# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_stepheno11a
_database_code_depnum_ccdc_archive 'CCDC 2121166'
loop_
_audit_author_name
_audit_author_address
'David L. Hughes'
;UEA, Norwich, UK
United Kingdom
;
_audit_update_record             
;
2021-11-09 deposited with the CCDC.	2023-04-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        (R)-6d
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_structural     4-MeO-C6H4-cyclo-(CHCH2OC(O)CH2)
_chemical_formula_moiety         'C11 H12 O3'
_chemical_formula_sum            'C11 H12 O3'
_chemical_formula_weight         192.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables 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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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+1/2, -z'

_cell_length_a                   7.0003(5)
_cell_length_b                   7.5875(3)
_cell_length_c                   9.1343(7)
_cell_angle_alpha                90
_cell_angle_beta                 106.874(7)
_cell_angle_gamma                90
_cell_volume                     464.28(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    102(4)
_cell_measurement_reflns_used    6495
_cell_measurement_theta_min      5.0140
_cell_measurement_theta_max      76.0720

_exptl_crystal_colour            colourless
_exptl_crystal_description       plate
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_F_000             204
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.304
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.049
_exptl_absorpt_coefficient_mu    0.822
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.82509
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      100.01(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184

_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_detector_area_resol_mean 10.0000

_diffrn_reflns_number            8875
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_av_R_equivalents  0.0740
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         5.060
_diffrn_reflns_theta_max         67.479
_diffrn_reflns_theta_full        67.479
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             1650
_reflns_number_gt                1630
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.827
_reflns_Friedel_fraction_max     0.976
_reflns_Friedel_fraction_full    0.976

_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       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015b)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976 and Farrugia, 2012)'
_computing_publication_material  
'SHELXL-2018/3 (Sheldrick, 2015b) and WINGX (Farrugia, 2012)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0747P)²+0.0981P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_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 722 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(11)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         1650
_refine_ls_number_parameters     141
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0418
_refine_ls_wR_factor_ref         0.1154
_refine_ls_wR_factor_gt          0.1152
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3440(4) 0.5444(4) 0.3386(3) 0.0320(7) Uani 1 1 d . . . . .
C2 C 0.4485(4) 0.4597(4) 0.4750(3) 0.0293(6) Uani 1 1 d . . . A 1
H2 H 0.561500 0.393792 0.477737 0.035 Uiso 1 1 calc R U . A 1
C3 C 0.3868(4) 0.4722(3) 0.6056(3) 0.0296(6) Uani 1 1 d . . . A 1
H3 H 0.460358 0.418096 0.695751 0.035 Uiso 1 1 calc R U . A 1
C4 C 0.2139(4) 0.5663(3) 0.6016(3) 0.0287(6) Uani 1 1 d . . . A 1
O4 O 0.1632(3) 0.5672(3) 0.7350(2) 0.0383(6) Uani 1 1 d . . . A 1
C41 C -0.0260(5) 0.6387(5) 0.7317(4) 0.0385(8) Uani 1 1 d . . . A 1
H41A H -0.026915 0.762976 0.711647 0.058 Uiso 1 1 calc R U . A 1
H41B H -0.049994 0.619351 0.828723 0.058 Uiso 1 1 calc R U . A 1
H41C H -0.128573 0.582128 0.652567 0.058 Uiso 1 1 calc R U . A 1
C5 C 0.1083(4) 0.6496(3) 0.4674(4) 0.0311(7) Uani 1 1 d . . . A 1
H5 H -0.006903 0.712533 0.464064 0.037 Uiso 1 1 calc R U . A 1
C6 C 0.1741(4) 0.6395(4) 0.3379(4) 0.0331(7) Uani 1 1 d . . . A 1
H6 H 0.103028 0.697486 0.249062 0.040 Uiso 1 1 calc R U . A 1
C7 C 0.4068(4) 0.5363(4) 0.1934(4) 0.0277(8) Uani 0.900(8) 1 d . . P A 1
H7 H 0.345725 0.635013 0.127082 0.033 Uiso 0.900(8) 1 calc R U P A 1
C8 C 0.3460(5) 0.3627(5) 0.1048(4) 0.0302(9) Uani 0.900(8) 1 d . . P A 1
H8A H 0.362864 0.263668 0.174513 0.036 Uiso 0.900(8) 1 calc R U P A 1
H8B H 0.207922 0.367184 0.042368 0.036 Uiso 0.900(8) 1 calc R U P A 1
O9 O 0.4797(3) 0.3476(4) 0.0094(3) 0.0324(7) Uani 0.900(8) 1 d . . P A 1
C10 C 0.6462(4) 0.4459(4) 0.0685(3) 0.0278(6) Uani 1 1 d . . . . .
O10 O 0.7798(3) 0.4477(3) 0.0097(2) 0.0364(5) Uani 1 1 d . . . . .
C11A C 0.6328(4) 0.5347(4) 0.2123(3) 0.0322(6) Uani 0.900(8) 1 d . . P A 1
H11A H 0.685987 0.653477 0.220066 0.039 Uiso 0.900(8) 1 calc R U P A 1
H11B H 0.704453 0.468371 0.302278 0.039 Uiso 0.900(8) 1 calc R U P A 1
C11B C 0.6328(4) 0.5347(4) 0.2123(3) 0.0322(6) Uani 0.100(8) 1 d . . P A 2
H11C H 0.602918 0.659444 0.198409 0.039 Uiso 0.100(8) 1 calc R U P A 2
H11D H 0.750685 0.516221 0.298259 0.039 Uiso 0.100(8) 1 calc R U P A 2
C21 C 0.438(4) 0.416(4) 0.224(3) 0.023(7) Uiso 0.100(8) 1 d . . P A 2
H21 H 0.461460 0.290935 0.251299 0.027 Uiso 0.100(8) 1 calc R U P A 2
C22 C 0.319(4) 0.459(5) 0.062(3) 0.024(7) Uiso 0.100(8) 1 d . . P A 2
H22A H 0.205686 0.380977 0.026897 0.029 Uiso 0.100(8) 1 calc R U P A 2
H22B H 0.272208 0.580184 0.054493 0.029 Uiso 0.100(8) 1 calc R U P A 2
O23 O 0.462(3) 0.433(4) -0.024(2) 0.024(5) Uiso 0.100(8) 1 d . . P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.390(4) . ?
C1 C2 1.404(4) . ?
C1 C7 1.515(4) . ?
C1 C21 1.70(3) . ?
C2 C3 1.385(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.397(4) . ?
C3 H3 0.9300 . ?
C4 O4 1.365(3) . ?
C4 C5 1.386(4) . ?
O4 C41 1.423(3) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C5 C6 1.391(4) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.540(4) . ?
C7 C11A 1.541(4) . ?
C7 H7 0.9800 . ?
C8 O9 1.456(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
O9 C10 1.357(4) . ?
C10 O10 1.206(3) . ?
C10 O23 1.32(2) . ?
C10 C11A 1.503(4) . ?
C10 C11B 1.503(4) . ?
C11A H11A 0.9700 . ?
C11A H11B 0.9700 . ?
C11B C21 1.66(2) . ?
C11B H11C 0.9700 . ?
C11B H11D 0.9700 . ?
C21 C22 1.51(4) . ?
C21 H21 0.9800 . ?
C22 O23 1.46(3) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?

