#------------------------------------------------------------------------------
#$Date: 2019-11-23 05:14:42 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232206 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/71/4347181.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_4347181
loop_
_publ_author_name
'Hogue, Ross W.'
'Feltham, Humphrey L. C.'
'Miller, Reece G.'
'Brooker, Sally'
_publ_section_title
;
 Spin Crossover in Dinuclear N4S2 Iron(II) Thioether-Triazole Complexes:
 Access to [HS-HS], [HS-LS], and [LS-LS] States.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4152
_journal_page_last               4165
_journal_paper_doi               10.1021/acs.inorgchem.5b02851
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C46 H46 Fe2 N10 S4'
_chemical_formula_weight         978.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 110.472(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0419(6)
_cell_length_b                   27.6191(11)
_cell_length_c                   14.6634(6)
_cell_measurement_reflns_used    7894
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.9490
_cell_measurement_theta_min      3.2210
_cell_volume                     6086.5(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.870
_diffrn_measurement_device_type  'Oxford Diffraction Supernova'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.870
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20288
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.870
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.593
_diffrn_reflns_theta_min         3.215
_exptl_absorpt_coefficient_mu    0.648
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 abspack'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.068
_exptl_crystal_description       Block
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_platon_squeeze_details
;
;
_refine_diff_density_max         1.364
_refine_diff_density_min         -1.528
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         7460
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0765
_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)+(0.0765P)²+47.2124P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1898
_refine_ls_wR_factor_ref         0.2004
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5627
_reflns_number_total             7460
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b02851_si_001.cif
_cod_data_source_block           RWH332_2_SQUEEZE
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4347181
_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_min   0.782
_shelx_estimated_absorpt_t_max   0.881
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y, -z-1/2'
'-x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -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
Fe1 Fe 0.43000(3) 0.67063(2) 0.59968(4) 0.01753(15) Uani 1 1 d . . .
C1 C 0.2701(4) 0.66845(18) 0.6628(4) 0.0404(11) Uani 1 1 d . . .
H1 H 0.3016 0.6946 0.7020 0.049 Uiso 1 1 calc R U .
C2 C 0.1939(4) 0.6526(2) 0.6757(5) 0.0598(19) Uani 1 1 d . . .
H2 H 0.1732 0.6674 0.7222 0.072 Uiso 1 1 calc R U .
C3 C 0.1471(3) 0.6136(2) 0.6179(5) 0.0507(15) Uani 1 1 d . . .
H3 H 0.0948 0.6010 0.6253 0.061 Uiso 1 1 calc R U .
C4 C 0.1790(3) 0.5951(2) 0.5527(4) 0.0470(14) Uani 1 1 d . . .
H4 H 0.1481 0.5691 0.5126 0.056 Uiso 1 1 calc R U .
C5 C 0.2562(3) 0.61278(17) 0.5414(3) 0.0319(9) Uani 1 1 d . . .
C6 C 0.2865(3) 0.59458(18) 0.4621(3) 0.0360(10) Uani 1 1 d . . .
H6A H 0.2527 0.6118 0.4011 0.043 Uiso 1 1 calc R U .
H6B H 0.2713 0.5598 0.4517 0.043 Uiso 1 1 calc R U .
C7 C 0.4530(3) 0.55325(15) 0.5687(3) 0.0307(9) Uani 1 1 d . . .
H7A H 0.4104 0.5260 0.5567 0.037 Uiso 1 1 calc R U .
H7B H 0.5070 0.5413 0.5579 0.037 Uiso 1 1 calc R U .
C8 C 0.4774(2) 0.56944(13) 0.6720(3) 0.0218(7) Uani 1 1 d . . .
C9 C 0.5000 0.48833(19) 0.7500 0.0285(12) Uani 1 2 d S T P
C10 C 0.4200(3) 0.46287(15) 0.7267(4) 0.0363(10) Uani 1 1 d . . .
H10 H 0.3653 0.4799 0.7111 0.044 Uiso 1 1 calc R U .
C11 C 0.4207(3) 0.41368(16) 0.7266(4) 0.0371(10) Uani 1 1 d . . .
H11 H 0.3662 0.3965 0.7102 0.045 Uiso 1 1 calc R U .
C12 C 0.5000 0.3883(2) 0.7500 0.0322(13) Uani 1 2 d S T P
C13 C 0.5000 0.3327(3) 0.7500 0.086(4) Uani 1 2 d S T P
H13A H 0.4387 0.3209 0.7319 0.103 Uiso 0.5 1 calc R U P
H13B H 0.5261 0.3209 0.7030 0.103 Uiso 0.5 1 calc R U P
H13C H 0.5351 0.3209 0.8151 0.103 Uiso 0.5 1 calc R U P
C14 C 0.6114(3) 0.66093(17) 0.5901(4) 0.0368(10) Uani 1 1 d . . .
