#------------------------------------------------------------------------------
#$Date: 2022-02-03 22:36:55 +0200 (Thu, 03 Feb 2022) $
#$Revision: 272458 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/92/4519288.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_4519288
loop_
_publ_author_name
'Fang, Xiaowu'
'Wen, Songwei'
'Jin, Peishen'
'Bao, Wenjing'
'Liu, Shanshan'
'Cong, Hengjiang'
'Shen, Xiao'
_publ_section_title
;
 Synthesis of Enantioenriched Fluorinated Enol Silanes Enabled by
 Asymmetric Reductive Coupling of Fluoroalkylacylsilanes and 1,3-Enynes
 and Brook Rearrangement
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              2150
_journal_page_last               2157
_journal_paper_doi               10.1021/acscatal.2c00100
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C20 H21 F2 N O3 Si'
_chemical_formula_sum            'C20 H21 F2 N O3 Si'
_chemical_formula_weight         389.47
_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             2019-12-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                97.232(4)
_cell_angle_beta                 97.041(5)
_cell_angle_gamma                109.612(6)
_cell_formula_units_Z            4
_cell_length_a                   9.1912(7)
_cell_length_b                   12.9247(8)
_cell_length_c                   18.6126(5)
_cell_measurement_reflns_used    6505
_cell_measurement_temperature    274(30)
_cell_measurement_theta_max      57.9010
_cell_measurement_theta_min      3.6310
_cell_volume                     2033.8(2)
_computing_cell_refinement
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_computing_data_collection
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_computing_data_reduction
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_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      air
_diffrn_ambient_temperature      274(30)
_diffrn_detector                 'Hybrid Pixel Counting (HPC) detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HyPix-6000HE'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -84.00  42.00   0.50    2.33    --    5.00 -38.00 120.00  252
  2  ω   -136.00 -13.00   0.50    2.33    --  -46.70 -57.00  60.00  246
  3  ω    -80.00  43.00   0.50    2.33    --  -46.70  57.00 -60.00  246
  4  ω   -136.00  -8.00   0.50    2.33    --  -46.70 -76.00 -30.00  256
  5  ω   -136.00  -8.00   0.50    2.33    --  -46.70 -76.00 120.00  256
  6  ω   -136.00  -8.00   0.50    2.33    --  -46.70 -76.00-120.00  256
  7  ω   -153.00 -26.00   0.50    2.33    --  -64.00 -75.00-146.78  254
  8  ω   -157.00 -30.00   0.50    2.33    --  -68.00 -76.00  84.65  254
  9  ω   -161.00 -34.00   0.50    2.33    --  -72.00 -74.00 -15.57  254
 10  ω   -161.00 -34.00   0.50    2.33    --  -72.00 -76.00 131.97  254
 11  ω   -165.00 -38.00   0.50    9.33    --  -76.00 -76.00  67.89  254
 12  ω   -165.00 -38.00   0.50    9.33    --  -76.00 -74.00 -43.44  254
 13  ω   -165.00 -38.00   0.50    9.33    --  -76.00 -76.00 -61.66  254
 14  ω   -165.00 -39.00   0.50    9.33    --  -76.00 -73.00-165.74  252
 15  ω   -165.00 -38.00   0.50    9.33    --  -76.00 -75.00 160.01  254
 16  ω   -169.00 -42.00   0.50    9.33    --  -80.00 -76.00 108.76  254
 17  ω   -169.00 -42.00   0.50    9.33    --  -80.00 -75.00  41.05  254
 18  ω   -177.00 -53.00   0.50    9.33    --  -88.00 -66.00  79.87  248
 19  ω   -177.00 -54.00   0.50    9.33    --  -88.00 -62.00 156.11  246
 20  ω   -177.00 -51.00   0.50    9.33    --  -88.00 -73.00 172.70  252
 21  ω   -177.00 -54.00   0.50    9.33    --  -88.00 -65.00  98.90  246
 22  ω   -177.00 -52.00   0.50    9.33    --  -88.00 -70.00 -55.19  250
 23  ω   -177.00 -51.00   0.50    9.33    --  -88.00 -72.00 -78.99  252
 24  ω   -177.00 -51.00   0.50    9.33    --  -88.00 -72.00-101.58  252
 25  ω   -177.00 -52.00   0.50    9.33    --  -88.00 -70.00  19.62  250
 26  ω   -177.00 -51.00   0.50    9.33    --  -88.00 -72.00-101.58  252
 27  ω   -181.00 -54.00   0.50    9.33    --  -92.00 -75.00 -21.11  254
 28  ω   -181.00 -58.00   0.50    9.33    --  -92.00 -63.00-132.19  246
 29  ω   -181.00 -54.00   0.50    9.33    --  -92.00 -75.00 148.18  254
 30  ω   -181.00 -54.00   0.50    9.33    --  -92.00 -76.00-145.79  254
 31  ω   -136.00  -8.00   0.50    9.33    --  -97.30  76.00 -30.00  256
 32  ω   -187.00 -64.00   0.50    9.33    --  -97.30 -57.00  60.00  246
 33  ω   -136.00  -8.00   0.50    9.33    --  -97.30  76.00 150.00  256
 34  ω   -186.00 -59.00   0.50    9.33    --  -97.30 -76.00   0.00  254
 35  ω    -94.00 -40.00   0.50    9.33    --  -97.30  76.00-150.00  108
 36  ω    -76.00 -24.00   0.50    9.33    --  -97.30  76.00 -90.00  104
 37  ω   -133.00 -82.00   0.50    9.33    --  -97.30  76.00 -90.00  102
 38  ω   -128.00-101.00   0.50    9.33    --  -97.30  76.00-150.00   54
 39  ω    -36.00  -8.00   0.50    9.33    --  -97.30  76.00  60.00   56
 40  ω   -135.00 -42.00   0.50    9.33    --  -97.30  76.00  60.00  186
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       'profile data from ω-scans and φ-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1800136000
_diffrn_orient_matrix_UB_12      0.0490773000
_diffrn_orient_matrix_UB_13      0.0080018000
_diffrn_orient_matrix_UB_21      0.0159978000
_diffrn_orient_matrix_UB_22      -0.0037842000
_diffrn_orient_matrix_UB_23      0.0829055000
