#------------------------------------------------------------------------------
#$Date: 2021-11-19 00:55:54 +0200 (Fri, 19 Nov 2021) $
#$Revision: 270747 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/92/7129269.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7129269
loop_
_publ_author_name
'Yang, Lei'
'Xu, Wen-Qiang'
'Liu, Tao'
'Wu, Yichen'
'Wang, Bi-Qin'
'Wang, Peng'
_publ_section_title
;
 Concise Synthesis and Application of Enantiopure Spirobiphenoxasilin-Diol
 and Its Related Chiral Ligands
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05576C
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_sum            'C24 H20 O6 Si'
_chemical_formula_weight         432.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2021-09-27 deposited with the CCDC.	2021-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.569(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1800(5)
_cell_length_b                   27.5745(18)
_cell_length_c                   9.1884(6)
_cell_measurement_reflns_used    9829
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      53.952
_cell_measurement_theta_min      4.772
_cell_volume                     2163.0(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            26188
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.497
_diffrn_reflns_theta_min         2.216
_exptl_absorpt_coefficient_mu    0.147
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6447
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
; 
 Flack x determined using 2546 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.02(6)
_refine_ls_extinction_coef       0.0055(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         8019
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0615P)²+0.1044P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1259
_reflns_Friedel_coverage         0.957
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                6455
_reflns_number_total             8019
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1cc05576c2.cif
_cod_data_source_block           mo_d8v21603_0m
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7129269
_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. 
;
_shelx_estimated_absorpt_t_min   0.980
_shelx_estimated_absorpt_t_max   0.988
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.8994(2) 0.37802(7) 0.9008(2) 0.0436(4) Uani 1 1 d . . . . .
O1 O 1.1452(7) 0.3138(3) 1.1636(7) 0.0721(18) Uani 1 1 d . . . . .
O2 O 0.6414(8) 0.4308(3) 0.6142(8) 0.084(2) Uani 1 1 d . . . . .
O3 O 0.6660(7) 0.4034(3) 1.0434(8) 0.0757(18) Uani 1 1 d . . . . .
H3 H 0.5965 0.4084 1.0776 0.114 Uiso 1 1 calc R U . . .
O4 O 1.1003(9) 0.4591(2) 1.0658(10) 0.088(2) Uani 1 1 d . . . . .
H4 H 1.1602 0.4810 1.1113 0.132 Uiso 1 1 calc R U . . .
C1 C 1.0896(9) 0.3523(3) 0.9116(9) 0.0457(18) Uani 1 1 d . . . . .
C2 C 1.1497(11) 0.3597(3) 0.7929(11) 0.058(2) Uani 1 1 d . . . . .
H2 H 1.0899 0.3775 0.7054 0.070 Uiso 1 1 calc R U . . .
C3 C 1.2889(12) 0.3423(4) 0.7989(14) 0.072(3) Uani 1 1 d . . . . .
H3A H 1.3231 0.3472 0.7165 0.087 Uiso 1 1 calc R U . . .
C4 C 1.3795(12) 0.3171(4) 0.9312(14) 0.072(3) Uani 1 1 d . . . . .
H4A H 1.4784 0.3062 0.9406 0.086 Uiso 1 1 calc R U . . .
C5 C 1.3258(10) 0.3081(4) 1.0459(11) 0.061(2) Uani 1 1 d . . . . .
H5 H 1.3859 0.2897 1.1317 0.074 Uiso 1 1 calc R U . . .
C6 C 1.1825(9) 0.3259(3) 1.0385(10) 0.0490(18) Uani 1 1 d . . . . .
C7 C 1.0133(9) 0.3297(3) 1.1927(10) 0.0571(19) Uani 1 1 d . . . . .
C8 C 1.0071(13) 0.3133(4) 1.3332(11) 0.074(3) Uani 1 1 d . . . . .
H8 H 1.0855 0.2933 1.3985 0.089 Uiso 1 1 calc R U . . .
C9 C 0.8848(13) 0.3268(5) 1.3739(12) 0.086(3) Uani 1 1 d . . . . .
H9 H 0.8795 0.3152 1.4668 0.104 Uiso 1 1 calc R U . . .
C10 C 0.7677(13) 0.3575(4) 1.2806(13) 0.085(3) Uani 1 1 d . . . . .
H10 H 0.6858 0.3674 1.3103 0.101 Uiso 1 1 calc R U . . .
C11 C 0.7784(10) 0.3722(4) 1.1450(11) 0.062(2) Uani 1 1 d . . . . .
C12 C 0.8987(8) 0.3593(3) 1.0927(9) 0.0480(18) Uani 1 1 d . . . . .
