#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:07:40 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179614 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/78/4507845.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_4507845
loop_
_publ_author_name
'Gabriel, C.'
'Raptopoulou, C. P.'
'Terzis, A.'
'Psycharis, V.'
'Gul-E-Noor, F.'
'Bertmer, M.'
'Mateescu, C.'
'Salifoglou, A.'
_publ_section_title
;
 Binary and Ternary Metal--Organic Hybrid Polymers in Aqueous
 Lead(II)--Dicarboxylic Acid--(Phen) Systems. The Influence of O- and
 S-Ligand Heteroatoms on the Assembly of Distinct Lattice Architecture,
 Dimensionality, and Spectroscopic Properties
;
_journal_issue                   6
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              2573
_journal_paper_doi               10.1021/cg400340y
_journal_volume                  13
_journal_year                    2013
_chemical_formula_sum            'C12 H12 O15 Pb3'
_chemical_formula_weight         1017.79
_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                114.3520(10)
_cell_angle_beta                 94.0390(10)
_cell_angle_gamma                91.2360(10)
_cell_formula_units_Z            2
_cell_length_a                   7.6283(2)
_cell_length_b                   10.8525(2)
_cell_length_c                   12.9010(3)
_cell_measurement_temperature    293(2)
_cell_volume                     969.08(4)
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ 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  0.0563
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            31021
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.20
_exptl_absorpt_coefficient_mu    26.073
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.010
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.807
_refine_diff_density_min         -1.257
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4415
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0276
_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)+(0.0179P)²+6.8360P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0683
_reflns_number_gt                4176
_reflns_number_total             4415
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg400340y_si_004.cif
_cod_data_source_block           salpb123
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4507845
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
Pb1 Pb 0.05258(3) 0.31300(3) 0.35586(2) 0.02938(7) Uani 1 1 d .
Pb2 Pb 0.43367(3) 0.96057(3) 0.64341(2) 0.02856(7) Uani 1 1 d .
Pb3 Pb 0.24577(4) -0.08533(3) -0.00646(2) 0.03365(8) Uani 1 1 d .
O1 O 0.1833(7) 0.5267(5) 0.5131(4) 0.0381(12) Uani 1 1 d .
O2 O 0.2583(9) 0.7346(6) 0.5379(6) 0.0607(19) Uani 1 1 d .
O3 O 0.3587(7) 0.4111(5) 0.3358(4) 0.0394(12) Uani 1 1 d .
O4 O 0.2421(9) 0.1633(6) 0.1931(5) 0.0553(17) Uani 1 1 d .
O5 O 0.4496(8) 0.1388(6) 0.0786(5) 0.0516(16) Uani 1 1 d .
C1 C 0.2706(10) 0.6090(8) 0.4877(6) 0.0371(16) Uani 1 1 d .
C2 C 0.3885(11) 0.5559(8) 0.3930(7) 0.0384(16) Uani 1 1 d .
H2A H 0.3636 0.5964 0.3395 0.046 Uiso 1 1 calc R
H2B H 0.5105 0.5790 0.4235 0.046 Uiso 1 1 calc R
C3 C 0.4457(12) 0.3517(8) 0.2357(7) 0.047(2) Uani 1 1 d .
H3A H 0.5706 0.3509 0.2556 0.056 Uiso 1 1 calc R
H3B H 0.4310 0.4047 0.1911 0.056 Uiso 1 1 calc R
C4 C 0.3721(10) 0.2090(8) 0.1660(6) 0.0355(16) Uani 1 1 d .
O11 O -0.1272(10) 0.3052(7) 0.1799(5) 0.0594(18) Uani 1 1 d .
O12 O 0.0139(11) 0.5036(8) 0.2607(6) 0.076(2) Uani 1 1 d .
O13 O -0.2576(11) 0.3446(6) 0.0077(5) 0.069(2) Uani 1 1 d .
O14 O -0.5153(9) 0.2273(7) -0.2572(5) 0.0567(17) Uani 1 1 d .
O15 O -0.3843(10) 0.1201(6) -0.1647(5) 0.0582(18) Uani 1 1 d .
C11 C -0.0860(11) 0.4183(9) 0.1826(7) 0.0454(19) Uani 1 1 d .
C12 C -0.1719(14) 0.4556(9) 0.0921(8) 0.053(2) Uani 1 1 d .
H12A H -0.2547 0.5249 0.1254 0.064 Uiso 1 1 calc R
H12B H -0.0832 0.4921 0.0604 0.064 Uiso 1 1 calc R
C13 C -0.3330(13) 0.3584(9) -0.0905(7) 0.048(2) Uani 1 1 d .
H13A H -0.2422 0.3893 -0.1247 0.057 Uiso 1 1 calc R
H13B H -0.4206 0.4259 -0.0683 0.057 Uiso 1 1 calc R
C14 C -0.4177(11) 0.2256(8) -0.1769(7) 0.0386(17) Uani 1 1 d .
O21 O 0.2503(10) 0.1871(8) 0.4478(6) 0.064(2) Uani 1 1 d .
