#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:52:06 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180402 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/71/7207182.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_7207182
loop_
_publ_author_name
'Li, Xian-Qiang'
'Zhang, Hua-Bin'
'Wu, Shu-Ting'
'Lin, Jian-Di'
'Lin, Ping'
'Li, Zhi-Hua'
'Du, Shao-Wu'
_publ_section_title
;
 Synthesis, structures and luminescent properties of new Pb(ii)/M(i) (M =
 K, Rb and Cs) frameworks based on dicarboxylic acids: a novel icosahedral
 Pb6-M6 SBU
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              936
_journal_paper_doi               10.1039/c1ce06111a
_journal_volume                  14
_journal_year                    2012
_chemical_formula_sum            'C80 H64 Cs6 N2 O39 Pb6'
_chemical_formula_weight         3717.99
_chemical_name_systematic
;
?
;
_space_group_IT_number           194
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c 2c'
_symmetry_space_group_name_H-M   'P 63/m m c'
_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            2
_cell_length_a                   16.231(3)
_cell_length_b                   16.231(3)
_cell_length_c                   24.466(5)
_cell_measurement_reflns_used    16790
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4816
_cell_measurement_theta_min      2.2063
_cell_volume                     5581.9(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0816
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            35165
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    11.019
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5447
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3383
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_refine_diff_density_max         3.327
_refine_diff_density_min         -2.058
_refine_diff_density_rms         0.311
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         1681
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0615
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1863P)²+126.3105P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2397
_refine_ls_wR_factor_ref         0.2407
_reflns_number_gt                1678
_reflns_number_total             1681
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce06111a.txt
_cod_data_source_block           compound_3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P63/mmc
_cod_database_code               7207182
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'-y, -x, -z+1/2'
'x-y, -y, -z'
'x, x-y, -z+1/2'
'y, x, -z'
'-x+y, y, -z+1/2'
'-x, -x+y, -z'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -z-1/2'
'y, x, z-1/2'
'-x+y, y, z'
'-x, -x+y, z-1/2'
'-y, -x, z'
'x-y, -y, z-1/2'
'x, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.29019(5) 0.14510(3) 0.02660(3) 0.0299(5) Uani 1 2 d S . .
Cs1 Cs 0.1724(7) 0.0862(3) -0.1394(7) 0.071(3) Uani 0.50 2 d SP . 1
Cs1' Cs 0.2056(7) 0.1028(4) -0.1527(7) 0.081(3) Uani 0.50 2 d SP A 2
O1 O 0.4094(7) 0.2938(7) -0.0065(4) 0.033(2) Uani 1 1 d . . .
O2 O 0.3000(7) 0.2574(7) -0.0700(5) 0.047(3) Uani 1 1 d . . .
O3 O 0.3847(11) 0.1924(5) 0.1044(6) 0.043(4) Uani 1 2 d S . .
O4 O 0.2429(12) 0.1214(6) 0.1448(6) 0.043(4) Uani 1 2 d S . .
O5 O 0.042(3) 0.084(5) -0.2500 0.050(16) Uani 0.33 4 d SPU . 1
O5' O 0.0000 0.0000 -0.2500 0.050(10) Uani 1 12 d S B 2
O6W O 0.0000 0.0000 0.0000 0.28(7) Uani 1 12 d SU . .
N1 N 0.6667 0.3333 0.0501(12) 0.036(7) Uani 1 6 d SU . .
C1 C 0.3803(10) 0.3098(11) -0.0497(6) 0.037(4) Uani 1 1 d . . .
C2 C 0.3292(15) 0.1646(8) 0.1456(8) 0.032(4) Uani 1 2 d S . .
C3 C 0.5349(7) 0.4651(7) -0.0542(8) 0.031(4) Uani 1 2 d S . .
H3A H 0.5502 0.4498 -0.0205 0.037 Uiso 1 2 calc SR . .
C4 C 0.4493(10) 0.4019(10) -0.0787(6) 0.033(3) Uani 1 1 d . . .
