#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:15:02 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178891 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/20/4112089.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_4112089
loop_
_publ_author_name
'Chunming Cui'
'Marilyn M. Olmstead'
'James C. Fettinger'
'Geoffrey H. Spikes'
'Philip P. Power'
_publ_section_title
;
 Reactions of the Heavier Group 14 Element Alkyne Analogues Ar'EEAr' (Ar'
 = C6H3-2,6(C6H3-2,6-Pri2)2; E = Ge, Sn) with Unsaturated Molecules:
 Probing the Character of the EE Multiple Bonds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17530
_journal_page_last               17541
_journal_paper_doi               10.1021/ja055372s
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C63 H83 Ge2 O5'
_chemical_formula_weight         1065.47
_chemical_name_common
'[Dipp*Ge(OH)(μ-OO)(μ-O)Ge(OH)Dipp*].0.5hexane'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 104.633(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.868(6)
_cell_length_b                   18.065(7)
_cell_length_c                   22.078(9)
_cell_measurement_reflns_used    571
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      29.0
_cell_measurement_theta_min      2.35
_cell_volume                     5738(4)
_computing_cell_refinement       'SAINT 6.45A (Bruker, 2003)'
_computing_data_collection       'SMART 5.054 (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       ω
_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  0.206
_diffrn_reflns_av_sigmaI/netI    0.205
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26109
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.094
_exptl_absorpt_correction_T_max  0.9470
_exptl_absorpt_correction_T_min  0.880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       block
_exptl_crystal_F_000             2260
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.623
_refine_diff_density_min         -1.327
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     648
_refine_ls_number_reflns         7505
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.1815
_refine_ls_R_factor_gt           0.0907
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1371P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2006
_refine_ls_wR_factor_ref         0.2620
_reflns_number_gt                3607
_reflns_number_total             7505
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja055372ssi20050805_073337.cif
_cod_data_source_block           mn1607
_cod_original_cell_volume        5737(4)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4112089
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Ge1 Ge 0.21827(8) 0.29830(7) 0.71808(6) 0.0287(4) Uani 1 1 d .
Ge2 Ge 0.40684(8) 0.25192(7) 0.72698(6) 0.0272(4) Uani 1 1 d .
O1 O 0.1312(5) 0.2313(4) 0.7146(4) 0.036(2) Uani 1 1 d .
O2 O 0.4660(5) 0.3368(4) 0.7341(4) 0.031(2) Uani 1 1 d .
H2 H 0.5115 0.3350 0.7074 0.037 Uiso 1 1 d .
O3 O 0.3233(5) 0.2694(4) 0.7686(4) 0.034(2) Uani 1 1 d .
O4 O 0.2548(5) 0.2992(4) 0.6453(4) 0.035(2) Uani 1 1 d .
O5 O 0.3290(5) 0.2419(4) 0.6484(4) 0.038(2) Uani 1 1 d .
C1 C 0.1748(7) 0.3958(6) 0.7316(6) 0.025(3) Uani 1 1 d .
C2 C 0.1407(7) 0.4436(6) 0.6787(6) 0.029(3) Uani 1 1 d .
C3 C 0.1167(7) 0.5162(6) 0.6897(5) 0.026(3) Uani 1 1 d .
H3 H 0.0945 0.5484 0.6551 0.032 Uiso 1 1 calc R
C4 C 0.1242(7) 0.5425(6) 0.7490(5) 0.029(3) Uani 1 1 d .
H4 H 0.1100 0.5927 0.7553 0.035 Uiso 1 1 calc R
C5 C 0.1527(7) 0.4952(6) 0.8000(6) 0.028(3) Uani 1 1 d .
H5 H 0.1559 0.5134 0.8409 0.034 Uiso 1 1 calc R
C6 C 0.1768(7) 0.4219(6) 0.7925(5) 0.027(3) Uani 1 1 d .
C7 C 0.2015(7) 0.3717(6) 0.8495(6) 0.026(3) Uani 1 1 d .
C8 C 0.2843(8) 0.3818(7) 0.8946(6) 0.031(3) Uani 1 1 d .
C9 C 0.3016(9) 0.3371(7) 0.9481(6) 0.036(3) Uani 1 1 d .
H9 H 0.3585 0.3419 0.9793 0.044 Uiso 1 1 calc R
C10 C 0.2354(10) 0.2854(8) 0.9558(6) 0.046(4) Uani 1 1 d .
