# Electronic Supplementary Material (ESI) for ChemComm.
# 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_ydkr
_database_code_depnum_ccdc_archive 'CCDC 1883887'
_audit_update_record             
;
2018-12-08 deposited with the CCDC.
2018-12-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H38 O Si2'
_chemical_formula_weight         482.79

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'
Si Si 0.0817 0.0704 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.441(6)
_cell_length_b                   11.776(6)
_cell_length_c                   12.121(7)
_cell_angle_alpha                76.44(2)
_cell_angle_beta                 80.25(2)
_cell_angle_gamma                76.74(2)
_cell_volume                     1399.6(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    93

_cell_measurement_reflns_used    3655

_cell_measurement_theta_min      2.4

_cell_measurement_theta_max      31.1


_exptl_crystal_description       Block

_exptl_crystal_colour            Orange

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_F_000             520
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.10

_exptl_crystal_size_mid          0.04

_exptl_crystal_size_min          0.04

_exptl_absorpt_coefficient_mu    0.148
_shelx_estimated_absorpt_T_min   0.985
_shelx_estimated_absorpt_T_max   0.994
_exptl_absorpt_correction_type   Multi-scan

_exptl_absorpt_correction_T_min  0.822

_exptl_absorpt_correction_T_max  1.000

_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communicatio'

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93

_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD'

_diffrn_measurement_method       'profile data from ω-scans'

_diffrn_detector_area_resol_mean 28.5714

_diffrn_reflns_number            10011
_diffrn_reflns_av_unetI/netI     0.1461
_diffrn_reflns_av_R_equivalents  0.0857
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.245
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measured_fraction_theta_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_point_group_measured_fraction_full 0.974
_reflns_number_total             5322
_reflns_number_gt                3365
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
Rigaku CrystalClear-SM Expert 2.0 r3
;
_computing_cell_refinement       
;
Rigaku CrystalClear-SM Expert 2.0 r3
;
_computing_data_reduction        
;
Rigaku CrystalClear-SM Expert 2.0 r3
;
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'

_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'

_computing_publication_material  
;Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)
;

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0367P)²+3.2854P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr

_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5322
_refine_ls_number_parameters     317
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1535
_refine_ls_R_factor_gt           0.0966
_refine_ls_wR_factor_ref         0.1881
_refine_ls_wR_factor_gt          0.1618
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.080
_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_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
C1 C 0.2700(4) 0.4880(4) 0.7987(4) 0.0154(10) Uani 1 1 d . . . . .
C2 C 0.2834(4) 0.5903(4) 0.8465(4) 0.0128(10) Uani 1 1 d . . . . .
C3 C 0.2102(4) 0.6936(4) 0.8758(4) 0.0116(10) Uani 1 1 d . . . . .
C4 C 0.3051(4) 0.7495(4) 0.9127(4) 0.0115(10) Uani 1 1 d . . . . .
C5 C 0.2870(5) 0.8533(4) 0.9542(4) 0.0185(11) Uani 1 1 d . . . . .
H5 H 0.2015 0.9030 0.9606 0.022 Uiso 1 1 calc R U . . .
C6 C 0.3933(5) 0.8844(4) 0.9861(4) 0.0215(11) Uani 1 1 d . . . . .
H6 H 0.3793 0.9551 1.0153 0.026 Uiso 1 1 calc R U . . .
C7 C 0.5213(5) 0.8141(4) 0.9765(4) 0.0182(11) Uani 1 1 d . . . . .
H7 H 0.5932 0.8373 0.9984 0.022 Uiso 1 1 calc R U . . .
C8 C 0.5420(4) 0.7102(4) 0.9346(4) 0.0162(10) Uani 1 1 d . . . . .
H8 H 0.6281 0.6617 0.9274 0.019 Uiso 1 1 calc R U . . .
C9 C 0.4350(4) 0.6780(4) 0.9033(4) 0.0140(10) Uani 1 1 d . . . . .
C10 C 0.4240(4) 0.5764(4) 0.8604(4) 0.0102(9) Uani 1 1 d . . . . .
C11 C 0.4960(4) 0.4784(4) 0.8215(4) 0.0108(9) Uani 1 1 d . . . . .
C12 C 0.6302(4) 0.4132(4) 0.7990(4) 0.0129(10) Uani 1 1 d . . . . .
C13 C 0.7519(5) 0.4303(4) 0.8167(4) 0.0169(10) Uani 1 1 d . . . . .
H13 H 0.7568 0.4912 0.8544 0.020 Uiso 1 1 calc R U . . .
C14 C 0.8666(4) 0.3560(4) 0.7779(4) 0.0199(11) Uani 1 1 d . . . . .
H14 H 0.9510 0.3663 0.7886 0.024 Uiso 1 1 calc R U . . .
C15 C 0.8577(5) 0.2670(4) 0.7238(4) 0.0231(12) Uani 1 1 d . . . . .
H15 H 0.9369 0.2175 0.6975 0.028 Uiso 1 1 calc R U . . .
C16 C 0.7366(4) 0.2481(4) 0.7070(4) 0.0202(11) Uani 1 1 d . . . . .
H16 H 0.7329 0.1867 0.6697 0.024 Uiso 1 1 calc R U . . .
C17 C 0.6203(4) 0.3210(4) 0.7459(4) 0.0159(10) Uani 1 1 d . . . . .
C18 C 0.4777(4) 0.3243(4) 0.7368(4) 0.0171(11) Uani 1 1 d . . . . .
C19 C 0.4084(4) 0.4191(4) 0.7825(4) 0.0136(10) Uani 1 1 d . . . . .
C20 C -0.0716(5) 0.6430(4) 0.8963(5) 0.0326(14) Uani 1 1 d . . . . .
H20 H -0.0768 0.6108 0.9788 0.049 Uiso 1 1 calc R U . . .
H20A H -0.0304 0.5788 0.8550 0.049 Uiso 1 1 calc R U . . .
H20B H -0.1610 0.6775 0.8752 0.049 Uiso 1 1 calc R U . . .
C21 C -0.0420(5) 0.8698(4) 0.9524(4) 0.0230(12) Uani 1 1 d . . . . .
H21 H -0.1390 0.8840 0.9597 0.035 Uiso 1 1 calc R U . . .
H21A H -0.0122 0.9450 0.9188 0.035 Uiso 1 1 calc R U . . .
H21B H -0.0124 0.8380 1.0281 0.035 Uiso 1 1 calc R U . . .
C22 C 0.0217(5) 0.8414(4) 0.7045(4) 0.0195(11) Uani 1 1 d . . . . .
C23 C 0.1171(6) 0.9290(5) 0.6735(5) 0.0342(14) Uani 1 1 d . . . . .
H23 H 0.2078 0.8849 0.6822 0.051 Uiso 1 1 calc R U . . .
H23A H 0.0919 0.9861 0.7243 0.051 Uiso 1 1 calc R U . . .
H23B H 0.1125 0.9718 0.5940 0.051 Uiso 1 1 calc R U . . .
C24 C -0.1209(5) 0.9122(5) 0.6918(5) 0.0345(14) Uani 1 1 d . . . . .
H24 H -0.1260 0.9551 0.6125 0.052 Uiso 1 1 calc R U . . .
H24A H -0.1444 0.9695 0.7426 0.052 Uiso 1 1 calc R U . . .
H24B H -0.1826 0.8572 0.7124 0.052 Uiso 1 1 calc R U . . .
C25 C 0.0591(5) 0.7554(5) 0.6212(5) 0.0352(15) Uani 1 1 d . . . . .
H25 H 0.0492 0.8005 0.5432 0.053 Uiso 1 1 calc R U . . .
H25A H 0.0006 0.6974 0.6420 0.053 Uiso 1 1 calc R U . . .
H25B H 0.1513 0.7133 0.6254 0.053 Uiso 1 1 calc R U . . .
C26 C 0.2494(5) 0.1925(4) 0.7585(5) 0.0255(12) Uani 1 1 d . . . . .
H26 H 0.1860 0.2687 0.7519 0.038 Uiso 1 1 calc R U . . .
H26A H 0.2604 0.1593 0.8391 0.038 Uiso 1 1 calc R U . . .
H26B H 0.2162 0.1368 0.7271 0.038 Uiso 1 1 calc R U . . .
C27 C 0.5257(5) 0.0671(4) 0.6949(5) 0.0266(13) Uani 1 1 d . . . . .
H27 H 0.5578 0.0471 0.7699 0.040 Uiso 1 1 calc R U . . .
H27A H 0.6011 0.0693 0.6347 0.040 Uiso 1 1 calc R U . . .
H27B H 0.4777 0.0066 0.6891 0.040 Uiso 1 1 calc R U . . .
C28 C 0.3947(6) 0.2833(5) 0.5237(5) 0.0327(14) Uani 1 1 d . . . . .
C29 C 0.5321(6) 0.2989(6) 0.4573(5) 0.0529(19) Uani 1 1 d . . . . .
H29 H 0.5235 0.3290 0.3758 0.079 Uiso 1 1 calc R U . . .
H29A H 0.5939 0.2219 0.4675 0.079 Uiso 1 1 calc R U . . .
H29B H 0.5659 0.3558 0.4866 0.079 Uiso 1 1 calc R U . . .
C30 C 0.2969(6) 0.4033(5) 0.5088(5) 0.0426(16) Uani 1 1 d . . . . .
H30 H 0.2868 0.4334 0.4275 0.064 Uiso 1 1 calc R U . . .
H30A H 0.3307 0.4605 0.5374 0.064 Uiso 1 1 calc R U . . .
H30B H 0.2107 0.3927 0.5518 0.064 Uiso 1 1 calc R U . . .
C31 C 0.3425(7) 0.1970(6) 0.4705(5) 0.0524(19) Uani 1 1 d . . . . .
H31 H 0.2534 0.1884 0.5082 0.079 Uiso 1 1 calc R U . . .
H31A H 0.4022 0.1189 0.4812 0.079 Uiso 1 1 calc R U . . .
H31B H 0.3388 0.2294 0.3886 0.079 Uiso 1 1 calc R U . . .
Si1 Si 0.02977(12) 0.76004(11) 0.85804(12) 0.0139(3) Uani 1 1 d . . . . .
Si2 Si 0.41138(13) 0.21678(12) 0.67765(12) 0.0172(3) Uani 1 1 d . . . . .
O1 O 0.1686(3) 0.4670(3) 0.7769(3) 0.0227(8) 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
C1 O1 1.223(5) . ?
C1 C19 1.492(6) . ?
C1 C2 1.496(6) . ?
C2 C3 1.370(6) . ?
C2 C10 1.473(6) . ?
C3 C4 1.484(6) . ?
C3 Si1 1.894(4) . ?
C4 C5 1.391(6) . ?
C4 C9 1.424(6) . ?
C5 C6 1.384(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.404(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.391(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.393(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.445(6) . ?
C10 C11 1.363(6) . ?
C11 C12 1.450(6) . ?
C11 C19 1.464(6) . ?
C12 C13 1.391(6) . ?
C12 C17 1.416(6) . ?
C13 C14 1.394(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.387(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.388(7) . ?
C15 H15 0.9500 . ?
C16 C17 1.396(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.502(6) . ?
C18 C19 1.364(6) . ?
C18 Si2 1.895(5) . ?
C20 Si1 1.854(5) . ?
C20 H20 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C21 Si1 1.871(5) . ?
C21 H21 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C22 C23 1.536(7) . ?
C22 C25 1.537(6) . ?
C22 C24 1.544(6) . ?
C22 Si1 1.889(5) . ?
C23 H23 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C24 H24 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C25 H25 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C26 Si2 1.852(5) . ?
C26 H26 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C27 Si2 1.877(5) . ?
C27 H27 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C28 C30 1.534(8) . ?
C28 C29 1.550(8) . ?
C28 C31 1.558(8) . ?
C28 Si2 1.868(6) . ?
C29 H29 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C30 H30 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C31 H31 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 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 C1 C19 128.2(4) . . ?
O1 C1 C2 127.7(4) . . ?
C19 C1 C2 104.1(4) . . ?
C3 C2 C10 110.9(4) . . ?
C3 C2 C1 140.9(4) . . ?
C10 C2 C1 108.0(4) . . ?
C2 C3 C4 105.6(4) . . ?
C2 C3 Si1 127.3(3) . . ?
C4 C3 Si1 126.8(3) . . ?
C5 C4 C9 118.3(4) . . ?
C5 C4 C3 131.5(4) . . ?
C9 C4 C3 110.2(4) . . ?
C6 C5 C4 120.1(4) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 121.6(4) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C8 C7 C6 119.4(4) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C7 C8 C9 119.2(4) . . ?
C7 C8 H8 120.4 . . ?
C9 C8 H8 120.4 . . ?
C8 C9 C4 121.5(4) . . ?
C8 C9 C10 132.2(4) . . ?
C4 C9 C10 106.3(4) . . ?
C11 C10 C9 143.3(4) . . ?
C11 C10 C2 109.5(4) . . ?
C9 C10 C2 106.9(4) . . ?
C10 C11 C12 143.0(4) . . ?
C10 C11 C19 110.0(4) . . ?
C12 C11 C19 106.9(4) . . ?
C13 C12 C17 121.8(4) . . ?
C13 C12 C11 131.9(4) . . ?
C17 C12 C11 106.2(4) . . ?
C12 C13 C14 118.3(4) . . ?
C12 C13 H13 120.8 . . ?
C14 C13 H13 120.8 . . ?
C15 C14 C13 120.1(4) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C14 C15 C16 122.0(4) . . ?
C14 C15 H15 119.0 . . ?
C16 C15 H15 119.0 . . ?
C15 C16 C17 118.9(4) . . ?
C15 C16 H16 120.5 . . ?
C17 C16 H16 120.5 . . ?
C16 C17 C12 118.8(4) . . ?
C16 C17 C18 130.9(4) . . ?
C12 C17 C18 110.3(4) . . ?
C19 C18 C17 104.8(4) . . ?
C19 C18 Si2 128.4(3) . . ?
C17 C18 Si2 126.8(3) . . ?
C18 C19 C11 111.8(4) . . ?
C18 C19 C1 139.7(4) . . ?
C11 C19 C1 108.3(4) . . ?
Si1 C20 H20 109.5 . . ?
Si1 C20 H20A 109.5 . . ?
H20 C20 H20A 109.5 . . ?
Si1 C20 H20B 109.5 . . ?
H20 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
Si1 C21 H21 109.5 . . ?
Si1 C21 H21A 109.5 . . ?
H21 C21 H21A 109.5 . . ?
Si1 C21 H21B 109.5 . . ?
H21 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C23 C22 C25 108.9(4) . . ?
C23 C22 C24 108.9(4) . . ?
C25 C22 C24 108.9(4) . . ?
C23 C22 Si1 109.3(3) . . ?
C25 C22 Si1 112.0(3) . . ?
C24 C22 Si1 108.8(4) . . ?
C22 C23 H23 109.5 . . ?
C22 C23 H23A 109.5 . . ?
H23 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C24 H24 109.5 . . ?
C22 C24 H24A 109.5 . . ?
H24 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C25 H25 109.5 . . ?
C22 C25 H25A 109.5 . . ?
H25 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
Si2 C26 H26 109.5 . . ?
Si2 C26 H26A 109.5 . . ?
H26 C26 H26A 109.5 . . ?
Si2 C26 H26B 109.5 . . ?
H26 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Si2 C27 H27 109.5 . . ?
Si2 C27 H27A 109.5 . . ?
H27 C27 H27A 109.5 . . ?
Si2 C27 H27B 109.5 . . ?
H27 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C30 C28 C29 110.1(5) . . ?
C30 C28 C31 108.1(5) . . ?
C29 C28 C31 107.5(5) . . ?
C30 C28 Si2 111.7(4) . . ?
C29 C28 Si2 110.0(4) . . ?
C31 C28 Si2 109.3(4) . . ?
C28 C29 H29 109.5 . . ?
C28 C29 H29A 109.5 . . ?
H29 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C30 H30 109.5 . . ?
C28 C30 H30A 109.5 . . ?
H30 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C31 H31 109.5 . . ?
C28 C31 H31A 109.5 . . ?
H31 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
H31 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C20 Si1 C21 107.3(2) . . ?
C20 Si1 C22 111.2(3) . . ?
C21 Si1 C22 108.2(2) . . ?
C20 Si1 C3 111.1(2) . . ?
C21 Si1 C3 111.4(2) . . ?
C22 Si1 C3 107.7(2) . . ?
C26 Si2 C28 111.0(3) . . ?
C26 Si2 C27 106.5(2) . . ?
C28 Si2 C27 111.2(2) . . ?
C26 Si2 C18 110.2(2) . . ?
C28 Si2 C18 107.3(2) . . ?
C27 Si2 C18 110.6(2) . . ?

