#------------------------------------------------------------------------------
#$Date: 2025-07-06 17:36:42 +0300 (Sun, 06 Jul 2025) $
#$Revision: 300647 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/42/1574229.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_1574229
loop_
_publ_author_name
'Kaźmierczak, Marcin'
'Weselski, Marek'
'Siczek, Miłosz'
'Wolny, Juliusz A.'
'Schünemann, Volker'
'Bronisz, Robert'
_publ_section_title
;
 [2 + 2] Photocyclization converts thermally induced spin crossover effect
 into “hidden hysteresis” one
;
_journal_issue                   18
_journal_name_full               'Chemical Science'
_journal_page_first              7884
_journal_page_last               7893
_journal_paper_doi               10.1039/D4SC05587J
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C66 H48 Fe N24 O12, 2(B F4), 4(C2 H3 N)'
_chemical_formula_sum            'C74 H60 B2 F8 Fe N28 O12'
_chemical_formula_weight         1762.97
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-04-19
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-06-13 deposited with the CCDC.	2025-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                93.25(2)
_cell_angle_beta                 99.83(2)
_cell_angle_gamma                113.15(3)
_cell_formula_units_Z            1
_cell_length_a                   10.755(2)
_cell_length_b                   13.221(3)
_cell_length_c                   14.686(3)
_cell_measurement_reflns_used    23732
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.8620
_cell_measurement_theta_min      2.1290
_cell_volume                     1874.1(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -9.00  18.00   0.50    0.70    --   32.00 -48.00-146.07   54
  2  ω     -8.00  19.00   0.50    0.70    --   32.00 -56.00  46.87   54
  3  ω     -2.00  24.00   0.50    0.70    --   40.00 -49.00  55.90   52
  4  ω     -8.00  17.00   0.50    0.70    --   32.00 -56.00 131.58   50
  5  ω     -4.00  21.00   0.50    0.70    --   36.00 -48.00 137.94   50
  6  ω     -9.00  18.00   0.50    0.70    --   32.00 -46.00 101.29   54
  7  ω     -3.00  22.00   0.50    0.70    --   36.00 -47.00 -19.35   50
  8  ω     -8.00  18.00   0.50    0.70    --   32.00 -47.00 -61.31   52
  9  ω    -10.00  18.00   0.50    0.70    --   32.00 -45.00-175.13   56
 10  ω     18.00  43.00   0.50    0.70    --    0.05  41.00 -56.24   50
 11  ω     14.00  40.00   0.50    0.70    --    0.05  53.00-170.98   52
 12  ω     13.00  38.00   0.50    0.70    --    0.05  59.00-120.74   50
 13  ω     15.00  40.00   0.50    0.70    --    0.05  51.00 -40.57   50
 14  ω     14.00  39.00   0.50    0.70    --    0.05  58.00  20.64   50
 15  ω      0.00  26.00   0.50    0.70    --    0.05  88.00  59.41   52
 16  ω      0.00  25.00   0.50    0.70    --    0.05  88.00 -19.62   50
 17  ω      2.00  28.00   0.50    0.70    --    0.05  85.00-118.22   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0099620000
_diffrn_orient_matrix_UB_12      0.0171453000
_diffrn_orient_matrix_UB_13      0.0438203000
_diffrn_orient_matrix_UB_21      0.0443649000
_diffrn_orient_matrix_UB_22      -0.0230194000
_diffrn_orient_matrix_UB_23      0.0227457000
_diffrn_orient_matrix_UB_31      0.0575706000
_diffrn_orient_matrix_UB_32      0.0514290000
_diffrn_orient_matrix_UB_33      0.0033139000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37167
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.000
_diffrn_reflns_theta_min         2.093
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.306
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.594
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_description       plate
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.511
_exptl_crystal_size_mid          0.312
_exptl_crystal_size_min          0.072
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         12787
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0386
_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)+(0.0445P)²+0.5160P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.0977
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10640
_reflns_number_total             12787
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4sc05587j10.cif
_cod_data_source_block           206b46v_100
_cod_depositor_comments
'Adding full bibliography for 1574226--1574232.cif.'
_cod_original_cell_volume        1874.25(6)
_cod_database_code               1574229
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C74H60B2F8FeN28O12
_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   0.978
_shelx_estimated_absorpt_t_min   0.859
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C13(H13), C14(H14)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10B,H10A), C21(H21B,H21A), C32(H32B,H32A)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C11(H11), C16(H16), C17(H17), C19(H19), C22(H22),
 C24(H24), C25(H25), C27(H27), C28(H28), C30(H30), C33(H33)
2.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C36(H36C,H36B,H36A)
;
_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 1.542
_oxdiff_exptl_absorpt_empirical_full_min 0.757
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
Fe1 Fe 0.000000 1.000000 0.500000 0.01022(5) Uani 1 2 d S . P . .
