#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/24/2232469.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_2232469
loop_
_publ_author_name
'Shahverdizadeh, Gholam Hossein'
'Ng, Seik Weng'
'Tiekink, Edward R. T.'
'Mirtamizdoust, Babak'
_publ_section_title
;
 catena-Poly[[lead(II)-μ-(2-oxidobenzaldehyde
 isonicotinoylhydrazonato)] methanol monosolvate]
;
_journal_coeditor_code           SU2329
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1583
_journal_paper_doi               10.1107/S1600536811043078
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Pb (C13 H9 N3 O2)], C H4 O'
_chemical_formula_moiety         'C13 H9 N3 O2 Pb, C H4 O'
_chemical_formula_sum            'C14 H13 N3 O3 Pb'
_chemical_formula_weight         478.46
_chemical_name_systematic
;
catena-Poly[[lead(II)-μ-(2-oxidobenzaldehyde
isonicotinoylhydrazonato)] methanol monosolvate]
;
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   28.6702(5)
_cell_length_b                   28.6702(5)
_cell_length_c                   9.0146(2)
_cell_measurement_reflns_used    12065
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.2941
_cell_measurement_theta_min      2.3988
_cell_volume                     6417.1(2)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2010)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2010)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2010)'
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg, 2006)
;
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4041
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'Agilent SuperNova Dual diffractometer with an Atlas detector'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  Mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0169
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            17626
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.40
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.844
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.34874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Agilent, 2010)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4032
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.950
_refine_diff_density_min         -0.600
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2958
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0161
_refine_ls_R_factor_gt           0.0146
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0114P)²+19.9099P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0318
_refine_ls_wR_factor_ref         0.0322
_reflns_number_gt                2816
_reflns_number_total             2958
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            su2329.cif
_cod_data_source_block           I
