#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/95/2209550.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_2209550
loop_
_publ_author_name
'E Yang'
'Fa-Fu Yang'
'Shun-Yu Chen'
_publ_section_title
Poly[μ-aqua-aqua(μ₄-2-oxidobenzene-1,3-dicarboxylato)(μ₂-2-oxidobenzene-1,3-dicarboxylato)cadmium(II)dicopper(II)]
_journal_coeditor_code           HK2059
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1586
_journal_page_last               m1588
_journal_paper_doi               10.1107/S1600536806022690
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Cd Cu2 (C8 H3 O5)2 (H2 O)2]'
_chemical_formula_moiety         'C16 H10 Cd Cu2 O12'
_chemical_formula_sum            'C16 H10 Cd Cu2 O12'
_chemical_formula_weight         633.72
_chemical_name_systematic
;
Poly[μ-aqua-aqua(μ₄-2-oxidobenzene-1,3-dicarboxylato)(μ₂-2-
oxidobenzene-1,3-dicarboxylato)cadmium(II)dicopper(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                102.026(2)
_cell_angle_beta                 109.877(3)
_cell_angle_gamma                103.9580(10)
_cell_formula_units_Z            2
_cell_length_a                   8.272(3)
_cell_length_b                   10.362(3)
_cell_length_c                   11.373(4)
_cell_measurement_reflns_used    2209
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.23
_cell_volume                     843.5(5)
_computing_cell_refinement       'SMART and SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0185
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6580
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.23
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.822
_exptl_absorpt_correction_T_max  0.830
_exptl_absorpt_correction_T_min  0.579
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.912
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         3811
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_gt           0.0268
_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)+(0.039P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0679
_reflns_number_gt                3324
_reflns_number_total             3811
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hk2059.cif
_cod_data_source_block           I
_cod_database_code               2209550
_cod_database_fobs_code          2209550
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Cd Cd1 -0.03643(3) 0.41267(2) 0.82589(2) 0.02158(8) Uani d . 1
Cu Cu2 0.16737(5) 0.12920(3) 0.97382(3) 0.01643(9) Uani d . 1
O O2W 0.1629(4) 0.3645(3) 0.7475(3) 0.0392(6) Uani d D 1
O O6 -0.2298(3) 0.1873(2) 0.6971(2) 0.0263(5) Uani d . 1
O O10 0.0284(3) -0.0664(2) 0.87509(19) 0.0190(4) Uani d . 1
O O8 0.3054(3) 0.3094(2) 1.0974(2) 0.0220(5) Uani d . 1
O O9 0.3339(3) 0.0428(2) 1.0576(2) 0.0192(4) Uani d . 1
O O7 0.5414(3) 0.4748(2) 1.2580(2) 0.0306(5) Uani d . 1
