#------------------------------------------------------------------------------
#$Date: 2023-10-07 02:57:14 +0300 (Sat, 07 Oct 2023) $
#$Revision: 286839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/21/2312176.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_2312176
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                 115.8437(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.38880(10)
_cell_length_b                   12.25120(10)
_cell_length_c                   16.90920(10)
_cell_measurement_reflns_used    18116
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.789
_cell_measurement_theta_min      1.884
_cell_volume                     3241.96(4)
_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 0.940
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.63582
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.940
_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            24298
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        22.426
_diffrn_reflns_theta_max         25.080
_diffrn_reflns_theta_min         1.889
_exptl_absorpt_coefficient_mu    0.464
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1424
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.0056(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   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         7566
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0332
_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)+(0.0506P)²+0.9083P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.0993
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6976
_reflns_number_total             7566
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Bia_Pmono_174K.cif
_cod_data_source_block           SC2_174K
_cod_depositor_comments
'Adding full bibliography for 2312165--2312274.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2312176
_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 0.75477(2) 0.28958(2) 0.81443(2) 0.03137(8) Uani 1 1 d . . . . .
S002 S 0.54618(3) 0.33203(3) 0.91715(3) 0.04056(10) Uani 1 1 d . . . . .
S001 S 0.94762(3) 0.13732(4) 1.07841(3) 0.04717(11) Uani 1 1 d . . . . .
N005 N 0.71367(8) 0.13840(9) 0.79464(7) 0.0308(2) Uani 1 1 d . . . . .
N006 N 0.79780(9) 0.43763(10) 0.82385(8) 0.0405(3) Uani 1 1 d . . . . .
N003 N 0.66939(8) 0.30257(9) 0.69178(8) 0.0322(2) Uani 1 1 d . . . . .
N004 N 0.83855(8) 0.26627(10) 0.76752(8) 0.0350(3) Uani 1 1 d . . . . .
N002 N 0.67182(9) 0.32482(11) 0.85778(8) 0.0407(3) Uani 1 1 d . . . . .
N001 N 0.83895(8) 0.25483(10) 0.93235(8) 0.0371(3) Uani 1 1 d . . . . .
C015 C 0.63561(10) 0.21203(11) 0.65532(9) 0.0351(3) Uani 1 1 d . . . . .
H015 H 0.597851 0.207948 0.596023 0.042 Uiso 1 1 calc R U . . .
C016 C 0.65907(9) 0.11700(11) 0.71079(9) 0.0336(3) Uani 1 1 d . . . . .
C003 C 0.64994(9) 0.39700(11) 0.63732(9) 0.0337(3) Uani 1 1 d . . . . .
C021 C 0.85073(10) 0.16715(12) 0.73085(10) 0.0351(3) Uani 1 1 d . . . . .
C024 C 0.86594(10) -0.02931(13) 0.65814(10) 0.0387(3) Uani 1 1 d D . . . .
C007 C 0.60298(10) 0.58205(12) 0.60888(10) 0.0384(3) Uani 1 1 d . . . . .
H007 H 0.583533 0.644796 0.625361 0.046 Uiso 1 1 calc R U . . .
C012 C 0.57146(12) 0.86576(13) 0.37320(12) 0.0456(4) Uani 1 1 d . . . . .
H012 H 0.563962 0.927694 0.338803 0.055 Uiso 1 1 calc R U . . .
C010 C 0.56212(10) 0.67263(13) 0.38574(10) 0.0393(3) Uani 1 1 d . . . . .
H010 H 0.547774 0.604484 0.359048 0.047 Uiso 1 1 calc R U . . .
C022 C 0.83250(11) 0.16187(13) 0.64309(10) 0.0407(3) Uani 1 1 d . . . . .
H022 H 0.814808 0.224041 0.608188 0.049 Uiso 1 1 calc R U . . .
C008 C 0.62216(10) 0.49090(12) 0.66199(10) 0.0369(3) Uani 1 1 d . . . . .
H008 H 0.616407 0.492693 0.714138 0.044 Uiso 1 1 calc R U . . .
C025 C 0.88373(10) -0.02198(13) 0.74606(10) 0.0396(3) Uani 1 1 d . . . . .
H025 H 0.900473 -0.084279 0.780905 0.048 Uiso 1 1 calc R U . . .
C002 C 0.61986(10) 0.32812(11) 0.88281(9) 0.0349(3) Uani 1 1 d . . . . .
C004 C 0.65818(10) 0.39469(12) 0.56016(10) 0.0377(3) Uani 1 1 d . . . . .
