#------------------------------------------------------------------------------
#$Date: 2022-08-06 14:47:09 +0300 (Sat, 06 Aug 2022) $
#$Revision: 277106 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/06/7710600.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_7710600
loop_
_publ_author_name
'Chegerev, Maxim'
'Demidov, Oleg'
'Vasilyev, Pavel'
'Efimov, Nikolay'
'Kubrin, Stanislav'
'Starikov, Andrey'
'Vlasenko, Valery'
'Piskunov, Alexander'
'Shapovalova, Svetlana'
'Guda, Alexander'
'Rusalev, Yury'
'Soldatov, Alexander'
_publ_section_title
;
 Spin transitions in ferric catecholate complexes mediated by outer-sphere
 counteranions.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10909
_journal_page_last               10919
_journal_paper_doi               10.1039/d2dt01207c
_journal_volume                  51
_journal_year                    2022
_chemical_compound_source        'Rostov-on-Don, Russia'
_chemical_formula_moiety         'C32 H38 Fe N4 O2, Cl O4, 0.5(H2 O)'
_chemical_formula_sum            'C32 H39 Cl Fe N4 O6.5'
_chemical_formula_weight         674.97
_chemical_name_common
'3 - (3,6-Di-tert-butylcatecholato)-(tris(2-pyridylmethyl)amine)-iron(iii) percholrate'
_chemical_name_systematic
'3 - (3,6-Di-tert-butylcatecholato)-(tris(2-pyridylmethyl)amine)-iron(iii) percholrate'
_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_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-04-03 deposited with the CCDC.	2022-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                97.511(2)
_cell_angle_beta                 92.574(2)
_cell_angle_gamma                106.888(2)
_cell_formula_units_Z            2
_cell_length_a                   8.3709(2)
_cell_length_b                   10.3122(2)
_cell_length_c                   19.7722(3)
_cell_measurement_reflns_used    15672
_cell_measurement_temperature    100.01(11)
_cell_measurement_theta_max      75.8030
_cell_measurement_theta_min      4.5070
_cell_volume                     1612.97(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2529
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -113.00 -13.00   1.00    1.00    --  -41.35 -57.00-180.00  100
  2  ω   -114.00 -62.00   1.00    1.00    --  -41.35-148.00-106.00   52
  3  ω   -116.00 -17.00   1.00    1.00    --  -41.35 -38.00 -90.00   99
  4  ω     27.00  97.00   1.00    1.00    --   41.35-125.00  60.00   70
  5  ω     17.00 116.00   1.00    1.00    --   41.35  38.00 120.00   99
  6  ω    -21.00  74.00   1.00    1.00    --   41.35 -77.00-120.00   95
  7  ω      8.00  42.00   1.00    1.00    --   41.35  80.00 153.97   34
  8  ω     61.00 146.00   1.00    2.57    --  112.00 178.00  90.00   85
  9  ω     30.00 106.00   1.00    2.57    --  112.00 -95.00-120.00   76
 10  ω     37.00 136.00   1.00    2.57    --  112.00 -36.00-159.88   99
 11  ω     84.00 178.00   1.00    2.57    --  112.00  30.00 -90.00   94
 12  ω     36.00 109.00   1.00    2.57    --  112.00-111.00 -30.00   73
 13  ω     36.00 145.00   1.00    2.57    --  112.00 -77.00  90.00  109
 14  ω    103.00 178.00   1.00    2.57    --  112.00  77.00 120.00   75
 15  ω    104.00 178.00   1.00    2.57    --  112.00 111.00 -60.00   74
 16  ω     61.00 146.00   1.00    2.57    --  112.00 178.00  30.00   85
 17  ω     30.00 106.00   1.00    2.57    --  112.00 -95.00 -90.00   76
 18  ω    104.00 178.00   1.00    2.57    --  112.00 111.00  90.00   74
 19  ω     36.00 145.00   1.00    2.57    --  112.00 -77.00 -30.00  109
 20  ω    104.00 178.00   1.00    2.57    --  112.00 111.00 -30.00   74
 21  ω     36.00 109.00   1.00    2.57    --  112.00-111.00  30.00   73
 22  ω     30.00 106.00   1.00    2.57    --  112.00 -95.00  90.00   76
 23  ω     61.00 146.00   1.00    2.57    --  112.00 178.00 -30.00   85
 24  ω     40.00 141.00   1.00    2.57    --  112.00 -61.00   0.00  101
 25  ω     30.00 165.00   1.00    2.57    --  112.00 -15.00 -90.00  135
 26  ω     39.00 138.00   1.00    2.57    --  112.00 -45.00-120.00   99
 27  ω     30.00 106.00   1.00    2.57    --  112.00 -95.00-180.00   76
 28  ω     40.00 141.00   1.00    2.57    --  112.00 -61.00  30.00  101
