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#$Date: 2025-08-20 17:12:52 +0300 (Wed, 20 Aug 2025) $
#$Revision: 301832 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/10/88/4108852.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_4108852
loop_
_publ_author_name
'Katsuhiko Takeuchi'
'Masaaki Ichinohe'
'Akira Sekiguchi'
_publ_section_title
;
 Reactivity of the Disilyne RSi\\tbSiR (R = SiiPr[CH(SiMe3)2]2) toward
 Silylcyanide: Two Pathways To Form the Bis-Adduct [RSiSiR(CNSiMe3)2] with
 Some Silaketenimine Character and a 1,4-Diaza-2,3-disilabenzene Analogue
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16848
_journal_page_last               16849
_journal_paper_doi               10.1021/ja807974a
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C36 H92 N2 Si12'
_chemical_formula_weight         890.20
_chemical_name_systematic
; 
 meso-1,1,4,4-Tetrakis[bis(trimethylsilyl)methyl]-
 3,4-dicyano-1,4-diisopropyltetrasilane 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.456(3)
_cell_angle_beta                 95.914(3)
_cell_angle_gamma                110.091(3)
_cell_formula_units_Z            1
_cell_length_a                   9.6270(5)
_cell_length_b                   10.9580(3)
_cell_length_c                   14.6080(8)
_cell_measurement_reflns_used    13853
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      28.05
_cell_measurement_theta_min      2.09
_cell_volume                     1362.31(12)
_computing_cell_refinement       'HKL scalepack'
_computing_data_collection       'MacScience Xpress'
_computing_data_reduction        Denzo
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device       'MacScience DIP2030 Image plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13853
_diffrn_reflns_theta_full        28.01
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.311
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_description       Plate
_exptl_crystal_F_000             490
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.044(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         6103
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0716P)²+0.7263P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1230
_reflns_number_gt                5339
_reflns_number_total             6103
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja807974a_si_002.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        1362.31(11)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4108852
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Si1 Si 0.44654(6) 0.06329(5) 0.05409(4) 0.02102(13) Uani 1 1 d .
H1 H 0.5375 0.2082 0.0671 0.022(5) Uiso 1 1 calc R
Si2 Si 0.41834(5) 0.05949(5) 0.21597(3) 0.01745(12) Uani 1 1 d .
Si3 Si 0.11428(6) -0.22961(5) 0.14908(4) 0.02311(13) Uani 1 1 d .
Si4 Si 0.14347(6) 0.00383(6) 0.33808(4) 0.02332(13) Uani 1 1 d .
Si5 Si 0.70774(6) 0.34479(5) 0.32549(4) 0.02267(13) Uani 1 1 d .
Si6 Si 0.39951(6) 0.36166(5) 0.24388(4) 0.02423(14) Uani 1 1 d .
N1 N 0.1442(2) 0.0087(2) -0.06456(16) 0.0443(5) Uani 1 1 d .
C1 C 0.2597(2) 0.0277(2) -0.01979(14) 0.0274(4) Uani 1 1 d .
C2 C 0.21288(19) -0.03719(18) 0.21915(12) 0.0195(3) Uani 1 1 d .
H2 H 0.1602 0.0006 0.1803 0.023 Uiso 1 1 calc R
C3 C 0.1521(3) -0.2737(2) 0.02366(15) 0.0343(5) Uani 1 1 d .
H3A H 0.2590 -0.2486 0.0279 0.051 Uiso 1 1 calc R
H3B H 0.1165 -0.2245 -0.0121 0.051 Uiso 1 1 calc R
H3C H 0.1002 -0.3706 -0.0090 0.051 Uiso 1 1 calc R
C4 C -0.0961(2) -0.2826(2) 0.13096(18) 0.0373(5) Uani 1 1 d .
H4A H -0.1232 -0.2628 0.1931 0.056 Uiso 1 1 calc R
H4B H -0.1449 -0.3794 0.0966 0.056 Uiso 1 1 calc R
H4C H -0.1280 -0.2330 0.0939 0.056 Uiso 1 1 calc R
C5 C 0.1606(3) -0.3496(2) 0.20688(17) 0.0344(5) Uani 1 1 d .
H5A H 0.2679 -0.3271 0.2179 0.052 Uiso 1 1 calc R
H5B H 0.1085 -0.4425 0.1644 0.052 Uiso 1 1 calc R
H5C H 0.1292 -0.3403 0.2678 0.052 Uiso 1 1 calc R
C6 C -0.0401(3) 0.0254(3) 0.31182(18) 0.0403(5) Uani 1 1 d .
