#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:52:06 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180402 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/71/7207180.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_7207180
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 K6 N2 O39 Pb6'
_chemical_formula_weight         3155.13
_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                   15.8708(6)
_cell_length_b                   15.8708(6)
_cell_length_c                   24.2726(16)
_cell_measurement_reflns_used    5073
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4797
_cell_measurement_theta_min      2.2386
_cell_volume                     5294.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type
;
Mercury2 (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  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0132
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            34219
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    9.820
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6444
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.979
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2951
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_refine_diff_density_max         2.225
_refine_diff_density_min         -1.590
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         1874
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0366
_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)+(0.0624P)²+45.5334P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1102
_refine_ls_wR_factor_ref         0.1115
_reflns_number_gt                1809
_reflns_number_total             1874
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce06111a.txt
_cod_data_source_block           compound_1
_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               7207180
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
Pb1 Pb -0.28067(2) -0.140335(12) 0.475857(14) 0.02920(17) Uani 1 2 d S
K1 K -0.1770(2) -0.08851(11) 0.63826(13) 0.0629(8) Uani 1 2 d S
O1 O -0.4040(3) -0.2919(3) 0.50769(19) 0.0354(10) Uani 1 1 d .
O2 O -0.2958(4) -0.2517(4) 0.5751(2) 0.0453(13) Uani 1 1 d .
O3 O -0.3712(5) -0.1856(2) 0.3962(3) 0.0358(15) Uani 1 2 d S
O4 O -0.2234(5) -0.1117(2) 0.3560(3) 0.0371(15) Uani 1 2 d S
O5 O 0.0000 0.0000 0.7068(12) 0.112(7) Uani 1 6 d SU
O6W O 0.0000 0.0000 0.530(2) 0.109(17) Uani 0.50 6 d SPU
N1 N -0.6667 -0.3333 0.4499(6) 0.032(3) Uani 1 6 d S
C1 C -0.3763(5) -0.3073(5) 0.5540(3) 0.0340(15) Uani 1 1 d .
C2 C -0.3138(8) -0.1569(4) 0.3546(4) 0.0303(19) Uani 1 2 d S
C3 C -0.5341(3) -0.4659(3) 0.5580(4) 0.030(2) Uani 1 2 d S
H3 H -0.5485 -0.4515 0.5233 0.037 Uiso 1 2 calc SR
C4 C -0.4472(5) -0.3998(5) 0.5831(3) 0.0320(14) Uani 1 1 d .
C5 C -0.4263(6) -0.4230(6) 0.6350(3) 0.0453(19) Uani 1 1 d .
H5 H -0.3686 -0.3797 0.6526 0.054 Uiso 1 1 calc R
C6 C -0.4906(5) -0.5094(5) 0.6602(4) 0.053(3) Uani 1 2 d S
H6 H -0.4754 -0.5246 0.6944 0.064 Uiso 1 2 calc SR
C7 C -0.3125(11) -0.1562(5) 0.2500 0.032(3) Uani 1 4 d S
H7 H -0.2448 -0.1224 0.2500 0.038 Uiso 1 4 calc SR
C8 C -0.3659(7) -0.1830(3) 0.3000(4) 0.032(2) Uani 1 2 d S
C9 C -0.4653(9) -0.2327(4) 0.2990(5) 0.108(8) Uani 1 2 d SU
H9 H -0.5000 -0.2500 0.3319 0.129 Uiso 1 2 calc SR
C10 C -0.5139(16) -0.2570(8) 0.2500 0.19(2) Uani 1 4 d SU
H10 H -0.5816 -0.2908 0.2500 0.225 Uiso 1 4 calc SR
C11 C -0.6667 -0.3333 0.5113(8) 0.063(6) Uani 1 6 d S
H11A H -0.6996 -0.3992 0.5245 0.094 Uiso 0.33 2 calc SPR
H11B H -0.6996 -0.3004 0.5245 0.094 Uiso 0.33 2 calc SPR
H11C H -0.6008 -0.3004 0.5245 0.094 Uiso 0.33 2 calc SPR
C12 C -0.6149(4) -0.2298(7) 0.4300(4) 0.046(3) Uani 1 2 d S
H12A H -0.6147 -0.2290 0.3904 0.069 Uiso 1 2 calc SR
H12B H -0.5491 -0.1972 0.4433 0.069 Uiso 0.50 1 calc PR
H12C H -0.6478 -0.1971 0.4435 0.069 Uiso 0.50 1 calc PR
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'
K K 0.2009 0.2494 '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 83.45(17) . 24
O3 Pb1 O1 83.45(17) . .
