#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:14:55 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180383 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/52/7205227.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_7205227
loop_
_publ_author_name
'Karmakar, Anirban'
'Goldberg, Israel'
_publ_section_title
;
 Coordination polymers of flexible tetracarboxylic acids with metal
 ions. II. Supramolecular assemblies of 5,5′-methylene- and
 5,5′-(ethane-1,2-diyl)-bis(oxy)diisophthalic acid ligands with
 d-transition metals
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              350
_journal_paper_doi               10.1039/c0ce00268b
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         'C18 H12 Cd O10'
_chemical_formula_sum            'C18 H12 Cd O10'
_chemical_formula_weight         500.68
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.1755(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8667(4)
_cell_length_b                   14.8068(4)
_cell_length_c                   14.6050(4)
_cell_measurement_reflns_used    3349
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.87
_cell_measurement_theta_min      2.97
_cell_volume                     2735.72(13)
_computing_cell_refinement       Denzo
_computing_data_collection       'Collect, Nonius B.V.'
_computing_data_reduction        'Denzo & Scalepack'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 12.8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. φ & ω 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  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23187
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         2.19
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.836
_exptl_absorpt_correction_T_max  0.8848
_exptl_absorpt_correction_T_min  0.8182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
;
_refine_diff_density_max         1.095
_refine_diff_density_min         -1.034
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.0017(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         3256
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0701P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.0974
_reflns_number_gt                2925
_reflns_number_total             3256
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CE00268B.TXT
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7205227
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Cd Cd 0.0000 0.568598(13) 0.2500 0.03365(12) Uani 1 2 d S . .
O1 O 0.12361(17) 0.45098(15) 0.24514(17) 0.0543(5) Uani 1 1 d . . .
O2 O 0.13184(14) 0.49622(12) 0.39049(15) 0.0515(4) Uani 1 1 d . . .
C3 C 0.1633(2) 0.44707(16) 0.3387(2) 0.0441(6) Uani 1 1 d . . .
C4 C 0.25142(18) 0.38059(16) 0.39089(19) 0.0446(5) Uani 1 1 d . . .
C5 C 0.28441(18) 0.32196(16) 0.33439(19) 0.0434(5) Uani 1 1 d . . .
H5 H 0.2524 0.3243 0.2632 0.052 Uiso 1 1 calc R . .
C6 C 0.36458(18) 0.26015(15) 0.3834(2) 0.0448(5) Uani 1 1 d . . .
C7 C 0.40246(18) 0.19693(16) 0.3246(2) 0.0482(6) Uani 1 1 d . . .
O8 O 0.36710(17) 0.19967(16) 0.23323(17) 0.0637(6) Uani 1 1 d . . .
O9 O 0.47186(15) 0.13917(12) 0.37516(16) 0.0569(5) Uani 1 1 d . . .
H9 H 0.5126 0.1546 0.3467 0.068 Uiso 1 1 d R . .
C10 C 0.41051(17) 0.25649(15) 0.4878(2) 0.0461(6) Uani 1 1 d . . .
H10 H 0.4649 0.2139 0.5211 0.055 Uiso 1 1 calc R . .
C11 C 0.37744(19) 0.31448(16) 0.54315(19) 0.0465(6) Uani 1 1 d . . .
C12 C 0.29716(19) 0.37679(16) 0.4950(2) 0.0480(6) Uani 1 1 d . . .
H12 H 0.2740 0.4163 0.5331 0.058 Uiso 1 1 calc R . .
O13 O 0.41851(15) 0.31570(12) 0.64593(14) 0.0554(5) Uani 1 1 d . . .
C14 C 0.4919(2) 0.24513(19) 0.6947(2) 0.0573(7) Uani 1 1 d . . .
H14A H 0.5598 0.2561 0.6895 0.069 Uiso 1 1 calc R . .
H14B H 0.4635 0.1862 0.6633 0.069 Uiso 1 1 calc R . .
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'
Cd Cd -0.8075 1.2024 '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'
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
O9 Cd O9 125.28(10) 4 3_455 ?
O9 Cd O2 125.29(7) 4 . ?
O9 Cd O2 80.64(6) 3_455 . ?
O9 Cd O2 80.65(6) 4 2 ?
O9 Cd O2 125.29(7) 3_455 2 ?
O2 Cd O2 126.29(9) . 2 ?
