#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:05:51 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179556 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/25/4502594.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_4502594
loop_
_publ_author_name
'Wang, Xiu-Li'
'Chen, Yong-Qiang'
'Gao, Qiang'
'Lin, Hong-Yan'
'Liu, Guo-Cheng'
'Zhang, Jin-Xia'
'Tian, Ai-Xiang'
_publ_section_title
;
 Coordination Behavior of 5,6-Substituted 1,10-Phenanthroline Derivatives
 and Structural Diversities by Coligands in the Construction of Lead(II)
 Complexes
;
_journal_issue                   5
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              2174
_journal_paper_doi               10.1021/cg901431r
_journal_volume                  10
_journal_year                    2010
_chemical_formula_sum            'C32 H19 N5 O4 Pb'
_chemical_formula_weight         744.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           152
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   15.0313(15)
_cell_length_b                   15.0313(15)
_cell_length_c                   20.896(2)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      1.84
_cell_volume                     4088.7(7)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0895
_diffrn_reflns_av_sigmaI/netI    0.0885
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20964
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    6.238
_exptl_absorpt_correction_T_max  0.287
_exptl_absorpt_correction_T_min  0.158
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.021(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         4832
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0431
_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)+(0.0230P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0742
_reflns_number_gt                3446
_reflns_number_total             4832
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg901431r_si_002.cif
_cod_data_source_block           compound8
_cod_database_code               4502594
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'y, x, -z'
'-x, -x+y, -z+1/3'
'x-y, -y, -z+2/3'
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
Pb1 Pb 0.08472(3) 1.34924(2) 0.247005(17) 0.04954(12) Uani 1 1 d .
O1 O 0.0407(6) 1.3369(5) 0.3672(3) 0.084(2) Uani 1 1 d .
O2 O 0.2006(6) 1.4473(5) 0.3370(3) 0.070(2) Uani 1 1 d .
O3 O 0.2217(5) 1.7504(5) 0.8426(3) 0.070(2) Uani 1 1 d .
O4 O 0.3020(5) 1.8969(6) 0.7902(3) 0.072(2) Uani 1 1 d .
N1 N 0.1834(8) 1.2372(7) 0.2450(4) 0.060(2) Uani 1 1 d .
N2 N -0.0268(7) 1.1292(6) 0.2487(3) 0.055(2) Uani 1 1 d .
N3 N -0.0074(7) 0.8145(6) 0.2531(4) 0.049(2) Uani 1 1 d .
N4 N 0.1628(7) 0.8988(7) 0.2515(4) 0.055(2) Uani 1 1 d .
H4A H 0.2249 0.9103 0.2507 0.066 Uiso 1 1 d R
C1 C 0.2841(11) 1.2903(10) 0.2436(6) 0.076(4) Uani 1 1 d .
H1A H 0.3166 1.3617 0.2431 0.092 Uiso 1 1 calc R
C2 C 0.3452(11) 1.2422(12) 0.2429(6) 0.085(4) Uani 1 1 d .
H2A H 0.4164 1.2815 0.2400 0.103 Uiso 1 1 calc R
C3 C 0.2992(11) 1.1401(11) 0.2465(5) 0.075(4) Uani 1 1 d .
H3A H 0.3389 1.1086 0.2471 0.090 Uiso 1 1 calc R
C4 C 0.1939(11) 1.0808(9) 0.2492(5) 0.059(3) Uani 1 1 d .
C5 C 0.1307(9) 0.9691(9) 0.2502(4) 0.053(3) Uani 1 1 d .
C6 C 0.0296(9) 0.9197(8) 0.2508(4) 0.057(3) Uani 1 1 d .
C7 C -0.0330(10) 0.9661(8) 0.2510(5) 0.046(3) Uani 1 1 d .
C8 C -0.1407(10) 0.9146(7) 0.2524(5) 0.061(3) Uani 1 1 d .
H8A H -0.1784 0.8432 0.2528 0.074 Uiso 1 1 calc R
C9 C -0.1885(10) 0.9696(9) 0.2530(5) 0.070(4) Uani 1 1 d .
H9A H -0.2598 0.9376 0.2542 0.084 Uiso 1 1 calc R
C10 C -0.1287(10) 1.0751(9) 0.2519(5) 0.064(3) Uani 1 1 d .
H10A H -0.1630 1.1121 0.2535 0.076 Uiso 1 1 calc R
C11 C 0.0236(9) 1.0768(8) 0.2485(4) 0.049(3) Uani 1 1 d .