O1 O 0.40539(9) 0.59648(7) -0.08975(6) 0.01984(17) Uani 1 1 d . . . . .
O2 O 0.32267(11) 0.55016(8) -0.24077(6) 0.0274(2) Uani 1 1 d . . . . .
N1 N 0.56954(10) 0.77723(8) 0.37902(7) 0.01867(19) Uani 1 1 d . . . . .
N2 N 0.64683(10) 0.75801(8) 0.32421(7) 0.01642(18) Uani 1 1 d . . . . .
N3 N 0.77840(10) 0.82487(8) 0.34717(6) 0.01595(18) Uani 1 1 d . . . . .
N4 N 0.79097(10) 0.89230(8) 0.42168(6) 0.01447(17) Uani 1 1 d . . . . .
C1 C 0.34360(13) 0.61475(10) -0.17295(8) 0.0188(2) Uani 1 1 d . . . . .
C2 C 0.30229(12) 0.71089(9) -0.17246(7) 0.0169(2) Uani 1 1 d . . . . .
H2 H 0.296330 0.735386 -0.235639 0.020 Uiso 1 1 calc R U . . .
C3 C 0.38709(12) 0.81268(9) -0.09631(7) 0.0162(2) Uani 1 1 d . . . . .
H3 H 0.444875 0.880573 -0.121080 0.019 Uiso 1 1 calc R U . . .
C4 C 0.46472(11) 0.78436(9) -0.01410(7) 0.01472(19) Uani 1 1 d . . . . .
C5 C 0.53105(12) 0.85953(9) 0.06771(8) 0.0160(2) Uani 1 1 d . . . . .
H5 H 0.545522 0.935049 0.066434 0.019 Uiso 1 1 calc R U . . .
C6 C 0.57648(12) 0.82721(9) 0.15082(8) 0.0167(2) Uani 1 1 d . . . . .
H6 H 0.620529 0.879961 0.205492 0.020 Uiso 1 1 calc R U . . .
C7 C 0.55693(11) 0.71660(9) 0.15343(8) 0.0159(2) Uani 1 1 d . . . . .
C8 C 0.50111(12) 0.64222(9) 0.07134(8) 0.0164(2) Uani 1 1 d . . . . .
H8 H 0.493107 0.568066 0.071421 0.020 Uiso 1 1 calc R U . . .
C9 C 0.45715(11) 0.67712(9) -0.01072(8) 0.0153(2) Uani 1 1 d . . . . .
C10 C 0.59021(13) 0.67228(10) 0.24287(8) 0.0208(2) Uani 1 1 d . . . . .
H10B H 0.504943 0.612036 0.252680 0.025 Uiso 1 1 calc R U . . .
H10A H 0.657905 0.640135 0.236732 0.025 Uiso 1 1 calc R U . . .
C11 C 0.66280(12) 0.86204(10) 0.43990(8) 0.0171(2) Uani 1 1 d . . . . .
H11 H 0.642328 0.897174 0.489991 0.021 Uiso 1 1 calc R U . . .
O3 O 0.14783(9) 0.61680(6) 0.01342(5) 0.01591(15) Uani 1 1 d . . . . .
O4 O 0.07447(9) 0.50477(7) -0.11922(6) 0.02072(17) Uani 1 1 d . . . . .
N5 N 0.09296(10) 0.73819(8) 0.37438(7) 0.01747(18) Uani 1 1 d . . . . .
N6 N 0.19693(9) 0.83253(8) 0.36694(6) 0.01335(17) Uani 1 1 d . . . . .
N7 N 0.19132(10) 0.92246(8) 0.40460(6) 0.01420(17) Uani 1 1 d . . . . .
N8 N 0.07766(10) 0.88756(8) 0.43907(6) 0.01409(17) Uani 1 1 d . . . . .
C12 C 0.12464(11) 0.59920(9) -0.08130(7) 0.0154(2) Uani 1 1 d . . . . .
C13 C 0.16807(12) 0.69584(9) -0.13528(7) 0.0155(2) Uani 1 1 d . . . . .
H13 H 0.090925 0.691765 -0.186260 0.019 Uiso 1 1 calc R U . . .
C14 C 0.24447(12) 0.81264(9) -0.07830(7) 0.0154(2) Uani 1 1 d . . . . .
H14 H 0.220724 0.869315 -0.110533 0.018 Uiso 1 1 calc R U . . .
C15 C 0.23181(11) 0.81891(9) 0.02133(7) 0.01450(19) Uani 1 1 d . . . . .
C16 C 0.27359(12) 0.91955(9) 0.07830(8) 0.0166(2) Uani 1 1 d . . . . .
