#------------------------------------------------------------------------------
#$Date: 2019-11-17 04:20:48 +0100 (Sun 17 de Nov de 2019) $
#$Revision: 228091 $
#$URL: svn://www.crystallography.net/cod/cif/7/12/18/7121833.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_7121833
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 H42 N2 O14 S12 Zn'
_chemical_formula_weight         1152.89
_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   geom
_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                 92.050(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.2765(19)
_cell_length_b                   10.2073(13)
_cell_length_c                   16.037(2)
_cell_measurement_reflns_used    6812
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.2
_cell_measurement_theta_min      2.4
_cell_volume                     2335.5(5)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0844
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18865
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.453
_exptl_absorpt_coefficient_mu    1.126
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.373
_refine_diff_density_min         -1.113
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4041
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.1121
_refine_ls_R_factor_gt           0.0872
_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)+(0.0010P)²+26.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1764
_refine_ls_wR_factor_ref         0.1917
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3049
_reflns_number_total             4041
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8cc03197e2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7121829--7121834.cif.'
_cod_database_code               7121833
_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   0.806
_shelx_estimated_absorpt_t_max   0.935
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
Zn1 Zn 1.000000 1.000000 0.500000 0.0241(3) Uani 1 2 d S . P
S1 S 0.68279(13) 0.6668(2) 0.49050(12) 0.0319(5) Uani 1 1 d . . .
S2 S 0.74316(14) 0.4656(2) 0.61393(11) 0.0325(5) Uani 1 1 d . . .
S3 S 0.55401(14) 0.4374(3) 0.39136(13) 0.0470(7) Uani 1 1 d . . .
S4 S 0.6256(2) 0.2418(3) 0.51657(16) 0.0592(8) Uani 1 1 d . . .
S5 S 0.4980(2) 0.2250(5) 0.26570(18) 0.0918(14) Uani 1 1 d . . .
S6 S 0.5822(2) 0.0020(4) 0.4146(2) 0.0774(10) Uani 1 1 d . . .
O1 O 0.7832(4) 0.9323(6) 0.5749(3) 0.0330(13) Uani 1 1 d . . .
O2 O 0.8990(3) 0.8451(5) 0.4997(3) 0.0268(12) Uani 1 1 d . . .
O3 O 0.9323(3) 0.7286(5) 0.6826(3) 0.0293(12) Uani 1 1 d . . .
O4 O 0.8941(4) 0.5256(5) 0.7262(3) 0.0309(13) Uani 1 1 d . . .
O5 O 0.9017(3) 1.1318(5) 0.5478(3) 0.0287(12) Uani 1 1 d . . .
O6 O 1.0402(4) 0.9337(6) 0.6213(3) 0.0319(13) Uani 1 1 d . . .
O7 O 0.9224(4) 1.2518(6) 0.6994(3) 0.0318(13) Uani 1 1 d . . .
N1 N 1.2212(4) 1.5835(8) 0.7150(4) 0.0346(17) Uani 1 1 d . . .
C1 C 0.7844(5) 0.7032(8) 0.5528(4) 0.0240(16) Uani 1 1 d . . .
C2 C 0.8102(5) 0.6113(8) 0.6103(4) 0.0251(17) Uani 1 1 d . . .
C3 C 0.6769(5) 0.5014(8) 0.5217(4) 0.0280(17) Uani 1 1 d . . .
C4 C 0.6254(5) 0.4082(9) 0.4815(5) 0.037(2) Uani 1 1 d . . .
C5 C 0.5459(6) 0.2643(12) 0.3663(6) 0.057(3) Uani 1 1 d . . .
C6 C 0.5800(7) 0.1778(12) 0.4220(6) 0.057(3) Uani 1 1 d . . .
C7 C 0.3824(10) 0.230(3) 0.2794(9) 0.164(11) Uani 1 1 d . . .
H7A H 0.364979 0.160962 0.318195 0.247 Uiso 1 1 calc R U .
H7B H 0.348810 0.217312 0.225676 0.247 Uiso 1 1 calc R U .
H7C H 0.365630 0.315766 0.302418 0.247 Uiso 1 1 calc R U .
C8 C 0.6981(9) -0.0163(13) 0.3749(7) 0.078(4) Uani 1 1 d . . .
H8A H 0.702792 0.034667 0.323402 0.117 Uiso 1 1 calc R U .
H8B H 0.709834 -0.108991 0.363102 0.117 Uiso 1 1 calc R U .
H8C H 0.744632 0.015367 0.416503 0.117 Uiso 1 1 calc R U .
C9 C 0.8257(5) 0.8375(8) 0.5424(4) 0.0258(17) Uani 1 1 d . . .
