# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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_yt14
_database_code_depnum_ccdc_archive 'CCDC 2403405'
loop_
_audit_author_name
_audit_author_address
'Hisako Hashimoto'
;Tohoku University
Japan
;
_audit_update_record             
;
2024-11-18 deposited with the CCDC.	2024-12-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H36 O3 Si2 W, 0.5(C12 H18)'
_chemical_formula_sum            'C26 H45 O3 Si2 W'
_chemical_formula_weight         645.65

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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                   8.6680(8)
_cell_length_b                   9.9938(5)
_cell_length_c                   17.0474(15)
_cell_angle_alpha                94.187(3)
_cell_angle_beta                 100.584(4)
_cell_angle_gamma                102.745(3)
_cell_volume                     1405.90(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8076
_cell_measurement_theta_min      2.98
_cell_measurement_theta_max      27.38

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_F_000             654
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    4.217
_shelx_estimated_absorpt_T_min   0.632
_shelx_estimated_absorpt_T_max   0.786
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6316
_exptl_absorpt_correction_T_max  0.7860
_exptl_absorpt_process_details   'NUMABS (Higashi, 1999),ABSCOR (Higashi, 1995)'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotation-anode X-ray tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.00
_diffrn_reflns_number            12190
_diffrn_reflns_av_unetI/netI     0.0956
_diffrn_reflns_av_R_equivalents  0.0976
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.306
_diffrn_reflns_theta_max         27.417
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measured_fraction_theta_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_point_group_measured_fraction_full 0.957

_reflns_number_total             6046
_reflns_number_gt                5141
_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       PROCESS-AUTO
_computing_cell_refinement       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver.1.11'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  
;
'SHELXL-97 (Sheldrick, 1997)', 'SHELXL-2018/3 (Sheldrick, 2018)'
;
_computing_molecular_graphics    'Yadokari-XG2009(Wakita, Nemoto et al.,2009)'
_computing_publication_material  'Yadokari-XG2009(Wakita, Nemoto et al.,2009)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0392P)²+22.2410P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6046
_refine_ls_number_parameters     304
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0713
_refine_ls_wR_factor_ref         0.1551
_refine_ls_wR_factor_gt          0.1480
_refine_ls_goodness_of_fit_ref   1.212
_refine_ls_restrained_S_all      1.212
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         2.297
_refine_diff_density_min         -3.192
_refine_diff_density_rms         0.259

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
W1 W 0.04267(5) 0.19953(4) 0.30601(3) 0.01583(13) Uani 1 1 d . . . . .
Si1 Si 0.1699(3) 0.1374(3) 0.19198(19) 0.0218(6) Uani 1 1 d . . . . .
Si2 Si 0.3050(3) 0.3639(3) 0.29587(18) 0.0199(6) Uani 1 1 d . . . . .
C1 C -0.0350(12) 0.3660(11) 0.2945(7) 0.022(2) Uani 1 1 d . . . . .
O1 O -0.0995(10) 0.4595(9) 0.2906(6) 0.040(2) Uani 1 1 d . . . . .
C2 C -0.1233(12) 0.1414(11) 0.2090(7) 0.023(2) Uani 1 1 d . . . . .
O2 O -0.2334(9) 0.1015(10) 0.1538(5) 0.039(2) Uani 1 1 d . . . . .
C3 C 0.1490(12) 0.0667(11) 0.4037(7) 0.021(2) Uani 1 1 d . . . . .
C4 C -0.0099(12) -0.0124(10) 0.3596(6) 0.019(2) Uani 1 1 d . . . . .
C5 C -0.1251(12) 0.0630(11) 0.3772(7) 0.022(2) Uani 1 1 d . . . . .
C6 C -0.0435(13) 0.1839(11) 0.4296(6) 0.022(2) Uani 1 1 d . . . . .
C7 C 0.1232(13) 0.1872(11) 0.4474(7) 0.023(2) Uani 1 1 d . . . . .
C8 C 0.2978(13) 0.0143(12) 0.4162(8) 0.030(3) Uani 1 1 d . . . . .
H8 H 0.382045 0.077932 0.456711 0.045 Uiso 1 1 calc R U . . .
H8A H 0.335009 0.007544 0.365471 0.045 Uiso 1 1 calc R U . . .
H8B H 0.274642 -0.077203 0.434697 0.045 Uiso 1 1 calc R U . . .
C9 C -0.0479(14) -0.1510(12) 0.3127(8) 0.031(3) Uani 1 1 d . . . . .
H9 H -0.063808 -0.222455 0.348783 0.046 Uiso 1 1 calc R U . . .
H9A H 0.041801 -0.159354 0.286547 0.046 Uiso 1 1 calc R U . . .
H9B H -0.146780 -0.162518 0.271690 0.046 Uiso 1 1 calc R U . . .
C10 C -0.3077(13) 0.0143(12) 0.3489(8) 0.030(3) Uani 1 1 d . . . . .
H10 H -0.356211 0.094019 0.350352 0.046 Uiso 1 1 calc R U . . .
H10A H -0.351454 -0.050355 0.384441 0.046 Uiso 1 1 calc R U . . .
H10B H -0.333067 -0.032096 0.293875 0.046 Uiso 1 1 calc R U . . .
C11 C -0.1177(14) 0.2865(12) 0.4677(7) 0.028(2) Uani 1 1 d . . . . .
H11 H -0.227497 0.278224 0.437163 0.041 Uiso 1 1 calc R U . . .
H11A H -0.052392 0.380024 0.467734 0.041 Uiso 1 1 calc R U . . .
H11B H -0.121858 0.268538 0.523099 0.041 Uiso 1 1 calc R U . . .
C12 C 0.2484(14) 0.2839(13) 0.5085(7) 0.032(3) Uani 1 1 d . . . . .
H12 H 0.231495 0.377475 0.506451 0.048 Uiso 1 1 calc R U . . .
H12A H 0.355388 0.282611 0.497774 0.048 Uiso 1 1 calc R U . . .
H12B H 0.241717 0.255996 0.561944 0.048 Uiso 1 1 calc R U . . .
C13 C 0.2429(16) -0.0268(12) 0.1853(8) 0.037(3) Uani 1 1 d . . . . .
H13 H 0.312464 -0.022902 0.145822 0.056 Uiso 1 1 calc R U . . .
H13A H 0.149883 -0.106142 0.168656 0.056 Uiso 1 1 calc R U . . .
H13B H 0.304376 -0.036694 0.238001 0.056 Uiso 1 1 calc R U . . .
C14 C 0.0894(15) 0.1585(14) 0.0845(7) 0.036(3) Uani 1 1 d . . . . .
H14 H 0.071257 0.251560 0.081516 0.054 Uiso 1 1 calc R U . . .
H14A H -0.012857 0.089880 0.064168 0.054 Uiso 1 1 calc R U . . .
H14B H 0.167889 0.145107 0.051767 0.054 Uiso 1 1 calc R U . . .
C15 C 0.3299(13) 0.5475(11) 0.2650(7) 0.026(2) Uani 1 1 d . . . . .
C16 C 0.4915(13) 0.3773(12) 0.3754(7) 0.028(2) Uani 1 1 d . . . . .
H16 H 0.489163 0.287403 0.395149 0.042 Uiso 1 1 calc R U . . .
H16A H 0.494821 0.446215 0.420034 0.042 Uiso 1 1 calc R U . . .
H16B H 0.587741 0.405409 0.352418 0.042 Uiso 1 1 calc R U . . .
C17 C 0.2938(16) 0.6387(12) 0.3336(8) 0.036(3) Uani 1 1 d . . . . .
H17 H 0.310350 0.734426 0.321109 0.055 Uiso 1 1 calc R U . . .
H17A H 0.366741 0.634914 0.384166 0.055 Uiso 1 1 calc R U . . .
H17B H 0.181598 0.604608 0.338776 0.055 Uiso 1 1 calc R U . . .
C18 C 0.5021(14) 0.6132(13) 0.2539(9) 0.038(3) Uani 1 1 d . . . . .
H18 H 0.514045 0.581328 0.200056 0.057 Uiso 1 1 calc R U . . .
H18A H 0.581391 0.585823 0.294372 0.057 Uiso 1 1 calc R U . . .
H18B H 0.520000 0.714002 0.260112 0.057 Uiso 1 1 calc R U . . .
C19 C 0.2093(15) 0.5480(13) 0.1870(8) 0.036(3) Uani 1 1 d . . . . .
H19 H 0.223767 0.642239 0.172107 0.054 Uiso 1 1 calc R U . . .
H19A H 0.098793 0.515148 0.195064 0.054 Uiso 1 1 calc R U . . .
H19B H 0.228203 0.487102 0.143871 0.054 Uiso 1 1 calc R U . . .
O3 O 0.3536(8) 0.2682(7) 0.2143(5) 0.0244(17) Uani 1 1 d . . . . .
C20 C 0.4930(15) 0.2843(16) 0.1747(8) 0.042(3) Uani 1 1 d . . . . .
H20 H 0.497135 0.193826 0.149975 0.064 Uiso 1 1 calc R U . . .
H20A H 0.592827 0.323311 0.214676 0.064 Uiso 1 1 calc R U . . .
H20B H 0.481741 0.346318 0.133229 0.064 Uiso 1 1 calc R U . . .
C21 C 0.5064(14) 0.6389(13) 0.0279(7) 0.032(3) Uani 1 1 d . . . . .
C22 C 0.6437(14) 0.5844(13) 0.0462(7) 0.032(3) Uani 1 1 d . . . . .
C23 C 0.6382(15) 0.4491(14) 0.0188(7) 0.033(3) Uani 1 1 d . . . . .
C24 C 0.513(2) 0.7855(15) 0.0558(10) 0.053(4) Uani 1 1 d . . . . .
H24 H 0.470896 0.789466 0.105217 0.079 Uiso 1 1 calc R U . . .
H24A H 0.447278 0.823589 0.014124 0.079 Uiso 1 1 calc R U . . .
H24B H 0.625219 0.839577 0.066244 0.079 Uiso 1 1 calc R U . . .
C25 C 0.7988(17) 0.6729(17) 0.0986(9) 0.050(4) Uani 1 1 d . . . . .
H25 H 0.772678 0.729255 0.141492 0.076 Uiso 1 1 calc R U . . .
H25A H 0.858070 0.733418 0.065772 0.076 Uiso 1 1 calc R U . . .
H25B H 0.865871 0.613130 0.122347 0.076 Uiso 1 1 calc R U . . .
C26 C 0.7899(17) 0.3923(19) 0.0372(10) 0.056(4) Uani 1 1 d . . . . .
H26 H 0.885492 0.465242 0.035941 0.084 Uiso 1 1 calc R U . . .
H26A H 0.781182 0.314556 -0.003171 0.084 Uiso 1 1 calc R U . . .
H26B H 0.800052 0.360863 0.090643 0.084 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
W1 C1 1.937(11) . ?
W1 C2 1.939(11) . ?
W1 C5 2.337(10) . ?
W1 C4 2.353(10) . ?
W1 C6 2.367(11) . ?
W1 C3 2.384(10) . ?
W1 C7 2.404(11) . ?
W1 Si1 2.509(3) . ?
W1 Si2 2.537(3) . ?
Si1 O3 1.782(7) . ?
Si1 C14 1.882(13) . ?
Si1 C13 1.888(12) . ?
Si1 Si2 2.668(4) . ?
Si2 O3 1.795(8) . ?
Si2 C16 1.882(11) . ?
Si2 C15 1.922(12) . ?
C1 O1 1.190(14) . ?
C2 O2 1.185(13) . ?
C3 C7 1.451(15) . ?
C3 C4 1.463(14) . ?
C3 C8 1.481(15) . ?
C4 C5 1.436(15) . ?
C4 C9 1.486(15) . ?
C5 C6 1.411(14) . ?
C5 C10 1.524(15) . ?
C6 C7 1.414(15) . ?
C6 C11 1.494(15) . ?
C7 C12 1.473(15) . ?
C15 C19 1.535(16) . ?
C15 C18 1.544(16) . ?
C15 C17 1.549(16) . ?
O3 C20 1.474(13) . ?
C21 C22 1.409(18) . ?
C21 C23 1.422(17) 2_665 ?
C21 C24 1.491(18) . ?
C22 C23 1.386(18) . ?
C22 C25 1.519(17) . ?
C23 C26 1.535(17) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 W1 C2 79.2(4) . . ?
C1 W1 C5 106.3(4) . . ?
C2 W1 C5 89.7(4) . . ?
C1 W1 C4 141.9(4) . . ?
C2 W1 C4 95.9(4) . . ?
C5 W1 C4 35.7(4) . . ?
C1 W1 C6 89.3(4) . . ?
C2 W1 C6 116.7(4) . . ?
C5 W1 C6 34.9(4) . . ?
C4 W1 C6 59.0(4) . . ?
C1 W1 C3 142.7(4) . . ?
C2 W1 C3 130.2(4) . . ?
C5 W1 C3 59.0(4) . . ?
C4 W1 C3 36.0(3) . . ?
C6 W1 C3 58.6(4) . . ?
C1 W1 C7 107.4(4) . . ?
C2 W1 C7 147.6(4) . . ?
C5 W1 C7 57.9(4) . . ?
C4 W1 C7 58.9(4) . . ?
C6 W1 C7 34.5(4) . . ?
C3 W1 C7 35.3(4) . . ?
C1 W1 Si1 112.6(3) . . ?
C2 W1 Si1 70.8(3) . . ?
C5 W1 Si1 131.5(3) . . ?
C4 W1 Si1 100.9(3) . . ?
C6 W1 Si1 158.1(3) . . ?
C3 W1 Si1 100.3(3) . . ?
C7 W1 Si1 129.8(3) . . ?
C1 W1 Si2 81.2(3) . . ?
C2 W1 Si2 117.8(3) . . ?
C5 W1 Si2 152.5(3) . . ?
C4 W1 Si2 131.8(3) . . ?
C6 W1 Si2 121.4(3) . . ?
C3 W1 Si2 98.8(2) . . ?
C7 W1 Si2 94.7(3) . . ?
Si1 W1 Si2 63.83(9) . . ?
O3 Si1 C14 101.2(5) . . ?
O3 Si1 C13 102.7(5) . . ?
C14 Si1 C13 104.4(6) . . ?
O3 Si1 W1 100.3(3) . . ?
C14 Si1 W1 123.2(4) . . ?
C13 Si1 W1 120.9(4) . . ?
O3 Si1 Si2 42.0(3) . . ?
C14 Si1 Si2 118.5(4) . . ?
C13 Si1 Si2 126.8(5) . . ?
W1 Si1 Si2 58.60(9) . . ?
O3 Si2 C16 100.0(5) . . ?
O3 Si2 C15 103.6(5) . . ?
C16 Si2 C15 103.7(5) . . ?
O3 Si2 W1 98.9(2) . . ?
C16 Si2 W1 119.2(4) . . ?
C15 Si2 W1 126.6(3) . . ?
O3 Si2 Si1 41.6(2) . . ?
C16 Si2 Si1 122.5(4) . . ?
C15 Si2 Si1 122.9(4) . . ?
W1 Si2 Si1 57.57(9) . . ?
O1 C1 W1 171.7(9) . . ?
O2 C2 W1 174.4(10) . . ?
C7 C3 C4 106.7(9) . . ?
C7 C3 C8 126.8(10) . . ?
C4 C3 C8 125.0(10) . . ?
C7 C3 W1 73.1(6) . . ?
C4 C3 W1 70.9(6) . . ?
C8 C3 W1 132.3(8) . . ?
C5 C4 C3 106.8(9) . . ?
C5 C4 C9 126.2(9) . . ?
C3 C4 C9 126.8(10) . . ?
C5 C4 W1 71.6(6) . . ?
C3 C4 W1 73.2(6) . . ?
C9 C4 W1 125.2(8) . . ?
C6 C5 C4 109.3(9) . . ?
C6 C5 C10 125.3(10) . . ?
C4 C5 C10 125.2(9) . . ?
C6 C5 W1 73.7(6) . . ?
C4 C5 W1 72.8(5) . . ?
C10 C5 W1 123.6(8) . . ?
C5 C6 C7 108.6(9) . . ?
C5 C6 C11 127.1(10) . . ?
C7 C6 C11 124.0(10) . . ?
C5 C6 W1 71.4(6) . . ?
C7 C6 W1 74.2(6) . . ?
C11 C6 W1 124.9(8) . . ?
C6 C7 C3 108.6(9) . . ?
C6 C7 C12 126.5(10) . . ?
C3 C7 C12 124.4(10) . . ?
C6 C7 W1 71.3(6) . . ?
C3 C7 W1 71.6(6) . . ?
C12 C7 W1 129.6(8) . . ?
C19 C15 C18 108.8(10) . . ?
C19 C15 C17 109.1(10) . . ?
C18 C15 C17 107.5(10) . . ?
C19 C15 Si2 110.6(8) . . ?
C18 C15 Si2 113.7(8) . . ?
C17 C15 Si2 107.1(8) . . ?
C20 O3 Si1 128.8(7) . . ?
C20 O3 Si2 134.8(7) . . ?
Si1 O3 Si2 96.4(4) . . ?
C22 C21 C23 118.2(12) . 2_665 ?
C22 C21 C24 120.9(12) . . ?
C23 C21 C24 120.9(12) 2_665 . ?
C23 C22 C21 120.8(11) . . ?
C23 C22 C25 119.2(12) . . ?
C21 C22 C25 120.0(12) . . ?
C22 C23 C21 121.0(12) . 2_665 ?
C22 C23 C26 120.3(12) . . ?
C21 C23 C26 118.7(13) 2_665 . ?

