#------------------------------------------------------------------------------
#$Date: 2024-10-06 09:23:16 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295151 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/36/7133645.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_7133645
loop_
_publ_author_name
'Liu, Chenghuan'
'Schmidtmann, Marc'
'Müller, Thomas'
_publ_section_title
;
 Metal ion-driven formation of 2H-silolides and -germolides.
;
_journal_issue                   80
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11295
_journal_page_last               11298
_journal_paper_doi               10.1039/d4cc03984j
_journal_volume                  60
_journal_year                    2024
_chemical_formula_structural     K(C12H24O6)[GeC4(CH3)2(Si(CH3)3)2Si(C15H23N2)]
_chemical_formula_sum            'C39 H71 Ge K N2 O6 Si3'
_chemical_formula_weight         859.93
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-07-05 deposited with the CCDC.	2024-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                95.5876(14)
_cell_angle_beta                 95.5032(14)
_cell_angle_gamma                115.7735(12)
_cell_formula_units_Z            2
_cell_length_a                   12.4586(4)
_cell_length_b                   13.0885(4)
_cell_length_c                   17.1275(6)
_cell_measurement_reflns_used    9820
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.92
_cell_measurement_theta_min      2.42
_cell_volume                     2473.14(14)
_computing_cell_refinement       'Bruker SAINT V8.40B'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT V8.40B'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Photon III CPAD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            137762
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.034
_diffrn_reflns_theta_min         1.749
_diffrn_source                   'I\mS microfocus'
_exptl_absorpt_coefficient_mu    0.816
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9206
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Sheldrick)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         14466
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0500P)²+0.9000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1075
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12038
_reflns_number_total             14466
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4cc03984j3.cif
_cod_data_source_block           lch0826ge
_cod_depositor_comments
'Adding full bibliography for 7133645--7133649.cif.'
_cod_database_code               7133645
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.828
_shelx_estimated_absorpt_t_max   0.881
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.21904(2) 0.23466(2) 0.29512(2) 0.03718(5) Uani 1 1 d . . . . .
K1 K 0.04201(3) 0.37360(3) 0.33298(2) 0.04296(8) Uani 1 1 d . . . . .
Si1 Si 0.35626(5) 0.09846(5) 0.35084(3) 0.04570(11) Uani 1 1 d . . . . .
Si2 Si 0.15721(5) 0.00229(4) 0.19243(3) 0.04698(11) Uani 1 1 d . . . . .
Si3 Si 0.30941(4) 0.47361(4) 0.24681(3) 0.03440(9) Uani 1 1 d . . . . .
O1 O 0.16057(15) 0.4836(2) 0.48426(10) 0.0778(5) Uani 1 1 d . . . . .
O2 O 0.11146(14) 0.61479(14) 0.37914(10) 0.0661(4) Uani 1 1 d . . . . .
O3 O -0.02495(14) 0.50542(14) 0.23226(10) 0.0633(4) Uani 1 1 d . . . . .
O4 O -0.17935(15) 0.27370(15) 0.21549(10) 0.0704(4) Uani 1 1 d . . . . .
O5 O -0.13431(15) 0.13975(14) 0.31671(12) 0.0728(5) Uani 1 1 d . . . . .
O6 O 0.00097(16) 0.24798(19) 0.46795(11) 0.0761(5) Uani 1 1 d . . . . .
N1 N 0.46377(12) 0.59986(11) 0.24942(8) 0.0361(3) Uani 1 1 d . . . . .
N2 N 0.32915(12) 0.52734(12) 0.14720(8) 0.0375(3) Uani 1 1 d . . . . .
C1 C 0.32712(13) 0.34149(13) 0.24028(9) 0.0338(3) Uani 1 1 d . . . . .
C2 C 0.40229(14) 0.29903(13) 0.20266(9) 0.0350(3) Uani 1 1 d . . . . .
C3 C 0.38470(14) 0.19033(14) 0.21042(9) 0.0368(3) Uani 1 1 d . . . . .
C4 C 0.28829(14) 0.12327(13) 0.25753(9) 0.0358(3) Uani 1 1 d . . . . .
C5 C 0.49852(17) 0.37467(16) 0.15822(12) 0.0478(4) Uani 1 1 d . . . . .
H5A H 0.573551 0.420360 0.195272 0.072 Uiso 1 1 calc R U . . .
H5B H 0.471912 0.426070 0.133752 0.072 Uiso 1 1 calc R U . . .
