#------------------------------------------------------------------------------
#$Date: 2021-03-05 04:25:58 +0200 (Fri, 05 Mar 2021) $
#$Revision: 262720 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/15/78/7157845.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_7157845
loop_
_publ_author_name
'Tsuda, Masato'
'Morita, Taiki'
'Fukuhara, Shintaro'
'Nakamura, Hiroyuki'
_publ_section_title
;
 Synthesis of 4-amino-5-allenylisoxazoles via gold(I)-catalysed
 propargyl aza-Claisen rearrangement.
;
_journal_issue                   6
_journal_name_full               'Organic & biomolecular chemistry'
_journal_page_first              1358
_journal_page_last               1364
_journal_paper_doi               10.1039/d0ob02544e
_journal_volume                  19
_journal_year                    2021
_chemical_formula_moiety         'C23 H26 N2 O3 S Si'
_chemical_formula_sum            'C23 H26 N2 O3 S Si'
_chemical_formula_weight         438.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-17
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2020-09-04 deposited with the CCDC.	2021-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                112.371(2)
_cell_angle_beta                 101.901(2)
_cell_angle_gamma                101.004(2)
_cell_formula_units_Z            2
_cell_length_a                   10.1798(2)
_cell_length_b                   10.3113(2)
_cell_length_c                   12.4879(3)
_cell_measurement_reflns_used    16377
_cell_measurement_temperature    90
_cell_measurement_theta_max      76.4560
_cell_measurement_theta_min      3.9870
_cell_volume                     1132.33(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      90
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     29.00  88.00   0.50    0.09    --   46.45  65.00 -79.00  118
  2  ω     86.00 175.00   0.50    0.34    --  104.75  77.00-150.00  178
  3  ω    138.00 164.00   0.50    0.34    --  104.75  45.00-120.00   52
  4  ω     87.00 168.00   0.50    0.34    --  104.75  65.00 -79.00  162
  5  ω     70.00 103.00   0.50    0.34    --  104.75 -94.00 150.00   66
  6  ω     80.00 111.00   0.50    0.34    --  104.75-125.00  30.00   62
  7  ω     36.00 105.00   0.50    0.34    --  104.75 -94.00   0.00  138
  8  ω     33.00  61.00   0.50    0.34    --  104.75-125.00-180.00   56
  9  ω     64.00 110.00   0.50    0.34    --  104.75-125.00-180.00   92
 10  ω     78.00 106.00   0.50    0.34    --  104.75 -94.00 -90.00   56
 11  ω     47.00  74.00   0.50    0.34    --  104.75 -94.00 -90.00   54
 12  ω     33.00  58.00   0.50    0.34    --  104.75 -77.00  30.00   50
 13  ω     33.00  80.00   0.50    0.34    --  104.75 -65.00 144.00   94
 14  ω    -15.00  62.00   0.50    0.09    --   46.45 -65.00 144.00  154
 15  ω     68.00 106.00   0.50    0.34    --  104.75 -77.00  30.00   76
 16  ω     32.00  64.00   0.50    0.34    --  104.75 -61.00 -60.00   64
 17  ω     38.00 106.00   0.50    0.34    --  104.75 -77.00-150.00  136
 18  ω    -18.00   9.00   0.50    0.09    --   46.45 -19.00-150.00   54
 19  ω    -20.00  21.00   0.50    0.09    --  -46.45  19.00  60.00   82
 20  ω    -19.00  18.00   0.50    0.09    --  -46.45  37.00  30.00   74
 21  ω    -18.00  24.00   0.50    0.09    --  -46.45  65.00 -79.00   84
 22  ω    -47.00 -21.00   0.50    0.09    --  -46.45  65.00 -79.00   52
 23  ω    -21.00  29.00   0.50    0.09    --  -46.45  19.00 -90.00  100
 24  ω    -23.00  10.00   0.50    0.09    --  -46.45  19.00-150.00   66
 25  ω    -76.00 -29.00   0.50    0.34    -- -102.00  65.00 -79.00   94
