 
data_IV-68-12 
  
_audit_creation_method            'SHELXL-2016/6' 
_shelx_SHELXL_version_number      '2016/6' 
_chemical_name_systematic         ? 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety 
 'C33 H44 N4 O4 S Si, C H4 O' 
_chemical_formula_sum 
 'C34 H48 N4 O5 S Si' 
_chemical_formula_weight          652.91 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0181   0.0091 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0311   0.0180 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0492   0.0322 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Si'  'Si'   0.2541   0.3302 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'S'  'S'   0.3331   0.5567 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_space_group_crystal_system       monoclinic 
_space_group_IT_number            4 
_space_group_name_H-M_alt         'P 21' 
_space_group_name_Hall            'P 2yb' 
  
_shelx_space_group_comment 
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
; 
  
loop_ 
 _space_group_symop_operation_xyz 
 'x, y, z' 
 '-x, y+1/2, -z' 
  
_cell_length_a                    7.9317(5) 
_cell_length_b                    15.4939(11) 
_cell_length_c                    13.8939(11) 
_cell_angle_alpha                 90 
_cell_angle_beta                  92.123(4) 
_cell_angle_gamma                 90 
_cell_volume                      1706.3(2) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     9924 
_cell_measurement_theta_min       3.18
_cell_measurement_theta_max       79.18
  
_exptl_crystal_description        needle 
_exptl_crystal_colour             colourless 
_exptl_crystal_density_meas       . 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_density_diffrn     1.271 
_exptl_crystal_F_000              700 
_exptl_transmission_factor_min    ? 
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.391 
_exptl_crystal_size_mid           0.033 
_exptl_crystal_size_min           0.022 
_exptl_absorpt_coefficient_mu     1.552 
_shelx_estimated_absorpt_T_min    0.582 
_shelx_estimated_absorpt_T_max    0.967 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.5696 
_exptl_absorpt_correction_T_max   0.7543
_exptl_absorpt_process_details    'SADABS (Herbst-Irmer et al., 2015)' 
_exptl_absorpt_special_details    ? 
_exptl_special_details 
; 
 Bruker D8 Venture Kappa DUO four-circle diffractometer, Bruker Photon2 CPAD.  
; 
_diffrn_ambient_temperature       100(2) 
_diffrn_radiation_wavelength      1.54178 
_diffrn_radiation_type            CuK\a 
_diffrn_source                    'I\mS micro-focus sealed tube, multilayer optics' 
_diffrn_measurement_device_type   'Bruker Photon2 CPAD' 
_diffrn_measurement_method        'φ and ω scans' 
_diffrn_detector_area_resol_mean  7.4 
_diffrn_reflns_number             22916 
_diffrn_reflns_av_unetI/netI      0.0691 
_diffrn_reflns_av_R_equivalents   0.0794 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -18 
_diffrn_reflns_limit_k_max        15 
_diffrn_reflns_limit_l_min        -16 
_diffrn_reflns_limit_l_max        16 
_diffrn_reflns_theta_min          3.183 
_diffrn_reflns_theta_max          68.231 
_diffrn_reflns_theta_full         67.679 
_diffrn_measured_fraction_theta_max   0.996 
_diffrn_measured_fraction_theta_full  0.996 
_diffrn_reflns_Laue_measured_fraction_max    0.996 
_diffrn_reflns_Laue_measured_fraction_full   0.996 
_diffrn_reflns_point_group_measured_fraction_max   0.868 
_diffrn_reflns_point_group_measured_fraction_full  0.869 
_reflns_number_total              5423 
_reflns_number_gt                 4396 
_reflns_threshold_expression      'I > 2σ(I)' 
_reflns_Friedel_coverage          0.676 
_reflns_Friedel_fraction_max      0.729 
_reflns_Friedel_fraction_full     0.731 
  
_reflns_special_details 
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
 
 Data collection was challenging due to the needle shape of the 
 crystal, ice buildup, and twinning. A high-resolution cutoff 
 of 0.83 A was applied to the data prior to refinement.
; 
  
_computing_data_collection        'APEX3 v2017.3.0 (Bruker-AXS, 2017)' 
_computing_cell_refinement        'SAINT 8.38A (Bruker-AXS, 2017)' 
_computing_data_reduction         'SAINT 8.38A (Bruker-AXS, 2017)' 
_computing_structure_solution     'SHELXT-2015 (Sheldrick, 2015)' 
_computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' 
_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 > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 Comments on checkCIF errors:
 
 Errors associated with close internuclear contacts are due to disorder 
 of the minor component of the methanol molecule and are expected. 
 The data is not of the highest quality due to the nature of the crystal 
 and ice buildup. As a result, C-C bond precision is compromised.
 
