#------------------------------------------------------------------------------
#$Date: 2016-11-08 21:49:06 +0200 (Tue, 08 Nov 2016) $
#$Revision: 188161 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/06/7040658.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_7040658
loop_
_publ_author_name
'Xiang, Jing'
'Shen, Chang'
'Cheng, Shun-Cheung'
'Yu, Fei'
'Chu, Wing-Kin'
'Feng, Hua'
'Yiu, Shek-Man'
'Ko, Chi-Chiu'
'Leung, Chi-Fai'
_publ_section_title
;
 Luminescence behaviour of Pb(2+)-based cage-containing and
 channel-containing porous coordination polymers.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16134
_journal_page_last               16138
_journal_paper_doi               10.1039/c6dt02986h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C26 H18 N17.89 O2 Pb2'
_chemical_formula_weight         1027.41
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2016-09-09 deposited with the CCDC.
2016-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   33.2975(17)
_cell_length_b                   33.2975(17)
_cell_length_c                   9.6334(5)
_cell_measurement_reflns_used    3157
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      62.0070
_cell_measurement_theta_min      4.5970
_cell_volume                     9249.8(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1729
_diffrn_reflns_av_unetI/netI     0.1194
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            19919
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.672
_diffrn_reflns_theta_min         2.654
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.392
_exptl_absorpt_correction_T_max  0.3983
_exptl_absorpt_correction_T_min  0.3588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_description       block
_exptl_crystal_F_000             4313
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_refine_diff_density_max         2.975
_refine_diff_density_min         -2.100
_refine_diff_density_rms         0.274
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         4022
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.1402
_refine_ls_R_factor_gt           0.0834
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1160P)²+533.3143P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2108
_refine_ls_wR_factor_ref         0.2604
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2386
_reflns_number_total             4022
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt02986h2.cif
_cod_data_source_block           r-3_sq
_cod_depositor_comments
'Adding full bibliography for 7040657--7040658.cif.'
_cod_original_cell_volume        9249.9(11)
_cod_database_code               7040658
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.372
_shelx_estimated_absorpt_t_max   0.412
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pb1 Pb 0.59858(2) 0.61885(3) 0.33369(9) 0.0555(3) Uani 1 1 d . . .
N1 N 0.5216(6) 0.5462(5) 0.227(2) 0.067(5) Uani 0.9444 1 d . . P
N2 N 0.5703(5) 0.5353(6) 0.4422(19) 0.062(4) Uani 1 1 d . . .
N3 N 0.6430(5) 0.6149(5) 0.5495(17) 0.054(4) Uani 1 1 d . . .
N4 N 0.6750(5) 0.6443(5) 0.635(2) 0.061(4) Uani 1 1 d . . .
N5 N 0.6825(6) 0.6203(5) 0.732(2) 0.062(4) Uani 1 1 d . . .
N6 N 0.6566(6) 0.5755(6) 0.712(2) 0.065(5) Uani 1 1 d . . .
N7 N 0.6407(6) 0.5902(6) 0.206(2) 0.068(5) Uani 1 1 d . . .
N8 N 0.6313(6) 0.5506(7) 0.202(2) 0.067(5) Uani 1 1 d . . .
N9 N 0.6243(9) 0.5126(7) 0.201(3) 0.110(9) Uani 1 1 d . . .
C1 C 0.4964(8) 0.5522(8) 0.130(3) 0.079(7) Uani 1 1 d . . .
H1 H 0.5052 0.5821 0.1002 0.095 Uiso 1 1 calc R U .
C2 C 0.4569(8) 0.5146(9) 0.071(3) 0.087(8) Uani 1 1 d . . .
H2 H 0.4393 0.5200 0.0066 0.104 Uiso 1 1 calc R U .
C3 C 0.4442(8) 0.4709(10) 0.106(3) 0.089(8) Uani 1 1 d . . .
H3 H 0.4191 0.4463 0.0624 0.107 Uiso 1 1 calc R U .
C4 C 0.4694(7) 0.4621(8) 0.212(2) 0.077(7) Uani 1 1 d . . .
C5 C 0.5081(7) 0.5022(7) 0.271(3) 0.073(7) Uani 1 1 d . . .
C6 C 0.4576(8) 0.4178(8) 0.259(3) 0.095(9) Uani 1 1 d . . .