H004 H 0.676531 0.331393 0.543215 0.045 Uiso 1 1 calc R U . . .
C020 C 0.73602(10) 0.05588(12) 0.85163(10) 0.0365(3) Uani 1 1 d . . . . .
H020 H 0.772300 0.069738 0.910279 0.044 Uiso 1 1 calc R U . . .
C005 C 0.63917(11) 0.48649(12) 0.50794(10) 0.0391(3) Uani 1 1 d . . . . .
H005 H 0.644655 0.484235 0.455660 0.047 Uiso 1 1 calc R U . . .
C009 C 0.59559(10) 0.68031(12) 0.47624(10) 0.0357(3) Uani 1 1 d . . . . .
C017 C 0.62780(11) 0.01416(12) 0.68192(10) 0.0411(3) Uani 1 1 d . . . . .
H017 H 0.590268 0.002083 0.623366 0.049 Uiso 1 1 calc R U . . .
C006 C 0.61209(10) 0.58194(11) 0.53164(9) 0.0354(3) Uani 1 1 d . . . . .
C018 C 0.65306(11) -0.07060(12) 0.74128(11) 0.0443(4) Uani 1 1 d . . . . .
H018 H 0.633525 -0.141200 0.723505 0.053 Uiso 1 1 calc R U . . .
C001 C 0.88467(10) 0.20858(11) 0.99407(10) 0.0348(3) Uani 1 1 d . . . . .
C011 C 0.54967(11) 0.76466(14) 0.33443(11) 0.0444(4) Uani 1 1 d . . . . .
H011 H 0.526541 0.758248 0.273612 0.053 Uiso 1 1 calc R U . . .
C026 C 0.87722(10) 0.07519(12) 0.78295(10) 0.0377(3) Uani 1 1 d . . . . .
H026 H 0.890521 0.079060 0.842441 0.045 Uiso 1 1 calc R U . . .
C028 C 0.85833(12) 0.45069(13) 0.79513(11) 0.0476(4) Uani 1 1 d . . . . .
C014 C 0.61625(12) 0.78298(12) 0.51408(11) 0.0436(4) Uani 1 1 d . . . . .
H014 H 0.638445 0.790076 0.574786 0.052 Uiso 1 1 calc R U . . .
C013 C 0.60429(13) 0.87479(13) 0.46279(12) 0.0485(4) Uani 1 1 d . . . . .
H013 H 0.618569 0.943149 0.489131 0.058 Uiso 1 1 calc R U . . .
C023 C 0.84060(11) 0.06409(14) 0.60728(10) 0.0431(3) Uani 1 1 d . . . . .
H023 H 0.828887 0.060818 0.548160 0.052 Uiso 1 1 calc R U . . .
C027 C 0.87784(11) 0.35169(13) 0.76169(11) 0.0442(4) Uani 1 1 d . . . . .
H027 H 0.916603 0.350069 0.737389 0.053 Uiso 1 1 calc R U . . .
C019 C 0.70753(11) -0.04880(12) 0.82702(11) 0.0409(3) Uani 1 1 d . . . . .
H019 H 0.725154 -0.104657 0.868409 0.049 Uiso 1 1 calc R U . . .
C032 C 0.77477(13) 0.52432(13) 0.85628(11) 0.0517(4) Uani 1 1 d . . . . .
H032 H 0.733364 0.516492 0.876754 0.062 Uiso 1 1 calc R U . . .
C031 C 0.81120(18) 0.62518(15) 0.85999(15) 0.0706(7) Uani 1 1 d . . . . .
H031 H 0.793290 0.684818 0.881677 0.085 Uiso 1 1 calc R U . . .
C029 C 0.89772(17) 0.54934(16) 0.79828(15) 0.0680(6) Uani 1 1 d . . . . .
H029 H 0.939507 0.555763 0.778183 0.082 Uiso 1 1 calc R U . . .
C030 C 0.8734(2) 0.63824(17) 0.83206(17) 0.0797(8) Uani 1 1 d . . . . .
H030 H 0.898936 0.705937 0.835750 0.096 Uiso 1 1 calc R U . . .
