#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/92/4339227.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_4339227
loop_
_publ_author_name
'Yang, Jin'
'Ma, Jian-Fang'
'Liu, Ying-Ying'
'Ma, Ji-Cheng'
'Batten, Stuart R.'
_publ_section_title
;
 Organic-acid effect on the structures of a series of lead(II) complexes.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6542
_journal_page_last               6555
_journal_paper_doi               10.1021/ic700613c
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C32 H18 N4 O4 Pb'
_chemical_formula_sum            'C32 H18 N4 O4 Pb'
_chemical_formula_weight         729.69
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 103.83(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7814(16)
_cell_length_b                   24.643(5)
_cell_length_c                   13.928(3)
_cell_measurement_reflns_used    16137
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.16
_cell_volume                     2593.4(10)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        PROCESS-AUTO
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1990)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotorating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_sigmaI/netI    0.0643
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24314
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.16
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    6.554
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.869
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.856
_refine_diff_density_min         -1.132
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5871
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0397
_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)+(0.0281P)²+0.7665P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0816
_reflns_number_gt                4105
_reflns_number_total             5871
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700613c-file003.cif
_cod_data_source_block           compound7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        2593.2(9)
_cod_original_sg_symbol_Hall     '-p 2ybc'
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4339227
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
C1 C 0.4687(8) 0.3271(2) -0.0052(5) 0.0477(16) Uani 1 1 d .
H1 H 0.5134 0.2920 -0.0035 0.057 Uiso 1 1 calc R
C2 C 0.3550(9) 0.3448(2) -0.0918(5) 0.0535(17) Uani 1 1 d .
H2 H 0.3254 0.3223 -0.1469 0.064 Uiso 1 1 calc R
C3 C 0.2869(8) 0.3964(2) -0.0944(5) 0.0442(15) Uani 1 1 d .
H3 H 0.2114 0.4095 -0.1519 0.053 Uiso 1 1 calc R
C4 C 0.3323(7) 0.42892(19) -0.0102(5) 0.0353(13) Uani 1 1 d .
C5 C 0.4511(7) 0.40884(19) 0.0726(5) 0.0351(13) Uani 1 1 d .
C6 C 0.5136(7) 0.44330(19) 0.1601(4) 0.0346(13) Uani 1 1 d .
C7 C 0.6992(8) 0.4533(2) 0.3130(5) 0.0468(15) Uani 1 1 d .
H7 H 0.7842 0.4390 0.3655 0.056 Uiso 1 1 calc R
C8 C 0.6465(8) 0.5065(2) 0.3189(5) 0.0448(15) Uani 1 1 d .
H8 H 0.6962 0.5274 0.3740 0.054 Uiso 1 1 calc R
C9 C 0.5223(8) 0.5277(2) 0.2439(5) 0.0449(15) Uani 1 1 d .
H9 H 0.4836 0.5632 0.2475 0.054 Uiso 1 1 calc R
C10 C 0.4526(7) 0.4961(2) 0.1610(4) 0.0342(12) Uani 1 1 d .
C11 C 0.3207(7) 0.51730(19) 0.0756(5) 0.0353(13) Uani 1 1 d .
C12 C 0.2624(7) 0.48413(19) -0.0094(4) 0.0345(13) Uani 1 1 d .
C13 C 0.0830(7) 0.5529(2) -0.0842(5) 0.0401(14) Uani 1 1 d .
C14 C 0.1434(7) 0.5862(2) 0.0000(5) 0.0419(14) Uani 1 1 d .
C15 C 0.0770(8) 0.6401(2) 0.0014(5) 0.0504(17) Uani 1 1 d .
H15 H 0.1169 0.6625 0.0560 0.060 Uiso 1 1 calc R
C16 C -0.0450(8) 0.6578(3) -0.0785(6) 0.0539(18) Uani 1 1 d .
H16 H -0.0871 0.6931 -0.0788 0.065 Uiso 1 1 calc R
C17 C -0.1104(8) 0.6245(3) -0.1609(6) 0.0538(17) Uani 1 1 d .
H17 H -0.1986 0.6375 -0.2132 0.065 Uiso 1 1 calc R
C18 C -0.0460(7) 0.5736(2) -0.1651(5) 0.0465(16) Uani 1 1 d .
