#------------------------------------------------------------------------------
#$Date: 2022-02-19 01:15:19 +0200 (Sat, 19 Feb 2022) $
#$Revision: 273036 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/63/1566387.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_1566387
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
_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                96.133(3)
_cell_angle_beta                 94.628(3)
_cell_angle_gamma                93.979(4)
_cell_formula_units_Z            2
_cell_length_a                   10.2254(4)
_cell_length_b                   10.1492(6)
_cell_length_c                   21.6116(6)
_cell_measurement_reflns_used    6419
_cell_measurement_temperature    330.00(15)
_cell_measurement_theta_max      71.4770
_cell_measurement_theta_min      4.0940
_cell_volume                     2215.84(17)
_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)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      330.00(15)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -92.00  -6.00   1.00    1.50    --  -42.16 125.00  90.00   86
  2  ω   -112.00 -18.00   1.00    1.50    --  -42.16 -57.00-120.00   94
  3  ω    -64.00  29.00   1.00    1.50    --  -42.16  57.00  30.00   93
  4  ω    -57.00  31.00   1.00    1.50    --  -42.16  38.00-180.00   88
  5  ω     29.00  95.00   1.00    6.00    --  103.72 -94.00 150.00   66
  6  ω     41.00 107.00   1.00    6.00    --  103.72 -94.00  60.00   66
  7  ω    118.00 164.00   1.00    6.00    --  103.72  45.00 -30.00   46
  8  ω     32.00 117.00   1.00    6.00    --  103.72-125.00  30.00   85
  9  ω     75.00 172.00   1.00    6.00    --  103.72  61.00-150.00   97
 10  ω     78.00 104.00   1.00    6.00    --  103.72  61.00-180.00   26
 11  ω    119.00 168.00   1.00    6.00    --  103.72  61.00-180.00   49
 12  ω     71.00 171.00   1.00    6.00    --  103.72  77.00  90.00  100
 13  ω    121.00 173.00   1.00    6.00    --  103.72 125.00  60.00   52
 14  ω     78.00 104.00   1.00    6.00    --  103.72  30.00 -60.00   26
 15  ω    142.00 171.00   1.00    6.00    --  103.72  30.00 -60.00   29
 16  ω     95.00 156.00   1.00    6.00    --  103.72 125.00  30.00   61
 17  ω     33.00 118.00   1.00    6.00    --  103.72-125.00 -90.00   85
 18  ω     31.00  75.00   1.00    6.00    --  103.72 -77.00   0.00   44
;
_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      -0.0792272056
_diffrn_orient_matrix_UB_12      -0.1356625162
_diffrn_orient_matrix_UB_13      -0.0030924640
_diffrn_orient_matrix_UB_21      0.1292717899
_diffrn_orient_matrix_UB_22      -0.0688203433
_diffrn_orient_matrix_UB_23      0.0063487711
_diffrn_orient_matrix_UB_31      -0.0013440592
_diffrn_orient_matrix_UB_32      0.0176424627
_diffrn_orient_matrix_UB_33      0.0716315980
_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  0.0398
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       12
_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       -22
_diffrn_reflns_number            16626
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.062
_diffrn_reflns_theta_min         4.131
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.456
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.137
_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    1.445
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.366
_exptl_crystal_size_mid          0.348
_exptl_crystal_size_min          0.246
_refine_diff_density_max         0.908
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         8476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0719
_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)+(0.1202P)²+0.5191P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2011
_refine_ls_wR_factor_ref         0.2128
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6971
_reflns_number_total             8476
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1sc04956a1.cif
_cod_data_source_block           ltb-106-002b_330_reduap_ref
_cod_original_cell_volume        2215.84(16)
_cod_database_code               1566387
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Fe C42 H34 B2 F8 N14'
_chemical_oxdiff_usercomment     '330 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 99.97
_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 1.466
_oxdiff_exptl_absorpt_empirical_full_min 0.739
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 0.23500(5) 0.18159(5) 0.75754(2) 0.05304(18) Uani 1 1 d . . . . .
F5 F 0.6973(3) 0.7711(3) 0.90934(13) 0.0972(8) Uani 1 1 d . . . . .
N3 N 0.1823(3) 0.2592(3) 0.84026(12) 0.0548(6) Uani 1 1 d . . . . .
N8 N 0.2924(3) 0.0919(3) 0.67853(12) 0.0565(6) Uani 1 1 d . . . . .
N4 N 0.3545(3) 0.0940(3) 0.82074(14) 0.0644(7) Uani 1 1 d . . . . .
N7 N 0.1047(3) 0.0144(3) 0.73927(15) 0.0668(8) Uani 1 1 d . . . . .
N2 N 0.0973(3) 0.3078(3) 0.73240(13) 0.0658(7) Uani 1 1 d . . . . .