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
C6 C1 C2 117.8(3) . . ?
C6 C1 C7 118.8(3) . . ?
C2 C1 C7 123.4(2) . . ?
C3 C2 C1 121.4(2) . . ?
C3 C2 H2 119.3 . . ?
C1 C2 H2 119.3 . . ?
C2 C3 C4 119.8(3) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
O4 C4 C5 125.2(2) . . ?
O4 C4 C3 115.3(3) . . ?
C5 C4 C3 119.5(3) . . ?
C4 O4 C41 117.7(2) . . ?
O4 C41 H41A 109.5 . . ?
O4 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
O4 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C4 C5 C6 120.2(2) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C1 C6 C5 121.2(3) . . ?
C1 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
C1 C7 C8 112.9(2) . . ?
C1 C7 C11A 116.8(2) . . ?
C8 C7 C11A 99.8(2) . . ?
C1 C7 H7 109.0 . . ?
C8 C7 H7 109.0 . . ?
C11A C7 H7 109.0 . . ?
O9 C8 C7 104.8(2) . . ?
O9 C8 H8A 110.8 . . ?
C7 C8 H8A 110.8 . . ?
O9 C8 H8B 110.8 . . ?
C7 C8 H8B 110.8 . . ?
H8A C8 H8B 108.9 . . ?
C10 O9 C8 110.2(2) . . ?
O10 C10 O23 117.0(9) . . ?
O10 C10 O9 121.1(3) . . ?
O10 C10 C11A 129.6(3) . . ?
O9 C10 C11A 109.2(2) . . ?
O10 C10 C11B 129.6(3) . . ?
O23 C10 C11B 107.2(9) . . ?
C10 C11A C7 103.2(2) . . ?
C10 C11A H11A 111.1 . . ?
C7 C11A H11A 111.1 . . ?
C10 C11A H11B 111.1 . . ?
C7 C11A H11B 111.1 . . ?
H11A C11A H11B 109.1 . . ?
C10 C11B C21 94.2(9) . . ?
C10 C11B H11C 112.9 . . ?
C21 C11B H11C 112.9 . . ?
C10 C11B H11D 112.9 . . ?
C21 C11B H11D 112.9 . . ?
H11C C11B H11D 110.3 . . ?
C22 C21 C11B 92.7(17) . . ?
C22 C21 C1 106(2) . . ?
C11B C21 C1 101.5(14) . . ?
C22 C21 H21 117.6 . . ?
C11B C21 H21 117.6 . . ?
C1 C21 H21 117.6 . . ?
O23 C22 C21 103(2) . . ?
O23 C22 H22A 111.1 . . ?
C21 C22 H22A 111.1 . . ?
O23 C22 H22B 111.1 . . ?
C21 C22 H22B 111.1 . . ?
H22A C22 H22B 109.1 . . ?
C10 O23 C22 109.8(17) . . ?