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
O1 C1 C2 C3 -5.4(10) . . . . ?
C19 C1 C2 C3 173.8(6) . . . . ?
O1 C1 C2 C10 178.8(5) . . . . ?
C19 C1 C2 C10 -2.0(5) . . . . ?
C10 C2 C3 C4 -1.1(5) . . . . ?
C1 C2 C3 C4 -176.8(6) . . . . ?
C10 C2 C3 Si1 173.0(3) . . . . ?
C1 C2 C3 Si1 -2.7(9) . . . . ?
C2 C3 C4 C5 -178.2(5) . . . . ?
Si1 C3 C4 C5 7.7(7) . . . . ?
C2 C3 C4 C9 0.7(5) . . . . ?
Si1 C3 C4 C9 -173.4(3) . . . . ?
C9 C4 C5 C6 -0.6(7) . . . . ?
C3 C4 C5 C6 178.1(5) . . . . ?
C4 C5 C6 C7 0.8(8) . . . . ?
C5 C6 C7 C8 -0.5(8) . . . . ?
C6 C7 C8 C9 -0.1(7) . . . . ?
C7 C8 C9 C4 0.4(7) . . . . ?
C7 C8 C9 C10 -178.4(5) . . . . ?
C5 C4 C9 C8 0.0(7) . . . . ?
C3 C4 C9 C8 -179.0(4) . . . . ?
C5 C4 C9 C10 179.0(4) . . . . ?
C3 C4 C9 C10 0.0(5) . . . . ?
C8 C9 C10 C11 -8.1(10) . . . . ?
C4 C9 C10 C11 173.0(6) . . . . ?
C8 C9 C10 C2 178.2(5) . . . . ?
C4 C9 C10 C2 -0.7(5) . . . . ?
C3 C2 C10 C11 -174.9(4) . . . . ?
C1 C2 C10 C11 2.3(5) . . . . ?
C3 C2 C10 C9 1.1(5) . . . . ?
C1 C2 C10 C9 178.3(4) . . . . ?
C9 C10 C11 C12 0.5(12) . . . . ?
C2 C10 C11 C12 174.1(6) . . . . ?
C9 C10 C11 C19 -175.2(6) . . . . ?
C2 C10 C11 C19 -1.6(5) . . . . ?
C10 C11 C12 C13 3.2(10) . . . . ?
C19 C11 C12 C13 178.9(5) . . . . ?
C10 C11 C12 C17 -174.3(6) . . . . ?
C19 C11 C12 C17 1.4(5) . . . . ?
C17 C12 C13 C14 1.7(7) . . . . ?
C11 C12 C13 C14 -175.4(5) . . . . ?
C12 C13 C14 C15 -0.4(7) . . . . ?
C13 C14 C15 C16 -0.4(8) . . . . ?
C14 C15 C16 C17 0.0(8) . . . . ?
C15 C16 C17 C12 1.3(7) . . . . ?
C15 C16 C17 C18 177.8(5) . . . . ?
C13 C12 C17 C16 -2.2(7) . . . . ?
C11 C12 C17 C16 175.6(4) . . . . ?
C13 C12 C17 C18 -179.4(4) . . . . ?
C11 C12 C17 C18 -1.6(5) . . . . ?
C16 C17 C18 C19 -175.6(5) . . . . ?
C12 C17 C18 C19 1.1(5) . . . . ?
C16 C17 C18 Si2 5.7(8) . . . . ?
C12 C17 C18 Si2 -177.5(4) . . . . ?
C17 C18 C19 C11 -0.2(5) . . . . ?
Si2 C18 C19 C11 178.4(4) . . . . ?
C17 C18 C19 C1 174.3(6) . . . . ?
Si2 C18 C19 C1 -7.1(9) . . . . ?
C10 C11 C19 C18 176.5(4) . . . . ?
C12 C11 C19 C18 -0.7(5) . . . . ?
C10 C11 C19 C1 0.2(5) . . . . ?
C12 C11 C19 C1 -177.0(4) . . . . ?
O1 C1 C19 C18 5.7(10) . . . . ?
C2 C1 C19 C18 -173.5(6) . . . . ?
O1 C1 C19 C11 -179.7(5) . . . . ?
C2 C1 C19 C11 1.1(5) . . . . ?
C23 C22 Si1 C20 -174.7(3) . . . . ?
C25 C22 Si1 C20 -53.9(4) . . . . ?
C24 C22 Si1 C20 66.5(4) . . . . ?
C23 C22 Si1 C21 67.8(4) . . . . ?
C25 C22 Si1 C21 -171.4(3) . . . . ?
C24 C22 Si1 C21 -51.0(4) . . . . ?
C23 C22 Si1 C3 -52.7(4) . . . . ?
C25 C22 Si1 C3 68.1(4) . . . . ?
C24 C22 Si1 C3 -171.5(3) . . . . ?
C2 C3 Si1 C20 41.2(5) . . . . ?
C4 C3 Si1 C20 -145.9(4) . . . . ?
C2 C3 Si1 C21 160.7(4) . . . . ?
C4 C3 Si1 C21 -26.4(5) . . . . ?
C2 C3 Si1 C22 -80.8(4) . . . . ?
C4 C3 Si1 C22 92.0(4) . . . . ?
C30 C28 Si2 C26 59.2(5) . . . . ?
C29 C28 Si2 C26 -178.2(4) . . . . ?
C31 C28 Si2 C26 -60.4(5) . . . . ?
C30 C28 Si2 C27 177.6(4) . . . . ?
C29 C28 Si2 C27 -59.9(5) . . . . ?
C31 C28 Si2 C27 57.9(5) . . . . ?
C30 C28 Si2 C18 -61.3(4) . . . . ?
C29 C28 Si2 C18 61.3(4) . . . . ?
C31 C28 Si2 C18 179.1(4) . . . . ?
C19 C18 Si2 C26 -33.7(5) . . . . ?
C17 C18 Si2 C26 144.7(4) . . . . ?
C19 C18 Si2 C28 87.3(5) . . . . ?
C17 C18 Si2 C28 -94.3(5) . . . . ?
C19 C18 Si2 C27 -151.2(5) . . . . ?
C17 C18 Si2 C27 27.2(5) . . . . ?

_refine_diff_density_max         1.031
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.082


