#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:28:39 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179724 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/24/7002418.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7002418
loop_
_publ_author_name
'Yu, Jie-Hui'
'Zhu, Yan-Chun'
'Wu, Di'
'Yu, Yang'
'Hou, Qin'
'Xu, Ji-Qing'
_publ_section_title
;
 Preparation and structural characterization of a series of
 monoacylhydrazidate-bridged coordination polymers
;
_journal_issue                   39
_journal_name_full               'Dalton Transactions'
_journal_page_first              8248
_journal_page_last               8256
_journal_paper_doi               10.1039/b908812a
_journal_year                    2009
_chemical_formula_sum            'C14 H8 N6 O4 Pb'
_chemical_formula_weight         531.45
_chemical_name_systematic
;
?
;
_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                99.219(4)
_cell_angle_beta                 91.433(4)
_cell_angle_gamma                93.907(4)
_cell_formula_units_Z            2
_cell_length_a                   4.1197(2)
_cell_length_b                   12.4547(10)
_cell_length_c                   16.4720(8)
_cell_measurement_temperature    293(2)
_cell_volume                     831.76(9)
_computing_cell_refinement       'Bruker SMART '
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART '
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Siements SMART CCD '
_diffrn_measurement_method       'Omega scan'
_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  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6030
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.174
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.122
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.044
_refine_diff_density_min         -1.946
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4092
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0368
_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)+(0.0648P)²+0.5133P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1038
_reflns_number_gt                3661
_reflns_number_total             4092
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b908812a.txt
_cod_data_source_block           12
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7002418
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.68466(5) 0.986504(19) 0.101134(13) 0.02873(10) Uani 1 1 d . . .
O1 O 0.9544(14) 1.1036(4) 0.0078(3) 0.0408(12) Uani 1 1 d . . .
O2 O 1.2930(16) 1.5308(4) 0.0961(4) 0.0518(15) Uani 1 1 d . . .
O3 O 1.1335(12) 1.0270(4) 0.1924(3) 0.0370(11) Uani 1 1 d . . .
O4 O 1.2230(18) 0.8802(6) 0.4814(4) 0.0631(18) Uani 1 1 d . . .
N1 N 0.7262(14) 1.2043(5) 0.1514(4) 0.0333(11) Uani 1 1 d . . .
N2 N 1.2158(16) 1.2601(5) -0.0161(4) 0.0383(13) Uani 1 1 d . . .
N3 N 1.2949(16) 1.3698(5) 0.0098(4) 0.0393(13) Uani 1 1 d . . .
H3A H 1.4182 1.4022 -0.0215 0.047 Uiso 1 1 calc R . .
N4 N 0.7453(15) 0.8446(5) 0.2102(4) 0.0348(12) Uani 1 1 d . . .
N5 N 1.3238(15) 1.0451(5) 0.3240(4) 0.0388(13) Uani 1 1 d . . .
N6 N 1.3313(15) 1.0029(6) 0.3962(3) 0.0455(16) Uani 1 1 d . . .
H6A H 1.4496 1.0403 0.4360 0.055 Uiso 1 1 calc R . .
C1 C 0.621(2) 1.2544(7) 0.2228(5) 0.0455(18) Uani 1 1 d . . .
H1A H 0.4918 1.2141 0.2543 0.055 Uiso 1 1 calc R . .
C2 C 0.701(2) 1.3680(7) 0.2528(6) 0.051(2) Uani 1 1 d . . .
H2B H 0.6304 1.4009 0.3033 0.062 Uiso 1 1 calc R . .
C3 C 0.887(2) 1.4269(6) 0.2042(5) 0.0424(16) Uani 1 1 d . . .
H3B H 0.9394 1.5011 0.2212 0.051 Uiso 1 1 calc R . .
C4 C 0.9949(16) 1.3748(5) 0.1296(4) 0.0313(13) Uani 1 1 d . . .
C5 C 0.9108(15) 1.2642(5) 0.1059(4) 0.0276(12) Uani 1 1 d . . .
C6 C 1.0301(17) 1.2081(5) 0.0298(4) 0.0307(13) Uani 1 1 d . . .
C7 C 1.2024(18) 1.4317(6) 0.0780(5) 0.0355(14) Uani 1 1 d . . .
C8 C 0.5804(19) 0.7508(6) 0.2157(5) 0.0441(17) Uani 1 1 d . . .
H8A H 0.4442 0.7176 0.1716 0.053 Uiso 1 1 calc R . .
C9 C 0.603(2) 0.7012(6) 0.2839(5) 0.0453(17) Uani 1 1 d . . .
H9A H 0.4930 0.6339 0.2854 0.054 Uiso 1 1 calc R . .
C10 C 0.797(2) 0.7544(7) 0.3514(5) 0.0480(18) Uani 1 1 d . . .
H10A H 0.8089 0.7246 0.3995 0.058 Uiso 1 1 calc R . .
