#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/82/2228240.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_2228240
loop_
_publ_author_name
'Dai, Jun'
'Yang, Juan'
'Li, Jiantong'
_publ_section_title
;
 Bis(benzoato-κ²O,O')(1,10-phenanthroline-κ²N,N')lead(II)
 benzoic acid monosolvate
;
_journal_coeditor_code           BT5413
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1661
_journal_page_last               m1662
_journal_paper_doi               10.1107/S1600536810048725
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Pb (C7 H5 O2)2 (C12 H8 N2)], C7 H6 O2'
_chemical_formula_moiety         'C26 H18 N2 O4 Pb, C7 H6 O2'
_chemical_formula_sum            'C33 H24 N2 O6 Pb'
_chemical_formula_weight         751.73
_chemical_name_systematic
;
Bis(benzoato-κ²O,O')(1,10-phenanthroline-
κ²N,N')lead(II) benzoic acid monosolvate
;
_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
_cell_angle_alpha                93.414(2)
_cell_angle_beta                 102.836(2)
_cell_angle_gamma                117.9720(10)
_cell_formula_units_Z            2
_cell_length_a                   10.0725(8)
_cell_length_b                   10.5697(8)
_cell_length_c                   15.5477(17)
_cell_measurement_reflns_used    3689
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.50
_cell_measurement_theta_min      1.37
_cell_volume                     1399.3(2)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       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  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0436
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8277
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.37
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    6.078
_exptl_absorpt_correction_T_max  0.582
_exptl_absorpt_correction_T_min  0.263
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.731
_refine_diff_density_min         -0.730
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5710
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0293
_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)+(0.0380P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0739
_reflns_number_gt                4950
_reflns_number_total             5710
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bt5413.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C33 H24 N2 O6 Pb1'
_cod_database_code               2228240
_cod_database_fobs_code          2228240
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_disorder_assembly
_atom_site_disorder_group
Pb Pb1 0.595637(19) 0.391099(18) 0.465657(12) 0.04103(7) Uani d . 1 . .
O O1 0.7152(4) 0.4830(4) 0.3537(2) 0.0547(9) Uani d . 1 . .
O O2 0.4876(4) 0.4755(4) 0.3081(3) 0.0577(9) Uani d . 1 . .
O O3 0.8489(4) 0.5402(4) 0.5653(3) 0.0659(11) Uani d . 1 . .
O O4 0.7626(4) 0.6979(4) 0.5547(3) 0.0567(9) Uani d . 1 . .
O O5 0.2159(4) 0.3215(4) 0.1819(3) 0.0696(11) Uani d . 1 . .
H H5 0.3118 0.3665 0.2014 0.084 Uiso d R 1 . .
O O6 0.1681(6) 0.5034(5) 0.1686(4) 0.0944(15) Uani d . 1 . .
N N1 0.4405(4) 0.1384(4) 0.3537(3) 0.0416(9) Uani d . 1 . .
N N2 0.7216(4) 0.2286(4) 0.4793(3) 0.0393(8) Uani d . 1 . .
C C1 0.6176(6) 0.5023(5) 0.2969(3) 0.0452(11) Uani d . 1 . .
C C2 0.6615(5) 0.5607(5) 0.2168(3) 0.0424(11) Uani d . 1 . .
C C3 0.5676(6) 0.5993(5) 0.1582(3) 0.0488(12) Uani d . 1 . .
H H3A 0.4771 0.5908 0.1695 0.059 Uiso calc R 1 . .
C C4 0.6080(7) 0.6507(6) 0.0828(4) 0.0582(13) Uani d . 1 . .
H H4A 0.5446 0.6765 0.0435 0.070 Uiso calc R 1 . .
C C5 0.7400(7) 0.6634(6) 0.0660(4) 0.0632(15) Uani d . 1 . .
H H5A 0.7654 0.6965 0.0147 0.076 Uiso calc R 1 . .
C C6 0.8358(7) 0.6282(6) 0.1236(4) 0.0607(14) Uani d . 1 . .
H H6A 0.9275 0.6402 0.1123 0.073 Uiso calc R 1 . .
C C7 0.7965(6) 0.5747(6) 0.1985(4) 0.0563(13) Uani d . 1 . .
H H7A 0.8602 0.5481 0.2367 0.068 Uiso calc R 1 . .
C C8 0.8635(6) 0.6642(5) 0.5888(3) 0.0444(11) Uani d . 1 . .
C C9 1.0096(5) 0.7720(5) 0.6587(3) 0.0385(10) Uani d . 1 . .
