#------------------------------------------------------------------------------
#$Date: 2016-11-08 21:49:06 +0200 (Tue, 08 Nov 2016) $
#$Revision: 188161 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/06/7040657.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_7040657
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            'C30 H19 N18 O1.5 Pb2.5'
_chemical_formula_weight         1173.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-08-26 deposited with the CCDC.
2016-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 128.268(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   37.7785(11)
_cell_length_b                   7.4676(2)
_cell_length_c                   29.5720(7)
_cell_measurement_reflns_used    6456
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.3860
_cell_measurement_theta_min      4.6800
_cell_volume                     6550.0(4)
_computing_cell_refinement       'SMART (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP-II (Johnson, 1976)'
_computing_publication_material  SHELXL-97
_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 1.000
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0778
_diffrn_reflns_av_sigmaI/netI    0.0758
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23455
_diffrn_reflns_theta_full        67.23
_diffrn_reflns_theta_max         67.23
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    25.133
_exptl_absorpt_correction_T_max  0.2721
_exptl_absorpt_correction_T_min  0.2384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4336
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.631
_refine_diff_density_min         -1.680
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         5852
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0332P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0981
_reflns_number_gt                4406
_reflns_number_total             5852
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt02986h2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7040657--7040658.cif.'
_cod_original_cell_volume        6550.0(3)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C30 H19 N18 O1.50 Pb2.50'
_cod_database_code               7040657
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
Pb1 Pb 0.629277(14) 0.74138(5) 0.812415(18) 0.02997(12) Uani 1 1 d .
Pb2 Pb 0.531161(14) 0.72691(5) 0.645203(18) 0.03122(12) Uani 1 1 d .
Pb3 Pb 0.5000 0.97235(8) 0.7500 0.03300(16) Uani 1 2 d S
N1 N 0.5983(3) 0.7465(11) 0.8670(4) 0.035(2) Uani 1 1 d .
N2 N 0.5578(3) 0.8020(12) 0.8480(4) 0.038(2) Uani 1 1 d .
N3 N 0.5520(3) 0.7562(13) 0.8860(4) 0.044(2) Uani 1 1 d .
N4 N 0.5884(3) 0.6769(14) 0.9315(4) 0.049(3) Uani 1 1 d .
N5 N 0.6862(3) 0.6022(11) 0.9374(4) 0.035(2) Uani 1 1 d .
N6 N 0.5812(3) 0.1670(12) 0.8070(4) 0.040(2) Uani 1 1 d .
N7 N 0.5805(3) 0.3416(12) 0.8133(4) 0.040(2) Uani 1 1 d .
N8 N 0.6107(3) 0.4190(10) 0.8083(3) 0.030(2) Uani 1 1 d .
N9 N 0.6118(3) 0.1266(12) 0.7988(4) 0.038(2) Uani 1 1 d .
N10 N 0.6848(3) 0.4652(12) 0.8107(4) 0.037(2) Uani 1 1 d .
N11 N 0.5280(3) 1.0491(11) 0.6503(3) 0.032(2) Uani 1 1 d .
N12 N 0.5158(3) 1.1524(13) 0.6759(4) 0.042(2) Uani 1 1 d .
N13 N 0.5240(4) 1.3230(13) 0.6727(4) 0.050(3) Uani 1 1 d .
N14 N 0.5422(3) 1.3310(12) 0.6448(4) 0.047(3) Uani 1 1 d .
N15 N 0.5485(3) 0.9340(11) 0.5812(4) 0.035(2) Uani 1 1 d .
N16 N 0.6133(3) 0.7475(13) 0.7091(4) 0.050(3) Uani 1 1 d .
N17 N 0.6298(3) 0.6576(15) 0.6931(4) 0.046(3) Uani 1 1 d .
N18 N 0.6458(4) 0.5660(16) 0.6778(5) 0.069(4) Uani 1 1 d .
O1 O 0.5501(2) 0.7603(8) 0.7369(3) 0.0296(16) Uani 1 1 d .
O2 O 0.5000 0.5298(13) 0.7500 0.043(3) Uani 1 2 d S
H2C H 0.5255 0.4862 0.7774 0.052 Uiso 0.50 1 d PR
H2D H 0.4909 0.5972 0.7641 0.052 Uiso 0.50 1 d PR
C1 C 0.6171(4) 0.6709(13) 0.9186(5) 0.032(2) Uani 1 1 d .
