#------------------------------------------------------------------------------
#$Date: 2023-10-07 02:57:14 +0300 (Sat, 07 Oct 2023) $
#$Revision: 286839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/21/2312169.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_2312169
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                 115.7714(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3653(2)
_cell_length_b                   12.30050(10)
_cell_length_c                   16.96810(10)
_cell_measurement_reflns_used    14902
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.737
_cell_measurement_theta_min      1.878
_cell_volume                     3263.92(6)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.971
_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  0.0359
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_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            24418
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        22.426
_diffrn_reflns_theta_max         25.079
_diffrn_reflns_theta_min         1.884
_exptl_absorpt_coefficient_mu    0.461
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1424
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.0054(6)
_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   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         7607
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0387
_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)+(0.0559P)²+0.9671P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1126
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6882
_reflns_number_total             7607
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Bia_Pmono_198K.cif
_cod_data_source_block           SC2_198K
_cod_depositor_comments
'Adding full bibliography for 2312165--2312274.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2312169
_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 0.75537(2) 0.29137(2) 0.81555(2) 0.03915(9) Uani 1 1 d . . . . .
S002 S 0.54648(3) 0.33381(4) 0.91776(3) 0.04849(12) Uani 1 1 d . . . . .
S001 S 0.94797(3) 0.13364(5) 1.07646(3) 0.05795(14) Uani 1 1 d . . . . .
N005 N 0.71322(8) 0.13924(10) 0.79416(8) 0.0361(3) Uani 1 1 d . . . . .
N006 N 0.79969(11) 0.43946(13) 0.82323(10) 0.0519(4) Uani 1 1 d . . . . .
N003 N 0.66937(9) 0.30388(10) 0.69111(9) 0.0380(3) Uani 1 1 d . . . . .
N004 N 0.84031(9) 0.26704(11) 0.76709(9) 0.0409(3) Uani 1 1 d . . . . .
N002 N 0.67191(11) 0.32739(15) 0.85804(11) 0.0557(4) Uani 1 1 d . . . . .
N001 N 0.84012(10) 0.25454(12) 0.93347(10) 0.0461(3) Uani 1 1 d . . . . .
C015 C 0.63642(11) 0.21342(13) 0.65524(10) 0.0404(3) Uani 1 1 d . . . . .
H015 H 0.599152 0.209054 0.596066 0.049 Uiso 1 1 calc R U . . .
C016 C 0.65951(10) 0.11851(12) 0.71047(10) 0.0387(3) Uani 1 1 d . . . . .
C003 C 0.64982(10) 0.39737(12) 0.63653(10) 0.0390(3) Uani 1 1 d . . . . .
C021 C 0.85203(11) 0.16831(13) 0.73033(11) 0.0407(3) Uani 1 1 d . . . . .
C024 C 0.86616(11) -0.02758(14) 0.65772(11) 0.0444(4) Uani 1 1 d D . . . .
C007 C 0.60324(12) 0.58169(13) 0.60792(11) 0.0448(4) Uani 1 1 d . . . . .
H007 H 0.583947 0.644337 0.624351 0.054 Uiso 1 1 calc R U . . .
C012 C 0.57109(14) 0.86288(16) 0.37188(14) 0.0551(5) Uani 1 1 d . . . . .
H012 H 0.563554 0.924352 0.337384 0.066 Uiso 1 1 calc R U . . .
C010 C 0.56166(12) 0.67116(15) 0.38539(12) 0.0472(4) Uani 1 1 d . . . . .
H010 H 0.546798 0.603235 0.358977 0.057 Uiso 1 1 calc R U . . .
C022 C 0.83366(12) 0.16285(15) 0.64288(11) 0.0472(4) Uani 1 1 d . . . . .
H022 H 0.816137 0.224789 0.608115 0.057 Uiso 1 1 calc R U . . .
C008 C 0.62263(11) 0.49136(14) 0.66103(11) 0.0436(4) Uani 1 1 d . . . . .
H008 H 0.617407 0.493706 0.713275 0.052 Uiso 1 1 calc R U . . .
C025 C 0.88387(11) -0.02022(14) 0.74525(11) 0.0453(4) Uani 1 1 d . . . . .
H025 H 0.900191 -0.082355 0.779872 0.054 Uiso 1 1 calc R U . . .
C002 C 0.62010(12) 0.33127(14) 0.88349(10) 0.0440(4) Uani 1 1 d . . . . .
C004 C 0.65754(12) 0.39469(13) 0.55922(11) 0.0442(4) Uani 1 1 d . . . . .
