#------------------------------------------------------------------------------
#$Date: 2022-07-06 11:09:49 +0300 (Wed, 06 Jul 2022) $
#$Revision: 276618 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/03/7710316.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7710316
loop_
_publ_author_name
'Bhar, Kishalay'
'Guo, Wenbin'
'Gonidec, Mathieu'
'Nikhil Raj M, Venkata'
'Bhatt, Surabhi'
'Perdih, Franc'
'Guionneau, Philippe'
'Chastanet, Guillaume'
'Sharma, Anuj K.'
_publ_section_title
;
 High temperature spin crossover behaviour of mononuclear
 bis-(thiocyanato)iron(II) complexes with judiciously designed bidentate
 N-donor Schiff bases with varying substituents.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9302
_journal_page_last               9313
_journal_paper_doi               10.1039/d2dt00416j
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         '2(C40 H32 Fe N6 S2)'
_chemical_formula_sum            'C80 H64 Fe2 N12 S4'
_chemical_formula_weight         1433.37
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-05-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-05-08 deposited with the CCDC.	2022-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.6315(3)
_cell_length_b                   17.6315(3)
_cell_length_c                   12.1717(3)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      27.07
_cell_measurement_theta_min      2.34
_cell_volume                     3783.81(13)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      250.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1028
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            75739
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.287
_diffrn_reflns_theta_min         2.033
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0728 before and 0.0601 after correction.
The Ratio of minimum to maximum transmission is 0.8706.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       prism
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 999 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         4243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0461
_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)+(0.0431P)²+0.3851P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0922
_reflns_Friedel_coverage         0.733
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                2982
_reflns_number_total             4243
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt00416j2.cif
_cod_data_source_block           sample2324250k-final
_cod_depositor_comments
'Adding full bibliography for 7710305--7710325.cif.'
_cod_original_cell_volume        3783.81(16)
_cod_database_code               7710316
_shelx_shelxl_version_number     2014/7
_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.
;
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.918
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C17(H17), C18(H18)
2.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/2, x+1/2, z+1/4'
'-x, -y, z+1/2'
'y+1/2, -x+1/2, z+3/4'
'x+1/2, -y+1/2, -z+3/4'
'y, x, -z'
'-x+1/2, y+1/2, -z+1/4'
'-y, -x, -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
Fe1 Fe 0.09441(3) 0.09441(3) 0.5000 0.03024(19) Uani 1 2 d S T P . .
S1 S -0.16906(6) 0.10332(8) 0.57285(12) 0.0689(4) Uani 1 1 d . . . . .
N1 N 0.08106(15) 0.11592(15) 0.3434(2) 0.0299(7) Uani 1 1 d . . . . .
N2 N 0.20482(14) 0.09370(15) 0.4942(2) 0.0299(6) Uani 1 1 d . . . . .
N3 N -0.01566(17) 0.09451(18) 0.5212(2) 0.0381(7) Uani 1 1 d . . . . .
C1 C 0.0740(2) 0.0661(2) 0.2611(3) 0.0408(9) Uani 1 1 d . . . . .
H1 H 0.0762 0.0140 0.2774 0.049 Uiso 1 1 calc R U . . .
C2 C 0.0637(2) 0.0880(2) 0.1529(3) 0.0530(11) Uani 1 1 d . . . . .
H2 H 0.0578 0.0513 0.0975 0.064 Uiso 1 1 calc R U . . .
C3 C 0.0621(3) 0.1640(2) 0.1270(3) 0.0561(12) Uani 1 1 d . . . . .
H3 H 0.0557 0.1799 0.0538 0.067 Uiso 1 1 calc R U . . .
C4 C 0.0701(3) 0.2165(2) 0.2107(3) 0.0502(11) Uani 1 1 d . . . . .
H4 H 0.0691 0.2688 0.1955 0.060 Uiso 1 1 calc R U . . .
C5 C 0.0794(2) 0.1908(2) 0.3169(3) 0.0342(9) Uani 1 1 d . . . . .