_diffrn_radiation_source         'rotating-anode X-ray tube'
_diffrn_radiation_monochromator  Confocal
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_nsk1129a_twin1_hklf4
_database_code_depnum_ccdc_archive 'CCDC 1883888'
_audit_update_record             
;
2018-12-08 deposited with the CCDC.
2018-12-28 downloaded from the CCDC.
;
_audit_creation_date             2018-12-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        Ge
_chemical_formula_moiety         'C26 H28 Ge'
_chemical_formula_sum            'C26 H28 Ge'
_chemical_formula_weight         413.07
_chemical_melting_point          ?
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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   16.8701(6)
_cell_length_b                   16.9405(6)
_cell_length_c                   18.3624(3)
_cell_angle_alpha                100.752(2)
_cell_angle_beta                 100.803(2)
_cell_angle_gamma                119.398(4)
_cell_volume                     4246.4(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    10593
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_shelx_estimated_absorpt_T_max   0.760
_shelx_estimated_absorpt_T_min   0.670
_exptl_absorpt_coefficient_mu    1.450
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Rigaku Pilatus 200K'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orangish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
_exptl_crystal_recrystallization_method 
'An orange hot hexane solution of the compound  was prepared. Crystals suitable for X-rayanalysis were obtained by cooling the solution at room temperature.'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.056
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.904
_diffrn_reflns_Laue_measured_fraction_max 0.759
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18557
_diffrn_reflns_point_group_measured_fraction_full 0.904
_diffrn_reflns_point_group_measured_fraction_max 0.759
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.599
_diffrn_reflns_theta_min         1.835
_diffrn_ambient_temperature      113
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.759
_diffrn_measurement_device_type  'XTalAB P200'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                14319
_reflns_number_total             18557
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1019
_refine_ls_number_reflns         18557
_refine_ls_number_restraints     62
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0297
_refine_ls_restrained_S_all      0.983
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0342P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0648
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.5472(5)
 0.4528(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C00Z-C02X \\sim C00Z-C0AA
 with sigma of 0.02
 C00Z-C030 \\sim C00Z-C0
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C00Z \\sim C02X \\sim C030 \\sim C0AA \\sim C0: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 C00Z, C02X, C030, C0AA, C0
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(H00A)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=Sof(C0)=Sof(H0A)=Sof(H0B)=
 Sof(H0C)=1-FVAR(1)
 Sof(H00Z)=Sof(C02X)=Sof(H02K)=Sof(H02L)=Sof(H02M)=Sof(C030)=Sof(H03A)=
 Sof(H03B)=Sof(H03C)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 C00J(H00J), C00W(H00W), C00Z(H00Z), C00Z(H00A), C010(H010), C01N(H01N),
 C01S(H01S), C026(H026), C02G(H9AA)
7.b Aromatic/amide H refined with riding coordinates:
 C00F(H00H), C00L(H00L), C00R(H00R), C00S(H00S), C00U(H00U), C012(H012),
 C014(H014), C018(H018), C01B(H01B), C01E(H01E), C01F(H01F), C01G(H01K),
 C01H(H01H), C01M(H01M), C01T(H01T), C01U(H01U), C01V(H01V), C01W(H01W),
 C01X(H01X), C01Y(H01Y), C021(H021), C022(H022), C02A(H02N), C02C(H02O),
 C02E(H02P), C02F(H02Q), C02H(H02J), C02J(H02X), C02K(H0BA), C02R(H02R),
 C02T(H02T), C02W(H02W)
7.c Idealised Me refined as rotating group:
 C00N(H00B,H00C,H00D), C00Y(H00E,H00F,H00G), C01C(H01A,H01C,H01D), C01D(H01G,
 H01I,H01J), C023(H7AA,H,HA), C025(H02A,H02B,H02C), C027(H8AA,HB,HC), C028(H1AA,
 HD,HE), C029(H02D,H02E,H02F), C02B(H2AA,HF,HG), C02D(H02G,H02H,H02I),
 C02I(H02S,H02U,H02V), C02L(H3AA,HH,HI), C02M(H02Y,HJ,HK), C02N(H1BA,HL,HM),
 C02O(H4AA,HN,HO), C02P(H02Z,HP,HQ), C02Q(H5AA,HR,HS), C02U(H6AA,HT,HU),
 C02V(H2BA,HV,HW), C02X(H02K,H02L,H02M), C02Y(H3BA,HX,HY), C02Z(H02,HZ,H4BA),
 C030(H03A,H03B,H03C), C0AA(H0AA,H0AB,H0AC), C0(H0A,H0B,H0C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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
Ge01 Ge 0.39859(2) 0.54547(2) 0.20900(2) 0.01730(10) Uani 1 1 d . . . . .
Ge02 Ge 0.69842(2) 0.34127(2) 0.29257(2) 0.01700(8) Uani 1 1 d . . . . .
Ge03 Ge 0.20128(2) 0.85257(2) 0.27681(2) 0.01875(9) Uani 1 1 d . . . . .
Ge04 Ge -0.08562(2) 0.04999(2) 0.21936(2) 0.01908(10) Uani 1 1 d . . . . .
C005 C 0.3797(2) 0.4232(2) 0.15711(18) 0.0176(7) Uani 1 1 d . . . . .
C006 C 0.3911(2) 0.5068(2) 0.30145(18) 0.0161(7) Uani 1 1 d . . . . .
C007 C -0.1289(2) -0.1315(2) 0.22294(19) 0.0163(7) Uani 1 1 d . . . . .
C008 C 0.9746(2) 0.3955(2) 0.40051(19) 0.0201(7) Uani 1 1 d . . . . .
C009 C 0.3790(2) 0.8779(2) 0.27510(18) 0.0172(7) Uani 1 1 d . . . . .
C00A C 0.9783(2) 0.4122(2) 0.32821(18) 0.0203(7) Uani 1 1 d . . . . .
C00B C 0.4700(2) 0.8916(2) 0.32088(18) 0.0177(7) Uani 1 1 d . . . . .
C00C C 0.8336(2) 0.3790(2) 0.21333(19) 0.0158(7) Uani 1 1 d . . . . .
C00D C 0.3187(2) 0.8609(2) 0.32720(19) 0.0182(7) Uani 1 1 d . . . . .
C00E C 0.3674(2) 0.4079(2) 0.28421(19) 0.0176(7) Uani 1 1 d . . . . .
C00F C -0.1198(2) -0.0269(2) 0.49790(18) 0.0227(7) Uani 1 1 d . . . . .
H00H H -0.112298 0.026981 0.533068 0.027 Uiso 1 1 calc R . . . .
C00G C -0.1079(2) -0.0739(2) 0.16988(18) 0.0157(7) Uani 1 1 d . . . . .
C00H C 0.3606(2) 0.3643(2) 0.20871(18) 0.0170(7) Uani 1 1 d . . . . .
C00I C -0.1034(2) 0.0111(2) 0.31104(18) 0.0178(7) Uani 1 1 d . . . . .
C00J C 0.2863(2) 0.5502(2) 0.16516(19) 0.0266(8) Uani 1 1 d . . . . .
H00J H 0.287365 0.560211 0.113269 0.032 Uiso 1 1 calc R . . . .
C00K C 0.3644(2) 0.8787(2) 0.12992(18) 0.0174(7) Uani 1 1 d . . . . .
C00L C -0.1427(2) -0.1860(2) 0.39415(19) 0.0228(7) Uani 1 1 d . . . . .
H00L H -0.150064 -0.239950 0.359220 0.027 Uiso 1 1 calc R . . . .
C00M C -0.1235(2) -0.0865(2) 0.29708(19) 0.0154(7) Uani 1 1 d . . . . .
C00N C 0.1937(2) 0.4574(3) 0.1518(2) 0.0361(9) Uani 1 1 d . . . . .
H00B H 0.191346 0.404417 0.116802 0.054 Uiso 1 1 calc GR . . . .
H00C H 0.138955 0.460852 0.127902 0.054 Uiso 1 1 calc GR . . . .
H00D H 0.190680 0.446577 0.202110 0.054 Uiso 1 1 calc GR . . . .
C00O C 0.3388(2) 0.8736(2) 0.20200(19) 0.0162(7) Uani 1 1 d . . . . .
C00P C 0.8247(2) 0.3644(2) 0.34053(18) 0.0162(7) Uani 1 1 d . . . . .
C00Q C 0.8784(2) 0.3663(2) 0.40663(19) 0.0198(7) Uani 1 1 d . . . . .
C00R C 0.3444(2) 0.2045(2) 0.03623(18) 0.0243(8) Uani 1 1 d . . . . .
H00R H 0.350967 0.209186 -0.013306 0.029 Uiso 1 1 calc R . . . .
C00S C 0.9253(2) 0.3967(2) 0.0374(2) 0.0261(8) Uani 1 1 d . . . . .
H00S H 0.978084 0.406373 0.020045 0.031 Uiso 1 1 calc R . . . .
C00T C 0.8811(2) 0.3888(2) 0.28518(18) 0.0166(7) Uani 1 1 d . . . . .
C00U C -0.1374(2) -0.2937(2) 0.05662(19) 0.0283(8) Uani 1 1 d . . . . .
H00U H -0.126114 -0.289014 0.008360 0.034 Uiso 1 1 calc R . . . .
C00V C 0.6971(2) 0.3514(2) 0.12447(17) 0.0177(7) Uani 1 1 d . . . . .
C00W C 0.2102(2) 0.9715(2) 0.32578(18) 0.0274(8) Uani 1 1 d . . . . .
H00W H 0.198556 0.969714 0.377058 0.033 Uiso 1 1 calc R . . . .
C00X C 0.8533(2) 0.3845(2) 0.13907(18) 0.0186(7) Uani 1 1 d . . . . .
C00Y C 0.4215(2) 0.6368(2) 0.42177(19) 0.0281(8) Uani 1 1 d . . . . .
H00E H 0.436225 0.677545 0.388415 0.042 Uiso 1 1 calc GR . . . .
H00F H 0.477144 0.666435 0.469215 0.042 Uiso 1 1 calc GR . . . .
H00G H 0.365840 0.629429 0.436408 0.042 Uiso 1 1 calc GR . . . .
C00Z C 0.5859(2) 0.2165(2) 0.2798(2) 0.0343(9) Uani 1 1 d D U . . .
H00Z H 0.529533 0.204284 0.238549 0.041 Uiso 0.625(10) 1 calc R . P A 1
H00A H 0.533131 0.228656 0.270739 0.041 Uiso 0.375(10) 1 calc R . P A 2
C010 C 0.07517(19) 0.74001(19) 0.26240(17) 0.0232(7) Uani 1 1 d . . . . .
H010 H 0.026222 0.743891 0.225785 0.028 Uiso 1 1 calc R . . . .
C011 C 0.7706(2) 0.3685(2) 0.08533(17) 0.0163(7) Uani 1 1 d . . . . .
C012 C 0.6282(2) 0.9192(2) 0.3615(2) 0.0281(8) Uani 1 1 d . . . . .
H012 H 0.685585 0.931919 0.350995 0.034 Uiso 1 1 calc R . . . .
C013 C 0.4610(2) 0.8806(2) 0.39348(19) 0.0212(7) Uani 1 1 d . . . . .
C014 C 0.4451(2) 0.8931(2) 0.0342(2) 0.0279(8) Uani 1 1 d . . . . .
H014 H 0.499420 0.901959 0.019969 0.033 Uiso 1 1 calc R . . . .
C015 C -0.1311(2) -0.1087(2) 0.36990(18) 0.0167(7) Uani 1 1 d . . . . .
C016 C 0.2861(2) 0.8680(2) 0.07365(18) 0.0166(7) Uani 1 1 d . . . . .
C017 C 0.3986(2) 0.5398(2) 0.37760(18) 0.0180(7) Uani 1 1 d . . . . .
C018 C 0.7660(2) 0.3670(2) 0.00933(18) 0.0239(7) Uani 1 1 d . . . . .
H018 H 0.710004 0.355545 -0.026461 0.029 Uiso 1 1 calc R . . . .
C019 C -0.1036(2) 0.0438(2) 0.38468(18) 0.0196(8) Uani 1 1 d . . . . .
C01A C 0.2419(2) 0.8588(2) 0.18382(18) 0.0179(7) Uani 1 1 d . . . . .
C01B C 1.0536(2) 0.4086(2) 0.45264(18) 0.0299(8) Uani 1 1 d . . . . .
H01B H 1.049980 0.394351 0.500025 0.036 Uiso 1 1 calc R . . . .
C01C C 0.7703(2) 0.5423(2) 0.3470(2) 0.0353(9) Uani 1 1 d . . . . .
H01A H 0.831036 0.551179 0.375100 0.053 Uiso 1 1 calc GR . . . .
H01C H 0.764913 0.593939 0.374594 0.053 Uiso 1 1 calc GR . . . .
H01D H 0.768933 0.543663 0.293655 0.053 Uiso 1 1 calc GR . . . .
C01D C -0.0905(2) 0.1370(2) 0.42467(19) 0.0273(8) Uani 1 1 d . . . . .
H01G H -0.076277 0.177061 0.390712 0.041 Uiso 1 1 calc GR . . . .
H01I H -0.037044 0.170298 0.474201 0.041 Uiso 1 1 calc GR . . . .
H01J H -0.149659 0.124685 0.435261 0.041 Uiso 1 1 calc GR . . . .
C01E C 0.3430(2) 0.3027(2) 0.3765(2) 0.0264(8) Uani 1 1 d . . . . .
H01E H 0.329814 0.247344 0.338886 0.032 Uiso 1 1 calc R . . . .
C01F C 0.5553(2) 0.9129(2) 0.30546(19) 0.0254(7) Uani 1 1 d . . . . .
H01F H 0.563260 0.922867 0.257428 0.031 Uiso 1 1 calc R . . . .
C01G C -0.1722(2) -0.3081(2) 0.19806(19) 0.0221(7) Uani 1 1 d . . . . .
H01K H -0.184928 -0.314384 0.245627 0.026 Uiso 1 1 calc R . . . .
C01H C 0.5334(2) 0.8871(2) 0.44892(18) 0.0266(8) Uani 1 1 d . . . . .
H01H H 0.525975 0.878124 0.497319 0.032 Uiso 1 1 calc R . . . .
C01I C 0.3805(2) 0.4640(2) 0.41248(19) 0.0196(7) Uani 1 1 d . . . . .
C01J C 0.3540(2) 0.2797(2) 0.09188(18) 0.0194(7) Uani 1 1 d . . . . .
C01K C -0.1453(2) -0.2239(2) 0.18190(17) 0.0180(7) Uani 1 1 d . . . . .
C01L C 0.3614(2) 0.3835(2) 0.35603(18) 0.0176(7) Uani 1 1 d . . . . .
C01M C 0.9307(2) 0.3971(2) 0.11351(19) 0.0233(7) Uani 1 1 d . . . . .
H01M H 0.986062 0.405817 0.147980 0.028 Uiso 1 1 calc R . . . .
C01N C 0.5203(2) 0.6624(2) 0.2217(2) 0.0282(9) Uani 1 1 d . . . . .
H01N H 0.530758 0.714684 0.265899 0.034 Uiso 1 1 calc R . . . .
C01O C 0.7335(2) 0.3559(2) 0.19874(18) 0.0172(7) Uani 1 1 d . . . . .
C01P C 0.3763(2) 0.3741(2) 0.08816(17) 0.0184(7) Uani 1 1 d . . . . .
C01Q C 0.3429(2) 0.2728(2) 0.16534(18) 0.0210(7) Uani 1 1 d . . . . .
C01R C -0.1188(2) -0.0292(2) 0.42258(18) 0.0181(7) Uani 1 1 d . . . . .
C01S C 0.6866(2) 0.4463(2) 0.34326(18) 0.0236(7) Uani 1 1 d . . . . .
H01S H 0.689800 0.447088 0.398335 0.028 Uiso 1 1 calc R . . . .
C01T C 0.3819(2) 0.4647(2) 0.48825(18) 0.0210(7) Uani 1 1 d . . . . .
H01T H 0.395356 0.519966 0.526206 0.025 Uiso 1 1 calc R . . . .
C01U C 0.2874(2) 0.8682(2) -0.00133(19) 0.0242(8) Uani 1 1 d . . . . .
H01U H 0.233946 0.858726 -0.039125 0.029 Uiso 1 1 calc R . . . .
C01V C -0.1432(2) -0.1826(3) 0.4709(2) 0.0285(8) Uani 1 1 d . . . . .
H01V H -0.151612 -0.234947 0.487925 0.034 Uiso 1 1 calc R . . . .
C01W C 0.6178(2) 0.9071(2) 0.4331(2) 0.0319(8) Uani 1 1 d . . . . .
H01W H 0.668516 0.912522 0.471119 0.038 Uiso 1 1 calc R . . . .
C01X C 0.3680(2) 0.8824(2) -0.0205(2) 0.0265(8) Uani 1 1 d . . . . .
H01X H 0.370780 0.884895 -0.071276 0.032 Uiso 1 1 calc R . . . .
C01Y C -0.1619(2) -0.3763(2) 0.0754(2) 0.0304(8) Uani 1 1 d . . . . .
H01Y H -0.165776 -0.428063 0.040510 0.036 Uiso 1 1 calc R . . . .
C01Z C -0.1294(2) -0.2173(2) 0.10950(18) 0.0199(7) Uani 1 1 d . . . . .
C020 C -0.1072(2) -0.1245(2) 0.10342(18) 0.0183(7) Uani 1 1 d . . . . .
C021 C 0.4437(2) 0.8911(2) 0.10901(19) 0.0233(7) Uani 1 1 d . . . . .
H021 H 0.496532 0.898135 0.145675 0.028 Uiso 1 1 calc R . . . .
C022 C -0.1807(2) -0.3839(2) 0.1440(2) 0.0313(8) Uani 1 1 d . . . . .
H022 H -0.199997 -0.442057 0.155029 0.038 Uiso 1 1 calc R . . . .
C023 C -0.2840(2) -0.0171(3) 0.1625(2) 0.0408(10) Uani 1 1 d . . . . .
H7AA H -0.293093 -0.077940 0.135257 0.061 Uiso 1 1 calc GR . . . .
H H -0.334470 -0.010922 0.133366 0.061 Uiso 1 1 calc GR . . . .
HA H -0.287428 -0.015502 0.215405 0.061 Uiso 1 1 calc GR . . . .
C024 C 0.2110(2) 0.8549(2) 0.10930(17) 0.0188(7) Uani 1 1 d . . . . .
C025 C 0.6019(2) 0.3349(2) 0.08605(18) 0.0304(8) Uani 1 1 d . . . . .
H02A H 0.611063 0.394286 0.078768 0.046 Uiso 1 1 calc GR . . . .
H02B H 0.561256 0.314896 0.119155 0.046 Uiso 1 1 calc GR . . . .
H02C H 0.570841 0.284587 0.034922 0.046 Uiso 1 1 calc GR . . . .
C026 C -0.1870(2) 0.0646(2) 0.16795(19) 0.0277(8) Uani 1 1 d . . . . .
H026 H -0.186097 0.061730 0.113238 0.033 Uiso 1 1 calc R . . . .
C027 C -0.0868(2) -0.0944(2) 0.03422(19) 0.0275(8) Uani 1 1 d . . . . .
H8AA H -0.078938 -0.031981 0.040619 0.041 Uiso 1 1 calc GR . . . .
HB H -0.140571 -0.141996 -0.013489 0.041 Uiso 1 1 calc GR . . . .
HC H -0.027637 -0.089603 0.030070 0.041 Uiso 1 1 calc GR . . . .
C028 C 0.3117(2) 1.0565(2) 0.34219(19) 0.0366(9) Uani 1 1 d . . . . .
H1AA H 0.358301 1.048469 0.375105 0.055 Uiso 1 1 calc GR . . . .
HD H 0.317686 1.115705 0.369477 0.055 Uiso 1 1 calc GR . . . .
HE H 0.324297 1.060073 0.292560 0.055 Uiso 1 1 calc GR . . . .
C029 C 0.5891(2) 0.4285(3) 0.3019(2) 0.0428(10) Uani 1 1 d . . . . .
H02D H 0.583751 0.426934 0.247555 0.064 Uiso 1 1 calc GR . . . .
H02E H 0.583403 0.480094 0.329153 0.064 Uiso 1 1 calc GR . . . .
H02F H 0.537592 0.367022 0.302620 0.064 Uiso 1 1 calc GR . . . .
C02A C 0.3134(3) 0.1150(2) 0.1254(2) 0.0428(10) Uani 1 1 d . . . . .
H02N H 0.299131 0.057905 0.136823 0.051 Uiso 1 1 calc R . . . .
C02B C 0.1184(2) 0.8418(2) 0.06598(18) 0.0292(8) Uani 1 1 d . . . . .
H2AA H 0.132094 0.899335 0.052187 0.044 Uiso 1 1 calc GR . . . .
HF H 0.077578 0.831165 0.099405 0.044 Uiso 1 1 calc GR . . . .
HG H 0.084917 0.786317 0.018076 0.044 Uiso 1 1 calc GR . . . .
C02C C 0.3222(3) 0.1892(2) 0.1810(2) 0.0389(9) Uani 1 1 d . . . . .
H02O H 0.313912 0.182631 0.229775 0.047 Uiso 1 1 calc R . . . .
C02D C 0.8505(2) 0.3430(2) 0.47567(19) 0.0256(8) Uani 1 1 d . . . . .
H02G H 0.842918 0.281853 0.475837 0.038 Uiso 1 1 calc GR . . . .
H02H H 0.789563 0.338031 0.472779 0.038 Uiso 1 1 calc GR . . . .
H02I H 0.900739 0.393745 0.523889 0.038 Uiso 1 1 calc GR . . . .
C02E C 0.3439(2) 0.3034(2) 0.4526(2) 0.0311(8) Uani 1 1 d . . . . .
H02P H 0.330918 0.248077 0.466582 0.037 Uiso 1 1 calc R . . . .
C02F C 0.3248(2) 0.1221(2) 0.0551(2) 0.0354(9) Uani 1 1 d . . . . .
H02Q H 0.319306 0.070583 0.018441 0.043 Uiso 1 1 calc R . . . .
C02G C 0.0478(3) 0.1572(2) 0.2366(2) 0.0441(10) Uani 1 1 d . . . . .
H9AA H 0.088405 0.129737 0.241347 0.053 Uiso 1 1 calc R . . . .
C02H C 0.8447(2) 0.3825(2) -0.01410(19) 0.0277(8) Uani 1 1 d . . . . .
H02J H 0.843130 0.383452 -0.065909 0.033 Uiso 1 1 calc R . . . .
C02I C 0.3936(2) 0.4047(2) 0.01861(19) 0.0261(8) Uani 1 1 d . . . . .
H02S H 0.401578 0.467301 0.026220 0.039 Uiso 1 1 calc GR . . . .
H02U H 0.338671 0.357476 -0.028467 0.039 Uiso 1 1 calc GR . . . .
H02V H 0.452103 0.409429 0.012357 0.039 Uiso 1 1 calc GR . . . .
C02J C 0.3634(2) 0.3836(3) 0.5079(2) 0.0274(8) Uani 1 1 d . . . . .
H02X H 0.364180 0.383237 0.559675 0.033 Uiso 1 1 calc R . . . .
C02K C -0.1318(2) -0.1040(2) 0.52193(19) 0.0276(8) Uani 1 1 d . . . . .
H0BA H -0.132052 -0.102522 0.573840 0.033 Uiso 1 1 calc R . . . .
C02L C 0.1344(2) 0.9808(2) 0.2751(2) 0.0431(9) Uani 1 1 d . . . . .
H3AA H 0.141618 0.977979 0.223107 0.065 Uiso 1 1 calc GR . . . .
HH H 0.143050 1.042229 0.299869 0.065 Uiso 1 1 calc GR . . . .
HI H 0.070072 0.928283 0.269815 0.065 Uiso 1 1 calc GR . . . .
C02M C 0.2937(2) 0.6354(3) 0.2188(2) 0.0504(10) Uani 1 1 d . . . . .
H02Y H 0.295252 0.628350 0.270697 0.076 Uiso 1 1 calc GR . . . .
HJ H 0.237788 0.638026 0.196636 0.076 Uiso 1 1 calc GR . . . .
HK H 0.352701 0.694618 0.223485 0.076 Uiso 1 1 calc GR . . . .
C02N C 0.0879(2) 0.2348(2) 0.3113(2) 0.0579(10) Uani 1 1 d . . . . .
H1BA H 0.048503 0.262228 0.310981 0.087 Uiso 1 1 calc GR . . . .
HL H 0.154002 0.284809 0.317676 0.087 Uiso 1 1 calc GR . . . .
HM H 0.087967 0.209056 0.354822 0.087 Uiso 1 1 calc GR . . . .
C02O C 0.3337(2) 0.8477(3) 0.4652(2) 0.0305(8) Uani 1 1 d . . . . .
H4AA H 0.383457 0.900586 0.512557 0.046 Uiso 1 1 calc GR . . . .
HN H 0.322596 0.786954 0.470847 0.046 Uiso 1 1 calc GR . . . .
HO H 0.273859 0.846105 0.457903 0.046 Uiso 1 1 calc GR . . . .
C02P C 0.5176(3) 0.6935(3) 0.1502(2) 0.0559(12) Uani 1 1 d . . . . .
H02Z H 0.505358 0.642934 0.105108 0.084 Uiso 1 1 calc GR . . . .
HP H 0.579440 0.752342 0.159444 0.084 Uiso 1 1 calc GR . . . .
HQ H 0.466070 0.705600 0.139425 0.084 Uiso 1 1 calc GR . . . .
C02Q C 0.0524(2) 0.7428(3) 0.3386(2) 0.0587(13) Uani 1 1 d . . . . .
H5AA H 0.098536 0.738590 0.376390 0.088 Uiso 1 1 calc GR . . . .
HR H -0.012914 0.688579 0.328758 0.088 Uiso 1 1 calc GR . . . .
HS H 0.057022 0.802920 0.360020 0.088 Uiso 1 1 calc GR . . . .
C02R C 1.1386(2) 0.4429(3) 0.4349(2) 0.0375(9) Uani 1 1 d . . . . .
H02R H 1.193693 0.452425 0.470525 0.045 Uiso 1 1 calc R . . . .
C02S C 0.3661(2) 0.8618(2) 0.39580(19) 0.0210(7) Uani 1 1 d . . . . .
C02T C 1.1438(2) 0.4633(2) 0.3656(2) 0.0397(9) Uani 1 1 d . . . . .
H02T H 1.202881 0.487772 0.354806 0.048 Uiso 1 1 calc R . . . .
C02U C 0.0656(2) 0.6474(2) 0.2228(3) 0.0674(14) Uani 1 1 d . . . . .
H6AA H 0.072761 0.646524 0.171006 0.101 Uiso 1 1 calc GR . . . .
HT H 0.002126 0.592950 0.217058 0.101 Uiso 1 1 calc GR . . . .
HU H 0.115740 0.642961 0.254893 0.101 Uiso 1 1 calc GR . . . .
C02V C -0.1699(3) 0.1626(2) 0.2088(2) 0.0477(9) Uani 1 1 d . . . . .
H2BA H -0.171041 0.167363 0.262541 0.072 Uiso 1 1 calc GR . . . .
HV H -0.220672 0.168556 0.179799 0.072 Uiso 1 1 calc GR . . . .
HW H -0.107164 0.214119 0.209902 0.072 Uiso 1 1 calc GR . . . .
C02W C 1.0647(2) 0.4488(2) 0.31199(18) 0.0277(8) Uani 1 1 d . . . . .
H02W H 1.069124 0.463526 0.264869 0.033 Uiso 1 1 calc R . . . .
C02X C 0.5650(6) 0.2234(6) 0.3594(4) 0.057(3) Uani 0.625(10) 1 d D U P A 1
H02K H 0.622812 0.243716 0.401743 0.086 Uiso 0.625(10) 1 calc GR . P A 1
H02L H 0.512135 0.160540 0.356449 0.086 Uiso 0.625(10) 1 calc GR . P A 1
H02M H 0.547012 0.270222 0.369839 0.086 Uiso 0.625(10) 1 calc GR . P A 1
C02Y C 0.0546(3) 0.1904(3) 0.1657(2) 0.0627(13) Uani 1 1 d . . . . .
H3BA H 0.032465 0.136119 0.119397 0.094 Uiso 1 1 calc GR . . . .
HX H 0.121622 0.240364 0.174586 0.094 Uiso 1 1 calc GR . . . .
HY H 0.014212 0.216309 0.157201 0.094 Uiso 1 1 calc GR . . . .
C02Z C 0.6037(2) 0.6525(3) 0.2435(3) 0.0726(16) Uani 1 1 d . . . . .
H02 H 0.605732 0.634192 0.291117 0.109 Uiso 1 1 calc GR . . . .
HZ H 0.663410 0.713686 0.253232 0.109 Uiso 1 1 calc GR . . . .
H4BA H 0.596827 0.602963 0.200675 0.109 Uiso 1 1 calc GR . . . .
C030 C 0.6014(5) 0.1390(4) 0.2550(5) 0.058(2) Uani 0.625(10) 1 d D U P A 1
H03A H 0.623093 0.143413 0.209155 0.087 Uiso 0.625(10) 1 calc GR . P A 1
H03B H 0.541018 0.076947 0.241400 0.087 Uiso 0.625(10) 1 calc GR . P A 1
H03C H 0.650482 0.144906 0.297910 0.087 Uiso 0.625(10) 1 calc GR . P A 1
C0AA C 0.5820(11) 0.1884(9) 0.3520(7) 0.060(4) Uani 0.375(10) 1 d D U P A 2
H0AA H 0.637245 0.183719 0.371373 0.090 Uiso 0.375(10) 1 calc GR . P A 2
H0AB H 0.522245 0.126125 0.339648 0.090 Uiso 0.375(10) 1 calc GR . P A 2
H0AC H 0.583837 0.236723 0.392305 0.090 Uiso 0.375(10) 1 calc GR . P A 2
C0 C 0.5537(10) 0.1394(7) 0.2064(8) 0.088(4) Uani 0.375(10) 1 d D U P A 2
H0A H 0.531493 0.155389 0.161475 0.131 Uiso 0.375(10) 1 calc GR . P A 2
H0B H 0.500887 0.078789 0.207071 0.131 Uiso 0.375(10) 1 calc GR . P A 2
H0C H 0.607508 0.133147 0.201981 0.131 Uiso 0.375(10) 1 calc GR . P A 2