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
C6 C1 C2 C3 -1.0(4) . . . . ?
C7 C1 C2 C3 179.3(3) . . . . ?
C1 C2 C3 C4 2.0(4) . . . . ?
C2 C3 C4 O4 178.5(2) . . . . ?
C2 C3 C4 C5 -1.5(4) . . . . ?
C5 C4 O4 C41 8.9(4) . . . . ?
C3 C4 O4 C41 -171.1(2) . . . . ?
O4 C4 C5 C6 -179.9(2) . . . . ?
C3 C4 C5 C6 0.0(4) . . . . ?
C2 C1 C6 C5 -0.5(4) . . . . ?
C7 C1 C6 C5 179.2(2) . . . . ?
C4 C5 C6 C1 1.0(4) . . . . ?
C6 C1 C7 C8 -100.6(3) . . . . ?
C2 C1 C7 C8 79.1(3) . . . . ?
C6 C1 C7 C11A 144.5(3) . . . . ?
C2 C1 C7 C11A -35.8(4) . . . . ?
C1 C7 C8 O9 -158.3(2) . . . . ?
C11A C7 C8 O9 -33.6(3) . . . . ?
C7 C8 O9 C10 21.9(3) . . . . ?
C8 O9 C10 O10 177.6(3) . . . . ?
C8 O9 C10 C11A 0.3(4) . . . . ?
O10 C10 C11A C7 160.7(3) . . . . ?
O9 C10 C11A C7 -22.3(3) . . . . ?
C1 C7 C11A C10 155.1(2) . . . . ?
C8 C7 C11A C10 33.1(3) . . . . ?
O10 C10 C11B C21 -165.2(10) . . . . ?
O23 C10 C11B C21 44.2(17) . . . . ?
C10 C11B C21 C22 -52.7(17) . . . . ?
C10 C11B C21 C1 -159.5(10) . . . . ?
C11B C21 C22 O23 46(2) . . . . ?
C1 C21 C22 O23 148.8(18) . . . . ?
O10 C10 O23 C22 -171.5(16) . . . . ?
C11B C10 O23 C22 -17(2) . . . . ?
C21 C22 O23 C10 -22(3) . . . . ?

_refine_diff_density_max         0.206
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.052

####################################################################### 
# 
# 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_stepheno10
_database_code_depnum_ccdc_archive 'CCDC 2121167'
loop_
_audit_author_name
_audit_author_address
'David L. Hughes'
;UEA, Norwich, UK
United Kingdom
;
_audit_update_record             
;
2021-11-09 deposited with the CCDC.	2023-04-20 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_structural     'butyrolactyl-C6H2-3,5-(OMe)2, 4-OSi-Me2,tBu'
_chemical_formula_moiety         'C18 H28 O5 Si'
_chemical_formula_sum            'C18 H28 O5 Si'
_chemical_formula_weight         352.49

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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+1/2, -z'

_cell_length_a                   7.1914(4)
_cell_length_b                   10.5484(5)
_cell_length_c                   24.6032(13)
_cell_angle_alpha                90
_cell_angle_beta                 91.051(4)
_cell_angle_gamma                90
_cell_volume                     1866.03(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.00(11)
_cell_measurement_reflns_used    4489
_cell_measurement_theta_min      2.0900
_cell_measurement_theta_max      30.2930

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_F_000             760
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.185
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.034
_exptl_absorpt_coefficient_mu    0.149
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.78699
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      100.01(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073

_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_detector_area_resol_mean 10.0000

_diffrn_reflns_number            13116
_diffrn_reflns_av_unetI/netI     0.0770
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.101
_diffrn_reflns_theta_max         30.796
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.775
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.775
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.682
_diffrn_reflns_point_group_measured_fraction_full 0.923
_reflns_number_total             7980
_reflns_number_gt                6444
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.677
_reflns_Friedel_fraction_max     0.579
_reflns_Friedel_fraction_full    0.846