C C3 0.7476(4) 0.0790(3) 1.3339(3) 0.0239(7) Uani d . 1
H H3A 0.8165 0.0245 1.3641 0.029 Uiso calc R 1
O O5 -0.0265(3) 0.1869(2) 0.87905(19) 0.0197(4) Uani d . 1
O O1W -0.1958(3) 0.4758(2) 0.9551(2) 0.0232(5) Uani d D 1
C C7 0.4877(4) 0.1010(3) 1.1696(3) 0.0158(6) Uani d . 1
C C10 -0.1876(4) -0.0315(3) 0.6924(3) 0.0167(6) Uani d . 1
C C8 0.4623(4) 0.3493(3) 1.1968(3) 0.0191(6) Uani d . 1
C C6 0.5488(4) 0.2457(3) 1.2391(3) 0.0174(6) Uani d . 1
C C14 -0.1631(4) -0.2624(3) 0.6814(3) 0.0172(6) Uani d . 1
C C16 -0.1047(4) -0.1187(3) 0.7517(3) 0.0139(5) Uani d . 1
C C4 0.8016(5) 0.2181(4) 1.4072(3) 0.0286(7) Uani d . 1
H H4A 0.9020 0.2559 1.4882 0.034 Uiso calc R 1
C C2 0.5912(4) 0.0183(3) 1.2151(3) 0.0174(6) Uani d . 1
C C12 -0.3782(5) -0.2287(3) 0.4932(3) 0.0271(7) Uani d . 1
H H12A -0.4673 -0.2645 0.4071 0.032 Uiso calc R 1
C C11 -0.3213(4) -0.0888(3) 0.5632(3) 0.0222(6) Uani d . 1
H H11A -0.3735 -0.0305 0.5232 0.027 Uiso calc R 1
C C13 -0.3011(4) -0.3147(3) 0.5529(3) 0.0227(6) Uani d . 1
H H13A -0.3414 -0.4099 0.5070 0.027 Uiso calc R 1
C C9 -0.1470(4) 0.1203(3) 0.7579(3) 0.0168(6) Uani d . 1
C C5 0.7047(4) 0.2997(3) 1.3584(3) 0.0256(7) Uani d . 1
H H5A 0.7439 0.3942 1.4063 0.031 Uiso calc R 1
C C15 -0.0954(4) -0.3674(3) 0.7356(3) 0.0180(6) Uani d . 1
C C1 0.5485(4) -0.1332(3) 1.1439(3) 0.0179(6) Uani d . 1
O O4 0.0461(3) -0.3322(2) 0.8454(2) 0.0208(4) Uani d . 1
O O2 0.6760(3) -0.1808(2) 1.1690(2) 0.0269(5) Uani d . 1
O O3 -0.1770(3) -0.4942(2) 0.6742(2) 0.0293(5) Uani d . 1
O O1 0.3856(3) -0.2117(2) 1.0590(2) 0.0228(5) Uani d . 1
Cu Cu1 0.19978(5) -0.15056(3) 0.96097(3) 0.01730(9) Uani d . 1
H H2A 0.222(5) 0.318(4) 0.779(4) 0.067(16) Uiso d D 1
H H1A -0.244(6) 0.527(4) 0.927(4) 0.069(16) Uiso d D 1
H H1B -0.282(5) 0.411(3) 0.941(5) 0.09(2) Uiso d D 1
H H2B 0.250(4) 0.423(4) 0.748(5) 0.063(16) Uiso d 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'
Cu Cu 0.3201 1.2651 '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'
Cd Cd -0.8075 1.2024 '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
O2W Cd1 O3 . 1_565 98.77(10) ?
O2W Cd1 O6 . . 86.44(10) yes
O3 Cd1 O6 1_565 . 92.31(8) ?
O2W Cd1 O1W . . 167.46(9) yes
O3 Cd1 O1W 1_565 . 91.41(9) ?
O6 Cd1 O1W . . 100.53(9) yes
O2W Cd1 O1W . 2_567 92.14(10) ?
O3 Cd1 O1W 1_565 2_567 130.47(8) ?
O6 Cd1 O1W . 2_567 136.71(7) ?
O1W Cd1 O1W . 2_567 75.61(9) ?
O2W Cd1 O4 . 1_565 97.85(9) ?
O3 Cd1 O4 1_565 1_565 53.83(7) ?
O6 Cd1 O4 . 1_565 146.15(7) ?
O1W Cd1 O4 . 1_565 82.22(8) ?
O1W Cd1 O4 2_567 1_565 76.91(7) ?
O2W Cd1 O5 . . 79.68(8) yes
O3 Cd1 O5 1_565 . 145.33(7) ?
O6 Cd1 O5 . . 53.05(7) yes
O1W Cd1 O5 . . 96.10(7) yes
O1W Cd1 O5 2_567 . 84.11(7) ?
O4 Cd1 O5 1_565 . 160.78(6) ?
O8 Cu2 O5 . . 93.89(9) yes
O8 Cu2 O9 . . 94.27(9) yes
O5 Cu2 O9 . . 171.10(8) ?
