#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/38/2203809.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_2203809
loop_
_publ_author_name
'Hong-Ping Xiao'
'Nan-Wen Zhu'
'Mao-Lin Hu'
_publ_section_title
Bis(μ-4-nitrophenolato-κ²O:O')bis[(2,2'-bipyridine-κ²N,N')nitratolead(II)]
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m800
_journal_page_last               m801
_journal_paper_doi               10.1107/S1600536804011419
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Pb2 (C6 H4 N O3)2 (C10 H8 N2)2 (N O3)2]'
_chemical_formula_moiety         'C32 H24 N8 O12 Pb2'
_chemical_formula_sum            'C32 H24 N8 O12 Pb2'
_chemical_formula_weight         1126.97
_chemical_name_systematic
Bis(μ-4-nitrophenolato-κ²O:O')bis[(2,2'-bipyridine-κ²N,N')nitrolead(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                91.4770(10)
_cell_angle_beta                 111.1070(10)
_cell_angle_gamma                109.9290(10)
_cell_formula_units_Z            1
_cell_length_a                   8.646(5)
_cell_length_b                   10.5079(6)
_cell_length_c                   10.7934(6)
_cell_measurement_reflns_used    4967
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.21
_cell_measurement_theta_min      2.67
_cell_volume                     847.6(5)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'XP (Bruker, 2002)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART APEX 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  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6259
_diffrn_reflns_theta_full        25.23
_diffrn_reflns_theta_max         25.23
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.996
_exptl_absorpt_correction_T_max  0.2104
_exptl_absorpt_correction_T_min  0.0613
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.208
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.963
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3047
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0213P)²+0.5091P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0516
_refine_ls_wR_factor_ref         0.0523
_reflns_number_gt                2909
_reflns_number_total             3047
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            su6103.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.

'_exptl_absorpt_correction_type' value 'Integration' changed
to 'integration' 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.

'_exptl_absorpt_correction_type' value 'Integration'
changed to 'integration' 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               2203809
_cod_database_fobs_code          2203809
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_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_type_symbol
Pb1 0.81434(2) 0.994827(17) 0.077745(16) 0.03365(7) Uani d . 1 Pb
O1 0.9527(4) 0.8645(3) 0.0140(3) 0.0368(7) Uani d . 1 O
