# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2018

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

data_jh54
_database_code_depnum_ccdc_archive 'CCDC 1402159'
_audit_update_record             
;
2015-05-21 deposited with the CCDC.
2018-03-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H11 N3 O'
_chemical_formula_sum            'C7 H11 N3 O'
_chemical_formula_weight         153.19

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   5.5524(17)
_cell_length_b                   7.337(2)
_cell_length_c                   9.871(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.581(7)
_cell_angle_gamma                90.00
_cell_volume                     402.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.06
_cell_measurement_theta_max      24.99

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             164
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'bruker smart apex II cCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4269
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0986
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.06
_diffrn_reflns_theta_max         24.99
_reflns_number_total             1395
_reflns_number_gt                1237
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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 > 2σ(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     
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0616P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(3)
_refine_ls_number_reflns         1395
_refine_ls_number_parameters     102
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0359
_refine_ls_wR_factor_ref         0.1336
_refine_ls_wR_factor_gt          0.1198
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 1.1732(4) 0.5349(3) 0.8094(2) 0.0625(6) Uani 1 1 d . . .
H1 H 1.2239 0.4300 0.8073 0.094 Uiso 1 1 d R . .
N1 N 0.5640(3) 0.9507(3) 0.7329(2) 0.0435(5) Uani 1 1 d . . .
N2 N 0.3871(4) 1.0701(3) 0.7066(2) 0.0561(7) Uani 1 1 d . . .
N3 N 0.4014(5) 1.1878(4) 0.8088(3) 0.0620(7) Uani 1 1 d . . .
C1 C 0.5853(5) 1.1416(4) 0.8954(3) 0.0540(7) Uani 1 1 d . . .
H1A H 0.6309 1.2035 0.9742 0.065 Uiso 1 1 calc R . .
C2 C 0.6918(4) 0.9882(3) 0.8467(2) 0.0424(6) Uani 1 1 d . . .
C3 C 0.8864(5) 0.8479(4) 0.8680(2) 0.0460(6) Uani 1 1 d . . .
H3A H 0.8509 0.7676 0.9429 0.055 Uiso 1 1 calc R . .
H3B H 1.0420 0.9048 0.8850 0.055 Uiso 1 1 calc R . .
C4 C 0.8800(4) 0.7433(3) 0.7314(2) 0.0408(6) Uani 1 1 d . . .
H4 H 1.0024 0.7972 0.6740 0.049 Uiso 1 1 calc R . .
C5 C 0.6316(4) 0.7818(4) 0.6639(3) 0.0488(7) Uani 1 1 d . . .
H5A H 0.6433 0.7998 0.5669 0.059 Uiso 1 1 calc R . .
H5B H 0.5183 0.6843 0.6808 0.059 Uiso 1 1 calc R . .
C6 C 0.9386(5) 0.5414(4) 0.7476(3) 0.0470(6) Uani 1 1 d . . .
H6 H 0.8237 0.4865 0.8092 0.056 Uiso 1 1 calc R . .
C7 C 0.9288(7) 0.4385(5) 0.6145(3) 0.0812(11) Uani 1 1 d . . .
H7A H 0.9759 0.3141 0.6299 0.122 Uiso 1 1 calc R . .
H7B H 1.0368 0.4941 0.5524 0.122 Uiso 1 1 calc R . .
H7C H 0.7677 0.4419 0.5768 0.122 Uiso 1 1 calc R . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
O1 C6 1.424(3) . ?
O1 H1 0.8200 . ?
N1 N2 1.336(3) . ?
N1 C2 1.340(3) . ?
N1 C5 1.469(3) . ?
N2 N3 1.328(4) . ?
N3 C1 1.357(3) . ?
C1 C2 1.365(4) . ?
C1 H1A 0.9300 . ?
C2 C3 1.503(3) . ?
C3 C4 1.551(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C6 1.524(4) . ?
C4 C5 1.541(3) . ?
C4 H4 0.9800 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.516(4) . ?
C6 H6 0.9800 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 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 O1 H1 109.4 . . ?
N2 N1 C2 113.4(2) . . ?
N2 N1 C5 131.2(2) . . ?
C2 N1 C5 115.22(18) . . ?
N3 N2 N1 104.5(2) . . ?
N2 N3 C1 110.1(2) . . ?
N3 C1 C2 108.1(2) . . ?
N3 C1 H1A 126.0 . . ?
C2 C1 H1A 126.0 . . ?
N1 C2 C1 103.9(2) . . ?
N1 C2 C3 109.8(2) . . ?
C1 C2 C3 146.3(2) . . ?
C2 C3 C4 102.59(18) . . ?
C2 C3 H3A 111.2 . . ?
C4 C3 H3A 111.2 . . ?
C2 C3 H3B 111.2 . . ?
C4 C3 H3B 111.2 . . ?
H3A C3 H3B 109.2 . . ?
C6 C4 C5 114.2(2) . . ?
C6 C4 C3 112.9(2) . . ?
C5 C4 C3 106.52(19) . . ?
C6 C4 H4 107.7 . . ?
C5 C4 H4 107.7 . . ?
C3 C4 H4 107.7 . . ?
N1 C5 C4 100.99(19) . . ?
N1 C5 H5A 111.6 . . ?
C4 C5 H5A 111.6 . . ?
N1 C5 H5B 111.6 . . ?
C4 C5 H5B 111.6 . . ?
H5A C5 H5B 109.4 . . ?
O1 C6 C7 111.4(2) . . ?
O1 C6 C4 105.6(2) . . ?
C7 C6 C4 113.0(2) . . ?
O1 C6 H6 108.9 . . ?
C7 C6 H6 108.9 . . ?
C4 C6 H6 108.9 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 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
C2 N1 N2 N3 -0.6(3) . . . . ?
C5 N1 N2 N3 175.1(3) . . . . ?
N1 N2 N3 C1 0.4(3) . . . . ?
N2 N3 C1 C2 -0.1(3) . . . . ?
N2 N1 C2 C1 0.5(3) . . . . ?
C5 N1 C2 C1 -175.9(2) . . . . ?
N2 N1 C2 C3 -179.8(2) . . . . ?
C5 N1 C2 C3 3.7(3) . . . . ?
N3 C1 C2 N1 -0.2(3) . . . . ?
N3 C1 C2 C3 -179.6(4) . . . . ?
N1 C2 C3 C4 10.6(3) . . . . ?
C1 C2 C3 C4 -170.0(4) . . . . ?
C2 C3 C4 C6 -146.1(2) . . . . ?
C2 C3 C4 C5 -20.0(3) . . . . ?
N2 N1 C5 C4 168.1(3) . . . . ?
C2 N1 C5 C4 -16.2(3) . . . . ?
C6 C4 C5 N1 146.9(2) . . . . ?
C3 C4 C5 N1 21.6(2) . . . . ?
C5 C4 C6 O1 179.3(2) . . . . ?
C3 C4 C6 O1 -58.9(3) . . . . ?
C5 C4 C6 C7 57.3(3) . . . . ?
C3 C4 C6 C7 179.2(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.155
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.046
####################################################################### 
# 
# 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_sn_jh_585_0m
_database_code_depnum_ccdc_archive 'CCDC 1502161'
_audit_update_record             
;
2016-09-01 deposited with the CCDC.
2018-03-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H32 O3 Si'
_chemical_formula_sum            'C26 H32 O3 Si'
_chemical_formula_weight         420.61

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   10.523(5)
_cell_length_b                   10.046(5)
_cell_length_c                   11.683(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 103.959(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     1198.6(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    13801
_cell_measurement_theta_min      1.80
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             452
_exptl_absorpt_coefficient_mu    0.121
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9762
_exptl_absorpt_correction_T_max  0.9880
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'bruker smart apex II CCD'
_diffrn_measurement_method       '\ w scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13801
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.80
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4156
_reflns_number_gt                3726
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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 > 2σ(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     
'calc w=1/[σ²(Fo²)+(0.0529P)²+0.0680P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(11)
_refine_ls_number_reflns         4156
_refine_ls_number_parameters     276
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0352
_refine_ls_wR_factor_ref         0.0917
_refine_ls_wR_factor_gt          0.0878
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.002
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3091(3) 0.4122(3) 0.1753(3) 0.0868(9) Uani 1 1 d . . .
H1A H 0.2902 0.3763 0.2456 0.130 Uiso 1 1 calc R . .
H1B H 0.3685 0.3540 0.1488 0.130 Uiso 1 1 calc R . .
H1C H 0.2294 0.4198 0.1150 0.130 Uiso 1 1 calc R . .
C2 C 0.37054(18) 0.5474(2) 0.20146(19) 0.0549(5) Uani 1 1 d . . .
H2A H 0.3877 0.5830 0.1285 0.066 Uiso 1 1 calc R . .
C3 C 0.28521(18) 0.6454(2) 0.24613(18) 0.0544(5) Uani 1 1 d . . .
H3 H 0.2642 0.6070 0.3165 0.065 Uiso 1 1 calc R . .
C4 C 0.3484(2) 0.7836(2) 0.2802(2) 0.0598(6) Uani 1 1 d . . .
H4A H 0.3858 0.7890 0.3645 0.072 Uiso 1 1 calc R . .
H4B H 0.4166 0.8007 0.2393 0.072 Uiso 1 1 calc R . .
C5 C 0.23775(19) 0.8808(3) 0.24288(19) 0.0584(6) Uani 1 1 d . . .
C6 C 0.2257(2) 1.0094(2) 0.21899(19) 0.0638(7) Uani 1 1 d . . .
H6 H 0.2923 1.0720 0.2403 0.077 Uiso 1 1 calc R . .
C7 C 0.0929(2) 1.0379(3) 0.1545(2) 0.0713(7) Uani 1 1 d . . .
C8 C 0.0186(2) 0.9067(3) 0.1336(3) 0.0817(8) Uani 1 1 d . . .
H8A H -0.0015 0.8827 0.0507 0.098 Uiso 1 1 calc R . .
H8B H -0.0625 0.9125 0.1589 0.098 Uiso 1 1 calc R . .
C9 C 0.1113(2) 0.8054(3) 0.2077(2) 0.0672(7) Uani 1 1 d . . .
H9 H 0.0807 0.7837 0.2784 0.081 Uiso 1 1 calc R . .
C10 C 0.15452(19) 0.6773(2) 0.15636(19) 0.0587(6) Uani 1 1 d . . .
H10 H 0.0904 0.6057 0.1523 0.070 Uiso 1 1 calc R . .
C11 C 0.75422(19) 0.5438(2) 0.40828(18) 0.0522(5) Uani 1 1 d . . .
C12 C 0.7372(2) 0.6641(2) 0.4596(2) 0.0653(6) Uani 1 1 d . . .
H12 H 0.6590 0.7104 0.4337 0.078 Uiso 1 1 calc R . .
C13 C 0.8359(4) 0.7170(3) 0.5501(3) 0.0892(9) Uani 1 1 d . . .
