#------------------------------------------------------------------------------
#$Date: 2023-10-07 02:57:14 +0300 (Sat, 07 Oct 2023) $
#$Revision: 286839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/22/2312229.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_2312229
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                   12.9162(3)
_cell_length_b                   14.9373(4)
_cell_length_c                   17.6220(4)
_cell_measurement_reflns_used    4090
_cell_measurement_temperature    185(2)
_cell_measurement_theta_max      24.841
_cell_measurement_theta_min      1.918
_cell_volume                     3399.87(14)
_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 0.820
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.65524
_diffrn_reflns_av_R_equivalents  0.0904
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.820
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            35120
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.820
_diffrn_reflns_theta_full        23.150
_diffrn_reflns_theta_max         32.912
_diffrn_reflns_theta_min         1.922
_exptl_absorpt_coefficient_mu    0.442
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1424
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.197
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         6672
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.197
_refine_ls_R_factor_all          0.1677
_refine_ls_R_factor_gt           0.1036
_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)+(0.0314P)²+2.9329P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1553
_refine_ls_wR_factor_ref         0.1765
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4131
_reflns_number_total             6672
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Bia_Portho_185K.cif
_cod_data_source_block           Bia_dw4400_185K
_cod_depositor_comments
'Adding full bibliography for 2312165--2312274.cif.'
_cod_database_code               2312229
_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 0.57766(3) 0.03811(16) Uani 1 2 d S T P . .
S002 S 0.91189(8) 0.55675(8) 0.39526(5) 0.0682(3) Uani 1 1 d . . . . .
N003 N 0.7455(2) 0.84481(16) 0.67582(13) 0.0416(5) Uani 1 1 d . . . . .
N004 N 0.8016(2) 0.66047(19) 0.49743(14) 0.0515(7) Uani 1 1 d . . . . .
N005 N 0.91115(19) 0.79607(17) 0.59467(13) 0.0422(6) Uani 1 1 d . . . . .
C006 C 0.6570(2) 0.8617(2) 0.72169(15) 0.0406(6) Uani 1 1 d . . . . .
C007 C 0.5641(2) 0.8833(2) 0.68678(16) 0.0428(7) Uani 1 1 d . . . . .
H007 H 0.561353 0.890402 0.634390 0.051 Uiso 1 1 calc R U . . .
C008 C 0.9265(2) 0.8478(2) 0.65614(17) 0.0456(7) Uani 1 1 d . . . . .
C009 C 0.8339(3) 0.8720(2) 0.69885(17) 0.0465(7) Uani 1 1 d . . . . .
H009 H 0.839134 0.906909 0.742399 0.056 Uiso 1 1 calc R U . . .
C00A C 0.6604(2) 0.8511(2) 0.80019(17) 0.0475(7) Uani 1 1 d . . . . .
H00A H 0.722334 0.836274 0.823961 0.057 Uiso 1 1 calc R U . . .
C00B C 0.4779(3) 0.8844(2) 0.80826(18) 0.0460(7) Uani 1 1 d . . . . .
C00C C 0.4760(2) 0.8943(2) 0.72962(18) 0.0468(7) Uani 1 1 d . . . . .
H00C H 0.413961 0.908552 0.705671 0.056 Uiso 1 1 calc R U . . .
C00D C 0.8475(2) 0.6177(2) 0.45458(16) 0.0433(7) Uani 1 1 d . . . . .
C00E C 0.5714(3) 0.8628(2) 0.84271(17) 0.0508(8) Uani 1 1 d . . . . .
H00E H 0.574123 0.856108 0.895137 0.061 Uiso 1 1 calc R U . . .
C00F C 0.3824(3) 0.8979(2) 0.85338(19) 0.0500(8) Uani 1 1 d . . . . .
C00G C 0.9941(3) 0.7729(2) 0.55393(19) 0.0522(8) Uani 1 1 d . . . . .
H00G H 0.984662 0.737625 0.511005 0.063 Uiso 1 1 calc R U . . .
C00H C 0.3849(3) 0.9422(3) 0.92282(19) 0.0569(9) Uani 1 1 d . . . . .
H00H H 0.447728 0.962596 0.941936 0.068 Uiso 1 1 calc R U . . .
C00I C 1.0239(3) 0.8770(3) 0.6781(2) 0.0601(9) Uani 1 1 d . . . . .
H00I H 1.032346 0.912892 0.720843 0.072 Uiso 1 1 calc R U . . .
C00J C 0.2873(3) 0.8671(3) 0.8274(2) 0.0652(10) Uani 1 1 d . . . . .
H00J H 0.283587 0.836502 0.781545 0.078 Uiso 1 1 calc R U . . .
C00K C 0.1977(3) 0.8815(3) 0.8690(3) 0.0757(11) Uani 1 1 d . . . . .
H00K H 0.134510 0.861042 0.850737 0.091 Uiso 1 1 calc R U . . .
