# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1874997'
_audit_update_record             
;
2018-10-24 deposited with the CCDC.
2018-12-03 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C16 H50 O22 Si12'
_chemical_formula_moiety         'C16 H50 O22 Si12'
_chemical_formula_weight         931.58
_chemical_melting_point          ?
_chemical_absolute_configuration unk

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
_space_group_IT_number           9
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 +X,-Y,1/2+Z
3 1/2+X,1/2+Y,+Z
4 1/2+X,1/2-Y,1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   17.2739(5)
_cell_length_b                   10.8748(3)
_cell_length_c                   23.2168(7)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.452(6)
_cell_angle_gamma                90.0000
_cell_volume                     4361.1(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    27796
_cell_measurement_theta_min      3.81
_cell_measurement_theta_max      68.21
_cell_measurement_temperature    123
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1960.00
_exptl_absorpt_coefficient_mu    4.021
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_absorpt_correction_T_min  0.448
_exptl_absorpt_correction_T_max  0.669

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      123
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            35301
_diffrn_reflns_av_R_equivalents  0.0882
_diffrn_reflns_theta_max         68.250
_diffrn_reflns_theta_min         3.808
_diffrn_reflns_theta_full        67.687
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             7872
_reflns_number_gt                5085
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.969
_reflns_Friedel_fraction_max     0.969
_reflns_Friedel_fraction_full    0.974

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0620
_refine_ls_wR_factor_ref         0.1350
_refine_ls_wR_factor_gt          0.1204
_refine_ls_number_restraints     75
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         7872
_refine_ls_number_parameters     467
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0610P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.30
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
 Flack x determined using 1804 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(16)

