#------------------------------------------------------------------------------
#$Date: 2023-10-07 02:57:14 +0300 (Sat, 07 Oct 2023) $
#$Revision: 286839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/22/2312267.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_2312267
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            'C10.86 H8 Fe0.29 N1.71 S0.57'
_chemical_formula_weight         196.75
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/2
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            14
_cell_length_a                   12.9604(6)
_cell_length_b                   15.2712(7)
_cell_length_c                   17.5958(6)
_cell_measurement_reflns_used    2498
_cell_measurement_temperature    325(2)
_cell_measurement_theta_max      20.211
_cell_measurement_theta_min      1.887
_cell_volume                     3482.6(3)
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.830
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.65524
_diffrn_reflns_av_R_equivalents  0.1011
_diffrn_reflns_av_unetI/netI     0.0760
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.830
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            36708
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.830
_diffrn_reflns_theta_full        23.150
_diffrn_reflns_theta_max         32.912
_diffrn_reflns_theta_min         1.900
_exptl_absorpt_coefficient_mu    0.432
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1424
_refine_diff_density_max         0.160
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.033
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         6914
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.2561
_refine_ls_R_factor_gt           0.1158
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0346P)²+1.3523P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1635
_refine_ls_wR_factor_ref         0.2061
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2668
_reflns_number_total             6914
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Bia_Portho_325K.cif
_cod_data_source_block           Bia_dw4400_325K
_cod_depositor_comments
'Adding full bibliography for 2312165--2312274.cif.'
_cod_database_code               2312267
_shelx_shelxl_version_number     2019/2
_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+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, 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 0.750000 0.750000 0.57560(4) 0.0750(3) Uani 1 2 d S T P . .
S002 S 0.90800(12) 0.55796(11) 0.39551(7) 0.1306(6) Uani 1 1 d . . . . .
N003 N 0.7438(3) 0.84304(19) 0.67414(16) 0.0768(8) Uani 1 1 d . . . . .
N004 N 0.8006(3) 0.6614(2) 0.49601(18) 0.0976(11) Uani 1 1 d . . . . .
N005 N 0.9097(2) 0.7963(2) 0.59343(18) 0.0813(8) Uani 1 1 d . . . . .
C006 C 0.6559(3) 0.8603(2) 0.7200(2) 0.0791(10) Uani 1 1 d . . . . .
C007 C 0.5643(3) 0.8820(2) 0.6848(2) 0.0834(11) Uani 1 1 d . . . . .
H007 H 0.561806 0.888430 0.632313 0.100 Uiso 1 1 calc R U . . .
C008 C 0.9248(3) 0.8469(3) 0.6546(2) 0.0841(11) Uani 1 1 d . . . . .
C009 C 0.8319(4) 0.8696(3) 0.6965(2) 0.0882(12) Uani 1 1 d . . . . .
H009 H 0.836799 0.903908 0.740030 0.106 Uiso 1 1 calc R U . . .
C00A C 0.6584(3) 0.8495(3) 0.7981(2) 0.0911(12) Uani 1 1 d . . . . .
H00A H 0.719674 0.834014 0.822146 0.109 Uiso 1 1 calc R U . . .
C00B C 0.4777(3) 0.8836(3) 0.8056(2) 0.0861(11) Uani 1 1 d . . . . .
C00C C 0.4765(3) 0.8940(2) 0.7276(2) 0.0886(11) Uani 1 1 d . . . . .
H00C H 0.415228 0.909445 0.703545 0.106 Uiso 1 1 calc R U . . .
C00D C 0.8454(3) 0.6191(3) 0.4543(2) 0.0826(11) Uani 1 1 d . . . . .
C00E C 0.5699(4) 0.8618(3) 0.8400(2) 0.0968(13) Uani 1 1 d . . . . .
H00E H 0.572330 0.855339 0.892480 0.116 Uiso 1 1 calc R U . . .
C00F C 0.3829(4) 0.8978(3) 0.8506(3) 0.0957(12) Uani 1 1 d . . . . .
C00G C 0.9925(4) 0.7740(3) 0.5527(2) 0.0972(13) Uani 1 1 d . . . . .
H00G H 0.983671 0.738880 0.510072 0.117 Uiso 1 1 calc R U . . .
C00H C 0.3846(4) 0.9417(3) 0.9189(3) 0.1060(14) Uani 1 1 d . . . . .
H00H H 0.447155 0.962029 0.937717 0.127 Uiso 1 1 calc R U . . .
C00I C 1.0206(4) 0.8765(3) 0.6764(3) 0.1161(16) Uani 1 1 d . . . . .
H00I H 1.028309 0.912186 0.718839 0.139 Uiso 1 1 calc R U . . .
C00J C 0.2892(5) 0.8679(4) 0.8254(3) 0.1242(17) Uani 1 1 d . . . . .
H00J H 0.285625 0.837560 0.779632 0.149 Uiso 1 1 calc R U . . .
C00K C 0.1986(5) 0.8822(4) 0.8670(4) 0.143(2) Uani 1 1 d . . . . .
