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#$Date: 2016-03-22 12:19:30 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178945 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/74/4117495.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_4117495
loop_
_publ_author_name
'Katsuhiko Takeuchi'
'Masaaki Ichinohe'
'Akira Sekiguchi'
_publ_section_title
;
 A New Disilene with π-Accepting Groups from the Reaction of Disilyne
 RSi\\tbSiR (R = SiiPr[CH(SiMe3)2]) with Isocyanides
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2954
_journal_page_last               2957
_journal_paper_doi               10.1021/ja212065a
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C36 H90 N2 Si12'
_chemical_formula_weight         888.18
_chemical_name_systematic
; 
 E-1,1,4,4-Tetrakis[bis(trimethylsilyl)methyl]-2,3-dicyano- 
 1,4-diisopropyl-2-tetrasilene 
;
_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                106.505(2)
_cell_angle_beta                 95.721(2)
_cell_angle_gamma                109.8770(10)
_cell_formula_units_Z            1
_cell_length_a                   9.5952(11)
_cell_length_b                   10.9258(13)
_cell_length_c                   14.635(3)
_cell_measurement_reflns_used    2524
_cell_measurement_temperature    120.0(1)
_cell_measurement_theta_max      24.55
_cell_measurement_theta_min      2.31
_cell_volume                     1350.2(4)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120.0(1)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_sigmaI/netI    0.1098
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15269
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.313
_exptl_absorpt_correction_T_max  0.9900
_exptl_absorpt_correction_T_min  0.9694
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
SADABS Sheldrick 1996 
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_description       Plate
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.0050(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         6014
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0982
_refine_ls_R_factor_gt           0.0562
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0577P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1417
_reflns_number_gt                3796
_reflns_number_total             6014
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja212065a_si_002.cif
_cod_data_source_block           cndisilene_0ma
_cod_original_cell_volume        1350.3(3)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4117495
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 0.56621(13) 0.96425(16) 0.44834(8) 0.0432(4) Uani 1 1 d .
Si2 Si 0.58518(10) 0.94935(9) 0.28364(7) 0.0159(2) Uani 1 1 d .
Si3 Si 0.29461(11) 0.66191(10) 0.17527(7) 0.0205(2) Uani 1 1 d .
Si4 Si 0.60341(11) 0.64803(10) 0.25938(8) 0.0254(3) Uani 1 1 d .
Si5 Si 0.85840(11) 1.00008(10) 0.16059(7) 0.0196(2) Uani 1 1 d .
Si6 Si 0.89257(11) 1.23809(10) 0.35152(7) 0.0209(2) Uani 1 1 d .
N1 N 0.8494(4) 0.9785(3) 0.5630(2) 0.0348(8) Uani 1 1 d .
C1 C 0.7430(4) 0.9746(3) 0.5208(2) 0.0208(8) Uani 1 1 d .
C2 C 0.5096(4) 0.7570(3) 0.2162(2) 0.0181(7) Uani 1 1 d .
H2 H 0.5403 0.7534 0.1524 0.022 Uiso 1 1 calc R
C3 C 0.1930(4) 0.7024(4) 0.2753(3) 0.0310(9) Uani 1 1 d .
H3A H 0.2334 0.6831 0.3314 0.046 Uiso 1 1 calc R
H3B H 0.0843 0.6450 0.2519 0.046 Uiso 1 1 calc R
H3C H 0.2081 0.8003 0.2949 0.046 Uiso 1 1 calc R
C4 C 0.2194(4) 0.6987(4) 0.0676(3) 0.0285(9) Uani 1 1 d .
H4A H 0.2730 0.6769 0.0155 0.043 Uiso 1 1 calc R
H4B H 0.2351 0.7968 0.0868 0.043 Uiso 1 1 calc R
H4C H 0.1106 0.6417 0.0439 0.043 Uiso 1 1 calc R
C5 C 0.2312(4) 0.4691(4) 0.1287(3) 0.0341(10) Uani 1 1 d .
H5A H 0.2814 0.4418 0.0759 0.051 Uiso 1 1 calc R
H5B H 0.1209 0.4268 0.1040 0.051 Uiso 1 1 calc R
H5C H 0.2581 0.4378 0.1819 0.051 Uiso 1 1 calc R
C6 C 0.5140(5) 0.5790(5) 0.3524(3) 0.0518(13) Uani 1 1 d .
