# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_opera1909b
_database_code_depnum_ccdc_archive 'CCDC 1987607'
loop_
_audit_author_name
_audit_author_address
'Jerome Marrot'
;Institut Lavoisier de Versailles
France
;
_audit_update_record             
;
2020-03-02 deposited with the CCDC.	2020-10-20 downloaded from the CCDC.
;
_audit_creation_date             2019-09-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C52 H62 Si2'
_chemical_formula_sum            'C52 H62 Si2'
_chemical_formula_weight         743.19
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.7000(5)
_cell_length_b                   8.2465(5)
_cell_length_c                   17.9156(8)
_cell_angle_alpha                89.138(4)
_cell_angle_beta                 79.878(4)
_cell_angle_gamma                75.346(5)
_cell_volume                     1082.95(11)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    5800
_cell_measurement_temperature    123
_cell_measurement_theta_max      30.5210
_cell_measurement_theta_min      2.7040
_shelx_estimated_absorpt_T_max   0.997
_shelx_estimated_absorpt_T_min   0.966
_exptl_absorpt_coefficient_mu    0.116
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94230
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             402
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17540
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         2.311
_diffrn_ambient_temperature      123
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -47.00 -20.00   0.50    6.05    --    5.00  45.00 120.00   54
  2  ω    -10.00  16.00   0.50    6.05    --  -10.00  45.00  30.00   52
  3  ω     27.00  54.00   0.50    6.05    --  -10.00  45.00  30.00   54
  4  ω    -99.00  78.00   0.50    6.05    --  -10.00  45.00 150.00  354
  5  ω    -99.00  79.00   0.50    6.05    --  -10.00  45.00  90.00  356
  6  ω    -30.00  47.00   0.50    6.05    --  -10.00  45.00   0.00  154
  7  ω    -66.00 -40.00   0.50    6.05    --  -10.00  45.00  30.00   52
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC HyPix-6000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0621918000
_diffrn_orient_matrix_UB_12      -0.0422534000
_diffrn_orient_matrix_UB_13      -0.0103913000
_diffrn_orient_matrix_UB_21      -0.0324021000
_diffrn_orient_matrix_UB_22      -0.0108276000
_diffrn_orient_matrix_UB_23      0.0388531000
_diffrn_orient_matrix_UB_31      -0.0666618000
_diffrn_orient_matrix_UB_32      0.0775169000
_diffrn_orient_matrix_UB_33      0.0011892000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              FR-E+
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3978
_reflns_number_total             4955
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 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)'
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         4955
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0448
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0622P)²+0.3606P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1234
_refine_special_details          ?
_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:
 C21(H21), C18(H18), C24(H24)
2.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C15(H15A,H15B), C14(H14A,H14B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C4(H4), C3(H3), C5(H5)
2.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C20(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.74422(6) 0.75881(5) 0.15820(2) 0.02168(13) Uani 1 1 d . . . . .
C8 C 0.17962(19) 0.69564(17) 0.48108(8) 0.0183(3) Uani 1 1 d . . . . .
C9 C 0.23339(19) 0.78181(18) 0.41341(8) 0.0178(3) Uani 1 1 d . . . . .
C7 C 0.28188(19) 0.51857(18) 0.46970(8) 0.0190(3) Uani 1 1 d . . . . .
C1 C 0.37148(19) 0.66762(18) 0.36446(8) 0.0185(3) Uani 1 1 d . . . . .
C2 C 0.39893(19) 0.50392(18) 0.39849(8) 0.0192(3) Uani 1 1 d . . . . .
C16 C 0.4798(2) 0.69633(17) 0.29595(8) 0.0199(3) Uani 1 1 d . . . . .
C11 C 0.02220(19) 1.04158(17) 0.46472(8) 0.0178(3) Uani 1 1 d . . . . .
C12 C -0.06152(19) 1.21871(17) 0.45833(8) 0.0180(3) Uani 1 1 d . . . . .
C13 C -0.0186(2) 1.30338(18) 0.38483(8) 0.0212(3) Uani 1 1 d . . . . .
H13A H 0.080992 1.357776 0.387572 0.025 Uiso 1 1 calc R . . . .
H13B H -0.127530 1.391825 0.377359 0.025 Uiso 1 1 calc R . . . .
C10 C 0.14954(19) 0.95309(18) 0.40487(8) 0.0180(3) Uani 1 1 d . . . . .
C15 C 0.1955(2) 1.03572(18) 0.33109(8) 0.0222(3) Uani 1 1 d . . . . .
H15A H 0.225142 0.951761 0.288818 0.027 Uiso 1 1 calc R . . . .
H15B H 0.304479 1.078181 0.331809 0.027 Uiso 1 1 calc R . . . .
C6 C 0.2788(2) 0.37545(19) 0.51151(9) 0.0232(3) Uani 1 1 d . . . . .
H6 H 0.198431 0.382122 0.558765 0.028 Uiso 1 1 calc R . . . .
C17 C 0.5811(2) 0.71455(19) 0.23854(9) 0.0234(3) Uani 1 1 d . . . . .
C14 C 0.0381(2) 1.17997(19) 0.31771(8) 0.0242(3) Uani 1 1 d . . . . .
H14A H 0.075669 1.237551 0.271065 0.029 Uiso 1 1 calc R . . . .
H14B H -0.066500 1.136197 0.310598 0.029 Uiso 1 1 calc R . . . .
C4 C 0.5118(2) 0.21026(19) 0.41369(9) 0.0267(3) Uani 1 1 d . . . . .
H4 H 0.590655 0.104695 0.395735 0.032 Uiso 1 1 calc R . . . .
C3 C 0.5143(2) 0.35033(19) 0.37052(9) 0.0225(3) Uani 1 1 d . . . . .
H3 H 0.593058 0.341927 0.322776 0.027 Uiso 1 1 calc R . . . .
C5 C 0.3946(2) 0.22256(19) 0.48328(9) 0.0262(3) Uani 1 1 d . . . . .
H5 H 0.393911 0.124796 0.511935 0.031 Uiso 1 1 calc R . . . .
C21 C 0.8163(2) 0.5729(2) 0.09012(9) 0.0287(4) Uani 1 1 d . . . . .
H21 H 0.906329 0.597865 0.046973 0.034 Uiso 1 1 calc R . . . .
C18 C 0.6199(2) 0.9496(2) 0.11229(10) 0.0343(4) Uani 1 1 d . . . . .
H18 H 0.506487 0.924610 0.100983 0.041 Uiso 1 1 calc R . . . .
C24 C 0.9398(3) 0.7985(2) 0.19857(10) 0.0349(4) Uani 1 1 d . . . . .
H24 H 0.899230 0.916633 0.219204 0.042 Uiso 1 1 calc R . . . .
C19 C 0.7254(3) 0.9897(2) 0.03686(11) 0.0420(5) Uani 1 1 d . . . . .
H19A H 0.835081 1.020719 0.045649 0.063 Uiso 1 1 calc GR . . . .
H19B H 0.648170 1.083213 0.014004 0.063 Uiso 1 1 calc GR . . . .
H19C H 0.760768 0.890876 0.002527 0.063 Uiso 1 1 calc GR . . . .
C22 C 0.9099(3) 0.4111(2) 0.12478(12) 0.0438(5) Uani 1 1 d . . . . .
H22A H 1.023119 0.423476 0.139042 0.066 Uiso 1 1 calc GR . . . .
H22B H 0.937938 0.318027 0.087596 0.066 Uiso 1 1 calc GR . . . .
H22C H 0.828612 0.387954 0.169941 0.066 Uiso 1 1 calc GR . . . .
C23 C 0.6550(3) 0.5469(3) 0.05733(12) 0.0488(5) Uani 1 1 d . . . . .
H23A H 0.561728 0.526383 0.098529 0.073 Uiso 1 1 calc GR . . . .
H23B H 0.696407 0.450307 0.021645 0.073 Uiso 1 1 calc GR . . . .
H23C H 0.603131 0.647432 0.030751 0.073 Uiso 1 1 calc GR . . . .
C25 C 0.9846(4) 0.6880(4) 0.26483(13) 0.0693(8) Uani 1 1 d . . . . .
H25A H 0.876789 0.706719 0.305056 0.104 Uiso 1 1 calc GR . . . .
H25B H 1.084804 0.716007 0.284433 0.104 Uiso 1 1 calc GR . . . .
H25C H 1.021031 0.569970 0.247704 0.104 Uiso 1 1 calc GR . . . .
C26 C 1.1106(3) 0.7876(4) 0.13943(12) 0.0609(7) Uani 1 1 d . . . . .
H26A H 1.155410 0.673548 0.117270 0.091 Uiso 1 1 calc GR . . . .
H26B H 1.204846 0.815232 0.163503 0.091 Uiso 1 1 calc GR . . . .
H26C H 1.081743 0.867076 0.099441 0.091 Uiso 1 1 calc GR . . . .
C20 C 0.5585(4) 1.1051(3) 0.16537(14) 0.0656(8) Uani 1 1 d . . . . .
H20A H 0.489666 1.079025 0.213422 0.098 Uiso 1 1 calc GR . . . .
H20B H 0.480893 1.196696 0.141614 0.098 Uiso 1 1 calc GR . . . .
H20C H 0.665841 1.139146 0.175037 0.098 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 C17 1.8337(15) . ?
Si1 C21 1.8800(16) . ?
Si1 C18 1.8824(18) . ?
Si1 C24 1.8804(18) . ?
C8 C9 1.4466(19) . ?
C8 C7 1.4712(19) . ?
C8 C12 1.362(2) 2_576 ?
C9 C1 1.4060(19) . ?
C9 C10 1.415(2) . ?
C7 C2 1.414(2) . ?
C7 C6 1.391(2) . ?
C1 C2 1.454(2) . ?
C1 C16 1.4107(19) . ?
C2 C3 1.392(2) . ?
C16 C17 1.209(2) . ?
C11 C11 1.458(3) 2_576 ?
C11 C12 1.4515(19) . ?
C11 C10 1.391(2) . ?
C12 C13 1.5055(19) . ?
C13 C14 1.517(2) . ?
C10 C15 1.5057(19) . ?
C15 C14 1.518(2) . ?
C6 C5 1.390(2) . ?
C4 C3 1.383(2) . ?
C4 C5 1.393(2) . ?
C21 C22 1.527(3) . ?
C21 C23 1.526(3) . ?
C18 C19 1.527(2) . ?
C18 C20 1.531(3) . ?
C24 C25 1.520(3) . ?
