#------------------------------------------------------------------------------
#$Date: 2022-10-07 04:07:08 +0300 (Fri, 07 Oct 2022) $
#$Revision: 278445 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/17/7061782.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7061782
loop_
_publ_author_name
'Goncharova, Irina K.'
'Ulianova, Eva A.'
'Novikov, Roman A.'
'Volodin, Alexander D.'
'Korlyukov, Alexander A.'
'Arzumanyan, Ashot V.'
_publ_section_title
;
 Siloxane-containing derivatives of benzoic acid: chemical transformation
 of the carboxyl group
;
_journal_issue                   37
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18041
_journal_page_last               18047
_journal_paper_doi               10.1039/D2NJ03872B
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C20 H28 N2 O3 Si2, C10 H15 N O2 Si'
_chemical_formula_sum            'C30 H43 N3 O5 Si3'
_chemical_formula_weight         609.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-08-27
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-08-27 deposited with the CCDC.	2022-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.806(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6295(8)
_cell_length_b                   14.8131(8)
_cell_length_c                   17.2611(9)
_cell_measurement_reflns_used    4391
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.848
_cell_measurement_theta_min      2.333
_cell_volume                     3278.8(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX3 v2019.11-0 (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'APEX QUEST'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0775
_diffrn_reflns_av_unetI/netI     0.0827
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20592
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         1.861
_exptl_absorpt_coefficient_mu    0.186
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1063 before and 0.0658 after correction.
The Ratio of minimum to maximum transmission is 0.7392.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.217
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         6426
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.216
_refine_ls_R_factor_all          0.1534
_refine_ls_R_factor_gt           0.1288
_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)+(0.0002P)²+37.1785P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2798
_refine_ls_wR_factor_ref         0.2902
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4962
_reflns_number_total             6426
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2nj03872b4.cif
_cod_data_source_block           ye105
_cod_depositor_comments
'Adding full bibliography for 7061778--7061786.cif.'
_cod_database_code               7061782
_shelxl_version_number           2014/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.959
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C27) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
3. Others
 Fixed Sof: C27A(0.5) H27A(0.5) C14(0.5) H14(0.5) C15A(0.5) H15A(0.5) C9A(0.5)
 H9A(0.5) C6A(0.5) H6A(0.5) C28A(0.5) H28A(0.5) C27(0.5) H27(0.5) C25(0.5)
 H25(0.5) C10(0.5) H10(0.5) C25A(0.5) H25A(0.5) C24(0.5) H24(0.5) C9(0.5)
 H9(0.5) C24A(0.5) H24A(0.5) C17(0.5) H17(0.5) C18A(0.5) H18A(0.5) C18(0.5)
 H18(0.5) C15(0.5) H15(0.5) C10A(0.5) H10A(0.5) C7(0.5) H7(0.5) C17A(0.5)
 H17A(0.5) C14A(0.5) H14A(0.5) C28(0.5) H28(0.5) C7A(0.5) H7A(0.5) C6(0.5)
 H6(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), N1(H1), C27A(H27A), C14(H14), C15A(H15A), C9A(H9A), C6A(H6A),
 C28A(H28A), C27(H27), C25(H25), C10(H10), C25A(H25A), C24(H24), C9(H9),
 C24A(H24A), C17(H17), C18A(H18A), C18(H18), C15(H15), C10A(H10A), C7(H7),
 C17A(H17A), C14A(H14A), C28(H28), C7A(H7A), C6(H6)
4.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C2(H2A,H2B,H2C), C20(H20A,H20B,H20C), C30(H30A,H30B,
 H30C), C22(H22A,H22B,H22C), C3(H3A,H3B,H3C), C21(H21A,H21B,H21C), C1(H1A,H1B,
 H1C), C4(H4A,H4B,H4C)
4.c Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.17743(16) 0.33826(14) 0.97190(12) 0.0199(4) Uani 1 1 d . . . . .
Si2 Si 0.18639(17) 0.55151(14) 0.95853(13) 0.0237(5) Uani 1 1 d . . . . .
Si3 Si 0.28963(16) 0.43221(14) 0.48683(13) 0.0254(5) Uani 1 1 d . . . . .
O1 O 0.1510(4) 0.4458(4) 0.9522(3) 0.0275(12) Uani 1 1 d . . . . .
O5 O -0.0247(5) 0.3102(3) 0.7081(3) 0.0291(13) Uani 1 1 d . . . . .
O4 O 0.2496(5) 0.3646(4) 0.4069(3) 0.0355(14) Uani 1 1 d . . . . .
