#------------------------------------------------------------------------------
#$Date: 2023-10-07 02:57:14 +0300 (Sat, 07 Oct 2023) $
#$Revision: 286839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/22/2312212.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2312212
loop_
_publ_author_name
'Shahed, H.'
'Sharma, N.'
'Angst, M.'
'Voigt, J.'
'Perßon, J'
'Prakash, P.'
'Törnroos, K W'
'Chernyshov, D.'
'Gildenast, H.'
'Ohl, M.'
'Saffarini, G.'
'Grzechnik, A.'
'Friese, K.'
_publ_section_title
;
 Structural insight into the cooperativity of spin crossover compounds.
;
_journal_issue                   'Pt 5'
_journal_name_full
'Acta crystallographica Section B, Structural science, crystal engineering and materials'
_journal_page_first              354
_journal_page_last               367
_journal_paper_doi               10.1107/S2052520623005814
_journal_volume                  79
_journal_year                    2023
_chemical_formula_sum            'C38 H28 Fe N6 S2'
_chemical_formula_weight         688.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 115.8449(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2283(2)
_cell_length_b                   12.25660(10)
_cell_length_c                   16.9197(2)
_cell_measurement_reflns_used    18726
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.001
_cell_measurement_theta_min      1.891
_cell_volume                     3215.41(7)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.63582
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23965
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        22.426
_diffrn_reflns_theta_max         25.078
_diffrn_reflns_theta_min         1.895
_exptl_absorpt_coefficient_mu    0.468
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1424
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0006(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         7491
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0500P)²+1.1117P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0913
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7006
_reflns_number_total             7491
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Bia_Pmono_117K.cif
_cod_data_source_block           SC2_117K
_cod_depositor_comments
'Adding full bibliography for 2312165--2312274.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2312212
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Fe01 Fe 0.75551(2) 0.29047(2) 0.81322(2) 0.02242(7) Uani 1 1 d . . . . .
S002 S 0.54587(2) 0.33250(3) 0.91718(2) 0.02862(9) Uani 1 1 d . . . . .
S001 S 0.94765(2) 0.13788(3) 1.07786(2) 0.03237(9) Uani 1 1 d . . . . .
N005 N 0.71404(7) 0.13969(8) 0.79421(7) 0.0227(2) Uani 1 1 d . . . . .
N006 N 0.79957(8) 0.43820(9) 0.82273(7) 0.0288(2) Uani 1 1 d . . . . .
N003 N 0.66998(7) 0.30311(9) 0.69086(7) 0.0237(2) Uani 1 1 d . . . . .
N004 N 0.84042(7) 0.26608(9) 0.76749(7) 0.0252(2) Uani 1 1 d . . . . .
N002 N 0.67186(8) 0.32653(10) 0.85628(8) 0.0288(2) Uani 1 1 d . . . . .
N001 N 0.83989(8) 0.25658(9) 0.93124(7) 0.0271(2) Uani 1 1 d . . . . .
C015 C 0.63594(9) 0.21253(10) 0.65444(9) 0.0256(3) Uani 1 1 d . . . . .
H015 H 0.597987 0.208320 0.595137 0.031 Uiso 1 1 calc R U . . .
C016 C 0.65951(9) 0.11762(10) 0.71008(8) 0.0242(2) Uani 1 1 d . . . . .
C003 C 0.65018(8) 0.39736(10) 0.63627(8) 0.0246(3) Uani 1 1 d . . . . .
C021 C 0.85218(9) 0.16663(11) 0.73105(9) 0.0255(3) Uani 1 1 d . . . . .
C024 C 0.86519(9) -0.03075(11) 0.65814(9) 0.0280(3) Uani 1 1 d D . . . .
C007 C 0.60238(9) 0.58250(11) 0.60792(9) 0.0278(3) Uani 1 1 d . . . . .
H007 H 0.582661 0.645141 0.624380 0.033 Uiso 1 1 calc R U . . .