H10 H 0.2479 0.2549 0.9921 0.056 Uiso 1 1 calc R
C11 C 0.1528(9) 0.2784(7) 0.9118(6) 0.041(4) Uani 1 1 d .
H11 H 0.1081 0.2439 0.9185 0.050 Uiso 1 1 calc R
C12 C 0.1323(8) 0.3211(7) 0.8565(6) 0.037(3) Uani 1 1 d .
C13 C 0.0375(8) 0.3183(7) 0.8135(6) 0.034(3) Uani 1 1 d .
H13 H 0.0442 0.3314 0.7708 0.041 Uiso 1 1 calc R
C14 C -0.0267(8) 0.3746(7) 0.8299(6) 0.047(4) Uani 1 1 d .
H14A H -0.0016 0.4244 0.8274 0.070 Uiso 1 1 calc R
H14B H -0.0322 0.3656 0.8726 0.070 Uiso 1 1 calc R
H14C H -0.0881 0.3706 0.8006 0.070 Uiso 1 1 calc R
C15 C -0.0079(9) 0.2390(7) 0.8083(7) 0.052(4) Uani 1 1 d .
H15A H 0.0336 0.2031 0.7959 0.078 Uiso 1 1 calc R
H15B H -0.0676 0.2398 0.7768 0.078 Uiso 1 1 calc R
H15C H -0.0178 0.2247 0.8489 0.078 Uiso 1 1 calc R
C16 C 0.3556(7) 0.4383(7) 0.8885(6) 0.033(3) Uani 1 1 d .
H16 H 0.3324 0.4642 0.8475 0.039 Uiso 1 1 calc R
C17 C 0.4517(8) 0.4030(8) 0.8894(6) 0.048(4) Uani 1 1 d .
H17A H 0.4446 0.3687 0.8541 0.072 Uiso 1 1 calc R
H17B H 0.4750 0.3760 0.9288 0.072 Uiso 1 1 calc R
H17C H 0.4959 0.4420 0.8860 0.072 Uiso 1 1 calc R
C18 C 0.3705(8) 0.4974(7) 0.9414(6) 0.050(4) Uani 1 1 d .
H18A H 0.3107 0.5199 0.9418 0.076 Uiso 1 1 calc R
H18B H 0.4130 0.5358 0.9338 0.076 Uiso 1 1 calc R
H18C H 0.3973 0.4737 0.9819 0.076 Uiso 1 1 calc R
C19 C 0.1175(8) 0.4184(6) 0.6114(6) 0.032(3) Uani 1 1 d .
C20 C 0.0266(8) 0.3879(7) 0.5871(6) 0.034(3) Uani 1 1 d .
C21 C 0.0029(9) 0.3724(7) 0.5238(7) 0.045(4) Uani 1 1 d .
H21 H -0.0571 0.3528 0.5054 0.055 Uiso 1 1 calc R
C22 C 0.0626(9) 0.3842(8) 0.4863(6) 0.048(4) Uani 1 1 d .
H22 H 0.0430 0.3729 0.4429 0.057 Uiso 1 1 calc R
C23 C 0.1503(10) 0.4122(7) 0.5109(6) 0.047(4) Uani 1 1 d .
H23 H 0.1910 0.4205 0.4846 0.056 Uiso 1 1 calc R
C24 C 0.1792(9) 0.4285(7) 0.5749(6) 0.039(3) Uani 1 1 d .
C25 C -0.0428(8) 0.3781(7) 0.6249(6) 0.040(3) Uani 1 1 d .
H25 H -0.0095 0.3876 0.6696 0.048 Uiso 1 1 calc R
C26 C -0.1206(8) 0.4330(7) 0.6079(7) 0.048(4) Uani 1 1 d .
H26A H -0.0950 0.4833 0.6114 0.072 Uiso 1 1 calc R
H26B H -0.1611 0.4275 0.6365 0.072 Uiso 1 1 calc R
H26C H -0.1567 0.4242 0.5648 0.072 Uiso 1 1 calc R
C27 C -0.0824(8) 0.2984(7) 0.6216(7) 0.052(4) Uani 1 1 d .
H27A H -0.0339 0.2646 0.6443 0.078 Uiso 1 1 calc R
H27B H -0.1032 0.2829 0.5778 0.078 Uiso 1 1 calc R
H27C H -0.1351 0.2974 0.6408 0.078 Uiso 1 1 calc R
C28 C 0.2764(8) 0.4594(7) 0.5997(6) 0.036(3) Uani 1 1 d .