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
O O 0.0492 0.0322
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Si Si 0.2541 0.3302
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.50621(14) 0.2741(2) 0.52309(11) 0.0370(6) Uani 1 1 d . . . . .
Si2 Si 0.41052(14) 0.4848(2) 0.55744(11) 0.0388(7) Uani 1 1 d . . . . .
Si3 Si 0.58039(14) 0.5039(2) 0.56061(11) 0.0396(7) Uani 1 1 d . . . . .
Si4 Si 0.50520(15) 0.3662(2) 0.40042(11) 0.0400(7) Uani 1 1 d . . . . .
Si5 Si 0.57924(14) 0.5956(2) 0.43855(12) 0.0411(7) Uani 1 1 d . . . . .
Si6 Si 0.26571(16) 0.7259(3) 0.39461(13) 0.0487(8) Uani 1 1 d . . . . .
Si7 Si 0.40870(14) 0.5747(2) 0.43549(11) 0.0392(7) Uani 1 1 d . . . . .
Si8 Si 0.70728(15) 0.7812(3) 0.40282(12) 0.0477(8) Uani 1 1 d . . . . .
Si9 Si 0.26960(15) 0.5195(3) 0.64127(12) 0.0474(7) Uani 1 1 d . . . . .
Si10 Si 0.52225(17) -0.0061(3) 0.53009(14) 0.0502(8) Uani 1 1 d . . . . .
Si11 Si 0.70456(17) 0.5821(3) 0.65367(13) 0.0537(8) Uani 1 1 d . . . . .
Si12 Si 0.52161(18) 0.2210(3) 0.28250(13) 0.0568(8) Uani 1 1 d . . . . .
O1 O 0.5768(3) 0.3584(5) 0.5464(2) 0.0397(15) Uani 1 1 d . . . . .
O2 O 0.6102(3) 0.5766(5) 0.5036(3) 0.0440(17) Uani 1 1 d . . . . .
O3 O 0.4277(3) 0.3410(5) 0.5436(2) 0.0376(15) Uani 1 1 d . . . . .
O4 O 0.4932(3) 0.5467(5) 0.5747(2) 0.0382(15) Uani 1 1 d . . . . .
O5 O 0.5109(3) 0.1386(5) 0.5481(3) 0.0468(17) Uani 1 1 d . . . . .
O6 O 0.4260(3) 0.4442(5) 0.4043(2) 0.0409(16) Uani 1 1 d . . . . .
O7 O 0.3771(3) 0.5496(5) 0.4997(3) 0.0404(16) Uani 1 1 d . . . . .
O8 O 0.2041(4) 0.6410(6) 0.3586(3) 0.062(2) Uani 1 1 d . . . . .
H8 H 0.1944 0.5769 0.3774 0.074 Uiso 1 1 calc R U . . .
O9 O 0.5760(3) 0.4625(5) 0.4070(3) 0.0410(16) Uani 1 1 d . . . . .
O10 O 0.4909(3) 0.6451(5) 0.4399(3) 0.0427(15) Uani 1 1 d . . . . .
O11 O 0.5081(3) 0.2711(5) 0.4535(2) 0.0401(16) Uani 1 1 d . . . . .
O12 O 0.2045(4) 0.4342(6) 0.6091(3) 0.0603(19) Uani 1 1 d . . . . .
H12 H 0.1819 0.3904 0.6336 0.072 Uiso 1 1 calc R U . . .
O13 O 0.3471(3) 0.6519(5) 0.3992(3) 0.0465(17) Uani 1 1 d . . . . .
O14 O 0.6124(4) -0.0312(6) 0.5150(3) 0.0541(18) Uani 1 1 d . . . . .
H14 H 0.6383 -0.0365 0.5457 0.065 Uiso 1 1 calc R U . . .
O15 O 0.5093(4) 0.2944(6) 0.3417(3) 0.0603(19) Uani 1 1 d . . . . .
O16 O 0.6341(3) 0.6872(6) 0.4050(3) 0.0532(18) Uani 1 1 d . . . . .
O17 O 0.3519(4) 0.4993(6) 0.6088(3) 0.0524(18) Uani 1 1 d . . . . .
O18 O 0.6363(4) 0.5271(7) 0.6137(3) 0.060(2) Uani 1 1 d . . . . .
O20 O 0.6845(4) 0.7237(6) 0.6687(3) 0.061(2) Uani 1 1 d . . . . .
H20 H 0.6679 0.7282 0.7026 0.073 Uiso 1 1 calc R U . . .
O21 O 0.6135(4) 0.2161(7) 0.2680(3) 0.068(2) Uani 1 1 d . . . . .
H21 H 0.6387 0.2025 0.2984 0.082 Uiso 1 1 calc R U . . .
O39 O 0.6772(4) 0.9212(6) 0.4121(3) 0.066(2) Uani 1 1 d . . . . .
H39 H 0.6610 0.9294 0.4459 0.080 Uiso 1 1 calc R U . . .
C22 C 0.2331(7) 0.7567(10) 0.4663(5) 0.073(4) Uani 1 1 d . . . . .
H22A H 0.1838 0.8014 0.4646 0.088 Uiso 1 1 calc R U . . .
H22B H 0.2257 0.6789 0.4868 0.088 Uiso 1 1 calc R U . . .
H22C H 0.2718 0.8066 0.4867 0.088 Uiso 1 1 calc R U . . .
C23 C 0.2802(6) 0.8646(9) 0.3522(5) 0.069(3) Uani 1 1 d . . . . .
H23A H 0.2313 0.9100 0.3492 0.083 Uiso 1 1 calc R U . . .
H23B H 0.3193 0.9165 0.3710 0.083 Uiso 1 1 calc R U . . .
H23C H 0.2977 0.8422 0.3136 0.083 Uiso 1 1 calc R U . . .
C24 C 0.7505(7) 0.7731(11) 0.3308(5) 0.073(4) Uani 1 1 d . . . . .
H24A H 0.7693 0.6895 0.3238 0.087 Uiso 1 1 calc R U . . .
H24B H 0.7114 0.7945 0.3017 0.087 Uiso 1 1 calc R U . . .
H24C H 0.7938 0.8311 0.3286 0.087 Uiso 1 1 calc R U . . .
C25 C 0.4651(8) -0.0361(10) 0.4638(6) 0.096(5) Uani 1 1 d . . . . .
H25A H 0.4101 -0.0218 0.4714 0.116 Uiso 1 1 calc R U . . .
H25B H 0.4822 0.0192 0.4331 0.116 Uiso 1 1 calc R U . . .
H25C H 0.4726 -0.1216 0.4518 0.116 Uiso 1 1 calc R U . . .
