#------------------------------------------------------------------------------
#$Date: 2023-10-07 02:57:14 +0300 (Sat, 07 Oct 2023) $
#$Revision: 286839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/21/2312168.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_2312168
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                 115.7793(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2809(2)
_cell_length_b                   12.47180(10)
_cell_length_c                   17.2385(2)
_cell_measurement_reflns_used    11075
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.215
_cell_measurement_theta_min      1.861
_cell_volume                     3345.55(7)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.970
_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  0.0303
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.970
_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            25099
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        22.426
_diffrn_reflns_theta_max         25.080
_diffrn_reflns_theta_min         1.872
_exptl_absorpt_coefficient_mu    0.450
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1424
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.0080(7)
_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   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         7802
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0375
_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)+(0.0585P)²+0.5810P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6750
_reflns_number_total             7802
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Bia_Pmono_249K.cif
_cod_data_source_block           SC2_249K
_cod_depositor_comments
'Adding full bibliography for 2312165--2312274.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2312168
_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 0.75886(2) 0.30365(2) 0.82507(2) 0.05177(9) Uani 1 1 d . . . . .
S002 S 0.54529(3) 0.34255(4) 0.92182(3) 0.06949(14) Uani 1 1 d . . . . .
S001 S 0.95209(4) 0.11522(4) 1.07030(4) 0.07635(15) Uani 1 1 d . . . . .
N005 N 0.71078(9) 0.14293(10) 0.79368(8) 0.0505(3) Uani 1 1 d . . . . .
N006 N 0.81108(11) 0.45684(12) 0.82150(9) 0.0657(4) Uani 1 1 d . . . . .
N003 N 0.66765(9) 0.31058(10) 0.68788(8) 0.0509(3) Uani 1 1 d . . . . .
N004 N 0.84825(9) 0.27523(10) 0.76623(8) 0.0506(3) Uani 1 1 d . . . . .
N002 N 0.67157(13) 0.36100(17) 0.86622(12) 0.0800(5) Uani 1 1 d . . . . .
N001 N 0.84773(11) 0.25466(13) 0.94410(9) 0.0654(4) Uani 1 1 d . . . . .
C015 C 0.63950(11) 0.21944(13) 0.65527(10) 0.0553(4) Uani 1 1 d . . . . .
H015 H 0.604781 0.212968 0.596472 0.066 Uiso 1 1 calc R U . . .
C016 C 0.66163(10) 0.12553(13) 0.70997(10) 0.0525(3) Uani 1 1 d . . . . .
C003 C 0.64812(10) 0.40003(12) 0.63186(10) 0.0511(3) Uani 1 1 d . . . . .
C021 C 0.85777(10) 0.17781(13) 0.72917(10) 0.0507(3) Uani 1 1 d . . . . .
C024 C 0.86632(11) -0.01637(14) 0.65577(11) 0.0569(4) Uani 1 1 d D . . . .
C007 C 0.60392(12) 0.58296(14) 0.60234(11) 0.0603(4) Uani 1 1 d . . . . .
H007 H 0.586233 0.646105 0.618470 0.072 Uiso 1 1 calc R U . . .
C012 C 0.56863(15) 0.85298(18) 0.36477(15) 0.0782(6) Uani 1 1 d . . . . .
H012 H 0.561227 0.912668 0.329899 0.094 Uiso 1 1 calc R U . . .
C010 C 0.55978(12) 0.66457(16) 0.38069(12) 0.0634(4) Uani 1 1 d . . . . .
H010 H 0.545334 0.597006 0.355649 0.076 Uiso 1 1 calc R U . . .
C022 C 0.83950(12) 0.17209(14) 0.64290(11) 0.0585(4) Uani 1 1 d . . . . .
H022 H 0.823851 0.233675 0.609140 0.070 Uiso 1 1 calc R U . . .
C008 C 0.62373(12) 0.49547(14) 0.65593(11) 0.0584(4) Uani 1 1 d . . . . .
H008 H 0.620776 0.500303 0.708411 0.070 Uiso 1 1 calc R U . . .
C025 C 0.88373(11) -0.00957(14) 0.74178(11) 0.0569(4) Uani 1 1 d . . . . .
H025 H 0.898399 -0.071300 0.775396 0.068 Uiso 1 1 calc R U . . .
C002 C 0.61915(13) 0.35261(14) 0.88961(11) 0.0591(4) Uani 1 1 d . . . . .
