#------------------------------------------------------------------------------
#$Date: 2021-07-05 19:53:37 +0300 (Mon, 05 Jul 2021) $
#$Revision: 267083 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/98/1559815.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_1559815
loop_
_publ_author_name
'Huang, Qi'
'Suravarapu, Sankar Rao'
'Renaud, Philippe'
_publ_section_title
;
 A Giese reaction for electron-rich alkenes.
;
_journal_issue                   6
_journal_name_full               'Chemical science'
_journal_page_first              2225
_journal_page_last               2230
_journal_paper_doi               10.1039/d0sc06341j
_journal_volume                  12
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C29 H46 O4 Si'
_chemical_formula_sum            'C29 H46 O4 Si'
_chemical_formula_weight         486.75
_chemical_name_systematic
'Ethyl 2-((8R,9S,13S,14S,16S,17S)-17-((tert-butyldimethylsilyl)oxy)-3-methoxy- 13-methyl-7,8,9,11,12,13,14,15,16,17-decahydro-6H-cyclopenta[a]phenanthren-16-yl)acetate'
_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             2020-08-07
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2020-09-10 deposited with the CCDC.	2020-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                101.7853(5)
_cell_angle_beta                 91.4615(5)
_cell_angle_gamma                98.5773(5)
_cell_formula_units_Z            2
_cell_length_a                   6.44725(4)
_cell_length_b                   10.18619(6)
_cell_length_c                   22.76512(12)
_cell_measurement_reflns_used    24477
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      78.7530
_cell_measurement_theta_min      3.9610
_cell_volume                     1444.746(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (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_environment      N~2~
_diffrn_ambient_temperature      173.00(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 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -56.00   8.00   0.50    1.00    --  -21.00 103.00 -66.00  128
  2  ω     42.00 107.00   0.50    5.00    --  113.25-103.00-168.00  130
  3  ω    106.00 171.00   0.50    5.00    --  113.25 103.00 -66.00  130
  4  ω    -68.00 -12.00   0.50    1.00    --  -21.00 125.00 -30.00  112
  5  ω    -68.00 -12.00   0.50    1.00    --  -21.00 125.00 -90.00  112
  6  ω    -93.00  -5.00   0.50    1.00    --  -21.00 -57.00-180.00  176
  7  ω    -26.00  23.00   0.50    1.00    --   47.89 -19.00 -90.00   98
  8  ω     33.00 121.00   0.50    1.00    --   47.89  57.00  30.00  176
  9  ω    -26.00  23.00   0.50    1.00    --   47.89 -19.00-180.00   98
 10  ω    -26.00  23.00   0.50    1.00    --   47.89 -19.00-120.00   98
 11  ω    -26.00  23.00   0.50    1.00    --   47.89 -19.00  60.00   98
 12  ω     15.00  84.00   0.50    1.00    --   47.89-103.00-168.00  138
 13  ω    101.00 171.00   0.50    5.00    --  113.25  30.00 120.00  140
 14  ω     42.00 102.00   0.50    5.00    --  113.25 -77.00 120.00  120
 15  ω     42.00  68.00   0.50    5.00    --  113.25 -61.00-150.00   52
 16  ω     42.00 106.00   0.50    5.00    --  113.25 -94.00 -30.00  128
 17  ω     91.00 171.00   0.50    5.00    --  113.25  77.00 -30.00  160
 18  ω     91.00 171.00   0.50    5.00    --  113.25  77.00-150.00  160
 19  ω     42.00 106.00   0.50    5.00    --  113.25 -94.00-180.00  128
 20  ω     42.00  68.00   0.50    5.00    --  113.25 -61.00 120.00   52
 21  ω     42.00  68.00   0.50    5.00    --  113.25 -61.00   0.00   52
 22  ω     42.00 106.00   0.50    5.00    --  113.25 -94.00  90.00  128
 23  ω     42.00  68.00   0.50    5.00    --  113.25 -61.00 -30.00   52
 24  ω     42.00 112.00   0.50    5.00    --  113.25-125.00  90.00  140
 25  ω    100.00 171.00   0.50    5.00    --  113.25  15.00-120.00  142
 26  ω     42.00 106.00   0.50    5.00    --  113.25 -94.00-150.00  128
 27  ω     97.00 171.00   0.50    5.00    --  113.25  61.00 150.00  148
 28  ω    100.00 171.00   0.50    5.00    --  113.25  15.00 -60.00  142
 29  ω     42.00 106.00   0.50    5.00    --  113.25 -94.00 -90.00  128
 30  ω    101.00 171.00   0.50    5.00    --  113.25  30.00 -90.00  140
 31  ω    101.00 171.00   0.50    5.00    --  113.25  45.00  30.00  140
 32  ω     42.00 112.00   0.50    5.00    --  113.25-125.00-180.00  140
 33  ω     42.00  68.00   0.50    5.00    --  113.25 -61.00  90.00   52
 34  ω     42.00 112.00   0.50    5.00    --  113.25-125.00  60.00  140
 35  ω     95.00 171.00   0.50    5.00    --  113.25 125.00 -30.00  152
 36  ω    101.00 171.00   0.50    5.00    --  113.25  30.00   0.00  140
 37  ω     42.00 112.00   0.50    5.00    --  113.25-125.00 120.00  140
 38  ω     97.00 171.00   0.50    5.00    --  113.25  61.00  90.00  148
 39  ω     42.00 106.00   0.50    5.00    --  113.25 -94.00 -60.00  128
 40  ω     42.00  68.00   0.50    5.00    --  113.25 -61.00-120.00   52
 41  ω     42.00 102.00   0.50    5.00    --  113.25 -77.00 -30.00  120
 42  ω     42.00  68.00   0.50    5.00    --  113.25 -61.00 -90.00   52
 43  ω    -68.00 -12.00   0.50    1.00    --  -21.00 125.00 150.00  112
 44  ω     26.00 121.00   0.50    1.00    --   47.89  77.00  90.00  190
 45  ω     33.00 121.00   0.50    1.00    --   47.89  57.00 -90.00  176
 46  ω     26.00 121.00   0.50    1.00    --   47.89  77.00-180.00  190
 47  ω     26.00 121.00   0.50    1.00    --   47.89  77.00  30.00  190
 48  ω     26.00 121.00   0.50    1.00    --   47.89  77.00 120.00  190
 49  ω     26.00 110.00   0.50    1.00    --   47.89  77.00-120.00  168
 50  ω     26.00 121.00   0.50    1.00    --   47.89  77.00 -60.00  190
;
_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      -0.1729792000
_diffrn_orient_matrix_UB_12      0.0563513000
_diffrn_orient_matrix_UB_13      -0.0306044000
_diffrn_orient_matrix_UB_21      0.1145732000
_diffrn_orient_matrix_UB_22      -0.0200911000
_diffrn_orient_matrix_UB_23      -0.0589725000
_diffrn_orient_matrix_UB_31      -0.1246691000
_diffrn_orient_matrix_UB_32      -0.1445656000
_diffrn_orient_matrix_UB_33      -0.0195065000
_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  0.0301
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            29329
_diffrn_reflns_point_group_measured_fraction_full 0.858
_diffrn_reflns_point_group_measured_fraction_max 0.840
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.501
_diffrn_reflns_theta_min         3.974
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.945
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.590
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.61a (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 whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_description       needle
_exptl_crystal_F_000             532
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Diethylether'
_exptl_crystal_size_max          0.251
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 3694 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         9878
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0501
_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)+(0.1029P)²+0.3937P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1512
_reflns_Friedel_coverage         0.683
_reflns_Friedel_fraction_full    0.717
_reflns_Friedel_fraction_max     0.682
_reflns_number_gt                9500
_reflns_number_total             9878
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc06341j2.cif
_cod_data_source_block           20pr012_absorption
_cod_depositor_comments
;Adding full bibliography for 1559814--1559816.cif.

