Interconversion between a planar 1,3-dichlorobicyclo[1.1.0]tetrasilane and a (chloro)(chlorosilyl)cyclotrisilene.
Nukazawa, Takumi; Iwamoto, Takeaki; Dalton transactions (Cambridge, England : 2003) 49 (2020) 16728–16735; doi:10.1039/d0dt03408h

data_7705858
_publ_section_title
;
 Interconversion between a planar 1,3-dichlorobicyclo[1.1.0]tetrasilane
 and a (chloro)(chlorosilyl)cyclotrisilene.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16728
_journal_page_last               16735
_journal_paper_doi               10.1039/d0dt03408h
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C39 H90 Cl2 N2 Si12, 2(C6 H6)'
_chemical_formula_sum            'C51 H102 Cl2 N2 Si12'
_chemical_formula_weight         1151.32
_chemical_melting_point          353
_chemical_name_systematic        (chloro)(chlorosilyl)cyclotrisilene-DMAP
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-09-19 deposited with the CCDC.	2020-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                89.3640(10)
_cell_angle_beta                 85.2090(10)
_cell_angle_gamma                76.7430(10)
_cell_formula_units_Z            2
_cell_length_a                   13.5086(3)
_cell_length_b                   15.0599(4)
_cell_length_c                   16.6833(4)
_cell_measurement_reflns_used    9712
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.94
_cell_measurement_theta_min      2.27
_cell_volume                     3291.92(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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0453
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            49798
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.225
_exptl_absorpt_coefficient_mu    0.350
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7081
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       plate
_exptl_crystal_F_000             1248
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     678
_refine_ls_number_reflns         15123
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0362P)^2^+1.1232P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0887
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11884
_reflns_number_total             15123
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03408h2.cif
_cod_data_source_block           tn49a_a
_cod_database_code               7705858
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.966
_shelx_estimated_absorpt_t_max   0.997
_shelx_res_checksum              87236