C10 C 0.8861(5) 0.6254(8) 0.6784(4) 0.0261(17) Uani 1 1 d . . .
C11 C 1.1973(6) 1.6608(10) 0.6501(5) 0.037(2) Uani 1 1 d . . .
H11 H 1.225929 1.744336 0.645418 0.045 Uiso 1 1 calc R U .
C12 C 1.1322(6) 1.6213(10) 0.5904(5) 0.038(2) Uani 1 1 d . . .
H12 H 1.115844 1.678129 0.545217 0.046 Uiso 1 1 calc R U .
C13 C 1.0900(5) 1.4995(9) 0.5952(4) 0.0299(18) Uani 1 1 d . . .
C14 C 1.1175(5) 1.4203(9) 0.6609(4) 0.034(2) Uani 1 1 d . . .
H14 H 1.092613 1.334226 0.664481 0.041 Uiso 1 1 calc R U .
C15 C 1.1809(6) 1.4640(10) 0.7219(5) 0.039(2) Uani 1 1 d . . .
H15 H 1.196302 1.410124 0.768753 0.047 Uiso 1 1 calc R U .
C16 C 1.0132(5) 1.4513(8) 0.5356(4) 0.0303(18) Uani 1 1 d . . .
H16A H 0.956622 1.432981 0.567597 0.036 Uiso 1 1 calc R U .
H16B H 1.033463 1.367711 0.510617 0.036 Uiso 1 1 calc R U .
C17 C 1.2872(6) 1.6298(10) 0.7827(5) 0.045(2) Uani 1 1 d . . .
H17A H 1.284912 1.725601 0.785813 0.067 Uiso 1 1 calc R U .
H17B H 1.350962 1.601784 0.770753 0.067 Uiso 1 1 calc R U .
H17C H 1.269029 1.592425 0.836036 0.067 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
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'
Zn Zn 0.2839 1.4301 '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 Zn1 O5 180.0 . 3_776
O5 Zn1 O6 91.84(19) . .
O5 Zn1 O6 88.2(2) 3_776 .
O5 Zn1 O6 88.16(19) . 3_776
O5 Zn1 O6 91.84(19) 3_776 3_776
O6 Zn1 O6 180.0 . 3_776
O5 Zn1 O2 90.86(19) . .
O5 Zn1 O2 89.14(19) 3_776 .
O6 Zn1 O2 85.80(19) . .
O6 Zn1 O2 94.20(19) 3_776 .
O5 Zn1 O2 89.14(19) . 3_776
O5 Zn1 O2 90.86(19) 3_776 3_776
O6 Zn1 O2 94.20(19) . 3_776
O6 Zn1 O2 85.80(19) 3_776 3_776
O2 Zn1 O2 180.00(19) . 3_776
C3 S1 C1 95.0(3) . .
C3 S2 C2 94.1(4) . .
C4 S3 C5 92.7(5) . .
C6 S4 C4 94.9(5) . .
C7 S5 C5 102.9(6) . .
C6 S6 C8 98.3(6) . .
C9 O2 Zn1 127.6(5) . .
C11 N1 C15 119.8(7) . .
C11 N1 C17 121.1(8) . .
C15 N1 C17 119.0(7) . .
C2 C1 C9 127.4(6) . .
C2 C1 S1 115.8(6) . .
C9 C1 S1 116.4(5) . .
C1 C2 C10 126.3(7) . .
C1 C2 S2 118.0(5) . .
C10 C2 S2 115.4(5) . .
C4 C3 S1 124.7(6) . .
C4 C3 S2 121.3(7) . .
S1 C3 S2 114.0(4) . .
C3 C4 S3 124.1(7) . .
C3 C4 S4 121.6(6) . .
S3 C4 S4 114.4(5) . .
C6 C5 S5 125.3(9) . .
C6 C5 S3 118.5(7) . .
S5 C5 S3 116.1(7) . .
C5 C6 S4 116.6(8) . .
C5 C6 S6 128.5(8) . .
S4 C6 S6 114.9(7) . .
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 126.2(7) . .
O1 C9 C1 117.1(6) . .
O2 C9 C1 116.6(7) . .
O3 C10 O4 127.3(7) . .
O3 C10 C2 118.9(7) . .
O4 C10 C2 113.8(7) . .
N1 C11 C12 121.1(9) . .
N1 C11 H11 119.4 . .
C12 C11 H11 119.4 . .
C11 C12 C13 120.7(8) . .
C11 C12 H12 119.7 . .
C13 C12 H12 119.7 . .
C14 C13 C12 117.2(7) . .
C14 C13 C16 118.3(8) . .
C12 C13 C16 124.4(7) . .
C15 C14 C13 121.0(9) . .
C15 C14 H14 119.5 . .
