#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/69/7116941.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7116941
loop_
_publ_author_name
'Urszula K. Klimczak'
'Bartosz K. Zambron'
_publ_section_title
;
 Effective 1,5-stereocontrol in Pd(0)/InI promoted reactions of chiral
 N-Ts-4-vinylazetidin-2-ones with aldehydes. An efficient entry into
 nonracemic semi-protected (3Z)-2,6-anti-enediols
;
_journal_name_full               Chem.Commun.
_journal_page_first              6796
_journal_paper_doi               10.1039/C5cc01485A
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C28.84 H42.57 N O6 S Si'
_chemical_formula_sum            'C28.84 H42.57 N O6 S Si'
_chemical_formula_weight         559.50
_chemical_melting_point          396.6(5)
_chemical_name_systematic
'(2R*,6S*,Z)-6-hydroxy-6-(4-methoxyphenyl)-N-tosyl-2-(triisopropylsilyloxy)hex-3-enamide '
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-02-09 deposited with the CCDC.
2015-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.208(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.627(2)
_cell_length_b                   13.4083(19)
_cell_length_c                   15.769(2)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      66.60
_cell_measurement_theta_min      4.45
_cell_volume                     3100.7(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.887
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_av_unetI/netI     0.0867
_diffrn_reflns_Laue_measured_fraction_full 0.887
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13497
_diffrn_reflns_point_group_measured_fraction_full 0.887
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.596
_diffrn_reflns_theta_min         4.450
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.622
_exptl_absorpt_correction_T_max  0.6970
_exptl_absorpt_correction_T_min  0.5900
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_description       prism
_exptl_crystal_F_000             1208
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Hexane/Ethyl acetate'
_exptl_crystal_size_max          0.364
_exptl_crystal_size_mid          0.353
_exptl_crystal_size_min          0.240
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         4970
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1831
_refine_ls_R_factor_gt           0.1077
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1548P)²+11.5689P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3289
_refine_ls_wR_factor_ref         0.3733
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2931
_reflns_number_total             4970
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5cc01485a2.cif
_cod_data_source_block           B2F145d_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '396.1-397.2' was changed to
'396.6(5)' - the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 3105 2015-03-04 15:46:00Z robertas 