_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
Ge01 C005 1.950(3) . ?
Ge01 C006 1.934(3) . ?
Ge01 C00J 1.961(3) . ?
Ge01 C01N 1.963(3) . ?
Ge02 C00P 1.953(3) . ?
Ge02 C00Z 1.959(3) . ?
Ge02 C01O 1.944(3) . ?
Ge02 C01S 1.968(3) . ?
Ge03 C00D 1.947(3) . ?
Ge03 C00W 1.966(3) . ?
Ge03 C010 1.962(3) . ?
Ge03 C01A 1.957(3) . ?
Ge04 C00G 1.939(3) . ?
Ge04 C00I 1.941(3) . ?
Ge04 C026 1.943(3) . ?
Ge04 C02G 1.992(3) . ?
C005 C00H 1.466(4) . ?
C005 C01P 1.353(4) . ?
C006 C00E 1.471(4) . ?
C006 C017 1.362(4) . ?
C007 C00G 1.473(4) . ?
C007 C00M 1.393(4) . ?
C007 C01K 1.467(4) . ?
C008 C00A 1.414(4) . ?
C008 C00Q 1.481(4) . ?
C008 C01B 1.376(4) . ?
C009 C00B 1.487(4) . ?
C009 C00D 1.488(4) . ?
C009 C00O 1.357(4) . ?
C00A C00T 1.494(4) . ?
C00A C02W 1.394(4) . ?
C00B C013 1.406(4) . ?
C00B C01F 1.400(4) . ?
C00C C00T 1.342(4) . ?
C00C C00X 1.472(4) . ?
C00C C01O 1.490(4) . ?
C00D C02S 1.352(4) . ?
C00E C00H 1.398(4) . ?
C00E C01L 1.460(4) . ?
C00F C01R 1.380(4) . ?
C00F C02K 1.389(4) . ?
C00G C020 1.360(4) . ?
C00H C01Q 1.457(4) . ?
C00I C00M 1.474(4) . ?
C00I C019 1.363(4) . ?
C00J C00N 1.508(4) . ?
C00J C02M 1.521(4) . ?
C00K C00O 1.471(4) . ?
C00K C016 1.424(4) . ?
C00K C021 1.390(4) . ?
C00L C015 1.396(4) . ?
C00L C01V 1.401(4) . ?
C00M C015 1.466(4) . ?
C00O C01A 1.487(4) . ?
C00P C00Q 1.356(4) . ?
C00P C00T 1.497(4) . ?
C00Q C02D 1.487(4) . ?
C00R C01J 1.393(4) . ?
C00R C02F 1.395(4) . ?
C00S C01M 1.382(4) . ?
C00S C02H 1.384(5) . ?
C00U C01Y 1.384(4) . ?
C00U C01Z 1.395(4) . ?
C00V C011 1.482(4) . ?
C00V C01O 1.358(4) . ?
C00V C025 1.489(4) . ?
C00W C028 1.523(4) . ?
C00W C02L 1.527(4) . ?
C00X C011 1.417(4) . ?
C00X C01M 1.401(4) . ?
C00Y C017 1.507(4) . ?
C00Z C02X 1.562(7) . ?
C00Z C030 1.469(6) . ?
C00Z C0AA 1.491(11) . ?
C00Z C0 1.480(10) . ?
C010 C02Q 1.518(4) . ?
C010 C02U 1.515(4) . ?
C011 C018 1.378(4) . ?
C012 C01F 1.392(4) . ?
C012 C01W 1.396(4) . ?
C013 C01H 1.379(4) . ?
C013 C02S 1.482(4) . ?
C014 C01X 1.394(5) . ?
C014 C021 1.384(4) . ?
C015 C01R 1.399(5) . ?
C016 C01U 1.382(4) . ?
C016 C024 1.473(4) . ?
C017 C01I 1.464(4) . ?
C018 C02H 1.389(4) . ?
C019 C01D 1.498(4) . ?
C019 C01R 1.469(4) . ?
C01A C024 1.347(4) . ?
C01B C02R 1.389(4) . ?
C01C C01S 1.520(4) . ?
C01E C01L 1.389(4) . ?
C01E C02E 1.391(4) . ?
C01G C01K 1.379(4) . ?
C01G C022 1.395(5) . ?
C01H C01W 1.395(4) . ?
C01I C01L 1.398(5) . ?
C01I C01T 1.385(4) . ?
C01J C01P 1.472(4) . ?
C01J C01Q 1.414(4) . ?
C01K C01Z 1.418(4) . ?
C01N C02P 1.504(4) . ?
C01N C02Z 1.488(4) . ?
C01P C02I 1.491(4) . ?
C01Q C02C 1.383(4) . ?
C01S C029 1.527(4) . ?
C01T C02J 1.386(4) . ?
C01U C01X 1.386(4) . ?
C01V C02K 1.379(5) . ?
C01Y C022 1.369(4) . ?
C01Z C020 1.459(4) . ?
C020 C027 1.491(4) . ?
C023 C026 1.505(4) . ?
C024 C02B 1.501(4) . ?
C026 C02V 1.545(4) . ?
C02A C02C 1.388(5) . ?
C02A C02F 1.360(5) . ?
C02E C02J 1.381(5) . ?
C02G C02N 1.474(4) . ?
C02G C02Y 1.513(4) . ?
C02O C02S 1.493(4) . ?
C02R C02T 1.387(4) . ?
C02T C02W 1.380(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C005 Ge01 C00J 111.38(13) . . ?
C005 Ge01 C01N 117.35(13) . . ?
C006 Ge01 C005 87.45(12) . . ?
C006 Ge01 C00J 110.45(13) . . ?
C006 Ge01 C01N 115.38(13) . . ?
C00J Ge01 C01N 112.46(13) . . ?
C00P Ge02 C00Z 116.90(14) . . ?
C00P Ge02 C01S 111.83(12) . . ?
C00Z Ge02 C01S 111.02(15) . . ?
C01O Ge02 C00P 87.84(12) . . ?
C01O Ge02 C00Z 115.77(14) . . ?
C01O Ge02 C01S 111.67(12) . . ?
C00D Ge03 C00W 109.65(13) . . ?
C00D Ge03 C010 120.23(12) . . ?
C00D Ge03 C01A 87.21(13) . . ?
C010 Ge03 C00W 110.79(13) . . ?
C01A Ge03 C00W 110.53(13) . . ?
C01A Ge03 C010 116.35(13) . . ?
C00G Ge04 C00I 87.70(13) . . ?
C00G Ge04 C026 112.17(12) . . ?
C00G Ge04 C02G 112.13(14) . . ?
C00I Ge04 C026 112.83(13) . . ?
C00I Ge04 C02G 113.93(14) . . ?
C026 Ge04 C02G 115.08(15) . . ?
C00H C005 Ge01 109.8(2) . . ?
C01P C005 Ge01 140.5(2) . . ?
C01P C005 C00H 109.6(3) . . ?
C00E C006 Ge01 110.4(2) . . ?
C017 C006 Ge01 141.2(2) . . ?
C017 C006 C00E 108.4(3) . . ?
C00M C007 C00G 116.3(3) . . ?
C00M C007 C01K 136.5(3) . . ?
C01K C007 C00G 107.0(3) . . ?
C00A C008 C00Q 109.1(3) . . ?
C01B C008 C00A 120.6(3) . . ?
C01B C008 C00Q 130.3(3) . . ?
C00B C009 C00D 105.8(3) . . ?
C00O C009 C00B 137.7(3) . . ?
C00O C009 C00D 116.4(3) . . ?
C008 C00A C00T 107.0(3) . . ?
C02W C00A C008 119.7(3) . . ?
C02W C00A C00T 133.2(3) . . ?
C013 C00B C009 107.0(3) . . ?
C01F C00B C009 133.3(3) . . ?
C01F C00B C013 119.6(3) . . ?
C00T C00C C00X 136.8(3) . . ?
C00T C00C C01O 117.3(3) . . ?
C00X C00C C01O 105.9(3) . . ?
C009 C00D Ge03 109.7(2) . . ?
C02S C00D Ge03 140.7(2) . . ?
C02S C00D C009 109.5(3) . . ?
C00H C00E C006 115.8(3) . . ?
C00H C00E C01L 137.1(3) . . ?
C01L C00E C006 107.1(3) . . ?
C01R C00F C02K 119.5(3) . . ?
C007 C00G Ge04 109.9(2) . . ?
C020 C00G Ge04 141.0(2) . . ?
C020 C00G C007 109.0(3) . . ?
C00E C00H C005 116.2(3) . . ?
C00E C00H C01Q 136.7(3) . . ?
C01Q C00H C005 107.1(3) . . ?
C00M C00I Ge04 110.2(2) . . ?
C019 C00I Ge04 141.1(3) . . ?
C019 C00I C00M 108.7(3) . . ?
C00N C00J Ge01 111.3(2) . . ?
C00N C00J C02M 111.8(3) . . ?
C02M C00J Ge01 109.5(2) . . ?
C016 C00K C00O 106.8(3) . . ?
C021 C00K C00O 134.1(3) . . ?
C021 C00K C016 119.1(3) . . ?
C015 C00L C01V 118.9(3) . . ?
C007 C00M C00I 115.7(3) . . ?
C007 C00M C015 137.4(3) . . ?
C015 C00M C00I 106.9(3) . . ?
C009 C00O C00K 137.3(3) . . ?
C009 C00O C01A 116.9(3) . . ?
C00K C00O C01A 105.8(3) . . ?
C00Q C00P Ge02 141.6(2) . . ?
C00Q C00P C00T 109.8(3) . . ?
C00T C00P Ge02 108.6(2) . . ?
C008 C00Q C02D 122.8(3) . . ?
C00P C00Q C008 108.7(3) . . ?
C00P C00Q C02D 128.6(3) . . ?
C01J C00R C02F 118.3(3) . . ?
C01M C00S C02H 121.3(3) . . ?
C00A C00T C00P 105.3(3) . . ?
C00C C00T C00A 137.9(3) . . ?
C00C C00T C00P 116.7(3) . . ?
C01Y C00U C01Z 119.1(3) . . ?
C011 C00V C025 123.5(3) . . ?
C01O C00V C011 108.2(3) . . ?
C01O C00V C025 128.3(3) . . ?
C028 C00W Ge03 109.1(2) . . ?
C028 C00W C02L 111.6(3) . . ?
C02L C00W Ge03 111.6(2) . . ?
C011 C00X C00C 107.2(3) . . ?
C01M C00X C00C 133.7(3) . . ?
C01M C00X C011 119.0(3) . . ?
C02X C00Z Ge02 107.3(4) . . ?
C030 C00Z Ge02 111.3(3) . . ?
C030 C00Z C02X 112.8(5) . . ?
C0AA C00Z Ge02 116.0(6) . . ?
C0 C00Z Ge02 115.2(4) . . ?
C0 C00Z C0AA 116.3(7) . . ?
C02Q C010 Ge03 111.4(2) . . ?
C02U C010 Ge03 111.8(2) . . ?
C02U C010 C02Q 113.4(3) . . ?
C00X C011 C00V 108.8(3) . . ?
C018 C011 C00V 130.0(3) . . ?
C018 C011 C00X 121.1(3) . . ?
C01F C012 C01W 120.7(3) . . ?
C00B C013 C02S 108.8(3) . . ?
C01H C013 C00B 121.1(3) . . ?
C01H C013 C02S 130.1(3) . . ?
C021 C014 C01X 121.2(3) . . ?
C00L C015 C00M 133.6(3) . . ?
C00L C015 C01R 119.7(3) . . ?
C01R C015 C00M 106.6(3) . . ?
C00K C016 C024 108.8(3) . . ?
C01U C016 C00K 121.0(3) . . ?
C01U C016 C024 130.2(3) . . ?
C006 C017 C00Y 127.9(3) . . ?
C006 C017 C01I 108.6(3) . . ?
C01I C017 C00Y 123.6(3) . . ?
C011 C018 C02H 118.9(3) . . ?
C00I C019 C01D 128.8(3) . . ?
C00I C019 C01R 108.3(3) . . ?
C01R C019 C01D 122.9(3) . . ?
C00O C01A Ge03 109.3(2) . . ?
C024 C01A Ge03 140.6(2) . . ?
C024 C01A C00O 110.1(3) . . ?
C008 C01B C02R 119.0(3) . . ?
C01L C01E C02E 119.5(3) . . ?
C012 C01F C00B 119.0(3) . . ?
C01K C01G C022 119.5(3) . . ?
C013 C01H C01W 119.2(3) . . ?
C01L C01I C017 109.2(3) . . ?
C01T C01I C017 129.6(3) . . ?
C01T C01I C01L 121.2(3) . . ?
C00R C01J C01P 129.6(3) . . ?
C00R C01J C01Q 121.2(3) . . ?
C01Q C01J C01P 109.1(3) . . ?
C01G C01K C007 134.9(3) . . ?
C01G C01K C01Z 119.1(3) . . ?
C01Z C01K C007 105.9(3) . . ?
C01E C01L C00E 134.1(3) . . ?
C01E C01L C01I 119.1(3) . . ?
C01I C01L C00E 106.7(3) . . ?
C00S C01M C00X 119.0(3) . . ?
C02P C01N Ge01 112.4(2) . . ?
C02Z C01N Ge01 112.0(2) . . ?
C02Z C01N C02P 110.4(3) . . ?
C00C C01O Ge02 109.1(2) . . ?
C00V C01O Ge02 141.2(2) . . ?
C00V C01O C00C 109.8(3) . . ?
C005 C01P C01J 107.9(2) . . ?
C005 C01P C02I 129.5(3) . . ?
C01J C01P C02I 122.6(3) . . ?
C01J C01Q C00H 106.2(3) . . ?
C02C C01Q C00H 135.3(3) . . ?
C02C C01Q C01J 118.4(3) . . ?
C00F C01R C015 120.8(3) . . ?
C00F C01R C019 129.8(3) . . ?
C015 C01R C019 109.4(3) . . ?
C01C C01S Ge02 110.6(2) . . ?
C01C C01S C029 112.5(3) . . ?
C029 C01S Ge02 110.5(2) . . ?
C01I C01T C02J 119.0(3) . . ?
C016 C01U C01X 118.9(3) . . ?
C02K C01V C00L 120.7(3) . . ?
C01H C01W C012 120.3(3) . . ?
C01U C01X C014 120.4(3) . . ?
C022 C01Y C00U 120.3(3) . . ?
C00U C01Z C01K 120.5(3) . . ?
C00U C01Z C020 130.1(3) . . ?
C01K C01Z C020 109.4(3) . . ?
C00G C020 C01Z 108.6(2) . . ?
C00G C020 C027 128.2(3) . . ?
C01Z C020 C027 123.2(3) . . ?
C014 C021 C00K 119.3(3) . . ?
C01Y C022 C01G 121.4(3) . . ?
C016 C024 C02B 122.8(3) . . ?
C01A C024 C016 108.5(3) . . ?
C01A C024 C02B 128.7(3) . . ?
C023 C026 Ge04 110.5(2) . . ?
C023 C026 C02V 111.6(3) . . ?
C02V C026 Ge04 111.9(2) . . ?
C02F C02A C02C 121.5(3) . . ?
C01Q C02C C02A 120.0(3) . . ?
C02J C02E C01E 120.7(3) . . ?
C02A C02F C00R 120.6(3) . . ?
C02N C02G Ge04 112.6(2) . . ?
C02N C02G C02Y 114.3(3) . . ?
C02Y C02G Ge04 111.3(2) . . ?
C00S C02H C018 120.6(3) . . ?
C02E C02J C01T 120.3(3) . . ?
C01V C02K C00F 120.4(3) . . ?
C02T C02R C01B 120.6(3) . . ?
C00D C02S C013 108.8(3) . . ?
C00D C02S C02O 128.5(3) . . ?
C013 C02S C02O 122.7(3) . . ?
C02W C02T C02R 121.2(3) . . ?
C02T C02W C00A 118.8(3) . . ?

