#------------------------------------------------------------------------------
#$Date: 2023-10-07 02:57:14 +0300 (Sat, 07 Oct 2023) $
#$Revision: 286839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/22/2312237.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_2312237
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                   12.9419(5)
_cell_length_b                   15.1124(5)
_cell_length_c                   17.6080(5)
_cell_measurement_reflns_used    3069
_cell_measurement_temperature    265(2)
_cell_measurement_theta_max      22.687
_cell_measurement_theta_min      1.896
_cell_volume                     3443.8(2)
_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 0.828
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.65524
_diffrn_reflns_av_R_equivalents  0.0929
_diffrn_reflns_av_unetI/netI     0.0687
_diffrn_reflns_Laue_measured_fraction_full 0.985
_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       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            36224
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_theta_full        23.150
_diffrn_reflns_theta_max         32.990
_diffrn_reflns_theta_min         1.910
_exptl_absorpt_coefficient_mu    0.437
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1424
_refine_diff_density_max         0.250
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         6855
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.2039
_refine_ls_R_factor_gt           0.0973
_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)+(0.0345P)²+1.6552P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1843
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3168
_reflns_number_total             6855
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Bia_Portho_265K.cif
_cod_data_source_block           Bia_dw4400_265K
_cod_depositor_comments
'Adding full bibliography for 2312165--2312274.cif.'
_cod_database_code               2312237
_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 0.57655(3) 0.0584(2) Uani 1 2 d S T P . .
S002 S 0.91001(10) 0.55758(9) 0.39539(6) 0.1022(4) Uani 1 1 d . . . . .
N003 N 0.7448(2) 0.84392(17) 0.67515(14) 0.0617(6) Uani 1 1 d . . . . .
N004 N 0.8014(2) 0.6610(2) 0.49666(15) 0.0761(8) Uani 1 1 d . . . . .
N005 N 0.9105(2) 0.79601(18) 0.59399(14) 0.0632(7) Uani 1 1 d . . . . .
C006 C 0.6566(3) 0.8609(2) 0.72073(17) 0.0605(8) Uani 1 1 d . . . . .
C007 C 0.5643(3) 0.8828(2) 0.68585(17) 0.0651(8) Uani 1 1 d . . . . .
H007 H 0.561612 0.889894 0.633422 0.078 Uiso 1 1 calc R U . . .
C008 C 0.9253(3) 0.8475(2) 0.65534(19) 0.0675(9) Uani 1 1 d . . . . .
C009 C 0.8328(3) 0.8708(2) 0.69752(19) 0.0696(9) Uani 1 1 d . . . . .
H009 H 0.837955 0.905448 0.740993 0.084 Uiso 1 1 calc R U . . .
C00A C 0.6592(3) 0.8507(2) 0.79909(18) 0.0716(9) Uani 1 1 d . . . . .
H00A H 0.720903 0.836030 0.823126 0.086 Uiso 1 1 calc R U . . .
C00B C 0.4782(3) 0.8841(2) 0.80722(19) 0.0678(9) Uani 1 1 d . . . . .
C00C C 0.4766(3) 0.8940(2) 0.72864(19) 0.0688(9) Uani 1 1 d . . . . .
H00C H 0.414804 0.908440 0.704652 0.083 Uiso 1 1 calc R U . . .
C00D C 0.8464(3) 0.6187(2) 0.45421(18) 0.0658(8) Uani 1 1 d . . . . .
C00E C 0.5706(3) 0.8622(2) 0.84122(19) 0.0754(10) Uani 1 1 d . . . . .
H00E H 0.573146 0.855097 0.893651 0.090 Uiso 1 1 calc R U . . .
C00F C 0.3827(3) 0.8977(2) 0.8518(2) 0.0749(10) Uani 1 1 d . . . . .
C00G C 0.9936(3) 0.7734(2) 0.5531(2) 0.0765(10) Uani 1 1 d . . . . .
H00G H 0.984459 0.738378 0.510210 0.092 Uiso 1 1 calc R U . . .
C00H C 0.3850(3) 0.9420(3) 0.9209(2) 0.0847(11) Uani 1 1 d . . . . .
H00H H 0.447765 0.962314 0.939851 0.102 Uiso 1 1 calc R U . . .
C00I C 1.0219(3) 0.8762(3) 0.6774(2) 0.0896(12) Uani 1 1 d . . . . .
H00I H 1.029972 0.911421 0.720259 0.107 Uiso 1 1 calc R U . . .
C00J C 0.2881(3) 0.8674(3) 0.8266(3) 0.0967(13) Uani 1 1 d . . . . .
H00J H 0.284167 0.836751 0.780927 0.116 Uiso 1 1 calc R U . . .
C00K C 0.1989(4) 0.8821(3) 0.8684(3) 0.1138(15) Uani 1 1 d . . . . .