 26  ω    -66.00 -35.00   0.50    0.34    -- -102.00  61.00   0.00   62
 27  ω    -67.00 -30.00   0.50    0.34    -- -102.00  61.00  90.00   74
 28  ω    -56.00 -31.00   0.50    0.34    -- -102.00  61.00 120.00   50
 29  ω   -112.00 -56.00   0.50    0.34    -- -102.00 125.00  60.00  112
 30  ω   -110.00 -77.00   0.50    0.34    -- -102.00 125.00-150.00   66
 31  ω   -174.00 -85.00   0.50    0.34    -- -102.00 -61.00-150.00  178
 32  ω   -173.00-115.00   0.50    0.34    -- -102.00 -30.00-180.00  116
 33  ω   -154.00 -92.00   0.50    0.34    -- -102.00 -45.00  30.00  124
 34  ω   -111.00 -40.00   0.50    0.09    --  -46.45 -65.00 144.00  142
 35  ω   -173.00 -90.00   0.50    0.34    -- -102.00 -65.00 144.00  166
 36  ω   -114.00 -87.00   0.50    0.34    -- -102.00-125.00 -90.00   54
 37  ω   -160.00-134.00   0.50    0.34    -- -102.00-125.00 -90.00   52
 38  ω     32.00  57.00   0.50    0.34    --  104.75 -65.00 144.00   50
 39  ω   -116.00 -89.00   0.50    0.09    --  -46.45 -42.00 -25.77   54
 40  ω    -55.00 -28.00   0.50    0.09    --  -46.45 -65.00 144.00   54
 41  ω    -94.00 -18.00   0.50    0.09    --  -46.45 125.00  60.00  152
 42  ω    -77.00 -35.00   0.50    0.09    --  -46.45 -19.00   0.00   84
 43  ω    -66.00 -34.00   0.50    0.09    --  -46.45 -42.00 -25.77   64
 44  ω     32.00  62.00   0.50    0.09    --   46.45  57.00-120.00   60
 45  ω     88.00 118.00   0.50    0.09    --   46.45  77.00 -30.00   60
 46  ω     24.00  53.00   0.50    0.09    --   46.45  77.00  90.00   58
 47  ω     30.00  56.00   0.50    0.09    --   46.45  77.00 120.00   52
 48  ω     35.00  62.00   0.50    0.09    --   46.45  37.00-180.00   54
 49  ω     24.00  79.00   0.50    0.09    --   46.45  77.00 -30.00  110
 50  ω     30.00  65.00   0.50    0.09    --   46.45  77.00-150.00   70
 51  ω     25.00  58.00   0.50    0.09    --   46.45  77.00 150.00   66
 52  ω     37.00  64.00   0.50    0.09    --   46.45  37.00 120.00   54
 53  ω     66.00 100.00   0.50    0.09    --   46.45  57.00-120.00   68
 54  ω     24.00  61.00   0.50    0.09    --   46.45  77.00  30.00   74
 55  ω     45.00  93.00   0.50    0.09    --   46.45  37.00-150.00   96
 56  ω     88.00 118.00   0.50    0.09    --   46.45  37.00 120.00   60
 57  ω     34.00  59.00   0.50    0.09    --   46.45  57.00   0.00   50
 58  ω     64.00 114.00   0.50    0.09    --   46.45  77.00 -90.00  100
 59  ω     24.00  50.00   0.50    0.09    --   46.45  77.00 -90.00   52
 60  ω   -173.00-118.00   0.50    0.34    -- -102.00 -80.00  79.18  110
 61  ω   -112.00 -80.00   0.50    0.34    -- -102.00 -74.00 -30.10   64
 62  ω   -107.00 -80.00   0.50    0.34    -- -102.00 -75.00 170.27   54
 63  ω   -173.00-147.00   0.50    0.34    -- -102.00 -75.00  50.02   52
 64  ω   -172.00-146.00   0.50    0.34    -- -102.00 -74.00 -30.10   52
 65  ω   -110.00 -80.00   0.50    0.34    -- -102.00 -75.00  50.02   60
 66  ω   -126.00 -85.00   0.50    0.34    -- -102.00 -61.00 -60.00   82
 67  ω   -114.00 -87.00   0.50    0.34    -- -102.00 -55.00-170.36   54
 68  ω   -157.00-130.00   0.50    0.34    -- -102.00 -77.00-120.00   54
 69  ω   -169.00-132.00   0.50    0.34    -- -102.00 -75.00 170.27   74
 70  ω   -166.00-118.00   0.50    0.34    -- -102.00 -51.00  85.01   96
 71  ω   -114.00 -84.00   0.50    0.34    -- -102.00 -65.00  24.99   60
 72  ω   -160.00-117.00   0.50    0.34    -- -102.00 -65.00  24.99   86
 73  ω   -113.00 -86.00   0.50    0.34    -- -102.00 -59.00 170.90   54
 74  ω   -105.00 -79.00   0.50    0.34    -- -102.00 -77.00 -60.00   52