_diffrn_orient_matrix_UB_31      0.0040767000
_diffrn_orient_matrix_UB_32      -0.1188124000
_diffrn_orient_matrix_UB_33      -0.0157267000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'VariMax VHF'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.3016
_diffrn_reflns_av_unetI/netI     0.1546
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            54460
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        64.998
_diffrn_reflns_theta_max         64.998
_diffrn_reflns_theta_min         2.431
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku MicroMax-007HF'
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    1.350
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48643
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.272
_exptl_crystal_description       plate
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.05(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     894
_refine_ls_number_reflns         13203
_refine_ls_number_restraints     675
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.2528
_refine_ls_R_factor_gt           0.1285
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3256
_refine_ls_wR_factor_ref         0.4322
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                5193
_reflns_number_total             13203
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cs2c00100_si_002.cif
_cod_data_source_block           wensongwei-wsw-4-74-250k-191223
_cod_database_code               4519288
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C78 H90 F3 N7 O16 Si4 '
_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   0.974
_shelx_estimated_absorpt_t_min   0.948
_reflns_odcompleteness_completeness 98.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.05(11)
 -0.05(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3. Uiso/Uaniso restraints and constraints
C68 \\sim C67 \\sim C66 \\sim C65 \\sim C64 \\sim C63 \\sim C62 \\sim C61:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C4 \\sim C3 \\sim C2 \\sim C1 \\sim C6 \\sim C5: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
F7 \\sim C72 \\sim F8: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 C49(H49), C69(H69), C52(H52), C29(H29), C32(H32), C12(H12), C9(H9), C72(H72)
4.b Aromatic/amide H refined with riding coordinates:
 C46(H46), C45(H45), C43(H43), C42(H42), C79(H79), C80(H80), C76(H76),
 C77(H77), C78(H78), C3(H3A), C2(H2), C6(H6), C5(H5), C22(H22), C23(H23),
 C25(H25), C26(H26), C40(H40), C39(H39), C38(H38), C37(H37), C36(H36), C20(H20),
  C19(H19), C18(H18), C17(H17), C16(H16), C66(H66), C65(H65), C63(H63),
 C62(H62), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60)
4.c Fitted hexagon refined as free rotating group:
 C41(C46,C45,C44,C43,C42), C79(C80,C75,C76,C77,C78), C4(C3,C2,C1,C6,C5),
 C21(C22,C23,C24,C25,C26), C35(C40,C39,C38,C37,C36), C15(C20,C19,C18,C17,C16),
 C66(C65,C64,C63,C62,C61), C55(C56,C57,C58,C59,C60)
4.d Idealised Me refined as rotating group:
 C73(H73A,H73B,H73C), C30(H30A,H30B,H30C), C54(H54A,H54B,H54C), C33(H33A,H33B,
 H33C), C34(H34A,H34B,H34C), C10(H10A,H10B,H10C), C50(H50A,H50B,H50C), C53(H53A,
 H53B,H53C), C70(H70A,H70B,H70C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C),
 C74(H74A,H74B,H74C)
4.e Idealised tetrahedral OH refined as rotating group:
 O3(H3), O6(H6A), O9(H9A), O12(H12A)
;
_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 5.280
_oxdiff_exptl_absorpt_empirical_full_min 0.168
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
Si1 Si 0.1232(7) 0.4773(5) 0.0346(3) 0.0851(16) Uani 1 1 d . U . . .
Si4 Si 0.6192(6) -0.0547(5) 0.9633(3) 0.0799(16) Uani 1 1 d . U . . .
Si3 Si 0.2926(7) 1.0582(5) 0.6048(4) 0.0903(18) Uani 1 1 d . U . . .
Si2 Si 0.6490(8) 0.5599(6) 0.3940(4) 0.0978(19) Uani 1 1 d . U . . .
F6 F 0.470(2) 1.1253(15) 0.7592(8) 0.139(5) Uani 1 1 d . U . . .
O3 O -0.1527(18) 0.3797(12) 0.0738(10) 0.102(4) Uani 1 1 d . U . . .
H3 H -0.228424 0.379697 0.092898 0.153 Uiso 1 1 calc GR . . . .
C47 C 0.368(3) 0.775(2) 0.6023(12) 0.081(5) Uani 1 1 d . U . . .
O6 O 0.6813(18) 0.7686(15) 0.3837(11) 0.118(5) Uani 1 1 d . U . . .
H6A H 0.654104 0.819769 0.372814 0.177 Uiso 1 1 calc GR . . . .
O8 O -0.030(2) 0.2927(15) 0.6459(13) 0.134(7) Uani 1 1 d . U . . .
F2 F 0.108(2) 0.4524(13) 0.1928(8) 0.132(5) Uani 1 1 d . U . . .
N1 N 1.457(3) 0.4451(17) 0.8519(15) 0.107(6) Uani 1 1 d . U . . .
O11 O 1.571(3) 0.4907(15) 0.9000(13) 0.130(6) Uani 1 1 d . U . . .
N2 N -0.058(3) 0.3406(17) 0.5968(16) 0.110(6) Uani 1 1 d . U . . .
O9 O 0.5933(19) 1.1778(13) 0.6288(10) 0.112(5) Uani 1 1 d . U . . .
H9A H 0.687889 1.191813 0.640267 0.168 Uiso 1 1 calc GR . . . .
C41 C 0.0567(16) 0.4493(10) 0.5988(8) 0.087(6) Uani 1 1 d . U . . .
C46 C 0.2030(18) 0.4884(11) 0.6439(8) 0.105(7) Uani 1 1 d G U . . .
H46 H 0.231482 0.442750 0.673320 0.126 Uiso 1 1 calc R . . . .
C45 C 0.3069(14) 0.5957(12) 0.6452(8) 0.096(7) Uani 1 1 d G U . . .
H45 H 0.404862 0.621807 0.675460 0.115 Uiso 1 1 calc R . . . .
C44 C 0.2644(16) 0.6639(9) 0.6013(8) 0.082(5) Uani 1 1 d G U . . .
C43 C 0.1181(18) 0.6248(12) 0.5561(8) 0.109(7) Uani 1 1 d G U . . .
H43 H 0.089623 0.670456 0.526745 0.131 Uiso 1 1 calc R . . . .
C42 C 0.0142(13) 0.5175(13) 0.5548(8) 0.100(7) Uani 1 1 d G U . . .
H42 H -0.083760 0.491400 0.524604 0.120 Uiso 1 1 calc R . . . .
C48 C 0.448(3) 0.8632(19) 0.5958(11) 0.075(5) Uani 1 1 d . U . . .
