#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:52:06 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180402 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/71/7207181.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_7207181
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 N2 O39 Pb6 Rb6'
_chemical_formula_weight         3433.35
_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                   16.03340(10)
_cell_length_b                   16.03340(10)
_cell_length_c                   24.3028(10)
_cell_measurement_reflns_used    15965
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4816
_cell_measurement_theta_min      2.2063
_cell_volume                     5410.5(2)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0782
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            33913
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    12.060
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4480
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.107
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3167
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_refine_diff_density_max         2.459
_refine_diff_density_min         -1.287
_refine_diff_density_rms         0.232
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1615
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0476
_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)+(0.0955P)²+65.3576P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1536
_refine_ls_wR_factor_ref         0.1543
_reflns_number_gt                1609
_reflns_number_total             1615
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce06111a.txt
_cod_data_source_block           compound_2
_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               7207181
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 0.28491(4) 0.142453(18) 0.02547(2) 0.0295(3) Uani 1 2 d S
Rb1 Rb 0.17889(14) 0.08945(7) -0.13822(9) 0.0630(6) Uani 1 2 d S
O1 O 0.4067(5) 0.1139(5) -0.0063(3) 0.0372(16) Uani 1 1 d .
O2 O 0.2980(5) 0.0437(6) -0.0725(3) 0.0460(19) Uani 1 1 d .
O3 O 0.3766(7) 0.1883(3) 0.1039(4) 0.039(2) Uani 1 2 d S
O4 O 0.2322(7) 0.1161(4) 0.1441(4) 0.039(2) Uani 1 2 d S
O5 O 0.0000 0.0000 -0.2073(13) 0.083(7) Uani 1 6 d S
O6W O 0.0000 0.0000 0.0000 0.15(2) Uani 1 12 d SU
N1 N 0.6667 0.3333 0.0530(12) 0.079(9) Uani 1 6 d S
C1 C 0.3786(7) 0.0701(7) -0.0513(4) 0.034(2) Uani 1 1 d .
C2 C 0.3214(11) 0.1607(6) 0.1459(6) 0.032(3) Uani 1 2 d S
C3 C 0.5347(5) 0.0694(10) -0.0564(6) 0.028(3) Uani 1 2 d S
H3A H 0.5499 0.0997 -0.0223 0.034 Uiso 1 2 calc SR
C4 C 0.4483(8) 0.0478(8) -0.0808(4) 0.038(2) Uani 1 1 d .
C5 C 0.4267(9) 0.0033(10) -0.1325(5) 0.050(3) Uani 1 1 d .
H5A H 0.3694 -0.0117 -0.1502 0.060 Uiso 1 1 calc R
C6 C 0.4912(8) -0.0176(16) -0.1567(7) 0.063(5) Uani 1 2 d S
H6A H 0.4763 -0.0474 -0.1910 0.076 Uiso 1 2 calc SR
C7 C 0.3234(15) 0.1617(7) 0.2500 0.031(4) Uani 1 4 d S
H7A H 0.2564 0.1282 0.2500 0.037 Uiso 1 4 calc SR
C8 C 0.3721(11) 0.1860(5) 0.2001(6) 0.045(4) Uani 1 2 d SU
C9 C 0.4700(13) 0.2350(6) 0.2020(8) 0.070(4) Uani 1 2 d SU
H9A H 0.5070 0.2783 0.1726 0.084 Uiso 0.50 1 d PR
C10 C 0.518(2) 0.220(3) 0.2500 0.058(7) Uani 0.50 2 d SPU
H10A H 0.5731 0.2112 0.2500 0.069 Uiso 0.50 2 d SPR
C11 C 0.6667 0.3333 -0.0136(14) 0.087(13) Uani 1 6 d S
H11A H 0.6993 0.3007 -0.0267 0.131 Uiso 0.33 2 calc SPR
H11B H 0.6993 0.3985 -0.0267 0.131 Uiso 0.33 2 calc SPR
H11C H 0.6015 0.3007 -0.0267 0.131 Uiso 0.33 2 calc SPR
C12 C 0.6152(8) 0.3848(8) 0.0703(8) 0.082(7) Uani 1 2 d S
H12A H 0.6135 0.3870 0.1097 0.123 Uiso 1 2 calc SR
H12B H 0.5506 0.3514 0.0562 0.123 Uiso 0.50 1 calc PR
H12C H 0.6483 0.4493 0.0560 0.123 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'
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'
Rb Rb -0.9393 2.9676 '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 82.7(3) . 24
O3 Pb1 O1 82.7(3) . .
