#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/76/2237647.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_2237647
loop_
_publ_author_name
'Zhu, Yi'
'Zhang, Ming-Xing'
'Yang, Shan-Shan'
'Xiao, Feng'
'Zhang, Xiao-Ping'
'Gao, Yuan-Yuan'
'Li, Bing-Jie'
'Huang, Kun-Lin'
_publ_section_title
;
 Poly[diaqua[μ₆-4,4'-(1,4-phenylene)bis(2,6-dimethylpyridine-3,5-dicarboxylato)]dilead(II)]
;
_journal_coeditor_code           IM2422
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m232
_journal_page_last               m233
_journal_paper_doi               10.1107/S1600536813007733
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Pb2 (C24 H16 N2 O8) (H2 O1)2]'
_chemical_formula_moiety         'C24 H20 N2 O10 Pb2'
_chemical_formula_sum            'C24 H20 N2 O10 Pb2'
_chemical_formula_weight         910.80
_chemical_name_systematic
Poly[diaqua[μ₆-4,4'-(1,4-phenylene)bis(2,6-dimethylpyridine-3,5-dicarboxylato)]dilead(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                79.202(2)
_cell_angle_beta                 71.683(2)
_cell_angle_gamma                85.494(3)
_cell_formula_units_Z            1
_cell_length_a                   7.2182(12)
_cell_length_b                   9.0635(14)
_cell_length_c                   9.9589(15)
_cell_measurement_reflns_used    1580
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.111
_cell_measurement_theta_min      2.675
_cell_volume                     607.43(17)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_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  0.0147
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3168
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.903
_exptl_absorpt_correction_T_max  0.1422
_exptl_absorpt_correction_T_min  0.1287
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             422
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.148
_refine_diff_density_min         -1.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2119
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0221
_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)+(0.0347P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0552
_reflns_number_gt                1932
_reflns_number_total             2119
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            im2422.cif
_cod_data_source_block           I
_cod_database_code               2237647
_cod_database_fobs_code          2237647
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
_atom_site_symmetry_multiplicity
Pb Pb1 0.24557(3) 0.11141(2) 0.47717(2) 0.02892(9) Uani d . 1 1
O O1 0.0452(5) 0.9117(4) 0.6086(4) 0.0281(8) Uani d . 1 1
O O2 0.3224(5) 0.8538(4) 0.6568(5) 0.0365(9) Uani d . 1 1
O O3 0.2253(5) 0.1995(4) 0.7194(4) 0.0343(9) Uani d . 1 1
O O4 -0.0248(6) 0.2448(5) 0.6332(5) 0.0382(10) Uani d . 1 1
O O5 0.3782(6) -0.0957(5) 0.3132(5) 0.0441(11) Uani d . 1 1
H H1 0.4881 -0.1412 0.3019 0.066 Uiso d R 1 1
H H2 0.2924 -0.1629 0.3379 0.066 Uiso d R 1 1
N N1 -0.2153(6) 0.5547(5) 0.9379(5) 0.0275(10) Uani d . 1 1
C C1 -0.1131(7) 0.6798(6) 0.8704(6) 0.0245(11) Uani d . 1 1
C C2 0.0591(7) 0.6774(5) 0.7553(5) 0.0220(11) Uani d . 1 1
C C3 0.1282(7) 0.5404(6) 0.7125(5) 0.0213(10) Uani d . 1 1
C C4 0.0148(7) 0.4140(6) 0.7758(5) 0.0233(11) Uani d . 1 1