C5 C 0.4237(13) 0.4244(12) -0.1290(7) 0.051(4) Uani 1 1 d . . .
H5A H 0.3645 0.3841 -0.1444 0.061 Uiso 1 1 calc R . .
C6 C 0.4898(10) 0.5102(10) -0.1559(10) 0.057(7) Uani 1 2 d S . .
H6A H 0.4771 0.5229 -0.1910 0.069 Uiso 1 2 calc SR . .
C7 C 0.334(2) 0.1669(10) 0.2500 0.033(6) Uani 1 4 d S . .
H7A H 0.2677 0.1339 0.2500 0.040 Uiso 1 4 calc SR . .
C8 C 0.3809(13) 0.1904(7) 0.2015(10) 0.034(5) Uani 1 2 d S . .
C9 C 0.478(2) 0.210(2) 0.2021(12) 0.039(7) Uani 0.50 1 d PU . .
H9A H 0.5003 0.1940 0.1687 0.047 Uiso 0.50 1 calc PR . .
C10 C 0.524(3) 0.212(3) 0.2500 0.044(10) Uani 0.50 2 d SP . .
H10A H 0.5842 0.2140 0.2500 0.052 Uiso 0.50 2 d SPR . .
C11 C 0.6163(8) 0.3837(8) 0.0700(10) 0.050(6) Uani 1 2 d SU . .
H11A H 0.6161 0.3839 0.1092 0.075 Uiso 1 2 calc SR . .
H11C H 0.5520 0.3514 0.0568 0.075 Uiso 0.50 1 calc PR . .
H11B H 0.6486 0.4480 0.0568 0.075 Uiso 0.50 1 calc PR . .
C12 C 0.6667 0.3333 -0.011(3) 0.093(19) Uani 1 6 d SU . .
H12B H 0.6989 0.3011 -0.0240 0.140 Uiso 0.33 2 calc SPR . .
H12C H 0.6989 0.3977 -0.0240 0.140 Uiso 0.33 2 calc SPR . .
H12A H 0.6023 0.3011 -0.0240 0.140 Uiso 0.33 2 calc SPR . .
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'
Cs Cs -0.3680 2.1192 '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
O3 Pb1 O1 82.8(4) . 24
O3 Pb1 O1 82.8(4) . .
O1 Pb1 O1 75.7(5) 24 .
O3 Pb1 O2 129.2(3) . 24
O1 Pb1 O2 47.7(3) 24 24
O1 Pb1 O2 93.1(3) . 24
O3 Pb1 O2 129.2(3) . .
O1 Pb1 O2 93.1(3) 24 .
O1 Pb1 O2 47.7(3) . .
O2 Pb1 O2 72.7(5) 24 .
O3 Pb1 C2 24.3(6) . .
O1 Pb1 C2 101.9(4) 24 .
O1 Pb1 C2 101.9(4) . .
O2 Pb1 C2 141.4(3) 24 .
O2 Pb1 C2 141.4(3) . .
O3 Pb1 O4 47.9(5) . .
O1 Pb1 O4 119.6(3) 24 .
O1 Pb1 O4 119.6(3) . .
O2 Pb1 O4 142.6(3) 24 .
O2 Pb1 O4 142.6(3) . .
C2 Pb1 O4 23.6(5) . .
O3 Pb1 C1 105.7(4) . 24
O1 Pb1 C1 23.3(4) 24 24
O1 Pb1 C1 83.2(4) . 24
O2 Pb1 C1 24.4(3) 24 24
O2 Pb1 C1 82.1(4) . 24
C2 Pb1 C1 122.5(4) . 24
O4 Pb1 C1 135.0(3) . 24
O3 Pb1 C1 105.7(4) . .
O1 Pb1 C1 83.2(4) 24 .
O1 Pb1 C1 23.3(4) . .
O2 Pb1 C1 82.1(4) 24 .
O2 Pb1 C1 24.4(3) . .
C2 Pb1 C1 122.5(4) . .
O4 Pb1 C1 135.0(3) . .
C1 Pb1 C1 81.4(5) 24 .
