# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Na-10
_database_code_depnum_ccdc_archive 'CCDC 926164'
_audit_update_record             
;
2014-05-01 deposited with the CCDC.
2016-10-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H40 Na O6 Si3, C21 H19 Si'
_chemical_formula_sum            'C37 H59 Na O6 Si4'
_chemical_formula_weight         735.19

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'
Na Na 0.0362 0.0249 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C 2/c'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.272(4)
_cell_length_b                   9.7485(17)
_cell_length_c                   37.173(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.149(2)
_cell_angle_gamma                90.00
_cell_volume                     8411(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9932
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      27.63

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3168
_exptl_absorpt_coefficient_mu    0.191
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9325
_exptl_absorpt_correction_T_max  0.9867
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            49332
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_sigmaI/netI    0.0520
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_theta_min         1.10
_diffrn_reflns_theta_max         27.92
_reflns_number_total             9999
_reflns_number_gt                6898
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0480P)²+5.4140P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9999
_refine_ls_number_parameters     444
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0465
_refine_ls_wR_factor_ref         0.1178
_refine_ls_wR_factor_gt          0.1045
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Si1 Si 0.32805(2) 0.44469(6) 0.038523(15) 0.02672(13) Uani 1 1 d . . .
Si2 Si 0.46059(2) 0.43096(6) 0.061654(15) 0.02738(13) Uani 1 1 d . . .
Si3 Si 0.39075(2) 0.69827(6) 0.074424(15) 0.02731(13) Uani 1 1 d . . .
Si21 Si 0.65888(2) 0.42017(6) 0.153338(16) 0.02881(14) Uani 1 1 d . . .
Na1 Na 0.36452(3) 0.41898(8) 0.13231(2) 0.02978(19) Uani 1 1 d . . .
O1 O 0.30193(5) 0.44224(14) 0.07890(4) 0.0290(3) Uani 1 1 d . . .
O2 O 0.26994(6) 0.36978(17) 0.14694(4) 0.0393(4) Uani 1 1 d . . .
O3 O 0.43674(6) 0.34083(14) 0.09546(4) 0.0311(3) Uani 1 1 d . . .
O4 O 0.40013(7) 0.21031(16) 0.15601(4) 0.0458(4) Uani 1 1 d . . .
O5 O 0.40398(6) 0.63991(14) 0.11629(4) 0.0301(3) Uani 1 1 d . . .
O6 O 0.40259(7) 0.53306(17) 0.18539(4) 0.0418(4) Uani 1 1 d . . .
C1 C 0.33458(10) 0.2647(2) 0.02309(7) 0.0474(6) Uani 1 1 d . . .
H1A H 0.2963 0.2224 0.0206 0.071 Uiso 1 1 calc R . .
H1B H 0.3592 0.2132 0.0408 0.071 Uiso 1 1 calc R . .
H1C H 0.3516 0.2634 -0.0003 0.071 Uiso 1 1 calc R . .
C2 C 0.27736(9) 0.5341(2) 0.00532(6) 0.0375(5) Uani 1 1 d . . .
H2A H 0.2394 0.4904 0.0050 0.056 Uiso 1 1 calc R . .
H2B H 0.2919 0.5282 -0.0187 0.056 Uiso 1 1 calc R . .
H2C H 0.2741 0.6306 0.0122 0.056 Uiso 1 1 calc R . .
C3 C 0.24660(9) 0.3824(3) 0.08407(6) 0.0411(6) Uani 1 1 d . . .
H3A H 0.2490 0.2814 0.0820 0.049 Uiso 1 1 calc R . .
H3B H 0.2178 0.4159 0.0652 0.049 Uiso 1 1 calc R . .
C4 C 0.22822(9) 0.4201(3) 0.12021(6) 0.0423(6) Uani 1 1 d . . .
H4A H 0.2250 0.5210 0.1222 0.051 Uiso 1 1 calc R . .
H4B H 0.1901 0.3794 0.1238 0.051 Uiso 1 1 calc R . .
C5 C 0.24937(12) 0.3769(3) 0.18199(7) 0.0511(7) Uani 1 1 d . . .
H5A H 0.2160 0.3161 0.1832 0.077 Uiso 1 1 calc R . .
H5B H 0.2380 0.4714 0.1870 0.077 Uiso 1 1 calc R . .
H5C H 0.2799 0.3481 0.1999 0.077 Uiso 1 1 calc R . .
C6 C 0.52584(9) 0.5275(3) 0.07831(6) 0.0407(6) Uani 1 1 d . . .
H6A H 0.5160 0.5907 0.0974 0.061 Uiso 1 1 calc R . .
H6B H 0.5405 0.5798 0.0584 0.061 Uiso 1 1 calc R . .
H6C H 0.5554 0.4631 0.0879 0.061 Uiso 1 1 calc R . .
C7 C 0.48305(10) 0.3133(3) 0.02579(6) 0.0424(6) Uani 1 1 d . . .
H7A H 0.5159 0.2579 0.0353 0.064 Uiso 1 1 calc R . .
H7B H 0.4942 0.3673 0.0052 0.064 Uiso 1 1 calc R . .
H7C H 0.4509 0.2528 0.0180 0.064 Uiso 1 1 calc R . .
C8 C 0.47405(10) 0.2534(3) 0.11730(8) 0.0592(8) Uani 1 1 d . . .
H8A H 0.4970 0.3097 0.1352 0.071 Uiso 1 1 calc R . .
H8B H 0.5011 0.2072 0.1019 0.071 Uiso 1 1 calc R . .
C9 C 0.44270(13) 0.1513(3) 0.13583(9) 0.0683(9) Uani 1 1 d . . .
H9A H 0.4243 0.0866 0.1180 0.082 Uiso 1 1 calc R . .
H9B H 0.4699 0.0984 0.1522 0.082 Uiso 1 1 calc R . .
C10 C 0.36937(15) 0.1071(3) 0.17286(11) 0.0910(12) Uani 1 1 d . . .
H10A H 0.3960 0.0532 0.1888 0.137 Uiso 1 1 calc R . .
H10B H 0.3506 0.0469 0.1545 0.137 Uiso 1 1 calc R . .
H10C H 0.3401 0.1494 0.1870 0.137 Uiso 1 1 calc R . .
C11 C 0.44470(10) 0.8296(2) 0.06357(6) 0.0411(6) Uani 1 1 d . . .
H11A H 0.4836 0.7923 0.0685 0.062 Uiso 1 1 calc R . .
H11B H 0.4401 0.9113 0.0785 0.062 Uiso 1 1 calc R . .
H11C H 0.4389 0.8545 0.0380 0.062 Uiso 1 1 calc R . .
C12 C 0.31932(9) 0.7852(2) 0.07226(7) 0.0403(5) Uani 1 1 d . . .
H12A H 0.3206 0.8619 0.0893 0.060 Uiso 1 1 calc R . .
H12B H 0.2897 0.7196 0.0785 0.060 Uiso 1 1 calc R . .
H12C H 0.3100 0.8198 0.0478 0.060 Uiso 1 1 calc R . .
C13 C 0.40517(10) 0.7271(2) 0.14717(6) 0.0387(5) Uani 1 1 d . . .
H13A H 0.3654 0.7526 0.1522 0.046 Uiso 1 1 calc R . .
H13B H 0.4266 0.8122 0.1424 0.046 Uiso 1 1 calc R . .
C14 C 0.43362(10) 0.6547(3) 0.17912(6) 0.0421(6) Uani 1 1 d . . .
H14A H 0.4739 0.6319 0.1746 0.050 Uiso 1 1 calc R . .
H14B H 0.4342 0.7149 0.2006 0.050 Uiso 1 1 calc R . .
C15 C 0.42529(15) 0.4624(3) 0.21697(7) 0.0722(9) Uani 1 1 d . . .
H15A H 0.4249 0.5236 0.2379 0.108 Uiso 1 1 calc R . .
H15B H 0.4650 0.4337 0.2138 0.108 Uiso 1 1 calc R . .
H15C H 0.4016 0.3814 0.2209 0.108 Uiso 1 1 calc R . .
C16 C 0.39741(8) 0.5405(2) 0.04618(5) 0.0243(4) Uani 1 1 d . . .
H16A H 0.4062 0.5749 0.0218 0.029 Uiso 1 1 calc R . .
C21 C 0.63044(8) 0.2558(2) 0.13612(5) 0.0286(4) Uani 1 1 d . . .
C22 C 0.62757(8) 0.1983(2) 0.10058(6) 0.0278(4) Uani 1 1 d . . .
C23 C 0.64495(9) 0.2473(2) 0.06726(6) 0.0325(5) Uani 1 1 d . . .
H23A H 0.6627 0.3348 0.0662 0.039 Uiso 1 1 calc R . .
C24 C 0.63640(9) 0.1697(2) 0.03636(6) 0.0376(5) Uani 1 1 d . . .
H24A H 0.6481 0.2051 0.0142 0.045 Uiso 1 1 calc R . .
C25 C 0.61089(9) 0.0402(2) 0.03688(7) 0.0416(6) Uani 1 1 d . . .
H25A H 0.6054 -0.0117 0.0153 0.050 Uiso 1 1 calc R . .
C26 C 0.59372(9) -0.0122(2) 0.06878(7) 0.0374(5) Uani 1 1 d . . .
H26A H 0.5765 -0.1005 0.0692 0.045 Uiso 1 1 calc R . .
C27 C 0.60152(8) 0.0641(2) 0.10067(6) 0.0306(5) Uani 1 1 d . . .
C28 C 0.58833(8) 0.0362(2) 0.13683(6) 0.0307(5) Uani 1 1 d . . .
C29 C 0.56416(9) -0.0783(2) 0.15280(7) 0.0399(6) Uani 1 1 d . . .
H29A H 0.5539 -0.1570 0.1387 0.048 Uiso 1 1 calc R . .
C30 C 0.55540(10) -0.0762(3) 0.18889(7) 0.0459(6) Uani 1 1 d . . .
H30A H 0.5390 -0.1538 0.1997 0.055 Uiso 1 1 calc R . .
C31 C 0.57034(10) 0.0391(3) 0.20996(7) 0.0452(6) Uani 1 1 d . . .
H31A H 0.5630 0.0397 0.2348 0.054 Uiso 1 1 calc R . .
C32 C 0.59574(9) 0.1520(2) 0.19515(6) 0.0384(5) Uani 1 1 d . . .
H32A H 0.6065 0.2285 0.2100 0.046 Uiso 1 1 calc R . .
C33 C 0.60566(8) 0.1541(2) 0.15827(6) 0.0300(5) Uani 1 1 d . . .
C34 C 0.71969(9) 0.3923(2) 0.18898(6) 0.0300(5) Uani 1 1 d . . .
C35 C 0.75006(9) 0.2698(2) 0.19097(6) 0.0380(5) Uani 1 1 d . . .
H35A H 0.7383 0.1973 0.1750 0.046 Uiso 1 1 calc R . .
C36 C 0.79718(10) 0.2497(3) 0.21558(6) 0.0437(6) Uani 1 1 d . . .
H36A H 0.8168 0.1642 0.2165 0.052 Uiso 1 1 calc R . .
C37 C 0.81532(10) 0.3535(3) 0.23855(6) 0.0424(6) Uani 1 1 d . . .
H37A H 0.8478 0.3405 0.2552 0.051 Uiso 1 1 calc R . .
C38 C 0.78617(10) 0.4768(3) 0.23743(6) 0.0433(6) Uani 1 1 d . . .
H38A H 0.7986 0.5490 0.2533 0.052 Uiso 1 1 calc R . .
C39 C 0.73883(10) 0.4951(2) 0.21313(6) 0.0373(5) Uani 1 1 d . . .
H39A H 0.7188 0.5801 0.2129 0.045 Uiso 1 1 calc R . .
C40 C 0.60303(10) 0.5248(3) 0.17504(7) 0.0442(6) Uani 1 1 d . . .
H40A H 0.5858 0.4696 0.1935 0.066 Uiso 1 1 calc R . .
H40B H 0.5730 0.5528 0.1567 0.066 Uiso 1 1 calc R . .
H40C H 0.6212 0.6065 0.1862 0.066 Uiso 1 1 calc R . .
C41 C 0.68997(10) 0.5306(2) 0.11836(6) 0.0402(5) Uani 1 1 d . . .
H41A H 0.7197 0.4793 0.1067 0.060 Uiso 1 1 calc R . .
H41B H 0.7070 0.6130 0.1298 0.060 Uiso 1 1 calc R . .
H41C H 0.6594 0.5573 0.1002 0.060 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Si1 O1 1.6596(15) . ?
Si1 C1 1.856(2) . ?
Si1 C2 1.861(2) . ?
Si1 C16 1.8686(19) . ?
Si2 O3 1.6613(15) . ?
Si2 C6 1.855(2) . ?
Si2 C7 1.862(2) . ?
Si2 C16 1.8735(19) . ?
Si3 O5 1.6645(15) . ?
Si3 C11 1.858(2) . ?
Si3 C12 1.862(2) . ?
Si3 C16 1.875(2) . ?
Si21 C21 1.832(2) . ?
Si21 C41 1.874(2) . ?
Si21 C40 1.879(2) . ?
Si21 C34 1.887(2) . ?
Na1 O4 2.3442(17) . ?
Na1 O2 2.3547(16) . ?
Na1 O3 2.3696(15) . ?
Na1 O6 2.3795(17) . ?
Na1 O1 2.3869(15) . ?
Na1 O5 2.4322(16) . ?
Na1 C8 3.102(3) . ?
O1 C3 1.439(2) . ?
O2 C5 1.422(3) . ?
O2 C4 1.425(3) . ?
O3 C8 1.427(2) . ?
O4 C10 1.408(3) . ?
O4 C9 1.408(3) . ?
O5 C13 1.427(2) . ?
O6 C14 1.417(3) . ?
O6 C15 1.429(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.485(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
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 C9 1.439(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
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 1.494(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 1.0000 . ?
C21 C22 1.432(3) . ?
C21 C33 1.436(3) . ?
C22 C23 1.414(3) . ?
C22 C27 1.442(3) . ?
C23 C24 1.378(3) . ?
C23 H23A 0.9500 . ?
C24 C25 1.396(3) . ?
C24 H24A 0.9500 . ?
C25 C26 1.377(3) . ?
C25 H25A 0.9500 . ?
C26 C27 1.400(3) . ?
C26 H26A 0.9500 . ?
C27 C28 1.426(3) . ?
C28 C29 1.401(3) . ?
C28 C33 1.440(3) . ?
C29 C30 1.371(3) . ?
C29 H29A 0.9500 . ?
C30 C31 1.399(4) . ?
C30 H30A 0.9500 . ?
C31 C32 1.383(3) . ?
C31 H31A 0.9500 . ?
C32 C33 1.407(3) . ?
C32 H32A 0.9500 . ?
C34 C35 1.387(3) . ?
C34 C39 1.397(3) . ?
C35 C36 1.390(3) . ?
C35 H35A 0.9500 . ?
C36 C37 1.370(3) . ?
C36 H36A 0.9500 . ?
C37 C38 1.379(4) . ?
C37 H37A 0.9500 . ?
C38 C39 1.385(3) . ?
C38 H38A 0.9500 . ?
C39 H39A 0.9500 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?