 Adding full bibliography for 1559814--1559816.cif.
;
_cod_database_code               1559815
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         C29H46O4Si
_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.
;
_diffrn_oxdiff_digest_frames
;
013244d805f3bce19929e5bf7ae48919fa0644402f9
;
_diffrn_oxdiff_digest_hkl
;
01242369a0dbfcfe40deb7ff6df98c50373c03
;
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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:
 C17B(H17C), C10B(H10C), C11B(H11C), C9B(H9B), C8A(H8A), C15A(H15A),
 C16B(H16B), C7A(H7A), C16A(H16A), C14A(H14A)
2.b Secondary CH2 refined with riding coordinates:
 C15B(H15B,H15C), C11A(H11A,H11B), C12A(H12A,H12B), C14B(H14B,H14C), C8B(H8BA,
 H8BB), C13B(H13A,H13B), C7B(H7BA,H7BB), C9A(H9AA,H9AB), C20B(H20C,H20D),
 C10A(H10A,H10B), C17A(H17A,H17B), C22B(H22C,H22D), C20A(H20A,H20B), C22A(H22A,
 H22B)
2.c Aromatic/amide H refined with riding coordinates:
 C6A(H6A), C2B(H2B), C6B(H6B), C5B(H5B), C2A(H2A), C3A(H3A)
2.d Idealised Me refined as rotating group:
 C18B(H18D,H18E,H18F), C19B(H19D,H19E,H19F), C18A(H18A,H18B,H18C), C19A(H19A,
 H19B,H19C), C24B(H24D,H24E,H24F), C27A(H27A,H27B,H27C), C28A(H28A,H28B,H28C),
 C24A(H24A,H24B,H24C), C29A(H29A,H29B,H29C), C28B(H28D,H28E,H28F), C25A(H25A,
 H25B,H25C), C25B(H25D,H25E,H25F), C29B(H29D,H29E,H29F), C27B(H27D,H27E,H27F),
 C23B(H23D,H23E,H23F), C23A(H23A,H23B,H23C)
;
_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 2.245
_oxdiff_exptl_absorpt_empirical_full_min 0.718
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
Si1A Si 0.06463(15) 0.28762(10) 0.80054(5) 0.0401(2) Uani 1 1 d . . . . .
Si52 Si 0.60393(14) 0.38814(12) 0.09700(4) 0.0421(3) Uani 1 1 d . . . . .
O65 O 0.9961(4) 0.1472(3) 0.58220(11) 0.0358(5) Uani 1 1 d . . . . .
O51 O 0.4763(4) 0.3776(3) 0.15773(11) 0.0375(5) Uani 1 1 d . . . . .
O4A O 0.2707(4) 0.3725(3) 0.77564(12) 0.0399(6) Uani 1 1 d . . . . .
O61 O 0.1868(5) 0.8527(3) 0.24515(15) 0.0496(7) Uani 1 1 d . . . . .
O1A O 0.3324(5) 0.8677(3) 0.38850(12) 0.0475(7) Uani 1 1 d . . . . .
O64 O 0.0028(4) 0.6658(3) 0.26697(15) 0.0464(7) Uani 1 1 d . . . . .
C17B C 0.5273(5) 0.4484(4) 0.21845(14) 0.0307(7) Uani 1 1 d . . . . .
H17C H 0.651449 0.517660 0.219707 0.037 Uiso 1 1 calc R . . . .
C10B C 0.8027(5) 0.3468(3) 0.37419(14) 0.0277(6) Uani 1 1 d . . . . .
H10C H 0.905251 0.429537 0.377090 0.033 Uiso 1 1 calc R . . . .
C13A C 0.3099(5) 0.5172(3) 0.69907(15) 0.0313(7) Uani 1 1 d . . . . .
C15B C 0.3555(5) 0.5142(4) 0.31291(14) 0.0317(7) Uani 1 1 d . . . . .
H15B H 0.364903 0.604782 0.337571 0.038 Uiso 1 1 calc R . . . .
H15C H 0.233059 0.457257 0.323137 0.038 Uiso 1 1 calc R . . . .
C1B C 0.9540(5) 0.1870(3) 0.52976(15) 0.0304(6) Uani 1 1 d . . . . .
C12B C 0.5689(5) 0.3559(3) 0.26139(14) 0.0284(6) Uani 1 1 d . . . . .
C11B C 0.5554(5) 0.4544(3) 0.32175(14) 0.0277(6) Uani 1 1 d . . . . .
H11C H 0.673230 0.528801 0.324642 0.033 Uiso 1 1 calc R . . . .
C4A C 0.2842(5) 0.7315(3) 0.54988(15) 0.0308(6) Uani 1 1 d . . . . .
C6A C 0.4852(6) 0.8640(4) 0.48730(17) 0.0370(7) Uani 1 1 d . . . . .
H6A H 0.606300 0.921381 0.481864 0.044 Uiso 1 1 calc R . . . .
C21B C 0.1603(6) 0.7234(4) 0.25085(16) 0.0348(7) Uani 1 1 d . . . . .
C9B C 0.5839(5) 0.3908(3) 0.37593(14) 0.0271(6) Uani 1 1 d . . . . .
H9B H 0.477143 0.309840 0.372164 0.032 Uiso 1 1 calc R . . . .
C11A C 0.1228(5) 0.5475(4) 0.60402(16) 0.0353(7) Uani 1 1 d . . . . .
H11A H 0.188067 0.482198 0.576373 0.042 Uiso 1 1 calc R . . . .
H11B H -0.016033 0.548018 0.586733 0.042 Uiso 1 1 calc R . . . .
C2B C 0.7963(5) 0.2676(3) 0.53114(14) 0.0298(6) Uani 1 1 d . . . . .
H2B H 0.723637 0.286889 0.565834 0.036 Uiso 1 1 calc R . . . .
C3B C 0.7458(5) 0.3198(3) 0.48154(15) 0.0285(6) Uani 1 1 d . . . . .
C5A C 0.4662(5) 0.8180(4) 0.54130(17) 0.0351(7) Uani 1 1 d . . . . .
C8A C 0.4617(5) 0.7039(3) 0.64637(15) 0.0318(7) Uani 1 1 d . . . . .
H8A H 0.546089 0.639212 0.624753 0.038 Uiso 1 1 calc R . . . .
C12A C 0.0993(5) 0.4999(4) 0.66393(16) 0.0340(7) Uani 1 1 d . . . . .
H12A H 0.005696 0.551583 0.688267 0.041 Uiso 1 1 calc R . . . .
H12B H 0.036051 0.404926 0.655801 0.041 Uiso 1 1 calc R . . . .
C4B C 0.8502(5) 0.2880(3) 0.42877(14) 0.0286(6) Uani 1 1 d . . . . .
O2A O 0.9027(7) 0.7004(5) 0.8615(2) 0.0775(11) Uani 1 1 d . . . . .
C14B C 0.8327(5) 0.2527(3) 0.31411(14) 0.0304(7) Uani 1 1 d . . . . .
H14B H 0.976319 0.234828 0.313602 0.036 Uiso 1 1 calc R . . . .
H14C H 0.740611 0.166743 0.310877 0.036 Uiso 1 1 calc R . . . .
C1A C 0.3277(6) 0.8258(4) 0.44216(16) 0.0357(7) Uani 1 1 d . . . . .
C6B C 1.0564(5) 0.1534(4) 0.47737(16) 0.0355(7) Uani 1 1 d . . . . .
H6B H 1.158666 0.097392 0.475331 0.043 Uiso 1 1 calc R . . . .
C15A C 0.3019(6) 0.5071(4) 0.76565(16) 0.0389(8) Uani 1 1 d . . . . .
