#------------------------------------------------------------------------------
#$Date: 2019-09-14 03:10:54 +0300 (Sat, 14 Sep 2019) $
#$Revision: 218281 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/41/7124157.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7124157
loop_
_publ_author_name
'Clemente Leon, Miguel'
'García-López, Víctor'
'Palacios-Corella, Mario'
'Cardona-Serra, Salvador'
'Coronado, Eugenio'
_publ_section_title
;
 Spin-crossover iron (II) complex showing thermal hysteresis around room
 temperature with symmetry breaking and an unusually high T(LIESST) of 120
 K.
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC05988A
_journal_year                    2019
_chemical_formula_moiety
'2(C39 H23 Cl Fe2 N15 O16), 4(Cl O4), 3(C3 H6 O), 2(O)'
_chemical_formula_sum            'C87 H74 Cl6 Fe4 N30 O53'
_chemical_formula_weight         2823.86
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-08-28
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-28 deposited with the CCDC.    2019-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                96.056(3)
_cell_angle_beta                 112.125(4)
_cell_angle_gamma                104.778(4)
_cell_formula_units_Z            1
_cell_length_a                   14.6268(6)
_cell_length_b                   15.0615(6)
_cell_length_c                   15.2862(6)
_cell_measurement_reflns_used    6069
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      24.5180
_cell_measurement_theta_min      3.6830
_cell_volume                     2939.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -84.00   7.00   1.00   22.50    --  -14.89 -57.00  30.00   91
  2  ω    -84.00   7.00   1.00   22.50    --  -14.89 -57.00-180.00   91
  3  ω    -79.00  -2.00   1.00   22.50    --  -14.89 -62.00 130.29   77
  4  ω    -83.00   3.00   1.00   22.50    --  -14.89 -68.00 -50.01   86
  5  ω    -53.00  37.00   1.00   22.50    --   15.67 -58.00-129.86   90
  6  ω    -53.00  38.00   1.00   22.50    --   15.67 -68.00  84.68   91
  7  ω    -53.00  37.00   1.00   22.50    --   15.67 -57.00 -60.00   90
  8  ω    -32.00  37.00   1.00   22.50    --   15.67 -57.00   0.00   69
  9  ω    -48.00  40.00   1.00   22.50    --   15.67 -67.00 153.65   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0396090000
_diffrn_orient_matrix_UB_12      0.0070640000
_diffrn_orient_matrix_UB_13      -0.0170541000
_diffrn_orient_matrix_UB_21      -0.0120221000
_diffrn_orient_matrix_UB_22      -0.0494845000
_diffrn_orient_matrix_UB_23      -0.0138845000
_diffrn_orient_matrix_UB_31      -0.0366001000
_diffrn_orient_matrix_UB_32      -0.0002511000
_diffrn_orient_matrix_UB_33      -0.0464673000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0880
_diffrn_reflns_av_unetI/netI     0.1527
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            43662
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.010
_diffrn_reflns_theta_min         3.306
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.728
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_description       prism
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.284
_refine_diff_density_min         -0.916
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     893
_refine_ls_number_reflns         12366
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1863
_refine_ls_R_factor_gt           0.0954
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1412P)²+1.6213P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2362
_refine_ls_wR_factor_ref         0.3061
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6106
_reflns_number_total             12366
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cc05988a3.cif
_cod_data_source_block           vg180bot_a
_cod_database_code               7124157
_shelx_shelxl_version_number     2018/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.918
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O25-C41
 1.2 with sigma of 0.02
 O26A-C44
 1.2 with sigma of 0.02
 O26B-C44
 1.2 with sigma of 0.02
 C42-C41 \\sim C41-C40
 with sigma of 0.02
3. Restrained planarity
 O25, C40, C41, C42
 with sigma of 0.1
4. Others
 Fixed Sof: O18A(0.5) O18B(0.5) O19A(0.5) O19B(0.5) O20A(0.5) O20B(0.5)
 O22A(0.5) O22B(0.5) O23A(0.5) O23B(0.5) O24A(0.5) O24B(0.5) O25(0.5) O26A(0.5)
 O26B(0.5) C40(0.5) H40A(0.5) H40B(0.5) H40C(0.5) C41(0.5) C42(0.5) H42A(0.5)
 H42B(0.5) H42C(0.5) C45A(0.5) H45A(0.5) H45B(0.5) H45C(0.5) C45B(0.5)
 H45D(0.5) H45E(0.5) H45F(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1A), C3(H3), C5(H5), C6(H6), C7(H7), C9(H9), C11(H11), C14(H14), C16(H16),
  C18(H18), C19(H19), C20(H20), C22(H22), C24(H24), C27(H27), C29(H29),
 C31(H31), C32(H32), C33(H33), C35(H35), C37(H37)
5.b Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C45A(H45A,H45B,
 H45C), C45B(H45D,H45E,H45F)
5.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.152
_oxdiff_exptl_absorpt_empirical_full_min 0.866
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.57417(7) 0.20335(7) 0.32985(6) 0.0308(3) Uani 1 1 d . . . .