C11 C 0.9675(18) 0.8505(6) 0.3457(4) 0.0356(14) Uani 1 1 d . . .
C12 C 0.9429(17) 0.8932(5) 0.2727(4) 0.0306(13) Uani 1 1 d . . .
C13 C 1.1334(15) 0.9938(5) 0.2640(4) 0.0310(13) Uani 1 1 d . . .
C14 C 1.1792(19) 0.9119(7) 0.4120(4) 0.0419(16) Uani 1 1 d . . .
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'
Pb Pb -3.3944 10.1111 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Pb1 O1 89.41(17) . . ?
O3 Pb1 O1 89.82(19) . 2_775 ?
O1 Pb1 O1 62.24(19) . 2_775 ?
O3 Pb1 N1 73.18(18) . . ?
O1 Pb1 N1 62.71(16) . . ?
O1 Pb1 N1 122.13(16) 2_775 . ?
O3 Pb1 N4 65.17(17) . . ?
O1 Pb1 N4 148.44(19) . . ?
O1 Pb1 N4 97.57(17) 2_775 . ?
N1 Pb1 N4 121.44(17) . . ?
C6 O1 Pb1 123.2(4) . . ?
C6 O1 Pb1 113.4(4) . 2_775 ?
Pb1 O1 Pb1 117.76(19) . 2_775 ?
C13 O3 Pb1 120.8(4) . . ?
C1 N1 C5 118.2(6) . . ?
C1 N1 Pb1 125.1(5) . . ?
C5 N1 Pb1 115.9(4) . . ?
C6 N2 N3 118.1(6) . . ?
C7 N3 N2 127.6(6) . . ?
C8 N4 C12 119.5(6) . . ?
C8 N4 Pb1 131.1(5) . . ?
C12 N4 Pb1 108.4(4) . . ?
C13 N5 N6 117.5(6) . . ?
C14 N6 N5 128.1(6) . . ?
N1 C1 C2 122.4(7) . . ?
C3 C2 C1 117.9(7) . . ?
C2 C3 C4 119.7(7) . . ?
C5 C4 C3 118.7(6) . . ?
C5 C4 C7 119.3(6) . . ?
C3 C4 C7 121.9(6) . . ?
N1 C5 C4 123.1(6) . . ?
N1 C5 C6 117.5(5) . . ?
C4 C5 C6 119.3(6) . . ?
N2 C6 O1 119.8(6) . . ?
N2 C6 C5 120.8(6) . . ?
O1 C6 C5 119.4(6) . . ?
O2 C7 N3 122.1(6) . . ?
O2 C7 C4 123.0(7) . . ?
N3 C7 C4 114.9(6) . . ?
N4 C8 C9 122.5(8) . . ?
C8 C9 C10 118.3(7) . . ?
C11 C10 C9 119.2(7) . . ?
C10 C11 C12 118.9(7) . . ?
C10 C11 C14 123.6(7) . . ?
C12 C11 C14 117.4(7) . . ?
N4 C12 C11 121.4(6) . . ?
N4 C12 C13 118.7(6) . . ?
C11 C12 C13 119.9(6) . . ?
N5 C13 O3 119.7(6) . . ?
N5 C13 C12 120.8(6) . . ?
O3 C13 C12 119.2(6) . . ?
O4 C14 N6 120.9(8) . . ?
O4 C14 C11 123.0(8) . . ?
N6 C14 C11 116.1(6) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O3 2.329(5) . ?
Pb1 O1 2.512(5) . ?
Pb1 O1 2.531(5) 2_775 ?
Pb1 N1 2.699(6) . ?
Pb1 N4 2.732(6) . ?
O1 C6 1.308(8) . ?
O1 Pb1 2.531(5) 2_775 ?
O2 C7 1.251(9) . ?
O3 C13 1.311(8) . ?
O4 C14 1.280(9) . ?
N1 C1 1.336(10) . ?
N1 C5 1.352(8) . ?
N2 C6 1.301(9) . ?
N2 N3 1.379(8) . ?
N3 C7 1.336(9) . ?
N4 C8 1.328(9) . ?
N4 C12 1.334(9) . ?
N5 C13 1.301(8) . ?
N5 N6 1.375(8) . ?
N6 C14 1.323(10) . ?
C1 C2 1.435(11) . ?
C2 C3 1.380(12) . ?
C3 C4 1.394(9) . ?
C4 C5 1.388(9) . ?
C4 C7 1.450(10) . ?
C5 C6 1.449(9) . ?
C8 C9 1.371(12) . ?
C9 C10 1.398(12) . ?
C10 C11 1.364(11) . ?
C11 C12 1.394(9) . ?
C11 C14 1.461(11) . ?
C12 C13 1.462(9) . ?
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
_geom_hbond_site_symmetry_A
N3 H3A O2 0.86 1.97 2.831(8) 177.1 2_885
N6 H6A O4 0.86 1.99 2.841(9) 171.8 2_876