H4 H 0.1844 0.3672 0.3861 0.053 Uiso 1 1 calc R U . . .
N2 N 0.5375(5) 0.6272(4) 0.7519(4) 0.0212(13) Uani 1 1 d . . . . .
H2 H 0.5173 0.6799 0.7645 0.025 Uiso 1 1 calc R U . . .
N3 N -0.0398(5) 0.4612(4) 0.7176(4) 0.0221(13) Uani 1 1 d . . . . .
H3 H -0.0200 0.5148 0.7065 0.026 Uiso 1 1 calc R U . . .
N1 N 0.5399(5) 0.2944(4) 0.7758(4) 0.0225(14) Uani 1 1 d . . . . .
H1 H 0.5123 0.3486 0.7727 0.027 Uiso 1 1 calc R U . . .
O3 O 0.5214(6) 0.4768(4) 0.7524(5) 0.058(2) Uani 1 1 d . . . A 2
C12 C 0.6218(6) 0.2800(5) 0.7408(5) 0.0241(16) Uani 1 1 d . . . . .
H12A H 0.6185 0.3275 0.7004 0.036 Uiso 1 1 calc R U . . .
H12B H 0.6122 0.2210 0.7136 0.036 Uiso 1 1 calc R U . . .
H12C H 0.6899 0.2818 0.7847 0.036 Uiso 1 1 calc R U . . .
C5 C 0.2753(5) 0.3010(5) 0.9233(4) 0.0200(15) Uani 1 1 d . . . . .
C2 C 0.0544(6) 0.2761(5) 0.9261(5) 0.0251(16) Uani 1 1 d . . . . .
H2A H 0.0071 0.2900 0.9565 0.038 Uiso 1 1 calc R U . . .
H2B H 0.0686 0.2111 0.9291 0.038 Uiso 1 1 calc R U . . .
H2C H 0.0218 0.2941 0.8684 0.038 Uiso 1 1 calc R U . . .
C20 C 0.6135(6) 0.6232(5) 0.7093(5) 0.0236(16) Uani 1 1 d . . . . .
H20A H 0.5811 0.5962 0.6547 0.035 Uiso 1 1 calc R U . . .
H20B H 0.6732 0.5863 0.7414 0.035 Uiso 1 1 calc R U . . .
H20C H 0.6374 0.6844 0.7033 0.035 Uiso 1 1 calc R U . . .
C11 C 0.5042(6) 0.2278(4) 0.8131(4) 0.0192(15) Uani 1 1 d . . . . .
C29 C -0.0033(6) 0.3875(5) 0.6916(4) 0.0226(16) Uani 1 1 d . . . . .
C23 C 0.2032(6) 0.4204(5) 0.5504(5) 0.0231(16) Uani 1 1 d . . . . .
C30 C -0.1116(6) 0.4550(5) 0.7637(5) 0.0283(17) Uani 1 1 d . . . . .
H30A H -0.1669 0.5001 0.7430 0.042 Uiso 1 1 calc R U . . .
H30B H -0.0736 0.4662 0.8222 0.042 Uiso 1 1 calc R U . . .
H30C H -0.1425 0.3945 0.7569 0.042 Uiso 1 1 calc R U . . .
C8 C 0.4231(6) 0.2530(4) 0.8492(4) 0.0186(15) Uani 1 1 d . . . . .
C26 C 0.0679(6) 0.4024(5) 0.6431(4) 0.0184(14) Uani 1 1 d . . . . .
C19 C 0.4985(6) 0.5522(5) 0.7716(5) 0.0276(17) Uani 1 1 d . . . . .
C13 C 0.2833(6) 0.5634(5) 0.9039(5) 0.0293(17) Uani 1 1 d . . . . .
C22 C 0.2853(7) 0.5536(6) 0.4527(5) 0.0327(18) Uani 1 1 d . . . . .
H22A H 0.3307 0.5613 0.4197 0.049 Uiso 1 1 calc R U . . .
H22B H 0.3093 0.5928 0.5012 0.049 Uiso 1 1 calc R U . . .
H22C H 0.2136 0.5696 0.4196 0.049 Uiso 1 1 calc R U . . .
C16 C 0.4231(6) 0.5619(5) 0.8176(5) 0.0268(17) Uani 1 1 d . . . . .
C3 C 0.0684(7) 0.6185(6) 0.9066(5) 0.036(2) Uani 1 1 d . . . . .
H3A H 0.0429 0.6042 0.8476 0.053 Uiso 1 1 calc R U . . .
H3B H 0.0853 0.6829 0.9141 0.053 Uiso 1 1 calc R U . . .