Fe2 Fe 0.65139(8) 0.32454(8) 0.85161(7) 0.0426(3) Uani 1 1 d . . . .
Cl1 Cl 0.30432(17) 0.18298(14) -0.04026(15) 0.0543(5) Uani 1 1 d . . . .
Cl2 Cl 0.29224(19) 0.23740(16) 0.46644(15) 0.0631(6) Uani 1 1 d . . . .
Cl3 Cl 0.77040(16) 0.42683(18) 0.72073(15) 0.0628(6) Uani 1 1 d . . . .
O1 O 0.1207(4) -0.0226(4) 0.0646(5) 0.0667(17) Uani 1 1 d . . . .
H1 H 0.085088 -0.058972 0.084492 0.100 Uiso 1 1 calc GR . . .
O2 O 0.0599(4) 0.0985(4) 0.0784(4) 0.0582(15) Uani 1 1 d . . . .
O3 O 1.0470(5) 0.4127(8) 0.6120(6) 0.130(4) Uani 1 1 d . . . .
O4 O 1.0129(5) 0.5464(8) 0.6326(6) 0.133(4) Uani 1 1 d . . . .
H4 H 1.076040 0.568314 0.664838 0.200 Uiso 1 1 calc GR . . .
O5 O 0.6152(5) 0.0986(4) -0.0870(3) 0.0598(15) Uani 1 1 d . . . .
O6 O 0.5969(4) 0.2421(4) -0.0620(3) 0.0442(12) Uani 1 1 d . . . .
O7 O 0.6344(5) 0.1031(4) 0.7592(4) 0.0667(18) Uani 1 1 d . . . .
O8 O 0.5832(4) 0.2279(4) 0.7298(3) 0.0468(13) Uani 1 1 d . . . .
O9 O 0.3254(5) 0.5764(5) 0.8080(6) 0.093(2) Uani 1 1 d . . . .
O10 O 0.2470(4) 0.4374(5) 0.7026(4) 0.0668(17) Uani 1 1 d . . . .
O11 O 1.0496(4) 0.2211(4) 0.9367(4) 0.0643(16) Uani 1 1 d . . . .
O12 O 1.1516(5) 0.3320(4) 1.0767(4) 0.0661(16) Uani 1 1 d . . . .
O13 O 0.1980(5) 0.1504(5) -0.0583(5) 0.097(2) Uani 1 1 d . . . .
O14 O 0.3438(5) 0.1056(4) -0.0271(4) 0.0658(16) Uani 1 1 d . . . .
O15 O 0.3579(4) 0.2563(4) 0.0469(4) 0.0620(15) Uani 1 1 d . . . .
O16 O 0.3137(8) 0.2165(5) -0.1188(6) 0.118(3) Uani 1 1 d . . . .
O17 O 0.2473(5) 0.2944(5) 0.4104(4) 0.085(2) Uani 1 1 d . . . .
O18A O 0.3658(15) 0.2750(12) 0.5597(10) 0.075(5) Uani 0.5 1 d . P A 1
O18B O 0.4029(10) 0.3016(9) 0.4868(12) 0.084(4) Uani 0.5 1 d . P A 2
O19A O 0.1979(13) 0.1751(12) 0.4784(14) 0.105(5) Uani 0.5 1 d . P A 1
O19B O 0.2978(16) 0.2462(13) 0.5582(12) 0.077(5) Uani 0.5 1 d . P A 2
O20A O 0.319(2) 0.167(2) 0.415(2) 0.076(8) Uani 0.5 1 d . P A 1
O20B O 0.290(3) 0.155(2) 0.4221(16) 0.103(12) Uani 0.5 1 d . P A 2
O21 O 0.7103(5) 0.4283(4) 0.7766(4) 0.0756(19) Uani 1 1 d . . . .