;
_cod_original_formula_sum        'C28.84 H42.57 N O6 S Si '
_cod_database_code               7116941
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.590
_shelx_estimated_absorpt_t_max   0.697
_shelxl_version_number           2014-3
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.52974(16) 0.88142(18) 0.21215(18) 0.0733(7) Uani 1 1 d . . . A 1
S1 S 0.95057(12) 0.83138(15) 0.36836(13) 0.0613(6) Uani 1 1 d . . . A 1
O1 O 0.7686(4) 0.7414(4) 0.2634(4) 0.0757(16) Uani 1 1 d . . . A 1
O2 O 0.6067(3) 0.8029(4) 0.2758(4) 0.0677(14) Uani 1 1 d . . . A 1
O3 O 0.8505(4) 0.9552(5) 0.5281(5) 0.093(2) Uani 1 1 d . . . A 1
H3 H 0.8933 0.9943 0.5465 0.140 Uiso 1 1 calc R U . A 1
O4 O 0.8311(6) 1.3090(5) 0.7832(5) 0.102(2) Uani 1 1 d . . . A 1
O5 O 1.0040(4) 0.9030(5) 0.4319(4) 0.0825(17) Uani 1 1 d . . . A 1
O6 O 0.9778(4) 0.7301(4) 0.3774(5) 0.0851(18) Uani 1 1 d . . . A 1
N1 N 0.8491(4) 0.8427(5) 0.3783(4) 0.0618(16) Uani 1 1 d . . . A 1
H1 H 0.8452 0.8792 0.4217 0.074 Uiso 1 1 calc R U . A 1
C1 C 0.7700(5) 0.7978(5) 0.3221(6) 0.0596(18) Uani 1 1 d . . . A 1
C2 C 0.6858(5) 0.8275(6) 0.3474(5) 0.0626(19) Uani 1 1 d . . . A 1
H2 H 0.6870 0.8994 0.3591 0.075 Uiso 1 1 calc R U . A 1
C3 C 0.6908(5) 0.7712(6) 0.4312(6) 0.067(2) Uani 1 1 d . . . A 1
H3A H 0.6861 0.7021 0.4261 0.081 Uiso 1 1 calc R U . A 1
C4 C 0.7010(6) 0.8085(6) 0.5107(7) 0.075(2) Uani 1 1 d . . . A 1
H4A H 0.7052 0.7621 0.5558 0.089 Uiso 1 1 calc R U . A 1
C5 C 0.7068(5) 0.9153(6) 0.5393(6) 0.073(2) Uani 1 1 d . . . A 1
H5A H 0.6695 0.9250 0.5767 0.087 Uiso 1 1 calc R U . A 1
H5B H 0.6821 0.9569 0.4861 0.087 Uiso 1 1 calc R U . A 1
C6 C 0.8051(5) 0.9486(6) 0.5923(6) 0.068(2) Uani 1 1 d . . . A 1
H6 H 0.8346 0.8960 0.6356 0.082 Uiso 1 1 calc R U . A 1
C7 C 0.8103(5) 1.0435(6) 0.6438(5) 0.0599(18) Uani 1 1 d . . . A 1
C8 C 0.8354(6) 1.0426(6) 0.7362(6) 0.070(2) Uani 1 1 d . . . A 1
H8 H 0.8483 0.9820 0.7666 0.084 Uiso 1 1 calc R U . A 1
C9 C 0.8420(6) 1.1291(7) 0.7851(6) 0.073(2) Uani 1 1 d . . . A 1
H9 H 0.8590 1.1269 0.8477 0.088 Uiso 1 1 calc R U . A 1
C10 C 0.8233(6) 1.2177(6) 0.7404(6) 0.069(2) Uani 1 1 d . . . A 1
C11 C 0.7972(6) 1.2202(7) 0.6488(6) 0.078(2) Uani 1 1 d . . . A 1
H11 H 0.7834 1.2809 0.6185 0.093 Uiso 1 1 calc R U . A 1
C12 C 0.7912(6) 1.1337(6) 0.6009(5) 0.069(2) Uani 1 1 d . . . A 1
H12 H 0.7739 1.1363 0.5382 0.083 Uiso 1 1 calc R U . A 1
C13 C 0.8539(11) 1.3098(9) 0.8782(8) 0.131(5) Uani 1 1 d . . . A 1
H13A H 0.8113 1.2692 0.8944 0.197 Uiso 1 1 calc R U . A 1
H13B H 0.8514 1.3770 0.8984 0.197 Uiso 1 1 calc R U . A 1
H13C H 0.9144 1.2839 0.9063 0.197 Uiso 1 1 calc R U . A 1
C14 C 0.4741(8) 0.9472(9) 0.2845(9) 0.109(4) Uani 1 1 d . . . A 1
H14 H 0.5211 0.9900 0.3257 0.131 Uiso 1 1 calc R U . A 1
C15 C 0.3962(11) 1.0181(11) 0.2285(14) 0.175(7) Uani 1 1 d . . . A 1