_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       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015b)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976 and Farrugia, 2012)'
_computing_publication_material  
'SHELXL-2018/3 (Sheldrick, 2015b) and WINGX (Farrugia, 2012)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0495P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2179 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.24(10)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         7980
_refine_ls_number_parameters     433
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0481
_refine_ls_wR_factor_ref         0.1049
_refine_ls_wR_factor_gt          0.0988
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3482(4) 0.5224(3) 0.59784(13) 0.0133(7) Uani 1 1 d . . . . .
C2 C 0.1655(4) 0.4796(3) 0.59207(13) 0.0139(7) Uani 1 1 d . . . . .
H2 H 0.102789 0.448514 0.621998 0.017 Uiso 1 1 calc R U . . .
C3 C 0.0775(4) 0.4837(3) 0.54124(13) 0.0138(7) Uani 1 1 d . . . . .
C4 C 0.1689(4) 0.5294(3) 0.49594(13) 0.0119(6) Uani 1 1 d . . . . .
C5 C 0.3532(4) 0.5708(3) 0.50190(14) 0.0130(7) Uani 1 1 d . . . . .
C6 C 0.4428(4) 0.5671(3) 0.55281(14) 0.0127(7) Uani 1 1 d . . . . .
H6 H 0.565221 0.594545 0.556592 0.015 Uiso 1 1 calc R U . . .
C7 C 0.4434(4) 0.5246(3) 0.65365(13) 0.0136(7) Uani 1 1 d . . . . .
H7 H 0.570838 0.555787 0.649648 0.016 Uiso 1 1 calc R U . . .
C8 C 0.4508(5) 0.3944(4) 0.68191(14) 0.0204(8) Uani 1 1 d . . . . .
H8A H 0.341908 0.344461 0.672124 0.024 Uiso 1 1 calc R U . . .
H8B H 0.561018 0.348028 0.671468 0.024 Uiso 1 1 calc R U . . .
O9 O 0.4555(3) 0.4206(3) 0.74007(10) 0.0225(6) Uani 1 1 d . . . . .
O10 O 0.3633(3) 0.5744(3) 0.79521(10) 0.0290(7) Uani 1 1 d . . . . .
C10 C 0.3859(4) 0.5372(4) 0.74952(15) 0.0207(8) Uani 1 1 d . . . . .
C11 C 0.3468(5) 0.6049(4) 0.69691(14) 0.0178(7) Uani 1 1 d . . . . .
H11A H 0.397343 0.690128 0.697920 0.021 Uiso 1 1 calc R U . . .
H11B H 0.214071 0.609685 0.689502 0.021 Uiso 1 1 calc R U . . .
O3 O -0.1029(3) 0.4471(2) 0.53205(9) 0.0181(5) Uani 1 1 d . . . . .
C31 C -0.1818(5) 0.3645(4) 0.57119(16) 0.0224(8) Uani 1 1 d . . . . .
H31A H -0.307918 0.345279 0.560680 0.034 Uiso 1 1 calc R U . . .
H31B H -0.110857 0.287526 0.573149 0.034 Uiso 1 1 calc R U . . .
H31C H -0.179923 0.405093 0.606123 0.034 Uiso 1 1 calc R U . . .
O4 O 0.0774(3) 0.5412(2) 0.44675(9) 0.0141(5) Uani 1 1 d . . . . .
Si1 Si 0.02232(12) 0.43005(9) 0.40081(4) 0.0140(2) Uani 1 1 d . . . . .
C41 C -0.2219(5) 0.3771(4) 0.40734(15) 0.0236(8) Uani 1 1 d . . . . .
H41A H -0.249232 0.313445 0.380479 0.035 Uiso 1 1 calc R U . . .
H41B H -0.239260 0.342396 0.442962 0.035 Uiso 1 1 calc R U . . .
H41C H -0.303834 0.448053 0.401973 0.035 Uiso 1 1 calc R U . . .
C42 C 0.1793(5) 0.2914(4) 0.40974(17) 0.0272(9) Uani 1 1 d . . . . .
H42A H 0.147364 0.227709 0.383307 0.041 Uiso 1 1 calc R U . . .
H42B H 0.305757 0.317623 0.404921 0.041 Uiso 1 1 calc R U . . .
H42C H 0.165882 0.257210 0.445621 0.041 Uiso 1 1 calc R U . . .
C43 C 0.0555(5) 0.5110(3) 0.33352(14) 0.0178(7) Uani 1 1 d . . . . .
C44 C 0.0299(5) 0.4155(4) 0.28681(15) 0.0251(8) Uani 1 1 d . . . . .
H44A H 0.118491 0.347983 0.291137 0.038 Uiso 1 1 calc R U . . .