C24 C26 1.522(3) . ?

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
C17 Si1 C21 108.15(7) . . ?
C17 Si1 C18 106.65(7) . . ?
C17 Si1 C24 106.65(7) . . ?
C21 Si1 C18 110.38(8) . . ?
C21 Si1 C24 112.65(8) . . ?
C24 Si1 C18 112.04(9) . . ?
C9 C8 C7 107.33(12) . . ?
C12 C8 C9 120.79(13) 2_576 . ?
C12 C8 C7 131.78(13) 2_576 . ?
C1 C9 C8 108.46(12) . . ?
C1 C9 C10 130.59(13) . . ?
C10 C9 C8 120.95(12) . . ?
C2 C7 C8 107.01(12) . . ?
C6 C7 C8 133.82(13) . . ?
C6 C7 C2 119.12(13) . . ?
C9 C1 C2 108.19(12) . . ?
C9 C1 C16 129.51(13) . . ?
C16 C1 C2 122.19(13) . . ?
C7 C2 C1 108.85(12) . . ?
C3 C2 C7 121.33(13) . . ?
C3 C2 C1 129.81(13) . . ?
C17 C16 C1 176.23(16) . . ?
C12 C11 C11 119.68(16) . 2_576 ?
C10 C11 C11 120.11(16) . 2_576 ?
C10 C11 C12 120.16(12) . . ?
C8 C12 C11 119.06(13) 2_576 . ?
C8 C12 C13 121.36(13) 2_576 . ?
C11 C12 C13 119.57(12) . . ?
C12 C13 C14 111.75(12) . . ?
C9 C10 C15 119.90(12) . . ?
C11 C10 C9 119.06(13) . . ?
C11 C10 C15 121.02(13) . . ?
C10 C15 C14 111.48(12) . . ?
C5 C6 C7 119.19(14) . . ?
C16 C17 Si1 173.20(14) . . ?
C13 C14 C15 110.03(13) . . ?
C3 C4 C5 120.59(14) . . ?
C4 C3 C2 118.59(14) . . ?
C6 C5 C4 121.14(14) . . ?
C22 C21 Si1 113.34(12) . . ?
C23 C21 Si1 111.13(12) . . ?
C23 C21 C22 109.94(16) . . ?
C19 C18 Si1 114.04(12) . . ?
C19 C18 C20 109.83(15) . . ?
C20 C18 Si1 112.52(15) . . ?
C25 C24 Si1 112.97(13) . . ?
C25 C24 C26 110.50(19) . . ?
C26 C24 Si1 113.51(13) . . ?

_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 1.150
_oxdiff_exptl_absorpt_empirical_full_min 0.872
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_opera2002a
_database_code_depnum_ccdc_archive 'CCDC 1987608'
loop_
_audit_author_name
_audit_author_address
'Jerome Marrot'
;Institut Lavoisier de Versailles
France
;
_audit_update_record             
;
2020-03-02 deposited with the CCDC.	2020-10-20 downloaded from the CCDC.
;
_audit_creation_date             2020-02-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H66 Si2, 2(C9 H12)'
_chemical_formula_sum            'C78 H90 Si2'
_chemical_formula_weight         1083.67
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
_chemical_oxdiff_usercomment     100K
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.8789(6)
_cell_length_b                   12.7356(5)
_cell_length_c                   14.6701(9)
_cell_angle_alpha                99.626(4)
_cell_angle_beta                 104.748(6)
_cell_angle_gamma                98.811(4)
_cell_volume                     1547.92(16)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    4693
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.8930
_cell_measurement_theta_min      2.4180
_shelx_estimated_absorpt_T_max   0.999
_shelx_estimated_absorpt_T_min   0.990
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             586
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17632
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.441
_diffrn_ambient_temperature      100
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -75.00 -47.00   0.50   45.00    --    4.70  45.00  90.00   56
  2  ω    -39.00  83.00   0.50   45.00    --    4.70  45.00  90.00  244
  3  ω    -72.00  12.00   0.50   45.00    --    4.70  45.00  30.00  168
  4  ω     39.00  87.00   0.50   45.00    --    4.70  45.00  30.00   96
  5  ω    -31.00  64.00   0.50   45.00    --    4.70  45.00 150.00  190
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC HyPix-6000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0174465000
_diffrn_orient_matrix_UB_12      -0.0045327000
_diffrn_orient_matrix_UB_13      -0.0506184000
_diffrn_orient_matrix_UB_21      0.0088038000
_diffrn_orient_matrix_UB_22      0.0573170000
_diffrn_orient_matrix_UB_23      0.0068007000
_diffrn_orient_matrix_UB_31      0.0821128000
_diffrn_orient_matrix_UB_32      0.0050731000
_diffrn_orient_matrix_UB_33      0.0036526000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              FR-E+
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4914
_reflns_number_total             6212
_reflns_odcompleteness_completeness 98.28
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (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)'
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6212
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0585
_refine_ls_restrained_S_all      1.030
_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)+(0.0560P)²+1.5843P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1336
_refine_ls_wR_factor_ref         0.1435
_refine_special_details          ?
_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:
 C00Q(H00Q), C00U(H00U), C00Z(H00Z)
2.b Secondary CH2 refined with riding coordinates:
 C00F(H00A,H00B), C00I(H00E,H00F), C00P(H00I,H00J)
2.c Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00D(H00D), C00G(H00G), C00H(H00H), C00L(H00L), C00M(H00M),
 C00N(H00X), C00O(H00Y), C00R(H00)
2.d Idealised Me refined as rotating group:
 C00T(H00K,H00N,H00O), C00W(H00P,H00R,H00S), C00X(H0AA,H,HA), C00Y(H00T,H00V,
 H00W), C010(H01J,H01K,H01L), C011(H01A,H01B,H01C), C012(H01M,H01N,H01O),
 C013(H01D,H01E,H01F), C014(H01G,H01H,H01I)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.33696(7) 0.49745(5) 0.29752(4) 0.02148(17) Uani 1 1 d . . . . .
C5 C 0.5239(2) 0.87325(16) 0.55806(14) 0.0157(4) Uani 1 1 d . . . . .
C1 C 0.5943(2) 0.81858(16) 0.49012(15) 0.0163(4) Uani 1 1 d . . . . .
C3 C 0.7640(2) 0.98485(16) 0.56766(14) 0.0154(4) Uani 1 1 d . . . . .
C20 C 0.5162(2) 0.71618(17) 0.42882(15) 0.0173(4) Uani 1 1 d . . . . .
C4 C 0.6284(2) 0.97641(16) 0.60774(14) 0.0158(4) Uani 1 1 d . . . . .
C2 C 0.7401(2) 0.88499(16) 0.49731(14) 0.0157(4) Uani 1 1 d . . . . .
C7 C 0.3399(2) 0.90584(16) 0.64951(15) 0.0171(4) Uani 1 1 d . . . . .
C19 C 1.0107(2) 1.05138(16) 0.53393(14) 0.0159(4) Uani 1 1 d . . . . .
C18 C 1.1453(2) 1.13273(16) 0.55168(14) 0.0158(4) Uani 1 1 d . . . . .
C12 C 0.4430(3) 1.00773(16) 0.69999(15) 0.0179(4) Uani 1 1 d . . . . .
C8 C 0.1973(3) 0.87497(17) 0.67249(16) 0.0212(5) Uani 1 1 d . . . . .
H8 H 0.128145 0.807336 0.639105 0.025 Uiso 1 1 calc R . . . .
C6 C 0.3847(2) 0.83917(16) 0.57805(15) 0.0170(4) Uani 1 1 d . . . . .
H6 H 0.318132 0.770847 0.544005 0.020 Uiso 1 1 calc R . . . .
C14 C 0.8920(2) 1.06713(16) 0.58377(14) 0.0160(4) Uani 1 1 d . . . . .
C17 C 1.1700(3) 1.23929(16) 0.62095(16) 0.0193(5) Uani 1 1 d . . . . .
H17A H 1.229466 1.297712 0.599141 0.023 Uiso 1 1 calc R . . . .
H17B H 1.234507 1.235154 0.685606 0.023 Uiso 1 1 calc R . . . .
C11 C 0.3982(3) 1.07282(17) 0.77213(16) 0.0217(5) Uani 1 1 d . . . . .
H11 H 0.465898 1.140495 0.806942 0.026 Uiso 1 1 calc R . . . .
C10 C 0.2588(3) 1.04015(18) 0.79286(17) 0.0245(5) Uani 1 1 d . . . . .
H10 H 0.230862 1.084971 0.841926 0.029 Uiso 1 1 calc R . . . .
C16 C 1.0125(3) 1.26709(16) 0.62787(17) 0.0216(5) Uani 1 1 d . . . . .
H16A H 0.954614 1.282009 0.565744 0.026 Uiso 1 1 calc R . . . .
H16B H 1.032493 1.333623 0.678669 0.026 Uiso 1 1 calc R . . . .
C35 C 0.2688(3) 0.12662(18) 0.07394(16) 0.0264(5) Uani 1 1 d . . . . .
C21 C 0.4430(3) 0.62838(17) 0.37905(15) 0.0205(5) Uani 1 1 d . . . . .
C13 C 0.5873(2) 1.04086(16) 0.67792(15) 0.0173(4) Uani 1 1 d . . . . .
H13 H 0.655806 1.108413 0.712223 0.021 Uiso 1 1 calc R . . . .
C9 C 0.1568(3) 0.94047(18) 0.74178(16) 0.0244(5) Uani 1 1 d . . . . .
H9 H 0.059346 0.918773 0.755683 0.029 Uiso 1 1 calc R . . . .
C36 C 0.4293(3) 0.12760(19) 0.08471(17) 0.0291(5) Uani 1 1 d . . . . .
H36 H 0.479114 0.079898 0.119912 0.035 Uiso 1 1 calc R . . . .
C32 C 0.4433(3) 0.26602(19) -0.00552(17) 0.0286(5) Uani 1 1 d . . . . .
H32 H 0.503315 0.314627 -0.031994 0.034 Uiso 1 1 calc R . . . .
C15 C 0.9110(3) 1.17416(16) 0.65159(16) 0.0207(5) Uani 1 1 d . . . . .
H15A H 0.960649 1.167928 0.718488 0.025 Uiso 1 1 calc R . . . .
H15B H 0.804640 1.190732 0.648256 0.025 Uiso 1 1 calc R . . . .
C28 C 0.2480(3) 0.41079(18) 0.37012(17) 0.0257(5) Uani 1 1 d . . . . .