C26 C 0.2416(7) 0.6799(10) 0.6331(6) 0.088(4) Uani 1 1 d . . . . .
H26A H 0.1921 0.6939 0.6524 0.105 Uiso 1 1 calc R U . . .
H26B H 0.2814 0.7327 0.6504 0.105 Uiso 1 1 calc R U . . .
H26C H 0.2361 0.6995 0.5921 0.105 Uiso 1 1 calc R U . . .
C27 C 0.4747(8) 0.3045(16) 0.2254(5) 0.121(6) Uani 1 1 d . . . . .
H27A H 0.4818 0.2606 0.1889 0.146 Uiso 1 1 calc R U . . .
H27B H 0.4193 0.3115 0.2335 0.146 Uiso 1 1 calc R U . . .
H27C H 0.4974 0.3868 0.2225 0.146 Uiso 1 1 calc R U . . .
C28 C 0.4953(7) -0.0991(10) 0.5918(6) 0.089(4) Uani 1 1 d . . . . .
H28A H 0.4408 -0.0843 0.6010 0.107 Uiso 1 1 calc R U . . .
H28B H 0.5027 -0.1863 0.5826 0.107 Uiso 1 1 calc R U . . .
H28C H 0.5279 -0.0769 0.6249 0.107 Uiso 1 1 calc R U . . .
C29 C 0.2830(6) 0.4720(11) 0.7161(5) 0.072(4) Uani 1 1 d . . . . .
H29A H 0.2344 0.4830 0.7369 0.086 Uiso 1 1 calc R U . . .
H29B H 0.2983 0.3852 0.7173 0.086 Uiso 1 1 calc R U . . .
H29C H 0.3236 0.5223 0.7341 0.086 Uiso 1 1 calc R U . . .
C30 C 0.7735(6) 0.7368(11) 0.4604(5) 0.079(4) Uani 1 1 d . . . . .
H30A H 0.7910 0.6522 0.4541 0.095 Uiso 1 1 calc R U . . .
H30B H 0.8182 0.7922 0.4606 0.095 Uiso 1 1 calc R U . . .
H30C H 0.7469 0.7421 0.4974 0.095 Uiso 1 1 calc R U . . .
C32 C 0.7938(7) 0.5796(14) 0.6119(7) 0.113(5) Uani 1 1 d . . . . .
H32A H 0.8364 0.6127 0.6353 0.136 Uiso 1 1 calc R U . . .
H32B H 0.8057 0.4948 0.6008 0.136 Uiso 1 1 calc R U . . .
H32C H 0.7871 0.6299 0.5772 0.136 Uiso 1 1 calc R U . . .
C33 C 0.7102(9) 0.4902(11) 0.7187(5) 0.107(5) Uani 1 1 d . . . . .
H33A H 0.7515 0.5221 0.7438 0.128 Uiso 1 1 calc R U . . .
H33B H 0.6607 0.4942 0.7390 0.128 Uiso 1 1 calc R U . . .
H33C H 0.7215 0.4046 0.7086 0.128 Uiso 1 1 calc R U . . .
C38 C 0.4851(11) 0.0664(15) 0.2948(9) 0.175(9) Uani 1 1 d . . . . .
H38A H 0.4913 0.0173 0.2597 0.210 Uiso 1 1 calc R U . . .
H38B H 0.5142 0.0281 0.3264 0.210 Uiso 1 1 calc R U . . .
H38C H 0.4302 0.0704 0.3048 0.210 Uiso 1 1 calc R U . . .
O31A O 0.4236(9) 0.2122(17) 0.7402(7) 0.109(5) Uani 0.599(10) 1 d D U P A 1
C35A C 0.4538(13) 0.246(3) 0.6880(9) 0.114(8) Uani 0.599(10) 1 d D U P A 1
H35A H 0.4325 0.3259 0.6753 0.137 Uiso 0.599(10) 1 calc R U P A 1
H35B H 0.4421 0.1832 0.6583 0.137 Uiso 0.599(10) 1 calc R U P A 1
C36A C 0.5402(13) 0.255(4) 0.6987(11) 0.125(9) Uani 0.599(10) 1 d D U P A 1
H36A H 0.5637 0.3205 0.6750 0.151 Uiso 0.599(10) 1 calc R U P A 1
H36B H 0.5664 0.1759 0.6905 0.151 Uiso 0.599(10) 1 calc R U P A 1
C37A C 0.5440(14) 0.286(4) 0.7625(10) 0.154(10) Uani 0.599(10) 1 d D U P A 1
H37A H 0.5617 0.3718 0.7682 0.185 Uiso 0.599(10) 1 calc R U P A 1
H37B H 0.5803 0.2302 0.7829 0.185 Uiso 0.599(10) 1 calc R U P A 1
C34A C 0.4619(14) 0.270(3) 0.7851(9) 0.103(8) Uani 0.599(10) 1 d D U P A 1
H34A H 0.4616 0.2182 0.8202 0.123 Uiso 0.599(10) 1 calc R U P A 1
H34B H 0.4380 0.3503 0.7939 0.123 Uiso 0.599(10) 1 calc R U P A 1
O31B O 0.4971(17) 0.333(3) 0.7012(10) 0.109(5) Uani 0.401(10) 1 d D . P A 2
C35B C 0.507(2) 0.204(3) 0.6938(14) 0.114(8) Uani 0.401(10) 1 d D . P A 2
H35C H 0.5225 0.1813 0.6543 0.137 Uiso 0.401(10) 1 calc R U P A 2
H35D H 0.4607 0.1560 0.7054 0.137 Uiso 0.401(10) 1 calc R U P A 2
C36B C 0.5738(18) 0.195(4) 0.7378(16) 0.125(9) Uani 0.401(10) 1 d D . P A 2
H36C H 0.5874 0.1092 0.7469 0.151 Uiso 0.401(10) 1 calc R U P A 2
H36D H 0.6204 0.2399 0.7246 0.151 Uiso 0.401(10) 1 calc R U P A 2
C37B C 0.536(2) 0.260(4) 0.7887(12) 0.154(10) Uani 0.401(10) 1 d D . P A 2
H37C H 0.5133 0.1997 0.8159 0.185 Uiso 0.401(10) 1 calc R U P A 2
H37D H 0.5730 0.3130 0.8096 0.185 Uiso 0.401(10) 1 calc R U P A 2
C34B C 0.473(3) 0.336(4) 0.7592(12) 0.103(8) Uani 0.401(10) 1 d D . P A 2
H34C H 0.4213 0.2976 0.7638 0.123 Uiso 0.401(10) 1 calc R U P A 2
H34D H 0.4717 0.4207 0.7742 0.123 Uiso 0.401(10) 1 calc R U P A 2


