#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/55/2215528.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2215528
loop_
_publ_author_name
'Fa-Qian Liu'
'Rong-Xun Li'
'Shao-Xiang Li'
'Li-Shui Sun'
'Guang-Ye Liu'
_publ_section_title
Tetra-μ-acetato-κ⁸O:O'-bis[(4-vinylpyridine-κN)copper(II)](Cu---Cu)
_journal_coeditor_code           HG2288
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2455
_journal_page_last               m2455
_journal_paper_doi               10.1107/S1600536807042328
_journal_volume                  63
_journal_year                    2007
_chemical_formula_moiety         'C22 H26 Cu2 N2 O8'
_chemical_formula_sum            'C22 H26 Cu2 N2 O8'
_chemical_formula_weight         573.53
_chemical_name_systematic
;
Tetra-μ-acetato-κ⁸O:O'-bis[(4-vinylpyridine-\kN)copper(II)](Cu---Cu)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.65(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.696(2)
_cell_length_b                   12.830(3)
_cell_length_c                   9.4820(19)
_cell_measurement_reflns_used    3329
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.14
_cell_measurement_theta_min      2.53
_cell_volume                     1253.0(5)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2001)'
_computing_publication_material
'SHELXTL (Sheldrick, 2001) and local programs'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2001)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1K CCD area-detector'
_diffrn_measurement_method       'thin-slice 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  0.0132
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2455
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         1.98
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.744
_exptl_absorpt_correction_T_max  0.8449
_exptl_absorpt_correction_T_min  0.6227
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.471
_refine_diff_density_min         -1.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2358
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.1P)²+3P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1641
_refine_ls_wR_factor_ref         0.1824
_reflns_number_gt                1830
_reflns_number_total             2358
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hg2288.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2215528
_cod_database_fobs_code          2215528
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Cu Cu 0.40251(7) 0.02266(5) 0.05538(7) 0.0441(3) Uani d . 1
O O1 0.3606(5) -0.1277(3) 0.0336(5) 0.0612(11) Uani d . 1
O O2 0.4745(5) 0.1639(3) 0.0554(5) 0.0630(12) Uani d . 1
O O3 0.3013(5) 0.0430(4) -0.1496(5) 0.0641(12) Uani d . 1
O O4 0.5344(5) -0.0066(4) 0.2417(5) 0.0663(12) Uani d . 1
N N 0.2542(5) 0.0760(4) 0.1573(5) 0.0508(11) Uani d . 1
C C1 -0.0518(10) 0.2562(8) 0.4014(10) 0.101 Uani d D 1
H H1A 0.0269 0.2911 0.4345 0.121 Uiso calc R 1
H H1B -0.1233 0.2774 0.4321 0.121 Uiso calc R 1
C C2 -0.0617(10) 0.1780(8) 0.3125(10) 0.100 Uani d D 1
H H2A -0.1386 0.1412 0.2771 0.120 Uiso calc R 1
C C3 0.0585(7) 0.1517(7) 0.2715(8) 0.074(2) Uani d . 1
C C4 0.1672(8) 0.2085(5) 0.2806(8) 0.0677(19) Uani d . 1
H H4A 0.1774 0.2736 0.3251 0.081 Uiso calc R 1
C C5 0.2638(6) 0.1679(5) 0.2221(7) 0.0562(15) Uani d . 1
H H5A 0.3382 0.2073 0.2293 0.067 Uiso calc R 1
C C6 0.1465(7) 0.0221(6) 0.1532(8) 0.0691(19) Uani d . 1
H H6A 0.1387 -0.0437 0.1106 0.083 Uiso calc R 1
C C7 0.0486(8) 0.0551(8) 0.2057(9) 0.083(2) Uani d . 1
H H7A -0.0243 0.0136 0.1978 0.099 Uiso calc R 1
C C8 0.6099(8) 0.3033(6) 0.0297(10) 0.082(2) Uani d . 1
H H8A 0.5859 0.3336 0.1111 0.123 Uiso calc R 1
H H8B 0.5659 0.3391 -0.0587 0.123 Uiso calc R 1
H H8C 0.7020 0.3093 0.0448 0.123 Uiso calc R 1
C C9 0.5718(6) 0.1895(5) 0.0165(7) 0.0501(14) Uani d . 1
C C10 0.7308(8) -0.0547(7) 0.4061(7) 0.080(2) Uani d . 1
H H10A 0.8105 -0.0162 0.4246 0.121 Uiso calc R 1
H H10B 0.7496 -0.1279 0.4161 0.121 Uiso calc R 1
H H10C 0.6842 -0.0343 0.4752 0.121 Uiso calc R 1
C C11 0.6490(7) -0.0322(4) 0.2527(7) 0.0563(16) Uani d . 1
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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 Cu O3 . . 89.4(2) y
O2 Cu O4 . . 89.4(2) ?
O3 Cu O4 . . 167.5(2) y
O2 Cu O1 . . 167.15(17) ?
O3 Cu O1 . . 88.7(2) y
O4 Cu O1 . . 89.7(2) y
O2 Cu N . . 92.43(19) y
O3 Cu N . . 97.14(19) y
O4 Cu N . . 95.30(19) y
O1 Cu N . . 100.41(19) y
O2 Cu Cu . 3_655 81.48(13) y
O3 Cu Cu . 3_655 85.37(14) y
O4 Cu Cu . 3_655 82.19(15) y
O1 Cu Cu . 3_655 85.69(13) y
N Cu Cu . 3_655 173.42(15) y
C9 O1 Cu 3_655 . 121.3(4) ?
C9 O2 Cu . . 127.2(4) ?
C11 O3 Cu 3_655 . 121.6(4) ?
C11 O4 Cu . . 125.0(4) ?
