#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/61/2216116.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_2216116
loop_
_publ_author_name
'Xuan, Xiao-Peng'
'Zhao, Pei-Zheng'
_publ_section_title
catena-Poly[[(2,9-dimethyl-1,10-phenanthroline-κ²N,N')lead(II)]-di-μ-2-hydroxybenzoato-κ³O¹,O^1'^:O²;κ³O²:O¹,O^1'^]
_journal_coeditor_code           SJ2340
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2678
_journal_page_last               m2678
_journal_paper_doi               10.1107/S1600536807045941
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Pb (C7 H5 O3)2 (C14 H12 N2)]'
_chemical_formula_moiety         'C28 H22 N2 O6 Pb'
_chemical_formula_sum            'C28 H22 N2 O6 Pb'
_chemical_formula_weight         689.67
_chemical_name_systematic
;
catena-Poly[(2,9-dimethyl-1,10-phenanthroline-κ²N,N')lead(II)]-
di-μ-2-hydroxybenzoato-κ³O¹,O^1'^:O²;κ³O²:O¹,O^1'^]
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.6407(19)
_cell_length_b                   12.9690(12)
_cell_length_c                   9.8195(9)
_cell_measurement_reflns_used    5195
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.85
_cell_measurement_theta_min      2.80
_cell_volume                     2501.2(4)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  'SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            17366
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         2.80
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.792
_exptl_absorpt_correction_T_max  0.443
_exptl_absorpt_correction_T_min  0.241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.831
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.677
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2323
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0181
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0159P)²+3.2022P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0392
_refine_ls_wR_factor_ref         0.0441
_reflns_number_gt                1682
_reflns_number_total             2323
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sj2340.cif
_cod_data_source_block           I
_cod_database_code               2216116
_cod_database_fobs_code          2216116
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, 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
Pb Pb1 0.5000 0.681947(12) 1.2500 0.02840(7) Uani d S 1
O O1 0.39415(14) 0.73146(19) 1.0950(3) 0.0421(7) Uani d . 1
O O2 0.46065(14) 0.6121(2) 1.0038(3) 0.0509(7) Uani d . 1