 29  ω     36.00 145.00   1.00    2.57    --  112.00 -77.00-180.00  109
 30  ω     30.00 165.00   1.00    2.57    --  112.00 -15.00  60.00  135
 31  ω     61.00 146.00   1.00    2.57    --  112.00 178.00 150.00   85
 32  ω     36.00 109.00   1.00    2.57    --  112.00-111.00-120.00   73
 33  ω     36.00 109.00   1.00    2.57    --  112.00-111.00 -60.00   73
 34  ω     39.00 111.00   1.00    2.57    --  112.00-124.00  58.00   72
 35  ω     30.00 106.00   1.00    2.57    --  112.00 -95.00 -30.00   76
 36  ω     73.00 106.00   1.00    2.57    --  112.00 -95.00 120.00   33
 37  ω     95.00 175.00   1.00    2.57    --  112.00  45.00  60.00   80
 38  ω     90.00 147.00   1.00    2.57    --  112.00 -86.00  30.95   57
 39  ω     84.00 116.00   1.00    2.57    --  112.00  61.00  30.00   32
 40  ω    135.00 162.00   1.00    2.57    --  112.00  61.00  30.00   27
 41  ω     40.00  68.00   1.00    2.57    --  112.00 -61.00  90.00   28
 42  ω     77.00 132.00   1.00    2.57    --  112.00 -30.00 -30.00   55
 43  ω     40.00  67.00   1.00    2.57    --  112.00 -86.00  30.95   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1880655000
_diffrn_orient_matrix_UB_12      -0.0361513000
_diffrn_orient_matrix_UB_13      0.0108268000
_diffrn_orient_matrix_UB_21      -0.0435410000
_diffrn_orient_matrix_UB_22      -0.0419626000
_diffrn_orient_matrix_UB_23      -0.0778507000
_diffrn_orient_matrix_UB_31      -0.0033656000
_diffrn_orient_matrix_UB_32      -0.1478900000
_diffrn_orient_matrix_UB_33      0.0067740000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33846
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.446
_diffrn_reflns_theta_min         2.263
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.936
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.664
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       block
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.232
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         6759
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0535P)²+0.8414P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0941
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6557
_reflns_number_total             6759
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt01207c2.cif
_cod_data_source_block           tpafe36clo4_100
_cod_depositor_comments
'Adding full bibliography for 7710599--7710604.cif.'
_cod_original_formula_sum        'C32 H39 Cl Fe N4 O6.50'
_cod_database_code               7710600
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C32 H38 Fe N4 O2, Cl O4'
_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   0.424
_shelx_estimated_absorpt_t_min   0.277
_reflns_odcompleteness_completeness 98.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.17
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O3A-O6A \\sim O6-O3
 with sigma of 0.04
 Cl1-O5 \\sim Cl1A-O5
 with sigma of 0.02
 Cl1-O3A \\sim Cl1A-O6
 with sigma of 0.02
 Cl1-O6A \\sim Cl1A-O3
 with sigma of 0.02
 Cl1-O4A \\sim Cl1A-O4
 with sigma of 0.02
 O5-O6A \\sim O5-O3
 with sigma of 0.04
 O6A-O4A \\sim O3-O4
 with sigma of 0.04
 O5-O3A \\sim O5-O6
 with sigma of 0.04
 O5-O4A \\sim O5-O4
 with sigma of 0.04
 O3A-O4A \\sim O6-O4
 with sigma of 0.04
3. Others
 Sof(O6)=Sof(O3)=Sof(Cl1A)=Sof(O4)=1-FVAR(1)
 Sof(Cl1)=Sof(O3A)=Sof(O6A)=Sof(O4A)=FVAR(1)
 Fixed Sof: O7(0.5) H7A(0.5) H7B(0.5)
4.a Free rotating group:
 O7(H7A,H7B)
4.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C20(H20A,H20B), C32(H32A,H32B)
4.c Aromatic/amide H refined with riding coordinates:
 C27(H27), C30(H30), C29(H29), C15(H15), C21(H21), C5(H5), C23(H23), C4(H4),
 C22(H22), C24(H24), C18(H18), C16(H16), C28(H28), C17(H17)
4.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C8(H8A,H8B,H8C),
 C10(H10A,H10B,H10C), C14(H14A,H14B,H14C)
;
_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 1.466
_oxdiff_exptl_absorpt_empirical_full_min 0.779
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_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe 0.42923(3) 0.18432(2) 0.76486(2) 0.01575(8) Uani 1 1 d . . . . .
O1 O 0.29075(14) 0.00313(11) 0.73180(6) 0.0182(2) Uani 1 1 d . . . . .