H28 H 0.335378 0.414397 0.429806 0.031 Uiso 1 1 calc R . . . .
C34 C 0.1971(3) 0.19619(19) 0.02209(17) 0.0281(5) Uani 1 1 d . . . . .
H34 H 0.087505 0.196037 0.014218 0.034 Uiso 1 1 calc R . . . .
C33 C 0.2829(3) 0.26620(19) -0.01860(17) 0.0296(5) Uani 1 1 d . . . . .
C29 C 0.1928(3) 0.29010(19) 0.31938(19) 0.0321(6) Uani 1 1 d . . . . .
H29A H 0.103792 0.281769 0.261463 0.048 Uiso 1 1 calc GR . . . .
H29B H 0.158457 0.248103 0.363322 0.048 Uiso 1 1 calc GR . . . .
H29C H 0.281046 0.263410 0.300967 0.048 Uiso 1 1 calc GR . . . .
C22 C 0.4867(3) 0.43169(19) 0.25265(19) 0.0334(6) Uani 1 1 d . . . . .
H22 H 0.429035 0.359287 0.210316 0.040 Uiso 1 1 calc R . . . .
C31 C 0.5181(3) 0.19674(19) 0.04516(17) 0.0278(5) Uani 1 1 d . . . . .
C30 C 0.1157(3) 0.4539(2) 0.4041(2) 0.0370(6) Uani 1 1 d . . . . .
H30A H 0.154687 0.530172 0.438134 0.056 Uiso 1 1 calc GR . . . .
H30B H 0.083031 0.410701 0.447775 0.056 Uiso 1 1 calc GR . . . .
H30C H 0.024345 0.448338 0.348132 0.056 Uiso 1 1 calc GR . . . .
C39 C 0.1749(3) 0.0509(2) 0.11760(19) 0.0354(6) Uani 1 1 d . . . . .
H39A H 0.185864 -0.023842 0.095854 0.053 Uiso 1 1 calc GR . . . .
H39B H 0.062419 0.055320 0.097206 0.053 Uiso 1 1 calc GR . . . .
H39C H 0.215219 0.071994 0.188149 0.053 Uiso 1 1 calc GR . . . .
C23 C 0.5707(3) 0.4942(2) 0.1934(2) 0.0394(7) Uani 1 1 d . . . . .
H23A H 0.493469 0.496318 0.133022 0.059 Uiso 1 1 calc GR . . . .
H23B H 0.654072 0.457835 0.178788 0.059 Uiso 1 1 calc GR . . . .
H23C H 0.618715 0.568627 0.230338 0.059 Uiso 1 1 calc GR . . . .
C25 C 0.1771(3) 0.5371(2) 0.2029(2) 0.0401(7) Uani 1 1 d . . . . .
H25 H 0.117242 0.577425 0.241149 0.048 Uiso 1 1 calc R . . . .
C38 C 0.2035(4) 0.3391(2) -0.0776(2) 0.0450(7) Uani 1 1 d . . . . .
H38A H 0.257406 0.415033 -0.049144 0.068 Uiso 1 1 calc GR . . . .
H38B H 0.091633 0.329879 -0.078221 0.068 Uiso 1 1 calc GR . . . .
H38C H 0.209929 0.319759 -0.143835 0.068 Uiso 1 1 calc GR . . . .
C27 C 0.2453(3) 0.6195(2) 0.1530(2) 0.0392(6) Uani 1 1 d . . . . .
H27A H 0.323291 0.678554 0.201342 0.059 Uiso 1 1 calc GR . . . .
H27B H 0.159324 0.649341 0.116607 0.059 Uiso 1 1 calc GR . . . .
H27C H 0.297364 0.584015 0.108612 0.059 Uiso 1 1 calc GR . . . .
C37 C 0.6914(3) 0.1957(3) 0.0568(2) 0.0464(7) Uani 1 1 d . . . . .
H37A H 0.752926 0.226666 0.124223 0.070 Uiso 1 1 calc GR . . . .
H37B H 0.729903 0.239225 0.015058 0.070 Uiso 1 1 calc GR . . . .
H37C H 0.704157 0.120695 0.038700 0.070 Uiso 1 1 calc GR . . . .
C26 C 0.0546(4) 0.4448(2) 0.1361(2) 0.0517(8) Uani 1 1 d . . . . .
H26A H 0.106085 0.396184 0.100782 0.078 Uiso 1 1 calc GR . . . .
H26B H -0.021557 0.472820 0.090183 0.078 Uiso 1 1 calc GR . . . .
H26C H -0.001501 0.404533 0.173163 0.078 Uiso 1 1 calc GR . . . .
C24 C 0.6105(4) 0.4110(3) 0.3367(3) 0.0516(8) Uani 1 1 d . . . . .
H24A H 0.674370 0.480602 0.377290 0.077 Uiso 1 1 calc GR . . . .
H24B H 0.680005 0.368140 0.311897 0.077 Uiso 1 1 calc GR . . . .
H24C H 0.557209 0.370748 0.374987 0.077 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 C21 1.837(2) . ?
Si1 C28 1.879(2) . ?
Si1 C22 1.872(3) . ?
Si1 C25 1.910(3) . ?
C5 C1 1.444(3) . ?
C5 C4 1.442(3) . ?
C5 C6 1.366(3) . ?
C1 C20 1.415(3) . ?
C1 C2 1.403(3) . ?
C3 C4 1.466(3) . ?
C3 C2 1.447(3) . ?
C3 C14 1.364(3) . ?
C20 C15 1.212(3) . ?
C4 C13 1.367(3) . ?
C2 C18 1.411(3) 2_776 ?
C7 C12 1.428(3) . ?
C7 C8 1.407(3) . ?
C7 C6 1.413(3) . ?
C19 C19 1.460(4) 2_776 ?
C19 C18 1.393(3) . ?
C19 C14 1.447(3) . ?
C18 C17 1.502(3) . ?
C12 C11 1.410(3) . ?
C12 C13 1.419(3) . ?
C8 C9 1.361(3) . ?
C14 C15 1.506(3) . ?
C17 C16 1.518(3) . ?
C11 C10 1.369(3) . ?
C10 C9 1.406(3) . ?
C16 C15 1.518(3) . ?
C35 C36 1.390(3) . ?
C35 C34 1.386(3) . ?
C35 C39 1.506(3) . ?
C36 C31 1.388(3) . ?
C32 C33 1.389(4) . ?
C32 C31 1.386(4) . ?
C28 C29 1.535(3) . ?
C28 C30 1.528(3) . ?
C34 C33 1.390(4) . ?
C33 C38 1.505(4) . ?
C22 C23 1.525(4) . ?
C22 C24 1.518(4) . ?
C31 C37 1.507(4) . ?
C25 C27 1.515(4) . ?
C25 C26 1.485(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
C21 Si1 C28 107.54(10) . . ?
C21 Si1 C22 107.72(11) . . ?
C21 Si1 C25 103.43(11) . . ?
C28 Si1 C25 111.82(12) . . ?
C22 Si1 C28 109.39(11) . . ?
C22 Si1 C25 116.38(13) . . ?
C4 C5 C1 108.63(18) . . ?
C6 C5 C1 129.36(19) . . ?
C6 C5 C4 122.01(18) . . ?
C20 C1 C5 121.47(19) . . ?
C2 C1 C5 108.32(17) . . ?
C2 C1 C20 130.19(19) . . ?
C2 C3 C4 107.30(17) . . ?
C14 C3 C4 131.55(19) . . ?
C14 C3 C2 121.09(19) . . ?
C21 C20 C1 176.4(2) . . ?
C5 C4 C3 106.59(17) . . ?
C13 C4 C5 118.66(19) . . ?
C13 C4 C3 134.74(19) . . ?
C1 C2 C3 109.11(18) . . ?
C1 C2 C18 130.25(18) . 2_776 ?
C18 C2 C3 120.64(18) 2_776 . ?
C8 C7 C12 119.11(19) . . ?
C8 C7 C6 122.12(19) . . ?
C6 C7 C12 118.77(19) . . ?
C18 C19 C19 120.4(2) . 2_776 ?
C18 C19 C4 120.35(18) . . ?
C14 C19 C19 119.3(2) . 2_776 ?
C2 C18 C17 119.34(18) 2_776 . ?
C19 C18 C2 119.23(18) . 2_776 ?
C19 C18 C17 121.42(18) . . ?
C11 C12 C7 118.26(19) . . ?
C11 C12 C13 121.55(19) . . ?
C13 C12 C7 120.19(18) . . ?
C9 C8 C7 121.1(2) . . ?
C5 C6 C7 119.80(18) . . ?
C3 C14 C19 119.26(18) . . ?
C3 C14 C15 121.23(19) . . ?
C19 C14 C15 119.51(18) . . ?
C18 C17 C16 111.31(17) . . ?
C10 C11 C12 121.1(2) . . ?
C11 C10 C9 120.2(2) . . ?
C15 C16 C17 110.80(18) . . ?
C36 C35 C39 120.5(2) . . ?
C34 C35 C36 118.8(2) . . ?
C34 C35 C39 120.7(2) . . ?
C20 C21 Si1 176.4(2) . . ?
C4 C13 C12 120.55(19) . . ?
C8 C9 C10 120.2(2) . . ?
C31 C36 C35 121.4(2) . . ?
C31 C32 C33 121.7(2) . . ?
C14 C15 C16 112.37(17) . . ?
C29 C28 Si1 113.31(17) . . ?
C30 C28 Si1 113.26(17) . . ?
C30 C28 C29 110.9(2) . . ?
C35 C34 C33 121.1(2) . . ?
C32 C33 C34 118.6(2) . . ?
C32 C33 C38 120.4(2) . . ?
C34 C33 C38 121.0(2) . . ?
C23 C22 Si1 115.21(18) . . ?
C24 C22 Si1 110.12(19) . . ?
C24 C22 C23 109.1(2) . . ?
C36 C31 C37 120.6(2) . . ?
C32 C31 C36 118.4(2) . . ?
C32 C31 C37 121.0(2) . . ?
C27 C25 Si1 112.85(19) . . ?
C26 C25 Si1 115.3(2) . . ?
C26 C25 C27 114.0(2) . . ?

_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 1.100
_oxdiff_exptl_absorpt_empirical_full_min 0.908
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_opera2001c
_database_code_depnum_ccdc_archive 'CCDC 1987610'
loop_
_audit_author_name
_audit_author_address
'Jerome Marrot'
;Institut Lavoisier de Versailles
France
;
_audit_update_record             
;
2020-03-02 deposited with the CCDC.	2020-10-20 downloaded from the CCDC.
