#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/10/4511038.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_4511038
loop_
_publ_author_name
'Yang, Jin'
'Ma, Jian-Fang'
'Liu, Ying-Ying'
'Ma, Ji-Cheng'
'Batten, Stuart R.'
_publ_section_title
;
 A Series of Lead(II) Complexes with π−π Stackings: Structural
 Diversities by Varying the Ligands
;
_journal_issue                   4
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1894
_journal_paper_doi               10.1021/cg801085d
_journal_volume                  9
_journal_year                    2009
_chemical_formula_moiety         'C44 H24 N8 O9 Pb2, 2(H2 O)'
_chemical_formula_sum            'C44 H30 N8 O11 Pb2'
_chemical_formula_weight         1261.14
_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                104.98(3)
_cell_angle_beta                 91.05(3)
_cell_angle_gamma                103.37(3)
_cell_formula_units_Z            1
_cell_length_a                   7.1636(14)
_cell_length_b                   9.2479(18)
_cell_length_c                   15.909(3)
_cell_measurement_reflns_used    8841
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.00
_cell_volume                     987.1(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 0.995
_diffrn_measured_fraction_theta_max 0.986
_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  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9746
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    8.595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.121
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             602
_exptl_crystal_size_max          0.247
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.052
_refine_diff_density_max         1.115
_refine_diff_density_min         -1.402
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4471
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0323
_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)+(0.0196P)²+3.8940P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0740
_reflns_number_gt                3997
_reflns_number_total             4471
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg801085d_si_002.cif
_cod_data_source_block           compound5
_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        987.1(3)
_cod_original_sg_symbol_Hall     '-p 1'
_cod_database_code               4511038
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 0.2302(8) -0.2739(6) 0.6261(4) 0.0313(12) Uani 1 1 d .
C2 C 0.1664(8) -0.4465(6) 0.6015(4) 0.0297(11) Uani 1 1 d .
C3 C 0.2903(9) -0.5320(7) 0.5574(5) 0.0433(15) Uani 1 1 d .
H3 H 0.4133 -0.4807 0.5488 0.052 Uiso 1 1 calc R
C4 C 0.2340(10) -0.6891(8) 0.5270(5) 0.0463(16) Uani 1 1 d .
H4 H 0.3173 -0.7443 0.4973 0.056 Uiso 1 1 calc R
C5 C 0.0525(9) -0.7648(7) 0.5406(4) 0.0386(13) Uani 1 1 d .
H5 H 0.0117 -0.8714 0.5181 0.046 Uiso 1 1 calc R
C6 C -0.0701(8) -0.6847(6) 0.5873(4) 0.0295(11) Uani 1 1 d .
C7 C -0.2657(9) -0.7709(6) 0.6056(4) 0.0346(13) Uani 1 1 d .
C8 C -0.0140(8) -0.5257(6) 0.6173(4) 0.0297(11) Uani 1 1 d .
H8 H -0.0968 -0.4714 0.6481 0.036 Uiso 1 1 calc R
C9 C 0.7071(9) -0.0447(8) 0.7344(4) 0.0434(15) Uani 1 1 d .
H9 H 0.7206 -0.0913 0.6764 0.052 Uiso 1 1 calc R
C10 C 0.8271(10) -0.0622(9) 0.7989(5) 0.0494(17) Uani 1 1 d .
H10 H 0.9158 -0.1219 0.7841 0.059 Uiso 1 1 calc R
C11 C 0.8127(9) 0.0098(8) 0.8843(5) 0.0442(15) Uani 1 1 d .
H11 H 0.8944 0.0017 0.9281 0.053 Uiso 1 1 calc R
C12 C 0.6754(9) 0.0952(7) 0.9056(4) 0.0369(13) Uani 1 1 d .
C13 C 0.5566(8) 0.1051(6) 0.8373(4) 0.0328(12) Uani 1 1 d .
C14 C 0.4070(8) 0.1944(7) 0.8577(4) 0.0331(12) Uani 1 1 d .
C15 C 0.1665(9) 0.2790(8) 0.8045(5) 0.0453(15) Uani 1 1 d .
H15 H 0.0931 0.2858 0.7575 0.054 Uiso 1 1 calc R
C16 C 0.1292(11) 0.3520(9) 0.8876(5) 0.0503(17) Uani 1 1 d .
H16 H 0.0320 0.4045 0.8959 0.060 Uiso 1 1 calc R
C17 C 0.2384(10) 0.3454(8) 0.9572(5) 0.0458(15) Uani 1 1 d .
