#------------------------------------------------------------------------------
#$Date: 2019-11-28 16:30:59 +0200 (Thu, 28 Nov 2019) $
#$Revision: 244109 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/83/7238309.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_7238309
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         'C22 H18 Cu N4 O6 S2, 2.24 (H2O)'
_chemical_formula_sum            'C22 H22.48 Cu N4 O8.24 S2'
_chemical_formula_weight         602.42
_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_Hall  '-P 1'
_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                108.8140(10)
_cell_angle_beta                 92.0370(10)
_cell_angle_gamma                97.0100(10)
_cell_formula_units_Z            2
_cell_length_a                   7.5515(3)
_cell_length_b                   11.1038(5)
_cell_length_c                   16.2388(7)
_cell_measurement_reflns_used    6305
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.018
_cell_measurement_theta_min      2.658
_cell_volume                     1275.17(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16420
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.075
_exptl_absorpt_correction_T_max  0.9000
_exptl_absorpt_correction_T_min  0.8552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 1997)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prizm
_exptl_crystal_F_000             619
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.315
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5559
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0549P)²+1.2674P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1065
_reflns_number_gt                4857
_reflns_number_total             5559
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c005228k.txt
_cod_data_source_block           51
_cod_database_code               7238309
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.47458(4) 0.15131(3) 0.189300(18) 0.01663(10) Uani 1 1 d . . .
S2 S -0.08586(9) 0.50501(6) 0.71399(4) 0.02579(15) Uani 1 1 d . . .
S3 S -0.21838(9) 0.40935(7) 0.59621(4) 0.02842(16) Uani 1 1 d . . .
N1 N 0.1213(3) 0.3726(2) 0.55817(15) 0.0290(5) Uani 1 1 d . . .
N2 N 0.0194(3) 0.4324(2) 0.84107(14) 0.0212(4) Uani 1 1 d . . .
N3 N 0.4852(3) 0.97316(19) 0.19326(13) 0.0191(4) Uani 1 1 d . . .
N4 N 0.4954(3) 0.33492(18) 0.19130(13) 0.0174(4) Uani 1 1 d . . .
O1 O 0.0930(2) 0.01512(17) 0.84654(12) 0.0253(4) Uani 1 1 d . . .
O2 O 0.1244(2) 0.18093(18) 0.97158(12) 0.0258(4) Uani 1 1 d . . .
O3 O 0.2894(2) 0.18132(17) 0.27102(11) 0.0229(4) Uani 1 1 d . . .
O4 O 0.4973(3) 0.2412(3) 0.38099(15) 0.0488(7) Uani 1 1 d . . .
C10 C -0.0477(3) 0.3555(3) 0.52533(17) 0.0246(5) Uani 1 1 d . . .
C11 C -0.1053(3) 0.2951(3) 0.43835(18) 0.0291(6) Uani 1 1 d . . .
H11A H -0.2279 0.2856 0.4188 0.035 Uiso 1 1 calc R . .
C12 C 0.0197(3) 0.2490(3) 0.38047(17) 0.0260(5) Uani 1 1 d . . .
H12A H -0.0156 0.2059 0.3203 0.031 Uiso 1 1 calc R . .
C13 C 0.1981(3) 0.2669(2) 0.41181(17) 0.0223(5) Uani 1 1 d . . .
C14 C 0.2405(3) 0.3289(3) 0.50033(17) 0.0286(6) Uani 1 1 d . . .
H14A H 0.3625 0.3414 0.5216 0.034 Uiso 1 1 calc R . .
C15 C 0.3401(3) 0.2266(2) 0.35147(17) 0.0243(5) Uani 1 1 d . . .
C20 C -0.0472(3) 0.3823(2) 0.75798(16) 0.0206(5) Uani 1 1 d . . .
C21 C -0.0761(3) 0.2514(3) 0.71218(17) 0.0239(5) Uani 1 1 d . . .
H21A H -0.1238 0.2198 0.6530 0.029 Uiso 1 1 calc R . .
C22 C -0.0335(3) 0.1682(2) 0.75500(17) 0.0235(5) Uani 1 1 d . . .
H22A H -0.0514 0.0781 0.7255 0.028 Uiso 1 1 calc R . .
C23 C 0.0358(3) 0.2176(2) 0.84182(16) 0.0189(5) Uani 1 1 d . . .
C24 C 0.0589(3) 0.3497(2) 0.88150(16) 0.0208(5) Uani 1 1 d . . .
H24A H 0.1055 0.3839 0.9408 0.025 Uiso 1 1 calc R . .
C25 C 0.0889(3) 0.1303(2) 0.89081(17) 0.0207(5) Uani 1 1 d . . .
