#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/48/2224819.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_2224819
loop_
_publ_author_name
'Qin, Yan-Tao'
'Tao, Lu'
'He, Tian-Jing'
'Liu, Yan-Cheng'
'Chen, Zhen-Feng'
_publ_section_title
catena-Poly[[(liriodenine-κ²N,O)lead(II)]-di-μ-chlorido]
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m29
_journal_paper_doi               10.1107/S1600536809051381
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Pb Cl2 (C17 H9 N O3)]'
_chemical_formula_moiety         'C17 H9 Cl2 N O3 Pb'
_chemical_formula_sum            'C17 H9 Cl2 N O3 Pb'
_chemical_formula_weight         553.34
_chemical_name_systematic
;
catena-Poly[[(liriodenine-κ²N,O)lead(II)]-
di-μ-chlorido]
;
_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                104.481(6)
_cell_angle_beta                 100.479(4)
_cell_angle_gamma                99.686(4)
_cell_formula_units_Z            2
_cell_length_a                   7.2280(18)
_cell_length_b                   10.332(3)
_cell_length_c                   11.307(3)
_cell_measurement_reflns_used    3068
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.1
_cell_volume                     783.4(4)
_computing_cell_refinement       'CrystalClear (Rigaku, 1999)'
_computing_data_collection       'CrystalClear (Rigaku, 1999)'
_computing_data_reduction
'CrystalStructure (Rigaku/MSC & Rigaku, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_av_sigmaI/netI    0.053
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7685
_diffrn_reflns_theta_full        25.3
_diffrn_reflns_theta_max         25.3
_diffrn_reflns_theta_min         3.1
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.125
_exptl_absorpt_correction_T_max  0.188
_exptl_absorpt_correction_T_min  0.077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(REQAB; Jacobson, 1998)'
_exptl_crystal_colour            brown-red
_exptl_crystal_density_diffrn    2.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.19
_refine_diff_density_min         -1.28
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2847
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.05
_refine_ls_R_factor_all          0.039
_refine_ls_R_factor_gt           0.033
_refine_ls_shift/su_max_lt       0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0269P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.063
_refine_ls_wR_factor_ref         0.065
_reflns_number_gt                2545
_reflns_number_total             2847
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ya2112.cif
_cod_data_source_block           I
_cod_original_cell_volume        783.4(3)
_cod_database_code               2224819
_cod_database_fobs_code          2224819
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 0.19801(4) 0.42620(2) 0.40684(2) 0.03726(11) Uani d . 1 . .
Cl Cl1 -0.1055(3) 0.29827(18) 0.4893(2) 0.0629(6) Uani d . 1 . .
Cl Cl2 0.4274(3) 0.44005(18) 0.62730(15) 0.0502(5) Uani d . 1 . .
O O1 0.1822(7) 0.3210(4) 0.1636(4) 0.0497(12) Uani d . 1 . .
O O2 0.3150(8) -0.4078(5) 0.0294(4) 0.0578(14) Uani d . 1 . .
O O3 0.2905(7) -0.2806(4) -0.1103(4) 0.0480(12) Uani d . 1 . .
N N1 0.2587(7) 0.1823(5) 0.3329(4) 0.0326(12) Uani d . 1 . .
C C1 0.2820(9) 0.1075(7) 0.4135(6) 0.0398(16) Uani d . 1 . .
H H1 0.2900 0.1488 0.4979 0.048 Uiso calc R 1 . .
C C2 0.2945(9) -0.0270(7) 0.3773(6) 0.0395(15) Uani d . 1 . .
H H2 0.3066 -0.0751 0.4366 0.047 Uiso calc R 1 . .
C C3 0.2895(8) -0.0921(6) 0.2529(5) 0.0313(14) Uani d . 1 . .
C C4 0.2695(8) -0.0126(6) 0.1654(5) 0.0273(13) Uani d . 1 . .
C C5 0.2517(8) 0.1231(6) 0.2115(5) 0.0276(13) Uani d . 1 . .
C C6 0.2153(8) 0.2068(6) 0.1253(5) 0.0302(14) Uani d . 1 . .
C C7 0.2194(8) 0.1492(6) -0.0059(5) 0.0303(14) Uani d . 1 . .
C C8 0.1938(9) 0.2315(6) -0.0863(6) 0.0365(15) Uani d . 1 . .
H H8 0.1783 0.3203 -0.0549 0.044 Uiso calc R 1 . .
C C9 0.1914(9) 0.1812(7) -0.2120(6) 0.0420(16) Uani d . 1 . .