H17 H 0.2174 0.3943 1.0138 0.055 Uiso 1 1 calc R
C18 C 0.3819(9) 0.2642(7) 0.9422(4) 0.0371(13) Uani 1 1 d .
C19 C 0.5081(9) 0.2559(7) 1.0140(4) 0.0373(13) Uani 1 1 d .
C20 C 0.6530(9) 0.1737(8) 0.9944(4) 0.0399(14) Uani 1 1 d .
C21 C 0.7556(11) 0.2375(9) 1.1362(5) 0.0556(19) Uani 1 1 d .
H21 H 0.8415 0.2382 1.1809 0.067 Uiso 1 1 calc R
C22 C 0.6057(12) 0.3172(10) 1.1578(5) 0.061(2) Uani 1 1 d .
H22 H 0.5940 0.3636 1.2161 0.074 Uiso 1 1 calc R
N1 N 0.5730(7) 0.0362(6) 0.7521(3) 0.0351(11) Uani 1 1 d .
N2 N 0.3009(7) 0.1995(6) 0.7874(3) 0.0377(11) Uani 1 1 d .
N3 N 0.7751(9) 0.1677(8) 1.0603(4) 0.0557(15) Uani 1 1 d .
N4 N 0.4833(9) 0.3267(7) 1.0969(3) 0.0486(14) Uani 1 1 d .
O1 O 0.3834(6) -0.2153(5) 0.5950(3) 0.0395(10) Uani 1 1 d .
O2 O 0.1311(6) -0.1961(5) 0.6722(3) 0.0402(10) Uani 1 1 d .
O1W O -0.2113(10) -0.5095(10) 0.8237(4) 0.090(2) Uani 1 1 d D
HW11 H -0.281(14) -0.444(10) 0.837(7) 0.109 Uiso 1 1 d D
HW12 H -0.276(14) -0.568(11) 0.777(4) 0.109 Uiso 1 1 d D
O3 O -0.3638(6) -0.6993(5) 0.6569(3) 0.0465(11) Uani 1 1 d .
O2W O 0.003(2) 0.0976(14) 0.6278(8) 0.077(4) Uani 0.50 1 d P
O4 O -0.3170(6) -0.9164(5) 0.5686(3) 0.0412(10) Uani 1 1 d .
Pb1 Pb 0.36213(3) 0.04634(2) 0.627566(14) 0.03037(7) 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
O2 C1 O1 123.6(5) . .
O2 C1 C2 119.7(5) . .
O1 C1 C2 116.7(5) . .
C8 C2 C3 118.5(5) . .
C8 C2 C1 122.8(5) . .
C3 C2 C1 118.6(5) . .
C4 C3 C2 121.3(5) . .
C4 C3 H3 119.3 . .
C2 C3 H3 119.3 . .
C3 C4 C5 119.2(6) . .
C3 C4 H4 120.4 . .
C5 C4 H4 120.4 . .
C4 C5 C6 121.0(5) . .
C4 C5 H5 119.5 . .
C6 C5 H5 119.5 . .
C8 C6 C5 119.8(5) . .
C8 C6 C7 120.0(5) . .
C5 C6 C7 120.2(5) . .
O3 C7 O4 123.9(5) . .
O3 C7 C6 119.2(5) . .
O4 C7 C6 116.9(5) . .
C6 C8 C2 120.1(5) . .
C6 C8 H8 120.0 . .
C2 C8 H8 120.0 . .
N1 C9 C10 123.0(6) . .
N1 C9 H9 118.5 . .
C10 C9 H9 118.5 . .
C11 C10 C9 119.0(6) . .
C11 C10 H10 120.5 . .
C9 C10 H10 120.5 . .
C10 C11 C12 119.8(6) . .
C10 C11 H11 120.1 . .
C12 C11 H11 120.1 . .
C11 C12 C13 118.0(6) . .
C11 C12 C20 122.5(6) . .
C13 C12 C20 119.5(6) . .
N1 C13 C12 122.3(5) . .
N1 C13 C14 118.2(5) . .
C12 C13 C14 119.5(5) . .
N2 C14 C18 123.9(6) . .
N2 C14 C13 115.4(5) . .
C18 C14 C13 120.7(5) . .
N2 C15 C16 124.2(6) . .
N2 C15 H15 117.9 . .
C16 C15 H15 117.9 . .
C17 C16 C15 118.5(6) . .
C17 C16 H16 120.7 . .
C15 C16 H16 120.7 . .
C16 C17 C18 119.1(6) . .
C16 C17 H17 120.4 . .
