#------------------------------------------------------------------------------
#$Date: 2016-03-26 20:53:06 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180453 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/22/7212220.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_7212220
loop_
_publ_author_name
'Jin, Juan'
'Jia, Ming-Jun'
'Peng, Yu'
'Hou, Qin'
'Yu, Jie-Hui'
'Xu, Ji-Qing'
_publ_section_title
;
 4-Carboxylphthalhydrazidate-bridged layered Pb(ii) coordination polymers
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              1850
_journal_paper_doi               10.1039/b922767a
_journal_volume                  12
_journal_year                    2010
_chemical_formula_sum            'C21 H12 N4 O4 Pb'
_chemical_formula_weight         591.54
_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                 94.849(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.5673(11)
_cell_length_b                   10.1496(5)
_cell_length_c                   16.1354(5)
_cell_measurement_temperature    293(2)
_cell_volume                     3519.4(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0933
_diffrn_reflns_av_sigmaI/netI    0.0694
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12459
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    9.628
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.599
_refine_diff_density_min         -2.279
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0404
_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)+(0.0527P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1031
_reflns_number_gt                3340
_reflns_number_total             4348
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b922767a.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7212220
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 0.451360(11) 0.15757(2) 0.081676(14) 0.02997(10) Uani 1 1 d .
N1 N 0.5374(2) -0.0187(5) 0.1371(3) 0.0323(12) Uani 1 1 d .
N2 N 0.5705(3) 0.0053(5) 0.2131(3) 0.0310(12) Uani 1 1 d .
H2A H 0.5747 0.0865 0.2276 0.037 Uiso 1 1 calc R
N3 N 0.3725(2) 0.3311(5) 0.0057(3) 0.0300(12) Uani 1 1 d .
N4 N 0.3575(2) 0.0665(5) -0.0234(3) 0.0313(12) Uani 1 1 d .
O1 O 0.4987(2) -0.1626(4) 0.0394(3) 0.0366(11) Uani 1 1 d .
O2 O 0.6259(2) -0.0502(4) 0.3329(3) 0.0414(11) Uani 1 1 d .
O3 O 0.5143(3) -0.6462(4) 0.1058(4) 0.0517(14) Uani 1 1 d .
O4 O 0.5754(3) -0.7151(5) 0.2174(4) 0.0553(14) Uani 1 1 d .
C1 C 0.5408(3) -0.3833(6) 0.1419(4) 0.0266(12) Uani 1 1 d .
H1A H 0.5172 -0.4028 0.0925 0.032 Uiso 1 1 calc R
C2 C 0.5648(3) -0.4834(6) 0.1931(4) 0.0259(12) Uani 1 1 d .
C3 C 0.6003(3) -0.4540(6) 0.2670(4) 0.0306(13) Uani 1 1 d .
H3A H 0.6168 -0.5220 0.3005 0.037 Uiso 1 1 calc R
C4 C 0.6112(3) -0.3243(5) 0.2910(4) 0.0299(13) Uani 1 1 d .
H4A H 0.6346 -0.3055 0.3406 0.036 Uiso 1 1 calc R
C5 C 0.5870(2) -0.2226(5) 0.2406(3) 0.0218(11) Uani 1 1 d .
C6 C 0.5525(2) -0.2507(6) 0.1656(4) 0.0232(12) Uani 1 1 d .
C7 C 0.5285(3) -0.1403(5) 0.1123(4) 0.0249(12) Uani 1 1 d .
C8 C 0.5966(3) -0.0844(6) 0.2669(4) 0.0267(12) Uani 1 1 d .
C9 C 0.5512(3) -0.6277(6) 0.1703(5) 0.0365(16) Uani 1 1 d .
C10 C 0.3793(3) 0.4606(6) 0.0193(4) 0.0363(15) Uani 1 1 d .
H10A H 0.4128 0.4893 0.0548 0.044 Uiso 1 1 calc R
C11 C 0.3384(4) 0.5546(7) -0.0175(5) 0.0481(19) Uani 1 1 d .
H11A H 0.3447 0.6436 -0.0060 0.058 Uiso 1 1 calc R
C12 C 0.2890(4) 0.5151(7) -0.0707(5) 0.0474(18) Uani 1 1 d .
H12A H 0.2606 0.5765 -0.0940 0.057 Uiso 1 1 calc R
C13 C 0.2818(3) 0.3798(7) -0.0897(4) 0.0339(14) Uani 1 1 d .
C14 C 0.2331(3) 0.3309(7) -0.1493(5) 0.0414(17) Uani 1 1 d .
H14A H 0.2041 0.3889 -0.1748 0.050 Uiso 1 1 calc R
C15 C 0.2300(3) 0.2030(8) -0.1674(4) 0.0413(16) Uani 1 1 d .
H15A H 0.1995 0.1741 -0.2076 0.050 Uiso 1 1 calc R
C16 C 0.2712(3) 0.1091(7) -0.1281(4) 0.0345(14) Uani 1 1 d .
C17 C 0.2692(3) -0.0278(7) -0.1451(5) 0.0412(16) Uani 1 1 d .
