#------------------------------------------------------------------------------
#$Date: 2025-08-22 10:56:18 +0200 (Fri 22 de Aug de 2025) $
#$Revision: 301860 $
#$URL: svn://www.crystallography.net/cod/cif/7/12/18/7121832.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_7121832
loop_
_publ_author_name
'Zhang, Ping'
'Huo, Peng'
'Zhang, Xuan'
'Zhu, Qin-Yu'
'Dai, Jie'
_publ_section_title
;
 C-C to C[double bond, length as m-dash]C conversion within a
 supramolecular framework of tetrathiafulvalene: a confinement effect and
 an oxygen related dehydrogenation.
;
_journal_issue                   53
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7334
_journal_page_last               7337
_journal_paper_doi               10.1039/c8cc03197e
_journal_volume                  54
_journal_year                    2018
_chemical_formula_sum            'C34 H40 Mn N2 O14 S12'
_chemical_formula_weight         1140.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-04-18 deposited with the CCDC.
2018-06-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.815(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.957(3)
_cell_length_b                   10.7952(19)
_cell_length_c                   15.701(3)
_cell_measurement_reflns_used    8610
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      3.1
_cell_volume                     2357.3(8)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_number            5311
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.491
_diffrn_reflns_theta_min         3.093
_exptl_absorpt_coefficient_mu    0.875
_exptl_absorpt_correction_T_max  0.9176
_exptl_absorpt_correction_T_min  0.7210
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_description       Block
_exptl_crystal_F_000             1174
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.772
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         5311
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      12.292
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0757P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1348
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3546
_reflns_number_total             5311
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8cc03197e2.cif
_cod_data_source_block           3'
_cod_depositor_comments
'Adding full bibliography for 7121829--7121834.cif.'
_cod_original_cell_volume        2357.3(7)
_cod_database_code               7121832
_shelx_shelxl_version_number     2016/6
_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   0.721
_shelx_estimated_absorpt_t_max   0.918
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Mn1 Mn 0.500000 0.500000 0.000000 0.03167(18) Uani 1 2 d S . P
S1 S 0.17830(7) 0.18320(8) -0.02157(5) 0.0381(2) Uani 1 1 d . . .
S2 S 0.24551(7) -0.01793(7) 0.09478(5) 0.0383(2) Uani 1 1 d . . .
S3 S 0.03992(7) -0.01538(8) -0.13362(5) 0.0397(2) Uani 1 1 d . . .
S4 S 0.10617(9) -0.20928(9) -0.01132(6) 0.0594(3) Uani 1 1 d . . .
S5 S -0.03504(8) -0.20119(9) -0.26754(6) 0.0466(3) Uani 1 1 d . . .
S6 S 0.04092(14) -0.41458(11) -0.13493(10) 0.1126(8) Uani 1 1 d . . .
O1 O 0.28342(18) 0.4245(2) 0.07364(16) 0.0453(6) Uani 1 1 d . . .
O2 O 0.39755(18) 0.3473(2) -0.00330(14) 0.0382(6) Uani 1 1 d . . .
O3 O 0.43167(18) 0.2288(2) 0.18546(14) 0.0429(6) Uani 1 1 d . . .
O4 O 0.4060(2) 0.0291(2) 0.21239(14) 0.0460(7) Uani 1 1 d . . .
O5 O 0.3903(2) 0.6261(2) 0.04231(16) 0.0417(6) Uani 1 1 d D . .
O6 O 0.5348(2) 0.4387(3) 0.13133(15) 0.0503(7) Uani 1 1 d D . .
O7 O 0.4274(2) 0.7658(3) 0.18243(18) 0.0494(8) Uani 1 1 d D . .
N1 N 0.7225(3) 0.1043(3) 0.2249(2) 0.0536(8) Uani 1 1 d . . .
C1 C 0.2826(2) 0.2109(3) 0.04573(17) 0.0265(6) Uani 1 1 d . . .
C2 C 0.3120(2) 0.1212(3) 0.10033(17) 0.0276(6) Uani 1 1 d . . .
C3 C 0.1717(2) 0.0257(3) 0.00404(19) 0.0327(7) Uani 1 1 d . . .