H15A H 0.191423 0.555289 0.784134 0.047 Uiso 1 1 calc R . . . .
C8B C 0.5657(5) 0.4851(4) 0.43572(15) 0.0317(7) Uani 1 1 d . . . . .
H8BA H 0.433269 0.519383 0.435537 0.038 Uiso 1 1 calc R . . . .
H8BB H 0.678486 0.561877 0.441695 0.038 Uiso 1 1 calc R . . . .
C16B C 0.3433(5) 0.5178(4) 0.24521(14) 0.0307(7) Uani 1 1 d . . . . .
H16B H 0.210897 0.463020 0.226739 0.037 Uiso 1 1 calc R . . . .
C18B C 0.3968(5) 0.2308(4) 0.25008(15) 0.0328(7) Uani 1 1 d . . . . .
H18D H 0.261457 0.259210 0.249648 0.049 Uiso 1 1 calc GR . . . .
H18E H 0.407337 0.181505 0.281475 0.049 Uiso 1 1 calc GR . . . .
H18F H 0.413904 0.173326 0.212046 0.049 Uiso 1 1 calc GR . . . .
C13B C 0.7859(5) 0.3132(4) 0.25964(14) 0.0293(6) Uani 1 1 d . . . . .
H13A H 0.891503 0.391526 0.259288 0.035 Uiso 1 1 calc R . . . .
H13B H 0.793266 0.246446 0.222988 0.035 Uiso 1 1 calc R . . . .
C5B C 1.0037(5) 0.2048(4) 0.42772(16) 0.0352(7) Uani 1 1 d . . . . .
H5B H 1.073384 0.182816 0.392649 0.042 Uiso 1 1 calc R . . . .
C2A C 0.1479(6) 0.7390(4) 0.45010(16) 0.0370(7) Uani 1 1 d . . . . .
H2A H 0.041160 0.711863 0.419883 0.044 Uiso 1 1 calc R . . . .
C3A C 0.1282(6) 0.6928(4) 0.50324(16) 0.0341(7) Uani 1 1 d . . . . .
H3A H 0.007398 0.634254 0.507964 0.041 Uiso 1 1 calc R . . . .
C7B C 0.5775(5) 0.4104(4) 0.48706(15) 0.0323(7) Uani 1 1 d . . . . .
H7BA H 0.604401 0.476791 0.524658 0.039 Uiso 1 1 calc R . . . .
H7BB H 0.442201 0.355315 0.488653 0.039 Uiso 1 1 calc R . . . .
C9A C 0.5812(6) 0.8464(4) 0.65088(17) 0.0394(8) Uani 1 1 d . . . . .
H9AA H 0.706206 0.860011 0.677423 0.047 Uiso 1 1 calc R . . . .
H9AB H 0.493724 0.912833 0.667570 0.047 Uiso 1 1 calc R . . . .
C7A C 0.2521(5) 0.6876(4) 0.60963(15) 0.0327(7) Uani 1 1 d . . . . .
H7A H 0.170405 0.751686 0.632919 0.039 Uiso 1 1 calc R . . . .
C26A C 0.1526(7) 0.1270(4) 0.81293(18) 0.0430(8) Uani 1 1 d . . . . .
C16A C 0.5200(7) 0.5832(4) 0.79390(19) 0.0468(9) Uani 1 1 d . . . . .
H16A H 0.616900 0.516706 0.789490 0.056 Uiso 1 1 calc R . . . .
C14A C 0.4142(6) 0.6661(4) 0.70639(15) 0.0342(7) Uani 1 1 d . . . . .
H14A H 0.311409 0.722037 0.724216 0.041 Uiso 1 1 calc R . . . .
C19B C 1.1581(7) 0.0662(4) 0.58145(18) 0.0422(8) Uani 1 1 d . . . . .
H19D H 1.120355 -0.016463 0.551813 0.063 Uiso 1 1 calc GR . . . .
H19E H 1.175982 0.045107 0.620298 0.063 Uiso 1 1 calc GR . . . .
H19F H 1.287092 0.115252 0.571713 0.063 Uiso 1 1 calc GR . . . .
C20B C 0.3542(6) 0.6606(4) 0.23334(18) 0.0375(7) Uani 1 1 d . . . . .
H20C H 0.476200 0.718181 0.255662 0.045 Uiso 1 1 calc R . . . .
H20D H 0.372680 0.657160 0.190922 0.045 Uiso 1 1 calc R . . . .
C21A C 0.7460(9) 0.7089(5) 0.8890(2) 0.0554(11) Uani 1 1 d . . . . .
C10A C 0.6432(6) 0.8655(4) 0.58871(18) 0.0401(8) Uani 1 1 d . . . . .
H10A H 0.693501 0.960966 0.590714 0.048 Uiso 1 1 calc R . . . .
H10B H 0.758133 0.815972 0.577021 0.048 Uiso 1 1 calc R . . . .
C18A C 0.4445(6) 0.4159(4) 0.66648(17) 0.0377(8) Uani 1 1 d . . . . .
H18A H 0.397027 0.327618 0.674341 0.057 Uiso 1 1 calc GR . . . .
H18B H 0.588814 0.444941 0.680683 0.057 Uiso 1 1 calc GR . . . .
H18C H 0.431729 0.411914 0.624014 0.057 Uiso 1 1 calc GR . . . .
C17A C 0.5940(7) 0.6854(4) 0.75433(18) 0.0443(9) Uani 1 1 d . . . . .
H17A H 0.617480 0.777566 0.777921 0.053 Uiso 1 1 calc R . . . .
H17B H 0.723110 0.665991 0.735909 0.053 Uiso 1 1 calc R . . . .
C19A C 0.5141(9) 0.9567(6) 0.3790(2) 0.0653(14) Uani 1 1 d . . . . .
H19A H 0.496179 0.982502 0.341196 0.098 Uiso 1 1 calc GR . . . .
H19B H 0.634540 0.911376 0.378731 0.098 Uiso 1 1 calc GR . . . .
H19C H 0.534453 1.036270 0.410811 0.098 Uiso 1 1 calc GR . . . .
C22B C 0.0088(8) 0.9233(5) 0.2581(3) 0.0596(12) Uani 1 1 d . . . . .
H22C H 0.058728 1.018796 0.274540 0.072 Uiso 1 1 calc R . . . .
H22D H -0.071909 0.886542 0.288112 0.072 Uiso 1 1 calc R . . . .
C26B C 0.5644(8) 0.2099(6) 0.0499(2) 0.0631(13) Uani 1 1 d . . . . .
O3A O 0.7375(10) 0.7716(7) 0.9424(2) 0.115(2) Uani 1 1 d . . . . .
C24B C 0.8899(7) 0.4545(7) 0.1152(2) 0.0645(14) Uani 1 1 d . . . . .
H24D H 0.905836 0.542154 0.141699 0.097 Uiso 1 1 calc GR . . . .
H24E H 0.958220 0.462291 0.078790 0.097 Uiso 1 1 calc GR . . . .
H24F H 0.952276 0.393091 0.134363 0.097 Uiso 1 1 calc GR . . . .
C27A C 0.2087(11) 0.0440(6) 0.7540(2) 0.0679(14) Uani 1 1 d . . . . .
H27A H 0.088322 0.021883 0.726044 0.102 Uiso 1 1 calc GR . . . .
H27B H 0.251749 -0.038134 0.760810 0.102 Uiso 1 1 calc GR . . . .
H27C H 0.321521 0.095715 0.737769 0.102 Uiso 1 1 calc GR . . . .
C28A C -0.0265(11) 0.0439(6) 0.8394(3) 0.0760(17) Uani 1 1 d . . . . .
H28A H -0.051428 0.092476 0.878658 0.114 Uiso 1 1 calc GR . . . .