O22A O 0.7255(16) 0.3599(12) 0.6378(13) 0.104(8) Uani 0.5 1 d . P B 1
O22B O 0.6956(10) 0.4130(11) 0.6259(10) 0.062(4) Uani 0.5 1 d . P B 2
O23A O 0.8592(9) 0.4233(9) 0.7868(11) 0.074(4) Uani 0.5 1 d . P B 1
O23B O 0.7975(11) 0.3339(12) 0.7196(10) 0.086(5) Uani 0.5 1 d . P B 2
O24A O 0.7889(12) 0.5246(9) 0.7012(10) 0.073(4) Uani 0.5 1 d . P B 1
O24B O 0.8631(11) 0.4919(12) 0.7357(9) 0.100(6) Uani 0.5 1 d . P B 2
O25 O 0.8627(12) 0.1288(9) 0.5398(12) 0.118(7) Uani 0.5 1 d D P . .
O26A O 0.8375(15) 0.187(2) 0.250(3) 0.097(14) Uani 0.5 1 d D P C 2
O26B O 0.841(3) 0.189(4) 0.260(3) 0.129(18) Uiso 0.5 1 d D P C 1
N1 N 0.5736(4) 0.1579(4) 0.4575(4) 0.0345(13) Uani 1 1 d . . . .
N2 N 0.6093(4) 0.0830(4) 0.4742(3) 0.0325(13) Uani 1 1 d . . . .
N3 N 0.6138(4) 0.0784(4) 0.3271(3) 0.0301(12) Uani 1 1 d . . . .
N4 N 0.6108(4) 0.0922(4) 0.1802(4) 0.0334(13) Uani 1 1 d . . . .
N5 N 0.5873(4) 0.1736(4) 0.1959(4) 0.0331(13) Uani 1 1 d . . . .
N6 N 0.7236(4) 0.3128(5) 0.4164(4) 0.0474(16) Uani 1 1 d . . . .
N7 N 0.7141(4) 0.3991(5) 0.4390(4) 0.0471(16) Uani 1 1 d . . . .
N8 N 0.5406(4) 0.3299(4) 0.3488(4) 0.0376(14) Uani 1 1 d . . . .
N9 N 0.3716(4) 0.2419(4) 0.2584(4) 0.0336(13) Uani 1 1 d . . . .
N10 N 0.4095(4) 0.1668(4) 0.2555(4) 0.0401(14) Uani 1 1 d . . . .
N11 N 0.5386(5) 0.3984(4) 0.8426(4) 0.0457(15) Uani 1 1 d . . . .
N12 N 0.5785(5) 0.4818(4) 0.9115(4) 0.0449(15) Uani 1 1 d . . . .
N13 N 0.7290(4) 0.4441(4) 0.9720(4) 0.0400(14) Uani 1 1 d . . . .
N14 N 0.8713(5) 0.3932(4) 1.0124(4) 0.0460(15) Uani 1 1 d . . . .
N15 N 0.8084(5) 0.3182(5) 0.9355(4) 0.0456(15) Uani 1 1 d . . . .
C1 C 0.5651(5) 0.1894(5) 0.5372(4) 0.0364(16) Uani 1 1 d . . . .
H1A H 0.542298 0.240436 0.546411 0.044 Uiso 1 1 calc R . . .
C2 C 0.5950(6) 0.1359(5) 0.6059(5) 0.0409(17) Uani 1 1 d . . . .
C3 C 0.6226(6) 0.0683(5) 0.5634(5) 0.0405(17) Uani 1 1 d . . . .
H3 H 0.645880 0.021527 0.590637 0.049 Uiso 1 1 calc R . . .
C4 C 0.6267(6) 0.0357(5) 0.4004(5) 0.0381(16) Uani 1 1 d . . . .
C5 C 0.6533(6) -0.0444(5) 0.4031(5) 0.052(2) Uani 1 1 d . . . .
H5 H 0.663292 -0.071369 0.456553 0.062 Uiso 1 1 calc R . . .
C6 C 0.6652(6) -0.0851(5) 0.3232(5) 0.050(2) Uani 1 1 d . . . .
H6 H 0.682598 -0.140349 0.321923 0.060 Uiso 1 1 calc R . . .