C49 C 0.555(2) 0.9835(18) 0.5930(12) 0.086(6) Uani 1 1 d . U . . .
H49 H 0.538737 0.995494 0.542155 0.103 Uiso 1 1 calc R . . . .
C68 C 0.956(3) -0.0507(19) 0.9095(12) 0.087(5) Uani 1 1 d . U . . .
F1 F -0.091(2) 0.4960(16) 0.2118(9) 0.151(6) Uani 1 1 d . U . . .
O12 O 0.5707(15) -0.2697(11) 0.9224(9) 0.089(4) Uani 1 1 d . U . . .
H12A H 0.609753 -0.318054 0.917916 0.133 Uiso 1 1 calc GR . . . .
C79 C 0.775(2) -0.1001(14) 1.1721(8) 0.108(7) Uani 1 1 d . U . . .
H79 H 0.758468 -0.159381 1.197600 0.129 Uiso 1 1 calc R . . . .
C80 C 0.7021(17) -0.1184(10) 1.0993(8) 0.090(6) Uani 1 1 d G U . . .
H80 H 0.636667 -0.189866 1.076089 0.108 Uiso 1 1 calc R . . . .
C75 C 0.7269(15) -0.0298(12) 1.0613(6) 0.077(5) Uani 1 1 d G U . . .
C76 C 0.8247(17) 0.0770(11) 1.0961(9) 0.093(6) Uani 1 1 d G U . . .
H76 H 0.841257 0.136249 1.070597 0.112 Uiso 1 1 calc R . . . .
C77 C 0.8976(17) 0.0953(12) 1.1689(9) 0.106(7) Uani 1 1 d G U . . .
H77 H 0.963060 0.166737 1.192108 0.127 Uiso 1 1 calc R . . . .
C78 C 0.8728(19) 0.0067(17) 1.2069(6) 0.115(8) Uani 1 1 d G U . . .
H78 H 0.921667 0.018923 1.255611 0.138 Uiso 1 1 calc R . . . .
C11 C -0.037(3) 0.488(2) 0.0908(13) 0.102(7) Uani 1 1 d . U . . .
F3 F 0.589(2) 0.6163(15) 0.2450(8) 0.144(6) Uani 1 1 d . U . . .
C69 C 0.844(2) -0.1578(17) 0.9248(13) 0.088(6) Uani 1 1 d . U . . .
H69 H 0.864385 -0.153700 0.978214 0.105 Uiso 1 1 calc R . . . .
C4 C 0.2010(12) 0.8980(8) 0.1254(7) 0.074(4) Uani 1 1 d . U . . .
C3 C 0.3527(13) 0.9224(9) 0.1625(7) 0.076(4) Uani 1 1 d G U . . .
H3A H 0.381256 0.866533 0.180120 0.092 Uiso 1 1 calc R . . . .
C2 C 0.4615(11) 1.0304(10) 0.1733(7) 0.080(4) Uani 1 1 d G U . . .
H2 H 0.562964 1.046754 0.198070 0.096 Uiso 1 1 calc R . . . .
C1 C 0.4188(13) 1.1140(8) 0.1469(8) 0.076(4) Uani 1 1 d G U . . .
C6 C 0.2672(14) 1.0896(9) 0.1099(7) 0.079(4) Uani 1 1 d G U . . .
H6 H 0.238561 1.145503 0.092237 0.095 Uiso 1 1 calc R . . . .
C5 C 0.1583(11) 0.9816(10) 0.0991(7) 0.079(4) Uani 1 1 d G U . . .
H5 H 0.056850 0.965281 0.074286 0.094 Uiso 1 1 calc R . . . .
F5 F 0.6873(19) 1.0993(16) 0.7506(8) 0.141(5) Uani 1 1 d . U . . .
C21 C -0.1363(18) 0.1552(10) 0.3929(9) 0.093(6) Uani 1 1 d . U . . .
C22 C 0.006(2) 0.1896(12) 0.4408(8) 0.118(8) Uani 1 1 d G U . . .
H22 H 0.025886 0.143254 0.472030 0.141 Uiso 1 1 calc R . . . .
C23 C 0.1194(16) 0.2934(13) 0.4420(8) 0.106(7) Uani 1 1 d G U . . .
H23 H 0.214827 0.316462 0.474017 0.127 Uiso 1 1 calc R . . . .
C24 C 0.0901(16) 0.3627(10) 0.3953(8) 0.082(5) Uani 1 1 d G U . . .
C25 C -0.0525(18) 0.3283(12) 0.3474(8) 0.097(6) Uani 1 1 d G U . . .
H25 H -0.072135 0.374629 0.316106 0.116 Uiso 1 1 calc R . . . .
C26 C -0.1657(15) 0.2245(12) 0.3462(8) 0.099(7) Uani 1 1 d G U . . .
H26 H -0.261077 0.201421 0.314118 0.119 Uiso 1 1 calc R . . . .
C73 C 0.400(2) -0.109(2) 0.9616(13) 0.102(7) Uani 1 1 d . U . . .
H73A H 0.368631 -0.183604 0.972505 0.153 Uiso 1 1 calc GR . . . .
H73B H 0.346578 -0.110889 0.913636 0.153 Uiso 1 1 calc GR . . . .
H73C H 0.374618 -0.061616 0.997652 0.153 Uiso 1 1 calc GR . . . .
C31 C 0.551(3) 0.667(2) 0.3653(13) 0.101(7) Uani 1 1 d . U . . .
C52 C 0.533(3) 1.061(2) 0.7196(14) 0.109(7) Uani 1 1 d . U . . .
H52 H 0.485224 0.983737 0.726073 0.131 Uiso 1 1 calc R . . . .
C67 C 1.047(2) 0.0293(18) 0.8966(12) 0.083(5) Uani 1 1 d . U . . .
C29 C 0.423(3) 0.673(2) 0.4104(12) 0.096(7) Uani 1 1 d . U . . .
H29 H 0.475614 0.696265 0.461875 0.115 Uiso 1 1 calc R . . . .
C30 C 0.347(3) 0.759(2) 0.3959(14) 0.103(7) Uani 1 1 d . U . . .
H30A H 0.426196 0.827709 0.391762 0.155 Uiso 1 1 calc GR . . . .
H30B H 0.294880 0.772340 0.435965 0.155 Uiso 1 1 calc GR . . . .
H30C H 0.271610 0.731210 0.351013 0.155 Uiso 1 1 calc GR . . . .
