#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/10/4511044.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_4511044
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         '2(C27 H16 N4 O4 Pb), 4(O), 0.5(O2)'
_chemical_formula_sum            'C54 H37 N8 O13 Pb2'
_chemical_formula_weight         1420.30
_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                101.071(2)
_cell_angle_beta                 90.383(3)
_cell_angle_gamma                114.053(3)
_cell_formula_units_Z            1
_cell_length_a                   9.3797(3)
_cell_length_b                   9.4191(3)
_cell_length_c                   15.6963(5)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.8724
_cell_measurement_theta_min      5.1796
_cell_volume                     1237.17(8)
_computing_cell_refinement       CrysAlis
_computing_data_collection       'CrysAlis (Oxford Diffraction, 2006)'
_computing_data_reduction        CrysAlis
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Oxford Diffraction Gemini R Ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0210
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12254
_diffrn_reflns_theta_full        66.99
_diffrn_reflns_theta_max         66.99
_diffrn_reflns_theta_min         5.19
_exptl_absorpt_coefficient_mu    13.726
_exptl_absorpt_correction_T_max  0.507
_exptl_absorpt_correction_T_min  0.319
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis (Oxford Diffraction, 2006)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.906
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             685
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.962
_refine_diff_density_rms         0.093
_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     352
_refine_ls_number_reflns         4327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0255
_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)+(0.0379P)²+1.4068P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0658
_reflns_number_gt                4062
_reflns_number_total             4327
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            cg801085d_si_002.cif
_cod_data_source_block           compound11
_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        1237.17(7)
_cod_original_sg_symbol_Hall     '-p 1'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4511044
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 0.4464(5) 0.6558(5) 0.0930(3) 0.0458(10) Uani 1 1 d .
C2 C 0.5477(5) 0.7829(5) 0.0471(3) 0.0407(9) Uani 1 1 d .
C3 C 0.4982(5) 0.7847(5) -0.0365(3) 0.0459(10) Uani 1 1 d .
H3 H 0.4034 0.7059 -0.0642 0.055 Uiso 1 1 calc R
C4 C 0.5883(6) 0.9020(6) -0.0781(3) 0.0517(11) Uani 1 1 d .
H4 H 0.5533 0.9041 -0.1332 0.062 Uiso 1 1 calc R
C5 C 0.7313(6) 1.0172(6) -0.0379(3) 0.0470(10) Uani 1 1 d .
H5 H 0.7929 1.0956 -0.0666 0.056 Uiso 1 1 calc R
C6 C 0.7839(5) 1.0163(5) 0.0457(3) 0.0412(9) Uani 1 1 d .
C7 C 0.9385(5) 1.1420(5) 0.0889(3) 0.0435(9) Uani 1 1 d .
C8 C 0.6904(5) 0.8990(5) 0.0871(3) 0.0409(9) Uani 1 1 d .
H8 H 0.7239 0.8980 0.1427 0.049 Uiso 1 1 calc R
C9 C 0.3553(6) 0.5063(7) 0.3842(3) 0.0566(12) Uani 1 1 d .
H9 H 0.4262 0.4622 0.3683 0.068 Uiso 1 1 calc R
C10 C 0.3544(6) 0.5704(7) 0.4726(3) 0.0587(13) Uani 1 1 d .
H10 H 0.4265 0.5718 0.5141 0.070 Uiso 1 1 calc R
C11 C 0.2475(6) 0.6307(6) 0.4976(3) 0.0485(10) Uani 1 1 d .
H11 H 0.2442 0.6708 0.5561 0.058 Uiso 1 1 calc R
C12 C 0.1434(5) 0.6312(5) 0.4338(3) 0.0405(9) Uani 1 1 d .
C13 C 0.1548(5) 0.5697(5) 0.3456(3) 0.0390(8) Uani 1 1 d .
C14 C 0.0566(5) 0.5768(5) 0.2758(2) 0.0383(8) Uani 1 1 d .
C15 C 0.0017(6) 0.5414(6) 0.1282(3) 0.0534(11) Uani 1 1 d .
H15 H 0.0200 0.5078 0.0713 0.064 Uiso 1 1 calc R
C16 C -0.1095(7) 0.6042(7) 0.1402(3) 0.0610(13) Uani 1 1 d .
H16 H -0.1616 0.6144 0.0927 0.073 Uiso 1 1 calc R
C17 C -0.1404(6) 0.6508(6) 0.2237(3) 0.0526(11) Uani 1 1 d .
H17 H -0.2178 0.6883 0.2336 0.063 Uiso 1 1 calc R
C18 C -0.0535(5) 0.6411(5) 0.2942(3) 0.0424(9) Uani 1 1 d .
C19 C -0.0661(5) 0.6973(5) 0.3844(3) 0.0428(9) Uani 1 1 d .
C20 C 0.0288(5) 0.6939(5) 0.4497(2) 0.0406(9) Uani 1 1 d .
C21 C -0.1198(5) 0.8058(5) 0.5071(3) 0.0427(9) Uani 1 1 d .