C7 C 0.6505(6) -0.0415(5) 0.2463(5) 0.0407(17) Uani 1 1 d . . . .
H7 H 0.656310 -0.067382 0.191374 0.049 Uiso 1 1 calc R . . .
C8 C 0.6275(6) 0.0396(5) 0.2524(5) 0.0379(16) Uani 1 1 d . . . .
C9 C 0.6170(6) 0.0774(5) 0.0936(5) 0.0439(18) Uani 1 1 d . . . .
H9 H 0.630977 0.026668 0.067332 0.053 Uiso 1 1 calc R . . .
C10 C 0.5987(5) 0.1509(4) 0.0524(4) 0.0310(15) Uani 1 1 d . . . .
C11 C 0.5793(5) 0.2082(5) 0.1181(5) 0.0378(16) Uani 1 1 d . . . .
H11 H 0.563023 0.263173 0.108076 0.045 Uiso 1 1 calc R . . .
C12 C 0.6052(6) 0.1566(6) 0.7061(5) 0.0439(18) Uani 1 1 d . . . .
C13 C 0.6026(6) 0.1663(6) -0.0379(5) 0.0432(18) Uani 1 1 d . . . .
C14 C 0.8245(6) 0.3264(8) 0.4694(6) 0.063(3) Uani 1 1 d . . . .
H14 H 0.856014 0.279950 0.469943 0.075 Uiso 1 1 calc R . . .
C15 C 0.8760(6) 0.4174(7) 0.5230(6) 0.060(2) Uani 1 1 d . . . .
C16 C 0.8065(6) 0.4626(6) 0.5043(5) 0.051(2) Uani 1 1 d . . . .
H16 H 0.818400 0.525204 0.530589 0.061 Uiso 1 1 calc R . . .
C17 C 0.6171(5) 0.4129(6) 0.4033(5) 0.0445(19) Uani 1 1 d . . . .
C18 C 0.5967(6) 0.4940(6) 0.4197(5) 0.051(2) Uani 1 1 d . . . .
H18 H 0.649687 0.549121 0.458659 0.061 Uiso 1 1 calc R . . .
C19 C 0.4948(6) 0.4921(6) 0.3767(6) 0.055(2) Uani 1 1 d . . . .
H19 H 0.479117 0.547608 0.384986 0.066 Uiso 1 1 calc R . . .
C20 C 0.4160(6) 0.4105(5) 0.3221(5) 0.0469(19) Uani 1 1 d . . . .
H20 H 0.347031 0.409275 0.294532 0.056 Uiso 1 1 calc R . . .
C21 C 0.4421(5) 0.3321(5) 0.3098(4) 0.0342(16) Uani 1 1 d . . . .
C22 C 0.2689(5) 0.2144(5) 0.2069(5) 0.0431(18) Uani 1 1 d . . . .
H22 H 0.226539 0.252335 0.199061 0.052 Uiso 1 1 calc R . . .
C23 C 0.2373(5) 0.1207(5) 0.1678(5) 0.0426(18) Uani 1 1 d . . . .
C24 C 0.3264(6) 0.0948(5) 0.2010(5) 0.0473(19) Uani 1 1 d . . . .
H24 H 0.327404 0.033617 0.186346 0.057 Uiso 1 1 calc R . . .
C25 C 0.9891(7) 0.4600(10) 0.5944(7) 0.074(3) Uani 1 1 d . . . .
C26 C 0.1312(6) 0.0640(6) 0.1002(6) 0.058(2) Uani 1 1 d . . . .
C27 C 0.4434(5) 0.3939(6) 0.7866(5) 0.0466(19) Uani 1 1 d . . . .
H27 H 0.397310 0.344180 0.734320 0.056 Uiso 1 1 calc R . . .
C28 C 0.4198(6) 0.4740(5) 0.8156(6) 0.0471(19) Uani 1 1 d . . . .
C29 C 0.5088(6) 0.5275(5) 0.8959(6) 0.049(2) Uani 1 1 d . . . .
H29 H 0.518569 0.585267 0.932593 0.058 Uiso 1 1 calc R . . .
C30 C 0.6816(6) 0.5055(5) 0.9847(5) 0.0413(17) Uani 1 1 d . . . .
C31 C 0.7275(6) 0.5825(5) 1.0601(5) 0.0490(19) Uani 1 1 d . . . .
