#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:05:59 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179740 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/36/7003612.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_7003612
loop_
_publ_author_name
'Schenk, Christian'
'Henke, Florian'
'Santiso-Quiñones, Gustavo'
'Krossing, Ingo'
'Schnepf, Andreas'
_publ_section_title
;
 [Si(SiMe3)3]6Ge18M (M = Cu, Ag, Au): metalloid cluster compounds as
 unusual building blocks for a supramolecular chemistry
;
_journal_issue                   33
_journal_name_full               'Dalton Transactions'
_journal_page_first              4436
_journal_page_last               4441
_journal_paper_doi               10.1039/b717506j
_journal_year                    2008
_chemical_formula_sum            'C78 H210 Cu Ge18 Li O6 Si24'
_chemical_formula_weight         3295.72
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-P 3*'
_symmetry_space_group_name_H-M   'R -3 :R'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.309(17)
_cell_angle_beta                 97.309(17)
_cell_angle_gamma                97.309(17)
_cell_formula_units_Z            1
_cell_length_a                   15.6548(18)
_cell_length_b                   15.6548(18)
_cell_length_c                   15.6548(18)
_cell_measurement_reflns_used    10596
_cell_measurement_temperature    149(2)
_cell_measurement_theta_max      23.93
_cell_measurement_theta_min      1.285
_cell_volume                     3734.2(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      149(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0673
_diffrn_reflns_av_sigmaI/netI    0.0559
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15371
_diffrn_reflns_theta_full        24.01
_diffrn_reflns_theta_max         24.01
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    3.928
_exptl_absorpt_correction_T_max  0.8191
_exptl_absorpt_correction_T_min  0.7262
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1670
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.092
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         3883
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0403
_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)+(0.0443P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0869
_reflns_number_gt                2733
_reflns_number_total             3883
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b717506j.txt
_cod_data_source_block           cs75r-3b
_cod_original_cell_volume        3734.2(7)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7003612
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'z, x, y'
'y, z, x'
'-x, -y, -z'
'-z, -x, -y'
'-y, -z, -x'
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
Ge1 Ge 0.43383(4) 0.46974(4) 0.33470(4) 0.03352(16) Uani 1 1 d . . .
Ge2 Ge 0.44181(4) 0.31576(4) 0.26982(4) 0.03530(16) Uani 1 1 d . . .
Ge3 Ge 0.32158(4) 0.19631(4) 0.28801(4) 0.03697(17) Uani 1 1 d . . .
Cu1 Cu 0.5000 0.5000 0.5000 0.0231(3) Uani 1 6 d S . .
Si1 Si 0.54460(9) 0.26780(10) 0.18194(10) 0.0321(3) Uani 1 1 d . . .
Si10 Si 0.58657(13) 0.14088(12) 0.23005(12) 0.0507(5) Uani 1 1 d . . .
Si11 Si 0.66249(11) 0.37944(12) 0.19895(12) 0.0473(4) Uani 1 1 d . . .
Si12 Si 0.47650(11) 0.23688(11) 0.03673(10) 0.0415(4) Uani 1 1 d . . .
C10C C 0.4960(6) 0.0487(6) 0.2095(9) 0.130(5) Uani 1 1 d . . .
H10A H 0.5166 -0.0024 0.2306 0.195 Uiso 1 1 calc R . .
H10B H 0.4752 0.0351 0.1469 0.195 Uiso 1 1 calc R . .
H10C H 0.4482 0.0648 0.2401 0.195 Uiso 1 1 calc R . .
C10B C 0.6714(7) 0.1018(7) 0.1712(9) 0.142(6) Uani 1 1 d . . .
H10D H 0.6876 0.0490 0.1925 0.213 Uiso 1 1 calc R . .
H10E H 0.7226 0.1468 0.1809 0.213 Uiso 1 1 calc R . .
H10F H 0.6493 0.0886 0.1088 0.213 Uiso 1 1 calc R . .
C10A C 0.6259(14) 0.1624(9) 0.3463(7) 0.245(12) Uani 1 1 d . . .
