#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:29:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179181 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/29/4312949.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_4312949
loop_
_publ_author_name
'Miao Du'
'Xian-He Bu'
'Zheng Huang'
'Shen-Tan Chen'
'Ya-Mei Guo'
'Carmen Diaz'
'Joan Ribas'
_publ_contact_author
; Xian-He Bu
  Department of Chemistry, Nankai University, Tianjin 300071,China
;
_publ_contact_author_email       buxh@nankai.edu.cn
_publ_section_title
;
 From Metallacyclophanes to 1-D Coordination Polymers: Role of Anions in
 Self-Assembly Processes of Copper(II) and
 2,5-Bis(3-pyridyl)-1,3,4-oxadiazole
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              552
_journal_page_last               559
_journal_paper_doi               10.1021/ic025851h
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C24 H40 Cu2 N8 O22 S2'
_chemical_formula_weight         983.84
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.511(6)
_cell_angle_beta                 105.265(6)
_cell_angle_gamma                94.042(6)
_cell_formula_units_Z            1
_cell_length_a                   7.078(3)
_cell_length_b                   11.565(4)
_cell_length_c                   12.561(5)
_cell_measurement_temperature    293(2)
_cell_volume                     920.7(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0752
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3806
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    1.368
_exptl_absorpt_correction_T_max  0.8211
_exptl_absorpt_correction_T_min  0.7715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            bluish-green
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             506
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         3233
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0600P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1194
_reflns_number_gt                2113
_reflns_number_total             3233
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025851h-2_s2_3.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN'
changed to 'multi-scan' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4312949
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 1.5000 0.5000 0.5000 0.0267(2) Uani 1 2 d S . .
Cu2 Cu 0.5000 0.5000 0.0000 0.0281(2) Uani 1 2 d S . .
N1 N 0.4708(6) 0.6508(4) 0.1316(3) 0.0290(9) Uani 1 1 d . . .
N2 N 0.7815(6) 0.9348(4) 0.5368(4) 0.0401(11) Uani 1 1 d . . .
N3 N 0.9692(6) 0.9442(4) 0.6159(4) 0.0394(11) Uani 1 1 d . . .
N4 N 1.4591(6) 0.6757(4) 0.5778(3) 0.0289(9) Uani 1 1 d . . .
O1 O 0.9340(5) 0.7910(3) 0.4464(3) 0.0305(8) Uani 1 1 d . . .
O2 O 1.2285(5) 0.4291(3) 0.4908(3) 0.0314(8) Uani 1 1 d D . .
O3 O 1.3862(5) 0.5053(4) 0.3061(3) 0.0386(9) Uani 1 1 d D . .
O4 O 0.2297(5) 0.4257(4) -0.0220(3) 0.0381(9) Uani 1 1 d D . .
C1 C 0.3008(7) 0.6950(5) 0.1246(4) 0.0345(12) Uani 1 1 d . . .
H1A H 0.1973 0.6618 0.0537 0.041 Uiso 1 1 calc R . .
C2 C 0.2733(7) 0.7880(5) 0.2187(5) 0.0382(13) Uani 1 1 d . . .
H2A H 0.1524 0.8163 0.2112 0.046 Uiso 1 1 calc R . .
C3 C 0.4242(7) 0.8387(5) 0.3230(5) 0.0371(13) Uani 1 1 d . . .
H3A H 0.4079 0.9015 0.3875 0.045 Uiso 1 1 calc R . .
C4 C 0.6027(7) 0.7943(4) 0.3307(4) 0.0276(11) Uani 1 1 d . . .
C5 C 0.6198(7) 0.7009(4) 0.2337(4) 0.0275(11) Uani 1 1 d . . .
H5A H 0.7393 0.6712 0.2390 0.033 Uiso 1 1 calc R . .
C6 C 0.7674(7) 0.8435(4) 0.4397(4) 0.0297(11) Uani 1 1 d . . .
C7 C 1.0510(7) 0.8582(4) 0.5602(4) 0.0300(11) Uani 1 1 d . . .
C8 C 1.2430(7) 0.8257(4) 0.6014(4) 0.0293(11) Uani 1 1 d . . .
C9 C 1.3829(8) 0.9036(5) 0.7069(4) 0.0375(13) Uani 1 1 d . . .