C13 C 0.7313(9) 0.3522(3) 0.7380(8) 0.0462(18) Uani 1 1 d . . . . .
C14 C 0.7006(11) 0.3029(4) 0.7292(12) 0.067(3) Uani 1 1 d . . . . .
H14 H 0.7673 0.2826 0.8056 0.080 Uiso 1 1 calc R U . . .
C15 C 0.5741(11) 0.2828(4) 0.6105(12) 0.078(3) Uani 1 1 d . . . . .
H15 H 0.5575 0.2495 0.6057 0.094 Uiso 1 1 calc R U . . .
C16 C 0.4726(11) 0.3132(5) 0.4990(12) 0.074(3) Uani 1 1 d . . . . .
H16 H 0.3854 0.3004 0.4200 0.089 Uiso 1 1 calc R U . . .
C17 C 0.4999(12) 0.3602(5) 0.5051(12) 0.067(3) Uani 1 1 d . . . . .
H17 H 0.4323 0.3801 0.4279 0.080 Uiso 1 1 calc R U . . .
C18 C 0.6267(8) 0.3811(4) 0.6235(9) 0.059(2) Uani 1 1 d . . . . .
C19 C 0.7540(12) 0.4592(4) 0.7160(13) 0.067(3) Uani 1 1 d . . . . .
C20 C 0.7415(14) 0.5086(4) 0.6745(18) 0.102(4) Uani 1 1 d . . . . .
H20 H 0.6656 0.5190 0.5811 0.123 Uiso 1 1 calc R U . . .
C21 C 0.8440(17) 0.5415(4) 0.775(2) 0.123(6) Uani 1 1 d . . . . .
H21 H 0.8260 0.5745 0.7558 0.148 Uiso 1 1 calc R U . . .
C22 C 0.9693(14) 0.5270(4) 0.8993(19) 0.103(4) Uani 1 1 d . . . . .
H22 H 1.0435 0.5494 0.9577 0.124 Uiso 1 1 calc R U . . .
C23 C 0.9860(10) 0.4771(4) 0.9398(14) 0.078(3) Uani 1 1 d . . . . .
C24 C 0.8766(10) 0.4422(3) 0.8445(11) 0.058(2) Uani 1 1 d . . . . .
Si2 Si 0.2508(2) 0.62452(8) 0.5610(2) 0.0445(5) Uani 1 1 d . . . . .
O5 O 0.5174(7) 0.6887(3) 0.8088(7) 0.073(2) Uani 1 1 d . . . . .
O6 O -0.0284(8) 0.5702(2) 0.2948(8) 0.079(2) Uani 1 1 d . . . . .
O7 O 0.3947(9) 0.6022(3) 0.3265(8) 0.086(2) Uani 1 1 d . . . . .
H7 H 0.3137 0.6172 0.2794 0.128 Uiso 1 1 calc R U . . .
O8 O 0.4149(10) 0.5441(3) 0.7654(8) 0.088(2) Uani 1 1 d . . . . .
H8A H 0.4862 0.5242 0.7942 0.132 Uiso 1 1 calc R U . . .
C25 C 0.2599(9) 0.6501(3) 0.7488(8) 0.0437(17) Uani 1 1 d . . . . .
C26 C 0.1379(10) 0.6427(4) 0.8033(11) 0.061(3) Uani 1 1 d . . . . .
H26 H 0.0503 0.6251 0.7423 0.074 Uiso 1 1 calc R U . . .
C27 C 0.1448(12) 0.6610(4) 0.9463(12) 0.075(3) Uani 1 1 d . . . . .
H27 H 0.0630 0.6551 0.9807 0.090 Uiso 1 1 calc R U . . .
C28 C 0.2709(12) 0.6877(4) 1.0369(11) 0.070(3) Uani 1 1 d . . . . .
H28 H 0.2741 0.7004 1.1318 0.084 Uiso 1 1 calc R U . . .
C29 C 0.3934(12) 0.6956(4) 0.9872(10) 0.065(3) Uani 1 1 d . . . . .
H29 H 0.4804 0.7134 1.0486 0.078 Uiso 1 1 calc R U . . .
C30 C 0.3855(8) 0.6767(3) 0.8430(8) 0.0479(18) Uani 1 1 d . . . . .
C31 C 0.5446(9) 0.6727(4) 0.6812(10) 0.057(2) Uani 1 1 d . . . . .
C32 C 0.6904(11) 0.6900(5) 0.6785(12) 0.076(3) Uani 1 1 d . . . . .
H32 H 0.7569 0.7091 0.7589 0.091 Uiso 1 1 calc R U . . .
C33 C 0.7285(13) 0.6770(5) 0.5514(15) 0.077(3) Uani 1 1 d . . . . .