O2 O 0.39048(14) 0.22140(11) 0.67736(6) 0.0192(2) Uani 1 1 d . . . . .
N3 N 0.24983(17) 0.24640(13) 0.80670(7) 0.0184(3) Uani 1 1 d . . . . .
N4 N 0.62462(17) 0.12062(14) 0.74714(7) 0.0196(3) Uani 1 1 d . . . . .
N1 N 0.56917(17) 0.37218(14) 0.79983(7) 0.0205(3) Uani 1 1 d . . . . .
N2 N 0.47339(17) 0.14388(14) 0.85867(7) 0.0190(3) Uani 1 1 d . . . . .
C1 C 0.26883(19) -0.01558(16) 0.66349(8) 0.0179(3) Uani 1 1 d . . . . .
C2 C 0.3215(2) 0.10599(16) 0.63302(8) 0.0188(3) Uani 1 1 d . . . . .
C27 C 0.7191(2) 0.14217(18) 0.69394(9) 0.0237(3) Uani 1 1 d . . . . .
H27 H 0.6902 0.1892 0.6607 0.028 Uiso 1 1 calc R U . . .
C31 C 0.6646(2) 0.05082(16) 0.79534(9) 0.0213(3) Uani 1 1 d . . . . .
C26 C 0.3076(2) 0.10902(17) 0.88758(8) 0.0217(3) Uani 1 1 d . . . . .
H26A H 0.3226 0.1148 0.9369 0.026 Uiso 1 1 calc R U . . .
H26B H 0.2414 0.0164 0.8685 0.026 Uiso 1 1 calc R U . . .
C6 C 0.1946(2) -0.14486(17) 0.62280(9) 0.0205(3) Uani 1 1 d . . . . .
C19 C 0.6222(2) 0.39354(17) 0.86659(9) 0.0227(3) Uani 1 1 d . . . . .
C3 C 0.3000(2) 0.10468(18) 0.56162(8) 0.0225(3) Uani 1 1 d . . . . .
C30 C 0.8043(2) 0.00477(17) 0.79236(10) 0.0257(3) Uani 1 1 d . . . . .
H30 H 0.8321 -0.0410 0.8265 0.031 Uiso 1 1 calc R U . . .
C25 C 0.2204(2) 0.21019(16) 0.86927(8) 0.0203(3) Uani 1 1 d . . . . .
C7 C 0.1467(2) -0.27838(17) 0.65382(9) 0.0222(3) Uani 1 1 d . . . . .
C29 C 0.9021(2) 0.02780(18) 0.73776(10) 0.0277(4) Uani 1 1 d . . . . .
H29 H 0.9964 -0.0024 0.7349 0.033 Uiso 1 1 calc R U . . .
C15 C 0.5908(2) 0.48022(17) 0.76567(9) 0.0246(3) Uani 1 1 d . . . . .
H15 H 0.5541 0.4650 0.7194 0.029 Uiso 1 1 calc R U . . .
C20 C 0.5954(2) 0.26735(17) 0.90051(9) 0.0231(3) Uani 1 1 d . . . . .
H20A H 0.7019 0.2494 0.9079 0.028 Uiso 1 1 calc R U . . .
H20B H 0.5543 0.2839 0.9449 0.028 Uiso 1 1 calc R U . . .
C21 C 0.1786(2) 0.33569(17) 0.78403(9) 0.0222(3) Uani 1 1 d . . . . .
H21 H 0.1973 0.3588 0.7405 0.027 Uiso 1 1 calc R U . . .
C32 C 0.5447(2) 0.02664(17) 0.85007(9) 0.0226(3) Uani 1 1 d . . . . .
H32A H 0.4561 -0.0589 0.8366 0.027 Uiso 1 1 calc R U . . .
H32B H 0.6030 0.0218 0.8927 0.027 Uiso 1 1 calc R U . . .
C11 C 0.3567(2) 0.23690(19) 0.52996(9) 0.0263(4) Uani 1 1 d . . . . .
C9 C 0.0208(2) -0.27520(17) 0.70757(9) 0.0250(3) Uani 1 1 d . . . . .
H9A H 0.0715 -0.2029 0.7448 0.038 Uiso 1 1 calc R U . . .
H9B H -0.0112 -0.3614 0.7245 0.038 Uiso 1 1 calc R U . . .
H9C H -0.0766 -0.2593 0.6871 0.038 Uiso 1 1 calc R U . . .
C5 C 0.1737(2) -0.14308(18) 0.55283(9) 0.0257(3) Uani 1 1 d . . . . .
H5 H 0.1239 -0.2257 0.5243 0.031 Uiso 1 1 calc R U . . .
