#------------------------------------------------------------------------------
#$Date: 2023-05-05 06:21:15 +0300 (Fri, 05 May 2023) $
#$Revision: 283466 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/15/92/7159217.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_7159217
loop_
_publ_author_name
'Offei, Samuel D.'
'Arman, Hadi D.'
'Yoshimoto, Francis K.'
_publ_section_title
;
 Synthesis of menarandroside A from dehydroepiandrosterone.
;
_journal_issue                   15
_journal_name_full               'Organic & biomolecular chemistry'
_journal_page_first              3172
_journal_page_last               3176
_journal_paper_doi               10.1039/d3ob00054k
_journal_volume                  21
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C27 H44 O3 Si'
_chemical_formula_sum            'C27 H44 O3 Si'
_chemical_formula_weight         444.71
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-12
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_audit_update_record
;
2020-11-20 deposited with the CCDC.	2023-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                92.2430(10)
_cell_angle_beta                 92.1110(10)
_cell_angle_gamma                102.967(2)
_cell_formula_units_Z            2
_cell_length_a                   6.38390(10)
_cell_length_b                   11.7026(2)
_cell_length_c                   17.9956(2)
_cell_measurement_reflns_used    22416
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.6290
_cell_measurement_theta_min      2.4660
_cell_volume                     1307.69(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_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 0.963
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -76.00  -4.00   0.50    0.10    --  -46.75 108.00  42.00  144
  2  ω     24.00  79.00   0.50    0.10    --   46.75-108.00 -54.00  110
  3  ω   -139.00-104.00   0.50    0.40    --  -88.50-108.00 -54.00   70
  4  ω    -73.00 -48.00   0.50    0.40    --  -88.50 108.00  42.00   50
  5  ω     48.00 107.00   0.50    0.40    --  105.44-108.00 -54.00  118
  6  ω    113.00 154.00   0.50    0.40    --  105.44 108.00  42.00   82
  7  ω     -7.00  22.00   0.50    0.10    --   12.00  74.00 171.16   58
  8  ω    -26.00   0.00   0.50    0.10    --  -24.00 -76.00  80.75   52
  9  ω      7.00  32.00   0.50    0.10    --   28.00  70.00 -51.76   50
 10  ω      7.00  32.00   0.50    0.10    --   28.00  70.00-156.80   50
 11  ω     13.00  38.00   0.50    0.10    --   32.00  65.00  22.17   50
 12  ω     18.00  43.00   0.50    0.10    --   36.00  63.00 -37.32   50
 13  ω     18.00  43.00   0.50    0.10    --   36.00  63.00  91.90   50
 14  ω     18.00  43.00   0.50    0.10    --   36.00  63.00-115.06   50
 15  ω     22.00  48.00   0.50    0.10    --   36.00  60.00-157.84   52
 16  ω    -48.00 -23.00   0.50    0.10    --  -40.00 -61.00  17.83   50
 17  ω     31.00  57.00   0.50    0.10    --   40.00  57.00  51.21   52
 18  ω     23.00  48.00   0.50    0.10    --   40.00  59.00 163.19   50
 19  ω     23.00  48.00   0.50    0.10    --   40.00  60.00 -90.15   50
 20  ω    -60.00 -29.00   0.50    0.10    --  -46.75  57.00  60.00   62
 21  ω     -1.00  26.00   0.50    0.10    --  -46.75  57.00  60.00   54
 22  ω     59.00  95.00   0.50    0.10    --   46.75-125.00-150.00   72
 23  ω     34.00  59.00   0.50    0.10    --   46.75  52.00 141.41   50
 24  ω   -108.00 -82.00   0.50    0.10    --  -56.00 -56.00-117.42   52
 25  ω    -73.00 -40.00   0.50    0.10    --  -56.00 -56.00 -40.67   66
 26  ω    -70.00 -43.00   0.50    0.10    --  -56.00 -55.00-144.81   54
 27  ω   -128.00-102.00   0.50    0.10    --  -56.00 -56.00 137.15   52
 28  ω    -82.00 -41.00   0.50    0.10    --  -56.00 -56.00 137.15   82
 29  ω   -100.00 -75.00   0.50    0.10    --  -56.00 -56.00 -40.67   50
 30  ω   -127.00 -84.00   0.50    0.10    --  -56.00 -52.00  84.01   86
 31  ω    -76.00 -43.00   0.50    0.10    --  -56.00 -52.00  84.01   66
 32  ω    -68.00 -41.00   0.50    0.10    --  -56.00 -56.00-117.42   54
 33  ω   -113.00 -45.00   0.50    0.10    --  -60.00 -54.00  36.85  136
 34  ω   -117.00 -91.00   0.50    0.40    --  -68.00 -52.00 -14.60   52
 35  ω    -91.00 -52.00   0.50    0.40    --  -68.00 -55.00 -67.82   78
 36  ω    -91.00 -55.00   0.50    0.40    --  -68.00 -52.00 168.11   72
 37  ω    -78.00 -53.00   0.50    0.40    --  -68.00 -52.00 -14.60   50
 38  ω    -81.00 -55.00   0.50    0.40    --  -72.00 -54.00  79.70   52
 39  ω    -86.00 -60.00   0.50    0.40    --  -76.00 -51.00-120.13   52
 40  ω    -85.00 -60.00   0.50    0.40    --  -76.00 -56.00 -79.21   50
 41  ω    -87.00 -61.00   0.50    0.40    --  -76.00 -54.00-170.38   52
 42  ω    -85.00 -59.00   0.50    0.40    --  -76.00 -54.00  16.96   52
 43  ω    -91.00 -65.00   0.50    0.40    --  -80.00 -51.00  41.32   52
 44  ω    -91.00 -65.00   0.50    0.40    --  -80.00 -55.00 123.58   52
 45  ω    -89.00 -63.00   0.50    0.40    --  -80.00 -54.00 147.11   52
 46  ω    -90.00 -64.00   0.50    0.40    --  -80.00 -56.00 -22.86   52
 47  ω    -98.00 -73.00   0.50    0.40    --  -88.50 -54.00-170.25   50
 48  ω   -160.00-127.00   0.50    0.40    --  -88.50 -94.00-120.00   66
 49  ω   -121.00 -73.00   0.50    0.40    --  -88.50 -54.00  80.36   96
 50  ω   -108.00 -72.00   0.50    0.40    --  -88.50 -54.00 -89.29   72
 51  ω   -113.00 -74.00   0.50    0.40    --  -88.50 -55.00-174.24   78
 52  ω   -159.00-111.00   0.50    0.40    --  -88.50 -54.00 -89.29   96
 53  ω   -160.00-127.00   0.50    0.40    --  -88.50 -51.00 -51.35   66
 54  ω   -157.00-125.00   0.50    0.40    --  -88.50 -49.00-116.17   64
 55  ω    -98.00 -73.00   0.50    0.40    --  -88.50 -55.00 -32.76   50
 56  ω   -134.00-108.00   0.50    0.40    --  -88.50 -55.00 -32.76   52
 57  ω   -100.00 -74.00   0.50    0.40    --  -88.50 -55.00-136.05   52
 58  ω   -106.00 -72.00   0.50    0.40    --  -88.50 -51.00 -51.35   68
 59  ω   -100.00 -73.00   0.50    0.40    --  -88.50 -53.00 119.32   54
 60  ω   -106.00 -73.00   0.50    0.40    --  -88.50 -52.00-152.18   66
 61  ω   -159.00-113.00   0.50    0.40    --  -88.50 -52.00-152.18   92
 62  ω   -101.00 -75.00   0.50    0.40    --  -88.50 -49.00-116.17   52
 63  ω   -160.00-108.00   0.50    0.40    --  -88.50 -55.00-136.05  104
 64  ω   -155.00-129.00   0.50    0.40    --  -88.50 -54.00-170.25   52
 65  ω   -116.00 -74.00   0.50    0.40    --  -88.50 -53.00 -78.80   84