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
C7 C3 C4 C5 0.7(11) . . . . ?
C8 C3 C4 C5 167.1(10) . . . . ?
W1 C3 C4 C5 -64.1(7) . . . . ?
C7 C3 C4 C9 -173.5(10) . . . . ?
C8 C3 C4 C9 -7.1(18) . . . . ?
W1 C3 C4 C9 121.7(11) . . . . ?
C7 C3 C4 W1 64.8(7) . . . . ?
C8 C3 C4 W1 -128.8(11) . . . . ?
C3 C4 C5 C6 0.1(12) . . . . ?
C9 C4 C5 C6 174.3(11) . . . . ?
W1 C4 C5 C6 -65.1(8) . . . . ?
C3 C4 C5 C10 -175.5(10) . . . . ?
C9 C4 C5 C10 -1.3(18) . . . . ?
W1 C4 C5 C10 119.3(11) . . . . ?
C3 C4 C5 W1 65.2(7) . . . . ?
C9 C4 C5 W1 -120.6(11) . . . . ?
C4 C5 C6 C7 -0.8(13) . . . . ?
C10 C5 C6 C7 174.7(10) . . . . ?
W1 C5 C6 C7 -65.4(8) . . . . ?
C4 C5 C6 C11 -175.3(10) . . . . ?
C10 C5 C6 C11 0.2(18) . . . . ?
W1 C5 C6 C11 120.1(11) . . . . ?
C4 C5 C6 W1 64.6(7) . . . . ?
C10 C5 C6 W1 -119.9(11) . . . . ?
C5 C6 C7 C3 1.3(12) . . . . ?
C11 C6 C7 C3 176.0(10) . . . . ?
W1 C6 C7 C3 -62.3(8) . . . . ?
C5 C6 C7 C12 -170.5(11) . . . . ?
C11 C6 C7 C12 4.2(18) . . . . ?
W1 C6 C7 C12 125.9(12) . . . . ?
C5 C6 C7 W1 63.6(8) . . . . ?
C11 C6 C7 W1 -121.7(11) . . . . ?
C4 C3 C7 C6 -1.2(12) . . . . ?
C8 C3 C7 C6 -167.3(11) . . . . ?
W1 C3 C7 C6 62.1(8) . . . . ?
C4 C3 C7 C12 170.8(10) . . . . ?
C8 C3 C7 C12 4.7(18) . . . . ?
W1 C3 C7 C12 -125.9(11) . . . . ?
C4 C3 C7 W1 -63.3(7) . . . . ?
C8 C3 C7 W1 130.6(11) . . . . ?
C14 Si1 O3 C20 -59.2(12) . . . . ?
C13 Si1 O3 C20 48.5(12) . . . . ?
W1 Si1 O3 C20 173.7(10) . . . . ?
Si2 Si1 O3 C20 -179.6(13) . . . . ?
C14 Si1 O3 Si2 120.4(5) . . . . ?
C13 Si1 O3 Si2 -131.9(5) . . . . ?
W1 Si1 O3 Si2 -6.7(4) . . . . ?
C16 Si2 O3 C20 -51.9(13) . . . . ?
C15 Si2 O3 C20 54.9(12) . . . . ?
W1 Si2 O3 C20 -173.9(11) . . . . ?
Si1 Si2 O3 C20 179.6(14) . . . . ?
C16 Si2 O3 Si1 128.5(5) . . . . ?
C15 Si2 O3 Si1 -124.7(4) . . . . ?
W1 Si2 O3 Si1 6.6(4) . . . . ?
C23 C21 C22 C23 0.5(19) 2_665 . . . ?
C24 C21 C22 C23 -178.7(12) . . . . ?
C23 C21 C22 C25 -177.6(11) 2_665 . . . ?
C24 C21 C22 C25 3.2(18) . . . . ?
C21 C22 C23 C21 -1(2) . . . 2_665 ?
C25 C22 C23 C21 177.6(11) . . . 2_665 ?
C21 C22 C23 C26 178.3(12) . . . . ?
C25 C22 C23 C26 -3.6(18) . . . . ?


_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# 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_mstuo04
_database_code_depnum_ccdc_archive 'CCDC 2403408'
loop_
_audit_author_name
_audit_author_address
'Hisako Hashimoto'
;Tohoku University
Japan
;
_audit_update_record             
;
2024-11-18 deposited with the CCDC.	2024-12-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H38 O3 Si2 W, C7 H8'
_chemical_formula_sum            'C30 H46 O3 Si2 W'
_chemical_formula_weight         694.70

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'
W W -0.8490 6.8722 '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                   13.6063(3)
_cell_length_b                   16.0363(4)
_cell_length_c                   14.7843(3)
_cell_angle_alpha                90
_cell_angle_beta                 104.0881(6)
_cell_angle_gamma                90
_cell_volume                     3128.83(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    140(2)
_cell_measurement_reflns_used    18529
_cell_measurement_theta_min      1.42
_cell_measurement_theta_max      27.47

_exptl_crystal_description       block
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_F_000             1408
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_exptl_absorpt_coefficient_mu    3.796
_shelx_estimated_absorpt_T_min   0.476
_shelx_estimated_absorpt_T_max   0.532
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.4756
_exptl_absorpt_correction_T_max  0.5324
_exptl_absorpt_process_details   'NUMABS (Higashi, 1999)'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      140(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating-anode X-ray tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.00
_diffrn_reflns_number            28817
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.905
_diffrn_reflns_theta_max         27.474
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_point_group_measured_fraction_full 0.987

_reflns_number_total             6990
_reflns_number_gt                6228
_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       PROCESS-AUTO
_computing_cell_refinement       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver.1.11'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  
;
'SHELXL-97 (Sheldrick, 1997)', 'SHELXL-2018/3 (Sheldrick, 2018)'
;
_computing_molecular_graphics    'Yadokari-XG2009(Wakita, Nemoto et al.,2009)'
_computing_publication_material  'Yadokari-XG2009(Wakita, Nemoto et al.,2009)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0217P)²+12.6164P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6990
_refine_ls_number_parameters     308
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0376
_refine_ls_wR_factor_ref         0.0825
_refine_ls_wR_factor_gt          0.0797
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_restrained_S_all      1.151
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.556
_refine_diff_density_min         -1.085
_refine_diff_density_rms         0.135

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
W1 W 0.22958(2) 0.25739(2) 0.93519(2) 0.01769(6) Uani 1 1 d . . . . .
C1 C 0.2907(4) 0.3605(3) 0.9926(3) 0.0250(9) Uani 1 1 d . . . . .
C2 C 0.3013(4) 0.2157(3) 1.0569(3) 0.0254(9) Uani 1 1 d . . . . .
O1 O 0.3177(3) 0.4230(2) 1.0303(3) 0.0367(8) Uani 1 1 d . . . . .
O2 O 0.3390(3) 0.1926(2) 1.1323(2) 0.0370(9) Uani 1 1 d . . . . .
C3 C 0.0801(3) 0.2225(3) 0.8188(3) 0.0232(9) Uani 1 1 d . . . . .
C4 C 0.0738(3) 0.3090(3) 0.8431(3) 0.0244(9) Uani 1 1 d . . . . .
C5 C 0.0703(3) 0.3126(3) 0.9380(4) 0.0277(10) Uani 1 1 d . . . . .
C6 C 0.0742(4) 0.2303(3) 0.9736(3) 0.0290(10) Uani 1 1 d . . . . .
C7 C 0.0793(3) 0.1739(3) 0.8994(3) 0.0239(9) Uani 1 1 d . . . . .
C8 C 0.0677(4) 0.1884(3) 0.7219(3) 0.0306(10) Uani 1 1 d . . . . .
H1 H 0.072437 0.234084 0.679108 0.046 Uiso 1 1 calc R U . . .
H2 H 0.001292 0.161478 0.701663 0.046 Uiso 1 1 calc R U . . .
H3 H 0.121127 0.147511 0.721798 0.046 Uiso 1 1 calc R U . . .
C9 C 0.0566(4) 0.3814(3) 0.7772(4) 0.0321(11) Uani 1 1 d . . . . .
H4 H 0.095079 0.429666 0.807481 0.048 Uiso 1 1 calc R U . . .
H5 H -0.015736 0.395094 0.759717 0.048 Uiso 1 1 calc R U . . .
H6 H 0.079237 0.366713 0.721141 0.048 Uiso 1 1 calc R U . . .
C10 C 0.0549(4) 0.3900(4) 0.9902(4) 0.0419(13) Uani 1 1 d . . . . .
H7 H -0.017149 0.395969 0.988783 0.063 Uiso 1 1 calc R U . . .
H8 H 0.077552 0.438784 0.960861 0.063 Uiso 1 1 calc R U . . .
H9 H 0.094237 0.385726 1.055060 0.063 Uiso 1 1 calc R U . . .
C11 C 0.0642(4) 0.2051(4) 1.0688(4) 0.0436(14) Uani 1 1 d . . . A 2
H10 H -0.007626 0.197871 1.067672 0.065 Uiso 1 1 calc R U . A 2
H11 H 0.093378 0.248589 1.114004 0.065 Uiso 1 1 calc R U . A 2
H12 H 0.100247 0.152512 1.086923 0.065 Uiso 1 1 calc R U . A 2
C12 C 0.0647(4) 0.0808(3) 0.9013(4) 0.0340(11) Uani 1 1 d . . . . .
H13 H 0.086243 0.055252 0.849052 0.051 Uiso 1 1 calc R U . . .
H14 H -0.007024 0.068336 0.895868 0.051 Uiso 1 1 calc R U . . .
H15 H 0.105370 0.058227 0.960179 0.051 Uiso 1 1 calc R U . . .
Si1 Si 0.34198(9) 0.29782(7) 0.82938(8) 0.0199(2) Uani 1 1 d . . . . .
Si2 Si 0.35000(9) 0.14769(7) 0.90751(8) 0.0203(2) Uani 1 1 d . . . . .
O3 O 0.3948(3) 0.19556(19) 0.8137(2) 0.0247(7) Uani 1 1 d . . . . .
C13 C 0.2816(4) 0.3254(3) 0.7048(3) 0.0321(11) Uani 1 1 d . . . . .
H16 H 0.234290 0.281192 0.676520 0.048 Uiso 1 1 calc R U . . .
H17 H 0.334226 0.331145 0.670215 0.048 Uiso 1 1 calc R U . . .
H18 H 0.244841 0.378169 0.702625 0.048 Uiso 1 1 calc R U . . .
C14 C 0.4616(4) 0.3661(3) 0.8629(3) 0.0262(10) Uani 1 1 d . . . . .
C15 C 0.4278(4) 0.4578(3) 0.8581(4) 0.0323(11) Uani 1 1 d . . . . .
H19 H 0.487690 0.493939 0.872621 0.048 Uiso 1 1 calc R U . . .
H20 H 0.387151 0.467539 0.903417 0.048 Uiso 1 1 calc R U . . .
H21 H 0.387192 0.470307 0.795223 0.048 Uiso 1 1 calc R U . . .
C16 C 0.5314(4) 0.3564(4) 0.7960(4) 0.0402(13) Uani 1 1 d . . . . .
H22 H 0.552594 0.298011 0.795281 0.060 Uiso 1 1 calc R U . . .
H23 H 0.591330 0.391799 0.817091 0.060 Uiso 1 1 calc R U . . .
H24 H 0.494913 0.373105 0.733052 0.060 Uiso 1 1 calc R U . . .
C17 C 0.5260(4) 0.3474(3) 0.9617(4) 0.0348(11) Uani 1 1 d . . . . .
H25 H 0.483855 0.352518 1.006542 0.052 Uiso 1 1 calc R U . . .
H26 H 0.582269 0.387152 0.977710 0.052 Uiso 1 1 calc R U . . .
H27 H 0.552971 0.290553 0.963775 0.052 Uiso 1 1 calc R U . . .
C18 C 0.3012(4) 0.0440(3) 0.8580(3) 0.0278(10) Uani 1 1 d . . . . .
H28 H 0.355757 0.013180 0.840214 0.042 Uiso 1 1 calc R U . . .
H29 H 0.245173 0.052451 0.802850 0.042 Uiso 1 1 calc R U . . .
H30 H 0.277016 0.012243 0.904889 0.042 Uiso 1 1 calc R U . . .
C19 C 0.4706(4) 0.1202(3) 0.9958(4) 0.0317(11) Uani 1 1 d . . . . .
H31 H 0.506236 0.171486 1.020881 0.048 Uiso 1 1 calc R U . . .
H32 H 0.513974 0.086757 0.965842 0.048 Uiso 1 1 calc R U . . .
H33 H 0.454331 0.088170 1.046716 0.048 Uiso 1 1 calc R U . . .
C20 C 0.4345(4) 0.1639(3) 0.7359(4) 0.0289(10) Uani 1 1 d . . . . .
H34 H 0.454(3) 0.217(3) 0.709(3) 0.012(11) Uiso 1 1 d . . . . .
C21 C 0.3554(4) 0.1213(3) 0.6675(3) 0.0296(10) Uani 1 1 d . . . . .
C22 C 0.2977(4) 0.0869(4) 0.6074(4) 0.0395(12) Uani 1 1 d . . . . .
H35 H 0.250899 0.058966 0.558554 0.047 Uiso 1 1 calc R U . . .
C23 C 0.5261(4) 0.1088(4) 0.7718(4) 0.0391(12) Uani 1 1 d . . . . .
H36 H 0.552570 0.089853 0.719243 0.059 Uiso 1 1 calc R U . . .
H37 H 0.506516 0.060436 0.803842 0.059 Uiso 1 1 calc R U . . .
H38 H 0.578636 0.140549 0.815370 0.059 Uiso 1 1 calc R U . . .
C24 C 0.2941(8) 0.3318(6) 0.3690(7) 0.084(3) Uiso 1 1 d . . . . .
C25 C 0.2723(5) 0.3979(4) 0.4289(5) 0.0556(17) Uiso 1 1 d . . . . .
H39 H 0.268207 0.386855 0.490996 0.067 Uiso 1 1 calc R U . . .
C26 C 0.2584(6) 0.4734(5) 0.3936(5) 0.0597(18) Uiso 1 1 d . . . . .
H40 H 0.241888 0.515729 0.432318 0.072 Uiso 1 1 calc R U . . .
C27 C 0.2655(8) 0.4976(7) 0.3037(7) 0.089(3) Uiso 1 1 d . . . . .
H41 H 0.255797 0.553158 0.281119 0.107 Uiso 1 1 calc R U . . .
C28 C 0.2870(8) 0.4353(7) 0.2550(8) 0.097(3) Uiso 1 1 d . . . . .
H42 H 0.294514 0.448833 0.194540 0.117 Uiso 1 1 calc R U . . .
C29 C 0.2993(6) 0.3582(5) 0.2781(6) 0.0638(19) Uiso 1 1 d . . . . .
H43 H 0.311882 0.318538 0.234503 0.077 Uiso 1 1 calc R U . . .
C30 C 0.3037(12) 0.2524(9) 0.4022(12) 0.148(6) Uiso 1 1 d . . . . .
H44 H 0.287849 0.213150 0.349866 0.222 Uiso 1 1 calc R U . . .
H45 H 0.256737 0.243604 0.442166 0.222 Uiso 1 1 calc R U . . .
H46 H 0.373326 0.243223 0.438521 0.222 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
W1 C2 1.945(5) . ?
W1 C1 1.950(5) . ?
W1 C5 2.351(4) . ?
W1 C6 2.358(5) . ?
W1 C4 2.372(5) . ?
W1 C3 2.389(4) . ?
W1 C7 2.393(4) . ?
W1 Si2 2.5047(12) . ?
W1 Si1 2.5241(12) . ?
C1 O1 1.162(6) . ?
C2 O2 1.168(6) . ?
C3 C7 1.428(6) . ?
C3 C4 1.441(6) . ?
C3 C8 1.503(6) . ?
C4 C5 1.416(7) . ?
C4 C9 1.497(6) . ?
C5 C6 1.417(7) . ?
C5 C10 1.503(7) . ?
C6 C7 1.436(7) . ?
C6 C11 1.503(7) . ?
C7 C12 1.507(6) . ?
Si1 O3 1.828(3) . ?
Si1 C13 1.878(5) . ?
Si1 C14 1.923(5) . ?
Si1 Si2 2.6610(17) . ?
Si2 O3 1.816(3) . ?
Si2 C18 1.872(5) . ?
Si2 C19 1.884(5) . ?
O3 C20 1.474(5) . ?
C14 C15 1.537(6) . ?
C14 C16 1.537(7) . ?
C14 C17 1.539(7) . ?
C20 C21 1.456(7) . ?
C20 C23 1.515(7) . ?
C21 C22 1.171(8) . ?
C24 C30 1.359(15) . ?
C24 C29 1.428(12) . ?
C24 C25 1.457(12) . ?
C25 C26 1.313(10) . ?
C26 C27 1.410(12) . ?
C27 C28 1.306(14) . ?
C28 C29 1.282(13) . ?