 75  ω   -107.00 -80.00   0.50    0.34    -- -102.00 -75.00 141.56   54
 76  ω   -105.00 -78.00   0.50    0.34    -- -102.00 -80.00  13.80   54
 77  ω   -141.00-115.00   0.50    0.34    -- -102.00 -80.00  13.80   52
 78  ω   -111.00 -83.00   0.50    0.34    -- -102.00 -72.00 128.45   56
 79  ω   -108.00 -82.00   0.50    0.34    -- -102.00 -71.00 -90.49   52
 80  ω   -161.00-117.00   0.50    0.34    -- -102.00 -72.00 128.45   88
 81  ω   -141.00 -85.00   0.50    0.34    -- -102.00 -61.00 -30.00  112
 82  ω    -58.00 -31.00   0.50    0.34    -- -102.00  61.00-120.00   54
 83  ω   -107.00 -80.00   0.50    0.34    -- -102.00 -76.00  22.36   54
 84  ω   -111.00 -85.00   0.50    0.34    -- -102.00 -61.00-120.00   52
 85  ω   -112.00 -85.00   0.50    0.34    -- -102.00 -61.00-180.00   54
 86  ω   -110.00 -84.00   0.50    0.34    -- -102.00 -68.00 114.48   52
 87  ω   -109.00 -78.00   0.50    0.34    -- -102.00 -79.00 -70.12   62
 88  ω   -155.00-128.00   0.50    0.34    -- -102.00 -79.00 -70.12   54
 89  ω   -113.00 -88.00   0.50    0.34    -- -102.00 -51.00  85.01   50
 90  ω   -105.00 -79.00   0.50    0.34    -- -102.00 -77.00-180.00   52
 91  ω   -174.00-147.00   0.50    0.34    -- -102.00 -77.00   0.00   54
 92  ω   -122.00 -79.00   0.50    0.34    -- -102.00 -77.00   0.00   86
 93  ω   -106.00 -79.00   0.50    0.34    -- -102.00 -77.00  60.00   54
 94  ω   -104.00 -78.00   0.50    0.34    -- -102.00 -79.00  35.99   52
 95  ω   -175.00-149.00   0.50    0.34    -- -102.00 -61.00-180.00   52
 96  ω   -140.00 -90.00   0.50    0.34    -- -102.00 -51.00  54.62  100
 97  ω   -104.00 -78.00   0.50    0.34    -- -102.00 -79.00-129.09   52
 98  ω   -113.00 -87.00   0.50    0.34    -- -102.00 -57.00-177.77   52
 99  ω   -113.00 -86.00   0.50    0.34    -- -102.00 -61.00  90.00   54
100  ω   -106.00 -79.00   0.50    0.34    -- -102.00 -76.00 155.84   54
101  ω   -156.00-131.00   0.50    0.34    -- -102.00 -79.00-129.09   50
102  ω   -105.00 -79.00   0.50    0.34    -- -102.00 -77.00-120.00   52
103  ω   -103.00 -78.00   0.50    0.34    -- -102.00 -80.00  79.18   50
104  ω   -143.00-117.00   0.50    0.34    -- -102.00 -68.00 114.48   52
105  ω   -107.00 -81.00   0.50    0.34    -- -102.00 -77.00  90.00   52
106  ω     88.00 113.00   0.50    0.34    --  104.75  65.00  93.29   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0834793000
_diffrn_orient_matrix_UB_12      0.0565613000
_diffrn_orient_matrix_UB_13      0.0886399000
_diffrn_orient_matrix_UB_21      0.0330597000
_diffrn_orient_matrix_UB_22      -0.1039090000
_diffrn_orient_matrix_UB_23      0.0564648000
_diffrn_orient_matrix_UB_31      0.1348471000
_diffrn_orient_matrix_UB_32      0.1210168000
_diffrn_orient_matrix_UB_33      0.0927715000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            30216
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.528
_diffrn_reflns_theta_min         4.023
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.993
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.109
_refine_diff_density_max         0.906
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         4555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0624P)²+0.7047P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1150
_refine_ls_wR_factor_ref         0.1175
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4169
_reflns_number_total             4555
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ob02544e2.cif
_cod_data_source_block           tsuda1
_cod_depositor_comments          'Adding full bibliography for 7157845.cif.'