H16 H 0.288262 0.985442 0.050654 0.020 Uiso 1 1 calc R U . . .
C17 C 0.29414(12) 0.92500(9) 0.17504(8) 0.0167(2) Uani 1 1 d . . . . .
H17 H 0.324069 0.994376 0.212862 0.020 Uiso 1 1 calc R U . . .
C18 C 0.27074(11) 0.82853(9) 0.21630(7) 0.01457(19) Uani 1 1 d . . . . .
C19 C 0.21756(11) 0.72614(9) 0.16024(7) 0.01436(19) Uani 1 1 d . . . . .
H19 H 0.195038 0.659358 0.187425 0.017 Uiso 1 1 calc R U . . .
C20 C 0.19797(11) 0.72323(9) 0.06384(7) 0.01361(19) Uani 1 1 d . . . . .
C21 C 0.30915(11) 0.83567(10) 0.32113(7) 0.0154(2) Uani 1 1 d . . . . .
H21B H 0.333815 0.773057 0.336500 0.018 Uiso 1 1 calc R U . . .
H21A H 0.391674 0.905520 0.345866 0.018 Uiso 1 1 calc R U . . .
C22 C 0.02029(12) 0.77557(9) 0.42033(8) 0.0169(2) Uani 1 1 d . . . . .
H22 H -0.062362 0.729132 0.438004 0.020 Uiso 1 1 calc R U . . .
O5 O -0.13788(10) 0.91953(7) 1.03287(6) 0.02170(18) Uani 1 1 d . . . . .
O6 O -0.07297(11) 1.02496(8) 1.16887(7) 0.0303(2) Uani 1 1 d . . . . .
N9 N -0.04057(10) 0.76256(8) 0.69673(7) 0.01711(18) Uani 1 1 d . . . . .
N10 N -0.15757(10) 0.77730(8) 0.68539(6) 0.01404(17) Uani 1 1 d . . . . .
N11 N -0.16081(10) 0.85484(8) 0.63463(6) 0.01450(17) Uani 1 1 d . . . . .
N12 N -0.03880(10) 0.89526(8) 0.61047(6) 0.01418(17) Uani 1 1 d . . . . .
C23 C -0.09015(13) 0.93696(11) 1.12850(8) 0.0212(2) Uani 1 1 d . . . . .
C24 C -0.06698(13) 0.84746(11) 1.17082(8) 0.0219(2) Uani 1 1 d . . . . .
H24 H -0.030533 0.858084 1.235982 0.026 Uiso 1 1 calc R U . . .
C25 C -0.09565(13) 0.75030(11) 1.12038(8) 0.0212(2) Uani 1 1 d . . . . .
H25 H -0.082018 0.692443 1.150191 0.025 Uiso 1 1 calc R U . . .
C26 C -0.14727(12) 0.73344(10) 1.02073(8) 0.0175(2) Uani 1 1 d . . . . .
C27 C -0.17757(14) 0.63549(10) 0.96278(8) 0.0217(2) Uani 1 1 d . . . . .
H27 H -0.167947 0.574304 0.989138 0.026 Uiso 1 1 calc R U . . .
C28 C -0.22146(13) 0.62703(10) 0.86731(8) 0.0201(2) Uani 1 1 d . . . . .
H28 H -0.241331 0.560321 0.828450 0.024 Uiso 1 1 calc R U . . .
C29 C -0.23667(12) 0.71660(9) 0.82785(8) 0.0159(2) Uani 1 1 d . . . . .
C30 C -0.20981(12) 0.81376(10) 0.88440(8) 0.0178(2) Uani 1 1 d . . . . .
H30 H -0.221820 0.874216 0.858214 0.021 Uiso 1 1 calc R U . . .
C31 C -0.16499(12) 0.82085(10) 0.98007(8) 0.0165(2) Uani 1 1 d . . . . .
C32 C -0.27723(12) 0.70982(9) 0.72337(7) 0.0163(2) Uani 1 1 d . . . . .
H32B H -0.313828 0.631531 0.694389 0.020 Uiso 1 1 calc R U . . .
H32A H -0.351267 0.736628 0.707986 0.020 Uiso 1 1 calc R U . . .
C33 C 0.03261(12) 0.83859(10) 0.64945(8) 0.0163(2) Uani 1 1 d . . . . .
H33 H 0.124130 0.851700 0.643627 0.020 Uiso 1 1 calc R U . . .
B1 B 0.39515(14) 0.85945(12) 0.62731(10) 0.0202(2) Uani 1 1 d . . . . .
F1 F 0.48849(8) 0.82769(7) 0.68361(6) 0.02699(17) Uani 1 1 d . . . . .