C30 C 0.4480(4) 0.8736(2) 0.11975(17) 0.0237(5) Uani 1 1 d . . .
H30A H 0.4157 0.8894 0.0675 0.028 Uiso 1 1 calc R . .
C31 C 0.4544(4) 0.7483(2) 0.11637(16) 0.0227(5) Uani 1 1 d . . .
H31A H 0.4273 0.6800 0.0625 0.027 Uiso 1 1 calc R . .
C32 C 0.5006(3) 0.7222(2) 0.19201(15) 0.0168(5) Uani 1 1 d . . .
C33 C 0.5384(4) 0.8262(2) 0.26837(18) 0.0293(6) Uani 1 1 d . . .
H33A H 0.5697 0.8132 0.3217 0.035 Uiso 1 1 calc R . .
C34 C 0.5302(4) 0.9493(2) 0.26633(18) 0.0295(6) Uani 1 1 d . . .
H34A H 0.5576 1.0197 0.3190 0.035 Uiso 1 1 calc R . .
C35 C 0.5037(3) 0.5884(2) 0.19139(15) 0.0168(5) Uani 1 1 d . . .
C36 C 0.4153(3) 0.4844(2) 0.12347(16) 0.0216(5) Uani 1 1 d . . .
H36A H 0.3554 0.4984 0.0756 0.026 Uiso 1 1 calc R . .
C37 C 0.4142(3) 0.3613(2) 0.12532(16) 0.0228(5) Uani 1 1 d . . .
H37A H 0.3535 0.2919 0.0779 0.027 Uiso 1 1 calc R . .
C38 C 0.5832(3) 0.4343(2) 0.25658(16) 0.0195(5) Uani 1 1 d . . .
H38A H 0.6428 0.4174 0.3033 0.023 Uiso 1 1 calc R . .
C39 C 0.5910(3) 0.5607(2) 0.25875(16) 0.0196(5) Uani 1 1 d . . .
H39A H 0.6556 0.6282 0.3060 0.024 Uiso 1 1 calc R . .
O5 O 0.2375(2) 0.07136(17) 0.08802(12) 0.0233(4) Uani 1 1 d . . .
O7 O 0.1509(2) 0.69514(17) 0.94042(12) 0.0266(4) Uani 1 1 d . . .
O6 O 0.6774(2) 0.12787(17) 0.11710(13) 0.0300(4) Uani 1 1 d . . .
H5A H 0.2082 0.1144 0.0606 0.036 Uiso 1 1 d R . .
H6A H 0.7309 0.1784 0.0980 0.036 Uiso 1 1 d R . .
H6B H 0.7482 0.0795 0.1162 0.036 Uiso 1 1 d R . .
H5B H 0.1458 0.0584 0.1103 0.036 Uiso 1 1 d R . .
H7A H 0.1037 0.6277 0.9064 0.036 Uiso 1 1 d R . .
H7B H 0.0736 0.7290 0.9681 0.036 Uiso 1 1 d R . .
O102 O 0.4759(10) 0.9022(8) 0.4884(5) 0.093(2) Uiso 0.48 1 d P A 1
H10A H 0.4809 0.8758 0.5286 0.112 Uiso 0.48 1 d PR A 1
H10B H 0.4313 0.8501 0.4436 0.112 Uiso 0.48 1 d PR A 1
O103 O 1.0000 0.0000 0.5000 0.175(7) Uiso 0.48 2 d SP B 1
O101 O 0.715(3) 0.003(2) 0.5117(14) 0.291(9) Uiso 0.52 1 d P C 2
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'
Cu Cu 0.3201 1.2651 '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
O3 Cu1 O6 174.44(8) . .
O3 Cu1 N3 92.74(8) . 1_545
O6 Cu1 N3 87.21(8) . 1_545
O3 Cu1 N4 90.55(8) . .
O6 Cu1 N4 88.92(8) . .
N3 Cu1 N4 173.01(8) 1_545 .
O3 Cu1 O5 83.43(7) . .
O6 Cu1 O5 102.13(8) . .
N3 Cu1 O5 89.23(7) 1_545 .
N4 Cu1 O5 97.28(7) . .
C20 S2 S3 104.36(9) . .
C10 S3 S2 104.83(9) . .
C10 N1 C14 115.7(2) . .
C20 N2 C24 117.1(2) . .
C30 N3 C34 117.9(2) . .
C30 N3 Cu1 118.94(16) . 1_565
C34 N3 Cu1 123.12(17) . 1_565
C38 N4 C37 117.4(2) . .
C38 N4 Cu1 123.38(16) . .
