#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/05/2220507.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_2220507
loop_
_publ_author_name
'Li, Chun-Xiang'
'Zha, Xiao-Lin'
'Liu, Chun-Bo'
'Li, Xiu-Ying'
'Che, Guang-Bo'
_publ_section_title
;
 Bis(imidazo[4,5-f][1,10]phenanthroline)dinitratolead(II)
;
_journal_coeditor_code           HB2871
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m54
_journal_paper_doi               10.1107/S1600536808041317
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Pb (N O3)2 (C13 H8 N4)2]'
_chemical_formula_moiety         'C26 H16 N10 O6 Pb'
_chemical_formula_sum            'C26 H16 N10 O6 Pb'
_chemical_formula_weight         771.68
_chemical_name_systematic
;
Bis(imidazo[4,5-f][1,10]phenanthroline)dinitratolead(II)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 100.48(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.203(4)
_cell_length_b                   7.3948(15)
_cell_length_c                   17.392(4)
_cell_measurement_reflns_used    3904
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      26.09
_cell_measurement_theta_min      2.16
_cell_volume                     2428.5(9)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics    'SHELXS97 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      292(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD'
_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  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10060
_diffrn_reflns_theta_full        26.09
_diffrn_reflns_theta_max         26.09
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.017
_exptl_absorpt_correction_T_max  0.453
_exptl_absorpt_correction_T_min  0.165
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.111
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.626
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         2402
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0304P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0638
_reflns_number_gt                2170
_reflns_number_total             2402
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb2871.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 'Monoclinic' changed to 'monoclinic'
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_original_cell_volume        2428.5(8)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2220507
_cod_database_fobs_code          2220507
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
C C1 0.3676(2) -0.2885(6) 0.1841(2) 0.0361(10) Uani d . 1 . .
H H1 0.3576 -0.2644 0.2334 0.043 Uiso calc R 1 . .
C C2 0.3181(3) -0.3843(7) 0.1316(3) 0.0472(12) Uani d . 1 . .
H H2 0.2772 -0.4283 0.1466 0.057 Uiso calc R 1 . .
C C3 0.3303(2) -0.4130(6) 0.0577(3) 0.0411(11) Uani d . 1 . .
H H3 0.2973 -0.4749 0.0214 0.049 Uiso calc R 1 . .
C C4 0.3927(2) -0.3486(5) 0.0372(2) 0.0270(9) Uani d . 1 . .
C C5 0.4423(2) -0.2606(5) 0.0951(2) 0.0242(8) Uani d . 1 . .
C C6 0.5099(2) -0.1997(5) 0.0783(2) 0.0242(8) Uani d . 1 . .
C C7 0.6190(2) -0.0678(6) 0.1228(3) 0.0329(9) Uani d . 1 . .
H H7 0.6505 -0.0117 0.1627 0.040 Uiso calc R 1 . .
C C8 0.6394(2) -0.0921(6) 0.0507(2) 0.0354(10) Uani d . 1 . .
H H8 0.6845 -0.0580 0.0439 0.043 Uiso calc R 1 . .
C C9 0.4103(2) -0.3613(5) -0.0386(2) 0.0284(9) Uani d . 1 . .
C C10 0.5268(2) -0.2217(5) 0.0028(2) 0.0251(8) Uani d . 1 . .
C C11 0.4729(2) -0.2999(5) -0.0565(2) 0.0272(9) Uani d . 1 . .
C C12 0.4129(3) -0.3952(6) -0.1631(2) 0.0386(11) Uani d . 1 . .
H H12 0.3985 -0.4253 -0.2155 0.046 Uiso calc R 1 . .
C C13 0.5931(2) -0.1660(5) -0.0100(2) 0.0296(9) Uani d . 1 . .
H H13 0.6055 -0.1790 -0.0590 0.035 Uiso calc R 1 . .
N N5 0.2959(2) 0.1066(5) 0.1716(2) 0.0387(9) Uani d . 1 . .
O O2 0.2564(2) 0.0783(8) 0.2184(3) 0.0874(14) Uani d . 1 . .
N N1 0.42843(17) -0.2294(4) 0.16763(18) 0.0268(7) Uani d . 1 . .
N N2 0.55658(17) -0.1214(4) 0.13726(18) 0.0262(7) Uani d . 1 . .
N N3 0.3723(2) -0.4235(5) -0.1083(2) 0.0359(8) Uani d . 1 . .
H H3A 0.3307 -0.4711 -0.1156 0.043 Uiso calc R 1 . .
N N4 0.4751(2) -0.3210(4) -0.13538(18) 0.0341(8) Uani d . 1 . .
