#------------------------------------------------------------------------------
#$Date: 2023-10-07 02:57:14 +0300 (Sat, 07 Oct 2023) $
#$Revision: 286839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/22/2312269.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_2312269
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                   12.9149(3)
_cell_length_b                   14.9270(4)
_cell_length_c                   17.6232(4)
_cell_measurement_reflns_used    4113
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      24.722
_cell_measurement_theta_min      2.178
_cell_volume                     3397.41(14)
_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 0.817
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.65524
_diffrn_reflns_av_R_equivalents  0.0854
_diffrn_reflns_av_unetI/netI     0.0671
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.817
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            34827
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.817
_diffrn_reflns_theta_full        23.150
_diffrn_reflns_theta_max         32.921
_diffrn_reflns_theta_min         1.922
_exptl_absorpt_coefficient_mu    0.443
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1424
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.230
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         6648
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.230
_refine_ls_R_factor_all          0.1627
_refine_ls_R_factor_gt           0.1052
_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)+(0.0348P)²+2.4598P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1565
_refine_ls_wR_factor_ref         0.1749
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4311
_reflns_number_total             6648
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Bia_Portho_180K.cif
_cod_data_source_block           Bia_dw4400_180K
_cod_depositor_comments
'Adding full bibliography for 2312165--2312274.cif.'
_cod_database_code               2312269
_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 0.57775(3) 0.03645(15) Uani 1 2 d S T P . .
S002 S 0.91211(8) 0.55666(8) 0.39525(5) 0.0660(3) Uani 1 1 d . . . . .
N003 N 0.74540(19) 0.84493(15) 0.67594(12) 0.0397(5) Uani 1 1 d . . . . .
N004 N 0.8018(2) 0.66055(18) 0.49746(14) 0.0497(6) Uani 1 1 d . . . . .
N005 N 0.91104(18) 0.79600(17) 0.59493(13) 0.0408(5) Uani 1 1 d . . . . .
C006 C 0.6570(2) 0.86164(19) 0.72186(15) 0.0385(6) Uani 1 1 d . . . . .
C007 C 0.5643(2) 0.88334(19) 0.68678(15) 0.0410(6) Uani 1 1 d . . . . .
H007 H 0.561684 0.890708 0.634408 0.049 Uiso 1 1 calc R U . . .
C008 C 0.9267(2) 0.8481(2) 0.65615(16) 0.0426(7) Uani 1 1 d . . . . .
C009 C 0.8337(2) 0.8721(2) 0.69892(16) 0.0450(7) Uani 1 1 d . . . . .
H009 H 0.838902 0.906811 0.742557 0.054 Uiso 1 1 calc R U . . .
C00A C 0.6606(2) 0.8513(2) 0.80005(16) 0.0456(7) Uani 1 1 d . . . . .
H00A H 0.722625 0.836589 0.823764 0.055 Uiso 1 1 calc R U . . .
C00B C 0.4780(2) 0.8842(2) 0.80841(16) 0.0437(7) Uani 1 1 d . . . . .
C00C C 0.4759(2) 0.8940(2) 0.72972(17) 0.0445(7) Uani 1 1 d . . . . .
H00C H 0.413821 0.907950 0.705785 0.053 Uiso 1 1 calc R U . . .
C00D C 0.8476(2) 0.6176(2) 0.45460(15) 0.0427(7) Uani 1 1 d . . . . .
C00E C 0.5716(3) 0.8629(2) 0.84266(17) 0.0490(7) Uani 1 1 d . . . . .
H00E H 0.574573 0.856386 0.895090 0.059 Uiso 1 1 calc R U . . .
C00F C 0.3818(3) 0.8977(2) 0.85329(18) 0.0479(7) Uani 1 1 d . . . . .
C00G C 0.9943(2) 0.7726(2) 0.55394(18) 0.0499(8) Uani 1 1 d . . . . .
H00G H 0.984935 0.736975 0.511204 0.060 Uiso 1 1 calc R U . . .
C00H C 0.3849(3) 0.9424(2) 0.92274(18) 0.0538(8) Uani 1 1 d . . . . .
H00H H 0.447888 0.962833 0.941571 0.065 Uiso 1 1 calc R U . . .
C00I C 1.0235(3) 0.8770(3) 0.6781(2) 0.0592(9) Uani 1 1 d . . . . .
H00I H 1.031587 0.913038 0.720717 0.071 Uiso 1 1 calc R U . . .
C00J C 0.2871(3) 0.8669(3) 0.8274(2) 0.0639(9) Uani 1 1 d . . . . .
H00J H 0.283378 0.836055 0.781653 0.077 Uiso 1 1 calc R U . . .
C00K C 0.1977(3) 0.8815(3) 0.8691(2) 0.0733(11) Uani 1 1 d . . . . .
H00K H 0.134350 0.861085 0.850823 0.088 Uiso 1 1 calc R U . . .