H28B H 0.012076 -0.042181 0.842203 0.114 Uiso 1 1 calc GR . . . .
H28C H -0.151907 0.029368 0.813711 0.114 Uiso 1 1 calc GR . . . .
C20A C 0.5209(10) 0.6456(6) 0.8594(2) 0.0667(13) Uani 1 1 d . . . . .
H20A H 0.459584 0.576701 0.880360 0.080 Uiso 1 1 calc R . . . .
H20B H 0.432911 0.716054 0.864515 0.080 Uiso 1 1 calc R . . . .
C24A C -0.1615(7) 0.2418(7) 0.7427(3) 0.0713(16) Uani 1 1 d . . . . .
H24A H -0.226647 0.320334 0.742149 0.107 Uiso 1 1 calc GR . . . .
H24B H -0.262345 0.171424 0.752647 0.107 Uiso 1 1 calc GR . . . .
H24C H -0.111102 0.210101 0.703885 0.107 Uiso 1 1 calc GR . . . .
C29A C 0.3463(9) 0.1623(7) 0.8562(3) 0.0741(16) Uani 1 1 d . . . . .
H29A H 0.452740 0.221546 0.841338 0.111 Uiso 1 1 calc GR . . . .
H29B H 0.398768 0.080618 0.859624 0.111 Uiso 1 1 calc GR . . . .
H29C H 0.309605 0.207000 0.895017 0.111 Uiso 1 1 calc GR . . . .
C28B C 0.6841(9) 0.2070(8) -0.0076(2) 0.082(2) Uani 1 1 d . . . . .
H28D H 0.645844 0.274709 -0.027771 0.123 Uiso 1 1 calc GR . . . .
H28E H 0.648899 0.118967 -0.033667 0.123 Uiso 1 1 calc GR . . . .
H28F H 0.832524 0.225333 0.002538 0.123 Uiso 1 1 calc GR . . . .
C25A C -0.0149(12) 0.3879(6) 0.8720(3) 0.0797(19) Uani 1 1 d . . . . .
H25A H 0.098088 0.404254 0.902134 0.120 Uiso 1 1 calc GR . . . .
H25B H -0.136852 0.338062 0.885135 0.120 Uiso 1 1 calc GR . . . .
H25C H -0.046758 0.473050 0.865392 0.120 Uiso 1 1 calc GR . . . .
C25B C 0.4882(10) 0.5028(9) 0.0559(3) 0.083(2) Uani 1 1 d . . . . .
H25D H 0.342966 0.467142 0.044797 0.124 Uiso 1 1 calc GR . . . .
H25E H 0.562770 0.508895 0.020299 0.124 Uiso 1 1 calc GR . . . .
H25F H 0.499293 0.591537 0.081278 0.124 Uiso 1 1 calc GR . . . .
C29B C 0.6505(14) 0.1134(8) 0.0848(3) 0.090(2) Uani 1 1 d . . . . .
H29D H 0.796086 0.146297 0.096578 0.135 Uiso 1 1 calc GR . . . .
H29E H 0.636659 0.024296 0.059577 0.135 Uiso 1 1 calc GR . . . .
H29F H 0.572674 0.109380 0.119920 0.135 Uiso 1 1 calc GR . . . .
C27B C 0.3312(11) 0.1627(10) 0.0329(3) 0.100(3) Uani 1 1 d . . . . .
H27D H 0.255237 0.165402 0.068777 0.150 Uiso 1 1 calc GR . . . .
H27E H 0.310628 0.071459 0.009608 0.150 Uiso 1 1 calc GR . . . .
H27F H 0.280871 0.221472 0.009725 0.150 Uiso 1 1 calc GR . . . .
C23B C -0.1273(11) 0.9091(8) 0.2033(4) 0.0866(19) Uani 1 1 d . . . . .
H23D H -0.044398 0.937159 0.172339 0.130 Uiso 1 1 calc GR . . . .
H23E H -0.234724 0.965014 0.212010 0.130 Uiso 1 1 calc GR . . . .
H23F H -0.191229 0.815963 0.190070 0.130 Uiso 1 1 calc GR . . . .
C22A C 0.9376(14) 0.8323(11) 0.9736(4) 0.108(3) Uani 1 1 d . . . . .
H22A H 1.039356 0.851941 0.944699 0.130 Uiso 1 1 calc R . . . .
H22B H 0.922901 0.917250 1.000351 0.130 Uiso 1 1 calc R . . . .
C23A C 1.0109(19) 0.7446(12) 1.0072(5) 0.144(5) Uani 1 1 d . . . . .
H23A H 1.011939 0.657373 0.981515 0.216 Uiso 1 1 calc GR . . . .
H23B H 0.919769 0.734641 1.039263 0.216 Uiso 1 1 calc GR . . . .
H23C H 1.150694 0.782154 1.023736 0.216 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'
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
0 6 0 0.0348
0 -6 0 0.0149
0 6 4 0.0331
-4 0 3 0.1040
0 0 -14 0.0231
3 -3 -7 0.0894
3 -5 -1 0.0773
1 -5 11 0.0355
0 2 13 0.0203
-2 6 -3 0.0644
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
O4A Si1A C26A 105.12(16) . . ?
O4A Si1A C24A 111.02(19) . . ?
O4A Si1A C25A 110.7(3) . . ?
C24A Si1A C26A 108.7(3) . . ?
C25A Si1A C26A 110.9(2) . . ?
C25A Si1A C24A 110.2(3) . . ?
O51 Si52 C26B 105.50(19) . . ?
O51 Si52 C24B 111.84(17) . . ?
O51 Si52 C25B 109.5(2) . . ?
C24B Si52 C26B 110.9(3) . . ?
C25B Si52 C26B 110.0(3) . . ?
C25B Si52 C24B 109.0(3) . . ?
C1B O65 C19B 116.2(3) . . ?
C17B O51 Si52 129.8(2) . . ?
C15A O4A Si1A 129.5(2) . . ?
C21B O61 C22B 116.2(3) . . ?
C1A O1A C19A 117.1(3) . . ?
O51 C17B H17C 109.2 . . ?
O51 C17B C12B 113.7(3) . . ?
O51 C17B C16B 111.3(3) . . ?
C12B C17B H17C 109.2 . . ?
C12B C17B C16B 104.2(2) . . ?
C16B C17B H17C 109.2 . . ?
C9B C10B H10C 106.6 . . ?
C4B C10B H10C 106.6 . . ?
C4B C10B C9B 111.5(2) . . ?
C4B C10B C14B 113.2(3) . . ?
C14B C10B H10C 106.6 . . ?
C14B C10B C9B 112.0(3) . . ?
C12A C13A C15A 116.7(3) . . ?
C12A C13A C14A 107.8(3) . . ?
C12A C13A C18A 109.7(3) . . ?
C14A C13A C15A 99.9(3) . . ?
C18A C13A C15A 109.5(3) . . ?
C18A C13A C14A 113.0(3) . . ?
H15B C15B H15C 108.9 . . ?
C11B C15B H15B 110.9 . . ?
C11B C15B H15C 110.9 . . ?
C11B C15B C16B 104.4(2) . . ?
C16B C15B H15B 110.9 . . ?
C16B C15B H15C 110.9 . . ?
O65 C1B C2B 115.8(3) . . ?
O65 C1B C6B 124.7(3) . . ?
C6B C1B C2B 119.5(3) . . ?
C17B C12B C11B 99.2(3) . . ?
C18B C12B C17B 109.4(3) . . ?
C18B C12B C11B 113.4(3) . . ?
C13B C12B C17B 115.4(3) . . ?
C13B C12B C11B 108.5(3) . . ?
C13B C12B C18B 110.5(3) . . ?
C15B C11B C12B 103.8(2) . . ?