O8 Cu2 O10 . . 169.46(9) ?
O5 Cu2 O10 . . 91.94(9) ?
O9 Cu2 O10 . . 79.45(8) ?
O8 Cu2 Cu1 . . 133.04(6) ?
O5 Cu2 Cu1 . . 132.08(6) ?
O9 Cu2 Cu1 . . 39.29(6) ?
O10 Cu2 Cu1 . . 40.17(6) ?
Cd1 O2W H2A . . 118(3) ?
Cd1 O2W H2B . . 125(3) ?
H2A O2W H2B . . 96(3) ?
C9 O6 Cd1 . . 99.46(18) ?
C16 O10 Cu1 . . 128.09(18) ?
C16 O10 Cu2 . . 126.81(17) ?
Cu1 O10 Cu2 . . 99.61(9) yes
C8 O8 Cu2 . . 128.62(19) ?
C7 O9 Cu1 . . 129.03(18) ?
C7 O9 Cu2 . . 128.69(18) ?
Cu1 O9 Cu2 . . 101.25(9) yes
C4 C3 C2 . . 121.4(3) ?
C4 C3 H3A . . 119.3 ?
C2 C3 H3A . . 119.3 ?
C9 O5 Cu2 . . 125.52(18) ?
C9 O5 Cd1 . . 86.68(15) ?
Cu2 O5 Cd1 . . 133.34(10) ?
Cd1 O1W Cd1 . 2_567 104.39(9) ?
Cd1 O1W H1A . . 108(4) ?
Cd1 O1W H1A 2_567 . 113(3) ?
Cd1 O1W H1B . . 111(4) ?
Cd1 O1W H1B 2_567 . 120(4) ?
H1A O1W H1B . . 101(3) ?
O9 C7 C2 . . 119.8(3) ?
O9 C7 C6 . . 120.4(2) ?
C2 C7 C6 . . 119.9(3) ?
C11 C10 C16 . . 119.0(3) ?
C11 C10 C9 . . 115.9(2) ?
C16 C10 C9 . . 125.1(2) ?
O7 C8 O8 . . 119.2(3) ?
O7 C8 C6 . . 119.2(3) ?
O8 C8 C6 . . 121.5(3) ?
C5 C6 C7 . . 118.1(3) ?
C5 C6 C8 . . 115.9(3) ?
C7 C6 C8 . . 126.0(3) ?
C13 C14 C16 . . 119.1(3) ?
C13 C14 C15 . . 116.1(3) ?
C16 C14 C15 . . 124.7(2) ?
O10 C16 C10 . . 120.7(2) ?
O10 C16 C14 . . 119.9(2) ?
C10 C16 C14 . . 119.3(2) ?
C5 C4 C3 . . 118.9(3) ?
C5 C4 H4A . . 120.5 ?
C3 C4 H4A . . 120.6 ?
C3 C2 C7 . . 119.2(3) ?
C3 C2 C1 . . 116.2(3) ?
C7 C2 C1 . . 124.6(2) ?
C11 C12 C13 . . 118.8(3) ?
C11 C12 H12A . . 120.6 ?
C13 C12 H12A . . 120.6 ?
C12 C11 C10 . . 122.1(3) ?
C12 C11 H11A . . 119.0 ?
C10 C11 H11A . . 119.0 ?
C12 C13 C14 . . 121.6(3) ?
C12 C13 H13A . . 119.2 ?
C14 C13 H13A . . 119.2 ?
O6 C9 O5 . . 117.8(3) ?
O6 C9 C10 . . 119.9(3) ?
O5 C9 C10 . . 122.3(2) ?
C4 C5 C6 . . 122.4(3) ?
C4 C5 H5A . . 118.8 ?
C6 C5 H5A . . 118.8 ?
O3 C15 O4 . . 118.0(3) ?
O3 C15 C14 . . 119.4(3) ?
O4 C15 C14 . . 122.6(2) ?
O2 C1 O1 . . 120.9(3) ?
