# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_M171016A
_database_code_depnum_ccdc_archive 'CCDC 1860674'
_audit_update_record             
;
2018-08-07 deposited with the CCDC.
2018-11-09 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C12 H10 N6 S'
_chemical_formula_moiety         'C12 H10 N6 S'
_chemical_formula_weight         270.31
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_IT_number           61
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2+X,1/2-Y,-Z
3 -X,1/2+Y,1/2-Z
4 1/2-X,-Y,1/2+Z
5 -X,-Y,-Z
6 -1/2-X,-1/2+Y,+Z
7 +X,-1/2-Y,-1/2+Z
8 -1/2+X,+Y,-1/2-Z
#------------------------------------------------------------------------------
_cell_length_a                   10.0603(4)
_cell_length_b                   11.0336(5)
_cell_length_c                   22.1907(8)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     2463.19(17)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    13218
_cell_measurement_theta_min      2.02
_cell_measurement_theta_max      27.43
_cell_measurement_temperature    150
#------------------------------------------------------------------------------
_exptl_crystal_description       platelet
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1120.00
_exptl_absorpt_coefficient_mu    0.258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.715
_exptl_absorpt_correction_T_max  0.992

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      150
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            22387
_diffrn_reflns_av_R_equivalents  0.0804
_diffrn_reflns_theta_max         27.441
_diffrn_reflns_theta_min         2.733
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             2816
_reflns_number_gt                2078
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0481
_refine_ls_wR_factor_ref         0.1032
_refine_ls_wR_factor_gt          0.0942
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_reflns         2816
_refine_ls_number_parameters     180
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0423P)²+1.2078P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.26
_refine_diff_density_min         -0.28
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
S1 S 0.13167(5) 0.17322(5) 0.16557(3) 0.02985(16) Uani 1 1 d . . . . .
N1 N 0.17930(19) -0.05805(17) 0.14538(9) 0.0256(4) Uani 1 1 d . . . . .
N2 N 0.64091(15) 0.09996(15) 0.10840(8) 0.0207(4) Uani 1 1 d . . . . .
N3 N 0.65222(15) 0.26949(15) 0.16915(8) 0.0210(4) Uani 1 1 d . . . . .
N4 N 0.59146(16) 0.37086(15) 0.19174(8) 0.0237(4) Uani 1 1 d . . . . .
N5 N 0.64647(16) -0.07129(15) 0.04909(8) 0.0228(4) Uani 1 1 d . . . . .
N6 N 0.58782(18) -0.17118(16) 0.02425(8) 0.0284(4) Uani 1 1 d . . . . .
C1 C 0.22603(19) 0.05387(19) 0.14775(9) 0.0211(4) Uani 1 1 d . . . . .
C2 C 0.37091(19) 0.06885(17) 0.13368(9) 0.0199(4) Uani 1 1 d . . . . .
C3 C 0.44205(19) 0.16287(18) 0.15981(9) 0.0203(4) Uani 1 1 d . . . . .
H3 H 0.400777 0.217454 0.187118 0.024 Uiso 1 1 calc R U . . .
C4 C 0.43696(19) -0.01163(18) 0.09543(9) 0.0208(4) Uani 1 1 d . . . . .
H4 H 0.391902 -0.077501 0.076916 0.025 Uiso 1 1 calc R U . . .
C5 C 0.57497(19) 0.17472(18) 0.14487(9) 0.0205(4) Uani 1 1 d . . . . .
C6 C 0.57122(19) 0.00887(18) 0.08568(9) 0.0208(4) Uani 1 1 d . . . . .
C7 C 0.78676(19) 0.2737(2) 0.17662(9) 0.0249(5) Uani 1 1 d . . . . .
H7 H 0.849117 0.213983 0.164347 0.030 Uiso 1 1 calc R U . . .
C8 C 0.8144(2) 0.3799(2) 0.20500(10) 0.0277(5) Uani 1 1 d . . . . .
H8 H 0.899058 0.409419 0.216972 0.033 Uiso 1 1 calc R U . . .
C9 C 0.6890(2) 0.4374(2) 0.21290(9) 0.0247(5) Uani 1 1 d . . . . .
H9 H 0.677335 0.514515 0.231239 0.030 Uiso 1 1 calc R U . . .
C10 C 0.7795(2) -0.0655(2) 0.03695(10) 0.0294(5) Uani 1 1 d . . . . .
H10 H 0.839884 -0.004670 0.049921 0.035 Uiso 1 1 calc R U . . .
C11 C 0.8083(2) -0.1644(2) 0.00252(10) 0.0343(6) Uani 1 1 d . . . . .
H11 H 0.892206 -0.186683 -0.013721 0.041 Uiso 1 1 calc R U . . .
C12 C 0.6871(2) -0.2262(2) -0.00370(10) 0.0323(5) Uani 1 1 d . . . . .
H12 H 0.677452 -0.299582 -0.025629 0.039 Uiso 1 1 calc R U . . .
H1A H 0.097(3) -0.071(2) 0.1555(11) 0.044(8) Uiso 1 1 d . . . . .
H1B H 0.239(3) -0.123(3) 0.1440(12) 0.046(7) Uiso 1 1 d . . . . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_computing_structure_refinement  'SHELXL Version 2017/1 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.5 (Rigaku, 2017)'
_computing_molecular_graphics    'CrystalStructure 4.2.5'

#==============================================================================
# MOLECULAR GEOMETRY

_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
S1 C1 1.671(2) . ?
N1 C1 1.322(3) . ?
N1 H1A 0.87(3) . ?
N1 H1B 0.93(3) . ?
N2 C6 1.325(3) . ?
N2 C5 1.333(3) . ?
N3 C7 1.364(2) . ?
N3 N4 1.370(2) . ?
N3 C5 1.410(3) . ?
N4 C9 1.313(3) . ?
N5 N6 1.366(2) . ?
N5 C10 1.367(3) . ?
N5 C6 1.419(2) . ?
N6 C12 1.323(3) . ?
C1 C2 1.500(3) . ?
C2 C3 1.387(3) . ?
C2 C4 1.397(3) . ?
C3 C5 1.384(3) . ?
C3 H3 0.9500 . ?
C4 C6 1.386(3) . ?
C4 H4 0.9500 . ?
C7 C8 1.359(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.422(3) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.363(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.403(3) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?

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
C1 N1 H1A 119.1(17) . . ?
C1 N1 H1B 118.8(17) . . ?
H1A N1 H1B 120(2) . . ?
C6 N2 C5 115.93(16) . . ?
C7 N3 N4 111.72(16) . . ?
C7 N3 C5 128.23(17) . . ?
N4 N3 C5 119.97(15) . . ?
C9 N4 N3 104.73(16) . . ?
N6 N5 C10 112.40(17) . . ?
N6 N5 C6 120.20(16) . . ?
C10 N5 C6 127.30(18) . . ?
C12 N6 N5 103.46(18) . . ?
N1 C1 C2 116.12(18) . . ?
N1 C1 S1 122.92(16) . . ?
C2 C1 S1 120.96(15) . . ?
C3 C2 C4 118.95(17) . . ?
C3 C2 C1 119.79(18) . . ?
C4 C2 C1 121.25(18) . . ?
C5 C3 C2 117.98(18) . . ?
C5 C3 H3 121.0 . . ?
C2 C3 H3 121.0 . . ?
C6 C4 C2 117.04(18) . . ?
C6 C4 H4 121.5 . . ?
C2 C4 H4 121.5 . . ?
N2 C5 C3 124.61(19) . . ?
N2 C5 N3 114.63(17) . . ?
C3 C5 N3 120.75(18) . . ?
N2 C6 C4 125.44(18) . . ?
N2 C6 N5 114.09(17) . . ?
C4 C6 N5 120.48(18) . . ?
C8 C7 N3 106.78(19) . . ?
C8 C7 H7 126.6 . . ?
N3 C7 H7 126.6 . . ?
C7 C8 C9 105.11(18) . . ?
C7 C8 H8 127.4 . . ?
C9 C8 H8 127.4 . . ?
N4 C9 C8 111.7(2) . . ?
N4 C9 H9 124.2 . . ?
C8 C9 H9 124.2 . . ?
C11 C10 N5 106.3(2) . . ?
C11 C10 H10 126.8 . . ?
N5 C10 H10 126.8 . . ?
C10 C11 C12 105.0(2) . . ?
C10 C11 H11 127.5 . . ?
C12 C11 H11 127.5 . . ?
N6 C12 C11 112.8(2) . . ?
N6 C12 H12 123.6 . . ?
C11 C12 H12 123.6 . . ?

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
C7 N3 N4 C9 0.2(2) . . . . ?
C5 N3 N4 C9 177.20(17) . . . . ?
C10 N5 N6 C12 -0.4(2) . . . . ?
C6 N5 N6 C12 -177.08(18) . . . . ?
N1 C1 C2 C3 -150.7(2) . . . . ?
S1 C1 C2 C3 29.0(3) . . . . ?
N1 C1 C2 C4 28.1(3) . . . . ?
S1 C1 C2 C4 -152.19(16) . . . . ?
C4 C2 C3 C5 2.2(3) . . . . ?
C1 C2 C3 C5 -178.95(18) . . . . ?
C3 C2 C4 C6 -0.5(3) . . . . ?
C1 C2 C4 C6 -179.30(18) . . . . ?
C6 N2 C5 C3 0.0(3) . . . . ?
C6 N2 C5 N3 178.97(17) . . . . ?
C2 C3 C5 N2 -2.1(3) . . . . ?
C2 C3 C5 N3 179.00(17) . . . . ?
C7 N3 C5 N2 -23.1(3) . . . . ?
N4 N3 C5 N2 160.40(17) . . . . ?
C7 N3 C5 C3 155.9(2) . . . . ?
N4 N3 C5 C3 -20.6(3) . . . . ?
C5 N2 C6 C4 2.0(3) . . . . ?
C5 N2 C6 N5 -177.56(17) . . . . ?
C2 C4 C6 N2 -1.8(3) . . . . ?
C2 C4 C6 N5 177.78(18) . . . . ?
N6 N5 C6 N2 178.05(17) . . . . ?
C10 N5 C6 N2 1.9(3) . . . . ?
N6 N5 C6 C4 -1.6(3) . . . . ?
C10 N5 C6 C4 -177.7(2) . . . . ?
N4 N3 C7 C8 0.3(2) . . . . ?
C5 N3 C7 C8 -176.39(19) . . . . ?
N3 C7 C8 C9 -0.7(2) . . . . ?
N3 N4 C9 C8 -0.6(2) . . . . ?
C7 C8 C9 N4 0.8(3) . . . . ?
N6 N5 C10 C11 0.6(2) . . . . ?
C6 N5 C10 C11 176.98(19) . . . . ?
N5 C10 C11 C12 -0.5(2) . . . . ?
N5 N6 C12 C11 0.1(2) . . . . ?
C10 C11 C12 N6 0.3(3) . . . . ?

#==============================================================================
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1A N4 . . 6_655 3.016(3) 0.88(3) 2.15(3) 169(2) no

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.



#==============================================================================
#     End of CIF
#==============================================================================
_chemical_name_systematic        
2,6-bis(pyrazol-1-yl)pyridine-4-carbothioamide
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Ethyleacetate'
####################################################################### 
# 
# 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_M171023A
_database_code_depnum_ccdc_archive 'CCDC 1860677'
_audit_update_record             
;
2018-08-07 deposited with the CCDC.
2018-11-09 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C26 H26 B2 F8 Fe N14 O4 S2'
_chemical_formula_moiety         '2(C12 H10 N6 S) Fe, 2(B F4), 2(C H3 N O2)'
_chemical_formula_weight         892.16
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
_space_group_IT_number           15
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
#------------------------------------------------------------------------------
_cell_length_a                   51.880(2)
_cell_length_b                   8.4111(4)
_cell_length_c                   17.1533(8)
_cell_angle_alpha                90.0000
_cell_angle_beta                 94.245(7)
_cell_angle_gamma                90.0000
_cell_volume                     7464.7(6)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    23785
_cell_measurement_theta_min      1.90
_cell_measurement_theta_max      27.43
_cell_measurement_temperature    290
#------------------------------------------------------------------------------
_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3616.00
_exptl_absorpt_coefficient_mu    0.610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.556
_exptl_absorpt_correction_T_max  0.970

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      290
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            34048
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_theta_max         27.435
_diffrn_reflns_theta_min         2.362
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_h_max       66
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             8497
_reflns_number_gt                6137
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0605
_refine_ls_wR_factor_ref         0.1827
_refine_ls_wR_factor_gt          0.1663
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_reflns         8497
_refine_ls_number_parameters     530
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.1016P)²+11.8490P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         0.97
_refine_diff_density_min         -0.58
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
B B 0.0013 0.0007
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
F F 0.0171 0.0103
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Fe Fe 0.3463 0.8444
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.12438(2) 0.24068(5) 0.02710(2) 0.03444(14) Uani 1 1 d . . . . .
S1 S 0.25795(2) 0.20859(15) 0.16123(6) 0.0620(3) Uani 1 1 d . . . . .
S2 S -0.01259(2) 0.27900(13) 0.03269(7) 0.0605(3) Uani 1 1 d . . . . .
F1 F 0.20278(9) -0.2772(7) -0.1580(2) 0.1512(19) Uani 1 1 d . . . . .
F2 F 0.22379(5) -0.3021(4) -0.04234(18) 0.0916(9) Uani 1 1 d . . . . .
F3 F 0.19816(5) -0.0896(4) -0.0674(3) 0.1160(13) Uani 1 1 d . . . . .
F4 F 0.18061(5) -0.3275(4) -0.0550(2) 0.1057(12) Uani 1 1 d . . . . .
F5 F 0.05415(5) 0.0675(5) -0.32909(16) 0.0935(10) Uani 1 1 d . . . . .
F6 F 0.07531(6) 0.1295(7) -0.2147(2) 0.152(2) Uani 1 1 d . . . . .
F7 F 0.03304(10) 0.1674(11) -0.2340(3) 0.222(4) Uani 1 1 d . . . . .
F8 F 0.04925(18) -0.0469(7) -0.2165(3) 0.244(4) Uani 1 1 d . . . . .
O1 O 0.19357(9) -0.3808(5) 0.1579(3) 0.1201(16) Uani 1 1 d . . . . .
O2 O 0.17680(8) -0.1565(5) 0.1349(3) 0.1135(14) Uani 1 1 d . . . . .
O3 O 0.06319(10) 0.4541(6) 0.3495(3) 0.1254(16) Uani 1 1 d . . . . .
O4 O 0.07776(11) 0.4077(7) 0.2404(4) 0.146(2) Uani 1 1 d . . . . .
N1 N 0.25097(6) 0.4460(4) 0.0615(2) 0.0589(9) Uani 1 1 d . . . . .
N2 N 0.16070(5) 0.2555(3) 0.04769(15) 0.0360(5) Uani 1 1 d . . . . .
N3 N 0.16055(5) 0.3316(4) -0.07781(15) 0.0413(6) Uani 1 1 d . . . . .
N4 N 0.13419(5) 0.3153(3) -0.07575(15) 0.0402(6) Uani 1 1 d . . . . .
N5 N 0.15276(5) 0.1717(3) 0.16852(15) 0.0386(6) Uani 1 1 d . . . . .
N6 N 0.12766(5) 0.1654(3) 0.13602(15) 0.0389(6) Uani 1 1 d . . . . .
N7 N -0.00168(7) 0.1484(6) -0.1005(3) 0.0726(12) Uani 1 1 d . . . . .
N8 N 0.08795(5) 0.2327(3) 0.00821(15) 0.0358(5) Uani 1 1 d . . . . .
N9 N 0.09508(5) -0.0143(3) -0.03610(16) 0.0397(6) Uani 1 1 d . . . . .
N10 N 0.12053(5) 0.0220(3) -0.01409(15) 0.0386(6) Uani 1 1 d . . . . .
N11 N 0.08888(5) 0.4804(3) 0.05795(16) 0.0406(6) Uani 1 1 d . . . . .
N12 N 0.11526(5) 0.4557(3) 0.06242(15) 0.0388(6) Uani 1 1 d . . . . .
N13 N 0.19567(8) -0.2420(5) 0.1456(3) 0.0725(10) Uani 1 1 d . . . . .
N14 N 0.06016(10) 0.4235(6) 0.2805(3) 0.0924(14) Uani 1 1 d . . . . .
C1 C 0.24094(6) 0.3277(5) 0.0996(2) 0.0468(8) Uani 1 1 d . . . . .
C2 C 0.21260(6) 0.2994(4) 0.0808(2) 0.0405(7) Uani 1 1 d . . . . .
C3 C 0.20172(6) 0.3297(4) 0.00555(19) 0.0407(7) Uani 1 1 d . . . . .
H3 H 0.211677 0.364557 -0.033999 0.049 Uiso 1 1 calc R U . . .
C4 C 0.19764(6) 0.2454(4) 0.1398(2) 0.0415(7) Uani 1 1 d . . . . .
H4 H 0.204851 0.224723 0.189993 0.050 Uiso 1 1 calc R U . . .
C5 C 0.17540(6) 0.3052(4) -0.00740(18) 0.0383(7) Uani 1 1 d . . . . .
C6 C 0.17148(6) 0.2242(4) 0.11970(18) 0.0373(7) Uani 1 1 d . . . . .
C7 C 0.16672(7) 0.3772(5) -0.1501(2) 0.0557(10) Uani 1 1 d . . . . .
H7 H 0.183234 0.395824 -0.165728 0.067 Uiso 1 1 calc R U . . .
C8 C 0.14433(8) 0.3903(6) -0.1948(2) 0.0640(11) Uani 1 1 d . . . . .
H8 H 0.142423 0.419896 -0.247163 0.077 Uiso 1 1 calc R U . . .
C9 C 0.12457(7) 0.3510(5) -0.1473(2) 0.0508(8) Uani 1 1 d . . . . .
H9 H 0.107068 0.350030 -0.163646 0.061 Uiso 1 1 calc R U . . .
C10 C 0.15445(7) 0.1101(5) 0.24183(19) 0.0501(8) Uani 1 1 d . . . . .
H10 H 0.169306 0.101232 0.275387 0.060 Uiso 1 1 calc R U . . .
C11 C 0.12998(7) 0.0635(5) 0.2567(2) 0.0546(9) Uani 1 1 d . . . . .
H11 H 0.124963 0.016040 0.302170 0.065 Uiso 1 1 calc R U . . .
C12 C 0.11417(6) 0.1011(4) 0.1904(2) 0.0451(8) Uani 1 1 d . . . . .
H12 H 0.096436 0.083431 0.184977 0.054 Uiso 1 1 calc R U . . .
C13 C 0.00653(6) 0.2116(5) -0.0338(2) 0.0501(9) Uani 1 1 d . . . . .
C14 C 0.03539(6) 0.2191(4) -0.0189(2) 0.0432(7) Uani 1 1 d . . . . .
C15 C 0.05023(6) 0.0895(4) -0.0380(2) 0.0435(7) Uani 1 1 d . . . . .
H15 H 0.042672 -0.001925 -0.059936 0.052 Uiso 1 1 calc R U . . .
C16 C 0.04683(6) 0.3556(4) 0.0148(2) 0.0446(7) Uani 1 1 d . . . . .
H16 H 0.036989 0.442265 0.028417 0.054 Uiso 1 1 calc R U . . .
C17 C 0.07666(6) 0.1016(4) -0.02304(18) 0.0377(7) Uani 1 1 d . . . . .
C18 C 0.07331(6) 0.3557(4) 0.02679(19) 0.0383(7) Uani 1 1 d . . . . .
C19 C 0.09331(7) -0.1607(4) -0.0699(2) 0.0462(8) Uani 1 1 d . . . . .
H19 H 0.078258 -0.211039 -0.089701 0.055 Uiso 1 1 calc R U . . .
C20 C 0.11779(8) -0.2193(4) -0.0693(2) 0.0500(8) Uani 1 1 d . . . . .
H20 H 0.122752 -0.317242 -0.088491 0.060 Uiso 1 1 calc R U . . .
C21 C 0.13392(7) -0.1033(4) -0.03428(19) 0.0446(7) Uani 1 1 d . . . . .
H21 H 0.151779 -0.112707 -0.026134 0.053 Uiso 1 1 calc R U . . .
C22 C 0.08327(7) 0.6214(4) 0.0911(2) 0.0488(8) Uani 1 1 d . . . . .
H22 H 0.066861 0.663568 0.095247 0.059 Uiso 1 1 calc R U . . .
C23 C 0.10596(8) 0.6894(5) 0.1171(2) 0.0537(9) Uani 1 1 d . . . . .
H23 H 0.108247 0.786581 0.142536 0.064 Uiso 1 1 calc R U . . .
C24 C 0.12527(7) 0.5832(4) 0.09778(19) 0.0476(8) Uani 1 1 d . . . . .
H24 H 0.142888 0.600257 0.108491 0.057 Uiso 1 1 calc R U . . .
C25 C 0.22149(10) -0.1745(7) 0.1406(3) 0.0863(15) Uani 1 1 d . . . . .
H25A H 0.220078 -0.062406 0.130602 0.104 Uiso 1 1 calc R U . . .
H25B H 0.231571 -0.191700 0.189131 0.104 Uiso 1 1 calc R U . . .
H25C H 0.229774 -0.224972 0.098969 0.104 Uiso 1 1 calc R U . . .
C26 C 0.03375(15) 0.4029(11) 0.2464(5) 0.146(3) Uani 1 1 d . . . . .
H26A H 0.021859 0.419453 0.285919 0.175 Uiso 1 1 calc R U . . .
H26B H 0.030352 0.478635 0.205032 0.175 Uiso 1 1 calc R U . . .
H26C H 0.031682 0.297187 0.225828 0.175 Uiso 1 1 calc R U . . .
B1 B 0.20137(9) -0.2490(6) -0.0820(3) 0.0620(12) Uani 1 1 d . . . . .
B2 B 0.05291(8) 0.0911(7) -0.2505(3) 0.0608(12) Uani 1 1 d . . . . .
H1A H 0.2687(10) 0.480(6) 0.071(3) 0.089(15) Uiso 1 1 d . . . . .
H1B H 0.2414(8) 0.502(6) 0.028(3) 0.066(13) Uiso 1 1 d . . . . .
H7A H 0.0077(8) 0.121(5) -0.137(2) 0.057(13) Uiso 1 1 d . . . . .
H7B H -0.0168(9) 0.121(6) -0.115(3) 0.069(13) Uiso 1 1 d . . . . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_computing_structure_refinement  'SHELXL Version 2017/1 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.5 (Rigaku, 2017)'
_computing_molecular_graphics    'CrystalStructure 4.2.5'

#==============================================================================
# MOLECULAR GEOMETRY

_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 N8 1.895(2) . ?
Fe1 N2 1.896(2) . ?
Fe1 N6 1.968(3) . ?
Fe1 N4 1.974(3) . ?
Fe1 N10 1.975(3) . ?
Fe1 N12 1.976(3) . ?
S1 C1 1.662(4) . ?
S2 C13 1.666(4) . ?
F1 B1 1.332(7) . ?
F2 B1 1.378(5) . ?
F3 B1 1.377(6) . ?
F4 B1 1.373(6) . ?
F5 B2 1.368(6) . ?
F6 B2 1.314(5) . ?
F7 B2 1.264(6) . ?
F8 B2 1.320(7) . ?
O1 N13 1.193(5) . ?
O2 N13 1.218(5) . ?
O3 N14 1.210(6) . ?
O4 N14 1.191(6) . ?
N1 C1 1.318(5) . ?
N1 H1A 0.97(5) . ?
N1 H1B 0.87(5) . ?
N2 C5 1.325(4) . ?
N2 C6 1.344(4) . ?
N3 C7 1.358(4) . ?
N3 N4 1.378(3) . ?
N3 C5 1.401(4) . ?
N4 C9 1.325(4) . ?
N5 C10 1.357(4) . ?
N5 N6 1.379(3) . ?
N5 C6 1.400(4) . ?
N6 C12 1.323(4) . ?
N7 C13 1.304(5) . ?
N7 H7A 0.85(4) . ?
N7 H7B 0.84(5) . ?
N8 C18 1.336(4) . ?
N8 C17 1.342(4) . ?
N9 C19 1.361(4) . ?
N9 N10 1.380(3) . ?
N9 C17 1.395(4) . ?
N10 C21 1.323(4) . ?
N11 C22 1.356(4) . ?
N11 N12 1.381(3) . ?
N11 C18 1.405(4) . ?
N12 C24 1.319(4) . ?
N13 C25 1.463(6) . ?
N14 C26 1.459(8) . ?
C1 C2 1.501(4) . ?
C2 C3 1.394(5) . ?
C2 C4 1.395(5) . ?
C3 C5 1.383(4) . ?
C3 H3 0.9300 . ?
C4 C6 1.387(4) . ?
C4 H4 0.9300 . ?
C7 C8 1.348(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.396(6) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 C11 1.371(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.389(5) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.501(4) . ?
C14 C15 1.388(5) . ?
C14 C16 1.398(5) . ?
C15 C17 1.379(4) . ?
C15 H15 0.9300 . ?
C16 C18 1.374(4) . ?
C16 H16 0.9300 . ?
C19 C20 1.362(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.393(5) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 C23 1.354(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.400(5) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?