C23 C 0.0490(2) 0.35802(18) 0.88811(10) 0.0267(4) Uani 1 1 d . . . . .
H23 H -0.0176 0.3965 0.9157 0.032 Uiso 1 1 calc R U . . .
C4 C 0.2241(2) -0.02297(19) 0.52325(9) 0.0274(4) Uani 1 1 d . . . . .
H4 H 0.2058 -0.0291 0.4760 0.033 Uiso 1 1 calc R U . . .
C12 C 0.2603(3) 0.33558(19) 0.55803(9) 0.0291(4) Uani 1 1 d . . . . .
H12A H 0.1422 0.2924 0.5473 0.044 Uiso 1 1 calc R U . . .
H12B H 0.2942 0.4176 0.5375 0.044 Uiso 1 1 calc R U . . .
H12C H 0.2844 0.3584 0.6068 0.044 Uiso 1 1 calc R U . . .
C22 C 0.0782(2) 0.39410(18) 0.82372(10) 0.0273(4) Uani 1 1 d . . . . .
H22 H 0.0312 0.4566 0.8074 0.033 Uiso 1 1 calc R U . . .
C24 C 0.1201(2) 0.26365(18) 0.91113(9) 0.0242(3) Uani 1 1 d . . . . .
H24 H 0.1004 0.2371 0.9539 0.029 Uiso 1 1 calc R U . . .
C18 C 0.7009(2) 0.52382(19) 0.90137(10) 0.0310(4) Uani 1 1 d . . . . .
H18 H 0.7389 0.5366 0.9474 0.037 Uiso 1 1 calc R U . . .
C16 C 0.6662(3) 0.61263(19) 0.79772(11) 0.0321(4) Uani 1 1 d . . . . .
H16 H 0.6791 0.6860 0.7735 0.039 Uiso 1 1 calc R U . . .
C28 C 0.8580(2) 0.09616(18) 0.68754(10) 0.0275(4) Uani 1 1 d . . . . .
H28 H 0.9209 0.1108 0.6501 0.033 Uiso 1 1 calc R U . . .
C13 C 0.5455(3) 0.3059(2) 0.54741(10) 0.0332(4) Uani 1 1 d . . . . .
H13A H 0.5685 0.3315 0.5961 0.050 Uiso 1 1 calc R U . . .
H13B H 0.5805 0.3862 0.5256 0.050 Uiso 1 1 calc R U . . .
H13C H 0.6056 0.2431 0.5314 0.050 Uiso 1 1 calc R U . . .
C8 C 0.3062(2) -0.29747(19) 0.68782(10) 0.0294(4) Uani 1 1 d . . . . .
H8A H 0.3819 -0.3063 0.6537 0.044 Uiso 1 1 calc R U . . .
H8B H 0.2765 -0.3786 0.7092 0.044 Uiso 1 1 calc R U . . .
H8C H 0.3595 -0.2193 0.7218 0.044 Uiso 1 1 calc R U . . .
C10 C 0.0652(3) -0.40330(18) 0.59886(10) 0.0312(4) Uani 1 1 d . . . . .
H10A H -0.0347 -0.3931 0.5775 0.047 Uiso 1 1 calc R U . . .
H10B H 0.0373 -0.4850 0.6198 0.047 Uiso 1 1 calc R U . . .
H10C H 0.1423 -0.4099 0.5650 0.047 Uiso 1 1 calc R U . . .
C17 C 0.7222(3) 0.6351(2) 0.86645(12) 0.0367(4) Uani 1 1 d . . . . .
H17 H 0.7736 0.7236 0.8889 0.044 Uiso 1 1 calc R U . . .
C14 C 0.3219(3) 0.2087(2) 0.45153(10) 0.0380(5) Uani 1 1 d . . . . .
H14A H 0.3821 0.1481 0.4327 0.057 Uiso 1 1 calc R U . . .
H14B H 0.3580 0.2934 0.4334 0.057 Uiso 1 1 calc R U . . .
H14C H 0.2040 0.1669 0.4395 0.057 Uiso 1 1 calc R U . . .
Cl1 Cl 0.1792(2) -0.22273(13) 0.93926(5) 0.0239(3) Uani 0.582(4) 1 d D . P A 1
O5 O 0.1301(2) -0.35050(15) 0.97001(7) 0.0417(4) Uani 1 1 d D . . . .
