#------------------------------------------------------------------------------
#$Date: 2023-10-07 02:57:14 +0300 (Sat, 07 Oct 2023) $
#$Revision: 286839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/22/2312209.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_2312209
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                 115.8222(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1718(2)
_cell_length_b                   12.26000(10)
_cell_length_c                   16.9206(2)
_cell_measurement_reflns_used    17389
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.998
_cell_measurement_theta_min      1.885
_cell_volume                     3206.54(7)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.63582
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.937
_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            23713
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        22.426
_diffrn_reflns_theta_max         25.078
_diffrn_reflns_theta_min         1.897
_exptl_absorpt_coefficient_mu    0.469
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1424
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0000(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   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         7460
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.099
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0547P)²+1.2047P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.0955
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6996
_reflns_number_total             7460
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Bia_Pmono_102K.cif
_cod_data_source_block           SC2_102K
_cod_depositor_comments
'Adding full bibliography for 2312165--2312274.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2312209
_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 0.75578(2) 0.29083(2) 0.81287(2) 0.02075(7) Uani 1 1 d . . . . .
S002 S 0.54584(2) 0.33277(3) 0.91721(2) 0.02621(9) Uani 1 1 d . . . . .
S001 S 0.94758(2) 0.13783(3) 1.07752(2) 0.02946(10) Uani 1 1 d . . . . .
N005 N 0.71421(7) 0.14011(9) 0.79398(7) 0.0211(2) Uani 1 1 d . . . . .
N006 N 0.80013(8) 0.43844(9) 0.82243(8) 0.0266(2) Uani 1 1 d . . . . .
N003 N 0.67018(8) 0.30338(9) 0.69059(7) 0.0220(2) Uani 1 1 d . . . . .
N004 N 0.84107(8) 0.26619(9) 0.76737(8) 0.0235(2) Uani 1 1 d . . . . .
N002 N 0.67184(8) 0.32723(10) 0.85580(8) 0.0267(2) Uani 1 1 d . . . . .
N001 N 0.84030(8) 0.25705(10) 0.93092(8) 0.0252(2) Uani 1 1 d . . . . .
C015 C 0.63612(9) 0.21271(10) 0.65406(9) 0.0235(3) Uani 1 1 d . . . . .
H015 H 0.598240 0.208423 0.594729 0.028 Uiso 1 1 calc R U . . .
C016 C 0.65969(9) 0.11798(10) 0.70984(9) 0.0222(3) Uani 1 1 d . . . . .
C003 C 0.65017(9) 0.39752(10) 0.63597(9) 0.0226(3) Uani 1 1 d . . . . .
C021 C 0.85272(9) 0.16648(11) 0.73106(9) 0.0239(3) Uani 1 1 d . . . . .
C024 C 0.86495(9) -0.03130(11) 0.65812(9) 0.0257(3) Uani 1 1 d D . . . .
C007 C 0.60229(9) 0.58247(11) 0.60758(9) 0.0254(3) Uani 1 1 d . . . . .
H007 H 0.582635 0.645149 0.624113 0.030 Uiso 1 1 calc R U . . .
C012 C 0.57073(10) 0.86614(12) 0.37172(10) 0.0294(3) Uani 1 1 d . . . . .
H012 H 0.563099 0.928062 0.337372 0.035 Uiso 1 1 calc R U . . .
C010 C 0.56170(9) 0.67289(11) 0.38420(9) 0.0256(3) Uani 1 1 d . . . . .
H010 H 0.547443 0.604761 0.357533 0.031 Uiso 1 1 calc R U . . .
C022 C 0.83363(10) 0.16049(11) 0.64311(9) 0.0270(3) Uani 1 1 d . . . . .
H022 H 0.816144 0.222605 0.608169 0.032 Uiso 1 1 calc R U . . .
C008 C 0.62214(9) 0.49145(11) 0.66070(9) 0.0248(3) Uani 1 1 d . . . . .
H008 H 0.616665 0.493306 0.713004 0.030 Uiso 1 1 calc R U . . .
C025 C 0.88381(9) -0.02317(11) 0.74634(9) 0.0265(3) Uani 1 1 d . . . . .
H025 H 0.900183 -0.085376 0.781244 0.032 Uiso 1 1 calc R U . . .
C002 C 0.61984(9) 0.32964(10) 0.88168(9) 0.0234(3) Uani 1 1 d . . . . .
C004 C 0.65814(9) 0.39498(11) 0.55860(9) 0.0253(3) Uani 1 1 d . . . . .