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
N8 Fe1 N2 178.04(11) . . ?
N8 Fe1 N6 99.55(11) . . ?
N2 Fe1 N6 80.18(10) . . ?
N8 Fe1 N4 100.27(11) . . ?
N2 Fe1 N4 80.05(10) . . ?
N6 Fe1 N4 160.16(10) . . ?
N8 Fe1 N10 80.36(10) . . ?
N2 Fe1 N10 101.58(11) . . ?
N6 Fe1 N10 92.26(11) . . ?
N4 Fe1 N10 90.12(11) . . ?
N8 Fe1 N12 80.02(10) . . ?
N2 Fe1 N12 98.04(11) . . ?
N6 Fe1 N12 90.53(11) . . ?
N4 Fe1 N12 93.81(11) . . ?
N10 Fe1 N12 160.37(10) . . ?
C1 N1 H1A 123(3) . . ?
C1 N1 H1B 121(3) . . ?
H1A N1 H1B 116(4) . . ?
C5 N2 C6 119.7(3) . . ?
C5 N2 Fe1 120.3(2) . . ?
C6 N2 Fe1 119.9(2) . . ?
C7 N3 N4 110.7(3) . . ?
C7 N3 C5 132.8(3) . . ?
N4 N3 C5 116.5(2) . . ?
C9 N4 N3 105.1(3) . . ?
C9 N4 Fe1 142.7(2) . . ?
N3 N4 Fe1 112.12(18) . . ?
C10 N5 N6 110.8(3) . . ?
C10 N5 C6 132.4(3) . . ?
N6 N5 C6 116.5(2) . . ?
C12 N6 N5 105.3(3) . . ?
C12 N6 Fe1 142.0(2) . . ?
N5 N6 Fe1 112.59(18) . . ?
C13 N7 H7A 126(3) . . ?
C13 N7 H7B 128(3) . . ?
H7A N7 H7B 106(4) . . ?
C18 N8 C17 119.5(3) . . ?
C18 N8 Fe1 120.6(2) . . ?
C17 N8 Fe1 119.9(2) . . ?
C19 N9 N10 110.5(3) . . ?
C19 N9 C17 132.5(3) . . ?
N10 N9 C17 117.0(2) . . ?
C21 N10 N9 105.2(3) . . ?
C21 N10 Fe1 142.6(2) . . ?
N9 N10 Fe1 111.93(18) . . ?
C22 N11 N12 110.5(3) . . ?
C22 N11 C18 132.6(3) . . ?
N12 N11 C18 116.7(2) . . ?
C24 N12 N11 105.0(3) . . ?
C24 N12 Fe1 142.2(2) . . ?
N11 N12 Fe1 112.29(19) . . ?
O1 N13 O2 121.5(5) . . ?
O1 N13 C25 119.1(5) . . ?
O2 N13 C25 119.4(5) . . ?
O4 N14 O3 122.6(6) . . ?
O4 N14 C26 119.5(7) . . ?
O3 N14 C26 117.9(6) . . ?
N1 C1 C2 115.5(3) . . ?
N1 C1 S1 124.0(3) . . ?
C2 C1 S1 120.4(3) . . ?
C3 C2 C4 121.5(3) . . ?
C3 C2 C1 119.5(3) . . ?
C4 C2 C1 119.0(3) . . ?
C5 C3 C2 116.7(3) . . ?
C5 C3 H3 121.7 . . ?
C2 C3 H3 121.7 . . ?
C6 C4 C2 116.7(3) . . ?
C6 C4 H4 121.7 . . ?
C2 C4 H4 121.7 . . ?
N2 C5 C3 123.1(3) . . ?
N2 C5 N3 110.9(3) . . ?
C3 C5 N3 126.0(3) . . ?
N2 C6 C4 122.4(3) . . ?
N2 C6 N5 110.6(3) . . ?
C4 C6 N5 127.0(3) . . ?
C8 C7 N3 106.9(3) . . ?
C8 C7 H7 126.5 . . ?
N3 C7 H7 126.5 . . ?
C7 C8 C9 106.7(3) . . ?
C7 C8 H8 126.6 . . ?
C9 C8 H8 126.6 . . ?
N4 C9 C8 110.6(3) . . ?
N4 C9 H9 124.7 . . ?
C8 C9 H9 124.7 . . ?
N5 C10 C11 106.5(3) . . ?
N5 C10 H10 126.7 . . ?
C11 C10 H10 126.7 . . ?
C10 C11 C12 106.3(3) . . ?
C10 C11 H11 126.8 . . ?
C12 C11 H11 126.8 . . ?
N6 C12 C11 111.1(3) . . ?
N6 C12 H12 124.5 . . ?
C11 C12 H12 124.5 . . ?
N7 C13 C14 115.0(3) . . ?
N7 C13 S2 124.6(3) . . ?
C14 C13 S2 120.4(3) . . ?
C15 C14 C16 121.1(3) . . ?
C15 C14 C13 119.4(3) . . ?
C16 C14 C13 119.5(3) . . ?
C17 C15 C14 117.3(3) . . ?
C17 C15 H15 121.3 . . ?
C14 C15 H15 121.3 . . ?
C18 C16 C14 116.9(3) . . ?
C18 C16 H16 121.6 . . ?
C14 C16 H16 121.6 . . ?
N8 C17 C15 122.2(3) . . ?
N8 C17 N9 110.8(2) . . ?
C15 C17 N9 127.0(3) . . ?
N8 C18 C16 122.9(3) . . ?
N8 C18 N11 110.3(3) . . ?
C16 C18 N11 126.7(3) . . ?
N9 C19 C20 106.9(3) . . ?
N9 C19 H19 126.5 . . ?
C20 C19 H19 126.5 . . ?
C19 C20 C21 106.2(3) . . ?
C19 C20 H20 126.9 . . ?
C21 C20 H20 126.9 . . ?
N10 C21 C20 111.2(3) . . ?
N10 C21 H21 124.4 . . ?
C20 C21 H21 124.4 . . ?
C23 C22 N11 107.4(3) . . ?
C23 C22 H22 126.3 . . ?
N11 C22 H22 126.3 . . ?
C22 C23 C24 105.8(3) . . ?
C22 C23 H23 127.1 . . ?
C24 C23 H23 127.1 . . ?
N12 C24 C23 111.3(3) . . ?
N12 C24 H24 124.3 . . ?
C23 C24 H24 124.3 . . ?
N13 C25 H25A 109.5 . . ?
N13 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
N13 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N14 C26 H26A 109.5 . . ?
N14 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
N14 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
F1 B1 F4 110.3(5) . . ?
F1 B1 F3 111.6(5) . . ?
F4 B1 F3 107.3(4) . . ?
F1 B1 F2 108.7(4) . . ?
F4 B1 F2 109.4(4) . . ?
F3 B1 F2 109.5(4) . . ?
F7 B2 F6 118.6(6) . . ?
F7 B2 F8 101.6(6) . . ?
F6 B2 F8 99.2(5) . . ?
F7 B2 F5 113.1(4) . . ?
F6 B2 F5 113.1(4) . . ?
F8 B2 F5 109.1(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
N6 Fe1 N2 C5 179.3(3) . . . . ?
N4 Fe1 N2 C5 1.0(2) . . . . ?
N10 Fe1 N2 C5 89.0(3) . . . . ?
N12 Fe1 N2 C5 -91.5(3) . . . . ?
N6 Fe1 N2 C6 -4.5(2) . . . . ?
N4 Fe1 N2 C6 177.2(3) . . . . ?
N10 Fe1 N2 C6 -94.8(2) . . . . ?
N12 Fe1 N2 C6 84.7(2) . . . . ?
C7 N3 N4 C9 0.1(4) . . . . ?
C5 N3 N4 C9 177.9(3) . . . . ?
C7 N3 N4 Fe1 177.7(3) . . . . ?
C5 N3 N4 Fe1 -4.5(4) . . . . ?
C10 N5 N6 C12 0.6(4) . . . . ?
C6 N5 N6 C12 175.1(3) . . . . ?
C10 N5 N6 Fe1 -176.3(2) . . . . ?
C6 N5 N6 Fe1 -1.9(3) . . . . ?
N6 Fe1 N8 C18 86.6(3) . . . . ?
N4 Fe1 N8 C18 -94.4(3) . . . . ?
N10 Fe1 N8 C18 177.2(3) . . . . ?
N12 Fe1 N8 C18 -2.3(2) . . . . ?
N6 Fe1 N8 C17 -92.5(3) . . . . ?
N4 Fe1 N8 C17 86.6(3) . . . . ?
N10 Fe1 N8 C17 -1.8(2) . . . . ?
N12 Fe1 N8 C17 178.7(3) . . . . ?
C19 N9 N10 C21 -0.5(4) . . . . ?
C17 N9 N10 C21 -178.4(3) . . . . ?
C19 N9 N10 Fe1 175.1(2) . . . . ?
C17 N9 N10 Fe1 -2.8(3) . . . . ?
C22 N11 N12 C24 -0.5(4) . . . . ?
C18 N11 N12 C24 -176.0(3) . . . . ?
C22 N11 N12 Fe1 172.8(2) . . . . ?
C18 N11 N12 Fe1 -2.7(3) . . . . ?
N1 C1 C2 C3 32.7(5) . . . . ?
S1 C1 C2 C3 -144.3(3) . . . . ?
N1 C1 C2 C4 -146.3(4) . . . . ?
S1 C1 C2 C4 36.7(4) . . . . ?
C4 C2 C3 C5 0.7(5) . . . . ?
C1 C2 C3 C5 -178.3(3) . . . . ?
C3 C2 C4 C6 -0.3(5) . . . . ?
C1 C2 C4 C6 178.7(3) . . . . ?
C6 N2 C5 C3 -1.1(5) . . . . ?
Fe1 N2 C5 C3 175.2(3) . . . . ?
C6 N2 C5 N3 -179.8(3) . . . . ?
Fe1 N2 C5 N3 -3.5(4) . . . . ?
C2 C3 C5 N2 0.0(5) . . . . ?
C2 C3 C5 N3 178.5(3) . . . . ?
C7 N3 C5 N2 -177.7(4) . . . . ?
N4 N3 C5 N2 5.2(4) . . . . ?
C7 N3 C5 C3 3.7(6) . . . . ?
N4 N3 C5 C3 -173.5(3) . . . . ?
C5 N2 C6 C4 1.5(5) . . . . ?
Fe1 N2 C6 C4 -174.7(2) . . . . ?
C5 N2 C6 N5 -179.3(3) . . . . ?
Fe1 N2 C6 N5 4.5(4) . . . . ?
C2 C4 C6 N2 -0.9(5) . . . . ?
C2 C4 C6 N5 -179.9(3) . . . . ?
C10 N5 C6 N2 171.5(3) . . . . ?
N6 N5 C6 N2 -1.4(4) . . . . ?
C10 N5 C6 C4 -9.3(6) . . . . ?
N6 N5 C6 C4 177.7(3) . . . . ?
N4 N3 C7 C8 0.0(5) . . . . ?
C5 N3 C7 C8 -177.3(4) . . . . ?
N3 C7 C8 C9 -0.1(5) . . . . ?
N3 N4 C9 C8 -0.2(4) . . . . ?
Fe1 N4 C9 C8 -176.5(3) . . . . ?
C7 C8 C9 N4 0.2(5) . . . . ?
N6 N5 C10 C11 0.0(4) . . . . ?
C6 N5 C10 C11 -173.3(4) . . . . ?
N5 C10 C11 C12 -0.5(4) . . . . ?
N5 N6 C12 C11 -0.9(4) . . . . ?
Fe1 N6 C12 C11 174.5(3) . . . . ?
C10 C11 C12 N6 0.9(4) . . . . ?
N7 C13 C14 C15 -42.3(5) . . . . ?
S2 C13 C14 C15 136.9(3) . . . . ?
N7 C13 C14 C16 138.5(4) . . . . ?
S2 C13 C14 C16 -42.2(5) . . . . ?
C16 C14 C15 C17 -0.6(5) . . . . ?
C13 C14 C15 C17 -179.8(3) . . . . ?
C15 C14 C16 C18 1.0(5) . . . . ?
C13 C14 C16 C18 -179.8(3) . . . . ?
C18 N8 C17 C15 1.0(5) . . . . ?
Fe1 N8 C17 C15 180.0(3) . . . . ?
C18 N8 C17 N9 -178.3(3) . . . . ?
Fe1 N8 C17 N9 0.7(4) . . . . ?
C14 C15 C17 N8 -0.4(5) . . . . ?
C14 C15 C17 N9 178.8(3) . . . . ?
C19 N9 C17 N8 -175.9(3) . . . . ?
N10 N9 C17 N8 1.4(4) . . . . ?
C19 N9 C17 C15 4.9(6) . . . . ?
N10 N9 C17 C15 -177.8(3) . . . . ?
C17 N8 C18 C16 -0.6(5) . . . . ?
Fe1 N8 C18 C16 -179.6(3) . . . . ?
C17 N8 C18 N11 -179.6(3) . . . . ?
Fe1 N8 C18 N11 1.4(4) . . . . ?
C14 C16 C18 N8 -0.4(5) . . . . ?
C14 C16 C18 N11 178.4(3) . . . . ?
C22 N11 C18 N8 -173.3(3) . . . . ?
N12 N11 C18 N8 1.0(4) . . . . ?
C22 N11 C18 C16 7.7(6) . . . . ?
N12 N11 C18 C16 -178.0(3) . . . . ?
N10 N9 C19 C20 0.3(4) . . . . ?
C17 N9 C19 C20 177.8(3) . . . . ?
N9 C19 C20 C21 0.0(4) . . . . ?
N9 N10 C21 C20 0.4(4) . . . . ?
Fe1 N10 C21 C20 -172.8(3) . . . . ?
C19 C20 C21 N10 -0.3(4) . . . . ?
N12 N11 C22 C23 0.2(4) . . . . ?
C18 N11 C22 C23 174.7(3) . . . . ?
N11 C22 C23 C24 0.2(4) . . . . ?
N11 N12 C24 C23 0.6(4) . . . . ?
Fe1 N12 C24 C23 -169.3(3) . . . . ?
C22 C23 C24 N12 -0.5(4) . . . . ?

#==============================================================================
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1A F3 . . 7_555 2.897(4) 0.97(5) 1.95(5) 165(4) no
N7 H7B F5 . . 2_554 2.974(5) 0.84(5) 2.15(5) 170(4) no

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.



#==============================================================================
#     End of CIF
#==============================================================================
_chemical_name_systematic        
'Iron(II) bis(2,6-bis(pyrazol-1-yl)pyridine-4-carbothioamide) tetrafluorobroate'
####################################################################### 
# 
# 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_ma-ctabpp-02a_cu_330k
_database_code_depnum_ccdc_archive 'CCDC 1860680'
_audit_update_record             
;
2018-08-07 deposited with the CCDC.
2018-11-09 downloaded from the CCDC.
;
_audit_creation_date             2017-09-05
_audit_creation_method           
;
Olex2 1.2-ac3
(compiled 2017.03.02 svn.r3394 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        
'Iron(II) bis(N-methyl-2,6-bis(pyrazol-1-yl)pyridine-4-carbothioamide ) tetrafluorobroate'
_chemical_formula_moiety         'C26 H24 Fe N12 S2, 2(B F4), C H3 N O2'
_chemical_formula_sum            'C27 H27 B2 F8 Fe N13 O2 S2'
_chemical_formula_weight         859.20
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C27 H27 B2 F8 Fe N13 O2 S2'
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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   8.25830(10)
_cell_length_b                   40.8625(4)
_cell_length_c                   10.80570(10)
_cell_angle_alpha                90
_cell_angle_beta                 94.7390(10)
_cell_angle_gamma                90
_cell_volume                     3633.97(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    13112
_cell_measurement_temperature    329.98(12)
_cell_measurement_theta_max      77.0310
_cell_measurement_theta_min      4.2520
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.207
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.408
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
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_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       ?
_exptl_crystal_F_000             1744
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 0 -1 0.1386
-2 -2 1 0.1627
0 -1 0 0.0540
0 1 0 0.0540
0 -2 -1 0.0231
0 2 1 0.0391
0 -3 1 0.0376
0 3 -1 0.0471
0 1 1 0.0317
-3 -1 0 0.1710
-3 1 2 0.1660
1 3 3 0.0774

_exptl_crystal_size_max          0.329
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.062
loop_
_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
1.9990 -0.0037 -0.9992 0.0289 0.0005 -0.3883
-1.9992 -1.9941 0.9998 -0.0867 0.0476 0.3841
-0.0001 -0.9989 0.0003 -0.0289 0.0241 -0.0021
0.0001 0.9989 -0.0003 0.0289 -0.0241 0.0021
-0.0007 -2.0027 -0.9987 0.0325 0.1536 -0.0385
0.0007 2.0027 0.9987 -0.0325 -0.1536 0.0385
0.0001 -2.9920 1.0001 -0.1769 -0.0333 0.0280
-0.0001 2.9920 -1.0001 0.1769 0.0333 -0.0280
0.0006 1.0037 0.9990 -0.0614 -0.1295 0.0364
-2.9993 -1.0006 0.0002 0.0631 0.1815 0.5289
-2.9981 1.0069 1.9982 -0.0596 -0.0776 0.6017
1.0015 3.0118 2.9971 -0.2147 -0.4410 -0.0678

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            20884
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.238
_diffrn_reflns_theta_min         4.246
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      329.98(12)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     17.00  71.00   0.50    1.60    --    0.57  19.00 -30.00  108
  2  ω     10.00  60.00   0.50    1.60    --    0.57  38.00-120.00  100
  3  ω     35.00  83.00   0.50    6.20    --  104.00 -45.00 -30.00   96
  4  ω     71.00 100.00   0.50    6.20    --  104.00 -94.00   0.00   58
  5  ω     37.00  64.00   0.50    6.20    --  104.00 -30.00 120.00   54
  6  ω     38.00 110.00   0.50    6.20    --  104.00 -77.00 120.00  144
  7  ω     34.00  59.00   0.50    6.20    --  104.00 -30.00   0.00   50
  8  ω     34.00  61.00   0.50    6.20    --  104.00 -15.00  30.00   54
  9  ω     37.00  65.00   0.50    6.20    --  104.00 -15.00   0.00   56
 10  ω    104.00 175.00   0.50    6.20    --  104.00  45.00 -60.00  142
 11  ω    130.00 169.00   0.50    6.20    --  104.00  77.00 -30.00   78
 12  ω     93.00 122.00   0.50    6.20    --  104.00  77.00 -30.00   58
 13  ω    134.00 175.00   0.50    6.20    --  104.00 125.00 150.00   82
 14  ω     93.00 119.00   0.50    6.20    --  104.00 125.00 150.00   52
 15  ω     33.00 108.00   0.50    6.20    --  104.00 -94.00-150.00  150
 16  ω     34.00  59.00   0.50    6.20    --  104.00 -30.00-180.00   50
 17  ω    -67.00 -11.00   0.50    1.60    --    0.57 -38.00  60.00  112
 18  ω    -54.00 -23.00   0.50    6.20    --  -82.50  30.00 -60.00   62
 19  ω     34.00 108.00   0.50    6.20    --  104.00 -94.00 120.00  148
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0306834000
_diffrn_orient_matrix_UB_12      0.0289053000
_diffrn_orient_matrix_UB_13      -0.0904374000
_diffrn_orient_matrix_UB_21      -0.0524653000
_diffrn_orient_matrix_UB_22      -0.0241098000
_diffrn_orient_matrix_UB_23      -0.1053812000
_diffrn_orient_matrix_UB_31      -0.1770384000
_diffrn_orient_matrix_UB_32      0.0021407000
_diffrn_orient_matrix_UB_33      0.0343974000
_diffrn_oxdiff_ac3_digest_frames 
;
01fa820f014a25903a845a8cfea8142a710165429a0
;
_diffrn_oxdiff_ac3_digest_hkl    
;
012e2ea6832b43c8494dc5cd3d332851769231
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5910
_reflns_number_total             6617
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         6617
_refine_ls_number_restraints     205
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0393
_refine_ls_restrained_S_all      1.138
_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)+(0.0624P)²+1.3133P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1076
_refine_ls_wR_factor_ref         0.1111
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F01B-B01G \\sim F4-B01G \\sim F2-B01G \\sim F01J-B01G \\sim F01H-B01G \\sim
F01K-B01G \\sim F016-B01G
 \\sim F01C-B01D \\sim F3-B01D \\sim F017-B01D \\sim F1-B01D \\sim F00E-B01D
\\sim F01E-B01D \\sim F0AA-B01D
 with sigma of 0.01
3. Rigid body (RIGU) restrains
 F016, B01G, F01J, F01B, F01H, F01K, F4, F2, F016, B01G, F01J, B01G, F01B,
 B01G, F01H, B01G, F01K, B01G, F4, B01G, F2, B01G
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1, F00E, B01D, F0AA, F017, F3, F01E, F01C, F00E, B01D, F0AA, B01D, F017,
 B01D, F3, B01D, F01E, B01D, F1, B01D, F01C, B01D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F01H)=Sof(F2)=Sof(F4)=1-FVAR(1)
 Sof(F01B)=Sof(F01J)=Sof(F01K)=FVAR(1)
 Sof(F1)=Sof(F0AA)=Sof(F3)=1-FVAR(2)
 Sof(F017)=Sof(F01C)=Sof(F01E)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C00J(H00J), N00K(H00K), N00L(H00L), C00M(H00M), C00O(H00O), C00Q(H00Q),
 C00R(H00R), C00S(H00S), C00T(H00T), C00V(H00V), C00W(H00W), C00X(H00X),
 C00Y(H00Y), C00Z(H00Z), C010(H010), C011(H011), C013(H013), C014(H014)
5.b Idealised Me refined as rotating group:
 C019(H01A,H01B,H01C), C01A(H01D,H01E,H01F), C01I(H01G,H01H,H01I)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Fe01 Fe 0.33396(4) 0.61519(2) 0.79549(3) 0.03697(11) Uani 1 1 d . . . . .
S002 S 0.37630(12) 0.44230(2) 0.82936(7) 0.0795(2) Uani 1 1 d . . . . .
S003 S 0.53039(12) 0.77730(2) 0.99633(7) 0.0756(2) Uani 1 1 d . . . . .
N004 N 0.3787(2) 0.66039(4) 0.81849(16) 0.0393(4) Uani 1 1 d . . . . .
N005 N 0.3029(2) 0.56954(4) 0.77606(16) 0.0397(4) Uani 1 1 d . . . . .
N006 N 0.6233(2) 0.64298(4) 0.89970(18) 0.0444(4) Uani 1 1 d . . . . .
N007 N 0.2421(2) 0.57097(4) 0.97552(16) 0.0439(4) Uani 1 1 d . . . . .
N008 N 0.1226(2) 0.66766(4) 0.73477(17) 0.0444(4) Uani 1 1 d . . . . .
N009 N 0.1210(2) 0.63382(4) 0.73370(17) 0.0431(4) Uani 1 1 d . . . . .
N00A N 0.3774(2) 0.57808(4) 0.58275(16) 0.0428(4) Uani 1 1 d . . . . .
N00B N 0.3925(2) 0.60986(4) 0.62312(17) 0.0422(4) Uani 1 1 d . . . . .
N00C N 0.5616(2) 0.61280(4) 0.86371(17) 0.0429(4) Uani 1 1 d . . . . .
N00D N 0.2620(2) 0.60410(4) 0.95989(17) 0.0430(4) Uani 1 1 d . . . . .
F00E F -0.0269(3) 0.72223(6) 0.92067(17) 0.0976(6) Uani 1 1 d D U . . .
C00F C 0.2669(3) 0.68278(5) 0.78095(19) 0.0402(4) Uani 1 1 d . . . . .
C00G C 0.2662(3) 0.55109(5) 0.87266(19) 0.0412(4) Uani 1 1 d . . . . .
C00H C 0.5240(3) 0.67013(5) 0.86915(19) 0.0410(4) Uani 1 1 d . . . . .
C00I C 0.3307(3) 0.55491(5) 0.66951(19) 0.0402(4) Uani 1 1 d . . . . .
C00J C 0.2975(3) 0.71588(5) 0.7890(2) 0.0469(5) Uani 1 1 d . . . . .
H00J H 0.220518 0.731153 0.759091 0.056 Uiso 1 1 calc R . . . .
N00K N 0.1572(3) 0.45785(5) 0.6460(3) 0.0702(6) Uani 1 1 d . . . . .
H00K H 0.106037 0.472972 0.603510 0.084 Uiso 1 1 calc R . . . .
N00L N 0.4751(3) 0.77736(5) 0.7515(2) 0.0686(6) Uani 1 1 d . . . . .
H00L H 0.451543 0.766447 0.684373 0.082 Uiso 1 1 calc R . . . .
C00M C 0.4419(3) 0.62640(6) 0.5277(2) 0.0502(5) Uani 1 1 d . . . . .
H00M H 0.461731 0.648798 0.527609 0.060 Uiso 1 1 calc R . . . .
C00N C 0.4479(3) 0.72549(5) 0.8435(2) 0.0465(5) Uani 1 1 d . . . . .
C00O C 0.4188(3) 0.57529(6) 0.4648(2) 0.0540(6) Uani 1 1 d . . . . .
H00O H 0.418884 0.556192 0.418048 0.065 Uiso 1 1 calc R . . . .
C00P C 0.2781(3) 0.50314(5) 0.7529(2) 0.0455(5) Uani 1 1 d . . . . .
C00Q C 0.2305(3) 0.61726(6) 1.0679(2) 0.0513(6) Uani 1 1 d . . . . .
H00Q H 0.233498 0.639556 1.085106 0.062 Uiso 1 1 calc R . . . .
C00R C 0.3160(3) 0.52182(5) 0.6515(2) 0.0452(5) Uani 1 1 d . . . . .
H00R H 0.330788 0.512278 0.575077 0.054 Uiso 1 1 calc R . . . .
C00S C 0.6768(3) 0.59172(6) 0.8978(2) 0.0520(6) Uani 1 1 d . . . . .
H00S H 0.669440 0.569255 0.884694 0.062 Uiso 1 1 calc R . . . .
C00T C 0.1925(3) 0.59310(7) 1.1515(2) 0.0599(6) Uani 1 1 d . . . . .
H00T H 0.166392 0.596263 1.232758 0.072 Uiso 1 1 calc R . . . .
C00U C 0.2622(3) 0.46693(5) 0.7379(2) 0.0518(6) Uani 1 1 d . . . . .
C00V C -0.0256(3) 0.62575(6) 0.6857(2) 0.0520(6) Uani 1 1 d . . . . .
H00V H -0.062111 0.604368 0.673375 0.062 Uiso 1 1 calc R . . . .
C00W C 0.4600(4) 0.60564(7) 0.4277(2) 0.0599(6) Uani 1 1 d . . . . .
H00W H 0.493662 0.611433 0.350611 0.072 Uiso 1 1 calc R . . . .
C00X C 0.5649(3) 0.70252(5) 0.8861(2) 0.0477(5) Uani 1 1 d . . . . .
H00X H 0.665346 0.708826 0.923844 0.057 Uiso 1 1 calc R . . . .
C00Y C -0.1190(3) 0.65369(7) 0.6558(3) 0.0612(7) Uani 1 1 d . . . . .
H00Y H -0.225686 0.654257 0.620693 0.073 Uiso 1 1 calc R . . . .
C00Z C 0.2557(3) 0.51765(5) 0.8668(2) 0.0473(5) Uani 1 1 d . . . . .
H00Z H 0.234550 0.505223 0.935722 0.057 Uiso 1 1 calc R . . . .
C010 C 0.7756(3) 0.63989(7) 0.9563(3) 0.0579(6) Uani 1 1 d . . . . .
H010 H 0.842278 0.656694 0.988674 0.069 Uiso 1 1 calc R . . . .
C011 C 0.8113(3) 0.60758(7) 0.9563(3) 0.0635(7) Uani 1 1 d . . . . .
H011 H 0.907189 0.597836 0.989126 0.076 Uiso 1 1 calc R . . . .
C012 C 0.4852(3) 0.76119(6) 0.8566(2) 0.0514(5) Uani 1 1 d . . . . .
C013 C -0.0230(3) 0.67978(6) 0.6882(2) 0.0537(6) Uani 1 1 d . . . . .
H013 H -0.051405 0.701744 0.680068 0.064 Uiso 1 1 calc R . . . .
C014 C 0.2009(3) 0.56391(7) 1.0914(2) 0.0550(6) Uani 1 1 d . . . . .
H014 H 0.182226 0.543266 1.123538 0.066 Uiso 1 1 calc R . . . .
N015 N 0.0047(5) 0.83312(8) 0.8562(3) 0.0973(9) Uani 1 1 d . . . . .
F016 F 0.1702(5) 0.48525(8) 0.1868(3) 0.1622(13) Uani 1 1 d D U . . .
F017 F 0.0546(11) 0.74499(10) 1.1069(5) 0.107(2) Uani 0.588(11) 1 d D U P A 1
O018 O -0.1246(5) 0.84589(9) 0.8289(5) 0.1631(17) Uani 1 1 d . . . . .
C019 C 0.1217(4) 0.42408(7) 0.6112(4) 0.0854(10) Uani 1 1 d . . . . .
H01A H 0.013949 0.422704 0.570705 0.128 Uiso 1 1 calc GR . . . .
H01B H 0.128893 0.410623 0.684246 0.128 Uiso 1 1 calc GR . . . .
H01C H 0.198698 0.416616 0.555584 0.128 Uiso 1 1 calc GR . . . .
C01A C 0.5009(5) 0.81245(7) 0.7401(3) 0.0892(11) Uani 1 1 d . . . . .
H01D H 0.501171 0.818157 0.653930 0.134 Uiso 1 1 calc GR . . . .
H01E H 0.603432 0.818287 0.782785 0.134 Uiso 1 1 calc GR . . . .
H01F H 0.415222 0.824035 0.776050 0.134 Uiso 1 1 calc GR . . . .
F01B F 0.3227(6) 0.4680(2) 0.3627(10) 0.158(4) Uani 0.581(11) 1 d D U P B 2
F01C F -0.0959(10) 0.7024(2) 1.0947(5) 0.147(4) Uani 0.588(11) 1 d D U P A 1
B01D B 0.0285(4) 0.71824(7) 1.0415(3) 0.0687(8) Uani 1 1 d D U . . .
F01E F 0.1561(12) 0.6980(3) 1.0438(7) 0.178(4) Uani 0.588(11) 1 d D U P A 1
O01F O 0.1236(5) 0.84853(11) 0.8688(5) 0.184(2) Uani 1 1 d . . . . .
B01G B 0.1868(4) 0.47925(8) 0.3089(3) 0.0735(9) Uani 1 1 d D U . . .
F01H F 0.0654(8) 0.4810(3) 0.3843(7) 0.121(4) Uani 0.419(11) 1 d D U P B 1
C01I C 0.0044(7) 0.79813(9) 0.8786(4) 0.1129(15) Uani 1 1 d . . . . .
H01G H -0.086788 0.792504 0.923972 0.169 Uiso 1 1 calc GR . . . .
H01H H 0.103219 0.791985 0.925927 0.169 Uiso 1 1 calc GR . . . .
H01I H -0.003414 0.786728 0.800635 0.169 Uiso 1 1 calc GR . . . .
F01J F 0.1447(11) 0.5055(2) 0.3674(8) 0.177(5) Uani 0.581(11) 1 d D U P B 2
F01K F 0.0742(8) 0.45503(18) 0.3116(9) 0.159(4) Uani 0.581(11) 1 d D U P B 2
F2 F 0.2853(19) 0.5045(3) 0.3502(9) 0.181(6) Uani 0.419(11) 1 d D U P B 1
F1 F 0.1566(17) 0.7389(3) 1.0582(11) 0.165(6) Uani 0.412(11) 1 d D U P A 2
F0AA F 0.0843(18) 0.69013(15) 1.0856(11) 0.144(5) Uani 0.412(11) 1 d D U P A 2
F3 F -0.0843(19) 0.7299(6) 1.1114(8) 0.233(10) Uani 0.412(11) 1 d D U P A 2
F4 F 0.2746(18) 0.4522(3) 0.3342(11) 0.158(5) Uani 0.419(11) 1 d D U P B 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
Fe01 N004 1.8957(17) . ?
Fe01 N005 1.8923(18) . ?
Fe01 N009 1.9812(19) . ?
Fe01 N00B 1.9746(18) . ?
Fe01 N00C 1.9644(19) . ?
Fe01 N00D 1.9719(19) . ?
F01Ca B01D 1.379(5) . ?
F017a B01D 1.310(4) . ?
F01Bb B01G 1.303(5) . ?
S002 C00U 1.650(3) . ?
S003 C012 1.661(2) . ?
N004 C00F 1.339(3) . ?
N004 C00H 1.338(3) . ?
N005 C00G 1.342(3) . ?
N005 C00I 1.334(3) . ?
N006 N00C 1.378(2) . ?
N006 C00H 1.403(3) . ?
N006 C010 1.358(3) . ?
N007 N00D 1.376(3) . ?
N007 C00G 1.404(3) . ?
N007 C014 1.356(3) . ?
N008 N009 1.383(2) . ?
N008 C00F 1.398(3) . ?
N008 C013 1.358(3) . ?
N009 C00V 1.319(3) . ?
N00A N00B 1.372(2) . ?
N00A C00I 1.409(3) . ?
N00A C00O 1.351(3) . ?
N00B C00M 1.325(3) . ?
N00C C00S 1.313(3) . ?
N00D C00Q 1.330(3) . ?
F00E B01D 1.357(3) . ?
C00F C00J 1.377(3) . ?
C00G C00Z 1.370(3) . ?
C00H C00X 1.375(3) . ?
C00I C00R 1.370(3) . ?
C00J C00N 1.386(3) . ?
N00K C00U 1.316(4) . ?
N00K C019 1.454(3) . ?
N00L C012 1.310(3) . ?
N00L C01A 1.456(3) . ?
C00M C00W 1.392(4) . ?
C00N C00X 1.398(3) . ?
C00N C012 1.495(3) . ?
C00O C00W 1.355(4) . ?
C00P C00R 1.393(3) . ?
C00P C00U 1.493(3) . ?
C00P C00Z 1.392(3) . ?
C00Q C00T 1.392(4) . ?
C00S C011 1.392(4) . ?
C00T C014 1.362(4) . ?
C00V C00Y 1.401(4) . ?
C00Y C013 1.357(4) . ?
C010 C011 1.353(4) . ?
N015 O018 1.203(5) . ?
N015 O01F 1.165(5) . ?
N015 C01I 1.450(4) . ?
F016 B01G 1.338(4) . ?
B01D F01E 1.339(5) . ?
B01D F1 1.354(6) . ?
B01D F0AA 1.312(6) . ?
B01D F3 1.336(6) . ?
B01G F01H 1.346(5) . ?
B01G F01J 1.305(5) . ?
B01G F01K 1.360(5) . ?
B01G F2 1.366(6) . ?
B01G F4 1.337(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
F01Ea B01D F00E 107.2(4) . . ?
N004 Fe01 N009 80.07(7) . . ?
N004 Fe01 N00B 99.84(7) . . ?
F017a B01D F00E 116.5(3) . . ?
N004 Fe01 N00C 80.18(7) . . ?
F1b B01D F00E 104.6(5) . . ?
N004 Fe01 N00D 100.12(7) . . ?
F3b B01D F00E 107.8(5) . . ?
F0AAb B01D F00E 122.3(5) . . ?
F01Ea B01D F01C 108.3(6) . . ?
F017a B01D F01C 105.2(4) . . ?
N005 Fe01 N004 176.46(8) . . ?
N005 Fe01 N009 103.46(8) . . ?
N005 Fe01 N00B 80.10(7) . . ?
N005 Fe01 N00C 96.28(7) . . ?
N005 Fe01 N00D 79.93(7) . . ?
N00B Fe01 N009 90.23(8) . . ?
N00C Fe01 N009 160.25(7) . . ?
N00C Fe01 N00B 92.70(8) . . ?
N00C Fe01 N00D 90.05(8) . . ?
N00D Fe01 N009 93.83(8) . . ?
F017a B01D F01E 114.3(6) . . ?
F3b B01D F1 105.9(10) . . ?
F0AAb B01D F1 104.5(8) . . ?
F0AAb B01D F3 110.3(8) . . ?
F01Bb B01G F016 121.3(5) . . ?
F4a B01G F016 111.3(6) . . ?
F01Jb B01G F016 108.5(5) . . ?
F4a B01G F01H 109.8(7) . . ?
F01Bb B01G F01J 109.0(6) . . ?
F01Bb B01G F01K 107.4(5) . . ?
F01Jb B01G F01K 112.1(6) . . ?
F4a B01G F2 105.0(8) . . ?
F01Ha B01G F2 102.4(6) . . ?
N00D Fe01 N00B 160.03(8) . . ?
C00F N004 Fe01 120.29(14) . . ?
C00H N004 Fe01 120.12(14) . . ?
C00H N004 C00F 119.56(18) . . ?
C00G N005 Fe01 120.31(14) . . ?
C00I N005 Fe01 120.41(14) . . ?
C00I N005 C00G 119.04(18) . . ?
N00C N006 C00H 116.50(17) . . ?
C010 N006 N00C 110.53(18) . . ?
C010 N006 C00H 132.9(2) . . ?
N00D N007 C00G 116.49(17) . . ?
C014 N007 N00D 111.37(18) . . ?
C014 N007 C00G 132.1(2) . . ?
N009 N008 C00F 116.90(17) . . ?
C013 N008 N009 110.75(18) . . ?
C013 N008 C00F 132.4(2) . . ?
N008 N009 Fe01 111.96(13) . . ?
C00V N009 Fe01 142.83(17) . . ?
C00V N009 N008 105.14(19) . . ?
N00B N00A C00I 116.56(17) . . ?
C00O N00A N00B 110.88(18) . . ?
C00O N00A C00I 132.49(19) . . ?
N00A N00B Fe01 112.42(13) . . ?
C00M N00B Fe01 142.45(16) . . ?
C00M N00B N00A 105.12(18) . . ?
N006 N00C Fe01 112.41(13) . . ?
C00S N00C Fe01 141.86(17) . . ?
C00S N00C N006 105.41(19) . . ?
N007 N00D Fe01 112.63(13) . . ?
C00Q N00D Fe01 142.45(17) . . ?
C00Q N00D N007 104.84(18) . . ?
N004 C00F N008 110.62(18) . . ?
N004 C00F C00J 122.2(2) . . ?
C00J C00F N008 127.1(2) . . ?
N005 C00G N007 110.26(18) . . ?
N005 C00G C00Z 122.8(2) . . ?
C00Z C00G N007 127.0(2) . . ?
N004 C00H N006 110.39(18) . . ?
N004 C00H C00X 122.9(2) . . ?
C00X C00H N006 126.7(2) . . ?
N005 C00I N00A 110.45(18) . . ?
N005 C00I C00R 123.1(2) . . ?
C00R C00I N00A 126.48(19) . . ?
C00F C00J C00N 117.3(2) . . ?
C00U N00K C019 124.7(3) . . ?
C012 N00L C01A 124.8(2) . . ?
N00B C00M C00W 110.7(2) . . ?
C00J C00N C00X 121.3(2) . . ?
C00J C00N C012 119.2(2) . . ?
C00X C00N C012 119.5(2) . . ?
N00A C00O C00W 107.0(2) . . ?
C00R C00P C00U 118.7(2) . . ?
C00Z C00P C00R 121.2(2) . . ?
C00Z C00P C00U 120.1(2) . . ?
N00D C00Q C00T 110.7(2) . . ?
C00I C00R C00P 116.9(2) . . ?
N00C C00S C011 110.8(2) . . ?
C014 C00T C00Q 106.7(2) . . ?
N00K C00U S002 125.99(19) . . ?
N00K C00U C00P 114.1(2) . . ?
C00P C00U S002 119.89(19) . . ?
N009 C00V C00Y 110.9(2) . . ?
C00O C00W C00M 106.4(2) . . ?
C00H C00X C00N 116.6(2) . . ?
C013 C00Y C00V 106.4(2) . . ?
C00G C00Z C00P 117.0(2) . . ?
C011 C010 N006 106.5(2) . . ?
C010 C011 C00S 106.8(2) . . ?
N00L C012 S003 125.56(18) . . ?
N00L C012 C00N 114.3(2) . . ?
C00N C012 S003 120.10(18) . . ?
C00Y C013 N008 106.8(2) . . ?
N007 C014 C00T 106.3(2) . . ?
O018 N015 C01I 117.0(4) . . ?
O01F N015 O018 121.1(4) . . ?
O01F N015 C01I 121.8(5) . . ?
F00E B01D F01C 104.7(4) . . ?
F016 B01G F01H 124.5(4) . . ?
F016 B01G F01K 98.1(4) . . ?
F016 B01G F2 101.2(5) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.374
_oxdiff_exptl_absorpt_empirical_full_min 0.747
####################################################################### 
# 
# 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_M171023B
_database_code_depnum_ccdc_archive 'CCDC 1860676'
_audit_update_record             
;
2018-08-07 deposited with the CCDC.
2018-11-09 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C26 H26 B2 F8 Fe N14 O4 S2'
_chemical_formula_moiety         '2(C12 H10 N6 S) Fe, 2(B F4), 2(C H3 N O2)'
_chemical_formula_weight         892.16
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
_space_group_IT_number           15
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
#------------------------------------------------------------------------------
_cell_length_a                   51.605(2)
_cell_length_b                   8.3203(4)
_cell_length_c                   16.7867(7)
_cell_angle_alpha                90.0000
_cell_angle_beta                 93.676(7)
_cell_angle_gamma                90.0000
_cell_volume                     7192.8(6)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    24895
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      27.45
_cell_measurement_temperature    100
#------------------------------------------------------------------------------
_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3616.00
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.511
_exptl_absorpt_correction_T_max  0.969

