# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_1_2CH3CN_100K_BnL_BF4
_database_code_depnum_ccdc_archive 'CCDC 1478564'
_audit_update_record             
;
2016-07-14 deposited with the CCDC.
2016-07-26 downloaded from the CCDC.
;
_audit_creation_date             2015-08-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C34 H32 Fe N12, 2(B F4), 2(C2 H3 N)'
_chemical_formula_sum            'C38 H38 B2 F8 Fe N14'
_chemical_formula_weight         920.29
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C34 H32 N12 Fe B2 F8 (C2 H3 N)2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   9.3961(2)
_cell_length_b                   26.1242(4)
_cell_length_c                   9.2160(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.468(3)
_cell_angle_gamma                90.00
_cell_volume                     2105.26(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8357
_cell_measurement_temperature    100.00(14)
_cell_measurement_theta_max      73.9160
_cell_measurement_theta_min      5.0010
_exptl_absorpt_coefficient_mu    3.603
_exptl_absorpt_correction_T_max  0.871
_exptl_absorpt_correction_T_min  0.524
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.3468
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.0444
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            20176
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         74.16
_diffrn_reflns_theta_min         3.38
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -49.00   35.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987   37.0000   60.0000 84

#__ type_ start__ end____ width___ exp.time_
  2 omega -124.00  -79.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  -99.0000  -60.0000 45

#__ type_ start__ end____ width___ exp.time_
  3 omega  -49.00   35.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987   37.0000    0.0000 84

#__ type_ start__ end____ width___ exp.time_
  4 omega -124.00  -79.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  -99.0000  -30.0000 45

#__ type_ start__ end____ width___ exp.time_
  5 omega    1.00   83.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       41.3987  -99.0000 -120.0000 82

#__ type_ start__ end____ width___ exp.time_
  6 omega   24.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -94.0000  -60.0000 85

#__ type_ start__ end____ width___ exp.time_
  7 omega   81.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   45.0000   60.0000 97

#__ type_ start__ end____ width___ exp.time_
  8 omega   30.00  142.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -77.0000   30.0000 112

#__ type_ start__ end____ width___ exp.time_
  9 omega   30.00   90.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -30.0000  120.0000 60

#__ type_ start__ end____ width___ exp.time_
 10 omega   34.00  139.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -61.0000  -30.0000 105

#__ type_ start__ end____ width___ exp.time_
 11 omega   24.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -94.0000  120.0000 85

#__ type_ start__ end____ width___ exp.time_
 12 omega   78.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   61.0000  150.0000 100

#__ type_ start__ end____ width___ exp.time_
 13 omega -115.00  -12.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  -57.0000  120.0000 103

#__ type_ start__ end____ width___ exp.time_
 14 omega -115.00  -12.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  -57.0000    0.0000 103

#__ type_ start__ end____ width___ exp.time_
 15 omega -115.00  -12.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  -57.0000 -120.0000 103

#__ type_ start__ end____ width___ exp.time_
 16 omega   78.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   61.0000    0.0000 100

#__ type_ start__ end____ width___ exp.time_
 17 omega   75.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   77.0000   90.0000 103

#__ type_ start__ end____ width___ exp.time_
 18 omega   78.00  117.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   61.0000 -180.0000 39

#__ type_ start__ end____ width___ exp.time_
 19 omega   47.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   15.0000  -60.0000 131
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0877969000
_diffrn_orient_matrix_UB_12      -0.0485436000
_diffrn_orient_matrix_UB_13      -0.0783538000
_diffrn_orient_matrix_UB_21      -0.0449079000
_diffrn_orient_matrix_UB_22      -0.0095424000
_diffrn_orient_matrix_UB_23      0.1426403000
_diffrn_orient_matrix_UB_31      -0.1459632000
_diffrn_orient_matrix_UB_32      0.0320895000
_diffrn_orient_matrix_UB_33      -0.0761017000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_number_gt                3809
_reflns_number_total             4228
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         4228
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0380
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0683P)²+0.4237P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1088
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17)
2.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Fe1 Fe 0.5000 0.5000 0.5000 0.02437(12) Uani 1 d . . 2 S T P
N1 N 0.39586(17) 0.56868(6) 0.72056(17) 0.0287(3) Uani 1 d . . 1 . . .
N2 N 0.40660(16) 0.52376(5) 0.65215(17) 0.0267(3) Uani 1 d . . 1 . . .
N22 N 0.48610(17) 0.41569(5) 0.69626(17) 0.0281(3) Uani 1 d . . 1 . . .
N21 N 0.58339(17) 0.44268(5) 0.64620(17) 0.0275(3) Uani 1 d . . 1 . . .
N12 N 0.25249(17) 0.43273(5) 0.48762(17) 0.0282(3) Uani 1 d . . 1 . . .
N11 N 0.31012(16) 0.46063(6) 0.39780(17) 0.0281(3) Uani 1 d . . 1 . . .
C1 C 0.3221(2) 0.56188(7) 0.8202(2) 0.0344(4) Uani 1 d . . 1 . . .
H1 H 0.3014 0.5878 0.8822 0.041 Uiso 1 calc . . 1 R . .
C2 C 0.2822(2) 0.51119(7) 0.8169(2) 0.0336(4) Uani 1 d . . 1 . . .
H2 H 0.2291 0.4949 0.8743 0.040 Uiso 1 calc . . 1 R . .
C3 C 0.3370(2) 0.48915(7) 0.7111(2) 0.0278(3) Uani 1 d . . 1 . . .
C23 C 0.5593(2) 0.37708(7) 0.7920(2) 0.0316(4) Uani 1 d . . 1 . . .
H23 H 0.5153 0.3532 0.8412 0.038 Uiso 1 calc . . 1 R . .
C22 C 0.7091(2) 0.37885(7) 0.8046(2) 0.0333(4) Uani 1 d . . 1 . . .
H22 H 0.7894 0.3566 0.8638 0.040 Uiso 1 calc . . 1 R . .
C21 C 0.7194(2) 0.42010(7) 0.7124(2) 0.0304(4) Uani 1 d . . 1 . . .
H21 H 0.8105 0.4306 0.6987 0.037 Uiso 1 calc . . 1 R . .
C13 C 0.1230(2) 0.40806(7) 0.4005(2) 0.0332(4) Uani 1 d . . 1 . . .
H13 H 0.0623 0.3866 0.4378 0.040 Uiso 1 calc . . 1 R . .
C12 C 0.0963(2) 0.42006(8) 0.2483(2) 0.0355(4) Uani 1 d . . 1 . . .
H12 H 0.0140 0.4085 0.1588 0.043 Uiso 1 calc . . 1 R . .
C11 C 0.2151(2) 0.45275(7) 0.2514(2) 0.0316(4) Uani 1 d . . 1 . . .
H11 H 0.2265 0.4673 0.1618 0.038 Uiso 1 calc . . 1 R . .
C4 C 0.3311(2) 0.43487(7) 0.6555(2) 0.0283(4) Uani 1 d . . 1 . . .
H4 H 0.2753 0.4132 0.7069 0.034 Uiso 1 calc . . 1 R . .
C30 C 0.4645(2) 0.61675(7) 0.6929(2) 0.0293(4) Uani 1 d . . 1 . . .
H30a H 0.4704 0.6160 0.5879 0.035 Uiso 1 calc . . 1 R . .
H30b H 0.5696 0.6203 0.7708 0.035 Uiso 1 calc . . 1 R . .
C31 C 0.3686(2) 0.66175(6) 0.7054(2) 0.0284(3) Uani 1 d . . 1 . . .
C32 C 0.4233(2) 0.69554(7) 0.8298(2) 0.0374(4) Uani 1 d . . 1 . . .
H32 H 0.5230 0.6910 0.9057 0.045 Uiso 1 calc . . 1 R . .
C33 C 0.3331(3) 0.73591(8) 0.8439(3) 0.0467(5) Uani 1 d . . 1 . . .
H33 H 0.3713 0.7588 0.9296 0.056 Uiso 1 calc . . 1 R . .
C34 C 0.1883(2) 0.74293(8) 0.7340(3) 0.0427(5) Uani 1 d . . 1 . . .
H34 H 0.1265 0.7704 0.7442 0.051 Uiso 1 calc . . 1 R . .
C35 C 0.1333(2) 0.70958(8) 0.6085(3) 0.0402(4) Uani 1 d . . 1 . . .
H35 H 0.0338 0.7144 0.5323 0.048 Uiso 1 calc . . 1 R . .
C36 C 0.2229(2) 0.66927(8) 0.5938(2) 0.0344(4) Uani 1 d . . 1 . . .
H36 H 0.1849 0.6467 0.5073 0.041 Uiso 1 calc . . 1 R . .
F1 F 0.07079(15) 0.36360(5) 0.71573(14) 0.0466(3) Uani 1 d . . 1 . . .
F2 F 0.28391(13) 0.37387(6) 0.93293(14) 0.0486(3) Uani 1 d . . 1 . . .
F3 F 0.07167(15) 0.33630(5) 0.95020(14) 0.0446(3) Uani 1 d . . 1 . . .
F4 F 0.07284(14) 0.42146(4) 0.89950(14) 0.0427(3) Uani 1 d . . 1 . . .
B1 B 0.1242(2) 0.37353(9) 0.8753(3) 0.0341(4) Uani 1 d . . 1 . . .
N7 N 0.3371(3) 0.18871(8) 1.0046(3) 0.0565(5) Uani 1 d . . 1 . . .
C18 C 0.2889(2) 0.21176(8) 0.8931(3) 0.0400(4) Uani 1 d . . 1 . . .
C19 C 0.2273(4) 0.24145(10) 0.7517(3) 0.0600(7) Uani 1 d . . 1 . . .
H19a H 0.1695 0.2190 0.6650 0.090 Uiso 1 calc . . 1 GR . .
H19b H 0.3112 0.2575 0.7292 0.090 Uiso 1 calc . . 1 GR . .
H19c H 0.1594 0.2680 0.7648 0.090 Uiso 1 calc . . 1 GR . .