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
O1 Si1 C1 108.02(10) . . ?
O1 Si1 C2 110.52(9) . . ?
C1 Si1 C2 107.44(11) . . ?
O1 Si1 C16 103.78(8) . . ?
C1 Si1 C16 115.50(10) . . ?
C2 Si1 C16 111.49(10) . . ?
O3 Si2 C6 109.05(9) . . ?
O3 Si2 C7 110.01(10) . . ?
C6 Si2 C7 106.63(11) . . ?
O3 Si2 C16 103.65(8) . . ?
C6 Si2 C16 114.75(10) . . ?
C7 Si2 C16 112.70(10) . . ?
O5 Si3 C11 110.88(9) . . ?
O5 Si3 C12 107.46(9) . . ?
C11 Si3 C12 106.99(11) . . ?
O5 Si3 C16 103.05(8) . . ?
C11 Si3 C16 111.05(10) . . ?
C12 Si3 C16 117.31(10) . . ?
C21 Si21 C41 114.10(10) . . ?
C21 Si21 C40 112.40(10) . . ?
C41 Si21 C40 107.45(11) . . ?
C21 Si21 C34 110.69(9) . . ?
C41 Si21 C34 105.21(10) . . ?
C40 Si21 C34 106.47(10) . . ?
O4 Na1 O2 92.72(6) . . ?
O4 Na1 O3 72.06(5) . . ?
O2 Na1 O3 141.44(6) . . ?
O4 Na1 O6 89.63(6) . . ?
O2 Na1 O6 101.65(6) . . ?
O3 Na1 O6 113.12(6) . . ?
O4 Na1 O1 124.96(6) . . ?
O2 Na1 O1 71.76(5) . . ?
O3 Na1 O1 88.01(5) . . ?
O6 Na1 O1 144.45(6) . . ?
O4 Na1 O5 136.97(6) . . ?
O2 Na1 O5 127.79(6) . . ?
O3 Na1 O5 81.20(5) . . ?
O6 Na1 O5 70.41(5) . . ?
O1 Na1 O5 86.02(5) . . ?
O4 Na1 C8 48.94(6) . . ?
O2 Na1 C8 136.86(7) . . ?
O3 Na1 C8 26.13(6) . . ?
O6 Na1 C8 97.52(8) . . ?
O1 Na1 C8 111.09(7) . . ?
O5 Na1 C8 95.00(7) . . ?
C3 O1 Si1 121.10(13) . . ?
C3 O1 Na1 110.39(12) . . ?
Si1 O1 Na1 120.82(7) . . ?
C5 O2 C4 111.38(18) . . ?
C5 O2 Na1 125.73(15) . . ?
C4 O2 Na1 111.72(12) . . ?
C8 O3 Si2 121.56(13) . . ?
C8 O3 Na1 106.91(13) . . ?
Si2 O3 Na1 123.84(8) . . ?
C10 O4 C9 110.2(2) . . ?
C10 O4 Na1 127.59(17) . . ?
C9 O4 Na1 113.44(14) . . ?
C13 O5 Si3 122.70(13) . . ?
C13 O5 Na1 108.41(12) . . ?
Si3 O5 Na1 118.95(7) . . ?
C14 O6 C15 112.1(2) . . ?
C14 O6 Na1 114.73(13) . . ?
C15 O6 Na1 123.31(16) . . ?
Si1 C1 H1A 109.5 . . ?
Si1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Si1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O1 C3 C4 109.87(19) . . ?
O1 C3 H3A 109.7 . . ?
C4 C3 H3A 109.7 . . ?
O1 C3 H3B 109.7 . . ?
C4 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
O2 C4 C3 108.61(18) . . ?
O2 C4 H4A 110.0 . . ?
C3 C4 H4A 110.0 . . ?
O2 C4 H4B 110.0 . . ?
C3 C4 H4B 110.0 . . ?
H4A C4 H4B 108.3 . . ?
O2 C5 H5A 109.5 . . ?
O2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
O2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O3 C8 C9 112.1(2) . . ?
O3 C8 Na1 46.97(10) . . ?
C9 C8 Na1 79.76(14) . . ?
O3 C8 H8A 109.2 . . ?
C9 C8 H8A 109.2 . . ?
Na1 C8 H8A 90.0 . . ?
O3 C8 H8B 109.2 . . ?
C9 C8 H8B 109.2 . . ?
Na1 C8 H8B 155.0 . . ?
H8A C8 H8B 107.9 . . ?
O4 C9 C8 111.9(2) . . ?
O4 C9 H9A 109.2 . . ?
C8 C9 H9A 109.2 . . ?
O4 C9 H9B 109.2 . . ?
C8 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
O4 C10 H10A 109.5 . . ?
O4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si3 C11 H11A 109.5 . . ?
Si3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si3 C12 H12A 109.5 . . ?
Si3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O5 C13 C14 109.90(18) . . ?
O5 C13 H13A 109.7 . . ?
C14 C13 H13A 109.7 . . ?
O5 C13 H13B 109.7 . . ?
C14 C13 H13B 109.7 . . ?
H13A C13 H13B 108.2 . . ?
O6 C14 C13 108.90(18) . . ?
O6 C14 H14A 109.9 . . ?
C13 C14 H14A 109.9 . . ?
O6 C14 H14B 109.9 . . ?
C13 C14 H14B 109.9 . . ?
H14A C14 H14B 108.3 . . ?
O6 C15 H15A 109.5 . . ?
O6 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O6 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si1 C16 Si2 114.34(10) . . ?
Si1 C16 Si3 112.94(10) . . ?
Si2 C16 Si3 112.98(10) . . ?
Si1 C16 H16A 105.2 . . ?
Si2 C16 H16A 105.2 . . ?
Si3 C16 H16A 105.2 . . ?
C22 C21 C33 105.38(18) . . ?
C22 C21 Si21 131.02(16) . . ?
C33 C21 Si21 123.60(16) . . ?
C23 C22 C21 132.73(19) . . ?
C23 C22 C27 117.13(19) . . ?
C21 C22 C27 110.14(18) . . ?
C24 C23 C22 120.8(2) . . ?
C24 C23 H23A 119.6 . . ?
C22 C23 H23A 119.6 . . ?
C23 C24 C25 121.4(2) . . ?
C23 C24 H24A 119.3 . . ?
C25 C24 H24A 119.3 . . ?
C26 C25 C24 119.8(2) . . ?
C26 C25 H25A 120.1 . . ?
C24 C25 H25A 120.1 . . ?
C25 C26 C27 120.3(2) . . ?
C25 C26 H26A 119.9 . . ?
C27 C26 H26A 119.9 . . ?
C26 C27 C28 132.3(2) . . ?
C26 C27 C22 120.6(2) . . ?
C28 C27 C22 107.12(18) . . ?
C29 C28 C27 132.2(2) . . ?
C29 C28 C33 120.4(2) . . ?
C27 C28 C33 107.38(18) . . ?
C30 C29 C28 119.7(2) . . ?
C30 C29 H29A 120.2 . . ?
C28 C29 H29A 120.2 . . ?
C29 C30 C31 120.8(2) . . ?
C29 C30 H30A 119.6 . . ?
C31 C30 H30A 119.6 . . ?
C32 C31 C30 120.8(2) . . ?
C32 C31 H31A 119.6 . . ?
C30 C31 H31A 119.6 . . ?
C31 C32 C33 120.3(2) . . ?
C31 C32 H32A 119.8 . . ?
C33 C32 H32A 119.8 . . ?
C32 C33 C21 132.1(2) . . ?
C32 C33 C28 117.94(19) . . ?
C21 C33 C28 109.97(19) . . ?
C35 C34 C39 116.5(2) . . ?
C35 C34 Si21 120.98(16) . . ?
C39 C34 Si21 122.44(17) . . ?
C34 C35 C36 122.1(2) . . ?
C34 C35 H35A 119.0 . . ?
C36 C35 H35A 119.0 . . ?
C37 C36 C35 119.9(2) . . ?
C37 C36 H36A 120.0 . . ?
C35 C36 H36A 120.0 . . ?
C36 C37 C38 119.7(2) . . ?
C36 C37 H37A 120.1 . . ?
C38 C37 H37A 120.1 . . ?
C37 C38 C39 119.9(2) . . ?
C37 C38 H38A 120.0 . . ?
C39 C38 H38A 120.0 . . ?
C38 C39 C34 121.9(2) . . ?
C38 C39 H39A 119.0 . . ?
C34 C39 H39A 119.0 . . ?
Si21 C40 H40A 109.5 . . ?
Si21 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
Si21 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
Si21 C41 H41A 109.5 . . ?
Si21 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
Si21 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?

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
C1 Si1 O1 C3 -59.97(18) . . . . ?
C2 Si1 O1 C3 57.31(18) . . . . ?
C16 Si1 O1 C3 176.94(16) . . . . ?
C1 Si1 O1 Na1 86.50(11) . . . . ?
C2 Si1 O1 Na1 -156.22(10) . . . . ?
C16 Si1 O1 Na1 -36.59(10) . . . . ?
O4 Na1 O1 C3 66.53(15) . . . . ?
O2 Na1 O1 C3 -13.71(14) . . . . ?
O3 Na1 O1 C3 132.94(14) . . . . ?
O6 Na1 O1 C3 -98.22(16) . . . . ?
O5 Na1 O1 C3 -145.75(14) . . . . ?
C8 Na1 O1 C3 120.42(14) . . . . ?
O4 Na1 O1 Si1 -83.17(10) . . . . ?
O2 Na1 O1 Si1 -163.41(10) . . . . ?
O3 Na1 O1 Si1 -16.76(9) . . . . ?
O6 Na1 O1 Si1 112.08(11) . . . . ?
O5 Na1 O1 Si1 64.55(9) . . . . ?
C8 Na1 O1 Si1 -29.28(11) . . . . ?
O4 Na1 O2 C5 75.97(18) . . . . ?
O3 Na1 O2 C5 140.18(17) . . . . ?
O6 Na1 O2 C5 -14.22(18) . . . . ?
O1 Na1 O2 C5 -157.99(18) . . . . ?
O5 Na1 O2 C5 -88.36(18) . . . . ?
C8 Na1 O2 C5 100.33(19) . . . . ?
O4 Na1 O2 C4 -143.68(15) . . . . ?
O3 Na1 O2 C4 -79.48(17) . . . . ?
O6 Na1 O2 C4 126.13(15) . . . . ?
O1 Na1 O2 C4 -17.65(14) . . . . ?
O5 Na1 O2 C4 51.99(17) . . . . ?
C8 Na1 O2 C4 -119.32(16) . . . . ?
C6 Si2 O3 C8 -51.0(2) . . . . ?
C7 Si2 O3 C8 65.6(2) . . . . ?
C16 Si2 O3 C8 -173.64(19) . . . . ?
C6 Si2 O3 Na1 94.38(11) . . . . ?
C7 Si2 O3 Na1 -149.01(10) . . . . ?
C16 Si2 O3 Na1 -28.28(11) . . . . ?
O4 Na1 O3 C8 -24.80(16) . . . . ?
O2 Na1 O3 C8 -95.76(18) . . . . ?
O6 Na1 O3 C8 56.83(17) . . . . ?
O1 Na1 O3 C8 -152.67(16) . . . . ?
O5 Na1 O3 C8 121.05(16) . . . . ?
O4 Na1 O3 Si2 -174.39(11) . . . . ?
O2 Na1 O3 Si2 114.65(11) . . . . ?
O6 Na1 O3 Si2 -92.75(10) . . . . ?
O1 Na1 O3 Si2 57.75(10) . . . . ?
O5 Na1 O3 Si2 -28.53(9) . . . . ?
C8 Na1 O3 Si2 -149.6(2) . . . . ?
O2 Na1 O4 C10 -1.5(3) . . . . ?
O3 Na1 O4 C10 -145.3(3) . . . . ?
O6 Na1 O4 C10 100.2(3) . . . . ?
O1 Na1 O4 C10 -71.0(3) . . . . ?
O5 Na1 O4 C10 160.3(2) . . . . ?
C8 Na1 O4 C10 -159.5(3) . . . . ?
O2 Na1 O4 C9 142.4(2) . . . . ?
O3 Na1 O4 C9 -1.43(19) . . . . ?
O6 Na1 O4 C9 -115.9(2) . . . . ?
O1 Na1 O4 C9 72.9(2) . . . . ?
O5 Na1 O4 C9 -55.8(2) . . . . ?
C8 Na1 O4 C9 -15.6(2) . . . . ?
C11 Si3 O5 C13 59.25(18) . . . . ?
C12 Si3 O5 C13 -57.35(18) . . . . ?
C16 Si3 O5 C13 178.13(15) . . . . ?
C11 Si3 O5 Na1 -159.12(10) . . . . ?
C12 Si3 O5 Na1 84.28(11) . . . . ?
C16 Si3 O5 Na1 -40.25(10) . . . . ?
O4 Na1 O5 C13 -89.79(15) . . . . ?
O2 Na1 O5 C13 66.92(14) . . . . ?
O3 Na1 O5 C13 -141.29(13) . . . . ?
O6 Na1 O5 C13 -22.81(13) . . . . ?
O1 Na1 O5 C13 130.11(13) . . . . ?
C8 Na1 O5 C13 -119.04(13) . . . . ?
O4 Na1 O5 Si3 123.62(10) . . . . ?
O2 Na1 O5 Si3 -79.68(10) . . . . ?
O3 Na1 O5 Si3 72.12(8) . . . . ?
O6 Na1 O5 Si3 -169.41(10) . . . . ?
O1 Na1 O5 Si3 -16.48(8) . . . . ?
C8 Na1 O5 Si3 94.37(10) . . . . ?
O4 Na1 O6 C14 133.09(15) . . . . ?
O2 Na1 O6 C14 -134.21(15) . . . . ?
O3 Na1 O6 C14 62.82(15) . . . . ?
O1 Na1 O6 C14 -59.35(19) . . . . ?
O5 Na1 O6 C14 -8.00(14) . . . . ?
C8 Na1 O6 C14 84.65(15) . . . . ?
O4 Na1 O6 C15 -9.9(2) . . . . ?
O2 Na1 O6 C15 82.8(2) . . . . ?
O3 Na1 O6 C15 -80.2(2) . . . . ?
O1 Na1 O6 C15 157.7(2) . . . . ?
O5 Na1 O6 C15 -151.0(2) . . . . ?
C8 Na1 O6 C15 -58.3(2) . . . . ?
Si1 O1 C3 C4 -167.82(14) . . . . ?
Na1 O1 C3 C4 42.6(2) . . . . ?
C5 O2 C4 C3 -167.83(19) . . . . ?
Na1 O2 C4 C3 46.0(2) . . . . ?
O1 C3 C4 O2 -59.9(2) . . . . ?
Si2 O3 C8 C9 -159.5(2) . . . . ?
Na1 O3 C8 C9 50.0(3) . . . . ?
Si2 O3 C8 Na1 150.43(19) . . . . ?
O4 Na1 C8 O3 148.0(2) . . . . ?
O2 Na1 C8 O3 114.92(14) . . . . ?
O6 Na1 C8 O3 -129.05(15) . . . . ?
O1 Na1 C8 O3 29.46(16) . . . . ?
O5 Na1 C8 O3 -58.19(15) . . . . ?
O4 Na1 C8 C9 14.21(17) . . . . ?
O2 Na1 C8 C9 -18.9(2) . . . . ?
O3 Na1 C8 C9 -133.8(3) . . . . ?
O6 Na1 C8 C9 97.1(2) . . . . ?
O1 Na1 C8 C9 -104.37(19) . . . . ?
O5 Na1 C8 C9 167.97(19) . . . . ?
C10 O4 C9 C8 178.3(3) . . . . ?
Na1 O4 C9 C8 28.1(3) . . . . ?
O3 C8 C9 O4 -54.1(4) . . . . ?
Na1 C8 C9 O4 -19.4(2) . . . . ?
Si3 O5 C13 C14 -164.35(14) . . . . ?
Na1 O5 C13 C14 50.58(19) . . . . ?
C15 O6 C14 C13 -176.4(2) . . . . ?
Na1 O6 C14 C13 36.4(2) . . . . ?
O5 C13 C14 O6 -59.1(2) . . . . ?
O1 Si1 C16 Si2 86.54(11) . . . . ?
C1 Si1 C16 Si2 -31.49(16) . . . . ?
C2 Si1 C16 Si2 -154.49(11) . . . . ?
O1 Si1 C16 Si3 -44.51(12) . . . . ?
C1 Si1 C16 Si3 -162.54(12) . . . . ?
C2 Si1 C16 Si3 74.46(13) . . . . ?
O3 Si2 C16 Si1 -49.21(12) . . . . ?
C6 Si2 C16 Si1 -168.01(11) . . . . ?
C7 Si2 C16 Si1 69.69(14) . . . . ?
O3 Si2 C16 Si3 81.82(11) . . . . ?
C6 Si2 C16 Si3 -36.98(14) . . . . ?
C7 Si2 C16 Si3 -159.28(11) . . . . ?
O5 Si3 C16 Si1 88.92(11) . . . . ?
C11 Si3 C16 Si1 -152.32(11) . . . . ?
C12 Si3 C16 Si1 -28.89(15) . . . . ?
O5 Si3 C16 Si2 -42.81(11) . . . . ?
C11 Si3 C16 Si2 75.95(13) . . . . ?
C12 Si3 C16 Si2 -160.61(11) . . . . ?
C41 Si21 C21 C22 -0.6(2) . . . . ?
C40 Si21 C21 C22 122.10(19) . . . . ?
C34 Si21 C21 C22 -118.99(19) . . . . ?
C41 Si21 C21 C33 178.76(16) . . . . ?
C40 Si21 C21 C33 -58.6(2) . . . . ?
C34 Si21 C21 C33 60.34(19) . . . . ?
C33 C21 C22 C23 -179.8(2) . . . . ?
Si21 C21 C22 C23 -0.4(3) . . . . ?
C33 C21 C22 C27 0.1(2) . . . . ?
Si21 C21 C22 C27 179.51(15) . . . . ?
C21 C22 C23 C24 -179.3(2) . . . . ?
C27 C22 C23 C24 0.8(3) . . . . ?
C22 C23 C24 C25 -0.6(3) . . . . ?
C23 C24 C25 C26 0.0(3) . . . . ?
C24 C25 C26 C27 0.3(3) . . . . ?
C25 C26 C27 C28 -179.8(2) . . . . ?
C25 C26 C27 C22 0.0(3) . . . . ?
C23 C22 C27 C26 -0.5(3) . . . . ?
C21 C22 C27 C26 179.57(17) . . . . ?
C23 C22 C27 C28 179.34(17) . . . . ?
C21 C22 C27 C28 -0.6(2) . . . . ?
C26 C27 C28 C29 1.5(4) . . . . ?
C22 C27 C28 C29 -178.3(2) . . . . ?
C26 C27 C28 C33 -179.4(2) . . . . ?
C22 C27 C28 C33 0.8(2) . . . . ?
C27 C28 C29 C30 -179.0(2) . . . . ?
C33 C28 C29 C30 2.0(3) . . . . ?
C28 C29 C30 C31 0.0(3) . . . . ?
C29 C30 C31 C32 -1.8(4) . . . . ?
C30 C31 C32 C33 1.6(3) . . . . ?
C31 C32 C33 C21 179.6(2) . . . . ?
C31 C32 C33 C28 0.3(3) . . . . ?
C22 C21 C33 C32 -178.9(2) . . . . ?
Si21 C21 C33 C32 1.6(3) . . . . ?
C22 C21 C33 C28 0.4(2) . . . . ?
Si21 C21 C33 C28 -179.05(14) . . . . ?
C29 C28 C33 C32 -2.1(3) . . . . ?
C27 C28 C33 C32 178.65(18) . . . . ?
C29 C28 C33 C21 178.46(18) . . . . ?
C27 C28 C33 C21 -0.8(2) . . . . ?
C21 Si21 C34 C35 21.4(2) . . . . ?
C41 Si21 C34 C35 -102.28(19) . . . . ?
C40 Si21 C34 C35 143.86(18) . . . . ?
C21 Si21 C34 C39 -162.55(17) . . . . ?
C41 Si21 C34 C39 73.7(2) . . . . ?
C40 Si21 C34 C39 -40.1(2) . . . . ?
C39 C34 C35 C36 -0.1(3) . . . . ?
Si21 C34 C35 C36 176.12(18) . . . . ?
C34 C35 C36 C37 -0.8(4) . . . . ?
C35 C36 C37 C38 0.9(4) . . . . ?
C36 C37 C38 C39 0.0(3) . . . . ?
C37 C38 C39 C34 -0.9(3) . . . . ?
C35 C34 C39 C38 1.0(3) . . . . ?
Si21 C34 C39 C38 -175.20(17) . . . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.052