H004 H 0.675509 0.331406 0.542208 0.053 Uiso 1 1 calc R U . . .
C020 C 0.73514(11) 0.05655(13) 0.85023(11) 0.0422(3) Uani 1 1 d . . . . .
H020 H 0.771101 0.069933 0.908796 0.051 Uiso 1 1 calc R U . . .
C005 C 0.63866(12) 0.48568(14) 0.50719(12) 0.0458(4) Uani 1 1 d . . . . .
H005 H 0.644005 0.483117 0.455013 0.055 Uiso 1 1 calc R U . . .
C009 C 0.59524(11) 0.67887(13) 0.47514(11) 0.0422(3) Uani 1 1 d . . . . .
C017 C 0.62850(12) 0.01620(14) 0.68090(12) 0.0488(4) Uani 1 1 d . . . . .
H017 H 0.591524 0.004492 0.622363 0.059 Uiso 1 1 calc R U . . .
C006 C 0.61185(11) 0.58113(13) 0.53080(11) 0.0413(3) Uani 1 1 d . . . . .
C018 C 0.65328(13) -0.06835(14) 0.73962(13) 0.0525(4) Uani 1 1 d . . . . .
H018 H 0.633878 -0.138581 0.721374 0.063 Uiso 1 1 calc R U . . .
C001 C 0.88546(11) 0.20672(13) 0.99390(11) 0.0422(3) Uani 1 1 d . . . . .
C011 C 0.54961(13) 0.76235(17) 0.33382(13) 0.0526(4) Uani 1 1 d . . . . .
H011 H 0.526923 0.755479 0.273303 0.063 Uiso 1 1 calc R U . . .
C026 C 0.87787(11) 0.07682(14) 0.78217(11) 0.0434(3) Uani 1 1 d . . . . .
H026 H 0.891093 0.080748 0.841411 0.052 Uiso 1 1 calc R U . . .
C028 C 0.85998(14) 0.45147(15) 0.79376(13) 0.0570(5) Uani 1 1 d . . . . .
C014 C 0.61591(14) 0.78152(15) 0.51239(13) 0.0517(4) Uani 1 1 d . . . . .
H014 H 0.638279 0.789016 0.572835 0.062 Uiso 1 1 calc R U . . .
C013 C 0.60373(15) 0.87244(15) 0.46097(15) 0.0583(5) Uani 1 1 d . . . . .
H013 H 0.617735 0.940717 0.486890 0.070 Uiso 1 1 calc R U . . .
C023 C 0.84132(13) 0.06552(16) 0.60721(12) 0.0498(4) Uani 1 1 d . . . . .
H023 H 0.829644 0.062229 0.548322 0.060 Uiso 1 1 calc R U . . .
C027 C 0.87885(13) 0.35214(15) 0.76031(13) 0.0514(4) Uani 1 1 d . . . . .
H027 H 0.916978 0.350354 0.735232 0.062 Uiso 1 1 calc R U . . .
C019 C 0.70691(12) -0.04763(14) 0.82527(12) 0.0474(4) Uani 1 1 d . . . . .
H019 H 0.724085 -0.103586 0.866202 0.057 Uiso 1 1 calc R U . . .
C032 C 0.77694(17) 0.52583(18) 0.85561(14) 0.0684(6) Uani 1 1 d . . . . .
H032 H 0.735765 0.518269 0.876458 0.082 Uiso 1 1 calc R U . . .
C031 C 0.8129(2) 0.6247(2) 0.8587(2) 0.0913(10) Uani 1 1 d . . . . .
H031 H 0.794939 0.684228 0.880158 0.110 Uiso 1 1 calc R U . . .
C029 C 0.8997(2) 0.5488(2) 0.79621(19) 0.0842(8) Uani 1 1 d . . . . .
H029 H 0.941305 0.554909 0.775817 0.101 Uiso 1 1 calc R U . . .
C030 C 0.8750(3) 0.6381(2) 0.8306(2) 0.1025(12) Uani 1 1 d . . . . .
H030 H 0.900480 0.705654 0.834405 0.123 Uiso 1 1 calc R U . . .