H15A H 0.3451 0.9792 0.1922 0.263 Uiso 1 1 calc R U . A 1
H15B H 0.4175 1.0591 0.1900 0.263 Uiso 1 1 calc R U . A 1
H15C H 0.3779 1.0597 0.2688 0.263 Uiso 1 1 calc R U . A 1
C16 C 0.4427(11) 0.8815(13) 0.3416(13) 0.167(8) Uani 0.974(15) 1 d . . P A 1
H16A H 0.4310 0.9201 0.3876 0.251 Uiso 0.974(15) 1 calc R U P A 1
H16B H 0.4888 0.8326 0.3692 0.251 Uiso 0.974(15) 1 calc R U P A 1
H16C H 0.3877 0.8485 0.3053 0.251 Uiso 0.974(15) 1 calc R U P A 1
C17 C 0.4480(11) 0.7968(11) 0.1318(11) 0.135(5) Uiso 0.974(15) 1 d . . P A 1
H17 H 0.4185 0.7621 0.1690 0.162 Uiso 0.974(15) 1 calc R U P A 1
C18 C 0.3717(18) 0.8434(18) 0.060(2) 0.243(12) Uiso 0.974(15) 1 d . . P A 1
H18A H 0.3897 0.8571 0.0089 0.365 Uiso 0.974(15) 1 calc R U P A 1
H18B H 0.3552 0.9045 0.0821 0.365 Uiso 0.974(15) 1 calc R U P A 1
H18C H 0.3205 0.7989 0.0424 0.365 Uiso 0.974(15) 1 calc R U P A 1
C19 C 0.4847(17) 0.7177(17) 0.0936(18) 0.226(10) Uiso 0.974(15) 1 d . . P A 1
H19A H 0.4397 0.6663 0.0715 0.339 Uiso 0.974(15) 1 calc R U P A 1
H19B H 0.5376 0.6905 0.1392 0.339 Uiso 0.974(15) 1 calc R U P A 1
H19C H 0.5015 0.7432 0.0447 0.339 Uiso 0.974(15) 1 calc R U P A 1
C20 C 0.5841(9) 0.9761(8) 0.1591(10) 0.114(4) Uani 1 1 d . . . . .
H20 H 0.5337 1.0115 0.1143 0.137 Uiso 1 1 calc R U . A 1
C21 C 0.6386(15) 1.0495(14) 0.2141(15) 0.220(10) Uani 1 1 d . . . . .
H21A H 0.6972 1.0499 0.2071 0.330 Uiso 1 1 calc R U . . .
H21B H 0.6460 1.0359 0.2760 0.330 Uiso 1 1 calc R U . . .
H21C H 0.6101 1.1134 0.1972 0.330 Uiso 1 1 calc R U . . .
C22' C 0.6404(13) 0.9300(13) 0.1061(13) 0.171(7) Uiso 0.974(15) 1 d . . P A 1
H22A H 0.6639 0.9821 0.0786 0.257 Uiso 0.974(15) 1 calc R U P A 1
H22B H 0.6023 0.8866 0.0601 0.257 Uiso 0.974(15) 1 calc R U P A 1
H22C H 0.6901 0.8925 0.1466 0.257 Uiso 0.974(15) 1 calc R U P A 1
C23 C 0.9339(5) 0.8728(5) 0.2588(5) 0.0576(18) Uani 1 1 d . . . . .
C24 C 0.9242(6) 0.9718(6) 0.2393(7) 0.078(2) Uani 1 1 d . . . . .
H24 H 0.9285 1.0189 0.2839 0.094 Uiso 1 1 calc R U . . .
C25 C 0.9074(7) 1.0003(8) 0.1493(9) 0.098(3) Uani 1 1 d . . . . .
H25 H 0.9007 1.0675 0.1341 0.118 Uiso 1 1 calc R U . . .
C26 C 0.9008(6) 0.9304(11) 0.0830(6) 0.096(3) Uani 1 1 d . . . . .
C27 C 0.9142(7) 0.8328(9) 0.1078(7) 0.089(3) Uani 1 1 d . . . . .
H27 H 0.9122 0.7852 0.0642 0.106 Uiso 1 1 calc R U . . .
C28 C 0.9302(6) 0.8035(6) 0.1926(6) 0.069(2) Uani 1 1 d . . . . .
H28 H 0.9388 0.7362 0.2073 0.083 Uiso 1 1 calc R U . . .
C29' C 0.8805(11) 0.9657(11) -0.0131(11) 0.140(5) Uiso 0.974(15) 1 d . . P A 1
H29A H 0.9306 0.9492 -0.0324 0.210 Uiso 0.974(15) 1 calc R U P A 1
H29B H 0.8717 1.0367 -0.0158 0.210 Uiso 0.974(15) 1 calc R U P A 1
H29C H 0.8261 0.9337 -0.0520 0.210 Uiso 0.974(15) 1 calc R U P A 1
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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O2 Si1 C17 102.2(5) . .