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SHELXT Version 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2014/6 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.4 (Rigaku, 2016)'
_computing_molecular_graphics    'CrystalStructure 4.2.4'

#==============================================================================
# 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
Si1 O5 1.585(6) . ?
Si1 O3 1.614(6) . ?
Si1 O1 1.615(6) . ?
Si1 O11 1.617(6) . ?
Si2 O17 1.578(6) . ?
Si2 O7 1.617(6) . ?
Si2 O3 1.624(6) . ?
Si2 O4 1.627(6) . ?
Si3 O18 1.581(7) . ?
Si3 O4 1.612(6) . ?
Si3 O1 1.618(6) . ?
Si3 O2 1.629(6) . ?
Si4 O15 1.574(7) . ?
Si4 O11 1.609(6) . ?
Si4 O6 1.612(6) . ?
Si4 O9 1.617(6) . ?
Si5 O16 1.584(6) . ?
Si5 O2 1.611(6) . ?
Si5 O10 1.618(6) . ?
Si5 O9 1.623(6) . ?
Si6 O13 1.623(6) . ?
Si6 O8 1.635(7) . ?
Si6 C22 1.793(11) . ?
Si6 C23 1.819(10) . ?
Si7 O13 1.592(6) . ?
Si7 O7 1.615(6) . ?
Si7 O10 1.617(6) . ?
Si7 O6 1.622(6) . ?
Si8 O39 1.624(7) . ?
Si8 O16 1.627(6) . ?
Si8 C30 1.817(11) . ?
Si8 C24 1.838(10) . ?
Si9 O17 1.630(6) . ?
Si9 O12 1.634(7) . ?
Si9 C26 1.820(11) . ?
Si9 C29 1.825(11) . ?
Si10 O14 1.622(7) . ?
Si10 O5 1.641(6) . ?
Si10 C28 1.816(11) . ?
Si10 C25 1.851(12) . ?
Si11 O18 1.609(7) . ?
Si11 O20 1.617(7) . ?
Si11 C33 1.814(13) . ?
Si11 C32 1.827(13) . ?
Si12 O15 1.605(7) . ?
Si12 O21 1.626(7) . ?
Si12 C27 1.795(14) . ?
Si12 C38 1.819(15) . ?
O8 H8 0.8400 . ?
O12 H12 0.8400 . ?
O14 H14 0.8400 . ?
O20 H20 0.8400 . ?
O21 H21 0.8400 . ?
O39 H39 0.8400 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
O31A C35A 1.373(16) . ?
O31A C34A 1.379(16) . ?
C35A C36A 1.514(17) . ?
C35A H35A 0.9900 . ?
C35A H35B 0.9900 . ?
C36A C37A 1.52(2) . ?
C36A H36A 0.9900 . ?
C36A H36B 0.9900 . ?
C37A C34A 1.526(17) . ?
C37A H37A 0.9900 . ?
C37A H37B 0.9900 . ?
C34A H34A 0.9900 . ?
C34A H34B 0.9900 . ?
O31B C34B 1.414(18) . ?
O31B C35B 1.420(19) . ?
C35B C36B 1.541(19) . ?
C35B H35C 0.9900 . ?
C35B H35D 0.9900 . ?
C36B C37B 1.53(2) . ?
C36B H36C 0.9900 . ?
C36B H36D 0.9900 . ?
C37B C34B 1.520(18) . ?
C37B H37C 0.9900 . ?
C37B H37D 0.9900 . ?
C34B H34C 0.9900 . ?
C34B H34D 0.9900 . ?

