#------------------------------------------------------------------------------
#$Date: 2018-06-12 05:03:57 +0300 (Tue, 12 Jun 2018) $
#$Revision: 208272 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/95/1549531.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_1549531
loop_
_publ_author_name
'Köferstein, Roberto'
'Robl, Christian'
_publ_section_title
;
 M2(H2O)[μ10-C6H2(COO)4] (M= Ba2+, Pb2+) - Two Isotypic Three-Dimensional
 Coordination Polymers with a Layer-like Separation between Anions and
 Cations
;
_journal_issue                   6
_journal_name_full
'Zeitschrift für anorganische und allgemeine Chemie'
_journal_page_first              1150
_journal_paper_doi               10.1002/zaac.201500050
_journal_volume                  641
_journal_year                    2015
_chemical_formula_sum            'C10 H4 O9 Pb2'
_chemical_formula_weight         682.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 113.590(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.5670(10)
_cell_length_b                   17.228(2)
_cell_length_c                   8.902(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1063.5(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0173
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1246
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    31.672
_exptl_crystal_density_diffrn    4.263
_exptl_crystal_F_000             1200
_refine_diff_density_max         3.414
_refine_diff_density_min         -4.925
_refine_diff_density_rms         0.510
_refine_ls_extinction_coef       0.0025(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.706
_refine_ls_goodness_of_fit_obs   1.800
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         1161
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.662
_refine_ls_restrained_S_obs      1.747
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_obs          0.0418
_refine_ls_shift/esd_max         -0.010
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0400P)²+5.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1062
_refine_ls_wR_factor_obs         0.1042
_reflns_number_observed          1016
_reflns_number_total             1161
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            PBPYRO2.cif
_cod_data_source_block           pbpyro2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. A new data item '_refine_ls_weighting_details' was
created with the value set to
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 5642 2017-10-24 12:04:52Z antanas 
;
_cod_database_code               1549531
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Pb1 Pb 1.0000 0.53067(4) -0.2500 0.0193(3) Uani 1 d S .
Pb2 Pb 0.5000 0.43748(4) -0.2500 0.0197(2) Uani 1 d S .
OW O 1.0000 0.6820(7) -0.2500 0.020(2) Uani 1 d SU .
O1 O 0.6755(11) 0.5394(5) 0.0355(9) 0.017(2) Uani 1 d U .
O2 O 0.6986(10) 0.5636(5) -0.2009(9) 0.014(2) Uani 1 d U .
O3 O 1.0848(11) 0.5845(5) 0.0711(10) 0.019(2) Uani 1 d U .
O4 O 1.2583(10) 0.6900(5) 0.1458(10) 0.023(2) Uani 1 d U .
C1 C 0.7079(13) 0.5857(6) -0.0612(12) 0.010(2) Uani 1 d U .
C2 C 1.1000(14) 0.6568(7) 0.0893(11) 0.014(2) Uani 1 d U .
C3 C 0.7339(13) 0.6709(6) -0.0240(11) 0.008(2) Uani 1 d U .
C4 C 0.9186(13) 0.7047(6) 0.0418(11) 0.009(2) Uani 1 d U .
C5 C 0.5707(14) 0.7150(6) -0.0621(12) 0.011(2) Uani 1 d U .
H1 H 0.4508(14) 0.6909(6) -0.1023(12) 0.050 Uiso 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'
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
O2 Pb1 O2 154.3(4) 2_754 .
O2 Pb1 OW 77.1(2) 2_754 .
O2 Pb1 OW 77.1(2) . .
O2 Pb1 O1 126.6(2) 2_754 6_565
O2 Pb1 O1 66.5(2) . 6_565
OW Pb1 O1 116.4(2) . 6_565
O2 Pb1 O1 66.5(2) 2_754 5_765
O2 Pb1 O1 126.6(2) . 5_765
OW Pb1 O1 116.4(2) . 5_765
O1 Pb1 O1 127.2(4) 6_565 5_765
O2 Pb1 O3 68.5(2) 2_754 6_565
O2 Pb1 O3 133.2(2) . 6_565
OW Pb1 O3 135.6(2) . 6_565
O1 Pb1 O3 68.3(2) 6_565 6_565
O1 Pb1 O3 74.6(2) 5_765 6_565
O2 Pb1 O3 133.2(2) 2_754 5_765
O2 Pb1 O3 68.5(2) . 5_765
OW Pb1 O3 135.6(2) . 5_765
O1 Pb1 O3 74.6(2) 6_565 5_765
O1 Pb1 O3 68.3(2) 5_765 5_765
O3 Pb1 O3 88.7(3) 6_565 5_765
O2 Pb1 O3 104.1(2) 2_754 .
O2 Pb1 O3 67.1(2) . .
OW Pb1 O3 70.8(2) . .
O1 Pb1 O3 129.3(2) 6_565 .
