#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/52/2225243.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_2225243
loop_
_publ_author_name
'Dai, Jun'
'Yang, Juan'
'Li, Yingjie'
_publ_section_title
(2,2'-Bipyridine-κ²N,N')bis(4-methylbenzoato-κ²O,O')lead(II)
_journal_coeditor_code           GK2256
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m298
_journal_paper_doi               10.1107/S1600536810005544
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Pb (C8 H7 O2)2 (C10 H8 N2)]'
_chemical_formula_moiety         'C26 H22 N2 O4 Pb'
_chemical_formula_sum            'C26 H22 N2 O4 Pb'
_chemical_formula_weight         633.65
_chemical_name_systematic
(2,2'-Bipyridine-κ²N,N')bis(4-methylbenzoato-κ²O,O')lead(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
_cell_angle_alpha                109.8650(10)
_cell_angle_beta                 97.3220(10)
_cell_angle_gamma                90.6430(10)
_cell_formula_units_Z            2
_cell_length_a                   9.5510(11)
_cell_length_b                   10.0805(12)
_cell_length_c                   13.2483(15)
_cell_measurement_reflns_used    7017
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.62
_cell_measurement_theta_min      2.22
_cell_volume                     1187.8(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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'φ and ω 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  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14285
_diffrn_reflns_theta_full        27.75
_diffrn_reflns_theta_max         27.75
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    7.136
_exptl_absorpt_correction_T_max  0.277
_exptl_absorpt_correction_T_min  0.124
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.774
_refine_diff_density_min         -0.763
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         5555
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0229
_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)+(0.0227P)²+0.1400P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0491
_refine_ls_wR_factor_ref         0.0508
_reflns_number_gt                4965
_reflns_number_total             5555
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            gk2256.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2225243
_cod_database_fobs_code          2225243
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 0.010726(12) 0.117736(12) 0.677133(9) 0.03988(5) Uani d U 1 . .
O O1 0.2108(2) 0.1792(2) 0.80800(18) 0.0483(5) Uani d . 1 . .
O O2 0.0648(2) 0.3523(2) 0.84728(18) 0.0543(6) Uani d U 1 . .
O O3 0.1789(3) 0.0320(3) 0.5511(2) 0.0601(6) Uani d . 1 . .
O O4 0.1595(3) 0.2603(2) 0.58236(19) 0.0556(6) Uani d U 1 . .
N N1 -0.0850(3) 0.0481(3) 0.8332(2) 0.0468(6) Uani d . 1 . .
N N2 0.0489(3) -0.1362(3) 0.6814(2) 0.0454(6) Uani d . 1 . .
C C1 0.1748(3) 0.2982(3) 0.8699(3) 0.0413(7) Uani d . 1 . .
C C2 0.2682(3) 0.3698(3) 0.9753(3) 0.0409(7) Uani d . 1 . .
C C3 0.4063(3) 0.3339(3) 0.9934(3) 0.0488(8) Uani d . 1 . .
H H3A 0.4430 0.2632 0.9395 0.059 Uiso calc R 1 . .
C C4 0.4895(4) 0.4025(4) 1.0911(3) 0.0586(10) Uani d . 1 . .
H H4A 0.5825 0.3781 1.1016 0.070 Uiso calc R 1 . .
C C5 0.4386(4) 0.5062(4) 1.1735(3) 0.0559(9) Uani d . 1 . .
C C6 0.3003(4) 0.5395(4) 1.1556(3) 0.0576(9) Uani d . 1 . .
H H6A 0.2630 0.6076 1.2108 0.069 Uiso calc R 1 . .
C C7 0.2156(4) 0.4740(3) 1.0576(3) 0.0470(7) Uani d . 1 . .
H H7A 0.1233 0.5000 1.0470 0.056 Uiso calc R 1 . .
C C8 0.5337(5) 0.5824(5) 1.2781(4) 0.0861(15) Uani d . 1 . .
