#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:02:21 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179948 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/43/7024314.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_7024314
loop_
_publ_author_name
'Delgado, Salomé'
'Santana, Adriano'
'Castillo, Oscar'
'Zamora, Félix'
_publ_section_title
;
 Dynamic combinatorial chemistry in a solvothermal process of Cu(I,II) and
 organosulfur ligands.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2280
_journal_page_last               2287
_journal_paper_doi               10.1039/b914835c
_journal_volume                  39
_journal_year                    2010
_chemical_formula_iupac          '[Cu2(mu-SO4)2(C10H8N2S)2(H2O)2].3H2O'
_chemical_formula_moiety         'C20 H20 Cu2 N4 O10 S4, 3(H2 O)'
_chemical_formula_sum            'C20 H26 Cu2 N4 O13 S4'
_chemical_formula_weight         785.77
_chemical_name_common
;
di-mu-sulphato-k4O,O'-bis(2,2'-dipyridylsulphide-k2N,N')-
dicopper(ii) - water (1
;
_chemical_name_systematic
;
di-mu-sulphato-k4O,O'-bis(2,2'-dipyridylsulphide-k2N,N')-dicopper(II) - water (1/3)
;
_space_group_IT_number           2
_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   geom
_cell_angle_alpha                113.487(4)
_cell_angle_beta                 93.318(4)
_cell_angle_gamma                98.026(4)
_cell_formula_units_Z            1
_cell_length_a                   7.1397(5)
_cell_length_b                   9.3421(9)
_cell_length_c                   11.5895(11)
_cell_measurement_reflns_used    30792
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.70
_cell_measurement_theta_min      1.93
_cell_volume                     696.52(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Sir92 (Altamore et al., 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            30792
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.900
_exptl_absorpt_correction_T_max  0.887
_exptl_absorpt_correction_T_min  0.801
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrysAlis RED (Oxford Diffraction, 2003)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.873
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3563
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0388
_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)+(0.0267P)²+3.1470P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1242
_reflns_number_gt                3413
_reflns_number_total             3563
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b914835c.txt
_cod_data_source_block           compound3
_cod_database_code               7024314
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 0.22280(6) 0.72121(5) 0.16720(4) 0.00821(12) Uani 1 1 d .
S1 S 0.27561(14) 1.09732(11) 0.23206(9) 0.0139(2) Uani 1 1 d .
S2 S -0.14342(12) 0.47641(10) 0.13214(8) 0.00867(18) Uani 1 1 d .
C1 C 0.2610(5) 1.0472(4) 0.3641(3) 0.0118(7) Uani 1 1 d .
C2 C 0.2688(6) 1.1668(5) 0.4834(4) 0.0167(8) Uani 1 1 d .
H2 H 0.2877 1.2749 0.4960 0.020 Uiso 1 1 calc R
C3 C 0.2481(6) 1.1240(5) 0.5846(4) 0.0188(8) Uani 1 1 d .
H3 H 0.2489 1.2026 0.6678 0.023 Uiso 1 1 calc R
C4 C 0.2263(6) 0.9657(5) 0.5627(4) 0.0178(8) Uani 1 1 d .
H4 H 0.2149 0.9345 0.6310 0.021 Uiso 1 1 calc R
C5 C 0.2213(5) 0.8535(5) 0.4411(4) 0.0149(7) Uani 1 1 d .
H5 H 0.2064 0.7448 0.4267 0.018 Uiso 1 1 calc R
C6 C 0.4676(5) 1.0023(4) 0.1682(3) 0.0102(7) Uani 1 1 d .
C7 C 0.6254(5) 1.0903(5) 0.1496(4) 0.0130(7) Uani 1 1 d .
H7 H 0.6335 1.2010 0.1735 0.016 Uiso 1 1 calc R
C8 C 0.7720(5) 1.0142(5) 0.0955(4) 0.0145(7) Uani 1 1 d .
H8 H 0.8813 1.0717 0.0804 0.017 Uiso 1 1 calc R
C9 C 0.7568(5) 0.8525(5) 0.0636(4) 0.0137(7) Uani 1 1 d .
H9 H 0.8564 0.7982 0.0278 0.016 Uiso 1 1 calc R
C10 C 0.5934(5) 0.7720(4) 0.0850(3) 0.0121(7) Uani 1 1 d .