H9A H 1.3561 0.9791 0.7516 0.045 Uiso 1 1 calc R . .
C10 C 1.5600(8) 0.8675(5) 0.7437(5) 0.0394(13) Uani 1 1 d . . .
H10A H 1.6574 0.9196 0.8124 0.047 Uiso 1 1 calc R . .
C11 C 1.5938(7) 0.7535(5) 0.6787(4) 0.0338(12) Uani 1 1 d . . .
H11A H 1.7143 0.7294 0.7055 0.041 Uiso 1 1 calc R . .
C12 C 1.2891(7) 0.7125(4) 0.5389(4) 0.0271(11) Uani 1 1 d . . .
H12A H 1.1975 0.6608 0.4674 0.032 Uiso 1 1 calc R . .
S1 S 0.14699(18) 0.59316(12) 0.79442(11) 0.0293(3) Uani 1 1 d . . .
O5 O 0.3533(5) 0.5826(3) 0.8442(3) 0.0356(8) Uani 1 1 d . . .
O6 O 0.1149(6) 0.7200(4) 0.8442(4) 0.0599(12) Uani 1 1 d . . .
O7 O 0.0143(5) 0.5101(4) 0.8204(3) 0.0483(10) Uani 1 1 d . . .
O8 O 0.0965(5) 0.5556(4) 0.6645(3) 0.0506(11) Uani 1 1 d . . .
O9 O 0.5120(8) 0.1176(4) -0.0087(4) 0.0817(15) Uani 1 1 d . . .
O10 O 0.0459(11) 0.9729(8) 0.8677(8) 0.176(3) Uani 1 1 d . . .
O11 O 0.1345(6) 0.2168(4) 1.0080(5) 0.0764(14) Uani 1 1 d . . .
H1 H 1.201(6) 0.464(4) 0.5595(18) 0.045(16) Uiso 1 1 d D . .
H2 H 1.128(5) 0.427(5) 0.428(2) 0.06(2) Uiso 1 1 d D . .
H3 H 1.460(5) 0.466(5) 0.262(3) 0.056(19) Uiso 1 1 d D . .
H4 H 1.259(3) 0.500(5) 0.264(3) 0.047(17) Uiso 1 1 d D . .
H5 H 0.139(6) 0.444(4) -0.076(4) 0.058(19) Uiso 1 1 d D . .
H6 H 0.196(7) 0.351(2) -0.019(4) 0.050(18) 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'
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
O2 Cu1 O2 180.0 . 2_866 ?
O2 Cu1 N4 88.11(15) . 2_866 ?
O2 Cu1 N4 91.89(14) 2_866 2_866 ?
O2 Cu1 N4 91.89(14) . . ?
O2 Cu1 N4 88.11(15) 2_866 . ?
N4 Cu1 N4 180.000(1) 2_866 . ?
O2 Cu1 O3 87.82(14) . 2_866 ?
O2 Cu1 O3 92.18(14) 2_866 2_866 ?
N4 Cu1 O3 92.99(14) 2_866 2_866 ?
N4 Cu1 O3 87.01(14) . 2_866 ?
O2 Cu1 O3 92.18(14) . . ?
O2 Cu1 O3 87.82(13) 2_866 . ?
N4 Cu1 O3 87.01(14) 2_866 . ?
N4 Cu1 O3 92.99(14) . . ?
O3 Cu1 O3 180.000(1) 2_866 . ?
O4 Cu2 O4 180.0(2) . 2_665 ?
O4 Cu2 N1 88.33(15) . . ?
O4 Cu2 N1 91.67(15) 2_665 . ?
O4 Cu2 N1 91.67(15) . 2_665 ?
O4 Cu2 N1 88.33(15) 2_665 2_665 ?
N1 Cu2 N1 180.0 . 2_665 ?
O5 Cu2 N1 92.95(15) 1_554 . ?
O5 Cu2 N1 87.12(15) 1_554 2_665 ?
O5 Cu2 O4 87.14(15) 1_554 . ?
O5 Cu2 O4 92.90(15) 1_554 2_665 ?
C1 N1 C5 118.3(4) . . ?
C1 N1 Cu2 122.1(3) . . ?
C5 N1 Cu2 119.4(3) . . ?