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
O5 Si1 O3 110.6(3) . . ?
O5 Si1 O1 111.6(3) . . ?
O3 Si1 O1 106.2(3) . . ?
O5 Si1 O11 110.2(3) . . ?
O3 Si1 O11 109.2(3) . . ?
O1 Si1 O11 108.9(3) . . ?
O17 Si2 O7 110.9(3) . . ?
O17 Si2 O3 111.4(3) . . ?
O7 Si2 O3 108.7(3) . . ?
O17 Si2 O4 109.9(3) . . ?
O7 Si2 O4 109.4(3) . . ?
O3 Si2 O4 106.5(3) . . ?
O18 Si3 O4 111.2(3) . . ?
O18 Si3 O1 109.8(4) . . ?
O4 Si3 O1 106.8(3) . . ?
O18 Si3 O2 111.2(4) . . ?
O4 Si3 O2 109.0(3) . . ?
O1 Si3 O2 108.7(3) . . ?
O15 Si4 O11 110.1(3) . . ?
O15 Si4 O6 110.7(4) . . ?
O11 Si4 O6 108.5(3) . . ?
O15 Si4 O9 111.4(4) . . ?
O11 Si4 O9 108.9(3) . . ?
O6 Si4 O9 107.2(3) . . ?
O16 Si5 O2 110.2(3) . . ?
O16 Si5 O10 111.6(3) . . ?
O2 Si5 O10 109.3(3) . . ?
O16 Si5 O9 111.0(3) . . ?
O2 Si5 O9 108.6(3) . . ?
O10 Si5 O9 106.1(3) . . ?
O13 Si6 O8 108.3(4) . . ?
O13 Si6 C22 108.1(4) . . ?
O8 Si6 C22 111.9(5) . . ?
O13 Si6 C23 108.9(4) . . ?
O8 Si6 C23 106.4(5) . . ?
C22 Si6 C23 113.2(5) . . ?
O13 Si7 O7 110.4(3) . . ?
O13 Si7 O10 111.5(3) . . ?
O7 Si7 O10 108.9(3) . . ?
O13 Si7 O6 110.5(3) . . ?
O7 Si7 O6 109.2(3) . . ?
O10 Si7 O6 106.1(3) . . ?
O39 Si8 O16 109.6(4) . . ?
O39 Si8 C30 110.6(5) . . ?
O16 Si8 C30 107.1(4) . . ?
O39 Si8 C24 107.3(5) . . ?
O16 Si8 C24 108.7(4) . . ?
C30 Si8 C24 113.5(6) . . ?
O17 Si9 O12 108.2(4) . . ?
O17 Si9 C26 108.3(5) . . ?
O12 Si9 C26 108.4(5) . . ?
O17 Si9 C29 107.3(4) . . ?
O12 Si9 C29 110.8(4) . . ?
C26 Si9 C29 113.7(6) . . ?
O14 Si10 O5 109.4(4) . . ?
O14 Si10 C28 109.2(4) . . ?
O5 Si10 C28 107.5(5) . . ?
O14 Si10 C25 107.4(5) . . ?
O5 Si10 C25 108.5(4) . . ?
C28 Si10 C25 114.8(7) . . ?
O18 Si11 O20 108.7(4) . . ?
O18 Si11 C33 108.0(5) . . ?
O20 Si11 C33 110.8(5) . . ?
O18 Si11 C32 107.8(6) . . ?
O20 Si11 C32 108.2(6) . . ?
C33 Si11 C32 113.2(7) . . ?
O15 Si12 O21 109.3(4) . . ?
O15 Si12 C27 108.6(5) . . ?
O21 Si12 C27 107.4(5) . . ?
O15 Si12 C38 106.1(7) . . ?
O21 Si12 C38 110.0(7) . . ?
C27 Si12 C38 115.4(9) . . ?
Si1 O1 Si3 130.7(4) . . ?
Si5 O2 Si3 136.0(4) . . ?
Si1 O3 Si2 130.4(4) . . ?
Si3 O4 Si2 130.6(4) . . ?
Si1 O5 Si10 143.5(4) . . ?
Si4 O6 Si7 130.2(4) . . ?
Si7 O7 Si2 135.9(4) . . ?
Si6 O8 H8 109.5 . . ?
Si4 O9 Si5 130.0(4) . . ?
Si7 O10 Si5 132.0(4) . . ?
Si4 O11 Si1 138.7(4) . . ?
Si9 O12 H12 109.5 . . ?
Si7 O13 Si6 150.6(4) . . ?
Si10 O14 H14 109.5 . . ?
Si4 O15 Si12 174.9(5) . . ?
Si5 O16 Si8 151.5(5) . . ?
Si2 O17 Si9 158.5(5) . . ?
Si3 O18 Si11 161.6(5) . . ?
Si11 O20 H20 109.5 . . ?
Si12 O21 H21 109.5 . . ?
Si8 O39 H39 109.5 . . ?
Si6 C22 H22A 109.5 . . ?
Si6 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si6 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si6 C23 H23A 109.5 . . ?
Si6 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si6 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si8 C24 H24A 109.5 . . ?
Si8 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si8 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si10 C25 H25A 109.5 . . ?
Si10 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
Si10 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Si9 C26 H26A 109.5 . . ?
Si9 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Si9 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Si12 C27 H27A 109.5 . . ?
Si12 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
Si12 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
Si10 C28 H28A 109.5 . . ?
Si10 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
Si10 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si9 C29 H29A 109.5 . . ?
Si9 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
Si9 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si8 C30 H30A 109.5 . . ?
Si8 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
Si8 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Si11 C32 H32A 109.5 . . ?
Si11 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
Si11 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
Si11 C33 H33A 109.5 . . ?
Si11 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
Si11 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
Si12 C38 H38A 109.5 . . ?
Si12 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
Si12 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C35A O31A C34A 111.2(19) . . ?
O31A C35A C36A 104.7(17) . . ?
O31A C35A H35A 110.8 . . ?
C36A C35A H35A 110.8 . . ?
O31A C35A H35B 110.8 . . ?
C36A C35A H35B 110.8 . . ?
H35A C35A H35B 108.9 . . ?
C35A C36A C37A 102.1(14) . . ?
C35A C36A H36A 111.4 . . ?
C37A C36A H36A 111.4 . . ?
C35A C36A H36B 111.4 . . ?
C37A C36A H36B 111.4 . . ?
H36A C36A H36B 109.2 . . ?
C36A C37A C34A 106.0(14) . . ?
C36A C37A H37A 110.5 . . ?
C34A C37A H37A 110.5 . . ?
C36A C37A H37B 110.5 . . ?
C34A C37A H37B 110.5 . . ?
H37A C37A H37B 108.7 . . ?
O31A C34A C37A 103.6(15) . . ?
O31A C34A H34A 111.0 . . ?
C37A C34A H34A 111.0 . . ?
O31A C34A H34B 111.0 . . ?
C37A C34A H34B 111.0 . . ?
H34A C34A H34B 109.0 . . ?
C34B O31B C35B 100(2) . . ?
O31B C35B C36B 94(2) . . ?
O31B C35B H35C 113.0 . . ?
C36B C35B H35C 113.0 . . ?
O31B C35B H35D 113.0 . . ?
C36B C35B H35D 113.0 . . ?
H35C C35B H35D 110.4 . . ?
C37B C36B C35B 99.2(19) . . ?
C37B C36B H36C 111.9 . . ?
C35B C36B H36C 111.9 . . ?
C37B C36B H36D 111.9 . . ?
C35B C36B H36D 111.9 . . ?
H36C C36B H36D 109.6 . . ?
C34B C37B C36B 102.1(16) . . ?
C34B C37B H37C 111.3 . . ?
C36B C37B H37C 111.3 . . ?
C34B C37B H37D 111.3 . . ?
C36B C37B H37D 111.3 . . ?
H37C C37B H37D 109.2 . . ?
O31B C34B C37B 102(2) . . ?
O31B C34B H34C 111.4 . . ?
C37B C34B H34C 111.4 . . ?
O31B C34B H34D 111.4 . . ?
C37B C34B H34D 111.4 . . ?
H34C C34B H34D 109.3 . . ?

