#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:54:30 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179905 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/01/7020189.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_7020189
loop_
_publ_author_name
'Jin, Juan'
'Jia, Ming-Jun'
'Li, Guang-Hua'
'Zeng, Guang'
'Yu, Jie-Hui'
'Xu, Ji-Qing'
_publ_section_title
;
 New metal complexes with di(mono)acylhydrazidate molecules.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10267
_journal_page_last               10275
_journal_paper_doi               10.1039/c2dt30941f
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C58 H40 N16 O10 Pb2'
_chemical_formula_weight         1535.44
_chemical_name_systematic
;
?
;
_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                 108.38(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.180(5)
_cell_length_b                   9.1064(18)
_cell_length_c                   24.826(5)
_cell_measurement_reflns_used    5817
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.12
_cell_volume                     5188(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      123(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_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  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            24156
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.12
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.564
_exptl_absorpt_correction_T_max  0.455
_exptl_absorpt_correction_T_min  0.389
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Process-auto, Higashi, T.(1995).Program for Absorption Correction.
Rigaku Corporation, Tokyo,Japan.
The larger diff. peak value is due to the existence of Q1
atom 0.791 ? away from Pb1.
Q1 is actually insignificant.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.966
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2976
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         6.089
_refine_diff_density_min         -3.678
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5817
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0438
_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)+(0.0000P)²+119.4978P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0854
_reflns_number_gt                4720
_reflns_number_total             5817
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30941f.txt
_cod_data_source_block           1
_cod_original_cell_volume        5187.7(18)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7020189
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_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
Pb1 Pb 0.078267(10) 0.58309(3) 0.009176(10) 0.01769(7) Uani 1 1 d .
O1 O 0.11613(19) 0.4332(5) -0.05436(19) 0.0243(10) Uani 1 1 d .
O2 O 0.02453(18) -0.1044(5) -0.05053(18) 0.0182(9) Uani 1 1 d .
O3 O 0.4026(2) 0.1389(5) -0.2619(2) 0.0291(11) Uani 1 1 d .
O4 O 0.33903(19) -0.0185(5) -0.08174(19) 0.0202(10) Uani 1 1 d .
N1 N 0.0690(2) 0.2711(6) -0.0165(2) 0.0192(11) Uani 1 1 d .
N2 N 0.0473(2) 0.1276(6) -0.0172(2) 0.0184(11) Uani 1 1 d .
H2A H 0.0319 0.1077 0.0089 0.022 Uiso 1 1 calc R
N3 N 0.4220(2) 0.0683(6) -0.1702(2) 0.0223(12) Uani 1 1 d .
H3A H 0.4585 0.0725 -0.1667 0.027 Uiso 1 1 calc R
N4 N 0.4086(2) 0.0250(6) -0.1225(2) 0.0216(12) Uani 1 1 d .
N5 N 0.1028(2) 0.8146(6) 0.0715(2) 0.0150(10) Uani 1 1 d .
N6 N 0.1491(2) 0.7507(6) -0.0141(2) 0.0171(11) Uani 1 1 d .
N7 N 0.1143(2) 0.2524(6) -0.2670(2) 0.0197(11) Uani 1 1 d .
N8 N 0.0574(2) 0.2747(6) -0.2686(2) 0.0242(12) Uani 1 1 d .
H8A H 0.0450 0.2376 -0.2427 0.029 Uiso 1 1 calc R
H8B H 0.0342 0.3257 -0.2955 0.029 Uiso 1 1 calc R
C1 C 0.1014(3) -0.0135(7) -0.1791(3) 0.0187(13) Uani 1 1 d .
H1A H 0.1020 -0.0814 -0.2069 0.022 Uiso 1 1 calc R
C2 C 0.0755(3) -0.0487(7) -0.1386(2) 0.0149(12) Uani 1 1 d .
H2B H 0.0579 -0.1399 -0.1397 0.018 Uiso 1 1 calc R
C3 C 0.0755(2) 0.0516(6) -0.0960(2) 0.0136(12) Uani 1 1 d .
C4 C 0.1008(3) 0.1907(7) -0.0950(3) 0.0162(12) Uani 1 1 d .
C5 C 0.1273(2) 0.2262(7) -0.1363(3) 0.0157(12) Uani 1 1 d .
H5A H 0.1452 0.3170 -0.1353 0.019 Uiso 1 1 calc R
C6 C 0.1270(2) 0.1261(7) -0.1782(2) 0.0146(12) Uani 1 1 d .
C7 C 0.0963(3) 0.3009(7) -0.0527(3) 0.0192(13) Uani 1 1 d .
