#------------------------------------------------------------------------------
#$Date: 2022-02-19 01:15:19 +0200 (Sat, 19 Feb 2022) $
#$Revision: 273036 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/64/1566401.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_1566401
loop_
_publ_author_name
'Birchall, Lee'
'Truccolo, Giada'
'Jackson, Lewis'
'Shepherd, Helena Jane'
_publ_section_title
;
 Co-crystallisation as a Modular Approach to the Discovery of
 Spin-Crossover Materials
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC04956A
_journal_year                    2022
_chemical_formula_moiety         'C22 H18 Fe N10, 2(B F4), 2(C10 H8 N2)'
_chemical_formula_sum            'C42 H34 B2 F8 Fe N14'
_chemical_formula_weight         964.30
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-11 deposited with the CCDC.	2022-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                96.262(2)
_cell_angle_beta                 96.200(2)
_cell_angle_gamma                93.852(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0861(3)
_cell_length_b                   10.1542(3)
_cell_length_c                   21.8490(6)
_cell_measurement_reflns_used    11541
_cell_measurement_temperature    249.99(15)
_cell_measurement_theta_max      71.7960
_cell_measurement_theta_min      4.4080
_cell_volume                     2204.26(11)
_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 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      249.99(15)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -67.00  32.00   1.00    3.00    --  -42.16  38.00 150.00   99
  2  ω    -70.00  31.00   1.00    3.00    --  -42.16  57.00 -90.00  101
  3  ω   -116.00 -18.00   1.00    3.00    --  -42.16 -38.00 -30.00   98
  4  ω     23.00  98.00   1.00    3.00    --   42.16-125.00 -60.00   75
  5  ω     94.00 177.00   1.00   12.00    --  103.72 125.00-180.00   83
  6  ω     75.00 178.00   1.00   12.00    --  103.72  30.00 -90.00  103
  7  ω     27.00 132.00   1.00   12.00    --  103.72 -30.00  90.00  105
  8  ω     21.00 109.00   1.00   12.00    --  103.72 -94.00 -30.00   88
  9  ω     94.00 177.00   1.00   12.00    --  103.72 125.00 120.00   83
 10  ω     94.00 177.00   1.00   12.00    --  103.72 125.00 -90.00   83
 11  ω     21.00 109.00   1.00   12.00    --  103.72 -94.00-150.00   88
 12  ω     94.00 177.00   1.00   12.00    --  103.72 125.00 150.00   83
 13  ω     31.00 118.00   1.00   12.00    --  103.72-125.00 -60.00   87
 14  ω     31.00 130.00   1.00   12.00    --  103.72 -45.00-150.00   99
 15  ω     31.00 118.00   1.00   12.00    --  103.72-125.00 150.00   87
 16  ω    125.00 161.00   1.00   12.00    --  103.72  45.00 -60.00   36
 17  ω     25.00  52.00   1.00   12.00    --  103.72 -94.00  90.00   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      -0.0002359000
_diffrn_orient_matrix_UB_12      -0.1154478000
_diffrn_orient_matrix_UB_13      0.0402658000
_diffrn_orient_matrix_UB_21      0.0321778000
_diffrn_orient_matrix_UB_22      0.1001723000
_diffrn_orient_matrix_UB_23      0.0588475000
_diffrn_orient_matrix_UB_31      -0.1507363000
_diffrn_orient_matrix_UB_32      0.0090541000
_diffrn_orient_matrix_UB_33      0.0040071000
_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  0.0219
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20325
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.988
_diffrn_reflns_theta_min         4.099
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.474
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.423
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.369
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.095
_refine_diff_density_max         3.404
_refine_diff_density_min         -0.947
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         8465
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0717
_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)+(0.1580P)²+1.4877P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2196
_refine_ls_wR_factor_ref         0.2237
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8029
_reflns_number_total             8465
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1sc04956a1.cif
_cod_data_source_block           ltb-19-003_a_250_red_ref
_cod_database_code               1566401
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Fe C42 H34 N14 B2 F8'
_chemical_oxdiff_usercomment     '250 K'
_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.
;
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N5(H5), N6(H6), N1(H1), N10(H10), C18(H18), C17(H17), C16(H16), C7(H7),
 C10(H10a), C13(H13), C5(H5a), C11(H11), C6(H6a), C12(H12), C2(H2), C29(H29),
 C36(H36), C26(H26), C31(H31), C30(H30), C35(H35), C39(H39), C21(H21), C1(H1a),
 C32(H32), C41(H41), C25(H25), C24(H24), C40(H40), C22(H22), C34(H34), C33(H33),
  C23(H23), C42(H42)
;
_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 1.118
_oxdiff_exptl_absorpt_empirical_full_min 0.882
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 0.23274(4) 0.17691(4) 0.75850(2) 0.03179(18) Uani 1 1 d . . . . .
F5 F 0.7022(3) 0.7655(3) 0.91167(12) 0.0684(7) Uani 1 1 d . . . . .