O2 C1 C2 . . 117.6(3) ?
O1 C1 C2 . . 121.5(3) ?
C15 O4 Cu1 . . 128.53(18) ?
C15 O4 Cd1 . 1_545 87.31(16) ?
Cu1 O4 Cd1 . 1_545 143.45(10) ?
C15 O3 Cd1 . 1_545 100.12(18) ?
C1 O1 Cu1 . . 126.54(18) ?
O4 Cu1 O1 . . 94.66(9) ?
O4 Cu1 O9 . . 171.24(8) ?
O1 Cu1 O9 . . 93.61(9) ?
O4 Cu1 O10 . . 92.06(9) ?
O1 Cu1 O10 . . 173.28(9) ?
O9 Cu1 O10 . . 79.68(8) ?
O4 Cu1 Cu2 . . 132.20(6) ?
O1 Cu1 Cu2 . . 133.07(6) ?
O9 Cu1 Cu2 . . 39.46(6) ?
O10 Cu1 Cu2 . . 40.22(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
Cd1 O2W . 2.230(3) yes
Cd1 O3 1_565 2.265(2) ?
Cd1 O6 . 2.310(2) yes
Cd1 O1W . 2.379(2) yes
Cd1 O1W 2_567 2.388(2) ?
Cd1 O4 1_565 2.507(2) ?
Cd1 O5 . 2.549(2) yes
Cu2 O8 . 1.884(2) yes
Cu2 O5 . 1.909(2) yes
Cu2 O9 . 1.914(2) yes
Cu2 O10 . 1.934(2) yes
Cu2 Cu1 . 2.9532(10) yes
O2W H2A . 0.82(4) ?
O2W H2B . 0.82(4) ?
O6 C9 . 1.240(3) ?
O10 C16 . 1.349(3) ?
O10 Cu1 . 1.932(2) yes
O8 C8 . 1.297(4) ?
O9 C7 . 1.347(3) ?
O9 Cu1 . 1.907(2) yes
O7 C8 . 1.227(3) ?
C3 C4 . 1.381(5) ?
C3 C2 . 1.400(4) ?
C3 H3A . 0.9300 ?
O5 C9 . 1.306(3) ?
O1W Cd1 2_567 2.388(2) ?
O1W H1A . 0.79(4) ?
O1W H1B . 0.80(4) ?
C7 C2 . 1.404(4) ?
C7 C6 . 1.413(4) ?
C10 C11 . 1.396(4) ?
C10 C16 . 1.407(4) ?
C10 C9 . 1.494(4) ?
C8 C6 . 1.500(4) ?
C6 C5 . 1.401(4) ?
C14 C13 . 1.403(4) ?
C14 C16 . 1.408(4) ?
C14 C15 . 1.490(4) ?
C4 C5 . 1.373(5) ?
C4 H4A . 0.9300 ?
C2 C1 . 1.501(4) ?
C12 C11 . 1.375(4) ?
C12 C13 . 1.377(4) ?
C12 H12A . 0.9300 ?
C11 H11A . 0.9300 ?
C13 H13A . 0.9300 ?
C5 H5A . 0.9300 ?
C15 O3 . 1.240(3) ?
C15 O4 . 1.293(3) ?
C1 O2 . 1.242(4) ?
C1 O1 . 1.292(4) ?
O4 Cu1 . 1.888(2) yes
O4 Cd1 1_545 2.507(2) ?
O3 Cd1 1_545 2.265(2) ?
O1 Cu1 . 1.899(2) yes
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
O1W H1A O8 2_567 0.79(4) 1.93(2) 2.701(3) 164(5) yes
O1W H1B O1 2_557 0.80(4) 2.04(3) 2.748(3) 149(5) yes
O2W H2A O2 2_657 0.82(4) 1.92(2) 2.724(3) 170(5) yes
O2W H2B O7 2_667 0.82(4) 1.83(2) 2.635(4) 169(5) yes
