#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/92/4339224.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_4339224
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         'C22 H12 N4 O4 Pb, H2 O'
_chemical_formula_sum            'C22 H14 N4 O5 Pb'
_chemical_formula_weight         621.58
_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                90.88(3)
_cell_angle_beta                 93.82(3)
_cell_angle_gamma                102.61(3)
_cell_formula_units_Z            2
_cell_length_a                   6.8124(14)
_cell_length_b                   8.1738(16)
_cell_length_c                   18.070(4)
_cell_measurement_reflns_used    8474
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.07
_cell_volume                     979.3(4)
_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 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotorating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0597
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9704
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.07
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    8.660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.108
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.27
_refine_diff_density_max         3.170
_refine_diff_density_min         -1.343
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         4454
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0371
_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)+(0.0376P)²+0.5629P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0800
_reflns_number_gt                3825
_reflns_number_total             4454
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700613c-file003.cif
_cod_data_source_block           compound4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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        979.3(3)
_cod_original_sg_symbol_Hall     '-p 1'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4339224
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
C1 C 0.5758(10) 0.6979(10) 0.3088(4) 0.0365(16) Uani 1 1 d .
H1 H 0.6619 0.7000 0.3511 0.044 Uiso 1 1 calc R
C2 C 0.6477(12) 0.7917(11) 0.2479(4) 0.052(2) Uani 1 1 d .
H2 H 0.7786 0.8563 0.2501 0.062 Uiso 1 1 calc R
C3 C 0.5229(11) 0.7864(11) 0.1860(4) 0.0460(19) Uani 1 1 d .
H3 H 0.5702 0.8452 0.1448 0.055 Uiso 1 1 calc R
C4 C 0.3247(11) 0.6942(9) 0.1832(4) 0.0353(15) Uani 1 1 d .
C5 C 0.2625(10) 0.6015(8) 0.2463(3) 0.0298(14) Uani 1 1 d .
C6 C 0.0588(9) 0.4995(8) 0.2469(3) 0.0282(13) Uani 1 1 d .
C7 C -0.0801(10) 0.4978(9) 0.1872(4) 0.0350(15) Uani 1 1 d .
C8 C -0.2703(12) 0.3974(11) 0.1904(4) 0.047(2) Uani 1 1 d .
H8 H -0.3660 0.3939 0.1509 0.056 Uiso 1 1 calc R
C9 C -0.3202(11) 0.3024(11) 0.2512(4) 0.049(2) Uani 1 1 d .
H9 H -0.4477 0.2336 0.2536 0.058 Uiso 1 1 calc R
C10 C -0.1714(10) 0.3138(10) 0.3091(4) 0.0375(16) Uani 1 1 d .
H10 H -0.2029 0.2503 0.3507 0.045 Uiso 1 1 calc R
C11 C -0.0222(11) 0.5978(9) 0.1223(3) 0.0350(15) Uani 1 1 d .
C12 C 0.1797(11) 0.6939(9) 0.1206(4) 0.0341(15) Uani 1 1 d .
C13 C 0.0993(13) 0.7836(10) 0.0064(4) 0.0445(18) Uani 1 1 d .
C14 C -0.1011(12) 0.6941(10) 0.0092(4) 0.0440(19) Uani 1 1 d .
C15 C -0.2436(15) 0.7056(13) -0.0505(4) 0.060(2) Uani 1 1 d .
H15 H -0.3768 0.6475 -0.0491 0.072 Uiso 1 1 calc R
C16 C 0.1555(15) 0.8830(12) -0.0562(4) 0.057(2) Uani 1 1 d .
H16 H 0.2876 0.9426 -0.0589 0.068 Uiso 1 1 calc R
C17 C 0.0130(15) 0.8894(12) -0.1119(4) 0.061(2) Uani 1 1 d .
H17 H 0.0495 0.9545 -0.1527 0.074 Uiso 1 1 calc R
C18 C -0.1868(16) 0.8008(14) -0.1096(5) 0.068(3) Uani 1 1 d .
H18 H -0.2809 0.8070 -0.1486 0.081 Uiso 1 1 calc R
C20 C 0.4373(9) 0.2001(7) 0.4593(3) 0.0254(13) Uani 1 1 d .
C22 C -0.0435(8) 0.2079(7) 0.5401(3) 0.0248(13) Uani 1 1 d .
C23 C 0.0047(9) 0.0401(8) 0.5320(3) 0.0260(12) Uani 1 1 d .
H23 H 0.0435 -0.0108 0.5746 0.031 Uiso 1 1 calc R
C21 C 0.4888(9) 0.0340(8) 0.4677(4) 0.0280(13) Uani 1 1 d .