C18 C17 H17 120.4 . .
C14 C18 C17 118.1(6) . .
C14 C18 C19 119.9(5) . .
C17 C18 C19 122.0(6) . .
N4 C19 C20 121.4(6) . .
N4 C19 C18 119.3(6) . .
C20 C19 C18 119.3(5) . .
N3 C20 C19 120.2(6) . .
N3 C20 C12 118.8(6) . .
C19 C20 C12 121.0(6) . .
N3 C21 C22 122.7(7) . .
N3 C21 H21 118.7 . .
C22 C21 H21 118.7 . .
N4 C22 C21 121.9(7) . .
N4 C22 H22 119.1 . .
C21 C22 H22 119.1 . .
C9 N1 C13 117.8(5) . .
C9 N1 Pb1 118.4(4) . .
C13 N1 Pb1 123.8(4) . .
C15 N2 C14 116.1(5) . .
C15 N2 Pb1 124.4(4) . .
C14 N2 Pb1 119.5(4) . .
C21 N3 C20 118.0(6) . .
C22 N4 C19 115.7(6) . .
C1 O1 Pb1 99.8(3) . .
C1 O2 Pb1 84.7(3) . .
HW11 O1W HW12 98(10) . .
C7 O3 Pb1 89.3(3) . 1_445
C7 O4 Pb1 94.8(3) . 1_445
O1 Pb1 O4 82.60(14) . 1_665
O1 Pb1 N1 75.29(16) . .
O4 Pb1 N1 78.35(15) 1_665 .
O1 Pb1 O3 129.77(14) . 1_665
O4 Pb1 O3 51.81(14) 1_665 1_665
N1 Pb1 O3 75.75(16) . 1_665
O1 Pb1 N2 121.65(15) . .
O4 Pb1 N2 123.10(15) 1_665 .
N1 Pb1 N2 63.13(16) . .
O3 Pb1 N2 78.06(15) 1_665 .
O1 Pb1 O2W 117.1(3) . .
O4 Pb1 O2W 148.0(3) 1_665 .
N1 Pb1 O2W 129.1(3) . .
O3 Pb1 O2W 113.0(3) 1_665 .
N2 Pb1 O2W 69.8(3) . .
O1 Pb1 O2 50.99(13) . .
O4 Pb1 O2 132.69(13) 1_665 .
N1 Pb1 O2 80.98(15) . .
O3 Pb1 O2 154.55(15) 1_665 .
N2 Pb1 O2 82.36(14) . .
O2W Pb1 O2 74.4(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O2 1.242(7) .
C1 O1 1.275(6) .
C1 C2 1.497(7) .
C2 C8 1.392(7) .
C2 C3 1.402(8) .
C3 C4 1.367(9) .
C3 H3 0.9300 .
C4 C5 1.377(9) .
C4 H4 0.9300 .
C5 C6 1.383(8) .
C5 H5 0.9300 .
C6 C8 1.382(7) .
C6 C7 1.517(7) .
C7 O3 1.247(7) .
C7 O4 1.283(7) .
C8 H8 0.9300 .
C9 N1 1.340(8) .
C9 C10 1.391(10) .
C9 H9 0.9300 .
C10 C11 1.367(10) .
C10 H10 0.9300 .
C11 C12 1.393(9) .
C11 H11 0.9300 .
C12 C13 1.402(9) .
C12 C20 1.443(8) .
C13 N1 1.361(7) .
C13 C14 1.489(8) .
C14 N2 1.357(7) .
C14 C18 1.368(8) .
C15 N2 1.333(8) .
C15 C16 1.381(9) .
C15 H15 0.9300 .
C16 C17 1.367(10) .
C16 H16 0.9300 .
C17 C18 1.397(9) .
C17 H17 0.9300 .
C18 C19 1.472(9) .
C19 N4 1.348(8) .
C19 C20 1.416(9) .
C20 N3 1.373(9) .
C21 N3 1.240(10) .
C21 C22 1.437(11) .
C21 H21 0.9300 .
C22 N4 1.328(10) .
C22 H22 0.9300 .
N1 Pb1 2.504(5) .
N2 Pb1 2.671(5) .
O1 Pb1 2.382(4) .
O2 Pb1 2.724(4) .
O1W HW11 0.86(2) .
O1W HW12 0.86(2) .
O3 Pb1 2.621(4) 1_445
O2W Pb1 2.721(14) .
O4 Pb1 2.482(4) 1_445
Pb1 O4 2.482(4) 1_665
Pb1 O3 2.621(4) 1_665
