Zn atoms, and all the B and F atoms were refined  anisotropically,
 using ISOR restraints for some partial F atoms. Attempts to refine the 
 partial N atoms anisotropically led to them becoming non-positive 
 definite, so they were left isotropic in the final least squares cycles. 
 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
2. Restrained distances
 B39-F40A
 1.39363 with sigma of 0.02
 B39-F41A
 1.39363 with sigma of 0.02
 B39-F42A
 1.39363 with sigma of 0.02
 B39-F43A
 1.39363 with sigma of 0.02
 B39-F40B
 1.39363 with sigma of 0.02
 B39-F41B
 1.39363 with sigma of 0.02
 B39-F42B
 1.39363 with sigma of 0.02
 B39-F43B
 1.39363 with sigma of 0.02
 F40A-F41A
 2.275798 with sigma of 0.02
 F40A-F42A
 2.275798 with sigma of 0.02
 F40A-F43A
 2.275798 with sigma of 0.02
 F41A-F42A
 2.275798 with sigma of 0.02
 F41A-F43A
 2.275798 with sigma of 0.02
 F42A-F43A
 2.275798 with sigma of 0.02
 F40B-F41B
 2.275798 with sigma of 0.02
 F40B-F42B
 2.275798 with sigma of 0.02
 F40B-F43B
 2.275798 with sigma of 0.02
 F41B-F42B
 2.275798 with sigma of 0.02
 F41B-F43B
 2.275798 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F40B) \\sim Ueq, Uanis(F41B) \\sim Ueq, Uanis(F42B) \\sim Ueq,
Uanis(F43B) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
4. Others
 1(DFIX)=1(DFIX)=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(DFIX)=1(DFIX)=1(DFIX)=
 1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: Fe1(0.54) N2A(0.54) C3A(0.54) C4A(0.54) H4A(0.54) C5A(0.54)
 H5A(0.54) C6A(0.54) H6A(0.54) C7A(0.54) N8A(0.54) N9A(0.54) C10A(0.54)
 H10A(0.54) C11A(0.54) H11A(0.54) C12A(0.54) H12A(0.54) N13A(0.54) N14A(0.54)
 C15A(0.54) H15A(0.54) C16A(0.54) H16A(0.54) C17A(0.54) H17A(0.54) N18A(0.54)
 C19A(0.54) C20A(0.46) H20A(0.46) C21A(0.54) H21A(0.54) C22A(0.54) H22A(0.54)
 C23A(0.54) N24A(0.54) N25A(0.54) C26A(0.54) H26A(0.54) C27A(0.54) H27A(0.54)
 C28A(0.54) H28A(0.54) N29A(0.54) N30A(0.54) C31A(0.54) H31A(0.54) C32A(0.54)
 H32A(0.54) C33A(0.54) H33A(0.54) Zn1(0.46) N2B(0.46) C3B(0.46) C4B(0.46)
 H4B(0.46) C5B(0.46) H5B(0.46) C6B(0.46) H6B(0.46) C7B(0.46) N8B(0.46)
 N9B(0.46) C10B(0.46) H10B(0.46) C11B(0.46) H11B(0.46) C12B(0.46) H12B(0.46)
 N13B(0.46) N14B(0.46) C15B(0.46) H15B(0.46) C16B(0.46) H16B(0.46) C17B(0.46)
 H17B(0.46) N18B(0.46) C19B(0.46) C20B(0.54) H20B(0.54) C21B(0.46) H21B(0.46)
 C22B(0.46) H22B(0.46) C23B(0.46) N24B(0.46) N25B(0.46) C26B(0.46) H26B(0.46)
 C27B(0.46) H27B(0.46) C28B(0.46) H28B(0.46) N29B(0.46) N30B(0.46) C31B(0.46)
 H31B(0.46) C32B(0.46) H32B(0.46) C33B(0.46) H33B(0.46) F40A(0.67) F41A(0.67)
 F42A(0.67) F43A(0.67) F40B(0.33) F41B(0.33) F42B(0.33) F43B(0.33)
5.a Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C5A(H5A), C6A(H6A), C10A(H10A), C11A(H11A), C12A(H12A), C15A(H15A),
 C16A(H16A), C17A(H17A), C20A(H20A), C21A(H21A), C22A(H22A), C26A(H26A),
 C27A(H27A), C28A(H28A), C31A(H31A), C32A(H32A), C33A(H33A), C4B(H4B), C5B(H5B),
  C6B(H6B), C10B(H10B), C11B(H11B), C12B(H12B), C15B(H15B), C16B(H16B),
 C17B(H17B), C20B(H20B), C21B(H21B), C22B(H22B), C26B(H26B), C27B(H27B),
 C28B(H28B), C31B(H31B), C32B(H32B), C33B(H33B)
;
_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 0.2781(7) 0.1608(10) 0.2532(3) 0.0147(5) Uani 0.54 1 d . . P A 1
N2A N 0.2825(5) 0.1452(7) 0.3562(2) 0.0189(10) Uiso 0.54 1 d . . P A 1
C3A C 0.4115(7) 0.0893(7) 0.3979(3) 0.0181(13) Uiso 0.54 1 d . . P A 1
C4A C 0.4215(12) 0.0807(12) 0.4791(5) 0.024(2) Uiso 0.54 1 d . . P A 1
H4A H 0.512940 0.043336 0.509662 0.029 Uiso 0.54 1 calc R U P A 1
C5A C 0.2834(7) 0.1330(8) 0.5055(3) 0.0284(15) Uiso 0.54 1 d . . P A 1
H5A H 0.279587 0.126361 0.556342 0.034 Uiso 0.54 1 calc R U P A 1
C6A C 0.1506(6) 0.1945(5) 0.4617(3) 0.0226(10) Uiso 0.54 1 d . . P A 1
H6A H 0.059689 0.231570 0.481702 0.027 Uiso 0.54 1 calc R U P A 1
C7A C 0.1584(5) 0.1987(5) 0.3877(2) 0.0158(8) Uiso 0.54 1 d . . P A 1
N8A N 0.5313(6) 0.0444(6) 0.3553(3) 0.0199(11) Uiso 0.54 1 d . . P A 1
N9A N 0.4944(6) 0.0705(5) 0.2812(2) 0.0212(10) Uiso 0.54 1 d . . P A 1
C10A C 0.6249(5) 0.0231(5) 0.2531(2) 0.0199(8) Uiso 0.54 1 d . . P A 1
H10A H 0.636284 0.026581 0.202834 0.024 Uiso 0.54 1 calc R U P A 1
C11A C 0.7434(5) -0.0328(5) 0.3084(2) 0.0238(9) Uiso 0.54 1 d . . P A 1
H11A H 0.845860 -0.072784 0.302453 0.029 Uiso 0.54 1 calc R U P A 1
C12A C 0.6801(6) -0.0176(5) 0.3721(3) 0.0229(10) Uiso 0.54 1 d . . P A 1
H12A H 0.730587 -0.045090 0.419221 0.027 Uiso 0.54 1 calc R U P A 1
N13A N 0.0383(4) 0.2600(4) 0.33501(19) 0.0181(7) Uiso 0.54 1 d . . P A 1
N14A N 0.0678(4) 0.2502(4) 0.2641(2) 0.0198(7) Uiso 0.54 1 d . . P A 1
C15A C -0.0583(5) 0.3170(5) 0.2254(2) 0.0223(7) Uiso 0.54 1 d . . P A 1
H15A H -0.073275 0.326485 0.173916 0.027 Uiso 0.54 1 calc R U P A 1
C16A C -0.1664(5) 0.3715(5) 0.2714(2) 0.0249(7) Uiso 0.54 1 d . . P A 1
H16A H -0.264439 0.424714 0.257001 0.030 Uiso 0.54 1 calc R U P A 1
C17A C -0.1030(5) 0.3333(5) 0.3403(2) 0.0235(7) Uiso 0.54 1 d . . P A 1
H17A H -0.148295 0.353694 0.383559 0.028 Uiso 0.54 1 calc R U P A 1
N18A N 0.2787(6) 0.1874(5) 0.1512(2) 0.0184(10) Uiso 0.54 1 d . . P A 1
C19A C 0.2215(8) 0.0728(7) 0.1046(3) 0.0183(13) Uiso 0.54 1 d . . P A 1
C20A C 0.2162(11) 0.0933(10) 0.0276(5) 0.026(2) Uiso 0.46 1 d . . P A 1
H20A H 0.173425 0.013914 -0.005470 0.032 Uiso 0.46 1 calc R U P A 1
C21A C 0.2755(7) 0.2326(6) 0.0031(3) 0.0228(11) Uiso 0.54 1 d . . P A 1
H21A H 0.277849 0.246954 -0.047490 0.027 Uiso 0.54 1 calc R U P A 1
C22A C 0.3317(6) 0.3521(6) 0.0512(3) 0.0206(10) Uiso 0.54 1 d . . P A 1
H22A H 0.368850 0.449366 0.034437 0.025 Uiso 0.54 1 calc R U P A 1
C23A C 0.3310(6) 0.3224(6) 0.1252(3) 0.0188(11) Uiso 0.54 1 d . . P A 1
N24A N 0.1666(6) -0.0551(6) 0.1420(3) 0.0201(10) Uiso 0.54 1 d . . P A 1
N25A N 0.1842(5) -0.0416(4) 0.2178(2) 0.0200(7) Uiso 0.54 1 d . . P A 1
C26A C 0.1163(5) -0.1721(5) 0.2399(2) 0.0222(7) Uiso 0.54 1 d . . P A 1
H26A H 0.109703 -0.196841 0.289351 0.027 Uiso 0.54 1 calc R U P A 1
C27A C 0.0553(5) -0.2687(5) 0.1805(2) 0.0265(8) Uiso 0.54 1 d . . P A 1
H27A H 0.001082 -0.366397 0.182487 0.032 Uiso 0.54 1 calc R U P A 1
C28A C 0.0905(7) -0.1928(6) 0.1200(3) 0.0283(11) Uiso 0.54 1 d . . P A 1
H28A H 0.066552 -0.228848 0.071340 0.034 Uiso 0.54 1 calc R U P A 1
N29A N 0.3845(5) 0.4271(5) 0.1818(2) 0.0189(8) Uiso 0.54 1 d . . P A 1
N30A N 0.3687(5) 0.3763(5) 0.2505(2) 0.0195(9) Uiso 0.54 1 d . . P A 1
C31A C 0.4124(5) 0.4971(5) 0.2933(2) 0.0202(7) Uiso 0.54 1 d . . P A 1
H31A H 0.411881 0.497656 0.344467 0.024 Uiso 0.54 1 calc R U P A 1
C32A C 0.4601(5) 0.6255(4) 0.2527(2) 0.0240(8) Uiso 0.54 1 d . . P A 1
H32A H 0.497608 0.725147 0.271001 0.029 Uiso 0.54 1 calc R U P A 1
C33A C 0.4412(5) 0.5770(5) 0.1820(2) 0.0233(8) Uiso 0.54 1 d . . P A 1
H33A H 0.463312 0.636277 0.141026 0.028 Uiso 0.54 1 calc R U P A 1
Zn1 Zn 0.2709(7) 0.1532(10) 0.2538(3) 0.0197(8) Uani 0.46 1 d . . P B 2
N2B N 0.2871(6) 0.1483(8) 0.3671(3) 0.0164(10) Uiso 0.46 1 d . . P B 2
C3B C 0.4153(9) 0.0889(8) 0.4077(4) 0.0186(15) Uiso 0.46 1 d . . P B 2
C4B C 0.4299(14) 0.0735(14) 0.4750(6) 0.025(3) Uiso 0.46 1 d . . P B 2
H4B H 0.523658 0.027660 0.500425 0.030 Uiso 0.46 1 calc R U P B 2
C5B C 0.3058(8) 0.1248(8) 0.5129(3) 0.0213(14) Uiso 0.46 1 d . . P B 2
H5B H 0.316171 0.117639 0.564442 0.026 Uiso 0.46 1 calc R U P B 2
C6B C 0.1695(7) 0.1853(6) 0.4743(3) 0.0205(11) Uiso 0.46 1 d . . P B 2
H6B H 0.082022 0.219101 0.497727 0.025 Uiso 0.46 1 calc R U P B 2
C7B C 0.1655(7) 0.1946(6) 0.4015(3) 0.0204(12) Uiso 0.46 1 d . . P B 2
N8B N 0.5337(7) 0.0447(7) 0.3658(3) 0.0178(12) Uiso 0.46 1 d . . P B 2
N9B N 0.5087(6) 0.0599(6) 0.2916(3) 0.0146(9) Uiso 0.46 1 d . . P B 2
C10B C 0.6411(6) 0.0109(6) 0.2690(3) 0.0187(9) Uiso 0.46 1 d . . P B 2
H10B H 0.658576 0.009505 0.219482 0.022 Uiso 0.46 1 calc R U P B 2
C11B C 0.7534(6) -0.0392(6) 0.3268(3) 0.0205(9) Uiso 0.46 1 d . . P B 2
H11B H 0.856868 -0.080742 0.324153 0.025 Uiso 0.46 1 calc R U P B 2
C12B C 0.6818(6) -0.0154(6) 0.3881(3) 0.0185(10) Uiso 0.46 1 d . . P B 2
H12B H 0.726857 -0.036620 0.436779 0.022 Uiso 0.46 1 calc R U P B 2
N13B N 0.0400(5) 0.2569(5) 0.3521(2) 0.0195(9) Uiso 0.46 1 d . . P B 2
N14B N 0.0456(5) 0.2445(5) 0.2784(2) 0.0212(9) Uiso 0.46 1 d . . P B 2
C15B C -0.0823(6) 0.3215(5) 0.2464(3) 0.0232(8) Uiso 0.46 1 d . . P B 2
H15B H -0.110384 0.331641 0.195304 0.028 Uiso 0.46 1 calc R U P B 2
C16B C -0.1691(6) 0.3850(6) 0.2985(3) 0.0254(8) Uiso 0.46 1 d . . P B 2
H16B H -0.264849 0.444777 0.289752 0.030 Uiso 0.46 1 calc R U P B 2
C17B C -0.0885(6) 0.3439(5) 0.3642(3) 0.0224(8) Uiso 0.46 1 d . . P B 2
H17B H -0.117252 0.371267 0.410448 0.027 Uiso 0.46 1 calc R U P B 2
N18B N 0.2693(6) 0.1792(7) 0.1410(3) 0.0160(10) Uiso 0.46 1 d . . P B 2
C19B C 0.2147(9) 0.0654(9) 0.0958(4) 0.0206(17) Uiso 0.46 1 d . . P B 2
C20B C 0.2138(8) 0.0720(8) 0.0254(3) 0.0208(14) Uiso 0.54 1 d . . P B 2
H20B H 0.176749 -0.014366 -0.004831 0.025 Uiso 0.54 1 calc R U P B 2
C21B C 0.2678(7) 0.2067(7) -0.0035(3) 0.0206(13) Uiso 0.46 1 d . . P B 2
H21B H 0.265761 0.215227 -0.054645 0.025 Uiso 0.46 1 calc R U P B 2
C22B C 0.3253(7) 0.3310(7) 0.0408(3) 0.0199(11) Uiso 0.46 1 d . . P B 2
H22B H 0.363836 0.424991 0.021486 0.024 Uiso 0.46 1 calc R U P B 2
C23B C 0.3237(7) 0.3111(7) 0.1138(3) 0.0175(12) Uiso 0.46 1 d . . P B 2
N24B N 0.1593(7) -0.0668(7) 0.1317(3) 0.0217(13) Uiso 0.46 1 d . . P B 2
N25B N 0.1676(5) -0.0651(5) 0.2059(2) 0.0178(8) Uiso 0.46 1 d . . P B 2
C26B C 0.0984(5) -0.1982(5) 0.2226(2) 0.0195(8) Uiso 0.46 1 d . . P B 2
H26B H 0.086761 -0.230641 0.270611 0.023 Uiso 0.46 1 calc R U P B 2
C27B C 0.0451(6) -0.2840(6) 0.1595(3) 0.0238(9) Uiso 0.46 1 d . . P B 2
H27B H -0.008036 -0.382942 0.156353 0.029 Uiso 0.46 1 calc R U P B 2
C28B C 0.0860(7) -0.1947(6) 0.1037(3) 0.0220(11) Uiso 0.46 1 d . . P B 2
H28B H 0.065420 -0.219961 0.053422 0.026 Uiso 0.46 1 calc R U P B 2
N29B N 0.3731(6) 0.4229(5) 0.1678(2) 0.0175(9) Uiso 0.46 1 d . . P B 2
N30B N 0.3578(6) 0.3912(6) 0.2390(3) 0.0192(10) Uiso 0.46 1 d . . P B 2
C31B C 0.4123(6) 0.5195(6) 0.2757(3) 0.0218(9) Uiso 0.46 1 d . . P B 2
H31B H 0.415802 0.531857 0.326817 0.026 Uiso 0.46 1 calc R U P B 2
C32B C 0.4629(5) 0.6322(5) 0.2302(2) 0.0236(9) Uiso 0.46 1 d . . P B 2
H32B H 0.506573 0.732747 0.243713 0.028 Uiso 0.46 1 calc R U P B 2
C33B C 0.4374(5) 0.5695(5) 0.1617(3) 0.0202(8) Uiso 0.46 1 d . . P B 2
H33B H 0.460113 0.618451 0.118203 0.024 Uiso 0.46 1 calc R U P B 2
B34 B 0.2049(3) 0.7048(3) 0.43290(14) 0.0307(5) Uani 1 1 d . . . . .
F35 F 0.32367(17) 0.75904(16) 0.39379(7) 0.0361(3) Uani 1 1 d . . . . .
F36 F 0.23483(19) 0.75784(17) 0.50500(8) 0.0408(3) Uani 1 1 d . . . . .
F37 F 0.20657(19) 0.54136(17) 0.43349(8) 0.0407(3) Uani 1 1 d . . . . .
F38 F 0.0572(2) 0.7602(2) 0.40177(9) 0.0579(5) Uani 1 1 d . . . . .
B39 B 0.2780(4) 0.7132(3) -0.06120(14) 0.0354(6) Uani 1 1 d D . . . .
F40A F 0.3579(11) 0.7290(11) 0.0121(3) 0.0299(9) Uani 0.67 1 d D . P C 1
F41A F 0.3162(6) 0.8515(5) -0.0974(2) 0.0277(7) Uani 0.67 1 d D . P C 1
F42A F 0.1185(7) 0.7014(6) -0.0598(4) 0.0437(12) Uani 0.67 1 d D . P C 1
F43A F 0.3439(4) 0.5820(4) -0.09063(19) 0.0425(7) Uani 0.67 1 d D . P C 1
F40B F 0.339(2) 0.709(2) 0.0070(8) 0.039(4) Uani 0.33 1 d D U P C 2
F41B F 0.3292(14) 0.8139(11) -0.1100(5) 0.042(2) Uani 0.33 1 d D U P C 2
F42B F 0.1050(14) 0.7491(13) -0.0646(8) 0.045(2) Uani 0.33 1 d D U P C 2
F43B F 0.2719(10) 0.5625(10) -0.0955(5) 0.063(2) Uani 0.33 1 d D U P C 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 N2A 1.912(7) . ?
Fe1 N9A 1.986(7) . ?
Fe1 N14A 1.967(7) . ?
Fe1 N18A 1.906(7) . ?
Fe1 N25A 1.968(9) . ?
Fe1 N30A 1.986(10) . ?
N2A C3A 1.337(7) . ?
N2A C7A 1.345(6) . ?
C3A C4A 1.500(11) . ?
C3A N8A 1.416(8) . ?
C4A H4A 0.9500 . ?
C4A C5A 1.396(11) . ?
C5A H5A 0.9500 . ?
C5A C6A 1.396(7) . ?
C6A H6A 0.9500 . ?
C6A C7A 1.384(6) . ?
C7A N13A 1.411(6) . ?
N8A N9A 1.388(7) . ?
N8A C12A 1.360(7) . ?
N9A C10A 1.342(6) . ?
C10A H10A 0.9500 . ?
C10A C11A 1.418(6) . ?
C11A H11A 0.9500 . ?
C11A C12A 1.365(7) . ?
C12A H12A 0.9500 . ?
N13A N14A 1.373(5) . ?
N13A C17A 1.361(5) . ?
N14A C15A 1.330(5) . ?
C15A H15A 0.9500 . ?
C15A C16A 1.408(6) . ?
C16A H16A 0.9500 . ?
C16A C17A 1.358(5) . ?
C17A H17A 0.9500 . ?
N18A C19A 1.348(7) . ?
N18A C23A 1.340(7) . ?
C19A C20A 1.434(10) . ?
C19A N24A 1.400(8) . ?
C20A H20A 0.9500 . ?
C20A C21A 1.384(10) . ?
C21A H21A 0.9500 . ?
C21A C22A 1.392(7) . ?
C22A H22A 0.9500 . ?
C22A C23A 1.397(7) . ?
C23A N29A 1.403(6) . ?
N24A N25A 1.399(6) . ?
N24A C28A 1.370(7) . ?
N25A C26A 1.337(6) . ?
C26A H26A 0.9500 . ?
C26A C27A 1.415(6) . ?
C27A H27A 0.9500 . ?
C27A C28A 1.360(7) . ?
C28A H28A 0.9500 . ?
N29A N30A 1.369(6) . ?
N29A C33A 1.360(6) . ?
N30A C31A 1.319(6) . ?
C31A H31A 0.9500 . ?
C31A C32A 1.413(6) . ?
C32A H32A 0.9500 . ?
C32A C33A 1.365(6) . ?
C33A H33A 0.9500 . ?
Zn1 N2B 2.088(7) . ?
Zn1 N9B 2.187(7) . ?
Zn1 N14B 2.159(7) . ?
Zn1 N18B 2.102(7) . ?
Zn1 N25B 2.186(9) . ?
Zn1 N30B 2.179(10) . ?
N2B C3B 1.334(9) . ?
N2B C7B 1.338(8) . ?
C3B C4B 1.245(13) . ?
C3B N8B 1.398(9) . ?
C4B H4B 0.9500 . ?
C4B C5B 1.407(13) . ?
C5B H5B 0.9500 . ?
C5B C6B 1.373(8) . ?
C6B H6B 0.9500 . ?
C6B C7B 1.349(7) . ?
C7B N13B 1.409(7) . ?
N8B N9B 1.370(7) . ?
N8B C12B 1.364(8) . ?
N9B C10B 1.313(7) . ?
C10B H10B 0.9500 . ?
C10B C11B 1.400(7) . ?
C11B H11B 0.9500 . ?
C11B C12B 1.372(7) . ?
C12B H12B 0.9500 . ?
N13B N14B 1.377(6) . ?
N13B C17B 1.357(6) . ?
N14B C15B 1.333(6) . ?
C15B H15B 0.9500 . ?
C15B C16B 1.397(7) . ?
C16B H16B 0.9500 . ?
C16B C17B 1.362(6) . ?
C17B H17B 0.9500 . ?
N18B C19B 1.322(9) . ?
N18B C23B 1.335(8) . ?
C19B C20B 1.306(10) . ?
C19B N24B 1.416(10) . ?
C20B H20B 0.9500 . ?
C20B C21B 1.366(9) . ?
C21B H21B 0.9500 . ?
C21B C22B 1.385(8) . ?
C22B H22B 0.9500 . ?
C22B C23B 1.367(8) . ?
C23B N29B 1.402(7) . ?
N24B N25B 1.368(7) . ?
N24B C28B 1.321(8) . ?
N25B C26B 1.327(6) . ?
C26B H26B 0.9500 . ?
C26B C27B 1.401(7) . ?
C27B H27B 0.9500 . ?
C27B C28B 1.365(7) . ?
C28B H28B 0.9500 . ?
N29B N30B 1.371(7) . ?
N29B C33B 1.368(7) . ?
N30B C31B 1.333(7) . ?
C31B H31B 0.9500 . ?
C31B C32B 1.381(7) . ?
C32B H32B 0.9500 . ?
C32B C33B 1.368(7) . ?
C33B H33B 0.9500 . ?
B34 F35 1.392(3) . ?
B34 F36 1.402(3) . ?
B34 F37 1.387(3) . ?
B34 F38 1.386(3) . ?
B39 F40A 1.442(7) . ?
B39 F41A 1.411(5) . ?
B39 F42A 1.355(6) . ?
B39 F43A 1.389(5) . ?
B39 F40B 1.302(13) . ?
B39 F41B 1.356(10) . ?
B39 F42B 1.486(12) . ?
B39 F43B 1.427(9) . ?

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 Fe1 N9A 79.4(3) . . ?
N2A Fe1 N14A 79.7(3) . . ?
N2A Fe1 N25A 103.1(4) . . ?
N2A Fe1 N30A 97.6(4) . . ?
N14A Fe1 N9A 159.1(3) . . ?
N14A Fe1 N25A 92.4(3) . . ?
N14A Fe1 N30A 90.2(3) . . ?
N18A Fe1 N2A 176.9(6) . . ?
N18A Fe1 N9A 100.5(3) . . ?
N18A Fe1 N14A 100.3(3) . . ?
N18A Fe1 N25A 80.0(3) . . ?
N18A Fe1 N30A 79.3(3) . . ?
N25A Fe1 N9A 93.8(4) . . ?
N25A Fe1 N30A 159.3(4) . . ?
N30A Fe1 N9A 91.0(3) . . ?
C3A N2A Fe1 120.6(4) . . ?
C3A N2A C7A 119.4(4) . . ?
C7A N2A Fe1 119.9(4) . . ?
N2A C3A C4A 122.1(6) . . ?
N2A C3A N8A 111.2(5) . . ?
N8A C3A C4A 126.7(6) . . ?
C3A C4A H4A 123.3 . . ?
C5A C4A C3A 113.5(7) . . ?
C5A C4A H4A 123.3 . . ?
C4A C5A H5A 118.0 . . ?
C4A C5A C6A 124.0(6) . . ?
C6A C5A H5A 118.0 . . ?
C5A C6A H6A 121.7 . . ?
C7A C6A C5A 116.5(5) . . ?
C7A C6A H6A 121.7 . . ?
N2A C7A C6A 124.3(4) . . ?
N2A C7A N13A 110.7(4) . . ?
C6A C7A N13A 124.9(4) . . ?
N9A N8A C3A 115.2(5) . . ?
C12A N8A C3A 133.2(5) . . ?
C12A N8A N9A 111.5(5) . . ?
N8A N9A Fe1 113.5(4) . . ?
C10A N9A Fe1 142.0(4) . . ?
C10A N9A N8A 104.5(4) . . ?
N9A C10A H10A 124.6 . . ?
N9A C10A C11A 110.9(4) . . ?
C11A C10A H10A 124.6 . . ?
C10A C11A H11A 127.0 . . ?
C12A C11A C10A 106.0(4) . . ?
C12A C11A H11A 127.0 . . ?
N8A C12A C11A 107.2(4) . . ?
N8A C12A H12A 126.4 . . ?
C11A C12A H12A 126.4 . . ?
N14A N13A C7A 115.8(4) . . ?
C17A N13A C7A 132.5(4) . . ?
C17A N13A N14A 111.6(3) . . ?
N13A N14A Fe1 113.8(3) . . ?
C15A N14A Fe1 141.1(4) . . ?
C15A N14A N13A 104.9(3) . . ?
N14A C15A H15A 124.7 . . ?
N14A C15A C16A 110.5(4) . . ?
C16A C15A H15A 124.7 . . ?
C15A C16A H16A 126.7 . . ?
C17A C16A C15A 106.6(4) . . ?
C17A C16A H16A 126.7 . . ?
N13A C17A H17A 126.8 . . ?
C16A C17A N13A 106.4(4) . . ?
C16A C17A H17A 126.8 . . ?
C19A N18A Fe1 120.2(5) . . ?
C23A N18A Fe1 120.2(4) . . ?
C23A N18A C19A 119.6(5) . . ?
N18A C19A C20A 120.8(6) . . ?
N18A C19A N24A 110.9(5) . . ?
N24A C19A C20A 128.3(6) . . ?
C19A C20A H20A 121.1 . . ?
C21A C20A C19A 117.8(7) . . ?
C21A C20A H20A 121.1 . . ?
C20A C21A H21A 119.3 . . ?
C20A C21A C22A 121.3(6) . . ?
C22A C21A H21A 119.3 . . ?
C21A C22A H22A 121.5 . . ?
C21A C22A C23A 116.9(5) . . ?
C23A C22A H22A 121.5 . . ?
N18A C23A C22A 123.5(5) . . ?
N18A C23A N29A 111.2(4) . . ?
C22A C23A N29A 125.3(5) . . ?
N25A N24A C19A 115.9(4) . . ?
C28A N24A C19A 133.4(5) . . ?
C28A N24A N25A 110.7(4) . . ?
N24A N25A Fe1 113.0(4) . . ?
C26A N25A Fe1 142.4(4) . . ?
C26A N25A N24A 104.3(4) . . ?
N25A C26A H26A 124.2 . . ?
N25A C26A C27A 111.6(4) . . ?
C27A C26A H26A 124.2 . . ?
C26A C27A H27A 127.1 . . ?
C28A C27A C26A 105.7(4) . . ?
C28A C27A H27A 127.1 . . ?
N24A C28A H28A 126.2 . . ?
C27A C28A N24A 107.7(4) . . ?
C27A C28A H28A 126.2 . . ?
N30A N29A C23A 115.9(4) . . ?
C33A N29A C23A 132.3(4) . . ?
C33A N29A N30A 111.7(4) . . ?
N29A N30A Fe1 113.5(3) . . ?
C31A N30A Fe1 141.1(4) . . ?
C31A N30A N29A 105.2(4) . . ?
N30A C31A H31A 124.6 . . ?
N30A C31A C32A 110.8(4) . . ?
C32A C31A H31A 124.6 . . ?
C31A C32A H32A 127.0 . . ?
C33A C32A C31A 106.0(3) . . ?
C33A C32A H32A 127.0 . . ?
N29A C33A C32A 106.3(4) . . ?
N29A C33A H33A 126.8 . . ?
C32A C33A H33A 126.8 . . ?
N2B Zn1 N9B 74.6(3) . . ?
N2B Zn1 N14B 74.7(3) . . ?
N2B Zn1 N18B 174.1(5) . . ?
N2B Zn1 N25B 111.2(4) . . ?
N2B Zn1 N30B 99.6(4) . . ?
N14B Zn1 N9B 149.3(3) . . ?
N14B Zn1 N25B 94.3(3) . . ?
N14B Zn1 N30B 90.9(3) . . ?
N18B Zn1 N9B 104.0(3) . . ?
N18B Zn1 N14B 106.5(3) . . ?
N18B Zn1 N25B 74.6(3) . . ?
N18B Zn1 N30B 74.7(3) . . ?
N25B Zn1 N9B 97.1(3) . . ?
N30B Zn1 N9B 93.7(3) . . ?
N30B Zn1 N25B 149.0(3) . . ?
C3B N2B Zn1 121.1(5) . . ?
C3B N2B C7B 117.3(5) . . ?
C7B N2B Zn1 121.5(4) . . ?
N2B C3B N8B 111.9(6) . . ?
C4B C3B N2B 124.9(8) . . ?
C4B C3B N8B 123.2(8) . . ?
C3B C4B H4B 120.4 . . ?
C3B C4B C5B 119.2(10) . . ?
C5B C4B H4B 120.4 . . ?
C4B C5B H5B 120.5 . . ?
C6B C5B C4B 118.9(7) . . ?
C6B C5B H5B 120.5 . . ?
C5B C6B H6B 121.5 . . ?
C7B C6B C5B 116.9(5) . . ?
C7B C6B H6B 121.5 . . ?
N2B C7B C6B 122.8(5) . . ?
N2B C7B N13B 111.0(5) . . ?
C6B C7B N13B 126.2(5) . . ?
N9B N8B C3B 120.5(6) . . ?
C12B N8B C3B 128.8(6) . . ?
C12B N8B N9B 110.7(5) . . ?
N8B N9B Zn1 111.6(4) . . ?
C10B N9B Zn1 142.9(4) . . ?
C10B N9B N8B 105.5(5) . . ?
N9B C10B H10B 124.1 . . ?
N9B C10B C11B 111.8(5) . . ?
C11B C10B H10B 124.1 . . ?
C10B C11B H11B 127.4 . . ?
C12B C11B C10B 105.2(4) . . ?
C12B C11B H11B 127.4 . . ?
N8B C12B C11B 106.9(5) . . ?
N8B C12B H12B 126.5 . . ?
C11B C12B H12B 126.5 . . ?
N14B N13B C7B 119.6(4) . . ?
C17B N13B C7B 130.2(4) . . ?
C17B N13B N14B 109.9(4) . . ?
N13B N14B Zn1 112.6(3) . . ?
C15B N14B Zn1 140.1(4) . . ?
C15B N14B N13B 105.8(4) . . ?
N14B C15B H15B 124.7 . . ?
N14B C15B C16B 110.5(4) . . ?
C16B C15B H15B 124.7 . . ?
C15B C16B H16B 127.0 . . ?
C17B C16B C15B 106.0(4) . . ?
C17B C16B H16B 127.0 . . ?
N13B C17B C16B 107.8(4) . . ?
N13B C17B H17B 126.1 . . ?
C16B C17B H17B 126.1 . . ?
C19B N18B Zn1 120.7(5) . . ?
C19B N18B C23B 118.8(5) . . ?
C23B N18B Zn1 120.5(5) . . ?
N18B C19B N24B 112.9(6) . . ?
C20B C19B N18B 124.0(7) . . ?
C20B C19B N24B 123.1(7) . . ?
C19B C20B H20B 121.0 . . ?
C19B C20B C21B 118.0(6) . . ?
C21B C20B H20B 121.0 . . ?
C20B C21B H21B 119.5 . . ?
C20B C21B C22B 120.9(6) . . ?
C22B C21B H21B 119.5 . . ?
C21B C22B H22B 121.8 . . ?
C23B C22B C21B 116.4(5) . . ?
C23B C22B H22B 121.8 . . ?
N18B C23B C22B 121.8(5) . . ?
N18B C23B N29B 112.5(5) . . ?
C22B C23B N29B 125.7(5) . . ?
N25B N24B C19B 119.3(5) . . ?
C28B N24B C19B 129.2(6) . . ?
C28B N24B N25B 111.3(5) . . ?
N24B N25B Zn1 112.5(4) . . ?
C26B N25B Zn1 142.2(4) . . ?
C26B N25B N24B 105.1(4) . . ?
N25B C26B H26B 124.8 . . ?
N25B C26B C27B 110.5(4) . . ?
C27B C26B H26B 124.8 . . ?
C26B C27B H27B 127.5 . . ?
C28B C27B C26B 105.0(4) . . ?
C28B C27B H27B 127.5 . . ?
N24B C28B C27B 108.0(5) . . ?
N24B C28B H28B 126.0 . . ?
C27B C28B H28B 126.0 . . ?
N30B N29B C23B 119.9(5) . . ?
C33B N29B C23B 129.8(5) . . ?
C33B N29B N30B 110.3(4) . . ?
N29B N30B Zn1 112.3(4) . . ?
C31B N30B Zn1 142.4(4) . . ?
C31B N30B N29B 105.2(4) . . ?
N30B C31B H31B 124.2 . . ?
N30B C31B C32B 111.5(5) . . ?
C32B C31B H31B 124.2 . . ?
C31B C32B H32B 127.0 . . ?
C33B C32B C31B 106.0(4) . . ?
C33B C32B H32B 127.0 . . ?
N29B C33B C32B 107.0(4) . . ?
N29B C33B H33B 126.5 . . ?
C32B C33B H33B 126.5 . . ?
F35 B34 F36 109.9(2) . . ?
F37 B34 F35 109.1(2) . . ?
F37 B34 F36 108.25(19) . . ?
F38 B34 F35 110.0(2) . . ?
F38 B34 F36 109.1(2) . . ?
F38 B34 F37 110.5(2) . . ?
F41A B39 F40A 105.3(5) . . ?
F42A B39 F40A 109.3(5) . . ?
F42A B39 F41A 111.2(4) . . ?
F42A B39 F43A 113.6(4) . . ?
F43A B39 F40A 106.4(4) . . ?
F43A B39 F41A 110.5(3) . . ?
F40B B39 F41B 123.2(10) . . ?
F40B B39 F42B 107.9(11) . . ?
F40B B39 F43B 113.1(10) . . ?
F41B B39 F42B 104.0(7) . . ?
F41B B39 F43B 105.2(5) . . ?
F43B B39 F42B 100.8(6) . . ?

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 N2A C3A C4A 177.8(6) . . . . ?
Fe1 N2A C3A N8A -1.3(8) . . . . ?
Fe1 N2A C7A C6A -179.2(5) . . . . ?
Fe1 N2A C7A N13A 0.4(6) . . . . ?
Fe1 N9A C10A C11A -180.0(6) . . . . ?
Fe1 N14A C15A C16A -173.2(5) . . . . ?
Fe1 N18A C19A C20A 177.9(6) . . . . ?
Fe1 N18A C19A N24A 0.3(7) . . . . ?
Fe1 N18A C23A C22A -178.5(5) . . . . ?
Fe1 N18A C23A N29A 1.8(6) . . . . ?
Fe1 N25A C26A C27A 172.5(5) . . . . ?
Fe1 N30A C31A C32A -175.8(5) . . . . ?
N2A C3A C4A C5A 1.3(11) . . . . ?
N2A C3A N8A N9A 1.7(7) . . . . ?
N2A C3A N8A C12A -179.9(6) . . . . ?
N2A C7A N13A N14A 1.6(5) . . . . ?
N2A C7A N13A C17A -176.1(5) . . . . ?
C3A N2A C7A C6A -2.8(8) . . . . ?
C3A N2A C7A N13A 176.9(5) . . . . ?
C3A C4A C5A C6A -2.8(11) . . . . ?
C3A N8A N9A Fe1 -1.3(7) . . . . ?
C3A N8A N9A C10A 178.6(5) . . . . ?
C3A N8A C12A C11A -178.4(6) . . . . ?
C4A C3A N8A N9A -177.4(7) . . . . ?
C4A C3A N8A C12A 1.0(11) . . . . ?
C4A C5A C6A C7A 1.7(9) . . . . ?
C5A C6A C7A N2A 1.3(7) . . . . ?
C5A C6A C7A N13A -178.3(4) . . . . ?
C6A C7A N13A N14A -178.7(4) . . . . ?
C6A C7A N13A C17A 3.6(7) . . . . ?
C7A N2A C3A C4A 1.4(10) . . . . ?
C7A N2A C3A N8A -177.8(5) . . . . ?
C7A N13A N14A Fe1 -2.8(5) . . . . ?
C7A N13A N14A C15A -178.8(3) . . . . ?
C7A N13A C17A C16A 177.8(4) . . . . ?
N8A C3A C4A C5A -179.7(6) . . . . ?
N8A N9A C10A C11A 0.1(5) . . . . ?
N9A N8A C12A C11A 0.1(6) . . . . ?
N9A C10A C11A C12A -0.1(5) . . . . ?
C10A C11A C12A N8A 0.0(5) . . . . ?
C12A N8A N9A Fe1 179.9(4) . . . . ?
C12A N8A N9A C10A -0.1(6) . . . . ?
N13A N14A C15A C16A 1.0(4) . . . . ?
N14A N13A C17A C16A 0.1(5) . . . . ?
N14A C15A C16A C17A -1.0(5) . . . . ?
C15A C16A C17A N13A 0.5(4) . . . . ?
C17A N13A N14A Fe1 175.3(4) . . . . ?
C17A N13A N14A C15A -0.7(4) . . . . ?
N18A C19A C20A C21A 1.6(11) . . . . ?
N18A C19A N24A N25A -1.3(7) . . . . ?
N18A C19A N24A C28A 175.2(6) . . . . ?
N18A C23A N29A N30A -2.2(6) . . . . ?
N18A C23A N29A C33A -177.2(5) . . . . ?
C19A N18A C23A C22A -0.8(8) . . . . ?
C19A N18A C23A N29A 179.5(5) . . . . ?
C19A C20A C21A C22A -2.9(11) . . . . ?
C19A N24A N25A Fe1 1.7(6) . . . . ?
C19A N24A N25A C26A 176.8(5) . . . . ?
C19A N24A C28A C27A -175.6(6) . . . . ?
C20A C19A N24A N25A -178.6(7) . . . . ?
C20A C19A N24A C28A -2.1(11) . . . . ?
C20A C21A C22A C23A 2.3(9) . . . . ?
C21A C22A C23A N18A -0.5(8) . . . . ?
C21A C22A C23A N29A 179.2(5) . . . . ?
C22A C23A N29A N30A 178.1(5) . . . . ?
C22A C23A N29A C33A 3.1(9) . . . . ?
C23A N18A C19A C20A 0.2(9) . . . . ?
C23A N18A C19A N24A -177.4(5) . . . . ?
C23A N29A N30A Fe1 1.7(6) . . . . ?
C23A N29A N30A C31A -174.6(4) . . . . ?
C23A N29A C33A C32A 174.1(5) . . . . ?
N24A C19A C20A C21A 178.7(6) . . . . ?
N24A N25A C26A C27A -0.1(5) . . . . ?
N25A N24A C28A C27A 1.1(6) . . . . ?
N25A C26A C27A C28A 0.7(5) . . . . ?
C26A C27A C28A N24A -1.1(6) . . . . ?
C28A N24A N25A Fe1 -175.7(4) . . . . ?
C28A N24A N25A C26A -0.6(5) . . . . ?
N29A N30A C31A C32A -1.3(5) . . . . ?
N30A N29A C33A C32A -1.0(5) . . . . ?
N30A C31A C32A C33A 0.7(5) . . . . ?
C31A C32A C33A N29A 0.2(5) . . . . ?
C33A N29A N30A Fe1 177.7(3) . . . . ?
C33A N29A N30A C31A 1.5(5) . . . . ?
Zn1 N2B C3B C4B -175.6(9) . . . . ?
Zn1 N2B C3B N8B 4.3(9) . . . . ?
Zn1 N2B C7B C6B 176.6(5) . . . . ?
Zn1 N2B C7B N13B -5.4(8) . . . . ?
Zn1 N9B C10B C11B -178.8(6) . . . . ?
Zn1 N14B C15B C16B -163.0(5) . . . . ?
Zn1 N18B C19B C20B -178.3(6) . . . . ?
Zn1 N18B C19B N24B 0.7(9) . . . . ?
Zn1 N18B C23B C22B 179.5(5) . . . . ?
Zn1 N18B C23B N29B -1.9(7) . . . . ?
Zn1 N25B C26B C27B 173.9(5) . . . . ?
Zn1 N30B C31B C32B 174.3(5) . . . . ?
N2B C3B C4B C5B -1.6(16) . . . . ?
N2B C3B N8B N9B -2.0(9) . . . . ?
N2B C3B N8B C12B 177.8(6) . . . . ?
N2B C7B N13B N14B 8.4(7) . . . . ?
N2B C7B N13B C17B -165.4(5) . . . . ?
C3B N2B C7B C6B 1.0(10) . . . . ?
C3B N2B C7B N13B 179.1(6) . . . . ?
C3B C4B C5B C6B 2.3(14) . . . . ?
C3B N8B N9B Zn1 -0.9(7) . . . . ?
C3B N8B N9B C10B 179.3(6) . . . . ?
C3B N8B C12B C11B -179.8(6) . . . . ?
C4B C3B N8B N9B 177.9(9) . . . . ?
C4B C3B N8B C12B -2.3(13) . . . . ?
C4B C5B C6B C7B -1.4(10) . . . . ?
C5B C6B C7B N2B -0.2(8) . . . . ?
C5B C6B C7B N13B -178.0(5) . . . . ?
C6B C7B N13B N14B -173.6(5) . . . . ?
C6B C7B N13B C17B 12.7(9) . . . . ?
C7B N2B C3B C4B 0.0(13) . . . . ?
C7B N2B C3B N8B 179.9(6) . . . . ?
C7B N13B N14B Zn1 -7.5(6) . . . . ?
C7B N13B N14B C15B -176.3(4) . . . . ?
C7B N13B C17B C16B 175.7(5) . . . . ?
N8B C3B C4B C5B 178.5(8) . . . . ?
N8B N9B C10B C11B 0.9(6) . . . . ?
N9B N8B C12B C11B 0.0(6) . . . . ?
N9B C10B C11B C12B -0.9(6) . . . . ?
C10B C11B C12B N8B 0.5(6) . . . . ?
C12B N8B N9B Zn1 179.3(4) . . . . ?
C12B N8B N9B C10B -0.5(6) . . . . ?
N13B N14B C15B C16B 0.7(5) . . . . ?
N14B N13B C17B C16B 1.5(5) . . . . ?
N14B C15B C16B C17B 0.1(6) . . . . ?
C15B C16B C17B N13B -1.0(5) . . . . ?
C17B N13B N14B Zn1 167.4(4) . . . . ?
C17B N13B N14B C15B -1.4(5) . . . . ?
N18B C19B C20B C21B -2.2(12) . . . . ?
N18B C19B N24B N25B -0.3(9) . . . . ?
N18B C19B N24B C28B 174.0(6) . . . . ?
N18B C23B N29B N30B -1.9(7) . . . . ?
N18B C23B N29B C33B 178.8(5) . . . . ?
C19B N18B C23B C22B -0.4(9) . . . . ?
C19B N18B C23B N29B 178.2(6) . . . . ?
C19B C20B C21B C22B 1.6(10) . . . . ?
C19B N24B N25B Zn1 -0.2(7) . . . . ?
C19B N24B N25B C26B 176.1(6) . . . . ?
C19B N24B C28B C27B -175.6(7) . . . . ?
C20B C19B N24B N25B 178.7(7) . . . . ?
C20B C19B N24B C28B -7.0(12) . . . . ?
C20B C21B C22B C23B -0.4(9) . . . . ?
C21B C22B C23B N18B -0.1(9) . . . . ?
C21B C22B C23B N29B -178.6(6) . . . . ?
C22B C23B N29B N30B 176.7(6) . . . . ?
C22B C23B N29B C33B -2.6(10) . . . . ?
C23B N18B C19B C20B 1.7(11) . . . . ?
C23B N18B C19B N24B -179.3(6) . . . . ?
C23B N29B N30B Zn1 4.4(6) . . . . ?
C23B N29B N30B C31B -179.1(5) . . . . ?
C23B N29B C33B C32B 179.2(5) . . . . ?
N24B C19B C20B C21B 178.9(7) . . . . ?
N24B N25B C26B C27B -0.4(6) . . . . ?
N25B N24B C28B C27B -0.9(7) . . . . ?
N25B C26B C27B C28B -0.1(6) . . . . ?
C26B C27B C28B N24B 0.6(6) . . . . ?
C28B N24B N25B Zn1 -175.4(4) . . . . ?
C28B N24B N25B C26B 0.8(6) . . . . ?
N29B N30B C31B C32B -0.3(6) . . . . ?
N30B N29B C33B C32B -0.2(6) . . . . ?
N30B C31B C32B C33B 0.2(6) . . . . ?
C31B C32B C33B N29B 0.0(5) . . . . ?
C33B N29B N30B Zn1 -176.2(4) . . . . ?
C33B N29B N30B C31B 0.3(6) . . . . ?