C54 C 0.143(3) 0.948(2) 0.6418(15) 0.118(8) Uani 1 1 d . U . . .
H54A H 0.040389 0.949530 0.625781 0.176 Uiso 1 1 calc GR . . . .
H54B H 0.166662 0.963484 0.694613 0.176 Uiso 1 1 calc GR . . . .
H54C H 0.146083 0.876310 0.623957 0.176 Uiso 1 1 calc GR . . . .
C7 C 0.094(3) 0.784(2) 0.1068(14) 0.098(7) Uani 1 1 d . U . . .
C35 C 0.6561(19) 0.5657(15) 0.4968(7) 0.096(6) Uani 1 1 d . U . . .
C40 C 0.7333(18) 0.6663(12) 0.5451(9) 0.098(6) Uani 1 1 d G U . . .
H40 H 0.773591 0.731953 0.526852 0.117 Uiso 1 1 calc R . . . .
C39 C 0.750(2) 0.6687(14) 0.6206(8) 0.117(8) Uani 1 1 d G U . . .
H39 H 0.802178 0.736002 0.652874 0.140 Uiso 1 1 calc R . . . .
C38 C 0.690(2) 0.5705(18) 0.6478(7) 0.115(8) Uani 1 1 d G U . . .
H38 H 0.701785 0.572140 0.698310 0.138 Uiso 1 1 calc R . . . .
C37 C 0.613(2) 0.4699(14) 0.5995(11) 0.118(8) Uani 1 1 d G U . . .
H37 H 0.572803 0.404228 0.617725 0.142 Uiso 1 1 calc R . . . .
C36 C 0.5959(19) 0.4675(12) 0.5240(10) 0.114(8) Uani 1 1 d G U . . .
H36 H 0.544215 0.400176 0.491702 0.136 Uiso 1 1 calc R . . . .
F4 F 0.456(2) 0.7251(16) 0.2589(9) 0.158(6) Uani 1 1 d . U . . .
C15 C 0.0478(19) 0.4802(13) -0.0641(7) 0.086(6) Uani 1 1 d . U . . .
C20 C -0.0933(19) 0.4001(13) -0.1013(10) 0.109(7) Uani 1 1 d G U . . .
H20 H -0.153384 0.347068 -0.076933 0.131 Uiso 1 1 calc R . . . .
C19 C -0.145(2) 0.3992(17) -0.1748(10) 0.139(9) Uani 1 1 d G U . . .
H19 H -0.239147 0.345605 -0.199723 0.167 Uiso 1 1 calc R . . . .
C18 C -0.055(3) 0.478(2) -0.2112(7) 0.146(10) Uani 1 1 d G U . . .
H18 H -0.089340 0.477870 -0.260425 0.176 Uiso 1 1 calc R . . . .
C17 C 0.086(3) 0.5586(16) -0.1740(9) 0.133(9) Uani 1 1 d G U . . .
H17 H 0.146232 0.611602 -0.198339 0.159 Uiso 1 1 calc R . . . .
C16 C 0.1376(18) 0.5595(12) -0.1004(9) 0.105(7) Uani 1 1 d G U . . .
H16 H 0.231999 0.613067 -0.075549 0.126 Uiso 1 1 calc R . . . .
O7 O -0.171(3) 0.3049(17) 0.5471(15) 0.147(8) Uani 1 1 d . U . . .
O10 O 1.425(2) 0.4815(17) 0.7992(13) 0.149(8) Uani 1 1 d . U . . .
C66 C 1.1993(15) 0.2937(10) 0.8258(7) 0.085(5) Uani 1 1 d . U . . .
H66 H 1.163570 0.334413 0.794720 0.102 Uiso 1 1 calc R . . . .
C65 C 1.0973(12) 0.1918(10) 0.8364(7) 0.088(5) Uani 1 1 d G U . . .
H65 H 0.993388 0.164468 0.812437 0.106 Uiso 1 1 calc R . . . .
C64 C 1.1506(13) 0.1309(9) 0.8828(7) 0.074(4) Uani 1 1 d G U . . .
C63 C 1.3059(14) 0.1718(10) 0.9186(7) 0.082(4) Uani 1 1 d G U . . .
H63 H 1.341603 0.131099 0.949595 0.099 Uiso 1 1 calc R . . . .
C62 C 1.4079(11) 0.2737(10) 0.9079(7) 0.081(4) Uani 1 1 d G U . . .
H62 H 1.511786 0.301043 0.931878 0.097 Uiso 1 1 calc R . . . .
C61 C 1.3546(14) 0.3346(8) 0.8615(8) 0.087(5) Uani 1 1 d G U . . .
C32 C 0.485(3) 0.636(2) 0.2843(13) 0.112(8) Uani 1 1 d . U . . .
H32 H 0.387639 0.570380 0.274837 0.134 Uiso 1 1 calc R . . . .
F7 F 0.627(2) -0.2579(16) 0.7808(9) 0.151(6) Uani 1 1 d . U . . .
C12 C 0.030(4) 0.518(2) 0.1732(15) 0.124(9) Uani 1 1 d . U . . .
H12 H 0.097663 0.596792 0.186508 0.149 Uiso 1 1 calc R . . . .
C9 C -0.113(3) 0.5742(19) 0.0659(14) 0.095(6) Uani 1 1 d . U . . .
H9 H -0.135910 0.558193 0.011950 0.113 Uiso 1 1 calc R . . . .
C33 C 0.854(3) 0.613(3) 0.3763(16) 0.124(9) Uani 1 1 d . U . . .
H33A H 0.851868 0.609165 0.324334 0.186 Uiso 1 1 calc GR . . . .
H33B H 0.909347 0.567866 0.394343 0.186 Uiso 1 1 calc GR . . . .
H33C H 0.904937 0.688863 0.401010 0.186 Uiso 1 1 calc GR . . . .
C55 C 0.2586(19) 1.0263(14) 0.5006(7) 0.091(6) Uani 1 1 d . U . . .
C56 C 0.1243(19) 0.9423(13) 0.4604(11) 0.117(8) Uani 1 1 d G U . . .
H56 H 0.053547 0.895710 0.484610 0.140 Uiso 1 1 calc R . . . .
C57 C 0.096(2) 0.9279(15) 0.3841(11) 0.134(9) Uani 1 1 d G U . . .
H57 H 0.005851 0.871655 0.357179 0.161 Uiso 1 1 calc R . . . .
