#------------------------------------------------------------------------------
#$Date: 2023-10-07 02:57:14 +0300 (Sat, 07 Oct 2023) $
#$Revision: 286839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/22/2312242.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_2312242
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                   12.9473(5)
_cell_length_b                   15.1502(6)
_cell_length_c                   17.6044(5)
_cell_measurement_reflns_used    2866
_cell_measurement_temperature    280(2)
_cell_measurement_theta_max      21.229
_cell_measurement_theta_min      1.889
_cell_volume                     3453.2(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 0.828
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.65524
_diffrn_reflns_av_R_equivalents  0.0927
_diffrn_reflns_av_unetI/netI     0.0694
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.828
_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            36387
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_theta_full        23.150
_diffrn_reflns_theta_max         32.986
_diffrn_reflns_theta_min         1.907
_exptl_absorpt_coefficient_mu    0.435
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1424
_refine_diff_density_max         0.199
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         6876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.2137
_refine_ls_R_factor_gt           0.1014
_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)+(0.0390P)²+1.2936P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1557
_refine_ls_wR_factor_ref         0.1912
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3040
_reflns_number_total             6876
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Bia_Portho_280K.cif
_cod_data_source_block           Bia_dw4400_280K
_cod_depositor_comments
'Adding full bibliography for 2312165--2312274.cif.'
_cod_database_code               2312242
_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 0.57634(3) 0.0623(2) Uani 1 2 d S T P . .
S002 S 0.90973(10) 0.55759(9) 0.39546(6) 0.1086(4) Uani 1 1 d . . . . .
N003 N 0.7446(2) 0.84382(17) 0.67481(14) 0.0650(6) Uani 1 1 d . . . . .
N004 N 0.8012(3) 0.6612(2) 0.49642(16) 0.0817(8) Uani 1 1 d . . . . .
N005 N 0.9103(2) 0.79617(19) 0.59412(15) 0.0680(7) Uani 1 1 d . . . . .
C006 C 0.6562(3) 0.8606(2) 0.72047(17) 0.0650(8) Uani 1 1 d . . . . .
C007 C 0.5645(3) 0.8827(2) 0.68548(18) 0.0694(9) Uani 1 1 d . . . . .
H007 H 0.562075 0.890009 0.633055 0.083 Uiso 1 1 calc R U . . .
C008 C 0.9256(3) 0.8475(2) 0.65506(19) 0.0710(9) Uani 1 1 d . . . . .
C009 C 0.8330(3) 0.8706(2) 0.69752(19) 0.0733(9) Uani 1 1 d . . . . .
H009 H 0.838116 0.904818 0.741199 0.088 Uiso 1 1 calc R U . . .
C00A C 0.6591(3) 0.8504(2) 0.79874(19) 0.0758(10) Uani 1 1 d . . . . .
H00A H 0.720759 0.835747 0.822721 0.091 Uiso 1 1 calc R U . . .
C00B C 0.4779(3) 0.8841(2) 0.8066(2) 0.0724(9) Uani 1 1 d . . . . .
C00C C 0.4767(3) 0.8941(2) 0.7282(2) 0.0737(9) Uani 1 1 d . . . . .
H00C H 0.415119 0.908721 0.704097 0.088 Uiso 1 1 calc R U . . .
C00D C 0.8462(3) 0.6187(2) 0.45414(18) 0.0692(9) Uani 1 1 d . . . . .
C00E C 0.5700(3) 0.8621(2) 0.8411(2) 0.0806(10) Uani 1 1 d . . . . .
H00E H 0.572305 0.855002 0.893593 0.097 Uiso 1 1 calc R U . . .
C00F C 0.3824(3) 0.8982(2) 0.8519(2) 0.0790(10) Uani 1 1 d . . . . .
C00G C 0.9932(3) 0.7734(3) 0.5529(2) 0.0823(10) Uani 1 1 d . . . . .
H00G H 0.984242 0.738285 0.510115 0.099 Uiso 1 1 calc R U . . .
C00H C 0.3849(3) 0.9420(3) 0.9205(2) 0.0903(12) Uani 1 1 d . . . . .
H00H H 0.447580 0.962260 0.939515 0.108 Uiso 1 1 calc R U . . .
C00I C 1.0217(3) 0.8768(3) 0.6773(3) 0.0949(12) Uani 1 1 d . . . . .
H00I H 1.029412 0.912518 0.719880 0.114 Uiso 1 1 calc R U . . .
C00J C 0.2884(4) 0.8676(3) 0.8263(3) 0.1040(13) Uani 1 1 d . . . . .
H00J H 0.284976 0.836838 0.780648 0.125 Uiso 1 1 calc R U . . .
C00K C 0.1988(4) 0.8820(4) 0.8676(3) 0.1215(16) Uani 1 1 d . . . . .
H00K H 0.135845 0.861470 0.849383 0.146 Uiso 1 1 calc R U . . .