_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_pg14ht
_database_code_depnum_ccdc_archive 'CCDC 2261789'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2023-05-09 deposited with the CCDC.	2023-08-30 downloaded from the CCDC.
;
_audit_creation_date             2023-03-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis[2,6-di(pyrazol-1-yl)pyridine]iron(II) bis[2,6-di(pyrazol-1-yl)pyridine]-ruthenium(II) ditetrafluoroborate 0.50:0.50 solid solution'
_chemical_formula_moiety         'C22 H18 Fe0.5 N10 Ru0.5, 2(B F4)'
_chemical_formula_sum            'C22 H18 B2 F8 Fe0.50 N10 Ru0.50'
_chemical_formula_weight         674.54
_chemical_absolute_configuration ab
_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 0.0019 0.0015 '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 0.0004 0.0006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0124 0.0097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.2961 0.8007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0037 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.5177 0.7911 '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           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   8.5460(1)
_cell_length_b                   8.5956(1)
_cell_length_c                   18.9251(2)
_cell_angle_alpha                90
_cell_angle_beta                 95.794(1)
_cell_angle_gamma                90
_cell_volume                     1383.10(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8292
_cell_measurement_temperature    300.15
_cell_measurement_theta_max      29.16
_cell_measurement_theta_min      1.04
_exptl_absorpt_coefficient_mu    0.596
_exptl_absorpt_correction_T_min  0.937
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
DIALS 3.12.1-2-g1c07bc2b3-release
Scaling & analysis of unmerged intensities, absorption correction using 
spherical harmonics
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             674
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17097
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        24.620
_diffrn_reflns_theta_max         27.993
_diffrn_reflns_theta_min         1.048
_diffrn_ambient_temperature      300.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_measurement_device       'Fixed χ 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_reflns_Friedel_coverage         0.783
_reflns_Friedel_fraction_full    0.942
_reflns_Friedel_fraction_max     0.884
_reflns_number_gt                5094
_reflns_number_total             6919
_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       'XIA2 0.4.0.438-g4431aaa (Winter, 2010)'
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction        'XIA2 0.4.0.438-g4431aaa (Winter, 2010)'
_computing_molecular_graphics    'XSEED (Barbour, 2020)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 
;
 Flack x determined using 1714 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.025(19)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         6919
_refine_ls_number_restraints     61
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0500
_refine_ls_restrained_S_all      1.094
_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)+(0.0636P)²+0.3657P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1422
_refine_special_details          
;
 Unlike the low temperature structure, separate partial [Fe(bpp)₂]2+
 and [Ru(bpp)₂]2+ molecule sites could not be refined at this temperature.
 Hence, the organic ligand framework was modelled as crystallographically
 ordered. Attempts to distinguish Fe and Zn half-atoms in the Fourier map
 were also unproductive, so a mixed Fe~0.50~/Ru~0.50~ metal site was 
 refined with the same atomic coordinates, but independently refined 
 displacement parameters. The metal occupancies from the 100 K structure
 were used, since these could be accurately refined.

 The F atoms of both anions are also disordered, over three sites with a
 0.50:0.25:0.25 occupancy ratio. These were treated with the refined
 distance restraints listed below. An EADP thermal parameter constraint
 between the two partial metal atoms was also required to make the
 refinement converge.

 All crystallographically ordered non-H atoms plus the partial metal sites 
 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
2. Restrained distances
 B34-F35A = B34-F36A = B34-F37A = B34-F38A
 1.38649 with sigma of 0.02
 B34-F35B = B34-F36B = B34-F37B = B34-F38B
 1.38649 with sigma of 0.02
 B34-F35C = B34-F36C = B34-F37C = B34-F38C
 1.38649 with sigma of 0.02
 B39-F40A = B39-F41A = B39-F42A = B39-F43A
 1.38649 with sigma of 0.02
 B39-F40B = B39-F41B = B39-F42B = B39-F43B
 1.38649 with sigma of 0.02
 B39-F40C = B39-F41C = B39-F42C = B39-F43C
 1.38649 with sigma of 0.02
 F35A-F36A = F35A-F37A = F35A-F38A = F36A-F37A = F36A-F38A = F37A-F38A
 2.264138 with sigma of 0.02
 F35B-F36B = F35B-F37B = F35B-F38B = F36B-F37B = F36B-F38B = F37B-F38B
 2.264138 with sigma of 0.02
 F35C-F36C = F35C-F37C = F35C-F38C = F36C-F37C = F36C-F38C = F37C-F38C
 2.264138 with sigma of 0.02
 F40A-F41A = F40A-F42A = F40A-F43A = F41A-F42A = F41A-F43A = F42A-F43A
 2.264138 with sigma of 0.02
 F40B-F41B = F40B-F42B = F40B-F43B = F41B-F42B = F41B-F43B = F42B-F43B
 2.264138 with sigma of 0.02
 F40C-F41C = F40C-F42C = F40C-F43C = F41C-F42C = F41C-F43C = F42C-F43C
 2.264138 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Fe1) = Uanis(Ru1)
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)
 X(Fe1)=X(Ru1)=FVAR(2)
 Y(Fe1)=Y(Ru1)=FVAR(3)
 Z(Fe1)=Z(Ru1)=FVAR(4)
 Fixed Sof: Fe1(0.5) Ru1(0.5) F35A(0.5) F36A(0.5) F37A(0.5) F38A(0.5)
 F35B(0.25) F36B(0.25) F37B(0.25) F38B(0.25) F35C(0.25) F36C(0.25) F37C(0.25)
 F38C(0.25) F40A(0.5) F41A(0.5) F42A(0.5) F43A(0.5) F40B(0.25) F41B(0.25)
 F42B(0.25) F43B(0.25) F40C(0.25) F41C(0.25) F42C(0.25) F43C(0.25)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16),
 C17(H17), C20(H20), C21(H21), C22(H22), C26(H26), C27(H27), C28(H28), C31(H31),
  C32(H32), C33(H33)
;
_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 0.72753(6) 0.81176(10) 0.74758(2) 0.06447(19) Uani 0.5 1 d . . P A 1
Ru1 Ru 0.72753(6) 0.81176(10) 0.74758(2) 0.06447(19) Uani 0.5 1 d . . P A 2
N2 N 0.7183(5) 0.8206(10) 0.6387(2) 0.0656(10) Uani 1 1 d . . . . .
C3 C 0.5925(7) 0.8773(7) 0.6001(3) 0.0696(14) Uani 1 1 d . . . . .
C4 C 0.5824(9) 0.8866(9) 0.5274(4) 0.0861(19) Uani 1 1 d . . . . .
H4 H 0.493743 0.927408 0.501327 0.103 Uiso 1 1 calc R U . . .
C5 C 0.7083(11) 0.8333(12) 0.4945(4) 0.097(2) Uani 1 1 d . . . . .
H5 H 0.704783 0.837722 0.445311 0.116 Uiso 1 1 calc R U . . .
C6 C 0.8385(10) 0.7738(9) 0.5330(4) 0.089(2) Uani 1 1 d . . . . .
H6 H 0.923480 0.737068 0.510865 0.107 Uiso 1 1 calc R U . . .
C7 C 0.8393(7) 0.7702(7) 0.6051(3) 0.0712(15) Uani 1 1 d . . . . .
N8 N 0.4748(6) 0.9242(6) 0.6428(3) 0.0721(12) Uani 1 1 d . . . . .
N9 N 0.5018(6) 0.9079(6) 0.7154(3) 0.0714(12) Uani 1 1 d . . . . .
C10 C 0.3738(8) 0.9578(8) 0.7404(4) 0.0819(18) Uani 1 1 d . . . . .
H10 H 0.357617 0.958599 0.788266 0.098 Uiso 1 1 calc R U . . .
C11 C 0.2648(9) 1.0095(10) 0.6856(5) 0.102(2) Uani 1 1 d . . . . .
H11 H 0.166046 1.051545 0.690098 0.122 Uiso 1 1 calc R U . . .
C12 C 0.3309(8) 0.9866(8) 0.6251(5) 0.090(2) Uani 1 1 d . . . . .
H12 H 0.286011 1.009310 0.579401 0.107 Uiso 1 1 calc R U . . .
N13 N 0.9609(6) 0.7107(6) 0.6531(3) 0.0781(14) Uani 1 1 d . . . . .
N14 N 0.9459(6) 0.7195(7) 0.7250(3) 0.0796(14) Uani 1 1 d . . . . .
C15 C 1.0729(9) 0.6510(10) 0.7562(5) 0.099(2) Uani 1 1 d . . . . .
H15 H 1.094547 0.637918 0.805014 0.119 Uiso 1 1 calc R U . . .
C16 C 1.1688(10) 0.6017(11) 0.7065(7) 0.126(4) Uani 1 1 d . . . . .
H16 H 1.265726 0.552720 0.715697 0.151 Uiso 1 1 calc R U . . .
C17 C 1.0953(10) 0.6379(10) 0.6415(6) 0.106(3) Uani 1 1 d . . . . .
H17 H 1.130968 0.616629 0.597653 0.127 Uiso 1 1 calc R U . . .
N18 N 0.7309(5) 0.7947(9) 0.8563(2) 0.0642(12) Uani 1 1 d . . . . .
C19 C 0.7846(7) 0.9086(8) 0.8989(3) 0.0684(14) Uani 1 1 d . . . . .
C20 C 0.7879(9) 0.9013(10) 0.9713(4) 0.0844(18) Uani 1 1 d . . . . .
H20 H 0.826391 0.982860 1.000288 0.101 Uiso 1 1 calc R U . . .
C21 C 0.7307(10) 0.7655(10) 0.9992(4) 0.093(3) Uani 1 1 d . . . . .
H21 H 0.729421 0.756200 1.048118 0.112 Uiso 1 1 calc R U . . .
C22 C 0.6763(8) 0.6455(10) 0.9563(4) 0.088(2) Uani 1 1 d . . . . .
H22 H 0.639612 0.553941 0.974959 0.105 Uiso 1 1 calc R U . . .
C23 C 0.6781(7) 0.6654(8) 0.8847(4) 0.0715(15) Uani 1 1 d . . . . .
N24 N 0.8393(6) 1.0358(7) 0.8607(3) 0.0744(13) Uani 1 1 d . . . . .
N25 N 0.8276(6) 1.0257(7) 0.7875(3) 0.0746(13) Uani 1 1 d . . . . .
C26 C 0.8934(9) 1.1552(9) 0.7676(5) 0.092(2) Uani 1 1 d . . . . .
H26 H 0.901452 1.183136 0.720670 0.111 Uiso 1 1 calc R U . . .
C27 C 0.9496(10) 1.2454(10) 0.8267(5) 0.104(2) Uani 1 1 d . . . . .
H27 H 1.002904 1.339682 0.826293 0.125 Uiso 1 1 calc R U . . .
C28 C 0.9108(9) 1.1679(10) 0.8833(5) 0.097(2) Uani 1 1 d . . . . .
H28 H 0.930080 1.199912 0.930309 0.116 Uiso 1 1 calc R U . . .
N29 N 0.6252(6) 0.5541(6) 0.8321(3) 0.0767(13) Uani 1 1 d . . . . .
N30 N 0.6390(6) 0.5874(7) 0.7629(3) 0.0779(14) Uani 1 1 d . . . . .
C31 C 0.5873(9) 0.4603(9) 0.7275(5) 0.097(2) Uani 1 1 d . . . . .
H31 H 0.584635 0.448596 0.678580 0.116 Uiso 1 1 calc R U . . .
C32 C 0.5395(10) 0.3510(9) 0.7715(6) 0.113(3) Uani 1 1 d . . . . .
H32 H 0.498420 0.253676 0.758692 0.136 Uiso 1 1 calc R U . . .
C33 C 0.5630(10) 0.4106(9) 0.8385(6) 0.106(3) Uani 1 1 d . . . . .
H33 H 0.540791 0.362218 0.880306 0.127 Uiso 1 1 calc R U . . .
B34 B 0.7977(11) 0.2703(10) 0.5724(4) 0.094(3) Uani 1 1 d D . . . .
F35A F 0.6755(19) 0.233(2) 0.6101(9) 0.116(7) Uiso 0.5 1 d D . P B 1
F36A F 0.7463(16) 0.2110(16) 0.4996(6) 0.111(4) Uiso 0.5 1 d D . P B 1
F37A F 0.8082(17) 0.4232(13) 0.5569(7) 0.131(5) Uiso 0.5 1 d D . P B 1
F38A F 0.9368(15) 0.2074(19) 0.5965(8) 0.130(5) Uiso 0.5 1 d D . P B 1
F35B F 0.711(2) 0.189(2) 0.6168(10) 0.084(5) Uiso 0.25 1 d D . P B 2
F36B F 0.9531(16) 0.279(2) 0.6094(8) 0.095(5) Uiso 0.25 1 d D . P B 2
F37B F 0.803(3) 0.212(3) 0.5083(8) 0.095(6) Uiso 0.25 1 d D . P B 2
F38B F 0.752(2) 0.4300(15) 0.5740(9) 0.078(4) Uiso 0.25 1 d D . P B 2
F35C F 0.651(2) 0.220(3) 0.5955(12) 0.080(6) Uiso 0.25 1 d D . P B 3
F36C F 0.901(2) 0.146(2) 0.5867(10) 0.101(6) Uiso 0.25 1 d D . P B 3
F37C F 0.786(3) 0.306(4) 0.5034(9) 0.144(8) Uiso 0.25 1 d D . P B 3
F38C F 0.848(4) 0.398(3) 0.6135(15) 0.176(12) Uiso 0.25 1 d D . P B 3
B39 B 0.7379(12) 0.2780(11) 1.0698(5) 0.108(3) Uani 1 1 d D . . . .
F40A F 0.6576(15) 0.2517(15) 0.9964(5) 0.100(4) Uiso 0.5 1 d D . P C 1
F41A F 0.6820(17) 0.1513(14) 1.1043(7) 0.099(4) Uiso 0.5 1 d D . P C 1
F42A F 0.8820(12) 0.2711(15) 1.0603(6) 0.122(4) Uiso 0.5 1 d D . P C 1
F43A F 0.682(2) 0.4139(16) 1.0957(8) 0.150(5) Uiso 0.5 1 d D . P C 1
F40B F 0.873(2) 0.351(3) 1.1023(13) 0.153(9) Uiso 0.25 1 d D . P C 2
F41B F 0.740(3) 0.282(3) 0.9981(8) 0.137(9) Uiso 0.25 1 d D . P C 2
F42B F 0.722(3) 0.130(2) 1.0945(14) 0.135(13) Uiso 0.25 1 d D . P C 2
F43B F 0.616(2) 0.379(2) 1.0881(11) 0.110(7) Uiso 0.25 1 d D . P C 2
F40C F 0.662(2) 0.220(2) 1.1233(8) 0.087(5) Uiso 0.25 1 d D . P C 3
F41C F 0.794(2) 0.4265(18) 1.0983(9) 0.097(5) Uiso 0.25 1 d D . P C 3
F42C F 0.8905(16) 0.193(2) 1.0716(8) 0.084(4) Uiso 0.25 1 d D . P C 3
F43C F 0.662(2) 0.297(3) 1.0056(8) 0.095(7) Uiso 0.25 1 d D . P C 3


_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 2.055(4) . ?
Fe1 N9 2.130(5) . ?
Fe1 N14 2.110(6) . ?
Fe1 N18 2.060(4) . ?
Fe1 N25 2.134(6) . ?
Fe1 N30 2.103(6) . ?
Ru1 N2 2.055(4) . ?
Ru1 N9 2.130(5) . ?
Ru1 N14 2.110(6) . ?
Ru1 N18 2.060(4) . ?
Ru1 N25 2.134(6) . ?
Ru1 N30 2.103(6) . ?
N2 C3 1.329(8) . ?
N2 C7 1.339(8) . ?
C3 C4 1.373(9) . ?
C3 N8 1.411(8) . ?
C4 H4 0.9300 . ?
C4 C5 1.374(11) . ?
C5 H5 0.9300 . ?
C5 C6 1.366(12) . ?
C6 H6 0.9300 . ?
C6 C7 1.364(10) . ?
C7 N13 1.406(9) . ?
N8 N9 1.377(7) . ?
N8 C12 1.353(8) . ?
N9 C10 1.308(8) . ?
C10 H10 0.9300 . ?
C10 C11 1.395(11) . ?
C11 H11 0.9300 . ?
C11 C12 1.342(12) . ?
C12 H12 0.9300 . ?
N13 N14 1.383(8) . ?
N13 C17 1.345(9) . ?
N14 C15 1.321(9) . ?
C15 H15 0.9300 . ?
C15 C16 1.375(13) . ?
C16 H16 0.9300 . ?
C16 C17 1.361(14) . ?
C17 H17 0.9300 . ?
N18 C19 1.320(9) . ?
N18 C23 1.333(10) . ?
C19 C20 1.370(9) . ?
C19 N24 1.415(8) . ?
C20 H20 0.9300 . ?
C20 C21 1.390(11) . ?
C21 H21 0.9300 . ?
C21 C22 1.365(11) . ?
C22 H22 0.9300 . ?
C22 C23 1.367(9) . ?
C23 N29 1.422(9) . ?
N24 N25 1.382(7) . ?
N24 C28 1.339(9) . ?
N25 C26 1.319(9) . ?
C26 H26 0.9300 . ?
C26 C27 1.404(12) . ?
C27 H27 0.9300 . ?
C27 C28 1.332(11) . ?
C28 H28 0.9300 . ?
N29 N30 1.357(8) . ?
N29 C33 1.354(9) . ?
N30 C31 1.333(9) . ?
C31 H31 0.9300 . ?
C31 C32 1.345(12) . ?
C32 H32 0.9300 . ?
C32 C33 1.363(13) . ?
C33 H33 0.9300 . ?
B34 F35A 1.360(14) . ?
B34 F36A 1.492(13) . ?
B34 F37A 1.352(13) . ?
B34 F38A 1.343(14) . ?
B34 F35B 1.369(15) . ?
B34 F36B 1.440(15) . ?
B34 F37B 1.317(15) . ?
B34 F38B 1.429(15) . ?
B34 F35C 1.436(16) . ?
B34 F36C 1.397(16) . ?
B34 F37C 1.335(16) . ?
B34 F38C 1.392(18) . ?
B39 F40A 1.503(13) . ?
B39 F41A 1.380(13) . ?
B39 F42A 1.264(12) . ?
B39 F43A 1.370(14) . ?
B39 F40B 1.405(18) . ?
B39 F41B 1.359(17) . ?
B39 F42B 1.365(18) . ?
B39 F43B 1.429(17) . ?
B39 F40C 1.352(15) . ?
B39 F41C 1.449(16) . ?
B39 F42C 1.493(15) . ?
B39 F43C 1.327(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 75.9(2) . . ?
N2 Fe1 N14 75.9(2) . . ?
N2 Fe1 N18 177.6(3) . . ?
N2 Fe1 N25 107.2(3) . . ?
N2 Fe1 N30 101.2(3) . . ?
N9 Fe1 N25 94.9(2) . . ?
N14 Fe1 N9 151.8(2) . . ?
N14 Fe1 N25 93.7(2) . . ?
N18 Fe1 N9 103.6(2) . . ?
N18 Fe1 N14 104.6(2) . . ?
N18 Fe1 N25 75.1(2) . . ?
N18 Fe1 N30 76.4(3) . . ?
N30 Fe1 N9 93.9(2) . . ?
N30 Fe1 N14 91.2(2) . . ?
N30 Fe1 N25 151.5(2) . . ?
N2 Ru1 N9 75.9(2) . . ?
N2 Ru1 N14 75.9(2) . . ?
N2 Ru1 N18 177.6(3) . . ?
N2 Ru1 N25 107.2(3) . . ?
N2 Ru1 N30 101.2(3) . . ?
N9 Ru1 N25 94.9(2) . . ?
N14 Ru1 N9 151.8(2) . . ?
N14 Ru1 N25 93.7(2) . . ?
N18 Ru1 N9 103.6(2) . . ?
N18 Ru1 N14 104.6(2) . . ?
N18 Ru1 N25 75.1(2) . . ?
N18 Ru1 N30 76.4(3) . . ?
N30 Ru1 N9 93.9(2) . . ?
N30 Ru1 N14 91.2(2) . . ?
N30 Ru1 N25 151.5(2) . . ?
C3 N2 Fe1 120.8(4) . . ?
C3 N2 Ru1 120.8(4) . . ?
C3 N2 C7 118.5(5) . . ?
C7 N2 Fe1 120.7(4) . . ?
C7 N2 Ru1 120.7(4) . . ?
N2 C3 C4 122.5(6) . . ?
N2 C3 N8 112.0(5) . . ?
C4 C3 N8 125.5(6) . . ?
C3 C4 H4 121.3 . . ?
C5 C4 C3 117.4(7) . . ?
C5 C4 H4 121.3 . . ?
C4 C5 H5 119.5 . . ?
C6 C5 C4 121.1(6) . . ?
C6 C5 H5 119.5 . . ?
C5 C6 H6 121.2 . . ?
C7 C6 C5 117.6(7) . . ?
C7 C6 H6 121.2 . . ?
N2 C7 C6 122.8(6) . . ?
N2 C7 N13 111.6(5) . . ?
C6 C7 N13 125.6(6) . . ?
N9 N8 C3 119.0(5) . . ?
C12 N8 C3 130.9(6) . . ?
C12 N8 N9 110.1(6) . . ?
N8 N9 Fe1 112.4(4) . . ?
N8 N9 Ru1 112.4(4) . . ?
C10 N9 Fe1 142.2(5) . . ?
C10 N9 Ru1 142.2(5) . . ?
C10 N9 N8 105.4(6) . . ?
N9 C10 H10 124.6 . . ?
N9 C10 C11 110.8(7) . . ?
C11 C10 H10 124.6 . . ?
C10 C11 H11 126.8 . . ?
C12 C11 C10 106.3(7) . . ?
C12 C11 H11 126.8 . . ?
N8 C12 H12 126.4 . . ?
C11 C12 N8 107.3(7) . . ?
C11 C12 H12 126.4 . . ?
N14 N13 C7 118.7(5) . . ?
C17 N13 C7 130.7(7) . . ?
C17 N13 N14 110.6(7) . . ?
N13 N14 Fe1 113.1(4) . . ?
N13 N14 Ru1 113.1(4) . . ?
C15 N14 Fe1 141.4(6) . . ?
C15 N14 Ru1 141.4(6) . . ?
C15 N14 N13 105.2(6) . . ?
N14 C15 H15 124.7 . . ?
N14 C15 C16 110.6(9) . . ?
C16 C15 H15 124.7 . . ?
C15 C16 H16 126.4 . . ?
C17 C16 C15 107.2(8) . . ?
C17 C16 H16 126.4 . . ?
N13 C17 C16 106.4(9) . . ?
N13 C17 H17 126.8 . . ?
C16 C17 H17 126.8 . . ?
C19 N18 Fe1 121.7(5) . . ?
C19 N18 Ru1 121.7(5) . . ?
C19 N18 C23 118.9(5) . . ?
C23 N18 Fe1 119.4(5) . . ?
C23 N18 Ru1 119.4(5) . . ?
N18 C19 C20 123.2(6) . . ?
N18 C19 N24 112.0(5) . . ?
C20 C19 N24 124.8(6) . . ?
C19 C20 H20 121.7 . . ?
C19 C20 C21 116.5(7) . . ?
C21 C20 H20 121.7 . . ?
C20 C21 H21 119.3 . . ?
C22 C21 C20 121.3(7) . . ?
C22 C21 H21 119.3 . . ?
C21 C22 H22 121.4 . . ?
C21 C22 C23 117.2(7) . . ?
C23 C22 H22 121.4 . . ?
N18 C23 C22 122.9(7) . . ?
N18 C23 N29 112.0(6) . . ?
C22 C23 N29 125.1(6) . . ?
N25 N24 C19 118.0(5) . . ?
C28 N24 C19 131.0(6) . . ?
C28 N24 N25 110.9(6) . . ?
N24 N25 Fe1 113.2(4) . . ?
N24 N25 Ru1 113.2(4) . . ?
C26 N25 Fe1 142.5(5) . . ?
C26 N25 Ru1 142.5(5) . . ?
C26 N25 N24 104.1(6) . . ?
N25 C26 H26 124.4 . . ?
N25 C26 C27 111.1(7) . . ?
C27 C26 H26 124.4 . . ?
C26 C27 H27 127.1 . . ?
C28 C27 C26 105.7(7) . . ?
C28 C27 H27 127.1 . . ?
N24 C28 H28 126.0 . . ?
C27 C28 N24 108.1(7) . . ?
C27 C28 H28 126.0 . . ?
N30 N29 C23 118.8(5) . . ?
C33 N29 C23 130.6(7) . . ?
C33 N29 N30 110.6(7) . . ?
N29 N30 Fe1 113.2(4) . . ?
N29 N30 Ru1 113.2(4) . . ?
C31 N30 Fe1 142.0(6) . . ?
C31 N30 Ru1 142.0(6) . . ?
C31 N30 N29 104.8(6) . . ?
N30 C31 H31 124.2 . . ?
N30 C31 C32 111.6(8) . . ?
C32 C31 H31 124.2 . . ?
C31 C32 H32 126.6 . . ?
C31 C32 C33 106.7(7) . . ?
C33 C32 H32 126.6 . . ?
N29 C33 C32 106.3(8) . . ?
N29 C33 H33 126.8 . . ?
C32 C33 H33 126.8 . . ?
F35A B34 F36A 103.6(10) . . ?
F37A B34 F35A 114.3(12) . . ?
F37A B34 F36A 98.8(9) . . ?
F38A B34 F35A 115.4(11) . . ?
F38A B34 F36A 110.1(10) . . ?
F38A B34 F37A 112.9(12) . . ?
F35B B34 F36B 105.0(12) . . ?
F35B B34 F38B 107.9(12) . . ?
F37B B34 F35B 116.3(14) . . ?
F37B B34 F36B 110.6(13) . . ?
F37B B34 F38B 114.9(13) . . ?
F38B B34 F36B 100.5(11) . . ?
F36C B34 F35C 105.5(12) . . ?
F37C B34 F35C 112.8(14) . . ?
F37C B34 F36C 110.4(14) . . ?
F37C B34 F38C 110.5(16) . . ?
F38C B34 F35C 107.3(15) . . ?
F38C B34 F36C 110.0(15) . . ?
F41A B39 F40A 99.8(9) . . ?
F42A B39 F40A 102.8(9) . . ?
F42A B39 F41A 114.8(11) . . ?
F42A B39 F43A 118.0(12) . . ?
F43A B39 F40A 108.4(11) . . ?
F43A B39 F41A 110.7(11) . . ?
F40B B39 F43B 102.1(14) . . ?
F41B B39 F40B 109.4(15) . . ?
F41B B39 F42B 112.1(16) . . ?
F41B B39 F43B 108.2(14) . . ?
F42B B39 F40B 112.1(16) . . ?
F42B B39 F43B 112.5(15) . . ?
F40C B39 F41C 102.4(12) . . ?
F40C B39 F42C 106.5(11) . . ?
F41C B39 F42C 99.6(12) . . ?
F43C B39 F40C 120.4(14) . . ?
F43C B39 F41C 110.1(14) . . ?
F43C B39 F42C 115.2(13) . . ?

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 179.4(5) . . . . ?
Fe1 N2 C3 N8 -0.9(8) . . . . ?
Fe1 N2 C7 C6 180.0(5) . . . . ?
Fe1 N2 C7 N13 1.8(8) . . . . ?
Fe1 N9 C10 C11 179.7(6) . . . . ?
Fe1 N14 C15 C16 172.4(6) . . . . ?
Fe1 N18 C19 C20 179.7(5) . . . . ?
Fe1 N18 C19 N24 -1.1(7) . . . . ?
Fe1 N18 C23 C22 -179.9(5) . . . . ?
Fe1 N18 C23 N29 0.0(7) . . . . ?
Fe1 N25 C26 C27 -173.6(6) . . . . ?
Fe1 N30 C31 C32 -177.9(6) . . . . ?
Ru1 N2 C3 C4 179.4(5) . . . . ?
Ru1 N2 C3 N8 -0.9(8) . . . . ?
Ru1 N2 C7 C6 180.0(5) . . . . ?
Ru1 N2 C7 N13 1.8(8) . . . . ?
Ru1 N9 C10 C11 179.7(6) . . . . ?
Ru1 N14 C15 C16 172.4(6) . . . . ?
Ru1 N18 C19 C20 179.7(5) . . . . ?
Ru1 N18 C19 N24 -1.1(7) . . . . ?
Ru1 N18 C23 C22 -179.9(5) . . . . ?
Ru1 N18 C23 N29 0.0(7) . . . . ?
Ru1 N25 C26 C27 -173.6(6) . . . . ?
Ru1 N30 C31 C32 -177.9(6) . . . . ?
N2 C3 C4 C5 0.5(11) . . . . ?
N2 C3 N8 N9 0.4(8) . . . . ?
N2 C3 N8 C12 -179.8(7) . . . . ?
N2 C7 N13 N14 -3.7(8) . . . . ?
N2 C7 N13 C17 173.9(8) . . . . ?
C3 N2 C7 C6 -0.4(11) . . . . ?
C3 N2 C7 N13 -178.6(6) . . . . ?
C3 C4 C5 C6 -0.2(13) . . . . ?
C3 N8 N9 Fe1 0.3(6) . . . . ?
C3 N8 N9 Ru1 0.3(6) . . . . ?
C3 N8 N9 C10 -179.1(5) . . . . ?
C3 N8 C12 C11 179.7(7) . . . . ?
C4 C3 N8 N9 -179.9(6) . . . . ?
C4 C3 N8 C12 -0.1(11) . . . . ?
C4 C5 C6 C7 -0.4(13) . . . . ?
C5 C6 C7 N2 0.7(11) . . . . ?
C5 C6 C7 N13 178.6(7) . . . . ?
C6 C7 N13 N14 178.2(6) . . . . ?
C6 C7 N13 C17 -4.2(11) . . . . ?
C7 N2 C3 C4 -0.3(11) . . . . ?
C7 N2 C3 N8 179.5(6) . . . . ?
C7 N13 N14 Fe1 3.8(7) . . . . ?
C7 N13 N14 Ru1 3.8(7) . . . . ?
C7 N13 N14 C15 178.0(6) . . . . ?
C7 N13 C17 C16 -178.6(7) . . . . ?
N8 C3 C4 C5 -179.1(7) . . . . ?
N8 N9 C10 C11 -1.3(8) . . . . ?
N9 N8 C12 C11 -0.4(8) . . . . ?
N9 C10 C11 C12 1.1(9) . . . . ?
C10 C11 C12 N8 -0.4(9) . . . . ?
C12 N8 N9 Fe1 -179.6(4) . . . . ?
C12 N8 N9 Ru1 -179.6(4) . . . . ?
C12 N8 N9 C10 1.1(7) . . . . ?
N13 N14 C15 C16 1.0(9) . . . . ?
N14 N13 C17 C16 -0.9(9) . . . . ?
N14 C15 C16 C17 -1.6(11) . . . . ?
C15 C16 C17 N13 1.5(10) . . . . ?
C17 N13 N14 Fe1 -174.2(5) . . . . ?
C17 N13 N14 Ru1 -174.2(5) . . . . ?
C17 N13 N14 C15 -0.1(8) . . . . ?
N18 C19 C20 C21 -0.1(10) . . . . ?
N18 C19 N24 N25 1.0(7) . . . . ?
N18 C19 N24 C28 -175.2(7) . . . . ?
N18 C23 N29 N30 2.3(8) . . . . ?
N18 C23 N29 C33 -179.5(6) . . . . ?
C19 N18 C23 C22 0.3(9) . . . . ?
C19 N18 C23 N29 -179.8(5) . . . . ?
C19 C20 C21 C22 0.9(12) . . . . ?
C19 N24 N25 Fe1 -0.5(6) . . . . ?
C19 N24 N25 Ru1 -0.5(6) . . . . ?
C19 N24 N25 C26 -177.1(6) . . . . ?
C19 N24 C28 C27 175.4(7) . . . . ?
C20 C19 N24 N25 -179.9(6) . . . . ?
C20 C19 N24 C28 4.0(11) . . . . ?
C20 C21 C22 C23 -1.0(12) . . . . ?
C21 C22 C23 N18 0.4(10) . . . . ?
C21 C22 C23 N29 -179.5(7) . . . . ?
C22 C23 N29 N30 -177.7(6) . . . . ?
C22 C23 N29 C33 0.4(11) . . . . ?
C23 N18 C19 C20 -0.5(9) . . . . ?
C23 N18 C19 N24 178.7(5) . . . . ?
C23 N29 N30 Fe1 -3.5(6) . . . . ?
C23 N29 N30 Ru1 -3.5(6) . . . . ?
C23 N29 N30 C31 177.2(6) . . . . ?
C23 N29 C33 C32 -177.3(6) . . . . ?
N24 C19 C20 C21 -179.1(6) . . . . ?
N24 N25 C26 C27 1.3(8) . . . . ?
N25 N24 C28 C27 -1.0(9) . . . . ?
N25 C26 C27 C28 -2.0(10) . . . . ?
C26 C27 C28 N24 1.7(9) . . . . ?
C28 N24 N25 Fe1 176.4(5) . . . . ?
C28 N24 N25 Ru1 176.4(5) . . . . ?
C28 N24 N25 C26 -0.2(7) . . . . ?
N29 N30 C31 C32 1.1(8) . . . . ?
N30 N29 C33 C32 1.0(8) . . . . ?
N30 C31 C32 C33 -0.5(9) . . . . ?
C31 C32 C33 N29 -0.3(9) . . . . ?
C33 N29 N30 Fe1 178.0(5) . . . . ?
C33 N29 N30 Ru1 178.0(5) . . . . ?
C33 N29 N30 C31 -1.3(7) . . . . ?

_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_mh202lto
_database_code_depnum_ccdc_archive 'CCDC 2261795'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2023-08-22 deposited with the CCDC.	2023-08-30 downloaded from the CCDC.
;
_audit_creation_date             2023-03-13
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis[2,6-di(pyrazol-1-yl)pyridine]iron(II) bis[2,6-di(pyrazol-1-yl)pyridine]-nickel(II) ditetrafluoroborate 0.46:0.54 solid solution (ordered refinement)'
_chemical_formula_moiety         'C22 H18 Fe0.46 N10 Ni0.54, 2(B F4)'
_chemical_formula_sum            'C22 H18 B2 F8 Fe0.46 N10 Ni0.54'
_chemical_formula_weight         653.48
_chemical_absolute_configuration ab
_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 0.0019 0.0015 '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 0.0004 0.0006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0124 0.0097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.2961 0.8007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0037 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.2866 1.0558 '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           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   8.4441(1)
_cell_length_b                   8.5062(1)
_cell_length_c                   18.4578(1)
_cell_angle_alpha                90
_cell_angle_beta                 97.907(1)
_cell_angle_gamma                90
_cell_volume                     1313.17(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    18528
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      35.82
_cell_measurement_theta_min      1.07
_exptl_absorpt_coefficient_mu    0.697
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.924
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
DIALS 3.12.1-2-g1c07bc2b3-release
Scaling & analysis of unmerged intensities, absorption correction using 
spherical harmonics
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       lath
_exptl_crystal_F_000             658
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            30085
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.886
_diffrn_reflns_theta_full        24.620
_diffrn_reflns_theta_max         36.139
_diffrn_reflns_theta_min         1.080
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.929
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_measurement_device       'Fixed χ 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_reflns_Friedel_coverage         0.813
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.837
_reflns_number_gt                11565
_reflns_number_total             12239
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_computing_cell_refinement       'XIA2 0.4.0.438-g4431aaa (Winter, 2010)'
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction        'XIA2 0.4.0.438-g4431aaa (Winter, 2010)'
_computing_molecular_graphics    'XSEED (Barbour, 2020)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.056(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         12239
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0398
_refine_ls_restrained_S_all      1.021
_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)+(0.0263P)²+0.7053P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0914
_refine_special_details          
;In this refinement, the low temperature dataset was treated as a single, 
 averaged [FeₓNi₁₋ₓ(bpp)₂]2+ cation site. Partial Fe and Ni atoms
 were refined with the same cartesian coordinates, using the Fe~0.46~/
 Ni~0.54~ occupancy ratio obtained from the disordered refinement model 
 from this dataset. No anion disorder is included in the model. However, 
 an EADP thermal parameter constraint between the two partial metal atoms 
 was required to make the model converge.