C4 C 0.1138(2) -0.0541(3) -0.0416(2) 0.0362(7) Uani 1 1 d . . .
C5 C 0.0237(3) -0.1706(3) -0.1661(2) 0.0404(8) Uani 1 1 d . . .
C6 C 0.0550(3) -0.2577(3) -0.1114(3) 0.0564(11) Uani 1 1 d . . .
C7 C -0.1521(4) -0.2226(8) -0.2415(3) 0.130(3) Uani 1 1 d . . .
H7A H -0.187722 -0.147226 -0.251611 0.196 Uiso 1 1 calc DR U .
H7B H -0.151724 -0.244919 -0.182287 0.196 Uiso 1 1 calc DR U .
H7C H -0.181715 -0.287596 -0.276189 0.196 Uiso 1 1 calc R U .
C8 C 0.1252(9) -0.4849(6) -0.0651(7) 0.280(9) Uani 1 1 d . . .
H8A H 0.146150 -0.427909 -0.020439 0.420 Uiso 1 1 calc R U .
H8B H 0.179245 -0.509551 -0.095163 0.420 Uiso 1 1 calc R U .
H8C H 0.097426 -0.556610 -0.040691 0.420 Uiso 1 1 calc R U .
C9 C 0.3256(3) 0.3391(3) 0.03926(19) 0.0323(7) Uani 1 1 d . . .
C10 C 0.3905(2) 0.1278(3) 0.17182(18) 0.0322(7) Uani 1 1 d . . .
C11 C 0.6925(3) -0.0113(4) 0.2253(3) 0.0595(11) Uani 1 1 d . . .
H11 H 0.713539 -0.062611 0.270631 0.071 Uiso 1 1 calc R U .
C12 C 0.6310(3) -0.0579(4) 0.1605(2) 0.0568(11) Uani 1 1 d . . .
H12 H 0.612151 -0.140490 0.161554 0.068 Uiso 1 1 calc R U .
C13 C 0.5969(3) 0.0181(4) 0.0933(2) 0.0508(10) Uani 1 1 d . . .
C14 C 0.6296(4) 0.1394(4) 0.0946(3) 0.0604(12) Uani 1 1 d . . .
H14 H 0.608426 0.193472 0.050877 0.072 Uiso 1 1 calc R U .
C15 C 0.6929(4) 0.1798(4) 0.1601(3) 0.0628(12) Uani 1 1 d . . .
H15 H 0.715734 0.260741 0.159571 0.075 Uiso 1 1 calc R U .
C16 C 0.5258(3) -0.0335(4) 0.0273(2) 0.0549(10) Uani 1 1 d . . .
H16 H 0.517835 -0.118958 0.025054 0.066 Uiso 1 1 calc R U .
C17 C 0.7865(4) 0.1516(5) 0.2970(3) 0.0745(14) Uani 1 1 d . . .
H17A H 0.749510 0.198134 0.334799 0.112 Uiso 1 1 calc R U .
H17B H 0.834511 0.204283 0.275705 0.112 Uiso 1 1 calc R U .
H17C H 0.817164 0.083371 0.327533 0.112 Uiso 1 1 calc R U .
H7D H 0.422(2) 0.827(3) 0.1863(19) 0.011(9) Uiso 1 1 d . . .
H6A H 0.502(3) 0.377(3) 0.143(2) 0.053(12) Uiso 1 1 d D . .
H6B H 0.549(4) 0.481(4) 0.176(2) 0.082(17) Uiso 1 1 d D . .
H5A H 0.403(4) 0.668(4) 0.088(2) 0.092(18) Uiso 1 1 d D . .
H7E H 0.473(4) 0.740(6) 0.217(4) 0.11(2) Uiso 1 1 d . . .
H5B H 0.342(3) 0.583(4) 0.050(3) 0.086(18) Uiso 1 1 d 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'
O O 0.0106 0.0060 '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'
Mn Mn 0.3368 0.7283 '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
O5 Mn1 O5 180.0 3_665 .
O5 Mn1 O2 89.81(10) 3_665 .