C C5 -0.1579(7) 0.4255(6) 0.8888(6) 0.0271(12) Uani d . 1 1
C C6 -0.1922(8) 0.8214(6) 0.9291(6) 0.0341(13) Uani d . 1 1
H H6A -0.2907 0.8662 0.8872 0.051 Uiso calc R 1 1
H H6B -0.0882 0.8906 0.9060 0.051 Uiso calc R 1 1
H H6C -0.2481 0.7975 1.0315 0.051 Uiso calc R 1 1
C C7 0.1542(7) 0.8222(6) 0.6705(6) 0.0242(11) Uani d . 1 1
C C8 0.0752(7) 0.2736(6) 0.7103(6) 0.0243(11) Uani d . 1 1
C C9 -0.2867(8) 0.2946(7) 0.9630(7) 0.0379(14) Uani d . 1 1
H H9A -0.2869 0.2692 1.0611 0.057 Uiso calc R 1 1
H H9B -0.2388 0.2102 0.9154 0.057 Uiso calc R 1 1
H H9C -0.4172 0.3203 0.9603 0.057 Uiso calc R 1 1
C C10 0.3206(7) 0.5253(5) 0.5999(5) 0.0192(10) Uani d . 1 1
C C11 0.3313(7) 0.5098(6) 0.4608(5) 0.0249(11) Uani d . 1 1
H H11 0.2177 0.5160 0.4347 0.030 Uiso calc R 1 1
C C12 0.5090(7) 0.4854(6) 0.3615(5) 0.0241(11) Uani d . 1 1
H H12 0.5146 0.4761 0.2689 0.029 Uiso calc R 1 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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 Pb1 O4 1_545 . 79.28(13)
O1 Pb1 O1 1_545 2_566 66.21(14)
O4 Pb1 O1 . 2_566 75.30(12)
O1 Pb1 O3 1_545 . 89.30(13)
O4 Pb1 O3 . . 51.16(12)
O1 Pb1 O3 2_566 . 124.84(11)
O1 Pb1 O5 1_545 . 78.92(13)
O4 Pb1 O5 . . 151.48(13)
O1 Pb1 O5 2_566 . 79.19(12)
O3 Pb1 O5 . . 146.08(13)
C8 O3 Pb1 . . 87.8(3)
C8 O4 Pb1 . . 94.7(3)
O3 C8 O4 . . 122.3(5)
O3 C8 C4 . . 121.6(5)
O4 C8 C4 . . 115.8(4)
C7 O1 Pb1 . 1_565 104.5(3)
C7 O1 Pb1 . 2_566 136.9(3)
Pb1 O1 Pb1 1_565 2_566 113.79(14)
C5 N1 C1 . . 119.3(4)
Pb1 O5 H1 . . 125.1
Pb1 O5 H2 . . 107.8
H1 O5 H2 . . 106.8
N1 C1 C2 . . 122.0(5)
N1 C1 C6 . . 115.8(5)
C2 C1 C6 . . 122.2(5)
C3 C2 C1 . . 118.6(5)
C3 C2 C7 . . 120.8(5)
C1 C2 C7 . . 120.2(4)
C4 C3 C2 . . 118.8(5)
C4 C3 C10 . . 119.1(4)
C2 C3 C10 . . 122.1(5)
C3 C4 C5 . . 119.1(5)
C3 C4 C8 . . 117.7(4)
C5 C4 C8 . . 122.9(5)
N1 C5 C4 . . 121.7(5)
N1 C5 C9 . . 116.0(5)
C4 C5 C9 . . 122.3(5)
C1 C6 H6A . . 109.5
C1 C6 H6B . . 109.5
H6A C6 H6B . . 109.5
C1 C6 H6C . . 109.5
H6A C6 H6C . . 109.5
H6B C6 H6C . . 109.5
O2 C7 O1 . . 121.6(5)
O2 C7 C2 . . 124.0(5)
O1 C7 C2 . . 114.4(4)
C5 C9 H9A . . 109.5
C5 C9 H9B . . 109.5
H9A C9 H9B . . 109.5
C5 C9 H9C . . 109.5
H9A C9 H9C . . 109.5
H9B C9 H9C . . 109.5
C12 C10 C11 2_666 . 119.3(4)
C12 C10 C3 2_666 . 118.9(4)
C11 C10 C3 . . 121.6(4)
C12 C11 C10 . . 120.7(5)
C12 C11 H11 . . 119.7
C10 C11 H11 . . 119.7
C11 C12 C10 . 2_666 120.0(5)
C11 C12 H12 . . 120.0
C10 C12 H12 2_666 . 120.0
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Pb1 O1 1_545 2.327(4)
Pb1 O4 . 2.472(4)
Pb1 O1 2_566 2.538(3)
Pb1 O3 . 2.638(4)
Pb1 O5 . 2.644(4)
O3 C8 . 1.248(6)
O4 C8 . 1.277(7)
C8 C4 . 1.510(7)
O1 C7 . 1.294(6)
O1 Pb1 1_565 2.327(4)
O1 Pb1 2_566 2.538(3)
N1 C5 . 1.338(7)
N1 C1 . 1.348(7)
O2 C7 . 1.230(6)
O5 H1 . 0.8500
O5 H2 . 0.8500
C1 C2 . 1.403(7)
C1 C6 . 1.507(7)
C2 C3 . 1.393(7)
C2 C7 . 1.507(7)
C3 C4 . 1.390(7)
C3 C10 . 1.501(7)
C4 C5 . 1.405(7)
C5 C9 . 1.494(8)
C6 H6A . 0.9600
C6 H6B . 0.9600
C6 H6C . 0.9600
C9 H9A . 0.9600
C9 H9B . 0.9600
C9 H9C . 0.9600
C10 C12 2_666 1.391(7)
C10 C11 . 1.395(7)
C11 C12 . 1.383(7)
C11 H11 . 0.9300
C12 C10 2_666 1.391(7)
C12 H12 . 0.9300
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
O5 H2 O4 2_556 0.85 2.04 2.834(6) 155.3
O5 H1 O3 2_656 0.85 2.05 2.879(5) 165.4