C6 C 0.24036(18) 0.0872(2) 0.5871(3) 0.0324(8) Uani 1 1 d . . . . .
C7 C 0.3237(2) 0.0847(2) 0.5998(3) 0.0352(9) Uani 1 1 d . . . . .
C8 C 0.3640(2) 0.0219(2) 0.5649(3) 0.0474(11) Uani 1 1 d . . . . .
H8 H 0.3384 -0.0193 0.5330 0.057 Uiso 1 1 calc R U . . .
C9 C 0.4415(3) 0.0197(3) 0.5766(4) 0.0597(13) Uani 1 1 d . . . . .
H9 H 0.4685 -0.0235 0.5539 0.072 Uiso 1 1 calc R U . . .
C10 C 0.4795(2) 0.0799(3) 0.6212(4) 0.0611(14) Uani 1 1 d . . . . .
H10 H 0.5327 0.0788 0.6263 0.073 Uiso 1 1 calc R U . . .
C11 C 0.4402(3) 0.1416(3) 0.6586(4) 0.0586(13) Uani 1 1 d . . . . .
H11 H 0.4660 0.1823 0.6917 0.070 Uiso 1 1 calc R U . . .
C12 C 0.3621(2) 0.1439(2) 0.6475(4) 0.0479(11) Uani 1 1 d . . . . .
H12 H 0.3351 0.1864 0.6728 0.058 Uiso 1 1 calc R U . . .
C13 C 0.24665(19) 0.1043(2) 0.3936(3) 0.0311(8) Uani 1 1 d . . . . .
C14 C 0.2780(2) 0.1733(2) 0.3691(3) 0.0397(9) Uani 1 1 d . . . . .
H14 H 0.2768 0.2129 0.4209 0.048 Uiso 1 1 calc R U . . .
C15 C 0.3114(2) 0.1842(2) 0.2679(3) 0.0487(11) Uani 1 1 d . . . . .
H15 H 0.3326 0.2319 0.2517 0.058 Uiso 1 1 calc R U . . .
C16 C 0.3148(2) 0.1280(3) 0.1902(3) 0.0504(11) Uani 1 1 d . . . . .
C17 C 0.2839(2) 0.0594(3) 0.2166(3) 0.0563(13) Uani 1 1 d . . . . .
H17 H 0.2857 0.0198 0.1649 0.068 Uiso 1 1 calc R U . . .
C18 C 0.2498(2) 0.0464(2) 0.3178(3) 0.0471(11) Uani 1 1 d . . . . .
H18 H 0.2292 -0.0014 0.3344 0.057 Uiso 1 1 calc R U . . .
C19 C 0.3507(3) 0.1416(3) 0.0787(4) 0.0847(18) Uani 1 1 d . . . . .
H19A H 0.3433 0.1941 0.0573 0.127 Uiso 1 1 calc R U . . .
H19B H 0.3273 0.1086 0.0247 0.127 Uiso 1 1 calc R U . . .
H19C H 0.4046 0.1308 0.0827 0.127 Uiso 1 1 calc R U . . .
C20 C -0.0795(2) 0.09892(19) 0.5416(3) 0.0363(8) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
N1 Fe1 N1 174.04(17) . 6_556 ?
N1 Fe1 N3 93.65(11) . 6_556 ?
N1 Fe1 N3 90.53(12) 6_556 6_556 ?
N1 Fe1 N3 90.53(12) . . ?
N1 Fe1 N3 93.65(11) 6_556 . ?
N2 Fe1 N1 80.85(12) 6_556 . ?
N2 Fe1 N1 94.93(12) 6_556 6_556 ?
N2 Fe1 N1 80.85(12) . 6_556 ?
N2 Fe1 N1 94.93(12) . . ?
N2 Fe1 N2 90.81(16) 6_556 . ?
N2 Fe1 N3 174.49(12) 6_556 6_556 ?
N2 Fe1 N3 174.49(12) . . ?
N2 Fe1 N3 89.31(12) . 6_556 ?
N2 Fe1 N3 89.31(12) 6_556 . ?