#==END
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Li-1
_database_code_depnum_ccdc_archive 'CCDC 1000501'
_audit_update_record             
;
2014-05-01 deposited with the CCDC.
2016-10-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H39 Li O6 Si3'
_chemical_formula_sum            'C16 H39 Li O6 Si3'
_chemical_formula_weight         418.68

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C c'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   9.531(5)
_cell_length_b                   17.403(8)
_cell_length_c                   15.039(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.873(6)
_cell_angle_gamma                90.00
_cell_volume                     2494(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1997
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      17.97

_exptl_crystal_description       chunk
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             912
_exptl_absorpt_coefficient_mu    0.214
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9444
_exptl_absorpt_correction_T_max  0.9831
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14494
_diffrn_reflns_av_R_equivalents  0.1480
_diffrn_reflns_av_sigmaI/netI    0.2370
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.34
_diffrn_reflns_theta_max         27.78
_reflns_number_total             5737
_reflns_number_gt                2346
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.

 The crystals of this compounds were invariably of low quality, and diffracted
 poorely.  This has resulted in the elevated values of
 _diffrn_reflns_av_R_equivalents and _diffrn_reflns_av_sigmaI/netI.  The flack
 parameter was found to be meaningless, due to weak anomalous scattering by
 the compound, and was removed.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0424P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5737
_refine_ls_number_parameters     244
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.2205
_refine_ls_R_factor_gt           0.0762
_refine_ls_wR_factor_ref         0.1585
_refine_ls_wR_factor_gt          0.1172
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_restrained_S_all      0.949
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Si1 Si 0.53364(17) 0.14222(10) 0.02929(12) 0.0390(5) Uani 1 1 d . . .
Si2 Si 0.4726(2) 0.11544(10) -0.17510(13) 0.0468(5) Uani 1 1 d . . .
Si3 Si 0.26260(18) 0.19498(10) -0.05194(13) 0.0402(5) Uani 1 1 d . . .
O1 O 0.6191(4) 0.2287(2) 0.0269(3) 0.0391(11) Uani 1 1 d . . .
O2 O 0.7250(4) 0.3669(2) 0.0024(3) 0.0534(13) Uani 1 1 d . . .
O3 O 0.5172(5) 0.1908(2) -0.2384(3) 0.0562(13) Uani 1 1 d . . .
O4 O 0.4887(5) 0.3466(2) -0.1478(3) 0.0496(12) Uani 1 1 d . . .
O5 O 0.3151(4) 0.2760(2) 0.0036(3) 0.0372(11) Uani 1 1 d . . .
O6 O 0.4268(4) 0.4050(2) 0.0628(3) 0.0434(11) Uani 1 1 d . . .
C1 C 0.6764(8) 0.0686(4) 0.0387(5) 0.076(3) Uani 1 1 d . . .
H1A H 0.6356 0.0171 0.0336 0.114 Uiso 1 1 calc R . .
H1B H 0.7245 0.0738 0.0964 0.114 Uiso 1 1 calc R . .
H1C H 0.7438 0.0764 -0.0091 0.114 Uiso 1 1 calc R . .
C2 C 0.4512(8) 0.1398(4) 0.1418(4) 0.063(2) Uani 1 1 d . . .
H2A H 0.3968 0.0924 0.1480 0.095 Uiso 1 1 calc R . .
H2B H 0.3890 0.1843 0.1482 0.095 Uiso 1 1 calc R . .
H2C H 0.5248 0.1416 0.1880 0.095 Uiso 1 1 calc R . .
C3 C 0.7302(7) 0.2528(4) 0.0852(5) 0.0475(18) Uani 1 1 d . . .
H3A H 0.7876 0.2081 0.1041 0.057 Uiso 1 1 calc R . .
H3B H 0.6913 0.2773 0.1389 0.057 Uiso 1 1 calc R . .
C4 C 0.8178(7) 0.3087(4) 0.0359(5) 0.056(2) Uani 1 1 d . . .
H4A H 0.8897 0.3316 0.0760 0.067 Uiso 1 1 calc R . .
H4B H 0.8658 0.2828 -0.0137 0.067 Uiso 1 1 calc R . .
C5 C 0.7990(9) 0.4269(4) -0.0422(6) 0.086(3) Uani 1 1 d . . .
H5A H 0.8632 0.4524 -0.0001 0.129 Uiso 1 1 calc R . .
H5B H 0.7317 0.4645 -0.0660 0.129 Uiso 1 1 calc R . .
H5C H 0.8528 0.4050 -0.0911 0.129 Uiso 1 1 calc R . .
C6 C 0.3349(8) 0.0704(4) -0.2475(5) 0.075(3) Uani 1 1 d . . .
H6A H 0.2541 0.1051 -0.2527 0.113 Uiso 1 1 calc R . .
H6B H 0.3051 0.0217 -0.2213 0.113 Uiso 1 1 calc R . .
H6C H 0.3730 0.0609 -0.3067 0.113 Uiso 1 1 calc R . .
C7 C 0.6258(8) 0.0474(4) -0.1796(5) 0.070(2) Uani 1 1 d . . .
H7A H 0.7120 0.0746 -0.1623 0.105 Uiso 1 1 calc R . .
H7B H 0.6347 0.0276 -0.2403 0.105 Uiso 1 1 calc R . .
H7C H 0.6105 0.0045 -0.1386 0.105 Uiso 1 1 calc R . .
C8 C 0.6240(7) 0.2445(4) -0.2108(5) 0.058(2) Uani 1 1 d . . .
H8A H 0.7087 0.2370 -0.2470 0.070 Uiso 1 1 calc R . .
H8B H 0.6500 0.2351 -0.1478 0.070 Uiso 1 1 calc R . .
C9 C 0.5723(8) 0.3258(4) -0.2215(4) 0.054(2) Uani 1 1 d . . .
H9A H 0.6533 0.3611 -0.2255 0.065 Uiso 1 1 calc R . .
H9B H 0.5161 0.3303 -0.2771 0.065 Uiso 1 1 calc R . .
C10 C 0.4143(8) 0.4170(4) -0.1656(5) 0.073(3) Uani 1 1 d . . .
H10A H 0.3470 0.4089 -0.2147 0.110 Uiso 1 1 calc R . .
H10B H 0.4812 0.4572 -0.1820 0.110 Uiso 1 1 calc R . .
H10C H 0.3639 0.4329 -0.1123 0.110 Uiso 1 1 calc R . .
C11 C 0.1686(7) 0.2320(4) -0.1550(5) 0.065(2) Uani 1 1 d . . .
H11A H 0.2375 0.2509 -0.1974 0.097 Uiso 1 1 calc R . .
H11B H 0.1054 0.2739 -0.1386 0.097 Uiso 1 1 calc R . .
H11C H 0.1140 0.1902 -0.1823 0.097 Uiso 1 1 calc R . .
C12 C 0.1211(6) 0.1487(4) 0.0157(5) 0.057(2) Uani 1 1 d . . .
H12A H 0.1582 0.1367 0.0752 0.086 Uiso 1 1 calc R . .
H12B H 0.0899 0.1012 -0.0136 0.086 Uiso 1 1 calc R . .
H12C H 0.0416 0.1841 0.0206 0.086 Uiso 1 1 calc R . .
C13 C 0.2230(6) 0.3295(4) 0.0456(5) 0.0474(19) Uani 1 1 d . . .
H13A H 0.1482 0.3019 0.0774 0.057 Uiso 1 1 calc R . .
H13B H 0.1785 0.3635 0.0005 0.057 Uiso 1 1 calc R . .
C14 C 0.3100(7) 0.3756(4) 0.1093(5) 0.054(2) Uani 1 1 d . . .
H14A H 0.2538 0.4184 0.1337 0.065 Uiso 1 1 calc R . .
H14B H 0.3424 0.3429 0.1594 0.065 Uiso 1 1 calc R . .
C15 C 0.5070(7) 0.4570(4) 0.1167(5) 0.064(2) Uani 1 1 d . . .
H15A H 0.4504 0.5026 0.1295 0.096 Uiso 1 1 calc R . .
H15B H 0.5915 0.4723 0.0850 0.096 Uiso 1 1 calc R . .
H15C H 0.5339 0.4317 0.1726 0.096 Uiso 1 1 calc R . .
C16 C 0.4198(6) 0.1394(3) -0.0654(4) 0.0346(15) Uani 1 1 d . . .
Li1 Li 0.5123(11) 0.3178(6) -0.0176(7) 0.043(3) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Si1 O1 1.711(4) . ?
Si1 C16 1.778(6) . ?
Si1 C1 1.872(7) . ?
Si1 C2 1.878(7) . ?
Si1 Li1 3.142(11) . ?
Si2 O3 1.679(5) . ?
Si2 C16 1.781(6) . ?
Si2 C6 1.866(7) . ?
Si2 C7 1.882(7) . ?
Si3 O5 1.710(4) . ?
Si3 C16 1.797(6) . ?
Si3 C12 1.882(6) . ?
Si3 C11 1.891(7) . ?
O1 C3 1.428(7) . ?
O1 Li1 1.967(11) . ?
O2 C4 1.431(7) . ?
O2 C5 1.433(7) . ?
O2 Li1 2.216(12) . ?
O3 C8 1.438(8) . ?
O4 C9 1.422(7) . ?
O4 C10 1.438(7) . ?
O4 Li1 2.031(11) . ?
O5 C13 1.433(6) . ?
O5 Li1 2.046(12) . ?
O6 C14 1.419(7) . ?
O6 C15 1.429(7) . ?
O6 Li1 2.112(11) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.488(9) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
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 C9 1.505(8) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
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 1.492(8) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?

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
O1 Si1 C16 107.0(2) . . ?
O1 Si1 C1 104.9(3) . . ?
C16 Si1 C1 118.4(3) . . ?
O1 Si1 C2 104.1(3) . . ?
C16 Si1 C2 117.6(3) . . ?
C1 Si1 C2 103.3(4) . . ?
O1 Si1 Li1 33.8(2) . . ?
C16 Si1 Li1 79.1(3) . . ?
C1 Si1 Li1 136.6(3) . . ?
C2 Si1 Li1 101.4(3) . . ?
O3 Si2 C16 114.8(3) . . ?
O3 Si2 C6 100.3(3) . . ?
C16 Si2 C6 115.6(3) . . ?
O3 Si2 C7 105.5(3) . . ?
C16 Si2 C7 114.3(3) . . ?
C6 Si2 C7 104.7(3) . . ?
O5 Si3 C16 105.1(2) . . ?
O5 Si3 C12 107.2(3) . . ?
C16 Si3 C12 115.8(3) . . ?
O5 Si3 C11 104.6(3) . . ?
C16 Si3 C11 118.4(3) . . ?
C12 Si3 C11 104.7(3) . . ?
C3 O1 Si1 126.5(4) . . ?
C3 O1 Li1 110.6(5) . . ?
Si1 O1 Li1 117.2(4) . . ?
C4 O2 C5 112.0(5) . . ?
C4 O2 Li1 109.5(4) . . ?
C5 O2 Li1 132.3(5) . . ?
C8 O3 Si2 121.9(4) . . ?
C9 O4 C10 110.6(5) . . ?
C9 O4 Li1 129.3(5) . . ?
C10 O4 Li1 115.9(5) . . ?
C13 O5 Si3 125.1(4) . . ?
C13 O5 Li1 114.1(5) . . ?
Si3 O5 Li1 118.7(4) . . ?
C14 O6 C15 111.4(5) . . ?
C14 O6 Li1 109.6(5) . . ?
C15 O6 Li1 124.9(5) . . ?
Si1 C1 H1A 109.5 . . ?
Si1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Si1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O1 C3 C4 107.6(6) . . ?
O1 C3 H3A 110.2 . . ?
C4 C3 H3A 110.2 . . ?
O1 C3 H3B 110.2 . . ?
C4 C3 H3B 110.2 . . ?
H3A C3 H3B 108.5 . . ?
O2 C4 C3 106.9(5) . . ?
O2 C4 H4A 110.3 . . ?
C3 C4 H4A 110.3 . . ?
O2 C4 H4B 110.3 . . ?
C3 C4 H4B 110.3 . . ?
H4A C4 H4B 108.6 . . ?
O2 C5 H5A 109.5 . . ?
O2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
O2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O3 C8 C9 110.5(6) . . ?
O3 C8 H8A 109.5 . . ?
C9 C8 H8A 109.5 . . ?
O3 C8 H8B 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
O4 C9 C8 110.1(5) . . ?
O4 C9 H9A 109.6 . . ?
C8 C9 H9A 109.6 . . ?
O4 C9 H9B 109.6 . . ?
C8 C9 H9B 109.6 . . ?
H9A C9 H9B 108.2 . . ?
O4 C10 H10A 109.5 . . ?
O4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si3 C11 H11A 109.5 . . ?
Si3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si3 C12 H12A 109.5 . . ?
Si3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O5 C13 C14 107.1(5) . . ?
O5 C13 H13A 110.3 . . ?
C14 C13 H13A 110.3 . . ?
O5 C13 H13B 110.3 . . ?
C14 C13 H13B 110.3 . . ?
H13A C13 H13B 108.5 . . ?
O6 C14 C13 108.0(5) . . ?
O6 C14 H14A 110.1 . . ?
C13 C14 H14A 110.1 . . ?
O6 C14 H14B 110.1 . . ?
C13 C14 H14B 110.1 . . ?
H14A C14 H14B 108.4 . . ?
O6 C15 H15A 109.5 . . ?
O6 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O6 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si1 C16 Si2 124.8(3) . . ?
Si1 C16 Si3 113.2(3) . . ?
Si2 C16 Si3 118.6(3) . . ?
O1 Li1 O4 124.9(5) . . ?
O1 Li1 O5 97.9(5) . . ?
O4 Li1 O5 98.6(5) . . ?
O1 Li1 O6 125.0(5) . . ?
O4 Li1 O6 109.7(5) . . ?
O5 Li1 O6 78.6(4) . . ?
O1 Li1 O2 77.9(4) . . ?
O4 Li1 O2 97.1(5) . . ?
O5 Li1 O2 163.1(6) . . ?
O6 Li1 O2 90.3(4) . . ?
O1 Li1 Si1 29.0(2) . . ?
O4 Li1 Si1 117.5(4) . . ?
O5 Li1 Si1 71.0(3) . . ?
O6 Li1 Si1 126.5(4) . . ?
O2 Li1 Si1 106.8(4) . . ?