H H9 0.1775 0.2360 -0.2655 0.050 Uiso calc R 1 . .
C C10 0.2102(9) 0.0463(7) -0.2573(6) 0.0447(17) Uani d . 1 . .
H H10 0.2059 0.0111 -0.3421 0.054 Uiso calc R 1 . .
C C11 0.2351(9) -0.0361(6) -0.1792(5) 0.0349(15) Uani d . 1 . .
H H11 0.2488 -0.1250 -0.2117 0.042 Uiso calc R 1 . .
C C12 0.2399(7) 0.0135(6) -0.0515(5) 0.0252(13) Uani d . 1 . .
C C13 0.2642(8) -0.0694(6) 0.0357(5) 0.0259(13) Uani d . 1 . .
C C14 0.2808(9) -0.2026(6) 0.0034(6) 0.0360(15) Uani d . 1 . .
C C15 0.2995(9) -0.2795(6) 0.0903(6) 0.0374(15) Uani d . 1 . .
C C16 0.3033(9) -0.2300(6) 0.2118(6) 0.0401(16) Uani d . 1 . .
H H16 0.3144 -0.2837 0.2666 0.048 Uiso calc R 1 . .
C C17 0.2998(14) -0.4135(7) -0.0990(7) 0.066(2) Uani d . 1 . .
H H17A 0.1845 -0.4802 -0.1511 0.079 Uiso calc R 1 . .
H H17B 0.4111 -0.4405 -0.1261 0.079 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'
Cl Cl 0.1484 0.1585 '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 Pb1 O1 . . 61.78(14) ?
N1 Pb1 Cl2 . . 84.80(11) ?
O1 Pb1 Cl2 . . 136.98(11) ?
N1 Pb1 Cl1 . . 84.76(11) ?
O1 Pb1 Cl1 . . 114.05(11) ?
Cl2 Pb1 Cl1 . . 86.77(6) ?
N1 Pb1 Cl2 . 2_666 93.28(11) ?
O1 Pb1 Cl2 . 2_666 75.61(11) ?
Cl2 Pb1 Cl2 . 2_666 80.49(5) ?
Cl1 Pb1 Cl2 . 2_666 167.23(6) ?
N1 Pb1 Cl1 . 2_566 174.35(11) ?
O1 Pb1 Cl1 . 2_566 122.56(10) ?
Cl2 Pb1 Cl1 . 2_566 92.96(6) ?
Cl1 Pb1 Cl1 . 2_566 89.95(5) ?
Cl2 Pb1 Cl1 2_666 2_566 91.45(5) ?
Pb1 Cl1 Pb1 . 2_566 90.05(5) ?
Pb1 Cl2 Pb1 . 2_666 99.51(5) ?
C6 O1 Pb1 . . 120.2(4) ?
C15 O2 C17 . . 107.0(5) ?
C14 O3 C17 . . 107.2(5) ?
C1 N1 C5 . . 118.2(5) ?
C1 N1 Pb1 . . 120.4(4) ?
C5 N1 Pb1 . . 121.2(4) ?
N1 C1 C2 . . 123.1(5) ?
N1 C1 H1 . . 118.5 ?
C2 C1 H1 . . 118.5 ?
C1 C2 C3 . . 120.7(6) ?
C1 C2 H2 . . 119.7 ?
C3 C2 H2 . . 119.7 ?
C2 C3 C16 . . 122.5(5) ?
C2 C3 C4 . . 117.1(5) ?
C16 C3 C4 . . 120.4(5) ?
C5 C4 C13 . . 120.8(5) ?
C5 C4 C3 . . 117.6(5) ?
C13 C4 C3 . . 121.6(5) ?
N1 C5 C4 . . 123.2(5) ?
N1 C5 C6 . . 116.2(5) ?
C4 C5 C6 . . 120.5(5) ?
O1 C6 C7 . . 121.7(5) ?
O1 C6 C5 . . 120.5(5) ?
C7 C6 C5 . . 117.8(5) ?
C8 C7 C12 . . 121.0(5) ?
C8 C7 C6 . . 117.6(5) ?
C12 C7 C6 . . 121.3(5) ?
C9 C8 C7 . . 120.2(6) ?
C9 C8 H8 . . 119.9 ?
C7 C8 H8 . . 119.9 ?
C8 C9 C10 . . 118.7(6) ?
C8 C9 H9 . . 120.6 ?
C10 C9 H9 . . 120.6 ?
C11 C10 C9 . . 121.7(6) ?
C11 C10 H10 . . 119.2 ?
C9 C10 H10 . . 119.2 ?