O5 Mn1 O2 90.19(10) . .
O5 Mn1 O2 90.19(10) 3_665 3_665
O5 Mn1 O2 89.81(10) . 3_665
O2 Mn1 O2 180.00(7) . 3_665
O5 Mn1 O6 89.55(11) 3_665 .
O5 Mn1 O6 90.45(11) . .
O2 Mn1 O6 83.51(9) . .
O2 Mn1 O6 96.49(9) 3_665 .
O5 Mn1 O6 90.45(11) 3_665 3_665
O5 Mn1 O6 89.55(11) . 3_665
O2 Mn1 O6 96.49(9) . 3_665
O2 Mn1 O6 83.51(9) 3_665 3_665
O6 Mn1 O6 180.0 . 3_665
C1 S1 C3 94.80(14) . .
C3 S2 C2 94.69(14) . .
C4 S3 C5 93.67(15) . .
C4 S4 C6 94.13(16) . .
C5 S5 C7 100.9(2) . .
C6 S6 C8 103.6(3) . .
C9 O2 Mn1 126.4(2) . .
Mn1 O5 H5A 119(4) . .
Mn1 O5 H5B 107(4) . .
H5A O5 H5B 106(5) . .
Mn1 O6 H6A 112(3) . .
Mn1 O6 H6B 129(3) . .
H6A O6 H6B 110(4) . .
H7D O7 H7E 110(5) . .
C11 N1 C15 120.1(4) . .
C11 N1 C17 119.9(4) . .
C15 N1 C17 120.0(4) . .
C2 C1 C9 127.1(3) . .
C2 C1 S1 117.3(2) . .
C9 C1 S1 115.4(2) . .
C1 C2 C10 127.7(3) . .
C1 C2 S2 117.0(2) . .
C10 C2 S2 115.1(2) . .
C4 C3 S1 122.7(2) . .
C4 C3 S2 123.1(3) . .
S1 C3 S2 114.19(17) . .
C3 C4 S4 121.1(2) . .
C3 C4 S3 124.8(3) . .
S4 C4 S3 114.06(18) . .
C6 C5 S5 123.9(3) . .
C6 C5 S3 117.5(3) . .
S5 C5 S3 118.6(2) . .
C5 C6 S6 121.9(3) . .
C5 C6 S4 117.3(3) . .
S6 C6 S4 120.8(2) . .
S5 C7 H7A 109.5 . .
S5 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
S5 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
S6 C8 H8A 109.5 . .
S6 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
S6 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
O1 C9 O2 127.5(3) . .
O1 C9 C1 116.4(3) . .
O2 C9 C1 116.1(3) . .
O4 C10 O3 127.0(3) . .
O4 C10 C2 115.1(3) . .
O3 C10 C2 117.9(3) . .
N1 C11 C12 121.6(4) . .
N1 C11 H11 119.2 . .
C12 C11 H11 119.2 . .
C11 C12 C13 120.0(4) . .
C11 C12 H12 120.0 . .
C13 C12 H12 120.0 . .
C14 C13 C12 117.1(4) . .
C14 C13 C16 124.4(4) . .
C12 C13 C16 118.4(4) . .
C13 C14 C15 120.2(4) . .
C13 C14 H14 119.9 . .
C15 C14 H14 119.9 . .
N1 C15 C14 120.9(4) . .
N1 C15 H15 119.5 . .
C14 C15 H15 119.5 . .
C16 C16 C13 123.9(6) 3_655 .
C16 C16 H16 118.1 3_655 .
C13 C16 H16 118.1 . .
N1 C17 H17A 109.5 . .
N1 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
N1 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O5 2.194(3) 3_665
Mn1 O5 2.194(3) .
Mn1 O2 2.180(2) .
Mn1 O2 2.180(2) 3_665
Mn1 O6 2.181(2) .
Mn1 O6 2.181(2) 3_665
S1 C1 1.751(3) .
S1 C3 1.751(3) .
S2 C3 1.751(3) .
S2 C2 1.764(3) .
S3 C4 1.754(3) .
S3 C5 1.761(3) .
S4 C4 1.747(3) .
S4 C6 1.750(4) .
