#------------------------------------------------------------------------------
#$Date: 2023-10-30 01:49:56 +0200 (Mon, 30 Oct 2023) $
#$Revision: 287163 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/43/7714339.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_7714339
loop_
_publ_author_name
'Díaz-Torres, Raúl'
'Gómez-Coca, Silvia'
'Ruiz, Eliseo'
'Harding, Phimphaka'
'Harding, David J.'
_publ_section_title
;
 Improving Spin Crossover Characteristics in Heteroleptic
 [FeIII(qsal-5-I)(qsal-5-OMe)]A Complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02503A
_journal_year                    2023
_chemical_formula_moiety         'C33 H23 Fe I N4 O3, B F4, 1.1[CH4O]'
_chemical_formula_sum            'C34.1 H27.4 B F4 Fe I N4 O4.1'
_chemical_formula_weight         828.36
_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             2023-09-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-13 deposited with the CCDC.	2023-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                104.192(5)
_cell_angle_beta                 99.345(4)
_cell_angle_gamma                94.337(4)
_cell_formula_units_Z            2
_cell_length_a                   10.8316(5)
_cell_length_b                   12.4983(6)
_cell_length_c                   12.8260(8)
_cell_measurement_reflns_used    8625
_cell_measurement_temperature    300.00(10)
_cell_measurement_theta_max      66.5240
_cell_measurement_theta_min      3.6000
_cell_volume                     1648.87(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      300.00(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.997
_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  78.00   0.50    3.00    --   40.91-106.00 155.00  174
  2  ω     29.00 107.00   0.50   11.50    --   96.59-106.00 155.00  156
  3  ω     83.00 157.00   0.50   11.50    --   96.59 106.00-105.00  148
  4  ω    -78.00   9.00   0.50    3.00    --  -40.91 106.00-105.00  174
  5  ω   -104.00 -25.00   0.50    3.00    --  -40.91 -50.00 120.00  158
  6  ω   -104.00 -25.00   0.50    3.00    --  -40.91 -50.00-180.00  158
  7  ω    -50.00  27.00   0.50    3.00    --  -40.91  25.00 150.00  154
  8  ω    -53.00  23.00   0.50    3.00    --  -40.91  37.00   0.00  152
  9  ω   -105.00 -29.00   0.50    3.00    --  -40.91 -37.00 -60.00  152
 10  ω     16.00  42.00   0.50    3.00    --   40.91  76.00  56.38   52
 11  ω     29.00 105.00   0.50    3.00    --   40.91  37.00-150.00  152
 12  ω     19.00 114.00   0.50    3.00    --   40.91  12.00  60.00  190
 13  ω     16.00  42.00   0.50    3.00    --   40.91  79.00  26.46   52
 14  ω     16.00  42.00   0.50    3.00    --   40.91  80.00 -42.19   52
 15  ω     14.00  97.00   0.50    3.00    --   40.91-138.00 -30.00  166
 16  ω     16.00  42.00   0.50    3.00    --   40.91  78.00  59.30   52
 17  ω     15.00  42.00   0.50    3.00    --   40.91  82.00-118.48   54
 18  ω    -22.00  57.00   0.50    3.00    --   40.91 -50.00   0.00  158
 19  ω     15.00  42.00   0.50    3.00    --   40.91  81.00 -73.30   54
 20  ω     32.00 109.00   0.50    3.00    --   40.91  25.00 120.00  154
 21  ω     16.00  42.00   0.50    3.00    --   40.91  80.00 119.17   52
 22  ω     16.00  42.00   0.50    3.00    --   40.91  76.00   1.93   52
 23  ω     16.00  42.00   0.50    3.00    --   40.91  78.00-145.78   52
 24  ω     15.00  42.00   0.50    3.00    --   40.91  77.00 167.78   54
 25  ω     31.00 106.00   0.50   11.50    --   96.59 -33.00  60.00  150
 26  ω     84.00 157.00   0.50   11.50    --   96.59  42.00 -60.00  146
 27  ω     32.00 109.00   0.50   11.50    --   96.59-117.00 -60.00  154
 28  ω     33.00 126.00   0.50   11.50    --   96.59-144.00-150.00  186
 29  ω     27.00 105.00   0.50   11.50    --   96.59 -96.00 -90.00  156
 30  ω     33.00 115.00   0.50   11.50    --   96.59 -59.00 120.00  164
 31  ω     88.00 157.00   0.50   11.50    --   96.59  25.00  90.00  138
 32  ω     32.00 109.00   0.50   11.50    --   96.59-117.00 120.00  154
 33  ω     32.00 122.00   0.50   11.50    --   96.59 -77.00 150.00  180
 34  ω     78.00 157.00   0.50   11.50    --   96.59  59.00   0.00  158
 35  ω     78.00 157.00   0.50   11.50    --   96.59  59.00-120.00  158
 36  ω     77.00 157.00   0.50   11.50    --   96.59  63.00 -37.32  160
 37  ω     27.00 105.00   0.50   11.50    --   96.59 -96.00-150.00  156
 38  ω     29.00 105.00   0.50   11.50    --   96.59 -25.00  90.00  152
 39  ω     33.00 115.00   0.50   11.50    --   96.59 -59.00  30.00  164