H31 H 0.692012 0.624103 1.066966 0.059 Uiso 1 1 calc R . . .
C32 C 0.8272(6) 0.5965(6) 1.1254(6) 0.053(2) Uani 1 1 d . . . .
H32 H 0.859737 0.647987 1.177926 0.064 Uiso 1 1 calc R . . .
C33 C 0.8814(6) 0.5345(6) 1.1146(6) 0.051(2) Uani 1 1 d . . . .
H33 H 0.949527 0.543229 1.157679 0.061 Uiso 1 1 calc R . . .
C34 C 0.8263(6) 0.4600(5) 1.0356(5) 0.0448(18) Uani 1 1 d . . . .
C35 C 0.9690(6) 0.3924(6) 1.0496(6) 0.053(2) Uani 1 1 d . . . .
H35 H 1.024361 0.436187 1.102366 0.063 Uiso 1 1 calc R . . .
C36 C 0.9740(6) 0.3166(6) 0.9972(6) 0.052(2) Uani 1 1 d . . . .
C37 C 0.8713(6) 0.2719(5) 0.9262(5) 0.0465(19) Uani 1 1 d . . . .
H37 H 0.850595 0.217433 0.879294 0.056 Uiso 1 1 calc R . . .
C38 C 0.3234(7) 0.4977(6) 0.7712(6) 0.056(2) Uani 1 1 d . . . .
C39 C 1.0662(7) 0.2904(6) 1.0077(6) 0.059(2) Uani 1 1 d . . . .
C40 C 0.9004(19) 0.085(2) 0.7040(15) 0.145(13) Uani 0.5 1 d D P . .
H40A H 0.857683 0.020144 0.679471 0.218 Uiso 0.5 1 calc GR P . .
H40B H 0.865398 0.120326 0.728235 0.218 Uiso 0.5 1 calc GR P . .
H40C H 0.965581 0.089760 0.755479 0.218 Uiso 0.5 1 calc GR P . .
C41 C 0.9224(19) 0.1288(13) 0.6145(17) 0.169(16) Uani 0.5 1 d D P . .
C42 C 1.048(2) 0.1623(17) 0.632(2) 0.173(17) Uani 0.5 1 d D P . .
H42A H 1.056114 0.197505 0.584649 0.259 Uiso 0.5 1 calc GR P . .
H42B H 1.069082 0.107560 0.624362 0.259 Uiso 0.5 1 calc GR P . .
H42C H 1.090909 0.201063 0.695655 0.259 Uiso 0.5 1 calc GR P . .
C43 C 1.0008(10) 0.2375(11) 0.2344(10) 0.124(5) Uani 1 1 d . . . .
H43A H 0.972061 0.265692 0.181355 0.187 Uiso 1 1 calc GR . . .
H43B H 1.043034 0.203589 0.220653 0.187 Uiso 1 1 calc GR . . .
H43C H 1.042903 0.285856 0.292516 0.187 Uiso 1 1 calc GR . . .
C44 C 0.9118(10) 0.1691(10) 0.2483(14) 0.160(8) Uani 1 1 d D . . .
C45A C 0.937(2) 0.092(2) 0.314(2) 0.135(10) Uiso 0.5 1 d . P C 1
H45A H 0.931108 0.108727 0.373720 0.202 Uiso 0.5 1 calc GR P C 1
H45B H 1.006238 0.090394 0.328219 0.202 Uiso 0.5 1 calc GR P C 1
H45C H 0.887907 0.030263 0.279107 0.202 Uiso 0.5 1 calc GR P C 1
C45B C 0.9250(19) 0.0711(18) 0.2332(18) 0.101(7) Uiso 0.5 1 d . P C 2
H45D H 0.902507 0.035668 0.274128 0.152 Uiso 0.5 1 calc GR P C 2
H45E H 0.996955 0.078260 0.249321 0.152 Uiso 0.5 1 calc GR P C 2
H45F H 0.883701 0.038437 0.166627 0.152 Uiso 0.5 1 calc GR P C 2
O27 O 0.8249(5) 0.3559(5) 0.2163(5) 0.084(2) Uani 1 1 d . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
N1 Fe1 N5 147.6(2) . .
N1 Fe1 N6 90.3(2) . .
N3 Fe1 N1 73.82(19) . .
N3 Fe1 N5 73.99(19) . .