H10G H 0.6434 0.1093 0.3659 0.367 Uiso 1 1 calc R . .
H10H H 0.5795 0.1807 0.3777 0.367 Uiso 1 1 calc R . .
H10I H 0.6761 0.2086 0.3578 0.367 Uiso 1 1 calc R . .
C11C C 0.7519(4) 0.3414(5) 0.1417(5) 0.068(2) Uani 1 1 d . . .
H11A H 0.8009 0.3886 0.1493 0.102 Uiso 1 1 calc R . .
H11B H 0.7303 0.3242 0.0795 0.102 Uiso 1 1 calc R . .
H11C H 0.7712 0.2914 0.1663 0.102 Uiso 1 1 calc R . .
C11B C 0.6303(6) 0.4751(5) 0.1510(7) 0.094(3) Uani 1 1 d . . .
H11D H 0.6807 0.5209 0.1590 0.141 Uiso 1 1 calc R . .
H11E H 0.5839 0.4970 0.1801 0.141 Uiso 1 1 calc R . .
H11F H 0.6093 0.4579 0.0888 0.141 Uiso 1 1 calc R . .
C11A C 0.7051(6) 0.4119(7) 0.3153(6) 0.111(4) Uani 1 1 d . . .
H11G H 0.7545 0.4586 0.3220 0.166 Uiso 1 1 calc R . .
H11H H 0.7243 0.3617 0.3398 0.166 Uiso 1 1 calc R . .
H11I H 0.6592 0.4325 0.3461 0.166 Uiso 1 1 calc R . .
C12C C 0.4374(5) 0.3343(5) -0.0028(5) 0.069(2) Uani 1 1 d . . .
H12A H 0.4095 0.3188 -0.0635 0.103 Uiso 1 1 calc R . .
H12B H 0.4869 0.3804 0.0010 0.103 Uiso 1 1 calc R . .
H12C H 0.3953 0.3549 0.0333 0.103 Uiso 1 1 calc R . .
C12B C 0.3833(4) 0.1479(5) 0.0240(4) 0.0606(18) Uani 1 1 d . . .
H12D H 0.3558 0.1359 -0.0370 0.091 Uiso 1 1 calc R . .
H12E H 0.3407 0.1655 0.0610 0.091 Uiso 1 1 calc R . .
H12F H 0.4042 0.0953 0.0412 0.091 Uiso 1 1 calc R . .
C12A C 0.5568(5) 0.1967(6) -0.0327(5) 0.073(2) Uani 1 1 d . . .
H12G H 0.5294 0.1835 -0.0936 0.109 Uiso 1 1 calc R . .
H12H H 0.5754 0.1439 -0.0133 0.109 Uiso 1 1 calc R . .
H12I H 0.6076 0.2417 -0.0272 0.109 Uiso 1 1 calc R . .
O100 O 0.1229(3) -0.0303(3) 0.0611(3) 0.0512(11) Uani 1 1 d . . .
C100 C 0.1851(5) -0.0776(5) 0.0236(5) 0.0629(19) Uani 1 1 d . . .
H10J H 0.2044 -0.0506 -0.0259 0.075 Uiso 1 1 calc R . .
H10K H 0.1586 -0.1386 0.0019 0.075 Uiso 1 1 calc R . .
C101 C 0.2600(5) -0.0749(7) 0.0926(6) 0.081(2) Uani 1 1 d . . .
H10L H 0.3072 -0.0276 0.0888 0.097 Uiso 1 1 calc R . .
H10M H 0.2833 -0.1309 0.0881 0.097 Uiso 1 1 calc R . .
C102 C 0.2229(5) -0.0582(5) 0.1752(5) 0.0645(19) Uani 1 1 d . . .
H10N H 0.1975 -0.1133 0.1929 0.077 Uiso 1 1 calc R . .
H10O H 0.2679 -0.0266 0.2229 0.077 Uiso 1 1 calc R . .