 40  ω     33.00 115.00   0.50   11.50    --   96.59 -59.00-120.00  164
 41  ω     32.00 109.00   0.50   11.50    --   96.59-117.00   0.00  154
 42  ω     32.00 122.00   0.50   11.50    --   96.59 -77.00   0.00  180
 43  ω     75.00 157.00   0.50   11.50    --   96.59  68.00  90.00  164
 44  ω     81.00 157.00   0.50   11.50    --   96.59  50.00  60.00  152
 45  ω     32.00 109.00   0.50   11.50    --   96.59-117.00  60.00  154
 46  ω     80.00 157.00   0.50   11.50    --   96.59  51.00  22.20  154
 47  ω     32.00 122.00   0.50   11.50    --   96.59 -77.00 -60.00  180
 48  ω     81.00 157.00   0.50   11.50    --   96.59 117.00   0.00  152
 49  ω     84.00 157.00   0.50   11.50    --   96.59  96.00-180.00  146
 50  ω    -50.00  27.00   0.50    3.00    --  -40.91  25.00  60.00  154
 51  ω   -104.00 -21.00   0.50    3.00    --  -40.91 -63.00   0.00  166
 52  ω   -104.00 -21.00   0.50    3.00    --  -40.91 -63.00 -90.00  166
 53  ω   -104.00 -25.00   0.50    3.00    --  -40.91 -50.00-150.00  158
 54  ω   -104.00 -21.00   0.50    3.00    --  -40.91 -63.00  60.00  166
 55  ω   -114.00 -19.00   0.50    3.00    --  -40.91 -12.00  90.00  190
 56  ω    -22.00  57.00   0.50    3.00    --   40.91 -50.00 120.00  158
 57  ω     16.00  42.00   0.50    3.00    --   40.91  80.00 -84.59   52
 58  ω     15.00  42.00   0.50    3.00    --   40.91  82.00 139.34   54
 59  ω     15.00  42.00   0.50    3.00    --   40.91  81.00 165.48   54
 60  ω     16.00  42.00   0.50    3.00    --   40.91  78.00  88.12   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24963
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.685
_diffrn_reflns_theta_min         3.619
_exptl_absorpt_coefficient_mu    11.615
_exptl_absorpt_correction_T_max  0.584
_exptl_absorpt_correction_T_min  0.180
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull dark black'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_description       block
_exptl_crystal_F_000             826
_exptl_crystal_size_max          0.211
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.435
_refine_diff_density_min         -1.057
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         5991
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0769
_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)+(0.1713P)²+0.2822P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2366
_refine_ls_wR_factor_ref         0.2512
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4522
_reflns_number_total             5991
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt02503a2.cif
_cod_data_source_block           rdt133-300k
_cod_original_formula_sum        'C34.10 H27.40 B F4 Fe I N4 O4.10'
_cod_database_code               7714339
_shelx_shelxl_version_number     2018/3
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O3-C13
 1.38 with sigma of 0.02
 O3-C33
 1.42 with sigma of 0.02
 O4-C34
 1.42 with sigma of 0.02
 O4-C29
 1.38 with sigma of 0.02
 C11-C12 \\sim C11-C12A
 with sigma of 0.02
 C12-C13 \\sim C12A-C13A
 with sigma of 0.02
 C13-C14 \\sim C13A-C14A
 with sigma of 0.02
 C13-O3 \\sim C13A-O3
 with sigma of 0.02
 C13-I1 \\sim C13A-I1
 with sigma of 0.02
 C14-C15 \\sim C14A-C15A
 with sigma of 0.02
 C15-C16 \\sim C15A-C16
 with sigma of 0.02
 C11-C13 \\sim C11-C13A
 with sigma of 0.04
 C12-C14 \\sim C12A-C14A
 with sigma of 0.04
 C12-O3 \\sim C12A-O3
 with sigma of 0.04
 C12-I1 \\sim C12A-I1
 with sigma of 0.04
 C13-C15 \\sim C13A-C15A
 with sigma of 0.04
 C14-C16 \\sim C14A-C16
 with sigma of 0.04
 C14-O3 \\sim C14A-O3
 with sigma of 0.04
 C14-I1 \\sim C14A-I1
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uiso(O3) = Uiso(C33)
4. Rigid body (RIGU) restrains
 C29, O4, C34
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C13, O3, C33
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: C12(0.4) H12(0.4) C13(0.4) C14(0.4) H14(0.4) C15(0.6) H15(0.6)
 I2(0.4) O3(0.4) C33(0.4) H33A(0.4) H33B(0.4) H33C(0.4) I1(0.6) O4(0.6)
 C34(0.6) H34A(0.6) H34B(0.6) H34C(0.6) C12A(0.6) H12A(0.6) C13A(0.6) C14A(0.6)
 H14A(0.6) C15A(0.4) H15A(0.4)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C10(H10), C12(H12), C14(H14),
 C15(H15), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C26(H26),
  C28(H28), C30(H30), C31(H31), C12A(H12A), C14A(H14A), C15A(H15A)
6.b Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 40 electrons were 
found in a volume of 188Å³ in 1 void per unit cell. 