H5C H 0.512455 0.326588 0.116831 0.072 Uiso 1 1 calc R U . . .
C6 C 0.46347(19) 0.14054(17) 0.17723(13) 0.0519(4) Uani 1 1 d . . . . .
H6A H 0.466067 0.149640 0.121219 0.078 Uiso 1 1 calc R U . . .
H6B H 0.429902 0.058771 0.181871 0.078 Uiso 1 1 calc R U . . .
H6C H 0.545316 0.181057 0.207164 0.078 Uiso 1 1 calc R U . . .
C7 C 0.2498(2) 0.0449(2) 0.42440(14) 0.0681(6) Uani 1 1 d . . . . .
H7A H 0.224806 0.103572 0.442327 0.102 Uiso 1 1 calc R U . . .
H7B H 0.290309 0.028773 0.470059 0.102 Uiso 1 1 calc R U . . .
H7C H 0.178619 -0.025527 0.399239 0.102 Uiso 1 1 calc R U . . .
C8 C 0.4873(3) 0.2357(2) 0.39902(17) 0.0846(8) Uani 1 1 d . . . . .
H8A H 0.545296 0.263346 0.362009 0.127 Uiso 1 1 calc R U . . .
H8B H 0.526247 0.222743 0.446925 0.127 Uiso 1 1 calc R U . . .
H8C H 0.459124 0.293225 0.413445 0.127 Uiso 1 1 calc R U . . .
C9 C 0.4172(3) -0.0105(2) 0.33722(18) 0.0764(7) Uani 1 1 d . . . . .
H9A H 0.352743 -0.083904 0.309463 0.115 Uiso 1 1 calc R U . . .
H9B H 0.447241 -0.021241 0.389285 0.115 Uiso 1 1 calc R U . . .
H9C H 0.483295 0.017031 0.305862 0.115 Uiso 1 1 calc R U . . .
C10 C 0.0271(2) -0.0741(2) 0.24588(17) 0.0699(6) Uani 1 1 d . . . . .
H10A H 0.051881 -0.109539 0.287283 0.105 Uiso 1 1 calc R U . . .
H10B H -0.040300 -0.133700 0.208077 0.105 Uiso 1 1 calc R U . . .
H10C H 0.001673 -0.018926 0.270199 0.105 Uiso 1 1 calc R U . . .
C11 C 0.1022(3) 0.0564(2) 0.10733(16) 0.0809(8) Uani 1 1 d . . . . .
H11A H 0.056402 0.096098 0.126129 0.121 Uiso 1 1 calc R U . . .
H11B H 0.050155 -0.008539 0.065950 0.121 Uiso 1 1 calc R U . . .
H11C H 0.171413 0.109825 0.085510 0.121 Uiso 1 1 calc R U . . .
C12 C 0.1915(3) -0.1143(2) 0.14422(17) 0.0747(7) Uani 1 1 d . . . . .
H12A H 0.249885 -0.082535 0.108026 0.112 Uiso 1 1 calc R U . . .
H12B H 0.116967 -0.176889 0.114348 0.112 Uiso 1 1 calc R U . . .
H12C H 0.225284 -0.143846 0.185315 0.112 Uiso 1 1 calc R U . . .
C13 C 0.43406(14) 0.61701(13) 0.17658(9) 0.0352(3) Uani 1 1 d . . . . .
C14 C 0.50187(16) 0.71662(14) 0.13623(10) 0.0394(3) Uani 1 1 d . . . . .
C15 C 0.46727(19) 0.80352(16) 0.13058(11) 0.0481(4) Uani 1 1 d . . . . .
H15 H 0.402483 0.803093 0.155860 0.058 Uiso 1 1 calc R U . . .
C16 C 0.5274(2) 0.89105(17) 0.08795(13) 0.0615(5) Uani 1 1 d . . . . .
H16 H 0.502930 0.949883 0.083699 0.074 Uiso 1 1 calc R U . . .
C17 C 0.6220(3) 0.89325(18) 0.05192(13) 0.0689(7) Uani 1 1 d . . . . .
H17 H 0.662099 0.952951 0.022372 0.083 Uiso 1 1 calc R U . . .
C18 C 0.6586(2) 0.8088(2) 0.05865(14) 0.0699(7) Uani 1 1 d . . . . .
H18 H 0.724932 0.811010 0.034403 0.084 Uiso 1 1 calc R U . . .