C58 C 0.201(3) 0.997(2) 0.3479(7) 0.143(10) Uani 1 1 d G U . . .
H58 H 0.182322 0.987831 0.296850 0.171 Uiso 1 1 calc R . . . .
C59 C 0.336(2) 1.0815(19) 0.3881(9) 0.143(10) Uani 1 1 d G U . . .
H59 H 0.406492 1.128062 0.363953 0.171 Uiso 1 1 calc R . . . .
C60 C 0.3643(17) 1.0959(14) 0.4645(9) 0.111(8) Uani 1 1 d G U . . .
H60 H 0.454191 1.152118 0.491385 0.133 Uiso 1 1 calc R . . . .
C51 C 0.508(3) 1.066(2) 0.6404(12) 0.102(7) Uani 1 1 d . U . . .
C34 C 0.538(3) 0.418(3) 0.3384(17) 0.140(10) Uani 1 1 d . U . . .
H34A H 0.427723 0.400279 0.338509 0.209 Uiso 1 1 calc GR . . . .
H34B H 0.571826 0.364167 0.359391 0.209 Uiso 1 1 calc GR . . . .
H34C H 0.556844 0.417102 0.288819 0.209 Uiso 1 1 calc GR . . . .
C8 C 0.002(3) 0.689(3) 0.0871(13) 0.099(7) Uani 1 1 d . U . . .
C10 C -0.267(3) 0.5722(17) 0.0919(16) 0.112(8) Uani 1 1 d . U . . .
H10A H -0.342962 0.497723 0.079076 0.168 Uiso 1 1 calc GR . . . .
H10B H -0.306537 0.621753 0.068396 0.168 Uiso 1 1 calc GR . . . .
H10C H -0.246975 0.595853 0.144251 0.168 Uiso 1 1 calc GR . . . .
C50 C 0.727(2) 0.989(2) 0.6136(15) 0.109(8) Uani 1 1 d . U . . .
H50A H 0.742847 0.972545 0.662076 0.163 Uiso 1 1 calc GR . . . .
H50B H 0.797286 1.063108 0.612648 0.163 Uiso 1 1 calc GR . . . .
H50C H 0.745928 0.936172 0.578852 0.163 Uiso 1 1 calc GR . . . .
C53 C 0.275(3) 1.199(2) 0.6382(16) 0.123(9) Uani 1 1 d . U . . .
H53A H 0.171744 1.197187 0.618975 0.184 Uiso 1 1 calc GR . . . .
H53B H 0.351930 1.257143 0.621299 0.184 Uiso 1 1 calc GR . . . .
H53C H 0.291281 1.213694 0.690960 0.184 Uiso 1 1 calc GR . . . .
C70 C 0.892(3) -0.2557(19) 0.8903(16) 0.111(8) Uani 1 1 d . U . . .
H70A H 0.893568 -0.254178 0.838985 0.166 Uiso 1 1 calc GR . . . .
H70B H 0.817078 -0.325577 0.895823 0.166 Uiso 1 1 calc GR . . . .
H70C H 0.994163 -0.247640 0.914940 0.166 Uiso 1 1 calc GR . . . .
C27 C 0.201(3) 0.471(2) 0.3980(13) 0.091(6) Uani 1 1 d . U . . .
C14 C 0.313(2) 0.595(2) 0.0682(14) 0.113(8) Uani 1 1 d . U . . .
H14A H 0.314003 0.657025 0.044512 0.170 Uiso 1 1 calc GR . . . .
H14B H 0.397931 0.571666 0.056949 0.170 Uiso 1 1 calc GR . . . .
H14C H 0.326143 0.617283 0.120468 0.170 Uiso 1 1 calc GR . . . .
C13 C 0.144(3) 0.339(2) 0.0403(14) 0.122(9) Uani 1 1 d . U . . .
H13A H 0.118407 0.317259 0.086012 0.183 Uiso 1 1 calc GR . . . .
H13B H 0.250378 0.344988 0.037883 0.183 Uiso 1 1 calc GR . . . .
H13C H 0.074453 0.283732 0.000100 0.183 Uiso 1 1 calc GR . . . .
C28 C 0.303(3) 0.557(3) 0.4053(12) 0.103(7) Uani 1 1 d . U . . .
C74 C 0.677(3) 0.080(2) 0.9296(12) 0.099(7) Uani 1 1 d . U . . .
H74A H 0.658903 0.134800 0.963400 0.148 Uiso 1 1 calc GR . . . .
H74B H 0.614803 0.070089 0.882088 0.148 Uiso 1 1 calc GR . . . .
H74C H 0.785687 0.103490 0.925767 0.148 Uiso 1 1 calc GR . . . .
F8 F 0.4804(17) -0.1626(13) 0.8073(7) 0.121(4) Uani 1 1 d . U . . .
O1 O 0.652(2) 1.2497(15) 0.1941(12) 0.128(6) Uani 1 1 d . U . . .
O4 O -0.360(3) 0.0104(19) 0.3445(14) 0.165(10) Uani 1 1 d . U . . .
N3 N -0.253(3) 0.0501(18) 0.3939(16) 0.114(7) Uani 1 1 d . U . . .
N4 N 0.530(2) 1.2225(17) 0.1528(13) 0.100(6) Uani 1 1 d . U . . .
O5 O -0.233(3) 0.0041(17) 0.4454(15) 0.163(9) Uani 1 1 d . U . . .
O2 O 0.508(2) 1.2842(15) 0.1155(13) 0.151(9) Uani 1 1 d . U . . .
C71 C 0.672(2) -0.1703(15) 0.9043(10) 0.074(5) Uani 1 1 d . U . . .
C72 C 0.634(4) -0.160(3) 0.8221(15) 0.123(7) Uani 1 1 d . U . . .
H72 H 0.709667 -0.094065 0.809432 0.148 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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C15 Si1 C11 106.9(9) . . ?
C14 Si1 C11 112.1(11) . . ?
C14 Si1 C15 109.5(10) . . ?
C14 Si1 C13 111.6(13) . . ?
C13 Si1 C11 107.2(11) . . ?
C13 Si1 C15 109.4(10) . . ?
C75 Si4 C71 107.8(7) . . ?
C73 Si4 C75 109.7(8) . . ?
C73 Si4 C71 108.0(10) . . ?
C74 Si4 C75 108.5(9) . . ?
C74 Si4 C73 109.6(11) . . ?
C74 Si4 C71 113.2(10) . . ?