F8 F 0.7362(4) 0.7019(4) 0.81164(14) 0.1244(12) Uani 1 1 d . . . . .
F7 F 0.7361(4) 0.5593(3) 0.8828(2) 0.1292(13) Uani 1 1 d . . . . .
N9 N 0.3875(3) 0.3095(3) 0.73904(16) 0.0686(8) Uani 1 1 d . . . . .
N5 N 0.4474(4) 0.0070(4) 0.82030(19) 0.0776(9) Uani 1 1 d . . . . .
H5 H 0.4783 -0.0280 0.7871 0.093 Uiso 1 1 calc R U . . .
N6 N 0.0062(4) -0.0454(4) 0.7664(2) 0.0857(11) Uani 1 1 d . . . . .
H6 H -0.0276 -0.0118 0.7991 0.103 Uiso 1 1 calc R U . . .
N1 N 0.0390(4) 0.3462(5) 0.67994(17) 0.0880(11) Uani 1 1 d . . . . .
H1 H 0.0567 0.3187 0.6427 0.106 Uiso 1 1 calc R U . . .
N10 N 0.4547(4) 0.4223(4) 0.7652(2) 0.0920(12) Uani 1 1 d . . . . .
H10 H 0.4358 0.4677 0.7988 0.110 Uiso 1 1 calc R U . . .
C15 C 0.2314(4) -0.0261(4) 0.65269(16) 0.0629(8) Uani 1 1 d . . . . .
F6 F 0.8986(3) 0.7168(4) 0.8876(2) 0.1351(14) Uani 1 1 d . . . . .
N12 N 0.8689(5) 0.7264(5) 0.43586(18) 0.0927(12) Uani 1 1 d . . . . .
C4 C 0.0915(4) 0.3490(4) 0.84226(16) 0.0586(8) Uani 1 1 d . . . . .
C9 C 0.3349(4) 0.1252(4) 0.88125(16) 0.0616(8) Uani 1 1 d . . . . .
C3 C 0.0421(4) 0.3734(4) 0.77983(17) 0.0645(8) Uani 1 1 d . . . . .
C20 C 0.4483(4) 0.2721(4) 0.68789(18) 0.0669(9) Uani 1 1 d . . . . .
C8 C 0.2381(4) 0.2219(4) 0.89360(15) 0.0588(8) Uani 1 1 d . . . . .
C14 C 0.1273(4) -0.0707(4) 0.68992(18) 0.0669(9) Uani 1 1 d . . . . .
C19 C 0.3929(4) 0.1478(4) 0.65153(16) 0.0612(8) Uani 1 1 d . . . . .
N13 N 0.8685(5) 0.0847(5) 0.8635(3) 0.1071(15) Uani 1 1 d . . . . .
N11 N 0.5786(6) 0.9193(6) 0.7147(2) 0.1149(18) Uani 1 1 d . . . . .
N14 N 0.6335(5) 0.4113(5) 1.1334(3) 0.1069(15) Uani 1 1 d . . . . .
C18 C 0.4326(4) 0.0907(5) 0.59609(18) 0.0733(10) Uani 1 1 d . . . . .
H18 H 0.5008 0.1313 0.5772 0.088 Uiso 1 1 calc R U . . .
F3 F 0.7545(6) 0.2428(4) 0.5599(2) 0.1595(18) Uani 1 1 d . . . . .
C17 C 0.3683(5) -0.0282(5) 0.56936(19) 0.0816(12) Uani 1 1 d . . . . .
H17 H 0.3930 -0.0680 0.5318 0.098 Uiso 1 1 calc R U . . .
C28 C 0.7592(5) 0.7967(5) 0.5476(2) 0.0788(11) Uani 1 1 d . . . . .
C38 C 0.7186(4) 0.2734(4) 1.0267(2) 0.0787(11) Uani 1 1 d . . . . .
C16 C 0.2687(5) -0.0882(5) 0.59740(19) 0.0781(11) Uani 1 1 d . . . . .
H16 H 0.2268 -0.1693 0.5797 0.094 Uiso 1 1 calc R U . . .
F1 F 0.7523(6) 0.4624(4) 0.57670(17) 0.1543(19) Uani 1 1 d . . . . .
C37 C 0.7672(4) 0.2051(4) 0.9701(3) 0.0814(12) Uani 1 1 d . . . . .
C7 C 0.2035(5) 0.2745(5) 0.95086(17) 0.0727(10) Uani 1 1 d . . . . .
H7 H 0.2420 0.2481 0.9876 0.087 Uiso 1 1 calc R U . . .
C10 C 0.4157(4) 0.0555(5) 0.9189(2) 0.0793(11) Uani 1 1 d . . . . .
H10A H 0.4212 0.0579 0.9621 0.095 Uiso 1 1 calc R U . . .