C22 C -0.1914(5) 0.8828(5) 0.5725(3) 0.0440(9) Uani 1 1 d .
C23 C -0.1424(6) 0.9154(6) 0.6609(3) 0.0561(12) Uani 1 1 d .
H23 H -0.0636 0.8884 0.6785 0.067 Uiso 1 1 calc R
C24 C -0.2101(7) 0.9873(7) 0.7224(3) 0.0622(13) Uani 1 1 d .
H24 H -0.1767 1.0085 0.7812 0.075 Uiso 1 1 calc R
C25 C -0.3269(7) 1.0281(7) 0.6972(4) 0.0644(13) Uani 1 1 d .
H25 H -0.3724 1.0767 0.7388 0.077 Uiso 1 1 calc R
C26 C -0.3755(7) 0.9963(8) 0.6101(4) 0.0683(15) Uani 1 1 d .
H26 H -0.4543 1.0238 0.5930 0.082 Uiso 1 1 calc R
C27 C -0.3094(6) 0.9244(7) 0.5479(3) 0.0568(12) Uani 1 1 d .
H27 H -0.3437 0.9035 0.4892 0.068 Uiso 1 1 calc R
O1 O 0.3239(4) 0.5459(4) 0.0514(2) 0.0559(8) Uani 1 1 d .
O2 O 0.4847(5) 0.6636(5) 0.1708(2) 0.0696(11) Uani 1 1 d .
O1W O 0.6451(5) 0.8621(5) 0.3257(2) 0.0655(9) Uani 1 1 d .
O3 O 0.9720(4) 1.1560(4) 0.1692(2) 0.0579(8) Uani 1 1 d .
O2W O 0.8126(5) 1.1746(5) 0.3150(2) 0.0716(10) Uani 1 1 d .
O4 O 1.0303(4) 1.2324(4) 0.04492(19) 0.0518(7) Uani 1 1 d .
O3W O 0.5883(15) 0.3293(14) 0.2897(8) 0.114(4) Uani 0.50 1 d P
Pb1 Pb 0.250156(19) 0.379805(19) 0.157802(10) 0.04354(7) Uani 1 1 d .
N1 N 0.2578(4) 0.5067(5) 0.3226(2) 0.0450(8) Uani 1 1 d .
N2 N 0.0829(4) 0.5263(4) 0.1921(2) 0.0436(8) Uani 1 1 d .
N3 N -0.0053(4) 0.7635(4) 0.5276(2) 0.0419(8) Uani 1 1 d .
H3A H 0.0378 0.7771 0.5788 0.050 Uiso 1 1 calc R
N4 N -0.1618(4) 0.7671(5) 0.4210(2) 0.0449(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 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 '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 122.2(4) . .
O2 C1 C2 119.6(4) . .
O1 C1 C2 118.2(4) . .
C8 C2 C3 119.2(4) . .
C8 C2 C1 120.6(4) . .
C3 C2 C1 120.2(4) . .
C4 C3 C2 120.6(4) . .
C4 C3 H3 119.7 . .
C2 C3 H3 119.7 . .
C3 C4 C5 119.9(4) . .
C3 C4 H4 120.1 . .
C5 C4 H4 120.1 . .
C4 C5 C6 120.4(4) . .
C4 C5 H5 119.8 . .
C6 C5 H5 119.8 . .
C8 C6 C5 118.8(4) . .
C8 C6 C7 121.1(4) . .
C5 C6 C7 120.0(4) . .
O4 C7 O3 121.8(4) . .
O4 C7 C6 119.2(4) . .
O3 C7 C6 119.0(4) . .
C6 C8 C2 121.1(4) . .
C6 C8 H8 119.4 . .
C2 C8 H8 119.4 . .
N1 C9 C10 121.9(4) . .
N1 C9 H9 119.0 . .
C10 C9 H9 119.0 . .
C11 C10 C9 119.9(4) . .
C11 C10 H10 120.1 . .
C9 C10 H10 120.1 . .
C10 C11 C12 119.0(4) . .
C10 C11 H11 120.5 . .
C12 C11 H11 120.5 . .
C11 C12 C13 118.0(4) . .
C11 C12 C20 125.2(4) . .
C13 C12 C20 116.7(3) . .
N1 C13 C12 122.1(4) . .
N1 C13 C14 117.4(4) . .
C12 C13 C14 120.5(4) . .
N2 C14 C18 122.0(4) . .
N2 C14 C13 117.0(4) . .
C18 C14 C13 120.9(4) . .
N2 C15 C16 124.3(4) . .
N2 C15 H15 117.8 . .
C16 C15 H15 117.8 . .
C17 C16 C15 118.5(4) . .
C17 C16 H16 120.7 . .
C15 C16 H16 120.7 . .
C16 C17 C18 119.1(4) . .
C16 C17 H17 120.4 . .
C18 C17 H17 120.4 . .
C14 C18 C17 118.3(4) . .
C14 C18 C19 117.2(4) . .
