#------------------------------------------------------------------------------
#$Date: 2023-10-07 02:57:14 +0300 (Sat, 07 Oct 2023) $
#$Revision: 286839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/22/2312259.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_2312259
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                   12.9567(6)
_cell_length_b                   15.2136(6)
_cell_length_c                   17.6020(6)
_cell_measurement_reflns_used    2609
_cell_measurement_temperature    305(2)
_cell_measurement_theta_max      21.065
_cell_measurement_theta_min      1.887
_cell_volume                     3469.7(2)
_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 0.827
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.65524
_diffrn_reflns_av_R_equivalents  0.0972
_diffrn_reflns_av_unetI/netI     0.0741
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.827
_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            36598
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.827
_diffrn_reflns_theta_full        23.150
_diffrn_reflns_theta_max         32.966
_diffrn_reflns_theta_min         1.903
_exptl_absorpt_coefficient_mu    0.433
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1424
_refine_diff_density_max         0.171
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         6892
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.2363
_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)+(0.0283P)²+1.5048P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1503
_refine_ls_wR_factor_ref         0.1882
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2818
_reflns_number_total             6892
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Bia_Portho_305K.cif
_cod_data_source_block           Bia_dw4400_305K
_cod_depositor_comments
'Adding full bibliography for 2312165--2312274.cif.'
_cod_database_code               2312259
_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 0.57595(4) 0.0693(2) Uani 1 2 d S T P . .
S002 S 0.90866(11) 0.55778(10) 0.39548(6) 0.1208(5) Uani 1 1 d . . . . .
N003 N 0.7443(2) 0.84335(18) 0.67449(15) 0.0714(7) Uani 1 1 d . . . . .
N004 N 0.8010(3) 0.6614(2) 0.49630(16) 0.0889(9) Uani 1 1 d . . . . .
N005 N 0.9100(2) 0.7964(2) 0.59373(16) 0.0755(8) Uani 1 1 d . . . . .
C006 C 0.6559(3) 0.8602(2) 0.72013(19) 0.0720(9) Uani 1 1 d . . . . .
C007 C 0.5642(3) 0.8826(2) 0.68514(19) 0.0752(9) Uani 1 1 d . . . . .
H007 H 0.561677 0.889920 0.632720 0.090 Uiso 1 1 calc R U . . .
C008 C 0.9252(3) 0.8470(2) 0.6550(2) 0.0792(10) Uani 1 1 d . . . . .
C009 C 0.8318(3) 0.8701(2) 0.6969(2) 0.0817(10) Uani 1 1 d . . . . .
H009 H 0.836618 0.904599 0.740408 0.098 Uiso 1 1 calc R U . . .
C00A C 0.6587(3) 0.8498(3) 0.7983(2) 0.0833(11) Uani 1 1 d . . . . .
H00A H 0.720192 0.834768 0.822243 0.100 Uiso 1 1 calc R U . . .
C00B C 0.4775(3) 0.8840(2) 0.8062(2) 0.0794(10) Uani 1 1 d . . . . .
C00C C 0.4767(3) 0.8939(2) 0.7281(2) 0.0817(10) Uani 1 1 d . . . . .
H00C H 0.415254 0.908685 0.704026 0.098 Uiso 1 1 calc R U . . .
C00D C 0.8460(3) 0.6189(3) 0.45424(19) 0.0765(10) Uani 1 1 d . . . . .
C00E C 0.5701(3) 0.8620(3) 0.8404(2) 0.0900(11) Uani 1 1 d . . . . .
H00E H 0.572660 0.855208 0.892865 0.108 Uiso 1 1 calc R U . . .
C00F C 0.3828(4) 0.8977(3) 0.8514(2) 0.0879(11) Uani 1 1 d . . . . .
C00G C 0.9930(3) 0.7740(3) 0.5530(2) 0.0909(12) Uani 1 1 d . . . . .
H00G H 0.983885 0.739281 0.510048 0.109 Uiso 1 1 calc R U . . .
C00H C 0.3848(4) 0.9420(3) 0.9200(2) 0.0988(13) Uani 1 1 d . . . . .
H00H H 0.447406 0.962601 0.938660 0.119 Uiso 1 1 calc R U . . .
C00I C 1.0208(4) 0.8767(3) 0.6768(3) 0.1061(14) Uani 1 1 d . . . . .
H00I H 1.028530 0.912469 0.719294 0.127 Uiso 1 1 calc R U . . .
C00J C 0.2890(4) 0.8679(3) 0.8258(3) 0.1153(15) Uani 1 1 d . . . . .
H00J H 0.285192 0.837864 0.779864 0.138 Uiso 1 1 calc R U . . .
C00K C 0.1995(4) 0.8820(4) 0.8676(3) 0.1322(18) Uani 1 1 d . . . . .
H00K H 0.136680 0.860899 0.849798 0.159 Uiso 1 1 calc R U . . .
