#------------------------------------------------------------------------------
#$Date: 2020-10-04 06:04:58 +0300 (Sun, 04 Oct 2020) $
#$Revision: 257047 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/76/4517695.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_4517695
loop_
_publ_author_name
'Fast, Caleb D.'
'Jones, Caleb A. H.'
'Schley, Nathan D.'
_publ_section_title
;
 Selectivity and Mechanism of Iridium-Catalyzed Cyclohexyl Methyl Ether
 Cleavage
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              6450
_journal_page_last               6456
_journal_paper_doi               10.1021/acscatal.0c01718
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C42 H64 O3 Si'
_chemical_formula_sum            'C42 H64 O3 Si'
_chemical_formula_weight         645.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.5320(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.55791(14)
_cell_length_b                   11.21470(10)
_cell_length_c                   14.01011(16)
_cell_measurement_reflns_used    10039
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.2440
_cell_measurement_theta_min      3.2850
_cell_volume                     1881.44(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1506
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_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  32.00   1.00    3.00    --  -37.09  38.00  60.00   88
  2  ω    -54.00  30.00   1.00    3.00    --  -37.09  57.00 120.00   84
  3  ω    -54.00  30.00   1.00    3.00    --  -37.09  57.00 150.00   84
  4  ω   -104.00 -20.00   1.00    3.00    --  -37.09 -57.00 150.00   84
  5  ω    -64.00  30.00   1.00    3.00    --  -37.09  77.00-180.00   94
  6  ω   -104.00 -20.00   1.00    3.00    --  -37.09 -57.00  60.00   84
  7  ω     20.00 104.00   1.00    3.00    --   37.09  57.00  90.00   84
  8  ω      8.00 108.00   1.00    3.00    --   37.09  19.00-150.00  100
  9  ω      4.00  33.00   1.00    3.00    --   37.09  88.00 162.77   29
 10  ω     10.00 105.00   1.00    3.00    --   37.09  77.00  90.00   95
 11  ω      4.00  33.00   1.00    3.00    --   37.09  88.00  25.98   29
 12  ω      3.00  32.00   1.00    3.00    --   37.09  90.00-109.70   29
 13  ω     20.00 104.00   1.00    3.00    --   37.09  57.00  60.00   84
 14  ω    -32.00  56.00   1.00    3.00    --   37.09 -38.00  30.00   88
 15  ω     42.00 145.00   1.00   16.00    --  111.00 -90.00 137.00  103
 16  ω     43.00 128.00   1.00   16.00    --  111.00 -45.00  90.00   85
 17  ω     41.00 132.00   1.00   16.00    --  111.00 -30.00-120.00   91
 18  ω     43.00 128.00   1.00   16.00    --  111.00 -45.00 120.00   85
 19  ω     42.00 144.00   1.00   16.00    --  111.00 -88.00 -58.30  102
 20  ω     42.00 178.00   1.00   16.00    --  111.00   0.00  30.00  136
 21  ω     43.00 128.00   1.00   16.00    --  111.00 -45.00   0.00   85
 22  ω     41.00 132.00   1.00   16.00    --  111.00 -30.00 -30.00   91
 23  ω     41.00 132.00   1.00   16.00    --  111.00 -30.00-180.00   91
 24  ω     42.00 145.00   1.00   16.00    --  111.00 -90.00  28.49  103
 25  ω     93.00 178.00   1.00   16.00    --  111.00  61.00  60.00   85
 26  ω     42.00 130.00   1.00   16.00    --  111.00 -90.00-122.69   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0860903000
_diffrn_orient_matrix_UB_12      -0.0294364000
_diffrn_orient_matrix_UB_13      0.1015204000
_diffrn_orient_matrix_UB_21      0.0088518000
_diffrn_orient_matrix_UB_22      0.1334301000
_diffrn_orient_matrix_UB_23      0.0274813000
_diffrn_orient_matrix_UB_31      -0.0951611000
_diffrn_orient_matrix_UB_32      -0.0142160000
_diffrn_orient_matrix_UB_33      0.0473678000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19098
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.383
_diffrn_reflns_theta_min         3.308
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.818
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.932
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_description       block
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.114
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.182
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details
;
 Flack x determined using 3058 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         7374
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0322
_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)+(0.0321P)²+0.2159P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0770
_reflns_Friedel_coverage         0.871
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.961
_reflns_number_gt                6948
_reflns_number_total             7374
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cs0c01718_si_002.cif
_cod_data_source_block           16
_cod_depositor_comments
'Adding full bibliography for 4517689--4517702.cif.'