H3C H 0.0144 0.6040 0.9303 0.053 Uiso 1 1 calc R U . . .
C21 C 0.4250(6) 0.4016(6) 0.5466(5) 0.0328(19) Uani 1 1 d . . . . .
H21A H 0.4283 0.3374 0.5611 0.049 Uiso 1 1 calc R U . . .
H21B H 0.4491 0.4380 0.5969 0.049 Uiso 1 1 calc R U . . .
H21C H 0.4696 0.4130 0.5135 0.049 Uiso 1 1 calc R U . . .
C1 C 0.2334(6) 0.3221(6) 1.0852(4) 0.0306(18) Uani 1 1 d . . . . .
H1A H 0.3031 0.3491 1.1059 0.046 Uiso 1 1 calc R U . . .
H1B H 0.2384 0.2574 1.0978 0.046 Uiso 1 1 calc R U . . .
H1C H 0.1883 0.3511 1.1115 0.046 Uiso 1 1 calc R U . . .
C4 C 0.2441(7) 0.5877(7) 1.0673(5) 0.043(2) Uani 1 1 d . . . . .
H4A H 0.1924 0.5808 1.0949 0.064 Uiso 1 1 calc R U . . .
H4B H 0.2652 0.6512 1.0694 0.064 Uiso 1 1 calc R U . . .
H4C H 0.3052 0.5504 1.0953 0.064 Uiso 1 1 calc R U . . .
C27A C 0.0604(11) 0.4774(9) 0.5906(8) 0.017(3) Uani 0.5 1 d . . P B 2
H27A H 0.0083 0.5217 0.5860 0.020 Uiso 0.5 1 calc R U P B 2
C14 C 0.2761(11) 0.6198(10) 0.8425(9) 0.022(3) Uani 0.5 1 d . . P C 1
H14 H 0.2191 0.6607 0.8257 0.026 Uiso 0.5 1 calc R U P C 1
C15A C 0.4376(11) 0.6115(9) 0.8794(9) 0.020(3) Uani 0.5 1 d . . P C 2
H15A H 0.4986 0.6478 0.8982 0.024 Uiso 0.5 1 calc R U P C 2
C9A C 0.3376(10) 0.3095(9) 0.8057(7) 0.017(3) Uani 0.5 1 d . . P D 2
H9A H 0.3300 0.3317 0.7523 0.020 Uiso 0.5 1 calc R U P D 2
C6A C 0.3520(13) 0.2394(11) 0.9587(10) 0.030(4) Uani 0.5 1 d . . P D 2
H6A H 0.3541 0.2117 1.0089 0.036 Uiso 0.5 1 calc R U P D 2
C28A C 0.1267(12) 0.4881(10) 0.5459(9) 0.023(3) Uani 0.5 1 d . . P B 2
H28A H 0.1215 0.5400 0.5125 0.028 Uiso 0.5 1 calc R U P B 2
C27 C 0.1292(12) 0.4755(10) 0.6545(10) 0.028(3) Uani 0.5 1 d . U P B 1
H27 H 0.1281 0.5202 0.6937 0.033 Uiso 0.5 1 calc R U P B 1
C25 C 0.0738(14) 0.3309(10) 0.5928(10) 0.025(3) Uani 0.5 1 d . . P B 1
H25 H 0.0339 0.2776 0.5890 0.030 Uiso 0.5 1 calc R U P B 1
C10 C 0.3731(11) 0.3438(9) 0.9470(8) 0.019(3) Uani 0.5 1 d . . P D 1
H10 H 0.3893 0.3883 0.9891 0.022 Uiso 0.5 1 calc R U P D 1
C25A C 0.1432(14) 0.3371(10) 0.6432(10) 0.026(3) Uani 0.5 1 d . . P B 2
H25A H 0.1485 0.2836 0.6747 0.032 Uiso 0.5 1 calc R U P B 2
C24 C 0.1396(14) 0.3411(10) 0.5494(10) 0.027(4) Uani 0.5 1 d . . P B 1
H24 H 0.1445 0.2922 0.5153 0.033 Uiso 0.5 1 calc R U P B 1
C9 C 0.4462(12) 0.3230(10) 0.9109(10) 0.026(3) Uani 0.5 1 d . . P D 1
H9 H 0.5107 0.3544 0.9263 0.031 Uiso 0.5 1 calc R U P D 1
C24A C 0.2099(14) 0.3490(11) 0.5984(11) 0.027(3) Uani 0.5 1 d . . P B 2
H24A H 0.2618 0.3047 0.6023 0.033 Uiso 0.5 1 calc R U P B 2
