#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/92/4339226.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_4339226
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         '2(C26 H14 N4 O4 Pb), 0.5(O2)'
_chemical_formula_sum            'C52 H30 N8 O9 Pb2'
_chemical_formula_weight         1325.22
_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                100.375(5)
_cell_angle_beta                 112.273(4)
_cell_angle_gamma                95.158(5)
_cell_formula_units_Z            1
_cell_length_a                   9.677(3)
_cell_length_b                   11.884(4)
_cell_length_c                   11.988(4)
_cell_measurement_reflns_used    4732
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.23
_cell_measurement_theta_min      1.89
_cell_volume                     1235.8(7)
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  'SHELXTL (Bruker, 1998)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_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  0.1196
_diffrn_reflns_av_sigmaI/netI    0.0823
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6794
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.23
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    6.867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SAINT; Bruker, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             634
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.23
_refine_diff_density_max         4.788
_refine_diff_density_min         -2.196
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4732
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0519
_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)+(0.0888P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1296
_reflns_number_gt                4135
_reflns_number_total             4732
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700613c-file003.cif
_cod_data_source_block           compound6
_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_sg_symbol_Hall     '-p 1'
_cod_database_code               4339226
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 0.2111(8) 0.4268(7) 0.8952(7) 0.0410(16) Uani 1 1 d .
C2 C 0.1011(8) 0.4641(6) 0.9486(7) 0.0384(15) Uani 1 1 d .
C3 C 0.1314(8) 0.4637(7) 1.0728(7) 0.0414(16) Uani 1 1 d .
H3 H 0.2181 0.4386 1.1208 0.050 Uiso 1 1 calc R
C4 C 0.0311(8) 0.5009(7) 1.1236(7) 0.0411(16) Uani 1 1 d .
H4 H 0.0524 0.5025 1.2064 0.049 Uiso 1 1 calc R
C5 C 0.2626(8) 0.1788(7) 0.6481(6) 0.0373(15) Uani 1 1 d .
C6 C 0.1279(8) 0.0831(6) 0.5711(6) 0.0347(14) Uani 1 1 d .
C7 C 0.0839(8) -0.0018(6) 0.6218(6) 0.0380(15) Uani 1 1 d .
H7 H 0.1399 -0.0030 0.7039 0.046 Uiso 1 1 calc R
C8 C -0.0426(9) -0.0841(7) 0.5508(6) 0.0392(15) Uani 1 1 d .
H8 H -0.0715 -0.1415 0.5850 0.047 Uiso 1 1 calc R
C9 C 0.6852(11) 0.2384(8) 0.6832(7) 0.054(2) Uani 1 1 d .
H9 H 0.6095 0.2529 0.6142 0.065 Uiso 1 1 calc R
C10 C 0.8132(11) 0.2009(9) 0.6723(7) 0.056(2) Uani 1 1 d .
H10 H 0.8239 0.1931 0.5976 0.067 Uiso 1 1 calc R
C11 C 0.9200(11) 0.1765(8) 0.7700(8) 0.052(2) Uani 1 1 d .
H11 H 1.0052 0.1509 0.7633 0.062 Uiso 1 1 calc R
C12 C 0.9036(9) 0.1895(6) 0.8837(7) 0.0400(16) Uani 1 1 d .
C13 C 0.7758(8) 0.2314(6) 0.8883(6) 0.0377(15) Uani 1 1 d .
C14 C 0.7547(8) 0.2511(6) 1.0058(6) 0.0362(14) Uani 1 1 d .
C15 C 0.8635(8) 0.2320(6) 1.1118(6) 0.0379(15) Uani 1 1 d .
C16 C 0.8407(10) 0.2557(8) 1.2219(7) 0.0494(19) Uani 1 1 d .
H16 H 0.9149 0.2477 1.2954 0.059 Uiso 1 1 calc R
C17 C 0.7115(11) 0.2901(9) 1.2212(8) 0.056(2) Uani 1 1 d .
H17 H 0.6923 0.3007 1.2925 0.068 Uiso 1 1 calc R
C18 C 0.6068(9) 0.3096(7) 1.1113(7) 0.0459(17) Uani 1 1 d .
H18 H 0.5195 0.3365 1.1113 0.055 Uiso 1 1 calc R
C19 C 1.0167(8) 0.1640(6) 0.9933(7) 0.0389(15) Uani 1 1 d .
C20 C 1.0015(9) 0.1891(7) 1.1083(7) 0.0412(16) Uani 1 1 d .
C21 C 1.2382(9) 0.1007(7) 1.0897(8) 0.0473(18) Uani 1 1 d .
C22 C 1.3641(10) 0.0504(8) 1.0846(10) 0.060(2) Uani 1 1 d .