C5 N C6 . . 115.7(6) ?
C5 N Cu . . 120.8(4) ?
C6 N Cu . . 123.4(5) ?
C2 C1 H1A . . 120.0 ?
C2 C1 H1B . . 120.0 ?
H1A C1 H1B . . 120.0 ?
C1 C2 C3 . . 115.1(10) ?
C1 C2 H2A . . 122.5 ?
C3 C2 H2A . . 122.5 ?
C4 C3 C7 . . 118.1(7) ?
C4 C3 C2 . . 130.7(9) ?
C7 C3 C2 . . 111.0(8) ?
C3 C4 C5 . . 119.2(7) ?
C3 C4 H4A . . 120.4 ?
C5 C4 H4A . . 120.4 ?
N C5 C4 . . 122.9(6) ?
N C5 H5A . . 118.5 ?
C4 C5 H5A . . 118.5 ?
N C6 C7 . . 125.4(8) ?
N C6 H6A . . 117.3 ?
C7 C6 H6A . . 117.3 ?
C6 C7 C3 . . 118.6(8) ?
C6 C7 H7A . . 120.7 ?
C3 C7 H7A . . 120.7 ?
C9 C8 H8A . . 109.5 ?
C9 C8 H8B . . 109.5 ?
H8A C8 H8B . . 109.5 ?
C9 C8 H8C . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
O2 C9 O1 . 3_655 124.3(6) ?
O2 C9 C8 . . 117.5(6) ?
O1 C9 C8 3_655 . 118.2(6) ?
C11 C10 H10A . . 109.5 ?
C11 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
C11 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
O3 C11 O4 3_655 . 125.8(6) ?
O3 C11 C10 3_655 . 118.6(7) ?
O4 C11 C10 . . 115.6(6) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu O2 . 1.969(4) y
Cu O3 . 1.971(4) y
Cu O4 . 1.977(5) y
Cu O1 . 1.979(4) y
Cu N . 2.178(5) y
Cu Cu 3_655 2.6405(14) y
O1 C9 3_655 1.251(7) ?
O2 C9 . 1.238(7) ?
O3 C11 3_655 1.240(8) ?
O4 C11 . 1.246(9) ?
N C5 . 1.320(8) ?
N C6 . 1.335(8) ?
C1 C2 . 1.296(8) ?
C1 H1A . 0.9300 ?
C1 H1B . 0.9300 ?
C2 C3 . 1.479(12) ?
C2 H2A . 0.9300 ?
C3 C4 . 1.355(11) ?
C3 C7 . 1.379(12) ?
C4 C5 . 1.399(9) ?
C4 H4A . 0.9300 ?
C5 H5A . 0.9300 ?
C6 C7 . 1.343(10) ?
C6 H6A . 0.9300 ?
C7 H7A . 0.9300 ?
C8 C9 . 1.511(9) ?
C8 H8A . 0.9600 ?
C8 H8B . 0.9600 ?
C8 H8C . 0.9600 ?
C9 O1 3_655 1.251(7) ?
C10 C11 . 1.509(8) ?
C10 H10A . 0.9600 ?
C10 H10B . 0.9600 ?
C10 H10C . 0.9600 ?
C11 O3 3_655 1.240(8) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C5 H5A O2 0.93 2.54 3.083(8) 118 y
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_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
O2 Cu O1 C9 . 3_655 4.5(12)
O3 Cu O1 C9 . 3_655 86.0(5)
O4 Cu O1 C9 . 3_655 -81.6(5)
N Cu O1 C9 . 3_655 -177.0(5)
Cu Cu O1 C9 3_655 3_655 0.6(5)
O3 Cu O2 C9 . . -87.1(6)
O4 Cu O2 C9 . . 80.5(6)
O1 Cu O2 C9 . . -5.7(12)
N Cu O2 C9 . . 175.8(5)
Cu Cu O2 C9 3_655 . -1.7(5)
O2 Cu O3 C11 . 3_655 80.3(5)
O4 Cu O3 C11 . 3_655 -4.3(13)
O1 Cu O3 C11 . 3_655 -87.0(5)
N Cu O3 C11 . 3_655 172.7(5)
Cu Cu O3 C11 3_655 3_655 -1.2(5)
O2 Cu O4 C11 . . -81.0(5)
O3 Cu O4 C11 . . 3.6(13)
O1 Cu O4 C11 . . 86.1(5)
N Cu O4 C11 . . -173.4(5)
Cu Cu O4 C11 3_655 . 0.4(5)
O2 Cu N C5 . . -16.0(5)
O3 Cu N C5 . . -105.7(5)
O4 Cu N C5 . . 73.6(5)
O1 Cu N C5 . . 164.3(5)
O2 Cu N C6 . . 160.8(6)
O3 Cu N C6 . . 71.1(6)
O4 Cu N C6 . . -109.6(6)
O1 Cu N C6 . . -18.9(6)
C1 C2 C3 C4 . . -18.3(14)
C1 C2 C3 C7 . . 166.1(9)
C7 C3 C4 C5 . . 0.6(11)
C2 C3 C4 C5 . . -174.6(7)
C6 N C5 C4 . . -1.4(9)
Cu N C5 C4 . . 175.7(5)
C3 C4 C5 N . . 0.2(10)
C5 N C6 C7 . . 1.8(12)
Cu N C6 C7 . . -175.2(7)
N C6 C7 C3 . . -1.0(14)
C4 C3 C7 C6 . . -0.3(12)
C2 C3 C7 C6 . . 175.8(8)
Cu O2 C9 O1 . 3_655 1.8(10)
Cu O2 C9 C8 . . -178.7(5)
Cu O4 C11 O3 . 3_655 0.4(10)
Cu O4 C11 C10 . . -177.7(5)