C17 C 0.4494(13) 0.5111(10) 0.8949(9) 0.025(3) Uani 0.5 1 d . . P C 1
H17 H 0.5123 0.4774 0.9145 0.030 Uiso 0.5 1 calc R U P C 1
C18A C 0.2549(12) 0.5097(11) 0.8245(9) 0.027(3) Uani 0.5 1 d . . P C 2
H18A H 0.1903 0.4786 0.8036 0.033 Uiso 0.5 1 calc R U P C 2
C18 C 0.3826(11) 0.5128(10) 0.9382(8) 0.020(3) Uani 0.5 1 d . . P C 1
H18 H 0.3991 0.4822 0.9894 0.024 Uiso 0.5 1 calc R U P C 1
C15 C 0.3491(12) 0.6218(10) 0.8012(10) 0.026(3) Uani 0.5 1 d . . P C 1
H15 H 0.3444 0.6671 0.7611 0.031 Uiso 0.5 1 calc R U P C 1
C10A C 0.2651(10) 0.3314(11) 0.8440(8) 0.022(3) Uani 0.5 1 d . . P D 2
H10A H 0.2070 0.3681 0.8153 0.026 Uiso 0.5 1 calc R U P D 2
C7 C 0.3314(12) 0.2070(10) 0.8311(8) 0.022(3) Uani 0.5 1 d . . P D 1
H7 H 0.3173 0.1575 0.7940 0.027 Uiso 0.5 1 calc R U P D 1
C17A C 0.3267(11) 0.5076(9) 0.7832(9) 0.021(3) Uani 0.5 1 d . . P C 2
H17A H 0.3144 0.4725 0.7348 0.026 Uiso 0.5 1 calc R U P C 2
C14A C 0.3656(12) 0.6145(10) 0.9217(9) 0.026(3) Uani 0.5 1 d . . P C 2
H14A H 0.3778 0.6562 0.9657 0.031 Uiso 0.5 1 calc R U P C 2
C28 C 0.1955(14) 0.4853(10) 0.6074(11) 0.031(4) Uani 0.5 1 d . . P B 1
H28 H 0.2369 0.5383 0.6146 0.037 Uiso 0.5 1 calc R U P B 1
C7A C 0.4280(11) 0.2151(9) 0.9239(9) 0.021(3) Uani 0.5 1 d . . P D 2
H7A H 0.4817 0.1735 0.9511 0.025 Uiso 0.5 1 calc R U P D 2
C6 C 0.2596(12) 0.2324(11) 0.8665(10) 0.029(4) Uani 0.5 1 d . . P D 1
H6 H 0.1952 0.2008 0.8510 0.035 Uiso 0.5 1 calc R U P D 1
O2 O 0.5389(4) 0.1493(3) 0.8179(3) 0.0243(11) Uani 1 1 d . . . . .
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'
N N 0.0061 0.0033 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Si1 C5 109.3(3) . . ?
O1 Si1 C2 107.0(3) . . ?
O1 Si1 C1 109.1(3) . . ?
C2 Si1 C5 110.0(3) . . ?
C2 Si1 C1 112.1(4) . . ?
C1 Si1 C5 109.3(3) . . ?
O1 Si2 C13 107.4(3) . . ?
O1 Si2 C3 107.2(4) . . ?
O1 Si2 C4 111.1(4) . . ?
C3 Si2 C13 110.6(4) . . ?
C3 Si2 C4 109.8(4) . . ?
C4 Si2 C13 110.7(4) . . ?
O4 Si3 C23 109.9(3) . . ?
O4 Si3 C22 110.7(4) . . ?
O4 Si3 C21 107.7(4) . . ?
C23 Si3 C22 108.2(3) . . ?
C21 Si3 C23 111.1(4) . . ?
C21 Si3 C22 109.2(4) . . ?
Si2 O1 Si1 151.4(4) . . ?
Si3 O4 H4 109.5 . . ?
C20 N2 H2 119.6 . . ?
C19 N2 H2 119.6 . . ?
C19 N2 C20 120.7(6) . . ?
C29 N3 H3 119.1 . . ?
C29 N3 C30 121.7(6) . . ?
C30 N3 H3 119.1 . . ?
C12 N1 H1 118.7 . . ?
C11 N1 H1 118.7 . . ?
C11 N1 C12 122.7(6) . . ?
N1 C12 H12A 109.5 . . ?
N1 C12 H12B 109.5 . . ?
N1 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C6A C5 Si1 123.1(8) . . ?
C6A C5 C10A 117.3(10) . . ?
