#------------------------------------------------------------------------------
#$Date: 2023-10-07 02:57:14 +0300 (Sat, 07 Oct 2023) $
#$Revision: 286839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/22/2312246.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_2312246
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                   12.9305(4)
_cell_length_b                   15.0243(4)
_cell_length_c                   17.6168(4)
_cell_measurement_reflns_used    3552
_cell_measurement_temperature    225(2)
_cell_measurement_theta_max      22.678
_cell_measurement_theta_min      1.91
_cell_volume                     3422.45(16)
_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 0.822
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.65524
_diffrn_reflns_av_R_equivalents  0.0908
_diffrn_reflns_av_unetI/netI     0.0732
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.822
_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            35250
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.822
_diffrn_reflns_theta_full        23.150
_diffrn_reflns_theta_max         32.904
_diffrn_reflns_theta_min         1.916
_exptl_absorpt_coefficient_mu    0.439
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1424
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         6719
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.1888
_refine_ls_R_factor_gt           0.1058
_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)+(0.0169P)²+2.5975P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1460
_refine_ls_wR_factor_ref         0.1712
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3748
_reflns_number_total             6719
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Bia_Portho_225K.cif
_cod_data_source_block           Bia_dw4400_225K
_cod_depositor_comments
'Adding full bibliography for 2312165--2312274.cif.'
_cod_database_code               2312246
_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 0.57709(3) 0.04634(17) Uani 1 2 d S T P . .
S002 S 0.91105(9) 0.55714(8) 0.39535(5) 0.0831(4) Uani 1 1 d . . . . .
N003 N 0.7450(2) 0.84430(16) 0.67547(13) 0.0501(6) Uani 1 1 d . . . . .
N004 N 0.8014(2) 0.6608(2) 0.49713(15) 0.0630(7) Uani 1 1 d . . . . .
N005 N 0.91070(19) 0.79599(18) 0.59457(14) 0.0514(6) Uani 1 1 d . . . . .
C006 C 0.6567(2) 0.8612(2) 0.72142(16) 0.0477(7) Uani 1 1 d . . . . .
C007 C 0.5640(2) 0.8830(2) 0.68628(17) 0.0528(8) Uani 1 1 d . . . . .
H007 H 0.561232 0.889876 0.633853 0.063 Uiso 1 1 calc R U . . .
C008 C 0.9263(3) 0.8477(2) 0.65571(18) 0.0543(8) Uani 1 1 d . . . . .
C009 C 0.8333(3) 0.8714(2) 0.69804(18) 0.0560(8) Uani 1 1 d . . . . .
H009 H 0.838359 0.906293 0.741480 0.067 Uiso 1 1 calc R U . . .
C00A C 0.6600(3) 0.8509(2) 0.79954(17) 0.0577(8) Uani 1 1 d . . . . .
H00A H 0.721801 0.836145 0.823379 0.069 Uiso 1 1 calc R U . . .
C00B C 0.4779(3) 0.8841(2) 0.80740(18) 0.0546(8) Uani 1 1 d . . . . .
C00C C 0.4764(3) 0.8942(2) 0.72918(18) 0.0554(8) Uani 1 1 d . . . . .
H00C H 0.414591 0.909035 0.705273 0.066 Uiso 1 1 calc R U . . .
C00D C 0.8471(2) 0.6182(2) 0.45461(16) 0.0522(8) Uani 1 1 d . . . . .
C00E C 0.5709(3) 0.8626(2) 0.84196(18) 0.0621(9) Uani 1 1 d . . . . .
H00E H 0.573556 0.855967 0.894411 0.075 Uiso 1 1 calc R U . . .
C00F C 0.3825(3) 0.8976(2) 0.8526(2) 0.0609(9) Uani 1 1 d . . . . .
C00G C 0.9940(3) 0.7730(2) 0.5536(2) 0.0623(9) Uani 1 1 d . . . . .
H00G H 0.984725 0.737707 0.510716 0.075 Uiso 1 1 calc R U . . .
C00H C 0.3850(3) 0.9423(3) 0.9219(2) 0.0682(10) Uani 1 1 d . . . . .
H00H H 0.447784 0.962928 0.940734 0.082 Uiso 1 1 calc R U . . .
C00I C 1.0231(3) 0.8769(3) 0.6777(2) 0.0732(10) Uani 1 1 d . . . . .
H00I H 1.031183 0.912760 0.720297 0.088 Uiso 1 1 calc R U . . .
C00J C 0.2877(3) 0.8670(3) 0.8269(2) 0.0787(11) Uani 1 1 d . . . . .
H00J H 0.283809 0.836445 0.781102 0.094 Uiso 1 1 calc R U . . .
C00K C 0.1983(4) 0.8813(3) 0.8690(3) 0.0924(13) Uani 1 1 d . . . . .
H00K H 0.135160 0.860377 0.851121 0.111 Uiso 1 1 calc R U . . .
