#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:24:39 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179326 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/23/4322313.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_4322313
loop_
_publ_author_name
'Isabel Castro'
'María Luisa Calatayud'
'Jorunn Sletten'
'Francesc Lloret'
'Juan Cano'
'Miguel Julve'
'Gunther Seitz'
'Klaus Mann'
_publ_section_title
;
 Ferro- and Antiferromagnetic Coupling through 1,n-Dithiosquarate Bridges
 (n= 2, 3) in Copper(II) Dimers. Syntheses, Crystal Structures, and
 Magnetic Properties of [Cu2(bpca)2(1,2-dtsq)(H2O)].2H2O and
 [Cu2(bpca)2(1,3-dtsq)].2H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4680
_journal_page_last               4687
_journal_paper_doi               10.1021/ic9904384
_journal_volume                  38
_journal_year                    1999
_chemical_formula_moiety         'C28 H20 Cu2 N6 O8 S2'
_chemical_formula_sum            'C28 H20 Cu2 N6 O8 S2'
_chemical_formula_weight         759.70
_chemical_name_systematic
; 
 ? 
;
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.02(2)
_cell_angle_beta                 97.40(2)
_cell_angle_gamma                110.27(2)
_cell_formula_units_Z            1
_cell_length_a                   7.656(2)
_cell_length_b                   9.351(3)
_cell_length_c                   11.587(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      19
_cell_measurement_theta_min      15
_cell_volume                     707.8(4)
_computing_cell_refinement       'Enraf-Nonius CAD4 EXPRESS'
_computing_data_collection       'Enraf-Nonius CAD4 EXPRESS'
_computing_data_reduction        XCAD
_computing_molecular_graphics    'XP Version 4.3'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_detector_area_resol_mean '2\q = 50 deg'
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       'ω/2θ scan'
_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  0.0527
_diffrn_reflns_av_sigmaI/netI    0.0736
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2752
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.99
_diffrn_standards_decay_%        8
_diffrn_standards_interval_time  '10800 sec'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.715
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_correction_T_min  0.488
_exptl_absorpt_correction_type   'empirical, \y-scan measurements'
_exptl_crystal_colour            'yellowish green'
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rods
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.026
_refine_diff_density_max         1.990
_refine_diff_density_min         -2.518
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         2381
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.1271
_refine_ls_R_factor_gt           0.0900
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1636P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2133
_refine_ls_wR_factor_ref         0.2381
_reflns_number_gt                1684
_reflns_number_total             2381
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9904384_2.cif
_cod_data_source_block           cu13dtsq
_cod_original_cell_volume        707.8(3)
_cod_database_code               4322313
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
Cu Cu 0.00088(16) 0.20816(13) 0.20613(9) 0.0288(4) Uani 1 1 d . . .
S S 0.1868(3) 0.4916(3) 0.3175(2) 0.0331(6) Uani 1 1 d . . .
O1 O -0.3229(12) -0.2218(9) -0.0959(7) 0.054(2) Uani 1 1 d . . .
O2 O -0.1903(13) -0.2851(9) 0.1189(8) 0.064(2) Uani 1 1 d . . .
O3 O -0.2079(10) 0.2386(8) 0.3639(6) 0.0395(16) Uani 1 1 d . . .
O41 O -0.341(2) -0.481(2) 0.2763(15) 0.052(4) Uiso 0.55 1 d P . .
O42 O -0.395(5) -0.452(5) 0.241(3) 0.116(11) Uiso 0.44 1 d P . .
N1 N -0.1625(11) 0.2128(10) 0.0579(6) 0.0328(18) Uani 1 1 d . . .
N2 N -0.1372(11) -0.0324(9) 0.1066(7) 0.0331(18) Uani 1 1 d . . .
N3 N 0.1299(11) 0.1305(9) 0.3229(7) 0.0299(17) Uani 1 1 d . . .
C1 C -0.1746(15) 0.3480(13) 0.0445(10) 0.041(2) Uani 1 1 d . . .
H1 H -0.0956 0.4533 0.1063 0.050 Uiso 1 1 d R . .
C2 C -0.3035(16) 0.3313(15) -0.0608(11) 0.048(3) Uani 1 1 d . . .
H2 H -0.3140 0.4244 -0.0680 0.058 Uiso 1 1 d R . .
C3 C -0.4125(16) 0.1762(16) -0.1531(10) 0.050(3) Uani 1 1 d . . .
H3 H -0.4972 0.1637 -0.2245 0.060 Uiso 1 1 d R . .
C4 C -0.3999(15) 0.0366(15) -0.1413(9) 0.047(3) Uani 1 1 d . . .
H4 H -0.4750 -0.0697 -0.2030 0.057 Uiso 1 1 d R . .
C5 C -0.2718(13) 0.0624(12) -0.0339(8) 0.032(2) Uani 1 1 d . . .
C6 C -0.2479(13) -0.0809(12) -0.0126(8) 0.035(2) Uani 1 1 d . . .
C7 C -0.1073(14) -0.1332(11) 0.1599(9) 0.034(2) Uani 1 1 d . . .
C8 C 0.0431(14) -0.0374(11) 0.2854(8) 0.032(2) Uani 1 1 d . . .
C9 C 0.1008(15) -0.1136(12) 0.3561(11) 0.043(2) Uani 1 1 d . . .
H9 H 0.0418 -0.2286 0.3281 0.051 Uiso 1 1 d R . .
C10 C 0.2458(16) -0.0206(15) 0.4692(12) 0.050(3) Uani 1 1 d . . .