_cod_database_code               4517695
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C42H64O3Si
_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.
;
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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:
 C3(H3), C5(H5), C8(H8), C9(H9), C12(H12), C14(H14), C17(H17), C20(H20)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1B,H1A), C2(H2A,H2B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B), C11(H11A,
 H11B), C15(H15A,H15B), C16(H16A,H16B), C22(H22A,H22B), C23(H23A,H23B),
 C24(H24A,H24B)
2.c Aromatic/amide H refined with riding coordinates:
 C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
 C40(H40), C41(H41), C42(H42)
2.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C)
;
_olex2_date_sample_data_collection 2019-08-15
_olex2_exptl_crystal_mounting_method 'mounted in a polyimide 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 1.307
_oxdiff_exptl_absorpt_empirical_full_min 0.858
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -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
Si1 Si 0.19780(4) 0.20310(5) 0.46761(4) 0.01198(11) Uani 1 1 d . . . . .
O1 O 0.67834(14) 0.72124(15) -0.12806(14) 0.0252(4) Uani 1 1 d . . . . .
O2 O 0.40526(12) 0.72539(13) 0.18235(11) 0.0160(3) Uani 1 1 d . . . . .
O3 O 0.20335(13) 0.30477(14) 0.38444(12) 0.0174(3) Uani 1 1 d . . . . .
C1 C 0.53587(19) 0.9799(2) -0.04186(17) 0.0185(4) Uani 1 1 d . . . . .
H1B H 0.551696 1.042494 -0.083407 0.022 Uiso 1 1 calc R . . . .
H1A H 0.545636 1.013411 0.024049 0.022 Uiso 1 1 calc R . . . .
C2 C 0.62122(19) 0.8802(2) -0.03238(18) 0.0199(5) Uani 1 1 d . . . . .
H2A H 0.696083 0.912489 -0.006599 0.024 Uiso 1 1 calc R . . . .
H2B H 0.611477 0.820590 0.014466 0.024 Uiso 1 1 calc R . . . .
C3 C 0.6069(2) 0.8224(2) -0.13390(17) 0.0193(4) Uani 1 1 d . . . . .
H3 H 0.622855 0.881605 -0.179205 0.023 Uiso 1 1 calc R . . . .
C4 C 0.48823(19) 0.7780(2) -0.17795(17) 0.0181(4) Uani 1 1 d . . . . .
H4A H 0.474106 0.715276 -0.135659 0.022 Uiso 1 1 calc R . . . .
H4B H 0.479770 0.744178 -0.243536 0.022 Uiso 1 1 calc R . . . .
C5 C 0.40151(19) 0.87800(19) -0.18772(16) 0.0167(4) Uani 1 1 d . . . . .
H5 H 0.416141 0.937950 -0.233098 0.020 Uiso 1 1 calc R . . . .
C6 C 0.2831(2) 0.8305(2) -0.23707(17) 0.0210(5) Uani 1 1 d . . . . .
H6A H 0.232026 0.897210 -0.257017 0.025 Uiso 1 1 calc R . . . .
H6B H 0.281764 0.786239 -0.296891 0.025 Uiso 1 1 calc R . . . .
C7 C 0.24392(19) 0.7495(2) -0.16634(16) 0.0195(5) Uani 1 1 d . . . . .
H7A H 0.289883 0.678350 -0.152378 0.023 Uiso 1 1 calc R . . . .
H7B H 0.167388 0.725247 -0.198677 0.023 Uiso 1 1 calc R . . . .
C8 C 0.25093(18) 0.8130(2) -0.06762(16) 0.0159(4) Uani 1 1 d . . . . .
H8 H 0.201111 0.882328 -0.082427 0.019 Uiso 1 1 calc R . . . .
C9 C 0.37178(18) 0.85723(18) -0.01680(16) 0.0142(4) Uani 1 1 d . . . . .
H9 H 0.420056 0.786708 -0.005660 0.017 Uiso 1 1 calc R . . . .
