#------------------------------------------------------------------------------
#$Date: 2023-10-07 02:57:14 +0300 (Sat, 07 Oct 2023) $
#$Revision: 286839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/22/2312222.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_2312222
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                   12.9526(5)
_cell_length_b                   15.1884(6)
_cell_length_c                   17.6032(6)
_cell_measurement_reflns_used    2724
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.921
_cell_measurement_theta_min      1.886
_cell_volume                     3463.1(2)
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.826
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.65524
_diffrn_reflns_av_R_equivalents  0.0968
_diffrn_reflns_av_unetI/netI     0.0724
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.826
_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            36519
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.826
_diffrn_reflns_theta_full        23.150
_diffrn_reflns_theta_max         32.994
_diffrn_reflns_theta_min         1.905
_exptl_absorpt_coefficient_mu    0.434
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1424
_refine_diff_density_max         0.159
_refine_diff_density_min         -0.179
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         6886
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.2285
_refine_ls_R_factor_gt           0.1033
_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)+(0.0325P)²+1.3626P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1492
_refine_ls_wR_factor_ref         0.1870
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2854
_reflns_number_total             6886
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Bia_Portho_295K.cif
_cod_data_source_block           Bia_dw4400_295K
_cod_depositor_comments
'Adding full bibliography for 2312165--2312274.cif.'
_cod_database_code               2312222
_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 0.57610(3) 0.0663(2) Uani 1 2 d S T P . .
S002 S 0.90898(10) 0.55770(9) 0.39544(6) 0.1158(5) Uani 1 1 d . . . . .
N003 N 0.7444(2) 0.84362(17) 0.67469(14) 0.0689(7) Uani 1 1 d . . . . .
N004 N 0.8007(3) 0.6612(2) 0.49629(16) 0.0861(9) Uani 1 1 d . . . . .
N005 N 0.9101(2) 0.79604(19) 0.59378(15) 0.0714(7) Uani 1 1 d . . . . .
C006 C 0.6559(3) 0.8603(2) 0.72048(18) 0.0678(8) Uani 1 1 d . . . . .
C007 C 0.5643(3) 0.8826(2) 0.68556(19) 0.0738(9) Uani 1 1 d . . . . .
H007 H 0.561837 0.889906 0.633139 0.089 Uiso 1 1 calc R U . . .
C008 C 0.9251(3) 0.8473(2) 0.6551(2) 0.0748(9) Uani 1 1 d . . . . .
C009 C 0.8321(3) 0.8703(2) 0.6971(2) 0.0784(10) Uani 1 1 d . . . . .
H009 H 0.836953 0.904667 0.740651 0.094 Uiso 1 1 calc R U . . .
C00A C 0.6589(3) 0.8501(2) 0.79851(19) 0.0814(10) Uani 1 1 d . . . . .
H00A H 0.720474 0.835123 0.822423 0.098 Uiso 1 1 calc R U . . .
C00B C 0.4778(3) 0.8839(2) 0.8065(2) 0.0752(9) Uani 1 1 d . . . . .
C00C C 0.4767(3) 0.8940(2) 0.7283(2) 0.0792(10) Uani 1 1 d . . . . .
H00C H 0.415158 0.908736 0.704181 0.095 Uiso 1 1 calc R U . . .
C00D C 0.8461(3) 0.6192(2) 0.45419(19) 0.0733(9) Uani 1 1 d . . . . .
C00E C 0.5705(3) 0.8623(3) 0.8408(2) 0.0860(11) Uani 1 1 d . . . . .
H00E H 0.573152 0.855948 0.893288 0.103 Uiso 1 1 calc R U . . .
C00F C 0.3827(3) 0.8978(3) 0.8512(2) 0.0834(10) Uani 1 1 d . . . . .
C00G C 0.9930(3) 0.7735(3) 0.5531(2) 0.0869(11) Uani 1 1 d . . . . .
H00G H 0.984149 0.738269 0.510376 0.104 Uiso 1 1 calc R U . . .
C00H C 0.3851(3) 0.9419(3) 0.9199(2) 0.0947(12) Uani 1 1 d . . . . .
H00H H 0.447843 0.962346 0.938665 0.114 Uiso 1 1 calc R U . . .
C00I C 1.0213(4) 0.8762(3) 0.6768(3) 0.1020(13) Uani 1 1 d . . . . .
H00I H 1.029072 0.911613 0.719553 0.122 Uiso 1 1 calc R U . . .
C00J C 0.2890(4) 0.8675(3) 0.8263(3) 0.1115(14) Uani 1 1 d . . . . .
H00J H 0.285438 0.836421 0.780869 0.134 Uiso 1 1 calc R U . . .
C00K C 0.1992(4) 0.8822(4) 0.8677(3) 0.1272(17) Uani 1 1 d . . . . .
H00K H 0.136181 0.861762 0.849451 0.153 Uiso 1 1 calc R U . . .