_olex2_submission_original_sample_id NSK1129
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.5472(5)
2 0.4528(5)

####################################################################### 
# 
# 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_ydkr_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1883889'
_audit_update_record             
;
2018-12-08 deposited with the CCDC.
2018-12-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H38 O2 S Si2'
_chemical_formula_weight         518.84

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'
S S 0.1246 0.1234 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.249(2)
_cell_length_b                   11.586(3)
_cell_length_c                   12.434(3)
_cell_angle_alpha                82.379(9)
_cell_angle_beta                 77.407(8)
_cell_angle_gamma                85.599(8)
_cell_volume                     1426.5(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    93

_cell_measurement_reflns_used    5068

_cell_measurement_theta_min      2.0

_cell_measurement_theta_max      30.9


_exptl_crystal_description       Platelet

_exptl_crystal_colour            Orange

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_F_000             556
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.33

_exptl_crystal_size_mid          0.32

_exptl_crystal_size_min          0.20

_exptl_absorpt_coefficient_mu    0.222
_shelx_estimated_absorpt_T_min   0.930
_shelx_estimated_absorpt_T_max   0.957
_exptl_absorpt_correction_type   Multi-scan

_exptl_absorpt_correction_T_min  0.942

_exptl_absorpt_correction_T_max  1.000

_exptl_absorpt_process_details   ?

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93

_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  
;
Rigaku CrystalClear-SM Expert 2.0 r3
;

_diffrn_measurement_method       'profile data from ω-scans'

_diffrn_detector_area_resol_mean 28.5714

_diffrn_reflns_number            17768
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.910
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.998
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.982
_reflns_number_total             4927
_reflns_number_gt                4741
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
Rigaku CrystalClear-SM Expert 2.0 r3
;
_computing_cell_refinement       
;
Rigaku CrystalClear-SM Expert 2.0 r3
;
_computing_data_reduction        
;
Rigaku CrystalClear-SM Expert 2.0 r3
;
_computing_structure_solution    ?

_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'

_computing_publication_material  
;Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)
;

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0366P)²+1.0590P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    ?