H18 H -0.0869 0.5523 -0.2210 0.056 Uiso 1 1 calc R
C19 C 0.5246(7) 0.3195(2) 0.3750(4) 0.0374(12) Uani 1 1 d .
C20 C 0.3907(7) 0.3204(2) 0.4354(4) 0.0363(12) Uani 1 1 d .
C21 C 0.2273(7) 0.2944(2) 0.3976(5) 0.0426(15) Uani 1 1 d .
H21 H 0.2055 0.2783 0.3355 0.051 Uiso 1 1 calc R
C22 C 0.1001(8) 0.2923(2) 0.4504(5) 0.0505(17) Uani 1 1 d .
H22 H -0.0063 0.2745 0.4244 0.061 Uiso 1 1 calc R
C23 C 0.1293(9) 0.3164(3) 0.5419(6) 0.0596(18) Uani 1 1 d .
H23 H 0.0426 0.3156 0.5776 0.072 Uiso 1 1 calc R
C24 C 0.2895(8) 0.3417(2) 0.5798(5) 0.0541(17) Uani 1 1 d .
H24 H 0.3087 0.3581 0.6416 0.065 Uiso 1 1 calc R
C25 C 0.4225(7) 0.3437(2) 0.5293(5) 0.0371(13) Uani 1 1 d .
C26 C 0.5873(8) 0.3736(2) 0.5758(4) 0.0380(13) Uani 1 1 d .
C27 C 0.6104(8) 0.4259(2) 0.5426(5) 0.0497(16) Uani 1 1 d .
H27 H 0.5281 0.4401 0.4888 0.060 Uiso 1 1 calc R
C28 C 0.7559(9) 0.4570(2) 0.5894(5) 0.0537(17) Uani 1 1 d .
H28 H 0.7712 0.4914 0.5652 0.064 Uiso 1 1 calc R
C29 C 0.8762(9) 0.4379(2) 0.6702(6) 0.0576(18) Uani 1 1 d .
H29 H 0.9711 0.4594 0.7020 0.069 Uiso 1 1 calc R
C30 C 0.7090(8) 0.2969(2) 0.6957(5) 0.0439(15) Uani 1 1 d .
C31 C 0.7141(7) 0.35394(19) 0.6570(5) 0.0392(14) Uani 1 1 d .
C32 C 0.8548(8) 0.3863(2) 0.7040(5) 0.0509(17) Uani 1 1 d .
H32 H 0.9361 0.3730 0.7592 0.061 Uiso 1 1 calc R
N1 N 0.5173(6) 0.35735(16) 0.0752(4) 0.0409(12) Uani 1 1 d .
N2 N 0.6340(6) 0.42190(17) 0.2360(4) 0.0426(12) Uani 1 1 d .
N3 N 0.1443(6) 0.50142(16) -0.0883(4) 0.0387(11) Uani 1 1 d .
N4 N 0.2641(6) 0.56786(17) 0.0796(4) 0.0419(12) Uani 1 1 d .
O1 O 0.6841(5) 0.32919(17) 0.4129(3) 0.0523(11) Uani 1 1 d .
O2 O 0.4713(5) 0.30956(15) 0.2820(3) 0.0465(10) Uani 1 1 d .
O3 O 0.6245(6) 0.26126(14) 0.6386(3) 0.0526(12) Uani 1 1 d .
O4 O 0.7925(7) 0.28604(16) 0.7806(4) 0.0730(16) Uani 1 1 d .
Pb1 Pb 0.73137(3) 0.317273(8) 0.233552(17) 0.03844(8) 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
N1 C1 C2 123.6(5) . .
N1 C1 H1 118.2 . .
C2 C1 H1 118.2 . .
C3 C2 C1 118.5(6) . .
C3 C2 H2 120.8 . .
C1 C2 H2 120.8 . .
C2 C3 C4 119.4(6) . .
C2 C3 H3 120.3 . .
C4 C3 H3 120.3 . .
C5 C4 C3 118.6(5) . .
C5 C4 C12 120.0(5) . .
C3 C4 C12 121.3(5) . .
N1 C5 C4 121.8(5) . .
N1 C5 C6 117.8(5) . .
C4 C5 C6 120.4(5) . .
N2 C6 C10 122.5(5) . .
N2 C6 C5 117.2(4) . .