H33 H 0.8214 0.6886 0.5453 0.093 Uiso 1 1 calc R U . . .
C34 C 0.6332(12) 0.6477(4) 0.4334(13) 0.077(3) Uani 1 1 d . . . . .
H34 H 0.6622 0.6390 0.3500 0.092 Uiso 1 1 calc R U . . .
C35 C 0.4949(11) 0.6313(4) 0.4408(10) 0.060(2) Uani 1 1 d . . . . .
C36 C 0.4437(10) 0.6426(3) 0.5640(10) 0.0497(19) Uani 1 1 d . . . . .
C37 C 0.0870(9) 0.6494(3) 0.3938(10) 0.051(2) Uani 1 1 d . . . . .
C38 C 0.0680(11) 0.6996(4) 0.3692(11) 0.064(3) Uani 1 1 d . . . . .
H38 H 0.1391 0.7204 0.4400 0.077 Uiso 1 1 calc R U . . .
C39 C -0.0519(12) 0.7192(4) 0.2443(12) 0.072(2) Uani 1 1 d . . . . .
H39 H -0.0618 0.7527 0.2317 0.086 Uiso 1 1 calc R U . . .
C40 C -0.1554(11) 0.6892(5) 0.1397(12) 0.075(3) Uani 1 1 d . . . . .
H40 H -0.2347 0.7024 0.0536 0.090 Uiso 1 1 calc R U . . .
C41 C -0.1457(12) 0.6396(4) 0.1584(11) 0.064(3) Uani 1 1 d . . . . .
H41 H -0.2186 0.6192 0.0878 0.076 Uiso 1 1 calc R U . . .
C42 C -0.0223(9) 0.6207(4) 0.2872(9) 0.056(2) Uani 1 1 d . . . . .
C43 C 0.0730(12) 0.5424(3) 0.4157(11) 0.064(2) Uani 1 1 d . . . . .
C44 C 0.0350(16) 0.4921(4) 0.3923(13) 0.090(3) Uani 1 1 d . . . . .
H44 H -0.0493 0.4813 0.3060 0.109 Uiso 1 1 calc R U . . .
C45 C 0.1266(19) 0.4608(5) 0.5007(15) 0.123(6) Uani 1 1 d . . . . .
H45 H 0.1008 0.4281 0.4911 0.148 Uiso 1 1 calc R U . . .
C46 C 0.2622(17) 0.4764(4) 0.6301(13) 0.094(4) Uani 1 1 d . . . . .
H46 H 0.3277 0.4544 0.7012 0.113 Uiso 1 1 calc R U . . .
C47 C 0.2895(14) 0.5250(4) 0.6430(11) 0.071(3) Uani 1 1 d . . . . .
C48 C 0.2010(11) 0.5594(3) 0.5375(9) 0.058(2) Uani 1 1 d . . . . .
O9 O 0.4696(10) 0.5767(2) 0.0839(8) 0.131(4) Uani 1 1 d G . . . .
H9A H 0.5082 0.5483 0.0932 0.196 Uiso 1 1 d G U . . .
H9B H 0.4154 0.5822 -0.0118 0.196 Uiso 1 1 d G U . . .
O10 O 0.4237(8) 0.4268(2) 0.1210(10) 0.125(3) Uani 1 1 d G . . . .
H10A H 0.4531 0.4550 0.1053 0.187 Uiso 1 1 d G U . . .
H10B H 0.3251 0.4267 0.0971 0.187 Uiso 1 1 d G U . . .
O11 O 0.6592(7) 0.5052(2) 0.0185(9) 0.107(2) Uani 1 1 d G . . . .
H11A H 0.6167 0.4774 0.0066 0.161 Uiso 1 1 d G U . . .
H11B H 0.7067 0.5113 0.1150 0.161 Uiso 1 1 d G U . . .
O12 O 0.3506(10) 0.4982(2) 0.3134(9) 0.143(4) Uani 1 1 d G . . . .
H12A H 0.4342 0.4972 0.2941 0.214 Uiso 1 1 d G U . . .
H12B H 0.3696 0.5110 0.4027 0.214 Uiso 1 1 d G U . . .
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'
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
C24 Si1 C12 120.1(4) . . ?
C24 Si1 C13 99.7(4) . . ?
C12 Si1 C13 111.8(3) . . ?
C24 Si1 C1 113.0(4) . . ?
C12 Si1 C1 100.2(3) . . ?
C13 Si1 C1 112.7(3) . . ?
C6 O1 C7 126.1(7) . . ?
C19 O2 C18 126.6(7) . . ?
C11 O3 H3 109.5 . . ?
C23 O4 H4 109.5 . . ?
C6 C1 C2 115.9(8) . . ?