N3 Fe1 N6 103.5(2) . .
N3 Fe1 N10 108.3(2) . .
N5 Fe1 N6 100.5(2) . .
N8 Fe1 N1 100.6(2) . .
N8 Fe1 N3 173.86(19) . .
N8 Fe1 N5 111.7(2) . .
N8 Fe1 N6 73.7(2) . .
N8 Fe1 N10 74.4(2) . .
N10 Fe1 N1 95.6(2) . .
N10 Fe1 N5 91.1(2) . .
N10 Fe1 N6 148.1(2) . .
O6 Fe2 O21 171.7(2) 1_556 .
O6 Fe2 N11 89.2(2) 1_556 .
O6 Fe2 N13 90.1(2) 1_556 .
O6 Fe2 N15 88.6(2) 1_556 .
O8 Fe2 O6 97.8(2) . 1_556
O8 Fe2 O21 89.7(2) . .
O8 Fe2 N11 104.3(2) . .
O8 Fe2 N13 171.8(2) . .
O8 Fe2 N15 109.4(2) . .
N11 Fe2 O21 85.5(2) . .
N11 Fe2 N15 146.2(2) . .
N13 Fe2 O21 82.3(2) . .
N13 Fe2 N11 73.6(2) . .
N13 Fe2 N15 72.8(2) . .
N15 Fe2 O21 92.1(2) . .
O13 Cl1 O14 107.8(4) . .
O13 Cl1 O15 108.1(4) . .
O14 Cl1 O15 110.0(3) . .
O16 Cl1 O13 109.3(5) . .
O16 Cl1 O14 110.5(4) . .
O16 Cl1 O15 111.1(4) . .
O17 Cl2 O18B 90.9(6) . .
O17 Cl2 O19A 101.1(7) . .
O17 Cl2 O20A 114.7(10) . .
O18A Cl2 O17 120.4(8) . .
O18A Cl2 O19A 103.7(11) . .
O18A Cl2 O20A 112.0(14) . .
O19B Cl2 O17 117.7(8) . .
O19B Cl2 O18B 100.6(10) . .
O20A Cl2 O19A 101.5(14) . .
O20B Cl2 O17 118.8(12) . .
O20B Cl2 O18B 101.8(15) . .
O20B Cl2 O19B 118.1(14) . .
O21 Cl3 O23B 108.7(6) . .
O21 Cl3 O24A 102.0(5) . .
O22A Cl3 O21 116.4(8) . .
O22A Cl3 O24A 111.5(11) . .
O22B Cl3 O21 102.2(7) . .
O22B Cl3 O23B 103.1(8) . .
O23A Cl3 O21 101.5(7) . .
O23A Cl3 O22A 115.9(13) . .
O23A Cl3 O24A 108.2(8) . .
O24B Cl3 O21 127.7(7) . .
O24B Cl3 O22B 110.8(9) . .
O24B Cl3 O23B 102.0(11) . .
C13 O6 Fe2 135.7(5) . 1_554
C12 O8 Fe2 130.1(5) . .
Cl3 O21 Fe2 132.3(4) . .
N2 N1 Fe1 114.6(4) . .
C1 N1 Fe1 138.6(5) . .
C1 N1 N2 105.5(5) . .
N1 N2 C4 117.9(5) . .
C3 N2 N1 111.0(5) . .
C3 N2 C4 131.1(6) . .
C4 N3 Fe1 121.0(4) . .
C4 N3 C8 117.4(6) . .
C8 N3 Fe1 121.6(4) . .
N5 N4 C8 119.0(5) . .
C9 N4 N5 111.0(5) . .
C9 N4 C8 130.0(6) . .
N4 N5 Fe1 114.3(4) . .
C11 N5 Fe1 140.6(5) . .
C11 N5 N4 105.1(5) . .
N7 N6 Fe1 113.2(4) . .
C14 N6 Fe1 142.9(7) . .
C14 N6 N7 102.9(7) . .
N6 N7 C17 121.0(6) . .
C16 N7 N6 111.8(6) . .
C16 N7 C17 127.0(7) . .
C17 N8 Fe1 121.7(5) . .
C21 N8 Fe1 121.2(5) . .
C21 N8 C17 117.1(6) . .
N10 N9 C21 118.9(5) . .
C22 N9 N10 111.0(6) . .
C22 N9 C21 130.1(6) . .