C19 C 0.5993(2) 0.72072(17) 0.10056(13) 0.0555(5) Uani 1 1 d . . . . .
H19 H 0.625026 0.662763 0.105047 0.067 Uiso 1 1 calc R U . . .
C20 C 0.25208(16) 0.49644(16) 0.06973(10) 0.0441(4) Uani 1 1 d . . . . .
C21 C 0.1699(3) 0.3687(2) 0.06191(15) 0.0789(8) Uani 1 1 d . . . . .
H21A H 0.218852 0.327210 0.066817 0.118 Uiso 1 1 calc R U . . .
H21B H 0.118410 0.341788 0.009948 0.118 Uiso 1 1 calc R U . . .
H21C H 0.119301 0.354462 0.103919 0.118 Uiso 1 1 calc R U . . .
C22 C 0.3265(2) 0.5180(3) 0.00162(12) 0.0674(6) Uani 1 1 d . . . . .
H22A H 0.370273 0.600791 0.001221 0.101 Uiso 1 1 calc R U . . .
H22B H 0.272628 0.480774 -0.048970 0.101 Uiso 1 1 calc R U . . .
H22C H 0.384246 0.486152 0.009002 0.101 Uiso 1 1 calc R U . . .
C23 C 0.1774(2) 0.5629(2) 0.06750(14) 0.0644(6) Uani 1 1 d . . . . .
H23A H 0.134989 0.552988 0.113599 0.097 Uiso 1 1 calc R U . . .
H23B H 0.118547 0.533728 0.018659 0.097 Uiso 1 1 calc R U . . .
H23C H 0.230819 0.644569 0.068804 0.097 Uiso 1 1 calc R U . . .
C24 C 0.55954(15) 0.67806(15) 0.31450(11) 0.0435(4) Uani 1 1 d . . . . .
C25 C 0.5475(2) 0.6095(2) 0.38330(12) 0.0602(5) Uani 1 1 d . . . . .
H25A H 0.467147 0.585548 0.398376 0.090 Uiso 1 1 calc R U . . .
H25B H 0.608955 0.657576 0.428814 0.090 Uiso 1 1 calc R U . . .
H25C H 0.558827 0.541455 0.366801 0.090 Uiso 1 1 calc R U . . .
C26 C 0.5412(2) 0.78371(17) 0.34023(13) 0.0574(5) Uani 1 1 d . . . . .
H26A H 0.554174 0.830442 0.297480 0.086 Uiso 1 1 calc R U . . .
H26B H 0.598835 0.829207 0.388006 0.086 Uiso 1 1 calc R U . . .
H26C H 0.458781 0.759241 0.351718 0.086 Uiso 1 1 calc R U . . .
C27 C 0.68493(19) 0.7149(2) 0.29129(15) 0.0665(6) Uani 1 1 d . . . . .
H27A H 0.695192 0.646619 0.273648 0.100 Uiso 1 1 calc R U . . .
H27B H 0.746280 0.761243 0.337256 0.100 Uiso 1 1 calc R U . . .
H27C H 0.693783 0.760466 0.248065 0.100 Uiso 1 1 calc R U . . .
C28 C 0.1842(2) 0.5981(3) 0.50832(17) 0.0890(10) Uani 1 1 d . . . . .
H28A H 0.252253 0.634335 0.552762 0.107 Uiso 1 1 calc R U . . .
H28B H 0.112307 0.600663 0.526730 0.107 Uiso 1 1 calc R U . . .
C29 C 0.2147(2) 0.6611(3) 0.4397(2) 0.0922(10) Uani 1 1 d . . . . .
H29A H 0.239784 0.743726 0.456775 0.111 Uiso 1 1 calc R U . . .
H29B H 0.282605 0.653335 0.418703 0.111 Uiso 1 1 calc R U . . .
C30 C 0.1328(3) 0.6692(2) 0.31155(19) 0.0771(7) Uani 1 1 d . . . . .
H30A H 0.192071 0.653239 0.284710 0.092 Uiso 1 1 calc R U . . .
H30B H 0.165920 0.753351 0.327003 0.092 Uiso 1 1 calc R U . . .
C31 C 0.0174(3) 0.6245(2) 0.25771(18) 0.0762(7) Uani 1 1 d . . . . .
H31A H -0.042575 0.637595 0.285578 0.091 Uiso 1 1 calc R U . . .
H31B H 0.028832 0.665379 0.211177 0.091 Uiso 1 1 calc R U . . .