F2 F 0.26588(8) 0.76912(6) 0.60361(6) 0.02640(16) Uani 1 1 d . . . . .
F3 F 0.44172(11) 0.89228(11) 0.54816(7) 0.0540(3) Uani 1 1 d . . . . .
F4 F 0.38045(9) 0.94471(7) 0.67764(8) 0.0435(2) Uani 1 1 d . . . . .
N13 N 0.22925(14) 0.53626(10) 0.31898(9) 0.0309(3) Uani 1 1 d . . . . .
C34 C -0.00995(17) 0.47735(12) 0.36440(11) 0.0331(3) Uani 1 1 d . . . . .
H34A H -0.075357 0.487584 0.314494 0.050 Uiso 1 1 calc R U . . .
H34B H 0.000147 0.523296 0.422237 0.050 Uiso 1 1 calc R U . . .
H34C H -0.044696 0.399081 0.373952 0.050 Uiso 1 1 calc R U . . .
C35 C 0.12393(16) 0.51016(11) 0.33843(9) 0.0262(3) Uani 1 1 d . . . . .
N14 N 0.27351(14) 0.38093(10) 0.51676(9) 0.0320(3) Uani 1 1 d . . . . .
C36 C 0.39030(16) 0.59647(12) 0.54376(10) 0.0307(3) Uani 1 1 d . . . . .
H36C H 0.329745 0.625765 0.507545 0.046 Uiso 1 1 calc R U . . .
H36B H 0.478771 0.622046 0.523710 0.046 Uiso 1 1 calc R U . . .
H36A H 0.406474 0.622932 0.610205 0.046 Uiso 1 1 calc R U . . .
C37 C 0.32479(13) 0.47558(11) 0.52862(9) 0.0232(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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 17 -2 0.2075
1 -18 2 0.2071
-14 2 2 0.1504
14 -2 -2 0.1496
0 0 -20 0.0384
0 -1 20 0.0295
0 0 1 0.0294
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
N4 Fe1 N4 180.0 1_455 2_676 ?
N8 Fe1 N4 89.12(4) 2_576 2_676 ?
N8 Fe1 N4 89.12(4) . 1_455 ?
N8 Fe1 N4 90.88(4) . 2_676 ?
N8 Fe1 N4 90.88(4) 2_576 1_455 ?
N8 Fe1 N8 180.0 . 2_576 ?
N12 Fe1 N4 87.99(4) 2_576 2_676 ?
N12 Fe1 N4 87.99(4) . 1_455 ?
N12 Fe1 N4 92.01(3) 2_576 1_455 ?
N12 Fe1 N4 92.01(3) . 2_676 ?
N12 Fe1 N8 87.11(3) . . ?
N12 Fe1 N8 92.89(3) . 2_576 ?
N12 Fe1 N8 87.11(3) 2_576 2_576 ?
N12 Fe1 N8 92.89(3) 2_576 . ?
N12 Fe1 N12 180.0 . 2_576 ?
C1 O1 C9 121.36(9) . . ?
C11 N1 N2 101.82(9) . . ?
N1 N2 C10 123.31(10) . . ?
N3 N2 N1 114.52(9) . . ?
N3 N2 C10 122.13(10) . . ?
N2 N3 N4 105.42(9) . . ?
N3 N4 Fe1 118.23(7) . 1_655 ?
N3 N4 C11 106.73(9) . . ?
C11 N4 Fe1 133.92(7) . 1_655 ?
O1 C1 C2 117.93(10) . . ?
O2 C1 O1 117.20(11) . . ?
O2 C1 C2 124.83(11) . . ?
C1 C2 H2 110.2 . . ?
C1 C2 C3 118.02(10) . . ?
C1 C2 C13 117.25(9) . . ?
C3 C2 H2 110.2 . . ?
C3 C2 C13 89.47(8) . . ?
C13 C2 H2 110.2 . . ?
C2 C3 H3 113.8 . . ?
C2 C3 C14 88.60(8) . . ?
C4 C3 C2 112.33(9) . . ?
C4 C3 H3 113.8 . . ?
C4 C3 C14 112.10(9) . . ?
C14 C3 H3 113.8 . . ?
C5 C4 C3 121.40(10) . . ?
C9 C4 C3 121.29(10) . . ?
C9 C4 C5 116.67(10) . . ?
C4 C5 H5 119.0 . . ?
C6 C5 C4 122.04(10) . . ?
C6 C5 H5 119.0 . . ?
C5 C6 H6 120.2 . . ?
C5 C6 C7 119.55(10) . . ?
C7 C6 H6 120.2 . . ?
C6 C7 C10 122.79(10) . . ?
C8 C7 C6 119.42(11) . . ?
C8 C7 C10 117.77(10) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 C7 119.55(10) . . ?