C10 C11 C12 . . 120.4(6) ?
C10 C11 H11 . . 119.8 ?
C12 C11 H11 . . 119.8 ?
C11 C12 C7 . . 118.0(5) ?
C11 C12 C13 . . 122.9(5) ?
C7 C12 C13 . . 119.1(5) ?
C14 C13 C4 . . 114.7(5) ?
C14 C13 C12 . . 125.1(5) ?
C4 C13 C12 . . 120.3(5) ?
O3 C14 C13 . . 127.8(6) ?
O3 C14 C15 . . 109.0(5) ?
C13 C14 C15 . . 123.1(5) ?
C16 C15 O2 . . 127.3(6) ?
C16 C15 C14 . . 123.8(6) ?
O2 C15 C14 . . 108.8(5) ?
C15 C16 C3 . . 116.5(6) ?
C15 C16 H16 . . 121.8 ?
C3 C16 H16 . . 121.8 ?
O2 C17 O3 . . 107.6(5) ?
O2 C17 H17A . . 110.2 ?
O3 C17 H17A . . 110.2 ?
O2 C17 H17B . . 110.2 ?
O3 C17 H17B . . 110.2 ?
H17A C17 H17B . . 108.5 ?
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 N1 . 2.587(5) ?
Pb1 O1 . 2.666(4) ?
Pb1 Cl2 . 2.6872(18) ?
Pb1 Cl1 . 2.7952(18) ?
Pb1 Cl2 2_666 2.9626(18) ?
Pb1 Cl1 2_566 3.031(2) ?
Cl1 Pb1 2_566 3.031(2) ?
Cl2 Pb1 2_666 2.9626(18) ?
O1 C6 . 1.230(7) ?
O2 C15 . 1.366(7) ?
O2 C17 . 1.422(8) ?
O3 C14 . 1.356(7) ?
O3 C17 . 1.422(8) ?
N1 C1 . 1.340(7) ?
N1 C5 . 1.344(7) ?
C1 C2 . 1.370(9) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.390(8) ?
C2 H2 . 0.9300 ?
C3 C16 . 1.411(8) ?
C3 C4 . 1.438(8) ?
C4 C5 . 1.405(8) ?
C4 C13 . 1.428(7) ?
C5 C6 . 1.474(8) ?
C6 C7 . 1.462(8) ?
C7 C8 . 1.401(8) ?
C7 C12 . 1.411(8) ?
C8 C9 . 1.382(8) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.399(9) ?
C9 H9 . 0.9300 ?
C10 C11 . 1.380(9) ?
C10 H10 . 0.9300 ?
C11 C12 . 1.397(8) ?
C11 H11 . 0.9300 ?
C12 C13 . 1.465(8) ?
C13 C14 . 1.365(8) ?
C14 C15 . 1.412(8) ?
C15 C16 . 1.334(8) ?
C16 H16 . 0.9300 ?
C17 H17A . 0.9700 ?
C17 H17B . 0.9700 ?
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 Pb1 Cl1 Pb1 . . . 2_566 178.04(11) ?
O1 Pb1 Cl1 Pb1 . . . 2_566 -126.08(11) ?
Cl2 Pb1 Cl1 Pb1 . . . 2_566 92.96(6) ?
Cl2 Pb1 Cl1 Pb1 2_666 . . 2_566 96.4(2) ?
Cl1 Pb1 Cl1 Pb1 2_566 . . 2_566 0.0 ?
N1 Pb1 Cl2 Pb1 . . . 2_666 94.22(11) ?
O1 Pb1 Cl2 Pb1 . . . 2_666 56.71(16) ?
Cl1 Pb1 Cl2 Pb1 . . . 2_666 179.24(6) ?
Cl2 Pb1 Cl2 Pb1 2_666 . . 2_666 0.0 ?
Cl1 Pb1 Cl2 Pb1 2_566 . . 2_666 -90.98(6) ?
N1 Pb1 O1 C6 . . . . -1.9(4) ?
Cl2 Pb1 O1 C6 . . . . 41.5(5) ?
Cl1 Pb1 O1 C6 . . . . -71.3(5) ?
Cl2 Pb1 O1 C6 2_666 . . . 99.9(5) ?
Cl1 Pb1 O1 C6 2_566 . . . -177.8(4) ?
O1 Pb1 N1 C1 . . . . -174.8(5) ?
Cl2 Pb1 N1 C1 . . . . 33.3(4) ?
Cl1 Pb1 N1 C1 . . . . -53.9(4) ?
Cl2 Pb1 N1 C1 2_666 . . . 113.5(4) ?