C6 C1 Si1 121.8(6) . . ?
C2 C1 Si1 122.3(7) . . ?
C3 C2 C1 123.7(9) . . ?
C3 C2 H2 118.2 . . ?
C1 C2 H2 118.2 . . ?
C2 C3 C4 118.0(9) . . ?
C2 C3 H3A 121.0 . . ?
C4 C3 H3A 121.0 . . ?
C5 C4 C3 120.5(9) . . ?
C5 C4 H4A 119.7 . . ?
C3 C4 H4A 119.7 . . ?
C4 C5 C6 121.0(9) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
O1 C6 C1 125.4(7) . . ?
O1 C6 C5 113.8(8) . . ?
C1 C6 C5 120.8(8) . . ?
C12 C7 C8 122.0(8) . . ?
C12 C7 O1 123.9(7) . . ?
C8 C7 O1 114.1(8) . . ?
C9 C8 C7 119.1(9) . . ?
C9 C8 H8 120.5 . . ?
C7 C8 H8 120.5 . . ?
C8 C9 C10 121.9(9) . . ?
C8 C9 H9 119.1 . . ?
C10 C9 H9 119.1 . . ?
C11 C10 C9 116.8(9) . . ?
C11 C10 H10 121.6 . . ?
C9 C10 H10 121.6 . . ?
C10 C11 C12 125.0(10) . . ?
C10 C11 O3 120.9(8) . . ?
C12 C11 O3 114.0(8) . . ?
C7 C12 C11 115.2(8) . . ?
C7 C12 Si1 122.2(6) . . ?
C11 C12 Si1 122.5(7) . . ?
C14 C13 C18 116.8(8) . . ?
C14 C13 Si1 121.1(6) . . ?
C18 C13 Si1 122.1(7) . . ?
C15 C14 C13 122.2(10) . . ?
C15 C14 H14 118.9 . . ?
C13 C14 H14 118.9 . . ?
C14 C15 C16 118.9(10) . . ?
C14 C15 H15 120.6 . . ?
C16 C15 H15 120.6 . . ?
C17 C16 C15 119.9(10) . . ?
C17 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
C16 C17 C18 122.0(10) . . ?
C16 C17 H17 119.0 . . ?
C18 C17 H17 119.0 . . ?
O2 C18 C13 124.1(7) . . ?
O2 C18 C17 115.7(8) . . ?
C13 C18 C17 120.2(10) . . ?
O2 C19 C24 124.5(8) . . ?
O2 C19 C20 114.0(10) . . ?
C24 C19 C20 121.4(11) . . ?
C21 C20 C19 119.1(12) . . ?
C21 C20 H20 120.4 . . ?
C19 C20 H20 120.4 . . ?
C22 C21 C20 121.8(10) . . ?
C22 C21 H21 119.1 . . ?
C20 C21 H21 119.1 . . ?
C21 C22 C23 119.0(10) . . ?
C21 C22 H22 120.5 . . ?
C23 C22 H22 120.5 . . ?
O4 C23 C22 124.1(10) . . ?
O4 C23 C24 115.5(8) . . ?
C22 C23 C24 120.5(10) . . ?
C19 C24 C23 117.5(8) . . ?
C19 C24 Si1 122.9(7) . . ?
C23 C24 Si1 119.6(7) . . ?
C36 Si2 C25 99.9(4) . . ?
C36 Si2 C37 113.5(4) . . ?
C25 Si2 C37 112.5(4) . . ?
C36 Si2 C48 117.6(4) . . ?
C25 Si2 C48 114.0(4) . . ?
C37 Si2 C48 100.0(4) . . ?
C31 O5 C30 124.5(6) . . ?
C43 O6 C42 124.3(7) . . ?
C35 O7 H7 109.5 . . ?
C47 O8 H8A 109.5 . . ?
C30 C25 C26 116.7(7) . . ?
C30 C25 Si2 122.4(6) . . ?
C26 C25 Si2 120.9(6) . . ?
C27 C26 C25 121.5(9) . . ?
C27 C26 H26 119.3 . . ?
C25 C26 H26 119.3 . . ?
C28 C27 C26 120.4(8) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C27 C28 C29 119.7(8) . . ?
C27 C28 H28 120.1 . . ?
C29 C28 H28 120.1 . . ?
C28 C29 C30 119.3(8) . . ?
C28 C29 H29 120.4 . . ?
C30 C29 H29 120.4 . . ?
C25 C30 O5 125.6(6) . . ?
C25 C30 C29 122.4(7) . . ?
O5 C30 C29 112.1(7) . . ?
O5 C31 C36 125.1(7) . . ?
O5 C31 C32 112.2(9) . . ?