C32 C -0.1365(3) 0.4577(3) 0.18392(19) 0.0881(9) Uani 1 1 d . . . . .
H32A H -0.133068 0.501856 0.139677 0.106 Uiso 1 1 calc R U . . .
H32B H -0.198691 0.460190 0.214913 0.106 Uiso 1 1 calc R U . . .
C33 C -0.1674(3) 0.3388(3) 0.15259(16) 0.0851(8) Uani 1 1 d . . . . .
H33A H -0.244214 0.304966 0.115190 0.102 Uiso 1 1 calc R U . . .
H33B H -0.103616 0.336586 0.123212 0.102 Uiso 1 1 calc R U . . .
C34 C -0.2082(3) 0.1599(3) 0.19018(19) 0.0879(8) Uani 1 1 d . . . . .
H34A H -0.139312 0.154525 0.169058 0.106 Uiso 1 1 calc R U . . .
H34B H -0.278470 0.126351 0.147181 0.106 Uiso 1 1 calc R U . . .
C35 C -0.2373(3) 0.0954(2) 0.2580(2) 0.0932(10) Uani 1 1 d . . . . .
H35A H -0.304423 0.102882 0.280266 0.112 Uiso 1 1 calc R U . . .
H35B H -0.262837 0.012941 0.239800 0.112 Uiso 1 1 calc R U . . .
C36 C -0.1536(3) 0.0839(3) 0.3840(2) 0.0865(9) Uani 1 1 d . . . . .
H36A H -0.185002 0.000151 0.367793 0.104 Uiso 1 1 calc R U . . .
H36B H -0.213858 0.097608 0.411281 0.104 Uiso 1 1 calc R U . . .
C37 C -0.0377(3) 0.1296(3) 0.43854(18) 0.0835(9) Uani 1 1 d . . . . .
H37A H -0.048014 0.085545 0.483411 0.100 Uiso 1 1 calc R U . . .
H37B H 0.024070 0.121131 0.409964 0.100 Uiso 1 1 calc R U . . .
C38 C 0.1127(3) 0.2971(4) 0.51720(17) 0.0922(10) Uani 1 1 d . . . . .
H38A H 0.175104 0.293631 0.486890 0.111 Uiso 1 1 calc R U . . .
H38B H 0.108513 0.253724 0.561967 0.111 Uiso 1 1 calc R U . . .
C39 C 0.1456(3) 0.4192(4) 0.54837(15) 0.0964(12) Uani 1 1 d . . . . .
H39A H 0.081384 0.422871 0.576591 0.116 Uiso 1 1 calc R U . . .
H39B H 0.221581 0.452381 0.586541 0.116 Uiso 1 1 calc R U . . .
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'
Si Si 0.0817 0.0704 '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'
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
C1 Ge1 C4 87.46(6) . . ?
C1 Ge1 K1 98.50(5) . . ?
C4 Ge1 K1 166.95(5) . . ?
O1 K1 O5 117.42(6) . . ?
O1 K1 O3 116.56(6) . . ?
O5 K1 O3 113.68(5) . . ?
O1 K1 O2 59.41(6) . . ?
O5 K1 O2 149.54(5) . . ?
O3 K1 O2 57.38(5) . . ?
O1 K1 O6 59.28(6) . . ?
O5 K1 O6 58.34(6) . . ?
O3 K1 O6 148.98(5) . . ?
O2 K1 O6 112.43(6) . . ?
O1 K1 O4 149.60(5) . . ?
O5 K1 O4 57.02(5) . . ?
O3 K1 O4 56.81(5) . . ?
O2 K1 O4 108.75(5) . . ?
O6 K1 O4 109.50(5) . . ?
O1 K1 Ge1 96.92(4) . . ?
O5 K1 Ge1 79.68(4) . . ?
O3 K1 Ge1 127.39(4) . . ?
O2 K1 Ge1 129.97(3) . . ?
O6 K1 Ge1 82.55(3) . . ?
O4 K1 Ge1 110.05(4) . . ?
O1 K1 Si3 94.02(4) . . ?
O5 K1 Si3 125.46(4) . . ?
O3 K1 Si3 84.89(3) . . ?
O2 K1 Si3 84.35(3) . . ?
O6 K1 Si3 125.03(3) . . ?
O4 K1 Si3 113.47(4) . . ?
Ge1 K1 Si3 51.650(9) . . ?
C4 Si1 C8 108.78(10) . . ?