C15B C11B H11C 106.5 . . ?
C12B C11B H11C 106.5 . . ?
C9B C11B C15B 119.8(2) . . ?
C9B C11B C12B 113.0(3) . . ?
C9B C11B H11C 106.5 . . ?
C5A C4A C7A 121.0(3) . . ?
C3A C4A C5A 117.9(3) . . ?
C3A C4A C7A 121.0(3) . . ?
C5A C6A H6A 119.3 . . ?
C1A C6A H6A 119.3 . . ?
C1A C6A C5A 121.3(3) . . ?
O61 C21B C20B 110.6(3) . . ?
O64 C21B O61 124.1(3) . . ?
O64 C21B C20B 125.3(3) . . ?
C10B C9B H9B 108.6 . . ?
C11B C9B C10B 107.6(2) . . ?
C11B C9B H9B 108.6 . . ?
C8B C9B C10B 109.4(3) . . ?
C8B C9B C11B 113.8(3) . . ?
C8B C9B H9B 108.6 . . ?
H11A C11A H11B 107.6 . . ?
C12A C11A H11A 108.7 . . ?
C12A C11A H11B 108.7 . . ?
C7A C11A H11A 108.7 . . ?
C7A C11A H11B 108.7 . . ?
C7A C11A C12A 114.3(3) . . ?
C1B C2B H2B 119.4 . . ?
C3B C2B C1B 121.2(3) . . ?
C3B C2B H2B 119.4 . . ?
C2B C3B C4B 119.6(3) . . ?
C2B C3B C7B 118.3(3) . . ?
C4B C3B C7B 122.1(3) . . ?
C4A C5A C6A 119.7(3) . . ?
C4A C5A C10A 122.0(3) . . ?
C6A C5A C10A 118.2(3) . . ?
C9A C8A H8A 108.1 . . ?
C9A C8A C7A 109.6(3) . . ?
C7A C8A H8A 108.1 . . ?
C14A C8A H8A 108.1 . . ?
C14A C8A C9A 114.8(3) . . ?
C14A C8A C7A 108.1(3) . . ?
C13A C12A C11A 112.1(3) . . ?
C13A C12A H12A 109.2 . . ?
C13A C12A H12B 109.2 . . ?
C11A C12A H12A 109.2 . . ?
C11A C12A H12B 109.2 . . ?
H12A C12A H12B 107.9 . . ?
C3B C4B C10B 120.9(3) . . ?
C5B C4B C10B 120.8(3) . . ?
C5B C4B C3B 118.3(3) . . ?
C10B C14B H14B 109.0 . . ?
C10B C14B H14C 109.0 . . ?
H14B C14B H14C 107.8 . . ?
C13B C14B C10B 112.7(3) . . ?
C13B C14B H14B 109.0 . . ?
C13B C14B H14C 109.0 . . ?
O1A C1A C6A 125.0(3) . . ?
O1A C1A C2A 115.7(3) . . ?
C6A C1A C2A 119.3(3) . . ?
C1B C6B H6B 120.6 . . ?
C1B C6B C5B 118.9(3) . . ?
C5B C6B H6B 120.6 . . ?
O4A C15A C13A 114.8(3) . . ?
O4A C15A H15A 109.4 . . ?
O4A C15A C16A 109.8(3) . . ?
C13A C15A H15A 109.4 . . ?
C13A C15A C16A 103.8(3) . . ?
C16A C15A H15A 109.4 . . ?
C9B C8B H8BA 109.5 . . ?
C9B C8B H8BB 109.5 . . ?
C9B C8B C7B 110.5(3) . . ?
H8BA C8B H8BB 108.1 . . ?
C7B C8B H8BA 109.5 . . ?
C7B C8B H8BB 109.5 . . ?
C17B C16B C15B 105.3(2) . . ?
C17B C16B H16B 108.7 . . ?
C15B C16B H16B 108.7 . . ?
C20B C16B C17B 111.9(3) . . ?
C20B C16B C15B 113.5(3) . . ?
C20B C16B H16B 108.7 . . ?
C12B C18B H18D 109.5 . . ?
C12B C18B H18E 109.5 . . ?
C12B C18B H18F 109.5 . . ?
H18D C18B H18E 109.5 . . ?
H18D C18B H18F 109.5 . . ?
H18E C18B H18F 109.5 . . ?
C12B C13B C14B 111.3(2) . . ?
C12B C13B H13A 109.4 . . ?
C12B C13B H13B 109.4 . . ?
C14B C13B H13A 109.4 . . ?
C14B C13B H13B 109.4 . . ?
H13A C13B H13B 108.0 . . ?
C4B C5B C6B 122.3(3) . . ?
C4B C5B H5B 118.8 . . ?
C6B C5B H5B 118.8 . . ?
C1A C2A H2A 120.1 . . ?
C3A C2A C1A 119.8(3) . . ?
C3A C2A H2A 120.1 . . ?
C4A C3A H3A 119.0 . . ?
C2A C3A C4A 122.0(3) . . ?
C2A C3A H3A 119.0 . . ?
C3B C7B C8B 113.9(3) . . ?
C3B C7B H7BA 108.8 . . ?
C3B C7B H7BB 108.8 . . ?
C8B C7B H7BA 108.8 . . ?
C8B C7B H7BB 108.8 . . ?
H7BA C7B H7BB 107.7 . . ?
C8A C9A H9AA 109.7 . . ?
C8A C9A H9AB 109.7 . . ?
C8A C9A C10A 109.6(3) . . ?
H9AA C9A H9AB 108.2 . . ?
C10A C9A H9AA 109.7 . . ?
C10A C9A H9AB 109.7 . . ?
C4A C7A C8A 111.6(3) . . ?
C4A C7A H7A 106.0 . . ?
C11A C7A C4A 114.2(3) . . ?
C11A C7A C8A 112.4(3) . . ?
C11A C7A H7A 106.0 . . ?
C8A C7A H7A 106.0 . . ?
C27A C26A Si1A 110.3(3) . . ?
C27A C26A C28A 109.6(4) . . ?
C27A C26A C29A 108.5(5) . . ?
C28A C26A Si1A 109.0(3) . . ?
C29A C26A Si1A 109.6(3) . . ?
C29A C26A C28A 109.9(4) . . ?
C15A C16A H16A 107.5 . . ?
C17A C16A C15A 105.8(3) . . ?
C17A C16A H16A 107.5 . . ?
C20A C16A C15A 114.2(4) . . ?
C20A C16A H16A 107.5 . . ?
C20A C16A C17A 114.1(4) . . ?
C13A C14A H14A 106.6 . . ?
C8A C14A C13A 112.3(3) . . ?
C8A C14A H14A 106.6 . . ?
C8A C14A C17A 119.1(3) . . ?
C17A C14A C13A 105.0(3) . . ?
C17A C14A H14A 106.6 . . ?
O65 C19B H19D 109.5 . . ?
O65 C19B H19E 109.5 . . ?
O65 C19B H19F 109.5 . . ?
H19D C19B H19E 109.5 . . ?
H19D C19B H19F 109.5 . . ?
H19E C19B H19F 109.5 . . ?
C21B C20B C16B 113.1(3) . . ?
C21B C20B H20C 109.0 . . ?
C21B C20B H20D 109.0 . . ?
C16B C20B H20C 109.0 . . ?
C16B C20B H20D 109.0 . . ?
H20C C20B H20D 107.8 . . ?
O2A C21A O3A 126.2(6) . . ?
O2A C21A C20A 122.2(5) . . ?
O3A C21A C20A 111.5(5) . . ?
C5A C10A C9A 113.5(3) . . ?
C5A C10A H10A 108.9 . . ?
C5A C10A H10B 108.9 . . ?
C9A C10A H10A 108.9 . . ?
