#------------------------------------------------------------------------------
#$Date: 2019-11-17 10:48:47 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229428 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/71/7047196.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_7047196
loop_
_publ_author_name
'Ishida, Shintaro'
'Tamura, Tomofumi'
'Iwamoto, Takeaki'
_publ_section_title
;
 Dearomative cycloadditions of a silylene with pyrazine and quinoxaline.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11317
_journal_page_last               11321
_journal_paper_doi               10.1039/c8dt02802h
_journal_volume                  47
_journal_year                    2018
_chemical_absolute_configuration unk
_chemical_formula_sum            'C36 H84 N2 Si10'
_chemical_formula_weight         825.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2018-04-16 deposited with the CCDC.
2018-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 129.5940(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.0673(7)
_cell_length_b                   9.5867(3)
_cell_length_c                   16.1406(5)
_cell_measurement_reflns_used    4117
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.97
_cell_measurement_theta_min      2.47
_cell_volume                     2511.98(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7978
_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         25.499
_diffrn_reflns_theta_min         1.934
_exptl_absorpt_coefficient_mu    0.287
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.6977
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_description       block
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.36(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         4641
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0346
_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)+(0.0500P)²+0.9851P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0851
_reflns_Friedel_coverage         0.881
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4466
_reflns_number_total             4641
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt02802h2.cif
_cod_data_source_block           TK23a_a
_cod_depositor_comments
'Adding full bibliography for 7047196--7047197.cif.'
_cod_original_cell_volume        2511.97(14)
_cod_database_code               7047196
_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.
;
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Si1 Si 0.42976(5) 0.51959(8) 0.32908(7) 0.01036(19) Uani 1 1 d . .
Si2 Si 0.49875(6) 0.71320(11) 0.24109(7) 0.0208(2) Uani 1 1 d . .
Si3 Si 0.53344(6) 0.39465(11) 0.26443(8) 0.0213(2) Uani 1 1 d . .
Si4 Si 0.23875(6) 0.57300(9) 0.19046(7) 0.0147(2) Uani 1 1 d . .
Si5 Si 0.29867(6) 0.27060(9) 0.26927(7) 0.0158(2) Uani 1 1 d . .
N1 N 0.41805(17) 0.6876(3) 0.3619(2) 0.0140(6) Uani 1 1 d . .
C1 C 0.4574(2) 0.7643(3) 0.4438(3) 0.0179(7) Uani 1 1 d . .
H1 H 0.435(3) 0.856(5) 0.436(3) 0.036(12) Uiso 1 1 d . .
C2 C 0.5078(2) 0.4455(3) 0.4660(2) 0.0120(6) Uani 1 1 d . .
H2 H 0.565(3) 0.449(4) 0.499(3) 0.021(10) Uiso 1 1 d . .
C3 C 0.4582(2) 0.5347(4) 0.2393(2) 0.0149(7) Uani 1 1 d . .
C4 C 0.3708(2) 0.5114(4) 0.1262(2) 0.0164(7) Uani 1 1 d . .
H3 H 0.3410 0.6015 0.0988 0.020 Uiso 1 1 calc R U
H4 H 0.3776 0.4766 0.0746 0.020 Uiso 1 1 calc R U
C5 C 0.3201(2) 0.4066(4) 0.1342(2) 0.0162(7) Uani 1 1 d . .
H5 H 0.3419 0.3115 0.1429 0.019 Uiso 1 1 calc R U
H6 H 0.2622 0.4086 0.0668 0.019 Uiso 1 1 calc R U
C6 C 0.3230(2) 0.4409(3) 0.2322(2) 0.0124(6) Uani 1 1 d . .
C7 C 0.4205(3) 0.8558(4) 0.1848(3) 0.0266(8) Uani 1 1 d . .
H7 H 0.4441 0.9432 0.1838 0.040 Uiso 1 1 calc R U
H8 H 0.4046 0.8672 0.2297 0.040 Uiso 1 1 calc R U
H9 H 0.3718 0.8316 0.1114 0.040 Uiso 1 1 calc R U
C8 C 0.5263(3) 0.7141(5) 0.1512(3) 0.0352(10) Uani 1 1 d . .
H10 H 0.4795 0.6797 0.0798 0.053 Uiso 1 1 calc R U
H11 H 0.5741 0.6537 0.1818 0.053 Uiso 1 1 calc R U
H12 H 0.5396 0.8095 0.1450 0.053 Uiso 1 1 calc R U
C9 C 0.5898(2) 0.7703(4) 0.3804(3) 0.0294(9) Uani 1 1 d . .