C36 C31 C32 122.7(9) . . ?
C33 C32 C31 117.3(11) . . ?
C33 C32 H32 121.3 . . ?
C31 C32 H32 121.3 . . ?
C34 C33 C32 122.0(10) . . ?
C34 C33 H33 119.0 . . ?
C32 C33 H33 119.0 . . ?
C35 C34 C33 119.0(9) . . ?
C35 C34 H34 120.5 . . ?
C33 C34 H34 120.5 . . ?
O7 C35 C34 121.8(9) . . ?
O7 C35 C36 114.6(8) . . ?
C34 C35 C36 123.7(9) . . ?
C31 C36 C35 115.2(8) . . ?
C31 C36 Si2 122.3(6) . . ?
C35 C36 Si2 122.2(7) . . ?
C42 C37 C38 116.1(8) . . ?
C42 C37 Si2 122.8(7) . . ?
C38 C37 Si2 121.1(7) . . ?
C39 C38 C37 122.4(10) . . ?
C39 C38 H38 118.8 . . ?
C37 C38 H38 118.8 . . ?
C40 C39 C38 119.3(10) . . ?
C40 C39 H39 120.4 . . ?
C38 C39 H39 120.4 . . ?
C39 C40 C41 121.4(9) . . ?
C39 C40 H40 119.3 . . ?
C41 C40 H40 119.3 . . ?
C40 C41 C42 117.9(9) . . ?
C40 C41 H41 121.1 . . ?
C42 C41 H41 121.1 . . ?
C37 C42 O6 125.0(7) . . ?
C37 C42 C41 122.9(9) . . ?
O6 C42 C41 112.1(8) . . ?
C48 C43 O6 125.7(8) . . ?
C48 C43 C44 122.9(10) . . ?
O6 C43 C44 111.2(9) . . ?
C45 C44 C43 117.3(10) . . ?
C45 C44 H44 121.4 . . ?
C43 C44 H44 121.4 . . ?
C44 C45 C46 122.3(12) . . ?
C44 C45 H45 118.8 . . ?
C46 C45 H45 118.8 . . ?
C47 C46 C45 116.3(12) . . ?
C47 C46 H46 121.9 . . ?
C45 C46 H46 121.9 . . ?
C46 C47 O8 121.2(10) . . ?
C46 C47 C48 124.9(11) . . ?
O8 C47 C48 113.9(9) . . ?
C43 C48 C47 116.2(9) . . ?
C43 C48 Si2 121.9(7) . . ?
C47 C48 Si2 121.9(7) . . ?
H9A O9 H9B 109.5 . . ?
H10A O10 H10B 109.5 . . ?
H11A O11 H11B 110.3 . . ?
H12A O12 H12B 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 C24 1.834(8) . ?
Si1 C12 1.840(8) . ?
Si1 C13 1.851(8) . ?
Si1 C1 1.853(8) . ?
O1 C6 1.356(10) . ?
O1 C7 1.403(9) . ?
O2 C19 1.359(13) . ?
O2 C18 1.382(12) . ?
O3 C11 1.403(12) . ?
O3 H3 0.8200 . ?
O4 C23 1.340(13) . ?
O4 H4 0.8200 . ?
C1 C6 1.373(12) . ?
C1 C2 1.406(11) . ?
C2 C3 1.346(13) . ?
C2 H2 0.9300 . ?
C3 C4 1.382(16) . ?
C3 H3A 0.9300 . ?
C4 C5 1.340(14) . ?
C4 H4A 0.9300 . ?
C5 C6 1.382(11) . ?
C5 H5 0.9300 . ?
C7 C12 1.380(12) . ?
C7 C8 1.388(12) . ?
C8 C9 1.359(14) . ?
C8 H8 0.9300 . ?
C9 C10 1.389(15) . ?
C9 H9 0.9300 . ?
C10 C11 1.348(14) . ?
C10 H10 0.9300 . ?
C11 C12 1.402(11) . ?
C13 C14 1.384(13) . ?
C13 C18 1.386(10) . ?
C14 C15 1.383(13) . ?
C14 H14 0.9300 . ?
C15 C16 1.384(15) . ?
C15 H15 0.9300 . ?
C16 C17 1.319(15) . ?
C16 H16 0.9300 . ?
C17 C18 1.392(15) . ?
C17 H17 0.9300 . ?
C19 C24 1.380(14) . ?
C19 C20 1.406(14) . ?
C20 C21 1.39(2) . ?
C20 H20 0.9300 . ?
C21 C22 1.350(18) . ?
C21 H21 0.9300 . ?
C22 C23 1.421(15) . ?
C22 H22 0.9300 . ?
C23 C24 1.433(14) . ?
Si2 C36 1.831(9) . ?