C4 Si1 C7 114.34(9) . . ?
C8 Si1 C7 108.45(14) . . ?
C4 Si1 C9 114.95(11) . . ?
C8 Si1 C9 105.88(14) . . ?
C7 Si1 C9 103.95(11) . . ?
C4 Si2 C10 113.35(10) . . ?
C4 Si2 C11 110.12(10) . . ?
C10 Si2 C11 108.22(14) . . ?
C4 Si2 C12 114.69(10) . . ?
C10 Si2 C12 105.07(12) . . ?
C11 Si2 C12 104.83(14) . . ?
C1 Si3 N2 108.29(7) . . ?
C1 Si3 N1 108.46(6) . . ?
N2 Si3 N1 67.69(6) . . ?
C1 Si3 C13 116.21(6) . . ?
N2 Si3 C13 33.94(6) . . ?
N1 Si3 C13 34.15(6) . . ?
C1 Si3 K1 97.53(5) . . ?
N2 Si3 K1 126.38(4) . . ?
N1 Si3 K1 144.69(4) . . ?
C13 Si3 K1 144.35(4) . . ?
C28 O1 C39 113.1(2) . . ?
C28 O1 K1 120.02(16) . . ?
C39 O1 K1 119.81(19) . . ?
C30 O2 C29 112.9(2) . . ?
C30 O2 K1 108.79(14) . . ?
C29 O2 K1 108.40(17) . . ?
C32 O3 C31 111.8(2) . . ?
C32 O3 K1 121.23(15) . . ?
C31 O3 K1 119.16(15) . . ?
C34 O4 C33 113.4(2) . . ?
C34 O4 K1 108.48(16) . . ?
C33 O4 K1 111.46(14) . . ?
C35 O5 C36 113.2(2) . . ?
C35 O5 K1 120.68(15) . . ?
C36 O5 K1 119.59(18) . . ?
C38 O6 C37 112.2(2) . . ?
C38 O6 K1 104.77(16) . . ?
C37 O6 K1 108.02(14) . . ?
C13 N1 C24 130.26(14) . . ?
C13 N1 Si3 92.54(10) . . ?
C24 N1 Si3 133.29(11) . . ?
C13 N2 C20 131.51(14) . . ?
C13 N2 Si3 92.85(10) . . ?
C20 N2 Si3 134.95(11) . . ?
C2 C1 Si3 135.95(11) . . ?
C2 C1 Ge1 112.74(10) . . ?
Si3 C1 Ge1 111.30(7) . . ?
C3 C2 C1 117.70(13) . . ?
C3 C2 C5 121.76(14) . . ?
C1 C2 C5 120.52(14) . . ?
C2 C3 C4 117.45(13) . . ?
C2 C3 C6 121.67(14) . . ?
C4 C3 C6 120.78(14) . . ?
C3 C4 Si1 110.72(11) . . ?
C3 C4 Si2 111.47(11) . . ?
Si1 C4 Si2 120.25(8) . . ?
C3 C4 Ge1 104.64(10) . . ?
Si1 C4 Ge1 104.42(7) . . ?
Si2 C4 Ge1 103.61(7) . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si1 C7 H7A 109.5 . . ?
Si1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si1 C8 H8A 109.5 . . ?
Si1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si1 C9 H9A 109.5 . . ?
Si1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si2 C10 H10A 109.5 . . ?
Si2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si2 C11 H11A 109.5 . . ?
Si2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si2 C12 H12A 109.5 . . ?
Si2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C13 N1 105.74(13) . . ?
N2 C13 C14 126.43(14) . . ?
N1 C13 C14 127.81(15) . . ?
N2 C13 Si3 53.21(8) . . ?
N1 C13 Si3 53.31(8) . . ?
C14 C13 Si3 171.31(11) . . ?
C15 C14 C19 119.03(16) . . ?
C15 C14 C13 121.47(15) . . ?
C19 C14 C13 119.45(15) . . ?
C16 C15 C14 119.96(19) . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C17 C16 C15 120.5(2) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
C16 C17 C18 119.92(19) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C17 C18 C19 120.2(2) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C18 C19 C14 120.3(2) . . ?
C18 C19 H19 119.9 . . ?
C14 C19 H19 119.9 . . ?
N2 C20 C21 105.47(15) . . ?
N2 C20 C23 110.38(15) . . ?
C21 C20 C23 110.1(2) . . ?
N2 C20 C22 111.52(15) . . ?