H14 H 0.6149 0.6367 0.6373 0.044 Uiso 1 1 calc R U .
C15 C 0.6834(3) 0.6673(2) 0.5605(4) 0.0477(13) Uani 1 1 d . . .
H15 H 0.7341 0.6469 0.5840 0.057 Uiso 1 1 calc R U .
C16 C 0.6800(4) 0.7043(3) 0.4955(4) 0.0593(17) Uani 1 1 d . . .
H16 H 0.7288 0.7102 0.4746 0.071 Uiso 1 1 calc R U .
C17 C 0.6057(3) 0.7319(3) 0.4624(4) 0.0595(18) Uani 1 1 d . . .
H17 H 0.6030 0.7580 0.4191 0.071 Uiso 1 1 calc R U .
C18 C 0.5343(3) 0.7227(2) 0.4909(3) 0.0384(11) Uani 1 1 d . . .
C19 C 0.4491(3) 0.7516(3) 0.4435(4) 0.0599(18) Uani 1 1 d . . .
H19A H 0.4254 0.7436 0.3733 0.072 Uiso 1 1 calc R U .
H19B H 0.4645 0.7864 0.4492 0.072 Uiso 1 1 calc R U .
C20 C 0.3870(3) 0.78852(18) 0.5838(4) 0.0449(13) Uani 1 1 d . . .
H20A H 0.4116 0.8169 0.5607 0.054 Uiso 1 1 calc R U .
H20B H 0.3315 0.7988 0.5934 0.054 Uiso 1 1 calc R U .
C21 C 0.4513(3) 0.77200(14) 0.6772(3) 0.0286(9) Uani 1 1 d . . .
C22 C 0.5000 0.8550(2) 0.7500 0.0394(16) Uani 1 2 d S T P
C23 C 0.5727(3) 0.87821(18) 0.7448(5) 0.0569(17) Uani 1 1 d . . .
H23 H 0.6219 0.8610 0.7390 0.068 Uiso 1 1 calc R U .
C24 C 0.5714(3) 0.92927(17) 0.7483(5) 0.0568(17) Uani 1 1 d . . .
H24 H 0.6230 0.9466 0.7496 0.068 Uiso 1 1 calc R U .
C25 C 0.5000 0.9546(3) 0.7500 0.055(2) Uani 1 2 d S T P
C26 C 0.5000 1.0093(3) 0.7500 0.065(3) Uani 1 2 d S T P
H26A H 0.5572 1.0211 0.7486 0.078 Uiso 0.5 1 calc R U P
H26B H 0.4518 1.0211 0.6924 0.078 Uiso 0.5 1 calc R U P
H26C H 0.4910 1.0211 0.8089 0.078 Uiso 0.5 1 calc R U P
N1 N 0.3028(2) 0.64933(13) 0.5982(3) 0.0286(7) Uani 1 1 d . . .
N2 N 0.48513(19) 0.61510(11) 0.6992(2) 0.0176(6) Uani 1 1 d . . .
N3 N 0.5000 0.53982(16) 0.7500 0.0241(10) Uani 1 2 d S T P
N4 N 0.5372(2) 0.68727(13) 0.5555(2) 0.0265(7) Uani 1 1 d . . .
N5 N 0.46893(19) 0.72647(12) 0.7023(2) 0.0226(7) Uani 1 1 d . . .
N6 N 0.5000 0.80211(18) 0.7500 0.0337(12) Uani 1 2 d S T P
S1 S 0.40369(7) 0.60141(4) 0.48315(7) 0.0315(3) Uani 1 1 d . . .
S2 S 0.36152(7) 0.74195(6) 0.49307(8) 0.0422(3) 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'
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'
Fe Fe 0.3463 0.8444 '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
N2 Fe1 N4 100.66(13) . .
N2 Fe1 N5 95.26(12) . .
N4 Fe1 N5 89.43(13) . .
N2 Fe1 N1 88.51(12) . .
N4 Fe1 N1 162.35(14) . .
N5 Fe1 N1 104.83(14) . .
N2 Fe1 S1 81.09(9) . .
N4 Fe1 S1 85.23(9) . .
N5 Fe1 S1 172.84(9) . .
N1 Fe1 S1 81.31(11) . .
N2 Fe1 S2 174.48(9) . .
N4 Fe1 S2 82.12(11) . .
N5 Fe1 S2 79.95(9) . .