C9 C8 H8 120.2 . . ?
C4 C9 O1 122.66(10) . . ?
C8 C9 O1 114.97(10) . . ?
C8 C9 C4 122.37(10) . . ?
N2 C10 C7 112.58(9) . . ?
N2 C10 H10B 109.1 . . ?
N2 C10 H10A 109.1 . . ?
C7 C10 H10B 109.1 . . ?
C7 C10 H10A 109.1 . . ?
H10B C10 H10A 107.8 . . ?
N1 C11 N4 111.51(10) . . ?
N1 C11 H11 124.2 . . ?
N4 C11 H11 124.2 . . ?
C12 O3 C20 122.46(9) . . ?
C22 N5 N6 101.53(9) . . ?
N5 N6 C21 122.94(9) . . ?
N7 N6 N5 114.46(9) . . ?
N7 N6 C21 122.60(9) . . ?
N6 N7 N8 105.58(9) . . ?
N7 N8 Fe1 123.25(7) . . ?
N7 N8 C22 106.40(9) . . ?
C22 N8 Fe1 130.08(8) . . ?
O3 C12 C13 120.12(9) . . ?
O4 C12 O3 118.06(10) . . ?
O4 C12 C13 121.73(10) . . ?
C2 C13 H13 112.0 . . ?
C12 C13 C2 112.07(9) . . ?
C12 C13 H13 112.0 . . ?
C12 C13 C14 116.99(9) . . ?
C14 C13 C2 89.89(8) . . ?
C14 C13 H13 112.0 . . ?
C3 C14 H14 111.8 . . ?
C13 C14 C3 88.83(8) . . ?
C13 C14 H14 111.8 . . ?
C15 C14 C3 115.64(9) . . ?
C15 C14 C13 115.13(9) . . ?
C15 C14 H14 111.8 . . ?
C16 C15 C14 122.60(10) . . ?
C20 C15 C14 119.14(10) . . ?
C20 C15 C16 117.47(10) . . ?
C15 C16 H16 119.5 . . ?
C17 C16 C15 121.10(10) . . ?
C17 C16 H16 119.5 . . ?
C16 C17 H17 120.0 . . ?
C16 C17 C18 119.94(10) . . ?
C18 C17 H17 120.0 . . ?
C17 C18 C21 120.07(10) . . ?
C19 C18 C17 119.67(10) . . ?
C19 C18 C21 120.20(10) . . ?
C18 C19 H19 120.5 . . ?
C20 C19 C18 118.97(10) . . ?
C20 C19 H19 120.5 . . ?
C15 C20 O3 122.72(9) . . ?
C15 C20 C19 122.37(10) . . ?
C19 C20 O3 114.84(9) . . ?
N6 C21 C18 112.67(9) . . ?
N6 C21 H21B 109.1 . . ?
N6 C21 H21A 109.1 . . ?
C18 C21 H21B 109.1 . . ?
C18 C21 H21A 109.1 . . ?
H21B C21 H21A 107.8 . . ?
N5 C22 N8 112.02(10) . . ?
N5 C22 H22 124.0 . . ?
N8 C22 H22 124.0 . . ?
C31 O5 C23 121.58(10) . . ?
C33 N9 N10 101.50(9) . . ?
N9 N10 C32 123.42(9) . . ?
N11 N10 N9 114.90(9) . . ?
N11 N10 C32 121.64(9) . . ?
N10 N11 N12 105.12(9) . . ?
N11 N12 Fe1 121.83(7) . . ?
N11 N12 C33 106.68(9) . . ?
C33 N12 Fe1 129.66(7) . . ?
O5 C23 C24 117.12(11) . . ?
O6 C23 O5 116.62(12) . . ?
O6 C23 C24 126.25(11) . . ?
C23 C24 H24 119.1 . . ?
C25 C24 C23 121.76(11) . . ?
C25 C24 H24 119.1 . . ?
C24 C25 H25 120.0 . . ?
C24 C25 C26 120.10(11) . . ?
C26 C25 H25 120.0 . . ?
C27 C26 C25 123.79(11) . . ?
C31 C26 C25 117.88(11) . . ?
C31 C26 C27 118.32(10) . . ?
C26 C27 H27 119.8 . . ?
C28 C27 C26 120.49(11) . . ?
C28 C27 H27 119.8 . . ?
C27 C28 H28 119.9 . . ?
C27 C28 C29 120.17(11) . . ?
C29 C28 H28 119.9 . . ?
C28 C29 C32 120.27(10) . . ?
C30 C29 C28 120.21(10) . . ?
C30 C29 C32 119.48(10) . . ?
C29 C30 H30 120.6 . . ?
C29 C30 C31 118.73(10) . . ?
C31 C30 H30 120.6 . . ?