;
_audit_creation_date             2020-01-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H66 Si2'
_chemical_formula_sum            'C60 H66 Si2'
_chemical_formula_weight         843.30
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H Si N'
_chemical_oxdiff_usercomment     100K
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2869(3)
_cell_length_b                   9.3544(4)
_cell_length_c                   15.0106(7)
_cell_angle_alpha                83.361(4)
_cell_angle_beta                 81.878(4)
_cell_angle_gamma                89.500(3)
_cell_volume                     1144.18(8)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    7410
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.5980
_cell_measurement_theta_min      2.1420
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.118
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             454
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26342
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         2.192
_diffrn_ambient_temperature      100
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  94.00   0.50    5.00    --    5.00  45.00 120.00  356
  2  ω    -99.00  -5.00   0.50    5.00    --  -10.30  45.00   0.00  188
  3  ω    -99.00  79.00   0.50    5.00    --  -10.30  45.00  90.00  356
  4  ω    -83.00 -57.00   0.50    5.00    --  -10.30  45.00  30.00   52
  5  ω    -26.00  63.00   0.50    5.00    --  -10.30  45.00  30.00  178
  6  ω    -99.00  78.00   0.50    5.00    --  -10.30  45.00 166.43  354
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC HyPix-6000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0004356000
_diffrn_orient_matrix_UB_12      -0.0755473000
_diffrn_orient_matrix_UB_13      -0.0013128000
_diffrn_orient_matrix_UB_21      -0.0854505000
_diffrn_orient_matrix_UB_22      0.0014657000
_diffrn_orient_matrix_UB_23      -0.0005382000
_diffrn_orient_matrix_UB_31      0.0131851000
_diffrn_orient_matrix_UB_32      0.0108722000
_diffrn_orient_matrix_UB_33      -0.0480330000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              FR-E+
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4265
_reflns_number_total             5252
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 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)'
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         5252
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0412
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0523P)²+0.4414P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1070
_refine_special_details          ?
_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:
 C22(H22), C25(H25), C28(H28)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B)
2.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18)
2.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.35672(5) 0.85293(4) 0.84812(3) 0.01347(11) Uani 1 1 d . . . . .
C1 C 0.26566(17) 0.39967(14) 0.54459(9) 0.0122(3) Uani 1 1 d . . . . .
C2 C 0.16712(17) 0.36005(14) 0.48554(9) 0.0123(3) Uani 1 1 d . . . . .
C3 C 0.20992(17) 0.23392(15) 0.43333(10) 0.0155(3) Uani 1 1 d . . . . .
H3A H 0.260620 0.160488 0.471025 0.019 Uiso 1 1 calc R . . . .
H3B H 0.288668 0.264737 0.380554 0.019 Uiso 1 1 calc R . . . .
C4 C 0.06298(18) 0.16961(15) 0.40293(10) 0.0168(3) Uani 1 1 d . . . . .
H4A H -0.006137 0.121576 0.455166 0.020 Uiso 1 1 calc R . . . .
H4B H 0.098496 0.098433 0.362344 0.020 Uiso 1 1 calc R . . . .
C5 C 0.03342(18) 0.71497(16) 0.64505(10) 0.0172(3) Uani 1 1 d . . . . .
H5A H 0.132053 0.757371 0.658862 0.021 Uiso 1 1 calc R . . . .
H5B H -0.030651 0.676935 0.701862 0.021 Uiso 1 1 calc R . . . .
C6 C 0.07814(17) 0.59433(15) 0.58895(9) 0.0130(3) Uani 1 1 d . . . . .
C7 C -0.02107(16) 0.55928(14) 0.52637(9) 0.0122(3) Uani 1 1 d . . . . .
C8 C 0.22117(17) 0.51448(15) 0.59870(9) 0.0125(3) Uani 1 1 d . . . . .
C9 C 0.34204(17) 0.52617(15) 0.65571(9) 0.0135(3) Uani 1 1 d . . . . .
C10 C 0.46420(17) 0.41852(15) 0.63701(9) 0.0132(3) Uani 1 1 d . . . . .
C11 C 0.60942(17) 0.38498(15) 0.67634(9) 0.0138(3) Uani 1 1 d . . . . .
C12 C 0.65765(18) 0.45170(16) 0.74807(10) 0.0178(3) Uani 1 1 d . . . . .
H12 H 0.591975 0.522317 0.772903 0.021 Uiso 1 1 calc R . . . .
C13 C 0.79931(19) 0.41454(17) 0.78188(10) 0.0199(3) Uani 1 1 d . . . . .
H13 H 0.828167 0.459759 0.829415 0.024 Uiso 1 1 calc R . . . .
C14 C 0.90111(18) 0.30906(16) 0.74553(10) 0.0189(3) Uani 1 1 d . . . . .
H14 H 0.998307 0.285814 0.767871 0.023 Uiso 1 1 calc R . . . .
C15 C 0.85668(18) 0.24064(16) 0.67711(10) 0.0175(3) Uani 1 1 d . . . . .
H15 H 0.924096 0.170069 0.653534 0.021 Uiso 1 1 calc R . . . .
C16 C 0.71064(17) 0.27471(15) 0.64140(9) 0.0144(3) Uani 1 1 d . . . . .
C17 C 0.66434(17) 0.20300(16) 0.57082(10) 0.0160(3) Uani 1 1 d . . . . .
H17 H 0.731460 0.131315 0.548415 0.019 Uiso 1 1 calc R . . . .
C18 C 0.52453(17) 0.23538(15) 0.53447(10) 0.0154(3) Uani 1 1 d . . . . .
H18 H 0.498086 0.187043 0.487656 0.018 Uiso 1 1 calc R . . . .
C19 C 0.42081(17) 0.34250(15) 0.56843(9) 0.0129(3) Uani 1 1 d . . . . .
C20 C 0.34878(17) 0.62852(15) 0.71748(10) 0.0148(3) Uani 1 1 d . . . . .
C21 C 0.35816(18) 0.71707(16) 0.76921(10) 0.0171(3) Uani 1 1 d . . . . .
C22 C 0.54740(18) 0.83030(16) 0.90266(10) 0.0174(3) Uani 1 1 d . . . . .
H22 H 0.545777 0.903026 0.944810 0.021 Uiso 1 1 calc R . . . .
C23 C 0.5568(2) 0.68230(17) 0.95773(11) 0.0237(3) Uani 1 1 d . . . . .
H23A H 0.552076 0.608182 0.918939 0.036 Uiso 1 1 calc GR . . . .
H23B H 0.466844 0.670913 1.005929 0.036 Uiso 1 1 calc GR . . . .
H23C H 0.657349 0.675281 0.982763 0.036 Uiso 1 1 calc GR . . . .
C24 C 0.70014(19) 0.85867(19) 0.83184(11) 0.0246(4) Uani 1 1 d . . . . .
H24A H 0.698967 0.956023 0.803521 0.037 Uiso 1 1 calc GR . . . .
H24B H 0.700999 0.793634 0.786776 0.037 Uiso 1 1 calc GR . . . .
H24C H 0.795832 0.844087 0.861012 0.037 Uiso 1 1 calc GR . . . .
C25 C 0.35410(18) 1.03510(15) 0.77956(10) 0.0164(3) Uani 1 1 d . . . . .
H25 H 0.460043 1.049016 0.741254 0.020 Uiso 1 1 calc R . . . .
C26 C 0.3339(2) 1.15678(16) 0.84004(11) 0.0236(3) Uani 1 1 d . . . . .
H26A H 0.419987 1.152408 0.876851 0.035 Uiso 1 1 calc GR . . . .
H26B H 0.230618 1.146528 0.878321 0.035 Uiso 1 1 calc GR . . . .
H26C H 0.338406 1.247774 0.802901 0.035 Uiso 1 1 calc GR . . . .
C27 C 0.2232(2) 1.04338(17) 0.71668(11) 0.0227(3) Uani 1 1 d . . . . .
H27A H 0.118550 1.021359 0.751834 0.034 Uiso 1 1 calc GR . . . .
H27B H 0.247095 0.975281 0.673523 0.034 Uiso 1 1 calc GR . . . .
H27C H 0.221873 1.138692 0.685253 0.034 Uiso 1 1 calc GR . . . .
C28 C 0.16448(18) 0.82370(16) 0.93263(10) 0.0177(3) Uani 1 1 d . . . . .
H28 H 0.078881 0.878869 0.905623 0.021 Uiso 1 1 calc R . . . .
C29 C 0.17829(19) 0.88415(17) 1.02184(10) 0.0213(3) Uani 1 1 d . . . . .
H29A H 0.206827 0.984443 1.009673 0.032 Uiso 1 1 calc GR . . . .
H29B H 0.261009 0.833052 1.051074 0.032 Uiso 1 1 calc GR . . . .
H29C H 0.075687 0.872829 1.060708 0.032 Uiso 1 1 calc GR . . . .
C30 C 0.1041(2) 0.66708(18) 0.95153(12) 0.0267(4) Uani 1 1 d . . . . .
H30A H 0.184779 0.608255 0.977644 0.040 Uiso 1 1 calc GR . . . .
H30B H 0.085398 0.633283 0.895820 0.040 Uiso 1 1 calc GR . . . .
H30C H 0.004231 0.661698 0.992936 0.040 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 C21 1.8336(15) . ?
Si1 C22 1.8792(15) . ?
Si1 C25 1.8878(15) . ?
Si1 C28 1.8916(15) . ?
C1 C2 1.3695(19) . ?
C1 C8 1.4350(19) . ?
C1 C19 1.4632(19) . ?
C2 C3 1.5034(19) . ?
C2 C7 1.4423(19) 2_566 ?
C3 C4 1.5119(19) . ?
C4 C5 1.513(2) 2_566 ?
C5 C6 1.4981(19) . ?
C6 C7 1.4001(19) . ?
C6 C8 1.4115(19) . ?
C7 C7 1.448(3) 2_566 ?
C8 C9 1.4189(19) . ?
C9 C10 1.444(2) . ?
C9 C20 1.414(2) . ?
C10 C11 1.4306(19) . ?
C10 C19 1.4047(19) . ?
C11 C12 1.411(2) . ?
C11 C16 1.424(2) . ?
C12 C13 1.370(2) . ?
C13 C14 1.401(2) . ?
C14 C15 1.365(2) . ?
