#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:21:30 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179574 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/39/4503959.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_4503959
loop_
_publ_author_name
'Zhao, Ya-Hui'
'Xu, Hong-Bin'
'Shao, Kui-Zhan'
'Xing, Yan'
'Su, Zhong-Min'
'Ma, Jian-Fang'
_publ_section_title
;
 Syntheses, Characterization, and Luminescent Properties of Three 3D
 Lead−Organic Frameworks with 1D Channels
;
_journal_issue                   3
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              513
_journal_paper_doi               10.1021/cg060535p
_journal_volume                  7
_journal_year                    2007
_chemical_formula_moiety         'C24 H16 N4 O17 Pb4, 8(O0.62), 0.25(O4)'
_chemical_formula_sum            'C24 H16 N4 O23 Pb4'
_chemical_formula_weight         1557.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           137
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4ac 2a'
_symmetry_space_group_name_H-M   'P 42/n m c :2'
_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                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.749(4)
_cell_length_b                   17.749(4)
_cell_length_c                   6.895(2)
_cell_measurement_temperature    293(2)
_cell_volume                     2172.1(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0725
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            12625
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.19
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    15.536
_exptl_absorpt_correction_T_max  0.1181
_exptl_absorpt_correction_T_min  0.0667
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.806
_refine_diff_density_min         -1.294
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         1428
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          5.159
_refine_ls_shift/su_mean         0.090
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0588P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1062
_reflns_number_gt                888
_reflns_number_total             1428
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg060535psi20060810_011505.cif
_cod_data_source_block           3
_cod_original_cell_volume        2171.9(10)
_cod_original_sg_symbol_H-M      P42/nmc
_cod_database_code               4503959
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z+1/2'
'y, -x+1/2, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y, -z'
'y+1/2, x+1/2, -z+1/2'
'-y, -x, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z-1/2'
'-y, x-1/2, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y, z'
'-y-1/2, -x-1/2, z-1/2'
'y, x, z-1/2'
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 0.4794(7) 0.6126(11) 0.7789(17) 0.107(4) Uani 1 1 d .
H1 H 0.4915 0.6631 0.7978 0.24(12) Uiso 1 1 calc R
C2 C 0.5336(8) 0.5615(8) 0.7809(17) 0.109(4) Uani 1 1 d .
H2 H 0.5832 0.5759 0.8025 2.0(13) Uiso 1 1 calc R
C3 C 0.5155(6) 0.4845(6) 0.7500 0.108(7) Uani 1 2 d S
C4 C 0.5734(7) 0.4266(7) 0.7500 0.108(6) Uani 1 2 d S
N1 N 0.4072(5) 0.5928(5) 0.7500 0.107(5) Uani 1 2 d S
O1 O 0.3549(3) 0.6451(3) 0.7500 0.103(4) Uani 1 2 d S
O2 O 0.7500 0.3274(4) 0.5992(10) 0.0469(17) Uani 1 2 d S
O3 O 0.6375(5) 0.4399(8) 0.7750(18) 0.183(6) Uani 1 1 d .
Pb1 Pb 0.7500 0.36050(2) 0.93301(6) 0.04827(19) Uani 1 2 d S
O3W O 0.2500 0.7500 0.7500 0.67(8) Uani 1 8 d S
O5 O 0.7500 0.4364(11) 0.472(3) 0.031(9) Uani 0.25(2) 2 d SP
O4 O 0.7500 0.549(3) 0.684(11) 0.98(9) Uani 1.24(7) 2 d SP
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 121.1(18) . .
N1 C1 H1 119.5 . .
C2 C1 H1 119.5 . .
C1 C2 C3 119.7(16) . .
C1 C2 H2 120.2 . .
C3 C2 H2 120.2 . .
C2 C3 C2 117.2(16) . 8_666
C2 C3 C4 121.4(8) . .
C2 C3 C4 121.4(8) 8_666 .
O3 C4 O3 114(2) . 8_666
O3 C4 C3 122.8(11) . .
O3 C4 C3 122.8(11) 8_666 .
O1 N1 C1 119.3(10) . .
O1 N1 C1 119.3(10) . 8_666
C1 N1 C1 121(2) . 8_666
Pb1 O2 Pb1 103.3(2) . 12_657
Pb1 O2 Pb1 103.3(2) . 11_667
Pb1 O2 Pb1 109.3(3) 12_657 11_667
C4 O3 Pb1 132.6(12) . .
O2 Pb1 O2 73.1(3) . 12_657
O2 Pb1 O2 73.1(3) . 11_667
O2 Pb1 O2 69.7(3) 12_657 11_667
O2 Pb1 O3 74.7(3) . 14_755
O2 Pb1 O3 144.9(3) 12_657 14_755
O2 Pb1 O3 88.0(3) 11_667 14_755
O2 Pb1 O3 74.7(3) . .
O2 Pb1 O3 88.0(3) 12_657 .
O2 Pb1 O3 144.9(3) 11_667 .
O3 Pb1 O3 96.5(6) 14_755 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.344(14) .
C1 C2 1.322(18) .
C1 H1 0.9300 .
C2 C3 1.421(14) .
C2 H2 0.9300 .
C3 C2 1.421(15) 8_666
C3 C4 1.45(2) .
C4 O3 1.174(10) .
C4 O3 1.174(10) 8_666
N1 O1 1.312(14) .
N1 C1 1.344(14) 8_666
O2 Pb1 2.375(7) .
O2 Pb1 2.405(4) 12_657
O2 Pb1 2.405(4) 11_667
O3 Pb1 2.676(10) .
Pb1 O2 2.405(4) 12_657
Pb1 O2 2.405(4) 11_667
Pb1 O3 2.676(10) 14_755
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N1 C1 C2 C3 0.7(16) . .
C1 C2 C3 C2 -0.3(8) . 8_666
C1 C2 C3 C4 179.7(8) . .
C2 C3 C4 O3 -0.1(9) . .
C2 C3 C4 O3 179.9(9) 8_666 .
C2 C3 C4 O3 179.9(9) . 8_666
C2 C3 C4 O3 -0.1(9) 8_666 8_666
C2 C1 N1 O1 179.6(8) . .
C2 C1 N1 C1 -0.4(8) . 8_666
O3 C4 O3 Pb1 -30.5(8) 8_666 .
C3 C4 O3 Pb1 149.5(8) . .
Pb1 O2 Pb1 O2 20.3(3) 12_657 12_657
Pb1 O2 Pb1 O2 -93.62(10) 11_667 12_657
Pb1 O2 Pb1 O2 93.62(10) 12_657 11_667
Pb1 O2 Pb1 O2 -20.3(3) 11_667 11_667
Pb1 O2 Pb1 O3 -173.7(4) 12_657 14_755
Pb1 O2 Pb1 O3 72.4(4) 11_667 14_755
Pb1 O2 Pb1 O3 -72.4(4) 12_657 .
Pb1 O2 Pb1 O3 173.7(4) 11_667 .
C4 O3 Pb1 O2 88.9(13) . .
C4 O3 Pb1 O2 15.9(12) . 12_657
C4 O3 Pb1 O2 65.1(14) . 11_667
C4 O3 Pb1 O3 161.0(10) . 14_755