O5 C31 C26 121.51(10) . . ?
O5 C31 C30 116.43(10) . . ?
C30 C31 C26 122.06(11) . . ?
N10 C32 C29 110.66(9) . . ?
N10 C32 H32B 109.5 . . ?
N10 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
C29 C32 H32A 109.5 . . ?
H32B C32 H32A 108.1 . . ?
N9 C33 N12 111.80(10) . . ?
N9 C33 H33 124.1 . . ?
N12 C33 H33 124.1 . . ?
F1 B1 F2 108.96(10) . . ?
F3 B1 F1 109.79(11) . . ?
F3 B1 F2 109.93(12) . . ?
F3 B1 F4 111.04(12) . . ?
F4 B1 F1 108.98(11) . . ?
F4 B1 F2 108.08(10) . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C35 C34 H34A 109.5 . . ?
C35 C34 H34B 109.5 . . ?
C35 C34 H34C 109.5 . . ?
N13 C35 C34 179.34(16) . . ?
H36C C36 H36B 109.5 . . ?
H36C C36 H36A 109.5 . . ?
H36B C36 H36A 109.5 . . ?
C37 C36 H36C 109.5 . . ?
C37 C36 H36B 109.5 . . ?
C37 C36 H36A 109.5 . . ?
N14 C37 C36 179.99(19) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N4 2.1953(9) 1_455 ?
Fe1 N4 2.1953(9) 2_676 ?
Fe1 N8 2.1883(9) . ?
Fe1 N8 2.1883(9) 2_576 ?
Fe1 N12 2.1807(9) . ?
Fe1 N12 2.1807(9) 2_576 ?
O1 C1 1.3694(14) . ?
O1 C9 1.4022(13) . ?
O2 C1 1.2032(14) . ?
N1 N2 1.3322(14) . ?
N1 C11 1.3261(15) . ?
N2 N3 1.3106(13) . ?
N2 C10 1.4622(15) . ?
N3 N4 1.3246(13) . ?
N4 C11 1.3552(14) . ?
C1 C2 1.5024(16) . ?
C2 H2 1.0000 . ?
C2 C3 1.5523(15) . ?
C2 C13 1.5739(16) . ?
C3 H3 1.0000 . ?
C3 C4 1.4992(16) . ?
C3 C14 1.6002(16) . ?
C4 C5 1.3981(15) . ?
C4 C9 1.3921(16) . ?
C5 H5 0.9500 . ?
C5 C6 1.3894(16) . ?
C6 H6 0.9500 . ?
C6 C7 1.3970(16) . ?
C7 C8 1.3911(15) . ?
C7 C10 1.5126(16) . ?
C8 H8 0.9500 . ?
C8 C9 1.3887(16) . ?
C10 H10B 0.9900 . ?
C10 H10A 0.9900 . ?
C11 H11 0.9500 . ?
O3 C12 1.3603(13) . ?
O3 C20 1.4029(13) . ?
O4 C12 1.2038(14) . ?
N5 N6 1.3338(13) . ?
N5 C22 1.3253(14) . ?
N6 N7 1.3101(12) . ?
N6 C21 1.4670(13) . ?
N7 N8 1.3258(13) . ?
N8 C22 1.3515(14) . ?
C12 C13 1.5005(15) . ?
C13 H13 1.0000 . ?
C13 C14 1.5432(15) . ?
C14 H14 1.0000 . ?
C14 C15 1.4932(15) . ?
C15 C16 1.3956(15) . ?
C15 C20 1.3884(15) . ?
C16 H16 0.9500 . ?
C16 C17 1.3932(15) . ?
C17 H17 0.9500 . ?
C17 C18 1.3945(16) . ?
C18 C19 1.3934(15) . ?
C18 C21 1.5118(15) . ?
C19 H19 0.9500 . ?
C19 C20 1.3912(14) . ?
C21 H21B 0.9900 . ?
C21 H21A 0.9900 . ?
C22 H22 0.9500 . ?
O5 C23 1.3831(14) . ?
O5 C31 1.3775(14) . ?
O6 C23 1.2060(16) . ?
N9 N10 1.3319(13) . ?
N9 C33 1.3251(15) . ?
N10 N11 1.3091(13) . ?
N10 C32 1.4704(14) . ?
N11 N12 1.3277(13) . ?
N12 C33 1.3526(14) . ?
C23 C24 1.4528(18) . ?
C24 H24 0.9500 . ?
C24 C25 1.3404(18) . ?
C25 H25 0.9500 . ?
C25 C26 1.4449(16) . ?
C26 C27 1.3986(17) . ?
C26 C31 1.3932(16) . ?
C27 H27 0.9500 . ?
C27 C28 1.3840(16) . ?
C28 H28 0.9500 . ?