Si2 C25 1.837(7) . ?
Si2 C37 1.842(8) . ?
Si2 C48 1.846(10) . ?
O5 C31 1.359(10) . ?
O5 C30 1.398(9) . ?
O6 C43 1.388(11) . ?
O6 C42 1.399(12) . ?
O7 C35 1.372(12) . ?
O7 H7 0.8200 . ?
O8 C47 1.384(13) . ?
O8 H8A 0.8200 . ?
C25 C30 1.372(11) . ?
C25 C26 1.400(12) . ?
C26 C27 1.387(13) . ?
C26 H26 0.9300 . ?
C27 C28 1.366(13) . ?
C27 H27 0.9300 . ?
C28 C29 1.379(14) . ?
C28 H28 0.9300 . ?
C29 C30 1.401(11) . ?
C29 H29 0.9300 . ?
C31 C36 1.405(13) . ?
C31 C32 1.429(12) . ?
C32 C33 1.384(15) . ?
C32 H32 0.9300 . ?
C33 C34 1.378(16) . ?
C33 H33 0.9300 . ?
C34 C35 1.373(14) . ?
C34 H34 0.9300 . ?
C35 C36 1.411(12) . ?
C37 C42 1.367(11) . ?
C37 C38 1.404(13) . ?
C38 C39 1.375(13) . ?
C38 H38 0.9300 . ?
C39 C40 1.356(15) . ?
C39 H39 0.9300 . ?
C40 C41 1.378(15) . ?
C40 H40 0.9300 . ?
C41 C42 1.403(14) . ?
C41 H41 0.9300 . ?
C43 C48 1.374(13) . ?
C43 C44 1.425(14) . ?
C44 C45 1.352(19) . ?
C44 H44 0.9300 . ?
C45 C46 1.434(17) . ?
C45 H45 0.9300 . ?
C46 C47 1.361(13) . ?
C46 H46 0.9300 . ?
C47 C48 1.386(13) . ?
O9 H9A 0.8501 . ?
O9 H9B 0.8500 . ?
O10 H10A 0.8502 . ?
O10 H10B 0.8499 . ?
O11 H11A 0.8501 . ?
O11 H11B 0.8489 . ?
O12 H12A 0.8499 . ?
O12 H12B 0.8500 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O11 H11A O3 0.85 2.09 2.815(10) 143.1 1_554
O10 H10B O4 0.85 2.17 2.959(10) 154.8 1_454
O9 H9B O8 0.85 2.30 2.923(10) 130.4 1_554
O9 H9A O11 0.85 2.12 2.836 141.3 .
O8 H8A O11 0.82 2.15 2.78(2) 133.7 1_556
O4 H4 O12 0.82 2.08 2.788(18) 143.8 1_656
O3 H3 O10 0.82 1.84 2.65(3) 169.1 1_556
O3 H3 O10 0.82 1.84 2.65(3) 169.1 1_556
O4 H4 O12 0.82 2.08 2.788(18) 143.8 1_656
O8 H8A O11 0.82 2.15 2.78(2) 133.7 1_556
O9 H9A O11 0.85 2.12 2.836 141.3 .
O9 H9B O8 0.85 2.30 2.923(10) 130.4 1_554
O10 H10B O4 0.85 2.17 2.959(10) 154.8 1_454
O11 H11A O3 0.85 2.09 2.815(10) 143.1 1_554
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
C24 Si1 C1 C6 131.2(7) . . . . ?
C12 Si1 C1 C6 2.2(7) . . . . ?
C13 Si1 C1 C6 -116.7(7) . . . . ?
C24 Si1 C1 C2 -47.0(8) . . . . ?
C12 Si1 C1 C2 -176.1(7) . . . . ?
C13 Si1 C1 C2 65.0(8) . . . . ?
C6 C1 C2 C3 0.2(14) . . . . ?
Si1 C1 C2 C3 178.6(8) . . . . ?
C1 C2 C3 C4 -1.8(16) . . . . ?
C2 C3 C4 C5 3.3(16) . . . . ?
C3 C4 C5 C6 -3.2(16) . . . . ?
C7 O1 C6 C1 -6.4(15) . . . . ?
C7 O1 C6 C5 175.0(8) . . . . ?
C2 C1 C6 O1 -178.4(8) . . . . ?
Si1 C1 C6 O1 3.2(12) . . . . ?
C2 C1 C6 C5 0.0(12) . . . . ?
Si1 C1 C6 C5 -178.3(7) . . . . ?
C4 C5 C6 O1 -179.9(10) . . . . ?
C4 C5 C6 C1 1.5(15) . . . . ?
C6 O1 C7 C12 2.2(14) . . . . ?