H6 H 0.4317 0.3919 0.2226 0.114 Uiso 1 1 calc R U .
C7 C 0.4849(7) 0.4123(6) 0.360(3) 0.082(8) Uani 1 1 d . . .
H7 H 0.4778 0.3826 0.3872 0.098 Uiso 1 1 calc R U .
C8 C 0.5236(7) 0.4518(7) 0.423(3) 0.071(6) Uani 1 1 d . . .
C9 C 0.5350(6) 0.4965(6) 0.381(3) 0.068(6) Uani 1 1 d . . .
C10 C 0.5962(7) 0.5293(7) 0.534(3) 0.069(6) Uani 1 1 d . . .
C11 C 0.5872(8) 0.4859(8) 0.584(3) 0.076(6) Uani 1 1 d . . .
H11 H 0.6053 0.4834 0.6532 0.091 Uiso 1 1 calc R U .
C12 C 0.5499(9) 0.4468(8) 0.525(3) 0.082(7) Uani 1 1 d . . .
H12 H 0.5428 0.4173 0.5538 0.098 Uiso 1 1 calc R U .
C13 C 0.6318(6) 0.5721(7) 0.594(2) 0.060(5) Uani 1 1 d . . .
O1 O 0.5187(12) 0.6552(11) 0.265(4) 0.221(17) Uani 1 1 d . . .
H1C H 0.5397 0.6626 0.2041 0.266 Uiso 1 1 d R U .
H1D H 0.5310 0.6712 0.3376 0.266 Uiso 1 1 d R U .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0192 0.0096 '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'
Pb Pb -4.0816 8.6988 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0330 0.0189 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0517 0.0336 '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_3
N7 Pb1 N3 86.0(6) .
N7 Pb1 N2 75.9(5) .
N3 Pb1 N2 62.9(5) .
N7 Pb1 N1 85.9(6) .
N3 Pb1 N1 124.8(6) .
N2 Pb1 N1 62.1(6) .
N7 Pb1 N5 74.3(5) 6_564
N3 Pb1 N5 146.8(5) 6_564
N2 Pb1 N5 133.5(5) 6_564
N1 Pb1 N5 80.9(6) 6_564
C1 N1 C5 119(2) .
C1 N1 Pb1 121.2(14) .
C5 N1 Pb1 119.9(16) .
C10 N2 C9 117.8(18) .
C10 N2 Pb1 120.3(13) .
C9 N2 Pb1 120.2(14) .
N4 N3 C13 106.4(16) .
N4 N3 Pb1 137.3(12) .
C13 N3 Pb1 116.3(12) .
N3 N4 N5 108.5(14) .
N6 N5 N4 111.6(17) .
N6 N5 Pb1 114.9(13) 8_655
N4 N5 Pb1 128.8(12) 8_655
N5 N6 C13 103.7(17) .
N8 N7 Pb1 125.1(14) .
N9 N8 N7 177(2) .
N1 C1 C2 122(2) .
N1 C1 H1 119.1 .
C2 C1 H1 119.1 .
C3 C2 C1 121(3) .
C3 C2 H2 119.6 .
C1 C2 H2 119.6 .
C2 C3 C4 120(2) .
C2 C3 H3 120.0 .
C4 C3 H3 120.0 .
C6 C4 C5 120(3) .
C6 C4 C3 124(2) .
C5 C4 C3 116(2) .
N1 C5 C4 123(3) .
N1 C5 C9 118.0(19) .
C4 C5 C9 119(2) .
C4 C6 C7 120(2) .
C4 C6 H6 120.0 .
C7 C6 H6 120.0 .
C6 C7 C8 121(2) .
C6 C7 H7 119.5 .
C8 C7 H7 119.5 .
C12 C8 C9 119(2) .
C12 C8 C7 121(2) .
C9 C8 C7 120(2) .
N2 C9 C8 122(2) .
N2 C9 C5 118.9(18) .
C8 C9 C5 119(2) .
N2 C10 C11 124(2) .
N2 C10 C13 113(2) .
C11 C10 C13 122(2) .
C12 C11 C10 117(2) .
C12 C11 H11 121.6 .
C10 C11 H11 121.6 .
C8 C12 C11 120(2) .
C8 C12 H12 119.9 .
C11 C12 H12 119.9 .
N3 C13 N6 109.8(17) .
N3 C13 C10 125(2) .
N6 C13 C10 124.9(19) .