C10 C5 Si1 118.9(7) . . ?
C10A C5 Si1 119.3(7) . . ?
C6 C5 Si1 124.8(8) . . ?
C6 C5 C10 116.3(9) . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 C20 H20A 109.5 . . ?
N2 C20 H20B 109.5 . . ?
N2 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N1 C11 C8 116.9(6) . . ?
O2 C11 N1 121.5(6) . . ?
O2 C11 C8 121.6(6) . . ?
O5 C29 N3 122.2(6) . . ?
O5 C29 C26 120.8(6) . . ?
N3 C29 C26 116.9(6) . . ?
C28A C23 Si3 119.7(7) . . ?
C24 C23 Si3 124.0(7) . . ?
C24A C23 Si3 121.1(8) . . ?
C24A C23 C28A 119.1(10) . . ?
C28 C23 Si3 123.9(8) . . ?
C28 C23 C24 112.0(9) . . ?
N3 C30 H30A 109.5 . . ?
N3 C30 H30B 109.5 . . ?
N3 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C9A C8 C11 121.1(7) . . ?
C9 C8 C11 118.8(8) . . ?
C7 C8 C11 122.1(8) . . ?
C7 C8 C9 118.8(10) . . ?
C7A C8 C11 118.7(8) . . ?
C7A C8 C9A 120.1(9) . . ?
C27A C26 C29 123.6(8) . . ?
C27 C26 C29 121.7(8) . . ?
C27 C26 C25 122.8(10) . . ?
C25 C26 C29 115.1(8) . . ?
C25A C26 C29 120.5(8) . . ?
C25A C26 C27A 115.7(9) . . ?
N2 C19 C16 117.5(6) . . ?
O3 C19 N2 122.0(7) . . ?
O3 C19 C16 120.5(7) . . ?
C14 C13 Si2 125.9(8) . . ?
C14 C13 C18 116.6(10) . . ?
C18A C13 Si2 113.4(7) . . ?
C18 C13 Si2 117.1(7) . . ?
C14A C13 Si2 129.4(8) . . ?
C14A C13 C18A 117.0(10) . . ?
Si3 C22 H22A 109.5 . . ?
Si3 C22 H22B 109.5 . . ?
Si3 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C15A C16 C19 124.4(9) . . ?
C15A C16 C17A 121.4(10) . . ?
C17 C16 C19 115.6(8) . . ?
C15 C16 C19 124.6(9) . . ?
C15 C16 C17 118.7(10) . . ?
C17A C16 C19 114.2(8) . . ?
Si2 C3 H3A 109.5 . . ?
Si2 C3 H3B 109.5 . . ?
Si2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si3 C21 H21A 109.5 . . ?
Si3 C21 H21B 109.5 . . ?
Si3 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si1 C1 H1A 109.5 . . ?
Si1 C1 H1B 109.5 . . ?
Si1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si2 C4 H4A 109.5 . . ?
Si2 C4 H4B 109.5 . . ?
Si2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C26 C27A H27A 119.1 . . ?
C28A C27A C26 121.9(11) . . ?
C28A C27A H27A 119.1 . . ?
C13 C14 H14 118.5 . . ?
C13 C14 C15 122.9(13) . . ?
C15 C14 H14 118.5 . . ?
C16 C15A H15A 119.3 . . ?
C16 C15A C14A 121.5(13) . . ?
C14A C15A H15A 119.3 . . ?
C8 C9A H9A 121.0 . . ?
C10A C9A C8 118.0(11) . . ?
C10A C9A H9A 121.0 . . ?
C5 C6A H6A 118.6 . . ?
C5 C6A C7A 122.7(13) . . ?
C7A C6A H6A 118.6 . . ?
C23 C28A H28A 120.2 . . ?
C27A C28A C23 119.5(12) . . ?
C27A C28A H28A 120.2 . . ?
C26 C27 H27 120.5 . . ?
C26 C27 C28 119.1(12) . . ?
C28 C27 H27 120.5 . . ?
C26 C25 H25 121.6 . . ?
C24 C25 C26 116.7(13) . . ?
C24 C25 H25 121.6 . . ?
C5 C10 H10 119.1 . . ?
C9 C10 C5 121.8(12) . . ?
C9 C10 H10 119.1 . . ?
C26 C25A H25A 119.1 . . ?
C24A C25A C26 121.7(13) . . ?
C24A C25A H25A 119.1 . . ?
C23 C24 H24 117.1 . . ?
C25 C24 C23 125.8(13) . . ?
C25 C24 H24 117.1 . . ?
C8 C9 H9 120.5 . . ?