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      100
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            32615
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_theta_max         27.467
_diffrn_reflns_theta_min         2.373
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_limit_h_min       -63
_diffrn_reflns_limit_h_max       66
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             8201
_reflns_number_gt                6529
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0442
_refine_ls_wR_factor_ref         0.1188
_refine_ls_wR_factor_gt          0.1097
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_reflns         8201
_refine_ls_number_parameters     530
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0535P)²+18.6222P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         0.60
_refine_diff_density_min         -0.75
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
B B 0.0013 0.0007
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
F F 0.0171 0.0103
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Fe Fe 0.3463 0.8444
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.12443(2) 0.24080(4) 0.02644(2) 0.01565(9) Uani 1 1 d . . . . .
S1 S 0.25818(2) 0.20988(9) 0.16709(4) 0.02454(15) Uani 1 1 d . . . . .
S2 S -0.01301(2) 0.28177(8) 0.04085(4) 0.02398(15) Uani 1 1 d . . . . .
F1 F 0.20078(4) -0.2903(3) -0.16030(10) 0.0435(5) Uani 1 1 d . . . . .
F2 F 0.22443(3) -0.3017(2) -0.04167(10) 0.0344(4) Uani 1 1 d . . . . .
F3 F 0.19763(3) -0.0884(2) -0.07001(12) 0.0389(4) Uani 1 1 d . . . . .
F4 F 0.18071(3) -0.3340(2) -0.04525(10) 0.0309(4) Uani 1 1 d . . . . .
F5 F 0.05419(3) 0.0696(2) -0.33169(9) 0.0308(4) Uani 1 1 d . . . . .
F6 F 0.07506(3) 0.1515(3) -0.21515(11) 0.0451(5) Uani 1 1 d . . . . .
F7 F 0.03115(4) 0.1698(3) -0.23219(11) 0.0451(5) Uani 1 1 d . . . . .
F8 F 0.05090(4) -0.0717(2) -0.21669(11) 0.0499(5) Uani 1 1 d . . . . .
O1 O 0.19411(4) -0.3827(3) 0.15765(14) 0.0398(5) Uani 1 1 d . . . . .
O2 O 0.17594(4) -0.1535(3) 0.13159(14) 0.0394(5) Uani 1 1 d . . . . .
O3 O 0.06412(4) 0.4669(3) 0.35253(12) 0.0376(5) Uani 1 1 d . . . . .
O4 O 0.07840(5) 0.4121(3) 0.23764(14) 0.0465(6) Uani 1 1 d . . . . .
N1 N 0.25141(4) 0.4478(3) 0.06342(14) 0.0247(5) Uani 1 1 d . . . . .
N2 N 0.16084(4) 0.2528(2) 0.04809(11) 0.0164(4) Uani 1 1 d . . . . .
N3 N 0.16137(4) 0.3316(3) -0.08040(12) 0.0185(4) Uani 1 1 d . . . . .
N4 N 0.13469(4) 0.3161(3) -0.07864(12) 0.0187(4) Uani 1 1 d . . . . .
N5 N 0.15224(4) 0.1691(3) 0.17098(12) 0.0175(4) Uani 1 1 d . . . . .
N6 N 0.12701(4) 0.1650(3) 0.13750(12) 0.0184(4) Uani 1 1 d . . . . .
N7 N -0.00259(5) 0.1560(3) -0.09891(15) 0.0293(5) Uani 1 1 d . . . . .
N8 N 0.08785(4) 0.2350(2) 0.00794(11) 0.0163(4) Uani 1 1 d . . . . .
N9 N 0.09464(4) -0.0150(3) -0.03803(12) 0.0178(4) Uani 1 1 d . . . . .
N10 N 0.12023(4) 0.0205(3) -0.01553(12) 0.0177(4) Uani 1 1 d . . . . .
N11 N 0.08929(4) 0.4850(2) 0.05928(12) 0.0183(4) Uani 1 1 d . . . . .
N12 N 0.11568(4) 0.4578(3) 0.06217(12) 0.0179(4) Uani 1 1 d . . . . .
N13 N 0.19522(5) -0.2392(3) 0.14219(14) 0.0278(5) Uani 1 1 d . . . . .
N14 N 0.06080(5) 0.4346(3) 0.28161(14) 0.0308(5) Uani 1 1 d . . . . .
C1 C 0.24132(5) 0.3270(3) 0.10233(14) 0.0201(5) Uani 1 1 d . . . . .
C2 C 0.21300(4) 0.2974(3) 0.08289(14) 0.0180(5) Uani 1 1 d . . . . .
C3 C 0.20240(5) 0.3275(3) 0.00548(14) 0.0187(5) Uani 1 1 d . . . . .
H3 H 0.212891 0.362763 -0.035597 0.022 Uiso 1 1 calc R U . . .
C4 C 0.19741(4) 0.2429(3) 0.14278(14) 0.0180(5) Uani 1 1 d . . . . .
H4 H 0.204458 0.221840 0.195406 0.022 Uiso 1 1 calc R U . . .
C5 C 0.17593(5) 0.3036(3) -0.00860(14) 0.0175(5) Uani 1 1 d . . . . .
C6 C 0.17136(5) 0.2214(3) 0.12171(14) 0.0173(5) Uani 1 1 d . . . . .
C7 C 0.16806(5) 0.3840(3) -0.15310(14) 0.0232(5) Uani 1 1 d . . . . .
H7 H 0.185113 0.404201 -0.168851 0.028 Uiso 1 1 calc R U . . .
C8 C 0.14537(5) 0.4017(4) -0.19903(15) 0.0270(6) Uani 1 1 d . . . . .
H8 H 0.143559 0.436745 -0.252965 0.032 Uiso 1 1 calc R U . . .
C9 C 0.12528(5) 0.3581(3) -0.15079(14) 0.0218(5) Uani 1 1 d . . . . .
H9 H 0.107358 0.358555 -0.167686 0.026 Uiso 1 1 calc R U . . .
C10 C 0.15346(5) 0.1001(3) 0.24511(14) 0.0210(5) Uani 1 1 d . . . . .
H10 H 0.168557 0.086945 0.279934 0.025 Uiso 1 1 calc R U . . .
C11 C 0.12882(5) 0.0536(3) 0.25946(15) 0.0222(5) Uani 1 1 d . . . . .
H11 H 0.123424 0.001697 0.305991 0.027 Uiso 1 1 calc R U . . .
C12 C 0.11304(5) 0.0979(3) 0.19177(14) 0.0201(5) Uani 1 1 d . . . . .
H12 H 0.094797 0.081772 0.185812 0.024 Uiso 1 1 calc R U . . .
C13 C 0.00592(5) 0.2180(3) -0.02927(15) 0.0214(5) Uani 1 1 d . . . . .
C14 C 0.03487(4) 0.2243(3) -0.01595(14) 0.0187(5) Uani 1 1 d . . . . .
C15 C 0.04967(5) 0.0922(3) -0.03786(14) 0.0200(5) Uani 1 1 d . . . . .
H15 H 0.041761 -0.000953 -0.061419 0.024 Uiso 1 1 calc R U . . .
C16 C 0.04669(5) 0.3609(3) 0.01856(14) 0.0195(5) Uani 1 1 d . . . . .
H16 H 0.036772 0.450044 0.034645 0.023 Uiso 1 1 calc R U . . .
C17 C 0.07636(5) 0.1035(3) -0.02360(14) 0.0176(5) Uani 1 1 d . . . . .
C18 C 0.07349(5) 0.3603(3) 0.02817(14) 0.0176(5) Uani 1 1 d . . . . .
C19 C 0.09255(5) -0.1632(3) -0.07179(14) 0.0203(5) Uani 1 1 d . . . . .
H19 H 0.076991 -0.213879 -0.091982 0.024 Uiso 1 1 calc R U . . .
C20 C 0.11707(5) -0.2255(3) -0.07120(14) 0.0215(5) Uani 1 1 d . . . . .
H20 H 0.121953 -0.327432 -0.090888 0.026 Uiso 1 1 calc R U . . .
C21 C 0.13360(5) -0.1078(3) -0.03547(14) 0.0205(5) Uani 1 1 d . . . . .
H21 H 0.151888 -0.118817 -0.026796 0.025 Uiso 1 1 calc R U . . .
C22 C 0.08385(5) 0.6284(3) 0.09396(15) 0.0225(5) Uani 1 1 d . . . . .
H22 H 0.067111 0.672876 0.099616 0.027 Uiso 1 1 calc R U . . .
C23 C 0.10710(5) 0.6955(3) 0.11896(15) 0.0240(5) Uani 1 1 d . . . . .
H23 H 0.109784 0.795594 0.145445 0.029 Uiso 1 1 calc R U . . .
C24 C 0.12626(5) 0.5864(3) 0.09755(14) 0.0207(5) Uani 1 1 d . . . . .
H24 H 0.144405 0.602782 0.107195 0.025 Uiso 1 1 calc R U . . .
C25 C 0.22103(6) -0.1641(4) 0.13609(18) 0.0331(6) Uani 1 1 d . . . . .
H25A H 0.218852 -0.049691 0.123517 0.040 Uiso 1 1 calc R U . . .
H25B H 0.231249 -0.175926 0.187011 0.040 Uiso 1 1 calc R U . . .
H25C H 0.230083 -0.216993 0.093715 0.040 Uiso 1 1 calc R U . . .
C26 C 0.03355(6) 0.4243(5) 0.2478(2) 0.0432(8) Uani 1 1 d . . . . .
H26A H 0.021695 0.445035 0.289953 0.052 Uiso 1 1 calc R U . . .
H26B H 0.030687 0.504390 0.205342 0.052 Uiso 1 1 calc R U . . .
H26C H 0.030277 0.316565 0.225760 0.052 Uiso 1 1 calc R U . . .
B1 B 0.20083(6) -0.2550(4) -0.08005(18) 0.0240(6) Uani 1 1 d . . . . .
B2 B 0.05291(5) 0.0806(4) -0.24823(17) 0.0235(6) Uani 1 1 d . . . . .
H1A H 0.2674(7) 0.475(4) 0.0711(19) 0.035(9) Uiso 1 1 d . . . . .
H1B H 0.2422(6) 0.515(4) 0.031(2) 0.036(9) Uiso 1 1 d . . . . .
H7A H 0.0083(6) 0.136(4) -0.1398(18) 0.026(8) Uiso 1 1 d . . . . .
H7B H -0.0174(7) 0.136(5) -0.108(2) 0.043(10) Uiso 1 1 d . . . . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL Version 2017/1 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.5 (Rigaku, 2017)'
_computing_molecular_graphics    'CrystalStructure 4.2.5'

#==============================================================================
# MOLECULAR GEOMETRY

_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 1.894(2) . ?
Fe1 N8 1.8939(19) . ?
Fe1 N12 1.964(2) . ?
Fe1 N6 1.965(2) . ?
Fe1 N10 1.971(2) . ?
Fe1 N4 1.976(2) . ?
S1 C1 1.664(3) . ?
S2 C13 1.664(3) . ?
F1 B1 1.379(4) . ?
F2 B1 1.396(3) . ?
F3 B1 1.408(4) . ?
F4 B1 1.389(3) . ?
F5 B2 1.410(3) . ?
F6 B2 1.372(3) . ?
F7 B2 1.387(3) . ?
F8 B2 1.380(4) . ?
O1 N13 1.224(3) . ?
O2 N13 1.228(3) . ?
O3 N14 1.222(3) . ?
O4 N14 1.221(3) . ?
N1 C1 1.323(3) . ?
N1 H1A 0.86(3) . ?
N1 H1B 0.90(4) . ?
N2 C5 1.336(3) . ?
N2 C6 1.343(3) . ?
N3 C7 1.361(3) . ?
N3 N4 1.385(3) . ?
N3 C5 1.398(3) . ?
N4 C9 1.323(3) . ?
N5 C10 1.368(3) . ?
N5 N6 1.385(3) . ?
N5 C6 1.397(3) . ?
N6 C12 1.321(3) . ?
N7 C13 1.326(4) . ?
N7 H7A 0.93(3) . ?
N7 H7B 0.79(4) . ?
N8 C18 1.336(3) . ?
N8 C17 1.337(3) . ?
N9 C19 1.358(3) . ?
N9 N10 1.382(3) . ?
N9 C17 1.397(3) . ?
N10 C21 1.326(3) . ?
N11 C22 1.365(3) . ?
N11 N12 1.378(3) . ?
N11 C18 1.400(3) . ?
N12 C24 1.324(3) . ?
N13 C25 1.481(4) . ?
N14 C26 1.485(4) . ?
C1 C2 1.498(3) . ?
C2 C3 1.400(3) . ?
C2 C4 1.402(3) . ?
C3 C5 1.385(3) . ?
C3 H3 0.9500 . ?
C4 C6 1.380(3) . ?
C4 H4 0.9500 . ?
C7 C8 1.368(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.403(4) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.365(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.404(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.497(3) . ?
C14 C16 1.398(3) . ?
C14 C15 1.401(3) . ?
C15 C17 1.386(3) . ?
C15 H15 0.9500 . ?
C16 C18 1.382(3) . ?
C16 H16 0.9500 . ?
C19 C20 1.367(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.408(4) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C23 1.365(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.406(4) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 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 N8 177.74(9) . . ?
N2 Fe1 N12 97.91(8) . . ?
N8 Fe1 N12 80.06(8) . . ?
N2 Fe1 N6 80.14(8) . . ?
N8 Fe1 N6 98.83(8) . . ?
N12 Fe1 N6 90.47(8) . . ?
N2 Fe1 N10 101.70(8) . . ?
N8 Fe1 N10 80.33(8) . . ?
N12 Fe1 N10 160.39(8) . . ?
N6 Fe1 N10 92.29(8) . . ?
N2 Fe1 N4 80.51(8) . . ?
N8 Fe1 N4 100.55(8) . . ?
N12 Fe1 N4 93.51(9) . . ?
N6 Fe1 N4 160.61(8) . . ?
N10 Fe1 N4 90.31(9) . . ?
C1 N1 H1A 122(2) . . ?
C1 N1 H1B 124(2) . . ?
H1A N1 H1B 113(3) . . ?
C5 N2 C6 119.8(2) . . ?
C5 N2 Fe1 119.77(16) . . ?
C6 N2 Fe1 120.25(16) . . ?
C7 N3 N4 111.00(19) . . ?
C7 N3 C5 132.3(2) . . ?
N4 N3 C5 116.49(19) . . ?
C9 N4 N3 105.2(2) . . ?
C9 N4 Fe1 142.91(18) . . ?
N3 N4 Fe1 111.85(14) . . ?
C10 N5 N6 110.2(2) . . ?
C10 N5 C6 132.6(2) . . ?
N6 N5 C6 116.65(19) . . ?
C12 N6 N5 105.71(19) . . ?
C12 N6 Fe1 141.57(17) . . ?
N5 N6 Fe1 112.45(15) . . ?
C13 N7 H7A 122.8(18) . . ?
C13 N7 H7B 121(3) . . ?
H7A N7 H7B 117(3) . . ?
C18 N8 C17 120.0(2) . . ?
C18 N8 Fe1 120.10(16) . . ?
C17 N8 Fe1 119.86(16) . . ?
C19 N9 N10 110.93(19) . . ?
C19 N9 C17 132.6(2) . . ?
N10 N9 C17 116.49(19) . . ?
C21 N10 N9 105.2(2) . . ?
C21 N10 Fe1 142.39(17) . . ?
N9 N10 Fe1 112.20(15) . . ?
C22 N11 N12 111.0(2) . . ?
C22 N11 C18 132.5(2) . . ?
N12 N11 C18 116.23(19) . . ?
C24 N12 N11 105.1(2) . . ?
C24 N12 Fe1 141.57(18) . . ?
N11 N12 Fe1 112.71(15) . . ?
O1 N13 O2 123.3(2) . . ?
O1 N13 C25 118.8(2) . . ?
O2 N13 C25 118.0(2) . . ?
O4 N14 O3 124.0(3) . . ?
O4 N14 C26 118.9(3) . . ?
O3 N14 C26 117.1(3) . . ?
N1 C1 C2 115.3(2) . . ?
N1 C1 S1 124.17(19) . . ?
C2 C1 S1 120.54(19) . . ?
C3 C2 C4 121.0(2) . . ?
C3 C2 C1 119.4(2) . . ?
C4 C2 C1 119.6(2) . . ?
C5 C3 C2 117.1(2) . . ?
C5 C3 H3 121.5 . . ?
C2 C3 H3 121.5 . . ?
C6 C4 C2 116.9(2) . . ?
C6 C4 H4 121.6 . . ?
C2 C4 H4 121.6 . . ?
N2 C5 C3 122.5(2) . . ?
N2 C5 N3 111.2(2) . . ?
C3 C5 N3 126.3(2) . . ?
N2 C6 C4 122.7(2) . . ?
N2 C6 N5 110.3(2) . . ?
C4 C6 N5 127.0(2) . . ?
N3 C7 C8 106.4(2) . . ?
N3 C7 H7 126.8 . . ?
C8 C7 H7 126.8 . . ?
C7 C8 C9 106.5(2) . . ?
C7 C8 H8 126.7 . . ?
C9 C8 H8 126.7 . . ?
N4 C9 C8 110.8(2) . . ?
N4 C9 H9 124.6 . . ?
C8 C9 H9 124.6 . . ?
C11 C10 N5 106.9(2) . . ?
C11 C10 H10 126.6 . . ?
N5 C10 H10 126.6 . . ?
C10 C11 C12 106.4(2) . . ?
C10 C11 H11 126.8 . . ?
C12 C11 H11 126.8 . . ?
N6 C12 C11 110.8(2) . . ?
N6 C12 H12 124.6 . . ?
C11 C12 H12 124.6 . . ?
N7 C13 C14 114.6(2) . . ?
N7 C13 S2 124.8(2) . . ?
C14 C13 S2 120.57(19) . . ?
C16 C14 C15 121.1(2) . . ?
C16 C14 C13 119.7(2) . . ?
C15 C14 C13 119.2(2) . . ?
C17 C15 C14 117.0(2) . . ?
C17 C15 H15 121.5 . . ?
C14 C15 H15 121.5 . . ?
C18 C16 C14 116.9(2) . . ?
C18 C16 H16 121.6 . . ?
C14 C16 H16 121.6 . . ?
N8 C17 C15 122.3(2) . . ?
N8 C17 N9 111.0(2) . . ?
C15 C17 N9 126.7(2) . . ?
N8 C18 C16 122.7(2) . . ?
N8 C18 N11 110.7(2) . . ?
C16 C18 N11 126.5(2) . . ?
N9 C19 C20 107.0(2) . . ?
N9 C19 H19 126.5 . . ?
C20 C19 H19 126.5 . . ?
C19 C20 C21 105.9(2) . . ?
C19 C20 H20 127.0 . . ?
C21 C20 H20 127.0 . . ?
N10 C21 C20 110.9(2) . . ?
N10 C21 H21 124.5 . . ?
C20 C21 H21 124.5 . . ?
N11 C22 C23 106.7(2) . . ?
N11 C22 H22 126.6 . . ?
C23 C22 H22 126.6 . . ?
C22 C23 C24 106.0(2) . . ?
C22 C23 H23 127.0 . . ?
C24 C23 H23 127.0 . . ?
N12 C24 C23 111.1(2) . . ?
N12 C24 H24 124.5 . . ?
C23 C24 H24 124.5 . . ?
N13 C25 H25A 109.5 . . ?
N13 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
N13 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N14 C26 H26A 109.5 . . ?
N14 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
N14 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
F1 B1 F4 110.8(2) . . ?
F1 B1 F2 109.8(2) . . ?
F4 B1 F2 109.1(2) . . ?
F1 B1 F3 109.5(2) . . ?
F4 B1 F3 108.6(2) . . ?
F2 B1 F3 108.9(2) . . ?
F6 B2 F8 108.7(2) . . ?
F6 B2 F7 110.8(3) . . ?
F8 B2 F7 109.6(2) . . ?
F6 B2 F5 109.8(2) . . ?
F8 B2 F5 109.3(2) . . ?
F7 B2 F5 108.5(2) . . ?

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
N12 Fe1 N2 C5 -90.96(19) . . . . ?
N6 Fe1 N2 C5 179.9(2) . . . . ?
N10 Fe1 N2 C5 89.63(19) . . . . ?
N4 Fe1 N2 C5 1.30(19) . . . . ?
N12 Fe1 N2 C6 84.34(19) . . . . ?
N6 Fe1 N2 C6 -4.76(18) . . . . ?
N10 Fe1 N2 C6 -95.07(19) . . . . ?
N4 Fe1 N2 C6 176.6(2) . . . . ?
C7 N3 N4 C9 0.5(3) . . . . ?
C5 N3 N4 C9 176.1(2) . . . . ?
C7 N3 N4 Fe1 -179.83(17) . . . . ?
C5 N3 N4 Fe1 -4.3(3) . . . . ?
C10 N5 N6 C12 1.6(3) . . . . ?
C6 N5 N6 C12 174.0(2) . . . . ?
C10 N5 N6 Fe1 -173.78(16) . . . . ?
C6 N5 N6 Fe1 -1.3(3) . . . . ?
N12 Fe1 N8 C18 -3.13(18) . . . . ?
N6 Fe1 N8 C18 85.79(19) . . . . ?
N10 Fe1 N8 C18 176.62(19) . . . . ?
N4 Fe1 N8 C18 -94.88(19) . . . . ?
N12 Fe1 N8 C17 178.53(19) . . . . ?
N6 Fe1 N8 C17 -92.54(18) . . . . ?
N10 Fe1 N8 C17 -1.71(18) . . . . ?
N4 Fe1 N8 C17 86.78(19) . . . . ?
C19 N9 N10 C21 -0.4(3) . . . . ?
C17 N9 N10 C21 -179.6(2) . . . . ?
C19 N9 N10 Fe1 175.76(16) . . . . ?
C17 N9 N10 Fe1 -3.5(2) . . . . ?
C22 N11 N12 C24 -1.0(3) . . . . ?
C18 N11 N12 C24 -176.4(2) . . . . ?
C22 N11 N12 Fe1 172.17(16) . . . . ?
C18 N11 N12 Fe1 -3.3(2) . . . . ?
N1 C1 C2 C3 33.0(3) . . . . ?
S1 C1 C2 C3 -145.6(2) . . . . ?
N1 C1 C2 C4 -145.8(2) . . . . ?
S1 C1 C2 C4 35.7(3) . . . . ?
C4 C2 C3 C5 1.0(4) . . . . ?
C1 C2 C3 C5 -177.8(2) . . . . ?
C3 C2 C4 C6 -0.2(4) . . . . ?
C1 C2 C4 C6 178.5(2) . . . . ?
C6 N2 C5 C3 -0.7(4) . . . . ?
Fe1 N2 C5 C3 174.61(19) . . . . ?
C6 N2 C5 N3 -179.2(2) . . . . ?
Fe1 N2 C5 N3 -3.9(3) . . . . ?
C2 C3 C5 N2 -0.6(4) . . . . ?
C2 C3 C5 N3 177.7(2) . . . . ?
C7 N3 C5 N2 179.6(3) . . . . ?
N4 N3 C5 N2 5.2(3) . . . . ?
C7 N3 C5 C3 1.2(4) . . . . ?
N4 N3 C5 C3 -173.2(2) . . . . ?
C5 N2 C6 C4 1.6(4) . . . . ?
Fe1 N2 C6 C4 -173.73(19) . . . . ?
C5 N2 C6 N5 -179.5(2) . . . . ?
Fe1 N2 C6 N5 5.1(3) . . . . ?
C2 C4 C6 N2 -1.1(4) . . . . ?
C2 C4 C6 N5 -179.8(2) . . . . ?
C10 N5 C6 N2 168.2(2) . . . . ?
N6 N5 C6 N2 -2.2(3) . . . . ?
C10 N5 C6 C4 -13.0(4) . . . . ?
N6 N5 C6 C4 176.6(2) . . . . ?
N4 N3 C7 C8 -0.3(3) . . . . ?
C5 N3 C7 C8 -174.9(3) . . . . ?
N3 C7 C8 C9 0.0(3) . . . . ?
N3 N4 C9 C8 -0.5(3) . . . . ?
Fe1 N4 C9 C8 180.0(2) . . . . ?
C7 C8 C9 N4 0.3(3) . . . . ?
N6 N5 C10 C11 -0.8(3) . . . . ?
C6 N5 C10 C11 -171.7(3) . . . . ?
N5 C10 C11 C12 -0.2(3) . . . . ?
N5 N6 C12 C11 -1.7(3) . . . . ?
Fe1 N6 C12 C11 171.4(2) . . . . ?
C10 C11 C12 N6 1.2(3) . . . . ?
N7 C13 C14 C16 137.9(3) . . . . ?
S2 C13 C14 C16 -43.4(3) . . . . ?
N7 C13 C14 C15 -42.6(3) . . . . ?
S2 C13 C14 C15 136.2(2) . . . . ?
C16 C14 C15 C17 0.1(4) . . . . ?
C13 C14 C15 C17 -179.4(2) . . . . ?
C15 C14 C16 C18 1.4(4) . . . . ?
C13 C14 C16 C18 -179.1(2) . . . . ?
C18 N8 C17 C15 1.2(3) . . . . ?
Fe1 N8 C17 C15 179.52(18) . . . . ?
C18 N8 C17 N9 -178.1(2) . . . . ?
Fe1 N8 C17 N9 0.3(3) . . . . ?
C14 C15 C17 N8 -1.5(4) . . . . ?
C14 C15 C17 N9 177.7(2) . . . . ?
C19 N9 C17 N8 -176.9(2) . . . . ?
N10 N9 C17 N8 2.2(3) . . . . ?
C19 N9 C17 C15 3.9(4) . . . . ?
N10 N9 C17 C15 -177.0(2) . . . . ?
C17 N8 C18 C16 0.5(4) . . . . ?
Fe1 N8 C18 C16 -177.82(18) . . . . ?
C17 N8 C18 N11 -179.5(2) . . . . ?
Fe1 N8 C18 N11 2.1(3) . . . . ?
C14 C16 C18 N8 -1.8(4) . . . . ?
C14 C16 C18 N11 178.3(2) . . . . ?
C22 N11 C18 N8 -173.3(2) . . . . ?
N12 N11 C18 N8 0.9(3) . . . . ?
C22 N11 C18 C16 6.6(4) . . . . ?
N12 N11 C18 C16 -179.2(2) . . . . ?
N10 N9 C19 C20 0.1(3) . . . . ?
C17 N9 C19 C20 179.2(2) . . . . ?
N9 C19 C20 C21 0.2(3) . . . . ?
N9 N10 C21 C20 0.5(3) . . . . ?
Fe1 N10 C21 C20 -173.7(2) . . . . ?
C19 C20 C21 N10 -0.4(3) . . . . ?
N12 N11 C22 C23 0.6(3) . . . . ?
C18 N11 C22 C23 175.0(2) . . . . ?
N11 C22 C23 C24 0.1(3) . . . . ?
N11 N12 C24 C23 1.0(3) . . . . ?
Fe1 N12 C24 C23 -168.8(2) . . . . ?
C22 C23 C24 N12 -0.7(3) . . . . ?