_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 2.0056(14) 3_666 ?
Fe1 N2 2.0056(14) . ?
Fe1 N21 1.9747(15) . ?
Fe1 N21 1.9747(15) 3_666 ?
Fe1 N11 1.9743(14) 3_666 ?
Fe1 N11 1.9743(14) . ?
N1 N2 1.353(2) . ?
N1 C1 1.350(2) . ?
N1 C30 1.476(2) . ?
N2 C3 1.341(2) . ?
N22 N21 1.362(2) . ?
N22 C23 1.351(2) . ?
N22 C4 1.454(2) . ?
N21 C21 1.335(2) . ?
N12 N11 1.356(2) . ?
N12 C13 1.351(2) . ?
N12 C4 1.451(2) . ?
N11 C11 1.334(2) . ?
C1 H1 0.9500 . ?
C1 C2 1.374(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.384(3) . ?
C3 C4 1.502(2) . ?
C23 H23 0.9500 . ?
C23 C22 1.370(3) . ?
C22 H22 0.9500 . ?
C22 C21 1.398(3) . ?
C21 H21 0.9500 . ?
C13 H13 0.9500 . ?
C13 C12 1.368(3) . ?
C12 H12 0.9500 . ?
C12 C11 1.397(3) . ?
C11 H11 0.9500 . ?
C4 H4 1.0000 . ?
C30 H30a 0.9900 . ?
C30 H30b 0.9900 . ?
C30 C31 1.511(2) . ?
C31 C32 1.388(3) . ?
C31 C36 1.393(3) . ?
C32 H32 0.9500 . ?
C32 C33 1.388(3) . ?
C33 H33 0.9500 . ?
C33 C34 1.379(3) . ?
C34 H34 0.9500 . ?
C34 C35 1.388(3) . ?
C35 H35 0.9500 . ?
C35 C36 1.386(3) . ?
C36 H36 0.9500 . ?
F1 B1 1.394(2) . ?
F2 B1 1.397(2) . ?
F3 B1 1.384(2) . ?
F4 B1 1.389(3) . ?
N7 C18 1.133(3) . ?
C18 C19 1.443(3) . ?
C19 H19a 0.9800 . ?
C19 H19b 0.9800 . ?
C19 H19c 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 180.0 . 3_666 ?
N21 Fe1 N2 85.61(6) . . ?
N21 Fe1 N2 94.39(6) . 3_666 ?
N21 Fe1 N2 94.39(6) 3_666 . ?
N21 Fe1 N2 85.61(6) 3_666 3_666 ?
N21 Fe1 N21 180.00(5) 3_666 . ?
N11 Fe1 N2 93.18(6) . 3_666 ?
N11 Fe1 N2 86.82(6) . . ?
N11 Fe1 N2 86.82(6) 3_666 3_666 ?
N11 Fe1 N2 93.18(6) 3_666 . ?
N11 Fe1 N21 89.66(6) . . ?
N11 Fe1 N21 89.66(6) 3_666 3_666 ?
N11 Fe1 N21 90.34(6) 3_666 . ?
N11 Fe1 N21 90.34(6) . 3_666 ?
N11 Fe1 N11 180.0 3_666 . ?
N2 N1 C30 123.07(13) . . ?
C1 N1 N2 110.33(14) . . ?
C1 N1 C30 126.52(15) . . ?
N1 N2 Fe1 136.09(11) . . ?
C3 N2 Fe1 118.49(11) . . ?
C3 N2 N1 105.40(14) . . ?
N21 N22 C4 117.86(14) . . ?
C23 N22 N21 111.29(15) . . ?
C23 N22 C4 130.46(15) . . ?
N22 N21 Fe1 118.42(11) . . ?
C21 N21 Fe1 136.14(13) . . ?
C21 N21 N22 105.41(14) . . ?
N11 N12 C4 117.98(14) . . ?
C13 N12 N11 111.58(15) . . ?
C13 N12 C4 130.40(15) . . ?
N12 N11 Fe1 118.81(11) . . ?
C11 N11 Fe1 135.79(13) . . ?
C11 N11 N12 105.40(14) . . ?
N1 C1 H1 125.8 . . ?
N1 C1 C2 108.40(16) . . ?
C2 C1 H1 125.8 . . ?
C1 C2 H2 127.8 . . ?
C1 C2 C3 104.34(16) . . ?
C3 C2 H2 127.8 . . ?
N2 C3 C2 111.53(16) . . ?
N2 C3 C4 117.48(15) . . ?
C2 C3 C4 130.99(17) . . ?
N22 C23 H23 126.5 . . ?
N22 C23 C22 106.98(16) . . ?
C22 C23 H23 126.5 . . ?
C23 C22 H22 127.1 . . ?
C23 C22 C21 105.80(16) . . ?
C21 C22 H22 127.1 . . ?
N21 C21 C22 110.51(16) . . ?
N21 C21 H21 124.7 . . ?
C22 C21 H21 124.7 . . ?
N12 C13 H13 126.7 . . ?
N12 C13 C12 106.70(16) . . ?
C12 C13 H13 126.7 . . ?
C13 C12 H12 127.1 . . ?
C13 C12 C11 105.90(17) . . ?
C11 C12 H12 127.1 . . ?
N11 C11 C12 110.43(16) . . ?
N11 C11 H11 124.8 . . ?
C12 C11 H11 124.8 . . ?
N22 C4 C3 109.18(14) . . ?
N22 C4 H4 109.4 . . ?
N12 C4 N22 109.46(13) . . ?
N12 C4 C3 109.92(14) . . ?
N12 C4 H4 109.4 . . ?
C3 C4 H4 109.4 . . ?
N1 C30 H30a 109.7 . . ?
N1 C30 H30b 109.7 . . ?
N1 C30 C31 109.80(14) . . ?
H30a C30 H30b 108.2 . . ?
C31 C30 H30a 109.7 . . ?
C31 C30 H30b 109.7 . . ?
C32 C31 C30 120.47(17) . . ?
C32 C31 C36 119.12(17) . . ?
C36 C31 C30 120.39(16) . . ?
C31 C32 H32 119.8 . . ?
C31 C32 C33 120.45(19) . . ?
C33 C32 H32 119.8 . . ?
C32 C33 H33 119.9 . . ?
C34 C33 C32 120.3(2) . . ?
C34 C33 H33 119.9 . . ?
C33 C34 H34 120.2 . . ?
C33 C34 C35 119.65(18) . . ?
C35 C34 H34 120.2 . . ?
C34 C35 H35 119.9 . . ?
C36 C35 C34 120.27(19) . . ?
C36 C35 H35 119.9 . . ?
C31 C36 H36 119.9 . . ?
C35 C36 C31 120.23(18) . . ?
C35 C36 H36 119.9 . . ?
F1 B1 F2 108.91(16) . . ?
F3 B1 F1 109.82(17) . . ?
F3 B1 F2 110.14(17) . . ?
F3 B1 F4 110.22(16) . . ?
F4 B1 F1 108.98(17) . . ?
F4 B1 F2 108.74(17) . . ?
N7 C18 C19 179.6(3) . . ?
C18 C19 H19a 109.5 . . ?
C18 C19 H19b 109.5 . . ?
C18 C19 H19c 109.5 . . ?
H19a C19 H19b 109.5 . . ?
H19a C19 H19c 109.5 . . ?
H19b C19 H19c 109.5 . . ?

