#------------------------------------------------------------------------------
#$Date: 2023-10-07 02:57:14 +0300 (Sat, 07 Oct 2023) $
#$Revision: 286839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/22/2312248.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_2312248
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                   12.9607(6)
_cell_length_b                   15.2577(8)
_cell_length_c                   17.5967(7)
_cell_measurement_reflns_used    2539
_cell_measurement_temperature    320(2)
_cell_measurement_theta_max      21.112
_cell_measurement_theta_min      1.889
_cell_volume                     3479.8(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 0.828
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.65524
_diffrn_reflns_av_R_equivalents  0.0980
_diffrn_reflns_av_unetI/netI     0.0745
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.828
_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            36633
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_theta_full        23.150
_diffrn_reflns_theta_max         32.948
_diffrn_reflns_theta_min         1.901
_exptl_absorpt_coefficient_mu    0.432
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1424
_refine_diff_density_max         0.172
_refine_diff_density_min         -0.188
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         6912
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.2465
_refine_ls_R_factor_gt           0.1059
_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)+(0.0410P)²+1.1147P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1614
_refine_ls_wR_factor_ref         0.2049
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2599
_reflns_number_total             6912
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Bia_Portho_320K.cif
_cod_data_source_block           Bia_dw4400_320K
_cod_depositor_comments
'Adding full bibliography for 2312165--2312274.cif.'
_cod_database_code               2312248
_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 0.57568(4) 0.0747(2) Uani 1 2 d S T P . .
S002 S 0.90810(11) 0.55796(10) 0.39555(7) 0.1299(5) Uani 1 1 d . . . . .
N003 N 0.7437(2) 0.84326(19) 0.67414(15) 0.0771(7) Uani 1 1 d . . . . .
N004 N 0.8006(3) 0.6616(2) 0.49613(17) 0.0974(10) Uani 1 1 d . . . . .
N005 N 0.9101(2) 0.7959(2) 0.59347(17) 0.0822(8) Uani 1 1 d . . . . .
C006 C 0.6561(3) 0.8601(2) 0.71983(19) 0.0776(9) Uani 1 1 d . . . . .
C007 C 0.5643(3) 0.8824(2) 0.6851(2) 0.0823(10) Uani 1 1 d . . . . .
H007 H 0.561821 0.889579 0.632695 0.099 Uiso 1 1 calc R U . . .
C008 C 0.9250(3) 0.8473(3) 0.6546(2) 0.0849(10) Uani 1 1 d . . . . .
C009 C 0.8317(3) 0.8699(2) 0.6968(2) 0.0878(11) Uani 1 1 d . . . . .
H009 H 0.836435 0.903977 0.740454 0.105 Uiso 1 1 calc R U . . .
C00A C 0.6587(3) 0.8498(3) 0.7979(2) 0.0894(11) Uani 1 1 d . . . . .
H00A H 0.720119 0.834624 0.821895 0.107 Uiso 1 1 calc R U . . .
C00B C 0.4782(3) 0.8836(2) 0.8056(2) 0.0839(10) Uani 1 1 d . . . . .
C00C C 0.4767(3) 0.8939(2) 0.7278(2) 0.0883(11) Uani 1 1 d . . . . .
H00C H 0.415306 0.908995 0.703776 0.106 Uiso 1 1 calc R U . . .
C00D C 0.8454(3) 0.6193(3) 0.4542(2) 0.0829(10) Uani 1 1 d . . . . .
C00E C 0.5704(3) 0.8619(3) 0.8403(2) 0.0952(12) Uani 1 1 d . . . . .
H00E H 0.572918 0.855518 0.892834 0.114 Uiso 1 1 calc R U . . .
C00F C 0.3826(4) 0.8976(3) 0.8506(3) 0.0948(12) Uani 1 1 d . . . . .
C00G C 0.9932(3) 0.7738(3) 0.5527(2) 0.0975(12) Uani 1 1 d . . . . .
H00G H 0.984544 0.738991 0.509765 0.117 Uiso 1 1 calc R U . . .
C00H C 0.3845(4) 0.9420(3) 0.9192(3) 0.1076(14) Uani 1 1 d . . . . .
H00H H 0.447303 0.962493 0.937645 0.129 Uiso 1 1 calc R U . . .
C00I C 1.0208(4) 0.8764(3) 0.6764(3) 0.1148(15) Uani 1 1 d . . . . .
H00I H 1.028779 0.911665 0.719125 0.138 Uiso 1 1 calc R U . . .
C00J C 0.2891(4) 0.8678(3) 0.8256(3) 0.1252(16) Uani 1 1 d . . . . .
H00J H 0.285236 0.837336 0.779897 0.150 Uiso 1 1 calc R U . . .
C00K C 0.1993(5) 0.8824(4) 0.8675(4) 0.1414(19) Uani 1 1 d . . . . .
H00K H 0.136256 0.861661 0.849783 0.170 Uiso 1 1 calc R U . . .