O2 0.9344(6) 0.3008(4) 0.1893(5) 0.0672(12) Uani d . 1 O
O3 1.2037(7) 0.4320(4) 0.3208(5) 0.0769(13) Uani d . 1 O
O4 0.5348(5) 0.7799(4) -0.0956(4) 0.0703(12) Uani d . 1 O
O5 0.3390(6) 0.7409(4) -0.2975(4) 0.0663(11) Uani d . 1 O
O6 0.4564(6) 0.9430(4) -0.1776(4) 0.0698(12) Uani d . 1 O
N1 1.0556(7) 0.4140(5) 0.2335(5) 0.0481(11) Uani d . 1 N
N2 0.7670(5) 0.8205(4) 0.2343(4) 0.0357(9) Uani d . 1 N
N3 1.0813(5) 1.0326(4) 0.2940(4) 0.0344(9) Uani d . 1 N
N4 0.4421(6) 0.8205(5) -0.1915(4) 0.0458(10) Uani d . 1 N
C1 0.9761(6) 0.7565(4) 0.0684(4) 0.0314(10) Uani d . 1 C
C2 0.8335(6) 0.6306(5) 0.0367(5) 0.0372(11) Uani d . 1 C
H2 0.7201 0.6221 -0.0226 0.045 Uiso calc R 1 H
C3 0.8579(6) 0.5192(5) 0.0916(4) 0.0378(11) Uani d . 1 C
H3 0.7622 0.4357 0.0699 0.045 Uiso calc R 1 H
C4 1.0267(6) 0.5329(4) 0.1794(5) 0.0346(10) Uani d . 1 C
C5 1.1699(7) 0.6551(5) 0.2134(5) 0.0393(11) Uani d . 1 C
H5 1.2824 0.6624 0.2734 0.047 Uiso calc R 1 H
C6 1.1458(6) 0.7659(5) 0.1585(5) 0.0358(10) Uani d . 1 C
H6 1.2428 0.8487 0.1810 0.043 Uiso calc R 1 H
C7 0.6120(7) 0.7139(5) 0.1979(5) 0.0477(13) Uani d . 1 C
H7 0.5138 0.7144 0.1248 0.057 Uiso calc R 1 H
C8 0.5921(8) 0.6036(6) 0.2643(6) 0.0572(15) Uani d . 1 C
H8 0.4825 0.5306 0.2361 0.069 Uiso calc R 1 H
C9 0.7350(9) 0.6025(6) 0.3722(6) 0.0591(16) Uani d . 1 C
H9 0.7247 0.5278 0.4173 0.071 Uiso calc R 1 H
C10 0.8945(8) 0.7131(5) 0.4135(5) 0.0499(13) Uani d . 1 C
H10 0.9928 0.7149 0.4880 0.060 Uiso calc R 1 H
C11 0.9073(6) 0.8218(5) 0.3430(4) 0.0348(10) Uani d . 1 C
C12 1.0750(6) 0.9442(5) 0.3817(4) 0.0311(10) Uani d . 1 C
C13 1.2211(7) 0.9662(5) 0.4999(5) 0.0427(12) Uani d . 1 C
H13 1.2159 0.9040 0.5594 0.051 Uiso calc R 1 H
C14 1.3741(7) 1.0803(6) 0.5296(5) 0.0481(13) Uani d . 1 C
H14 1.4722 1.0972 0.6102 0.058 Uiso calc R 1 H
C15 1.3803(7) 1.1696(6) 0.4382(5) 0.0482(13) Uani d . 1 C
H15 1.4831 1.2468 0.4551 0.058 Uiso calc R 1 H
C16 1.2314(7) 1.1417(5) 0.3221(5) 0.0414(11) Uani d . 1 C
H16 1.2352 1.2015 0.2603 0.050 Uiso calc R 1 H
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 N3 . . 78.42(12) yes
O1 Pb1 N2 . . 84.12(11) yes
N3 Pb1 N2 . . 64.26(12) yes
O1 Pb1 O1 . 2_775 67.41(12) yes
N3 Pb1 O1 . 2_775 85.27(11) yes
N2 Pb1 O1 . 2_775 142.17(11) yes
O1 Pb1 O4 . . 77.28(13) yes
N3 Pb1 O4 . . 137.30(12) yes
N2 Pb1 O4 . . 78.73(12) yes
O1 Pb1 O4 2_775 . 116.19(12) yes
C1 O1 Pb1 . . 124.2(3) ?
C1 O1 Pb1 . 2_775 117.2(3) ?
Pb1 O1 Pb1 . 2_775 112.59(12) ?
N4 O4 Pb1 . . 110.3(3) ?
O2 N1 O3 . . 123.0(5) ?
O2 N1 C4 . . 119.1(5) ?
O3 N1 C4 . . 117.9(5) ?
C7 N2 C11 . . 118.7(4) ?
C7 N2 Pb1 . . 120.5(3) ?
C11 N2 Pb1 . . 119.8(3) ?
C16 N3 C12 . . 119.1(4) ?
C16 N3 Pb1 . . 119.7(3) ?
C12 N3 Pb1 . . 121.2(3) ?
O5 N4 O4 . . 120.2(5) ?
O5 N4 O6 . . 121.0(5) ?
O4 N4 O6 . . 118.8(5) ?
O1 C1 C2 . . 121.1(4) ?
O1 C1 C6 . . 120.9(4) ?
C2 C1 C6 . . 118.0(4) ?