C004 C 0.65352(12) 0.39473(13) 0.55513(11) 0.0582(4) Uani 1 1 d . . . . .
H004 H 0.670070 0.331069 0.538556 0.070 Uiso 1 1 calc R U . . .
C020 C 0.73106(12) 0.05933(14) 0.84656(11) 0.0585(4) Uani 1 1 d . . . . .
H020 H 0.764323 0.070858 0.905099 0.070 Uiso 1 1 calc R U . . .
C005 C 0.63465(12) 0.48287(14) 0.50252(11) 0.0598(4) Uani 1 1 d . . . . .
H005 H 0.638670 0.477972 0.450564 0.072 Uiso 1 1 calc R U . . .
C009 C 0.59315(11) 0.67425(13) 0.46888(12) 0.0572(4) Uani 1 1 d . . . . .
C017 C 0.63362(13) 0.02501(15) 0.67797(12) 0.0672(5) Uani 1 1 d . . . . .
H017 H 0.599774 0.014938 0.619350 0.081 Uiso 1 1 calc R U . . .
C006 C 0.60973(11) 0.57909(13) 0.52498(11) 0.0550(4) Uani 1 1 d . . . . .
C018 C 0.65611(14) -0.06055(15) 0.73343(14) 0.0735(5) Uani 1 1 d . . . . .
H018 H 0.638077 -0.129486 0.712999 0.088 Uiso 1 1 calc R U . . .
C001 C 0.89159(12) 0.19757(13) 0.99754(11) 0.0558(4) Uani 1 1 d . . . . .
C011 C 0.54742(14) 0.75317(18) 0.32887(14) 0.0723(5) Uani 1 1 d . . . . .
H011 H 0.524612 0.745070 0.269402 0.087 Uiso 1 1 calc R U . . .
C026 C 0.87978(10) 0.08665(13) 0.77851(10) 0.0531(3) Uani 1 1 d . . . . .
H026 H 0.891968 0.089996 0.836588 0.064 Uiso 1 1 calc R U . . .
C028 C 0.86706(13) 0.46038(15) 0.78682(12) 0.0675(5) Uani 1 1 d . . . . .
C014 C 0.61256(15) 0.77624(16) 0.50331(14) 0.0727(5) Uani 1 1 d . . . . .
H014 H 0.634149 0.785285 0.562602 0.087 Uiso 1 1 calc R U . . .
C013 C 0.60058(17) 0.86468(17) 0.45159(16) 0.0839(6) Uani 1 1 d . . . . .
H013 H 0.614362 0.932582 0.476098 0.101 Uiso 1 1 calc R U . . .
C023 C 0.84440(12) 0.07590(15) 0.60703(11) 0.0632(4) Uani 1 1 d . . . . .
H023 H 0.832797 0.072830 0.549093 0.076 Uiso 1 1 calc R U . . .
C027 C 0.88222(12) 0.35982(14) 0.75444(12) 0.0620(4) Uani 1 1 d . . . . .
H027 H 0.916517 0.357156 0.725255 0.074 Uiso 1 1 calc R U . . .
C019 C 0.70525(13) -0.04286(15) 0.81884(13) 0.0670(5) Uani 1 1 d . . . . .
H019 H 0.721045 -0.099500 0.857790 0.080 Uiso 1 1 calc R U . . .
C032 C 0.79409(19) 0.54815(18) 0.85188(14) 0.0901(7) Uani 1 1 d . . . . .
H032 H 0.754982 0.547578 0.875619 0.108 Uiso 1 1 calc R U . . .
C031 C 0.8336(3) 0.6432(2) 0.8486(2) 0.1184(12) Uani 1 1 d . . . . .
H031 H 0.820653 0.705976 0.869698 0.142 Uiso 1 1 calc R U . . .
C029 C 0.90899(19) 0.55308(18) 0.78275(18) 0.0974(8) Uani 1 1 d . . . . .
H029 H 0.948038 0.552385 0.758937 0.117 Uiso 1 1 calc R U . . .
C030 C 0.8919(3) 0.6451(2) 0.8143(2) 0.1230(12) Uani 1 1 d . . . . .
H030 H 0.919268 0.708643 0.812681 0.148 Uiso 1 1 calc R U . . .