C00L C 1.1044(4) 0.8520(4) 0.6336(4) 0.1325(18) Uani 1 1 d . . . . .
H00L H 1.170294 0.870626 0.646907 0.159 Uiso 1 1 calc R U . . .
C00M C 0.2959(5) 0.9567(4) 0.9612(3) 0.1267(17) Uani 1 1 d . . . . .
H00M H 0.298918 0.986599 1.007238 0.152 Uiso 1 1 calc R U . . .
C00N C 0.2043(5) 0.9267(4) 0.9340(4) 0.136(2) Uani 1 1 d . . . . .
H00N H 0.144214 0.936729 0.961446 0.163 Uiso 1 1 calc R U . . .
C00O C 1.0901(4) 0.8007(4) 0.5718(3) 0.1194(15) Uani 1 1 d . . . . .
H00O H 1.146253 0.783727 0.542352 0.143 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 93.96(19) . 2_665 ?
N004 Fe01 N005 90.30(13) . . ?
N004 Fe01 N005 100.82(13) 2_665 . ?
N004 Fe01 N005 100.82(13) . 2_665 ?
N004 Fe01 N005 90.30(13) 2_665 2_665 ?
N005 Fe01 N005 163.73(16) . 2_665 ?
N004 Fe01 N003 95.64(12) . 2_665 ?
N004 Fe01 N003 162.86(13) 2_665 2_665 ?
N005 Fe01 N003 93.31(11) . 2_665 ?
N005 Fe01 N003 73.96(12) 2_665 2_665 ?
N004 Fe01 N003 162.86(13) . . ?
N004 Fe01 N003 95.64(12) 2_665 . ?
N005 Fe01 N003 73.96(12) . . ?
N005 Fe01 N003 93.31(11) 2_665 . ?
N003 Fe01 N003 78.88(14) 2_665 . ?
C009 N003 C006 118.8(3) . . ?
C009 N003 Fe01 114.3(3) . . ?
C006 N003 Fe01 125.7(2) . . ?
C00D N004 Fe01 167.7(4) . . ?
C00G N005 C008 117.4(4) . . ?
C00G N005 Fe01 126.8(3) . . ?
C008 N005 Fe01 115.7(3) . . ?
C007 C006 C00A 119.2(3) . . ?
C007 C006 N003 119.0(3) . . ?
C00A C006 N003 121.6(3) . . ?
C00C C007 C006 120.2(3) . . ?
N005 C008 C00I 122.8(4) . . ?
N005 C008 C009 115.1(4) . . ?
C00I C008 C009 122.1(4) . . ?
N003 C009 C008 120.5(4) . . ?
C00E C00A C006 120.1(4) . . ?
C00C C00B C00E 118.6(4) . . ?
C00C C00B C00F 120.0(4) . . ?
C00E C00B C00F 121.4(4) . . ?
C007 C00C C00B 121.1(4) . . ?
N004 C00D S002 179.0(4) . . ?
C00A C00E C00B 120.7(4) . . ?
C00J C00F C00H 117.4(4) . . ?
C00J C00F C00B 121.3(4) . . ?
C00H C00F C00B 121.3(4) . . ?
N005 C00G C00O 122.3(5) . . ?
C00F C00H C00M 122.0(5) . . ?
C00L C00I C008 118.2(5) . . ?
C00F C00J C00K 121.1(5) . . ?
C00N C00K C00J 119.8(6) . . ?
C00O C00L C00I 119.4(5) . . ?
C00N C00M C00H 118.7(5) . . ?
C00K C00N C00M 121.1(6) . . ?
C00L C00O C00G 119.9(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 2.052(3) . ?
Fe01 N004 2.052(3) 2_665 ?
Fe01 N005 2.212(3) . ?
Fe01 N005 2.212(3) 2_665 ?
Fe01 N003 2.243(3) 2_665 ?
Fe01 N003 2.243(3) . ?
S002 C00D 1.613(4) . ?
N003 C009 1.274(4) . ?
N003 C006 1.415(4) . ?
N004 C00D 1.139(4) . ?
N005 C00G 1.338(5) . ?
N005 C008 1.345(5) . ?
C006 C007 1.379(5) . ?
C006 C00A 1.384(5) . ?
C007 C00C 1.372(5) . ?
C008 C00I 1.373(6) . ?
C008 C009 1.461(5) . ?
C00A C00E 1.378(5) . ?
C00B C00C 1.379(5) . ?
C00B C00E 1.382(5) . ?
C00B C00F 1.486(6) . ?
C00F C00J 1.367(6) . ?
C00F C00H 1.384(6) . ?
C00G C00O 1.363(6) . ?
C00H C00M 1.385(6) . ?
C00I C00L 1.371(7) . ?
C00J C00K 1.395(7) . ?
C00K C00N 1.352(7) . ?
C00L C00O 1.354(7) . ?
C00M C00N 1.360(8) . ?