H17A H 0.2393 -0.0608 -0.1846 0.049 Uiso 1 1 calc R
C18 C 0.3102(4) -0.1110(8) -0.1045(5) 0.0473(18) Uani 1 1 d .
H18A H 0.3101 -0.2001 -0.1181 0.057 Uiso 1 1 calc R
C19 C 0.3531(3) -0.0616(6) -0.0417(5) 0.0393(16) Uani 1 1 d .
H19A H 0.3794 -0.1204 -0.0118 0.047 Uiso 1 1 calc R
C20 C 0.3245(3) 0.2903(6) -0.0481(4) 0.0279(13) Uani 1 1 d .
C21 C 0.3174(3) 0.1505(6) -0.0663(4) 0.0285(13) 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
O1 Pb1 O3 79.78(18) 5_655 1_565
O1 Pb1 N3 85.50(16) 5_655 .
O3 Pb1 N3 81.83(18) 1_565 .
O1 Pb1 N1 86.43(15) 5_655 .
O3 Pb1 N1 97.62(19) 1_565 .
N3 Pb1 N1 171.89(16) . .
O1 Pb1 N4 81.63(16) 5_655 .
O3 Pb1 N4 139.87(18) 1_565 .
N3 Pb1 N4 61.46(15) . .
N1 Pb1 N4 116.37(16) . .
C7 N1 N2 119.2(5) . .
C7 N1 Pb1 116.7(4) . .
N2 N1 Pb1 117.9(4) . .
C8 N2 N1 127.3(5) . .
C10 N3 C20 118.1(6) . .
C10 N3 Pb1 121.1(4) . .
C20 N3 Pb1 120.9(4) . .
C19 N4 C21 117.8(6) . .
C19 N4 Pb1 120.7(4) . .
C21 N4 Pb1 121.1(4) . .
C7 O1 Pb1 121.8(4) . 5_655
C9 O3 Pb1 123.9(4) . 1_545
C2 C1 C6 119.1(6) . .
C1 C2 C3 120.3(5) . .
C1 C2 C9 120.3(6) . .
C3 C2 C9 119.3(6) . .
C4 C3 C2 120.7(6) . .
C3 C4 C5 119.7(6) . .
C4 C5 C6 120.1(5) . .
C4 C5 C8 120.1(5) . .
C6 C5 C8 119.7(5) . .
C5 C6 C1 120.0(5) . .
C5 C6 C7 118.9(5) . .
C1 C6 C7 121.1(5) . .
N1 C7 O1 119.1(5) . .
N1 C7 C6 120.2(5) . .
O1 C7 C6 120.7(5) . .
O2 C8 N2 121.2(6) . .
O2 C8 C5 124.2(5) . .
N2 C8 C5 114.6(5) . .
O4 C9 O3 126.3(6) . .
O4 C9 C2 118.1(7) . .
O3 C9 C2 115.6(6) . .
N3 C10 C11 123.0(7) . .
C12 C11 C10 119.7(7) . .
C11 C12 C13 119.0(7) . .
C12 C13 C20 117.6(7) . .
C12 C13 C14 122.5(6) . .
C20 C13 C14 119.9(6) . .
C15 C14 C13 120.0(6) . .
C14 C15 C16 122.6(7) . .
C21 C16 C17 115.9(6) . .
C21 C16 C15 119.6(6) . .
C17 C16 C15 124.4(7) . .
C18 C17 C16 120.8(7) . .
C17 C18 C19 119.3(7) . .
N4 C19 C18 122.6(7) . .
N3 C20 C13 122.4(6) . .
N3 C20 C21 119.2(6) . .
C13 C20 C21 118.4(6) . .
N4 C21 C16 123.5(6) . .
N4 C21 C20 117.2(6) . .
C16 C21 C20 119.2(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O1 2.310(5) 5_655
Pb1 O3 2.423(4) 1_565
Pb1 N3 2.673(5) .
Pb1 N1 2.677(5) .
Pb1 N4 2.691(5) .
N1 C7 1.306(7) .
N1 N2 1.387(8) .
N2 C8 1.348(8) .
N3 C10 1.338(7) .
N3 C20 1.360(8) .
N4 C19 1.336(8) .
N4 C21 1.362(8) .
O1 C7 1.312(7) .
O1 Pb1 2.310(5) 5_655
O2 C8 1.242(7) .
O3 C9 1.271(9) .
O3 Pb1 2.423(4) 1_545
O4 C9 1.252(9) .
C1 C2 1.382(9) .
C1 C6 1.417(8) .
C2 C3 1.393(9) .
C2 C9 1.532(8) .
C3 C4 1.386(8) .
C4 C5 1.388(8) .
C5 C6 1.394(8) .
C5 C8 1.475(8) .
C6 C7 1.480(8) .
C10 C11 1.397(10) .
C11 C12 1.372(11) .
C12 C13 1.413(10) .
C13 C20 1.421(9) .
C13 C14 1.449(10) .
C14 C15 1.332(10) .
C15 C16 1.417(10) .
C16 C21 1.413(9) .
C16 C17 1.416(10) .
C17 C18 1.351(11) .
C18 C19 1.405(10) .
C20 C21 1.454(8) .