N9 N10 Fe1 114.5(4) . .
C24 N10 Fe1 141.3(5) . .
C24 N10 N9 104.1(6) . .
N12 N11 Fe2 114.1(4) . .
C27 N11 Fe2 140.2(5) . .
C27 N11 N12 105.4(6) . .
N11 N12 C30 118.5(6) . .
C29 N12 N11 110.8(6) . .
C29 N12 C30 130.7(6) . .
C30 N13 Fe2 121.0(5) . .
C34 N13 Fe2 121.3(5) . .
C34 N13 C30 117.7(6) . .
N15 N14 C34 117.7(6) . .
C35 N14 N15 111.4(6) . .
C35 N14 C34 130.8(7) . .
N14 N15 Fe2 114.9(4) . .
C37 N15 Fe2 138.9(5) . .
C37 N15 N14 104.8(6) . .
N1 C1 C2 111.1(6) . .
C1 C2 C12 125.7(7) . .
C3 C2 C1 105.5(6) . .
C3 C2 C12 128.4(7) . .
N2 C3 C2 106.9(6) . .
N3 C4 N2 112.0(6) . .
N3 C4 C5 123.6(6) . .
C5 C4 N2 124.4(6) . .
C4 C5 C6 118.1(7) . .
C7 C6 C5 118.4(7) . .
C8 C7 C6 118.6(6) . .
N3 C8 N4 111.0(5) . .
N3 C8 C7 123.8(6) . .
C7 C8 N4 125.1(6) . .
N4 C9 C10 107.3(6) . .
C9 C10 C11 105.4(6) . .
C9 C10 C13 126.2(6) . .
C11 C10 C13 128.4(6) . .
N5 C11 C10 111.2(6) . .
O7 C12 O8 125.9(6) . .
O7 C12 C2 118.1(7) . .
O8 C12 C2 116.0(6) . .
O5 C13 C10 115.2(6) . .
O6 C13 O5 124.9(6) . .
O6 C13 C10 119.8(7) . .
N6 C14 C15 111.8(8) . .
C14 C15 C25 128.2(10) . .
C16 C15 C14 107.1(7) . .
C16 C15 C25 124.6(10) . .
C15 C16 N7 106.4(8) . .
N8 C17 N7 110.2(7) . .
C18 C17 N7 127.1(7) . .
C18 C17 N8 122.6(7) . .
C17 C18 C19 117.6(7) . .
C20 C19 C18 121.5(8) . .
C21 C20 C19 117.5(7) . .
N8 C21 N9 111.0(6) . .
C20 C21 N8 123.6(6) . .
C20 C21 N9 125.4(6) . .
N9 C22 C23 107.5(6) . .
C22 C23 C24 105.4(6) . .
C22 C23 C26 125.2(7) . .
C24 C23 C26 129.3(8) . .
N10 C24 C23 112.0(7) . .
O3 C25 O4 126.1(10) . .
O3 C25 C15 121.0(12) . .
O4 C25 C15 112.9(10) . .
O1 C26 C23 114.6(8) . .
O2 C26 O1 124.5(7) . .
O2 C26 C23 120.9(8) . .
N11 C27 C28 111.5(7) . .
C27 C28 C38 128.8(7) . .
C29 C28 C27 104.4(6) . .
C29 C28 C38 126.8(7) . .
N12 C29 C28 107.9(7) . .
N13 C30 N12 112.5(6) . .
N13 C30 C31 123.3(7) . .
C31 C30 N12 124.2(7) . .
C30 C31 C32 117.9(7) . .
C31 C32 C33 121.2(7) . .
C34 C33 C32 115.0(7) . .
N13 C34 N14 113.1(6) . .
N13 C34 C33 125.0(7) . .
C33 C34 N14 121.9(7) . .
N14 C35 C36 108.2(7) . .
C35 C36 C37 104.9(7) . .
C35 C36 C39 127.7(8) . .
C37 C36 C39 127.3(8) . .
N15 C37 C36 110.7(7) . .
O9 C38 O10 126.2(8) . .
O9 C38 C28 115.7(8) . .
O10 C38 C28 118.1(8) . .
O11 C39 C36 113.9(7) . .
O12 C39 O11 124.8(8) . .
O12 C39 C36 121.2(8) . .
O25 C41 C40 128(2) . .
O25 C41 C42 116(2) . .