O1 Pb1 O1 75.3(4) 24 .
O3 Pb1 O2 129.9(2) . 24
O1 Pb1 O2 48.3(2) 24 24
O1 Pb1 O2 92.3(2) . 24
O3 Pb1 O2 129.9(2) . .
O1 Pb1 O2 92.3(2) 24 .
O1 Pb1 O2 48.3(2) . .
O2 Pb1 O2 70.6(3) 24 .
O3 Pb1 C2 23.9(4) . .
O1 Pb1 C2 101.6(3) 24 .
O1 Pb1 C2 101.6(3) . .
O2 Pb1 C2 142.31(18) 24 .
O2 Pb1 C2 142.31(18) . .
O3 Pb1 C1 106.2(3) . 24
O1 Pb1 C1 23.8(3) 24 24
O1 Pb1 C1 82.6(3) . 24
O2 Pb1 C1 24.5(2) 24 24
O2 Pb1 C1 80.4(3) . 24
C2 Pb1 C1 123.0(3) . 24
O3 Pb1 C1 106.2(3) . .
O1 Pb1 C1 82.6(3) 24 .
O1 Pb1 C1 23.8(3) . .
O2 Pb1 C1 80.4(3) 24 .
O2 Pb1 C1 24.5(2) . .
C2 Pb1 C1 123.0(3) . .
C1 Pb1 C1 80.1(4) 24 .
O3 Pb1 O4 48.0(3) . .
O1 Pb1 O4 119.7(2) 24 .
O1 Pb1 O4 119.7(2) . .
O2 Pb1 O4 143.53(17) 24 .
O2 Pb1 O4 143.53(17) . .
C2 Pb1 O4 24.1(4) . .
C1 Pb1 O4 135.8(2) 24 .
C1 Pb1 O4 135.8(2) . .
O3 Pb1 O2 76.22(18) . 17
O1 Pb1 O2 70.7(2) 24 17
O1 Pb1 O2 141.7(2) . 17
O2 Pb1 O2 77.9(2) 24 17
O2 Pb1 O2 147.85(18) . 17
C2 Pb1 O2 69.44(17) . 17
C1 Pb1 O2 73.3(2) 24 17
C1 Pb1 O2 152.7(2) . 17
O4 Pb1 O2 66.17(14) . 17
O3 Pb1 O2 76.22(18) . 8
O1 Pb1 O2 141.7(2) 24 8
O1 Pb1 O2 70.7(2) . 8
O2 Pb1 O2 147.85(18) 24 8
O2 Pb1 O2 77.9(2) . 8
C2 Pb1 O2 69.44(17) . 8
C1 Pb1 O2 152.7(2) 24 8
C1 Pb1 O2 73.3(2) . 8
O4 Pb1 O2 66.17(14) . 8
O2 Pb1 O2 132.1(3) 17 8
O3 Pb1 Pb1 120.89(7) . 15
O1 Pb1 Pb1 138.63(18) 24 15
O1 Pb1 Pb1 74.98(18) . 15
O2 Pb1 Pb1 105.32(14) 24 15
O2 Pb1 Pb1 46.31(17) . 15
C2 Pb1 Pb1 112.06(14) . 15
C1 Pb1 Pb1 123.6(2) 24 15
C1 Pb1 Pb1 59.31(19) . 15
O4 Pb1 Pb1 99.91(10) . 15
O2 Pb1 Pb1 143.27(14) 17 15
O2 Pb1 Pb1 44.85(15) 8 15
O2 Rb1 O2 72.6(3) . 24
O2 Rb1 O4 68.6(2) . 8
O2 Rb1 O4 139.9(3) 24 8
O2 Rb1 O4 139.9(3) . 10
O2 Rb1 O4 68.6(2) 24 10
O4 Rb1 O4 144.9(3) 8 10
O2 Rb1 O5 142.5(2) . 1
O2 Rb1 O5 142.5(2) 24 1
O4 Rb1 O5 74.08(18) 8 1
O4 Rb1 O5 74.08(18) 10 1
C1 O1 Pb1 107.1(6) . .
C1 O2 Rb1 148.6(7) . .
C1 O2 Pb1 79.9(6) . .
Rb1 O2 Pb1 94.5(2) . .
