Functionalized Cyclic Disilenes via Ring Expansion of Cyclotrisilenes with Isocyanides
Ohmori, Yu; Ichinohe, Masaaki; Sekiguchi, Akira; Cowley, Michael J.; Huch, Volker; Scheschkewitz, David; Organometallics 32 (2013) 1591–; doi:10.1021/om400054u

data_4080521
_publ_section_title
;
 Functionalized Cyclic Disilenes via Ring Expansion of Cyclotrisilenes
 with Isocyanides
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1591
_journal_paper_doi               10.1021/om400054u
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C45 H93 N Si7'
_chemical_formula_weight         844.83
_chemical_name_systematic
; 
 1,2,3,3-Tetrakis(di-tert-butylmethylsilyl)-4-[N-(2,6-dimethylphenyl)imino]- 
 1,2,3-trisilacyclobutene 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.714(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.0059(6)
_cell_length_b                   14.7795(5)
_cell_length_c                   20.1475(6)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      28.05
_cell_measurement_theta_min      2.24
_cell_volume                     5367.2(3)
_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(1)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29883
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    0.206
_exptl_absorpt_correction_T_max  0.9568
_exptl_absorpt_correction_T_min  0.9072
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
SADABS Sheldrick 1996 
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.046
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.758
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         12057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0418
_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/[\s^2^(Fo^2^)+(0.0489P)^2^+5.2803P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1122
_reflns_number_gt                9908
_reflns_number_total             12057
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400054u_si_006.cif
_cod_data_source_block           Compound2d
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P2(1)/n  '
_cod_database_code               4080521