H28 H 0.2915 0.4540 0.6462 0.044 Uiso 1 1 calc R
C29 C 0.3509(8) 0.4175(7) 0.5783(6) 0.047(4) Uani 1 1 d .
H29A H 0.3399 0.3642 0.5803 0.070 Uiso 1 1 calc R
H29B H 0.4120 0.4297 0.6055 0.070 Uiso 1 1 calc R
H29C H 0.3491 0.4314 0.5351 0.070 Uiso 1 1 calc R
C30 C 0.2802(9) 0.5431(7) 0.5864(6) 0.049(4) Uani 1 1 d .
H30A H 0.2348 0.5692 0.6040 0.073 Uiso 1 1 calc R
H30B H 0.2656 0.5514 0.5411 0.073 Uiso 1 1 calc R
H30C H 0.3427 0.5619 0.6058 0.073 Uiso 1 1 calc R
C31 C 0.4796(7) 0.1620(6) 0.7386(5) 0.020(3) Uani 1 1 d .
C32 C 0.4359(7) 0.0933(6) 0.7445(5) 0.021(3) Uani 1 1 d .
C33 C 0.4850(8) 0.0273(6) 0.7475(5) 0.029(3) Uani 1 1 d .
H33 H 0.4546 -0.0180 0.7514 0.035 Uiso 1 1 calc R
C34 C 0.5774(8) 0.0259(7) 0.7451(5) 0.027(3) Uani 1 1 d .
H34 H 0.6101 -0.0195 0.7469 0.033 Uiso 1 1 calc R
C35 C 0.6202(8) 0.0925(6) 0.7400(5) 0.031(3) Uani 1 1 d .
H35 H 0.6836 0.0929 0.7388 0.037 Uiso 1 1 calc R
C36 C 0.5728(7) 0.1586(6) 0.7367(5) 0.027(3) Uani 1 1 d .
C37 C 0.6255(7) 0.2311(6) 0.7328(6) 0.025(3) Uani 1 1 d .
C38 C 0.6738(7) 0.2672(6) 0.7890(6) 0.030(3) Uani 1 1 d .
C39 C 0.7134(7) 0.3349(6) 0.7844(6) 0.031(3) Uani 1 1 d .
H39 H 0.7446 0.3599 0.8216 0.037 Uiso 1 1 calc R
C40 C 0.7094(7) 0.3681(7) 0.7270(6) 0.034(3) Uani 1 1 d .
H40 H 0.7356 0.4157 0.7251 0.041 Uiso 1 1 calc R
C41 C 0.6668(7) 0.3307(6) 0.6727(6) 0.029(3) Uani 1 1 d .
H41 H 0.6658 0.3522 0.6332 0.035 Uiso 1 1 calc R
C42 C 0.6257(7) 0.2625(6) 0.6751(5) 0.025(3) Uani 1 1 d .
C43 C 0.6812(8) 0.2312(6) 0.8530(5) 0.030(3) Uani 1 1 d .
H43A H 0.6610 0.1784 0.8462 0.036 Uiso 1 1 calc R
C44 C 0.7801(8) 0.2327(7) 0.8925(6) 0.040(3) Uani 1 1 d .
H44A H 0.7841 0.2056 0.9316 0.061 Uiso 1 1 calc R
H44B H 0.7995 0.2841 0.9022 0.061 Uiso 1 1 calc R
H44C H 0.8209 0.2094 0.8695 0.061 Uiso 1 1 calc R
C45 C 0.6171(9) 0.2705(7) 0.8871(6) 0.047(4) Uani 1 1 d .
H45A H 0.5522 0.2633 0.8638 0.071 Uiso 1 1 calc R
H45B H 0.6315 0.3235 0.8900 0.071 Uiso 1 1 calc R
H45C H 0.6265 0.2499 0.9293 0.071 Uiso 1 1 calc R
C46 C 0.5855(7) 0.2206(7) 0.6129(5) 0.029(3) Uani 1 1 d .
H46 H 0.5529 0.1754 0.6225 0.035 Uiso 1 1 calc R
C47 C 0.6638(9) 0.1958(8) 0.5846(6) 0.053(4) Uani 1 1 d .