H13 H 0.8229 0.7980 0.5841 0.107 Uiso 1 1 calc R . .
C14 C 0.9512(3) 0.6505(4) 0.5887(3) 0.0916(10) Uani 1 1 d . . .
H14 H 1.0178 0.6876 0.6471 0.110 Uiso 1 1 calc R . .
C15 C 0.9689(3) 0.5308(4) 0.5421(3) 0.0963(10) Uani 1 1 d . . .
H15 H 1.0468 0.4847 0.5700 0.116 Uiso 1 1 calc R . .
C16 C 0.8722(2) 0.4772(3) 0.4538(2) 0.0764(7) Uani 1 1 d . . .
H16 H 0.8856 0.3943 0.4233 0.092 Uiso 1 1 calc R . .
C17 C 0.63226(19) 0.2914(2) 0.2887(2) 0.0553(5) Uani 1 1 d . . .
C18 C 0.5791(3) 0.2385(3) 0.3776(2) 0.0764(7) Uani 1 1 d . . .
H18 H 0.5415 0.2953 0.4230 0.092 Uiso 1 1 calc R . .
C19 C 0.5813(3) 0.1026(3) 0.3994(3) 0.0966(10) Uani 1 1 d . . .
H19 H 0.5474 0.0693 0.4601 0.116 Uiso 1 1 calc R . .
C20 C 0.6335(3) 0.0176(3) 0.3314(4) 0.0962(11) Uani 1 1 d . . .
H20 H 0.6363 -0.0734 0.3465 0.115 Uiso 1 1 calc R . .
C21 C 0.6815(3) 0.0669(3) 0.2414(4) 0.0926(10) Uani 1 1 d . . .
H21 H 0.7142 0.0087 0.1936 0.111 Uiso 1 1 calc R . .
C22 C 0.6821(2) 0.2016(2) 0.2204(3) 0.0688(7) Uani 1 1 d . . .
H22 H 0.7165 0.2332 0.1593 0.083 Uiso 1 1 calc R . .
C23 C 0.6803(2) 0.5401(3) 0.1382(2) 0.0636(6) Uani 1 1 d . . .
C24 C 0.8254(2) 0.5077(3) 0.1452(3) 0.0853(9) Uani 1 1 d . . .
H24A H 0.8792 0.5445 0.2163 0.128 Uiso 1 1 calc R . .
H24B H 0.8502 0.5455 0.0783 0.128 Uiso 1 1 calc R . .
H24C H 0.8370 0.4129 0.1452 0.128 Uiso 1 1 calc R . .
C25 C 0.5961(2) 0.4784(4) 0.0243(2) 0.0836(7) Uani 1 1 d . . .
H25A H 0.6095 0.3838 0.0256 0.125 Uiso 1 1 calc R . .
H25B H 0.6211 0.5159 -0.0427 0.125 Uiso 1 1 calc R . .
H25C H 0.5054 0.4971 0.0189 0.125 Uiso 1 1 calc R . .
C26 C 0.6652(3) 0.6930(3) 0.1338(3) 0.0926(9) Uani 1 1 d . . .
H26A H 0.6918 0.7270 0.0664 0.139 Uiso 1 1 calc R . .
H26B H 0.7192 0.7310 0.2044 0.139 Uiso 1 1 calc R . .
H26C H 0.5754 0.7160 0.1280 0.139 Uiso 1 1 calc R . .
O1 O 0.49345(12) 0.53987(14) 0.28902(12) 0.0525(3) Uani 1 1 d . . .
O2 O 0.18131(14) 0.70132(19) 0.04569(14) 0.0664(4) Uani 1 1 d . . .
H2 H 0.1140 0.6920 -0.0064 0.100 Uiso 1 1 calc R . .
O3 O 0.04783(19) 1.1473(2) 0.11814(16) 0.0908(6) Uani 1 1 d . . .
Si1 Si 0.63361(5) 0.47825(5) 0.27570(5) 0.04603(15) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.504(3) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 O1 1.445(2) . ?
C2 C3 1.508(3) . ?
C2 H2A 0.9800 . ?
C3 C4 1.549(3) . ?
C3 C10 1.549(3) . ?
C3 H3 0.9800 . ?
C4 C5 1.501(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.321(4) . ?
C5 C9 1.500(3) . ?
C6 C7 1.447(3) . ?
C6 H6 0.9300 . ?
C7 O3 1.231(3) . ?
C7 C8 1.522(4) . ?
C8 C9 1.527(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.535(4) . ?
C9 H9 0.9800 . ?
C10 O2 1.409(3) . ?
C10 H10 0.9800 . ?
C11 C12 1.379(3) . ?
C11 C16 1.398(3) . ?
C11 Si1 1.870(2) . ?
C12 C13 1.396(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.364(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.351(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.373(4) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 C22 1.388(3) . ?
C17 C18 1.398(4) . ?
C17 Si1 1.884(2) . ?
C18 C19 1.388(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.368(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.365(5) . ?
C20 H20 0.9300 . ?
C21 C22 1.376(4) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 C25 1.540(4) . ?
C23 C26 1.543(4) . ?
C23 C24 1.545(3) . ?
C23 Si1 1.895(2) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
O1 Si1 1.6412(16) . ?
O2 H2 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C1 111.3(2) . . ?
O1 C2 C3 107.19(16) . . ?
C1 C2 C3 113.41(19) . . ?
O1 C2 H2A 108.3 . . ?
C1 C2 H2A 108.3 . . ?
C3 C2 H2A 108.3 . . ?
C2 C3 C4 114.82(18) . . ?
C2 C3 C10 113.98(18) . . ?
C4 C3 C10 104.17(18) . . ?
C2 C3 H3 107.8 . . ?
C4 C3 H3 107.8 . . ?
C10 C3 H3 107.8 . . ?
C5 C4 C3 104.70(17) . . ?
C5 C4 H4A 110.8 . . ?
C3 C4 H4A 110.8 . . ?
C5 C4 H4B 110.8 . . ?
C3 C4 H4B 110.8 . . ?
H4A C4 H4B 108.9 . . ?
C6 C5 C9 113.7(2) . . ?
C6 C5 C4 136.5(2) . . ?
C9 C5 C4 109.0(2) . . ?
C5 C6 C7 109.6(2) . . ?
C5 C6 H6 125.2 . . ?
C7 C6 H6 125.2 . . ?
O3 C7 C6 126.9(3) . . ?
O3 C7 C8 125.2(2) . . ?
C6 C7 C8 107.8(2) . . ?
C7 C8 C9 104.6(2) . . ?
C7 C8 H8A 110.8 . . ?
C9 C8 H8A 110.8 . . ?
C7 C8 H8B 110.8 . . ?
C9 C8 H8B 110.8 . . ?
H8A C8 H8B 108.9 . . ?
C5 C9 C8 102.8(2) . . ?
C5 C9 C10 101.74(17) . . ?
C8 C9 C10 123.1(2) . . ?
C5 C9 H9 109.4 . . ?
C8 C9 H9 109.4 . . ?
C10 C9 H9 109.4 . . ?
O2 C10 C9 111.0(2) . . ?
O2 C10 C3 108.38(16) . . ?
C9 C10 C3 101.96(18) . . ?
O2 C10 H10 111.7 . . ?
C9 C10 H10 111.7 . . ?
C3 C10 H10 111.7 . . ?
C12 C11 C16 116.8(2) . . ?
C12 C11 Si1 122.38(17) . . ?
C16 C11 Si1 120.64(18) . . ?
C11 C12 C13 120.8(3) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
C14 C13 C12 120.3(3) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C15 C14 C13 120.1(3) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C16 120.2(3) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C15 C16 C11 121.8(3) . . ?
C15 C16 H16 119.1 . . ?
C11 C16 H16 119.1 . . ?
C22 C17 C18 117.1(2) . . ?
C22 C17 Si1 126.1(2) . . ?
C18 C17 Si1 116.79(18) . . ?
C19 C18 C17 121.2(3) . . ?
C19 C18 H18 119.4 . . ?
C17 C18 H18 119.4 . . ?
C20 C19 C18 120.0(3) . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C21 C20 C19 119.7(3) . . ?
C21 C20 H20 120.1 . . ?
C19 C20 H20 120.1 . . ?
C20 C21 C22 120.9(3) . . ?
C20 C21 H21 119.6 . . ?
C22 C21 H21 119.6 . . ?
C21 C22 C17 121.2(3) . . ?
C21 C22 H22 119.4 . . ?
C17 C22 H22 119.4 . . ?
C25 C23 C26 109.8(2) . . ?
C25 C23 C24 108.4(2) . . ?
C26 C23 C24 107.7(2) . . ?
C25 C23 Si1 112.84(18) . . ?
C26 C23 Si1 108.00(18) . . ?
C24 C23 Si1 109.94(18) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C2 O1 Si1 128.63(13) . . ?
C10 O2 H2 109.5 . . ?
O1 Si1 C11 103.56(9) . . ?
O1 Si1 C17 110.11(9) . . ?
C11 Si1 C17 107.53(9) . . ?
O1 Si1 C23 112.29(9) . . ?
C11 Si1 C23 108.91(11) . . ?
C17 Si1 C23 113.82(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C2 C3 C4 53.6(2) . . . . ?
C1 C2 C3 C4 176.9(2) . . . . ?
O1 C2 C3 C10 173.67(18) . . . . ?
C1 C2 C3 C10 -63.1(3) . . . . ?
C2 C3 C4 C5 143.11(19) . . . . ?
C10 C3 C4 C5 17.8(2) . . . . ?
C3 C4 C5 C6 -159.7(3) . . . . ?
C3 C4 C5 C9 9.2(2) . . . . ?
C9 C5 C6 C7 -5.4(3) . . . . ?
C4 C5 C6 C7 163.2(2) . . . . ?
C5 C6 C7 O3 -179.9(3) . . . . ?
C5 C6 C7 C8 -2.6(3) . . . . ?
O3 C7 C8 C9 -173.7(3) . . . . ?
C6 C7 C8 C9 9.0(3) . . . . ?
C6 C5 C9 C8 10.8(3) . . . . ?
C4 C5 C9 C8 -160.9(2) . . . . ?
C6 C5 C9 C10 139.1(2) . . . . ?
C4 C5 C9 C10 -32.6(2) . . . . ?
C7 C8 C9 C5 -11.3(3) . . . . ?
C7 C8 C9 C10 -124.7(2) . . . . ?
C5 C9 C10 O2 -72.9(2) . . . . ?
C8 C9 C10 O2 41.1(3) . . . . ?
C5 C9 C10 C3 42.4(2) . . . . ?
C8 C9 C10 C3 156.4(2) . . . . ?
C2 C3 C10 O2 -46.1(3) . . . . ?
C4 C3 C10 O2 79.8(2) . . . . ?
C2 C3 C10 C9 -163.27(19) . . . . ?
C4 C3 C10 C9 -37.4(2) . . . . ?
C16 C11 C12 C13 1.9(4) . . . . ?
