#------------------------------------------------------------------------------
#$Date: 2023-10-07 02:57:14 +0300 (Sat, 07 Oct 2023) $
#$Revision: 286839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/22/2312253.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_2312253
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                   12.9555(5)
_cell_length_b                   15.2018(6)
_cell_length_c                   17.6028(6)
_cell_measurement_reflns_used    2666
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      20.932
_cell_measurement_theta_min      1.886
_cell_volume                     3466.8(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  0.0990
_diffrn_reflns_av_unetI/netI     0.0735
_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            36550
_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         32.977
_diffrn_reflns_theta_min         1.904
_exptl_absorpt_coefficient_mu    0.434
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1424
_refine_diff_density_max         0.178
_refine_diff_density_min         -0.197
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_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      1.147
_refine_ls_R_factor_all          0.2336
_refine_ls_R_factor_gt           0.1038
_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)+(0.0360P)²+1.2606P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1929
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2801
_reflns_number_total             6892
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Bia_Portho_300K.cif
_cod_data_source_block           Bia_dw4400_300K
_cod_depositor_comments
'Adding full bibliography for 2312165--2312274.cif.'
_cod_database_code               2312253
_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 0.57601(4) 0.0678(2) Uani 1 2 d S T P . .
S002 S 0.90899(10) 0.55779(10) 0.39548(6) 0.1181(5) Uani 1 1 d . . . . .
N003 N 0.7444(2) 0.84342(18) 0.67471(15) 0.0701(7) Uani 1 1 d . . . . .
N004 N 0.8010(3) 0.6614(2) 0.49656(16) 0.0886(9) Uani 1 1 d . . . . .
N005 N 0.9100(2) 0.7962(2) 0.59383(16) 0.0741(7) Uani 1 1 d . . . . .
C006 C 0.6563(3) 0.8603(2) 0.72021(18) 0.0698(9) Uani 1 1 d . . . . .
C007 C 0.5640(3) 0.8825(2) 0.68544(19) 0.0746(9) Uani 1 1 d . . . . .
H007 H 0.561411 0.889619 0.633006 0.090 Uiso 1 1 calc R U . . .
C008 C 0.9252(3) 0.8472(2) 0.6548(2) 0.0763(9) Uani 1 1 d . . . . .
C009 C 0.8323(3) 0.8700(2) 0.6972(2) 0.0796(10) Uani 1 1 d . . . . .
H009 H 0.837314 0.904036 0.740938 0.096 Uiso 1 1 calc R U . . .
C00A C 0.6593(3) 0.8498(3) 0.79840(19) 0.0826(10) Uani 1 1 d . . . . .
H00A H 0.720651 0.834482 0.822392 0.099 Uiso 1 1 calc R U . . .
C00B C 0.4781(3) 0.8840(2) 0.8062(2) 0.0769(10) Uani 1 1 d . . . . .
C00C C 0.4767(3) 0.8940(2) 0.7281(2) 0.0795(10) Uani 1 1 d . . . . .
H00C H 0.415145 0.908759 0.704045 0.095 Uiso 1 1 calc R U . . .
C00D C 0.8455(3) 0.6190(3) 0.45397(19) 0.0754(10) Uani 1 1 d . . . . .
C00E C 0.5706(3) 0.8621(3) 0.8403(2) 0.0883(11) Uani 1 1 d . . . . .
H00E H 0.573126 0.855436 0.892794 0.106 Uiso 1 1 calc R U . . .
C00F C 0.3831(3) 0.8978(3) 0.8512(2) 0.0862(11) Uani 1 1 d . . . . .
C00G C 0.9929(3) 0.7740(3) 0.5528(2) 0.0877(11) Uani 1 1 d . . . . .
H00G H 0.983774 0.739397 0.509691 0.105 Uiso 1 1 calc R U . . .
C00H C 0.3849(4) 0.9422(3) 0.9198(2) 0.0971(13) Uani 1 1 d . . . . .
H00H H 0.447398 0.962930 0.938581 0.116 Uiso 1 1 calc R U . . .
C00I C 1.0212(3) 0.8764(3) 0.6768(3) 0.1015(13) Uani 1 1 d . . . . .
H00I H 1.029075 0.911841 0.719411 0.122 Uiso 1 1 calc R U . . .
C00J C 0.2889(4) 0.8675(3) 0.8260(3) 0.1129(15) Uani 1 1 d . . . . .
H00J H 0.285505 0.836755 0.780398 0.135 Uiso 1 1 calc R U . . .
C00K C 0.1989(4) 0.8819(4) 0.8671(3) 0.1305(17) Uani 1 1 d . . . . .
H00K H 0.135940 0.861328 0.848976 0.157 Uiso 1 1 calc R U . . .
C00L C 1.1049(4) 0.8518(4) 0.6342(3) 0.1214(16) Uani 1 1 d . . . . .