C54 Si3 C55 110.9(10) . . ?
C54 Si3 C51 111.4(10) . . ?
C54 Si3 C53 107.7(13) . . ?
C55 Si3 C51 107.2(9) . . ?
C55 Si3 C53 110.6(10) . . ?
C53 Si3 C51 109.1(12) . . ?
C35 Si2 C31 107.0(9) . . ?
C33 Si2 C31 106.4(12) . . ?
C33 Si2 C35 108.5(11) . . ?
C33 Si2 C34 110.8(14) . . ?
C34 Si2 C31 110.1(12) . . ?
C34 Si2 C35 113.6(13) . . ?
C11 O3 H3 109.5 . . ?
C48 C47 C44 173(2) . . ?
C31 O6 H6A 109.5 . . ?
O11 N1 C61 115(2) . . ?
O10 N1 O11 126(2) . . ?
O10 N1 C61 119(2) . . ?
O8 N2 C41 115(3) . . ?
O8 N2 O7 126(2) . . ?
O7 N2 C41 118(2) . . ?
C51 O9 H9A 109.5 . . ?
C46 C41 N2 122.6(16) . . ?
C46 C41 C42 120.0 . . ?
C42 C41 N2 117.3(16) . . ?
C41 C46 H46 120.0 . . ?
C45 C46 C41 120.0 . . ?
C45 C46 H46 120.0 . . ?
C46 C45 H45 120.0 . . ?
C46 C45 C44 120.0 . . ?
C44 C45 H45 120.0 . . ?
C45 C44 C47 121.0(12) . . ?
C45 C44 C43 120.0 . . ?
C43 C44 C47 118.9(12) . . ?
C44 C43 H43 120.0 . . ?
C42 C43 C44 120.0 . . ?
C42 C43 H43 120.0 . . ?
C41 C42 H42 120.0 . . ?
C43 C42 C41 120.0 . . ?
C43 C42 H42 120.0 . . ?
C47 C48 C49 176(2) . . ?
C48 C49 H49 108.0 . . ?
C48 C49 C50 106.6(17) . . ?
C51 C49 C48 109.7(16) . . ?
C51 C49 H49 108.0 . . ?
C51 C49 C50 116(2) . . ?
C50 C49 H49 108.0 . . ?
C67 C68 C69 177(2) . . ?
C71 O12 H12A 109.5 . . ?
C80 C79 H79 120.0 . . ?
C80 C79 C78 120.0 . . ?
C78 C79 H79 120.0 . . ?
C79 C80 H80 120.0 . . ?
C79 C80 C75 120.0 . . ?
C75 C80 H80 120.0 . . ?
C80 C75 Si4 119.6(8) . . ?
C76 C75 Si4 120.4(8) . . ?
C76 C75 C80 120.0 . . ?
C75 C76 H76 120.0 . . ?
C77 C76 C75 120.0 . . ?
C77 C76 H76 120.0 . . ?
C76 C77 H77 120.0 . . ?
C78 C77 C76 120.0 . . ?
C78 C77 H77 120.0 . . ?
C79 C78 H78 120.0 . . ?
C77 C78 C79 120.0 . . ?
C77 C78 H78 120.0 . . ?
O3 C11 Si1 104.4(17) . . ?
O3 C11 C12 110.3(17) . . ?
O3 C11 C9 108.7(19) . . ?
C12 C11 Si1 110.7(19) . . ?
C12 C11 C9 111(2) . . ?
C9 C11 Si1 111.8(13) . . ?
C68 C69 H69 106.2 . . ?
C68 C69 C70 107.8(19) . . ?
C68 C69 C71 113.0(16) . . ?
C70 C69 H69 106.2 . . ?
C71 C69 H69 106.2 . . ?
C71 C69 C70 116.6(19) . . ?
C3 C4 C5 120.0 . . ?
C3 C4 C7 119.9(12) . . ?
C5 C4 C7 119.7(12) . . ?
C4 C3 H3A 120.0 . . ?
C4 C3 C2 120.0 . . ?
C2 C3 H3A 120.0 . . ?
C3 C2 H2 120.0 . . ?
C3 C2 C1 120.0 . . ?
C1 C2 H2 120.0 . . ?
C2 C1 N4 121.1(12) . . ?
C6 C1 C2 120.0 . . ?
C6 C1 N4 118.8(12) . . ?
C1 C6 H6 120.0 . . ?
C1 C6 C5 120.0 . . ?
C5 C6 H6 120.0 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C22 C21 C26 120.0 . . ?
C22 C21 N3 119.3(17) . . ?
C26 C21 N3 120.7(17) . . ?
C21 C22 H22 120.0 . . ?
C21 C22 C23 120.0 . . ?
C23 C22 H22 120.0 . . ?
C22 C23 H23 120.0 . . ?
C24 C23 C22 120.0 . . ?
C24 C23 H23 120.0 . . ?
C23 C24 C25 120.0 . . ?
C23 C24 C27 120.9(14) . . ?
C25 C24 C27 119.0(14) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 C24 120.0 . . ?
C26 C25 H25 120.0 . . ?
C21 C26 H26 120.0 . . ?
C25 C26 C21 120.0 . . ?
C25 C26 H26 120.0 . . ?
Si4 C73 H73A 109.5 . . ?
Si4 C73 H73B 109.5 . . ?
Si4 C73 H73C 109.5 . . ?
H73A C73 H73B 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
O6 C31 Si2 101.1(15) . . ?
O6 C31 C29 110(2) . . ?
O6 C31 C32 113(2) . . ?
C29 C31 Si2 112.4(17) . . ?
C32 C31 Si2 109.3(18) . . ?
C32 C31 C29 111(2) . . ?
F6 C52 H52 108.7 . . ?
F6 C52 C51 112(2) . . ?
F5 C52 F6 105(2) . . ?
F5 C52 H52 108.7 . . ?
F5 C52 C51 113(2) . . ?
C51 C52 H52 108.7 . . ?
C68 C67 C64 176(2) . . ?
C31 C29 H29 105.6 . . ?
C30 C29 C31 117(2) . . ?
C30 C29 H29 105.6 . . ?
C28 C29 C31 110(2) . . ?
C28 C29 H29 105.6 . . ?
C28 C29 C30 112.6(19) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Si3 C54 H54A 109.5 . . ?
Si3 C54 H54B 109.5 . . ?
Si3 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C8 C7 C4 176(2) . . ?
C40 C35 Si2 120.1(11) . . ?