 All non-H atoms were refined anisotropically, and H atoms were placed in 
 calculated positions and refined using a riding model. A minor inversion 
 twin domain was included in the refinement, to account for the slightly 
 high Flack parameter.,Twin
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.944(10)
 0.056(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(Fe1) = Uanis(Ni1)
4. Others
 X(Fe1)=X(Ni1)=FVAR(1)
 Y(Fe1)=Y(Ni1)=FVAR(2)
 Z(Fe1)=Z(Ni1)=FVAR(3)
 Fixed Sof: Fe1(0.46) Ni1(0.54)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16),
 C17(H17), C20(H20), C21(H21), C22(H22), C26(H26), C27(H27), C28(H28), C31(H31),
  C32(H32), C33(H33)
;
_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 0.71881(3) 0.82246(3) 0.74643(2) 0.01321(5) Uani 0.46 1 d . . P A 1
Ni1 Ni 0.71881(3) 0.82246(3) 0.74643(2) 0.01321(5) Uani 0.54 1 d . . P A 2
N2 N 0.7131(2) 0.8388(2) 0.64047(9) 0.0155(3) Uani 1 1 d . . . . .
C3 C 0.5845(2) 0.8973(2) 0.59899(11) 0.0159(3) Uani 1 1 d . . . . .
C4 C 0.5744(3) 0.9105(3) 0.52369(11) 0.0192(3) Uani 1 1 d . . . . .
H4 H 0.484136 0.951560 0.495500 0.023 Uiso 1 1 calc R U . . .
C5 C 0.7058(3) 0.8593(3) 0.49234(12) 0.0216(4) Uani 1 1 d . . . . .
H5 H 0.703590 0.867033 0.441952 0.026 Uiso 1 1 calc R U . . .
C6 C 0.8405(3) 0.7968(2) 0.53433(12) 0.0203(4) Uani 1 1 d . . . . .
H6 H 0.928492 0.762737 0.513330 0.024 Uiso 1 1 calc R U . . .
C7 C 0.8370(3) 0.7879(2) 0.60884(11) 0.0168(3) Uani 1 1 d . . . . .
N8 N 0.4657(2) 0.9408(2) 0.64126(10) 0.0168(3) Uani 1 1 d . . . . .
N9 N 0.4962(2) 0.9164(2) 0.71546(10) 0.0174(3) Uani 1 1 d . . . . .
C10 C 0.3650(3) 0.9644(3) 0.74142(14) 0.0215(4) Uani 1 1 d . . . . .
H10 H 0.350789 0.961114 0.790470 0.026 Uiso 1 1 calc R U . . .
C11 C 0.2506(3) 1.0208(3) 0.68473(15) 0.0253(4) Uani 1 1 d . . . . .
H11 H 0.150124 1.061425 0.689114 0.030 Uiso 1 1 calc R U . . .
C12 C 0.3177(3) 1.0036(3) 0.62186(14) 0.0221(4) Uani 1 1 d . . . . .
H12 H 0.271116 1.029871 0.574813 0.026 Uiso 1 1 calc R U . . .
N13 N 0.9575(2) 0.7251(2) 0.66039(10) 0.0178(3) Uani 1 1 d . . . . .
N14 N 0.9354(2) 0.7331(2) 0.73269(11) 0.0197(3) Uani 1 1 d . . . . .
C15 C 1.0613(3) 0.6620(3) 0.76943(15) 0.0260(5) Uani 1 1 d . . . . .
H15 H 1.078892 0.650539 0.820008 0.031 Uiso 1 1 calc R U . . .
C16 C 1.1643(3) 0.6065(3) 0.72171(18) 0.0307(5) Uani 1 1 d . . . . .
H16 H 1.259747 0.552246 0.734262 0.037 Uiso 1 1 calc R U . . .
C17 C 1.0957(3) 0.6482(3) 0.65301(16) 0.0267(5) Uani 1 1 d . . . . .
H17 H 1.135928 0.627984 0.609496 0.032 Uiso 1 1 calc R U . . .
N18 N 0.7220(2) 0.79568(19) 0.85199(9) 0.0158(3) Uani 1 1 d . . . . .
C19 C 0.7795(2) 0.9091(2) 0.89823(11) 0.0162(3) Uani 1 1 d . . . . .
C20 C 0.7851(3) 0.8955(3) 0.97318(11) 0.0191(4) Uani 1 1 d . . . . .
H20 H 0.824898 0.975779 1.004726 0.023 Uiso 1 1 calc R U . . .
C21 C 0.7283(3) 0.7556(3) 0.99908(12) 0.0208(4) Uani 1 1 d . . . . .
H21 H 0.729116 0.742606 1.049156 0.025 Uiso 1 1 calc R U . . .
C22 C 0.6704(3) 0.6347(3) 0.95202(12) 0.0203(4) Uani 1 1 d . . . . .
H22 H 0.634235 0.540522 0.969360 0.024 Uiso 1 1 calc R U . . .
C23 C 0.6694(2) 0.6620(2) 0.87808(11) 0.0164(3) Uani 1 1 d . . . . .
N24 N 0.8334(2) 1.0385(2) 0.86115(10) 0.0176(3) Uani 1 1 d . . . . .
N25 N 0.8175(2) 1.0309(2) 0.78604(10) 0.0183(3) Uani 1 1 d . . . . .
C26 C 0.8860(3) 1.1618(3) 0.76563(14) 0.0239(4) Uani 1 1 d . . . . .
H26 H 0.892986 1.189256 0.717409 0.029 Uiso 1 1 calc R U . . .
C27 C 0.9463(3) 1.2529(3) 0.82709(16) 0.0284(5) Uani 1 1 d . . . . .
H27 H 0.999219 1.348783 0.827120 0.034 Uiso 1 1 calc R U . . .
C28 C 0.9109(3) 1.1710(3) 0.88679(15) 0.0243(4) Uani 1 1 d . . . . .
H28 H 0.935291 1.200745 0.935541 0.029 Uiso 1 1 calc R U . . .
N29 N 0.6156(2) 0.5556(2) 0.82182(10) 0.0181(3) Uani 1 1 d . . . . .
N30 N 0.6296(2) 0.6013(2) 0.75162(10) 0.0180(3) Uani 1 1 d . . . . .
C31 C 0.5813(3) 0.4781(3) 0.70985(14) 0.0232(4) Uani 1 1 d . . . . .
H31 H 0.578776 0.474823 0.659339 0.028 Uiso 1 1 calc R U . . .
C32 C 0.5348(3) 0.3538(3) 0.75236(17) 0.0280(5) Uani 1 1 d . . . . .
H32 H 0.495896 0.256020 0.735840 0.034 Uiso 1 1 calc R U . . .
C33 C 0.5586(3) 0.4066(3) 0.82341(15) 0.0244(4) Uani 1 1 d . . . . .
H33 H 0.539303 0.350886 0.864672 0.029 Uiso 1 1 calc R U . . .
B34 B 0.7960(3) 0.2814(3) 0.56449(15) 0.0226(5) Uani 1 1 d . . . . .
F35 F 0.6773(2) 0.22811(18) 0.60368(9) 0.0269(3) Uani 1 1 d . . . . .
F36 F 0.7664(2) 0.2291(2) 0.49224(9) 0.0311(3) Uani 1 1 d . . . . .
F37 F 0.7956(2) 0.44563(19) 0.56444(10) 0.0323(4) Uani 1 1 d . . . . .
F38 F 0.9443(2) 0.2260(3) 0.59662(10) 0.0444(5) Uani 1 1 d . . . . .
B39 B 0.7186(4) 0.2628(3) 1.05830(15) 0.0246(5) Uani 1 1 d . . . . .
F40 F 0.6432(2) 0.2521(2) 0.98614(8) 0.0276(3) Uani 1 1 d . . . . .
F41 F 0.68111(19) 0.1318(2) 1.09805(9) 0.0315(4) Uani 1 1 d . . . . .
F42 F 0.8837(2) 0.2642(3) 1.05779(10) 0.0430(5) Uani 1 1 d . . . . .
F43 F 0.6671(4) 0.3977(3) 1.08959(11) 0.0540(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 1.9547(17) . ?
Fe1 N9 2.0504(19) . ?
Fe1 N14 2.029(2) . ?
Fe1 N18 1.9582(17) . ?
Fe1 N25 2.051(2) . ?
Fe1 N30 2.0332(19) . ?
Ni1 N2 1.9547(17) . ?
Ni1 N9 2.0504(19) . ?
Ni1 N14 2.029(2) . ?
Ni1 N18 1.9582(17) . ?
Ni1 N25 2.051(2) . ?
Ni1 N30 2.0332(19) . ?
N2 C3 1.336(3) . ?
N2 C7 1.338(3) . ?
C3 C4 1.385(3) . ?
C3 N8 1.403(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.390(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.391(3) . ?
C6 H6 0.9300 . ?
C6 C7 1.382(3) . ?
C7 N13 1.400(3) . ?
N8 N9 1.374(3) . ?
N8 C12 1.361(3) . ?
N9 C10 1.330(3) . ?
C10 H10 0.9300 . ?
C10 C11 1.407(4) . ?
C11 H11 0.9300 . ?
C11 C12 1.367(4) . ?
C12 H12 0.9300 . ?
N13 N14 1.374(3) . ?
N13 C17 1.361(3) . ?
N14 C15 1.325(3) . ?
C15 H15 0.9300 . ?
C15 C16 1.402(4) . ?
C16 H16 0.9300 . ?
C16 C17 1.366(4) . ?
C17 H17 0.9300 . ?
N18 C19 1.334(3) . ?
N18 C23 1.335(3) . ?
C19 C20 1.382(3) . ?
C19 N24 1.405(3) . ?
C20 H20 0.9300 . ?
C20 C21 1.392(3) . ?
C21 H21 0.9300 . ?
C21 C22 1.390(3) . ?
C22 H22 0.9300 . ?
C22 C23 1.383(3) . ?
C23 N29 1.405(3) . ?
N24 N25 1.376(3) . ?
N24 C28 1.356(3) . ?
N25 C26 1.332(3) . ?
C26 H26 0.9300 . ?
C26 C27 1.410(4) . ?
C27 H27 0.9300 . ?
C27 C28 1.371(4) . ?
C28 H28 0.9300 . ?
N29 N30 1.373(3) . ?
N29 C33 1.358(3) . ?
N30 C31 1.331(3) . ?
C31 H31 0.9300 . ?
C31 C32 1.405(4) . ?
C32 H32 0.9300 . ?
C32 C33 1.375(4) . ?
C33 H33 0.9300 . ?
B34 F35 1.390(3) . ?
B34 F36 1.395(3) . ?
B34 F37 1.397(3) . ?
B34 F38 1.392(3) . ?
B39 F40 1.398(3) . ?
B39 F41 1.394(3) . ?
B39 F42 1.396(3) . ?
B39 F43 1.381(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 78.35(7) . . ?
N2 Fe1 N14 78.46(7) . . ?
N2 Fe1 N18 177.32(8) . . ?
N2 Fe1 N25 104.37(8) . . ?
N2 Fe1 N30 98.89(8) . . ?
N9 Fe1 N25 94.27(7) . . ?
N14 Fe1 N9 156.79(7) . . ?
N14 Fe1 N25 92.25(8) . . ?
N14 Fe1 N30 90.31(8) . . ?
N18 Fe1 N9 102.08(7) . . ?
N18 Fe1 N14 101.05(8) . . ?
N18 Fe1 N25 78.26(7) . . ?
N18 Fe1 N30 78.46(7) . . ?
N30 Fe1 N9 92.43(8) . . ?
N30 Fe1 N25 156.64(7) . . ?
N2 Ni1 N9 78.35(7) . . ?
N2 Ni1 N14 78.46(7) . . ?
N2 Ni1 N18 177.32(8) . . ?
N2 Ni1 N25 104.37(8) . . ?
N2 Ni1 N30 98.89(8) . . ?
N9 Ni1 N25 94.27(7) . . ?
N14 Ni1 N9 156.79(7) . . ?
N14 Ni1 N25 92.25(8) . . ?
N14 Ni1 N30 90.31(8) . . ?
N18 Ni1 N9 102.08(7) . . ?
N18 Ni1 N14 101.05(8) . . ?
N18 Ni1 N25 78.26(7) . . ?
N18 Ni1 N30 78.46(7) . . ?
N30 Ni1 N9 92.43(8) . . ?
N30 Ni1 N25 156.64(7) . . ?
C3 N2 Fe1 120.40(14) . . ?
C3 N2 Ni1 120.40(14) . . ?
C3 N2 C7 119.55(18) . . ?
C7 N2 Fe1 120.04(14) . . ?
C7 N2 Ni1 120.04(14) . . ?
N2 C3 C4 122.57(19) . . ?
N2 C3 N8 111.52(17) . . ?
C4 C3 N8 125.91(19) . . ?
C3 C4 H4 121.6 . . ?
C3 C4 C5 116.7(2) . . ?
C5 C4 H4 121.6 . . ?
C4 C5 H5 119.1 . . ?
C4 C5 C6 121.8(2) . . ?
C6 C5 H5 119.1 . . ?
C5 C6 H6 121.7 . . ?
C7 C6 C5 116.6(2) . . ?
C7 C6 H6 121.7 . . ?
N2 C7 C6 122.8(2) . . ?
N2 C7 N13 111.44(18) . . ?
C6 C7 N13 125.75(19) . . ?
N9 N8 C3 117.66(17) . . ?
C12 N8 C3 131.2(2) . . ?
C12 N8 N9 111.16(19) . . ?
N8 N9 Fe1 112.07(13) . . ?
N8 N9 Ni1 112.07(13) . . ?
C10 N9 Fe1 142.77(17) . . ?
C10 N9 Ni1 142.77(17) . . ?
C10 N9 N8 105.16(19) . . ?
N9 C10 H10 124.5 . . ?
N9 C10 C11 110.9(2) . . ?
C11 C10 H10 124.5 . . ?
C10 C11 H11 127.1 . . ?
C12 C11 C10 105.8(2) . . ?
C12 C11 H11 127.1 . . ?
N8 C12 C11 106.9(2) . . ?
N8 C12 H12 126.5 . . ?
C11 C12 H12 126.5 . . ?
N14 N13 C7 117.27(17) . . ?
C17 N13 C7 131.9(2) . . ?
C17 N13 N14 110.7(2) . . ?
N13 N14 Fe1 112.64(14) . . ?
N13 N14 Ni1 112.64(14) . . ?
C15 N14 Fe1 141.29(19) . . ?
C15 N14 Ni1 141.29(19) . . ?
C15 N14 N13 105.5(2) . . ?
N14 C15 H15 124.6 . . ?
N14 C15 C16 110.8(2) . . ?
C16 C15 H15 124.6 . . ?
C15 C16 H16 127.0 . . ?
C17 C16 C15 106.0(2) . . ?
C17 C16 H16 127.0 . . ?
N13 C17 C16 107.0(2) . . ?
N13 C17 H17 126.5 . . ?
C16 C17 H17 126.5 . . ?
C19 N18 Fe1 120.43(14) . . ?
C19 N18 Ni1 120.43(14) . . ?
C19 N18 C23 119.66(18) . . ?
C23 N18 Fe1 119.90(14) . . ?
C23 N18 Ni1 119.90(14) . . ?
N18 C19 C20 122.6(2) . . ?
N18 C19 N24 111.62(18) . . ?
C20 C19 N24 125.7(2) . . ?
C19 C20 H20 121.7 . . ?
C19 C20 C21 116.7(2) . . ?
C21 C20 H20 121.7 . . ?
C20 C21 H21 119.1 . . ?
C22 C21 C20 121.7(2) . . ?
C22 C21 H21 119.1 . . ?
C21 C22 H22 121.7 . . ?
C23 C22 C21 116.5(2) . . ?
C23 C22 H22 121.7 . . ?
N18 C23 C22 122.8(2) . . ?
N18 C23 N29 111.82(17) . . ?
C22 C23 N29 125.39(19) . . ?
N25 N24 C19 117.45(18) . . ?
C28 N24 C19 130.9(2) . . ?
C28 N24 N25 111.49(19) . . ?
N24 N25 Fe1 112.23(13) . . ?
N24 N25 Ni1 112.23(13) . . ?
C26 N25 Fe1 142.41(17) . . ?
C26 N25 Ni1 142.41(17) . . ?
C26 N25 N24 105.1(2) . . ?
N25 C26 H26 124.6 . . ?
N25 C26 C27 110.8(2) . . ?
C27 C26 H26 124.6 . . ?
C26 C27 H27 127.1 . . ?
C28 C27 C26 105.8(2) . . ?
C28 C27 H27 127.1 . . ?
N24 C28 C27 106.8(2) . . ?
N24 C28 H28 126.6 . . ?
C27 C28 H28 126.6 . . ?
N30 N29 C23 117.01(17) . . ?
C33 N29 C23 131.7(2) . . ?
C33 N29 N30 111.20(19) . . ?
N29 N30 Fe1 112.76(14) . . ?
N29 N30 Ni1 112.76(14) . . ?
C31 N30 Fe1 141.89(17) . . ?
C31 N30 Ni1 141.89(17) . . ?
C31 N30 N29 105.32(19) . . ?
N30 C31 H31 124.6 . . ?
N30 C31 C32 110.9(2) . . ?
C32 C31 H31 124.6 . . ?
C31 C32 H32 127.1 . . ?
C33 C32 C31 105.8(2) . . ?
C33 C32 H32 127.1 . . ?
N29 C33 C32 106.9(2) . . ?
N29 C33 H33 126.6 . . ?
C32 C33 H33 126.6 . . ?
F35 B34 F36 110.3(2) . . ?
F35 B34 F37 108.9(2) . . ?
F35 B34 F38 109.8(2) . . ?
F36 B34 F37 108.5(2) . . ?
F38 B34 F36 109.4(2) . . ?
F38 B34 F37 109.9(2) . . ?
F41 B39 F40 110.1(2) . . ?
F41 B39 F42 108.1(2) . . ?
F42 B39 F40 108.6(2) . . ?
F43 B39 F40 108.9(2) . . ?
F43 B39 F41 109.7(2) . . ?
F43 B39 F42 111.6(3) . . ?

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 -179.66(16) . . . . ?
Fe1 N2 C3 N8 0.1(2) . . . . ?
Fe1 N2 C7 C6 -179.73(16) . . . . ?
Fe1 N2 C7 N13 0.9(2) . . . . ?
Fe1 N9 C10 C11 179.55(19) . . . . ?
Fe1 N14 C15 C16 169.8(2) . . . . ?
Fe1 N18 C19 C20 -179.63(16) . . . . ?
Fe1 N18 C19 N24 -0.4(2) . . . . ?
Fe1 N18 C23 C22 179.11(16) . . . . ?
Fe1 N18 C23 N29 -0.5(2) . . . . ?
Fe1 N25 C26 C27 -172.4(2) . . . . ?
Fe1 N30 C31 C32 178.37(19) . . . . ?
Ni1 N2 C3 C4 -179.66(16) . . . . ?
Ni1 N2 C3 N8 0.1(2) . . . . ?
Ni1 N2 C7 C6 -179.73(16) . . . . ?
Ni1 N2 C7 N13 0.9(2) . . . . ?
Ni1 N9 C10 C11 179.55(19) . . . . ?
Ni1 N14 C15 C16 169.8(2) . . . . ?
Ni1 N18 C19 C20 -179.63(16) . . . . ?
Ni1 N18 C19 N24 -0.4(2) . . . . ?
Ni1 N18 C23 C22 179.11(16) . . . . ?
Ni1 N18 C23 N29 -0.5(2) . . . . ?
Ni1 N25 C26 C27 -172.4(2) . . . . ?
Ni1 N30 C31 C32 178.37(19) . . . . ?
N2 C3 C4 C5 0.1(3) . . . . ?
N2 C3 N8 N9 -0.8(3) . . . . ?
N2 C3 N8 C12 -179.7(2) . . . . ?
N2 C7 N13 N14 -3.5(3) . . . . ?
N2 C7 N13 C17 173.2(2) . . . . ?
C3 N2 C7 C6 1.8(3) . . . . ?
C3 N2 C7 N13 -177.56(18) . . . . ?
C3 C4 C5 C6 0.4(3) . . . . ?
C3 N8 N9 Fe1 1.1(2) . . . . ?
C3 N8 N9 Ni1 1.1(2) . . . . ?
C3 N8 N9 C10 -178.86(18) . . . . ?
C3 N8 C12 C11 179.1(2) . . . . ?
C4 C3 N8 N9 178.9(2) . . . . ?
C4 C3 N8 C12 0.0(4) . . . . ?
C4 C5 C6 C7 0.1(3) . . . . ?
C5 C6 C7 N2 -1.3(3) . . . . ?
C5 C6 C7 N13 178.0(2) . . . . ?
C6 C7 N13 N14 177.1(2) . . . . ?
C6 C7 N13 C17 -6.1(4) . . . . ?
C7 N2 C3 C4 -1.2(3) . . . . ?
C7 N2 C3 N8 178.52(18) . . . . ?
C7 N13 N14 Fe1 4.4(2) . . . . ?
C7 N13 N14 Ni1 4.4(2) . . . . ?
C7 N13 N14 C15 177.92(19) . . . . ?
C7 N13 C17 C16 -177.1(2) . . . . ?
N8 C3 C4 C5 -179.6(2) . . . . ?
N8 N9 C10 C11 -0.5(2) . . . . ?
N9 N8 C12 C11 0.1(3) . . . . ?
N9 C10 C11 C12 0.6(3) . . . . ?
C10 C11 C12 N8 -0.4(3) . . . . ?
C12 N8 N9 Fe1 -179.79(14) . . . . ?
C12 N8 N9 Ni1 -179.79(14) . . . . ?
C12 N8 N9 C10 0.3(2) . . . . ?
N13 N14 C15 C16 -0.6(3) . . . . ?
N14 N13 C17 C16 -0.2(3) . . . . ?
N14 C15 C16 C17 0.5(3) . . . . ?
C15 C16 C17 N13 -0.1(3) . . . . ?
C17 N13 N14 Fe1 -173.00(15) . . . . ?
C17 N13 N14 Ni1 -173.00(15) . . . . ?
C17 N13 N14 C15 0.5(2) . . . . ?
N18 C19 C20 C21 0.4(3) . . . . ?
N18 C19 N24 N25 1.0(3) . . . . ?
N18 C19 N24 C28 -174.0(2) . . . . ?
N18 C23 N29 N30 2.0(3) . . . . ?
N18 C23 N29 C33 177.4(2) . . . . ?
C19 N18 C23 C22 0.5(3) . . . . ?
C19 N18 C23 N29 -179.13(18) . . . . ?
C19 C20 C21 C22 0.7(3) . . . . ?
C19 N24 N25 Fe1 -1.1(2) . . . . ?
C19 N24 N25 Ni1 -1.1(2) . . . . ?
C19 N24 N25 C26 -176.23(19) . . . . ?
C19 N24 C28 C27 175.4(2) . . . . ?
C20 C19 N24 N25 -179.8(2) . . . . ?
C20 C19 N24 C28 5.2(4) . . . . ?
C20 C21 C22 C23 -1.2(3) . . . . ?
C21 C22 C23 N18 0.6(3) . . . . ?
C21 C22 C23 N29 -179.9(2) . . . . ?
C22 C23 N29 N30 -177.6(2) . . . . ?
C22 C23 N29 C33 -2.2(4) . . . . ?
C23 N18 C19 C20 -1.0(3) . . . . ?
C23 N18 C19 N24 178.19(18) . . . . ?
C23 N29 N30 Fe1 -2.5(2) . . . . ?
C23 N29 N30 Ni1 -2.5(2) . . . . ?
C23 N29 N30 C31 175.97(19) . . . . ?
C23 N29 C33 C32 -175.6(2) . . . . ?
N24 C19 C20 C21 -178.7(2) . . . . ?
N24 N25 C26 C27 0.3(3) . . . . ?
N25 N24 C28 C27 0.2(3) . . . . ?
N25 C26 C27 C28 -0.2(3) . . . . ?
C26 C27 C28 N24 0.0(3) . . . . ?
C28 N24 N25 Fe1 174.88(16) . . . . ?
C28 N24 N25 Ni1 174.88(16) . . . . ?
C28 N24 N25 C26 -0.3(2) . . . . ?
N29 N30 C31 C32 0.6(3) . . . . ?
N30 N29 C33 C32 0.0(3) . . . . ?
N30 C31 C32 C33 -0.6(3) . . . . ?
C31 C32 C33 N29 0.3(3) . . . . ?
C33 N29 N30 Fe1 -178.88(15) . . . . ?
C33 N29 N30 Ni1 -178.88(15) . . . . ?
C33 N29 N30 C31 -0.4(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.944(10)
2 0.056(10)

_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_mh453lto
_database_code_depnum_ccdc_archive 'CCDC 2261787'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2023-08-21 deposited with the CCDC.	2023-08-30 downloaded from the CCDC.
;
_audit_creation_date             2023-03-06
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis[2,6-di(pyrazol-1-yl)pyridine]iron(II) bis[2,6-di(pyrazol-1-yl)pyridine]-zinc(II) ditetrafluoroborate 0.54:0.46 solid solution (ordered refinement)'
_chemical_formula_moiety         
'0.54(C22 H18 Fe N10), 0.46(C22 H18 N10 Zn), 2(B F4)'
_chemical_formula_sum            'C22 H18 B2 F8 Fe0.54 N10 Zn0.46'
_chemical_formula_weight         656.31
_chemical_absolute_configuration ab
_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 0.0019 0.0015 '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 0.0004 0.0006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0124 0.0097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.2961 0.8007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0037 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2335 1.3591 '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           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   8.4486(1)
_cell_length_b                   8.4867(1)
_cell_length_c                   18.5535(1)
_cell_angle_alpha                90
_cell_angle_beta                 97.618(1)
_cell_angle_gamma                90
_cell_volume                     1318.56(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    13086
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      35.15
_cell_measurement_theta_min      2.14
_exptl_absorpt_coefficient_mu    0.766
_exptl_absorpt_correction_T_min  0.897
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
DIALS 3.12.1-2-g1c07bc2b3-release
Scaling & analysis of unmerged intensities, absorption correction using 
spherical harmonics
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       lath
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0724
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            29979
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        24.620
_diffrn_reflns_theta_max         36.109
_diffrn_reflns_theta_min         1.073
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.930
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_measurement_device       'Fixed χ 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.979
_reflns_Friedel_fraction_max     0.844
_reflns_number_gt                9617
_reflns_number_total             12312
_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       'XIA2 0.4.0.438-g4431aaa (Winter, 2010)'
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction        'XIA2 0.4.0.438-g4431aaa (Winter, 2010)'
_computing_molecular_graphics    'XSEED (Barbour, 2020)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 
;
 Flack x determined using 3008 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         12313
_refine_ls_number_restraints     68
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0380
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0308P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0763
_refine_special_details          
;
 In this refinement, the low temperature dataset was treated as a single, 
 averaged [FeₓZn₁₋ₓ(bpp)₂]2+ cation site. Partial Fe and Zn atoms
 were refined with the same cartesian coordinates, using the Fe~0.54~/
 Zn~0.46~ occupancy ratio obtained from the disordered refinement model 
 from this dataset. 

 The F atoms of one BF₄⁻ ion were also disordered over two orientations, 
 with refined occupancies of 0.67:0.33. The refined distance restraints 
 listed below were applied to that moiety. An EADP thermal parameter 
 constraint between the two partial metal atoms was also required to make 
 the model converge. All non-H atoms were refined anisotropically in the
 final least squares cycles, with ISOR restraints applied to the partial 
 F atoms.  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
2. Restrained distances
 B39-F40A
 1.39818 with sigma of 0.02
 B39-F41A
 1.39818 with sigma of 0.02
 B39-F42A
 1.39818 with sigma of 0.02
 B39-F43A
 1.39818 with sigma of 0.02
 B39-F40B
 1.39818 with sigma of 0.02
 B39-F41B
 1.39818 with sigma of 0.02
 B39-F42B
 1.39818 with sigma of 0.02
 B39-F43B
 1.39818 with sigma of 0.02
 F40A-F41A
 2.283228 with sigma of 0.02
 F40A-F42A
 2.283228 with sigma of 0.02
 F40A-F43A
 2.283228 with sigma of 0.02
 F41A-F42A
 2.283228 with sigma of 0.02
 F41A-F43A
 2.283228 with sigma of 0.02
 F42A-F43A
 2.283228 with sigma of 0.02
 F40B-F41B
 2.283228 with sigma of 0.02
 F40B-F42B
 2.283228 with sigma of 0.02
 F40B-F43B
 2.283228 with sigma of 0.02
 F41B-F42B
 2.283228 with sigma of 0.02
 F41B-F43B
 2.283228 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F40A) \\sim Ueq, Uanis(F41A) \\sim Ueq, Uanis(F42A) \\sim Ueq,
Uanis(F43A) \\sim Ueq, Uanis(F40B) \\sim Ueq, Uanis(F41B) \\sim Ueq,
Uanis(F42B) \\sim Ueq, Uanis(F43B) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(Fe1) = Uanis(Zn1)
4. Others
 1(DFIX)=1(DFIX)=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(DFIX)=1(DFIX)=1(DFIX)=
 1(DFIX)=1(DFIX)=1.633*FVAR(2)
 X(Fe1)=X(Zn1)=FVAR(2)
 Y(Fe1)=Y(Zn1)=FVAR(3)
 Z(Fe1)=Z(Zn1)=FVAR(4)
 Fixed Sof: Fe1(0.54) Zn1(0.46) F40A(0.67) F41A(0.67) F42A(0.67) F43A(0.67)
 F40B(0.33) F41B(0.33) F42B(0.33) F43B(0.33)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16),
 C17(H17), C20(H20), C21(H21), C22(H22), C26(H26), C27(H27), C28(H28), C31(H31),
  C32(H32), C33(H33)
;
_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 0.27465(3) 0.17898(3) 0.25349(2) 0.01786(5) Uani 0.54 1 d . . P A 1
Zn1 Zn 0.27465(3) 0.17898(3) 0.25349(2) 0.01786(5) Uani 0.46 1 d . . P A 2
N2 N 0.28463(17) 0.1685(2) 0.36133(8) 0.0212(3) Uani 1 1 d . . . . .
C3 C 0.4133(2) 0.1109(2) 0.40238(10) 0.0213(3) Uani 1 1 d . . . . .
C4 C 0.4253(3) 0.0994(2) 0.47719(11) 0.0259(4) Uani 1 1 d . . . . .
H4 H 0.516316 0.059441 0.504831 0.031 Uiso 1 1 calc R U . . .
C5 C 0.2944(3) 0.1506(2) 0.50916(11) 0.0295(4) Uani 1 1 d . . . . .
H5 H 0.297084 0.143456 0.559328 0.035 Uiso 1 1 calc R U . . .
C6 C 0.1595(3) 0.2122(2) 0.46746(12) 0.0288(4) Uani 1 1 d . . . . .
H6 H 0.072075 0.247213 0.488647 0.035 Uiso 1 1 calc R U . . .
C7 C 0.1612(2) 0.2189(2) 0.39352(11) 0.0240(4) Uani 1 1 d . . . . .
N8 N 0.53236(19) 0.06658(19) 0.36022(9) 0.0222(3) Uani 1 1 d . . . . .
N9 N 0.5014(2) 0.08714(19) 0.28637(9) 0.0230(3) Uani 1 1 d . . . . .
C10 C 0.6325(3) 0.0394(3) 0.26035(13) 0.0302(4) Uani 1 1 d . . . . .
H10 H 0.646312 0.040971 0.211453 0.036 Uiso 1 1 calc R U . . .
C11 C 0.7478(3) -0.0140(3) 0.31710(14) 0.0340(5) Uani 1 1 d . . . . .
H11 H 0.848492 -0.054216 0.312797 0.041 Uiso 1 1 calc R U . . .
C12 C 0.6810(2) 0.0055(2) 0.37968(13) 0.0294(4) Uani 1 1 d . . . . .
H12 H 0.728013 -0.018321 0.426594 0.035 Uiso 1 1 calc R U . . .
N13 N 0.0391(2) 0.2808(2) 0.34256(11) 0.0284(4) Uani 1 1 d . . . . .
N14 N 0.0580(2) 0.2696(2) 0.27044(11) 0.0323(4) Uani 1 1 d . . . . .
C15 C -0.0690(3) 0.3408(3) 0.23477(17) 0.0467(7) Uani 1 1 d . . . . .
H15 H -0.089491 0.350158 0.184457 0.056 Uiso 1 1 calc R U . . .
C16 C -0.1677(3) 0.3997(3) 0.2833(2) 0.0579(9) Uani 1 1 d . . . . .
H16 H -0.262685 0.454938 0.271686 0.069 Uiso 1 1 calc R U . . .
C17 C -0.0968(3) 0.3598(3) 0.35093(18) 0.0455(7) Uani 1 1 d . . . . .
H17 H -0.134374 0.382490 0.394679 0.055 Uiso 1 1 calc R U . . .
N18 N 0.27434(19) 0.20543(19) 0.14640(8) 0.0213(3) Uani 1 1 d . . . . .
C19 C 0.2185(2) 0.0914(2) 0.10065(10) 0.0220(3) Uani 1 1 d . . . . .
C20 C 0.2148(2) 0.1028(3) 0.02638(11) 0.0260(4) Uani 1 1 d . . . . .
H20 H 0.176083 0.021363 -0.004601 0.031 Uiso 1 1 calc R U . . .
C21 C 0.2719(3) 0.2425(3) 0.00007(11) 0.0279(4) Uani 1 1 d . . . . .
H21 H 0.272026 0.254578 -0.049746 0.034 Uiso 1 1 calc R U . . .
C22 C 0.3286(2) 0.3642(3) 0.04646(11) 0.0270(4) Uani 1 1 d . . . . .
H22 H 0.365385 0.458093 0.028883 0.032 Uiso 1 1 calc R U . . .
C23 C 0.3277(2) 0.3391(2) 0.12001(11) 0.0229(3) Uani 1 1 d . . . . .
N24 N 0.1631(2) -0.0385(2) 0.13740(9) 0.0249(3) Uani 1 1 d . . . . .
N25 N 0.1767(2) -0.0305(2) 0.21233(10) 0.0288(4) Uani 1 1 d . . . . .
C26 C 0.1080(3) -0.1621(3) 0.23199(15) 0.0383(6) Uani 1 1 d . . . . .
H26 H 0.099186 -0.189781 0.279790 0.046 Uiso 1 1 calc R U . . .
C27 C 0.0506(3) -0.2537(3) 0.17091(16) 0.0429(6) Uani 1 1 d . . . . .
H27 H -0.002007 -0.349961 0.170641 0.051 Uiso 1 1 calc R U . . .
C28 C 0.0883(3) -0.1719(3) 0.11201(14) 0.0340(5) Uani 1 1 d . . . . .
H28 H 0.066441 -0.202395 0.063560 0.041 Uiso 1 1 calc R U . . .
N29 N 0.3793(2) 0.4470(2) 0.17535(10) 0.0251(3) Uani 1 1 d . . . . .
N30 N 0.3637(2) 0.4051(2) 0.24516(9) 0.0252(3) Uani 1 1 d . . . . .
C31 C 0.4124(3) 0.5292(3) 0.28554(15) 0.0357(5) Uani 1 1 d . . . . .
H31 H 0.413737 0.534738 0.335675 0.043 Uiso 1 1 calc R U . . .
C32 C 0.4616(3) 0.6503(3) 0.24271(17) 0.0428(6) Uani 1 1 d . . . . .
H32 H 0.501243 0.748349 0.258542 0.051 Uiso 1 1 calc R U . . .
C33 C 0.4394(3) 0.5955(3) 0.17252(16) 0.0369(5) Uani 1 1 d . . . . .
H33 H 0.461203 0.649042 0.131224 0.044 Uiso 1 1 calc R U . . .
B34 B 0.2049(3) 0.7268(3) 0.43295(14) 0.0307(5) Uani 1 1 d . . . . .
F35 F 0.32364(18) 0.78098(16) 0.39381(7) 0.0362(3) Uani 1 1 d . . . . .
F36 F 0.2349(2) 0.77974(18) 0.50505(8) 0.0410(3) Uani 1 1 d . . . . .
F37 F 0.20663(19) 0.56315(17) 0.43342(8) 0.0405(3) Uani 1 1 d . . . . .
F38 F 0.0572(2) 0.7819(2) 0.40181(9) 0.0577(5) Uani 1 1 d . . . . .
B39 B 0.2782(4) 0.7353(3) -0.06120(14) 0.0358(6) Uani 1 1 d D . . . .
F40A F 0.3531(13) 0.7513(13) 0.0119(4) 0.0315(11) Uani 0.67 1 d D U P B 1
F41A F 0.3171(6) 0.8741(5) -0.0976(2) 0.0277(7) Uani 0.67 1 d D U P B 1
F42A F 0.1116(8) 0.7536(6) -0.0604(4) 0.0505(14) Uani 0.67 1 d D U P B 1
F43A F 0.3435(4) 0.6040(4) -0.09076(19) 0.0418(7) Uani 0.67 1 d D U P B 1
F40B F 0.351(3) 0.730(3) 0.0075(8) 0.040(4) Uani 0.33 1 d D U P B 2
F41B F 0.3272(14) 0.8344(10) -0.1099(5) 0.042(2) Uani 0.33 1 d D U P B 2
F42B F 0.1199(14) 0.7084(11) -0.0626(7) 0.0343(18) Uani 0.33 1 d D U P B 2
F43B F 0.2714(10) 0.5839(10) -0.0955(5) 0.063(2) Uani 0.33 1 d D U 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
Fe1 N2 1.9934(15) . ?
Fe1 N9 2.0830(18) . ?
Fe1 N14 2.048(2) . ?
Fe1 N18 1.9992(15) . ?
Fe1 N25 2.064(2) . ?
Fe1 N30 2.0748(18) . ?
Zn1 N2 1.9934(15) . ?
Zn1 N9 2.0830(18) . ?
Zn1 N14 2.048(2) . ?
Zn1 N18 1.9992(15) . ?
Zn1 N25 2.064(2) . ?
Zn1 N30 2.0748(18) . ?
N2 C3 1.335(2) . ?
N2 C7 1.339(2) . ?
C3 C4 1.382(3) . ?
C3 N8 1.405(2) . ?
C4 H4 0.9300 . ?
C4 C5 1.392(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.392(3) . ?
C6 H6 0.9300 . ?
C6 C7 1.375(3) . ?
C7 N13 1.406(3) . ?
N8 N9 1.372(2) . ?
N8 C12 1.362(3) . ?
N9 C10 1.329(3) . ?
C10 H10 0.9300 . ?
C10 C11 1.411(4) . ?
C11 H11 0.9300 . ?
C11 C12 1.367(3) . ?
C12 H12 0.9300 . ?
N13 N14 1.372(3) . ?
N13 C17 1.356(3) . ?
N14 C15 1.329(3) . ?
C15 H15 0.9300 . ?
C15 C16 1.398(5) . ?
C16 H16 0.9300 . ?
C16 C17 1.359(4) . ?
C17 H17 0.9300 . ?
N18 C19 1.332(3) . ?
N18 C23 1.338(3) . ?
C19 C20 1.378(3) . ?
C19 N24 1.409(3) . ?
C20 H20 0.9300 . ?
C20 C21 1.393(3) . ?
C21 H21 0.9300 . ?
C21 C22 1.388(3) . ?
C22 H22 0.9300 . ?
C22 C23 1.382(3) . ?
C23 N29 1.401(3) . ?
N24 N25 1.381(2) . ?
N24 C28 1.351(3) . ?
N25 C26 1.332(3) . ?
C26 H26 0.9300 . ?
C26 C27 1.406(4) . ?
C27 H27 0.9300 . ?
C27 C28 1.367(3) . ?
C28 H28 0.9300 . ?
N29 N30 1.366(2) . ?
N29 C33 1.362(3) . ?
N30 C31 1.326(3) . ?
C31 H31 0.9300 . ?
C31 C32 1.396(4) . ?
C32 H32 0.9300 . ?
C32 C33 1.372(4) . ?
C33 H33 0.9300 . ?
B34 F35 1.392(3) . ?
B34 F36 1.402(3) . ?
B34 F37 1.389(3) . ?
B34 F38 1.385(3) . ?
B39 F40A 1.425(7) . ?
B39 F41A 1.417(5) . ?
B39 F42A 1.418(7) . ?
B39 F43A 1.389(5) . ?
B39 F40B 1.340(14) . ?
B39 F41B 1.339(10) . ?
B39 F42B 1.354(12) . ?
B39 F43B 1.432(9) . ?

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 76.96(6) . . ?
N2 Fe1 N14 77.43(7) . . ?
N2 Fe1 N18 175.47(8) . . ?
N2 Fe1 N25 107.12(7) . . ?
N2 Fe1 N30 98.54(7) . . ?
N14 Fe1 N9 154.36(7) . . ?
N14 Fe1 N25 93.31(7) . . ?
N14 Fe1 N30 90.24(7) . . ?
N18 Fe1 N9 102.30(6) . . ?
N18 Fe1 N14 103.12(7) . . ?
N18 Fe1 N25 77.37(7) . . ?
N18 Fe1 N30 76.99(7) . . ?
N25 Fe1 N9 95.40(7) . . ?
N25 Fe1 N30 154.26(7) . . ?
N30 Fe1 N9 92.26(7) . . ?
N2 Zn1 N9 76.96(6) . . ?
N2 Zn1 N14 77.43(7) . . ?
N2 Zn1 N18 175.47(8) . . ?
N2 Zn1 N25 107.12(7) . . ?
N2 Zn1 N30 98.54(7) . . ?
N14 Zn1 N9 154.36(7) . . ?
N14 Zn1 N25 93.31(7) . . ?
N14 Zn1 N30 90.24(7) . . ?
N18 Zn1 N9 102.30(6) . . ?
N18 Zn1 N14 103.12(7) . . ?
N18 Zn1 N25 77.37(7) . . ?
N18 Zn1 N30 76.99(7) . . ?
N25 Zn1 N9 95.40(7) . . ?
N25 Zn1 N30 154.26(7) . . ?
N30 Zn1 N9 92.26(7) . . ?
C3 N2 Fe1 120.80(13) . . ?
C3 N2 Zn1 120.80(13) . . ?
C3 N2 C7 119.08(17) . . ?
C7 N2 Fe1 120.12(13) . . ?
C7 N2 Zn1 120.12(13) . . ?
N2 C3 C4 123.00(18) . . ?
N2 C3 N8 111.68(16) . . ?
C4 C3 N8 125.32(18) . . ?
C3 C4 H4 121.6 . . ?
C3 C4 C5 116.72(19) . . ?
C5 C4 H4 121.6 . . ?
C4 C5 H5 119.4 . . ?
C6 C5 C4 121.25(19) . . ?
C6 C5 H5 119.4 . . ?
C5 C6 H6 121.5 . . ?
C7 C6 C5 116.98(19) . . ?
C7 C6 H6 121.5 . . ?
N2 C7 C6 122.96(19) . . ?
N2 C7 N13 111.41(18) . . ?
C6 C7 N13 125.61(19) . . ?
N9 N8 C3 117.80(16) . . ?
C12 N8 C3 131.07(18) . . ?
C12 N8 N9 111.13(17) . . ?
N8 N9 Fe1 112.74(12) . . ?
N8 N9 Zn1 112.74(12) . . ?
C10 N9 Fe1 141.82(16) . . ?
C10 N9 Zn1 141.82(16) . . ?
C10 N9 N8 105.44(18) . . ?
N9 C10 H10 124.7 . . ?
N9 C10 C11 110.7(2) . . ?
C11 C10 H10 124.7 . . ?
C10 C11 H11 127.1 . . ?
C12 C11 C10 105.84(19) . . ?
C12 C11 H11 127.1 . . ?
N8 C12 C11 106.9(2) . . ?
N8 C12 H12 126.5 . . ?
C11 C12 H12 126.5 . . ?
N14 N13 C7 117.39(17) . . ?
C17 N13 C7 131.7(2) . . ?
C17 N13 N14 110.8(2) . . ?
N13 N14 Fe1 113.45(12) . . ?
N13 N14 Zn1 113.45(12) . . ?
C15 N14 Fe1 140.7(2) . . ?
C15 N14 Zn1 140.7(2) . . ?
C15 N14 N13 105.3(2) . . ?
N14 C15 H15 124.7 . . ?
N14 C15 C16 110.7(3) . . ?
C16 C15 H15 124.7 . . ?
C15 C16 H16 126.9 . . ?
C17 C16 C15 106.2(2) . . ?
C17 C16 H16 126.9 . . ?
N13 C17 C16 107.1(3) . . ?
N13 C17 H17 126.5 . . ?
C16 C17 H17 126.5 . . ?
C19 N18 Fe1 120.36(13) . . ?
C19 N18 Zn1 120.36(13) . . ?
C19 N18 C23 119.43(17) . . ?
C23 N18 Fe1 120.20(13) . . ?
C23 N18 Zn1 120.20(13) . . ?
N18 C19 C20 123.07(18) . . ?
N18 C19 N24 111.88(17) . . ?
C20 C19 N24 125.05(19) . . ?
C19 C20 H20 121.7 . . ?
C19 C20 C21 116.6(2) . . ?
C21 C20 H20 121.7 . . ?
C20 C21 H21 119.2 . . ?
C22 C21 C20 121.54(19) . . ?
C22 C21 H21 119.2 . . ?
C21 C22 H22 121.6 . . ?
C23 C22 C21 116.82(19) . . ?
C23 C22 H22 121.6 . . ?
N18 C23 C22 122.56(19) . . ?
N18 C23 N29 111.90(16) . . ?
C22 C23 N29 125.54(18) . . ?
N25 N24 C19 117.38(17) . . ?
C28 N24 C19 131.09(19) . . ?
C28 N24 N25 111.42(18) . . ?
N24 N25 Fe1 112.99(12) . . ?
N24 N25 Zn1 112.99(12) . . ?
C26 N25 Fe1 142.09(17) . . ?
C26 N25 Zn1 142.09(17) . . ?
C26 N25 N24 104.7(2) . . ?
N25 C26 H26 124.5 . . ?
N25 C26 C27 111.0(2) . . ?
C27 C26 H26 124.5 . . ?
C26 C27 H27 127.1 . . ?
C28 C27 C26 105.8(2) . . ?
C28 C27 H27 127.1 . . ?
N24 C28 C27 107.1(2) . . ?
N24 C28 H28 126.4 . . ?
C27 C28 H28 126.4 . . ?
N30 N29 C23 117.73(16) . . ?
C33 N29 C23 131.1(2) . . ?
C33 N29 N30 111.11(19) . . ?
N29 N30 Fe1 113.11(12) . . ?
N29 N30 Zn1 113.11(12) . . ?
C31 N30 Fe1 141.36(18) . . ?
C31 N30 Zn1 141.36(18) . . ?
C31 N30 N29 105.53(19) . . ?
N30 C31 H31 124.6 . . ?
N30 C31 C32 110.9(2) . . ?
C32 C31 H31 124.6 . . ?
C31 C32 H32 127.0 . . ?
C33 C32 C31 106.1(2) . . ?
C33 C32 H32 127.0 . . ?
N29 C33 C32 106.4(2) . . ?
N29 C33 H33 126.8 . . ?
C32 C33 H33 126.8 . . ?
F35 B34 F36 109.9(2) . . ?
F37 B34 F35 109.0(2) . . ?
F37 B34 F36 108.3(2) . . ?
F38 B34 F35 110.0(2) . . ?
F38 B34 F36 109.2(2) . . ?
F38 B34 F37 110.4(2) . . ?
F41A B39 F40A 105.8(5) . . ?
F41A B39 F42A 102.0(4) . . ?
F42A B39 F40A 107.2(5) . . ?
F43A B39 F40A 107.6(5) . . ?
F43A B39 F41A 110.4(3) . . ?
F43A B39 F42A 122.6(3) . . ?
F40B B39 F42B 109.8(12) . . ?
F40B B39 F43B 112.3(10) . . ?
F41B B39 F40B 121.3(11) . . ?
F41B B39 F42B 119.1(7) . . ?
F41B B39 F43B 105.1(5) . . ?
F42B B39 F43B 81.9(6) . . ?