; 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
'w=1/[σ²(Fo²)+(0.1146P)²+0.5462P] 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-2016/6 (Sheldrick 2016)' 
_refine_ls_extinction_coef        0.0050(10) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_abs_structure_details 
; 
 Flack x determined using 1415 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
; 
_refine_ls_abs_structure_Flack    0.061(16) 
_chemical_absolute_configuration  syn 
_refine_ls_number_reflns          5423 
_refine_ls_number_parameters      437 
_refine_ls_number_restraints      3 
_refine_ls_R_factor_all           0.0794 
_refine_ls_R_factor_gt            0.0665 
_refine_ls_wR_factor_ref          0.1861 
_refine_ls_wR_factor_gt           0.1736 
_refine_ls_goodness_of_fit_ref    1.067 
_refine_ls_restrained_S_all       1.067 
_refine_ls_shift/su_max           0.033 
_refine_ls_shift/su_mean          0.001 
  
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_site_symmetry_order 
 _atom_site_calc_flag 
 _atom_site_refinement_flags_posn 
 _atom_site_refinement_flags_adp 
 _atom_site_refinement_flags_occupancy 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
S1 S 1.00829(16) 0.53376(11) 0.78807(12) 0.0430(4) Uani 1 1 d . . . . . 
Si1 Si 1.2162(2) 0.76969(13) 0.94231(15) 0.0477(5) Uani 1 1 d . . . . . 
O1 O 0.2873(6) 0.4707(4) 0.3156(4) 0.0535(13) Uani 1 1 d . . . . . 
O2 O 0.3550(6) 0.1961(3) 0.6332(4) 0.0545(13) Uani 1 1 d . . . . . 
O3 O 1.0628(5) 0.5037(3) 0.6959(4) 0.0463(12) Uani 1 1 d . . . . . 
O4 O 1.0145(5) 0.4765(3) 0.8681(4) 0.0464(11) Uani 1 1 d . . . . . 
N1 N 0.4284(6) 0.4475(4) 0.5130(4) 0.0422(13) Uani 1 1 d . . . . . 
C2 C 0.5984(8) 0.4568(5) 0.4733(6) 0.0475(17) Uani 1 1 d . . . . . 
H2A H 0.585968 0.469252 0.403523 0.057 Uiso 1 1 calc R U . . . 
H2B H 0.659441 0.401329 0.480927 0.057 Uiso 1 1 calc R U . . . 
C3 C 0.7060(7) 0.5298(5) 0.5229(5) 0.0470(16) Uani 1 1 d . . . . . 
H3A H 0.824664 0.510614 0.531839 0.056 Uiso 1 1 calc R U . . . 
H3B H 0.703799 0.582000 0.481863 0.056 Uiso 1 1 calc R U . . . 
C3A C 0.6331(7) 0.5507(4) 0.6210(5) 0.0398(15) Uani 1 1 d . . . . . 
C4 C 0.3355(7) 0.5994(5) 0.5484(5) 0.0421(15) Uani 1 1 d . . . . . 
C4A C 0.4821(7) 0.6089(5) 0.6058(5) 0.0417(16) Uani 1 1 d . . . . . 
C5 C 0.2156(8) 0.6652(5) 0.5445(5) 0.0449(16) Uani 1 1 d . . . . . 
H5 H 0.112952 0.657351 0.508128 0.054 Uiso 1 1 calc R U . . . 
C6 C 0.2449(8) 0.7412(5) 0.5927(6) 0.0497(18) Uani 1 1 d . . . . . 
H6 H 0.161472 0.785191 0.589374 0.060 Uiso 1 1 calc R U . . . 
C7 C 0.3957(8) 0.7557(5) 0.6473(6) 0.0482(18) Uani 1 1 d . . . . . 
H7 H 0.417669 0.809136 0.678791 0.058 Uiso 1 1 calc R U . . . 