#==============================================================================
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1A F3 . . 7_555 2.874(3) 0.86(3) 2.04(3) 165(3) no
N1 H1B F2 . . 1_565 3.013(3) 0.90(3) 2.12(3) 172(3) no
N7 H7A F7 . . . 2.924(3) 0.93(3) 2.03(3) 161(3) no
N7 H7B F5 . . 2_554 2.927(3) 0.79(4) 2.17(4) 162(4) no

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.



#==============================================================================
#     End of CIF
#==============================================================================
_chemical_name_systematic        
'Iron(II) bis(2,6-bis(pyrazol-1-yl)pyridine-4-carbothioamide) tetrafluorobroate'
####################################################################### 
# 
# 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_cambpp-02b
_database_code_depnum_ccdc_archive 'CCDC 1860683'
_audit_update_record             
;
2018-09-07 deposited with the CCDC.
2018-11-09 downloaded from the CCDC.
;
_audit_creation_date             2018-09-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C26 H24 Fe N12 S2, 2(Cl O4)'
_chemical_formula_sum            'C26 H24 Cl2 Fe N12 O8 S2'
_chemical_formula_weight         823.44
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C26 H24 Cl2 Fe N12 O9 S'
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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   8.2808(2)
_cell_length_b                   10.2621(3)
_cell_length_c                   20.5898(5)
_cell_angle_alpha                81.158(2)
_cell_angle_beta                 86.276(2)
_cell_angle_gamma                89.446(2)
_cell_volume                     1725.24(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11677
_cell_measurement_temperature    369.99(10)
_cell_measurement_theta_max      77.3220
_cell_measurement_theta_min      4.2960
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    6.640
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.418
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.3a (Rigaku Oxford Diffraction, 2018)
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_absorpt_special_details   ?
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             840
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 -13 0.0317
0 1 13 0.0427
-5 -2 -5 0.0988
5 2 5 0.0988
0 -7 -4 0.0277
0 7 4 0.0277
0 -7 0 0.0291

_exptl_crystal_size_max          0.249
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.055
loop_
_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
0.0056 -1.0193 -12.9945 -0.2691 -0.8839 -0.3096
-0.0056 1.0193 12.9945 0.2691 0.8839 0.3096
-4.9966 -1.9825 -4.9854 -0.0261 0.0165 -1.0102
4.9966 1.9825 4.9854 0.0261 -0.0165 1.0102
-0.0064 -6.9860 -3.9473 -1.0076 0.0851 -0.3102
0.0064 6.9860 3.9473 1.0076 -0.0851 0.3102
-0.0085 -6.9792 0.0533 -0.9673 0.3734 -0.2248

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18366
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         4.566
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      369.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -12.00  55.00   0.50    4.00    --   49.80 -19.00 -60.00  134
  2  ω     38.00 109.00   0.50   16.25    --  105.75 -99.00 -60.00  142
  3  ω     74.00 101.00   0.50   16.25    --  105.75 -99.00   0.00   54
  4  ω     70.00 102.00   0.50   16.25    --  105.75 -19.00  90.00   64
  5  ω     55.00 109.00   0.50   16.25    --  105.75 -99.00  90.00  108
  6  ω     71.00 108.00   0.50   16.25    --  105.75 -99.00 150.00   74
  7  ω     34.00  68.00   0.50   16.25    --  105.75 -99.00 150.00   68
  8  ω     34.00  59.00   0.50   16.25    --  105.75 -37.00 120.00   50
  9  ω     35.00  67.00   0.50   16.25    --  105.75 -19.00  90.00   64
 10  ω     34.00  82.00   0.50   16.25    --  105.75 -57.00  60.00   96
 11  ω     34.00  59.00   0.50   16.25    --  105.75 -99.00   0.00   50
 12  ω     41.00  85.00   0.50   16.25    --  105.75 -57.00 -30.00   88
 13  ω     65.00 102.00   0.50   16.25    --  105.75   0.00 -90.00   74
 14  ω    104.00 147.00   0.50   16.25    --  105.75  19.00 -90.00   86
 15  ω     81.00 107.00   0.50   16.25    --  105.75 -77.00-150.00   52
 16  ω     66.00 112.00   0.50   16.25    --  105.75   0.00-180.00   92
 17  ω     49.00  86.00   0.50   16.25    --  105.75 -57.00-150.00   74
 18  ω     34.00  59.00   0.50   16.25    --  105.75 -37.00 -60.00   50
 19  ω     34.00  62.00   0.50   16.25    --  105.75 -37.00   0.00   56
 20  ω     37.00  62.00   0.50   16.25    --  105.75 -37.00 -30.00   50
 21  ω     35.00  60.00   0.50   16.25    --  105.75 -37.00 -90.00   50
 22  ω     34.00  62.00   0.50   16.25    --  105.75 -37.00-180.00   56
 23  ω     38.00  72.00   0.50   16.25    --  105.75 -57.00-180.00   68
 24  ω    124.00 175.00   0.50   16.25    --  105.75 125.00-180.00  102
 25  ω    -47.00  19.00   0.50    4.00    --  -49.80  37.00-180.00  132
 26  ω    -53.00 -19.00   0.50   16.25    --  -84.25  77.00-120.00   68
 27  ω    -88.00 -12.00   0.50   16.25    --  -84.25  19.00   0.00  152
 28  ω    -65.00  20.00   0.50    4.00    --  -49.80  77.00  30.00  170
 29  ω    -97.00 -46.00   0.50    4.00    --  -49.80   0.00  30.00  102
 30  ω   -109.00 -79.00   0.50   16.25    --  -84.25 -19.00  30.00   60
 31  ω   -128.00 -97.00   0.50   16.25    --  -84.25   0.00 120.00   62
 32  ω   -153.00-113.00   0.50   16.25    --  -84.25 -19.00  30.00   80
 33  ω   -118.00 -85.00   0.50    4.00    --  -49.80-125.00 120.00   66
 34  ω   -104.00 -79.00   0.50    4.00    --  -49.80-125.00  60.00   50
 35  ω   -112.00 -87.00   0.50    4.00    --  -49.80-125.00  30.00   50
 36  ω    -97.00 -62.00   0.50   16.25    --  -84.25  77.00-120.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0596044000
_diffrn_orient_matrix_UB_12      0.1387440000
_diffrn_orient_matrix_UB_13      0.0097974000
_diffrn_orient_matrix_UB_21      -0.0543072000
_diffrn_orient_matrix_UB_22      -0.0528886000
_diffrn_orient_matrix_UB_23      0.0721426000
_diffrn_orient_matrix_UB_31      0.1680933000
_diffrn_orient_matrix_UB_32      0.0321645000
_diffrn_orient_matrix_UB_33      0.0213763000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5401
_reflns_number_total             6085
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.3a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.3a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.3a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.0008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         6085
_refine_ls_number_restraints     58
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0468
_refine_ls_restrained_S_all      1.115
_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)+(0.0856P)²+0.6531P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1401
_refine_ls_wR_factor_ref         0.1439
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-H1
 0.86 with sigma of 0.01
 Cl2-O11 \\sim Cl2-O10 \\sim Cl2-O6 \\sim Cl2-O7 \\sim Cl2-O8 \\sim Cl2-O5
\\sim Cl2-O9
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
O11 \\sim O6 \\sim O7 \\sim O8 \\sim O9 \\sim O10: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O8(0.5) O6(0.5) O10(0.5) O11(0.5) O9(0.5) O7(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 N7(H7), C4(H4), C17(H17), C18(H18), C5(H5), C8(H8), C10(H10), C9(H9),
 C24(H24), C26(H26), C11(H11), C23(H23), C12(H12), C22(H22), C21(H21), C13(H13),
  C25(H25)
5.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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 0.40579(5) 0.50267(4) 0.25946(2) 0.05533(17) Uani 1 1 d . . . . .
Cl1 Cl -0.23768(11) 0.10103(9) 0.46247(4) 0.0739(2) Uani 1 1 d . . . . .
Cl2 Cl 0.63255(12) 1.03582(10) 0.10735(5) 0.0854(3) Uani 1 1 d D . . . .
S2 S 0.81964(12) 0.58604(9) -0.07093(4) 0.0764(3) Uani 1 1 d . . . . .
S1 S 0.13669(19) 0.47298(11) 0.60912(5) 0.1065(4) Uani 1 1 d . . . . .
N8 N 0.5122(3) 0.5534(2) 0.16336(11) 0.0511(5) Uani 1 1 d . . . . .
N2 N 0.3329(3) 0.4527(2) 0.36031(11) 0.0542(5) Uani 1 1 d . . . . .
N3 N 0.2579(3) 0.2555(2) 0.33384(11) 0.0573(6) Uani 1 1 d . . . . .
N9 N 0.7221(3) 0.4229(2) 0.19974(11) 0.0572(6) Uani 1 1 d . . . . .
N11 N 0.2839(3) 0.6718(2) 0.14066(12) 0.0549(5) Uani 1 1 d . . . . .
N12 N 0.2247(3) 0.6135(3) 0.20130(13) 0.0619(6) Uani 1 1 d . . . . .
N5 N 0.4235(3) 0.6558(2) 0.37174(12) 0.0599(6) Uani 1 1 d . . . . .
N10 N 0.6362(3) 0.4057(3) 0.25927(11) 0.0619(6) Uani 1 1 d . . . . .
N4 N 0.2983(3) 0.3096(3) 0.27013(12) 0.0627(6) Uani 1 1 d . . . . .
N6 N 0.4614(3) 0.6700(3) 0.30565(13) 0.0671(7) Uani 1 1 d . . . . .
C20 C 0.4408(3) 0.6373(3) 0.11838(13) 0.0504(6) Uani 1 1 d . . . . .
C19 C 0.6599(3) 0.5083(3) 0.14792(13) 0.0525(6) Uani 1 1 d . . . . .
N7 N 0.7871(4) 0.8167(3) -0.02910(14) 0.0730(7) Uani 1 1 d . . . . .
H7 H 0.7462 0.8610 0.0002 0.088 Uiso 1 1 calc R . . . .
C16 C 0.6665(3) 0.6384(3) 0.04288(13) 0.0526(6) Uani 1 1 d . . . . .
C6 C 0.2631(3) 0.3372(3) 0.38258(14) 0.0537(6) Uani 1 1 d . . . . .
C7 C 0.3473(4) 0.5381(3) 0.40248(15) 0.0568(7) Uani 1 1 d . . . . .
C4 C 0.2025(4) 0.3016(3) 0.44667(14) 0.0597(7) Uani 1 1 d . . . . .
H4 H 0.1531 0.2201 0.4605 0.072 Uiso 1 1 calc R . . . .
C15 C 0.7590(3) 0.6894(3) -0.02034(13) 0.0548(6) Uani 1 1 d . . . . .
C3 C 0.2176(4) 0.3916(3) 0.49005(14) 0.0571(7) Uani 1 1 d . . . . .
C2 C 0.1479(4) 0.3612(3) 0.56026(14) 0.0591(7) Uani 1 1 d . . . . .
C17 C 0.7402(3) 0.5456(3) 0.08761(14) 0.0572(7) Uani 1 1 d . . . . .
H17 H 0.8404 0.5098 0.0771 0.069 Uiso 1 1 calc R . . . .
C18 C 0.5128(4) 0.6857(3) 0.05769(14) 0.0564(7) Uani 1 1 d . . . . .
H18 H 0.4614 0.7471 0.0279 0.068 Uiso 1 1 calc R . . . .
O1 O -0.3694(4) 0.1880(4) 0.45049(16) 0.1177(12) Uani 1 1 d . . . . .
C5 C 0.2923(4) 0.5127(3) 0.46759(15) 0.0592(7) Uani 1 1 d . . . . .
H5 H 0.3046 0.5742 0.4957 0.071 Uiso 1 1 calc R . . . .
N1 N 0.0984(6) 0.2420(4) 0.57946(16) 0.1054(13) Uani 1 1 d D . . . .
H1 H 0.139(5) 0.179(3) 0.561(2) 0.097(14) Uiso 1 1 d D . . . .
C8 C 0.2351(5) 0.1239(3) 0.33909(17) 0.0697(8) Uani 1 1 d . . . . .
H8 H 0.2076 0.0659 0.3775 0.084 Uiso 1 1 calc R . . . .
C10 C 0.2990(5) 0.2089(4) 0.23689(17) 0.0720(9) Uani 1 1 d . . . . .
H10 H 0.3229 0.2156 0.1917 0.086 Uiso 1 1 calc R . . . .
C9 C 0.2598(5) 0.0930(4) 0.27793(18) 0.0772(9) Uani 1 1 d . . . . .
H9 H 0.2520 0.0098 0.2658 0.093 Uiso 1 1 calc R . . . .
C24 C 0.1714(4) 0.7490(4) 0.10921(19) 0.0739(9) Uani 1 1 d . . . . .
H24 H 0.1840 0.7969 0.0670 0.089 Uiso 1 1 calc R . . . .
C26 C 0.0741(4) 0.6596(4) 0.2067(2) 0.0749(9) Uani 1 1 d . . . . .
H26 H 0.0029 0.6379 0.2435 0.090 Uiso 1 1 calc R . . . .
C11 C 0.4690(5) 0.7629(3) 0.3972(2) 0.0738(9) Uani 1 1 d . . . . .
H11 H 0.4560 0.7748 0.4411 0.089 Uiso 1 1 calc R . . . .
C23 C 0.7181(4) 0.3172(4) 0.29735(16) 0.0720(9) Uani 1 1 d . . . . .
H23 H 0.6878 0.2858 0.3412 0.086 Uiso 1 1 calc R . . . .
C12 C 0.5370(5) 0.8494(4) 0.3467(2) 0.0852(11) Uani 1 1 d . . . . .
H12 H 0.5794 0.9321 0.3488 0.102 Uiso 1 1 calc R . . . .
C22 C 0.8547(5) 0.2772(4) 0.26371(19) 0.0840(11) Uani 1 1 d . . . . .
H22 H 0.9310 0.2158 0.2801 0.101 Uiso 1 1 calc R . . . .
C21 C 0.8552(4) 0.3454(4) 0.20216(18) 0.0776(10) Uani 1 1 d . . . . .
H21 H 0.9326 0.3400 0.1679 0.093 Uiso 1 1 calc R . . . .
C13 C 0.5299(5) 0.7888(4) 0.2916(2) 0.0831(10) Uani 1 1 d . . . . .
H13 H 0.5685 0.8265 0.2495 0.100 Uiso 1 1 calc R . . . .
O4 O -0.1223(5) 0.1124(5) 0.4095(2) 0.158(2) Uani 1 1 d . . . . .
C25 C 0.0372(4) 0.7437(4) 0.1504(2) 0.0824(10) Uani 1 1 d . . . . .
H25 H -0.0600 0.7876 0.1425 0.099 Uiso 1 1 calc R . . . .
C14 C 0.8828(6) 0.8887(4) -0.0851(2) 0.0981(14) Uani 1 1 d . . . . .
H14A H 0.8119 0.9295 -0.1173 0.147 Uiso 1 1 calc GR . . . .
H14B H 0.9538 0.8286 -0.1044 0.147 Uiso 1 1 calc GR . . . .
H14C H 0.9458 0.9553 -0.0704 0.147 Uiso 1 1 calc GR . . . .
O3 O -0.2907(7) -0.0270(4) 0.4802(3) 0.178(2) Uani 1 1 d . . . . .
O2 O -0.1677(6) 0.1277(7) 0.5193(3) 0.188(2) Uani 1 1 d . . . . .
C1 C 0.0238(7) 0.1921(5) 0.6443(2) 0.1124(18) Uani 1 1 d . . . . .
H1A H 0.0008 0.0998 0.6470 0.169 Uiso 1 1 calc GR . . . .
H1B H -0.0751 0.2390 0.6514 0.169 Uiso 1 1 calc GR . . . .
H1C H 0.0964 0.2045 0.6773 0.169 Uiso 1 1 calc GR . . . .
O5 O 0.4813(5) 0.9796(7) 0.1232(4) 0.209(3) Uani 1 1 d D . . . .
O8 O 0.664(2) 1.0522(15) 0.0398(2) 0.183(5) Uani 0.5 1 d D U P A 1
O6 O 0.616(3) 1.1594(7) 0.1249(7) 0.180(5) Uani 0.5 1 d D U P A 1
O10 O 0.7182(15) 0.9232(10) 0.1269(7) 0.187(4) Uani 0.5 1 d D U P A 1
O11 O 0.7346(11) 1.0143(11) 0.1589(4) 0.144(3) Uani 0.5 1 d D U P A 2
O9 O 0.7282(16) 1.0115(15) 0.0529(5) 0.169(4) Uani 0.5 1 d D U P A 2
O7 O 0.608(3) 1.1697(6) 0.0934(6) 0.187(5) Uani 0.5 1 d D U P A 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 N8 2.104(2) . ?
Fe1 N2 2.111(2) . ?
Fe1 N12 2.181(3) . ?
Fe1 N10 2.144(3) . ?
Fe1 N4 2.155(3) . ?
Fe1 N6 2.153(3) . ?
Cl1 O1 1.412(3) . ?
Cl1 O4 1.394(4) . ?
Cl1 O3 1.377(4) . ?
Cl1 O2 1.403(5) . ?
Cl2 O5 1.383(4) . ?
Cl2 O8 1.382(4) . ?
Cl2 O6 1.374(4) . ?
Cl2 O10 1.371(4) . ?
Cl2 O11 1.388(4) . ?
Cl2 O9 1.382(4) . ?
Cl2 O7 1.375(4) . ?
S2 C15 1.651(3) . ?
S1 C2 1.636(3) . ?
N8 C20 1.329(3) . ?
N8 C19 1.339(3) . ?
N2 C6 1.327(4) . ?
N2 C7 1.336(4) . ?
N3 N4 1.365(3) . ?
N3 C6 1.406(4) . ?
N3 C8 1.352(4) . ?
N9 N10 1.364(3) . ?
N9 C19 1.395(4) . ?
N9 C21 1.352(4) . ?
N11 N12 1.361(3) . ?
N11 C20 1.410(3) . ?
N11 C24 1.350(4) . ?
N12 C26 1.333(4) . ?
N5 N6 1.362(4) . ?
N5 C7 1.409(4) . ?
N5 C11 1.355(4) . ?
N10 C23 1.318(4) . ?
N4 C10 1.324(4) . ?
N6 C13 1.333(5) . ?
C20 C18 1.372(4) . ?
C19 C17 1.372(4) . ?
N7 H7 0.8600 . ?
N7 C15 1.312(4) . ?
N7 C14 1.461(4) . ?
C16 C15 1.491(4) . ?
C16 C17 1.386(4) . ?
C16 C18 1.389(4) . ?
C6 C4 1.377(4) . ?
C7 C5 1.374(4) . ?
C4 H4 0.9300 . ?
C4 C3 1.392(4) . ?
C3 C2 1.509(4) . ?
C3 C5 1.393(4) . ?
C2 N1 1.288(5) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C5 H5 0.9300 . ?
N1 H1 0.858(10) . ?
N1 C1 1.454(5) . ?
C8 H8 0.9300 . ?
C8 C9 1.348(5) . ?
C10 H10 0.9300 . ?
C10 C9 1.377(5) . ?
C9 H9 0.9300 . ?
C24 H24 0.9300 . ?
C24 C25 1.349(5) . ?
C26 H26 0.9300 . ?
C26 C25 1.384(6) . ?
C11 H11 0.9300 . ?
C11 C12 1.355(5) . ?
C23 H23 0.9300 . ?
C23 C22 1.380(5) . ?
C12 H12 0.9300 . ?
C12 C13 1.380(6) . ?
C22 H22 0.9300 . ?
C22 C21 1.350(5) . ?
C21 H21 0.9300 . ?
C13 H13 0.9300 . ?
C25 H25 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?

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
N8 Fe1 N2 171.82(9) . . ?
N8 Fe1 N12 73.23(9) . . ?
N8 Fe1 N10 74.19(9) . . ?
N8 Fe1 N4 109.65(9) . . ?
N8 Fe1 N6 102.96(10) . . ?
N2 Fe1 N12 113.84(9) . . ?
N2 Fe1 N10 99.07(9) . . ?
N2 Fe1 N4 74.08(9) . . ?
N2 Fe1 N6 73.35(10) . . ?
N10 Fe1 N12 146.94(9) . . ?
N10 Fe1 N4 87.02(11) . . ?
N10 Fe1 N6 100.44(11) . . ?
N4 Fe1 N12 98.73(10) . . ?
N6 Fe1 N12 92.12(11) . . ?
N6 Fe1 N4 147.34(10) . . ?
O4 Cl1 O1 112.5(2) . . ?
O4 Cl1 O2 110.3(3) . . ?
O3 Cl1 O1 110.9(3) . . ?
O3 Cl1 O4 111.5(4) . . ?
O3 Cl1 O2 103.0(4) . . ?
O2 Cl1 O1 108.1(3) . . ?
O5 Cl2 O11 113.3(6) . . ?
O8 Cl2 O5 109.3(10) . . ?
O6 Cl2 O5 104.0(10) . . ?
O6 Cl2 O8 107.3(9) . . ?
O10 Cl2 O5 95.8(7) . . ?
O10 Cl2 O8 101.2(8) . . ?
O10 Cl2 O6 137.0(11) . . ?
O9 Cl2 O5 122.2(7) . . ?
O9 Cl2 O11 104.4(8) . . ?
O7 Cl2 O5 106.5(11) . . ?
O7 Cl2 O11 107.1(9) . . ?
O7 Cl2 O9 101.9(10) . . ?
C20 N8 Fe1 121.26(17) . . ?
C20 N8 C19 118.6(2) . . ?
C19 N8 Fe1 119.98(18) . . ?
C6 N2 Fe1 120.19(19) . . ?
C6 N2 C7 118.3(2) . . ?
C7 N2 Fe1 121.40(19) . . ?
N4 N3 C6 117.9(2) . . ?
C8 N3 N4 110.9(2) . . ?
C8 N3 C6 130.7(3) . . ?
N10 N9 C19 118.2(2) . . ?
C21 N9 N10 110.4(2) . . ?
C21 N9 C19 131.3(3) . . ?
N12 N11 C20 118.3(2) . . ?
C24 N11 N12 111.3(2) . . ?
C24 N11 C20 130.2(3) . . ?
N11 N12 Fe1 113.66(17) . . ?
C26 N12 Fe1 141.4(2) . . ?
C26 N12 N11 104.3(3) . . ?
N6 N5 C7 118.1(2) . . ?
C11 N5 N6 111.4(3) . . ?
C11 N5 C7 130.5(3) . . ?
N9 N10 Fe1 114.59(17) . . ?
C23 N10 Fe1 139.5(2) . . ?
C23 N10 N9 105.1(2) . . ?
N3 N4 Fe1 114.04(18) . . ?
C10 N4 Fe1 137.8(2) . . ?
C10 N4 N3 104.7(3) . . ?
N5 N6 Fe1 115.28(19) . . ?
C13 N6 Fe1 140.8(3) . . ?
C13 N6 N5 103.9(3) . . ?
N8 C20 N11 112.2(2) . . ?
N8 C20 C18 123.7(2) . . ?
C18 C20 N11 124.2(2) . . ?
N8 C19 N9 112.8(2) . . ?
N8 C19 C17 122.6(3) . . ?
C17 C19 N9 124.6(2) . . ?
C15 N7 H7 117.7 . . ?
C15 N7 C14 124.7(3) . . ?
C14 N7 H7 117.7 . . ?
C17 C16 C15 118.1(2) . . ?
C17 C16 C18 120.7(2) . . ?
C18 C16 C15 121.1(3) . . ?
N2 C6 N3 112.8(2) . . ?
N2 C6 C4 123.4(3) . . ?
C4 C6 N3 123.7(3) . . ?
N2 C7 N5 111.7(2) . . ?
N2 C7 C5 123.3(3) . . ?
C5 C7 N5 125.0(3) . . ?
C6 C4 H4 121.1 . . ?
C6 C4 C3 117.7(3) . . ?
C3 C4 H4 121.1 . . ?
N7 C15 S2 126.2(2) . . ?
N7 C15 C16 114.2(3) . . ?
C16 C15 S2 119.5(2) . . ?
C4 C3 C2 120.5(3) . . ?
C4 C3 C5 119.5(3) . . ?
C5 C3 C2 119.9(3) . . ?
C3 C2 S1 121.9(2) . . ?
N1 C2 S1 122.1(2) . . ?
N1 C2 C3 116.0(3) . . ?
C19 C17 C16 117.5(3) . . ?
C19 C17 H17 121.2 . . ?
C16 C17 H17 121.2 . . ?
C20 C18 C16 116.7(3) . . ?
C20 C18 H18 121.6 . . ?
C16 C18 H18 121.6 . . ?
C7 C5 C3 117.7(3) . . ?
C7 C5 H5 121.1 . . ?
C3 C5 H5 121.1 . . ?
C2 N1 H1 120(3) . . ?
C2 N1 C1 125.3(3) . . ?
C1 N1 H1 111(3) . . ?
N3 C8 H8 126.6 . . ?
C9 C8 N3 106.7(3) . . ?
C9 C8 H8 126.6 . . ?
N4 C10 H10 124.4 . . ?
N4 C10 C9 111.1(3) . . ?
C9 C10 H10 124.4 . . ?
C8 C9 C10 106.5(3) . . ?
C8 C9 H9 126.7 . . ?
C10 C9 H9 126.7 . . ?
N11 C24 H24 126.4 . . ?
C25 C24 N11 107.2(3) . . ?
C25 C24 H24 126.4 . . ?
N12 C26 H26 124.3 . . ?
N12 C26 C25 111.3(3) . . ?
C25 C26 H26 124.3 . . ?
N5 C11 H11 126.4 . . ?
N5 C11 C12 107.1(3) . . ?
C12 C11 H11 126.4 . . ?
N10 C23 H23 124.4 . . ?
N10 C23 C22 111.2(3) . . ?
C22 C23 H23 124.4 . . ?
C11 C12 H12 127.3 . . ?
C11 C12 C13 105.5(3) . . ?
C13 C12 H12 127.3 . . ?
C23 C22 H22 127.0 . . ?
C21 C22 C23 106.1(3) . . ?
C21 C22 H22 127.0 . . ?
N9 C21 H21 126.4 . . ?
C22 C21 N9 107.1(3) . . ?
C22 C21 H21 126.4 . . ?
N6 C13 C12 112.1(3) . . ?
N6 C13 H13 123.9 . . ?
C12 C13 H13 123.9 . . ?
C24 C25 C26 105.9(3) . . ?
C24 C25 H25 127.1 . . ?
C26 C25 H25 127.1 . . ?
N7 C14 H14A 109.5 . . ?
N7 C14 H14B 109.5 . . ?
N7 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 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 N8 C20 N11 -7.2(3) . . . . ?
Fe1 N8 C20 C18 172.1(2) . . . . ?
Fe1 N8 C19 N9 3.7(3) . . . . ?
Fe1 N8 C19 C17 -175.2(2) . . . . ?
Fe1 N2 C6 N3 4.6(3) . . . . ?
Fe1 N2 C6 C4 -175.4(2) . . . . ?
Fe1 N2 C7 N5 -3.6(3) . . . . ?
Fe1 N2 C7 C5 175.9(2) . . . . ?
Fe1 N12 C26 C25 170.3(3) . . . . ?
Fe1 N10 C23 C22 168.9(3) . . . . ?
Fe1 N4 C10 C9 156.5(3) . . . . ?
Fe1 N6 C13 C12 -176.4(3) . . . . ?
S1 C2 N1 C1 1.9(7) . . . . ?
N8 C20 C18 C16 2.7(5) . . . . ?
N8 C19 C17 C16 3.2(5) . . . . ?
N2 C6 C4 C3 -0.8(5) . . . . ?
N2 C7 C5 C3 -0.2(5) . . . . ?
N3 N4 C10 C9 0.1(4) . . . . ?
N3 C6 C4 C3 179.2(3) . . . . ?
N3 C8 C9 C10 0.5(4) . . . . ?
N9 N10 C23 C22 0.1(4) . . . . ?
N9 C19 C17 C16 -175.6(3) . . . . ?
N11 N12 C26 C25 0.9(4) . . . . ?
N11 C20 C18 C16 -178.2(3) . . . . ?
N11 C24 C25 C26 -0.7(5) . . . . ?
N12 N11 C20 N8 -2.7(4) . . . . ?
N12 N11 C20 C18 178.0(3) . . . . ?
N12 N11 C24 C25 1.3(4) . . . . ?
N12 C26 C25 C24 -0.1(5) . . . . ?
N5 N6 C13 C12 0.3(4) . . . . ?
N5 C7 C5 C3 179.2(3) . . . . ?
N5 C11 C12 C13 -0.3(5) . . . . ?
N10 N9 C19 N8 -5.8(4) . . . . ?
N10 N9 C19 C17 173.0(3) . . . . ?
N10 N9 C21 C22 0.2(5) . . . . ?
N10 C23 C22 C21 0.1(5) . . . . ?
N4 N3 C6 N2 -10.2(4) . . . . ?
N4 N3 C6 C4 169.8(3) . . . . ?
N4 N3 C8 C9 -0.5(4) . . . . ?
N4 C10 C9 C8 -0.4(5) . . . . ?
N6 N5 C7 N2 3.9(4) . . . . ?
N6 N5 C7 C5 -175.6(3) . . . . ?
N6 N5 C11 C12 0.5(4) . . . . ?
C20 N8 C19 N9 179.0(3) . . . . ?
C20 N8 C19 C17 0.1(4) . . . . ?
C20 N11 N12 Fe1 10.5(3) . . . . ?
C20 N11 N12 C26 -176.7(3) . . . . ?
C20 N11 C24 C25 175.9(3) . . . . ?
C19 N8 C20 N11 177.6(2) . . . . ?
C19 N8 C20 C18 -3.2(4) . . . . ?
C19 N9 N10 Fe1 5.3(4) . . . . ?
C19 N9 N10 C23 177.3(3) . . . . ?
C19 N9 C21 C22 -176.8(4) . . . . ?
C6 N2 C7 N5 180.0(2) . . . . ?
C6 N2 C7 C5 -0.5(4) . . . . ?
C6 N3 N4 Fe1 10.9(3) . . . . ?
C6 N3 N4 C10 173.7(3) . . . . ?
C6 N3 C8 C9 -172.9(3) . . . . ?
C6 C4 C3 C2 177.5(3) . . . . ?
C6 C4 C3 C5 0.0(4) . . . . ?
C7 N2 C6 N3 -178.9(2) . . . . ?
C7 N2 C6 C4 1.1(4) . . . . ?
C7 N5 N6 Fe1 -2.5(3) . . . . ?
C7 N5 N6 C13 179.8(3) . . . . ?
C7 N5 C11 C12 -179.8(3) . . . . ?
C4 C3 C2 S1 -169.8(3) . . . . ?
C4 C3 C2 N1 10.5(5) . . . . ?
C4 C3 C5 C7 0.5(4) . . . . ?
C15 C16 C17 C19 174.2(3) . . . . ?
C15 C16 C18 C20 -176.9(3) . . . . ?
C3 C2 N1 C1 -178.4(5) . . . . ?
C2 C3 C5 C7 -177.1(3) . . . . ?
C17 C16 C15 S2 60.3(4) . . . . ?
C17 C16 C15 N7 -118.3(3) . . . . ?
C17 C16 C18 C20 0.9(5) . . . . ?
C18 C16 C15 S2 -121.9(3) . . . . ?
C18 C16 C15 N7 59.5(4) . . . . ?
C18 C16 C17 C19 -3.6(5) . . . . ?
C5 C3 C2 S1 7.7(4) . . . . ?
C5 C3 C2 N1 -172.0(4) . . . . ?
C8 N3 N4 Fe1 -162.6(2) . . . . ?
C8 N3 N4 C10 0.2(4) . . . . ?
C8 N3 C6 N2 161.8(3) . . . . ?
C8 N3 C6 C4 -18.2(5) . . . . ?
C24 N11 N12 Fe1 -174.2(2) . . . . ?
C24 N11 N12 C26 -1.4(4) . . . . ?
C24 N11 C20 N8 -177.0(3) . . . . ?
C24 N11 C20 C18 3.8(5) . . . . ?
C11 N5 N6 Fe1 177.2(2) . . . . ?
C11 N5 N6 C13 -0.4(4) . . . . ?
C11 N5 C7 N2 -175.8(3) . . . . ?
C11 N5 C7 C5 4.7(5) . . . . ?
C11 C12 C13 N6 0.0(5) . . . . ?
C23 C22 C21 N9 -0.2(5) . . . . ?
C21 N9 N10 Fe1 -172.3(3) . . . . ?
C21 N9 N10 C23 -0.2(4) . . . . ?
C21 N9 C19 N8 171.1(3) . . . . ?
C21 N9 C19 C17 -10.1(6) . . . . ?
C14 N7 C15 S2 -2.1(5) . . . . ?
C14 N7 C15 C16 176.3(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.331
_oxdiff_exptl_absorpt_empirical_full_min 0.713
####################################################################### 
# 
# 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_M171106B
_database_code_depnum_ccdc_archive 'CCDC 1860681'
_audit_update_record             
;
2018-09-05 deposited with the CCDC.
2018-11-09 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C26 H24 Cl2 Fe N12 O8 S2'
_chemical_formula_moiety         '2(C13 H12 N6 S) Fe, 2(Cl O4)'
_chemical_formula_weight         823.42
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_space_group_IT_number           2
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,-Y,-Z
#------------------------------------------------------------------------------
_cell_length_a                   8.2973(4)
_cell_length_b                   9.7480(4)
_cell_length_c                   20.6211(9)
_cell_angle_alpha                81.087(7)
_cell_angle_beta                 83.793(7)
_cell_angle_gamma                90.517(6)
_cell_volume                     1637.52(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11600
_cell_measurement_theta_min      2.01
_cell_measurement_theta_max      27.46
_cell_measurement_temperature    102
#------------------------------------------------------------------------------
_exptl_crystal_description       needle
_exptl_crystal_colour            dark
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.060
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             840.00
_exptl_absorpt_coefficient_mu    0.820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.551
_exptl_absorpt_correction_T_max  0.952