C12 C 0.1327(9) 1.1314(8) 0.2487(4) 0.047(3) Uani 1 1 d .
C13 C 0.0775(13) 0.8119(9) 0.2532(4) 0.077(4) Uani 1 1 d .
C14 C 0.0744(9) 0.7085(9) 0.2566(5) 0.061(3) Uiso 1 1 d .
C15 C -0.0147(10) 0.6203(9) 0.2550(5) 0.077(4) Uiso 1 1 d .
H15A H -0.0763 0.6206 0.2535 0.093 Uiso 1 1 calc R
H16A H -0.0770 0.4670 0.2544 0.093 Uiso 1 1 d R
H17A H 0.2201 0.6098 0.2667 0.093 Uiso 1 1 d R
C18 C 0.1621(10) 0.7052(9) 0.2576(5) 0.078(4) Uiso 1 1 d .
H18A H 0.2250 0.7658 0.2557 0.094 Uiso 1 1 calc R
C20 C 0.1272(10) 1.4161(8) 0.3765(5) 0.064(3) Uani 1 1 d .
C21 C 0.1408(8) 1.4769(8) 0.4353(4) 0.057(2) Uani 1 1 d .
C22 C 0.0661(8) 1.4449(9) 0.4813(5) 0.085(4) Uani 1 1 d .
H22A H 0.0042 1.3844 0.4748 0.102 Uiso 1 1 calc R
C23 C 0.0795(8) 1.4991(9) 0.5368(5) 0.079(4) Uani 1 1 d .
H23A H 0.0264 1.4755 0.5666 0.095 Uiso 1 1 calc R
C24 C 0.1715(8) 1.5888(7) 0.5491(5) 0.054(3) Uani 1 1 d .
C25 C 0.2471(8) 1.6237(7) 0.5014(4) 0.061(3) Uani 1 1 d .
H25A H 0.3083 1.6852 0.5073 0.073 Uiso 1 1 calc R
C26 C 0.2322(8) 1.5687(8) 0.4463(5) 0.066(3) Uani 1 1 d .
H26A H 0.2839 1.5929 0.4156 0.079 Uiso 1 1 calc R
C27 C 0.1909(8) 1.6448(8) 0.6101(5) 0.056(3) Uani 1 1 d .
C28 C 0.2457(8) 1.7492(8) 0.6134(5) 0.065(3) Uiso 1 1 d .
H28A H 0.2695 1.7871 0.5759 0.078 Uiso 1 1 calc R
C29 C 0.2669(8) 1.8002(8) 0.6717(5) 0.068(3) Uani 1 1 d .
H29A H 0.3039 1.8716 0.6726 0.082 Uiso 1 1 calc R
C30 C 0.2329(7) 1.7452(8) 0.7291(5) 0.050(3) Uani 1 1 d .
C31 C 0.2544(7) 1.8011(9) 0.7931(5) 0.049(3) Uani 1 1 d .
C32 C 0.1762(8) 1.6404(9) 0.7259(5) 0.069(3) Uani 1 1 d .
H32A H 0.1520 1.6025 0.7634 0.083 Uiso 1 1 calc R
C33 C 0.1536(8) 1.5887(9) 0.6664(5) 0.074(3) Uiso 1 1 d .
H33A H 0.1139 1.5175 0.6649 0.088 Uiso 1 1 calc R
N5 N 0.0700(8) 0.5223(7) 0.2587(4) 0.073(3) Uiso 1 1 d .
C16 C -0.0145(9) 0.5277(9) 0.2557(6) 0.073(4) Uiso 1 1 d .
C17 C 0.1590(9) 0.6107(9) 0.2615(5) 0.074(4) Uiso 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 Pb1 O1 52.0(2) . .
O2 Pb1 O4 135.6(2) . 4_366
O1 Pb1 O4 93.7(2) . 4_366
O2 Pb1 O3 83.0(2) . 2_784
O1 Pb1 O3 134.9(2) . 2_784
O4 Pb1 O3 121.1(2) 4_366 2_784
O2 Pb1 O4 127.6(2) . 2_784
O1 Pb1 O4 160.2(2) . 2_784
O4 Pb1 O4 74.5(2) 4_366 2_784
O3 Pb1 O4 48.5(2) 2_784 2_784
O2 Pb1 N5 74.6(2) . 1_565
O1 Pb1 N5 80.9(2) . 1_565
O4 Pb1 N5 72.5(3) 4_366 1_565
O3 Pb1 N5 83.4(2) 2_784 1_565
O4 Pb1 N5 80.4(2) 2_784 1_565
O2 Pb1 N1 86.7(2) . .