H47A H 0.7091 0.1669 0.6156 0.080 Uiso 1 1 calc R
H47B H 0.6946 0.2394 0.5726 0.080 Uiso 1 1 calc R
H47C H 0.6384 0.1653 0.5476 0.080 Uiso 1 1 calc R
C48 C 0.5159(9) 0.2663(8) 0.5653(6) 0.060(4) Uani 1 1 d .
H48A H 0.4896 0.2360 0.5282 0.090 Uiso 1 1 calc R
H48B H 0.5474 0.3094 0.5532 0.090 Uiso 1 1 calc R
H48C H 0.4660 0.2829 0.5838 0.090 Uiso 1 1 calc R
C49 C 0.3352(7) 0.0866(6) 0.7485(5) 0.024(3) Uani 1 1 d .
C50 C 0.3179(8) 0.0866(6) 0.8098(6) 0.028(3) Uani 1 1 d .
C51 C 0.2299(7) 0.0731(6) 0.8157(6) 0.027(3) Uani 1 1 d .
H51 H 0.2181 0.0739 0.8560 0.032 Uiso 1 1 calc R
C52 C 0.1579(8) 0.0585(6) 0.7637(6) 0.034(3) Uani 1 1 d .
H52 H 0.0970 0.0498 0.7684 0.041 Uiso 1 1 calc R
C53 C 0.1754(8) 0.0567(6) 0.7028(6) 0.033(3) Uani 1 1 d .
H53 H 0.1268 0.0448 0.6670 0.040 Uiso 1 1 calc R
C54 C 0.2634(7) 0.0722(6) 0.6964(5) 0.021(3) Uani 1 1 d .
C55 C 0.3971(8) 0.0975(6) 0.8697(5) 0.031(3) Uani 1 1 d .
H55 H 0.4551 0.1093 0.8564 0.037 Uiso 1 1 calc R
C56 C 0.3768(9) 0.1621(7) 0.9076(6) 0.045(4) Uani 1 1 d .
H56A H 0.3720 0.2075 0.8827 0.067 Uiso 1 1 calc R
H56B H 0.4271 0.1673 0.9457 0.067 Uiso 1 1 calc R
H56C H 0.3180 0.1534 0.9189 0.067 Uiso 1 1 calc R
C57 C 0.4141(8) 0.0264(7) 0.9074(6) 0.039(3) Uani 1 1 d .
H57A H 0.4332 -0.0126 0.8825 0.059 Uiso 1 1 calc R
H57B H 0.3569 0.0115 0.9183 0.059 Uiso 1 1 calc R
H57C H 0.4633 0.0345 0.9457 0.059 Uiso 1 1 calc R
C58 C 0.2807(8) 0.0714(7) 0.6303(5) 0.031(3) Uani 1 1 d .
H58 H 0.3395 0.0992 0.6321 0.038 Uiso 1 1 calc R
C59 C 0.2026(9) 0.1091(7) 0.5820(6) 0.049(4) Uani 1 1 d .
H59A H 0.2153 0.1061 0.5406 0.074 Uiso 1 1 calc R
H59B H 0.1986 0.1612 0.5935 0.074 Uiso 1 1 calc R
H59C H 0.1436 0.0843 0.5809 0.074 Uiso 1 1 calc R
C60 C 0.2940(8) -0.0078(6) 0.6106(5) 0.037(3) Uani 1 1 d .
H60A H 0.3425 -0.0318 0.6430 0.055 Uiso 1 1 calc R
H60B H 0.3124 -0.0074 0.5710 0.055 Uiso 1 1 calc R
H60C H 0.2355 -0.0351 0.6052 0.055 Uiso 1 1 calc R
C61 C 0.0287(9) 0.5336(8) 1.0029(7) 0.056(4) Uani 1 1 d .
H61A H 0.0755 0.5316 1.0437 0.067 Uiso 1 1 calc R
H61B H -0.0118 0.5767 1.0041 0.067 Uiso 1 1 calc R
C62 C 0.0779(10) 0.5469(9) 0.9537(7) 0.067(5) Uani 1 1 d .
H62A H 0.0318 0.5466 0.9125 0.081 Uiso 1 1 calc R
H62B H 0.1214 0.5054 0.9539 0.081 Uiso 1 1 calc R
C63 C 0.1320(10) 0.6186(8) 0.9598(7) 0.063(4) Uani 1 1 d .