H44B H -0.093791 0.381327 0.287384 0.038 Uiso 1 1 calc R U . . .
H44C H 0.049009 0.457433 0.252743 0.038 Uiso 1 1 calc R U . . .
C45 C 0.2532(5) 0.5677(4) 0.33115(16) 0.0255(9) Uani 1 1 d . . . . .
H45A H 0.270460 0.627546 0.360195 0.038 Uiso 1 1 calc R U . . .
H45B H 0.343312 0.500983 0.334851 0.038 Uiso 1 1 calc R U . . .
H45C H 0.268586 0.609763 0.296927 0.038 Uiso 1 1 calc R U . . .
C46 C -0.0866(5) 0.6191(4) 0.32653(15) 0.0237(8) Uani 1 1 d . . . . .
H46A H -0.070699 0.678868 0.355690 0.036 Uiso 1 1 calc R U . . .
H46B H -0.067445 0.661051 0.292455 0.036 Uiso 1 1 calc R U . . .
H46C H -0.210245 0.584945 0.327097 0.036 Uiso 1 1 calc R U . . .
O5 O 0.4341(3) 0.6119(2) 0.45530(9) 0.0147(5) Uani 1 1 d . . . . .
C51 C 0.6078(4) 0.6775(4) 0.46077(14) 0.0178(7) Uani 1 1 d . . . . .
H51A H 0.650236 0.701424 0.425458 0.027 Uiso 1 1 calc R U . . .
H51B H 0.591482 0.752092 0.482530 0.027 Uiso 1 1 calc R U . . .
H51C H 0.698023 0.622974 0.477999 0.027 Uiso 1 1 calc R U . . .
C101 C 0.8381(4) 0.5511(3) 0.90238(13) 0.0135(7) Uani 1 1 d . . . . .
C102 C 0.6555(4) 0.5095(3) 0.90745(14) 0.0144(7) Uani 1 1 d . . . . .
H102 H 0.590533 0.478312 0.877277 0.017 Uiso 1 1 calc R U . . .
C103 C 0.5703(4) 0.5148(3) 0.95763(13) 0.0127(7) Uani 1 1 d . . . . .
C104 C 0.6651(4) 0.5608(3) 1.00377(13) 0.0120(7) Uani 1 1 d . . . . .
C105 C 0.8494(4) 0.6006(3) 0.99872(14) 0.0129(7) Uani 1 1 d . . . . .
C106 C 0.9350(4) 0.5955(3) 0.94835(14) 0.0129(7) Uani 1 1 d . . . . .
H106 H 1.057734 0.621870 0.945318 0.015 Uiso 1 1 calc R U . . .
C107 C 0.9293(4) 0.5524(3) 0.84736(13) 0.0152(7) Uani 1 1 d . . . . .
H107 H 1.061003 0.574027 0.852584 0.018 Uiso 1 1 calc R U . . .
C108 C 0.8401(5) 0.6498(4) 0.80829(14) 0.0209(8) Uani 1 1 d . . . . .
H10A H 0.708348 0.658361 0.815228 0.025 Uiso 1 1 calc R U . . .
H10B H 0.898701 0.732015 0.812793 0.025 Uiso 1 1 calc R U . . .
O109 O 0.8687(4) 0.6014(3) 0.75350(10) 0.0246(6) Uani 1 1 d . . . . .
C110 C 0.9115(5) 0.4759(4) 0.75555(14) 0.0209(8) Uani 1 1 d . . . . .
O110 O 0.9410(4) 0.4188(3) 0.71449(10) 0.0301(6) Uani 1 1 d . . . . .
C111 C 0.9157(4) 0.4307(4) 0.81343(13) 0.0179(7) Uani 1 1 d . . . . .
H11C H 1.022379 0.376467 0.820369 0.022 Uiso 1 1 calc R U . . .
H11D H 0.803316 0.384190 0.821639 0.022 Uiso 1 1 calc R U . . .
O103 O 0.3898(3) 0.4788(2) 0.96622(9) 0.0178(5) Uani 1 1 d . . . . .
C131 C 0.3084(5) 0.3944(4) 0.92659(15) 0.0210(8) Uani 1 1 d . . . . .
H13A H 0.182906 0.375270 0.936372 0.031 Uiso 1 1 calc R U . . .
H13B H 0.308536 0.434096 0.891483 0.031 Uiso 1 1 calc R U . . .
H13C H 0.379523 0.317435 0.925449 0.031 Uiso 1 1 calc R U . . .
O104 O 0.5774(3) 0.5722(2) 1.05239(9) 0.0125(5) Uani 1 1 d . . . . .
Si2 Si 0.52496(12) 0.45904(9) 1.09719(4) 0.0135(2) Uani 1 1 d . . . . .
C141 C 0.2788(5) 0.4066(4) 1.08900(15) 0.0223(8) Uani 1 1 d . . . . .
H14A H 0.253120 0.341799 1.115215 0.033 Uiso 1 1 calc R U . . .
H14B H 0.197567 0.477435 1.094553 0.033 Uiso 1 1 calc R U . . .
H14C H 0.258923 0.373498 1.053017 0.033 Uiso 1 1 calc R U . . .
C142 C 0.6808(6) 0.3212(4) 1.08726(17) 0.0277(9) Uani 1 1 d . . . . .
H14D H 0.651138 0.255939 1.112906 0.042 Uiso 1 1 calc R U . . .
H14E H 0.664150 0.289102 1.050980 0.042 Uiso 1 1 calc R U . . .
H14F H 0.807707 0.347060 1.092767 0.042 Uiso 1 1 calc R U . . .