H6A H 0.4044 0.5286 0.3266 0.078 Uiso 1 1 calc R
H6B H 0.5323 0.6561 0.4125 0.078 Uiso 1 1 calc R
H6C H 0.5586 0.5162 0.3667 0.078 Uiso 1 1 calc R
C7 C 0.5939(5) 0.5005(4) 0.1511(3) 0.0428(11) Uani 1 1 d .
H7A H 0.4877 0.4451 0.1171 0.064 Uiso 1 1 calc R
H7B H 0.6378 0.4423 0.1733 0.064 Uiso 1 1 calc R
H7C H 0.6511 0.5372 0.1065 0.064 Uiso 1 1 calc R
C8 C 0.8102(4) 0.7414(4) 0.3151(3) 0.0293(9) Uani 1 1 d .
H8A H 0.8626 0.7791 0.2690 0.044 Uiso 1 1 calc R
H8B H 0.8514 0.6770 0.3302 0.044 Uiso 1 1 calc R
H8C H 0.8253 0.8171 0.3752 0.044 Uiso 1 1 calc R
C9 C 0.7911(3) 1.0443(3) 0.2799(2) 0.0152(7) Uani 1 1 d .
H9 H 0.8446 1.0051 0.3189 0.018 Uiso 1 1 calc R
C10 C 0.7329(4) 0.8375(4) 0.0587(3) 0.0292(9) Uani 1 1 d .
H10A H 0.7097 0.7588 0.0823 0.044 Uiso 1 1 calc R
H10B H 0.7852 0.8224 0.0048 0.044 Uiso 1 1 calc R
H10C H 0.6384 0.8461 0.0357 0.044 Uiso 1 1 calc R
C11 C 1.0434(4) 0.9796(4) 0.1865(3) 0.0322(9) Uani 1 1 d .
H11A H 1.0301 0.9085 0.2171 0.048 Uiso 1 1 calc R
H11B H 1.1205 1.0678 0.2308 0.048 Uiso 1 1 calc R
H11C H 1.0760 0.9518 0.1253 0.048 Uiso 1 1 calc R
C12 C 0.8904(4) 1.1363(4) 0.1032(3) 0.0319(9) Uani 1 1 d .
H12A H 0.7955 1.1493 0.0888 0.048 Uiso 1 1 calc R
H12B H 0.9242 1.1079 0.0425 0.048 Uiso 1 1 calc R
H12C H 0.9684 1.2234 0.1481 0.048 Uiso 1 1 calc R
C13 C 1.1030(4) 1.2905(4) 0.3656(3) 0.0326(9) Uani 1 1 d .
H13A H 1.1274 1.2694 0.3009 0.049 Uiso 1 1 calc R
H13B H 1.1376 1.2395 0.4018 0.049 Uiso 1 1 calc R
H13C H 1.1539 1.3901 0.4014 0.049 Uiso 1 1 calc R
C14 C 0.8432(4) 1.3587(4) 0.2967(3) 0.0285(9) Uani 1 1 d .
H14A H 0.8570 1.3380 0.2294 0.043 Uiso 1 1 calc R
H14B H 0.9096 1.4546 0.3352 0.043 Uiso 1 1 calc R
H14C H 0.7371 1.3461 0.2971 0.043 Uiso 1 1 calc R
C15 C 0.8619(5) 1.2830(4) 0.4787(3) 0.0325(9) Uani 1 1 d .
H15A H 0.8868 1.2226 0.5101 0.049 Uiso 1 1 calc R
H15B H 0.7555 1.2703 0.4771 0.049 Uiso 1 1 calc R
H15C H 0.9275 1.3796 0.5158 0.049 Uiso 1 1 calc R
C16 C 0.4548(4) 1.0291(3) 0.2408(2) 0.0195(8) Uani 1 1 d .
H16 H 0.3486 0.9613 0.2298 0.023 Uiso 1 1 calc R
C17 C 0.4763(4) 1.0457(4) 0.1418(3) 0.0269(9) Uani 1 1 d .