N3 N 0.1840(3) 0.2533(3) 0.83728(12) 0.0353(5) Uani 1 1 d . . . . .
N8 N 0.2837(3) 0.0907(3) 0.68188(12) 0.0350(5) Uani 1 1 d . . . . .
N4 N 0.3529(3) 0.0890(3) 0.81769(13) 0.0393(6) Uani 1 1 d . . . . .
N7 N 0.1022(3) 0.0171(3) 0.74271(13) 0.0383(6) Uani 1 1 d . . . . .
N2 N 0.0968(3) 0.2982(3) 0.73062(13) 0.0392(6) Uani 1 1 d . . . . .
F8 F 0.7323(4) 0.7024(4) 0.81350(13) 0.0902(10) Uani 1 1 d . . . . .
F7 F 0.7395(4) 0.5531(3) 0.8825(2) 0.0949(11) Uani 1 1 d . . . . .
N9 N 0.3813(3) 0.3032(3) 0.74363(13) 0.0404(6) Uani 1 1 d . . . . .
N5 N 0.4459(3) 0.0007(3) 0.81565(15) 0.0451(7) Uani 1 1 d . . . . .
H5 H 0.4746 -0.0332 0.7822 0.054 Uiso 1 1 calc R U . . .
N6 N 0.0043(3) -0.0396(3) 0.77102(15) 0.0475(7) Uani 1 1 d . . . . .
H6 H -0.0255 -0.0039 0.8038 0.057 Uiso 1 1 calc R U . . .
N1 N 0.0394(3) 0.3334(4) 0.67716(14) 0.0492(7) Uani 1 1 d . . . . .
H1 H 0.0576 0.3030 0.6410 0.059 Uiso 1 1 calc R U . . .
N10 N 0.4474(3) 0.4165(3) 0.77136(16) 0.0509(7) Uani 1 1 d . . . . .
H10 H 0.4289 0.4590 0.8052 0.061 Uiso 1 1 calc R U . . .
C15 C 0.2206(3) -0.0275(3) 0.65652(15) 0.0384(7) Uani 1 1 d . . . . .
F6 F 0.9053(3) 0.7152(4) 0.8880(2) 0.1113(14) Uani 1 1 d . . . . .
N12 N 0.8668(4) 0.7326(4) 0.43741(15) 0.0561(8) Uani 1 1 d . . . . .
C4 C 0.0905(3) 0.3433(3) 0.83854(15) 0.0385(7) Uani 1 1 d . . . . .
C9 C 0.3373(3) 0.1175(3) 0.87785(15) 0.0399(7) Uani 1 1 d . . . . .
C3 C 0.0413(3) 0.3672(3) 0.77632(16) 0.0401(7) Uani 1 1 d . . . . .
C20 C 0.4413(3) 0.2700(4) 0.69232(16) 0.0422(7) Uani 1 1 d . . . . .
C8 C 0.2404(3) 0.2152(3) 0.89034(15) 0.0390(7) Uani 1 1 d . . . . .
C14 C 0.1183(3) -0.0701(3) 0.69381(16) 0.0403(7) Uani 1 1 d . . . . .
C19 C 0.3845(3) 0.1469(3) 0.65541(15) 0.0377(7) Uani 1 1 d . . . . .
N13 N 0.8648(4) 0.0847(4) 0.8655(2) 0.0690(11) Uani 1 1 d . . . . .
N11 N 0.5791(4) 0.9189(4) 0.71304(18) 0.0682(11) Uani 1 1 d . . . . .
N14 N 0.6293(4) 0.4141(4) 1.1293(2) 0.0707(11) Uani 1 1 d . . . . .
C18 C 0.4227(4) 0.0887(4) 0.60045(16) 0.0442(7) Uani 1 1 d . . . . .
H18 H 0.4909 0.1290 0.5819 0.053 Uiso 1 1 calc R U . . .
F3 F 0.7227(6) 0.2384(4) 0.5577(2) 0.1319(18) Uani 1 1 d . . . . .
C17 C 0.3562(4) -0.0319(4) 0.57364(17) 0.0479(8) Uani 1 1 d . . . . .
H17 H 0.3796 -0.0729 0.5366 0.057 Uiso 1 1 calc R U . . .
C28 C 0.7592(4) 0.8008(4) 0.54841(17) 0.0463(8) Uani 1 1 d . . . . .
C38 C 0.7123(4) 0.2729(4) 1.0252(2) 0.0503(9) Uani 1 1 d . . . . .
C16 C 0.2552(4) -0.0910(4) 0.60214(17) 0.0473(8) Uani 1 1 d . . . . .
H16 H 0.2114 -0.1722 0.5848 0.057 Uiso 1 1 calc R U . . .
F1 F 0.6998(9) 0.4549(4) 0.57569(18) 0.172(3) Uani 1 1 d . . . . .
C37 C 0.7606(4) 0.2047(4) 0.9696(2) 0.0511(9) Uani 1 1 d . . . . .