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 W1 C1 79.9(2) . . ?
C2 W1 C5 111.75(19) . . ?
C1 W1 C5 88.28(18) . . ?
C2 W1 C6 89.51(19) . . ?
C1 W1 C6 111.31(18) . . ?
C5 W1 C6 35.03(17) . . ?
C2 W1 C4 145.91(18) . . ?
C1 W1 C4 100.41(18) . . ?
C5 W1 C4 34.90(17) . . ?
C6 W1 C4 58.29(16) . . ?
C2 W1 C3 137.19(18) . . ?
C1 W1 C3 135.25(18) . . ?
C5 W1 C3 58.28(16) . . ?
C6 W1 C3 58.32(16) . . ?
C4 W1 C3 35.23(15) . . ?
C2 W1 C7 102.78(18) . . ?
C1 W1 C7 145.23(17) . . ?
C5 W1 C7 58.20(16) . . ?
C6 W1 C7 35.17(16) . . ?
C4 W1 C7 58.17(15) . . ?
C3 W1 C7 34.74(15) . . ?
C2 W1 Si2 73.05(14) . . ?
C1 W1 Si2 116.12(14) . . ?
C5 W1 Si2 155.51(12) . . ?
C6 W1 Si2 124.76(13) . . ?
C4 W1 Si2 132.85(12) . . ?
C3 W1 Si2 101.18(11) . . ?
C7 W1 Si2 97.38(12) . . ?
C2 W1 Si1 114.73(14) . . ?
C1 W1 Si1 78.10(14) . . ?
C5 W1 Si1 127.91(13) . . ?
C6 W1 Si1 155.53(13) . . ?
C4 W1 Si1 98.41(12) . . ?
C3 W1 Si1 98.70(11) . . ?
C7 W1 Si1 128.37(12) . . ?
Si2 W1 Si1 63.90(4) . . ?
O1 C1 W1 172.6(4) . . ?
O2 C2 W1 175.4(4) . . ?
C7 C3 C4 107.7(4) . . ?
C7 C3 C8 125.1(4) . . ?
C4 C3 C8 126.1(4) . . ?
C7 C3 W1 72.8(3) . . ?
C4 C3 W1 71.7(3) . . ?
C8 C3 W1 130.6(3) . . ?
C5 C4 C3 107.8(4) . . ?
C5 C4 C9 125.2(4) . . ?
C3 C4 C9 126.3(4) . . ?
C5 C4 W1 71.7(3) . . ?
C3 C4 W1 73.0(3) . . ?
C9 C4 W1 128.4(3) . . ?
C4 C5 C6 108.8(4) . . ?
C4 C5 C10 125.8(5) . . ?
C6 C5 C10 125.2(5) . . ?
C4 C5 W1 73.4(3) . . ?
C6 C5 W1 72.8(3) . . ?
C10 C5 W1 124.4(4) . . ?
C5 C6 C7 107.9(4) . . ?
C5 C6 C11 126.5(5) . . ?
C7 C6 C11 125.3(5) . . ?
C5 C6 W1 72.2(3) . . ?
C7 C6 W1 73.7(3) . . ?
C11 C6 W1 124.5(4) . . ?
C3 C7 C6 107.7(4) . . ?
C3 C7 C12 125.8(4) . . ?
C6 C7 C12 125.4(4) . . ?
C3 C7 W1 72.4(2) . . ?
C6 C7 W1 71.1(3) . . ?
C12 C7 W1 131.3(3) . . ?
O3 Si1 C13 100.3(2) . . ?
O3 Si1 C14 102.08(18) . . ?
C13 Si1 C14 105.0(2) . . ?
O3 Si1 W1 99.48(11) . . ?
C13 Si1 W1 118.82(17) . . ?
C14 Si1 W1 126.06(15) . . ?
O3 Si1 Si2 42.91(10) . . ?
C13 Si1 Si2 126.92(17) . . ?
C14 Si1 Si2 117.42(16) . . ?
W1 Si1 Si2 57.70(4) . . ?
O3 Si2 C18 103.28(19) . . ?
O3 Si2 C19 103.3(2) . . ?
C18 Si2 C19 103.3(2) . . ?
O3 Si2 W1 100.52(11) . . ?
C18 Si2 W1 120.24(16) . . ?
C19 Si2 W1 123.03(17) . . ?
O3 Si2 Si1 43.26(10) . . ?
C18 Si2 Si1 131.33(16) . . ?
C19 Si2 Si1 116.69(17) . . ?
W1 Si2 Si1 58.41(4) . . ?
C20 O3 Si2 134.9(3) . . ?
C20 O3 Si1 129.6(3) . . ?
Si2 O3 Si1 93.83(15) . . ?
C15 C14 C16 107.0(4) . . ?
C15 C14 C17 109.0(4) . . ?
C16 C14 C17 107.0(4) . . ?
C15 C14 Si1 108.0(3) . . ?
C16 C14 Si1 113.2(3) . . ?
C17 C14 Si1 112.6(3) . . ?
C21 C20 O3 110.7(4) . . ?
C21 C20 C23 112.1(4) . . ?
O3 C20 C23 110.7(4) . . ?
C22 C21 C20 173.9(5) . . ?
C30 C24 C29 126.5(11) . . ?
C30 C24 C25 118.6(11) . . ?
C29 C24 C25 114.8(8) . . ?
C26 C25 C24 117.4(8) . . ?
C25 C26 C27 126.3(8) . . ?
C28 C27 C26 112.6(10) . . ?
C29 C28 C27 128.6(12) . . ?
C28 C29 C24 120.2(9) . . ?

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
C7 C3 C4 C5 0.6(5) . . . . ?
C8 C3 C4 C5 168.8(4) . . . . ?
W1 C3 C4 C5 -63.8(3) . . . . ?
C7 C3 C4 C9 -170.1(4) . . . . ?
C8 C3 C4 C9 -1.9(8) . . . . ?
W1 C3 C4 C9 125.5(5) . . . . ?
C7 C3 C4 W1 64.4(3) . . . . ?
C8 C3 C4 W1 -127.4(5) . . . . ?
C3 C4 C5 C6 0.0(5) . . . . ?
C9 C4 C5 C6 170.8(4) . . . . ?
W1 C4 C5 C6 -64.7(3) . . . . ?
C3 C4 C5 C10 -174.7(5) . . . . ?
C9 C4 C5 C10 -3.8(8) . . . . ?
W1 C4 C5 C10 120.7(5) . . . . ?
C3 C4 C5 W1 64.6(3) . . . . ?
C9 C4 C5 W1 -124.5(5) . . . . ?
C4 C5 C6 C7 -0.6(5) . . . . ?
C10 C5 C6 C7 174.1(5) . . . . ?
W1 C5 C6 C7 -65.6(3) . . . . ?
C4 C5 C6 C11 -174.8(5) . . . . ?
C10 C5 C6 C11 -0.2(8) . . . . ?
W1 C5 C6 C11 120.1(5) . . . . ?
C4 C5 C6 W1 65.0(3) . . . . ?
C10 C5 C6 W1 -120.3(5) . . . . ?
C4 C3 C7 C6 -1.0(5) . . . . ?
C8 C3 C7 C6 -169.3(4) . . . . ?
W1 C3 C7 C6 62.7(3) . . . . ?
C4 C3 C7 C12 167.6(4) . . . . ?
C8 C3 C7 C12 -0.7(7) . . . . ?
W1 C3 C7 C12 -128.7(5) . . . . ?
C4 C3 C7 W1 -63.7(3) . . . . ?
C8 C3 C7 W1 127.9(4) . . . . ?
C5 C6 C7 C3 1.0(5) . . . . ?
C11 C6 C7 C3 175.3(5) . . . . ?
W1 C6 C7 C3 -63.6(3) . . . . ?
C5 C6 C7 C12 -167.7(4) . . . . ?
C11 C6 C7 C12 6.6(8) . . . . ?
W1 C6 C7 C12 127.7(5) . . . . ?
C5 C6 C7 W1 64.6(3) . . . . ?
C11 C6 C7 W1 -121.1(5) . . . . ?
C18 Si2 O3 C20 -27.8(5) . . . . ?
C19 Si2 O3 C20 79.6(5) . . . . ?
W1 Si2 O3 C20 -152.6(4) . . . . ?
Si1 Si2 O3 C20 -165.5(5) . . . . ?
C18 Si2 O3 Si1 137.67(19) . . . . ?
C19 Si2 O3 Si1 -114.9(2) . . . . ?
W1 Si2 O3 Si1 12.91(14) . . . . ?
C13 Si1 O3 C20 32.1(4) . . . . ?
C14 Si1 O3 C20 -75.8(4) . . . . ?
W1 Si1 O3 C20 153.9(4) . . . . ?
Si2 Si1 O3 C20 166.7(5) . . . . ?
C13 Si1 O3 Si2 -134.6(2) . . . . ?
C14 Si1 O3 Si2 117.48(19) . . . . ?
W1 Si1 O3 Si2 -12.77(14) . . . . ?
Si2 O3 C20 C21 68.1(6) . . . . ?
Si1 O3 C20 C21 -92.9(5) . . . . ?
Si2 O3 C20 C23 -56.8(6) . . . . ?
Si1 O3 C20 C23 142.1(4) . . . . ?
C30 C24 C25 C26 -176.7(11) . . . . ?
C29 C24 C25 C26 0.9(12) . . . . ?
C24 C25 C26 C27 -2.1(13) . . . . ?
C25 C26 C27 C28 0.9(15) . . . . ?
C26 C27 C28 C29 1.7(18) . . . . ?
C27 C28 C29 C24 -2.8(18) . . . . ?
C30 C24 C29 C28 178.7(13) . . . . ?
C25 C24 C29 C28 1.3(14) . . . . ?


####################################################################### 
# 
# 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_st59
_database_code_depnum_ccdc_archive 'CCDC 2403407'
loop_
_audit_author_name
_audit_author_address
'Hisako Hashimoto'
;Tohoku University
Japan
;
_audit_update_record             
;
2024-11-18 deposited with the CCDC.	2024-12-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H42 O3 Si2 W'
_chemical_formula_sum            'C24 H42 O3 Si2 W'
_chemical_formula_weight         618.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   26.4496(13)
_cell_length_b                   15.6024(11)
_cell_length_c                   15.8880(9)
_cell_angle_alpha                90
_cell_angle_beta                 125.3613(12)
_cell_angle_gamma                90
_cell_volume                     5347.0(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    21474
_cell_measurement_theta_min      2.61
_cell_measurement_theta_max      27.45

_exptl_crystal_description       block
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_F_000             2496
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.28
_exptl_absorpt_coefficient_mu    4.432
_shelx_estimated_absorpt_T_min   0.246
_shelx_estimated_absorpt_T_max   0.370
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.2459
_exptl_absorpt_correction_T_max  0.3700
_exptl_absorpt_process_details   'NUMABS (Higashi, 1999)'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating-anode X-ray tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.00
_diffrn_reflns_number            24851
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.565
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999

_reflns_number_total             6120
_reflns_number_gt                5690
_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       PROCESS-AUTO
_computing_cell_refinement       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver.1.11'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  
;
'SHELXL-97 (Sheldrick, 1997)', 'SHELXL-2018/3 (Sheldrick, 2018)'
;
_computing_molecular_graphics    'Yadokari-XG2009(Wakita, Nemoto et al.,2009)'
_computing_publication_material  'Yadokari-XG2009(Wakita, Nemoto et al.,2009)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0320P)²+8.4675P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6120
_refine_ls_number_parameters     287
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0263
_refine_ls_wR_factor_ref         0.0660
_refine_ls_wR_factor_gt          0.0643
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_restrained_S_all      1.118
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.879
_refine_diff_density_min         -1.754
_refine_diff_density_rms         0.121