 66  ω   -144.00-118.00   0.50    0.40    --  -88.50 -77.00 -30.00   52
 67  ω   -159.00-123.00   0.50    0.40    --  -88.50 -55.00-174.24   72
 68  ω   -102.00 -76.00   0.50    0.40    --  -88.50 -52.00 152.11   52
 69  ω   -158.00-123.00   0.50    0.40    --  -88.50 -52.00 152.11   70
 70  ω   -100.00 -73.00   0.50    0.40    --  -88.50 -52.00  42.61   54
 71  ω    -48.00 -23.00   0.50    0.40    --  -88.50  45.00 120.00   50
 72  ω    -68.00 -19.00   0.50    0.40    --  -88.50  77.00-180.00   98
 73  ω   -106.00 -73.00   0.50    0.40    --  -88.50 -53.00  26.61   66
 74  ω   -157.00-122.00   0.50    0.40    --  -88.50 -53.00  26.61   70
 75  ω   -116.00 -73.00   0.50    0.40    --  -88.50 -52.00-129.01   86
 76  ω   -100.00 -74.00   0.50    0.40    --  -88.50 -53.00-118.71   52
 77  ω   -150.00-124.00   0.50    0.40    --  -88.50 -52.00-129.01   52
 78  ω   -102.00 -73.00   0.50    0.40    --  -88.50 -53.00 102.73   58
 79  ω   -109.00 -73.00   0.50    0.40    --  -88.50 -55.00  13.23   72
 80  ω    -99.00 -73.00   0.50    0.40    --  -88.50 -51.00 137.42   52
 81  ω   -145.00-119.00   0.50    0.40    --  -88.50 -55.00  13.23   52
 82  ω   -148.00-122.00   0.50    0.40    --  -88.50 -51.00 137.42   52
 83  ω   -158.00-133.00   0.50    0.40    --  -88.50 -53.00 170.63   50
 84  ω   -109.00 -74.00   0.50    0.40    --  -88.50 -53.00 170.63   70
 85  ω   -115.00 -81.00   0.50    0.40    --  -88.50 -56.00  -9.61   68
 86  ω   -160.00-124.00   0.50    0.40    --  -88.50 -56.00  -9.61   72
 87  ω     33.00 105.00   0.50    0.40    --  105.44 -94.00  90.00  144
 88  ω     33.00  96.00   0.50    0.40    --  105.44 -94.00-180.00  126
 89  ω     34.00  60.00   0.50    0.40    --  105.44 -61.00 120.00   52
 90  ω     35.00  71.00   0.50    0.40    --  105.44 -61.00-120.00   72
 91  ω     35.00 111.00   0.50    0.40    --  105.44-125.00 -90.00  152
 92  ω     34.00  60.00   0.50    0.40    --  105.44 -61.00  30.00   52
 93  ω     96.00 176.00   0.50    0.40    --  105.44  61.00  30.00  160
 94  ω    135.00 170.00   0.50    0.40    --  105.44  61.00 -30.00   70
 95  ω     92.00 131.00   0.50    0.40    --  105.44  61.00 -30.00   78
 96  ω     35.00 104.00   0.50    0.40    --  105.44 -94.00  60.00  138
 97  ω     56.00  99.00   0.50    0.40    --  105.44 -94.00 -30.00   86
 98  ω     77.00 105.00   0.50    0.40    --  105.44 -94.00   0.00   56
 99  ω     34.00  73.00   0.50    0.40    --  105.44 -94.00   0.00   78
100  ω     37.00  71.00   0.50    0.40    --  105.44 -61.00  90.00   68
101  ω     91.00 177.00   0.50    0.40    --  105.44  61.00  90.00  172
102  ω     33.00  58.00   0.50    0.40    --  105.44 -61.00 -60.00   50
103  ω    128.00 178.00   0.50    0.40    --  105.44  61.00  12.37  100
104  ω     93.00 123.00   0.50    0.40    --  105.44  61.00  12.37   60
105  ω     84.00 110.00   0.50    0.10    --   46.75  57.00  90.00   52
106  ω    -84.00 -36.00   0.50    0.10    --  -52.00 -56.00-153.16   96
107  ω   -128.00 -94.00   0.50    0.10    --  -56.00 -55.00  -4.07   68
108  ω    -68.00 -42.00   0.50    0.10    --  -56.00 -55.00  -4.07   52
109  ω    -66.00 -40.00   0.50    0.10    --  -56.00 -55.00  89.20   52
110  ω   -126.00-100.00   0.50    0.40    --  -76.00 -56.00 -48.39   52
111  ω    -87.00 -61.00   0.50    0.40    --  -76.00 -56.00  97.00   52
112  ω    -85.00 -60.00   0.50    0.40    --  -76.00 -56.00 -48.39   50
113  ω    -92.00 -67.00   0.50    0.40    --  -84.00 -54.00 -68.66   50
114  ω   -127.00 -77.00   0.50    0.40    --  -88.50 -52.00 157.71  100
115  ω   -109.00 -76.00   0.50    0.40    --  -88.50 -54.00  53.34   66
116  ω    -99.00 -73.00   0.50    0.40    --  -88.50 -53.00-162.96   52
117  ω   -157.00-131.00   0.50    0.40    --  -88.50 -53.00-162.96   52
118  ω   -158.00-132.00   0.50    0.40    --  -88.50 -54.00  53.34   52
119  ω    -71.00 -46.00   0.50    0.40    --  -88.50  61.00   0.00   50
120  ω     80.00 106.00   0.50    0.40    --  105.44 -99.00 103.86   52
121  ω     84.00 110.00   0.50    0.40    --  105.44-125.00 -60.00   52
122  ω     92.00 118.00   0.50    0.40    --  105.44  61.00 120.00   52
123  ω     80.00 105.00   0.50    0.40    --  105.44 -94.00  30.00   50
124  ω     33.00  59.00   0.50    0.40    --  105.44 -94.00  30.00   52
125  ω    100.00 143.00   0.50    0.40    --  105.44  62.00-133.10   86
126  ω     37.00  63.00   0.50    0.40    --  105.44 -61.00 120.00   52
127  ω    131.00 157.00   0.50    0.40    --  105.44  61.00 120.00   52
128  ω    122.00 162.00   0.50    0.40    --  105.44  15.00 -60.00   80
129  ω     37.00  66.00   0.50    0.40    --  105.44 -61.00-150.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0194343000
_diffrn_orient_matrix_UB_12      0.0404382000
_diffrn_orient_matrix_UB_13      0.0829693000
_diffrn_orient_matrix_UB_21      0.2359394000
_diffrn_orient_matrix_UB_22      0.0637919000
_diffrn_orient_matrix_UB_23      -0.0088063000
_diffrn_orient_matrix_UB_31      -0.0735680000
_diffrn_orient_matrix_UB_32      0.1121934000
_diffrn_orient_matrix_UB_33      -0.0198648000
_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  0.0590
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39956
_diffrn_reflns_point_group_measured_fraction_full 0.941
_diffrn_reflns_point_group_measured_fraction_max 0.876
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.934
_diffrn_reflns_theta_min         2.460
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.969
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.398
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.63a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_description       block
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.246
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 3815 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.020(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         9535
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0601
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0200P)²+2.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1445
_refine_ls_wR_factor_ref         0.1457
_reflns_Friedel_coverage         0.819
_reflns_Friedel_fraction_full    0.882
_reflns_Friedel_fraction_max     0.789
_reflns_number_gt                9072
_reflns_number_total             9535
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3ob00054k2.cif
_cod_data_source_block           hpd200
_cod_depositor_comments
'Adding full bibliography for 7159215--7159218.cif.'
