#------------------------------------------------------------------------------
#$Date: 2016-03-25 08:28:39 +0100 (vie 25 de mar de 2016) $
#$Revision: 179724 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/24/7002419.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_7002419
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           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.840(2)
_cell_length_b                   14.977(3)
_cell_length_c                   3.7771(8)
_cell_measurement_temperature    293(2)
_cell_volume                     669.8(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        PROCESS-AUTO
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       w
_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  0.0193
_diffrn_reflns_av_sigmaI/netI    0.0234
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            6316
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.22
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.635
_exptl_absorpt_correction_T_max  0.5
_exptl_absorpt_correction_T_min  0.13385
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;Higashi, T.(1995).Program for Absorption Correction
Rigaku Corporation, Tokyo,Japan.
;
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    2.635
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.452
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.003(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         1504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0132
_refine_ls_R_factor_gt           0.0124
_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)+(0.0133P)²+0.3873P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0289
_refine_ls_wR_factor_ref         0.0307
_reflns_number_gt                1476
_reflns_number_total             1504
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b908812a.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      P21212
_cod_database_code               7002419
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -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 0.5000 0.5000 0.70483(3) 0.02024(5) Uani 1 2 d S . .
C1 C 0.4173(2) 0.27575(19) 0.6506(9) 0.0228(6) Uani 1 1 d . . .
H1A H 0.4906 0.2795 0.5635 0.027 Uiso 1 1 calc R . .
C2 C 0.3623(2) 0.19358(19) 0.6374(9) 0.0187(6) Uani 1 1 d . . .
C3 C 0.2514(2) 0.1876(2) 0.7638(8) 0.0183(6) Uani 1 1 d . . .
C4 C 0.2020(2) 0.2639(2) 0.9028(9) 0.0222(6) Uani 1 1 d . . .
H4A H 0.1288 0.2623 0.9914 0.027 Uiso 1 1 calc R . .
C5 C 0.2638(2) 0.3422(2) 0.9074(10) 0.0252(6) Uani 1 1 d . . .
H5A H 0.2302 0.3930 1.0024 0.030 Uiso 1 1 calc R . .
C6 C 0.4188(3) 0.11505(19) 0.4949(10) 0.0240(7) Uani 1 1 d . . .
C7 C 0.1926(2) 0.1018(2) 0.7282(8) 0.0206(6) Uani 1 1 d . . .
O1 O 0.51843(17) 0.11482(15) 0.3910(9) 0.0383(6) Uani 1 1 d . . .
O2 O 0.08626(17) 0.09522(15) 0.8224(7) 0.0269(5) Uani 1 1 d . . .
N1 N 0.3696(2) 0.34917(17) 0.7824(7) 0.0253(6) Uani 1 1 d . . .
N2 N 0.3540(2) 0.04114(17) 0.4853(9) 0.0285(6) Uani 1 1 d . . .
H2A H 0.3859 -0.0063 0.4045 0.034 Uiso 1 1 calc R . .
N3 N 0.2419(2) 0.03207(17) 0.5903(9) 0.0255(6) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.02452(8) 0.01494(7) 0.02127(8) 0.000 0.000 0.00344(8)
C1 0.0168(12) 0.0163(15) 0.0354(18) 0.0044(13) -0.0018(14) -0.0013(11)
C2 0.0165(13) 0.0145(14) 0.0252(15) 0.0031(11) -0.0025(13) 0.0006(10)
C3 0.0166(13) 0.0171(15) 0.0211(15) 0.0029(11) -0.0053(12) -0.0010(11)
C4 0.0188(13) 0.0222(16) 0.0255(16) 0.0007(13) 0.0012(14) 0.0018(11)
C5 0.0263(14) 0.0181(15) 0.0313(17) -0.0024(13) -0.0047(15) 0.0024(11)
C6 0.0232(14) 0.0153(15) 0.0335(19) 0.0049(12) 0.0031(16) 0.0029(12)
C7 0.0179(13) 0.0181(16) 0.0257(16) 0.0048(12) -0.0038(12) -0.0049(11)
O1 0.0245(12) 0.0233(12) 0.0671(16) 0.0074(11) 0.0160(16) 0.0038(9)
O2 0.0164(9) 0.0261(12) 0.0382(14) 0.0046(10) 0.0007(10) -0.0061(8)
N1 0.0233(12) 0.0132(13) 0.0394(17) 0.0007(11) -0.0070(12) -0.0018(10)
N2 0.0258(12) 0.0141(12) 0.0455(18) -0.0052(12) 0.0045(14) -0.0001(10)
N3 0.0222(11) 0.0176(12) 0.0367(15) -0.0006(11) -0.0004(13) -0.0040(9)
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Pb1 O2 88.98(11) 4_557 3_557 ?
