Dearomative cycloadditions of a silylene with pyrazine and quinoxaline.
Ishida, Shintaro; Tamura, Tomofumi; Iwamoto, Takeaki; Dalton transactions (Cambridge, England : 2003) 47 (2018) 11317–11321; doi:10.1039/c8dt02802h

data_7047197
_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_formula_sum            'C47 H94 N2 Si10'
_chemical_formula_weight         968.14
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_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                77.1630(10)
_cell_angle_beta                 84.5050(10)
_cell_angle_gamma                72.1030(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4668(3)
_cell_length_b                   13.4537(4)
_cell_length_c                   20.1191(6)
_cell_measurement_reflns_used    9583
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.87
_cell_measurement_theta_min      2.16
_cell_volume                     2878.51(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0214
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36402
_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         25.500
_diffrn_reflns_theta_min         1.038
_exptl_absorpt_coefficient_mu    0.260
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_correction_T_min  0.6978
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.117
_exptl_crystal_description       block
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     557
_refine_ls_number_reflns         10714
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0301
_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/[\s^2^(Fo^2^)+(0.0336P)^2^+1.8231P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0765
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9596
_reflns_number_total             10714
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02802h2.cif
_cod_data_source_block           yy22a_a
_cod_depositor_comments
'Adding full bibliography for 7047196--7047197.cif.'
_cod_original_cell_volume        2878.52(14)
_cod_database_code               7047197
_shelx_estimated_absorpt_t_min   0.950
_shelx_estimated_absorpt_t_max   0.974
_shelxl_version_number           2014-3
_shelx_res_checksum              97977