_cod_database_code               7159217
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O'
_chemical_oxdiff_usercomment     SODXVI_060
_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   0.946
_shelx_estimated_absorpt_t_min   0.796
_reflns_odcompleteness_completeness 99.98
_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 C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C5(H5), C1(H1), C13(H13), C39(H39), C40(H40), C28(H28), C32(H32), C12(H12)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C6(H6A,H6B), C17(H17A,H17B), C29(H29A,H29B), C33(H33A,H33B),
 C38(H38A,H38B), C30(H30A,H30B), C14(H14A,H14B), C11(H11A,H11B), C44(H44A,H44B),
  C3(H3A,H3B), C37(H37A,H37B), C10(H10A,H10B), C41(H41A,H41B)
2.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C53(H53), C42(H42), C26(H26)
2.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C51(H51A,H51B,H51C), C49(H49A,H49B,H49C), C21(H21A,H21B,
 H21C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C46(H46A,H46B,H46C), C19(H19A,
 H19B,H19C), C25(H25A,H25B,H25C), C23(H23A,H23B,H23C), C45(H45A,H45B,H45C),
 C18(H18A,H18B,H18C), C54(H54A,H54B,H54C), C48(H48A,H48B,H48C), C22(H22A,H22B,
 H22C), C27(H27A,H27B,H27C)
;
_olex2_exptl_crystal_mounting_method 'nylon loop'
_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 1.824
_oxdiff_exptl_absorpt_empirical_full_min 0.652
loop_
_space_group_symop_operation_xyz
'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
Si2 Si 0.12388(19) 0.80822(12) 0.85916(8) 0.0319(3) Uani 1 1 d . . . . .
Si1 Si 0.9759(2) 0.24392(13) 0.13086(8) 0.0362(3) Uani 1 1 d . . . . .
O1 O 0.7972(5) 0.2714(3) 0.18821(19) 0.0340(8) Uani 1 1 d . . . . .
O4 O 0.1940(6) 0.7183(3) 0.79695(19) 0.0359(8) Uani 1 1 d . . . . .
O6 O 0.5858(7) 0.5942(4) 0.1960(2) 0.0504(11) Uani 1 1 d . . . . .
O2 O 0.7032(8) 0.4520(4) 0.6665(2) 0.0576(12) Uani 1 1 d . . . . .
O5 O 0.7506(6) 0.6794(5) 0.3504(2) 0.0623(14) Uani 1 1 d . . . . .
C5 C 0.6873(8) 0.2708(4) 0.5034(3) 0.0297(10) Uani 1 1 d . . . . .
H5 H 0.845372 0.306371 0.506328 0.036 Uiso 1 1 calc R U . . .
C1 C 0.8158(8) 0.2780(4) 0.2672(3) 0.0295(11) Uani 1 1 d . . . . .
H1 H 0.971642 0.299644 0.283593 0.035 Uiso 1 1 calc R U . . .
C4 C 0.6229(7) 0.2583(4) 0.4190(3) 0.0269(10) Uani 1 1 d . . . . .
C13 C 0.6633(8) 0.1517(4) 0.5396(3) 0.0298(10) Uani 1 1 d . . . . .
H13 H 0.509872 0.107830 0.532402 0.036 Uiso 1 1 calc R U . . .
C7 C 0.6230(9) 0.3624(5) 0.6308(3) 0.0379(12) Uani 1 1 d . . . . .
C39 C 0.3264(9) 0.8087(5) 0.3620(3) 0.0326(11) Uani 1 1 d . . . . .
H39 H 0.463053 0.867726 0.375750 0.039 Uiso 1 1 calc R U . . .
C2 C 0.7050(9) 0.3707(5) 0.2983(3) 0.0325(11) Uani 1 1 d . . . . .
H2A H 0.552094 0.351839 0.280364 0.039 Uiso 1 1 calc R U . . .
H2B H 0.774333 0.448323 0.280302 0.039 Uiso 1 1 calc R U . . .
C34 C 0.5712(8) 0.6792(5) 0.3697(3) 0.0391(12) Uani 1 1 d . . . . .
C40 C 0.2222(9) 0.7748(5) 0.4346(3) 0.0312(11) Uani 1 1 d . . . . .
H40 H 0.095280 0.707655 0.424179 0.037 Uiso 1 1 calc R U . . .
C6 C 0.5851(9) 0.3596(5) 0.5465(3) 0.0379(13) Uani 1 1 d . . . . .
H6A H 0.644031 0.439033 0.528988 0.046 Uiso 1 1 calc R U . . .
H6B H 0.428146 0.340116 0.534611 0.046 Uiso 1 1 calc R U . . .
C28 C 0.2691(9) 0.7466(5) 0.7249(3) 0.0329(11) Uani 1 1 d . . . . .
H28 H 0.373466 0.824563 0.728392 0.039 Uiso 1 1 calc R U . . .
C15 C 0.7980(8) 0.0856(4) 0.4195(3) 0.0318(11) Uani 1 1 d . . . . .
H15 H 0.858491 0.031109 0.391909 0.038 Uiso 1 1 calc R U . . .
C31 C 0.2815(8) 0.6864(4) 0.5597(3) 0.0277(10) Uani 1 1 d . . . . .
C17 C 0.7130(8) 0.1592(4) 0.2974(3) 0.0307(10) Uani 1 1 d . . . . .
H17A H 0.562675 0.134206 0.277139 0.037 Uiso 1 1 calc R U . . .
H17B H 0.791916 0.100254 0.279888 0.037 Uiso 1 1 calc R U . . .
O3 O 0.4095(10) 0.3531(6) 0.7889(3) 0.0831(19) Uani 1 1 d . . . . .
C24 C 0.3747(8) 0.2266(5) 0.4057(3) 0.0345(11) Uani 1 1 d . . . . .
H24A H 0.311662 0.164361 0.438472 0.052 Uiso 1 1 calc R U . . .
H24B H 0.338010 0.199308 0.353675 0.052 Uiso 1 1 calc R U . . .
H24C H 0.317678 0.296245 0.416566 0.052 Uiso 1 1 calc R U . . .
C29 C 0.3816(9) 0.6534(5) 0.6960(3) 0.0360(12) Uani 1 1 d . . . . .
H29A H 0.280056 0.575655 0.694022 0.043 Uiso 1 1 calc R U . . .
H29B H 0.504318 0.650231 0.730496 0.043 Uiso 1 1 calc R U . . .
C33 C 0.5086(9) 0.6509(5) 0.4488(3) 0.0388(13) Uani 1 1 d . . . . .