H6A H -0.0263 0.0953 0.2816 0.060 Uiso 1 1 calc R
H6B H -0.0722 0.0517 0.3715 0.060 Uiso 1 1 calc R
H6C H -0.1157 -0.0598 0.2689 0.060 Uiso 1 1 calc R
C7 C 0.1078(3) -0.1343(2) 0.39629(17) 0.0380(5) Uani 1 1 d .
H7A H 0.1997 -0.1482 0.4108 0.057 Uiso 1 1 calc R
H7B H 0.0312 -0.2181 0.3525 0.057 Uiso 1 1 calc R
H7C H 0.0744 -0.1071 0.4553 0.057 Uiso 1 1 calc R
C8 C 0.2685(3) 0.1632(2) 0.44083(15) 0.0354(5) Uani 1 1 d .
H8A H 0.2932 0.2411 0.4182 0.053 Uiso 1 1 calc R
H8B H 0.3598 0.1535 0.4639 0.053 Uiso 1 1 calc R
H8C H 0.2162 0.1764 0.4928 0.053 Uiso 1 1 calc R
C9 C 0.49345(19) 0.25155(18) 0.28499(13) 0.0197(3) Uani 1 1 d .
H9 H 0.4635 0.2521 0.3472 0.024 Uiso 1 1 calc R
C10 C 0.7841(2) 0.3043(2) 0.43233(16) 0.0345(5) Uani 1 1 d .
H10A H 0.7319 0.3234 0.4835 0.052 Uiso 1 1 calc R
H10B H 0.8903 0.3598 0.4551 0.052 Uiso 1 1 calc R
H10C H 0.7690 0.2090 0.4129 0.052 Uiso 1 1 calc R
C11 C 0.7705(3) 0.5361(2) 0.37343(18) 0.0393(5) Uani 1 1 d .
H11A H 0.7204 0.5602 0.4248 0.059 Uiso 1 1 calc R
H11B H 0.7452 0.5690 0.3220 0.059 Uiso 1 1 calc R
H11C H 0.8781 0.5771 0.3981 0.059 Uiso 1 1 calc R
C12 C 0.8101(2) 0.3076(2) 0.22609(16) 0.0343(5) Uani 1 1 d .
H12A H 0.7813 0.2102 0.1991 0.051 Uiso 1 1 calc R
H12B H 0.9173 0.3509 0.2520 0.051 Uiso 1 1 calc R
H12C H 0.7841 0.3427 0.1761 0.051 Uiso 1 1 calc R
C13 C 0.4022(3) 0.4993(2) 0.35452(18) 0.0397(5) Uani 1 1 d .
H13A H 0.5048 0.5530 0.3898 0.060 Uiso 1 1 calc R
H13B H 0.3441 0.4573 0.3955 0.060 Uiso 1 1 calc R
H13C H 0.3591 0.5576 0.3346 0.060 Uiso 1 1 calc R
C14 C 0.4915(3) 0.4465(3) 0.15732(19) 0.0400(5) Uani 1 1 d .
H14A H 0.5976 0.4974 0.1849 0.060 Uiso 1 1 calc R
H14B H 0.4455 0.5077 0.1460 0.060 Uiso 1 1 calc R
H14C H 0.4783 0.3777 0.0968 0.060 Uiso 1 1 calc R
C15 C 0.1953(3) 0.2668(2) 0.18258(19) 0.0384(5) Uani 1 1 d .
H15A H 0.1416 0.2210 0.2235 0.058 Uiso 1 1 calc R
H15B H 0.1859 0.2002 0.1218 0.058 Uiso 1 1 calc R
H15C H 0.1532 0.3304 0.1709 0.058 Uiso 1 1 calc R
C16 C 0.5490(2) -0.01900(19) 0.26125(14) 0.0231(4) Uani 1 1 d .
H16 H 0.6529 0.0472 0.2717 0.028 Uiso 1 1 calc R
C17 C 0.5387(2) -0.1551(2) 0.18987(16) 0.0299(4) Uani 1 1 d .
H17A H 0.5527 -0.1435 0.1282 0.045 Uiso 1 1 calc R
H17B H 0.4410 -0.2253 0.1817 0.045 Uiso 1 1 calc R
H17C H 0.6160 -0.1814 0.2152 0.045 Uiso 1 1 calc R
C18 C 0.5267(3) -0.0366(2) 0.36018(15) 0.0328(4) Uani 1 1 d .
H18A H 0.5337 0.0487 0.4045 0.049 Uiso 1 1 calc R
H18B H 0.6037 -0.0632 0.3856 0.049 Uiso 1 1 calc R
H18C H 0.4287 -0.1063 0.3523 0.049 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
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
C1 Si1 Si1 104.01(7) . 2_655
C1 Si1 Si2 109.08(6) . .
Si1 Si1 Si2 127.76(4) 2_655 .
C1 Si1 H1 104.6 . .