C3 C2 C1 . . 121.1(4) ?
C3 C2 H2 . . 119.5 ?
C1 C2 H2 . . 119.5 ?
C2 C3 C4 . . 119.0(4) ?
C2 C3 H3 . . 120.5 ?
C4 C3 H3 . . 120.5 ?
C5 C4 C3 . . 121.6(4) ?
C5 C4 N1 . . 118.9(4) ?
C3 C4 N1 . . 119.4(4) ?
C6 C5 C4 . . 119.4(4) ?
C6 C5 H5 . . 120.3 ?
C4 C5 H5 . . 120.3 ?
C5 C6 C1 . . 120.8(4) ?
C5 C6 H6 . . 119.6 ?
C1 C6 H6 . . 119.6 ?
N2 C7 C8 . . 122.5(5) ?
N2 C7 H7 . . 118.8 ?
C8 C7 H7 . . 118.8 ?
C9 C8 C7 . . 119.2(5) ?
C9 C8 H8 . . 120.4 ?
C7 C8 H8 . . 120.4 ?
C8 C9 C10 . . 119.2(5) ?
C8 C9 H9 . . 120.4 ?
C10 C9 H9 . . 120.4 ?
C9 C10 C11 . . 119.2(5) ?
C9 C10 H10 . . 120.4 ?
C11 C10 H10 . . 120.4 ?
N2 C11 C10 . . 121.2(5) ?
N2 C11 C12 . . 116.6(4) ?
C10 C11 C12 . . 122.2(4) ?
N3 C12 C13 . . 120.7(4) ?
N3 C12 C11 . . 116.9(4) ?
C13 C12 C11 . . 122.3(4) ?
C14 C13 C12 . . 119.9(5) ?
C14 C13 H13 . . 120.1 ?
C12 C13 H13 . . 120.1 ?
C13 C14 C15 . . 119.1(5) ?
C13 C14 H14 . . 120.5 ?
C15 C14 H14 . . 120.5 ?
C16 C15 C14 . . 118.4(5) ?
C16 C15 H15 . . 120.8 ?
C14 C15 H15 . . 120.8 ?
N3 C16 C15 . . 122.8(5) ?
N3 C16 H16 . . 118.6 ?
C15 C16 H16 . . 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(3) yes
Pb1 N3 . 2.526(4) yes
Pb1 N2 . 2.554(4) yes
Pb1 O1 2_775 2.590(3) yes
Pb1 O4 . 2.692(4) yes
O1 C1 . 1.334(5) ?
O1 Pb1 2_775 2.590(3) ?
O2 N1 . 1.226(6) ?
O3 N1 . 1.233(6) ?
O4 N4 . 1.246(5) ?
O5 N4 . 1.229(5) ?
O6 N4 . 1.250(6) ?
N1 C4 . 1.452(6) ?
N2 C7 . 1.334(6) ?
N2 C11 . 1.346(6) ?
N3 C16 . 1.332(6) ?
N3 C12 . 1.345(6) ?
C1 C2 . 1.396(6) ?
C1 C6 . 1.405(6) ?
C2 C3 . 1.371(6) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.379(7) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.371(7) ?
C5 C6 . 1.365(6) ?
C5 H5 . 0.9300 ?
C6 H6 . 0.9300 ?
C7 C8 . 1.372(8) ?
C7 H7 . 0.9300 ?
C8 C9 . 1.362(8) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.375(8) ?
C9 H9 . 0.9300 ?
C10 C11 . 1.384(7) ?
C10 H10 . 0.9300 ?
C11 C12 . 1.481(7) ?
C12 C13 . 1.379(7) ?
C13 C14 . 1.372(7) ?
C13 H13 . 0.9300 ?
C14 C15 . 1.381(8) ?
C14 H14 . 0.9300 ?
C15 C16 . 1.370(7) ?
C15 H15 . 0.9300 ?
C16 H16 . 0.9300 ?