H00K H 0.135633 0.861636 0.849075 0.171 Uiso 1 1 calc R U . . .
C00L C 1.1045(4) 0.8519(4) 0.6338(4) 0.1347(19) Uani 1 1 d . . . . .
H00L H 1.170361 0.870022 0.647586 0.162 Uiso 1 1 calc R U . . .
C00M C 0.2947(5) 0.9563(4) 0.9605(3) 0.1263(18) Uani 1 1 d . . . . .
H00M H 0.297339 0.986488 1.006391 0.152 Uiso 1 1 calc R U . . .
C00N C 0.2036(5) 0.9262(4) 0.9336(4) 0.137(2) Uani 1 1 d . . . . .
H00N H 0.143518 0.935897 0.961310 0.164 Uiso 1 1 calc R U . . .
C00O C 1.0906(4) 0.8010(4) 0.5716(3) 0.1228(17) Uani 1 1 d . . . . .
H00O H 1.146682 0.784565 0.541922 0.147 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Fe Fe 0.3265 0.6960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
N004 Fe01 N004 94.1(2) 2_665 . ?
N004 Fe01 N005 90.49(14) 2_665 2_665 ?
N004 Fe01 N005 100.66(13) . 2_665 ?
N004 Fe01 N005 100.66(13) 2_665 . ?
N004 Fe01 N005 90.49(14) . . ?
N005 Fe01 N005 163.67(16) 2_665 . ?
N004 Fe01 N003 95.65(12) 2_665 . ?
N004 Fe01 N003 162.82(14) . . ?
N005 Fe01 N003 93.41(12) 2_665 . ?
N005 Fe01 N003 73.80(13) . . ?
N004 Fe01 N003 162.82(14) 2_665 2_665 ?
N004 Fe01 N003 95.65(12) . 2_665 ?
N005 Fe01 N003 73.80(13) 2_665 2_665 ?
N005 Fe01 N003 93.41(12) . 2_665 ?
N003 Fe01 N003 78.75(15) . 2_665 ?
C009 N003 C006 118.9(3) . . ?
C009 N003 Fe01 114.1(3) . . ?
C006 N003 Fe01 125.8(3) . . ?
C00D N004 Fe01 167.7(4) . . ?
C00G N005 C008 117.5(4) . . ?
C00G N005 Fe01 126.5(3) . . ?
C008 N005 Fe01 115.8(3) . . ?
C007 C006 C00A 119.7(4) . . ?
C007 C006 N003 118.7(3) . . ?
C00A C006 N003 121.5(4) . . ?
C00C C007 C006 119.9(3) . . ?
N005 C008 C00I 123.0(4) . . ?
N005 C008 C009 115.1(4) . . ?
C00I C008 C009 121.9(4) . . ?
N003 C009 C008 120.7(4) . . ?
C00E C00A C006 119.7(4) . . ?
C00E C00B C00C 118.2(4) . . ?
C00E C00B C00F 121.4(4) . . ?
C00C C00B C00F 120.4(4) . . ?
C007 C00C C00B 121.2(4) . . ?
N004 C00D S002 179.2(4) . . ?
C00A C00E C00B 121.4(4) . . ?
C00J C00F C00H 117.2(5) . . ?
C00J C00F C00B 121.0(5) . . ?
C00H C00F C00B 121.7(5) . . ?
N005 C00G C00O 122.5(5) . . ?
C00F C00H C00M 121.6(5) . . ?
C00L C00I C008 118.2(5) . . ?
C00F C00J C00K 121.4(6) . . ?
C00N C00K C00J 119.4(6) . . ?
C00O C00L C00I 119.5(5) . . ?
C00N C00M C00H 119.4(5) . . ?
C00K C00N C00M 120.9(6) . . ?
C00L C00O C00G 119.3(5) . . ?
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 N004 2.054(3) 2_665 ?
Fe01 N004 2.054(3) . ?
Fe01 N005 2.210(3) 2_665 ?
Fe01 N005 2.210(3) . ?
Fe01 N003 2.243(3) . ?
Fe01 N003 2.243(3) 2_665 ?
S002 C00D 1.613(4) . ?
N003 C009 1.274(5) . ?
N003 C006 1.421(4) . ?
N004 C00D 1.137(4) . ?
N005 C00G 1.335(5) . ?
N005 C008 1.340(5) . ?
C006 C007 1.379(5) . ?
C006 C00A 1.384(5) . ?
C007 C00C 1.376(5) . ?
C008 C00I 1.376(6) . ?
C008 C009 1.453(6) . ?
C00A C00E 1.376(5) . ?
C00B C00E 1.380(5) . ?
C00B C00C 1.382(5) . ?
C00B C00F 1.476(6) . ?
C00F C00J 1.372(6) . ?
C00F C00H 1.376(6) . ?
C00G C00O 1.377(6) . ?
C00H C00M 1.394(6) . ?
C00I C00L 1.373(7) . ?
C00J C00K 1.401(7) . ?
C00K C00N 1.352(8) . ?
C00L C00O 1.354(7) . ?
C00M C00N 1.353(8) . ?