C13 C 0.0429(6) -0.1846(5) 0.6868(3) 0.0918(14) Uani 1 1 d . . . . .
H13 H 0.0383 -0.2593 0.6575 0.110 Uiso 1 1 calc R U . . .
C27 C 0.6990(5) 0.8379(5) 0.6063(2) 0.0829(12) Uani 1 1 d . . . . .
C5 C 0.0544(4) 0.4051(4) 0.89876(18) 0.0702(10) Uani 1 1 d . . . . .
H5A H -0.0079 0.4676 0.8999 0.084 Uiso 1 1 calc R U . . .
C11 C 0.4855(5) -0.0179(5) 0.8776(3) 0.0895(14) Uani 1 1 d . . . . .
H11 H 0.5487 -0.0753 0.8881 0.107 Uiso 1 1 calc R U . . .
C6 C 0.1106(5) 0.3670(5) 0.95275(18) 0.0769(11) Uani 1 1 d . . . . .
H6A H 0.0863 0.4036 0.9910 0.092 Uiso 1 1 calc R U . . .
C12 C -0.0313(6) -0.1641(6) 0.7353(3) 0.1008(16) Uani 1 1 d . . . . .
H12 H -0.0978 -0.2232 0.7453 0.121 Uiso 1 1 calc R U . . .
C2 C -0.0513(5) 0.4546(5) 0.7570(2) 0.0905(14) Uani 1 1 d . . . . .
H2 H -0.1026 0.5107 0.7798 0.109 Uiso 1 1 calc R U . . .
C29 C 0.6970(5) 0.6987(5) 0.5033(2) 0.0874(13) Uani 1 1 d . . . . .
H29 H 0.6175 0.6545 0.5100 0.105 Uiso 1 1 calc R U . . .
C36 C 0.8377(5) 0.0946(5) 0.9725(3) 0.0947(14) Uani 1 1 d . . . . .
H36 H 0.8532 0.0583 1.0099 0.114 Uiso 1 1 calc R U . . .
C26 C 0.7283(6) 0.9645(6) 0.6380(3) 0.0978(15) Uani 1 1 d . . . . .
H26 H 0.7890 1.0248 0.6241 0.117 Uiso 1 1 calc R U . . .
C31 C 0.7571(6) 0.6684(6) 0.4488(2) 0.0939(14) Uani 1 1 d . . . . .
H31 H 0.7151 0.6024 0.4193 0.113 Uiso 1 1 calc R U . . .
C30 C 0.8794(6) 0.8536(6) 0.5346(3) 0.0954(14) Uani 1 1 d . . . . .
H30 H 0.9265 0.9172 0.5637 0.114 Uiso 1 1 calc R U . . .
F4 F 0.6216(6) 0.3451(8) 0.5057(4) 0.258(4) Uani 1 1 d . . . . .
C35 C 0.7453(5) 0.2511(5) 0.9123(3) 0.0974(16) Uani 1 1 d . . . . .
H35 H 0.6958 0.3236 0.9080 0.117 Uiso 1 1 calc R U . . .
C39 C 0.6054(5) 0.3412(6) 1.0238(3) 0.0964(15) Uani 1 1 d . . . . .
H39 H 0.5556 0.3421 0.9860 0.116 Uiso 1 1 calc R U . . .
C21 C 0.5544(6) 0.3607(6) 0.6823(3) 0.1002(16) Uani 1 1 d . . . . .
H21 H 0.6128 0.3572 0.6515 0.120 Uiso 1 1 calc R U . . .
C1 C -0.0498(6) 0.4325(6) 0.6934(3) 0.1017(17) Uani 1 1 d . . . . .
H1A H -0.1022 0.4713 0.6643 0.122 Uiso 1 1 calc R U . . .
C32 C 0.9287(6) 0.8170(7) 0.4795(3) 0.1006(16) Uani 1 1 d . . . . .
H32 H 1.0092 0.8578 0.4719 0.121 Uiso 1 1 calc R U . . .
C41 C 0.5678(6) 0.4071(6) 1.0778(4) 0.1079(18) Uani 1 1 d . . . . .
H41 H 0.4913 0.4514 1.0750 0.130 Uiso 1 1 calc R U . . .
C25 C 0.6100(7) 0.7533(6) 0.6303(3) 0.1060(18) Uani 1 1 d . . . . .
H25 H 0.5886 0.6673 0.6110 0.127 Uiso 1 1 calc R U . . .
C24 C 0.6646(7) 0.9976(7) 0.6906(3) 0.1116(19) Uani 1 1 d . . . . .
H24 H 0.6839 1.0830 0.7110 0.134 Uiso 1 1 calc R U . . .
C40 C 0.7851(5) 0.2731(5) 1.0848(3) 0.0984(16) Uani 1 1 d . . . . .