C1 O2 Pb1 112.7(6) . 15
Rb1 O2 Pb1 98.0(2) . 15
Pb1 O2 Pb1 88.8(2) . 15
C2 O3 Pb1 109.3(9) . .
C2 O4 Pb1 77.7(8) . .
C12 N1 C12 112.4(12) 5_665 3_655
C12 N1 C12 112.4(12) 5_665 .
C12 N1 C12 112.4(12) 3_655 .
C12 N1 C11 106.3(14) 5_665 .
C12 N1 C11 106.3(14) 3_655 .
C12 N1 C11 106.3(14) . .
O2 C1 O1 124.7(10) . .
O2 C1 C4 119.0(9) . .
O1 C1 C4 116.3(9) . .
O2 C1 Pb1 75.7(6) . .
O1 C1 Pb1 49.1(5) . .
C4 C1 Pb1 165.2(7) . .
O4 C2 O3 125.0(14) . .
O4 C2 C8 120.0(13) . .
O3 C2 C8 114.9(13) . .
O4 C2 Pb1 78.3(8) . .
O3 C2 Pb1 46.8(7) . .
C8 C2 Pb1 161.7(10) . .
C4 C3 C4 122.5(13) 20_655 .
C4 C3 H3A 118.7 20_655 .
C4 C3 H3A 118.7 . .
C3 C4 C5 118.3(10) . .
C3 C4 C1 120.3(9) . .
C5 C4 C1 121.4(10) . .
C6 C5 C4 119.1(11) . .
C6 C5 H5A 120.5 . .
C4 C5 H5A 120.5 . .
C5 C6 C5 122.7(16) . 20_655
C5 C6 H6A 118.7 . .
C5 C6 H6A 118.7 20_655 .
C8 C7 C8 122(2) . 16_556
C8 C7 H7A 119.2 . .
C8 C7 H7A 119.2 16_556 .
C9 C8 C7 117.3(16) . .
C9 C8 C2 119.9(15) . .
C7 C8 C2 122.7(14) . .
C8 C9 C10 118.4(18) . .
C8 C9 C10 118.4(18) . 9
C10 C9 C10 50(3) . 9
C8 C9 H9A 120.6 . .
C10 C9 H9A 121.0 . .
C10 C9 H9A 99.7 9 .
C10 C10 C9 65.1(15) 9 .
C10 C10 C9 65.1(15) 9 16_556
C9 C10 C9 104(2) . 16_556
C10 C10 H10A 127.4 9 .
C9 C10 H10A 127.9 . .
C9 C10 H10A 127.9 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 2.293(10) .
Pb1 O1 2.348(7) 24
Pb1 O1 2.348(7) .
Pb1 O2 2.924(8) 24
Pb1 O2 2.924(8) .
Pb1 C2 2.969(15) .
Pb1 C1 2.971(10) 24
Pb1 C1 2.971(10) .
Pb1 O4 2.976(10) .
Pb1 O2 2.998(9) 17
Pb1 O2 2.998(9) 8
Pb1 Pb1 4.1451(6) 15
Rb1 O2 2.854(7) .
Rb1 O2 2.854(7) 24
Rb1 O4 2.929(7) 8
Rb1 O4 2.929(7) 10
Rb1 O5 2.998(18) 1
O1 C1 1.256(13) .
O2 C1 1.250(12) .
O2 Pb1 2.998(9) 15
O3 C2 1.276(17) .
O4 C2 1.239(19) .
O5 O5 0.00(6) 1
N1 C12 1.49(2) 5_665
N1 C12 1.49(2) 3_655
N1 C12 1.49(2) .
N1 C11 1.62(5) .
C1 C4 1.514(15) .
C2 C8 1.50(2) .
C3 C4 1.382(13) 20_655
C3 C4 1.382(13) .
C3 H3A 0.9300 .
C4 C5 1.401(15) .
C5 C6 1.369(14) .
C5 H5A 0.9300 .
C6 C5 1.369(14) 20_655
C6 H6A 0.9300 .
C7 C8 1.388(18) .
C7 C8 1.388(18) 16_556
C7 H7A 0.9300 .
C8 C9 1.36(2) .
C9 C10 1.48(3) .
C9 C10 1.48(3) 9
C9 H9A 0.9643 .
C10 C10 1.25(8) 9
C10 C9 1.48(3) 16_556
C10 H10A 0.9601 .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