H21 H 0.5062 -0.0251 0.4252 0.034 Uiso 1 1 calc R
N1 N 0.0112(8) 0.4094(7) 0.3083(3) 0.0304(12) Uani 1 1 d .
N2 N 0.3906(8) 0.6072(7) 0.3078(3) 0.0329(12) Uani 1 1 d .
N3 N 0.2421(10) 0.7838(8) 0.0625(3) 0.0442(15) Uani 1 1 d .
N4 N -0.1614(9) 0.5993(8) 0.0682(3) 0.0422(15) Uani 1 1 d .
O1 O 0.4404(7) 0.2923(5) 0.5163(2) 0.0310(10) Uani 1 1 d .
O2 O 0.3863(8) 0.2409(6) 0.3951(2) 0.0356(11) Uani 1 1 d .
O1W O 1.1615(13) 0.9962(10) 0.2843(3) 0.075(2) Uani 1 1 d D
HW11 H 1.249(13) 1.072(8) 0.307(5) 0.090 Uiso 1 1 d D
HW12 H 1.135(16) 0.917(8) 0.314(4) 0.090 Uiso 1 1 d D
O3 O -0.0675(7) 0.2897(5) 0.4835(2) 0.0301(10) Uani 1 1 d .
O4 O -0.0648(7) 0.2575(6) 0.6050(3) 0.0360(11) Uani 1 1 d .
Pb1 Pb 0.23679(3) 0.49416(3) 0.429244(12) 0.02184(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 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3940 10.1110 '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
N2 C1 C2 122.1(6) . .
N2 C1 H1 119.0 . .
C2 C1 H1 119.0 . .
C3 C2 C1 118.8(7) . .
C3 C2 H2 120.6 . .
C1 C2 H2 120.6 . .
C2 C3 C4 121.0(7) . .
C2 C3 H3 119.5 . .
C4 C3 H3 119.5 . .
C3 C4 C5 117.3(6) . .
C3 C4 C12 123.4(6) . .
C5 C4 C12 119.2(6) . .
N2 C5 C4 120.8(6) . .
N2 C5 C6 118.7(6) . .
C4 C5 C6 120.5(6) . .
N1 C6 C7 122.0(6) . .
N1 C6 C5 117.4(5) . .
C7 C6 C5 120.5(6) . .
C8 C7 C6 118.0(6) . .
C8 C7 C11 121.9(6) . .
C6 C7 C11 120.1(6) . .
C9 C8 C7 120.9(6) . .
C9 C8 H8 119.6 . .
C7 C8 H8 119.6 . .
C8 C9 C10 117.1(7) . .
C8 C9 H9 121.5 . .
C10 C9 H9 121.5 . .
N1 C10 C9 123.7(6) . .
N1 C10 H10 118.1 . .
C9 C10 H10 118.1 . .
N4 C11 C12 122.3(6) . .
N4 C11 C7 118.3(6) . .
C12 C11 C7 119.5(6) . .
N3 C12 C11 122.1(6) . .
N3 C12 C4 117.8(6) . .
C11 C12 C4 120.1(6) . .
N3 C13 C14 122.4(7) . .
N3 C13 C16 118.1(8) . .
C14 C13 C16 119.5(7) . .
N4 C14 C13 121.4(6) . .
N4 C14 C15 119.6(7) . .
C13 C14 C15 119.0(7) . .
C18 C15 C14 120.5(9) . .
C18 C15 H15 119.8 . .
C14 C15 H15 119.8 . .
C17 C16 C13 119.1(9) . .
C17 C16 H16 120.5 . .
C13 C16 H16 120.5 . .
C16 C17 C18 121.8(8) . .
C16 C17 H17 119.1 . .
C18 C17 H17 119.1 . .
C15 C18 C17 120.1(8) . .
C15 C18 H18 120.0 . .
C17 C18 H18 120.0 . .
O2 C20 O1 122.8(6) . .
O2 C20 C21 117.9(5) . .
O1 C20 C21 119.2(5) . .
O3 C22 O4 123.4(6) . .
O3 C22 C23 119.6(6) . .
O4 C22 C23 116.9(5) . .
C23 C23 C22 123.4(7) 2_556 .
C23 C23 H23 118.3 2_556 .
C22 C23 H23 118.3 . .
C21 C21 C20 123.4(8) 2_656 .
C21 C21 H21 118.3 2_656 .
C20 C21 H21 118.3 . .
C10 N1 C6 118.2(5) . .