O2 Si1 C14 108.9(4) . .
C17 Si1 C14 110.5(7) . .
O2 Si1 C20 110.8(5) . .
C17 Si1 C20 115.0(7) . .
C14 Si1 C20 109.2(6) . .
O6 S1 O5 119.4(4) . .
O6 S1 N1 110.1(3) . .
O5 S1 N1 102.7(3) . .
O6 S1 C23 110.0(4) . .
O5 S1 C23 109.3(4) . .
N1 S1 C23 104.2(3) . .
C2 O2 Si1 126.6(5) . .
C6 O3 H3 109.5 . .
C10 O4 C13 118.1(8) . .
C1 N1 S1 125.0(5) . .
C1 N1 H1 117.5 . .
S1 N1 H1 117.5 . .
O1 C1 N1 123.1(7) . .
O1 C1 C2 124.9(7) . .
N1 C1 C2 111.9(6) . .
O2 C2 C3 110.8(6) . .
O2 C2 C1 108.9(6) . .
C3 C2 C1 107.8(6) . .
O2 C2 H2 109.7 . .
C3 C2 H2 109.7 . .
C1 C2 H2 109.7 . .
C4 C3 C2 127.1(8) . .
C4 C3 H3A 116.5 . .
C2 C3 H3A 116.5 . .
C3 C4 C5 129.1(8) . .
C3 C4 H4A 115.4 . .
C5 C4 H4A 115.4 . .
C4 C5 C6 112.8(7) . .
C4 C5 H5A 109.0 . .
C6 C5 H5A 109.0 . .
C4 C5 H5B 109.0 . .
C6 C5 H5B 109.0 . .
H5A C5 H5B 107.8 . .
O3 C6 C7 112.7(6) . .
O3 C6 C5 106.3(7) . .
C7 C6 C5 113.5(6) . .
O3 C6 H6 108.1 . .
C7 C6 H6 108.1 . .
C5 C6 H6 108.1 . .
C12 C7 C8 117.8(7) . .
C12 C7 C6 121.4(7) . .
C8 C7 C6 120.7(7) . .
C7 C8 C9 121.8(8) . .
C7 C8 H8 119.1 . .
C9 C8 H8 119.1 . .
C10 C9 C8 119.0(8) . .
C10 C9 H9 120.5 . .
C8 C9 H9 120.5 . .
C11 C10 C9 120.3(8) . .
C11 C10 O4 116.1(8) . .
C9 C10 O4 123.6(8) . .
C10 C11 C12 120.2(8) . .
C10 C11 H11 119.9 . .
C12 C11 H11 119.9 . .
C7 C12 C11 121.0(7) . .
C7 C12 H12 119.5 . .
C11 C12 H12 119.5 . .
O4 C13 H13A 109.5 . .
O4 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
O4 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C16 C14 C15 110.7(11) . .
C16 C14 Si1 114.5(10) . .
C15 C14 Si1 112.2(10) . .
C16 C14 H14 106.2 . .
C15 C14 H14 106.2 . .
Si1 C14 H14 106.2 . .
C14 C15 H15A 109.5 . .
C14 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C14 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C14 C16 H16A 109.5 . .
C14 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C14 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C19 C17 C18 109(2) . .
C19 C17 Si1 117.4(14) . .
C18 C17 Si1 116.9(14) . .
C19 C17 H17 103.8 . .
C18 C17 H17 103.8 . .
Si1 C17 H17 103.8 . .
C17 C18 H18A 109.5 . .
C17 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C17 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C17 C19 H19A 109.5 . .
C17 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
C17 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
C21 C20 C22' 106.4(15) . .
C21 C20 Si1 118.3(12) . .
C22' C20 Si1 113.7(9) . .
C21 C20 H20 105.8 . .
C22' C20 H20 105.8 . .
Si1 C20 H20 105.8 . .
C20 C21 H21A 109.5 . .
