# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2015

####################################################################### 
# 
# 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_lkc258
_database_code_depnum_ccdc_archive 'CCDC 1060840'
_audit_update_record             
;
2015-04-21 deposited with the CCDC.
2015-06-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
[2,6-Di(pyrazol-1-yl)pyrid-4-yl]methylsulfone 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H11 N5 O2 S'
_chemical_formula_sum            'C12 H11 N5 O2 S'
_chemical_formula_weight         289.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   5.63390(10)
_cell_length_b                   14.1865(4)
_cell_length_c                   16.1192(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.402(2)
_cell_angle_gamma                90.00
_cell_volume                     1287.95(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2498
_cell_measurement_theta_min      4.14
_cell_measurement_theta_max      73.41

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             600
_exptl_absorpt_coefficient_mu    2.338
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.896
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            4740
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         4.15
_diffrn_reflns_theta_max         73.70
_reflns_number_total             2515
_reflns_number_gt                2160
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 No disorder is present in the model, and no restraints were applied. All 
 non-H atoms are refined anisotropically, while H atoms were placed in 
 calculated positions and refined using a riding model.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0454P)²+0.2286P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2515
_refine_ls_number_parameters     182
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0360
_refine_ls_wR_factor_ref         0.0925
_refine_ls_wR_factor_gt          0.0877
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.4858(3) 0.69378(10) 0.30987(9) 0.0201(3) Uani 1 1 d . . .
C2 C 0.2928(3) 0.64102(12) 0.31645(10) 0.0196(3) Uani 1 1 d . . .
C3 C 0.1835(3) 0.62015(12) 0.39085(11) 0.0203(3) Uani 1 1 d . . .
H3 H 0.0461 0.5815 0.3930 0.024 Uiso 1 1 calc R . .
C4 C 0.2878(3) 0.65924(12) 0.46122(10) 0.0197(3) Uani 1 1 d . . .
C5 C 0.4877(3) 0.71536(12) 0.45835(10) 0.0202(3) Uani 1 1 d . . .
H5 H 0.5593 0.7421 0.5069 0.024 Uiso 1 1 calc R . .
C6 C 0.5777(3) 0.73024(12) 0.37971(10) 0.0195(3) Uani 1 1 d . . .
N7 N 0.1942(3) 0.60699(11) 0.24095(9) 0.0206(3) Uani 1 1 d . . .
N8 N -0.0045(3) 0.55191(12) 0.24130(9) 0.0257(3) Uani 1 1 d . . .
C9 C -0.0582(4) 0.53837(14) 0.16168(11) 0.0271(4) Uani 1 1 d . . .
H9 H -0.1893 0.5020 0.1419 0.032 Uiso 1 1 calc R . .
C10 C 0.1035(4) 0.58464(13) 0.10987(11) 0.0262(4) Uani 1 1 d . . .
H10 H 0.1019 0.5851 0.0509 0.031 Uiso 1 1 calc R . .
C11 C 0.2619(3) 0.62838(13) 0.16201(11) 0.0235(4) Uani 1 1 d . . .
H11 H 0.3931 0.6661 0.1468 0.028 Uiso 1 1 calc R . .
N12 N 0.7765(3) 0.78841(11) 0.36997(9) 0.0212(3) Uani 1 1 d . . .
N13 N 0.8782(3) 0.83181(11) 0.43760(9) 0.0253(3) Uani 1 1 d . . .
C14 C 1.0578(3) 0.87899(14) 0.40707(12) 0.0276(4) Uani 1 1 d . . .
H14 H 1.1637 0.9167 0.4396 0.033 Uiso 1 1 calc R . .
C15 C 1.0748(3) 0.86708(13) 0.32067(12) 0.0278(4) Uani 1 1 d . . .
H15 H 1.1893 0.8939 0.2854 0.033 Uiso 1 1 calc R . .
C16 C 0.8916(3) 0.80886(13) 0.29859(11) 0.0245(4) Uani 1 1 d . . .
H16 H 0.8519 0.7869 0.2443 0.029 Uiso 1 1 calc R . .
S17 S 0.16094(7) 0.63715(3) 0.55967(2) 0.01986(13) Uani 1 1 d . . .
O18 O -0.0755(2) 0.60109(10) 0.54580(8) 0.0260(3) Uani 1 1 d . . .
O19 O 0.1943(3) 0.72059(9) 0.60941(8) 0.0282(3) Uani 1 1 d . . .
C20 C 0.3429(3) 0.54637(13) 0.60082(11) 0.0232(4) Uani 1 1 d . . .
H20A H 0.5074 0.5686 0.6055 0.035 Uiso 1 1 calc R . .
H20B H 0.3346 0.4915 0.5640 0.035 Uiso 1 1 calc R . .
H20C H 0.2878 0.5287 0.6559 0.035 Uiso 1 1 calc R . .


_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
N1 C2 1.326(2) . ?
N1 C6 1.332(2) . ?
C2 C3 1.393(2) . ?
C2 N7 1.411(2) . ?
C3 C4 1.381(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.381(3) . ?
C4 S17 1.7839(17) . ?
C5 C6 1.393(2) . ?
C5 H5 0.9500 . ?
C6 N12 1.403(2) . ?
N7 N8 1.366(2) . ?
N7 C11 1.371(2) . ?
N8 C9 1.325(2) . ?
C9 C10 1.412(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.361(3) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
N12 C16 1.366(2) . ?
N12 N13 1.366(2) . ?
N13 C14 1.319(3) . ?
C14 C15 1.408(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.362(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
S17 O18 1.4393(14) . ?
S17 O19 1.4394(14) . ?
S17 C20 1.7655(18) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 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
C2 N1 C6 117.00(15) . . ?
N1 C2 C3 124.70(16) . . ?
N1 C2 N7 115.49(15) . . ?
C3 C2 N7 119.79(16) . . ?
C4 C3 C2 115.70(16) . . ?
C4 C3 H3 122.2 . . ?
C2 C3 H3 122.2 . . ?
C3 C4 C5 122.34(16) . . ?
C3 C4 S17 119.25(14) . . ?
C5 C4 S17 118.42(13) . . ?
C4 C5 C6 115.67(16) . . ?
C4 C5 H5 122.2 . . ?
C6 C5 H5 122.2 . . ?
N1 C6 C5 124.59(16) . . ?
N1 C6 N12 115.38(15) . . ?
C5 C6 N12 120.02(16) . . ?
N8 N7 C11 112.15(14) . . ?
N8 N7 C2 119.87(14) . . ?
C11 N7 C2 127.76(15) . . ?
C9 N8 N7 104.27(15) . . ?
N8 C9 C10 111.73(17) . . ?
N8 C9 H9 124.1 . . ?
C10 C9 H9 124.1 . . ?
C11 C10 C9 105.63(16) . . ?
C11 C10 H10 127.2 . . ?
C9 C10 H10 127.2 . . ?
C10 C11 N7 106.21(16) . . ?
C10 C11 H11 126.9 . . ?
N7 C11 H11 126.9 . . ?
C16 N12 N13 112.23(15) . . ?
C16 N12 C6 128.02(15) . . ?
N13 N12 C6 119.74(14) . . ?
C14 N13 N12 103.98(15) . . ?
N13 C14 C15 112.29(17) . . ?
N13 C14 H14 123.9 . . ?
C15 C14 H14 123.9 . . ?
C16 C15 C14 105.19(17) . . ?
C16 C15 H15 127.4 . . ?
C14 C15 H15 127.4 . . ?
C15 C16 N12 106.31(17) . . ?
C15 C16 H16 126.8 . . ?
N12 C16 H16 126.8 . . ?
O18 S17 O19 119.11(8) . . ?
O18 S17 C20 109.02(8) . . ?
O19 S17 C20 108.90(9) . . ?
O18 S17 C4 108.28(8) . . ?
O19 S17 C4 107.54(8) . . ?
C20 S17 C4 102.75(8) . . ?
S17 C20 H20A 109.5 . . ?
S17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
S17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.970
_diffrn_reflns_theta_full        73.70
_diffrn_measured_fraction_theta_full 0.970
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.056
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: chloroform/pentane'
####################################################################### 
# 
# 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_lkc266rt
_database_code_depnum_ccdc_archive 'CCDC 1060841'
_audit_update_record             
;
2015-04-21 deposited with the CCDC.
2015-06-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
Bis[2,6-di(pyrazol-1-yl)4-methylsulfanylpyridine]iron(II)diperchlorate
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H22 Fe N10 S2, 2[Cl O4]'
_chemical_formula_sum            'C24 H22 Cl2 Fe N10 O8 S2'
_chemical_formula_weight         769.39

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'
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'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P b c n'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'

_cell_length_a                   54.8011(19)
_cell_length_b                   10.6074(3)
_cell_length_c                   16.3787(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     9520.9(5)
_cell_formula_units_Z            12
_cell_measurement_temperature    280(2)
_cell_measurement_reflns_used    3879
_cell_measurement_theta_min      4.18
_cell_measurement_theta_max      73.64

_exptl_crystal_description       fragment
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4704
_exptl_absorpt_coefficient_mu    7.153
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.544
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28e (release 10-06-2013 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      280(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            22818
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_min       -61
_diffrn_reflns_limit_h_max       66
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         4.25
_diffrn_reflns_theta_max         73.73
_reflns_number_total             9301
_reflns_number_gt                6320
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The asymmetric unit contains 1.5 formula units, with half a complex cation 
 spanning the C₂ axis 1/2, y, 3/4 (molecule A); and, a whole complex dication 
 (molecule B) and three unique BF₄⁻ anions lying on general crystallographic 
 sites. All three anions are disordered, over three sites with occupancies of
 0.40:0.30:0.30, that share a common wholly occupied Cl atom (Cl48-O52); or, 
 over two sites with refined occupancies close to 0.6:0.4 (Cl38-O42 and 
 Cl43-O47). The refined restraints Cl---O = 1.42(2) and O...O = 2.32(2) Å 
 were applied to these residues. 

 All wholly occupied non-H atoms, plus the major partial Cl atoms where those 
 were resolved in the disordered anions, were refined anisotropically. All H 
 atoms were placed in calculated positions and refined using a riding model. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0979P)²+26.5933P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9301
_refine_ls_number_parameters     653
_refine_ls_number_restraints     70
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0780
_refine_ls_wR_factor_ref         0.2215
_refine_ls_wR_factor_gt          0.2019
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1A Fe 0.5000 0.86327(12) 0.7500 0.0405(3) Uani 1 2 d S . .
N2A N 0.53847(7) 0.8592(4) 0.7399(3) 0.0391(10) Uani 1 1 d . . .
C3A C 0.55006(10) 0.9327(5) 0.6864(3) 0.0427(12) Uani 1 1 d . . .
C4A C 0.57482(10) 0.9338(6) 0.6752(4) 0.0473(13) Uani 1 1 d . . .
H4A H 0.5823 0.9897 0.6394 0.057 Uiso 1 1 calc R . .
C5A C 0.58833(10) 0.8458(6) 0.7209(4) 0.0483(14) Uani 1 1 d . . .
C6A C 0.57663(10) 0.7679(6) 0.7759(4) 0.0484(14) Uani 1 1 d . . .
H6A H 0.5853 0.7098 0.8069 0.058 Uiso 1 1 calc R . .
C7A C 0.55197(9) 0.7786(5) 0.7836(3) 0.0412(12) Uani 1 1 d . . .
N8A N 0.53397(8) 1.0099(5) 0.6420(3) 0.0488(11) Uani 1 1 d . . .
N9A N 0.50961(8) 1.0019(5) 0.6579(3) 0.0506(12) Uani 1 1 d . . .
C10A C 0.49913(14) 1.0800(7) 0.6059(4) 0.0679(19) Uani 1 1 d . . .
H10A H 0.4824 1.0944 0.6029 0.081 Uiso 1 1 calc R . .
C11A C 0.51615(16) 1.1372(8) 0.5567(5) 0.087(3) Uani 1 1 d . . .
H11A H 0.5131 1.1955 0.5156 0.105 Uiso 1 1 calc R . .
C12A C 0.53841(14) 1.0918(7) 0.5802(5) 0.074(2) Uani 1 1 d . . .
H12A H 0.5535 1.1128 0.5582 0.089 Uiso 1 1 calc R . .
N13A N 0.53767(8) 0.7061(4) 0.8372(3) 0.0426(10) Uani 1 1 d . . .
N14A N 0.51302(8) 0.7205(5) 0.8357(3) 0.0450(11) Uani 1 1 d . . .
C15A C 0.50455(11) 0.6360(6) 0.8883(4) 0.0519(14) Uani 1 1 d . . .
H15A H 0.4881 0.6237 0.8998 0.062 Uiso 1 1 calc R . .
C16A C 0.52343(12) 0.5684(7) 0.9239(4) 0.0609(17) Uani 1 1 d . . .
H16A H 0.5221 0.5050 0.9629 0.073 Uiso 1 1 calc R . .
C17A C 0.54411(11) 0.6139(6) 0.8903(4) 0.0572(16) Uani 1 1 d . . .
H17A H 0.5599 0.5868 0.9014 0.069 Uiso 1 1 calc R . .
S18A S 0.61980(3) 0.82424(19) 0.71042(12) 0.0669(5) Uani 1 1 d . . .
C19A C 0.62809(12) 0.9327(9) 0.6321(6) 0.089(3) Uani 1 1 d . . .
H19A H 0.6186 0.9159 0.5840 0.133 Uiso 1 1 calc R A 1
H19B H 0.6451 0.9233 0.6197 0.133 Uiso 1 1 calc R A 1
H19C H 0.6250 1.0172 0.6504 0.133 Uiso 1 1 calc R A 1
Fe1B Fe 0.667630(14) 0.37328(8) 0.70175(5) 0.0405(2) Uani 1 1 d . B 1
N2B N 0.70602(8) 0.3927(4) 0.7156(3) 0.0426(10) Uani 1 1 d . B 1
C3B C 0.71541(10) 0.4763(6) 0.7685(4) 0.0490(14) Uani 1 1 d . B 1
C4B C 0.73975(10) 0.4955(7) 0.7794(4) 0.0572(16) Uani 1 1 d . B 1
H4B H 0.7456 0.5556 0.8158 0.069 Uiso 1 1 calc R B 1
C5B C 0.75546(11) 0.4210(7) 0.7334(4) 0.0602(17) Uani 1 1 d . B 1
C6B C 0.74646(10) 0.3324(7) 0.6785(4) 0.0559(16) Uani 1 1 d . B 1
H6B H 0.7568 0.2824 0.6471 0.067 Uiso 1 1 calc R B 1
C7B C 0.72140(10) 0.3228(6) 0.6730(3) 0.0454(13) Uani 1 1 d . B 1
N8B N 0.69710(9) 0.5419(5) 0.8125(3) 0.0515(12) Uani 1 1 d . B 1
N9B N 0.67335(8) 0.5157(5) 0.7960(3) 0.0524(12) Uani 1 1 d . B 1
C10B C 0.66053(13) 0.5891(7) 0.8457(4) 0.0662(18) Uani 1 1 d . B 1
H10B H 0.6436 0.5907 0.8486 0.079 Uiso 1 1 calc R B 1
C11B C 0.67585(15) 0.6622(8) 0.8925(5) 0.080(2) Uani 1 1 d . B 1
H11B H 0.6713 0.7218 0.9312 0.096 Uiso 1 1 calc R B 1
C12B C 0.69894(15) 0.6304(7) 0.8710(5) 0.074(2) Uani 1 1 d . B 1
H12B H 0.7133 0.6634 0.8925 0.089 Uiso 1 1 calc R B 1
N13B N 0.70944(8) 0.2380(5) 0.6212(3) 0.0484(11) Uani 1 1 d . B 1
N14B N 0.68465(9) 0.2342(5) 0.6233(3) 0.0487(11) Uani 1 1 d . B 1
C15B C 0.67839(13) 0.1441(6) 0.5709(4) 0.0597(16) Uani 1 1 d . B 1
H15B H 0.6624 0.1208 0.5593 0.072 Uiso 1 1 calc R B 1
C16B C 0.69884(15) 0.0896(7) 0.5356(4) 0.070(2) Uani 1 1 d . B 1
H16B H 0.6992 0.0247 0.4975 0.084 Uiso 1 1 calc R B 1
C17B C 0.71824(14) 0.1508(7) 0.5684(4) 0.0661(18) Uani 1 1 d . B 1
H17B H 0.7346 0.1357 0.5567 0.079 Uiso 1 1 calc R B 1
S18B S 0.78672(3) 0.4428(3) 0.75162(14) 0.0851(6) Uani 1 1 d . B 1
C19B C 0.80117(13) 0.3285(9) 0.6888(5) 0.088(3) Uani 1 1 d . B 1
H19D H 0.7951 0.2461 0.7023 0.133 Uiso 1 1 calc R B 1
H19E H 0.8185 0.3311 0.6977 0.133 Uiso 1 1 calc R B 1
H19F H 0.7977 0.3464 0.6325 0.133 Uiso 1 1 calc R B 1
N20B N 0.62918(8) 0.3914(5) 0.6940(3) 0.0428(10) Uani 1 1 d . B 1
C21B C 0.61460(10) 0.3242(6) 0.7418(3) 0.0450(13) Uani 1 1 d . B 1
C22B C 0.58958(10) 0.3367(7) 0.7426(4) 0.0544(15) Uani 1 1 d . B 1
H22B H 0.5798 0.2882 0.7766 0.065 Uiso 1 1 calc R B 1
C23B C 0.57977(11) 0.4265(7) 0.6895(4) 0.0576(16) Uani 1 1 d . B 1
C24B C 0.59465(10) 0.4970(7) 0.6389(4) 0.0547(15) Uani 1 1 d . B 1
H24B H 0.5882 0.5567 0.6033 0.066 Uiso 1 1 calc R B 1
C25B C 0.61922(10) 0.4755(6) 0.6435(3) 0.0453(13) Uani 1 1 d . B 1
N26B N 0.62744(8) 0.2344(5) 0.7887(3) 0.0456(11) Uani 1 1 d . B 1
N27B N 0.65226(8) 0.2297(5) 0.7811(3) 0.0464(11) Uani 1 1 d . B 1
C28B C 0.65909(13) 0.1338(6) 0.8269(4) 0.0582(16) Uani 1 1 d . B 1
H28B H 0.6752 0.1072 0.8329 0.070 Uiso 1 1 calc R B 1
C29B C 0.63921(13) 0.0775(7) 0.8650(4) 0.0650(18) Uani 1 1 d . B 1
H29B H 0.6395 0.0090 0.9004 0.078 Uiso 1 1 calc R B 1
C30B C 0.61930(13) 0.1430(7) 0.8400(4) 0.0622(17) Uani 1 1 d . B 1
H30B H 0.6032 0.1282 0.8550 0.075 Uiso 1 1 calc R B 1
N31B N 0.63648(8) 0.5364(5) 0.5936(3) 0.0482(11) Uani 1 1 d . B 1
N32B N 0.66052(8) 0.5082(5) 0.6055(3) 0.0486(11) Uani 1 1 d . B 1
C33B C 0.67215(13) 0.5756(7) 0.5496(4) 0.0610(17) Uani 1 1 d . B 1
H33B H 0.6890 0.5755 0.5426 0.073 Uiso 1 1 calc R B 1
C34B C 0.65617(15) 0.6459(8) 0.5029(5) 0.076(2) Uani 1 1 d . B 1
H34B H 0.6601 0.7006 0.4605 0.091 Uiso 1 1 calc R B 1
C35B C 0.63369(13) 0.6185(7) 0.5319(4) 0.0678(19) Uani 1 1 d . B 1
H35B H 0.6190 0.6506 0.5126 0.081 Uiso 1 1 calc R B 1
S36B S 0.54838(3) 0.4536(3) 0.67983(14) 0.0900(7) Uani 1 1 d . B 1
C37B C 0.53472(13) 0.3369(11) 0.7432(6) 0.113(4) Uani 1 1 d . B 1
H37A H 0.5405 0.2550 0.7274 0.169 Uiso 1 1 calc R B 1
H37B H 0.5173 0.3403 0.7373 0.169 Uiso 1 1 calc R B 1
H37C H 0.5390 0.3525 0.7991 0.169 Uiso 1 1 calc R B 1
Cl38A Cl 0.56285(13) 0.2553(6) 0.9713(4) 0.0613(15) Uani 0.60 1 d PD C 1
O39A O 0.5422(2) 0.2670(13) 1.0129(8) 0.122(5) Uiso 0.60 1 d PD C 1
O40A O 0.5820(2) 0.1772(13) 1.0070(8) 0.119(5) Uiso 0.60 1 d PD C 1
O41A O 0.5735(2) 0.3658(8) 0.9425(6) 0.090(3) Uiso 0.60 1 d PD C 1
O42A O 0.5584(2) 0.1879(11) 0.8934(6) 0.096(4) Uiso 0.60 1 d PD C 1
Cl38B Cl 0.5631(2) 0.2303(9) 0.9737(6) 0.051(2) Uiso 0.40 1 d PD D 2
O39B O 0.5428(2) 0.2044(16) 1.0252(9) 0.092(5) Uiso 0.40 1 d PD D 2
O40B O 0.5845(2) 0.2164(15) 1.0227(8) 0.074(4) Uiso 0.40 1 d PD D 2
O41B O 0.5623(4) 0.3576(14) 0.9468(14) 0.168(11) Uiso 0.40 1 d PD D 2
O42B O 0.5627(3) 0.1441(13) 0.9087(7) 0.072(4) Uiso 0.40 1 d PD D 2
Cl43A Cl 0.60523(14) 0.2166(9) 0.4898(5) 0.0530(16) Uani 0.64 1 d PD E 1
O44A O 0.5905(2) 0.1280(10) 0.4458(7) 0.119(4) Uiso 0.64 1 d PD E 1
O45A O 0.5998(2) 0.3420(9) 0.4621(7) 0.092(3) Uiso 0.64 1 d PD E 1
O46A O 0.62980(19) 0.1867(13) 0.4736(8) 0.146(5) Uiso 0.64 1 d PD E 1
O47A O 0.59973(19) 0.2028(9) 0.5731(5) 0.101(3) Uiso 0.64 1 d PD E 1
Cl43B Cl 0.6064(3) 0.2323(17) 0.4854(11) 0.071(5) Uiso 0.36 1 d PD F 2
O44B O 0.6081(4) 0.3512(16) 0.4463(12) 0.109(8) Uiso 0.36 1 d PD F 2
O45B O 0.6225(4) 0.2300(19) 0.5529(11) 0.129(7) Uiso 0.36 1 d PD F 2
O46B O 0.6124(5) 0.1411(19) 0.4259(13) 0.161(10) Uiso 0.36 1 d PD F 2
O47B O 0.5819(3) 0.216(3) 0.5119(17) 0.213(13) Uiso 0.36 1 d PD F 2
Cl48 Cl 0.72651(3) 0.24248(18) 0.94322(11) 0.0687(5) Uani 1 1 d D . .
O49A O 0.7020(2) 0.1922(16) 0.9608(11) 0.121(6) Uiso 0.40 1 d PD G 1
O50A O 0.7293(4) 0.2324(18) 0.8588(8) 0.142(7) Uiso 0.40 1 d PD G 1
O51A O 0.7421(2) 0.1459(11) 0.9809(8) 0.076(4) Uiso 0.40 1 d PD G 1
O52A O 0.7289(3) 0.3612(11) 0.9771(10) 0.075(4) Uiso 0.40 1 d PD G 1
O49B O 0.7285(5) 0.1165(14) 0.9608(17) 0.208(18) Uiso 0.30 1 d PD G 2
O50B O 0.7062(2) 0.2839(18) 0.8957(9) 0.077(5) Uiso 0.30 1 d PD G 2
O51B O 0.7481(2) 0.2815(14) 0.8974(8) 0.053(3) Uiso 0.30 1 d PD G 2
O52B O 0.7260(3) 0.3155(15) 1.0188(8) 0.065(4) Uiso 0.30 1 d PD G 2
O51C O 0.7233(4) 0.199(2) 1.0220(10) 0.126(8) Uiso 0.30 1 d PD G 3
O50C O 0.7251(6) 0.3820(14) 0.9494(19) 0.19(2) Uiso 0.30 1 d PD G 3
O52C O 0.7498(3) 0.223(3) 0.9094(15) 0.139(11) Uiso 0.30 1 d PD G 3
O49C O 0.7085(4) 0.203(2) 0.8893(13) 0.129(9) Uiso 0.30 1 d PD G 3


