#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/10/4511039.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_4511039
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         'C22 H12 N4 O4 Pb, O'
_chemical_formula_sum            'C22 H14 N4 O5 Pb'
_chemical_formula_weight         621.56
_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                113.17(3)
_cell_angle_beta                 96.48(3)
_cell_angle_gamma                92.11(3)
_cell_formula_units_Z            2
_cell_length_a                   7.2740(15)
_cell_length_b                   12.231(2)
_cell_length_c                   12.714(3)
_cell_measurement_reflns_used    9294
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.99
_cell_volume                     1029.2(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 0.996
_diffrn_measured_fraction_theta_max 0.987
_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  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0441
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10079
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.99
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    8.240
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.006
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.462
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.188
_refine_diff_density_max         1.790
_refine_diff_density_min         -1.607
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4661
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0370P)²+1.0882P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0729
_reflns_number_gt                4309
_reflns_number_total             4661
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg801085d_si_002.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_cell_volume        1029.1(4)
_cod_original_sg_symbol_Hall     '-p 1'
_cod_database_code               4511039
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 1.7688(10) 0.2190(5) 0.1254(5) 0.0566(16) Uani 1 1 d .
H1 H 1.7650 0.1811 0.1759 0.068 Uiso 1 1 calc R
C2 C 1.7926(12) 0.1505(5) 0.0104(6) 0.072(2) Uani 1 1 d .
H2 H 1.8038 0.0689 -0.0145 0.086 Uiso 1 1 calc R
C3 C 1.7989(10) 0.2052(5) -0.0635(5) 0.0570(15) Uani 1 1 d .
H3 H 1.8172 0.1617 -0.1395 0.068 Uiso 1 1 calc R
C4 C 1.7779(7) 0.3263(4) -0.0251(4) 0.0384(11) Uani 1 1 d .
C5 C 1.7526(6) 0.3893(4) 0.0908(4) 0.0353(10) Uani 1 1 d .
C6 C 1.7304(6) 0.5166(4) 0.1337(4) 0.0332(10) Uani 1 1 d .
C7 C 1.6845(8) 0.6895(5) 0.2856(5) 0.0472(13) Uani 1 1 d .
H7 H 1.6668 0.7288 0.3624 0.057 Uiso 1 1 calc R
C8 C 1.6896(8) 0.7543(5) 0.2187(6) 0.0521(14) Uani 1 1 d .
H8 H 1.6750 0.8356 0.2505 0.063 Uiso 1 1 calc R
C9 C 1.7158(8) 0.6998(5) 0.1060(5) 0.0466(13) Uani 1 1 d .
H9 H 1.7199 0.7432 0.0603 0.056 Uiso 1 1 calc R
C10 C 1.7363(6) 0.5772(4) 0.0603(4) 0.0351(10) Uani 1 1 d .
C11 C 1.7618(6) 0.5121(5) -0.0592(4) 0.0363(10) Uani 1 1 d .
C12 C 1.7793(7) 0.3892(5) -0.1014(4) 0.0380(11) Uani 1 1 d .
C13 C 1.7986(8) 0.3859(5) -0.2796(5) 0.0487(13) Uani 1 1 d .
H13 H 1.8084 0.3453 -0.3576 0.058 Uiso 1 1 calc R
C14 C 1.7846(8) 0.5081(6) -0.2370(5) 0.0512(14) Uani 1 1 d .
H14 H 1.7890 0.5465 -0.2870 0.061 Uiso 1 1 calc R
C15 C 1.4253(6) 0.2967(4) 0.4068(4) 0.0306(9) Uani 1 1 d .
C16 C 1.3138(6) 0.1850(4) 0.3959(4) 0.0297(9) Uani 1 1 d .
C17 C 1.4134(7) 0.0883(4) 0.3898(5) 0.0421(12) Uani 1 1 d .