C012 C 0.57086(10) 0.86624(12) 0.37206(10) 0.0325(3) Uani 1 1 d . . . . .
H012 H 0.563146 0.928182 0.337684 0.039 Uiso 1 1 calc R U . . .
C010 C 0.56176(9) 0.67291(11) 0.38460(9) 0.0281(3) Uani 1 1 d . . . . .
H010 H 0.547360 0.604778 0.357932 0.034 Uiso 1 1 calc R U . . .
C022 C 0.83324(10) 0.16088(11) 0.64322(9) 0.0294(3) Uani 1 1 d . . . . .
H022 H 0.815550 0.222982 0.608266 0.035 Uiso 1 1 calc R U . . .
C008 C 0.62213(9) 0.49130(11) 0.66103(9) 0.0267(3) Uani 1 1 d . . . . .
H008 H 0.616588 0.493048 0.713280 0.032 Uiso 1 1 calc R U . . .
C025 C 0.88378(9) -0.02294(11) 0.74630(9) 0.0288(3) Uani 1 1 d . . . . .
H025 H 0.900271 -0.085206 0.781156 0.035 Uiso 1 1 calc R U . . .
C002 C 0.61980(9) 0.32921(10) 0.88193(8) 0.0250(3) Uani 1 1 d . . . . .
C004 C 0.65813(9) 0.39496(10) 0.55907(9) 0.0273(3) Uani 1 1 d . . . . .
H004 H 0.676548 0.331617 0.542120 0.033 Uiso 1 1 calc R U . . .
C020 C 0.73637(9) 0.05764(11) 0.85152(9) 0.0266(3) Uani 1 1 d . . . . .
H020 H 0.772486 0.071986 0.910193 0.032 Uiso 1 1 calc R U . . .
C005 C 0.63878(9) 0.48664(11) 0.50657(9) 0.0281(3) Uani 1 1 d . . . . .
H005 H 0.644156 0.484274 0.454242 0.034 Uiso 1 1 calc R U . . .
C009 C 0.59495(9) 0.68064(11) 0.47522(9) 0.0259(3) Uani 1 1 d . . . . .
C017 C 0.62854(9) 0.01447(11) 0.68144(9) 0.0296(3) Uani 1 1 d . . . . .
H017 H 0.591141 0.002007 0.622827 0.035 Uiso 1 1 calc R U . . .
C006 C 0.61149(9) 0.58217(10) 0.53042(9) 0.0257(3) Uani 1 1 d . . . . .
C018 C 0.65389(10) -0.07003(11) 0.74108(10) 0.0312(3) Uani 1 1 d . . . . .
H018 H 0.634753 -0.140809 0.723382 0.037 Uiso 1 1 calc R U . . .
C001 C 0.88526(9) 0.20986(10) 0.99322(9) 0.0253(3) Uani 1 1 d . . . . .
C011 C 0.54973(10) 0.76483(12) 0.33332(10) 0.0312(3) Uani 1 1 d . . . . .
H011 H 0.527360 0.758263 0.272608 0.037 Uiso 1 1 calc R U . . .
C026 C 0.87837(9) 0.07466(11) 0.78328(9) 0.0275(3) Uani 1 1 d . . . . .
H026 H 0.892185 0.078855 0.842813 0.033 Uiso 1 1 calc R U . . .
C028 C 0.86163(10) 0.45022(12) 0.79537(9) 0.0333(3) Uani 1 1 d . . . . .
C014 C 0.61521(10) 0.78337(11) 0.51295(10) 0.0307(3) Uani 1 1 d . . . . .
H014 H 0.637066 0.790478 0.573579 0.037 Uiso 1 1 calc R U . . .
C013 C 0.60340(11) 0.87537(11) 0.46181(10) 0.0341(3) Uani 1 1 d . . . . .
H013 H 0.617500 0.943701 0.488169 0.041 Uiso 1 1 calc R U . . .
C023 C 0.84061(10) 0.06256(12) 0.60729(9) 0.0308(3) Uani 1 1 d . . . . .