O1 Pb1 N1 C5 . . . . -0.4(4) ?
Cl2 Pb1 N1 C5 . . . . -152.2(4) ?
Cl1 Pb1 N1 C5 . . . . 120.5(4) ?
Cl2 Pb1 N1 C5 2_666 . . . -72.1(4) ?
C5 N1 C1 C2 . . . . -1.5(9) ?
Pb1 N1 C1 C2 . . . . 173.0(5) ?
N1 C1 C2 C3 . . . . 2.0(10) ?
C1 C2 C3 C16 . . . . 179.6(6) ?
C1 C2 C3 C4 . . . . -0.4(9) ?
C2 C3 C4 C5 . . . . -1.6(8) ?
C16 C3 C4 C5 . . . . 178.4(5) ?
C2 C3 C4 C13 . . . . 179.6(5) ?
C16 C3 C4 C13 . . . . -0.4(8) ?
C1 N1 C5 C4 . . . . -0.7(8) ?
Pb1 N1 C5 C4 . . . . -175.2(4) ?
C1 N1 C5 C6 . . . . 176.8(5) ?
Pb1 N1 C5 C6 . . . . 2.2(7) ?
C13 C4 C5 N1 . . . . -179.0(5) ?
C3 C4 C5 N1 . . . . 2.2(8) ?
C13 C4 C5 C6 . . . . 3.7(8) ?
C3 C4 C5 C6 . . . . -175.1(5) ?
Pb1 O1 C6 C7 . . . . -176.2(4) ?
Pb1 O1 C6 C5 . . . . 3.9(7) ?
N1 C5 C6 O1 . . . . -4.1(8) ?
C4 C5 C6 O1 . . . . 173.4(5) ?
N1 C5 C6 C7 . . . . 176.0(5) ?
C4 C5 C6 C7 . . . . -6.5(8) ?
O1 C6 C7 C8 . . . . 3.1(9) ?
C5 C6 C7 C8 . . . . -177.1(5) ?
O1 C6 C7 C12 . . . . -174.1(5) ?
C5 C6 C7 C12 . . . . 5.7(8) ?
C12 C7 C8 C9 . . . . -1.1(9) ?
C6 C7 C8 C9 . . . . -178.3(6) ?
C7 C8 C9 C10 . . . . 1.6(9) ?
C8 C9 C10 C11 . . . . -1.4(10) ?
C9 C10 C11 C12 . . . . 0.8(10) ?
C10 C11 C12 C7 . . . . -0.3(8) ?
C10 C11 C12 C13 . . . . 179.4(6) ?
C8 C7 C12 C11 . . . . 0.4(8) ?
C6 C7 C12 C11 . . . . 177.6(5) ?
C8 C7 C12 C13 . . . . -179.3(5) ?
C6 C7 C12 C13 . . . . -2.2(8) ?
C5 C4 C13 C14 . . . . -179.2(5) ?
C3 C4 C13 C14 . . . . -0.5(8) ?
C5 C4 C13 C12 . . . . 0.0(8) ?
C3 C4 C13 C12 . . . . 178.8(5) ?
C11 C12 C13 C14 . . . . -1.3(9) ?
C7 C12 C13 C14 . . . . 178.4(5) ?
C11 C12 C13 C4 . . . . 179.5(5) ?
C7 C12 C13 C4 . . . . -0.8(8) ?
C17 O3 C14 C13 . . . . -177.9(7) ?
C17 O3 C14 C15 . . . . 4.7(7) ?
C4 C13 C14 O3 . . . . -176.3(6) ?
C12 C13 C14 O3 . . . . 4.5(10) ?
C4 C13 C14 C15 . . . . 0.8(9) ?
C12 C13 C14 C15 . . . . -178.5(6) ?
C17 O2 C15 C16 . . . . 179.0(7) ?
C17 O2 C15 C14 . . . . -1.8(8) ?
O3 C14 C15 C16 . . . . 177.3(6) ?
C13 C14 C15 C16 . . . . -0.2(10) ?
O3 C14 C15 O2 . . . . -1.8(7) ?
C13 C14 C15 O2 . . . . -179.4(6) ?
O2 C15 C16 C3 . . . . 178.3(6) ?
C14 C15 C16 C3 . . . . -0.7(10) ?
C2 C3 C16 C15 . . . . -179.0(6) ?
C4 C3 C16 C15 . . . . 0.9(9) ?
C15 O2 C17 O3 . . . . 4.7(8) ?
C14 O3 C17 O2 . . . . -5.8(8) ?