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 C2 178.42(13) . . . . ?
Fe1 N2 C3 C4 -1.4(2) . . . . ?
Fe1 N21 C21 C22 -177.86(13) . . . . ?
Fe1 N11 C11 C12 179.53(13) . . . . ?
N1 N2 C3 C2 -0.2(2) . . . . ?
N1 N2 C3 C4 179.99(15) . . . . ?
N1 C1 C2 C3 0.2(2) . . . . ?
N1 C30 C31 C32 110.17(19) . . . . ?
N1 C30 C31 C36 -68.5(2) . . . . ?
N2 Fe1 N2 N1 -30(9) 3_666 . . . ?
N2 Fe1 N2 C3 151(9) 3_666 . . . ?
N2 Fe1 N21 N22 -129.69(12) 3_666 . . . ?
N2 Fe1 N21 N22 50.31(12) . . . . ?
N2 Fe1 N21 C21 -132.09(18) . . . . ?
N2 Fe1 N21 C21 47.91(18) 3_666 . . . ?
N2 Fe1 N11 N12 -45.93(12) . . . . ?
N2 Fe1 N11 N12 134.08(12) 3_666 . . . ?
N2 Fe1 N11 C11 135.03(18) . . . . ?
N2 Fe1 N11 C11 -44.96(18) 3_666 . . . ?
N2 N1 C1 C2 -0.4(2) . . . . ?
N2 N1 C30 C31 148.67(16) . . . . ?
N2 C3 C4 N22 61.1(2) . . . . ?
N2 C3 C4 N12 -59.0(2) . . . . ?
N22 N21 C21 C22 -0.06(19) . . . . ?
N22 C23 C22 C21 0.1(2) . . . . ?
N21 Fe1 N2 N1 133.21(17) . . . . ?
N21 Fe1 N2 N1 -46.79(17) 3_666 . . . ?
N21 Fe1 N2 C3 -44.92(13) . . . . ?
N21 Fe1 N2 C3 135.08(13) 3_666 . . . ?
N21 Fe1 N21 N22 -135(32) 3_666 . . . ?
N21 Fe1 N21 C21 42(32) 3_666 . . . ?
N21 Fe1 N11 N12 39.70(12) . . . . ?
N21 Fe1 N11 N12 -140.30(12) 3_666 . . . ?
N21 Fe1 N11 C11 -139.34(18) . . . . ?
N21 Fe1 N11 C11 40.66(18) 3_666 . . . ?
N21 N22 C23 C22 -0.1(2) . . . . ?
N21 N22 C4 N12 64.86(19) . . . . ?
N21 N22 C4 C3 -55.51(19) . . . . ?
N12 N11 C11 C12 0.4(2) . . . . ?
N12 C13 C12 C11 -0.3(2) . . . . ?
N11 Fe1 N2 N1 -136.88(17) . . . . ?
N11 Fe1 N2 N1 43.12(17) 3_666 . . . ?
N11 Fe1 N2 C3 44.98(13) . . . . ?
N11 Fe1 N2 C3 -135.02(13) 3_666 . . . ?
N11 Fe1 N21 N22 -36.52(12) . . . . ?
N11 Fe1 N21 N22 143.48(12) 3_666 . . . ?
N11 Fe1 N21 C21 -38.93(18) 3_666 . . . ?
N11 Fe1 N21 C21 141.07(18) . . . . ?
N11 Fe1 N11 N12 42(4) 3_666 . . . ?
N11 Fe1 N11 C11 -137(4) 3_666 . . . ?
N11 N12 C13 C12 0.5(2) . . . . ?
N11 N12 C4 N22 -61.33(19) . . . . ?
N11 N12 C4 C3 58.59(19) . . . . ?
C1 N1 N2 Fe1 -177.92(14) . . . . ?
C1 N1 N2 C3 0.4(2) . . . . ?
C1 N1 C30 C31 -35.0(2) . . . . ?
C1 C2 C3 N2 0.0(2) . . . . ?
C1 C2 C3 C4 179.74(19) . . . . ?
C2 C3 C4 N22 -118.6(2) . . . . ?
C2 C3 C4 N12 121.3(2) . . . . ?
C23 N22 N21 Fe1 178.38(11) . . . . ?
C23 N22 N21 C21 0.11(19) . . . . ?
C23 N22 C4 N12 -122.95(18) . . . . ?
C23 N22 C4 C3 116.68(19) . . . . ?
C23 C22 C21 N21 0.0(2) . . . . ?
C13 N12 N11 Fe1 -179.88(12) . . . . ?
C13 N12 N11 C11 -0.57(19) . . . . ?
C13 N12 C4 N22 121.24(19) . . . . ?
C13 N12 C4 C3 -118.8(2) . . . . ?
C13 C12 C11 N11 -0.1(2) . . . . ?
C4 N22 N21 Fe1 -7.99(19) . . . . ?
C4 N22 N21 C21 173.74(14) . . . . ?
C4 N22 C23 C22 -172.72(17) . . . . ?
C4 N12 N11 Fe1 2.22(19) . . . . ?
C4 N12 N11 C11 -178.47(14) . . . . ?
C4 N12 C13 C12 178.08(17) . . . . ?
C30 N1 N2 Fe1 -1.0(3) . . . . ?
C30 N1 N2 C3 177.26(15) . . . . ?
C30 N1 C1 C2 -177.13(17) . . . . ?
C30 C31 C32 C33 -177.84(19) . . . . ?
C30 C31 C36 C35 177.78(17) . . . . ?
C31 C32 C33 C34 -0.2(3) . . . . ?
C32 C31 C36 C35 -0.9(3) . . . . ?
C32 C33 C34 C35 -0.4(3) . . . . ?
C33 C34 C35 C36 0.3(3) . . . . ?
C34 C35 C36 C31 0.3(3) . . . . ?
C36 C31 C32 C33 0.8(3) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-5 10 0 0.0137 -5.0018 10.0124 -0.0022 -0.0467 0.1288 1.0515
5 -10 0 0.0347 5.0018 -10.0124 0.0022 0.0467 -0.1288 -1.0515
4 12 0 0.0172 3.9993 11.9960 -0.0033 -0.9332 -0.2945 -0.1986
-4 -12 0 0.0272 -3.9993 -11.9960 0.0033 0.9332 0.2945 0.1986
-1 -4 6 0.1293 -1.0000 -3.9906 5.9990 -0.1885 0.9387 -0.4386
-1 7 -5 0.1398 -1.0007 6.9968 -5.0000 0.1400 -0.7350 0.7511
0 17 0 0.0075 -0.0018 17.0051 -0.0044 -0.8250 -0.1628 0.5463
2 14 -3 0.0766 1.9989 13.9961 -3.0027 -0.6196 -0.6516 0.3859

_olex2_date_sample_submission    2015-08-24
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_2_2CH3CN_TsL_BF4
_database_code_depnum_ccdc_archive 'CCDC 1478566'
_audit_update_record             
;
2016-07-14 deposited with the CCDC.
2016-07-26 downloaded from the CCDC.
;
_audit_creation_date             2016-02-22
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         
'C34 H32 Fe N12 O4 S2, B F4, 2(B0.5 F1.37), 2(C2 H3 N), 1.26(F)'
_chemical_formula_sum            'C38 H38 B2 F8 Fe N14 O4 S2'
_chemical_formula_weight         1048.41
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C34 H32 N12 S2 O4 Fe B2 F8 C H3 N'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z+1/2'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x, -y, z-1/2'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.4741(4)
_cell_length_b                   17.7632(3)
_cell_length_c                   10.49352(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.3163(17)
_cell_angle_gamma                90.00
_cell_volume                     4368.21(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10831
_cell_measurement_temperature    99.8(4)
_cell_measurement_theta_max      29.2190
_cell_measurement_theta_min      2.8910
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.5237
_exptl_crystal_size_mid          0.3004
_exptl_crystal_size_min          0.1559
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            24870
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.45
_diffrn_reflns_theta_min         2.85
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.8(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -100.00  -55.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5916  178.0000   30.0000 45

#__ type_ start__ end____ width___ exp.time_
  2 omega  -20.00   30.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5916  -99.0000  150.0000 50

#__ type_ start__ end____ width___ exp.time_
  3 omega   34.00  100.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6697 -178.0000  120.0000 66

#__ type_ start__ end____ width___ exp.time_
  4 omega  -35.00   93.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6697   19.0000 -150.0000 128

#__ type_ start__ end____ width___ exp.time_
  5 omega  -88.00   15.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5916  -37.0000 -120.0000 103