H63A H 0.1613 0.6231 0.9248 0.095 Uiso 1 1 calc R
H63B H 0.1800 0.6188 0.9994 0.095 Uiso 1 1 calc R
H63C H 0.0896 0.6604 0.9590 0.095 Uiso 1 1 calc R
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'
O O 0.0106 0.0060 '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
O3 Ge1 O1 110.5(4) .
O3 Ge1 O4 98.5(3) .
O1 Ge1 O4 110.3(4) .
O3 Ge1 C1 117.0(4) .
O1 Ge1 C1 111.3(4) .
O4 Ge1 C1 108.4(4) .
O3 Ge1 Ge2 34.6(2) .
O1 Ge1 Ge2 119.7(2) .
O4 Ge1 Ge2 64.0(2) .
C1 Ge1 Ge2 127.9(3) .
O3 Ge2 O2 101.6(4) .
O3 Ge2 O5 98.8(4) .
O2 Ge2 O5 110.7(4) .
O3 Ge2 C31 122.0(4) .
O2 Ge2 C31 118.1(4) .
O5 Ge2 C31 103.9(4) .
O3 Ge2 Ge1 34.6(2) .
O2 Ge2 Ge1 102.0(2) .
O5 Ge2 Ge1 66.1(2) .
C31 Ge2 Ge1 139.0(3) .
Ge2 O2 H2 108.4 .
Ge2 O3 Ge1 110.8(4) .
O5 O4 Ge1 109.5(5) .
O4 O5 Ge2 104.8(5) .
C6 C1 C2 119.3(10) .
C6 C1 Ge1 121.6(9) .
C2 C1 Ge1 119.2(8) .
C3 C2 C1 118.4(11) .
C3 C2 C19 116.8(10) .
C1 C2 C19 124.4(10) .
C4 C3 C2 121.9(11) .
C4 C3 H3 119.0 .
C2 C3 H3 119.0 .
C3 C4 C5 119.7(11) .
C3 C4 H4 120.1 .
C5 C4 H4 120.1 .
C4 C5 C6 121.5(11) .
C4 C5 H5 119.3 .
C6 C5 H5 119.3 .
C5 C6 C1 119.0(11) .
C5 C6 C7 119.0(10) .
C1 C6 C7 122.0(10) .
C8 C7 C12 123.1(11) .
C8 C7 C6 120.0(10) .
C12 C7 C6 116.5(11) .
C7 C8 C9 118.1(11) .
C7 C8 C16 123.0(10) .
C9 C8 C16 118.9(11) .
C10 C9 C8 120.2(13) .
C10 C9 H9 119.9 .
C8 C9 H9 119.9 .
C11 C10 C9 120.6(12) .
C11 C10 H10 119.7 .
C9 C10 H10 119.7 .
C10 C11 C12 121.7(12) .
C10 C11 H11 119.2 .
C12 C11 H11 119.2 .
C11 C12 C7 116.3(12) .
C11 C12 C13 119.8(11) .
C7 C12 C13 123.4(11) .
C12 C13 C14 112.4(10) .
C12 C13 C15 113.3(11) .
C14 C13 C15 110.3(9) .
C12 C13 H13 106.8 .
C14 C13 H13 106.8 .
C15 C13 H13 106.8 .
C13 C14 H14A 109.5 .
C13 C14 H14B 109.5 .
H14A C14 H14B 109.5 .
C13 C14 H14C 109.5 .
H14A C14 H14C 109.5 .
H14B C14 H14C 109.5 .
C13 C15 H15A 109.5 .
C13 C15 H15B 109.5 .
H15A C15 H15B 109.5 .
C13 C15 H15C 109.5 .
H15A C15 H15C 109.5 .
H15B C15 H15C 109.5 .
C8 C16 C18 111.6(10) .
C8 C16 C17 112.7(10) .
C18 C16 C17 108.3(10) .
C8 C16 H16 108.0 .
C18 C16 H16 108.0 .
C17 C16 H16 108.0 .
C16 C17 H17A 109.5 .
C16 C17 H17B 109.5 .
H17A C17 H17B 109.5 .
C16 C17 H17C 109.5 .
H17A C17 H17C 109.5 .
H17B C17 H17C 109.5 .
C16 C18 H18A 109.5 .
C16 C18 H18B 109.5 .
H18A C18 H18B 109.5 .
C16 C18 H18C 109.5 .
H18A C18 H18C 109.5 .
H18B C18 H18C 109.5 .
C24 C19 C20 122.5(11) .