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
W1 W 0.13175(2) 0.16432(2) 0.07153(2) 0.01972(5) Uani 1 1 d . . . . .
Si1 Si 0.08915(4) 0.22276(5) 0.16534(6) 0.02394(16) Uani 1 1 d . . . . .
Si2 Si 0.18951(3) 0.28946(5) 0.18946(6) 0.01977(14) Uani 1 1 d . . . . .
C1 C 0.21711(14) 0.1234(2) 0.1511(2) 0.0298(6) Uani 1 1 d . . . . .
O1 O 0.26582(11) 0.09170(17) 0.1912(2) 0.0452(6) Uani 1 1 d . . . . .
C2 C 0.12825(16) 0.0674(2) 0.1449(2) 0.0319(7) Uani 1 1 d . . . . .
O2 O 0.12722(16) 0.00581(17) 0.1848(2) 0.0529(7) Uani 1 1 d . . . . .
O3 O 0.13328(10) 0.32146(13) 0.21537(16) 0.0244(4) Uani 1 1 d . . . . .
C3 C 0.19750(15) 0.3910(2) 0.1337(2) 0.0312(6) Uani 1 1 d . . . . .
H1 H 0.157024 0.407002 0.071548 0.047 Uiso 1 1 calc R U . . .
H2 H 0.226903 0.381649 0.115948 0.047 Uiso 1 1 calc R U . . .
H3 H 0.212738 0.437185 0.184772 0.047 Uiso 1 1 calc R U . . .
C4 C 0.26598(13) 0.28185(19) 0.3256(2) 0.0257(6) Uani 1 1 d . . . . .
C5 C 0.27752(16) 0.3598(2) 0.3943(3) 0.0376(7) Uani 1 1 d . . . . .
H4 H 0.244647 0.363150 0.405030 0.056 Uiso 1 1 calc R U . . .
H5 H 0.277520 0.412278 0.360371 0.056 Uiso 1 1 calc R U . . .
H6 H 0.317742 0.353501 0.461028 0.056 Uiso 1 1 calc R U . . .
C6 C 0.31935(14) 0.2793(2) 0.3128(3) 0.0355(7) Uani 1 1 d . . . . .
H7 H 0.358646 0.269808 0.380147 0.053 Uiso 1 1 calc R U . . .
H8 H 0.321107 0.333831 0.284018 0.053 Uiso 1 1 calc R U . . .
H9 H 0.312265 0.232460 0.265923 0.053 Uiso 1 1 calc R U . . .
C7 C 0.26914(16) 0.2016(2) 0.3842(2) 0.0359(7) Uani 1 1 d . . . . .
H10 H 0.260897 0.150704 0.341990 0.054 Uiso 1 1 calc R U . . .
H11 H 0.238019 0.205817 0.399016 0.054 Uiso 1 1 calc R U . . .
H12 H 0.310512 0.197138 0.449198 0.054 Uiso 1 1 calc R U . . .
C8 C 0.00558(15) 0.2576(2) 0.0917(3) 0.0372(7) Uani 1 1 d . . . . .
H13 H -0.000317 0.292809 0.136535 0.056 Uiso 1 1 calc R U . . .
H14 H -0.021181 0.206984 0.069106 0.056 Uiso 1 1 calc R U . . .
H15 H -0.005172 0.291239 0.031360 0.056 Uiso 1 1 calc R U . . .
C9 C 0.10036(19) 0.1690(2) 0.2806(3) 0.0388(8) Uani 1 1 d . . . . .
H16 H 0.144150 0.153839 0.329863 0.058 Uiso 1 1 calc R U . . .
H17 H 0.075027 0.116883 0.258590 0.058 Uiso 1 1 calc R U . . .
H18 H 0.087767 0.208066 0.313626 0.058 Uiso 1 1 calc R U . . .
C10 C 0.03491(14) 0.1594(2) -0.0928(2) 0.0298(7) Uani 1 1 d . . . . .
C11 C 0.06534(14) 0.2370(2) -0.0874(2) 0.0295(6) Uani 1 1 d . . . . .
C12 C 0.12050(14) 0.2138(2) -0.0798(2) 0.0298(6) Uani 1 1 d . . . . .
C13 C 0.12425(14) 0.1223(2) -0.0774(2) 0.0313(7) Uani 1 1 d . . . . .
C14 C 0.07132(15) 0.0894(2) -0.0853(2) 0.0316(7) Uani 1 1 d . . . . .
C15 C -0.03025(15) 0.1522(3) -0.1233(3) 0.0415(9) Uani 1 1 d . . . . .
H19 H -0.058313 0.139500 -0.197179 0.062 Uiso 1 1 calc R U . . .
H20 H -0.042475 0.206357 -0.108621 0.062 Uiso 1 1 calc R U . . .
H21 H -0.032513 0.105900 -0.083834 0.062 Uiso 1 1 calc R U . . .
C16 C 0.03890(18) 0.3256(2) -0.1063(3) 0.0416(8) Uani 1 1 d . . . . .
H22 H -0.000307 0.328306 -0.175131 0.062 Uiso 1 1 calc R U . . .
H23 H 0.068244 0.366867 -0.101992 0.062 Uiso 1 1 calc R U . . .
H24 H 0.031476 0.339495 -0.054160 0.062 Uiso 1 1 calc R U . . .
C17 C 0.15980(17) 0.2741(3) -0.0924(3) 0.0412(8) Uani 1 1 d . . . . .
H25 H 0.199554 0.246657 -0.067030 0.062 Uiso 1 1 calc R U . . .
H26 H 0.167137 0.326523 -0.052902 0.062 Uiso 1 1 calc R U . . .
H27 H 0.138406 0.288428 -0.165582 0.062 Uiso 1 1 calc R U . . .
C18 C 0.17218(17) 0.0703(3) -0.0766(3) 0.0428(9) Uani 1 1 d . . . . .
H28 H 0.174884 0.013249 -0.048425 0.064 Uiso 1 1 calc R U . . .
H29 H 0.212508 0.098915 -0.033612 0.064 Uiso 1 1 calc R U . . .
H30 H 0.160475 0.064719 -0.147208 0.064 Uiso 1 1 calc R U . . .
C19 C 0.05396(19) -0.0039(3) -0.0926(3) 0.0459(9) Uani 1 1 d . . . . .
H31 H 0.030638 -0.022524 -0.164734 0.069 Uiso 1 1 calc R U . . .
H32 H 0.028305 -0.011249 -0.066917 0.069 Uiso 1 1 calc R U . . .
H33 H 0.091685 -0.038489 -0.050865 0.069 Uiso 1 1 calc R U . . .
C20 C 0.12438(15) 0.4055(2) 0.2480(3) 0.0331(7) Uani 1 1 d . . . . .
H34 H 0.1622(14) 0.436(2) 0.276(2) 0.014(7) Uiso 1 1 d . . . . .
C21 C 0.07371(17) 0.4539(2) 0.1557(3) 0.0450(9) Uani 1 1 d . . . . .
H35 H 0.033941 0.428210 0.112262 0.054 Uiso 1 1 calc R U . . .
C22 C 0.0827(2) 0.5300(4) 0.1334(4) 0.0728(15) Uani 1 1 d . . . . .
H36 H 0.122219 0.556364 0.176222 0.087 Uiso 1 1 calc R U . . .
H37 H 0.049691 0.559235 0.074372 0.087 Uiso 1 1 calc R U . . .
C23 C 0.1121(2) 0.3911(3) 0.3285(3) 0.0527(10) Uani 1 1 d . . . . .
H38 H 0.068873 0.370931 0.293436 0.063 Uiso 1 1 calc R U . . .
H39 H 0.139711 0.344628 0.375052 0.063 Uiso 1 1 calc R U . . .
C24 C 0.1210(5) 0.4647(4) 0.3904(5) 0.112(3) Uani 1 1 d . . . . .
H40 H 0.161853 0.489684 0.418935 0.168 Uiso 1 1 calc R U . . .
H41 H 0.118254 0.447093 0.446877 0.168 Uiso 1 1 calc R U . . .
H42 H 0.088766 0.507285 0.347411 0.168 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
W1 C2 1.945(3) . ?
W1 C1 1.949(3) . ?
W1 C14 2.349(3) . ?
W1 C13 2.350(3) . ?
W1 C11 2.369(3) . ?
W1 C12 2.374(3) . ?
W1 C10 2.376(3) . ?
W1 Si1 2.5034(8) . ?
W1 Si2 2.5187(8) . ?
Si1 O3 1.814(2) . ?
Si1 C9 1.876(3) . ?
Si1 C8 1.886(3) . ?
Si1 Si2 2.6645(10) . ?
Si2 O3 1.827(2) . ?
Si2 C3 1.886(3) . ?
Si2 C4 1.929(3) . ?
C1 O1 1.166(4) . ?
C2 O2 1.160(4) . ?
O3 C20 1.478(4) . ?
C3 H1 0.9800 . ?
C3 H2 0.9800 . ?
C3 H3 0.9800 . ?
C4 C7 1.533(4) . ?
C4 C6 1.539(4) . ?
C4 C5 1.542(4) . ?
C5 H4 0.9800 . ?
C5 H5 0.9800 . ?
C5 H6 0.9800 . ?
C6 H7 0.9800 . ?
C6 H8 0.9800 . ?
C6 H9 0.9800 . ?
C7 H10 0.9800 . ?
C7 H11 0.9800 . ?
C7 H12 0.9800 . ?
C8 H13 0.9800 . ?
C8 H14 0.9800 . ?
C8 H15 0.9800 . ?
C9 H16 0.9800 . ?
C9 H17 0.9800 . ?
C9 H18 0.9800 . ?
C10 C14 1.416(5) . ?
C10 C11 1.428(5) . ?
C10 C15 1.501(4) . ?
C11 C12 1.438(4) . ?
C11 C16 1.499(5) . ?
C12 C13 1.430(5) . ?
C12 C17 1.499(5) . ?
C13 C14 1.427(4) . ?
C13 C18 1.499(5) . ?
C14 C19 1.510(5) . ?
C15 H19 0.9800 . ?
C15 H20 0.9800 . ?
C15 H21 0.9800 . ?
C16 H22 0.9800 . ?
C16 H23 0.9800 . ?
C16 H24 0.9800 . ?
C17 H25 0.9800 . ?
C17 H26 0.9800 . ?
C17 H27 0.9800 . ?
C18 H28 0.9800 . ?
C18 H29 0.9800 . ?
C18 H30 0.9800 . ?
C19 H31 0.9800 . ?
C19 H32 0.9800 . ?
C19 H33 0.9800 . ?
C20 C21 1.497(5) . ?
C20 C23 1.508(5) . ?
C20 H34 0.96(3) . ?
C21 C22 1.300(6) . ?
C21 H35 0.9500 . ?
C22 H36 0.9500 . ?
C22 H37 0.9500 . ?
C23 C24 1.440(6) . ?
C23 H38 0.9900 . ?
C23 H39 0.9900 . ?
C24 H40 0.9800 . ?
C24 H41 0.9800 . ?
C24 H42 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
C2 W1 C1 78.20(14) . . ?
C2 W1 C14 90.52(12) . . ?
C1 W1 C14 110.28(12) . . ?
C2 W1 C13 112.39(13) . . ?
C1 W1 C13 87.31(12) . . ?
C14 W1 C13 35.36(11) . . ?
C2 W1 C11 138.42(12) . . ?
C1 W1 C11 135.57(12) . . ?
C14 W1 C11 58.56(13) . . ?
C13 W1 C11 58.80(11) . . ?
C2 W1 C12 147.00(12) . . ?
C1 W1 C12 100.54(12) . . ?
C14 W1 C12 58.59(11) . . ?
C13 W1 C12 35.25(13) . . ?
C11 W1 C12 35.31(10) . . ?
C2 W1 C10 103.82(12) . . ?
C1 W1 C10 144.08(12) . . ?
C14 W1 C10 34.86(11) . . ?
C13 W1 C10 58.36(11) . . ?
C11 W1 C10 35.03(11) . . ?
C12 W1 C10 58.26(11) . . ?
C2 W1 Si1 74.48(10) . . ?
C1 W1 Si1 118.98(9) . . ?
C14 W1 Si1 123.24(8) . . ?
C13 W1 Si1 153.66(8) . . ?
C11 W1 Si1 98.55(8) . . ?
C12 W1 Si1 130.43(8) . . ?
C10 W1 Si1 95.48(8) . . ?
C2 W1 Si2 112.09(9) . . ?
C1 W1 Si2 78.18(9) . . ?
C14 W1 Si2 157.27(9) . . ?
C13 W1 Si2 128.80(8) . . ?
C11 W1 Si2 100.27(8) . . ?
C12 W1 Si2 99.65(8) . . ?
C10 W1 Si2 130.28(8) . . ?
Si1 W1 Si2 64.08(3) . . ?
O3 Si1 C9 104.71(14) . . ?
O3 Si1 C8 104.64(14) . . ?
C9 Si1 C8 101.58(17) . . ?
O3 Si1 W1 99.95(7) . . ?
C9 Si1 W1 123.17(12) . . ?
C8 Si1 W1 120.38(11) . . ?
O3 Si1 Si2 43.17(7) . . ?
C9 Si1 Si2 116.93(13) . . ?
C8 Si1 Si2 133.56(12) . . ?
W1 Si1 Si2 58.24(2) . . ?
O3 Si2 C3 101.73(13) . . ?
O3 Si2 C4 103.07(11) . . ?
C3 Si2 C4 104.39(14) . . ?
O3 Si2 W1 99.03(7) . . ?
C3 Si2 W1 119.12(10) . . ?
C4 Si2 W1 125.28(10) . . ?
O3 Si2 Si1 42.78(7) . . ?
C3 Si2 Si1 129.32(11) . . ?
C4 Si2 Si1 116.62(9) . . ?
W1 Si2 Si1 57.68(2) . . ?
O1 C1 W1 172.6(3) . . ?
O2 C2 W1 175.1(3) . . ?
C20 O3 Si1 135.57(19) . . ?
C20 O3 Si2 129.54(19) . . ?
Si1 O3 Si2 94.05(10) . . ?
Si2 C3 H1 109.5 . . ?
Si2 C3 H2 109.5 . . ?
H1 C3 H2 109.5 . . ?
Si2 C3 H3 109.5 . . ?
H1 C3 H3 109.5 . . ?
H2 C3 H3 109.5 . . ?
C7 C4 C6 109.1(3) . . ?
C7 C4 C5 107.2(3) . . ?
C6 C4 C5 107.1(3) . . ?
C7 C4 Si2 112.6(2) . . ?
C6 C4 Si2 107.5(2) . . ?
C5 C4 Si2 113.2(2) . . ?
C4 C5 H4 109.5 . . ?
C4 C5 H5 109.5 . . ?
H4 C5 H5 109.5 . . ?
C4 C5 H6 109.5 . . ?
H4 C5 H6 109.5 . . ?
H5 C5 H6 109.5 . . ?
C4 C6 H7 109.5 . . ?
C4 C6 H8 109.5 . . ?
H7 C6 H8 109.5 . . ?
C4 C6 H9 109.5 . . ?
H7 C6 H9 109.5 . . ?
H8 C6 H9 109.5 . . ?
C4 C7 H10 109.5 . . ?
C4 C7 H11 109.5 . . ?
H10 C7 H11 109.5 . . ?
C4 C7 H12 109.5 . . ?
H10 C7 H12 109.5 . . ?
H11 C7 H12 109.5 . . ?
Si1 C8 H13 109.5 . . ?
Si1 C8 H14 109.5 . . ?
H13 C8 H14 109.5 . . ?
Si1 C8 H15 109.5 . . ?
H13 C8 H15 109.5 . . ?
H14 C8 H15 109.5 . . ?
Si1 C9 H16 109.5 . . ?
Si1 C9 H17 109.5 . . ?
H16 C9 H17 109.5 . . ?
Si1 C9 H18 109.5 . . ?
H16 C9 H18 109.5 . . ?
H17 C9 H18 109.5 . . ?
C14 C10 C11 108.5(3) . . ?
C14 C10 C15 124.5(3) . . ?
C11 C10 C15 125.9(3) . . ?
C14 C10 W1 71.55(17) . . ?
C11 C10 W1 72.23(16) . . ?
C15 C10 W1 131.5(2) . . ?
C10 C11 C12 107.5(3) . . ?
C10 C11 C16 126.0(3) . . ?
C12 C11 C16 125.5(3) . . ?
C10 C11 W1 72.74(17) . . ?
C12 C11 W1 72.52(17) . . ?
C16 C11 W1 128.8(2) . . ?
C13 C12 C11 107.7(3) . . ?
C13 C12 C17 125.9(3) . . ?
C11 C12 C17 125.4(3) . . ?
C13 C12 W1 71.46(16) . . ?
C11 C12 W1 72.17(16) . . ?
C17 C12 W1 130.5(2) . . ?
C14 C13 C12 107.9(3) . . ?
C14 C13 C18 126.0(3) . . ?
C12 C13 C18 125.9(3) . . ?
C14 C13 W1 72.30(16) . . ?
C12 C13 W1 73.29(16) . . ?
C18 C13 W1 124.4(2) . . ?
C10 C14 C13 108.3(3) . . ?
C10 C14 C19 125.2(3) . . ?
C13 C14 C19 126.4(3) . . ?
C10 C14 W1 73.59(17) . . ?
C13 C14 W1 72.34(17) . . ?
C19 C14 W1 123.5(2) . . ?
C10 C15 H19 109.5 . . ?
C10 C15 H20 109.5 . . ?
H19 C15 H20 109.5 . . ?
C10 C15 H21 109.5 . . ?
H19 C15 H21 109.5 . . ?
H20 C15 H21 109.5 . . ?
C11 C16 H22 109.5 . . ?
C11 C16 H23 109.5 . . ?
H22 C16 H23 109.5 . . ?
C11 C16 H24 109.5 . . ?
H22 C16 H24 109.5 . . ?
H23 C16 H24 109.5 . . ?
C12 C17 H25 109.5 . . ?
C12 C17 H26 109.5 . . ?
H25 C17 H26 109.5 . . ?
C12 C17 H27 109.5 . . ?
H25 C17 H27 109.5 . . ?
H26 C17 H27 109.5 . . ?
C13 C18 H28 109.5 . . ?
C13 C18 H29 109.5 . . ?
H28 C18 H29 109.5 . . ?
C13 C18 H30 109.5 . . ?
H28 C18 H30 109.5 . . ?
H29 C18 H30 109.5 . . ?
C14 C19 H31 109.5 . . ?
C14 C19 H32 109.5 . . ?
H31 C19 H32 109.5 . . ?
C14 C19 H33 109.5 . . ?
H31 C19 H33 109.5 . . ?
H32 C19 H33 109.5 . . ?
O3 C20 C21 109.7(3) . . ?
O3 C20 C23 108.7(3) . . ?
C21 C20 C23 113.3(3) . . ?
O3 C20 H34 106.0(18) . . ?
C21 C20 H34 107.7(19) . . ?
C23 C20 H34 111.2(18) . . ?
C22 C21 C20 121.7(4) . . ?
C22 C21 H35 119.1 . . ?
C20 C21 H35 119.1 . . ?
C21 C22 H36 120.0 . . ?
C21 C22 H37 120.0 . . ?
H36 C22 H37 120.0 . . ?
C24 C23 C20 115.5(5) . . ?
C24 C23 H38 108.4 . . ?
C20 C23 H38 108.4 . . ?
C24 C23 H39 108.4 . . ?
C20 C23 H39 108.4 . . ?
H38 C23 H39 107.5 . . ?
C23 C24 H40 109.5 . . ?
C23 C24 H41 109.5 . . ?
H40 C24 H41 109.5 . . ?
C23 C24 H42 109.5 . . ?
H40 C24 H42 109.5 . . ?
H41 C24 H42 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 Si1 O3 C20 -76.4(3) . . . . ?
C8 Si1 O3 C20 30.0(3) . . . . ?
W1 Si1 O3 C20 155.3(3) . . . . ?
Si2 Si1 O3 C20 169.7(3) . . . . ?
C9 Si1 O3 Si2 113.87(14) . . . . ?
C8 Si1 O3 Si2 -139.68(13) . . . . ?
W1 Si1 O3 Si2 -14.47(9) . . . . ?
C3 Si2 O3 C20 -33.9(3) . . . . ?
C4 Si2 O3 C20 74.1(3) . . . . ?
W1 Si2 O3 C20 -156.3(2) . . . . ?
Si1 Si2 O3 C20 -170.7(3) . . . . ?
C3 Si2 O3 Si1 136.77(12) . . . . ?
C4 Si2 O3 Si1 -115.24(12) . . . . ?
W1 Si2 O3 Si1 14.34(9) . . . . ?
C14 C10 C11 C12 1.9(3) . . . . ?
C15 C10 C11 C12 -166.5(3) . . . . ?
W1 C10 C11 C12 64.66(19) . . . . ?
C14 C10 C11 C16 171.4(3) . . . . ?
C15 C10 C11 C16 3.0(5) . . . . ?
W1 C10 C11 C16 -125.9(3) . . . . ?
C14 C10 C11 W1 -62.8(2) . . . . ?
C15 C10 C11 W1 128.9(3) . . . . ?
C10 C11 C12 C13 -1.8(3) . . . . ?
C16 C11 C12 C13 -171.3(3) . . . . ?
W1 C11 C12 C13 63.04(19) . . . . ?
C10 C11 C12 C17 167.7(3) . . . . ?
C16 C11 C12 C17 -1.8(5) . . . . ?
W1 C11 C12 C17 -127.5(3) . . . . ?
C10 C11 C12 W1 -64.8(2) . . . . ?
C16 C11 C12 W1 125.7(3) . . . . ?
C11 C12 C13 C14 1.0(3) . . . . ?
C17 C12 C13 C14 -168.4(3) . . . . ?
W1 C12 C13 C14 64.5(2) . . . . ?
C11 C12 C13 C18 175.8(3) . . . . ?
C17 C12 C13 C18 6.4(5) . . . . ?
W1 C12 C13 C18 -120.7(3) . . . . ?
C11 C12 C13 W1 -63.50(19) . . . . ?
C17 C12 C13 W1 127.1(3) . . . . ?
C11 C10 C14 C13 -1.3(3) . . . . ?
C15 C10 C14 C13 167.3(3) . . . . ?
W1 C10 C14 C13 -64.5(2) . . . . ?
C11 C10 C14 C19 -177.1(3) . . . . ?
C15 C10 C14 C19 -8.5(5) . . . . ?
W1 C10 C14 C19 119.7(3) . . . . ?
C11 C10 C14 W1 63.2(2) . . . . ?
C15 C10 C14 W1 -128.2(3) . . . . ?
C12 C13 C14 C10 0.2(3) . . . . ?
C18 C13 C14 C10 -174.6(3) . . . . ?
W1 C13 C14 C10 65.3(2) . . . . ?
C12 C13 C14 C19 175.9(3) . . . . ?
C18 C13 C14 C19 1.1(5) . . . . ?
W1 C13 C14 C19 -119.0(3) . . . . ?
C12 C13 C14 W1 -65.1(2) . . . . ?
C18 C13 C14 W1 120.0(3) . . . . ?
Si1 O3 C20 C21 -69.8(4) . . . . ?
Si2 O3 C20 C21 96.8(3) . . . . ?
Si1 O3 C20 C23 54.6(4) . . . . ?
Si2 O3 C20 C23 -138.7(3) . . . . ?
O3 C20 C21 C22 -123.9(5) . . . . ?
C23 C20 C21 C22 114.4(5) . . . . ?
O3 C20 C23 C24 161.9(5) . . . . ?
C21 C20 C23 C24 -75.8(6) . . . . ?