H13 H 0.5832 0.8685 0.3905 0.044 Uiso 1 1 calc R U
H14 H 0.6403 0.7593 0.3899 0.044 Uiso 1 1 calc R U
H15 H 0.5933 0.7130 0.4335 0.044 Uiso 1 1 calc R U
C10 C 0.5137(3) 0.3496(6) 0.1366(3) 0.0419(12) Uani 1 1 d . .
H16 H 0.5095 0.4356 0.1005 0.063 Uiso 1 1 calc R U
H17 H 0.4621 0.2971 0.0893 0.063 Uiso 1 1 calc R U
H18 H 0.5593 0.2927 0.1533 0.063 Uiso 1 1 calc R U
C11 C 0.6434(2) 0.4512(5) 0.3658(3) 0.0284(9) Uani 1 1 d . .
H19 H 0.6798 0.3737 0.3808 0.043 Uiso 1 1 calc R U
H20 H 0.6544 0.4791 0.4323 0.043 Uiso 1 1 calc R U
H21 H 0.6536 0.5304 0.3373 0.043 Uiso 1 1 calc R U
C12 C 0.5273(3) 0.2232(4) 0.3152(4) 0.0340(9) Uani 1 1 d . .
H22 H 0.5696 0.1599 0.3289 0.051 Uiso 1 1 calc R U
H23 H 0.4727 0.1819 0.2612 0.051 Uiso 1 1 calc R U
H24 H 0.5364 0.2382 0.3821 0.051 Uiso 1 1 calc R U
C13 C 0.2305(2) 0.7277(4) 0.1138(3) 0.0256(8) Uani 1 1 d . .
H25 H 0.1853 0.7876 0.0950 0.038 Uiso 1 1 calc R U
H26 H 0.2195 0.6963 0.0480 0.038 Uiso 1 1 calc R U
H27 H 0.2822 0.7802 0.1582 0.038 Uiso 1 1 calc R U
C14 C 0.1334(2) 0.4939(4) 0.0930(3) 0.0219(8) Uani 1 1 d . .
H28 H 0.0916 0.5644 0.0716 0.033 Uiso 1 1 calc R U
H29 H 0.1283 0.4153 0.1273 0.033 Uiso 1 1 calc R U
H30 H 0.1251 0.4609 0.0293 0.033 Uiso 1 1 calc R U
C15 C 0.2498(2) 0.6405(4) 0.3088(3) 0.0248(8) Uani 1 1 d . .
H31 H 0.2613 0.7409 0.3169 0.037 Uiso 1 1 calc R U
H32 H 0.2953 0.5920 0.3742 0.037 Uiso 1 1 calc R U
H33 H 0.1986 0.6238 0.2968 0.037 Uiso 1 1 calc R U
C16 C 0.2193(3) 0.1690(4) 0.1434(3) 0.0281(9) Uani 1 1 d . .
H34 H 0.2430 0.1376 0.1106 0.042 Uiso 1 1 calc R U
H35 H 0.1715 0.2286 0.0927 0.042 Uiso 1 1 calc R U
H36 H 0.2020 0.0877 0.1615 0.042 Uiso 1 1 calc R U
C17 C 0.2603(2) 0.2959(4) 0.3458(3) 0.0230(8) Uani 1 1 d . .
H37 H 0.2473 0.2050 0.3595 0.035 Uiso 1 1 calc R U
H38 H 0.2106 0.3539 0.3036 0.035 Uiso 1 1 calc R U
H39 H 0.3029 0.3420 0.4144 0.035 Uiso 1 1 calc R U
C18 C 0.3852(2) 0.1434(4) 0.3528(3) 0.0255(8) Uani 1 1 d . .
H40 H 0.4315 0.1887 0.4194 0.038 Uiso 1 1 calc R U
H41 H 0.4028 0.1113 0.3126 0.038 Uiso 1 1 calc R U
H42 H 0.3665 0.0634 0.3701 0.038 Uiso 1 1 calc R U
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
N1 Si1 C2 100.34(13) . .
N1 Si1 C3 109.48(14) . .
C2 Si1 C3 117.84(15) . .
N1 Si1 C6 107.00(14) . .
C2 Si1 C6 120.91(14) . .
C3 Si1 C6 100.78(14) . .
C7 Si2 C8 103.41(19) . .
C7 Si2 C9 106.21(19) . .
C8 Si2 C9 109.95(18) . .
C7 Si2 C3 113.64(17) . .
C8 Si2 C3 110.49(19) . .
C9 Si2 C3 112.66(16) . .
C11 Si3 C10 108.10(19) . .
C11 Si3 C12 105.3(2) . .
C10 Si3 C12 104.5(2) . .