C10 C6 C5 120.3(5) . .
N2 C7 C8 122.8(6) . .
N2 C7 H7 118.6 . .
C8 C7 H7 118.6 . .
C9 C8 C7 119.4(6) . .
C9 C8 H8 120.3 . .
C7 C8 H8 120.3 . .
C8 C9 C10 119.4(5) . .
C8 C9 H9 120.3 . .
C10 C9 H9 120.3 . .
C6 C10 C9 117.8(5) . .
C6 C10 C11 120.0(5) . .
C9 C10 C11 122.2(5) . .
N4 C11 C12 122.2(5) . .
N4 C11 C10 118.3(5) . .
C12 C11 C10 119.5(5) . .
N3 C12 C11 121.8(5) . .
N3 C12 C4 118.5(5) . .
C11 C12 C4 119.7(5) . .
N3 C13 C18 119.4(6) . .
N3 C13 C14 121.6(5) . .
C18 C13 C14 119.0(5) . .
N4 C14 C13 121.0(5) . .
N4 C14 C15 118.9(6) . .
C13 C14 C15 120.0(6) . .
C16 C15 C14 118.3(7) . .
C16 C15 H15 120.9 . .
C14 C15 H15 120.9 . .
C15 C16 C17 122.1(6) . .
C15 C16 H16 118.9 . .
C17 C16 H16 118.9 . .
C18 C17 C16 120.6(6) . .
C18 C17 H17 119.7 . .
C16 C17 H17 119.7 . .
C17 C18 C13 119.8(7) . .
C17 C18 H18 120.1 . .
C13 C18 H18 120.1 . .
O1 C19 O2 120.7(5) . .
O1 C19 C20 121.1(5) . .
O2 C19 C20 118.2(5) . .
O1 C19 Pb1 68.0(3) . .
O2 C19 Pb1 52.7(3) . .
C20 C19 Pb1 170.7(4) . .
C25 C20 C21 118.7(5) . .
C25 C20 C19 123.0(5) . .
C21 C20 C19 118.2(5) . .
C22 C21 C20 121.3(6) . .
C22 C21 H21 119.3 . .
C20 C21 H21 119.3 . .
C21 C22 C23 120.1(6) . .
C21 C22 H22 119.9 . .
C23 C22 H22 119.9 . .
C22 C23 C24 119.0(6) . .
C22 C23 H23 120.5 . .
C24 C23 H23 120.5 . .
C23 C24 C25 122.5(6) . .
C23 C24 H24 118.8 . .
C25 C24 H24 118.8 . .
C24 C25 C20 118.4(5) . .
C24 C25 C26 117.9(6) . .
C20 C25 C26 123.7(5) . .
C27 C26 C31 117.8(5) . .
C27 C26 C25 118.7(5) . .
C31 C26 C25 123.3(5) . .
C28 C27 C26 120.5(6) . .
C28 C27 H27 119.8 . .
C26 C27 H27 119.8 . .
C29 C28 C27 121.1(6) . .
C29 C28 H28 119.4 . .
C27 C28 H28 119.4 . .
C28 C29 C32 119.0(6) . .
C28 C29 H29 120.5 . .
C32 C29 H29 120.5 . .
O4 C30 O3 122.0(5) . .
O4 C30 C31 119.4(5) . .
O3 C30 C31 118.6(6) . .
O4 C30 Pb1 67.4(3) . 4_566
O3 C30 Pb1 55.2(3) . 4_566
C31 C30 Pb1 167.5(4) . 4_566
C32 C31 C26 120.5(5) . .
C32 C31 C30 116.9(5) . .
C26 C31 C30 122.6(5) . .
C29 C32 C31 121.0(6) . .
C29 C32 H32 119.5 . .
C31 C32 H32 119.5 . .
C1 N1 C5 118.1(5) . .
C1 N1 Pb1 119.7(4) . .
C5 N1 Pb1 122.2(4) . .
C7 N2 C6 118.0(5) . .
C7 N2 Pb1 121.1(4) . .
C6 N2 Pb1 120.8(3) . .
C12 N3 C13 116.5(5) . .
C11 N4 C14 116.9(5) . .
C19 O1 Pb1 85.8(4) . .
C19 O2 Pb1 100.7(3) . .