C10 C 0.41255(19) 0.94197(18) -0.08664(17) 0.0163(4) Uani 1 1 d . . . . .
C11 C 0.38404(19) 0.91161(19) 0.08703(16) 0.0171(4) Uani 1 1 d . . . . .
H11A H 0.462389 0.928033 0.119849 0.020 Uiso 1 1 calc R . . . .
H11B H 0.344449 0.987041 0.078053 0.020 Uiso 1 1 calc R . . . .
C12 C 0.33966(18) 0.83172(18) 0.15576(16) 0.0151(4) Uani 1 1 d . . . . .
H12 H 0.342767 0.875957 0.216865 0.018 Uiso 1 1 calc R . . . .
C13 C 0.21859(18) 0.79306(18) 0.10440(16) 0.0140(4) Uani 1 1 d . . . . .
C14 C 0.21521(17) 0.73196(18) 0.00420(16) 0.0149(4) Uani 1 1 d . . . . .
H14 H 0.269236 0.666375 0.020959 0.018 Uiso 1 1 calc R . . . .
C15 C 0.09934(19) 0.6750(2) -0.03064(17) 0.0225(5) Uani 1 1 d . . . . .
H15A H 0.098943 0.605942 -0.072457 0.027 Uiso 1 1 calc R . . . .
H15B H 0.043930 0.731588 -0.067889 0.027 Uiso 1 1 calc R . . . .
C16 C 0.07627(19) 0.6381(2) 0.06838(18) 0.0221(5) Uani 1 1 d . . . . .
H16A H 0.005027 0.669650 0.070282 0.027 Uiso 1 1 calc R . . . .
H16B H 0.074494 0.551896 0.073704 0.027 Uiso 1 1 calc R . . . .
C17 C 0.17268(17) 0.69054(19) 0.15526(16) 0.0147(4) Uani 1 1 d . . . . .
H17 H 0.231078 0.629470 0.174460 0.018 Uiso 1 1 calc R . . . .
C18 C 0.1415(2) 0.9028(2) 0.08947(19) 0.0214(5) Uani 1 1 d . . . . .
H18A H 0.065173 0.878030 0.062017 0.032 Uiso 1 1 calc GR . . . .
H18B H 0.160088 0.957665 0.044333 0.032 Uiso 1 1 calc GR . . . .
H18C H 0.151148 0.941221 0.152775 0.032 Uiso 1 1 calc GR . . . .
C19 C 0.3435(2) 1.0576(2) -0.10653(19) 0.0230(5) Uani 1 1 d . . . . .
H19A H 0.365322 1.105466 -0.154303 0.035 Uiso 1 1 calc GR . . . .
H19B H 0.356418 1.101260 -0.045121 0.035 Uiso 1 1 calc GR . . . .
H19C H 0.265582 1.038369 -0.132565 0.035 Uiso 1 1 calc GR . . . .
C20 C 0.13707(18) 0.71828(19) 0.24888(17) 0.0182(4) Uani 1 1 d . . . . .
H20 H 0.076773 0.777261 0.229725 0.022 Uiso 1 1 calc R . . . .
C21 C 0.2310(2) 0.7712(2) 0.33571(18) 0.0224(5) Uani 1 1 d . . . . .
H21A H 0.297371 0.724023 0.346313 0.034 Uiso 1 1 calc GR . . . .
H21B H 0.208630 0.771163 0.395453 0.034 Uiso 1 1 calc GR . . . .
H21C H 0.245811 0.851519 0.319625 0.034 Uiso 1 1 calc GR . . . .
C22 C 0.09007(19) 0.6058(2) 0.28473(17) 0.0185(4) Uani 1 1 d . . . . .
H22A H 0.061341 0.627645 0.339300 0.022 Uiso 1 1 calc R . . . .
H22B H 0.027900 0.576291 0.230368 0.022 Uiso 1 1 calc R . . . .
C23 C 0.17495(19) 0.5052(2) 0.32003(18) 0.0188(4) Uani 1 1 d . . . . .
H23A H 0.205657 0.483963 0.266547 0.023 Uiso 1 1 calc R . . . .
H23B H 0.235834 0.532552 0.376545 0.023 Uiso 1 1 calc R . . . .
C24 C 0.12184(19) 0.3969(2) 0.35030(17) 0.0181(4) Uani 1 1 d . . . . .
