#------------------------------------------------------------------------------
#$Date: 2022-02-19 01:15:19 +0200 (Sat, 19 Feb 2022) $
#$Revision: 273036 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/63/1566399.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_1566399
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      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-09-03 deposited with the CCDC.	2022-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.403(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2076(3)
_cell_length_b                   18.9941(9)
_cell_length_c                   22.8634(8)
_cell_measurement_reflns_used    5682
_cell_measurement_temperature    300.0(2)
_cell_measurement_theta_max      71.7920
_cell_measurement_theta_min      4.4920
_cell_volume                     4405.2(3)
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300.0(2)
_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 0.982
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -116.00 -17.00   1.00    5.00    --  -41.91 -38.00-180.00   99
  2  ω    -92.00  -2.00   1.00    5.00    --  -41.91 125.00 -30.00   90
  3  ω      9.00 118.00   1.00    5.00    --   41.91  77.00 120.00  109
  4  ω     27.00 132.00   1.00   20.00    --  103.72 -30.00-180.00  105
  5  ω     31.00 118.00   1.00   20.00    --  103.72-125.00-180.00   87
  6  ω     31.00 130.00   1.00   20.00    --  103.72 -45.00 -90.00   99
  7  ω     94.00 177.00   1.00   20.00    --  103.72 125.00-180.00   83
  8  ω     31.00 130.00   1.00   20.00    --  103.72 -45.00  90.00   99
  9  ω     97.00 174.00   1.00   20.00    --  103.72  45.00-180.00   77
 10  ω     43.00 130.00   1.00   20.00    --  103.72 -77.00  90.00   87
;
_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      -0.0729265000
_diffrn_orient_matrix_UB_12      -0.0608448000
_diffrn_orient_matrix_UB_13      -0.0343779000
_diffrn_orient_matrix_UB_21      -0.0438176000
_diffrn_orient_matrix_UB_22      0.0506758000
_diffrn_orient_matrix_UB_23      -0.0510153000
_diffrn_orient_matrix_UB_31      0.1257820000
_diffrn_orient_matrix_UB_32      -0.0175552000
_diffrn_orient_matrix_UB_33      -0.0285402000
_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  0.0476
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            25065
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.973
_diffrn_reflns_theta_min         3.891
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.477
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.302
_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    1.454
_exptl_crystal_description       block
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.143
_refine_diff_density_max         2.814
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.109
_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         8525
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1197
_refine_ls_R_factor_gt           0.0982
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2572
_refine_ls_wR_factor_ref         0.2914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5993
_reflns_number_total             8525
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1sc04956a1.cif
_cod_data_source_block           ltb-137-001_300ah_red_ref
_cod_database_code               1566399
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Fe C42 H34 N14 B2 F8'
_chemical_oxdiff_usercomment     '300 K After heating to 400 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 99.96
_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), C7(H7), C16(H16), C5(H5a), C18(H18),
 C10(H10a), C6(H6a), C17(H17), C25(H25), C11(H11), C26(H26), C13(H13), C12(H12),
  C2(H2), C36(H36), C40(H40), C42(H42), C30(H30), C29(H29), C35(H35), C32(H32),
 C23(H23), C24(H24), C31(H31), C1(H1a), C21(H21), C33(H33), C34(H34), C22(H22),
 C41(H41), C39(H39)
;
_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 1.229
_oxdiff_exptl_absorpt_empirical_full_min 0.817
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.27110(5) 0.71402(3) 0.67957(2) 0.0455(2) Uani 1 1 d . . . . .
F6 F 0.2100(3) 0.56765(19) 0.38963(14) 0.0867(9) Uani 1 1 d . . . . .
F5 F 0.2533(4) 0.5496(2) 0.29731(17) 0.1045(12) Uani 1 1 d . . . . .
N4 N 0.1474(3) 0.6380(2) 0.63996(17) 0.0586(9) Uani 1 1 d . . . . .
N8 N 0.2163(3) 0.71046(17) 0.76086(15) 0.0495(7) Uani 1 1 d . . . . .
N3 N 0.3250(3) 0.70914(17) 0.59814(15) 0.0501(7) Uani 1 1 d . . . . .
F8 F 0.2515(4) 0.6593(2) 0.3328(2) 0.1072(12) Uani 1 1 d . . . . .
N7 N 0.3982(3) 0.6402(2) 0.72093(17) 0.0599(9) Uani 1 1 d . . . . .
N9 N 0.1248(4) 0.7884(2) 0.67551(17) 0.0580(8) Uani 1 1 d . . . . .
N2 N 0.4153(4) 0.7892(2) 0.68186(16) 0.0594(9) Uani 1 1 d . . . . .
N5 N 0.0520(4) 0.5939(2) 0.6549(2) 0.0711(11) Uani 1 1 d . . . . .
H5 H 0.0215 0.5935 0.6885 0.085 Uiso 1 1 calc R U . . .
