Addition of a Cyclopropyl Alkyne to Tetramesityldisilene: Evidence for a Biradical Intermediate and Formation of a Stable 1,2-Disilacyclohepta-3,4-diene
Gottschling, Stephen E.; Milnes, Kaarina K.; Jennings, Michael C.; Baines, Kim M.; Organometallics 24 (2005) 3811–; doi:10.1021/om0504250

data_4076006
_publ_section_title
;
 Addition of a Cyclopropyl Alkyne to Tetramesityldisilene:&#x00A0;
 Evidence for a Biradical Intermediate and Formation of a Stable
 1,2-Disilacyclohepta-3,4-diene
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              3811
_journal_paper_doi               10.1021/om0504250
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C49 H58 O Si2'
_chemical_formula_weight         719.13
_chemical_name_systematic
; 
1,1,2,2-Tetramesityl-6-methoxy-5-methyl-7-phenyl-1,2-disilacyclohepta-3,4-diene
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                74.628(3)
_cell_angle_beta                 74.146(3)
_cell_angle_gamma                77.839(2)
_cell_formula_units_Z            4
_cell_length_a                   15.9840(8)
_cell_length_b                   16.6589(7)
_cell_length_c                   17.1723(6)
_cell_measurement_temperature    295(2)
_cell_volume                     4193.9(3)
_computing_cell_refinement       'Nonius DENZO'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Nonius DENZO'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       'phi/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  0.064
_diffrn_reflns_av_sigmaI/netI    0.1486
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32293
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.119
_exptl_absorpt_correction_T_max  0.9852
_exptl_absorpt_correction_T_min  0.9105
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     817
_refine_ls_number_reflns         14711
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1903
_refine_ls_R_factor_gt           0.0781
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1246P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2008
_refine_ls_wR_factor_ref         0.2526
_reflns_number_gt                6664
_reflns_number_total             14711
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0504250si20050527_121006.cif
_cod_data_source_block           04037
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4076006