O3A O 0.1958(16) -0.2594(14) 0.8680(4) 0.043(2) Uani 0.582(4) 1 d D . P A 1
O6A O 0.3378(4) -0.1353(3) 0.97208(14) 0.0363(7) Uani 0.582(4) 1 d D . P A 1
O4A O 0.0574(3) -0.1493(3) 0.94538(16) 0.0443(8) Uani 0.582(4) 1 d D . P A 1
O6 O 0.2342(8) -0.1235(4) 0.9854(2) 0.0471(13) Uani 0.418(4) 1 d D . P A 2
O3 O 0.161(2) -0.2420(19) 0.8731(6) 0.042(3) Uani 0.418(4) 1 d D . P A 2
Cl1A Cl 0.2369(3) -0.24466(18) 0.93913(8) 0.0271(4) Uani 0.418(4) 1 d D . P A 2
O4 O 0.4057(6) -0.2453(6) 0.9352(2) 0.0634(16) Uani 0.418(4) 1 d D . P A 2
O7 O -0.0711(6) -0.0594(4) 0.9473(2) 0.0584(9) Uani 0.5 1 d G . P B 2
H7A H 0.0191 -0.0735 0.9611 0.088 Uiso 0.5 1 d G U P B 2
H7B H -0.0801 0.0061 0.9763 0.088 Uiso 0.5 1 d G U P B 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 5 5 0.1558
5 0 -4 0.1311
5 0 -1 0.0988
0 -6 3 0.1034
5 -1 4 0.1148
-5 0 -3 0.1292
0 -6 0 0.0994
3 0 10 0.1387
2 -4 11 0.1570
-1 7 -3 0.0988
0 1 12 0.1463
-1 -5 8 0.1460
3 -6 -2 0.1139
-5 0 4 0.1311
-5 0 0 0.1102
-4 -3 -2 0.1115
0 -6 1 0.0981
5 0 3 0.1102
1 4 6 0.1372
-1 0 -12 0.1577
0 -1 -13 0.1615
1 -6 -1 0.1021
-1 5 8 0.1472
2 -2 -11 0.1662
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
O1 Fe N3 95.20(5) . . ?
O1 Fe N4 88.23(5) . . ?
O1 Fe N1 179.03(5) . . ?
O1 Fe N2 94.18(5) . . ?
O2 Fe O1 85.84(5) . . ?
O2 Fe N3 97.45(5) . . ?
O2 Fe N4 96.76(5) . . ?
O2 Fe N1 94.38(6) . . ?
O2 Fe N2 179.31(5) . . ?
N3 Fe N2 83.24(6) . . ?
N4 Fe N3 165.58(6) . . ?
N4 Fe N1 92.68(6) . . ?
N4 Fe N2 82.55(6) . . ?
N1 Fe N3 83.83(6) . . ?
N1 Fe N2 85.61(6) . . ?
C1 O1 Fe 110.02(9) . . ?
C2 O2 Fe 111.65(9) . . ?
C25 N3 Fe 113.62(11) . . ?
C21 N3 Fe 125.99(11) . . ?
C21 N3 C25 119.46(14) . . ?
C27 N4 Fe 126.50(12) . . ?
C27 N4 C31 119.55(14) . . ?
C31 N4 Fe 113.94(11) . . ?
C19 N1 Fe 114.57(11) . . ?
C19 N1 C15 119.47(15) . . ?
C15 N1 Fe 125.04(12) . . ?
C26 N2 Fe 105.47(10) . . ?
C26 N2 C20 111.39(13) . . ?
C26 N2 C32 112.80(13) . . ?
C20 N2 Fe 109.67(10) . . ?
C32 N2 Fe 106.58(10) . . ?
C32 N2 C20 110.66(13) . . ?
O1 C1 C2 115.21(14) . . ?
O1 C1 C6 123.80(14) . . ?
C6 C1 C2 120.97(15) . . ?
O2 C2 C1 114.87(14) . . ?
O2 C2 C3 122.85(14) . . ?
C3 C2 C1 122.28(15) . . ?
N4 C27 H27 119.1 . . ?
N4 C27 C28 121.73(16) . . ?
C28 C27 H27 119.1 . . ?
N4 C31 C30 121.26(16) . . ?
N4 C31 C32 114.68(14) . . ?
C30 C31 C32 124.04(15) . . ?
N2 C26 H26A 110.2 . . ?
N2 C26 H26B 110.2 . . ?
N2 C26 C25 107.55(13) . . ?
H26A C26 H26B 108.5 . . ?
C25 C26 H26A 110.2 . . ?
C25 C26 H26B 110.2 . . ?
C1 C6 C7 122.04(15) . . ?
C5 C6 C1 115.55(15) . . ?
C5 C6 C7 122.37(15) . . ?
N1 C19 C20 116.02(15) . . ?
N1 C19 C18 121.69(16) . . ?
C18 C19 C20 122.26(16) . . ?
C2 C3 C11 121.40(15) . . ?
C4 C3 C2 115.43(15) . . ?