H33A H 0.641129 0.651531 0.479290 0.047 Uiso 1 1 calc R U . . .
H33B H 0.417685 0.570279 0.447855 0.047 Uiso 1 1 calc R U . . .
C38 C 0.2107(11) 0.8623(5) 0.3013(3) 0.0454(14) Uani 1 1 d . . . . .
H38A H 0.200451 0.943081 0.316345 0.054 Uiso 1 1 calc R U . . .
H38B H 0.064457 0.813829 0.288992 0.054 Uiso 1 1 calc R U . . .
C30 C 0.4629(9) 0.6801(5) 0.6185(3) 0.0358(12) Uani 1 1 d . . . . .
H30A H 0.537004 0.618576 0.601696 0.043 Uiso 1 1 calc R U . . .
H30B H 0.569971 0.756018 0.621531 0.043 Uiso 1 1 calc R U . . .
C43 C 0.1518(9) 0.7699(5) 0.5919(3) 0.0333(11) Uani 1 1 d . . . . .
C8 C 0.5683(8) 0.2407(5) 0.6629(3) 0.0361(12) Uani 1 1 d . . . . .
C14 C 0.8039(8) 0.0799(5) 0.5018(3) 0.0326(11) Uani 1 1 d . . . . .
H14A H 0.954366 0.108480 0.521362 0.039 Uiso 1 1 calc R U . . .
H14B H 0.756036 -0.003090 0.514729 0.039 Uiso 1 1 calc R U . . .
C53 C 0.5365(9) 0.7024(6) 0.1897(3) 0.0425(13) Uani 1 1 d . . . . .
H53 H 0.567580 0.742692 0.145220 0.051 Uiso 1 1 calc R U . . .
C32 C 0.3863(8) 0.7351(4) 0.4874(3) 0.0294(10) Uani 1 1 d . . . . .
H32 H 0.497205 0.807706 0.503266 0.035 Uiso 1 1 calc R U . . .
C11 C 0.7337(9) 0.0758(5) 0.6740(3) 0.0417(13) Uani 1 1 d . . . . .
H11A H 0.858859 0.041973 0.663184 0.050 Uiso 1 1 calc R U . . .
H11B H 0.601252 0.012461 0.670190 0.050 Uiso 1 1 calc R U . . .
C44 C 0.0829(9) 0.7516(5) 0.6701(3) 0.0364(12) Uani 1 1 d . . . . .
H44A H -0.027645 0.677329 0.670973 0.044 Uiso 1 1 calc R U . . .
H44B H 0.016224 0.816363 0.686592 0.044 Uiso 1 1 calc R U . . .
C16 C 0.7138(7) 0.1620(4) 0.3811(3) 0.0279(10) Uani 1 1 d . . . . .
C47 C 0.1308(8) 0.7324(5) 0.9496(3) 0.0387(12) Uani 1 1 d . . . . .
C3 C 0.7187(9) 0.3756(4) 0.3831(3) 0.0322(11) Uani 1 1 d . . . . .
H3A H 0.642963 0.435437 0.401482 0.039 Uiso 1 1 calc R U . . .
H3B H 0.871863 0.401851 0.400165 0.039 Uiso 1 1 calc R U . . .
C51 C 0.1319(8) 0.5646(5) 0.5453(3) 0.0339(11) Uani 1 1 d . . . . .
H51A H 0.218096 0.506485 0.535640 0.051 Uiso 1 1 calc R U . . .
H51B H 0.034895 0.565765 0.501968 0.051 Uiso 1 1 calc R U . . .
H51C H 0.047102 0.543580 0.589048 0.051 Uiso 1 1 calc R U . . .
C49 C 0.0775(11) 0.8084(6) 1.0147(3) 0.0499(15) Uani 1 1 d . . . . .
H49A H 0.179070 0.885007 1.017405 0.075 Uiso 1 1 calc R U . . .
H49B H 0.088887 0.769264 1.061419 0.075 Uiso 1 1 calc R U . . .
H49C H -0.069323 0.819263 1.006932 0.075 Uiso 1 1 calc R U . . .
C36 C 0.4465(9) 0.7522(5) 0.2442(3) 0.0367(12) Uani 1 1 d . . . . .
C12 C 0.7172(8) 0.1726(5) 0.6221(3) 0.0320(11) Uani 1 1 d . . . . .
H12 H 0.862828 0.227004 0.625910 0.038 Uiso 1 1 calc R U . . .
C9 C 0.6298(9) 0.2321(6) 0.7441(3) 0.0427(13) Uani 1 1 d . . . . .
C35 C 0.3931(7) 0.7052(5) 0.3198(3) 0.0300(10) Uani 1 1 d . . . . .
C21 C 0.6556(10) 0.2410(7) 0.0197(3) 0.0537(17) Uani 1 1 d . . . . .
H21A H 0.564574 0.255063 0.060227 0.081 Uiso 1 1 calc R U . . .
H21B H 0.564987 0.198576 -0.022191 0.081 Uiso 1 1 calc R U . . .
H21C H 0.737779 0.316343 0.003565 0.081 Uiso 1 1 calc R U . . .
C42 C 0.1010(11) 0.8551(5) 0.5521(3) 0.0465(15) Uani 1 1 d . . . . .
H42 H 0.028512 0.907048 0.576874 0.056 Uiso 1 1 calc R U . . .
C50 C 0.3547(9) 0.7091(6) 0.9654(3) 0.0448(14) Uani 1 1 d . . . . .
H50A H 0.389270 0.659481 0.924651 0.067 Uiso 1 1 calc R U . . .
H50B H 0.356227 0.669175 1.012205 0.067 Uiso 1 1 calc R U . . .
H50C H 0.461699 0.783877 0.969433 0.067 Uiso 1 1 calc R U . . .
C37 C 0.3570(12) 0.8620(5) 0.2358(3) 0.0479(15) Uani 1 1 d . . . . .
H37A H 0.474714 0.933583 0.238437 0.057 Uiso 1 1 calc R U . . .
H37B H 0.274218 0.857901 0.187820 0.057 Uiso 1 1 calc R U . . .
C52 C 0.2094(8) 0.5949(5) 0.3089(3) 0.0346(11) Uani 1 1 d . . . . .
H52A H 0.161629 0.567672 0.357606 0.052 Uiso 1 1 calc R U . . .
H52B H 0.260686 0.533021 0.281792 0.052 Uiso 1 1 calc R U . . .
H52C H 0.088792 0.613701 0.280381 0.052 Uiso 1 1 calc R U . . .
C10 C 0.7626(10) 0.1401(6) 0.7506(3) 0.0481(15) Uani 1 1 d . . . . .
H10A H 0.709274 0.085365 0.789803 0.058 Uiso 1 1 calc R U . . .
H10B H 0.915995 0.177379 0.762436 0.058 Uiso 1 1 calc R U . . .
C41 C 0.1472(11) 0.8757(5) 0.4734(3) 0.0462(15) Uani 1 1 d . . . . .
H41A H 0.259868 0.948688 0.470721 0.055 Uiso 1 1 calc R U . . .
H41B H 0.015667 0.887078 0.446635 0.055 Uiso 1 1 calc R U . . .
C46 C 0.3139(9) 0.9553(5) 0.8626(3) 0.0428(13) Uani 1 1 d . . . . .