C40 C41 C42 114.8(19) . .
O26A C44 C43 124.7(18) . .
O26A C44 C45B 127.6(19) . .
O26B C44 C43 125(3) . .
O26B C44 C45A 105(3) . .
C43 C44 C45A 119.6(14) . .
C45B C44 C43 106.2(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 2.137(5) .
Fe1 N3 2.106(5) .
Fe1 N5 2.140(5) .
Fe1 N6 2.184(6) .
Fe1 N8 2.104(6) .
Fe1 N10 2.128(5) .
Fe2 O6 2.134(5) 1_556
Fe2 O8 1.967(5) .
Fe2 O21 2.221(6) .
Fe2 N11 2.185(6) .
Fe2 N13 2.146(6) .
Fe2 N15 2.202(6) .
Cl1 O13 1.412(7) .
Cl1 O14 1.427(6) .
Cl1 O15 1.439(5) .
Cl1 O16 1.390(7) .
Cl2 O17 1.386(6) .
Cl2 O18A 1.368(14) .
Cl2 O18B 1.553(14) .
Cl2 O19A 1.543(14) .
Cl2 O19B 1.365(15) .
Cl2 O20A 1.46(2) .
Cl2 O20B 1.33(3) .
Cl3 O21 1.441(6) .
Cl3 O22A 1.350(14) .
Cl3 O22B 1.402(13) .
Cl3 O23A 1.329(11) .
Cl3 O23B 1.548(15) .
Cl3 O24A 1.510(11) .
Cl3 O24B 1.376(12) .
O1 C26 1.306(10) .
O2 C26 1.232(9) .
O3 C25 1.214(13) .
O4 C25 1.269(14) .
O5 C13 1.295(9) .
O6 C13 1.250(8) .
O7 C12 1.243(8) .
O8 C12 1.252(8) .
O9 C38 1.244(9) .
O10 C38 1.253(10) .
O11 C39 1.325(9) .
O12 C39 1.239(9) .
O25 C41 1.147(18) .
O26A C44 1.196(17) .
O26B C44 1.221(18) .
N1 N2 1.369(7) .
N1 C1 1.321(8) .
N2 C3 1.354(8) .
N2 C4 1.408(8) .
N3 C4 1.327(8) .
N3 C8 1.333(8) .
N4 N5 1.375(7) .
N4 C8 1.409(8) .
N4 C9 1.360(8) .
N5 C11 1.326(8) .
N6 N7 1.365(9) .
N6 C14 1.337(9) .
N7 C16 1.364(9) .
N7 C17 1.395(9) .
N8 C17 1.368(9) .
N8 C21 1.347(8) .
N9 N10 1.384(8) .
N9 C21 1.406(8) .
N9 C22 1.331(8) .
N10 C24 1.312(9) .
N11 N12 1.382(8) .
N11 C27 1.311(8) .
N12 C29 1.334(9) .
N12 C30 1.423(9) .
N13 C30 1.328(9) .
N13 C34 1.328(9) .
N14 N15 1.371(8) .
N14 C34 1.419(9) .
N14 C35 1.327(9) .
N15 C37 1.325(8) .
C1 C2 1.399(9) .
C2 C3 1.374(9) .
C2 C12 1.473(9) .
C4 C5 1.359(9) .
C5 C6 1.398(10) .
C6 C7 1.381(9) .
C7 C8 1.349(9) .
C9 C10 1.365(9) .
C10 C11 1.411(9) .
C10 C13 1.442(9) .
C14 C15 1.374(12) .
C15 C16 1.325(11) .
C15 C25 1.513(12) .
C17 C18 1.348(10) .
C18 C19 1.375(10) .
C19 C20 1.368(10) .
C20 C21 1.347(9) .
C22 C23 1.357(10) .
C23 C24 1.383(10) .
C23 C26 1.461(10) .
C27 C28 1.410(10) .
C28 C29 1.380(10) .
C28 C38 1.471(10) .
C30 C31 1.364(10) .
C31 C32 1.368(10) .
C32 C33 1.404(10) .
C33 C34 1.373(10) .
C35 C36 1.358(11) .
C36 C37 1.411(10) .
C36 C39 1.458(11) .
C40 C41 1.68(2) .
C41 C42 1.69(2) .
C43 C44 1.54(2) .
C44 C45A 1.64(3) .
C44 C45B 1.54(3) .