H24A H 0.090283 0.417947 0.403268 0.022 Uiso 1 1 calc R . . . .
H24B H 0.061848 0.368288 0.293591 0.022 Uiso 1 1 calc R . . . .
C25 C 0.7909(2) 0.7509(3) -0.1154(2) 0.0333(6) Uani 1 1 d . . . . .
H25A H 0.795338 0.800890 -0.169689 0.050 Uiso 1 1 calc GR . . . .
H25B H 0.833134 0.679397 -0.114548 0.050 Uiso 1 1 calc GR . . . .
H25C H 0.820816 0.792751 -0.053246 0.050 Uiso 1 1 calc GR . . . .
C26 C 0.50519(19) 0.7425(2) 0.26184(18) 0.0248(5) Uani 1 1 d . . . . .
H26A H 0.554642 0.793368 0.239830 0.037 Uiso 1 1 calc GR . . . .
H26B H 0.540551 0.666835 0.282035 0.037 Uiso 1 1 calc GR . . . .
H26C H 0.488032 0.778877 0.317474 0.037 Uiso 1 1 calc GR . . . .
C27 C 0.06454(18) 0.11249(19) 0.42187(16) 0.0151(4) Uani 1 1 d . . . . .
C28 C 0.07044(19) -0.00575(19) 0.47902(18) 0.0198(5) Uani 1 1 d . . . . .
H28A H 0.131909 -0.052416 0.472373 0.030 Uiso 1 1 calc GR . . . .
H28B H 0.002127 -0.049191 0.451803 0.030 Uiso 1 1 calc GR . . . .
H28C H 0.080975 0.010599 0.548515 0.030 Uiso 1 1 calc GR . . . .
C29 C -0.03705(17) 0.1836(2) 0.42962(17) 0.0182(4) Uani 1 1 d . . . . .
H29A H -0.026747 0.204494 0.498267 0.027 Uiso 1 1 calc GR . . . .
H29B H -0.103177 0.135929 0.405236 0.027 Uiso 1 1 calc GR . . . .
H29C H -0.044706 0.254921 0.390192 0.027 Uiso 1 1 calc GR . . . .
C30 C 0.0504(2) 0.0809(2) 0.31123(17) 0.0203(5) Uani 1 1 d . . . . .
H30A H 0.044214 0.152964 0.272906 0.030 Uiso 1 1 calc GR . . . .
H30B H -0.015833 0.033895 0.285019 0.030 Uiso 1 1 calc GR . . . .
H30C H 0.114175 0.036371 0.307115 0.030 Uiso 1 1 calc GR . . . .
C31 C 0.20974(17) 0.28293(19) 0.58854(16) 0.0144(4) Uani 1 1 d . . . . .
C32 C 0.25293(18) 0.4000(2) 0.60155(17) 0.0173(4) Uani 1 1 d . . . . .
H32 H 0.273993 0.435650 0.550069 0.021 Uiso 1 1 calc R . . . .
C33 C 0.26476(19) 0.4633(2) 0.68942(18) 0.0214(5) Uani 1 1 d . . . . .
H33 H 0.294311 0.539973 0.696564 0.026 Uiso 1 1 calc R . . . .
C34 C 0.2324(2) 0.4119(2) 0.76665(17) 0.0224(5) Uani 1 1 d . . . . .
H34 H 0.239486 0.454369 0.825250 0.027 Uiso 1 1 calc R . . . .
C35 C 0.1894(2) 0.2971(2) 0.75604(18) 0.0224(5) Uani 1 1 d . . . . .
H35 H 0.167551 0.262520 0.807488 0.027 Uiso 1 1 calc R . . . .
C36 C 0.17911(18) 0.2336(2) 0.66838(17) 0.0186(4) Uani 1 1 d . . . . .
H36 H 0.151100 0.156309 0.662604 0.022 Uiso 1 1 calc R . . . .
C37 C 0.32136(18) 0.10620(19) 0.47703(17) 0.0160(4) Uani 1 1 d . . . . .
C38 C 0.3794(2) 0.1115(2) 0.40599(19) 0.0219(5) Uani 1 1 d . . . . .
H38 H 0.358681 0.167302 0.354593 0.026 Uiso 1 1 calc R . . . .