H004 H 0.676554 0.331615 0.541638 0.030 Uiso 1 1 calc R U . . .
C020 C 0.73633(9) 0.05832(11) 0.85129(9) 0.0247(3) Uani 1 1 d . . . . .
H020 H 0.772251 0.072767 0.910002 0.030 Uiso 1 1 calc R U . . .
C005 C 0.63875(10) 0.48672(11) 0.50611(9) 0.0259(3) Uani 1 1 d . . . . .
H005 H 0.644313 0.484442 0.453869 0.031 Uiso 1 1 calc R U . . .
C009 C 0.59469(9) 0.68055(11) 0.47464(9) 0.0239(3) Uani 1 1 d . . . . .
C017 C 0.62882(9) 0.01484(11) 0.68121(9) 0.0270(3) Uani 1 1 d . . . . .
H017 H 0.591450 0.002341 0.622581 0.032 Uiso 1 1 calc R U . . .
C006 C 0.61114(9) 0.58214(11) 0.52988(9) 0.0239(3) Uani 1 1 d . . . . .
C018 C 0.65416(10) -0.06965(11) 0.74082(10) 0.0287(3) Uani 1 1 d . . . . .
H018 H 0.635163 -0.140467 0.723082 0.034 Uiso 1 1 calc R U . . .
C001 C 0.88551(9) 0.21026(10) 0.99291(9) 0.0238(3) Uani 1 1 d . . . . .
C011 C 0.54961(10) 0.76473(12) 0.33294(10) 0.0287(3) Uani 1 1 d . . . . .
H011 H 0.527212 0.758174 0.272245 0.034 Uiso 1 1 calc R U . . .
C026 C 0.87885(9) 0.07465(11) 0.78329(9) 0.0253(3) Uani 1 1 d . . . . .
H026 H 0.892945 0.079008 0.842860 0.030 Uiso 1 1 calc R U . . .
C028 C 0.86275(10) 0.45008(12) 0.79543(10) 0.0302(3) Uani 1 1 d . . . . .
C014 C 0.61477(10) 0.78342(11) 0.51251(10) 0.0282(3) Uani 1 1 d . . . . .
H014 H 0.636351 0.790518 0.573094 0.034 Uiso 1 1 calc R U . . .
C013 C 0.60313(11) 0.87527(11) 0.46143(11) 0.0310(3) Uani 1 1 d . . . . .
H013 H 0.617248 0.943581 0.487783 0.037 Uiso 1 1 calc R U . . .
C023 C 0.84053(10) 0.06223(12) 0.60716(10) 0.0284(3) Uani 1 1 d . . . . .
H023 H 0.828672 0.058648 0.548098 0.034 Uiso 1 1 calc R U . . .
C027 C 0.88208(10) 0.35069(12) 0.76245(10) 0.0287(3) Uani 1 1 d . . . . .
H027 H 0.921988 0.348174 0.739001 0.034 Uiso 1 1 calc R U . . .
C019 C 0.70806(10) -0.04699(11) 0.82697(10) 0.0270(3) Uani 1 1 d . . . . .
H019 H 0.725389 -0.102386 0.868684 0.032 Uiso 1 1 calc R U . . .
C032 C 0.77671(11) 0.52566(12) 0.85381(10) 0.0330(3) Uani 1 1 d . . . . .
H032 H 0.733999 0.518601 0.873306 0.040 Uiso 1 1 calc R U . . .
C031 C 0.81439(13) 0.62637(13) 0.85807(12) 0.0435(4) Uani 1 1 d . . . . .
H031 H 0.795743 0.686580 0.878586 0.052 Uiso 1 1 calc R U . . .
C029 C 0.90373(13) 0.54834(13) 0.79983(12) 0.0413(4) Uani 1 1 d . . . . .
H029 H 0.947192 0.553886 0.781242 0.050 Uiso 1 1 calc R U . . .
C030 C 0.87893(14) 0.63765(13) 0.83222(13) 0.0480(5) Uani 1 1 d . . . . .
H030 H 0.905694 0.704772 0.836472 0.058 Uiso 1 1 calc R U . . .