C13 C14 H14 119.5 . .
N1 C15 C14 120.1(8) . .
N1 C15 H15 120.0 . .
C14 C15 H15 120.0 . .
C13 C16 C16 114.1(8) . 3_786
C13 C16 H16A 108.7 . .
C16 C16 H16A 108.7 3_786 .
C13 C16 H16B 108.7 . .
C16 C16 H16B 108.7 3_786 .
H16A C16 H16B 107.6 . .
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
Zn1 O5 2.108(5) .
Zn1 O5 2.108(5) 3_776
Zn1 O6 2.119(5) .
Zn1 O6 2.119(5) 3_776
Zn1 O2 2.140(5) .
Zn1 O2 2.140(5) 3_776
S1 C3 1.764(9) .
S1 C1 1.771(7) .
S2 C3 1.765(7) .
S2 C2 1.770(8) .
S3 C4 1.765(8) .
S3 C5 1.815(12) .
S4 C6 1.755(9) .
S4 C4 1.789(10) .
S5 C7 1.673(14) .
S5 C5 1.776(9) .
S6 C6 1.799(12) .
S6 C8 1.804(12) .
O1 C9 1.264(9) .
O2 C9 1.273(8) .
O3 C10 1.243(9) .
O4 C10 1.277(9) .
N1 C11 1.340(11) .
N1 C15 1.355(11) .
N1 C17 1.488(10) .
C1 C2 1.357(10) .
C1 C9 1.504(11) .
C2 C10 1.518(10) .
C3 C4 1.352(11) .
C5 C6 1.335(15) .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C11 C12 1.371(11) .
C11 H11 0.9500 .
C12 C13 1.385(12) .
C12 H12 0.9500 .
C13 C14 1.375(11) .
C13 C16 1.510(10) .
C14 C15 1.383(11) .
C14 H14 0.9500 .
C15 H15 0.9500 .
C16 C16 1.551(15) 3_786
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
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 -11.8(6) .
C3 S1 C1 C9 174.6(5) .
C9 C1 C2 C10 1.2(12) .
S1 C1 C2 C10 -171.6(6) .
C9 C1 C2 S2 175.0(6) .
S1 C1 C2 S2 2.2(8) .
C3 S2 C2 C1 8.6(6) .
C3 S2 C2 C10 -176.9(5) .
C1 S1 C3 C4 -164.0(7) .
C1 S1 C3 S2 17.5(4) .
C2 S2 C3 C4 165.0(7) .
C2 S2 C3 S1 -16.4(5) .
S1 C3 C4 S3 -0.9(10) .
S2 C3 C4 S3 177.5(4) .
S1 C3 C4 S4 178.7(4) .
S2 C3 C4 S4 -2.9(10) .
C5 S3 C4 C3 163.6(7) .
C5 S3 C4 S4 -16.0(5) .
C6 S4 C4 C3 -162.2(7) .
C6 S4 C4 S3 17.4(6) .
C7 S5 C5 C6 100.4(13) .
C7 S5 C5 S3 -83.2(11) .
C4 S3 C5 C6 8.4(9) .
C4 S3 C5 S5 -168.3(5) .
S5 C5 C6 S4 178.8(5) .
S3 C5 C6 S4 2.5(12) .
S5 C5 C6 S6 -3.5(15) .
S3 C5 C6 S6 -179.8(6) .
C4 S4 C6 C5 -11.8(9) .
C4 S4 C6 S6 170.2(6) .
C8 S6 C6 C5 94.4(11) .
C8 S6 C6 S4 -87.8(7) .
Zn1 O2 C9 O1 21.7(10) .
Zn1 O2 C9 C1 -160.3(4) .
C2 C1 C9 O1 -97.7(9) .
S1 C1 C9 O1 75.1(7) .
C2 C1 C9 O2 84.1(9) .
S1 C1 C9 O2 -103.2(6) .
C1 C2 C10 O3 -1.9(11) .
S2 C2 C10 O3 -175.9(5) .
C1 C2 C10 O4 177.7(7) .
S2 C2 C10 O4 3.8(8) .
C15 N1 C11 C12 0.3(12) .
C17 N1 C11 C12 -176.0(7) .
N1 C11 C12 C13 -0.6(12) .
C11 C12 C13 C14 -1.2(11) .
C11 C12 C13 C16 175.8(7) .
C12 C13 C14 C15 3.5(11) .
C16 C13 C14 C15 -173.8(7) .
C11 N1 C15 C14 2.0(11) .
C17 N1 C15 C14 178.3(7) .
C13 C14 C15 N1 -3.9(12) .
C14 C13 C16 C16 179.4(8) 3_786
C12 C13 C16 C16 2.3(12) 3_786