C7A C 0.5107(7) 0.6881(5) 0.6527(5) 0.0419(16) Uani 1 1 d . . . . . 
N8 N 0.6657(6) 0.6873(4) 0.7029(5) 0.0464(15) Uani 1 1 d . . . . . 
C8 C 0.7578(8) 0.7642(5) 0.7316(6) 0.0529(18) Uani 1 1 d . . . . . 
H8A H 0.850778 0.773320 0.688217 0.079 Uiso 1 1 calc R U . . . 
H8B H 0.803128 0.757299 0.797702 0.079 Uiso 1 1 calc R U . . . 
H8C H 0.681728 0.814030 0.728291 0.079 Uiso 1 1 calc R U . . . 
C8A C 0.7569(7) 0.6077(4) 0.6833(5) 0.0425(16) Uani 1 1 d . . . . . 
H8A1 H 0.858161 0.621530 0.645390 0.051 Uiso 1 1 calc R U . . . 
C9 C 0.3086(7) 0.5170(4) 0.4891(5) 0.0408(15) Uani 1 1 d . . . . . 
H9 H 0.192815 0.494983 0.501339 0.049 Uiso 1 1 calc R U . . . 
C10 C 0.3133(8) 0.5409(5) 0.3842(5) 0.0487(17) Uani 1 1 d . . . . . 
H10 H 0.405285 0.581982 0.368155 0.058 Uiso 1 1 calc R U . . . 
C11 C 0.1675(8) 0.5400(6) 0.3141(5) 0.0510(17) Uani 1 1 d . . . . . 
C12 C 0.1742(11) 0.5980(7) 0.2288(7) 0.067(2) Uani 1 1 d . . . . . 
H12A H 0.291850 0.612962 0.217353 0.100 Uiso 1 1 calc R U . . . 
H12B H 0.110199 0.650799 0.240855 0.100 Uiso 1 1 calc R U . . . 
H12C H 0.124952 0.568527 0.172038 0.100 Uiso 1 1 calc R U . . . 
C13 C -0.0086(8) 0.5170(6) 0.3432(6) 0.060(2) Uani 1 1 d . . . . . 
H13A H -0.072272 0.492844 0.287728 0.091 Uiso 1 1 calc R U . . . 
H13B H -0.065660 0.568934 0.365667 0.091 Uiso 1 1 calc R U . . . 
H13C H -0.002184 0.474201 0.395210 0.091 Uiso 1 1 calc R U . . . 
N1X N 0.4519(6) 0.3322(4) 0.6304(5) 0.0445(14) Uani 1 1 d . . . . . 
C2X C 0.6136(8) 0.3087(5) 0.6768(6) 0.0489(18) Uani 1 1 d . . . . . 
H2X1 H 0.667361 0.260996 0.641683 0.059 Uiso 1 1 calc R U . . . 
H2X2 H 0.598837 0.290556 0.744290 0.059 Uiso 1 1 calc R U . . . 
C3X C 0.7199(7) 0.3911(4) 0.6727(6) 0.0424(15) Uani 1 1 d . . . . . 
H3X1 H 0.785745 0.392624 0.613549 0.051 Uiso 1 1 calc R U . . . 
H3X2 H 0.798426 0.395506 0.729563 0.051 Uiso 1 1 calc R U . . . 
C3AX C 0.5869(7) 0.4648(4) 0.6723(5) 0.0379(14) Uani 1 1 d . . . . . 
C4AX C 0.5541(7) 0.4839(4) 0.7788(5) 0.0389(15) Uani 1 1 d . . . . . 
C4X C 0.4196(7) 0.4495(5) 0.8296(5) 0.0458(17) Uani 1 1 d . . . . . 
H4X H 0.333810 0.416992 0.796741 0.055 Uiso 1 1 calc R U . . . 
C5X C 0.4129(8) 0.4634(5) 0.9284(6) 0.0508(18) Uani 1 1 d . . . . . 
H5X H 0.321618 0.440294 0.962506 0.061 Uiso 1 1 calc R U . . . 
C6X C 0.5367(8) 0.5100(5) 0.9776(6) 0.0508(19) Uani 1 1 d . . . . . 
H6X H 0.530854 0.519109 1.044991 0.061 Uiso 1 1 calc R U . . . 
C7X C 0.6702(7) 0.5437(5) 0.9272(5) 0.0462(16) Uani 1 1 d . . . . . 
H7X H 0.756987 0.575307 0.960419 0.055 Uiso 1 1 calc R U . . . 
C7AX C 0.6765(7) 0.5312(5) 0.8300(5) 0.0419(14) Uani 1 1 d . . . . . 