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
O5 Si1 O1 Si3 -147.1(5) . . . . ?
O3 Si1 O1 Si3 -26.5(6) . . . . ?
O11 Si1 O1 Si3 90.9(5) . . . . ?
O18 Si3 O1 Si1 145.2(5) . . . . ?
O4 Si3 O1 Si1 24.6(6) . . . . ?
O2 Si3 O1 Si1 -92.9(5) . . . . ?
O16 Si5 O2 Si3 175.9(5) . . . . ?
O10 Si5 O2 Si3 52.9(7) . . . . ?
O9 Si5 O2 Si3 -62.4(6) . . . . ?
O18 Si3 O2 Si5 -177.1(5) . . . . ?
O4 Si3 O2 Si5 -54.1(7) . . . . ?
O1 Si3 O2 Si5 62.0(6) . . . . ?
O5 Si1 O3 Si2 147.8(4) . . . . ?
O1 Si1 O3 Si2 26.5(6) . . . . ?
O11 Si1 O3 Si2 -90.7(5) . . . . ?
O17 Si2 O3 Si1 -144.5(5) . . . . ?
O7 Si2 O3 Si1 93.1(5) . . . . ?
O4 Si2 O3 Si1 -24.6(6) . . . . ?
O18 Si3 O4 Si2 -141.4(5) . . . . ?
O1 Si3 O4 Si2 -21.7(6) . . . . ?
O2 Si3 O4 Si2 95.6(5) . . . . ?
O17 Si2 O4 Si3 142.5(5) . . . . ?
O7 Si2 O4 Si3 -95.6(5) . . . . ?
O3 Si2 O4 Si3 21.7(6) . . . . ?
O3 Si1 O5 Si10 126.0(7) . . . . ?
O1 Si1 O5 Si10 -116.0(7) . . . . ?
O11 Si1 O5 Si10 5.2(8) . . . . ?
O14 Si10 O5 Si1 75.2(8) . . . . ?
C28 Si10 O5 Si1 -166.3(7) . . . . ?
C25 Si10 O5 Si1 -41.7(9) . . . . ?
O15 Si4 O6 Si7 -147.5(5) . . . . ?
O11 Si4 O6 Si7 91.7(5) . . . . ?
O9 Si4 O6 Si7 -25.8(6) . . . . ?
O13 Si7 O6 Si4 144.9(5) . . . . ?
O7 Si7 O6 Si4 -93.5(5) . . . . ?
O10 Si7 O6 Si4 23.8(6) . . . . ?
O13 Si7 O7 Si2 -176.8(5) . . . . ?
O10 Si7 O7 Si2 -54.0(7) . . . . ?
O6 Si7 O7 Si2 61.5(7) . . . . ?
O17 Si2 O7 Si7 175.7(5) . . . . ?
O3 Si2 O7 Si7 -61.6(6) . . . . ?
O4 Si2 O7 Si7 54.3(7) . . . . ?
O15 Si4 O9 Si5 146.9(5) . . . . ?
O11 Si4 O9 Si5 -91.5(5) . . . . ?
O6 Si4 O9 Si5 25.7(6) . . . . ?
O16 Si5 O9 Si4 -145.0(5) . . . . ?
O2 Si5 O9 Si4 93.7(5) . . . . ?
O10 Si5 O9 Si4 -23.7(6) . . . . ?
O13 Si7 O10 Si5 -142.1(5) . . . . ?
O7 Si7 O10 Si5 95.7(6) . . . . ?
O6 Si7 O10 Si5 -21.7(6) . . . . ?
O16 Si5 O10 Si7 142.7(5) . . . . ?
O2 Si5 O10 Si7 -95.2(5) . . . . ?
O9 Si5 O10 Si7 21.7(6) . . . . ?
O15 Si4 O11 Si1 -179.5(5) . . . . ?
O6 Si4 O11 Si1 -58.3(7) . . . . ?
O9 Si4 O11 Si1 58.1(6) . . . . ?
O5 Si1 O11 Si4 179.5(5) . . . . ?
O3 Si1 O11 Si4 57.8(6) . . . . ?
O1 Si1 O11 Si4 -57.7(6) . . . . ?
O7 Si7 O13 Si6 3.9(10) . . . . ?
O10 Si7 O13 Si6 -117.4(9) . . . . ?
O6 Si7 O13 Si6 124.8(8) . . . . ?
O8 Si6 O13 Si7 -106.2(9) . . . . ?
C22 Si6 O13 Si7 15.2(10) . . . . ?
C23 Si6 O13 Si7 138.5(9) . . . . ?
O2 Si5 O16 Si8 -4.6(11) . . . . ?
O10 Si5 O16 Si8 117.0(9) . . . . ?
O9 Si5 O16 Si8 -124.9(9) . . . . ?
O39 Si8 O16 Si5 -94.7(10) . . . . ?
C30 Si8 O16 Si5 25.3(11) . . . . ?
C24 Si8 O16 Si5 148.3(10) . . . . ?
O7 Si2 O17 Si9 23.8(14) . . . . ?
O3 Si2 O17 Si9 -97.4(13) . . . . ?
O4 Si2 O17 Si9 144.8(12) . . . . ?
O12 Si9 O17 Si2 44.5(14) . . . . ?
C26 Si9 O17 Si2 -72.8(14) . . . . ?
C29 Si9 O17 Si2 164.1(12) . . . . ?
O4 Si3 O18 Si11 -112.8(16) . . . . ?
O1 Si3 O18 Si11 129.3(16) . . . . ?
O2 Si3 O18 Si11 8.9(18) . . . . ?
O20 Si11 O18 Si3 67.3(18) . . . . ?
C33 Si11 O18 Si3 -172.4(16) . . . . ?
C32 Si11 O18 Si3 -49.8(18) . . . . ?
C34A O31A C35A C36A 38(4) . . . . ?
O31A C35A C36A C37A -27(4) . . . . ?
C35A C36A C37A C34A 10(4) . . . . ?
C35A O31A C34A C37A -31(3) . . . . ?
C36A C37A C34A O31A 11(3) . . . . ?
C34B O31B C35B C36B -65(3) . . . . ?
O31B C35B C36B C37B 52(4) . . . . ?
C35B C36B C37B C34B -22(4) . . . . ?
C35B O31B C34B C37B 52(4) . . . . ?
C36B C37B C34B O31B -16(4) . . . . ?