C1A C 0.8665(7) -0.1360(5) 0.6152(7) 0.0241(12) Uani 0.56(3) 1 d DG . P A 1
C2A C 0.8279(7) -0.2251(7) 0.6347(6) 0.0346(13) Uani 0.56(3) 1 d G . P A 1
H2A H 0.794717 -0.215203 0.665293 0.041 Uiso 0.56(3) 1 calc R U P A 1
C3A C 0.8389(7) -0.3291(5) 0.6084(7) 0.0411(14) Uani 0.56(3) 1 d G . P A 1
H3A H 0.813116 -0.388768 0.621449 0.049 Uiso 0.56(3) 1 calc R U P A 1
C4A C 0.8885(7) -0.3440(5) 0.5626(7) 0.0350(15) Uani 0.56(3) 1 d G . P A 1
H4A H 0.895878 -0.413541 0.545068 0.042 Uiso 0.56(3) 1 calc R U P A 1
C5A C 0.9271(7) -0.2548(8) 0.5431(6) 0.0336(14) Uani 0.56(3) 1 d G . P A 1
H5A H 0.960241 -0.264749 0.512531 0.040 Uiso 0.56(3) 1 calc R U P A 1
C6A C 0.9160(7) -0.1508(6) 0.5694(6) 0.0292(12) Uani 0.56(3) 1 d G . P A 1
H6A H 0.941843 -0.091183 0.556374 0.035 Uiso 0.56(3) 1 calc R U P A 1
C1B C 0.8820(8) -0.1389(6) 0.6288(8) 0.0228(14) Uani 0.44(3) 1 d DG . P A 2
C2B C 0.8453(9) -0.2360(8) 0.6385(6) 0.0256(14) Uani 0.44(3) 1 d G . P A 2
H2B H 0.813869 -0.237501 0.671476 0.031 Uiso 0.44(3) 1 calc R U P A 2
C3B C 0.8555(9) -0.3308(6) 0.5989(7) 0.0349(18) Uani 0.44(3) 1 d G . P A 2
H3B H 0.830863 -0.395702 0.605373 0.042 Uiso 0.44(3) 1 calc R U P A 2
C4B C 0.9024(9) -0.3285(9) 0.5496(8) 0.0360(19) Uani 0.44(3) 1 d G . P A 2
H4B H 0.909223 -0.391877 0.523103 0.043 Uiso 0.44(3) 1 calc R U P A 2
C5B C 0.9392(9) -0.2314(12) 0.5399(8) 0.0413(17) Uani 0.44(3) 1 d G . P A 2
H5B H 0.970590 -0.229851 0.506937 0.050 Uiso 0.44(3) 1 calc R U P A 2
C6B C 0.9290(9) -0.1366(8) 0.5795(9) 0.0377(18) Uani 0.44(3) 1 d G . P A 2
H6B H 0.953598 -0.071648 0.573039 0.045 Uiso 0.44(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 94.78(5) . . ?
N001 Fe01 N006 91.31(5) . . ?
N002 Fe01 N004 175.47(5) . . ?
N001 Fe01 N004 91.13(5) . . ?
N006 Fe01 N004 80.95(5) . . ?
N002 Fe01 N003 92.27(5) . . ?
N001 Fe01 N003 172.10(5) . . ?
N006 Fe01 N003 95.83(5) . . ?
N004 Fe01 N003 86.68(5) . . ?
N002 Fe01 N005 90.04(5) . . ?
N001 Fe01 N005 91.31(5) . . ?
N006 Fe01 N005 174.49(5) . . ?
N004 Fe01 N005 94.15(5) . . ?
N003 Fe01 N005 81.29(5) . . ?
C020 N005 C016 117.70(11) . . ?
C020 N005 Fe01 128.67(10) . . ?
C016 N005 Fe01 113.51(9) . . ?
C032 N006 C028 118.34(13) . . ?
C032 N006 Fe01 127.28(12) . . ?
C028 N006 Fe01 114.36(10) . . ?
C015 N003 C003 117.34(12) . . ?
C015 N003 Fe01 114.64(9) . . ?
C003 N003 Fe01 127.51(9) . . ?
C027 N004 C021 119.00(13) . . ?
C027 N004 Fe01 115.49(11) . . ?
C021 N004 Fe01 125.08(9) . . ?
C002 N002 Fe01 168.08(11) . . ?
C001 N001 Fe01 162.43(11) . . ?
N003 C015 C016 116.39(12) . . ?
N005 C016 C017 122.76(12) . . ?
N005 C016 C015 113.45(11) . . ?
C017 C016 C015 123.78(12) . . ?
C004 C003 C008 119.99(12) . . ?
C004 C003 N003 120.25(12) . . ?
C008 C003 N003 119.76(12) . . ?
C022 C021 C026 120.37(13) . . ?
C022 C021 N004 120.02(12) . . ?
C026 C021 N004 119.52(13) . . ?
C023 C024 C025 118.42(13) . . ?
C023 C024 C1A 118.5(4) . . ?
C025 C024 C1A 123.0(4) . . ?