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
C16 Si1 O1 C3 -173.7(5) . . . . ?
C1 Si1 O1 C3 -47.1(6) . . . . ?
C2 Si1 O1 C3 61.1(5) . . . . ?
Li1 Si1 O1 C3 150.6(7) . . . . ?
C16 Si1 O1 Li1 35.8(5) . . . . ?
C1 Si1 O1 Li1 162.3(5) . . . . ?
C2 Si1 O1 Li1 -89.4(5) . . . . ?
C16 Si2 O3 C8 55.9(5) . . . . ?
C6 Si2 O3 C8 -179.4(5) . . . . ?
C7 Si2 O3 C8 -70.9(5) . . . . ?
C16 Si3 O5 C13 -166.1(5) . . . . ?
C12 Si3 O5 C13 -42.4(5) . . . . ?
C11 Si3 O5 C13 68.4(5) . . . . ?
C16 Si3 O5 Li1 31.7(5) . . . . ?
C12 Si3 O5 Li1 155.5(4) . . . . ?
C11 Si3 O5 Li1 -93.8(5) . . . . ?
Si1 O1 C3 C4 152.0(4) . . . . ?
Li1 O1 C3 C4 -55.9(7) . . . . ?
C5 O2 C4 C3 176.5(6) . . . . ?
Li1 O2 C4 C3 -27.5(7) . . . . ?
O1 C3 C4 O2 53.4(7) . . . . ?
Si2 O3 C8 C9 -131.2(5) . . . . ?
C10 O4 C9 C8 -167.6(6) . . . . ?
Li1 O4 C9 C8 36.6(9) . . . . ?
O3 C8 C9 O4 81.3(7) . . . . ?
Si3 O5 C13 C14 162.0(4) . . . . ?
Li1 O5 C13 C14 -35.1(7) . . . . ?
C15 O6 C14 C13 173.4(5) . . . . ?
Li1 O6 C14 C13 -44.2(6) . . . . ?
O5 C13 C14 O6 51.7(7) . . . . ?
O1 Si1 C16 Si2 81.1(4) . . . . ?
C1 Si1 C16 Si2 -37.1(5) . . . . ?
C2 Si1 C16 Si2 -162.3(4) . . . . ?
Li1 Si1 C16 Si2 100.4(4) . . . . ?
O1 Si1 C16 Si3 -77.6(3) . . . . ?
C1 Si1 C16 Si3 164.3(3) . . . . ?
C2 Si1 C16 Si3 39.0(5) . . . . ?
Li1 Si1 C16 Si3 -58.3(3) . . . . ?
O3 Si2 C16 Si1 -92.8(4) . . . . ?
C6 Si2 C16 Si1 151.1(4) . . . . ?
C7 Si2 C16 Si1 29.4(5) . . . . ?
O3 Si2 C16 Si3 64.8(4) . . . . ?
C6 Si2 C16 Si3 -51.3(5) . . . . ?
C7 Si2 C16 Si3 -173.0(4) . . . . ?
O5 Si3 C16 Si1 39.2(4) . . . . ?
C12 Si3 C16 Si1 -78.9(4) . . . . ?
C11 Si3 C16 Si1 155.4(3) . . . . ?
O5 Si3 C16 Si2 -120.9(3) . . . . ?
C12 Si3 C16 Si2 121.0(4) . . . . ?
C11 Si3 C16 Si2 -4.7(5) . . . . ?
C3 O1 Li1 O4 120.5(7) . . . . ?
Si1 O1 Li1 O4 -84.5(7) . . . . ?
C3 O1 Li1 O5 -133.2(5) . . . . ?
Si1 O1 Li1 O5 21.8(5) . . . . ?
C3 O1 Li1 O6 -51.6(8) . . . . ?
Si1 O1 Li1 O6 103.4(6) . . . . ?
C3 O1 Li1 O2 30.2(5) . . . . ?
Si1 O1 Li1 O2 -174.8(3) . . . . ?
C3 O1 Li1 Si1 -155.0(6) . . . . ?
C9 O4 Li1 O1 -21.3(10) . . . . ?
C10 O4 Li1 O1 -176.0(6) . . . . ?
C9 O4 Li1 O5 -127.3(5) . . . . ?
C10 O4 Li1 O5 78.0(6) . . . . ?
C9 O4 Li1 O6 151.8(5) . . . . ?
C10 O4 Li1 O6 -2.9(7) . . . . ?
C9 O4 Li1 O2 58.9(7) . . . . ?
C10 O4 Li1 O2 -95.8(6) . . . . ?
C9 O4 Li1 Si1 -54.2(8) . . . . ?
C10 O4 Li1 Si1 151.0(5) . . . . ?
C13 O5 Li1 O1 133.7(5) . . . . ?
Si3 O5 Li1 O1 -62.3(5) . . . . ?
C13 O5 Li1 O4 -99.1(5) . . . . ?
Si3 O5 Li1 O4 65.0(5) . . . . ?
C13 O5 Li1 O6 9.4(5) . . . . ?
Si3 O5 Li1 O6 173.4(3) . . . . ?
C13 O5 Li1 O2 59(2) . . . . ?
Si3 O5 Li1 O2 -136.7(18) . . . . ?
C13 O5 Li1 Si1 144.6(4) . . . . ?
Si3 O5 Li1 Si1 -51.3(3) . . . . ?
C14 O6 Li1 O1 -71.9(8) . . . . ?
C15 O6 Li1 O1 64.3(9) . . . . ?
C14 O6 Li1 O4 115.0(6) . . . . ?
C15 O6 Li1 O4 -108.8(6) . . . . ?
C14 O6 Li1 O5 19.8(5) . . . . ?
C15 O6 Li1 O5 156.0(5) . . . . ?
C14 O6 Li1 O2 -147.3(4) . . . . ?
C15 O6 Li1 O2 -11.2(7) . . . . ?
C14 O6 Li1 Si1 -36.0(7) . . . . ?
C15 O6 Li1 Si1 100.1(6) . . . . ?
C4 O2 Li1 O1 -0.4(5) . . . . ?
C5 O2 Li1 O1 149.0(6) . . . . ?
C4 O2 Li1 O4 -124.7(5) . . . . ?
C5 O2 Li1 O4 24.7(8) . . . . ?
C4 O2 Li1 O5 77(2) . . . . ?
C5 O2 Li1 O5 -133.7(19) . . . . ?
C4 O2 Li1 O6 125.5(5) . . . . ?
C5 O2 Li1 O6 -85.2(7) . . . . ?
C4 O2 Li1 Si1 -3.0(6) . . . . ?
C5 O2 Li1 Si1 146.3(6) . . . . ?
C16 Si1 Li1 O1 -145.3(4) . . . . ?
C1 Si1 Li1 O1 -25.3(6) . . . . ?
C2 Si1 Li1 O1 98.5(4) . . . . ?
O1 Si1 Li1 O4 112.9(7) . . . . ?
C16 Si1 Li1 O4 -32.3(5) . . . . ?
C1 Si1 Li1 O4 87.7(6) . . . . ?
C2 Si1 Li1 O4 -148.6(5) . . . . ?
O1 Si1 Li1 O5 -157.1(6) . . . . ?
C16 Si1 Li1 O5 57.6(3) . . . . ?
C1 Si1 Li1 O5 177.7(4) . . . . ?
C2 Si1 Li1 O5 -58.6(4) . . . . ?
O1 Si1 Li1 O6 -98.0(7) . . . . ?
C16 Si1 Li1 O6 116.7(6) . . . . ?
C1 Si1 Li1 O6 -123.2(6) . . . . ?
C2 Si1 Li1 O6 0.5(6) . . . . ?
O1 Si1 Li1 O2 5.3(3) . . . . ?
C16 Si1 Li1 O2 -140.0(4) . . . . ?
C1 Si1 Li1 O2 -19.9(7) . . . . ?
C2 Si1 Li1 O2 103.8(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.069
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Na-5
_database_code_depnum_ccdc_archive 'CCDC 1000506'
_audit_update_record             
;
2014-05-01 deposited with the CCDC.
2016-10-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H39 Ge Na O6 Si3'
_chemical_formula_sum            'C15 H39 Ge Na O6 Si3'
_chemical_formula_weight         495.31

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'
Na Na 0.0362 0.0249 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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'

_cell_length_a                   15.729(2)
_cell_length_b                   9.9209(13)
_cell_length_c                   17.212(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.3515(14)
_cell_angle_gamma                90.00
_cell_volume                     2685.8(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9848
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      27.81

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1048
_exptl_absorpt_coefficient_mu    1.313
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6493
_exptl_absorpt_correction_T_max  0.8274
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31353
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.37
_diffrn_reflns_theta_max         27.88
_reflns_number_total             6374
_reflns_number_gt                5224
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0335P)²+0.5007P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6374
_refine_ls_number_parameters     244
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0266
_refine_ls_wR_factor_ref         0.0682
_refine_ls_wR_factor_gt          0.0645
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.245481(11) 0.614063(18) 0.076184(9) 0.03445(6) Uani 1 1 d . . .
Si1 Si 0.22948(3) 0.77856(4) 0.17523(3) 0.03209(10) Uani 1 1 d . . .
Si2 Si 0.14251(3) 0.45989(4) 0.12285(3) 0.03099(10) Uani 1 1 d . . .
Si3 Si 0.36871(3) 0.51060(5) 0.12904(3) 0.03581(11) Uani 1 1 d . . .
Na1 Na 0.24978(4) 0.49806(6) 0.30167(3) 0.02874(13) Uani 1 1 d . . .
O1 O 0.20892(7) 0.71222(11) 0.26278(6) 0.0380(3) Uani 1 1 d . . .
O2 O 0.15388(7) 0.58892(12) 0.39512(7) 0.0381(3) Uani 1 1 d . . .
O3 O 0.16905(7) 0.38796(11) 0.20827(6) 0.0358(3) Uani 1 1 d . . .
O4 O 0.22425(8) 0.27247(11) 0.34534(7) 0.0428(3) Uani 1 1 d . . .
O5 O 0.37279(7) 0.51557(14) 0.22712(6) 0.0433(3) Uani 1 1 d . . .
O6 O 0.36875(8) 0.50986(15) 0.38716(7) 0.0517(3) Uani 1 1 d . . .
C1 C 0.32566(12) 0.8884(2) 0.18918(12) 0.0511(5) Uani 1 1 d . . .
H1A H 0.3156 0.9516 0.2319 0.077 Uiso 1 1 calc R . .
H1B H 0.3365 0.9389 0.1413 0.077 Uiso 1 1 calc R . .
H1C H 0.3751 0.8320 0.2016 0.077 Uiso 1 1 calc R . .
C2 C 0.13775(13) 0.89556(19) 0.15381(13) 0.0549(5) Uani 1 1 d . . .
H2A H 0.1257 0.9502 0.1999 0.082 Uiso 1 1 calc R . .
H2B H 0.0873 0.8424 0.1401 0.082 Uiso 1 1 calc R . .
H2C H 0.1525 0.9548 0.1104 0.082 Uiso 1 1 calc R . .
C3 C 0.19660(12) 0.78851(17) 0.33220(10) 0.0441(4) Uani 1 1 d . . .
H3A H 0.1800 0.8820 0.3189 0.053 Uiso 1 1 calc R . .
H3B H 0.2502 0.7918 0.3626 0.053 Uiso 1 1 calc R . .
C4 C 0.12867(11) 0.72355(18) 0.37884(10) 0.0403(4) Uani 1 1 d . . .
H4A H 0.1203 0.7737 0.4279 0.048 Uiso 1 1 calc R . .
H4B H 0.0744 0.7239 0.3494 0.048 Uiso 1 1 calc R . .
C5 C 0.08962(14) 0.5171(2) 0.43551(12) 0.0608(6) Uani 1 1 d . . .
H5A H 0.0762 0.5644 0.4839 0.091 Uiso 1 1 calc R . .
H5B H 0.1100 0.4260 0.4476 0.091 Uiso 1 1 calc R . .
H5C H 0.0384 0.5113 0.4029 0.091 Uiso 1 1 calc R . .
C6 C 0.12598(13) 0.3150(2) 0.05346(11) 0.0540(5) Uani 1 1 d . . .
H6A H 0.1083 0.3499 0.0026 0.081 Uiso 1 1 calc R . .
H6B H 0.0818 0.2551 0.0736 0.081 Uiso 1 1 calc R . .
H6C H 0.1792 0.2647 0.0481 0.081 Uiso 1 1 calc R . .
C7 C 0.03490(11) 0.5369(2) 0.13806(13) 0.0544(5) Uani 1 1 d . . .
H7A H 0.0167 0.5831 0.0905 0.082 Uiso 1 1 calc R . .
H7B H 0.0379 0.6019 0.1809 0.082 Uiso 1 1 calc R . .
H7C H -0.0061 0.4660 0.1508 0.082 Uiso 1 1 calc R . .
C8 C 0.11920(11) 0.28894(17) 0.24668(11) 0.0421(4) Uani 1 1 d . . .
H8A H 0.0856 0.2371 0.2081 0.050 Uiso 1 1 calc R . .
H8B H 0.0792 0.3332 0.2828 0.050 Uiso 1 1 calc R . .
C9 C 0.17683(12) 0.19639(17) 0.29064(11) 0.0442(4) Uani 1 1 d . . .
H9A H 0.1429 0.1269 0.3178 0.053 Uiso 1 1 calc R . .
H9B H 0.2158 0.1503 0.2543 0.053 Uiso 1 1 calc R . .
C10 C 0.28585(15) 0.1921(2) 0.38458(13) 0.0644(6) Uani 1 1 d . . .
H10A H 0.2571 0.1202 0.4134 0.097 Uiso 1 1 calc R . .
H10B H 0.3184 0.2485 0.4208 0.097 Uiso 1 1 calc R . .
H10C H 0.3245 0.1521 0.3465 0.097 Uiso 1 1 calc R . .
C11 C 0.46762(12) 0.6001(2) 0.09516(13) 0.0588(6) Uani 1 1 d . . .
H11A H 0.4667 0.6068 0.0384 0.088 Uiso 1 1 calc R . .
H11B H 0.5179 0.5492 0.1118 0.088 Uiso 1 1 calc R . .
H11C H 0.4696 0.6907 0.1177 0.088 Uiso 1 1 calc R . .
C12 C 0.38187(13) 0.3288(2) 0.10146(13) 0.0597(5) Uani 1 1 d . . .
H12A H 0.3842 0.3210 0.0448 0.090 Uiso 1 1 calc R . .
H12B H 0.3336 0.2767 0.1210 0.090 Uiso 1 1 calc R . .
H12C H 0.4347 0.2939 0.1242 0.090 Uiso 1 1 calc R . .
C13 C 0.44427(13) 0.4734(3) 0.27107(12) 0.0723(8) Uani 1 1 d . . .
H13A H 0.4971 0.4957 0.2429 0.087 Uiso 1 1 calc R . .
H13B H 0.4423 0.3745 0.2787 0.087 Uiso 1 1 calc R . .
C14 C 0.44392(12) 0.5429(3) 0.34795(12) 0.0668(6) Uani 1 1 d . . .
H14A H 0.4938 0.5141 0.3791 0.080 Uiso 1 1 calc R . .
H14B H 0.4473 0.6416 0.3404 0.080 Uiso 1 1 calc R . .
C15 C 0.36443(18) 0.5634(4) 0.46335(13) 0.1013(11) Uani 1 1 d . . .
H15A H 0.4090 0.5226 0.4957 0.152 Uiso 1 1 calc R . .
H15B H 0.3086 0.5435 0.4856 0.152 Uiso 1 1 calc R . .
H15C H 0.3727 0.6613 0.4614 0.152 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 Si3 2.3699(5) . ?
Ge1 Si2 2.3714(5) . ?
Ge1 Si1 2.3745(5) . ?
Si1 O1 1.6776(11) . ?
Si1 C1 1.8786(18) . ?
Si1 C2 1.8865(19) . ?
Si2 O3 1.6845(12) . ?
Si2 C7 1.8769(18) . ?
Si2 C6 1.8858(19) . ?
Si3 O5 1.6897(12) . ?
Si3 C12 1.877(2) . ?
Si3 C11 1.8865(19) . ?
Na1 O3 2.3163(12) . ?
Na1 O1 2.3173(12) . ?
Na1 O5 2.3346(13) . ?
Na1 O6 2.3762(13) . ?
Na1 O2 2.3884(12) . ?
Na1 O4 2.3956(13) . ?
Na1 C3 3.0470(18) . ?
Na1 C8 3.0652(18) . ?
Na1 C13 3.117(2) . ?
O1 C3 1.4286(19) . ?
O2 C4 1.421(2) . ?
O2 C5 1.422(2) . ?
O3 C8 1.4223(19) . ?
O4 C9 1.416(2) . ?
O4 C10 1.423(2) . ?
O5 C13 1.415(2) . ?
O6 C14 1.404(2) . ?
O6 C15 1.417(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.487(2) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
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 C9 1.493(2) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
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 1.492(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?