H023 H 0.828911 0.059070 0.548243 0.037 Uiso 1 1 calc R U . . .
C027 C 0.88086(10) 0.35099(12) 0.76231(10) 0.0317(3) Uani 1 1 d . . . . .
H027 H 0.920401 0.348752 0.738558 0.038 Uiso 1 1 calc R U . . .
C019 C 0.70806(9) -0.04748(11) 0.82725(9) 0.0295(3) Uani 1 1 d . . . . .
H019 H 0.725482 -0.102948 0.868927 0.035 Uiso 1 1 calc R U . . .
C032 C 0.77610(11) 0.52536(12) 0.85435(10) 0.0365(3) Uani 1 1 d . . . . .
H032 H 0.733643 0.518109 0.873980 0.044 Uiso 1 1 calc R U . . .
C031 C 0.81357(13) 0.62621(13) 0.85854(12) 0.0482(5) Uani 1 1 d . . . . .
H031 H 0.795100 0.686326 0.879294 0.058 Uiso 1 1 calc R U . . .
C029 C 0.90236(13) 0.54856(14) 0.79952(12) 0.0463(4) Uani 1 1 d . . . . .
H029 H 0.945442 0.554261 0.780625 0.056 Uiso 1 1 calc R U . . .
C030 C 0.87769(15) 0.63782(14) 0.83227(13) 0.0537(5) Uani 1 1 d . . . . .
H030 H 0.904232 0.705050 0.836467 0.064 Uiso 1 1 calc R U . . .
C1A C 0.8681(8) -0.1360(5) 0.6162(7) 0.0280(13) Uani 0.53(3) 1 d DG . P A 1
C2A C 0.8288(8) -0.2249(7) 0.6349(6) 0.0390(15) Uani 0.53(3) 1 d G . P A 1
H2A H 0.795532 -0.214739 0.665291 0.047 Uiso 0.53(3) 1 calc R U P A 1
C3A C 0.8391(7) -0.3289(6) 0.6081(7) 0.0434(14) Uani 0.53(3) 1 d G . P A 1
H3A H 0.812779 -0.388324 0.620603 0.052 Uiso 0.53(3) 1 calc R U P A 1
C4A C 0.8887(7) -0.3440(6) 0.5626(7) 0.0372(16) Uani 0.53(3) 1 d G . P A 1
H4A H 0.895660 -0.413596 0.544709 0.045 Uiso 0.53(3) 1 calc R U P A 1
C5A C 0.9281(7) -0.2552(9) 0.5439(6) 0.0364(15) Uani 0.53(3) 1 d G . P A 1
H5A H 0.961292 -0.265284 0.513501 0.044 Uiso 0.53(3) 1 calc R U P A 1
C6A C 0.9177(7) -0.1512(6) 0.5707(7) 0.0315(12) Uani 0.53(3) 1 d G . P A 1
H6A H 0.944045 -0.091698 0.558188 0.038 Uiso 0.53(3) 1 calc R U P A 1
C1B C 0.8805(9) -0.1375(6) 0.6266(8) 0.0289(14) Uani 0.47(3) 1 d DG . P A 2
C2B C 0.8448(9) -0.2353(8) 0.6365(7) 0.0316(14) Uani 0.47(3) 1 d G . P A 2
H2B H 0.812877 -0.237299 0.668834 0.038 Uiso 0.47(3) 1 calc R U P A 2
C3B C 0.8568(9) -0.3300(6) 0.5981(7) 0.0395(17) Uani 0.47(3) 1 d G . P A 2
H3B H 0.832959 -0.395452 0.604692 0.047 Uiso 0.47(3) 1 calc R U P A 2
C4B C 0.9046(8) -0.3270(9) 0.5498(7) 0.0396(18) Uani 0.47(3) 1 d G . P A 2
H4B H 0.912621 -0.390414 0.524042 0.048 Uiso 0.47(3) 1 calc R U P A 2
C5B C 0.9403(8) -0.2292(12) 0.5399(7) 0.0448(16) Uani 0.47(3) 1 d G . P A 2
H5B H 0.972203 -0.227222 0.507533 0.054 Uiso 0.47(3) 1 calc R U P A 2
C6B C 0.9282(8) -0.1345(9) 0.5783(8) 0.0435(18) Uani 0.47(3) 1 d G . P A 2
H6B H 0.952121 -0.069067 0.571674 0.052 Uiso 0.47(3) 1 calc R U P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0024 0.0013 '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'
N N 0.0049 0.0027 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1051 0.1002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3265 0.6960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
N002 Fe01 N001 90.48(5) . . ?