C103 C 0.1546(5) -0.0038(5) 0.1528(4) 0.0632(19) Uani 1 1 d . . .
H10P H 0.1068 -0.0135 0.1878 0.076 Uiso 1 1 calc R . .
H10Q H 0.1792 0.0587 0.1641 0.076 Uiso 1 1 calc R . .
Li1 Li 0.0000 0.0000 0.0000 0.039(5) Uani 1 6 d S . .
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'
Li Li -0.0003 0.0001 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 '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
_geom_angle_publ_flag
Ge2 Ge1 Ge2 91.99(4) . 2 ?
Ge2 Ge1 Cu1 111.15(3) . . ?
Ge2 Ge1 Cu1 111.05(3) 2 . ?
Ge2 Ge1 Ge1 55.65(2) . 3 ?
Ge2 Ge1 Ge1 98.84(2) 2 3 ?
Cu1 Ge1 Ge1 57.112(15) . 3 ?
Ge2 Ge1 Ge1 98.915(19) . 2 ?
Ge2 Ge1 Ge1 55.55(2) 2 2 ?
Cu1 Ge1 Ge1 57.112(15) . 2 ?
Ge1 Ge1 Ge1 60.0 3 2 ?
Si1 Ge2 Ge1 127.24(5) . . ?
Si1 Ge2 Ge1 122.50(4) . 3 ?
Ge1 Ge2 Ge1 68.80(3) . 3 ?
Si1 Ge2 Ge3 114.37(5) . . ?
Ge1 Ge2 Ge3 118.20(3) . . ?
Ge1 Ge2 Ge3 83.50(4) 3 . ?
Si1 Ge2 Ge3 118.43(5) . 2 ?
Ge1 Ge2 Ge3 83.52(4) . 2 ?
Ge1 Ge2 Ge3 118.11(3) 3 2 ?
Ge3 Ge2 Ge3 62.35(3) . 2 ?
Ge2 Ge3 Ge2 90.61(4) . 3 ?
Ge2 Ge3 Ge3 101.17(2) . 3 ?
Ge2 Ge3 Ge3 58.79(3) 3 3 ?
Ge2 Ge3 Ge3 58.86(3) . 2 ?
Ge2 Ge3 Ge3 101.12(2) 3 2 ?
Ge3 Ge3 Ge3 60.0 3 2 ?
Ge1 Cu1 Ge1 114.23(3) 4_666 3 ?
Ge1 Cu1 Ge1 65.78(3) 4_666 6_666 ?
Ge1 Cu1 Ge1 180.000(10) 3 6_666 ?
Ge1 Cu1 Ge1 114.23(3) 4_666 2 ?
Ge1 Cu1 Ge1 65.78(3) 3 2 ?
Ge1 Cu1 Ge1 114.22(3) 6_666 2 ?
Ge1 Cu1 Ge1 180.0 4_666 . ?
Ge1 Cu1 Ge1 65.78(3) 3 . ?
Ge1 Cu1 Ge1 114.22(3) 6_666 . ?
Ge1 Cu1 Ge1 65.78(3) 2 . ?
Ge1 Cu1 Ge1 65.78(3) 4_666 5_666 ?
Ge1 Cu1 Ge1 114.22(3) 3 5_666 ?
Ge1 Cu1 Ge1 65.78(3) 6_666 5_666 ?
Ge1 Cu1 Ge1 180.0 2 5_666 ?
Ge1 Cu1 Ge1 114.22(3) . 5_666 ?
Si11 Si1 Si12 111.10(9) . . ?
Si11 Si1 Si10 111.75(9) . . ?
Si12 Si1 Si10 110.30(9) . . ?
Si11 Si1 Ge2 107.91(7) . . ?
Si12 Si1 Ge2 108.27(7) . . ?
Si10 Si1 Ge2 107.35(7) . . ?
C10A Si10 C10B 109.7(8) . . ?
C10A Si10 C10C 108.5(8) . . ?
C10B Si10 C10C 104.9(6) . . ?
C10A Si10 Si1 109.8(4) . . ?