C39 C 0.4680(2) 0.0339(2) 0.4115(2) 0.0285(6) Uani 1 1 d . . . . .
H39 H 0.505964 0.038383 0.363946 0.034 Uiso 1 1 calc R . . . .
C40 C 0.4998(2) -0.0500(2) 0.4879(2) 0.0260(5) Uani 1 1 d . . . . .
H40 H 0.558662 -0.101821 0.491243 0.031 Uiso 1 1 calc R . . . .
C41 C 0.4437(2) -0.0563(2) 0.55876(19) 0.0238(5) Uani 1 1 d . . . . .
H41 H 0.465002 -0.112046 0.610155 0.029 Uiso 1 1 calc R . . . .
C42 C 0.35555(19) 0.0208(2) 0.55312(17) 0.0190(4) Uani 1 1 d . . . . .
H42 H 0.318197 0.015563 0.601091 0.023 Uiso 1 1 calc R . . . .
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
7 -1 -6 0.0301
-7 0 6 0.0184
-2 -7 0 0.0462
7 3 -5 0.0266
-3 6 4 0.0469
1 0 8 0.0086
-1 0 -8 0.0116
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
O3 Si1 C27 110.67(9) . . ?
O3 Si1 C31 107.39(9) . . ?
O3 Si1 C37 103.99(9) . . ?
C31 Si1 C27 112.45(10) . . ?
C37 Si1 C27 110.01(10) . . ?
C37 Si1 C31 111.99(9) . . ?
C25 O1 C3 113.99(19) . . ?
C26 O2 C12 113.27(17) . . ?
C24 O3 Si1 123.90(14) . . ?
H1B C1 H1A 107.5 . . ?
C2 C1 H1B 108.5 . . ?
C2 C1 H1A 108.5 . . ?
C2 C1 C10 115.17(18) . . ?
C10 C1 H1B 108.5 . . ?
C10 C1 H1A 108.5 . . ?
C1 C2 H2A 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
C3 C2 C1 110.36(19) . . ?
C3 C2 H2A 109.6 . . ?
C3 C2 H2B 109.6 . . ?
O1 C3 C2 112.80(19) . . ?
O1 C3 H3 109.1 . . ?
O1 C3 C4 106.57(18) . . ?
C2 C3 H3 109.1 . . ?
C4 C3 C2 110.18(19) . . ?
C4 C3 H3 109.1 . . ?
C3 C4 H4A 109.1 . . ?
C3 C4 H4B 109.1 . . ?
C3 C4 C5 112.30(19) . . ?
H4A C4 H4B 107.9 . . ?
C5 C4 H4A 109.1 . . ?
C5 C4 H4B 109.1 . . ?
C4 C5 H5 106.9 . . ?
C4 C5 C10 112.83(18) . . ?
C6 C5 C4 110.54(19) . . ?
C6 C5 H5 106.9 . . ?
C6 C5 C10 112.26(18) . . ?
C10 C5 H5 106.9 . . ?
C5 C6 H6A 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?
C7 C6 C5 111.79(18) . . ?
C7 C6 H6A 109.3 . . ?
C7 C6 H6B 109.3 . . ?
C6 C7 H7A 109.3 . . ?
C6 C7 H7B 109.3 . . ?
C6 C7 C8 111.47(19) . . ?
H7A C7 H7B 108.0 . . ?
C8 C7 H7A 109.3 . . ?
C8 C7 H7B 109.3 . . ?
C7 C8 H8 108.5 . . ?
C7 C8 C9 110.16(17) . . ?
C9 C8 H8 108.5 . . ?
C14 C8 C7 111.77(18) . . ?
C14 C8 H8 108.5 . . ?
C14 C8 C9 109.28(17) . . ?
C8 C9 H9 106.7 . . ?
C8 C9 C10 111.60(17) . . ?
C10 C9 H9 106.7 . . ?
C11 C9 C8 111.43(17) . . ?
C11 C9 H9 106.7 . . ?
C11 C9 C10 113.16(17) . . ?
C1 C10 C5 107.46(18) . . ?
C1 C10 C9 113.07(18) . . ?
C9 C10 C5 109.54(17) . . ?
C19 C10 C1 106.44(18) . . ?
C19 C10 C5 109.46(18) . . ?