H10 H 0.2836 -0.0710 0.5189 0.061 Uiso 1 1 d R . .
C11 C 0.3311(17) 0.1469(15) 0.5031(10) 0.050(3) Uani 1 1 d . . .
H11 H 0.4310 0.2139 0.5774 0.060 Uiso 1 1 d R . .
C12 C 0.2684(16) 0.2178(13) 0.4288(9) 0.043(2) Uani 1 1 d . . .
H12 H 0.3277 0.3325 0.4544 0.052 Uiso 1 1 d R . .
C13 C 0.0725(13) 0.5022(11) 0.4333(8) 0.030(2) Uani 1 1 d . . .
C14 C -0.0966(12) 0.3816(10) 0.4385(8) 0.0284(19) Uani 1 1 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'
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
_geom_angle_publ_flag
N2 Cu N1 81.5(3) . . ?
N2 Cu N3 81.6(3) . . ?
N1 Cu N3 163.0(3) . . ?
N2 Cu S 175.1(2) . . ?
N1 Cu S 99.4(2) . . ?
N3 Cu S 97.3(2) . . ?
N2 Cu O3 98.4(3) . . ?
N1 Cu O3 100.0(3) . . ?
N3 Cu O3 84.1(3) . . ?
S Cu O3 86.20(16) . . ?
N2 Cu O1 91.5(3) . 2 ?
N1 Cu O1 94.3(3) . 2 ?
N3 Cu O1 84.5(3) . 2 ?
S Cu O1 83.65(15) . 2 ?
O3 Cu O1 163.6(2) . 2 ?
C13 S Cu 93.0(3) . . ?
C6 O1 Cu 98.1(6) . 2 ?
C14 O3 Cu 96.4(6) . . ?
C5 N1 C1 118.9(8) . . ?
C5 N1 Cu 113.8(7) . . ?
C1 N1 Cu 127.3(6) . . ?
C7 N2 C6 126.2(8) . . ?
C7 N2 Cu 117.4(6) . . ?
C6 N2 Cu 116.3(6) . . ?
C12 N3 C8 118.4(8) . . ?
C12 N3 Cu 129.6(7) . . ?
C8 N3 Cu 111.8(6) . . ?
N1 C1 C2 120.9(9) . . ?
N1 C1 H1 119.5 . . ?
C2 C1 H1 119.6 . . ?
C3 C2 C1 118.7(11) . . ?
C3 C2 H2 120.9 . . ?
C1 C2 H2 120.4 . . ?
C2 C3 C4 120.9(10) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 117.1(10) . . ?
C5 C4 H4 121.4 . . ?
C3 C4 H4 121.5 . . ?
N1 C5 C4 123.4(10) . . ?
N1 C5 C6 115.6(8) . . ?
C4 C5 C6 121.0(9) . . ?
O1 C6 N2 126.7(10) . . ?
O1 C6 C5 121.6(9) . . ?
N2 C6 C5 111.8(8) . . ?
O2 C7 N2 127.7(9) . . ?
O2 C7 C8 120.3(9) . . ?
N2 C7 C8 111.9(8) . . ?
N3 C8 C9 120.9(9) . . ?
N3 C8 C7 116.5(8) . . ?
C9 C8 C7 122.5(9) . . ?
C8 C9 C10 120.6(9) . . ?
C8 C9 H9 119.7 . . ?
C10 C9 H9 119.7 . . ?
C11 C10 C9 116.9(10) . . ?
C11 C10 H10 121.9 . . ?
C9 C10 H10 121.2 . . ?
C10 C11 C12 120.4(11) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
N3 C12 C11 122.7(10) . . ?
N3 C12 H12 118.4 . . ?
C11 C12 H12 118.8 . . ?
C14 C13 C14 91.2(7) . 2_566 ?
C14 C13 S 129.7(7) . . ?
C14 C13 S 139.1(7) 2_566 . ?
O3 C14 C13 133.2(8) . . ?
O3 C14 C13 138.0(9) . 2_566 ?
C13 C14 C13 88.8(7) . 2_566 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu N2 1.963(7) . ?
Cu N1 2.012(7) . ?
Cu N3 2.032(8) . ?
Cu S 2.324(3) . ?
Cu O3 2.590(7) . ?
Cu O1 2.903(8) 2 ?
S C13 1.688(9) . ?
O1 C6 1.225(12) . ?
O1 Cu 2.903(8) 2 ?
O2 C7 1.226(12) . ?
O3 C14 1.236(11) . ?
N1 C5 1.338(12) . ?
N1 C1 1.355(13) . ?
N2 C7 1.347(12) . ?
N2 C6 1.362(12) . ?
N3 C12 1.308(13) . ?
N3 C8 1.362(12) . ?
C1 C2 1.395(15) . ?
C1 H1 0.9300 . ?
C2 C3 1.365(17) . ?
C2 H2 0.9299 . ?
C3 C4 1.390(17) . ?
C3 H3 0.9300 . ?
C4 C5 1.376(14) . ?
C4 H4 0.9300 . ?
C5 C6 1.504(14) . ?
C7 C8 1.500(14) . ?
C8 C9 1.370(14) . ?
C9 C10 1.386(16) . ?
C9 H9 0.9299 . ?
C10 C11 1.363(16) . ?
C10 H10 0.9301 . ?
C11 C12 1.377(14) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.416(13) . ?
C13 C14 1.470(11) 2_566 ?
C14 C13 1.470(11) 2_566 ?