F7 F 0.4125(3) 0.5859(3) 0.3657(2) 0.1272(17) Uani 1 1 d . . . . .
C9 C 0.1667(4) 0.6212(2) 0.58458(19) 0.0550(9) Uani 1 1 d . . . . .
C15 C 0.2744(4) 0.6651(2) 0.80014(18) 0.0546(9) Uani 1 1 d . . . . .
N6 N 0.4936(4) 0.5964(2) 0.7072(2) 0.0767(12) Uani 1 1 d . . . . .
H6 H 0.5264 0.5965 0.6742 0.092 Uiso 1 1 calc R U . . .
C4 C 0.4204(4) 0.7524(2) 0.58308(17) 0.0515(9) Uani 1 1 d . . . . .
N1 N 0.4781(5) 0.8337(3) 0.7205(2) 0.0780(12) Uani 1 1 d . . . . .
H1 H 0.4600 0.8393 0.7561 0.094 Uiso 1 1 calc R U . . .
C8 C 0.2666(4) 0.6632(2) 0.55951(17) 0.0531(9) Uani 1 1 d . . . . .
F3 F 0.7770(6) 0.9441(2) 0.56134(18) 0.1309(17) Uani 1 1 d . . . . .
N10 N 0.0614(5) 0.8322(3) 0.6357(2) 0.0779(12) Uani 1 1 d . . . . .
H10 H 0.0794 0.8366 0.6000 0.094 Uiso 1 1 calc R U . . .
C3 C 0.4729(4) 0.7967(2) 0.6321(2) 0.0555(9) Uani 1 1 d . . . . .
C20 C 0.0668(4) 0.7967(2) 0.7252(2) 0.0579(10) Uani 1 1 d . . . . .
C14 C 0.3742(4) 0.6231(2) 0.7757(2) 0.0592(10) Uani 1 1 d . . . . .
C19 C 0.1196(4) 0.7534(2) 0.77486(18) 0.0550(9) Uani 1 1 d . . . . .
C7 C 0.3013(5) 0.6592(3) 0.5024(2) 0.0663(11) Uani 1 1 d . . . . .
H7 H 0.2607 0.6271 0.4756 0.080 Uiso 1 1 calc R U . . .
F4 F 0.8226(6) 0.9377(3) 0.4684(2) 0.144(2) Uani 1 1 d . . . . .
N12 N 0.6342(6) 0.6125(3) 0.6060(3) 0.1008(18) Uani 1 1 d . . . . .
C16 C 0.2381(5) 0.6616(3) 0.8566(2) 0.0669(12) Uani 1 1 d . . . . .
H16 H 0.2783 0.6295 0.8836 0.080 Uiso 1 1 calc R U . . .
C5 C 0.4584(5) 0.7510(3) 0.5268(2) 0.0613(10) Uani 1 1 d . . . . .
H5A H 0.5238 0.7812 0.5164 0.074 Uiso 1 1 calc R U . . .
N13 N 0.1454(5) 0.8567(3) 0.5254(2) 0.0833(13) Uani 1 1 d . . . . .
C27 C 0.7937(4) 0.6242(3) 0.4409(3) 0.0708(13) Uani 1 1 d . . . . .
C18 C 0.0803(4) 0.7530(3) 0.8310(2) 0.0638(11) Uani 1 1 d . . . . .
H18 H 0.0145 0.7833 0.8408 0.077 Uiso 1 1 calc R U . . .
C10 C 0.0837(5) 0.5665(3) 0.5643(3) 0.0717(13) Uani 1 1 d . . . . .
H10A H 0.0778 0.5449 0.5276 0.086 Uiso 1 1 calc R U . . .
C28 C 0.7419(5) 0.6199(3) 0.4988(3) 0.0722(13) Uani 1 1 d . . . . .
F1 F 0.7742(6) 0.8412(2) 0.5143(3) 0.143(2) Uani 1 1 d . . . . .
N11 N 0.8899(5) 0.6392(3) 0.3321(2) 0.0922(16) Uani 1 1 d . . . . .
N14 N 0.4265(6) 0.8953(4) 0.2588(3) 0.109(2) Uani 1 1 d . . . . .
C37 C 0.2503(5) 0.8758(3) 0.4191(2) 0.0694(12) Uani 1 1 d . . . . .
C6 C 0.3976(6) 0.7043(3) 0.4865(2) 0.0700(13) Uani 1 1 d . . . . .
H6A H 0.4214 0.7030 0.4484 0.084 Uiso 1 1 calc R U . . .
C17 C 0.1415(5) 0.7064(3) 0.8722(2) 0.0702(13) Uani 1 1 d . . . . .
H17 H 0.1174 0.7054 0.9103 0.084 Uiso 1 1 calc R U . . .
C25 C 0.9121(5) 0.6585(4) 0.4353(3) 0.0836(16) Uani 1 1 d . . . . .