C21 C20 C22 108.9(2) . . ?
C23 C20 C22 110.30(17) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N1 C24 C27 111.76(16) . . ?
N1 C24 C26 110.74(15) . . ?
C27 C24 C26 110.02(18) . . ?
N1 C24 C25 105.69(14) . . ?
C27 C24 C25 109.15(17) . . ?
C26 C24 C25 109.36(17) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O1 C28 C29 108.6(2) . . ?
O1 C28 H28A 110.0 . . ?
C29 C28 H28A 110.0 . . ?
O1 C28 H28B 110.0 . . ?
C29 C28 H28B 110.0 . . ?
H28A C28 H28B 108.4 . . ?
O2 C29 C28 109.2(2) . . ?
O2 C29 H29A 109.8 . . ?
C28 C29 H29A 109.8 . . ?
O2 C29 H29B 109.8 . . ?
C28 C29 H29B 109.8 . . ?
H29A C29 H29B 108.3 . . ?
O2 C30 C31 108.1(2) . . ?
O2 C30 H30A 110.1 . . ?
C31 C30 H30A 110.1 . . ?
O2 C30 H30B 110.1 . . ?
C31 C30 H30B 110.1 . . ?
H30A C30 H30B 108.4 . . ?
O3 C31 C30 109.4(2) . . ?
O3 C31 H31A 109.8 . . ?
C30 C31 H31A 109.8 . . ?
O3 C31 H31B 109.8 . . ?
C30 C31 H31B 109.8 . . ?
H31A C31 H31B 108.2 . . ?
O3 C32 C33 108.6(2) . . ?
O3 C32 H32A 110.0 . . ?
C33 C32 H32A 110.0 . . ?
O3 C32 H32B 110.0 . . ?
C33 C32 H32B 110.0 . . ?
H32A C32 H32B 108.4 . . ?
O4 C33 C32 110.1(2) . . ?
O4 C33 H33A 109.6 . . ?
C32 C33 H33A 109.6 . . ?
O4 C33 H33B 109.6 . . ?
C32 C33 H33B 109.6 . . ?
H33A C33 H33B 108.1 . . ?
O4 C34 C35 109.2(3) . . ?
O4 C34 H34A 109.8 . . ?
C35 C34 H34A 109.8 . . ?
O4 C34 H34B 109.8 . . ?
C35 C34 H34B 109.8 . . ?
H34A C34 H34B 108.3 . . ?
O5 C35 C34 109.2(2) . . ?
O5 C35 H35A 109.8 . . ?
C34 C35 H35A 109.8 . . ?
O5 C35 H35B 109.8 . . ?
C34 C35 H35B 109.8 . . ?
H35A C35 H35B 108.3 . . ?
O5 C36 C37 108.86(19) . . ?
O5 C36 H36A 109.9 . . ?
C37 C36 H36A 109.9 . . ?
O5 C36 H36B 109.9 . . ?
C37 C36 H36B 109.9 . . ?
H36A C36 H36B 108.3 . . ?
O6 C37 C36 109.6(2) . . ?
O6 C37 H37A 109.7 . . ?
C36 C37 H37A 109.7 . . ?
O6 C37 H37B 109.7 . . ?
C36 C37 H37B 109.7 . . ?
H37A C37 H37B 108.2 . . ?
O6 C38 C39 109.6(2) . . ?
O6 C38 H38A 109.8 . . ?
C39 C38 H38A 109.8 . . ?
O6 C38 H38B 109.8 . . ?
C39 C38 H38B 109.8 . . ?
H38A C38 H38B 108.2 . . ?
O1 C39 C38 109.7(2) . . ?
O1 C39 H39A 109.7 . . ?
C38 C39 H39A 109.7 . . ?
O1 C39 H39B 109.7 . . ?
C38 C39 H39B 109.7 . . ?
H39A C39 H39B 108.2 . . ?
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 C1 1.8739(14) . ?
Ge1 C4 2.0741(15) . ?
Ge1 K1 3.4820(4) . ?
K1 O1 2.7675(17) . ?
K1 O5 2.8532(17) . ?
K1 O3 2.8644(15) . ?
K1 O2 2.8891(17) . ?
K1 O6 2.9231(16) . ?
K1 O4 2.9414(16) . ?
K1 Si3 3.5379(5) . ?
Si1 C4 1.8594(17) . ?
Si1 C8 1.864(3) . ?
Si1 C7 1.877(2) . ?