C8 C 0.0473(3) 0.0171(7) -0.0533(3) 0.0172(13) Uani 1 1 d .
C9 C 0.1474(3) 0.1762(7) -0.2264(3) 0.0157(12) Uani 1 1 d .
C10 C 0.2244(3) 0.1855(7) -0.2743(3) 0.0220(14) Uani 1 1 d .
H10A H 0.1972 0.2259 -0.3061 0.026 Uiso 1 1 calc R
C11 C 0.2811(3) 0.1653(7) -0.2735(3) 0.0245(15) Uani 1 1 d .
H11A H 0.2917 0.1894 -0.3054 0.029 Uiso 1 1 calc R
C12 C 0.3228(3) 0.1091(7) -0.2256(3) 0.0217(14) Uani 1 1 d .
C13 C 0.3071(3) 0.0668(7) -0.1778(3) 0.0189(13) Uani 1 1 d .
C14 C 0.2485(2) 0.0815(7) -0.1802(3) 0.0162(12) Uani 1 1 d .
H14A H 0.2370 0.0481 -0.1499 0.019 Uiso 1 1 calc R
C15 C 0.2075(3) 0.1446(7) -0.2265(3) 0.0194(14) Uani 1 1 d .
C16 C 0.3854(3) 0.1046(7) -0.2212(3) 0.0244(15) Uani 1 1 d .
C17 C 0.3531(3) 0.0213(7) -0.1263(3) 0.0205(14) Uani 1 1 d .
C18 C 0.0777(3) 0.8504(7) 0.1096(3) 0.0166(12) Uani 1 1 d .
H18A H 0.0498 0.7872 0.1154 0.020 Uiso 1 1 calc R
C27 C 0.1698(3) 0.7242(7) -0.0570(3) 0.0197(13) Uani 1 1 d .
H27A H 0.1568 0.6413 -0.0793 0.024 Uiso 1 1 calc R
C28 C 0.1681(3) 0.8719(7) 0.0178(3) 0.0170(13) Uani 1 1 d .
C29 C 0.1439(2) 0.9054(7) 0.0627(2) 0.0162(12) Uani 1 1 d .
C19 C 0.0910(3) 0.9794(8) 0.1418(3) 0.0231(14) Uani 1 1 d .
H19A H 0.0711 1.0031 0.1671 0.028 Uiso 1 1 calc R
C20 C 0.1334(3) 1.0695(8) 0.1357(3) 0.0264(15) Uani 1 1 d .
H20A H 0.1436 1.1538 0.1577 0.032 Uiso 1 1 calc R
C21 C 0.1616(3) 1.0345(7) 0.0957(3) 0.0203(14) Uani 1 1 d .
C22 C 0.2063(3) 1.1247(8) 0.0860(3) 0.0287(16) Uani 1 1 d .
H22A H 0.2196 1.2066 0.1088 0.034 Uiso 1 1 calc R
C23 C 0.2291(3) 1.0922(8) 0.0443(3) 0.0269(15) Uani 1 1 d .
H23A H 0.2582 1.1520 0.0391 0.032 Uiso 1 1 calc R
C24 C 0.2098(3) 0.9692(7) 0.0085(3) 0.0190(13) Uani 1 1 d .
C25 C 0.2311(3) 0.9376(8) -0.0368(3) 0.0232(15) Uani 1 1 d .
H25A H 0.2589 0.9981 -0.0441 0.028 Uiso 1 1 calc R
C26 C 0.2107(3) 0.8177(8) -0.0699(3) 0.0223(14) Uani 1 1 d .
H26A H 0.2236 0.7974 -0.1006 0.027 Uiso 1 1 calc R
OW1 O 0.4606(2) 0.9726(6) 0.1657(2) 0.0315(12) 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'
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
O4 Pb1 O1 87.32(15) 7 .
O4 Pb1 N6 81.24(16) 7 .
O1 Pb1 N6 76.71(16) . .
O4 Pb1 N5 76.15(16) 7 .
O1 Pb1 N5 140.89(15) . .
N6 Pb1 N5 66.00(16) . .
C7 O1 Pb1 106.0(4) . .
C17 O4 Pb1 109.8(4) . 7
C7 N1 N2 117.0(5) . .
C8 N2 N1 128.6(5) . .
C16 N3 N4 128.2(5) . .
C17 N4 N3 117.1(6) . .
C18 N5 C29 119.4(5) . .
C18 N5 Pb1 124.4(4) . .
C29 N5 Pb1 116.3(4) . .
C27 N6 C28 118.2(5) . .
C27 N6 Pb1 122.2(4) . .
C28 N6 Pb1 119.6(4) . .
C9 N7 N8 118.3(5) . .
