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#$Date: 2016-03-25 10:05:59 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179740 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/36/7003611.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_7003611
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 Ag Ge18 Li O6 Si24'
_chemical_formula_weight         3340.05
_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                97.049(17)
_cell_angle_beta                 97.049(17)
_cell_angle_gamma                97.049(17)
_cell_formula_units_Z            1
_cell_length_a                   15.6343(18)
_cell_length_b                   15.6343(18)
_cell_length_c                   15.6343(18)
_cell_measurement_reflns_used    18451
_cell_measurement_temperature    149(2)
_cell_measurement_theta_max      25.955
_cell_measurement_theta_min      1.705
_cell_volume                     3727.0(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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0513
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13286
_diffrn_reflns_theta_full        25.94
_diffrn_reflns_theta_max         25.94
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    3.925
_exptl_absorpt_correction_T_max  0.4943
_exptl_absorpt_correction_T_min  0.4022
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         4833
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0348
_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)+(0.0420P)²+2.8876P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0882
_reflns_number_gt                3990
_reflns_number_total             4833
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b717506j.txt
_cod_data_source_block           cs68p-3
_cod_original_cell_volume        3727.0(7)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7003611
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
Ag1 Ag 0.5000 0.5000 0.5000 0.03367(15) Uani 1 6 d S . .
Ge1 Ge 0.30882(3) 0.43613(3) 0.26417(3) 0.03642(11) Uani 1 1 d . . .
Ge2 Ge 0.32698(2) 0.46254(2) 0.42753(2) 0.03087(10) Uani 1 1 d . . .
Ge3 Ge 0.19038(2) 0.31609(3) 0.28333(3) 0.03456(11) Uani 1 1 d . . .
Si1 Si 0.26436(7) 0.54330(6) 0.18036(6) 0.0321(2) Uani 1 1 d . . .
Si2 Si 0.23213(8) 0.47924(7) 0.03436(7) 0.0409(3) Uani 1 1 d . . .
Si3 Si 0.37963(8) 0.65810(7) 0.20031(8) 0.0459(3) Uani 1 1 d . . .
Si4 Si 0.13891(8) 0.58786(9) 0.23136(9) 0.0505(3) Uani 1 1 d . . .
C2C C 0.1929(4) 0.5618(3) -0.0336(3) 0.0712(16) Uani 1 1 d . . .
H2CA H 0.1793 0.5354 -0.0948 0.107 Uiso 1 1 calc R . .
H2CB H 0.2385 0.6119 -0.0280 0.107 Uiso 1 1 calc R . .
H2CC H 0.1406 0.5810 -0.0135 0.107 Uiso 1 1 calc R . .
C2B C 0.1419(3) 0.3869(3) 0.0216(3) 0.0604(13) Uani 1 1 d . . .
H2BA H 0.1290 0.3607 -0.0396 0.091 Uiso 1 1 calc R . .
H2BB H 0.0898 0.4084 0.0403 0.091 Uiso 1 1 calc R . .
H2BC H 0.1593 0.3431 0.0575 0.091 Uiso 1 1 calc R . .
C2A C 0.3296(4) 0.4386(4) -0.0068(3) 0.0659(14) Uani 1 1 d . . .
H2AA H 0.3140 0.4123 -0.0678 0.099 Uiso 1 1 calc R . .
H2AB H 0.3493 0.3950 0.0281 0.099 Uiso 1 1 calc R . .
H2AC H 0.3765 0.4873 -0.0023 0.099 Uiso 1 1 calc R . .
C3C C 0.4746(3) 0.6235(4) 0.1503(5) 0.0789(17) Uani 1 1 d . . .
H3CA H 0.5219 0.6724 0.1594 0.118 Uiso 1 1 calc R . .
H3CB H 0.4572 0.6050 0.0877 0.118 Uiso 1 1 calc R . .
H3CC H 0.4946 0.5749 0.1775 0.118 Uiso 1 1 calc R . .
C3B C 0.4138(5) 0.6948(4) 0.3179(4) 0.098(3) Uani 1 1 d . . .
H3BA H 0.4620 0.7427 0.3259 0.148 Uiso 1 1 calc R . .
H3BB H 0.4329 0.6463 0.3460 0.148 Uiso 1 1 calc R . .
H3BC H 0.3647 0.7147 0.3442 0.148 Uiso 1 1 calc R . .
C3A C 0.3449(4) 0.7513(3) 0.1467(4) 0.0685(15) Uani 1 1 d . . .
H3AA H 0.3935 0.7989 0.1554 0.103 Uiso 1 1 calc R . .
H3AB H 0.2957 0.7716 0.1724 0.103 Uiso 1 1 calc R . .
H3AC H 0.3274 0.7322 0.0843 0.103 Uiso 1 1 calc R . .
C4B C 0.1632(7) 0.6261(11) 0.3479(5) 0.234(9) Uani 1 1 d . . .
H4BA H 0.1110 0.6447 0.3692 0.352 Uiso 1 1 calc R . .