_cod_database_code               7157845
_shelx_shelxl_version_number     2018/3
_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_max   0.812
_shelx_estimated_absorpt_t_min   0.760
_diffrn_oxdiff_digest_frames
;
015bf584c7d866277c684d377a7df9357400075089b
;
_diffrn_oxdiff_digest_hkl
;
01a1b1b71b2c820cf44551e8db2af199c68921
;
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Riding coordinates:
 N10(H10)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C17(H17), C5(H5), C15(H15), C3(H3), C16(H16), C13(H13),
 C25(H25), C14(H14)
2.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C11(H11A,H11B,H11C), C30(H30A,H30B,
 H30C), C26(H26A,H26B,H26C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.389
_oxdiff_exptl_absorpt_empirical_full_min 0.783
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.94629(4) 0.81115(4) 0.30827(4) 0.02242(13) Uani 1 1 d . . . . .
Si1 Si 0.37634(5) 0.55161(5) 0.23797(4) 0.02390(14) Uani 1 1 d . . . . .
O8 O 1.07711(13) 0.89794(14) 0.40387(11) 0.0276(3) Uani 1 1 d . . . . .
O9 O 0.94046(13) 0.76605(14) 0.18356(11) 0.0274(3) Uani 1 1 d . . . . .
O10 O 0.48352(13) 0.79166(14) 0.14583(11) 0.0270(3) Uani 1 1 d . . . . .
N10 N 0.84088(15) 0.91344(16) 0.33585(13) 0.0229(3) Uani 1 1 d . . . . .
H10 H 0.829323 0.929594 0.405598 0.027 Uiso 1 1 d R . . . .
N22 N 0.54903(16) 0.86980(17) 0.08964(14) 0.0269(3) Uani 1 1 d . . . . .
C20 C 0.58181(18) 0.79802(19) 0.24038(15) 0.0238(3) Uani 1 1 d . . . . .
C18 C 0.68387(18) 0.92005(19) 0.15090(15) 0.0235(3) Uani 1 1 d . . . . .
C1 C 0.88102(18) 0.65378(19) 0.32843(16) 0.0242(4) Uani 1 1 d . . . . .
C19 C 0.71021(18) 0.87726(18) 0.24785(15) 0.0223(3) Uani 1 1 d . . . . .
C12 C 0.78049(19) 1.00955(19) 0.11394(16) 0.0242(4) Uani 1 1 d . . . . .
C23 C 0.53152(18) 0.7247(2) 0.31097(16) 0.0250(4) Uani 1 1 d . . . . .
C6 C 0.8059(2) 0.5213(2) 0.22846(18) 0.0300(4) Uani 1 1 d . . . . .
H6 H 0.790974 0.513604 0.148349 0.036 Uiso 1 1 calc R . . . .
C2 C 0.9051(2) 0.6659(2) 0.44646(17) 0.0290(4) Uani 1 1 d . . . . .
H2 H 0.957721 0.756903 0.514448 0.035 Uiso 1 1 calc R . . . .
C17 C 0.9197(2) 1.0850(2) 0.18470(18) 0.0322(4) Uani 1 1 d . . . . .
H17 H 0.956016 1.077420 0.257803 0.039 Uiso 1 1 calc R . . . .
C4 C 0.7743(2) 0.4093(2) 0.3643(2) 0.0329(4) Uani 1 1 d . . . . .
C5 C 0.7526(2) 0.3996(2) 0.24707(19) 0.0339(4) Uani 1 1 d . . . . .