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1A N2A 2.115(4) . ?
Fe1A N9A 2.172(5) . ?
Fe1A N14A 2.185(5) . ?
N2A C3A 1.334(7) . ?
N2A C7A 1.338(7) . ?
C3A C4A 1.369(7) . ?
C3A N8A 1.406(7) . ?
C4A C5A 1.406(8) . ?
C4A H4A 0.9300 . ?
C5A C6A 1.381(8) . ?
C5A S18A 1.748(6) . ?
C6A C7A 1.362(7) . ?
C6A H6A 0.9300 . ?
C7A N13A 1.407(7) . ?
N8A C12A 1.356(8) . ?
N8A N9A 1.362(6) . ?
N9A C10A 1.320(8) . ?
C10A C11A 1.374(10) . ?
C10A H10A 0.9300 . ?
C11A C12A 1.366(10) . ?
C11A H11A 0.9300 . ?
C12A H12A 0.9300 . ?
N13A C17A 1.355(7) . ?
N13A N14A 1.360(6) . ?
N14A C15A 1.327(7) . ?
C15A C16A 1.387(9) . ?
C15A H15A 0.9300 . ?
C16A C17A 1.349(8) . ?
C16A H16A 0.9300 . ?
C17A H17A 0.9300 . ?
S18A C19A 1.782(8) . ?
C19A H19A 0.9600 . ?
C19A H19B 0.9600 . ?
C19A H19C 0.9600 . ?
Fe1B N20B 2.120(4) . ?
Fe1B N2B 2.126(4) . ?
Fe1B N32B 2.165(5) . ?
Fe1B N14B 2.168(5) . ?
Fe1B N27B 2.172(5) . ?
Fe1B N9B 2.182(5) . ?
N2B C7B 1.323(7) . ?
N2B C3B 1.341(7) . ?
C3B C4B 1.361(8) . ?
C3B N8B 1.418(7) . ?
C4B C5B 1.390(9) . ?
C4B H4B 0.9300 . ?
C5B C6B 1.391(10) . ?
C5B S18B 1.755(6) . ?
C6B C7B 1.380(8) . ?
C6B H6B 0.9300 . ?
C7B N13B 1.399(8) . ?
N8B C12B 1.345(8) . ?
N8B N9B 1.358(6) . ?
N9B C10B 1.328(8) . ?
C10B C11B 1.376(10) . ?
C10B H10B 0.9300 . ?
C11B C12B 1.356(11) . ?
C11B H11B 0.9300 . ?
C12B H12B 0.9300 . ?
N13B C17B 1.355(8) . ?
N13B N14B 1.359(6) . ?
N14B C15B 1.330(8) . ?
C15B C16B 1.387(10) . ?
C15B H15B 0.9300 . ?
C16B C17B 1.356(10) . ?
C16B H16B 0.9300 . ?
C17B H17B 0.9300 . ?
S18B C19B 1.776(9) . ?
C19B H19D 0.9600 . ?
C19B H19E 0.9600 . ?
C19B H19F 0.9600 . ?
N20B C21B 1.326(7) . ?
N20B C25B 1.333(7) . ?
C21B C22B 1.378(8) . ?
C21B N26B 1.412(7) . ?
C22B C23B 1.397(9) . ?
C22B H22B 0.9300 . ?
C23B C24B 1.382(9) . ?
C23B S36B 1.751(6) . ?
C24B C25B 1.368(8) . ?
C24B H24B 0.9300 . ?
C25B N31B 1.407(7) . ?
N26B C30B 1.358(8) . ?
N26B N27B 1.367(6) . ?
N27B C28B 1.318(8) . ?
C28B C29B 1.391(9) . ?
C28B H28B 0.9300 . ?
C29B C30B 1.357(10) . ?
C29B H29B 0.9300 . ?
C30B H30B 0.9300 . ?
N31B C35B 1.343(8) . ?
N31B N32B 1.365(6) . ?
N32B C33B 1.325(7) . ?
C33B C34B 1.381(10) . ?
C33B H33B 0.9300 . ?
C34B C35B 1.352(10) . ?
C34B H34B 0.9300 . ?
C35B H35B 0.9300 . ?
S36B C37B 1.780(10) . ?
C37B H37A 0.9600 . ?
C37B H37B 0.9600 . ?
C37B H37C 0.9600 . ?
Cl38A O39A 1.328(11) . ?
Cl38A O41A 1.393(10) . ?
Cl38A O40A 1.459(11) . ?
Cl38A O42A 1.482(10) . ?
Cl38B O42B 1.404(12) . ?
Cl38B O39B 1.420(13) . ?
Cl38B O41B 1.422(14) . ?
Cl38B O40B 1.428(13) . ?
Cl43A O47A 1.404(11) . ?
Cl43A O46A 1.409(12) . ?
Cl43A O44A 1.433(11) . ?
Cl43A O45A 1.435(11) . ?
Cl43B O46B 1.412(16) . ?
Cl43B O45B 1.417(16) . ?
Cl43B O44B 1.419(16) . ?
Cl43B O47B 1.419(16) . ?
Cl48 O52A 1.383(10) . ?
Cl48 O50A 1.395(12) . ?
Cl48 O51A 1.470(10) . ?
Cl48 O49A 1.475(12) . ?
Cl48 O49B 1.371(14) . ?
Cl48 O50B 1.426(12) . ?
Cl48 O52B 1.461(11) . ?
Cl48 O51B 1.461(11) . ?
Cl48 O51C 1.382(14) . ?
Cl48 O49C 1.389(14) . ?
Cl48 O52C 1.408(14) . ?
Cl48 O50C 1.485(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2A Fe1A N2A 177.7(3) 4_656 . ?
N2A Fe1A N9A 108.06(17) . 4_656 ?
N2A Fe1A N9A 73.61(17) . . ?
N9A Fe1A N9A 94.7(3) 4_656 . ?
N2A Fe1A N14A 105.13(17) . 4_656 ?
N9A Fe1A N14A 95.88(18) . 4_656 ?
N2A Fe1A N14A 73.18(16) . . ?
N9A Fe1A N14A 146.78(16) . . ?
N14A Fe1A N14A 92.2(3) 4_656 . ?
C3A N2A C7A 117.5(4) . . ?
C3A N2A Fe1A 120.9(4) . . ?
C7A N2A Fe1A 121.5(3) . . ?
N2A C3A C4A 124.4(5) . . ?
N2A C3A N8A 112.4(5) . . ?
C4A C3A N8A 123.2(5) . . ?
C3A C4A C5A 116.5(5) . . ?
C3A C4A H4A 121.8 . . ?
C5A C4A H4A 121.8 . . ?
C6A C5A C4A 120.0(5) . . ?
C6A C5A S18A 116.3(5) . . ?
C4A C5A S18A 123.7(5) . . ?
C7A C6A C5A 118.1(5) . . ?
C7A C6A H6A 121.0 . . ?
C5A C6A H6A 121.0 . . ?
N2A C7A C6A 123.6(5) . . ?
N2A C7A N13A 112.0(4) . . ?
C6A C7A N13A 124.4(5) . . ?
C12A N8A N9A 111.0(5) . . ?
C12A N8A C3A 130.3(5) . . ?
N9A N8A C3A 118.7(4) . . ?
C10A N9A N8A 105.4(5) . . ?
C10A N9A Fe1A 140.1(5) . . ?
N8A N9A Fe1A 114.3(3) . . ?
N9A C10A C11A 111.1(6) . . ?
N9A C10A H10A 124.5 . . ?
C11A C10A H10A 124.5 . . ?
C12A C11A C10A 106.6(7) . . ?
C12A C11A H11A 126.7 . . ?
C10A C11A H11A 126.7 . . ?
N8A C12A C11A 106.0(7) . . ?
N8A C12A H12A 127.0 . . ?
C11A C12A H12A 127.0 . . ?
C17A N13A N14A 110.6(5) . . ?
C17A N13A C7A 130.6(5) . . ?
N14A N13A C7A 118.7(4) . . ?
C15A N14A N13A 105.1(5) . . ?
C15A N14A Fe1A 140.5(4) . . ?
N13A N14A Fe1A 114.5(3) . . ?
N14A C15A C16A 111.2(5) . . ?
N14A C15A H15A 124.4 . . ?
C16A C15A H15A 124.4 . . ?
C17A C16A C15A 105.7(6) . . ?
C17A C16A H16A 127.2 . . ?
C15A C16A H16A 127.2 . . ?
C16A C17A N13A 107.5(5) . . ?
C16A C17A H17A 126.2 . . ?
N13A C17A H17A 126.2 . . ?
C5A S18A C19A 103.7(3) . . ?
S18A C19A H19A 109.5 . . ?
S18A C19A H19B 109.5 . . ?
S18A C19A H19C 109.5 . . ?
N20B Fe1B N2B 168.89(19) . . ?
N20B Fe1B N32B 73.60(17) . . ?
N2B Fe1B N32B 101.06(17) . . ?
N20B Fe1B N14B 117.01(18) . . ?
N2B Fe1B N14B 72.76(18) . . ?
N32B Fe1B N14B 95.50(19) . . ?
N20B Fe1B N27B 73.36(18) . . ?
N2B Fe1B N27B 112.82(18) . . ?
N32B Fe1B N27B 146.05(17) . . ?
N14B Fe1B N27B 92.53(18) . . ?
N20B Fe1B N9B 97.03(18) . . ?
N2B Fe1B N9B 73.44(18) . . ?
N32B Fe1B N9B 94.8(2) . . ?
N14B Fe1B N9B 145.96(18) . . ?
N27B Fe1B N9B 96.79(19) . . ?
C7B N2B C3B 117.9(5) . . ?
C7B N2B Fe1B 121.3(4) . . ?
C3B N2B Fe1B 120.8(4) . . ?
N2B C3B C4B 124.0(6) . . ?
N2B C3B N8B 112.4(5) . . ?
C4B C3B N8B 123.6(6) . . ?
C3B C4B C5B 116.8(6) . . ?
C3B C4B H4B 121.6 . . ?
C5B C4B H4B 121.6 . . ?
C4B C5B C6B 121.0(5) . . ?
C4B C5B S18B 116.0(5) . . ?
C6B C5B S18B 123.0(5) . . ?
C7B C6B C5B 116.4(6) . . ?
C7B C6B H6B 121.8 . . ?
C5B C6B H6B 121.8 . . ?
N2B C7B C6B 123.9(6) . . ?
N2B C7B N13B 112.5(5) . . ?
C6B C7B N13B 123.6(5) . . ?
C12B N8B N9B 110.9(5) . . ?
C12B N8B C3B 130.7(6) . . ?
N9B N8B C3B 118.4(5) . . ?
C10B N9B N8B 105.3(5) . . ?
C10B N9B Fe1B 139.8(5) . . ?
N8B N9B Fe1B 114.9(4) . . ?
N9B C10B C11B 110.5(6) . . ?
N9B C10B H10B 124.8 . . ?
C11B C10B H10B 124.8 . . ?
C12B C11B C10B 106.5(6) . . ?
C12B C11B H11B 126.7 . . ?
C10B C11B H11B 126.7 . . ?
N8B C12B C11B 106.8(7) . . ?
N8B C12B H12B 126.6 . . ?
C11B C12B H12B 126.6 . . ?
C17B N13B N14B 110.6(5) . . ?
C17B N13B C7B 131.2(5) . . ?
N14B N13B C7B 118.2(5) . . ?
C15B N14B N13B 105.2(5) . . ?
C15B N14B Fe1B 139.5(4) . . ?
N13B N14B Fe1B 115.1(4) . . ?
N14B C15B C16B 111.1(6) . . ?
N14B C15B H15B 124.4 . . ?
C16B C15B H15B 124.4 . . ?
C17B C16B C15B 105.6(6) . . ?
C17B C16B H16B 127.2 . . ?
C15B C16B H16B 127.2 . . ?
N13B C17B C16B 107.5(6) . . ?
N13B C17B H17B 126.3 . . ?
C16B C17B H17B 126.3 . . ?
C5B S18B C19B 104.3(4) . . ?
C21B N20B C25B 118.6(5) . . ?
C21B N20B Fe1B 121.0(4) . . ?
C25B N20B Fe1B 120.3(4) . . ?
N20B C21B C22B 123.6(6) . . ?
N20B C21B N26B 112.6(5) . . ?
C22B C21B N26B 123.8(5) . . ?
C21B C22B C23B 116.3(6) . . ?
C21B C22B H22B 121.9 . . ?
C23B C22B H22B 121.9 . . ?
C24B C23B C22B 121.0(5) . . ?
C24B C23B S36B 115.9(5) . . ?
C22B C23B S36B 123.1(5) . . ?
C25B C24B C23B 117.2(6) . . ?
C25B C24B H24B 121.4 . . ?
C23B C24B H24B 121.4 . . ?
N20B C25B C24B 123.3(5) . . ?
N20B C25B N31B 113.1(5) . . ?
C24B C25B N31B 123.6(5) . . ?
C30B N26B N27B 111.0(5) . . ?
C30B N26B C21B 130.9(5) . . ?
N27B N26B C21B 118.1(4) . . ?
C28B N27B N26B 105.0(5) . . ?
C28B N27B Fe1B 140.5(4) . . ?
N26B N27B Fe1B 114.5(3) . . ?
N27B C28B C29B 111.4(6) . . ?
N27B C28B H28B 124.3 . . ?
C29B C28B H28B 124.3 . . ?
C30B C29B C28B 105.9(6) . . ?
C30B C29B H29B 127.0 . . ?
C28B C29B H29B 127.0 . . ?
C29B C30B N26B 106.7(6) . . ?
C29B C30B H30B 126.6 . . ?
N26B C30B H30B 126.6 . . ?
C35B N31B N32B 111.0(5) . . ?
C35B N31B C25B 131.2(5) . . ?
N32B N31B C25B 117.7(5) . . ?
C33B N32B N31B 104.3(5) . . ?
C33B N32B Fe1B 140.7(4) . . ?
N31B N32B Fe1B 115.0(3) . . ?
N32B C33B C34B 111.6(6) . . ?
N32B C33B H33B 124.2 . . ?
C34B C33B H33B 124.2 . . ?
C35B C34B C33B 105.5(6) . . ?
C35B C34B H34B 127.2 . . ?
C33B C34B H34B 127.2 . . ?
N31B C35B C34B 107.4(6) . . ?
N31B C35B H35B 126.3 . . ?
C34B C35B H35B 126.3 . . ?
C23B S36B C37B 104.3(4) . . ?
O39A Cl38A O41A 116.9(9) . . ?
O39A Cl38A O40A 117.4(9) . . ?
O41A Cl38A O40A 108.2(8) . . ?
O39A Cl38A O42A 110.2(8) . . ?
O41A Cl38A O42A 100.6(7) . . ?
O40A Cl38A O42A 101.0(8) . . ?
O42B Cl38B O39B 108.1(10) . . ?
O42B Cl38B O41B 112.5(12) . . ?
O39B Cl38B O41B 110.1(12) . . ?
O42B Cl38B O40B 111.9(10) . . ?
O39B Cl38B O40B 106.8(10) . . ?
O41B Cl38B O40B 107.3(12) . . ?
O47A Cl43A O46A 111.4(8) . . ?
O47A Cl43A O44A 107.4(9) . . ?
O46A Cl43A O44A 107.2(8) . . ?
O47A Cl43A O45A 111.1(7) . . ?
O46A Cl43A O45A 110.2(9) . . ?
O44A Cl43A O45A 109.4(7) . . ?
O46B Cl43B O45B 112.4(14) . . ?
O46B Cl43B O44B 106.3(14) . . ?
O45B Cl43B O44B 108.9(14) . . ?
O46B Cl43B O47B 110.3(15) . . ?
O45B Cl43B O47B 110.5(14) . . ?
O44B Cl43B O47B 108.2(14) . . ?
O52A Cl48 O50A 117.2(10) . . ?
O52A Cl48 O51A 114.3(8) . . ?
O50A Cl48 O51A 107.5(9) . . ?
O52A Cl48 O49A 109.7(8) . . ?
O50A Cl48 O49A 105.3(9) . . ?
O51A Cl48 O49A 101.3(8) . . ?
O49B Cl48 O50B 118.5(12) . . ?
O49B Cl48 O52B 109.8(12) . . ?
O50B Cl48 O52B 106.6(8) . . ?
O49B Cl48 O51B 108.7(12) . . ?
O50B Cl48 O51B 105.3(8) . . ?
O52B Cl48 O51B 107.5(8) . . ?
O51C Cl48 O50C 105.2(12) . . ?
O51C Cl48 O49C 113.6(12) . . ?
O51C Cl48 O52C 115.8(12) . . ?
O49C Cl48 O52C 110.5(12) . . ?
O49C Cl48 O50C 107.9(12) . . ?
O52C Cl48 O50C 102.8(12) . . ?