C15 C16 1.411(2) . ?
C16 C17 1.415(2) . ?
C17 C18 1.366(2) . ?
C18 C19 1.408(2) . ?
C20 C21 1.209(2) . ?
C22 C23 1.536(2) . ?
C22 C24 1.537(2) . ?
C25 C26 1.530(2) . ?
C25 C27 1.531(2) . ?
C28 C29 1.532(2) . ?
C28 C30 1.534(2) . ?

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
C21 Si1 C22 107.81(7) . . ?
C21 Si1 C25 107.26(7) . . ?
C21 Si1 C28 107.39(7) . . ?
C22 Si1 C25 110.80(7) . . ?
C22 Si1 C28 112.84(7) . . ?
C25 Si1 C28 110.49(7) . . ?
C2 C1 C8 121.13(13) . . ?
C2 C1 C19 131.66(13) . . ?
C8 C1 C19 107.20(12) . . ?
C1 C2 C3 120.67(12) . . ?
C1 C2 C7 119.35(12) . 2_566 ?
C7 C2 C3 119.98(12) 2_566 . ?
C2 C3 C4 112.64(12) . . ?
C3 C4 C5 110.82(12) . 2_566 ?
C6 C5 C4 112.03(12) . 2_566 ?
C7 C6 C5 120.56(12) . . ?
C7 C6 C8 119.19(13) . . ?
C8 C6 C5 120.25(12) . . ?
C2 C7 C7 119.35(15) 2_566 2_566 ?
C6 C7 C2 120.34(12) . 2_566 ?
C6 C7 C7 120.31(16) . 2_566 ?
C6 C8 C1 120.58(12) . . ?
C6 C8 C9 131.12(13) . . ?
C9 C8 C1 108.30(12) . . ?
C8 C9 C10 108.06(12) . . ?
C20 C9 C8 126.97(13) . . ?
C20 C9 C10 124.90(13) . . ?
C11 C10 C9 130.20(13) . . ?
C19 C10 C9 108.63(12) . . ?
C19 C10 C11 121.17(13) . . ?
C12 C11 C10 124.61(13) . . ?
C12 C11 C16 117.92(13) . . ?
C16 C11 C10 117.47(13) . . ?
C13 C12 C11 121.32(14) . . ?
C12 C13 C14 120.62(14) . . ?
C15 C14 C13 119.56(14) . . ?
C14 C15 C16 121.40(14) . . ?
C15 C16 C11 119.15(13) . . ?
C15 C16 C17 121.29(13) . . ?
C17 C16 C11 119.56(13) . . ?
C18 C17 C16 122.31(13) . . ?
C17 C18 C19 119.47(13) . . ?
C10 C19 C1 107.78(12) . . ?
C10 C19 C18 119.98(13) . . ?
C18 C19 C1 132.22(13) . . ?
C21 C20 C9 178.43(16) . . ?
C20 C21 Si1 175.94(13) . . ?
C23 C22 Si1 112.75(11) . . ?
C23 C22 C24 110.62(13) . . ?
C24 C22 Si1 111.00(10) . . ?
C26 C25 Si1 111.78(10) . . ?
C26 C25 C27 110.77(13) . . ?
C27 C25 Si1 111.86(10) . . ?
C29 C28 Si1 112.60(10) . . ?
C29 C28 C30 110.12(13) . . ?
C30 C28 Si1 114.47(11) . . ?

_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 1.202
_oxdiff_exptl_absorpt_empirical_full_min 0.873
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_TJ133_5_a
_database_code_depnum_ccdc_archive 'CCDC 1987611'
loop_
_audit_author_name
_audit_author_address
'Jerome Marrot'
;Institut Lavoisier de Versailles
France
;
_audit_update_record             
;
2020-03-02 deposited with the CCDC.	2020-10-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H60 O Si2'
_chemical_formula_weight         757.18

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.6952(3)
_cell_length_b                   12.3024(3)
_cell_length_c                   18.2803(5)
_cell_angle_alpha                72.9220(10)
_cell_angle_beta                 72.8590(10)
_cell_angle_gamma                66.6350(10)
_cell_volume                     2259.89(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9882
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      27.55

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_F_000             816
_exptl_transmission_factor_min   0.7016
_exptl_transmission_factor_max   0.7456
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.114
_shelx_estimated_absorpt_T_min   0.967
_shelx_estimated_absorpt_T_max   0.995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS (Sheldrick, V2014/5)'

_exptl_special_details           
; 
  'Blessing, Acta Cryst. (1995) A51, 33-38'  
;
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            55136
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.841
_diffrn_reflns_theta_max         27.592
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10425
_reflns_number_gt                7533
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1150P)²+1.1249P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10425
_refine_ls_number_parameters     509
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.1077
_refine_ls_R_factor_gt           0.0801
_refine_ls_wR_factor_ref         0.2323
_refine_ls_wR_factor_gt          0.2111
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

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 0.49449(4) 0.44086(4) 0.25655(3) 0.05499(13) Uani 1 1 d . . . . .
Si2 Si -0.14771(7) 0.85456(7) 0.94112(4) 0.0921(2) Uani 1 1 d . . . . .
C1 C 0.08913(12) 0.88613(12) 0.63727(8) 0.0384(4) Uani 1 1 d . . . . .
C2 C 0.09256(13) 0.91449(13) 0.70417(9) 0.0417(4) Uani 1 1 d . . . . .
C3 C 0.17988(13) 0.98196(13) 0.68292(9) 0.0426(4) Uani 1 1 d . . . . .
C4 C 0.21456(15) 1.03011(15) 0.72928(10) 0.0543(4) Uani 1 1 d . . . . .
H4 H 0.184166 1.017979 0.783051 0.065 Uiso 1 1 calc R U . . .
C5 C 0.29509(16) 1.09644(16) 0.69421(11) 0.0608(5) Uani 1 1 d . . . . .
H5 H 0.319694 1.128571 0.724743 0.073 Uiso 1 1 calc R U . . .
C6 C 0.33929(15) 1.11544(15) 0.61442(11) 0.0582(5) Uani 1 1 d . . . . .
H6 H 0.392189 1.161522 0.591762 0.070 Uiso 1 1 calc R U . . .
C7 C 0.30621(14) 1.06695(14) 0.56722(10) 0.0497(4) Uani 1 1 d . . . . .
H7 H 0.336231 1.080772 0.513424 0.060 Uiso 1 1 calc R U . . .
C8 C 0.22761(12) 0.99748(12) 0.60144(9) 0.0403(4) Uani 1 1 d . . . . .
C9 C 0.17461(12) 0.93287(12) 0.57116(8) 0.0373(3) Uani 1 1 d . . . . .
C10 C 0.19840(12) 0.90818(12) 0.49920(8) 0.0373(3) Uani 1 1 d . . . . .
C11 C 0.29377(14) 0.94929(14) 0.43221(9) 0.0478(4) Uani 1 1 d . . . . .
H11A H 0.361766 0.948936 0.452537 0.057 Uiso 1 1 calc R U . . .
H11B H 0.252493 1.031677 0.407041 0.057 Uiso 1 1 calc R U . . .
C12 C 0.35018(14) 0.86953(16) 0.37203(10) 0.0525(4) Uani 1 1 d . . . . .
H12A H 0.404130 0.903827 0.327745 0.063 Uiso 1 1 calc R U . . .
H12B H 0.402282 0.789875 0.394778 0.063 Uiso 1 1 calc R U . . .
C13 C 0.24603(14) 0.85879(15) 0.34476(9) 0.0496(4) Uani 1 1 d . . . . .
H13A H 0.283583 0.803310 0.309002 0.059 Uiso 1 1 calc R U . . .
H13B H 0.200358 0.937143 0.316659 0.059 Uiso 1 1 calc R U . . .
C14 C 0.15381(12) 0.81399(13) 0.41240(8) 0.0400(4) Uani 1 1 d . . . . .
C15 C 0.08791(13) 0.74773(13) 0.40264(9) 0.0433(4) Uani 1 1 d . . . . .
C16 C 0.10451(14) 0.70566(14) 0.32804(9) 0.0469(4) Uani 1 1 d . . . . .
C17 C 0.00251(14) 0.64794(14) 0.35201(10) 0.0532(4) Uani 1 1 d . . . . .
C18 C -0.03176(18) 0.60131(17) 0.30476(12) 0.0699(5) Uani 1 1 d . . . . .
H18 H 0.008752 0.602637 0.252592 0.084 Uiso 1 1 calc R U . . .
C19 C -0.12839(19) 0.55250(19) 0.33756(14) 0.0833(6) Uani 1 1 d . . . . .
H19 H -0.153937 0.521753 0.306700 0.100 Uiso 1 1 calc R U . . .
C20 C -0.18677(18) 0.54889(18) 0.41473(14) 0.0781(6) Uani 1 1 d . . . . .
H20 H -0.250549 0.514745 0.435430 0.094 Uiso 1 1 calc R U . . .
C21 C -0.15280(16) 0.59507(15) 0.46265(13) 0.0643(5) Uani 1 1 d . . . . .
H21 H -0.192603 0.591676 0.515042 0.077 Uiso 1 1 calc R U . . .
C22 C -0.05689(14) 0.64710(14) 0.43022(10) 0.0503(4) Uani 1 1 d . . . . .
C23 C -0.00183(12) 0.70971(13) 0.46132(9) 0.0436(4) Uani 1 1 d . . . . .
C24 C -0.02764(13) 0.73350(13) 0.53700(9) 0.0432(4) Uani 1 1 d . . . . .
C25 C -0.11439(15) 0.69355(15) 0.60102(11) 0.0558(4) Uani 1 1 d . . . . .
H25 H -0.159446 0.651237 0.593816 0.067 Uiso 1 1 calc R U . . .
C26 C -0.13317(16) 0.71607(16) 0.67336(11) 0.0623(5) Uani 1 1 d . . . . .
H26 H -0.190694 0.688929 0.714663 0.075 Uiso 1 1 calc R U . . .
C27 C -0.06797(15) 0.77836(15) 0.68559(10) 0.0543(4) Uani 1 1 d . . . . .
H27 H -0.082523 0.792906 0.735239 0.065 Uiso 1 1 calc R U . . .
C28 C 0.01959(13) 0.82041(12) 0.62550(9) 0.0402(4) Uani 1 1 d . . . . .
C29 C 0.04131(12) 0.79841(12) 0.54947(8) 0.0383(3) Uani 1 1 d . . . . .