Si1 C11 C12 C13 -172.7(2) . . . . ?
C11 C12 C13 C14 0.3(4) . . . . ?
C12 C13 C14 C15 -2.2(5) . . . . ?
C13 C14 C15 C16 1.6(5) . . . . ?
C14 C15 C16 C11 0.7(5) . . . . ?
C12 C11 C16 C15 -2.5(4) . . . . ?
Si1 C11 C16 C15 172.3(2) . . . . ?
C22 C17 C18 C19 2.7(4) . . . . ?
Si1 C17 C18 C19 -175.7(2) . . . . ?
C17 C18 C19 C20 -1.6(4) . . . . ?
C18 C19 C20 C21 -0.9(4) . . . . ?
C19 C20 C21 C22 2.2(4) . . . . ?
C20 C21 C22 C17 -1.0(4) . . . . ?
C18 C17 C22 C21 -1.4(3) . . . . ?
Si1 C17 C22 C21 176.8(2) . . . . ?
C1 C2 O1 Si1 71.2(3) . . . . ?
C3 C2 O1 Si1 -164.27(15) . . . . ?
C2 O1 Si1 C11 165.32(17) . . . . ?
C2 O1 Si1 C17 -79.95(19) . . . . ?
C2 O1 Si1 C23 48.0(2) . . . . ?
C12 C11 Si1 O1 -30.0(2) . . . . ?
C16 C11 Si1 O1 155.52(19) . . . . ?
C12 C11 Si1 C17 -146.56(19) . . . . ?
C16 C11 Si1 C17 39.0(2) . . . . ?
C12 C11 Si1 C23 89.7(2) . . . . ?
C16 C11 Si1 C23 -84.8(2) . . . . ?
C22 C17 Si1 O1 138.68(18) . . . . ?
C18 C17 Si1 O1 -43.10(19) . . . . ?
C22 C17 Si1 C11 -109.1(2) . . . . ?
C18 C17 Si1 C11 69.08(19) . . . . ?
C22 C17 Si1 C23 11.6(2) . . . . ?
C18 C17 Si1 C23 -170.19(17) . . . . ?
C25 C23 Si1 O1 -72.5(2) . . . . ?
C26 C23 Si1 O1 49.1(2) . . . . ?
C24 C23 Si1 O1 166.30(17) . . . . ?
C25 C23 Si1 C11 173.37(19) . . . . ?
C26 C23 Si1 C11 -65.0(2) . . . . ?
C24 C23 Si1 C11 52.2(2) . . . . ?
C25 C23 Si1 C17 53.4(2) . . . . ?
C26 C23 Si1 C17 175.02(18) . . . . ?
C24 C23 Si1 C17 -67.7(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.151
_refine_diff_density_min         -0.143
_refine_diff_density_rms         0.026
####################################################################### 
# 
# 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_dd440r
_database_code_depnum_ccdc_archive 'CCDC 1407794'
_audit_update_record             
;
2015-06-19 deposited with the CCDC.
2018-03-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H33 N3 O2 Si'
_chemical_formula_weight         435.63

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   10.558(3)
_cell_length_b                   39.473(12)
_cell_length_c                   11.458(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4775(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1872
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            56546
_diffrn_reflns_av_R_equivalents  0.1453
_diffrn_reflns_av_sigmaI/netI    0.2080
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.03
_diffrn_reflns_theta_max         25.00
_reflns_number_total             15822
_reflns_number_gt                9529
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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 > 2σ(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     
'calc w=1/[σ²(Fo²)+(0.0933P)²+0.3397P] 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     SHELXL
_refine_ls_extinction_coef       0.078(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.4(2)
_refine_ls_number_reflns         15822
_refine_ls_number_parameters     1118
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1580
_refine_ls_R_factor_gt           0.1078
_refine_ls_wR_factor_ref         0.2781
_refine_ls_wR_factor_gt          0.2381
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3146(8) 0.4170(2) 0.8219(7) 0.045(2) Uani 1 1 d . . .
H1 H 0.2791 0.4030 0.7652 0.054 Uiso 1 1 calc R . .
C2 C 0.4423(7) 0.4479(2) 0.9087(6) 0.0364(19) Uani 1 1 d . . .
H2 H 0.5127 0.4608 0.9289 0.044 Uiso 1 1 calc R . .
C3 C 0.3136(9) 0.4597(3) 1.0887(9) 0.066(3) Uani 1 1 d . . .
H3A H 0.2237 0.4579 1.1047 0.079 Uiso 1 1 calc R . .
H3B H 0.3582 0.4466 1.1474 0.079 Uiso 1 1 calc R . .
C4 C 0.3501(8) 0.4944(3) 1.0991(9) 0.064(3) Uani 1 1 d . . .
H4 H 0.3232 0.5070 1.0296 0.076 Uiso 1 1 calc R . .
C5 C 0.5154(9) 0.5196(2) 1.2097(8) 0.051(2) Uani 1 1 d . . .
H5 H 0.5360 0.5059 1.2784 0.061 Uiso 1 1 calc R . .
C6 C 0.6259(11) 0.5399(4) 1.1778(12) 0.128(7) Uani 1 1 d . . .
H6A H 0.6972 0.5252 1.1655 0.191 Uiso 1 1 calc R . .
H6B H 0.6447 0.5556 1.2395 0.191 Uiso 1 1 calc R . .
H6C H 0.6083 0.5522 1.1074 0.191 Uiso 1 1 calc R . .
C7 C 0.2977(9) 0.5113(3) 1.2072(10) 0.085(4) Uani 1 1 d . . .
H7A H 0.2918 0.4954 1.2715 0.102 Uiso 1 1 calc R . .
H7B H 0.2146 0.5209 1.1924 0.102 Uiso 1 1 calc R . .
C8 C 0.3957(8) 0.5395(3) 1.2337(8) 0.055(3) Uani 1 1 d . . .
H8 H 0.3871 0.5579 1.1770 0.066 Uiso 1 1 calc R . .
C9 C 0.3806(9) 0.5528(3) 1.3535(7) 0.055(3) Uani 1 1 d . . .
H9A H 0.2990 0.5639 1.3609 0.067 Uiso 1 1 calc R . .
H9B H 0.3834 0.5343 1.4090 0.067 Uiso 1 1 calc R . .
C10 C 0.4657(7) 0.5907(2) 1.7420(7) 0.039(2) Uani 1 1 d . . .
H10 H 0.4383 0.6130 1.7487 0.046 Uiso 1 1 calc R . .
C11 C 0.4847(7) 0.5717(2) 1.8397(8) 0.044(2) Uani 1 1 d . . .
H11 H 0.4700 0.5815 1.9123 0.052 Uiso 1 1 calc R . .
C12 C 0.5244(7) 0.5389(3) 1.8350(8) 0.044(2) Uani 1 1 d . . .
H12 H 0.5384 0.5268 1.9033 0.053 Uiso 1 1 calc R . .
C13 C 0.5435(7) 0.5241(3) 1.7276(9) 0.050(2) Uani 1 1 d . . .
H13 H 0.5686 0.5015 1.7232 0.060 Uiso 1 1 calc R . .
C14 C 0.5255(7) 0.5425(2) 1.6267(8) 0.043(2) Uani 1 1 d . . .
H14 H 0.5388 0.5323 1.5547 0.052 Uiso 1 1 calc R . .
C15 C 0.4873(7) 0.5767(2) 1.6315(7) 0.039(2) Uani 1 1 d . . .
C16 C 0.3254(8) 0.6273(2) 1.4865(7) 0.043(2) Uani 1 1 d . . .
C17 C 0.3010(9) 0.6481(2) 1.3915(8) 0.055(2) Uani 1 1 d . . .
H17 H 0.3614 0.6501 1.3328 0.066 Uiso 1 1 calc R . .
C18 C 0.1893(11) 0.6658(3) 1.3823(10) 0.066(3) Uani 1 1 d . . .
H18 H 0.1763 0.6800 1.3187 0.079 Uiso 1 1 calc R . .
C19 C 0.0972(11) 0.6629(3) 1.4652(11) 0.075(4) Uani 1 1 d . . .
H19 H 0.0218 0.6749 1.4576 0.089 Uiso 1 1 calc R . .
C20 C 0.1166(9) 0.6418(3) 1.5612(11) 0.071(3) Uani 1 1 d . . .
H20 H 0.0539 0.6395 1.6177 0.085 Uiso 1 1 calc R . .
C21 C 0.2289(8) 0.6243(3) 1.5720(9) 0.056(3) Uani 1 1 d . . .
H21 H 0.2417 0.6103 1.6363 0.067 Uiso 1 1 calc R . .
C22 C 0.6228(8) 0.6287(2) 1.4775(7) 0.044(2) Uani 1 1 d . . .
C23 C 0.7413(8) 0.6070(3) 1.5084(9) 0.058(3) Uani 1 1 d . . .
H23A H 0.7449 0.5876 1.4578 0.087 Uiso 1 1 calc R . .
H23B H 0.7356 0.5996 1.5880 0.087 Uiso 1 1 calc R . .
H23C H 0.8164 0.6204 1.4983 0.087 Uiso 1 1 calc R . .
C24 C 0.6389(12) 0.6430(3) 1.3536(10) 0.081(4) Uani 1 1 d . . .
H24A H 0.6381 0.6248 1.2983 0.122 Uiso 1 1 calc R . .
H24B H 0.7180 0.6549 1.3484 0.122 Uiso 1 1 calc R . .
H24C H 0.5707 0.6583 1.3368 0.122 Uiso 1 1 calc R . .
C25 C 0.6221(10) 0.6592(3) 1.5605(9) 0.069(3) Uani 1 1 d . . .
H25A H 0.6134 0.6514 1.6394 0.104 Uiso 1 1 calc R . .
H25B H 0.5524 0.6738 1.5415 0.104 Uiso 1 1 calc R . .
H25C H 0.7001 0.6715 1.5526 0.104 Uiso 1 1 calc R . .
C26 C 0.2062(8) 0.4135(2) 0.3411(8) 0.050(2) Uani 1 1 d . . .
H26 H 0.2385 0.3967 0.2925 0.060 Uiso 1 1 calc R . .
C27 C 0.0840(8) 0.4495(2) 0.4110(7) 0.044(2) Uani 1 1 d . . .
H27 H 0.0147 0.4634 0.4249 0.053 Uiso 1 1 calc R . .
C28 C 0.2375(8) 0.4749(3) 0.5571(7) 0.056(3) Uani 1 1 d . . .
H28A H 0.2568 0.4965 0.5210 0.067 Uiso 1 1 calc R . .
H28B H 0.3153 0.4661 0.5905 0.067 Uiso 1 1 calc R . .
C29 C 0.1429(7) 0.4804(2) 0.6531(7) 0.048(2) Uani 1 1 d . . .
H29 H 0.1175 0.4582 0.6839 0.057 Uiso 1 1 calc R . .