C1A C 0.8730(6) -0.1236(5) 0.6206(6) 0.064(2) Uani 0.52(3) 1 d DG . P A 1
C2A C 0.8255(7) -0.2074(6) 0.6313(6) 0.094(2) Uani 0.52(3) 1 d G . P A 1
H2A H 0.790537 -0.195371 0.659032 0.113 Uiso 0.52(3) 1 calc R U P A 1
C3A C 0.8301(9) -0.3091(5) 0.6007(7) 0.107(3) Uani 0.52(3) 1 d G . P A 1
H3A H 0.798308 -0.365148 0.607869 0.128 Uiso 0.52(3) 1 calc R U P A 1
C4A C 0.8823(8) -0.3271(8) 0.5593(7) 0.097(3) Uani 0.52(3) 1 d G . P A 1
H4A H 0.885417 -0.395142 0.538803 0.116 Uiso 0.52(3) 1 calc R U P A 1
C5A C 0.9298(6) -0.2433(12) 0.5486(7) 0.091(3) Uani 0.52(3) 1 d G . P A 1
H5A H 0.964756 -0.255360 0.520899 0.110 Uiso 0.52(3) 1 calc R U P A 1
C6A C 0.9252(5) -0.1416(10) 0.5792(7) 0.0774(19) Uani 0.52(3) 1 d G . P A 1
H6A H 0.956987 -0.085582 0.572061 0.093 Uiso 0.52(3) 1 calc R U P A 1
C1B C 0.8750(7) -0.1159(6) 0.6156(6) 0.076(3) Uani 0.48(3) 1 d DG . P A 2
C2B C 0.8438(9) -0.2136(7) 0.6286(6) 0.087(2) Uani 0.48(3) 1 d G . P A 2
H2B H 0.811532 -0.216530 0.659926 0.105 Uiso 0.48(3) 1 calc R U P A 2
C3B C 0.8608(13) -0.3071(6) 0.5948(6) 0.102(3) Uani 0.48(3) 1 d G . P A 2
H3B H 0.839906 -0.372456 0.603521 0.123 Uiso 0.48(3) 1 calc R U P A 2
C4B C 0.9090(11) -0.3027(10) 0.5480(6) 0.098(3) Uani 0.48(3) 1 d G . P A 2
H4B H 0.920339 -0.365244 0.525392 0.117 Uiso 0.48(3) 1 calc R U P A 2
C5B C 0.9402(7) -0.2050(13) 0.5350(7) 0.095(3) Uani 0.48(3) 1 d G . P A 2
H5B H 0.972400 -0.202106 0.503668 0.114 Uiso 0.48(3) 1 calc R U P A 2
C6B C 0.9232(7) -0.1116(10) 0.5688(8) 0.0809(19) Uani 0.48(3) 1 d G . P A 2
H6B H 0.944027 -0.046179 0.560073 0.097 Uiso 0.48(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
N001 Fe01 N002 95.80(7) . . ?
N001 Fe01 N006 98.88(6) . . ?
N002 Fe01 N006 94.70(8) . . ?
N001 Fe01 N005 90.76(6) . . ?
N002 Fe01 N005 98.64(7) . . ?
N006 Fe01 N005 162.67(6) . . ?
N001 Fe01 N003 164.19(6) . . ?
N002 Fe01 N003 93.85(6) . . ?
N006 Fe01 N003 92.77(5) . . ?
N005 Fe01 N003 75.40(5) . . ?
N001 Fe01 N004 92.44(6) . . ?
N002 Fe01 N004 167.71(7) . . ?
N006 Fe01 N004 74.99(6) . . ?
N005 Fe01 N004 90.32(5) . . ?
N003 Fe01 N004 80.23(5) . . ?
C020 N005 C016 117.90(14) . . ?
C020 N005 Fe01 127.04(11) . . ?
C016 N005 Fe01 114.73(10) . . ?
C032 N006 C028 118.0(2) . . ?
C032 N006 Fe01 125.83(18) . . ?
C028 N006 Fe01 116.12(12) . . ?
C015 N003 C003 118.16(14) . . ?
C015 N003 Fe01 113.50(11) . . ?
C003 N003 Fe01 127.62(10) . . ?
C027 N004 C021 119.34(15) . . ?
C027 N004 Fe01 113.87(12) . . ?
C021 N004 Fe01 125.83(10) . . ?
C002 N002 Fe01 154.37(18) . . ?
C001 N001 Fe01 158.80(15) . . ?
N003 C015 C016 119.68(15) . . ?
N005 C016 C017 122.05(15) . . ?
N005 C016 C015 115.86(14) . . ?
C017 C016 C015 122.09(15) . . ?
C004 C003 C008 119.27(15) . . ?