This is consistent with the presence of 
1.1[CH4O] per Asymmetric Unit 
which account for 40 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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
;
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 0.48115(7) 0.72217(5) 0.37464(6) 0.0640(3) Uani 1 1 d . . . . .
O1 O 0.3731(4) 0.7515(3) 0.4783(3) 0.0816(9) Uani 1 1 d . . . . .
O2 O 0.6325(4) 0.7404(3) 0.4776(3) 0.0853(10) Uani 1 1 d . . . . .
N1 N 0.5740(4) 0.6568(3) 0.2446(4) 0.0719(10) Uani 1 1 d . . . . .
N2 N 0.4453(4) 0.5537(3) 0.3556(3) 0.0669(9) Uani 1 1 d . . . . .
N3 N 0.3326(4) 0.7316(3) 0.2519(3) 0.0692(9) Uani 1 1 d . . . . .
N4 N 0.5163(4) 0.8845(3) 0.3673(3) 0.0670(9) Uani 1 1 d . . . . .
C1 C 0.6340(6) 0.7122(5) 0.1904(5) 0.0869(15) Uani 1 1 d . . . . .
H1 H 0.638272 0.789344 0.211085 0.104 Uiso 1 1 calc R U . . .
C2 C 0.6922(7) 0.6647(6) 0.1038(6) 0.1018(19) Uani 1 1 d . . . . .
H2 H 0.732076 0.708223 0.066876 0.122 Uiso 1 1 calc R U . . .
C3 C 0.6883(7) 0.5513(7) 0.0755(6) 0.104(2) Uani 1 1 d . . . . .
H3 H 0.727694 0.516669 0.019207 0.125 Uiso 1 1 calc R U . . .
C4 C 0.6260(6) 0.4880(5) 0.1300(5) 0.0897(16) Uani 1 1 d . . . . .
C5 C 0.6146(8) 0.3697(6) 0.1062(7) 0.115(2) Uani 1 1 d . . . . .
H5 H 0.649749 0.329815 0.049378 0.138 Uiso 1 1 calc R U . . .
C6 C 0.5525(7) 0.3139(6) 0.1657(7) 0.110(2) Uani 1 1 d . . . . .
H6 H 0.549483 0.237022 0.151085 0.132 Uiso 1 1 calc R U . . .
C7 C 0.4935(6) 0.3715(5) 0.2483(6) 0.0943(17) Uani 1 1 d . . . . .
H7 H 0.448961 0.332256 0.286129 0.113 Uiso 1 1 calc R U . . .
C8 C 0.5009(5) 0.4846(4) 0.2736(4) 0.0720(12) Uani 1 1 d . . . . .
C9 C 0.5666(5) 0.5433(4) 0.2155(4) 0.0756(13) Uani 1 1 d . . . . .
C10 C 0.3786(5) 0.5090(4) 0.4139(4) 0.0685(11) Uani 1 1 d . . . . .
H10 H 0.374536 0.432374 0.402811 0.082 Uiso 1 1 calc R U . . .
C11 C 0.3129(5) 0.5656(4) 0.4912(4) 0.0700(11) Uani 1 1 d D . . . .
C12 C 0.2476(17) 0.5060(14) 0.5547(16) 0.072(6) Uiso 0.4 1 d D . P A 1
H12 H 0.254794 0.430840 0.546404 0.087 Uiso 0.4 1 calc R U P A 1
C13 C 0.178(2) 0.5559(16) 0.624(2) 0.094(10) Uiso 0.4 1 d D . P A 1
C14 C 0.1837(19) 0.6718(15) 0.6564(16) 0.087(6) Uiso 0.4 1 d D . P A 1
H14 H 0.144607 0.706856 0.712744 0.105 Uiso 0.4 1 calc R U P A 1
C15 C 0.2191(13) 0.7198(13) 0.5850(11) 0.093(5) Uiso 0.6 1 d D . P A 2
H15 H 0.204166 0.793676 0.596164 0.112 Uiso 0.6 1 calc R U P A 2
C16 C 0.3069(5) 0.6834(4) 0.5199(4) 0.0696(11) Uani 1 1 d D . . . .
C17 C 0.2429(5) 0.6496(5) 0.1949(4) 0.0812(14) Uani 1 1 d . . . . .
H17 H 0.246470 0.579297 0.206585 0.097 Uiso 1 1 calc R U . . .
C18 C 0.1433(6) 0.6659(6) 0.1178(5) 0.0916(17) Uani 1 1 d . . . . .
H18 H 0.080739 0.607830 0.080505 0.110 Uiso 1 1 calc R U . . .
C19 C 0.1397(7) 0.7689(7) 0.0983(6) 0.112(2) Uani 1 1 d . . . . .