C1A C 0.8727(8) -0.1350(5) 0.6171(8) 0.0423(15) Uani 0.53(3) 1 d DG . P A 1
C2A C 0.8315(7) -0.2236(7) 0.6331(7) 0.0599(19) Uani 0.53(3) 1 d G . P A 1
H2A H 0.797665 -0.213480 0.662550 0.072 Uiso 0.53(3) 1 calc R U P A 1
C3A C 0.8408(7) -0.3272(5) 0.6050(7) 0.0658(18) Uani 0.53(3) 1 d G . P A 1
H3A H 0.813191 -0.386497 0.615621 0.079 Uiso 0.53(3) 1 calc R U P A 1
C4A C 0.8913(7) -0.3424(7) 0.5609(7) 0.0585(19) Uani 0.53(3) 1 d G . P A 1
H4A H 0.897524 -0.411714 0.542076 0.070 Uiso 0.53(3) 1 calc R U P A 1
C5A C 0.9325(7) -0.2538(10) 0.5449(6) 0.0549(18) Uani 0.53(3) 1 d G . P A 1
H5A H 0.966331 -0.263913 0.515458 0.066 Uiso 0.53(3) 1 calc R U P A 1
C6A C 0.9232(7) -0.1501(8) 0.5731(7) 0.0491(13) Uani 0.53(3) 1 d G . P A 1
H6A H 0.950805 -0.090895 0.562386 0.059 Uiso 0.53(3) 1 calc R U P A 1
C1B C 0.8797(9) -0.1336(6) 0.6249(9) 0.0454(18) Uani 0.47(3) 1 d DG . P A 2
C2B C 0.8468(9) -0.2336(8) 0.6343(7) 0.0509(17) Uani 0.47(3) 1 d G . P A 2
H2B H 0.814402 -0.238201 0.665758 0.061 Uiso 0.47(3) 1 calc R U P A 2
C3B C 0.8624(10) -0.3268(6) 0.5967(6) 0.062(2) Uani 0.47(3) 1 d G . P A 2
H3B H 0.840414 -0.393719 0.602927 0.074 Uiso 0.47(3) 1 calc R U P A 2
C4B C 0.9108(9) -0.3199(10) 0.5496(7) 0.057(2) Uani 0.47(3) 1 d G . P A 2
H4B H 0.921256 -0.382283 0.524460 0.069 Uiso 0.47(3) 1 calc R U P A 2
C5B C 0.9437(7) -0.2199(13) 0.5403(7) 0.0603(19) Uani 0.47(3) 1 d G . P A 2
H5B H 0.976087 -0.215330 0.508822 0.072 Uiso 0.47(3) 1 calc R U P A 2
C6B C 0.9281(9) -0.1267(10) 0.5779(9) 0.0582(18) Uani 0.47(3) 1 d G . P A 2
H6B H 0.950076 -0.059810 0.571652 0.070 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 90.73(6) . . ?
N002 Fe01 N006 94.87(6) . . ?
N001 Fe01 N006 91.69(5) . . ?
N002 Fe01 N004 175.33(5) . . ?
N001 Fe01 N004 91.32(5) . . ?
N006 Fe01 N004 80.88(6) . . ?
N002 Fe01 N005 89.94(5) . . ?
N001 Fe01 N005 91.36(5) . . ?
N006 Fe01 N005 174.26(5) . . ?
N004 Fe01 N005 94.20(5) . . ?
N002 Fe01 N003 92.12(5) . . ?
N001 Fe01 N003 171.89(5) . . ?
N006 Fe01 N003 95.62(5) . . ?
N004 Fe01 N003 86.42(5) . . ?
N005 Fe01 N003 81.06(5) . . ?
C020 N005 C016 117.65(12) . . ?
C020 N005 Fe01 128.58(10) . . ?
C016 N005 Fe01 113.67(9) . . ?
C032 N006 C028 118.38(15) . . ?
C032 N006 Fe01 127.09(14) . . ?
C028 N006 Fe01 114.52(11) . . ?
C015 N003 C003 117.54(12) . . ?
C015 N003 Fe01 114.57(10) . . ?
C003 N003 Fe01 127.33(9) . . ?
C027 N004 C021 118.70(14) . . ?
C027 N004 Fe01 115.40(12) . . ?
C021 N004 Fe01 125.43(10) . . ?
C002 N002 Fe01 169.01(13) . . ?
C001 N001 Fe01 163.07(12) . . ?
N003 C015 C016 116.56(13) . . ?
N005 C016 C017 122.78(13) . . ?
N005 C016 C015 113.52(12) . . ?
C017 C016 C015 123.68(13) . . ?
C004 C003 C008 119.96(13) . . ?
C004 C003 N003 120.24(13) . . ?
C008 C003 N003 119.80(13) . . ?
C022 C021 C026 120.37(14) . . ?
C022 C021 N004 120.16(13) . . ?
C026 C021 N004 119.41(13) . . ?