Si1 C9 1.892(2) . ?
Si2 C4 1.8643(17) . ?
Si2 C10 1.876(2) . ?
Si2 C11 1.878(2) . ?
Si2 C12 1.892(2) . ?
Si3 C1 1.8304(15) . ?
Si3 N2 1.9050(13) . ?
Si3 N1 1.9070(14) . ?
Si3 C13 2.3757(15) . ?
O1 C28 1.405(4) . ?
O1 C39 1.427(4) . ?
O2 C30 1.405(3) . ?
O2 C29 1.429(3) . ?
O3 C32 1.390(3) . ?
O3 C31 1.416(3) . ?
O4 C34 1.384(3) . ?
O4 C33 1.417(3) . ?
O5 C35 1.409(3) . ?
O5 C36 1.409(3) . ?
O6 C38 1.398(3) . ?
O6 C37 1.428(4) . ?
N1 C13 1.335(2) . ?
N1 C24 1.475(2) . ?
N2 C13 1.328(2) . ?
N2 C20 1.470(2) . ?
C1 C2 1.449(2) . ?
C2 C3 1.364(2) . ?
C2 C5 1.512(2) . ?
C3 C4 1.507(2) . ?
C3 C6 1.517(2) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.490(2) . ?
C14 C15 1.389(2) . ?
C14 C19 1.393(2) . ?
C15 C16 1.389(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.372(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.378(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.383(3) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.518(3) . ?
C20 C23 1.525(3) . ?
C20 C22 1.531(3) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C27 1.527(3) . ?
C24 C26 1.528(3) . ?
C24 C25 1.529(3) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
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 1.486(5) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.473(4) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.461(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.482(4) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.482(4) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.492(5) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Si3 C1 C2 37.03(19) . . . . ?
N1 Si3 C1 C2 -34.85(19) . . . . ?
C13 Si3 C1 C2 1.2(2) . . . . ?
K1 Si3 C1 C2 169.39(16) . . . . ?
N2 Si3 C1 Ge1 -141.97(7) . . . . ?
N1 Si3 C1 Ge1 146.15(7) . . . . ?
C13 Si3 C1 Ge1 -177.76(7) . . . . ?
K1 Si3 C1 Ge1 -9.61(8) . . . . ?
C4 Ge1 C1 C2 -1.12(12) . . . . ?
K1 Ge1 C1 C2 -169.46(11) . . . . ?
C4 Ge1 C1 Si3 178.12(9) . . . . ?
K1 Ge1 C1 Si3 9.79(8) . . . . ?
Si3 C1 C2 C3 -178.05(14) . . . . ?
Ge1 C1 C2 C3 0.93(19) . . . . ?
Si3 C1 C2 C5 3.4(3) . . . . ?
Ge1 C1 C2 C5 -177.65(13) . . . . ?
C1 C2 C3 C4 0.0(2) . . . . ?
C5 C2 C3 C4 178.60(16) . . . . ?
C1 C2 C3 C6 -176.49(16) . . . . ?
C5 C2 C3 C6 2.1(3) . . . . ?
C2 C3 C4 Si1 -112.81(15) . . . . ?
C6 C3 C4 Si1 63.74(19) . . . . ?
C2 C3 C4 Si2 110.51(15) . . . . ?
C6 C3 C4 Si2 -72.94(18) . . . . ?
C2 C3 C4 Ge1 -0.85(18) . . . . ?
C6 C3 C4 Ge1 175.70(14) . . . . ?
C8 Si1 C4 C3 45.88(16) . . . . ?
C7 Si1 C4 C3 167.25(13) . . . . ?
C9 Si1 C4 C3 -72.61(15) . . . . ?
C8 Si1 C4 Si2 178.23(14) . . . . ?
C7 Si1 C4 Si2 -60.41(14) . . . . ?
C9 Si1 C4 Si2 59.74(14) . . . . ?
C8 Si1 C4 Ge1 -66.22(14) . . . . ?
C7 Si1 C4 Ge1 55.15(12) . . . . ?
C9 Si1 C4 Ge1 175.29(10) . . . . ?
C10 Si2 C4 C3 -173.53(13) . . . . ?
C11 Si2 C4 C3 -52.14(16) . . . . ?
C12 Si2 C4 C3 65.80(15) . . . . ?
C10 Si2 C4 Si1 54.44(14) . . . . ?
C11 Si2 C4 Si1 175.83(13) . . . . ?