H25 H 0.9615 0.6774 0.4682 0.100 Uiso 1 1 calc R U . . .
C11 C 0.0124(5) 0.5510(3) 0.6100(3) 0.0854(17) Uani 1 1 d . . . . .
H11 H -0.0525 0.5167 0.6097 0.102 Uiso 1 1 calc R U . . .
B2 B 0.2828(5) 0.5905(3) 0.3459(2) 0.0627(12) Uani 1 1 d . . . . .
C38 C 0.3087(5) 0.8837(3) 0.3634(3) 0.0766(14) Uani 1 1 d . . . . .
C26 C 0.7281(5) 0.5948(4) 0.3901(3) 0.0860(17) Uani 1 1 d . . . . .
H26 H 0.6503 0.5698 0.3918 0.103 Uiso 1 1 calc R U . . .
C13 C 0.4566(5) 0.5669(3) 0.7967(3) 0.0802(14) Uani 1 1 d . . . . .
H13 H 0.4605 0.5444 0.8330 0.096 Uiso 1 1 calc R U . . .
C12 C 0.5301(5) 0.5533(3) 0.7510(3) 0.0885(18) Uani 1 1 d . . . . .
H12 H 0.5953 0.5190 0.7511 0.106 Uiso 1 1 calc R U . . .
C2 C 0.5726(6) 0.8469(3) 0.6395(3) 0.0826(15) Uani 1 1 d . . . . .
H2 H 0.6269 0.8624 0.6121 0.099 Uiso 1 1 calc R U . . .
C36 C 0.1314(6) 0.8413(4) 0.4217(3) 0.0858(16) Uani 1 1 d . . . . .
H36 H 0.0846 0.8235 0.3877 0.103 Uiso 1 1 calc R U . . .
C40 C 0.2800(6) 0.8364(4) 0.3166(3) 0.0890(17) Uani 1 1 d . . . . .
H40 H 0.2199 0.8002 0.3200 0.107 Uiso 1 1 calc R U . . .
C42 C 0.3393(7) 0.8427(4) 0.2657(4) 0.103(2) Uani 1 1 d . . . . .
H42 H 0.3193 0.8104 0.2354 0.124 Uiso 1 1 calc R U . . .
F2 F 0.6240(5) 0.9175(4) 0.4899(4) 0.207(3) Uani 1 1 d . . . . .
C30 C 0.6641(6) 0.5636(3) 0.5131(3) 0.0862(16) Uani 1 1 d . . . . .
H30 H 0.6465 0.5267 0.4866 0.103 Uiso 1 1 calc R U . . .
C29 C 0.7674(6) 0.6710(3) 0.5413(3) 0.0830(16) Uani 1 1 d . . . . .
H29 H 0.8221 0.7087 0.5348 0.100 Uiso 1 1 calc R U . . .
C35 C 0.3122(5) 0.9026(3) 0.4704(3) 0.0781(14) Uani 1 1 d . . . . .
H35 H 0.3908 0.9273 0.4704 0.094 Uiso 1 1 calc R U . . .
C32 C 0.6137(7) 0.5626(4) 0.5659(3) 0.096(2) Uani 1 1 d . . . . .
H32 H 0.5618 0.5245 0.5742 0.116 Uiso 1 1 calc R U . . .
C23 C 0.9553(6) 0.6644(4) 0.3808(3) 0.0889(17) Uani 1 1 d . . . . .
H23 H 1.0348 0.6873 0.3780 0.107 Uiso 1 1 calc R U . . .
C24 C 0.7787(6) 0.6029(4) 0.3374(3) 0.0928(19) Uani 1 1 d . . . . .
H24 H 0.7343 0.5824 0.3039 0.111 Uiso 1 1 calc R U . . .
C31 C 0.7117(7) 0.6665(4) 0.5938(3) 0.099(2) Uani 1 1 d . . . . .
H31 H 0.7287 0.7021 0.6215 0.119 Uiso 1 1 calc R U . . .
C1 C 0.5721(7) 0.8683(3) 0.6968(3) 0.0936(19) Uani 1 1 d . . . . .
H1A H 0.6284 0.9015 0.7159 0.112 Uiso 1 1 calc R U . . .
C21 C -0.0343(6) 0.8467(4) 0.7159(3) 0.0901(17) Uani 1 1 d . . . . .
H21 H -0.0901 0.8622 0.7428 0.108 Uiso 1 1 calc R U . . .
C33 C 0.2570(7) 0.8925(3) 0.5227(3) 0.0857(16) Uani 1 1 d . . . . .
H33 H 0.2996 0.9116 0.5572 0.103 Uiso 1 1 calc R U . . .
C34 C 0.0835(6) 0.8336(4) 0.4750(3) 0.0885(17) Uani 1 1 d . . . . .