H46A H 0.461514 0.945900 0.870988 0.064 Uiso 1 1 calc R U . . .
H46B H 0.278113 1.004670 0.903249 0.064 Uiso 1 1 calc R U . . .
H46C H 0.301817 0.992545 0.815240 0.064 Uiso 1 1 calc R U . . .
C20 C 0.8117(9) 0.1675(6) 0.0473(3) 0.0431(13) Uani 1 1 d . . . . .
C19 C 1.1554(10) 0.3853(6) 0.1051(4) 0.0558(17) Uani 1 1 d . . . . .
H19A H 1.067227 0.438150 0.087249 0.084 Uiso 1 1 calc R U . . .
H19B H 1.248516 0.369501 0.065705 0.084 Uiso 1 1 calc R U . . .
H19C H 1.244356 0.422305 0.148884 0.084 Uiso 1 1 calc R U . . .
C25 C 0.3280(9) 0.1808(6) 0.6483(4) 0.0520(16) Uani 1 1 d . . . . .
H25A H 0.239959 0.222772 0.677625 0.078 Uiso 1 1 calc R U . . .
H25B H 0.302737 0.099186 0.662826 0.078 Uiso 1 1 calc R U . . .
H25C H 0.288944 0.182560 0.595273 0.078 Uiso 1 1 calc R U . . .
C23 C 0.6811(11) 0.0464(6) 0.0692(4) 0.0544(16) Uani 1 1 d . . . . .
H23A H 0.780197 -0.001633 0.085532 0.082 Uiso 1 1 calc R U . . .
H23B H 0.592101 0.006805 0.026135 0.082 Uiso 1 1 calc R U . . .
H23C H 0.588442 0.057289 0.109903 0.082 Uiso 1 1 calc R U . . .
C45 C -0.1527(9) 0.8322(6) 0.8390(3) 0.0475(14) Uani 1 1 d . . . . .
H45A H -0.151472 0.879711 0.795323 0.071 Uiso 1 1 calc R U . . .
H45B H -0.197445 0.873284 0.882058 0.071 Uiso 1 1 calc R U . . .
H45C H -0.253864 0.756256 0.829215 0.071 Uiso 1 1 calc R U . . .
C26 C 0.5567(13) 0.2839(7) 0.8004(4) 0.065(2) Uani 1 1 d . . . . .
H26 H 0.605397 0.273698 0.849753 0.078 Uiso 1 1 calc R U . . .
C18 C 1.1440(11) 0.1477(7) 0.1728(4) 0.0576(18) Uani 1 1 d . . . . .
H18A H 1.225395 0.188414 0.217095 0.086 Uiso 1 1 calc R U . . .
H18B H 1.244192 0.130370 0.136316 0.086 Uiso 1 1 calc R U . . .
H18C H 1.050043 0.074225 0.186903 0.086 Uiso 1 1 calc R U . . .
C54 C 0.7245(11) 0.5685(7) 0.1415(3) 0.0548(17) Uani 1 1 d . . . . .
H54A H 0.663801 0.577780 0.091874 0.082 Uiso 1 1 calc R U . . .
H54B H 0.740077 0.487532 0.145536 0.082 Uiso 1 1 calc R U . . .
H54C H 0.865875 0.622451 0.149266 0.082 Uiso 1 1 calc R U . . .
C48 C -0.0357(10) 0.6141(6) 0.9433(4) 0.0493(14) Uani 1 1 d . . . . .
H48A H -0.179268 0.628029 0.932654 0.074 Uiso 1 1 calc R U . . .
H48B H -0.034509 0.574687 0.990361 0.074 Uiso 1 1 calc R U . . .
H48C H 0.000913 0.564393 0.902995 0.074 Uiso 1 1 calc R U . . .
C22 C 0.9596(12) 0.1486(7) -0.0158(4) 0.0616(19) Uani 1 1 d . . . . .
H22A H 1.037301 0.224872 -0.031950 0.092 Uiso 1 1 calc R U . . .
H22B H 0.872375 0.104353 -0.057861 0.092 Uiso 1 1 calc R U . . .
H22C H 1.063056 0.104435 0.002431 0.092 Uiso 1 1 calc R U . . .
C27 C 0.3880(19) 0.4280(9) 0.8468(5) 0.097(3) Uani 1 1 d . . . . .
H27A H 0.254121 0.454570 0.838971 0.145 Uiso 1 1 calc R U . . .
H27B H 0.510395 0.495900 0.849443 0.145 Uiso 1 1 calc R U . . .
H27C H 0.383873 0.387233 0.893429 0.145 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 7 -3 0.0842
-3 -3 -3 0.1309
2 -7 3 0.1010
3 3 3 0.0879
0 0 -12 0.0327
-1 1 11 0.0019
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 Si2 C47 104.2(2) . . ?
O4 Si2 C46 110.9(2) . . ?
O4 Si2 C45 112.8(2) . . ?
C46 Si2 C47 112.2(3) . . ?
C46 Si2 C45 107.1(3) . . ?
C45 Si2 C47 109.7(3) . . ?
O1 Si1 C20 104.4(2) . . ?
O1 Si1 C19 109.7(3) . . ?
O1 Si1 C18 111.8(2) . . ?
C20 Si1 C18 110.8(3) . . ?
C19 Si1 C20 110.6(3) . . ?
C19 Si1 C18 109.5(3) . . ?
C1 O1 Si1 127.0(3) . . ?
C28 O4 Si2 126.6(3) . . ?
C53 O6 C54 113.6(5) . . ?
C4 C5 H5 105.1 . . ?
C13 C5 H5 105.1 . . ?
C13 C5 C4 113.0(4) . . ?
C13 C5 C6 114.1(4) . . ?
C6 C5 H5 105.1 . . ?
C6 C5 C4 113.3(4) . . ?
O1 C1 H1 109.1 . . ?
O1 C1 C2 110.3(4) . . ?
O1 C1 C17 110.1(4) . . ?
C2 C1 H1 109.1 . . ?
C2 C1 C17 109.2(4) . . ?
C17 C1 H1 109.1 . . ?
C24 C4 C5 111.1(4) . . ?
C16 C4 C5 110.5(4) . . ?
C16 C4 C24 108.4(4) . . ?
C16 C4 C3 108.2(4) . . ?
C3 C4 C5 108.8(4) . . ?
C3 C4 C24 109.8(4) . . ?
C5 C13 H13 108.4 . . ?
C14 C13 C5 110.0(4) . . ?
C14 C13 H13 108.4 . . ?
C12 C13 C5 109.2(4) . . ?
C12 C13 H13 108.4 . . ?
C12 C13 C14 112.5(4) . . ?
O2 C7 C6 121.9(5) . . ?
O2 C7 C8 124.5(5) . . ?
C6 C7 C8 113.3(5) . . ?
C40 C39 H39 106.1 . . ?
C40 C39 C38 121.2(5) . . ?
C40 C39 C35 113.3(4) . . ?
C38 C39 H39 106.1 . . ?
C38 C39 C35 103.2(4) . . ?
C35 C39 H39 106.1 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 C3 110.5(4) . . ?
H2A C2 H2B 108.1 . . ?
C3 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
O5 C34 C33 120.6(5) . . ?
O5 C34 C35 124.7(5) . . ?
C35 C34 C33 114.7(4) . . ?
C39 C40 H40 108.8 . . ?
C39 C40 C32 109.0(4) . . ?