C143 C 0.5640(4) 0.5364(4) 1.16549(14) 0.0181(7) Uani 1 1 d . . . . .
C144 C 0.5388(5) 0.4373(4) 1.21053(14) 0.0229(8) Uani 1 1 d . . . . .
H14G H 0.625642 0.369270 1.205678 0.034 Uiso 1 1 calc R U . . .
H14H H 0.560828 0.476156 1.245345 0.034 Uiso 1 1 calc R U . . .
H14I H 0.414326 0.404543 1.208723 0.034 Uiso 1 1 calc R U . . .
C145 C 0.4250(5) 0.6446(4) 1.17351(16) 0.0243(8) Uani 1 1 d . . . . .
H14J H 0.440227 0.706791 1.145441 0.036 Uiso 1 1 calc R U . . .
H14K H 0.300652 0.611624 1.171737 0.036 Uiso 1 1 calc R U . . .
H14L H 0.447154 0.683237 1.208359 0.036 Uiso 1 1 calc R U . . .
C146 C 0.7624(5) 0.5905(4) 1.16924(15) 0.0279(9) Uani 1 1 d . . . . .
H14M H 0.850602 0.523341 1.164265 0.042 Uiso 1 1 calc R U . . .
H14N H 0.777888 0.653348 1.141479 0.042 Uiso 1 1 calc R U . . .
H14O H 0.782538 0.628469 1.204309 0.042 Uiso 1 1 calc R U . . .
O105 O 0.9344(3) 0.6422(2) 1.04554(9) 0.0154(5) Uani 1 1 d . . . . .
C151 C 1.1079(4) 0.7085(4) 1.04010(15) 0.0190(8) Uani 1 1 d . . . . .
H15A H 1.154197 0.732994 1.075412 0.028 Uiso 1 1 calc R U . . .
H15B H 1.196568 0.653953 1.023119 0.028 Uiso 1 1 calc R U . . .
H15C H 1.088832 0.782750 1.018140 0.028 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
C1 C6 1.393(5) . ?
C1 C2 1.394(4) . ?
C1 C7 1.523(4) . ?
C2 C3 1.392(4) . ?
C2 H2 0.9300 . ?
C3 O3 1.368(4) . ?
C3 C4 1.390(5) . ?
C4 O4 1.373(4) . ?
C4 C5 1.401(4) . ?
C5 O5 1.366(4) . ?
C5 C6 1.398(4) . ?
C6 H6 0.9300 . ?
C7 C11 1.536(5) . ?
C7 C8 1.541(5) . ?
C7 H7 0.9800 . ?
C8 O9 1.457(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
O9 C10 1.350(5) . ?
O10 C10 1.205(4) . ?
C10 C11 1.500(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
O3 C31 1.424(4) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
O4 Si1 1.671(2) . ?
Si1 C41 1.853(3) . ?
Si1 C42 1.858(4) . ?
Si1 C43 1.882(4) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 C44 1.537(5) . ?
C43 C46 1.539(5) . ?
C43 C45 1.544(5) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
O5 C51 1.432(4) . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C101 C102 1.393(4) . ?
C101 C106 1.398(5) . ?
C101 C107 1.515(4) . ?
C102 C103 1.389(5) . ?
C102 H102 0.9300 . ?
C103 O103 1.373(4) . ?
C103 C104 1.400(5) . ?
C104 O104 1.368(4) . ?
C104 C105 1.398(4) . ?
C105 O105 1.367(4) . ?
C105 C106 1.395(5) . ?
C106 H106 0.9300 . ?
C107 C111 1.533(5) . ?
C107 C108 1.539(5) . ?
C107 H107 0.9800 . ?
C108 O109 1.460(4) . ?
C108 H10A 0.9700 . ?
C108 H10B 0.9700 . ?
O109 C110 1.360(5) . ?
C110 O110 1.198(4) . ?
C110 C111 1.501(5) . ?
C111 H11C 0.9700 . ?
C111 H11D 0.9700 . ?
O103 C131 1.437(4) . ?
C131 H13A 0.9600 . ?
C131 H13B 0.9600 . ?
C131 H13C 0.9600 . ?
O104 Si2 1.673(2) . ?
Si2 C142 1.855(4) . ?
Si2 C141 1.862(3) . ?
Si2 C143 1.884(4) . ?
C141 H14A 0.9600 . ?
C141 H14B 0.9600 . ?
C141 H14C 0.9600 . ?
C142 H14D 0.9600 . ?
C142 H14E 0.9600 . ?
C142 H14F 0.9600 . ?
C143 C145 1.532(5) . ?
C143 C144 1.536(5) . ?
C143 C146 1.538(5) . ?
C144 H14G 0.9600 . ?
C144 H14H 0.9600 . ?
C144 H14I 0.9600 . ?
C145 H14J 0.9600 . ?
C145 H14K 0.9600 . ?
C145 H14L 0.9600 . ?
C146 H14M 0.9600 . ?
C146 H14N 0.9600 . ?
C146 H14O 0.9600 . ?
O105 C151 1.439(4) . ?
C151 H15A 0.9600 . ?
C151 H15B 0.9600 . ?
C151 H15C 0.9600 . ?