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
Si3 Ge1 Si2 98.588(19) . . ?
Si3 Ge1 Si1 96.434(17) . . ?
Si2 Ge1 Si1 97.152(17) . . ?
O1 Si1 C1 105.81(8) . . ?
O1 Si1 C2 105.39(8) . . ?
C1 Si1 C2 106.40(9) . . ?
O1 Si1 Ge1 113.40(4) . . ?
C1 Si1 Ge1 113.68(7) . . ?
C2 Si1 Ge1 111.52(7) . . ?
O3 Si2 C7 105.64(8) . . ?
O3 Si2 C6 105.21(8) . . ?
C7 Si2 C6 106.12(9) . . ?
O3 Si2 Ge1 113.75(4) . . ?
C7 Si2 Ge1 113.77(7) . . ?
C6 Si2 Ge1 111.65(7) . . ?
O5 Si3 C12 106.10(9) . . ?
O5 Si3 C11 105.59(8) . . ?
C12 Si3 C11 106.35(10) . . ?
O5 Si3 Ge1 113.38(4) . . ?
C12 Si3 Ge1 114.22(7) . . ?
C11 Si3 Ge1 110.59(8) . . ?
O3 Na1 O1 94.70(5) . . ?
O3 Na1 O5 96.10(5) . . ?
O1 Na1 O5 90.13(5) . . ?
O3 Na1 O6 151.56(5) . . ?
O1 Na1 O6 110.47(5) . . ?
O5 Na1 O6 71.61(5) . . ?
O3 Na1 O2 107.43(5) . . ?
O1 Na1 O2 70.93(4) . . ?
O5 Na1 O2 150.57(5) . . ?
O6 Na1 O2 93.59(5) . . ?
O3 Na1 O4 71.64(4) . . ?
O1 Na1 O4 154.22(5) . . ?
O5 Na1 O4 112.52(5) . . ?
O6 Na1 O4 89.12(5) . . ?
O2 Na1 O4 91.92(5) . . ?
O3 Na1 C3 114.57(5) . . ?
O1 Na1 C3 26.72(4) . . ?
O5 Na1 C3 104.70(5) . . ?
O6 Na1 C3 93.59(5) . . ?
O2 Na1 C3 49.60(4) . . ?
O4 Na1 C3 141.51(5) . . ?
O3 Na1 C8 26.23(4) . . ?
O1 Na1 C8 110.32(5) . . ?
O5 Na1 C8 115.89(5) . . ?
O6 Na1 C8 138.43(5) . . ?
O2 Na1 C8 92.22(5) . . ?
O4 Na1 C8 49.55(4) . . ?
C3 Na1 C8 120.61(5) . . ?
O3 Na1 C13 112.34(6) . . ?
O1 Na1 C13 107.09(6) . . ?
O5 Na1 C13 25.23(5) . . ?
O6 Na1 C13 48.59(5) . . ?
O2 Na1 C13 140.17(6) . . ?
O4 Na1 C13 98.41(7) . . ?
C3 Na1 C13 111.97(7) . . ?
C8 Na1 C13 123.45(7) . . ?
C3 O1 Si1 124.84(10) . . ?
C3 O1 Na1 106.44(9) . . ?
Si1 O1 Na1 124.37(6) . . ?
C4 O2 C5 111.67(14) . . ?
C4 O2 Na1 113.49(9) . . ?
C5 O2 Na1 126.44(12) . . ?
C8 O3 Si2 124.32(10) . . ?
C8 O3 Na1 107.73(10) . . ?
Si2 O3 Na1 122.54(6) . . ?
C9 O4 C10 111.79(14) . . ?
C9 O4 Na1 112.22(9) . . ?
C10 O4 Na1 123.91(12) . . ?
C13 O5 Si3 123.42(11) . . ?
C13 O5 Na1 110.04(11) . . ?
Si3 O5 Na1 121.36(6) . . ?
C14 O6 C15 113.75(19) . . ?
C14 O6 Na1 112.10(10) . . ?
C15 O6 Na1 123.34(13) . . ?
Si1 C1 H1A 109.5 . . ?
Si1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Si1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O1 C3 C4 108.87(14) . . ?
O1 C3 Na1 46.84(7) . . ?
C4 C3 Na1 83.23(10) . . ?
O1 C3 H3A 109.9 . . ?
C4 C3 H3A 109.9 . . ?
Na1 C3 H3A 156.7 . . ?
O1 C3 H3B 109.9 . . ?
C4 C3 H3B 109.9 . . ?
Na1 C3 H3B 83.6 . . ?
H3A C3 H3B 108.3 . . ?
O2 C4 C3 108.26(13) . . ?
O2 C4 H4A 110.0 . . ?
C3 C4 H4A 110.0 . . ?
O2 C4 H4B 110.0 . . ?
C3 C4 H4B 110.0 . . ?
H4A C4 H4B 108.4 . . ?
O2 C5 H5A 109.5 . . ?
O2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
O2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O3 C8 C9 109.01(14) . . ?
O3 C8 Na1 46.04(7) . . ?
C9 C8 Na1 81.73(10) . . ?
O3 C8 H8A 109.9 . . ?
C9 C8 H8A 109.9 . . ?
Na1 C8 H8A 155.8 . . ?
O3 C8 H8B 109.9 . . ?
C9 C8 H8B 109.9 . . ?
Na1 C8 H8B 86.2 . . ?
H8A C8 H8B 108.3 . . ?
O4 C9 C8 108.96(14) . . ?
O4 C9 H9A 109.9 . . ?
C8 C9 H9A 109.9 . . ?
O4 C9 H9B 109.9 . . ?
C8 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
O4 C10 H10A 109.5 . . ?
O4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si3 C11 H11A 109.5 . . ?
Si3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si3 C12 H12A 109.5 . . ?
Si3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O5 C13 C14 109.30(18) . . ?
C14 C13 Na1 78.75(11) . . ?
O5 C13 H13A 109.8 . . ?
C14 C13 H13A 109.8 . . ?
Na1 C13 H13A 153.3 . . ?
O5 C13 H13B 109.8 . . ?
C14 C13 H13B 109.8 . . ?
Na1 C13 H13B 91.4 . . ?
H13A C13 H13B 108.3 . . ?
O6 C14 C13 109.05(18) . . ?
O6 C14 H14A 109.9 . . ?
C13 C14 H14A 109.9 . . ?
O6 C14 H14B 109.9 . . ?
C13 C14 H14B 109.9 . . ?
H14A C14 H14B 108.3 . . ?
O6 C15 H15A 109.5 . . ?
O6 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O6 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?

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
Si3 Ge1 Si1 O1 -64.17(5) . . . . ?
Si2 Ge1 Si1 O1 35.37(5) . . . . ?
Si3 Ge1 Si1 C1 56.76(8) . . . . ?
Si2 Ge1 Si1 C1 156.29(7) . . . . ?
Si3 Ge1 Si1 C2 177.05(8) . . . . ?
Si2 Ge1 Si1 C2 -83.42(8) . . . . ?
Si3 Ge1 Si2 O3 30.93(5) . . . . ?
Si1 Ge1 Si2 O3 -66.73(5) . . . . ?
Si3 Ge1 Si2 C7 151.96(8) . . . . ?
Si1 Ge1 Si2 C7 54.31(8) . . . . ?
Si3 Ge1 Si2 C6 -87.96(8) . . . . ?
Si1 Ge1 Si2 C6 174.39(7) . . . . ?
Si2 Ge1 Si3 O5 -66.84(6) . . . . ?
Si1 Ge1 Si3 O5 31.43(6) . . . . ?
Si2 Ge1 Si3 C12 54.88(8) . . . . ?
Si1 Ge1 Si3 C12 153.14(8) . . . . ?
Si2 Ge1 Si3 C11 174.79(7) . . . . ?
Si1 Ge1 Si3 C11 -86.95(7) . . . . ?
C1 Si1 O1 C3 54.67(15) . . . . ?
C2 Si1 O1 C3 -57.81(15) . . . . ?
Ge1 Si1 O1 C3 179.94(12) . . . . ?
C1 Si1 O1 Na1 -98.65(9) . . . . ?
C2 Si1 O1 Na1 148.87(9) . . . . ?
Ge1 Si1 O1 Na1 26.61(9) . . . . ?
O3 Na1 O1 C3 139.85(10) . . . . ?
O5 Na1 O1 C3 -124.02(10) . . . . ?
O6 Na1 O1 C3 -53.64(11) . . . . ?
O2 Na1 O1 C3 33.01(10) . . . . ?
O4 Na1 O1 C3 83.66(15) . . . . ?
C8 Na1 O1 C3 118.17(10) . . . . ?
C13 Na1 O1 C3 -105.05(11) . . . . ?
O3 Na1 O1 Si1 -62.75(8) . . . . ?
O5 Na1 O1 Si1 33.39(8) . . . . ?
O6 Na1 O1 Si1 103.76(8) . . . . ?
O2 Na1 O1 Si1 -169.58(9) . . . . ?
O4 Na1 O1 Si1 -118.93(11) . . . . ?
C3 Na1 O1 Si1 157.41(15) . . . . ?
C8 Na1 O1 Si1 -84.42(9) . . . . ?
C13 Na1 O1 Si1 52.36(9) . . . . ?
O3 Na1 O2 C4 -92.35(11) . . . . ?
O1 Na1 O2 C4 -3.36(10) . . . . ?
O5 Na1 O2 C4 49.22(15) . . . . ?
O6 Na1 O2 C4 107.07(11) . . . . ?
O4 Na1 O2 C4 -163.69(11) . . . . ?
C3 Na1 O2 C4 15.41(10) . . . . ?
C8 Na1 O2 C4 -114.11(11) . . . . ?
C13 Na1 O2 C4 90.72(14) . . . . ?
O3 Na1 O2 C5 52.87(15) . . . . ?
O1 Na1 O2 C5 141.86(15) . . . . ?
O5 Na1 O2 C5 -165.56(15) . . . . ?
O6 Na1 O2 C5 -107.71(15) . . . . ?
O4 Na1 O2 C5 -18.47(15) . . . . ?
C3 Na1 O2 C5 160.63(17) . . . . ?
C8 Na1 O2 C5 31.11(15) . . . . ?
C13 Na1 O2 C5 -124.06(16) . . . . ?
C7 Si2 O3 C8 56.78(15) . . . . ?
C6 Si2 O3 C8 -55.24(15) . . . . ?
Ge1 Si2 O3 C8 -177.74(11) . . . . ?
C7 Si2 O3 Na1 -94.04(9) . . . . ?
C6 Si2 O3 Na1 153.94(9) . . . . ?
Ge1 Si2 O3 Na1 31.44(8) . . . . ?
O1 Na1 O3 C8 -128.41(10) . . . . ?
O5 Na1 O3 C8 140.95(10) . . . . ?
O6 Na1 O3 C8 78.90(15) . . . . ?
O2 Na1 O3 C8 -56.94(10) . . . . ?
O4 Na1 O3 C8 29.21(10) . . . . ?
C3 Na1 O3 C8 -109.82(10) . . . . ?
C13 Na1 O3 C8 120.94(11) . . . . ?
O1 Na1 O3 Si2 26.58(8) . . . . ?
O5 Na1 O3 Si2 -64.06(8) . . . . ?
O6 Na1 O3 Si2 -126.11(10) . . . . ?
O2 Na1 O3 Si2 98.05(8) . . . . ?
O4 Na1 O3 Si2 -175.80(8) . . . . ?
C3 Na1 O3 Si2 45.17(9) . . . . ?
C8 Na1 O3 Si2 154.99(14) . . . . ?
C13 Na1 O3 Si2 -84.07(9) . . . . ?
O3 Na1 O4 C9 1.45(11) . . . . ?
O1 Na1 O4 C9 62.19(17) . . . . ?
O5 Na1 O4 C9 -87.61(11) . . . . ?
O6 Na1 O4 C9 -157.25(11) . . . . ?
O2 Na1 O4 C9 109.19(11) . . . . ?
C3 Na1 O4 C9 108.09(13) . . . . ?
C8 Na1 O4 C9 17.91(11) . . . . ?
C13 Na1 O4 C9 -109.39(11) . . . . ?
O3 Na1 O4 C10 140.73(15) . . . . ?
O1 Na1 O4 C10 -158.53(15) . . . . ?
O5 Na1 O4 C10 51.67(15) . . . . ?
O6 Na1 O4 C10 -17.97(15) . . . . ?
O2 Na1 O4 C10 -111.53(15) . . . . ?
C3 Na1 O4 C10 -112.63(16) . . . . ?
C8 Na1 O4 C10 157.19(17) . . . . ?
C13 Na1 O4 C10 29.89(15) . . . . ?
C12 Si3 O5 C13 60.9(2) . . . . ?
C11 Si3 O5 C13 -51.7(2) . . . . ?
Ge1 Si3 O5 C13 -172.96(17) . . . . ?
C12 Si3 O5 Na1 -91.14(10) . . . . ?
C11 Si3 O5 Na1 156.24(10) . . . . ?
Ge1 Si3 O5 Na1 35.02(9) . . . . ?
O3 Na1 O5 C13 -132.06(15) . . . . ?
O1 Na1 O5 C13 133.20(15) . . . . ?
O6 Na1 O5 C13 21.62(15) . . . . ?
O2 Na1 O5 C13 84.55(18) . . . . ?
O4 Na1 O5 C13 -59.44(16) . . . . ?
C3 Na1 O5 C13 110.53(15) . . . . ?
C8 Na1 O5 C13 -114.03(15) . . . . ?
O3 Na1 O5 Si3 23.31(9) . . . . ?
O1 Na1 O5 Si3 -71.44(8) . . . . ?
O6 Na1 O5 Si3 176.99(9) . . . . ?
O2 Na1 O5 Si3 -120.08(10) . . . . ?
O4 Na1 O5 Si3 95.93(8) . . . . ?
C3 Na1 O5 Si3 -94.10(9) . . . . ?
C8 Na1 O5 Si3 41.34(10) . . . . ?
C13 Na1 O5 Si3 155.37(19) . . . . ?
O3 Na1 O6 C14 77.61(19) . . . . ?
O1 Na1 O6 C14 -73.17(15) . . . . ?
O5 Na1 O6 C14 9.85(15) . . . . ?
O2 Na1 O6 C14 -144.15(15) . . . . ?
O4 Na1 O6 C14 123.98(15) . . . . ?
C3 Na1 O6 C14 -94.45(15) . . . . ?
C8 Na1 O6 C14 118.43(16) . . . . ?
C13 Na1 O6 C14 21.94(15) . . . . ?
O3 Na1 O6 C15 -140.5(2) . . . . ?
O1 Na1 O6 C15 68.8(2) . . . . ?
O5 Na1 O6 C15 151.8(2) . . . . ?
O2 Na1 O6 C15 -2.2(2) . . . . ?
O4 Na1 O6 C15 -94.1(2) . . . . ?
C3 Na1 O6 C15 47.5(2) . . . . ?
C8 Na1 O6 C15 -99.6(2) . . . . ?
C13 Na1 O6 C15 163.9(2) . . . . ?
Si1 O1 C3 C4 142.14(12) . . . . ?
Na1 O1 C3 C4 -60.58(15) . . . . ?
Si1 O1 C3 Na1 -157.27(15) . . . . ?
O3 Na1 C3 O1 -44.96(11) . . . . ?
O5 Na1 C3 O1 58.97(11) . . . . ?
O6 Na1 C3 O1 130.89(10) . . . . ?
O2 Na1 C3 O1 -137.45(13) . . . . ?
O4 Na1 C3 O1 -136.01(10) . . . . ?
C8 Na1 C3 O1 -73.85(11) . . . . ?
C13 Na1 C3 O1 84.46(11) . . . . ?
O3 Na1 C3 C4 78.93(11) . . . . ?
O1 Na1 C3 C4 123.90(16) . . . . ?
O5 Na1 C3 C4 -177.14(10) . . . . ?
O6 Na1 C3 C4 -105.21(11) . . . . ?
O2 Na1 C3 C4 -13.56(9) . . . . ?
O4 Na1 C3 C4 -12.11(15) . . . . ?
C8 Na1 C3 C4 50.04(12) . . . . ?
C13 Na1 C3 C4 -151.64(10) . . . . ?
C5 O2 C4 C3 -176.29(16) . . . . ?
Na1 O2 C4 C3 -25.88(16) . . . . ?
O1 C3 C4 O2 58.20(18) . . . . ?
Na1 C3 C4 O2 18.42(12) . . . . ?
Si2 O3 C8 C9 148.50(12) . . . . ?
Na1 O3 C8 C9 -57.07(15) . . . . ?
Si2 O3 C8 Na1 -154.43(14) . . . . ?
O1 Na1 C8 O3 56.38(10) . . . . ?
O5 Na1 C8 O3 -44.13(11) . . . . ?
O6 Na1 C8 O3 -135.22(10) . . . . ?
O2 Na1 C8 O3 126.85(10) . . . . ?
O4 Na1 C8 O3 -142.52(12) . . . . ?
C3 Na1 C8 O3 83.80(11) . . . . ?
C13 Na1 C8 O3 -71.95(11) . . . . ?
O3 Na1 C8 C9 126.68(16) . . . . ?
O1 Na1 C8 C9 -176.94(10) . . . . ?
O5 Na1 C8 C9 82.55(11) . . . . ?
O6 Na1 C8 C9 -8.53(14) . . . . ?
O2 Na1 C8 C9 -106.46(11) . . . . ?
O4 Na1 C8 C9 -15.83(10) . . . . ?
C3 Na1 C8 C9 -149.51(10) . . . . ?
C13 Na1 C8 C9 54.73(12) . . . . ?
C10 O4 C9 C8 -174.87(16) . . . . ?
Na1 O4 C9 C8 -30.54(17) . . . . ?
O3 C8 C9 O4 59.43(19) . . . . ?
Na1 C8 C9 O4 21.81(12) . . . . ?
Si3 O5 C13 C14 155.58(15) . . . . ?
Na1 O5 C13 C14 -49.7(2) . . . . ?
Si3 O5 C13 Na1 -154.76(19) . . . . ?
O3 Na1 C13 O5 52.95(16) . . . . ?
O1 Na1 C13 O5 -49.70(15) . . . . ?
O6 Na1 C13 O5 -152.21(19) . . . . ?
O2 Na1 C13 O5 -130.21(12) . . . . ?
O4 Na1 C13 O5 126.48(14) . . . . ?
C3 Na1 C13 O5 -77.63(15) . . . . ?
C8 Na1 C13 O5 79.98(16) . . . . ?
O3 Na1 C13 C14 -174.23(14) . . . . ?
O1 Na1 C13 C14 83.12(15) . . . . ?
O5 Na1 C13 C14 132.8(3) . . . . ?
O6 Na1 C13 C14 -19.40(13) . . . . ?
O2 Na1 C13 C14 2.6(2) . . . . ?
O4 Na1 C13 C14 -100.70(15) . . . . ?
C3 Na1 C13 C14 55.19(16) . . . . ?
C8 Na1 C13 C14 -147.21(14) . . . . ?
C15 O6 C14 C13 176.0(2) . . . . ?
Na1 O6 C14 C13 -38.3(2) . . . . ?
O5 C13 C14 O6 59.6(3) . . . . ?
Na1 C13 C14 O6 26.49(16) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.050
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_K-5
_database_code_depnum_ccdc_archive 'CCDC 1000507'
_audit_update_record             
;
2014-05-01 deposited with the CCDC.
2016-10-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H39 Ge K O6 Si3'
_chemical_formula_sum            'C15 H39 Ge K O6 Si3'
_chemical_formula_weight         511.42