O2 Pb1 O2 94.14(7) 4_557 4_556 ?
O2 Pb1 O2 176.89(8) 3_557 4_556 ?
O2 Pb1 O2 176.89(8) 4_557 3_556 ?
O2 Pb1 O2 94.14(7) 3_557 3_556 ?
O2 Pb1 O2 82.75(10) 4_556 3_556 ?
O2 Pb1 N1 99.36(8) 4_557 2_665 ?
O2 Pb1 N1 71.66(8) 3_557 2_665 ?
O2 Pb1 N1 107.76(8) 4_556 2_665 ?
O2 Pb1 N1 81.65(8) 3_556 2_665 ?
O2 Pb1 N1 71.66(8) 4_557 . ?
O2 Pb1 N1 99.36(8) 3_557 . ?
O2 Pb1 N1 81.65(8) 4_556 . ?
O2 Pb1 N1 107.76(8) 3_556 . ?
N1 Pb1 N1 167.77(12) 2_665 . ?
N1 C1 C2 123.0(3) . . ?
C1 C2 C3 118.8(3) . . ?
C1 C2 C6 120.8(3) . . ?
C3 C2 C6 120.4(3) . . ?
C4 C3 C2 118.2(3) . . ?
C4 C3 C7 123.8(3) . . ?
C2 C3 C7 118.0(3) . . ?
C5 C4 C3 118.8(3) . . ?
N1 C5 C4 123.7(3) . . ?
O1 C6 N2 122.0(3) . . ?
O1 C6 C2 123.7(3) . . ?
N2 C6 C2 114.4(3) . . ?
N3 C7 O2 118.5(3) . . ?
N3 C7 C3 121.7(3) . . ?
O2 C7 C3 119.7(3) . . ?
C7 O2 Pb1 128.87(19) . 3_547 ?
C7 O2 Pb1 101.89(19) . 3_546 ?
Pb1 O2 Pb1 94.14(7) 3_547 3_546 ?
C1 N1 C5 117.6(3) . . ?
C1 N1 Pb1 113.6(2) . . ?
C5 N1 Pb1 128.6(2) . . ?
C6 N2 N3 128.0(3) . . ?
C7 N3 N2 117.5(2) . . ?
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 O2 2.503(2) 4_557 ?
Pb1 O2 2.503(2) 3_557 ?
Pb1 O2 2.654(2) 4_556 ?
Pb1 O2 2.654(2) 3_556 ?
Pb1 N1 2.752(3) 2_665 ?
Pb1 N1 2.752(3) . ?
C1 N1 1.333(4) . ?
C1 C2 1.393(4) . ?
C2 C3 1.400(4) . ?
C2 C6 1.456(4) . ?
C3 C4 1.386(4) . ?
C3 C7 1.468(4) . ?
C4 C5 1.383(4) . ?
C5 N1 1.342(4) . ?
C6 O1 1.244(4) . ?
C6 N2 1.347(4) . ?
C7 N3 1.304(4) . ?
C7 O2 1.312(4) . ?
O2 Pb1 2.503(2) 3_547 ?
O2 Pb1 2.654(2) 3_546 ?
N2 N3 1.393(3) . ?
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
N2 H2A O1 0.86 1.98 2.804(3) 159.5 2_655