H17A H 0.4681 0.9574 0.0956 0.040 Uiso 1 1 calc R
H17B H 0.5767 1.1166 0.1500 0.040 Uiso 1 1 calc R
H17C H 0.3978 1.0735 0.1167 0.040 Uiso 1 1 calc R
C18 C 0.4649(4) 1.1656(4) 0.3128(3) 0.0262(8) Uani 1 1 d .
H18A H 0.4502 1.1543 0.3756 0.039 Uiso 1 1 calc R
H18B H 0.3860 1.1927 0.2871 0.039 Uiso 1 1 calc R
H18C H 0.5651 1.2376 0.3218 0.039 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 107.96(13) . 2_676
C1 Si1 Si2 111.93(12) . .
Si1 Si1 Si2 136.48(9) 2_676 .
C2 Si2 C16 110.95(15) . .
C2 Si2 C9 113.61(14) . .
C16 Si2 C9 112.09(15) . .
C2 Si2 Si1 103.27(11) . .
C16 Si2 Si1 106.51(11) . .
C9 Si2 Si1 109.79(11) . .
C3 Si3 C4 110.07(18) . .
C3 Si3 C5 105.89(18) . .
C4 Si3 C5 102.84(17) . .
C3 Si3 C2 112.97(16) . .
C4 Si3 C2 110.99(16) . .
C5 Si3 C2 113.50(16) . .
C8 Si4 C6 106.16(18) . .
C8 Si4 C7 103.95(18) . .
C6 Si4 C7 109.8(2) . .
C8 Si4 C2 114.37(15) . .
C6 Si4 C2 112.84(18) . .
C7 Si4 C2 109.32(17) . .
C12 Si5 C10 103.51(18) . .
C12 Si5 C11 107.63(18) . .
C10 Si5 C11 105.12(18) . .
C12 Si5 C9 113.17(16) . .
C10 Si5 C9 117.93(15) . .
C11 Si5 C9 108.77(15) . .
C15 Si6 C13 105.07(18) . .
C15 Si6 C14 106.82(17) . .
C13 Si6 C14 105.69(17) . .
C15 Si6 C9 111.97(16) . .
C13 Si6 C9 109.97(16) . .
C14 Si6 C9 116.53(15) . .
N1 C1 Si1 178.6(4) . .
Si2 C2 Si3 117.22(17) . .
Si2 C2 Si4 118.98(17) . .
Si3 C2 Si4 111.66(16) . .
Si2 C2 H2 101.8 . .
Si3 C2 H2 101.8 . .
Si4 C2 H2 101.8 . .
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 . .
Si2 C9 Si5 119.92(17) . .
Si2 C9 Si6 119.87(16) . .
Si5 C9 Si6 109.68(16) . .
Si2 C9 H9 100.9 . .
Si5 C9 H9 100.9 . .
Si6 C9 H9 100.9 . .
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 109.8(3) . .
C18 C16 Si2 115.9(2) . .
C17 C16 Si2 111.0(2) . .
C18 C16 H16 106.5 . .
C17 C16 H16 106.5 . .
Si2 C16 H16 106.5 . .
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 1.860(4) .
Si1 Si1 2.213(2) 2_676
Si1 Si2 2.3989(15) .
Si2 C2 1.887(3) .
Si2 C16 1.900(3) .
Si2 C9 1.909(3) .
Si3 C3 1.870(4) .
Si3 C4 1.870(4) .
Si3 C5 1.871(4) .
Si3 C2 1.906(3) .
Si4 C8 1.863(4) .
Si4 C6 1.881(4) .
Si4 C7 1.881(4) .
Si4 C2 1.916(3) .
Si5 C12 1.862(4) .
Si5 C10 1.874(4) .
Si5 C11 1.878(4) .
Si5 C9 1.913(3) .
Si6 C15 1.865(4) .
Si6 C13 1.873(4) .
Si6 C14 1.885(4) .
Si6 C9 1.914(3) .
N1 C1 1.120(4) .
C2 H2 1.0000 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 H9 1.0000 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 C18 1.527(5) .
C16 C17 1.536(5) .
C16 H16 1.0000 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
