#------------------------------------------------------------------------------
#$Date: 2023-10-07 02:57:14 +0300 (Sat, 07 Oct 2023) $
#$Revision: 286839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/22/2312238.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_2312238
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                   12.9212(3)
_cell_length_b                   14.9706(4)
_cell_length_c                   17.6196(4)
_cell_measurement_reflns_used    3927
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.218
_cell_measurement_theta_min      1.924
_cell_volume                     3408.30(14)
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.814
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.65524
_diffrn_reflns_av_R_equivalents  0.0871
_diffrn_reflns_av_unetI/netI     0.0688
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.814
_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            35009
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.814
_diffrn_reflns_theta_full        23.150
_diffrn_reflns_theta_max         32.975
_diffrn_reflns_theta_min         1.919
_exptl_absorpt_coefficient_mu    0.441
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1424
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.223
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         6668
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.223
_refine_ls_R_factor_all          0.1753
_refine_ls_R_factor_gt           0.1085
_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)+(0.0205P)²+2.8498P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1685
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4112
_reflns_number_total             6668
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Bia_Portho_200K.cif
_cod_data_source_block           Bia_dw4400_200K
_cod_depositor_comments
'Adding full bibliography for 2312165--2312274.cif.'
_cod_database_code               2312238
_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 0.57746(3) 0.04058(16) Uani 1 2 d S T P . .
S002 S 0.91161(8) 0.55684(8) 0.39521(5) 0.0730(3) Uani 1 1 d . . . . .
N003 N 0.7454(2) 0.84465(16) 0.67549(13) 0.0440(5) Uani 1 1 d . . . . .
N004 N 0.8017(2) 0.66054(19) 0.49741(14) 0.0552(7) Uani 1 1 d . . . . .
N005 N 0.91069(19) 0.79610(17) 0.59464(13) 0.0448(6) Uani 1 1 d . . . . .
C006 C 0.6567(2) 0.86145(19) 0.72158(15) 0.0423(7) Uani 1 1 d . . . . .
C007 C 0.5641(2) 0.8832(2) 0.68662(16) 0.0458(7) Uani 1 1 d . . . . .
H007 H 0.561529 0.890292 0.634220 0.055 Uiso 1 1 calc R U . . .
C008 C 0.9263(2) 0.8478(2) 0.65603(17) 0.0472(7) Uani 1 1 d . . . . .
C009 C 0.8337(3) 0.8718(2) 0.69854(17) 0.0497(8) Uani 1 1 d . . . . .
H009 H 0.838776 0.906671 0.742082 0.060 Uiso 1 1 calc R U . . .
C00A C 0.6601(3) 0.8512(2) 0.79993(17) 0.0509(8) Uani 1 1 d . . . . .
H00A H 0.722076 0.836401 0.823716 0.061 Uiso 1 1 calc R U . . .
C00B C 0.4779(3) 0.8842(2) 0.80802(17) 0.0489(7) Uani 1 1 d . . . . .
C00C C 0.4760(3) 0.8942(2) 0.72937(18) 0.0489(7) Uani 1 1 d . . . . .
H00C H 0.414092 0.908526 0.705396 0.059 Uiso 1 1 calc R U . . .
C00D C 0.8474(2) 0.6181(2) 0.45445(16) 0.0462(7) Uani 1 1 d . . . . .
C00E C 0.5714(3) 0.8629(2) 0.84232(17) 0.0542(8) Uani 1 1 d . . . . .
H00E H 0.574327 0.856473 0.894770 0.065 Uiso 1 1 calc R U . . .
C00F C 0.3820(3) 0.8974(2) 0.85297(19) 0.0539(8) Uani 1 1 d . . . . .
C00G C 0.9941(3) 0.7731(2) 0.55381(19) 0.0546(8) Uani 1 1 d . . . . .
H00G H 0.984686 0.737942 0.510862 0.066 Uiso 1 1 calc R U . . .
C00H C 0.3850(3) 0.9422(3) 0.92242(19) 0.0610(9) Uani 1 1 d . . . . .
H00H H 0.447914 0.962638 0.941289 0.073 Uiso 1 1 calc R U . . .
C00I C 1.0235(3) 0.8770(3) 0.6779(2) 0.0651(9) Uani 1 1 d . . . . .
H00I H 1.031605 0.912946 0.720515 0.078 Uiso 1 1 calc R U . . .
C00J C 0.2872(3) 0.8671(3) 0.8271(2) 0.0691(10) Uani 1 1 d . . . . .
H00J H 0.283420 0.836769 0.781130 0.083 Uiso 1 1 calc R U . . .
C00K C 0.1982(3) 0.8814(3) 0.8688(3) 0.0817(12) Uani 1 1 d . . . . .
H00K H 0.134955 0.860650 0.850698 0.098 Uiso 1 1 calc R U . . .