C7 C 0.2078(4) 0.2674(4) 0.94733(16) 0.0495(8) Uani 1 1 d . . . . .
H7 H 0.2478 0.2405 0.9838 0.059 Uiso 1 1 calc R U . . .
C10 C 0.4206(4) 0.0457(4) 0.91454(19) 0.0515(9) Uani 1 1 d . . . . .
H10A H 0.4290 0.0467 0.9574 0.062 Uiso 1 1 calc R U . . .
C13 C 0.0303(4) -0.1835(4) 0.6914(2) 0.0542(9) Uani 1 1 d . . . . .
H13 H 0.0216 -0.2588 0.6626 0.065 Uiso 1 1 calc R U . . .
C27 C 0.6991(4) 0.8400(4) 0.60648(17) 0.0495(8) Uani 1 1 d . . . . .
C5 C 0.0539(4) 0.3997(4) 0.89436(17) 0.0478(8) Uani 1 1 d . . . . .
H5A H -0.0094 0.4622 0.8951 0.057 Uiso 1 1 calc R U . . .
C11 C 0.4878(4) -0.0275(4) 0.8723(2) 0.0536(9) Uani 1 1 d . . . . .
H11 H 0.5516 -0.0864 0.8819 0.064 Uiso 1 1 calc R U . . .
C6 C 0.1134(4) 0.3612(4) 0.94867(17) 0.0531(9) Uani 1 1 d . . . . .
H6A H 0.0903 0.3982 0.9865 0.064 Uiso 1 1 calc R U . . .
C12 C -0.0402(4) -0.1589(4) 0.7410(2) 0.0580(10) Uani 1 1 d . . . . .
H12 H -0.1077 -0.2156 0.7520 0.070 Uiso 1 1 calc R U . . .
C2 C -0.0530(4) 0.4471(5) 0.7509(2) 0.0565(10) Uani 1 1 d . . . . .
H2 H -0.1057 0.5041 0.7719 0.068 Uiso 1 1 calc R U . . .
C29 C 0.6940(4) 0.7033(4) 0.50320(18) 0.0539(9) Uani 1 1 d . . . . .
H29 H 0.6134 0.6589 0.5091 0.065 Uiso 1 1 calc R U . . .
C36 C 0.8322(4) 0.0935(4) 0.9726(2) 0.0597(10) Uani 1 1 d . . . . .
H36 H 0.8471 0.0566 1.0096 0.072 Uiso 1 1 calc R U . . .
C26 C 0.7275(5) 0.9675(5) 0.6381(2) 0.0597(10) Uani 1 1 d . . . . .
H26 H 0.7867 1.0289 0.6244 0.072 Uiso 1 1 calc R U . . .
C31 C 0.7529(5) 0.6743(4) 0.44907(19) 0.0579(10) Uani 1 1 d . . . . .
H31 H 0.7090 0.6093 0.4191 0.070 Uiso 1 1 calc R U . . .
C30 C 0.8807(4) 0.8588(4) 0.5371(2) 0.0557(9) Uani 1 1 d . . . . .
H30 H 0.9287 0.9220 0.5667 0.067 Uiso 1 1 calc R U . . .
F4 F 0.6509(6) 0.3528(5) 0.4798(2) 0.155(2) Uani 1 1 d . . . . .
C35 C 0.7394(5) 0.2519(4) 0.9122(2) 0.0619(11) Uani 1 1 d . . . . .
H35 H 0.6899 0.3249 0.9075 0.074 Uiso 1 1 calc R U . . .
C39 C 0.5968(4) 0.3387(4) 1.0209(2) 0.0600(10) Uani 1 1 d . . . . .
H39 H 0.5448 0.3373 0.9829 0.072 Uiso 1 1 calc R U . . .
C21 C 0.5464(4) 0.3635(5) 0.6881(2) 0.0597(10) Uani 1 1 d . . . . .
H21 H 0.6038 0.3639 0.6576 0.072 Uiso 1 1 calc R U . . .
C1 C -0.0503(5) 0.4226(5) 0.6880(2) 0.0625(11) Uani 1 1 d . . . . .
H1A H -0.1019 0.4613 0.6580 0.075 Uiso 1 1 calc R U . . .
C32 C 0.9303(5) 0.8233(5) 0.4822(2) 0.0587(10) Uani 1 1 d . . . . .
H32 H 1.0120 0.8641 0.4757 0.070 Uiso 1 1 calc R U . . .
C41 C 0.5597(5) 0.4068(5) 1.0739(3) 0.0669(12) Uani 1 1 d . . . . .
H41 H 0.4813 0.4500 1.0705 0.080 Uiso 1 1 calc R U . . .
C25 C 0.6104(5) 0.7538(5) 0.6298(2) 0.0608(10) Uani 1 1 d . . . . .
H25 H 0.5897 0.6677 0.6103 0.073 Uiso 1 1 calc R U . . .
C24 C 0.6651(5) 1.0000(5) 0.6903(2) 0.0649(11) Uani 1 1 d . . . . .