C8AX C 0.4337(8) 0.4256(4) 0.6151(5) 0.0418(16) Uani 1 1 d . . . . . 
H8AX H 0.327171 0.445614 0.644293 0.050 Uiso 1 1 calc R U . . . 
N8X N 0.8112(6) 0.5680(4) 0.7745(4) 0.0407(13) Uani 1 1 d . . . . . 
C1XX C 0.3320(8) 0.2733(6) 0.6134(6) 0.0520(18) Uani 1 1 d . . . . . 
C2XX C 0.1684(9) 0.3040(6) 0.5647(7) 0.065(2) Uani 1 1 d . . . . . 
H2X3 H 0.190287 0.323766 0.499374 0.097 Uiso 1 1 calc R U . . . 
H2X4 H 0.122125 0.351662 0.601794 0.097 Uiso 1 1 calc R U . . . 
H2X5 H 0.087224 0.256283 0.561591 0.097 Uiso 1 1 calc R U . . . 
C20 C 1.1272(7) 0.6287(5) 0.8167(5) 0.0441(16) Uani 1 1 d . . . . . 
H20A H 1.248749 0.614904 0.813405 0.053 Uiso 1 1 calc R U . . . 
H20B H 1.100480 0.673053 0.767172 0.053 Uiso 1 1 calc R U . . . 
C21 C 1.0960(8) 0.6666(5) 0.9147(5) 0.0448(16) Uani 1 1 d . . . . . 
H21A H 1.127322 0.623241 0.964476 0.054 Uiso 1 1 calc R U . . . 
H21B H 0.973834 0.678358 0.919044 0.054 Uiso 1 1 calc R U . . . 
C22 C 1.1866(11) 0.7965(6) 1.0703(6) 0.065(2) Uani 1 1 d . . . . . 
H22A H 1.240028 0.852132 1.085333 0.098 Uiso 1 1 calc R U . . . 
H22B H 1.238431 0.751498 1.111229 0.098 Uiso 1 1 calc R U . . . 
H22C H 1.065792 0.799946 1.082117 0.098 Uiso 1 1 calc R U . . . 
C23 C 1.1327(11) 0.8578(6) 0.8637(7) 0.067(2) Uani 1 1 d . . . . . 
H23A H 1.017473 0.871986 0.881458 0.100 Uiso 1 1 calc R U . . . 
H23B H 1.131886 0.839044 0.796372 0.100 Uiso 1 1 calc R U . . . 
H23C H 1.204525 0.908932 0.871907 0.100 Uiso 1 1 calc R U . . . 
C24 C 1.4428(9) 0.7525(6) 0.9223(7) 0.060(2) Uani 1 1 d . . . . . 
H24A H 1.455989 0.725398 0.859271 0.090 Uiso 1 1 calc R U . . . 
H24B H 1.490976 0.714901 0.972846 0.090 Uiso 1 1 calc R U . . . 
H24C H 1.501451 0.808200 0.924014 0.090 Uiso 1 1 calc R U . . . 
O30A O 0.3556(18) 0.1440(9) 0.8188(8) 0.120(5) Uani 0.785(13) 1 d D . P A 1 
H30A H 0.356079 0.147974 0.758492 0.180 Uiso 0.785(13) 1 calc DR U P A 1 
C30A C 0.2552(17) 0.2083(11) 0.8550(9) 0.084(4) Uani 0.785(13) 1 d D . P A 1 
H30B H 0.326788 0.253346 0.884555 0.125 Uiso 0.785(13) 1 calc R U P A 1 
H30C H 0.182441 0.183874 0.903499 0.125 Uiso 0.785(13) 1 calc R U P A 1 
H30D H 0.185243 0.233400 0.802494 0.125 Uiso 0.785(13) 1 calc R U P A 1 
O30B O 0.442(3) -0.0433(17) 0.7837(17) 0.051(7) Uani 0.215(13) 1 d D . P A 2 
H30E H 0.442053 -0.062054 0.726988 0.076 Uiso 0.215(13) 1 calc R U P A 2 
C30B C 0.413(5) 0.044(3) 0.782(3) 0.10(2) Uani 0.215(13) 1 d D . P A 2 
H30F H 0.352060 0.060683 0.839667 0.145 Uiso 0.215(13) 1 calc R U P A 2 
H30G H 0.344710 0.059207 0.724417 0.145 Uiso 0.215(13) 1 calc R U P A 2 
H30H H 0.520660 0.074862 0.781866 0.145 Uiso 0.215(13) 1 calc R U P A 2 
  