C10 C9 C8 119.0(12) . . ?
C10 C9 H9 120.5 . . ?
C23 C24A C25A 121.9(14) . . ?
C23 C24A H24A 119.0 . . ?
C25A C24A H24A 119.0 . . ?
C16 C17 H17 120.4 . . ?
C18 C17 C16 119.2(13) . . ?
C18 C17 H17 120.4 . . ?
C13 C18A H18A 121.1 . . ?
C17A C18A C13 117.7(12) . . ?
C17A C18A H18A 121.1 . . ?
C13 C18 H18 120.7 . . ?
C17 C18 C13 118.7(12) . . ?
C17 C18 H18 120.7 . . ?
C16 C15 C14 120.3(13) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C5 C10A H10A 118.9 . . ?
C9A C10A C5 122.3(12) . . ?
C9A C10A H10A 118.9 . . ?
C8 C7 H7 120.1 . . ?
C8 C7 C6 119.9(12) . . ?
C6 C7 H7 120.1 . . ?
C16 C17A H17A 121.1 . . ?
C18A C17A C16 117.7(13) . . ?
C18A C17A H17A 121.1 . . ?
C13 C14A C15A 123.8(13) . . ?
C13 C14A H14A 118.1 . . ?
C15A C14A H14A 118.1 . . ?
C23 C28 C27 123.1(13) . . ?
C23 C28 H28 118.4 . . ?
C27 C28 H28 118.4 . . ?
C8 C7A C6A 118.9(12) . . ?
C8 C7A H7A 120.6 . . ?
C6A C7A H7A 120.6 . . ?
C5 C6 H6 118.0 . . ?
C7 C6 C5 123.9(13) . . ?
C7 C6 H6 118.0 . . ?
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 O1 1.643(6) . ?
Si1 C5 1.883(7) . ?
Si1 C2 1.840(8) . ?
Si1 C1 1.858(7) . ?
Si2 O1 1.631(6) . ?
Si2 C13 1.873(8) . ?
Si2 C3 1.843(8) . ?
Si2 C4 1.852(8) . ?
Si3 O4 1.641(6) . ?
Si3 C23 1.870(7) . ?
Si3 C22 1.886(8) . ?
Si3 C21 1.839(8) . ?
O5 C29 1.239(9) . ?
O4 H4 0.8400 . ?
N2 H2 0.8800 . ?
N2 C20 1.460(8) . ?
N2 C19 1.324(9) . ?
N3 H3 0.8800 . ?
N3 C29 1.339(9) . ?
N3 C30 1.459(9) . ?
N1 H1 0.8800 . ?
N1 C12 1.455(8) . ?
N1 C11 1.354(9) . ?
O3 C19 1.236(9) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C5 C6A 1.366(17) . ?
C5 C10 1.407(16) . ?
C5 C10A 1.402(16) . ?
C5 C6 1.377(16) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C11 C8 1.489(9) . ?
C11 O2 1.247(8) . ?
C29 C26 1.498(9) . ?
C23 C28A 1.430(16) . ?
C23 C24 1.456(17) . ?
C23 C24A 1.327(18) . ?
C23 C28 1.405(17) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C8 C9A 1.425(15) . ?
C8 C9 1.442(17) . ?
C8 C7 1.364(16) . ?
C8 C7A 1.386(15) . ?
C26 C27A 1.416(14) . ?
C26 C27 1.342(17) . ?
C26 C25 1.388(16) . ?
C26 C25A 1.410(17) . ?
C19 C16 1.503(10) . ?
C13 C14 1.327(15) . ?
C13 C18A 1.518(17) . ?
C13 C18 1.483(17) . ?
C13 C14A 1.300(18) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C16 C15A 1.255(16) . ?
C16 C17 1.467(16) . ?
C16 C15 1.300(17) . ?
C16 C17A 1.482(17) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C27A H27A 0.9500 . ?
C27A C28A 1.381(19) . ?
C14 H14 0.9500 . ?
C14 C15 1.41(2) . ?
C15A H15A 0.9500 . ?
C15A C14A 1.408(19) . ?
C9A H9A 0.9500 . ?
C9A C10A 1.401(18) . ?
C6A H6A 0.9500 . ?
C6A C7A 1.41(2) . ?
C28A H28A 0.9500 . ?
C27 H27 0.9500 . ?
C27 C28 1.41(2) . ?
C25 H25 0.9500 . ?
C25 C24 1.36(2) . ?
C10 H10 0.9500 . ?
C10 C9 1.38(2) . ?
C25A H25A 0.9500 . ?