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

data_matsuo02
_database_code_depnum_ccdc_archive 'CCDC 2403406'
loop_
_audit_author_name
_audit_author_address
'Hisako Hashimoto'
;Tohoku University
Japan
;
_audit_update_record             
;
2024-11-18 deposited with the CCDC.	2024-12-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H48 O3 Si2 W'
_chemical_formula_sum            'C29 H48 O3 Si2 W'
_chemical_formula_weight         684.70

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'
W W -0.8490 6.8722 '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      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

_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+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   17.1114(6)
_cell_length_b                   10.5152(5)
_cell_length_c                   16.3940(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2949.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    140(2)
_cell_measurement_reflns_used    36306
_cell_measurement_theta_min      1.72
_cell_measurement_theta_max      27.41

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_F_000             1392
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_exptl_absorpt_coefficient_mu    4.025
_shelx_estimated_absorpt_T_min   0.500
_shelx_estimated_absorpt_T_max   0.565
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.4999
_exptl_absorpt_correction_T_max  0.5652
_exptl_absorpt_process_details   'NUMABS (Higashi, 1999)'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      140(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating-anode X-ray tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.00
_diffrn_reflns_number            24264
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.301
_diffrn_reflns_theta_max         27.404
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.997

_reflns_number_total             6660
_reflns_number_gt                6054
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_max     0.988
_reflns_Friedel_fraction_full    0.994

_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       PROCESS-AUTO
_computing_cell_refinement       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver.1.11'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  
;
'SHELXL-97 (Sheldrick, 1997)', 'SHELXL-2018/3 (Sheldrick, 2018)'
;
_computing_molecular_graphics    'Yadokari-XG2009(Wakita, Nemoto et al.,2009)'
_computing_publication_material  'Yadokari-XG2009(Wakita, Nemoto et al.,2009)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0139P)²+9.2217P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2486 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(7)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6660
_refine_ls_number_parameters     327
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0368
_refine_ls_wR_factor_ref         0.0666
_refine_ls_wR_factor_gt          0.0650
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_restrained_S_all      1.173
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.247
_refine_diff_density_min         -1.543
_refine_diff_density_rms         0.117

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
W1 W 0.85843(2) 0.47963(2) 0.72844(2) 0.01715(7) Uani 1 1 d . . . . .
Si1 Si 0.73156(13) 0.3596(2) 0.74960(11) 0.0182(5) Uani 1 1 d . . . . .
Si2 Si 0.79573(15) 0.5007(2) 0.86561(14) 0.0216(5) Uani 1 1 d . . . . .
O1 O 0.6987(3) 0.4381(5) 0.8462(3) 0.0169(11) Uani 1 1 d . . . . .
C1 C 0.9009(5) 0.3099(8) 0.7118(5) 0.026(2) Uani 1 1 d . . . . .
C2 C 0.9363(5) 0.4765(9) 0.8144(5) 0.0261(18) Uani 1 1 d . . . . .
O2 O 0.9330(4) 0.2143(6) 0.6988(4) 0.0385(17) Uani 1 1 d . . . . .
O3 O 0.9860(4) 0.4825(8) 0.8622(4) 0.0408(19) Uani 1 1 d . . . . .
C3 C 0.8039(5) 0.6404(9) 0.6440(6) 0.029(2) Uani 1 1 d . . . . .
C4 C 0.8355(6) 0.5457(9) 0.5927(5) 0.029(2) Uani 1 1 d . . . . .
C5 C 0.9170(6) 0.5410(9) 0.6047(5) 0.031(2) Uani 1 1 d . . . . .
C6 C 0.9368(5) 0.6331(8) 0.6635(5) 0.028(2) Uani 1 1 d . . . . .
C7 C 0.8672(6) 0.6949(8) 0.6890(5) 0.0287(19) Uani 1 1 d . . . . .
C8 C 0.7227(6) 0.6968(10) 0.6430(7) 0.045(3) Uani 1 1 d . . . . .
H8 H 0.689689 0.648525 0.605166 0.068 Uiso 1 1 calc R U . . .
H8A H 0.725441 0.785659 0.625161 0.068 Uiso 1 1 calc R U . . .
H8B H 0.700259 0.692811 0.697904 0.068 Uiso 1 1 calc R U . . .
C9 C 0.7951(8) 0.4708(11) 0.5250(6) 0.047(3) Uani 1 1 d . . . . .
H9 H 0.739547 0.493441 0.523424 0.071 Uiso 1 1 calc R U . . .
H9A H 0.800404 0.379488 0.535757 0.071 Uiso 1 1 calc R U . . .
H9B H 0.819326 0.491240 0.472502 0.071 Uiso 1 1 calc R U . . .
C10 C 0.9761(8) 0.4579(12) 0.5594(7) 0.050(4) Uani 1 1 d . . . . .
H10 H 0.988748 0.497190 0.506784 0.075 Uiso 1 1 calc R U . . .
H10A H 0.953561 0.373454 0.550159 0.075 Uiso 1 1 calc R U . . .
H10B H 1.023741 0.449923 0.592083 0.075 Uiso 1 1 calc R U . . .
C11 C 1.0185(6) 0.6710(11) 0.6899(7) 0.047(3) Uani 1 1 d . . . . .
H11 H 1.054968 0.601778 0.677653 0.070 Uiso 1 1 calc R U . . .
H11A H 1.018771 0.688024 0.748656 0.070 Uiso 1 1 calc R U . . .
H11B H 1.034465 0.747810 0.660394 0.070 Uiso 1 1 calc R U . . .
C12 C 0.8628(7) 0.8126(8) 0.7403(9) 0.046(3) Uani 1 1 d . . . . .
H12 H 0.898421 0.804404 0.786833 0.070 Uiso 1 1 calc R U . . .
H12A H 0.809232 0.823802 0.760219 0.070 Uiso 1 1 calc R U . . .
H12B H 0.877860 0.886508 0.707490 0.070 Uiso 1 1 calc R U . . .
C13 C 0.6487(5) 0.3931(9) 0.6760(5) 0.0271(19) Uani 1 1 d . . . . .
H13 H 0.603297 0.340999 0.690540 0.041 Uiso 1 1 calc R U . . .
H13A H 0.665344 0.372449 0.620339 0.041 Uiso 1 1 calc R U . . .
H13B H 0.634500 0.483328 0.678948 0.041 Uiso 1 1 calc R U . . .
C14 C 0.7262(5) 0.1763(8) 0.7648(6) 0.0241(19) Uani 1 1 d . . . . .
C15 C 0.7449(6) 0.1224(10) 0.6778(6) 0.035(2) Uani 1 1 d . . . . .
H15 H 0.747907 0.029452 0.680337 0.053 Uiso 1 1 calc R U . . .
H15A H 0.795042 0.156620 0.658994 0.053 Uiso 1 1 calc R U . . .
H15B H 0.703512 0.147562 0.639805 0.053 Uiso 1 1 calc R U . . .
C16 C 0.6465(6) 0.1229(8) 0.7882(6) 0.036(2) Uani 1 1 d . . . . .
H16 H 0.647533 0.029968 0.783768 0.054 Uiso 1 1 calc R U . . .
H16A H 0.606580 0.157179 0.751451 0.054 Uiso 1 1 calc R U . . .
H16B H 0.634201 0.147139 0.844491 0.054 Uiso 1 1 calc R U . . .
C17 C 0.7853(5) 0.1288(9) 0.8265(6) 0.029(2) Uani 1 1 d . . . . .
H17 H 0.774367 0.166936 0.879840 0.044 Uiso 1 1 calc R U . . .
H17A H 0.837984 0.152663 0.808874 0.044 Uiso 1 1 calc R U . . .
H17B H 0.781669 0.036001 0.830667 0.044 Uiso 1 1 calc R U . . .
C18 C 0.7875(6) 0.6663(9) 0.9080(6) 0.033(2) Uani 1 1 d . . . . .
H18 H 0.758520 0.719888 0.869541 0.050 Uiso 1 1 calc R U . . .
H18A H 0.839909 0.701603 0.916177 0.050 Uiso 1 1 calc R U . . .
H18B H 0.759779 0.663656 0.960241 0.050 Uiso 1 1 calc R U . . .
C19 C 0.8273(6) 0.4043(10) 0.9573(5) 0.030(2) Uani 1 1 d . . . . .
H19 H 0.781232 0.380301 0.989269 0.045 Uiso 1 1 calc R U . . .
H19A H 0.862635 0.455177 0.991139 0.045 Uiso 1 1 calc R U . . .
H19B H 0.854415 0.327345 0.938864 0.045 Uiso 1 1 calc R U . . .
C20 C 0.6371(5) 0.4017(8) 0.9061(5) 0.0249(17) Uani 1 1 d . . . . .
H20 H 0.651740 0.317750 0.930332 0.030 Uiso 1 1 calc R U . . .
C21 C 0.6295(5) 0.4982(8) 0.9755(6) 0.0287(19) Uani 1 1 d . . . . .
H21 H 0.681822 0.511576 1.001392 0.034 Uiso 1 1 calc R U . . .
C22 C 0.5975(6) 0.6254(9) 0.9463(6) 0.034(2) Uani 1 1 d . . . . .
H22 H 0.633652 0.663030 0.905774 0.041 Uiso 1 1 calc R U . . .
H22A H 0.593214 0.684772 0.992932 0.041 Uiso 1 1 calc R U . . .
C23 C 0.5172(6) 0.6059(10) 0.9077(7) 0.038(2) Uani 1 1 d . . . . .
H23 H 0.496345 0.689588 0.888580 0.045 Uiso 1 1 calc R U . . .
C24 C 0.5261(6) 0.5165(9) 0.8351(6) 0.032(2) Uani 1 1 d . . . . .
H24 H 0.562514 0.554049 0.794806 0.038 Uiso 1 1 calc R U . . .
H24A H 0.474828 0.504397 0.808265 0.038 Uiso 1 1 calc R U . . .
C25 C 0.5579(5) 0.3873(8) 0.8643(6) 0.0277(19) Uani 1 1 d . . . . .
H25 H 0.563146 0.328666 0.816521 0.033 Uiso 1 1 calc R U . . .
C26 C 0.5013(6) 0.3290(10) 0.9267(6) 0.035(2) Uani 1 1 d . . . . .
H26 H 0.521462 0.245810 0.945596 0.042 Uiso 1 1 calc R U . . .
H26A H 0.449527 0.315145 0.901205 0.042 Uiso 1 1 calc R U . . .
C27 C 0.4933(7) 0.4209(11) 0.9999(7) 0.041(3) Uani 1 1 d . . . . .
H27 H 0.456940 0.383371 1.041078 0.049 Uiso 1 1 calc R U . . .
C28 C 0.5731(6) 0.4409(11) 1.0385(6) 0.040(2) Uani 1 1 d . . . . .
H28 H 0.593831 0.358532 1.058203 0.048 Uiso 1 1 calc R U . . .
H28A H 0.568299 0.498822 1.085835 0.048 Uiso 1 1 calc R U . . .
C29 C 0.4606(7) 0.5478(11) 0.9703(7) 0.047(3) Uani 1 1 d . . . . .
H29 H 0.454139 0.606441 1.017032 0.056 Uiso 1 1 calc R U . . .
H29A H 0.408771 0.534556 0.944837 0.056 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
W1 C2 1.940(8) . ?
W1 C1 1.947(9) . ?
W1 C6 2.353(8) . ?
W1 C5 2.353(8) . ?
W1 C7 2.359(8) . ?
W1 C4 2.364(8) . ?
W1 C3 2.377(8) . ?
W1 Si2 2.502(2) . ?
W1 Si1 2.535(2) . ?
Si1 O1 1.873(5) . ?
Si1 C13 1.896(8) . ?
Si1 C14 1.945(9) . ?
Si1 Si2 2.651(3) . ?
Si2 O1 1.815(6) . ?
Si2 C18 1.879(9) . ?
Si2 C19 1.892(10) . ?
O1 C20 1.490(10) . ?
C1 O2 1.165(10) . ?
C2 O3 1.159(11) . ?
C3 C4 1.411(14) . ?
C3 C7 1.431(13) . ?
C3 C8 1.510(13) . ?
C4 C5 1.410(15) . ?
C4 C9 1.526(13) . ?
C5 C6 1.407(13) . ?
C5 C10 1.529(15) . ?
C6 C7 1.420(13) . ?
C6 C11 1.516(13) . ?
C7 C12 1.499(14) . ?
C14 C17 1.515(13) . ?
C14 C16 1.523(13) . ?
C14 C15 1.568(12) . ?
C20 C25 1.528(12) . ?
C20 C21 1.530(12) . ?
C21 C22 1.522(13) . ?
C21 C28 1.537(13) . ?
C22 C23 1.526(14) . ?
C23 C24 1.525(14) . ?
C23 C29 1.538(15) . ?
C24 C25 1.539(12) . ?
C25 C26 1.537(12) . ?
C26 C27 1.546(14) . ?
C27 C28 1.520(16) . ?
C27 C29 1.526(15) . ?