_diffrn_measured_fraction_theta_max 0.965
_diffrn_reflns_theta_full        73.73
_diffrn_measured_fraction_theta_full 0.965
_refine_diff_density_max         0.827
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.083
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: nitromethane/diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lkc266253
_database_code_depnum_ccdc_archive 'CCDC 1060842'
_audit_update_record             
;
2015-04-21 deposited with the CCDC.
2015-06-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
Bis[2,6-di(pyrazol-1-yl)4-methylsulfanylpyridine]iron(II)diperchlorate
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H22 Fe N10 S2, 2[Cl O4]'
_chemical_formula_sum            'C24 H22 Cl2 Fe N10 O8 S2'
_chemical_formula_weight         769.39

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'
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'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P b c n'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'

_cell_length_a                   53.7002(12)
_cell_length_b                   10.6448(2)
_cell_length_c                   16.3472(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     9344.5(3)
_cell_formula_units_Z            12
_cell_measurement_temperature    253(2)
_cell_measurement_reflns_used    6136
_cell_measurement_theta_min      4.22
_cell_measurement_theta_max      73.63

_exptl_crystal_description       fragment
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4704
_exptl_absorpt_coefficient_mu    7.288
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.633
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28e (release 10-06-2013 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      253(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            18968
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_min       -65
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         4.23
_diffrn_reflns_theta_max         73.84
_reflns_number_total             9050
_reflns_number_gt                7279
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The asymmetric unit contains 1.5 formula units, with half a complex cation 
 spanning the C₂ axis 1/2, y, 3/4 (molecule A); and, a whole complex dication 
 (molecule B) and three unique BF₄⁻ anions lying on general crystallographic 
 sites. All three anions are disordered, over three sites with occupancies of
 0.40:0.40:0.20 (Cl38-O42); over three sites with occupancies of 0.40:0.30:0.30 
 that share a common wholly occupied Cl atom (Cl48-O52); or, over two sites with 
 refined occupancies of 0.65:0.35 (Cl43-O47). The refined restraints 
 Cl---O = 1.42(2) and O...O = 2.32(2) Å were applied to these residues. 

 All wholly occupied non-H atoms, plus disordered Cl atoms with >0.5 occupancy, 
 were refined anisotropically. All H atoms were placed in calculated positions 
 and refined using a riding model. The highest residual Fourier peak of 
 +1.4 e.Å⁻³ is close to S18A, and may represent a minor (ca. 5 %) disorder 
 site for this mehtylsulfanyl group.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1343P)²+13.2989P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9050
_refine_ls_number_parameters     668
_refine_ls_number_restraints     56
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0796
_refine_ls_wR_factor_ref         0.2307
_refine_ls_wR_factor_gt          0.2170
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1A Fe 0.5000 0.85794(10) 0.7500 0.0443(3) Uani 1 2 d S . .
N2A N 0.53762(8) 0.8522(4) 0.7362(2) 0.0507(9) Uani 1 1 d . . .
C3A C 0.54909(10) 0.9269(5) 0.6827(3) 0.0540(11) Uani 1 1 d . . .
C4A C 0.57449(10) 0.9274(5) 0.6714(3) 0.0610(13) Uani 1 1 d . . .
H4A H 0.5821 0.9841 0.6360 0.073 Uiso 1 1 calc R . .
C5A C 0.58852(10) 0.8386(5) 0.7157(3) 0.0589(12) Uani 1 1 d . . .
C6A C 0.57675(9) 0.7595(5) 0.7705(3) 0.0558(11) Uani 1 1 d . . .
H6A H 0.5856 0.7001 0.8003 0.067 Uiso 1 1 calc R . .
C7A C 0.55136(9) 0.7719(5) 0.7793(3) 0.0508(10) Uani 1 1 d . . .
N8A N 0.53222(9) 1.0036(4) 0.6420(3) 0.0650(11) Uani 1 1 d . . .
N9A N 0.50717(9) 0.9925(4) 0.6610(3) 0.0648(11) Uani 1 1 d . . .
C10A C 0.49553(17) 1.0718(7) 0.6113(4) 0.096(2) Uani 1 1 d . . .
H10A H 0.4784 1.0841 0.6097 0.115 Uiso 1 1 calc R . .
C11A C 0.5126(2) 1.1337(7) 0.5622(5) 0.113(3) Uani 1 1 d . . .
H11A H 0.5090 1.1956 0.5238 0.135 Uiso 1 1 calc R . .
C12A C 0.53554(17) 1.0878(7) 0.5801(4) 0.094(2) Uani 1 1 d . . .
H12A H 0.5505 1.1093 0.5552 0.112 Uiso 1 1 calc R . .
N13A N 0.53671(7) 0.6986(4) 0.8323(2) 0.0534(9) Uani 1 1 d . . .
N14A N 0.51151(7) 0.7201(4) 0.8331(2) 0.0519(9) Uani 1 1 d . . .
C15A C 0.50256(12) 0.6371(5) 0.8855(3) 0.0666(14) Uani 1 1 d . . .
H15A H 0.4858 0.6289 0.8985 0.080 Uiso 1 1 calc R . .
C16A C 0.52138(13) 0.5634(6) 0.9189(4) 0.0762(17) Uani 1 1 d . . .
H16A H 0.5196 0.4993 0.9571 0.091 Uiso 1 1 calc R . .
C17A C 0.54301(12) 0.6041(6) 0.8844(4) 0.0709(15) Uani 1 1 d . . .
H17A H 0.5589 0.5734 0.8945 0.085 Uiso 1 1 calc R . .
S18A S 0.62061(3) 0.81675(16) 0.70615(11) 0.0754(4) Uani 1 1 d . . .
C19A C 0.62914(12) 0.9263(7) 0.6282(6) 0.103(3) Uani 1 1 d . . .
H19A H 0.6206 0.9058 0.5784 0.155 Uiso 1 1 calc R . .
H19B H 0.6468 0.9222 0.6192 0.155 Uiso 1 1 calc R . .
H19C H 0.6246 1.0096 0.6451 0.155 Uiso 1 1 calc R . .
Fe1B Fe 0.667449(11) 0.37467(7) 0.70777(4) 0.0439(2) Uani 1 1 d . A 1
N2B N 0.70283(8) 0.3820(4) 0.7255(3) 0.0529(9) Uani 1 1 d . A 1
C3B C 0.71228(9) 0.4644(5) 0.7793(3) 0.0560(12) Uani 1 1 d . A 1
C4B C 0.73735(10) 0.4802(6) 0.7914(3) 0.0631(13) Uani 1 1 d . A 1
H4B H 0.7435 0.5383 0.8287 0.076 Uiso 1 1 calc R A 1
C5B C 0.75321(10) 0.4045(6) 0.7445(4) 0.0662(14) Uani 1 1 d . A 1
C6B C 0.74383(10) 0.3183(6) 0.6889(3) 0.0622(13) Uani 1 1 d . A 1
H6B H 0.7542 0.2674 0.6577 0.075 Uiso 1 1 calc R A 1
C7B C 0.71816(9) 0.3121(5) 0.6823(3) 0.0538(11) Uani 1 1 d . A 1
N8B N 0.69335(8) 0.5301(4) 0.8196(3) 0.0581(10) Uani 1 1 d . A 1
N9B N 0.66944(7) 0.5051(4) 0.7955(3) 0.0567(10) Uani 1 1 d . A 1
C10B C 0.65508(12) 0.5787(6) 0.8412(4) 0.0694(14) Uani 1 1 d . A 1
H10B H 0.6378 0.5813 0.8385 0.083 Uiso 1 1 calc R A 1
C11B C 0.66955(13) 0.6511(7) 0.8937(5) 0.0829(19) Uani 1 1 d . A 1
H11B H 0.6638 0.7101 0.9312 0.099 Uiso 1 1 calc R A 1
C12B C 0.69322(13) 0.6197(6) 0.8800(4) 0.0770(17) Uani 1 1 d . A 1
H12B H 0.7071 0.6525 0.9064 0.092 Uiso 1 1 calc R A 1
N13B N 0.70467(8) 0.2323(4) 0.6281(3) 0.0567(10) Uani 1 1 d . A 1
N14B N 0.67909(7) 0.2449(4) 0.6291(3) 0.0537(9) Uani 1 1 d . A 1
C15B C 0.67065(11) 0.1619(5) 0.5759(4) 0.0649(13) Uani 1 1 d . A 1
H15B H 0.6540 0.1506 0.5627 0.078 Uiso 1 1 calc R A 1
C16B C 0.69019(13) 0.0940(6) 0.5427(4) 0.0778(17) Uani 1 1 d . A 1
H16B H 0.6890 0.0282 0.5054 0.093 Uiso 1 1 calc R A 1
C17B C 0.71146(12) 0.1426(6) 0.5752(4) 0.0696(15) Uani 1 1 d . A 1
H17B H 0.7277 0.1180 0.5630 0.084 Uiso 1 1 calc R A 1
S18B S 0.78503(3) 0.4277(2) 0.76432(12) 0.0867(5) Uani 1 1 d . A 1
C19B C 0.79879(15) 0.3167(7) 0.7017(5) 0.098(2) Uani 1 1 d . A 1
H19D H 0.7915 0.2359 0.7121 0.147 Uiso 1 1 calc R A 1
H19E H 0.8163 0.3134 0.7127 0.147 Uiso 1 1 calc R A 1
H19F H 0.7962 0.3392 0.6455 0.147 Uiso 1 1 calc R A 1
N20B N 0.63183(7) 0.3822(4) 0.6941(2) 0.0479(8) Uani 1 1 d . A 1
C21B C 0.61703(8) 0.3131(5) 0.7416(3) 0.0494(10) Uani 1 1 d . A 1
C22B C 0.59150(9) 0.3226(6) 0.7409(3) 0.0594(13) Uani 1 1 d . A 1
H22B H 0.5815 0.2742 0.7751 0.071 Uiso 1 1 calc R A 1
C23B C 0.58132(10) 0.4103(6) 0.6852(4) 0.0651(14) Uani 1 1 d . A 1
C24B C 0.59638(9) 0.4835(5) 0.6361(3) 0.0606(13) Uani 1 1 d . A 1
H24B H 0.5897 0.5423 0.6001 0.073 Uiso 1 1 calc R A 1
C25B C 0.62175(8) 0.4652(5) 0.6428(3) 0.0515(11) Uani 1 1 d . A 1
N26B N 0.63106(8) 0.2318(4) 0.7913(3) 0.0543(9) Uani 1 1 d . A 1
N27B N 0.65648(7) 0.2420(4) 0.7863(2) 0.0509(9) Uani 1 1 d . A 1
C28B C 0.66566(11) 0.1519(6) 0.8328(3) 0.0641(14) Uani 1 1 d . A 1
H28B H 0.6825 0.1363 0.8406 0.077 Uiso 1 1 calc R A 1
C29B C 0.64629(13) 0.0833(6) 0.8689(4) 0.0772(17) Uani 1 1 d . A 1
H29B H 0.6479 0.0162 0.9049 0.093 Uiso 1 1 calc R A 1
C30B C 0.62456(12) 0.1346(5) 0.8406(4) 0.0680(15) Uani 1 1 d . A 1
H30B H 0.6085 0.1080 0.8527 0.082 Uiso 1 1 calc R A 1
N31B N 0.64014(7) 0.5284(4) 0.5979(3) 0.0550(9) Uani 1 1 d . A 1
N32B N 0.66453(7) 0.5031(4) 0.6194(3) 0.0537(9) Uani 1 1 d . A 1
C33B C 0.67824(11) 0.5719(5) 0.5680(4) 0.0679(14) Uani 1 1 d . A 1
H33B H 0.6956 0.5735 0.5672 0.081 Uiso 1 1 calc R A 1
C34B C 0.66298(14) 0.6410(6) 0.5160(4) 0.084(2) Uani 1 1 d . A 1
H34B H 0.6681 0.6964 0.4754 0.101 Uiso 1 1 calc R A 1
C35B C 0.63908(13) 0.6118(6) 0.5360(4) 0.0732(16) Uani 1 1 d . A 1
H35B H 0.6247 0.6434 0.5116 0.088 Uiso 1 1 calc R A 1
S36B S 0.54939(3) 0.4348(2) 0.67359(13) 0.0955(6) Uani 1 1 d . A 1
C37B C 0.53597(13) 0.3225(10) 0.7421(6) 0.120(3) Uani 1 1 d . A 1
H37A H 0.5444 0.2435 0.7363 0.179 Uiso 1 1 calc R A 1
H37B H 0.5186 0.3119 0.7293 0.179 Uiso 1 1 calc R A 1
H37C H 0.5376 0.3518 0.7973 0.179 Uiso 1 1 calc R A 1
Cl3A Cl 0.56676(18) 0.2614(11) 0.9694(7) 0.067(3) Uiso 0.40 1 d P B 1
O39A O 0.5454(4) 0.2791(19) 1.0096(13) 0.123(6) Uiso 0.40 1 d P B 1
O40A O 0.5875(3) 0.2359(15) 1.0189(10) 0.093(4) Uiso 0.40 1 d P B 1
O41A O 0.5775(4) 0.3665(15) 0.9337(10) 0.087(4) Uiso 0.40 1 d P B 1
O42A O 0.5656(2) 0.1532(13) 0.9031(8) 0.074(3) Uiso 0.40 1 d P B 1
Cl3B Cl 0.56645(15) 0.2389(7) 0.9670(5) 0.065(2) Uiso 0.40 1 d P C 2
O39B O 0.5451(3) 0.2119(16) 1.0206(10) 0.101(4) Uiso 0.40 1 d P C 2
O40B O 0.5876(3) 0.1862(14) 1.0068(9) 0.081(4) Uiso 0.40 1 d P C 2
O41B O 0.5670(5) 0.372(3) 0.9488(17) 0.158(10) Uiso 0.40 1 d P C 2
O42B O 0.5615(3) 0.1953(16) 0.8931(10) 0.097(5) Uiso 0.40 1 d P C 2
Cl3C Cl 0.5634(2) 0.2710(16) 0.9852(8) 0.071(4) Uiso 0.20 1 d P D 3
O39C O 0.5464(6) 0.296(3) 0.9211(18) 0.156(14) Uiso 0.20 1 d PD D 3
O40C O 0.5719(6) 0.141(2) 0.9760(18) 0.113(9) Uiso 0.20 1 d PD D 3
O41C O 0.5871(7) 0.345(3) 0.952(2) 0.18(3) Uiso 0.20 1 d PD D 3
O42C O 0.5589(5) 0.311(2) 1.0577(14) 0.096(7) Uiso 0.20 1 d PD D 3
Cl4A Cl 0.60209(17) 0.2104(9) 0.4812(6) 0.061(3) Uani 0.65 1 d PD E 1
O44A O 0.57878(16) 0.1574(9) 0.4520(6) 0.104(3) Uiso 0.65 1 d PD E 1
O45A O 0.60156(18) 0.3410(7) 0.4584(5) 0.085(2) Uiso 0.65 1 d PD E 1
O46A O 0.62207(18) 0.1529(9) 0.4424(6) 0.120(3) Uiso 0.65 1 d PD E 1
O47A O 0.60163(17) 0.1906(8) 0.5678(5) 0.087(2) Uiso 0.65 1 d PD E 1
Cl4B Cl 0.6014(3) 0.2188(16) 0.4817(10) 0.059(5) Uiso 0.35 1 d PD F 2
O44B O 0.6103(4) 0.3364(16) 0.4530(14) 0.136(9) Uiso 0.35 1 d PD F 2
O45B O 0.6107(3) 0.2049(16) 0.5613(8) 0.092(5) Uiso 0.35 1 d PD F 2
O46B O 0.6100(4) 0.1222(16) 0.4284(11) 0.129(7) Uiso 0.35 1 d PD F 2
O47B O 0.5750(3) 0.2201(18) 0.4770(12) 0.123(6) Uiso 0.35 1 d PD F 2
Cl48 Cl 0.73162(3) 0.22357(14) 0.95970(9) 0.0694(4) Uani 1 1 d D . .
O49A O 0.7071(2) 0.1637(14) 0.9773(10) 0.114(5) Uiso 0.40 1 d PD G 1
O50A O 0.7338(3) 0.2267(17) 0.8752(7) 0.127(7) Uiso 0.40 1 d PD G 1
O51A O 0.7492(3) 0.1360(12) 0.9962(9) 0.098(4) Uiso 0.40 1 d PD G 1
O52A O 0.7323(3) 0.3394(11) 1.0000(11) 0.087(5) Uiso 0.40 1 d PD G 1
O49B O 0.7333(5) 0.1039(14) 0.9932(15) 0.170(11) Uiso 0.30 1 d PD G 2
O50B O 0.7118(3) 0.2498(18) 0.9062(11) 0.117(6) Uiso 0.30 1 d PD G 2
O51B O 0.7543(2) 0.2543(12) 0.9154(8) 0.071(3) Uiso 0.30 1 d PD G 2
O52B O 0.7304(3) 0.3095(14) 1.0300(8) 0.078(5) Uiso 0.30 1 d PD G 2
O49C O 0.7255(3) 0.1980(14) 0.8744(7) 0.067(4) Uiso 0.30 1 d PD G 3
O50C O 0.7312(3) 0.3548(11) 0.9717(11) 0.079(5) Uiso 0.30 1 d PD G 3
O51C O 0.7149(4) 0.1617(19) 1.0124(11) 0.123(8) Uiso 0.30 1 d PD G 3
O52C O 0.7566(2) 0.1769(15) 0.9701(10) 0.086(5) Uiso 0.30 1 d PD G 3