#__ type_ start__ end____ width___ exp.time_
  6 omega  -64.00  -25.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6697  -37.0000 -180.0000 39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0022449000
_diffrn_orient_matrix_UB_12      -0.0233651000
_diffrn_orient_matrix_UB_13      -0.0548882000
_diffrn_orient_matrix_UB_21      -0.0264026000
_diffrn_orient_matrix_UB_22      -0.0141520000
_diffrn_orient_matrix_UB_23      0.0193404000
_diffrn_orient_matrix_UB_31      -0.0146168000
_diffrn_orient_matrix_UB_32      0.0291371000
_diffrn_orient_matrix_UB_33      -0.0345972000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_number_gt                4575
_reflns_number_total             5524
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         5524
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0390
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0348P)²+8.5278P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0949
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uiso(N7) = Uiso(N7A)
Uiso(F4) = Uiso(F7) = Uiso(F3)
3. Same fragment restrains
{N7, C18, C19} sigma for 1-2: 0.02, 1-3: 0.04
as
{N7A, C18A, C19A}
4. Others
 Sof(N7A)=Sof(C18A)=Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=1-FVAR(1)
 Sof(N7)=Sof(C18)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(1)
 Sof(F7)=1-FVAR(2)
 Sof(F8)=Sof(F9)=0.5*(1-FVAR(3))
 Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=0.5*FVAR(3)
 Fixed Sof: B2(0.5)
5.a Ternary CH refined with riding coordinates:
 C1(H1)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C12(H12),
 C13(H13), C15(H15), C16(H16)
5.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C19A(H19D,H19E,H19F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Fe1 Fe 0.7500 0.7500 0.5000 0.01489(9) Uani 1 d . . 2 S T P
S1 S 0.732980(18) 0.56319(3) 0.24102(4) 0.01824(11) Uani 1 d . . 1 . . .
O1 O 0.70493(6) 0.50378(8) 0.17093(13) 0.0271(3) Uani 1 d . . 1 . . .
O2 O 0.74762(6) 0.63119(7) 0.17985(12) 0.0237(3) Uani 1 d . . 1 . . .
N22 N 0.62399(6) 0.78264(8) 0.50468(14) 0.0159(3) Uani 1 d . . 1 . . .
N21 N 0.67356(6) 0.81149(8) 0.46426(14) 0.0161(3) Uani 1 d . . 1 . . .
N12 N 0.66133(6) 0.71329(8) 0.68691(14) 0.0159(3) Uani 1 d . . 1 . . .
N11 N 0.71885(6) 0.71766(8) 0.67785(14) 0.0161(3) Uani 1 d . . 1 . . .
N2 N 0.68873(6) 0.64869(8) 0.42563(13) 0.0152(3) Uani 1 d . . 1 . . .
N1 N 0.68555(6) 0.58481(8) 0.35207(14) 0.0179(3) Uani 1 d . . 1 . . .
C4 C 0.62407(7) 0.71071(10) 0.57156(16) 0.0150(3) Uani 1 d . . 1 . . .
H4 H 0.5844 0.7011 0.5974 0.018 Uiso 1 calc . . 1 R . .
C23 C 0.57845(7) 0.82232(10) 0.45812(17) 0.0205(4) Uani 1 d . . 1 . . .
H23 H 0.5396 0.8123 0.4723 0.025 Uiso 1 calc . . 1 R . .
C22 C 0.59882(8) 0.87978(11) 0.38648(18) 0.0233(4) Uani 1 d . . 1 . . .
H22 H 0.5772 0.9176 0.3416 0.028 Uiso 1 calc . . 1 R . .
C21 C 0.65783(8) 0.87110(10) 0.39326(17) 0.0193(4) Uani 1 d . . 1 . . .
H21 H 0.6835 0.9033 0.3527 0.023 Uiso 1 calc . . 1 R . .
C13 C 0.64760(8) 0.70346(10) 0.80911(17) 0.0202(4) Uani 1 d . . 1 . . .
H13 H 0.6102 0.6986 0.8384 0.024 Uiso 1 calc . . 1 R . .
C12 C 0.69781(8) 0.70180(11) 0.88282(17) 0.0210(4) Uani 1 d . . 1 . . .
H12 H 0.7024 0.6958 0.9728 0.025 Uiso 1 calc . . 1 R . .
C11 C 0.74081(8) 0.71083(10) 0.79706(16) 0.0186(4) Uani 1 d . . 1 . . .
H11 H 0.7805 0.7119 0.8208 0.022 Uiso 1 calc . . 1 R . .
C3 C 0.63991(7) 0.64765(10) 0.48485(16) 0.0161(3) Uani 1 d . . 1 . . .
C2 C 0.60601(8) 0.58513(11) 0.4519(2) 0.0246(4) Uani 1 d . . 1 . . .
H2 H 0.5699 0.5726 0.4826 0.030 Uiso 1 calc . . 1 R . .
C1 C 0.63590(8) 0.54607(11) 0.3662(2) 0.0251(4) Uani 1 d . . 1 . . .
H1 H 0.6245 0.5007 0.3242 0.030 Uiso 1 calc . . 1 R . .
C31 C 0.79282(7) 0.52703(10) 0.32684(16) 0.0167(3) Uani 1 d . . 1 . . .
C32 C 0.84609(8) 0.55614(10) 0.30366(17) 0.0198(4) Uani 1 d . . 1 . . .
H32 H 0.8496 0.6005 0.2542 0.024 Uiso 1 calc . . 1 R . .
C33 C 0.89403(8) 0.51874(11) 0.35460(18) 0.0225(4) Uani 1 d . . 1 . . .
H33 H 0.9308 0.5378 0.3395 0.027 Uiso 1 calc . . 1 R . .
C34 C 0.88923(8) 0.45393(11) 0.42737(19) 0.0235(4) Uani 1 d . . 1 . . .
C35 C 0.83506(8) 0.42749(11) 0.45266(18) 0.0223(4) Uani 1 d . . 1 . . .
H35 H 0.8315 0.3843 0.5050 0.027 Uiso 1 calc . . 1 R . .
C36 C 0.78659(8) 0.46339(10) 0.40241(16) 0.0190(4) Uani 1 d . . 1 . . .
H36 H 0.7497 0.4450 0.4191 0.023 Uiso 1 calc . . 1 R . .
C37 C 0.94169(9) 0.41253(13) 0.4780(2) 0.0377(5) Uani 1 d . . 1 . . .
H37a H 0.9458 0.4181 0.5710 0.057 Uiso 1 calc . . 1 GR . .
H37b H 0.9754 0.4335 0.4399 0.057 Uiso 1 calc . . 1 GR . .
H37c H 0.9381 0.3590 0.4561 0.057 Uiso 1 calc . . 1 GR . .
F1 F 0.49078(5) 0.74737(7) 0.64145(12) 0.0327(3) Uani 1 d . . 1 . . .
F2 F 0.54781(8) 0.83451(10) 0.73452(14) 0.0663(5) Uani 1 d . . 1 . . .
B1 B 0.5000 0.79182(18) 0.7500 0.0276(7) Uani 1 d . . 2 S T P
F3 F 0.5523(3) 0.5935(3) 0.7424(6) 0.0241(5) Uiso 0.343(3) d A -1 1 . . .
F4 F 0.46331(16) 0.5963(2) 0.8198(4) 0.0241(5) Uiso 0.343(3) d A -1 1 . . .
F5 F 0.50524(18) 0.48622(15) 0.7682(5) 0.0203(8) Uiso 0.343(3) d A -1 1 . . .
F6 F 0.47279(17) 0.5686(2) 0.6101(3) 0.0332(10) Uiso 0.343(3) d A -1 1 . . .
B2 B 0.4982(3) 0.56085(18) 0.7337(5) 0.0179(8) Uiso 0.50 d A -1 1 . . .
N7 N 0.6147(2) 0.7310(3) 0.1770(5) 0.0416(7) Uiso 0.573(5) d B 1 1 D . .
C18 C 0.5953(2) 0.6806(3) 0.1259(5) 0.0261(10) Uani 0.573(5) d B 1 1 D . .
C19 C 0.5738(2) 0.6121(2) 0.0635(4) 0.0411(12) Uani 0.573(5) d B 1 1 D . .
H19a H 0.5490 0.6253 -0.0114 0.062 Uiso 0.573(5) calc B 1 1 GR . .
H19b H 0.5521 0.5829 0.1233 0.062 Uiso 0.573(5) calc B 1 1 GR . .
H19c H 0.6060 0.5819 0.0367 0.062 Uiso 0.573(5) calc B 1 1 GR . .
N7A N 0.6230(3) 0.7371(4) 0.1501(7) 0.0416(7) Uiso 0.427(5) d B 2 1 D . .
C18A C 0.5810(2) 0.7062(4) 0.1486(7) 0.0274(14) Uani 0.427(5) d B 2 1 D . .
C19A C 0.5256(2) 0.6706(3) 0.1371(5) 0.0374(15) Uani 0.427(5) d B 2 1 D . .
H19d H 0.5140 0.6638 0.0466 0.056 Uiso 0.427(5) calc B 2 1 GR . .
H19e H 0.4977 0.7024 0.1774 0.056 Uiso 0.427(5) calc B 2 1 GR . .
H19f H 0.5276 0.6215 0.1795 0.056 Uiso 0.427(5) calc B 2 1 GR . .
F7 F 0.5479(3) 0.6024(4) 0.7294(7) 0.0241(5) Uiso 0.315(7) d A 2 1 . . .
F8 F 0.4916(4) 0.4991(6) 0.6750(12) 0.037(2) Uiso 0.157(3) d A -2 1 . . .
F9 F 0.5108(4) 0.5309(6) 0.8844(9) 0.037(2) Uiso 0.157(3) d A -2 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 N21 2.1156(14) . ?
Fe1 N21 2.1156(14) 7_666 ?
Fe1 N11 2.1227(14) 7_666 ?
Fe1 N11 2.1227(14) . ?
Fe1 N2 2.4055(14) . ?
Fe1 N2 2.4056(14) 7_666 ?
S1 O1 1.4255(14) . ?
S1 O2 1.4194(14) . ?
S1 N1 1.7015(15) . ?
S1 C31 1.7464(18) . ?
N22 N21 1.3614(19) . ?
N22 C4 1.458(2) . ?
N22 C23 1.348(2) . ?
N21 C21 1.334(2) . ?
N12 N11 1.3611(19) . ?
N12 C4 1.453(2) . ?
N12 C13 1.351(2) . ?
N11 C11 1.331(2) . ?
N2 N1 1.372(2) . ?
N2 C3 1.335(2) . ?
N1 C1 1.369(2) . ?
C4 H4 1.0000 . ?
C4 C3 1.503(2) . ?
C23 H23 0.9500 . ?
C23 C22 1.370(3) . ?
C22 H22 0.9500 . ?
C22 C21 1.391(3) . ?
C21 H21 0.9500 . ?
C13 H13 0.9500 . ?
C13 C12 1.372(3) . ?
C12 H12 0.9500 . ?
C12 C11 1.400(2) . ?
C11 H11 0.9500 . ?
C3 C2 1.398(3) . ?
C2 H2 0.9500 . ?
C2 C1 1.362(3) . ?
C1 H1 0.9500 . ?
C31 C32 1.388(2) . ?
C31 C36 1.393(2) . ?
C32 H32 0.9500 . ?
C32 C33 1.387(3) . ?
C33 H33 0.9500 . ?
C33 C34 1.390(3) . ?
C34 C35 1.395(3) . ?
C34 C37 1.505(3) . ?
C35 H35 0.9500 . ?
C35 C36 1.382(3) . ?
C36 H36 0.9500 . ?
C37 H37a 0.9800 . ?
C37 H37b 0.9800 . ?
C37 H37c 0.9800 . ?
F1 B1 1.393(2) . ?
F2 B1 1.372(2) . ?
B1 F1 1.393(2) 2_656 ?
B1 F2 1.372(2) 2_656 ?
F3 B2 1.393(9) . ?
F4 B2 1.404(7) . ?
F5 B2 1.382(4) . ?
F6 B2 1.402(6) . ?
N7 C18 1.126(6) . ?
C18 C19 1.459(6) . ?
C19 H19a 0.9800 . ?
C19 H19b 0.9800 . ?
C19 H19c 0.9800 . ?
N7A C18A 1.128(8) . ?
C18A C19A 1.444(7) . ?
C19A H19d 0.9800 . ?
C19A H19e 0.9800 . ?
C19A H19f 0.9800 . ?