H10 H 0.5825 0.6615 0.0628 0.015 Uiso 1 1 calc R
N1 N 0.2367(4) 0.8928(4) 0.3420(3) 0.0109(6) Uani 1 1 d .
N2 N 0.4501(4) 0.8450(4) 0.1359(3) 0.0095(6) Uani 1 1 d .
O1 O -0.2157(4) 0.4487(3) 0.0006(2) 0.0120(5) Uani 1 1 d .
O2 O -0.0316(4) 0.6415(3) 0.1932(2) 0.0108(5) Uani 1 1 d .
O3 O -0.0242(4) 0.3615(3) 0.1325(3) 0.0132(5) Uani 1 1 d .
O4 O -0.3053(4) 0.4711(3) 0.2030(3) 0.0143(5) Uani 1 1 d .
O1W O 0.3413(4) 0.5522(3) 0.2402(3) 0.0145(5) Uani 1 1 d .
H1A H 0.2628 0.4672 0.2254 0.022 Uiso 1 1 d .
H1B H 0.4531 0.5326 0.2494 0.022 Uiso 1 1 d .
O2W O 0.0533(10) 0.6377(8) 0.6089(6) 0.0258(14) Uiso 0.50 1 d P
O3W O 0.2675(9) 0.5683(8) 0.5540(6) 0.0241(13) Uiso 0.50 1 d P
O4W O 0.3789(10) 0.5373(8) 0.4925(7) 0.0278(14) Uiso 0.50 1 d P
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
O2 Cu1 O1 94.67(11) . 2_565
O2 Cu1 N2 165.43(12) . .
O1 Cu1 N2 89.95(12) 2_565 .
O2 Cu1 N1 86.00(12) . .
O1 Cu1 N1 178.07(12) 2_565 .
N2 Cu1 N1 89.84(13) . .
O2 Cu1 O1W 88.77(11) . .
O1 Cu1 O1W 84.83(11) 2_565 .
N2 Cu1 O1W 105.43(11) . .
N1 Cu1 O1W 93.37(12) . .
C1 S1 C6 99.25(17) . .
O3 S2 O4 111.48(16) . .
O3 S2 O1 111.31(16) . .
O4 S2 O1 109.07(16) . .
O3 S2 O2 110.69(16) . .
O4 S2 O2 107.16(16) . .
O1 S2 O2 106.94(15) . .
N1 C1 C2 123.1(4) . .
N1 C1 S1 117.9(3) . .
C2 C1 S1 119.0(3) . .
C1 C2 C3 117.9(4) . .
C1 C2 H2 121.0 . .
C3 C2 H2 121.0 . .
C4 C3 C2 119.2(4) . .
C4 C3 H3 120.4 . .
C2 C3 H3 120.4 . .
C5 C4 C3 119.4(4) . .
C5 C4 H4 120.3 . .
C3 C4 H4 120.3 . .
N1 C5 C4 122.0(4) . .
N1 C5 H5 119.0 . .
C4 C5 H5 119.0 . .
N2 C6 C7 122.7(3) . .
N2 C6 S1 118.3(3) . .
C7 C6 S1 119.0(3) . .
C6 C7 C8 118.7(4) . .
C6 C7 H7 120.6 . .
C8 C7 H7 120.6 . .
C7 C8 C9 119.1(4) . .
C7 C8 H8 120.4 . .
C9 C8 H8 120.4 . .
C10 C9 C8 118.7(3) . .
C10 C9 H9 120.6 . .
C8 C9 H9 120.6 . .
N2 C10 C9 122.3(3) . .
N2 C10 H10 118.9 . .
C9 C10 H10 118.9 . .
C5 N1 C1 118.3(3) . .
C5 N1 Cu1 119.4(3) . .
C1 N1 Cu1 122.3(3) . .
C10 N2 C6 118.4(3) . .
C10 N2 Cu1 119.6(3) . .
C6 N2 Cu1 121.9(3) . .
S2 O1 Cu1 135.12(17) . 2_565
S2 O2 Cu1 128.71(16) . .
Cu1 O1W H1A 114.0 . .
Cu1 O1W H1B 133.0 . .
H1A O1W H1B 107.0 . .