C9A C10A H10B 108.9 . . ?
H10A C10A H10B 107.7 . . ?
C13A C18A H18A 109.5 . . ?
C13A C18A H18B 109.5 . . ?
C13A C18A H18C 109.5 . . ?
H18A C18A H18B 109.5 . . ?
H18A C18A H18C 109.5 . . ?
H18B C18A H18C 109.5 . . ?
C16A C17A H17A 110.8 . . ?
C16A C17A H17B 110.8 . . ?
C14A C17A C16A 104.7(3) . . ?
C14A C17A H17A 110.8 . . ?
C14A C17A H17B 110.8 . . ?
H17A C17A H17B 108.9 . . ?
O1A C19A H19A 109.5 . . ?
O1A C19A H19B 109.5 . . ?
O1A C19A H19C 109.5 . . ?
H19A C19A H19B 109.5 . . ?
H19A C19A H19C 109.5 . . ?
H19B C19A H19C 109.5 . . ?
O61 C22B H22C 109.4 . . ?
O61 C22B H22D 109.4 . . ?
O61 C22B C23B 111.0(5) . . ?
H22C C22B H22D 108.0 . . ?
C23B C22B H22C 109.4 . . ?
C23B C22B H22D 109.4 . . ?
C28B C26B Si52 110.0(4) . . ?
C28B C26B C29B 107.8(5) . . ?
C29B C26B Si52 110.3(4) . . ?
C27B C26B Si52 109.4(4) . . ?
C27B C26B C28B 109.1(4) . . ?
C27B C26B C29B 110.3(6) . . ?
C21A O3A C22A 115.6(7) . . ?
Si52 C24B H24D 109.5 . . ?
Si52 C24B H24E 109.5 . . ?
Si52 C24B H24F 109.5 . . ?
H24D C24B H24E 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B H24F 109.5 . . ?
C26A C27A H27A 109.5 . . ?
C26A C27A H27B 109.5 . . ?
C26A C27A H27C 109.5 . . ?
H27A C27A H27B 109.5 . . ?
H27A C27A H27C 109.5 . . ?
H27B C27A H27C 109.5 . . ?
C26A C28A H28A 109.5 . . ?
C26A C28A H28B 109.5 . . ?
C26A C28A H28C 109.5 . . ?
H28A C28A H28B 109.5 . . ?
H28A C28A H28C 109.5 . . ?
H28B C28A H28C 109.5 . . ?
C16A C20A C21A 113.7(5) . . ?
C16A C20A H20A 108.8 . . ?
C16A C20A H20B 108.8 . . ?
C21A C20A H20A 108.8 . . ?
C21A C20A H20B 108.8 . . ?
H20A C20A H20B 107.7 . . ?
Si1A C24A H24A 109.5 . . ?
Si1A C24A H24B 109.5 . . ?
Si1A C24A H24C 109.5 . . ?
H24A C24A H24B 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
C26A C29A H29A 109.5 . . ?
C26A C29A H29B 109.5 . . ?
C26A C29A H29C 109.5 . . ?
H29A C29A H29B 109.5 . . ?
H29A C29A H29C 109.5 . . ?
H29B C29A H29C 109.5 . . ?
C26B C28B H28D 109.5 . . ?
C26B C28B H28E 109.5 . . ?
C26B C28B H28F 109.5 . . ?
H28D C28B H28E 109.5 . . ?
H28D C28B H28F 109.5 . . ?
H28E C28B H28F 109.5 . . ?
Si1A C25A H25A 109.5 . . ?
Si1A C25A H25B 109.5 . . ?
Si1A C25A H25C 109.5 . . ?
H25A C25A H25B 109.5 . . ?
H25A C25A H25C 109.5 . . ?
H25B C25A H25C 109.5 . . ?
Si52 C25B H25D 109.5 . . ?
Si52 C25B H25E 109.5 . . ?
Si52 C25B H25F 109.5 . . ?
H25D C25B H25E 109.5 . . ?
H25D C25B H25F 109.5 . . ?
H25E C25B H25F 109.5 . . ?
C26B C29B H29D 109.5 . . ?
C26B C29B H29E 109.5 . . ?
C26B C29B H29F 109.5 . . ?
H29D C29B H29E 109.5 . . ?
H29D C29B H29F 109.5 . . ?
H29E C29B H29F 109.5 . . ?
C26B C27B H27D 109.5 . . ?
C26B C27B H27E 109.5 . . ?
C26B C27B H27F 109.5 . . ?
H27D C27B H27E 109.5 . . ?
H27D C27B H27F 109.5 . . ?
H27E C27B H27F 109.5 . . ?
C22B C23B H23D 109.5 . . ?
C22B C23B H23E 109.5 . . ?
C22B C23B H23F 109.5 . . ?
H23D C23B H23E 109.5 . . ?
H23D C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
O3A C22A H22A 109.4 . . ?
O3A C22A H22B 109.4 . . ?
H22A C22A H22B 108.0 . . ?
C23A C22A O3A 111.0(8) . . ?
C23A C22A H22A 109.4 . . ?
C23A C22A H22B 109.4 . . ?
C22A C23A H23A 109.5 . . ?
C22A C23A H23B 109.5 . . ?
C22A C23A H23C 109.5 . . ?
H23A C23A H23B 109.5 . . ?
H23A C23A H23C 109.5 . . ?
H23B C23A H23C 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
Si1A O4A 1.652(3) . ?
Si1A C26A 1.880(4) . ?
Si1A C24A 1.877(5) . ?
Si1A C25A 1.863(5) . ?
Si52 O51 1.641(2) . ?
Si52 C26B 1.887(6) . ?
Si52 C24B 1.871(5) . ?
Si52 C25B 1.863(5) . ?
O65 C1B 1.370(4) . ?
O65 C19B 1.423(4) . ?
O51 C17B 1.428(4) . ?
O4A C15A 1.422(5) . ?
O61 C21B 1.335(5) . ?
O61 C22B 1.449(5) . ?
O1A C1A 1.373(4) . ?
O1A C19A 1.420(5) . ?
O64 C21B 1.200(5) . ?
C17B H17C 0.9800 . ?
C17B C12B 1.534(4) . ?
C17B C16B 1.546(4) . ?
C10B H10C 0.9800 . ?
C10B C9B 1.542(4) . ?
C10B C4B 1.528(4) . ?
C10B C14B 1.536(4) . ?
C13A C12A 1.527(5) . ?
C13A C15A 1.541(5) . ?
C13A C14A 1.538(5) . ?
C13A C18A 1.535(5) . ?
C15B H15B 0.9700 . ?
C15B H15C 0.9700 . ?
C15B C11B 1.531(4) . ?
C15B C16B 1.550(4) . ?
C1B C2B 1.396(5) . ?
C1B C6B 1.384(5) . ?
C12B C11B 1.540(4) . ?
C12B C18B 1.533(5) . ?
C12B C13B 1.525(4) . ?
C11B H11C 0.9800 . ?
C11B C9B 1.525(4) . ?
C4A C5A 1.402(5) . ?
C4A C3A 1.397(5) . ?
C4A C7A 1.526(5) . ?
C6A H6A 0.9300 . ?
C6A C5A 1.404(5) . ?
C6A C1A 1.380(6) . ?
C21B C20B 1.514(5) . ?
C9B H9B 0.9800 . ?
C9B C8B 1.515(4) . ?
C11A H11A 0.9700 . ?
C11A H11B 0.9700 . ?
C11A C12A 1.542(5) . ?
C11A C7A 1.521(5) . ?
C2B H2B 0.9300 . ?
C2B C3B 1.393(5) . ?
C3B C4B 1.396(4) . ?
C3B C7B 1.518(4) . ?
C5A C10A 1.503(5) . ?
C8A H8A 0.9800 . ?