C1A C 0.8720(8) -0.1330(5) 0.6170(8) 0.0498(17) Uani 0.55(3) 1 d DG . P A 1
C2A C 0.8298(8) -0.2206(8) 0.6322(7) 0.071(2) Uani 0.55(3) 1 d G . P A 1
H2A H 0.795666 -0.210035 0.661310 0.085 Uiso 0.55(3) 1 calc R U P A 1
C3A C 0.8385(8) -0.3239(5) 0.6040(7) 0.078(2) Uani 0.55(3) 1 d G . P A 1
H3A H 0.810187 -0.382575 0.614192 0.094 Uiso 0.55(3) 1 calc R U P A 1
C4A C 0.8895(8) -0.3397(7) 0.5606(7) 0.068(2) Uani 0.55(3) 1 d G . P A 1
H4A H 0.895271 -0.408868 0.541679 0.082 Uiso 0.55(3) 1 calc R U P A 1
C5A C 0.9317(7) -0.2521(11) 0.5454(6) 0.065(2) Uani 0.55(3) 1 d G . P A 1
H5A H 0.965835 -0.262623 0.516283 0.078 Uiso 0.55(3) 1 calc R U P A 1
C6A C 0.9230(8) -0.1487(8) 0.5736(8) 0.0578(15) Uani 0.55(3) 1 d G . P A 1
H6A H 0.951315 -0.090082 0.563401 0.069 Uiso 0.55(3) 1 calc R U P A 1
C1B C 0.8797(10) -0.1314(7) 0.6242(10) 0.054(2) Uani 0.45(3) 1 d DG . P A 2
C2B C 0.8478(10) -0.2314(9) 0.6342(7) 0.060(2) Uani 0.45(3) 1 d G . P A 2
H2B H 0.815873 -0.236299 0.666154 0.072 Uiso 0.45(3) 1 calc R U P A 2
C3B C 0.8634(11) -0.3239(6) 0.5965(7) 0.073(3) Uani 0.45(3) 1 d G . P A 2
H3B H 0.842048 -0.390841 0.603227 0.088 Uiso 0.45(3) 1 calc R U P A 2
C4B C 0.9111(10) -0.3165(11) 0.5488(7) 0.068(3) Uani 0.45(3) 1 d G . P A 2
H4B H 0.921582 -0.378498 0.523546 0.081 Uiso 0.45(3) 1 calc R U P A 2
C5B C 0.9431(8) -0.2166(15) 0.5387(8) 0.070(2) Uani 0.45(3) 1 d G . P A 2
H5B H 0.974941 -0.211612 0.506791 0.084 Uiso 0.45(3) 1 calc R U P A 2
C6B C 0.9274(10) -0.1240(11) 0.5764(10) 0.069(2) Uani 0.45(3) 1 d G . P A 2
H6B H 0.948766 -0.057068 0.569718 0.083 Uiso 0.45(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 91.39(7) . . ?
N002 Fe01 N006 95.67(8) . . ?
N001 Fe01 N006 92.76(6) . . ?
N002 Fe01 N005 90.44(7) . . ?
N001 Fe01 N005 91.28(6) . . ?
N006 Fe01 N005 172.59(6) . . ?
N002 Fe01 N003 92.27(6) . . ?
N001 Fe01 N003 170.87(6) . . ?
N006 Fe01 N003 95.19(6) . . ?
N005 Fe01 N003 80.34(5) . . ?
N002 Fe01 N004 175.02(7) . . ?
N001 Fe01 N004 91.41(6) . . ?
N006 Fe01 N004 80.09(7) . . ?
N005 Fe01 N004 93.62(6) . . ?
N003 Fe01 N004 85.57(6) . . ?
C020 N005 C016 117.57(14) . . ?
C020 N005 Fe01 128.47(11) . . ?
C016 N005 Fe01 113.84(10) . . ?
C032 N006 C028 118.8(2) . . ?
C032 N006 Fe01 126.18(18) . . ?
C028 N006 Fe01 114.99(13) . . ?
C015 N003 C003 117.60(13) . . ?
C015 N003 Fe01 114.30(11) . . ?
C003 N003 Fe01 127.54(10) . . ?
C027 N004 C021 118.80(16) . . ?
C027 N004 Fe01 115.13(13) . . ?
C021 N004 Fe01 125.53(11) . . ?
C002 N002 Fe01 169.08(18) . . ?
C001 N001 Fe01 162.47(14) . . ?
N003 C015 C016 117.10(14) . . ?
N005 C016 C017 122.82(15) . . ?
N005 C016 C015 113.79(13) . . ?
C017 C016 C015 123.38(15) . . ?
C004 C003 C008 119.70(15) . . ?
C004 C003 N003 120.46(14) . . ?
C008 C003 N003 119.84(14) . . ?
C022 C021 C026 120.44(16) . . ?
C022 C021 N004 120.32(15) . . ?