C10 N1 Pb1 121.2(4) . .
C6 N1 Pb1 118.2(4) . .
C1 N2 C5 120.0(6) . .
C1 N2 Pb1 120.9(4) . .
C5 N2 Pb1 117.5(4) . .
C12 N3 C13 115.5(7) . .
C11 N4 C14 116.3(6) . .
C20 O1 Pb1 123.3(4) . 2_666
C20 O1 Pb1 88.5(3) . .
Pb1 O1 Pb1 102.91(15) 2_666 .
C20 O2 Pb1 99.3(4) . .
HW11 O1W HW12 106(3) . .
C22 O3 Pb1 121.3(4) . .
C22 O3 Pb1 89.0(4) . 2_566
Pb1 O3 Pb1 103.05(14) . 2_566
C22 O4 Pb1 98.5(4) . 2_566
N1 Pb1 O2 84.08(17) . .
N1 Pb1 N2 63.81(16) . .
O2 Pb1 N2 82.19(17) . .
N1 Pb1 O1 142.21(16) . 2_666
O2 Pb1 O1 101.15(15) . 2_666
N2 Pb1 O1 79.70(16) . 2_666
N1 Pb1 O4 72.09(16) . 2_566
O2 Pb1 O4 152.56(14) . 2_566
N2 Pb1 O4 75.27(17) . 2_566
O1 Pb1 O4 90.14(14) 2_666 2_566
N1 Pb1 O3 80.81(15) . .
O2 Pb1 O3 89.65(15) . .
N2 Pb1 O3 144.26(16) . .
O1 Pb1 O3 136.02(14) 2_666 .
O4 Pb1 O3 99.51(15) 2_566 .
N1 Pb1 O1 127.77(16) . .
O2 Pb1 O1 48.24(13) . .
N2 Pb1 O1 117.89(16) . .
O1 Pb1 O1 77.09(15) 2_666 .
O4 Pb1 O1 158.88(14) 2_566 .
O3 Pb1 O1 79.25(13) . .
N1 Pb1 O3 109.31(16) . 2_566
O2 Pb1 O3 158.87(13) . 2_566
N2 Pb1 O3 118.12(16) . 2_566
O1 Pb1 O3 78.54(14) 2_666 2_566
O4 Pb1 O3 47.83(13) 2_566 2_566
O3 Pb1 O3 76.95(14) . 2_566
O1 Pb1 O3 112.28(13) . 2_566
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N2 1.315(9) .
C1 C2 1.404(10) .
C1 H1 0.9300 .
C2 C3 1.353(10) .
C2 H2 0.9300 .
C3 C4 1.393(10) .
C3 H3 0.9300 .
C4 C5 1.417(9) .
C4 C12 1.451(9) .
C5 N2 1.360(8) .
C5 C6 1.455(9) .
C6 N1 1.358(8) .
C6 C7 1.386(9) .
C7 C8 1.380(10) .
C7 C11 1.465(9) .
C8 C9 1.373(10) .
C8 H8 0.9300 .
C9 C10 1.396(9) .
C9 H9 0.9300 .
C10 N1 1.318(8) .
C10 H10 0.9300 .
C11 N4 1.318(8) .
C11 C12 1.430(10) .
C12 N3 1.331(9) .
C13 N3 1.357(9) .
C13 C14 1.406(11) .
C13 C16 1.427(11) .
C14 N4 1.361(9) .
C14 C15 1.420(10) .
C15 C18 1.359(12) .
C15 H15 0.9300 .
C16 C17 1.361(11) .
C16 H16 0.9300 .
C17 C18 1.399(14) .
C17 H17 0.9300 .
C18 H18 0.9300 .
C20 O2 1.259(7) .
C20 O1 1.263(8) .
C20 C21 1.482(8) .
C22 O3 1.252(7) .
C22 O4 1.263(8) .
C22 C23 1.486(8) .
C23 C23 1.312(12) 2_556
C23 H23 0.9300 .
C21 C21 1.314(12) 2_656
C21 H21 0.9300 .
N1 Pb1 2.581(5) .
N2 Pb1 2.592(5) .
O1 Pb1 2.615(4) 2_666
O1 Pb1 2.812(4) .
O2 Pb1 2.582(5) .
O1W HW11 0.84(2) .
O1W HW12 0.85(2) .
O3 Pb1 2.619(5) .
O3 Pb1 2.826(4) 2_566
O4 Pb1 2.618(5) 2_566
Pb1 O1 2.615(4) 2_666
Pb1 O4 2.618(5) 2_566
Pb1 O3 2.826(4) 2_566