H5 H 0.700705 0.308469 0.178923 0.041 Uiso 1 1 calc R . . . .
C24 C 0.5968(2) 0.7826(2) 0.42887(18) 0.0320(4) Uani 1 1 d . . . . .
C15 C 0.9554(2) 1.1846(2) 0.04335(18) 0.0345(4) Uani 1 1 d . . . . .
H15 H 1.015273 1.243276 0.019158 0.041 Uiso 1 1 calc R . . . .
C28 C 0.4034(2) 0.4507(2) 0.33301(19) 0.0338(4) Uani 1 1 d . . . . .
H28A H 0.498007 0.439566 0.344080 0.051 Uiso 1 1 calc GR . . . .
H28B H 0.333431 0.353536 0.292307 0.051 Uiso 1 1 calc GR . . . .
H28C H 0.392824 0.506163 0.412577 0.051 Uiso 1 1 calc GR . . . .
C3 C 0.8513(2) 0.5437(2) 0.46328(19) 0.0330(4) Uani 1 1 d . . . . .
H3 H 0.867166 0.551544 0.543484 0.040 Uiso 1 1 calc R . . . .
C16 C 1.0059(2) 1.1715(2) 0.14904(19) 0.0363(4) Uani 1 1 d . . . . .
H16 H 1.100908 1.222250 0.197998 0.044 Uiso 1 1 calc R . . . .
C13 C 0.7297(2) 1.0241(2) 0.00776(18) 0.0345(4) Uani 1 1 d . . . . .
H13 H 0.634746 0.973763 -0.041420 0.041 Uiso 1 1 calc R . . . .
C29 C 0.3756(2) 0.4378(2) 0.08107(18) 0.0350(4) Uani 1 1 d . . . . .
H29A H 0.375368 0.496489 0.035119 0.053 Uiso 1 1 calc GR . . . .
H29B H 0.291345 0.352366 0.040599 0.053 Uiso 1 1 calc GR . . . .
H29C H 0.459634 0.404434 0.084786 0.053 Uiso 1 1 calc GR . . . .
C11 C 0.7153(3) 0.2777(2) 0.3843(2) 0.0436(5) Uani 1 1 d . . . . .
H11A H 0.650068 0.299241 0.431766 0.065 Uiso 1 1 calc GR . . . .
H11B H 0.792282 0.255429 0.428634 0.065 Uiso 1 1 calc GR . . . .
H11C H 0.665224 0.193011 0.305466 0.065 Uiso 1 1 calc GR . . . .
C25 C 0.6561(2) 0.8387(2) 0.54614(18) 0.0349(4) Uani 1 1 d . . . . .
H25 H 0.730559 0.805704 0.575401 0.042 Uiso 1 1 calc R . . . .
C14 C 0.8168(2) 1.1114(2) -0.02675(19) 0.0398(5) Uani 1 1 d . . . . .
H14 H 0.780740 1.120757 -0.099039 0.048 Uiso 1 1 calc R . . . .
C30 C 0.2112(2) 0.6045(2) 0.2363(2) 0.0363(4) Uani 1 1 d . . . . .
H30A H 0.218421 0.673011 0.318817 0.054 Uiso 1 1 calc GR . . . .
H30B H 0.131510 0.516518 0.207378 0.054 Uiso 1 1 calc GR . . . .
H30C H 0.196737 0.651881 0.181924 0.054 Uiso 1 1 calc GR . . . .
C26 C 0.6129(3) 0.9526(3) 0.6374(2) 0.0447(5) Uani 1 1 d . . . . .
H26A H 0.526105 0.964280 0.596267 0.067 Uiso 1 1 calc GR . . . .
H26B H 0.687591 1.046486 0.675790 0.067 Uiso 1 1 calc GR . . . .
H26C H 0.596935 0.921338 0.699810 0.067 Uiso 1 1 calc GR . . . .
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'
S S 0.3331 0.5567 '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'
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
O8 S1 N10 104.35(8) . . ?
O8 S1 C1 107.52(8) . . ?
O9 S1 O8 120.38(8) . . ?
O9 S1 N10 107.38(8) . . ?
O9 S1 C1 108.58(8) . . ?
N10 S1 C1 108.05(8) . . ?
