#------------------------------------------------------------------------------
#$Date: 2023-10-07 02:57:14 +0300 (Sat, 07 Oct 2023) $
#$Revision: 286839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/22/2312251.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_2312251
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                   12.9344(4)
_cell_length_b                   15.0561(5)
_cell_length_c                   17.6128(4)
_cell_measurement_reflns_used    3358
_cell_measurement_temperature    235(2)
_cell_measurement_theta_max      22.6760
_cell_measurement_theta_min      1.9030
_cell_volume                     3429.95(17)
_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 0.825
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.65524
_diffrn_reflns_av_R_equivalents  0.0885
_diffrn_reflns_av_unetI/netI     0.0663
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.825
_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            36033
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.825
_diffrn_reflns_theta_full        23.150
_diffrn_reflns_theta_max         33.020
_diffrn_reflns_theta_min         1.914
_exptl_absorpt_coefficient_mu    0.438
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1424
_refine_diff_density_max         0.212
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         6822
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.1853
_refine_ls_R_factor_gt           0.0950
_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)+(0.0280P)²+1.7500P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1670
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3407
_reflns_number_total             6822
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Bia_Portho_235K.cif
_cod_data_source_block           Bia_dw4400_235K
_cod_depositor_comments
'Adding full bibliography for 2312165--2312274.cif.'
_cod_original_cell_volume        3429.94(17)
_cod_database_code               2312251
_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 0.57693(3) 0.05261(17) Uani 1 2 d S T P . .
S002 S 0.91062(9) 0.55722(8) 0.39542(5) 0.0920(4) Uani 1 1 d . . . . .
N003 N 0.7448(2) 0.84411(15) 0.67519(13) 0.0563(5) Uani 1 1 d . . . . .
N004 N 0.8015(2) 0.66065(19) 0.49676(14) 0.0700(7) Uani 1 1 d . . . . .
N005 N 0.91068(19) 0.79608(17) 0.59442(13) 0.0575(6) Uani 1 1 d . . . . .
C006 C 0.6566(2) 0.86095(19) 0.72123(16) 0.0549(7) Uani 1 1 d . . . . .
C007 C 0.5641(2) 0.88293(19) 0.68625(16) 0.0586(7) Uani 1 1 d . . . . .
H007 H 0.561524 0.890050 0.633833 0.070 Uiso 1 1 calc R U . . .
C008 C 0.9260(2) 0.8476(2) 0.65556(17) 0.0604(8) Uani 1 1 d . . . . .
C009 C 0.8331(3) 0.8711(2) 0.69813(17) 0.0627(8) Uani 1 1 d . . . . .
H009 H 0.838161 0.905570 0.741786 0.075 Uiso 1 1 calc R U . . .
C00A C 0.6597(3) 0.8506(2) 0.79939(17) 0.0649(8) Uani 1 1 d . . . . .
H00A H 0.721460 0.835781 0.823275 0.078 Uiso 1 1 calc R U . . .
C00B C 0.4779(3) 0.8840(2) 0.80733(18) 0.0614(8) Uani 1 1 d . . . . .
C00C C 0.4763(3) 0.8942(2) 0.72906(18) 0.0631(8) Uani 1 1 d . . . . .
H00C H 0.414533 0.908911 0.705101 0.076 Uiso 1 1 calc R U . . .
C00D C 0.8471(2) 0.6182(2) 0.45422(16) 0.0594(8) Uani 1 1 d . . . . .
C00E C 0.5709(3) 0.8625(2) 0.84179(17) 0.0683(9) Uani 1 1 d . . . . .
H00E H 0.573519 0.855882 0.894253 0.082 Uiso 1 1 calc R U . . .
C00F C 0.3822(3) 0.8978(2) 0.85263(19) 0.0674(9) Uani 1 1 d . . . . .
C00G C 0.9936(3) 0.7732(2) 0.55346(19) 0.0691(9) Uani 1 1 d . . . . .
H00G H 0.984279 0.738088 0.510576 0.083 Uiso 1 1 calc R U . . .
C00H C 0.3851(3) 0.9424(2) 0.92141(19) 0.0761(10) Uani 1 1 d . . . . .
H00H H 0.447829 0.963216 0.940050 0.091 Uiso 1 1 calc R U . . .
C00I C 1.0226(3) 0.8767(3) 0.6773(2) 0.0811(10) Uani 1 1 d . . . . .
H00I H 1.030723 0.912397 0.719985 0.097 Uiso 1 1 calc R U . . .
C00J C 0.2881(3) 0.8673(3) 0.8266(2) 0.0870(11) Uani 1 1 d . . . . .
H00J H 0.284503 0.836904 0.780690 0.104 Uiso 1 1 calc R U . . .
C00K C 0.1984(3) 0.8816(3) 0.8685(3) 0.1013(13) Uani 1 1 d . . . . .
H00K H 0.135318 0.860856 0.850406 0.122 Uiso 1 1 calc R U . . .