  
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
  
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
S1 O4 1.421(5) . ? 
S1 O3 1.444(5) . ? 
S1 N8X 1.655(5) . ? 
S1 C20 1.785(7) . ? 
Si1 C24 1.848(8) . ? 
Si1 C22 1.849(9) . ? 
Si1 C23 1.855(9) . ? 
Si1 C21 1.892(7) . ? 
O1 C11 1.433(9) . ? 
O1 C10 1.455(9) . ? 
O2 C1XX 1.239(10) . ? 
N1 C8AX 1.458(9) . ? 
N1 C9 1.465(8) . ? 
N1 C2 1.482(9) . ? 
C2 C3 1.562(10) . ? 
C2 H2A 0.9900 . ? 
C2 H2B 0.9900 . ? 
C3 C3A 1.535(10) . ? 
C3 H3A 0.9900 . ? 
C3 H3B 0.9900 . ? 
C3A C4A 1.509(8) . ? 
C3A C8A 1.559(8) . ? 
C3A C3AX 1.560(9) . ? 
C4 C5 1.394(10) . ? 
C4 C4A 1.394(8) . ? 
C4 C9 1.529(10) . ? 
C4A C7A 1.403(10) . ? 
C5 C6 1.370(11) . ? 
C5 H5 0.9500 . ? 
C6 C7 1.410(8) . ? 
C6 H6 0.9500 . ? 
C7 C7A 1.389(10) . ? 
C7 H7 0.9500 . ? 
C7A N8 1.391(7) . ? 
N8 C8 1.446(9) . ? 
N8 C8A 1.459(9) . ? 
C8 H8A 0.9800 . ? 
C8 H8B 0.9800 . ? 
C8 H8C 0.9800 . ? 
C8A N8X 1.459(9) . ? 
C8A H8A1 1.0000 . ? 
C9 C10 1.506(10) . ? 
C9 H9 1.0000 . ? 
C10 C11 1.484(8) . ? 
C10 H10 1.0000 . ? 
C11 C12 1.490(12) . ? 
C11 C13 1.512(10) . ? 
C12 H12A 0.9800 . ? 
C12 H12B 0.9800 . ? 
C12 H12C 0.9800 . ? 
C13 H13A 0.9800 . ? 
C13 H13B 0.9800 . ? 
C13 H13C 0.9800 . ? 
N1X C1XX 1.333(9) . ? 
N1X C2X 1.460(7) . ? 
N1X C8AX 1.468(9) . ? 
C2X C3X 1.533(10) . ? 
C2X H2X1 0.9900 . ? 
C2X H2X2 0.9900 . ? 
C3X C3AX 1.555(9) . ? 
C3X H3X1 0.9900 . ? 
C3X H3X2 0.9900 . ? 
C3AX C4AX 1.539(9) . ? 
C3AX C8AX 1.552(8) . ? 
C4AX C7AX 1.392(9) . ? 
C4AX C4X 1.406(9) . ? 
C4X C5X 1.392(10) . ? 
C4X H4X 0.9500 . ? 
C5X C6X 1.380(10) . ? 
C5X H5X 0.9500 . ? 
C6X C7X 1.392(10) . ? 
C6X H6X 0.9500 . ? 
C7X C7AX 1.367(10) . ? 
C7X H7X 0.9500 . ? 
C7AX N8X 1.457(9) . ? 
C8AX H8AX 1.0000 . ? 
C1XX C2XX 1.517(9) . ? 
C2XX H2X3 0.9800 . ? 
C2XX H2X4 0.9800 . ? 
C2XX H2X5 0.9800 . ? 
C20 C21 1.511(10) . ? 
C20 H20A 0.9900 . ? 
C20 H20B 0.9900 . ? 
C21 H21A 0.9900 . ? 
C21 H21B 0.9900 . ? 
C22 H22A 0.9800 . ? 
C22 H22B 0.9800 . ? 
C22 H22C 0.9800 . ? 
C23 H23A 0.9800 . ? 
C23 H23B 0.9800 . ? 
C23 H23C 0.9800 . ? 
C24 H24A 0.9800 . ? 
C24 H24B 0.9800 . ? 
C24 H24C 0.9800 . ? 
O30A C30A 1.382(18) . ? 
O30A H30A 0.8400 . ? 
C30A H30B 0.9800 . ? 
C30A H30C 0.9800 . ? 
C30A H30D 0.9800 . ? 
O30B C30B 1.37(3) . ? 
O30B H30E 0.8400 . ? 
C30B H30F 0.9800 . ? 
C30B H30G 0.9800 . ? 
C30B H30H 0.9800 . ? 
  
