#------------------------------------------------------------------------------
#$Date: 2023-10-07 02:57:14 +0300 (Sat, 07 Oct 2023) $
#$Revision: 286839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/22/2312271.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_2312271
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                   12.9392(4)
_cell_length_b                   15.0898(5)
_cell_length_c                   17.6092(5)
_cell_measurement_reflns_used    3151
_cell_measurement_temperature    255(2)
_cell_measurement_theta_max      22.369
_cell_measurement_theta_min      1.923
_cell_volume                     3438.20(18)
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.826
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.65524
_diffrn_reflns_av_R_equivalents  0.0902
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.826
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            36172
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.826
_diffrn_reflns_theta_full        23.150
_diffrn_reflns_theta_max         33.015
_diffrn_reflns_theta_min         1.911
_exptl_absorpt_coefficient_mu    0.437
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1424
_refine_diff_density_max         0.225
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         6844
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.1960
_refine_ls_R_factor_gt           0.0980
_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)+(0.0392P)²+1.5075P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1542
_refine_ls_wR_factor_ref         0.1864
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3286
_reflns_number_total             6844
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Bia_Portho_255K.cif
_cod_data_source_block           Bia_dw4400_255K
_cod_depositor_comments
'Adding full bibliography for 2312165--2312274.cif.'
_cod_database_code               2312271
_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 0.57666(3) 0.05606(19) Uani 1 2 d S T P . .
S002 S 0.91029(9) 0.55745(9) 0.39542(6) 0.0978(4) Uani 1 1 d . . . . .
N003 N 0.7449(2) 0.84395(16) 0.67511(14) 0.0586(6) Uani 1 1 d . . . . .
N004 N 0.8014(2) 0.6608(2) 0.49684(15) 0.0743(8) Uani 1 1 d . . . . .
N005 N 0.9104(2) 0.79619(18) 0.59432(14) 0.0618(7) Uani 1 1 d . . . . .
C006 C 0.6565(2) 0.8609(2) 0.72087(16) 0.0580(7) Uani 1 1 d . . . . .
C007 C 0.5642(3) 0.8830(2) 0.68575(17) 0.0619(8) Uani 1 1 d . . . . .
H007 H 0.561707 0.890252 0.633338 0.074 Uiso 1 1 calc R U . . .
C008 C 0.9257(3) 0.8475(2) 0.65549(18) 0.0643(8) Uani 1 1 d . . . . .
C009 C 0.8330(3) 0.8709(2) 0.69780(19) 0.0668(9) Uani 1 1 d . . . . .
H009 H 0.838085 0.905568 0.741323 0.080 Uiso 1 1 calc R U . . .
C00A C 0.6594(3) 0.8506(2) 0.79914(18) 0.0683(9) Uani 1 1 d . . . . .
H00A H 0.721108 0.835721 0.823079 0.082 Uiso 1 1 calc R U . . .
C00B C 0.4781(3) 0.8843(2) 0.80691(19) 0.0652(8) Uani 1 1 d . . . . .
C00C C 0.4762(3) 0.8941(2) 0.72869(19) 0.0665(8) Uani 1 1 d . . . . .
H00C H 0.414398 0.908548 0.704749 0.080 Uiso 1 1 calc R U . . .
C00D C 0.8468(2) 0.6183(2) 0.45442(17) 0.0630(8) Uani 1 1 d . . . . .
C00E C 0.5705(3) 0.8625(2) 0.84149(18) 0.0718(9) Uani 1 1 d . . . . .
H00E H 0.572905 0.855832 0.893960 0.086 Uiso 1 1 calc R U . . .
C00F C 0.3824(3) 0.8978(2) 0.8522(2) 0.0726(9) Uani 1 1 d . . . . .
C00G C 0.9936(3) 0.7731(2) 0.5532(2) 0.0736(10) Uani 1 1 d . . . . .
H00G H 0.984501 0.737710 0.510424 0.088 Uiso 1 1 calc R U . . .
C00H C 0.3854(3) 0.9420(3) 0.9212(2) 0.0807(11) Uani 1 1 d . . . . .
H00H H 0.448245 0.962189 0.940106 0.097 Uiso 1 1 calc R U . . .
C00I C 1.0222(3) 0.8766(3) 0.6772(2) 0.0864(11) Uani 1 1 d . . . . .
H00I H 1.030312 0.912385 0.719796 0.104 Uiso 1 1 calc R U . . .
C00J C 0.2880(3) 0.8674(3) 0.8266(3) 0.0932(12) Uani 1 1 d . . . . .
H00J H 0.284213 0.836931 0.780804 0.112 Uiso 1 1 calc R U . . .
C00K C 0.1988(4) 0.8816(3) 0.8683(3) 0.1076(14) Uani 1 1 d . . . . .
H00K H 0.135772 0.860863 0.850267 0.129 Uiso 1 1 calc R U . . .
