#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:48:09 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179078 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/40/4304040.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_4304040
loop_
_publ_author_name
'A. Thirumurugan'
'R. A. Sanguramath'
'C. N. R. Rao'
_publ_section_title
;
Hybrid Structures Formed by Lead 1,3-Cyclohexanedicarboxylates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              823
_journal_page_last               831
_journal_paper_doi               10.1021/ic701323q
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C16 H22 O9 Pb2'
_chemical_formula_weight         772.72
_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                92.922(3)
_cell_angle_beta                 97.147(2)
_cell_angle_gamma                107.695(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1442(5)
_cell_length_b                   9.7893(5)
_cell_length_c                   11.0738(6)
_cell_measurement_temperature    273(2)
_cell_volume                     932.89(9)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker,2000)'
_computing_data_reduction        'SAINT (Bruker,2000)'
_computing_molecular_graphics    DIAMOND
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_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  0.0479
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17716
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    18.071
_exptl_absorpt_correction_T_max  0.114000
_exptl_absorpt_correction_T_min  0.059600
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    2.751
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rod
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.412
_refine_diff_density_min         -2.518
_refine_diff_density_rms         0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         3343
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0467P)²+6.7206P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0930
_reflns_number_gt                3035
_reflns_number_total             3343
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701323q-file003_3.cif
_cod_data_source_block           compoundIII
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4304040
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
C1 C 0.1561(10) -0.1141(11) 0.1798(8) 0.033(2) Uani 1 1 d . . .
C2 C -0.0055(10) -0.2117(10) 0.1850(8) 0.0293(19) Uani 1 1 d . . .
H2 H -0.0059 -0.2491 0.2655 0.035 Uiso 1 1 calc R . .
C3 C -0.0608(12) -0.3411(11) 0.0879(9) 0.042(2) Uani 1 1 d . . .
H3A H -0.0588 -0.3072 0.0071 0.050 Uiso 1 1 calc R . .
H3B H 0.0088 -0.3986 0.0980 0.050 Uiso 1 1 calc R . .
C4 C -0.2246(12) -0.4335(10) 0.0991(9) 0.041(2) Uani 1 1 d . . .
H4A H -0.2253 -0.4731 0.1776 0.049 Uiso 1 1 calc R . .
H4B H -0.2591 -0.5130 0.0355 0.049 Uiso 1 1 calc R . .
C5 C 0.6649(10) -0.3437(10) 0.0874(9) 0.034(2) Uani 1 1 d . . .
H5A H 0.6599 -0.3104 0.0065 0.040 Uiso 1 1 calc R . .
H5B H 0.5616 -0.4034 0.0971 0.040 Uiso 1 1 calc R . .
C6 C -0.1168(9) -0.1226(9) 0.1749(7) 0.0255(17) Uani 1 1 d . . .
H6A H -0.1138 -0.0794 0.0980 0.031 Uiso 1 1 calc R . .
H6B H -0.0839 -0.0456 0.2407 0.031 Uiso 1 1 calc R . .
C7 C 0.7170(9) -0.2162(9) 0.1819(7) 0.0237(17) Uani 1 1 d . . .
H7 H 0.7161 -0.2531 0.2625 0.028 Uiso 1 1 calc R . .
C8 C 0.6131(9) -0.1225(9) 0.1736(7) 0.0220(17) Uani 1 1 d . . .
C21 C 1.0135(12) 0.2305(10) 0.4374(8) 0.040(2) Uani 1 1 d . . .
C22 C 1.131(2) 0.3557(16) 0.3966(11) 0.116(9) Uani 1 1 d . . .
H22 H 1.0528 0.3997 0.3641 0.140 Uiso 1 1 calc R . .
C23 C 1.183(2) 0.3475(15) 0.2884(13) 0.094(6) Uani 1 1 d . . .
H23A H 1.0940 0.3077 0.2256 0.113 Uiso 1 1 calc R . .
H23B H 1.2410 0.2790 0.2924 0.113 Uiso 1 1 calc R . .
C24 C 1.2831(17) 0.4818(16) 0.2480(11) 0.072(4) Uani 1 1 d . . .
H24A H 1.3573 0.4572 0.2028 0.087 Uiso 1 1 calc R . .
H24B H 1.2182 0.5193 0.1916 0.087 Uiso 1 1 calc R . .