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 W1 C1 80.2(4) . . ?
C2 W1 C6 87.1(3) . . ?
C1 W1 C6 110.7(3) . . ?
C2 W1 C5 109.8(4) . . ?
C1 W1 C5 88.4(3) . . ?
C6 W1 C5 34.8(3) . . ?
C2 W1 C7 99.9(4) . . ?
C1 W1 C7 144.9(3) . . ?
C6 W1 C7 35.1(3) . . ?
C5 W1 C7 58.2(3) . . ?
C2 W1 C4 143.4(4) . . ?
C1 W1 C4 101.5(3) . . ?
C6 W1 C4 57.8(3) . . ?
C5 W1 C4 34.8(4) . . ?
C7 W1 C4 58.0(3) . . ?
C2 W1 C3 134.9(4) . . ?
C1 W1 C3 135.8(3) . . ?
C6 W1 C3 58.2(3) . . ?
C5 W1 C3 58.0(3) . . ?
C7 W1 C3 35.2(3) . . ?
C4 W1 C3 34.6(3) . . ?
C2 W1 Si2 69.1(3) . . ?
C1 W1 Si2 111.6(2) . . ?
C6 W1 Si2 126.2(2) . . ?
C5 W1 Si2 159.0(2) . . ?
C7 W1 Si2 100.9(2) . . ?
C4 W1 Si2 138.5(3) . . ?
C3 W1 Si2 107.0(2) . . ?
C2 W1 Si1 118.7(3) . . ?
C1 W1 Si1 83.2(3) . . ?
C6 W1 Si1 153.1(2) . . ?
C5 W1 Si1 128.3(3) . . ?
C7 W1 Si1 124.7(2) . . ?
C4 W1 Si1 97.6(3) . . ?
C3 W1 Si1 95.6(2) . . ?
Si2 W1 Si1 63.51(7) . . ?
O1 Si1 C13 103.4(3) . . ?
O1 Si1 C14 108.3(3) . . ?
C13 Si1 C14 103.3(4) . . ?
O1 Si1 W1 98.84(18) . . ?
C13 Si1 W1 117.5(3) . . ?
C14 Si1 W1 123.5(3) . . ?
O1 Si1 Si2 43.18(18) . . ?
C13 Si1 Si2 131.5(3) . . ?
C14 Si1 Si2 118.8(3) . . ?
W1 Si1 Si2 57.63(7) . . ?
O1 Si2 C18 109.4(4) . . ?
O1 Si2 C19 101.9(4) . . ?
C18 Si2 C19 103.0(5) . . ?
O1 Si2 W1 101.69(19) . . ?
C18 Si2 W1 116.5(3) . . ?
C19 Si2 W1 122.9(3) . . ?
O1 Si2 Si1 44.92(18) . . ?
C18 Si2 Si1 138.8(4) . . ?
C19 Si2 Si1 112.8(3) . . ?
W1 Si2 Si1 58.86(7) . . ?
C20 O1 Si2 128.6(5) . . ?
C20 O1 Si1 131.1(5) . . ?
Si2 O1 Si1 91.9(3) . . ?
O2 C1 W1 173.1(7) . . ?
O3 C2 W1 174.3(8) . . ?
C4 C3 C7 107.4(8) . . ?
C4 C3 C8 128.6(9) . . ?
C7 C3 C8 123.0(9) . . ?
C4 C3 W1 72.2(5) . . ?
C7 C3 W1 71.7(5) . . ?
C8 C3 W1 130.3(7) . . ?
C5 C4 C3 108.7(8) . . ?
C5 C4 C9 122.1(10) . . ?
C3 C4 C9 128.6(10) . . ?
C5 C4 W1 72.2(5) . . ?
C3 C4 W1 73.2(5) . . ?
C9 C4 W1 127.4(6) . . ?
C6 C5 C4 108.0(8) . . ?
C6 C5 C10 124.5(10) . . ?
C4 C5 C10 127.3(10) . . ?
C6 C5 W1 72.6(5) . . ?
C4 C5 W1 73.0(5) . . ?
C10 C5 W1 123.0(7) . . ?
C5 C6 C7 108.3(8) . . ?
C5 C6 C11 126.7(9) . . ?
C7 C6 C11 124.7(9) . . ?
C5 C6 W1 72.6(5) . . ?
C7 C6 W1 72.7(5) . . ?
C11 C6 W1 125.2(6) . . ?
C6 C7 C3 107.5(8) . . ?
C6 C7 C12 125.8(9) . . ?
C3 C7 C12 125.6(9) . . ?
C6 C7 W1 72.2(5) . . ?
C3 C7 W1 73.1(5) . . ?
C12 C7 W1 129.4(7) . . ?
C17 C14 C16 107.9(8) . . ?
C17 C14 C15 110.5(7) . . ?
C16 C14 C15 106.2(8) . . ?
C17 C14 Si1 112.4(6) . . ?
C16 C14 Si1 116.1(6) . . ?
C15 C14 Si1 103.4(6) . . ?
O1 C20 C25 110.9(6) . . ?
O1 C20 C21 112.4(7) . . ?
C25 C20 C21 108.9(7) . . ?
C22 C21 C20 112.3(8) . . ?
C22 C21 C28 109.3(8) . . ?
C20 C21 C28 107.0(8) . . ?
C21 C22 C23 109.7(8) . . ?
C24 C23 C22 108.4(8) . . ?
C24 C23 C29 109.8(9) . . ?
C22 C23 C29 110.1(9) . . ?
C23 C24 C25 109.7(8) . . ?
C20 C25 C26 107.4(7) . . ?
C20 C25 C24 111.4(7) . . ?
C26 C25 C24 109.7(8) . . ?
C25 C26 C27 108.8(8) . . ?
C28 C27 C29 110.0(10) . . ?
C28 C27 C26 109.3(8) . . ?
C29 C27 C26 109.4(9) . . ?
C27 C28 C21 109.8(8) . . ?
C27 C29 C23 109.2(9) . . ?

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
C18 Si2 O1 C20 -68.8(7) . . . . ?
C19 Si2 O1 C20 39.7(7) . . . . ?
W1 Si2 O1 C20 167.4(5) . . . . ?
Si1 Si2 O1 C20 150.2(7) . . . . ?
C18 Si2 O1 Si1 141.0(4) . . . . ?
C19 Si2 O1 Si1 -110.5(4) . . . . ?
W1 Si2 O1 Si1 17.2(2) . . . . ?
C13 Si1 O1 C20 73.1(7) . . . . ?
C14 Si1 O1 C20 -36.1(7) . . . . ?
W1 Si1 O1 C20 -165.8(6) . . . . ?
Si2 Si1 O1 C20 -149.0(7) . . . . ?
C13 Si1 O1 Si2 -137.9(3) . . . . ?
C14 Si1 O1 Si2 113.0(4) . . . . ?
W1 Si1 O1 Si2 -16.8(2) . . . . ?
C7 C3 C4 C5 -0.3(10) . . . . ?
C8 C3 C4 C5 168.3(9) . . . . ?
W1 C3 C4 C5 -63.9(6) . . . . ?
C7 C3 C4 C9 -171.7(9) . . . . ?
C8 C3 C4 C9 -3.0(16) . . . . ?
W1 C3 C4 C9 124.8(10) . . . . ?
C7 C3 C4 W1 63.5(6) . . . . ?
C8 C3 C4 W1 -127.8(10) . . . . ?
C3 C4 C5 C6 -0.1(10) . . . . ?
C9 C4 C5 C6 171.9(8) . . . . ?
W1 C4 C5 C6 -64.6(6) . . . . ?
C3 C4 C5 C10 -176.6(9) . . . . ?
C9 C4 C5 C10 -4.6(15) . . . . ?
W1 C4 C5 C10 118.9(10) . . . . ?
C3 C4 C5 W1 64.5(6) . . . . ?
C9 C4 C5 W1 -123.5(8) . . . . ?
C4 C5 C6 C7 0.5(10) . . . . ?
C10 C5 C6 C7 177.2(9) . . . . ?
W1 C5 C6 C7 -64.4(6) . . . . ?
C4 C5 C6 C11 -173.7(9) . . . . ?
C10 C5 C6 C11 2.9(15) . . . . ?
W1 C5 C6 C11 121.4(9) . . . . ?
C4 C5 C6 W1 64.9(6) . . . . ?
C10 C5 C6 W1 -118.4(9) . . . . ?
C5 C6 C7 C3 -0.8(10) . . . . ?
C11 C6 C7 C3 173.7(8) . . . . ?
W1 C6 C7 C3 -65.1(6) . . . . ?
C5 C6 C7 C12 -169.4(9) . . . . ?
C11 C6 C7 C12 5.0(15) . . . . ?
W1 C6 C7 C12 126.2(10) . . . . ?
C5 C6 C7 W1 64.3(6) . . . . ?
C11 C6 C7 W1 -121.3(9) . . . . ?
C4 C3 C7 C6 0.7(10) . . . . ?
C8 C3 C7 C6 -168.7(8) . . . . ?
W1 C3 C7 C6 64.5(6) . . . . ?
C4 C3 C7 C12 169.4(9) . . . . ?
C8 C3 C7 C12 -0.1(14) . . . . ?
W1 C3 C7 C12 -126.8(10) . . . . ?
C4 C3 C7 W1 -63.9(6) . . . . ?
C8 C3 C7 W1 126.7(9) . . . . ?
Si2 O1 C20 C25 164.9(5) . . . . ?
Si1 O1 C20 C25 -56.2(9) . . . . ?
Si2 O1 C20 C21 42.8(9) . . . . ?
Si1 O1 C20 C21 -178.4(5) . . . . ?
O1 C20 C21 C22 67.8(9) . . . . ?
C25 C20 C21 C22 -55.5(9) . . . . ?
O1 C20 C21 C28 -172.3(7) . . . . ?
C25 C20 C21 C28 64.4(9) . . . . ?
C20 C21 C22 C23 59.1(10) . . . . ?
C28 C21 C22 C23 -59.5(10) . . . . ?
C21 C22 C23 C24 -60.6(10) . . . . ?
C21 C22 C23 C29 59.5(10) . . . . ?
C22 C23 C24 C25 60.9(10) . . . . ?
C29 C23 C24 C25 -59.5(11) . . . . ?
O1 C20 C25 C26 170.9(7) . . . . ?
C21 C20 C25 C26 -64.9(9) . . . . ?
O1 C20 C25 C24 -69.0(9) . . . . ?
C21 C20 C25 C24 55.2(9) . . . . ?
C23 C24 C25 C20 -59.4(10) . . . . ?
C23 C24 C25 C26 59.4(10) . . . . ?
C20 C25 C26 C27 61.6(10) . . . . ?
C24 C25 C26 C27 -59.6(10) . . . . ?
C25 C26 C27 C28 -59.7(11) . . . . ?
C25 C26 C27 C29 60.7(11) . . . . ?
C29 C27 C28 C21 -60.0(11) . . . . ?
C26 C27 C28 C21 60.1(11) . . . . ?
C22 C21 C28 C27 59.9(11) . . . . ?
C20 C21 C28 C27 -61.9(10) . . . . ?
C28 C27 C29 C23 59.2(11) . . . . ?
C26 C27 C29 C23 -60.9(13) . . . . ?
C24 C23 C29 C27 60.4(12) . . . . ?
C22 C23 C29 C27 -58.9(12) . . . . ?