O1 Pb1 O3 70.1(2) 5_765 .
O3 Pb1 O3 143.6(3) 6_565 .
O3 Pb1 O3 70.4(3) 5_765 .
O2 Pb1 O3 67.1(2) 2_754 2_754
O2 Pb1 O3 104.1(2) . 2_754
OW Pb1 O3 70.8(2) . 2_754
O1 Pb1 O3 70.1(2) 6_565 2_754
O1 Pb1 O3 129.3(2) 5_765 2_754
O3 Pb1 O3 70.4(3) 6_565 2_754
O3 Pb1 O3 143.6(3) 5_765 2_754
O3 Pb1 O3 141.7(3) . 2_754
O2 Pb1 Pb2 166.6(2) 2_754 .
O2 Pb1 Pb2 37.0(2) . .
OW Pb1 Pb2 112.994(13) . .
O1 Pb1 Pb2 41.7(2) 6_565 .
O1 Pb1 Pb2 113.5(2) 5_765 .
O3 Pb1 Pb2 98.3(2) 6_565 .
O3 Pb1 Pb2 45.3(2) 5_765 .
O3 Pb1 Pb2 88.0(2) . .
O3 Pb1 Pb2 107.0(2) 2_754 .
O2 Pb1 Pb2 37.0(2) 2_754 1_655
O2 Pb1 Pb2 166.6(2) . 1_655
OW Pb1 Pb2 112.994(13) . 1_655
O1 Pb1 Pb2 113.5(2) 6_565 1_655
O1 Pb1 Pb2 41.7(2) 5_765 1_655
O3 Pb1 Pb2 45.3(2) 6_565 1_655
O3 Pb1 Pb2 98.3(2) 5_765 1_655
O3 Pb1 Pb2 107.0(2) . 1_655
O3 Pb1 Pb2 88.0(2) 2_754 1_655
Pb2 Pb1 Pb2 134.01(3) . 1_655
O2 Pb2 O2 65.1(3) . 2_654
O2 Pb2 O1 99.8(2) . 5_665
O2 Pb2 O1 65.5(2) 2_654 5_665
O2 Pb2 O1 65.5(2) . 6_565
O2 Pb2 O1 99.8(2) 2_654 6_565
O1 Pb2 O1 163.4(4) 5_665 6_565
O2 Pb2 O4 170.8(2) . 6_465
O2 Pb2 O4 110.5(2) 2_654 6_465
O1 Pb2 O4 84.8(2) 5_665 6_465
O1 Pb2 O4 108.6(2) 6_565 6_465
O2 Pb2 O4 110.5(2) . 5_765
O2 Pb2 O4 170.8(2) 2_654 5_765
O1 Pb2 O4 108.6(2) 5_665 5_765
O1 Pb2 O4 84.8(2) 6_565 5_765
O4 Pb2 O4 75.1(3) 6_465 5_765
O2 Pb2 O1 47.0(2) . .
O2 Pb2 O1 70.9(2) 2_654 .
O1 Pb2 O1 59.3(3) 5_665 .
O1 Pb2 O1 109.7(2) 6_565 .
O4 Pb2 O1 140.7(2) 6_465 .
O4 Pb2 O1 100.1(2) 5_765 .
O2 Pb2 O1 70.9(2) . 2_654
O2 Pb2 O1 47.0(2) 2_654 2_654
O1 Pb2 O1 109.7(2) 5_665 2_654
O1 Pb2 O1 59.3(3) 6_565 2_654
O4 Pb2 O1 100.1(2) 6_465 2_654
O4 Pb2 O1 140.7(2) 5_765 2_654
O1 Pb2 O1 106.5(3) . 2_654
O2 Pb2 O3 128.9(2) . 6_465
O2 Pb2 O3 65.8(2) 2_654 6_465
O1 Pb2 O3 71.7(2) 5_665 6_465
O1 Pb2 O3 110.6(2) 6_565 6_465
O4 Pb2 O3 45.0(2) 6_465 6_465
O4 Pb2 O3 120.1(2) 5_765 6_465
O1 Pb2 O3 124.4(2) . 6_465
O1 Pb2 O3 65.8(2) 2_654 6_465
O2 Pb2 O3 65.8(2) . 5_765
O2 Pb2 O3 128.9(2) 2_654 5_765
O1 Pb2 O3 110.6(2) 5_665 5_765
O1 Pb2 O3 71.7(2) 6_565 5_765
O4 Pb2 O3 120.1(2) 6_465 5_765
O4 Pb2 O3 45.0(2) 5_765 5_765
O1 Pb2 O3 65.8(2) . 5_765
O1 Pb2 O3 124.4(2) 2_654 5_765
O3 Pb2 O3 165.1(3) 6_465 5_765
O2 Pb2 C1 23.5(2) . .
O2 Pb2 C1 62.3(2) 2_654 .