H19 H 0.075573 0.780497 0.045962 0.134 Uiso 1 1 calc R U . . .
C20 C 0.2308(6) 0.8551(6) 0.1561(5) 0.0920(16) Uani 1 1 d . . . . .
C21 C 0.2346(8) 0.9661(7) 0.1440(7) 0.117(2) Uani 1 1 d . . . . .
H21 H 0.172147 0.982754 0.093610 0.140 Uiso 1 1 calc R U . . .
C22 C 0.3270(8) 1.0478(7) 0.2043(8) 0.117(2) Uani 1 1 d . . . . .
H22 H 0.326549 1.119508 0.195526 0.140 Uiso 1 1 calc R U . . .
C23 C 0.4230(6) 1.0238(5) 0.2796(6) 0.0936(17) Uani 1 1 d . . . . .
H23 H 0.486477 1.079918 0.319737 0.112 Uiso 1 1 calc R U . . .
C24 C 0.4252(5) 0.9195(4) 0.2950(4) 0.0727(12) Uani 1 1 d . . . . .
C25 C 0.3285(5) 0.8340(4) 0.2326(4) 0.0736(12) Uani 1 1 d . . . . .
C26 C 0.6141(5) 0.9542(4) 0.4257(4) 0.0697(11) Uani 1 1 d . . . . .
H26 H 0.617585 1.026813 0.419195 0.084 Uiso 1 1 calc R U . . .
C27 C 0.7144(5) 0.9294(4) 0.4974(4) 0.0735(12) Uani 1 1 d . . . . .
C28 C 0.8141(6) 1.0170(5) 0.5504(5) 0.0864(15) Uani 1 1 d . . . . .
H28 H 0.811190 1.086237 0.536084 0.104 Uiso 1 1 calc R U . . .
C29 C 0.9128(6) 0.9996(5) 0.6213(6) 0.0960(17) Uani 1 1 d D . . . .
C30 C 0.9204(7) 0.8986(6) 0.6445(7) 0.113(2) Uani 1 1 d . . . . .
H30 H 0.989526 0.887788 0.692551 0.136 Uiso 1 1 calc R U . . .
C31 C 0.8236(6) 0.8121(5) 0.5952(6) 0.0989(19) Uani 1 1 d . . . . .
H31 H 0.827649 0.744080 0.612064 0.119 Uiso 1 1 calc R U . . .
C32 C 0.7219(6) 0.8262(4) 0.5219(5) 0.0790(13) Uani 1 1 d . . . . .
I2 I 1.05044(19) 1.1370(2) 0.6954(2) 0.1730(10) Uani 0.4 1 d . . P B 1
O3 O 0.1367(17) 0.4737(13) 0.6691(13) 0.134(4) Uiso 0.4 1 d D . P A 1
C33 C 0.082(2) 0.528(2) 0.7669(19) 0.134(4) Uiso 0.4 1 d D . P A 1
H33A H 0.136875 0.593592 0.809492 0.201 Uiso 0.4 1 calc R U P A 1
H33B H 0.073233 0.477240 0.811064 0.201 Uiso 0.4 1 calc R U P A 1
H33C H 0.000650 0.548708 0.742442 0.201 Uiso 0.4 1 calc R U P A 1
I1 I 0.05015(11) 0.45669(10) 0.68033(11) 0.1403(5) Uani 0.6 1 d . . P A 2
O4 O 1.0080(9) 1.0731(7) 0.6730(8) 0.119(3) Uani 0.6 1 d D . P B 2
C34 C 1.0106(11) 1.1827(9) 0.6438(11) 0.097(3) Uani 0.6 1 d D . P B 2
H34A H 1.001822 1.169845 0.565918 0.145 Uiso 0.6 1 calc R U P B 2
H34B H 1.089159 1.227474 0.679040 0.145 Uiso 0.6 1 calc R U P B 2
H34C H 0.942301 1.220556 0.667905 0.145 Uiso 0.6 1 calc R U P B 2
F1 F 0.2036(5) 0.3493(5) 0.2358(4) 0.1465(18) Uani 1 1 d . . . . .
F2 F 0.0206(4) 0.2510(5) 0.1520(4) 0.1313(15) Uani 1 1 d . . . . .
F3 F 0.1092(4) 0.3781(3) 0.0799(4) 0.1108(11) Uani 1 1 d . . . . .
F4 F 0.1903(7) 0.2194(4) 0.0773(5) 0.160(2) Uani 1 1 d . . . . .
B1 B 0.1326(7) 0.3011(6) 0.1346(6) 0.0881(18) Uani 1 1 d . . . . .