H34 H 0.0030 0.8109 0.4759 0.106 Uiso 1 1 calc R U . . .
C22 C -0.0331(7) 0.8678(4) 0.6588(3) 0.0980(19) Uani 1 1 d . . . . .
H22 H -0.0885 0.9013 0.6393 0.118 Uiso 1 1 calc R U . . .
C41 C 0.4510(8) 0.9394(4) 0.3020(4) 0.120(3) Uani 1 1 d . . . . .
H41 H 0.5112 0.9752 0.2976 0.144 Uiso 1 1 calc R U . . .
B1 B 0.7483(6) 0.9112(4) 0.5089(3) 0.0741(14) Uani 1 1 d . . . . .
C39 C 0.3946(7) 0.9374(4) 0.3541(4) 0.104(2) Uani 1 1 d . . . . .
H39 H 0.4144 0.9719 0.3826 0.125 Uiso 1 1 calc R U . . .
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
-4 -9 -3 0.0890
4 -7 6 0.0670
-4 -1 12 0.1754
3 10 5 0.0821
4 -7 -9 0.1558
1 5 -14 0.1380
1 -6 12 0.1093
-4 7 -8 0.0752
-5 3 -8 0.0730
5 -3 9 0.0796
3 -1 -13 0.1666
1 12 2 0.0764
5 -7 -7 0.1447
3 -11 3 0.0581
0 -11 8 0.0993
-1 11 -5 0.0825
-6 0 -6 0.0743
0 -12 1 0.0602
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 N7 92.77(18) . . ?
N8 Fe1 N4 99.39(14) . . ?
N8 Fe1 N3 175.40(15) . . ?
N8 Fe1 N7 77.19(14) . . ?
N8 Fe1 N9 77.73(14) . . ?
N8 Fe1 N2 105.94(14) . . ?
N3 Fe1 N4 77.14(14) . . ?
N3 Fe1 N7 99.83(14) . . ?
N3 Fe1 N9 105.33(14) . . ?
N3 Fe1 N2 77.57(14) . . ?
N9 Fe1 N4 93.17(15) . . ?
N9 Fe1 N7 154.85(15) . . ?
N2 Fe1 N4 154.67(15) . . ?
N2 Fe1 N7 92.79(15) . . ?
N2 Fe1 N9 92.21(16) . . ?
N5 N4 Fe1 138.1(3) . . ?
C9 N4 Fe1 115.7(3) . . ?
C9 N4 N5 106.1(4) . . ?
C15 N8 Fe1 119.8(3) . . ?
C15 N8 C19 120.9(3) . . ?
C19 N8 Fe1 119.3(3) . . ?
C4 N3 Fe1 119.4(3) . . ?
C8 N3 Fe1 119.8(3) . . ?
C8 N3 C4 120.8(4) . . ?
N6 N7 Fe1 138.4(3) . . ?
C14 N7 Fe1 114.9(3) . . ?
C14 N7 N6 106.2(4) . . ?
N10 N9 Fe1 138.6(3) . . ?
N10 N9 C20 106.0(4) . . ?
C20 N9 Fe1 115.4(3) . . ?
N1 N2 Fe1 138.5(4) . . ?
N1 N2 C3 105.7(4) . . ?
C3 N2 Fe1 115.6(3) . . ?
N4 N5 H5 124.9 . . ?
C11 N5 N4 110.2(4) . . ?
C11 N5 H5 124.9 . . ?
N4 C9 C8 115.1(4) . . ?
N4 C9 C10 110.1(4) . . ?
C10 C9 C8 134.8(4) . . ?
N8 C15 C14 111.9(4) . . ?
N8 C15 C16 121.0(4) . . ?
C16 C15 C14 127.1(4) . . ?
N7 N6 H6 124.5 . . ?
C12 N6 N7 111.1(4) . . ?
C12 N6 H6 124.5 . . ?
N3 C4 C3 111.7(3) . . ?
N3 C4 C5 120.7(4) . . ?
C5 C4 C3 127.5(4) . . ?
N2 N1 H1 124.5 . . ?
C1 N1 N2 111.0(5) . . ?
C1 N1 H1 124.5 . . ?
N3 C8 C9 112.2(4) . . ?
N3 C8 C7 121.0(4) . . ?
C7 C8 C9 126.9(4) . . ?
N9 N10 H10 124.5 . . ?
C22 N10 N9 111.1(5) . . ?
C22 N10 H10 124.5 . . ?
N2 C3 C4 115.6(4) . . ?
N2 C3 C2 110.6(4) . . ?
C2 C3 C4 133.7(5) . . ?
N9 C20 C19 115.6(4) . . ?
N9 C20 C21 109.7(5) . . ?
C21 C20 C19 134.7(5) . . ?
N7 C14 C15 115.7(4) . . ?
N7 C14 C13 109.8(4) . . ?
C13 C14 C15 134.5(5) . . ?