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
O4 S1 O3 119.3(3) . . ? 
O4 S1 N8X 107.1(3) . . ? 
O3 S1 N8X 108.4(3) . . ? 
O4 S1 C20 109.7(3) . . ? 
O3 S1 C20 106.9(3) . . ? 
N8X S1 C20 104.5(3) . . ? 
C24 Si1 C22 109.6(4) . . ? 
C24 Si1 C23 110.2(4) . . ? 
C22 Si1 C23 110.2(5) . . ? 
C24 Si1 C21 109.5(4) . . ? 
C22 Si1 C21 107.7(4) . . ? 
C23 Si1 C21 109.6(3) . . ? 
C11 O1 C10 61.8(4) . . ? 
C8AX N1 C9 112.7(5) . . ? 
C8AX N1 C2 113.0(5) . . ? 
C9 N1 C2 115.8(5) . . ? 
N1 C2 C3 113.3(6) . . ? 
N1 C2 H2A 108.9 . . ? 
C3 C2 H2A 108.9 . . ? 
N1 C2 H2B 108.9 . . ? 
C3 C2 H2B 108.9 . . ? 
H2A C2 H2B 107.7 . . ? 
C3A C3 C2 109.1(6) . . ? 
C3A C3 H3A 109.9 . . ? 
C2 C3 H3A 109.9 . . ? 
C3A C3 H3B 109.9 . . ? 
C2 C3 H3B 109.9 . . ? 
H3A C3 H3B 108.3 . . ? 
C4A C3A C3 109.0(5) . . ? 
C4A C3A C8A 102.6(5) . . ? 
C3 C3A C8A 111.3(5) . . ? 
C4A C3A C3AX 112.0(5) . . ? 
C3 C3A C3AX 109.2(6) . . ? 
C8A C3A C3AX 112.6(5) . . ? 
C5 C4 C4A 119.8(7) . . ? 
C5 C4 C9 120.6(5) . . ? 
C4A C4 C9 119.6(6) . . ? 
C4 C4A C7A 118.4(6) . . ? 
C4 C4A C3A 131.1(6) . . ? 
C7A C4A C3A 110.1(5) . . ? 
C6 C5 C4 120.5(5) . . ? 
C6 C5 H5 119.8 . . ? 
C4 C5 H5 119.8 . . ? 
C5 C6 C7 121.6(7) . . ? 
C5 C6 H6 119.2 . . ? 
C7 C6 H6 119.2 . . ? 
C7A C7 C6 116.8(7) . . ? 
C7A C7 H7 121.6 . . ? 
C6 C7 H7 121.6 . . ? 
C7 C7A N8 126.9(6) . . ? 
C7 C7A C4A 122.6(5) . . ? 
N8 C7A C4A 110.4(6) . . ? 
C7A N8 C8 124.0(6) . . ? 
C7A N8 C8A 110.4(5) . . ? 
C8 N8 C8A 119.9(5) . . ? 
N8 C8 H8A 109.5 . . ? 
N8 C8 H8B 109.5 . . ? 
H8A C8 H8B 109.5 . . ? 
N8 C8 H8C 109.5 . . ? 
H8A C8 H8C 109.5 . . ? 
H8B C8 H8C 109.5 . . ? 
N8X C8A N8 109.1(6) . . ? 
N8X C8A C3A 113.7(5) . . ? 
N8 C8A C3A 106.0(4) . . ? 
N8X C8A H8A1 109.3 . . ? 
N8 C8A H8A1 109.3 . . ? 
C3A C8A H8A1 109.3 . . ? 
N1 C9 C10 111.1(6) . . ? 
N1 C9 C4 114.5(5) . . ? 
C10 C9 C4 107.9(6) . . ? 