C30 C 0.1967(9) 0.5015(3) 0.7532(8) 0.059(3) Uani 1 1 d . . .
H30A H 0.2228 0.4872 0.8176 0.071 Uiso 1 1 calc R . .
H30B H 0.2689 0.5148 0.7274 0.071 Uiso 1 1 calc R . .
C31 C 0.0881(8) 0.5243(2) 0.7887(7) 0.043(2) Uani 1 1 d . . .
H31 H 0.0322 0.5118 0.8418 0.052 Uiso 1 1 calc R . .
C32 C 0.0202(8) 0.5298(2) 0.6748(7) 0.040(2) Uani 1 1 d . . .
H32 H 0.0653 0.5473 0.6304 0.048 Uiso 1 1 calc R . .
C33 C -0.1162(8) 0.5385(2) 0.6776(8) 0.054(3) Uani 1 1 d . . .
H33A H -0.1465 0.5416 0.5994 0.081 Uiso 1 1 calc R . .
H33B H -0.1280 0.5591 0.7211 0.081 Uiso 1 1 calc R . .
H33C H -0.1626 0.5205 0.7143 0.081 Uiso 1 1 calc R . .
C34 C 0.1320(8) 0.5567(2) 0.8489(7) 0.043(2) Uani 1 1 d . . .
H34A H 0.1793 0.5510 0.9188 0.051 Uiso 1 1 calc R . .
H34B H 0.1875 0.5692 0.7972 0.051 Uiso 1 1 calc R . .
C35 C 0.1776(8) 0.6279(2) 0.9866(7) 0.039(2) Uani 1 1 d . . .
C36 C 0.2035(8) 0.6495(2) 0.8938(7) 0.046(2) Uani 1 1 d . . .
H36 H 0.1410 0.6524 0.8375 0.055 Uiso 1 1 calc R . .
C37 C 0.3174(11) 0.6671(3) 0.8799(10) 0.070(3) Uani 1 1 d . . .
H37 H 0.3316 0.6810 0.8156 0.084 Uiso 1 1 calc R . .
C38 C 0.4066(9) 0.6631(3) 0.9646(9) 0.055(3) Uani 1 1 d . . .
H38 H 0.4839 0.6742 0.9574 0.066 Uiso 1 1 calc R . .
C39 C 0.3844(8) 0.6425(3) 1.0631(10) 0.060(3) Uani 1 1 d . . .
H39 H 0.4458 0.6404 1.1209 0.072 Uiso 1 1 calc R . .
C40 C 0.2707(8) 0.6255(2) 1.0729(8) 0.047(2) Uani 1 1 d . . .
H40 H 0.2556 0.6122 1.1385 0.057 Uiso 1 1 calc R . .
C41 C 0.0175(7) 0.5782(2) 1.1295(6) 0.0354(19) Uani 1 1 d . . .
C42 C -0.0159(7) 0.5440(2) 1.1273(7) 0.0340(18) Uani 1 1 d . . .
H42 H -0.0269 0.5339 1.0547 0.041 Uiso 1 1 calc R . .
C43 C -0.0341(8) 0.5240(2) 1.2258(7) 0.042(2) Uani 1 1 d . . .
H43 H -0.0573 0.5013 1.2190 0.050 Uiso 1 1 calc R . .
C44 C -0.0164(8) 0.5388(3) 1.3342(7) 0.046(2) Uani 1 1 d . . .
H44 H -0.0281 0.5262 1.4020 0.055 Uiso 1 1 calc R . .
C45 C 0.0191(8) 0.5726(3) 1.3405(7) 0.047(2) Uani 1 1 d . . .
H45 H 0.0330 0.5823 1.4133 0.056 Uiso 1 1 calc R . .
C46 C 0.0343(7) 0.5920(2) 1.2423(7) 0.040(2) Uani 1 1 d . . .
H46 H 0.0561 0.6147 1.2500 0.048 Uiso 1 1 calc R . .
C47 C -0.1235(7) 0.6292(2) 0.9757(8) 0.042(2) Uani 1 1 d . . .
C48 C -0.1389(10) 0.6423(3) 0.8510(9) 0.068(3) Uani 1 1 d . . .
H48A H -0.0670 0.6560 0.8306 0.102 Uiso 1 1 calc R . .
H48B H -0.2146 0.6556 0.8456 0.102 Uiso 1 1 calc R . .
H48C H -0.1446 0.6234 0.7983 0.102 Uiso 1 1 calc R . .
C49 C -0.2376(8) 0.6076(2) 1.0014(9) 0.057(3) Uani 1 1 d . . .
H49A H -0.2308 0.5986 1.0788 0.085 Uiso 1 1 calc R . .
H49B H -0.2418 0.5894 0.9461 0.085 Uiso 1 1 calc R . .
H49C H -0.3128 0.6212 0.9956 0.085 Uiso 1 1 calc R . .
C50 C -0.1200(9) 0.6596(2) 1.0588(9) 0.061(3) Uani 1 1 d . . .
H50A H -0.0476 0.6734 1.0411 0.092 Uiso 1 1 calc R . .
H50B H -0.1143 0.6517 1.1378 0.092 Uiso 1 1 calc R . .
H50C H -0.1958 0.6728 1.0494 0.092 Uiso 1 1 calc R . .
C51 C -0.0537(7) 0.4454(2) 0.9004(7) 0.041(2) Uani 1 1 d . . .
H51 H 0.0178 0.4330 0.8795 0.049 Uiso 1 1 calc R . .
C52 C -0.1835(8) 0.4754(2) 0.9866(8) 0.051(2) Uani 1 1 d . . .
H52 H -0.2202 0.4886 1.0448 0.061 Uiso 1 1 calc R . .
C53 C -0.1894(10) 0.4333(3) 0.7202(8) 0.062(3) Uani 1 1 d . . .
H53A H -0.2805 0.4342 0.7096 0.074 Uiso 1 1 calc R . .
H53B H -0.1512 0.4472 0.6598 0.074 Uiso 1 1 calc R . .
C54 C -0.1476(7) 0.3985(2) 0.7048(8) 0.047(2) Uani 1 1 d . . .
H54 H -0.1743 0.3856 0.7735 0.056 Uiso 1 1 calc R . .
C55 C -0.2029(9) 0.3815(3) 0.5978(10) 0.078(4) Uani 1 1 d . . .
H55A H -0.2093 0.3973 0.5332 0.094 Uiso 1 1 calc R . .
H55B H -0.2860 0.3722 0.6141 0.094 Uiso 1 1 calc R . .
C56 C -0.1079(8) 0.3537(2) 0.5718(8) 0.050(2) Uani 1 1 d . . .
H56 H -0.1184 0.3356 0.6295 0.060 Uiso 1 1 calc R . .
C57 C 0.0113(7) 0.3728(2) 0.5989(8) 0.046(2) Uani 1 1 d . . .
H57 H 0.0341 0.3864 0.5305 0.055 Uiso 1 1 calc R . .
C58 C 0.1214(10) 0.3504(3) 0.6289(12) 0.098(5) Uani 1 1 d . . .
H58A H 0.1948 0.3642 0.6433 0.147 Uiso 1 1 calc R . .
H58B H 0.1381 0.3353 0.5651 0.147 Uiso 1 1 calc R . .
H58C H 0.1018 0.3375 0.6975 0.147 Uiso 1 1 calc R . .
C59 C -0.1227(7) 0.3390(2) 0.4524(8) 0.049(2) Uani 1 1 d . . .
H59A H -0.2055 0.3285 0.4460 0.058 Uiso 1 1 calc R . .
H59B H -0.1180 0.3571 0.3951 0.058 Uiso 1 1 calc R . .
C60 C -0.0156(7) 0.3156(2) 0.1782(6) 0.0336(18) Uani 1 1 d . . .
C61 C -0.0328(7) 0.3024(2) 0.0651(7) 0.043(2) Uani 1 1 d . . .
H61 H -0.0589 0.2800 0.0574 0.052 Uiso 1 1 calc R . .
C62 C -0.0121(8) 0.3216(2) -0.0372(7) 0.042(2) Uani 1 1 d . . .
H62 H -0.0252 0.3120 -0.1103 0.050 Uiso 1 1 calc R . .
C63 C 0.0277(7) 0.3548(2) -0.0274(7) 0.042(2) Uani 1 1 d . . .
H63 H 0.0448 0.3674 -0.0941 0.051 Uiso 1 1 calc R . .
C64 C 0.0420(7) 0.3690(2) 0.0804(7) 0.041(2) Uani 1 1 d . . .
H64 H 0.0632 0.3918 0.0864 0.050 Uiso 1 1 calc R . .
C65 C 0.0252(7) 0.3497(2) 0.1830(7) 0.040(2) Uani 1 1 d . . .
H65 H 0.0413 0.3596 0.2552 0.048 Uiso 1 1 calc R . .
C66 C -0.1888(7) 0.2665(2) 0.3108(6) 0.038(2) Uani 1 1 d . . .
C67 C -0.2172(8) 0.2433(2) 0.3962(8) 0.048(2) Uani 1 1 d . . .
H67 H -0.1569 0.2382 0.4527 0.057 Uiso 1 1 calc R . .
C68 C -0.3326(7) 0.2274(2) 0.4000(7) 0.044(2) Uani 1 1 d . . .
H68 H -0.3487 0.2117 0.4585 0.053 Uiso 1 1 calc R . .
C69 C -0.4280(8) 0.2346(2) 0.3162(7) 0.041(2) Uani 1 1 d . . .
H69 H -0.5066 0.2239 0.3175 0.049 Uiso 1 1 calc R . .
C70 C -0.3967(7) 0.2583(2) 0.2330(7) 0.043(2) Uani 1 1 d . . .
H70 H -0.4567 0.2639 0.1768 0.052 Uiso 1 1 calc R . .
C71 C -0.2798(8) 0.2741(2) 0.2294(7) 0.046(2) Uani 1 1 d . . .
H71 H -0.2627 0.2899 0.1714 0.055 Uiso 1 1 calc R . .
C72 C 0.1114(8) 0.2620(2) 0.3286(7) 0.040(2) Uani 1 1 d . . .
C73 C 0.2288(8) 0.2824(3) 0.3008(9) 0.058(3) Uani 1 1 d . . .
H73A H 0.2352 0.3011 0.3542 0.086 Uiso 1 1 calc R . .
H73B H 0.2234 0.2908 0.2224 0.086 Uiso 1 1 calc R . .
H73C H 0.3023 0.2682 0.3083 0.086 Uiso 1 1 calc R . .
C74 C 0.1232(9) 0.2485(3) 0.4545(9) 0.070(3) Uani 1 1 d . . .
H74A H 0.0494 0.2354 0.4736 0.105 Uiso 1 1 calc R . .
H74B H 0.1304 0.2672 0.5076 0.105 Uiso 1 1 calc R . .
H74C H 0.1972 0.2344 0.4606 0.105 Uiso 1 1 calc R . .
C75 C 0.1037(10) 0.2325(3) 0.2400(9) 0.065(3) Uani 1 1 d . . .