C30 C 0.13133(12) 0.83994(12) 0.48612(8) 0.0370(3) Uani 1 1 d . . . . .
C31 C 0.02207(15) 0.89126(14) 0.78145(9) 0.0499(4) Uani 1 1 d . . . . .
C32 C -0.04015(19) 0.87637(18) 0.84652(11) 0.0657(5) Uani 1 1 d . . . . .
C33 C -0.2110(4) 0.7389(4) 0.9413(3) 0.2278(17) Uani 1 1 d D . . . .
H33 H -0.256617 0.781706 0.898313 0.273 Uiso 1 1 calc R U . . .
C34 C -0.1222(5) 0.6315(3) 0.9094(4) 0.228(3) Uani 1 1 d D . . . .
H34A H -0.058170 0.587114 0.940264 0.342 Uiso 1 1 calc R U . . .
H34B H -0.082612 0.656451 0.856377 0.342 Uiso 1 1 calc R U . . .
H34C H -0.168066 0.580977 0.910770 0.342 Uiso 1 1 calc R U . . .
C35 C -0.3148(5) 0.7134(5) 1.0021(3) 0.286(3) Uani 1 1 d D . . . .
H35A H -0.313147 0.633928 1.004259 0.429 Uiso 1 1 calc R U . . .
H35B H -0.394269 0.771923 0.990667 0.429 Uiso 1 1 calc R U . . .
H35C H -0.305466 0.717633 1.051543 0.429 Uiso 1 1 calc R U . . .
C36 C -0.0634(4) 0.8238(4) 1.01842(18) 0.1596(18) Uani 1 1 d D . . . .
H36 H -0.049199 0.899715 1.011975 0.192 Uiso 1 1 calc R U . . .
C37 C 0.0639(5) 0.7353(5) 1.0103(3) 0.227(3) Uani 1 1 d D . . . .
H37A H 0.108481 0.742197 1.044253 0.340 Uiso 1 1 calc R U . . .
H37B H 0.108650 0.749620 0.957131 0.340 Uiso 1 1 calc R U . . .
H37C H 0.058826 0.655582 1.024045 0.340 Uiso 1 1 calc R U . . .
C38 C -0.1453(6) 0.8089(6) 1.1002(2) 0.275(3) Uani 1 1 d . . . . .
H38A H -0.150965 0.729269 1.115593 0.412 Uiso 1 1 calc R U . . .
H38B H -0.228979 0.867966 1.100199 0.412 Uiso 1 1 calc R U . . .
H38C H -0.107602 0.820037 1.136289 0.412 Uiso 1 1 calc R U . . .
C39 C -0.2887(5) 0.9968(5) 0.9434(3) 0.266(3) Uani 1 1 d D . . . .
H39 H -0.348290 0.985550 0.993165 0.320 Uiso 1 1 calc R U . . .
C40 C -0.2627(6) 1.1025(4) 0.9362(4) 0.264(4) Uani 1 1 d D . . . .
H40A H -0.239607 1.136525 0.881877 0.396 Uiso 1 1 calc R U . . .
H40B H -0.193717 1.082779 0.961501 0.396 Uiso 1 1 calc R U . . .
H40C H -0.336956 1.160199 0.960328 0.396 Uiso 1 1 calc R U . . .
C41 C -0.3582(6) 1.0146(12) 0.8728(3) 0.527(11) Uani 1 1 d D . . . .
H41A H -0.365920 0.939388 0.873621 0.791 Uiso 1 1 calc R U . . .
H41B H -0.308014 1.039790 0.823440 0.791 Uiso 1 1 calc R U . . .
H41C H -0.441172 1.074951 0.879882 0.791 Uiso 1 1 calc R U . . .
C42 C 0.23217(14) 0.61535(14) 0.30919(9) 0.0477(4) Uani 1 1 d . . . . .
C43 C 0.33506(15) 0.54308(15) 0.29249(10) 0.0534(5) Uani 1 1 d . . . . .
C44 C 0.54965(19) 0.3211(2) 0.34269(16) 0.0898(9) Uani 1 1 d . . . . .
H44 H 0.636797 0.270680 0.323683 0.108 Uiso 1 1 calc R U . . .
C45 C 0.4710(3) 0.2389(3) 0.3755(3) 0.1605(18) Uani 1 1 d . . . . .
H45A H 0.504550 0.177325 0.417642 0.241 Uiso 1 1 calc R U . . .
H45B H 0.474025 0.201815 0.335146 0.241 Uiso 1 1 calc R U . . .
H45C H 0.384459 0.285297 0.394426 0.241 Uiso 1 1 calc R U . . .
C46 C 0.5547(3) 0.3742(4) 0.40602(17) 0.1427(16) Uani 1 1 d . . . . .
H46A H 0.473576 0.433822 0.420548 0.214 Uiso 1 1 calc R U . . .
H46B H 0.618990 0.411415 0.386910 0.214 Uiso 1 1 calc R U . . .
H46C H 0.574570 0.311231 0.450793 0.214 Uiso 1 1 calc R U . . .
C47 C 0.6029(2) 0.5312(2) 0.21043(15) 0.0799(7) Uani 1 1 d . . . . .
H47 H 0.585848 0.567094 0.157596 0.096 Uiso 1 1 calc R U . . .
C48 C 0.5780(3) 0.6356(2) 0.2438(2) 0.1317(13) Uani 1 1 d . . . . .
H48A H 0.576795 0.609696 0.298819 0.198 Uiso 1 1 calc R U . . .
H48B H 0.497142 0.694974 0.235447 0.198 Uiso 1 1 calc R U . . .
H48C H 0.643706 0.670399 0.218783 0.198 Uiso 1 1 calc R U . . .
C49 C 0.7434(2) 0.4533(2) 0.19732(18) 0.1042(9) Uani 1 1 d . . . . .
H49A H 0.794485 0.504436 0.176064 0.156 Uiso 1 1 calc R U . . .
H49B H 0.759928 0.402837 0.161444 0.156 Uiso 1 1 calc R U . . .
H49C H 0.764241 0.403486 0.246214 0.156 Uiso 1 1 calc R U . . .
C50 C 0.4709(3) 0.3777(2) 0.18240(16) 0.1032(8) Uani 1 1 d . . . . .
H50 H 0.409669 0.335837 0.210103 0.124 Uiso 1 1 calc R U . . .
C51 C 0.5909(4) 0.2840(3) 0.1484(2) 0.1956(13) Uani 1 1 d . . . . .
H51A H 0.568421 0.235455 0.126178 0.293 Uiso 1 1 calc R U . . .
H51B H 0.636436 0.233308 0.189028 0.293 Uiso 1 1 calc R U . . .
H51C H 0.643751 0.324112 0.108509 0.293 Uiso 1 1 calc R U . . .
C52 C 0.4113(4) 0.4768(4) 0.1184(2) 0.1819(16) Uani 1 1 d . . . . .
H52A H 0.473544 0.510963 0.083897 0.273 Uiso 1 1 calc R U . . .
H52B H 0.340976 0.538694 0.141479 0.273 Uiso 1 1 calc R U . . .
H52C H 0.381593 0.443260 0.089410 0.273 Uiso 1 1 calc R U . . .
O53 O 0.09091(11) 0.79978(11) 0.25985(7) 0.0603(3) Uani 1 1 d . . . . .
H53 H 0.016270 0.843960 0.263529 0.090 Uiso 1 1 calc R U . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 C43 1.8420(16) . ?
Si1 C47 1.868(2) . ?
Si1 C50 1.878(3) . ?
Si1 C44 1.884(2) . ?
Si2 C36 1.823(4) . ?
Si2 C32 1.8325(19) . ?
Si2 C33 1.845(5) . ?
Si2 C39 1.870(5) . ?
C1 C2 1.382(2) . ?
C1 C28 1.445(2) . ?
C1 C9 1.4581(19) . ?
C2 C31 1.421(2) . ?
C2 C3 1.460(2) . ?
C3 C4 1.386(3) . ?
C3 C8 1.412(2) . ?
C4 C5 1.382(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.379(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.390(3) . ?
C6 H6 0.9300 . ?
C7 C8 1.392(2) . ?
C7 H7 0.9300 . ?
C8 C9 1.474(2) . ?
C9 C10 1.361(2) . ?
C10 C30 1.459(2) . ?
C10 C11 1.509(2) . ?
C11 C12 1.517(2) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.508(3) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.510(2) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.398(2) . ?
C14 C30 1.402(2) . ?
C15 C23 1.379(2) . ?
C15 C16 1.531(2) . ?
C16 O53 1.4294(19) . ?
C16 C42 1.4791(19) . ?
C16 C17 1.517(3) . ?
C17 C18 1.383(3) . ?
C17 C22 1.392(2) . ?
C18 C19 1.387(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.370(3) . ?
C19 H19 0.9300 . ?
C20 C21 1.387(3) . ?
C20 H20 0.9300 . ?
C21 C22 1.405(3) . ?
C21 H21 0.9300 . ?
C22 C23 1.482(3) . ?
C23 C24 1.419(2) . ?
C24 C25 1.414(2) . ?
C24 C29 1.437(2) . ?
C25 C26 1.367(3) . ?
C25 H25 0.9300 . ?
C26 C27 1.372(3) . ?
C26 H26 0.9300 . ?
C27 C28 1.395(2) . ?
C27 H27 0.9300 . ?
C28 C29 1.424(2) . ?
C29 C30 1.4391(19) . ?
C31 C32 1.202(2) . ?
C33 C35 1.452(6) . ?
C33 C34 1.473(6) . ?
C33 H33 0.9800 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 C37 1.450(6) . ?
C36 C38 1.523(5) . ?
C36 H36 0.9800 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 C40 1.411(8) . ?
C39 C41 1.639(9) . ?
C39 H39 0.9800 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 C43 1.194(2) . ?
C44 C45 1.511(4) . ?
C44 C46 1.512(5) . ?
C44 H44 0.9800 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 C48 1.471(4) . ?
C47 C49 1.527(3) . ?
C47 H47 0.9800 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 C52 1.520(5) . ?
C50 C51 1.519(4) . ?
C50 H50 0.9800 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
O53 H53 0.8200 . ?

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
C43 Si1 C47 108.58(9) . . ?
C43 Si1 C50 104.67(10) . . ?
C47 Si1 C50 111.23(12) . . ?
C43 Si1 C44 107.67(9) . . ?
C47 Si1 C44 111.64(11) . . ?
C50 Si1 C44 112.66(13) . . ?