N1 Fe1 S2 90.08(9) . .
S1 Fe1 S2 103.97(4) . .
N1 C1 C2 124.0(6) . .
C1 C2 C3 118.2(5) . .
C4 C3 C2 117.7(5) . .
C3 C4 C5 122.1(6) . .
N1 C5 C4 120.6(5) . .
N1 C5 C6 118.0(4) . .
C4 C5 C6 121.3(5) . .
C5 C6 S1 115.7(3) . .
C8 C7 S1 112.3(3) . .
N2 C8 N3 110.8(3) . .
N2 C8 C7 123.9(4) . .
N3 C8 C7 125.1(3) . .
C10 C9 C10 119.5(5) 6_657 .
C10 C9 N3 120.2(3) 6_657 .
C10 C9 N3 120.2(3) . .
C11 C10 C9 119.8(4) . .
C10 C11 C12 120.9(4) . .
C11 C12 C11 119.2(5) 6_657 .
C11 C12 C13 120.4(3) 6_657 .
C11 C12 C13 120.4(3) . .
N4 C14 C15 123.0(5) . .
C14 C15 C16 118.3(5) . .
C17 C16 C15 118.8(5) . .
C16 C17 C18 120.6(6) . .
N4 C18 C17 121.4(5) . .
N4 C18 C19 120.3(4) . .
C17 C18 C19 118.2(5) . .
C18 C19 S2 115.9(3) . .
C21 C20 S2 111.9(3) . .
N5 C21 N6 110.9(4) . .
N5 C21 C20 124.8(4) . .
N6 C21 C20 124.3(4) . .
C23 C22 C23 123.5(6) 6_657 .
C23 C22 N6 118.2(3) 6_657 .
C23 C22 N6 118.2(3) . .
C22 C23 C24 116.5(5) . .
C25 C24 C23 122.8(5) . .
C24 C25 C24 117.6(7) 6_657 .
C24 C25 C26 121.2(3) 6_657 .
C24 C25 C26 121.2(3) . .
C1 N1 C5 117.4(4) . .
C1 N1 Fe1 119.8(3) . .
C5 N1 Fe1 122.4(3) . .
C8 N2 N2 106.5(2) . 6_657
C8 N2 Fe1 121.3(3) . .
N2 N2 Fe1 130.45(11) 6_657 .
C8 N3 C8 105.3(4) . 6_657
C8 N3 C9 127.3(2) . .
C8 N3 C9 127.3(2) 6_657 .
C14 N4 C18 117.9(4) . .
C14 N4 Fe1 118.9(3) . .
C18 N4 Fe1 123.2(3) . .
C21 N5 N5 106.7(2) . 6_657
C21 N5 Fe1 121.5(3) . .
N5 N5 Fe1 130.18(11) 6_657 .
C21 N6 C21 104.8(5) . 6_657
C21 N6 C22 127.6(2) . .
C21 N6 C22 127.6(2) 6_657 .
C6 S1 C7 102.6(2) . .
C6 S1 Fe1 96.54(17) . .
C7 S1 Fe1 99.20(14) . .
C20 S2 C19 100.6(3) . .
C20 S2 Fe1 99.45(15) . .
C19 S2 Fe1 97.6(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N2 2.088(3) .
Fe1 N4 2.089(3) .
Fe1 N5 2.092(3) .
Fe1 N1 2.117(4) .
Fe1 S1 2.4996(12) .
Fe1 S2 2.5159(14) .
C1 N1 1.340(6) .
C1 C2 1.373(8) .
C2 C3 1.413(10) .
C3 C4 1.335(9) .
C4 C5 1.393(6) .
C5 N1 1.355(6) .
C5 C6 1.497(7) .
C6 S1 1.804(4) .
C7 C8 1.494(6) .
C7 S1 1.810(5) .
C8 N2 1.315(5) .
C8 N3 1.349(5) .
C9 C10 1.396(5) 6_657
C9 C10 1.396(5) .
C9 N3 1.422(7) .
C10 C11 1.359(6) .
C11 C12 1.386(5) .
C12 C11 1.386(6) 6_657
C12 C13 1.535(9) .
C14 N4 1.336(6) .
C14 C15 1.380(7) .
C15 C16 1.384(9) .
C16 C17 1.354(9) .
C17 C18 1.374(7) .
C18 N4 1.351(6) .
C18 C19 1.525(7) .
C19 S2 1.813(5) .
C20 C21 1.470(6) .
C20 S2 1.792(6) .
C21 N5 1.313(5) .
C21 N6 1.363(5) .
C22 C23 1.357(6) 6_657
C22 C23 1.357(6) .