O3 Pb1 O2 78.4(3) . 15
O1 Pb1 O2 70.3(3) 24 15
O1 Pb1 O2 142.8(3) . 15
O2 Pb1 O2 75.1(4) 24 15
O2 Pb1 O2 146.9(3) . 15
C2 Pb1 O2 71.5(2) . 15
O4 Pb1 O2 67.8(2) . 15
C1 Pb1 O2 71.6(3) 24 15
C1 Pb1 O2 152.7(3) . 15
O3 Pb1 O2 78.4(3) . 10
O1 Pb1 O2 142.8(3) 24 10
O1 Pb1 O2 70.3(3) . 10
O2 Pb1 O2 146.9(3) 24 10
O2 Pb1 O2 75.1(4) . 10
C2 Pb1 O2 71.5(2) . 10
O4 Pb1 O2 67.8(2) . 10
C1 Pb1 O2 152.7(3) 24 10
C1 Pb1 O2 71.6(3) . 10
O2 Pb1 O2 134.8(4) 15 10
O3 Pb1 Pb1 121.47(10) . 15
O1 Pb1 Pb1 74.2(2) 24 15
O1 Pb1 Pb1 137.8(2) . 15
O2 Pb1 Pb1 44.7(3) 24 15
O2 Pb1 Pb1 105.5(2) . 15
C2 Pb1 Pb1 112.77(19) . 15
O4 Pb1 Pb1 100.93(17) . 15
C1 Pb1 Pb1 58.3(3) 24 15
C1 Pb1 Pb1 123.4(3) . 15
O2 Pb1 Pb1 43.3(2) 15 15
O2 Pb1 Pb1 142.74(19) 10 15
O2 Cs1 O2 70.4(6) . 24
O2 Cs1 O4 136.3(6) . 8
O2 Cs1 O4 66.7(4) 24 8
O2 Cs1 O4 66.7(4) . 10
O2 Cs1 O4 136.3(6) 24 10
O4 Cs1 O4 152.3(6) 8 10
O2 Cs1 O5 126.1(12) . 1
O2 Cs1 O5 159.0(8) 24 1
O4 Cs1 O5 97.5(13) 8 1
O4 Cs1 O5 63.3(11) 10 1
C1 O1 Pb1 107.7(9) . .
C1 O2 Pb1 79.5(9) . .
C1 O2 Pb1 114.8(10) . 17
Pb1 O2 Pb1 92.0(3) . 17
C1 O2 Cs1 148.3(11) . .
Pb1 O2 Cs1 94.7(4) . .
Pb1 O2 Cs1 96.4(3) 17 .
C2 O3 Pb1 107.3(13) . .
C2 O4 Pb1 78.0(12) . .
C12 N1 C11 109.0(15) . 5_665
C12 N1 C11 109.0(15) . 3_655
C11 N1 C11 109.9(14) 5_665 3_655
C12 N1 C11 109.0(15) . .
C11 N1 C11 109.9(14) 5_665 .
C11 N1 C11 109.9(14) 3_655 .
O1 C1 O2 125.1(14) . .
O1 C1 C4 115.8(13) . .
O2 C1 C4 119.1(14) . .
O1 C1 Pb1 49.0(7) . .
O2 C1 Pb1 76.2(9) . .
C4 C1 Pb1 164.7(10) . .
O4 C2 O3 126.8(19) . .
O4 C2 C8 118.9(17) . .
O3 C2 C8 114.3(18) . .
O4 C2 Pb1 78.4(11) . .
O3 C2 Pb1 48.4(10) . .
C8 C2 Pb1 162.7(14) . .
C4 C3 C4 121(2) . 22_665
C4 C3 H3A 119.3 . .
C4 C3 H3A 119.3 22_665 .
C3 C4 C5 120.3(15) . .
C3 C4 C1 119.9(14) . .
C5 C4 C1 119.8(13) . .
C4 C5 C6 118.9(16) . .
C4 C5 H5A 120.6 . .
C6 C5 H5A 120.6 . .
C5 C6 C5 120(2) 22_665 .