C12A C 0.2347(12) 0.4976(10) 0.5330(12) 0.077(5) Uiso 0.6 1 d D . P A 2
H12A H 0.231751 0.420768 0.509719 0.093 Uiso 0.6 1 calc R U P A 2
C13A C 0.1651(15) 0.5420(12) 0.6053(14) 0.090(6) Uiso 0.6 1 d D . P A 2
C14A C 0.1547(12) 0.6553(10) 0.6327(10) 0.079(3) Uiso 0.6 1 d D . P A 2
H14A H 0.104880 0.685491 0.682409 0.095 Uiso 0.6 1 calc R U P A 2
C15A C 0.2479(16) 0.7313(14) 0.6030(12) 0.067(4) Uiso 0.4 1 d D . P A 1
H15A H 0.252054 0.808434 0.623739 0.081 Uiso 0.4 1 calc R U P A 1
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'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 5 -2 0.0722
-2 -3 5 0.1087
-3 5 2 0.0986
-1 0 -5 0.0205
1 -5 -4 0.0773
1 0 5 0.0341
-5 4 1 0.1061
0 -1 -5 0.0348
-1 -1 -5 0.0247
-5 1 3 0.0936
0 -5 2 0.0970
5 -1 -3 0.0895
0 0 -1 0.0234
-5 -1 -3 0.0640
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 N1 167.36(16) . . ?
O1 Fe1 N2 91.06(16) . . ?
O1 Fe1 N3 89.41(17) . . ?
O1 Fe1 N4 96.01(15) . . ?
O2 Fe1 O1 96.41(18) . . ?
O2 Fe1 N1 91.01(17) . . ?
O2 Fe1 N2 94.81(15) . . ?
O2 Fe1 N3 167.49(16) . . ?
O2 Fe1 N4 90.07(16) . . ?
N2 Fe1 N1 78.08(16) . . ?
N2 Fe1 N3 96.15(15) . . ?
N2 Fe1 N4 170.91(16) . . ?
N3 Fe1 N1 85.38(16) . . ?
N4 Fe1 N1 94.20(16) . . ?
N4 Fe1 N3 78.28(16) . . ?
C16 O1 Fe1 131.2(3) . . ?
C32 O2 Fe1 132.2(3) . . ?
C1 N1 Fe1 127.2(4) . . ?
C1 N1 C9 118.5(5) . . ?
C9 N1 Fe1 114.2(4) . . ?
C8 N2 Fe1 115.6(3) . . ?
C10 N2 Fe1 124.2(3) . . ?
C10 N2 C8 120.2(4) . . ?
C17 N3 Fe1 126.6(4) . . ?
C17 N3 C25 118.7(4) . . ?
C25 N3 Fe1 114.7(3) . . ?
C24 N4 Fe1 115.4(3) . . ?
C26 N4 Fe1 124.4(3) . . ?
C26 N4 C24 120.2(4) . . ?
N1 C1 H1 117.5 . . ?
N1 C1 C2 124.9(6) . . ?
C2 C1 H1 117.5 . . ?
C1 C2 H2 121.3 . . ?
C3 C2 C1 117.3(6) . . ?
C3 C2 H2 121.3 . . ?
C2 C3 H3 119.8 . . ?
C2 C3 C4 120.3(6) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 C5 125.0(6) . . ?
C3 C4 C9 118.5(6) . . ?
C9 C4 C5 116.5(6) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 C4 120.9(6) . . ?
C6 C5 H5 119.5 . . ?
C5 C6 H6 119.6 . . ?
C5 C6 C7 120.7(6) . . ?
C7 C6 H6 119.6 . . ?
C6 C7 H7 119.8 . . ?
C8 C7 C6 120.4(7) . . ?
C8 C7 H7 119.8 . . ?
C7 C8 N2 126.3(5) . . ?
C7 C8 C9 119.6(5) . . ?
C9 C8 N2 114.0(4) . . ?
N1 C9 C4 120.4(5) . . ?
N1 C9 C8 118.0(5) . . ?
C8 C9 C4 121.7(5) . . ?
N2 C10 H10 116.9 . . ?
N2 C10 C11 126.2(4) . . ?
C11 C10 H10 116.9 . . ?
C10 C11 C12 120.4(8) . . ?
C10 C11 C16 125.5(5) . . ?
C10 C11 C12A 115.4(6) . . ?
C16 C11 C12 114.0(8) . . ?
C12A C11 C16 118.6(6) . . ?
C11 C12 H12 119.0 . . ?
C13 C12 C11 122.0(13) . . ?
C13 C12 H12 119.0 . . ?
C12 C13 C14 121.3(15) . . ?
C12 C13 O3 104.0(14) . . ?
O3 C13 C14 132.6(17) . . ?
C13 C14 H14 121.0 . . ?
C15A C14 C13 117.9(14) . . ?
C15A C14 H14 121.0 . . ?
C16 C15 H15 117.8 . . ?
C14A C15 H15 117.8 . . ?
C14A C15 C16 124.4(13) . . ?
O1 C16 C11 121.6(4) . . ?
O1 C16 C15 122.5(8) . . ?
O1 C16 C15A 117.1(8) . . ?
C15 C16 C11 115.7(8) . . ?
C15A C16 C11 120.6(9) . . ?
N3 C17 H17 118.9 . . ?
N3 C17 C18 122.2(6) . . ?