C25 C 0.631(2) 0.4029(16) 0.6571(16) 0.115(8) Uani 1 1 d . . .
H25A H 0.6201 0.3123 0.6924 0.138 Uiso 1 1 calc R . .
H25B H 0.5273 0.4104 0.6381 0.138 Uiso 1 1 calc R . .
C26 C 1.2074(11) 0.4758(9) 0.4938(8) 0.0316(19) Uani 1 1 d . . .
H26A H 1.1277 0.5027 0.5301 0.038 Uiso 1 1 calc R . .
H26B H 1.2662 0.4410 0.5574 0.038 Uiso 1 1 calc R . .
C27 C 0.6869(19) 0.3935(13) 0.5477(11) 0.077(5) Uani 1 1 d . . .
H27 H 0.7682 0.3529 0.5792 0.092 Uiso 1 1 calc R . .
C28 C 0.6061(14) 0.2739(12) 0.4494(14) 0.059(3) Uani 1 1 d . . .
O1 O 0.2065(9) -0.0971(10) 0.0806(6) 0.059(2) Uani 1 1 d . . .
O2 O 0.2364(9) -0.0441(12) 0.2756(7) 0.073(3) Uani 1 1 d . . .
O3 O 0.5990(7) -0.0553(7) 0.2697(5) 0.0329(14) Uani 1 1 d . . .
O4 O 0.5452(8) -0.1057(8) 0.0735(6) 0.0383(16) Uani 1 1 d . . .
O5 O 0.8835(9) 0.1848(9) 0.3762(8) 0.064(2) Uani 1 1 d . . .
O6 O 1.0525(10) 0.1668(9) 0.5254(7) 0.059(2) Uani 1 1 d . . .
O7 O 0.5628(12) 0.3115(11) 0.3465(9) 0.082(3) Uani 1 1 d . . .
O8 O 0.5655(10) 0.1481(8) 0.4679(11) 0.076(3) Uani 1 1 d . . .
O9 O 0.7523(9) 0.2192(9) 0.1399(7) 0.0435(17) Uani 1 1 d D . .
Pb1 Pb 0.46506(4) 0.09979(3) 0.16941(3) 0.02741(12) Uani 1 1 d . . .
Pb2 Pb 0.73694(4) 0.00070(3) 0.49092(3) 0.02804(12) Uani 1 1 d . . .
H9A H 0.821(10) 0.211(14) 0.196(8) 0.06(4) Uiso 1 1 d D . .
H9B H 0.810(19) 0.23(2) 0.085(13) 0.15(9) 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'
Pb Pb -3.3944 10.1111 '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
O1 C1 O2 120.0(9) . . ?
O1 C1 C2 120.6(8) . . ?
O2 C1 C2 119.2(8) . . ?
C1 C2 C6 108.7(8) . . ?
C1 C2 C3 114.0(7) . . ?
C6 C2 C3 110.7(7) . . ?
C4 C3 C2 110.6(8) . . ?
C3 C4 C5 110.3(8) . 1_455 ?
C7 C5 C4 111.4(7) . 1_655 ?
C2 C6 C7 111.1(7) . 1_455 ?
C5 C7 C8 113.7(7) . . ?
C5 C7 C6 111.4(7) . 1_655 ?
C8 C7 C6 108.7(7) . 1_655 ?
O4 C8 O3 119.2(8) . . ?
O4 C8 C7 121.4(7) . . ?
O3 C8 C7 119.3(7) . . ?
O5 C21 O6 121.5(9) . . ?
O5 C21 C22 118.2(11) . . ?
O6 C21 C22 120.0(12) . . ?
C23 C22 C26 122.6(11) . . ?
C23 C22 C21 121.8(11) . . ?
C26 C22 C21 114.4(9) . . ?
C22 C23 C24 118.0(12) . . ?
C25 C24 C23 117.1(11) 2_766 . ?
C27 C25 C24 119.7(12) . 2_766 ?
C27 C26 C22 115.1(9) 2_766 . ?
C25 C27 C26 119.7(11) . 2_766 ?
C25 C27 C28 121.7(11) . . ?
C26 C27 C28 115.2(10) 2_766 . ?
O8 C28 O7 119.9(13) . . ?
O8 C28 C27 123.4(14) . . ?
