#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/10/4511045.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_4511045
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         'C27 H16 N4 O4 Pb, 0.25(O2), 0.25(O)'
_chemical_formula_sum            'C27 H19 N4 O4.75 Pb'
_chemical_formula_weight         682.65
_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                94.19(3)
_cell_angle_beta                 106.42(3)
_cell_angle_gamma                105.72(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4663(19)
_cell_length_b                   10.833(2)
_cell_length_c                   13.159(3)
_cell_measurement_reflns_used    10973
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.26
_cell_volume                     1229.5(5)
_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 0.993
_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  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0528
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12119
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.26
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    6.906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.844
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             658
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.085
_refine_diff_density_max         1.329
_refine_diff_density_min         -1.078
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5545
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0353
_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)+(0.0381P)²+0.3692P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0788
_reflns_number_gt                4773
_reflns_number_total             5545
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg801085d_si_002.cif
_cod_data_source_block           compound12
_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        1229.5(4)
_cod_original_sg_symbol_Hall     '-p 1'
_cod_database_code               4511045
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 0.4022(6) -0.1248(6) 0.1859(4) 0.0394(13) Uani 1 1 d .
H1 H 0.4804 -0.1343 0.1591 0.047 Uiso 1 1 calc R
C2 C 0.3086(7) -0.2337(6) 0.2079(5) 0.0452(14) Uani 1 1 d .
H2 H 0.3245 -0.3139 0.1962 0.054 Uiso 1 1 calc R
C3 C 0.1928(6) -0.2239(6) 0.2469(5) 0.0399(12) Uani 1 1 d .
H3 H 0.1289 -0.2967 0.2624 0.048 Uiso 1 1 calc R
C4 C 0.1717(5) -0.1006(5) 0.2633(4) 0.0313(11) Uani 1 1 d .
C5 C 0.2708(5) 0.0055(5) 0.2387(4) 0.0288(10) Uani 1 1 d .
C6 C 0.2513(5) 0.1346(5) 0.2517(4) 0.0293(10) Uani 1 1 d .
C7 C 0.3336(6) 0.3496(6) 0.2354(5) 0.0454(14) Uani 1 1 d .
H7 H 0.4008 0.4168 0.2161 0.055 Uiso 1 1 calc R
C8 C 0.2186(7) 0.3768(6) 0.2718(6) 0.0520(16) Uani 1 1 d .
H8 H 0.2107 0.4606 0.2776 0.062 Uiso 1 1 calc R
C9 C 0.1179(6) 0.2783(6) 0.2988(5) 0.0407(13) Uani 1 1 d .
H9 H 0.0411 0.2950 0.3238 0.049 Uiso 1 1 calc R
C10 C 0.1302(5) 0.1532(5) 0.2889(4) 0.0308(11) Uani 1 1 d .
C11 C 0.0326(5) 0.0426(5) 0.3117(4) 0.0301(11) Uani 1 1 d .
C12 C 0.0503(5) -0.0785(5) 0.3006(4) 0.0310(11) Uani 1 1 d .
C13 C -0.1460(5) -0.1015(5) 0.3547(4) 0.0324(11) Uani 1 1 d .
C14 C -0.2748(6) -0.1605(6) 0.3953(4) 0.0362(12) Uani 1 1 d .
C15 C -0.3282(6) -0.2950(6) 0.3841(5) 0.0467(15) Uani 1 1 d .
H15 H -0.2886 -0.3456 0.3464 0.056 Uiso 1 1 calc R
C16 C -0.4410(7) -0.3549(6) 0.4290(5) 0.0528(16) Uani 1 1 d .
H16 H -0.4749 -0.4449 0.4226 0.063 Uiso 1 1 calc R
C17 C -0.5018(6) -0.2795(7) 0.4828(5) 0.0487(15) Uani 1 1 d .
H17 H -0.5776 -0.3190 0.5124 0.058 Uiso 1 1 calc R
C18 C -0.4514(6) -0.1473(7) 0.4928(5) 0.0492(16) Uani 1 1 d .
H18 H -0.4932 -0.0973 0.5292 0.059 Uiso 1 1 calc R
C19 C -0.3381(6) -0.0865(6) 0.4490(4) 0.0412(13) Uani 1 1 d .
H19 H -0.3049 0.0037 0.4558 0.049 Uiso 1 1 calc R
C20 C 0.7829(5) 0.0953(6) 0.0757(4) 0.0370(13) Uani 1 1 d .
C21 C 0.8966(5) 0.0439(6) 0.0373(4) 0.0333(12) Uani 1 1 d .
C22 C 0.8893(5) -0.0846(6) 0.0325(4) 0.0364(12) Uani 1 1 d .
H22 H 0.8144 -0.1417 0.0539 0.044 Uiso 1 1 calc R
C23 C 0.9925(5) -0.1304(6) -0.0041(4) 0.0387(13) Uani 1 1 d .