C004 C003 N003 121.67(14) . . ?
C008 C003 N003 119.06(14) . . ?
C026 C021 C022 119.80(15) . . ?
C026 C021 N004 119.16(14) . . ?
C022 C021 N004 120.88(14) . . ?
C023 C024 C025 118.50(16) . . ?
C023 C024 C1B 118.6(4) . . ?
C025 C024 C1B 122.8(4) . . ?
C023 C024 C1A 123.4(4) . . ?
C025 C024 C1A 118.1(4) . . ?
C008 C007 C006 121.35(15) . . ?
C013 C012 C011 119.78(19) . . ?
C009 C010 C011 121.19(19) . . ?
C023 C022 C021 120.10(16) . . ?
C007 C008 C003 120.04(15) . . ?
C026 C025 C024 121.17(15) . . ?
N002 C002 S002 179.18(18) . . ?
C003 C004 C005 120.29(15) . . ?
N005 C020 C019 122.95(16) . . ?
C004 C005 C006 121.52(16) . . ?
C010 C009 C014 117.51(17) . . ?
C010 C009 C006 121.39(16) . . ?
C014 C009 C006 121.08(17) . . ?
C016 C017 C018 119.20(17) . . ?
C007 C006 C005 117.52(15) . . ?
C007 C006 C009 121.94(15) . . ?
C005 C006 C009 120.51(15) . . ?
C019 C018 C017 118.86(17) . . ?
N001 C001 S001 178.43(16) . . ?
C012 C011 C010 120.1(2) . . ?
C021 C026 C025 119.67(15) . . ?
N006 C028 C029 123.1(2) . . ?
N006 C028 C027 115.56(16) . . ?
C029 C028 C027 121.3(2) . . ?
C013 C014 C009 121.3(2) . . ?
C012 C013 C014 120.1(2) . . ?
C022 C023 C024 120.75(16) . . ?
N004 C027 C028 119.19(18) . . ?
C018 C019 C020 119.02(17) . . ?
N006 C032 C031 121.2(3) . . ?
C030 C031 C032 120.0(3) . . ?
C030 C029 C028 118.5(3) . . ?
C029 C030 C031 119.2(3) . . ?
C2A C1A C6A 120.0 . . ?
C2A C1A C024 117.7(5) . . ?
C6A C1A C024 122.3(5) . . ?
C1A C2A C3A 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 122.8(6) . . ?
C6B C1B C024 116.9(6) . . ?
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 N001 2.0496(15) . ?
Fe01 N002 2.0545(18) . ?
Fe01 N006 2.1253(16) . ?
Fe01 N005 2.1472(13) . ?
Fe01 N003 2.2005(13) . ?
Fe01 N004 2.2145(14) . ?
S002 C002 1.603(2) . ?
S001 C001 1.6064(18) . ?
N005 C020 1.328(2) . ?
N005 C016 1.336(2) . ?
N006 C032 1.338(3) . ?
N006 C028 1.341(3) . ?
N003 C015 1.268(2) . ?
N003 C003 1.417(2) . ?
N004 C027 1.266(2) . ?
N004 C021 1.415(2) . ?
N002 C002 1.145(3) . ?
N001 C001 1.150(2) . ?
C015 C016 1.447(2) . ?
C016 C017 1.370(2) . ?
C003 C004 1.368(2) . ?
C003 C008 1.385(2) . ?
C021 C026 1.371(2) . ?
C021 C022 1.381(2) . ?
C024 C023 1.377(2) . ?
C024 C025 1.381(2) . ?
C024 C1B 1.460(6) . ?
C024 C1A 1.494(5) . ?
C007 C008 1.374(2) . ?
C007 C006 1.381(2) . ?
C012 C013 1.359(3) . ?
C012 C011 1.367(3) . ?
C010 C009 1.377(3) . ?
C010 C011 1.378(3) . ?
C022 C023 1.369(3) . ?
C025 C026 1.372(2) . ?
C004 C005 1.371(2) . ?
C020 C019 1.366(2) . ?
C005 C006 1.386(2) . ?
C009 C014 1.382(3) . ?
C009 C006 1.478(2) . ?
C017 C018 1.371(3) . ?
C018 C019 1.360(3) . ?
C028 C029 1.382(3) . ?
C028 C027 1.442(3) . ?
C014 C013 1.376(3) . ?
C032 C031 1.381(4) . ?
C031 C030 1.373(5) . ?
C029 C030 1.357(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 . ?
