#------------------------------------------------------------------------------
#$Date: 2023-10-07 02:57:14 +0300 (Sat, 07 Oct 2023) $
#$Revision: 286839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/22/2312274.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_2312274
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                   12.9317(4)
_cell_length_b                   15.0357(4)
_cell_length_c                   17.6142(4)
_cell_measurement_reflns_used    3498
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      22.686
_cell_measurement_theta_min      1.9040
_cell_volume                     3424.86(16)
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.824
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.65524
_diffrn_reflns_av_R_equivalents  0.0925
_diffrn_reflns_av_unetI/netI     0.0754
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.824
_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            35337
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.824
_diffrn_reflns_theta_full        23.150
_diffrn_reflns_theta_max         32.891
_diffrn_reflns_theta_min         1.915
_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         0.261
_refine_diff_density_min         -0.307
_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         6733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.1948
_refine_ls_R_factor_gt           0.1078
_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)+(0.0021P)²+2.6091P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1425
_refine_ls_wR_factor_ref         0.1674
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3666
_reflns_number_total             6733
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Bia_Portho_230K.cif
_cod_data_source_block           Bia_dw4400_230K
_cod_depositor_comments
'Adding full bibliography for 2312165--2312274.cif.'
_cod_original_cell_volume        3424.85(16)
_cod_database_code               2312274
_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 0.57705(3) 0.04762(17) Uani 1 2 d S T P . .
S002 S 0.91086(9) 0.55719(8) 0.39538(5) 0.0855(4) Uani 1 1 d . . . . .
N003 N 0.7450(2) 0.84425(16) 0.67554(13) 0.0512(6) Uani 1 1 d . . . . .
N004 N 0.8014(2) 0.6608(2) 0.49719(15) 0.0644(7) Uani 1 1 d . . . . .
N005 N 0.91085(19) 0.79609(18) 0.59446(14) 0.0528(6) Uani 1 1 d . . . . .
C006 C 0.6566(2) 0.8612(2) 0.72117(16) 0.0498(7) Uani 1 1 d . . . . .
C007 C 0.5645(2) 0.8830(2) 0.68614(17) 0.0532(8) Uani 1 1 d . . . . .
H007 H 0.562073 0.890253 0.633734 0.064 Uiso 1 1 calc R U . . .
C008 C 0.9261(3) 0.8477(2) 0.65558(17) 0.0552(8) Uani 1 1 d . . . . .
C009 C 0.8331(3) 0.8714(2) 0.69806(18) 0.0582(8) Uani 1 1 d . . . . .
H009 H 0.838179 0.906378 0.741467 0.070 Uiso 1 1 calc R U . . .
C00A C 0.6598(3) 0.8508(2) 0.79957(18) 0.0593(8) Uani 1 1 d . . . . .
H00A H 0.721531 0.835887 0.823458 0.071 Uiso 1 1 calc R U . . .
C00B C 0.4778(3) 0.8842(2) 0.80756(18) 0.0566(8) Uani 1 1 d . . . . .
C00C C 0.4762(3) 0.8941(2) 0.72898(18) 0.0570(8) Uani 1 1 d . . . . .
H00C H 0.414416 0.908514 0.704915 0.068 Uiso 1 1 calc R U . . .
C00D C 0.8469(2) 0.6182(2) 0.45450(17) 0.0545(8) Uani 1 1 d . . . . .
C00E C 0.5707(3) 0.8627(2) 0.84192(18) 0.0623(9) Uani 1 1 d . . . . .
H00E H 0.573371 0.856088 0.894381 0.075 Uiso 1 1 calc R U . . .
C00F C 0.3824(3) 0.8978(2) 0.8525(2) 0.0621(9) Uani 1 1 d . . . . .
C00G C 0.9938(3) 0.7730(2) 0.55359(19) 0.0627(9) Uani 1 1 d . . . . .
H00G H 0.984536 0.737644 0.510832 0.075 Uiso 1 1 calc R U . . .
C00H C 0.3854(3) 0.9423(3) 0.9216(2) 0.0712(10) Uani 1 1 d . . . . .
H00H H 0.448207 0.962897 0.940474 0.085 Uiso 1 1 calc R U . . .
C00I C 1.0228(3) 0.8768(3) 0.6779(2) 0.0753(10) Uani 1 1 d . . . . .
H00I H 1.030794 0.912340 0.720674 0.090 Uiso 1 1 calc R U . . .
C00J C 0.2881(3) 0.8671(3) 0.8266(2) 0.0808(11) Uani 1 1 d . . . . .
H00J H 0.284416 0.836544 0.780835 0.097 Uiso 1 1 calc R U . . .
C00K C 0.1986(4) 0.8817(3) 0.8686(3) 0.0939(13) Uani 1 1 d . . . . .
H00K H 0.135445 0.861152 0.850372 0.113 Uiso 1 1 calc R U . . .