H17 H 1.5417 0.0948 0.3919 0.050 Uiso 1 1 calc R
C18 C 1.3249(8) -0.0164(4) 0.3805(5) 0.0479(13) Uani 1 1 d .
H18 H 1.3931 -0.0805 0.3761 0.057 Uiso 1 1 calc R
C19 C 1.1364(8) -0.0272(4) 0.3778(5) 0.0464(13) Uani 1 1 d .
H19 H 1.0769 -0.0986 0.3714 0.056 Uiso 1 1 calc R
C20 C 1.0334(7) 0.0684(4) 0.3846(5) 0.0408(11) Uani 1 1 d .
H20 H 0.9052 0.0606 0.3822 0.049 Uiso 1 1 calc R
C21 C 1.1220(6) 0.1759(4) 0.3950(4) 0.0296(9) Uani 1 1 d .
C22 C 1.0073(6) 0.2771(4) 0.4021(4) 0.0300(9) Uani 1 1 d .
N1 N 1.7515(6) 0.3348(4) 0.1648(4) 0.0426(10) Uani 1 1 d .
N2 N 1.7040(6) 0.5729(4) 0.2451(4) 0.0388(9) Uani 1 1 d .
N3 N 1.7652(6) 0.5722(4) -0.1283(4) 0.0466(10) Uani 1 1 d .
N4 N 1.7985(6) 0.3252(4) -0.2141(4) 0.0483(11) Uani 1 1 d .
O1 O 1.4581(4) 0.3025(3) 0.3141(3) 0.0389(8) Uani 1 1 d .
O2 O 1.4919(4) 0.3711(3) 0.5050(3) 0.0381(8) Uani 1 1 d .
O1W O 1.2592(12) 0.1584(6) 0.0963(6) 0.121(3) Uani 1 1 d .
O3 O 1.0859(4) 0.3734(3) 0.4083(3) 0.0393(8) Uani 1 1 d .
O4 O 0.8356(5) 0.2617(3) 0.4004(4) 0.0569(11) Uani 1 1 d .
Pb1 Pb 1.72602(2) 0.447286(13) 0.386987(14) 0.02949(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
N1 C1 C2 122.8(6) . .
N1 C1 H1 118.6 . .
C2 C1 H1 118.6 . .
C3 C2 C1 118.9(5) . .
C3 C2 H2 120.6 . .
C1 C2 H2 120.6 . .
C2 C3 C4 119.6(5) . .
C2 C3 H3 120.2 . .
C4 C3 H3 120.2 . .
C3 C4 C5 118.5(5) . .
C3 C4 C12 122.0(5) . .
C5 C4 C12 119.5(4) . .
N1 C5 C4 121.5(4) . .
N1 C5 C6 118.7(4) . .
C4 C5 C6 119.8(5) . .
N2 C6 C10 121.9(5) . .
N2 C6 C5 117.7(4) . .
C10 C6 C5 120.4(4) . .
N2 C7 C8 122.8(5) . .
N2 C7 H7 118.6 . .
C8 C7 H7 118.6 . .
C9 C8 C7 120.2(5) . .
C9 C8 H8 119.9 . .
C7 C8 H8 119.9 . .
C8 C9 C10 118.7(5) . .
C8 C9 H9 120.7 . .
C10 C9 H9 120.7 . .
C9 C10 C6 118.1(5) . .
C9 C10 C11 122.2(5) . .
C6 C10 C11 119.7(5) . .
N3 C11 C12 121.3(5) . .
N3 C11 C10 118.6(5) . .
C12 C11 C10 120.1(5) . .
N4 C12 C11 121.3(5) . .
N4 C12 C4 118.2(5) . .
C11 C12 C4 120.5(4) . .
N4 C13 C14 122.6(5) . .
N4 C13 H13 118.7 . .
C14 C13 H13 118.7 . .
N3 C14 C13 122.7(6) . .
N3 C14 H14 118.6 . .
C13 C14 H14 118.6 . .