O22 O 0.3214(7) 0.0141(6) 0.4843(4) 0.0372(12) Uani 1 1 d .
O23 O 0.1270(7) 0.0738(5) 0.6541(4) 0.0364(11) Uani 1 1 d .
O24 O 0.2137(10) -0.0433(7) 0.7918(5) 0.0580(18) Uani 1 1 d .
O25 O 0.0562(8) 0.0886(7) 0.9281(5) 0.0461(14) Uani 1 1 d .
C21 C 0.2346(10) 0.1179(8) 0.5021(6) 0.0352(16) Uani 1 1 d .
C22 C 0.1118(11) 0.1621(8) 0.5973(7) 0.0382(16) Uani 1 1 d .
H22A H 0.1434 0.2548 0.6510 0.046 Uiso 1 1 calc R
H22B H -0.0086 0.1577 0.5658 0.046 Uiso 1 1 calc R
C23 C 0.0482(12) 0.1243(9) 0.7595(7) 0.0456(19) Uani 1 1 d .
H23A H -0.0789 0.1128 0.7448 0.055 Uiso 1 1 calc R
H23B H 0.0796 0.2203 0.8012 0.055 Uiso 1 1 calc R
C24 C 0.1100(10) 0.0494(8) 0.8307(6) 0.0370(16) Uani 1 1 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'
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
O1 Pb1 O11 123.6(2) . .
O1 Pb1 O21 86.4(2) . .
O11 Pb1 O21 147.8(2) . .
O1 Pb1 O4 120.50(19) . .
O11 Pb1 O4 78.6(2) . .
O21 Pb1 O4 75.3(2) . .
O1 Pb1 O3 60.91(16) . .
O11 Pb1 O3 101.6(2) . .
O21 Pb1 O3 81.9(2) . .
O4 Pb1 O3 60.68(18) . .
O1 Pb1 O1 65.5(2) . 2_566
O11 Pb1 O1 89.2(2) . 2_566
O21 Pb1 O1 116.5(2) . 2_566
O4 Pb1 O1 167.8(2) . 2_566
O3 Pb1 O1 121.63(16) . 2_566
O22 Pb2 O2 85.8(2) 1_565 .
O22 Pb2 O15 128.5(2) 1_565 1_666
O2 Pb2 O15 145.1(2) . 1_666
O22 Pb2 O14 80.78(19) 1_565 1_666
O2 Pb2 O14 156.4(2) . 1_666
O15 Pb2 O14 49.07(19) 1_666 1_666
O22 Pb2 O24 118.66(19) 1_565 1_565
O2 Pb2 O24 76.4(2) . 1_565
O15 Pb2 O24 80.2(2) 1_666 1_565
O14 Pb2 O24 93.1(2) 1_666 1_565
O22 Pb2 O23 60.95(16) 1_565 1_565
O2 Pb2 O23 86.1(2) . 1_565
O15 Pb2 O23 104.0(2) 1_666 1_565
O14 Pb2 O23 70.39(19) 1_666 1_565
O24 Pb2 O23 59.67(17) 1_565 1_565
O22 Pb2 O22 65.4(2) 1_565 2_666
O2 Pb2 O22 109.9(2) . 2_666
O15 Pb2 O22 92.9(2) 1_666 2_666
O14 Pb2 O22 81.9(2) 1_666 2_666
O24 Pb2 O22 173.1(2) 1_565 2_666
O23 Pb2 O22 122.28(15) 1_565 2_666
O15 Pb3 O5 83.4(2) 2 2_655
O15 Pb3 O25 87.7(2) 2 2_556
O5 Pb3 O25 165.4(2) 2_655 2_556
O15 Pb3 O11 115.17(19) 2 2
O5 Pb3 O11 87.2(2) 2_655 2
O25 Pb3 O11 86.2(2) 2_556 2
O15 Pb3 O5 83.7(2) 2 .
O5 Pb3 O5 70.9(2) 2_655 .
O25 Pb3 O5 119.65(18) 2_556 .
O11 Pb3 O5 149.7(2) 2 .
C1 O1 Pb1 118.7(4) . .
C1 O1 Pb1 101.8(4) . 2_566
Pb1 O1 Pb1 114.5(2) . 2_566
C1 O2 Pb2 144.1(6) . .
C3 O3 C2 113.8(6) . .
C3 O3 Pb1 121.7(5) . .
C2 O3 Pb1 116.0(4) . .
C4 O4 Pb1 123.0(5) . .
C4 O5 Pb3 142.6(5) . 2_655
C4 O5 Pb3 100.8(5) . .
Pb3 O5 Pb3 109.1(2) 2_655 .
O2 C1 O1 122.0(7) . .
O2 C1 C2 118.6(7) . .
O1 C1 C2 119.4(7) . .
O3 C2 C1 108.8(6) . .
O3 C2 H2A 109.9 . .
C1 C2 H2A 109.9 . .
O3 C2 H2B 109.9 . .
C1 C2 H2B 109.9 . .
H2A C2 H2B 108.3 . .
O3 C3 C4 110.2(6) . .
O3 C3 H3A 109.6 . .