C C10 1.0375(6) 0.9115(6) 0.6866(3) 0.0482(12) Uani d . 1 . .
H H10A 0.9629 0.9374 0.6620 0.058 Uiso calc R 1 . .
C C11 1.1724(6) 1.0110(6) 0.7493(4) 0.0569(13) Uani d . 1 . .
H H11A 1.1885 1.1038 0.7675 0.068 Uiso calc R 1 . .
C C12 1.2841(6) 0.9756(7) 0.7857(4) 0.0644(15) Uani d . 1 . .
H H12A 1.3764 1.0442 0.8282 0.077 Uiso calc R 1 . .
C C13 1.2596(6) 0.8381(7) 0.7592(4) 0.0623(15) Uani d . 1 . .
H H13A 1.3351 0.8134 0.7842 0.075 Uiso calc R 1 . .
C C14 1.1226(6) 0.7364(6) 0.6955(3) 0.0484(12) Uani d . 1 . .
H H14A 1.1067 0.6437 0.6773 0.058 Uiso calc R 1 . .
C C15 0.3050(6) 0.0935(6) 0.2932(4) 0.0534(13) Uani d . 1 . .
H H15A 0.2721 0.1612 0.2819 0.064 Uiso calc R 1 . .
C C16 0.2095(6) -0.0469(6) 0.2458(4) 0.0574(14) Uani d . 1 . .
H H16A 0.1150 -0.0730 0.2037 0.069 Uiso calc R 1 . .
C C17 0.2566(6) -0.1472(5) 0.2620(3) 0.0504(12) Uani d . 1 . .
H H17A 0.1938 -0.2429 0.2306 0.060 Uiso calc R 1 . .
C C18 0.3980(5) -0.1070(5) 0.3252(3) 0.0421(10) Uani d . 1 . .
C C19 0.4560(6) -0.2050(5) 0.3430(3) 0.0457(11) Uani d . 1 . .
H H19A 0.3956 -0.3019 0.3135 0.055 Uiso calc R 1 . .
C C20 0.5954(6) -0.1606(5) 0.4015(3) 0.0452(11) Uani d . 1 . .
H H20A 0.6318 -0.2262 0.4111 0.054 Uiso calc R 1 . .
C C21 0.6893(5) -0.0133(5) 0.4495(3) 0.0376(10) Uani d . 1 . .
C C22 0.8359(6) 0.0362(5) 0.5108(3) 0.0451(11) Uani d . 1 . .
H H22A 0.8740 -0.0278 0.5224 0.054 Uiso calc R 1 . .
C C23 0.9227(6) 0.1780(6) 0.5534(4) 0.0524(12) Uani d . 1 . .
H H23A 1.0210 0.2123 0.5936 0.063 Uiso calc R 1 . .
C C24 0.8615(5) 0.2722(5) 0.5357(3) 0.0442(11) Uani d . 1 . .
H H24A 0.9218 0.3693 0.5649 0.053 Uiso calc R 1 . .
C C25 0.6365(5) 0.0866(5) 0.4351(3) 0.0355(9) Uani d . 1 . .
C C26 0.4878(5) 0.0390(5) 0.3695(3) 0.0371(10) Uani d . 1 . .
C C27 0.1292(6) 0.3771(7) 0.1484(4) 0.0581(14) Uani d . 1 . .
C C28 -0.0215(6) 0.2676(6) 0.0814(4) 0.0506(12) Uani d . 1 . .
C C29 -0.1214(8) 0.3134(8) 0.0389(5) 0.083(2) Uani d . 1 . .
H H29A -0.0936 0.4112 0.0515 0.100 Uiso calc R 1 . .
C C30 -0.2625(9) 0.2159(10) -0.0223(5) 0.102(3) Uani d . 1 . .
H H30A -0.3299 0.2480 -0.0499 0.122 Uiso calc R 1 . .
C C31 -0.3037(8) 0.0742(9) -0.0426(5) 0.089(2) Uani d . 1 . .
H H31A -0.3990 0.0085 -0.0839 0.107 Uiso calc R 1 . .
C C32 -0.2035(9) 0.0287(7) -0.0015(5) 0.084(2) Uani d . 1 . .
H H32A -0.2310 -0.0688 -0.0155 0.100 Uiso calc R 1 . .
C C33 -0.0624(7) 0.1247(6) 0.0603(4) 0.0641(15) Uani d . 1 . .
H H33A 0.0048 0.0920 0.0875 0.077 Uiso calc R 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
_geom_angle_publ_flag
O1 Pb1 O3 . . 84.82(14) ?
O1 Pb1 N2 . . 88.82(12) ?