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      102
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            15925
_diffrn_reflns_av_unetI/netI     0.0760
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_theta_max         27.458
_diffrn_reflns_theta_min         2.012
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             7476
_reflns_number_gt                5745
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
    Two reflections, -2 -1 1 and -2 0 1, have been omitted from the least 
square calculations because of large differences between each Fo and Fc, which 
probably caused by a measurement error of the IP system. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0564
_refine_ls_wR_factor_ref         0.1410
_refine_ls_wR_factor_gt          0.1310
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         7476
_refine_ls_number_parameters     460
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0573P)²+3.4308P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.87
_refine_diff_density_min         -0.51
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Fe Fe 0.3463 0.8444
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.57313(6) 0.50188(5) 0.24024(2) 0.01518(13) Uani 1 1 d . . . . .
Cl1 Cl 0.24237(11) 0.88854(8) 0.02421(4) 0.02046(19) Uani 1 1 d . . . . .
Cl2 Cl 0.35896(11) 0.95393(9) 0.40120(4) 0.0237(2) Uani 1 1 d . . . . .
S1 S 0.89003(12) 0.51041(9) -0.09614(4) 0.0226(2) Uani 1 1 d . . . . .
S2 S 0.18132(12) 0.42245(9) 0.57062(4) 0.0225(2) Uani 1 1 d . . . . .
O1 O 0.1643(4) 0.8608(4) -0.03142(14) 0.0418(8) Uani 1 1 d . . . . .
O2 O 0.3101(4) 1.0270(3) 0.00999(18) 0.0426(8) Uani 1 1 d . . . . .
O3 O 0.3703(3) 0.7918(2) 0.03528(12) 0.0216(5) Uani 1 1 d . . . . .
O4 O 0.1242(3) 0.8765(3) 0.08148(13) 0.0289(6) Uani 1 1 d . . . . .
O5 O 0.5267(4) 0.9960(4) 0.38444(17) 0.0426(8) Uani 1 1 d . . . . .
O6 O 0.2612(4) 1.0684(4) 0.37812(18) 0.0513(10) Uani 1 1 d . . . . .
O7 O 0.3252(5) 0.8362(4) 0.3730(2) 0.0694(13) Uani 1 1 d . . . . .
O8 O 0.3202(5) 0.9269(4) 0.47175(15) 0.0515(9) Uani 1 1 d . . . . .
N1 N 0.8625(4) 0.7716(3) -0.07757(14) 0.0202(6) Uani 1 1 d . . . . .
H1 H 0.825351 0.833399 -0.053169 0.024 Uiso 1 1 calc R U . . .
N2 N 0.6537(3) 0.5442(3) 0.14951(13) 0.0157(6) Uani 1 1 d . . . . .
N3 N 0.7323(4) 0.7488(3) 0.17564(13) 0.0172(6) Uani 1 1 d . . . . .
N4 N 0.6720(4) 0.6880(3) 0.23887(14) 0.0185(6) Uani 1 1 d . . . . .
N5 N 0.5486(4) 0.3340(3) 0.14219(14) 0.0178(6) Uani 1 1 d . . . . .
N6 N 0.5034(4) 0.3316(3) 0.20904(14) 0.0186(6) Uani 1 1 d . . . . .
N7 N 0.2000(4) 0.1774(3) 0.52919(15) 0.0239(7) Uani 1 1 d . . . . .
H7 H 0.239918 0.128598 0.498981 0.029 Uiso 1 1 calc R U . . .
N8 N 0.4774(3) 0.4541(3) 0.32903(13) 0.0159(6) Uani 1 1 d . . . . .
N9 N 0.7057(4) 0.3376(3) 0.34497(14) 0.0178(6) Uani 1 1 d . . . . .
N10 N 0.7536(4) 0.4001(3) 0.28063(14) 0.0178(6) Uani 1 1 d . . . . .
N11 N 0.2688(4) 0.5794(3) 0.29296(14) 0.0176(6) Uani 1 1 d . . . . .
N12 N 0.3640(4) 0.5929(3) 0.23334(14) 0.0183(6) Uani 1 1 d . . . . .
C1 C 0.9444(5) 0.8204(4) -0.14313(18) 0.0251(8) Uani 1 1 d . . . . .
H1A H 0.946764 0.922178 -0.151449 0.030 Uiso 1 1 calc R U . . .
H1B H 1.055615 0.787047 -0.145994 0.030 Uiso 1 1 calc R U . . .
H1C H 0.886010 0.784846 -0.176172 0.030 Uiso 1 1 calc R U . . .
C2 C 0.8415(4) 0.6380(3) -0.05299(16) 0.0167(7) Uani 1 1 d . . . . .
C3 C 0.7697(4) 0.6071(3) 0.01770(16) 0.0167(7) Uani 1 1 d . . . . .
C4 C 0.7932(4) 0.7017(3) 0.06063(16) 0.0176(7) Uani 1 1 d . . . . .
H4 H 0.850627 0.787392 0.045561 0.021 Uiso 1 1 calc R U . . .
C5 C 0.6859(4) 0.4806(3) 0.04138(16) 0.0171(7) Uani 1 1 d . . . . .
H5 H 0.667720 0.415792 0.012806 0.020 Uiso 1 1 calc R U . . .
C6 C 0.7292(4) 0.6653(3) 0.12589(16) 0.0158(6) Uani 1 1 d . . . . .
C7 C 0.6308(4) 0.4539(3) 0.10804(16) 0.0161(7) Uani 1 1 d . . . . .
C8 C 0.7717(4) 0.8859(3) 0.17313(17) 0.0193(7) Uani 1 1 d . . . . .
H8 H 0.813432 0.949218 0.135142 0.023 Uiso 1 1 calc R U . . .
C9 C 0.7392(5) 0.9141(4) 0.23590(18) 0.0228(8) Uani 1 1 d . . . . .
H9 H 0.755758 1.000406 0.250470 0.027 Uiso 1 1 calc R U . . .
C10 C 0.6762(4) 0.7894(4) 0.27492(17) 0.0211(7) Uani 1 1 d . . . . .
H10 H 0.641453 0.779372 0.320878 0.025 Uiso 1 1 calc R U . . .
C11 C 0.5050(4) 0.2123(4) 0.12364(18) 0.0207(7) Uani 1 1 d . . . . .
H11 H 0.521756 0.189128 0.080372 0.025 Uiso 1 1 calc R U . . .
C12 C 0.4323(5) 0.1292(4) 0.17886(18) 0.0231(8) Uani 1 1 d . . . . .
H12 H 0.388786 0.037761 0.181634 0.028 Uiso 1 1 calc R U . . .
C13 C 0.4354(4) 0.2074(4) 0.23070(18) 0.0207(7) Uani 1 1 d . . . . .
H13 H 0.394211 0.175152 0.275315 0.025 Uiso 1 1 calc R U . . .
C14 C 0.1009(5) 0.1034(4) 0.5871(2) 0.0294(9) Uani 1 1 d . . . . .
H14A H 0.093260 0.004577 0.583347 0.035 Uiso 1 1 calc R U . . .
H14B H 0.150854 0.114136 0.627002 0.035 Uiso 1 1 calc R U . . .
H14C H -0.007982 0.141715 0.589736 0.035 Uiso 1 1 calc R U . . .
C15 C 0.2341(4) 0.3111(3) 0.51881(16) 0.0174(7) Uani 1 1 d . . . . .
C16 C 0.3252(4) 0.3642(3) 0.45292(16) 0.0168(7) Uani 1 1 d . . . . .
C17 C 0.4799(4) 0.3165(3) 0.43570(16) 0.0172(7) Uani 1 1 d . . . . .
H17 H 0.532796 0.252526 0.465439 0.021 Uiso 1 1 calc R U . . .
C18 C 0.2472(4) 0.4580(4) 0.40877(17) 0.0198(7) Uani 1 1 d . . . . .
H18 H 0.143882 0.493140 0.421133 0.024 Uiso 1 1 calc R U . . .
C19 C 0.5517(4) 0.3682(3) 0.37250(16) 0.0159(6) Uani 1 1 d . . . . .
C20 C 0.3279(4) 0.4967(3) 0.34662(16) 0.0174(7) Uani 1 1 d . . . . .
C21 C 0.8295(4) 0.2650(4) 0.37132(18) 0.0213(7) Uani 1 1 d . . . . .
H21 H 0.827058 0.215089 0.414816 0.026 Uiso 1 1 calc R U . . .
C22 C 0.9575(4) 0.2781(4) 0.32308(18) 0.0229(8) Uani 1 1 d . . . . .
H22 H 1.060798 0.237927 0.326113 0.027 Uiso 1 1 calc R U . . .
C23 C 0.9055(4) 0.3636(4) 0.26752(18) 0.0203(7) Uani 1 1 d . . . . .
H23 H 0.970494 0.390841 0.226621 0.024 Uiso 1 1 calc R U . . .
C24 C 0.1329(4) 0.6557(4) 0.28800(18) 0.0213(7) Uani 1 1 d . . . . .
H24 H 0.049258 0.663575 0.322428 0.026 Uiso 1 1 calc R U . . .
C25 C 0.1404(4) 0.7188(4) 0.22381(18) 0.0225(8) Uani 1 1 d . . . . .
H25 H 0.062730 0.778715 0.204702 0.027 Uiso 1 1 calc R U . . .
C26 C 0.2853(4) 0.6776(4) 0.19160(17) 0.0199(7) Uani 1 1 d . . . . .
H26 H 0.322058 0.706404 0.146223 0.024 Uiso 1 1 calc R U . . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_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 1.898(3) . ?
Fe1 N8 1.901(3) . ?
Fe1 N12 1.964(3) . ?
Fe1 N6 1.975(3) . ?
Fe1 N4 1.979(3) . ?
Fe1 N10 1.990(3) . ?
Cl1 O2 1.432(3) . ?
Cl1 O1 1.436(3) . ?
Cl1 O3 1.440(2) . ?
Cl1 O4 1.440(3) . ?
Cl2 O7 1.403(3) . ?
Cl2 O6 1.437(3) . ?
Cl2 O5 1.438(3) . ?
Cl2 O8 1.438(3) . ?
S1 C2 1.666(3) . ?
S2 C15 1.667(4) . ?
N1 C2 1.325(4) . ?
N1 C1 1.453(5) . ?
N1 H1 0.8800 . ?
N2 C6 1.329(4) . ?
N2 C7 1.344(4) . ?
N3 C8 1.365(4) . ?
N3 N4 1.384(4) . ?
N3 C6 1.407(4) . ?
N4 C10 1.328(5) . ?
N5 C11 1.360(4) . ?
N5 N6 1.386(4) . ?
N5 C7 1.398(4) . ?
N6 C13 1.322(4) . ?
N7 C15 1.310(5) . ?
N7 C14 1.460(5) . ?
N7 H7 0.8800 . ?
N8 C19 1.334(4) . ?
N8 C20 1.342(4) . ?
N9 C21 1.366(4) . ?
N9 N10 1.386(4) . ?
N9 C19 1.395(4) . ?
N10 C23 1.323(5) . ?
N11 C24 1.361(4) . ?
N11 N12 1.375(4) . ?
N11 C20 1.401(4) . ?
N12 C26 1.327(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.498(5) . ?
C3 C4 1.399(5) . ?
C3 C5 1.402(5) . ?
C4 C6 1.383(5) . ?
C4 H4 0.9500 . ?
C5 C7 1.385(5) . ?
C5 H5 0.9500 . ?
C8 C9 1.364(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.411(5) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.368(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.408(5) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.496(5) . ?
C16 C17 1.397(5) . ?
C16 C18 1.401(4) . ?
C17 C19 1.390(5) . ?
C17 H17 0.9500 . ?
C18 C20 1.376(5) . ?
C18 H18 0.9500 . ?
C21 C22 1.365(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.418(5) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 C25 1.365(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.402(5) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?

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 N8 175.52(12) . . ?
N2 Fe1 N12 96.96(12) . . ?
N8 Fe1 N12 80.22(12) . . ?
N2 Fe1 N6 79.93(12) . . ?
N8 Fe1 N6 96.78(12) . . ?
N12 Fe1 N6 94.75(12) . . ?
N2 Fe1 N4 80.21(12) . . ?
N8 Fe1 N4 103.06(12) . . ?
N12 Fe1 N4 87.63(12) . . ?
N6 Fe1 N4 160.13(12) . . ?
N2 Fe1 N10 103.28(12) . . ?
N8 Fe1 N10 79.66(12) . . ?
N12 Fe1 N10 159.71(12) . . ?
N6 Fe1 N10 90.15(12) . . ?
N4 Fe1 N10 94.41(12) . . ?
O2 Cl1 O1 108.7(2) . . ?
O2 Cl1 O3 109.27(17) . . ?
O1 Cl1 O3 109.43(17) . . ?
O2 Cl1 O4 109.51(18) . . ?
O1 Cl1 O4 109.20(19) . . ?
O3 Cl1 O4 110.70(15) . . ?
O7 Cl2 O6 111.3(3) . . ?
O7 Cl2 O5 110.2(2) . . ?
O6 Cl2 O5 108.3(2) . . ?
O7 Cl2 O8 110.7(3) . . ?
O6 Cl2 O8 105.9(2) . . ?
O5 Cl2 O8 110.3(2) . . ?
C2 N1 C1 122.7(3) . . ?
C2 N1 H1 118.6 . . ?
C1 N1 H1 118.6 . . ?
C6 N2 C7 119.2(3) . . ?
C6 N2 Fe1 120.3(2) . . ?
C7 N2 Fe1 120.5(2) . . ?
C8 N3 N4 111.5(3) . . ?
C8 N3 C6 131.9(3) . . ?
N4 N3 C6 116.4(3) . . ?
C10 N4 N3 104.7(3) . . ?
C10 N4 Fe1 141.7(3) . . ?
N3 N4 Fe1 111.9(2) . . ?
C11 N5 N6 110.4(3) . . ?
C11 N5 C7 132.9(3) . . ?
N6 N5 C7 116.6(3) . . ?
C13 N6 N5 105.5(3) . . ?
C13 N6 Fe1 141.8(3) . . ?
N5 N6 Fe1 112.5(2) . . ?
C15 N7 C14 125.0(3) . . ?
C15 N7 H7 117.5 . . ?
C14 N7 H7 117.5 . . ?
C19 N8 C20 119.6(3) . . ?
C19 N8 Fe1 120.3(2) . . ?
C20 N8 Fe1 119.8(2) . . ?
C21 N9 N10 110.8(3) . . ?
C21 N9 C19 132.0(3) . . ?
N10 N9 C19 116.9(3) . . ?
C23 N10 N9 105.6(3) . . ?
C23 N10 Fe1 142.7(2) . . ?
N9 N10 Fe1 111.6(2) . . ?
C24 N11 N12 111.1(3) . . ?
C24 N11 C20 132.0(3) . . ?
N12 N11 C20 116.8(3) . . ?
C26 N12 N11 105.4(3) . . ?
C26 N12 Fe1 141.5(3) . . ?
N11 N12 Fe1 112.58(19) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 115.4(3) . . ?
N1 C2 S1 123.6(3) . . ?
C3 C2 S1 121.0(2) . . ?
C4 C3 C5 120.2(3) . . ?
C4 C3 C2 119.8(3) . . ?
C5 C3 C2 119.9(3) . . ?
C6 C4 C3 117.3(3) . . ?
C6 C4 H4 121.4 . . ?
C3 C4 H4 121.4 . . ?
C7 C5 C3 117.4(3) . . ?
C7 C5 H5 121.3 . . ?
C3 C5 H5 121.3 . . ?
N2 C6 C4 123.2(3) . . ?
N2 C6 N3 110.9(3) . . ?
C4 C6 N3 125.9(3) . . ?
N2 C7 C5 122.6(3) . . ?
N2 C7 N5 110.4(3) . . ?
C5 C7 N5 127.0(3) . . ?
C9 C8 N3 106.5(3) . . ?
C9 C8 H8 126.8 . . ?
N3 C8 H8 126.8 . . ?
C8 C9 C10 106.3(3) . . ?
C8 C9 H9 126.8 . . ?
C10 C9 H9 126.8 . . ?
N4 C10 C9 111.0(3) . . ?
N4 C10 H10 124.5 . . ?
C9 C10 H10 124.5 . . ?
N5 C11 C12 107.3(3) . . ?
N5 C11 H11 126.3 . . ?
C12 C11 H11 126.3 . . ?
C11 C12 C13 105.8(3) . . ?
C11 C12 H12 127.1 . . ?
C13 C12 H12 127.1 . . ?
N6 C13 C12 111.0(3) . . ?
N6 C13 H13 124.5 . . ?
C12 C13 H13 124.5 . . ?
N7 C14 H14A 109.5 . . ?
N7 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N7 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N7 C15 C16 114.7(3) . . ?
N7 C15 S2 126.1(3) . . ?
C16 C15 S2 119.2(2) . . ?
C17 C16 C18 121.8(3) . . ?
C17 C16 C15 120.5(3) . . ?
C18 C16 C15 117.7(3) . . ?
C19 C17 C16 116.0(3) . . ?
C19 C17 H17 122.0 . . ?
C16 C17 H17 122.0 . . ?
C20 C18 C16 116.6(3) . . ?
C20 C18 H18 121.7 . . ?
C16 C18 H18 121.7 . . ?
N8 C19 C17 123.1(3) . . ?
N8 C19 N9 110.7(3) . . ?
C17 C19 N9 126.2(3) . . ?
N8 C20 C18 122.8(3) . . ?
N8 C20 N11 110.4(3) . . ?
C18 C20 N11 126.8(3) . . ?
C22 C21 N9 106.7(3) . . ?
C22 C21 H21 126.6 . . ?
N9 C21 H21 126.6 . . ?
C21 C22 C23 106.3(3) . . ?
C21 C22 H22 126.8 . . ?
C23 C22 H22 126.8 . . ?
N10 C23 C22 110.5(3) . . ?
N10 C23 H23 124.8 . . ?
C22 C23 H23 124.8 . . ?
N11 C24 C25 106.5(3) . . ?
N11 C24 H24 126.8 . . ?
C25 C24 H24 126.8 . . ?
C24 C25 C26 106.5(3) . . ?
C24 C25 H25 126.7 . . ?
C26 C25 H25 126.7 . . ?
N12 C26 C25 110.5(3) . . ?
N12 C26 H26 124.7 . . ?
C25 C26 H26 124.7 . . ?

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
N12 Fe1 N2 C6 85.1(3) . . . . ?
N6 Fe1 N2 C6 178.7(3) . . . . ?
N4 Fe1 N2 C6 -1.3(2) . . . . ?
N10 Fe1 N2 C6 -93.5(3) . . . . ?
N12 Fe1 N2 C7 -92.9(3) . . . . ?
N6 Fe1 N2 C7 0.7(2) . . . . ?
N4 Fe1 N2 C7 -179.3(3) . . . . ?
N10 Fe1 N2 C7 88.5(3) . . . . ?
C8 N3 N4 C10 -0.4(4) . . . . ?
C6 N3 N4 C10 -175.2(3) . . . . ?
C8 N3 N4 Fe1 168.3(2) . . . . ?
C6 N3 N4 Fe1 -6.5(3) . . . . ?
C11 N5 N6 C13 1.2(4) . . . . ?
C7 N5 N6 C13 -177.3(3) . . . . ?
C11 N5 N6 Fe1 177.1(2) . . . . ?
C7 N5 N6 Fe1 -1.3(3) . . . . ?
C21 N9 N10 C23 1.0(4) . . . . ?
C19 N9 N10 C23 175.7(3) . . . . ?
C21 N9 N10 Fe1 178.3(2) . . . . ?
C19 N9 N10 Fe1 -7.1(3) . . . . ?
C24 N11 N12 C26 -0.3(4) . . . . ?
C20 N11 N12 C26 -178.4(3) . . . . ?
C24 N11 N12 Fe1 173.5(2) . . . . ?
C20 N11 N12 Fe1 -4.6(4) . . . . ?
C1 N1 C2 C3 174.1(3) . . . . ?
C1 N1 C2 S1 -5.9(5) . . . . ?
N1 C2 C3 C4 -27.5(4) . . . . ?
S1 C2 C3 C4 152.5(3) . . . . ?
N1 C2 C3 C5 155.5(3) . . . . ?
S1 C2 C3 C5 -24.5(4) . . . . ?
C5 C3 C4 C6 -0.7(5) . . . . ?
C2 C3 C4 C6 -177.7(3) . . . . ?
C4 C3 C5 C7 -0.8(5) . . . . ?
C2 C3 C5 C7 176.1(3) . . . . ?
C7 N2 C6 C4 -3.1(5) . . . . ?
Fe1 N2 C6 C4 178.9(2) . . . . ?
C7 N2 C6 N3 176.2(3) . . . . ?
Fe1 N2 C6 N3 -1.9(4) . . . . ?
C3 C4 C6 N2 2.7(5) . . . . ?
C3 C4 C6 N3 -176.4(3) . . . . ?
C8 N3 C6 N2 -168.0(3) . . . . ?
N4 N3 C6 N2 5.5(4) . . . . ?
C8 N3 C6 C4 11.3(6) . . . . ?
N4 N3 C6 C4 -175.3(3) . . . . ?
C6 N2 C7 C5 1.4(5) . . . . ?
Fe1 N2 C7 C5 179.4(2) . . . . ?
C6 N2 C7 N5 -179.6(3) . . . . ?
Fe1 N2 C7 N5 -1.6(4) . . . . ?
C3 C5 C7 N2 0.5(5) . . . . ?
C3 C5 C7 N5 -178.3(3) . . . . ?
C11 N5 C7 N2 -176.2(3) . . . . ?
N6 N5 C7 N2 1.8(4) . . . . ?
C11 N5 C7 C5 2.8(6) . . . . ?
N6 N5 C7 C5 -179.2(3) . . . . ?
N4 N3 C8 C9 1.1(4) . . . . ?
C6 N3 C8 C9 174.8(3) . . . . ?
N3 C8 C9 C10 -1.2(4) . . . . ?
N3 N4 C10 C9 -0.4(4) . . . . ?
Fe1 N4 C10 C9 -163.4(3) . . . . ?
C8 C9 C10 N4 1.0(4) . . . . ?
N6 N5 C11 C12 -0.7(4) . . . . ?
C7 N5 C11 C12 177.4(3) . . . . ?
N5 C11 C12 C13 -0.1(4) . . . . ?
N5 N6 C13 C12 -1.2(4) . . . . ?
Fe1 N6 C13 C12 -175.2(3) . . . . ?
C11 C12 C13 N6 0.9(4) . . . . ?
C14 N7 C15 C16 -174.6(3) . . . . ?
C14 N7 C15 S2 3.7(5) . . . . ?
N7 C15 C16 C17 -62.3(4) . . . . ?
S2 C15 C16 C17 119.2(3) . . . . ?
N7 C15 C16 C18 115.0(4) . . . . ?
S2 C15 C16 C18 -63.4(4) . . . . ?
C18 C16 C17 C19 0.4(5) . . . . ?
C15 C16 C17 C19 177.6(3) . . . . ?
C17 C16 C18 C20 2.5(5) . . . . ?
C15 C16 C18 C20 -174.9(3) . . . . ?
C20 N8 C19 C17 1.8(5) . . . . ?
Fe1 N8 C19 C17 -172.2(3) . . . . ?
C20 N8 C19 N9 -179.4(3) . . . . ?
Fe1 N8 C19 N9 6.6(4) . . . . ?
C16 C17 C19 N8 -2.6(5) . . . . ?
C16 C17 C19 N9 178.8(3) . . . . ?
C21 N9 C19 N8 174.1(3) . . . . ?
N10 N9 C19 N8 0.8(4) . . . . ?
C21 N9 C19 C17 -7.1(6) . . . . ?
N10 N9 C19 C17 179.6(3) . . . . ?
C19 N8 C20 C18 1.4(5) . . . . ?
Fe1 N8 C20 C18 175.5(3) . . . . ?
C19 N8 C20 N11 -176.7(3) . . . . ?
Fe1 N8 C20 N11 -2.7(4) . . . . ?
C16 C18 C20 N8 -3.4(5) . . . . ?
C16 C18 C20 N11 174.3(3) . . . . ?
C24 N11 C20 N8 -172.9(3) . . . . ?
N12 N11 C20 N8 4.7(4) . . . . ?
C24 N11 C20 C18 9.1(6) . . . . ?
N12 N11 C20 C18 -173.3(3) . . . . ?
N10 N9 C21 C22 -1.4(4) . . . . ?
C19 N9 C21 C22 -174.9(3) . . . . ?
N9 C21 C22 C23 1.1(4) . . . . ?
N9 N10 C23 C22 -0.3(4) . . . . ?
Fe1 N10 C23 C22 -176.1(3) . . . . ?
C21 C22 C23 N10 -0.5(4) . . . . ?
N12 N11 C24 C25 0.4(4) . . . . ?
C20 N11 C24 C25 178.1(4) . . . . ?
N11 C24 C25 C26 -0.4(4) . . . . ?
N11 N12 C26 C25 0.0(4) . . . . ?
Fe1 N12 C26 C25 -170.7(3) . . . . ?
C24 C25 C26 N12 0.2(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1 O2 . . 2_675 2.883(4) 0.880 2.024 165.3 no
N7 H7 O8 . . 1_545 3.008(5) 0.880 2.216 149.6 no

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


####################################################################### 
# 
# 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_M171016B
_database_code_depnum_ccdc_archive 'CCDC 1860675'
_audit_update_record             
;
2018-08-07 deposited with the CCDC.
2018-11-09 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C13 H12 N6 S'
_chemical_formula_moiety         'C13 H12 N6 S'
_chemical_formula_weight         284.34
_chemical_melting_point          ?
_chemical_absolute_configuration unk

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
_space_group_IT_number           19
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2-X,-Y,1/2+Z
3 1/2+X,1/2-Y,-Z
4 -X,1/2+Y,1/2-Z
#------------------------------------------------------------------------------
_cell_length_a                   6.4725(2)
_cell_length_b                   13.6562(5)
_cell_length_c                   31.8638(11)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     2816.44(16)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    24162
_cell_measurement_theta_min      1.92
_cell_measurement_theta_max      27.45
_cell_measurement_temperature    290
#------------------------------------------------------------------------------
_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.300
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1184.00
_exptl_absorpt_coefficient_mu    0.229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.790
_exptl_absorpt_correction_T_max  0.934

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      290
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            27122
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_theta_max         27.455
_diffrn_reflns_theta_min         2.429
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       40
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             6444
_reflns_number_gt                5745
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.747
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    1.000

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0325
_refine_ls_wR_factor_ref         0.0884
_refine_ls_wR_factor_gt          0.0851
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_reflns         6444
_refine_ls_number_parameters     369
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0523P)²+0.3042P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.29
_refine_diff_density_min         -0.30
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
 Flack x determined using 2227 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.054(13)

