#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:43:56 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179933 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/28/7022853.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_7022853
loop_
_publ_author_name
'Hu, Sheng'
'Yu, Fang-Yong'
'Zhang, Peng'
'Lin, Dian-Rong'
_publ_section_title
;
 In situ amination and side group effect of multifunctional heterocyclic
 thione ligand toward discrete and polymeric cluster constructions.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7731
_journal_page_last               7740
_journal_paper_doi               10.1039/c3dt50165e
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C18 H15 Cu N8 S4'
_chemical_formula_weight         535.16
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.330(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1491(6)
_cell_length_b                   10.3660(4)
_cell_length_c                   17.8580(9)
_cell_measurement_temperature    293(2)
_cell_volume                     2042.10(17)
_computing_cell_refinement       'SAINT-PLUS, Ver. 6.0, 1997'
_computing_data_collection       'SMART, 1998.'
_computing_data_reduction        'SAINT-PLUS, Ver. 6.0, 1997'
_computing_molecular_graphics    'XP, Ver. 6.10, Bruker AXS Inc., 2000'
_computing_publication_material  'SHELXTL-Bruker AXS Inc., 1998'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7115
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    1.505
_exptl_absorpt_correction_T_max  0.7840
_exptl_absorpt_correction_T_min  0.6694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         1984
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0342
_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)+(0.0302P)²+4.9655P] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0812
_reflns_number_gt                1672
_reflns_number_total             1984
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50165e.txt
_cod_data_source_block           complex2
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7022853
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.0000 0.80259(5) 0.7500 0.03255(16) Uani 1 2 d S . .
S1 S -0.17154(7) 0.70422(8) 0.77486(4) 0.0351(2) Uani 1 1 d . . .
S2 S -0.55473(6) 0.45559(7) 0.64618(4) 0.02678(17) Uani 1 1 d . . .
N1 N -0.3493(2) 0.5741(2) 0.69833(13) 0.0288(5) Uani 1 1 d . . .
H1 H -0.3726 0.5653 0.7419 0.035 Uiso 1 1 calc R . .
N2 N -0.38105(19) 0.5368(2) 0.57003(13) 0.0263(5) Uani 1 1 d . . .
H2 H -0.4250 0.5114 0.5291 0.032 Uiso 0.50 1 calc PR A -1
N3 N -0.19854(19) 0.6406(2) 0.62812(13) 0.0255(5) Uani 1 1 d . . .
N4 N -0.2318(2) 0.5859(2) 0.50010(13) 0.0288(5) Uani 1 1 d . . .
H4 H -0.2849 0.5556 0.4648 0.035 Uiso 1 1 calc R . .
C1 C -0.2407(2) 0.6363(3) 0.69415(15) 0.0243(6) Uani 1 1 d . . .
C2 C -0.4207(2) 0.5264(2) 0.63656(15) 0.0232(5) Uani 1 1 d . . .
C3 C -0.2675(2) 0.5895(2) 0.56813(15) 0.0236(5) Uani 1 1 d . . .
C4 C -0.1206(2) 0.6237(3) 0.47564(16) 0.0265(6) Uani 1 1 d . . .
C5 C -0.0235(3) 0.6790(3) 0.52158(18) 0.0332(7) Uani 1 1 d . . .
H5 H -0.0270 0.6934 0.5726 0.040 Uiso 1 1 calc R . .
C6 C 0.0792(3) 0.7124(3) 0.4903(2) 0.0423(8) Uani 1 1 d . . .
H6 H 0.1444 0.7501 0.5209 0.051 Uiso 1 1 calc R . .
C7 C 0.0867(3) 0.6911(3) 0.4149(2) 0.0429(8) Uani 1 1 d . . .
H7 H 0.1558 0.7149 0.3947 0.052 Uiso 1 1 calc R . .
C8 C -0.0091(3) 0.6344(4) 0.3702(2) 0.0479(9) Uani 1 1 d . . .
H8 H -0.0043 0.6181 0.3195 0.057 Uiso 1 1 calc R . .
C9 C -0.1133(3) 0.6010(3) 0.39975(18) 0.0392(7) Uani 1 1 d . . .
H9 H -0.1782 0.5635 0.3688 0.047 Uiso 1 1 calc R . .
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'
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
S1 Cu1 S1 126.55(5) . 2_556
S1 Cu1 S2 105.53(3) . 4_456
S1 Cu1 S2 108.35(3) 2_556 4_456
S1 Cu1 S2 108.35(3) . 3
S1 Cu1 S2 105.53(3) 2_556 3
S2 Cu1 S2 99.27(4) 4_456 3
C1 S1 Cu1 108.33(9) . .
C2 S2 Cu1 103.33(9) . 3_445
C2 N1 C1 122.8(2) . .
C2 N1 H1 118.6 . .
C1 N1 H1 118.6 . .
C2 N2 C3 118.5(2) . .
C2 N2 H2 120.7 . .
C3 N2 H2 120.7 . .
C1 N3 C3 117.5(2) . .
C3 N4 C4 131.2(2) . .
C3 N4 H4 114.4 . .
C4 N4 H4 114.4 . .
N3 C1 N1 119.1(2) . .
N3 C1 S1 124.5(2) . .
N1 C1 S1 116.3(2) . .
N2 C2 N1 117.7(2) . .
N2 C2 S2 122.5(2) . .
N1 C2 S2 119.8(2) . .
N4 C3 N3 121.9(2) . .
N4 C3 N2 114.0(2) . .
N3 C3 N2 124.0(2) . .
C5 C4 C9 119.8(3) . .
C5 C4 N4 124.9(3) . .
C9 C4 N4 115.4(3) . .
C4 C5 C6 119.0(3) . .
C4 C5 H5 120.5 . .
C6 C5 H5 120.5 . .
C7 C6 C5 121.5(3) . .
C7 C6 H6 119.2 . .
C5 C6 H6 119.2 . .
C8 C7 C6 119.0(3) . .
C8 C7 H7 120.5 . .
C6 C7 H7 120.5 . .
C7 C8 C9 120.6(3) . .
C7 C8 H8 119.7 . .
C9 C8 H8 119.7 . .
C8 C9 C4 120.0(3) . .
C8 C9 H9 120.0 . .
C4 C9 H9 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 S1 2.2672(7) .
Cu1 S1 2.2672(7) 2_556
Cu1 S2 2.4489(8) 4_456
Cu1 S2 2.4489(8) 3
S1 C1 1.687(3) .
S2 C2 1.696(3) .
S2 Cu1 2.4489(8) 3_445
N1 C2 1.356(3) .
N1 C1 1.384(3) .
N1 H1 0.8600 .
N2 C2 1.331(3) .
N2 C3 1.383(3) .
N2 H2 0.8600 .
N3 C1 1.332(3) .
N3 C3 1.334(3) .
N4 C3 1.333(4) .
N4 C4 1.427(3) .
N4 H4 0.8600 .
C4 C5 1.384(4) .
C4 C9 1.389(4) .
C5 C6 1.389(4) .
C5 H5 0.9300 .
C6 C7 1.379(5) .
C6 H6 0.9300 .
C7 C8 1.371(5) .
C7 H7 0.9300 .
C8 C9 1.388(5) .
C8 H8 0.9300 .
C9 H9 0.9300 .