C4 C3 H3A 109.6 . .
O3 C3 H3B 109.6 . .
C4 C3 H3B 109.6 . .
H3A C3 H3B 108.1 . .
O4 C4 O5 121.9(7) . .
O4 C4 C3 121.2(6) . .
O5 C4 C3 116.9(7) . .
C11 O11 Pb1 101.4(5) . .
C11 O11 Pb3 129.0(6) . 2
Pb1 O11 Pb3 125.0(3) . 2
C12 O13 C13 117.7(7) . .
C14 O14 Pb2 93.4(5) . 1_444
C14 O15 Pb3 131.1(5) . 2
C14 O15 Pb2 93.8(5) . 1_444
Pb3 O15 Pb2 133.9(3) 2 1_444
O12 C11 O11 122.7(9) . .
O12 C11 C12 119.2(9) . .
O11 C11 C12 118.0(7) . .
O13 C12 C11 110.0(7) . .
O13 C12 H12A 109.7 . .
C11 C12 H12A 109.7 . .
O13 C12 H12B 109.7 . .
C11 C12 H12B 109.7 . .
H12A C12 H12B 108.2 . .
O13 C13 C14 111.0(7) . .
O13 C13 H13A 109.4 . .
C14 C13 H13A 109.4 . .
O13 C13 H13B 109.4 . .
C14 C13 H13B 109.4 . .
H13A C13 H13B 108.0 . .
O14 C14 O15 123.6(8) . .
O14 C14 C13 117.9(7) . .
O15 C14 C13 118.5(7) . .
C21 O21 Pb1 138.7(6) . .
C21 O22 Pb2 120.9(5) . 1_545
C21 O22 Pb2 102.3(4) . 2_666
Pb2 O22 Pb2 114.6(2) 1_545 2_666
C23 O23 C22 112.6(6) . .
C23 O23 Pb2 118.8(5) . 1_545
C22 O23 Pb2 114.9(4) . 1_545
C24 O24 Pb2 120.1(5) . 1_545
C24 O25 Pb3 135.2(5) . 2_556
O21 C21 O22 122.4(7) . .
O21 C21 C22 118.7(7) . .
O22 C21 C22 118.9(6) . .
O23 C22 C21 108.5(6) . .
O23 C22 H22A 110.0 . .
C21 C22 H22A 110.0 . .
O23 C22 H22B 110.0 . .
C21 C22 H22B 110.0 . .
H22A C22 H22B 108.4 . .
O23 C23 C24 110.2(6) . .
O23 C23 H23A 109.6 . .
C24 C23 H23A 109.6 . .
O23 C23 H23B 109.6 . .
C24 C23 H23B 109.6 . .
H23A C23 H23B 108.1 . .
O24 C24 O25 123.9(8) . .
O24 C24 C23 119.5(6) . .
O25 C24 C23 116.5(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O1 2.494(5) .
Pb1 O11 2.538(6) .
Pb1 O21 2.592(6) .
Pb1 O4 2.619(5) .
Pb1 O3 2.619(5) .
Pb1 O1 2.695(5) 2_566
Pb2 O22 2.458(5) 1_565
Pb2 O2 2.551(6) .
Pb2 O15 2.633(6) 1_666
Pb2 O14 2.645(7) 1_666
Pb2 O24 2.646(6) 1_565
Pb2 O23 2.652(5) 1_565
Pb2 O22 2.659(5) 2_666
Pb3 O15 2.551(6) 2
Pb3 O5 2.554(5) 2_655
Pb3 O25 2.585(5) 2_556
Pb3 O11 2.596(7) 2
Pb3 O5 2.633(6) .
O1 C1 1.263(10) .
O1 Pb1 2.695(5) 2_566
O2 C1 1.253(9) .
O3 C3 1.406(9) .
O3 C2 1.439(9) .
O4 C4 1.234(10) .
O5 C4 1.267(9) .
O5 Pb3 2.554(5) 2_655
C1 C2 1.493(10) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 C4 1.505(11) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
O11 C11 1.246(11) .
O11 Pb3 2.596(6) 2
O12 C11 1.243(10) .
O13 C12 1.360(10) .
O13 C13 1.420(10) .
O14 C14 1.239(10) .
O14 Pb2 2.645(7) 1_444
O15 C14 1.248(10) .
O15 Pb3 2.551(6) 2
O15 Pb2 2.633(6) 1_444
C11 C12 1.501(13) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C13 C14 1.507(11) .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
O21 C21 1.229(9) .
O22 C21 1.265(9) .
O22 Pb2 2.458(5) 1_545
O22 Pb2 2.659(5) 2_666
O23 C23 1.424(8) .
O23 C22 1.428(9) .
O23 Pb2 2.652(5) 1_545
O24 C24 1.251(10) .
O24 Pb2 2.646(6) 1_545
O25 C24 1.253(9) .
O25 Pb3 2.585(5) 2_556
C21 C22 1.520(10) .
C22 H22A 0.9700 .
C22 H22B 0.9700 .
C23 C24 1.515(11) .
C23 H23A 0.9700 .
C23 H23B 0.9700 .