C00L C 1.1083(3) 0.8514(3) 0.6357(2) 0.0686(10) Uani 1 1 d . . . . .
H00L H 1.174598 0.869293 0.649630 0.082 Uiso 1 1 calc R U . . .
C00M C 0.2952(3) 0.9566(3) 0.9639(2) 0.0647(10) Uani 1 1 d . . . . .
H00M H 0.298271 0.987177 1.009828 0.078 Uiso 1 1 calc R U . . .
C00N C 0.2021(3) 0.9261(3) 0.9375(2) 0.0703(11) Uani 1 1 d . . . . .
H00N H 0.142052 0.935363 0.965580 0.084 Uiso 1 1 calc R U . . .
C00O C 1.0933(3) 0.7993(3) 0.5727(2) 0.0627(9) Uani 1 1 d . . . . .
H00O H 1.149246 0.782032 0.542860 0.075 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 93.09(15) . 2_665 ?
N004 Fe01 N005 89.42(10) . . ?
N004 Fe01 N005 101.45(10) 2_665 . ?
N004 Fe01 N005 101.44(10) . 2_665 ?
N004 Fe01 N005 89.42(10) 2_665 2_665 ?
N005 Fe01 N005 164.26(12) . 2_665 ?
N004 Fe01 N003 162.11(10) . . ?
N004 Fe01 N003 96.45(9) 2_665 . ?
N005 Fe01 N003 73.88(9) . . ?
N005 Fe01 N003 93.77(9) 2_665 . ?
N004 Fe01 N003 96.45(9) . 2_665 ?
N004 Fe01 N003 162.11(10) 2_665 2_665 ?
N005 Fe01 N003 93.77(9) . 2_665 ?
N005 Fe01 N003 73.88(9) 2_665 2_665 ?
N003 Fe01 N003 78.67(12) . 2_665 ?
C009 N003 C006 118.8(2) . . ?
C009 N003 Fe01 115.0(2) . . ?
C006 N003 Fe01 124.94(19) . . ?
C00D N004 Fe01 167.8(3) . . ?
C00G N005 C008 117.5(3) . . ?
C00G N005 Fe01 126.8(2) . . ?
C008 N005 Fe01 115.49(19) . . ?
C007 C006 C00A 119.9(3) . . ?
C007 C006 N003 118.7(2) . . ?
C00A C006 N003 121.3(3) . . ?
C00C C007 C006 119.8(3) . . ?
N005 C008 C00I 122.8(3) . . ?
N005 C008 C009 115.6(3) . . ?
C00I C008 C009 121.6(3) . . ?
N003 C009 C008 119.5(3) . . ?
C00E C00A C006 119.8(3) . . ?
C00E C00B C00C 118.2(3) . . ?
C00E C00B C00F 121.8(3) . . ?
C00C C00B C00F 119.9(3) . . ?
C007 C00C C00B 121.2(3) . . ?
N004 C00D S002 179.4(3) . . ?
C00A C00E C00B 121.1(3) . . ?
C00J C00F C00H 118.2(3) . . ?
C00J C00F C00B 121.2(3) . . ?
C00H C00F C00B 120.5(3) . . ?
N005 C00G C00O 122.6(3) . . ?
C00M C00H C00F 120.6(4) . . ?
C00L C00I C008 118.8(3) . . ?
C00F C00J C00K 120.6(4) . . ?
C00N C00K C00J 120.3(4) . . ?
C00O C00L C00I 118.9(3) . . ?
C00N C00M C00H 120.5(4) . . ?
C00M C00N C00K 119.6(4) . . ?
C00L C00O C00G 119.3(3) . . ?
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 2.057(3) . ?
Fe01 N004 2.057(3) 2_665 ?
Fe01 N005 2.211(2) . ?
Fe01 N005 2.211(2) 2_665 ?
Fe01 N003 2.237(2) . ?
Fe01 N003 2.237(2) 2_665 ?
S002 C00D 1.617(3) . ?
N003 C009 1.276(4) . ?
N003 C006 1.422(4) . ?
N004 C00D 1.154(4) . ?
N005 C00G 1.342(4) . ?
N005 C008 1.346(4) . ?
C006 C007 1.386(4) . ?
C006 C00A 1.387(4) . ?
C007 C00C 1.378(4) . ?
C008 C00I 1.378(4) . ?
C008 C009 1.462(4) . ?
C00A C00E 1.384(4) . ?
C00B C00E 1.388(4) . ?
C00B C00C 1.395(4) . ?
C00B C00F 1.487(4) . ?
C00F C00J 1.385(5) . ?
C00F C00H 1.394(5) . ?
C00G C00O 1.379(5) . ?
C00H C00M 1.383(5) . ?
C00I C00L 1.380(5) . ?
C00J C00K 1.386(5) . ?
C00K C00N 1.378(6) . ?
C00L C00O 1.370(5) . ?
C00M C00N 1.368(6) . ?