_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4927
_refine_ls_number_parameters     326
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0357
_refine_ls_wR_factor_ref         0.0884
_refine_ls_wR_factor_gt          0.0874
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_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_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
S1 S 0.77127(4) 0.20901(3) 0.50828(3) 0.01225(11) Uani 1 1 d . . . . .
Si1 Si 0.97913(4) 0.15354(4) 0.22305(4) 0.01308(12) Uani 1 1 d . . . . .
Si2 Si 0.59383(4) 0.34683(4) 0.76626(4) 0.01359(12) Uani 1 1 d . . . . .
O1 O 0.83105(11) 0.32018(10) 0.47860(9) 0.0180(3) Uani 1 1 d . . . . .
O2 O 0.83917(11) 0.11763(10) 0.56909(9) 0.0179(3) Uani 1 1 d . . . . .
C2 C 0.79768(15) 0.13044(13) 0.29166(13) 0.0128(3) Uani 1 1 d . . . . .
C18 C 0.60076(15) 0.22245(13) 0.57458(13) 0.0121(3) Uani 1 1 d . . . . .
C17 C 0.52965(15) 0.26781(13) 0.66585(13) 0.0130(3) Uani 1 1 d . . . . .
C9 C 0.58719(15) 0.13618(13) 0.41513(13) 0.0121(3) Uani 1 1 d . . . . .
C1 C 0.73071(15) 0.15606(13) 0.39325(13) 0.0119(3) Uani 1 1 d . . . . .
C10 C 0.51732(15) 0.17199(13) 0.51265(13) 0.0124(3) Uani 1 1 d . . . . .
C3 C 0.69304(15) 0.08697(13) 0.24245(13) 0.0132(3) Uani 1 1 d . . . . .
C7 C 0.45334(16) 0.05287(14) 0.28966(13) 0.0145(3) Uani 1 1 d . . . . .
H1 H 0.369007 0.055278 0.339797 0.017 Uiso 1 1 calc R U . . .
C11 C 0.38036(15) 0.18650(13) 0.57531(13) 0.0130(3) Uani 1 1 d . . . . .
C16 C 0.38731(16) 0.24582(14) 0.66705(13) 0.0137(3) Uani 1 1 d . . . . .
C12 C 0.25795(16) 0.15830(14) 0.55762(13) 0.0159(3) Uani 1 1 d . . . . .
H2 H 0.253951 0.118002 0.496761 0.019 Uiso 1 1 calc R U . . .
C8 C 0.56643(15) 0.09057(13) 0.31680(13) 0.0125(3) Uani 1 1 d . . . . .
C19 C 1.07916(16) 0.16293(15) 0.32931(14) 0.0180(4) Uani 1 1 d . . . . .
H9 H 1.075076 0.089822 0.379326 0.027 Uiso 1 1 calc R U . . .
H10 H 1.042707 0.227631 0.372074 0.027 Uiso 1 1 calc R U . . .
H11 H 1.172449 0.176291 0.292547 0.027 Uiso 1 1 calc R U . . .
C6 C 0.46631(16) 0.01156(14) 0.18756(14) 0.0181(4) Uani 1 1 d . . . . .
H3 H 0.390000 -0.014265 0.167641 0.022 Uiso 1 1 calc R U . . .
C26 C 0.77440(17) 0.30478(16) 0.76012(15) 0.0211(4) Uani 1 1 d . . . . .
H12 H 0.804502 0.337832 0.818608 0.032 Uiso 1 1 calc R U . . .
H13 H 0.827071 0.334801 0.687519 0.032 Uiso 1 1 calc R U . . .
H14 H 0.786517 0.219621 0.771023 0.032 Uiso 1 1 calc R U . . .
C13 C 0.14132(16) 0.19013(15) 0.63063(14) 0.0196(4) Uani 1 1 d . . . . .
H4 H 0.056859 0.171914 0.619348 0.024 Uiso 1 1 calc R U . . .
C25 C 0.50204(19) 0.30185(17) 0.91140(14) 0.0248(4) Uani 1 1 d . . . . .
H15 H 0.499311 0.216686 0.924296 0.037 Uiso 1 1 calc R U . . .
H16 H 0.410508 0.336434 0.922016 0.037 Uiso 1 1 calc R U . . .
H17 H 0.548216 0.328864 0.963939 0.037 Uiso 1 1 calc R U . . .
C24 C 0.98733(17) 0.29398(15) 0.12405(14) 0.0188(4) Uani 1 1 d . . . . .
C4 C 0.70411(16) 0.04541(14) 0.14086(14) 0.0172(3) Uani 1 1 d . . . . .
H5 H 0.788025 0.042654 0.090189 0.021 Uiso 1 1 calc R U . . .
C5 C 0.58999(17) 0.00773(15) 0.11436(14) 0.0194(4) Uani 1 1 d . . . . .
H6 H 0.596958 -0.021011 0.045129 0.023 Uiso 1 1 calc R U . . .
C15 C 0.27048(16) 0.27639(15) 0.73918(14) 0.0183(4) Uani 1 1 d . . . . .
H7 H 0.273583 0.315777 0.800838 0.022 Uiso 1 1 calc R U . . .
C20 C 1.05058(17) 0.02729(16) 0.14545(15) 0.0243(4) Uani 1 1 d . . . . .
H18 H 1.148335 0.029876 0.125531 0.036 Uiso 1 1 calc R U . . .
H19 H 1.015138 0.031758 0.077823 0.036 Uiso 1 1 calc R U . . .
H20 H 1.025659 -0.045819 0.192384 0.036 Uiso 1 1 calc R U . . .
C30 C 0.57067(17) 0.50958(15) 0.72629(15) 0.0214(4) Uani 1 1 d . . . . .
C14 C 0.14773(16) 0.24849(16) 0.72005(14) 0.0213(4) Uani 1 1 d . . . . .
H8 H 0.067211 0.269792 0.769044 0.026 Uiso 1 1 calc R U . . .
C22 C 0.88782(19) 0.29858(18) 0.04721(16) 0.0285(4) Uani 1 1 d . . . . .
H21 H 0.796358 0.296316 0.091849 0.043 Uiso 1 1 calc R U . . .
H22 H 0.906432 0.231514 0.004798 0.043 Uiso 1 1 calc R U . . .
H23 H 0.897161 0.370847 -0.004030 0.043 Uiso 1 1 calc R U . . .
C23 C 1.12994(18) 0.30162(17) 0.05213(15) 0.0254(4) Uani 1 1 d . . . . .
H24 H 1.147412 0.238925 0.004378 0.038 Uiso 1 1 calc R U . . .
H25 H 1.194937 0.293594 0.100273 0.038 Uiso 1 1 calc R U . . .
H26 H 1.138189 0.377220 0.005984 0.038 Uiso 1 1 calc R U . . .
C21 C 0.95602(18) 0.39861(16) 0.19145(15) 0.0242(4) Uani 1 1 d . . . . .
H27 H 0.956020 0.470956 0.140704 0.036 Uiso 1 1 calc R U . . .
H28 H 1.024255 0.400358 0.235425 0.036 Uiso 1 1 calc R U . . .
H29 H 0.867834 0.391158 0.241141 0.036 Uiso 1 1 calc R U . . .
C27 C 0.4229(2) 0.54732(17) 0.7350(2) 0.0406(6) Uani 1 1 d . . . . .
H30 H 0.373095 0.524315 0.810569 0.061 Uiso 1 1 calc R U . . .
H31 H 0.386842 0.509655 0.682338 0.061 Uiso 1 1 calc R U . . .
H32 H 0.413880 0.632178 0.717510 0.061 Uiso 1 1 calc R U . . .
C28 C 0.6278(2) 0.57358(18) 0.8045(2) 0.0401(5) Uani 1 1 d . . . . .
H33 H 0.616661 0.657929 0.784594 0.060 Uiso 1 1 calc R U . . .
H34 H 0.723197 0.551369 0.797819 0.060 Uiso 1 1 calc R U . . .
H35 H 0.580160 0.552405 0.881149 0.060 Uiso 1 1 calc R U . . .
C29 C 0.6466(3) 0.54355(18) 0.60710(19) 0.0446(6) Uani 1 1 d . . . . .
H36 H 0.608753 0.505324 0.555910 0.067 Uiso 1 1 calc R U . . .
H37 H 0.741298 0.518743 0.600518 0.067 Uiso 1 1 calc R U . . .
H38 H 0.638268 0.628314 0.588626 0.067 Uiso 1 1 calc R U . . .


_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
S1 O1 1.4376(12) . ?
S1 O2 1.4425(12) . ?
S1 C18 1.7669(16) . ?
S1 C1 1.7681(16) . ?
Si1 C19 1.8586(17) . ?
Si1 C20 1.8733(18) . ?
Si1 C2 1.8925(16) . ?
Si1 C24 1.9012(18) . ?
Si2 C26 1.8649(17) . ?
Si2 C25 1.8706(18) . ?
Si2 C17 1.8930(16) . ?
Si2 C30 1.8955(18) . ?
C2 C1 1.358(2) . ?
C2 C3 1.493(2) . ?
C18 C17 1.354(2) . ?
C18 C10 1.466(2) . ?
C17 C16 1.497(2) . ?
C9 C10 1.366(2) . ?
C9 C8 1.457(2) . ?
C9 C1 1.467(2) . ?
C10 C11 1.459(2) . ?
C3 C4 1.390(2) . ?
C3 C8 1.421(2) . ?
C7 C8 1.391(2) . ?
C7 C6 1.391(2) . ?
C7 H1 0.9500 . ?
C11 C12 1.390(2) . ?
C11 C16 1.425(2) . ?
C16 C15 1.384(2) . ?
C12 C13 1.392(2) . ?
C12 H2 0.9500 . ?
C19 H9 0.9800 . ?
C19 H10 0.9800 . ?
C19 H11 0.9800 . ?
C6 C5 1.392(2) . ?
C6 H3 0.9500 . ?
C26 H12 0.9800 . ?
C26 H13 0.9800 . ?
C26 H14 0.9800 . ?
C13 C14 1.391(2) . ?
C13 H4 0.9500 . ?
C25 H15 0.9800 . ?
C25 H16 0.9800 . ?
C25 H17 0.9800 . ?
C24 C22 1.536(2) . ?
C24 C21 1.539(3) . ?
C24 C23 1.540(2) . ?
C4 C5 1.397(2) . ?
C4 H5 0.9500 . ?
C5 H6 0.9500 . ?
C15 C14 1.399(2) . ?
C15 H7 0.9500 . ?
C20 H18 0.9800 . ?
C20 H19 0.9800 . ?
C20 H20 0.9800 . ?
C30 C27 1.529(3) . ?
C30 C28 1.531(3) . ?
C30 C29 1.532(3) . ?
C14 H8 0.9500 . ?
C22 H21 0.9800 . ?
C22 H22 0.9800 . ?
C22 H23 0.9800 . ?
C23 H24 0.9800 . ?
C23 H25 0.9800 . ?
C23 H26 0.9800 . ?
C21 H27 0.9800 . ?
C21 H28 0.9800 . ?
C21 H29 0.9800 . ?
C27 H30 0.9800 . ?
C27 H31 0.9800 . ?
C27 H32 0.9800 . ?
C28 H33 0.9800 . ?
C28 H34 0.9800 . ?
C28 H35 0.9800 . ?
C29 H36 0.9800 . ?
C29 H37 0.9800 . ?
C29 H38 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 S1 O2 117.93(7) . . ?
O1 S1 C18 112.11(7) . . ?
O2 S1 C18 109.97(7) . . ?
O1 S1 C1 112.16(7) . . ?
O2 S1 C1 109.86(7) . . ?
C18 S1 C1 91.78(7) . . ?
C19 Si1 C20 107.85(8) . . ?
C19 Si1 C2 110.38(7) . . ?
C20 Si1 C2 109.85(8) . . ?
C19 Si1 C24 110.17(8) . . ?
C20 Si1 C24 110.24(8) . . ?
C2 Si1 C24 108.36(7) . . ?
C26 Si2 C25 107.19(9) . . ?
C26 Si2 C17 109.60(7) . . ?
C25 Si2 C17 109.82(8) . . ?
C26 Si2 C30 110.31(8) . . ?
C25 Si2 C30 111.31(8) . . ?
C17 Si2 C30 108.59(8) . . ?
C1 C2 C3 104.17(13) . . ?
C1 C2 Si1 128.36(12) . . ?
C3 C2 Si1 127.36(12) . . ?
C17 C18 C10 113.46(14) . . ?
C17 C18 S1 136.28(13) . . ?
C10 C18 S1 110.26(11) . . ?
C18 C17 C16 104.31(13) . . ?
C18 C17 Si2 128.14(12) . . ?
C16 C17 Si2 127.51(12) . . ?
C10 C9 C8 140.96(14) . . ?
C10 C9 C1 113.54(14) . . ?
C8 C9 C1 105.29(13) . . ?
C2 C1 C9 113.36(14) . . ?
C2 C1 S1 136.43(12) . . ?
C9 C1 S1 110.21(11) . . ?
C9 C10 C11 140.78(15) . . ?
C9 C10 C18 113.59(14) . . ?
C11 C10 C18 105.38(13) . . ?
C4 C3 C8 119.51(14) . . ?
C4 C3 C2 129.97(15) . . ?
C8 C3 C2 110.52(13) . . ?
C8 C7 C6 118.63(15) . . ?
C8 C7 H1 120.7 . . ?
C6 C7 H1 120.7 . . ?
C12 C11 C16 120.93(14) . . ?
C12 C11 C10 132.50(15) . . ?
C16 C11 C10 106.51(13) . . ?
C15 C16 C11 119.53(15) . . ?
C15 C16 C17 130.14(15) . . ?
C11 C16 C17 110.31(13) . . ?
C11 C12 C13 118.83(15) . . ?
C11 C12 H2 120.6 . . ?
C13 C12 H2 120.6 . . ?
C7 C8 C3 121.06(14) . . ?
C7 C8 C9 132.29(15) . . ?
C3 C8 C9 106.64(13) . . ?
Si1 C19 H9 109.5 . . ?
Si1 C19 H10 109.5 . . ?
H9 C19 H10 109.5 . . ?
Si1 C19 H11 109.5 . . ?
H9 C19 H11 109.5 . . ?
H10 C19 H11 109.5 . . ?
C7 C6 C5 120.62(15) . . ?
C7 C6 H3 119.7 . . ?
C5 C6 H3 119.7 . . ?
Si2 C26 H12 109.5 . . ?
Si2 C26 H13 109.5 . . ?
H12 C26 H13 109.5 . . ?
Si2 C26 H14 109.5 . . ?
H12 C26 H14 109.5 . . ?
H13 C26 H14 109.5 . . ?
C14 C13 C12 120.38(15) . . ?
C14 C13 H4 119.8 . . ?
C12 C13 H4 119.8 . . ?
Si2 C25 H15 109.5 . . ?
Si2 C25 H16 109.5 . . ?
H15 C25 H16 109.5 . . ?
Si2 C25 H17 109.5 . . ?
H15 C25 H17 109.5 . . ?
H16 C25 H17 109.5 . . ?
C22 C24 C21 109.07(15) . . ?
C22 C24 C23 108.63(14) . . ?
C21 C24 C23 109.26(14) . . ?
C22 C24 Si1 111.95(12) . . ?
C21 C24 Si1 109.28(12) . . ?
C23 C24 Si1 108.61(12) . . ?
C3 C4 C5 119.01(15) . . ?
C3 C4 H5 120.5 . . ?
C5 C4 H5 120.5 . . ?
C6 C5 C4 121.17(15) . . ?
C6 C5 H6 119.4 . . ?
C4 C5 H6 119.4 . . ?
C16 C15 C14 119.06(15) . . ?
C16 C15 H7 120.5 . . ?
C14 C15 H7 120.5 . . ?
Si1 C20 H18 109.5 . . ?
Si1 C20 H19 109.5 . . ?
H18 C20 H19 109.5 . . ?
Si1 C20 H20 109.5 . . ?
H18 C20 H20 109.5 . . ?
H19 C20 H20 109.5 . . ?
C27 C30 C28 109.08(16) . . ?
C27 C30 C29 108.90(18) . . ?
C28 C30 C29 108.67(17) . . ?
C27 C30 Si2 111.46(13) . . ?
C28 C30 Si2 108.64(13) . . ?
C29 C30 Si2 110.05(13) . . ?
C13 C14 C15 121.26(15) . . ?
C13 C14 H8 119.4 . . ?
C15 C14 H8 119.4 . . ?
C24 C22 H21 109.5 . . ?
C24 C22 H22 109.5 . . ?
H21 C22 H22 109.5 . . ?
C24 C22 H23 109.5 . . ?
H21 C22 H23 109.5 . . ?
H22 C22 H23 109.5 . . ?
C24 C23 H24 109.5 . . ?
C24 C23 H25 109.5 . . ?
H24 C23 H25 109.5 . . ?
C24 C23 H26 109.5 . . ?
H24 C23 H26 109.5 . . ?
H25 C23 H26 109.5 . . ?
C24 C21 H27 109.5 . . ?
C24 C21 H28 109.5 . . ?
H27 C21 H28 109.5 . . ?
C24 C21 H29 109.5 . . ?
H27 C21 H29 109.5 . . ?
H28 C21 H29 109.5 . . ?
C30 C27 H30 109.5 . . ?
C30 C27 H31 109.5 . . ?
H30 C27 H31 109.5 . . ?
C30 C27 H32 109.5 . . ?
H30 C27 H32 109.5 . . ?
H31 C27 H32 109.5 . . ?
C30 C28 H33 109.5 . . ?
C30 C28 H34 109.5 . . ?
H33 C28 H34 109.5 . . ?
C30 C28 H35 109.5 . . ?
H33 C28 H35 109.5 . . ?
H34 C28 H35 109.5 . . ?
C30 C29 H36 109.5 . . ?
C30 C29 H37 109.5 . . ?
H36 C29 H37 109.5 . . ?
C30 C29 H38 109.5 . . ?
H36 C29 H38 109.5 . . ?
H37 C29 H38 109.5 . . ?