C18 C17 H17 118.9 . . ?
C17 C18 H18 120.5 . . ?
C19 C18 C17 118.9(6) . . ?
C19 C18 H18 120.5 . . ?
C18 C19 H19 120.0 . . ?
C18 C19 C20 120.1(6) . . ?
C20 C19 H19 120.0 . . ?
C19 C20 C21 124.7(6) . . ?
C19 C20 C25 118.5(6) . . ?
C25 C20 C21 116.8(6) . . ?
C20 C21 H21 119.1 . . ?
C22 C21 C20 121.8(6) . . ?
C22 C21 H21 119.1 . . ?
C21 C22 H22 120.1 . . ?
C21 C22 C23 119.9(6) . . ?
C23 C22 H22 120.1 . . ?
C22 C23 H23 119.3 . . ?
C24 C23 C22 121.3(6) . . ?
C24 C23 H23 119.3 . . ?
N4 C24 C25 114.2(4) . . ?
C23 C24 N4 126.8(5) . . ?
C23 C24 C25 119.0(5) . . ?
N3 C25 C20 121.5(5) . . ?
N3 C25 C24 117.2(4) . . ?
C20 C25 C24 121.2(5) . . ?
N4 C26 H26 116.9 . . ?
N4 C26 C27 126.2(4) . . ?
C27 C26 H26 116.9 . . ?
C26 C27 C28 117.1(5) . . ?
C32 C27 C26 124.9(5) . . ?
C32 C27 C28 118.0(5) . . ?
C27 C28 H28 119.8 . . ?
C29 C28 C27 120.4(5) . . ?
C29 C28 H28 119.8 . . ?
C28 C29 C30 121.5(6) . . ?
C28 C29 I2 116.1(5) . . ?
C30 C29 I2 122.4(5) . . ?
O4 C29 C28 125.2(7) . . ?
O4 C29 C30 113.3(6) . . ?
C29 C30 H30 120.3 . . ?
C29 C30 C31 119.4(6) . . ?
C31 C30 H30 120.3 . . ?
C30 C31 H31 119.5 . . ?
C32 C31 C30 120.9(6) . . ?
C32 C31 H31 119.5 . . ?
O2 C32 C27 122.2(5) . . ?
O2 C32 C31 118.0(5) . . ?
C31 C32 C27 119.8(5) . . ?
C13 O3 C33 107.7(16) . . ?
O3 C33 H33A 109.5 . . ?
O3 C33 H33B 109.5 . . ?
O3 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C29 O4 C34 115.8(8) . . ?
O4 C34 H34A 109.5 . . ?
O4 C34 H34B 109.5 . . ?
O4 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
F1 B1 F2 106.2(6) . . ?
F3 B1 F1 110.3(6) . . ?
F3 B1 F2 110.7(6) . . ?
F3 B1 F4 111.0(6) . . ?
F4 B1 F1 111.0(6) . . ?
F4 B1 F2 107.5(6) . . ?
C11 C12A H12A 119.5 . . ?
C13A C12A C11 120.9(10) . . ?
C13A C12A H12A 119.5 . . ?
C12A C13A I1 126.6(10) . . ?
C12A C13A C14A 121.6(11) . . ?
C14A C13A I1 111.6(8) . . ?
C15 C14A C13A 117.8(10) . . ?
C15 C14A H14A 121.1 . . ?
C13A C14A H14A 121.1 . . ?
C14 C15A C16 123.1(14) . . ?
C14 C15A H15A 118.5 . . ?
C16 C15A H15A 118.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 1.898(4) . ?
Fe1 O2 1.891(4) . ?
Fe1 N1 2.113(4) . ?
Fe1 N2 2.059(4) . ?
Fe1 N3 2.092(4) . ?
Fe1 N4 2.064(4) . ?
O1 C16 1.333(6) . ?
O2 C32 1.334(7) . ?
N1 C1 1.303(7) . ?
N1 C9 1.367(7) . ?
N2 C8 1.433(6) . ?
N2 C10 1.308(7) . ?
N3 C17 1.335(7) . ?
N3 C25 1.363(6) . ?
N4 C24 1.411(6) . ?
N4 C26 1.313(6) . ?
C1 H1 0.9300 . ?
C1 C2 1.394(9) . ?
C2 H2 0.9300 . ?
C2 C3 1.369(10) . ?
C3 H3 0.9300 . ?
C3 C4 1.384(10) . ?
C4 C5 1.426(10) . ?
C4 C9 1.421(8) . ?
C5 H5 0.9300 . ?
C5 C6 1.370(12) . ?
C6 H6 0.9300 . ?
C6 C7 1.402(9) . ?
C7 H7 0.9300 . ?
C7 C8 1.364(7) . ?
C8 C9 1.401(8) . ?
C10 H10 0.9300 . ?
C10 C11 1.397(7) . ?
C11 C12 1.458(13) . ?
C11 C16 1.437(7) . ?
C11 C12A 1.410(11) . ?
C12 H12 0.9300 . ?