O1 Pb1 N1 99.7(2) . .
O4 Pb1 N1 131.2(3) 4_366 .
O3 Pb1 N1 79.2(2) 2_784 .
O4 Pb1 N1 100.1(2) 2_784 .
N5 Pb1 N1 155.8(3) 1_565 .
O2 Pb1 C20 26.4(2) . .
O1 Pb1 C20 26.4(2) . .
O4 Pb1 C20 113.1(3) 4_366 .
O3 Pb1 C20 108.5(3) 2_784 .
O4 Pb1 C20 146.5(2) 2_784 .
N5 Pb1 C20 71.9(3) 1_565 .
N1 Pb1 C20 97.8(3) . .
C20 O1 Pb1 88.7(6) . .
C20 O2 Pb1 92.9(7) . .
C31 O3 Pb1 93.2(6) . 3_475
C31 O4 Pb1 159.0(7) . 4_476
C31 O4 Pb1 92.4(6) . 3_475
Pb1 O4 Pb1 97.4(2) 4_476 3_475
C1 N1 C12 120.5(10) . .
C1 N1 Pb1 116.1(8) . .
C12 N1 Pb1 123.3(7) . .
C10 N2 C11 117.3(8) . .
C13 N3 C6 101.3(9) . .
C13 N4 C5 103.0(9) . .
C13 N4 H4A 129.2 . .
C5 N4 H4A 127.8 . .
N1 C1 C2 122.1(12) . .
N1 C1 H1A 119.0 . .
C2 C1 H1A 119.0 . .
C3 C2 C1 119.3(13) . .
C3 C2 H2A 120.4 . .
C1 C2 H2A 120.4 . .
C2 C3 C4 121.0(12) . .
C2 C3 H3A 119.5 . .
C4 C3 H3A 119.5 . .
C3 C4 C12 118.9(11) . .
C3 C4 C5 128.5(11) . .
C12 C4 C5 112.6(11) . .
C6 C5 N4 108.6(11) . .
C6 C5 C4 123.6(11) . .
N4 C5 C4 127.8(11) . .
C5 C6 N3 109.5(11) . .
C5 C6 C7 125.6(12) . .
N3 C6 C7 124.8(11) . .
C8 C7 C6 126.3(10) . .
C8 C7 C11 119.4(9) . .
C6 C7 C11 114.3(11) . .
C9 C8 C7 119.0(9) . .
C9 C8 H8A 120.5 . .
C7 C8 H8A 120.5 . .
C8 C9 C10 117.9(12) . .
C8 C9 H9A 121.1 . .
C10 C9 H9A 121.1 . .
N2 C10 C9 126.5(10) . .
N2 C10 H10A 116.7 . .
C9 C10 H10A 116.7 . .
N2 C11 C12 119.3(9) . .
N2 C11 C7 119.8(10) . .
C12 C11 C7 120.8(9) . .
N1 C12 C11 118.6(9) . .
N1 C12 C4 118.2(11) . .
C11 C12 C4 123.1(10) . .
N4 C13 N3 117.6(11) . .
N4 C13 C14 122.4(13) . .
N3 C13 C14 120.0(12) . .
C15 C14 C18 118.7(12) . .
C15 C14 C13 120.8(12) . .
C18 C14 C13 120.4(12) . .
C14 C15 C16 119.4(13) . .
C14 C15 H15A 120.3 . .
C16 C15 H15A 120.3 . .
C14 C18 C17 120.2(12) . .
C14 C18 H18A 119.9 . .
C17 C18 H18A 119.9 . .
O1 C20 O2 123.0(10) . .
O1 C20 C21 117.9(11) . .
O2 C20 C21 119.0(10) . .
O1 C20 Pb1 65.0(5) . .
O2 C20 Pb1 60.7(6) . .
C21 C20 Pb1 160.5(7) . .
C22 C21 C26 117.4(9) . .
C22 C21 C20 121.9(10) . .
C26 C21 C20 120.7(10) . .
C21 C22 C23 122.2(10) . .
C21 C22 H22A 118.9 . .
C23 C22 H22A 118.9 . .
C22 C23 C24 120.8(10) . .
C22 C23 H23A 119.6 . .
C24 C23 H23A 119.6 . .
C23 C24 C25 117.3(9) . .
C23 C24 C27 122.0(9) . .