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 -179.20(15) . . . . ?
Fe1 N2 C3 N8 1.5(2) . . . . ?
Fe1 N2 C7 C6 178.78(15) . . . . ?
Fe1 N2 C7 N13 -2.5(2) . . . . ?
Fe1 N9 C10 C11 -179.34(17) . . . . ?
Fe1 N14 C15 C16 -168.8(2) . . . . ?
Fe1 N18 C19 C20 179.83(15) . . . . ?
Fe1 N18 C19 N24 0.6(2) . . . . ?
Fe1 N18 C23 C22 -179.29(14) . . . . ?
Fe1 N18 C23 N29 0.1(2) . . . . ?
Fe1 N25 C26 C27 173.05(18) . . . . ?
Fe1 N30 C31 C32 179.55(17) . . . . ?
Zn1 N2 C3 C4 -179.20(15) . . . . ?
Zn1 N2 C3 N8 1.5(2) . . . . ?
Zn1 N2 C7 C6 178.78(15) . . . . ?
Zn1 N2 C7 N13 -2.5(2) . . . . ?
Zn1 N9 C10 C11 -179.34(17) . . . . ?
Zn1 N14 C15 C16 -168.8(2) . . . . ?
Zn1 N18 C19 C20 179.83(15) . . . . ?
Zn1 N18 C19 N24 0.6(2) . . . . ?
Zn1 N18 C23 C22 -179.29(14) . . . . ?
Zn1 N18 C23 N29 0.1(2) . . . . ?
Zn1 N25 C26 C27 173.05(18) . . . . ?
Zn1 N30 C31 C32 179.55(17) . . . . ?
N2 C3 C4 C5 0.4(3) . . . . ?
N2 C3 N8 N9 -0.2(2) . . . . ?
N2 C3 N8 C12 178.99(19) . . . . ?
N2 C7 N13 N14 4.8(2) . . . . ?
N2 C7 N13 C17 -171.5(2) . . . . ?
C3 N2 C7 C6 -0.9(3) . . . . ?
C3 N2 C7 N13 177.77(18) . . . . ?
C3 C4 C5 C6 -0.9(3) . . . . ?
C3 N8 N9 Fe1 -1.1(2) . . . . ?
C3 N8 N9 Zn1 -1.1(2) . . . . ?
C3 N8 N9 C10 178.86(16) . . . . ?
C3 N8 C12 C11 -179.22(19) . . . . ?
C4 C3 N8 N9 -179.46(18) . . . . ?
C4 C3 N8 C12 -0.3(3) . . . . ?
C4 C5 C6 C7 0.5(3) . . . . ?
C5 C6 C7 N2 0.4(3) . . . . ?
C5 C6 C7 N13 -178.09(19) . . . . ?
C6 C7 N13 N14 -176.50(18) . . . . ?
C6 C7 N13 C17 7.2(3) . . . . ?
C7 N2 C3 C4 0.5(3) . . . . ?
C7 N2 C3 N8 -178.81(17) . . . . ?
C7 N13 N14 Fe1 -4.9(2) . . . . ?
C7 N13 N14 Zn1 -4.9(2) . . . . ?
C7 N13 N14 C15 -177.87(18) . . . . ?
C7 N13 C17 C16 176.9(2) . . . . ?
N8 C3 C4 C5 179.60(18) . . . . ?
N8 N9 C10 C11 0.7(2) . . . . ?
N9 N8 C12 C11 0.0(2) . . . . ?
N9 C10 C11 C12 -0.8(2) . . . . ?
C10 C11 C12 N8 0.5(2) . . . . ?
C12 N8 N9 Fe1 179.61(13) . . . . ?
C12 N8 N9 Zn1 179.61(13) . . . . ?
C12 N8 N9 C10 -0.4(2) . . . . ?
N13 N14 C15 C16 1.0(3) . . . . ?
N14 N13 C17 C16 0.4(3) . . . . ?
N14 C15 C16 C17 -0.8(3) . . . . ?
C15 C16 C17 N13 0.2(3) . . . . ?
C17 N13 N14 Fe1 172.10(15) . . . . ?
C17 N13 N14 Zn1 172.10(15) . . . . ?
C17 N13 N14 C15 -0.8(2) . . . . ?
N18 C19 C20 C21 -0.5(3) . . . . ?
N18 C19 N24 N25 -1.1(2) . . . . ?
N18 C19 N24 C28 174.7(2) . . . . ?
N18 C23 N29 N30 -2.1(2) . . . . ?
N18 C23 N29 C33 -179.1(2) . . . . ?
C19 N18 C23 C22 -0.4(3) . . . . ?
C19 N18 C23 N29 178.95(16) . . . . ?
C19 C20 C21 C22 -0.4(3) . . . . ?
C19 N24 N25 Fe1 1.0(2) . . . . ?
C19 N24 N25 Zn1 1.0(2) . . . . ?
C19 N24 N25 C26 176.49(17) . . . . ?
C19 N24 C28 C27 -175.7(2) . . . . ?
C20 C19 N24 N25 179.72(18) . . . . ?
C20 C19 N24 C28 -4.5(3) . . . . ?
C20 C21 C22 C23 0.9(3) . . . . ?
C21 C22 C23 N18 -0.5(3) . . . . ?
C21 C22 C23 N29 -179.77(18) . . . . ?
C22 C23 N29 N30 177.28(18) . . . . ?
C22 C23 N29 C33 0.3(3) . . . . ?
C23 N18 C19 C20 1.0(3) . . . . ?
C23 N18 C19 N24 -178.26(16) . . . . ?
C23 N29 N30 Fe1 3.0(2) . . . . ?
C23 N29 N30 Zn1 3.0(2) . . . . ?
C23 N29 N30 C31 -176.76(17) . . . . ?
C23 N29 C33 C32 176.7(2) . . . . ?
N24 C19 C20 C21 178.58(18) . . . . ?
N24 N25 C26 C27 -0.1(2) . . . . ?
N25 N24 C28 C27 0.3(2) . . . . ?
N25 C26 C27 C28 0.3(3) . . . . ?
C26 C27 C28 N24 -0.4(3) . . . . ?
C28 N24 N25 Fe1 -175.56(14) . . . . ?
C28 N24 N25 Zn1 -175.56(14) . . . . ?
C28 N24 N25 C26 -0.1(2) . . . . ?
N29 N30 C31 C32 -0.8(2) . . . . ?
N30 N29 C33 C32 -0.5(2) . . . . ?
N30 C31 C32 C33 0.5(3) . . . . ?
C31 C32 C33 N29 0.0(3) . . . . ?
C33 N29 N30 Fe1 -179.42(13) . . . . ?
C33 N29 N30 Zn1 -179.42(13) . . . . ?
C33 N29 N30 C31 0.8(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_pg14lto
_database_code_depnum_ccdc_archive 'CCDC 2261791'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2023-05-09 deposited with the CCDC.	2023-08-30 downloaded from the CCDC.
;
_audit_creation_date             2023-03-13
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis[2,6-di(pyrazol-1-yl)pyridine]iron(II) bis[2,6-di(pyrazol-1-yl)pyridine]-ruthenium(II) ditetrafluoroborate 0.50:0.50 solid solution'
_chemical_formula_moiety         'C22 H18 Fe0.5 N10 Ru0.5, 2(B F4)'
_chemical_formula_sum            'C22 H18 B2 F8 Fe0.50 N10 Ru0.50'
_chemical_formula_weight         674.54
_chemical_absolute_configuration ab
_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 0.0019 0.0015 '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 0.0004 0.0006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0124 0.0097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.2961 0.8007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0037 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.5177 0.7911 '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           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   8.4455(1)
_cell_length_b                   8.5114(1)
_cell_length_c                   18.4035(1)
_cell_angle_alpha                90
_cell_angle_beta                 98.071(1)
_cell_angle_gamma                90
_cell_volume                     1309.80(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    18949
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      35.72
_cell_measurement_theta_min      1.08
_exptl_absorpt_coefficient_mu    0.629
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.901
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
DIALS 3.12.1-2-g1c07bc2b3-release
Scaling & analysis of unmerged intensities, absorption correction using 
spherical harmonics
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             674
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_unetI/netI     0.0735
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            30092
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        24.620
_diffrn_reflns_theta_max         36.110
_diffrn_reflns_theta_min         1.083
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.931
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_measurement_device       'Fixed χ 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_reflns_Friedel_coverage         0.819
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.845
_reflns_number_gt                11034
_reflns_number_total             12265
_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       'XIA2 0.4.0.438-g4431aaa (Winter, 2010)'
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction        'XIA2 0.4.0.438-g4431aaa (Winter, 2010)'
_computing_molecular_graphics    'XSEED (Barbour, 2020)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 
;
 Flack x determined using 3839 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(12)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         12265
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0433
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0247P)²+0.4984P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0890
_refine_special_details          
;
 In this refinement, the low temperature dataset was treated as a single, 
 averaged [FeₓRu₁₋ₓ(bpp)₂]2+ cation site. Partial Fe and Ru atoms
 were refined with the same cartesian coordinates, using the Fe~0.50~/
 Ru~0.50~ occupancy ratio obtained from the disordered refinement model 
 from this dataset. No anion disorder is included in the model. However, 
 an EADP thermal parameter constraint between the two partial metal atoms 
 was required to make the model converge.

 All 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
2. Uiso/Uaniso restraints and constraints
Uanis(Fe1) = Uanis(Ru1)
3. Others
 X(Fe1)=X(Ru1)=FVAR(1)
 Y(Fe1)=Y(Ru1)=FVAR(2)
 Z(Fe1)=Z(Ru1)=FVAR(3)
 Fixed Sof: Fe1(0.5) Ru1(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16),
 C17(H17), C20(H20), C21(H21), C22(H22), C26(H26), C27(H27), C28(H28), C31(H31),
  C32(H32), C33(H33)
;
_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 0.71686(2) 0.81310(3) 0.74640(2) 0.01168(5) Uani 0.5 1 d . . P A 1
Ru1 Ru 0.71686(2) 0.81310(3) 0.74640(2) 0.01168(5) Uani 0.5 1 d . . P A 2
N2 N 0.7125(2) 0.8318(3) 0.64073(10) 0.0148(4) Uani 1 1 d . . . . .
C3 C 0.5833(3) 0.8914(3) 0.59894(13) 0.0161(4) Uani 1 1 d . . . . .
C4 C 0.5738(3) 0.9046(3) 0.52321(13) 0.0191(4) Uani 1 1 d . . . . .
H4 H 0.481614 0.946347 0.494051 0.023 Uiso 1 1 calc R U . . .
C5 C 0.7057(3) 0.8539(3) 0.49217(13) 0.0212(5) Uani 1 1 d . . . . .
H5 H 0.704043 0.863321 0.440634 0.025 Uiso 1 1 calc R U . . .
C6 C 0.8401(3) 0.7899(3) 0.53406(13) 0.0200(5) Uani 1 1 d . . . . .
H6 H 0.929264 0.754255 0.512417 0.024 Uiso 1 1 calc R U . . .
C7 C 0.8370(3) 0.7808(3) 0.60918(12) 0.0162(4) Uani 1 1 d . . . . .
N8 N 0.4655(2) 0.9337(3) 0.64170(11) 0.0165(4) Uani 1 1 d . . . . .
N9 N 0.4965(2) 0.9081(3) 0.71659(11) 0.0162(3) Uani 1 1 d . . . . .
C10 C 0.3655(3) 0.9559(3) 0.74292(15) 0.0201(5) Uani 1 1 d . . . . .
H10 H 0.351228 0.951732 0.793171 0.024 Uiso 1 1 calc R U . . .
C11 C 0.2511(3) 1.0137(4) 0.68605(16) 0.0236(5) Uani 1 1 d . . . . .
H11 H 0.148699 1.055283 0.690835 0.028 Uiso 1 1 calc R U . . .
C12 C 0.3170(3) 0.9978(3) 0.62241(15) 0.0212(5) Uani 1 1 d . . . . .
H12 H 0.268878 1.025747 0.574375 0.025 Uiso 1 1 calc R U . . .
N13 N 0.9566(2) 0.7171(3) 0.66164(12) 0.0169(4) Uani 1 1 d . . . . .
N14 N 0.9319(2) 0.7225(3) 0.73422(11) 0.0162(4) Uani 1 1 d . . . . .
C15 C 1.0579(3) 0.6520(4) 0.77151(15) 0.0214(5) Uani 1 1 d . . . . .
H15 H 1.074353 0.638372 0.823256 0.026 Uiso 1 1 calc R U . . .
C16 C 1.1639(3) 0.6001(4) 0.72404(17) 0.0263(6) Uani 1 1 d . . . . .
H16 H 1.262264 0.546231 0.737243 0.032 Uiso 1 1 calc R U . . .
C17 C 1.0962(3) 0.6431(4) 0.65489(16) 0.0219(5) Uani 1 1 d . . . . .
H17 H 1.138892 0.624590 0.610570 0.026 Uiso 1 1 calc R U . . .
N18 N 0.7204(2) 0.7862(3) 0.85200(11) 0.0168(4) Uani 1 1 d . . . . .
C19 C 0.7796(3) 0.8996(3) 0.89847(12) 0.0160(4) Uani 1 1 d . . . . .
C20 C 0.7860(3) 0.8846(4) 0.97383(13) 0.0190(4) Uani 1 1 d . . . . .
H20 H 0.826987 0.966113 1.006407 0.023 Uiso 1 1 calc R U . . .
C21 C 0.7298(3) 0.7448(4) 0.99946(13) 0.0202(5) Uani 1 1 d . . . . .
H21 H 0.731771 0.731019 1.050812 0.024 Uiso 1 1 calc R U . . .
C22 C 0.6706(3) 0.6242(4) 0.95226(13) 0.0199(5) Uani 1 1 d . . . . .
H22 H 0.633866 0.528067 0.970120 0.024 Uiso 1 1 calc R U . . .
C23 C 0.6679(3) 0.6514(3) 0.87804(13) 0.0163(4) Uani 1 1 d . . . . .
N24 N 0.8319(2) 1.0283(3) 0.86091(11) 0.0169(4) Uani 1 1 d . . . . .
N25 N 0.8165(2) 1.0203(3) 0.78501(11) 0.0169(4) Uani 1 1 d . . . . .
C26 C 0.8839(3) 1.1504(3) 0.76432(14) 0.0203(5) Uani 1 1 d . . . . .
H26 H 0.890444 1.177936 0.714804 0.024 Uiso 1 1 calc R U . . .
C27 C 0.9447(3) 1.2423(4) 0.82561(16) 0.0239(5) Uani 1 1 d . . . . .
H27 H 0.998587 1.340245 0.825277 0.029 Uiso 1 1 calc R U . . .
C28 C 0.9098(3) 1.1612(4) 0.88596(15) 0.0215(5) Uani 1 1 d . . . . .
H28 H 0.935434 1.192341 0.935800 0.026 Uiso 1 1 calc R U . . .
N29 N 0.6135(2) 0.5468(3) 0.82060(12) 0.0173(4) Uani 1 1 d . . . . .
N30 N 0.6264(2) 0.5941(3) 0.75003(11) 0.0168(4) Uani 1 1 d . . . . .
C31 C 0.5786(3) 0.4718(3) 0.70781(15) 0.0203(5) Uani 1 1 d . . . . .
H31 H 0.575298 0.469534 0.656009 0.024 Uiso 1 1 calc R U . . .
C32 C 0.5335(3) 0.3459(3) 0.75003(17) 0.0238(5) Uani 1 1 d . . . . .
H32 H 0.494502 0.246030 0.732717 0.029 Uiso 1 1 calc R U . . .
C33 C 0.5575(3) 0.3974(3) 0.82156(16) 0.0218(5) Uani 1 1 d . . . . .
H33 H 0.538488 0.339562 0.863626 0.026 Uiso 1 1 calc R U . . .
B34 B 0.7966(4) 0.2744(4) 0.56384(16) 0.0221(6) Uani 1 1 d . . . . .
F35 F 0.6775(2) 0.2216(2) 0.60281(9) 0.0259(3) Uani 1 1 d . . . . .
F36 F 0.7666(3) 0.2234(2) 0.49098(10) 0.0301(4) Uani 1 1 d . . . . .
F37 F 0.7976(3) 0.4388(2) 0.56409(11) 0.0313(4) Uani 1 1 d . . . . .
F38 F 0.9447(2) 0.2174(3) 0.59609(11) 0.0430(6) Uani 1 1 d . . . . .
B39 B 0.7173(4) 0.2514(4) 1.05724(16) 0.0240(6) Uani 1 1 d . . . . .
F40 F 0.6420(2) 0.2401(2) 0.98476(9) 0.0268(4) Uani 1 1 d . . . B 1
F41 F 0.6816(2) 0.1206(3) 1.09747(10) 0.0293(4) Uani 1 1 d . . . C 1
F42 F 0.8825(2) 0.2545(3) 1.05685(10) 0.0404(6) Uani 1 1 d . . . D 1
F43 F 0.6652(4) 0.3859(3) 1.08896(12) 0.0502(7) Uani 1 1 d . . . E 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 1.9464(18) . ?
Fe1 N9 2.033(2) . ?
Fe1 N14 2.015(2) . ?
Fe1 N18 1.9528(19) . ?
Fe1 N25 2.038(2) . ?
Fe1 N30 2.019(2) . ?
Ru1 N2 1.9464(18) . ?
Ru1 N9 2.033(2) . ?
Ru1 N14 2.015(2) . ?
Ru1 N18 1.9528(19) . ?
Ru1 N25 2.038(2) . ?
Ru1 N30 2.019(2) . ?
N2 C3 1.344(3) . ?
N2 C7 1.343(3) . ?
C3 C4 1.389(3) . ?
C3 N8 1.399(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.391(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.390(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.389(3) . ?
C7 N13 1.404(3) . ?
N8 N9 1.383(3) . ?
N8 C12 1.368(3) . ?
N9 C10 1.332(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.410(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.372(4) . ?
C12 H12 0.9500 . ?
N13 N14 1.381(3) . ?
N13 C17 1.358(3) . ?
N14 C15 1.326(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.407(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.370(4) . ?
C17 H17 0.9500 . ?
N18 C19 1.339(3) . ?
N18 C23 1.342(3) . ?
C19 C20 1.386(3) . ?
C19 N24 1.399(3) . ?
C20 H20 0.9500 . ?
C20 C21 1.388(4) . ?
C21 H21 0.9500 . ?
C21 C22 1.391(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.382(3) . ?
C23 N29 1.409(3) . ?
N24 N25 1.386(3) . ?
N24 C28 1.357(4) . ?
N25 C26 1.325(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.409(4) . ?
C27 H27 0.9500 . ?
C27 C28 1.374(4) . ?
C28 H28 0.9500 . ?
N29 N30 1.378(3) . ?
N29 C33 1.358(4) . ?
N30 C31 1.328(3) . ?
C31 H31 0.9500 . ?
C31 C32 1.407(4) . ?
C32 H32 0.9500 . ?
C32 C33 1.376(4) . ?
C33 H33 0.9500 . ?
B34 F35 1.390(4) . ?
B34 F36 1.398(4) . ?
B34 F37 1.399(4) . ?
B34 F38 1.394(4) . ?
B39 F40 1.398(4) . ?
B39 F41 1.393(4) . ?
B39 F42 1.397(4) . ?
B39 F43 1.384(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 79.03(8) . . ?
N2 Fe1 N14 79.10(8) . . ?
N2 Fe1 N18 177.94(11) . . ?
N2 Fe1 N25 103.09(9) . . ?
N2 Fe1 N30 98.88(9) . . ?
N9 Fe1 N25 93.87(9) . . ?
N14 Fe1 N9 158.11(8) . . ?
N14 Fe1 N25 92.02(9) . . ?
N14 Fe1 N30 90.10(9) . . ?
N18 Fe1 N9 101.59(8) . . ?
N18 Fe1 N14 100.23(8) . . ?
N18 Fe1 N25 78.85(9) . . ?
N18 Fe1 N30 79.15(9) . . ?
N30 Fe1 N9 92.29(9) . . ?
N30 Fe1 N25 157.93(8) . . ?
N2 Ru1 N9 79.03(8) . . ?
N2 Ru1 N14 79.10(8) . . ?
N2 Ru1 N18 177.94(11) . . ?
N2 Ru1 N25 103.09(9) . . ?
N2 Ru1 N30 98.88(9) . . ?
N9 Ru1 N25 93.87(9) . . ?
N14 Ru1 N9 158.11(8) . . ?
N14 Ru1 N25 92.02(9) . . ?
N14 Ru1 N30 90.10(9) . . ?
N18 Ru1 N9 101.59(8) . . ?
N18 Ru1 N14 100.23(8) . . ?
N18 Ru1 N25 78.85(9) . . ?
N18 Ru1 N30 79.15(9) . . ?
N30 Ru1 N9 92.29(9) . . ?
N30 Ru1 N25 157.93(8) . . ?
C3 N2 Fe1 120.17(16) . . ?
C3 N2 Ru1 120.17(16) . . ?
C7 N2 Fe1 119.98(15) . . ?
C7 N2 Ru1 119.98(15) . . ?
C7 N2 C3 119.82(19) . . ?
N2 C3 C4 122.2(2) . . ?
N2 C3 N8 111.1(2) . . ?
C4 C3 N8 126.7(2) . . ?
C3 C4 H4 121.6 . . ?
C3 C4 C5 116.8(2) . . ?
C5 C4 H4 121.6 . . ?
C4 C5 H5 118.9 . . ?
C6 C5 C4 122.2(2) . . ?
C6 C5 H5 118.9 . . ?
C5 C6 H6 121.7 . . ?
C7 C6 C5 116.5(2) . . ?
C7 C6 H6 121.7 . . ?
N2 C7 C6 122.5(2) . . ?
N2 C7 N13 111.0(2) . . ?
C6 C7 N13 126.5(2) . . ?
N9 N8 C3 118.04(19) . . ?
C12 N8 C3 130.9(2) . . ?
C12 N8 N9 111.1(2) . . ?
N8 N9 Fe1 111.67(15) . . ?
N8 N9 Ru1 111.67(15) . . ?
C10 N9 Fe1 143.02(18) . . ?
C10 N9 Ru1 143.02(18) . . ?
C10 N9 N8 105.3(2) . . ?
N9 C10 H10 124.6 . . ?
N9 C10 C11 110.7(2) . . ?
C11 C10 H10 124.6 . . ?
C10 C11 H11 126.8 . . ?
C12 C11 C10 106.3(2) . . ?
C12 C11 H11 126.8 . . ?
N8 C12 C11 106.5(2) . . ?
N8 C12 H12 126.7 . . ?
C11 C12 H12 126.7 . . ?
N14 N13 C7 117.44(19) . . ?
C17 N13 C7 131.8(2) . . ?
C17 N13 N14 110.8(2) . . ?
N13 N14 Fe1 112.38(14) . . ?
N13 N14 Ru1 112.38(14) . . ?
C15 N14 Fe1 141.83(18) . . ?
C15 N14 Ru1 141.83(18) . . ?
C15 N14 N13 105.5(2) . . ?
N14 C15 H15 124.6 . . ?
N14 C15 C16 110.8(2) . . ?
C16 C15 H15 124.6 . . ?
C15 C16 H16 127.0 . . ?
C17 C16 C15 105.9(2) . . ?
C17 C16 H16 127.0 . . ?
N13 C17 C16 107.1(2) . . ?
N13 C17 H17 126.5 . . ?
C16 C17 H17 126.5 . . ?
C19 N18 Fe1 120.22(17) . . ?
C19 N18 Ru1 120.22(17) . . ?
C19 N18 C23 120.0(2) . . ?
C23 N18 Fe1 119.73(17) . . ?
C23 N18 Ru1 119.73(17) . . ?
N18 C19 C20 122.1(2) . . ?
N18 C19 N24 111.4(2) . . ?
C20 C19 N24 126.6(2) . . ?
C19 C20 H20 121.6 . . ?
C19 C20 C21 116.9(2) . . ?
C21 C20 H20 121.6 . . ?
C20 C21 H21 119.0 . . ?
C20 C21 C22 122.0(2) . . ?
C22 C21 H21 119.0 . . ?
C21 C22 H22 121.7 . . ?
C23 C22 C21 116.6(3) . . ?
C23 C22 H22 121.7 . . ?
N18 C23 C22 122.4(2) . . ?
N18 C23 N29 111.2(2) . . ?
C22 C23 N29 126.4(2) . . ?
N25 N24 C19 117.9(2) . . ?
C28 N24 C19 131.0(2) . . ?
C28 N24 N25 110.8(2) . . ?
N24 N25 Fe1 111.69(16) . . ?
N24 N25 Ru1 111.69(16) . . ?
C26 N25 Fe1 142.72(18) . . ?
C26 N25 Ru1 142.72(18) . . ?
C26 N25 N24 105.4(2) . . ?
N25 C26 H26 124.5 . . ?
N25 C26 C27 110.9(2) . . ?
C27 C26 H26 124.5 . . ?
C26 C27 H27 127.1 . . ?
C28 C27 C26 105.8(3) . . ?
C28 C27 H27 127.1 . . ?
N24 C28 C27 107.0(2) . . ?
N24 C28 H28 126.5 . . ?
C27 C28 H28 126.5 . . ?
N30 N29 C23 117.5(2) . . ?
C33 N29 C23 131.3(2) . . ?
C33 N29 N30 111.1(2) . . ?
N29 N30 Fe1 112.41(16) . . ?
N29 N30 Ru1 112.41(16) . . ?
C31 N30 Fe1 142.19(19) . . ?
C31 N30 Ru1 142.19(19) . . ?
C31 N30 N29 105.3(2) . . ?
N30 C31 H31 124.5 . . ?
N30 C31 C32 111.0(2) . . ?
C32 C31 H31 124.5 . . ?
C31 C32 H32 127.2 . . ?
C33 C32 C31 105.7(2) . . ?
C33 C32 H32 127.2 . . ?
N29 C33 C32 106.9(2) . . ?
N29 C33 H33 126.5 . . ?
C32 C33 H33 126.5 . . ?
F35 B34 F36 110.3(3) . . ?
F35 B34 F37 109.0(2) . . ?
F35 B34 F38 109.8(2) . . ?
F36 B34 F37 108.3(2) . . ?
F38 B34 F36 109.4(2) . . ?
F38 B34 F37 110.0(3) . . ?
F41 B39 F40 110.4(3) . . ?
F41 B39 F42 108.0(3) . . ?
F42 B39 F40 108.5(2) . . ?
F43 B39 F40 109.3(3) . . ?
F43 B39 F41 109.3(2) . . ?
F43 B39 F42 111.3(3) . . ?

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(2) . . . . ?
Fe1 N2 C3 N8 0.3(3) . . . . ?
Fe1 N2 C7 C6 179.4(2) . . . . ?
Fe1 N2 C7 N13 0.6(3) . . . . ?
Fe1 N9 C10 C11 179.9(2) . . . . ?
Fe1 N14 C15 C16 172.2(2) . . . . ?
Fe1 N18 C19 C20 -179.27(18) . . . . ?
Fe1 N18 C19 N24 0.4(3) . . . . ?
Fe1 N18 C23 C22 178.61(18) . . . . ?
Fe1 N18 C23 N29 -0.9(3) . . . . ?
Fe1 N25 C26 C27 -173.1(2) . . . . ?
Fe1 N30 C31 C32 176.8(2) . . . . ?
Ru1 N2 C3 C4 -179.0(2) . . . . ?
Ru1 N2 C3 N8 0.3(3) . . . . ?
Ru1 N2 C7 C6 179.4(2) . . . . ?
Ru1 N2 C7 N13 0.6(3) . . . . ?
Ru1 N9 C10 C11 179.9(2) . . . . ?
Ru1 N14 C15 C16 172.2(2) . . . . ?
Ru1 N18 C19 C20 -179.27(18) . . . . ?
Ru1 N18 C19 N24 0.4(3) . . . . ?
Ru1 N18 C23 C22 178.61(18) . . . . ?
Ru1 N18 C23 N29 -0.9(3) . . . . ?
Ru1 N25 C26 C27 -173.1(2) . . . . ?
Ru1 N30 C31 C32 176.8(2) . . . . ?
N2 C3 C4 C5 -0.4(4) . . . . ?
N2 C3 N8 N9 -0.6(3) . . . . ?
N2 C3 N8 C12 -179.9(3) . . . . ?
N2 C7 N13 N14 -2.6(3) . . . . ?
N2 C7 N13 C17 174.9(3) . . . . ?
C3 N2 C7 C6 1.4(4) . . . . ?
C3 N2 C7 N13 -177.5(2) . . . . ?
C3 C4 C5 C6 1.3(4) . . . . ?
C3 N8 N9 Fe1 0.6(3) . . . . ?
C3 N8 N9 Ru1 0.6(3) . . . . ?
C3 N8 N9 C10 -179.0(2) . . . . ?
C3 N8 C12 C11 179.3(3) . . . . ?
C4 C3 N8 N9 178.6(3) . . . . ?
C4 C3 N8 C12 -0.7(5) . . . . ?
C4 C5 C6 C7 -0.8(4) . . . . ?
C5 C6 C7 N2 -0.5(4) . . . . ?
C5 C6 C7 N13 178.2(3) . . . . ?
C6 C7 N13 N14 178.6(2) . . . . ?
C6 C7 N13 C17 -3.9(5) . . . . ?
C7 N2 C3 C4 -0.9(4) . . . . ?
C7 N2 C3 N8 178.4(2) . . . . ?
C7 N13 N14 Fe1 3.3(3) . . . . ?
C7 N13 N14 Ru1 3.3(3) . . . . ?
C7 N13 N14 C15 178.3(2) . . . . ?
C7 N13 C17 C16 -177.8(3) . . . . ?
N8 C3 C4 C5 -179.6(3) . . . . ?
N8 N9 C10 C11 -0.6(3) . . . . ?
N9 N8 C12 C11 0.0(3) . . . . ?
N9 C10 C11 C12 0.6(3) . . . . ?
C10 C11 C12 N8 -0.4(3) . . . . ?
C12 N8 N9 Fe1 -179.95(18) . . . . ?
C12 N8 N9 Ru1 -179.95(18) . . . . ?
C12 N8 N9 C10 0.4(3) . . . . ?
N13 N14 C15 C16 -0.3(3) . . . . ?
N14 N13 C17 C16 -0.2(3) . . . . ?
N14 C15 C16 C17 0.2(4) . . . . ?
C15 C16 C17 N13 0.0(3) . . . . ?
C17 N13 N14 Fe1 -174.66(19) . . . . ?
C17 N13 N14 Ru1 -174.66(19) . . . . ?
C17 N13 N14 C15 0.3(3) . . . . ?
N18 C19 C20 C21 0.8(4) . . . . ?
N18 C19 N24 N25 -0.3(3) . . . . ?
N18 C19 N24 C28 -174.2(2) . . . . ?
N18 C23 N29 N30 1.9(3) . . . . ?
N18 C23 N29 C33 176.9(2) . . . . ?
C19 N18 C23 C22 0.7(3) . . . . ?
C19 N18 C23 N29 -178.8(2) . . . . ?
C19 C20 C21 C22 0.5(4) . . . . ?
C19 N24 N25 Fe1 0.1(3) . . . . ?
C19 N24 N25 Ru1 0.1(3) . . . . ?
C19 N24 N25 C26 -175.9(2) . . . . ?
C19 N24 C28 C27 174.8(3) . . . . ?
C20 C19 N24 N25 179.4(2) . . . . ?
C20 C19 N24 C28 5.5(4) . . . . ?
C20 C21 C22 C23 -1.1(4) . . . . ?
C21 C22 C23 N18 0.5(4) . . . . ?
C21 C22 C23 N29 180.0(2) . . . . ?
C22 C23 N29 N30 -177.6(2) . . . . ?
C22 C23 N29 C33 -2.6(4) . . . . ?
C23 N18 C19 C20 -1.4(3) . . . . ?
C23 N18 C19 N24 178.3(2) . . . . ?
C23 N29 N30 Fe1 -2.0(3) . . . . ?
C23 N29 N30 Ru1 -2.0(3) . . . . ?
C23 N29 N30 C31 175.6(2) . . . . ?
C23 N29 C33 C32 -175.2(2) . . . . ?
N24 C19 C20 C21 -178.9(2) . . . . ?
N24 N25 C26 C27 0.7(3) . . . . ?
N25 N24 C28 C27 0.6(3) . . . . ?
N25 C26 C27 C28 -0.3(3) . . . . ?
C26 C27 C28 N24 -0.2(3) . . . . ?
C28 N24 N25 Fe1 175.14(17) . . . . ?
C28 N24 N25 Ru1 175.14(17) . . . . ?
C28 N24 N25 C26 -0.8(3) . . . . ?
N29 N30 C31 C32 0.5(3) . . . . ?
N30 N29 C33 C32 0.1(3) . . . . ?
N30 C31 C32 C33 -0.5(3) . . . . ?
C31 C32 C33 N29 0.2(3) . . . . ?
C33 N29 N30 Fe1 -177.95(16) . . . . ?
C33 N29 N30 Ru1 -177.95(16) . . . . ?
C33 N29 N30 C31 -0.4(3) . . . . ?

_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_mh202ht
_database_code_depnum_ccdc_archive 'CCDC 2261793'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2023-05-09 deposited with the CCDC.	2023-08-30 downloaded from the CCDC.
;
_audit_creation_date             2023-03-24
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis[2,6-di(pyrazol-1-yl)pyridine]iron(II) bis[2,6-di(pyrazol-1-yl)pyridine]-nickel(II) ditetrafluoroborate 0.46:0.54 solid solution'
_chemical_formula_moiety         'C22 H18 Fe0.46 N10 Ni0.54, 2(B F4)'
_chemical_formula_sum            'C22 H18 B2 F8 Fe0.46 N10 Ni0.54'
_chemical_formula_weight         653.48
_chemical_absolute_configuration ab
_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 0.0019 0.0015 '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 0.0004 0.0006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0124 0.0097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.2961 0.8007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0037 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.2866 1.0558 '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           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   8.5413(1)
_cell_length_b                   8.5895(1)
_cell_length_c                   18.9944(2)
_cell_angle_alpha                90
_cell_angle_beta                 95.702(1)
_cell_angle_gamma                90
_cell_volume                     1386.64(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9726
_cell_measurement_temperature    350.15
_cell_measurement_theta_max      28.18
_cell_measurement_theta_min      1.04
_exptl_absorpt_coefficient_mu    0.660
_exptl_absorpt_correction_T_min  0.958
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
DIALS 3.12.1-2-g1c07bc2b3-release
Scaling & analysis of unmerged intensities, absorption correction using 
spherical harmonics
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       lath
_exptl_crystal_F_000             658
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17249
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        24.620
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         1.044
_diffrn_ambient_temperature      350.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_measurement_device       'Fixed χ 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_reflns_Friedel_coverage         0.750
_reflns_Friedel_fraction_full    0.912
_reflns_Friedel_fraction_max     0.847
_reflns_number_gt                4516
_reflns_number_total             6811
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'XIA2 0.4.0.438-g4431aaa (Winter, 2010)'
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction        'XIA2 0.4.0.438-g4431aaa (Winter, 2010)'
_computing_molecular_graphics    'XSEED (Barbour, 2020)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         6811
_refine_ls_number_restraints     61
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0618
_refine_ls_restrained_S_all      1.187
_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)+(0.0915P)²+0.2121P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1634
_refine_ls_wR_factor_ref         0.2042
_refine_special_details          
;Unlike the low temperature structure, separate partial [Fe(bpp)₂]2+
 and [Ni(bpp)₂]2+ molecule sites could not be refined at this temperature.
 Hence, the organic ligand framework was modelled as crystallographically
 ordered. Attempts to distinguish Fe and Zn half-atoms in the Fourier map
 were also unproductive, so a mixed Fe~0.46~/Ni~0.54~ metal site was 
 refined with the same atomic coordinates, but independently refined 
 displacement parameters. The metal occupancies from the 100 K structure
 were used, since these could be accurately refined.

 The F atoms of both anions are also disordered, over three sites with a
 0.50:0.25:0.25 occupancy ratio. These were treated with the refined
 distance restraints listed below. An EADP thermal parameter constraint
 between the two partial metal atoms was also required to make the
 refinement converge.

 All crystallographically ordered non-H atoms plus the partial metal sites 
 were refined anisotropically, and H atoms were placed in calculated positions 
 and refined using a riding model.

 A minor merohedral twin domain was included in the refinement, to account for
 the slightly high Flack parameter given by this crystal at low temperature.,Twin
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.98(3)
 0.02(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 B34-F35A = B34-F36A = B34-F37A = B34-F38A
 1.39004 with sigma of 0.02
 B34-F35B = B34-F36B = B34-F37B = B34-F38B
 1.39004 with sigma of 0.02
 B34-F35C = B34-F36C = B34-F37C = B34-F38C
 1.39004 with sigma of 0.02
 B39-F40A = B39-F41A = B39-F42A = B39-F43A
 1.39004 with sigma of 0.02
 B39-F40B = B39-F41B = B39-F42B = B39-F43B
 1.39004 with sigma of 0.02
 B39-F40C = B39-F41C = B39-F42C = B39-F43C
 1.39004 with sigma of 0.02
 F35A-F36A = F35A-F37A = F35A-F38A = F36A-F37A = F36A-F38A = F37A-F38A
 2.269935 with sigma of 0.02
 F35B-F36B = F35B-F37B = F35B-F38B = F36B-F37B = F36B-F38B = F37B-F38B
 2.269935 with sigma of 0.02
 F35C-F36C = F35C-F37C = F35C-F38C = F36C-F37C = F36C-F38C = F37C-F38C
 2.269935 with sigma of 0.02
 F40A-F41A = F40A-F42A = F40A-F43A = F41A-F42A = F41A-F43A = F42A-F43A
 2.269935 with sigma of 0.02
 F40B-F41B = F40B-F42B = F40B-F43B = F41B-F42B = F41B-F43B = F42B-F43B
 2.269935 with sigma of 0.02
 F40C-F41C = F40C-F42C = F40C-F43C = F41C-F42C = F41C-F43C = F42C-F43C
 2.269935 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Fe1) = Uanis(Ni1)
5. 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)
 X(Fe1)=X(Ni1)=FVAR(2)
 Y(Fe1)=Y(Ni1)=FVAR(3)
 Z(Fe1)=Z(Ni1)=FVAR(4)
 Fixed Sof: Fe1(0.46) Ni1(0.54) F35A(0.5) F36A(0.5) F37A(0.5) F38A(0.5)
 F35B(0.25) F36B(0.25) F37B(0.25) F38B(0.25) F35C(0.25) F36C(0.25) F37C(0.25)
 F38C(0.25) F40A(0.5) F41A(0.5) F42A(0.5) F43A(0.5) F40B(0.25) F41B(0.25)
 F42B(0.25) F43B(0.25) F40C(0.25) F41C(0.25) F42C(0.25) F43C(0.25)
6.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16),
 C17(H17), C20(H20), C21(H21), C22(H22), C26(H26), C27(H27), C28(H28), C31(H31),
  C32(H32), C33(H33)
;
_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 0.73084(9) 0.81275(14) 0.74764(4) 0.0681(3) Uani 0.46 1 d . . P A 1
Ni1 Ni 0.73084(9) 0.81275(14) 0.74764(4) 0.0681(3) Uani 0.54 1 d . . P A 2
N2 N 0.7201(5) 0.8188(9) 0.6387(2) 0.0647(10) Uani 1 1 d . . . . .
C3 C 0.5936(8) 0.8743(8) 0.6007(3) 0.0708(15) Uani 1 1 d . . . . .
C4 C 0.5822(11) 0.8823(10) 0.5277(4) 0.090(2) Uani 1 1 d . . . . .
H4 H 0.492709 0.921606 0.501848 0.107 Uiso 1 1 calc R U . . .
C5 C 0.7075(12) 0.8303(14) 0.4951(4) 0.100(2) Uani 1 1 d . . . . .
H5 H 0.703850 0.834959 0.446068 0.120 Uiso 1 1 calc R U . . .
C6 C 0.8394(11) 0.7708(11) 0.5336(4) 0.091(2) Uani 1 1 d . . . . .
H6 H 0.924432 0.733840 0.511540 0.109 Uiso 1 1 calc R U . . .
C7 C 0.8397(8) 0.7686(8) 0.6050(4) 0.0722(17) Uani 1 1 d . . . . .
N8 N 0.4750(6) 0.9218(7) 0.6428(3) 0.0730(13) Uani 1 1 d . . . . .
N9 N 0.5023(7) 0.9070(7) 0.7146(3) 0.0748(14) Uani 1 1 d . . . . .
C10 C 0.3727(9) 0.9576(9) 0.7393(5) 0.086(2) Uani 1 1 d . . . . .
H10 H 0.356562 0.959150 0.787042 0.103 Uiso 1 1 calc R U . . .
C11 C 0.2633(10) 1.0084(11) 0.6851(6) 0.102(3) Uani 1 1 d . . . . .
H11 H 0.164224 1.049888 0.689703 0.122 Uiso 1 1 calc R U . . .
C12 C 0.3303(9) 0.9851(10) 0.6244(6) 0.097(3) Uani 1 1 d . . . . .
H12 H 0.286115 1.007825 0.578777 0.117 Uiso 1 1 calc R U . . .
N13 N 0.9631(7) 0.7093(7) 0.6516(4) 0.0788(15) Uani 1 1 d . . . . .
N14 N 0.9505(7) 0.7204(8) 0.7229(3) 0.0798(16) Uani 1 1 d . . . . .
C15 C 1.0765(9) 0.6505(11) 0.7533(5) 0.097(2) Uani 1 1 d . . . . .
H15 H 1.098760 0.636860 0.801787 0.116 Uiso 1 1 calc R U . . .
C16 C 1.1717(11) 0.5998(13) 0.7027(7) 0.123(4) Uani 1 1 d . . . . .
H16 H 1.269201 0.551669 0.711304 0.147 Uiso 1 1 calc R U . . .
C17 C 1.0965(10) 0.6334(11) 0.6387(6) 0.105(3) Uani 1 1 d . . . . .
H17 H 1.129329 0.609424 0.594772 0.125 Uiso 1 1 calc R U . . .
N18 N 0.7330(5) 0.7952(9) 0.8562(2) 0.0663(13) Uani 1 1 d . . . . .
C19 C 0.7841(7) 0.9087(9) 0.8986(3) 0.0696(15) Uani 1 1 d . . . . .
C20 C 0.7869(9) 0.9034(11) 0.9713(4) 0.0837(19) Uani 1 1 d . . . . .
H20 H 0.825039 0.985538 0.999982 0.100 Uiso 1 1 calc R U . . .
C21 C 0.7298(11) 0.7688(13) 0.9988(5) 0.102(3) Uani 1 1 d . . . . .
H21 H 0.727105 0.759902 1.047489 0.123 Uiso 1 1 calc R U . . .
C22 C 0.6767(9) 0.6476(11) 0.9558(4) 0.088(2) Uani 1 1 d . . . . .
H22 H 0.639993 0.556265 0.974727 0.105 Uiso 1 1 calc R U . . .
C23 C 0.6791(7) 0.6647(9) 0.8847(4) 0.0703(15) Uani 1 1 d . . . . .
N24 N 0.8407(6) 1.0367(7) 0.8612(3) 0.0721(14) Uani 1 1 d . . . . .
N25 N 0.8300(7) 1.0287(8) 0.7891(3) 0.0779(14) Uani 1 1 d . . . . .
C26 C 0.8968(9) 1.1577(10) 0.7691(5) 0.088(2) Uani 1 1 d . . . . .
H26 H 0.906425 1.185026 0.722359 0.105 Uiso 1 1 calc R U . . .
C27 C 0.9515(11) 1.2481(11) 0.8283(6) 0.101(3) Uani 1 1 d . . . . .
H27 H 1.003106 1.343444 0.828462 0.121 Uiso 1 1 calc R U . . .
C28 C 0.9132(10) 1.1676(12) 0.8838(5) 0.096(2) Uani 1 1 d . . . . .
H28 H 0.933680 1.197645 0.930826 0.116 Uiso 1 1 calc R U . . .
N29 N 0.6275(7) 0.5528(7) 0.8328(4) 0.0788(15) Uani 1 1 d . . . . .
N30 N 0.6411(7) 0.5847(7) 0.7644(4) 0.0808(15) Uani 1 1 d . . . . .
C31 C 0.5902(9) 0.4569(10) 0.7298(5) 0.092(2) Uani 1 1 d . . . . .
H31 H 0.588538 0.443940 0.681089 0.111 Uiso 1 1 calc R U . . .
C32 C 0.5411(11) 0.3478(11) 0.7744(7) 0.117(3) Uani 1 1 d . . . . .
H32 H 0.499343 0.250449 0.762076 0.141 Uiso 1 1 calc R U . . .
C33 C 0.5652(11) 0.4093(10) 0.8413(7) 0.108(3) Uani 1 1 d . . . . .
H33 H 0.543419 0.362651 0.883415 0.129 Uiso 1 1 calc R U . . .
B34 B 0.7968(11) 0.2677(10) 0.5732(5) 0.093(3) Uani 1 1 d D . . . .
F35A F 0.6739(18) 0.220(2) 0.6092(9) 0.098(5) Uiso 0.5 1 d D . P B 1
F36A F 0.7470(17) 0.2106(18) 0.5000(6) 0.113(5) Uiso 0.5 1 d D . P B 1
F37A F 0.8067(18) 0.4207(14) 0.5598(8) 0.130(5) Uiso 0.5 1 d D . P B 1
F38A F 0.9344(16) 0.202(2) 0.5971(8) 0.126(5) Uiso 0.5 1 d D . P B 1
F35B F 0.717(3) 0.184(3) 0.6203(11) 0.102(8) Uiso 0.25 1 d D . P B 2
F36B F 0.9544(18) 0.277(3) 0.6091(10) 0.097(6) Uiso 0.25 1 d D . P B 2
F37B F 0.800(3) 0.206(3) 0.5095(9) 0.091(6) Uiso 0.25 1 d D . P B 2
F38B F 0.748(2) 0.4274(17) 0.5750(10) 0.090(5) Uiso 0.25 1 d D . P B 2
F35C F 0.648(2) 0.232(4) 0.5932(15) 0.115(12) Uiso 0.25 1 d D . P B 3
F36C F 0.895(3) 0.138(3) 0.5874(14) 0.126(9) Uiso 0.25 1 d D . P B 3
F37C F 0.798(3) 0.319(4) 0.5073(10) 0.141(8) Uiso 0.25 1 d D . P B 3
F38C F 0.862(4) 0.386(3) 0.6207(15) 0.172(12) Uiso 0.25 1 d D . P B 3
B39 B 0.7367(12) 0.2802(12) 1.0703(5) 0.108(3) Uani 1 1 d D . . . .
F40A F 0.6547(17) 0.2557(18) 0.9977(6) 0.105(5) Uiso 0.5 1 d D . P C 1
F41A F 0.6822(17) 0.1502(15) 1.1036(6) 0.098(3) Uiso 0.5 1 d D . P C 1
F42A F 0.8860(13) 0.2731(19) 1.0615(7) 0.129(4) Uiso 0.5 1 d D . P C 1
F43A F 0.685(2) 0.4154(17) 1.0961(9) 0.150(6) Uiso 0.5 1 d D . P C 1
F40B F 0.871(3) 0.359(4) 1.1031(15) 0.164(12) Uiso 0.25 1 d D . P C 2
F41B F 0.740(4) 0.290(4) 0.9988(9) 0.151(11) Uiso 0.25 1 d D . P C 2
F42B F 0.733(4) 0.132(2) 1.0948(18) 0.172(18) Uiso 0.25 1 d D . P C 2
F43B F 0.612(3) 0.377(3) 1.0891(13) 0.121(8) Uiso 0.25 1 d D . P C 2
F40C F 0.6590(19) 0.218(2) 1.1233(9) 0.080(4) Uiso 0.25 1 d D . P C 3
F41C F 0.793(3) 0.428(2) 1.0973(11) 0.106(6) Uiso 0.25 1 d D . P C 3
F42C F 0.8890(17) 0.192(2) 1.0729(9) 0.083(4) Uiso 0.25 1 d D . P C 3
F43C F 0.665(3) 0.296(4) 1.0060(9) 0.100(8) Uiso 0.25 1 d D . P C 3