####################################################################### 
# 
# 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_shelx_trans
_database_code_depnum_ccdc_archive 'CCDC 2403409'
loop_
_audit_author_name
_audit_author_address
'Hisako Hashimoto'
;Tohoku University
Japan
;
_audit_update_record             
;
2024-11-18 deposited with the CCDC.	2024-12-10 downloaded from the CCDC.
;
_audit_creation_date             2024-11-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C26 H44 N2 O2 Si2 W, C7 H8'
_chemical_formula_sum            'C33 H52 N2 O2 Si2 W'
_chemical_formula_weight         748.79
_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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   14.2410(2)
_cell_length_b                   33.3455(6)
_cell_length_c                   14.4026(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6839.4(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    84720
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.22
_shelx_estimated_absorpt_T_max   0.465
_shelx_estimated_absorpt_T_min   0.422
_exptl_absorpt_coefficient_mu    3.478
_exptl_absorpt_correction_T_max  0.4650
_exptl_absorpt_correction_T_min  0.4218
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Higashi, 1999)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3056
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.26
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            48098
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         1.540
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'Rigaku curved IP area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'Imaging plate area detector'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku RAPID S'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'sealed X-ray tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7171
_reflns_number_total             7894
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.741
_refine_diff_density_min         -2.155
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.375
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         7894
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0595
_refine_ls_restrained_S_all      1.375
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+68.3199P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1119
_refine_ls_wR_factor_ref         0.1141
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Sof: H27A(0.5) H27B(0.5) H27C(0.5) H34A(0.5) H34B(0.5) H34C(0.5)
 Fixed U12: C27(0) C28(0) C29(0) C30(0) C31(0) C32(0) C33(0) C34(0) C35(0)
 C38(0)
 Fixed U23: C27(0) C28(0) C29(0) C30(0) C31(0) C32(0) C33(0) C34(0) C35(0)
 C38(0)
 Fixed Uiso: H8A(0.072) H8B(0.072) H8C(0.072) H9A(0.068) H9B(0.068) H9C(0.068)
 H10A(0.062) H10B(0.062) H10C(0.062) H11A(0.06) H11B(0.06) H11C(0.06)
 H12A(0.067) H12B(0.067) H12C(0.067) H13A(0.087) H13B(0.087) H13C(0.087)
 H15A(0.088) H15B(0.088) H15C(0.088) H16A(0.08) H16B(0.08) H16C(0.08)
 H17A(0.08) H17B(0.08) H17C(0.08) H18A(0.064) H18B(0.064) H18C(0.064)
 H19A(0.056) H19B(0.056) H19C(0.056) H20(0.033) H21(0.034) H23(0.034)
 H24(0.037) H25A(0.059) H25B(0.059) H25C(0.059) H26A(0.049) H26B(0.049)
 H26C(0.049) H27A(0.074) H27B(0.074) H27C(0.074) H29(0.042) H30(0.053)
 H31(0.05) H32(0.05) H33(0.044) H34A(0.161) H34B(0.161) H34C(0.161) H36(0.071)
 H37(0.092) H38(0.098)
 Fixed X: H8A(0.300301) H8B(0.305901) H8C(0.3999) H9A(0.36151) H9B(0.4684)
 H9C(0.3941) H10A(0.5149) H10B(0.4268) H10C(0.432488) H11A(0.348701)
 H11B(0.3728) H11C(0.4548) H12A(0.383201) H12B(0.277489) H12C(0.3022)
 H13A(0.0592) H13B(0.16561) H13C(0.081) H15A(-0.023312) H15B(-0.0162) H15C(-
 0.1155) H16A(-0.0527) H16B(-0.0366) H16C(-0.134689) H17A(-0.147699) H17B(-
 0.0519) H17C(-0.0916) H18A(0.2162) H18B(0.3076) H18C(0.2125) H19A(0.0543)
 H19B(0.03599) H19C(0.0749) H20(0.301701) H21(0.36291) H23(0.3016) H24(0.23399)
 H25A(0.4597) H25B(0.4386) H25C(0.3594) H26A(0.31181) H26B(0.4129) H26C(0.4049)
 H27A(0.32431) H27B(0.301001) H27C(0.307) H29(0.1448) H30(-0.0158) H31(-0.0741)
 H32(0.030399) H33(0.1925) H34A(0.4739) H34B(0.4381) H34C(0.473489)
 H36(0.325211) H37(0.1749) H38(0.10521)
 Fixed Y: H8A(0.19521) H8B(0.206589) H8C(0.2042) H9A(0.148211) H9B(0.136)
 H9C(0.1026) H10A(0.0505) H10B(0.023001) H10C(0.0435) H11A(0.06881)
 H11B(0.0343) H11C(0.062201) H12A(0.16571) H12B(0.173901) H12C(0.134399)
 H13A(0.2078) H13B(0.2041) H13C(0.19591) H15A(0.06311) H15B(0.0898)
 H15C(0.0837) H16A(0.14171) H16B(0.094399) H16C(0.113911) H17A(0.1491)
 H17B(0.168211) H17C(0.180901) H18A(0.076589) H18B(0.0498) H18C(0.029201)
 H19A(0.0144) H19B(0.045) H19C(0.0009) H20(-0.02) H21(-0.0825) H23(-0.0691)
 H24(-0.0089) H25A(-0.131089) H25B(-0.1704) H25C(-0.1526) H26A(-0.1434) H26B(-
 0.1628) H26C(-0.11869) C27(0.25) H27A(0.2432) H27B(0.2302) H27C(0.276689)
 C28(0.25) C29(0.25) H29(0.25) C30(0.25) H30(0.25) C31(0.25) H31(0.25)
 C32(0.25) H32(0.25) C33(0.25) H33(0.25) C34(-0.25) H34A(-0.2262) H34B(-0.2497)
 H34C(-0.274199) C35(-0.25) H36(-0.3101) H37(-0.308789) C38(-0.25) H38(-0.25)
 Fixed Z: H8A(0.112801) H8B(0.005) H8C(0.065701) H9A(0.219) H9B(0.199901)
 H9C(0.2308) H10A(0.0741) H10B(0.0475) H10C(0.147901) H11A(-0.181499) H11B(-
 0.10819) H11C(-0.14819) H12A(-0.1704) H12B(-0.138189) H12C(-0.196) H13A(-
 0.0516) H13B(-0.0167) H13C(0.05391) H15A(-0.0704) H15B(-0.1625) H15C(-0.1123)
 H16A(0.0916) H16B(0.0811) H16C(0.051101) H17A(-0.1059) H17B(-0.1434) H17C(-
 0.0437) H18A(0.2958) H18B(0.2779) H18C(0.31321) H19A(0.0991) H19B(0.1827)
 H19C(0.2037) H20(0.255301) H21(0.2319) H23(-0.043611) H24(-0.0093)
 H25A(0.1825) H25B(0.122211) H25C(0.189301) H26A(-0.0403) H26B(-0.0217) H26C(-
 0.0649) H27A(0.625311) H27B(0.7297) H27C(0.703) H29(0.7946) H30(0.7684)
 H31(0.6175) H32(0.493) H33(0.518001) H34A(-0.222511) H34B(-0.312699) H34C(-
 0.223711) H36(-0.2026) H37(-0.136689) H38(-0.1)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_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
W1 W 0.23333(2) 0.09722(2) 0.03667(2) 0.01848(8) Uani 1 1 d . . . . .
Si1 Si 0.10274(15) 0.13829(6) -0.04411(15) 0.0276(4) Uani 1 1 d . . . . .
H1 H 0.114(7) 0.137(3) -0.137(7) 0.06(3) Uiso 1 1 d . . . . .
Si2 Si 0.20109(14) 0.04248(6) 0.14928(13) 0.0237(4) Uani 1 1 d . . . . .
C1 C 0.1513(5) 0.1177(2) 0.1342(5) 0.0233(14) Uani 1 1 d . . . . .
O1 O 0.1098(4) 0.13187(17) 0.1954(4) 0.0367(13) Uani 1 1 d . . . . .
C2 C 0.1651(5) 0.0595(2) -0.0400(5) 0.0233(14) Uani 1 1 d . . . . .
O2 O 0.1331(4) 0.03557(16) -0.0909(4) 0.0325(12) Uani 1 1 d . . . . .
C3 C 0.3477(5) 0.1487(2) 0.0313(6) 0.0290(16) Uani 1 1 d . . . . .
C4 C 0.3794(5) 0.1193(2) 0.0948(5) 0.0260(15) Uani 1 1 d . . . . .
C5 C 0.3969(4) 0.0830(2) 0.0446(6) 0.0267(15) Uani 1 1 d . . . . .
C6 C 0.3741(4) 0.0902(2) -0.0502(5) 0.0277(16) Uani 1 1 d . . . . .
C7 C 0.3434(5) 0.1311(2) -0.0596(5) 0.0302(16) Uani 1 1 d . . . . .
C8 C 0.3375(7) 0.1924(2) 0.0561(8) 0.048(2) Uani 1 1 d . . . . .
H8A H 0.300301 0.195210 0.112801 0.072 Uiso 1 1 d . U . . .
H8B H 0.305901 0.206589 0.005000 0.072 Uiso 1 1 d . U . . .
H8C H 0.399900 0.204200 0.065701 0.072 Uiso 1 1 d . U . . .
C9 C 0.4028(6) 0.1270(3) 0.1947(7) 0.045(2) Uani 1 1 d . . . . .
H9A H 0.361510 0.148211 0.219000 0.068 Uiso 1 1 d . U . . .
H9B H 0.468400 0.136000 0.199901 0.068 Uiso 1 1 d . U . . .
H9C H 0.394100 0.102600 0.230800 0.068 Uiso 1 1 d . U . . .
C10 C 0.4467(5) 0.0467(3) 0.0819(7) 0.041(2) Uani 1 1 d . . . . .
H10A H 0.514900 0.050500 0.074100 0.062 Uiso 1 1 d . U . . .
H10B H 0.426800 0.023001 0.047500 0.062 Uiso 1 1 d . U . . .
H10C H 0.432488 0.043500 0.147901 0.062 Uiso 1 1 d . U . . .
C11 C 0.3886(6) 0.0613(3) -0.1288(6) 0.038(2) Uani 1 1 d . . . . .
H11A H 0.348701 0.068810 -0.181499 0.060 Uiso 1 1 d . U . . .
H11B H 0.372800 0.034300 -0.108190 0.060 Uiso 1 1 d . U . . .
H11C H 0.454800 0.062201 -0.148190 0.060 Uiso 1 1 d . U . . .
C12 C 0.3248(6) 0.1529(3) -0.1483(6) 0.044(2) Uani 1 1 d . . . . .
H12A H 0.383201 0.165710 -0.170400 0.067 Uiso 1 1 d . U . . .
H12B H 0.277489 0.173901 -0.138189 0.067 Uiso 1 1 d . U . . .
H12C H 0.302200 0.134399 -0.196000 0.067 Uiso 1 1 d . U . . .
C13 C 0.1026(8) 0.1930(3) -0.0098(9) 0.061(3) Uani 1 1 d . . . . .
H13A H 0.059200 0.207800 -0.051600 0.087 Uiso 1 1 d . U . . .
H13B H 0.165610 0.204100 -0.016700 0.087 Uiso 1 1 d . U . . .
H13C H 0.081000 0.195910 0.053910 0.087 Uiso 1 1 d . U . . .
C14 C -0.0295(5) 0.1241(2) -0.0428(6) 0.0330(17) Uani 1 1 d . . . . .
C15 C -0.0476(6) 0.0866(3) -0.1019(9) 0.059(3) Uani 1 1 d . . . . .
H15A H -0.023312 0.063110 -0.070400 0.088 Uiso 1 1 d . U . . .
H15B H -0.016200 0.089800 -0.162500 0.088 Uiso 1 1 d . U . . .
H15C H -0.115500 0.083700 -0.112300 0.088 Uiso 1 1 d . U . . .
C16 C -0.0663(6) 0.1178(4) 0.0540(7) 0.054(3) Uani 1 1 d . . . . .
H16A H -0.052700 0.141710 0.091600 0.080 Uiso 1 1 d . U . . .
H16B H -0.036600 0.094399 0.081100 0.080 Uiso 1 1 d . U . . .
H16C H -0.134689 0.113911 0.051101 0.080 Uiso 1 1 d . U . . .
C17 C -0.0850(6) 0.1584(3) -0.0884(8) 0.054(3) Uani 1 1 d . . . . .
H17A H -0.147699 0.149100 -0.105900 0.080 Uiso 1 1 d . U . . .
H17B H -0.051900 0.168211 -0.143400 0.080 Uiso 1 1 d . U . . .
H17C H -0.091600 0.180901 -0.043700 0.080 Uiso 1 1 d . U . . .
C18 C 0.2385(7) 0.0504(2) 0.2738(5) 0.042(2) Uani 1 1 d . . . . .
H18A H 0.216200 0.076589 0.295800 0.064 Uiso 1 1 d . U . . .
H18B H 0.307600 0.049800 0.277900 0.064 Uiso 1 1 d . U . . .
H18C H 0.212500 0.029201 0.313210 0.064 Uiso 1 1 d . U . . .
C19 C 0.0768(6) 0.0234(2) 0.1603(6) 0.0372(19) Uani 1 1 d . . . . .
H19A H 0.054300 0.014400 0.099100 0.056 Uiso 1 1 d . U . . .
H19B H 0.035990 0.045000 0.182700 0.056 Uiso 1 1 d . U . . .
H19C H 0.074900 0.000900 0.203700 0.056 Uiso 1 1 d . U . . .
N1 N 0.2616(4) -0.00768(16) 0.1260(4) 0.0249(12) Uani 1 1 d . . . . .
C20 C 0.3002(5) -0.0305(2) 0.1941(5) 0.0272(15) Uani 1 1 d . . . . .
H20 H 0.301701 -0.020000 0.255301 0.033 Uiso 1 1 d . U . . .
C21 C 0.3382(5) -0.0678(2) 0.1803(5) 0.0275(15) Uani 1 1 d . . . . .
H21 H 0.362910 -0.082500 0.231900 0.034 Uiso 1 1 d . U . . .
C22 C 0.3404(4) -0.0844(2) 0.0894(5) 0.0235(14) Uani 1 1 d . . . . .
C23 C 0.3014(6) -0.0600(2) 0.0192(5) 0.0273(15) Uani 1 1 d . . . . .
H23 H 0.301600 -0.069100 -0.043611 0.034 Uiso 1 1 d . U . . .
C24 C 0.2628(6) -0.0237(2) 0.0401(5) 0.0299(15) Uani 1 1 d . . . . .
H24 H 0.233990 -0.008900 -0.009300 0.037 Uiso 1 1 d . U . . .
N2 N 0.3770(4) -0.12074(17) 0.0720(4) 0.0271(13) Uani 1 1 d . . . . .
C25 C 0.4117(6) -0.1455(2) 0.1478(6) 0.0392(19) Uani 1 1 d . . . . .
H25A H 0.459700 -0.131089 0.182500 0.059 Uiso 1 1 d . U . . .
H25B H 0.438600 -0.170400 0.122211 0.059 Uiso 1 1 d . U . . .
H25C H 0.359400 -0.152600 0.189301 0.059 Uiso 1 1 d . U . . .
C26 C 0.3772(6) -0.1376(2) -0.0212(6) 0.0331(17) Uani 1 1 d . . . . .
H26A H 0.311810 -0.143400 -0.040300 0.049 Uiso 1 1 d . U . . .
H26B H 0.412900 -0.162800 -0.021700 0.049 Uiso 1 1 d . U . . .
H26C H 0.404900 -0.118690 -0.064900 0.049 Uiso 1 1 d . U . . .
C27 C 0.2883(10) 0.250000 0.6811(11) 0.052(4) Uani 1 2 d S T P . .
H27A H 0.324310 0.243200 0.625311 0.074 Uiso 0.5 1 d . U P . .
H27B H 0.301001 0.230200 0.729700 0.074 Uiso 0.5 1 d . U P . .
H27C H 0.307000 0.276689 0.703000 0.074 Uiso 0.5 1 d . U P . .
C28 C 0.1835(7) 0.250000 0.6583(8) 0.031(2) Uani 1 2 d S T P . .
C29 C 0.1214(9) 0.250000 0.7336(8) 0.036(3) Uani 1 2 d S T P . .
H29 H 0.144800 0.250000 0.794600 0.042 Uiso 1 2 d S U P . .
C30 C 0.0260(8) 0.250000 0.7170(11) 0.045(3) Uani 1 2 d S T P . .
H30 H -0.015800 0.250000 0.768400 0.053 Uiso 1 2 d S U P . .
C31 C -0.0083(8) 0.250000 0.6278(11) 0.042(3) Uani 1 2 d S T P . .
H31 H -0.074100 0.250000 0.617500 0.050 Uiso 1 2 d S U P . .
C32 C 0.0533(9) 0.250000 0.5544(9) 0.041(3) Uani 1 2 d S T P . .
H32 H 0.030399 0.250000 0.493000 0.050 Uiso 1 2 d S U P . .
C33 C 0.1501(8) 0.250000 0.5690(9) 0.037(3) Uani 1 2 d S T P . .
H33 H 0.192500 0.250000 0.518001 0.044 Uiso 1 2 d S U P . .
C34 C 0.4403(14) -0.250000 -0.2471(15) 0.110(8) Uani 1 2 d S T P . .
H34A H 0.473900 -0.226200 -0.222511 0.161 Uiso 0.5 1 d . U P . .
H34B H 0.438100 -0.249700 -0.312699 0.161 Uiso 1 2 d S U P . .
H34C H 0.473489 -0.274199 -0.223711 0.161 Uiso 0.5 1 d . U P . .
C35 C 0.3434(9) -0.250000 -0.2069(8) 0.043(3) Uani 1 2 d S T P . .
C36 C 0.2973(9) -0.2853(3) -0.1888(7) 0.058(3) Uani 1 1 d . . . . .
H36 H 0.325211 -0.310100 -0.202600 0.071 Uiso 1 1 d . U . . .
C37 C 0.2072(10) -0.2848(4) -0.1498(8) 0.078(4) Uani 1 1 d . . . . .
H37 H 0.174900 -0.308789 -0.136689 0.092 Uiso 1 1 d . U . . .
C38 C 0.1651(12) -0.250000 -0.1299(13) 0.087(7) Uani 1 2 d S T P . .
H38 H 0.105210 -0.250000 -0.100000 0.098 Uiso 1 2 d S U P . .