O9 Cd O1 134.28(7) 4 2 ?
O9 Cd O1 87.20(8) 3_455 2 ?
O2 Cd O1 87.40(7) . 2 ?
O2 Cd O1 53.64(7) 2 2 ?
O9 Cd O1 87.21(8) 4 . ?
O9 Cd O1 134.28(7) 3_455 . ?
O2 Cd O1 53.64(7) . . ?
O2 Cd O1 87.40(7) 2 . ?
O1 Cd O1 90.09(12) 2 . ?
O9 Cd O8 85.99(7) 4 3_455 ?
O9 Cd O8 52.30(7) 3_455 3_455 ?
O2 Cd O8 132.80(6) . 3_455 ?
O2 Cd O8 89.45(7) 2 3_455 ?
O1 Cd O8 93.17(10) 2 3_455 ?
O1 Cd O8 172.89(7) . 3_455 ?
O9 Cd O8 52.30(7) 4 4 ?
O9 Cd O8 85.99(7) 3_455 4 ?
O2 Cd O8 89.45(7) . 4 ?
O2 Cd O8 132.80(6) 2 4 ?
O1 Cd O8 172.89(7) 2 4 ?
O1 Cd O8 93.17(10) . 4 ?
O8 Cd O8 84.31(11) 3_455 4 ?
C3 O1 Cd 90.09(16) . . ?
C3 O2 Cd 94.37(16) . . ?
O1 C3 O2 121.9(2) . . ?
O1 C3 C4 119.1(2) . . ?
O2 C3 C4 119.0(3) . . ?
C12 C4 C5 120.5(2) . . ?
C12 C4 C3 119.4(2) . . ?
C5 C4 C3 120.0(2) . . ?
C6 C5 C4 119.4(2) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
C5 C6 C10 120.0(2) . . ?
C5 C6 C7 120.6(2) . . ?
C10 C6 C7 119.4(2) . . ?
O8 C7 O9 121.8(2) . . ?
O8 C7 C6 121.8(2) . . ?
O9 C7 C6 116.4(3) . . ?
C7 O8 Cd 85.45(16) . 3_545 ?
C7 O9 Cd 100.38(18) . 3_545 ?
C7 O9 H9 91.8 . . ?
C11 C10 C6 120.3(2) . . ?
C11 C10 H10 119.8 . . ?
C6 C10 H10 119.8 . . ?
O13 C11 C10 124.1(2) . . ?
O13 C11 C12 115.6(2) . . ?
C10 C11 C12 120.3(2) . . ?
C4 C12 C11 119.4(2) . . ?
C4 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C11 O13 C14 115.4(2) . . ?
O13 C14 C14 107.0(2) . 2_656 ?
O13 C14 H14A 110.3 . . ?
C14 C14 H14A 110.3 2_656 . ?
O13 C14 H14B 110.3 . . ?
C14 C14 H14B 110.3 2_656 . ?
H14A C14 H14B 108.6 . . ?
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
Cd O9 2.274(2) 4 ?
Cd O9 2.274(2) 3_455 ?
Cd O2 2.3724(18) . ?
Cd O2 2.3724(18) 2 ?
Cd O1 2.4649(19) 2 ?
Cd O1 2.4649(19) . ?
Cd O8 2.618(2) 3_455 ?
Cd O8 2.618(2) 4 ?
O1 C3 1.248(4) . ?
O2 C3 1.250(3) . ?
C3 C4 1.510(3) . ?
C4 C12 1.388(4) . ?
C4 C5 1.397(3) . ?
C5 C6 1.391(3) . ?
C5 H5 0.9500 . ?
C6 C10 1.392(4) . ?
C6 C7 1.503(3) . ?
C7 O8 1.219(4) . ?
C7 O9 1.273(3) . ?
O8 Cd 2.618(2) 3_545 ?
O9 Cd 2.274(2) 3_545 ?
O9 H9 0.8574 . ?
C10 C11 1.380(4) . ?
C10 H10 0.9500 . ?
C11 O13 1.370(3) . ?
C11 C12 1.394(3) . ?
C12 H12 0.9500 . ?
O13 C14 1.428(3) . ?
C14 C14 1.535(6) 2_656 ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
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_site_symmetry_A
O9 H9 O8 0.86 2.49 3.345(3) 179 2_655
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.012 -0.007 -0.010 1194 297 ' '