_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 2.063(4) . ?
Fe1 N9 2.149(6) . ?
Fe1 N14 2.132(6) . ?
Fe1 N18 2.066(5) . ?
Fe1 N25 2.155(7) . ?
Fe1 N30 2.139(7) . ?
Ni1 N2 2.063(4) . ?
Ni1 N9 2.149(6) . ?
Ni1 N14 2.132(6) . ?
Ni1 N18 2.066(5) . ?
Ni1 N25 2.155(7) . ?
Ni1 N30 2.139(7) . ?
N2 C3 1.328(8) . ?
N2 C7 1.331(8) . ?
C3 C4 1.381(10) . ?
C3 N8 1.412(9) . ?
C4 H4 0.9300 . ?
C4 C5 1.364(13) . ?
C5 H5 0.9300 . ?
C5 C6 1.379(13) . ?
C6 H6 0.9300 . ?
C6 C7 1.355(10) . ?
C7 N13 1.403(10) . ?
N8 N9 1.366(8) . ?
N8 C12 1.364(9) . ?
N9 C10 1.319(9) . ?
C10 H10 0.9300 . ?
C10 C11 1.390(13) . ?
C11 H11 0.9300 . ?
C11 C12 1.353(14) . ?
C12 H12 0.9300 . ?
N13 N14 1.373(9) . ?
N13 C17 1.356(10) . ?
N14 C15 1.314(10) . ?
C15 H15 0.9300 . ?
C15 C16 1.389(14) . ?
C16 H16 0.9300 . ?
C16 C17 1.347(15) . ?
C17 H17 0.9300 . ?
N18 C19 1.311(9) . ?
N18 C23 1.346(10) . ?
C19 C20 1.381(10) . ?
C19 N24 1.420(9) . ?
C20 H20 0.9300 . ?
C20 C21 1.378(13) . ?
C21 H21 0.9300 . ?
C21 C22 1.373(13) . ?
C22 H22 0.9300 . ?
C22 C23 1.361(10) . ?
C23 N29 1.415(9) . ?
N24 N25 1.364(8) . ?
N24 C28 1.334(10) . ?
N25 C26 1.320(10) . ?
C26 H26 0.9300 . ?
C26 C27 1.407(12) . ?
C27 H27 0.9300 . ?
C27 C28 1.329(13) . ?
C28 H28 0.9300 . ?
N29 N30 1.344(9) . ?
N29 C33 1.359(11) . ?
N30 C31 1.329(10) . ?
C31 H31 0.9300 . ?
C31 C32 1.358(14) . ?
C32 H32 0.9300 . ?
C32 C33 1.372(14) . ?
C33 H33 0.9300 . ?
B34 F35A 1.369(14) . ?
B34 F36A 1.495(14) . ?
B34 F37A 1.343(14) . ?
B34 F38A 1.344(14) . ?
B34 F35B 1.381(16) . ?
B34 F36B 1.449(16) . ?
B34 F37B 1.325(16) . ?
B34 F38B 1.434(16) . ?
B34 F35C 1.396(18) . ?
B34 F36C 1.408(18) . ?
B34 F37C 1.328(17) . ?
B34 F38C 1.437(19) . ?
B39 F40A 1.498(14) . ?
B39 F41A 1.388(13) . ?
B39 F42A 1.304(14) . ?
B39 F43A 1.350(15) . ?
B39 F40B 1.422(19) . ?
B39 F41B 1.362(18) . ?
B39 F42B 1.357(19) . ?
B39 F43B 1.427(18) . ?
B39 F40C 1.371(15) . ?
B39 F41C 1.439(17) . ?
B39 F42C 1.502(16) . ?
B39 F43C 1.319(17) . ?

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 75.4(2) . . ?
N2 Fe1 N14 75.0(2) . . ?
N2 Fe1 N18 176.6(3) . . ?
N2 Fe1 N25 108.8(3) . . ?
N2 Fe1 N30 101.0(3) . . ?
N9 Fe1 N25 95.5(2) . . ?
N14 Fe1 N9 150.4(2) . . ?
N14 Fe1 N25 94.5(2) . . ?
N14 Fe1 N30 91.6(3) . . ?
N18 Fe1 N9 103.7(2) . . ?
N18 Fe1 N14 105.8(2) . . ?
N18 Fe1 N25 74.5(3) . . ?
N18 Fe1 N30 75.7(3) . . ?
N30 Fe1 N9 93.4(2) . . ?
N30 Fe1 N25 150.2(2) . . ?
N2 Ni1 N9 75.4(2) . . ?
N2 Ni1 N14 75.0(2) . . ?
N2 Ni1 N18 176.6(3) . . ?
N2 Ni1 N25 108.8(3) . . ?
N2 Ni1 N30 101.0(3) . . ?
N9 Ni1 N25 95.5(2) . . ?
N14 Ni1 N9 150.4(2) . . ?
N14 Ni1 N25 94.5(2) . . ?
N14 Ni1 N30 91.6(3) . . ?
N18 Ni1 N9 103.7(2) . . ?
N18 Ni1 N14 105.8(2) . . ?
N18 Ni1 N25 74.5(3) . . ?
N18 Ni1 N30 75.7(3) . . ?
N30 Ni1 N9 93.4(2) . . ?
N30 Ni1 N25 150.2(2) . . ?
C3 N2 Fe1 120.5(4) . . ?
C3 N2 Ni1 120.5(4) . . ?
C3 N2 C7 118.5(5) . . ?
C7 N2 Fe1 121.0(4) . . ?
C7 N2 Ni1 121.0(4) . . ?
N2 C3 C4 122.4(7) . . ?
N2 C3 N8 112.7(6) . . ?
C4 C3 N8 124.9(6) . . ?
C3 C4 H4 121.3 . . ?
C5 C4 C3 117.3(7) . . ?
C5 C4 H4 121.3 . . ?
C4 C5 H5 119.4 . . ?
C4 C5 C6 121.2(7) . . ?
C6 C5 H5 119.4 . . ?
C5 C6 H6 121.4 . . ?
C7 C6 C5 117.1(7) . . ?
C7 C6 H6 121.4 . . ?
N2 C7 C6 123.4(7) . . ?
N2 C7 N13 112.2(6) . . ?
C6 C7 N13 124.3(7) . . ?
N9 N8 C3 118.6(5) . . ?
C12 N8 C3 130.7(7) . . ?
C12 N8 N9 110.7(7) . . ?
N8 N9 Fe1 112.8(4) . . ?
N8 N9 Ni1 112.8(4) . . ?
C10 N9 Fe1 142.2(6) . . ?
C10 N9 Ni1 142.2(6) . . ?
C10 N9 N8 105.0(6) . . ?
N9 C10 H10 124.3 . . ?
N9 C10 C11 111.4(8) . . ?
C11 C10 H10 124.3 . . ?
C10 C11 H11 127.0 . . ?
C12 C11 C10 106.0(7) . . ?
C12 C11 H11 127.0 . . ?
N8 C12 H12 126.6 . . ?
C11 C12 N8 106.8(8) . . ?
C11 C12 H12 126.6 . . ?
N14 N13 C7 118.1(5) . . ?
C17 N13 C7 130.7(8) . . ?
C17 N13 N14 111.2(7) . . ?
N13 N14 Fe1 113.6(4) . . ?
N13 N14 Ni1 113.6(4) . . ?
C15 N14 Fe1 140.7(6) . . ?
C15 N14 Ni1 140.7(6) . . ?
C15 N14 N13 105.0(7) . . ?
N14 C15 H15 124.7 . . ?
N14 C15 C16 110.5(9) . . ?
C16 C15 H15 124.7 . . ?
C15 C16 H16 126.4 . . ?
C17 C16 C15 107.3(8) . . ?
C17 C16 H16 126.4 . . ?
N13 C17 H17 127.0 . . ?
C16 C17 N13 105.9(9) . . ?
C16 C17 H17 127.0 . . ?
C19 N18 Fe1 121.9(5) . . ?
C19 N18 Ni1 121.9(5) . . ?
C19 N18 C23 118.6(6) . . ?
C23 N18 Fe1 119.5(5) . . ?
C23 N18 Ni1 119.5(5) . . ?
N18 C19 C20 124.2(7) . . ?
N18 C19 N24 112.2(6) . . ?
C20 C19 N24 123.6(7) . . ?
C19 C20 H20 122.1 . . ?
C21 C20 C19 115.8(8) . . ?
C21 C20 H20 122.1 . . ?
C20 C21 H21 119.4 . . ?
C22 C21 C20 121.3(8) . . ?
C22 C21 H21 119.4 . . ?
C21 C22 H22 120.9 . . ?
C23 C22 C21 118.2(8) . . ?
C23 C22 H22 120.9 . . ?
N18 C23 C22 121.9(7) . . ?
N18 C23 N29 112.4(6) . . ?
C22 C23 N29 125.7(7) . . ?
N25 N24 C19 118.1(6) . . ?
C28 N24 C19 131.5(7) . . ?
C28 N24 N25 110.4(7) . . ?
N24 N25 Fe1 113.3(4) . . ?
N24 N25 Ni1 113.3(4) . . ?
C26 N25 Fe1 141.5(6) . . ?
C26 N25 Ni1 141.5(6) . . ?
C26 N25 N24 105.0(7) . . ?
N25 C26 H26 124.7 . . ?
N25 C26 C27 110.6(8) . . ?
C27 C26 H26 124.7 . . ?
C26 C27 H27 127.5 . . ?
C28 C27 C26 105.0(8) . . ?
C28 C27 H27 127.5 . . ?
N24 C28 H28 125.5 . . ?
C27 C28 N24 109.0(8) . . ?
C27 C28 H28 125.5 . . ?
N30 N29 C23 119.0(6) . . ?
N30 N29 C33 111.8(8) . . ?
C33 N29 C23 129.2(8) . . ?
N29 N30 Fe1 113.4(5) . . ?
N29 N30 Ni1 113.4(5) . . ?
C31 N30 Fe1 141.9(7) . . ?
C31 N30 Ni1 141.9(7) . . ?
C31 N30 N29 104.8(7) . . ?
N30 C31 H31 124.2 . . ?
N30 C31 C32 111.5(9) . . ?
C32 C31 H31 124.2 . . ?
C31 C32 H32 126.7 . . ?
C31 C32 C33 106.6(8) . . ?
C33 C32 H32 126.7 . . ?
N29 C33 C32 105.3(9) . . ?
N29 C33 H33 127.4 . . ?
C32 C33 H33 127.4 . . ?
F35A B34 F36A 101.9(11) . . ?
F37A B34 F35A 116.8(12) . . ?
F37A B34 F36A 99.4(10) . . ?
F37A B34 F38A 114.1(13) . . ?
F38A B34 F35A 113.2(12) . . ?
F38A B34 F36A 109.5(11) . . ?
F35B B34 F36B 102.8(13) . . ?
F35B B34 F38B 108.5(13) . . ?
F37B B34 F35B 116.2(14) . . ?
F37B B34 F36B 110.4(13) . . ?
F37B B34 F38B 116.0(13) . . ?
F38B B34 F36B 101.2(12) . . ?
F35C B34 F36C 108.5(15) . . ?
F35C B34 F38C 107.0(16) . . ?
F36C B34 F38C 104.8(15) . . ?
F37C B34 F35C 114.9(15) . . ?
F37C B34 F36C 112.6(15) . . ?
F37C B34 F38C 108.4(16) . . ?
F41A B39 F40A 99.2(10) . . ?
F42A B39 F40A 104.5(10) . . ?
F42A B39 F41A 113.4(11) . . ?
F42A B39 F43A 116.4(13) . . ?
F43A B39 F40A 108.4(12) . . ?
F43A B39 F41A 113.0(11) . . ?
F40B B39 F43B 101.7(15) . . ?
F41B B39 F40B 108.3(16) . . ?
F41B B39 F43B 107.6(15) . . ?
F42B B39 F40B 110.0(17) . . ?
F42B B39 F41B 113.8(18) . . ?
F42B B39 F43B 114.6(17) . . ?
F40C B39 F41C 104.8(13) . . ?
F40C B39 F42C 105.0(11) . . ?
F41C B39 F42C 100.1(13) . . ?
F43C B39 F40C 120.4(15) . . ?
F43C B39 F41C 110.4(16) . . ?
F43C B39 F42C 113.9(14) . . ?

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(6) . . . . ?
Fe1 N2 C3 N8 -1.3(9) . . . . ?
Fe1 N2 C7 C6 -179.5(6) . . . . ?
Fe1 N2 C7 N13 2.2(8) . . . . ?
Fe1 N9 C10 C11 178.9(7) . . . . ?
Fe1 N14 C15 C16 171.3(7) . . . . ?
Fe1 N18 C19 C20 179.5(5) . . . . ?
Fe1 N18 C19 N24 -2.2(7) . . . . ?
Fe1 N18 C23 C22 -179.4(5) . . . . ?
Fe1 N18 C23 N29 0.5(7) . . . . ?
Fe1 N25 C26 C27 -173.3(6) . . . . ?
Fe1 N30 C31 C32 -177.6(6) . . . . ?
Ni1 N2 C3 C4 179.2(6) . . . . ?
Ni1 N2 C3 N8 -1.3(9) . . . . ?
Ni1 N2 C7 C6 -179.5(6) . . . . ?
Ni1 N2 C7 N13 2.2(8) . . . . ?
Ni1 N9 C10 C11 178.9(7) . . . . ?
Ni1 N14 C15 C16 171.3(7) . . . . ?
Ni1 N18 C19 C20 179.5(5) . . . . ?
Ni1 N18 C19 N24 -2.2(7) . . . . ?
Ni1 N18 C23 C22 -179.4(5) . . . . ?
Ni1 N18 C23 N29 0.5(7) . . . . ?
Ni1 N25 C26 C27 -173.3(6) . . . . ?
Ni1 N30 C31 C32 -177.6(6) . . . . ?
N2 C3 C4 C5 0.0(12) . . . . ?
N2 C3 N8 N9 0.4(9) . . . . ?
N2 C3 N8 C12 179.5(8) . . . . ?
N2 C7 N13 N14 -4.4(9) . . . . ?
N2 C7 N13 C17 172.3(8) . . . . ?
C3 N2 C7 C6 -0.1(11) . . . . ?
C3 N2 C7 N13 -178.4(7) . . . . ?
C3 C4 C5 C6 0.6(15) . . . . ?
C3 N8 N9 Fe1 0.6(7) . . . . ?
C3 N8 N9 Ni1 0.6(7) . . . . ?
C3 N8 N9 C10 -179.2(6) . . . . ?
C3 N8 C12 C11 179.8(7) . . . . ?
C4 C3 N8 N9 179.9(7) . . . . ?
C4 C3 N8 C12 -1.0(12) . . . . ?
C4 C5 C6 C7 -0.9(15) . . . . ?
C5 C6 C7 N2 0.7(12) . . . . ?
C5 C6 C7 N13 178.7(8) . . . . ?
C6 C7 N13 N14 177.4(7) . . . . ?
C6 C7 N13 C17 -6.0(12) . . . . ?
C7 N2 C3 C4 -0.2(11) . . . . ?
C7 N2 C3 N8 179.3(6) . . . . ?
C7 N13 N14 Fe1 4.5(8) . . . . ?
C7 N13 N14 Ni1 4.5(8) . . . . ?
C7 N13 N14 C15 177.1(6) . . . . ?
C7 N13 C17 C16 -178.6(8) . . . . ?
N8 C3 C4 C5 -179.5(8) . . . . ?
N8 N9 C10 C11 -1.4(9) . . . . ?
N9 N8 C12 C11 -1.1(9) . . . . ?
N9 C10 C11 C12 0.8(11) . . . . ?
C10 C11 C12 N8 0.2(10) . . . . ?
C12 N8 N9 Fe1 -178.7(5) . . . . ?
C12 N8 N9 Ni1 -178.7(5) . . . . ?
C12 N8 N9 C10 1.5(8) . . . . ?
N13 N14 C15 C16 2.0(10) . . . . ?
N14 N13 C17 C16 -1.8(10) . . . . ?
N14 C15 C16 C17 -3.2(12) . . . . ?
C15 C16 C17 N13 2.9(12) . . . . ?
C17 N13 N14 Fe1 -172.8(6) . . . . ?
C17 N13 N14 Ni1 -172.8(6) . . . . ?
C17 N13 N14 C15 -0.2(9) . . . . ?
N18 C19 C20 C21 -0.7(11) . . . . ?
N18 C19 N24 N25 2.3(8) . . . . ?
N18 C19 N24 C28 -173.8(7) . . . . ?
N18 C23 N29 N30 1.9(8) . . . . ?
N18 C23 N29 C33 -179.4(7) . . . . ?
C19 N18 C23 C22 -0.1(9) . . . . ?
C19 N18 C23 N29 179.8(5) . . . . ?
C19 C20 C21 C22 1.2(13) . . . . ?
C19 N24 N25 Fe1 -1.4(7) . . . . ?
C19 N24 N25 Ni1 -1.4(7) . . . . ?
C19 N24 N25 C26 -177.2(6) . . . . ?
C19 N24 C28 C27 176.4(7) . . . . ?
C20 C19 N24 N25 -179.4(6) . . . . ?
C20 C19 N24 C28 4.5(11) . . . . ?
C20 C21 C22 C23 -1.2(13) . . . . ?
C21 C22 C23 N18 0.6(11) . . . . ?
C21 C22 C23 N29 -179.3(7) . . . . ?
C22 C23 N29 N30 -178.3(6) . . . . ?
C22 C23 N29 C33 0.5(12) . . . . ?
C23 N18 C19 C20 0.2(10) . . . . ?
C23 N18 C19 N24 178.5(5) . . . . ?
C23 N29 N30 Fe1 -3.1(7) . . . . ?
C23 N29 N30 Ni1 -3.1(7) . . . . ?
C23 N29 N30 C31 177.3(6) . . . . ?
C23 N29 C33 C32 -177.9(7) . . . . ?
N24 C19 C20 C21 -178.9(7) . . . . ?
N24 N25 C26 C27 0.4(8) . . . . ?
N25 N24 C28 C27 0.1(9) . . . . ?
N25 C26 C27 C28 -0.4(10) . . . . ?
C26 C27 C28 N24 0.2(10) . . . . ?
C28 N24 N25 Fe1 175.4(5) . . . . ?
C28 N24 N25 Ni1 175.4(5) . . . . ?
C28 N24 N25 C26 -0.3(8) . . . . ?
N29 N30 C31 C32 1.7(9) . . . . ?
N30 N29 C33 C32 1.0(9) . . . . ?
N30 C31 C32 C33 -1.2(10) . . . . ?
C31 C32 C33 N29 0.1(10) . . . . ?
C33 N29 N30 Fe1 177.9(5) . . . . ?
C33 N29 N30 Ni1 177.9(5) . . . . ?
C33 N29 N30 C31 -1.7(8) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.98(3)
2 0.02(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_mh202mt
_database_code_depnum_ccdc_archive 'CCDC 2261794'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2023-08-21 deposited with the CCDC.	2023-08-30 downloaded from the CCDC.
;
_audit_creation_date             2023-03-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis[2,6-di(pyrazol-1-yl)pyridine]iron(II) bis[2,6-di(pyrazol-1-yl)pyridine]-nickel(II) ditetrafluoroborate 0.46:0.54 solid solution'
_chemical_formula_moiety         
'0.46(C22 H18 Fe N10), 0.54(C22 H18 N10 Ni), 2(B F4)'
_chemical_formula_sum            'C22 H18 B2 F8 Fe0.46 N10 Ni0.54'
_chemical_formula_weight         653.48
_chemical_absolute_configuration ab
_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 0.0019 0.0015 '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 0.0004 0.0006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0124 0.0097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.2961 0.8007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0037 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.2866 1.0558 '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           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   8.4832(1)
_cell_length_b                   8.5546(1)
_cell_length_c                   18.5399(1)
_cell_angle_alpha                90
_cell_angle_beta                 97.609(1)
_cell_angle_gamma                90
_cell_volume                     1333.60(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    16157
_cell_measurement_temperature    200.15
_cell_measurement_theta_max      35.24
_cell_measurement_theta_min      1.07
_exptl_absorpt_coefficient_mu    0.687
_exptl_absorpt_correction_T_min  0.944
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
DIALS 3.12.1-2-g1c07bc2b3-release
Scaling & analysis of unmerged intensities, absorption correction using 
spherical harmonics
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       lath
_exptl_crystal_F_000             658
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            30659
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        24.620
_diffrn_reflns_theta_max         36.108
_diffrn_reflns_theta_min         1.074
_diffrn_ambient_temperature      200.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.933
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_measurement_device       'Fixed χ 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_reflns_Friedel_coverage         0.815
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.842
_reflns_number_gt                10200
_reflns_number_total             12471
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'XIA2 0.4.0.438-g4431aaa (Winter, 2010)'
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction        'XIA2 0.4.0.438-g4431aaa (Winter, 2010)'
_computing_molecular_graphics    'XSEED (Barbour, 2020)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.018(13)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         12471
_refine_ls_number_restraints     55
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0482
_refine_ls_restrained_S_all      1.052
_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)+(0.0226P)²+0.5032P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.1027
_refine_special_details          
;In this refinement, the low temperature dataset was treated as a single, 
 averaged [FeₓNi₁₋ₓ(bpp)₂]2+ cation site. Partial Fe and Ni atoms
 were refined with the same cartesian coordinates, using the Fe~0.46~/
 Ni~0.54~ occupancy ratio obtained from the disordered refinement model 
 from this dataset. One BF₄⁻ ion is disordered by rotation about a 
 B---F bond, over two orientations with occupancies of 0.67:0.33. This
 was treated with the distance restraints listed below. An EADP thermal 
 parameter constraint between the two partial metal atoms was required 
 to make the model converge.

 All non-H atoms were refined anisotropically, with ISOR restraints applied 
 to the disordered F atoms. H atoms were placed in calculated positions and 
 refined using a riding model. A minor inversion twin domain was included 
 in the refinement, to account for the slightly high Flack parameter in the 
 100 K refinements.,Twin
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.982(13)
 0.018(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 B39-F40
 1.38157 with sigma of 0.02
 B39-F41A
 1.38157 with sigma of 0.02
 B39-F42A
 1.38157 with sigma of 0.02
 B39-F43A
 1.38157 with sigma of 0.02
 B39-F41B
 1.38157 with sigma of 0.02
 B39-F42B
 1.38157 with sigma of 0.02
 B39-F43B
 1.38157 with sigma of 0.02
 F40-F41A
 2.256104 with sigma of 0.02
 F40-F42A
 2.256104 with sigma of 0.02
 F40-F43A
 2.256104 with sigma of 0.02
 F41A-F42A
 2.256104 with sigma of 0.02
 F41A-F43A
 2.256104 with sigma of 0.02
 F42A-F43A
 2.256104 with sigma of 0.02
 F40-F41B
 2.256104 with sigma of 0.02
 F40-F42B
 2.256104 with sigma of 0.02
 F40-F43B
 2.256104 with sigma of 0.02
 F41B-F42B
 2.256104 with sigma of 0.02
 F41B-F43B
 2.256104 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(F41A) \\sim Ueq, Uanis(F42A) \\sim Ueq, Uanis(F43A) \\sim Ueq,
Uanis(F41B) \\sim Ueq, Uanis(F42B) \\sim Ueq, Uanis(F43B) \\sim Ueq: with sigma
of 0.002 and sigma for terminal atoms of 0.004
Uanis(Fe1) = Uanis(Ni1)
5. Others
 1(DFIX)=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(DFIX)=1(DFIX)=1(DFIX)=
 1(DFIX)=1(DFIX)=1.633*FVAR(2)
 X(Fe1)=X(Ni1)=FVAR(2)
 Y(Fe1)=Y(Ni1)=FVAR(3)
 Z(Fe1)=Z(Ni1)=FVAR(4)
 Fixed Sof: Fe1(0.46) Ni1(0.54) F41A(0.5) F42A(0.5) F43A(0.5) F41B(0.5)
 F42B(0.5) F43B(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16),
 C17(H17), C20(H20), C21(H21), C22(H22), C26(H26), C27(H27), C28(H28), C31(H31),
  C32(H32), C33(H33)
;
_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 0.71932(4) 0.82293(4) 0.74659(2) 0.02609(7) Uani 0.46 1 d . . P A 1
Ni1 Ni 0.71932(4) 0.82293(4) 0.74659(2) 0.02609(7) Uani 0.54 1 d . . P A 2
N2 N 0.7128(2) 0.8389(3) 0.64108(11) 0.0283(4) Uani 1 1 d . . . . .
C3 C 0.5854(3) 0.8978(3) 0.60013(14) 0.0296(5) Uani 1 1 d . . . . .
C4 C 0.5747(4) 0.9108(4) 0.52540(16) 0.0379(6) Uani 1 1 d . . . . .
H4 H 0.484927 0.951951 0.497598 0.045 Uiso 1 1 calc R U . . .
C5 C 0.7054(4) 0.8591(4) 0.49394(16) 0.0410(7) Uani 1 1 d . . . . .
H5 H 0.703058 0.866538 0.443771 0.049 Uiso 1 1 calc R U . . .
C6 C 0.8380(4) 0.7972(4) 0.53478(15) 0.0381(6) Uani 1 1 d . . . . .
H6 H 0.924843 0.762848 0.513343 0.046 Uiso 1 1 calc R U . . .
C7 C 0.8362(3) 0.7883(3) 0.60926(14) 0.0306(5) Uani 1 1 d . . . . .
N8 N 0.4677(3) 0.9415(3) 0.64271(13) 0.0319(4) Uani 1 1 d . . . . .
N9 N 0.4982(3) 0.9175(3) 0.71634(13) 0.0318(4) Uani 1 1 d . . . . .
C10 C 0.3682(4) 0.9655(4) 0.74257(19) 0.0393(6) Uani 1 1 d . . . . .
H10 H 0.354340 0.962651 0.791472 0.047 Uiso 1 1 calc R U . . .
C11 C 0.2548(4) 1.0211(4) 0.6866(2) 0.0464(8) Uani 1 1 d . . . . .
H11 H 0.154891 1.061334 0.691305 0.056 Uiso 1 1 calc R U . . .
C12 C 0.3204(4) 1.0043(4) 0.6240(2) 0.0412(7) Uani 1 1 d . . . . .
H12 H 0.273686 1.030722 0.577356 0.049 Uiso 1 1 calc R U . . .
N13 N 0.9558(3) 0.7259(3) 0.65997(13) 0.0329(5) Uani 1 1 d . . . . .
N14 N 0.9345(3) 0.7331(3) 0.73209(13) 0.0342(5) Uani 1 1 d . . . . .
C15 C 1.0600(4) 0.6635(4) 0.7680(2) 0.0434(7) Uani 1 1 d . . . . .
H15 H 1.078260 0.651812 0.818295 0.052 Uiso 1 1 calc R U . . .
C16 C 1.1618(4) 0.6096(4) 0.7197(2) 0.0535(9) Uani 1 1 d . . . . .
H16 H 1.257377 0.556387 0.731542 0.064 Uiso 1 1 calc R U . . .
C17 C 1.0931(4) 0.6505(4) 0.6523(2) 0.0458(8) Uani 1 1 d . . . . .
H17 H 1.132736 0.630654 0.608760 0.055 Uiso 1 1 calc R U . . .
N18 N 0.7231(3) 0.7976(3) 0.85183(11) 0.0290(5) Uani 1 1 d . . . . .
C19 C 0.7803(3) 0.9099(3) 0.89748(14) 0.0306(5) Uani 1 1 d . . . . .
C20 C 0.7852(4) 0.8976(4) 0.97201(15) 0.0374(6) Uani 1 1 d . . . . .
H20 H 0.824260 0.977946 1.003130 0.045 Uiso 1 1 calc R U . . .
C21 C 0.7289(4) 0.7589(4) 0.99811(17) 0.0403(7) Uani 1 1 d . . . . .
H21 H 0.729961 0.746186 1.047995 0.048 Uiso 1 1 calc R U . . .
C22 C 0.6713(4) 0.6395(4) 0.95184(16) 0.0383(6) Uani 1 1 d . . . . .
H22 H 0.634640 0.546390 0.969439 0.046 Uiso 1 1 calc R U . . .
C23 C 0.6706(3) 0.6648(3) 0.87815(15) 0.0313(5) Uani 1 1 d . . . . .
N24 N 0.8340(3) 1.0385(3) 0.86027(13) 0.0326(5) Uani 1 1 d . . . . .
N25 N 0.8180(3) 1.0304(3) 0.78550(13) 0.0328(5) Uani 1 1 d . . . . .
C26 C 0.8852(4) 1.1606(4) 0.76512(19) 0.0415(7) Uani 1 1 d . . . . .
H26 H 0.891557 1.187982 0.717042 0.050 Uiso 1 1 calc R U . . .
C27 C 0.9451(4) 1.2512(4) 0.8253(2) 0.0479(8) Uani 1 1 d . . . . .
H27 H 0.997396 1.346650 0.824974 0.057 Uiso 1 1 calc R U . . .
C28 C 0.9108(4) 1.1699(4) 0.88500(19) 0.0423(7) Uani 1 1 d . . . . .
H28 H 0.935755 1.199726 0.933405 0.051 Uiso 1 1 calc R U . . .
N29 N 0.6166(3) 0.5588(3) 0.82258(14) 0.0329(5) Uani 1 1 d . . . . .
N30 N 0.6298(3) 0.6029(3) 0.75245(13) 0.0329(5) Uani 1 1 d . . . . .
C31 C 0.5812(4) 0.4806(4) 0.71169(19) 0.0409(7) Uani 1 1 d . . . . .
H31 H 0.578012 0.476578 0.661396 0.049 Uiso 1 1 calc R U . . .
C32 C 0.5354(4) 0.3588(4) 0.7543(2) 0.0490(8) Uani 1 1 d . . . . .
H32 H 0.496555 0.261472 0.738157 0.059 Uiso 1 1 calc R U . . .
C33 C 0.5592(4) 0.4109(4) 0.8244(2) 0.0442(7) Uani 1 1 d . . . . .
H33 H 0.539766 0.355709 0.865580 0.053 Uiso 1 1 calc R U . . .
B34 B 0.7979(5) 0.2827(4) 0.5648(2) 0.0425(8) Uani 1 1 d . . . . .
F35 F 0.6776(3) 0.2319(3) 0.60296(11) 0.0530(5) Uani 1 1 d . . . . .
F36 F 0.7667(3) 0.2311(3) 0.49261(12) 0.0615(6) Uani 1 1 d . . . . .
F37 F 0.7964(3) 0.4440(3) 0.56364(14) 0.0676(7) Uani 1 1 d . . . . .
F38 F 0.9413(3) 0.2259(4) 0.59576(14) 0.0882(10) Uani 1 1 d . . . . .
B39 B 0.7238(5) 0.2690(5) 1.0594(2) 0.0481(9) Uani 1 1 d D . . . .
F40 F 0.8850(3) 0.2605(4) 1.05834(13) 0.0863(11) Uani 1 1 d D . . . .
F41A F 0.649(2) 0.2747(16) 0.9907(6) 0.054(3) Uani 0.5 1 d D U P B 1
F42A F 0.6742(12) 0.1662(9) 1.1060(5) 0.059(2) Uani 0.5 1 d D U P B 1
F43A F 0.7234(10) 0.4184(9) 1.0931(4) 0.084(2) Uani 0.5 1 d D U P B 1
F41B F 0.6467(17) 0.2446(16) 0.9865(6) 0.0438(19) Uani 0.5 1 d D U P B 2
F42B F 0.6871(12) 0.1251(8) 1.0946(5) 0.0414(14) Uani 0.5 1 d D U P B 2
F43B F 0.6475(7) 0.3931(7) 1.0872(3) 0.0530(13) Uani 0.5 1 d D U 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
Fe1 N2 1.954(2) . ?
Fe1 N9 2.052(2) . ?
Fe1 N14 2.031(3) . ?
Fe1 N18 1.959(2) . ?
Fe1 N25 2.052(3) . ?
Fe1 N30 2.038(3) . ?
Ni1 N2 1.954(2) . ?
Ni1 N9 2.052(2) . ?
Ni1 N14 2.031(3) . ?
Ni1 N18 1.959(2) . ?
Ni1 N25 2.052(3) . ?
Ni1 N30 2.038(3) . ?
N2 C3 1.335(3) . ?
N2 C7 1.339(3) . ?
C3 C4 1.381(4) . ?
C3 N8 1.403(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.392(5) . ?
C5 H5 0.9300 . ?
C5 C6 1.376(5) . ?
C6 H6 0.9300 . ?
C6 C7 1.385(4) . ?
C7 N13 1.395(4) . ?
N8 N9 1.371(3) . ?
N8 C12 1.362(4) . ?
N9 C10 1.328(4) . ?
C10 H10 0.9300 . ?
C10 C11 1.402(5) . ?
C11 H11 0.9300 . ?
C11 C12 1.359(5) . ?
C12 H12 0.9300 . ?
N13 N14 1.374(3) . ?
N13 C17 1.355(4) . ?
N14 C15 1.320(4) . ?
C15 H15 0.9300 . ?
C15 C16 1.403(5) . ?
C16 H16 0.9300 . ?
C16 C17 1.353(5) . ?
C17 H17 0.9300 . ?
N18 C19 1.328(4) . ?
N18 C23 1.336(4) . ?
C19 C20 1.381(4) . ?
C19 N24 1.406(4) . ?
C20 H20 0.9300 . ?
C20 C21 1.390(5) . ?
C21 H21 0.9300 . ?
C21 C22 1.381(5) . ?
C22 H22 0.9300 . ?
C22 C23 1.382(4) . ?
C23 N29 1.403(4) . ?
N24 N25 1.377(3) . ?
N24 C28 1.349(4) . ?
N25 C26 1.329(4) . ?
C26 H26 0.9300 . ?
C26 C27 1.398(5) . ?
C27 H27 0.9300 . ?
C27 C28 1.370(5) . ?
C28 H28 0.9300 . ?
N29 N30 1.372(3) . ?
N29 C33 1.358(4) . ?
N30 C31 1.324(4) . ?
C31 H31 0.9300 . ?
C31 C32 1.394(5) . ?
C32 H32 0.9300 . ?
C32 C33 1.364(5) . ?
C33 H33 0.9300 . ?
B34 F35 1.386(4) . ?
B34 F36 1.401(4) . ?
B34 F37 1.380(5) . ?
B34 F38 1.364(5) . ?
B39 F40 1.373(5) . ?
B39 F41A 1.345(11) . ?
B39 F42A 1.338(9) . ?
B39 F43A 1.423(8) . ?
B39 F41B 1.437(11) . ?
B39 F42B 1.446(9) . ?
B39 F43B 1.378(7) . ?

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 78.18(9) . . ?
N2 Fe1 N14 78.51(10) . . ?
N2 Fe1 N18 177.57(11) . . ?
N2 Fe1 N25 104.33(10) . . ?
N2 Fe1 N30 99.01(10) . . ?
N9 Fe1 N25 94.07(10) . . ?
N14 Fe1 N9 156.68(9) . . ?
N14 Fe1 N25 92.39(10) . . ?
N14 Fe1 N30 90.31(10) . . ?
N18 Fe1 N9 102.09(9) . . ?
N18 Fe1 N14 101.16(9) . . ?
N18 Fe1 N25 78.07(10) . . ?
N18 Fe1 N30 78.58(10) . . ?
N30 Fe1 N9 92.57(10) . . ?
N30 Fe1 N25 156.58(9) . . ?
N2 Ni1 N9 78.18(9) . . ?
N2 Ni1 N14 78.51(10) . . ?
N2 Ni1 N18 177.57(11) . . ?
N2 Ni1 N25 104.33(10) . . ?
N2 Ni1 N30 99.01(10) . . ?
N9 Ni1 N25 94.07(10) . . ?
N14 Ni1 N9 156.68(9) . . ?
N14 Ni1 N25 92.39(10) . . ?
N14 Ni1 N30 90.31(10) . . ?
N18 Ni1 N9 102.09(9) . . ?
N18 Ni1 N14 101.16(9) . . ?
N18 Ni1 N25 78.07(10) . . ?
N18 Ni1 N30 78.58(10) . . ?
N30 Ni1 N9 92.57(10) . . ?
N30 Ni1 N25 156.58(9) . . ?
C3 N2 Fe1 120.61(17) . . ?
C3 N2 Ni1 120.61(17) . . ?
C3 N2 C7 119.5(2) . . ?
C7 N2 Fe1 119.88(18) . . ?
C7 N2 Ni1 119.88(18) . . ?
N2 C3 C4 122.8(3) . . ?
N2 C3 N8 111.3(2) . . ?
C4 C3 N8 125.9(3) . . ?
C3 C4 H4 121.8 . . ?
C3 C4 C5 116.4(3) . . ?
C5 C4 H4 121.8 . . ?
C4 C5 H5 119.0 . . ?
C6 C5 C4 122.0(3) . . ?
C6 C5 H5 119.0 . . ?
C5 C6 H6 121.5 . . ?
C5 C6 C7 117.0(3) . . ?
C7 C6 H6 121.5 . . ?
N2 C7 C6 122.3(3) . . ?
N2 C7 N13 111.6(2) . . ?
C6 C7 N13 126.1(3) . . ?
N9 N8 C3 117.8(2) . . ?
C12 N8 C3 131.2(3) . . ?
C12 N8 N9 111.0(2) . . ?
N8 N9 Fe1 112.12(16) . . ?
N8 N9 Ni1 112.12(16) . . ?
C10 N9 Fe1 142.7(2) . . ?
C10 N9 Ni1 142.7(2) . . ?
C10 N9 N8 105.2(3) . . ?
N9 C10 H10 124.6 . . ?
N9 C10 C11 110.8(3) . . ?
C11 C10 H10 124.6 . . ?
C10 C11 H11 126.9 . . ?
C12 C11 C10 106.2(3) . . ?
C12 C11 H11 126.9 . . ?
N8 C12 H12 126.6 . . ?
C11 C12 N8 106.8(3) . . ?
C11 C12 H12 126.6 . . ?
N14 N13 C7 117.4(2) . . ?
C17 N13 C7 132.1(3) . . ?
C17 N13 N14 110.4(3) . . ?
N13 N14 Fe1 112.47(17) . . ?
N13 N14 Ni1 112.47(17) . . ?
C15 N14 Fe1 141.5(2) . . ?
C15 N14 Ni1 141.5(2) . . ?
C15 N14 N13 105.6(3) . . ?
N14 C15 H15 124.8 . . ?
N14 C15 C16 110.5(3) . . ?
C16 C15 H15 124.8 . . ?
C15 C16 H16 126.9 . . ?
C17 C16 C15 106.1(3) . . ?
C17 C16 H16 126.9 . . ?
N13 C17 H17 126.3 . . ?
C16 C17 N13 107.3(3) . . ?
C16 C17 H17 126.3 . . ?
C19 N18 Fe1 120.74(18) . . ?
C19 N18 Ni1 120.74(18) . . ?
C19 N18 C23 119.6(2) . . ?
C23 N18 Fe1 119.69(19) . . ?
C23 N18 Ni1 119.69(19) . . ?
N18 C19 C20 122.9(3) . . ?
N18 C19 N24 111.6(2) . . ?
C20 C19 N24 125.6(3) . . ?
C19 C20 H20 121.7 . . ?
C19 C20 C21 116.6(3) . . ?
C21 C20 H20 121.7 . . ?
C20 C21 H21 119.2 . . ?
C22 C21 C20 121.6(3) . . ?
C22 C21 H21 119.2 . . ?
C21 C22 H22 121.5 . . ?
C21 C22 C23 117.0(3) . . ?
C23 C22 H22 121.5 . . ?
N18 C23 C22 122.4(3) . . ?
N18 C23 N29 111.9(2) . . ?
C22 C23 N29 125.7(3) . . ?
N25 N24 C19 117.4(2) . . ?
C28 N24 C19 131.2(3) . . ?
C28 N24 N25 111.3(2) . . ?
N24 N25 Fe1 112.24(17) . . ?
N24 N25 Ni1 112.24(17) . . ?
C26 N25 Fe1 142.7(2) . . ?
C26 N25 Ni1 142.7(2) . . ?
C26 N25 N24 104.8(3) . . ?
N25 C26 H26 124.4 . . ?
N25 C26 C27 111.2(3) . . ?
C27 C26 H26 124.4 . . ?
C26 C27 H27 127.2 . . ?
C28 C27 C26 105.7(3) . . ?
C28 C27 H27 127.2 . . ?
N24 C28 C27 107.0(3) . . ?
N24 C28 H28 126.5 . . ?
C27 C28 H28 126.5 . . ?
N30 N29 C23 117.3(2) . . ?
C33 N29 C23 131.8(3) . . ?
C33 N29 N30 110.8(3) . . ?
N29 N30 Fe1 112.45(18) . . ?
N29 N30 Ni1 112.45(18) . . ?
C31 N30 Fe1 142.1(2) . . ?
C31 N30 Ni1 142.1(2) . . ?
C31 N30 N29 105.4(3) . . ?
N30 C31 H31 124.6 . . ?
N30 C31 C32 110.9(3) . . ?
C32 C31 H31 124.6 . . ?
C31 C32 H32 126.9 . . ?
C33 C32 C31 106.2(3) . . ?
C33 C32 H32 126.9 . . ?
N29 C33 C32 106.8(3) . . ?
N29 C33 H33 126.6 . . ?
C32 C33 H33 126.6 . . ?
F35 B34 F36 109.3(3) . . ?
F37 B34 F35 108.4(3) . . ?
F37 B34 F36 107.5(3) . . ?
F38 B34 F35 110.4(3) . . ?
F38 B34 F36 109.6(3) . . ?
F38 B34 F37 111.6(4) . . ?
F40 B39 F43A 96.6(5) . . ?
F40 B39 F41B 108.0(7) . . ?
F40 B39 F42B 103.6(5) . . ?
F40 B39 F43B 124.4(4) . . ?
F41A B39 F40 109.3(8) . . ?
F41A B39 F43A 110.8(7) . . ?
F42A B39 F40 111.9(6) . . ?
F42A B39 F41A 119.1(9) . . ?
F42A B39 F43A 106.8(5) . . ?
F41B B39 F42B 101.7(7) . . ?
F43B B39 F41B 106.6(7) . . ?
F43B B39 F42B 110.4(5) . . ?