C20 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C20 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C20 C22' H22A 109.5 . .
C20 C22' H22B 109.5 . .
H22A C22' H22B 109.5 . .
C20 C22' H22C 109.5 . .
H22A C22' H22C 109.5 . .
H22B C22' H22C 109.5 . .
C24 C23 C28 120.8(8) . .
C24 C23 S1 120.1(6) . .
C28 C23 S1 119.1(6) . .
C23 C24 C25 117.5(9) . .
C23 C24 H24 121.3 . .
C25 C24 H24 121.3 . .
C26 C25 C24 121.3(9) . .
C26 C25 H25 119.3 . .
C24 C25 H25 119.3 . .
C27 C26 C25 118.1(9) . .
C27 C26 C29' 123.1(12) . .
C25 C26 C29' 118.7(12) . .
C28 C27 C26 121.9(9) . .
C28 C27 H27 119.0 . .
C26 C27 H27 119.0 . .
C27 C28 C23 120.3(9) . .
C27 C28 H28 119.9 . .
C23 C28 H28 119.9 . .
C26 C29' H29A 109.5 . .
C26 C29' H29B 109.5 . .
H29A C29' H29B 109.5 . .
C26 C29' H29C 109.5 . .
H29A C29' H29C 109.5 . .
H29B C29' H29C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 O2 1.652(6) .
Si1 C17 1.846(16) .
Si1 C14 1.877(11) .
Si1 C20 1.878(11) .
S1 O6 1.416(6) .
S1 O5 1.430(6) .
S1 N1 1.653(6) .
S1 C23 1.746(8) .
O1 C1 1.190(9) .
O2 C2 1.396(9) .
O3 C6 1.426(9) .
O3 H3 0.8200 .
O4 C10 1.383(10) .
O4 C13 1.415(13) .
N1 C1 1.385(9) .
N1 H1 0.8600 .
C1 C2 1.553(10) .
C2 C3 1.501(12) .
C2 H2 0.9800 .
C3 C4 1.307(12) .
C3 H3A 0.9300 .
C4 C5 1.494(11) .
C4 H4A 0.9300 .
C5 C6 1.540(11) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 C7 1.496(10) .
C6 H6 0.9800 .
C7 C12 1.367(11) .
C7 C8 1.372(11) .
C8 C9 1.376(12) .
C8 H8 0.9300 .
C9 C10 1.361(12) .
C9 H9 0.9300 .
C10 C11 1.359(12) .
C11 C12 1.370(11) .
C11 H11 0.9300 .
C12 H12 0.9300 .
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
C14 C16 1.461(17) .
C14 C15 1.557(17) .
C14 H14 0.9800 .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
C17 C19 1.43(2) .
C17 C18 1.47(3) .
C17 H17 0.9800 .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
C19 H19A 0.9600 .
C19 H19B 0.9600 .
C19 H19C 0.9600 .
C20 C21 1.39(2) .
C20 C22' 1.536(19) .
C20 H20 0.9800 .
C21 H21A 0.9600 .
C21 H21B 0.9600 .
C21 H21C 0.9600 .
C22' H22A 0.9600 .
C22' H22B 0.9600 .
C22' H22C 0.9600 .
C23 C24 1.359(10) .
C23 C28 1.385(11) .
C24 C25 1.404(15) .
C24 H24 0.9300 .
C25 C26 1.380(16) .
C25 H25 0.9300 .
C26 C27 1.361(15) .
C26 C29' 1.513(18) .
C27 C28 1.332(13) .
C27 H27 0.9300 .
C28 H28 0.9300 .
C29' H29A 0.9600 .
C29' H29B 0.9600 .
C29' H29C 0.9600 .
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
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
O3 H3 O5 0.82 2.05 2.862(8) 169.6 3_776
N1 H1 O3 0.86 1.94 2.796(8) 173.1 .
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
C17_a Si1_a O2_a C2_a 178.8(7) . . . .
C14 Si1 O2 C2 -64.3(7) . . . .
C20 Si1 O2 C2 55.8(8) . . . .