O O3 0.41486(16) 0.4894(2) 0.8289(3) 0.0676(10) Uani d . 1
H H3 0.4414 0.5131 0.8854 0.101 Uiso d R 1
N N1 0.54686(15) 0.8440(2) 1.1448(3) 0.0283(7) Uani d . 1
C C1 0.59274(19) 0.8427(3) 1.0457(4) 0.0330(8) Uani d . 1
C C2 0.61983(19) 0.9346(3) 0.9934(4) 0.0410(9) Uani d . 1
H H2 0.6525 0.9320 0.9249 0.049 Uiso calc R 1
C C3 0.5986(2) 1.0276(3) 1.0422(4) 0.0412(10) Uani d . 1
H H3A 0.6164 1.0884 1.0069 0.049 Uiso calc R 1
C C4 0.54957(19) 1.0310(3) 1.1463(4) 0.0325(8) Uani d . 1
C C5 0.52573(17) 0.9357(3) 1.1951(3) 0.0271(7) Uani d . 1
C C6 0.5238(2) 1.1256(3) 1.2008(4) 0.0408(10) Uani d . 1
H H6 0.5401 1.1880 1.1675 0.049 Uiso calc R 1
C C7 0.6143(2) 0.7411(3) 0.9886(4) 0.0452(10) Uani d . 1
H H7A 0.6383 0.7027 1.0571 0.068 Uiso calc R 1
H H7B 0.6437 0.7521 0.9118 0.068 Uiso calc R 1
H H7C 0.5749 0.7030 0.9601 0.068 Uiso calc R 1
C C8 0.3607(2) 0.5531(3) 0.8161(4) 0.0420(9) Uani d . 1
C C9 0.35326(18) 0.6393(3) 0.9001(4) 0.0309(8) Uani d . 1
C C10 0.29722(19) 0.7031(3) 0.8802(4) 0.0418(10) Uani d . 1
H H10 0.2917 0.7608 0.9353 0.050 Uiso calc R 1
C C11 0.2497(2) 0.6826(3) 0.7808(4) 0.0505(12) Uani d . 1
H H11 0.2128 0.7264 0.7677 0.061 Uiso calc R 1
C C12 0.2578(2) 0.5956(4) 0.7005(5) 0.0552(12) Uani d . 1
H H12 0.2257 0.5810 0.6336 0.066 Uiso calc R 1
C C13 0.3120(2) 0.5310(3) 0.7180(4) 0.0555(12) Uani d . 1
H H13 0.3163 0.4723 0.6642 0.067 Uiso calc R 1
C C14 0.40548(19) 0.6634(3) 1.0067(4) 0.0326(8) Uani d . 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
N1 Pb1 N1 . 3_657 66.71(13)
N1 Pb1 O1 . . 81.32(9)
N1 Pb1 O1 3_657 . 75.34(8)
N1 Pb1 O1 . 3_657 75.34(8)
N1 Pb1 O1 3_657 3_657 81.32(9)
O1 Pb1 O1 . 3_657 152.01(11)
N1 Pb1 O2 . . 91.01(9)
N1 Pb1 O2 3_657 . 122.98(9)
O1 Pb1 O2 . . 48.90(8)
O1 Pb1 O2 3_657 . 145.09(8)
N1 Pb1 O2 . 3_657 122.97(9)
N1 Pb1 O2 3_657 3_657 91.01(9)
O1 Pb1 O2 . 3_657 145.09(8)
O1 Pb1 O2 3_657 3_657 48.90(8)
O2 Pb1 O2 . 3_657 140.70(12)
N1 Pb1 O3 . 7_566 164.79(9)
N1 Pb1 O3 3_657 7_566 108.72(10)
O1 Pb1 O3 . 7_566 83.49(8)
O1 Pb1 O3 3_657 7_566 119.06(8)
O2 Pb1 O3 . 7_566 79.39(9)
O2 Pb1 O3 3_657 7_566 70.51(8)
N1 Pb1 O3 . 5_667 108.72(10)
N1 Pb1 O3 3_657 5_667 164.79(9)
O1 Pb1 O3 . 5_667 119.06(8)
O1 Pb1 O3 3_657 5_667 83.49(8)
O2 Pb1 O3 . 5_667 70.51(8)
O2 Pb1 O3 3_657 5_667 79.39(9)
O3 Pb1 O3 7_566 5_667 79.34(14)
N1 Pb1 C14 . . 88.10(9)
N1 Pb1 C14 3_657 . 99.53(10)
O1 Pb1 C14 . . 24.37(8)
O1 Pb1 C14 3_657 . 161.67(9)
O2 Pb1 C14 . . 24.75(8)
O2 Pb1 C14 3_657 . 148.74(9)
O3 Pb1 C14 7_566 . 78.23(9)