C12 C13 1.331(16) . ?
C13 C14 1.399(17) . ?
C13 O3 1.374(16) . ?
C14 H14 0.9300 . ?
C14 C15A 1.35(2) . ?
C15 H15 0.9300 . ?
C15 C16 1.395(11) . ?
C15 C14A 1.344(18) . ?
C16 C15A 1.367(12) . ?
C17 H17 0.9300 . ?
C17 C18 1.402(8) . ?
C18 H18 0.9300 . ?
C18 C19 1.373(10) . ?
C19 H19 0.9300 . ?
C19 C20 1.376(10) . ?
C20 C21 1.431(10) . ?
C20 C25 1.409(7) . ?
C21 H21 0.9300 . ?
C21 C22 1.360(11) . ?
C22 H22 0.9300 . ?
C22 C23 1.403(10) . ?
C23 H23 0.9300 . ?
C23 C24 1.368(7) . ?
C24 C25 1.420(8) . ?
C26 H26 0.9300 . ?
C26 C27 1.410(7) . ?
C27 C28 1.430(8) . ?
C27 C32 1.405(7) . ?
C28 H28 0.9300 . ?
C28 C29 1.353(9) . ?
C29 C30 1.373(10) . ?
C29 I2 2.104(6) . ?
C29 O4 1.297(10) . ?
C30 H30 0.9300 . ?
C30 C31 1.394(10) . ?
C31 H31 0.9300 . ?
C31 C32 1.379(8) . ?
O3 C33 1.508(17) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
I1 C13A 2.075(12) . ?
O4 C34 1.505(13) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
F1 B1 1.364(8) . ?
F2 B1 1.399(9) . ?
F3 B1 1.340(8) . ?
F4 B1 1.360(9) . ?
C12A H12A 0.9300 . ?
C12A C13A 1.332(13) . ?
C13A C14A 1.391(14) . ?
C14A H14A 0.9300 . ?
C15A H15A 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 O1 C16 C11 2.5(8) . . . . ?
Fe1 O1 C16 C15 -171.3(8) . . . . ?
Fe1 O1 C16 C15A 173.0(9) . . . . ?
Fe1 O2 C32 C27 1.7(9) . . . . ?
Fe1 O2 C32 C31 -179.2(5) . . . . ?
Fe1 N1 C1 C2 -179.0(5) . . . . ?
Fe1 N1 C9 C4 -179.3(4) . . . . ?
Fe1 N1 C9 C8 -0.4(6) . . . . ?
Fe1 N2 C8 C7 178.1(5) . . . . ?
Fe1 N2 C8 C9 -2.9(5) . . . . ?
Fe1 N2 C10 C11 5.5(7) . . . . ?
Fe1 N3 C17 C18 176.7(4) . . . . ?
Fe1 N3 C25 C20 -177.0(4) . . . . ?
Fe1 N3 C25 C24 1.4(6) . . . . ?
Fe1 N4 C24 C23 176.4(5) . . . . ?
Fe1 N4 C24 C25 -4.6(6) . . . . ?
Fe1 N4 C26 C27 4.0(7) . . . . ?
O1 Fe1 O2 C32 -97.1(5) . . . . ?
O1 C16 C15A C14 -176.2(15) . . . . ?
O2 Fe1 O1 C16 -93.1(5) . . . . ?
N1 Fe1 O1 C16 32.4(10) . . . . ?
N1 Fe1 O2 C32 93.2(5) . . . . ?
N1 C1 C2 C3 -1.5(11) . . . . ?
N2 Fe1 O1 C16 1.8(5) . . . . ?
N2 Fe1 O2 C32 171.3(5) . . . . ?
N2 C8 C9 N1 2.1(7) . . . . ?
N2 C8 C9 C4 -179.0(5) . . . . ?
N2 C10 C11 C12 -176.7(10) . . . . ?
N2 C10 C11 C16 0.2(8) . . . . ?
N2 C10 C11 C12A 172.1(8) . . . . ?
N3 Fe1 O1 C16 98.0(5) . . . . ?
N3 Fe1 O2 C32 20.2(11) . . . . ?
N3 C17 C18 C19 1.7(9) . . . . ?
N4 Fe1 O1 C16 176.1(5) . . . . ?
N4 Fe1 O2 C32 -1.0(5) . . . . ?
N4 C24 C25 N3 2.1(7) . . . . ?
N4 C24 C25 C20 -179.5(5) . . . . ?
N4 C26 C27 C28 177.9(5) . . . . ?
N4 C26 C27 C32 -3.4(9) . . . . ?
C1 N1 C9 C4 1.6(8) . . . . ?
C1 N1 C9 C8 -179.4(5) . . . . ?
C1 C2 C3 C4 1.4(11) . . . . ?
C2 C3 C4 C5 179.1(7) . . . . ?
C2 C3 C4 C9 0.1(10) . . . . ?
C3 C4 C5 C6 179.1(7) . . . . ?
C3 C4 C9 N1 -1.7(9) . . . . ?