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1A N2A 2.034(4) . ?
Fe1A N9A 2.078(5) . ?
Fe1A N14A 2.092(4) . ?
N2A C7A 1.332(6) . ?
N2A C3A 1.332(6) . ?
C3A C4A 1.376(7) . ?
C3A N8A 1.389(7) . ?
C4A C5A 1.409(8) . ?
C4A H4A 0.9300 . ?
C5A C6A 1.382(7) . ?
C5A S18A 1.746(5) . ?
C6A C7A 1.378(7) . ?
C6A H6A 0.9300 . ?
C7A N13A 1.406(6) . ?
N8A C12A 1.364(7) . ?
N8A N9A 1.386(6) . ?
N9A C10A 1.327(8) . ?
C10A C11A 1.386(12) . ?
C10A H10A 0.9300 . ?
C11A C12A 1.357(12) . ?
C11A H11A 0.9300 . ?
C12A H12A 0.9300 . ?
N13A C17A 1.361(7) . ?
N13A N14A 1.373(5) . ?
N14A C15A 1.323(7) . ?
C15A C16A 1.391(9) . ?
C15A H15A 0.9300 . ?
C16A C17A 1.362(8) . ?
C16A H16A 0.9300 . ?
C17A H17A 0.9300 . ?
S18A C19A 1.787(7) . ?
C19A H19A 0.9600 . ?
C19A H19B 0.9600 . ?
C19A H19C 0.9600 . ?
Fe1B N2B 1.924(4) . ?
Fe1B N20B 1.927(4) . ?
Fe1B N14B 1.988(4) . ?
Fe1B N32B 1.995(4) . ?
Fe1B N27B 1.997(4) . ?
Fe1B N9B 1.999(5) . ?
N2B C7B 1.315(7) . ?
N2B C3B 1.342(7) . ?
C3B C4B 1.371(7) . ?
C3B N8B 1.399(7) . ?
C4B C5B 1.401(8) . ?
C4B H4B 0.9300 . ?
C5B C6B 1.387(8) . ?
C5B S18B 1.756(6) . ?
C6B C7B 1.384(7) . ?
C6B H6B 0.9300 . ?
C7B N13B 1.425(7) . ?
N8B N9B 1.369(6) . ?
N8B C12B 1.372(7) . ?
N9B C10B 1.329(7) . ?
C10B C11B 1.391(9) . ?
C10B H10B 0.9300 . ?
C11B C12B 1.333(9) . ?
C11B H11B 0.9300 . ?
C12B H12B 0.9300 . ?
N13B C17B 1.339(7) . ?
N13B N14B 1.381(6) . ?
N14B C15B 1.319(7) . ?
C15B C16B 1.386(9) . ?
C15B H15B 0.9300 . ?
C16B C17B 1.362(9) . ?
C16B H16B 0.9300 . ?
C17B H17B 0.9300 . ?
S18B C19B 1.729(9) . ?
C19B H19D 0.9600 . ?
C19B H19E 0.9600 . ?
C19B H19F 0.9600 . ?
N20B C21B 1.332(6) . ?
N20B C25B 1.333(6) . ?
C21B C22B 1.375(7) . ?
C21B N26B 1.406(7) . ?
C22B C23B 1.414(9) . ?
C22B H22B 0.9300 . ?
C23B C24B 1.381(8) . ?
C23B S36B 1.745(5) . ?
C24B C25B 1.380(6) . ?
C24B H24B 0.9300 . ?
C25B N31B 1.403(6) . ?
N26B C30B 1.357(7) . ?
N26B N27B 1.372(5) . ?
N27B C28B 1.320(7) . ?
C28B C29B 1.402(8) . ?
C28B H28B 0.9300 . ?
C29B C30B 1.369(9) . ?
C29B H29B 0.9300 . ?
C30B H30B 0.9300 . ?
N31B C35B 1.347(7) . ?
N31B N32B 1.383(5) . ?
N32B C33B 1.336(7) . ?
C33B C34B 1.391(9) . ?
C33B H33B 0.9300 . ?
C34B C35B 1.360(9) . ?
C34B H34B 0.9300 . ?
C35B H35B 0.9300 . ?
S36B C37B 1.790(9) . ?
C37B H37A 0.9600 . ?
C37B H37B 0.9600 . ?
C37B H37C 0.9600 . ?
Cl3A O39A 1.33(2) . ?
Cl3A O41A 1.387(18) . ?
Cl3A O40A 1.405(18) . ?
Cl3A O42A 1.582(18) . ?
Cl3B O42B 1.321(18) . ?
Cl3B O40B 1.423(15) . ?
Cl3B O41B 1.45(3) . ?
Cl3B O39B 1.471(18) . ?
Cl3C O42C 1.28(2) . ?
Cl3C O39C 1.41(3) . ?
Cl3C O40C 1.46(3) . ?
Cl3C O41C 1.59(3) . ?
Cl4A O46A 1.388(11) . ?
Cl4A O47A 1.432(10) . ?
Cl4A O45A 1.439(10) . ?
Cl4A O44A 1.454(11) . ?
Cl4B O45B 1.403(16) . ?
Cl4B O47B 1.420(16) . ?
Cl4B O44B 1.421(16) . ?
Cl4B O46B 1.425(16) . ?
Cl48 O50A 1.387(12) . ?
Cl48 O51A 1.453(10) . ?
Cl48 O52A 1.398(10) . ?
Cl48 O49A 1.493(11) . ?
Cl48 O49B 1.390(13) . ?
Cl48 O50B 1.405(12) . ?
Cl48 O51B 1.455(10) . ?
Cl48 O52B 1.471(11) . ?
Cl48 O51C 1.408(12) . ?
Cl48 O50C 1.411(11) . ?
Cl48 O52C 1.442(11) . ?
Cl48 O49C 1.458(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2A Fe1A N2A 176.6(2) 4_656 . ?
N2A Fe1A N9A 106.39(17) . 4_656 ?
N2A Fe1A N9A 76.05(17) . . ?
N9A Fe1A N9A 92.8(3) 4_656 . ?
N2A Fe1A N14A 101.56(16) . 4_656 ?
N9A Fe1A N14A 94.81(17) . 4_656 ?
N2A Fe1A N14A 75.98(15) . . ?
N9A Fe1A N14A 152.03(16) . . ?
N14A Fe1A N14A 91.0(2) 4_656 . ?
C7A N2A C3A 118.3(4) . . ?
C7A N2A Fe1A 120.7(3) . . ?
C3A N2A Fe1A 121.0(4) . . ?
N2A C3A C4A 123.3(5) . . ?
N2A C3A N8A 111.3(4) . . ?
C4A C3A N8A 125.4(5) . . ?
C3A C4A C5A 117.3(5) . . ?
C3A C4A H4A 121.4 . . ?
C5A C4A H4A 121.4 . . ?
C6A C5A C4A 119.8(5) . . ?
C6A C5A S18A 115.4(4) . . ?
C4A C5A S18A 124.8(4) . . ?
C7A C6A C5A 117.5(5) . . ?
C7A C6A H6A 121.2 . . ?
C5A C6A H6A 121.2 . . ?
N2A C7A C6A 123.7(5) . . ?
N2A C7A N13A 111.9(4) . . ?
C6A C7A N13A 124.4(5) . . ?
C12A N8A N9A 110.4(6) . . ?
C12A N8A C3A 131.0(6) . . ?
N9A N8A C3A 118.4(4) . . ?
C10A N9A N8A 105.4(6) . . ?
C10A N9A Fe1A 141.2(5) . . ?
N8A N9A Fe1A 113.2(3) . . ?
N9A C10A C11A 110.2(7) . . ?
N9A C10A H10A 124.9 . . ?
C11A C10A H10A 124.9 . . ?
C12A C11A C10A 107.7(6) . . ?
C12A C11A H11A 126.2 . . ?
C10A C11A H11A 126.2 . . ?
C11A C12A N8A 106.2(7) . . ?
C11A C12A H12A 126.9 . . ?
N8A C12A H12A 126.9 . . ?
C17A N13A N14A 111.3(4) . . ?
C17A N13A C7A 131.0(5) . . ?
N14A N13A C7A 117.7(4) . . ?
C15A N14A N13A 104.6(4) . . ?
C15A N14A Fe1A 141.5(4) . . ?
N13A N14A Fe1A 113.7(3) . . ?
N14A C15A C16A 111.5(5) . . ?
N14A C15A H15A 124.2 . . ?
C16A C15A H15A 124.2 . . ?
C17A C16A C15A 106.2(5) . . ?
C17A C16A H16A 126.9 . . ?
C15A C16A H16A 126.9 . . ?
N13A C17A C16A 106.4(6) . . ?
N13A C17A H17A 126.8 . . ?
C16A C17A H17A 126.8 . . ?
C5A S18A C19A 103.3(3) . . ?
S18A C19A H19A 109.5 . . ?
S18A C19A H19B 109.5 . . ?
H19A C19A H19B 109.5 . . ?
S18A C19A H19C 109.5 . . ?
H19A C19A H19C 109.5 . . ?
H19B C19A H19C 109.5 . . ?
N2B Fe1B N20B 174.88(18) . . ?
N2B Fe1B N14B 79.35(17) . . ?
N20B Fe1B N14B 105.42(16) . . ?
N2B Fe1B N32B 99.12(17) . . ?
N20B Fe1B N32B 79.05(16) . . ?
N14B Fe1B N32B 91.85(18) . . ?
N2B Fe1B N27B 102.92(17) . . ?
N20B Fe1B N27B 79.09(16) . . ?
N14B Fe1B N27B 90.97(17) . . ?
N32B Fe1B N27B 157.93(16) . . ?
N2B Fe1B N9B 79.11(17) . . ?
N20B Fe1B N9B 96.15(17) . . ?
N14B Fe1B N9B 158.42(17) . . ?
N32B Fe1B N9B 92.72(19) . . ?
N27B Fe1B N9B 92.66(18) . . ?
C7B N2B C3B 119.0(4) . . ?
C7B N2B Fe1B 121.0(3) . . ?
C3B N2B Fe1B 119.9(4) . . ?
N2B C3B C4B 123.1(5) . . ?
N2B C3B N8B 111.1(4) . . ?
C4B C3B N8B 125.8(5) . . ?
C3B C4B C5B 116.6(5) . . ?
C3B C4B H4B 121.7 . . ?
C5B C4B H4B 121.7 . . ?
C6B C5B C4B 121.2(5) . . ?
C6B C5B S18B 124.6(5) . . ?
C4B C5B S18B 114.2(4) . . ?
C7B C6B C5B 116.4(5) . . ?
C7B C6B H6B 121.8 . . ?
C5B C6B H6B 121.8 . . ?
N2B C7B C6B 123.7(5) . . ?
N2B C7B N13B 110.7(4) . . ?
C6B C7B N13B 125.6(5) . . ?
N9B N8B C12B 109.7(5) . . ?
N9B N8B C3B 116.7(4) . . ?
C12B N8B C3B 133.6(5) . . ?
C10B N9B N8B 105.5(5) . . ?
C10B N9B Fe1B 141.4(4) . . ?
N8B N9B Fe1B 113.1(3) . . ?
N9B C10B C11B 110.5(6) . . ?
N9B C10B H10B 124.8 . . ?
C11B C10B H10B 124.8 . . ?
C12B C11B C10B 106.8(6) . . ?
C12B C11B H11B 126.6 . . ?
C10B C11B H11B 126.6 . . ?
C11B C12B N8B 107.5(6) . . ?
C11B C12B H12B 126.3 . . ?
N8B C12B H12B 126.3 . . ?
C17B N13B N14B 110.4(5) . . ?
C17B N13B C7B 133.5(5) . . ?
N14B N13B C7B 116.1(4) . . ?
C15B N14B N13B 105.6(4) . . ?
C15B N14B Fe1B 141.6(4) . . ?
N13B N14B Fe1B 112.8(3) . . ?
N14B C15B C16B 110.4(5) . . ?
N14B C15B H15B 124.8 . . ?
C16B C15B H15B 124.8 . . ?
C17B C16B C15B 106.5(6) . . ?
C17B C16B H16B 126.8 . . ?
C15B C16B H16B 126.8 . . ?
N13B C17B C16B 107.1(6) . . ?
N13B C17B H17B 126.4 . . ?
C16B C17B H17B 126.4 . . ?
C19B S18B C5B 102.2(3) . . ?
C21B N20B C25B 119.3(4) . . ?
C21B N20B Fe1B 120.1(3) . . ?
C25B N20B Fe1B 120.2(3) . . ?
N20B C21B C22B 123.4(5) . . ?
N20B C21B N26B 110.9(4) . . ?
C22B C21B N26B 125.7(5) . . ?
C21B C22B C23B 116.0(5) . . ?
C21B C22B H22B 122.0 . . ?
C23B C22B H22B 122.0 . . ?
C24B C23B C22B 121.4(5) . . ?
C24B C23B S36B 115.3(5) . . ?
C22B C23B S36B 123.3(5) . . ?
C25B C24B C23B 116.9(5) . . ?
C25B C24B H24B 121.6 . . ?
C23B C24B H24B 121.6 . . ?
N20B C25B C24B 123.0(5) . . ?
N20B C25B N31B 111.2(4) . . ?
C24B C25B N31B 125.8(5) . . ?
C30B N26B N27B 110.6(5) . . ?
C30B N26B C21B 132.4(5) . . ?
N27B N26B C21B 116.7(4) . . ?
C28B N27B N26B 106.3(4) . . ?
C28B N27B Fe1B 140.7(4) . . ?
N26B N27B Fe1B 112.8(3) . . ?
N27B C28B C29B 110.1(5) . . ?
N27B C28B H28B 124.9 . . ?
C29B C28B H28B 124.9 . . ?
C30B C29B C28B 106.4(5) . . ?
C30B C29B H29B 126.8 . . ?
C28B C29B H29B 126.8 . . ?
N26B C30B C29B 106.6(5) . . ?
N26B C30B H30B 126.7 . . ?
C29B C30B H30B 126.7 . . ?
C35B N31B N32B 111.1(4) . . ?
C35B N31B C25B 132.8(5) . . ?
N32B N31B C25B 116.1(4) . . ?
C33B N32B N31B 104.8(4) . . ?
C33B N32B Fe1B 142.0(4) . . ?
N31B N32B Fe1B 113.1(3) . . ?
N32B C33B C34B 110.5(5) . . ?
N32B C33B H33B 124.8 . . ?
C34B C33B H33B 124.8 . . ?
C35B C34B C33B 106.8(5) . . ?
C35B C34B H34B 126.6 . . ?
C33B C34B H34B 126.6 . . ?
N31B C35B C34B 106.9(6) . . ?
N31B C35B H35B 126.5 . . ?
C34B C35B H35B 126.5 . . ?
C23B S36B C37B 103.2(4) . . ?
O39A Cl3A O41A 116.8(15) . . ?
O39A Cl3A O40A 115.1(13) . . ?
O41A Cl3A O40A 93.9(12) . . ?
O39A Cl3A O42A 114.0(12) . . ?
O41A Cl3A O42A 108.4(11) . . ?
O40A Cl3A O42A 106.5(11) . . ?
O42B Cl3B O40B 116.1(12) . . ?
O42B Cl3B O41B 99.3(14) . . ?
O40B Cl3B O41B 117.5(13) . . ?
O42B Cl3B O39B 108.6(11) . . ?
O40B Cl3B O39B 105.7(10) . . ?
O41B Cl3B O39B 109.2(14) . . ?
O42C Cl3C O39C 120.0(19) . . ?
O42C Cl3C O40C 118.0(18) . . ?
O39C Cl3C O40C 107.5(18) . . ?
O42C Cl3C O41C 107.4(18) . . ?
O39C Cl3C O41C 100.0(17) . . ?
O40C Cl3C O41C 100.6(16) . . ?
O46A Cl4A O47A 113.5(8) . . ?
O46A Cl4A O45A 108.8(8) . . ?
O47A Cl4A O45A 113.5(7) . . ?
O46A Cl4A O44A 110.1(8) . . ?
O47A Cl4A O44A 104.6(8) . . ?
O45A Cl4A O44A 105.8(8) . . ?
O45B Cl4B O47B 114.1(14) . . ?
O45B Cl4B O44B 106.1(13) . . ?
O47B Cl4B O44B 108.2(13) . . ?
O45B Cl4B O46B 112.0(13) . . ?
O47B Cl4B O46B 107.4(13) . . ?
O44B Cl4B O46B 108.9(14) . . ?
O50A Cl48 O52A 116.4(10) . . ?
O50A Cl48 O51A 111.7(9) . . ?
O52A Cl48 O51A 110.8(8) . . ?
O50A Cl48 O49A 106.1(9) . . ?
O52A Cl48 O49A 108.0(8) . . ?
O51A Cl48 O49A 102.7(8) . . ?
O49B Cl48 O50B 118.4(11) . . ?
O49B Cl48 O51B 110.4(11) . . ?
O50B Cl48 O51B 106.3(9) . . ?
O49B Cl48 O52B 105.4(11) . . ?
O50B Cl48 O52B 109.2(9) . . ?
O51B Cl48 O52B 106.7(7) . . ?
O51C Cl48 O50C 111.6(10) . . ?
O51C Cl48 O52C 111.1(10) . . ?
O50C Cl48 O52C 109.9(9) . . ?
O51C Cl48 O49C 110.7(10) . . ?
O50C Cl48 O49C 108.3(9) . . ?
O52C Cl48 O49C 104.9(8) . . ?

_diffrn_measured_fraction_theta_max 0.955
_diffrn_reflns_theta_full        73.84
_diffrn_measured_fraction_theta_full 0.955
_refine_diff_density_max         1.419
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.100
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: nitromethane/diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lkc266mt
_database_code_depnum_ccdc_archive 'CCDC 1060843'
_audit_update_record             
;
2015-04-21 deposited with the CCDC.
2015-06-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
Bis[2,6-di(pyrazol-1-yl)4-methylsulfanylpyridine]iron(II)diperchlorate
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H22 Fe N10 S2, 2[Cl O4]'
_chemical_formula_sum            'C24 H22 Cl2 Fe N10 O8 S2'
_chemical_formula_weight         769.39

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   16.3532(4)
_cell_length_b                   17.2208(5)
_cell_length_c                   21.9658(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6185.9(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    240(2)
_cell_measurement_reflns_used    7025
_cell_measurement_theta_min      3.33
_cell_measurement_theta_max      73.42

_exptl_crystal_description       fragment
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3136
_exptl_absorpt_coefficient_mu    7.340
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.553
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28e (release 10-06-2013 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      240(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            17806
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0681
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.26
_diffrn_reflns_theta_max         74.29
_reflns_number_total             10969
_reflns_number_gt                7684
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The crystal refined as a racemic twin. Although the Flack parameter is 
 close to 0.5, ADSYMM and NEWSYMM analyses both supported this choice of 
 space group.