O2 C15 O1 124.2(4) . .
O2 C15 C16 119.0(4) . .
O1 C15 C16 116.5(4) . .
C17 C16 C21 119.5(4) . .
C17 C16 C15 116.5(4) . .
C21 C16 C15 123.9(4) . .
C18 C17 C16 120.8(4) . .
C18 C17 H17 119.6 . .
C16 C17 H17 119.6 . .
C19 C18 C17 120.3(4) . .
C19 C18 H18 119.9 . .
C17 C18 H18 119.9 . .
C18 C19 C20 120.2(4) . .
C18 C19 H19 119.9 . .
C20 C19 H19 119.9 . .
C19 C20 C21 120.2(4) . .
C19 C20 H20 119.9 . .
C21 C20 H20 119.9 . .
C16 C21 C20 119.1(4) . .
C16 C21 C22 122.1(4) . .
C20 C21 C22 118.9(4) . .
O4 C22 O3 122.7(4) . .
O4 C22 C21 118.2(4) . .
O3 C22 C21 119.2(4) . .
C1 N1 C5 118.6(5) . .
C1 N1 Pb1 117.5(4) . .
C5 N1 Pb1 123.9(3) . .
C7 N2 C6 118.3(5) . .
C7 N2 Pb1 122.3(4) . .
C6 N2 Pb1 119.1(3) . .
C14 N3 C11 116.1(5) . .
C13 N4 C12 115.9(5) . .
C15 O1 Pb1 99.7(3) . .
C15 O2 Pb1 84.1(3) . .
C22 O4 Pb1 102.0(3) . 1_455
O1 Pb1 O4 74.52(12) . 1_655
O1 Pb1 N1 76.12(13) . .
O4 Pb1 N1 84.22(15) 1_655 .
O1 Pb1 O2 50.19(11) . .
O4 Pb1 O2 71.32(11) 1_655 .
N1 Pb1 O2 124.78(12) . .
O1 Pb1 N2 105.03(12) . .
O4 Pb1 N2 142.67(14) 1_655 .
N1 Pb1 N2 60.29(13) . .
O2 Pb1 N2 137.53(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.320(7) .
C1 C2 1.404(9) .
C1 H1 0.9300 .
C2 C3 1.354(9) .
C2 H2 0.9300 .
C3 C4 1.386(7) .
C3 H3 0.9300 .
C4 C5 1.406(7) .
C4 C12 1.456(7) .
C5 N1 1.351(7) .
C5 C6 1.455(7) .
C6 N2 1.349(6) .
C6 C10 1.405(7) .
C7 N2 1.332(6) .
C7 C8 1.374(8) .
C7 H7 0.9300 .
C8 C9 1.361(8) .
C8 H8 0.9300 .
C9 C10 1.399(7) .
C9 H9 0.9300 .
C10 C11 1.448(7) .
C11 N3 1.351(7) .
C11 C12 1.400(7) .
C12 N4 1.362(7) .
C13 N4 1.317(8) .
C13 C14 1.387(9) .
C13 H13 0.9300 .
C14 N3 1.320(8) .
C14 H14 0.9300 .
C15 O2 1.249(6) .
C15 O1 1.256(6) .
C15 C16 1.513(6) .
C16 C17 1.391(6) .
C16 C21 1.394(6) .
C17 C18 1.368(7) .
C17 H17 0.9300 .
C18 C19 1.367(8) .
C18 H18 0.9300 .
C19 C20 1.391(7) .
C19 H19 0.9300 .
C20 C21 1.394(6) .
C20 H20 0.9300 .
C21 C22 1.497(6) .
C22 O4 1.253(5) .
C22 O3 1.260(5) .
N1 Pb1 2.643(4) .
N2 Pb1 2.788(4) .
O1 Pb1 2.416(3) .
O2 Pb1 2.753(4) .
O4 Pb1 2.495(4) 1_455
Pb1 O4 2.495(4) 1_655