H24 H 0.6849 1.0850 0.7112 0.078 Uiso 1 1 calc R U . . .
C40 C 0.7826(4) 0.2758(5) 1.0839(2) 0.0635(11) Uani 1 1 d . . . . .
H40 H 0.8589 0.2298 1.0895 0.076 Uiso 1 1 calc R U . . .
C22 C 0.5462(5) 0.4550(5) 0.7393(2) 0.0644(11) Uani 1 1 d . . . . .
H22 H 0.6047 0.5308 0.7498 0.077 Uiso 1 1 calc R U . . .
C34 C 0.8817(5) 0.0377(5) 0.9194(3) 0.0675(12) Uani 1 1 d . . . . .
H34 H 0.9293 -0.0372 0.9221 0.081 Uiso 1 1 calc R U . . .
C33 C 0.7926(5) 0.1892(5) 0.8622(3) 0.0695(12) Uani 1 1 d . . . . .
H33 H 0.7771 0.2219 0.8241 0.083 Uiso 1 1 calc R U . . .
C23 C 0.5529(6) 0.7964(5) 0.6823(2) 0.0709(13) Uani 1 1 d . . . . .
H23 H 0.4930 0.7373 0.6971 0.085 Uiso 1 1 calc R U . . .
C42 C 0.7374(5) 0.3478(5) 1.1333(3) 0.0730(13) Uani 1 1 d . . . . .
H42 H 0.7862 0.3499 1.1721 0.088 Uiso 1 1 calc R U . . .
B2 B 0.7705(4) 0.6834(4) 0.8740(2) 0.0485(9) Uani 1 1 d . . . . .
B1 B 0.7213(5) 0.3566(5) 0.5347(2) 0.0550(10) Uani 1 1 d . . . . .
F2 F 0.8412(5) 0.3850(8) 0.5201(5) 0.221(4) 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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 6 -6 0.0389
7 0 -3 0.1666
0 2 12 0.0796
6 0 0 0.1612
0 -6 6 0.0533
-6 -2 5 0.1771
4 -5 4 0.1323
4 4 -7 0.1286
0 -2 -12 0.0461
-1 -2 -12 0.0647
-6 -1 -5 0.1506
-6 2 8 0.2022
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
N3 Fe1 N8 176.53(11) . . ?
N3 Fe1 N4 78.88(11) . . ?
N3 Fe1 N7 99.40(11) . . ?
N3 Fe1 N2 79.01(11) . . ?
N3 Fe1 N9 102.72(11) . . ?
N8 Fe1 N4 98.16(11) . . ?
N8 Fe1 N7 78.80(11) . . ?
N8 Fe1 N2 103.98(11) . . ?
N8 Fe1 N9 79.09(11) . . ?
N7 Fe1 N4 91.67(12) . . ?
N7 Fe1 N2 93.21(12) . . ?
N2 Fe1 N4 157.84(12) . . ?
N9 Fe1 N4 92.07(12) . . ?
N9 Fe1 N7 157.88(12) . . ?
N9 Fe1 N2 91.50(12) . . ?
C4 N3 Fe1 119.7(2) . . ?
C8 N3 Fe1 120.1(2) . . ?
C8 N3 C4 120.2(3) . . ?
C15 N8 Fe1 119.7(2) . . ?
C19 N8 Fe1 119.7(2) . . ?
C19 N8 C15 120.6(3) . . ?
N5 N4 Fe1 138.4(2) . . ?
N5 N4 C9 106.0(3) . . ?
C9 N4 Fe1 115.5(2) . . ?
N6 N7 Fe1 138.0(2) . . ?
C14 N7 Fe1 115.7(2) . . ?
C14 N7 N6 105.9(3) . . ?
N1 N2 Fe1 138.2(2) . . ?
N1 N2 C3 106.4(3) . . ?
C3 N2 Fe1 115.4(2) . . ?
N10 N9 Fe1 138.4(2) . . ?
N10 N9 C20 105.8(3) . . ?
C20 N9 Fe1 115.8(2) . . ?
N4 N5 H5 124.5 . . ?
C11 N5 N4 110.9(3) . . ?
C11 N5 H5 124.5 . . ?
N7 N6 H6 124.7 . . ?
C12 N6 N7 110.7(3) . . ?
C12 N6 H6 124.7 . . ?
N2 N1 H1 124.7 . . ?
N2 N1 C1 110.6(3) . . ?
C1 N1 H1 124.7 . . ?
N9 N10 H10 124.5 . . ?
N9 N10 C22 110.9(3) . . ?
C22 N10 H10 124.5 . . ?
N8 C15 C14 110.8(3) . . ?
N8 C15 C16 120.8(3) . . ?
C16 C15 C14 128.4(3) . . ?
C31 N12 C32 116.6(4) . . ?
N3 C4 C3 110.8(3) . . ?
N3 C4 C5 120.9(3) . . ?
C5 C4 C3 128.4(3) . . ?
