#------------------------------------------------------------------------------
#$Date: 2023-10-07 02:57:14 +0300 (Sat, 07 Oct 2023) $
#$Revision: 286839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/22/2312249.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_2312249
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                   12.3353(2)
_cell_length_b                   14.6851(2)
_cell_length_c                   18.2738(2)
_cell_measurement_reflns_used    6229
_cell_measurement_temperature    090(2)
_cell_measurement_theta_max      29.642
_cell_measurement_theta_min      1.969
_cell_volume                     3310.21(8)
_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 0.813
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.65524
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.813
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            34166
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.813
_diffrn_reflns_theta_full        23.150
_diffrn_reflns_theta_max         32.972
_diffrn_reflns_theta_min         1.988
_exptl_absorpt_coefficient_mu    0.454
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1424
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         6467
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0664
_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)+(0.0458P)²+2.3431P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1245
_refine_ls_wR_factor_ref         0.1363
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4859
_reflns_number_total             6467
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Bia_Portho_090K.cif
_cod_data_source_block           Bia_dw4400_090K
_cod_depositor_comments
'Adding full bibliography for 2312165--2312274.cif.'
_cod_database_code               2312249
_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 0.59011(2) 0.01905(9) Uani 1 2 d S T P . .
S002 S 0.84741(4) 0.55992(4) 0.39212(3) 0.02743(12) Uani 1 1 d . . . . .
N003 N 0.72524(13) 0.83928(12) 0.66855(9) 0.0205(3) Uani 1 1 d . . . . .
N004 N 0.79075(14) 0.66498(12) 0.51387(9) 0.0241(3) Uani 1 1 d . . . . .
N005 N 0.89583(13) 0.80316(12) 0.59555(9) 0.0217(3) Uani 1 1 d . . . . .
C006 C 0.62707(15) 0.84943(14) 0.70942(10) 0.0207(4) Uani 1 1 d . . . . .
C007 C 0.53208(16) 0.87501(15) 0.67369(10) 0.0223(4) Uani 1 1 d . . . . .
H007 H 0.532604 0.886877 0.623702 0.027 Uiso 1 1 calc R U . . .
C008 C 0.90885(16) 0.86551(15) 0.64919(11) 0.0239(4) Uani 1 1 d . . . . .
C009 C 0.81007(17) 0.88293(14) 0.68990(11) 0.0234(4) Uani 1 1 d . . . . .
H009 H 0.808120 0.923250 0.729119 0.028 Uiso 1 1 calc R U . . .
C00A C 0.62564(16) 0.83145(15) 0.78419(11) 0.0237(4) Uani 1 1 d . . . . .
H00A H 0.688961 0.814135 0.808050 0.028 Uiso 1 1 calc R U . . .
C00B C 0.43370(16) 0.86567(14) 0.78857(11) 0.0227(4) Uani 1 1 d . . . . .
C00C C 0.43692(16) 0.88258(14) 0.71334(11) 0.0224(4) Uani 1 1 d . . . . .
H00C H 0.373517 0.899335 0.689317 0.027 Uiso 1 1 calc R U . . .
C00D C 0.81284(15) 0.62206(15) 0.46282(11) 0.0221(4) Uani 1 1 d . . . . .
C00E C 0.52953(17) 0.83944(15) 0.82300(11) 0.0251(4) Uani 1 1 d . . . . .
H00E H 0.529019 0.827077 0.872912 0.030 Uiso 1 1 calc R U . . .
C00F C 0.33221(16) 0.87995(15) 0.83103(11) 0.0244(4) Uani 1 1 d . . . . .
C00G C 0.98228(17) 0.78311(16) 0.55348(11) 0.0260(4) Uani 1 1 d . . . . .
H00G H 0.974409 0.740888 0.515929 0.031 Uiso 1 1 calc R U . . .
C00H C 0.33733(19) 0.91362(16) 0.90219(11) 0.0282(4) Uani 1 1 d . . . . .
H00H H 0.404517 0.925683 0.923151 0.034 Uiso 1 1 calc R U . . .
C00I C 1.00695(18) 0.90888(17) 0.66256(13) 0.0302(5) Uani 1 1 d . . . . .
H00I H 1.013220 0.951491 0.699970 0.036 Uiso 1 1 calc R U . . .
C00J C 0.23024(17) 0.86213(16) 0.80094(12) 0.0277(4) Uani 1 1 d . . . . .
H00J H 0.225087 0.839638 0.753493 0.033 Uiso 1 1 calc R U . . .
C00K C 0.13628(18) 0.87771(17) 0.84125(14) 0.0330(5) Uani 1 1 d . . . . .
H00K H 0.068854 0.865447 0.820720 0.040 Uiso 1 1 calc R U . . .
C00L C 1.09512(18) 0.88741(18) 0.61910(14) 0.0336(5) Uani 1 1 d . . . . .