O3 Pb1 C14 5_667 . 94.70(9)
N1 Pb1 C14 . 3_657 99.53(10)
N1 Pb1 C14 3_657 3_657 88.10(9)
O1 Pb1 C14 . 3_657 161.67(9)
O1 Pb1 C14 3_657 3_657 24.37(8)
O2 Pb1 C14 . 3_657 148.74(9)
O2 Pb1 C14 3_657 3_657 24.75(8)
O3 Pb1 C14 7_566 3_657 94.70(9)
O3 Pb1 C14 5_667 3_657 78.23(9)
C14 Pb1 C14 . 3_657 170.91(13)
C14 O1 Pb1 . . 95.0(2)
C14 O2 Pb1 . . 92.7(2)
C8 O3 Pb1 . 5_667 154.2(2)
C8 O3 H3 . . 109.5
Pb1 O3 H3 5_667 . 95.9
C1 N1 C5 . . 119.1(3)
C1 N1 Pb1 . . 122.6(2)
C5 N1 Pb1 . . 118.2(2)
N1 C1 C2 . . 121.1(3)
N1 C1 C7 . . 118.6(3)
C2 C1 C7 . . 120.3(3)
C3 C2 C1 . . 120.4(4)
C3 C2 H2 . . 119.8
C1 C2 H2 . . 119.8
C2 C3 C4 . . 119.5(4)
C2 C3 H3A . . 120.2
C4 C3 H3A . . 120.2
C5 C4 C3 . . 116.7(3)
C5 C4 C6 . . 120.6(3)
C3 C4 C6 . . 122.7(3)
N1 C5 C4 . . 123.1(3)
N1 C5 C5 . 3_657 118.42(19)
C4 C5 C5 . 3_657 118.5(2)
C6 C6 C4 3_657 . 121.0(2)
C6 C6 H6 3_657 . 119.5
C4 C6 H6 . . 119.5
C1 C7 H7A . . 109.5
C1 C7 H7B . . 109.5
H7A C7 H7B . . 109.5
C1 C7 H7C . . 109.5
H7A C7 H7C . . 109.5
H7B C7 H7C . . 109.5
O3 C8 C13 . . 118.7(4)
O3 C8 C9 . . 121.1(3)
C13 C8 C9 . . 120.2(4)
C10 C9 C8 . . 118.4(3)
C10 C9 C14 . . 121.0(3)
C8 C9 C14 . . 120.5(3)
C11 C10 C9 . . 121.4(4)
C11 C10 H10 . . 119.3
C9 C10 H10 . . 119.3
C10 C11 C12 . . 118.9(4)
C10 C11 H11 . . 120.6
C12 C11 H11 . . 120.6
C13 C12 C11 . . 121.2(4)
C13 C12 H12 . . 119.4
C11 C12 H12 . . 119.4
C12 C13 C8 . . 119.8(4)
C12 C13 H13 . . 120.1
C8 C13 H13 . . 120.1
O1 C14 O2 . . 122.3(3)
O1 C14 C9 . . 120.5(3)
O2 C14 C9 . . 117.3(3)
O1 C14 Pb1 . . 60.66(19)
O2 C14 Pb1 . . 62.50(19)
C9 C14 Pb1 . . 170.1(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Pb1 N1 . 2.516(3)
Pb1 N1 3_657 2.516(3)
Pb1 O1 . 2.656(3)
Pb1 O1 3_657 2.656(3)
Pb1 O2 . 2.695(3)
Pb1 O2 3_657 2.695(3)
Pb1 O3 7_566 2.887(3)
Pb1 O3 5_667 2.887(3)
Pb1 C14 . 3.035(4)
Pb1 C14 3_657 3.035(4)
O1 C14 . 1.257(4)
O2 C14 . 1.272(4)
O3 C8 . 1.353(4)
O3 Pb1 5_667 2.887(3)
O3 H3 . 0.8200
N1 C1 . 1.326(4)
N1 C5 . 1.353(4)
C1 C2 . 1.402(5)
C1 C7 . 1.495(5)
C2 C3 . 1.364(5)
C2 H2 . 0.9300
C3 C4 . 1.405(5)
C3 H3A . 0.9300
C4 C5 . 1.405(5)
C4 C6 . 1.432(5)
C5 C5 3_657 1.478(7)
C6 C6 3_657 1.344(8)
C6 H6 . 0.9300
C7 H7A . 0.9600
C7 H7B . 0.9600
C7 H7C . 0.9600
C8 C13 . 1.387(5)
C8 C9 . 1.397(5)
C9 C10 . 1.390(5)
C9 C14 . 1.499(5)
C10 C11 . 1.377(5)
C10 H10 . 0.9300
C11 C12 . 1.385(6)
C11 H11 . 0.9300
C12 C13 . 1.366(6)
C12 H12 . 0.9300
C13 H13 . 0.9300
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
O3 H3 O2 0.82 1.77 2.507(4) 148.2
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