H4BB H 0.2102 0.6754 0.3585 0.352 Uiso 1 1 calc R . .
H4BC H 0.1813 0.5789 0.3785 0.352 Uiso 1 1 calc R . .
C4C C 0.1013(4) 0.6753(5) 0.1730(6) 0.112(3) Uani 1 1 d . . .
H4CA H 0.0491 0.6930 0.1951 0.168 Uiso 1 1 calc R . .
H4CB H 0.0875 0.6540 0.1106 0.168 Uiso 1 1 calc R . .
H4CC H 0.1473 0.7254 0.1824 0.168 Uiso 1 1 calc R . .
C4A C 0.0464(4) 0.4980(5) 0.2112(7) 0.129(4) Uani 1 1 d . . .
H4AA H -0.0044 0.5189 0.2332 0.193 Uiso 1 1 calc R . .
H4AB H 0.0625 0.4496 0.2413 0.193 Uiso 1 1 calc R . .
H4AC H 0.0324 0.4781 0.1486 0.193 Uiso 1 1 calc R . .
O100 O -0.0322(2) 0.1197(2) 0.0649(2) 0.0508(7) Uani 1 1 d . . .
C100 C -0.0796(4) 0.1836(3) 0.0304(3) 0.0614(12) Uani 1 1 d . . .
H10A H -0.1418 0.1596 0.0130 0.074 Uiso 1 1 calc R . .
H10B H -0.0556 0.2022 -0.0212 0.074 Uiso 1 1 calc R . .
C101 C -0.0697(5) 0.2585(4) 0.1016(4) 0.0801(17) Uani 1 1 d . . .
H10C H -0.0186 0.3014 0.0981 0.096 Uiso 1 1 calc R . .
H10D H -0.1223 0.2880 0.0987 0.096 Uiso 1 1 calc R . .
C102 C -0.0576(4) 0.2181(4) 0.1820(4) 0.0657(14) Uani 1 1 d . . .
H10E H -0.1142 0.1951 0.1985 0.079 Uiso 1 1 calc R . .
H10F H -0.0247 0.2602 0.2310 0.079 Uiso 1 1 calc R . .
C103 C -0.0066(3) 0.1459(3) 0.1568(3) 0.0617(13) Uani 1 1 d . . .
H10G H 0.0567 0.1667 0.1695 0.074 Uiso 1 1 calc R . .
H10H H -0.0201 0.0965 0.1892 0.074 Uiso 1 1 calc R . .
Li1 Li 0.0000 0.0000 0.0000 0.050(4) 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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 '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 Ag1 Ge2 117.80(3) 6_666 2 ?
Ge2 Ag1 Ge2 62.20(3) 6_666 4_666 ?
Ge2 Ag1 Ge2 117.80(3) 2 4_666 ?
Ge2 Ag1 Ge2 117.80(3) 6_666 . ?
Ge2 Ag1 Ge2 62.20(3) 2 . ?
Ge2 Ag1 Ge2 180.000(7) 4_666 . ?
Ge2 Ag1 Ge2 62.20(3) 6_666 5_666 ?
Ge2 Ag1 Ge2 180.0 2 5_666 ?
Ge2 Ag1 Ge2 62.20(3) 4_666 5_666 ?
Ge2 Ag1 Ge2 117.80(3) . 5_666 ?
Ge2 Ag1 Ge2 180.000(1) 6_666 3 ?
Ge2 Ag1 Ge2 62.20(3) 2 3 ?
Ge2 Ag1 Ge2 117.80(3) 4_666 3 ?
Ge2 Ag1 Ge2 62.20(3) . 3 ?
Ge2 Ag1 Ge2 117.80(3) 5_666 3 ?
Si1 Ge1 Ge2 125.41(3) . 3 ?
Si1 Ge1 Ge2 121.08(3) . . ?
Ge2 Ge1 Ge2 69.34(3) 3 . ?
Si1 Ge1 Ge3 116.27(3) . . ?
Ge2 Ge1 Ge3 118.22(3) 3 . ?
Ge2 Ge1 Ge3 83.10(3) . . ?
Si1 Ge1 Ge3 120.12(3) . 3 ?
Ge2 Ge1 Ge3 83.13(3) 3 3 ?
Ge2 Ge1 Ge3 118.12(3) . 3 ?
Ge3 Ge1 Ge3 62.70(3) . 3 ?
Ge1 Ge2 Ge1 92.33(3) 2 . ?
Ge1 Ge2 Ag1 112.27(3) 2 . ?
Ge1 Ge2 Ag1 112.15(3) . . ?
Ge1 Ge2 Ge2 98.812(14) 2 3 ?
Ge1 Ge2 Ge2 55.272(18) . 3 ?
Ag1 Ge2 Ge2 58.901(13) . 3 ?
Ge1 Ge2 Ge2 55.388(18) 2 2 ?
Ge1 Ge2 Ge2 98.728(14) . 2 ?
Ag1 Ge2 Ge2 58.901(13) . 2 ?
Ge2 Ge2 Ge2 60.0 3 2 ?