C4 C3 C11 123.16(15) . . ?
C31 C30 H30 120.5 . . ?
C31 C30 C29 119.10(16) . . ?
C29 C30 H30 120.5 . . ?
N3 C25 C26 113.52(14) . . ?
N3 C25 C24 121.70(15) . . ?
C24 C25 C26 124.78(15) . . ?
C6 C7 C8 109.01(14) . . ?
C6 C7 C10 111.51(14) . . ?
C9 C7 C6 111.13(13) . . ?
C9 C7 C8 109.23(15) . . ?
C9 C7 C10 107.32(15) . . ?
C10 C7 C8 108.58(14) . . ?
C30 C29 H29 120.3 . . ?
C28 C29 C30 119.38(16) . . ?
C28 C29 H29 120.3 . . ?
N1 C15 H15 119.2 . . ?
N1 C15 C16 121.55(17) . . ?
C16 C15 H15 119.2 . . ?
N2 C20 C19 112.31(13) . . ?
N2 C20 H20A 109.1 . . ?
N2 C20 H20B 109.1 . . ?
C19 C20 H20A 109.1 . . ?
C19 C20 H20B 109.1 . . ?
H20A C20 H20B 107.9 . . ?
N3 C21 H21 119.1 . . ?
N3 C21 C22 121.72(16) . . ?
C22 C21 H21 119.1 . . ?
N2 C32 C31 107.17(13) . . ?
N2 C32 H32A 110.3 . . ?
N2 C32 H32B 110.3 . . ?
C31 C32 H32A 110.3 . . ?
C31 C32 H32B 110.3 . . ?
H32A C32 H32B 108.5 . . ?
C3 C11 C12 109.47(14) . . ?
C3 C11 C13 110.24(14) . . ?
C3 C11 C14 111.61(16) . . ?
C12 C11 C14 107.87(15) . . ?
C13 C11 C12 109.41(16) . . ?
C13 C11 C14 108.18(16) . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C5 H5 118.4 . . ?
C6 C5 C4 123.19(16) . . ?
C4 C5 H5 118.4 . . ?
C22 C23 H23 120.3 . . ?
C22 C23 C24 119.41(16) . . ?
C24 C23 H23 120.3 . . ?
C3 C4 C5 122.56(16) . . ?
C3 C4 H4 118.7 . . ?
C5 C4 H4 118.7 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C21 C22 C23 118.94(16) . . ?
C21 C22 H22 120.5 . . ?
C23 C22 H22 120.5 . . ?
C25 C24 C23 118.77(16) . . ?
C25 C24 H24 120.6 . . ?
C23 C24 H24 120.6 . . ?
C19 C18 H18 120.5 . . ?
C19 C18 C17 118.91(18) . . ?
C17 C18 H18 120.5 . . ?
C15 C16 H16 120.4 . . ?
C15 C16 C17 119.18(17) . . ?
C17 C16 H16 120.4 . . ?
C27 C28 C29 118.95(17) . . ?
C27 C28 H28 120.5 . . ?
C29 C28 H28 120.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C18 C17 H17 120.4 . . ?
C16 C17 C18 119.18(18) . . ?
C16 C17 H17 120.4 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O3A Cl1 O5 107.8(6) . . ?
O3A Cl1 O6A 109.3(6) . . ?
O3A Cl1 O4A 108.7(4) . . ?
O6A Cl1 O5 109.38(16) . . ?
O4A Cl1 O5 112.52(16) . . ?
O4A Cl1 O6A 109.0(2) . . ?
O5 Cl1A O6 101.1(3) . . ?
O5 Cl1A O3 109.3(8) . . ?
O3 Cl1A O6 109.0(7) . . ?
O4 Cl1A O5 116.8(3) . . ?
O4 Cl1A O6 108.9(4) . . ?
O4 Cl1A O3 111.1(6) . . ?
H7A O7 H7B 104.5 . . ?
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
Fe O1 1.9017(12) . ?
Fe O2 1.8545(11) . ?
Fe N3 1.9701(14) . ?
Fe N4 1.9608(14) . ?
Fe N1 1.9652(14) . ?
Fe N2 1.9952(13) . ?
O1 C1 1.3358(19) . ?
O2 C2 1.342(2) . ?
N3 C25 1.351(2) . ?
N3 C21 1.344(2) . ?
N4 C27 1.348(2) . ?
N4 C31 1.352(2) . ?
N1 C19 1.343(2) . ?
N1 C15 1.349(2) . ?
N2 C26 1.489(2) . ?
N2 C20 1.497(2) . ?
N2 C32 1.491(2) . ?
C1 C2 1.424(2) . ?
C1 C6 1.416(2) . ?
C2 C3 1.413(2) . ?