C28 C29 1.4009(16) . ?
C29 C30 1.3887(16) . ?
C29 C32 1.5092(15) . ?
C30 H30 0.9500 . ?
C30 C31 1.3906(15) . ?
C32 H32B 0.9900 . ?
C32 H32A 0.9900 . ?
C33 H33 0.9500 . ?
B1 F1 1.3982(16) . ?
B1 F2 1.4011(16) . ?
B1 F3 1.3695(16) . ?
B1 F4 1.3882(17) . ?
N13 C35 1.139(2) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C34 C35 1.457(2) . ?
N14 C37 1.1404(18) . ?
C36 H36C 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36A 0.9800 . ?
C36 C37 1.4565(19) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N4 C11 N1 -167.10(8) 1_655 . . . ?
Fe1 N8 C22 N5 173.49(7) . . . . ?
Fe1 N12 C33 N9 -163.78(8) . . . . ?
O1 C1 C2 C3 28.64(15) . . . . ?
O1 C1 C2 C13 -76.56(13) . . . . ?
O2 C1 C2 C3 -153.74(12) . . . . ?
O2 C1 C2 C13 101.06(14) . . . . ?
N1 N2 N3 N4 0.44(13) . . . . ?
N1 N2 C10 C7 93.82(13) . . . . ?
N2 N1 C11 N4 0.17(13) . . . . ?
N2 N3 N4 Fe1 169.25(7) . . . 1_655 ?
N2 N3 N4 C11 -0.30(12) . . . . ?
N3 N2 C10 C7 -83.90(13) . . . . ?
N3 N4 C11 N1 0.08(13) . . . . ?
C1 O1 C9 C4 -8.05(16) . . . . ?
C1 O1 C9 C8 172.26(10) . . . . ?
C1 C2 C3 C4 -20.83(14) . . . . ?
C1 C2 C3 C14 -134.21(10) . . . . ?
C1 C2 C13 C12 16.11(13) . . . . ?
C1 C2 C13 C14 135.37(10) . . . . ?
C2 C3 C4 C5 -170.58(10) . . . . ?
C2 C3 C4 C9 -0.04(15) . . . . ?
C2 C3 C14 C13 13.57(8) . . . . ?
C2 C3 C14 C15 131.05(10) . . . . ?
C2 C13 C14 C3 -13.37(8) . . . . ?
C2 C13 C14 C15 -131.31(10) . . . . ?
C3 C2 C13 C12 -105.47(9) . . . . ?
C3 C2 C13 C14 13.79(8) . . . . ?
C3 C4 C5 C6 165.36(11) . . . . ?
C3 C4 C9 O1 15.21(16) . . . . ?
C3 C4 C9 C8 -165.12(11) . . . . ?
C3 C14 C15 C16 89.72(13) . . . . ?
C3 C14 C15 C20 -79.86(13) . . . . ?
C4 C3 C14 C13 -100.03(9) . . . . ?
C4 C3 C14 C15 17.45(13) . . . . ?
C4 C5 C6 C7 0.56(17) . . . . ?
C5 C4 C9 O1 -173.82(10) . . . . ?
C5 C4 C9 C8 5.85(16) . . . . ?
C5 C6 C7 C8 4.49(17) . . . . ?
C5 C6 C7 C10 -173.71(11) . . . . ?
C6 C7 C8 C9 -4.27(17) . . . . ?
C6 C7 C10 N2 -1.18(17) . . . . ?
C7 C8 C9 O1 178.66(10) . . . . ?
C7 C8 C9 C4 -1.03(17) . . . . ?
C8 C7 C10 N2 -179.41(10) . . . . ?
C9 O1 C1 O2 168.03(11) . . . . ?
C9 O1 C1 C2 -14.16(16) . . . . ?
C9 C4 C5 C6 -5.60(16) . . . . ?
C10 N2 N3 N4 178.34(10) . . . . ?
C10 C7 C8 C9 174.02(11) . . . . ?
C11 N1 N2 N3 -0.38(13) . . . . ?
C11 N1 N2 C10 -178.25(10) . . . . ?
O3 C12 C13 C2 104.48(11) . . . . ?
O3 C12 C13 C14 2.70(15) . . . . ?
O4 C12 C13 C2 -72.21(14) . . . . ?
O4 C12 C13 C14 -173.99(11) . . . . ?
N5 N6 N7 N8 -0.23(12) . . . . ?
N5 N6 C21 C18 82.81(13) . . . . ?
N6 N5 C22 N8 0.42(12) . . . . ?
N6 N7 N8 Fe1 -174.11(7) . . . . ?
N6 N7 N8 C22 0.46(11) . . . . ?
N7 N6 C21 C18 -97.73(12) . . . . ?