N4 C9 C8 114.7(3) . . ?
N4 C9 C10 110.7(3) . . ?
C10 C9 C8 134.7(3) . . ?
N2 C3 C4 115.1(3) . . ?
N2 C3 C2 109.9(3) . . ?
C2 C3 C4 135.0(3) . . ?
N9 C20 C19 114.5(3) . . ?
N9 C20 C21 110.4(3) . . ?
C21 C20 C19 135.1(3) . . ?
N3 C8 C9 110.7(3) . . ?
N3 C8 C7 121.6(3) . . ?
C7 C8 C9 127.6(3) . . ?
N7 C14 C15 114.8(3) . . ?
N7 C14 C13 110.3(3) . . ?
C13 C14 C15 135.0(3) . . ?
N8 C19 C20 110.8(3) . . ?
N8 C19 C18 121.2(3) . . ?
C18 C19 C20 128.0(3) . . ?
C34 N13 C33 117.0(4) . . ?
C24 N11 C23 116.3(4) . . ?
C42 N14 C41 116.8(4) . . ?
C19 C18 H18 120.8 . . ?
C19 C18 C17 118.3(3) . . ?
C17 C18 H18 120.8 . . ?
C18 C17 H17 120.0 . . ?
C16 C17 C18 120.0(3) . . ?
C16 C17 H17 120.0 . . ?
C29 C28 C27 120.8(4) . . ?
C30 C28 C27 121.8(4) . . ?
C30 C28 C29 117.4(4) . . ?
C39 C38 C37 121.3(4) . . ?
C39 C38 C40 117.3(4) . . ?
C40 C38 C37 121.4(4) . . ?
C15 C16 C17 119.0(3) . . ?
C15 C16 H16 120.5 . . ?
C17 C16 H16 120.5 . . ?
C36 C37 C38 121.6(4) . . ?
C36 C37 C35 117.0(4) . . ?
C35 C37 C38 121.4(4) . . ?
C8 C7 H7 120.9 . . ?
C8 C7 C6 118.2(3) . . ?
C6 C7 H7 120.9 . . ?
C9 C10 H10A 128.1 . . ?
C11 C10 C9 103.9(3) . . ?
C11 C10 H10A 128.1 . . ?
C14 C13 H13 127.7 . . ?
C12 C13 C14 104.7(4) . . ?
C12 C13 H13 127.7 . . ?
C26 C27 C28 120.6(4) . . ?
C25 C27 C28 121.6(4) . . ?
C25 C27 C26 117.7(4) . . ?
C4 C5 H5A 120.7 . . ?
C6 C5 C4 118.6(3) . . ?
C6 C5 H5A 120.7 . . ?
N5 C11 C10 108.5(3) . . ?
N5 C11 H11 125.7 . . ?
C10 C11 H11 125.7 . . ?
C7 C6 H6A 119.7 . . ?
C5 C6 C7 120.5(3) . . ?
C5 C6 H6A 119.7 . . ?
N6 C12 C13 108.5(3) . . ?
N6 C12 H12 125.7 . . ?
C13 C12 H12 125.7 . . ?
C3 C2 H2 127.7 . . ?
C1 C2 C3 104.7(4) . . ?
C1 C2 H2 127.7 . . ?
C28 C29 H29 120.9 . . ?
C31 C29 C28 118.1(4) . . ?
C31 C29 H29 120.9 . . ?
C37 C36 H36 120.4 . . ?
C37 C36 C34 119.1(5) . . ?
C34 C36 H36 120.4 . . ?
C27 C26 H26 120.9 . . ?
C24 C26 C27 118.1(5) . . ?
C24 C26 H26 120.9 . . ?
N12 C31 C29 124.5(4) . . ?
N12 C31 H31 117.7 . . ?
C29 C31 H31 117.7 . . ?
C28 C30 H30 120.0 . . ?
C32 C30 C28 120.0(4) . . ?
C32 C30 H30 120.0 . . ?
C37 C35 H35 120.3 . . ?
C33 C35 C37 119.4(4) . . ?
C33 C35 H35 120.3 . . ?
C38 C39 H39 120.5 . . ?
C38 C39 C41 118.9(5) . . ?
C41 C39 H39 120.5 . . ?
C20 C21 H21 127.8 . . ?
C22 C21 C20 104.5(4) . . ?
C22 C21 H21 127.8 . . ?
N1 C1 C2 108.5(3) . . ?
N1 C1 H1A 125.8 . . ?
C2 C1 H1A 125.8 . . ?
N12 C32 C30 123.4(4) . . ?
N12 C32 H32 118.3 . . ?
C30 C32 H32 118.3 . . ?
N14 C41 C39 123.9(4) . . ?
N14 C41 H41 118.1 . . ?
C39 C41 H41 118.1 . . ?
C27 C25 H25 120.2 . . ?
C23 C25 C27 119.6(5) . . ?
C23 C25 H25 120.2 . . ?
N11 C24 C26 125.0(5) . . ?
N11 C24 H24 117.5 . . ?
