#------------------------------------------------------------------------------
#$Date: 2022-10-27 01:14:21 +0300 (Thu, 27 Oct 2022) $
#$Revision: 278817 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/09/7130903.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_7130903
loop_
_publ_author_name
'Hsieh, Chang-Chih'
'Li, Cheng-Yao'
'Chiang, Ming-Hsi'
'Horng, Yih-Chern'
_publ_section_title
;
 Catalytic O2 Activation toward Oxidative N-S Bond Formation by a Thiolato
 Fe(III) Complex
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC05375F
_journal_year                    2022
_chemical_formula_sum            'C27 H26 N4 O3 S2'
_chemical_formula_weight         518.64
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-07-28 deposited with the CCDC.	2022-10-26 downloaded from the CCDC.
;
_cell_angle_alpha                101.184(13)
_cell_angle_beta                 95.225(12)
_cell_angle_gamma                101.995(12)
_cell_formula_units_Z            2
_cell_length_a                   8.9627(17)
_cell_length_b                   9.6003(15)
_cell_length_c                   15.312(3)
_cell_measurement_reflns_used    940
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18.18
_cell_measurement_theta_min      2.35
_cell_volume                     1252.4(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_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       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1084
_diffrn_reflns_av_unetI/netI     0.1453
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13798
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.222
_exptl_absorpt_coefficient_mu    0.250
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.970
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       needle
_exptl_crystal_F_000             434
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4890
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.1499
_refine_ls_R_factor_gt           0.0703
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1000P)²+0.0400P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1596
_refine_ls_wR_factor_ref         0.2096
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2514
_reflns_number_total             4890
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2cc05375f2.cif
_cod_data_source_block           compound2n
_cod_database_code               7130903
_shelx_shelxl_version_number     2018/3
_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, -y, -z'
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
S2 S 0.93136(15) 0.68263(13) 0.94176(8) 0.0351(3) Uani 1 1 d . . . . .
S1 S 0.98567(14) 0.68975(14) 1.07448(8) 0.0361(4) Uani 1 1 d . . . . .
C20 C 0.9099(6) 0.8380(5) 0.7888(3) 0.0311(11) Uani 1 1 d . . . . .
C7 C 0.9809(5) 0.6420(5) 1.2603(3) 0.0308(11) Uani 1 1 d . . . . .
C14 C 0.8331(5) 0.8920(5) 0.8669(3) 0.0284(10) Uani 1 1 d . . . . .
C1 C 0.8323(5) 0.5649(4) 1.1041(3) 0.0282(10) Uani 1 1 d . . . . .
C15 C 0.8388(5) 0.8306(5) 0.9420(3) 0.0290(11) Uani 1 1 d . . . . .
C16 C 0.7024(5) 1.0025(5) 1.0142(4) 0.0373(12) Uani 1 1 d . . . . .
H16 H 0.660295 1.042408 1.065477 0.045 Uiso 1 1 calc R U . . .
C17 C 0.7577(6) 1.0043(5) 0.8653(3) 0.0367(12) Uani 1 1 d . . . . .
H17 H 0.752231 1.044313 0.813354 0.044 Uiso 1 1 calc R U . . .
C21 C 1.0644(5) 0.8910(5) 0.6719(3) 0.0350(11) Uani 1 1 d . . . . .
H21A H 1.120691 0.816723 0.683810 0.042 Uiso 1 1 calc R U . . .
H21B H 1.140719 0.976604 0.663744 0.042 Uiso 1 1 calc R U . . .
C2 C 0.7061(5) 0.4805(5) 1.0440(3) 0.0358(12) Uani 1 1 d . . . . .
H2 H 0.694381 0.491921 0.983650 0.043 Uiso 1 1 calc R U . . .
C18 C 0.7745(5) 0.8893(5) 1.0165(3) 0.0336(11) Uani 1 1 d . . . . .
H18 H 0.780565 0.851002 1.069151 0.040 Uiso 1 1 calc R U . . .
C10 C 1.4072(6) 0.8693(6) 1.3508(4) 0.0429(13) Uani 1 1 d . . . . .
H10 H 1.377173 0.923178 1.402381 0.051 Uiso 1 1 calc R U . . .
C23 C 0.9311(6) 0.6870(5) 0.5410(3) 0.0394(12) Uani 1 1 d . . . . .
H23 H 0.987444 0.625122 0.563803 0.047 Uiso 1 1 calc R U . . .