N7 N8 C22 N5 -0.58(13) . . . . ?
C12 O3 C20 C15 -2.06(16) . . . . ?
C12 O3 C20 C19 -179.11(10) . . . . ?
C12 C13 C14 C3 101.50(10) . . . . ?
C12 C13 C14 C15 -16.44(14) . . . . ?
C13 C2 C3 C4 100.09(10) . . . . ?
C13 C2 C3 C14 -13.30(8) . . . . ?
C13 C14 C15 C16 -168.72(10) . . . . ?
C13 C14 C15 C20 21.69(15) . . . . ?
C14 C3 C4 C5 -72.63(13) . . . . ?
C14 C3 C4 C9 97.91(12) . . . . ?
C14 C15 C16 C17 -163.32(11) . . . . ?
C14 C15 C20 O3 -13.26(16) . . . . ?
C14 C15 C20 C19 163.57(10) . . . . ?
C15 C16 C17 C18 -1.04(17) . . . . ?
C16 C15 C20 O3 176.62(10) . . . . ?
C16 C15 C20 C19 -6.54(16) . . . . ?
C16 C17 C18 C19 -4.52(16) . . . . ?
C16 C17 C18 C21 172.65(10) . . . . ?
C17 C18 C19 C20 4.45(16) . . . . ?
C17 C18 C21 N6 88.74(12) . . . . ?
C18 C19 C20 O3 178.24(9) . . . . ?
C18 C19 C20 C15 1.18(16) . . . . ?
C19 C18 C21 N6 -94.11(12) . . . . ?
C20 O3 C12 O4 -176.03(10) . . . . ?
C20 O3 C12 C13 7.16(15) . . . . ?
C20 C15 C16 C17 6.43(16) . . . . ?
C21 N6 N7 N8 -179.72(9) . . . . ?
C21 C18 C19 C20 -172.71(10) . . . . ?
C22 N5 N6 N7 -0.11(12) . . . . ?
C22 N5 N6 C21 179.38(10) . . . . ?
O5 C23 C24 C25 -2.62(18) . . . . ?
O6 C23 C24 C25 176.65(13) . . . . ?
N9 N10 N11 N12 -0.24(12) . . . . ?
N9 N10 C32 C29 57.62(13) . . . . ?
N10 N9 C33 N12 -0.81(12) . . . . ?
N10 N11 N12 Fe1 165.70(7) . . . . ?
N10 N11 N12 C33 -0.28(11) . . . . ?
N11 N10 C32 C29 -124.73(11) . . . . ?
N11 N12 C33 N9 0.72(13) . . . . ?
C23 O5 C31 C26 0.84(17) . . . . ?
C23 O5 C31 C30 -178.71(11) . . . . ?
C23 C24 C25 C26 1.85(19) . . . . ?
C24 C25 C26 C27 178.91(12) . . . . ?
C24 C25 C26 C31 0.29(17) . . . . ?
C25 C26 C27 C28 -177.40(12) . . . . ?
C25 C26 C31 O5 -1.65(17) . . . . ?
C25 C26 C31 C30 177.87(11) . . . . ?
C26 C27 C28 C29 -0.34(19) . . . . ?
C27 C26 C31 O5 179.66(11) . . . . ?
C27 C26 C31 C30 -0.82(18) . . . . ?
C27 C28 C29 C30 -0.97(18) . . . . ?
C27 C28 C29 C32 176.77(11) . . . . ?
C28 C29 C30 C31 1.35(17) . . . . ?
C28 C29 C32 N10 -105.32(12) . . . . ?
C29 C30 C31 O5 179.09(10) . . . . ?
C29 C30 C31 C26 -0.46(18) . . . . ?
C30 C29 C32 N10 72.44(13) . . . . ?
C31 O5 C23 O6 -178.09(11) . . . . ?
C31 O5 C23 C24 1.25(17) . . . . ?
C31 C26 C27 C28 1.22(18) . . . . ?
C32 N10 N11 N12 -178.08(9) . . . . ?
C32 C29 C30 C31 -176.40(10) . . . . ?
C33 N9 N10 N11 0.65(12) . . . . ?
C33 N9 N10 C32 178.44(10) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.7147 17.4633 -2.2634 0.2073 -0.4852 0.8495
0.8547 -17.5230 2.2501 -0.2104 0.4925 -0.8445
-14.4181 2.0081 1.9370 0.2629 -0.6418 -0.7204
14.3364 -1.6735 -1.9700 -0.2578 0.6297 0.7328
-0.2742 0.2886 -20.1663 -0.8760 -0.4775 -0.0678
-0.1532 -0.9651 20.3755 0.8778 0.4789 0.0091
-0.0085 -0.0007 0.9964 0.0437 0.0223 0.0028