#==============================================================================
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O8 H8 O39 . . 3_445 2.735(9) 0.840 1.900 172.9 no
O12 H12 O20 . . 3_445 2.698(9) 0.840 1.988 141.7 no
O14 H14 O12 . . 3_545 2.718(9) 0.840 1.884 171.8 no
O20 H20 O21 . . 2_565 2.700(10) 0.840 1.892 160.9 no
O21 H21 O8 . . 3_545 2.737(10) 0.840 1.911 167.6 no
O39 H39 O14 . . 1_565 2.697(9) 0.840 1.867 169.4 no

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.

_shelxl_version_number           2014/6


####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 1874998'
_audit_update_record             
;
2018-10-24 deposited with the CCDC.
2018-12-03 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C15 H48 O18 Si12'
_chemical_formula_moiety         'C15 H48 O18 Si12'
_chemical_formula_weight         853.56
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
_space_group_IT_number           15
loop_
_space_group_symop_operation_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                   19.8884(4)
_cell_length_b                   14.1218(3)
_cell_length_c                   16.2519(3)
_cell_angle_alpha                90.0000
_cell_angle_beta                 101.415(7)
_cell_angle_gamma                90.0000
_cell_volume                     4474.2(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    21099
_cell_measurement_theta_min      3.87
_cell_measurement_theta_max      68.38
_cell_measurement_temperature    123
#------------------------------------------------------------------------------
_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1800.00
_exptl_absorpt_coefficient_mu    3.802
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_absorpt_correction_T_min  0.293
_exptl_absorpt_correction_T_max  0.467

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      123
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            25058
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_theta_max         68.243
_diffrn_reflns_theta_min         3.865
_diffrn_reflns_theta_full        67.687
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             4061
_reflns_number_gt                3019
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_gt           0.0831
_refine_ls_wR_factor_ref         0.2426
_refine_ls_wR_factor_gt          0.2268
_refine_ls_number_restraints     384
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         4061
_refine_ls_number_parameters     232
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0949P)²+27.5000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.74
_refine_diff_density_min         -0.50
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
O O 0.0492 0.0322
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Si Si 0.2541 0.3302
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.43857(8) 0.40831(12) 0.67331(9) 0.0476(4) Uani 1 1 d . U . . .
Si2 Si 0.48842(9) 0.22549(12) 0.61414(10) 0.0542(5) Uani 1 1 d . U . . .
Si3 Si 0.34409(8) 0.49650(14) 0.51867(10) 0.0575(5) Uani 1 1 d . U . . .
Si4 Si 0.61128(9) 0.22706(14) 0.76552(11) 0.0601(5) Uani 1 1 d . U . . .
Si5 Si 0.55122(12) 0.19666(16) 0.45883(13) 0.0768(6) Uani 1 1 d . U . . .
O7 O 0.5568(2) 0.1968(3) 0.6810(3) 0.0599(11) Uani 1 1 d . U . . .
O8 O 0.3900(2) 0.4798(3) 0.6122(2) 0.0633(11) Uani 1 1 d . U . . .
O9 O 0.4980(2) 0.1960(3) 0.5216(3) 0.0678(12) Uani 1 1 d . U . . .
O10 O 0.3080(2) 0.6008(4) 0.5191(3) 0.0797(14) Uani 1 1 d . U . . .
H10 H 0.2849 0.6026 0.5570 0.119 Uiso 1 1 calc R U . . .
O11 O 0.6247(3) 0.2429(4) 0.5076(3) 0.0814(14) Uani 1 1 d . U . . .
H11 H 0.6176 0.2969 0.5260 0.122 Uiso 1 1 calc R U . . .
O12 O 0.6874(2) 0.1994(4) 0.7547(3) 0.0833(15) Uani 1 1 d . U . . .
O13 O 0.7163(3) 0.1433(5) 0.6118(3) 0.107(2) Uani 1 1 d . U . . .
H13A H 0.6799 0.1749 0.5993 0.161 Uiso 0.657(10) 1 calc R U P A 1
H13B H 0.6753 0.1599 0.5948 0.161 Uiso 0.343(10) 1 calc R U P A 2
O14 O 0.39182(18) 0.3415(3) 0.7209(2) 0.0526(10) Uani 1 1 d . U . . .
O15 O 0.47758(18) 0.3398(3) 0.6176(2) 0.0474(9) Uani 1 1 d . U . . .
C16 C 0.4135(4) 0.1696(5) 0.6431(4) 0.0646(17) Uani 1 1 d . U . . .
H16A H 0.4237 0.1020 0.6562 0.078 Uiso 1 1 calc R U . . .
H16B H 0.3744 0.1726 0.5948 0.078 Uiso 1 1 calc R U . . .
C17 C 0.4004(4) 0.4988(6) 0.4421(4) 0.075(2) Uani 1 1 d . U . . .
H17A H 0.3729 0.5089 0.3857 0.113 Uiso 1 1 calc R U . . .
H17B H 0.4337 0.5504 0.4559 0.113 Uiso 1 1 calc R U . . .
H17C H 0.4249 0.4384 0.4437 0.113 Uiso 1 1 calc R U . . .
C18 C 0.2778(4) 0.4069(7) 0.4991(5) 0.099(3) Uani 1 1 d . U . . .
H18A H 0.2496 0.4161 0.4430 0.149 Uiso 1 1 calc R U . . .
H18B H 0.2989 0.3440 0.5026 0.149 Uiso 1 1 calc R U . . .
H18C H 0.2488 0.4122 0.5412 0.149 Uiso 1 1 calc R U . . .
C19 C 0.5170(5) 0.2771(7) 0.3717(5) 0.105(3) Uani 1 1 d . U . . .
H19A H 0.5484 0.2790 0.3323 0.157 Uiso 1 1 calc R U . . .
H19B H 0.4720 0.2544 0.3426 0.157 Uiso 1 1 calc R U . . .
H19C H 0.5123 0.3408 0.3938 0.157 Uiso 1 1 calc R U . . .
C21 C 0.5658(7) 0.0769(8) 0.4301(8) 0.148(4) Uani 1 1 d . U . . .
H21A H 0.5981 0.0763 0.3918 0.223 Uiso 1 1 calc R U . . .
H21B H 0.5848 0.0404 0.4806 0.223 Uiso 1 1 calc R U . . .
H21C H 0.5222 0.0485 0.4021 0.223 Uiso 1 1 calc R U . . .
C23 C 0.5000 0.4755(6) 0.7500 0.0508(18) Uani 1 2 d S TU P . .
H23A H 0.4737 0.5171 0.7812 0.061 Uiso 0.5 1 calc R U P . .
H23B H 0.5263 0.5171 0.7188 0.061 Uiso 0.5 1 calc R U P . .
Si6A Si 0.7370(2) 0.1306(4) 0.7144(2) 0.0821(17) Uani 0.657(10) 1 d . U P A 1
C20A C 0.8262(7) 0.1760(13) 0.7525(12) 0.100(4) Uani 0.657(10) 1 d . U P A 1
H20A H 0.8587 0.1365 0.7297 0.150 Uiso 0.657(10) 1 calc R U P A 1
H20B H 0.8293 0.2415 0.7337 0.150 Uiso 0.657(10) 1 calc R U P A 1
H20C H 0.8373 0.1737 0.8139 0.150 Uiso 0.657(10) 1 calc R U P A 1
C22A C 0.7244(8) 0.0066(11) 0.7424(8) 0.106(4) Uani 0.657(10) 1 d . U P A 1
H22A H 0.7549 -0.0342 0.7175 0.159 Uiso 0.657(10) 1 calc R U P A 1
H22B H 0.7351 -0.0003 0.8036 0.159 Uiso 0.657(10) 1 calc R U P A 1
H22C H 0.6766 -0.0117 0.7210 0.159 Uiso 0.657(10) 1 calc R U P A 1
Si6B Si 0.7501(4) 0.2028(13) 0.7047(6) 0.113(3) Uani 0.343(10) 1 d . U P A 2
C20B C 0.8182(17) 0.119(3) 0.752(2) 0.115(9) Uani 0.343(10) 1 d . U P A 2
H20D H 0.8558 0.1216 0.7208 0.173 Uiso 0.343(10) 1 calc R U P A 2
H20E H 0.8355 0.1357 0.8105 0.173 Uiso 0.343(10) 1 calc R U P A 2
H20F H 0.7994 0.0544 0.7485 0.173 Uiso 0.343(10) 1 calc R U P A 2
C22B C 0.7749(17) 0.324(3) 0.693(2) 0.148(9) Uani 0.343(10) 1 d . U P A 2
H22D H 0.8129 0.3261 0.6632 0.222 Uiso 0.343(10) 1 calc R U P A 2
H22E H 0.7358 0.3595 0.6619 0.222 Uiso 0.343(10) 1 calc R U P A 2
H22F H 0.7896 0.3525 0.7491 0.222 Uiso 0.343(10) 1 calc R U P A 2