H H8A 0.5932 0.5164 1.2977 0.129 Uiso calc R 1 . .
H H8B 0.4770 0.6244 1.3343 0.129 Uiso calc R 1 . .
H H8C 0.5913 0.6548 1.2687 0.129 Uiso calc R 1 . .
C C9 0.2085(3) 0.1461(4) 0.5346(3) 0.0449(7) Uani d . 1 . .
C C10 0.3033(3) 0.1363(3) 0.4516(2) 0.0413(7) Uani d . 1 . .
C C11 0.3697(4) 0.0135(4) 0.4040(3) 0.0522(8) Uani d . 1 . .
H H11A 0.3569 -0.0640 0.4254 0.063 Uiso calc R 1 . .
C C12 0.4548(4) 0.0043(4) 0.3251(3) 0.0571(9) Uani d . 1 . .
H H12A 0.4985 -0.0792 0.2947 0.068 Uiso calc R 1 . .
C C13 0.4757(4) 0.1168(4) 0.2909(3) 0.0532(8) Uani d . 1 . .
C C14 0.4090(4) 0.2395(4) 0.3393(3) 0.0662(11) Uani d . 1 . .
H H14A 0.4209 0.3168 0.3173 0.079 Uiso calc R 1 . .
C C15 0.3258(4) 0.2498(4) 0.4188(3) 0.0584(9) Uani d . 1 . .
H H15A 0.2844 0.3342 0.4508 0.070 Uiso calc R 1 . .
C C16 0.5663(5) 0.1044(5) 0.2032(3) 0.0709(11) Uani d . 1 . .
H H16A 0.6455 0.0495 0.2118 0.106 Uiso calc R 1 . .
H H16B 0.5998 0.1970 0.2084 0.106 Uiso calc R 1 . .
H H16C 0.5113 0.0589 0.1335 0.106 Uiso calc R 1 . .
C C17 -0.1533(4) 0.1412(4) 0.9053(3) 0.0553(9) Uani d . 1 . .
H H17A -0.1560 0.2331 0.9046 0.066 Uiso calc R 1 . .
C C18 -0.2200(4) 0.1079(4) 0.9806(3) 0.0599(10) Uani d . 1 . .
H H18A -0.2657 0.1759 1.0301 0.072 Uiso calc R 1 . .
C C19 -0.2174(4) -0.0266(4) 0.9810(3) 0.0640(10) Uani d . 1 . .
H H19A -0.2606 -0.0521 1.0313 0.077 Uiso calc R 1 . .
C C20 -0.1495(4) -0.1250(4) 0.9053(3) 0.0600(10) Uani d . 1 . .
H H20A -0.1487 -0.2182 0.9032 0.072 Uiso calc R 1 . .
C C21 -0.0830(3) -0.0847(3) 0.8330(3) 0.0435(7) Uani d . 1 . .
C C22 -0.0052(3) -0.1848(3) 0.7519(3) 0.0441(7) Uani d . 1 . .
C C23 0.0131(5) -0.3217(4) 0.7493(4) 0.0672(11) Uani d . 1 . .
H H23A -0.0239 -0.3531 0.7993 0.081 Uiso calc R 1 . .
C C24 0.0856(5) -0.4114(4) 0.6734(4) 0.0755(12) Uani d . 1 . .
H H24A 0.0987 -0.5035 0.6713 0.091 Uiso calc R 1 . .
C C25 0.1376(5) -0.3618(4) 0.6014(4) 0.0736(12) Uani d . 1 . .
H H25A 0.1864 -0.4203 0.5485 0.088 Uiso calc R 1 . .
C C26 0.1179(4) -0.2249(4) 0.6073(3) 0.0600(9) Uani d . 1 . .
H H26A 0.1542 -0.1925 0.5575 0.072 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 . . 84.31(9) ?
O1 Pb1 N2 . . 83.74(8) ?
O3 Pb1 N2 . . 77.33(8) ?