C00L C 1.1079(3) 0.8515(3) 0.6351(2) 0.0717(11) Uani 1 1 d . . . . .
H00L H 1.174242 0.869976 0.648480 0.086 Uiso 1 1 calc R U . . .
C00M C 0.2947(3) 0.9562(3) 0.9638(2) 0.0671(11) Uani 1 1 d . . . . .
H00M H 0.297457 0.986510 1.009861 0.081 Uiso 1 1 calc R U . . .
C00N C 0.2020(3) 0.9259(3) 0.9370(2) 0.0715(11) Uani 1 1 d . . . . .
H00N H 0.141792 0.935244 0.964882 0.086 Uiso 1 1 calc R U . . .
C00O C 1.0933(3) 0.7991(3) 0.5728(2) 0.0649(10) Uani 1 1 d . . . . .
H00O H 1.149311 0.781191 0.543371 0.078 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 93.17(15) 2_665 . ?
N004 Fe01 N005 101.29(10) 2_665 . ?
N004 Fe01 N005 89.45(10) . . ?
N004 Fe01 N005 89.45(10) 2_665 2_665 ?
N004 Fe01 N005 101.29(10) . 2_665 ?
N005 Fe01 N005 164.43(12) . 2_665 ?
N004 Fe01 N003 162.12(10) 2_665 2_665 ?
N004 Fe01 N003 96.40(10) . 2_665 ?
N005 Fe01 N003 93.88(9) . 2_665 ?
N005 Fe01 N003 73.90(9) 2_665 2_665 ?
N004 Fe01 N003 96.40(10) 2_665 . ?
N004 Fe01 N003 162.12(10) . . ?
N005 Fe01 N003 73.90(9) . . ?
N005 Fe01 N003 93.88(9) 2_665 . ?
N003 Fe01 N003 78.66(12) 2_665 . ?
C009 N003 C006 118.8(3) . . ?
C009 N003 Fe01 115.1(2) . . ?
C006 N003 Fe01 124.9(2) . . ?
C00D N004 Fe01 167.6(3) . . ?
C00G N005 C008 117.6(3) . . ?
C00G N005 Fe01 127.0(2) . . ?
C008 N005 Fe01 115.2(2) . . ?
C007 C006 C00A 119.6(3) . . ?
C007 C006 N003 119.0(2) . . ?
C00A C006 N003 121.3(3) . . ?
C00C C007 C006 120.0(3) . . ?
N005 C008 C00I 122.6(3) . . ?
N005 C008 C009 115.9(3) . . ?
C00I C008 C009 121.5(3) . . ?
N003 C009 C008 119.3(3) . . ?
C00E C00A C006 119.8(3) . . ?
C00E C00B C00C 118.3(3) . . ?
C00E C00B C00F 121.4(3) . . ?
C00C C00B C00F 120.3(3) . . ?
C007 C00C C00B 121.2(3) . . ?
N004 C00D S002 179.3(3) . . ?
C00A C00E C00B 121.0(3) . . ?
C00J C00F C00H 117.9(3) . . ?
C00J C00F C00B 121.0(3) . . ?
C00H C00F C00B 121.1(3) . . ?
N005 C00G C00O 122.8(3) . . ?
C00M C00H C00F 120.7(4) . . ?
C00L C00I C008 118.3(3) . . ?
C00K C00J C00F 120.8(4) . . ?
C00N C00K C00J 120.3(4) . . ?
C00O C00L C00I 119.6(3) . . ?
C00N C00M C00H 120.5(4) . . ?
C00M C00N C00K 119.9(4) . . ?
C00L C00O C00G 119.1(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) 2_665 ?
Fe01 N004 2.057(3) . ?
Fe01 N005 2.213(3) . ?
Fe01 N005 2.213(2) 2_665 ?
Fe01 N003 2.236(2) 2_665 ?
Fe01 N003 2.236(2) . ?
S002 C00D 1.617(3) . ?
N003 C009 1.278(4) . ?
N003 C006 1.422(4) . ?
N004 C00D 1.153(4) . ?
N005 C00G 1.336(4) . ?
N005 C008 1.345(4) . ?
C006 C007 1.387(4) . ?
C006 C00A 1.393(4) . ?
C007 C00C 1.376(4) . ?
C008 C00I 1.388(5) . ?
C008 C009 1.458(4) . ?
C00A C00E 1.384(4) . ?
C00B C00E 1.389(4) . ?
C00B C00C 1.394(4) . ?
C00B C00F 1.481(4) . ?
C00F C00J 1.389(5) . ?
C00F C00H 1.391(5) . ?
C00G C00O 1.380(5) . ?
C00H C00M 1.386(5) . ?
C00I C00L 1.378(5) . ?
C00J C00K 1.386(5) . ?
C00K C00N 1.370(6) . ?
C00L C00O 1.361(6) . ?
C00M C00N 1.365(6) . ?