N8 C19 C20 112.0(4) . . ?
N8 C19 C18 120.8(4) . . ?
C18 C19 C20 127.2(4) . . ?
C8 C7 H7 120.8 . . ?
C6 C7 C8 118.5(4) . . ?
C6 C7 H7 120.8 . . ?
C32 N12 C31 117.1(6) . . ?
C15 C16 H16 120.5 . . ?
C17 C16 C15 119.0(5) . . ?
C17 C16 H16 120.5 . . ?
C4 C5 H5A 120.6 . . ?
C6 C5 C4 118.8(4) . . ?
C6 C5 H5A 120.6 . . ?
C34 N13 C33 117.0(5) . . ?
C25 C27 C28 120.6(6) . . ?
C25 C27 C26 116.9(5) . . ?
C26 C27 C28 122.5(5) . . ?
C19 C18 H18 120.8 . . ?
C19 C18 C17 118.4(4) . . ?
C17 C18 H18 120.8 . . ?
C9 C10 H10A 127.4 . . ?
C11 C10 C9 105.2(5) . . ?
C11 C10 H10A 127.4 . . ?
C30 C28 C27 121.5(6) . . ?
C29 C28 C27 122.1(5) . . ?
C29 C28 C30 116.4(5) . . ?
C23 N11 C24 117.5(5) . . ?
C41 N14 C42 117.3(6) . . ?
C36 C37 C38 121.8(6) . . ?
C35 C37 C38 120.7(5) . . ?
C35 C37 C36 117.5(5) . . ?
C7 C6 H6A 119.9 . . ?
C5 C6 C7 120.3(4) . . ?
C5 C6 H6A 119.9 . . ?
C16 C17 C18 119.9(4) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C27 C25 H25 120.2 . . ?
C23 C25 C27 119.5(6) . . ?
C23 C25 H25 120.2 . . ?
N5 C11 C10 108.4(4) . . ?
N5 C11 H11 125.8 . . ?
C10 C11 H11 125.8 . . ?
F5 B2 F6 108.9(4) . . ?
F5 B2 F8 109.9(5) . . ?
F8 B2 F6 109.1(5) . . ?
F7 B2 F6 108.8(5) . . ?
F7 B2 F5 110.8(5) . . ?
F7 B2 F8 109.3(5) . . ?
C40 C38 C37 121.6(5) . . ?
C39 C38 C37 122.3(6) . . ?
C39 C38 C40 116.0(6) . . ?
C27 C26 H26 120.1 . . ?
C24 C26 C27 119.7(6) . . ?
C24 C26 H26 120.1 . . ?
C14 C13 H13 128.1 . . ?
C12 C13 C14 103.8(5) . . ?
C12 C13 H13 128.1 . . ?
N6 C12 C13 109.2(5) . . ?
N6 C12 H12 125.4 . . ?
C13 C12 H12 125.4 . . ?
C3 C2 H2 128.1 . . ?
C1 C2 C3 103.8(5) . . ?
C1 C2 H2 128.1 . . ?
C37 C36 H36 120.4 . . ?
C34 C36 C37 119.3(6) . . ?
C34 C36 H36 120.4 . . ?
C38 C40 H40 119.5 . . ?
C42 C40 C38 121.0(7) . . ?
C42 C40 H40 119.5 . . ?
N14 C42 C40 121.2(8) . . ?
N14 C42 H42 119.4 . . ?
C40 C42 H42 119.4 . . ?
C28 C30 H30 120.1 . . ?
C32 C30 C28 119.9(7) . . ?
C32 C30 H30 120.1 . . ?
C28 C29 H29 119.9 . . ?
C28 C29 C31 120.2(6) . . ?
C31 C29 H29 119.9 . . ?
C37 C35 H35 120.2 . . ?
C37 C35 C33 119.6(5) . . ?
C33 C35 H35 120.2 . . ?
N12 C32 C30 124.0(6) . . ?
N12 C32 H32 118.0 . . ?
C30 C32 H32 118.0 . . ?
N11 C23 C25 123.5(6) . . ?
N11 C23 H23 118.2 . . ?
C25 C23 H23 118.2 . . ?
N11 C24 C26 122.7(7) . . ?
N11 C24 H24 118.7 . . ?
C26 C24 H24 118.7 . . ?
N12 C31 C29 122.4(7) . . ?
N12 C31 H31 118.8 . . ?
C29 C31 H31 118.8 . . ?
N1 C1 C2 108.9(5) . . ?
N1 C1 H1A 125.5 . . ?
C2 C1 H1A 125.5 . . ?
C20 C21 H21 127.5 . . ?
C22 C21 C20 104.9(5) . . ?
C22 C21 H21 127.5 . . ?
N13 C33 C35 122.7(6) . . ?
N13 C33 H33 118.6 . . ?
C35 C33 H33 118.6 . . ?