C00L C 1.1057(3) 0.8519(3) 0.6347(3) 0.1113(15) Uani 1 1 d . . . . .
H00L H 1.171726 0.870012 0.648428 0.134 Uiso 1 1 calc R U . . .
C00M C 0.2950(4) 0.9564(3) 0.9616(3) 0.1056(14) Uani 1 1 d . . . . .
H00M H 0.297563 0.986820 1.007451 0.127 Uiso 1 1 calc R U . . .
C00N C 0.2030(4) 0.9260(4) 0.9349(3) 0.1158(17) Uani 1 1 d . . . . .
H00N H 0.142917 0.935354 0.962658 0.139 Uiso 1 1 calc R U . . .
C00O C 1.0913(3) 0.8005(3) 0.5722(3) 0.1011(13) Uani 1 1 d . . . . .
H00O H 1.147476 0.783769 0.542591 0.121 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 93.68(17) . 2_665 ?
N004 Fe01 N005 101.08(12) . 2_665 ?
N004 Fe01 N005 90.08(12) 2_665 2_665 ?
N004 Fe01 N005 90.08(12) . . ?
N004 Fe01 N005 101.08(12) 2_665 . ?
N005 Fe01 N005 163.74(14) 2_665 . ?
N004 Fe01 N003 162.46(12) . . ?
N004 Fe01 N003 95.96(11) 2_665 . ?
N005 Fe01 N003 93.54(10) 2_665 . ?
N005 Fe01 N003 73.71(11) . . ?
N004 Fe01 N003 95.97(11) . 2_665 ?
N004 Fe01 N003 162.46(12) 2_665 2_665 ?
N005 Fe01 N003 73.71(11) 2_665 2_665 ?
N005 Fe01 N003 93.54(10) . 2_665 ?
N003 Fe01 N003 78.77(13) . 2_665 ?
C009 N003 C006 119.2(3) . . ?
C009 N003 Fe01 114.5(2) . . ?
C006 N003 Fe01 125.1(2) . . ?
C00D N004 Fe01 167.8(3) . . ?
C008 N005 C00G 117.7(3) . . ?
C008 N005 Fe01 115.8(2) . . ?
C00G N005 Fe01 126.4(3) . . ?
C007 C006 C00A 119.6(3) . . ?
C007 C006 N003 119.0(3) . . ?
C00A C006 N003 121.3(3) . . ?
C00C C007 C006 119.9(3) . . ?
N005 C008 C00I 123.2(4) . . ?
N005 C008 C009 115.4(3) . . ?
C00I C008 C009 121.3(4) . . ?
N003 C009 C008 120.0(3) . . ?
C00E C00A C006 119.9(3) . . ?
C00E C00B C00C 118.3(3) . . ?
C00E C00B C00F 121.1(3) . . ?
C00C C00B C00F 120.6(3) . . ?
C007 C00C C00B 121.4(3) . . ?
N004 C00D S002 179.1(3) . . ?
C00B C00E C00A 120.9(3) . . ?
C00J C00F C00H 118.0(4) . . ?
C00J C00F C00B 120.7(4) . . ?
C00H C00F C00B 121.3(4) . . ?
N005 C00G C00O 121.9(4) . . ?
C00F C00H C00M 120.8(4) . . ?
C00L C00I C008 118.1(4) . . ?
C00F C00J C00K 120.9(5) . . ?
C00N C00K C00J 120.1(5) . . ?
C00O C00L C00I 119.3(4) . . ?
C00N C00M C00H 120.1(4) . . ?
C00M C00N C00K 120.1(5) . . ?
C00L C00O C00G 119.7(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 2.057(3) . ?
Fe01 N004 2.057(3) 2_665 ?
Fe01 N005 2.213(3) 2_665 ?
Fe01 N005 2.213(3) . ?
Fe01 N003 2.243(3) . ?
Fe01 N003 2.243(3) 2_665 ?
S002 C00D 1.613(4) . ?
N003 C009 1.278(4) . ?
N003 C006 1.421(4) . ?
N004 C00D 1.144(4) . ?
N005 C008 1.339(4) . ?
N005 C00G 1.340(4) . ?
C006 C007 1.379(4) . ?
C006 C00A 1.387(4) . ?
C007 C00C 1.374(4) . ?
C008 C00I 1.378(5) . ?
C008 C009 1.456(5) . ?
C00A C00E 1.385(5) . ?
C00B C00E 1.380(5) . ?
C00B C00C 1.388(5) . ?
C00B C00F 1.487(5) . ?
C00F C00J 1.379(6) . ?
C00F C00H 1.379(5) . ?
C00G C00O 1.377(5) . ?
C00H C00M 1.387(6) . ?
C00I C00L 1.374(6) . ?
C00J C00K 1.386(6) . ?
C00K C00N 1.360(7) . ?
C00L C00O 1.361(6) . ?
C00M C00N 1.360(7) . ?