_cod_original_cell_volume        6417.1(3)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               2232469
_cod_database_fobs_code          2232469
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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_symmetry_multiplicity
Pb Pb 0.172066(4) 0.851864(4) 1.061072(10) 0.01156(4) Uani d . 1 1
O O1 0.09837(8) 0.86813(8) 1.0476(2) 0.0186(4) Uani d . 1 1
O O2 0.25307(7) 0.88497(8) 1.19856(19) 0.0147(4) Uani d . 1 1
O O3 0.08109(8) 0.83045(11) 0.7716(2) 0.0318(6) Uani d . 1 1
H H3o 0.0854 0.8444 0.8561 0.051(12) Uiso calc R 1 1
N N1 0.17051(9) 0.89277(9) 1.2955(2) 0.0119(4) Uani d . 1 1
N N2 0.21170(9) 0.90223(9) 1.3966(2) 0.0118(5) Uani d . 1 1
N N3 0.39001(9) 0.94432(9) 1.6044(2) 0.0152(5) Uani d . 1 1
C C1 0.07467(11) 0.88735(11) 1.1315(3) 0.0144(6) Uani d . 1 1
C C2 0.03012(11) 0.89079(11) 1.0785(3) 0.0189(6) Uani d . 1 1
H H2 0.0177 0.8792 0.9803 0.023 Uiso calc R 1 1
C C3 0.00415(12) 0.91040(12) 1.1650(3) 0.0227(6) Uani d . 1 1
H H3 -0.0252 0.9129 1.1248 0.027 Uiso calc R 1 1
C C4 0.02038(12) 0.92671(13) 1.3109(3) 0.0242(7) Uani d . 1 1
H H4 0.0025 0.9403 1.3702 0.029 Uiso calc R 1 1
C C5 0.06267(12) 0.92271(12) 1.3669(3) 0.0207(6) Uani d . 1 1
H H5 0.0733 0.9330 1.4669 0.025 Uiso calc R 1 1
C C6 0.09089(11) 0.90384(11) 1.2809(3) 0.0145(6) Uani d . 1 1
C C7 0.13591(11) 0.90432(11) 1.3515(3) 0.0141(5) Uani d . 1 1
H H7 0.1411 0.9145 1.4531 0.017 Uiso calc R 1 1
C C8 0.25097(10) 0.89833(10) 1.3328(3) 0.0119(5) Uani d . 1 1
C C9 0.38059(11) 0.91341(11) 1.4841(3) 0.0146(5) Uani d . 1 1
H H9 0.4057 0.9022 1.4592 0.017 Uiso calc R 1 1
C C10 0.33565(10) 0.89697(10) 1.3940(3) 0.0130(5) Uani d . 1 1
H H10 0.3306 0.8756 1.3084 0.016 Uiso calc R 1 1
C C11 0.29821(10) 0.91231(10) 1.4312(3) 0.0116(5) Uani d . 1 1
C C12 0.30750(11) 0.94353(11) 1.5581(3) 0.0170(6) Uani d . 1 1
H H12 0.2822 0.9539 1.5884 0.020 Uiso calc R 1 1
C C13 0.35383(12) 0.95919(12) 1.6392(3) 0.0197(6) Uani d . 1 1
H H13 0.3604 0.9815 1.7235 0.024 Uiso calc R 1 1
C C14 0.02725(13) 0.81018(16) 0.7254(4) 0.0360(9) Uani d . 1 1
H H14A 0.0034 0.7974 0.8120 0.054 Uiso calc R 1 1
H H14B 0.0171 0.7802 0.6562 0.054 Uiso calc R 1 1
H H14C 0.0239 0.8388 0.6759 0.054 Uiso calc R 1 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_3
_geom_angle
O2 Pb O1 . 137.27(6)
O2 Pb N1 . 66.59(7)
O1 Pb N1 . 73.59(7)
O2 Pb N3 6_464 83.72(7)
O1 Pb N3 6_464 82.01(7)
N1 Pb N3 6_464 90.94(7)
C1 O1 Pb . 138.69(17)
C8 O2 Pb . 115.50(16)
C14 O3 H3o . 109.5
C7 N1 N2 . 112.0(2)
C7 N1 Pb . 131.62(18)
N2 N1 Pb . 116.13(15)
C8 N2 N1 . 111.8(2)
C9 N3 C13 . 117.9(2)
C9 N3 Pb 8_665 119.49(17)
C13 N3 Pb 8_665 121.59(18)
O1 C1 C2 . 120.8(2)
O1 C1 C6 . 122.2(2)
C2 C1 C6 . 116.9(2)
C3 C2 C1 . 122.0(3)
C3 C2 H2 . 119.0
C1 C2 H2 . 119.0
C2 C3 C4 . 120.8(3)
C2 C3 H3 . 119.6