C39 C40 C41 112.6(4) . . ?
C32 C40 H40 108.8 . . ?
C41 C40 H40 108.8 . . ?
C41 C40 C32 108.6(4) . . ?
C5 C6 H6A 108.7 . . ?
C5 C6 H6B 108.7 . . ?
C7 C6 C5 114.3(4) . . ?
C7 C6 H6A 108.7 . . ?
C7 C6 H6B 108.7 . . ?
H6A C6 H6B 107.6 . . ?
O4 C28 H28 109.2 . . ?
O4 C28 C29 109.4(4) . . ?
O4 C28 C44 111.1(4) . . ?
C29 C28 H28 109.2 . . ?
C29 C28 C44 108.6(4) . . ?
C44 C28 H28 109.2 . . ?
C14 C15 H15 117.5 . . ?
C16 C15 H15 117.5 . . ?
C16 C15 C14 125.0(4) . . ?
C43 C31 C30 107.6(4) . . ?
C43 C31 C32 109.9(4) . . ?
C43 C31 C51 108.8(4) . . ?
C32 C31 C30 108.8(4) . . ?
C51 C31 C30 109.9(4) . . ?
C51 C31 C32 111.8(4) . . ?
C1 C17 H17A 109.0 . . ?
C1 C17 H17B 109.0 . . ?
H17A C17 H17B 107.8 . . ?
C16 C17 C1 112.9(4) . . ?
C16 C17 H17A 109.0 . . ?
C16 C17 H17B 109.0 . . ?
C27 O3 C26 116.4(7) . . ?
C4 C24 H24A 109.5 . . ?
C4 C24 H24B 109.5 . . ?
C4 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 C30 110.9(4) . . ?
H29A C29 H29B 108.0 . . ?
C30 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
C34 C33 H33A 108.4 . . ?
C34 C33 H33B 108.4 . . ?
C34 C33 C32 115.4(5) . . ?
H33A C33 H33B 107.5 . . ?
C32 C33 H33A 108.4 . . ?
C32 C33 H33B 108.4 . . ?
C39 C38 H38A 111.3 . . ?
C39 C38 H38B 111.3 . . ?
C39 C38 C37 102.3(5) . . ?
H38A C38 H38B 109.2 . . ?
C37 C38 H38A 111.3 . . ?
C37 C38 H38B 111.3 . . ?
C31 C30 H30A 108.9 . . ?
C31 C30 H30B 108.9 . . ?
C29 C30 C31 113.5(4) . . ?
C29 C30 H30A 108.9 . . ?
C29 C30 H30B 108.9 . . ?
H30A C30 H30B 107.7 . . ?
C44 C43 C31 116.7(4) . . ?
C42 C43 C31 121.7(5) . . ?
C42 C43 C44 121.6(5) . . ?
C7 C8 C12 103.8(4) . . ?
C7 C8 C25 111.5(5) . . ?
C9 C8 C7 117.3(5) . . ?
C9 C8 C12 102.9(4) . . ?
C9 C8 C25 109.1(5) . . ?
C25 C8 C12 111.8(5) . . ?
C13 C14 H14A 108.9 . . ?
C13 C14 H14B 108.9 . . ?
C15 C14 C13 113.4(4) . . ?
C15 C14 H14A 108.9 . . ?
C15 C14 H14B 108.9 . . ?
H14A C14 H14B 107.7 . . ?
O6 C53 H53 119.0 . . ?
C36 C53 O6 122.0(5) . . ?
C36 C53 H53 119.0 . . ?
C40 C32 C31 111.5(4) . . ?
C40 C32 H32 106.2 . . ?
C31 C32 H32 106.2 . . ?
C33 C32 C40 113.4(4) . . ?
C33 C32 C31 112.8(4) . . ?
C33 C32 H32 106.2 . . ?
H11A C11 H11B 109.2 . . ?
C12 C11 H11A 111.2 . . ?
C12 C11 H11B 111.2 . . ?
C12 C11 C10 102.6(5) . . ?
C10 C11 H11A 111.2 . . ?
C10 C11 H11B 111.2 . . ?
C28 C44 H44A 109.0 . . ?
C28 C44 H44B 109.0 . . ?
C43 C44 C28 113.0(4) . . ?
C43 C44 H44A 109.0 . . ?
C43 C44 H44B 109.0 . . ?
H44A C44 H44B 107.8 . . ?
C15 C16 C4 122.7(4) . . ?
C15 C16 C17 120.7(4) . . ?
C17 C16 C4 116.6(4) . . ?
C49 C47 Si2 110.8(4) . . ?
C49 C47 C48 109.3(5) . . ?
C50 C47 Si2 110.1(4) . . ?
C50 C47 C49 108.8(5) . . ?
C50 C47 C48 108.9(5) . . ?
C48 C47 Si2 109.0(4) . . ?
C4 C3 H3A 108.5 . . ?
C4 C3 H3B 108.5 . . ?
C2 C3 C4 115.1(4) . . ?
C2 C3 H3A 108.5 . . ?
C2 C3 H3B 108.5 . . ?
H3A C3 H3B 107.5 . . ?
C31 C51 H51A 109.5 . . ?
C31 C51 H51B 109.5 . . ?
C31 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C53 C36 C35 127.2(5) . . ?
C53 C36 C37 124.0(5) . . ?
C35 C36 C37 108.5(4) . . ?
C13 C12 C8 113.6(4) . . ?
C13 C12 C11 123.6(5) . . ?
C13 C12 H12 104.9 . . ?
C8 C12 H12 104.9 . . ?
C11 C12 C8 103.3(4) . . ?
C11 C12 H12 104.9 . . ?
C8 C9 C10 108.8(5) . . ?
C26 C9 C8 125.5(6) . . ?
C26 C9 C10 125.1(6) . . ?
C34 C35 C39 103.8(4) . . ?
C34 C35 C52 109.5(4) . . ?
C36 C35 C39 103.3(4) . . ?
C36 C35 C34 119.0(4) . . ?
C36 C35 C52 108.1(4) . . ?
C52 C35 C39 113.2(4) . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
C43 C42 H42 117.0 . . ?
C43 C42 C41 126.0(5) . . ?
C41 C42 H42 117.0 . . ?
C47 C50 H50A 109.5 . . ?
C47 C50 H50B 109.5 . . ?
C47 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C38 C37 C36 104.6(5) . . ?
C38 C37 H37A 110.8 . . ?
C38 C37 H37B 110.8 . . ?
C36 C37 H37A 110.8 . . ?
C36 C37 H37B 110.8 . . ?
H37A C37 H37B 108.9 . . ?
C35 C52 H52A 109.5 . . ?
C35 C52 H52B 109.5 . . ?
C35 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C11 C10 H10A 110.9 . . ?
C11 C10 H10B 110.9 . . ?
C9 C10 C11 104.5(5) . . ?
C9 C10 H10A 110.9 . . ?
C9 C10 H10B 110.9 . . ?
H10A C10 H10B 108.9 . . ?
C40 C41 H41A 109.0 . . ?
C40 C41 H41B 109.0 . . ?
C42 C41 C40 112.8(5) . . ?
C42 C41 H41A 109.0 . . ?
C42 C41 H41B 109.0 . . ?
H41A C41 H41B 107.8 . . ?
Si2 C46 H46A 109.5 . . ?
Si2 C46 H46B 109.5 . . ?