H75A H 0.0289 0.2193 0.2548 0.098 Uiso 1 1 calc R . .
H75B H 0.1771 0.2183 0.2479 0.098 Uiso 1 1 calc R . .
H75C H 0.1003 0.2415 0.1622 0.098 Uiso 1 1 calc R . .
C76 C -0.2261(7) 0.4642(2) 1.3786(7) 0.0366(19) Uani 1 1 d . . .
H76 H -0.1434 0.4685 1.3549 0.044 Uiso 1 1 calc R . .
C77 C -0.4124(7) 0.4668(2) 1.4756(6) 0.0337(18) Uani 1 1 d . . .
H77 H -0.4739 0.4733 1.5291 0.040 Uiso 1 1 calc R . .
C78 C -0.2651(8) 0.4172(3) 1.2486(7) 0.055(3) Uani 1 1 d . . .
H78A H -0.2465 0.3955 1.2845 0.066 Uiso 1 1 calc R . .
H78B H -0.1871 0.4258 1.2151 0.066 Uiso 1 1 calc R . .
C79 C -0.3607(7) 0.4120(2) 1.1521(7) 0.044(2) Uani 1 1 d . . .
H79 H -0.3871 0.4341 1.1216 0.053 Uiso 1 1 calc R . .
C80 C -0.3043(8) 0.3902(2) 1.0503(7) 0.048(2) Uani 1 1 d . . .
H80A H -0.2778 0.4044 0.9857 0.058 Uiso 1 1 calc R . .
H80B H -0.2327 0.3769 1.0768 0.058 Uiso 1 1 calc R . .
C81 C -0.4154(7) 0.3674(2) 1.0151(8) 0.041(2) Uani 1 1 d . . .
H81 H -0.4731 0.3802 0.9646 0.050 Uiso 1 1 calc R . .
C82 C -0.4763(8) 0.3629(2) 1.1346(7) 0.040(2) Uani 1 1 d . . .
H82 H -0.4270 0.3462 1.1787 0.048 Uiso 1 1 calc R . .
C83 C -0.6163(9) 0.3510(2) 1.1303(8) 0.054(2) Uani 1 1 d . . .
H83A H -0.6476 0.3481 1.2083 0.081 Uiso 1 1 calc R . .
H83B H -0.6216 0.3298 1.0892 0.081 Uiso 1 1 calc R . .
H83C H -0.6665 0.3677 1.0906 0.081 Uiso 1 1 calc R . .
C84 C -0.3703(7) 0.3368(2) 0.9518(7) 0.0369(19) Uani 1 1 d . . .
H84A H -0.3293 0.3436 0.8798 0.044 Uiso 1 1 calc R . .
H84B H -0.3085 0.3249 0.9993 0.044 Uiso 1 1 calc R . .
C85 C -0.4862(7) 0.3152(2) 0.6755(7) 0.0342(19) Uani 1 1 d . . .
C86 C -0.5192(7) 0.3488(2) 0.6812(7) 0.040(2) Uani 1 1 d . . .
H86 H -0.5290 0.3584 0.7548 0.048 Uiso 1 1 calc R . .
C87 C -0.5391(7) 0.3693(2) 0.5852(7) 0.0374(19) Uani 1 1 d . . .
H87 H -0.5609 0.3921 0.5931 0.045 Uiso 1 1 calc R . .
C88 C -0.5242(7) 0.3538(2) 0.4726(7) 0.039(2) Uani 1 1 d . . .
H88 H -0.5366 0.3667 0.4056 0.047 Uiso 1 1 calc R . .
C89 C -0.4924(7) 0.3206(2) 0.4624(7) 0.039(2) Uani 1 1 d . . .
H89 H -0.4833 0.3107 0.3893 0.047 Uiso 1 1 calc R . .
C90 C -0.4733(7) 0.3013(2) 0.5654(7) 0.039(2) Uani 1 1 d . . .
H90 H -0.4513 0.2786 0.5585 0.047 Uiso 1 1 calc R . .
C91 C -0.3153(7) 0.2651(2) 0.8092(7) 0.0346(19) Uani 1 1 d . . .
C92 C -0.2244(7) 0.2714(2) 0.7244(7) 0.0362(19) Uani 1 1 d . . .
H92 H -0.2437 0.2863 0.6642 0.043 Uiso 1 1 calc R . .
C93 C -0.1068(8) 0.2563(2) 0.7256(7) 0.046(2) Uani 1 1 d . . .
H93 H -0.0475 0.2610 0.6678 0.055 Uiso 1 1 calc R . .
C94 C -0.0788(8) 0.2336(2) 0.8170(8) 0.053(2) Uani 1 1 d . . .
H94 H -0.0009 0.2226 0.8181 0.063 Uiso 1 1 calc R . .
C95 C -0.1645(8) 0.2274(2) 0.9039(7) 0.046(2) Uani 1 1 d . . .
H95 H -0.1444 0.2127 0.9645 0.055 Uiso 1 1 calc R . .
C96 C -0.2834(8) 0.2435(2) 0.9011(7) 0.044(2) Uani 1 1 d . . .
H96 H -0.3412 0.2396 0.9609 0.053 Uiso 1 1 calc R . .
C97 C -0.6129(8) 0.2611(2) 0.8308(8) 0.042(2) Uani 1 1 d . . .
C98 C -0.6085(10) 0.2321(3) 0.7475(11) 0.079(4) Uani 1 1 d . . .
H98A H -0.5335 0.2189 0.7615 0.119 Uiso 1 1 calc R . .
H98B H -0.6072 0.2406 0.6690 0.119 Uiso 1 1 calc R . .
H98C H -0.6819 0.2181 0.7584 0.119 Uiso 1 1 calc R . .
C99 C -0.7311(8) 0.2820(3) 0.8076(8) 0.058(3) Uani 1 1 d . . .
H99A H -0.7341 0.3007 0.8611 0.087 Uiso 1 1 calc R . .
H99B H -0.8049 0.2681 0.8179 0.087 Uiso 1 1 calc R . .
H99C H -0.7290 0.2905 0.7290 0.087 Uiso 1 1 calc R . .
C100 C -0.6286(8) 0.2478(2) 0.9557(8) 0.055(2) Uani 1 1 d . . .
H10A H -0.6324 0.2666 1.0089 0.082 Uiso 1 1 calc R . .
H10B H -0.5579 0.2336 0.9753 0.082 Uiso 1 1 calc R . .
H10C H -0.7055 0.2349 0.9612 0.082 Uiso 1 1 calc R . .
N1 N 0.3398(6) 0.44493(19) 0.9725(6) 0.0454(18) Uani 1 1 d . . .
N2 N 0.2523(6) 0.42482(19) 0.9167(6) 0.0507(19) Uani 1 1 d . . .
N3 N 0.4313(6) 0.42967(18) 0.8093(6) 0.0431(17) Uani 1 1 d . . .
N4 N 0.1924(6) 0.45131(17) 0.4668(6) 0.0403(17) Uani 1 1 d . . .
N5 N 0.2738(7) 0.4277(2) 0.4239(7) 0.0511(19) Uani 1 1 d . . .
N6 N 0.0872(7) 0.42494(18) 0.3320(6) 0.0469(18) Uani 1 1 d . . .
N7 N -0.1582(6) 0.44796(18) 0.8347(6) 0.0447(18) Uani 1 1 d . . .
N8 N -0.2417(7) 0.46844(19) 0.8924(7) 0.051(2) Uani 1 1 d . . .
N9 N -0.0647(6) 0.4624(2) 0.9974(6) 0.0471(18) Uani 1 1 d . . .
N10 N -0.3087(6) 0.44062(18) 1.3382(5) 0.0391(17) Uani 1 1 d . . .
N11 N -0.4177(9) 0.4428(2) 1.3953(8) 0.074(3) Uani 1 1 d . . .
N12 N -0.2928(10) 0.4794(3) 1.4596(10) 0.094(3) Uani 1 1 d . . .
O1 O 0.4838(5) 0.49703(15) 1.1121(5) 0.0426(14) Uani 1 1 d . . .
O2 O 0.4810(5) 0.57669(15) 1.3789(5) 0.0407(14) Uani 1 1 d . . .
O3 O 0.0300(5) 0.49813(14) 0.6132(4) 0.0381(13) Uani 1 1 d . . .
O4 O 0.0246(5) 0.57720(13) 0.8795(4) 0.0335(12) Uani 1 1 d . . .
O5 O -0.0149(5) 0.39518(15) 0.6937(5) 0.0456(15) Uani 1 1 d . . .
O6 O -0.0274(5) 0.31448(15) 0.4280(4) 0.0404(14) Uani 1 1 d . . .
O7 O -0.4701(5) 0.39394(15) 1.1931(4) 0.0431(14) Uani 1 1 d . . .
O8 O -0.4723(5) 0.31481(14) 0.9261(4) 0.0348(13) Uani 1 1 d . . .
Si1 Si 0.4766(2) 0.60210(6) 1.49309(19) 0.0378(6) Uani 1 1 d . . .
Si2 Si 0.02556(19) 0.60321(6) 0.99248(18) 0.0350(5) Uani 1 1 d . . .
Si3 Si -0.03158(19) 0.29023(6) 0.31228(18) 0.0340(5) Uani 1 1 d . . .
Si4 Si -0.47078(19) 0.28934(6) 0.81239(18) 0.0340(5) Uani 1 1 d . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 N2 1.307(10) . ?
C1 N3 1.337(11) . ?
C2 N1 1.311(9) . ?
C2 N3 1.352(10) . ?
C3 C4 1.428(14) . ?
C3 N1 1.480(11) . ?
C4 O1 1.422(10) . ?
C4 C7 1.511(13) . ?
C5 C6 1.461(14) . ?
C5 O1 1.469(10) . ?
C5 C8 1.512(13) . ?
C7 C8 1.548(14) . ?
C8 C9 1.479(12) . ?
C9 O2 1.448(11) . ?
C10 C11 1.362(12) . ?
C10 C15 1.400(11) . ?
C11 C12 1.361(13) . ?
C12 C13 1.379(13) . ?
C13 C14 1.379(12) . ?
C14 C15 1.411(12) . ?
C15 Si1 1.879(9) . ?
C16 C17 1.388(12) . ?
C16 C21 1.418(13) . ?
C16 Si1 1.882(9) . ?
C17 C18 1.375(13) . ?
C18 C19 1.364(16) . ?
C19 C20 1.395(16) . ?
C20 C21 1.378(13) . ?
C22 C25 1.532(12) . ?
C22 C24 1.537(13) . ?
C22 C23 1.557(12) . ?
C22 Si1 1.877(9) . ?
C26 N5 1.314(11) . ?
C26 N6 1.340(11) . ?
C27 N4 1.313(10) . ?
C27 N6 1.326(11) . ?
C28 N4 1.472(11) . ?
C28 C29 1.502(11) . ?
C29 O3 1.456(9) . ?
