#------------------------------------------------------------------------------
#$Date: 2023-10-07 02:57:14 +0300 (Sat, 07 Oct 2023) $
#$Revision: 286839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/22/2312264.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_2312264
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                   12.9281(4)
_cell_length_b                   15.0131(4)
_cell_length_c                   17.6172(4)
_cell_measurement_reflns_used    3676
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      22.68
_cell_measurement_theta_min      1.91
_cell_volume                     3419.34(16)
_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 0.821
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.65524
_diffrn_reflns_av_R_equivalents  0.0878
_diffrn_reflns_av_unetI/netI     0.0711
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.821
_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            35242
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.821
_diffrn_reflns_theta_full        23.150
_diffrn_reflns_theta_max         32.919
_diffrn_reflns_theta_min         1.916
_exptl_absorpt_coefficient_mu    0.440
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1424
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         6713
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.1866
_refine_ls_R_factor_gt           0.1079
_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)+(0.0175P)²+2.5716P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1468
_refine_ls_wR_factor_ref         0.1700
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3859
_reflns_number_total             6713
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Bia_Portho_220K.cif
_cod_data_source_block           Bia_dw4400_220K
_cod_depositor_comments
'Adding full bibliography for 2312165--2312274.cif.'
_cod_database_code               2312264
_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 0.57717(3) 0.04532(17) Uani 1 2 d S T P . .
S002 S 0.91118(9) 0.55711(8) 0.39531(5) 0.0814(3) Uani 1 1 d . . . . .
N003 N 0.7451(2) 0.84432(16) 0.67537(13) 0.0484(5) Uani 1 1 d . . . . .
N004 N 0.8016(2) 0.66056(19) 0.49723(15) 0.0614(7) Uani 1 1 d . . . . .
N005 N 0.91077(19) 0.79609(17) 0.59464(14) 0.0502(6) Uani 1 1 d . . . . .
C006 C 0.6568(2) 0.8613(2) 0.72134(16) 0.0476(7) Uani 1 1 d . . . . .
C007 C 0.5643(2) 0.8831(2) 0.68641(16) 0.0503(7) Uani 1 1 d . . . . .
H007 H 0.561609 0.890307 0.634020 0.060 Uiso 1 1 calc R U . . .
C008 C 0.9264(3) 0.8480(2) 0.65586(17) 0.0539(8) Uani 1 1 d . . . . .
C009 C 0.8334(3) 0.8715(2) 0.69831(18) 0.0551(8) Uani 1 1 d . . . . .
H009 H 0.838355 0.906073 0.741933 0.066 Uiso 1 1 calc R U . . .
C00A C 0.6599(3) 0.8510(2) 0.79971(17) 0.0565(8) Uani 1 1 d . . . . .
H00A H 0.721762 0.836203 0.823556 0.068 Uiso 1 1 calc R U . . .
C00B C 0.4779(3) 0.8841(2) 0.80799(18) 0.0538(8) Uani 1 1 d . . . . .
C00C C 0.4764(3) 0.8941(2) 0.72934(18) 0.0554(8) Uani 1 1 d . . . . .
H00C H 0.414595 0.908638 0.705359 0.067 Uiso 1 1 calc R U . . .
C00D C 0.8473(2) 0.6181(2) 0.45449(17) 0.0512(7) Uani 1 1 d . . . . .
C00E C 0.5712(3) 0.8627(2) 0.84217(17) 0.0590(8) Uani 1 1 d . . . . .
H00E H 0.574032 0.856041 0.894614 0.071 Uiso 1 1 calc R U . . .
C00F C 0.3824(3) 0.8976(2) 0.85289(19) 0.0592(9) Uani 1 1 d . . . . .
C00G C 0.9939(3) 0.7732(2) 0.5536(2) 0.0610(9) Uani 1 1 d . . . . .
H00G H 0.984460 0.738016 0.510699 0.073 Uiso 1 1 calc R U . . .
C00H C 0.3852(3) 0.9422(3) 0.92194(19) 0.0667(10) Uani 1 1 d . . . . .
H00H H 0.448038 0.962719 0.940790 0.080 Uiso 1 1 calc R U . . .
C00I C 1.0231(3) 0.8767(3) 0.6777(2) 0.0713(10) Uani 1 1 d . . . . .
H00I H 1.031288 0.912288 0.720443 0.086 Uiso 1 1 calc R U . . .
C00J C 0.2878(3) 0.8673(3) 0.8270(2) 0.0773(11) Uani 1 1 d . . . . .
H00J H 0.284109 0.836973 0.781088 0.093 Uiso 1 1 calc R U . . .
C00K C 0.1980(4) 0.8815(3) 0.8688(3) 0.0915(13) Uani 1 1 d . . . . .
H00K H 0.134842 0.860841 0.850764 0.110 Uiso 1 1 calc R U . . .