N1 Pb1 O1 C14 . . 104.8(2)
N1 Pb1 O1 C14 3_657 . 172.9(2)
O1 Pb1 O1 C14 3_657 . 138.4(2)
O2 Pb1 O1 C14 . . 5.8(2)
O2 Pb1 O1 C14 3_657 . -117.2(2)
O3 Pb1 O1 C14 7_566 . -75.8(2)
O3 Pb1 O1 C14 5_667 . -1.8(2)
C14 Pb1 O1 C14 3_657 . -161.1(3)
N1 Pb1 O2 C14 . . -83.3(2)
N1 Pb1 O2 C14 3_657 . -20.6(3)
O1 Pb1 O2 C14 . . -5.7(2)
O1 Pb1 O2 C14 3_657 . -148.6(2)
O2 Pb1 O2 C14 3_657 . 125.0(2)
O3 Pb1 O2 C14 7_566 . 84.9(2)
O3 Pb1 O2 C14 5_667 . 167.2(2)
C14 Pb1 O2 C14 3_657 . 166.4(2)
N1 Pb1 N1 C1 3_657 . 178.7(3)
O1 Pb1 N1 C1 . . -103.6(3)
O1 Pb1 N1 C1 3_657 . 92.0(3)
O2 Pb1 N1 C1 . . -55.5(3)
O2 Pb1 N1 C1 3_657 . 103.5(3)
O3 Pb1 N1 C1 7_566 . -105.9(4)
O3 Pb1 N1 C1 5_667 . 14.2(3)
C14 Pb1 N1 C1 . . -80.1(3)
C14 Pb1 N1 C1 3_657 . 94.9(3)
N1 Pb1 N1 C5 3_657 . 0.90(19)
O1 Pb1 N1 C5 . . 78.6(2)
O1 Pb1 N1 C5 3_657 . -85.8(2)
O2 Pb1 N1 C5 . . 126.7(2)
O2 Pb1 N1 C5 3_657 . -74.2(3)
O3 Pb1 N1 C5 7_566 . 76.3(4)
O3 Pb1 N1 C5 5_667 . -163.5(2)
C14 Pb1 N1 C5 . . 102.1(3)
C14 Pb1 N1 C5 3_657 . -82.8(3)
C5 N1 C1 C2 . . 0.4(5)
Pb1 N1 C1 C2 . . -177.3(3)
C5 N1 C1 C7 . . -178.5(3)
Pb1 N1 C1 C7 . . 3.8(5)
N1 C1 C2 C3 . . -1.0(6)
C7 C1 C2 C3 . . 177.8(4)
C1 C2 C3 C4 . . 0.4(6)
C2 C3 C4 C5 . . 0.7(5)
C2 C3 C4 C6 . . -178.7(4)
C1 N1 C5 C4 . . 0.7(5)
Pb1 N1 C5 C4 . . 178.6(3)
C1 N1 C5 C5 . 3_657 179.6(4)
Pb1 N1 C5 C5 . 3_657 -2.5(5)
C3 C4 C5 N1 . . -1.3(5)
C6 C4 C5 N1 . . 178.1(4)
C3 C4 C5 C5 . 3_657 179.8(4)
C6 C4 C5 C5 . 3_657 -0.8(6)
C5 C4 C6 C6 . 3_657 -0.1(7)
C3 C4 C6 C6 . 3_657 179.2(5)
Pb1 O3 C8 C13 5_667 . 6.3(9)
Pb1 O3 C8 C9 5_667 . -174.0(4)
O3 C8 C9 C10 . . 178.7(4)
C13 C8 C9 C10 . . -1.6(6)
O3 C8 C9 C14 . . 0.0(6)
C13 C8 C9 C14 . . 179.7(4)
C8 C9 C10 C11 . . 0.1(6)
C14 C9 C10 C11 . . 178.7(3)
C9 C10 C11 C12 . . 0.9(6)
C10 C11 C12 C13 . . -0.4(7)
C11 C12 C13 C8 . . -1.1(7)
O3 C8 C13 C12 . . -178.2(4)
C9 C8 C13 C12 . . 2.1(7)
Pb1 O1 C14 O2 . . -11.0(4)
Pb1 O1 C14 C9 . . 168.7(3)
Pb1 O2 C14 O1 . . 10.8(4)
Pb1 O2 C14 C9 . . -168.9(3)
C10 C9 C14 O1 . . 11.9(5)
C8 C9 C14 O1 . . -169.5(4)
C10 C9 C14 O2 . . -168.5(4)
C8 C9 C14 O2 . . 10.2(5)
N1 Pb1 C14 O1 . . -73.0(2)
N1 Pb1 C14 O1 3_657 . -7.0(2)
O1 Pb1 C14 O1 3_657 . -98.1(4)
O2 Pb1 C14 O1 . . -169.5(4)
O2 Pb1 C14 O1 3_657 . 101.1(3)
O3 Pb1 C14 O1 7_566 . 100.3(2)
O3 Pb1 C14 O1 5_667 . 178.4(2)
N1 Pb1 C14 O2 . . 96.5(2)
N1 Pb1 C14 O2 3_657 . 162.5(2)
O1 Pb1 C14 O2 . . 169.5(4)
O1 Pb1 C14 O2 3_657 . 71.4(4)
O2 Pb1 C14 O2 3_657 . -89.3(3)
O3 Pb1 C14 O2 7_566 . -90.2(2)
O3 Pb1 C14 O2 5_667 . -12.1(2)