Si1 Si1 H1 104.6 2_655 .
Si2 Si1 H1 104.6 . .
C16 Si2 C2 111.72(8) . .
C16 Si2 C9 110.08(8) . .
C2 Si2 C9 113.62(8) . .
C16 Si2 Si1 108.44(6) . .
C2 Si2 Si1 111.82(6) . .
C9 Si2 Si1 100.54(6) . .
C4 Si3 C3 105.30(11) . .
C4 Si3 C5 105.81(10) . .
C3 Si3 C5 106.28(11) . .
C4 Si3 C2 109.80(9) . .
C3 Si3 C2 112.15(9) . .
C5 Si3 C2 116.72(9) . .
C7 Si4 C6 107.09(11) . .
C7 Si4 C8 102.96(11) . .
C6 Si4 C8 105.14(12) . .
C7 Si4 C2 113.72(10) . .
C6 Si4 C2 109.00(9) . .
C8 Si4 C2 118.10(9) . .
C12 Si5 C11 106.46(11) . .
C12 Si5 C10 109.27(11) . .
C11 Si5 C10 102.62(11) . .
C12 Si5 C9 113.28(9) . .
C11 Si5 C9 113.07(10) . .
C10 Si5 C9 111.49(9) . .
C15 Si6 C14 105.42(12) . .
C15 Si6 C13 104.82(11) . .
C14 Si6 C13 108.45(12) . .
C15 Si6 C9 114.32(9) . .
C14 Si6 C9 114.54(9) . .
C13 Si6 C9 108.72(9) . .
N1 C1 Si1 178.4(2) . .
Si2 C2 Si3 119.83(9) . .
Si2 C2 Si4 119.93(9) . .
Si3 C2 Si4 109.53(8) . .
Si2 C2 H2 101.0 . .
Si3 C2 H2 101.0 . .
Si4 C2 H2 101.0 . .
Si3 C3 H3A 109.5 . .
Si3 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
Si3 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
Si3 C4 H4A 109.5 . .
Si3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
Si3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
Si3 C5 H5A 109.5 . .
Si3 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
Si3 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
Si4 C6 H6A 109.5 . .
Si4 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
Si4 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
Si4 C7 H7A 109.5 . .
Si4 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
Si4 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
Si4 C8 H8A 109.5 . .
Si4 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
Si4 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
Si5 C9 Si2 116.62(9) . .
Si5 C9 Si6 112.08(9) . .
Si2 C9 Si6 119.28(9) . .
Si5 C9 H9 101.7 . .
Si2 C9 H9 101.7 . .
Si6 C9 H9 101.7 . .
Si5 C10 H10A 109.5 . .
Si5 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
Si5 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
Si5 C11 H11A 109.5 . .
Si5 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
Si5 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
Si5 C12 H12A 109.5 . .
Si5 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
Si5 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
Si6 C13 H13A 109.5 . .
Si6 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
Si6 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
Si6 C14 H14A 109.5 . .
Si6 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
Si6 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
Si6 C15 H15A 109.5 . .
Si6 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
Si6 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C18 C16 C17 109.84(16) . .
C18 C16 Si2 111.32(13) . .
C17 C16 Si2 115.19(13) . .
C18 C16 H16 106.7 . .
C17 C16 H16 106.7 . .
Si2 C16 H16 106.7 . .
C16 C17 H17A 109.5 . .
C16 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C16 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C16 C18 H18A 109.5 . .
C16 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C16 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 C1 1.857(2) .
Si1 Si1 2.3723(10) 2_655
Si1 Si2 2.4176(7) .
Si1 H1 1.4750 .
Si2 C16 1.9066(18) .
Si2 C2 1.9085(18) .
Si2 C9 1.9083(18) .
Si3 C4 1.873(2) .
Si3 C3 1.873(2) .
Si3 C5 1.887(2) .
Si3 C2 1.9155(18) .
Si4 C7 1.876(2) .
Si4 C6 1.876(2) .
Si4 C8 1.881(2) .
Si4 C2 1.9225(18) .
Si5 C12 1.871(2) .
Si5 C11 1.874(2) .
Si5 C10 1.879(2) .
Si5 C9 1.9047(18) .
Si6 C15 1.867(2) .
Si6 C14 1.881(2) .
Si6 C13 1.885(2) .
Si6 C9 1.9127(19) .
N1 C1 1.151(3) .
C2 H2 0.9800 .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
C5 H5A 0.9600 .
C5 H5B 0.9600 .
C5 H5C 0.9600 .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 H9 0.9800 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
C16 C18 1.535(3) .
C16 C17 1.539(3) .
C16 H16 0.9800 .
C17 H17A 0.9600 .
C17 H17B 0.9600 .
C17 H17C 0.9600 .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 101567334