O1 Pb1 O2 . . 52.25(7) ?
O3 Pb1 O2 . . 121.72(8) ?
N2 Pb1 O2 . . 124.68(8) ?
O1 Pb1 N1 . . 79.77(8) ?
O3 Pb1 N1 . . 137.27(8) ?
N2 Pb1 N1 . . 61.75(8) ?
O2 Pb1 N1 . . 77.17(8) ?
O1 Pb1 O4 . . 82.72(8) ?
O3 Pb1 O4 . . 50.77(8) ?
N2 Pb1 O4 . . 127.29(8) ?
O2 Pb1 O4 . . 83.26(7) ?
N1 Pb1 O4 . . 159.20(9) ?
C1 O1 Pb1 . . 99.27(19) ?
C1 O2 Pb1 . . 85.80(18) ?
C9 O3 Pb1 . . 99.36(19) ?
C9 O4 Pb1 . . 87.0(2) ?
C17 N1 C21 . . 118.3(3) ?
C17 N1 Pb1 . . 119.9(2) ?
C21 N1 Pb1 . . 121.1(2) ?
C26 N2 C22 . . 118.0(3) ?
C26 N2 Pb1 . . 119.3(2) ?
C22 N2 Pb1 . . 122.6(2) ?
O2 C1 O1 . . 122.5(3) ?
O2 C1 C2 . . 119.8(3) ?
O1 C1 C2 . . 117.7(3) ?
C7 C2 C3 . . 118.6(3) ?
C7 C2 C1 . . 119.6(3) ?
C3 C2 C1 . . 121.8(3) ?
C4 C3 C2 . . 120.3(3) ?
C4 C3 H3A . . 119.9 ?
C2 C3 H3A . . 119.9 ?
C5 C4 C3 . . 121.7(3) ?
C5 C4 H4A . . 119.2 ?
C3 C4 H4A . . 119.2 ?
C4 C5 C6 . . 117.7(3) ?
C4 C5 C8 . . 120.4(4) ?
C6 C5 C8 . . 121.9(4) ?
C5 C6 C7 . . 121.6(3) ?
C5 C6 H6A . . 119.2 ?
C7 C6 H6A . . 119.2 ?
C6 C7 C2 . . 120.1(3) ?
C6 C7 H7A . . 120.0 ?
C2 C7 H7A . . 120.0 ?
C5 C8 H8A . . 109.5 ?
C5 C8 H8B . . 109.5 ?
H8A C8 H8B . . 109.5 ?
C5 C8 H8C . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
O4 C9 O3 . . 122.8(3) ?
O4 C9 C10 . . 120.4(3) ?
O3 C9 C10 . . 116.8(3) ?
C15 C10 C11 . . 118.0(3) ?
C15 C10 C9 . . 120.4(3) ?
C11 C10 C9 . . 121.6(3) ?
C12 C11 C10 . . 121.2(3) ?
C12 C11 H11A . . 119.4 ?
C10 C11 H11A . . 119.4 ?
C13 C12 C11 . . 121.0(3) ?
C13 C12 H12A . . 119.5 ?
C11 C12 H12A . . 119.5 ?
C12 C13 C14 . . 117.4(3) ?
C12 C13 C16 . . 120.5(3) ?
C14 C13 C16 . . 122.1(3) ?
C15 C14 C13 . . 121.8(4) ?
C15 C14 H14A . . 119.1 ?
C13 C14 H14A . . 119.1 ?
C14 C15 C10 . . 120.6(3) ?
C14 C15 H15A . . 119.7 ?
C10 C15 H15A . . 119.7 ?
C13 C16 H16A . . 109.5 ?
C13 C16 H16B . . 109.5 ?
H16A C16 H16B . . 109.5 ?
C13 C16 H16C . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
N1 C17 C18 . . 123.3(3) ?
N1 C17 H17A . . 118.4 ?
C18 C17 H17A . . 118.4 ?