C37 N4 Cu1 119.17(16) . .
C15 O3 Cu1 117.24(16) . .
N1 C10 C11 124.7(2) . .
N1 C10 S3 119.8(2) . .
C11 C10 S3 115.55(19) . .
C12 C11 C10 118.4(2) . .
C12 C11 H11A 120.8 . .
C10 C11 H11A 120.8 . .
C11 C12 C13 118.8(2) . .
C11 C12 H12A 120.6 . .
C13 C12 H12A 120.6 . .
C14 C13 C12 117.8(2) . .
C14 C13 C15 121.0(2) . .
C12 C13 C15 121.1(2) . .
N1 C14 C13 124.6(2) . .
N1 C14 H14A 117.7 . .
C13 C14 H14A 117.7 . .
O4 C15 O3 124.0(2) . .
O4 C15 C13 119.9(2) . .
O3 C15 C13 116.1(2) . .
N2 C20 C21 123.7(2) . .
N2 C20 S2 111.10(18) . .
C21 C20 S2 125.2(2) . .
C22 C21 C20 118.2(2) . .
C22 C21 H21A 120.9 . .
C20 C21 H21A 120.9 . .
C21 C22 C23 119.5(2) . .
C21 C22 H22A 120.2 . .
C23 C22 H22A 120.2 . .
C24 C23 C22 117.7(2) . .
C24 C23 C25 120.9(2) . .
C22 C23 C25 121.4(2) . .
N2 C24 C23 123.9(2) . .
N2 C24 H24A 118.1 . .
C23 C24 H24A 118.1 . .
O2 C25 O1 126.6(2) . .
O2 C25 C23 116.6(2) . .
O1 C25 C23 116.9(2) . .
N3 C30 C31 122.7(2) . .
N3 C30 H30A 118.6 . .
C31 C30 H30A 118.6 . .
C30 C31 C32 119.9(2) . .
C30 C31 H31A 120.1 . .
C32 C31 H31A 120.1 . .
C33 C32 C31 117.1(2) . .
C33 C32 C35 121.5(2) . .
C31 C32 C35 121.4(2) . .
C34 C33 C32 119.6(2) . .
C34 C33 H33A 120.2 . .
C32 C33 H33A 120.2 . .
N3 C34 C33 122.8(2) . .
N3 C34 H34A 118.6 . .
C33 C34 H34A 118.6 . .
C36 C35 C39 116.8(2) . .
C36 C35 C32 120.9(2) . .
C39 C35 C32 122.3(2) . .
C37 C36 C35 120.2(2) . .
C37 C36 H36A 119.9 . .
C35 C36 H36A 119.9 . .
N4 C37 C36 122.9(2) . .
N4 C37 H37A 118.6 . .
C36 C37 H37A 118.6 . .
N4 C38 C39 122.8(2) . .
N4 C38 H38A 118.6 . .
C39 C38 H38A 118.6 . .
C38 C39 C35 119.8(2) . .
C38 C39 H39A 120.1 . .
C35 C39 H39A 120.1 . .
Cu1 O5 H5A 118.8 . .
Cu1 O5 H5B 111.6 . .
H5A O5 H5B 101.1 . .
H7A O7 H7B 107.0 . .
Cu1 O6 H6A 128.1 . .
Cu1 O6 H6B 125.7 . .
H6A O6 H6B 102.2 . .
H10A O102 H10B 114.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O3 1.9463(17) .
Cu1 O6 1.9535(18) .
Cu1 N3 2.011(2) 1_545
Cu1 N4 2.0152(19) .
Cu1 O5 2.2712(18) .
S2 C20 1.778(2) .
S2 S3 2.0203(10) .
S3 C10 1.787(3) .
N1 C10 1.333(3) .
N1 C14 1.342(3) .
N2 C20 1.335(3) .
N2 C24 1.344(3) .
N3 C30 1.333(3) .
N3 C34 1.337(3) .
N3 Cu1 2.0109(19) 1_565
N4 C38 1.341(3) .
N4 C37 1.345(3) .
O1 C25 1.254(3) .
O2 C25 1.253(3) .
O3 C15 1.265(3) .
O4 C15 1.236(3) .
C10 C11 1.381(4) .
C11 C12 1.381(4) .
C11 H11A 0.9500 .
C12 C13 1.391(4) .
C12 H12A 0.9500 .
C13 C14 1.385(4) .
C13 C15 1.490(3) .
C14 H14A 0.9500 .
C20 C21 1.389(4) .
C21 C22 1.382(4) .
C21 H21A 0.9500 .
C22 C23 1.393(4) .
