#------------------------------------------------------------------------------
#$Date: 2023-10-07 02:57:14 +0300 (Sat, 07 Oct 2023) $
#$Revision: 286839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/21/2312166.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_2312166
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                   12.9662(8)
_cell_length_b                   15.3404(9)
_cell_length_c                   17.5869(8)
_cell_measurement_reflns_used    2304
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.2810
_cell_measurement_theta_min      2.154
_cell_volume                     3498.2(3)
_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 0.830
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.65524
_diffrn_reflns_av_R_equivalents  0.1024
_diffrn_reflns_av_unetI/netI     0.0821
_diffrn_reflns_Laue_measured_fraction_full 0.985
_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            36859
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.830
_diffrn_reflns_theta_full        23.150
_diffrn_reflns_theta_max         32.975
_diffrn_reflns_theta_min         1.896
_exptl_absorpt_coefficient_mu    0.430
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1424
_refine_diff_density_max         0.206
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         6983
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.2757
_refine_ls_R_factor_gt           0.1137
_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)+(0.0584P)²+1.0695P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1938
_refine_ls_wR_factor_ref         0.2535
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2327
_reflns_number_total             6983
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ne5010sup1.cif
_cod_data_source_block           Bia_dw4400_350K
_cod_depositor_comments
'Adding full bibliography for 2312165--2312274.cif.'
_cod_database_code               2312166
_cod_database_fobs_code          2312166
_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 0.57521(4) 0.0851(3) Uani 1 2 d S T P . .
S002 S 0.90709(14) 0.55818(12) 0.39553(8) 0.1458(7) Uani 1 1 d . . . . .
N003 N 0.7442(3) 0.8426(2) 0.67390(18) 0.0881(9) Uani 1 1 d . . . . .
N004 N 0.8005(3) 0.6616(3) 0.4959(2) 0.1096(12) Uani 1 1 d . . . . .
N005 N 0.9098(3) 0.7964(3) 0.5931(2) 0.0934(10) Uani 1 1 d . . . . .
C006 C 0.6563(4) 0.8594(3) 0.7195(2) 0.0878(12) Uani 1 1 d . . . . .
C007 C 0.5640(4) 0.8818(3) 0.6844(2) 0.0947(13) Uani 1 1 d . . . . .
H007 H 0.561399 0.888589 0.631930 0.114 Uiso 1 1 calc R U . . .
C008 C 0.9242(4) 0.8464(3) 0.6543(3) 0.0962(13) Uani 1 1 d . . . . .
C009 C 0.8313(4) 0.8696(3) 0.6963(3) 0.0993(14) Uani 1 1 d . . . . .
H009 H 0.835924 0.904310 0.739481 0.119 Uiso 1 1 calc R U . . .
C00A C 0.6583(4) 0.8488(3) 0.7974(2) 0.1027(14) Uani 1 1 d . . . . .
H00A H 0.719423 0.833378 0.821537 0.123 Uiso 1 1 calc R U . . .
C00B C 0.4779(4) 0.8838(3) 0.8049(3) 0.0973(13) Uani 1 1 d . . . . .
C00C C 0.4771(4) 0.8940(3) 0.7271(3) 0.0994(13) Uani 1 1 d . . . . .
H00C H 0.415922 0.909434 0.703062 0.119 Uiso 1 1 calc R U . . .
C00D C 0.8450(3) 0.6195(3) 0.4539(2) 0.0940(13) Uani 1 1 d . . . . .
C00E C 0.5695(4) 0.8613(3) 0.8398(3) 0.1106(15) Uani 1 1 d . . . . .
H00E H 0.571562 0.854337 0.892301 0.133 Uiso 1 1 calc R U . . .
C00F C 0.3823(4) 0.8981(3) 0.8499(3) 0.1078(14) Uani 1 1 d . . . . .
C00G C 0.9927(4) 0.7741(4) 0.5520(3) 0.1115(15) Uani 1 1 d . . . . .
H00G H 0.984231 0.739295 0.509172 0.134 Uiso 1 1 calc R U . . .
C00H C 0.3838(5) 0.9420(4) 0.9186(3) 0.1216(18) Uani 1 1 d . . . . .
H00H H 0.446323 0.962317 0.937616 0.146 Uiso 1 1 calc R U . . .
C00I C 1.0202(5) 0.8761(4) 0.6763(3) 0.1303(19) Uani 1 1 d . . . . .
H00I H 1.027666 0.911710 0.718735 0.156 Uiso 1 1 calc R U . . .
C00J C 0.2892(5) 0.8678(4) 0.8248(4) 0.140(2) Uani 1 1 d . . . . .
H00J H 0.285787 0.836936 0.779344 0.168 Uiso 1 1 calc R U . . .
C00K C 0.1991(6) 0.8827(5) 0.8665(5) 0.163(2) Uani 1 1 d . . . . .
H00K H 0.136194 0.862272 0.848379 0.196 Uiso 1 1 calc R U . . .