H1C O1 H1D 108.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 N7 2.392(19) .
Pb1 N3 2.591(16) .
Pb1 N2 2.665(16) .
Pb1 N1 2.699(18) .
Pb1 N5 2.768(19) 6_564
N1 C1 1.34(3) .
N1 C5 1.37(3) .
N2 C10 1.32(3) .
N2 C9 1.37(3) .
N3 N4 1.31(2) .
N3 C13 1.35(2) .
N4 N5 1.33(2) .
N5 N6 1.31(2) .
N5 Pb1 2.768(19) 8_655
N6 C13 1.38(3) .
N7 N8 1.20(2) .
N8 N9 1.16(3) .
C1 C2 1.40(3) .
C1 H1 0.9300 .
C2 C3 1.34(4) .
C2 H2 0.9300 .
C3 C4 1.44(4) .
C3 H3 0.9300 .
C4 C6 1.40(4) .
C4 C5 1.43(3) .
C5 C9 1.46(3) .
C6 C7 1.41(4) .
C6 H6 0.9300 .
C7 C8 1.43(3) .
C7 H7 0.9300 .
C8 C12 1.38(3) .
C8 C9 1.40(3) .
C10 C11 1.41(3) .
C10 C13 1.44(3) .
C11 C12 1.40(3) .
C11 H11 0.9300 .
C12 H12 0.9300 .
O1 H1C 0.8501 .
O1 H1D 0.8499 .
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
C13 N3 N4 N5 -2(2) . .
Pb1 N3 N4 N5 177.5(13) . .
N3 N4 N5 N6 1(2) . .
N3 N4 N5 Pb1 -153.3(12) . 8_655
N4 N5 N6 C13 0(2) . .
Pb1 N5 N6 C13 158.5(12) 8_655 .
C5 N1 C1 C2 -1(4) . .
Pb1 N1 C1 C2 178.5(17) . .
N1 C1 C2 C3 -3(4) . .
C1 C2 C3 C4 4(4) . .
C2 C3 C4 C6 178(2) . .
C2 C3 C4 C5 -1(3) . .
C1 N1 C5 C4 3(3) . .
Pb1 N1 C5 C4 -176.0(15) . .
C1 N1 C5 C9 -178(2) . .
Pb1 N1 C5 C9 3(2) . .
C6 C4 C5 N1 179(2) . .
C3 C4 C5 N1 -2(3) . .
C6 C4 C5 C9 -1(3) . .
C3 C4 C5 C9 179(2) . .
C5 C4 C6 C7 -2(4) . .
C3 C4 C6 C7 178(2) . .
C4 C6 C7 C8 3(4) . .
C6 C7 C8 C12 179(2) . .
C6 C7 C8 C9 -1(4) . .
C10 N2 C9 C8 6(3) . .
Pb1 N2 C9 C8 170.9(15) . .
C10 N2 C9 C5 -175.3(19) . .
Pb1 N2 C9 C5 -10(2) . .
C12 C8 C9 N2 -3(3) . .
C7 C8 C9 N2 177(2) . .
C12 C8 C9 C5 178(2) . .
C7 C8 C9 C5 -2(3) . .
N1 C5 C9 N2 5(3) . .
C4 C5 C9 N2 -176.2(18) . .
N1 C5 C9 C8 -176.5(19) . .
C4 C5 C9 C8 3(3) . .
C9 N2 C10 C11 -6(3) . .
Pb1 N2 C10 C11 -171.5(16) . .
C9 N2 C10 C13 -179.1(18) . .
Pb1 N2 C10 C13 16(2) . .
N2 C10 C11 C12 4(3) . .
C13 C10 C11 C12 176(2) . .
C9 C8 C12 C11 0(4) . .
C7 C8 C12 C11 -180(2) . .
C10 C11 C12 C8 0(4) . .
N4 N3 C13 N6 2(2) . .
Pb1 N3 C13 N6 -177.4(12) . .
N4 N3 C13 C10 176.7(19) . .
Pb1 N3 C13 C10 -3(3) . .
N5 N6 C13 N3 -2(2) . .
N5 N6 C13 C10 -176.1(18) . .
N2 C10 C13 N3 -9(3) . .
C11 C10 C13 N3 178(2) . .
N2 C10 C13 N6 165.0(19) . .
C11 C10 C13 N6 -8(3) . .