H40 H 0.8603 0.2273 1.0894 0.118 Uiso 1 1 calc R U . . .
C22 C 0.5541(7) 0.4550(6) 0.7328(3) 0.1123(19) Uani 1 1 d . . . . .
H22 H 0.6137 0.5293 0.7426 0.135 Uiso 1 1 calc R U . . .
C34 C 0.8847(6) 0.0389(6) 0.9187(4) 0.1074(18) Uani 1 1 d . . . . .
H34 H 0.9311 -0.0362 0.9211 0.129 Uiso 1 1 calc R U . . .
C33 C 0.7974(7) 0.1888(6) 0.8616(3) 0.1095(19) Uani 1 1 d . . . . .
H33 H 0.7819 0.2217 0.8233 0.131 Uiso 1 1 calc R U . . .
C23 C 0.5531(7) 0.7986(7) 0.6837(3) 0.120(2) Uani 1 1 d . . . . .
H23 H 0.4926 0.7405 0.6991 0.144 Uiso 1 1 calc R U . . .
C42 C 0.7378(6) 0.3424(6) 1.1366(3) 0.1108(19) Uani 1 1 d . . . . .
H42 H 0.7826 0.3399 1.1756 0.133 Uiso 1 1 calc R U . . .
B2 B 0.7667(5) 0.6867(5) 0.8725(2) 0.0708(11) Uani 1 1 d . . . . .
B1 B 0.7362(6) 0.3564(6) 0.5347(3) 0.0852(14) Uani 1 1 d . . . . .
F2 F 0.8174(7) 0.3661(5) 0.4890(3) 0.193(3) 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'
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'
N N 0.0311 0.0180 '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
5 -5 1 0.1371
4 5 -3 0.1927
-4 4 -7 0.1664
0 0 -14 0.1925
-4 -5 1 0.1570
0 0 14 0.0524
0 1 -14 0.1879
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 N4 77.19(11) . . ?
N3 Fe1 N7 100.89(12) . . ?
N3 Fe1 N2 77.30(12) . . ?
N3 Fe1 N9 104.44(13) . . ?
N8 Fe1 N3 175.37(11) . . ?
N8 Fe1 N4 98.58(12) . . ?
N8 Fe1 N7 77.28(12) . . ?
N8 Fe1 N2 106.97(12) . . ?
N8 Fe1 N9 77.42(12) . . ?
N7 Fe1 N4 92.70(14) . . ?
N2 Fe1 N4 154.43(12) . . ?
N2 Fe1 N7 93.77(13) . . ?
N2 Fe1 N9 92.37(13) . . ?
N9 Fe1 N4 92.27(14) . . ?
N9 Fe1 N7 154.66(13) . . ?
C4 N3 Fe1 119.8(2) . . ?
C4 N3 C8 120.2(3) . . ?
C8 N3 Fe1 120.1(2) . . ?
C15 N8 Fe1 120.1(2) . . ?
C19 N8 Fe1 119.9(2) . . ?
C19 N8 C15 120.0(3) . . ?
N5 N4 Fe1 138.8(3) . . ?
N5 N4 C9 105.9(3) . . ?
C9 N4 Fe1 115.3(2) . . ?
N6 N7 Fe1 138.3(3) . . ?
C14 N7 Fe1 115.3(3) . . ?
C14 N7 N6 106.0(4) . . ?
N1 N2 Fe1 138.6(3) . . ?
N1 N2 C3 105.7(3) . . ?
C3 N2 Fe1 115.7(2) . . ?
N10 N9 Fe1 138.8(3) . . ?
N10 N9 C20 105.3(4) . . ?
C20 N9 Fe1 115.8(3) . . ?
N4 N5 H5 124.4 . . ?
C11 N5 N4 111.3(4) . . ?
C11 N5 H5 124.4 . . ?
N7 N6 H6 124.9 . . ?
C12 N6 N7 110.2(4) . . ?
C12 N6 H6 124.9 . . ?
N2 N1 H1 124.6 . . ?
C1 N1 N2 110.9(4) . . ?
C1 N1 H1 124.6 . . ?
N9 N10 H10 124.4 . . ?
C22 N10 N9 111.3(4) . . ?
C22 N10 H10 124.4 . . ?
N8 C15 C14 111.3(3) . . ?
N8 C15 C16 120.7(4) . . ?
C16 C15 C14 128.1(4) . . ?
C31 N12 C32 116.4(5) . . ?
N3 C4 C3 111.4(3) . . ?
N3 C4 C5 120.9(3) . . ?
C5 C4 C3 127.7(3) . . ?
N4 C9 C8 115.8(3) . . ?
N4 C9 C10 110.0(4) . . ?
C10 C9 C8 134.2(4) . . ?
N2 C3 C4 115.8(3) . . ?
N2 C3 C2 110.5(4) . . ?