C8A C9A 1.520(5) . ?
C8A C7A 1.540(5) . ?
C8A C14A 1.520(5) . ?
C12A H12A 0.9700 . ?
C12A H12B 0.9700 . ?
C4B C5B 1.393(4) . ?
O2A C21A 1.207(7) . ?
C14B H14B 0.9700 . ?
C14B H14C 0.9700 . ?
C14B C13B 1.535(4) . ?
C1A C2A 1.389(5) . ?
C6B H6B 0.9300 . ?
C6B C5B 1.394(5) . ?
C15A H15A 0.9800 . ?
C15A C16A 1.555(6) . ?
C8B H8BA 0.9700 . ?
C8B H8BB 0.9700 . ?
C8B C7B 1.525(5) . ?
C16B H16B 0.9800 . ?
C16B C20B 1.525(5) . ?
C18B H18D 0.9600 . ?
C18B H18E 0.9600 . ?
C18B H18F 0.9600 . ?
C13B H13A 0.9700 . ?
C13B H13B 0.9700 . ?
C5B H5B 0.9300 . ?
C2A H2A 0.9300 . ?
C2A C3A 1.387(5) . ?
C3A H3A 0.9300 . ?
C7B H7BA 0.9700 . ?
C7B H7BB 0.9700 . ?
C9A H9AA 0.9700 . ?
C9A H9AB 0.9700 . ?
C9A C10A 1.523(5) . ?
C7A H7A 0.9800 . ?
C26A C27A 1.516(6) . ?
C26A C28A 1.538(6) . ?
C26A C29A 1.523(7) . ?
C16A H16A 0.9800 . ?
C16A C17A 1.542(6) . ?
C16A C20A 1.496(6) . ?
C14A H14A 0.9800 . ?
C14A C17A 1.534(5) . ?
C19B H19D 0.9600 . ?
C19B H19E 0.9600 . ?
C19B H19F 0.9600 . ?
C20B H20C 0.9700 . ?
C20B H20D 0.9700 . ?
C21A O3A 1.259(7) . ?
C21A C20A 1.572(8) . ?
C10A H10A 0.9700 . ?
C10A H10B 0.9700 . ?
C18A H18A 0.9600 . ?
C18A H18B 0.9600 . ?
C18A H18C 0.9600 . ?
C17A H17A 0.9700 . ?
C17A H17B 0.9700 . ?
C19A H19A 0.9600 . ?
C19A H19B 0.9600 . ?
C19A H19C 0.9600 . ?
C22B H22C 0.9700 . ?
C22B H22D 0.9700 . ?
C22B C23B 1.476(9) . ?
C26B C28B 1.535(6) . ?
C26B C29B 1.537(9) . ?
C26B C27B 1.523(8) . ?
O3A C22A 1.445(9) . ?
C24B H24D 0.9600 . ?
C24B H24E 0.9600 . ?
C24B H24F 0.9600 . ?
C27A H27A 0.9600 . ?
C27A H27B 0.9600 . ?
C27A H27C 0.9600 . ?
C28A H28A 0.9600 . ?
C28A H28B 0.9600 . ?
C28A H28C 0.9600 . ?
C20A H20A 0.9700 . ?
C20A H20B 0.9700 . ?
C24A H24A 0.9600 . ?
C24A H24B 0.9600 . ?
C24A H24C 0.9600 . ?
C29A H29A 0.9600 . ?
C29A H29B 0.9600 . ?
C29A H29C 0.9600 . ?
C28B H28D 0.9600 . ?
C28B H28E 0.9600 . ?
C28B H28F 0.9600 . ?
C25A H25A 0.9600 . ?
C25A H25B 0.9600 . ?
C25A H25C 0.9600 . ?
C25B H25D 0.9600 . ?
C25B H25E 0.9600 . ?
C25B H25F 0.9600 . ?
C29B H29D 0.9600 . ?
C29B H29E 0.9600 . ?
C29B H29F 0.9600 . ?
C27B H27D 0.9600 . ?
C27B H27E 0.9600 . ?
C27B H27F 0.9600 . ?
C23B H23D 0.9600 . ?
C23B H23E 0.9600 . ?
C23B H23F 0.9600 . ?
C22A H22A 0.9700 . ?
C22A H22B 0.9700 . ?
C22A C23A 1.411(13) . ?
C23A H23A 0.9600 . ?
C23A H23B 0.9600 . ?
C23A H23C 0.9600 . ?
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
Si1A O4A C15A C13A -111.1(3) . . . . ?
Si1A O4A C15A C16A 132.5(3) . . . . ?
Si52 O51 C17B C12B -115.8(3) . . . . ?
Si52 O51 C17B C16B 126.8(3) . . . . ?
O65 C1B C2B C3B 177.0(3) . . . . ?
O65 C1B C6B C5B -177.6(3) . . . . ?
O51 Si52 C26B C28B -178.2(3) . . . . ?
O51 Si52 C26B C29B -59.4(4) . . . . ?
O51 Si52 C26B C27B 62.1(5) . . . . ?
O51 C17B C12B C11B -165.0(3) . . . . ?
O51 C17B C12B C18B -46.1(3) . . . . ?
O51 C17B C12B C13B 79.3(4) . . . . ?
O51 C17B C16B C15B 147.6(3) . . . . ?
O51 C17B C16B C20B -88.6(3) . . . . ?
O4A Si1A C26A C27A -62.5(4) . . . . ?
O4A Si1A C26A C28A 177.2(4) . . . . ?
O4A Si1A C26A C29A 56.9(4) . . . . ?
O4A C15A C16A C17A 149.2(3) . . . . ?
O4A C15A C16A C20A -84.4(4) . . . . ?
O61 C21B C20B C16B 173.8(3) . . . . ?
O1A C1A C2A C3A -179.2(3) . . . . ?
O64 C21B C20B C16B -7.0(5) . . . . ?
C17B C12B C11B C15B 46.9(3) . . . . ?
C17B C12B C11B C9B 178.2(2) . . . . ?
C17B C12B C13B C14B 165.5(3) . . . . ?
C17B C16B C20B C21B 171.6(3) . . . . ?
C10B C9B C8B C7B -64.3(3) . . . . ?
C10B C4B C5B C6B 177.6(3) . . . . ?
C10B C14B C13B C12B -53.3(4) . . . . ?
C13A C15A C16A C17A 26.0(4) . . . . ?
C13A C15A C16A C20A 152.4(4) . . . . ?
C13A C14A C17A C16A -28.4(4) . . . . ?
C15B C11B C9B C10B -177.2(3) . . . . ?
C15B C11B C9B C8B -55.8(4) . . . . ?
C15B C16B C20B C21B -69.4(4) . . . . ?
C1B C2B C3B C4B 1.8(5) . . . . ?
C1B C2B C3B C7B -178.0(3) . . . . ?
C1B C6B C5B C4B -0.6(6) . . . . ?
C12B C17B C16B C15B 24.6(3) . . . . ?
C12B C17B C16B C20B 148.4(3) . . . . ?
C12B C11B C9B C10B 60.0(3) . . . . ?
C12B C11B C9B C8B -178.5(3) . . . . ?
C11B C15B C16B C17B 4.7(4) . . . . ?
C11B C15B C16B C20B -118.0(3) . . . . ?
C11B C12B C13B C14B 55.3(3) . . . . ?
C11B C9B C8B C7B 175.2(3) . . . . ?
C4A C5A C10A C9A -16.8(5) . . . . ?
C6A C5A C10A C9A 162.4(3) . . . . ?
C6A C1A C2A C3A 0.5(5) . . . . ?
C21B O61 C22B C23B -90.7(5) . . . . ?
C9B C10B C4B C3B -22.3(4) . . . . ?
C9B C10B C4B C5B 159.8(3) . . . . ?
