#------------------------------------------------------------------------------
#$Date: 2019-11-28 15:30:59 +0100 (jue 28 de nov de 2019) $
#$Revision: 244109 $
#$URL: svn://www.crystallography.net/cod/cif/7/23/83/7238308.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_7238308
loop_
_publ_author_name
'Zhang, Ya-Nan'
'Wang, Yao-Yu'
'Hou, Lei'
'Liu, Ping'
'Liu, Jian-Qiang'
'Shi, Qi-Zhen'
_publ_section_title
;
 A series of metal--organic coordination polymers assembled with disulfide
 ligand involving in situ cleavage of S--S under co-ligand intervention
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              3840
_journal_paper_doi               10.1039/c005228k
_journal_volume                  12
_journal_year                    2010
_chemical_formula_moiety         'C46 H40 Cu2 N8 O12 S4'
_chemical_formula_sum            'C46 H40 Cu2 N8 O12 S4'
_chemical_formula_weight         1152.18
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                113.038(3)
_cell_angle_beta                 92.382(3)
_cell_angle_gamma                112.130(2)
_cell_formula_units_Z            1
_cell_length_a                   9.3823(12)
_cell_length_b                   12.2541(16)
_cell_length_c                   12.379(3)
_cell_measurement_reflns_used    2084
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.58
_cell_measurement_theta_min      2.37
_cell_volume                     1183.0(4)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        APEX2
_computing_molecular_graphics    APEX2
_computing_publication_material  APEX2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX SMART II'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0177
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5982
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.149
_exptl_absorpt_correction_T_max  0.8466
_exptl_absorpt_correction_T_min  0.7622
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 1997)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         4174
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0688P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1067
_reflns_number_gt                3236
_reflns_number_total             4174
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c005228k.txt
_cod_data_source_block           xb2916
_cod_database_code               7238308
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cu1 Cu 0.20230(4) 0.16082(3) -0.07161(3) 0.03417(14) Uani 1 1 d .
S2 S -0.31303(9) 0.40404(9) 0.55390(7) 0.0488(2) Uani 1 1 d .
S1 S -0.22548(9) 0.52689(8) 0.47659(8) 0.0494(2) Uani 1 1 d .
O1 O 0.0420(3) 0.3487(2) -0.0165(2) 0.0600(6) Uani 1 1 d .
O2 O 0.0665(2) 0.2021(2) 0.03828(19) 0.0461(5) Uani 1 1 d .
O3 O -1.0235(3) -0.0909(2) 0.3194(2) 0.0576(6) Uani 1 1 d .
O4 O -1.0239(2) -0.00835(19) 0.18805(18) 0.0425(5) Uani 1 1 d .
O5 O 0.2184(3) 0.0284(2) 0.0150(2) 0.0542(6) Uani 1 1 d D
N2 N 0.3606(3) 0.1375(2) -0.1726(2) 0.0355(5) Uani 1 1 d .
N1 N 0.3962(3) 0.3225(2) 0.0393(2) 0.0343(5) Uani 1 1 d .
N4 N -0.5843(3) 0.2185(2) 0.5195(2) 0.0443(6) Uani 1 1 d .
N3 N -0.0828(3) 0.5205(2) 0.3038(2) 0.0444(6) Uani 1 1 d .
C13 C -0.0353(3) 0.3449(3) 0.1619(3) 0.0377(7) Uani 1 1 d .
C22 C -0.9632(3) -0.0071(3) 0.2839(3) 0.0401(7) Uani 1 1 d .
C17 C -0.5106(3) 0.2960(3) 0.4693(2) 0.0372(7) Uani 1 1 d .
C5 C 0.5275(3) 0.3419(3) -0.0069(2) 0.0339(6) Uani 1 1 d .
C6 C 0.5102(3) 0.2338(3) -0.1230(3) 0.0362(7) Uani 1 1 d .
C16 C -0.1492(3) 0.4444(3) 0.3571(3) 0.0395(7) Uani 1 1 d .
C1 C 0.4032(4) 0.4173(3) 0.1450(3) 0.0415(7) Uani 1 1 d .
H1 H 0.3146 0.4042 0.1783 0.050 Uiso 1 1 calc R
C20 C -0.8061(3) 0.1082(3) 0.3524(2) 0.0353(6) Uani 1 1 d .
C15 C -0.1587(4) 0.3195(3) 0.3219(3) 0.0478(8) Uani 1 1 d .
H15 H -0.2051 0.2700 0.3624 0.057 Uiso 1 1 calc R
C11 C 0.0274(3) 0.2959(3) 0.0511(3) 0.0421(7) Uani 1 1 d .
C14 C -0.0967(4) 0.2713(3) 0.2246(3) 0.0468(8) Uani 1 1 d .