C00L C 1.1068(3) 0.8517(3) 0.6351(3) 0.0861(13) Uani 1 1 d . . . . .
H00L H 1.172992 0.869927 0.648758 0.103 Uiso 1 1 calc R U . . .
C00M C 0.2951(4) 0.9564(3) 0.9632(2) 0.0810(12) Uani 1 1 d . . . . .
H00M H 0.297940 0.986688 1.009175 0.097 Uiso 1 1 calc R U . . .
C00N C 0.2029(4) 0.9261(3) 0.9365(3) 0.0879(13) Uani 1 1 d . . . . .
H00N H 0.142723 0.935920 0.964183 0.105 Uiso 1 1 calc R U . . .
C00O C 1.0925(3) 0.7996(3) 0.5724(2) 0.0798(11) Uani 1 1 d . . . . .
H00O H 1.148562 0.782324 0.542801 0.096 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 93.47(16) 2_665 . ?
N004 Fe01 N005 101.28(11) 2_665 . ?
N004 Fe01 N005 89.73(11) . . ?
N004 Fe01 N005 89.73(11) 2_665 2_665 ?
N004 Fe01 N005 101.28(11) . 2_665 ?
N005 Fe01 N005 163.99(13) . 2_665 ?
N004 Fe01 N003 162.27(11) 2_665 2_665 ?
N004 Fe01 N003 96.22(10) . 2_665 ?
N005 Fe01 N003 93.60(10) . 2_665 ?
N005 Fe01 N003 73.84(10) 2_665 2_665 ?
N004 Fe01 N003 96.22(10) 2_665 . ?
N004 Fe01 N003 162.27(11) . . ?
N005 Fe01 N003 73.84(10) . . ?
N005 Fe01 N003 93.60(10) 2_665 . ?
N003 Fe01 N003 78.59(12) 2_665 . ?
C009 N003 C006 119.0(3) . . ?
C009 N003 Fe01 114.7(2) . . ?
C006 N003 Fe01 125.2(2) . . ?
C00D N004 Fe01 167.6(3) . . ?
C00G N005 C008 117.4(3) . . ?
C00G N005 Fe01 126.8(2) . . ?
C008 N005 Fe01 115.7(2) . . ?
C00A C006 C007 119.7(3) . . ?
C00A C006 N003 121.3(3) . . ?
C007 C006 N003 118.8(3) . . ?
C00C C007 C006 119.7(3) . . ?
N005 C008 C00I 123.0(3) . . ?
N005 C008 C009 115.3(3) . . ?
C00I C008 C009 121.7(3) . . ?
N003 C009 C008 120.0(3) . . ?
C00E C00A C006 119.8(3) . . ?
C00E C00B C00C 118.4(3) . . ?
C00E C00B C00F 121.2(3) . . ?
C00C C00B C00F 120.4(3) . . ?
C007 C00C C00B 121.5(3) . . ?
N004 C00D S002 179.3(3) . . ?
C00A C00E C00B 120.9(3) . . ?
C00J C00F C00H 117.8(3) . . ?
C00J C00F C00B 121.0(3) . . ?
C00H C00F C00B 121.1(3) . . ?
N005 C00G C00O 122.6(4) . . ?
C00M C00H C00F 120.9(4) . . ?
C00L C00I C008 118.3(4) . . ?
C00F C00J C00K 120.7(4) . . ?
C00N C00K C00J 120.3(5) . . ?
C00O C00L C00I 119.6(4) . . ?
C00N C00M C00H 120.1(4) . . ?
C00M C00N C00K 120.2(4) . . ?
C00L C00O C00G 119.2(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 2.055(3) 2_665 ?
Fe01 N004 2.055(3) . ?
Fe01 N005 2.211(3) . ?
Fe01 N005 2.211(3) 2_665 ?
Fe01 N003 2.239(2) 2_665 ?
Fe01 N003 2.239(2) . ?
S002 C00D 1.617(3) . ?
N003 C009 1.275(4) . ?
N003 C006 1.423(4) . ?
N004 C00D 1.149(4) . ?
N005 C00G 1.342(4) . ?
N005 C008 1.343(4) . ?
C006 C00A 1.386(4) . ?
C006 C007 1.388(4) . ?
C007 C00C 1.372(4) . ?
C008 C00I 1.381(5) . ?
C008 C009 1.460(5) . ?
C00A C00E 1.383(5) . ?
C00B C00E 1.386(4) . ?
C00B C00C 1.386(4) . ?
C00B C00F 1.483(5) . ?
C00F C00J 1.385(5) . ?
C00F C00H 1.394(5) . ?
C00G C00O 1.375(5) . ?
C00H C00M 1.387(5) . ?
C00I C00L 1.371(6) . ?
C00J C00K 1.389(6) . ?
C00K C00N 1.368(6) . ?
C00L C00O 1.367(6) . ?
C00M C00N 1.361(6) . ?