Ge1 Ge3 Ge1 90.77(3) . 2 ?
Ge1 Ge3 Ge3 58.690(19) . 3 ?
Ge1 Ge3 Ge3 101.018(15) 2 3 ?
Ge1 Ge3 Ge3 101.074(15) . 2 ?
Ge1 Ge3 Ge3 58.611(18) 2 2 ?
Ge3 Ge3 Ge3 60.0 3 2 ?
Si3 Si1 Si2 111.55(7) . . ?
Si3 Si1 Si4 111.91(6) . . ?
Si2 Si1 Si4 110.49(6) . . ?
Si3 Si1 Ge1 107.50(5) . . ?
Si2 Si1 Ge1 107.97(5) . . ?
Si4 Si1 Ge1 107.19(5) . . ?
C2B Si2 C2A 109.2(3) . . ?
C2B Si2 C2C 107.0(3) . . ?
C2A Si2 C2C 109.7(3) . . ?
C2B Si2 Si1 110.24(17) . . ?
C2A Si2 Si1 111.55(17) . . ?
C2C Si2 Si1 109.04(18) . . ?
C3B Si3 C3C 109.1(4) . . ?
C3B Si3 C3A 109.3(3) . . ?
C3C Si3 C3A 107.6(3) . . ?
C3B Si3 Si1 109.8(2) . . ?
C3C Si3 Si1 110.91(19) . . ?
C3A Si3 Si1 110.11(18) . . ?
C4B Si4 C4C 110.0(6) . . ?
C4B Si4 C4A 109.2(7) . . ?
C4C Si4 C4A 105.7(4) . . ?
C4B Si4 Si1 109.4(3) . . ?
C4C Si4 Si1 110.7(2) . . ?
C4A Si4 Si1 111.8(2) . . ?
C100 O100 C103 108.9(4) . . ?
C100 O100 Li1 129.8(3) . . ?
C103 O100 Li1 121.3(3) . . ?
O100 C100 C101 106.1(4) . . ?
C102 C101 C100 103.9(5) . . ?
C101 C102 C103 102.6(5) . . ?
O100 C103 C102 106.1(4) . . ?
O100 Li1 O100 87.58(11) 4 3 ?
O100 Li1 O100 92.42(11) 4 5 ?
O100 Li1 O100 87.58(11) 3 5 ?
O100 Li1 O100 180.0(2) 4 . ?
O100 Li1 O100 92.42(11) 3 . ?
O100 Li1 O100 87.58(11) 5 . ?
O100 Li1 O100 87.58(11) 4 2 ?
O100 Li1 O100 92.42(11) 3 2 ?
O100 Li1 O100 180.00(16) 5 2 ?
O100 Li1 O100 92.42(11) . 2 ?
O100 Li1 O100 92.42(11) 4 6 ?
O100 Li1 O100 180.00(17) 3 6 ?
O100 Li1 O100 92.42(11) 5 6 ?
O100 Li1 O100 87.58(11) . 6 ?
O100 Li1 O100 87.58(11) 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
Ag1 Ge2 2.7641(8) 6_666 ?
Ag1 Ge2 2.7641(7) 2 ?
Ag1 Ge2 2.7641(7) 4_666 ?
Ag1 Ge2 2.7641(7) . ?
Ag1 Ge2 2.7641(7) 5_666 ?
Ag1 Ge2 2.7641(7) 3 ?
Ge1 Si1 2.3684(11) . ?
Ge1 Ge2 2.5080(6) 3 ?
Ge1 Ge2 2.5116(7) . ?
Ge1 Ge3 2.5421(7) . ?
Ge1 Ge3 2.5442(7) 3 ?
Ge2 Ge1 2.5080(6) 2 ?
Ge2 Ge2 2.8554(8) 3 ?
Ge2 Ge2 2.8554(8) 2 ?
Ge3 Ge1 2.5442(7) 2 ?
Ge3 Ge3 2.6462(8) 3 ?
Ge3 Ge3 2.6462(8) 2 ?
Si1 Si3 2.3445(16) . ?
Si1 Si2 2.3452(15) . ?
Si1 Si4 2.3561(16) . ?
Si2 C2B 1.865(5) . ?
Si2 C2A 1.876(6) . ?
Si2 C2C 1.882(5) . ?
Si3 C3B 1.849(6) . ?
Si3 C3C 1.867(6) . ?
Si3 C3A 1.871(5) . ?
Si4 C4B 1.824(7) . ?
Si4 C4C 1.850(6) . ?
Si4 C4A 1.855(7) . ?
O100 C100 1.434(6) . ?
O100 C103 1.437(6) . ?
O100 Li1 2.162(3) . ?
C100 C101 1.493(8) . ?
C101 C102 1.478(8) . ?
C102 C103 1.503(7) . ?
Li1 O100 2.162(3) 4 ?
Li1 O100 2.162(3) 3 ?
Li1 O100 2.162(3) 5 ?
Li1 O100 2.162(3) 2 ?
Li1 O100 2.162(3) 6 ?