H14 H -0.0958 0.1896 0.2008 0.056 Uiso 1 1 calc R
C19 C -0.7282(3) 0.1941(3) 0.3057(3) 0.0418(7) Uani 1 1 d .
H19 H -0.7770 0.1872 0.2349 0.050 Uiso 1 1 calc R
C21 C -0.7315(4) 0.1271(3) 0.4614(3) 0.0425(7) Uani 1 1 d .
H21 H -0.7864 0.0736 0.4962 0.051 Uiso 1 1 calc R
C4 C 0.6643(4) 0.4559(3) 0.0501(3) 0.0439(7) Uani 1 1 d .
H4 H 0.7528 0.4669 0.0168 0.053 Uiso 1 1 calc R
C3 C 0.6687(4) 0.5533(3) 0.1567(3) 0.0467(8) Uani 1 1 d .
H3 H 0.7593 0.6317 0.1952 0.056 Uiso 1 1 calc R
C18 C -0.5774(3) 0.2903(3) 0.3649(3) 0.0413(7) Uani 1 1 d .
H18 H -0.5227 0.3493 0.3352 0.050 Uiso 1 1 calc R
C2 C 0.5374(4) 0.5333(3) 0.2057(3) 0.0464(8) Uani 1 1 d .
H2 H 0.5391 0.5970 0.2787 0.056 Uiso 1 1 calc R
C7 C 0.6318(4) 0.2278(3) -0.1797(3) 0.0511(8) Uani 1 1 d .
H7 H 0.7337 0.2935 -0.1442 0.061 Uiso 1 1 calc R
C12 C -0.0297(3) 0.4689(3) 0.2067(3) 0.0445(7) Uani 1 1 d .
H12 H 0.0136 0.5199 0.1669 0.053 Uiso 1 1 calc R
C9 C 0.4509(4) 0.0259(3) -0.3401(3) 0.0505(8) Uani 1 1 d .
H9 H 0.4285 -0.0458 -0.4137 0.061 Uiso 1 1 calc R
C10 C 0.3335(4) 0.0366(3) -0.2794(3) 0.0420(7) Uani 1 1 d .
H10 H 0.2312 -0.0289 -0.3139 0.050 Uiso 1 1 calc R
C8 C 0.6011(4) 0.1230(4) -0.2901(3) 0.0579(9) Uani 1 1 d .
H8 H 0.6820 0.1185 -0.3300 0.070 Uiso 1 1 calc R
C23 C 0.3342(6) 0.0011(5) 0.0527(5) 0.1040(17) Uani 1 1 d .
H23A H 0.3525 -0.0604 -0.0155 0.156 Uiso 1 1 calc R
H23B H 0.3019 -0.0359 0.1079 0.156 Uiso 1 1 calc R
H23C H 0.4296 0.0805 0.0922 0.156 Uiso 1 1 calc R
O6 O 0.0964(4) 0.8134(2) 0.4585(3) 0.0744(8) Uani 1 1 d D
H6A H 0.068(6) 0.839(4) 0.413(3) 0.112 Uiso 1 1 d D
H6B H 0.066(5) 0.7320(12) 0.420(3) 0.112 Uiso 1 1 d D
H5A H 0.129(3) -0.031(4) -0.002(6) 0.18(3) 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'
Cu Cu 0.3201 1.2651 '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'
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
O4 Cu1 O2 90.79(9) 2_455 .
O4 Cu1 N2 95.31(9) 2_455 .
O2 Cu1 N2 173.81(9) . .
O4 Cu1 N1 175.43(8) 2_455 .
O2 Cu1 N1 92.94(9) . .
N2 Cu1 N1 80.92(9) . .
O4 Cu1 O5 86.53(9) 2_455 .
O2 Cu1 O5 85.71(9) . .
N2 Cu1 O5 95.68(9) . .
N1 Cu1 O5 96.38(9) . .
C17 S2 S1 105.53(10) . .
C16 S1 S2 105.40(11) . .
C11 O2 Cu1 120.32(19) . .
C22 O4 Cu1 121.37(18) . 2_455
C23 O5 Cu1 136.2(3) . .
C23 O5 H5A 113(4) . .
Cu1 O5 H5A 108(5) . .
C10 N2 C6 118.5(3) . .
C10 N2 Cu1 126.6(2) . .
C6 N2 Cu1 114.83(19) . .
C1 N1 C5 118.2(2) . .
C1 N1 Cu1 126.9(2) . .
C5 N1 Cu1 114.46(18) . .
C17 N4 C21 116.8(2) . .
C16 N3 C12 117.0(3) . .
C12 C13 C14 117.1(3) . .
C12 C13 C11 119.8(3) . .
C14 C13 C11 123.0(3) . .
O3 C22 O4 124.7(3) . .
O3 C22 C20 120.9(3) . .
O4 C22 C20 114.4(2) . .