C25A C24A 1.39(2) . ?
C24 H24 0.9500 . ?
C9 H9 0.9500 . ?
C24A H24A 0.9500 . ?
C17 H17 0.9500 . ?
C17 C18 1.360(19) . ?
C18A H18A 0.9500 . ?
C18A C17A 1.392(19) . ?
C18 H18 0.9500 . ?
C15 H15 0.9500 . ?
C10A H10A 0.9500 . ?
C7 H7 0.9500 . ?
C7 C6 1.37(2) . ?
C17A H17A 0.9500 . ?
C14A H14A 0.9500 . ?
C28 H28 0.9500 . ?
C7A H7A 0.9500 . ?
C6 H6 0.9500 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Si1 C5 C6A C7A -176.8(11) . . . . ?
Si1 C5 C10 C9 -176.6(10) . . . . ?
Si1 C5 C10A C9A 177.1(10) . . . . ?
Si1 C5 C6 C7 179.2(12) . . . . ?
Si2 C13 C14 C15 -176.4(11) . . . . ?
Si2 C13 C18A C17A -174.3(11) . . . . ?
Si2 C13 C18 C17 172.3(11) . . . . ?
Si2 C13 C14A C15A 174.3(10) . . . . ?
Si3 C23 C28A C27A 177.6(10) . . . . ?
Si3 C23 C24 C25 -178.1(14) . . . . ?
Si3 C23 C24A C25A -177.1(13) . . . . ?
Si3 C23 C28 C27 179.5(12) . . . . ?
O1 Si1 C5 C6A 144.1(10) . . . . ?
O1 Si1 C5 C10 59.7(8) . . . . ?
O1 Si1 C5 C10A -41.4(9) . . . . ?
O1 Si1 C5 C6 -121.9(10) . . . . ?
O1 Si2 C13 C14 124.3(10) . . . . ?
O1 Si2 C13 C18A 40.9(9) . . . . ?
O1 Si2 C13 C18 -63.0(8) . . . . ?
O1 Si2 C13 C14A -144.0(11) . . . . ?
O5 C29 C26 C27A 149.8(9) . . . . ?
O5 C29 C26 C27 -149.2(11) . . . . ?
O5 C29 C26 C25 24.1(13) . . . . ?
O5 C29 C26 C25A -25.7(13) . . . . ?
O4 Si3 C23 C28A -103.2(9) . . . . ?
O4 Si3 C23 C24 22.7(11) . . . . ?
O4 Si3 C23 C24A 75.3(11) . . . . ?
O4 Si3 C23 C28 -160.2(10) . . . . ?
N2 C19 C16 C15A -47.5(13) . . . . ?
N2 C19 C16 C17 -125.9(10) . . . . ?
N2 C19 C16 C15 42.0(14) . . . . ?
N2 C19 C16 C17A 132.0(9) . . . . ?
N3 C29 C26 C27A -31.8(12) . . . . ?
N3 C29 C26 C27 29.2(13) . . . . ?
N3 C29 C26 C25 -157.5(10) . . . . ?
N3 C29 C26 C25A 152.7(10) . . . . ?
N1 C11 C8 C9A 43.7(11) . . . . ?
N1 C11 C8 C9 -57.9(11) . . . . ?
N1 C11 C8 C7 127.7(10) . . . . ?
N1 C11 C8 C7A -140.9(9) . . . . ?
O3 C19 C16 C15A 133.5(12) . . . . ?
O3 C19 C16 C17A -47.0(12) . . . . ?
C12 N1 C11 C8 177.6(6) . . . . ?
C12 N1 C11 O2 -1.5(11) . . . . ?
C5 Si1 O1 Si2 -61.4(8) . . . . ?
C5 C6A C7A C8 -2(2) . . . . ?
C5 C10 C9 C8 -2(2) . . . . ?
C2 Si1 O1 Si2 179.5(7) . . . . ?
C2 Si1 C5 C6A -98.7(10) . . . . ?
C2 Si1 C5 C10 176.9(8) . . . . ?
C2 Si1 C5 C10A 75.8(9) . . . . ?
C2 Si1 C5 C6 -4.7(11) . . . . ?
C20 N2 C19 O3 -2.8(13) . . . . ?
C20 N2 C19 C16 178.2(7) . . . . ?
C11 C8 C9A C10A -179.1(10) . . . . ?
C11 C8 C9 C10 -177.2(11) . . . . ?
C11 C8 C7 C6 179.5(12) . . . . ?
C11 C8 C7A C6A 179.4(11) . . . . ?
C29 C26 C27A C28A -179.1(11) . . . . ?