C2 C 0.6619(4) 0.5950(13) 0.9558(4) 0.035(3) Uani 1 1 d .
C3 C 0.6789(4) 0.5229(16) 1.0102(5) 0.047(3) Uani 1 1 d .
H3 H 0.6609 0.5209 1.0216 0.056 Uiso 1 1 calc R
C4 C 0.7209(4) 0.4576(17) 1.0452(5) 0.054(3) Uani 1 1 d .
H4 H 0.7317 0.4073 1.0804 0.065 Uiso 1 1 calc R
C5 C 0.7491(4) 0.4654(15) 1.0285(5) 0.045(3) Uani 1 1 d .
C6 C 0.7298(4) 0.5409(14) 0.9728(4) 0.039(3) Uani 1 1 d .
C7 C 0.7562(4) 0.5526(15) 0.9546(5) 0.044(3) Uani 1 1 d .
H7 H 0.7439 0.6014 0.9187 0.053 Uiso 1 1 calc R
C8 C 0.7994(4) 0.4941(17) 0.9884(6) 0.059(4) Uani 1 1 d .
H8 H 0.8167 0.5027 0.9759 0.071 Uiso 1 1 calc R
C9 C 0.8179(5) 0.4198(17) 1.0429(6) 0.069(4) Uani 1 1 d .
H9 H 0.8475 0.3783 1.0659 0.083 Uiso 1 1 calc R
C10 C 0.7937(4) 0.4077(18) 1.0624(5) 0.059(4) Uani 1 1 d .
H10 H 0.8070 0.3603 1.0988 0.070 Uiso 1 1 calc R
C11 C 0.6291(3) 0.2835(13) 0.7989(4) 0.031(2) Uani 1 1 d .
C12 C 0.6666(4) 0.3083(15) 0.7968(4) 0.036(3) Uani 1 1 d .
C13 C 0.6818(4) 0.1557(16) 0.7846(5) 0.048(3) Uani 1 1 d .
H13 H 0.6662 0.0476 0.7725 0.057 Uiso 1 1 calc R
C14 C 0.7205(5) 0.1787(18) 0.7919(6) 0.060(4) Uani 1 1 d .
H14 H 0.7328 0.0815 0.7863 0.072 Uiso 1 1 calc R
C15 C 0.7430(4) 0.344(2) 0.8078(5) 0.053(4) Uani 1 1 d .
C16 C 0.7224(4) 0.4891(17) 0.8143(5) 0.045(3) Uani 1 1 d .
C17 C 0.7435(4) 0.6559(18) 0.8282(5) 0.054(3) Uani 1 1 d .
H17 H 0.7300 0.7536 0.8316 0.065 Uiso 1 1 calc R
C18 C 0.7832(4) 0.681(2) 0.8371(6) 0.075(5) Uani 1 1 d .
H18 H 0.7961 0.7943 0.8467 0.090 Uiso 1 1 calc R
C19 C 0.8045(5) 0.543(3) 0.8323(7) 0.096(7) Uani 1 1 d .
H19 H 0.8316 0.5605 0.8386 0.115 Uiso 1 1 calc R
C20 C 0.7846(5) 0.376(3) 0.8179(7) 0.081(5) Uani 1 1 d .
H20 H 0.7988 0.2813 0.8147 0.097 Uiso 1 1 calc R
C21 C 0.5431(4) 1.1616(14) 0.6315(5) 0.034(3) Uani 1 1 d .
C22 C 0.5567(4) 1.1031(15) 0.5968(5) 0.038(3) Uani 1 1 d .
C23 C 0.5762(4) 1.2215(15) 0.5812(5) 0.049(3) Uani 1 1 d .
H23 H 0.5826 1.3389 0.5946 0.059 Uiso 1 1 calc R
C24 C 0.5855(4) 1.1631(17) 0.5465(6) 0.056(4) Uani 1 1 d .
H24 H 0.5983 1.2407 0.5357 0.068 Uiso 1 1 calc R
C25 C 0.5759(4) 0.9845(17) 0.5264(5) 0.045(3) Uani 1 1 d .