H00K H 0.135826 0.861456 0.850340 0.137 Uiso 1 1 calc R U . . .
C00L C 1.1060(3) 0.8516(3) 0.6345(3) 0.1064(15) Uani 1 1 d . . . . .
H00L H 1.172025 0.870074 0.648037 0.128 Uiso 1 1 calc R U . . .
C00M C 0.2955(4) 0.9564(3) 0.9621(2) 0.0988(14) Uani 1 1 d . . . . .
H00M H 0.298552 0.986613 1.008040 0.119 Uiso 1 1 calc R U . . .
C00N C 0.2029(4) 0.9264(3) 0.9355(3) 0.1065(15) Uani 1 1 d . . . . .
H00N H 0.142752 0.936279 0.963219 0.128 Uiso 1 1 calc R U . . .
C00O C 1.0915(3) 0.7998(3) 0.5720(3) 0.0948(12) Uani 1 1 d . . . . .
H00O H 1.147609 0.782507 0.542430 0.114 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 93.69(17) . 2_665 ?
N004 Fe01 N005 101.15(11) . 2_665 ?
N004 Fe01 N005 89.80(11) 2_665 2_665 ?
N004 Fe01 N005 89.80(11) . . ?
N004 Fe01 N005 101.15(11) 2_665 . ?
N005 Fe01 N005 164.04(13) 2_665 . ?
N004 Fe01 N003 96.08(10) . 2_665 ?
N004 Fe01 N003 162.30(11) 2_665 2_665 ?
N005 Fe01 N003 73.85(10) 2_665 2_665 ?
N005 Fe01 N003 93.62(10) . 2_665 ?
N004 Fe01 N003 162.30(11) . . ?
N004 Fe01 N003 96.08(10) 2_665 . ?
N005 Fe01 N003 93.62(10) 2_665 . ?
N005 Fe01 N003 73.85(10) . . ?
N003 Fe01 N003 78.60(13) 2_665 . ?
C009 N003 C006 119.2(3) . . ?
C009 N003 Fe01 114.5(2) . . ?
C006 N003 Fe01 125.2(2) . . ?
C00D N004 Fe01 167.9(3) . . ?
C00G N005 C008 117.7(3) . . ?
C00G N005 Fe01 126.8(2) . . ?
C008 N005 Fe01 115.3(2) . . ?
C007 C006 C00A 119.3(3) . . ?
C007 C006 N003 119.1(3) . . ?
C00A C006 N003 121.5(3) . . ?
C00C C007 C006 120.0(3) . . ?
N005 C008 C00I 122.5(4) . . ?
N005 C008 C009 115.7(3) . . ?
C00I C008 C009 121.8(3) . . ?
N003 C009 C008 120.2(3) . . ?
C00E C00A C006 120.0(3) . . ?
C00E C00B C00C 118.1(3) . . ?
C00E C00B C00F 121.9(3) . . ?
C00C C00B C00F 120.0(3) . . ?
C007 C00C C00B 121.3(3) . . ?
N004 C00D S002 179.0(3) . . ?
C00B C00E C00A 121.3(3) . . ?
C00J C00F C00H 117.4(4) . . ?
C00J C00F C00B 121.7(4) . . ?
C00H C00F C00B 120.9(4) . . ?
N005 C00G C00O 122.6(4) . . ?
C00M C00H C00F 121.1(4) . . ?
C00L C00I C008 118.5(4) . . ?
C00F C00J C00K 121.0(4) . . ?
C00N C00K C00J 120.6(5) . . ?
C00O C00L C00I 119.3(4) . . ?
C00N C00M C00H 120.3(4) . . ?
C00K C00N C00M 119.6(5) . . ?
C00L C00O C00G 119.3(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 2.212(3) 2_665 ?
Fe01 N005 2.212(3) . ?
Fe01 N003 2.243(3) 2_665 ?
Fe01 N003 2.243(3) . ?
S002 C00D 1.613(4) . ?
N003 C009 1.272(4) . ?
N003 C006 1.419(4) . ?
N004 C00D 1.143(4) . ?
N005 C00G 1.339(4) . ?
N005 C008 1.345(4) . ?
C006 C007 1.383(4) . ?
C006 C00A 1.389(4) . ?
C007 C00C 1.373(4) . ?
C008 C00I 1.379(5) . ?
C008 C009 1.452(5) . ?
C00A C00E 1.377(5) . ?
C00B C00E 1.377(5) . ?
C00B C00C 1.392(5) . ?
C00B C00F 1.479(5) . ?
C00F C00J 1.380(5) . ?
C00F C00H 1.389(5) . ?
C00G C00O 1.370(5) . ?
C00H C00M 1.383(5) . ?
C00I C00L 1.376(6) . ?
C00J C00K 1.387(6) . ?
C00K C00N 1.360(6) . ?
C00L C00O 1.364(6) . ?
C00M C00N 1.364(7) . ?