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SHELXT Version 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2014/6 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.4 (Rigaku, 2016)'
_computing_molecular_graphics    'CrystalStructure 4.2.4'

#==============================================================================
# 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
Si1 O8 1.599(4) . ?
Si1 O15 1.624(4) . ?
Si1 O14 1.624(4) . ?
Si1 C23 1.829(5) . ?
Si2 O9 1.608(4) . ?
Si2 O7 1.615(5) . ?
Si2 O15 1.631(4) . ?
Si2 C16 1.829(6) . ?
Si3 O8 1.628(4) . ?
Si3 O10 1.639(5) . ?
Si3 C18 1.810(8) . ?
Si3 C17 1.833(6) . ?
Si4 O12 1.606(4) . ?
Si4 O7 1.629(5) . ?
Si4 O14 1.634(5) 2_656 ?
Si4 C16 1.843(6) 2_656 ?
Si5 O9 1.609(4) . ?
Si5 O11 1.654(6) . ?
Si5 C21 1.794(10) . ?
Si5 C19 1.837(9) . ?
O10 H10 0.8400 . ?
O11 H11 0.8400 . ?
O12 Si6A 1.612(5) . ?
O12 Si6B 1.619(9) . ?
O13 Si6A 1.646(6) . ?
O13 Si6B 1.743(14) . ?
O13 H13A 0.8400 . ?
O13 H13B 0.8400 . ?
O14 Si4 1.634(5) 2_656 ?
C16 Si4 1.843(6) 2_656 ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C23 Si1 1.829(5) 2_656 ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
Si6A C22A 1.839(16) . ?
Si6A C20A 1.872(18) . ?
C20A H20A 0.9800 . ?
C20A H20B 0.9800 . ?
C20A H20C 0.9800 . ?
C22A H22A 0.9800 . ?
C22A H22B 0.9800 . ?
C22A H22C 0.9800 . ?
Si6B C22B 1.80(4) . ?
Si6B C20B 1.85(4) . ?
C20B H20D 0.9800 . ?
C20B H20E 0.9800 . ?
C20B H20F 0.9800 . ?
C22B H22D 0.9800 . ?
C22B H22E 0.9800 . ?
C22B H22F 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
O8 Si1 O15 109.0(2) . . ?
O8 Si1 O14 109.3(2) . . ?
O15 Si1 O14 107.5(2) . . ?
O8 Si1 C23 109.6(3) . . ?
O15 Si1 C23 111.16(19) . . ?
O14 Si1 C23 110.20(19) . . ?
O9 Si2 O7 108.9(2) . . ?
O9 Si2 O15 109.3(2) . . ?
O7 Si2 O15 108.9(2) . . ?
O9 Si2 C16 112.5(3) . . ?
O7 Si2 C16 109.9(3) . . ?
O15 Si2 C16 107.4(3) . . ?
O8 Si3 O10 107.0(3) . . ?
O8 Si3 C18 108.5(3) . . ?
O10 Si3 C18 108.9(4) . . ?
O8 Si3 C17 109.3(3) . . ?
O10 Si3 C17 108.3(3) . . ?
C18 Si3 C17 114.6(4) . . ?
O12 Si4 O7 109.1(3) . . ?
O12 Si4 O14 108.5(3) . 2_656 ?
O7 Si4 O14 109.7(2) . 2_656 ?
O12 Si4 C16 112.9(3) . 2_656 ?
O7 Si4 C16 109.0(3) . 2_656 ?
O14 Si4 C16 107.7(3) 2_656 2_656 ?
O9 Si5 O11 109.2(3) . . ?
O9 Si5 C21 108.6(4) . . ?
O11 Si5 C21 109.0(5) . . ?
O9 Si5 C19 107.6(4) . . ?
O11 Si5 C19 106.4(4) . . ?
C21 Si5 C19 115.9(6) . . ?
Si2 O7 Si4 146.3(3) . . ?
Si1 O8 Si3 146.1(3) . . ?
Si2 O9 Si5 143.7(3) . . ?
Si3 O10 H10 109.5 . . ?
Si5 O11 H11 109.5 . . ?
Si4 O12 Si6A 149.0(5) . . ?
Si4 O12 Si6B 152.2(5) . . ?
Si6A O13 H13A 109.5 . . ?
Si6B O13 H13B 109.5 . . ?
Si1 O14 Si4 132.8(2) . 2_656 ?
Si1 O15 Si2 133.6(2) . . ?
Si2 C16 Si4 112.3(3) . 2_656 ?
Si2 C16 H16A 109.2 . . ?
Si4 C16 H16A 109.2 2_656 . ?
Si2 C16 H16B 109.2 . . ?
Si4 C16 H16B 109.2 2_656 . ?
H16A C16 H16B 107.9 . . ?
Si3 C17 H17A 109.5 . . ?
Si3 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si3 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si3 C18 H18A 109.5 . . ?
Si3 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Si3 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si5 C19 H19A 109.5 . . ?
Si5 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Si5 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si5 C21 H21A 109.5 . . ?
Si5 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si5 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si1 C23 Si1 117.5(4) . 2_656 ?
Si1 C23 H23A 107.9 . . ?
Si1 C23 H23A 107.9 2_656 . ?
Si1 C23 H23B 107.9 . . ?
Si1 C23 H23B 107.9 2_656 . ?
H23A C23 H23B 107.2 . . ?
O12 Si6A O13 107.2(3) . . ?
O12 Si6A C22A 110.4(6) . . ?
O13 Si6A C22A 109.6(6) . . ?
O12 Si6A C20A 106.0(7) . . ?
O13 Si6A C20A 109.2(7) . . ?
C22A Si6A C20A 114.2(7) . . ?
Si6A C20A H20A 109.5 . . ?
Si6A C20A H20B 109.5 . . ?
H20A C20A H20B 109.5 . . ?
Si6A C20A H20C 109.5 . . ?
H20A C20A H20C 109.5 . . ?
H20B C20A H20C 109.5 . . ?
Si6A C22A H22A 109.5 . . ?
Si6A C22A H22B 109.5 . . ?
H22A C22A H22B 109.5 . . ?
Si6A C22A H22C 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
O12 Si6B O13 102.5(7) . . ?
O12 Si6B C22B 109.5(13) . . ?
O13 Si6B C22B 115.9(14) . . ?
O12 Si6B C20B 110.4(14) . . ?
O13 Si6B C20B 100.0(15) . . ?
C22B Si6B C20B 117.3(19) . . ?
Si6B C20B H20D 109.5 . . ?
Si6B C20B H20E 109.5 . . ?
H20D C20B H20E 109.5 . . ?
Si6B C20B H20F 109.5 . . ?
H20D C20B H20F 109.5 . . ?
H20E C20B H20F 109.5 . . ?
Si6B C22B H22D 109.5 . . ?
Si6B C22B H22E 109.5 . . ?
H22D C22B H22E 109.5 . . ?
Si6B C22B H22F 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 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
O9 Si2 O7 Si4 140.6(5) . . . . ?
O15 Si2 O7 Si4 21.5(6) . . . . ?
C16 Si2 O7 Si4 -95.8(5) . . . . ?
O12 Si4 O7 Si2 -140.0(5) . . . . ?
O14 Si4 O7 Si2 -21.3(6) 2_656 . . . ?
C16 Si4 O7 Si2 96.3(5) 2_656 . . . ?
O15 Si1 O8 Si3 28.8(6) . . . . ?
O14 Si1 O8 Si3 -88.5(6) . . . . ?
C23 Si1 O8 Si3 150.6(5) . . . . ?
O10 Si3 O8 Si1 177.2(5) . . . . ?
C18 Si3 O8 Si1 59.8(7) . . . . ?
C17 Si3 O8 Si1 -65.7(6) . . . . ?
O7 Si2 O9 Si5 -43.6(6) . . . . ?
O15 Si2 O9 Si5 75.3(6) . . . . ?
C16 Si2 O9 Si5 -165.6(5) . . . . ?
O11 Si5 O9 Si2 1.9(7) . . . . ?
C21 Si5 O9 Si2 120.6(7) . . . . ?
C19 Si5 O9 Si2 -113.2(6) . . . . ?
O7 Si4 O12 Si6A -30.0(8) . . . . ?
O14 Si4 O12 Si6A -149.4(7) 2_656 . . . ?
C16 Si4 O12 Si6A 91.4(8) 2_656 . . . ?
O7 Si4 O12 Si6B 54.7(15) . . . . ?
O14 Si4 O12 Si6B -64.7(15) 2_656 . . . ?
C16 Si4 O12 Si6B 176.1(15) 2_656 . . . ?
O8 Si1 O14 Si4 130.4(3) . . . 2_656 ?
O15 Si1 O14 Si4 12.2(4) . . . 2_656 ?
C23 Si1 O14 Si4 -109.0(4) . . . 2_656 ?
O8 Si1 O15 Si2 -130.7(3) . . . . ?
O14 Si1 O15 Si2 -12.3(4) . . . . ?
C23 Si1 O15 Si2 108.4(4) . . . . ?
O9 Si2 O15 Si1 152.6(3) . . . . ?
O7 Si2 O15 Si1 -88.5(4) . . . . ?
C16 Si2 O15 Si1 30.4(4) . . . . ?
O9 Si2 C16 Si4 -164.3(3) . . . 2_656 ?
O7 Si2 C16 Si4 74.2(4) . . . 2_656 ?
O15 Si2 C16 Si4 -44.0(5) . . . 2_656 ?
O8 Si1 C23 Si1 -179.74(19) . . . 2_656 ?
O15 Si1 C23 Si1 -59.16(17) . . . 2_656 ?
O14 Si1 C23 Si1 59.94(17) . . . 2_656 ?
Si4 O12 Si6A O13 63.4(9) . . . . ?
Si4 O12 Si6A C22A -55.9(9) . . . . ?
Si4 O12 Si6A C20A 179.9(8) . . . . ?
Si4 O12 Si6B O13 -65.5(19) . . . . ?
Si4 O12 Si6B C22B 58(2) . . . . ?
Si4 O12 Si6B C20B -171.2(16) . . . . ?

#==============================================================================
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O10 H10 O13 . . 3_455 2.654(8) 0.840 1.861 157.0 no
O11 H11 O10 . . 5_666 2.660(8) 0.840 2.289 107.1 no
O13 H13A O11 . . . 2.635(7) 0.840 1.924 141.7 no
O13 H13B O11 . . . 2.635(7) 0.840 1.958 137.0 no

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.

_shelxl_version_number           2014/6