C00L C 1.1062(3) 0.8515(3) 0.6343(3) 0.1022(14) Uani 1 1 d . . . . .
H00L H 1.172333 0.869694 0.647957 0.123 Uiso 1 1 calc R U . . .
C00M C 0.2953(4) 0.9564(3) 0.9623(2) 0.0944(13) Uani 1 1 d . . . . .
H00M H 0.298036 0.986823 1.008222 0.113 Uiso 1 1 calc R U . . .
C00N C 0.2031(4) 0.9260(3) 0.9356(3) 0.1033(15) Uani 1 1 d . . . . .
H00N H 0.143001 0.935577 0.963400 0.124 Uiso 1 1 calc R U . . .
C00O C 1.0919(3) 0.8000(3) 0.5722(3) 0.0925(12) Uani 1 1 d . . . . .
H00O H 1.148018 0.783007 0.542576 0.111 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 93.76(16) . 2_665 ?
N004 Fe01 N005 89.92(11) . . ?
N004 Fe01 N005 101.16(11) 2_665 . ?
N004 Fe01 N005 101.16(11) . 2_665 ?
N004 Fe01 N005 89.92(11) 2_665 2_665 ?
N005 Fe01 N005 163.83(13) . 2_665 ?
N004 Fe01 N003 162.24(11) . . ?
N004 Fe01 N003 96.05(10) 2_665 . ?
N005 Fe01 N003 73.69(10) . . ?
N005 Fe01 N003 93.63(10) 2_665 . ?
N004 Fe01 N003 96.05(10) . 2_665 ?
N004 Fe01 N003 162.24(11) 2_665 2_665 ?
N005 Fe01 N003 93.63(10) . 2_665 ?
N005 Fe01 N003 73.69(10) 2_665 2_665 ?
N003 Fe01 N003 78.61(12) . 2_665 ?
C009 N003 C006 119.0(3) . . ?
C009 N003 Fe01 114.7(2) . . ?
C006 N003 Fe01 125.1(2) . . ?
C00D N004 Fe01 167.8(3) . . ?
C008 N005 C00G 117.6(3) . . ?
C008 N005 Fe01 115.7(2) . . ?
C00G N005 Fe01 126.5(2) . . ?
C007 C006 C00A 119.6(3) . . ?
C007 C006 N003 118.9(3) . . ?
C00A C006 N003 121.3(3) . . ?
C00C C007 C006 119.8(3) . . ?
N005 C008 C00I 122.8(3) . . ?
N005 C008 C009 115.4(3) . . ?
C00I C008 C009 121.8(3) . . ?
N003 C009 C008 119.9(3) . . ?
C00E C00A C006 119.9(3) . . ?
C00E C00B C00C 118.6(3) . . ?
C00E C00B C00F 121.1(3) . . ?
C00C C00B C00F 120.2(3) . . ?
C007 C00C C00B 121.2(3) . . ?
N004 C00D S002 179.3(3) . . ?
C00B C00E C00A 120.9(3) . . ?
C00J C00F C00H 118.1(4) . . ?
C00J C00F C00B 121.1(3) . . ?
C00H C00F C00B 120.8(4) . . ?
N005 C00G C00O 122.2(4) . . ?
C00F C00H C00M 120.6(4) . . ?
C00L C00I C008 118.4(4) . . ?
C00F C00J C00K 120.9(4) . . ?
C00N C00K C00J 120.2(5) . . ?
C00O C00L C00I 119.5(4) . . ?
C00N C00M C00H 120.2(4) . . ?
C00M C00N C00K 120.1(4) . . ?
C00L C00O C00G 119.5(4) . . ?
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 2.057(3) . ?
Fe01 N004 2.057(3) 2_665 ?
Fe01 N005 2.211(3) . ?
Fe01 N005 2.211(3) 2_665 ?
Fe01 N003 2.240(2) . ?
Fe01 N003 2.241(2) 2_665 ?
S002 C00D 1.612(4) . ?
N003 C009 1.275(4) . ?
N003 C006 1.423(4) . ?
N004 C00D 1.147(4) . ?
N005 C008 1.341(4) . ?
N005 C00G 1.344(4) . ?
C006 C007 1.385(4) . ?
C006 C00A 1.387(4) . ?
C007 C00C 1.377(4) . ?
C008 C00I 1.377(5) . ?
C008 C009 1.456(5) . ?
C00A C00E 1.383(5) . ?
C00B C00E 1.381(5) . ?
C00B C00C 1.386(4) . ?
C00B C00F 1.487(5) . ?
C00F C00J 1.380(6) . ?
C00F C00H 1.387(5) . ?
C00G C00O 1.376(5) . ?
C00H C00M 1.389(5) . ?
C00I C00L 1.377(6) . ?
C00J C00K 1.384(6) . ?
C00K C00N 1.363(6) . ?
C00L C00O 1.355(6) . ?
C00M C00N 1.362(6) . ?