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
S1 S 0.16262(11) 0.48641(5) 0.05987(2) 0.05765(18) Uani 1 1 d . . . . .
S2 S 0.24925(12) -0.17446(5) 0.07269(3) 0.0674(2) Uani 1 1 d . . . . .
N1 N -0.1594(3) 0.58376(16) 0.08882(6) 0.0475(5) Uani 1 1 d . . . . .
N2 N 0.2825(3) 0.60653(14) 0.21657(6) 0.0422(4) Uani 1 1 d . . . . .
N3 N 0.0113(3) 0.52808(15) 0.24951(6) 0.0450(4) Uani 1 1 d . . . . .
N4 N -0.1729(4) 0.4793(2) 0.24851(7) 0.0613(6) Uani 1 1 d . . . . .
N5 N 0.5606(3) 0.68918(15) 0.18811(6) 0.0450(4) Uani 1 1 d . . . . .
N6 N 0.6747(3) 0.72075(16) 0.15485(7) 0.0526(5) Uani 1 1 d . . . . .
N7 N 0.5757(3) -0.07082(16) 0.04980(7) 0.0490(5) Uani 1 1 d . . . . .
N8 N 0.1480(3) 0.20387(13) 0.10423(5) 0.0363(4) Uani 1 1 d . . . . .
N9 N 0.4289(3) 0.23437(14) 0.14671(6) 0.0410(4) Uani 1 1 d . . . . .
N10 N 0.6102(3) 0.20817(16) 0.16489(6) 0.0521(5) Uani 1 1 d . . . . .
N11 N -0.1385(3) 0.18629(13) 0.06132(5) 0.0359(4) Uani 1 1 d . . . . .
N12 N -0.2507(3) 0.13637(14) 0.03235(6) 0.0413(4) Uani 1 1 d . . . . .
C1 C -0.2737(4) 0.5721(2) 0.04993(8) 0.0580(6) Uani 1 1 d . . . . .
H1A H -0.406484 0.602895 0.052582 0.070 Uiso 1 1 calc R U . . .
H1B H -0.198452 0.602165 0.027387 0.070 Uiso 1 1 calc R U . . .
H1C H -0.291878 0.503711 0.044118 0.070 Uiso 1 1 calc R U . . .
C2 C 0.0279(4) 0.54948(17) 0.09493(6) 0.0405(5) Uani 1 1 d . . . . .
C3 C 0.1172(4) 0.56900(16) 0.13766(6) 0.0393(5) Uani 1 1 d . . . . .
C4 C 0.0151(4) 0.53712(17) 0.17328(7) 0.0418(5) Uani 1 1 d . . . . .
H4 H -0.109060 0.503098 0.171499 0.050 Uiso 1 1 calc R U . . .
C5 C 0.3037(4) 0.61899(16) 0.14147(7) 0.0412(5) Uani 1 1 d . . . . .
H5 H 0.376731 0.639998 0.118003 0.049 Uiso 1 1 calc R U . . .
C6 C 0.1058(4) 0.55802(16) 0.21195(6) 0.0407(5) Uani 1 1 d . . . . .
C7 C 0.3754(3) 0.63600(16) 0.18160(7) 0.0402(4) Uani 1 1 d . . . . .
C8 C 0.0771(5) 0.5434(2) 0.28964(7) 0.0521(6) Uani 1 1 d . . . . .
H8 H 0.197625 0.575152 0.297898 0.062 Uiso 1 1 calc R U . . .
C9 C -0.0674(5) 0.5035(2) 0.31503(8) 0.0594(7) Uani 1 1 d . . . . .
H9 H -0.066158 0.501689 0.344210 0.071 Uiso 1 1 calc R U . . .
C10 C -0.2168(5) 0.4659(2) 0.28879(9) 0.0657(8) Uani 1 1 d . . . . .
H10 H -0.335555 0.434554 0.298264 0.079 Uiso 1 1 calc R U . . .
C11 C 0.6394(4) 0.7223(2) 0.22502(8) 0.0600(7) Uani 1 1 d . . . . .
H11 H 0.587123 0.709995 0.251689 0.072 Uiso 1 1 calc R U . . .
C12 C 0.8089(4) 0.7767(2) 0.21564(9) 0.0659(8) Uani 1 1 d . . . . .
H12 H 0.895499 0.809370 0.234243 0.079 Uiso 1 1 calc R U . . .
C13 C 0.8249(4) 0.7727(2) 0.17209(9) 0.0609(7) Uani 1 1 d . . . . .
H13 H 0.929235 0.803206 0.156854 0.073 Uiso 1 1 calc R U . . .
C14 C 0.6871(5) -0.1574(2) 0.03486(12) 0.0698(8) Uani 1 1 d . . . . .
H14A H 0.819665 -0.138128 0.024159 0.084 Uiso 1 1 calc R U . . .
H14B H 0.705705 -0.202525 0.057670 0.084 Uiso 1 1 calc R U . . .
H14C H 0.609078 -0.188460 0.012960 0.084 Uiso 1 1 calc R U . . .
C15 C 0.3893(3) -0.07410(16) 0.06624(7) 0.0410(5) Uani 1 1 d . . . . .
C16 C 0.3059(3) 0.02343(15) 0.07967(6) 0.0364(4) Uani 1 1 d . . . . .
C17 C 0.4146(3) 0.08119(16) 0.10785(6) 0.0378(4) Uani 1 1 d . . . . .
H17 H 0.540516 0.061040 0.118936 0.045 Uiso 1 1 calc R U . . .
C18 C 0.1181(3) 0.05604(16) 0.06371(6) 0.0379(4) Uani 1 1 d . . . . .
H18 H 0.042284 0.018445 0.044876 0.046 Uiso 1 1 calc R U . . .
C19 C 0.3271(3) 0.17035(15) 0.11879(6) 0.0360(4) Uani 1 1 d . . . . .
C20 C 0.0487(3) 0.14693(15) 0.07705(6) 0.0336(4) Uani 1 1 d . . . . .
C21 C 0.3764(5) 0.32726(19) 0.15615(8) 0.0546(6) Uani 1 1 d . . . . .
H21 H 0.259224 0.360388 0.146980 0.066 Uiso 1 1 calc R U . . .
C22 C 0.5269(5) 0.3635(2) 0.18160(9) 0.0604(7) Uani 1 1 d . . . . .
H22 H 0.534741 0.425747 0.193372 0.072 Uiso 1 1 calc R U . . .
C23 C 0.6654(4) 0.2873(2) 0.18605(8) 0.0569(6) Uani 1 1 d . . . . .
H23 H 0.784817 0.291171 0.202209 0.068 Uiso 1 1 calc R U . . .
C24 C -0.2221(3) 0.27532(16) 0.06972(7) 0.0416(5) Uani 1 1 d . . . . .
H24 H -0.171527 0.321576 0.088521 0.050 Uiso 1 1 calc R U . . .
C25 C -0.3940(4) 0.28401(18) 0.04539(7) 0.0462(5) Uani 1 1 d . . . . .
H25 H -0.484664 0.336736 0.043968 0.055 Uiso 1 1 calc R U . . .
C26 C -0.4040(4) 0.19609(19) 0.02301(7) 0.0454(5) Uani 1 1 d . . . . .
H26 H -0.507185 0.181380 0.003710 0.054 Uiso 1 1 calc R U . . .
H1N H -0.213(5) 0.617(2) 0.1063(9) 0.051(8) Uiso 1 1 d . . . . .
H7N H 0.630(4) -0.018(2) 0.0454(9) 0.050(7) Uiso 1 1 d . . . . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_computing_structure_refinement  'SHELXL Version 2017/1 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.5 (Rigaku, 2017)'
_computing_molecular_graphics    'CrystalStructure 4.2.5'

#==============================================================================
# MOLECULAR GEOMETRY

_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
S1 C2 1.658(2) . ?
S2 C15 1.656(2) . ?
N1 C2 1.314(3) . ?
N1 C1 1.452(3) . ?
N1 H1N 0.80(3) . ?
N2 C7 1.329(3) . ?
N2 C6 1.330(3) . ?
N3 C8 1.364(3) . ?
N3 N4 1.366(3) . ?
N3 C6 1.405(3) . ?
N4 C10 1.327(3) . ?
N5 C11 1.359(3) . ?
N5 N6 1.362(3) . ?
N5 C7 1.417(3) . ?
N6 C13 1.323(3) . ?
N7 C15 1.316(3) . ?
N7 C14 1.465(3) . ?
N7 H7N 0.82(3) . ?
N8 C20 1.330(3) . ?
N8 C19 1.330(3) . ?
N9 C21 1.347(3) . ?
N9 N10 1.357(3) . ?
N9 C19 1.411(3) . ?
N10 C23 1.323(3) . ?
N11 C24 1.357(3) . ?
N11 N12 1.358(2) . ?
N11 C20 1.417(3) . ?
N12 C26 1.318(3) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.503(3) . ?
C3 C4 1.383(3) . ?
C3 C5 1.392(3) . ?
C4 C6 1.394(3) . ?
C4 H4 0.9300 . ?
C5 C7 1.380(3) . ?
C5 H5 0.9300 . ?
C8 C9 1.352(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.378(4) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.358(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.393(4) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.500(3) . ?
C16 C17 1.387(3) . ?
C16 C18 1.391(3) . ?
C17 C19 1.387(3) . ?
C17 H17 0.9300 . ?
C18 C20 1.387(3) . ?
C18 H18 0.9300 . ?
C21 C22 1.361(4) . ?
C21 H21 0.9300 . ?
C22 C23 1.381(4) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 C25 1.361(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.398(4) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?

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
C2 N1 C1 123.9(2) . . ?
C2 N1 H1N 120(2) . . ?
C1 N1 H1N 116(2) . . ?
C7 N2 C6 116.56(18) . . ?
C8 N3 N4 111.7(2) . . ?
C8 N3 C6 128.2(2) . . ?
N4 N3 C6 120.12(19) . . ?
C10 N4 N3 103.4(2) . . ?
C11 N5 N6 111.4(2) . . ?
C11 N5 C7 127.9(2) . . ?
N6 N5 C7 120.48(19) . . ?
C13 N6 N5 104.2(2) . . ?
C15 N7 C14 123.6(2) . . ?
C15 N7 H7N 119.7(19) . . ?
C14 N7 H7N 116(2) . . ?
C20 N8 C19 116.58(18) . . ?
C21 N9 N10 111.80(19) . . ?
C21 N9 C19 127.3(2) . . ?
N10 N9 C19 120.65(19) . . ?
C23 N10 N9 103.6(2) . . ?
C24 N11 N12 111.74(17) . . ?
C24 N11 C20 127.66(18) . . ?
N12 N11 C20 120.48(17) . . ?
C26 N12 N11 104.20(18) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 115.2(2) . . ?
N1 C2 S1 124.77(18) . . ?
C3 C2 S1 120.02(17) . . ?
C4 C3 C5 119.8(2) . . ?
C4 C3 C2 120.2(2) . . ?
C5 C3 C2 119.96(19) . . ?
C3 C4 C6 117.4(2) . . ?
C3 C4 H4 121.3 . . ?
C6 C4 H4 121.3 . . ?
C7 C5 C3 117.1(2) . . ?
C7 C5 H5 121.5 . . ?
C3 C5 H5 121.5 . . ?
N2 C6 C4 124.2(2) . . ?
N2 C6 N3 115.13(18) . . ?
C4 C6 N3 120.7(2) . . ?
N2 C7 C5 125.0(2) . . ?
N2 C7 N5 114.55(19) . . ?
C5 C7 N5 120.4(2) . . ?
C9 C8 N3 106.4(2) . . ?
C9 C8 H8 126.8 . . ?
N3 C8 H8 126.8 . . ?
C8 C9 C10 105.8(2) . . ?
C8 C9 H9 127.1 . . ?
C10 C9 H9 127.1 . . ?
N4 C10 C9 112.7(3) . . ?
N4 C10 H10 123.7 . . ?
C9 C10 H10 123.7 . . ?
C12 C11 N5 107.1(2) . . ?
C12 C11 H11 126.4 . . ?
N5 C11 H11 126.4 . . ?
C11 C12 C13 105.0(2) . . ?
C11 C12 H12 127.5 . . ?
C13 C12 H12 127.5 . . ?
N6 C13 C12 112.3(2) . . ?
N6 C13 H13 123.8 . . ?
C12 C13 H13 123.8 . . ?
N7 C14 H14A 109.5 . . ?
N7 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N7 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N7 C15 C16 114.4(2) . . ?
N7 C15 S2 125.41(18) . . ?
C16 C15 S2 120.17(16) . . ?
C17 C16 C18 119.86(19) . . ?
C17 C16 C15 120.50(19) . . ?
C18 C16 C15 119.64(19) . . ?
C16 C17 C19 117.06(19) . . ?
C16 C17 H17 121.5 . . ?
C19 C17 H17 121.5 . . ?
C20 C18 C16 117.25(18) . . ?
C20 C18 H18 121.4 . . ?
C16 C18 H18 121.4 . . ?
N8 C19 C17 124.77(19) . . ?
N8 C19 N9 114.45(19) . . ?
C17 C19 N9 120.78(19) . . ?
N8 C20 C18 124.48(19) . . ?
N8 C20 N11 114.95(18) . . ?
C18 C20 N11 120.56(18) . . ?
N9 C21 C22 107.2(2) . . ?
N9 C21 H21 126.4 . . ?
C22 C21 H21 126.4 . . ?
C21 C22 C23 104.6(2) . . ?
C21 C22 H22 127.7 . . ?
C23 C22 H22 127.7 . . ?
N10 C23 C22 112.8(2) . . ?
N10 C23 H23 123.6 . . ?
C22 C23 H23 123.6 . . ?
N11 C24 C25 107.0(2) . . ?
N11 C24 H24 126.5 . . ?
C25 C24 H24 126.5 . . ?
C24 C25 C26 104.7(2) . . ?
C24 C25 H25 127.7 . . ?
C26 C25 H25 127.7 . . ?
N12 C26 C25 112.4(2) . . ?
N12 C26 H26 123.8 . . ?
C25 C26 H26 123.8 . . ?

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
C8 N3 N4 C10 0.2(3) . . . . ?
C6 N3 N4 C10 -178.2(2) . . . . ?
C11 N5 N6 C13 0.5(3) . . . . ?
C7 N5 N6 C13 175.6(2) . . . . ?
C21 N9 N10 C23 0.7(3) . . . . ?
C19 N9 N10 C23 175.7(2) . . . . ?
C24 N11 N12 C26 0.2(2) . . . . ?
C20 N11 N12 C26 -176.07(18) . . . . ?
C1 N1 C2 C3 -179.5(2) . . . . ?
C1 N1 C2 S1 -0.9(4) . . . . ?
N1 C2 C3 C4 57.4(3) . . . . ?
S1 C2 C3 C4 -121.3(2) . . . . ?
N1 C2 C3 C5 -122.9(2) . . . . ?
S1 C2 C3 C5 58.5(3) . . . . ?
C5 C3 C4 C6 0.6(3) . . . . ?
C2 C3 C4 C6 -179.7(2) . . . . ?
C4 C3 C5 C7 -1.3(3) . . . . ?
C2 C3 C5 C7 178.9(2) . . . . ?
C7 N2 C6 C4 -0.1(3) . . . . ?
C7 N2 C6 N3 -179.9(2) . . . . ?
C3 C4 C6 N2 0.2(3) . . . . ?
C3 C4 C6 N3 180.0(2) . . . . ?
C8 N3 C6 N2 0.7(4) . . . . ?
N4 N3 C6 N2 178.7(2) . . . . ?
C8 N3 C6 C4 -179.1(2) . . . . ?
N4 N3 C6 C4 -1.1(4) . . . . ?
C6 N2 C7 C5 -0.8(3) . . . . ?
C6 N2 C7 N5 178.7(2) . . . . ?
C3 C5 C7 N2 1.5(3) . . . . ?
C3 C5 C7 N5 -177.9(2) . . . . ?
C11 N5 C7 N2 -8.1(4) . . . . ?
N6 N5 C7 N2 177.8(2) . . . . ?
C11 N5 C7 C5 171.4(3) . . . . ?
N6 N5 C7 C5 -2.7(3) . . . . ?
N4 N3 C8 C9 0.2(3) . . . . ?
C6 N3 C8 C9 178.4(2) . . . . ?
N3 C8 C9 C10 -0.5(3) . . . . ?
N3 N4 C10 C9 -0.5(4) . . . . ?
C8 C9 C10 N4 0.6(4) . . . . ?
N6 N5 C11 C12 0.0(3) . . . . ?
C7 N5 C11 C12 -174.6(3) . . . . ?
N5 C11 C12 C13 -0.5(3) . . . . ?
N5 N6 C13 C12 -0.8(3) . . . . ?
C11 C12 C13 N6 0.8(4) . . . . ?
C14 N7 C15 C16 179.6(2) . . . . ?
C14 N7 C15 S2 -0.3(4) . . . . ?
N7 C15 C16 C17 -56.2(3) . . . . ?
S2 C15 C16 C17 123.6(2) . . . . ?
N7 C15 C16 C18 123.8(2) . . . . ?
S2 C15 C16 C18 -56.3(3) . . . . ?
C18 C16 C17 C19 0.1(3) . . . . ?
C15 C16 C17 C19 -179.90(18) . . . . ?
C17 C16 C18 C20 0.3(3) . . . . ?
C15 C16 C18 C20 -179.73(18) . . . . ?
C20 N8 C19 C17 -0.4(3) . . . . ?
C20 N8 C19 N9 178.54(17) . . . . ?
C16 C17 C19 N8 0.0(3) . . . . ?
C16 C17 C19 N9 -178.93(19) . . . . ?
C21 N9 C19 N8 -7.8(3) . . . . ?
N10 N9 C19 N8 178.06(19) . . . . ?
C21 N9 C19 C17 171.2(2) . . . . ?
N10 N9 C19 C17 -2.9(3) . . . . ?
C19 N8 C20 C18 0.9(3) . . . . ?
C19 N8 C20 N11 -178.27(17) . . . . ?
C16 C18 C20 N8 -0.8(3) . . . . ?
C16 C18 C20 N11 178.29(18) . . . . ?
C24 N11 C20 N8 2.4(3) . . . . ?
N12 N11 C20 N8 177.95(17) . . . . ?
C24 N11 C20 C18 -176.8(2) . . . . ?
N12 N11 C20 C18 -1.2(3) . . . . ?
N10 N9 C21 C22 -0.4(3) . . . . ?
C19 N9 C21 C22 -175.0(2) . . . . ?
N9 C21 C22 C23 0.0(3) . . . . ?
N9 N10 C23 C22 -0.7(3) . . . . ?
C21 C22 C23 N10 0.5(4) . . . . ?
N12 N11 C24 C25 -0.2(2) . . . . ?
C20 N11 C24 C25 175.70(19) . . . . ?
N11 C24 C25 C26 0.1(2) . . . . ?
N11 N12 C26 C25 -0.1(2) . . . . ?
C24 C25 C26 N12 0.0(3) . . . . ?

#==============================================================================
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1N N6 . . 1_455 3.013(3) 0.80(3) 2.22(3) 173(3) no
N7 H7N N12 . . 1_655 3.095(3) 0.82(3) 2.28(3) 174(3) no

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.



#==============================================================================
#     End of CIF
#==============================================================================
_chemical_name_systematic        
N-methyl-2,6-bis(pyrazol-1-yl)pyridine-4-carbothioamide
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Ethyleacetate and ether'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_M171019B
_database_code_depnum_ccdc_archive 'CCDC 1860678'
_audit_update_record             
;
2018-08-07 deposited with the CCDC.
2018-11-09 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C27 H27 B2 F8 Fe N13 O2 S2'
_chemical_formula_moiety         '2(C13 H12 N6 S) Fe, 2(B F4), C H3 N O2'
_chemical_formula_weight         859.17
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
_space_group_IT_number           14
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 +X,-1/2-Y,-1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   8.0479(3)
_cell_length_b                   40.9514(14)
_cell_length_c                   10.6303(4)
_cell_angle_alpha                90.0000
_cell_angle_beta                 92.164(7)
_cell_angle_gamma                90.0000
_cell_volume                     3501.0(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    29995
_cell_measurement_theta_min      1.92
_cell_measurement_theta_max      27.47
_cell_measurement_temperature    100
#------------------------------------------------------------------------------
_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.250
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1744.00
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.116
_exptl_absorpt_correction_T_max  0.852

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      100
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            32970
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_theta_max         27.470
_diffrn_reflns_theta_min         2.160
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             8012
_reflns_number_gt                7073
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0440
_refine_ls_wR_factor_ref         0.1227
_refine_ls_wR_factor_gt          0.1182
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         8012
_refine_ls_number_parameters     504
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0654P)²+2.7849P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         0.71
_refine_diff_density_min         -0.55
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Fe Fe 0.3463 0.8444
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
B B 0.0013 0.0007
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
F F 0.0171 0.0103
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.33862(4) 0.11508(2) 0.30145(2) 0.01890(9) Uani 1 1 d . . . . .
S1 S 0.51688(8) 0.27750(2) 0.50882(5) 0.02930(14) Uani 1 1 d . . . . .
S2 S 0.36732(8) -0.05802(2) 0.32810(5) 0.02975(14) Uani 1 1 d . . . . .
F1 F 0.0599(2) 0.24621(4) 0.61289(14) 0.0450(4) Uani 1 1 d . . . . .
F2 F -0.03305(17) 0.22332(3) 0.42803(12) 0.0326(3) Uani 1 1 d . . . . .
F3 F -0.1297(2) 0.20587(5) 0.61302(15) 0.0551(5) Uani 1 1 d . . . . .
F4 F 0.1350(3) 0.19471(5) 0.56434(17) 0.0610(5) Uani 1 1 d . . . . .
F5 F -0.2956(2) 0.04539(5) 0.16438(17) 0.0619(5) Uani 1 1 d . . . . .
F7 F -0.1591(2) 0.01597(4) 0.31715(13) 0.0437(4) Uani 1 1 d . . . . .
F61 F -0.0541(2) 0.02061(6) 0.1185(2) 0.0513(6) Uani 0.809(3) 1 d . . P . .
F62 F -0.0505(10) 0.0440(3) 0.1755(9) 0.0513(6) Uani 0.191(3) 1 d . . P . .
F81 F -0.2884(4) -0.00829(6) 0.1502(2) 0.0638(8) Uani 0.784(4) 1 d . . P . .
F82 F -0.1613(16) -0.0071(2) 0.1320(8) 0.0638(8) Uani 0.216(4) 1 d . . P . .
O1 O 0.1308(3) 0.15175(5) -0.1271(2) 0.0573(6) Uani 1 1 d . . . . .
O2 O -0.1348(3) 0.15385(5) -0.1543(2) 0.0493(5) Uani 1 1 d . . . . .
N1 N 0.4708(2) 0.27714(4) 0.25931(17) 0.0260(4) Uani 1 1 d . . . . .
H1 H 0.450262 0.265966 0.189745 0.031 Uiso 1 1 calc R U . . .
N2 N 0.3796(2) 0.16012(4) 0.32668(15) 0.0202(3) Uani 1 1 d . . . . .
N3 N 0.1196(2) 0.16669(4) 0.24421(16) 0.0215(3) Uani 1 1 d . . . . .
N4 N 0.1216(2) 0.13286(4) 0.24145(15) 0.0218(3) Uani 1 1 d . . . . .
N5 N 0.6274(2) 0.14319(4) 0.40790(16) 0.0218(3) Uani 1 1 d . . . . .
N6 N 0.5692(2) 0.11304(4) 0.36727(15) 0.0212(3) Uani 1 1 d . . . . .
N7 N 0.1556(2) -0.04078(4) 0.14055(18) 0.0277(4) Uani 1 1 d . . . . .
H7 H 0.105470 -0.024906 0.098146 0.033 Uiso 1 1 calc R U . . .
N8 N 0.3075(2) 0.06959(4) 0.28051(15) 0.0206(3) Uani 1 1 d . . . . .
N9 N 0.2427(2) 0.07041(4) 0.48488(15) 0.0216(3) Uani 1 1 d . . . . .
N10 N 0.2630(2) 0.10362(4) 0.46960(16) 0.0214(3) Uani 1 1 d . . . . .
N11 N 0.3857(2) 0.07895(4) 0.08214(15) 0.0214(3) Uani 1 1 d . . . . .
N12 N 0.4021(2) 0.11061(4) 0.12537(16) 0.0210(3) Uani 1 1 d . . . . .
N13 N -0.0006(3) 0.16672(5) -0.13242(19) 0.0335(4) Uani 1 1 d . . . . .
C1 C 0.4936(3) 0.31248(5) 0.2487(2) 0.0296(5) Uani 1 1 d . . . . .
H1A H 0.481839 0.318949 0.160074 0.035 Uiso 1 1 calc R U . . .
H1B H 0.409396 0.323725 0.297005 0.035 Uiso 1 1 calc R U . . .
H1C H 0.604673 0.318437 0.282009 0.035 Uiso 1 1 calc R U . . .
C2 C 0.4792(3) 0.26104(5) 0.36670(19) 0.0230(4) Uani 1 1 d . . . . .
C3 C 0.4448(3) 0.22525(5) 0.35423(18) 0.0224(4) Uani 1 1 d . . . . .
C4 C 0.2922(3) 0.21542(5) 0.29951(18) 0.0221(4) Uani 1 1 d . . . . .
H4 H 0.211577 0.230803 0.269816 0.027 Uiso 1 1 calc R U . . .
C5 C 0.5647(3) 0.20262(5) 0.39679(19) 0.0232(4) Uani 1 1 d . . . . .
H5 H 0.667069 0.209284 0.436137 0.028 Uiso 1 1 calc R U . . .
C6 C 0.2647(3) 0.18209(5) 0.29081(18) 0.0209(4) Uani 1 1 d . . . . .
C7 C 0.5258(3) 0.17007(5) 0.37838(18) 0.0207(4) Uani 1 1 d . . . . .
C8 C -0.0278(3) 0.17854(5) 0.19595(19) 0.0248(4) Uani 1 1 d . . . . .
H8 H -0.059137 0.200845 0.188683 0.030 Uiso 1 1 calc R U . . .
C9 C -0.1218(3) 0.15201(6) 0.1600(2) 0.0274(4) Uani 1 1 d . . . . .
H9 H -0.230598 0.152267 0.122098 0.033 Uiso 1 1 calc R U . . .
C10 C -0.0249(3) 0.12431(5) 0.19039(19) 0.0251(4) Uani 1 1 d . . . . .
H10 H -0.059827 0.102410 0.176250 0.030 Uiso 1 1 calc R U . . .
C11 C 0.7804(3) 0.14015(5) 0.4675(2) 0.0262(4) Uani 1 1 d . . . . .
H11 H 0.846074 0.157266 0.503623 0.031 Uiso 1 1 calc R U . . .
C12 C 0.8202(3) 0.10785(6) 0.4650(2) 0.0285(4) Uani 1 1 d . . . . .
H12 H 0.918823 0.098006 0.499061 0.034 Uiso 1 1 calc R U . . .
C13 C 0.6866(3) 0.09194(5) 0.40200(19) 0.0242(4) Uani 1 1 d . . . . .
H13 H 0.681293 0.069117 0.386466 0.029 Uiso 1 1 calc R U . . .
C14 C 0.1186(3) -0.07420(6) 0.1018(2) 0.0314(5) Uani 1 1 d . . . . .
H14A H 0.038646 -0.073991 0.029951 0.038 Uiso 1 1 calc R U . . .
H14B H 0.221222 -0.084992 0.077467 0.038 Uiso 1 1 calc R U . . .
H14C H 0.071098 -0.086094 0.171900 0.038 Uiso 1 1 calc R U . . .
C15 C 0.2593(3) -0.03256(5) 0.23516(19) 0.0233(4) Uani 1 1 d . . . . .
C16 C 0.2789(3) 0.00336(5) 0.25298(19) 0.0222(4) Uani 1 1 d . . . . .
C17 C 0.2544(3) 0.01740(5) 0.37081(19) 0.0232(4) Uani 1 1 d . . . . .
H17 H 0.229678 0.004512 0.442017 0.028 Uiso 1 1 calc R U . . .
C18 C 0.3210(3) 0.02246(5) 0.14982(19) 0.0228(4) Uani 1 1 d . . . . .
H18 H 0.337674 0.013053 0.069592 0.027 Uiso 1 1 calc R U . . .
C19 C 0.2679(3) 0.05090(5) 0.37828(18) 0.0213(4) Uani 1 1 d . . . . .
C20 C 0.3372(2) 0.05560(5) 0.17007(18) 0.0211(4) Uani 1 1 d . . . . .
C21 C 0.2010(3) 0.06313(5) 0.60454(19) 0.0252(4) Uani 1 1 d . . . . .
H21 H 0.181556 0.041975 0.637604 0.030 Uiso 1 1 calc R U . . .
C22 C 0.1925(3) 0.09204(5) 0.6680(2) 0.0264(4) Uani 1 1 d . . . . .
H22 H 0.165283 0.095022 0.753440 0.032 Uiso 1 1 calc R U . . .
C23 C 0.2322(3) 0.11658(5) 0.58107(19) 0.0241(4) Uani 1 1 d . . . . .
H23 H 0.236385 0.139266 0.599580 0.029 Uiso 1 1 calc R U . . .
C24 C 0.4290(3) 0.07663(5) -0.03988(19) 0.0246(4) Uani 1 1 d . . . . .
H24 H 0.428701 0.057386 -0.089780 0.030 Uiso 1 1 calc R U . . .
C25 C 0.4729(3) 0.10730(5) -0.07706(19) 0.0260(4) Uani 1 1 d . . . . .
H25 H 0.509205 0.113548 -0.157573 0.031 Uiso 1 1 calc R U . . .
C26 C 0.4536(3) 0.12774(5) 0.02771(19) 0.0235(4) Uani 1 1 d . . . . .
H26 H 0.474297 0.150582 0.028669 0.028 Uiso 1 1 calc R U . . .
C27 C 0.0040(4) 0.20237(6) -0.1085(2) 0.0399(6) Uani 1 1 d . . . . .
H27A H 0.119393 0.209321 -0.092431 0.048 Uiso 1 1 calc R U . . .
H27B H -0.042975 0.213954 -0.182257 0.048 Uiso 1 1 calc R U . . .
H27C H -0.061329 0.207403 -0.035019 0.048 Uiso 1 1 calc R U . . .
B1 B 0.0097(3) 0.21766(6) 0.5545(2) 0.0295(5) Uani 1 1 d . . . . .
B2 B -0.1932(3) 0.01959(7) 0.1897(2) 0.0310(5) Uani 1 1 d . . . . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_computing_structure_refinement  'SHELXL Version 2017/1 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.5 (Rigaku, 2017)'
_computing_molecular_graphics    'CrystalStructure 4.2.5'