C6 O1 C7 C8 -177.5(9) . . . . ?
C12 C7 C8 C9 -0.3(17) . . . . ?
O1 C7 C8 C9 179.5(11) . . . . ?
C7 C8 C9 C10 -1.4(19) . . . . ?
C8 C9 C10 C11 1.9(19) . . . . ?
C9 C10 C11 C12 -0.7(17) . . . . ?
C9 C10 C11 O3 -179.7(10) . . . . ?
C8 C7 C12 C11 1.4(13) . . . . ?
O1 C7 C12 C11 -178.4(8) . . . . ?
C8 C7 C12 Si1 -176.0(8) . . . . ?
O1 C7 C12 Si1 4.3(12) . . . . ?
C10 C11 C12 C7 -0.9(14) . . . . ?
O3 C11 C12 C7 178.2(8) . . . . ?
C10 C11 C12 Si1 176.5(9) . . . . ?
O3 C11 C12 Si1 -4.5(11) . . . . ?
C24 Si1 C12 C7 -130.0(7) . . . . ?
C13 Si1 C12 C7 113.9(7) . . . . ?
C1 Si1 C12 C7 -5.7(8) . . . . ?
C24 Si1 C12 C11 52.9(8) . . . . ?
C13 Si1 C12 C11 -63.3(8) . . . . ?
C1 Si1 C12 C11 177.2(7) . . . . ?
C24 Si1 C13 C14 179.4(7) . . . . ?
C12 Si1 C13 C14 -52.6(8) . . . . ?
C1 Si1 C13 C14 59.3(7) . . . . ?
C24 Si1 C13 C18 -3.4(7) . . . . ?
C12 Si1 C13 C18 124.6(7) . . . . ?
C1 Si1 C13 C18 -123.5(7) . . . . ?
C18 C13 C14 C15 1.4(13) . . . . ?
Si1 C13 C14 C15 178.7(8) . . . . ?
C13 C14 C15 C16 -1.6(15) . . . . ?
C14 C15 C16 C17 1.7(14) . . . . ?
C15 C16 C17 C18 -1.6(14) . . . . ?
C19 O2 C18 C13 -2.6(15) . . . . ?
C19 O2 C18 C17 179.4(9) . . . . ?
C14 C13 C18 O2 -179.1(8) . . . . ?
Si1 C13 C18 O2 3.5(12) . . . . ?
C14 C13 C18 C17 -1.2(11) . . . . ?
Si1 C13 C18 C17 -178.5(6) . . . . ?
C16 C17 C18 O2 179.5(9) . . . . ?
C16 C17 C18 C13 1.4(13) . . . . ?
C18 O2 C19 C24 2.2(16) . . . . ?
C18 O2 C19 C20 178.5(9) . . . . ?
O2 C19 C20 C21 176.0(11) . . . . ?
C24 C19 C20 C21 -7.6(18) . . . . ?
C19 C20 C21 C22 10(2) . . . . ?
C20 C21 C22 C23 -8(2) . . . . ?
C21 C22 C23 O4 -176.0(13) . . . . ?
C21 C22 C23 C24 4(2) . . . . ?
O2 C19 C24 C23 179.7(9) . . . . ?
C20 C19 C24 C23 3.6(15) . . . . ?
O2 C19 C24 Si1 -2.8(14) . . . . ?
C20 C19 C24 Si1 -178.9(8) . . . . ?
O4 C23 C24 C19 178.1(9) . . . . ?
C22 C23 C24 C19 -1.6(15) . . . . ?
O4 C23 C24 Si1 0.4(12) . . . . ?
C22 C23 C24 Si1 -179.2(9) . . . . ?
C12 Si1 C24 C19 -119.2(8) . . . . ?
C13 Si1 C24 C19 3.0(9) . . . . ?
C1 Si1 C24 C19 122.9(8) . . . . ?
C12 Si1 C24 C23 58.3(8) . . . . ?
C13 Si1 C24 C23 -179.5(7) . . . . ?
C1 Si1 C24 C23 -59.6(8) . . . . ?
C36 Si2 C25 C30 3.2(8) . . . . ?
C37 Si2 C25 C30 -117.6(7) . . . . ?
C48 Si2 C25 C30 129.5(7) . . . . ?
C36 Si2 C25 C26 -176.2(7) . . . . ?
C37 Si2 C25 C26 63.1(8) . . . . ?
C48 Si2 C25 C26 -49.9(8) . . . . ?
C30 C25 C26 C27 -0.7(13) . . . . ?
Si2 C25 C26 C27 178.7(8) . . . . ?
C25 C26 C27 C28 1.2(16) . . . . ?
C26 C27 C28 C29 -1.2(16) . . . . ?