O3 Pb1 N2 . . 75.08(11) ?
O1 Pb1 N1 . . 85.71(12) ?
O3 Pb1 N1 . . 137.85(11) ?
N2 Pb1 N1 . . 63.74(12) ?
O1 Pb1 O2 . . 49.51(10) ?
O3 Pb1 O2 . . 121.87(13) ?
N2 Pb1 O2 . . 127.06(11) ?
N1 Pb1 O2 . . 79.89(11) ?
C1 O1 Pb1 . . 105.9(3) ?
C1 O2 Pb1 . . 83.1(3) ?
C8 O3 Pb1 . . 107.8(3) ?
C27 O5 H5 . . 125.4 ?
C15 N1 C26 . . 117.5(4) ?
C15 N1 Pb1 . . 123.7(3) ?
C26 N1 Pb1 . . 117.7(3) ?
C24 N2 C25 . . 117.8(4) ?
C24 N2 Pb1 . . 122.2(3) ?
C25 N2 Pb1 . . 119.5(3) ?
O2 C1 O1 . . 121.4(5) ?
O2 C1 C2 . . 120.2(4) ?
O1 C1 C2 . . 118.4(4) ?
C3 C2 C7 . . 118.8(5) ?
C3 C2 C1 . . 120.7(4) ?
C7 C2 C1 . . 120.4(4) ?
C2 C3 C4 . . 120.1(5) ?
C2 C3 H3A . . 119.9 ?
C4 C3 H3A . . 119.9 ?
C5 C4 C3 . . 120.2(5) ?
C5 C4 H4A . . 119.9 ?
C3 C4 H4A . . 119.9 ?
C4 C5 C6 . . 120.8(5) ?
C4 C5 H5A . . 119.6 ?
C6 C5 H5A . . 119.6 ?
C5 C6 C7 . . 120.0(5) ?
C5 C6 H6A . . 120.0 ?
C7 C6 H6A . . 120.0 ?
C6 C7 C2 . . 120.0(5) ?
C6 C7 H7A . . 120.0 ?
C2 C7 H7A . . 120.0 ?
O4 C8 O3 . . 122.7(5) ?
O4 C8 C9 . . 120.2(4) ?
O3 C8 C9 . . 117.0(4) ?
C14 C9 C10 . . 118.4(4) ?
C14 C9 C8 . . 120.5(4) ?
C10 C9 C8 . . 121.0(4) ?
C11 C10 C9 . . 121.1(5) ?
C11 C10 H10A . . 119.5 ?
C9 C10 H10A . . 119.5 ?
C10 C11 C12 . . 120.4(5) ?
C10 C11 H11A . . 119.8 ?
C12 C11 H11A . . 119.8 ?
C11 C12 C13 . . 119.7(5) ?
C11 C12 H12A . . 120.1 ?
C13 C12 H12A . . 120.1 ?
C12 C13 C14 . . 120.1(5) ?
C12 C13 H13A . . 120.0 ?
C14 C13 H13A . . 120.0 ?
C9 C14 C13 . . 120.2(5) ?
C9 C14 H14A . . 119.9 ?
C13 C14 H14A . . 119.9 ?
N1 C15 C16 . . 124.2(5) ?
N1 C15 H15A . . 117.9 ?
C16 C15 H15A . . 117.9 ?
C17 C16 C15 . . 118.4(5) ?
C17 C16 H16A . . 120.8 ?
C15 C16 H16A . . 120.8 ?
C16 C17 C18 . . 120.3(5) ?
C16 C17 H17A . . 119.8 ?
C18 C17 H17A . . 119.8 ?
C17 C18 C26 . . 117.1(4) ?
C17 C18 C19 . . 123.0(4) ?
C26 C18 C19 . . 119.8(4) ?
C20 C19 C18 . . 121.2(4) ?
C20 C19 H19A . . 119.4 ?
C18 C19 H19A . . 119.4 ?
C19 C20 C21 . . 120.7(4) ?
C19 C20 H20A . . 119.6 ?
C21 C20 H20A . . 119.6 ?
C22 C21 C25 . . 117.9(4) ?
C22 C21 C20 . . 121.9(4) ?
C25 C21 C20 . . 120.2(4) ?
C23 C22 C21 . . 119.9(4) ?
C23 C22 H22A . . 120.1 ?
C21 C22 H22A . . 120.1 ?
C22 C23 C24 . . 119.0(5) ?
C22 C23 H23A . . 120.5 ?
C24 C23 H23A . . 120.5 ?
N2 C24 C23 . . 122.9(5) ?
N2 C24 H24A . . 118.6 ?