S5 C5 1.760(3) .
S5 C7 1.733(6) .
S6 C6 1.741(4) .
S6 C8 1.716(6) .
O1 C9 1.242(4) .
O2 C9 1.255(4) .
O3 C10 1.243(4) .
O4 C10 1.251(4) .
O5 H5A 0.853(19) .
O5 H5B 0.843(19) .
O6 H6A 0.838(19) .
O6 H6B 0.839(19) .
O7 H7D 0.67(3) .
O7 H7E 0.85(6) .
N1 C11 1.317(6) .
N1 C15 1.342(5) .
N1 C17 1.474(6) .
C1 C2 1.334(4) .
C1 C9 1.515(4) .
C2 C10 1.503(4) .
C3 C4 1.347(4) .
C5 C6 1.323(5) .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C11 C12 1.370(6) .
C11 H11 0.9300 .
C12 C13 1.389(5) .
C12 H12 0.9300 .
C13 C14 1.386(6) .
C13 C16 1.481(6) .
C14 C15 1.370(6) .
C14 H14 0.9300 .
C15 H15 0.9300 .
C16 C16 1.294(8) 3_655
C16 H16 0.9300 .
C17 H17A 0.9600 .
C17 H17B 0.9600 .
C17 H17C 0.9600 .
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_4
C3 S1 C1 C2 -10.3(3) .
C3 S1 C1 C9 173.8(3) .
C9 C1 C2 C10 4.1(6) .
S1 C1 C2 C10 -171.3(3) .
C9 C1 C2 S2 178.3(3) .
S1 C1 C2 S2 3.0(4) .
C3 S2 C2 C1 6.0(3) .
C3 S2 C2 C10 -179.0(2) .
C1 S1 C3 C4 -166.8(3) .
C1 S1 C3 S2 14.1(2) .
C2 S2 C3 C4 168.1(3) .
C2 S2 C3 S1 -12.9(2) .
S1 C3 C4 S4 -177.5(2) .
S2 C3 C4 S4 1.5(5) .
S1 C3 C4 S3 1.9(5) .
S2 C3 C4 S3 -179.1(2) .
C6 S4 C4 C3 -162.3(4) .
C6 S4 C4 S3 18.3(3) .
C5 S3 C4 C3 163.1(3) .
C5 S3 C4 S4 -17.5(2) .
C7 S5 C5 C6 83.9(5) .
C7 S5 C5 S3 -94.6(4) .
C4 S3 C5 C6 9.5(4) .
C4 S3 C5 S5 -171.8(2) .
S5 C5 C6 S6 0.0(6) .
S3 C5 C6 S6 178.6(3) .
S5 C5 C6 S4 -176.8(2) .
S3 C5 C6 S4 1.8(5) .
C8 S6 C6 C5 160.2(7) .
C8 S6 C6 S4 -23.2(7) .
C4 S4 C6 C5 -12.2(4) .
C4 S4 C6 S6 171.0(3) .
Mn1 O2 C9 O1 20.3(5) .
Mn1 O2 C9 C1 -162.87(18) .
C2 C1 C9 O1 -99.9(4) .
S1 C1 C9 O1 75.5(3) .
C2 C1 C9 O2 82.9(4) .
S1 C1 C9 O2 -101.6(3) .
C1 C2 C10 O4 -177.9(3) .
S2 C2 C10 O4 7.7(4) .
C1 C2 C10 O3 3.2(5) .
S2 C2 C10 O3 -171.2(3) .
C15 N1 C11 C12 0.0(7) .
C17 N1 C11 C12 178.3(4) .
N1 C11 C12 C13 -1.6(7) .
C11 C12 C13 C14 1.4(6) .
C11 C12 C13 C16 -176.2(4) .
C12 C13 C14 C15 0.2(6) .
C16 C13 C14 C15 177.6(4) .
C11 N1 C15 C14 1.6(7) .
C17 N1 C15 C14 -176.7(4) .
C13 C14 C15 N1 -1.7(7) .
C14 C13 C16 C16 -12.6(8) 3_655
C12 C13 C16 C16 164.8(5) 3_655
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168350682