N002 Fe01 N006 94.84(5) . . ?
N001 Fe01 N006 91.37(5) . . ?
N002 Fe01 N004 175.50(5) . . ?
N001 Fe01 N004 91.17(5) . . ?
N006 Fe01 N004 80.93(5) . . ?
N002 Fe01 N003 92.27(5) . . ?
N001 Fe01 N003 172.09(5) . . ?
N006 Fe01 N003 95.78(5) . . ?
N004 Fe01 N003 86.64(5) . . ?
N002 Fe01 N005 89.95(5) . . ?
N001 Fe01 N005 91.32(5) . . ?
N006 Fe01 N005 174.48(5) . . ?
N004 Fe01 N005 94.19(5) . . ?
N003 Fe01 N005 81.27(5) . . ?
C020 N005 C016 117.68(11) . . ?
C020 N005 Fe01 128.65(9) . . ?
C016 N005 Fe01 113.56(8) . . ?
C032 N006 C028 118.39(13) . . ?
C032 N006 Fe01 127.14(12) . . ?
C028 N006 Fe01 114.45(9) . . ?
C015 N003 C003 117.44(11) . . ?
C015 N003 Fe01 114.60(9) . . ?
C003 N003 Fe01 127.44(9) . . ?
C027 N004 C021 118.99(13) . . ?
C027 N004 Fe01 115.33(10) . . ?
C021 N004 Fe01 125.22(9) . . ?
C002 N002 Fe01 168.36(11) . . ?
C001 N001 Fe01 162.53(11) . . ?
N003 C015 C016 116.51(12) . . ?
N005 C016 C017 122.78(12) . . ?
N005 C016 C015 113.37(11) . . ?
C017 C016 C015 123.84(12) . . ?
C004 C003 C008 119.97(12) . . ?
C004 C003 N003 120.33(12) . . ?
C008 C003 N003 119.70(12) . . ?
C022 C021 C026 120.42(13) . . ?
C022 C021 N004 120.06(12) . . ?
C026 C021 N004 119.43(12) . . ?
C023 C024 C025 118.51(13) . . ?
C023 C024 C1B 124.2(5) . . ?
C025 C024 C1B 117.1(5) . . ?
C023 C024 C1A 119.1(4) . . ?
C025 C024 C1A 122.3(4) . . ?
C008 C007 C006 121.04(12) . . ?
C013 C012 C011 119.65(13) . . ?
C011 C010 C009 121.03(13) . . ?
C021 C022 C023 119.73(13) . . ?
C007 C008 C003 119.78(13) . . ?
C026 C025 C024 121.42(13) . . ?
N002 C002 S002 179.47(13) . . ?
C003 C004 C005 119.93(12) . . ?
N005 C020 C019 122.52(13) . . ?
C004 C005 C006 121.20(13) . . ?
C014 C009 C010 118.11(13) . . ?
C014 C009 C006 120.73(13) . . ?
C010 C009 C006 121.11(12) . . ?
C016 C017 C018 118.85(13) . . ?
C005 C006 C007 118.06(12) . . ?
C005 C006 C009 120.20(12) . . ?
C007 C006 C009 121.72(12) . . ?
C019 C018 C017 118.56(12) . . ?
N001 C001 S001 176.97(12) . . ?
C012 C011 C010 120.04(14) . . ?
C025 C026 C021 119.21(13) . . ?