H22 H 1.3748 0.0321 1.0099 0.072 Uiso 1 1 calc R
C23 C 1.4666(11) 0.0294(9) 1.1861(10) 0.065(2) Uani 1 1 d .
H23 H 1.5465 -0.0063 1.1811 0.078 Uiso 1 1 calc R
C24 C 1.4560(11) 0.0600(10) 1.2996(11) 0.073(3) Uani 1 1 d .
H24 H 1.5309 0.0475 1.3703 0.088 Uiso 1 1 calc R
C25 C 1.3372(11) 0.1083(9) 1.3087(9) 0.063(2) Uani 1 1 d .
H25 H 1.3303 0.1270 1.3850 0.076 Uiso 1 1 calc R
C26 C 1.2243(9) 0.1300(7) 1.2026(7) 0.0454(17) Uani 1 1 d .
N1 N 0.6692(7) 0.2538(6) 0.7899(6) 0.0439(14) Uani 1 1 d .
N2 N 0.6284(7) 0.2908(5) 1.0066(5) 0.0381(13) Uani 1 1 d .
N3 N 1.1333(7) 0.1192(6) 0.9836(6) 0.0455(14) Uani 1 1 d .
N4 N 1.1043(7) 0.1732(6) 1.2111(6) 0.0468(15) Uani 1 1 d .
O1 O 0.3103(7) 0.2473(5) 0.5987(5) 0.0533(15) Uani 1 1 d .
O2 O 0.3197(6) 0.1871(5) 0.7657(4) 0.0459(13) Uani 1 1 d .
O3 O 0.1790(7) 0.4153(7) 0.7827(5) 0.0581(15) Uani 1 1 d .
O4 O 0.3390(7) 0.4125(6) 0.9702(5) 0.0526(14) Uani 1 1 d .
OW1 O -0.038(2) 0.3964(17) 0.5373(14) 0.099(5) Uani 0.50 1 d PU
Pb1 Pb 0.46569(3) 0.37395(2) 0.82556(2) 0.03941(14) 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
O3 C1 O4 122.3(8) . .
O3 C1 C2 120.3(7) . .
O4 C1 C2 117.3(7) . .
C4 C2 C3 119.8(7) 2_567 .
C4 C2 C1 120.7(7) 2_567 .
C3 C2 C1 119.6(7) . .
C4 C3 C2 119.7(7) . .
C4 C3 H3 120.1 . .
C2 C3 H3 120.1 . .
C3 C4 C2 120.5(7) . 2_567
C3 C4 H4 119.8 . .
C2 C4 H4 119.8 2_567 .
O1 C5 O2 122.7(7) . .
O1 C5 C6 120.6(6) . .
O2 C5 C6 116.6(6) . .
O1 C5 Pb1 68.3(4) . .
O2 C5 Pb1 55.5(4) . .
C6 C5 Pb1 164.9(5) . .
C7 C6 C8 119.3(7) . 2_556
C7 C6 C5 121.4(6) . .
C8 C6 C5 119.2(6) 2_556 .
C8 C7 C6 119.8(6) . .
C8 C7 H7 120.1 . .
C6 C7 H7 120.1 . .
C7 C8 C6 120.9(7) . 2_556
C7 C8 H8 119.5 . .
C6 C8 H8 119.5 2_556 .
N1 C9 C10 121.5(8) . .
N1 C9 H9 119.3 . .
C10 C9 H9 119.3 . .
C11 C10 C9 119.5(7) . .
C11 C10 H10 120.2 . .
C9 C10 H10 120.2 . .
C10 C11 C12 120.0(9) . .
C10 C11 H11 120.0 . .
C12 C11 H11 120.0 . .
C13 C12 C11 117.0(7) . .
C13 C12 C19 120.7(6) . .
C11 C12 C19 122.3(7) . .
N1 C13 C12 122.4(6) . .
N1 C13 C14 117.9(7) . .
C12 C13 C14 119.7(6) . .
N2 C14 C15 121.5(6) . .
N2 C14 C13 118.1(6) . .
C15 C14 C13 120.4(7) . .
C14 C15 C16 118.3(7) . .
C14 C15 C20 120.3(6) . .
C16 C15 C20 121.4(7) . .
C17 C16 C15 120.1(8) . .
C17 C16 H16 119.9 . .
C15 C16 H16 119.9 . .
C16 C17 C18 118.7(7) . .
C16 C17 H17 120.7 . .
C18 C17 H17 120.7 . .
N2 C18 C17 122.0(8) . .
N2 C18 H18 119.0 . .
C17 C18 H18 119.0 . .
N3 C19 C20 121.3(7) . .
N3 C19 C12 118.8(6) . .
C20 C19 C12 119.9(7) . .