C023 C024 C025 118.43(15) . . ?
C023 C024 C1B 123.2(5) . . ?
C025 C024 C1B 118.3(5) . . ?
C023 C024 C1A 119.7(5) . . ?
C025 C024 C1A 121.9(5) . . ?
C008 C007 C006 121.28(14) . . ?
C013 C012 C011 119.67(15) . . ?
C011 C010 C009 120.98(15) . . ?
C023 C022 C021 119.68(14) . . ?
C007 C008 C003 119.66(14) . . ?
C026 C025 C024 121.41(14) . . ?
N002 C002 S002 179.42(15) . . ?
C003 C004 C005 119.77(14) . . ?
N005 C020 C019 122.47(14) . . ?
C004 C005 C006 121.40(14) . . ?
C010 C009 C014 118.17(14) . . ?
C010 C009 C006 121.22(14) . . ?
C014 C009 C006 120.57(14) . . ?
C016 C017 C018 118.78(14) . . ?
C007 C006 C005 117.91(13) . . ?
C007 C006 C009 121.88(13) . . ?
C005 C006 C009 120.19(14) . . ?
C019 C018 C017 118.61(14) . . ?
N001 C001 S001 177.00(14) . . ?
C012 C011 C010 120.05(16) . . ?
C025 C026 C021 119.29(14) . . ?
N006 C028 C029 122.90(19) . . ?
N006 C028 C027 113.36(14) . . ?
C029 C028 C027 123.74(19) . . ?
C013 C014 C009 120.81(16) . . ?
C012 C013 C014 120.32(16) . . ?
C022 C023 C024 120.81(15) . . ?
N004 C027 C028 115.75(16) . . ?
C018 C019 C020 119.68(14) . . ?
N006 C032 C031 121.2(2) . . ?
C030 C031 C032 120.5(2) . . ?
C028 C029 C030 118.1(2) . . ?
C031 C030 C029 118.88(19) . . ?
C2A C1A C6A 120.0 . . ?
C2A C1A C024 115.7(6) . . ?
C6A C1A C024 124.0(6) . . ?
C3A C2A C1A 120.0 . . ?
C2A C3A C4A 120.0 . . ?
C5A C4A C3A 120.0 . . ?
C6A C5A C4A 120.0 . . ?
C5A C6A C1A 120.0 . . ?
C2B C1B C6B 120.0 . . ?
C2B C1B C024 125.8(7) . . ?
C6B C1B C024 114.2(7) . . ?
C3B C2B C1B 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 1.9303(15) . ?
Fe01 N001 1.9379(12) . ?
Fe01 N006 1.9420(13) . ?
Fe01 N004 1.9599(14) . ?
Fe01 N005 1.9608(11) . ?
Fe01 N003 1.9612(12) . ?
S002 C002 1.6214(17) . ?
S001 C001 1.6226(15) . ?
N005 C020 1.3323(18) . ?
N005 C016 1.3442(18) . ?
N006 C032 1.334(2) . ?
N006 C028 1.347(2) . ?
N003 C015 1.2805(18) . ?
N003 C003 1.4246(17) . ?
N004 C027 1.277(2) . ?
N004 C021 1.4207(19) . ?
N002 C002 1.154(2) . ?
N001 C001 1.148(2) . ?
C015 C016 1.4381(19) . ?
C016 C017 1.3747(19) . ?
C003 C004 1.373(2) . ?
C003 C008 1.381(2) . ?
C021 C022 1.377(2) . ?
C021 C026 1.380(2) . ?
C024 C023 1.383(2) . ?
C024 C025 1.383(2) . ?
C024 C1B 1.456(6) . ?
C024 C1A 1.498(5) . ?
C007 C008 1.380(2) . ?
C007 C006 1.383(2) . ?
C012 C013 1.371(3) . ?
C012 C011 1.375(2) . ?
C010 C011 1.381(2) . ?
C010 C009 1.383(2) . ?
C022 C023 1.377(2) . ?
C025 C026 1.371(2) . ?
C004 C005 1.378(2) . ?
C020 C019 1.373(2) . ?
C005 C006 1.383(2) . ?
C009 C014 1.386(2) . ?
C009 C006 1.4758(19) . ?
C017 C018 1.376(2) . ?
C018 C019 1.369(2) . ?
C028 C029 1.379(2) . ?
C028 C027 1.440(2) . ?
C014 C013 1.380(2) . ?
C032 C031 1.377(3) . ?
C031 C030 1.365(4) . ?
C029 C030 1.379(4) . ?
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 . ?