H23 H 0.9880 -0.2174 -0.0065 0.046 Uiso 1 1 calc R
C24 C 0.7540(5) 0.3367(5) 0.3146(4) 0.0300(11) Uani 1 1 d .
C25 C 0.8812(5) 0.4204(5) 0.4112(4) 0.0278(10) Uani 1 1 d .
C26 C 0.9584(5) 0.5471(5) 0.4051(4) 0.0323(11) Uani 1 1 d .
H26 H 0.9312 0.5789 0.3410 0.039 Uiso 1 1 calc R
C27 C 1.0755(5) 0.6271(5) 0.4932(4) 0.0336(11) Uani 1 1 d .
H27 H 1.1248 0.7122 0.4882 0.040 Uiso 1 1 calc R
N1 N 0.3513(5) 0.2331(4) 0.2271(3) 0.0350(10) Uani 1 1 d .
N2 N 0.3877(4) -0.0069(4) 0.2005(3) 0.0326(10) Uani 1 1 d .
N3 N -0.0601(5) -0.1684(4) 0.3280(4) 0.0354(10) Uani 1 1 d .
N4 N -0.0946(4) 0.0266(4) 0.3471(3) 0.0318(9) Uani 1 1 d .
H4 H -0.1337 0.0861 0.3615 0.038 Uiso 1 1 calc R
O1 O 0.6694(4) 0.0116(4) 0.0895(3) 0.0451(10) Uani 1 1 d .
O2 O 0.8021(4) 0.2132(4) 0.0908(4) 0.0527(12) Uani 1 1 d .
O1W O 0.9331(17) 0.4723(12) 0.0819(13) 0.110(5) Uani 0.50 1 d P
O3 O 0.6914(4) 0.3929(4) 0.2438(3) 0.0411(9) Uani 1 1 d .
O2W O 0.757(2) 0.6126(17) 0.1252(18) 0.066(5) Uani 0.25 1 d P
O4 O 0.7174(4) 0.2143(4) 0.3086(3) 0.0373(9) Uani 1 1 d .
Pb1 Pb 0.532803(18) 0.176839(19) 0.121908(14) 0.03089(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
N2 C1 C2 123.9(5) . .
N2 C1 H1 118.1 . .
C2 C1 H1 118.1 . .
C3 C2 C1 119.9(5) . .
C3 C2 H2 120.1 . .
C1 C2 H2 120.1 . .
C2 C3 C4 118.5(5) . .
C2 C3 H3 120.7 . .
C4 C3 H3 120.7 . .
C5 C4 C3 118.5(4) . .
C5 C4 C12 117.7(5) . .
C3 C4 C12 123.8(5) . .
N2 C5 C4 121.8(5) . .
N2 C5 C6 117.7(4) . .
C4 C5 C6 120.6(4) . .
N1 C6 C10 122.1(5) . .
N1 C6 C5 117.6(4) . .
C10 C6 C5 120.3(5) . .
N1 C7 C8 123.0(6) . .
N1 C7 H7 118.5 . .
C8 C7 H7 118.5 . .
C9 C8 C7 119.0(6) . .
C9 C8 H8 120.5 . .
C7 C8 H8 120.5 . .
C8 C9 C10 119.9(5) . .
C8 C9 H9 120.0 . .
C10 C9 H9 120.0 . .
C9 C10 C11 125.9(4) . .
C9 C10 C6 117.3(5) . .
C11 C10 C6 116.9(5) . .
C12 C11 N4 105.1(4) . .
C12 C11 C10 123.4(4) . .
N4 C11 C10 131.5(4) . .
C11 C12 N3 111.5(4) . .
C11 C12 C4 121.1(5) . .
N3 C12 C4 127.4(5) . .
N3 C13 N4 112.3(4) . .
N3 C13 C14 122.4(5) . .
N4 C13 C14 125.2(4) . .
C19 C14 C15 119.1(5) . .
C19 C14 C13 122.3(5) . .
C15 C14 C13 118.5(5) . .
C14 C15 C16 120.5(5) . .
C14 C15 H15 119.7 . .
C16 C15 H15 119.7 . .
C17 C16 C15 119.5(6) . .
C17 C16 H16 120.3 . .
C15 C16 H16 120.3 . .
C18 C17 C16 120.3(5) . .
C18 C17 H17 119.9 . .
C16 C17 H17 119.9 . .
C17 C18 C19 120.7(5) . .
C17 C18 H18 119.6 . .
C19 C18 H18 119.6 . .
C14 C19 C18 119.8(6) . .
C14 C19 H19 120.1 . .
C18 C19 H19 120.1 . .
O2 C20 O1 123.0(5) . .
O2 C20 C21 120.1(5) . .
O1 C20 C21 117.0(5) . .
C22 C21 C23 120.2(4) . 2_755
C22 C21 C20 121.3(5) . .
C23 C21 C20 118.5(5) 2_755 .
C21 C22 C23 120.6(5) . .