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
N21 Fe1 N21 179.998(1) . 7_666 ?
N21 Fe1 N11 87.92(5) . . ?
N21 Fe1 N11 92.08(5) . 7_666 ?
N21 Fe1 N11 92.08(5) 7_666 . ?
N21 Fe1 N11 87.92(5) 7_666 7_666 ?
N21 Fe1 N2 99.00(5) 7_666 . ?
N21 Fe1 N2 81.00(5) 7_666 7_666 ?
N21 Fe1 N2 99.00(5) . 7_666 ?
N21 Fe1 N2 81.00(5) . . ?
N11 Fe1 N11 179.999(2) 7_666 . ?
N11 Fe1 N2 81.54(5) . . ?
N11 Fe1 N2 98.46(5) . 7_666 ?
N11 Fe1 N2 81.54(5) 7_666 7_666 ?
N11 Fe1 N2 98.46(5) 7_666 . ?
N2 Fe1 N2 179.999(1) . 7_666 ?
O1 S1 N1 102.68(8) . . ?
O1 S1 C31 109.12(8) . . ?
O2 S1 O1 120.89(8) . . ?
O2 S1 N1 107.62(8) . . ?
O2 S1 C31 109.73(8) . . ?
N1 S1 C31 105.57(8) . . ?
N21 N22 C4 120.17(13) . . ?
C23 N22 N21 111.37(14) . . ?
C23 N22 C4 127.71(14) . . ?
N22 N21 Fe1 118.81(11) . . ?
C21 N21 Fe1 135.48(12) . . ?
C21 N21 N22 105.00(14) . . ?
N11 N12 C4 119.70(13) . . ?
C13 N12 N11 111.45(14) . . ?
C13 N12 C4 128.42(14) . . ?
N12 N11 Fe1 118.06(10) . . ?
C11 N11 Fe1 135.79(12) . . ?
C11 N11 N12 105.13(14) . . ?
N1 N2 Fe1 144.41(11) . . ?
C3 N2 Fe1 111.87(11) . . ?
C3 N2 N1 103.32(14) . . ?
N2 N1 S1 123.75(12) . . ?
C1 N1 S1 123.74(13) . . ?
C1 N1 N2 111.95(14) . . ?
N22 C4 H4 107.7 . . ?
N22 C4 C3 110.80(14) . . ?
N12 C4 N22 110.95(14) . . ?
N12 C4 H4 107.7 . . ?
N12 C4 C3 111.70(13) . . ?
C3 C4 H4 107.7 . . ?
N22 C23 H23 126.5 . . ?
N22 C23 C22 107.08(16) . . ?
C22 C23 H23 126.5 . . ?
C23 C22 H22 127.2 . . ?
C23 C22 C21 105.52(16) . . ?
C21 C22 H22 127.2 . . ?
N21 C21 C22 111.03(16) . . ?
N21 C21 H21 124.5 . . ?
C22 C21 H21 124.5 . . ?
N12 C13 H13 126.5 . . ?
N12 C13 C12 107.06(15) . . ?
C12 C13 H13 126.5 . . ?
C13 C12 H12 127.4 . . ?
C13 C12 C11 105.24(16) . . ?
C11 C12 H12 127.4 . . ?
N11 C11 C12 111.12(16) . . ?
N11 C11 H11 124.4 . . ?
C12 C11 H11 124.4 . . ?
N2 C3 C4 121.37(15) . . ?
N2 C3 C2 112.79(16) . . ?
C2 C3 C4 125.77(15) . . ?
C3 C2 H2 127.4 . . ?
C1 C2 C3 105.11(16) . . ?
C1 C2 H2 127.4 . . ?
N1 C1 H1 126.6 . . ?
C2 C1 N1 106.83(16) . . ?
C2 C1 H1 126.6 . . ?
C32 C31 S1 118.60(14) . . ?
C32 C31 C36 121.82(16) . . ?
C36 C31 S1 118.95(13) . . ?
C31 C32 H32 120.9 . . ?
C33 C32 C31 118.25(17) . . ?
C33 C32 H32 120.9 . . ?
C32 C33 H33 119.4 . . ?
C32 C33 C34 121.24(17) . . ?
C34 C33 H33 119.4 . . ?
C33 C34 C35 119.15(17) . . ?
C33 C34 C37 120.54(18) . . ?
C35 C34 C37 120.30(18) . . ?
C34 C35 H35 119.6 . . ?
C36 C35 C34 120.75(17) . . ?
C36 C35 H35 119.6 . . ?
C31 C36 H36 120.6 . . ?
C35 C36 C31 118.71(16) . . ?
C35 C36 H36 120.6 . . ?
C34 C37 H37a 109.5 . . ?
C34 C37 H37b 109.5 . . ?
C34 C37 H37c 109.5 . . ?
H37a C37 H37b 109.5 . . ?
H37a C37 H37c 109.5 . . ?
H37b C37 H37c 109.5 . . ?
F1 B1 F1 110.9(2) . 2_656 ?
F2 B1 F1 108.71(9) . 2_656 ?
F2 B1 F1 108.71(9) 2_656 . ?
F2 B1 F1 107.82(8) 2_656 2_656 ?
F2 B1 F1 107.82(8) . . ?
F2 B1 F2 112.9(3) . 2_656 ?
F3 B2 F4 109.5(4) . . ?
F3 B2 F6 110.9(5) . . ?
F5 B2 F3 106.8(5) . . ?
F5 B2 F4 109.1(4) . . ?
F5 B2 F6 112.0(4) . . ?
F6 B2 F4 108.5(4) . . ?
N7 C18 C19 175.6(6) . . ?
N7A C18A C19A 175.0(8) . . ?
C18A C19A H19d 109.5 . . ?
C18A C19A H19e 109.5 . . ?
C18A C19A H19f 109.5 . . ?
H19d C19A H19e 109.5 . . ?
H19d C19A H19f 109.5 . . ?
H19e C19A H19f 109.5 . . ?

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 N21 C21 C22 168.82(13) . . . . ?
Fe1 N11 C11 C12 167.85(13) . . . . ?
Fe1 N2 N1 S1 -16.7(3) . . . . ?
Fe1 N2 N1 C1 171.55(15) . . . . ?
Fe1 N2 C3 C4 8.59(19) . . . . ?
Fe1 N2 C3 C2 -174.33(12) . . . . ?
S1 N1 C1 C2 -172.29(14) . . . . ?
S1 C31 C32 C33 -168.80(14) . . . . ?
S1 C31 C36 C35 169.16(14) . . . . ?
O1 S1 N1 N2 -166.59(14) . . . . ?
O1 S1 N1 C1 4.22(17) . . . . ?
O1 S1 C31 C32 120.63(15) . . . . ?
O1 S1 C31 C36 -50.49(16) . . . . ?
O2 S1 N1 N2 -38.01(16) . . . . ?
O2 S1 N1 C1 132.80(16) . . . . ?
O2 S1 C31 C32 -13.92(16) . . . . ?
O2 S1 C31 C36 174.96(13) . . . . ?
N22 N21 C21 C22 -0.9(2) . . . . ?
N22 C4 C3 N2 56.2(2) . . . . ?
N22 C4 C3 C2 -120.47(19) . . . . ?
N22 C23 C22 C21 0.4(2) . . . . ?
N21 Fe1 N21 N22 64(25) 7_666 . . . ?
N21 Fe1 N21 C21 -105(25) 7_666 . . . ?
N21 Fe1 N11 N12 28.40(12) . . . . ?
N21 Fe1 N11 N12 -151.59(12) 7_666 . . . ?
N21 Fe1 N11 C11 41.97(18) 7_666 . . . ?
N21 Fe1 N11 C11 -138.04(18) . . . . ?
N21 Fe1 N2 N1 139.43(19) . . . . ?
N21 Fe1 N2 N1 -40.57(19) 7_666 . . . ?
N21 Fe1 N2 C3 130.41(12) 7_666 . . . ?
N21 Fe1 N2 C3 -49.59(12) . . . . ?
N21 N22 C4 N12 58.96(19) . . . . ?
N21 N22 C4 C3 -65.72(19) . . . . ?
N21 N22 C23 C22 -1.0(2) . . . . ?
N12 N11 C11 C12 0.2(2) . . . . ?
N12 C4 C3 N2 -68.0(2) . . . . ?
N12 C4 C3 C2 115.28(19) . . . . ?
N12 C13 C12 C11 -0.2(2) . . . . ?
N11 Fe1 N21 N22 -36.66(12) . . . . ?
N11 Fe1 N21 N22 143.34(12) 7_666 . . . ?
N11 Fe1 N21 C21 154.66(17) . . . . ?
N11 Fe1 N21 C21 -25.34(17) 7_666 . . . ?
N11 Fe1 N11 N12 134(100) 7_666 . . . ?
N11 Fe1 N11 C11 -33(100) 7_666 . . . ?
N11 Fe1 N2 N1 -131.34(19) . . . . ?
N11 Fe1 N2 N1 48.66(19) 7_666 . . . ?
N11 Fe1 N2 C3 39.63(12) . . . . ?
N11 Fe1 N2 C3 -140.37(12) 7_666 . . . ?
N11 N12 C4 N22 -69.27(19) . . . . ?
N11 N12 C4 C3 54.9(2) . . . . ?
N11 N12 C13 C12 0.4(2) . . . . ?
N2 Fe1 N21 N22 -134.91(12) 7_666 . . . ?
N2 Fe1 N21 N22 45.09(12) . . . . ?
N2 Fe1 N21 C21 56.42(17) 7_666 . . . ?
N2 Fe1 N21 C21 -123.58(17) . . . . ?
N2 Fe1 N11 N12 -52.81(12) . . . . ?
N2 Fe1 N11 N12 127.19(12) 7_666 . . . ?
N2 Fe1 N11 C11 140.75(18) . . . . ?
N2 Fe1 N11 C11 -39.25(18) 7_666 . . . ?
N2 Fe1 N2 N1 -34(15) 7_666 . . . ?
N2 Fe1 N2 C3 137(15) 7_666 . . . ?
N2 N1 C1 C2 -0.5(2) . . . . ?
N2 C3 C2 C1 -0.6(2) . . . . ?
N1 S1 C31 C32 -129.63(14) . . . . ?
N1 S1 C31 C36 59.25(15) . . . . ?
N1 N2 C3 C4 -176.79(15) . . . . ?
N1 N2 C3 C2 0.29(19) . . . . ?
C4 N22 N21 Fe1 0.15(19) . . . . ?
C4 N22 N21 C21 171.96(15) . . . . ?
C4 N22 C23 C22 -170.89(16) . . . . ?
C4 N12 N11 Fe1 16.28(19) . . . . ?
C4 N12 N11 C11 -173.47(15) . . . . ?
C4 N12 C13 C12 172.72(16) . . . . ?
C4 C3 C2 C1 176.32(17) . . . . ?
C23 N22 N21 Fe1 -170.64(12) . . . . ?
C23 N22 N21 C21 1.16(19) . . . . ?
C23 N22 C4 N12 -131.90(17) . . . . ?
C23 N22 C4 C3 103.42(19) . . . . ?
C23 C22 C21 N21 0.4(2) . . . . ?
C13 N12 N11 Fe1 -170.63(12) . . . . ?
C13 N12 N11 C11 -0.38(19) . . . . ?
C13 N12 C4 N22 118.94(18) . . . . ?
C13 N12 C4 C3 -116.88(19) . . . . ?
C13 C12 C11 N11 0.0(2) . . . . ?
C3 N2 N1 S1 171.92(12) . . . . ?
C3 N2 N1 C1 0.15(19) . . . . ?
C3 C2 C1 N1 0.7(2) . . . . ?
C31 S1 N1 N2 79.13(15) . . . . ?
C31 S1 N1 C1 -110.06(16) . . . . ?
C31 C32 C33 C34 -0.2(3) . . . . ?
C32 C31 C36 C35 -1.7(3) . . . . ?
C32 C33 C34 C35 -2.0(3) . . . . ?
C32 C33 C34 C37 177.82(19) . . . . ?
C33 C34 C35 C36 2.4(3) . . . . ?
C34 C35 C36 C31 -0.6(3) . . . . ?
C36 C31 C32 C33 2.0(3) . . . . ?
C37 C34 C35 C36 -177.42(19) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-33 0 -1 0.0955 -33.0000 -0.0000 -1.0000 0.1290 0.8519 0.5170
33 0 1 0.0605 33.0000 0.0000 1.0000 -0.1290 -0.8519 -0.5170
9 12 12 0.0756 8.9999 11.9999 11.9999 -0.9592 -0.1754 -0.1971
-7 -5 -14 0.1088 -6.9999 -4.9999 -13.9999 0.9010 -0.0152 0.4410
9 -13 12 0.1422 9.0000 -13.0001 12.0000 -0.3751 0.1784 -0.9255
24 -17 1 0.1819 24.0001 -17.0000 1.0000 0.2884 -0.3737 -0.8807
-29 10 -3 0.1396 -29.0000 10.0000 -3.0000 -0.0039 0.5661 0.8191
20 20 0 0.1989 20.0000 20.0001 -0.0000 -0.5122 -0.8111 0.2904
-15 12 -11 0.1623 -15.0000 12.0001 -11.0000 0.3571 0.0135 0.9495
-17 -21 -2 0.2268 -17.0000 -21.0001 -2.0000 0.6386 0.7074 -0.2942