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'
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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.141(2)
_cell_length_b                   19.245(6)
_cell_length_c                   16.727(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.528(4)
_cell_angle_gamma                90.00
_cell_volume                     2620.5(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7435
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      26.51

_exptl_crystal_description       chunk
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1080
_exptl_absorpt_coefficient_mu    1.489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6315
_exptl_absorpt_correction_T_max  0.7073
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27981
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.06
_diffrn_reflns_theta_max         27.91
_reflns_number_total             6104
_reflns_number_gt                5262
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The data were found to show twinning, with a twin law of
 -1 0 0 0 -1 0 0 0 1. The twin fraction refined to 0.20.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+40.7327P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6104
_refine_ls_number_parameters     245
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1094
_refine_ls_R_factor_gt           0.0960
_refine_ls_wR_factor_ref         0.2175
_refine_ls_wR_factor_gt          0.2123
_refine_ls_goodness_of_fit_ref   1.279
_refine_ls_restrained_S_all      1.279
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.95139(11) 0.10688(4) 0.75061(6) 0.0184(2) Uani 1 1 d . . .
K1 K 0.3953(2) 0.10996(9) 0.74738(13) 0.0201(4) Uani 1 1 d . . .
Si1 Si 0.8062(3) 0.04559(12) 0.64889(15) 0.0179(5) Uani 1 1 d . . .
Si2 Si 0.8076(4) 0.06449(12) 0.86287(14) 0.0178(5) Uani 1 1 d . . .
Si3 Si 0.8138(3) 0.21479(11) 0.73782(14) 0.0204(5) Uani 1 1 d . . .
O1 O 0.6171(8) 0.0216(3) 0.6750(4) 0.0210(14) Uani 1 1 d . . .
O2 O 0.3223(9) -0.0282(3) 0.7333(4) 0.0294(16) Uani 1 1 d . . .
O3 O 0.6174(8) 0.0974(4) 0.8702(4) 0.0263(15) Uani 1 1 d . . .
O4 O 0.3396(10) 0.1772(4) 0.8882(4) 0.0328(18) Uani 1 1 d . . .
O5 O 0.6234(9) 0.2082(3) 0.7014(5) 0.0302(17) Uani 1 1 d . . .
O6 O 0.3223(10) 0.1929(4) 0.6200(4) 0.0327(17) Uani 1 1 d . . .
C1 C 0.9229(14) -0.0374(6) 0.6247(8) 0.042(3) Uani 1 1 d . . .
H1A H 0.8674 -0.0617 0.5806 0.064 Uiso 1 1 calc R . .
H1B H 0.9260 -0.0675 0.6720 0.064 Uiso 1 1 calc R . .
H1C H 1.0353 -0.0257 0.6091 0.064 Uiso 1 1 calc R . .
C2 C 0.7778(14) 0.0944(6) 0.5520(6) 0.034(3) Uani 1 1 d . . .
H2A H 0.7150 0.0657 0.5142 0.051 Uiso 1 1 calc R . .
H2B H 0.8855 0.1051 0.5294 0.051 Uiso 1 1 calc R . .
H2C H 0.7181 0.1377 0.5620 0.051 Uiso 1 1 calc R . .
C3 C 0.5160(11) -0.0228(5) 0.6285(6) 0.0225(19) Uani 1 1 d . . .
H3A H 0.5846 -0.0509 0.5922 0.027 Uiso 1 1 calc R . .
H3B H 0.4390 0.0051 0.5956 0.027 Uiso 1 1 calc R . .
C4 C 0.4211(13) -0.0700(5) 0.6830(7) 0.029(2) Uani 1 1 d . . .
H4A H 0.3509 -0.1018 0.6511 0.034 Uiso 1 1 calc R . .
H4B H 0.4977 -0.0984 0.7157 0.034 Uiso 1 1 calc R . .
C5 C 0.2396(13) -0.0666(6) 0.7937(8) 0.039(3) Uani 1 1 d . . .
H5A H 0.1624 -0.0992 0.7686 0.058 Uiso 1 1 calc R . .
H5B H 0.1793 -0.0345 0.8282 0.058 Uiso 1 1 calc R . .
H5C H 0.3201 -0.0925 0.8258 0.058 Uiso 1 1 calc R . .
C6 C 0.9230(15) 0.0894(6) 0.9570(6) 0.032(2) Uani 1 1 d . . .
H6A H 0.8751 0.0653 1.0029 0.048 Uiso 1 1 calc R . .
H6B H 0.9152 0.1397 0.9651 0.048 Uiso 1 1 calc R . .
H6C H 1.0387 0.0761 0.9520 0.048 Uiso 1 1 calc R . .
C7 C 0.7807(15) -0.0327(5) 0.8666(6) 0.031(2) Uani 1 1 d . . .
H7A H 0.7174 -0.0452 0.9141 0.046 Uiso 1 1 calc R . .
H7B H 0.8887 -0.0551 0.8693 0.046 Uiso 1 1 calc R . .
H7C H 0.7220 -0.0483 0.8185 0.046 Uiso 1 1 calc R . .
C8 C 0.5129(13) 0.0887(6) 0.9375(6) 0.029(2) Uani 1 1 d . . .
H8A H 0.5781 0.0729 0.9843 0.035 Uiso 1 1 calc R . .
H8B H 0.4283 0.0531 0.9255 0.035 Uiso 1 1 calc R . .
C9 C 0.4326(14) 0.1564(6) 0.9557(6) 0.031(2) Uani 1 1 d . . .
H9A H 0.3601 0.1513 1.0025 0.037 Uiso 1 1 calc R . .
H9B H 0.5169 0.1918 0.9684 0.037 Uiso 1 1 calc R . .
C10 C 0.268(2) 0.2431(7) 0.8982(8) 0.059(4) Uani 1 1 d . . .
H10A H 0.1935 0.2420 0.9438 0.088 Uiso 1 1 calc R . .
H10B H 0.2063 0.2555 0.8497 0.088 Uiso 1 1 calc R . .
H10C H 0.3545 0.2776 0.9079 0.088 Uiso 1 1 calc R . .
C11 C 0.7939(17) 0.2650(5) 0.8337(6) 0.039(3) Uani 1 1 d . . .
H11A H 0.7138 0.3025 0.8263 0.059 Uiso 1 1 calc R . .
H11B H 0.9007 0.2848 0.8486 0.059 Uiso 1 1 calc R . .
H11C H 0.7567 0.2338 0.8762 0.059 Uiso 1 1 calc R . .
C12 C 0.9283(13) 0.2719(5) 0.6656(6) 0.028(2) Uani 1 1 d . . .
H12A H 0.8820 0.3189 0.6666 0.043 Uiso 1 1 calc R . .
H12B H 0.9179 0.2528 0.6115 0.043 Uiso 1 1 calc R . .
H12C H 1.0446 0.2738 0.6811 0.043 Uiso 1 1 calc R . .
C13 C 0.5225(14) 0.2653(5) 0.6802(8) 0.041(3) Uani 1 1 d . . .
H13A H 0.5917 0.3068 0.6716 0.049 Uiso 1 1 calc R . .
H13B H 0.4462 0.2755 0.7245 0.049 Uiso 1 1 calc R . .
C14 C 0.4260(14) 0.2499(6) 0.6058(7) 0.039(3) Uani 1 1 d . . .
H14A H 0.3597 0.2910 0.5903 0.047 Uiso 1 1 calc R . .
H14B H 0.5015 0.2391 0.5614 0.047 Uiso 1 1 calc R . .
C15 C 0.2468(18) 0.1661(8) 0.5501(7) 0.053(4) Uani 1 1 d . . .
H15A H 0.1794 0.2023 0.5250 0.080 Uiso 1 1 calc R . .
H15B H 0.1771 0.1265 0.5642 0.080 Uiso 1 1 calc R . .
H15C H 0.3316 0.1508 0.5128 0.080 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 Si2 2.367(3) . ?
Ge1 Si3 2.369(3) . ?
Ge1 Si1 2.376(3) . ?
K1 O6 2.723(7) . ?
K1 O4 2.730(7) . ?
K1 O2 2.735(6) . ?
K1 O3 2.735(7) . ?
K1 O5 2.764(7) . ?
K1 O1 2.767(7) . ?
Si1 O1 1.669(7) . ?
Si1 C2 1.886(11) . ?
Si1 C1 1.904(10) . ?
Si2 O3 1.678(7) . ?
Si2 C7 1.884(9) . ?
Si2 C6 1.889(10) . ?
Si3 O5 1.664(8) . ?
Si3 C11 1.881(10) . ?
Si3 C12 1.887(9) . ?
O1 C3 1.415(11) . ?
O2 C4 1.419(11) . ?
O2 C5 1.425(12) . ?
O3 C8 1.427(11) . ?
O4 C10 1.405(14) . ?
O4 C9 1.411(13) . ?
O5 C13 1.414(12) . ?
O6 C14 1.407(13) . ?
O6 C15 1.413(14) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.505(14) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
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 C9 1.490(15) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
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 1.496(18) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?