C5 C6 H6A 120.1 22_665 .
C5 C6 H6A 120.1 . .
C8 C7 C8 122(3) 16_556 .
C8 C7 H7A 119.1 16_556 .
C8 C7 H7A 119.1 . .
C7 C8 C9 117(2) . 24
C7 C8 C9 117(2) . .
C9 C8 C9 38(2) 24 .
C7 C8 C2 122.9(18) . .
C9 C8 C2 117(2) 24 .
C9 C8 C2 117(2) . .
C9 C9 C10 104(2) 24 .
C9 C9 C8 70.8(12) 24 .
C10 C9 C8 122(3) . .
C9 C9 C10 46.3(14) 24 9
C10 C9 C10 58(3) . 9
C8 C9 C10 96(2) . 9
C9 C9 H9A 116.5 24 .
C10 C9 H9A 116.5 . .
C8 C9 H9A 116.5 . .
C10 C9 H9A 136.0 9 .
C9 C10 C9 116(4) . 16_556
C9 C10 C10 76(2) . 9
C9 C10 C10 76(2) 16_556 9
C9 C10 C9 102(3) . 9
C9 C10 C9 30(2) 16_556 9
C10 C10 C9 46.3(14) 9 9
C9 C10 C9 30(2) . 24
C9 C10 C9 102(3) 16_556 24
C10 C10 C9 46.3(14) 9 24
C9 C10 C9 78(3) 9 24
C9 C10 H10A 122.1 . .
C9 C10 H10A 122.1 16_556 .
C10 C10 H10A 118.7 9 .
C9 C10 H10A 129.9 9 .
C9 C10 H10A 129.9 24 .
N1 C11 H11A 109.5 . .
N1 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
N1 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
H11C C11 H11B 109.5 . .
N1 C12 H12B 109.5 . .
N1 C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
N1 C12 H12A 109.5 . .
H12B C12 H12A 109.5 . .
H12C C12 H12A 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O3 2.320(14) .
Pb1 O1 2.357(9) 24
Pb1 O1 2.357(9) .
Pb1 O2 2.939(12) 24
Pb1 O2 2.939(12) .
Pb1 C2 2.96(2) .
Pb1 O4 2.967(15) .
Pb1 C1 2.976(16) 24
Pb1 C1 2.976(16) .
Pb1 O2 3.012(13) 15
Pb1 O2 3.012(13) 10
Pb1 Pb1 4.2817(11) 15
Cs1 O2 3.023(15) .
Cs1 O2 3.023(15) 24
Cs1 O4 3.045(12) 8
Cs1 O4 3.045(12) 10
Cs1 O5 3.424(14) 1
O1 C1 1.235(19) .
O2 C1 1.249(18) .
O2 Pb1 3.012(13) 17
O3 C2 1.28(3) .
O4 C2 1.21(3) .
O5 O5 0.00(17) 1
N1 C12 1.49(7) .
N1 C11 1.50(2) 5_665
N1 C11 1.50(2) 3_655
N1 C11 1.50(2) .
C1 C4 1.52(2) .
C2 C8 1.55(3) .
C3 C4 1.384(18) .
C3 C4 1.384(18) 22_665
C3 H3A 0.9300 .
C4 C5 1.40(2) .
C5 C6 1.42(2) .
C5 H5A 0.9300 .
C6 C5 1.42(2) 22_665
C6 H6A 0.9300 .
C7 C8 1.36(3) 16_556
C7 C8 1.36(3) .
C7 H7A 0.9300 .
C8 C9 1.44(3) 24
C8 C9 1.44(3) .
C9 C9 0.95(6) 24
C9 C10 1.38(4) .
C9 C10 1.86(5) 9
C9 H9A 0.9800 .
C10 C9 1.38(4) 16_556
C10 C10 1.61(9) 9
C10 C9 1.86(5) 9
C10 C9 1.86(5) 24
C10 H10A 0.9599 .
C11 H11A 0.9600 .
C11 H11C 0.9600 .
C11 H11B 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C12 H12A 0.9600 .