O4W O3W O2W 158.8(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O2 1.952(3) .
Cu1 O1 1.952(3) 2_565
Cu1 N2 1.995(3) .
Cu1 N1 2.006(3) .
Cu1 O1W 2.298(3) .
S1 C1 1.774(4) .
S1 C6 1.775(4) .
S2 O3 1.461(3) .
S2 O4 1.463(3) .
S2 O1 1.488(3) .
S2 O2 1.496(3) .
C1 N1 1.345(5) .
C1 C2 1.380(5) .
C2 C3 1.391(6) .
C2 H2 0.9500 .
C3 C4 1.381(6) .
C3 H3 0.9500 .
C4 C5 1.376(5) .
C4 H4 0.9500 .
C5 N1 1.344(5) .
C5 H5 0.9500 .
C6 N2 1.349(5) .
C6 C7 1.379(5) .
C7 C8 1.387(6) .
C7 H7 0.9500 .
C8 C9 1.391(6) .
C8 H8 0.9500 .
C9 C10 1.387(5) .
C9 H9 0.9500 .
C10 N2 1.344(5) .
C10 H10 0.9500 .
O1 Cu1 1.952(3) 2_565
O1W H1A 0.8539 .
O1W H1B 0.8534 .
O2W O3W 1.796(10) .
O3W O4W 1.091(9) .
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
_geom_torsion_site_symmetry_4
C6 S1 C1 N1 -56.0(3) . .
C6 S1 C1 C2 126.0(3) . .
N1 C1 C2 C3 -0.8(6) . .
S1 C1 C2 C3 177.0(3) . .
C1 C2 C3 C4 1.8(6) . .
C2 C3 C4 C5 -1.4(6) . .
C3 C4 C5 N1 -0.1(6) . .
C1 S1 C6 N2 57.5(3) . .
C1 S1 C6 C7 -124.5(3) . .
N2 C6 C7 C8 0.1(6) . .
S1 C6 C7 C8 -177.7(3) . .
C6 C7 C8 C9 -1.1(6) . .
C7 C8 C9 C10 1.2(6) . .
C8 C9 C10 N2 -0.3(6) . .
C4 C5 N1 C1 1.2(6) . .
C4 C5 N1 Cu1 -178.8(3) . .
C2 C1 N1 C5 -0.7(6) . .
S1 C1 N1 C5 -178.6(3) . .
C2 C1 N1 Cu1 179.3(3) . .
S1 C1 N1 Cu1 1.4(4) . .
O2 Cu1 N1 C5 60.2(3) . .
N2 Cu1 N1 C5 -133.8(3) . .
O1W Cu1 N1 C5 -28.3(3) . .
O2 Cu1 N1 C1 -119.8(3) . .
N2 Cu1 N1 C1 46.2(3) . .
O1W Cu1 N1 C1 151.7(3) . .
C9 C10 N2 C6 -0.6(5) . .
C9 C10 N2 Cu1 -178.6(3) . .
C7 C6 N2 C10 0.7(5) . .
S1 C6 N2 C10 178.6(3) . .
C7 C6 N2 Cu1 178.6(3) . .
S1 C6 N2 Cu1 -3.5(4) . .
O2 Cu1 N2 C10 -153.7(4) . .
O1 Cu1 N2 C10 -45.0(3) 2_565 .
N1 Cu1 N2 C10 133.1(3) . .
O1W Cu1 N2 C10 39.6(3) . .
O2 Cu1 N2 C6 28.4(6) . .
O1 Cu1 N2 C6 137.1(3) 2_565 .
N1 Cu1 N2 C6 -44.8(3) . .
O1W Cu1 N2 C6 -138.3(3) . .
O3 S2 O1 Cu1 11.8(3) . 2_565
O4 S2 O1 Cu1 -111.6(2) . 2_565
O2 S2 O1 Cu1 132.8(2) . 2_565
O3 S2 O2 Cu1 46.1(3) . .
O4 S2 O2 Cu1 167.9(2) . .
O1 S2 O2 Cu1 -75.3(2) . .
O1 Cu1 O2 S2 23.0(2) 2_565 .
N2 Cu1 O2 S2 131.1(4) . .
N1 Cu1 O2 S2 -155.2(2) . .
O1W Cu1 O2 S2 -61.7(2) . .