Si2 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C21 C20 Si1 110.0(4) . . ?
C21 C20 C23 109.2(5) . . ?
C21 C20 C22 109.4(5) . . ?
C23 C20 Si1 109.1(4) . . ?
C22 C20 Si1 110.4(4) . . ?
C22 C20 C23 108.8(5) . . ?
Si1 C19 H19A 109.5 . . ?
Si1 C19 H19B 109.5 . . ?
Si1 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C8 C25 H25A 109.5 . . ?
C8 C25 H25B 109.5 . . ?
C8 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si2 C45 H45A 109.5 . . ?
Si2 C45 H45B 109.5 . . ?
Si2 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
O3 C26 H26 119.6 . . ?
C9 C26 O3 120.9(6) . . ?
C9 C26 H26 119.6 . . ?
Si1 C18 H18A 109.5 . . ?
Si1 C18 H18B 109.5 . . ?
Si1 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O6 C54 H54A 109.5 . . ?
O6 C54 H54B 109.5 . . ?
O6 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O3 C27 H27A 109.5 . . ?
O3 C27 H27B 109.5 . . ?
O3 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 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
Si2 O4 1.648(4) . ?
Si2 C47 1.889(6) . ?
Si2 C46 1.867(6) . ?
Si2 C45 1.874(6) . ?
Si1 O1 1.642(4) . ?
Si1 C20 1.875(6) . ?
Si1 C19 1.875(7) . ?
Si1 C18 1.881(6) . ?
O1 C1 1.420(6) . ?
O4 C28 1.424(6) . ?
O6 C53 1.380(8) . ?
O6 C54 1.413(7) . ?
O2 C7 1.206(7) . ?
O5 C34 1.209(6) . ?
C5 H5 1.0000 . ?
C5 C4 1.551(7) . ?
C5 C13 1.541(7) . ?
C5 C6 1.545(7) . ?
C1 H1 1.0000 . ?
C1 C2 1.522(7) . ?
C1 C17 1.528(7) . ?
C4 C24 1.551(7) . ?
C4 C16 1.527(6) . ?
C4 C3 1.548(7) . ?
C13 H13 1.0000 . ?
C13 C14 1.521(7) . ?
C13 C12 1.509(7) . ?
C7 C6 1.525(7) . ?
C7 C8 1.530(8) . ?
C39 H39 1.0000 . ?
C39 C40 1.513(7) . ?
C39 C38 1.529(7) . ?
C39 C35 1.551(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.523(7) . ?
C34 C33 1.521(7) . ?
C34 C35 1.514(7) . ?
C40 H40 1.0000 . ?
C40 C32 1.548(6) . ?
C40 C41 1.524(7) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C28 H28 1.0000 . ?
C28 C29 1.520(7) . ?
C28 C44 1.529(7) . ?
C15 H15 0.9500 . ?
C15 C14 1.484(7) . ?
C15 C16 1.343(7) . ?
C31 C30 1.557(6) . ?
C31 C43 1.527(6) . ?
C31 C32 1.554(6) . ?
C31 C51 1.534(7) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C16 1.505(7) . ?
O3 C26 1.387(9) . ?
O3 C27 1.365(9) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.524(7) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C32 1.548(7) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C37 1.530(9) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C43 C44 1.500(7) . ?
C43 C42 1.339(8) . ?
C8 C12 1.557(7) . ?
C8 C9 1.511(7) . ?
C8 C25 1.545(8) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C53 H53 0.9500 . ?
C53 C36 1.333(8) . ?
C32 H32 1.0000 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.515(7) . ?
C11 C10 1.529(9) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C47 C49 1.537(8) . ?
C47 C50 1.532(8) . ?
C47 C48 1.542(9) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C36 C35 1.509(7) . ?
C36 C37 1.530(9) . ?
C12 H12 1.0000 . ?
C9 C10 1.518(9) . ?
C9 C26 1.314(9) . ?
C35 C52 1.538(7) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C21 C20 1.537(9) . ?
C42 H42 0.9500 . ?
C42 C41 1.476(8) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C20 C23 1.548(9) . ?
C20 C22 1.544(8) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C26 H26 0.9500 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 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
Si2 O4 C28 C29 162.0(4) . . . . ?
Si2 O4 C28 C44 -78.1(5) . . . . ?
Si1 O1 C1 C2 145.4(4) . . . . ?
Si1 O1 C1 C17 -94.1(4) . . . . ?
O1 Si1 C20 C21 52.6(5) . . . . ?
O1 Si1 C20 C23 -67.1(5) . . . . ?
O1 Si1 C20 C22 173.4(5) . . . . ?
O1 C1 C2 C3 178.3(4) . . . . ?
O1 C1 C17 C16 -176.1(4) . . . . ?
O4 Si2 C47 C49 177.7(4) . . . . ?
O4 Si2 C47 C50 57.3(5) . . . . ?
O4 Si2 C47 C48 -62.0(4) . . . . ?
O4 C28 C29 C30 179.5(4) . . . . ?
O4 C28 C44 C43 -174.6(4) . . . . ?
O6 C53 C36 C35 2.6(9) . . . . ?
O6 C53 C36 C37 -170.1(6) . . . . ?
O2 C7 C6 C5 124.9(6) . . . . ?
O2 C7 C8 C12 -115.9(6) . . . . ?
O2 C7 C8 C9 -3.2(8) . . . . ?
O2 C7 C8 C25 123.6(6) . . . . ?
O5 C34 C33 C32 133.6(6) . . . . ?
O5 C34 C35 C39 -123.5(7) . . . . ?
O5 C34 C35 C36 -9.5(9) . . . . ?
O5 C34 C35 C52 115.3(7) . . . . ?
C5 C4 C16 C15 12.3(6) . . . . ?
C5 C4 C16 C17 -165.3(4) . . . . ?
C5 C4 C3 C2 169.3(4) . . . . ?
C5 C13 C14 C15 -42.1(6) . . . . ?
C5 C13 C12 C8 60.5(5) . . . . ?
C5 C13 C12 C11 -173.3(4) . . . . ?
C1 C2 C3 C4 -57.2(6) . . . . ?
C1 C17 C16 C4 51.6(6) . . . . ?
C1 C17 C16 C15 -126.1(5) . . . . ?
C4 C5 C13 C14 59.3(5) . . . . ?
C4 C5 C13 C12 -176.8(4) . . . . ?
C4 C5 C6 C7 172.8(5) . . . . ?
C13 C5 C4 C24 77.0(5) . . . . ?
C13 C5 C4 C16 -43.4(5) . . . . ?
C13 C5 C4 C3 -162.0(4) . . . . ?
C13 C5 C6 C7 41.5(7) . . . . ?
C7 C8 C12 C13 -66.3(5) . . . . ?
C7 C8 C12 C11 157.3(4) . . . . ?
C7 C8 C9 C10 -126.5(5) . . . . ?
C7 C8 C9 C26 61.9(8) . . . . ?
C39 C40 C32 C31 -173.8(4) . . . . ?
C39 C40 C32 C33 -45.2(6) . . . . ?
C39 C40 C41 C42 -164.3(5) . . . . ?
C39 C38 C37 C36 33.5(6) . . . . ?
C2 C1 C17 C16 -54.9(5) . . . . ?
C34 C33 C32 C40 38.7(7) . . . . ?