C00L C 1.1080(3) 0.8516(3) 0.6352(2) 0.0756(11) Uani 1 1 d . . . . .
H00L H 1.174261 0.869800 0.648847 0.091 Uiso 1 1 calc R U . . .
C00M C 0.2953(3) 0.9564(3) 0.9634(2) 0.0715(11) Uani 1 1 d . . . . .
H00M H 0.298159 0.986893 1.009355 0.086 Uiso 1 1 calc R U . . .
C00N C 0.2024(4) 0.9259(3) 0.9368(2) 0.0782(12) Uani 1 1 d . . . . .
H00N H 0.142306 0.935282 0.964669 0.094 Uiso 1 1 calc R U . . .
C00O C 1.0928(3) 0.7993(3) 0.5726(2) 0.0691(10) Uani 1 1 d . . . . .
H00O H 1.148762 0.781558 0.542940 0.083 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 93.40(16) . 2_665 ?
N004 Fe01 N005 101.30(10) . 2_665 ?
N004 Fe01 N005 89.54(11) 2_665 2_665 ?
N004 Fe01 N005 89.54(11) . . ?
N004 Fe01 N005 101.30(10) 2_665 . ?
N005 Fe01 N005 164.25(12) 2_665 . ?
N004 Fe01 N003 162.09(11) . . ?
N004 Fe01 N003 96.23(10) 2_665 . ?
N005 Fe01 N003 93.86(9) 2_665 . ?
N005 Fe01 N003 73.80(9) . . ?
N004 Fe01 N003 96.23(10) . 2_665 ?
N004 Fe01 N003 162.09(11) 2_665 2_665 ?
N005 Fe01 N003 73.80(9) 2_665 2_665 ?
N005 Fe01 N003 93.86(9) . 2_665 ?
N003 Fe01 N003 78.78(12) . 2_665 ?
C009 N003 C006 118.7(3) . . ?
C009 N003 Fe01 115.1(2) . . ?
C006 N003 Fe01 125.0(2) . . ?
C00D N004 Fe01 167.7(3) . . ?
C00G N005 C008 117.3(3) . . ?
C00G N005 Fe01 127.0(2) . . ?
C008 N005 Fe01 115.5(2) . . ?
C007 C006 C00A 119.7(3) . . ?
C007 C006 N003 118.8(2) . . ?
C00A C006 N003 121.3(3) . . ?
C00C C007 C006 120.0(3) . . ?
N005 C008 C00I 122.8(3) . . ?
N005 C008 C009 115.6(3) . . ?
C00I C008 C009 121.6(3) . . ?
N003 C009 C008 119.4(3) . . ?
C00E C00A C006 119.8(3) . . ?
C00E C00B C00C 118.2(3) . . ?
C00E C00B C00F 121.7(3) . . ?
C00C C00B C00F 120.1(3) . . ?
C007 C00C C00B 121.2(3) . . ?
N004 C00D S002 178.8(3) . . ?
C00A C00E C00B 121.1(3) . . ?
C00J C00F C00H 118.1(3) . . ?
C00J C00F C00B 121.3(3) . . ?
C00H C00F C00B 120.6(3) . . ?
N005 C00G C00O 123.0(3) . . ?
C00M C00H C00F 120.6(4) . . ?
C00L C00I C008 118.7(4) . . ?
C00K C00J C00F 120.8(4) . . ?
C00N C00K C00J 120.4(4) . . ?
C00O C00L C00I 119.0(4) . . ?
C00N C00M C00H 120.3(4) . . ?
C00M C00N C00K 119.8(4) . . ?
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 2.209(3) 2_665 ?
Fe01 N005 2.209(3) . ?
Fe01 N003 2.235(2) . ?
Fe01 N003 2.235(2) 2_665 ?
S002 C00D 1.619(3) . ?
N003 C009 1.277(4) . ?
N003 C006 1.427(4) . ?
N004 C00D 1.151(4) . ?
N005 C00G 1.340(4) . ?
N005 C008 1.345(4) . ?
C006 C007 1.384(4) . ?
C006 C00A 1.390(4) . ?
C007 C00C 1.375(4) . ?
C008 C00I 1.384(5) . ?
C008 C009 1.457(4) . ?
C00A C00E 1.379(4) . ?
C00B C00E 1.388(4) . ?
C00B C00C 1.394(4) . ?
C00B C00F 1.483(4) . ?
C00F C00J 1.384(5) . ?
C00F C00H 1.396(5) . ?
C00G C00O 1.375(5) . ?
C00H C00M 1.382(5) . ?
C00I C00L 1.379(5) . ?
C00J C00K 1.382(5) . ?
C00K C00N 1.371(6) . ?
C00L C00O 1.368(6) . ?
C00M C00N 1.367(6) . ?