_olex2_date_sample_data_collection 2016-02-20
_olex2_date_sample_submission    2016-02-19
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_3_HL_BF4
_database_code_depnum_ccdc_archive 'CCDC 1478567'
_audit_update_record             
;
2016-07-14 deposited with the CCDC.
2016-07-26 downloaded from the CCDC.
;
_audit_creation_date             2016-04-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C20 H20 Fe N12, 2(B F4)'
_chemical_formula_sum            'C20 H20 B2 F8 Fe N12'
_chemical_formula_weight         657.95
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C20 H20 Fe B2 F8'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.0567(3)
_cell_length_b                   7.6103(2)
_cell_length_c                   17.2769(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.843(3)
_cell_angle_gamma                90.00
_cell_volume                     1309.91(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6136
_cell_measurement_temperature    99.95(10)
_cell_measurement_theta_max      73.7170
_cell_measurement_theta_min      4.7870
_exptl_absorpt_coefficient_mu    5.490
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.520
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.2926
_exptl_crystal_size_mid          0.0371
_exptl_crystal_size_min          0.0201
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5451
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         74.20
_diffrn_reflns_theta_min         4.82
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -124.00  -79.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  -99.0000    0.0000 90

#__ type_ start__ end____ width___ exp.time_
  2 omega -124.00  -79.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  -99.0000   90.0000 90

#__ type_ start__ end____ width___ exp.time_
  3 omega -115.00  -12.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  -57.0000  -30.0000 206

#__ type_ start__ end____ width___ exp.time_
  4 omega -124.00  -79.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  -99.0000   60.0000 90

#__ type_ start__ end____ width___ exp.time_
  5 omega  -71.00   33.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987   57.0000  120.0000 208

#__ type_ start__ end____ width___ exp.time_
  6 omega    1.00   83.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.3987  -99.0000  -90.0000 164

#__ type_ start__ end____ width___ exp.time_
  7 omega   23.00   99.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.3987 -125.0000 -120.0000 152

#__ type_ start__ end____ width___ exp.time_
  8 omega   24.00  109.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -94.0000   30.0000 170

#__ type_ start__ end____ width___ exp.time_
  9 omega   34.00   98.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -45.0000    0.0000 128

#__ type_ start__ end____ width___ exp.time_
 10 omega   24.00  109.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -94.0000  -30.0000 170

#__ type_ start__ end____ width___ exp.time_
 11 omega   34.00   98.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -45.0000 -120.0000 128

#__ type_ start__ end____ width___ exp.time_
 12 omega   33.00  122.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878 -125.0000  150.0000 178

#__ type_ start__ end____ width___ exp.time_
 13 omega   30.00   90.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -30.0000   90.0000 120

#__ type_ start__ end____ width___ exp.time_
 14 omega   30.00   90.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -30.0000  -90.0000 120

#__ type_ start__ end____ width___ exp.time_
 15 omega   30.00   90.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -30.0000  120.0000 120

#__ type_ start__ end____ width___ exp.time_
 16 omega   34.00   98.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -45.0000 -180.0000 128

#__ type_ start__ end____ width___ exp.time_
 17 omega   78.00  178.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   30.0000  -60.0000 200

#__ type_ start__ end____ width___ exp.time_
 18 omega   33.00  122.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878 -125.0000  -60.0000 178

#__ type_ start__ end____ width___ exp.time_
 19 omega   30.00  142.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -77.0000  120.0000 224

#__ type_ start__ end____ width___ exp.time_
 20 omega   25.00  170.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -15.0000  -60.0000 290

#__ type_ start__ end____ width___ exp.time_
 21 omega -124.00  -79.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  -99.0000  150.0000 90

#__ type_ start__ end____ width___ exp.time_
 22 omega -124.00  -79.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  -99.0000 -150.0000 90

#__ type_ start__ end____ width___ exp.time_
 23 omega -115.00  -12.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  -57.0000  150.0000 206

#__ type_ start__ end____ width___ exp.time_
 24 omega -115.00  -12.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  -57.0000 -120.0000 206

#__ type_ start__ end____ width___ exp.time_
 25 omega -115.00  -12.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  -57.0000   60.0000 206

#__ type_ start__ end____ width___ exp.time_
 26 omega   47.00  178.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   15.0000 -150.0000 262

#__ type_ start__ end____ width___ exp.time_
 27 omega   78.00  178.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   61.0000  -60.0000 200

#__ type_ start__ end____ width___ exp.time_
 28 omega   47.00  178.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   15.0000   90.0000 262

#__ type_ start__ end____ width___ exp.time_
 29 omega   75.00  178.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   77.0000 -180.0000 206

#__ type_ start__ end____ width___ exp.time_
 30 omega   78.00  178.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   61.0000   90.0000 200

#__ type_ start__ end____ width___ exp.time_
 31 omega   81.00  178.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   45.0000 -120.0000 194

#__ type_ start__ end____ width___ exp.time_
 32 omega   78.00  178.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   61.0000   60.0000 200

#__ type_ start__ end____ width___ exp.time_
 33 omega   78.00  178.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   61.0000  120.0000 200

#__ type_ start__ end____ width___ exp.time_
 34 omega   75.00  178.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   77.0000    0.0000 206

#__ type_ start__ end____ width___ exp.time_
 35 omega   78.00  178.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   61.0000  -30.0000 200

#__ type_ start__ end____ width___ exp.time_
 36 omega    1.00   83.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.3987  -99.0000   30.0000 164
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0196424000
_diffrn_orient_matrix_UB_12      0.1861738000
_diffrn_orient_matrix_UB_13      0.0315175000
_diffrn_orient_matrix_UB_21      0.0429754000
_diffrn_orient_matrix_UB_22      0.0793181000
_diffrn_orient_matrix_UB_23      -0.0748255000
_diffrn_orient_matrix_UB_31      -0.1472576000
_diffrn_orient_matrix_UB_32      -0.0020781000
_diffrn_orient_matrix_UB_33      -0.0388623000
loop_
_diffrn_oxdiff_twin_id
_diffrn_oxdiff_twin_ratio
_diffrn_oxdiff_twin_reflns_isolated
_diffrn_oxdiff_twin_reflns_overlapped
1 0.5073 14986 9490
2 0.4927 15016 9490