_refine_diff_density_max         0.365
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.046


_diffrn_radiation_source         ?
_diffrn_radiation_monochromator  Confocal
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_ydkr_merge
_database_code_depnum_ccdc_archive 'CCDC 1883890'
_audit_update_record             
;
2018-12-08 deposited with the CCDC.
2018-12-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H43 O P Si2'
_chemical_formula_weight         578.85

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'
P P 0.1023 0.0942 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_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                   15.237(4)
_cell_length_b                   10.387(3)
_cell_length_c                   20.841(5)
_cell_angle_alpha                90
_cell_angle_beta                 107.636(3)
_cell_angle_gamma                90
_cell_volume                     3143.4(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    93

_cell_measurement_reflns_used    10678

_cell_measurement_theta_min      2.4

_cell_measurement_theta_max      31.2


_exptl_crystal_description       Block

_exptl_crystal_colour            Orange

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_F_000             1240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.191
_shelx_estimated_absorpt_T_min   0.945
_shelx_estimated_absorpt_T_max   0.981
_exptl_absorpt_correction_type   Multi-scan

_exptl_absorpt_correction_T_min  0.892

_exptl_absorpt_correction_T_max  1.000

_exptl_absorpt_process_details   ?

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  
;
Rigaku CrystalClear-SM Expert 2.0 r3
;

_diffrn_measurement_method       'profile data from ω-scans'

_diffrn_detector_area_resol_mean 28.5714

_diffrn_reflns_number            27633
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.411
_diffrn_reflns_theta_max         31.302
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.864
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.864
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.864
_diffrn_reflns_point_group_measured_fraction_full 0.983
_reflns_number_total             8879
_reflns_number_gt                7593
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
Rigaku CrystalClear-SM Expert 2.0 r3
;
_computing_cell_refinement       
;
Rigaku CrystalClear-SM Expert 2.0 r3
;
_computing_data_reduction        
;
Rigaku CrystalClear-SM Expert 2.0 r3
;
_computing_structure_solution    ?

_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'

_computing_publication_material  
;Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)
;

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0468P)²+1.5093P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    ?

_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8879
_refine_ls_number_parameters     371
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0454
_refine_ls_wR_factor_ref         0.1092
_refine_ls_wR_factor_gt          0.1024
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.073
_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_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
C1 C 0.22540(9) 0.37781(12) 0.51189(7) 0.0132(2) Uani 1 1 d . . . . .
C2 C 0.17424(9) 0.41615(12) 0.55214(7) 0.0134(2) Uani 1 1 d . . . . .
C3 C 0.18434(9) 0.55894(12) 0.55763(7) 0.0139(3) Uani 1 1 d . . . . .
C4 C 0.14432(10) 0.64798(13) 0.58991(7) 0.0167(3) Uani 1 1 d . . . . .
H1 H 0.104467 0.620277 0.614483 0.020 Uiso 1 1 calc R U . . .
C5 C 0.16338(10) 0.77901(13) 0.58582(7) 0.0182(3) Uani 1 1 d . . . . .
H2 H 0.136076 0.840197 0.607811 0.022 Uiso 1 1 calc R U . . .
C6 C 0.22161(11) 0.82106(13) 0.55010(8) 0.0192(3) Uani 1 1 d . . . . .
H3 H 0.234296 0.910316 0.548329 0.023 Uiso 1 1 calc R U . . .
C7 C 0.26146(10) 0.73283(13) 0.51689(7) 0.0176(3) Uani 1 1 d . . . . .
H4 H 0.300310 0.761625 0.491737 0.021 Uiso 1 1 calc R U . . .
C8 C 0.24377(9) 0.60211(13) 0.52094(7) 0.0138(3) Uani 1 1 d . . . . .
C9 C 0.27251(9) 0.48785(12) 0.49204(7) 0.0134(2) Uani 1 1 d . . . . .
C10 C 0.33047(9) 0.45416(12) 0.45590(7) 0.0132(2) Uani 1 1 d . . . . .
C11 C 0.39823(10) 0.51390(13) 0.42901(7) 0.0142(3) Uani 1 1 d . . . . .
C12 C 0.43428(10) 0.63802(13) 0.43424(7) 0.0167(3) Uani 1 1 d . . . . .
H5 H 0.411323 0.703652 0.456580 0.020 Uiso 1 1 calc R U . . .
C13 C 0.50461(10) 0.66451(14) 0.40617(8) 0.0188(3) Uani 1 1 d . . . . .
H6 H 0.529751 0.748787 0.409173 0.023 Uiso 1 1 calc R U . . .
C14 C 0.53794(10) 0.56758(15) 0.37380(8) 0.0199(3) Uani 1 1 d . . . . .
H7 H 0.585952 0.586798 0.354995 0.024 Uiso 1 1 calc R U . . .
C15 C 0.50247(10) 0.44256(14) 0.36829(7) 0.0188(3) Uani 1 1 d . . . . .
H8 H 0.525740 0.377551 0.345782 0.023 Uiso 1 1 calc R U . . .
C16 C 0.43254(10) 0.41490(13) 0.39628(7) 0.0147(3) Uani 1 1 d . . . . .
C17 C 0.38691(9) 0.28992(13) 0.40160(7) 0.0140(3) Uani 1 1 d . . . . .
C18 C 0.32870(9) 0.31581(12) 0.43874(7) 0.0133(2) Uani 1 1 d . . . . .
C19 C 0.15209(9) 0.18446(12) 0.41024(7) 0.0135(3) Uani 1 1 d . . . . .
C20 C 0.09770(10) 0.27764(13) 0.36830(7) 0.0168(3) Uani 1 1 d . . . . .
H9 H 0.112811 0.366232 0.375837 0.020 Uiso 1 1 calc R U . . .
C21 C 0.02150(10) 0.24087(15) 0.31555(8) 0.0205(3) Uani 1 1 d . . . . .
H10 H -0.015436 0.304222 0.286907 0.025 Uiso 1 1 calc R U . . .
C22 C -0.00063(10) 0.11113(15) 0.30474(8) 0.0208(3) Uani 1 1 d . . . . .
H11 H -0.052625 0.085895 0.268582 0.025 Uiso 1 1 calc R U . . .
C23 C 0.05306(10) 0.01845(14) 0.34663(8) 0.0192(3) Uani 1 1 d . . . . .
H12 H 0.037794 -0.070072 0.338982 0.023 Uiso 1 1 calc R U . . .
C24 C 0.12898(10) 0.05460(13) 0.39968(7) 0.0161(3) Uani 1 1 d . . . . .
H13 H 0.165089 -0.008926 0.428704 0.019 Uiso 1 1 calc R U . . .
C25 C 0.00261(10) 0.39076(15) 0.60140(8) 0.0199(3) Uani 1 1 d . . . . .
H14 H -0.025775 0.437641 0.559421 0.030 Uiso 1 1 calc R U . . .
H15 H 0.017633 0.451178 0.639293 0.030 Uiso 1 1 calc R U . . .
H16 H -0.040474 0.325650 0.607896 0.030 Uiso 1 1 calc R U . . .
C26 C 0.07872(10) 0.15491(14) 0.55038(8) 0.0187(3) Uani 1 1 d . . . . .
H17 H 0.038431 0.172236 0.504732 0.028 Uiso 1 1 calc R U . . .
H18 H 0.046347 0.100001 0.574086 0.028 Uiso 1 1 calc R U . . .
H19 H 0.134569 0.111067 0.547937 0.028 Uiso 1 1 calc R U . . .
C27 C 0.19139(10) 0.28069(13) 0.68498(7) 0.0155(3) Uani 1 1 d . . . . .
C28 C 0.22556(13) 0.40895(15) 0.72002(8) 0.0281(4) Uani 1 1 d . . . . .
H20 H 0.172788 0.460163 0.722753 0.042 Uiso 1 1 calc R U . . .
H21 H 0.259141 0.456333 0.694207 0.042 Uiso 1 1 calc R U . . .
H22 H 0.266586 0.392366 0.765520 0.042 Uiso 1 1 calc R U . . .
C29 C 0.14111(11) 0.20696(15) 0.72726(8) 0.0210(3) Uani 1 1 d . . . . .
H23 H 0.122851 0.121901 0.707331 0.032 Uiso 1 1 calc R U . . .
H24 H 0.086160 0.255105 0.728108 0.032 Uiso 1 1 calc R U . . .
H25 H 0.182230 0.196824 0.773307 0.032 Uiso 1 1 calc R U . . .
C30 C 0.27490(10) 0.20113(15) 0.68178(8) 0.0226(3) Uani 1 1 d . . . . .
H26 H 0.316436 0.187858 0.727446 0.034 Uiso 1 1 calc R U . . .
H27 H 0.307601 0.247225 0.654898 0.034 Uiso 1 1 calc R U . . .
H28 H 0.253966 0.117527 0.660947 0.034 Uiso 1 1 calc R U . . .
C31 C 0.36819(11) -0.00633(14) 0.40371(8) 0.0227(3) Uani 1 1 d . . . . .
H29 H 0.384438 -0.086931 0.385645 0.034 Uiso 1 1 calc R U . . .
H30 H 0.301436 -0.003082 0.395642 0.034 Uiso 1 1 calc R U . . .
H31 H 0.399659 -0.002063 0.452221 0.034 Uiso 1 1 calc R U . . .
C32 C 0.52922(11) 0.10722(16) 0.36970(9) 0.0254(3) Uani 1 1 d . . . . .
H32 H 0.566309 0.124516 0.416247 0.038 Uiso 1 1 calc R U . . .
H33 H 0.547872 0.165686 0.339291 0.038 Uiso 1 1 calc R U . . .
H34 H 0.538742 0.017951 0.358115 0.038 Uiso 1 1 calc R U . . .
C33 C 0.33312(10) 0.13847(13) 0.26861(7) 0.0172(3) Uani 1 1 d . . . . .
C34 C 0.22981(11) 0.14380(17) 0.26191(8) 0.0244(3) Uani 1 1 d . . . . .
H35 H 0.193978 0.147252 0.214164 0.037 Uiso 1 1 calc R U . . .
H36 H 0.217071 0.220729 0.284827 0.037 Uiso 1 1 calc R U . . .
H37 H 0.212571 0.066811 0.282479 0.037 Uiso 1 1 calc R U . . .
C35 C 0.35738(12) 0.25663(16) 0.23305(8) 0.0247(3) Uani 1 1 d . . . . .
H38 H 0.423117 0.254820 0.237010 0.037 Uiso 1 1 calc R U . . .
H39 H 0.343402 0.335227 0.254076 0.037 Uiso 1 1 calc R U . . .
H40 H 0.321094 0.255248 0.185370 0.037 Uiso 1 1 calc R U . . .
C36 C 0.35193(13) 0.01668(16) 0.23320(9) 0.0290(4) Uani 1 1 d . . . . .
H41 H 0.338209 -0.059598 0.256135 0.043 Uiso 1 1 calc R U . . .
H42 H 0.416802 0.015031 0.234629 0.043 Uiso 1 1 calc R U . . .
H43 H 0.312788 0.016824 0.186224 0.043 Uiso 1 1 calc R U . . .
P1 P 0.25404(2) 0.23034(3) 0.47695(2) 0.01201(8) Uani 1 1 d . . . . .
Si1 Si 0.11072(3) 0.30992(3) 0.59679(2) 0.01281(9) Uani 1 1 d . . . . .
Si2 Si 0.40450(3) 0.13305(4) 0.36102(2) 0.01484(9) Uani 1 1 d . . . . .
O1 O 0.29419(7) 0.12226(9) 0.52304(5) 0.0160(2) 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
C1 C2 1.3661(18) . ?
C1 C9 1.4740(18) . ?
C1 P1 1.8055(14) . ?
C2 C3 1.4919(18) . ?
C2 Si1 1.8883(14) . ?
C3 C4 1.3887(19) . ?
C3 C8 1.4230(18) . ?
C4 C5 1.3996(19) . ?
C4 H1 0.9500 . ?
C5 C6 1.390(2) . ?
C5 H2 0.9500 . ?
C6 C7 1.394(2) . ?
C6 H3 0.9500 . ?
C7 C8 1.3919(18) . ?
C7 H4 0.9500 . ?
C8 C9 1.4570(18) . ?
C9 C10 1.3686(19) . ?
C10 C11 1.4544(18) . ?
C10 C18 1.4791(18) . ?
C11 C12 1.3926(18) . ?
C11 C16 1.4186(19) . ?
C12 C13 1.395(2) . ?
C12 H5 0.9500 . ?
C13 C14 1.391(2) . ?
C13 H6 0.9500 . ?
C14 C15 1.398(2) . ?
C14 H7 0.9500 . ?
C15 C16 1.3911(19) . ?
C15 H8 0.9500 . ?
C16 C17 1.4925(18) . ?
C17 C18 1.3689(18) . ?
C17 Si2 1.8920(15) . ?
C18 P1 1.8070(14) . ?
C19 C24 1.3946(18) . ?
C19 C20 1.3960(19) . ?
C19 P1 1.8067(15) . ?
C20 C21 1.389(2) . ?
C20 H9 0.9500 . ?
C21 C22 1.391(2) . ?
C21 H10 0.9500 . ?
C22 C23 1.388(2) . ?
C22 H11 0.9500 . ?
C23 C24 1.388(2) . ?
C23 H12 0.9500 . ?
C24 H13 0.9500 . ?
C25 Si1 1.8772(15) . ?
C25 H14 0.9800 . ?
C25 H15 0.9800 . ?
C25 H16 0.9800 . ?
C26 Si1 1.8654(15) . ?
C26 H17 0.9800 . ?
C26 H18 0.9800 . ?
C26 H19 0.9800 . ?
C27 C28 1.533(2) . ?
C27 C30 1.536(2) . ?
C27 C29 1.5360(19) . ?
C27 Si1 1.9005(15) . ?
C28 H20 0.9800 . ?
C28 H21 0.9800 . ?
C28 H22 0.9800 . ?
C29 H23 0.9800 . ?
C29 H24 0.9800 . ?
C29 H25 0.9800 . ?
C30 H26 0.9800 . ?
C30 H27 0.9800 . ?
C30 H28 0.9800 . ?
C31 Si2 1.8685(15) . ?
C31 H29 0.9800 . ?
C31 H30 0.9800 . ?
C31 H31 0.9800 . ?
C32 Si2 1.8729(16) . ?
C32 H32 0.9800 . ?
C32 H33 0.9800 . ?
C32 H34 0.9800 . ?
C33 C36 1.535(2) . ?
C33 C35 1.536(2) . ?
C33 C34 1.539(2) . ?
C33 Si2 1.9042(16) . ?
C34 H35 0.9800 . ?
C34 H36 0.9800 . ?
C34 H37 0.9800 . ?
C35 H38 0.9800 . ?
C35 H39 0.9800 . ?
C35 H40 0.9800 . ?
C36 H41 0.9800 . ?
C36 H42 0.9800 . ?
C36 H43 0.9800 . ?
P1 O1 1.4837(10) . ?