C26 C24 H24 117.5 . . ?
C38 C40 H40 120.6 . . ?
C42 C40 C38 118.9(4) . . ?
C42 C40 H40 120.6 . . ?
N10 C22 C21 108.4(4) . . ?
N10 C22 H22 125.8 . . ?
C21 C22 H22 125.8 . . ?
N13 C34 C36 123.8(4) . . ?
N13 C34 H34 118.1 . . ?
C36 C34 H34 118.1 . . ?
N13 C33 C35 123.6(5) . . ?
N13 C33 H33 118.2 . . ?
C35 C33 H33 118.2 . . ?
N11 C23 C25 123.2(5) . . ?
N11 C23 H23 118.4 . . ?
C25 C23 H23 118.4 . . ?
N14 C42 C40 124.2(5) . . ?
N14 C42 H42 117.9 . . ?
C40 C42 H42 117.9 . . ?
F8 B2 F5 108.2(4) . . ?
F8 B2 F7 109.9(4) . . ?
F7 B2 F5 109.6(4) . . ?
F6 B2 F5 109.5(4) . . ?
F6 B2 F8 109.6(4) . . ?
F6 B2 F7 110.1(4) . . ?
F1 B1 F3 113.1(4) . . ?
F1 B1 F4 115.1(5) . . ?
F4 B1 F3 114.4(5) . . ?
F2 B1 F3 107.0(5) . . ?
F2 B1 F1 105.4(7) . . ?
F2 B1 F4 100.1(6) . . ?
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 N3 1.936(3) . ?
Fe1 N8 1.939(3) . ?
Fe1 N4 1.999(3) . ?
Fe1 N7 1.994(3) . ?
Fe1 N2 1.995(3) . ?
Fe1 N9 1.984(3) . ?
F5 B2 1.378(5) . ?
N3 C4 1.357(4) . ?
N3 C8 1.343(4) . ?
N8 C15 1.353(4) . ?
N8 C19 1.347(4) . ?
N4 N5 1.342(4) . ?
N4 C9 1.343(4) . ?
N7 N6 1.350(4) . ?
N7 C14 1.342(4) . ?
N2 N1 1.341(4) . ?
N2 C3 1.350(4) . ?
F8 B2 1.373(5) . ?
F7 B2 1.376(5) . ?
N9 N10 1.339(4) . ?
N9 C20 1.352(4) . ?
N5 H5 0.8600 . ?
N5 C11 1.331(5) . ?
N6 H6 0.8600 . ?
N6 C12 1.338(5) . ?
N1 H1 0.8600 . ?
N1 C1 1.344(6) . ?
N10 H10 0.8600 . ?
N10 C22 1.340(6) . ?
C15 C14 1.453(5) . ?
C15 C16 1.379(5) . ?
F6 B2 1.369(5) . ?
N12 C31 1.319(6) . ?
N12 C32 1.344(6) . ?
C4 C3 1.448(5) . ?
C4 C5 1.387(5) . ?
C9 C8 1.464(5) . ?
C9 C10 1.394(5) . ?
C3 C2 1.399(5) . ?
C20 C19 1.457(5) . ?
C20 C21 1.392(5) . ?
C8 C7 1.381(5) . ?
C14 C13 1.399(5) . ?
C19 C18 1.384(5) . ?
N13 C34 1.317(7) . ?
N13 C33 1.332(7) . ?
N11 C24 1.328(7) . ?
N11 C23 1.344(7) . ?
N14 C41 1.324(7) . ?
N14 C42 1.320(7) . ?
C18 H18 0.9300 . ?
C18 C17 1.393(6) . ?
F3 B1 1.351(6) . ?
C17 H17 0.9300 . ?
C17 C16 1.386(6) . ?
C28 C27 1.491(5) . ?
C28 C29 1.395(6) . ?
C28 C30 1.382(6) . ?
C38 C37 1.477(5) . ?
C38 C39 1.381(6) . ?
C38 C40 1.393(7) . ?
C16 H16 0.9300 . ?
F1 B1 1.312(6) . ?
C37 C36 1.384(6) . ?
C37 C35 1.392(7) . ?
C7 H7 0.9300 . ?
C7 C6 1.392(6) . ?
C10 H10A 0.9300 . ?
C10 C11 1.385(6) . ?
C13 H13 0.9300 . ?
C13 C12 1.369(6) . ?
C27 C26 1.395(6) . ?
C27 C25 1.384(6) . ?
C5 H5A 0.9300 . ?
C5 C6 1.378(6) . ?
C11 H11 0.9300 . ?
C6 H6A 0.9300 . ?
C12 H12 0.9300 . ?
C2 H2 0.9300 . ?
C2 C1 1.373(6) . ?
C29 H29 0.9300 . ?
C29 C31 1.392(6) . ?
C36 H36 0.9300 . ?
C36 C34 1.393(7) . ?
C26 H26 0.9300 . ?
C26 C24 1.381(6) . ?