C22 C 0.9532(5) 0.8294(5) 0.5868(3) 0.0306(11) Uani 1 1 d . . . . .
C3 C 0.8492(5) 0.5466(5) 1.1933(3) 0.0300(11) Uani 1 1 d . . . . .
C24 C 0.8690(6) 0.9157(5) 0.5508(4) 0.0408(13) Uani 1 1 d . . . . .
H24 H 0.882095 1.014492 0.581151 0.049 Uiso 1 1 calc R U . . .
C19 C 0.6910(6) 1.0582(5) 0.9379(4) 0.0408(13) Uani 1 1 d . . . . .
H19 H 0.637346 1.133243 0.935620 0.049 Uiso 1 1 calc R U . . .
C9 C 1.3308(5) 0.7230(5) 1.3208(3) 0.0339(11) Uani 1 1 d . . . . .
C11 C 1.3772(6) 0.6469(6) 1.2456(3) 0.0456(14) Uani 1 1 d . . . . .
H11 H 1.328270 0.547199 1.221582 0.055 Uiso 1 1 calc R U . . .
C25 C 0.7695(5) 0.8648(5) 0.4745(3) 0.0356(12) Uani 1 1 d . . . . .
H25 H 0.713345 0.926137 0.450950 0.043 Uiso 1 1 calc R U . . .
C4 C 0.7408(6) 0.4404(5) 1.2183(4) 0.0385(12) Uani 1 1 d . . . . .
H4 H 0.753524 0.424446 1.277580 0.046 Uiso 1 1 calc R U . . .
C8 C 1.2043(6) 0.6548(5) 1.3670(3) 0.0377(12) Uani 1 1 d . . . . .
H8A H 1.241719 0.587738 1.400691 0.045 Uiso 1 1 calc R U . . .
H8B H 1.176124 0.732076 1.410886 0.045 Uiso 1 1 calc R U . . .
C5 C 0.6145(6) 0.3577(5) 1.1577(4) 0.0429(13) Uani 1 1 d . . . . .
H5 H 0.540344 0.286262 1.175517 0.052 Uiso 1 1 calc R U . . .
C26 C 0.7519(6) 0.7270(6) 0.4332(4) 0.0507(15) Uani 1 1 d . . . . .
H26 H 0.681117 0.691612 0.379477 0.061 Uiso 1 1 calc R U . . .
C6 C 0.5972(6) 0.3795(5) 1.0719(4) 0.0414(13) Uani 1 1 d . . . . .
H6 H 0.509260 0.324471 1.030890 0.050 Uiso 1 1 calc R U . . .
C13 C 1.5601(6) 0.8606(6) 1.2404(4) 0.0476(14) Uani 1 1 d . . . . .
H13 H 1.639261 0.907739 1.211632 0.057 Uiso 1 1 calc R U . . .
C12 C 1.4945(6) 0.7160(6) 1.2056(4) 0.0509(15) Uani 1 1 d . . . . .
H12 H 1.528979 0.664194 1.154984 0.061 Uiso 1 1 calc R U . . .
O1 O 1.0055(4) 0.7770(3) 1.2746(2) 0.0377(8) Uani 1 1 d . . . . .
O2 O 0.9012(4) 0.7044(3) 0.7645(2) 0.0425(9) Uani 1 1 d . . . . .
N1 N 1.0671(5) 0.5736(4) 1.3038(3) 0.0342(10) Uani 1 1 d . . . . .
N3 N 0.9874(5) 0.9353(4) 0.7495(3) 0.0306(9) Uani 1 1 d . . . . .
N2 N 1.5192(5) 0.9398(5) 1.3127(3) 0.0458(11) Uani 1 1 d . . . . .
N4 N 0.8286(6) 0.6314(5) 0.4624(3) 0.0615(14) Uani 1 1 d . . . . .
O3 O 0.6283(6) 0.2521(5) 0.3763(4) 0.0961(17) Uani 1 1 d . . . . .
H3 H 0.630330 0.188875 0.407052 0.144 Uiso 1 1 calc R U . . .
C27 C 0.4993(9) 0.3072(7) 0.3877(6) 0.101(3) Uani 1 1 d . . . . .
H27A H 0.461641 0.288279 0.443388 0.152 Uiso 1 1 calc R U . . .
H27B H 0.418852 0.259870 0.336674 0.152 Uiso 1 1 calc R U . . .