C40 C35 C36 120.0 . . ?
C36 C35 Si2 119.7(11) . . ?
C35 C40 H40 120.0 . . ?
C35 C40 C39 120.0 . . ?
C39 C40 H40 120.0 . . ?
C40 C39 H39 120.0 . . ?
C38 C39 C40 120.0 . . ?
C38 C39 H39 120.0 . . ?
C39 C38 H38 120.0 . . ?
C37 C38 C39 120.0 . . ?
C37 C38 H38 120.0 . . ?
C38 C37 H37 120.0 . . ?
C38 C37 C36 120.0 . . ?
C36 C37 H37 120.0 . . ?
C35 C36 H36 120.0 . . ?
C37 C36 C35 120.0 . . ?
C37 C36 H36 120.0 . . ?
C20 C15 Si1 120.1(10) . . ?
C20 C15 C16 120.0 . . ?
C16 C15 Si1 119.8(10) . . ?
C15 C20 H20 120.0 . . ?
C19 C20 C15 120.0 . . ?
C19 C20 H20 120.0 . . ?
C20 C19 H19 120.0 . . ?
C20 C19 C18 120.0 . . ?
C18 C19 H19 120.0 . . ?
C19 C18 H18 120.0 . . ?
C19 C18 C17 120.0 . . ?
C17 C18 H18 120.0 . . ?
C18 C17 H17 120.0 . . ?
C16 C17 C18 120.0 . . ?
C16 C17 H17 120.0 . . ?
C15 C16 H16 120.0 . . ?
C17 C16 C15 120.0 . . ?
C17 C16 H16 120.0 . . ?
C65 C66 H66 120.0 . . ?
C65 C66 C61 120.0 . . ?
C61 C66 H66 120.0 . . ?
C66 C65 H65 120.0 . . ?
C66 C65 C64 120.0 . . ?
C64 C65 H65 120.0 . . ?
C65 C64 C67 120.8(11) . . ?
C63 C64 C67 119.1(11) . . ?
C63 C64 C65 120.0 . . ?
C64 C63 H63 120.0 . . ?
C64 C63 C62 120.0 . . ?
C62 C63 H63 120.0 . . ?
C63 C62 H62 120.0 . . ?
C61 C62 C63 120.0 . . ?
C61 C62 H62 120.0 . . ?
C66 C61 N1 118.5(14) . . ?
C62 C61 N1 121.4(14) . . ?
C62 C61 C66 120.0 . . ?
F3 C32 C31 111(2) . . ?
F3 C32 F4 105(2) . . ?
F3 C32 H32 110.3 . . ?
C31 C32 H32 110.3 . . ?
F4 C32 C31 110(2) . . ?
F4 C32 H32 110.3 . . ?
F2 C12 F1 104.8(18) . . ?
F2 C12 C11 111(2) . . ?
F2 C12 H12 110.5 . . ?
F1 C12 C11 109(3) . . ?
F1 C12 H12 110.5 . . ?
C11 C12 H12 110.5 . . ?
C11 C9 H9 106.6 . . ?
C8 C9 C11 110.2(19) . . ?
C8 C9 H9 106.6 . . ?
C8 C9 C10 108(2) . . ?
C10 C9 C11 118.0(17) . . ?
C10 C9 H9 106.6 . . ?
Si2 C33 H33A 109.5 . . ?
Si2 C33 H33B 109.5 . . ?
Si2 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C56 C55 Si3 121.4(10) . . ?
C56 C55 C60 120.0 . . ?
C60 C55 Si3 118.3(10) . . ?
C55 C56 H56 120.0 . . ?
C55 C56 C57 120.0 . . ?
C57 C56 H56 120.0 . . ?
C56 C57 H57 120.0 . . ?
C58 C57 C56 120.0 . . ?
C58 C57 H57 120.0 . . ?
C57 C58 H58 120.0 . . ?
C57 C58 C59 120.0 . . ?
C59 C58 H58 120.0 . . ?
C58 C59 H59 120.0 . . ?
C58 C59 C60 120.0 . . ?
C60 C59 H59 120.0 . . ?
C55 C60 H60 120.0 . . ?
C59 C60 C55 120.0 . . ?
C59 C60 H60 120.0 . . ?
O9 C51 Si3 98.7(16) . . ?
O9 C51 C49 109.0(17) . . ?
O9 C51 C52 109.6(19) . . ?
C49 C51 Si3 112.6(15) . . ?
C52 C51 Si3 111.7(18) . . ?
C52 C51 C49 114(2) . . ?
Si2 C34 H34A 109.5 . . ?
Si2 C34 H34B 109.5 . . ?
Si2 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C7 C8 C9 177(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
Si3 C53 H53A 109.5 . . ?
Si3 C53 H53B 109.5 . . ?
Si3 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C69 C70 H70A 109.5 . . ?
C69 C70 H70B 109.5 . . ?
C69 C70 H70C 109.5 . . ?
H70A C70 H70B 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C28 C27 C24 173(3) . . ?
Si1 C14 H14A 109.5 . . ?
Si1 C14 H14B 109.5 . . ?
Si1 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si1 C13 H13A 109.5 . . ?
Si1 C13 H13B 109.5 . . ?
Si1 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C27 C28 C29 174(3) . . ?
Si4 C74 H74A 109.5 . . ?
Si4 C74 H74B 109.5 . . ?
Si4 C74 H74C 109.5 . . ?
H74A C74 H74B 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
O4 N3 C21 119(2) . . ?
O4 N3 O5 123(3) . . ?
O5 N3 C21 117(3) . . ?
O1 N4 C1 119(2) . . ?
O2 N4 C1 121(2) . . ?
O2 N4 O1 119(2) . . ?
O12 C71 Si4 102.0(12) . . ?
O12 C71 C69 111.3(14) . . ?
O12 C71 C72 113.5(18) . . ?
C69 C71 Si4 112.6(14) . . ?
C69 C71 C72 110.4(19) . . ?
C72 C71 Si4 106.8(15) . . ?
F7 C72 F8 103(2) . . ?
F7 C72 C71 107(2) . . ?
F7 C72 H72 112.6 . . ?
F8 C72 C71 109(2) . . ?
F8 C72 H72 112.6 . . ?
C71 C72 H72 112.6 . . ?
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 C11 1.93(3) . ?
Si1 C15 1.891(13) . ?
Si1 C14 1.86(2) . ?
Si1 C13 1.88(3) . ?