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
C6 C1 C2 120.1(3) . . ?
C6 C1 C7 119.6(3) . . ?
C2 C1 C7 120.3(3) . . ?
C3 C2 C1 119.6(3) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
O3 C3 C4 115.2(3) . . ?
O3 C3 C2 123.6(3) . . ?
C4 C3 C2 121.1(3) . . ?
O4 C4 C3 120.8(3) . . ?
O4 C4 C5 120.1(3) . . ?
C3 C4 C5 119.0(3) . . ?
O5 C5 C6 124.4(3) . . ?
O5 C5 C4 115.3(3) . . ?
C6 C5 C4 120.3(3) . . ?
C1 C6 C5 119.9(3) . . ?
C1 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
C1 C7 C11 115.6(3) . . ?
C1 C7 C8 113.8(3) . . ?
C11 C7 C8 101.0(3) . . ?
C1 C7 H7 108.7 . . ?
C11 C7 H7 108.7 . . ?
C8 C7 H7 108.7 . . ?
O9 C8 C7 105.9(3) . . ?
O9 C8 H8A 110.6 . . ?
C7 C8 H8A 110.6 . . ?
O9 C8 H8B 110.6 . . ?
C7 C8 H8B 110.6 . . ?
H8A C8 H8B 108.7 . . ?
C10 O9 C8 109.9(3) . . ?
O10 C10 O9 121.0(3) . . ?
O10 C10 C11 128.6(4) . . ?
O9 C10 C11 110.4(3) . . ?
C10 C11 C7 104.8(3) . . ?
C10 C11 H11A 110.8 . . ?
C7 C11 H11A 110.8 . . ?
C10 C11 H11B 110.8 . . ?
C7 C11 H11B 110.8 . . ?
H11A C11 H11B 108.9 . . ?
C3 O3 C31 116.7(2) . . ?
O3 C31 H31A 109.5 . . ?
O3 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
O3 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C4 O4 Si1 129.5(2) . . ?
O4 Si1 C41 111.47(15) . . ?
O4 Si1 C42 109.65(15) . . ?
C41 Si1 C42 109.11(19) . . ?
O4 Si1 C43 104.14(14) . . ?
C41 Si1 C43 110.41(16) . . ?
C42 Si1 C43 112.01(18) . . ?
Si1 C41 H41A 109.5 . . ?
Si1 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
Si1 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
Si1 C42 H42A 109.5 . . ?
Si1 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
Si1 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 C43 C46 109.4(3) . . ?
C44 C43 C45 108.9(3) . . ?
C46 C43 C45 108.6(3) . . ?
C44 C43 Si1 110.2(3) . . ?
C46 C43 Si1 109.9(2) . . ?
C45 C43 Si1 109.9(2) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C43 C46 H46A 109.5 . . ?
C43 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C43 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C5 O5 C51 117.3(2) . . ?
O5 C51 H51A 109.5 . . ?
O5 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
O5 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C102 C101 C106 119.3(3) . . ?
C102 C101 C107 120.5(3) . . ?
C106 C101 C107 120.1(3) . . ?
C103 C102 C101 119.9(3) . . ?
C103 C102 H102 120.0 . . ?
C101 C102 H102 120.0 . . ?
O103 C103 C102 124.0(3) . . ?
O103 C103 C104 114.8(3) . . ?
C102 C103 C104 121.2(3) . . ?
O104 C104 C105 120.3(3) . . ?
O104 C104 C103 121.0(3) . . ?
C105 C104 C103 118.7(3) . . ?
O105 C105 C106 124.3(3) . . ?
O105 C105 C104 115.6(3) . . ?
C106 C105 C104 120.1(3) . . ?
C105 C106 C101 120.7(3) . . ?
C105 C106 H106 119.7 . . ?
C101 C106 H106 119.7 . . ?
C101 C107 C111 117.0(3) . . ?
C101 C107 C108 112.5(3) . . ?
C111 C107 C108 101.3(3) . . ?
C101 C107 H107 108.5 . . ?
C111 C107 H107 108.5 . . ?
C108 C107 H107 108.5 . . ?
O109 C108 C107 106.2(3) . . ?
O109 C108 H10A 110.5 . . ?
C107 C108 H10A 110.5 . . ?
O109 C108 H10B 110.5 . . ?
C107 C108 H10B 110.5 . . ?
H10A C108 H10B 108.7 . . ?
C110 O109 C108 110.0(3) . . ?
O110 C110 O109 120.1(3) . . ?
O110 C110 C111 129.8(4) . . ?
O109 C110 C111 110.1(3) . . ?
C110 C111 C107 104.5(3) . . ?
C110 C111 H11C 110.8 . . ?
C107 C111 H11C 110.8 . . ?
C110 C111 H11D 110.8 . . ?
C107 C111 H11D 110.8 . . ?
H11C C111 H11D 108.9 . . ?
C103 O103 C131 116.2(3) . . ?
O103 C131 H13A 109.5 . . ?
O103 C131 H13B 109.5 . . ?
H13A C131 H13B 109.5 . . ?
O103 C131 H13C 109.5 . . ?
H13A C131 H13C 109.5 . . ?
H13B C131 H13C 109.5 . . ?
C104 O104 Si2 128.8(2) . . ?
O104 Si2 C142 109.19(15) . . ?
O104 Si2 C141 111.49(14) . . ?
C142 Si2 C141 109.16(19) . . ?
O104 Si2 C143 104.29(15) . . ?
C142 Si2 C143 112.12(18) . . ?
C141 Si2 C143 110.54(16) . . ?
Si2 C141 H14A 109.5 . . ?
Si2 C141 H14B 109.5 . . ?
H14A C141 H14B 109.5 . . ?
Si2 C141 H14C 109.5 . . ?
H14A C141 H14C 109.5 . . ?
H14B C141 H14C 109.5 . . ?
Si2 C142 H14D 109.5 . . ?
Si2 C142 H14E 109.5 . . ?
H14D C142 H14E 109.5 . . ?
Si2 C142 H14F 109.5 . . ?
H14D C142 H14F 109.5 . . ?
H14E C142 H14F 109.5 . . ?
C145 C143 C144 109.2(3) . . ?
C145 C143 C146 108.8(3) . . ?
C144 C143 C146 109.3(3) . . ?
C145 C143 Si2 110.5(2) . . ?