O6 S1 N1 C1 -60.6(7) . . . .
O5 S1 N1 C1 171.2(6) . . . .
C23 S1 N1 C1 57.3(7) . . . .
S1 N1 C1 O1 4.4(11) . . . .
S1 N1 C1 C2 -177.4(5) . . . .
Si1 O2 C2 C3 126.8(6) . . . .
Si1 O2 C2 C1 -114.8(6) . . . .
O1 C1 C2 O2 -17.7(11) . . . .
N1 C1 C2 O2 164.2(6) . . . .
O1 C1 C2 C3 102.7(9) . . . .
N1 C1 C2 C3 -75.4(8) . . . .
O2 C2 C3 C4 -125.5(9) . . . .
C1 C2 C3 C4 115.4(9) . . . .
C2 C3 C4 C5 2.6(14) . . . .
C3 C4 C5 C6 -102.6(11) . . . .
C4 C5 C6 O3 72.2(9) . . . .
C4 C5 C6 C7 -163.4(7) . . . .
O3 C6 C7 C12 47.6(10) . . . .
C5 C6 C7 C12 -73.3(10) . . . .
O3 C6 C7 C8 -131.7(8) . . . .
C5 C6 C7 C8 107.5(9) . . . .
C12 C7 C8 C9 -0.3(12) . . . .
C6 C7 C8 C9 179.0(7) . . . .
C7 C8 C9 C10 -0.2(13) . . . .
C8 C9 C10 C11 1.0(13) . . . .
C8 C9 C10 O4 -177.6(8) . . . .
C13 O4 C10 C11 177.1(10) . . . .
C13 O4 C10 C9 -4.3(14) . . . .
C9 C10 C11 C12 -1.2(14) . . . .
O4 C10 C11 C12 177.5(8) . . . .
C8 C7 C12 C11 0.1(12) . . . .
C6 C7 C12 C11 -179.2(8) . . . .
C10 C11 C12 C7 0.7(14) . . . .
O2 Si1 C14 C16 -49.1(12) . . . .
C17 Si1 C14 C16 62.5(13) . . . .
C20 Si1 C14 C16 -170.1(12) . . . .
O2 Si1 C14 C15 -176.5(9) . . . .
C17 Si1 C14 C15 -64.9(12) . . . .
C20 Si1 C14 C15 62.5(11) . . . .
O2 Si1 C17 C19 -43.7(17) . . . .
C14 Si1 C17 C19 -159.4(15) . . . .
C20 Si1 C17 C19 76.4(17) . . . .
O2 Si1 C17 C18 -176.3(16) . . . .
C14 Si1 C17 C18 68.0(17) . . . .
C20 Si1 C17 C18 -56.2(17) . . . .
O2 Si1 C20 C21 -71.8(14) . . . .
C17 Si1 C20 C21 172.9(14) . . . .
C14 Si1 C20 C21 48.1(15) . . . .
O2 Si1 C20 C22' 54.1(13) . . . .
C17 Si1 C20 C22' -61.2(14) . . . .
C14 Si1 C20 C22' 174.0(11) . . . .
O6 S1 C23 C24 -167.7(6) . . . .
O5 S1 C23 C24 -34.9(8) . . . .
N1 S1 C23 C24 74.3(7) . . . .
O6 S1 C23 C28 12.8(7) . . . .
O5 S1 C23 C28 145.6(6) . . . .
N1 S1 C23 C28 -105.2(6) . . . .
C28 C23 C24 C25 1.9(12) . . . .
S1 C23 C24 C25 -177.6(7) . . . .
C23 C24 C25 C26 0.2(14) . . . .
C24 C25 C26 C27 -2.3(15) . . . .
C24 C25 C26 C29' 178.6(10) . . . .
C25 C26 C27 C28 2.4(15) . . . .
C29' C26 C27 C28 -178.6(10) . . . .
C26 C27 C28 C23 -0.3(14) . . . .
C24 C23 C28 C27 -2.0(13) . . . .
S1 C23 C28 C27 177.5(7) . . . .