C19 C10 C9 110.75(18) . . ?
C9 C11 H11A 108.7 . . ?
C9 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
C12 C11 C9 114.11(17) . . ?
C12 C11 H11A 108.7 . . ?
C12 C11 H11B 108.7 . . ?
O2 C12 C11 111.05(17) . . ?
O2 C12 H12 109.0 . . ?
O2 C12 C13 107.29(16) . . ?
C11 C12 H12 109.0 . . ?
C13 C12 C11 111.45(18) . . ?
C13 C12 H12 109.0 . . ?
C12 C13 C14 107.58(17) . . ?
C12 C13 C17 116.51(17) . . ?
C12 C13 C18 109.32(18) . . ?
C17 C13 C14 100.12(16) . . ?
C18 C13 C14 112.66(18) . . ?
C18 C13 C17 110.42(17) . . ?
C8 C14 C13 113.69(17) . . ?
C8 C14 H14 106.6 . . ?
C8 C14 C15 118.75(18) . . ?
C13 C14 H14 106.6 . . ?
C15 C14 C13 103.74(17) . . ?
C15 C14 H14 106.6 . . ?
C14 C15 H15A 111.0 . . ?
C14 C15 H15B 111.0 . . ?
C14 C15 C16 103.98(18) . . ?
H15A C15 H15B 109.0 . . ?
C16 C15 H15A 111.0 . . ?
C16 C15 H15B 111.0 . . ?
C15 C16 H16A 110.4 . . ?
C15 C16 H16B 110.4 . . ?
H16A C16 H16B 108.6 . . ?
C17 C16 C15 106.72(18) . . ?
C17 C16 H16A 110.4 . . ?
C17 C16 H16B 110.4 . . ?
C13 C17 H17 107.0 . . ?
C16 C17 C13 103.35(17) . . ?
C16 C17 H17 107.0 . . ?
C20 C17 C13 119.00(18) . . ?
C20 C17 C16 112.76(17) . . ?
C20 C17 H17 107.0 . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C10 C19 H19A 109.5 . . ?
C10 C19 H19B 109.5 . . ?
C10 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20 107.6 . . ?
C21 C20 C17 113.69(18) . . ?
C21 C20 H20 107.6 . . ?
C21 C20 C22 109.68(18) . . ?
C22 C20 C17 110.52(18) . . ?
C22 C20 H20 107.6 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 108.7 . . ?
C20 C22 H22B 108.7 . . ?
H22A C22 H22B 107.6 . . ?
C23 C22 C20 114.32(18) . . ?
C23 C22 H22A 108.7 . . ?
C23 C22 H22B 108.7 . . ?
C22 C23 H23A 109.4 . . ?
C22 C23 H23B 109.4 . . ?
H23A C23 H23B 108.0 . . ?
C24 C23 C22 111.19(18) . . ?
C24 C23 H23A 109.4 . . ?
C24 C23 H23B 109.4 . . ?
O3 C24 C23 110.08(18) . . ?
O3 C24 H24A 109.6 . . ?
O3 C24 H24B 109.6 . . ?
C23 C24 H24A 109.6 . . ?
C23 C24 H24B 109.6 . . ?
H24A C24 H24B 108.2 . . ?
O1 C25 H25A 109.5 . . ?
O1 C25 H25B 109.5 . . ?
O1 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O2 C26 H26A 109.5 . . ?
O2 C26 H26B 109.5 . . ?
O2 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 Si1 112.73(15) . . ?
C28 C27 C30 107.28(18) . . ?
C29 C27 Si1 111.40(14) . . ?
C29 C27 C28 108.76(18) . . ?
C29 C27 C30 110.04(18) . . ?
C30 C27 Si1 106.50(14) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 Si1 118.82(17) . . ?
C36 C31 Si1 124.35(17) . . ?
C36 C31 C32 116.8(2) . . ?
C31 C32 H32 119.2 . . ?
C33 C32 C31 121.6(2) . . ?
C33 C32 H32 119.2 . . ?
C32 C33 H33 120.0 . . ?
C34 C33 C32 119.9(2) . . ?
C34 C33 H33 120.0 . . ?
C33 C34 H34 120.1 . . ?
C35 C34 C33 119.8(2) . . ?
C35 C34 H34 120.1 . . ?