#==============================================================================
# MOLECULAR GEOMETRY

_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 1.8913(17) . ?
Fe1 N8 1.8914(17) . ?
Fe1 N6 1.9602(18) . ?
Fe1 N10 1.9668(17) . ?
Fe1 N12 1.9673(17) . ?
Fe1 N4 1.9755(18) . ?
S1 C2 1.671(2) . ?
S2 C15 1.660(2) . ?
F1 B1 1.377(3) . ?
F2 B1 1.395(3) . ?
F3 B1 1.390(3) . ?
F4 B1 1.379(3) . ?
F5 B2 1.360(3) . ?
F7 B2 1.380(3) . ?
F61 F62 1.133(11) . ?
F61 B2 1.375(3) . ?
F61 F82 1.437(9) . ?
F62 B2 1.534(11) . ?
F81 F82 1.049(11) . ?
F81 B2 1.429(4) . ?
F82 B2 1.285(10) . ?
O1 N13 1.222(3) . ?
O2 N13 1.216(3) . ?
N1 C2 1.318(3) . ?
N1 C1 1.464(3) . ?
N2 C6 1.335(3) . ?
N2 C7 1.343(3) . ?
N3 C8 1.363(3) . ?
N3 N4 1.386(2) . ?
N3 C6 1.402(3) . ?
N4 C10 1.327(3) . ?
N5 C11 1.369(3) . ?
N5 N6 1.384(2) . ?
N5 C7 1.400(3) . ?
N6 C13 1.322(3) . ?
N7 C15 1.326(3) . ?
N7 C14 1.457(3) . ?
N8 C20 1.336(3) . ?
N8 C19 1.339(3) . ?
N9 C21 1.361(3) . ?
N9 N10 1.380(2) . ?
N9 C19 1.407(3) . ?
N10 C23 1.330(3) . ?
N11 C24 1.359(3) . ?
N11 N12 1.380(2) . ?
N11 C20 1.403(3) . ?
N12 C26 1.332(3) . ?
N13 C27 1.482(3) . ?
C2 C3 1.497(3) . ?
C3 C4 1.398(3) . ?
C3 C5 1.401(3) . ?
C4 C6 1.385(3) . ?
C5 C7 1.382(3) . ?
C8 C9 1.370(3) . ?
C9 C10 1.407(3) . ?
C11 C12 1.362(3) . ?
C12 C13 1.405(3) . ?
C15 C16 1.490(3) . ?
C16 C17 1.399(3) . ?
C16 C18 1.399(3) . ?
C17 C19 1.378(3) . ?
C18 C20 1.379(3) . ?
C21 C22 1.366(3) . ?
C22 C23 1.410(3) . ?
C24 C25 1.367(3) . ?
C25 C26 1.407(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N8 177.22(7) . . ?
N2 Fe1 N6 80.40(7) . . ?
N8 Fe1 N6 96.85(7) . . ?
N2 Fe1 N10 99.32(7) . . ?
N8 Fe1 N10 80.09(7) . . ?
N6 Fe1 N10 89.25(7) . . ?
N2 Fe1 N12 100.11(7) . . ?
N8 Fe1 N12 80.47(7) . . ?
N6 Fe1 N12 93.39(7) . . ?
N10 Fe1 N12 160.56(7) . . ?
N2 Fe1 N4 80.41(7) . . ?
N8 Fe1 N4 102.34(7) . . ?
N6 Fe1 N4 160.80(7) . . ?
N10 Fe1 N4 94.65(7) . . ?
N12 Fe1 N4 89.17(7) . . ?
F62 F61 B2 74.7(5) . . ?
F62 F61 F82 128.2(6) . . ?
B2 F61 F82 54.3(5) . . ?
F61 F62 B2 59.9(5) . . ?
F82 F81 B2 60.2(5) . . ?
F81 F82 B2 74.7(7) . . ?
F81 F82 F61 130.3(9) . . ?
B2 F82 F61 60.4(4) . . ?
C2 N1 C1 123.97(18) . . ?
C6 N2 C7 119.94(17) . . ?
C6 N2 Fe1 120.11(14) . . ?
C7 N2 Fe1 119.93(14) . . ?
C8 N3 N4 111.03(16) . . ?
C8 N3 C6 132.40(18) . . ?
N4 N3 C6 116.54(16) . . ?
C10 N4 N3 105.15(17) . . ?
C10 N4 Fe1 142.78(15) . . ?
N3 N4 Fe1 111.89(12) . . ?
C11 N5 N6 110.58(17) . . ?
C11 N5 C7 133.07(18) . . ?
N6 N5 C7 116.32(16) . . ?
C13 N6 N5 105.42(17) . . ?
C13 N6 Fe1 141.64(15) . . ?
N5 N6 Fe1 112.23(12) . . ?
C15 N7 C14 124.68(19) . . ?
C20 N8 C19 119.51(18) . . ?
C20 N8 Fe1 119.90(14) . . ?
C19 N8 Fe1 120.40(14) . . ?
C21 N9 N10 111.12(16) . . ?
C21 N9 C19 132.55(18) . . ?
N10 N9 C19 116.33(16) . . ?
C23 N10 N9 105.16(16) . . ?
C23 N10 Fe1 142.09(15) . . ?
N9 N10 Fe1 112.58(12) . . ?
C24 N11 N12 111.03(16) . . ?
C24 N11 C20 132.53(17) . . ?
N12 N11 C20 116.36(16) . . ?
C26 N12 N11 105.31(16) . . ?
C26 N12 Fe1 142.39(14) . . ?
N11 N12 Fe1 112.28(12) . . ?
O2 N13 O1 123.5(2) . . ?
O2 N13 C27 118.4(2) . . ?
O1 N13 C27 118.1(2) . . ?
N1 C2 C3 114.20(17) . . ?
N1 C2 S1 125.65(16) . . ?
C3 C2 S1 120.11(15) . . ?
C4 C3 C5 121.82(19) . . ?
C4 C3 C2 118.42(18) . . ?
C5 C3 C2 119.76(18) . . ?
C6 C4 C3 116.57(19) . . ?
C7 C5 C3 116.31(18) . . ?
N2 C6 C4 122.52(19) . . ?
N2 C6 N3 110.89(17) . . ?
C4 C6 N3 126.59(18) . . ?
N2 C7 C5 122.73(18) . . ?
N2 C7 N5 110.43(17) . . ?
C5 C7 N5 126.85(18) . . ?
N3 C8 C9 106.62(19) . . ?
C8 C9 C10 106.25(19) . . ?
N4 C10 C9 110.95(19) . . ?
C12 C11 N5 106.68(19) . . ?
C11 C12 C13 106.48(19) . . ?
N6 C13 C12 110.84(19) . . ?
N7 C15 C16 114.04(18) . . ?
N7 C15 S2 126.35(16) . . ?
C16 C15 S2 119.60(15) . . ?
C17 C16 C18 121.22(19) . . ?
C17 C16 C15 120.11(18) . . ?
C18 C16 C15 118.67(18) . . ?
C19 C17 C16 116.57(18) . . ?
C20 C18 C16 116.88(19) . . ?
N8 C19 C17 123.02(18) . . ?
N8 C19 N9 110.25(17) . . ?
C17 C19 N9 126.73(18) . . ?
N8 C20 C18 122.69(18) . . ?
N8 C20 N11 110.89(17) . . ?
C18 C20 N11 126.42(18) . . ?
N9 C21 C22 106.89(19) . . ?
C21 C22 C23 106.09(19) . . ?
N10 C23 C22 110.74(18) . . ?
N11 C24 C25 106.86(18) . . ?
C24 C25 C26 106.29(18) . . ?
N12 C26 C25 110.51(18) . . ?
F1 B1 F4 110.1(2) . . ?
F1 B1 F3 108.7(2) . . ?
F4 B1 F3 109.2(2) . . ?
F1 B1 F2 110.53(19) . . ?
F4 B1 F2 109.8(2) . . ?
F3 B1 F2 108.4(2) . . ?
F82 B2 F5 134.2(5) . . ?
F82 B2 F61 65.3(5) . . ?
F5 B2 F61 111.5(2) . . ?
F82 B2 F7 109.9(5) . . ?
F5 B2 F7 112.0(2) . . ?
F61 B2 F7 114.0(2) . . ?
F82 B2 F81 45.1(5) . . ?
F5 B2 F81 104.4(2) . . ?
F61 B2 F81 107.5(2) . . ?
F7 B2 F81 106.7(2) . . ?
F82 B2 F62 110.1(7) . . ?
F5 B2 F62 85.7(4) . . ?
F61 B2 F62 45.4(4) . . ?
F7 B2 F62 92.6(4) . . ?
F81 B2 F62 152.4(4) . . ?

#==============================================================================
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N7 H7 F61 . . 3_555 2.960(3) 0.880 2.331 128.5 no
N7 H7 F82 . . . 2.897(12) 0.880 2.308 124.3 no

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.



#==============================================================================
#     End of CIF
#==============================================================================
_chemical_name_systematic        
'Iron(II) bis(N-methyl-2,6-bis(pyrazol-1-yl)pyridine-4-carbothioamide ) tetrafluorobroate'
####################################################################### 
# 
# 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_M171106A
_database_code_depnum_ccdc_archive 'CCDC 1860682'
_audit_update_record             
;
2018-09-05 deposited with the CCDC.
2018-11-09 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C26 H24 Cl2 Fe N12 O8 S2'
_chemical_formula_moiety         '2(C13 H12 N6 S) Fe, 2(Cl O4)'
_chemical_formula_weight         823.42
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_space_group_IT_number           2
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,-Y,-Z
#------------------------------------------------------------------------------
_cell_length_a                   8.2899(3)
_cell_length_b                   9.9601(3)
_cell_length_c                   20.7440(6)
_cell_angle_alpha                80.302(6)
_cell_angle_beta                 83.941(6)
_cell_angle_gamma                89.321(6)
_cell_volume                     1678.85(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11598
_cell_measurement_theta_min      2.00
_cell_measurement_theta_max      27.45
_cell_measurement_temperature    290
#------------------------------------------------------------------------------
_exptl_crystal_description       needle
_exptl_crystal_colour            dark
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.060
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             840.00
_exptl_absorpt_coefficient_mu    0.800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.735
_exptl_absorpt_correction_T_max  0.953

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      290
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            16514
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_theta_max         27.451
_diffrn_reflns_theta_min         2.003
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             7649
_reflns_number_gt                5786
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
Two reflections, -2 -1 1 and -2 0 1, have been omitted from the least 
square calculations because of large differences between each Fo and Fc, which 
probably caused by a measurement error of the IP system. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0639
_refine_ls_wR_factor_ref         0.1750
_refine_ls_wR_factor_gt          0.1618
_refine_ls_number_restraints     4
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_reflns         7649
_refine_ls_number_parameters     463
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0723P)²+3.8359P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         1.26
_refine_diff_density_min         -1.07
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Fe Fe 0.3463 0.8444
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.57169(7) 0.49890(6) 0.24096(2) 0.03150(16) Uani 1 1 d . . . . .
Cl1 Cl 0.24883(16) 0.89550(12) 0.03013(6) 0.0549(3) Uani 1 1 d . . . . .
Cl2 Cl 0.35359(16) 0.95516(14) 0.40086(6) 0.0590(3) Uani 1 1 d . . . . .
S1 S 0.8681(2) 0.52330(14) -0.09697(6) 0.0778(5) Uani 1 1 d . . . . .
S2 S 0.18454(15) 0.42390(12) 0.56973(5) 0.0486(3) Uani 1 1 d . . . . .
O1 O 0.1999(11) 0.9188(12) -0.0308(3) 0.217(5) Uani 1 1 d . . . . .
O2 O 0.3129(9) 1.0153(6) 0.0364(6) 0.215(5) Uani 1 1 d . . . . .
O3 O 0.3685(5) 0.7928(4) 0.03492(18) 0.0651(10) Uani 1 1 d . . . . .
O4 O 0.1146(6) 0.8639(5) 0.0773(2) 0.0960(16) Uani 1 1 d . . . . .
O5 O 0.5157(6) 1.0017(8) 0.3841(3) 0.128(2) Uani 1 1 d . . . . .
O6 O 0.2580(8) 1.0622(8) 0.3779(4) 0.181(4) Uani 1 1 d . . . . .
O7 O 0.3310(12) 0.8433(11) 0.3772(6) 0.262(7) Uani 1 1 d . . . . .
O8 O 0.3063(11) 0.9317(8) 0.4686(3) 0.154(3) Uani 1 1 d . . . . .
N1 N 0.8897(8) 0.7652(5) -0.0710(2) 0.096(2) Uani 1 1 d D . . . .
H1 H 0.830(4) 0.8256(19) -0.0531(8) 0.116 Uiso 1 1 d D U . . .
N2 N 0.6525(4) 0.5427(3) 0.15074(14) 0.0310(7) Uani 1 1 d . . . . .
N3 N 0.7229(4) 0.7427(3) 0.17730(15) 0.0368(7) Uani 1 1 d . . . . .
N4 N 0.6645(4) 0.6818(3) 0.23973(15) 0.0364(7) Uani 1 1 d . . . . .
N5 N 0.5535(4) 0.3378(3) 0.14275(15) 0.0358(7) Uani 1 1 d . . . . .
N6 N 0.5060(4) 0.3340(4) 0.20908(15) 0.0380(7) Uani 1 1 d . . . . .
N7 N 0.2091(5) 0.1837(4) 0.53047(19) 0.0509(10) Uani 1 1 d . . . . .
H7 H 0.246651 0.137149 0.500930 0.061 Uiso 1 1 calc R U . . .
N8 N 0.4775(4) 0.4522(3) 0.32951(14) 0.0330(7) Uani 1 1 d . . . . .
N9 N 0.7086(4) 0.3373(3) 0.34611(15) 0.0363(7) Uani 1 1 d . . . . .
N10 N 0.7539(4) 0.3975(3) 0.28211(15) 0.0362(7) Uani 1 1 d . . . . .
N11 N 0.2656(4) 0.5769(4) 0.29346(15) 0.0381(8) Uani 1 1 d . . . . .
N12 N 0.3599(4) 0.5890(3) 0.23372(15) 0.0367(7) Uani 1 1 d . . . . .
C1 C 0.9702(10) 0.8165(6) -0.1362(3) 0.094(3) Uani 1 1 d D . . . .
H1A H 0.990724 0.912314 -0.140194 0.113 Uiso 1 1 calc R U . . .
H1B H 1.071088 0.769725 -0.142585 0.113 Uiso 1 1 calc R U . . .
H1C H 0.901898 0.801157 -0.168929 0.113 Uiso 1 1 calc R U . . .
C2 C 0.8454(5) 0.6396(4) -0.05006(19) 0.0370(9) Uani 1 1 d D . . . .
C3 C 0.7710(5) 0.6080(4) 0.02040(18) 0.0340(8) Uani 1 1 d . . . . .
C4 C 0.7851(5) 0.7006(4) 0.06284(19) 0.0379(9) Uani 1 1 d . . . . .
H4 H 0.835022 0.784882 0.047995 0.046 Uiso 1 1 calc R U . . .
C5 C 0.6929(5) 0.4824(4) 0.04347(18) 0.0354(8) Uani 1 1 d . . . . .
H5 H 0.680698 0.419920 0.015681 0.043 Uiso 1 1 calc R U . . .
C6 C 0.7231(5) 0.6634(4) 0.12731(18) 0.0327(8) Uani 1 1 d . . . . .
C7 C 0.6348(5) 0.4556(4) 0.10917(18) 0.0328(8) Uani 1 1 d . . . . .
C8 C 0.7583(6) 0.8760(4) 0.1751(2) 0.0452(10) Uani 1 1 d . . . . .
H8 H 0.797463 0.937901 0.138195 0.054 Uiso 1 1 calc R U . . .
C9 C 0.7255(7) 0.9016(5) 0.2376(2) 0.0516(11) Uani 1 1 d . . . . .
H9 H 0.739677 0.983844 0.251954 0.062 Uiso 1 1 calc R U . . .
C10 C 0.6661(6) 0.7797(5) 0.2759(2) 0.0446(10) Uani 1 1 d . . . . .
H10 H 0.632206 0.768658 0.320641 0.054 Uiso 1 1 calc R U . . .
C11 C 0.5091(6) 0.2208(4) 0.1231(2) 0.0464(10) Uani 1 1 d . . . . .
H11 H 0.526577 0.199526 0.080983 0.056 Uiso 1 1 calc R U . . .
C12 C 0.4339(6) 0.1416(5) 0.1776(2) 0.0529(12) Uani 1 1 d . . . . .
H12 H 0.390202 0.055175 0.179905 0.063 Uiso 1 1 calc R U . . .
C13 C 0.4350(6) 0.2142(5) 0.2288(2) 0.0460(10) Uani 1 1 d . . . . .
H13 H 0.391097 0.182485 0.271780 0.055 Uiso 1 1 calc R U . . .
C14 C 0.1170(7) 0.1113(6) 0.5888(3) 0.0672(15) Uani 1 1 d . . . . .
H14A H 0.111107 0.016476 0.585674 0.081 Uiso 1 1 calc R U . . .
H14B H 0.169267 0.121525 0.626869 0.081 Uiso 1 1 calc R U . . .
H14C H 0.009394 0.147921 0.592631 0.081 Uiso 1 1 calc R U . . .
C15 C 0.2399(5) 0.3151(4) 0.51912(18) 0.0357(8) Uani 1 1 d . . . . .
C16 C 0.3285(5) 0.3664(4) 0.45346(18) 0.0350(8) Uani 1 1 d . . . . .
C17 C 0.4841(5) 0.3197(4) 0.43618(18) 0.0363(8) Uani 1 1 d . . . . .
H17 H 0.537973 0.258888 0.465568 0.044 Uiso 1 1 calc R U . . .
C18 C 0.2491(5) 0.4584(4) 0.40874(18) 0.0383(9) Uani 1 1 d . . . . .
H18 H 0.147761 0.493164 0.420595 0.046 Uiso 1 1 calc R U . . .
C19 C 0.5531(5) 0.3681(4) 0.37375(18) 0.0324(8) Uani 1 1 d . . . . .
C20 C 0.3274(5) 0.4950(4) 0.34673(18) 0.0350(8) Uani 1 1 d . . . . .
C21 C 0.8315(6) 0.2657(5) 0.3727(2) 0.0473(11) Uani 1 1 d . . . . .
H21 H 0.829673 0.218211 0.415360 0.057 Uiso 1 1 calc R U . . .
C22 C 0.9601(6) 0.2767(5) 0.3244(2) 0.0506(11) Uani 1 1 d . . . . .
H22 H 1.062098 0.237658 0.327540 0.061 Uiso 1 1 calc R U . . .
C23 C 0.9051(5) 0.3590(5) 0.2695(2) 0.0448(10) Uani 1 1 d . . . . .
H23 H 0.967302 0.383449 0.229331 0.054 Uiso 1 1 calc R U . . .
C24 C 0.1303(5) 0.6528(5) 0.2878(2) 0.0477(11) Uani 1 1 d . . . . .
H24 H 0.048162 0.660392 0.321130 0.057 Uiso 1 1 calc R U . . .
C25 C 0.1367(6) 0.7156(5) 0.2244(2) 0.0536(12) Uani 1 1 d . . . . .
H25 H 0.060765 0.775613 0.205876 0.064 Uiso 1 1 calc R U . . .
C26 C 0.2796(6) 0.6727(5) 0.1923(2) 0.0443(10) Uani 1 1 d . . . . .
H26 H 0.313673 0.699376 0.147859 0.053 Uiso 1 1 calc R U . . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_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 1.900(3) . ?
Fe1 N8 1.902(3) . ?
Fe1 N12 1.971(3) . ?
Fe1 N6 1.974(4) . ?
Fe1 N4 1.981(4) . ?
Fe1 N10 1.994(3) . ?
Cl1 O2 1.343(6) . ?
Cl1 O1 1.350(6) . ?
Cl1 O4 1.404(4) . ?
Cl1 O3 1.415(4) . ?
Cl2 O7 1.313(7) . ?
Cl2 O6 1.371(6) . ?
Cl2 O8 1.400(5) . ?
Cl2 O5 1.416(6) . ?
S1 C2 1.631(4) . ?
S2 C15 1.661(4) . ?
N1 C2 1.297(6) . ?
N1 C1 1.457(6) . ?
N1 H1 0.879(9) . ?
N2 C6 1.336(5) . ?
N2 C7 1.341(5) . ?
N3 C8 1.356(5) . ?
N3 N4 1.375(4) . ?
N3 C6 1.405(5) . ?
N4 C10 1.327(5) . ?
N5 C11 1.364(5) . ?
N5 N6 1.385(4) . ?
N5 C7 1.400(5) . ?
N6 C13 1.319(5) . ?
N7 C15 1.313(5) . ?
N7 C14 1.447(6) . ?
N7 H7 0.8600 . ?
N8 C19 1.337(5) . ?
N8 C20 1.343(5) . ?
N9 C21 1.349(5) . ?
N9 N10 1.377(4) . ?
N9 C19 1.406(5) . ?
N10 C23 1.319(5) . ?
N11 C24 1.349(5) . ?
N11 N12 1.382(4) . ?
N11 C20 1.398(5) . ?
N12 C26 1.320(5) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.508(5) . ?
C3 C4 1.392(5) . ?
C3 C5 1.402(5) . ?
C4 C6 1.372(5) . ?
C4 H4 0.9300 . ?
C5 C7 1.379(5) . ?
C5 H5 0.9300 . ?
C8 C9 1.362(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.398(7) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.360(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.384(7) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.490(5) . ?
C16 C17 1.397(5) . ?
C16 C18 1.400(5) . ?
C17 C19 1.370(5) . ?
C17 H17 0.9300 . ?
C18 C20 1.371(5) . ?
C18 H18 0.9300 . ?
C21 C22 1.375(6) . ?
C21 H21 0.9300 . ?
C22 C23 1.401(7) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 C25 1.354(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.396(6) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?

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 N8 176.25(14) . . ?
N2 Fe1 N12 97.12(13) . . ?
N8 Fe1 N12 80.16(13) . . ?
N2 Fe1 N6 79.70(13) . . ?
N8 Fe1 N6 97.89(14) . . ?
N12 Fe1 N6 94.70(15) . . ?
N2 Fe1 N4 80.11(13) . . ?
N8 Fe1 N4 102.24(14) . . ?
N12 Fe1 N4 87.05(14) . . ?
N6 Fe1 N4 159.80(13) . . ?
N2 Fe1 N10 103.48(13) . . ?
N8 Fe1 N10 79.33(13) . . ?
N12 Fe1 N10 159.35(12) . . ?
N6 Fe1 N10 90.43(14) . . ?
N4 Fe1 N10 94.99(14) . . ?
O2 Cl1 O1 103.8(7) . . ?
O2 Cl1 O4 109.5(5) . . ?
O1 Cl1 O4 110.0(5) . . ?
O2 Cl1 O3 110.2(4) . . ?
O1 Cl1 O3 110.6(4) . . ?
O4 Cl1 O3 112.4(3) . . ?
O7 Cl2 O6 114.5(8) . . ?
O7 Cl2 O8 109.1(6) . . ?
O6 Cl2 O8 103.1(5) . . ?
O7 Cl2 O5 110.6(5) . . ?
O6 Cl2 O5 105.9(4) . . ?
O8 Cl2 O5 113.6(5) . . ?
C2 N1 C1 124.8(4) . . ?
C2 N1 H1 114.7(18) . . ?
C1 N1 H1 114.5(13) . . ?
C6 N2 C7 118.9(3) . . ?
C6 N2 Fe1 120.1(2) . . ?
C7 N2 Fe1 120.9(3) . . ?
C8 N3 N4 111.4(3) . . ?
C8 N3 C6 131.5(3) . . ?
N4 N3 C6 116.9(3) . . ?
C10 N4 N3 104.8(3) . . ?
C10 N4 Fe1 141.7(3) . . ?
N3 N4 Fe1 112.0(2) . . ?
C11 N5 N6 110.7(3) . . ?
C11 N5 C7 132.6(3) . . ?
N6 N5 C7 116.7(3) . . ?
C13 N6 N5 104.8(3) . . ?
C13 N6 Fe1 142.5(3) . . ?
N5 N6 Fe1 112.7(2) . . ?
C15 N7 C14 125.0(4) . . ?
C15 N7 H7 117.5 . . ?
C14 N7 H7 117.5 . . ?
C19 N8 C20 119.2(3) . . ?
C19 N8 Fe1 120.9(2) . . ?
C20 N8 Fe1 119.7(3) . . ?
C21 N9 N10 111.4(3) . . ?
C21 N9 C19 131.4(3) . . ?
N10 N9 C19 116.9(3) . . ?
C23 N10 N9 104.9(3) . . ?
C23 N10 Fe1 142.9(3) . . ?
N9 N10 Fe1 112.1(2) . . ?
C24 N11 N12 110.7(3) . . ?
C24 N11 C20 133.0(3) . . ?
N12 N11 C20 116.3(3) . . ?
C26 N12 N11 105.1(3) . . ?
C26 N12 Fe1 141.7(3) . . ?
N11 N12 Fe1 112.6(2) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 115.8(4) . . ?
N1 C2 S1 122.1(3) . . ?
C3 C2 S1 122.1(3) . . ?
C4 C3 C5 120.2(3) . . ?
C4 C3 C2 120.3(3) . . ?
C5 C3 C2 119.5(3) . . ?
C6 C4 C3 117.8(4) . . ?
C6 C4 H4 121.1 . . ?
C3 C4 H4 121.1 . . ?
C7 C5 C3 117.1(3) . . ?
C7 C5 H5 121.4 . . ?
C3 C5 H5 121.4 . . ?
N2 C6 C4 122.9(3) . . ?
N2 C6 N3 110.6(3) . . ?
C4 C6 N3 126.5(4) . . ?
N2 C7 C5 122.9(3) . . ?
N2 C7 N5 110.1(3) . . ?
C5 C7 N5 127.0(3) . . ?
N3 C8 C9 106.6(4) . . ?
N3 C8 H8 126.7 . . ?
C9 C8 H8 126.7 . . ?
C8 C9 C10 106.3(4) . . ?
C8 C9 H9 126.8 . . ?
C10 C9 H9 126.8 . . ?
N4 C10 C9 110.9(4) . . ?
N4 C10 H10 124.5 . . ?
C9 C10 H10 124.5 . . ?
C12 C11 N5 106.1(4) . . ?
C12 C11 H11 126.9 . . ?
N5 C11 H11 126.9 . . ?
C11 C12 C13 106.9(4) . . ?
C11 C12 H12 126.5 . . ?
C13 C12 H12 126.5 . . ?
N6 C13 C12 111.4(4) . . ?
N6 C13 H13 124.3 . . ?
C12 C13 H13 124.3 . . ?
N7 C14 H14A 109.5 . . ?
N7 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N7 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N7 C15 C16 114.6(4) . . ?
N7 C15 S2 125.9(3) . . ?
C16 C15 S2 119.5(3) . . ?
C17 C16 C18 121.0(3) . . ?
C17 C16 C15 120.7(3) . . ?
C18 C16 C15 118.2(3) . . ?
C19 C17 C16 116.6(3) . . ?
C19 C17 H17 121.7 . . ?
C16 C17 H17 121.7 . . ?
C20 C18 C16 117.1(4) . . ?
C20 C18 H18 121.4 . . ?
C16 C18 H18 121.4 . . ?
N8 C19 C17 123.4(3) . . ?
N8 C19 N9 110.0(3) . . ?
C17 C19 N9 126.6(4) . . ?
N8 C20 C18 122.5(4) . . ?
N8 C20 N11 111.0(3) . . ?
C18 C20 N11 126.5(4) . . ?
N9 C21 C22 106.8(4) . . ?
N9 C21 H21 126.6 . . ?
C22 C21 H21 126.6 . . ?
C21 C22 C23 105.4(4) . . ?
C21 C22 H22 127.3 . . ?
C23 C22 H22 127.3 . . ?
N10 C23 C22 111.5(4) . . ?
N10 C23 H23 124.3 . . ?
C22 C23 H23 124.3 . . ?
N11 C24 C25 107.1(4) . . ?
N11 C24 H24 126.5 . . ?
C25 C24 H24 126.5 . . ?
C24 C25 C26 106.4(4) . . ?
C24 C25 H25 126.8 . . ?
C26 C25 H25 126.8 . . ?
N12 C26 C25 110.7(4) . . ?
N12 C26 H26 124.7 . . ?
C25 C26 H26 124.7 . . ?