C27 H27 0.9300 . ?
C27 C28 1.382(2) . ?
C31 C30 1.385(2) . ?
C31 C32 1.504(2) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C25 1.506(2) . ?
C6 C7 1.535(2) . ?
C6 C5 1.390(2) . ?
C19 C20 1.505(2) . ?
C19 C18 1.384(3) . ?
C3 C11 1.533(2) . ?
C3 C4 1.386(3) . ?
C30 H30 0.9300 . ?
C30 C29 1.388(3) . ?
C25 C24 1.381(2) . ?
C7 C9 1.534(2) . ?
C7 C8 1.543(2) . ?
C7 C10 1.537(2) . ?
C29 H29 0.9300 . ?
C29 C28 1.386(3) . ?
C15 H15 0.9300 . ?
C15 C16 1.379(3) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21 0.9300 . ?
C21 C22 1.383(2) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C11 C12 1.538(2) . ?
C11 C13 1.535(3) . ?
C11 C14 1.538(3) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C5 H5 0.9300 . ?
C5 C4 1.401(3) . ?
C23 H23 0.9300 . ?
C23 C22 1.385(3) . ?
C23 C24 1.392(3) . ?
C4 H4 0.9300 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C22 H22 0.9300 . ?
C24 H24 0.9300 . ?
C18 H18 0.9300 . ?
C18 C17 1.387(3) . ?
C16 H16 0.9300 . ?
C16 C17 1.385(3) . ?
C28 H28 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C17 H17 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
Cl1 O5 1.4805(18) . ?
Cl1 O3A 1.434(9) . ?
Cl1 O6A 1.439(3) . ?
Cl1 O4A 1.437(3) . ?
O5 Cl1A 1.421(2) . ?
O6 Cl1A 1.456(5) . ?
O3 Cl1A 1.435(12) . ?
Cl1A O4 1.420(5) . ?
O7 H7A 0.8498 . ?
O7 H7B 0.8502 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe O1 C1 C2 -12.13(16) . . . . ?
Fe O1 C1 C6 169.64(12) . . . . ?
Fe O2 C2 C1 9.55(16) . . . . ?
Fe O2 C2 C3 -171.38(12) . . . . ?
Fe N3 C25 C26 -10.72(17) . . . . ?
Fe N3 C25 C24 168.94(13) . . . . ?
Fe N3 C21 C22 -166.85(13) . . . . ?
Fe N4 C27 C28 177.89(13) . . . . ?
Fe N4 C31 C30 -176.70(13) . . . . ?
Fe N4 C31 C32 4.30(18) . . . . ?
Fe N1 C19 C20 11.25(18) . . . . ?
Fe N1 C19 C18 -170.49(14) . . . . ?
Fe N1 C15 C16 168.35(14) . . . . ?
Fe N2 C26 C25 -42.87(14) . . . . ?
Fe N2 C20 C19 11.97(16) . . . . ?
Fe N2 C32 C31 40.70(14) . . . . ?
O1 Fe O2 C2 -12.99(10) . . . . ?
O1 C1 C2 O2 2.0(2) . . . . ?
O1 C1 C2 C3 -177.06(14) . . . . ?
O1 C1 C6 C7 -5.7(2) . . . . ?
O1 C1 C6 C5 176.48(14) . . . . ?
O2 C2 C3 C11 0.6(2) . . . . ?
O2 C2 C3 C4 -178.96(15) . . . . ?
N3 Fe O2 C2 -107.70(10) . . . . ?
N3 C25 C24 C23 -0.5(3) . . . . ?
N3 C21 C22 C23 -0.8(3) . . . . ?
N4 Fe O2 C2 74.73(11) . . . . ?
N4 C27 C28 C29 -0.9(3) . . . . ?
N4 C31 C30 C29 -1.7(3) . . . . ?
N4 C31 C32 N2 -30.35(19) . . . . ?
N1 Fe O2 C2 167.96(10) . . . . ?
N1 C19 C20 N2 -15.5(2) . . . . ?
N1 C19 C18 C17 1.3(3) . . . . ?
N1 C15 C16 C17 0.6(3) . . . . ?
N2 C26 C25 N3 36.25(18) . . . . ?
N2 C26 C25 C24 -143.39(16) . . . . ?
C1 C2 C3 C11 179.64(15) . . . . ?
C1 C2 C3 C4 0.0(2) . . . . ?
C1 C6 C7 C9 59.1(2) . . . . ?
C1 C6 C7 C8 -61.3(2) . . . . ?
C1 C6 C7 C10 178.81(15) . . . . ?
C1 C6 C5 C4 0.9(2) . . . . ?
C2 C1 C6 C7 176.15(14) . . . . ?