C28 Si1 C23 106.46(9) . . ?
C29 Si1 C23 109.17(8) . . ?
C29 Si1 C28 109.87(10) . . ?
C29 Si1 C30 111.07(10) . . ?
C30 Si1 C23 108.90(9) . . ?
C30 Si1 C28 111.23(10) . . ?
C20 O10 N22 109.30(13) . . ?
S1 N10 H10 110.3 . . ?
C19 N10 S1 120.71(12) . . ?
C19 N10 H10 110.3 . . ?
C18 N22 O10 106.08(13) . . ?
O10 C20 C19 108.69(15) . . ?
O10 C20 C23 116.64(15) . . ?
C19 C20 C23 134.67(17) . . ?
N22 C18 C19 110.49(15) . . ?
N22 C18 C12 118.60(15) . . ?
C19 C18 C12 130.90(16) . . ?
C6 C1 S1 120.22(14) . . ?
C6 C1 C2 120.97(17) . . ?
C2 C1 S1 118.80(14) . . ?
N10 C19 C18 127.46(15) . . ?
C20 C19 N10 127.07(16) . . ?
C20 C19 C18 105.44(15) . . ?
C17 C12 C18 121.94(16) . . ?
C17 C12 C13 118.54(17) . . ?
C13 C12 C18 119.46(17) . . ?
C20 C23 Si1 122.06(13) . . ?
C24 C23 Si1 119.63(14) . . ?
C24 C23 C20 118.31(16) . . ?
C1 C6 H6 120.5 . . ?
C1 C6 C5 119.04(18) . . ?
C5 C6 H6 120.5 . . ?
C1 C2 H2 120.4 . . ?
C3 C2 C1 119.21(18) . . ?
C3 C2 H2 120.4 . . ?
C12 C17 H17 119.8 . . ?
C16 C17 C12 120.32(18) . . ?
C16 C17 H17 119.8 . . ?
C5 C4 C11 121.0(2) . . ?
C3 C4 C5 118.71(18) . . ?
C3 C4 C11 120.3(2) . . ?
C6 C5 C4 121.05(19) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C25 C24 C23 177.6(2) . . ?
C16 C15 H15 120.4 . . ?
C16 C15 C14 119.14(18) . . ?
C14 C15 H15 120.4 . . ?
Si1 C28 H28A 109.5 . . ?
Si1 C28 H28B 109.5 . . ?
Si1 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C2 C3 C4 121.02(19) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C17 C16 H16 119.5 . . ?
C15 C16 C17 120.91(19) . . ?
C15 C16 H16 119.5 . . ?
C12 C13 H13 119.7 . . ?
C14 C13 C12 120.63(19) . . ?
C14 C13 H13 119.7 . . ?
Si1 C29 H29A 109.5 . . ?
Si1 C29 H29B 109.5 . . ?
Si1 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C4 C11 H11A 109.5 . . ?
C4 C11 H11B 109.5 . . ?
C4 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C24 C25 H25 118.2 . . ?
C24 C25 C26 123.5(2) . . ?
C26 C25 H25 118.2 . . ?
C15 C14 C13 120.45(19) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
Si1 C30 H30A 109.5 . . ?
Si1 C30 H30B 109.5 . . ?
Si1 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O8 1.4407(13) . ?
S1 O9 1.4301(12) . ?
S1 N10 1.6403(15) . ?
S1 C1 1.7625(18) . ?
Si1 C23 1.8981(18) . ?
Si1 C28 1.865(2) . ?
Si1 C29 1.859(2) . ?
Si1 C30 1.863(2) . ?
O10 N22 1.4159(19) . ?
O10 C20 1.352(2) . ?
N10 H10 0.8600 . ?
N10 C19 1.418(2) . ?
N22 C18 1.316(2) . ?
C20 C19 1.367(2) . ?
C20 C23 1.469(2) . ?
C18 C19 1.432(2) . ?
C18 C12 1.482(2) . ?
C1 C6 1.385(3) . ?
C1 C2 1.395(3) . ?
C12 C17 1.391(3) . ?
C12 C13 1.395(3) . ?
C23 C24 1.320(3) . ?
C6 H6 0.9500 . ?
C6 C5 1.392(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.384(3) . ?