 The asymmetric unit contains two formula units (Z' = 2), with all cations 
 and anions lying on general crystallographic sites. All four of the unique 
 perchlorate ions are disordered over two orientations. Three of these were 
 modelled with equally ordered disorder sites, and the fourth with a 
 0.75:0.25 occupancy ratio. The refined restraints Cl---O = 1.43(2) and 
 O...O = 2.34(2) Å were applied to the partial anions. All 
 crystallographically ordered non-H atoms were refined anisotropically, 
 while H atoms were placed in calculated positions and refined using a 
 riding model.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0877P)²+0.8594P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.462(7)
_refine_ls_number_reflns         10969
_refine_ls_number_parameters     833
_refine_ls_number_restraints     80
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0576
_refine_ls_wR_factor_ref         0.1628
_refine_ls_wR_factor_gt          0.1432
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1A Fe 0.77029(6) 0.50412(5) 0.69192(5) 0.0328(2) Uani 1 1 d . . .
N2A N 0.7860(3) 0.6131(3) 0.6843(3) 0.0365(12) Uani 1 1 d . . .
C3A C 0.8439(4) 0.6404(4) 0.6464(3) 0.0382(15) Uani 1 1 d . . .
C4A C 0.8544(4) 0.7186(4) 0.6369(3) 0.0429(16) Uani 1 1 d . . .
H4A H 0.8947 0.7371 0.6100 0.051 Uiso 1 1 calc R . .
C5A C 0.8034(4) 0.7699(4) 0.6684(4) 0.0446(17) Uani 1 1 d . . .
C6A C 0.7434(4) 0.7422(4) 0.7089(3) 0.0434(17) Uani 1 1 d . . .
H6A H 0.7086 0.7758 0.7305 0.052 Uiso 1 1 calc R . .
C7A C 0.7391(4) 0.6626(4) 0.7145(3) 0.0388(15) Uani 1 1 d . . .
N8A N 0.8875(3) 0.5801(3) 0.6199(3) 0.0423(13) Uani 1 1 d . . .
N9A N 0.8625(3) 0.5055(3) 0.6334(3) 0.0395(12) Uani 1 1 d . . .
C10A C 0.9102(4) 0.4580(5) 0.6021(3) 0.0471(18) Uani 1 1 d . . .
H10A H 0.9065 0.4036 0.6020 0.056 Uiso 1 1 calc R . .
C11A C 0.9675(5) 0.5019(5) 0.5690(4) 0.0559(19) Uani 1 1 d . . .
H11A H 1.0088 0.4823 0.5435 0.067 Uiso 1 1 calc R . .
C12A C 0.9519(4) 0.5782(5) 0.5807(4) 0.0515(19) Uani 1 1 d . . .
H12A H 0.9801 0.6212 0.5647 0.062 Uiso 1 1 calc R . .
N13A N 0.6836(3) 0.6213(3) 0.7524(3) 0.0397(13) Uani 1 1 d . . .
N14A N 0.6875(3) 0.5419(3) 0.7496(3) 0.0394(13) Uani 1 1 d . . .
C15A C 0.6355(4) 0.5171(4) 0.7912(3) 0.0427(17) Uani 1 1 d . . .
H15A H 0.6251 0.4644 0.7996 0.051 Uiso 1 1 calc R . .
C16A C 0.5982(4) 0.5785(5) 0.8207(4) 0.0519(19) Uani 1 1 d . . .
H16A H 0.5588 0.5756 0.8518 0.062 Uiso 1 1 calc R . .
C17A C 0.6300(4) 0.6440(5) 0.7958(3) 0.0461(17) Uani 1 1 d . . .
H17A H 0.6173 0.6953 0.8067 0.055 Uiso 1 1 calc R . .
S18A S 0.82048(14) 0.86848(11) 0.65550(12) 0.0650(6) Uani 1 1 d . . .
C19A C 0.7481(5) 0.9155(4) 0.7040(5) 0.065(2) Uani 1 1 d . . .
H19A H 0.6933 0.9064 0.6887 0.098 Uiso 1 1 calc R . .
H19B H 0.7589 0.9709 0.7046 0.098 Uiso 1 1 calc R . .
H19C H 0.7528 0.8948 0.7449 0.098 Uiso 1 1 calc R . .
N20A N 0.7514(3) 0.3952(3) 0.6989(3) 0.0355(12) Uani 1 1 d . . .
C21A C 0.6992(4) 0.3593(4) 0.6620(3) 0.0369(14) Uani 1 1 d . . .
C22A C 0.6832(4) 0.2808(4) 0.6658(3) 0.0407(16) Uani 1 1 d . . .
H22A H 0.6468 0.2564 0.6388 0.049 Uiso 1 1 calc R . .
C23A C 0.7233(4) 0.2391(4) 0.7112(4) 0.0433(17) Uani 1 1 d . . .
C24A C 0.7788(4) 0.2768(4) 0.7496(3) 0.0426(16) Uani 1 1 d . . .
H24A H 0.8074 0.2492 0.7798 0.051 Uiso 1 1 calc R . .
C25A C 0.7904(4) 0.3540(3) 0.7422(3) 0.0391(15) Uani 1 1 d . . .
N26A N 0.6623(3) 0.4130(3) 0.6221(3) 0.0412(13) Uani 1 1 d . . .
N27A N 0.6882(3) 0.4885(3) 0.6266(2) 0.0393(12) Uani 1 1 d . . .
C28A C 0.6456(4) 0.5271(4) 0.5850(4) 0.0485(18) Uani 1 1 d . . .
H28A H 0.6498 0.5807 0.5774 0.058 Uiso 1 1 calc R . .
C29A C 0.5927(5) 0.4755(5) 0.5536(4) 0.055(2) Uani 1 1 d . . .
H29A H 0.5564 0.4883 0.5220 0.066 Uiso 1 1 calc R . .
C30A C 0.6044(4) 0.4046(5) 0.5780(4) 0.0498(18) Uani 1 1 d . . .
H30A H 0.5779 0.3584 0.5668 0.060 Uiso 1 1 calc R . .
N31A N 0.8411(3) 0.4018(3) 0.7764(3) 0.0386(13) Uani 1 1 d . . .
N32A N 0.8441(3) 0.4792(3) 0.7608(3) 0.0371(12) Uani 1 1 d . . .
C33A C 0.8938(4) 0.5115(4) 0.8008(3) 0.0462(17) Uani 1 1 d . . .
H33A H 0.9089 0.5642 0.8008 0.055 Uiso 1 1 calc R . .
C34A C 0.9211(6) 0.4566(5) 0.8432(4) 0.064(2) Uani 1 1 d . . .
H34A H 0.9556 0.4655 0.8767 0.076 Uiso 1 1 calc R . .
C35A C 0.8878(5) 0.3884(5) 0.8261(4) 0.059(2) Uani 1 1 d . . .
H35A H 0.8957 0.3401 0.8453 0.070 Uiso 1 1 calc R . .
S36A S 0.70890(13) 0.14002(10) 0.72388(12) 0.0606(6) Uani 1 1 d . . .
C37A C 0.6178(5) 0.1193(5) 0.6827(4) 0.067(2) Uani 1 1 d . . .
H37A H 0.5793 0.1617 0.6879 0.101 Uiso 1 1 calc R . .
H37B H 0.5937 0.0717 0.6979 0.101 Uiso 1 1 calc R . .
H37C H 0.6306 0.1134 0.6398 0.101 Uiso 1 1 calc R . .
Fe1B Fe 0.26618(6) 0.50606(5) 0.56216(5) 0.0332(2) Uani 1 1 d . . .
N2B N 0.2804(3) 0.6154(3) 0.5547(2) 0.0331(12) Uani 1 1 d . . .
C3B C 0.3352(4) 0.6534(4) 0.5883(3) 0.0405(16) Uani 1 1 d . . .
C4B C 0.3452(4) 0.7313(4) 0.5862(3) 0.0428(16) Uani 1 1 d . . .
H4B H 0.3836 0.7563 0.6114 0.051 Uiso 1 1 calc R . .
C5B C 0.2970(4) 0.7732(4) 0.5458(4) 0.0447(17) Uani 1 1 d . . .
C6B C 0.2395(4) 0.7348(4) 0.5097(4) 0.0425(16) Uani 1 1 d . . .
H6B H 0.2062 0.7622 0.4822 0.051 Uiso 1 1 calc R . .
C7B C 0.2330(4) 0.6553(4) 0.5156(3) 0.0376(14) Uani 1 1 d . . .
N8B N 0.3795(3) 0.5998(3) 0.6236(3) 0.0420(14) Uani 1 1 d . . .
N9B N 0.3578(3) 0.5233(3) 0.6203(3) 0.0413(13) Uani 1 1 d . . .
C10B C 0.4098(4) 0.4857(5) 0.6560(4) 0.0511(18) Uani 1 1 d . . .
H10B H 0.4094 0.4319 0.6633 0.061 Uiso 1 1 calc R . .
C11B C 0.4651(5) 0.5382(5) 0.6809(4) 0.057(2) Uani 1 1 d . . .
H11B H 0.5078 0.5265 0.7081 0.068 Uiso 1 1 calc R . .
C12B C 0.4461(4) 0.6093(5) 0.6589(3) 0.0510(19) Uani 1 1 d . . .
H12B H 0.4738 0.6561 0.6667 0.061 Uiso 1 1 calc R . .
N13B N 0.1798(3) 0.6062(3) 0.4844(3) 0.0397(13) Uani 1 1 d . . .
N14B N 0.1864(3) 0.5285(3) 0.4979(3) 0.0390(13) Uani 1 1 d . . .
C15B C 0.1363(4) 0.4933(4) 0.4598(3) 0.0416(15) Uani 1 1 d . . .
H15B H 0.1267 0.4395 0.4585 0.050 Uiso 1 1 calc R . .
C16B C 0.0993(4) 0.5484(4) 0.4214(4) 0.0484(18) Uani 1 1 d . . .
H16B H 0.0621 0.5381 0.3898 0.058 Uiso 1 1 calc R . .
C17B C 0.1267(4) 0.6174(4) 0.4382(4) 0.0454(17) Uani 1 1 d . . .
H17B H 0.1119 0.6654 0.4211 0.055 Uiso 1 1 calc R . .
S18B S 0.30185(13) 0.87383(11) 0.53515(13) 0.0674(6) Uani 1 1 d . . .
C19B C 0.3970(5) 0.8983(4) 0.5707(4) 0.061(2) Uani 1 1 d . . .
H19D H 0.3920 0.8925 0.6144 0.092 Uiso 1 1 calc R . .
H19E H 0.4111 0.9516 0.5610 0.092 Uiso 1 1 calc R . .
H19F H 0.4396 0.8639 0.5558 0.092 Uiso 1 1 calc R . .
N20B N 0.2478(3) 0.3977(3) 0.5696(3) 0.0358(12) Uani 1 1 d . . .
C21B C 0.1918(4) 0.3710(4) 0.6097(3) 0.0392(15) Uani 1 1 d . . .
C22B C 0.1762(4) 0.2940(4) 0.6164(3) 0.0451(17) Uani 1 1 d . . .
H22B H 0.1375 0.2764 0.6449 0.054 Uiso 1 1 calc R . .
C23B C 0.2193(4) 0.2413(4) 0.5798(4) 0.0458(18) Uani 1 1 d . . .
C24B C 0.2763(4) 0.2680(4) 0.5376(4) 0.0457(17) Uani 1 1 d . . .
H24B H 0.3057 0.2338 0.5125 0.055 Uiso 1 1 calc R . .
C25B C 0.2871(4) 0.3467(4) 0.5346(3) 0.0382(15) Uani 1 1 d . . .
N26B N 0.1563(3) 0.4319(3) 0.6411(3) 0.0408(13) Uani 1 1 d . . .
N27B N 0.1821(3) 0.5058(3) 0.6271(2) 0.0412(13) Uani 1 1 d . . .
C28B C 0.1404(5) 0.5527(5) 0.6637(4) 0.0517(19) Uani 1 1 d . . .
H28B H 0.1455 0.6070 0.6643 0.062 Uiso 1 1 calc R . .
C29B C 0.0876(4) 0.5099(5) 0.7011(4) 0.058(2) Uani 1 1 d . . .
H29B H 0.0517 0.5299 0.7307 0.070 Uiso 1 1 calc R . .
C30B C 0.0983(4) 0.4343(5) 0.6865(4) 0.0500(18) Uani 1 1 d . . .
H30B H 0.0714 0.3916 0.7040 0.060 Uiso 1 1 calc R . .
N31B N 0.3403(3) 0.3863(3) 0.4942(3) 0.0422(13) Uani 1 1 d . . .
N32B N 0.3427(3) 0.4666(3) 0.4997(3) 0.0380(12) Uani 1 1 d . . .
C33B C 0.3918(4) 0.4890(4) 0.4559(3) 0.0466(17) Uani 1 1 d . . .
H33B H 0.4065 0.5409 0.4485 0.056 Uiso 1 1 calc R . .
C34B C 0.4196(6) 0.4253(5) 0.4213(4) 0.065(2) Uani 1 1 d . . .
H34B H 0.4542 0.4268 0.3872 0.078 Uiso 1 1 calc R . .
C35B C 0.3867(5) 0.3625(4) 0.4472(4) 0.060(2) Uani 1 1 d . . .
H35B H 0.3946 0.3109 0.4348 0.072 Uiso 1 1 calc R . .
S36B S 0.19670(14) 0.14287(11) 0.59063(12) 0.0658(6) Uani 1 1 d . . .
C37B C 0.2646(5) 0.0946(4) 0.5401(5) 0.073(3) Uani 1 1 d . . .
H37D H 0.2515 0.1087 0.4985 0.109 Uiso 1 1 calc R . .
H37E H 0.2591 0.0389 0.5452 0.109 Uiso 1 1 calc R . .
H37F H 0.3204 0.1099 0.5492 0.109 Uiso 1 1 calc R . .
Cl38A Cl 0.4923(3) 0.3279(3) 0.7713(2) 0.053(2) Uiso 0.75 1 d PD A 1
O39A O 0.5788(5) 0.3205(5) 0.7851(4) 0.072(2) Uiso 0.75 1 d PD A 1
O40A O 0.4710(6) 0.4073(4) 0.7890(4) 0.058(2) Uiso 0.75 1 d PD A 1
O42A O 0.4481(6) 0.2749(6) 0.8107(5) 0.087(3) Uiso 0.75 1 d PD A 1
O41A O 0.4787(6) 0.3140(5) 0.7107(4) 0.082(3) Uiso 0.75 1 d PD A 1
Cl38B Cl 0.4888(8) 0.3334(8) 0.7773(6) 0.042(5) Uiso 0.25 1 d PD B 2
O39B O 0.5627(13) 0.296(2) 0.7600(15) 0.161(19) Uiso 0.25 1 d PD B 2
O40B O 0.494(2) 0.4129(12) 0.7874(17) 0.19(3) Uiso 0.25 1 d PD B 2
O41B O 0.4298(10) 0.3206(10) 0.7258(7) 0.041(4) Uiso 0.25 1 d PD B 2
O42B O 0.4557(16) 0.2938(17) 0.8296(9) 0.081(10) Uiso 0.25 1 d PD B 2
Cl43A Cl 0.5281(4) 0.6930(4) 0.4903(3) 0.043(3) Uiso 0.50 1 d PD C 1
O44A O 0.5942(8) 0.6452(8) 0.4642(6) 0.070(4) Uiso 0.50 1 d PD C 1
O45A O 0.5476(9) 0.6970(8) 0.5529(5) 0.069(4) Uiso 0.50 1 d PD C 1
O46A O 0.5374(9) 0.7681(6) 0.4631(6) 0.074(4) Uiso 0.50 1 d PD C 1
O47A O 0.4527(8) 0.6595(10) 0.4792(8) 0.099(7) Uiso 0.50 1 d PD C 1
Cl43B Cl 0.5297(5) 0.6946(4) 0.4824(3) 0.045(3) Uiso 0.50 1 d PD D 2
O44B O 0.5766(9) 0.6268(7) 0.4718(7) 0.078(5) Uiso 0.50 1 d PD D 2
O45B O 0.5350(9) 0.7183(9) 0.5444(5) 0.076(5) Uiso 0.50 1 d PD D 2
O46B O 0.5571(8) 0.7549(7) 0.4425(6) 0.070(4) Uiso 0.50 1 d PD D 2
O47B O 0.4443(6) 0.6797(9) 0.4707(7) 0.062(4) Uiso 0.50 1 d PD D 2
Cl48A Cl 0.5051(4) 0.1886(3) 0.5314(3) 0.0495(19) Uiso 0.50 1 d PD E 1
O49A O 0.5915(6) 0.1946(9) 0.5206(7) 0.067(5) Uiso 0.50 1 d PD E 1
O50A O 0.4891(9) 0.1108(7) 0.5529(7) 0.064(5) Uiso 0.50 1 d PD E 1
O51A O 0.4748(8) 0.2425(7) 0.5743(6) 0.075(4) Uiso 0.50 1 d PD E 1
O52A O 0.4614(9) 0.1956(8) 0.4740(5) 0.082(4) Uiso 0.50 1 d PD E 1
Cl48B Cl 0.5107(3) 0.1983(3) 0.5227(3) 0.0444(17) Uiso 0.50 1 d PD F 2
O49B O 0.5979(6) 0.2032(7) 0.5379(6) 0.050(3) Uiso 0.50 1 d PD F 2
O50B O 0.4816(10) 0.1292(8) 0.5517(8) 0.075(6) Uiso 0.50 1 d PD F 2
O51B O 0.4755(7) 0.2652(6) 0.5510(5) 0.056(3) Uiso 0.50 1 d PD F 2
O52B O 0.4960(7) 0.1972(7) 0.4610(4) 0.060(3) Uiso 0.50 1 d PD F 2
Cl53A Cl 0.0088(4) 0.7159(4) 0.7637(3) 0.046(2) Uiso 0.50 1 d PD G 1
O54A O 0.0352(10) 0.7831(8) 0.7992(7) 0.092(6) Uiso 0.50 1 d PD G 1
O55A O 0.0337(7) 0.7134(7) 0.7045(4) 0.041(3) Uiso 0.50 1 d PD G 1
O56A O 0.0411(9) 0.6517(7) 0.7997(6) 0.078(4) Uiso 0.50 1 d PD G 1
O57A O -0.0796(6) 0.7095(8) 0.7691(6) 0.057(4) Uiso 0.50 1 d PD G 1
Cl53B Cl 0.0129(4) 0.7189(4) 0.7719(3) 0.046(2) Uiso 0.50 1 d PD H 2
O54B O 0.0230(8) 0.7975(6) 0.7843(6) 0.062(4) Uiso 0.50 1 d PD H 2
O55B O 0.0279(16) 0.7102(14) 0.7052(6) 0.162(14) Uiso 0.50 1 d PD H 2
O56B O 0.0703(8) 0.6695(8) 0.7996(7) 0.080(4) Uiso 0.50 1 d PD H 2
O57B O -0.0697(6) 0.6907(7) 0.7808(6) 0.055(4) Uiso 0.50 1 d PD H 2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1A N2A 1.902(5) . ?
Fe1A N20A 1.908(5) . ?
Fe1A N14A 1.966(6) . ?
Fe1A N9A 1.982(5) . ?
Fe1A N32A 1.982(6) . ?
Fe1A N27A 1.983(6) . ?
N2A C7A 1.325(8) . ?
N2A C3A 1.346(8) . ?
C3A C4A 1.374(9) . ?
C3A N8A 1.388(9) . ?
C4A C5A 1.398(10) . ?
C4A H4A 0.9400 . ?
C5A C6A 1.407(10) . ?
C5A S18A 1.744(7) . ?
C6A C7A 1.379(9) . ?
C6A H6A 0.9400 . ?
C7A N13A 1.420(8) . ?
N8A C12A 1.362(9) . ?
N8A N9A 1.380(8) . ?
N9A C10A 1.323(8) . ?
C10A C11A 1.406(11) . ?
C10A H10A 0.9400 . ?
C11A C12A 1.364(11) . ?
C11A H11A 0.9400 . ?
C12A H12A 0.9400 . ?
N13A C17A 1.354(9) . ?
N13A N14A 1.371(8) . ?
N14A C15A 1.318(8) . ?
C15A C16A 1.384(10) . ?
C15A H15A 0.9400 . ?
C16A C17A 1.356(11) . ?
C16A H16A 0.9400 . ?
C17A H17A 0.9400 . ?