N4 C17 C18 124.2(3) . .
N4 C17 S2 110.5(2) . .
C18 C17 S2 125.2(2) . .
N1 C5 C4 121.9(3) . .
N1 C5 C6 114.9(2) . .
C4 C5 C6 123.3(3) . .
N2 C6 C7 121.1(3) . .
N2 C6 C5 114.5(2) . .
C7 C6 C5 124.4(3) . .
N3 C16 C15 124.1(3) . .
N3 C16 S1 109.7(2) . .
C15 C16 S1 126.1(2) . .
N1 C1 C2 122.2(3) . .
N1 C1 H1 118.9 . .
C2 C1 H1 118.9 . .
C19 C20 C21 117.9(3) . .
C19 C20 C22 121.2(3) . .
C21 C20 C22 120.8(3) . .
C14 C15 C16 117.4(3) . .
C14 C15 H15 121.3 . .
C16 C15 H15 121.3 . .
O1 C11 O2 125.3(3) . .
O1 C11 C13 119.3(3) . .
O2 C11 C13 115.3(3) . .
C15 C14 C13 120.0(3) . .
C15 C14 H14 120.0 . .
C13 C14 H14 120.0 . .
C20 C19 C18 119.6(3) . .
C20 C19 H19 120.2 . .
C18 C19 H19 120.2 . .
N4 C21 C20 123.5(3) . .
N4 C21 H21 118.3 . .
C20 C21 H21 118.3 . .
C3 C4 C5 119.4(3) . .
C3 C4 H4 120.3 . .
C5 C4 H4 120.3 . .
C4 C3 C2 119.2(3) . .
C4 C3 H3 120.4 . .
C2 C3 H3 120.4 . .
C17 C18 C19 117.8(3) . .
C17 C18 H18 121.1 . .
C19 C18 H18 121.1 . .
C3 C2 C1 119.2(3) . .
C3 C2 H2 120.4 . .
C1 C2 H2 120.4 . .
C6 C7 C8 119.4(3) . .
C6 C7 H7 120.3 . .
C8 C7 H7 120.3 . .
N3 C12 C13 124.1(3) . .
N3 C12 H12 118.0 . .
C13 C12 H12 118.0 . .
C8 C9 C10 118.7(3) . .
C8 C9 H9 120.7 . .
C10 C9 H9 120.7 . .
N2 C10 C9 122.7(3) . .
N2 C10 H10 118.7 . .
C9 C10 H10 118.7 . .
C9 C8 C7 119.6(3) . .
C9 C8 H8 120.2 . .
C7 C8 H8 120.2 . .
O5 C23 H23A 109.5 . .
O5 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
O5 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
H6A O6 H6B 108(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O4 1.9251(19) 2_455
Cu1 O2 1.955(2) .
Cu1 N2 2.012(2) .
Cu1 N1 2.017(2) .
Cu1 O5 2.310(2) .
S2 C17 1.786(3) .
S2 S1 2.0293(13) .
S1 C16 1.785(3) .
O1 C11 1.227(4) .
O2 C11 1.289(4) .
O3 C22 1.227(3) .
O4 C22 1.287(3) .
O4 Cu1 1.9251(19) 2_455
O5 C23 1.366(5) .
O5 H5A 0.83(5) .
N2 C10 1.340(4) .
N2 C6 1.361(4) .
N1 C1 1.346(4) .
N1 C5 1.358(4) .
N4 C17 1.330(4) .
N4 C21 1.342(4) .
N3 C16 1.330(4) .
N3 C12 1.336(4) .
C13 C12 1.378(4) .
C13 C14 1.394(4) .
C13 C11 1.508(4) .
C22 C20 1.508(4) .
C17 C18 1.378(4) .
C5 C4 1.378(4) .
C5 C6 1.474(4) .
C6 C7 1.375(4) .
C16 C15 1.383(4) .
C1 C2 1.381(4) .
C1 H1 0.9300 .
C20 C19 1.381(4) .
C20 C21 1.386(4) .
C15 C14 1.378(4) .
C15 H15 0.9300 .
C14 H14 0.9300 .
C19 C18 1.383(4) .
C19 H19 0.9300 .
C21 H21 0.9300 .
C4 C3 1.377(5) .
C4 H4 0.9300 .
C3 C2 1.377(4) .
C3 H3 0.9300 .
C18 H18 0.9300 .
C2 H2 0.9300 .
C7 C8 1.384(5) .
C7 H7 0.9300 .
C12 H12 0.9300 .
C9 C8 1.368(5) .
C9 C10 1.377(4) .
C9 H9 0.9300 .
C10 H10 0.9300 .
C8 H8 0.9300 .
C23 H23A 0.9600 .
C23 H23B 0.9600 .
C23 H23C 0.9600 .