C026 C021 N004 119.17(15) . . ?
C023 C024 C025 118.39(16) . . ?
C023 C024 C1B 122.9(6) . . ?
C025 C024 C1B 118.6(6) . . ?
C023 C024 C1A 119.9(5) . . ?
C025 C024 C1A 121.7(5) . . ?
C008 C007 C006 121.33(15) . . ?
C013 C012 C011 119.69(17) . . ?
C009 C010 C011 121.29(18) . . ?
C023 C022 C021 119.72(16) . . ?
C007 C008 C003 119.83(16) . . ?
C026 C025 C024 121.44(16) . . ?
N002 C002 S002 178.51(18) . . ?
C005 C004 C003 119.88(15) . . ?
N005 C020 C019 122.73(16) . . ?
C004 C005 C006 121.40(16) . . ?
C010 C009 C014 117.89(16) . . ?
C010 C009 C006 121.46(16) . . ?
C014 C009 C006 120.62(16) . . ?
C018 C017 C016 118.61(16) . . ?
C007 C006 C005 117.85(15) . . ?
C007 C006 C009 122.03(15) . . ?
C005 C006 C009 120.11(15) . . ?
C019 C018 C017 118.94(16) . . ?
N001 C001 S001 177.15(16) . . ?
C012 C011 C010 119.94(18) . . ?
C025 C026 C021 119.15(16) . . ?
N006 C028 C029 123.0(2) . . ?
N006 C028 C027 113.46(16) . . ?
C029 C028 C027 123.6(2) . . ?
C013 C014 C009 120.82(19) . . ?
C012 C013 C014 120.37(19) . . ?
C022 C023 C024 120.84(16) . . ?
N004 C027 C028 116.22(19) . . ?
C018 C019 C020 119.31(16) . . ?
N006 C032 C031 121.1(3) . . ?
C032 C031 C030 121.0(3) . . ?
C028 C029 C030 117.2(3) . . ?
C031 C030 C029 118.9(2) . . ?
C2A C1A C6A 120.0 . . ?
C2A C1A C024 116.1(6) . . ?
C6A C1A C024 123.6(6) . . ?
C1A C2A C3A 120.0 . . ?
C4A C3A C2A 120.0 . . ?
C3A C4A C5A 120.0 . . ?
C4A C5A C6A 120.0 . . ?
C5A C6A C1A 120.0 . . ?
C2B C1B C6B 120.0 . . ?
C2B C1B C024 125.9(8) . . ?
C6B C1B C024 114.1(8) . . ?
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 1.9302(18) . ?
Fe01 N001 1.9530(15) . ?
Fe01 N006 1.9596(17) . ?
Fe01 N005 1.9845(13) . ?
Fe01 N003 1.9926(13) . ?
Fe01 N004 1.9990(15) . ?
S002 C002 1.619(2) . ?
S001 C001 1.6206(18) . ?
N005 C020 1.330(2) . ?
N005 C016 1.342(2) . ?
N006 C032 1.332(3) . ?
N006 C028 1.350(3) . ?
N003 C015 1.278(2) . ?
N003 C003 1.4219(19) . ?
N004 C027 1.274(2) . ?
N004 C021 1.420(2) . ?
N002 C002 1.156(3) . ?
N001 C001 1.147(2) . ?
C015 C016 1.441(2) . ?
C016 C017 1.375(2) . ?
C003 C004 1.376(2) . ?
C003 C008 1.379(2) . ?
C021 C022 1.377(2) . ?
C021 C026 1.378(2) . ?
C024 C023 1.382(3) . ?
C024 C025 1.383(2) . ?
C024 C1B 1.458(7) . ?
C024 C1A 1.493(5) . ?
C007 C008 1.377(2) . ?
C007 C006 1.380(2) . ?
C012 C013 1.369(3) . ?
C012 C011 1.370(3) . ?
C010 C009 1.377(2) . ?
C010 C011 1.382(3) . ?
C022 C023 1.374(3) . ?
C025 C026 1.373(2) . ?
C004 C005 1.374(2) . ?
C020 C019 1.372(2) . ?
C005 C006 1.385(2) . ?
C009 C014 1.388(2) . ?
C009 C006 1.478(2) . ?
C017 C018 1.374(3) . ?
C018 C019 1.367(3) . ?
C028 C029 1.373(3) . ?
C028 C027 1.444(3) . ?
C014 C013 1.377(3) . ?
C032 C031 1.358(4) . ?
C031 C030 1.364(5) . ?
C029 C030 1.397(5) . ?
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 . ?