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
N12 Fe1 N2 C6 83.7(3) . . . . ?
N6 Fe1 N2 C6 177.2(3) . . . . ?
N4 Fe1 N2 C6 -2.0(3) . . . . ?
N10 Fe1 N2 C6 -94.8(3) . . . . ?
N12 Fe1 N2 C7 -93.9(3) . . . . ?
N6 Fe1 N2 C7 -0.4(3) . . . . ?
N4 Fe1 N2 C7 -179.6(3) . . . . ?
N10 Fe1 N2 C7 87.5(3) . . . . ?
C8 N3 N4 C10 -0.5(5) . . . . ?
C6 N3 N4 C10 -175.5(4) . . . . ?
C8 N3 N4 Fe1 168.7(3) . . . . ?
C6 N3 N4 Fe1 -6.2(4) . . . . ?
C11 N5 N6 C13 0.6(5) . . . . ?
C7 N5 N6 C13 -179.4(4) . . . . ?
C11 N5 N6 Fe1 178.6(3) . . . . ?
C7 N5 N6 Fe1 -1.4(4) . . . . ?
C21 N9 N10 C23 1.5(5) . . . . ?
C19 N9 N10 C23 176.5(4) . . . . ?
C21 N9 N10 Fe1 178.2(3) . . . . ?
C19 N9 N10 Fe1 -6.8(4) . . . . ?
C24 N11 N12 C26 -0.1(5) . . . . ?
C20 N11 N12 C26 -178.4(4) . . . . ?
C24 N11 N12 Fe1 173.0(3) . . . . ?
C20 N11 N12 Fe1 -5.4(4) . . . . ?
C1 N1 C2 C3 177.2(7) . . . . ?
C1 N1 C2 S1 -3.0(10) . . . . ?
N1 C2 C3 C4 -14.1(7) . . . . ?
S1 C2 C3 C4 166.0(3) . . . . ?
N1 C2 C3 C5 168.3(5) . . . . ?
S1 C2 C3 C5 -11.6(6) . . . . ?
C5 C3 C4 C6 1.1(6) . . . . ?
C2 C3 C4 C6 -176.5(4) . . . . ?
C4 C3 C5 C7 -1.1(6) . . . . ?
C2 C3 C5 C7 176.5(4) . . . . ?
C7 N2 C6 C4 -3.0(6) . . . . ?
Fe1 N2 C6 C4 179.4(3) . . . . ?
C7 N2 C6 N3 176.9(3) . . . . ?
Fe1 N2 C6 N3 -0.8(4) . . . . ?
C3 C4 C6 N2 0.9(6) . . . . ?
C3 C4 C6 N3 -178.9(4) . . . . ?
C8 N3 C6 N2 -169.0(4) . . . . ?
N4 N3 C6 N2 4.7(5) . . . . ?
C8 N3 C6 C4 10.8(7) . . . . ?
N4 N3 C6 C4 -175.5(4) . . . . ?
C6 N2 C7 C5 3.0(6) . . . . ?
Fe1 N2 C7 C5 -179.3(3) . . . . ?
C6 N2 C7 N5 -177.9(3) . . . . ?
Fe1 N2 C7 N5 -0.2(4) . . . . ?
C3 C5 C7 N2 -1.0(6) . . . . ?
C3 C5 C7 N5 -180.0(4) . . . . ?
C11 N5 C7 N2 -179.0(4) . . . . ?
N6 N5 C7 N2 1.1(5) . . . . ?
C11 N5 C7 C5 0.1(7) . . . . ?
N6 N5 C7 C5 -179.9(4) . . . . ?
N4 N3 C8 C9 1.2(5) . . . . ?
C6 N3 C8 C9 175.2(4) . . . . ?
N3 C8 C9 C10 -1.4(5) . . . . ?
N3 N4 C10 C9 -0.4(5) . . . . ?
Fe1 N4 C10 C9 -164.1(4) . . . . ?
C8 C9 C10 N4 1.1(6) . . . . ?
N6 N5 C11 C12 -0.5(5) . . . . ?
C7 N5 C11 C12 179.6(4) . . . . ?
N5 C11 C12 C13 0.2(6) . . . . ?
N5 N6 C13 C12 -0.5(5) . . . . ?
Fe1 N6 C13 C12 -177.5(4) . . . . ?
C11 C12 C13 N6 0.2(6) . . . . ?
C14 N7 C15 C16 -176.3(5) . . . . ?
C14 N7 C15 S2 1.8(7) . . . . ?
N7 C15 C16 C17 -62.2(5) . . . . ?
S2 C15 C16 C17 119.6(4) . . . . ?
N7 C15 C16 C18 115.3(4) . . . . ?
S2 C15 C16 C18 -62.9(5) . . . . ?
C18 C16 C17 C19 -0.3(6) . . . . ?
C15 C16 C17 C19 177.2(4) . . . . ?
C17 C16 C18 C20 3.1(6) . . . . ?
C15 C16 C18 C20 -174.4(4) . . . . ?
C20 N8 C19 C17 1.5(6) . . . . ?
Fe1 N8 C19 C17 -173.0(3) . . . . ?
C20 N8 C19 N9 -179.3(3) . . . . ?
Fe1 N8 C19 N9 6.2(5) . . . . ?
C16 C17 C19 N8 -2.1(6) . . . . ?
C16 C17 C19 N9 178.8(4) . . . . ?
C21 N9 C19 N8 174.7(4) . . . . ?
N10 N9 C19 N8 0.9(5) . . . . ?
C21 N9 C19 C17 -6.1(7) . . . . ?
N10 N9 C19 C17 -180.0(4) . . . . ?
C19 N8 C20 C18 1.6(6) . . . . ?
Fe1 N8 C20 C18 176.2(3) . . . . ?
C19 N8 C20 N11 -177.3(3) . . . . ?
Fe1 N8 C20 N11 -2.8(5) . . . . ?
C16 C18 C20 N8 -3.8(6) . . . . ?
C16 C18 C20 N11 175.0(4) . . . . ?
C24 N11 C20 N8 -172.6(5) . . . . ?
N12 N11 C20 N8 5.3(5) . . . . ?
C24 N11 C20 C18 8.5(8) . . . . ?
N12 N11 C20 C18 -173.6(4) . . . . ?
N10 N9 C21 C22 -1.4(5) . . . . ?
C19 N9 C21 C22 -175.5(4) . . . . ?
N9 C21 C22 C23 0.7(6) . . . . ?
N9 N10 C23 C22 -1.0(5) . . . . ?
Fe1 N10 C23 C22 -175.9(4) . . . . ?
C21 C22 C23 N10 0.2(6) . . . . ?
N12 N11 C24 C25 -0.6(5) . . . . ?
C20 N11 C24 C25 177.4(5) . . . . ?
N11 C24 C25 C26 0.9(6) . . . . ?
N11 N12 C26 C25 0.6(5) . . . . ?
Fe1 N12 C26 C25 -168.9(4) . . . . ?
C24 C25 C26 N12 -1.0(6) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1 O2 . . 2_675 2.882(9) 0.879 2.023 165.2 no
N7 H7 O8 . . 1_545 3.068(9) 0.860 2.291 150.4 no

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


####################################################################### 
# 
# 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_M171019A
_database_code_depnum_ccdc_archive 'CCDC 1860679'
_audit_update_record             
;
2018-09-05 deposited with the CCDC.
2018-11-09 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C27 H27 B2 F8 Fe N13 O2 S2'
_chemical_formula_moiety         '2(C13 H12 N6 S) Fe, 2(B F4), C H3 N O2'
_chemical_formula_weight         859.17
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
_space_group_IT_number           14
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 +X,-1/2-Y,-1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   8.2211(3)
_cell_length_b                   40.8700(18)
_cell_length_c                   10.7721(4)
_cell_angle_alpha                90.0000
_cell_angle_beta                 94.349(7)
_cell_angle_gamma                90.0000
_cell_volume                     3608.9(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    27248
_cell_measurement_theta_min      1.90
_cell_measurement_theta_max      27.47
_cell_measurement_temperature    290
#------------------------------------------------------------------------------
_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.250
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1744.00
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.218
_exptl_absorpt_correction_T_max  0.856

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      290
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            32472
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_theta_max         27.472
_diffrn_reflns_theta_min         2.142
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             8119
_reflns_number_gt                6106
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
    Four reflections, -3 8 4, 5 4 2, -6 5 1 and -5 5 5, have been omitted from 
the least square calculations because of large differences between each Fo and 
Fc, which probably caused by a measurement error of the IP system. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0773
_refine_ls_wR_factor_ref         0.2351
_refine_ls_wR_factor_gt          0.2155
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         8119
_refine_ls_number_parameters     496
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.1083P)²+10.5529P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         1.23
_refine_diff_density_min         -0.80
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Fe Fe 0.3463 0.8444
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
B B 0.0013 0.0007
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
F F 0.0171 0.0103
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.33297(8) 0.11514(2) 0.29650(6) 0.03358(19) Uani 1 1 d . . . . .
S1 S 0.5267(2) 0.27726(3) 0.49887(14) 0.0658(5) Uani 1 1 d . . . . .
S2 S 0.3772(2) -0.05765(3) 0.32906(15) 0.0684(5) Uani 1 1 d . . . . .
F1 F 0.0663(11) 0.24440(12) 0.6005(6) 0.185(4) Uani 1 1 d . . . . .
F2 F -0.0301(5) 0.22230(11) 0.4216(4) 0.0826(11) Uani 1 1 d . . . . .
F3 F -0.1088(10) 0.2058(2) 0.5989(6) 0.193(4) Uani 1 1 d . . . . .
F4 F 0.1288(12) 0.19456(18) 0.5598(7) 0.202(4) Uani 1 1 d . . . . .
F5 F -0.3107(8) 0.0379(2) 0.1505(8) 0.201(4) Uani 1 1 d . . . . .
F6 F -0.0647(8) 0.0344(4) 0.1561(12) 0.318(9) Uani 1 1 d . . . . .
F7 F -0.1695(9) 0.01526(15) 0.3145(5) 0.137(2) Uani 1 1 d . . . . .
F8 F -0.180(2) -0.0061(3) 0.1377(9) 0.289(8) Uani 1 1 d . . . . .
O1 O 0.1227(10) 0.15164(19) -0.1322(10) 0.155(4) Uani 1 1 d . . . . .
O2 O -0.1269(9) 0.15426(15) -0.1681(8) 0.133(3) Uani 1 1 d . . . . .
N1 N 0.4733(6) 0.27723(10) 0.2529(4) 0.0576(12) Uani 1 1 d . . . . .
H1 H 0.451358 0.266194 0.185748 0.069 Uiso 1 1 calc R U . . .
N2 N 0.3782(4) 0.16029(8) 0.3192(3) 0.0346(7) Uani 1 1 d . . . . .
N3 N 0.1204(5) 0.16742(8) 0.2355(4) 0.0393(8) Uani 1 1 d . . . . .
N4 N 0.1194(5) 0.13358(8) 0.2347(4) 0.0397(8) Uani 1 1 d . . . . .
N5 N 0.6226(4) 0.14284(9) 0.4010(4) 0.0391(8) Uani 1 1 d . . . . .
N6 N 0.5609(5) 0.11274(8) 0.3644(3) 0.0373(8) Uani 1 1 d . . . . .
N7 N 0.1580(6) -0.04216(10) 0.1451(5) 0.0605(12) Uani 1 1 d . . . . .
H7 H 0.107903 -0.027050 0.101739 0.073 Uiso 1 1 calc R U . . .
N8 N 0.3012(4) 0.06946(8) 0.2767(3) 0.0351(7) Uani 1 1 d . . . . .
N9 N 0.2404(5) 0.07088(9) 0.4769(4) 0.0405(8) Uani 1 1 d . . . . .
N10 N 0.2609(5) 0.10409(9) 0.4614(4) 0.0385(8) Uani 1 1 d . . . . .
N11 N 0.3773(5) 0.07822(8) 0.0829(4) 0.0390(8) Uani 1 1 d . . . . .
N12 N 0.3921(5) 0.11007(8) 0.1237(3) 0.0364(8) Uani 1 1 d . . . . .
N13 N 0.0019(10) 0.16703(14) -0.1406(6) 0.0826(17) Uani 1 1 d . . . . .
C1 C 0.4974(10) 0.31233(13) 0.2413(7) 0.075(2) Uani 1 1 d . . . . .
H1A H 0.484573 0.318418 0.155014 0.090 Uiso 1 1 calc R U . . .
H1B H 0.418360 0.323736 0.286213 0.090 Uiso 1 1 calc R U . . .
H1C H 0.605200 0.317995 0.274914 0.090 Uiso 1 1 calc R U . . .
C2 C 0.4826(6) 0.26115(11) 0.3595(5) 0.0460(11) Uani 1 1 d . . . . .
C3 C 0.4464(6) 0.22545(10) 0.3455(4) 0.0412(10) Uani 1 1 d . . . . .
C4 C 0.2954(6) 0.21567(10) 0.2908(4) 0.0421(10) Uani 1 1 d . . . . .
H4 H 0.217954 0.230926 0.261180 0.051 Uiso 1 1 calc R U . . .
C5 C 0.5647(6) 0.20239(11) 0.3887(4) 0.0416(10) Uani 1 1 d . . . . .
H5 H 0.665235 0.208676 0.426521 0.050 Uiso 1 1 calc R U . . .
C6 C 0.2648(5) 0.18267(10) 0.2821(4) 0.0368(9) Uani 1 1 d . . . . .
C7 C 0.5230(5) 0.17002(10) 0.3716(4) 0.0381(9) Uani 1 1 d . . . . .
C8 C -0.0250(6) 0.17959(12) 0.1894(5) 0.0478(11) Uani 1 1 d . . . . .
H8 H -0.054094 0.201540 0.182414 0.057 Uiso 1 1 calc R U . . .
C9 C -0.1209(6) 0.15318(14) 0.1551(5) 0.0525(12) Uani 1 1 d . . . . .
H9 H -0.226943 0.153617 0.118291 0.063 Uiso 1 1 calc R U . . .
C10 C -0.0276(6) 0.12560(12) 0.1866(5) 0.0473(11) Uani 1 1 d . . . . .
H10 H -0.064320 0.104211 0.175240 0.057 Uiso 1 1 calc R U . . .
C11 C 0.7749(6) 0.13965(13) 0.4579(5) 0.0516(12) Uani 1 1 d . . . . .
H11 H 0.841087 0.156399 0.491341 0.062 Uiso 1 1 calc R U . . .
C12 C 0.8116(6) 0.10749(13) 0.4563(6) 0.0543(13) Uani 1 1 d . . . . .
H12 H 0.908547 0.097824 0.487835 0.065 Uiso 1 1 calc R U . . .
C13 C 0.6766(6) 0.09154(11) 0.3985(5) 0.0441(10) Uani 1 1 d . . . . .
H13 H 0.669111 0.069068 0.385729 0.053 Uiso 1 1 calc R U . . .
C14 C 0.1230(9) -0.07585(14) 0.1106(7) 0.0747(19) Uani 1 1 d . . . . .
H14A H 0.044201 -0.076390 0.040135 0.090 Uiso 1 1 calc R U . . .
H14B H 0.221463 -0.086420 0.089570 0.090 Uiso 1 1 calc R U . . .
H14C H 0.080032 -0.087060 0.179312 0.090 Uiso 1 1 calc R U . . .
C15 C 0.2610(6) -0.03310(10) 0.2381(5) 0.0458(11) Uani 1 1 d . . . . .
C16 C 0.2779(6) 0.00313(10) 0.2527(5) 0.0402(10) Uani 1 1 d . . . . .
C17 C 0.2550(6) 0.01747(10) 0.3672(5) 0.0428(10) Uani 1 1 d . . . . .
H17 H 0.233604 0.004967 0.436261 0.051 Uiso 1 1 calc R U . . .
C18 C 0.3151(6) 0.02188(10) 0.1507(4) 0.0404(10) Uani 1 1 d . . . . .
H18 H 0.329246 0.012407 0.073749 0.048 Uiso 1 1 calc R U . . .
C19 C 0.2656(6) 0.05108(10) 0.3735(4) 0.0382(9) Uani 1 1 d . . . . .
C20 C 0.3300(5) 0.05520(10) 0.1692(4) 0.0364(9) Uani 1 1 d . . . . .
C21 C 0.2001(6) 0.06384(13) 0.5934(4) 0.0472(11) Uani 1 1 d . . . . .
H21 H 0.182018 0.043146 0.625487 0.057 Uiso 1 1 calc R U . . .
C22 C 0.1913(7) 0.09304(14) 0.6551(5) 0.0519(12) Uani 1 1 d . . . . .
H22 H 0.165662 0.096175 0.736893 0.062 Uiso 1 1 calc R U . . .
C23 C 0.2286(6) 0.11715(12) 0.5696(5) 0.0451(11) Uani 1 1 d . . . . .
H23 H 0.230598 0.139472 0.586493 0.054 Uiso 1 1 calc R U . . .
C24 C 0.4168(7) 0.07548(12) -0.0362(4) 0.0470(11) Uani 1 1 d . . . . .
H24 H 0.414044 0.056441 -0.083631 0.056 Uiso 1 1 calc R U . . .
C25 C 0.4617(7) 0.10596(13) -0.0741(5) 0.0522(12) Uani 1 1 d . . . . .
H25 H 0.497175 0.111712 -0.151130 0.063 Uiso 1 1 calc R U . . .
C26 C 0.4429(6) 0.12658(11) 0.0272(4) 0.0427(10) Uani 1 1 d . . . . .
H26 H 0.463231 0.148962 0.027319 0.051 Uiso 1 1 calc R U . . .
C27 C 0.0034(13) 0.20206(17) -0.1194(7) 0.097(3) Uani 1 1 d . . . . .
H27A H -0.105972 0.210375 -0.130323 0.116 Uiso 1 1 calc R U . . .
H27B H 0.047739 0.206530 -0.036080 0.116 Uiso 1 1 calc R U . . .
H27C H 0.069409 0.212477 -0.177649 0.116 Uiso 1 1 calc R U . . .
B1 B 0.0257(9) 0.21813(16) 0.5445(6) 0.0581(15) Uani 1 1 d . . . . .
B2 B -0.1903(10) 0.02078(18) 0.1914(8) 0.0660(18) Uani 1 1 d . . . . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_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 N8 1.895(3) . ?
Fe1 N2 1.894(3) . ?
Fe1 N6 1.962(4) . ?
Fe1 N10 1.967(4) . ?
Fe1 N12 1.971(4) . ?
Fe1 N4 1.979(4) . ?
S1 C2 1.654(5) . ?
S2 C15 1.655(5) . ?
F1 B1 1.264(8) . ?
F2 B1 1.379(8) . ?
F3 B1 1.385(10) . ?
F4 B1 1.286(9) . ?
F5 B2 1.265(9) . ?
F6 B2 1.256(10) . ?
F7 B2 1.343(9) . ?
F8 B2 1.246(10) . ?
O1 N13 1.173(9) . ?
O2 N13 1.197(9) . ?
N1 C2 1.320(7) . ?
N1 C1 1.455(6) . ?
N1 H1 0.8600 . ?
N2 C7 1.339(6) . ?
N2 C6 1.345(5) . ?
N3 C8 1.354(6) . ?
N3 N4 1.383(5) . ?
N3 C6 1.400(5) . ?
N4 C10 1.319(6) . ?
N5 C11 1.358(6) . ?
N5 N6 1.377(5) . ?
N5 C7 1.402(5) . ?
N6 C13 1.318(6) . ?
N7 C15 1.315(7) . ?
N7 C14 1.449(6) . ?
N7 H7 0.8600 . ?
N8 C20 1.333(6) . ?
N8 C19 1.336(6) . ?
N9 C21 1.353(6) . ?
N9 N10 1.379(5) . ?
N9 C19 1.404(6) . ?
N10 C23 1.327(6) . ?
N11 C24 1.352(6) . ?
N11 N12 1.376(5) . ?
N11 C20 1.398(6) . ?
N12 C26 1.332(6) . ?
N13 C27 1.450(8) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.494(6) . ?
C3 C4 1.392(6) . ?
C3 C5 1.408(6) . ?
C4 C6 1.374(6) . ?
C4 H4 0.9300 . ?
C5 C7 1.375(6) . ?
C5 H5 0.9300 . ?
C8 C9 1.371(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.391(7) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.349(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.393(7) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.494(6) . ?
C16 C17 1.392(7) . ?
C16 C18 1.392(7) . ?
C17 C19 1.378(6) . ?
C17 H17 0.9300 . ?
C18 C20 1.380(6) . ?
C18 H18 0.9300 . ?
C21 C22 1.371(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.398(8) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 C25 1.370(7) . ?
C24 H24 0.9300 . ?
C25 C26 1.397(7) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?

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
N8 Fe1 N2 176.53(15) . . ?
N8 Fe1 N6 96.44(15) . . ?
N2 Fe1 N6 80.11(14) . . ?
N8 Fe1 N10 80.04(15) . . ?
N2 Fe1 N10 100.19(15) . . ?
N6 Fe1 N10 89.81(16) . . ?
N8 Fe1 N12 80.31(15) . . ?
N2 Fe1 N12 99.46(15) . . ?
N6 Fe1 N12 92.84(16) . . ?
N10 Fe1 N12 160.34(15) . . ?
N8 Fe1 N4 103.06(15) . . ?
N2 Fe1 N4 80.39(15) . . ?
N6 Fe1 N4 160.49(14) . . ?
N10 Fe1 N4 94.06(16) . . ?
N12 Fe1 N4 89.92(16) . . ?
C2 N1 C1 124.5(5) . . ?
C2 N1 H1 117.7 . . ?
C1 N1 H1 117.7 . . ?
C7 N2 C6 119.8(4) . . ?
C7 N2 Fe1 120.2(3) . . ?
C6 N2 Fe1 120.0(3) . . ?
C8 N3 N4 111.1(4) . . ?
C8 N3 C6 132.0(4) . . ?
N4 N3 C6 116.9(3) . . ?
C10 N4 N3 104.8(4) . . ?
C10 N4 Fe1 143.2(3) . . ?
N3 N4 Fe1 111.9(3) . . ?
C11 N5 N6 110.5(4) . . ?
C11 N5 C7 132.9(4) . . ?
N6 N5 C7 116.6(3) . . ?
C13 N6 N5 105.4(4) . . ?
C13 N6 Fe1 141.8(3) . . ?
N5 N6 Fe1 112.5(3) . . ?
C15 N7 C14 124.5(5) . . ?
C15 N7 H7 117.7 . . ?
C14 N7 H7 117.7 . . ?
C20 N8 C19 119.8(4) . . ?
C20 N8 Fe1 119.8(3) . . ?
C19 N8 Fe1 120.2(3) . . ?
C21 N9 N10 111.2(4) . . ?
C21 N9 C19 132.4(4) . . ?
N10 N9 C19 116.4(4) . . ?
C23 N10 N9 104.8(4) . . ?
C23 N10 Fe1 142.6(3) . . ?
N9 N10 Fe1 112.5(3) . . ?
C24 N11 N12 111.0(4) . . ?
C24 N11 C20 132.4(4) . . ?
N12 N11 C20 116.6(4) . . ?
C26 N12 N11 104.8(4) . . ?
C26 N12 Fe1 142.9(3) . . ?
N11 N12 Fe1 112.2(3) . . ?
O1 N13 O2 120.8(8) . . ?
O1 N13 C27 121.4(9) . . ?
O2 N13 C27 117.8(8) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 113.6(4) . . ?
N1 C2 S1 125.8(4) . . ?
C3 C2 S1 120.6(4) . . ?
C4 C3 C5 121.3(4) . . ?
C4 C3 C2 119.2(4) . . ?
C5 C3 C2 119.5(4) . . ?
C6 C4 C3 117.6(4) . . ?
C6 C4 H4 121.2 . . ?
C3 C4 H4 121.2 . . ?
C7 C5 C3 116.2(4) . . ?
C7 C5 H5 121.9 . . ?
C3 C5 H5 121.9 . . ?
N2 C6 C4 121.9(4) . . ?
N2 C6 N3 110.7(4) . . ?
C4 C6 N3 127.4(4) . . ?
N2 C7 C5 123.1(4) . . ?
N2 C7 N5 110.2(4) . . ?
C5 C7 N5 126.6(4) . . ?
N3 C8 C9 106.5(4) . . ?
N3 C8 H8 126.8 . . ?
C9 C8 H8 126.8 . . ?
C8 C9 C10 106.1(4) . . ?
C8 C9 H9 127.0 . . ?
C10 C9 H9 127.0 . . ?
N4 C10 C9 111.6(4) . . ?
N4 C10 H10 124.2 . . ?
C9 C10 H10 124.2 . . ?
C12 C11 N5 106.7(4) . . ?
C12 C11 H11 126.6 . . ?
N5 C11 H11 126.6 . . ?
C11 C12 C13 106.8(4) . . ?
C11 C12 H12 126.6 . . ?
C13 C12 H12 126.6 . . ?
N6 C13 C12 110.5(4) . . ?
N6 C13 H13 124.7 . . ?
C12 C13 H13 124.7 . . ?
N7 C14 H14A 109.5 . . ?
N7 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N7 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N7 C15 C16 114.1(4) . . ?
N7 C15 S2 126.1(4) . . ?
C16 C15 S2 119.6(4) . . ?
C17 C16 C18 121.4(4) . . ?
C17 C16 C15 119.5(4) . . ?
C18 C16 C15 119.1(4) . . ?
C19 C17 C16 116.8(4) . . ?
C19 C17 H17 121.6 . . ?
C16 C17 H17 121.6 . . ?
C20 C18 C16 116.8(4) . . ?
C20 C18 H18 121.6 . . ?
C16 C18 H18 121.6 . . ?
N8 C19 C17 122.6(4) . . ?
N8 C19 N9 110.4(4) . . ?
C17 C19 N9 126.9(4) . . ?
N8 C20 C18 122.5(4) . . ?
N8 C20 N11 111.1(3) . . ?
C18 C20 N11 126.4(4) . . ?
N9 C21 C22 106.9(4) . . ?
N9 C21 H21 126.6 . . ?
C22 C21 H21 126.6 . . ?
C21 C22 C23 105.8(5) . . ?
C21 C22 H22 127.1 . . ?
C23 C22 H22 127.1 . . ?
N10 C23 C22 111.3(4) . . ?
N10 C23 H23 124.3 . . ?
C22 C23 H23 124.3 . . ?
N11 C24 C25 107.3(4) . . ?
N11 C24 H24 126.4 . . ?
C25 C24 H24 126.4 . . ?
C24 C25 C26 105.5(4) . . ?
C24 C25 H25 127.2 . . ?
C26 C25 H25 127.2 . . ?
N12 C26 C25 111.3(4) . . ?
N12 C26 H26 124.3 . . ?
C25 C26 H26 124.3 . . ?
N13 C27 H27A 109.5 . . ?
N13 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N13 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
F1 B1 F4 115.3(8) . . ?
F1 B1 F2 114.2(6) . . ?
F4 B1 F2 112.6(6) . . ?
F1 B1 F3 107.2(8) . . ?
F4 B1 F3 102.3(8) . . ?
F2 B1 F3 103.5(6) . . ?
F8 B2 F6 99.4(12) . . ?
F8 B2 F5 113.8(10) . . ?
F6 B2 F5 106.8(8) . . ?
F8 B2 F7 107.6(8) . . ?
F6 B2 F7 109.1(9) . . ?
F5 B2 F7 118.4(8) . . ?

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
N6 Fe1 N2 C7 -3.6(4) . . . . ?
N10 Fe1 N2 C7 84.4(4) . . . . ?
N12 Fe1 N2 C7 -94.8(4) . . . . ?
N4 Fe1 N2 C7 176.9(4) . . . . ?
N6 Fe1 N2 C6 176.2(4) . . . . ?
N10 Fe1 N2 C6 -95.8(3) . . . . ?
N12 Fe1 N2 C6 84.9(4) . . . . ?
N4 Fe1 N2 C6 -3.4(3) . . . . ?
C8 N3 N4 C10 0.5(5) . . . . ?
C6 N3 N4 C10 -179.7(4) . . . . ?
C8 N3 N4 Fe1 178.1(3) . . . . ?
C6 N3 N4 Fe1 -2.1(5) . . . . ?
C11 N5 N6 C13 -0.4(5) . . . . ?
C7 N5 N6 C13 178.2(4) . . . . ?
C11 N5 N6 Fe1 174.3(3) . . . . ?
C7 N5 N6 Fe1 -7.1(5) . . . . ?
N6 Fe1 N8 C20 -91.2(3) . . . . ?
N10 Fe1 N8 C20 -179.9(4) . . . . ?
N12 Fe1 N8 C20 0.6(3) . . . . ?
N4 Fe1 N8 C20 88.2(4) . . . . ?
N6 Fe1 N8 C19 82.2(4) . . . . ?
N10 Fe1 N8 C19 -6.4(3) . . . . ?
N12 Fe1 N8 C19 174.0(4) . . . . ?
N4 Fe1 N8 C19 -98.3(4) . . . . ?
C21 N9 N10 C23 -1.4(5) . . . . ?
C19 N9 N10 C23 179.2(4) . . . . ?
C21 N9 N10 Fe1 176.4(3) . . . . ?
C19 N9 N10 Fe1 -2.9(5) . . . . ?
C24 N11 N12 C26 -0.5(5) . . . . ?
C20 N11 N12 C26 178.0(4) . . . . ?
C24 N11 N12 Fe1 179.3(3) . . . . ?
C20 N11 N12 Fe1 -2.2(5) . . . . ?
C1 N1 C2 C3 177.8(6) . . . . ?
C1 N1 C2 S1 -1.3(9) . . . . ?
N1 C2 C3 C4 -59.0(7) . . . . ?
S1 C2 C3 C4 120.1(5) . . . . ?
N1 C2 C3 C5 121.5(5) . . . . ?
S1 C2 C3 C5 -59.3(6) . . . . ?
C5 C3 C4 C6 1.0(7) . . . . ?
C2 C3 C4 C6 -178.5(4) . . . . ?
C4 C3 C5 C7 1.0(7) . . . . ?
C2 C3 C5 C7 -179.5(4) . . . . ?
C7 N2 C6 C4 3.3(7) . . . . ?
Fe1 N2 C6 C4 -176.5(4) . . . . ?
C7 N2 C6 N3 -177.2(4) . . . . ?
Fe1 N2 C6 N3 3.0(5) . . . . ?
C3 C4 C6 N2 -3.2(7) . . . . ?
C3 C4 C6 N3 177.3(5) . . . . ?
C8 N3 C6 N2 179.3(5) . . . . ?
N4 N3 C6 N2 -0.4(6) . . . . ?
C8 N3 C6 C4 -1.2(9) . . . . ?
N4 N3 C6 C4 179.1(5) . . . . ?
C6 N2 C7 C5 -1.0(7) . . . . ?
Fe1 N2 C7 C5 178.8(4) . . . . ?
C6 N2 C7 N5 -179.1(4) . . . . ?
Fe1 N2 C7 N5 0.7(5) . . . . ?
C3 C5 C7 N2 -1.1(7) . . . . ?
C3 C5 C7 N5 176.7(5) . . . . ?
C11 N5 C7 N2 -177.5(5) . . . . ?
N6 N5 C7 N2 4.3(6) . . . . ?
C11 N5 C7 C5 4.5(9) . . . . ?
N6 N5 C7 C5 -173.7(5) . . . . ?
N4 N3 C8 C9 -1.5(6) . . . . ?
C6 N3 C8 C9 178.8(5) . . . . ?
N3 C8 C9 C10 1.8(6) . . . . ?
N3 N4 C10 C9 0.7(6) . . . . ?
Fe1 N4 C10 C9 -175.6(4) . . . . ?
C8 C9 C10 N4 -1.6(6) . . . . ?
N6 N5 C11 C12 0.7(6) . . . . ?
C7 N5 C11 C12 -177.5(5) . . . . ?
N5 C11 C12 C13 -0.7(6) . . . . ?
N5 N6 C13 C12 -0.1(6) . . . . ?
Fe1 N6 C13 C12 -172.1(4) . . . . ?
C11 C12 C13 N6 0.5(7) . . . . ?
C14 N7 C15 C16 178.8(5) . . . . ?
C14 N7 C15 S2 3.3(9) . . . . ?
N7 C15 C16 C17 126.3(5) . . . . ?
S2 C15 C16 C17 -57.9(6) . . . . ?
N7 C15 C16 C18 -53.2(7) . . . . ?
S2 C15 C16 C18 122.6(5) . . . . ?
C18 C16 C17 C19 2.1(7) . . . . ?
C15 C16 C17 C19 -177.4(4) . . . . ?
C17 C16 C18 C20 0.8(7) . . . . ?
C15 C16 C18 C20 -179.8(4) . . . . ?
C20 N8 C19 C17 -0.8(7) . . . . ?
Fe1 N8 C19 C17 -174.3(4) . . . . ?
C20 N8 C19 N9 179.8(4) . . . . ?
Fe1 N8 C19 N9 6.4(5) . . . . ?
C16 C17 C19 N8 -2.1(7) . . . . ?
C16 C17 C19 N9 177.1(4) . . . . ?
C21 N9 C19 N8 179.0(5) . . . . ?
N10 N9 C19 N8 -1.9(6) . . . . ?
C21 N9 C19 C17 -0.3(8) . . . . ?
N10 N9 C19 C17 178.8(4) . . . . ?
C19 N8 C20 C18 4.0(7) . . . . ?
Fe1 N8 C20 C18 177.5(3) . . . . ?
C19 N8 C20 N11 -175.3(4) . . . . ?
Fe1 N8 C20 N11 -1.8(5) . . . . ?
C16 C18 C20 N8 -3.9(7) . . . . ?
C16 C18 C20 N11 175.3(4) . . . . ?
C24 N11 C20 N8 -179.3(5) . . . . ?
N12 N11 C20 N8 2.6(6) . . . . ?
C24 N11 C20 C18 1.4(8) . . . . ?
N12 N11 C20 C18 -176.7(4) . . . . ?
N10 N9 C21 C22 1.1(6) . . . . ?
C19 N9 C21 C22 -179.7(5) . . . . ?
N9 C21 C22 C23 -0.2(6) . . . . ?
N9 N10 C23 C22 1.3(5) . . . . ?
Fe1 N10 C23 C22 -175.4(4) . . . . ?
C21 C22 C23 N10 -0.7(6) . . . . ?
N12 N11 C24 C25 1.2(6) . . . . ?
C20 N11 C24 C25 -177.0(5) . . . . ?
N11 C24 C25 C26 -1.3(6) . . . . ?
N11 N12 C26 C25 -0.3(5) . . . . ?
Fe1 N12 C26 C25 179.9(4) . . . . ?
C24 C25 C26 N12 1.0(6) . . . . ?


#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