C29 C30 1.528(12) . ?
C30 C31 1.513(12) . ?
C31 C32 1.506(11) . ?
C31 C34 1.524(12) . ?
C32 O3 1.440(10) . ?
C32 C33 1.481(12) . ?
C34 O4 1.438(9) . ?
C35 C36 1.389(11) . ?
C35 C40 1.397(12) . ?
C35 Si2 1.879(8) . ?
C36 C37 1.400(13) . ?
C37 C38 1.362(15) . ?
C38 C39 1.410(14) . ?
C39 C40 1.379(12) . ?
C41 C42 1.392(11) . ?
C41 C46 1.414(11) . ?
C41 Si2 1.858(8) . ?
C42 C43 1.392(11) . ?
C43 C44 1.386(12) . ?
C44 C45 1.387(13) . ?
C45 C46 1.372(12) . ?
C47 C49 1.504(11) . ?
C47 C48 1.528(13) . ?
C47 C50 1.532(12) . ?
C47 Si2 1.889(8) . ?
C51 N9 1.304(10) . ?
C51 N7 1.340(10) . ?
C52 N8 1.272(11) . ?
C52 N9 1.361(11) . ?
C53 C54 1.454(13) . ?
C53 N7 1.471(11) . ?
C54 O5 1.413(9) . ?
C54 C55 1.514(13) . ?
C55 C56 1.516(13) . ?
C56 C59 1.494(12) . ?
C56 C57 1.499(12) . ?
C57 O5 1.427(10) . ?
C57 C58 1.499(13) . ?
C59 O6 1.425(10) . ?
C60 C61 1.408(11) . ?
C60 C65 1.415(12) . ?
C60 Si3 1.841(8) . ?
C61 C62 1.413(12) . ?
C62 C63 1.380(12) . ?
C63 C64 1.366(12) . ?
C64 C65 1.413(11) . ?
C66 C71 1.372(12) . ?
C66 C67 1.374(12) . ?
C66 Si3 1.906(9) . ?
C67 C68 1.371(11) . ?
C68 C69 1.420(12) . ?
C69 C70 1.377(12) . ?
C70 C71 1.384(11) . ?
C72 C73 1.513(12) . ?
C72 C74 1.542(12) . ?
C72 C75 1.547(12) . ?
C72 Si3 1.886(8) . ?
C76 N12 1.311(13) . ?
C76 N10 1.357(10) . ?
C77 N11 1.319(11) . ?
C77 N12 1.370(12) . ?
C78 N10 1.457(11) . ?
C78 C79 1.512(12) . ?
C79 O7 1.435(9) . ?
C79 C80 1.566(11) . ?
C80 C81 1.533(11) . ?
C81 C84 1.487(11) . ?
C81 C82 1.524(11) . ?
C82 O7 1.399(10) . ?
C82 C83 1.553(12) . ?
C84 O8 1.413(9) . ?
C85 C86 1.371(12) . ?
C85 C90 1.382(10) . ?
C85 Si4 1.879(8) . ?
C86 C87 1.384(11) . ?
C87 C88 1.438(11) . ?
C88 C89 1.356(12) . ?
C89 C90 1.418(11) . ?
C91 C92 1.388(11) . ?
C91 C96 1.398(11) . ?
C91 Si4 1.899(8) . ?
C92 C93 1.376(11) . ?
C93 C94 1.412(12) . ?
C94 C95 1.367(12) . ?
C95 C96 1.406(12) . ?
C97 C98 1.490(13) . ?
C97 C99 1.522(12) . ?
C97 C100 1.534(12) . ?
C97 Si4 1.882(9) . ?
N1 N2 1.376(9) . ?
N4 N5 1.361(9) . ?
N7 N8 1.367(9) . ?
N10 N11 1.326(11) . ?
O2 Si1 1.649(6) . ?
O4 Si2 1.653(6) . ?
O6 Si3 1.636(6) . ?
O8 Si4 1.646(5) . ?

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
N2 C1 N3 117.7(7) . . ?
N1 C2 N3 110.5(7) . . ?
C4 C3 N1 113.8(8) . . ?
O1 C4 C3 110.2(8) . . ?
O1 C4 C7 104.2(7) . . ?
C3 C4 C7 113.1(10) . . ?
C6 C5 O1 108.9(7) . . ?
C6 C5 C8 115.4(10) . . ?
O1 C5 C8 105.3(7) . . ?
C4 C7 C8 103.4(8) . . ?
C9 C8 C5 116.3(8) . . ?
C9 C8 C7 111.4(8) . . ?
C5 C8 C7 98.7(8) . . ?
O2 C9 C8 109.8(7) . . ?
C11 C10 C15 120.2(8) . . ?
C12 C11 C10 122.4(9) . . ?
C11 C12 C13 119.1(9) . . ?
C12 C13 C14 120.2(9) . . ?
C13 C14 C15 120.8(9) . . ?
C10 C15 C14 117.3(8) . . ?
C10 C15 Si1 122.9(7) . . ?
C14 C15 Si1 119.7(6) . . ?
C17 C16 C21 117.2(8) . . ?
C17 C16 Si1 120.1(7) . . ?
C21 C16 Si1 122.5(7) . . ?
C18 C17 C16 121.3(10) . . ?
C19 C18 C17 121.0(10) . . ?
C18 C19 C20 119.7(9) . . ?
C21 C20 C19 119.7(10) . . ?
C20 C21 C16 121.0(10) . . ?
C25 C22 C24 106.6(8) . . ?
C25 C22 C23 107.1(8) . . ?
C24 C22 C23 108.9(8) . . ?
C25 C22 Si1 112.1(6) . . ?
C24 C22 Si1 112.6(6) . . ?
C23 C22 Si1 109.3(6) . . ?
N5 C26 N6 114.9(8) . . ?
N4 C27 N6 110.5(8) . . ?
N4 C28 C29 112.9(7) . . ?
O3 C29 C28 112.5(7) . . ?
O3 C29 C30 106.1(7) . . ?
C28 C29 C30 112.3(8) . . ?
C31 C30 C29 104.1(7) . . ?
C32 C31 C30 102.4(7) . . ?
C32 C31 C34 114.5(7) . . ?
C30 C31 C34 112.9(7) . . ?
O3 C32 C33 106.4(7) . . ?
O3 C32 C31 105.4(7) . . ?
C33 C32 C31 118.5(7) . . ?
O4 C34 C31 110.1(6) . . ?
C36 C35 C40 116.4(8) . . ?
C36 C35 Si2 120.9(7) . . ?
C40 C35 Si2 122.8(7) . . ?
C35 C36 C37 124.2(9) . . ?
C38 C37 C36 117.0(9) . . ?
C37 C38 C39 121.6(8) . . ?
C40 C39 C38 119.3(9) . . ?
C39 C40 C35 121.5(9) . . ?
C42 C41 C46 114.9(8) . . ?
C42 C41 Si2 120.7(6) . . ?
C46 C41 Si2 124.1(7) . . ?
C43 C42 C41 124.8(8) . . ?
C44 C43 C42 117.8(8) . . ?
C43 C44 C45 119.3(8) . . ?
C46 C45 C44 121.8(8) . . ?
C45 C46 C41 121.3(8) . . ?
C49 C47 C48 106.8(8) . . ?
C49 C47 C50 110.0(7) . . ?
C48 C47 C50 108.7(8) . . ?
C49 C47 Si2 109.8(6) . . ?
C48 C47 Si2 111.5(6) . . ?
C50 C47 Si2 110.0(6) . . ?
N9 C51 N7 111.5(7) . . ?
N8 C52 N9 116.2(7) . . ?
C54 C53 N7 114.3(8) . . ?
O5 C54 C53 113.6(8) . . ?
O5 C54 C55 105.5(7) . . ?
C53 C54 C55 113.5(8) . . ?
C54 C55 C56 103.0(8) . . ?
C59 C56 C57 118.2(7) . . ?
C59 C56 C55 113.1(8) . . ?
C57 C56 C55 98.7(8) . . ?
O5 C57 C56 107.8(6) . . ?
O5 C57 C58 109.9(8) . . ?
C56 C57 C58 113.8(9) . . ?
O6 C59 C56 111.8(7) . . ?
C61 C60 C65 115.3(7) . . ?
C61 C60 Si3 123.8(6) . . ?
C65 C60 Si3 120.8(6) . . ?
C60 C61 C62 123.1(8) . . ?
C63 C62 C61 119.2(8) . . ?
C64 C63 C62 119.9(8) . . ?
C63 C64 C65 121.0(8) . . ?
C64 C65 C60 121.3(8) . . ?
C71 C66 C67 118.4(8) . . ?
C71 C66 Si3 120.6(7) . . ?
C67 C66 Si3 120.8(6) . . ?
C68 C67 C66 121.5(8) . . ?
C67 C68 C69 121.2(8) . . ?
C70 C69 C68 115.7(8) . . ?
C69 C70 C71 122.7(8) . . ?
C66 C71 C70 120.5(8) . . ?
C73 C72 C74 108.3(7) . . ?
C73 C72 C75 107.8(7) . . ?
C74 C72 C75 111.0(8) . . ?
C73 C72 Si3 108.6(6) . . ?
C74 C72 Si3 111.2(5) . . ?
C75 C72 Si3 109.8(6) . . ?
N12 C76 N10 102.1(8) . . ?
N11 C77 N12 101.9(8) . . ?
N10 C78 C79 113.0(7) . . ?
O7 C79 C78 111.4(7) . . ?
O7 C79 C80 106.1(7) . . ?
C78 C79 C80 111.4(7) . . ?
C81 C80 C79 103.2(6) . . ?
C84 C81 C82 118.6(7) . . ?
C84 C81 C80 111.2(6) . . ?
C82 C81 C80 98.9(7) . . ?
O7 C82 C81 108.0(6) . . ?
O7 C82 C83 109.0(7) . . ?
C81 C82 C83 114.1(7) . . ?
O8 C84 C81 110.9(6) . . ?
C86 C85 C90 116.9(8) . . ?
C86 C85 Si4 120.4(6) . . ?
C90 C85 Si4 122.6(6) . . ?
C85 C86 C87 124.6(8) . . ?
C86 C87 C88 116.5(8) . . ?
C89 C88 C87 121.1(8) . . ?
C88 C89 C90 118.8(8) . . ?
C85 C90 C89 122.2(8) . . ?
C92 C91 C96 117.9(7) . . ?
C92 C91 Si4 121.5(6) . . ?
C96 C91 Si4 120.1(6) . . ?
C93 C92 C91 122.7(8) . . ?
C92 C93 C94 118.1(8) . . ?
C95 C94 C93 121.0(8) . . ?
C94 C95 C96 119.6(8) . . ?
C91 C96 C95 120.6(8) . . ?
C98 C97 C99 109.4(8) . . ?
C98 C97 C100 109.8(8) . . ?
C99 C97 C100 105.1(7) . . ?
C98 C97 Si4 111.0(6) . . ?