C11 Si3 C3 112.25(18) . .
C10 Si3 C3 110.83(18) . .
C12 Si3 C3 115.35(16) . .
C13 Si4 C14 101.79(17) . .
C13 Si4 C15 107.33(18) . .
C14 Si4 C15 107.69(17) . .
C13 Si4 C6 115.59(16) . .
C14 Si4 C6 111.29(15) . .
C15 Si4 C6 112.40(16) . .
C18 Si5 C17 103.93(18) . .
C18 Si5 C16 103.17(18) . .
C17 Si5 C16 108.56(18) . .
C18 Si5 C6 116.67(16) . .
C17 Si5 C6 114.14(15) . .
C16 Si5 C6 109.56(16) . .
C1 N1 Si1 136.6(3) . .
N1 C1 C1 137.1(3) . 2_656
N1 C1 H1 117(3) . .
C1 C1 H1 105(3) 2_656 .
C2 C2 Si1 118.9(3) 2_656 .
C2 C2 H2 115(2) 2_656 .
Si1 C2 H2 119(2) . .
C4 C3 Si1 99.8(2) . .
C4 C3 Si2 109.0(2) . .
Si1 C3 Si2 114.53(17) . .
C4 C3 Si3 110.1(2) . .
Si1 C3 Si3 114.07(17) . .
Si2 C3 Si3 108.88(17) . .
C5 C4 C3 110.9(3) . .
C5 C4 H3 109.5 . .
C3 C4 H3 109.5 . .
C5 C4 H4 109.5 . .
C3 C4 H4 109.5 . .
H3 C4 H4 108.0 . .
C4 C5 C6 111.4(3) . .
C4 C5 H5 109.4 . .
C6 C5 H5 109.4 . .
C4 C5 H6 109.4 . .
C6 C5 H6 109.4 . .
H5 C5 H6 108.0 . .
C5 C6 Si1 100.2(2) . .
C5 C6 Si5 106.8(2) . .
Si1 C6 Si5 119.66(17) . .
C5 C6 Si4 110.4(2) . .
Si1 C6 Si4 111.88(16) . .
Si5 C6 Si4 107.45(16) . .
Si2 C7 H7 109.5 . .
Si2 C7 H8 109.5 . .
H7 C7 H8 109.5 . .
Si2 C7 H9 109.5 . .
H7 C7 H9 109.5 . .
H8 C7 H9 109.5 . .
Si2 C8 H10 109.5 . .
Si2 C8 H11 109.5 . .
H10 C8 H11 109.5 . .
Si2 C8 H12 109.5 . .
H10 C8 H12 109.5 . .
H11 C8 H12 109.5 . .
Si2 C9 H13 109.5 . .
Si2 C9 H14 109.5 . .
H13 C9 H14 109.5 . .
Si2 C9 H15 109.5 . .
H13 C9 H15 109.5 . .
H14 C9 H15 109.5 . .
Si3 C10 H16 109.5 . .
Si3 C10 H17 109.5 . .
H16 C10 H17 109.5 . .
Si3 C10 H18 109.5 . .
H16 C10 H18 109.5 . .
H17 C10 H18 109.5 . .
Si3 C11 H19 109.5 . .
Si3 C11 H20 109.5 . .
H19 C11 H20 109.5 . .
Si3 C11 H21 109.5 . .
H19 C11 H21 109.5 . .
H20 C11 H21 109.5 . .
Si3 C12 H22 109.5 . .
Si3 C12 H23 109.5 . .
H22 C12 H23 109.5 . .
Si3 C12 H24 109.5 . .
H22 C12 H24 109.5 . .
H23 C12 H24 109.5 . .
Si4 C13 H25 109.5 . .
Si4 C13 H26 109.5 . .
H25 C13 H26 109.5 . .
Si4 C13 H27 109.5 . .
H25 C13 H27 109.5 . .
H26 C13 H27 109.5 . .
Si4 C14 H28 109.5 . .
Si4 C14 H29 109.5 . .
H28 C14 H29 109.5 . .
Si4 C14 H30 109.5 . .
H28 C14 H30 109.5 . .
H29 C14 H30 109.5 . .
Si4 C15 H31 109.5 . .
Si4 C15 H32 109.5 . .
H31 C15 H32 109.5 . .
Si4 C15 H33 109.5 . .
H31 C15 H33 109.5 . .
H32 C15 H33 109.5 . .
Si5 C16 H34 109.5 . .
Si5 C16 H35 109.5 . .
H34 C16 H35 109.5 . .
Si5 C16 H36 109.5 . .
H34 C16 H36 109.5 . .
H35 C16 H36 109.5 . .
