#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/46/2204609.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_2204609
loop_
_publ_author_name
'Fan, Sai-Rong'
'Xiao, Hong-Ping'
'Zhang, Li-Ping'
'Zhu, Long-Guan'
_publ_section_title
Bis(μ-4-sulfobenzoato-κ²O:O')bis[aqua(2,2'-bipyridine-κ²N,N')copper(II)]
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1833
_journal_page_last               m1835
_journal_paper_doi               10.1107/S1600536804028958
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Cu2 (C7 H4 O5 S)2 (C10 H8 N2)2 (H2 O)2]'
_chemical_formula_moiety         'C34 H28 Cu2 N4 O12 S2'
_chemical_formula_sum            'C34 H28 Cu2 N4 O12 S2'
_chemical_formula_weight         875.80
_chemical_name_systematic
Bis(μ-4-sulfobenzoato-κ²O:O')bis[aqua(2,2'-bipyridine-κ²N,N')copper(II)]
_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                92.3060(10)
_cell_angle_beta                 112.3340(10)
_cell_angle_gamma                103.5660(10)
_cell_formula_units_Z            1
_cell_length_a                   8.9013(6)
_cell_length_b                   10.2224(7)
_cell_length_c                   10.4902(7)
_cell_measurement_reflns_used    5311
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      56.4
_cell_measurement_theta_min      4.2
_cell_volume                     849.36(10)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker,1997)'
_computing_data_reduction        'SHELXTL (Bruker, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and 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  0.0134
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4512
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         2.12
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.448
_exptl_absorpt_correction_T_max  0.8121
_exptl_absorpt_correction_T_min  0.5682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             446
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.520
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         3002
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0319
_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)+(0.0548P)²+0.3207P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0888
_reflns_number_gt                2799
_reflns_number_total             3002
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            br6171.cif
_cod_data_source_block           I
_cod_original_cell_volume        849.40(10)
_cod_database_code               2204609
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_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
_atom_site_type_symbol
Cu1 -0.13916(3) 0.54131(3) 0.11298(3) 0.03029(12) Uani d . 1 Cu
S1 0.28146(7) 1.20261(5) -0.24989(6) 0.02923(15) Uani d . 1 S
O1 -0.0481(2) 0.67975(18) 0.01954(18) 0.0385(4) Uani d . 1 O
O2 -0.2759(2) 0.68004(19) -0.1694(2) 0.0505(5) Uani d . 1 O
O4 0.4562(2) 1.22492(19) -0.1545(2) 0.0471(5) Uani d . 1 O