C6 N2 N3 106.4(4) . . ?
C7 N3 N2 106.2(4) . . ?
C12 N4 C11 118.2(4) . . ?
C12 N4 Cu1 121.0(3) . . ?
C11 N4 Cu1 120.3(3) . . ?
C6 O1 C7 102.5(3) . . ?
Cu1 O2 H1 112(3) . . ?
Cu1 O2 H2 116(3) . . ?
H1 O2 H2 111.9(17) . . ?
Cu1 O3 H3 110(3) . . ?
Cu1 O3 H4 127(3) . . ?
H3 O3 H4 113.5(17) . . ?
Cu2 O4 H5 112(3) . . ?
Cu2 O4 H6 125(3) . . ?
H5 O4 H6 113.5(18) . . ?
N1 C1 C2 122.2(5) . . ?
N1 C1 H1A 118.9 . . ?
C2 C1 H1A 118.9 . . ?
C3 C2 C1 119.7(4) . . ?
C3 C2 H2A 120.2 . . ?
C1 C2 H2A 120.2 . . ?
C2 C3 C4 118.5(4) . . ?
C2 C3 H3A 120.7 . . ?
C4 C3 H3A 120.7 . . ?
C5 C4 C3 118.8(4) . . ?
C5 C4 C6 120.2(4) . . ?
C3 C4 C6 121.0(4) . . ?
N1 C5 C4 122.5(4) . . ?
N1 C5 H5A 118.7 . . ?
C4 C5 H5A 118.7 . . ?
N2 C6 O1 112.3(4) . . ?
N2 C6 C4 128.6(4) . . ?
O1 C6 C4 119.1(4) . . ?
N3 C7 O1 112.6(4) . . ?
N3 C7 C8 128.9(4) . . ?
O1 C7 C8 118.4(4) . . ?
C9 C8 C12 118.3(4) . . ?
C9 C8 C7 121.0(4) . . ?
C12 C8 C7 120.6(4) . . ?
C10 C9 C8 118.8(5) . . ?
C10 C9 H9A 120.6 . . ?
C8 C9 H9A 120.6 . . ?
C9 C10 C11 119.7(5) . . ?
C9 C10 H10A 120.2 . . ?
C11 C10 H10A 120.2 . . ?
N4 C11 C10 122.5(5) . . ?
N4 C11 H11A 118.8 . . ?
C10 C11 H11A 118.8 . . ?
N4 C12 C8 122.5(4) . . ?
N4 C12 H12A 118.8 . . ?
C8 C12 H12A 118.8 . . ?
O6 S1 O5 110.9(2) . . ?
O6 S1 O7 109.1(2) . . ?
O5 S1 O7 109.5(2) . . ?
O6 S1 O8 108.9(2) . . ?
O5 S1 O8 110.0(2) . . ?
O7 S1 O8 108.4(2) . . ?
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
Cu1 O2 1.994(3) . ?
Cu1 O2 1.994(3) 2_866 ?
Cu1 N4 2.018(4) 2_866 ?
Cu1 N4 2.018(4) . ?
Cu1 O3 2.379(4) 2_866 ?
Cu1 O3 2.379(4) . ?
Cu2 O4 1.951(3) . ?
Cu2 O4 1.951(3) 2_665 ?
Cu2 N1 2.030(4) . ?
Cu2 N1 2.030(4) 2_665 ?
Cu2 O5 2.478(3) 1_554 ?
N1 C1 1.333(6) . ?
N1 C5 1.341(6) . ?
N2 C6 1.294(6) . ?
N2 N3 1.406(5) . ?
N3 C7 1.282(6) . ?
N4 C12 1.330(6) . ?
N4 C11 1.344(6) . ?
O1 C6 1.360(5) . ?
O1 C7 1.370(5) . ?
O2 H1 0.900(10) . ?
O2 H2 0.903(10) . ?
O3 H3 0.896(10) . ?
O3 H4 0.898(10) . ?
O4 H5 0.895(10) . ?
O4 H6 0.900(10) . ?
C1 C2 1.376(7) . ?
C1 H1A 0.9300 . ?
C2 C3 1.366(7) . ?
C2 H2A 0.9300 . ?
C3 C4 1.389(6) . ?