N1 C9 H9 107.7 . . ? 
C10 C9 H9 107.7 . . ? 
C4 C9 H9 107.7 . . ? 
O1 C10 C11 58.3(5) . . ? 
O1 C10 C9 116.2(6) . . ? 
C11 C10 C9 125.9(6) . . ? 
O1 C10 H10 114.6 . . ? 
C11 C10 H10 114.6 . . ? 
C9 C10 H10 114.6 . . ? 
O1 C11 C10 59.8(4) . . ? 
O1 C11 C12 114.9(7) . . ? 
C10 C11 C12 117.8(7) . . ? 
O1 C11 C13 116.0(7) . . ? 
C10 C11 C13 122.1(7) . . ? 
C12 C11 C13 114.6(6) . . ? 
C11 C12 H12A 109.5 . . ? 
C11 C12 H12B 109.5 . . ? 
H12A C12 H12B 109.5 . . ? 
C11 C12 H12C 109.5 . . ? 
H12A C12 H12C 109.5 . . ? 
H12B C12 H12C 109.5 . . ? 
C11 C13 H13A 109.5 . . ? 
C11 C13 H13B 109.5 . . ? 
H13A C13 H13B 109.5 . . ? 
C11 C13 H13C 109.5 . . ? 
H13A C13 H13C 109.5 . . ? 
H13B C13 H13C 109.5 . . ? 
C1XX N1X C2X 121.1(6) . . ? 
C1XX N1X C8AX 125.7(5) . . ? 
C2X N1X C8AX 112.9(5) . . ? 
N1X C2X C3X 104.5(6) . . ? 
N1X C2X H2X1 110.8 . . ? 
C3X C2X H2X1 110.8 . . ? 
N1X C2X H2X2 110.8 . . ? 
C3X C2X H2X2 110.8 . . ? 
H2X1 C2X H2X2 108.9 . . ? 
C2X C3X C3AX 103.8(5) . . ? 
C2X C3X H3X1 111.0 . . ? 
C3AX C3X H3X1 111.0 . . ? 
C2X C3X H3X2 111.0 . . ? 
C3AX C3X H3X2 111.0 . . ? 
H3X1 C3X H3X2 109.0 . . ? 
C4AX C3AX C8AX 114.2(5) . . ? 
C4AX C3AX C3X 106.0(5) . . ? 
C8AX C3AX C3X 103.4(5) . . ? 
C4AX C3AX C3A 109.1(5) . . ? 
C8AX C3AX C3A 107.1(5) . . ? 
C3X C3AX C3A 117.2(5) . . ? 
C7AX C4AX C4X 118.0(6) . . ? 
C7AX C4AX C3AX 117.0(5) . . ? 
C4X C4AX C3AX 124.7(6) . . ? 
C5X C4X C4AX 119.6(6) . . ? 
C5X C4X H4X 120.2 . . ? 
C4AX C4X H4X 120.2 . . ? 
C6X C5X C4X 121.1(7) . . ? 
C6X C5X H5X 119.4 . . ? 
C4X C5X H5X 119.4 . . ? 
C5X C6X C7X 119.2(7) . . ? 
C5X C6X H6X 120.4 . . ? 
C7X C6X H6X 120.4 . . ? 
C7AX C7X C6X 120.0(6) . . ? 
C7AX C7X H7X 120.0 . . ? 
C6X C7X H7X 120.0 . . ? 
C7X C7AX C4AX 122.0(6) . . ? 
C7X C7AX N8X 121.5(6) . . ? 
C4AX C7AX N8X 116.5(6) . . ? 
N1 C8AX N1X 111.7(6) . . ? 
N1 C8AX C3AX 113.6(5) . . ? 