C9B C10B C14B C13B 53.3(4) . . . . ?
C9B C8B C7B C3B 43.0(4) . . . . ?
C2B C1B C6B C5B 2.1(5) . . . . ?
C2B C3B C4B C10B -178.3(3) . . . . ?
C2B C3B C4B C5B -0.3(5) . . . . ?
C2B C3B C7B C8B 168.0(3) . . . . ?
C3B C4B C5B C6B -0.3(5) . . . . ?
C5A C4A C3A C2A -1.0(5) . . . . ?
C5A C4A C7A C11A -149.4(3) . . . . ?
C5A C4A C7A C8A -20.6(4) . . . . ?
C5A C6A C1A O1A 179.0(3) . . . . ?
C5A C6A C1A C2A -0.7(5) . . . . ?
C8A C9A C10A C5A 47.2(4) . . . . ?
C8A C14A C17A C16A -155.2(3) . . . . ?
C12A C13A C15A O4A 81.9(4) . . . . ?
C12A C13A C15A C16A -158.2(3) . . . . ?
C12A C13A C14A C8A -62.8(3) . . . . ?
C12A C13A C14A C17A 166.4(3) . . . . ?
C12A C11A C7A C4A 177.2(3) . . . . ?
C12A C11A C7A C8A 48.7(4) . . . . ?
C4B C10B C9B C11B 177.1(3) . . . . ?
C4B C10B C9B C8B 53.0(4) . . . . ?
C4B C10B C14B C13B -179.6(3) . . . . ?
C4B C3B C7B C8B -11.8(5) . . . . ?
O2A C21A O3A C22A -3.4(11) . . . . ?
O2A C21A C20A C16A -3.8(8) . . . . ?
C14B C10B C9B C11B -54.9(3) . . . . ?
C14B C10B C9B C8B -179.0(3) . . . . ?
C14B C10B C4B C3B -149.6(3) . . . . ?
C14B C10B C4B C5B 32.5(4) . . . . ?
C1A C6A C5A C4A 0.0(5) . . . . ?
C1A C6A C5A C10A -179.2(3) . . . . ?
C1A C2A C3A C4A 0.3(5) . . . . ?
C6B C1B C2B C3B -2.7(5) . . . . ?
C15A C13A C12A C11A 165.3(3) . . . . ?
C15A C13A C14A C8A 174.9(3) . . . . ?
C15A C13A C14A C17A 44.1(3) . . . . ?
C15A C16A C17A C14A 1.3(4) . . . . ?
C15A C16A C20A C21A 173.9(4) . . . . ?
C16B C17B C12B C11B -43.6(3) . . . . ?
C16B C17B C12B C18B 75.3(3) . . . . ?
C16B C17B C12B C13B -159.3(3) . . . . ?
C16B C15B C11B C12B -32.3(3) . . . . ?
C16B C15B C11B C9B -159.4(3) . . . . ?
C18B C12B C11B C15B -69.0(3) . . . . ?
C18B C12B C11B C9B 62.3(3) . . . . ?
C18B C12B C13B C14B -69.7(3) . . . . ?
C13B C12B C11B C15B 167.8(3) . . . . ?
C13B C12B C11B C9B -60.9(3) . . . . ?
C3A C4A C5A C6A 0.9(5) . . . . ?
C3A C4A C5A C10A -180.0(3) . . . . ?
C3A C4A C7A C11A 34.1(4) . . . . ?
C3A C4A C7A C8A 162.9(3) . . . . ?
C7B C3B C4B C10B 1.6(5) . . . . ?
C7B C3B C4B C5B 179.6(3) . . . . ?
C9A C8A C7A C4A 51.0(4) . . . . ?
C9A C8A C7A C11A -179.3(3) . . . . ?
C9A C8A C14A C13A -175.2(3) . . . . ?
C9A C8A C14A C17A -52.0(4) . . . . ?
C7A C4A C5A C6A -175.7(3) . . . . ?
C7A C4A C5A C10A 3.4(5) . . . . ?
C7A C4A C3A C2A 175.6(3) . . . . ?
C7A C11A C12A C13A -49.4(4) . . . . ?
C7A C8A C9A C10A -65.3(4) . . . . ?
C7A C8A C14A C13A 62.2(3) . . . . ?
C7A C8A C14A C17A -174.6(3) . . . . ?
C26A Si1A O4A C15A -171.8(3) . . . . ?
C14A C13A C12A C11A 54.0(4) . . . . ?
C14A C13A C15A O4A -162.4(3) . . . . ?
C14A C13A C15A C16A -42.5(3) . . . . ?
C14A C8A C9A C10A 172.9(3) . . . . ?
C14A C8A C7A C4A 176.7(3) . . . . ?
C14A C8A C7A C11A -53.5(4) . . . . ?
C19B O65 C1B C2B -179.4(3) . . . . ?
C19B O65 C1B C6B 0.3(5) . . . . ?
C21A O3A C22A C23A -94.4(11) . . . . ?
C18A C13A C12A C11A -69.4(4) . . . . ?
C18A C13A C15A O4A -43.5(4) . . . . ?
C18A C13A C15A C16A 76.4(4) . . . . ?
C18A C13A C14A C8A 58.7(4) . . . . ?
C18A C13A C14A C17A -72.2(4) . . . . ?
C17A C16A C20A C21A -64.1(6) . . . . ?
C19A O1A C1A C6A 0.3(6) . . . . ?
C19A O1A C1A C2A 180.0(4) . . . . ?
C22B O61 C21B O64 -1.7(6) . . . . ?
C22B O61 C21B C20B 177.5(4) . . . . ?
C26B Si52 O51 C17B 143.8(3) . . . . ?
O3A C21A C20A C16A 173.6(5) . . . . ?
C24B Si52 O51 C17B 23.1(4) . . . . ?
C24B Si52 C26B C28B -56.9(4) . . . . ?
C24B Si52 C26B C29B 61.9(5) . . . . ?
C24B Si52 C26B C27B -176.6(4) . . . . ?
C20A C16A C17A C14A -125.1(4) . . . . ?
C20A C21A O3A C22A 179.4(7) . . . . ?
C24A Si1A O4A C15A 70.8(4) . . . . ?
C24A Si1A C26A C27A 56.4(4) . . . . ?
C24A Si1A C26A C28A -63.9(4) . . . . ?
C24A Si1A C26A C29A 175.8(4) . . . . ?
C25A Si1A O4A C15A -52.0(4) . . . . ?
C25A Si1A C26A C27A 177.8(4) . . . . ?
C25A Si1A C26A C28A 57.5(5) . . . . ?
C25A Si1A C26A C29A -62.8(4) . . . . ?
C25B Si52 O51 C17B -97.9(4) . . . . ?
C25B Si52 C26B C28B 63.9(4) . . . . ?
C25B Si52 C26B C29B -177.4(4) . . . . ?
C25B Si52 C26B C27B -55.9(5) . . . . ?
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
-0.0008 5.9985 0.0027 0.3381 -0.1208 -0.8671
0.0008 -5.9985 -0.0027 -0.3381 0.1208 0.8671
-0.0009 5.9981 4.0033 0.2156 -0.3567 -0.9451
-4.0006 0.0032 2.9934 0.6006 -0.6350 0.4399
0.0005 0.0016 -14.0021 0.4285 0.8258 0.2728
3.0011 -3.0012 -6.9971 -0.4741 0.8168 0.1962
3.0011 -5.0014 -0.9971 -0.7704 0.5031 0.3683
1.0004 -5.0009 11.0011 -0.7915 -0.4337 0.3837
-0.0008 1.9981 13.0028 -0.2852 -0.8070 -0.5424
-2.0009 6.0007 -3.0013 0.7761 -0.1728 -0.5595