_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
W1 Si1 2.586(2) . ?
W1 Si2 2.4846(19) . ?
W1 C1 1.951(7) . ?
W1 C2 1.936(7) . ?
W1 C3 2.368(6) . ?
W1 C4 2.359(7) . ?
W1 C5 2.380(6) . ?
W1 C6 2.375(6) . ?
W1 C7 2.378(7) . ?
Si1 H1 1.35(11) . ?
Si1 C13 1.890(9) . ?
Si1 C14 1.941(8) . ?
Si2 C18 1.890(8) . ?
Si2 C19 1.888(8) . ?
Si2 N1 1.911(6) . ?
C1 O1 1.162(8) . ?
C2 O2 1.175(8) . ?
C3 C4 1.416(11) . ?
C3 C7 1.436(11) . ?
C3 C8 1.507(11) . ?
C4 C5 1.429(10) . ?
C4 C9 1.500(11) . ?
C5 C6 1.424(11) . ?
C5 C10 1.503(10) . ?
C6 C7 1.438(11) . ?
C6 C11 1.499(10) . ?
C7 C12 1.494(11) . ?
C8 H8A 0.978(10) . ?
C8 H8B 0.984(11) . ?
C8 H8C 0.982(9) . ?
C9 H9A 0.985(10) . ?
C9 H9B 0.984(8) . ?
C9 H9C 0.973(11) . ?
C10 H10A 0.986(8) . ?
C10 H10B 0.975(9) . ?
C10 H10C 0.978(10) . ?
C11 H11A 0.981(9) . ?
C11 H11B 0.975(9) . ?
C11 H11C 0.984(8) . ?
C12 H12A 0.988(8) . ?
C12 H12B 0.983(9) . ?
C12 H12C 0.977(10) . ?
C13 H13A 0.994(10) . ?
C13 H13B 0.976(11) . ?
C13 H13C 0.972(13) . ?
C14 C15 1.536(13) . ?
C14 C16 1.505(12) . ?
C14 C17 1.538(11) . ?
C15 H15A 0.968(12) . ?
C15 H15B 0.987(12) . ?
C15 H15C 0.983(9) . ?
C16 H16A 0.983(12) . ?
C16 H16B 0.970(11) . ?
C16 H16C 0.983(9) . ?
C17 H17A 0.978(10) . ?
C17 H17B 0.978(11) . ?
C17 H17C 0.993(11) . ?
C18 H18A 0.983(8) . ?
C18 H18B 0.985(10) . ?
C18 H18C 0.979(8) . ?
C19 H19A 0.985(9) . ?
C19 H19B 0.980(8) . ?
C19 H19C 0.976(8) . ?
N1 C20 1.358(9) . ?
N1 C24 1.348(9) . ?
C20 H20 0.949(7) . ?
C20 C21 1.369(10) . ?
C21 H21 0.958(7) . ?
C21 C22 1.422(10) . ?
C22 C23 1.411(10) . ?
C22 N2 1.342(9) . ?
C23 H23 0.954(7) . ?
C23 C24 1.364(10) . ?
C24 H24 0.958(7) . ?
N2 C25 1.455(10) . ?
N2 C26 1.456(10) . ?
C25 H25A 0.974(9) . ?
C25 H25B 0.986(8) . ?
C25 H25C 0.983(9) . ?
C26 H26A 0.991(8) . ?
C26 H26B 0.983(7) . ?
C26 H26C 0.973(8) . ?
C27 H27A 0.980(14) 7_565 ?
C27 H27A 0.980(14) . ?
C27 H27B 0.979(12) . ?
C27 H27B 0.979(12) 7_565 ?
C27 H27C 0.981(7) . ?
C27 H27C 0.981(7) 7_565 ?
C27 C28 1.529(17) . ?
C28 C29 1.399(16) . ?
C28 C33 1.372(17) . ?
C29 H29 0.940(11) . ?
C29 C30 1.379(17) . ?
C30 H30 0.950(13) . ?
C30 C31 1.37(2) . ?
C31 H31 0.949(12) . ?
C31 C32 1.374(19) . ?
C32 H32 0.943(13) . ?
C32 C33 1.394(17) . ?
C33 H33 0.950(12) . ?
C34 H34A 0.992(13) . ?
C34 H34B 0.95(2) . ?
C34 H34C 0.994(13) . ?
C34 C35 1.50(2) . ?
C35 C36 1.374(13) 7 ?
C35 C36 1.374(13) . ?
C36 H36 0.937(10) . ?
C36 C37 1.402(17) . ?
C37 H37 0.942(11) . ?
C37 C38 1.337(16) . ?
C38 H38 0.956(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Si2 W1 Si1 123.36(7) . . ?
C1 W1 Si1 73.0(2) . . ?
C1 W1 Si2 71.2(2) . . ?
C1 W1 C3 100.5(3) . . ?
C1 W1 C4 99.4(3) . . ?
C1 W1 C5 128.4(3) . . ?
C1 W1 C6 156.9(3) . . ?
C1 W1 C7 130.4(3) . . ?
C2 W1 Si1 74.1(2) . . ?
C2 W1 Si2 78.6(2) . . ?
C2 W1 C1 109.8(3) . . ?
C2 W1 C3 142.9(3) . . ?
C2 W1 C4 147.9(3) . . ?
C2 W1 C5 112.9(3) . . ?
C2 W1 C6 93.4(3) . . ?
C2 W1 C7 107.9(3) . . ?
C3 W1 Si1 95.48(19) . . ?
C3 W1 Si2 133.0(2) . . ?
C3 W1 C5 58.2(2) . . ?
C3 W1 C6 58.3(2) . . ?
C3 W1 C7 35.2(3) . . ?
C4 W1 Si1 128.93(19) . . ?
C4 W1 Si2 99.22(19) . . ?
C4 W1 C3 34.9(3) . . ?
C4 W1 C5 35.1(2) . . ?
C4 W1 C6 58.2(2) . . ?
C4 W1 C7 58.5(3) . . ?
C5 W1 Si1 146.18(19) . . ?
C5 W1 Si2 90.19(19) . . ?
C6 W1 Si1 114.98(19) . . ?
C6 W1 Si2 115.29(19) . . ?
C6 W1 C5 34.9(3) . . ?
C6 W1 C7 35.2(3) . . ?
C7 W1 Si1 87.7(2) . . ?
C7 W1 Si2 148.3(2) . . ?
C7 W1 C5 58.5(3) . . ?
W1 Si1 H1 110(4) . . ?
C13 Si1 W1 113.2(3) . . ?
C13 Si1 H1 107(4) . . ?
C13 Si1 C14 103.4(4) . . ?
C14 Si1 W1 124.3(3) . . ?
C14 Si1 H1 97(4) . . ?
C18 Si2 W1 117.7(3) . . ?
C18 Si2 N1 99.3(3) . . ?
C19 Si2 W1 118.4(3) . . ?
C19 Si2 C18 103.4(4) . . ?
C19 Si2 N1 98.2(3) . . ?
N1 Si2 W1 116.44(19) . . ?
O1 C1 W1 173.5(6) . . ?
O2 C2 W1 172.6(6) . . ?
C4 C3 W1 72.2(4) . . ?
C4 C3 C7 108.5(6) . . ?
C4 C3 C8 123.2(8) . . ?
C7 C3 W1 72.8(4) . . ?
C7 C3 C8 127.5(8) . . ?
C8 C3 W1 128.8(5) . . ?
C3 C4 W1 72.9(4) . . ?
C3 C4 C5 108.4(6) . . ?
C3 C4 C9 124.9(7) . . ?
C5 C4 W1 73.2(4) . . ?
C5 C4 C9 126.2(7) . . ?
C9 C4 W1 126.2(5) . . ?
C4 C5 W1 71.7(4) . . ?
C4 C5 C10 125.7(7) . . ?
C6 C5 W1 72.4(4) . . ?
C6 C5 C4 107.7(6) . . ?
C6 C5 C10 125.8(7) . . ?
C10 C5 W1 129.7(5) . . ?
C5 C6 W1 72.7(4) . . ?
C5 C6 C7 108.5(6) . . ?
C5 C6 C11 125.8(7) . . ?
C7 C6 W1 72.5(4) . . ?
C7 C6 C11 125.4(7) . . ?
C11 C6 W1 125.3(5) . . ?
C3 C7 W1 72.0(4) . . ?
C3 C7 C6 106.9(7) . . ?
C3 C7 C12 126.0(7) . . ?
C6 C7 W1 72.3(4) . . ?
C6 C7 C12 126.5(7) . . ?
C12 C7 W1 127.7(5) . . ?
C3 C8 H8A 110.1(7) . . ?
C3 C8 H8B 109.4(9) . . ?
C3 C8 H8C 109.5(8) . . ?
H8A C8 H8B 109.3(9) . . ?
H8A C8 H8C 109.5(10) . . ?
H8B C8 H8C 109.1(8) . . ?
C4 C9 H9A 109.4(8) . . ?
C4 C9 H9B 109.7(8) . . ?
C4 C9 H9C 109.9(8) . . ?
H9A C9 H9B 108.7(9) . . ?
H9A C9 H9C 109.6(9) . . ?
H9B C9 H9C 109.6(9) . . ?
C5 C10 H10A 108.7(7) . . ?
C5 C10 H10B 109.5(8) . . ?
C5 C10 H10C 109.7(7) . . ?
H10A C10 H10B 109.5(8) . . ?
H10A C10 H10C 109.2(9) . . ?
H10B C10 H10C 110.2(9) . . ?
C6 C11 H11A 110.0(8) . . ?
C6 C11 H11B 109.4(7) . . ?
C6 C11 H11C 109.1(7) . . ?
H11A C11 H11B 109.7(8) . . ?
H11A C11 H11C 109.1(8) . . ?
H11B C11 H11C 109.6(9) . . ?
C7 C12 H12A 109.7(8) . . ?
C7 C12 H12B 110.0(8) . . ?
C7 C12 H12C 110.7(8) . . ?
H12A C12 H12B 108.4(9) . . ?
H12A C12 H12C 108.9(9) . . ?
H12B C12 H12C 109.2(9) . . ?
Si1 C13 H13A 108.8(8) . . ?
Si1 C13 H13B 109.8(8) . . ?
Si1 C13 H13C 110.1(7) . . ?
H13A C13 H13B 108.7(10) . . ?
H13A C13 H13C 109.0(10) . . ?
H13B C13 H13C 110.4(11) . . ?
C15 C14 Si1 110.9(5) . . ?
C15 C14 C17 106.4(8) . . ?
C16 C14 Si1 112.4(6) . . ?
C16 C14 C15 109.9(8) . . ?
C16 C14 C17 108.7(7) . . ?
C17 C14 Si1 108.3(6) . . ?
C14 C15 H15A 109.8(10) . . ?
C14 C15 H15B 108.9(9) . . ?
C14 C15 H15C 109.2(8) . . ?
H15A C15 H15B 109.9(9) . . ?
H15A C15 H15C 110.2(10) . . ?
H15B C15 H15C 108.8(11) . . ?
C14 C16 H16A 109.1(9) . . ?
C14 C16 H16B 109.4(9) . . ?
C14 C16 H16C 108.9(8) . . ?
H16A C16 H16B 110.2(9) . . ?
H16A C16 H16C 109.0(10) . . ?
H16B C16 H16C 110.1(11) . . ?
C14 C17 H17A 110.1(9) . . ?
C14 C17 H17B 110.3(8) . . ?
C14 C17 H17C 109.5(9) . . ?
H17A C17 H17B 109.7(10) . . ?
H17A C17 H17C 108.7(9) . . ?
H17B C17 H17C 108.5(10) . . ?
Si2 C18 H18A 109.8(6) . . ?
Si2 C18 H18B 109.6(6) . . ?
Si2 C18 H18C 110.0(7) . . ?
H18A C18 H18B 108.8(8) . . ?
H18A C18 H18C 109.4(8) . . ?
H18B C18 H18C 109.3(8) . . ?
Si2 C19 H19A 109.4(6) . . ?
Si2 C19 H19B 109.6(6) . . ?
Si2 C19 H19C 109.8(7) . . ?
H19A C19 H19B 109.0(9) . . ?
H19A C19 H19C 109.3(8) . . ?
H19B C19 H19C 109.8(8) . . ?
C20 N1 Si2 123.2(5) . . ?
C24 N1 Si2 120.9(5) . . ?
C24 N1 C20 115.8(6) . . ?
N1 C20 H20 118.1(7) . . ?
N1 C20 C21 124.3(7) . . ?
C21 C20 H20 117.5(7) . . ?
C20 C21 H21 119.8(7) . . ?
C20 C21 C22 119.8(7) . . ?
C22 C21 H21 120.4(7) . . ?
C23 C22 C21 115.2(6) . . ?
N2 C22 C21 122.2(6) . . ?
N2 C22 C23 122.6(7) . . ?
C22 C23 H23 119.7(7) . . ?
C24 C23 C22 120.8(6) . . ?
C24 C23 H23 119.5(7) . . ?
N1 C24 C23 124.0(6) . . ?
N1 C24 H24 118.2(6) . . ?
C23 C24 H24 117.8(7) . . ?
C22 N2 C25 120.3(6) . . ?
C22 N2 C26 121.4(6) . . ?
C25 N2 C26 118.2(6) . . ?
N2 C25 H25A 110.0(7) . . ?
N2 C25 H25B 109.2(8) . . ?
N2 C25 H25C 109.6(7) . . ?
H25A C25 H25B 109.5(8) . . ?
H25A C25 H25C 109.8(9) . . ?
H25B C25 H25C 108.7(8) . . ?
N2 C26 H26A 109.2(7) . . ?
N2 C26 H26B 109.7(7) . . ?
N2 C26 H26C 110.4(7) . . ?
H26A C26 H26B 108.4(7) . . ?
H26A C26 H26C 109.2(8) . . ?
H26B C26 H26C 109.9(7) . . ?
H27A C27 H27A 26.8(4) . 7_565 ?
H27A C27 H27B 109.5(8) 7_565 7_565 ?
H27A C27 H27B 109.5(8) . . ?
H27A C27 H27B 130.2(12) . 7_565 ?
H27A C27 H27C 109.4(11) 7_565 7_565 ?
H27A C27 H27C 109.4(11) . . ?
H27A C27 H27C 84.9(7) . 7_565 ?
H27B C27 H27A 130.2(12) . 7_565 ?
H27B C27 H27B 84.8(13) . 7_565 ?
H27B C27 H27C 109.4(15) . . ?
H27B C27 H27C 26.9(3) . 7_565 ?
H27B C27 H27C 109.4(15) 7_565 7_565 ?
H27C C27 H27A 84.9(7) . 7_565 ?
H27C C27 H27B 26.9(3) . 7_565 ?
H27C C27 H27C 130.2(17) . 7_565 ?
C28 C27 H27A 109.6(13) . 7_565 ?
C28 C27 H27A 109.6(13) . . ?
C28 C27 H27B 109.5(10) . . ?
C28 C27 H27B 109.5(10) . 7_565 ?
C28 C27 H27C 109.5(8) . . ?
C28 C27 H27C 109.5(8) . 7_565 ?
C29 C28 C27 116.8(11) . . ?
C33 C28 C27 122.7(11) . . ?
C33 C28 C29 120.5(10) . . ?
C28 C29 H29 120.0(12) . . ?
C30 C29 C28 119.2(11) . . ?
C30 C29 H29 120.8(13) . . ?
C29 C30 H30 118.8(15) . . ?
C31 C30 C29 120.8(12) . . ?
C31 C30 H30 120.4(13) . . ?
C30 C31 H31 119.8(14) . . ?
C30 C31 C32 119.5(11) . . ?
C32 C31 H31 120.6(14) . . ?
C31 C32 H32 120.1(13) . . ?
C31 C32 C33 121.0(12) . . ?
C33 C32 H32 118.9(14) . . ?
C28 C33 C32 118.9(11) . . ?
C28 C33 H33 120.3(12) . . ?
C32 C33 H33 120.8(13) . . ?
H34A C34 H34B 111.3(13) . . ?
H34A C34 H34C 107(2) . . ?
H34B C34 H34C 111.2(14) . . ?
C35 C34 H34A 107.9(13) . . ?
C35 C34 H34B 110.9(18) . . ?
C35 C34 H34C 108.0(13) . . ?
C36 C35 C34 120.9(7) 7 . ?
C36 C35 C34 120.9(7) . . ?
C36 C35 C36 118.1(14) 7 . ?
C35 C36 H36 120.9(12) . . ?
C35 C36 C37 120.2(10) . . ?
C37 C36 H36 119.0(12) . . ?
C36 C37 H37 121.1(15) . . ?
C38 C37 C36 120.5(12) . . ?
C38 C37 H37 118.4(14) . . ?
C37 C38 C37 120.4(17) 7 . ?
C37 C38 H38 119.8(9) . . ?
C37 C38 H38 119.8(9) 7 . ?

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
W1 C3 C4 C5 65.1(5) . . . . ?
W1 C3 C4 C9 -122.5(7) . . . . ?
W1 C3 C7 C6 -64.4(5) . . . . ?
W1 C3 C7 C12 124.0(7) . . . . ?
W1 C4 C5 C6 63.9(4) . . . . ?
W1 C4 C5 C10 -126.3(7) . . . . ?
W1 C5 C6 C7 64.1(5) . . . . ?
W1 C5 C6 C11 -121.4(7) . . . . ?
W1 C6 C7 C3 64.2(5) . . . . ?
W1 C6 C7 C12 -124.3(7) . . . . ?
Si2 N1 C20 C21 175.4(6) . . . . ?
Si2 N1 C24 C23 -177.3(6) . . . . ?
C3 C4 C5 W1 -64.9(5) . . . . ?
C3 C4 C5 C6 -1.0(7) . . . . ?
C3 C4 C5 C10 168.8(7) . . . . ?
C4 C3 C7 W1 63.9(5) . . . . ?
C4 C3 C7 C6 -0.5(7) . . . . ?
C4 C3 C7 C12 -172.1(7) . . . . ?
C4 C5 C6 W1 -63.4(4) . . . . ?
C4 C5 C6 C7 0.7(7) . . . . ?
C4 C5 C6 C11 175.2(6) . . . . ?
C5 C6 C7 W1 -64.3(5) . . . . ?
C5 C6 C7 C3 -0.1(7) . . . . ?
C5 C6 C7 C12 171.4(7) . . . . ?
C7 C3 C4 W1 -64.2(5) . . . . ?
C7 C3 C4 C5 0.9(8) . . . . ?
C7 C3 C4 C9 173.3(7) . . . . ?
C8 C3 C4 W1 125.3(7) . . . . ?
C8 C3 C4 C5 -169.6(7) . . . . ?
C8 C3 C4 C9 2.7(11) . . . . ?
C8 C3 C7 W1 -126.1(7) . . . . ?
C8 C3 C7 C6 169.5(7) . . . . ?
C8 C3 C7 C12 -2.1(12) . . . . ?
C9 C4 C5 W1 122.9(7) . . . . ?
C9 C4 C5 C6 -173.2(7) . . . . ?
C9 C4 C5 C10 -3.4(11) . . . . ?
C10 C5 C6 W1 126.7(7) . . . . ?
C10 C5 C6 C7 -169.1(7) . . . . ?
C10 C5 C6 C11 5.3(11) . . . . ?
C11 C6 C7 W1 121.2(7) . . . . ?
C11 C6 C7 C3 -174.6(6) . . . . ?
C11 C6 C7 C12 -3.1(11) . . . . ?
N1 C20 C21 C22 1.2(12) . . . . ?
C20 N1 C24 C23 -1.5(11) . . . . ?
C20 C21 C22 C23 -0.1(10) . . . . ?
C20 C21 C22 N2 179.9(7) . . . . ?
C21 C22 C23 C24 -1.6(11) . . . . ?
C21 C22 N2 C25 3.4(10) . . . . ?
C21 C22 N2 C26 179.0(7) . . . . ?
C22 C23 C24 N1 2.5(12) . . . . ?
C23 C22 N2 C25 -176.6(7) . . . . ?
C23 C22 N2 C26 -1.0(10) . . . . ?
C24 N1 C20 C21 -0.4(11) . . . . ?
N2 C22 C23 C24 178.4(7) . . . . ?
C27 C28 C29 C30 180.000(3) . . . . ?
C27 C28 C33 C32 180.000(2) . . . . ?
C28 C29 C30 C31 0.000(4) . . . . ?
C29 C28 C33 C32 0.000(3) . . . . ?
C29 C30 C31 C32 0.000(4) . . . . ?
C30 C31 C32 C33 0.000(3) . . . . ?
C31 C32 C33 C28 0.000(3) . . . . ?
C33 C28 C29 C30 0.000(4) . . . . ?
C34 C35 C36 C37 179.0(14) . . . . ?
C35 C36 C37 C38 0.1(19) . . . . ?
C36 C35 C36 C37 -2.3(19) 7 . . . ?
C36 C37 C38 C37 2(3) . . . 7 ?

_olex2_submission_special_instructions 'No special instructions were received'