C2 C3 C4 133.7(4) . . ?
N9 C20 C19 115.4(4) . . ?
N9 C20 C21 110.8(4) . . ?
C21 C20 C19 133.8(4) . . ?
N3 C8 C9 111.6(3) . . ?
N3 C8 C7 120.9(3) . . ?
C7 C8 C9 127.5(3) . . ?
N7 C14 C15 115.8(4) . . ?
N7 C14 C13 109.6(4) . . ?
C13 C14 C15 134.6(4) . . ?
N8 C19 C20 111.5(3) . . ?
N8 C19 C18 121.5(4) . . ?
C18 C19 C20 127.1(4) . . ?
C33 N13 C34 115.6(5) . . ?
C24 N11 C23 115.0(5) . . ?
C42 N14 C41 116.6(5) . . ?
C19 C18 H18 120.9 . . ?
C19 C18 C17 118.2(4) . . ?
C17 C18 H18 120.9 . . ?
C18 C17 H17 119.6 . . ?
C16 C17 C18 120.9(4) . . ?
C16 C17 H17 119.6 . . ?
C29 C28 C27 121.2(5) . . ?
C30 C28 C27 122.0(5) . . ?
C30 C28 C29 116.8(5) . . ?
C39 C38 C37 121.8(5) . . ?
C40 C38 C37 121.1(4) . . ?
C40 C38 C39 117.1(5) . . ?
C15 C16 H16 120.6 . . ?
C17 C16 C15 118.8(4) . . ?
C17 C16 H16 120.6 . . ?
C36 C37 C38 121.6(5) . . ?
C36 C37 C35 117.2(5) . . ?
C35 C37 C38 121.2(4) . . ?
C8 C7 H7 120.6 . . ?
C8 C7 C6 118.8(4) . . ?
C6 C7 H7 120.6 . . ?
C9 C10 H10A 127.8 . . ?
C11 C10 C9 104.5(4) . . ?
C11 C10 H10A 127.8 . . ?
C14 C13 H13 127.3 . . ?
C12 C13 C14 105.4(5) . . ?
C12 C13 H13 127.3 . . ?
C26 C27 C28 121.0(5) . . ?
C25 C27 C28 121.2(5) . . ?
C25 C27 C26 117.8(5) . . ?
C4 C5 H5A 120.5 . . ?
C6 C5 C4 118.9(4) . . ?
C6 C5 H5A 120.5 . . ?
N5 C11 C10 108.4(4) . . ?
N5 C11 H11 125.8 . . ?
C10 C11 H11 125.8 . . ?
C7 C6 H6A 119.8 . . ?
C5 C6 C7 120.3(3) . . ?
C5 C6 H6A 119.8 . . ?
N6 C12 C13 108.9(5) . . ?
N6 C12 H12 125.5 . . ?
C13 C12 H12 125.5 . . ?
C3 C2 H2 128.0 . . ?
C1 C2 C3 104.1(5) . . ?
C1 C2 H2 128.0 . . ?
C28 C29 H29 121.0 . . ?
C28 C29 C31 118.0(5) . . ?
C31 C29 H29 121.0 . . ?
C37 C36 H36 120.6 . . ?
C34 C36 C37 118.8(6) . . ?
C34 C36 H36 120.6 . . ?
C27 C26 H26 121.1 . . ?
C24 C26 C27 117.7(6) . . ?
C24 C26 H26 121.1 . . ?
N12 C31 C29 124.7(5) . . ?
N12 C31 H31 117.6 . . ?
C29 C31 H31 117.6 . . ?
C28 C30 H30 119.9 . . ?
C32 C30 C28 120.2(6) . . ?
C32 C30 H30 119.9 . . ?
C37 C35 H35 120.3 . . ?
C33 C35 C37 119.3(5) . . ?
C33 C35 H35 120.3 . . ?
C38 C39 H39 120.4 . . ?
C41 C39 C38 119.1(6) . . ?
C41 C39 H39 120.4 . . ?
C20 C21 H21 127.9 . . ?
C22 C21 C20 104.2(5) . . ?
C22 C21 H21 127.9 . . ?
N1 C1 C2 108.9(4) . . ?
N1 C1 H1A 125.6 . . ?
C2 C1 H1A 125.6 . . ?
N12 C32 C30 123.8(6) . . ?
N12 C32 H32 118.1 . . ?
C30 C32 H32 118.1 . . ?
N14 C41 C39 124.2(5) . . ?
N14 C41 H41 117.9 . . ?
C39 C41 H41 117.9 . . ?
C27 C25 H25 120.6 . . ?
C27 C25 C23 118.8(6) . . ?
C23 C25 H25 120.6 . . ?
N11 C24 C26 126.0(7) . . ?
N11 C24 H24 117.0 . . ?
C26 C24 H24 117.0 . . ?