O O1 0.35914(17) 0.1449(5) 0.19411(19) 0.0508(9) Uani d . 1 . .
O O3 0.2706(2) 0.0901(7) 0.1014(2) 0.0747(12) Uani d . 1 . .
Pb Pb 0.5000 0.01345(3) 0.2500 0.02722(9) Uani d S 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
N1 C1 C2 . . 123.5(4) ?
N1 C1 H1 . . 118.3 ?
C2 C1 H1 . . 118.3 ?
C3 C2 C1 . . 119.0(4) ?
C3 C2 H2 . . 120.5 ?
C1 C2 H2 . . 120.5 ?
C2 C3 C4 . . 119.4(4) ?
C2 C3 H3 . . 120.3 ?
C4 C3 H3 . . 120.3 ?
C3 C4 C5 . . 118.3(4) ?
C3 C4 C9 . . 125.0(4) ?
C5 C4 C9 . . 116.6(4) ?
N1 C5 C4 . . 121.4(3) ?
N1 C5 C6 . . 118.0(3) ?
C4 C5 C6 . . 120.7(3) ?
N2 C6 C10 . . 121.1(4) ?
N2 C6 C5 . . 118.0(3) ?
C10 C6 C5 . . 120.9(3) ?
N2 C7 C8 . . 122.9(4) ?
N2 C7 H7 . . 118.6 ?
C8 C7 H7 . . 118.6 ?
C13 C8 C7 . . 119.9(4) ?
C13 C8 H8 . . 120.1 ?
C7 C8 H8 . . 120.1 ?
C11 C9 N3 . . 105.0(3) ?
C11 C9 C4 . . 123.6(4) ?
N3 C9 C4 . . 131.4(4) ?
C13 C10 C6 . . 118.9(4) ?
C13 C10 C11 . . 124.2(3) ?
C6 C10 C11 . . 116.9(4) ?
C9 C11 N4 . . 111.8(4) ?
C9 C11 C10 . . 121.0(3) ?
N4 C11 C10 . . 127.1(4) ?
N4 C12 N3 . . 113.9(4) ?
N4 C12 H12 . . 123.0 ?
N3 C12 H12 . . 123.0 ?
C8 C13 C10 . . 118.7(4) ?
C8 C13 H13 . . 120.6 ?
C10 C13 H13 . . 120.6 ?
O2 N5 O3 . . 117.3(4) ?
O2 N5 O1 . . 121.2(4) ?
O3 N5 O1 . . 121.4(4) ?
C1 N1 C5 . . 118.4(3) ?
C1 N1 Pb . . 121.2(3) ?
C5 N1 Pb . . 117.9(2) ?
C7 N2 C6 . . 118.5(3) ?
C7 N2 Pb . . 122.8(3) ?
C6 N2 Pb . . 115.0(2) ?
C12 N3 C9 . . 106.7(4) ?
C12 N3 H3A . . 126.7 ?
C9 N3 H3A . . 126.7 ?
C12 N4 C11 . . 102.6(4) ?
N1 Pb N1 . 2_655 90.01(14) n
N1 Pb N2 . 2_655 84.09(10) ?
N1 Pb N2 2_655 2_655 64.03(10) ?
N1 Pb N2 . . 64.03(10) n
N1 Pb N2 2_655 . 84.09(10) n
N2 Pb N2 2_655 . 135.02(14) n
O1 Pb N1 . . 70.65(10) n
O1 Pb N2 . . 111.75(10) n
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
C1 N1 . 1.327(5) ?
C1 C2 . 1.387(6) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.364(6) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.396(6) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.413(5) ?
C4 C9 . 1.423(5) ?
C5 N1 . 1.355(5) ?
C5 C6 . 1.453(5) ?
C6 N2 . 1.362(5) ?
C6 C10 . 1.418(5) ?
C7 N2 . 1.329(5) ?
C7 C8 . 1.392(6) ?
C7 H7 . 0.9300 ?
C8 C13 . 1.365(6) ?
C8 H8 . 0.9300 ?
C9 C11 . 1.372(6) ?
C9 N3 . 1.376(5) ?
C10 C13 . 1.393(6) ?
C10 C11 . 1.442(5) ?
C11 N4 . 1.390(5) ?
C12 N4 . 1.323(5) ?
C12 N3 . 1.353(6) ?
C12 H12 . 0.9300 ?
C13 H13 . 0.9300 ?
N5 O2 . 1.227(5) ?
N5 O3 . 1.235(5) ?
N5 O1 . 1.239(5) ?