C2 C1 C6 C5 -1.6(2) . . . . ?
C2 C3 C11 C12 -61.4(2) . . . . ?
C2 C3 C11 C13 59.0(2) . . . . ?
C2 C3 C11 C14 179.27(16) . . . . ?
C2 C3 C4 C5 -0.8(3) . . . . ?
C27 N4 C31 C30 2.2(2) . . . . ?
C27 N4 C31 C32 -176.84(15) . . . . ?
C31 N4 C27 C28 -0.8(3) . . . . ?
C31 C30 C29 C28 0.0(3) . . . . ?
C26 N2 C20 C19 -104.41(16) . . . . ?
C26 N2 C32 C31 155.98(13) . . . . ?
C26 C25 C24 C23 179.09(16) . . . . ?
C6 C1 C2 O2 -179.71(13) . . . . ?
C6 C1 C2 C3 1.2(2) . . . . ?
C6 C5 C4 C3 0.3(3) . . . . ?
C19 N1 C15 C16 -0.1(3) . . . . ?
C19 C18 C17 C16 -0.8(3) . . . . ?
C30 C31 C32 N2 150.69(16) . . . . ?
C30 C29 C28 C27 1.3(3) . . . . ?
C25 N3 C21 C22 1.4(2) . . . . ?
C7 C6 C5 C4 -176.85(16) . . . . ?
C15 N1 C19 C20 -179.15(15) . . . . ?
C15 N1 C19 C18 -0.9(2) . . . . ?
C15 C16 C17 C18 -0.1(3) . . . . ?
C20 N2 C26 C25 76.04(16) . . . . ?
C20 N2 C32 C31 -78.48(16) . . . . ?
C20 C19 C18 C17 179.47(18) . . . . ?
C21 N3 C25 C26 179.68(14) . . . . ?
C21 N3 C25 C24 -0.7(2) . . . . ?
C32 N2 C26 C25 -158.81(13) . . . . ?
C32 N2 C20 C19 129.26(14) . . . . ?
C32 C31 C30 C29 177.16(16) . . . . ?
C11 C3 C4 C5 179.62(16) . . . . ?
C5 C6 C7 C9 -123.24(17) . . . . ?
C5 C6 C7 C8 116.33(18) . . . . ?
C5 C6 C7 C10 -3.5(2) . . . . ?
C4 C3 C11 C12 118.19(19) . . . . ?
C4 C3 C11 C13 -121.40(19) . . . . ?
C4 C3 C11 C14 -1.2(2) . . . . ?
C22 C23 C24 C25 1.0(3) . . . . ?
C24 C23 C22 C21 -0.4(3) . . . . ?
C18 C19 C20 N2 166.23(16) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-3.4188 5.0662 5.4696 0.5190 -0.4895 -0.7007
5.0699 -0.2542 -4.3632 -0.9915 0.1296 -0.0090
5.2129 -0.0814 -0.5191 -0.9830 -0.1831 -0.0090
-0.4252 -6.2188 2.8146 0.3353 0.0604 0.9402
5.0496 -1.3313 3.9064 -0.8592 -0.4681 0.2063
-4.8443 -0.1053 -3.3733 0.8783 0.4780 0.0090
-0.4373 -6.1116 -0.4664 0.2981 0.3118 0.9022
2.7633 0.4479 9.8116 -0.4296 -0.9030 -0.0091
1.8771 -3.6634 11.0187 -0.1013 -0.7858 0.6101
-1.4419 6.6613 -2.9038 -0.0011 0.0093 -1.0000
-0.3782 0.6425 12.4925 0.1831 -0.9830 -0.0091
-0.7861 -5.1097 8.3007 0.4224 -0.3976 0.8146
2.7296 -6.2693 -1.9252 -0.3075 0.2941 0.9049
-5.0962 0.3757 4.3124 0.9915 -0.1296 -0.0092
-5.2392 0.2029 0.4683 0.9830 0.1831 -0.0092
-3.5412 -3.2822 -1.6272 0.7670 0.4186 0.4863
-0.4894 -6.1943 1.2779 0.3298 0.1818 0.9264
4.8706 -0.0161 3.4241 -0.8783 -0.4780 0.0092
1.3917 4.2353 6.3261 -0.3463 -0.7308 -0.5882
-1.2809 -0.4487 -11.7780 0.1296 0.9915 -0.0091
0.3519 -0.5211 -12.5433 -0.1831 0.9830 -0.0091
1.4928 -6.4946 -1.4316 -0.0615 0.3190 0.9458
-1.1937 4.6240 8.0250 0.1442 -0.7668 -0.6255
2.1850 -1.7478 -11.3882 -0.4710 0.8648 0.1740