O1 Pb1 O1 74.9(2) 24 .
O3 Pb1 O2 130.84(14) . 24
O1 Pb1 O2 48.33(15) 24 24
O1 Pb1 O2 91.14(17) . 24
O3 Pb1 O2 130.84(14) . .
O1 Pb1 O2 91.14(17) 24 .
O1 Pb1 O2 48.33(15) . .
O2 Pb1 O2 68.5(2) 24 .
O3 Pb1 C2 24.0(3) . .
O1 Pb1 C2 102.41(19) 24 .
O1 Pb1 C2 102.4(2) . .
O2 Pb1 C2 143.40(12) 24 .
O2 Pb1 C2 143.40(12) . .
O3 Pb1 C1 107.25(18) . 24
O1 Pb1 C1 24.10(17) 24 24
O1 Pb1 C1 81.81(18) . 24
O2 Pb1 C1 24.24(16) 24 24
O2 Pb1 C1 78.57(17) . 24
C2 Pb1 C1 124.14(18) . 24
O3 Pb1 C1 107.25(18) . .
O1 Pb1 C1 81.81(18) 24 .
O1 Pb1 C1 24.10(17) . .
O2 Pb1 C1 78.57(17) 24 .
O2 Pb1 C1 24.24(16) . .
C2 Pb1 C1 124.14(19) . .
C1 Pb1 C1 78.6(2) 24 .
O3 Pb1 O2 74.02(12) . 15_556
O1 Pb1 O2 71.60(15) 24 15_556
O1 Pb1 O2 141.24(15) . 15_556
O2 Pb1 O2 80.92(17) 24 15_556
O2 Pb1 O2 148.96(12) . 15_556
C2 Pb1 O2 67.19(11) . 15_556
C1 Pb1 O2 75.54(15) 24 15_556
C1 Pb1 O2 153.14(16) . 15_556
O3 Pb1 O2 74.02(12) . 10_556
O1 Pb1 O2 141.24(15) 24 10_556
O1 Pb1 O2 71.60(15) . 10_556
O2 Pb1 O2 148.96(12) 24 10_556
O2 Pb1 O2 80.92(16) . 10_556
C2 Pb1 O2 67.19(11) . 10_556
C1 Pb1 O2 153.14(16) 24 10_556
C1 Pb1 O2 75.54(15) . 10_556
O2 Pb1 O2 128.58(19) 15_556 10_556
O3 Pb1 O4 47.9(2) . .
O1 Pb1 O4 120.43(15) 24 .
O1 Pb1 O4 120.43(15) . .
O2 Pb1 O4 144.42(12) 24 .
O2 Pb1 O4 144.42(12) . .
C2 Pb1 O4 23.9(2) . .
C1 Pb1 O4 136.80(14) 24 .
C1 Pb1 O4 136.80(14) . .
O2 Pb1 O4 64.32(9) 15_556 .
O2 Pb1 O4 64.32(9) 10_556 .
O3 Pb1 Pb1 120.22(5) . 15_556
O1 Pb1 Pb1 75.30(12) 24 15_556
O1 Pb1 Pb1 138.91(12) . 15_556
O2 Pb1 Pb1 47.79(11) 24 15_556
O2 Pb1 Pb1 105.15(10) . 15_556
C2 Pb1 Pb1 111.13(9) . 15_556
C1 Pb1 Pb1 60.05(13) 24 15_556
C1 Pb1 Pb1 123.42(13) . 15_556
O2 Pb1 Pb1 46.35(10) 15_556 15_556
O2 Pb1 Pb1 143.41(9) 10_556 15_556
O4 Pb1 Pb1 98.96(7) . 15_556
O2 K1 O2 72.7(2) . 24
O2 K1 O4 140.85(19) . 8_556
O2 K1 O4 69.78(17) 24 8_556
O2 K1 O4 69.78(17) . 10_556
O2 K1 O4 140.85(19) 24 10_556
O4 K1 O4 142.3(2) 8_556 10_556
O2 K1 O5 142.76(15) . 1
O2 K1 O5 142.76(16) 24 1
O4 K1 O5 73.04(14) 8_556 1
O4 K1 O5 73.04(14) 10_556 1
C1 O1 Pb1 107.2(4) . .