N1X C8AX C3AX 104.0(5) . . ? 
N1 C8AX H8AX 109.1 . . ? 
N1X C8AX H8AX 109.1 . . ? 
C3AX C8AX H8AX 109.1 . . ? 
C7AX N8X C8A 115.2(4) . . ? 
C7AX N8X S1 121.5(4) . . ? 
C8A N8X S1 118.8(4) . . ? 
O2 C1XX N1X 121.5(6) . . ? 
O2 C1XX C2XX 121.2(7) . . ? 
N1X C1XX C2XX 117.2(7) . . ? 
C1XX C2XX H2X3 109.5 . . ? 
C1XX C2XX H2X4 109.5 . . ? 
H2X3 C2XX H2X4 109.5 . . ? 
C1XX C2XX H2X5 109.5 . . ? 
H2X3 C2XX H2X5 109.5 . . ? 
H2X4 C2XX H2X5 109.5 . . ? 
C21 C20 S1 114.7(5) . . ? 
C21 C20 H20A 108.6 . . ? 
S1 C20 H20A 108.6 . . ? 
C21 C20 H20B 108.6 . . ? 
S1 C20 H20B 108.6 . . ? 
H20A C20 H20B 107.6 . . ? 
C20 C21 Si1 114.4(5) . . ? 
C20 C21 H21A 108.7 . . ? 
Si1 C21 H21A 108.7 . . ? 
C20 C21 H21B 108.7 . . ? 
Si1 C21 H21B 108.7 . . ? 
H21A C21 H21B 107.6 . . ? 
Si1 C22 H22A 109.5 . . ? 
Si1 C22 H22B 109.5 . . ? 
H22A C22 H22B 109.5 . . ? 
Si1 C22 H22C 109.5 . . ? 
H22A C22 H22C 109.5 . . ? 
H22B C22 H22C 109.5 . . ? 
Si1 C23 H23A 109.5 . . ? 
Si1 C23 H23B 109.5 . . ? 
H23A C23 H23B 109.5 . . ? 
Si1 C23 H23C 109.5 . . ? 
H23A C23 H23C 109.5 . . ? 
H23B C23 H23C 109.5 . . ? 
Si1 C24 H24A 109.5 . . ? 
Si1 C24 H24B 109.5 . . ? 
H24A C24 H24B 109.5 . . ? 
Si1 C24 H24C 109.5 . . ? 
H24A C24 H24C 109.5 . . ? 
H24B C24 H24C 109.5 . . ? 
C30A O30A H30A 109.5 . . ? 
O30A C30A H30B 109.5 . . ? 
O30A C30A H30C 109.5 . . ? 
H30B C30A H30C 109.5 . . ? 
O30A C30A H30D 109.5 . . ? 
H30B C30A H30D 109.5 . . ? 
H30C C30A H30D 109.5 . . ? 
C30B O30B H30E 109.5 . . ? 
O30B C30B H30F 109.5 . . ? 
O30B C30B H30G 109.5 . . ? 
H30F C30B H30G 109.5 . . ? 
O30B C30B H30H 109.5 . . ? 
H30F C30B H30H 109.5 . . ? 
H30G C30B H30H 109.5 . . ? 
  
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 
O30A H30A O2  0.84 1.89 2.702(13) 161.0 . 
  
_refine_diff_density_max    0.539 
_refine_diff_density_min   -0.688 
_refine_diff_density_rms    0.079 
  
  
  