N4 C20 C19 122.2(7) . .
N4 C20 C15 118.9(6) . .
C19 C20 C15 118.9(7) . .
N3 C21 C26 121.4(8) . .
N3 C21 C22 119.1(8) . .
C26 C21 C22 119.6(8) . .
C23 C22 C21 120.4(9) . .
C23 C22 H22 119.8 . .
C21 C22 H22 119.8 . .
C22 C23 C24 120.8(10) . .
C22 C23 H23 119.6 . .
C24 C23 H23 119.6 . .
C25 C24 C23 120.8(10) . .
C25 C24 H24 119.6 . .
C23 C24 H24 119.6 . .
C24 C25 C26 120.1(10) . .
C24 C25 H25 119.9 . .
C26 C25 H25 119.9 . .
N4 C26 C21 121.8(7) . .
N4 C26 C25 119.9(8) . .
C21 C26 C25 118.3(8) . .
C9 N1 C13 119.6(7) . .
C9 N1 Pb1 120.8(6) . .
C13 N1 Pb1 118.0(5) . .
C18 N2 C14 119.3(6) . .
C18 N2 Pb1 119.4(5) . .
C14 N2 Pb1 119.8(4) . .
C19 N3 C21 116.4(7) . .
C20 N4 C26 116.9(7) . .
C5 O1 Pb1 85.8(4) . .
C5 O2 Pb1 97.8(4) . .
C1 O3 Pb1 88.4(5) . .
C1 O4 Pb1 99.6(5) . .
O2 Pb1 O4 83.8(2) . .
O2 Pb1 N2 81.16(18) . .
O4 Pb1 N2 78.15(19) . .
O2 Pb1 O1 52.41(17) . .
O4 Pb1 O1 119.8(2) . .
N2 Pb1 O1 123.5(2) . .
O2 Pb1 N1 82.1(2) . .
O4 Pb1 N1 140.4(2) . .
N2 Pb1 N1 63.20(19) . .
O1 Pb1 N1 78.5(2) . .
O2 Pb1 O3 76.2(2) . .
O4 Pb1 O3 49.73(18) . .
N2 Pb1 O3 124.49(18) . .
O1 Pb1 O3 78.2(2) . .
N1 Pb1 O3 154.8(2) . .
O2 Pb1 C5 26.76(19) . .
O4 Pb1 C5 100.8(2) . .
N2 Pb1 C5 104.7(2) . .
O1 Pb1 C5 25.93(19) . .
N1 Pb1 C5 81.9(2) . .
O3 Pb1 C5 72.9(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O3 1.243(9) .
C1 O4 1.272(9) .
C1 C2 1.496(11) .
C2 C4 1.395(10) 2_567
C2 C3 1.405(10) .
C3 C4 1.392(11) .
C3 H3 0.9300 .
C4 C2 1.395(10) 2_567
C4 H4 0.9300 .
C5 O1 1.240(9) .
C5 O2 1.285(8) .
C5 C6 1.513(10) .
C5 Pb1 2.829(7) .
C6 C7 1.381(10) .
C6 C8 1.382(10) 2_556
C7 C8 1.369(10) .
C7 H7 0.9300 .
C8 C6 1.382(10) 2_556
C8 H8 0.9300 .
C9 N1 1.328(10) .
C9 C10 1.396(13) .
C9 H9 0.9300 .
C10 C11 1.336(13) .
C10 H10 0.9300 .
C11 C12 1.414(10) .
C11 H11 0.9300 .
C12 C13 1.390(11) .
C12 C19 1.460(11) .
C13 N1 1.330(10) .
C13 C14 1.480(9) .
C14 N2 1.351(9) .
C14 C15 1.381(10) .
C15 C16 1.402(10) .
C15 C20 1.485(11) .
C16 C17 1.348(12) .
C16 H16 0.9300 .
C17 C18 1.399(12) .
C17 H17 0.9300 .
C18 N2 1.332(9) .
C18 H18 0.9300 .
C19 N3 1.325(10) .
C19 C20 1.422(10) .
C20 N4 1.316(10) .
C21 N3 1.364(11) .
C21 C26 1.396(12) .
C21 C22 1.420(12) .
C22 C23 1.329(14) .
C22 H22 0.9300 .
C23 C24 1.389(16) .
C23 H23 0.9300 .
C24 C25 1.361(15) .
C24 H24 0.9300 .
C25 C26 1.412(12) .
C25 H25 0.9300 .
C26 N4 1.342(11) .
N1 Pb1 2.650(7) .
N2 Pb1 2.574(6) .
O1 Pb1 2.635(5) .
O2 Pb1 2.353(5) .
O3 Pb1 2.731(6) .
O4 Pb1 2.479(6) .