Si5 C17 H37 109.5 . .
Si5 C17 H38 109.5 . .
H37 C17 H38 109.5 . .
Si5 C17 H39 109.5 . .
H37 C17 H39 109.5 . .
H38 C17 H39 109.5 . .
Si5 C18 H40 109.5 . .
Si5 C18 H41 109.5 . .
H40 C18 H41 109.5 . .
Si5 C18 H42 109.5 . .
H40 C18 H42 109.5 . .
H41 C18 H42 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 N1 1.761(3) .
Si1 C2 1.860(3) .
Si1 C3 1.893(3) .
Si1 C6 1.894(3) .
Si2 C7 1.871(4) .
Si2 C8 1.875(4) .
Si2 C9 1.881(4) .
Si2 C3 1.905(3) .
Si3 C11 1.872(4) .
Si3 C10 1.877(4) .
Si3 C12 1.878(4) .
Si3 C3 1.914(4) .
Si4 C13 1.867(4) .
Si4 C14 1.878(4) .
Si4 C15 1.885(4) .
Si4 C6 1.920(3) .
Si5 C18 1.869(4) .
Si5 C17 1.874(4) .
Si5 C16 1.882(4) .
Si5 C6 1.917(3) .
N1 C1 1.257(4) .
C1 C1 1.537(7) 2_656
C1 H1 0.97(5) .
C2 C2 1.332(6) 2_656
C2 H2 0.96(4) .
C3 C4 1.578(4) .
C4 C5 1.530(5) .
C4 H3 0.9900 .
C4 H4 0.9900 .
C5 C6 1.579(4) .
C5 H5 0.9900 .
C5 H6 0.9900 .
C7 H7 0.9800 .
C7 H8 0.9800 .
C7 H9 0.9800 .
C8 H10 0.9800 .
C8 H11 0.9800 .
C8 H12 0.9800 .
C9 H13 0.9800 .
C9 H14 0.9800 .
C9 H15 0.9800 .
C10 H16 0.9800 .
C10 H17 0.9800 .
C10 H18 0.9800 .
C11 H19 0.9800 .
C11 H20 0.9800 .
C11 H21 0.9800 .
C12 H22 0.9800 .
C12 H23 0.9800 .
C12 H24 0.9800 .
C13 H25 0.9800 .
C13 H26 0.9800 .
C13 H27 0.9800 .
C14 H28 0.9800 .
C14 H29 0.9800 .
C14 H30 0.9800 .
C15 H31 0.9800 .
C15 H32 0.9800 .
C15 H33 0.9800 .
C16 H34 0.9800 .
C16 H35 0.9800 .
C16 H36 0.9800 .
C17 H37 0.9800 .
C17 H38 0.9800 .
C17 H39 0.9800 .
C18 H40 0.9800 .
C18 H41 0.9800 .
C18 H42 0.9800 .
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_4
C2 Si1 N1 C1 16.6(4) .
C3 Si1 N1 C1 -108.0(4) .
C6 Si1 N1 C1 143.6(4) .
Si1 N1 C1 C1 10.4(8) 2_656
N1 Si1 C2 C2 55.3(2) 2_656
C3 Si1 C2 C2 173.96(18) 2_656
C6 Si1 C2 C2 -61.8(2) 2_656
N1 Si1 C3 C4 -98.5(2) .
C2 Si1 C3 C4 147.8(2) .
C6 Si1 C3 C4 14.1(2) .
N1 Si1 C3 Si2 17.8(2) .
C2 Si1 C3 Si2 -95.9(2) .
C6 Si1 C3 Si2 130.29(18) .
N1 Si1 C3 Si3 144.17(16) .
C2 Si1 C3 Si3 30.5(2) .
C6 Si1 C3 Si3 -103.31(18) .
Si1 C3 C4 C5 -35.1(3) .
Si2 C3 C4 C5 -155.4(2) .
Si3 C3 C4 C5 85.2(3) .
C3 C4 C5 C6 47.2(4) .
C4 C5 C6 Si1 -31.5(3) .
C4 C5 C6 Si5 -156.9(2) .
C4 C5 C6 Si4 86.6(3) .
N1 Si1 C6 C5 123.3(2) .
C2 Si1 C6 C5 -123.0(2) .
C3 Si1 C6 C5 8.9(2) .
N1 Si1 C6 Si5 -120.64(18) .
C2 Si1 C6 Si5 -7.0(3) .
C3 Si1 C6 Si5 124.96(19) .
N1 Si1 C6 Si4 6.27(19) .
C2 Si1 C6 Si4 119.95(17) .
C3 Si1 C6 Si4 -108.13(17) .