C00L C 1.1042(5) 0.8517(5) 0.6339(4) 0.149(2) Uani 1 1 d . . . . .
H00L H 1.170086 0.869525 0.647795 0.179 Uiso 1 1 calc R U . . .
C00M C 0.2942(7) 0.9563(4) 0.9599(3) 0.142(2) Uani 1 1 d . . . . .
H00M H 0.296791 0.986226 1.005822 0.171 Uiso 1 1 calc R U . . .
C00N C 0.2032(6) 0.9266(5) 0.9330(5) 0.152(3) Uani 1 1 d . . . . .
H00N H 0.142963 0.936351 0.960449 0.183 Uiso 1 1 calc R U . . .
C00O C 1.0898(5) 0.8015(5) 0.5715(4) 0.1360(19) Uani 1 1 d . . . . .
H00O H 1.146070 0.785492 0.541839 0.163 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 94.4(2) 2_665 . ?
N004 Fe01 N005 100.54(15) 2_665 . ?
N004 Fe01 N005 90.60(16) . . ?
N004 Fe01 N005 90.60(16) 2_665 2_665 ?
N004 Fe01 N005 100.54(15) . 2_665 ?
N005 Fe01 N005 163.63(19) . 2_665 ?
N004 Fe01 N003 162.62(16) 2_665 2_665 ?
N004 Fe01 N003 95.55(14) . 2_665 ?
N005 Fe01 N003 93.56(14) . 2_665 ?
N005 Fe01 N003 73.59(15) 2_665 2_665 ?
N004 Fe01 N003 95.55(14) 2_665 . ?
N004 Fe01 N003 162.62(16) . . ?
N005 Fe01 N003 73.59(15) . . ?
N005 Fe01 N003 93.56(14) 2_665 . ?
N003 Fe01 N003 78.66(17) 2_665 . ?
C009 N003 C006 118.8(4) . . ?
C009 N003 Fe01 114.7(3) . . ?
C006 N003 Fe01 125.4(3) . . ?
C00D N004 Fe01 167.8(4) . . ?
C008 N005 C00G 118.0(4) . . ?
C008 N005 Fe01 115.5(3) . . ?
C00G N005 Fe01 126.3(4) . . ?
C00A C006 C007 119.1(4) . . ?
C00A C006 N003 121.7(4) . . ?
C007 C006 N003 119.2(4) . . ?
C00C C007 C006 120.0(4) . . ?
N005 C008 C00I 122.8(5) . . ?
N005 C008 C009 115.6(4) . . ?
C00I C008 C009 121.5(5) . . ?
N003 C009 C008 120.0(4) . . ?
C006 C00A C00E 120.2(4) . . ?
C00C C00B C00E 118.4(4) . . ?
C00C C00B C00F 120.4(5) . . ?
C00E C00B C00F 121.1(4) . . ?
C007 C00C C00B 121.6(4) . . ?
N004 C00D S002 178.8(5) . . ?
C00B C00E C00A 120.7(4) . . ?
C00J C00F C00H 117.4(5) . . ?
C00J C00F C00B 120.9(5) . . ?
C00H C00F C00B 121.7(5) . . ?
N005 C00G C00O 121.6(5) . . ?
C00F C00H C00M 121.4(6) . . ?
C00L C00I C008 118.2(6) . . ?
C00F C00J C00K 120.9(6) . . ?
C00N C00K C00J 120.2(8) . . ?
C00O C00L C00I 119.1(6) . . ?
C00N C00M C00H 119.7(6) . . ?
C00K C00N C00M 120.4(7) . . ?
C00L C00O C00G 120.3(6) . . ?
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 2.053(4) 2_665 ?
Fe01 N004 2.053(4) . ?
Fe01 N005 2.213(4) . ?
Fe01 N005 2.213(4) 2_665 ?
Fe01 N003 2.244(3) 2_665 ?
Fe01 N003 2.244(3) . ?
S002 C00D 1.608(5) . ?
N003 C009 1.265(5) . ?
N003 C006 1.418(5) . ?
N004 C00D 1.138(5) . ?
N005 C008 1.335(5) . ?
N005 C00G 1.340(6) . ?
C006 C00A 1.381(5) . ?
C006 C007 1.389(6) . ?
C007 C00C 1.367(6) . ?
C008 C00I 1.380(7) . ?
C008 C009 1.457(6) . ?
C00A C00E 1.384(6) . ?
C00B C00C 1.376(6) . ?
C00B C00E 1.381(6) . ?
C00B C00F 1.486(7) . ?
C00F C00J 1.367(7) . ?
C00F C00H 1.384(7) . ?
C00G C00O 1.371(7) . ?
C00H C00M 1.387(8) . ?
C00I C00L 1.372(8) . ?
C00J C00K 1.398(9) . ?
C00K C00N 1.351(9) . ?
C00L C00O 1.353(8) . ?
C00M C00N 1.351(9) . ?