C00L C 1.1055(4) 0.8520(4) 0.6345(3) 0.1186(16) Uani 1 1 d . . . . .
H00L H 1.171399 0.870418 0.648098 0.142 Uiso 1 1 calc R U . . .
C00M C 0.2953(5) 0.9563(3) 0.9614(3) 0.1115(15) Uani 1 1 d . . . . .
H00M H 0.298009 0.986300 1.007385 0.134 Uiso 1 1 calc R U . . .
C00N C 0.2034(5) 0.9261(4) 0.9344(3) 0.1218(17) Uani 1 1 d . . . . .
H00N H 0.143267 0.935834 0.961985 0.146 Uiso 1 1 calc R U . . .
C00O C 1.0909(3) 0.8003(4) 0.5720(3) 0.1074(14) Uani 1 1 d . . . . .
H00O H 1.146930 0.783333 0.542416 0.129 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 93.74(17) . 2_665 ?
N004 Fe01 N005 90.22(12) . . ?
N004 Fe01 N005 100.87(12) 2_665 . ?
N004 Fe01 N005 100.87(12) . 2_665 ?
N004 Fe01 N005 90.22(12) 2_665 2_665 ?
N005 Fe01 N005 163.81(14) . 2_665 ?
N004 Fe01 N003 95.89(11) . 2_665 ?
N004 Fe01 N003 162.65(12) 2_665 2_665 ?
N005 Fe01 N003 93.50(11) . 2_665 ?
N005 Fe01 N003 73.82(11) 2_665 2_665 ?
N004 Fe01 N003 162.65(12) . . ?
N004 Fe01 N003 95.89(11) 2_665 . ?
N005 Fe01 N003 73.82(11) . . ?
N005 Fe01 N003 93.50(11) 2_665 . ?
N003 Fe01 N003 78.73(13) 2_665 . ?
C009 N003 C006 119.2(3) . . ?
C009 N003 Fe01 114.4(2) . . ?
C006 N003 Fe01 125.2(2) . . ?
C00D N004 Fe01 167.4(3) . . ?
C00G N005 C008 117.5(3) . . ?
C00G N005 Fe01 126.7(3) . . ?
C008 N005 Fe01 115.6(2) . . ?
C007 C006 C00A 119.6(3) . . ?
C007 C006 N003 118.9(3) . . ?
C00A C006 N003 121.3(3) . . ?
C00C C007 C006 119.9(3) . . ?
N005 C008 C00I 122.7(4) . . ?
N005 C008 C009 115.2(3) . . ?
C00I C008 C009 122.1(4) . . ?
N003 C009 C008 120.5(3) . . ?
C00E C00A C006 119.9(3) . . ?
C00E C00B C00C 118.0(3) . . ?
C00E C00B C00F 121.7(3) . . ?
C00C C00B C00F 120.3(4) . . ?
C007 C00C C00B 121.5(3) . . ?
N004 C00D S002 178.7(4) . . ?
C00A C00E C00B 121.1(3) . . ?
C00J C00F C00H 117.5(4) . . ?
C00J C00F C00B 121.4(4) . . ?
C00H C00F C00B 121.1(4) . . ?
N005 C00G C00O 122.5(4) . . ?
C00F C00H C00M 121.1(5) . . ?
C00L C00I C008 118.9(4) . . ?
C00F C00J C00K 121.4(5) . . ?
C00N C00K C00J 120.0(6) . . ?
C00O C00L C00I 118.8(4) . . ?
C00N C00M C00H 119.7(5) . . ?
C00K C00N C00M 120.3(5) . . ?
C00L C00O C00G 119.6(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) . ?
Fe01 N004 2.055(3) 2_665 ?
Fe01 N005 2.210(3) . ?
Fe01 N005 2.210(3) 2_665 ?
Fe01 N003 2.245(3) 2_665 ?
Fe01 N003 2.245(3) . ?
S002 C00D 1.614(4) . ?
N003 C009 1.269(4) . ?
N003 C006 1.424(4) . ?
N004 C00D 1.141(4) . ?
N005 C00G 1.336(4) . ?
N005 C008 1.345(4) . ?
C006 C007 1.379(4) . ?
C006 C00A 1.383(4) . ?
C007 C00C 1.372(5) . ?
C008 C00I 1.375(5) . ?
C008 C009 1.457(5) . ?
C00A C00E 1.379(5) . ?
C00B C00E 1.383(5) . ?
C00B C00C 1.385(5) . ?
C00B C00F 1.477(5) . ?
C00F C00J 1.370(6) . ?
C00F C00H 1.384(5) . ?
C00G C00O 1.372(6) . ?
C00H C00M 1.391(6) . ?
C00I C00L 1.372(6) . ?
C00J C00K 1.391(6) . ?
C00K C00N 1.352(7) . ?
C00L C00O 1.364(6) . ?
C00M C00N 1.360(7) . ?