C36 Si2 C32 108.57(15) . . ?
C36 Si2 C33 117.1(2) . . ?
C32 Si2 C33 107.29(15) . . ?
C36 Si2 C39 111.5(2) . . ?
C32 Si2 C39 107.13(14) . . ?
C33 Si2 C39 104.8(3) . . ?
C2 C1 C28 131.04(13) . . ?
C2 C1 C9 109.15(14) . . ?
C28 C1 C9 119.80(14) . . ?
C1 C2 C31 129.07(16) . . ?
C1 C2 C3 108.24(13) . . ?
C31 C2 C3 122.62(16) . . ?
C4 C3 C8 121.10(15) . . ?
C4 C3 C2 129.88(14) . . ?
C8 C3 C2 109.00(15) . . ?
C5 C4 C3 118.87(16) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
C6 C5 C4 120.63(19) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C5 C6 C7 121.18(17) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 H6 119.4 . . ?
C6 C7 C8 119.20(16) . . ?
C6 C7 H7 120.4 . . ?
C8 C7 H7 120.4 . . ?
C7 C8 C3 118.96(16) . . ?
C7 C8 C9 134.23(15) . . ?
C3 C8 C9 106.79(13) . . ?
C10 C9 C1 121.45(14) . . ?
C10 C9 C8 131.72(13) . . ?
C1 C9 C8 106.71(13) . . ?
C9 C10 C30 119.68(12) . . ?
C9 C10 C11 121.40(15) . . ?
C30 C10 C11 118.92(13) . . ?
C10 C11 C12 112.46(14) . . ?
C10 C11 H11A 109.1 . . ?
C12 C11 H11A 109.1 . . ?
C10 C11 H11B 109.1 . . ?
C12 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
C13 C12 C11 110.43(12) . . ?
C13 C12 H12A 109.6 . . ?
C11 C12 H12A 109.6 . . ?
C13 C12 H12B 109.6 . . ?
C11 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
C12 C13 C14 111.64(13) . . ?
C12 C13 H13A 109.3 . . ?
C14 C13 H13A 109.3 . . ?
C12 C13 H13B 109.3 . . ?
C14 C13 H13B 109.3 . . ?
H13A C13 H13B 108.0 . . ?
C15 C14 C30 118.74(13) . . ?
C15 C14 C13 120.94(14) . . ?
C30 C14 C13 120.32(15) . . ?
C23 C15 C14 123.36(15) . . ?
C23 C15 C16 110.45(15) . . ?
C14 C15 C16 126.19(13) . . ?
O53 C16 C42 105.97(12) . . ?
O53 C16 C17 113.23(13) . . ?
C42 C16 C17 110.76(13) . . ?
O53 C16 C15 114.57(13) . . ?
C42 C16 C15 111.24(13) . . ?
C17 C16 C15 101.19(12) . . ?
C18 C17 C22 122.02(17) . . ?
C18 C17 C16 126.55(16) . . ?
C22 C17 C16 111.42(16) . . ?
C17 C18 C19 117.98(19) . . ?
C17 C18 H18 121.0 . . ?
C19 C18 H18 121.0 . . ?
C20 C19 C18 121.0(2) . . ?
C20 C19 H19 119.5 . . ?
C18 C19 H19 119.5 . . ?
C19 C20 C21 121.4(2) . . ?
C19 C20 H20 119.3 . . ?
C21 C20 H20 119.3 . . ?
C20 C21 C22 118.49(19) . . ?
C20 C21 H21 120.8 . . ?
C22 C21 H21 120.8 . . ?
C17 C22 C21 119.05(18) . . ?
C17 C22 C23 107.46(14) . . ?
C21 C22 C23 133.46(16) . . ?
C15 C23 C24 119.96(15) . . ?
C15 C23 C22 109.25(14) . . ?
C24 C23 C22 130.79(14) . . ?
C25 C24 C23 123.46(16) . . ?
C25 C24 C29 118.54(15) . . ?
C23 C24 C29 117.97(13) . . ?
C26 C25 C24 121.12(18) . . ?
C26 C25 H25 119.4 . . ?
C24 C25 H25 119.4 . . ?
C25 C26 C27 120.63(16) . . ?
C25 C26 H26 119.7 . . ?
C27 C26 H26 119.7 . . ?
C26 C27 C28 121.72(17) . . ?
C26 C27 H27 119.1 . . ?
C28 C27 H27 119.1 . . ?
C27 C28 C29 119.01(16) . . ?
C27 C28 C1 122.51(15) . . ?
C29 C28 C1 118.48(12) . . ?
C28 C29 C24 118.98(13) . . ?
C28 C29 C30 120.59(14) . . ?
C24 C29 C30 120.44(14) . . ?
C14 C30 C29 119.49(15) . . ?
C14 C30 C10 120.68(12) . . ?
C29 C30 C10 119.83(13) . . ?
C32 C31 C2 177.44(18) . . ?
C31 C32 Si2 174.2(2) . . ?
C35 C33 C34 112.4(4) . . ?
C35 C33 Si2 121.9(4) . . ?
C34 C33 Si2 118.2(3) . . ?
C35 C33 H33 99.2 . . ?
C34 C33 H33 99.2 . . ?
Si2 C33 H33 99.2 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C37 C36 C38 114.5(4) . . ?
C37 C36 Si2 116.1(3) . . ?
C38 C36 Si2 113.4(4) . . ?
C37 C36 H36 103.6 . . ?
C38 C36 H36 103.6 . . ?
Si2 C36 H36 103.6 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40 C39 C41 109.5(6) . . ?
C40 C39 Si2 115.7(4) . . ?
C41 C39 Si2 107.4(5) . . ?
C40 C39 H39 108.0 . . ?
C41 C39 H39 108.0 . . ?
Si2 C39 H39 108.0 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C42 C16 178.74(17) . . ?
C42 C43 Si1 174.18(15) . . ?
C45 C44 C46 110.9(3) . . ?
C45 C44 Si1 112.3(2) . . ?
C46 C44 Si1 112.24(19) . . ?
C45 C44 H44 107.0 . . ?
C46 C44 H44 107.0 . . ?
Si1 C44 H44 107.0 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C48 C47 C49 112.4(2) . . ?
C48 C47 Si1 116.90(18) . . ?
C49 C47 Si1 113.17(17) . . ?
C48 C47 H47 104.2 . . ?
C49 C47 H47 104.2 . . ?
Si1 C47 H47 104.2 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C52 C50 C51 111.4(3) . . ?
C52 C50 Si1 112.0(2) . . ?
C51 C50 Si1 113.4(2) . . ?
C52 C50 H50 106.5 . . ?
C51 C50 H50 106.5 . . ?
Si1 C50 H50 106.5 . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C50 C52 H52A 109.5 . . ?
C50 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C50 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C16 O53 H53 109.5 . . ?

_refine_diff_density_max         0.643
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.062

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_opera1909e
_database_code_depnum_ccdc_archive 'CCDC 1987609'
loop_
_audit_author_name
_audit_author_address
'Jerome Marrot'
;Institut Lavoisier de Versailles
France
;
_audit_update_record             
;
2020-03-02 deposited with the CCDC.	2020-10-20 downloaded from the CCDC.
;
_audit_creation_date             2019-09-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H66 Si2'
_chemical_formula_sum            'C60 H66 Si2'
_chemical_formula_weight         843.30
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.1631(3)
_cell_length_b                   13.8454(6)
_cell_length_c                   21.1693(8)
_cell_angle_alpha                90
_cell_angle_beta                 91.995(4)
_cell_angle_gamma                90
_cell_volume                     2391.13(18)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7081
_cell_measurement_temperature    123
_cell_measurement_theta_max      31.1090
_cell_measurement_theta_min      2.3590
_shelx_estimated_absorpt_T_max   0.999
_shelx_estimated_absorpt_T_min   0.967
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85036
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21124
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.423
_diffrn_ambient_temperature      123
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -23.00  73.00   0.50  120.00    --  -10.00  45.00   0.00  192
  2  ω    -80.00  71.00   0.50  120.00    --  -10.00  45.00 120.00  302
  3  ω    -98.00 -51.00   0.50  120.00    --  -10.00  45.00   0.00   94
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC HyPix-6000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0063090000
_diffrn_orient_matrix_UB_12      -0.0433339000
_diffrn_orient_matrix_UB_13      -0.0178638000
_diffrn_orient_matrix_UB_21      0.0739369000
_diffrn_orient_matrix_UB_22      -0.0168557000
_diffrn_orient_matrix_UB_23      0.0147199000
_diffrn_orient_matrix_UB_31      -0.0453633000
_diffrn_orient_matrix_UB_32      -0.0216057000
_diffrn_orient_matrix_UB_33      0.0241961000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              FR-E+
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4380
_reflns_number_total             5474
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 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)'
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         5474
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0421
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0465P)²+0.9999P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1027
_refine_special_details          ?
_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:
 C28(H28), C23(H23), C25(H25)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C5(H5A,H5B), C6(H6A,H6B)
2.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C11(H11), C14(H14), C15(H15), C12(H12), C16(H16)
2.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C24(H24A,H24B,H24C), C27(H27A,H27B,H27C), C29(H29A,H29B,
 H29C), C31(H31A,H31B,H31C), C26(H26A,H26B,H26C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.29062(5) 0.43090(3) 0.70995(2) 0.01637(10) Uani 1 1 d . . . . .
C19 C 0.94257(16) 0.53343(10) 0.51385(6) 0.0150(3) Uani 1 1 d . . . . .
C3 C 1.12721(16) 0.66854(10) 0.49811(6) 0.0155(3) Uani 1 1 d . . . . .
C2 C 0.80015(16) 0.23476(10) 0.50726(6) 0.0167(3) Uani 1 1 d . . . . .
C8 C 0.79884(16) 0.49726(10) 0.53859(6) 0.0158(3) Uani 1 1 d . . . . .
C9 C 0.77161(16) 0.39682(10) 0.53769(6) 0.0158(3) Uani 1 1 d . . . . .
C1 C 0.67976(16) 0.24168(11) 0.55304(6) 0.0178(3) Uani 1 1 d . . . . .
C4 C 0.98110(16) 0.63532(10) 0.51934(6) 0.0153(3) Uani 1 1 d . . . . .
C7 C 0.66978(17) 0.56363(10) 0.56368(7) 0.0195(3) Uani 1 1 d . . . . .
H7A H 0.684358 0.568996 0.610171 0.023 Uiso 1 1 calc R . . . .