C17 H17 0.9500 . ?
C17 C16 1.388(3) . ?
C4 C5 1.396(3) . ?
C4 C3 1.395(3) . ?
C4 C11 1.507(3) . ?
C5 H5 0.9500 . ?
C24 C25 1.304(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.381(3) . ?
C15 C14 1.382(3) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C3 H3 0.9500 . ?
C16 H16 0.9500 . ?
C13 H13 0.9500 . ?
C13 C14 1.389(3) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C25 H25 0.9500 . ?
C25 C26 1.502(3) . ?
C14 H14 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
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
S1 N10 C19 C20 94.88(19) . . . . ?
S1 N10 C19 C18 -87.5(2) . . . . ?
S1 C1 C6 C5 -178.46(14) . . . . ?
S1 C1 C2 C3 178.47(14) . . . . ?
O8 S1 N10 C19 167.77(13) . . . . ?
O8 S1 C1 C6 -146.66(15) . . . . ?
O8 S1 C1 C2 34.06(16) . . . . ?
O9 S1 N10 C19 38.93(15) . . . . ?
O9 S1 C1 C6 -14.93(17) . . . . ?
O9 S1 C1 C2 165.79(14) . . . . ?
O10 N22 C18 C19 -0.16(19) . . . . ?
O10 N22 C18 C12 -179.04(14) . . . . ?
O10 C20 C19 N10 178.25(15) . . . . ?
O10 C20 C19 C18 0.21(19) . . . . ?
O10 C20 C23 Si1 33.2(2) . . . . ?
O10 C20 C23 C24 -146.42(18) . . . . ?
N10 S1 C1 C6 101.23(15) . . . . ?
N10 S1 C1 C2 -78.04(16) . . . . ?
N22 O10 C20 C19 -0.32(18) . . . . ?
N22 O10 C20 C23 178.83(14) . . . . ?
N22 C18 C19 N10 -178.05(16) . . . . ?
N22 C18 C19 C20 0.0(2) . . . . ?
N22 C18 C12 C17 169.95(17) . . . . ?
N22 C18 C12 C13 -7.4(3) . . . . ?
C20 O10 N22 C18 0.30(18) . . . . ?
C18 C12 C17 C16 -177.99(18) . . . . ?
C18 C12 C13 C14 177.78(19) . . . . ?
C1 S1 N10 C19 -78.01(14) . . . . ?
C1 C6 C5 C4 -0.2(3) . . . . ?
C1 C2 C3 C4 0.2(3) . . . . ?
C19 C20 C23 Si1 -147.93(17) . . . . ?
C19 C20 C23 C24 32.5(3) . . . . ?
C19 C18 C12 C17 -8.7(3) . . . . ?
C19 C18 C12 C13 174.03(18) . . . . ?
C12 C18 C19 N10 0.6(3) . . . . ?
C12 C18 C19 C20 178.67(17) . . . . ?
C12 C17 C16 C15 0.2(3) . . . . ?
C12 C13 C14 C15 0.4(3) . . . . ?
C23 C20 C19 N10 -0.7(3) . . . . ?
C23 C20 C19 C18 -178.72(18) . . . . ?
C6 C1 C2 C3 -0.8(3) . . . . ?
C2 C1 C6 C5 0.8(3) . . . . ?
C17 C12 C13 C14 0.4(3) . . . . ?
C5 C4 C3 C2 0.3(3) . . . . ?
C28 Si1 C23 C20 152.99(14) . . . . ?
C28 Si1 C23 C24 -27.39(18) . . . . ?
C3 C4 C5 C6 -0.3(3) . . . . ?
C16 C15 C14 C13 -0.8(3) . . . . ?
C13 C12 C17 C16 -0.7(3) . . . . ?
C29 Si1 C23 C20 34.43(17) . . . . ?
C29 Si1 C23 C24 -145.95(17) . . . . ?
C11 C4 C5 C6 179.39(18) . . . . ?
C11 C4 C3 C2 -179.39(18) . . . . ?
C14 C15 C16 C17 0.6(3) . . . . ?
C30 Si1 C23 C20 -86.99(16) . . . . ?
C30 Si1 C23 C24 92.63(18) . . . . ?