C24 C19 C2 121.1(10) .
C20 C19 C2 116.4(11) .
C21 C20 C19 115.6(11) .
C21 C20 C25 120.4(11) .
C19 C20 C25 123.8(11) .
C22 C21 C20 122.7(12) .
C22 C21 H21 118.6 .
C20 C21 H21 118.6 .
C21 C22 C23 120.6(12) .
C21 C22 H22 119.7 .
C23 C22 H22 119.7 .
C22 C23 C24 119.6(13) .
C22 C23 H23 120.2 .
C24 C23 H23 120.2 .
C19 C24 C23 118.9(12) .
C19 C24 C28 123.5(11) .
C23 C24 C28 117.6(12) .
C20 C25 C26 112.5(11) .
C20 C25 C27 113.1(10) .
C26 C25 C27 110.0(10) .
C20 C25 H25 107.0 .
C26 C25 H25 107.0 .
C27 C25 H25 107.0 .
C25 C26 H26A 109.5 .
C25 C26 H26B 109.5 .
H26A C26 H26B 109.5 .
C25 C26 H26C 109.5 .
H26A C26 H26C 109.5 .
H26B C26 H26C 109.5 .
C25 C27 H27A 109.5 .
C25 C27 H27B 109.5 .
H27A C27 H27B 109.5 .
C25 C27 H27C 109.5 .
H27A C27 H27C 109.5 .
H27B C27 H27C 109.5 .
C29 C28 C24 114.1(10) .
C29 C28 C30 111.5(10) .
C24 C28 C30 111.7(10) .
C29 C28 H28 106.3 .
C24 C28 H28 106.3 .
C30 C28 H28 106.3 .
C28 C29 H29A 109.5 .
C28 C29 H29B 109.5 .
H29A C29 H29B 109.5 .
C28 C29 H29C 109.5 .
H29A C29 H29C 109.5 .
H29B C29 H29C 109.5 .
C28 C30 H30A 109.5 .
C28 C30 H30B 109.5 .
H30A C30 H30B 109.5 .
C28 C30 H30C 109.5 .
H30A C30 H30C 109.5 .
H30B C30 H30C 109.5 .
C36 C31 C32 116.3(10) .
C36 C31 Ge2 124.0(8) .
C32 C31 Ge2 119.5(8) .
C33 C32 C31 120.4(10) .
C33 C32 C49 116.1(10) .
C31 C32 C49 123.5(9) .
C34 C33 C32 121.8(11) .
C34 C33 H33 119.1 .
C32 C33 H33 119.1 .
C35 C34 C33 117.9(11) .
C35 C34 H34 121.0 .
C33 C34 H34 121.0 .
C36 C35 C34 121.3(10) .
C36 C35 H35 119.3 .
C34 C35 H35 119.3 .
C35 C36 C31 122.2(11) .
C35 C36 C37 118.6(9) .
C31 C36 C37 119.1(10) .
C42 C37 C38 119.5(10) .
C42 C37 C36 120.9(10) .
C38 C37 C36 119.6(10) .
C39 C38 C37 118.3(11) .
C39 C38 C43 121.0(11) .
C37 C38 C43 120.7(10) .
C38 C39 C40 122.1(12) .
C38 C39 H39 118.9 .
C40 C39 H39 118.9 .
C41 C40 C39 119.1(11) .
C41 C40 H40 120.5 .
C39 C40 H40 120.5 .
C40 C41 C42 120.7(11) .
C40 C41 H41 119.6 .
C42 C41 H41 119.6 .
C41 C42 C37 120.0(11) .
C41 C42 C46 118.4(10) .
C37 C42 C46 121.5(10) .
C44 C43 C45 110.2(10) .
C44 C43 C38 110.9(9) .
C45 C43 C38 110.3(9) .
C44 C43 H43A 108.4 .
C45 C43 H43A 108.4 .
C38 C43 H43A 108.4 .
C43 C44 H44A 109.5 .
C43 C44 H44B 109.5 .
H44A C44 H44B 109.5 .
C43 C44 H44C 109.5 .
H44A C44 H44C 109.5 .
H44B C44 H44C 109.5 .
C43 C45 H45A 109.5 .
C43 C45 H45B 109.5 .
H45A C45 H45B 109.5 .
C43 C45 H45C 109.5 .
H45A C45 H45C 109.5 .
H45B C45 H45C 109.5 .
C48 C46 C47 109.5(10) .