C31 H31 0.9300 . ?
C30 H30 0.9300 . ?
C30 C32 1.370(6) . ?
F4 B1 1.320(6) . ?
C35 H35 0.9300 . ?
C35 C33 1.381(7) . ?
C39 H39 0.9300 . ?
C39 C41 1.384(6) . ?
C21 H21 0.9300 . ?
C21 C22 1.373(6) . ?
C1 H1A 0.9300 . ?
C32 H32 0.9300 . ?
C41 H41 0.9300 . ?
C25 H25 0.9300 . ?
C25 C23 1.381(6) . ?
C24 H24 0.9300 . ?
C40 H40 0.9300 . ?
C40 C42 1.374(7) . ?
C22 H22 0.9300 . ?
C34 H34 0.9300 . ?
C33 H33 0.9300 . ?
C23 H23 0.9300 . ?
C42 H42 0.9300 . ?
B1 F2 1.305(7) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N3 C4 C3 -0.1(4) . . . . ?
Fe1 N3 C4 C5 -179.9(3) . . . . ?
Fe1 N3 C8 C9 1.2(4) . . . . ?
Fe1 N3 C8 C7 -179.9(3) . . . . ?
Fe1 N8 C15 C14 0.5(4) . . . . ?
Fe1 N8 C15 C16 -179.9(3) . . . . ?
Fe1 N8 C19 C20 0.7(4) . . . . ?
Fe1 N8 C19 C18 -179.4(2) . . . . ?
Fe1 N4 N5 C11 -175.8(3) . . . . ?
Fe1 N4 C9 C8 -3.7(4) . . . . ?
Fe1 N4 C9 C10 176.8(2) . . . . ?
Fe1 N7 N6 C12 -172.3(3) . . . . ?
Fe1 N7 C14 C15 -5.8(4) . . . . ?
Fe1 N7 C14 C13 173.9(3) . . . . ?
Fe1 N2 N1 C1 179.3(3) . . . . ?
Fe1 N2 C3 C4 0.7(4) . . . . ?
Fe1 N2 C3 C2 -179.4(3) . . . . ?
Fe1 N9 N10 C22 177.5(3) . . . . ?
Fe1 N9 C20 C19 1.2(4) . . . . ?
Fe1 N9 C20 C21 -177.9(3) . . . . ?
N3 C4 C3 N2 -0.4(4) . . . . ?
N3 C4 C3 C2 179.7(4) . . . . ?
N3 C4 C5 C6 -0.8(6) . . . . ?
N3 C8 C7 C6 0.3(6) . . . . ?
N8 C15 C14 N7 3.4(4) . . . . ?
N8 C15 C14 C13 -176.1(4) . . . . ?
N8 C15 C16 C17 0.1(5) . . . . ?
N8 C19 C18 C17 -1.5(5) . . . . ?
N4 N5 C11 C10 -0.3(5) . . . . ?
N4 C9 C8 N3 1.7(4) . . . . ?
N4 C9 C8 C7 -177.2(4) . . . . ?
N4 C9 C10 C11 0.3(4) . . . . ?
N7 N6 C12 C13 0.4(5) . . . . ?
N7 C14 C13 C12 0.7(5) . . . . ?
N2 N1 C1 C2 -0.2(5) . . . . ?
N2 C3 C2 C1 -0.2(5) . . . . ?
N9 N10 C22 C21 -0.2(6) . . . . ?
N9 C20 C19 N8 -1.2(4) . . . . ?
N9 C20 C19 C18 178.9(3) . . . . ?
N9 C20 C21 C22 -0.3(5) . . . . ?
N5 N4 C9 C8 179.0(3) . . . . ?
N5 N4 C9 C10 -0.5(4) . . . . ?
N6 N7 C14 C15 179.9(3) . . . . ?
N6 N7 C14 C13 -0.4(4) . . . . ?
N1 N2 C3 C4 -179.8(3) . . . . ?
N1 N2 C3 C2 0.1(4) . . . . ?
N10 N9 C20 C19 179.3(3) . . . . ?
N10 N9 C20 C21 0.2(4) . . . . ?
C15 N8 C19 C20 -177.2(3) . . . . ?
C15 N8 C19 C18 2.7(5) . . . . ?
C15 C14 C13 C12 -179.8(4) . . . . ?
C4 N3 C8 C9 179.7(3) . . . . ?
C4 N3 C8 C7 -1.3(5) . . . . ?
C4 C3 C2 C1 179.7(4) . . . . ?
C4 C5 C6 C7 -0.2(6) . . . . ?
C9 N4 N5 C11 0.5(4) . . . . ?
C9 C8 C7 C6 179.1(4) . . . . ?
C9 C10 C11 N5 0.0(4) . . . . ?
C3 N2 N1 C1 0.1(4) . . . . ?
C3 C4 C5 C6 179.4(4) . . . . ?
C3 C2 C1 N1 0.3(5) . . . . ?
C20 N9 N10 C22 0.0(5) . . . . ?