C34 C35 H35 120.0 . . ?
C34 C35 C36 120.0(2) . . ?
C36 C35 H35 120.0 . . ?
C31 C36 H36 119.1 . . ?
C35 C36 C31 121.8(2) . . ?
C35 C36 H36 119.1 . . ?
C38 C37 Si1 121.64(17) . . ?
C42 C37 Si1 120.64(17) . . ?
C42 C37 C38 117.6(2) . . ?
C37 C38 H38 119.6 . . ?
C39 C38 C37 120.7(2) . . ?
C39 C38 H38 119.6 . . ?
C38 C39 H39 119.9 . . ?
C40 C39 C38 120.3(2) . . ?
C40 C39 H39 119.9 . . ?
C39 C40 H40 120.1 . . ?
C41 C40 C39 119.8(2) . . ?
C41 C40 H40 120.1 . . ?
C40 C41 H41 120.1 . . ?
C40 C41 C42 119.9(2) . . ?
C42 C41 H41 120.1 . . ?
C37 C42 H42 119.2 . . ?
C41 C42 C37 121.7(2) . . ?
C41 C42 H42 119.2 . . ?
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
Si1 O3 1.6467(15) . ?
Si1 C27 1.897(2) . ?
Si1 C31 1.882(2) . ?
Si1 C37 1.866(2) . ?
O1 C3 1.433(3) . ?
O1 C25 1.410(3) . ?
O2 C12 1.433(2) . ?
O2 C26 1.418(3) . ?
O3 C24 1.431(3) . ?
C1 H1B 0.9700 . ?
C1 H1A 0.9700 . ?
C1 C2 1.527(3) . ?
C1 C10 1.545(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.524(3) . ?
C3 H3 0.9800 . ?
C3 C4 1.515(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.540(3) . ?
C5 H5 0.9800 . ?
C5 C6 1.533(3) . ?
C5 C10 1.556(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.531(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.534(3) . ?
C8 H8 0.9800 . ?
C8 C9 1.551(3) . ?
C8 C14 1.520(3) . ?
C9 H9 0.9800 . ?
C9 C10 1.557(3) . ?
C9 C11 1.542(3) . ?
C10 C19 1.539(3) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.537(3) . ?
C12 H12 0.9800 . ?
C12 C13 1.536(3) . ?
C13 C14 1.551(3) . ?
C13 C17 1.552(3) . ?
C13 C18 1.541(3) . ?
C14 H14 0.9800 . ?
C14 C15 1.528(3) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.556(3) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.551(3) . ?
C17 H17 0.9800 . ?
C17 C20 1.540(3) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20 0.9800 . ?
C20 C21 1.536(3) . ?
C20 C22 1.540(3) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.528(3) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.507(3) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 C28 1.539(3) . ?
C27 C29 1.536(3) . ?
C27 C30 1.547(3) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C32 1.411(3) . ?
C31 C36 1.401(3) . ?
C32 H32 0.9300 . ?
C32 C33 1.390(3) . ?
C33 H33 0.9300 . ?
C33 C34 1.391(4) . ?
C34 H34 0.9300 . ?
C34 C35 1.386(4) . ?
C35 H35 0.9300 . ?
C35 C36 1.391(3) . ?
C36 H36 0.9300 . ?
C37 C38 1.401(3) . ?
C37 C42 1.401(3) . ?
C38 H38 0.9300 . ?
C38 C39 1.397(3) . ?
C39 H39 0.9300 . ?
C39 C40 1.390(4) . ?
C40 H40 0.9300 . ?
C40 C41 1.381(4) . ?
C41 H41 0.9300 . ?
C41 C42 1.388(3) . ?
C42 H42 0.9300 . ?
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
7.0000 -1.0000 -6.0000 0.0229 -0.2364 -0.9361
-7.0000 -0.0000 6.0000 0.0065 0.1029 0.9503
-2.0000 -7.0000 0.0000 0.0339 -0.9517 0.2898
7.0000 3.0000 -5.0000 0.0067 0.3248 -0.9456
-3.0000 6.0000 4.0000 -0.0288 0.8840 0.3897
1.0000 -0.0000 8.0000 0.8983 0.2287 0.2838
-1.0000 0.0000 -8.0000 -0.8983 -0.2287 -0.2838