C144 C143 Si2 109.3(3) . . ?
C146 C143 Si2 109.7(2) . . ?
C143 C144 H14G 109.5 . . ?
C143 C144 H14H 109.5 . . ?
H14G C144 H14H 109.5 . . ?
C143 C144 H14I 109.5 . . ?
H14G C144 H14I 109.5 . . ?
H14H C144 H14I 109.5 . . ?
C143 C145 H14J 109.5 . . ?
C143 C145 H14K 109.5 . . ?
H14J C145 H14K 109.5 . . ?
C143 C145 H14L 109.5 . . ?
H14J C145 H14L 109.5 . . ?
H14K C145 H14L 109.5 . . ?
C143 C146 H14M 109.5 . . ?
C143 C146 H14N 109.5 . . ?
H14M C146 H14N 109.5 . . ?
C143 C146 H14O 109.5 . . ?
H14M C146 H14O 109.5 . . ?
H14N C146 H14O 109.5 . . ?
C105 O105 C151 116.9(3) . . ?
O105 C151 H15A 109.5 . . ?
O105 C151 H15B 109.5 . . ?
H15A C151 H15B 109.5 . . ?
O105 C151 H15C 109.5 . . ?
H15A C151 H15C 109.5 . . ?
H15B C151 H15C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -0.9(5) . . . . ?
C7 C1 C2 C3 177.0(3) . . . . ?
C1 C2 C3 O3 -178.1(3) . . . . ?
C1 C2 C3 C4 0.2(5) . . . . ?
O3 C3 C4 O4 2.9(5) . . . . ?
C2 C3 C4 O4 -175.5(3) . . . . ?
O3 C3 C4 C5 179.0(3) . . . . ?
C2 C3 C4 C5 0.6(5) . . . . ?
O4 C4 C5 O5 -5.1(5) . . . . ?
C3 C4 C5 O5 178.8(3) . . . . ?
O4 C4 C5 C6 175.5(3) . . . . ?
C3 C4 C5 C6 -0.6(5) . . . . ?
C2 C1 C6 C5 0.9(5) . . . . ?
C7 C1 C6 C5 -177.1(3) . . . . ?
O5 C5 C6 C1 -179.4(3) . . . . ?
C4 C5 C6 C1 -0.1(5) . . . . ?
C6 C1 C7 C11 119.4(3) . . . . ?
C2 C1 C7 C11 -58.6(4) . . . . ?
C6 C1 C7 C8 -124.3(3) . . . . ?
C2 C1 C7 C8 57.7(4) . . . . ?
C1 C7 C8 O9 -152.4(3) . . . . ?
C11 C7 C8 O9 -27.9(3) . . . . ?
C7 C8 O9 C10 22.1(3) . . . . ?
C8 O9 C10 O10 174.2(3) . . . . ?
C8 O9 C10 C11 -6.1(4) . . . . ?
O10 C10 C11 C7 167.3(3) . . . . ?
O9 C10 C11 C7 -12.4(4) . . . . ?
C1 C7 C11 C10 147.3(3) . . . . ?
C8 C7 C11 C10 24.0(3) . . . . ?
C4 C3 O3 C31 160.7(3) . . . . ?
C2 C3 O3 C31 -20.9(5) . . . . ?
C3 C4 O4 Si1 -78.1(4) . . . . ?
C5 C4 O4 Si1 105.9(3) . . . . ?
C4 O4 Si1 C41 98.3(3) . . . . ?
C4 O4 Si1 C42 -22.7(3) . . . . ?
C4 O4 Si1 C43 -142.7(3) . . . . ?
O4 Si1 C43 C44 173.9(2) . . . . ?
C41 Si1 C43 C44 -66.3(3) . . . . ?
C42 Si1 C43 C44 55.5(3) . . . . ?
O4 Si1 C43 C46 -65.4(3) . . . . ?
C41 Si1 C43 C46 54.3(3) . . . . ?
C42 Si1 C43 C46 176.1(2) . . . . ?
O4 Si1 C43 C45 54.0(3) . . . . ?
C41 Si1 C43 C45 173.8(3) . . . . ?
C42 Si1 C43 C45 -64.4(3) . . . . ?
C6 C5 O5 C51 -12.4(5) . . . . ?
C4 C5 O5 C51 168.2(3) . . . . ?
C106 C101 C102 C103 1.2(5) . . . . ?
C107 C101 C102 C103 -176.7(3) . . . . ?
C101 C102 C103 O103 178.5(3) . . . . ?
C101 C102 C103 C104 -0.3(5) . . . . ?
O103 C103 C104 O104 -2.5(5) . . . . ?
C102 C103 C104 O104 176.4(3) . . . . ?
O103 C103 C104 C105 -179.6(3) . . . . ?
C102 C103 C104 C105 -0.6(5) . . . . ?
O104 C104 C105 O105 4.0(5) . . . . ?
C103 C104 C105 O105 -178.9(3) . . . . ?
O104 C104 C105 C106 -176.4(3) . . . . ?
C103 C104 C105 C106 0.7(5) . . . . ?
O105 C105 C106 C101 179.8(3) . . . . ?
C104 C105 C106 C101 0.2(5) . . . . ?
C102 C101 C106 C105 -1.1(5) . . . . ?
C107 C101 C106 C105 176.8(3) . . . . ?
C102 C101 C107 C111 -49.8(4) . . . . ?
C106 C101 C107 C111 132.3(3) . . . . ?
C102 C101 C107 C108 67.0(4) . . . . ?
C106 C101 C107 C108 -111.0(4) . . . . ?
C101 C107 C108 O109 -152.3(3) . . . . ?
C111 C107 C108 O109 -26.6(3) . . . . ?
C107 C108 O109 C110 17.7(4) . . . . ?
C108 O109 C110 O110 -179.7(3) . . . . ?
C108 O109 C110 C111 -0.3(4) . . . . ?
O110 C110 C111 C107 162.2(4) . . . . ?
O109 C110 C111 C107 -17.0(4) . . . . ?
C101 C107 C111 C110 148.5(3) . . . . ?
C108 C107 C111 C110 25.8(3) . . . . ?
C102 C103 O103 C131 21.0(5) . . . . ?
C104 C103 O103 C131 -160.1(3) . . . . ?
C105 C104 O104 Si2 -105.7(3) . . . . ?
C103 C104 O104 Si2 77.3(4) . . . . ?
C104 O104 Si2 C142 22.6(3) . . . . ?
C104 O104 Si2 C141 -98.1(3) . . . . ?
C104 O104 Si2 C143 142.6(3) . . . . ?
O104 Si2 C143 C145 65.4(3) . . . . ?
C142 Si2 C143 C145 -176.6(3) . . . . ?
C141 Si2 C143 C145 -54.6(3) . . . . ?
O104 Si2 C143 C144 -174.4(2) . . . . ?
C142 Si2 C143 C144 -56.4(3) . . . . ?
C141 Si2 C143 C144 65.6(3) . . . . ?
O104 Si2 C143 C146 -54.6(3) . . . . ?
C142 Si2 C143 C146 63.4(3) . . . . ?
C141 Si2 C143 C146 -174.5(3) . . . . ?
C106 C105 O105 C151 13.3(5) . . . . ?
C104 C105 O105 C151 -167.1(3) . . . . ?

_refine_diff_density_max         0.321
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.058