O1 Pb2 C1 77.7(2) 5_665 .
O1 Pb2 C1 88.6(3) 6_565 .
O4 Pb2 C1 162.5(2) 6_465 .
O4 Pb2 C1 110.2(2) 5_765 .
O1 Pb2 C1 24.0(2) . .
O1 Pb2 C1 86.1(2) 2_654 .
O3 Pb2 C1 126.9(2) 6_465 .
O3 Pb2 C1 67.2(2) 5_765 .
O2 Pb2 C1 62.3(2) . 2_654
O2 Pb2 C1 23.5(2) 2_654 2_654
O1 Pb2 C1 88.6(3) 5_665 2_654
O1 Pb2 C1 77.7(2) 6_565 2_654
O4 Pb2 C1 110.2(2) 6_465 2_654
O4 Pb2 C1 162.5(2) 5_765 2_654
O1 Pb2 C1 86.1(2) . 2_654
O1 Pb2 C1 24.0(2) 2_654 2_654
O3 Pb2 C1 67.2(2) 6_465 2_654
O3 Pb2 C1 126.9(2) 5_765 2_654
C1 Pb2 C1 69.9(4) . 2_654
C1 O1 Pb1 113.0(6) . 5_765
C1 O1 Pb2 131.1(7) . 5_665
Pb1 O1 Pb2 97.4(2) 5_765 5_665
C1 O1 Pb2 86.1(6) . .
Pb1 O1 Pb2 108.2(3) 5_765 .
Pb2 O1 Pb2 120.7(3) 5_665 .
C1 O2 Pb1 121.9(6) . .
C1 O2 Pb2 102.6(6) . .
Pb1 O2 Pb2 106.5(3) . .
C2 O3 Pb1 131.7(6) . 5_765
C2 O3 Pb1 115.4(6) . .
Pb1 O3 Pb1 109.6(3) 5_765 .
C2 O3 Pb2 92.0(6) . 5_765
Pb1 O3 Pb2 92.3(2) 5_765 5_765
Pb1 O3 Pb2 105.6(2) . 5_765
C2 O4 Pb2 99.9(7) . 5_765
O1 C1 O2 121.6(10) . .
O1 C1 C3 120.7(9) . .
O2 C1 C3 117.3(9) . .
O1 C1 Pb2 69.9(6) . .
O2 C1 Pb2 53.9(5) . .
C3 C1 Pb2 156.1(7) . .
O3 C2 O4 122.3(10) . .
O3 C2 C4 118.7(9) . .
O4 C2 C4 119.0(10) . .
O3 C2 Pb2 65.0(6) . 5_765
O4 C2 Pb2 57.8(6) . 5_765
C4 C2 Pb2 170.8(6) . 5_765
C5 C3 C4 121.3(9) . .
C5 C3 C1 117.5(9) . .
C4 C3 C1 121.1(9) . .
C5 C4 C3 117.5(9) 7_665 .
C5 C4 C2 120.5(9) 7_665 .
C3 C4 C2 122.1(10) . .
C4 C5 C3 121.2(9) 7_665 .
C4 C5 H1 119.4(5) 7_665 .
C3 C5 H1 119.4(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O2 2.552(7) 2_754
Pb1 O2 2.552(7) .
Pb1 OW 2.607(13) .
Pb1 O1 2.716(8) 6_565
Pb1 O1 2.716(8) 5_765
Pb1 O3 2.775(8) 6_565
Pb1 O3 2.775(8) 5_765
Pb1 O3 2.824(8) .
Pb1 O3 2.824(8) 2_754
Pb1 Pb2 4.1101(6) .
Pb1 Pb2 4.1101(6) 1_655
Pb2 O2 2.578(8) .
Pb2 O2 2.578(8) 2_654
Pb2 O1 2.756(7) 5_665
Pb2 O1 2.756(7) 6_565
Pb2 O4 2.769(8) 6_465
Pb2 O4 2.769(8) 5_765
Pb2 O1 2.934(8) .
Pb2 O1 2.934(8) 2_654
Pb2 O3 2.923(8) 6_465
Pb2 O3 2.923(8) 5_765
Pb2 C1 3.116(10) .
Pb2 C1 3.116(10) 2_654
O1 C1 1.268(13) .
O1 Pb1 2.716(8) 5_765
O1 Pb2 2.756(7) 5_665
O2 C1 1.275(12) .
O3 C2 1.256(13) .
O3 Pb1 2.775(8) 5_765
O3 Pb2 2.923(8) 5_765
O4 C2 1.238(13) .
O4 Pb2 2.769(8) 5_765
C1 C3 1.500(14) .
C2 C4 1.510(14) .
C2 Pb2 3.222(11) 5_765
C3 C5 1.371(14) .
C3 C4 1.407(13) .
C4 C5 1.393(14) 7_665
C5 C4 1.393(14) 7_665
C5 H1 0.93 .