C26 C 0.5579(4) 0.8698(16) 0.5462(5) 0.040(3) Uani 1 1 d .
C27 C 0.5481(4) 0.6962(16) 0.5274(5) 0.050(3) Uani 1 1 d .
H27 H 0.5359 0.6215 0.5397 0.060 Uiso 1 1 calc R
C28 C 0.5558(4) 0.6288(18) 0.4907(5) 0.055(4) Uani 1 1 d .
H28 H 0.5487 0.5108 0.4781 0.066 Uiso 1 1 calc R
C29 C 0.5749(5) 0.743(2) 0.4727(6) 0.065(4) Uani 1 1 d .
H29 H 0.5812 0.6975 0.4492 0.078 Uiso 1 1 calc R
C30 C 0.5841(4) 0.916(2) 0.4887(5) 0.059(4) Uani 1 1 d .
H30 H 0.5957 0.9892 0.4753 0.071 Uiso 1 1 calc R
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'
N N 0.0311 0.0180 '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'
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
O1 Pb1 N8 81.9(2) . .
O1 Pb1 N1 77.7(2) . .
N8 Pb1 N1 79.5(3) . .
O1 Pb1 N16 70.7(3) . .
N8 Pb1 N16 95.8(3) . .
N1 Pb1 N16 148.4(3) . .
O1 Pb2 N11 79.3(2) . .
O1 Pb2 N16 76.5(3) . .
N11 Pb2 N16 88.7(3) . .
O1 Pb2 N3 81.0(3) . 2_656
N11 Pb2 N3 81.2(3) . 2_656
N16 Pb2 N3 156.7(3) . 2_656
N2 Pb3 N2 122.3(4) 2_656 .
N2 Pb3 O1 74.6(2) 2_656 .
N2 Pb3 O1 72.2(2) . .
N2 Pb3 O1 72.2(2) 2_656 2_656
N2 Pb3 O1 74.6(2) . 2_656
O1 Pb3 O1 107.4(3) . 2_656
N2 N1 C1 105.9(8) . .
N2 N1 Pb1 127.2(6) . .
C1 N1 Pb1 126.3(7) . .
N3 N2 N1 108.3(9) . .
N3 N2 Pb3 126.9(7) . .
N1 N2 Pb3 124.7(6) . .
N2 N3 N4 111.3(9) . .
N2 N3 Pb2 120.5(7) . 2_656
N4 N3 Pb2 124.9(7) . 2_656
N3 N4 C1 103.8(9) . .
C2 N5 C6 118.9(9) . .
N7 N6 N9 110.0(8) . .
N6 N7 N8 108.0(8) . .
C11 N8 N7 106.0(8) . .
C11 N8 Pb1 124.7(7) . .
N7 N8 Pb1 129.2(6) . .
C11 N9 N6 105.9(8) . .
C12 N10 C16 117.9(10) . .
C21 N11 N12 105.2(9) . .
C21 N11 Pb2 123.8(7) . .
N12 N11 Pb2 130.7(7) . .
N13 N12 N11 109.4(8) . .
N12 N13 N14 108.2(8) . .
C21 N14 N13 104.6(9) . .
C22 N15 C26 119.0(10) . .
N17 N16 Pb2 112.4(8) . .
N17 N16 Pb1 128.9(8) . .
Pb2 N16 Pb1 99.2(3) . .
N18 N17 N16 178.4(13) . .
Pb2 O1 Pb1 112.6(2) . .
Pb2 O1 Pb3 119.5(2) . .
Pb1 O1 Pb3 119.3(2) . .
N1 C1 N4 110.6(10) . .
N1 C1 C2 125.3(9) . .
N4 C1 C2 124.2(10) . .
N5 C2 C3 122.5(10) . .
N5 C2 C1 116.9(9) . .
C3 C2 C1 120.6(10) . .
C4 C3 C2 120.2(11) . .
C3 C4 C5 119.9(11) . .
C10 C5 C4 124.7(12) . .
C10 C5 C6 118.3(11) . .
C4 C5 C6 117.0(11) . .
N5 C6 C7 119.5(10) . .
N5 C6 C5 121.4(10) . .
C7 C6 C5 119.1(10) . .