C23 C24 H24A . . 118.6 ?
N2 C25 C21 . . 122.5(4) ?
N2 C25 C26 . . 118.7(4) ?
C21 C25 C26 . . 118.8(4) ?
N1 C26 C18 . . 122.5(4) ?
N1 C26 C25 . . 118.2(4) ?
C18 C26 C25 . . 119.2(4) ?
O6 C27 O5 . . 123.2(6) ?
O6 C27 C28 . . 124.0(5) ?
O5 C27 C28 . . 112.8(5) ?
C33 C28 C29 . . 118.9(6) ?
C33 C28 C27 . . 122.5(5) ?
C29 C28 C27 . . 118.6(5) ?
C28 C29 C30 . . 120.6(6) ?
C28 C29 H29A . . 119.7 ?
C30 C29 H29A . . 119.7 ?
C31 C30 C29 . . 120.5(7) ?
C31 C30 H30A . . 119.7 ?
C29 C30 H30A . . 119.7 ?
C30 C31 C32 . . 119.0(7) ?
C30 C31 H31A . . 120.5 ?
C32 C31 H31A . . 120.5 ?
C31 C32 C33 . . 121.2(7) ?
C31 C32 H32A . . 119.4 ?
C33 C32 H32A . . 119.4 ?
C28 C33 C32 . . 119.8(6) ?
C28 C33 H33A . . 120.1 ?
C32 C33 H33A . . 120.1 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pb1 O1 . 2.337(3) y
Pb1 O3 . 2.361(4) y
Pb1 N2 . 2.564(3) y
Pb1 N1 . 2.632(4) y
Pb1 O2 . 2.822(3) y
Pb1 O4 . 2.928(4) y
O1 C1 . 1.269(6) ?
O2 C1 . 1.259(6) ?
O3 C8 . 1.269(5) ?
O4 C8 . 1.250(5) ?
O5 C27 . 1.303(6) ?
O5 H5 . 0.8200 ?
O6 C27 . 1.199(6) ?
N1 C15 . 1.320(6) ?
N1 C26 . 1.356(6) ?
N2 C24 . 1.327(6) ?
N2 C25 . 1.367(5) ?
C1 C2 . 1.485(7) ?
C2 C3 . 1.384(7) ?
C2 C7 . 1.393(7) ?
C3 C4 . 1.384(7) ?
C3 H3A . 0.9300 ?
C4 C5 . 1.358(8) ?
C4 H4A . 0.9300 ?
C5 C6 . 1.365(8) ?
C5 H5A . 0.9300 ?
C6 C7 . 1.381(8) ?
C6 H6A . 0.9300 ?
C7 H7A . 0.9300 ?
C8 C9 . 1.488(7) ?
C9 C14 . 1.380(6) ?
C9 C10 . 1.385(6) ?
C10 C11 . 1.361(7) ?
C10 H10A . 0.9300 ?
C11 C12 . 1.366(8) ?
C11 H11A . 0.9300 ?
C12 C13 . 1.374(8) ?
C12 H12A . 0.9300 ?
C13 C14 . 1.384(7) ?
C13 H13A . 0.9300 ?
C14 H14A . 0.9300 ?
C15 C16 . 1.373(7) ?
C15 H15A . 0.9300 ?
C16 C17 . 1.365(7) ?
C16 H16A . 0.9300 ?
C17 C18 . 1.391(7) ?
C17 H17A . 0.9300 ?
C18 C26 . 1.401(6) ?
C18 C19 . 1.422(6) ?
C19 C20 . 1.335(7) ?
C19 H19A . 0.9300 ?
C20 C21 . 1.429(6) ?
C20 H20A . 0.9300 ?
C21 C22 . 1.397(6) ?
C21 C25 . 1.397(6) ?
C22 C23 . 1.359(8) ?
C22 H22A . 0.9300 ?
C23 C24 . 1.407(7) ?
C23 H23A . 0.9300 ?
C24 H24A . 0.9300 ?
C25 C26 . 1.445(6) ?
C27 C28 . 1.495(8) ?
C28 C33 . 1.363(7) ?
C28 C29 . 1.372(8) ?
C29 C30 . 1.377(10) ?
C29 H29A . 0.9300 ?
C30 C31 . 1.348(10) ?
C30 H30A . 0.9300 ?
C31 C32 . 1.365(10) ?
C31 H31A . 0.9300 ?
C32 C33 . 1.377(9) ?
C32 H32A . 0.9300 ?
C33 H33A . 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
_geom_hbond_publ_flag
O5 H5 O2 . 0.82 1.94 2.654(5) 145 y