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
Si2 Ge1 Si3 97.86(9) . . ?
Si2 Ge1 Si1 98.66(9) . . ?
Si3 Ge1 Si1 97.97(10) . . ?
O6 K1 O4 111.1(2) . . ?
O6 K1 O2 117.2(2) . . ?
O4 K1 O2 119.8(2) . . ?
O6 K1 O3 141.0(2) . . ?
O4 K1 O3 60.5(2) . . ?
O2 K1 O3 96.9(2) . . ?
O6 K1 O5 61.6(2) . . ?
O4 K1 O5 91.9(2) . . ?
O2 K1 O5 141.9(2) . . ?
O3 K1 O5 80.1(2) . . ?
O6 K1 O1 99.0(2) . . ?
O4 K1 O1 141.6(2) . . ?
O2 K1 O1 60.5(2) . . ?
O3 K1 O1 81.1(2) . . ?
O5 K1 O1 81.71(19) . . ?
O6 K1 C8 151.2(3) . . ?
O4 K1 C8 44.3(2) . . ?
O2 K1 C8 91.3(2) . . ?
O3 K1 C8 24.7(2) . . ?
O5 K1 C8 99.3(3) . . ?
O1 K1 C8 99.2(2) . . ?
O1 Si1 C2 104.9(4) . . ?
O1 Si1 C1 106.7(5) . . ?
C2 Si1 C1 107.0(6) . . ?
O1 Si1 Ge1 113.8(2) . . ?
C2 Si1 Ge1 115.1(4) . . ?
C1 Si1 Ge1 108.8(4) . . ?
O3 Si2 C7 105.3(5) . . ?
O3 Si2 C6 107.2(5) . . ?
C7 Si2 C6 106.3(5) . . ?
O3 Si2 Ge1 113.0(2) . . ?
C7 Si2 Ge1 115.3(3) . . ?
C6 Si2 Ge1 109.2(4) . . ?
O5 Si3 C11 105.3(5) . . ?
O5 Si3 C12 105.9(5) . . ?
C11 Si3 C12 107.1(5) . . ?
O5 Si3 Ge1 113.9(2) . . ?
C11 Si3 Ge1 114.7(4) . . ?
C12 Si3 Ge1 109.4(3) . . ?
C3 O1 Si1 123.9(6) . . ?
C3 O1 K1 103.5(5) . . ?
Si1 O1 K1 123.5(3) . . ?
C4 O2 C5 113.6(7) . . ?
C4 O2 K1 118.6(5) . . ?
C5 O2 K1 123.1(6) . . ?
C8 O3 Si2 124.8(6) . . ?
C8 O3 K1 102.0(6) . . ?
Si2 O3 K1 125.6(3) . . ?
C10 O4 C9 112.4(9) . . ?
C10 O4 K1 127.0(7) . . ?
C9 O4 K1 117.6(6) . . ?
C13 O5 Si3 124.7(7) . . ?
C13 O5 K1 102.1(6) . . ?
Si3 O5 K1 125.2(4) . . ?
C14 O6 C15 113.7(9) . . ?
C14 O6 K1 117.6(7) . . ?
C15 O6 K1 121.6(8) . . ?
Si1 C1 H1A 109.5 . . ?
Si1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Si1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O1 C3 C4 109.4(8) . . ?
O1 C3 H3A 109.8 . . ?
C4 C3 H3A 109.8 . . ?
O1 C3 H3B 109.8 . . ?
C4 C3 H3B 109.8 . . ?
H3A C3 H3B 108.2 . . ?
O2 C4 C3 108.3(7) . . ?
O2 C4 H4A 110.0 . . ?
C3 C4 H4A 110.0 . . ?
O2 C4 H4B 110.0 . . ?
C3 C4 H4B 110.0 . . ?
H4A C4 H4B 108.4 . . ?
O2 C5 H5A 109.5 . . ?
O2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
O2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O3 C8 C9 108.9(8) . . ?
O3 C8 H8A 109.9 . . ?
C9 C8 H8A 109.9 . . ?
O3 C8 H8B 109.9 . . ?
C9 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
O4 C9 C8 108.5(8) . . ?
O4 C9 H9A 110.0 . . ?
C8 C9 H9A 110.0 . . ?
O4 C9 H9B 110.0 . . ?
C8 C9 H9B 110.0 . . ?
H9A C9 H9B 108.4 . . ?
O4 C10 H10A 109.5 . . ?
O4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si3 C11 H11A 109.5 . . ?
Si3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si3 C12 H12A 109.5 . . ?
Si3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O5 C13 C14 110.8(9) . . ?
O5 C13 H13A 109.5 . . ?
C14 C13 H13A 109.5 . . ?
O5 C13 H13B 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 108.1 . . ?
O6 C14 C13 108.9(8) . . ?
O6 C14 H14A 109.9 . . ?
C13 C14 H14A 109.9 . . ?
O6 C14 H14B 109.9 . . ?
C13 C14 H14B 109.9 . . ?
H14A C14 H14B 108.3 . . ?
O6 C15 H15A 109.5 . . ?
O6 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O6 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?

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
Si2 Ge1 Si1 O1 23.8(3) . . . . ?
Si3 Ge1 Si1 O1 -75.5(3) . . . . ?
Si2 Ge1 Si1 C2 144.9(4) . . . . ?
Si3 Ge1 Si1 C2 45.6(4) . . . . ?
Si2 Ge1 Si1 C1 -95.0(5) . . . . ?
Si3 Ge1 Si1 C1 165.7(5) . . . . ?
Si3 Ge1 Si2 O3 26.8(3) . . . . ?
Si1 Ge1 Si2 O3 -72.6(3) . . . . ?
Si3 Ge1 Si2 C7 148.0(4) . . . . ?
Si1 Ge1 Si2 C7 48.7(4) . . . . ?
Si3 Ge1 Si2 C6 -92.4(4) . . . . ?
Si1 Ge1 Si2 C6 168.2(4) . . . . ?
Si2 Ge1 Si3 O5 -73.5(3) . . . . ?
Si1 Ge1 Si3 O5 26.4(3) . . . . ?
Si2 Ge1 Si3 C11 47.9(4) . . . . ?
Si1 Ge1 Si3 C11 147.8(4) . . . . ?
Si2 Ge1 Si3 C12 168.2(4) . . . . ?
Si1 Ge1 Si3 C12 -91.9(4) . . . . ?
C2 Si1 O1 C3 61.8(8) . . . . ?
C1 Si1 O1 C3 -51.5(9) . . . . ?
Ge1 Si1 O1 C3 -171.6(6) . . . . ?
C2 Si1 O1 K1 -79.5(5) . . . . ?
C1 Si1 O1 K1 167.2(5) . . . . ?
Ge1 Si1 O1 K1 47.1(4) . . . . ?
O6 K1 O1 C3 -75.9(5) . . . . ?
O4 K1 O1 C3 142.2(5) . . . . ?
O2 K1 O1 C3 40.3(5) . . . . ?
O3 K1 O1 C3 143.5(5) . . . . ?
O5 K1 O1 C3 -135.3(5) . . . . ?
O6 K1 O1 Si1 71.8(4) . . . . ?
O4 K1 O1 Si1 -70.1(5) . . . . ?
O2 K1 O1 Si1 -172.0(5) . . . . ?
O3 K1 O1 Si1 -68.8(4) . . . . ?
O5 K1 O1 Si1 12.5(4) . . . . ?
O6 K1 O2 C4 72.9(7) . . . . ?
O4 K1 O2 C4 -147.4(7) . . . . ?
O3 K1 O2 C4 -87.6(7) . . . . ?
O5 K1 O2 C4 -4.8(9) . . . . ?
O1 K1 O2 C4 -12.0(6) . . . . ?
O6 K1 O2 C5 -132.9(7) . . . . ?
O4 K1 O2 C5 6.8(8) . . . . ?
O3 K1 O2 C5 66.6(8) . . . . ?
O5 K1 O2 C5 149.4(7) . . . . ?
O1 K1 O2 C5 142.2(8) . . . . ?
C7 Si2 O3 C8 62.6(9) . . . . ?
C6 Si2 O3 C8 -50.3(9) . . . . ?
Ge1 Si2 O3 C8 -170.6(7) . . . . ?
C7 Si2 O3 K1 -81.4(5) . . . . ?
C6 Si2 O3 K1 165.7(4) . . . . ?
Ge1 Si2 O3 K1 45.3(5) . . . . ?
O6 K1 O3 C8 130.2(6) . . . . ?
O4 K1 O3 C8 42.5(5) . . . . ?
O2 K1 O3 C8 -78.0(6) . . . . ?
O5 K1 O3 C8 140.4(6) . . . . ?
O1 K1 O3 C8 -136.6(6) . . . . ?
O6 K1 O3 Si2 -79.4(5) . . . . ?
O4 K1 O3 Si2 -167.0(5) . . . . ?
O2 K1 O3 Si2 72.5(4) . . . . ?
O5 K1 O3 Si2 -69.2(4) . . . . ?
O1 K1 O3 Si2 13.9(4) . . . . ?
O6 K1 O4 C10 5.9(11) . . . . ?
O2 K1 O4 C10 -136.0(10) . . . . ?
O3 K1 O4 C10 143.6(11) . . . . ?
O5 K1 O4 C10 66.1(10) . . . . ?
O1 K1 O4 C10 145.1(10) . . . . ?
O6 K1 O4 C9 -153.0(7) . . . . ?
O2 K1 O4 C9 65.1(7) . . . . ?
O3 K1 O4 C9 -15.4(6) . . . . ?
O5 K1 O4 C9 -92.9(7) . . . . ?
O1 K1 O4 C9 -13.8(9) . . . . ?
C11 Si3 O5 C13 60.6(10) . . . . ?
C12 Si3 O5 C13 -52.7(10) . . . . ?
Ge1 Si3 O5 C13 -172.9(8) . . . . ?
C11 Si3 O5 K1 -82.6(5) . . . . ?
C12 Si3 O5 K1 164.1(4) . . . . ?
Ge1 Si3 O5 K1 43.8(5) . . . . ?
O6 K1 O5 C13 38.5(7) . . . . ?
O4 K1 O5 C13 -74.6(7) . . . . ?
O2 K1 O5 C13 137.2(7) . . . . ?
O3 K1 O5 C13 -134.2(7) . . . . ?
O1 K1 O5 C13 143.5(7) . . . . ?
O6 K1 O5 Si3 -171.7(5) . . . . ?
O4 K1 O5 Si3 75.2(4) . . . . ?
O2 K1 O5 Si3 -73.0(6) . . . . ?
O3 K1 O5 Si3 15.5(4) . . . . ?
O1 K1 O5 Si3 -66.8(4) . . . . ?
O4 K1 O6 C14 69.8(7) . . . . ?
O2 K1 O6 C14 -147.3(6) . . . . ?
O3 K1 O6 C14 1.0(8) . . . . ?
O5 K1 O6 C14 -10.5(6) . . . . ?
O1 K1 O6 C14 -85.9(7) . . . . ?
O4 K1 O6 C15 -141.7(8) . . . . ?
O2 K1 O6 C15 1.3(9) . . . . ?
O3 K1 O6 C15 149.5(8) . . . . ?
O5 K1 O6 C15 138.0(9) . . . . ?
O1 K1 O6 C15 62.6(8) . . . . ?
Si1 O1 C3 C4 142.3(7) . . . . ?
K1 O1 C3 C4 -70.1(7) . . . . ?
Si1 O1 C3 K1 -147.6(7) . . . . ?
O6 K1 C3 O1 106.4(5) . . . . ?
O4 K1 C3 O1 -71.1(8) . . . . ?
O2 K1 C3 O1 -125.8(7) . . . . ?
O3 K1 C3 O1 -36.7(5) . . . . ?
O5 K1 C3 O1 44.8(5) . . . . ?
O6 K1 C3 C4 -136.2(6) . . . . ?
O4 K1 C3 C4 46.3(9) . . . . ?
O2 K1 C3 C4 -8.5(5) . . . . ?
O3 K1 C3 C4 80.7(6) . . . . ?
O5 K1 C3 C4 162.2(6) . . . . ?
O1 K1 C3 C4 117.4(9) . . . . ?
C5 O2 C4 C3 -173.6(9) . . . . ?
K1 O2 C4 C3 -17.0(10) . . . . ?
O1 C3 C4 O2 60.4(10) . . . . ?
Si2 O3 C8 C9 136.8(8) . . . . ?
K1 O3 C8 C9 -72.4(8) . . . . ?
Si2 O3 C8 K1 -150.8(8) . . . . ?
O6 K1 C8 O3 -84.9(7) . . . . ?
O4 K1 C8 O3 -122.7(7) . . . . ?
O2 K1 C8 O3 103.8(5) . . . . ?
O5 K1 C8 O3 -39.5(6) . . . . ?
O1 K1 C8 O3 43.5(6) . . . . ?
O6 K1 C8 C9 30.7(9) . . . . ?
O4 K1 C8 C9 -7.1(5) . . . . ?
O2 K1 C8 C9 -140.7(6) . . . . ?
O3 K1 C8 C9 115.5(9) . . . . ?
O5 K1 C8 C9 76.0(6) . . . . ?
O1 K1 C8 C9 159.0(6) . . . . ?
C10 O4 C9 C8 -176.0(10) . . . . ?
K1 O4 C9 C8 -14.1(10) . . . . ?
O3 C8 C9 O4 60.1(11) . . . . ?
Si3 O5 C13 C14 141.0(7) . . . . ?
K1 O5 C13 C14 -69.0(9) . . . . ?
Si3 O5 C13 K1 -149.9(9) . . . . ?
O6 K1 C13 O5 -128.2(8) . . . . ?
O4 K1 C13 O5 104.8(7) . . . . ?
O2 K1 C13 O5 -78.1(10) . . . . ?
O3 K1 C13 O5 45.4(7) . . . . ?
O1 K1 C13 O5 -36.9(7) . . . . ?
O6 K1 C13 C14 -9.2(5) . . . . ?
O4 K1 C13 C14 -136.1(6) . . . . ?
O2 K1 C13 C14 40.9(9) . . . . ?
O3 K1 C13 C14 164.4(6) . . . . ?
O5 K1 C13 C14 119.0(10) . . . . ?
O1 K1 C13 C14 82.1(6) . . . . ?
C15 O6 C14 C13 -169.4(10) . . . . ?
K1 O6 C14 C13 -18.5(10) . . . . ?
O5 C13 C14 O6 62.0(11) . . . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.152
_refine_diff_density_min         -2.425
_refine_diff_density_rms         0.165
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_K-1
_database_code_depnum_ccdc_archive 'CCDC 1013011'
_audit_update_record             
;
2014-07-09 deposited with the CCDC.
2016-10-07 downloaded from the CCDC.
;

_audit_creation_date             2014-06-04T13:39:43-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_sum            'C16 H39 K O6 Si3'
_chemical_formula_weight         450.84

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.698(6)
_cell_length_b                   18.417(12)
_cell_length_c                   16.289(11)
_cell_angle_alpha                90
_cell_angle_beta                 90.200(10)
_cell_angle_gamma                90
_cell_volume                     2609(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7089
_cell_measurement_theta_min      2.14
_cell_measurement_theta_max      25.7

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       blocky
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.145
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_F_000             976
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.365
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_correction_T_min  0.6086
_exptl_absorpt_correction_T_max  0.7452

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.1401
_diffrn_reflns_number            26816
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.106
_diffrn_reflns_theta_max         25.816
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.99
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.99
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.99
_reflns_number_total             4942
_reflns_number_gt                3052
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          Twin
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1045P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef       0.0196(19)
_refine_ls_number_reflns         4942
_refine_ls_number_parameters     237
_refine_ls_number_restraints     369
_refine_ls_R_factor_all          0.1153
_refine_ls_R_factor_gt           0.0699
_refine_ls_wR_factor_ref         0.1863
_refine_ls_wR_factor_gt          0.1627
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_restrained_S_all      0.908
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.11

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
O O 0.0106 0.006 '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'