N006 C028 C029 122.71(15) . . ?
N006 C028 C027 113.21(12) . . ?
C029 C028 C027 124.08(16) . . ?
C013 C014 C009 120.95(14) . . ?
C012 C013 C014 120.21(14) . . ?
C022 C023 C024 120.68(13) . . ?
N004 C027 C028 115.98(14) . . ?
C018 C019 C020 119.59(13) . . ?
N006 C032 C031 121.35(18) . . ?
C030 C031 C032 120.16(17) . . ?
C030 C029 C028 118.39(18) . . ?
C031 C030 C029 118.96(16) . . ?
C2A C1A C6A 120.0 . . ?
C2A C1A C024 116.8(6) . . ?
C6A C1A C024 122.6(6) . . ?
C3A C2A C1A 120.0 . . ?
C2A C3A C4A 120.0 . . ?
C5A C4A C3A 120.0 . . ?
C4A C5A C6A 120.0 . . ?
C5A C6A C1A 120.0 . . ?
C2B C1B C6B 120.0 . . ?
C2B C1B C024 124.1(7) . . ?
C6B C1B C024 115.6(7) . . ?
C1B C2B C3B 120.0 . . ?
C2B C3B C4B 120.0 . . ?
C5B C4B C3B 120.0 . . ?
C4B C5B C6B 120.0 . . ?
C5B C6B C1B 120.0 . . ?
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
Fe01 N002 1.9282(13) . ?
Fe01 N001 1.9346(12) . ?
Fe01 N006 1.9426(11) . ?
Fe01 N004 1.9532(12) . ?
Fe01 N003 1.9549(11) . ?
Fe01 N005 1.9567(11) . ?
S002 C002 1.6252(15) . ?
S001 C001 1.6255(14) . ?
N005 C020 1.3320(16) . ?
N005 C016 1.3476(16) . ?
N006 C032 1.3341(19) . ?
N006 C028 1.346(2) . ?
N003 C015 1.2811(16) . ?
N003 C003 1.4245(16) . ?
N004 C027 1.2766(18) . ?
N004 C021 1.4199(17) . ?
N002 C002 1.155(2) . ?
N001 C001 1.1506(18) . ?
C015 C016 1.4392(17) . ?
C016 C017 1.3757(17) . ?
C003 C004 1.372(2) . ?
C003 C008 1.3824(18) . ?
C021 C022 1.3773(19) . ?
C021 C026 1.3811(18) . ?
C024 C023 1.382(2) . ?
C024 C025 1.386(2) . ?
C024 C1B 1.480(6) . ?
C024 C1A 1.484(5) . ?
C007 C008 1.3806(18) . ?
C007 C006 1.387(2) . ?
C012 C013 1.375(2) . ?
C012 C011 1.378(2) . ?
C010 C011 1.3814(19) . ?
C010 C009 1.3864(19) . ?
C022 C023 1.380(2) . ?
C025 C026 1.3718(19) . ?
C004 C005 1.3801(18) . ?
C020 C019 1.3756(18) . ?
C005 C006 1.3857(18) . ?
C009 C014 1.3858(19) . ?
C009 C006 1.4759(17) . ?
C017 C018 1.3774(19) . ?
C018 C019 1.374(2) . ?
C028 C029 1.381(2) . ?
C028 C027 1.436(2) . ?
C014 C013 1.3813(19) . ?
C032 C031 1.382(2) . ?
C031 C030 1.366(3) . ?
C029 C030 1.375(3) . ?
C1A C2A 1.3900 . ?
C1A C6A 1.3900 . ?
C2A C3A 1.3900 . ?
C3A C4A 1.3900 . ?
C4A C5A 1.3900 . ?
C5A C6A 1.3900 . ?
C1B C2B 1.3900 . ?
C1B C6B 1.3900 . ?
C2B C3B 1.3900 . ?
C3B C4B 1.3900 . ?
C4B C5B 1.3900 . ?
C5B C6B 1.3900 . ?