C29 C26 C27 C28 179.4(12) . . . . ?
C29 C26 C25 C24 -178.4(13) . . . . ?
C29 C26 C25A C24A 179.7(13) . . . . ?
C30 N3 C29 O5 -3.1(12) . . . . ?
C30 N3 C29 C26 178.6(6) . . . . ?
C8 C9A C10A C5 1.2(19) . . . . ?
C8 C7 C6 C5 -3(2) . . . . ?
C26 C27A C28A C23 2(2) . . . . ?
C26 C27 C28 C23 -2(2) . . . . ?
C26 C25 C24 C23 -1(3) . . . . ?
C26 C25A C24A C23 -3(3) . . . . ?
C19 C16 C15A C14A -177.3(11) . . . . ?
C19 C16 C17 C18 -176.9(11) . . . . ?
C19 C16 C15 C14 173.8(11) . . . . ?
C19 C16 C17A C18A 177.2(11) . . . . ?
C13 Si2 O1 Si1 62.8(8) . . . . ?
C13 C14 C15 C16 6(2) . . . . ?
C13 C18A C17A C16 -3.2(19) . . . . ?
C22 Si3 C23 C28A 17.8(10) . . . . ?
C22 Si3 C23 C24 143.7(10) . . . . ?
C22 Si3 C23 C24A -163.7(11) . . . . ?
C22 Si3 C23 C28 -39.3(11) . . . . ?
C16 C15A C14A C13 4(2) . . . . ?
C16 C17 C18 C13 2(2) . . . . ?
C3 Si2 O1 Si1 -178.4(7) . . . . ?
C3 Si2 C13 C14 7.6(11) . . . . ?
C3 Si2 C13 C18A -75.8(9) . . . . ?
C3 Si2 C13 C18 -179.6(8) . . . . ?
C3 Si2 C13 C14A 99.4(11) . . . . ?
C21 Si3 C23 C28A 137.7(9) . . . . ?
C21 Si3 C23 C24 -96.4(11) . . . . ?
C21 Si3 C23 C24A -43.8(11) . . . . ?
C21 Si3 C23 C28 80.7(11) . . . . ?
C1 Si1 O1 Si2 58.0(8) . . . . ?
C1 Si1 C5 C6A 24.9(11) . . . . ?
C1 Si1 C5 C10 -59.6(9) . . . . ?
C1 Si1 C5 C10A -160.6(8) . . . . ?
C1 Si1 C5 C6 118.9(11) . . . . ?
C4 Si2 O1 Si1 -58.5(8) . . . . ?
C4 Si2 C13 C14 -114.3(11) . . . . ?
C4 Si2 C13 C18A 162.3(9) . . . . ?
C4 Si2 C13 C18 58.5(9) . . . . ?
C4 Si2 C13 C14A -22.5(12) . . . . ?
C27A C26 C25A C24A 4(2) . . . . ?
C14 C13 C18 C17 -14.3(18) . . . . ?
C15A C16 C17A C18A -3.3(18) . . . . ?
C9A C8 C7A C6A -5.1(18) . . . . ?
C6A C5 C10A C9A -8.0(19) . . . . ?
C28A C23 C24A C25A 1(2) . . . . ?
C27 C26 C25 C24 -5(2) . . . . ?
C25 C26 C27 C28 7(2) . . . . ?
C10 C5 C6 C7 -2(2) . . . . ?
C25A C26 C27A C28A -3.4(18) . . . . ?
C24 C23 C28 C27 -3(2) . . . . ?
C9 C8 C7 C6 5.1(19) . . . . ?
C24A C23 C28A C27A -1(2) . . . . ?
C17 C16 C15 C14 -19(2) . . . . ?
C18A C13 C14A C15A -11(2) . . . . ?
C18 C13 C14 C15 10.8(19) . . . . ?
C15 C16 C17 C18 14.4(19) . . . . ?
C10A C5 C6A C7A 9(2) . . . . ?
C7 C8 C9 C10 -2.6(18) . . . . ?
C17A C16 C15A C14A 3.3(19) . . . . ?
C14A C13 C18A C17A 9.9(19) . . . . ?
C28 C23 C24 C25 5(2) . . . . ?
C7A C8 C9A C10A 5.5(17) . . . . ?
C6 C5 C10 C9 4.8(18) . . . . ?
O2 C11 C8 C9A -137.3(9) . . . . ?
O2 C11 C8 C9 121.2(10) . . . . ?
O2 C11 C8 C7 -53.2(12) . . . . ?
O2 C11 C8 C7A 38.1(12) . . . . ?