_diffrn_oxdiff_twin_integration_method simultaneous
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_number_gt                4977
_reflns_number_total             5451
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5451
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0454
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0767P)²+0.6176P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1257
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.5083(10) 0.4917(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
3. Shared sites
{N3, C8A}
{N3A, C8}
{C7, N5A}
{C7A, N5}
4. Rigid bond restraints
 F1, F2, F3, F4, B1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F1A, F2A, F3A, F4A, B1A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(N3) = Uanis(C8A)
Uanis(N3A) = Uanis(C8)
Uanis(C7) = Uanis(N5A)
Uanis(C7A) = Uanis(N5)
6. Same fragment restrains
{F1, F2, F3, F4, B1} sigma for 1-2: 0.02, 1-3: 0.04
as
{F1A, F2A, F3A, F4A, B1A}
7. Others
 Sof(H1B)=Sof(C8A)=Sof(H5B)=Sof(H6B)=Sof(N5A)=Sof(H5AA)=Sof(C7A)=Sof(H7A)=
 Sof(N3A)=Sof(H9B)=Sof(H10A)=1-FVAR(1)
 Sof(H1A)=Sof(N3)=Sof(H5A)=Sof(H6A)=Sof(C7)=Sof(H7)=Sof(N5)=Sof(H5)=Sof(C8)=
 Sof(H9A)=Sof(H10)=FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(B1A)=1-FVAR(2)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(B1)=FVAR(2)
8.a Ternary CH refined with riding coordinates:
 C1(H1A), C1(H1B)
8.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5A), C5(H5B), C6(H6A), C6(H6B), C7(H7), N5A(H5AA),
  N5(H5), C7A(H7A), C9(H9A), C9(H9B), C10(H10), C10(H10A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Fe1 Fe 0.5000 0.5000 0.5000 0.02253(12) Uani 1 d . . 2 S T P
C1 C 0.72940(18) 0.6523(2) 0.42505(11) 0.0260(4) Uani 1 d . . 1 . . .
H1A H 0.8053 0.7027 0.4004 0.031 Uiso 0.643(15) calc A 1 1 R . .
H1B H 0.8053 0.7027 0.4004 0.031 Uiso 0.357(15) calc A 2 1 R . .
N1 N 0.73576(15) 0.4611(2) 0.42307(9) 0.0262(3) Uani 1 d A . 1 . . .
N2 N 0.63993(15) 0.3692(2) 0.45432(9) 0.0258(3) Uani 1 d . . 1 . . .
C2 C 0.82561(18) 0.3524(3) 0.39544(11) 0.0286(4) Uani 1 d . . 1 . . .
H2 H 0.9010 0.3862 0.3712 0.034 Uiso 1 calc A . 1 R . .
C3 C 0.78598(19) 0.1843(3) 0.40937(12) 0.0310(4) Uani 1 d A . 1 . . .
H3 H 0.8282 0.0782 0.3970 0.037 Uiso 1 calc . . 1 R . .
C4 C 0.67090(19) 0.2013(3) 0.44544(12) 0.0275(4) Uani 1 d A . 1 . . .
H4 H 0.6210 0.1053 0.4616 0.033 Uiso 1 calc . . 1 R . .
N3 N 0.60153(16) 0.7108(2) 0.38186(10) 0.0255(4) Uani 0.643(15) d A 1 1 . . .
C8A C 0.60153(16) 0.7108(2) 0.38186(10) 0.0255(4) Uani 0.357(15) d A 2 1 . . .
N4 N 0.48750(15) 0.6561(2) 0.40846(9) 0.0254(3) Uani 1 d . . 1 . . .
C5 C 0.5729(2) 0.8199(3) 0.31926(11) 0.0316(4) Uani 1 d . . 1 . . .
H5A H 0.6356 0.8747 0.2906 0.038 Uiso 0.643(15) calc A 1 1 R . .
H5B H 0.6356 0.8747 0.2906 0.038 Uiso 0.357(15) calc A 2 1 R . .
C6 C 0.4364(2) 0.8349(3) 0.30579(12) 0.0334(4) Uani 1 d A . 1 . . .
H6A H 0.3854 0.9028 0.2662 0.040 Uiso 0.643(15) calc A 1 1 R . .
H6B H 0.3854 0.9028 0.2662 0.040 Uiso 0.357(15) calc A 2 1 R . .
C7 C 0.38696(18) 0.7315(3) 0.36148(11) 0.0297(4) Uani 0.643(15) d A 1 1 . . .
H7 H 0.2944 0.7163 0.3657 0.036 Uiso 0.643(15) calc A 1 1 R . .
N5A N 0.38696(18) 0.7315(3) 0.36148(11) 0.0297(4) Uani 0.357(15) d A 2 1 . . .
H5AA H 0.3013 0.7174 0.3653 0.036 Uiso 0.357(15) calc A 2 1 R . .
N5 N 0.67305(17) 0.7280(2) 0.61994(10) 0.0291(4) Uani 0.643(15) d A 1 1 . . .
H5 H 0.6267 0.7121 0.6590 0.035 Uiso 0.643(15) calc A 1 1 R . .
C7A C 0.67305(17) 0.7280(2) 0.61994(10) 0.0291(4) Uani 0.357(15) d A 2 1 . . .
H7A H 0.6230 0.7108 0.6621 0.035 Uiso 0.357(15) calc A 2 1 R . .
N6 N 0.64351(15) 0.6546(2) 0.54879(9) 0.0259(3) Uani 1 d . . 1 . . .
C8 C 0.73915(16) 0.7118(2) 0.50668(11) 0.0257(4) Uani 0.643(15) d A 1 1 . . .
N3A N 0.73915(16) 0.7118(2) 0.50668(11) 0.0257(4) Uani 0.357(15) d A 2 1 . . .
C9 C 0.82856(19) 0.8208(3) 0.55103(13) 0.0324(4) Uani 1 d . . 1 . . .
H9A H 0.9045 0.8773 0.5351 0.039 Uiso 0.643(15) calc A 1 1 R . .
H9B H 0.9045 0.8773 0.5351 0.039 Uiso 0.357(15) calc A 2 1 R . .
C10 C 0.7856(2) 0.8312(3) 0.62304(13) 0.0336(4) Uani 1 d A . 1 . . .
H10 H 0.8261 0.8972 0.6667 0.040 Uiso 0.643(15) calc A 1 1 R . .
H10A H 0.8261 0.8972 0.6667 0.040 Uiso 0.357(15) calc A 2 1 R . .
F1 F 0.5902(6) 0.8898(6) 0.8503(4) 0.0750(18) Uani 0.655(17) d B 1 1 D U .
F2 F 0.5838(3) 0.6580(6) 0.7699(3) 0.0505(11) Uani 0.655(17) d B 1 1 D U .
F3 F 0.3962(7) 0.8221(9) 0.7819(4) 0.0580(15) Uani 0.655(17) d B 1 1 D U .
F4 F 0.4808(15) 0.6405(13) 0.8782(6) 0.0409(17) Uani 0.655(17) d B 1 1 D U .
B1 B 0.5114(8) 0.7509(10) 0.8187(5) 0.0361(18) Uani 0.655(17) d B 1 1 D U .
F1A F 0.5855(12) 0.864(2) 0.8191(11) 0.112(5) Uani 0.345(17) d B 2 1 D U .
F2A F 0.538(3) 0.620(2) 0.7507(10) 0.133(6) Uani 0.345(17) d B 2 1 D U .
F3A F 0.3738(11) 0.791(2) 0.7762(9) 0.059(3) Uani 0.345(17) d B 2 1 D U .
F4A F 0.497(3) 0.646(3) 0.8775(10) 0.042(3) Uani 0.345(17) d B 2 1 D U .
B1A B 0.4947(16) 0.727(2) 0.8057(10) 0.044(4) Uani 0.345(17) d B 2 1 D U .