O5 0.2500(2) 1.15542(17) -0.39156(17) 0.0396(4) Uani d . 1 O
O3 0.2166(3) 1.31978(17) -0.2428(2) 0.0479(5) Uani d . 1 O
O6 -0.3501(3) 0.4803(2) -0.0481(2) 0.0568(6) Uani d D 1 O
N1 -0.1977(2) 0.39135(19) 0.2157(2) 0.0295(4) Uani d . 1 N
N2 0.0876(2) 0.5677(2) 0.2664(2) 0.0332(4) Uani d . 1 N
C1 -0.1253(3) 0.7276(2) -0.0897(2) 0.0314(5) Uani d . 1 C
C2 -0.0233(3) 0.8489(2) -0.1234(2) 0.0279(5) Uani d . 1 C
C3 0.1478(3) 0.9017(2) -0.0448(2) 0.0342(5) Uani d . 1 C
H3 0.2008 0.8628 0.0328 0.041 Uiso calc R 1 H
C4 0.2407(3) 1.0110(2) -0.0798(2) 0.0330(5) Uani d . 1 C
H4 0.3555 1.0456 -0.0259 0.040 Uiso calc R 1 H
C5 0.1626(3) 1.0695(2) -0.1959(2) 0.0276(5) Uani d . 1 C
C6 -0.0090(3) 1.0181(2) -0.2745(3) 0.0378(6) Uani d . 1 C
H6 -0.0622 1.0579 -0.3512 0.045 Uiso calc R 1 H
C7 -0.1008(3) 0.9086(3) -0.2393(3) 0.0373(6) Uani d . 1 C
H7 -0.2157 0.8740 -0.2933 0.045 Uiso calc R 1 H
C8 -0.3510(3) 0.3057(2) 0.1831(2) 0.0353(5) Uani d . 1 C
H8 -0.4428 0.3192 0.1095 0.042 Uiso calc R 1 H
C9 -0.3768(4) 0.1988(3) 0.2545(3) 0.0413(6) Uani d . 1 C
H9 -0.4845 0.1416 0.2299 0.050 Uiso calc R 1 H
C10 -0.2414(4) 0.1775(3) 0.3629(3) 0.0420(6) Uani d . 1 C
H10 -0.2559 0.1037 0.4103 0.050 Uiso calc R 1 H
C11 -0.0842(3) 0.2667(3) 0.4004(3) 0.0390(6) Uani d . 1 C
H11 0.0084 0.2549 0.4744 0.047 Uiso calc R 1 H
C12 -0.0663(3) 0.3743(2) 0.3261(2) 0.0308(5) Uani d . 1 C
C13 0.0946(3) 0.4793(2) 0.3589(2) 0.0306(5) Uani d . 1 C
C14 0.2398(3) 0.4906(3) 0.4764(3) 0.0384(6) Uani d . 1 C
H14 0.2423 0.4290 0.5396 0.046 Uiso calc R 1 H
C15 0.3816(3) 0.5954(3) 0.4982(3) 0.0426(6) Uani d . 1 C
H15 0.4802 0.6061 0.5773 0.051 Uiso calc R 1 H
C16 0.3754(3) 0.6834(3) 0.4022(3) 0.0462(7) Uani d . 1 C
H16 0.4703 0.7529 0.4142 0.055 Uiso calc R 1 H
C17 0.2269(3) 0.6675(3) 0.2878(3) 0.0426(6) Uani d . 1 C
H17 0.2227 0.7277 0.2232 0.051 Uiso calc R 1 H
H6A -0.407(4) 0.3942(15) -0.086(4) 0.080 Uiso d D 1 H
H6B -0.351(5) 0.533(3) -0.114(3) 0.080 Uiso d D 1 H
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_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O6 Cu1 O1 . 91.72(8) yes
O6 Cu1 N1 . 94.19(8) yes
O1 Cu1 N1 . 170.77(7) yes
O6 Cu1 N2 . 167.67(9) yes
O1 Cu1 N2 . 91.55(8) yes
N1 Cu1 N2 . 81.23(8) yes
O6 Cu1 O3 2_575 99.13(9) yes
O1 Cu1 O3 2_575 97.93(7) yes
N1 Cu1 O3 2_575 88.13(7) yes
N2 Cu1 O3 2_575 92.18(8) yes
O5 S1 O4 . 113.20(10) ?
O5 S1 O3 . 111.20(10) ?
O4 S1 O3 . 113.10(10) ?
O5 S1 C5 . 106.00(10) ?
O4 S1 C5 . 106.30(10) ?
O3 S1 C5 . 106.50(10) ?
C1 O1 Cu1 . 129.3(2) ?
S1 O3 Cu1 2_575 147.20(10) ?
Cu1 O6 H6A . 127(2) ?
Cu1 O6 H6B . 110(2) ?
H6A O6 H6B . 111(3) ?
C8 N1 C12 . 118.5(2) ?
C8 N1 Cu1 . 126.6(2) ?
C12 N1 Cu1 . 114.9(2) ?
C17 N2 C13 . 118.8(2) ?
C17 N2 Cu1 . 126.1(2) ?
C13 N2 Cu1 . 114.9(2) ?
O2 C1 O1 . 125.0(2) ?
O2 C1 C2 . 118.5(2) ?
O1 C1 C2 . 116.5(2) ?
C3 C2 C7 . 118.8(2) ?
C3 C2 C1 . 121.7(2) ?
C7 C2 C1 . 119.5(2) ?
C4 C3 C2 . 120.9(2) ?
C4 C3 H3 . 119.5 ?