C25 C24 C27 120.6(9) . .
C26 C25 C24 121.0(9) . .
C26 C25 H25A 119.5 . .
C24 C25 H25A 119.5 . .
C25 C26 C21 121.2(9) . .
C25 C26 H26A 119.4 . .
C21 C26 H26A 119.4 . .
C28 C27 C33 118.9(10) . .
C28 C27 C24 122.4(10) . .
C33 C27 C24 118.7(10) . .
C27 C28 C29 121.4(11) . .
C27 C28 H28A 119.3 . .
C29 C28 H28A 119.3 . .
C28 C29 C30 120.7(10) . .
C28 C29 H29A 119.7 . .
C30 C29 H29A 119.7 . .
C32 C30 C29 118.1(10) . .
C32 C30 C31 121.0(10) . .
C29 C30 C31 120.8(10) . .
O3 C31 O4 125.2(10) . .
O3 C31 C30 119.1(10) . .
O4 C31 C30 115.6(10) . .
C30 C32 C33 121.1(11) . .
C30 C32 H32A 119.5 . .
C33 C32 H32A 119.5 . .
C27 C33 C32 119.8(11) . .
C27 C33 H33A 120.1 . .
C32 C33 H33A 120.1 . .
C16 N5 C17 117.3(11) . .
C16 N5 Pb1 126.6(8) . 1_545
C17 N5 Pb1 115.7(8) . 1_545
N5 C16 C15 123.1(12) . .
N5 C16 H16A 118.3 . .
C15 C16 H16A 118.5 . .
N5 C17 C18 121.0(12) . .
N5 C17 H17A 119.7 . .
C18 C17 H17A 119.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O2 2.486(7) .
Pb1 O1 2.580(6) .
Pb1 O4 2.660(8) 4_366
Pb1 O3 2.677(7) 2_784
Pb1 O4 2.685(7) 2_784
Pb1 N5 2.730(9) 1_565
Pb1 N1 2.746(8) .
Pb1 C20 2.847(11) .
O1 C20 1.264(11) .
O2 C20 1.266(12) .
O3 C31 1.232(11) .
O3 Pb1 2.677(6) 3_475
O4 C31 1.249(11) .
O4 Pb1 2.660(8) 4_476
O4 Pb1 2.685(7) 3_475
N1 C1 1.311(14) .
N1 C12 1.379(12) .
N2 C10 1.329(12) .
N2 C11 1.338(12) .
N3 C13 1.295(15) .
N3 C6 1.389(12) .
N4 C13 1.295(14) .
N4 C5 1.365(12) .
N4 H4A 0.8601 .
C1 C2 1.426(16) .
C1 H1A 0.9300 .
C2 C3 1.332(15) .
C2 H2A 0.9300 .
C3 C4 1.377(14) .
C3 H3A 0.9300 .
C4 C12 1.457(14) .
C4 C5 1.458(14) .
C5 C6 1.316(13) .
C6 C7 1.425(14) .
C7 C8 1.402(14) .
C7 C11 1.442(13) .
C8 C9 1.340(13) .
C8 H8A 0.9300 .
C9 C10 1.377(14) .
C9 H9A 0.9300 .
C10 H10A 0.9300 .
C11 C12 1.420(14) .
C13 C14 1.534(15) .
C14 C15 1.333(14) .
C14 C18 1.343(14) .
C15 C16 1.393(15) .
C15 H15A 0.9300 .
C18 C17 1.400(15) .
C18 H18A 0.9300 .
C20 C21 1.483(13) .
C21 C22 1.370(12) .
C21 C26 1.396(12) .
C22 C23 1.373(13) .
C22 H22A 0.9300 .
C23 C24 1.390(12) .
C23 H23A 0.9300 .
C24 C25 1.401(12) .
C24 C27 1.473(12) .
C25 C26 1.370(12) .
C25 H25A 0.9300 .
C26 H26A 0.9300 .
C27 C28 1.361(12) .
C27 C33 1.391(13) .
C28 C29 1.389(13) .
C28 H28A 0.9300 .
C29 C30 1.400(13) .
C29 H29A 0.9300 .
C30 C32 1.368(13) .
C30 C31 1.525(13) .
C32 C33 1.415(14) .
C32 H32A 0.9300 .
C33 H33A 0.9300 .
N5 C16 1.315(14) .
N5 C17 1.336(13) .
N5 Pb1 2.730(9) 1_545
C16 H16A 0.9265 .
C17 H17A 0.9318 .