C1 O2 K1 150.0(5) . .
C1 O2 Pb1 80.5(4) . .
K1 O2 Pb1 94.52(16) . .
C1 O2 Pb1 110.8(4) . 17_556
K1 O2 Pb1 98.26(16) . 17_556
Pb1 O2 Pb1 85.86(14) . 17_556
C2 O3 Pb1 109.3(6) . .
C2 O4 Pb1 76.4(5) . .
C11 N1 C12 108.8(7) . 3_455
C11 N1 C12 108.8(7) . .
C12 N1 C12 110.1(6) 3_455 .
C11 N1 C12 108.8(7) . 5_445
C12 N1 C12 110.1(6) 3_455 5_445
C12 N1 C12 110.1(6) . 5_445
O2 C1 O1 123.9(6) . .
O2 C1 C4 120.1(6) . .
O1 C1 C4 116.0(6) . .
O2 C1 Pb1 75.2(4) . .
O1 C1 Pb1 48.7(3) . .
C4 C1 Pb1 164.6(5) . .
O4 C2 O3 126.4(8) . .
O4 C2 C8 120.0(8) . .
O3 C2 C8 113.7(8) . .
O4 C2 Pb1 79.6(5) . .
O3 C2 Pb1 46.8(4) . .
C8 C2 Pb1 160.4(7) . .
C4 C3 C4 122.1(9) . 22_445
C4 C3 H3 119.0 . .
C4 C3 H3 119.0 22_445 .
C3 C4 C5 118.2(7) . .
C3 C4 C1 120.5(6) . .
C5 C4 C1 121.2(6) . .
C6 C5 C4 120.5(7) . .
C6 C5 H5 119.8 . .
C4 C5 H5 119.8 . .
C5 C6 C5 120.5(10) . 22_445
C5 C6 H6 119.7 . .
C5 C6 H6 119.7 22_445 .
C8 C7 C8 117.6(13) 16_556 .
C8 C7 H7 121.2 16_556 .
C8 C7 H7 121.2 . .
C9 C8 C7 120.2(10) . .
C9 C8 C2 119.4(10) . .
C7 C8 C2 120.4(9) . .
C10 C9 C8 120.4(13) . .
C10 C9 H9 119.8 . .
C8 C9 H9 119.8 . .
C9 C10 C9 121.3(19) . 16_556
C9 C10 H10 119.3 . .
C9 C10 H10 119.3 16_556 .
N1 C11 H11A 109.5 . .
N1 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
N1 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
N1 C12 H12A 109.5 . .
N1 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
N1 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 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 2.299(7) .
Pb1 O1 2.347(5) 24
Pb1 O1 2.347(5) .
Pb1 O2 2.925(5) 24
Pb1 O2 2.925(5) .
Pb1 C2 2.978(9) .
Pb1 C1 2.984(7) 24
Pb1 C1 2.984(7) .
Pb1 O2 2.994(6) 15_556
Pb1 O2 2.994(6) 10_556
Pb1 O4 3.014(6) .
Pb1 Pb1 4.0318(4) 15_556
K1 O2 2.780(5) .
K1 O2 2.780(5) 24
K1 O4 2.810(5) 8_556
K1 O4 2.810(5) 10_556
K1 O5 2.948(17) 1
O1 C1 1.275(8) .
O2 C1 1.242(8) .
O2 Pb1 2.994(6) 17_556
O3 C2 1.282(11) .
O4 C2 1.243(12) .
O5 O5 0.00(6) 1
O6W O6W 1.45(9) 13_556
N1 C11 1.49(2) .
N1 C12 1.503(11) 3_455
N1 C12 1.503(11) .
N1 C12 1.503(11) 5_445
C1 C4 1.506(9) .
C2 C8 1.507(13) .
C3 C4 1.388(8) .
C3 C4 1.388(8) 22_445
C3 H3 0.9300 .
C4 C5 1.397(9) .
C5 C6 1.377(9) .
C5 H5 0.9300 .
C6 C5 1.377(9) 22_445
C6 H6 0.9300 .
C7 C8 1.418(12) 16_556
C7 C8 1.418(12) .
C7 H7 0.9300 .
C8 C9 1.366(14) .
C9 C10 1.364(17) .
C9 H9 0.9300 .
C10 C9 1.364(17) 16_556
C10 H10 0.9300 .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