O7 C28 C27 116.1(11) . . ?
C1 O1 Pb1 95.5(6) . . ?
C1 O2 Pb2 146.9(7) . 2_656 ?
C1 O2 Pb1 95.3(6) . . ?
Pb2 O2 Pb1 117.8(3) 2_656 . ?
C8 O3 Pb1 97.0(5) . . ?
C8 O3 Pb2 136.1(5) . . ?
Pb1 O3 Pb2 123.0(2) . . ?
C8 O4 Pb1 92.0(5) . . ?
C8 O4 Pb1 149.2(6) . 2_655 ?
Pb1 O4 Pb1 111.8(2) . 2_655 ?
C21 O5 Pb2 104.5(6) . . ?
C28 O7 Pb1 114.1(8) . . ?
C28 O8 Pb2 124.7(8) . . ?
O3 Pb1 O4 51.05(19) . . ?
O3 Pb1 O2 83.5(3) . . ?
O4 Pb1 O2 100.8(3) . . ?
O3 Pb1 O1 98.4(3) . . ?
O4 Pb1 O1 74.8(2) . . ?
O2 Pb1 O1 49.2(2) . . ?
O3 Pb1 O9 76.8(2) . . ?
O4 Pb1 O9 75.5(2) . . ?
O2 Pb1 O9 157.3(3) . . ?
O1 Pb1 O9 144.8(2) . . ?
O3 Pb1 O7 95.5(3) . . ?
O4 Pb1 O7 141.0(3) . . ?
O2 Pb1 O7 93.2(3) . . ?
O1 Pb1 O7 137.4(3) . . ?
O9 Pb1 O7 77.6(3) . . ?
O3 Pb1 O4 117.58(19) . 2_655 ?
O4 Pb1 O4 68.2(2) . 2_655 ?
O2 Pb1 O4 124.4(2) . 2_655 ?
O1 Pb1 O4 76.0(2) . 2_655 ?
O9 Pb1 O4 75.7(2) . 2_655 ?
O7 Pb1 O4 130.4(3) . 2_655 ?
O5 Pb2 O8 80.1(3) . . ?
O5 Pb2 O3 73.6(3) . . ?
O8 Pb2 O3 73.6(3) . . ?
O5 Pb2 O2 120.0(3) . 2_656 ?
O8 Pb2 O2 90.1(4) . 2_656 ?
O3 Pb2 O2 157.2(2) . 2_656 ?
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
C1 O1 1.244(12) . ?
C1 O2 1.249(11) . ?
C1 C2 1.506(13) . ?
C2 C6 1.527(12) . ?
C2 C3 1.534(13) . ?
C3 C4 1.520(15) . ?
C4 C5 1.526(13) 1_455 ?
C5 C7 1.504(12) . ?
C5 C4 1.526(13) 1_655 ?
C6 C7 1.531(11) 1_455 ?
C7 C8 1.506(12) . ?
C7 C6 1.531(11) 1_655 ?
C8 O4 1.245(10) . ?
C8 O3 1.264(10) . ?
C21 O5 1.233(13) . ?
C21 O6 1.256(13) . ?
C21 C22 1.493(14) . ?
C22 C23 1.354(18) . ?
C22 C26 1.489(14) . ?
C23 C24 1.481(17) . ?
C24 C25 1.459(19) 2_766 ?
C25 C27 1.382(19) . ?
C25 C24 1.459(19) 2_766 ?
C26 C27 1.483(13) 2_766 ?
C27 C26 1.483(13) 2_766 ?
C27 C28 1.499(16) . ?
C28 O8 1.209(15) . ?
C28 O7 1.270(17) . ?
O1 Pb1 2.594(7) . ?
O2 Pb2 2.568(7) 2_656 ?
O2 Pb1 2.594(8) . ?
O3 Pb1 2.450(6) . ?
O3 Pb2 2.562(6) . ?
O4 Pb1 2.566(6) . ?
O4 Pb1 2.685(6) 2_655 ?
O5 Pb2 2.418(8) . ?
O7 Pb1 2.639(9) . ?
O8 Pb2 2.433(9) . ?
O9 Pb1 2.599(8) . ?
Pb1 O4 2.685(6) 2_655 ?
Pb2 O2 2.568(7) 2_656 ?