C38 C40 H40 120.5 . . ?
C38 C40 C42 119.0(5) . . ?
C42 C40 H40 120.5 . . ?
N10 C22 C21 108.4(5) . . ?
N10 C22 H22 125.8 . . ?
C21 C22 H22 125.8 . . ?
N13 C34 C36 124.8(6) . . ?
N13 C34 H34 117.6 . . ?
C36 C34 H34 117.6 . . ?
N13 C33 C35 124.3(6) . . ?
N13 C33 H33 117.9 . . ?
C35 C33 H33 117.9 . . ?
N11 C23 C25 124.7(7) . . ?
N11 C23 H23 117.7 . . ?
C25 C23 H23 117.7 . . ?
N14 C42 C40 123.8(6) . . ?
N14 C42 H42 118.1 . . ?
C40 C42 H42 118.1 . . ?
F8 B2 F5 109.3(4) . . ?
F8 B2 F7 110.2(4) . . ?
F8 B2 F6 109.6(5) . . ?
F7 B2 F5 109.7(4) . . ?
F7 B2 F6 108.7(4) . . ?
F6 B2 F5 109.3(4) . . ?
F3 B1 F2 108.6(6) . . ?
F1 B1 F3 112.7(5) . . ?
F1 B1 F2 111.7(6) . . ?
F4 B1 F3 108.0(7) . . ?
F4 B1 F1 111.5(6) . . ?
F4 B1 F2 103.8(7) . . ?
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 2.005(3) . ?
Fe1 N8 1.998(3) . ?
Fe1 N4 2.071(3) . ?
Fe1 N7 2.066(4) . ?
Fe1 N2 2.048(3) . ?
Fe1 N9 2.052(4) . ?
F5 B2 1.379(5) . ?
N3 C4 1.345(4) . ?
N3 C8 1.347(4) . ?
N8 C15 1.353(5) . ?
N8 C19 1.344(5) . ?
N4 N5 1.341(4) . ?
N4 C9 1.347(5) . ?
N7 N6 1.347(5) . ?
N7 C14 1.345(5) . ?
N2 N1 1.345(5) . ?
N2 C3 1.346(5) . ?
F8 B2 1.354(6) . ?
F7 B2 1.355(6) . ?
N9 N10 1.339(5) . ?
N9 C20 1.344(5) . ?
N5 H5 0.8600 . ?
N5 C11 1.323(6) . ?
N6 H6 0.8600 . ?
N6 C12 1.331(7) . ?
N1 H1 0.8600 . ?
N1 C1 1.332(7) . ?
N10 H10 0.8600 . ?
N10 C22 1.324(8) . ?
C15 C14 1.461(6) . ?
C15 C16 1.384(5) . ?
F6 B2 1.367(6) . ?
N12 C31 1.314(7) . ?
N12 C32 1.323(7) . ?
C4 C3 1.454(5) . ?
C4 C5 1.384(5) . ?
C9 C8 1.461(5) . ?
C9 C10 1.393(5) . ?
C3 C2 1.398(6) . ?
C20 C19 1.465(6) . ?
C20 C21 1.382(7) . ?
C8 C7 1.377(5) . ?
C14 C13 1.387(6) . ?
C19 C18 1.378(5) . ?
N13 C34 1.328(8) . ?
N13 C33 1.326(8) . ?
N11 C24 1.319(9) . ?
N11 C23 1.329(9) . ?
N14 C41 1.324(8) . ?
N14 C42 1.316(8) . ?
C18 H18 0.9300 . ?
C18 C17 1.379(7) . ?
F3 B1 1.345(7) . ?
C17 H17 0.9300 . ?
C17 C16 1.366(7) . ?
C28 C27 1.488(7) . ?
C28 C29 1.386(7) . ?
C28 C30 1.384(7) . ?
C38 C37 1.481(7) . ?
C38 C39 1.387(7) . ?
C38 C40 1.378(8) . ?
C16 H16 0.9300 . ?
F1 B1 1.323(7) . ?
C37 C36 1.378(7) . ?
C37 C35 1.386(8) . ?
C7 H7 0.9300 . ?
C7 C6 1.382(6) . ?
C10 H10A 0.9300 . ?
C10 C11 1.377(7) . ?
C13 H13 0.9300 . ?
C13 C12 1.349(8) . ?
C27 C26 1.391(8) . ?
C27 C25 1.377(8) . ?
C5 H5A 0.9300 . ?
C5 C6 1.364(6) . ?
C11 H11 0.9300 . ?
C6 H6A 0.9300 . ?
C12 H12 0.9300 . ?
C2 H2 0.9300 . ?
C2 C1 1.371(8) . ?
C29 H29 0.9300 . ?
C29 C31 1.387(8) . ?
C36 H36 0.9300 . ?
C36 C34 1.376(8) . ?