C30 O3 Pb1 99.0(4) . 4_566
C30 O4 Pb1 87.1(3) . 4_566
O2 Pb1 O3 83.12(15) . 4_565
O2 Pb1 N1 81.39(15) . .
O3 Pb1 N1 76.78(13) 4_565 .
O2 Pb1 O1 52.71(14) . .
O3 Pb1 O1 120.63(14) 4_565 .
N1 Pb1 O1 123.58(14) . .
O2 Pb1 O4 88.07(15) . 4_565
O3 Pb1 O4 51.12(13) 4_565 4_565
N1 Pb1 O4 127.76(13) . 4_565
O1 Pb1 O4 85.98(15) . 4_565
O2 Pb1 N2 78.71(14) . .
O3 Pb1 N2 136.45(14) 4_565 .
N1 Pb1 N2 61.63(14) . .
O1 Pb1 N2 77.10(14) . .
O4 Pb1 N2 162.66(16) 4_565 .
O2 Pb1 C19 26.54(15) . .
O3 Pb1 C19 102.79(15) 4_565 .
N1 Pb1 C19 103.07(15) . .
O1 Pb1 C19 26.17(13) . .
O4 Pb1 C19 86.82(16) 4_565 .
N2 Pb1 C19 76.33(15) . .
O2 Pb1 C30 87.34(15) . 4_565
O3 Pb1 C30 25.78(16) 4_565 4_565
N1 Pb1 C30 102.56(16) . 4_565
O1 Pb1 C30 105.61(17) . 4_565
O4 Pb1 C30 25.53(16) 4_565 4_565
N2 Pb1 C30 160.11(16) . 4_565
C19 Pb1 C30 97.34(17) . 4_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.324(7) .
C1 C2 1.384(9) .
C1 H1 0.9300 .
C2 C3 1.376(8) .
C2 H2 0.9300 .
C3 C4 1.394(8) .
C3 H3 0.9300 .
C4 C5 1.385(8) .
C4 C12 1.466(7) .
C5 N1 1.367(6) .
C5 C6 1.470(7) .
C6 N2 1.342(7) .
C6 C10 1.387(7) .
C7 N2 1.321(7) .
C7 C8 1.382(7) .
C7 H7 0.9300 .
C8 C9 1.347(8) .
C8 H8 0.9300 .
C9 C10 1.390(8) .
C9 H9 0.9300 .
C10 C11 1.469(8) .
C11 N4 1.327(6) .
C11 C12 1.421(8) .
C12 N3 1.323(7) .
C13 N3 1.362(6) .
C13 C18 1.413(8) .
C13 C14 1.415(9) .
C14 N4 1.348(8) .
C14 C15 1.428(7) .
C15 C16 1.351(9) .
C15 H15 0.9300 .
C16 C17 1.403(10) .
C16 H16 0.9300 .
C17 C18 1.359(8) .
C17 H17 0.9300 .
C18 H18 0.9300 .
C19 O1 1.250(6) .
C19 O2 1.285(7) .
C19 C20 1.488(8) .
C19 Pb1 2.826(6) .
C20 C25 1.395(8) .
C20 C21 1.409(7) .
C21 C22 1.368(8) .
C21 H21 0.9300 .
C22 C23 1.374(9) .
C22 H22 0.9300 .
C23 C24 1.381(9) .
C23 H23 0.9300 .
C24 C25 1.385(8) .
C24 H24 0.9300 .
C25 C26 1.487(8) .
C26 C27 1.395(7) .
C26 C31 1.398(8) .
C27 C28 1.393(9) .
C27 H27 0.9300 .
C28 C29 1.364(9) .
C28 H28 0.9300 .
C29 C32 1.381(8) .
C29 H29 0.9300 .
C30 O4 1.234(8) .
C30 O3 1.259(7) .
C30 C31 1.509(8) .
C30 Pb1 2.860(6) 4_566
C31 C32 1.386(8) .
C32 H32 0.9300 .
N1 Pb1 2.618(5) .
N2 Pb1 2.690(4) .
O1 Pb1 2.627(4) .
O2 Pb1 2.289(4) .
O3 Pb1 2.379(4) 4_566
O4 Pb1 2.643(4) 4_566
Pb1 O3 2.379(4) 4_565
Pb1 O4 2.643(4) 4_565
Pb1 C30 2.860(6) 4_565