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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.45141(19) 0.45687(6) 0.24271(8) 0.0366(4) Uani 1 d . .
Si1 Si 0.5385(2) 0.28180(8) 0.32518(10) 0.0354(5) Uani 1 d . .
Si2 Si 0.8208(2) 0.37284(8) 0.28003(10) 0.0358(5) Uani 1 d . .
Si3 Si 0.6251(2) 0.30427(8) 0.14096(10) 0.0376(5) Uani 1 d . .
O1 O 0.6025(6) 0.5881(2) 0.2682(3) 0.0593(14) Uani 1 d . .
O2 O 0.7641(5) 0.45683(19) 0.2480(3) 0.0392(10) Uani 1 d . .
O3 O 0.4534(5) 0.35730(19) 0.3630(2) 0.0362(10) Uani 1 d . .
O4 O 0.4750(6) 0.3613(2) 0.1195(2) 0.0397(11) Uani 1 d . .
O5 O 0.2915(6) 0.4846(2) 0.0942(3) 0.0476(12) Uani 1 d . .
O6 O 0.2553(5) 0.4751(2) 0.3760(2) 0.0417(11) Uani 1 d . .
C1 C 0.6720(8) 0.3099(3) 0.2492(4) 0.0343(13) Uani 1 d . .
C2 C 0.4325(9) 0.3844(3) 0.0396(4) 0.0452(17) Uani 1 d . .
H2A H 0.4258 0.3428 0.0034 0.054 Uiso 1 calc . .
H2B H 0.5102 0.4171 0.0182 0.054 Uiso 1 calc . .
C3 C 0.2789(9) 0.4229(3) 0.0423(4) 0.0466(17) Uani 1 d . .
H3A H 0.249 0.4379 -0.0125 0.056 Uiso 1 calc . .
H3B H 0.2007 0.3902 0.0632 0.056 Uiso 1 calc . .
C4 C 1.0180(7) 0.3590(3) 0.2404(4) 0.0424(16) Uani 1 d . .
H4A H 1.0547 0.3121 0.2571 0.064 Uiso 1 calc . .
H4B H 1.0168 0.3618 0.1816 0.064 Uiso 1 calc . .
H4C H 1.0846 0.3959 0.2621 0.064 Uiso 1 calc . .
C5 C 0.6180(9) 0.2325(3) 0.4181(4) 0.0510(19) Uani 1 d . .
H5A H 0.6683 0.1887 0.4008 0.076 Uiso 1 calc . .
H5B H 0.6906 0.2632 0.4459 0.076 Uiso 1 calc . .
H5C H 0.5355 0.2206 0.4546 0.076 Uiso 1 calc . .
C6 C 0.2189(10) 0.5487(3) 0.3955(5) 0.055(2) Uani 1 d . .
H6A H 0.1876 0.5737 0.3465 0.082 Uiso 1 calc . .
H6B H 0.1367 0.5497 0.4347 0.082 Uiso 1 calc . .
H6C H 0.3079 0.5721 0.4184 0.082 Uiso 1 calc . .
C7 C 0.3032(9) 0.4345(3) 0.4472(4) 0.0422(17) Uani 1 d . .
H7A H 0.2232 0.4356 0.4885 0.051 Uiso 1 calc . .
H7B H 0.3955 0.4559 0.4705 0.051 Uiso 1 calc . .
C8 C 0.3342(9) 0.3579(3) 0.4218(4) 0.0448(17) Uani 1 d . .
H8A H 0.3642 0.3294 0.4693 0.054 Uiso 1 calc . .
H8B H 0.2418 0.3366 0.3985 0.054 Uiso 1 calc . .
C9 C 0.7529(9) 0.5854(3) 0.2377(5) 0.0515(17) Uani 1 d . .
H9A H 0.806 0.6301 0.2512 0.062 Uiso 1 calc . .
H9B H 0.7498 0.581 0.1783 0.062 Uiso 1 calc . .
C10 C 0.5628(10) 0.2127(3) 0.0996(4) 0.054(2) Uani 1 d . .
H10A H 0.6424 0.1776 0.1096 0.081 Uiso 1 calc . .
H10B H 0.4702 0.1976 0.1266 0.081 Uiso 1 calc . .
H10C H 0.5443 0.2164 0.0416 0.081 Uiso 1 calc . .
C11 C 0.1474(10) 0.5231(4) 0.0973(4) 0.057(2) Uani 1 d . .
H11A H 0.1576 0.5646 0.1325 0.086 Uiso 1 calc . .
H11B H 0.1195 0.5387 0.043 0.086 Uiso 1 calc . .
H11C H 0.069 0.4915 0.1183 0.086 Uiso 1 calc . .
C12 C 0.8373(9) 0.5235(3) 0.2726(4) 0.0510(18) Uani 1 d . .
H12A H 0.9428 0.5241 0.2535 0.061 Uiso 1 calc . .
H12B H 0.8385 0.527 0.332 0.061 Uiso 1 calc . .
C13 C 0.5193(10) 0.6501(4) 0.2385(7) 0.096(4) Uani 1 d . .
H13A H 0.4173 0.6499 0.2608 0.144 Uiso 1 calc . .
H13B H 0.5714 0.6937 0.2551 0.144 Uiso 1 calc . .
H13C H 0.5136 0.6483 0.1796 0.144 Uiso 1 calc . .
C14 C 0.3763(9) 0.2231(3) 0.2871(4) 0.0457(17) Uani 1 d . .
H14A H 0.4171 0.179 0.2647 0.069 Uiso 1 calc . .
H14B H 0.3089 0.2118 0.3319 0.069 Uiso 1 calc . .
H14C H 0.3199 0.2486 0.2454 0.069 Uiso 1 calc . .
C15 C 0.7795(9) 0.3328(4) 0.0703(4) 0.0498(18) Uani 1 d . .
H15A H 0.8685 0.3029 0.0789 0.075 Uiso 1 calc . .
H15B H 0.7447 0.3278 0.0146 0.075 Uiso 1 calc . .
H15C H 0.8055 0.3827 0.0807 0.075 Uiso 1 calc . .
C16 C 0.8522(10) 0.3818(4) 0.3948(4) 0.0526(19) Uani 1 d . .
H16A H 0.8846 0.336 0.4168 0.079 Uiso 1 calc . .
H16B H 0.93 0.4177 0.4052 0.079 Uiso 1 calc . .
H16C H 0.7579 0.3964 0.4204 0.079 Uiso 1 calc . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
K1 O4 2.678(4) . ?
K1 O3 2.684(4) . ?
K1 O2 2.721(5) . ?
K1 O1 2.781(5) . ?
K1 O6 2.786(5) . ?
K1 O5 2.832(5) . ?
Si1 O3 1.692(4) . ?
Si1 C1 1.777(6) . ?
Si1 C14 1.881(7) . ?
Si1 C5 1.894(7) . ?
Si2 O2 1.705(4) . ?
Si2 C1 1.807(6) . ?
Si2 C4 1.852(7) . ?
Si2 C16 1.895(7) . ?
Si3 O4 1.711(5) . ?
Si3 C1 1.811(6) . ?
Si3 C15 1.848(7) . ?
Si3 C10 1.895(6) . ?
O1 C9 1.402(9) . ?
O1 C13 1.435(8) . ?
O2 C12 1.439(7) . ?
O3 C8 1.415(7) . ?
O4 C2 1.417(7) . ?
O5 C3 1.421(7) . ?
O5 C11 1.441(9) . ?
O6 C6 1.427(7) . ?
O6 C7 1.440(7) . ?
C2 C3 1.513(10) . ?
C2 H2A 0.97 . ?
C2 H2B 0.97 . ?
C3 H3A 0.97 . ?
C3 H3B 0.97 . ?
C4 H4A 0.96 . ?
C4 H4B 0.96 . ?
C4 H4C 0.96 . ?
C5 H5A 0.96 . ?
C5 H5B 0.96 . ?
C5 H5C 0.96 . ?
C6 H6A 0.96 . ?
C6 H6B 0.96 . ?
C6 H6C 0.96 . ?
C7 C8 1.495(8) . ?
C7 H7A 0.97 . ?
C7 H7B 0.97 . ?
C8 H8A 0.97 . ?
C8 H8B 0.97 . ?
C9 C12 1.470(9) . ?
C9 H9A 0.97 . ?
C9 H9B 0.97 . ?
C10 H10A 0.96 . ?
C10 H10B 0.96 . ?
C10 H10C 0.96 . ?
C11 H11A 0.96 . ?
C11 H11B 0.96 . ?
C11 H11C 0.96 . ?
C12 H12A 0.97 . ?
C12 H12B 0.97 . ?
C13 H13A 0.96 . ?
C13 H13B 0.96 . ?
C13 H13C 0.96 . ?
C14 H14A 0.96 . ?
C14 H14B 0.96 . ?
C14 H14C 0.96 . ?
C15 H15A 0.96 . ?
C15 H15B 0.96 . ?
C15 H15C 0.96 . ?
C16 H16A 0.96 . ?
C16 H16B 0.96 . ?
C16 H16C 0.96 . ?

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
O4 K1 O3 95.62(13) . . ?
O4 K1 O2 86.82(14) . . ?
O3 K1 O2 88.43(14) . . ?
O4 K1 O1 130.20(16) . . ?
O3 K1 O1 118.88(15) . . ?
O2 K1 O1 61.57(13) . . ?
O4 K1 O6 135.40(14) . . ?
O3 K1 O6 61.05(13) . . ?
O2 K1 O6 126.15(14) . . ?
O1 K1 O6 93.97(14) . . ?
O4 K1 O5 61.13(13) . . ?
O3 K1 O5 138.48(14) . . ?
O2 K1 O5 121.00(15) . . ?
O1 K1 O5 101.59(15) . . ?
O6 K1 O5 110.09(15) . . ?
O4 K1 C1 56.09(14) . . ?
O3 K1 C1 54.36(14) . . ?
O2 K1 C1 54.62(13) . . ?
O1 K1 C1 115.54(16) . . ?
O6 K1 C1 115.41(13) . . ?
O5 K1 C1 117.15(14) . . ?
O4 K1 C9 111.34(17) . . ?
O3 K1 C9 118.14(16) . . ?
O2 K1 C9 42.19(14) . . ?
O1 K1 C9 21.76(15) . . ?
O6 K1 C9 113.19(16) . . ?
O5 K1 C9 102.80(16) . . ?
C1 K1 C9 96.77(17) . . ?
O4 K1 Si1 70.86(10) . . ?
O3 K1 Si1 26.89(9) . . ?
O2 K1 Si1 77.12(9) . . ?
O1 K1 Si1 128.95(12) . . ?
O6 K1 Si1 86.88(9) . . ?
O5 K1 Si1 125.92(10) . . ?
C1 K1 Si1 29.59(11) . . ?
C9 K1 Si1 117.17(13) . . ?
O4 K1 Si3 26.88(10) . . ?
O3 K1 Si3 78.52(10) . . ?
O2 K1 Si3 65.99(9) . . ?
O1 K1 Si3 123.26(12) . . ?
O6 K1 Si3 135.43(9) . . ?
O5 K1 Si3 87.32(11) . . ?
C1 K1 Si3 30.00(11) . . ?
C9 K1 Si3 101.51(13) . . ?
Si1 K1 Si3 51.65(6) . . ?
O4 K1 Si2 76.96(11) . . ?
O3 K1 Si2 65.24(11) . . ?
O2 K1 Si2 26.75(8) . . ?
O1 K1 Si2 85.87(12) . . ?
O6 K1 Si2 117.82(10) . . ?
O5 K1 Si2 130.86(11) . . ?
C1 K1 Si2 29.82(11) . . ?
C9 K1 Si2 68.38(13) . . ?
Si1 K1 Si2 50.46(5) . . ?
Si3 K1 Si2 50.86(5) . . ?
O3 Si1 C1 107.6(2) . . ?
O3 Si1 C14 105.3(3) . . ?
C1 Si1 C14 115.4(3) . . ?
O3 Si1 C5 105.2(3) . . ?
C1 Si1 C5 117.3(3) . . ?
C14 Si1 C5 105.0(3) . . ?
O3 Si1 K1 45.81(13) . . ?
C1 Si1 K1 67.24(19) . . ?
C14 Si1 K1 103.7(2) . . ?
C5 Si1 K1 144.1(2) . . ?
O2 Si2 C1 106.9(3) . . ?
O2 Si2 C4 106.6(2) . . ?
C1 Si2 C4 118.6(3) . . ?
O2 Si2 C16 105.2(3) . . ?
C1 Si2 C16 115.5(3) . . ?
C4 Si2 C16 103.0(4) . . ?
O2 Si2 K1 45.92(16) . . ?
C1 Si2 K1 66.0(2) . . ?
C4 Si2 K1 145.5(2) . . ?
C16 Si2 K1 104.7(3) . . ?
O4 Si3 C1 109.4(3) . . ?
O4 Si3 C15 104.7(3) . . ?
C1 Si3 C15 115.4(3) . . ?
O4 Si3 C10 104.9(3) . . ?
C1 Si3 C10 117.4(3) . . ?
C15 Si3 C10 103.9(3) . . ?
O4 Si3 K1 45.02(14) . . ?
C1 Si3 K1 66.43(19) . . ?
C15 Si3 K1 111.8(2) . . ?
C10 Si3 K1 137.6(3) . . ?
C9 O1 C13 112.3(6) . . ?
C9 O1 K1 110.9(4) . . ?
C13 O1 K1 113.8(4) . . ?
C12 O2 Si2 124.2(4) . . ?
C12 O2 K1 116.7(4) . . ?
Si2 O2 K1 107.34(19) . . ?
C8 O3 Si1 125.2(3) . . ?
C8 O3 K1 119.1(3) . . ?
Si1 O3 K1 107.30(18) . . ?
C2 O4 Si3 124.6(4) . . ?
C2 O4 K1 118.1(3) . . ?
Si3 O4 K1 108.1(2) . . ?
C3 O5 C11 110.4(5) . . ?
C3 O5 K1 113.6(4) . . ?
C11 O5 K1 119.0(4) . . ?
C6 O6 C7 112.2(5) . . ?
C6 O6 K1 115.1(4) . . ?
C7 O6 K1 112.8(4) . . ?
Si1 C1 Si2 117.5(3) . . ?
Si1 C1 Si3 121.1(4) . . ?
Si2 C1 Si3 117.8(3) . . ?
Si1 C1 K1 83.2(2) . . ?
Si2 C1 K1 84.2(2) . . ?
Si3 C1 K1 83.6(2) . . ?
O4 C2 C3 110.0(5) . . ?
O4 C2 H2A 109.7 . . ?
C3 C2 H2A 109.7 . . ?
O4 C2 H2B 109.7 . . ?
C3 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
O5 C3 C2 109.0(6) . . ?
O5 C3 H3A 109.9 . . ?
C2 C3 H3A 109.9 . . ?
O5 C3 H3B 109.9 . . ?
C2 C3 H3B 109.9 . . ?
H3A C3 H3B 108.3 . . ?
Si2 C4 H4A 109.5 . . ?
Si2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si1 C5 H5A 109.5 . . ?
Si1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O6 C6 H6A 109.5 . . ?
O6 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
O6 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O6 C7 C8 108.6(5) . . ?
O6 C7 H7A 110 . . ?
C8 C7 H7A 110 . . ?
O6 C7 H7B 110 . . ?
C8 C7 H7B 110 . . ?
H7A C7 H7B 108.3 . . ?
O3 C8 C7 109.1(5) . . ?
O3 C8 H8A 109.9 . . ?
C7 C8 H8A 109.9 . . ?
O3 C8 H8B 109.9 . . ?
C7 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
O1 C9 C12 110.8(6) . . ?
O1 C9 K1 47.3(3) . . ?
C12 C9 K1 80.9(4) . . ?
O1 C9 H9A 109.5 . . ?
C12 C9 H9A 109.5 . . ?
K1 C9 H9A 156.5 . . ?
O1 C9 H9B 109.5 . . ?
C12 C9 H9B 109.5 . . ?
K1 C9 H9B 87.1 . . ?
H9A C9 H9B 108.1 . . ?
Si3 C10 H10A 109.5 . . ?
Si3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O5 C11 H11A 109.5 . . ?
O5 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
O5 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O2 C12 C9 109.5(6) . . ?
O2 C12 H12A 109.8 . . ?
C9 C12 H12A 109.8 . . ?
O2 C12 H12B 109.8 . . ?
C9 C12 H12B 109.8 . . ?
H12A C12 H12B 108.2 . . ?
O1 C13 H13A 109.5 . . ?
O1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
O1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si1 C14 H14A 109.5 . . ?
Si1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si3 C15 H15A 109.5 . . ?
Si3 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si3 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si2 C16 H16A 109.5 . . ?
Si2 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Si2 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?

_shelxl_version_number           2014-3


# END of CIF
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Cold hexane'
_chemical_properties_physical    Air-sensitive