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 -179.6(2) . . . . ?
Fe1 N2 C3 N8 -0.3(3) . . . . ?
Fe1 N2 C7 C6 -179.8(2) . . . . ?
Fe1 N2 C7 N13 1.1(3) . . . . ?
Fe1 N9 C10 C11 179.9(3) . . . . ?
Fe1 N14 C15 C16 170.8(3) . . . . ?
Fe1 N18 C19 C20 179.9(2) . . . . ?
Fe1 N18 C19 N24 -0.3(3) . . . . ?
Fe1 N18 C23 C22 179.5(2) . . . . ?
Fe1 N18 C23 N29 -0.5(3) . . . . ?
Fe1 N25 C26 C27 -172.8(3) . . . . ?
Fe1 N30 C31 C32 178.3(2) . . . . ?
Ni1 N2 C3 C4 -179.6(2) . . . . ?
Ni1 N2 C3 N8 -0.3(3) . . . . ?
Ni1 N2 C7 C6 -179.8(2) . . . . ?
Ni1 N2 C7 N13 1.1(3) . . . . ?
Ni1 N9 C10 C11 179.9(3) . . . . ?
Ni1 N14 C15 C16 170.8(3) . . . . ?
Ni1 N18 C19 C20 179.9(2) . . . . ?
Ni1 N18 C19 N24 -0.3(3) . . . . ?
Ni1 N18 C23 C22 179.5(2) . . . . ?
Ni1 N18 C23 N29 -0.5(3) . . . . ?
Ni1 N25 C26 C27 -172.8(3) . . . . ?
Ni1 N30 C31 C32 178.3(2) . . . . ?
N2 C3 C4 C5 -0.2(4) . . . . ?
N2 C3 N8 N9 -0.5(3) . . . . ?
N2 C3 N8 C12 -179.4(3) . . . . ?
N2 C7 N13 N14 -3.4(3) . . . . ?
N2 C7 N13 C17 173.6(3) . . . . ?
C3 N2 C7 C6 1.1(4) . . . . ?
C3 N2 C7 N13 -178.0(2) . . . . ?
C3 C4 C5 C6 0.5(5) . . . . ?
C3 N8 N9 Fe1 0.9(3) . . . . ?
C3 N8 N9 Ni1 0.9(3) . . . . ?
C3 N8 N9 C10 -178.9(2) . . . . ?
C3 N8 C12 C11 178.9(3) . . . . ?
C4 C3 N8 N9 178.9(3) . . . . ?
C4 C3 N8 C12 0.0(5) . . . . ?
C4 C5 C6 C7 0.0(5) . . . . ?
C5 C6 C7 N2 -0.8(4) . . . . ?
C5 C6 C7 N13 178.1(3) . . . . ?
C6 C7 N13 N14 177.6(3) . . . . ?
C6 C7 N13 C17 -5.4(5) . . . . ?
C7 N2 C3 C4 -0.6(4) . . . . ?
C7 N2 C3 N8 178.8(2) . . . . ?
C7 N13 N14 Fe1 4.0(3) . . . . ?
C7 N13 N14 Ni1 4.0(3) . . . . ?
C7 N13 N14 C15 178.3(3) . . . . ?
C7 N13 C17 C16 -177.6(3) . . . . ?
N8 C3 C4 C5 -179.4(3) . . . . ?
N8 N9 C10 C11 -0.4(3) . . . . ?
N9 N8 C12 C11 0.0(3) . . . . ?
N9 C10 C11 C12 0.4(4) . . . . ?
C10 C11 C12 N8 -0.2(4) . . . . ?
C12 N8 N9 Fe1 -179.95(19) . . . . ?
C12 N8 N9 Ni1 -179.95(19) . . . . ?
C12 N8 N9 C10 0.2(3) . . . . ?
N13 N14 C15 C16 -0.6(4) . . . . ?
N14 N13 C17 C16 -0.4(4) . . . . ?
N14 C15 C16 C17 0.4(4) . . . . ?
C15 C16 C17 N13 0.0(4) . . . . ?
C17 N13 N14 Fe1 -173.6(2) . . . . ?
C17 N13 N14 Ni1 -173.6(2) . . . . ?
C17 N13 N14 C15 0.7(3) . . . . ?
N18 C19 C20 C21 1.0(4) . . . . ?
N18 C19 N24 N25 0.8(3) . . . . ?
N18 C19 N24 C28 -174.0(3) . . . . ?
N18 C23 N29 N30 2.0(3) . . . . ?
N18 C23 N29 C33 177.6(3) . . . . ?
C19 N18 C23 C22 0.9(4) . . . . ?
C19 N18 C23 N29 -179.2(2) . . . . ?
C19 C20 C21 C22 0.1(5) . . . . ?
C19 N24 N25 Fe1 -0.9(3) . . . . ?
C19 N24 N25 Ni1 -0.9(3) . . . . ?
C19 N24 N25 C26 -176.5(2) . . . . ?
C19 N24 C28 C27 175.6(3) . . . . ?
C20 C19 N24 N25 -179.4(3) . . . . ?
C20 C19 N24 C28 5.7(5) . . . . ?
C20 C21 C22 C23 -0.7(5) . . . . ?
C21 C22 C23 N18 0.2(4) . . . . ?
C21 C22 C23 N29 -179.8(3) . . . . ?
C22 C23 N29 N30 -178.1(3) . . . . ?
C22 C23 N29 C33 -2.4(5) . . . . ?
C23 N18 C19 C20 -1.5(4) . . . . ?
C23 N18 C19 N24 178.3(2) . . . . ?
C23 N29 N30 Fe1 -2.4(3) . . . . ?
C23 N29 N30 Ni1 -2.4(3) . . . . ?
C23 N29 N30 C31 176.1(2) . . . . ?
C23 N29 C33 C32 -175.7(3) . . . . ?
N24 C19 C20 C21 -178.8(3) . . . . ?
N24 N25 C26 C27 0.6(3) . . . . ?
N25 N24 C28 C27 0.6(4) . . . . ?
N25 C26 C27 C28 -0.2(4) . . . . ?
C26 C27 C28 N24 -0.2(4) . . . . ?
C28 N24 N25 Fe1 174.9(2) . . . . ?
C28 N24 N25 Ni1 174.9(2) . . . . ?
C28 N24 N25 C26 -0.7(3) . . . . ?
N29 N30 C31 C32 0.5(3) . . . . ?
N30 N29 C33 C32 0.2(3) . . . . ?
N30 C31 C32 C33 -0.5(4) . . . . ?
C31 C32 C33 N29 0.2(4) . . . . ?
C33 N29 N30 Fe1 -178.97(19) . . . . ?
C33 N29 N30 Ni1 -178.97(19) . . . . ?
C33 N29 N30 C31 -0.4(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.982(13)
2 0.018(13)

_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_mh202ltd
_database_code_depnum_ccdc_archive 'CCDC 2261796'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2023-08-22 deposited with the CCDC.	2023-08-30 downloaded from the CCDC.
;
_audit_creation_date             2023-03-13
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis[2,6-di(pyrazol-1-yl)pyridine]iron(II) bis[2,6-di(pyrazol-1-yl)pyridine]-nickel(II) ditetrafluoroborate 0.46:0.54 solid solution (disordered refinement)'
_chemical_formula_moiety         
'0.46(C22 H18 Fe N10), 0.54(C22 H18 N10 Ni), 2(B F4)'
_chemical_formula_sum            'C22 H18 B2 F8 Fe0.46 N10 Ni0.54'
_chemical_formula_weight         653.48
_chemical_absolute_configuration ab
_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 0.0019 0.0015 '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 0.0004 0.0006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0124 0.0097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.2961 0.8007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0037 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.2866 1.0558 '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           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   8.4441(1)
_cell_length_b                   8.5062(1)
_cell_length_c                   18.4578(1)
_cell_angle_alpha                90
_cell_angle_beta                 97.907(1)
_cell_angle_gamma                90
_cell_volume                     1313.17(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    18528
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      35.82
_cell_measurement_theta_min      1.07
_exptl_absorpt_coefficient_mu    0.697
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.924
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
DIALS 3.12.1-2-g1c07bc2b3-release
Scaling & analysis of unmerged intensities, absorption correction using 
spherical harmonics
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       lath
_exptl_crystal_F_000             658
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            30085
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.886
_diffrn_reflns_theta_full        24.620
_diffrn_reflns_theta_max         36.139
_diffrn_reflns_theta_min         1.080
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.929
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_measurement_device       'Fixed χ 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_reflns_Friedel_coverage         0.813
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.837
_reflns_number_gt                11565
_reflns_number_total             12239
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'XIA2 0.4.0.438-g4431aaa (Winter, 2010)'
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction        'XIA2 0.4.0.438-g4431aaa (Winter, 2010)'
_computing_molecular_graphics    'XSEED (Barbour, 2020)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.057(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         12239
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0408
_refine_ls_restrained_S_all      1.018
_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)+(0.0239P)²+0.8194P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0922
_refine_special_details          
;Following an initial structure solution, discrete partial (low-spin) 
 [Fe(bpp)₂]2+ and [Ni(bpp)₂]2+ molecule sites were constructed and 
 refined without restraints. The Fe:Ni occupancy ratio refined to 0.46:0.54, 
 so those occupancies were used for those disorder sites in the final least 
 squares cycles. No distance restraints were applied to the model, but a 
 SIMU constraint was applied to Fe1 and Ni1, whose Ueq values correlated
 with each other.

 The Fe, Ni, B and F atoms were refined anisotropically. Attempts to
 refine the partial N atoms anisotropically led to them becoming non-
 positive definite, so they were left isotropic in the final least squares 
 cycles. H atoms were placed in calculated positions and refined using a 
 riding model. 

 A minor inversion twin domain was included in the refinement, to 
 account for the slightly high Flack parameter.,Twin
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.943(10)
 0.057(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Uiso/Uaniso restraints and constraints
Fe1 \\sim Ni1: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
4. Others
 Fixed Sof: Fe1(0.46) N2A(0.46) C3A(0.46) C4A(0.46) H4A(0.46) C5A(0.46)
 H5A(0.46) C6A(0.46) H6A(0.46) C7A(0.46) N8A(0.46) N9A(0.46) C10A(0.46)
 H10A(0.46) C11A(0.46) H11A(0.46) C12A(0.46) H12A(0.46) N13A(0.46) N14A(0.46)
 C15A(0.46) H15A(0.46) C16A(0.46) H16A(0.46) C17A(0.46) H17A(0.46) N18A(0.46)
 C19A(0.46) C20A(0.46) H20A(0.46) C21A(0.46) H21A(0.46) C22A(0.46) H22A(0.46)
 C23A(0.46) N24A(0.46) N25A(0.46) C26A(0.46) H26A(0.46) C27A(0.46) H27A(0.46)
 C28A(0.46) H28A(0.46) N29A(0.46) N30A(0.46) C31A(0.46) H31A(0.46) C32A(0.46)
 H32A(0.46) C33A(0.46) H33A(0.46) Ni1(0.54) N2B(0.54) C3B(0.54) C4B(0.54)
 H4B(0.54) C5B(0.54) H5B(0.54) C6B(0.54) H6B(0.54) C7B(0.54) N8B(0.54)
 N9B(0.54) C10B(0.54) H10B(0.54) C11B(0.54) H11B(0.54) C12B(0.54) H12B(0.54)
 N13B(0.54) N14B(0.54) C15B(0.54) H15B(0.54) C16B(0.54) H16B(0.54) C17B(0.54)
 H17B(0.54) N18B(0.54) C19B(0.54) C20B(0.54) H20B(0.54) C21B(0.54) H21B(0.54)
 C22B(0.54) H22B(0.54) C23B(0.54) N24B(0.54) N25B(0.54) C26B(0.54) H26B(0.54)
 C27B(0.54) H27B(0.54) C28B(0.54) H28B(0.54) N29B(0.54) N30B(0.54) C31B(0.54)
 H31B(0.54) C32B(0.54) H32B(0.54) C33B(0.54) H33B(0.54)
5.a Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C5A(H5A), C6A(H6A), C10A(H10A), C11A(H11A), C12A(H12A), C15A(H15A),
 C16A(H16A), C17A(H17A), C20A(H20A), C21A(H21A), C22A(H22A), C26A(H26A),
 C27A(H27A), C28A(H28A), C31A(H31A), C32A(H32A), C33A(H33A), C4B(H4B), C5B(H5B),
  C6B(H6B), C10B(H10B), C11B(H11B), C12B(H12B), C15B(H15B), C16B(H16B),
 C17B(H17B), C20B(H20B), C21B(H21B), C22B(H22B), C26B(H26B), C27B(H27B),
 C28B(H28B), C31B(H31B), C32B(H32B), C33B(H33B)
;
_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 0.7141(13) 0.8392(19) 0.7455(5) 0.0121(4) Uani 0.46 1 d . U P A 1
N2A N 0.7152(14) 0.8603(14) 0.6424(6) 0.012(3) Uiso 0.46 1 d . . P A 1
C3A C 0.590(2) 0.915(2) 0.5985(10) 0.020(4) Uiso 0.46 1 d . . P A 1
C4A C 0.5832(10) 0.9236(10) 0.5224(5) 0.017(2) Uiso 0.46 1 d . . P A 1
H4A H 0.491824 0.963470 0.492181 0.020 Uiso 0.46 1 calc R U P A 1
C5A C 0.7167(9) 0.8716(9) 0.4934(4) 0.0173(17) Uiso 0.46 1 d . . P A 1
H5A H 0.717516 0.877678 0.442049 0.021 Uiso 0.46 1 calc R U P A 1
C6A C 0.8485(10) 0.8112(10) 0.5370(5) 0.0149(18) Uiso 0.46 1 d . . P A 1
H6A H 0.940747 0.777242 0.517191 0.018 Uiso 0.46 1 calc R U P A 1
C7A C 0.8393(13) 0.8026(12) 0.6117(6) 0.013(2) Uiso 0.46 1 d . . P A 1
N8A N 0.4669(15) 0.9635(14) 0.6430(7) 0.015(3) Uiso 0.46 1 d . . P A 1
N9A N 0.5008(13) 0.9293(12) 0.7183(6) 0.021(3) Uiso 0.46 1 d . . P A 1
C10A C 0.3716(8) 0.9782(8) 0.7473(4) 0.0152(14) Uiso 0.46 1 d . . P A 1
H10A H 0.361695 0.974362 0.797901 0.018 Uiso 0.46 1 calc R U P A 1
C11A C 0.2531(9) 1.0358(8) 0.6926(4) 0.0201(14) Uiso 0.46 1 d . . P A 1
H11A H 0.151373 1.076603 0.699157 0.024 Uiso 0.46 1 calc R U P A 1
C12A C 0.3139(11) 1.0210(10) 0.6282(5) 0.023(2) Uiso 0.46 1 d . . P A 1
H12A H 0.259660 1.046262 0.581071 0.027 Uiso 0.46 1 calc R U P A 1
N13A N 0.9587(9) 0.7422(9) 0.6644(4) 0.0126(16) Uiso 0.46 1 d . . P A 1
N14A N 0.9273(9) 0.7496(9) 0.7358(4) 0.0177(17) Uiso 0.46 1 d . . P A 1
C15A C 1.0531(7) 0.6831(7) 0.7763(3) 0.0159(11) Uiso 0.46 1 d . . P A 1
H15A H 1.066057 0.672391 0.828004 0.019 Uiso 0.46 1 calc R U P A 1
C16A C 1.1649(7) 0.6308(7) 0.7304(3) 0.0168(10) Uiso 0.46 1 d . . P A 1
H16A H 1.263340 0.578375 0.745248 0.020 Uiso 0.46 1 calc R U P A 1
C17A C 1.1026(8) 0.6707(7) 0.6611(4) 0.0182(12) Uiso 0.46 1 d . . P A 1
H17A H 1.150246 0.652366 0.618143 0.022 Uiso 0.46 1 calc R U P A 1
N18A N 0.7191(11) 0.8078(11) 0.8505(5) 0.013(2) Uiso 0.46 1 d . . P A 1
C19A C 0.7771(13) 0.9184(11) 0.8979(6) 0.017(3) Uiso 0.46 1 d . . P A 1
C20A C 0.7840(10) 0.9014(10) 0.9730(5) 0.0184(18) Uiso 0.46 1 d . . P A 1
H20A H 0.826768 0.980991 1.006167 0.022 Uiso 0.46 1 calc R U P A 1
C21A C 0.7246(8) 0.7609(9) 0.9970(4) 0.0161(14) Uiso 0.46 1 d . . P A 1
H21A H 0.723765 0.745616 1.047966 0.019 Uiso 0.46 1 calc R U P A 1
C22A C 0.6670(9) 0.6438(9) 0.9493(4) 0.0150(16) Uiso 0.46 1 d . . P A 1
H22A H 0.629469 0.547068 0.966262 0.018 Uiso 0.46 1 calc R U P A 1
C23A C 0.6661(11) 0.6726(10) 0.8758(5) 0.014(2) Uiso 0.46 1 d . . P A 1
N24A N 0.8372(15) 1.0509(14) 0.8617(7) 0.020(3) Uiso 0.46 1 d . . P A 1
N25A N 0.8135(8) 1.0384(8) 0.7831(4) 0.0156(14) Uiso 0.46 1 d . . P A 1
C26A C 0.8803(8) 1.1703(7) 0.7598(4) 0.0156(12) Uiso 0.46 1 d . . P A 1
H26A H 0.885870 1.194485 0.709984 0.019 Uiso 0.46 1 calc R U P A 1
C27A C 0.9408(9) 1.2678(9) 0.8196(4) 0.0223(15) Uiso 0.46 1 d . . P A 1
H27A H 0.994879 1.365204 0.817124 0.027 Uiso 0.46 1 calc R U P A 1
C28A C 0.9060(12) 1.1941(11) 0.8816(5) 0.023(2) Uiso 0.46 1 d . . P A 1
H28A H 0.925929 1.234797 0.929954 0.028 Uiso 0.46 1 calc R U P A 1
N29A N 0.6113(12) 0.5735(12) 0.8184(5) 0.016(2) Uiso 0.46 1 d . . P A 1
N30A N 0.6278(11) 0.6277(10) 0.7488(5) 0.019(2) Uiso 0.46 1 d . . P A 1
C31A C 0.5823(7) 0.5056(7) 0.7040(3) 0.0141(11) Uiso 0.46 1 d . . P A 1
H31A H 0.581604 0.507129 0.652453 0.017 Uiso 0.46 1 calc R U P A 1
C32A C 0.5363(7) 0.3764(7) 0.7432(4) 0.0198(11) Uiso 0.46 1 d . . P A 1
H32A H 0.497998 0.277905 0.723895 0.024 Uiso 0.46 1 calc R U P A 1
C33A C 0.5579(8) 0.4213(8) 0.8152(4) 0.0187(13) Uiso 0.46 1 d . . P A 1
H33A H 0.539199 0.358184 0.855594 0.022 Uiso 0.46 1 calc R U P A 1
Ni1 Ni 0.7225(10) 0.8420(13) 0.7471(4) 0.0133(5) Uani 0.54 1 d . U P B 2
N2B N 0.7111(13) 0.8541(14) 0.6387(6) 0.017(3) Uiso 0.54 1 d . . P B 2
C3B C 0.5811(15) 0.9163(14) 0.5993(7) 0.012(3) Uiso 0.54 1 d . . P B 2
C4B C 0.5671(9) 0.9331(9) 0.5248(4) 0.0164(16) Uiso 0.54 1 d . . P B 2
H4B H 0.474137 0.976913 0.497354 0.020 Uiso 0.54 1 calc R U P B 2
C5B C 0.6962(9) 0.8826(8) 0.4914(4) 0.0190(15) Uiso 0.54 1 d . . P B 2
H5B H 0.690980 0.891749 0.439815 0.023 Uiso 0.54 1 calc R U P B 2
C6B C 0.8330(9) 0.8190(9) 0.5317(4) 0.0200(19) Uiso 0.54 1 d . . P B 2
H6B H 0.920602 0.783644 0.508815 0.024 Uiso 0.54 1 calc R U P B 2
C7B C 0.8349(12) 0.8098(11) 0.6061(5) 0.018(2) Uiso 0.54 1 d . . P B 2
N8B N 0.4645(14) 0.9552(12) 0.6397(6) 0.017(3) Uiso 0.54 1 d . . P B 2
N9B N 0.4932(9) 0.9384(8) 0.7136(4) 0.0122(15) Uiso 0.54 1 d . . P B 2
C10B C 0.3592(8) 0.9866(7) 0.7363(4) 0.0179(13) Uiso 0.54 1 d . . P B 2
H10B H 0.340493 0.983769 0.785821 0.022 Uiso 0.54 1 calc R U P B 2
C11B C 0.2486(7) 1.0421(7) 0.6786(3) 0.0182(11) Uiso 0.54 1 d . . P B 2
H11B H 0.145426 1.084290 0.681393 0.022 Uiso 0.54 1 calc R U P B 2
C12B C 0.3203(7) 1.0226(7) 0.6176(4) 0.0150(12) Uiso 0.54 1 d . . P B 2
H12B H 0.277728 1.050751 0.569020 0.018 Uiso 0.54 1 calc R U P B 2
N13B N 0.9561(9) 0.7446(9) 0.6564(4) 0.0189(17) Uiso 0.54 1 d . . P B 2
N14B N 0.9420(8) 0.7528(8) 0.7301(4) 0.0165(14) Uiso 0.54 1 d . . P B 2
C15B C 1.0687(7) 0.6776(6) 0.7632(3) 0.0194(11) Uiso 0.54 1 d . . P B 2
H15B H 1.092025 0.665041 0.814718 0.023 Uiso 0.54 1 calc R U P B 2
C16B C 1.1639(7) 0.6191(7) 0.7135(3) 0.0225(10) Uiso 0.54 1 d . . P B 2
H16B H 1.260303 0.560903 0.724209 0.027 Uiso 0.54 1 calc R U P B 2
C17B C 1.0900(7) 0.6629(6) 0.6461(3) 0.0189(10) Uiso 0.54 1 d . . P B 2
H17B H 1.125300 0.640540 0.600524 0.023 Uiso 0.54 1 calc R U P B 2
N18B N 0.7245(10) 0.8195(11) 0.8533(4) 0.0158(19) Uiso 0.54 1 d . . P B 2
C19B C 0.7812(9) 0.9338(9) 0.8985(4) 0.0123(18) Uiso 0.54 1 d . . P B 2
C20B C 0.7860(8) 0.9230(8) 0.9732(3) 0.0144(13) Uiso 0.54 1 d . . P B 2
H20B H 0.825203 1.006977 1.004552 0.017 Uiso 0.54 1 calc R U P B 2
C21B C 0.7314(7) 0.7849(7) 1.0009(3) 0.0166(12) Uiso 0.54 1 d . . P B 2
H21B H 0.733490 0.773759 1.052209 0.020 Uiso 0.54 1 calc R U P B 2
C22B C 0.6734(9) 0.6617(9) 0.9546(4) 0.0190(16) Uiso 0.54 1 d . . P B 2
H22B H 0.636876 0.566025 0.973066 0.023 Uiso 0.54 1 calc R U P B 2
C23B C 0.6722(9) 0.6871(9) 0.8800(4) 0.0152(18) Uiso 0.54 1 d . . P B 2
N24B N 0.8306(12) 1.0611(11) 0.8608(5) 0.014(2) Uiso 0.54 1 d . . P B 2
N25B N 0.8206(7) 1.0580(6) 0.7884(3) 0.0143(11) Uiso 0.54 1 d . . P B 2
C26B C 0.8910(7) 1.1889(7) 0.7709(3) 0.0187(11) Uiso 0.54 1 d . . P B 2
H26B H 0.899670 1.220558 0.722270 0.022 Uiso 0.54 1 calc R U P B 2
C27B C 0.9507(8) 1.2743(7) 0.8331(3) 0.0215(12) Uiso 0.54 1 d . . P B 2
H27B H 1.004663 1.372500 0.835208 0.026 Uiso 0.54 1 calc R U P B 2
C28B C 0.9146(9) 1.1857(9) 0.8908(4) 0.0195(16) Uiso 0.54 1 d . . P B 2
H28B H 0.942866 1.207568 0.941356 0.023 Uiso 0.54 1 calc R U P B 2
N29B N 0.6196(11) 0.5743(10) 0.8248(4) 0.0172(19) Uiso 0.54 1 d . . P B 2
N30B N 0.6311(8) 0.6137(8) 0.7537(4) 0.0140(14) Uiso 0.54 1 d . . P B 2
C31B C 0.5804(7) 0.4878(7) 0.7155(3) 0.0191(12) Uiso 0.54 1 d . . P B 2
H31B H 0.576529 0.479607 0.663923 0.023 Uiso 0.54 1 calc R U P B 2
C32B C 0.5337(6) 0.3690(5) 0.7594(3) 0.0177(9) Uiso 0.54 1 d . . P B 2
H32B H 0.492742 0.268494 0.744222 0.021 Uiso 0.54 1 calc R U P B 2
C33B C 0.5591(6) 0.4276(6) 0.8297(3) 0.0162(10) Uiso 0.54 1 d . . P B 2
H33B H 0.538293 0.375595 0.872903 0.019 Uiso 0.54 1 calc R U P B 2
B34 B 0.7961(4) 0.2996(3) 0.56451(15) 0.0227(5) Uani 1 1 d . . . . .
F35 F 0.6773(2) 0.2464(2) 0.60368(9) 0.0269(3) Uani 1 1 d . . . . .
F36 F 0.7664(2) 0.2474(2) 0.49225(9) 0.0311(4) Uani 1 1 d . . . . .
F37 F 0.7956(2) 0.4639(2) 0.56445(10) 0.0323(4) Uani 1 1 d . . . . .
F38 F 0.9443(2) 0.2442(3) 0.59658(10) 0.0444(5) Uani 1 1 d . . . . .
B39 B 0.7186(4) 0.2811(4) 1.05834(15) 0.0246(5) Uani 1 1 d . . . . .
F40 F 0.6432(2) 0.2704(2) 0.98615(8) 0.0276(3) Uani 1 1 d . . . C 1
F41 F 0.6811(2) 0.1502(2) 1.09805(9) 0.0315(4) Uani 1 1 d . . . D 1
F42 F 0.8836(2) 0.2825(3) 1.05780(10) 0.0430(5) Uani 1 1 d . . . E 1
F43 F 0.6671(4) 0.4160(3) 1.08959(11) 0.0543(6) Uani 1 1 d . . . F 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 N2A 1.914(15) . ?
Fe1 N9A 1.959(16) . ?
Fe1 N14A 1.985(14) . ?
Fe1 N18A 1.950(14) . ?
Fe1 N25A 1.974(16) . ?
Fe1 N30A 1.945(18) . ?
N2A C3A 1.33(2) . ?
N2A C7A 1.350(16) . ?
C3A C4A 1.40(2) . ?
C3A N8A 1.47(2) . ?
C4A H4A 0.9500 . ?
C4A C5A 1.386(12) . ?
C5A H5A 0.9500 . ?
C5A C6A 1.381(12) . ?
C6A H6A 0.9500 . ?
C6A C7A 1.393(13) . ?
C7A N13A 1.399(13) . ?
N8A N9A 1.410(16) . ?
N8A C12A 1.373(16) . ?
N9A C10A 1.345(13) . ?
C10A H10A 0.9500 . ?
C10A C11A 1.408(11) . ?
C11A H11A 0.9500 . ?
C11A C12A 1.363(11) . ?
C12A H12A 0.9500 . ?
N13A N14A 1.382(11) . ?
N13A C17A 1.367(10) . ?
N14A C15A 1.337(10) . ?
C15A H15A 0.9500 . ?
C15A C16A 1.424(9) . ?
C16A H16A 0.9500 . ?
C16A C17A 1.357(9) . ?
C17A H17A 0.9500 . ?
N18A C19A 1.332(14) . ?
N18A C23A 1.342(13) . ?
C19A C20A 1.387(14) . ?
C19A N24A 1.438(16) . ?
C20A H20A 0.9500 . ?
C20A C21A 1.391(12) . ?
C21A H21A 0.9500 . ?
C21A C22A 1.374(11) . ?
C22A H22A 0.9500 . ?
C22A C23A 1.377(12) . ?
C23A N29A 1.383(13) . ?
N24A N25A 1.441(15) . ?
N24A C28A 1.378(16) . ?
N25A C26A 1.352(9) . ?
C26A H26A 0.9500 . ?
C26A C27A 1.418(10) . ?
C27A H27A 0.9500 . ?
C27A C28A 1.373(12) . ?
C28A H28A 0.9500 . ?
N29A N30A 1.391(13) . ?
N29A C33A 1.369(12) . ?
N30A C31A 1.351(11) . ?
C31A H31A 0.9500 . ?
C31A C32A 1.400(9) . ?
C32A H32A 0.9500 . ?
C32A C33A 1.370(9) . ?
C33A H33A 0.9500 . ?
Ni1 N2B 1.993(13) . ?
Ni1 N9B 2.116(12) . ?
Ni1 N14B 2.066(11) . ?
Ni1 N18B 1.968(11) . ?
Ni1 N25B 2.114(13) . ?
Ni1 N30B 2.099(14) . ?
N2B C3B 1.340(17) . ?
N2B C7B 1.330(15) . ?
C3B C4B 1.372(15) . ?
C3B N8B 1.356(17) . ?
C4B H4B 0.9500 . ?
C4B C5B 1.391(10) . ?
C5B H5B 0.9500 . ?
C5B C6B 1.394(10) . ?
C6B H6B 0.9500 . ?
C6B C7B 1.373(12) . ?
C7B N13B 1.398(12) . ?
N8B N9B 1.358(13) . ?
N8B C12B 1.357(13) . ?
N9B C10B 1.324(10) . ?
C10B H10B 0.9500 . ?
C10B C11B 1.398(9) . ?
C11B H11B 0.9500 . ?
C11B C12B 1.359(9) . ?
C12B H12B 0.9500 . ?
N13B N14B 1.384(10) . ?
N13B C17B 1.362(10) . ?
N14B C15B 1.322(8) . ?
C15B H15B 0.9500 . ?
C15B C16B 1.393(8) . ?
C16B H16B 0.9500 . ?
C16B C17B 1.364(8) . ?
C17B H17B 0.9500 . ?
N18B C19B 1.326(11) . ?
N18B C23B 1.329(12) . ?
C19B C20B 1.378(10) . ?
C19B N24B 1.382(12) . ?
C20B H20B 0.9500 . ?
C20B C21B 1.384(9) . ?
C21B H21B 0.9500 . ?
C21B C22B 1.397(10) . ?
C22B H22B 0.9500 . ?
C22B C23B 1.393(11) . ?
C23B N29B 1.425(11) . ?
N24B N25B 1.328(11) . ?
N24B C28B 1.351(12) . ?
N25B C26B 1.323(8) . ?
C26B H26B 0.9500 . ?
C26B C27B 1.394(9) . ?
C27B H27B 0.9500 . ?
C27B C28B 1.371(10) . ?
C28B H28B 0.9500 . ?
N29B N30B 1.369(11) . ?
N29B C33B 1.356(10) . ?
N30B C31B 1.322(9) . ?
C31B H31B 0.9500 . ?
C31B C32B 1.386(8) . ?
C32B H32B 0.9500 . ?
C32B C33B 1.379(8) . ?
C33B H33B 0.9500 . ?
B34 F35 1.390(3) . ?
B34 F36 1.395(3) . ?
B34 F37 1.397(3) . ?
B34 F38 1.391(3) . ?
B39 F40 1.398(3) . ?
B39 F41 1.394(3) . ?
B39 F42 1.395(4) . ?
B39 F43 1.381(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
N2A Fe1 N9A 80.7(6) . . ?
N2A Fe1 N14A 79.5(6) . . ?
N2A Fe1 N18A 177.1(10) . . ?
N2A Fe1 N25A 102.1(7) . . ?
N2A Fe1 N30A 99.8(7) . . ?
N9A Fe1 N14A 160.1(7) . . ?
N9A Fe1 N25A 95.0(7) . . ?
N18A Fe1 N9A 101.7(6) . . ?
N18A Fe1 N14A 98.1(6) . . ?
N18A Fe1 N25A 79.5(6) . . ?
N25A Fe1 N14A 90.8(6) . . ?
N30A Fe1 N9A 92.0(7) . . ?
N30A Fe1 N14A 89.8(7) . . ?
N30A Fe1 N18A 78.4(6) . . ?
N30A Fe1 N25A 157.8(7) . . ?
C3A N2A Fe1 121.8(11) . . ?
C3A N2A C7A 118.2(12) . . ?
C7A N2A Fe1 119.6(9) . . ?
N2A C3A C4A 123.3(13) . . ?
N2A C3A N8A 108.9(14) . . ?
C4A C3A N8A 127.8(14) . . ?
C3A C4A H4A 121.7 . . ?
C5A C4A C3A 116.7(10) . . ?
C5A C4A H4A 121.7 . . ?
C4A C5A H5A 119.1 . . ?
C6A C5A C4A 121.8(8) . . ?
C6A C5A H5A 119.1 . . ?
C5A C6A H6A 121.7 . . ?
C5A C6A C7A 116.5(8) . . ?
C7A C6A H6A 121.7 . . ?
N2A C7A C6A 123.2(10) . . ?
N2A C7A N13A 111.6(9) . . ?
C6A C7A N13A 125.0(9) . . ?
N9A N8A C3A 115.4(12) . . ?
C12A N8A C3A 135.0(12) . . ?
C12A N8A N9A 109.1(10) . . ?
N8A N9A Fe1 112.9(9) . . ?
C10A N9A Fe1 141.8(8) . . ?
C10A N9A N8A 105.2(9) . . ?
N9A C10A H10A 124.6 . . ?
N9A C10A C11A 110.9(7) . . ?
C11A C10A H10A 124.6 . . ?
C10A C11A H11A 126.9 . . ?
C12A C11A C10A 106.1(7) . . ?
C12A C11A H11A 126.9 . . ?
N8A C12A H12A 125.8 . . ?
C11A C12A N8A 108.4(9) . . ?
C11A C12A H12A 125.8 . . ?
N14A N13A C7A 115.6(8) . . ?
C17A N13A C7A 133.8(8) . . ?
C17A N13A N14A 110.6(7) . . ?
N13A N14A Fe1 113.5(6) . . ?
C15A N14A Fe1 140.6(7) . . ?
C15A N14A N13A 105.7(7) . . ?
N14A C15A H15A 125.0 . . ?
N14A C15A C16A 109.9(6) . . ?
C16A C15A H15A 125.0 . . ?
C15A C16A H16A 126.9 . . ?
C17A C16A C15A 106.3(5) . . ?
C17A C16A H16A 126.9 . . ?
N13A C17A H17A 126.3 . . ?
C16A C17A N13A 107.5(6) . . ?
C16A C17A H17A 126.3 . . ?
C19A N18A Fe1 120.8(9) . . ?
C19A N18A C23A 119.1(9) . . ?
C23A N18A Fe1 120.1(8) . . ?
N18A C19A C20A 123.0(9) . . ?
N18A C19A N24A 111.7(10) . . ?
C20A C19A N24A 125.3(10) . . ?
C19A C20A H20A 121.9 . . ?
C19A C20A C21A 116.1(8) . . ?
C21A C20A H20A 121.9 . . ?
C20A C21A H21A 119.0 . . ?
C22A C21A C20A 122.0(7) . . ?
C22A C21A H21A 119.0 . . ?
C21A C22A H22A 121.4 . . ?
C21A C22A C23A 117.1(7) . . ?
C23A C22A H22A 121.4 . . ?
N18A C23A C22A 122.6(8) . . ?
N18A C23A N29A 110.4(8) . . ?
C22A C23A N29A 127.0(8) . . ?
C19A N24A N25A 113.7(10) . . ?
C28A N24A C19A 137.0(11) . . ?
C28A N24A N25A 109.2(10) . . ?
N24A N25A Fe1 114.2(7) . . ?
C26A N25A Fe1 140.9(6) . . ?
C26A N25A N24A 104.7(7) . . ?
N25A C26A H26A 124.5 . . ?
N25A C26A C27A 111.1(6) . . ?
C27A C26A H26A 124.5 . . ?
C26A C27A H27A 126.7 . . ?
C28A C27A C26A 106.6(7) . . ?
C28A C27A H27A 126.7 . . ?
N24A C28A H28A 125.9 . . ?
C27A C28A N24A 108.2(9) . . ?
C27A C28A H28A 125.9 . . ?
C23A N29A N30A 116.1(9) . . ?
C33A N29A C23A 133.1(9) . . ?
C33A N29A N30A 110.3(8) . . ?
N29A N30A Fe1 114.9(7) . . ?
C31A N30A Fe1 140.2(7) . . ?
C31A N30A N29A 104.8(7) . . ?
N30A C31A H31A 124.4 . . ?
N30A C31A C32A 111.2(6) . . ?
C32A C31A H31A 124.4 . . ?
C31A C32A H32A 127.1 . . ?
C33A C32A C31A 105.9(5) . . ?
C33A C32A H32A 127.1 . . ?
N29A C33A C32A 107.8(7) . . ?
N29A C33A H33A 126.1 . . ?
C32A C33A H33A 126.1 . . ?
N2B Ni1 N9B 76.7(5) . . ?
N2B Ni1 N14B 77.7(5) . . ?
N2B Ni1 N25B 106.2(6) . . ?
N2B Ni1 N30B 98.0(6) . . ?
N14B Ni1 N9B 154.4(5) . . ?
N14B Ni1 N25B 93.3(4) . . ?
N14B Ni1 N30B 90.8(5) . . ?
N18B Ni1 N2B 176.6(8) . . ?
N18B Ni1 N9B 102.2(5) . . ?
N18B Ni1 N14B 103.4(5) . . ?
N18B Ni1 N25B 77.1(4) . . ?
N18B Ni1 N30B 78.7(5) . . ?
N25B Ni1 N9B 93.8(5) . . ?
N30B Ni1 N9B 92.7(5) . . ?
N30B Ni1 N25B 155.8(5) . . ?
C3B N2B Ni1 119.2(9) . . ?
C7B N2B Ni1 120.5(8) . . ?
C7B N2B C3B 120.2(10) . . ?
N2B C3B C4B 122.4(11) . . ?
N2B C3B N8B 113.6(11) . . ?
N8B C3B C4B 123.9(11) . . ?
C3B C4B H4B 121.7 . . ?
C3B C4B C5B 116.6(8) . . ?
C5B C4B H4B 121.7 . . ?
C4B C5B H5B 119.2 . . ?
C4B C5B C6B 121.7(7) . . ?
C6B C5B H5B 119.2 . . ?
C5B C6B H6B 121.6 . . ?
C7B C6B C5B 116.8(7) . . ?
C7B C6B H6B 121.6 . . ?
N2B C7B C6B 122.3(9) . . ?
N2B C7B N13B 111.2(8) . . ?
C6B C7B N13B 126.4(8) . . ?
C3B N8B N9B 118.9(10) . . ?
C3B N8B C12B 128.8(10) . . ?
C12B N8B N9B 112.0(9) . . ?
N8B N9B Ni1 111.3(7) . . ?
C10B N9B Ni1 144.6(6) . . ?
C10B N9B N8B 104.0(8) . . ?
N9B C10B H10B 124.0 . . ?
N9B C10B C11B 112.0(6) . . ?
C11B C10B H10B 124.0 . . ?
C10B C11B H11B 127.4 . . ?
C12B C11B C10B 105.2(5) . . ?
C12B C11B H11B 127.4 . . ?
N8B C12B C11B 106.6(7) . . ?
N8B C12B H12B 126.7 . . ?
C11B C12B H12B 126.7 . . ?
N14B N13B C7B 118.6(7) . . ?
C17B N13B C7B 131.0(7) . . ?
C17B N13B N14B 110.3(6) . . ?
N13B N14B Ni1 111.6(5) . . ?
C15B N14B Ni1 142.5(6) . . ?
C15B N14B N13B 104.9(6) . . ?
N14B C15B H15B 124.1 . . ?
N14B C15B C16B 111.8(5) . . ?
C16B C15B H15B 124.1 . . ?
C15B C16B H16B 127.2 . . ?
C17B C16B C15B 105.7(5) . . ?
C17B C16B H16B 127.2 . . ?
N13B C17B C16B 107.3(5) . . ?
N13B C17B H17B 126.4 . . ?
C16B C17B H17B 126.4 . . ?
C19B N18B Ni1 120.5(7) . . ?
C19B N18B C23B 119.9(8) . . ?
C23B N18B Ni1 119.6(7) . . ?
N18B C19B C20B 122.6(7) . . ?
N18B C19B N24B 111.5(8) . . ?
C20B C19B N24B 125.9(8) . . ?
C19B C20B H20B 121.3 . . ?
C19B C20B C21B 117.4(6) . . ?
C21B C20B H20B 121.3 . . ?
C20B C21B H21B 119.4 . . ?
C20B C21B C22B 121.2(6) . . ?
C22B C21B H21B 119.4 . . ?
C21B C22B H22B 121.9 . . ?
C23B C22B C21B 116.3(6) . . ?
C23B C22B H22B 121.9 . . ?
N18B C23B C22B 122.7(7) . . ?
N18B C23B N29B 113.1(7) . . ?
C22B C23B N29B 124.2(7) . . ?
N25B N24B C19B 120.6(8) . . ?
N25B N24B C28B 112.6(8) . . ?
C28B N24B C19B 126.0(9) . . ?
N24B N25B Ni1 110.3(6) . . ?
C26B N25B Ni1 144.2(5) . . ?
C26B N25B N24B 105.1(6) . . ?
N25B C26B H26B 124.4 . . ?
N25B C26B C27B 111.2(5) . . ?
C27B C26B H26B 124.4 . . ?
C26B C27B H27B 127.5 . . ?
C28B C27B C26B 105.0(6) . . ?
C28B C27B H27B 127.5 . . ?
N24B C28B C27B 105.9(7) . . ?
N24B C28B H28B 127.0 . . ?
C27B C28B H28B 127.0 . . ?
N30B N29B C23B 117.6(7) . . ?
C33B N29B C23B 130.9(7) . . ?
C33B N29B N30B 111.5(7) . . ?
N29B N30B Ni1 110.9(6) . . ?
C31B N30B Ni1 144.4(6) . . ?
C31B N30B N29B 104.7(6) . . ?
N30B C31B H31B 124.0 . . ?
N30B C31B C32B 112.1(6) . . ?
C32B C31B H31B 124.0 . . ?
C31B C32B H32B 127.3 . . ?
C33B C32B C31B 105.5(4) . . ?
C33B C32B H32B 127.3 . . ?
N29B C33B C32B 106.3(5) . . ?
N29B C33B H33B 126.8 . . ?
C32B C33B H33B 126.8 . . ?
F35 B34 F36 110.2(2) . . ?
F35 B34 F37 108.9(2) . . ?
F35 B34 F38 109.8(2) . . ?
F36 B34 F37 108.5(2) . . ?
F38 B34 F36 109.3(2) . . ?
F38 B34 F37 110.0(2) . . ?
F41 B39 F40 110.0(2) . . ?
F41 B39 F42 108.1(2) . . ?
F42 B39 F40 108.5(2) . . ?
F43 B39 F40 108.9(2) . . ?
F43 B39 F41 109.7(2) . . ?
F43 B39 F42 111.6(3) . . ?