C21 C22 H22 119.7 . .
C23 C22 H22 119.7 . .
C22 C23 C21 119.2(6) . 2_755
C22 C23 H23 120.4 . .
C21 C23 H23 120.4 2_755 .
O3 C24 O4 123.6(4) . .
O3 C24 C25 117.4(5) . .
O4 C24 C25 119.0(5) . .
O3 C24 Pb1 62.7(3) . .
O4 C24 Pb1 61.0(3) . .
C25 C24 Pb1 174.9(3) . .
C26 C25 C27 119.1(4) . 2_766
C26 C25 C24 119.8(5) . .
C27 C25 C24 121.1(5) 2_766 .
C25 C26 C27 121.1(5) . .
C25 C26 H26 119.4 . .
C27 C26 H26 119.4 . .
C26 C27 C25 119.8(5) . 2_766
C26 C27 H27 120.1 . .
C25 C27 H27 120.1 2_766 .
C7 N1 C6 118.8(4) . .
C7 N1 Pb1 121.2(4) . .
C6 N1 Pb1 118.5(3) . .
C1 N2 C5 117.5(5) . .
C1 N2 Pb1 120.1(3) . .
C5 N2 Pb1 121.0(4) . .
C13 N3 C12 104.4(4) . .
C13 N4 C11 106.8(4) . .
C13 N4 H4 126.6 . .
C11 N4 H4 126.6 . .
C20 O1 Pb1 94.4(3) . .
C20 O2 Pb1 91.9(3) . .
C24 O3 Pb1 91.4(3) . .
C24 O4 Pb1 92.8(3) . .
O4 Pb1 O3 51.96(13) . .
O4 Pb1 O1 82.48(12) . .
O3 Pb1 O1 118.94(12) . .
O4 Pb1 N2 79.26(13) . .
O3 Pb1 N2 118.81(13) . .
O1 Pb1 N2 82.01(13) . .
O4 Pb1 O2 76.71(13) . .
O3 Pb1 O2 78.30(12) . .
O1 Pb1 O2 50.29(13) . .
N2 Pb1 O2 128.52(14) . .
O4 Pb1 N1 82.18(12) . .
O3 Pb1 N1 74.60(13) . .
O1 Pb1 N1 143.85(14) . .
N2 Pb1 N1 63.05(13) . .
O2 Pb1 N1 152.31(13) . .
O4 Pb1 C24 26.20(14) . .
O3 Pb1 C24 25.80(14) . .
O1 Pb1 C24 100.66(13) . .
N2 Pb1 C24 100.35(14) . .
O2 Pb1 C24 74.92(13) . .
N1 Pb1 C24 78.21(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N2 1.327(7) .
C1 C2 1.375(8) .
C1 H1 0.9300 .
C2 C3 1.360(7) .
C2 H2 0.9300 .
C3 C4 1.414(7) .
C3 H3 0.9300 .
C4 C5 1.395(7) .
C4 C12 1.439(6) .
C5 N2 1.371(5) .
C5 C6 1.462(7) .
C6 N1 1.348(7) .
C6 C10 1.422(6) .
C7 N1 1.318(7) .
C7 C8 1.396(7) .
C7 H7 0.9300 .
C8 C9 1.367(8) .
C8 H8 0.9300 .
C9 C10 1.392(8) .
C9 H9 0.9300 .
C10 C11 1.410(7) .
C11 C12 1.369(7) .
C11 N4 1.383(5) .
C12 N3 1.372(6) .
C13 N3 1.325(6) .
C13 N4 1.362(7) .
C13 C14 1.475(7) .
C14 C19 1.385(7) .
C14 C15 1.388(9) .
C15 C16 1.395(8) .
C15 H15 0.9300 .
C16 C17 1.378(8) .
C16 H16 0.9300 .
C17 C18 1.365(9) .
C17 H17 0.9300 .
C18 C19 1.392(8) .
C18 H18 0.9300 .
C19 H19 0.9300 .
C20 O2 1.233(7) .
C20 O1 1.271(7) .
C20 C21 1.522(6) .
C21 C22 1.371(8) .
C21 C23 1.398(7) 2_755
C22 C23 1.387(7) .
C22 H22 0.9300 .
C23 C21 1.398(7) 2_755
C23 H23 0.9300 .
C24 O3 1.247(7) .
C24 O4 1.266(6) .
C24 C25 1.504(6) .
C24 Pb1 2.865(5) .
C25 C26 1.389(7) .
C25 C27 1.391(7) 2_766
C26 C27 1.389(7) .
C26 H26 0.9300 .
C27 C25 1.391(7) 2_766
C27 H27 0.9300 .
N1 Pb1 2.651(4) .
N2 Pb1 2.558(5) .
N4 H4 0.8600 .
O1 Pb1 2.551(4) .
O2 Pb1 2.625(4) .
O3 Pb1 2.548(4) .
O4 Pb1 2.510(4) .