C26 H26 0.9300 . ?
C26 C24 1.378(8) . ?
C31 H31 0.9300 . ?
C30 H30 0.9300 . ?
C30 C32 1.356(8) . ?
F4 B1 1.275(8) . ?
C35 H35 0.9300 . ?
C35 C33 1.371(8) . ?
C39 H39 0.9300 . ?
C39 C41 1.377(8) . ?
C21 H21 0.9300 . ?
C21 C22 1.373(9) . ?
C1 H1A 0.9300 . ?
C32 H32 0.9300 . ?
C41 H41 0.9300 . ?
C25 H25 0.9300 . ?
C25 C23 1.384(8) . ?
C24 H24 0.9300 . ?
C40 H40 0.9300 . ?
C40 C42 1.396(8) . ?
C22 H22 0.9300 . ?
C34 H34 0.9300 . ?
C33 H33 0.9300 . ?
C23 H23 0.9300 . ?
C42 H42 0.9300 . ?
B1 F2 1.348(8) . ?
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 1.4(4) . . . . ?
Fe1 N3 C4 C5 -179.3(3) . . . . ?
Fe1 N3 C8 C9 0.4(4) . . . . ?
Fe1 N3 C8 C7 179.8(3) . . . . ?
Fe1 N8 C15 C14 -0.3(4) . . . . ?
Fe1 N8 C15 C16 178.9(3) . . . . ?
Fe1 N8 C19 C20 1.2(4) . . . . ?
Fe1 N8 C19 C18 -178.1(3) . . . . ?
Fe1 N4 N5 C11 -176.2(4) . . . . ?
Fe1 N4 C9 C8 -3.5(4) . . . . ?
Fe1 N4 C9 C10 176.9(3) . . . . ?
Fe1 N7 N6 C12 -171.6(4) . . . . ?
Fe1 N7 C14 C15 -6.2(4) . . . . ?
Fe1 N7 C14 C13 173.5(3) . . . . ?
Fe1 N2 N1 C1 178.1(4) . . . . ?
Fe1 N2 C3 C4 2.2(5) . . . . ?
Fe1 N2 C3 C2 -179.1(3) . . . . ?
Fe1 N9 N10 C22 174.8(4) . . . . ?
Fe1 N9 C20 C19 2.4(5) . . . . ?
Fe1 N9 C20 C21 -176.0(3) . . . . ?
N3 C4 C3 N2 -2.3(5) . . . . ?
N3 C4 C3 C2 179.4(5) . . . . ?
N3 C4 C5 C6 -0.6(6) . . . . ?
N3 C8 C7 C6 -0.3(6) . . . . ?
N8 C15 C14 N7 4.3(5) . . . . ?
N8 C15 C14 C13 -175.4(5) . . . . ?
N8 C15 C16 C17 0.0(7) . . . . ?
N8 C19 C18 C17 -1.6(6) . . . . ?
N4 N5 C11 C10 -0.1(6) . . . . ?
N4 C9 C8 N3 2.1(5) . . . . ?
N4 C9 C8 C7 -177.3(4) . . . . ?
N4 C9 C10 C11 0.6(5) . . . . ?
N7 N6 C12 C13 0.1(7) . . . . ?
N7 C14 C13 C12 0.6(6) . . . . ?
N2 N1 C1 C2 0.6(7) . . . . ?
N2 C3 C2 C1 0.8(6) . . . . ?
N9 N10 C22 C21 0.1(8) . . . . ?
N9 C20 C19 N8 -2.3(5) . . . . ?
N9 C20 C19 C18 176.9(4) . . . . ?
N9 C20 C21 C22 -0.5(6) . . . . ?
N5 N4 C9 C8 178.9(3) . . . . ?
N5 N4 C9 C10 -0.7(5) . . . . ?
N6 N7 C14 C15 179.8(3) . . . . ?
N6 N7 C14 C13 -0.5(5) . . . . ?
N1 N2 C3 C4 -179.1(4) . . . . ?
N1 N2 C3 C2 -0.4(5) . . . . ?
N10 N9 C20 C19 178.9(4) . . . . ?
N10 N9 C20 C21 0.6(5) . . . . ?
C15 N8 C19 C20 -177.8(3) . . . . ?
C15 N8 C19 C18 2.9(5) . . . . ?
C15 C14 C13 C12 -179.8(5) . . . . ?
C4 N3 C8 C9 -179.3(3) . . . . ?
C4 N3 C8 C7 0.1(6) . . . . ?
C4 C3 C2 C1 179.1(5) . . . . ?
C4 C5 C6 C7 0.3(7) . . . . ?
C9 N4 N5 C11 0.5(5) . . . . ?
C9 C8 C7 C6 179.0(4) . . . . ?
C9 C10 C11 N5 -0.3(6) . . . . ?