C00L C 1.1067(3) 0.8517(3) 0.6346(3) 0.0957(13) Uani 1 1 d . . . . .
H00L H 1.172783 0.870251 0.648130 0.115 Uiso 1 1 calc R U . . .
C00M C 0.2952(4) 0.9561(3) 0.9627(2) 0.0904(12) Uani 1 1 d . . . . .
H00M H 0.298043 0.986006 1.008907 0.108 Uiso 1 1 calc R U . . .
C00N C 0.2027(4) 0.9261(3) 0.9359(3) 0.0955(13) Uani 1 1 d . . . . .
H00N H 0.142530 0.935892 0.963630 0.115 Uiso 1 1 calc R U . . .
C00O C 1.0922(3) 0.7995(3) 0.5722(2) 0.0869(11) Uani 1 1 d . . . . .
H00O H 1.148287 0.781996 0.542745 0.104 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 93.51(15) 2_665 . ?
N004 Fe01 N005 101.22(10) 2_665 . ?
N004 Fe01 N005 89.78(10) . . ?
N004 Fe01 N005 89.79(10) 2_665 2_665 ?
N004 Fe01 N005 101.22(10) . 2_665 ?
N005 Fe01 N005 163.99(12) . 2_665 ?
N004 Fe01 N003 162.33(10) 2_665 2_665 ?
N004 Fe01 N003 96.14(9) . 2_665 ?
N005 Fe01 N003 93.61(9) . 2_665 ?
N005 Fe01 N003 73.84(9) 2_665 2_665 ?
N004 Fe01 N003 96.14(9) 2_665 . ?
N004 Fe01 N003 162.33(10) . . ?
N005 Fe01 N003 73.84(9) . . ?
N005 Fe01 N003 93.61(9) 2_665 . ?
N003 Fe01 N003 78.68(12) 2_665 . ?
C009 N003 C006 118.7(3) . . ?
C009 N003 Fe01 114.8(2) . . ?
C006 N003 Fe01 125.29(19) . . ?
C00D N004 Fe01 167.6(3) . . ?
C00G N005 C008 117.6(3) . . ?
C00G N005 Fe01 126.7(2) . . ?
C008 N005 Fe01 115.6(2) . . ?
C00A C006 C007 119.5(3) . . ?
C00A C006 N003 121.6(3) . . ?
C007 C006 N003 118.8(2) . . ?
C00C C007 C006 120.0(3) . . ?
N005 C008 C00I 122.7(3) . . ?
N005 C008 C009 115.5(3) . . ?
C00I C008 C009 121.7(3) . . ?
N003 C009 C008 119.7(3) . . ?
C00E C00A C006 119.9(3) . . ?
C00E C00B C00C 118.3(3) . . ?
C00E C00B C00F 121.3(3) . . ?
C00C C00B C00F 120.3(3) . . ?
C007 C00C C00B 121.3(3) . . ?
N004 C00D S002 179.0(3) . . ?
C00A C00E C00B 121.0(3) . . ?
C00J C00F C00H 118.4(3) . . ?
C00J C00F C00B 120.7(3) . . ?
C00H C00F C00B 121.0(3) . . ?
N005 C00G C00O 122.7(3) . . ?
C00F C00H C00M 120.6(4) . . ?
C00L C00I C008 118.6(4) . . ?
C00F C00J C00K 120.5(4) . . ?
C00N C00K C00J 120.3(4) . . ?
C00O C00L C00I 119.3(4) . . ?
C00N C00M C00H 120.3(4) . . ?
C00M C00N C00K 120.0(4) . . ?
C00L C00O C00G 119.1(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 2.061(3) 2_665 ?
Fe01 N004 2.061(3) . ?
Fe01 N005 2.213(2) . ?
Fe01 N005 2.213(2) 2_665 ?
Fe01 N003 2.238(2) 2_665 ?
Fe01 N003 2.238(2) . ?
S002 C00D 1.609(3) . ?
N003 C009 1.277(4) . ?
N003 C006 1.423(4) . ?
N004 C00D 1.148(4) . ?
N005 C00G 1.338(4) . ?
N005 C008 1.342(4) . ?
C006 C00A 1.386(4) . ?
C006 C007 1.386(4) . ?
C007 C00C 1.374(4) . ?
C008 C00I 1.379(4) . ?
C008 C009 1.460(4) . ?
C00A C00E 1.382(4) . ?
C00B C00E 1.385(4) . ?
C00B C00C 1.387(4) . ?
C00B C00F 1.487(4) . ?
C00F C00J 1.380(5) . ?
C00F C00H 1.385(5) . ?
C00G C00O 1.376(5) . ?
C00H C00M 1.387(5) . ?
C00I C00L 1.375(5) . ?
C00J C00K 1.391(5) . ?
C00K C00N 1.365(6) . ?
C00L C00O 1.364(6) . ?
C00M C00N 1.363(6) . ?