S18A C19A 1.786(9) . ?
C19A H19A 0.9700 . ?
C19A H19B 0.9700 . ?
C19A H19C 0.9700 . ?
N20A C21A 1.330(8) . ?
N20A C25A 1.347(8) . ?
C21A C22A 1.379(9) . ?
C21A N26A 1.410(9) . ?
C22A C23A 1.393(10) . ?
C22A H22A 0.9400 . ?
C23A C24A 1.398(10) . ?
C23A S36A 1.745(7) . ?
C24A C25A 1.353(9) . ?
C24A H24A 0.9400 . ?
C25A N31A 1.389(8) . ?
N26A C30A 1.361(9) . ?
N26A N27A 1.372(8) . ?
N27A C28A 1.329(9) . ?
C28A C29A 1.418(11) . ?
C28A H28A 0.9400 . ?
C29A C30A 1.347(11) . ?
C29A H29A 0.9400 . ?
C30A H30A 0.9400 . ?
N31A C35A 1.353(9) . ?
N31A N32A 1.378(7) . ?
N32A C33A 1.319(9) . ?
C33A C34A 1.401(11) . ?
C33A H33A 0.9400 . ?
C34A C35A 1.348(11) . ?
C34A H34A 0.9400 . ?
C35A H35A 0.9400 . ?
S36A C37A 1.780(8) . ?
C37A H37A 0.9700 . ?
C37A H37B 0.9700 . ?
C37A H37C 0.9700 . ?
Fe1B N20B 1.898(5) . ?
Fe1B N2B 1.904(5) . ?
Fe1B N14B 1.961(6) . ?
Fe1B N32B 1.978(6) . ?
Fe1B N27B 1.982(6) . ?
Fe1B N9B 1.992(6) . ?
N2B C3B 1.334(8) . ?
N2B C7B 1.345(8) . ?
C3B C4B 1.351(10) . ?
C3B N8B 1.406(9) . ?
C4B C5B 1.390(10) . ?
C4B H4B 0.9400 . ?
C5B C6B 1.398(10) . ?
C5B S18B 1.750(7) . ?
C6B C7B 1.379(9) . ?
C6B H6B 0.9400 . ?
C7B N13B 1.393(8) . ?
N8B C12B 1.347(9) . ?
N8B N9B 1.366(8) . ?
N9B C10B 1.325(9) . ?
C10B C11B 1.391(11) . ?
C10B H10B 0.9400 . ?
C11B C12B 1.352(11) . ?
C11B H11B 0.9400 . ?
C12B H12B 0.9400 . ?
N13B C17B 1.350(9) . ?
N13B N14B 1.375(7) . ?
N14B C15B 1.319(9) . ?
C15B C16B 1.405(10) . ?
C15B H15B 0.9400 . ?
C16B C17B 1.323(10) . ?
C16B H16B 0.9400 . ?
C17B H17B 0.9400 . ?
S18B C19B 1.791(8) . ?
C19B H19D 0.9700 . ?
C19B H19E 0.9700 . ?
C19B H19F 0.9700 . ?
N20B C25B 1.333(9) . ?
N20B C21B 1.351(8) . ?
C21B C22B 1.359(10) . ?
C21B N26B 1.383(9) . ?
C22B C23B 1.403(11) . ?
C22B H22B 0.9400 . ?
C23B C24B 1.392(11) . ?
C23B S36B 1.751(7) . ?
C24B C25B 1.368(9) . ?
C24B H24B 0.9400 . ?
C25B N31B 1.418(9) . ?
N26B N27B 1.375(8) . ?
N26B C30B 1.377(9) . ?
N27B C28B 1.327(9) . ?
C28B C29B 1.402(11) . ?
C28B H28B 0.9400 . ?
C29B C30B 1.353(11) . ?
C29B H29B 0.9400 . ?
C30B H30B 0.9400 . ?
N31B C35B 1.344(10) . ?
N31B N32B 1.389(8) . ?
N32B C33B 1.311(9) . ?
C33B C34B 1.408(11) . ?
C33B H33B 0.9400 . ?
C34B C35B 1.335(11) . ?
C34B H34B 0.9400 . ?
C35B H35B 0.9400 . ?
S36B C37B 1.776(10) . ?
C37B H37D 0.9700 . ?
C37B H37E 0.9700 . ?
C37B H37F 0.9700 . ?
Cl38A O41A 1.372(8) . ?
Cl38A O42A 1.449(9) . ?
Cl38A O39A 1.453(8) . ?
Cl38A O40A 1.464(8) . ?
Cl38B O40B 1.390(16) . ?
Cl38B O39B 1.424(16) . ?
Cl38B O42B 1.443(15) . ?
Cl38B O41B 1.503(15) . ?
Cl43A O47A 1.383(12) . ?
Cl43A O45A 1.413(11) . ?
Cl43A O46A 1.434(11) . ?
Cl43A O44A 1.474(11) . ?
Cl43B O44B 1.415(11) . ?
Cl43B O45B 1.426(12) . ?
Cl43B O46B 1.431(11) . ?
Cl43B O47B 1.444(11) . ?
Cl48A O51A 1.411(10) . ?
Cl48A O49A 1.436(11) . ?
Cl48A O50A 1.445(11) . ?
Cl48A O52A 1.455(11) . ?
Cl48B O52B 1.377(10) . ?
Cl48B O51B 1.430(10) . ?
Cl48B O50B 1.431(12) . ?
Cl48B O49B 1.466(10) . ?
Cl53A O55A 1.363(10) . ?
Cl53A O57A 1.455(11) . ?
Cl53A O56A 1.459(11) . ?
Cl53A O54A 1.460(12) . ?
Cl53B O54B 1.390(11) . ?
Cl53B O56B 1.406(11) . ?
Cl53B O57B 1.449(11) . ?
Cl53B O55B 1.492(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2A Fe1A N20A 178.4(2) . . ?
N2A Fe1A N14A 79.8(2) . . ?
N20A Fe1A N14A 99.3(2) . . ?
N2A Fe1A N9A 80.1(2) . . ?
N20A Fe1A N9A 100.8(2) . . ?
N14A Fe1A N9A 159.8(2) . . ?
N2A Fe1A N32A 101.4(2) . . ?
N20A Fe1A N32A 79.9(2) . . ?
N14A Fe1A N32A 89.9(2) . . ?
N9A Fe1A N32A 92.0(2) . . ?
N2A Fe1A N27A 99.3(2) . . ?
N20A Fe1A N27A 79.3(2) . . ?
N14A Fe1A N27A 92.6(2) . . ?
N9A Fe1A N27A 92.7(2) . . ?
N32A Fe1A N27A 159.2(2) . . ?
C7A N2A C3A 119.5(6) . . ?
C7A N2A Fe1A 120.8(4) . . ?
C3A N2A Fe1A 119.6(4) . . ?
N2A C3A C4A 121.6(6) . . ?
N2A C3A N8A 111.0(6) . . ?
C4A C3A N8A 127.3(6) . . ?
C3A C4A C5A 118.0(7) . . ?
C3A C4A H4A 121.0 . . ?
C5A C4A H4A 121.0 . . ?
C4A C5A C6A 121.0(6) . . ?
C4A C5A S18A 116.0(6) . . ?
C6A C5A S18A 123.0(6) . . ?
C7A C6A C5A 115.4(7) . . ?
C7A C6A H6A 122.3 . . ?
C5A C6A H6A 122.3 . . ?
N2A C7A C6A 124.4(7) . . ?
N2A C7A N13A 109.9(5) . . ?
C6A C7A N13A 125.7(6) . . ?
C12A N8A N9A 110.1(6) . . ?
C12A N8A C3A 132.8(7) . . ?
N9A N8A C3A 117.1(5) . . ?
C10A N9A N8A 106.8(6) . . ?
C10A N9A Fe1A 141.2(5) . . ?
N8A N9A Fe1A 112.0(4) . . ?
N9A C10A C11A 109.3(7) . . ?
N9A C10A H10A 125.4 . . ?
C11A C10A H10A 125.4 . . ?
C12A C11A C10A 107.2(6) . . ?
C12A C11A H11A 126.4 . . ?
C10A C11A H11A 126.4 . . ?
N8A C12A C11A 106.7(7) . . ?
N8A C12A H12A 126.7 . . ?
C11A C12A H12A 126.7 . . ?
C17A N13A N14A 110.3(6) . . ?
C17A N13A C7A 133.0(6) . . ?
N14A N13A C7A 116.4(5) . . ?
C15A N14A N13A 105.3(6) . . ?
C15A N14A Fe1A 141.6(5) . . ?
N13A N14A Fe1A 112.9(4) . . ?
N14A C15A C16A 111.1(7) . . ?
N14A C15A H15A 124.4 . . ?
C16A C15A H15A 124.4 . . ?
C17A C16A C15A 106.1(6) . . ?
C17A C16A H16A 127.0 . . ?
C15A C16A H16A 127.0 . . ?
N13A C17A C16A 107.1(7) . . ?
N13A C17A H17A 126.5 . . ?
C16A C17A H17A 126.5 . . ?
C5A S18A C19A 103.8(4) . . ?
S18A C19A H19A 109.5 . . ?
S18A C19A H19B 109.5 . . ?
H19A C19A H19B 109.5 . . ?
S18A C19A H19C 109.5 . . ?
H19A C19A H19C 109.5 . . ?
H19B C19A H19C 109.5 . . ?
C21A N20A C25A 119.4(5) . . ?
C21A N20A Fe1A 120.8(4) . . ?
C25A N20A Fe1A 119.8(4) . . ?
N20A C21A C22A 122.7(6) . . ?
N20A C21A N26A 110.4(5) . . ?
C22A C21A N26A 126.8(6) . . ?
C21A C22A C23A 117.3(6) . . ?
C21A C22A H22A 121.3 . . ?
C23A C22A H22A 121.3 . . ?
C22A C23A C24A 119.9(6) . . ?
C22A C23A S36A 123.7(5) . . ?
C24A C23A S36A 116.5(5) . . ?
C25A C24A C23A 118.4(7) . . ?
C25A C24A H24A 120.8 . . ?
C23A C24A H24A 120.8 . . ?
N20A C25A C24A 122.4(6) . . ?
N20A C25A N31A 110.7(5) . . ?
C24A C25A N31A 127.0(6) . . ?
C30A N26A N27A 111.5(6) . . ?
C30A N26A C21A 132.1(6) . . ?
N27A N26A C21A 116.4(5) . . ?
C28A N27A N26A 105.2(6) . . ?
C28A N27A Fe1A 141.8(5) . . ?
N26A N27A Fe1A 113.0(4) . . ?
N27A C28A C29A 109.9(7) . . ?
N27A C28A H28A 125.0 . . ?
C29A C28A H28A 125.0 . . ?
C30A C29A C28A 106.7(7) . . ?
C30A C29A H29A 126.6 . . ?
C28A C29A H29A 126.6 . . ?
C29A C30A N26A 106.6(7) . . ?
C29A C30A H30A 126.7 . . ?
N26A C30A H30A 126.7 . . ?
C35A N31A N32A 110.3(6) . . ?
C35A N31A C25A 132.2(6) . . ?
N32A N31A C25A 117.4(5) . . ?
C33A N32A N31A 105.3(6) . . ?
C33A N32A Fe1A 142.4(5) . . ?
N31A N32A Fe1A 112.2(4) . . ?
N32A C33A C34A 110.8(6) . . ?
N32A C33A H33A 124.6 . . ?
C34A C33A H33A 124.6 . . ?
C35A C34A C33A 106.0(7) . . ?
C35A C34A H34A 127.0 . . ?
C33A C34A H34A 127.0 . . ?
C34A C35A N31A 107.6(7) . . ?
C34A C35A H35A 126.2 . . ?
N31A C35A H35A 126.2 . . ?
C23A S36A C37A 103.2(4) . . ?
S36A C37A H37A 109.5 . . ?
S36A C37A H37B 109.5 . . ?
H37A C37A H37B 109.5 . . ?
S36A C37A H37C 109.5 . . ?
H37A C37A H37C 109.5 . . ?
H37B C37A H37C 109.5 . . ?
N20B Fe1B N2B 177.9(2) . . ?
N20B Fe1B N14B 98.7(2) . . ?
N2B Fe1B N14B 79.9(2) . . ?
N20B Fe1B N32B 79.7(2) . . ?
N2B Fe1B N32B 101.7(2) . . ?
N14B Fe1B N32B 89.4(2) . . ?
N20B Fe1B N27B 80.0(2) . . ?
N2B Fe1B N27B 98.6(2) . . ?
N14B Fe1B N27B 93.3(2) . . ?
N32B Fe1B N27B 159.7(2) . . ?
N20B Fe1B N9B 102.2(2) . . ?
N2B Fe1B N9B 79.4(2) . . ?
N14B Fe1B N9B 158.9(2) . . ?
N32B Fe1B N9B 91.2(2) . . ?
N27B Fe1B N9B 93.5(2) . . ?
C3B N2B C7B 119.3(5) . . ?
C3B N2B Fe1B 121.3(4) . . ?
C7B N2B Fe1B 119.3(4) . . ?
N2B C3B C4B 123.4(7) . . ?
N2B C3B N8B 109.2(6) . . ?
C4B C3B N8B 127.4(7) . . ?
C3B C4B C5B 117.9(7) . . ?
C3B C4B H4B 121.0 . . ?
C5B C4B H4B 121.0 . . ?
C4B C5B C6B 119.9(6) . . ?
C4B C5B S18B 125.1(6) . . ?
C6B C5B S18B 115.0(5) . . ?
C7B C6B C5B 117.9(7) . . ?
C7B C6B H6B 121.1 . . ?
C5B C6B H6B 121.1 . . ?
N2B C7B C6B 121.6(6) . . ?
N2B C7B N13B 111.3(5) . . ?
C6B C7B N13B 127.1(6) . . ?
C12B N8B N9B 110.9(6) . . ?
C12B N8B C3B 130.8(6) . . ?
N9B N8B C3B 118.1(6) . . ?
C10B N9B N8B 105.9(6) . . ?
C10B N9B Fe1B 142.1(5) . . ?
N8B N9B Fe1B 111.9(4) . . ?
N9B C10B C11B 109.4(7) . . ?
N9B C10B H10B 125.3 . . ?
C11B C10B H10B 125.3 . . ?
C12B C11B C10B 107.3(7) . . ?
C12B C11B H11B 126.3 . . ?
C10B C11B H11B 126.3 . . ?
N8B C12B C11B 106.4(7) . . ?
N8B C12B H12B 126.8 . . ?
C11B C12B H12B 126.8 . . ?
C17B N13B N14B 110.5(6) . . ?
C17B N13B C7B 133.3(6) . . ?
N14B N13B C7B 115.8(5) . . ?
C15B N14B N13B 105.2(6) . . ?
C15B N14B Fe1B 141.3(5) . . ?
N13B N14B Fe1B 113.5(4) . . ?
N14B C15B C16B 109.8(6) . . ?
N14B C15B H15B 125.1 . . ?
C16B C15B H15B 125.1 . . ?
C17B C16B C15B 107.0(7) . . ?
C17B C16B H16B 126.5 . . ?
C15B C16B H16B 126.5 . . ?
C16B C17B N13B 107.4(7) . . ?
C16B C17B H17B 126.3 . . ?
N13B C17B H17B 126.3 . . ?
C5B S18B C19B 102.3(4) . . ?
S18B C19B H19D 109.5 . . ?
S18B C19B H19E 109.5 . . ?
H19D C19B H19E 109.5 . . ?
S18B C19B H19F 109.5 . . ?
H19D C19B H19F 109.5 . . ?
H19E C19B H19F 109.5 . . ?
C25B N20B C21B 118.6(6) . . ?
C25B N20B Fe1B 121.5(4) . . ?
C21B N20B Fe1B 119.8(4) . . ?
N20B C21B C22B 122.0(7) . . ?
N20B C21B N26B 110.6(6) . . ?
C22B C21B N26B 127.4(7) . . ?
C21B C22B C23B 118.3(7) . . ?
C21B C22B H22B 120.9 . . ?
C23B C22B H22B 120.9 . . ?
C24B C23B C22B 120.3(6) . . ?
C24B C23B S36B 123.5(6) . . ?
C22B C23B S36B 116.2(6) . . ?
C25B C24B C23B 116.5(7) . . ?
C25B C24B H24B 121.8 . . ?
C23B C24B H24B 121.8 . . ?
N20B C25B C24B 124.2(7) . . ?
N20B C25B N31B 109.9(5) . . ?
C24B C25B N31B 125.9(7) . . ?
N27B N26B C30B 110.1(6) . . ?
N27B N26B C21B 117.5(5) . . ?
C30B N26B C21B 132.3(6) . . ?
C28B N27B N26B 105.8(6) . . ?
C28B N27B Fe1B 142.2(5) . . ?
N26B N27B Fe1B 112.0(4) . . ?
N27B C28B C29B 110.6(7) . . ?
N27B C28B H28B 124.7 . . ?
C29B C28B H28B 124.7 . . ?
C30B C29B C28B 106.6(7) . . ?
C30B C29B H29B 126.7 . . ?
C28B C29B H29B 126.7 . . ?
C29B C30B N26B 106.9(7) . . ?
C29B C30B H30B 126.5 . . ?
N26B C30B H30B 126.5 . . ?
C35B N31B N32B 110.7(6) . . ?
C35B N31B C25B 132.9(6) . . ?
N32B N31B C25B 116.3(6) . . ?
C33B N32B N31B 104.3(6) . . ?
C33B N32B Fe1B 142.7(5) . . ?
N31B N32B Fe1B 112.6(4) . . ?
N32B C33B C34B 111.4(7) . . ?
N32B C33B H33B 124.3 . . ?
C34B C33B H33B 124.3 . . ?
C35B C34B C33B 105.7(7) . . ?
C35B C34B H34B 127.2 . . ?
C33B C34B H34B 127.2 . . ?
C34B C35B N31B 108.0(7) . . ?
C34B C35B H35B 126.0 . . ?
N31B C35B H35B 126.0 . . ?
C23B S36B C37B 103.6(4) . . ?
S36B C37B H37D 109.5 . . ?
S36B C37B H37E 109.5 . . ?
H37D C37B H37E 109.5 . . ?
S36B C37B H37F 109.5 . . ?
H37D C37B H37F 109.5 . . ?
H37E C37B H37F 109.5 . . ?
O41A Cl38A O42A 112.9(7) . . ?
O41A Cl38A O39A 110.1(6) . . ?
O42A Cl38A O39A 107.9(6) . . ?
O41A Cl38A O40A 112.5(6) . . ?
O42A Cl38A O40A 108.1(6) . . ?
O39A Cl38A O40A 104.9(6) . . ?
O40B Cl38B O39B 115.8(16) . . ?
O40B Cl38B O42B 111.4(15) . . ?
O39B Cl38B O42B 108.4(14) . . ?
O40B Cl38B O41B 107.9(14) . . ?
O39B Cl38B O41B 106.1(14) . . ?
O42B Cl38B O41B 106.8(13) . . ?
O47A Cl43A O45A 113.1(10) . . ?
O47A Cl43A O46A 113.4(10) . . ?
O45A Cl43A O46A 109.8(9) . . ?
O47A Cl43A O44A 110.6(10) . . ?
O45A Cl43A O44A 103.9(9) . . ?
O46A Cl43A O44A 105.3(9) . . ?
O44B Cl43B O45B 111.2(9) . . ?
O44B Cl43B O46B 109.2(9) . . ?
O45B Cl43B O46B 111.0(9) . . ?
O44B Cl43B O47B 110.5(9) . . ?
O45B Cl43B O47B 106.2(9) . . ?
O46B Cl43B O47B 108.8(9) . . ?
O51A Cl48A O49A 114.1(8) . . ?
O51A Cl48A O50A 109.2(9) . . ?
O49A Cl48A O50A 107.4(8) . . ?
O51A Cl48A O52A 110.5(8) . . ?
O49A Cl48A O52A 109.5(9) . . ?
O50A Cl48A O52A 105.7(8) . . ?
O52B Cl48B O51B 111.5(7) . . ?
O52B Cl48B O50B 111.6(8) . . ?
O51B Cl48B O50B 110.0(8) . . ?
O52B Cl48B O49B 113.3(8) . . ?
O51B Cl48B O49B 104.3(7) . . ?
O50B Cl48B O49B 105.7(8) . . ?
O55A Cl53A O57A 111.9(8) . . ?
O55A Cl53A O56A 112.7(8) . . ?
O57A Cl53A O56A 104.9(8) . . ?
O55A Cl53A O54A 116.5(9) . . ?
O57A Cl53A O54A 108.1(9) . . ?
O56A Cl53A O54A 101.8(9) . . ?
O54B Cl53B O56B 115.2(9) . . ?
O54B Cl53B O57B 114.2(8) . . ?
O56B Cl53B O57B 111.2(9) . . ?
O54B Cl53B O55B 105.7(11) . . ?
O56B Cl53B O55B 104.8(11) . . ?
O57B Cl53B O55B 104.6(11) . . ?