C48 C46 C42 113.0(10) .
C47 C46 C42 110.0(9) .
C48 C46 H46 108.0 .
C47 C46 H46 108.0 .
C42 C46 H46 108.0 .
C46 C47 H47A 109.5 .
C46 C47 H47B 109.5 .
H47A C47 H47B 109.5 .
C46 C47 H47C 109.5 .
H47A C47 H47C 109.5 .
H47B C47 H47C 109.5 .
C46 C48 H48A 109.5 .
C46 C48 H48B 109.5 .
H48A C48 H48B 109.5 .
C46 C48 H48C 109.5 .
H48A C48 H48C 109.5 .
H48B C48 H48C 109.5 .
C54 C49 C50 119.8(10) .
C54 C49 C32 122.0(10) .
C50 C49 C32 117.7(10) .
C51 C50 C49 119.4(11) .
C51 C50 C55 118.8(11) .
C49 C50 C55 121.7(10) .
C50 C51 C52 120.9(11) .
C50 C51 H51 119.5 .
C52 C51 H51 119.5 .
C51 C52 C53 119.8(10) .
C51 C52 H52 120.1 .
C53 C52 H52 120.1 .
C54 C53 C52 119.5(11) .
C54 C53 H53 120.3 .
C52 C53 H53 120.3 .
C53 C54 C49 120.5(10) .
C53 C54 C58 118.9(10) .
C49 C54 C58 120.6(9) .
C56 C55 C57 112.3(10) .
C56 C55 C50 110.9(9) .
C57 C55 C50 110.3(9) .
C56 C55 H55 107.7 .
C57 C55 H55 107.7 .
C50 C55 H55 107.7 .
C55 C56 H56A 109.5 .
C55 C56 H56B 109.5 .
H56A C56 H56B 109.5 .
C55 C56 H56C 109.5 .
H56A C56 H56C 109.5 .
H56B C56 H56C 109.5 .
C55 C57 H57A 109.5 .
C55 C57 H57B 109.5 .
H57A C57 H57B 109.5 .
C55 C57 H57C 109.5 .
H57A C57 H57C 109.5 .
H57B C57 H57C 109.5 .
C59 C58 C60 110.6(10) .
C59 C58 C54 112.1(10) .
C60 C58 C54 110.0(9) .
C59 C58 H58 108.0 .
C60 C58 H58 108.0 .
C54 C58 H58 108.0 .
C58 C59 H59A 109.5 .
C58 C59 H59B 109.5 .
H59A C59 H59B 109.5 .
C58 C59 H59C 109.5 .
H59A C59 H59C 109.5 .
H59B C59 H59C 109.5 .
C58 C60 H60A 109.5 .
C58 C60 H60B 109.5 .
H60A C60 H60B 109.5 .
C58 C60 H60C 109.5 .
H60A C60 H60C 109.5 .
H60B C60 H60C 109.5 .
C61 C61 C62 117.1(16) 3_567
C61 C61 H61A 108.0 3_567
C62 C61 H61A 108.0 .
C61 C61 H61B 108.0 3_567
C62 C61 H61B 108.0 .
H61A C61 H61B 107.3 .
C61 C62 C63 115.2(14) .
C61 C62 H62A 108.5 .
C63 C62 H62A 108.5 .
C61 C62 H62B 108.5 .
C63 C62 H62B 108.5 .
H62A C62 H62B 107.5 .
C62 C63 H63A 109.5 .
C62 C63 H63B 109.5 .
H63A C63 H63B 109.5 .
C62 C63 H63C 109.5 .
H63A C63 H63C 109.5 .
H63B C63 H63C 109.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ge1 O3 1.754(7) .
Ge1 O1 1.759(7) .
Ge1 O4 1.822(7) .
Ge1 C1 1.925(11) .
Ge1 Ge2 2.8849(19) .
Ge2 O3 1.750(7) .
Ge2 O2 1.755(7) .
Ge2 O5 1.836(8) .
Ge2 C31 1.932(11) .
O2 H2 1.0045 .
O4 O5 1.501(10) .
C1 C6 1.419(15) .
C1 C2 1.438(16) .
C2 C3 1.397(15) .
C2 C19 1.508(16) .
C3 C4 1.371(15) .
C3 H3 0.9500 .
C4 C5 1.391(15) .
C4 H4 0.9500 .
C5 C6 1.393(15) .
C5 H5 0.9500 .