C2 C1 C6 119.6(6) . .
C1 C2 C3 120.6(6) . .
C2 C3 C4 120.0(5) . .
C2 C3 C8 121.3(5) . .
C4 C3 C8 118.7(5) . .
C3 C4 C5 119.3(5) . .
C3 C4 C7 119.7(5) . .
C5 C4 C7 120.9(6) . .
C6 C5 C4 120.1(6) . .
C5 C6 C1 120.4(5) . .
C5 C6 C9 118.3(5) . .
C1 C6 C9 120.8(5) . .
N1 C7 O1 119.2(6) . .
N1 C7 C4 121.0(6) . .
O1 C7 C4 119.6(5) . .
O2 C8 N2 122.3(5) . .
O2 C8 C3 123.0(6) . .
N2 C8 C3 114.8(6) . .
N7 C9 C15 118.4(5) . .
N7 C9 C6 120.7(5) . .
C15 C9 C6 120.7(5) . .
C11 C10 C15 120.1(6) . .
C10 C11 C12 120.6(6) . .
C11 C12 C13 120.5(6) . .
C11 C12 C16 121.3(6) . .
C13 C12 C16 118.1(6) . .
C14 C13 C12 118.3(6) . .
C14 C13 C17 122.7(5) . .
C12 C13 C17 118.7(6) . .
C15 C14 C13 121.5(6) . .
C14 C15 C10 118.8(6) . .
C14 C15 C9 121.7(5) . .
C10 C15 C9 119.4(6) . .
O3 C16 N3 122.6(6) . .
O3 C16 C12 121.8(7) . .
N3 C16 C12 115.5(5) . .
O4 C17 N4 118.5(6) . .
O4 C17 C13 119.3(6) . .
N4 C17 C13 122.1(6) . .
N5 C18 C19 122.8(6) . .
N6 C27 C26 122.4(6) . .
N6 C28 C24 122.9(6) . .
N6 C28 C29 118.7(5) . .
C24 C28 C29 118.4(6) . .
N5 C29 C21 120.9(5) . .
N5 C29 C28 119.2(6) . .
C21 C29 C28 119.8(6) . .
C20 C19 C18 119.3(6) . .
C19 C20 C21 119.6(6) . .
C20 C21 C29 117.9(6) . .
C20 C21 C22 123.1(6) . .
C29 C21 C22 118.9(6) . .
C23 C22 C21 120.9(7) . .
C22 C23 C24 121.4(6) . .
C25 C24 C23 122.2(6) . .
C25 C24 C28 117.5(6) . .
C23 C24 C28 120.2(6) . .
C26 C25 C24 119.5(6) . .
C25 C26 C27 119.5(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O4 2.306(5) 7
Pb1 O1 2.470(4) .
Pb1 N6 2.494(5) .
Pb1 N5 2.571(5) .
O1 C7 1.302(8) .
O2 C8 1.247(8) .
O3 C16 1.246(8) .
O4 C17 1.308(7) .
O4 Pb1 2.306(5) 7
N1 C7 1.300(8) .
N1 N2 1.406(7) .
N2 C8 1.347(8) .
N3 C16 1.338(9) .
N3 N4 1.380(7) .
N4 C17 1.316(8) .
N5 C18 1.316(8) .
N5 C29 1.363(8) .
N6 C27 1.334(7) .
N6 C28 1.352(8) .
N7 C9 1.276(8) .
N7 N8 1.380(7) .
C1 C2 1.380(8) .
C1 C6 1.410(9) .
C2 C3 1.398(8) .
C3 C4 1.404(8) .
C3 C8 1.466(8) .
C4 C5 1.408(8) .
C4 C7 1.481(9) .
C5 C6 1.382(8) .
C6 C9 1.504(8) .
C9 C15 1.480(8) .
C10 C11 1.378(9) .
C10 C15 1.422(8) .
C11 C12 1.392(10) .
C12 C13 1.407(8) .
C12 C16 1.484(9) .
C13 C14 1.407(8) .
C13 C17 1.465(10) .
C14 C15 1.385(9) .
C18 C19 1.401(9) .
C27 C26 1.416(9) .
C28 C24 1.417(9) .
C28 C29 1.446(8) .
C29 C21 1.419(9) .
C19 C20 1.358(10) .
C20 C21 1.408(9) .
C21 C22 1.435(9) .
C22 C23 1.351(10) .
C23 C24 1.415(10) .
C24 C25 1.405(9) .
C25 C26 1.361(10) .
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 O2 0.86 1.96 2.779(6) 160.0 5
N3 H3A OW1 0.86 1.99 2.830(7) 164.8 5_665