C2 C3 H3 . 119.5 ?
C3 C4 C5 . 119.9(2) ?
C3 C4 H4 . 120.0 ?
C5 C4 H4 . 120.0 ?
C6 C5 C4 . 119.5(2) ?
C6 C5 S1 . 119.6(2) ?
C4 C5 S1 . 120.8(2) ?
C7 C6 C5 . 120.2(2) ?
C7 C6 H6 . 119.9 ?
C5 C6 H6 . 119.9 ?
C6 C7 C2 . 120.6(2) ?
C6 C7 H7 . 119.7 ?
C2 C7 H7 . 119.7 ?
N1 C8 C9 . 122.3(2) ?
N1 C8 H8 . 118.9 ?
C9 C8 H8 . 118.9 ?
C8 C9 C10 . 119.3(2) ?
C8 C9 H9 . 120.4 ?
C10 C9 H9 . 120.4 ?
C9 C10 C11 . 119.2(2) ?
C9 C10 H10 . 120.4 ?
C11 C10 H10 . 120.4 ?
C10 C11 C12 . 119.0(2) ?
C10 C11 H11 . 120.5 ?
C12 C11 H11 . 120.5 ?
N1 C12 C11 . 121.7(2) ?
N1 C12 C13 . 114.2(2) ?
C11 C12 C13 . 124.1(2) ?
N2 C13 C14 . 121.7(2) ?
N2 C13 C12 . 114.4(2) ?
C14 C13 C12 . 123.8(2) ?
C13 C14 C15 . 118.7(2) ?
C13 C14 H14 . 120.6 ?
C15 C14 H14 . 120.6 ?
C16 C15 C14 . 119.4(2) ?
C16 C15 H15 . 120.3 ?
C14 C15 H15 . 120.3 ?
C15 C16 C17 . 119.1(3) ?
C15 C16 H16 . 120.4 ?
C17 C16 H16 . 120.4 ?
N2 C17 C16 . 122.1(2) ?
N2 C17 H17 . 118.9 ?
C16 C17 H17 . 118.9 ?
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
Cu1 O6 . 1.930(2) yes
Cu1 O1 . 1.949(2) yes
Cu1 N1 . 1.992(2) yes
Cu1 N2 . 1.995(2) yes
Cu1 O3 2_575 2.316(2) yes
S1 O5 . 1.443(2) ?
S1 O4 . 1.451(2) ?
S1 O3 . 1.457(2) ?
S1 C5 . 1.770(2) ?
O1 C1 . 1.276(3) ?
O2 C1 . 1.242(3) ?
O3 Cu1 2_575 2.316(2) ?
O6 H6A . 0.890(10) ?
O6 H6B . 0.89(3) ?
N1 C8 . 1.344(3) ?
N1 C12 . 1.350(3) ?
N2 C17 . 1.343(3) ?
N2 C13 . 1.347(3) ?
C1 C2 . 1.496(3) ?
C2 C3 . 1.384(3) ?
C2 C7 . 1.395(3) ?
C3 C4 . 1.378(3) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.391(3) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.386(3) ?
C6 C7 . 1.375(3) ?
C6 H6 . 0.9300 ?
C7 H7 . 0.9300 ?
C8 C9 . 1.374(3) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.377(4) ?
C9 H9 . 0.9300 ?
C10 C11 . 1.378(4) ?
C10 H10 . 0.9300 ?
C11 C12 . 1.387(3) ?
C11 H11 . 0.9300 ?
C12 C13 . 1.482(3) ?
C13 C14 . 1.382(3) ?
C14 C15 . 1.386(4) ?
C14 H14 . 0.9300 ?
C15 C16 . 1.371(4) ?
C15 H15 . 0.9300 ?
C16 C17 . 1.375(4) ?
C16 H16 . 0.9300 ?
C17 H17 . 0.9300 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O6 H6A O4 1_445 0.890(10) 1.800(10) 2.688(3) 172(3) yes
O6 H6B O2 . 0.89(3) 1.71(2) 2.538(3) 153(4) yes