C20 C19 C18 C17 178.4(3) . . . . ?
C20 C21 C22 N10 0.3(6) . . . . ?
C8 N3 C4 C3 -178.6(3) . . . . ?
C8 N3 C4 C5 1.6(5) . . . . ?
C8 C9 C10 C11 -179.1(4) . . . . ?
C8 C7 C6 C5 0.4(6) . . . . ?
C14 N7 N6 C12 0.0(4) . . . . ?
C14 C15 C16 C17 179.6(4) . . . . ?
C14 C13 C12 N6 -0.6(5) . . . . ?
C19 N8 C15 C14 178.5(3) . . . . ?
C19 N8 C15 C16 -1.9(5) . . . . ?
C19 C20 C21 C22 -179.2(4) . . . . ?
C19 C18 C17 C16 -0.3(6) . . . . ?
C18 C17 C16 C15 1.0(6) . . . . ?
C28 C27 C26 C24 177.6(4) . . . . ?
C28 C27 C25 C23 -177.3(4) . . . . ?
C28 C29 C31 N12 0.1(6) . . . . ?
C28 C30 C32 N12 -0.3(7) . . . . ?
C38 C37 C36 C34 -176.5(4) . . . . ?
C38 C37 C35 C33 176.5(4) . . . . ?
C38 C39 C41 N14 0.6(7) . . . . ?
C38 C40 C42 N14 0.9(8) . . . . ?
C16 C15 C14 N7 -176.1(3) . . . . ?
C16 C15 C14 C13 4.3(7) . . . . ?
C37 C38 C39 C41 -176.7(4) . . . . ?
C37 C38 C40 C42 175.9(4) . . . . ?
C37 C36 C34 N13 0.2(7) . . . . ?
C37 C35 C33 N13 -0.3(7) . . . . ?
C10 C9 C8 N3 -178.9(4) . . . . ?
C10 C9 C8 C7 2.2(7) . . . . ?
C27 C28 C29 C31 177.8(3) . . . . ?
C27 C28 C30 C32 -177.7(4) . . . . ?
C27 C26 C24 N11 -0.2(7) . . . . ?
C27 C25 C23 N11 -0.5(8) . . . . ?
C5 C4 C3 N2 179.4(3) . . . . ?
C5 C4 C3 C2 -0.5(7) . . . . ?
C29 C28 C27 C26 -152.3(4) . . . . ?
C29 C28 C27 C25 25.6(5) . . . . ?
C29 C28 C30 C32 2.3(6) . . . . ?
C36 C37 C35 C33 -1.7(6) . . . . ?
C26 C27 C25 C23 0.7(6) . . . . ?
C31 N12 C32 C30 -1.8(6) . . . . ?
C30 C28 C27 C26 27.7(5) . . . . ?
C30 C28 C27 C25 -154.5(4) . . . . ?
C30 C28 C29 C31 -2.2(5) . . . . ?
C35 C37 C36 C34 1.7(6) . . . . ?
C39 C38 C37 C36 -149.9(4) . . . . ?
C39 C38 C37 C35 32.0(6) . . . . ?
C39 C38 C40 C42 -2.8(6) . . . . ?
C21 C20 C19 N8 177.6(4) . . . . ?
C21 C20 C19 C18 -2.3(7) . . . . ?
C32 N12 C31 C29 1.8(6) . . . . ?
C41 N14 C42 C40 1.7(8) . . . . ?
C25 C27 C26 C24 -0.3(6) . . . . ?
C24 N11 C23 C25 0.0(7) . . . . ?
C40 C38 C37 C36 31.5(6) . . . . ?
C40 C38 C37 C35 -146.7(4) . . . . ?
C40 C38 C39 C41 2.0(6) . . . . ?
C34 N13 C33 C35 2.2(7) . . . . ?
C33 N13 C34 C36 -2.1(7) . . . . ?
C23 N11 C24 C26 0.4(7) . . . . ?
C42 N14 C41 C39 -2.5(7) . . . . ?
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
-0.2038 6.1645 -6.4353 -0.9708 0.2323 0.0607
6.5233 -0.3077 -2.7160 -0.0754 0.0193 -0.9970
0.0816 2.3382 12.4733 0.2323 0.9709 0.0589
6.4951 -0.3389 0.2026 0.0457 0.1870 -0.9813
0.0807 -6.1556 6.4833 0.9717 -0.2325 -0.0419
-5.9916 -1.8915 4.7977 0.4130 -0.0999 0.9052
4.1281 -5.1471 3.5276 0.7353 -0.1752 -0.6547
4.1801 4.3368 -6.5435 -0.7651 0.1839 -0.6171
-0.0149 -2.3448 -12.4878 -0.2321 -0.9702 -0.0690
-1.4311 -2.1517 -11.8973 -0.2303 -0.9617 0.1486
-5.6874 -0.6131 -5.0211 -0.1301 -0.5399 0.8316
-5.5159 1.7933 7.8434 0.1101 0.4637 0.8791