C023 C024 C1B 125.3(5) . . ?
C025 C024 C1B 115.9(5) . . ?
C008 C007 C006 121.14(13) . . ?
C013 C012 C011 119.66(13) . . ?
C011 C010 C009 121.08(13) . . ?
C023 C022 C021 119.81(13) . . ?
C007 C008 C003 119.78(13) . . ?
C026 C025 C024 121.45(13) . . ?
N002 C002 S002 179.45(13) . . ?
C003 C004 C005 119.86(13) . . ?
N005 C020 C019 122.49(13) . . ?
C004 C005 C006 121.19(13) . . ?
C010 C009 C014 118.14(13) . . ?
C010 C009 C006 121.19(12) . . ?
C014 C009 C006 120.64(13) . . ?
C016 C017 C018 118.90(13) . . ?
C005 C006 C007 118.03(12) . . ?
C005 C006 C009 120.09(13) . . ?
C007 C006 C009 121.86(12) . . ?
C019 C018 C017 118.51(13) . . ?
N001 C001 S001 176.82(13) . . ?
C012 C011 C010 120.00(14) . . ?
C025 C026 C021 119.25(13) . . ?
N006 C028 C029 122.54(15) . . ?
N006 C028 C027 113.29(12) . . ?
C029 C028 C027 124.18(16) . . ?
C013 C014 C009 120.87(14) . . ?
C012 C013 C014 120.24(14) . . ?
C022 C023 C024 120.66(13) . . ?
N004 C027 C028 115.82(14) . . ?
C018 C019 C020 119.59(13) . . ?
N006 C032 C031 121.50(17) . . ?
C030 C031 C032 120.10(17) . . ?
C030 C029 C028 118.55(18) . . ?
C031 C030 C029 118.94(16) . . ?
C2A C1A C6A 120.0 . . ?
C2A C1A C024 117.0(6) . . ?
C6A C1A C024 122.2(5) . . ?
C1A C2A C3A 120.0 . . ?
C4A C3A C2A 120.0 . . ?
C3A C4A C5A 120.0 . . ?
C6A C5A C4A 120.0 . . ?
C5A C6A C1A 120.0 . . ?
C2B C1B C6B 120.0 . . ?
C2B C1B C024 123.8(7) . . ?
C6B C1B C024 115.7(7) . . ?
C1B C2B C3B 120.0 . . ?
C4B C3B C2B 120.0 . . ?
C3B C4B C5B 120.0 . . ?
C6B C5B C4B 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 1.9278(13) . ?
Fe01 N001 1.9344(12) . ?
Fe01 N006 1.9427(12) . ?
Fe01 N004 1.9522(13) . ?
Fe01 N003 1.9534(11) . ?
Fe01 N005 1.9563(11) . ?
S002 C002 1.6258(16) . ?
S001 C001 1.6263(14) . ?
N005 C020 1.3302(17) . ?
N005 C016 1.3475(17) . ?
N006 C032 1.3316(19) . ?
N006 C028 1.346(2) . ?
N003 C015 1.2825(17) . ?
N003 C003 1.4240(16) . ?
N004 C027 1.2756(18) . ?
N004 C021 1.4208(17) . ?
N002 C002 1.154(2) . ?
N001 C001 1.1500(19) . ?
C015 C016 1.4390(18) . ?
C016 C017 1.3751(18) . ?
C003 C004 1.375(2) . ?
C003 C008 1.3815(19) . ?
C021 C022 1.379(2) . ?
C021 C026 1.3800(19) . ?
C024 C023 1.385(2) . ?
C024 C025 1.386(2) . ?
C024 C1A 1.481(5) . ?
C024 C1B 1.483(7) . ?
C007 C008 1.3794(18) . ?
C007 C006 1.388(2) . ?
C012 C013 1.375(2) . ?
C012 C011 1.379(2) . ?
C010 C011 1.3807(19) . ?
C010 C009 1.384(2) . ?
C022 C023 1.378(2) . ?
C025 C026 1.3720(19) . ?
C004 C005 1.3810(18) . ?
C020 C019 1.3776(18) . ?
C005 C006 1.3860(19) . ?
C009 C014 1.3883(19) . ?
C009 C006 1.4763(18) . ?
C017 C018 1.377(2) . ?
C018 C019 1.372(2) . ?
C028 C029 1.381(2) . ?
C028 C027 1.438(2) . ?
C014 C013 1.3800(19) . ?
C032 C031 1.381(2) . ?
C031 C030 1.364(3) . ?
C029 C030 1.373(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 . ?