N3 Fe1 N3 91.11(19) . 6_556 ?
C1 N1 Fe1 127.8(2) . . ?
C1 N1 C5 117.3(3) . . ?
C5 N1 Fe1 115.0(2) . . ?
C6 N2 Fe1 116.8(2) . . ?
C6 N2 C13 120.3(3) . . ?
C13 N2 Fe1 122.8(2) . . ?
C20 N3 Fe1 173.9(3) . . ?
N1 C1 H1 118.6 . . ?
N1 C1 C2 122.7(3) . . ?
C2 C1 H1 118.6 . . ?
C1 C2 H2 120.2 . . ?
C3 C2 C1 119.5(4) . . ?
C3 C2 H2 120.2 . . ?
C2 C3 H3 120.6 . . ?
C2 C3 C4 118.7(4) . . ?
C4 C3 H3 120.6 . . ?
C3 C4 H4 120.6 . . ?
C5 C4 C3 118.8(4) . . ?
C5 C4 H4 120.6 . . ?
N1 C5 C4 123.0(3) . . ?
N1 C5 C6 112.8(3) . 6_556 ?
C4 C5 C6 124.2(3) . 6_556 ?
N2 C6 C5 114.5(3) . 6_556 ?
N2 C6 C7 125.0(3) . . ?
C5 C6 C7 120.4(3) 6_556 . ?
C8 C7 C6 120.2(4) . . ?
C12 C7 C6 120.8(3) . . ?
C12 C7 C8 119.0(4) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 C7 120.2(4) . . ?
C9 C8 H8 119.9 . . ?
C8 C9 H9 119.8 . . ?
C10 C9 C8 120.4(5) . . ?
C10 C9 H9 119.8 . . ?
C9 C10 H10 120.0 . . ?
C9 C10 C11 120.0(4) . . ?
C11 C10 H10 120.0 . . ?
C10 C11 H11 120.2 . . ?
C10 C11 C12 119.6(5) . . ?
C12 C11 H11 120.2 . . ?
C7 C12 C11 120.7(4) . . ?
C7 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C14 C13 N2 120.4(3) . . ?
C14 C13 C18 119.7(3) . . ?
C18 C13 N2 119.6(3) . . ?
C13 C14 H14 120.3 . . ?
C13 C14 C15 119.4(4) . . ?
C15 C14 H14 120.3 . . ?
C14 C15 H15 118.9 . . ?
C16 C15 C14 122.2(4) . . ?
C16 C15 H15 118.9 . . ?
C15 C16 C19 121.4(4) . . ?
C17 C16 C15 117.5(4) . . ?
C17 C16 C19 121.1(4) . . ?
C16 C17 H17 119.1 . . ?
C16 C17 C18 121.8(4) . . ?
C18 C17 H17 119.1 . . ?
C13 C18 C17 119.3(4) . . ?
C13 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N3 C20 S1 178.4(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
Fe1 N1 1.958(2) 6_556 ?
Fe1 N1 1.958(2) . ?
Fe1 N2 1.948(3) . ?
Fe1 N2 1.948(3) 6_556 ?
Fe1 N3 1.958(3) . ?
Fe1 N3 1.958(3) 6_556 ?
S1 C20 1.627(4) . ?
N1 C1 1.338(4) . ?
N1 C5 1.359(4) . ?
N2 C6 1.298(4) . ?
N2 C13 1.442(4) . ?
N3 C20 1.154(4) . ?
C1 H1 0.9400 . ?
C1 C2 1.385(5) . ?
C2 H2 0.9400 . ?
C2 C3 1.376(5) . ?
C3 H3 0.9400 . ?
C3 C4 1.385(5) . ?
C4 H4 0.9400 . ?
C4 C5 1.380(5) . ?
C5 C6 1.466(5) 6_556 ?
C6 C5 1.466(5) 6_556 ?
C6 C7 1.479(5) . ?
C7 C8 1.381(5) . ?
C7 C12 1.373(5) . ?