C99 C97 Si4 108.2(6) . . ?
C100 C97 Si4 113.2(6) . . ?
C2 N1 N2 110.3(7) . . ?
C2 N1 C3 128.3(7) . . ?
N2 N1 C3 121.4(7) . . ?
C1 N2 N1 100.7(7) . . ?
C1 N3 C2 100.8(6) . . ?
C27 N4 N5 109.7(7) . . ?
C27 N4 C28 131.3(7) . . ?
N5 N4 C28 118.9(7) . . ?
C26 N5 N4 102.1(7) . . ?
C27 N6 C26 102.6(7) . . ?
C51 N7 N8 107.7(7) . . ?
C51 N7 C53 131.0(7) . . ?
N8 N7 C53 121.3(7) . . ?
C52 N8 N7 103.1(7) . . ?
C51 N9 C52 101.4(7) . . ?
N11 N10 C76 110.2(7) . . ?
N11 N10 C78 131.6(8) . . ?
C76 N10 C78 118.2(7) . . ?
C77 N11 N10 110.8(8) . . ?
C76 N12 C77 115.1(9) . . ?
C4 O1 C5 110.4(6) . . ?
C9 O2 Si1 122.3(5) . . ?
C32 O3 C29 108.8(6) . . ?
C34 O4 Si2 122.4(5) . . ?
C54 O5 C57 108.6(6) . . ?
C59 O6 Si3 122.6(5) . . ?
C82 O7 C79 108.4(6) . . ?
C84 O8 Si4 122.2(4) . . ?
O2 Si1 C22 104.0(3) . . ?
O2 Si1 C15 110.1(4) . . ?
C22 Si1 C15 109.2(4) . . ?
O2 Si1 C16 108.3(3) . . ?
C22 Si1 C16 113.5(4) . . ?
C15 Si1 C16 111.5(4) . . ?
O4 Si2 C41 109.3(3) . . ?
O4 Si2 C35 107.4(3) . . ?
C41 Si2 C35 110.2(4) . . ?
O4 Si2 C47 104.6(3) . . ?
C41 Si2 C47 109.7(4) . . ?
C35 Si2 C47 115.3(4) . . ?
O6 Si3 C60 110.9(3) . . ?
O6 Si3 C72 104.1(3) . . ?
C60 Si3 C72 109.3(4) . . ?
O6 Si3 C66 108.5(3) . . ?
C60 Si3 C66 109.8(4) . . ?
C72 Si3 C66 114.0(4) . . ?
O8 Si4 C85 109.2(3) . . ?
O8 Si4 C97 105.4(3) . . ?
C85 Si4 C97 110.3(4) . . ?
O8 Si4 C91 109.3(3) . . ?
C85 Si4 C91 109.4(3) . . ?
C97 Si4 C91 113.1(4) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.193
####################################################################### 
# 
# 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_sn_jh_610_0m
_database_code_depnum_ccdc_archive 'CCDC 1528322'
_audit_update_record             
;
2017-01-18 deposited with the CCDC.
2018-03-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H34 O3 Si'
_chemical_formula_sum            'C27 H34 O3 Si'
_chemical_formula_weight         434.63

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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'

_cell_length_a                   8.2816(14)
_cell_length_b                   11.7445(19)
_cell_length_c                   25.888(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2517.9(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    29078
_cell_measurement_theta_min      1.57
_cell_measurement_theta_max      24.99

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9769
_exptl_absorpt_correction_T_max  0.9884
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'bruker smart apex II CCD'
_diffrn_measurement_method       '\ w scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29078
_diffrn_reflns_av_R_equivalents  0.1226
_diffrn_reflns_av_sigmaI/netI    0.0817
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.57
_diffrn_reflns_theta_max         24.99
_reflns_number_total             4417
_reflns_number_gt                2488
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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 > 2σ(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     
'calc w=1/[σ²(Fo²)+(0.0587P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0078(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.10(19)
_refine_ls_number_reflns         4417
_refine_ls_number_parameters     286
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1160
_refine_ls_R_factor_gt           0.0568
_refine_ls_wR_factor_ref         0.1396
_refine_ls_wR_factor_gt          0.1161
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_restrained_S_all      0.981
_refine_ls_shift/su_max          0.007
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0971(5) 1.3231(4) 0.93703(16) 0.0645(11) Uani 1 1 d . . .
C2 C 0.1390(5) 1.2039(3) 0.93097(15) 0.0660(12) Uani 1 1 d . . .
H2 H 0.0646 1.1450 0.9277 0.079 Uiso 1 1 calc R . .
C3 C 0.3001(5) 1.1904(3) 0.93075(15) 0.0611(11) Uani 1 1 d . . .
C4 C 0.3886(5) 1.3013(3) 0.93702(15) 0.0622(11) Uani 1 1 d . . .
H4 H 0.4421 1.3014 0.9708 0.075 Uiso 1 1 calc R . .
C5 C 0.2527(5) 1.3909(3) 0.93788(16) 0.0724(12) Uani 1 1 d . . .
H5A H 0.2591 1.4371 0.9689 0.087 Uiso 1 1 calc R . .
H5B H 0.2596 1.4403 0.9079 0.087 Uiso 1 1 calc R . .
C6 C 0.5167(5) 1.3130(3) 0.89543(16) 0.0664(11) Uani 1 1 d . . .
H6A H 0.5817 1.3801 0.9023 0.080 Uiso 1 1 calc R . .
H6B H 0.4647 1.3232 0.8622 0.080 Uiso 1 1 calc R . .
C7 C 0.6263(4) 1.2079(3) 0.89340(15) 0.0609(10) Uani 1 1 d . . .
H7 H 0.7041 1.2180 0.8652 0.073 Uiso 1 1 calc R . .
C8 C 0.5292(4) 1.1004(3) 0.88300(15) 0.0552(10) Uani 1 1 d . . .
H8 H 0.4742 1.1119 0.8499 0.066 Uiso 1 1 calc R . .
C9 C 0.3969(5) 1.0851(3) 0.92380(16) 0.0638(11) Uani 1 1 d . . .
H9A H 0.3261 1.0234 0.9135 0.077 Uiso 1 1 calc R . .
H9B H 0.4462 1.0644 0.9565 0.077 Uiso 1 1 calc R . .
C10 C 0.6266(4) 0.9899(3) 0.87800(15) 0.0589(10) Uani 1 1 d . . .
H10 H 0.6397 0.9567 0.9125 0.071 Uiso 1 1 calc R . .
C11 C 0.7918(5) 1.0030(4) 0.85380(18) 0.0843(14) Uani 1 1 d . . .
H11A H 0.8383 0.9292 0.8482 0.126 Uiso 1 1 calc R . .
H11B H 0.8600 1.0463 0.8765 0.126 Uiso 1 1 calc R . .
H11C H 0.7818 1.0420 0.8213 0.126 Uiso 1 1 calc R . .
C12 C 0.6874(5) 0.7338(4) 0.79260(17) 0.0653(11) Uani 1 1 d . . .
C13 C 0.7367(5) 0.8143(4) 0.75588(17) 0.0767(13) Uani 1 1 d . . .
H13 H 0.6988 0.8884 0.7592 0.092 Uiso 1 1 calc R . .
C14 C 0.8370(6) 0.7902(5) 0.71566(19) 0.0916(15) Uani 1 1 d . . .
H14 H 0.8659 0.8463 0.6920 0.110 Uiso 1 1 calc R . .
C15 C 0.8947(7) 0.6808(6) 0.7109(2) 0.107(2) Uani 1 1 d . . .
H15 H 0.9650 0.6634 0.6840 0.128 Uiso 1 1 calc R . .
C16 C 0.8513(7) 0.5982(5) 0.7443(2) 0.1036(19) Uani 1 1 d . . .
H16 H 0.8912 0.5247 0.7403 0.124 Uiso 1 1 calc R . .
C17 C 0.7458(6) 0.6235(4) 0.78512(19) 0.0856(14) Uani 1 1 d . . .
H17 H 0.7143 0.5659 0.8076 0.103 Uiso 1 1 calc R . .
C18 C 0.5633(5) 0.7086(3) 0.90612(16) 0.0649(11) Uani 1 1 d . . .
C19 C 0.6807(6) 0.6289(4) 0.9186(2) 0.0854(15) Uani 1 1 d . . .
H19 H 0.7566 0.6092 0.8937 0.102 Uiso 1 1 calc R . .
C20 C 0.6896(7) 0.5773(4) 0.9669(2) 0.1019(18) Uani 1 1 d . . .
H20 H 0.7683 0.5227 0.9735 0.122 Uiso 1 1 calc R . .
C21 C 0.5841(8) 0.6065(5) 1.0040(2) 0.0981(17) Uani 1 1 d . . .
H21 H 0.5901 0.5719 1.0363 0.118 Uiso 1 1 calc R . .
C22 C 0.4685(7) 0.6863(5) 0.9948(2) 0.1085(18) Uani 1 1 d . . .
H22 H 0.3970 0.7075 1.0208 0.130 Uiso 1 1 calc R . .
C23 C 0.4585(6) 0.7360(4) 0.94601(19) 0.0959(15) Uani 1 1 d . . .
H23 H 0.3782 0.7897 0.9400 0.115 Uiso 1 1 calc R . .
C24 C 0.3275(5) 0.7390(4) 0.81256(17) 0.0663(12) Uani 1 1 d . . .
C25 C 0.3192(6) 0.7889(5) 0.75846(17) 0.1007(17) Uani 1 1 d . . .
H25A H 0.2124 0.7788 0.7448 0.151 Uiso 1 1 calc R . .
H25B H 0.3957 0.7508 0.7366 0.151 Uiso 1 1 calc R . .
H25C H 0.3442 0.8687 0.7598 0.151 Uiso 1 1 calc R . .
C26 C 0.1878(5) 0.7862(5) 0.8439(2) 0.1119(18) Uani 1 1 d . . .
H26A H 0.2043 0.8660 0.8497 0.168 Uiso 1 1 calc R . .
H26B H 0.1820 0.7472 0.8764 0.168 Uiso 1 1 calc R . .
H26C H 0.0888 0.7751 0.8253 0.168 Uiso 1 1 calc R . .
C27 C 0.3103(6) 0.6088(4) 0.8091(2) 0.1093(19) Uani 1 1 d . . .
H27A H 0.3868 0.5795 0.7846 0.164 Uiso 1 1 calc R . .
H27B H 0.2029 0.5899 0.7981 0.164 Uiso 1 1 calc R . .
H27C H 0.3304 0.5758 0.8424 0.164 Uiso 1 1 calc R . .
O1 O -0.0397(4) 1.3636(3) 0.93975(12) 0.0904(10) Uani 1 1 d . . .
O2 O 0.5276(3) 0.91477(19) 0.84765(10) 0.0579(7) Uani 1 1 d . . .
O3 O 0.7133(3) 1.1931(2) 0.94030(11) 0.0739(8) Uani 1 1 d . . .