Si4 C75 1.899(12) . ?
Si4 C73 1.89(2) . ?
Si4 C74 1.85(2) . ?
Si4 C71 1.97(2) . ?
Si3 C54 1.88(2) . ?
Si3 C55 1.894(14) . ?
Si3 C51 1.97(3) . ?
Si3 C53 1.92(2) . ?
Si2 C31 1.98(3) . ?
Si2 C35 1.897(14) . ?
Si2 C33 1.86(3) . ?
Si2 C34 1.86(3) . ?
F6 C52 1.36(3) . ?
O3 H3 0.8200 . ?
O3 C11 1.41(3) . ?
C47 C44 1.43(3) . ?
C47 C48 1.16(3) . ?
O6 H6A 0.8200 . ?
O6 C31 1.41(3) . ?
O8 N2 1.21(3) . ?
F2 C12 1.34(3) . ?
N1 O11 1.21(3) . ?
N1 O10 1.19(3) . ?
N1 C61 1.47(2) . ?
N2 C41 1.44(2) . ?
N2 O7 1.22(3) . ?
O9 H9A 0.8200 . ?
O9 C51 1.46(3) . ?
C41 C46 1.3900 . ?
C41 C42 1.3900 . ?
C46 H46 0.9300 . ?
C46 C45 1.3900 . ?
C45 H45 0.9300 . ?
C45 C44 1.3900 . ?
C44 C43 1.3900 . ?
C43 H43 0.9300 . ?
C43 C42 1.3900 . ?
C42 H42 0.9300 . ?
C48 C49 1.55(3) . ?
C49 H49 0.9800 . ?
C49 C51 1.50(3) . ?
C49 C50 1.55(3) . ?
C68 C69 1.51(3) . ?
C68 C67 1.16(3) . ?
F1 C12 1.36(3) . ?
O12 H12A 0.8200 . ?
O12 C71 1.42(2) . ?
C79 H79 0.9300 . ?
C79 C80 1.3900 . ?
C79 C78 1.3900 . ?
C80 H80 0.9300 . ?
C80 C75 1.3900 . ?
C75 C76 1.3900 . ?
C76 H76 0.9300 . ?
C76 C77 1.3900 . ?
C77 H77 0.9300 . ?
C77 C78 1.3900 . ?
C78 H78 0.9300 . ?
C11 C12 1.53(4) . ?
C11 C9 1.59(3) . ?
F3 C32 1.34(3) . ?
C69 H69 0.9800 . ?
C69 C70 1.56(3) . ?
C69 C71 1.53(3) . ?
C4 C3 1.3900 . ?
C4 C5 1.3900 . ?
C4 C7 1.44(3) . ?
C3 H3A 0.9300 . ?
C3 C2 1.3900 . ?
C2 H2 0.9300 . ?
C2 C1 1.3900 . ?
C1 C6 1.3900 . ?
C1 N4 1.41(2) . ?
C6 H6 0.9300 . ?
C6 C5 1.3900 . ?
C5 H5 0.9300 . ?
F5 C52 1.35(3) . ?
C21 C22 1.3900 . ?
C21 C26 1.3900 . ?
C21 N3 1.42(2) . ?
C22 H22 0.9300 . ?
C22 C23 1.3900 . ?
C23 H23 0.9300 . ?
C23 C24 1.3900 . ?
C24 C25 1.3900 . ?
C24 C27 1.42(3) . ?
C25 H25 0.9300 . ?
C25 C26 1.3900 . ?
C26 H26 0.9300 . ?
C73 H73A 0.9600 . ?
C73 H73B 0.9600 . ?
C73 H73C 0.9600 . ?
C31 C29 1.55(3) . ?
C31 C32 1.50(3) . ?
C52 H52 0.9800 . ?
C52 C51 1.48(3) . ?
C67 C64 1.42(2) . ?
C29 H29 0.9800 . ?
C29 C30 1.53(3) . ?
C29 C28 1.52(4) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C7 C8 1.21(3) . ?
C35 C40 1.3900 . ?
C35 C36 1.3900 . ?
C40 H40 0.9300 . ?
C40 C39 1.3900 . ?
C39 H39 0.9300 . ?
C39 C38 1.3900 . ?
C38 H38 0.9300 . ?
C38 C37 1.3900 . ?
C37 H37 0.9300 . ?
C37 C36 1.3900 . ?
C36 H36 0.9300 . ?
F4 C32 1.39(3) . ?
C15 C20 1.3900 . ?
C15 C16 1.3900 . ?
C20 H20 0.9300 . ?
C20 C19 1.3900 . ?
C19 H19 0.9300 . ?
C19 C18 1.3900 . ?
C18 H18 0.9300 . ?
C18 C17 1.3900 . ?
C17 H17 0.9300 . ?
C17 C16 1.3900 . ?
C16 H16 0.9300 . ?
C66 H66 0.9300 . ?
C66 C65 1.3900 . ?
C66 C61 1.3900 . ?
C65 H65 0.9300 . ?
C65 C64 1.3900 . ?
C64 C63 1.3900 . ?
C63 H63 0.9300 . ?
C63 C62 1.3900 . ?
C62 H62 0.9300 . ?
C62 C61 1.3900 . ?
C32 H32 0.9800 . ?
F7 C72 1.37(3) . ?
C12 H12 0.9800 . ?
C9 H9 0.9800 . ?
C9 C8 1.47(4) . ?
C9 C10 1.55(3) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C55 C56 1.3900 . ?
C55 C60 1.3900 . ?
C56 H56 0.9300 . ?
C56 C57 1.3900 . ?
C57 H57 0.9300 . ?
C57 C58 1.3900 . ?
C58 H58 0.9300 . ?
C58 C59 1.3900 . ?
C59 H59 0.9300 . ?
C59 C60 1.3900 . ?
C60 H60 0.9300 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C70 H70A 0.9600 . ?
C70 H70B 0.9600 . ?
C70 H70C 0.9600 . ?
C27 C28 1.16(3) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C74 H74A 0.9600 . ?
C74 H74B 0.9600 . ?
C74 H74C 0.9600 . ?
F8 C72 1.39(3) . ?
O1 N4 1.20(2) . ?
O4 N3 1.18(3) . ?
N3 O5 1.22(3) . ?
N4 O2 1.17(2) . ?
C71 C72 1.56(3) . ?
C72 H72 0.9800 . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 1.05(11)
2 -0.05(11)