H27C H 0.525648 0.412654 0.391239 0.152 Uiso 1 1 calc R U . . .
H7 H 0.987(6) 1.031(5) 0.767(3) 0.045(15) Uiso 1 1 d . . . . .
H1 H 1.051(6) 0.482(6) 1.289(4) 0.060(18) Uiso 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
H H 0.0000 0.0000 '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
C15 S2 S1 103.33(16) . . ?
C1 S1 S2 106.27(17) . . ?
O2 C20 N3 122.7(4) . . ?
O2 C20 C14 119.3(4) . . ?
N3 C20 C14 118.0(4) . . ?
O1 C7 N1 122.4(5) . . ?
O1 C7 C3 121.4(4) . . ?
N1 C7 C3 116.2(4) . . ?
C17 C14 C15 120.0(4) . . ?
C17 C14 C20 120.3(4) . . ?
C15 C14 C20 119.8(4) . . ?
C2 C1 C3 119.6(4) . . ?
C2 C1 S1 124.0(4) . . ?
C3 C1 S1 116.2(3) . . ?
C14 C15 C18 118.6(4) . . ?
C14 C15 S2 119.4(3) . . ?
C18 C15 S2 122.0(4) . . ?
C18 C16 C19 120.4(5) . . ?
C19 C17 C14 120.8(5) . . ?
N3 C21 C22 112.4(4) . . ?
C6 C2 C1 120.0(5) . . ?
C16 C18 C15 120.5(5) . . ?
N2 C10 C9 125.2(5) . . ?
C22 C23 N4 121.6(5) . . ?
C23 C22 C24 117.1(5) . . ?
C23 C22 C21 122.1(4) . . ?
C24 C22 C21 120.8(4) . . ?
C4 C3 C1 119.0(4) . . ?
C4 C3 C7 120.8(4) . . ?
C1 C3 C7 120.2(4) . . ?
C25 C24 C22 122.5(5) . . ?
C17 C19 C16 119.5(4) . . ?
C11 C9 C10 116.2(5) . . ?
C11 C9 C8 122.6(5) . . ?
C10 C9 C8 121.2(5) . . ?
C12 C11 C9 119.9(5) . . ?
C26 C25 C24 118.1(5) . . ?
C5 C4 C3 120.7(5) . . ?
N1 C8 C9 112.3(4) . . ?
C6 C5 C4 119.6(5) . . ?
C25 C26 N4 124.7(5) . . ?
C5 C6 C2 121.0(5) . . ?
N2 C13 C12 123.9(5) . . ?
C13 C12 C11 118.7(5) . . ?
C7 N1 C8 121.2(4) . . ?
C20 N3 C21 121.3(4) . . ?
C10 N2 C13 116.0(5) . . ?
C26 N4 C23 116.0(5) . . ?
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
S2 C15 1.787(4) . ?
S2 S1 2.0306(18) . ?
S1 C1 1.781(5) . ?
C20 O2 1.249(5) . ?
C20 N3 1.319(6) . ?
C20 C14 1.494(6) . ?
C7 O1 1.241(5) . ?
C7 N1 1.325(6) . ?
C7 C3 1.500(6) . ?
C14 C17 1.389(6) . ?
C14 C15 1.392(6) . ?
C1 C2 1.387(6) . ?
C1 C3 1.409(6) . ?
C15 C18 1.399(6) . ?
C16 C18 1.379(6) . ?
C16 C19 1.380(7) . ?
C17 C19 1.374(6) . ?
C21 N3 1.464(6) . ?
C21 C22 1.503(6) . ?
C2 C6 1.385(7) . ?
C10 N2 1.336(6) . ?
C10 C9 1.395(7) . ?
C23 C22 1.375(6) . ?
C23 N4 1.386(7) . ?
C22 C24 1.386(6) . ?
C3 C4 1.392(6) . ?
C24 C25 1.344(7) . ?
C9 C11 1.386(7) . ?
C9 C8 1.494(7) . ?
C11 C12 1.380(7) . ?
C25 C26 1.321(7) . ?
C4 C5 1.387(7) . ?
C8 N1 1.466(6) . ?
C5 C6 1.370(7) . ?
C26 N4 1.371(7) . ?
C13 N2 1.341(7) . ?
C13 C12 1.369(7) . ?
O3 C27 1.379(7) . ?