_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 1.9740(15) . ?
Fe1 N2 1.9740(15) 3_666 ?
Fe1 N4 1.9685(15) . ?
Fe1 N4 1.9684(15) 3_666 ?
Fe1 N6 1.9612(16) . ?
Fe1 N6 1.9612(16) 3_666 ?
C1 H1A 1.0000 . ?
C1 H1B 1.0000 . ?
C1 N1 1.457(2) . ?
C1 N3 1.465(2) . ?
C1 C8 1.472(3) . ?
N1 N2 1.361(2) . ?
N1 C2 1.359(2) . ?
N2 C4 1.329(2) . ?
C2 H2 0.9500 . ?
C2 C3 1.371(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.393(3) . ?
C4 H4 0.9500 . ?
N3 N4 1.358(2) . ?
N3 C5 1.363(3) . ?
N4 C7 1.336(2) . ?
C5 H5A 0.9500 . ?
C5 H5B 0.9500 . ?
C5 C6 1.366(3) . ?
C6 H6A 0.9500 . ?
C6 H6B 0.9500 . ?
C6 C7 1.387(3) . ?
C7 H7 0.9500 . ?
N5 H5 0.8800 . ?
N5 N6 1.346(2) . ?
N5 C10 1.373(3) . ?
N6 C8 1.355(2) . ?
C8 C9 1.377(3) . ?
C9 H9A 0.9500 . ?
C9 H9B 0.9500 . ?
C9 C10 1.374(3) . ?
C10 H10 0.9500 . ?
C10 H10A 0.9500 . ?
F1 B1 1.387(8) . ?
F2 B1 1.381(7) . ?
F3 B1 1.357(7) . ?
F4 B1 1.394(7) . ?
F1A B1A 1.385(14) . ?
F2A B1A 1.366(14) . ?
F3A B1A 1.344(13) . ?
F4A B1A 1.383(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 180.0 3_666 . ?
N4 Fe1 N2 87.36(6) 3_666 3_666 ?
N4 Fe1 N2 92.64(6) 3_666 . ?
N4 Fe1 N2 87.36(6) . . ?
N4 Fe1 N2 92.64(6) . 3_666 ?
N4 Fe1 N4 180.0 3_666 . ?
N6 Fe1 N2 92.79(6) . 3_666 ?
N6 Fe1 N2 87.21(6) . . ?
N6 Fe1 N2 87.21(6) 3_666 3_666 ?
N6 Fe1 N2 92.79(6) 3_666 . ?
N6 Fe1 N4 86.88(6) . . ?
N6 Fe1 N4 93.11(6) 3_666 . ?
N6 Fe1 N4 93.12(6) . 3_666 ?
N6 Fe1 N4 86.88(6) 3_666 3_666 ?
N6 Fe1 N6 180.0 3_666 . ?
H1A C1 H1B 0.0 . . ?
N1 C1 H1A 109.6 . . ?
N1 C1 H1B 109.6 . . ?
N1 C1 N3 109.27(15) . . ?
N1 C1 C8 109.43(15) . . ?
N3 C1 H1A 109.6 . . ?
N3 C1 H1B 109.6 . . ?
N3 C1 C8 109.47(15) . . ?
C8 C1 H1A 109.6 . . ?
C8 C1 H1B 109.6 . . ?
N2 N1 C1 117.92(15) . . ?
C2 N1 C1 130.53(16) . . ?
C2 N1 N2 111.54(16) . . ?
N1 N2 Fe1 118.79(12) . . ?
C4 N2 Fe1 136.22(13) . . ?
C4 N2 N1 104.99(15) . . ?
N1 C2 H2 126.8 . . ?
N1 C2 C3 106.47(16) . . ?
C3 C2 H2 126.8 . . ?
C2 C3 H3 127.1 . . ?
C2 C3 C4 105.70(17) . . ?
C4 C3 H3 127.1 . . ?
N2 C4 C3 111.30(17) . . ?
N2 C4 H4 124.4 . . ?
C3 C4 H4 124.4 . . ?
N4 N3 C1 117.23(15) . . ?
N4 N3 C5 111.02(16) . . ?
C5 N3 C1 131.69(16) . . ?
N3 N4 Fe1 119.52(12) . . ?
C7 N4 Fe1 135.00(12) . . ?
C7 N4 N3 105.48(15) . . ?
N3 C5 H5A 126.7 . . ?
N3 C5 H5B 126.7 . . ?
N3 C5 C6 106.55(17) . . ?
H5A C5 H5B 0.0 . . ?
C6 C5 H5A 126.7 . . ?
C6 C5 H5B 126.7 . . ?
C5 C6 H6A 126.8 . . ?
C5 C6 H6B 126.8 . . ?
C5 C6 C7 106.34(18) . . ?
H6A C6 H6B 0.0 . . ?
C7 C6 H6A 126.8 . . ?
C7 C6 H6B 126.8 . . ?
N4 C7 C6 110.61(17) . . ?
N4 C7 H7 124.7 . . ?
C6 C7 H7 124.7 . . ?
N6 N5 H5 124.7 . . ?
N6 N5 C10 110.55(17) . . ?
C10 N5 H5 124.7 . . ?
N5 N6 Fe1 134.36(12) . . ?
N5 N6 C8 105.83(15) . . ?
C8 N6 Fe1 119.79(13) . . ?
N6 C8 C1 117.15(15) . . ?
N6 C8 C9 110.63(17) . . ?
C9 C8 C1 132.22(17) . . ?
C8 C9 H9A 127.0 . . ?
C8 C9 H9B 127.0 . . ?
H9A C9 H9B 0.0 . . ?
C10 C9 C8 106.05(17) . . ?
C10 C9 H9A 127.0 . . ?
C10 C9 H9B 127.0 . . ?
N5 C10 C9 106.94(18) . . ?
N5 C10 H10 126.5 . . ?
N5 C10 H10A 126.5 . . ?
C9 C10 H10 126.5 . . ?
C9 C10 H10A 126.5 . . ?
H10 C10 H10A 0.0 . . ?
F1 B1 F4 109.9(8) . . ?
F2 B1 F1 108.1(5) . . ?
F2 B1 F4 109.3(7) . . ?
F3 B1 F1 106.6(6) . . ?
F3 B1 F2 114.0(7) . . ?
F3 B1 F4 109.0(8) . . ?
F2A B1A F1A 107.4(13) . . ?
F2A B1A F4A 113.0(15) . . ?
F3A B1A F1A 109.3(13) . . ?
F3A B1A F2A 108.1(15) . . ?
F3A B1A F4A 113.9(16) . . ?
F4A B1A F1A 104.8(15) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N5A H5AA F1A 0.88 2.29 3.107(12) 153.7 4_575
N5 H5 F2 0.88 2.06 2.905(5) 160.1 .

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 C4 C3 -178.57(15) . . . . ?
Fe1 N4 C7 C6 178.51(15) . . . . ?
Fe1 N6 C8 C1 -0.3(2) . . . . ?
Fe1 N6 C8 C9 178.90(13) . . . . ?
C1 N1 N2 Fe1 -0.1(2) . . . . ?
C1 N1 N2 C4 -179.29(16) . . . . ?
C1 N1 C2 C3 178.89(19) . . . . ?
C1 N3 N4 Fe1 -1.5(2) . . . . ?
C1 N3 N4 C7 177.82(16) . . . . ?
C1 N3 C5 C6 -176.95(19) . . . . ?
C1 C8 C9 C10 178.76(19) . . . . ?
N1 C1 N3 N4 61.0(2) . . . . ?
N1 C1 N3 C5 -122.2(2) . . . . ?
N1 C1 C8 N6 -59.7(2) . . . . ?
N1 C1 C8 C9 121.4(2) . . . . ?
N1 N2 C4 C3 0.4(2) . . . . ?
N1 C2 C3 C4 0.2(2) . . . . ?
N2 Fe1 N2 N1 93(8) 3_666 . . . ?
N2 Fe1 N2 C4 -88(8) 3_666 . . . ?
N2 Fe1 N4 N3 137.34(14) 3_666 . . . ?
N2 Fe1 N4 N3 -42.66(14) . . . . ?
N2 Fe1 N4 C7 138.32(19) . . . . ?
N2 Fe1 N4 C7 -41.68(19) 3_666 . . . ?
N2 Fe1 N6 N5 -137.67(18) . . . . ?
N2 Fe1 N6 N5 42.33(18) 3_666 . . . ?
N2 Fe1 N6 C8 -136.20(14) 3_666 . . . ?
N2 Fe1 N6 C8 43.79(14) . . . . ?
N2 N1 C2 C3 0.1(2) . . . . ?
C2 N1 N2 Fe1 178.90(12) . . . . ?
C2 N1 N2 C4 -0.3(2) . . . . ?
C2 C3 C4 N2 -0.4(2) . . . . ?
N3 C1 N1 N2 -60.1(2) . . . . ?
N3 C1 N1 C2 121.2(2) . . . . ?
N3 C1 C8 N6 60.0(2) . . . . ?
N3 C1 C8 C9 -118.9(2) . . . . ?
N3 N4 C7 C6 -0.6(2) . . . . ?
N3 C5 C6 C7 -0.4(2) . . . . ?
N4 Fe1 N2 N1 -136.58(14) 3_666 . . . ?
N4 Fe1 N2 N1 43.42(14) . . . . ?
N4 Fe1 N2 C4 -137.7(2) . . . . ?
N4 Fe1 N2 C4 42.3(2) 3_666 . . . ?
N4 Fe1 N4 N3 -120(5) 3_666 . . . ?
N4 Fe1 N4 C7 61(5) 3_666 . . . ?
N4 Fe1 N6 N5 -45.17(18) 3_666 . . . ?
N4 Fe1 N6 N5 134.83(18) . . . . ?
N4 Fe1 N6 C8 136.29(14) 3_666 . . . ?
N4 Fe1 N6 C8 -43.71(14) . . . . ?
N4 N3 C5 C6 0.1(2) . . . . ?
C5 N3 N4 Fe1 -178.95(13) . . . . ?
C5 N3 N4 C7 0.3(2) . . . . ?
C5 C6 C7 N4 0.7(2) . . . . ?
N5 N6 C8 C1 -179.17(15) . . . . ?
N5 N6 C8 C9 0.0(2) . . . . ?
N6 Fe1 N2 N1 -43.59(14) . . . . ?
N6 Fe1 N2 N1 136.41(14) 3_666 . . . ?
N6 Fe1 N2 C4 -44.7(2) 3_666 . . . ?
N6 Fe1 N2 C4 135.3(2) . . . . ?
N6 Fe1 N4 N3 -135.31(14) 3_666 . . . ?
N6 Fe1 N4 N3 44.69(14) . . . . ?
N6 Fe1 N4 C7 -134.33(19) . . . . ?
N6 Fe1 N4 C7 45.67(19) 3_666 . . . ?
N6 Fe1 N6 N5 114(40) 3_666 . . . ?
N6 Fe1 N6 C8 -65(40) 3_666 . . . ?
N6 N5 C10 C9 -0.4(2) . . . . ?
N6 C8 C9 C10 -0.2(2) . . . . ?
C8 C1 N1 N2 59.8(2) . . . . ?
C8 C1 N1 C2 -119.0(2) . . . . ?
C8 C1 N3 N4 -58.9(2) . . . . ?
C8 C1 N3 C5 118.0(2) . . . . ?
C8 C9 C10 N5 0.4(2) . . . . ?
C10 N5 N6 Fe1 -178.42(14) . . . . ?
C10 N5 N6 C8 0.3(2) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 4 -5 0.0039 -0.0026 4.0004 -4.9993 0.5872 0.6913 0.1864
0 -4 5 0.0169 0.0026 -4.0004 4.9993 -0.5872 -0.6913 -0.1864
0 4 5 0.0101 -0.0051 4.0002 5.0049 0.9026 -0.0574 -0.2021
0 -4 -5 0.0101 0.0051 -4.0002 -5.0049 -0.9026 0.0574 0.2021
6 1 -2 0.1402 5.9999 1.0014 -1.7954 0.0120 0.4716 -0.8158
-6 -1 2 0.1402 -5.9999 -1.0014 1.7954 -0.0120 -0.4716 0.8158

_olex2_date_sample_data_collection 2016-04-16
_olex2_date_sample_submission    2016-04-11
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.5083(10)
2 0.4917(10)

