A Stable Two-Coordinate Acyclic Silylene
Andrey V. Protchenko; Krishna Hassomal Birjkumar; Deepak Dange; Andrew D. Schwarz; Dragoslav Vidovic; Cameron Jones; Nikolas Kaltsoyannis; Philip Mountford; Simon Aldridge; Journal of the American Chemical Society 134 (2012) 6500–6503; doi:10.1021/ja301042u

data_4117836
_publ_contact_author
;
 Prof S. Aldridge
 Chemistry Research Laboratory
 Mansfield Road
 Oxford
 OX1 3TA
 UK
;
_publ_contact_author_email       Simon.Aldridge@chem.ox.ac.uk
_publ_contact_author_fax         '+44 1865 272690'
_publ_contact_author_phone       '+44 1865 285201'
_publ_section_title
;
 A Stable Two-Coordinate Acyclic Silylene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6500
_journal_page_last               6503
_journal_paper_doi               10.1021/ja301042u
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C41 H64 B1 N3 Si2'
_chemical_formula_sum            'C41 H64 B N3 Si2'
_chemical_formula_weight         665.96
_chemical_name_systematic
;
H2Si{B(NDippCH)2}{N(Dipp)SiMe3}
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 100.0774(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0507(2)
_cell_length_b                   21.7304(4)
_cell_length_c                   17.4807(3)
_cell_measurement_reflns_used    9253
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     4132.99(13)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.046
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17705
_diffrn_reflns_theta_full        26.648
_diffrn_reflns_theta_max         27.472
_diffrn_reflns_theta_min         5.096
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.116
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.070
_exptl_crystal_description       prism
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.26
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.1274
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         5404
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.0002359
_refine_ls_shift/su_mean         0.0000256
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.755 0.367 0.643 0.137 0.157 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0713
_refine_ls_wR_factor_gt          0.0457
_refine_ls_wR_factor_ref         0.0420
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              28
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                6131
_reflns_number_total             9398
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.28
_oxford_diffrn_Wilson_scale      13.85
_oxford_refine_ls_r_factor_ref   0.0438
_oxford_refine_ls_scale          0.3093(4)
_oxford_reflns_number_all        9398
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ja301042u_si_002_7.cif
_cod_data_source_block           COMPOUND_6
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C41 H64 B1 N3 Si2'
_cod_database_code               4117836