C00L C 1.1069(3) 0.8519(3) 0.6351(3) 0.0895(13) Uani 1 1 d . . . . .
H00L H 1.173038 0.870391 0.648718 0.107 Uiso 1 1 calc R U . . .
C00M C 0.2953(4) 0.9563(3) 0.9627(2) 0.0825(12) Uani 1 1 d . . . . .
H00M H 0.298029 0.986839 1.008562 0.099 Uiso 1 1 calc R U . . .
C00N C 0.2025(4) 0.9257(3) 0.9363(3) 0.0899(13) Uani 1 1 d . . . . .
H00N H 0.142435 0.934845 0.964239 0.108 Uiso 1 1 calc R U . . .
C00O C 1.0924(3) 0.7997(3) 0.5724(3) 0.0804(11) Uani 1 1 d . . . . .
H00O H 1.148458 0.782418 0.542790 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 93.54(16) . 2_665 ?
N004 Fe01 N005 89.71(11) . . ?
N004 Fe01 N005 101.23(11) 2_665 . ?
N004 Fe01 N005 101.23(11) . 2_665 ?
N004 Fe01 N005 89.71(11) 2_665 2_665 ?
N005 Fe01 N005 164.08(13) . 2_665 ?
N004 Fe01 N003 162.23(11) . . ?
N004 Fe01 N003 96.21(10) 2_665 . ?
N005 Fe01 N003 73.85(10) . . ?
N005 Fe01 N003 93.66(10) 2_665 . ?
N004 Fe01 N003 96.21(10) . 2_665 ?
N004 Fe01 N003 162.23(11) 2_665 2_665 ?
N005 Fe01 N003 93.66(10) . 2_665 ?
N005 Fe01 N003 73.85(10) 2_665 2_665 ?
N003 Fe01 N003 78.55(12) . 2_665 ?
C009 N003 C006 119.1(3) . . ?
C009 N003 Fe01 114.7(2) . . ?
C006 N003 Fe01 125.1(2) . . ?
C00D N004 Fe01 167.8(3) . . ?
C00G N005 C008 117.6(3) . . ?
C00G N005 Fe01 126.7(2) . . ?
C008 N005 Fe01 115.5(2) . . ?
C007 C006 C00A 119.7(3) . . ?
C007 C006 N003 118.9(3) . . ?
C00A C006 N003 121.2(3) . . ?
C00C C007 C006 119.9(3) . . ?
N005 C008 C00I 123.0(3) . . ?
N005 C008 C009 115.5(3) . . ?
C00I C008 C009 121.5(3) . . ?
N003 C009 C008 119.9(3) . . ?
C00E C00A C006 119.8(3) . . ?
C00E C00B C00C 118.2(3) . . ?
C00E C00B C00F 121.4(3) . . ?
C00C C00B C00F 120.4(3) . . ?
C007 C00C C00B 121.3(3) . . ?
N004 C00D S002 179.2(3) . . ?
C00A C00E C00B 121.1(3) . . ?
C00J C00F C00H 118.3(4) . . ?
C00J C00F C00B 120.9(3) . . ?
C00H C00F C00B 120.8(3) . . ?
N005 C00G C00O 122.5(4) . . ?
C00M C00H C00F 120.4(4) . . ?
C00L C00I C008 118.3(4) . . ?
C00F C00J C00K 120.5(4) . . ?
C00N C00K C00J 120.6(5) . . ?
C00O C00L C00I 119.3(4) . . ?
C00N C00M C00H 120.6(4) . . ?
C00K C00N C00M 119.6(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 2.054(3) . ?
Fe01 N004 2.054(3) 2_665 ?
Fe01 N005 2.214(3) . ?
Fe01 N005 2.214(3) 2_665 ?
Fe01 N003 2.241(2) . ?
Fe01 N003 2.241(2) 2_665 ?
S002 C00D 1.616(3) . ?
N003 C009 1.273(4) . ?
N003 C006 1.420(4) . ?
N004 C00D 1.150(4) . ?
N005 C00G 1.338(4) . ?
N005 C008 1.341(4) . ?
C006 C007 1.381(4) . ?
C006 C00A 1.390(4) . ?
C007 C00C 1.379(4) . ?
C008 C00I 1.382(5) . ?
C008 C009 1.461(5) . ?
C00A C00E 1.384(5) . ?
C00B C00E 1.384(4) . ?
C00B C00C 1.392(4) . ?
C00B C00F 1.479(5) . ?
C00F C00J 1.382(5) . ?
C00F C00H 1.390(5) . ?
C00G C00O 1.377(5) . ?
C00H C00M 1.388(5) . ?
C00I C00L 1.375(6) . ?
C00J C00K 1.390(6) . ?
C00K C00N 1.365(6) . ?
C00L C00O 1.369(6) . ?
C00M C00N 1.367(6) . ?