Pb N1 . 2.540(3) y
Pb N2 . 2.606(3) y
Pb O1 . 2.872(5) y
N3 H3A . 0.8600 ?
Pb N1 2_655 2.540(3) ?
Pb N2 2_655 2.606(3) ?
O1 Pb 2_655 2.872(5) ?
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
N3 H3A O3 7_545 0.86 2.19 3.030(6) 165
N3 H3A O2 7_545 0.86 2.35 3.059(6) 140
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N1 C1 C2 C3 . . . . -3.2(7) ?
C1 C2 C3 C4 . . . . 1.2(7) ?
C2 C3 C4 C5 . . . . 2.1(7) ?
C2 C3 C4 C9 . . . . -176.7(4) ?
C3 C4 C5 N1 . . . . -3.8(6) ?
C9 C4 C5 N1 . . . . 175.1(3) ?
C3 C4 C5 C6 . . . . 176.6(4) ?
C9 C4 C5 C6 . . . . -4.5(5) ?
N1 C5 C6 N2 . . . . 2.6(5) ?
C4 C5 C6 N2 . . . . -177.7(3) ?
N1 C5 C6 C10 . . . . -177.6(3) ?
C4 C5 C6 C10 . . . . 2.0(5) ?
N2 C7 C8 C13 . . . . 3.2(7) ?
C3 C4 C9 C11 . . . . -178.6(4) ?
C5 C4 C9 C11 . . . . 2.6(6) ?
C3 C4 C9 N3 . . . . 4.8(7) ?
C5 C4 C9 N3 . . . . -173.9(4) ?
N2 C6 C10 C13 . . . . 1.6(5) ?
C5 C6 C10 C13 . . . . -178.1(3) ?
N2 C6 C10 C11 . . . . -177.7(3) ?
C5 C6 C10 C11 . . . . 2.5(5) ?
N3 C9 C11 N4 . . . . 0.2(4) ?
C4 C9 C11 N4 . . . . -177.1(4) ?
N3 C9 C11 C10 . . . . 179.3(3) ?
C4 C9 C11 C10 . . . . 2.0(6) ?
C13 C10 C11 C9 . . . . 176.2(4) ?
C6 C10 C11 C9 . . . . -4.5(5) ?
C13 C10 C11 N4 . . . . -4.9(6) ?
C6 C10 C11 N4 . . . . 174.4(4) ?
C7 C8 C13 C10 . . . . -2.3(6) ?
C6 C10 C13 C8 . . . . 0.0(6) ?
C11 C10 C13 C8 . . . . 179.3(4) ?
C2 C1 N1 C5 . . . . 1.6(6) ?
C2 C1 N1 Pb . . . . 163.1(4) ?
C4 C5 N1 C1 . . . . 2.0(5) ?
C6 C5 N1 C1 . . . . -178.4(3) ?
C4 C5 N1 Pb . . . . -160.2(3) ?
C6 C5 N1 Pb . . . . 19.5(4) ?
C8 C7 N2 C6 . . . . -1.5(6) ?
C8 C7 N2 Pb . . . . -158.6(3) ?
C10 C6 N2 C7 . . . . -0.9(5) ?
C5 C6 N2 C7 . . . . 178.9(3) ?
C10 C6 N2 Pb . . . . 157.9(3) ?
C5 C6 N2 Pb . . . . -22.3(4) ?
N4 C12 N3 C9 . . . . 0.6(5) ?
C11 C9 N3 C12 . . . . -0.5(4) ?
C4 C9 N3 C12 . . . . 176.5(4) ?
N3 C12 N4 C11 . . . . -0.4(5) ?
C9 C11 N4 C12 . . . . 0.1(4) ?
C10 C11 N4 C12 . . . . -178.9(4) ?
C1 N1 Pb N1 . . . 2_655 93.6(3) ?
C5 N1 Pb N1 . . . 2_655 -104.8(3) ?
C1 N1 Pb N2 . . . 2_655 29.7(3) ?
C5 N1 Pb N2 . . . 2_655 -168.7(3) ?
C1 N1 Pb N2 . . . . 177.0(3) ?
C5 N1 Pb N2 . . . . -21.4(2) ?
C7 N2 Pb N1 . . . . 179.9(3) ?
C6 N2 Pb N1 . . . . 22.2(2) ?
C7 N2 Pb N1 . . . 2_655 -87.2(3) ?
C6 N2 Pb N1 . . . 2_655 115.1(3) ?
C7 N2 Pb N2 . . . 2_655 -130.6(3) ?
C6 N2 Pb N2 . . . 2_655 71.7(2) ?