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
C2 C1 C9 111.30(12) . . ?
C2 C1 P1 138.39(10) . . ?
C9 C1 P1 110.30(10) . . ?
C1 C2 C3 105.78(11) . . ?
C1 C2 Si1 127.25(10) . . ?
C3 C2 Si1 126.84(10) . . ?
C4 C3 C8 119.65(12) . . ?
C4 C3 C2 130.47(13) . . ?
C8 C3 C2 109.86(11) . . ?
C3 C4 C5 119.25(13) . . ?
C3 C4 H1 120.4 . . ?
C5 C4 H1 120.4 . . ?
C6 C5 C4 121.06(13) . . ?
C6 C5 H2 119.5 . . ?
C4 C5 H2 119.5 . . ?
C5 C6 C7 120.28(13) . . ?
C5 C6 H3 119.9 . . ?
C7 C6 H3 119.9 . . ?
C8 C7 C6 119.32(13) . . ?
C8 C7 H4 120.3 . . ?
C6 C7 H4 120.3 . . ?
C7 C8 C3 120.43(12) . . ?
C7 C8 C9 132.96(13) . . ?
C3 C8 C9 106.58(11) . . ?
C10 C9 C8 139.53(12) . . ?
C10 C9 C1 113.99(12) . . ?
C8 C9 C1 106.42(11) . . ?
C9 C10 C11 139.00(12) . . ?
C9 C10 C18 114.45(12) . . ?
C11 C10 C18 106.53(11) . . ?
C12 C11 C16 120.97(13) . . ?
C12 C11 C10 132.38(13) . . ?
C16 C11 C10 106.50(11) . . ?
C11 C12 C13 118.99(13) . . ?
C11 C12 H5 120.5 . . ?
C13 C12 H5 120.5 . . ?
C14 C13 C12 120.03(13) . . ?
C14 C13 H6 120.0 . . ?
C12 C13 H6 120.0 . . ?
C13 C14 C15 121.57(13) . . ?
C13 C14 H7 119.2 . . ?
C15 C14 H7 119.2 . . ?
C16 C15 C14 118.92(13) . . ?
C16 C15 H8 120.5 . . ?
C14 C15 H8 120.5 . . ?
C15 C16 C11 119.52(13) . . ?
C15 C16 C17 130.10(13) . . ?
C11 C16 C17 110.30(12) . . ?
C18 C17 C16 105.50(11) . . ?
C18 C17 Si2 128.74(10) . . ?
C16 C17 Si2 125.70(10) . . ?
C17 C18 C10 111.11(12) . . ?
C17 C18 P1 139.01(11) . . ?
C10 C18 P1 109.79(9) . . ?
C24 C19 C20 119.88(13) . . ?
C24 C19 P1 119.59(11) . . ?
C20 C19 P1 120.52(10) . . ?
C21 C20 C19 120.02(13) . . ?
C21 C20 H9 120.0 . . ?
C19 C20 H9 120.0 . . ?
C20 C21 C22 119.88(14) . . ?
C20 C21 H10 120.1 . . ?
C22 C21 H10 120.1 . . ?
C23 C22 C21 120.17(14) . . ?
C23 C22 H11 119.9 . . ?
C21 C22 H11 119.9 . . ?
C24 C23 C22 120.24(14) . . ?
C24 C23 H12 119.9 . . ?
C22 C23 H12 119.9 . . ?
C23 C24 C19 119.81(14) . . ?
C23 C24 H13 120.1 . . ?
C19 C24 H13 120.1 . . ?
Si1 C25 H14 109.5 . . ?
Si1 C25 H15 109.5 . . ?
H14 C25 H15 109.5 . . ?
Si1 C25 H16 109.5 . . ?
H14 C25 H16 109.5 . . ?
H15 C25 H16 109.5 . . ?
Si1 C26 H17 109.5 . . ?
Si1 C26 H18 109.5 . . ?
H17 C26 H18 109.5 . . ?
Si1 C26 H19 109.5 . . ?
H17 C26 H19 109.5 . . ?
H18 C26 H19 109.5 . . ?
C28 C27 C30 108.80(13) . . ?
C28 C27 C29 108.45(13) . . ?
C30 C27 C29 108.69(12) . . ?
C28 C27 Si1 110.42(10) . . ?
C30 C27 Si1 110.22(10) . . ?
C29 C27 Si1 110.21(10) . . ?
C27 C28 H20 109.5 . . ?
C27 C28 H21 109.5 . . ?
H20 C28 H21 109.5 . . ?
C27 C28 H22 109.5 . . ?
H20 C28 H22 109.5 . . ?
H21 C28 H22 109.5 . . ?
C27 C29 H23 109.5 . . ?
C27 C29 H24 109.5 . . ?
H23 C29 H24 109.5 . . ?
C27 C29 H25 109.5 . . ?
H23 C29 H25 109.5 . . ?
H24 C29 H25 109.5 . . ?
C27 C30 H26 109.5 . . ?
C27 C30 H27 109.5 . . ?
H26 C30 H27 109.5 . . ?
C27 C30 H28 109.5 . . ?
H26 C30 H28 109.5 . . ?
H27 C30 H28 109.5 . . ?
Si2 C31 H29 109.5 . . ?
Si2 C31 H30 109.5 . . ?
H29 C31 H30 109.5 . . ?
Si2 C31 H31 109.5 . . ?
H29 C31 H31 109.5 . . ?
H30 C31 H31 109.5 . . ?
Si2 C32 H32 109.5 . . ?
Si2 C32 H33 109.5 . . ?
H32 C32 H33 109.5 . . ?
Si2 C32 H34 109.5 . . ?
H32 C32 H34 109.5 . . ?
H33 C32 H34 109.5 . . ?
C36 C33 C35 108.63(13) . . ?
C36 C33 C34 108.72(13) . . ?
C35 C33 C34 108.46(13) . . ?
C36 C33 Si2 109.23(11) . . ?
C35 C33 Si2 111.38(10) . . ?
C34 C33 Si2 110.36(10) . . ?
C33 C34 H35 109.5 . . ?
C33 C34 H36 109.5 . . ?
H35 C34 H36 109.5 . . ?
C33 C34 H37 109.5 . . ?
H35 C34 H37 109.5 . . ?
H36 C34 H37 109.5 . . ?
C33 C35 H38 109.5 . . ?
C33 C35 H39 109.5 . . ?
H38 C35 H39 109.5 . . ?
C33 C35 H40 109.5 . . ?
H38 C35 H40 109.5 . . ?
H39 C35 H40 109.5 . . ?
C33 C36 H41 109.5 . . ?
C33 C36 H42 109.5 . . ?
H41 C36 H42 109.5 . . ?
C33 C36 H43 109.5 . . ?
H41 C36 H43 109.5 . . ?
H42 C36 H43 109.5 . . ?
O1 P1 C1 118.91(6) . . ?
O1 P1 C19 112.85(6) . . ?
C1 P1 C19 106.12(6) . . ?
O1 P1 C18 117.77(6) . . ?
C1 P1 C18 91.28(6) . . ?
C19 P1 C18 107.44(6) . . ?
C26 Si1 C25 108.48(7) . . ?
C26 Si1 C2 109.96(6) . . ?
C25 Si1 C2 110.64(7) . . ?
C26 Si1 C27 110.76(7) . . ?
C25 Si1 C27 110.03(7) . . ?
C2 Si1 C27 106.98(6) . . ?
C31 Si2 C32 106.33(7) . . ?
C31 Si2 C17 110.61(7) . . ?
C32 Si2 C17 110.93(7) . . ?
C31 Si2 C33 110.10(7) . . ?
C32 Si2 C33 110.72(7) . . ?
C17 Si2 C33 108.17(6) . . ?

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
C9 C1 C2 C3 2.17(16) . . . . ?
P1 C1 C2 C3 -179.32(13) . . . . ?
C9 C1 C2 Si1 -173.86(10) . . . . ?
P1 C1 C2 Si1 4.7(2) . . . . ?
C1 C2 C3 C4 177.01(15) . . . . ?
Si1 C2 C3 C4 -6.9(2) . . . . ?
C1 C2 C3 C8 -1.18(16) . . . . ?
Si1 C2 C3 C8 174.88(10) . . . . ?
C8 C3 C4 C5 -0.1(2) . . . . ?
C2 C3 C4 C5 -178.13(14) . . . . ?
C3 C4 C5 C6 -0.1(2) . . . . ?
C4 C5 C6 C7 0.7(2) . . . . ?
C5 C6 C7 C8 -1.2(2) . . . . ?
C6 C7 C8 C3 1.1(2) . . . . ?
C6 C7 C8 C9 178.81(15) . . . . ?
C4 C3 C8 C7 -0.4(2) . . . . ?
C2 C3 C8 C7 177.99(13) . . . . ?
C4 C3 C8 C9 -178.69(13) . . . . ?
C2 C3 C8 C9 -0.28(15) . . . . ?
C7 C8 C9 C10 6.9(3) . . . . ?
C3 C8 C9 C10 -175.17(17) . . . . ?
C7 C8 C9 C1 -176.43(15) . . . . ?
C3 C8 C9 C1 1.53(15) . . . . ?
C2 C1 C9 C10 175.26(12) . . . . ?
P1 C1 C9 C10 -3.69(15) . . . . ?
C2 C1 C9 C8 -2.40(16) . . . . ?
P1 C1 C9 C8 178.66(9) . . . . ?
C8 C9 C10 C11 3.5(3) . . . . ?
C1 C9 C10 C11 -173.06(16) . . . . ?
C8 C9 C10 C18 -178.49(16) . . . . ?
C1 C9 C10 C18 4.98(17) . . . . ?
C9 C10 C11 C12 4.0(3) . . . . ?
C18 C10 C11 C12 -174.11(15) . . . . ?
C9 C10 C11 C16 179.47(17) . . . . ?
C18 C10 C11 C16 1.33(15) . . . . ?
C16 C11 C12 C13 0.6(2) . . . . ?
C10 C11 C12 C13 175.45(14) . . . . ?
C11 C12 C13 C14 -0.2(2) . . . . ?
C12 C13 C14 C15 0.2(2) . . . . ?
C13 C14 C15 C16 -0.4(2) . . . . ?
C14 C15 C16 C11 0.7(2) . . . . ?
C14 C15 C16 C17 -175.64(14) . . . . ?
C12 C11 C16 C15 -0.8(2) . . . . ?
C10 C11 C16 C15 -176.85(13) . . . . ?
C12 C11 C16 C17 176.22(13) . . . . ?
C10 C11 C16 C17 0.14(15) . . . . ?
C15 C16 C17 C18 174.91(15) . . . . ?
C11 C16 C17 C18 -1.67(16) . . . . ?
C15 C16 C17 Si2 -7.6(2) . . . . ?
C11 C16 C17 Si2 175.84(10) . . . . ?
C16 C17 C18 C10 2.52(15) . . . . ?
Si2 C17 C18 C10 -174.89(10) . . . . ?
C16 C17 C18 P1 -173.45(13) . . . . ?
Si2 C17 C18 P1 9.1(2) . . . . ?
C9 C10 C18 C17 178.84(12) . . . . ?
C11 C10 C18 C17 -2.51(16) . . . . ?
C9 C10 C18 P1 -3.97(15) . . . . ?
C11 C10 C18 P1 174.69(9) . . . . ?
C24 C19 C20 C21 -1.0(2) . . . . ?
P1 C19 C20 C21 177.50(11) . . . . ?
C19 C20 C21 C22 0.2(2) . . . . ?
C20 C21 C22 C23 0.2(2) . . . . ?
C21 C22 C23 C24 0.2(2) . . . . ?
C22 C23 C24 C19 -0.9(2) . . . . ?
C20 C19 C24 C23 1.3(2) . . . . ?
P1 C19 C24 C23 -177.14(10) . . . . ?
C2 C1 P1 O1 -54.41(18) . . . . ?
C9 C1 P1 O1 124.11(10) . . . . ?
C2 C1 P1 C19 74.01(17) . . . . ?
C9 C1 P1 C19 -107.47(10) . . . . ?
C2 C1 P1 C18 -177.42(17) . . . . ?
C9 C1 P1 C18 1.11(10) . . . . ?
C24 C19 P1 O1 -11.05(13) . . . . ?
C20 C19 P1 O1 170.49(10) . . . . ?
C24 C19 P1 C1 -142.95(11) . . . . ?
C20 C19 P1 C1 38.59(12) . . . . ?
C24 C19 P1 C18 120.44(11) . . . . ?
C20 C19 P1 C18 -58.02(12) . . . . ?
C17 C18 P1 O1 53.53(18) . . . . ?
C10 C18 P1 O1 -122.48(10) . . . . ?
C17 C18 P1 C1 177.46(17) . . . . ?
C10 C18 P1 C1 1.46(10) . . . . ?
C17 C18 P1 C19 -75.19(17) . . . . ?
C10 C18 P1 C19 108.80(10) . . . . ?
C1 C2 Si1 C26 -26.71(15) . . . . ?
C3 C2 Si1 C26 158.06(12) . . . . ?
C1 C2 Si1 C25 -146.52(13) . . . . ?
C3 C2 Si1 C25 38.25(14) . . . . ?
C1 C2 Si1 C27 93.64(13) . . . . ?
C3 C2 Si1 C27 -81.59(13) . . . . ?
C18 C17 Si2 C31 -22.77(15) . . . . ?
C16 C17 Si2 C31 160.30(12) . . . . ?
C18 C17 Si2 C32 -140.51(13) . . . . ?
C16 C17 Si2 C32 42.57(14) . . . . ?
C18 C17 Si2 C33 97.88(14) . . . . ?
C16 C17 Si2 C33 -79.05(13) . . . . ?

_refine_diff_density_max         0.408
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.060


_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_diffrn_radiation_source         ?
_diffrn_radiation_monochromator  Confocal
_chemical_absolute_configuration ?