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 N2A C3A C4A -176.5(12) . . . . ?
Fe1 N2A C3A N8A 4.6(19) . . . . ?
Fe1 N2A C7A C6A 179.2(9) . . . . ?
Fe1 N2A C7A N13A -4.1(14) . . . . ?
Fe1 N9A C10A C11A 179.1(12) . . . . ?
Fe1 N14A C15A C16A 174.3(10) . . . . ?
Fe1 N18A C19A C20A -179.7(9) . . . . ?
Fe1 N18A C19A N24A -2.5(13) . . . . ?
Fe1 N18A C23A C22A 179.9(8) . . . . ?
Fe1 N18A C23A N29A -0.9(12) . . . . ?
Fe1 N25A C26A C27A -175.9(8) . . . . ?
Fe1 N30A C31A C32A 176.6(9) . . . . ?
N2A C3A C4A C5A 0(2) . . . . ?
N2A C3A N8A N9A -5.9(18) . . . . ?
N2A C3A N8A C12A -176.8(13) . . . . ?
N2A C7A N13A N14A 1.2(12) . . . . ?
N2A C7A N13A C17A 178.8(9) . . . . ?
C3A N2A C7A C6A 6.5(18) . . . . ?
C3A N2A C7A N13A -176.8(12) . . . . ?
C3A C4A C5A C6A 1.1(14) . . . . ?
C3A N8A N9A Fe1 4.8(15) . . . . ?
C3A N8A N9A C10A -177.7(11) . . . . ?
C3A N8A C12A C11A 175.9(14) . . . . ?
C4A C3A N8A N9A 175.3(14) . . . . ?
C4A C3A N8A C12A 4(3) . . . . ?
C4A C5A C6A C7A 1.1(12) . . . . ?
C5A C6A C7A N2A -5.1(15) . . . . ?
C5A C6A C7A N13A 178.6(8) . . . . ?
C6A C7A N13A N14A 177.9(9) . . . . ?
C6A C7A N13A C17A -4.5(16) . . . . ?
C7A N2A C3A C4A -4(2) . . . . ?
C7A N2A C3A N8A 177.2(11) . . . . ?
C7A N13A N14A Fe1 1.9(11) . . . . ?
C7A N13A N14A C15A 178.5(7) . . . . ?
C7A N13A C17A C16A -177.5(9) . . . . ?
N8A C3A C4A C5A 178.9(13) . . . . ?
N8A N9A C10A C11A 2.8(11) . . . . ?
N9A N8A C12A C11A 4.5(12) . . . . ?
N9A C10A C11A C12A -0.1(9) . . . . ?
C10A C11A C12A N8A -2.7(10) . . . . ?
C12A N8A N9A Fe1 178.0(9) . . . . ?
C12A N8A N9A C10A -4.5(12) . . . . ?
N13A N14A C15A C16A -0.8(8) . . . . ?
N14A N13A C17A C16A 0.3(8) . . . . ?
N14A C15A C16A C17A 1.0(7) . . . . ?
C15A C16A C17A N13A -0.8(7) . . . . ?
C17A N13A N14A Fe1 -176.3(7) . . . . ?
C17A N13A N14A C15A 0.3(9) . . . . ?
N18A C19A C20A C21A -0.7(14) . . . . ?
N18A C19A N24A N25A 3.2(13) . . . . ?
N18A C19A N24A C28A 179.0(13) . . . . ?
N18A C23A N29A N30A 2.8(13) . . . . ?
N18A C23A N29A C33A 174.2(10) . . . . ?
C19A N18A C23A C22A 0.9(15) . . . . ?
C19A N18A C23A N29A -179.9(10) . . . . ?
C19A C20A C21A C22A 2.0(12) . . . . ?
C19A N24A N25A Fe1 -2.7(12) . . . . ?
C19A N24A N25A C26A -178.7(8) . . . . ?
C19A N24A C28A C27A 178.7(13) . . . . ?
C20A C19A N24A N25A -179.6(9) . . . . ?
C20A C19A N24A C28A -4(2) . . . . ?
C20A C21A C22A C23A -1.8(12) . . . . ?
C21A C22A C23A N18A 0.3(13) . . . . ?
C21A C22A C23A N29A -178.7(9) . . . . ?
C22A C23A N29A N30A -178.1(9) . . . . ?
C22A C23A N29A C33A -6.6(18) . . . . ?
C23A N18A C19A C20A -0.7(16) . . . . ?
C23A N18A C19A N24A 176.5(9) . . . . ?
C23A N29A N30A Fe1 -3.5(12) . . . . ?
C23A N29A N30A C31A 173.8(8) . . . . ?
C23A N29A C33A C32A -173.0(10) . . . . ?
N24A C19A C20A C21A -177.5(10) . . . . ?
N24A N25A C26A C27A -1.7(9) . . . . ?
N25A N24A C28A C27A -5.5(12) . . . . ?
N25A C26A C27A C28A -1.5(9) . . . . ?
C26A C27A C28A N24A 4.3(10) . . . . ?
C28A N24A N25A Fe1 -179.6(8) . . . . ?
C28A N24A N25A C26A 4.4(11) . . . . ?
N29A N30A C31A C32A 0.5(9) . . . . ?
N30A N29A C33A C32A -1.2(10) . . . . ?
N30A C31A C32A C33A -1.2(8) . . . . ?
C31A C32A C33A N29A 1.4(8) . . . . ?
C33A N29A N30A Fe1 -176.8(7) . . . . ?
C33A N29A N30A C31A 0.4(10) . . . . ?
Ni1 N2B C3B C4B 177.9(9) . . . . ?
Ni1 N2B C3B N8B -4.2(15) . . . . ?
Ni1 N2B C7B C6B -178.8(8) . . . . ?
Ni1 N2B C7B N13B 5.5(13) . . . . ?
Ni1 N9B C10B C11B 179.6(9) . . . . ?
Ni1 N14B C15B C16B 165.6(8) . . . . ?
Ni1 N18B C19B C20B -179.5(7) . . . . ?
Ni1 N18B C19B N24B 1.3(11) . . . . ?
Ni1 N18B C23B C22B 178.5(7) . . . . ?
Ni1 N18B C23B N29B 0.0(11) . . . . ?
Ni1 N25B C26B C27B -169.3(7) . . . . ?
Ni1 N30B C31B C32B 179.8(8) . . . . ?
N2B C3B C4B C5B -0.3(15) . . . . ?
N2B C3B N8B N9B 4.3(16) . . . . ?
N2B C3B N8B C12B 178.6(10) . . . . ?
N2B C7B N13B N14B -7.9(12) . . . . ?
N2B C7B N13B C17B 168.3(9) . . . . ?
C3B N2B C7B C6B -2.8(17) . . . . ?
C3B N2B C7B N13B -178.5(10) . . . . ?
C3B C4B C5B C6B -0.3(12) . . . . ?
C3B N8B N9B Ni1 -2.3(13) . . . . ?
C3B N8B N9B C10B 179.5(9) . . . . ?
C3B N8B C12B C11B -178.2(11) . . . . ?
C4B C3B N8B N9B -177.9(10) . . . . ?
C4B C3B N8B C12B -3.5(19) . . . . ?
C4B C5B C6B C7B -0.6(12) . . . . ?
C5B C6B C7B N2B 2.2(14) . . . . ?
C5B C6B C7B N13B 177.2(8) . . . . ?
C6B C7B N13B N14B 176.6(8) . . . . ?
C6B C7B N13B C17B -7.2(16) . . . . ?
C7B N2B C3B C4B 1.8(18) . . . . ?
C7B N2B C3B N8B 179.7(11) . . . . ?
C7B N13B N14B Ni1 6.6(10) . . . . ?
C7B N13B N14B C15B 177.7(7) . . . . ?
C7B N13B C17B C16B -177.0(9) . . . . ?
N8B C3B C4B C5B -177.9(10) . . . . ?
N8B N9B C10B C11B -3.3(9) . . . . ?
N9B N8B C12B C11B -3.6(10) . . . . ?
N9B C10B C11B C12B 1.3(7) . . . . ?
C10B C11B C12B N8B 1.4(8) . . . . ?
C12B N8B N9B Ni1 -177.6(7) . . . . ?
C12B N8B N9B C10B 4.2(10) . . . . ?
N13B N14B C15B C16B -0.7(7) . . . . ?
N14B N13B C17B C16B -0.6(8) . . . . ?
N14B C15B C16B C17B 0.4(7) . . . . ?
C15B C16B C17B N13B 0.1(7) . . . . ?
C17B N13B N14B Ni1 -170.3(6) . . . . ?
C17B N13B N14B C15B 0.8(8) . . . . ?
N18B C19B C20B C21B 1.2(11) . . . . ?
N18B C19B N24B N25B -1.1(12) . . . . ?
N18B C19B N24B C28B -169.7(9) . . . . ?
N18B C23B N29B N30B 1.0(11) . . . . ?
N18B C23B N29B C33B -180.0(9) . . . . ?
C19B N18B C23B C22B 0.3(13) . . . . ?
C19B N18B C23B N29B -178.3(8) . . . . ?
C19B C20B C21B C22B -0.2(10) . . . . ?
C19B N24B N25B Ni1 0.4(10) . . . . ?
C19B N24B N25B C26B -174.1(8) . . . . ?
C19B N24B C28B C27B 174.0(8) . . . . ?
C20B C19B N24B N25B 179.8(7) . . . . ?
C20B C19B N24B C28B 11.1(15) . . . . ?
C20B C21B C22B C23B -0.7(10) . . . . ?
C21B C22B C23B N18B 0.7(11) . . . . ?
C21B C22B C23B N29B 179.1(7) . . . . ?
C22B C23B N29B N30B -177.5(8) . . . . ?
C22B C23B N29B C33B 1.6(14) . . . . ?
C23B N18B C19B C20B -1.3(13) . . . . ?
C23B N18B C19B N24B 179.6(8) . . . . ?
C23B N29B N30B Ni1 -1.4(10) . . . . ?
C23B N29B N30B C31B 177.8(7) . . . . ?
C23B N29B C33B C32B -177.9(8) . . . . ?
N24B C19B C20B C21B -179.7(8) . . . . ?
N24B N25B C26B C27B 1.8(8) . . . . ?
N25B N24B C28B C27B 4.6(10) . . . . ?
N25B C26B C27B C28B 0.9(7) . . . . ?
C26B C27B C28B N24B -3.2(8) . . . . ?
C28B N24B N25B Ni1 170.5(6) . . . . ?
C28B N24B N25B C26B -4.0(9) . . . . ?
N29B N30B C31B C32B 1.1(8) . . . . ?
N30B N29B C33B C32B 1.2(8) . . . . ?
N30B C31B C32B C33B -0.4(7) . . . . ?
C31B C32B C33B N29B -0.5(7) . . . . ?
C33B N29B N30B Ni1 179.4(6) . . . . ?
C33B N29B N30B C31B -1.5(9) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.943(10)
2 0.057(10)

_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_pg14mt
_database_code_depnum_ccdc_archive 'CCDC 2261790'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2023-05-09 deposited with the CCDC.	2023-08-30 downloaded from the CCDC.
;
_audit_creation_date             2023-03-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis[2,6-di(pyrazol-1-yl)pyridine]iron(II) bis[2,6-di(pyrazol-1-yl)pyridine]-ruthenium(II) ditetrafluoroborate 0.50:0.50 solid solution'
_chemical_formula_moiety         
'0.5(C22 H18 Fe N10), 0.5(C22 H18 N10 Ru), 2(B F4)'
_chemical_formula_sum            'C22 H18 B2 F8 Fe0.50 N10 Ru0.50'
_chemical_formula_weight         674.54
_chemical_absolute_configuration ab
_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 0.0019 0.0015 '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 0.0004 0.0006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0124 0.0097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.2961 0.8007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0037 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.5177 0.7911 '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           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   8.4842(1)
_cell_length_b                   8.5569(1)
_cell_length_c                   18.4642(1)
_cell_angle_alpha                90
_cell_angle_beta                 97.843(1)
_cell_angle_gamma                90
_cell_volume                     1327.93(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    17723
_cell_measurement_temperature    200.15
_cell_measurement_theta_max      35.29
_cell_measurement_theta_min      1.08
_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_T_min  0.946
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
DIALS 3.12.1-2-g1c07bc2b3-release
Scaling & analysis of unmerged intensities, absorption correction using 
spherical harmonics
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             674
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            30473
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        24.620
_diffrn_reflns_theta_max         36.084
_diffrn_reflns_theta_min         1.079
_diffrn_ambient_temperature      200.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.934
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_measurement_device       'Fixed χ 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_reflns_Friedel_coverage         0.821
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.850
_reflns_number_gt                10877
_reflns_number_total             12455
_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       'XIA2 0.4.0.438-g4431aaa (Winter, 2010)'
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction        'XIA2 0.4.0.438-g4431aaa (Winter, 2010)'
_computing_molecular_graphics    'XSEED (Barbour, 2020)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 
;
 Flack x determined using 3869 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.036(12)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         12455
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0454
_refine_ls_restrained_S_all      1.034
_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)+(0.0345P)²+0.4434P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1025
_refine_special_details          
;
 In this refinement, the 200 K temperature dataset was treated as a single, 
 averaged [FeₓRu₁₋ₓ(bpp)₂]2+ cation site. Partial Fe and Ru atoms
 were refined with the same cartesian coordinates, using the Fe~0.50~/
 Ru~0.50~ occupancy ratio obtained from the disordered refinement model 
 at 100 K. No anion disorder is included in the model. However, 
 an EADP thermal parameter constraint between the two partial metal atoms 
 was required to make the model converge.

 All 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
2. Uiso/Uaniso restraints and constraints
Uanis(Fe1) = Uanis(Ru1)
3. Others
 X(Fe1)=X(Ru1)=FVAR(1)
 Y(Fe1)=Y(Ru1)=FVAR(2)
 Z(Fe1)=Z(Ru1)=FVAR(3)
 Fixed Sof: Fe1(0.5) Ru1(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16),
 C17(H17), C20(H20), C21(H21), C22(H22), C26(H26), C27(H27), C28(H28), C31(H31),
  C32(H32), C33(H33)
;
_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 0.71691(3) 0.81279(3) 0.74661(2) 0.02420(6) Uani 0.5 1 d . . P A 1
Ru1 Ru 0.71691(3) 0.81279(3) 0.74661(2) 0.02420(6) Uani 0.5 1 d . . P A 2
N2 N 0.7118(3) 0.8315(3) 0.64146(12) 0.0259(5) Uani 1 1 d . . . . .
C3 C 0.5838(3) 0.8911(3) 0.60040(15) 0.0287(5) Uani 1 1 d . . . . .
C4 C 0.5740(4) 0.9041(4) 0.52545(16) 0.0353(6) Uani 1 1 d . . . . .
H4 H 0.482490 0.946316 0.496716 0.042 Uiso 1 1 calc R U . . .
C5 C 0.7041(5) 0.8527(4) 0.49406(17) 0.0390(7) Uani 1 1 d . . . . .
H5 H 0.701563 0.861167 0.442615 0.047 Uiso 1 1 calc R U . . .
C6 C 0.8379(4) 0.7892(4) 0.53531(16) 0.0349(7) Uani 1 1 d . . . . .
H6 H 0.926603 0.753651 0.513541 0.042 Uiso 1 1 calc R U . . .
C7 C 0.8347(3) 0.7807(3) 0.60952(15) 0.0290(6) Uani 1 1 d . . . . .
N8 N 0.4667(3) 0.9337(3) 0.64355(14) 0.0298(5) Uani 1 1 d . . . . .
N9 N 0.4986(3) 0.9080(3) 0.71791(13) 0.0283(4) Uani 1 1 d . . . . .
C10 C 0.3697(4) 0.9560(4) 0.7447(2) 0.0358(6) Uani 1 1 d . . . . .
H10 H 0.356164 0.951726 0.794880 0.043 Uiso 1 1 calc R U . . .
C11 C 0.2555(4) 1.0141(4) 0.6886(2) 0.0412(7) Uani 1 1 d . . . . .
H11 H 0.154082 1.056146 0.693972 0.049 Uiso 1 1 calc R U . . .
C12 C 0.3196(4) 0.9980(4) 0.6252(2) 0.0374(7) Uani 1 1 d . . . . .
H12 H 0.271140 1.026003 0.577497 0.045 Uiso 1 1 calc R U . . .
N13 N 0.9548(3) 0.7172(3) 0.66163(14) 0.0299(5) Uani 1 1 d . . . . .
N14 N 0.9297(3) 0.7224(3) 0.73392(13) 0.0297(5) Uani 1 1 d . . . . .
C15 C 1.0558(4) 0.6533(4) 0.77098(19) 0.0369(7) Uani 1 1 d . . . . .
H15 H 1.072815 0.640308 0.822554 0.044 Uiso 1 1 calc R U . . .
C16 C 1.1606(4) 0.6022(5) 0.7231(2) 0.0454(8) Uani 1 1 d . . . . .
H16 H 1.258829 0.549139 0.736011 0.054 Uiso 1 1 calc R U . . .
C17 C 1.0935(4) 0.6436(4) 0.6548(2) 0.0399(7) Uani 1 1 d . . . . .
H17 H 1.135832 0.624600 0.610591 0.048 Uiso 1 1 calc R U . . .
N18 N 0.7211(3) 0.7870(3) 0.85140(12) 0.0271(5) Uani 1 1 d . . . . .
C19 C 0.7798(3) 0.8991(4) 0.89750(15) 0.0281(5) Uani 1 1 d . . . . .
C20 C 0.7862(4) 0.8857(4) 0.97248(17) 0.0352(6) Uani 1 1 d . . . . .
H20 H 0.827351 0.967094 1.004643 0.042 Uiso 1 1 calc R U . . .
C21 C 0.7295(4) 0.7471(5) 0.99830(17) 0.0365(7) Uani 1 1 d . . . . .
H21 H 0.730980 0.734064 1.049479 0.044 Uiso 1 1 calc R U . . .
C22 C 0.6706(4) 0.6268(4) 0.95172(17) 0.0346(6) Uani 1 1 d . . . . .
H22 H 0.633906 0.531417 0.969742 0.042 Uiso 1 1 calc R U . . .
C23 C 0.6684(3) 0.6534(4) 0.87773(16) 0.0286(5) Uani 1 1 d . . . . .
N24 N 0.8323(3) 1.0273(3) 0.85969(13) 0.0300(5) Uani 1 1 d . . . . .
N25 N 0.8163(3) 1.0178(3) 0.78413(13) 0.0288(5) Uani 1 1 d . . . . .
C26 C 0.8822(4) 1.1477(4) 0.76304(18) 0.0350(6) Uani 1 1 d . . . . .
H26 H 0.887725 1.175069 0.713597 0.042 Uiso 1 1 calc R U . . .
C27 C 0.9428(4) 1.2394(4) 0.8238(2) 0.0414(7) Uani 1 1 d . . . . .
H27 H 0.996367 1.336772 0.823120 0.050 Uiso 1 1 calc R U . . .
C28 C 0.9090(4) 1.1599(4) 0.8837(2) 0.0390(7) Uani 1 1 d . . . . .
H28 H 0.934538 1.191679 0.933153 0.047 Uiso 1 1 calc R U . . .
N29 N 0.6139(3) 0.5493(3) 0.82091(14) 0.0302(5) Uani 1 1 d . . . . .
N30 N 0.6260(3) 0.5957(3) 0.75051(13) 0.0292(5) Uani 1 1 d . . . . .
C31 C 0.5780(4) 0.4743(4) 0.70896(19) 0.0361(6) Uani 1 1 d . . . . .
H31 H 0.574692 0.471550 0.657336 0.043 Uiso 1 1 calc R U . . .
C32 C 0.5326(4) 0.3505(4) 0.7509(2) 0.0428(8) Uani 1 1 d . . . . .
H32 H 0.492699 0.251544 0.733788 0.051 Uiso 1 1 calc R U . . .
C33 C 0.5575(4) 0.4011(4) 0.8218(2) 0.0398(7) Uani 1 1 d . . . . .
H33 H 0.538874 0.343394 0.863772 0.048 Uiso 1 1 calc R U . . .
B34 B 0.7989(5) 0.2747(5) 0.5633(2) 0.0404(8) Uani 1 1 d . . . . .
F35 F 0.6787(3) 0.2253(3) 0.60187(12) 0.0489(5) Uani 1 1 d . . . . .
F36 F 0.7669(4) 0.2243(3) 0.49100(13) 0.0582(7) Uani 1 1 d . . . . .
F37 F 0.7991(4) 0.4366(3) 0.56273(15) 0.0642(7) Uani 1 1 d . . . . .
F38 F 0.9418(4) 0.2158(5) 0.59465(15) 0.0831(11) Uani 1 1 d . . . . .
B39 B 0.7217(6) 0.2562(6) 1.0580(2) 0.0448(9) Uani 1 1 d . . . . .
F40 F 0.6462(3) 0.2455(3) 0.98636(12) 0.0521(6) Uani 1 1 d . . . B 1
F41 F 0.6826(3) 0.1290(4) 1.09848(13) 0.0598(7) Uani 1 1 d . . . C 1
F42 F 0.8841(3) 0.2506(5) 1.05669(14) 0.0791(11) Uani 1 1 d . . . D 1
F43 F 0.6731(6) 0.3897(4) 1.08870(17) 0.1033(15) Uani 1 1 d . . . E 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 1.943(2) . ?
Fe1 N9 2.027(3) . ?
Fe1 N14 2.007(3) . ?
Fe1 N18 1.943(2) . ?
Fe1 N25 2.027(3) . ?
Fe1 N30 2.016(3) . ?
Ru1 N2 1.943(2) . ?
Ru1 N9 2.027(3) . ?
Ru1 N14 2.007(3) . ?
Ru1 N18 1.943(2) . ?
Ru1 N25 2.027(3) . ?
Ru1 N30 2.016(3) . ?
N2 C3 1.337(4) . ?
N2 C7 1.339(4) . ?
C3 C4 1.379(4) . ?
C3 N8 1.404(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.386(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.389(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.376(4) . ?
C7 N13 1.411(4) . ?
N8 N9 1.380(3) . ?
N8 C12 1.364(4) . ?
N9 C10 1.325(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.408(5) . ?
C11 H11 0.9500 . ?
C11 C12 1.365(5) . ?
C12 H12 0.9500 . ?
N13 N14 1.381(4) . ?
N13 C17 1.355(4) . ?
N14 C15 1.327(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.406(5) . ?
C16 H16 0.9500 . ?
C16 C17 1.358(5) . ?
C17 H17 0.9500 . ?
N18 C19 1.333(4) . ?
N18 C23 1.342(4) . ?
C19 C20 1.383(4) . ?
C19 N24 1.405(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.389(5) . ?
C21 H21 0.9500 . ?
C21 C22 1.390(5) . ?
C22 H22 0.9500 . ?
C22 C23 1.383(4) . ?
C23 N29 1.406(4) . ?
N24 N25 1.386(3) . ?
N24 C28 1.351(4) . ?
N25 C26 1.326(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.407(5) . ?
C27 H27 0.9500 . ?
C27 C28 1.362(5) . ?
C28 H28 0.9500 . ?
N29 N30 1.376(4) . ?
N29 C33 1.356(4) . ?
N30 C31 1.323(4) . ?
C31 H31 0.9500 . ?
C31 C32 1.397(5) . ?
C32 H32 0.9500 . ?
C32 C33 1.367(5) . ?
C33 H33 0.9500 . ?
B34 F35 1.388(5) . ?
B34 F36 1.393(5) . ?
B34 F37 1.385(5) . ?
B34 F38 1.367(5) . ?
B39 F40 1.391(5) . ?
B39 F41 1.386(5) . ?
B39 F42 1.382(5) . ?
B39 F43 1.364(6) . ?

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 79.07(10) . . ?
N2 Fe1 N14 79.22(10) . . ?
N2 Fe1 N18 178.20(13) . . ?
N2 Fe1 N25 102.81(11) . . ?
N2 Fe1 N30 98.93(11) . . ?
N9 Fe1 N25 93.68(10) . . ?
N14 Fe1 N9 158.27(10) . . ?
N14 Fe1 N25 91.99(11) . . ?
N14 Fe1 N30 90.21(11) . . ?
N18 Fe1 N9 101.43(10) . . ?
N18 Fe1 N14 100.24(10) . . ?
N18 Fe1 N25 78.91(10) . . ?
N18 Fe1 N30 79.33(10) . . ?
N30 Fe1 N9 92.25(10) . . ?
N30 Fe1 N25 158.18(10) . . ?
N2 Ru1 N9 79.07(10) . . ?
N2 Ru1 N14 79.22(10) . . ?
N2 Ru1 N18 178.20(13) . . ?
N2 Ru1 N25 102.81(11) . . ?
N2 Ru1 N30 98.93(11) . . ?
N9 Ru1 N25 93.68(10) . . ?
N14 Ru1 N9 158.27(10) . . ?
N14 Ru1 N25 91.99(11) . . ?
N14 Ru1 N30 90.21(11) . . ?
N18 Ru1 N9 101.43(10) . . ?
N18 Ru1 N14 100.24(10) . . ?
N18 Ru1 N25 78.91(10) . . ?
N18 Ru1 N30 79.33(10) . . ?
N30 Ru1 N9 92.25(10) . . ?
N30 Ru1 N25 158.18(10) . . ?
C3 N2 Fe1 120.3(2) . . ?
C3 N2 Ru1 120.3(2) . . ?
C3 N2 C7 119.7(2) . . ?
C7 N2 Fe1 120.05(19) . . ?
C7 N2 Ru1 120.05(19) . . ?
N2 C3 C4 122.2(3) . . ?
N2 C3 N8 111.1(2) . . ?
C4 C3 N8 126.7(3) . . ?
C3 C4 H4 121.6 . . ?
C3 C4 C5 116.8(3) . . ?
C5 C4 H4 121.6 . . ?
C4 C5 H5 118.9 . . ?
C4 C5 C6 122.2(3) . . ?
C6 C5 H5 118.9 . . ?
C5 C6 H6 121.9 . . ?
C7 C6 C5 116.2(3) . . ?
C7 C6 H6 121.9 . . ?
N2 C7 C6 122.9(3) . . ?
N2 C7 N13 111.0(2) . . ?
C6 C7 N13 126.1(3) . . ?
N9 N8 C3 117.7(2) . . ?
C12 N8 C3 131.2(3) . . ?
C12 N8 N9 111.1(3) . . ?
N8 N9 Fe1 111.86(18) . . ?
N8 N9 Ru1 111.86(18) . . ?
C10 N9 Fe1 143.0(2) . . ?
C10 N9 Ru1 143.0(2) . . ?
C10 N9 N8 105.2(3) . . ?
N9 C10 H10 124.6 . . ?
N9 C10 C11 110.8(3) . . ?
C11 C10 H10 124.6 . . ?
C10 C11 H11 126.9 . . ?
C12 C11 C10 106.3(3) . . ?
C12 C11 H11 126.9 . . ?
N8 C12 C11 106.6(3) . . ?
N8 C12 H12 126.7 . . ?
C11 C12 H12 126.7 . . ?
N14 N13 C7 117.0(2) . . ?
C17 N13 C7 132.1(3) . . ?
C17 N13 N14 110.8(3) . . ?
N13 N14 Fe1 112.65(18) . . ?
N13 N14 Ru1 112.65(18) . . ?
C15 N14 Fe1 141.8(2) . . ?
C15 N14 Ru1 141.8(2) . . ?
C15 N14 N13 105.3(3) . . ?
N14 C15 H15 124.8 . . ?
N14 C15 C16 110.4(3) . . ?
C16 C15 H15 124.8 . . ?
C15 C16 H16 126.8 . . ?
C17 C16 C15 106.3(3) . . ?
C17 C16 H16 126.8 . . ?
N13 C17 C16 107.1(3) . . ?
N13 C17 H17 126.4 . . ?
C16 C17 H17 126.4 . . ?
C19 N18 Fe1 120.6(2) . . ?
C19 N18 Ru1 120.6(2) . . ?
C19 N18 C23 119.7(2) . . ?
C23 N18 Fe1 119.7(2) . . ?
C23 N18 Ru1 119.7(2) . . ?
N18 C19 C20 122.7(3) . . ?
N18 C19 N24 111.2(2) . . ?
C20 C19 N24 126.2(3) . . ?
C19 C20 H20 121.8 . . ?
C19 C20 C21 116.5(3) . . ?
C21 C20 H20 121.8 . . ?
C20 C21 H21 118.9 . . ?
C20 C21 C22 122.2(3) . . ?
C22 C21 H21 118.9 . . ?
C21 C22 H22 121.8 . . ?
C23 C22 C21 116.4(3) . . ?
C23 C22 H22 121.8 . . ?
N18 C23 C22 122.5(3) . . ?
N18 C23 N29 111.2(2) . . ?
C22 C23 N29 126.3(3) . . ?
N25 N24 C19 117.4(2) . . ?
C28 N24 C19 131.6(3) . . ?
C28 N24 N25 110.8(3) . . ?
N24 N25 Fe1 111.99(19) . . ?
N24 N25 Ru1 111.99(19) . . ?
C26 N25 Fe1 142.9(2) . . ?
C26 N25 Ru1 142.9(2) . . ?
C26 N25 N24 105.0(3) . . ?
N25 C26 H26 124.6 . . ?
N25 C26 C27 110.9(3) . . ?
C27 C26 H26 124.6 . . ?
C26 C27 H27 127.1 . . ?
C28 C27 C26 105.9(3) . . ?
C28 C27 H27 127.1 . . ?
N24 C28 C27 107.4(3) . . ?
N24 C28 H28 126.3 . . ?
C27 C28 H28 126.3 . . ?
N30 N29 C23 117.5(2) . . ?
C33 N29 C23 131.6(3) . . ?
C33 N29 N30 110.7(3) . . ?
N29 N30 Fe1 112.21(18) . . ?
N29 N30 Ru1 112.21(18) . . ?
C31 N30 Fe1 142.4(2) . . ?
C31 N30 Ru1 142.4(2) . . ?
C31 N30 N29 105.3(3) . . ?
N30 C31 H31 124.4 . . ?
N30 C31 C32 111.1(3) . . ?
C32 C31 H31 124.4 . . ?
C31 C32 H32 127.1 . . ?
C33 C32 C31 105.8(3) . . ?
C33 C32 H32 127.1 . . ?
N29 C33 C32 107.0(3) . . ?
N29 C33 H33 126.5 . . ?
C32 C33 H33 126.5 . . ?
F35 B34 F36 109.7(3) . . ?
F37 B34 F35 108.0(3) . . ?
F37 B34 F36 107.6(3) . . ?
F38 B34 F35 109.9(3) . . ?
F38 B34 F36 109.7(3) . . ?
F38 B34 F37 111.8(4) . . ?
F41 B39 F40 110.4(4) . . ?
F42 B39 F40 108.2(3) . . ?
F42 B39 F41 107.2(4) . . ?
F43 B39 F40 108.9(4) . . ?
F43 B39 F41 109.0(3) . . ?
F43 B39 F42 113.2(4) . . ?

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 -178.9(2) . . . . ?
Fe1 N2 C3 N8 0.3(3) . . . . ?
Fe1 N2 C7 C6 179.4(2) . . . . ?
Fe1 N2 C7 N13 0.3(3) . . . . ?
Fe1 N9 C10 C11 179.8(3) . . . . ?
Fe1 N14 C15 C16 173.0(3) . . . . ?
Fe1 N18 C19 C20 -179.6(2) . . . . ?
Fe1 N18 C19 N24 0.2(3) . . . . ?
Fe1 N18 C23 C22 178.9(2) . . . . ?
Fe1 N18 C23 N29 -0.8(3) . . . . ?
Fe1 N25 C26 C27 -173.7(3) . . . . ?
Fe1 N30 C31 C32 176.9(3) . . . . ?
Ru1 N2 C3 C4 -178.9(2) . . . . ?
Ru1 N2 C3 N8 0.3(3) . . . . ?
Ru1 N2 C7 C6 179.4(2) . . . . ?
Ru1 N2 C7 N13 0.3(3) . . . . ?
Ru1 N9 C10 C11 179.8(3) . . . . ?
Ru1 N14 C15 C16 173.0(3) . . . . ?
Ru1 N18 C19 C20 -179.6(2) . . . . ?
Ru1 N18 C19 N24 0.2(3) . . . . ?
Ru1 N18 C23 C22 178.9(2) . . . . ?
Ru1 N18 C23 N29 -0.8(3) . . . . ?
Ru1 N25 C26 C27 -173.7(3) . . . . ?
Ru1 N30 C31 C32 176.9(3) . . . . ?
N2 C3 C4 C5 -0.2(5) . . . . ?
N2 C3 N8 N9 -0.5(4) . . . . ?
N2 C3 N8 C12 180.0(3) . . . . ?
N2 C7 N13 N14 -2.1(4) . . . . ?
N2 C7 N13 C17 175.0(3) . . . . ?
C3 N2 C7 C6 1.3(5) . . . . ?
C3 N2 C7 N13 -177.8(3) . . . . ?
C3 C4 C5 C6 0.7(5) . . . . ?
C3 N8 N9 Fe1 0.5(3) . . . . ?
C3 N8 N9 Ru1 0.5(3) . . . . ?
C3 N8 N9 C10 -179.2(3) . . . . ?
C3 N8 C12 C11 179.6(3) . . . . ?
C4 C3 N8 N9 178.6(3) . . . . ?
C4 C3 N8 C12 -0.9(5) . . . . ?
C4 C5 C6 C7 -0.3(5) . . . . ?
C5 C6 C7 N2 -0.7(5) . . . . ?
C5 C6 C7 N13 178.2(3) . . . . ?
C6 C7 N13 N14 178.9(3) . . . . ?
C6 C7 N13 C17 -4.1(5) . . . . ?
C7 N2 C3 C4 -0.8(5) . . . . ?
C7 N2 C3 N8 178.4(3) . . . . ?
C7 N13 N14 Fe1 2.8(3) . . . . ?
C7 N13 N14 Ru1 2.8(3) . . . . ?
C7 N13 N14 C15 178.6(3) . . . . ?
C7 N13 C17 C16 -178.0(3) . . . . ?
N8 C3 C4 C5 -179.2(3) . . . . ?
N8 N9 C10 C11 -0.7(4) . . . . ?
N9 N8 C12 C11 0.0(4) . . . . ?
N9 C10 C11 C12 0.7(4) . . . . ?
C10 C11 C12 N8 -0.4(4) . . . . ?
C12 N8 N9 Fe1 -179.9(2) . . . . ?
C12 N8 N9 Ru1 -179.9(2) . . . . ?
C12 N8 N9 C10 0.4(3) . . . . ?
N13 N14 C15 C16 -0.7(4) . . . . ?
N14 N13 C17 C16 -0.8(4) . . . . ?
N14 C15 C16 C17 0.3(4) . . . . ?
C15 C16 C17 N13 0.3(4) . . . . ?
C17 N13 N14 Fe1 -174.8(2) . . . . ?
C17 N13 N14 Ru1 -174.8(2) . . . . ?
C17 N13 N14 C15 0.9(4) . . . . ?
N18 C19 C20 C21 0.7(5) . . . . ?
N18 C19 N24 N25 -0.1(4) . . . . ?
N18 C19 N24 C28 -174.6(3) . . . . ?
N18 C23 N29 N30 1.6(4) . . . . ?
N18 C23 N29 C33 176.9(3) . . . . ?
C19 N18 C23 C22 0.7(4) . . . . ?
C19 N18 C23 N29 -179.0(2) . . . . ?
C19 C20 C21 C22 0.7(5) . . . . ?
C19 N24 N25 Fe1 0.0(3) . . . . ?
C19 N24 N25 Ru1 0.0(3) . . . . ?
C19 N24 N25 C26 -176.5(3) . . . . ?
C19 N24 C28 C27 175.3(3) . . . . ?
C20 C19 N24 N25 179.6(3) . . . . ?
C20 C19 N24 C28 5.1(5) . . . . ?
C20 C21 C22 C23 -1.2(5) . . . . ?
C21 C22 C23 N18 0.6(4) . . . . ?
C21 C22 C23 N29 -179.8(3) . . . . ?
C22 C23 N29 N30 -178.1(3) . . . . ?
C22 C23 N29 C33 -2.8(5) . . . . ?
C23 N18 C19 C20 -1.3(4) . . . . ?
C23 N18 C19 N24 178.4(2) . . . . ?
C23 N29 N30 Fe1 -1.7(3) . . . . ?
C23 N29 N30 Ru1 -1.7(3) . . . . ?
C23 N29 N30 C31 175.7(3) . . . . ?
C23 N29 C33 C32 -175.5(3) . . . . ?
N24 C19 C20 C21 -179.1(3) . . . . ?
N24 N25 C26 C27 1.0(4) . . . . ?
N25 N24 C28 C27 0.5(4) . . . . ?
N25 C26 C27 C28 -0.7(4) . . . . ?
C26 C27 C28 N24 0.1(4) . . . . ?
C28 N24 N25 Fe1 175.6(2) . . . . ?
C28 N24 N25 Ru1 175.6(2) . . . . ?
C28 N24 N25 C26 -0.9(3) . . . . ?
N29 N30 C31 C32 0.9(4) . . . . ?
N30 N29 C33 C32 0.0(4) . . . . ?
N30 C31 C32 C33 -0.9(4) . . . . ?
C31 C32 C33 N29 0.5(4) . . . . ?
C33 N29 N30 Fe1 -177.9(2) . . . . ?
C33 N29 N30 Ru1 -177.9(2) . . . . ?
C33 N29 N30 C31 -0.5(3) . . . . ?

_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_pg14ltd
_database_code_depnum_ccdc_archive 'CCDC 2261792'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2023-05-09 deposited with the CCDC.	2023-08-30 downloaded from the CCDC.
;
_audit_creation_date             2023-03-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis[2,6-di(pyrazol-1-yl)pyridine]iron(II) bis[2,6-di(pyrazol-1-yl)pyridine]-ruthenium(II) ditetrafluoroborate 0.50:0.50 solid solution (disordered refinement)'
_chemical_formula_moiety         
'0.5(C22 H18 Fe N10), 0.5(C22 H18 N10 Ru), 2(B F4)'
_chemical_formula_sum            'C22 H18 B2 F8 Fe0.50 N10 Ru0.50'
_chemical_formula_weight         674.54
_chemical_absolute_configuration ab
_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 0.0019 0.0015 '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 0.0004 0.0006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0124 0.0097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.2961 0.8007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0037 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.5177 0.7911 '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           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   8.4455(1)
_cell_length_b                   8.5114(1)
_cell_length_c                   18.4035(1)
_cell_angle_alpha                90
_cell_angle_beta                 98.071(1)
_cell_angle_gamma                90
_cell_volume                     1309.80(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    18949
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      35.72
_cell_measurement_theta_min      1.08
_exptl_absorpt_coefficient_mu    0.629
_exptl_absorpt_correction_T_min  0.901
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
DIALS 3.12.1-2-g1c07bc2b3-release
Scaling & analysis of unmerged intensities, absorption correction using 
spherical harmonics
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             674
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_unetI/netI     0.0735
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            30093
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        24.620
_diffrn_reflns_theta_max         36.110
_diffrn_reflns_theta_min         1.083
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.931
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_measurement_device       'Fixed χ 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_reflns_Friedel_coverage         0.819
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.846
_reflns_number_gt                11034
_reflns_number_total             12266
_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       'XIA2 0.4.0.438-g4431aaa (Winter, 2010)'
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction        'XIA2 0.4.0.438-g4431aaa (Winter, 2010)'
_computing_molecular_graphics    'XSEED (Barbour, 2020)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 
;
 Flack x determined using 3838 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(12)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         12266
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0439
_refine_ls_restrained_S_all      1.037
_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)+(0.0203P)²+0.6386P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0891
_refine_special_details          
;
 Following an initial structure solution, discrete partial (low-spin) 
 [Fe(bpp)₂]2+ and [Ru(bpp)₂]2+ molecule sites were constructed and 
 refined without restraints. The Fe:Ru occupancy ratio refined to 0.50:0.50, 
 so those occupancies were used for those disorder sites in the final least 
 squares cycles. No anion disorder is included in the model. However SIMU 
 restraints were also applied to C3A/C3B, C7A/C7B and C19A/C19B, whose 
 Uiso values tended to correlate with each other.