C19 C18 C17 . . 118.5(4) ?
C19 C18 H18A . . 120.7 ?
C17 C18 H18A . . 120.7 ?
C18 C19 C20 . . 118.9(3) ?
C18 C19 H19A . . 120.5 ?
C20 C19 H19A . . 120.5 ?
C21 C20 C19 . . 119.8(3) ?
C21 C20 H20A . . 120.1 ?
C19 C20 H20A . . 120.1 ?
N1 C21 C20 . . 121.1(3) ?
N1 C21 C22 . . 116.7(3) ?
C20 C21 C22 . . 122.2(3) ?
N2 C22 C23 . . 120.9(3) ?
N2 C22 C21 . . 117.2(3) ?
C23 C22 C21 . . 121.9(3) ?
C24 C23 C22 . . 120.4(4) ?
C24 C23 H23A . . 119.8 ?
C22 C23 H23A . . 119.8 ?
C25 C24 C23 . . 118.1(4) ?
C25 C24 H24A . . 120.9 ?
C23 C24 H24A . . 120.9 ?
C24 C25 C26 . . 119.6(4) ?
C24 C25 H25A . . 120.2 ?
C26 C25 H25A . . 120.2 ?
N2 C26 C25 . . 122.9(4) ?
N2 C26 H26A . . 118.6 ?
C25 C26 H26A . . 118.6 ?
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 . 2.333(2) y
Pb1 O3 . 2.418(2) y
Pb1 N2 . 2.608(3) y
Pb1 O2 . 2.644(2) y
Pb1 N1 . 2.656(3) y
Pb1 O4 . 2.701(2) y
O1 C1 . 1.282(4) ?
O2 C1 . 1.239(4) ?
O3 C9 . 1.277(4) ?
O4 C9 . 1.240(4) ?
N1 C17 . 1.335(4) ?
N1 C21 . 1.339(4) ?
N2 C26 . 1.333(4) ?
N2 C22 . 1.345(4) ?
C1 C2 . 1.500(4) ?
C2 C7 . 1.384(4) ?
C2 C3 . 1.385(4) ?
C3 C4 . 1.379(5) ?
C3 H3A . 0.9300 ?
C4 C5 . 1.375(5) ?
C4 H4A . 0.9300 ?
C5 C6 . 1.377(5) ?
C5 C8 . 1.508(5) ?
C6 C7 . 1.383(5) ?
C6 H6A . 0.9300 ?
C7 H7A . 0.9300 ?
C8 H8A . 0.9600 ?
C8 H8B . 0.9600 ?
C8 H8C . 0.9600 ?
C9 C10 . 1.490(4) ?
C10 C15 . 1.379(5) ?
C10 C11 . 1.386(4) ?
C11 C12 . 1.383(5) ?
C11 H11A . 0.9300 ?
C12 C13 . 1.378(5) ?
C12 H12A . 0.9300 ?
C13 C14 . 1.389(5) ?
C13 C16 . 1.509(5) ?
C14 C15 . 1.376(5) ?
C14 H14A . 0.9300 ?
C15 H15A . 0.9300 ?
C16 H16A . 0.9600 ?
C16 H16B . 0.9600 ?
C16 H16C . 0.9600 ?
C17 C18 . 1.378(5) ?
C17 H17A . 0.9300 ?
C18 C19 . 1.358(5) ?
C18 H18A . 0.9300 ?
C19 C20 . 1.384(5) ?
C19 H19A . 0.9300 ?
C20 C21 . 1.378(5) ?
C20 H20A . 0.9300 ?
C21 C22 . 1.486(5) ?
C22 C23 . 1.382(5) ?
C23 C24 . 1.372(6) ?
C23 H23A . 0.9300 ?
C24 C25 . 1.359(6) ?
C24 H24A . 0.9300 ?
C25 C26 . 1.372(5) ?
C25 H25A . 0.9300 ?
C26 H26A . 0.9300 ?