C27 C28 C29 C30 0.8(15) . . . . ?
C26 C25 C30 O5 -178.9(8) . . . . ?
Si2 C25 C30 O5 1.7(12) . . . . ?
C26 C25 C30 C29 0.3(12) . . . . ?
Si2 C25 C30 C29 -179.1(6) . . . . ?
C31 O5 C30 C25 -4.8(14) . . . . ?
C31 O5 C30 C29 176.0(8) . . . . ?
C28 C29 C30 C25 -0.3(14) . . . . ?
C28 C29 C30 O5 179.0(9) . . . . ?
C30 O5 C31 C36 1.1(14) . . . . ?
C30 O5 C31 C32 -178.6(8) . . . . ?
O5 C31 C32 C33 -178.3(9) . . . . ?
C36 C31 C32 C33 2.0(16) . . . . ?
C31 C32 C33 C34 -1.8(17) . . . . ?
C32 C33 C34 C35 1.1(17) . . . . ?
C33 C34 C35 O7 179.6(9) . . . . ?
C33 C34 C35 C36 -0.4(15) . . . . ?
O5 C31 C36 C35 178.9(8) . . . . ?
C32 C31 C36 C35 -1.4(13) . . . . ?
O5 C31 C36 Si2 5.0(12) . . . . ?
C32 C31 C36 Si2 -175.3(8) . . . . ?
O7 C35 C36 C31 -179.5(8) . . . . ?
C34 C35 C36 C31 0.5(13) . . . . ?
O7 C35 C36 Si2 -5.5(10) . . . . ?
C34 C35 C36 Si2 174.5(8) . . . . ?
C25 Si2 C36 C31 -6.2(7) . . . . ?
C37 Si2 C36 C31 113.7(7) . . . . ?
C48 Si2 C36 C31 -130.1(7) . . . . ?
C25 Si2 C36 C35 -179.8(7) . . . . ?
C37 Si2 C36 C35 -59.8(8) . . . . ?
C48 Si2 C36 C35 56.4(8) . . . . ?
C36 Si2 C37 C42 121.6(7) . . . . ?
C25 Si2 C37 C42 -126.0(7) . . . . ?
C48 Si2 C37 C42 -4.6(8) . . . . ?
C36 Si2 C37 C38 -58.4(8) . . . . ?
C25 Si2 C37 C38 54.1(8) . . . . ?
C48 Si2 C37 C38 175.4(7) . . . . ?
C42 C37 C38 C39 -0.9(14) . . . . ?
Si2 C37 C38 C39 179.1(8) . . . . ?
C37 C38 C39 C40 -0.5(15) . . . . ?
C38 C39 C40 C41 1.9(14) . . . . ?
C39 C40 C41 C42 -1.7(14) . . . . ?
C38 C37 C42 O6 -176.9(8) . . . . ?
Si2 C37 C42 O6 3.1(12) . . . . ?
C38 C37 C42 C41 1.0(13) . . . . ?
Si2 C37 C42 C41 -178.9(7) . . . . ?
C43 O6 C42 C37 2.5(14) . . . . ?
C43 O6 C42 C41 -175.6(8) . . . . ?
C40 C41 C42 C37 0.2(14) . . . . ?
C40 C41 C42 O6 178.4(7) . . . . ?
C42 O6 C43 C48 -5.8(15) . . . . ?
C42 O6 C43 C44 178.6(9) . . . . ?
C48 C43 C44 C45 3.2(18) . . . . ?
O6 C43 C44 C45 179.0(12) . . . . ?
C43 C44 C45 C46 -3(2) . . . . ?
C44 C45 C46 C47 3(2) . . . . ?
C45 C46 C47 O8 178.5(12) . . . . ?
C45 C46 C47 C48 -3.1(17) . . . . ?
O6 C43 C48 C47 -177.9(10) . . . . ?
C44 C43 C48 C47 -2.8(14) . . . . ?
O6 C43 C48 Si2 2.8(14) . . . . ?
C44 C43 C48 Si2 177.9(8) . . . . ?
C46 C47 C48 C43 2.9(14) . . . . ?
O8 C47 C48 C43 -178.6(9) . . . . ?
C46 C47 C48 Si2 -177.9(9) . . . . ?
O8 C47 C48 Si2 0.7(12) . . . . ?
C36 Si2 C48 C43 -121.5(8) . . . . ?
C25 Si2 C48 C43 122.0(8) . . . . ?
C37 Si2 C48 C43 1.8(9) . . . . ?
C36 Si2 C48 C47 59.3(9) . . . . ?
C25 Si2 C48 C47 -57.1(9) . . . . ?
C37 Si2 C48 C47 -177.3(8) . . . . ?