N13 C34 C36 123.8(6) . . ?
N13 C34 H34 118.1 . . ?
C36 C34 H34 118.1 . . ?
N10 C22 C21 108.3(5) . . ?
N10 C22 H22 125.9 . . ?
C21 C22 H22 125.9 . . ?
N14 C41 H41 117.4 . . ?
N14 C41 C39 125.2(7) . . ?
C39 C41 H41 117.4 . . ?
F3 B1 F4 110.5(6) . . ?
F3 B1 F1 110.6(6) . . ?
F4 B1 F1 107.9(6) . . ?
F2 B1 F3 111.1(7) . . ?
F2 B1 F4 109.7(7) . . ?
F2 B1 F1 107.0(7) . . ?
C38 C39 C41 119.2(8) . . ?
C38 C39 H39 120.4 . . ?
C41 C39 H39 120.4 . . ?
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 2.061(4) . ?
Fe1 N8 2.001(3) . ?
Fe1 N3 2.001(3) . ?
Fe1 N7 2.066(4) . ?
Fe1 N9 2.050(4) . ?
Fe1 N2 2.048(4) . ?
F6 B2 1.380(6) . ?
F5 B2 1.362(7) . ?
N4 N5 1.356(5) . ?
N4 C9 1.341(6) . ?
N8 C15 1.334(6) . ?
N8 C19 1.346(5) . ?
N3 C4 1.348(5) . ?
N3 C8 1.334(5) . ?
F8 B2 1.371(7) . ?
N7 N6 1.345(5) . ?
N7 C14 1.341(6) . ?
N9 N10 1.345(6) . ?
N9 C20 1.348(6) . ?
N2 N1 1.334(5) . ?
N2 C3 1.344(6) . ?
N5 H5 0.8600 . ?
N5 C11 1.337(8) . ?
F7 B2 1.354(7) . ?
C9 C8 1.461(6) . ?
C9 C10 1.388(6) . ?
C15 C14 1.455(6) . ?
C15 C16 1.384(6) . ?
N6 H6 0.8600 . ?
N6 C12 1.314(8) . ?
C4 C3 1.456(6) . ?
C4 C5 1.385(6) . ?
N1 H1 0.8600 . ?
N1 C1 1.327(9) . ?
C8 C7 1.392(6) . ?
F3 B1 1.355(8) . ?
N10 H10 0.8600 . ?
N10 C22 1.335(8) . ?
C3 C2 1.392(7) . ?
C20 C19 1.455(6) . ?
C20 C21 1.402(7) . ?
C14 C13 1.409(7) . ?
C19 C18 1.387(6) . ?
C7 H7 0.9300 . ?
C7 C6 1.382(7) . ?
F4 B1 1.357(8) . ?
N12 C32 1.318(10) . ?
N12 C31 1.344(9) . ?
C16 H16 0.9300 . ?
C16 C17 1.379(7) . ?
C5 H5A 0.9300 . ?
C5 C6 1.376(7) . ?
N13 C33 1.334(8) . ?
N13 C34 1.325(8) . ?
C27 C28 1.481(8) . ?
C27 C25 1.391(7) . ?
C27 C26 1.393(9) . ?
C18 H18 0.9300 . ?
C18 C17 1.391(8) . ?
C10 H10A 0.9300 . ?
C10 C11 1.369(8) . ?
C28 C30 1.391(7) . ?
C28 C29 1.378(9) . ?
F1 B1 1.360(8) . ?
N11 C23 1.322(9) . ?
N11 C24 1.345(9) . ?
N14 C42 1.360(10) . ?
N14 C41 1.299(11) . ?
C37 C38 1.473(8) . ?
C37 C36 1.387(8) . ?
C37 C35 1.368(8) . ?
C6 H6A 0.9300 . ?
C17 H17 0.9300 . ?
C25 H25 0.9300 . ?
C25 C23 1.371(9) . ?
C11 H11 0.9300 . ?
C38 C40 1.404(9) . ?
C38 C39 1.378(9) . ?
C26 H26 0.9300 . ?
C26 C24 1.370(8) . ?
C13 H13 0.9300 . ?
C13 C12 1.378(9) . ?
C12 H12 0.9300 . ?
C2 H2 0.9300 . ?
C2 C1 1.371(9) . ?
C36 H36 0.9300 . ?
C36 C34 1.370(9) . ?
C40 H40 0.9300 . ?
C40 C42 1.375(9) . ?
C42 H42 0.9300 . ?
F2 B1 1.300(8) . ?
C30 H30 0.9300 . ?
C30 C32 1.366(9) . ?
C29 H29 0.9300 . ?
C29 C31 1.386(9) . ?
C35 H35 0.9300 . ?
C35 C33 1.389(9) . ?
C32 H32 0.9300 . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C31 H31 0.9300 . ?
C1 H1A 0.9300 . ?
C21 H21 0.9300 . ?