C00L C 1.1048(4) 0.8519(4) 0.6342(3) 0.1235(17) Uani 1 1 d . . . . .
H00L H 1.170639 0.870428 0.647827 0.148 Uiso 1 1 calc R U . . .
C00M C 0.2955(5) 0.9564(3) 0.9614(3) 0.1172(16) Uani 1 1 d . . . . .
H00M H 0.298338 0.986366 1.007424 0.141 Uiso 1 1 calc R U . . .
C00N C 0.2035(5) 0.9264(4) 0.9343(3) 0.1257(18) Uani 1 1 d . . . . .
H00N H 0.143238 0.936472 0.961627 0.151 Uiso 1 1 calc R U . . .
C00O C 1.0911(4) 0.8003(4) 0.5719(3) 0.1125(15) Uani 1 1 d . . . . .
H00O H 1.147253 0.783025 0.542565 0.135 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 93.90(18) . 2_665 ?
N004 Fe01 N005 90.24(12) . . ?
N004 Fe01 N005 100.89(12) 2_665 . ?
N004 Fe01 N005 100.89(12) . 2_665 ?
N004 Fe01 N005 90.24(12) 2_665 2_665 ?
N005 Fe01 N005 163.73(15) . 2_665 ?
N004 Fe01 N003 162.54(12) . . ?
N004 Fe01 N003 95.85(11) 2_665 . ?
N005 Fe01 N003 73.72(11) . . ?
N005 Fe01 N003 93.53(11) 2_665 . ?
N004 Fe01 N003 95.85(11) . 2_665 ?
N004 Fe01 N003 162.54(12) 2_665 2_665 ?
N005 Fe01 N003 93.53(11) . 2_665 ?
N005 Fe01 N003 73.71(11) 2_665 2_665 ?
N003 Fe01 N003 78.69(13) . 2_665 ?
C009 N003 C006 119.1(3) . . ?
C009 N003 Fe01 114.5(2) . . ?
C006 N003 Fe01 125.3(2) . . ?
C00D N004 Fe01 167.9(3) . . ?
C00G N005 C008 117.4(3) . . ?
C00G N005 Fe01 126.7(3) . . ?
C008 N005 Fe01 115.8(2) . . ?
C007 C006 C00A 119.6(3) . . ?
C007 C006 N003 119.0(3) . . ?
C00A C006 N003 121.3(3) . . ?
C00C C007 C006 119.7(3) . . ?
N005 C008 C00I 123.1(4) . . ?
N005 C008 C009 115.1(3) . . ?
C00I C008 C009 121.8(4) . . ?
N003 C009 C008 120.4(3) . . ?
C00E C00A C006 119.8(4) . . ?
C00C C00B C00E 117.7(4) . . ?
C00C C00B C00F 120.9(4) . . ?
C00E C00B C00F 121.3(3) . . ?
C007 C00C C00B 121.9(4) . . ?
N004 C00D S002 179.2(4) . . ?
C00A C00E C00B 121.3(3) . . ?
C00J C00F C00H 117.6(4) . . ?
C00J C00F C00B 120.8(4) . . ?
C00H C00F C00B 121.6(4) . . ?
N005 C00G C00O 122.7(4) . . ?
C00F C00H C00M 121.5(5) . . ?
C008 C00I C00L 118.1(5) . . ?
C00F C00J C00K 120.9(5) . . ?
C00N C00K C00J 120.3(6) . . ?
C00O C00L C00I 119.7(5) . . ?
C00N C00M C00H 119.5(5) . . ?
C00K C00N C00M 120.2(5) . . ?
C00L C00O C00G 118.9(5) . . ?
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 2.054(3) . ?
Fe01 N004 2.054(3) 2_665 ?
Fe01 N005 2.212(3) . ?
Fe01 N005 2.212(3) 2_665 ?
Fe01 N003 2.243(3) . ?
Fe01 N003 2.243(3) 2_665 ?
S002 C00D 1.611(4) . ?
N003 C009 1.268(4) . ?
N003 C006 1.422(4) . ?
N004 C00D 1.143(4) . ?
N005 C00G 1.336(4) . ?
N005 C008 1.340(4) . ?
C006 C007 1.381(5) . ?
C006 C00A 1.385(4) . ?
C007 C00C 1.374(5) . ?
C008 C00I 1.374(5) . ?
C008 C009 1.460(5) . ?
C00A C00E 1.379(5) . ?
C00B C00C 1.382(5) . ?
C00B C00E 1.384(5) . ?
C00B C00F 1.477(5) . ?
C00F C00J 1.374(6) . ?
C00F C00H 1.384(5) . ?
C00G C00O 1.373(6) . ?
C00H C00M 1.385(6) . ?
C00I C00L 1.374(6) . ?
C00J C00K 1.389(6) . ?
C00K C00N 1.355(7) . ?
C00L C00O 1.361(6) . ?
C00M C00N 1.363(7) . ?