H7B H 0.559687 0.536274 0.554035 0.023 Uiso 1 1 calc R . . . .
C10 C 0.65883(16) 0.34154(10) 0.57051(6) 0.0173(3) Uani 1 1 d . . . . .
C18 C 0.82173(16) 0.14449(10) 0.47614(7) 0.0179(3) Uani 1 1 d . . . . .
C5 C 0.85429(17) 0.70125(10) 0.54621(7) 0.0179(3) Uani 1 1 d . . . . .
H5A H 0.863342 0.766013 0.526821 0.021 Uiso 1 1 calc R . . . .
H5B H 0.875756 0.708138 0.592301 0.021 Uiso 1 1 calc R . . . .
C20 C 0.54599(17) 0.37192(10) 0.61592(6) 0.0181(3) Uani 1 1 d . . . . .
C6 C 0.68195(17) 0.66286(11) 0.53421(7) 0.0199(3) Uani 1 1 d . . . . .
H6A H 0.601523 0.706980 0.552969 0.024 Uiso 1 1 calc R . . . .
H6B H 0.657216 0.658837 0.488166 0.024 Uiso 1 1 calc R . . . .
C13 C 0.74465(17) 0.06135(11) 0.50222(7) 0.0212(3) Uani 1 1 d . . . . .
C17 C 0.90465(17) 0.13147(11) 0.41882(7) 0.0203(3) Uani 1 1 d . . . . .
H17 H 0.946470 0.186214 0.397651 0.024 Uiso 1 1 calc R . . . .
C28 C 0.08838(18) 0.38927(11) 0.67392(7) 0.0216(3) Uani 1 1 d . . . . .
H28 H 0.063220 0.433010 0.637265 0.026 Uiso 1 1 calc R . . . .
C11 C 0.59846(18) 0.15989(11) 0.57597(7) 0.0221(3) Uani 1 1 d . . . . .
H11 H 0.518338 0.166371 0.607179 0.027 Uiso 1 1 calc R . . . .
C23 C 0.34693(18) 0.37542(12) 0.78908(7) 0.0236(3) Uani 1 1 d . . . . .
H23 H 0.265136 0.398227 0.819847 0.028 Uiso 1 1 calc R . . . .
C21 C 0.44717(17) 0.39332(11) 0.65465(7) 0.0197(3) Uani 1 1 d . . . . .
C14 C 0.77292(18) -0.03038(11) 0.47531(8) 0.0254(3) Uani 1 1 d . . . . .
H14 H 0.727651 -0.086087 0.494242 0.031 Uiso 1 1 calc R . . . .
C15 C 0.86320(19) -0.04075(12) 0.42307(8) 0.0279(4) Uani 1 1 d . . . . .
H15 H 0.884153 -0.103206 0.406611 0.033 Uiso 1 1 calc R . . . .
C12 C 0.63635(19) 0.07167(11) 0.55277(7) 0.0240(3) Uani 1 1 d . . . . .
H12 H 0.589454 0.015668 0.570732 0.029 Uiso 1 1 calc R . . . .
C16 C 0.92528(19) 0.04168(11) 0.39363(8) 0.0249(3) Uani 1 1 d . . . . .
H16 H 0.982546 0.034898 0.355573 0.030 Uiso 1 1 calc R . . . .
C30 C 0.0934(2) 0.28683(12) 0.64720(8) 0.0270(3) Uani 1 1 d . . . . .
H30A H 0.180670 0.282280 0.616686 0.041 Uiso 1 1 calc GR . . . .
H30B H -0.012172 0.271652 0.626080 0.041 Uiso 1 1 calc GR . . . .
H30C H 0.115039 0.240871 0.681696 0.041 Uiso 1 1 calc GR . . . .
C25 C 0.30482(19) 0.56665(11) 0.71498(7) 0.0242(3) Uani 1 1 d . . . . .
H25 H 0.422639 0.582142 0.724773 0.029 Uiso 1 1 calc R . . . .
C24 C 0.5164(2) 0.41005(14) 0.81288(8) 0.0332(4) Uani 1 1 d . . . . .
H24A H 0.599467 0.388235 0.783765 0.050 Uiso 1 1 calc GR . . . .
H24B H 0.540722 0.383309 0.855032 0.050 Uiso 1 1 calc GR . . . .
H24C H 0.517280 0.480751 0.815072 0.050 Uiso 1 1 calc GR . . . .
C27 C 0.2609(2) 0.61507(12) 0.65180(8) 0.0324(4) Uani 1 1 d . . . . .
H27A H 0.324202 0.585402 0.618439 0.049 Uiso 1 1 calc GR . . . .
H27B H 0.286651 0.684106 0.654514 0.049 Uiso 1 1 calc GR . . . .
H27C H 0.143526 0.606762 0.641930 0.049 Uiso 1 1 calc GR . . . .
C29 C -0.0545(2) 0.39924(15) 0.71837(9) 0.0370(4) Uani 1 1 d . . . . .
H29A H -0.034173 0.358603 0.755727 0.055 Uiso 1 1 calc GR . . . .
H29B H -0.156227 0.378699 0.696385 0.055 Uiso 1 1 calc GR . . . .
H29C H -0.064552 0.466812 0.731463 0.055 Uiso 1 1 calc GR . . . .
C31 C 0.3415(2) 0.26476(13) 0.78836(8) 0.0377(4) Uani 1 1 d . . . . .
H31A H 0.228629 0.243162 0.779718 0.057 Uiso 1 1 calc GR . . . .
H31B H 0.380519 0.239936 0.829550 0.057 Uiso 1 1 calc GR . . . .
H31C H 0.411968 0.240420 0.755353 0.057 Uiso 1 1 calc GR . . . .
C26 C 0.2071(2) 0.61198(13) 0.76790(9) 0.0380(4) Uani 1 1 d . . . . .
H26A H 0.089537 0.604090 0.758266 0.057 Uiso 1 1 calc GR . . . .
H26B H 0.233303 0.680900 0.771223 0.057 Uiso 1 1 calc GR . . . .
H26C H 0.235849 0.579931 0.808041 0.057 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 C28 1.8846(15) . ?
Si1 C23 1.8851(15) . ?
Si1 C21 1.8380(15) . ?
Si1 C25 1.8859(16) . ?
C19 C19 1.455(3) 3_766 ?
C19 C8 1.3945(19) . ?
C19 C4 1.449(2) . ?
C3 C2 1.4704(19) 3_766 ?
C3 C9 1.4556(19) 3_766 ?
C3 C4 1.3687(19) . ?
C2 C1 1.4073(19) . ?
C2 C18 1.427(2) . ?
C8 C9 1.408(2) . ?
C8 C7 1.5084(19) . ?
C9 C10 1.4002(19) . ?
C1 C10 1.443(2) . ?
C1 C11 1.407(2) . ?
C4 C5 1.5064(18) . ?
C7 C6 1.514(2) . ?
C10 C20 1.4180(19) . ?
C18 C13 1.432(2) . ?
C18 C17 1.421(2) . ?
C5 C6 1.5170(19) . ?
C20 C21 1.207(2) . ?
C13 C14 1.414(2) . ?
C13 C12 1.419(2) . ?
C17 C16 1.365(2) . ?
C28 C30 1.528(2) . ?
C28 C29 1.530(2) . ?
C11 C12 1.356(2) . ?
C23 C24 1.532(2) . ?
C23 C31 1.533(2) . ?
C14 C15 1.358(2) . ?
C15 C16 1.404(2) . ?
C25 C27 1.528(2) . ?
C25 C26 1.532(2) . ?

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
C28 Si1 C23 114.71(7) . . ?
C28 Si1 C25 112.26(7) . . ?
C23 Si1 C25 110.08(7) . . ?
C21 Si1 C28 105.93(7) . . ?
C21 Si1 C23 107.29(7) . . ?
C21 Si1 C25 105.98(7) . . ?
C8 C19 C19 119.02(16) . 3_766 ?
C8 C19 C4 120.17(12) . . ?
C4 C19 C19 120.70(15) . 3_766 ?
C9 C3 C2 106.74(11) 3_766 3_766 ?
C4 C3 C2 133.61(13) . 3_766 ?
C4 C3 C9 118.61(13) . 3_766 ?
C1 C2 C3 106.52(12) . 3_766 ?
C1 C2 C18 118.56(13) . . ?
C18 C2 C3 134.87(12) . 3_766 ?
C19 C8 C9 118.94(12) . . ?
C19 C8 C7 121.37(13) . . ?
C9 C8 C7 119.64(12) . . ?
C8 C9 C3 121.92(12) . 3_766 ?
C10 C9 C3 108.26(12) . 3_766 ?
C10 C9 C8 129.73(13) . . ?
C2 C1 C10 109.49(12) . . ?
C2 C1 C11 122.12(13) . . ?
C11 C1 C10 128.39(13) . . ?
C19 C4 C5 118.04(12) . . ?
C3 C4 C19 119.33(12) . . ?
C3 C4 C5 122.58(13) . . ?
C8 C7 C6 110.56(11) . . ?
C9 C10 C1 108.10(12) . . ?
C9 C10 C20 128.90(13) . . ?
C20 C10 C1 122.93(13) . . ?
C2 C18 C13 117.60(13) . . ?
C17 C18 C2 125.14(13) . . ?
C17 C18 C13 117.12(13) . . ?
C4 C5 C6 111.71(12) . . ?
C21 C20 C10 176.87(15) . . ?
C7 C6 C5 108.83(12) . . ?
C14 C13 C18 119.12(14) . . ?
C14 C13 C12 120.60(14) . . ?
C12 C13 C18 120.24(14) . . ?
C16 C17 C18 121.19(14) . . ?
C30 C28 Si1 113.52(10) . . ?
C30 C28 C29 110.02(13) . . ?
C29 C28 Si1 113.53(11) . . ?
C12 C11 C1 118.92(13) . . ?
C24 C23 Si1 110.74(11) . . ?
C24 C23 C31 109.96(14) . . ?
C31 C23 Si1 113.11(11) . . ?
C20 C21 Si1 176.44(13) . . ?
C15 C14 C13 121.60(15) . . ?
C14 C15 C16 119.36(15) . . ?
C11 C12 C13 121.32(14) . . ?
C17 C16 C15 121.03(14) . . ?
C27 C25 Si1 112.07(11) . . ?
C27 C25 C26 110.36(14) . . ?
C26 C25 Si1 114.64(12) . . ?

_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 1.207
_oxdiff_exptl_absorpt_empirical_full_min 0.810