 The Fe, Ru, B and F atoms were refined anisotropically. Attempts to refine
 the partial N atoms anisotropically led to them becoming non-positive 
 definite, so they were left isotropic in the final least squares cycles. 
 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
2. Uiso/Uaniso restraints and constraints
C3A \\sim C3B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C7A \\sim C7B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C19A \\sim C19B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
3. Others
 Fixed Sof: Fe1(0.5) N2A(0.5) C3A(0.5) C4A(0.5) H4A(0.5) C5A(0.5) H5A(0.5)
 C6A(0.5) H6A(0.5) C7A(0.5) N8A(0.5) N9A(0.5) C10A(0.5) H10A(0.5) C11A(0.5)
 H11A(0.5) C12A(0.5) H12A(0.5) N13A(0.5) N14A(0.5) C15A(0.5) H15A(0.5)
 C16A(0.5) H16A(0.5) C17A(0.5) H17A(0.5) N18A(0.5) C19A(0.5) C20A(0.5)
 H20A(0.5) C21A(0.5) H21A(0.5) C22A(0.5) H22A(0.5) C23A(0.5) N24A(0.5)
 N25A(0.5) C26A(0.5) H26A(0.5) C27A(0.5) H27A(0.5) C28A(0.5) H28A(0.5)
 N29A(0.5) N30A(0.5) C31A(0.5) H31A(0.5) C32A(0.5) H32A(0.5) C33A(0.5)
 H33A(0.5) Ru1(0.5) N2B(0.5) C3B(0.5) C4B(0.5) H4B(0.5) C5B(0.5) H5B(0.5)
 C6B(0.5) H6B(0.5) C7B(0.5) N8B(0.5) N9B(0.5) C10B(0.5) H10B(0.5) C11B(0.5)
 H11B(0.5) C12B(0.5) H12B(0.5) N13B(0.5) N14B(0.5) C15B(0.5) H15B(0.5)
 C16B(0.5) H16B(0.5) C17B(0.5) H17B(0.5) N18B(0.5) C19B(0.5) C20B(0.5)
 H20B(0.5) C21B(0.5) H21B(0.5) C22B(0.5) H22B(0.5) C23B(0.5) N24B(0.5)
 N25B(0.5) C26B(0.5) H26B(0.5) C27B(0.5) H27B(0.5) C28B(0.5) H28B(0.5)
 N29B(0.5) N30B(0.5) C31B(0.5) H31B(0.5) C32B(0.5) H32B(0.5) C33B(0.5) H33B(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C5A(H5A), C6A(H6A), C10A(H10A), C11A(H11A), C12A(H12A), C15A(H15A),
 C16A(H16A), C17A(H17A), C20A(H20A), C21A(H21A), C22A(H22A), C26A(H26A),
 C27A(H27A), C28A(H28A), C31A(H31A), C32A(H32A), C33A(H33A), C4B(H4B), C5B(H5B),
  C6B(H6B), C10B(H10B), C11B(H11B), C12B(H12B), C15B(H15B), C16B(H16B),
 C17B(H17B), C20B(H20B), C21B(H21B), C22B(H22B), C26B(H26B), C27B(H27B),
 C28B(H28B), C31B(H31B), C32B(H32B), C33B(H33B)
;
_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 0.7165(4) 0.8414(6) 0.74660(17) 0.0124(11) Uani 0.5 1 d . . P A 1
N2A N 0.7115(13) 0.8656(15) 0.6428(6) 0.017(3) Uiso 0.5 1 d . . P A 1
C3A C 0.580(2) 0.924(2) 0.5994(10) 0.0154(9) Uiso 0.5 1 d . U P A 1
C4A C 0.5657(10) 0.9360(11) 0.5241(4) 0.0126(17) Uiso 0.5 1 d . . P A 1
H4A H 0.471382 0.975637 0.495826 0.015 Uiso 0.5 1 calc R U P A 1
C5A C 0.6967(11) 0.8876(11) 0.4917(5) 0.0174(19) Uiso 0.5 1 d . . P A 1
H5A H 0.693478 0.899447 0.440209 0.021 Uiso 0.5 1 calc R U P A 1
C6A C 0.8319(11) 0.8226(14) 0.5321(5) 0.019(2) Uiso 0.5 1 d . . P A 1
H6A H 0.918872 0.785384 0.509273 0.023 Uiso 0.5 1 calc R U P A 1
C7A C 0.8334(15) 0.8147(16) 0.6085(7) 0.0155(9) Uiso 0.5 1 d . U P A 1
N8A N 0.4697(11) 0.9674(12) 0.6411(5) 0.012(2) Uiso 0.5 1 d . . P A 1
N9A N 0.5027(12) 0.9345(14) 0.7183(6) 0.015(2) Uiso 0.5 1 d . . P A 1
C10A C 0.3698(10) 0.9801(11) 0.7466(5) 0.0146(18) Uiso 0.5 1 d . . P A 1
H10A H 0.357844 0.972571 0.797004 0.018 Uiso 0.5 1 calc R U P A 1
C11A C 0.2518(9) 1.0400(10) 0.6917(4) 0.0169(15) Uiso 0.5 1 d . . P A 1
H11A H 0.150712 1.082431 0.698168 0.020 Uiso 0.5 1 calc R U P A 1
C12A C 0.3132(11) 1.0244(12) 0.6275(5) 0.020(2) Uiso 0.5 1 d . . P A 1
H12A H 0.257585 1.048746 0.580324 0.024 Uiso 0.5 1 calc R U P A 1
N13A N 0.9577(12) 0.7441(13) 0.6641(6) 0.011(2) Uiso 0.5 1 d . . P A 1
N14A N 0.9268(13) 0.7562(14) 0.7354(6) 0.020(3) Uiso 0.5 1 d . . P A 1
C15A C 1.0530(9) 0.6823(10) 0.7756(4) 0.0139(15) Uiso 0.5 1 d . . P A 1
H15A H 1.064692 0.667236 0.827251 0.017 Uiso 0.5 1 calc R U P A 1
C16A C 1.1640(10) 0.6312(11) 0.7300(5) 0.0204(17) Uiso 0.5 1 d . . P A 1
H16A H 1.262015 0.577829 0.744773 0.024 Uiso 0.5 1 calc R U P A 1
C17A C 1.1017(10) 0.6740(11) 0.6607(5) 0.0208(19) Uiso 0.5 1 d . . P A 1
H17A H 1.149857 0.657875 0.617692 0.025 Uiso 0.5 1 calc R U P A 1
N18A N 0.7194(9) 0.8060(11) 0.8523(4) 0.0115(16) Uiso 0.5 1 d . . P A 1
C19A C 0.7783(16) 0.9211(13) 0.8986(7) 0.0147(9) Uiso 0.5 1 d . U P A 1
C20A C 0.7836(12) 0.9018(12) 0.9740(5) 0.018(2) Uiso 0.5 1 d . . P A 1
H20A H 0.825125 0.981474 1.007549 0.022 Uiso 0.5 1 calc R U P A 1
C21A C 0.7257(10) 0.7617(11) 0.9983(5) 0.0166(18) Uiso 0.5 1 d . . P A 1
H21A H 0.724665 0.746875 1.049351 0.020 Uiso 0.5 1 calc R U P A 1
C22A C 0.6687(11) 0.6418(11) 0.9497(5) 0.018(2) Uiso 0.5 1 d . . P A 1
H22A H 0.634054 0.543687 0.966434 0.022 Uiso 0.5 1 calc R U P A 1
C23A C 0.6659(13) 0.6738(14) 0.8770(6) 0.012(2) Uiso 0.5 1 d . . P A 1
N24A N 0.8264(13) 1.0598(15) 0.8604(6) 0.015(3) Uiso 0.5 1 d . . P A 1
N25A N 0.8133(9) 1.0386(9) 0.7842(4) 0.0140(18) Uiso 0.5 1 d . . P A 1
C26A C 0.8784(10) 1.1706(11) 0.7604(5) 0.0184(19) Uiso 0.5 1 d . . P A 1
H26A H 0.882029 1.194741 0.710287 0.022 Uiso 0.5 1 calc R U P A 1
C27A C 0.9421(15) 1.2706(17) 0.8214(6) 0.023(3) Uiso 0.5 1 d . . P A 1
H27A H 0.997827 1.366989 0.818832 0.027 Uiso 0.5 1 calc R U P A 1
C28A C 0.9059(12) 1.1982(12) 0.8832(6) 0.020(2) Uiso 0.5 1 d . . P A 1
H28A H 0.930285 1.235184 0.932227 0.024 Uiso 0.5 1 calc R U P A 1
N29A N 0.6117(14) 0.5725(15) 0.8178(6) 0.016(3) Uiso 0.5 1 d . . P A 1
N30A N 0.6270(14) 0.6302(13) 0.7489(6) 0.018(3) Uiso 0.5 1 d . . P A 1
C31A C 0.5786(9) 0.5067(10) 0.7042(4) 0.0131(16) Uiso 0.5 1 d . . P A 1
H31A H 0.575417 0.508263 0.652368 0.016 Uiso 0.5 1 calc R U P A 1
C32A C 0.5342(8) 0.3774(9) 0.7435(4) 0.0189(15) Uiso 0.5 1 d . . P A 1
H32A H 0.497306 0.278229 0.724371 0.023 Uiso 0.5 1 calc R U P A 1
C33A C 0.5551(10) 0.4239(11) 0.8154(5) 0.0207(19) Uiso 0.5 1 d . . P A 1
H33A H 0.533697 0.362814 0.856129 0.025 Uiso 0.5 1 calc R U P A 1
Ru1 Ru 0.7170(2) 0.8414(2) 0.74630(9) 0.0117(5) Uani 0.5 1 d . . P B 2
N2B N 0.7136(11) 0.8555(15) 0.6389(5) 0.011(2) Uiso 0.5 1 d . . P B 2
C3B C 0.586(2) 0.916(2) 0.5986(10) 0.0158(9) Uiso 0.5 1 d . U P B 2
C4B C 0.5838(11) 0.9292(13) 0.5223(5) 0.021(2) Uiso 0.5 1 d . . P B 2
H4B H 0.494414 0.973433 0.492103 0.025 Uiso 0.5 1 calc R U P B 2
C5B C 0.7151(10) 0.8761(11) 0.4927(5) 0.019(2) Uiso 0.5 1 d . . P B 2
H5B H 0.714498 0.882291 0.441140 0.022 Uiso 0.5 1 calc R U P B 2
C6B C 0.8477(11) 0.8140(12) 0.5359(5) 0.0151(19) Uiso 0.5 1 d . . P B 2
H6B H 0.939012 0.780030 0.515402 0.018 Uiso 0.5 1 calc R U P B 2
C7B C 0.8407(15) 0.8040(16) 0.6098(7) 0.0150(8) Uiso 0.5 1 d . U P B 2
N8B N 0.4605(13) 0.9557(13) 0.6424(6) 0.018(3) Uiso 0.5 1 d . . P B 2
N9B N 0.4906(12) 0.9381(14) 0.7149(6) 0.015(2) Uiso 0.5 1 d . . P B 2
C10B C 0.3603(12) 0.9890(13) 0.7387(5) 0.020(2) Uiso 0.5 1 d . . P B 2
H10B H 0.342924 0.988559 0.788607 0.024 Uiso 0.5 1 calc R U P B 2
C11B C 0.2502(10) 1.0441(11) 0.6798(5) 0.0210(18) Uiso 0.5 1 d . . P B 2
H11B H 0.146664 1.085193 0.682549 0.025 Uiso 0.5 1 calc R U P B 2
C12B C 0.3204(9) 1.0273(11) 0.6180(5) 0.0152(17) Uiso 0.5 1 d . . P B 2
H12B H 0.280329 1.058566 0.569375 0.018 Uiso 0.5 1 calc R U P B 2
N13B N 0.9551(15) 0.7470(17) 0.6585(6) 0.021(3) Uiso 0.5 1 d . . P B 2
N14B N 0.9357(11) 0.7466(12) 0.7333(5) 0.0105(19) Uiso 0.5 1 d . . P B 2
C15B C 1.0637(10) 0.6780(12) 0.7664(5) 0.021(2) Uiso 0.5 1 d . . P B 2
H15B H 1.085931 0.665019 0.818052 0.025 Uiso 0.5 1 calc R U P B 2
C16B C 1.1640(10) 0.6258(11) 0.7178(5) 0.0219(18) Uiso 0.5 1 d . . P B 2
H16B H 1.262527 0.571486 0.729513 0.026 Uiso 0.5 1 calc R U P B 2
C17B C 1.0915(9) 0.6690(10) 0.6499(4) 0.0150(15) Uiso 0.5 1 d . . P B 2
H17B H 1.129574 0.648229 0.604640 0.018 Uiso 0.5 1 calc R U P B 2
N18B N 0.7217(10) 0.8248(14) 0.8517(5) 0.018(2) Uiso 0.5 1 d . . P B 2
C19B C 0.7809(16) 0.9346(14) 0.8984(7) 0.0149(9) Uiso 0.5 1 d . U P B 2
C20B C 0.7884(10) 0.9227(11) 0.9737(5) 0.0141(18) Uiso 0.5 1 d . . P B 2
H20B H 0.829263 1.005673 1.005380 0.017 Uiso 0.5 1 calc R U P B 2
C21B C 0.7334(10) 0.7841(11) 1.0007(5) 0.0161(18) Uiso 0.5 1 d . . P B 2
H21B H 0.737570 0.771857 1.052271 0.019 Uiso 0.5 1 calc R U P B 2
C22B C 0.6723(10) 0.6626(11) 0.9547(5) 0.0154(18) Uiso 0.5 1 d . . P B 2
H22B H 0.634105 0.567896 0.973309 0.018 Uiso 0.5 1 calc R U P B 2
C23B C 0.6703(16) 0.6872(15) 0.8792(7) 0.019(3) Uiso 0.5 1 d . . P B 2
N24B N 0.8378(14) 1.0533(15) 0.8614(7) 0.017(3) Uiso 0.5 1 d . . P B 2
N25B N 0.8197(9) 1.0585(10) 0.7857(4) 0.0142(18) Uiso 0.5 1 d . . P B 2
C26B C 0.8891(10) 1.1859(10) 0.7679(5) 0.0152(17) Uiso 0.5 1 d . . P B 2
H26B H 0.898590 1.216370 0.719031 0.018 Uiso 0.5 1 calc R U P B 2
C27B C 0.9472(14) 1.2709(16) 0.8296(6) 0.021(2) Uiso 0.5 1 d . . P B 2
H27B H 0.999309 1.370058 0.831401 0.026 Uiso 0.5 1 calc R U P B 2
C28B C 0.9136(11) 1.1814(12) 0.8885(5) 0.017(2) Uiso 0.5 1 d . . P B 2
H28B H 0.939934 1.207145 0.939014 0.021 Uiso 0.5 1 calc R U P B 2
N29B N 0.6156(14) 0.5779(15) 0.8235(6) 0.017(3) Uiso 0.5 1 d . . P B 2
N30B N 0.6259(12) 0.6157(12) 0.7510(6) 0.013(2) Uiso 0.5 1 d . . P B 2
C31B C 0.5787(11) 0.4920(12) 0.7125(5) 0.022(2) Uiso 0.5 1 d . . P B 2
H31B H 0.575866 0.484606 0.660780 0.026 Uiso 0.5 1 calc R U P B 2
C32B C 0.5328(8) 0.3715(9) 0.7565(4) 0.0188(15) Uiso 0.5 1 d . . P B 2
H32B H 0.491573 0.271311 0.740864 0.023 Uiso 0.5 1 calc R U P B 2
C33B C 0.5595(9) 0.4275(10) 0.8270(4) 0.0156(15) Uiso 0.5 1 d . . P B 2
H33B H 0.542318 0.372421 0.870074 0.019 Uiso 0.5 1 calc R U P B 2
B34 B 0.7966(4) 0.3028(4) 0.56386(17) 0.0222(6) Uani 1 1 d . . . . .
F35 F 0.6775(2) 0.2500(2) 0.60282(10) 0.0260(4) Uani 1 1 d . . . . .
F36 F 0.7665(3) 0.2516(3) 0.49097(10) 0.0303(4) Uani 1 1 d . . . . .
F37 F 0.7976(3) 0.4671(3) 0.56411(11) 0.0315(4) Uani 1 1 d . . . . .
F38 F 0.9447(2) 0.2458(3) 0.59608(11) 0.0429(6) Uani 1 1 d . . . . .
B39 B 0.7174(4) 0.2797(5) 1.05723(17) 0.0241(6) Uani 1 1 d . . . . .
F40 F 0.6420(2) 0.2684(3) 0.98479(9) 0.0269(4) Uani 1 1 d . . . . .
F41 F 0.6816(2) 0.1489(3) 1.09746(10) 0.0295(4) Uani 1 1 d . . . . .
F42 F 0.8825(2) 0.2829(3) 1.05685(10) 0.0404(6) Uani 1 1 d . . . . .
F43 F 0.6652(4) 0.4141(3) 1.08894(12) 0.0505(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 N2A 1.915(11) . ?
Fe1 N9A 1.974(11) . ?
Fe1 N14A 1.956(11) . ?
Fe1 N18A 1.966(9) . ?
Fe1 N25A 1.951(9) . ?
Fe1 N30A 1.953(11) . ?
N2A C3A 1.37(2) . ?
N2A C7A 1.352(16) . ?
C3A C4A 1.378(19) . ?
C3A N8A 1.342(19) . ?
C4A H4A 0.9500 . ?
C4A C5A 1.391(13) . ?
C5A H5A 0.9500 . ?
C5A C6A 1.386(13) . ?
C6A H6A 0.9500 . ?
C6A C7A 1.407(15) . ?
C7A N13A 1.486(15) . ?
N8A N9A 1.438(14) . ?
N8A C12A 1.397(13) . ?
N9A C10A 1.358(14) . ?
C10A H10A 0.9500 . ?
C10A C11A 1.411(13) . ?
C11A H11A 0.9500 . ?
C11A C12A 1.361(12) . ?
C12A H12A 0.9500 . ?
N13A N14A 1.378(16) . ?
N13A C17A 1.364(14) . ?
N14A C15A 1.363(14) . ?
C15A H15A 0.9500 . ?
C15A C16A 1.411(12) . ?
C16A H16A 0.9500 . ?
C16A C17A 1.359(12) . ?
C17A H17A 0.9500 . ?
N18A C19A 1.346(16) . ?
N18A C23A 1.317(15) . ?
C19A C20A 1.393(17) . ?
C19A N24A 1.460(17) . ?
C20A H20A 0.9500 . ?
C20A C21A 1.386(14) . ?
C21A H21A 0.9500 . ?
C21A C22A 1.397(13) . ?
C22A H22A 0.9500 . ?
C22A C23A 1.363(14) . ?
C23A N29A 1.414(16) . ?
N24A N25A 1.403(14) . ?
N24A C28A 1.392(16) . ?
N25A C26A 1.350(12) . ?
C26A H26A 0.9500 . ?
C26A C27A 1.450(15) . ?
C27A H27A 0.9500 . ?
C27A C28A 1.366(16) . ?
C28A H28A 0.9500 . ?
N29A N30A 1.382(16) . ?
N29A C33A 1.351(16) . ?
N30A C31A 1.363(14) . ?
C31A H31A 0.9500 . ?
C31A C32A 1.397(12) . ?
C32A H32A 0.9500 . ?
C32A C33A 1.369(11) . ?
C33A H33A 0.9500 . ?
Ru1 N2B 1.976(10) . ?
Ru1 N9B 2.088(10) . ?
Ru1 N14B 2.060(10) . ?
Ru1 N18B 1.939(9) . ?
Ru1 N25B 2.125(8) . ?
Ru1 N30B 2.076(11) . ?
N2B C3B 1.321(19) . ?
N2B C7B 1.339(16) . ?
C3B C4B 1.41(2) . ?
C3B N8B 1.46(2) . ?
C4B H4B 0.9500 . ?
C4B C5B 1.378(13) . ?
C5B H5B 0.9500 . ?
C5B C6B 1.384(13) . ?
C6B H6B 0.9500 . ?
C6B C7B 1.372(16) . ?
C7B N13B 1.314(17) . ?
N8B N9B 1.331(15) . ?
N8B C12B 1.351(14) . ?
N9B C10B 1.313(15) . ?
C10B H10B 0.9500 . ?
C10B C11B 1.406(13) . ?
C11B H11B 0.9500 . ?
C11B C12B 1.361(12) . ?
C12B H12B 0.9500 . ?
N13B N14B 1.410(15) . ?
N13B C17B 1.358(15) . ?
N14B C15B 1.302(13) . ?
C15B H15B 0.9500 . ?
C15B C16B 1.387(12) . ?
C16B H16B 0.9500 . ?
C16B C17B 1.364(12) . ?
C17B H17B 0.9500 . ?
N18B C19B 1.320(17) . ?
N18B C23B 1.370(17) . ?
C19B C20B 1.382(16) . ?
C19B N24B 1.344(18) . ?
C20B H20B 0.9500 . ?
C20B C21B 1.385(13) . ?
C21B H21B 0.9500 . ?
C21B C22B 1.390(13) . ?
C22B H22B 0.9500 . ?
C22B C23B 1.401(16) . ?
C23B N29B 1.414(17) . ?
N24B N25B 1.381(15) . ?
N24B C28B 1.325(17) . ?
N25B C26B 1.297(12) . ?
C26B H26B 0.9500 . ?
C26B C27B 1.378(15) . ?
C27B H27B 0.9500 . ?
C27B C28B 1.387(16) . ?
C28B H28B 0.9500 . ?
N29B N30B 1.387(16) . ?
N29B C33B 1.370(15) . ?
N30B C31B 1.300(14) . ?
C31B H31B 0.9500 . ?
C31B C32B 1.396(12) . ?
C32B H32B 0.9500 . ?
C32B C33B 1.370(11) . ?
C33B H33B 0.9500 . ?
B34 F35 1.389(4) . ?
B34 F36 1.399(4) . ?
B34 F37 1.398(4) . ?
B34 F38 1.394(4) . ?
B39 F40 1.398(4) . ?
B39 F41 1.394(4) . ?
B39 F42 1.395(4) . ?
B39 F43 1.384(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
N2A Fe1 N9A 78.6(5) . . ?
N2A Fe1 N14A 80.1(5) . . ?
N2A Fe1 N18A 177.3(5) . . ?
N2A Fe1 N25A 102.2(5) . . ?
N2A Fe1 N30A 99.6(5) . . ?
N14A Fe1 N9A 158.7(5) . . ?
N14A Fe1 N18A 99.3(4) . . ?
N18A Fe1 N9A 101.9(4) . . ?
N25A Fe1 N9A 94.1(5) . . ?
N25A Fe1 N14A 90.9(5) . . ?
N25A Fe1 N18A 80.5(4) . . ?
N25A Fe1 N30A 158.2(4) . . ?
N30A Fe1 N9A 91.9(5) . . ?
N30A Fe1 N14A 91.2(5) . . ?
N30A Fe1 N18A 77.8(4) . . ?
C3A N2A Fe1 121.7(10) . . ?
C7A N2A Fe1 121.3(9) . . ?
C7A N2A C3A 116.8(12) . . ?
N2A C3A C4A 124.6(13) . . ?
N8A C3A N2A 109.8(14) . . ?
N8A C3A C4A 125.7(13) . . ?
C3A C4A H4A 121.8 . . ?
C3A C4A C5A 116.4(10) . . ?
C5A C4A H4A 121.8 . . ?
C4A C5A H5A 118.9 . . ?
C6A C5A C4A 122.3(8) . . ?
C6A C5A H5A 118.9 . . ?
C5A C6A H6A 121.8 . . ?
C5A C6A C7A 116.5(9) . . ?
C7A C6A H6A 121.8 . . ?
N2A C7A C6A 123.4(10) . . ?
N2A C7A N13A 108.6(10) . . ?
C6A C7A N13A 127.9(10) . . ?
C3A N8A N9A 117.2(11) . . ?
C3A N8A C12A 135.3(11) . . ?
C12A N8A N9A 106.9(8) . . ?
N8A N9A Fe1 112.5(7) . . ?
C10A N9A Fe1 142.0(8) . . ?
C10A N9A N8A 105.5(9) . . ?
N9A C10A H10A 124.2 . . ?
N9A C10A C11A 111.6(8) . . ?
C11A C10A H10A 124.2 . . ?
C10A C11A H11A 127.2 . . ?
C12A C11A C10A 105.6(7) . . ?
C12A C11A H11A 127.2 . . ?
N8A C12A H12A 124.9 . . ?
C11A C12A N8A 110.2(8) . . ?
C11A C12A H12A 124.9 . . ?
N14A N13A C7A 114.5(10) . . ?
C17A N13A C7A 134.0(10) . . ?
C17A N13A N14A 111.4(10) . . ?
N13A N14A Fe1 115.1(8) . . ?
C15A N14A Fe1 140.1(8) . . ?
C15A N14A N13A 104.1(9) . . ?
N14A C15A H15A 124.6 . . ?
N14A C15A C16A 110.7(8) . . ?
C16A C15A H15A 124.6 . . ?
C15A C16A H16A 127.1 . . ?
C17A C16A C15A 105.9(7) . . ?
C17A C16A H16A 127.1 . . ?
N13A C17A H17A 126.1 . . ?
C16A C17A N13A 107.8(8) . . ?
C16A C17A H17A 126.1 . . ?
C19A N18A Fe1 117.8(8) . . ?
C23A N18A Fe1 121.0(7) . . ?
C23A N18A C19A 121.2(10) . . ?
N18A C19A C20A 120.1(10) . . ?
N18A C19A N24A 112.8(11) . . ?
C20A C19A N24A 127.1(11) . . ?
C19A C20A H20A 121.4 . . ?
C21A C20A C19A 117.3(9) . . ?
C21A C20A H20A 121.4 . . ?
C20A C21A H21A 119.0 . . ?
C20A C21A C22A 121.9(9) . . ?
C22A C21A H21A 119.0 . . ?
C21A C22A H22A 122.0 . . ?
C23A C22A C21A 116.0(9) . . ?
C23A C22A H22A 122.0 . . ?
N18A C23A C22A 123.4(10) . . ?
N18A C23A N29A 110.2(10) . . ?
C22A C23A N29A 126.4(11) . . ?
N25A N24A C19A 112.9(10) . . ?
C28A N24A C19A 134.0(11) . . ?
C28A N24A N25A 112.1(10) . . ?
N24A N25A Fe1 115.8(7) . . ?
C26A N25A Fe1 140.3(7) . . ?
C26A N25A N24A 103.8(8) . . ?
N25A C26A H26A 124.4 . . ?
N25A C26A C27A 111.2(8) . . ?
C27A C26A H26A 124.4 . . ?
C26A C27A H27A 126.9 . . ?
C28A C27A C26A 106.1(11) . . ?
C28A C27A H27A 126.9 . . ?
N24A C28A H28A 126.7 . . ?
C27A C28A N24A 106.6(10) . . ?
C27A C28A H28A 126.7 . . ?
N30A N29A C23A 115.3(11) . . ?
C33A N29A C23A 132.1(11) . . ?
C33A N29A N30A 112.4(10) . . ?
N29A N30A Fe1 115.7(9) . . ?
C31A N30A Fe1 141.4(8) . . ?
C31A N30A N29A 102.8(9) . . ?
N30A C31A H31A 124.0 . . ?
N30A C31A C32A 112.0(8) . . ?
C32A C31A H31A 124.0 . . ?
C31A C32A H32A 127.3 . . ?
C33A C32A C31A 105.4(7) . . ?
C33A C32A H32A 127.3 . . ?
N29A C33A C32A 107.4(8) . . ?
N29A C33A H33A 126.3 . . ?
C32A C33A H33A 126.3 . . ?
N2B Ru1 N9B 79.4(4) . . ?
N2B Ru1 N14B 78.2(4) . . ?
N2B Ru1 N25B 103.7(4) . . ?
N2B Ru1 N30B 98.3(5) . . ?
N9B Ru1 N25B 93.8(4) . . ?
N14B Ru1 N9B 157.5(4) . . ?
N14B Ru1 N25B 92.9(4) . . ?
N14B Ru1 N30B 89.2(4) . . ?
N18B Ru1 N2B 179.2(6) . . ?
N18B Ru1 N9B 101.2(4) . . ?
N18B Ru1 N14B 101.2(4) . . ?
N18B Ru1 N25B 76.8(4) . . ?
N18B Ru1 N30B 81.2(4) . . ?
N30B Ru1 N9B 92.6(4) . . ?
N30B Ru1 N25B 157.9(4) . . ?
C3B N2B Ru1 118.8(10) . . ?
C3B N2B C7B 122.5(11) . . ?
C7B N2B Ru1 118.7(8) . . ?
N2B C3B C4B 119.3(13) . . ?
N2B C3B N8B 112.2(14) . . ?
C4B C3B N8B 128.5(13) . . ?
C3B C4B H4B 121.1 . . ?
C5B C4B C3B 117.9(10) . . ?
C5B C4B H4B 121.1 . . ?
C4B C5B H5B 119.0 . . ?
C4B C5B C6B 122.0(9) . . ?
C6B C5B H5B 119.0 . . ?
C5B C6B H6B 121.7 . . ?
C7B C6B C5B 116.7(9) . . ?
C7B C6B H6B 121.7 . . ?
N2B C7B C6B 121.6(10) . . ?
N13B C7B N2B 113.7(11) . . ?
N13B C7B C6B 124.6(11) . . ?
N9B N8B C3B 118.4(11) . . ?
N9B N8B C12B 114.7(10) . . ?
C12B N8B C3B 126.4(11) . . ?
N8B N9B Ru1 111.1(8) . . ?
C10B N9B Ru1 144.6(9) . . ?
C10B N9B N8B 104.3(10) . . ?
N9B C10B H10B 124.9 . . ?
N9B C10B C11B 110.3(9) . . ?
C11B C10B H10B 124.9 . . ?
C10B C11B H11B 126.5 . . ?
C12B C11B C10B 106.9(8) . . ?
C12B C11B H11B 126.5 . . ?
N8B C12B C11B 103.5(8) . . ?
N8B C12B H12B 128.2 . . ?
C11B C12B H12B 128.2 . . ?
C7B N13B N14B 119.4(12) . . ?
C7B N13B C17B 131.0(11) . . ?
C17B N13B N14B 109.2(10) . . ?
N13B N14B Ru1 110.0(8) . . ?
C15B N14B Ru1 145.2(8) . . ?
C15B N14B N13B 104.8(9) . . ?
N14B C15B H15B 123.7 . . ?
N14B C15B C16B 112.6(8) . . ?
C16B C15B H15B 123.7 . . ?
C15B C16B H16B 127.2 . . ?
C17B C16B C15B 105.6(8) . . ?
C17B C16B H16B 127.2 . . ?
N13B C17B C16B 107.7(8) . . ?
N13B C17B H17B 126.2 . . ?
C16B C17B H17B 126.2 . . ?
C19B N18B Ru1 123.5(9) . . ?
C19B N18B C23B 118.3(10) . . ?
C23B N18B Ru1 118.0(8) . . ?
N18B C19B C20B 124.1(11) . . ?
N18B C19B N24B 109.4(12) . . ?
N24B C19B C20B 126.4(11) . . ?
C19B C20B H20B 121.5 . . ?
C19B C20B C21B 116.9(9) . . ?
C21B C20B H20B 121.5 . . ?
C20B C21B H21B 119.0 . . ?
C20B C21B C22B 121.9(8) . . ?
C22B C21B H21B 119.0 . . ?
C21B C22B H22B 121.8 . . ?
C21B C22B C23B 116.4(9) . . ?
C23B C22B H22B 121.8 . . ?
N18B C23B C22B 122.3(10) . . ?
N18B C23B N29B 112.4(11) . . ?
C22B C23B N29B 125.3(11) . . ?
C19B N24B N25B 122.5(12) . . ?
C28B N24B C19B 128.0(12) . . ?
C28B N24B N25B 109.5(10) . . ?
N24B N25B Ru1 107.4(7) . . ?
C26B N25B Ru1 144.9(7) . . ?
C26B N25B N24B 107.0(9) . . ?
N25B C26B H26B 124.7 . . ?
N25B C26B C27B 110.6(9) . . ?
C27B C26B H26B 124.7 . . ?
C26B C27B H27B 127.2 . . ?
C26B C27B C28B 105.5(10) . . ?
C28B C27B H27B 127.2 . . ?
N24B C28B C27B 107.4(10) . . ?
N24B C28B H28B 126.3 . . ?
C27B C28B H28B 126.3 . . ?
N30B N29B C23B 119.2(11) . . ?
C33B N29B C23B 131.4(11) . . ?
C33B N29B N30B 109.3(9) . . ?
N29B N30B Ru1 109.2(8) . . ?
C31B N30B Ru1 144.4(8) . . ?
C31B N30B N29B 106.4(9) . . ?
N30B C31B H31B 124.2 . . ?
N30B C31B C32B 111.5(9) . . ?
C32B C31B H31B 124.2 . . ?
C31B C32B H32B 127.1 . . ?
C33B C32B C31B 105.8(8) . . ?
C33B C32B H32B 127.1 . . ?
N29B C33B C32B 107.1(8) . . ?
N29B C33B H33B 126.5 . . ?
C32B C33B H33B 126.5 . . ?
F35 B34 F36 110.3(3) . . ?
F35 B34 F37 109.1(3) . . ?
F35 B34 F38 109.8(2) . . ?
F37 B34 F36 108.4(2) . . ?
F38 B34 F36 109.3(3) . . ?
F38 B34 F37 110.0(3) . . ?
F41 B39 F40 110.3(3) . . ?
F41 B39 F42 108.0(3) . . ?
F42 B39 F40 108.5(2) . . ?
F43 B39 F40 109.3(3) . . ?
F43 B39 F41 109.3(2) . . ?
F43 B39 F42 111.3(3) . . ?

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 N2A C3A C4A -176.4(11) . . . . ?
Fe1 N2A C3A N8A 4.3(19) . . . . ?
Fe1 N2A C7A C6A 176.7(10) . . . . ?
Fe1 N2A C7A N13A -0.1(16) . . . . ?
Fe1 N9A C10A C11A -179.4(11) . . . . ?
Fe1 N14A C15A C16A 171.7(11) . . . . ?
Fe1 N18A C19A C20A -179.8(9) . . . . ?
Fe1 N18A C19A N24A 2.1(13) . . . . ?
Fe1 N18A C23A C22A 178.4(8) . . . . ?
Fe1 N18A C23A N29A 0.1(12) . . . . ?
Fe1 N25A C26A C27A -175.2(8) . . . . ?
Fe1 N30A C31A C32A 175.4(10) . . . . ?
N2A C3A C4A C5A -1(2) . . . . ?
N2A C3A N8A N9A -5.0(19) . . . . ?
N2A C3A N8A C12A -175.6(12) . . . . ?
N2A C7A N13A N14A -4.2(16) . . . . ?
N2A C7A N13A C17A 179.0(13) . . . . ?
C3A N2A C7A C6A 2(2) . . . . ?
C3A N2A C7A N13A -175.2(13) . . . . ?
C3A C4A C5A C6A 3.2(16) . . . . ?
C3A N8A N9A Fe1 3.9(15) . . . . ?
C3A N8A N9A C10A -176.0(12) . . . . ?
C3A N8A C12A C11A 175.8(15) . . . . ?
C4A C3A N8A N9A 175.7(13) . . . . ?
C4A C3A N8A C12A 5(3) . . . . ?
C4A C5A C6A C7A -2.9(16) . . . . ?
C5A C6A C7A N2A 0(2) . . . . ?
C5A C6A C7A N13A 176.6(12) . . . . ?
C6A C7A N13A N14A 179.2(13) . . . . ?
C6A C7A N13A C17A 2(2) . . . . ?
C7A N2A C3A C4A -1(2) . . . . ?
C7A N2A C3A N8A 179.4(13) . . . . ?
C7A N13A N14A Fe1 6.6(14) . . . . ?
C7A N13A N14A C15A 178.9(10) . . . . ?
C7A N13A C17A C16A -179.9(13) . . . . ?
N8A C3A C4A C5A 178.2(14) . . . . ?
N8A N9A C10A C11A 0.4(12) . . . . ?
N9A N8A C12A C11A 4.6(12) . . . . ?
N9A C10A C11A C12A 2.4(12) . . . . ?
C10A C11A C12A N8A -4.3(11) . . . . ?
C12A N8A N9A Fe1 176.9(7) . . . . ?
C12A N8A N9A C10A -3.0(12) . . . . ?
N13A N14A C15A C16A 2.5(12) . . . . ?
N14A N13A C17A C16A 3.2(13) . . . . ?
N14A C15A C16A C17A -0.7(11) . . . . ?
C15A C16A C17A N13A -1.5(11) . . . . ?
C17A N13A N14A Fe1 -175.8(8) . . . . ?
C17A N13A N14A C15A -3.5(13) . . . . ?
N18A C19A C20A C21A -0.3(16) . . . . ?
N18A C19A N24A N25A -4.9(14) . . . . ?
N18A C19A N24A C28A -172.5(12) . . . . ?
N18A C23A N29A N30A 0.7(14) . . . . ?
N18A C23A N29A C33A 176.2(11) . . . . ?
C19A N18A C23A C22A -1.4(16) . . . . ?
C19A N18A C23A N29A -179.7(10) . . . . ?
C19A C20A C21A C22A 2.0(14) . . . . ?
C19A N24A N25A Fe1 5.7(12) . . . . ?
C19A N24A N25A C26A -173.6(9) . . . . ?
C19A N24A C28A C27A 169.1(13) . . . . ?
C20A C19A N24A N25A 177.2(11) . . . . ?
C20A C19A N24A C28A 10(2) . . . . ?
C20A C21A C22A C23A -3.2(14) . . . . ?
C21A C22A C23A N18A 2.9(15) . . . . ?
C21A C22A C23A N29A -179.1(10) . . . . ?
C22A C23A N29A N30A -177.5(11) . . . . ?
C22A C23A N29A C33A -2(2) . . . . ?
C23A N18A C19A C20A -0.1(17) . . . . ?
C23A N18A C19A N24A -178.1(10) . . . . ?
C23A N29A N30A Fe1 -1.2(14) . . . . ?
C23A N29A N30A C31A 175.5(9) . . . . ?
C23A N29A C33A C32A -174.4(11) . . . . ?
N24A C19A C20A C21A 177.5(11) . . . . ?
N24A N25A C26A C27A 3.7(11) . . . . ?
N25A N24A C28A C27A 1.4(13) . . . . ?
N25A C26A C27A C28A -3.1(12) . . . . ?
C26A C27A C28A N24A 0.9(12) . . . . ?
C28A N24A N25A Fe1 176.1(7) . . . . ?
C28A N24A N25A C26A -3.2(11) . . . . ?
N29A N30A C31A C32A 0.2(11) . . . . ?
N30A N29A C33A C32A 1.2(12) . . . . ?
N30A C31A C32A C33A 0.5(10) . . . . ?
C31A C32A C33A N29A -1.0(10) . . . . ?
C33A N29A N30A Fe1 -177.5(8) . . . . ?
C33A N29A N30A C31A -0.9(13) . . . . ?
Ru1 N2B C3B C4B 178.8(11) . . . . ?
Ru1 N2B C3B N8B -3.3(18) . . . . ?
Ru1 N2B C7B C6B -178.3(10) . . . . ?
Ru1 N2B C7B N13B 0.7(18) . . . . ?
Ru1 N9B C10B C11B 178.9(12) . . . . ?
Ru1 N14B C15B C16B 172.4(10) . . . . ?
Ru1 N18B C19B C20B -178.5(9) . . . . ?
Ru1 N18B C19B N24B -1.2(15) . . . . ?
Ru1 N18B C23B C22B 178.6(9) . . . . ?
Ru1 N18B C23B N29B -1.9(14) . . . . ?
Ru1 N25B C26B C27B -170.7(9) . . . . ?
Ru1 N30B C31B C32B 178.1(10) . . . . ?
N2B C3B C4B C5B 1(2) . . . . ?
N2B C3B N8B N9B 4(2) . . . . ?
N2B C3B N8B C12B 175.9(12) . . . . ?
N2B C7B N13B N14B -1(2) . . . . ?
N2B C7B N13B C17B 171.5(14) . . . . ?
C3B N2B C7B C6B 1(2) . . . . ?
C3B N2B C7B N13B -179.6(15) . . . . ?
C3B C4B C5B C6B -1.2(17) . . . . ?
C3B N8B N9B Ru1 -3.4(15) . . . . ?
C3B N8B N9B C10B 177.3(12) . . . . ?
C3B N8B C12B C11B -177.2(12) . . . . ?
C4B C3B N8B N9B -177.9(14) . . . . ?
C4B C3B N8B C12B -6(2) . . . . ?
C4B C5B C6B C7B 1.6(16) . . . . ?
C5B C6B C7B N2B -1.7(19) . . . . ?
C5B C6B C7B N13B 179.4(13) . . . . ?
C6B C7B N13B N14B 178.4(12) . . . . ?
C6B C7B N13B C17B -10(3) . . . . ?
C7B N2B C3B C4B -1(2) . . . . ?
C7B N2B C3B N8B 177.0(13) . . . . ?
C7B N13B N14B Ru1 0.3(16) . . . . ?
C7B N13B N14B C15B 177.4(13) . . . . ?
C7B N13B C17B C16B -175.8(15) . . . . ?
N8B C3B C4B C5B -176.7(14) . . . . ?
N8B N9B C10B C11B -2.1(13) . . . . ?
N9B N8B C12B C11B -5.5(12) . . . . ?
N9B C10B C11B C12B -1.1(12) . . . . ?
C10B C11B C12B N8B 3.7(11) . . . . ?
C12B N8B N9B Ru1 -175.8(7) . . . . ?
C12B N8B N9B C10B 4.8(14) . . . . ?
N13B N14B C15B C16B -2.9(13) . . . . ?
N14B N13B C17B C16B -3.1(13) . . . . ?
N14B C15B C16B C17B 1.0(12) . . . . ?
C15B C16B C17B N13B 1.3(11) . . . . ?
C17B N13B N14B Ru1 -173.4(8) . . . . ?
C17B N13B N14B C15B 3.7(13) . . . . ?
N18B C19B C20B C21B 1.8(17) . . . . ?
N18B C19B N24B N25B 5.4(17) . . . . ?
N18B C19B N24B C28B -176.3(11) . . . . ?
N18B C23B N29B N30B 2.8(16) . . . . ?
N18B C23B N29B C33B 177.9(11) . . . . ?
C19B N18B C23B C22B 2.7(18) . . . . ?
C19B N18B C23B N29B -177.7(11) . . . . ?
C19B C20B C21B C22B -0.5(14) . . . . ?
C19B N24B N25B Ru1 -6.5(13) . . . . ?
C19B N24B N25B C26B -179.2(11) . . . . ?
C19B N24B C28B C27B -179.2(12) . . . . ?
C20B C19B N24B N25B -177.4(11) . . . . ?
C20B C19B N24B C28B 1(2) . . . . ?
C20B C21B C22B C23B 0.4(14) . . . . ?
C21B C22B C23B N18B -1.5(16) . . . . ?
C21B C22B C23B N29B 179.0(11) . . . . ?
C22B C23B N29B N30B -177.6(11) . . . . ?
C22B C23B N29B C33B -3(2) . . . . ?
C23B N18B C19B C20B -2.9(18) . . . . ?
C23B N18B C19B N24B 174.4(11) . . . . ?
C23B N29B N30B Ru1 -2.4(13) . . . . ?
C23B N29B N30B C31B 175.6(11) . . . . ?
C23B N29B C33B C32B -176.1(12) . . . . ?
N24B C19B C20B C21B -175.0(11) . . . . ?
N24B N25B C26B C27B -2.9(11) . . . . ?
N25B N24B C28B C27B -0.7(12) . . . . ?
N25B C26B C27B C28B 2.4(12) . . . . ?
C26B C27B C28B N24B -1.0(12) . . . . ?
C28B N24B N25B Ru1 175.0(7) . . . . ?
C28B N24B N25B C26B 2.2(12) . . . . ?
N29B N30B C31B C32B 1.4(12) . . . . ?
N30B N29B C33B C32B -0.7(11) . . . . ?
N30B C31B C32B C33B -1.8(10) . . . . ?
C31B C32B C33B N29B 1.4(10) . . . . ?
C33B N29B N30B Ru1 -178.4(7) . . . . ?
C33B N29B N30B C31B -0.4(12) . . . . ?

_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'