H00L H 1.161727 0.915574 0.626578 0.040 Uiso 1 1 calc R U . . .
C00M C 0.2436(2) 0.92944(18) 0.94229(12) 0.0334(5) Uani 1 1 d . . . . .
H00M H 0.248474 0.952174 0.989679 0.040 Uiso 1 1 calc R U . . .
C00N C 0.1431(2) 0.91154(18) 0.91205(14) 0.0350(5) Uani 1 1 d . . . . .
H00N H 0.080366 0.922098 0.938993 0.042 Uiso 1 1 calc R U . . .
C00O C 1.08246(18) 0.82336(17) 0.56438(13) 0.0322(5) Uani 1 1 d . . . . .
H00O H 1.140991 0.807365 0.534995 0.039 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 88.02(11) . 2_665 ?
N004 Fe01 N005 91.02(7) . 2_665 ?
N004 Fe01 N005 93.15(7) 2_665 2_665 ?
N004 Fe01 N005 93.15(7) . . ?
N004 Fe01 N005 91.02(7) 2_665 . ?
N005 Fe01 N005 174.20(10) 2_665 . ?
N004 Fe01 N003 93.11(7) . 2_665 ?
N004 Fe01 N003 173.87(7) 2_665 2_665 ?
N005 Fe01 N003 80.81(7) 2_665 2_665 ?
N005 Fe01 N003 94.93(7) . 2_665 ?
N004 Fe01 N003 173.87(7) . . ?
N004 Fe01 N003 93.11(7) 2_665 . ?
N005 Fe01 N003 94.93(7) 2_665 . ?
N005 Fe01 N003 80.81(7) . . ?
N003 Fe01 N003 86.41(10) 2_665 . ?
C009 N003 C006 118.54(17) . . ?
C009 N003 Fe01 115.25(14) . . ?
C006 N003 Fe01 125.56(13) . . ?
C00D N004 Fe01 172.29(17) . . ?
C00G N005 C008 117.91(18) . . ?
C00G N005 Fe01 127.55(15) . . ?
C008 N005 Fe01 114.52(13) . . ?
C00A C006 C007 120.04(18) . . ?
C00A C006 N003 120.24(17) . . ?
C007 C006 N003 119.70(17) . . ?
C00C C007 C006 119.33(18) . . ?
N005 C008 C00I 122.8(2) . . ?
N005 C008 C009 113.07(17) . . ?
C00I C008 C009 124.1(2) . . ?
N003 C009 C008 116.07(19) . . ?
C00E C00A C006 119.80(18) . . ?
C00E C00B C00C 117.98(18) . . ?
C00E C00B C00F 121.16(18) . . ?
C00C C00B C00F 120.79(18) . . ?
C007 C00C C00B 121.66(18) . . ?
N004 C00D S002 178.12(19) . . ?
C00A C00E C00B 121.19(18) . . ?
C00H C00F C00J 118.34(19) . . ?
C00H C00F C00B 119.92(19) . . ?
C00J C00F C00B 121.73(19) . . ?
N005 C00G C00O 122.1(2) . . ?
C00M C00H C00F 121.0(2) . . ?
C00L C00I C008 118.6(2) . . ?
C00K C00J C00F 120.7(2) . . ?
C00N C00K C00J 120.1(2) . . ?
C00O C00L C00I 118.8(2) . . ?
C00N C00M C00H 120.3(2) . . ?
C00M C00N C00K 119.6(2) . . ?
C00L C00O C00G 119.7(2) . . ?
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 1.9371(18) . ?
Fe01 N004 1.9371(18) 2_665 ?
Fe01 N005 1.9635(17) 2_665 ?
Fe01 N005 1.9635(17) . ?
Fe01 N003 1.9663(17) 2_665 ?
Fe01 N003 1.9663(17) . ?
S002 C00D 1.638(2) . ?
N003 C009 1.288(3) . ?
N003 C006 1.430(2) . ?
N004 C00D 1.158(3) . ?
N005 C00G 1.347(3) . ?
N005 C008 1.351(3) . ?
C006 C00A 1.392(3) . ?
C006 C007 1.393(3) . ?
C007 C00C 1.384(3) . ?
C008 C00I 1.389(3) . ?
C008 C009 1.450(3) . ?
C00A C00E 1.386(3) . ?
C00B C00E 1.393(3) . ?
C00B C00C 1.398(3) . ?
C00B C00F 1.488(3) . ?
C00F C00H 1.393(3) . ?
C00F C00J 1.397(3) . ?
C00G C00O 1.384(3) . ?
C00H C00M 1.388(3) . ?
C00I C00L 1.383(3) . ?
C00J C00K 1.392(3) . ?
C00K C00N 1.388(4) . ?
C00L C00O 1.382(4) . ?
C00M C00N 1.383(4) . ?