C4 C3 H3 . 119.6
C5 C4 C3 . 118.7(3)
C5 C4 H4 . 120.6
C3 C4 H4 . 120.6
C4 C5 C6 . 122.1(3)
C4 C5 H5 . 119.0
C6 C5 H5 . 119.0
C5 C6 C1 . 119.5(3)
C5 C6 C7 . 116.0(2)
C1 C6 C7 . 124.5(2)
N1 C7 C6 . 128.7(2)
N1 C7 H7 . 115.6
C6 C7 H7 . 115.6
O2 C8 N2 . 127.5(2)
O2 C8 C11 . 118.0(2)
N2 C8 C11 . 114.6(2)
N3 C9 C10 . 122.9(3)
N3 C9 H9 . 118.6
C10 C9 H9 . 118.6
C11 C10 C9 . 118.9(2)
C11 C10 H10 . 120.6
C9 C10 H10 . 120.6
C10 C11 C12 . 118.2(2)
C10 C11 C8 . 120.7(2)
C12 C11 C8 . 121.0(2)
C13 C12 C11 . 119.2(3)
C13 C12 H12 . 120.4
C11 C12 H12 . 120.4
N3 C13 C12 . 123.0(3)
N3 C13 H13 . 118.5
C12 C13 H13 . 118.5
O3 C14 H14A . 109.5
O3 C14 H14B . 109.5
H14A C14 H14B . 109.5
O3 C14 H14C . 109.5
H14A C14 H14C . 109.5
H14B C14 H14C . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Pb O1 . 2.3837(19)
Pb O2 . 2.3721(18)
Pb N1 . 2.428(2)
Pb N3 6_464 2.530(2)
O1 C1 . 1.308(3)
O2 C8 . 1.280(3)
O3 C14 . 1.413(4)
O3 H3o . 0.8400
N1 C7 . 1.295(3)
N1 N2 . 1.406(3)
N2 C8 . 1.318(3)
N3 C9 . 1.340(3)
N3 C13 . 1.341(4)
N3 Pb 8_665 2.530(2)
C1 C2 . 1.412(4)
C1 C6 . 1.426(4)
C2 C3 . 1.377(4)
C2 H2 . 0.9500
C3 C4 . 1.395(4)
C3 H3 . 0.9500
C4 C5 . 1.370(4)
C4 H4 . 0.9500
C5 C6 . 1.410(4)
C5 H5 . 0.9500
C6 C7 . 1.433(4)
C7 H7 . 0.9500
C8 C11 . 1.497(4)
C9 C10 . 1.391(4)
C9 H9 . 0.9500
C10 C11 . 1.389(4)
C10 H10 . 0.9500
C11 C12 . 1.393(4)
C12 C13 . 1.380(4)
C12 H12 . 0.9500
C13 H13 . 0.9500
C14 H14A . 0.9800
C14 H14B . 0.9800
C14 H14C . 0.9800
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O3 H3o O1 0.84 1.82 2.659(3) 172
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
O2 Pb O1 C1 . -23.4(3)
N1 Pb O1 C1 . -1.6(3)
N3 Pb O1 C1 6_464 -95.0(3)
O1 Pb O2 C8 . 34.3(2)
N1 Pb O2 C8 . 11.55(17)
N3 Pb O2 C8 6_464 105.32(18)
O2 Pb N1 C7 . 172.3(3)
O1 Pb N1 C7 . 8.1(2)
N3 Pb N1 C7 6_464 89.5(2)
O2 Pb N1 N2 . -13.71(15)
O1 Pb N1 N2 . -177.83(18)
N3 Pb N1 N2 6_464 -96.45(17)
C7 N1 N2 C8 . -170.4(2)
Pb N1 N2 C8 . 14.4(3)
Pb O1 C1 C2 . 179.32(19)
Pb O1 C1 C6 . -3.1(4)
O1 C1 C2 C3 . 179.4(3)
C6 C1 C2 C3 . 1.7(4)
C1 C2 C3 C4 . -1.4(5)
C2 C3 C4 C5 . -0.2(5)
C3 C4 C5 C6 . 1.5(5)
C4 C5 C6 C1 . -1.2(4)
C4 C5 C6 C7 . 177.0(3)
O1 C1 C6 C5 . -178.1(3)
C2 C1 C6 C5 . -0.4(4)
O1 C1 C6 C7 . 3.9(4)
C2 C1 C6 C7 . -178.4(3)
N2 N1 C7 C6 . 175.1(3)
Pb N1 C7 C6 . -10.7(4)
C5 C6 C7 N1 . -174.9(3)
C1 C6 C7 N1 . 3.1(5)
Pb O2 C8 N2 . -9.3(3)
Pb O2 C8 C11 . 171.80(17)
N1 N2 C8 O2 . -3.6(4)
N1 N2 C8 C11 . 175.3(2)
C13 N3 C9 C10 . 0.9(4)
Pb N3 C9 C10 8_665 -167.6(2)
N3 C9 C10 C11 . -1.2(4)
C9 C10 C11 C12 . -0.1(4)
C9 C10 C11 C8 . 176.4(2)
O2 C8 C11 C10 . -17.9(4)
N2 C8 C11 C10 . 163.1(2)
O2 C8 C11 C12 . 158.5(2)
N2 C8 C11 C12 . -20.5(4)
C10 C11 C12 C13 . 1.7(4)
C8 C11 C12 C13 . -174.8(3)
C9 N3 C13 C12 . 0.9(4)
Pb N3 C13 C12 8_665 169.1(2)
C11 C12 C13 N3 . -2.2(5)