O6 H6A 0.82(5) .
O6 H6B 0.839(10) .
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
C17 S2 S1 C16 -86.62(14) .
O4 Cu1 O2 C11 -104.2(2) 2_455
N2 Cu1 O2 C11 66.1(9) .
N1 Cu1 O2 C11 73.2(2) .
O5 Cu1 O2 C11 169.3(2) .
O4 Cu1 O5 C23 130.4(4) 2_455
O2 Cu1 O5 C23 -138.5(4) .
N2 Cu1 O5 C23 35.4(4) .
N1 Cu1 O5 C23 -46.0(4) .
O4 Cu1 N2 C10 -5.1(2) 2_455
O2 Cu1 N2 C10 -175.4(7) .
N1 Cu1 N2 C10 177.5(3) .
O5 Cu1 N2 C10 81.9(2) .
O4 Cu1 N2 C6 177.03(19) 2_455
O2 Cu1 N2 C6 6.8(9) .
N1 Cu1 N2 C6 -0.37(18) .
O5 Cu1 N2 C6 -95.95(19) .
O4 Cu1 N1 C1 141.6(11) 2_455
O2 Cu1 N1 C1 -3.0(2) .
N2 Cu1 N1 C1 176.2(3) .
O5 Cu1 N1 C1 -89.0(2) .
O4 Cu1 N1 C5 -30.3(12) 2_455
O2 Cu1 N1 C5 -174.98(19) .
N2 Cu1 N1 C5 4.25(19) .
O5 Cu1 N1 C5 99.0(2) .
Cu1 O4 C22 O3 -11.2(4) 2_455
Cu1 O4 C22 C20 168.29(18) 2_455
C21 N4 C17 C18 2.0(5) .
C21 N4 C17 S2 -176.4(2) .
S1 S2 C17 N4 -174.26(19) .
S1 S2 C17 C18 7.4(3) .
C1 N1 C5 C4 -1.3(4) .
Cu1 N1 C5 C4 171.4(2) .
C1 N1 C5 C6 -179.8(2) .
Cu1 N1 C5 C6 -7.2(3) .
C10 N2 C6 C7 -0.8(4) .
Cu1 N2 C6 C7 177.3(2) .
C10 N2 C6 C5 178.7(2) .
Cu1 N2 C6 C5 -3.3(3) .
N1 C5 C6 N2 6.9(4) .
C4 C5 C6 N2 -171.6(3) .
N1 C5 C6 C7 -173.7(3) .
C4 C5 C6 C7 7.8(5) .
C12 N3 C16 C15 3.6(4) .
C12 N3 C16 S1 -175.4(2) .
S2 S1 C16 N3 -177.39(18) .
S2 S1 C16 C15 3.7(3) .
C5 N1 C1 C2 1.3(4) .
Cu1 N1 C1 C2 -170.4(2) .
O3 C22 C20 C19 171.9(3) .
O4 C22 C20 C19 -7.6(4) .
O3 C22 C20 C21 -4.6(4) .
O4 C22 C20 C21 175.8(3) .
N3 C16 C15 C14 -0.8(5) .
S1 C16 C15 C14 178.0(2) .
Cu1 O2 C11 O1 14.9(4) .
Cu1 O2 C11 C13 -162.69(18) .
C12 C13 C11 O1 -19.9(4) .
C14 C13 C11 O1 161.6(3) .
C12 C13 C11 O2 157.9(3) .
C14 C13 C11 O2 -20.6(4) .
C16 C15 C14 C13 -3.3(5) .
C12 C13 C14 C15 4.5(5) .
C11 C13 C14 C15 -177.0(3) .
C21 C20 C19 C18 3.4(4) .
C22 C20 C19 C18 -173.3(3) .
C17 N4 C21 C20 1.9(5) .
C19 C20 C21 N4 -4.6(5) .
C22 C20 C21 N4 172.1(3) .
N1 C5 C4 C3 -0.2(4) .
C6 C5 C4 C3 178.3(3) .
C5 C4 C3 C2 1.7(5) .
N4 C17 C18 C19 -2.9(5) .
S2 C17 C18 C19 175.2(2) .
C20 C19 C18 C17 0.1(4) .
C4 C3 C2 C1 -1.7(5) .
N1 C1 C2 C3 0.2(5) .
N2 C6 C7 C8 1.0(5) .
C5 C6 C7 C8 -178.4(3) .
C16 N3 C12 C13 -2.2(4) .
C14 C13 C12 N3 -1.7(5) .
C11 C13 C12 N3 179.7(3) .
C6 N2 C10 C9 0.6(4) .
Cu1 N2 C10 C9 -177.2(2) .
C8 C9 C10 N2 -0.7(5) .
C10 C9 C8 C7 1.0(5) .
C6 C7 C8 C9 -1.1(5) .