C34 C33 C32 C31 166.7(4) . . . . ?
C40 C39 C38 C37 -170.9(5) . . . . ?
C40 C39 C35 C34 -66.9(5) . . . . ?
C40 C39 C35 C36 168.4(4) . . . . ?
C40 C39 C35 C52 51.8(6) . . . . ?
C6 C5 C4 C24 -54.9(6) . . . . ?
C6 C5 C4 C16 -175.2(4) . . . . ?
C6 C5 C4 C3 66.1(5) . . . . ?
C6 C5 C13 C14 -169.3(4) . . . . ?
C6 C5 C13 C12 -45.4(5) . . . . ?
C6 C7 C8 C12 58.8(5) . . . . ?
C6 C7 C8 C9 171.5(5) . . . . ?
C6 C7 C8 C25 -61.7(6) . . . . ?
C28 C29 C30 C31 -59.4(6) . . . . ?
C31 C43 C44 C28 51.9(6) . . . . ?
C31 C43 C42 C41 4.2(10) . . . . ?
C17 C1 C2 C3 57.2(5) . . . . ?
C24 C4 C16 C15 -109.6(5) . . . . ?
C24 C4 C16 C17 72.8(5) . . . . ?
C24 C4 C3 C2 -68.9(5) . . . . ?
C29 C28 C44 C43 -54.3(6) . . . . ?
C33 C34 C35 C39 56.8(6) . . . . ?
C33 C34 C35 C36 170.8(5) . . . . ?
C33 C34 C35 C52 -64.3(6) . . . . ?
C38 C39 C40 C32 -174.3(5) . . . . ?
C38 C39 C40 C41 -53.7(7) . . . . ?
C38 C39 C35 C34 160.4(5) . . . . ?
C38 C39 C35 C36 35.6(5) . . . . ?
C38 C39 C35 C52 -81.0(5) . . . . ?
C30 C31 C43 C44 -47.9(6) . . . . ?
C30 C31 C43 C42 132.4(6) . . . . ?
C30 C31 C32 C40 -164.9(4) . . . . ?
C30 C31 C32 C33 66.2(5) . . . . ?
C43 C31 C30 C29 51.2(6) . . . . ?
C43 C31 C32 C40 -47.4(5) . . . . ?
C43 C31 C32 C33 -176.3(4) . . . . ?
C43 C42 C41 C40 11.4(10) . . . . ?
C8 C7 C6 C5 -50.0(6) . . . . ?
C8 C9 C10 C11 -12.6(6) . . . . ?
C8 C9 C26 O3 0.4(12) . . . . ?
C14 C13 C12 C8 -177.1(4) . . . . ?
C14 C13 C12 C11 -50.9(6) . . . . ?
C14 C15 C16 C4 3.4(8) . . . . ?
C14 C15 C16 C17 -179.1(5) . . . . ?
C53 C36 C35 C39 171.6(5) . . . . ?
C53 C36 C35 C34 57.3(8) . . . . ?
C53 C36 C35 C52 -68.2(7) . . . . ?
C53 C36 C37 C38 162.4(6) . . . . ?
C32 C40 C41 C42 -43.4(7) . . . . ?
C32 C31 C30 C29 170.2(4) . . . . ?
C32 C31 C43 C44 -166.2(4) . . . . ?
C32 C31 C43 C42 14.1(7) . . . . ?
C44 C28 C29 C30 58.1(6) . . . . ?
C44 C43 C42 C41 -175.5(6) . . . . ?
C16 C4 C3 C2 49.2(5) . . . . ?
C16 C15 C14 C13 12.2(7) . . . . ?
C47 Si2 O4 C28 -161.9(4) . . . . ?
C3 C4 C16 C15 131.4(5) . . . . ?
C3 C4 C16 C17 -46.2(5) . . . . ?
C51 C31 C30 C29 -67.1(5) . . . . ?
C51 C31 C43 C44 71.1(5) . . . . ?
C51 C31 C43 C42 -108.6(6) . . . . ?
C51 C31 C32 C40 73.5(5) . . . . ?
C51 C31 C32 C33 -55.4(6) . . . . ?
C12 C13 C14 C15 -164.0(4) . . . . ?
C12 C8 C9 C10 -13.4(6) . . . . ?
C12 C8 C9 C26 175.0(7) . . . . ?
C12 C11 C10 C9 34.1(6) . . . . ?
C9 C8 C12 C13 170.9(4) . . . . ?
C9 C8 C12 C11 34.6(5) . . . . ?
C35 C39 C40 C32 62.3(5) . . . . ?
C35 C39 C40 C41 -177.0(5) . . . . ?
C35 C39 C38 C37 -42.9(5) . . . . ?
C35 C34 C33 C32 -46.7(7) . . . . ?
C35 C36 C37 C38 -11.5(6) . . . . ?
C42 C43 C44 C28 -128.4(6) . . . . ?
C37 C36 C35 C39 -14.8(5) . . . . ?
C37 C36 C35 C34 -129.0(5) . . . . ?
C37 C36 C35 C52 105.4(5) . . . . ?
C10 C11 C12 C13 -173.2(4) . . . . ?
C10 C11 C12 C8 -42.7(5) . . . . ?
C10 C9 C26 O3 -169.9(7) . . . . ?
C41 C40 C32 C31 63.1(6) . . . . ?
C41 C40 C32 C33 -168.3(5) . . . . ?
C46 Si2 O4 C28 -41.0(5) . . . . ?
C46 Si2 C47 C49 57.6(5) . . . . ?
C46 Si2 C47 C50 -62.7(5) . . . . ?
C46 Si2 C47 C48 177.9(4) . . . . ?
C20 Si1 O1 C1 149.5(4) . . . . ?
C19 Si1 O1 C1 -92.0(5) . . . . ?
C19 Si1 C20 C21 -65.3(5) . . . . ?
C19 Si1 C20 C23 175.0(4) . . . . ?
C19 Si1 C20 C22 55.5(6) . . . . ?
C25 C8 C12 C13 54.0(6) . . . . ?
C25 C8 C12 C11 -82.3(5) . . . . ?
C25 C8 C9 C10 105.5(6) . . . . ?
C25 C8 C9 C26 -66.1(8) . . . . ?
C45 Si2 O4 C28 79.1(5) . . . . ?
C45 Si2 C47 C49 -61.3(5) . . . . ?
C45 Si2 C47 C50 178.3(4) . . . . ?
C45 Si2 C47 C48 59.0(5) . . . . ?
C26 C9 C10 C11 159.1(7) . . . . ?
C18 Si1 O1 C1 29.6(5) . . . . ?
C18 Si1 C20 C21 173.1(4) . . . . ?
C18 Si1 C20 C23 53.4(5) . . . . ?
C18 Si1 C20 C22 -66.1(6) . . . . ?
C54 O6 C53 C36 -165.7(6) . . . . ?
C27 O3 C26 C9 -162.5(8) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-2.1863 6.9087 -3.1521 -0.0246 -0.0474 0.9986
-3.1730 -2.8310 -3.0676 -0.4307 -0.9022 -0.0233
1.9262 -7.1332 2.8997 -0.0104 -0.0261 -0.9996
3.1583 2.8798 3.0461 0.4306 0.9021 0.0302
0.4757 0.2134 -11.6452 -0.9483 0.2284 0.2203
-0.9606 1.4406 11.2412 0.9723 -0.2337 0.0090