C8 C7 C6 121.2(11) . .
C7 C8 C9 119.2(12) . .
C10 C9 C8 121.6(13) . .
C9 C10 C5 120.6(13) . .
N9 C11 N8 110.0(9) . .
N9 C11 C12 126.3(10) . .
N8 C11 C12 123.2(9) . .
N10 C12 C13 126.0(11) . .
N10 C12 C11 116.1(9) . .
C13 C12 C11 117.6(11) . .
C14 C13 C12 115.2(12) . .
C13 C14 C15 122.4(12) . .
C14 C15 C16 116.7(11) . .
C14 C15 C20 125.2(14) . .
C16 C15 C20 118.0(14) . .
N10 C16 C17 121.0(11) . .
N10 C16 C15 121.4(12) . .
C17 C16 C15 117.5(11) . .
C18 C17 C16 122.4(14) . .
C17 C18 C19 121.5(16) . .
C20 C19 C18 117.9(15) . .
C19 C20 C15 122.5(15) . .
N11 C21 N14 112.6(9) . .
N11 C21 C22 122.4(9) . .
N14 C21 C22 124.9(10) . .
N15 C22 C23 123.4(10) . .
N15 C22 C21 114.9(10) . .
C23 C22 C21 121.7(10) . .
C24 C23 C22 119.0(12) . .
C23 C24 C25 120.3(11) . .
C24 C25 C26 117.3(11) . .
C24 C25 C30 123.0(12) . .
C26 C25 C30 119.6(12) . .
C27 C26 N15 120.3(11) . .
C27 C26 C25 118.8(11) . .
N15 C26 C25 120.8(11) . .
C26 C27 C28 121.9(12) . .
C27 C28 C29 118.6(13) . .
C30 C29 C28 122.0(12) . .
C29 C30 C25 119.1(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O1 2.383(7) .
Pb1 N8 2.489(8) .
Pb1 N1 2.515(8) .
Pb1 N16 2.722(10) .
Pb2 O1 2.350(6) .
Pb2 N11 2.418(8) .
Pb2 N16 2.440(10) .
Pb2 N3 2.679(9) 2_656
Pb3 N2 2.636(9) 2_656
Pb3 N2 2.636(9) .
Pb3 O1 2.674(6) .
Pb3 O1 2.674(6) 2_656
N1 N2 1.326(11) .
N1 C1 1.344(12) .
N2 N3 1.317(11) .
N3 N4 1.326(12) .
N3 Pb2 2.679(9) 2_656
N4 C1 1.354(12) .
N5 C2 1.329(12) .
N5 C6 1.370(12) .
N6 N7 1.320(11) .
N6 N9 1.353(11) .
N7 N8 1.368(10) .
N8 C11 1.350(11) .
N9 C11 1.342(12) .
N10 C12 1.291(13) .
N10 C16 1.369(12) .
N11 C21 1.318(12) .
N11 N12 1.348(10) .
N12 N13 1.328(13) .
N13 N14 1.367(11) .
N14 C21 1.331(13) .
N15 C22 1.314(13) .
N15 C26 1.374(12) .
N16 N17 1.197(12) .
N17 N18 1.172(12) .
C1 C2 1.444(14) .
C2 C3 1.417(13) .
C3 C4 1.339(15) .
C4 C5 1.424(15) .
C5 C10 1.393(15) .
C5 C6 1.442(14) .
C6 C7 1.401(13) .
C7 C8 1.352(15) .
C8 C9 1.413(17) .
C9 C10 1.354(16) .
C11 C12 1.465(13) .
C12 C13 1.419(14) .
C13 C14 1.349(16) .
C14 C15 1.407(17) .
C15 C16 1.411(15) .
C15 C20 1.426(17) .
C16 C17 1.396(16) .
C17 C18 1.364(15) .
C18 C19 1.37(2) .
C19 C20 1.37(2) .
C21 C22 1.469(13) .
C22 C23 1.398(14) .
C23 C24 1.348(15) .
C24 C25 1.413(16) .
C25 C26 1.424(15) .
C25 C30 1.427(14) .
C26 C27 1.368(15) .
C27 C28 1.382(14) .
C28 C29 1.416(17) .
C29 C30 1.339(17) .