C3 N2 N1 C1 -0.1(6) . . . . ?
C3 C4 C5 C6 178.6(4) . . . . ?
C3 C2 C1 N1 -0.8(7) . . . . ?
C20 N9 N10 C22 -0.4(6) . . . . ?
C20 C19 C18 C17 179.3(4) . . . . ?
C20 C21 C22 N10 0.2(7) . . . . ?
C8 N3 C4 C3 -178.9(3) . . . . ?
C8 N3 C4 C5 0.4(6) . . . . ?
C8 C9 C10 C11 -178.8(5) . . . . ?
C8 C7 C6 C5 0.1(7) . . . . ?
C14 N7 N6 C12 0.2(5) . . . . ?
C14 C15 C16 C17 179.0(4) . . . . ?
C14 C13 C12 N6 -0.4(7) . . . . ?
C19 N8 C15 C14 178.7(3) . . . . ?
C19 N8 C15 C16 -2.1(6) . . . . ?
C19 C20 C21 C22 -178.4(5) . . . . ?
C19 C18 C17 C16 -0.5(7) . . . . ?
C18 C17 C16 C15 1.3(7) . . . . ?
C28 C27 C26 C24 177.3(5) . . . . ?
C28 C27 C25 C23 -177.4(5) . . . . ?
C28 C29 C31 N12 -0.2(8) . . . . ?
C28 C30 C32 N12 -0.8(9) . . . . ?
C38 C37 C36 C34 -177.4(5) . . . . ?
C38 C37 C35 C33 176.9(5) . . . . ?
C38 C39 C41 N14 0.5(9) . . . . ?
C38 C40 C42 N14 -1.3(9) . . . . ?
C16 C15 C14 N7 -174.8(4) . . . . ?
C16 C15 C14 C13 5.6(8) . . . . ?
C37 C38 C39 C41 -177.6(5) . . . . ?
C37 C38 C40 C42 178.0(5) . . . . ?
C37 C36 C34 N13 0.7(9) . . . . ?
C37 C35 C33 N13 0.4(9) . . . . ?
C10 C9 C8 N3 -178.5(5) . . . . ?
C10 C9 C8 C7 2.2(8) . . . . ?
C27 C28 C29 C31 178.0(4) . . . . ?
C27 C28 C30 C32 -177.5(5) . . . . ?
C27 C26 C24 N11 1.0(9) . . . . ?
C27 C25 C23 N11 -0.6(11) . . . . ?
C5 C4 C3 N2 178.5(4) . . . . ?
C5 C4 C3 C2 0.2(8) . . . . ?
C29 C28 C27 C26 -154.0(5) . . . . ?
C29 C28 C27 C25 24.4(7) . . . . ?
C29 C28 C30 C32 2.7(8) . . . . ?
C36 C37 C35 C33 -2.2(8) . . . . ?
C26 C27 C25 C23 1.0(8) . . . . ?
C31 N12 C32 C30 -1.7(9) . . . . ?
C30 C28 C27 C26 26.2(7) . . . . ?
C30 C28 C27 C25 -155.4(5) . . . . ?
C30 C28 C29 C31 -2.2(7) . . . . ?
C35 C37 C36 C34 1.7(8) . . . . ?
C39 C38 C37 C36 -150.8(5) . . . . ?
C39 C38 C37 C35 30.2(7) . . . . ?
C39 C38 C40 C42 -1.5(8) . . . . ?
C21 C20 C19 N8 175.6(5) . . . . ?
C21 C20 C19 C18 -5.2(8) . . . . ?
C32 N12 C31 C29 2.2(8) . . . . ?
C41 N14 C42 C40 3.6(9) . . . . ?
C25 C27 C26 C24 -1.2(8) . . . . ?
C24 N11 C23 C25 0.4(10) . . . . ?
C40 C38 C37 C36 29.7(7) . . . . ?
C40 C38 C37 C35 -149.3(5) . . . . ?
C40 C38 C39 C41 1.9(8) . . . . ?
C34 N13 C33 C35 1.9(9) . . . . ?
C33 N13 C34 C36 -2.5(9) . . . . ?
C23 N11 C24 C26 -0.6(9) . . . . ?
C42 N14 C41 C39 -3.2(9) . . . . ?
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
4.9938 -4.6552 1.0201 0.2327 0.9724 -0.0158
4.3833 4.6129 -2.8761 -0.9642 0.2309 -0.1305
-4.2782 4.2241 -6.8359 -0.2130 -0.8872 -0.4094
0.4201 -0.2967 -13.8608 0.0498 -0.0133 -0.9987
-4.3430 -4.6605 1.2562 0.9725 -0.2327 0.0136
-0.3856 0.3334 13.8463 -0.0575 0.0151 0.9982
-0.1484 0.6686 -13.9527 -0.0358 -0.1538 -0.9875