C3 H3A 0.9300 . ?
C4 C5 1.372(6) . ?
C4 C6 1.450(6) . ?
C5 H5A 0.9300 . ?
C7 C8 1.445(6) . ?
C8 C9 1.391(6) . ?
C8 C12 1.395(6) . ?
C9 C10 1.363(7) . ?
C9 H9A 0.9300 . ?
C10 C11 1.374(7) . ?
C10 H10A 0.9300 . ?
C11 H11A 0.9300 . ?
C12 H12A 0.9300 . ?
S1 O6 1.450(4) . ?
S1 O5 1.460(3) . ?
S1 O7 1.468(4) . ?
S1 O8 1.476(4) . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 Cu2 N1 C1 -38.1(4) . . . . ?
O4 Cu2 N1 C1 141.9(4) 2_665 . . . ?
N1 Cu2 N1 C1 85(100) 2_665 . . . ?
O4 Cu2 N1 C5 135.4(4) . . . . ?
O4 Cu2 N1 C5 -44.6(4) 2_665 . . . ?
N1 Cu2 N1 C5 -101(100) 2_665 . . . ?
C6 N2 N3 C7 -0.3(6) . . . . ?
O2 Cu1 N4 C12 -43.3(4) . . . . ?
O2 Cu1 N4 C12 136.7(4) 2_866 . . . ?
N4 Cu1 N4 C12 107(100) 2_866 . . . ?
O3 Cu1 N4 C12 -131.1(4) 2_866 . . . ?
O3 Cu1 N4 C12 48.9(4) . . . . ?
O2 Cu1 N4 C11 128.6(4) . . . . ?
O2 Cu1 N4 C11 -51.4(4) 2_866 . . . ?
N4 Cu1 N4 C11 -81(100) 2_866 . . . ?
O3 Cu1 N4 C11 40.9(4) 2_866 . . . ?
O3 Cu1 N4 C11 -139.1(4) . . . . ?
C5 N1 C1 C2 -1.0(8) . . . . ?
Cu2 N1 C1 C2 172.5(4) . . . . ?
N1 C1 C2 C3 0.6(8) . . . . ?
C1 C2 C3 C4 0.2(8) . . . . ?
C2 C3 C4 C5 -0.5(7) . . . . ?
C2 C3 C4 C6 -179.3(5) . . . . ?
C1 N1 C5 C4 0.7(7) . . . . ?
Cu2 N1 C5 C4 -173.0(4) . . . . ?
C3 C4 C5 N1 0.0(7) . . . . ?
C6 C4 C5 N1 178.8(4) . . . . ?
N3 N2 C6 O1 -0.9(6) . . . . ?
N3 N2 C6 C4 179.3(5) . . . . ?
C7 O1 C6 N2 1.6(5) . . . . ?
C7 O1 C6 C4 -178.5(4) . . . . ?
C5 C4 C6 N2 176.1(5) . . . . ?
C3 C4 C6 N2 -5.1(8) . . . . ?
C5 C4 C6 O1 -3.7(7) . . . . ?
C3 C4 C6 O1 175.0(4) . . . . ?
N2 N3 C7 O1 1.4(6) . . . . ?
N2 N3 C7 C8 -178.9(5) . . . . ?
C6 O1 C7 N3 -1.8(6) . . . . ?
C6 O1 C7 C8 178.4(4) . . . . ?
N3 C7 C8 C9 -11.8(8) . . . . ?
O1 C7 C8 C9 167.9(5) . . . . ?
N3 C7 C8 C12 165.2(5) . . . . ?
O1 C7 C8 C12 -15.0(7) . . . . ?
C12 C8 C9 C10 1.2(8) . . . . ?
C7 C8 C9 C10 178.3(5) . . . . ?
C8 C9 C10 C11 -2.4(8) . . . . ?
C12 N4 C11 C10 1.4(7) . . . . ?
Cu1 N4 C11 C10 -170.7(4) . . . . ?
C9 C10 C11 N4 1.1(8) . . . . ?
C11 N4 C12 C8 -2.7(7) . . . . ?
Cu1 N4 C12 C8 169.4(4) . . . . ?
C9 C8 C12 N4 1.5(7) . . . . ?
C7 C8 C12 N4 -175.7(4) . . . . ?