C22 H22A 0.9500 .
C23 C24 1.385(3) .
C23 C25 1.517(3) .
C24 H24A 0.9500 .
C30 C31 1.381(3) .
C30 H30A 0.9500 .
C31 C32 1.392(3) .
C31 H31A 0.9500 .
C32 C33 1.387(3) .
C32 C35 1.486(3) .
C33 C34 1.387(4) .
C33 H33A 0.9500 .
C34 H34A 0.9500 .
C35 C36 1.390(3) .
C35 C39 1.393(3) .
C36 C37 1.376(3) .
C36 H36A 0.9500 .
C37 H37A 0.9500 .
C38 C39 1.386(3) .
C38 H38A 0.9500 .
C39 H39A 0.9500 .
O5 H5A 0.7953 .
O5 H5B 0.8114 .
O7 H7A 0.8044 .
O7 H7B 0.8053 .
O6 H6A 0.8001 .
O6 H6B 0.8000 .
O102 H10A 0.8000 .
O102 H10B 0.8000 .
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
C20 S2 S3 C10 -81.92(13) .
O3 Cu1 N4 C38 77.90(19) .
O6 Cu1 N4 C38 -96.56(19) .
O5 Cu1 N4 C38 161.35(19) .
O3 Cu1 N4 C37 -100.46(19) .
O6 Cu1 N4 C37 85.08(19) .
O5 Cu1 N4 C37 -17.01(19) .
N3 Cu1 O3 C15 87.95(19) 1_545
N4 Cu1 O3 C15 -85.88(19) .
O5 Cu1 O3 C15 176.86(19) .
C14 N1 C10 C11 1.2(4) .
C14 N1 C10 S3 179.8(2) .
S2 S3 C10 N1 6.1(2) .
S2 S3 C10 C11 -175.2(2) .
N1 C10 C11 C12 -0.1(5) .
S3 C10 C11 C12 -178.8(2) .
C10 C11 C12 C13 -1.0(4) .
C11 C12 C13 C14 0.9(4) .
C11 C12 C13 C15 -176.0(3) .
C10 N1 C14 C13 -1.3(4) .
C12 C13 C14 N1 0.3(4) .
C15 C13 C14 N1 177.2(3) .
Cu1 O3 C15 O4 -7.1(4) .
Cu1 O3 C15 C13 171.21(16) .
C14 C13 C15 O4 4.6(4) .
C12 C13 C15 O4 -178.6(3) .
C14 C13 C15 O3 -173.8(2) .
C12 C13 C15 O3 3.0(4) .
C24 N2 C20 C21 -0.3(4) .
C24 N2 C20 S2 -178.39(17) .
S3 S2 C20 N2 -171.86(15) .
S3 S2 C20 C21 10.0(2) .
N2 C20 C21 C22 -0.1(4) .
S2 C20 C21 C22 177.81(19) .
C20 C21 C22 C23 0.2(4) .
C21 C22 C23 C24 0.0(4) .
C21 C22 C23 C25 -178.4(2) .
C20 N2 C24 C23 0.5(4) .
C22 C23 C24 N2 -0.4(4) .
C25 C23 C24 N2 178.1(2) .
C24 C23 C25 O2 11.9(3) .
C22 C23 C25 O2 -169.7(2) .
C24 C23 C25 O1 -168.0(2) .
C22 C23 C25 O1 10.4(3) .
C34 N3 C30 C31 -0.1(4) .
Cu1 N3 C30 C31 179.1(2) 1_565
N3 C30 C31 C32 0.3(4) .
C30 C31 C32 C33 0.0(4) .
C30 C31 C32 C35 178.2(2) .
C31 C32 C33 C34 -0.5(4) .
C35 C32 C33 C34 -178.6(3) .
C30 N3 C34 C33 -0.4(4) .
Cu1 N3 C34 C33 -179.5(2) 1_565
C32 C33 C34 N3 0.7(5) .
C33 C32 C35 C36 160.1(2) .
C31 C32 C35 C36 -18.0(4) .
C33 C32 C35 C39 -18.5(4) .
C31 C32 C35 C39 163.4(2) .
C39 C35 C36 C37 1.0(4) .
C32 C35 C36 C37 -177.7(2) .
C38 N4 C37 C36 -1.3(4) .
Cu1 N4 C37 C36 177.1(2) .
C35 C36 C37 N4 0.4(4) .
C37 N4 C38 C39 0.9(4) .
Cu1 N4 C38 C39 -177.53(18) .
N4 C38 C39 C35 0.5(4) .
C36 C35 C39 C38 -1.4(3) .
C32 C35 C39 C38 177.3(2) .
