Reactions of a tetrasilabicyclo[1.1.0]but-1(3)-ene with carbon tetrachloride and methanol.
Nukazawa, Takumi; Kosai, Tomoyuki; Honda, Shunya; Ishida, Shintaro; Iwamoto, Takeaki; Dalton transactions (Cambridge, England : 2003) 48 (2019) 10874–10880; doi:10.1039/c9dt01627a

data_7701500
_publ_section_title
;
 Reactions of a tetrasilabicyclo[1.1.0]but-1(3)-ene with carbon
 tetrachloride and methanol.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10874
_journal_page_last               10880
_journal_paper_doi               10.1039/c9dt01627a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C36 H91 Cl2 O Si12'
_chemical_formula_weight         948.06
_chemical_melting_point          436
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2019-05-07 deposited with the CCDC.	2019-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.1569(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4326(8)
_cell_length_b                   12.7398(6)
_cell_length_c                   23.2524(10)
_cell_measurement_reflns_used    9428
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.64
_cell_measurement_theta_min      2.37
_cell_volume                     5452.0(4)
_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  0.0258
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34636
_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         25.997
_diffrn_reflns_theta_min         1.106
_exptl_absorpt_coefficient_mu    0.409
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.6471
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_description       block
_exptl_crystal_F_000             2068
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.521
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         10706
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0514P)^2^+6.5712P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1130
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9306
_reflns_number_total             10706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01627a2.cif
_cod_data_source_block           TK89a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7701500
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.887
_shelx_estimated_absorpt_t_max   0.887
_shelx_res_checksum              70860