C21 C22 1.369(10) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C22 H22 0.9300 . ?
C41 H41 0.9300 . ?
C41 C39 1.379(10) . ?
C39 H39 0.9300 . ?
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 N5 C11 -175.0(4) . . . . ?
Fe1 N4 C9 C8 -4.1(5) . . . . ?
Fe1 N4 C9 C10 176.0(3) . . . . ?
Fe1 N8 C15 C14 -0.1(5) . . . . ?
Fe1 N8 C15 C16 -179.9(3) . . . . ?
Fe1 N8 C19 C20 1.1(5) . . . . ?
Fe1 N8 C19 C18 -179.1(3) . . . . ?
Fe1 N3 C4 C3 1.4(5) . . . . ?
Fe1 N3 C4 C5 -179.0(3) . . . . ?
Fe1 N3 C8 C9 -0.1(5) . . . . ?
Fe1 N3 C8 C7 179.3(3) . . . . ?
Fe1 N7 N6 C12 -171.3(4) . . . . ?
Fe1 N7 C14 C15 -7.5(5) . . . . ?
Fe1 N7 C14 C13 173.3(3) . . . . ?
Fe1 N9 N10 C22 177.2(4) . . . . ?
Fe1 N9 C20 C19 1.9(5) . . . . ?
Fe1 N9 C20 C21 -177.7(4) . . . . ?
Fe1 N2 N1 C1 175.9(4) . . . . ?
Fe1 N2 C3 C4 2.7(5) . . . . ?
Fe1 N2 C3 C2 -177.5(4) . . . . ?
N4 N5 C11 C10 0.6(6) . . . . ?
N4 C9 C8 N3 2.8(5) . . . . ?
N4 C9 C8 C7 -176.6(4) . . . . ?
N4 C9 C10 C11 0.4(6) . . . . ?
N8 C15 C14 N7 5.1(6) . . . . ?
N8 C15 C14 C13 -176.0(5) . . . . ?
N8 C15 C16 C17 -0.8(7) . . . . ?
N8 C19 C18 C17 -1.0(7) . . . . ?
N3 C4 C3 N2 -2.6(6) . . . . ?
N3 C4 C3 C2 177.6(5) . . . . ?
N3 C4 C5 C6 -0.5(7) . . . . ?
N3 C8 C7 C6 -0.2(7) . . . . ?
N7 N6 C12 C13 0.7(7) . . . . ?
N7 C14 C13 C12 0.5(6) . . . . ?
N9 N10 C22 C21 -0.7(8) . . . . ?
N9 C20 C19 N8 -2.0(5) . . . . ?
N9 C20 C19 C18 178.3(4) . . . . ?
N9 C20 C21 C22 -0.3(7) . . . . ?
N2 N1 C1 C2 0.6(7) . . . . ?
N2 C3 C2 C1 0.8(7) . . . . ?
N5 N4 C9 C8 179.8(4) . . . . ?
N5 N4 C9 C10 0.0(5) . . . . ?
C9 N4 N5 C11 -0.3(6) . . . . ?
C9 C8 C7 C6 179.1(5) . . . . ?
C9 C10 C11 N5 -0.6(6) . . . . ?
C15 N8 C19 C20 -178.0(4) . . . . ?
C15 N8 C19 C18 1.7(6) . . . . ?
C15 C14 C13 C12 -178.5(5) . . . . ?
C15 C16 C17 C18 1.4(8) . . . . ?
N6 N7 C14 C15 179.1(4) . . . . ?
N6 N7 C14 C13 -0.1(5) . . . . ?
C4 N3 C8 C9 179.8(4) . . . . ?
C4 N3 C8 C7 -0.8(6) . . . . ?
C4 C3 C2 C1 -179.5(5) . . . . ?
C4 C5 C6 C7 -0.5(8) . . . . ?
N1 N2 C3 C4 179.7(4) . . . . ?
N1 N2 C3 C2 -0.5(6) . . . . ?
C8 N3 C4 C3 -178.4(4) . . . . ?
C8 N3 C4 C5 1.2(6) . . . . ?
C8 C9 C10 C11 -179.4(5) . . . . ?
C8 C7 C6 C5 0.9(8) . . . . ?
N10 N9 C20 C19 179.5(4) . . . . ?
N10 N9 C20 C21 -0.1(6) . . . . ?
C3 N2 N1 C1 -0.1(6) . . . . ?
C3 C4 C5 C6 179.0(5) . . . . ?
C3 C2 C1 N1 -0.8(7) . . . . ?
C20 N9 N10 C22 0.5(6) . . . . ?
C20 C19 C18 C17 178.6(5) . . . . ?
C20 C21 C22 N10 0.6(8) . . . . ?
C14 N7 N6 C12 -0.4(6) . . . . ?
C14 C15 C16 C17 179.4(5) . . . . ?
