#------------------------------------------------------------------------------
#$Date: 2023-10-07 02:57:14 +0300 (Sat, 07 Oct 2023) $
#$Revision: 286839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/22/2312245.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_2312245
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                   12.9442(4)
_cell_length_b                   15.1256(5)
_cell_length_c                   17.6073(5)
_cell_measurement_reflns_used    3030
_cell_measurement_temperature    270(2)
_cell_measurement_theta_max      22.695
_cell_measurement_theta_min      1.893
_cell_volume                     3447.31(18)
_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 0.829
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.65524
_diffrn_reflns_av_R_equivalents  0.0917
_diffrn_reflns_av_unetI/netI     0.0690
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.829
_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            36281
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.829
_diffrn_reflns_theta_full        23.150
_diffrn_reflns_theta_max         32.975
_diffrn_reflns_theta_min         1.909
_exptl_absorpt_coefficient_mu    0.436
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1424
_refine_diff_density_max         0.164
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         6865
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.2064
_refine_ls_R_factor_gt           0.0998
_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)+(0.0405P)²+1.3803P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1559
_refine_ls_wR_factor_ref         0.1907
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3138
_reflns_number_total             6865
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Bia_Portho_270K.cif
_cod_data_source_block           Bia_dw4400_270K
_cod_depositor_comments
'Adding full bibliography for 2312165--2312274.cif.'
_cod_database_code               2312245
_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 0.57645(3) 0.0595(2) Uani 1 2 d S T P . .
S002 S 0.90986(10) 0.55752(9) 0.39545(6) 0.1043(4) Uani 1 1 d . . . . .
N003 N 0.7447(2) 0.84394(17) 0.67509(14) 0.0631(6) Uani 1 1 d . . . . .
N004 N 0.8013(3) 0.6610(2) 0.49639(15) 0.0779(8) Uani 1 1 d . . . . .
N005 N 0.9104(2) 0.79600(19) 0.59411(15) 0.0653(7) Uani 1 1 d . . . . .
C006 C 0.6566(3) 0.8607(2) 0.72074(17) 0.0614(8) Uani 1 1 d . . . . .
C007 C 0.5643(3) 0.8827(2) 0.68564(17) 0.0658(8) Uani 1 1 d . . . . .
H007 H 0.561688 0.889794 0.633207 0.079 Uiso 1 1 calc R U . . .
C008 C 0.9256(3) 0.8473(2) 0.65525(19) 0.0678(9) Uani 1 1 d . . . . .
C009 C 0.8327(3) 0.8708(2) 0.69754(19) 0.0702(9) Uani 1 1 d . . . . .
H009 H 0.837753 0.905567 0.740972 0.084 Uiso 1 1 calc R U . . .
C00A C 0.6592(3) 0.8502(2) 0.79890(18) 0.0723(9) Uani 1 1 d . . . . .
H00A H 0.720711 0.835068 0.822923 0.087 Uiso 1 1 calc R U . . .
C00B C 0.4780(3) 0.8840(2) 0.80691(19) 0.0695(9) Uani 1 1 d . . . . .
C00C C 0.4765(3) 0.8941(2) 0.7285(2) 0.0713(9) Uani 1 1 d . . . . .
H00C H 0.414857 0.908895 0.704546 0.086 Uiso 1 1 calc R U . . .
C00D C 0.8464(3) 0.6185(2) 0.45417(18) 0.0670(9) Uani 1 1 d . . . . .
C00E C 0.5707(3) 0.8624(2) 0.84097(19) 0.0780(10) Uani 1 1 d . . . . .
H00E H 0.573386 0.855873 0.893451 0.094 Uiso 1 1 calc R U . . .
C00F C 0.3829(3) 0.8978(2) 0.8520(2) 0.0758(10) Uani 1 1 d . . . . .
C00G C 0.9935(3) 0.7737(3) 0.5531(2) 0.0791(10) Uani 1 1 d . . . . .
H00G H 0.984391 0.738984 0.510032 0.095 Uiso 1 1 calc R U . . .
C00H C 0.3848(3) 0.9420(3) 0.9207(2) 0.0874(12) Uani 1 1 d . . . . .
H00H H 0.447540 0.962573 0.939470 0.105 Uiso 1 1 calc R U . . .
C00I C 1.0216(3) 0.8765(3) 0.6773(2) 0.0915(12) Uani 1 1 d . . . . .
H00I H 1.029518 0.912219 0.719926 0.110 Uiso 1 1 calc R U . . .
C00J C 0.2881(4) 0.8680(3) 0.8262(3) 0.0997(13) Uani 1 1 d . . . . .
H00J H 0.284101 0.838116 0.780064 0.120 Uiso 1 1 calc R U . . .
C00K C 0.1986(4) 0.8820(3) 0.8683(3) 0.1142(15) Uani 1 1 d . . . . .
H00K H 0.135510 0.861118 0.850603 0.137 Uiso 1 1 calc R U . . .