C22 N6 1.460(8) .
C23 C24 1.411(7) .
C24 C25 1.349(7) .
C25 C24 1.349(7) 6_657
C25 C26 1.511(10) .
N2 N2 1.396(6) 6_657
N3 C8 1.349(5) 6_657
N5 N5 1.404(6) 6_657
N6 C21 1.363(5) 6_657
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_4
N1 C1 C2 C3 0.3(7) . .
C1 C2 C3 C4 -1.3(7) . .
C2 C3 C4 C5 0.7(7) . .
C3 C4 C5 N1 1.1(7) . .
C3 C4 C5 C6 -174.6(4) . .
N1 C5 C6 S1 27.7(5) . .
C4 C5 C6 S1 -156.5(4) . .
S1 C7 C8 N2 -17.2(5) . .
S1 C7 C8 N3 167.3(3) . .
C10 C9 C10 C11 -0.3(4) 6_657 .
N3 C9 C10 C11 179.7(4) . .
C9 C10 C11 C12 0.5(7) . .
C10 C11 C12 C11 -0.3(4) . 6_657
C10 C11 C12 C13 179.7(4) . .
N4 C14 C15 C16 3.3(8) . .
C14 C15 C16 C17 -1.3(9) . .
C15 C16 C17 C18 -1.5(9) . .
C16 C17 C18 N4 2.7(9) . .
C16 C17 C18 C19 -173.9(6) . .
N4 C18 C19 S2 9.3(7) . .
C17 C18 C19 S2 -174.0(5) . .
S2 C20 C21 N5 -19.0(6) . .
S2 C20 C21 N6 162.0(3) . .
C23 C22 C23 C24 2.1(5) 6_657 .
N6 C22 C23 C24 -177.9(5) . .
C22 C23 C24 C25 -4.5(10) . .
C23 C24 C25 C24 2.3(5) . 6_657
C23 C24 C25 C26 -177.7(5) . .
C2 C1 N1 C5 1.4(6) . .
C2 C1 N1 Fe1 -171.4(4) . .
C4 C5 N1 C1 -2.0(6) . .
C6 C5 N1 C1 173.7(4) . .
C4 C5 N1 Fe1 170.5(3) . .
C6 C5 N1 Fe1 -13.7(5) . .
N3 C8 N2 N2 0.3(4) . 6_657
C7 C8 N2 N2 -175.7(4) . 6_657
N3 C8 N2 Fe1 -166.35(18) . .
C7 C8 N2 Fe1 17.6(5) . .
N2 C8 N3 C8 -0.12(18) . 6_657
C7 C8 N3 C8 175.9(4) . 6_657
N2 C8 N3 C9 179.88(18) . .
C7 C8 N3 C9 -4.1(4) . .
C10 C9 N3 C8 103.3(3) 6_657 .
C10 C9 N3 C8 -76.7(3) . .
C10 C9 N3 C8 -76.7(3) 6_657 6_657
C10 C9 N3 C8 103.3(3) . 6_657
C15 C14 N4 C18 -2.2(7) . .
C15 C14 N4 Fe1 175.9(4) . .
C17 C18 N4 C14 -0.9(7) . .
C19 C18 N4 C14 175.7(5) . .
C17 C18 N4 Fe1 -178.8(4) . .
C19 C18 N4 Fe1 -2.2(6) . .
N6 C21 N5 N5 1.3(5) . 6_657
C20 C21 N5 N5 -177.8(5) . 6_657
N6 C21 N5 Fe1 -165.8(2) . .
C20 C21 N5 Fe1 15.1(6) . .
N5 C21 N6 C21 -0.5(2) . 6_657
C20 C21 N6 C21 178.6(5) . 6_657
N5 C21 N6 C22 179.5(2) . .
C20 C21 N6 C22 -1.4(5) . .
C23 C22 N6 C21 71.3(4) 6_657 .
C23 C22 N6 C21 -108.7(4) . .
C23 C22 N6 C21 -108.7(4) 6_657 6_657
C23 C22 N6 C21 71.3(4) . 6_657
C5 C6 S1 C7 76.5(4) . .
C5 C6 S1 Fe1 -24.4(3) . .
C8 C7 S1 C6 -90.7(3) . .
C8 C7 S1 Fe1 8.2(3) . .
C21 C20 S2 C19 -87.5(4) . .
C21 C20 S2 Fe1 12.2(4) . .
C18 C19 S2 C20 91.4(5) . .
C18 C19 S2 Fe1 -9.7(5) . .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 0.000 1052 408 ' '
2 1.000 0.500 0.129 1051 408 ' '