H3 H 0.7817 1.2433 0.9429 0.111 Uiso 1 1 calc R . .
Si1 Si 0.53118(13) 0.77567(9) 0.84165(5) 0.0596(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.231(5) . ?
C1 C2 1.451(5) . ?
C1 C5 1.514(6) . ?
C2 C3 1.344(5) . ?
C2 H2 0.9300 . ?
C3 C9 1.485(5) . ?
C3 C4 1.504(5) . ?
C4 C6 1.517(5) . ?
C4 C5 1.541(5) . ?
C4 H4 0.9800 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.534(5) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 O3 1.422(4) . ?
C7 C8 1.521(5) . ?
C7 H7 0.9800 . ?
C8 C9 1.532(5) . ?
C8 C10 1.534(5) . ?
C8 H8 0.9800 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 O2 1.438(4) . ?
C10 C11 1.512(5) . ?
C10 H10 0.9800 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C17 1.396(6) . ?
C12 C13 1.402(6) . ?
C12 Si1 1.878(4) . ?
C13 C14 1.362(6) . ?
C13 H13 0.9300 . ?
C14 C15 1.376(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.348(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.403(7) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C23 1.387(6) . ?
C18 C19 1.388(5) . ?
C18 Si1 1.865(4) . ?
C19 C20 1.391(7) . ?
C19 H19 0.9300 . ?
C20 C21 1.344(7) . ?
C20 H20 0.9300 . ?
C21 C22 1.360(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.394(6) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 C26 1.518(6) . ?
C24 C25 1.520(6) . ?
C24 C27 1.538(6) . ?
C24 Si1 1.897(4) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
O2 Si1 1.641(3) . ?
O3 H3 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 126.8(4) . . ?
O1 C1 C5 125.4(4) . . ?
C2 C1 C5 107.8(4) . . ?
C3 C2 C1 110.6(4) . . ?
C3 C2 H2 124.7 . . ?
C1 C2 H2 124.7 . . ?
C2 C3 C9 129.4(4) . . ?
C2 C3 C4 112.4(4) . . ?
C9 C3 C4 118.2(3) . . ?
C3 C4 C6 110.0(3) . . ?
C3 C4 C5 103.7(3) . . ?
C6 C4 C5 117.3(3) . . ?
C3 C4 H4 108.5 . . ?
C6 C4 H4 108.5 . . ?
C5 C4 H4 108.5 . . ?
C1 C5 C4 105.2(3) . . ?
C1 C5 H5A 110.7 . . ?
C4 C5 H5A 110.7 . . ?
C1 C5 H5B 110.7 . . ?
C4 C5 H5B 110.7 . . ?
H5A C5 H5B 108.8 . . ?
C4 C6 C7 111.4(3) . . ?
C4 C6 H6A 109.3 . . ?
C7 C6 H6A 109.3 . . ?
C4 C6 H6B 109.3 . . ?
C7 C6 H6B 109.3 . . ?
H6A C6 H6B 108.0 . . ?
O3 C7 C8 108.5(3) . . ?
O3 C7 C6 111.6(3) . . ?
C8 C7 C6 111.2(3) . . ?
O3 C7 H7 108.5 . . ?
C8 C7 H7 108.5 . . ?
C6 C7 H7 108.5 . . ?
C7 C8 C9 110.7(3) . . ?
C7 C8 C10 116.0(3) . . ?
C9 C8 C10 109.6(3) . . ?
C7 C8 H8 106.7 . . ?
C9 C8 H8 106.7 . . ?
C10 C8 H8 106.7 . . ?
C3 C9 C8 111.8(3) . . ?
C3 C9 H9A 109.3 . . ?
C8 C9 H9A 109.3 . . ?
C3 C9 H9B 109.3 . . ?
C8 C9 H9B 109.3 . . ?
H9A C9 H9B 107.9 . . ?
O2 C10 C11 110.6(3) . . ?
O2 C10 C8 105.4(3) . . ?
C11 C10 C8 115.1(3) . . ?
O2 C10 H10 108.5 . . ?
C11 C10 H10 108.5 . . ?
C8 C10 H10 108.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C17 C12 C13 115.5(4) . . ?
C17 C12 Si1 125.1(4) . . ?
C13 C12 Si1 118.9(3) . . ?
C14 C13 C12 123.8(5) . . ?
C14 C13 H13 118.1 . . ?
C12 C13 H13 118.1 . . ?
C13 C14 C15 118.3(5) . . ?
C13 C14 H14 120.8 . . ?
C15 C14 H14 120.8 . . ?
C16 C15 C14 121.4(6) . . ?
C16 C15 H15 119.3 . . ?
C14 C15 H15 119.3 . . ?
C15 C16 C17 119.8(5) . . ?
C15 C16 H16 120.1 . . ?
C17 C16 H16 120.1 . . ?
C12 C17 C16 121.1(5) . . ?
C12 C17 H17 119.4 . . ?
C16 C17 H17 119.4 . . ?
C23 C18 C19 114.9(4) . . ?
C23 C18 Si1 118.6(3) . . ?
C19 C18 Si1 126.4(4) . . ?
C18 C19 C20 122.7(5) . . ?
C18 C19 H19 118.6 . . ?
C20 C19 H19 118.6 . . ?
C21 C20 C19 119.8(5) . . ?
C21 C20 H20 120.1 . . ?
C19 C20 H20 120.1 . . ?
C20 C21 C22 120.5(5) . . ?
C20 C21 H21 119.7 . . ?
C22 C21 H21 119.7 . . ?
C21 C22 C23 119.3(5) . . ?
C21 C22 H22 120.4 . . ?
C23 C22 H22 120.4 . . ?
C18 C23 C22 122.7(5) . . ?
C18 C23 H23 118.7 . . ?
C22 C23 H23 118.7 . . ?
C26 C24 C25 108.5(4) . . ?
C26 C24 C27 108.9(4) . . ?
C25 C24 C27 109.0(4) . . ?
C26 C24 Si1 112.5(3) . . ?
C25 C24 Si1 108.6(3) . . ?
C27 C24 Si1 109.4(3) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C10 O2 Si1 130.7(2) . . ?
C7 O3 H3 109.5 . . ?
O2 Si1 C18 109.78(16) . . ?
O2 Si1 C12 109.71(18) . . ?
C18 Si1 C12 113.34(19) . . ?
O2 Si1 C24 104.33(17) . . ?
C18 Si1 C24 112.72(19) . . ?
C12 Si1 C24 106.53(19) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 -178.5(4) . . . . ?
C5 C1 C2 C3 3.2(5) . . . . ?
C1 C2 C3 C9 -177.7(4) . . . . ?
C1 C2 C3 C4 0.3(5) . . . . ?
C2 C3 C4 C6 -129.8(4) . . . . ?
C9 C3 C4 C6 48.4(5) . . . . ?
C2 C3 C4 C5 -3.5(5) . . . . ?
C9 C3 C4 C5 174.7(3) . . . . ?
O1 C1 C5 C4 176.5(4) . . . . ?
C2 C1 C5 C4 -5.2(4) . . . . ?
C3 C4 C5 C1 5.1(4) . . . . ?
C6 C4 C5 C1 126.6(4) . . . . ?
C3 C4 C6 C7 -52.0(4) . . . . ?
C5 C4 C6 C7 -170.2(3) . . . . ?
C4 C6 C7 O3 -62.7(4) . . . . ?
C4 C6 C7 C8 58.7(4) . . . . ?
O3 C7 C8 C9 66.5(4) . . . . ?
C6 C7 C8 C9 -56.6(4) . . . . ?
O3 C7 C8 C10 -59.1(4) . . . . ?
C6 C7 C8 C10 177.7(3) . . . . ?
C2 C3 C9 C8 130.2(5) . . . . ?
C4 C3 C9 C8 -47.7(5) . . . . ?
C7 C8 C9 C3 50.0(4) . . . . ?
C10 C8 C9 C3 179.2(3) . . . . ?
C7 C8 C10 O2 -155.9(3) . . . . ?
C9 C8 C10 O2 77.8(4) . . . . ?
C7 C8 C10 C11 -33.8(5) . . . . ?
C9 C8 C10 C11 -160.1(3) . . . . ?
C17 C12 C13 C14 -1.1(6) . . . . ?
Si1 C12 C13 C14 -173.4(3) . . . . ?
C12 C13 C14 C15 -0.6(7) . . . . ?
C13 C14 C15 C16 1.3(8) . . . . ?
C14 C15 C16 C17 -0.3(8) . . . . ?
C13 C12 C17 C16 2.1(6) . . . . ?
Si1 C12 C17 C16 173.9(4) . . . . ?
C15 C16 C17 C12 -1.5(8) . . . . ?
C23 C18 C19 C20 2.1(6) . . . . ?
Si1 C18 C19 C20 -175.5(4) . . . . ?
C18 C19 C20 C21 -1.8(8) . . . . ?
C19 C20 C21 C22 0.0(8) . . . . ?
C20 C21 C22 C23 1.3(9) . . . . ?
C19 C18 C23 C22 -0.8(7) . . . . ?
Si1 C18 C23 C22 177.0(4) . . . . ?
C21 C22 C23 C18 -0.8(8) . . . . ?
C11 C10 O2 Si1 75.0(4) . . . . ?
C8 C10 O2 Si1 -160.0(2) . . . . ?
C10 O2 Si1 C18 41.8(3) . . . . ?
C10 O2 Si1 C12 -83.4(3) . . . . ?
C10 O2 Si1 C24 162.8(3) . . . . ?
C23 C18 Si1 O2 54.9(4) . . . . ?
C19 C18 Si1 O2 -127.5(4) . . . . ?
C23 C18 Si1 C12 178.0(3) . . . . ?
C19 C18 Si1 C12 -4.4(4) . . . . ?
C23 C18 Si1 C24 -60.9(4) . . . . ?
C19 C18 Si1 C24 116.7(4) . . . . ?
C17 C12 Si1 O2 166.5(3) . . . . ?
C13 C12 Si1 O2 -22.0(4) . . . . ?
C17 C12 Si1 C18 43.4(4) . . . . ?
C13 C12 Si1 C18 -145.0(3) . . . . ?
C17 C12 Si1 C24 -81.1(4) . . . . ?
C13 C12 Si1 C24 90.4(4) . . . . ?
C26 C24 Si1 O2 -54.3(4) . . . . ?
C25 C24 Si1 O2 65.8(3) . . . . ?
C27 C24 Si1 O2 -175.4(3) . . . . ?
C26 C24 Si1 C18 64.8(4) . . . . ?
C25 C24 Si1 C18 -175.2(3) . . . . ?
C27 C24 Si1 C18 -56.3(4) . . . . ?
C26 C24 Si1 C12 -170.3(4) . . . . ?
C25 C24 Si1 C12 -50.2(4) . . . . ?
C27 C24 Si1 C12 68.6(4) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.160
_refine_diff_density_min         -0.157
_refine_diff_density_rms         0.037