C14 C13 C12 N6 -0.7(7) . . . . ?
C19 N8 C15 C14 179.0(4) . . . . ?
C19 N8 C15 C16 -0.8(6) . . . . ?
C19 C20 C21 C22 -179.8(6) . . . . ?
C19 C18 C17 C16 -0.5(8) . . . . ?
C16 C15 C14 N7 -175.1(4) . . . . ?
C16 C15 C14 C13 3.8(9) . . . . ?
C5 C4 C3 N2 177.8(4) . . . . ?
C5 C4 C3 C2 -2.0(9) . . . . ?
C27 C28 C30 C32 -177.4(5) . . . . ?
C27 C28 C29 C31 176.9(5) . . . . ?
C27 C25 C23 N11 0.4(10) . . . . ?
C27 C26 C24 N11 -0.9(10) . . . . ?
C10 C9 C8 N3 -177.4(5) . . . . ?
C10 C9 C8 C7 3.2(8) . . . . ?
C28 C27 C25 C23 -177.3(5) . . . . ?
C28 C27 C26 C24 177.6(5) . . . . ?
C28 C30 C32 N12 -0.3(10) . . . . ?
C28 C29 C31 N12 1.4(10) . . . . ?
N14 C41 C39 C38 2.5(13) . . . . ?
C37 C38 C40 C42 -177.4(5) . . . . ?
C37 C38 C39 C41 176.6(6) . . . . ?
C37 C36 C34 N13 -0.9(10) . . . . ?
C37 C35 C33 N13 0.8(9) . . . . ?
C25 C27 C28 C30 -150.6(6) . . . . ?
C25 C27 C28 C29 29.6(7) . . . . ?
C25 C27 C26 C24 -2.4(8) . . . . ?
C38 C37 C36 C34 178.0(5) . . . . ?
C38 C37 C35 C33 -178.0(5) . . . . ?
C38 C40 C42 N14 -0.7(10) . . . . ?
C26 C27 C28 C30 29.4(7) . . . . ?
C26 C27 C28 C29 -150.4(6) . . . . ?
C26 C27 C25 C23 2.7(8) . . . . ?
C36 C37 C38 C40 -25.2(8) . . . . ?
C36 C37 C38 C39 154.9(6) . . . . ?
C36 C37 C35 C33 2.0(8) . . . . ?
C40 C38 C39 C41 -3.2(10) . . . . ?
C42 N14 C41 C39 -0.6(12) . . . . ?
C30 C28 C29 C31 -2.9(8) . . . . ?
C29 C28 C30 C32 2.4(8) . . . . ?
C35 C37 C38 C40 154.8(6) . . . . ?
C35 C37 C38 C39 -25.1(8) . . . . ?
C35 C37 C36 C34 -2.0(8) . . . . ?
C32 N12 C31 C29 0.8(10) . . . . ?
C23 N11 C24 C26 3.9(9) . . . . ?
C24 N11 C23 C25 -3.6(10) . . . . ?
C31 N12 C32 C30 -1.4(10) . . . . ?
C21 C20 C19 N8 177.5(6) . . . . ?
C21 C20 C19 C18 -2.2(9) . . . . ?
C33 N13 C34 C36 3.6(10) . . . . ?
C34 N13 C33 C35 -3.6(9) . . . . ?
C41 N14 C42 C40 -0.3(10) . . . . ?
C39 C38 C40 C42 2.5(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
-3.9556 -9.2155 -3.2815 0.9620 -0.1263 -0.2421
4.2925 -6.9517 6.4970 -0.1134 -0.8718 0.4765
-4.2135 -0.8710 12.3907 -0.0657 -0.4916 -0.8683
2.5686 10.1849 5.3661 -0.9915 0.1298 -0.0089
4.2594 -6.5955 -9.1482 0.4052 -0.0542 0.9126
0.9137 4.7221 -13.7052 0.1172 0.8984 0.4232
1.4826 -6.3404 11.8487 -0.1297 -0.9907 -0.0404
-3.7842 6.9882 -7.8245 0.1198 0.9191 -0.3754
-5.0517 2.7951 -7.6801 0.4624 0.7548 -0.4653
4.5077 -2.5771 9.2364 -0.4895 -0.7993 0.3486
3.3628 -1.2136 -13.4645 0.2915 0.4780 0.8286
0.5458 12.1977 1.6115 -0.8374 0.5120 -0.1915
4.6913 -7.1519 -7.1142 0.3376 -0.2051 0.9187
2.8288 -10.7112 3.0234 0.3415 -0.8210 0.4576
-0.1398 -10.5071 7.7609 0.3827 -0.9223 -0.0546
-1.4621 10.9967 -5.4764 -0.3742 0.9007 -0.2207
-5.8373 -0.0956 -5.5166 0.6212 0.5324 -0.5751
0.2860 -12.3044 0.6454 0.7056 -0.6690 0.2336