C10B Si10 Si1 111.2(3) . . ?
C10C Si10 Si1 112.6(3) . . ?
C11A Si11 C11B 109.8(5) . . ?
C11A Si11 C11C 108.5(5) . . ?
C11B Si11 C11C 107.4(4) . . ?
C11A Si11 Si1 109.9(3) . . ?
C11B Si11 Si1 111.0(3) . . ?
C11C Si11 Si1 110.2(2) . . ?
C12B Si12 C12C 109.2(4) . . ?
C12B Si12 C12A 106.9(4) . . ?
C12C Si12 C12A 109.6(4) . . ?
C12B Si12 Si1 110.7(2) . . ?
C12C Si12 Si1 111.9(3) . . ?
C12A Si12 Si1 108.4(3) . . ?
C100 O100 C103 108.1(5) . . ?
C100 O100 Li1 129.4(4) . . ?
C103 O100 Li1 122.4(4) . . ?
O100 C100 C101 107.5(6) . . ?
C100 C101 C102 104.0(6) . . ?
C103 C102 C101 103.3(6) . . ?
O100 C103 C102 106.2(5) . . ?
O100 Li1 O100 87.54(15) 5 3 ?
O100 Li1 O100 87.54(15) 5 . ?
O100 Li1 O100 92.46(15) 3 . ?
O100 Li1 O100 92.46(15) 5 4 ?
O100 Li1 O100 87.54(15) 3 4 ?
O100 Li1 O100 180.0(3) . 4 ?
O100 Li1 O100 180.0(3) 5 2 ?
O100 Li1 O100 92.46(15) 3 2 ?
O100 Li1 O100 92.46(15) . 2 ?
O100 Li1 O100 87.54(15) 4 2 ?
O100 Li1 O100 92.46(15) 5 6 ?
O100 Li1 O100 180.0(2) 3 6 ?
O100 Li1 O100 87.54(15) . 6 ?
O100 Li1 O100 92.46(15) 4 6 ?
O100 Li1 O100 87.54(15) 2 6 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 Ge2 2.5186(9) . ?
Ge1 Ge2 2.5217(9) 2 ?
Ge1 Cu1 2.6221(8) . ?
Ge1 Ge1 2.8475(10) 3 ?
Ge1 Ge1 2.8475(10) 2 ?
Ge2 Si1 2.3777(15) . ?
Ge2 Ge1 2.5217(9) 3 ?
Ge2 Ge3 2.5489(9) . ?
Ge2 Ge3 2.5508(9) 2 ?
Ge3 Ge2 2.5508(9) 3 ?
Ge3 Ge3 2.6400(11) 3 ?
Ge3 Ge3 2.6400(11) 2 ?
Cu1 Ge1 2.6221(8) 4_666 ?
Cu1 Ge1 2.6221(8) 3 ?
Cu1 Ge1 2.6221(8) 6_666 ?
Cu1 Ge1 2.6221(8) 2 ?
Cu1 Ge1 2.6221(8) 5_666 ?
Si1 Si11 2.338(2) . ?
Si1 Si12 2.347(2) . ?
Si1 Si10 2.352(2) . ?
Si10 C10A 1.819(10) . ?
Si10 C10B 1.833(8) . ?
Si10 C10C 1.855(10) . ?
Si11 C11A 1.841(9) . ?
Si11 C11B 1.855(9) . ?
Si11 C11C 1.875(6) . ?
Si12 C12B 1.857(7) . ?
Si12 C12C 1.861(7) . ?
Si12 C12A 1.879(7) . ?
O100 C100 1.435(8) . ?
O100 C103 1.446(8) . ?
O100 Li1 2.173(4) . ?
C100 C101 1.482(10) . ?
C101 C102 1.491(11) . ?
C102 C103 1.484(9) . ?
Li1 O100 2.173(4) 5 ?
Li1 O100 2.173(4) 3 ?
Li1 O100 2.173(4) 4 ?
Li1 O100 2.173(4) 2 ?
Li1 O100 2.173(4) 6 ?