C12 Si2 C4 Si1 -66.23(14) . . . . ?
C10 Si2 C4 Ge1 -61.53(12) . . . . ?
C11 Si2 C4 Ge1 59.86(13) . . . . ?
C12 Si2 C4 Ge1 177.80(10) . . . . ?
C20 N2 C13 N1 -179.04(16) . . . . ?
Si3 N2 C13 N1 9.64(12) . . . . ?
C20 N2 C13 C14 2.1(3) . . . . ?
Si3 N2 C13 C14 -169.17(14) . . . . ?
C20 N2 C13 Si3 171.3(2) . . . . ?
C24 N1 C13 N2 -169.17(15) . . . . ?
Si3 N1 C13 N2 -9.63(12) . . . . ?
C24 N1 C13 C14 9.6(3) . . . . ?
Si3 N1 C13 C14 169.16(14) . . . . ?
C24 N1 C13 Si3 -159.54(19) . . . . ?
N2 C13 C14 C15 76.9(2) . . . . ?
N1 C13 C14 C15 -101.7(2) . . . . ?
N2 C13 C14 C19 -100.5(2) . . . . ?
N1 C13 C14 C19 80.9(2) . . . . ?
C19 C14 C15 C16 1.8(3) . . . . ?
C13 C14 C15 C16 -175.64(18) . . . . ?
C14 C15 C16 C17 -0.7(3) . . . . ?
C15 C16 C17 C18 -0.7(4) . . . . ?
C16 C17 C18 C19 1.0(4) . . . . ?
C17 C18 C19 C14 0.1(4) . . . . ?
C15 C14 C19 C18 -1.5(3) . . . . ?
C13 C14 C19 C18 176.0(2) . . . . ?
C13 N2 C20 C21 161.0(2) . . . . ?
Si3 N2 C20 C21 -31.3(2) . . . . ?
C13 N2 C20 C23 -80.1(2) . . . . ?
Si3 N2 C20 C23 87.6(2) . . . . ?
C13 N2 C20 C22 42.9(3) . . . . ?
Si3 N2 C20 C22 -149.39(16) . . . . ?
C13 N1 C24 C27 -62.0(2) . . . . ?
Si3 N1 C24 C27 146.72(15) . . . . ?
C13 N1 C24 C26 61.1(2) . . . . ?
Si3 N1 C24 C26 -90.23(18) . . . . ?
C13 N1 C24 C25 179.43(17) . . . . ?
Si3 N1 C24 C25 28.1(2) . . . . ?
C39 O1 C28 C29 172.3(2) . . . . ?
K1 O1 C28 C29 -37.1(3) . . . . ?
C30 O2 C29 C28 -179.6(2) . . . . ?
K1 O2 C29 C28 -59.0(3) . . . . ?
O1 C28 C29 O2 65.3(3) . . . . ?
C29 O2 C30 C31 -173.3(2) . . . . ?
K1 O2 C30 C31 66.3(2) . . . . ?
C32 O3 C31 C30 177.4(2) . . . . ?
K1 O3 C31 C30 27.7(3) . . . . ?
O2 C30 C31 O3 -63.3(3) . . . . ?
C31 O3 C32 C33 173.4(2) . . . . ?
K1 O3 C32 C33 -37.7(3) . . . . ?
C34 O4 C33 C32 -179.8(2) . . . . ?
K1 O4 C33 C32 -57.1(3) . . . . ?
O3 C32 C33 O4 63.0(3) . . . . ?
C33 O4 C34 C35 -171.3(2) . . . . ?
K1 O4 C34 C35 64.4(3) . . . . ?
C36 O5 C35 C34 179.6(3) . . . . ?
K1 O5 C35 C34 28.1(3) . . . . ?
O4 C34 C35 O5 -62.9(3) . . . . ?
C35 O5 C36 C37 174.9(3) . . . . ?
K1 O5 C36 C37 -33.2(3) . . . . ?
C38 O6 C37 C36 -177.5(2) . . . . ?
K1 O6 C37 C36 -62.5(2) . . . . ?
O5 C36 C37 O6 65.3(3) . . . . ?
C37 O6 C38 C39 -177.8(2) . . . . ?
K1 O6 C38 C39 65.2(2) . . . . ?
C28 O1 C39 C38 176.1(2) . . . . ?
K1 O1 C39 C38 25.5(3) . . . . ?
O6 C38 C39 O1 -63.8(3) . . . . ?