C3 C4 C9 C8 179.4(6) . . . . ?
C4 C5 C6 C7 3.0(13) . . . . ?
C5 C4 C9 N1 179.3(6) . . . . ?
C5 C4 C9 C8 0.4(9) . . . . ?
C5 C6 C7 C8 -2.5(12) . . . . ?
C6 C7 C8 N2 179.9(6) . . . . ?
C6 C7 C8 C9 0.9(9) . . . . ?
C7 C8 C9 N1 -178.8(5) . . . . ?
C7 C8 C9 C4 0.1(8) . . . . ?
C8 N2 C10 C11 -175.7(4) . . . . ?
C9 N1 C1 C2 0.0(9) . . . . ?
C9 C4 C5 C6 -1.9(11) . . . . ?
C10 N2 C8 C7 -0.8(8) . . . . ?
C10 N2 C8 C9 178.2(4) . . . . ?
C10 C11 C12 C13 -176.0(19) . . . . ?
C10 C11 C16 O1 -4.6(8) . . . . ?
C10 C11 C16 C15 169.5(8) . . . . ?
C10 C11 C16 C15A -174.8(10) . . . . ?
C10 C11 C12A C13A -178.4(13) . . . . ?
C11 C12 C13 C14 -13(4) . . . . ?
C11 C12 C13 O3 -178.3(17) . . . . ?
C11 C16 C15A C14 -6(2) . . . . ?
C11 C12A C13A I1 -177.5(10) . . . . ?
C11 C12A C13A C14A 8(3) . . . . ?
C12 C11 C16 O1 172.5(10) . . . . ?
C12 C11 C16 C15A 2.3(14) . . . . ?
C12 C13 C14 C15A 9(4) . . . . ?
C12 C13 O3 C33 167(2) . . . . ?
C13 C14 C15A C16 0(3) . . . . ?
C14 C13 O3 C33 4(4) . . . . ?
C16 C11 C12 C13 7(3) . . . . ?
C16 C11 C12A C13A -6.0(18) . . . . ?
C16 C15 C14A C13A -8(2) . . . . ?
C17 N3 C25 C20 1.4(8) . . . . ?
C17 N3 C25 C24 179.8(5) . . . . ?
C17 C18 C19 C20 -1.8(11) . . . . ?
C18 C19 C20 C21 -178.6(7) . . . . ?
C18 C19 C20 C25 1.7(11) . . . . ?
C19 C20 C21 C22 179.6(8) . . . . ?
C19 C20 C25 N3 -1.5(9) . . . . ?
C19 C20 C25 C24 -179.8(6) . . . . ?
C20 C21 C22 C23 0.9(14) . . . . ?
C21 C20 C25 N3 178.8(6) . . . . ?
C21 C20 C25 C24 0.5(9) . . . . ?
C21 C22 C23 C24 -0.8(12) . . . . ?
C22 C23 C24 N4 179.6(6) . . . . ?
C22 C23 C24 C25 0.6(10) . . . . ?
C23 C24 C25 N3 -178.8(5) . . . . ?
C23 C24 C25 C20 -0.4(8) . . . . ?
C24 N4 C26 C27 -177.3(5) . . . . ?
C25 N3 C17 C18 -1.5(8) . . . . ?
C25 C20 C21 C22 -0.8(12) . . . . ?
C26 N4 C24 C23 -2.5(8) . . . . ?
C26 N4 C24 C25 176.6(4) . . . . ?
C26 C27 C28 C29 179.2(6) . . . . ?
C26 C27 C32 O2 0.4(9) . . . . ?
C26 C27 C32 C31 -178.7(6) . . . . ?
C27 C28 C29 C30 0.0(11) . . . . ?
C27 C28 C29 I2 -178.8(5) . . . . ?
C27 C28 C29 O4 179.6(8) . . . . ?
C28 C27 C32 O2 179.0(5) . . . . ?
C28 C27 C32 C31 0.0(9) . . . . ?
C28 C29 C30 C31 -1.0(12) . . . . ?
C28 C29 O4 C34 -4.6(15) . . . . ?
C29 C30 C31 C32 1.4(12) . . . . ?
C30 C29 O4 C34 175.0(9) . . . . ?
C30 C31 C32 O2 180.0(7) . . . . ?
C30 C31 C32 C27 -1.0(11) . . . . ?
C32 C27 C28 C29 0.5(9) . . . . ?
I2 C29 C30 C31 177.8(6) . . . . ?
O3 C13 C14 C15A 170(3) . . . . ?
I1 C13A C14A C15 -176.5(11) . . . . ?
O4 C29 C30 C31 179.4(9) . . . . ?
C12A C11 C16 O1 -176.2(8) . . . . ?
C12A C11 C16 C15 -2.1(11) . . . . ?
C12A C13A C14A C15 -1(3) . . . . ?
C14A C15 C16 O1 -176.8(11) . . . . ?
C14A C15 C16 C11 9.2(18) . . . . ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.233 0.000 0.000 188.1 40.5 '2.2 MeOH'