C00L C 1.1057(4) 0.8516(3) 0.6346(3) 0.1080(14) Uani 1 1 d . . . . .
H00L H 1.171734 0.869854 0.648237 0.130 Uiso 1 1 calc R U . . .
C00M C 0.2957(4) 0.9562(3) 0.9622(2) 0.1002(14) Uani 1 1 d . . . . .
H00M H 0.298697 0.986029 1.008281 0.120 Uiso 1 1 calc R U . . .
C00N C 0.2035(4) 0.9263(3) 0.9353(3) 0.1088(15) Uani 1 1 d . . . . .
H00N H 0.143445 0.936306 0.963059 0.131 Uiso 1 1 calc R U . . .
C00O C 1.0916(3) 0.8000(3) 0.5722(3) 0.0980(13) Uani 1 1 d . . . . .
H00O H 1.147724 0.782700 0.542735 0.118 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 93.61(17) . 2_665 ?
N004 Fe01 N005 89.94(12) . . ?
N004 Fe01 N005 101.15(11) 2_665 . ?
N004 Fe01 N005 101.16(11) . 2_665 ?
N004 Fe01 N005 89.94(12) 2_665 2_665 ?
N005 Fe01 N005 163.84(14) . 2_665 ?
N004 Fe01 N003 162.39(11) . . ?
N004 Fe01 N003 96.08(10) 2_665 . ?
N005 Fe01 N003 73.78(10) . . ?
N005 Fe01 N003 93.54(10) 2_665 . ?
N004 Fe01 N003 96.08(10) . 2_665 ?
N004 Fe01 N003 162.39(11) 2_665 2_665 ?
N005 Fe01 N003 93.54(10) . 2_665 ?
N005 Fe01 N003 73.78(10) 2_665 2_665 ?
N003 Fe01 N003 78.64(13) . 2_665 ?
C009 N003 C006 119.1(3) . . ?
C009 N003 Fe01 114.6(2) . . ?
C006 N003 Fe01 125.2(2) . . ?
C00D N004 Fe01 167.9(3) . . ?
C00G N005 C008 117.5(3) . . ?
C00G N005 Fe01 126.8(3) . . ?
C008 N005 Fe01 115.6(2) . . ?
C00A C006 C007 119.4(3) . . ?
C00A C006 N003 121.5(3) . . ?
C007 C006 N003 118.9(3) . . ?
C00C C007 C006 119.9(3) . . ?
N005 C008 C00I 123.0(4) . . ?
N005 C008 C009 115.5(3) . . ?
C00I C008 C009 121.5(3) . . ?
N003 C009 C008 120.1(3) . . ?
C00E C00A C006 119.9(3) . . ?
C00E C00B C00C 118.0(3) . . ?
C00E C00B C00F 121.6(3) . . ?
C00C C00B C00F 120.4(3) . . ?
C007 C00C C00B 121.4(3) . . ?
N004 C00D S002 179.3(3) . . ?
C00A C00E C00B 121.4(3) . . ?
C00H C00F C00J 117.5(4) . . ?
C00H C00F C00B 121.5(4) . . ?
C00J C00F C00B 121.0(4) . . ?
N005 C00G C00O 122.6(4) . . ?
C00F C00H C00M 121.5(4) . . ?
C00L C00I C008 118.2(4) . . ?
C00F C00J C00K 120.8(5) . . ?
C00N C00K C00J 120.0(5) . . ?
C00O C00L C00I 119.5(4) . . ?
C00N C00M C00H 119.8(4) . . ?
C00K C00N C00M 120.4(5) . . ?
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 2.059(3) . ?
Fe01 N004 2.059(3) 2_665 ?
Fe01 N005 2.212(3) . ?
Fe01 N005 2.212(3) 2_665 ?
Fe01 N003 2.245(3) . ?
Fe01 N003 2.245(3) 2_665 ?
S002 C00D 1.611(4) . ?
N003 C009 1.272(4) . ?
N003 C006 1.418(4) . ?
N004 C00D 1.143(4) . ?
N005 C00G 1.338(4) . ?
N005 C008 1.341(4) . ?
C006 C00A 1.386(4) . ?
C006 C007 1.387(4) . ?
C007 C00C 1.375(4) . ?
C008 C00I 1.375(5) . ?
C008 C009 1.459(5) . ?
C00A C00E 1.377(5) . ?
C00B C00E 1.381(5) . ?
C00B C00C 1.389(5) . ?
C00B C00F 1.480(5) . ?
C00F C00H 1.382(5) . ?
C00F C00J 1.385(6) . ?
C00G C00O 1.372(5) . ?
C00H C00M 1.383(6) . ?
C00I C00L 1.376(6) . ?
C00J C00K 1.392(6) . ?
C00K C00N 1.359(6) . ?
C00L C00O 1.360(6) . ?
C00M C00N 1.360(7) . ?