C8 H8 0.9400 . ?
C8 C9 1.373(6) . ?
C9 H9 0.9400 . ?
C9 C10 1.368(6) . ?
C10 H10 0.9400 . ?
C10 C11 1.369(6) . ?
C11 H11 0.9400 . ?
C11 C12 1.383(6) . ?
C12 H12 0.9400 . ?
C13 C14 1.370(5) . ?
C13 C18 1.376(5) . ?
C14 H14 0.9400 . ?
C14 C15 1.378(5) . ?
C15 H15 0.9400 . ?
C15 C16 1.371(5) . ?
C16 C17 1.366(6) . ?
C16 C19 1.518(6) . ?
C17 H17 0.9400 . ?
C17 C18 1.389(5) . ?
C18 H18 0.9400 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 H19C 0.9700 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N1 C1 C2 179.0(3) . . . . ?
Fe1 N1 C5 C4 -179.6(3) . . . . ?
Fe1 N1 C5 C6 -0.7(4) . . . 6_556 ?
Fe1 N2 C6 C5 1.4(4) . . . 6_556 ?
Fe1 N2 C6 C7 179.3(3) . . . . ?
Fe1 N2 C13 C14 100.5(3) . . . . ?
Fe1 N2 C13 C18 -74.3(4) . . . . ?
N1 C1 C2 C3 1.5(6) . . . . ?
N2 C6 C7 C8 -70.3(5) . . . . ?
N2 C6 C7 C12 110.4(4) . . . . ?
N2 C13 C14 C15 -173.8(3) . . . . ?
N2 C13 C18 C17 173.8(4) . . . . ?
C1 N1 C5 C4 0.8(5) . . . . ?
C1 N1 C5 C6 179.7(3) . . . 6_556 ?
C1 C2 C3 C4 -0.7(7) . . . . ?
C2 C3 C4 C5 0.1(7) . . . . ?
C3 C4 C5 N1 -0.1(7) . . . . ?
C3 C4 C5 C6 -178.9(4) . . . 6_556 ?
C5 N1 C1 C2 -1.5(5) . . . . ?
C5 C6 C7 C8 107.4(4) 6_556 . . . ?
C5 C6 C7 C12 -71.9(5) 6_556 . . . ?
C6 N2 C13 C14 -75.8(4) . . . . ?
C6 N2 C13 C18 109.4(4) . . . . ?
C6 C7 C8 C9 179.9(4) . . . . ?
C6 C7 C12 C11 -179.5(4) . . . . ?
C7 C8 C9 C10 -1.1(7) . . . . ?
C8 C7 C12 C11 1.2(6) . . . . ?
C8 C9 C10 C11 2.6(7) . . . . ?
C9 C10 C11 C12 -2.3(7) . . . . ?
C10 C11 C12 C7 0.3(7) . . . . ?
C12 C7 C8 C9 -0.8(6) . . . . ?
C13 N2 C6 C5 177.9(3) . . . 6_556 ?
C13 N2 C6 C7 -4.2(5) . . . . ?
C13 C14 C15 C16 -0.3(6) . . . . ?
C14 C13 C18 C17 -1.0(6) . . . . ?
C14 C15 C16 C17 -0.4(6) . . . . ?
C14 C15 C16 C19 179.1(4) . . . . ?
C15 C16 C17 C18 0.4(7) . . . . ?
C16 C17 C18 C13 0.3(7) . . . . ?
C18 C13 C14 C15 1.0(6) . . . . ?
C19 C16 C17 C18 -179.1(5) . . . . ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.149 0.851 0.750 72.0 9.2 ?
2 0.231 0.231 0.000 27.7 0.0 ?
3 0.269 0.731 0.250 27.7 0.0 ?
4 0.351 0.351 0.500 72.0 8.9 ?
5 0.649 0.649 0.000 72.0 9.0 ?
6 0.731 0.269 0.750 27.7 0.0 ?
7 0.769 0.769 0.500 27.7 0.0 ?
8 0.851 0.149 0.250 72.0 9.0 ?