C6 C7 1.520(16) .
C7 C8 1.386(16) .
C7 C12 1.412(15) .
C8 C9 1.400(16) .
C8 C16 1.503(16) .
C9 C10 1.399(17) .
C9 H9 0.9500 .
C10 C11 1.366(17) .
C10 H10 0.9500 .
C11 C12 1.410(17) .
C11 H11 0.9500 .
C12 C13 1.489(16) .
C13 C14 1.500(15) .
C13 C15 1.576(16) .
C13 H13 1.0000 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 C18 1.555(17) .
C16 C17 1.561(15) .
C16 H16 1.0000 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C19 C24 1.379(16) .
C19 C20 1.432(16) .
C20 C21 1.381(17) .
C20 C25 1.491(16) .
C21 C22 1.376(17) .
C21 H21 0.9500 .
C22 C23 1.377(18) .
C22 H22 0.9500 .
C23 C24 1.399(16) .
C23 H23 0.9500 .
C24 C28 1.517(16) .
C25 C26 1.498(16) .
C25 C27 1.551(16) .
C25 H25 1.0000 .
C26 H26A 0.9800 .
C26 H26B 0.9800 .
C26 H26C 0.9800 .
C27 H27A 0.9800 .
C27 H27B 0.9800 .
C27 H27C 0.9800 .
C28 C29 1.513(16) .
C28 C30 1.543(17) .
C28 H28 1.0000 .
C29 H29A 0.9800 .
C29 H29B 0.9800 .
C29 H29C 0.9800 .
C30 H30A 0.9800 .
C30 H30B 0.9800 .
C30 H30C 0.9800 .
C31 C36 1.399(14) .
C31 C32 1.423(14) .
C32 C33 1.390(14) .
C32 C49 1.526(14) .
C33 C34 1.387(15) .
C33 H33 0.9500 .
C34 C35 1.380(15) .
C34 H34 0.9500 .
C35 C36 1.378(15) .
C35 H35 0.9500 .
C36 C37 1.540(14) .
C37 C42 1.395(15) .
C37 C38 1.425(16) .
C38 C39 1.372(15) .
C38 C43 1.535(15) .
C39 C40 1.389(16) .
C39 H39 0.9500 .
C40 C41 1.382(16) .
C40 H40 0.9500 .
C41 C42 1.384(15) .
C41 H41 0.9500 .
C42 C46 1.550(15) .
C43 C44 1.508(15) .
C43 C45 1.529(16) .
C43 H43A 1.0000 .
C44 H44A 0.9800 .
C44 H44B 0.9800 .
C44 H44C 0.9800 .
C45 H45A 0.9800 .
C45 H45B 0.9800 .
C45 H45C 0.9800 .
C46 C48 1.518(17) .
C46 C47 1.521(15) .
C46 H46 1.0000 .
C47 H47A 0.9800 .
C47 H47B 0.9800 .
C47 H47C 0.9800 .
C48 H48A 0.9800 .
C48 H48B 0.9800 .
C48 H48C 0.9800 .
C49 C54 1.382(15) .
C49 C50 1.440(15) .
C50 C51 1.369(15) .
C50 C55 1.545(16) .
C51 C52 1.383(16) .
C51 H51 0.9500 .
C52 C53 1.435(16) .
C52 H52 0.9500 .
C53 C54 1.379(15) .
C53 H53 0.9500 .
C54 C58 1.547(14) .
C55 C56 1.511(15) .
C55 C57 1.516(15) .
C55 H55 1.0000 .
C56 H56A 0.9800 .
C56 H56B 0.9800 .
C56 H56C 0.9800 .
C57 H57A 0.9800 .
C57 H57B 0.9800 .
C57 H57C 0.9800 .
C58 C59 1.524(16) .
C58 C60 1.522(16) .
C58 H58 1.0000 .
C59 H59A 0.9800 .
C59 H59B 0.9800 .
C59 H59C 0.9800 .
C60 H60A 0.9800 .
C60 H60B 0.9800 .
C60 H60C 0.9800 .
C61 C61 1.47(3) 3_567
C61 C62 1.476(18) .
C61 H61A 0.9900 .
C61 H61B 0.9900 .
C62 C63 1.512(19) .
C62 H62A 0.9900 .
C62 H62B 0.9900 .
C63 H63A 0.9800 .
C63 H63B 0.9800 .
C63 H63C 0.9800 .