H00L H 1.170780 0.870123 0.647900 0.146 Uiso 1 1 calc R U . . .
C00M C 0.2956(5) 0.9563(3) 0.9611(3) 0.1156(16) Uani 1 1 d . . . . .
H00M H 0.298335 0.986249 1.007174 0.139 Uiso 1 1 calc R U . . .
C00N C 0.2035(5) 0.9262(4) 0.9340(3) 0.1235(18) Uani 1 1 d . . . . .
H00N H 0.143399 0.936061 0.961619 0.148 Uiso 1 1 calc R U . . .
C00O C 1.0910(4) 0.8003(4) 0.5718(3) 0.1108(14) Uani 1 1 d . . . . .
H00O H 1.147126 0.783119 0.542451 0.133 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 94.03(18) . 2_665 ?
N004 Fe01 N005 90.20(12) . . ?
N004 Fe01 N005 100.95(12) 2_665 . ?
N004 Fe01 N005 100.95(12) . 2_665 ?
N004 Fe01 N005 90.20(12) 2_665 2_665 ?
N005 Fe01 N005 163.68(15) . 2_665 ?
N004 Fe01 N003 95.83(11) . 2_665 ?
N004 Fe01 N003 162.47(12) 2_665 2_665 ?
N005 Fe01 N003 93.48(11) . 2_665 ?
N005 Fe01 N003 73.72(11) 2_665 2_665 ?
N004 Fe01 N003 162.47(12) . . ?
N004 Fe01 N003 95.84(11) 2_665 . ?
N005 Fe01 N003 73.72(11) . . ?
N005 Fe01 N003 93.48(11) 2_665 . ?
N003 Fe01 N003 78.60(13) 2_665 . ?
C009 N003 C006 119.2(3) . . ?
C009 N003 Fe01 114.4(2) . . ?
C006 N003 Fe01 125.3(2) . . ?
C00D N004 Fe01 168.1(3) . . ?
C00G N005 C008 117.5(3) . . ?
C00G N005 Fe01 126.6(3) . . ?
C008 N005 Fe01 115.8(2) . . ?
C007 C006 C00A 119.4(3) . . ?
C007 C006 N003 119.3(3) . . ?
C00A C006 N003 121.1(3) . . ?
C00C C007 C006 120.1(3) . . ?
N005 C008 C00I 123.0(4) . . ?
N005 C008 C009 115.3(3) . . ?
C00I C008 C009 121.7(4) . . ?
N003 C009 C008 120.3(3) . . ?
C00E C00A C006 119.5(4) . . ?
C00E C00B C00C 118.0(3) . . ?
C00E C00B C00F 121.6(3) . . ?
C00C C00B C00F 120.4(4) . . ?
C007 C00C C00B 121.3(3) . . ?
N004 C00D S002 178.7(4) . . ?
C00A C00E C00B 121.6(3) . . ?
C00J C00F C00H 117.3(4) . . ?
C00J C00F C00B 121.1(4) . . ?
C00H C00F C00B 121.6(4) . . ?
N005 C00G C00O 122.5(4) . . ?
C00M C00H C00F 121.4(5) . . ?
C00L C00I C008 118.3(4) . . ?
C00F C00J C00K 121.5(5) . . ?
C00N C00K C00J 119.5(6) . . ?
C00O C00L C00I 119.6(4) . . ?
C00N C00M C00H 119.7(5) . . ?
C00K C00N C00M 120.6(5) . . ?
C00L C00O C00G 119.2(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 2.051(3) . ?
Fe01 N004 2.051(3) 2_665 ?
Fe01 N005 2.211(3) . ?
Fe01 N005 2.211(3) 2_665 ?
Fe01 N003 2.245(3) 2_665 ?
Fe01 N003 2.245(3) . ?
S002 C00D 1.613(4) . ?
N003 C009 1.271(4) . ?
N003 C006 1.418(4) . ?
N004 C00D 1.144(4) . ?
N005 C00G 1.338(4) . ?
N005 C008 1.339(4) . ?
C006 C007 1.384(4) . ?
C006 C00A 1.386(4) . ?
C007 C00C 1.369(5) . ?
C008 C00I 1.376(5) . ?
C008 C009 1.458(5) . ?
C00A C00E 1.378(5) . ?
C00B C00E 1.381(5) . ?
C00B C00C 1.384(5) . ?
C00B C00F 1.478(5) . ?
C00F C00J 1.378(6) . ?
C00F C00H 1.384(5) . ?
C00G C00O 1.373(6) . ?
C00H C00M 1.383(6) . ?
C00I C00L 1.370(6) . ?
C00J C00K 1.391(7) . ?
C00K C00N 1.358(7) . ?
C00L C00O 1.361(6) . ?
C00M C00N 1.364(7) . ?