_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_theta_full        74.29
_diffrn_measured_fraction_theta_full 0.972
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.092
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: nitromethane/diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lkc266
_database_code_depnum_ccdc_archive 'CCDC 1060844'
_audit_update_record             
;
2015-04-21 deposited with the CCDC.
2015-06-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
Bis[2,6-di(pyrazol-1-yl)4-methylsulfanylpyridine]iron(II)diperchlorate
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H22 Fe N10 S2, 2[Cl O4]'
_chemical_formula_sum            'C24 H22 Cl2 Fe N10 O8 S2'
_chemical_formula_weight         769.39

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   16.2202(4)
_cell_length_b                   17.1650(4)
_cell_length_c                   21.9195(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6102.8(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5095
_cell_measurement_theta_min      3.26
_cell_measurement_theta_max      73.06

_exptl_crystal_description       fragment
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3136
_exptl_absorpt_coefficient_mu    7.440
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.647
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28e (release 10-06-2013 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            17530
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_sigmaI/netI    0.0671
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.27
_diffrn_reflns_theta_max         73.88
_reflns_number_total             10533
_reflns_number_gt                8825
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The crystal refined as a racemic twin. Although the Flack parameter is 
 close to 0.5, ADSYMM and NEWSYMM analyses both supported this choice of 
 space group.