C17 C18 C19 124.5(4) . .
C20 C19 N4 108.7(4) . .
C20 C19 C18 121.7(4) . .
N4 C19 C18 129.5(4) . .
C19 C20 N3 107.9(4) . .
C19 C20 C12 122.9(4) . .
N3 C20 C12 129.2(4) . .
N4 C21 N3 112.4(4) . .
N4 C21 C22 124.5(4) . .
N3 C21 C22 123.1(4) . .
C27 C22 C23 118.6(4) . .
C27 C22 C21 120.9(4) . .
C23 C22 C21 120.5(4) . .
C24 C23 C22 120.4(5) . .
C24 C23 H23 119.8 . .
C22 C23 H23 119.8 . .
C25 C24 C23 120.5(5) . .
C25 C24 H24 119.8 . .
C23 C24 H24 119.8 . .
C26 C25 C24 119.3(5) . .
C26 C25 H25 120.3 . .
C24 C25 H25 120.3 . .
C25 C26 C27 121.0(5) . .
C25 C26 H26 119.5 . .
C27 C26 H26 119.5 . .
C26 C27 C22 120.2(5) . .
C26 C27 H27 119.9 . .
C22 C27 H27 119.9 . .
C1 O1 Pb1 98.4(3) . .
C1 O2 Pb1 87.7(3) . .
C7 O3 Pb1 88.9(3) . 1_665
C7 O4 Pb1 97.9(3) . 1_665
O1 Pb1 O4 78.90(10) . 1_445
O1 Pb1 N2 79.94(12) . .
O4 Pb1 N2 78.21(11) 1_445 .
O1 Pb1 N1 120.18(12) . .
O4 Pb1 N1 131.05(11) 1_445 .
N2 Pb1 N1 63.75(11) . .
O1 Pb1 O3 127.72(10) . 1_445
O4 Pb1 O3 51.19(10) 1_445 1_445
N2 Pb1 O3 76.00(12) . 1_445
N1 Pb1 O3 88.86(11) . 1_445
O1 Pb1 O2 51.09(10) . .
O4 Pb1 O2 129.51(10) 1_445 .
N2 Pb1 O2 85.79(14) . .
N1 Pb1 O2 79.04(12) . .
O3 Pb1 O2 161.27(14) 1_445 .
C9 N1 C13 119.0(4) . .
C9 N1 Pb1 122.7(3) . .
C13 N1 Pb1 118.2(3) . .
C15 N2 C14 117.7(4) . .
C15 N2 Pb1 119.6(3) . .
C14 N2 Pb1 122.3(3) . .
C21 N3 C20 105.8(3) . .
C21 N3 H3A 127.1 . .
C20 N3 H3A 127.1 . .
C21 N4 C19 105.2(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O2 1.251(5) .
C1 O1 1.257(5) .
C1 C2 1.506(6) .
C2 C8 1.384(6) .
C2 C3 1.393(6) .
C3 C4 1.373(7) .
C3 H3 0.9300 .
C4 C5 1.383(7) .
C4 H4 0.9300 .
C5 C6 1.402(6) .
C5 H5 0.9300 .
C6 C8 1.380(6) .
C6 C7 1.498(6) .
C7 O4 1.257(5) .
C7 O3 1.264(5) .
C8 H8 0.9300 .
C9 N1 1.329(6) .
C9 C10 1.405(7) .
C9 H9 0.9300 .
C10 C11 1.366(7) .
C10 H10 0.9300 .
C11 C12 1.397(6) .
C11 H11 0.9300 .
C12 C13 1.417(6) .
C12 C20 1.424(6) .
C13 N1 1.344(6) .
C13 C14 1.456(5) .
C14 N2 1.368(5) .
C14 C18 1.400(6) .
C15 N2 1.320(6) .
C15 C16 1.391(7) .
C15 H15 0.9300 .
C16 C17 1.371(7) .
C16 H16 0.9300 .
C17 C18 1.409(6) .
C17 H17 0.9300 .
C18 C19 1.437(6) .
C19 C20 1.366(6) .
C19 N4 1.382(6) .
C20 N3 1.378(5) .
C21 N4 1.343(5) .
C21 N3 1.345(6) .
C21 C22 1.466(6) .
C22 C27 1.391(7) .
C22 C23 1.393(6) .
C23 C24 1.379(7) .
C23 H23 0.9300 .
C24 C25 1.378(8) .
C24 H24 0.9300 .
C25 C26 1.375(8) .
C25 H25 0.9300 .
C26 C27 1.376(7) .
C26 H26 0.9300 .
C27 H27 0.9300 .
O1 Pb1 2.419(3) .
O2 Pb1 2.649(3) .
O3 Pb1 2.636(3) 1_665
O4 Pb1 2.448(3) 1_665
Pb1 O4 2.448(3) 1_445
Pb1 N2 2.479(4) .
Pb1 N1 2.620(4) .
Pb1 O3 2.636(3) 1_445
N3 H3A 0.8600 .