C00L C 1.1071(3) 0.8517(3) 0.6351(3) 0.0849(12) Uani 1 1 d . . . . .
H00L H 1.173271 0.870065 0.648801 0.102 Uiso 1 1 calc R U . . .
C00M C 0.2951(4) 0.9564(3) 0.9631(2) 0.0806(12) Uani 1 1 d . . . . .
H00M H 0.297848 0.986766 1.009074 0.097 Uiso 1 1 calc R U . . .
C00N C 0.2028(4) 0.9260(3) 0.9364(3) 0.0862(13) Uani 1 1 d . . . . .
H00N H 0.142709 0.935464 0.964334 0.103 Uiso 1 1 calc R U . . .
C00O C 1.0925(3) 0.7995(3) 0.5723(2) 0.0778(11) Uani 1 1 d . . . . .
H00O H 1.148492 0.782037 0.542719 0.093 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 93.58(16) . 2_665 ?
N004 Fe01 N005 89.72(11) . . ?
N004 Fe01 N005 101.28(11) 2_665 . ?
N004 Fe01 N005 101.28(11) . 2_665 ?
N004 Fe01 N005 89.72(11) 2_665 2_665 ?
N005 Fe01 N005 164.00(13) . 2_665 ?
N004 Fe01 N003 96.15(10) . 2_665 ?
N004 Fe01 N003 162.19(11) 2_665 2_665 ?
N005 Fe01 N003 93.66(9) . 2_665 ?
N005 Fe01 N003 73.79(10) 2_665 2_665 ?
N004 Fe01 N003 162.19(11) . . ?
N004 Fe01 N003 96.15(10) 2_665 . ?
N005 Fe01 N003 73.79(10) . . ?
N005 Fe01 N003 93.66(9) 2_665 . ?
N003 Fe01 N003 78.65(12) 2_665 . ?
C009 N003 C006 118.7(3) . . ?
C009 N003 Fe01 114.9(2) . . ?
C006 N003 Fe01 125.2(2) . . ?
C00D N004 Fe01 167.6(3) . . ?
C00G N005 C008 117.4(3) . . ?
C00G N005 Fe01 126.7(2) . . ?
C008 N005 Fe01 115.7(2) . . ?
C007 C006 C00A 119.5(3) . . ?
C007 C006 N003 118.9(3) . . ?
C00A C006 N003 121.5(3) . . ?
C00C C007 C006 119.9(3) . . ?
N005 C008 C00I 122.7(3) . . ?
N005 C008 C009 115.3(3) . . ?
C00I C008 C009 122.0(3) . . ?
N003 C009 C008 119.8(3) . . ?
C00E C00A C006 120.0(3) . . ?
C00E C00B C00C 118.0(3) . . ?
C00E C00B C00F 121.7(3) . . ?
C00C C00B C00F 120.3(3) . . ?
C007 C00C C00B 121.5(3) . . ?
N004 C00D S002 179.1(3) . . ?
C00A C00E C00B 121.1(3) . . ?
C00J C00F C00H 118.0(3) . . ?
C00J C00F C00B 121.1(3) . . ?
C00H C00F C00B 120.9(3) . . ?
N005 C00G C00O 122.7(4) . . ?
C00M C00H C00F 120.7(4) . . ?
C00L C00I C008 118.8(4) . . ?
C00F C00J C00K 120.9(4) . . ?
C00N C00K C00J 119.9(5) . . ?
C00O C00L C00I 119.2(4) . . ?
C00N C00M C00H 120.2(4) . . ?
C00M C00N C00K 120.3(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 2.057(3) . ?
Fe01 N004 2.057(3) 2_665 ?
Fe01 N005 2.212(3) . ?
Fe01 N005 2.212(3) 2_665 ?
Fe01 N003 2.237(2) 2_665 ?
Fe01 N003 2.237(2) . ?
S002 C00D 1.615(3) . ?
N003 C009 1.277(4) . ?
N003 C006 1.423(4) . ?
N004 C00D 1.150(4) . ?
N005 C00G 1.340(4) . ?
N005 C008 1.345(4) . ?
C006 C007 1.384(4) . ?
C006 C00A 1.390(4) . ?
C007 C00C 1.375(4) . ?
C008 C00I 1.377(5) . ?
C008 C009 1.459(5) . ?
C00A C00E 1.381(4) . ?
C00B C00E 1.385(4) . ?
C00B C00C 1.394(4) . ?
C00B C00F 1.480(5) . ?
C00F C00J 1.383(5) . ?
C00F C00H 1.389(5) . ?
C00G C00O 1.375(5) . ?
C00H C00M 1.389(5) . ?
C00I C00L 1.372(5) . ?
C00J C00K 1.391(6) . ?
C00K C00N 1.367(6) . ?
C00L C00O 1.370(6) . ?
C00M C00N 1.362(6) . ?