 The asymmetric unit contains two formula units (Z' = 2), with all cations 
 and anions lying on general crystallographic sites. No disorder is 
 present in the model, and no restraints were applied. All non-H atoms were
 refined anisotropically, while H atoms were placed in calculated positions
 and refined using a riding model.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0573P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.546(5)
_refine_ls_number_reflns         10533
_refine_ls_number_parameters     852
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0488
_refine_ls_wR_factor_ref         0.1198
_refine_ls_wR_factor_gt          0.1110
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1A Fe 0.77068(5) 0.50407(4) 0.69241(3) 0.01947(16) Uani 1 1 d . . .
N2A N 0.7868(3) 0.6128(2) 0.68447(19) 0.0226(9) Uani 1 1 d . . .
C3A C 0.8442(3) 0.6409(3) 0.6467(2) 0.0225(10) Uani 1 1 d . . .
C4A C 0.8562(3) 0.7194(3) 0.6362(3) 0.0306(12) Uani 1 1 d . . .
H4A H 0.8974 0.7376 0.6089 0.037 Uiso 1 1 calc R . .
C5A C 0.8041(3) 0.7712(3) 0.6683(3) 0.0291(12) Uani 1 1 d . . .
C6A C 0.7444(3) 0.7425(3) 0.7091(2) 0.0262(11) Uani 1 1 d . . .
H6A H 0.7096 0.7766 0.7314 0.031 Uiso 1 1 calc R . .
C7A C 0.7384(3) 0.6629(3) 0.7152(2) 0.0253(11) Uani 1 1 d . . .
N8A N 0.8896(3) 0.5799(3) 0.62057(19) 0.0252(9) Uani 1 1 d . . .
N9A N 0.8634(3) 0.5052(3) 0.63366(19) 0.0256(9) Uani 1 1 d . . .
C10A C 0.9120(3) 0.4586(3) 0.6026(3) 0.0306(12) Uani 1 1 d . . .
H10A H 0.9083 0.4033 0.6028 0.037 Uiso 1 1 calc R . .
C11A C 0.9704(4) 0.5014(4) 0.5687(3) 0.0376(13) Uani 1 1 d . . .
H11A H 1.0121 0.4814 0.5426 0.045 Uiso 1 1 calc R . .
C12A C 0.9544(3) 0.5780(4) 0.5814(3) 0.0320(13) Uani 1 1 d . . .
H12A H 0.9833 0.6217 0.5657 0.038 Uiso 1 1 calc R . .
N13A N 0.6834(3) 0.6219(2) 0.7526(2) 0.0237(9) Uani 1 1 d . . .
N14A N 0.6876(3) 0.5425(2) 0.75047(18) 0.0226(9) Uani 1 1 d . . .
C15A C 0.6369(3) 0.5166(3) 0.7930(2) 0.0253(11) Uani 1 1 d . . .
H15A H 0.6277 0.4632 0.8022 0.030 Uiso 1 1 calc R . .
C16A C 0.5986(4) 0.5794(4) 0.8228(3) 0.0318(12) Uani 1 1 d . . .
H16A H 0.5589 0.5765 0.8546 0.038 Uiso 1 1 calc R . .
C17A C 0.6296(3) 0.6448(3) 0.7972(2) 0.0288(12) Uani 1 1 d . . .
H17A H 0.6165 0.6969 0.8081 0.035 Uiso 1 1 calc R . .
S18A S 0.82097(10) 0.86991(8) 0.65546(8) 0.0405(4) Uani 1 1 d . . .
C19A C 0.7475(4) 0.9169(3) 0.7035(3) 0.0413(15) Uani 1 1 d . . .
H19A H 0.6916 0.9024 0.6907 0.062 Uiso 1 1 calc R . .
H19B H 0.7541 0.9735 0.7004 0.062 Uiso 1 1 calc R . .
H19C H 0.7562 0.9006 0.7459 0.062 Uiso 1 1 calc R . .
N20A N 0.7514(2) 0.3954(2) 0.69940(19) 0.0207(9) Uani 1 1 d . . .
C21A C 0.6982(3) 0.3595(3) 0.6623(2) 0.0239(10) Uani 1 1 d . . .
C22A C 0.6820(3) 0.2807(3) 0.6656(2) 0.0250(11) Uani 1 1 d . . .
H22A H 0.6445 0.2563 0.6383 0.030 Uiso 1 1 calc R . .
C23A C 0.7231(3) 0.2384(3) 0.7105(2) 0.0256(11) Uani 1 1 d . . .
C24A C 0.7790(3) 0.2755(3) 0.7494(2) 0.0262(11) Uani 1 1 d . . .
H24A H 0.8082 0.2474 0.7799 0.031 Uiso 1 1 calc R . .
C25A C 0.7900(3) 0.3535(3) 0.7420(2) 0.0235(10) Uani 1 1 d . . .
N26A N 0.6618(3) 0.4129(3) 0.6223(2) 0.0251(9) Uani 1 1 d . . .
N27A N 0.6882(3) 0.4898(3) 0.62690(19) 0.0247(9) Uani 1 1 d . . .
C28A C 0.6452(3) 0.5274(3) 0.5847(2) 0.0282(11) Uani 1 1 d . . .
H28A H 0.6501 0.5816 0.5767 0.034 Uiso 1 1 calc R . .
C29A C 0.5918(4) 0.4775(3) 0.5533(3) 0.0334(13) Uani 1 1 d . . .
H29A H 0.5551 0.4912 0.5213 0.040 Uiso 1 1 calc R . .
C30A C 0.6029(4) 0.4055(4) 0.5778(3) 0.0327(13) Uani 1 1 d . . .
H30A H 0.5752 0.3590 0.5663 0.039 Uiso 1 1 calc R . .
N31A N 0.8418(3) 0.4014(2) 0.7767(2) 0.0255(9) Uani 1 1 d . . .
N32A N 0.8450(3) 0.4790(2) 0.76131(19) 0.0217(8) Uani 1 1 d . . .
C33A C 0.8942(3) 0.5116(3) 0.8017(2) 0.0291(11) Uani 1 1 d . . .
H33A H 0.9088 0.5652 0.8019 0.035 Uiso 1 1 calc R . .
C34A C 0.9224(4) 0.4567(4) 0.8445(3) 0.0387(14) Uani 1 1 d . . .
H34A H 0.9577 0.4661 0.8782 0.046 Uiso 1 1 calc R . .
C35A C 0.8884(4) 0.3870(4) 0.8274(3) 0.0351(13) Uani 1 1 d . . .
H35A H 0.8958 0.3381 0.8470 0.042 Uiso 1 1 calc R . .
S36A S 0.70738(9) 0.13878(8) 0.72335(7) 0.0364(3) Uani 1 1 d . . .
C37A C 0.6129(4) 0.1199(3) 0.6825(3) 0.0381(14) Uani 1 1 d . . .
H37A H 0.5705 0.1571 0.6955 0.057 Uiso 1 1 calc R . .
H37B H 0.5942 0.0668 0.6911 0.057 Uiso 1 1 calc R . .
H37C H 0.6226 0.1257 0.6386 0.057 Uiso 1 1 calc R . .
Fe1B Fe 0.26764(5) 0.50825(4) 0.56258(3) 0.01897(16) Uani 1 1 d . . .
N2B N 0.2821(3) 0.6178(2) 0.55422(18) 0.0206(9) Uani 1 1 d . . .
C3B C 0.3370(3) 0.6560(3) 0.5880(2) 0.0240(11) Uani 1 1 d . . .
C4B C 0.3463(3) 0.7354(3) 0.5858(2) 0.0241(11) Uani 1 1 d . . .
H4B H 0.3844 0.7616 0.6115 0.029 Uiso 1 1 calc R . .
C5B C 0.2973(3) 0.7761(3) 0.5441(3) 0.0283(11) Uani 1 1 d . . .
C6B C 0.2399(3) 0.7372(3) 0.5076(3) 0.0256(11) Uani 1 1 d . . .
H6B H 0.2065 0.7643 0.4791 0.031 Uiso 1 1 calc R . .
C7B C 0.2341(3) 0.6577(3) 0.5150(2) 0.0228(10) Uani 1 1 d . . .
N8B N 0.3822(3) 0.6029(3) 0.6230(2) 0.0247(9) Uani 1 1 d . . .
N9B N 0.3587(3) 0.5262(3) 0.62138(19) 0.0233(9) Uani 1 1 d . . .
C10B C 0.4114(3) 0.4890(3) 0.6570(2) 0.0301(12) Uani 1 1 d . . .
H10B H 0.4106 0.4345 0.6647 0.036 Uiso 1 1 calc R . .
C11B C 0.4686(4) 0.5416(4) 0.6817(3) 0.0341(13) Uani 1 1 d . . .
H11B H 0.5123 0.5293 0.7089 0.041 Uiso 1 1 calc R . .
C12B C 0.4499(3) 0.6131(3) 0.6596(2) 0.0305(12) Uani 1 1 d . . .
H12B H 0.4779 0.6606 0.6678 0.037 Uiso 1 1 calc R . .
N13B N 0.1809(3) 0.6075(2) 0.48366(19) 0.0231(9) Uani 1 1 d . . .
N14B N 0.1872(3) 0.5295(2) 0.49794(19) 0.0219(9) Uani 1 1 d . . .
C15B C 0.1381(3) 0.4935(3) 0.4594(2) 0.0264(11) Uani 1 1 d . . .
H15B H 0.1292 0.4388 0.4586 0.032 Uiso 1 1 calc R . .
C16B C 0.1007(3) 0.5466(3) 0.4196(3) 0.0284(12) Uani 1 1 d . . .
H16B H 0.0633 0.5348 0.3876 0.034 Uiso 1 1 calc R . .
C17B C 0.1284(3) 0.6182(3) 0.4359(3) 0.0270(11) Uani 1 1 d . . .
H17B H 0.1140 0.6664 0.4176 0.032 Uiso 1 1 calc R . .
S18B S 0.30295(9) 0.87723(8) 0.53354(8) 0.0381(3) Uani 1 1 d . . .
C19B C 0.4000(4) 0.9017(3) 0.5681(3) 0.0351(13) Uani 1 1 d . . .
H19D H 0.3964 0.8942 0.6124 0.053 Uiso 1 1 calc R . .
H19E H 0.4133 0.9562 0.5594 0.053 Uiso 1 1 calc R . .
H19F H 0.4433 0.8680 0.5515 0.053 Uiso 1 1 calc R . .
N20B N 0.2485(2) 0.3994(2) 0.5710(2) 0.0228(9) Uani 1 1 d . . .
C21B C 0.1919(3) 0.3728(3) 0.6111(2) 0.0235(10) Uani 1 1 d . . .
C22B C 0.1755(3) 0.2961(3) 0.6181(2) 0.0262(11) Uani 1 1 d . . .
H22B H 0.1358 0.2787 0.6469 0.031 Uiso 1 1 calc R . .
C23B C 0.2190(3) 0.2431(3) 0.5815(3) 0.0277(12) Uani 1 1 d . . .
C24B C 0.2765(3) 0.2700(3) 0.5397(3) 0.0279(11) Uani 1 1 d . . .
H24B H 0.3067 0.2350 0.5146 0.034 Uiso 1 1 calc R . .
C25B C 0.2882(3) 0.3488(3) 0.5360(2) 0.0239(11) Uani 1 1 d . . .
N26B N 0.1562(3) 0.4347(3) 0.6421(2) 0.0241(9) Uani 1 1 d . . .
N27B N 0.1822(3) 0.5094(3) 0.62799(18) 0.0238(9) Uani 1 1 d . . .
C28B C 0.1417(4) 0.5565(3) 0.6637(2) 0.0304(12) Uani 1 1 d . . .
H28B H 0.1472 0.6116 0.6637 0.036 Uiso 1 1 calc R . .
C29B C 0.0884(3) 0.5143(4) 0.7025(3) 0.0338(13) Uani 1 1 d . . .
H29B H 0.0526 0.5350 0.7328 0.041 Uiso 1 1 calc R . .
C30B C 0.0986(3) 0.4387(4) 0.6877(3) 0.0309(12) Uani 1 1 d . . .
H30B H 0.0709 0.3958 0.7057 0.037 Uiso 1 1 calc R . .
N31B N 0.3420(3) 0.3876(3) 0.4954(2) 0.0255(9) Uani 1 1 d . . .
N32B N 0.3444(3) 0.4674(2) 0.5006(2) 0.0222(9) Uani 1 1 d . . .
C33B C 0.3942(3) 0.4910(3) 0.4563(2) 0.0292(11) Uani 1 1 d . . .
H33B H 0.4089 0.5436 0.4485 0.035 Uiso 1 1 calc R . .
C34B C 0.4223(4) 0.4259(4) 0.4221(3) 0.0415(15) Uani 1 1 d . . .
H34B H 0.4582 0.4271 0.3878 0.050 Uiso 1 1 calc R . .
C35B C 0.3883(4) 0.3617(3) 0.4478(3) 0.0371(14) Uani 1 1 d . . .
H35B H 0.3954 0.3092 0.4352 0.045 Uiso 1 1 calc R . .
S36B S 0.19503(10) 0.14432(8) 0.59211(8) 0.0406(4) Uani 1 1 d . . .
C37B C 0.2626(4) 0.0949(3) 0.5397(3) 0.0425(15) Uani 1 1 d . . .
H37D H 0.2539 0.1153 0.4984 0.064 Uiso 1 1 calc R . .
H37E H 0.2506 0.0389 0.5402 0.064 Uiso 1 1 calc R . .
H37F H 0.3200 0.1035 0.5518 0.064 Uiso 1 1 calc R . .
Cl38 Cl 0.49317(8) 0.33158(7) 0.77304(6) 0.0290(3) Uani 1 1 d . . .
O39 O 0.5800(3) 0.3211(3) 0.7846(2) 0.0450(11) Uani 1 1 d . . .
O40 O 0.4716(3) 0.4112(2) 0.7862(2) 0.0415(10) Uani 1 1 d . . .
O41 O 0.4763(4) 0.3139(3) 0.7111(2) 0.0560(13) Uani 1 1 d . . .
O42 O 0.4472(3) 0.2804(3) 0.8132(3) 0.0569(14) Uani 1 1 d . . .
Cl43 Cl 0.53075(8) 0.69459(7) 0.48650(6) 0.0278(3) Uani 1 1 d . . .
O44 O 0.5866(3) 0.6342(3) 0.4694(2) 0.0508(12) Uani 1 1 d . . .
O45 O 0.5399(3) 0.7097(3) 0.55033(19) 0.0471(12) Uani 1 1 d . . .
O46 O 0.5503(3) 0.7631(3) 0.4527(3) 0.0592(15) Uani 1 1 d . . .
O47 O 0.4473(3) 0.6727(3) 0.4735(2) 0.0443(11) Uani 1 1 d . . .
Cl48 Cl 0.51071(8) 0.19325(8) 0.52522(6) 0.0321(3) Uani 1 1 d . . .
O49 O 0.5990(2) 0.1992(3) 0.5299(2) 0.0423(10) Uani 1 1 d . . .
O50 O 0.4850(3) 0.1198(3) 0.5501(2) 0.0494(12) Uani 1 1 d . . .
O51 O 0.4747(3) 0.2559(3) 0.5588(3) 0.0703(17) Uani 1 1 d . . .
O52 O 0.4862(4) 0.1971(3) 0.4633(2) 0.0668(16) Uani 1 1 d . . .
Cl53 Cl 0.01114(8) 0.71804(7) 0.76677(6) 0.0286(3) Uani 1 1 d . . .
O54 O 0.0257(3) 0.7949(2) 0.7890(2) 0.0451(11) Uani 1 1 d . . .
O55 O 0.0317(3) 0.7134(3) 0.70306(19) 0.0399(10) Uani 1 1 d . . .
O56 O 0.0598(3) 0.6635(3) 0.7996(2) 0.0555(13) Uani 1 1 d . . .
O57 O -0.0757(2) 0.6996(3) 0.7740(2) 0.0404(10) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1A N2A 1.893(4) . ?
Fe1A N20A 1.897(4) . ?
Fe1A N14A 1.967(4) . ?
Fe1A N27A 1.978(4) . ?
Fe1A N32A 1.980(4) . ?
Fe1A N9A 1.981(4) . ?
N2A C3A 1.335(7) . ?
N2A C7A 1.345(7) . ?
C3A C4A 1.380(7) . ?
C3A N8A 1.403(7) . ?
C4A C5A 1.415(8) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.406(8) . ?
C5A S18A 1.740(5) . ?
C6A C7A 1.377(7) . ?
C6A H6A 0.9500 . ?
C7A N13A 1.402(7) . ?
N8A C12A 1.357(7) . ?
N8A N9A 1.381(6) . ?
N9A C10A 1.314(7) . ?
C10A C11A 1.411(8) . ?
C10A H10A 0.9500 . ?
C11A C12A 1.368(8) . ?
C11A H11A 0.9500 . ?
C12A H12A 0.9500 . ?
N13A N14A 1.366(6) . ?
N13A C17A 1.368(7) . ?
N14A C15A 1.321(6) . ?
C15A C16A 1.405(8) . ?
C15A H15A 0.9500 . ?
C16A C17A 1.352(8) . ?
C16A H16A 0.9500 . ?
C17A H17A 0.9500 . ?
S18A C19A 1.784(7) . ?
C19A H19A 0.9800 . ?
C19A H19B 0.9800 . ?
C19A H19C 0.9800 . ?
N20A C25A 1.335(6) . ?
N20A C21A 1.336(7) . ?
C21A C22A 1.381(7) . ?
C21A N26A 1.400(7) . ?
C22A C23A 1.393(8) . ?
C22A H22A 0.9500 . ?
C23A C24A 1.400(7) . ?
C23A S36A 1.751(5) . ?
C24A C25A 1.360(7) . ?
C24A H24A 0.9500 . ?
C25A N31A 1.401(7) . ?
N26A C30A 1.371(7) . ?
N26A N27A 1.390(6) . ?
N27A C28A 1.327(7) . ?
C28A C29A 1.400(8) . ?
C28A H28A 0.9500 . ?
C29A C30A 1.359(8) . ?
C29A H29A 0.9500 . ?
C30A H30A 0.9500 . ?
N31A C35A 1.367(7) . ?
N31A N32A 1.374(6) . ?
N32A C33A 1.317(7) . ?
C33A C34A 1.405(8) . ?
C33A H33A 0.9500 . ?
C34A C35A 1.370(8) . ?
C34A H34A 0.9500 . ?
C35A H35A 0.9500 . ?
S36A C37A 1.805(6) . ?
C37A H37A 0.9800 . ?
C37A H37B 0.9800 . ?
C37A H37C 0.9800 . ?
Fe1B N20B 1.902(4) . ?
Fe1B N2B 1.904(4) . ?
Fe1B N14B 1.960(4) . ?
Fe1B N32B 1.971(4) . ?
Fe1B N9B 1.985(4) . ?
Fe1B N27B 1.994(4) . ?
N2B C3B 1.330(7) . ?
N2B C7B 1.347(7) . ?
C3B C4B 1.371(7) . ?
C3B N8B 1.400(7) . ?
C4B C5B 1.398(8) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.396(8) . ?
C5B S18B 1.754(5) . ?
C6B C7B 1.377(7) . ?
C6B H6B 0.9500 . ?
C7B N13B 1.401(7) . ?
N8B N9B 1.371(6) . ?
N8B C12B 1.371(7) . ?
N9B C10B 1.322(7) . ?
C10B C11B 1.404(8) . ?
C10B H10B 0.9500 . ?
C11B C12B 1.355(8) . ?
C11B H11B 0.9500 . ?
C12B H12B 0.9500 . ?
N13B C17B 1.361(7) . ?
N13B N14B 1.378(6) . ?
N14B C15B 1.315(7) . ?
C15B C16B 1.399(8) . ?
C15B H15B 0.9500 . ?
C16B C17B 1.357(8) . ?
C16B H16B 0.9500 . ?
C17B H17B 0.9500 . ?
S18B C19B 1.798(6) . ?
C19B H19D 0.9800 . ?
C19B H19E 0.9800 . ?
C19B H19F 0.9800 . ?
N20B C25B 1.325(7) . ?
N20B C21B 1.350(6) . ?
C21B C22B 1.352(7) . ?
C21B N26B 1.389(7) . ?
C22B C23B 1.403(8) . ?
C22B H22B 0.9500 . ?
C23B C24B 1.387(8) . ?
C23B S36B 1.754(5) . ?
C24B C25B 1.369(7) . ?
C24B H24B 0.9500 . ?
C25B N31B 1.413(7) . ?
N26B C30B 1.370(7) . ?
N26B N27B 1.385(6) . ?
N27B C28B 1.303(7) . ?
C28B C29B 1.412(8) . ?
C28B H28B 0.9500 . ?
C29B C30B 1.348(8) . ?
C29B H29B 0.9500 . ?
C30B H30B 0.9500 . ?
N31B C35B 1.361(7) . ?
N31B N32B 1.374(6) . ?
N32B C33B 1.327(7) . ?
C33B C34B 1.420(8) . ?
C33B H33B 0.9500 . ?
C34B C35B 1.355(8) . ?
C34B H34B 0.9500 . ?
C35B H35B 0.9500 . ?
S36B C37B 1.801(7) . ?
C37B H37D 0.9800 . ?
C37B H37E 0.9800 . ?
C37B H37F 0.9800 . ?
Cl38 O41 1.418(5) . ?
Cl38 O40 1.439(4) . ?
Cl38 O39 1.443(4) . ?
Cl38 O42 1.449(5) . ?
Cl43 O46 1.426(5) . ?
Cl43 O44 1.426(4) . ?
Cl43 O45 1.431(4) . ?
Cl43 O47 1.433(4) . ?
Cl48 O52 1.416(5) . ?
Cl48 O51 1.428(5) . ?
Cl48 O50 1.436(5) . ?
Cl48 O49 1.439(4) . ?
Cl53 O56 1.421(5) . ?
Cl53 O54 1.426(4) . ?
Cl53 O55 1.438(4) . ?
Cl53 O57 1.453(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2A Fe1A N20A 178.33(18) . . ?
N2A Fe1A N14A 79.86(18) . . ?
N20A Fe1A N14A 99.45(18) . . ?
N2A Fe1A N27A 98.59(18) . . ?
N20A Fe1A N27A 79.91(18) . . ?
N14A Fe1A N27A 92.77(17) . . ?
N2A Fe1A N32A 101.57(17) . . ?
N20A Fe1A N32A 79.92(17) . . ?
N14A Fe1A N32A 89.81(17) . . ?
N27A Fe1A N32A 159.82(18) . . ?
N2A Fe1A N9A 79.95(19) . . ?
N20A Fe1A N9A 100.80(19) . . ?
N14A Fe1A N9A 159.68(19) . . ?
N27A Fe1A N9A 92.44(17) . . ?
N32A Fe1A N9A 92.03(18) . . ?
C3A N2A C7A 119.1(4) . . ?
C3A N2A Fe1A 120.6(3) . . ?
C7A N2A Fe1A 120.2(4) . . ?
N2A C3A C4A 123.7(5) . . ?
N2A C3A N8A 110.4(4) . . ?
C4A C3A N8A 125.9(5) . . ?
C3A C4A C5A 116.4(5) . . ?
C3A C4A H4A 121.8 . . ?
C5A C4A H4A 121.8 . . ?
C6A C5A C4A 120.5(5) . . ?
C6A C5A S18A 123.5(4) . . ?
C4A C5A S18A 115.9(4) . . ?
C7A C6A C5A 117.2(5) . . ?
C7A C6A H6A 121.4 . . ?
C5A C6A H6A 121.4 . . ?
N2A C7A C6A 123.0(5) . . ?
N2A C7A N13A 110.2(4) . . ?
C6A C7A N13A 126.9(5) . . ?
C12A N8A N9A 110.3(4) . . ?
C12A N8A C3A 133.1(5) . . ?
N9A N8A C3A 116.6(4) . . ?
C10A N9A N8A 105.9(4) . . ?
C10A N9A Fe1A 141.9(4) . . ?
N8A N9A Fe1A 112.2(3) . . ?
N9A C10A C11A 111.0(5) . . ?
N9A C10A H10A 124.5 . . ?
C11A C10A H10A 124.5 . . ?
C12A C11A C10A 105.4(5) . . ?
C12A C11A H11A 127.3 . . ?
C10A C11A H11A 127.3 . . ?
N8A C12A C11A 107.4(5) . . ?
N8A C12A H12A 126.3 . . ?
C11A C12A H12A 126.3 . . ?
N14A N13A C17A 110.2(4) . . ?
N14A N13A C7A 116.6(4) . . ?
C17A N13A C7A 132.8(5) . . ?
C15A N14A N13A 106.3(4) . . ?
C15A N14A Fe1A 140.4(4) . . ?
N13A N14A Fe1A 113.0(3) . . ?
N14A C15A C16A 110.2(5) . . ?
N14A C15A H15A 124.9 . . ?
C16A C15A H15A 124.9 . . ?
C17A C16A C15A 106.3(5) . . ?
C17A C16A H16A 126.9 . . ?
C15A C16A H16A 126.9 . . ?
C16A C17A N13A 107.1(5) . . ?
C16A C17A H17A 126.5 . . ?
N13A C17A H17A 126.5 . . ?
C5A S18A C19A 103.8(3) . . ?
S18A C19A H19A 109.5 . . ?
S18A C19A H19B 109.5 . . ?
H19A C19A H19B 109.5 . . ?
S18A C19A H19C 109.5 . . ?
H19A C19A H19C 109.5 . . ?
H19B C19A H19C 109.5 . . ?
C25A N20A C21A 118.7(4) . . ?
C25A N20A Fe1A 120.6(3) . . ?
C21A N20A Fe1A 120.7(3) . . ?
N20A C21A C22A 122.9(5) . . ?
N20A C21A N26A 110.6(4) . . ?
C22A C21A N26A 126.5(5) . . ?
C21A C22A C23A 117.2(5) . . ?
C21A C22A H22A 121.4 . . ?
C23A C22A H22A 121.4 . . ?
C22A C23A C24A 120.2(5) . . ?
C22A C23A S36A 123.6(4) . . ?
C24A C23A S36A 116.2(4) . . ?
C25A C24A C23A 117.4(5) . . ?
C25A C24A H24A 121.3 . . ?
C23A C24A H24A 121.3 . . ?
N20A C25A C24A 123.5(5) . . ?
N20A C25A N31A 110.2(4) . . ?
C24A C25A N31A 126.2(5) . . ?
C30A N26A N27A 110.8(4) . . ?
C30A N26A C21A 132.8(5) . . ?
N27A N26A C21A 116.4(4) . . ?
C28A N27A N26A 104.4(4) . . ?
C28A N27A Fe1A 143.2(4) . . ?
N26A N27A Fe1A 112.3(3) . . ?
N27A C28A C29A 111.7(5) . . ?
N27A C28A H28A 124.2 . . ?
C29A C28A H28A 124.2 . . ?
C30A C29A C28A 106.3(5) . . ?
C30A C29A H29A 126.9 . . ?
C28A C29A H29A 126.9 . . ?
C29A C30A N26A 106.8(5) . . ?
C29A C30A H30A 126.6 . . ?
N26A C30A H30A 126.6 . . ?
C35A N31A N32A 110.8(4) . . ?
C35A N31A C25A 131.8(5) . . ?
N32A N31A C25A 117.2(4) . . ?
C33A N32A N31A 105.6(4) . . ?
C33A N32A Fe1A 142.1(4) . . ?
N31A N32A Fe1A 112.1(3) . . ?
N32A C33A C34A 111.1(5) . . ?
N32A C33A H33A 124.4 . . ?
C34A C33A H33A 124.4 . . ?
C35A C34A C33A 105.9(5) . . ?
C35A C34A H34A 127.1 . . ?
C33A C34A H34A 127.1 . . ?
N31A C35A C34A 106.6(5) . . ?
N31A C35A H35A 126.7 . . ?
C34A C35A H35A 126.7 . . ?
C23A S36A C37A 102.6(3) . . ?
S36A C37A H37A 109.5 . . ?
S36A C37A H37B 109.5 . . ?
H37A C37A H37B 109.5 . . ?
S36A C37A H37C 109.5 . . ?
H37A C37A H37C 109.5 . . ?
H37B C37A H37C 109.5 . . ?
N20B Fe1B N2B 177.72(19) . . ?
N20B Fe1B N14B 98.32(18) . . ?
N2B Fe1B N14B 80.14(17) . . ?
N20B Fe1B N32B 79.66(18) . . ?
N2B Fe1B N32B 101.95(18) . . ?
N14B Fe1B N32B 89.34(18) . . ?
N20B Fe1B N9B 102.16(18) . . ?
N2B Fe1B N9B 79.46(18) . . ?
N14B Fe1B N9B 159.36(18) . . ?
N32B Fe1B N9B 91.87(18) . . ?
N20B Fe1B N27B 80.03(18) . . ?
N2B Fe1B N27B 98.33(18) . . ?
N14B Fe1B N27B 93.18(17) . . ?
N32B Fe1B N27B 159.69(18) . . ?
N9B Fe1B N27B 92.79(17) . . ?
C3B N2B C7B 119.4(4) . . ?
C3B N2B Fe1B 121.1(3) . . ?
C7B N2B Fe1B 119.5(3) . . ?
N2B C3B C4B 123.0(5) . . ?
N2B C3B N8B 109.5(4) . . ?
C4B C3B N8B 127.5(5) . . ?
C3B C4B C5B 117.2(5) . . ?
C3B C4B H4B 121.4 . . ?
C5B C4B H4B 121.4 . . ?
C6B C5B C4B 120.9(5) . . ?
C6B C5B S18B 115.6(4) . . ?
C4B C5B S18B 123.5(4) . . ?
C7B C6B C5B 116.9(5) . . ?
C7B C6B H6B 121.6 . . ?
C5B C6B H6B 121.6 . . ?
N2B C7B C6B 122.6(5) . . ?
N2B C7B N13B 110.9(4) . . ?
C6B C7B N13B 126.5(5) . . ?
N9B N8B C12B 111.2(4) . . ?
N9B N8B C3B 117.8(4) . . ?
C12B N8B C3B 131.1(5) . . ?
C10B N9B N8B 105.6(4) . . ?
C10B N9B Fe1B 142.1(4) . . ?
N8B N9B Fe1B 111.9(3) . . ?
N9B C10B C11B 110.1(5) . . ?
N9B C10B H10B 124.9 . . ?
C11B C10B H10B 124.9 . . ?
C12B C11B C10B 107.2(5) . . ?
C12B C11B H11B 126.4 . . ?
C10B C11B H11B 126.4 . . ?
C11B C12B N8B 105.8(5) . . ?
C11B C12B H12B 127.1 . . ?
N8B C12B H12B 127.1 . . ?
C17B N13B N14B 110.6(4) . . ?
C17B N13B C7B 132.8(5) . . ?
N14B N13B C7B 116.1(4) . . ?
C15B N14B N13B 105.3(4) . . ?
C15B N14B Fe1B 141.3(4) . . ?
N13B N14B Fe1B 113.3(3) . . ?
N14B C15B C16B 111.0(5) . . ?
N14B C15B H15B 124.5 . . ?
C16B C15B H15B 124.5 . . ?
C17B C16B C15B 106.3(5) . . ?
C17B C16B H16B 126.8 . . ?
C15B C16B H16B 126.8 . . ?
C16B C17B N13B 106.7(5) . . ?
C16B C17B H17B 126.6 . . ?
N13B C17B H17B 126.6 . . ?
C5B S18B C19B 102.8(3) . . ?
S18B C19B H19D 109.5 . . ?
S18B C19B H19E 109.5 . . ?
H19D C19B H19E 109.5 . . ?
S18B C19B H19F 109.5 . . ?
H19D C19B H19F 109.5 . . ?
H19E C19B H19F 109.5 . . ?
C25B N20B C21B 119.0(4) . . ?
C25B N20B Fe1B 120.6(4) . . ?
C21B N20B Fe1B 120.4(3) . . ?
N20B C21B C22B 122.5(5) . . ?
N20B C21B N26B 110.0(4) . . ?
C22B C21B N26B 127.4(5) . . ?
C21B C22B C23B 117.9(5) . . ?
C21B C22B H22B 121.1 . . ?
C23B C22B H22B 121.1 . . ?
C24B C23B C22B 120.0(5) . . ?
C24B C23B S36B 123.9(4) . . ?
C22B C23B S36B 116.1(4) . . ?
C25B C24B C23B 117.4(5) . . ?
C25B C24B H24B 121.3 . . ?
C23B C24B H24B 121.3 . . ?
N20B C25B C24B 123.2(5) . . ?
N20B C25B N31B 110.8(4) . . ?
C24B C25B N31B 126.0(5) . . ?
C30B N26B N27B 108.9(4) . . ?
C30B N26B C21B 132.8(5) . . ?
N27B N26B C21B 118.2(4) . . ?
C28B N27B N26B 106.6(4) . . ?
C28B N27B Fe1B 142.1(4) . . ?
N26B N27B Fe1B 111.3(3) . . ?
N27B C28B C29B 110.7(5) . . ?
N27B C28B H28B 124.7 . . ?
C29B C28B H28B 124.7 . . ?
C30B C29B C28B 105.8(5) . . ?
C30B C29B H29B 127.1 . . ?
C28B C29B H29B 127.1 . . ?
C29B C30B N26B 107.9(5) . . ?
C29B C30B H30B 126.0 . . ?
N26B C30B H30B 126.0 . . ?
C35B N31B N32B 111.9(4) . . ?
C35B N31B C25B 132.0(5) . . ?
N32B N31B C25B 115.8(4) . . ?
C33B N32B N31B 105.1(4) . . ?
C33B N32B Fe1B 141.3(4) . . ?
N31B N32B Fe1B 113.2(3) . . ?
N32B C33B C34B 110.0(5) . . ?
N32B C33B H33B 125.0 . . ?
C34B C33B H33B 125.0 . . ?
C35B C34B C33B 106.8(5) . . ?
C35B C34B H34B 126.6 . . ?
C33B C34B H34B 126.6 . . ?
C34B C35B N31B 106.2(5) . . ?
C34B C35B H35B 126.9 . . ?
N31B C35B H35B 126.9 . . ?
C23B S36B C37B 103.6(3) . . ?
S36B C37B H37D 109.5 . . ?
S36B C37B H37E 109.5 . . ?
H37D C37B H37E 109.5 . . ?
S36B C37B H37F 109.5 . . ?
H37D C37B H37F 109.5 . . ?
H37E C37B H37F 109.5 . . ?
O41 Cl38 O40 110.4(3) . . ?
O41 Cl38 O39 109.2(3) . . ?
O40 Cl38 O39 108.7(3) . . ?
O41 Cl38 O42 110.6(3) . . ?
O40 Cl38 O42 109.2(3) . . ?
O39 Cl38 O42 108.7(3) . . ?
O46 Cl43 O44 108.7(3) . . ?
O46 Cl43 O45 109.6(3) . . ?
O44 Cl43 O45 108.9(3) . . ?
O46 Cl43 O47 108.8(3) . . ?
O44 Cl43 O47 110.9(3) . . ?
O45 Cl43 O47 109.9(3) . . ?
O52 Cl48 O51 110.1(4) . . ?
O52 Cl48 O50 108.8(3) . . ?
O51 Cl48 O50 110.3(3) . . ?
O52 Cl48 O49 110.1(4) . . ?
O51 Cl48 O49 108.5(3) . . ?
O50 Cl48 O49 108.9(3) . . ?
O56 Cl53 O54 110.2(3) . . ?
O56 Cl53 O55 109.1(3) . . ?
O54 Cl53 O55 110.2(3) . . ?
O56 Cl53 O57 109.9(3) . . ?
O54 Cl53 O57 109.0(3) . . ?
O55 Cl53 O57 108.5(3) . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        73.88
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.085
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: nitromethane/diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
