Reactivity of Boryl- and Silyl-Substituted Carbenoids toward Alkynes: Insertion and Cycloaddition Chemistry
Protchenko, Andrey V.; Blake, Matthew P.; Schwarz, Andrew D.; Jones, Cameron; Mountford, Philip; Aldridge, Simon; Organometallics 34 (2015) 2126–; doi:10.1021/om501252m

data_4085471
_publ_section_title
;
 Reactivity of Boryl- and Silyl-Substituted Carbenoids toward Alkynes:
 Insertion and Cycloaddition Chemistry
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2126
_journal_paper_doi               10.1021/om501252m
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C46 H62 N2 Si2 Sn2'
_chemical_formula_sum            'C46 H62 N2 Si2 Sn2'
_chemical_formula_weight         936.56
_chemical_name_systematic
;
{Sn(N(Dipp)SiMe3)(CCPh)}2
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             12-12-11
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 111.4663(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.01113(11)
_cell_length_b                   14.37422(10)
_cell_length_c                   14.20295(11)
_cell_measurement_reflns_used    15247
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      3
_cell_volume                     2282.05(3)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.020
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22420
_diffrn_reflns_theta_full        75.067
_diffrn_reflns_theta_max         76.599
_diffrn_reflns_theta_min         3.955
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.436
_exptl_absorpt_correction_T_max  0.39
_exptl_absorpt_correction_T_min  0.15
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.66
_refine_diff_density_min         -0.45
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0565
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4527
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0195
_refine_ls_R_factor_gt           0.0188
_refine_ls_shift/su_max          0.0022880
_refine_ls_shift/su_mean         0.0000553
_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: 
 4.62 -4.51 1.59 -0.523 -1.45 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0184
_refine_ls_wR_factor_gt          0.0183
_refine_ls_wR_factor_ref         0.0182
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                4594
_reflns_number_total             4759
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.72
_oxford_diffrn_Wilson_scale      0.08
_oxford_refine_ls_r_factor_ref   0.0183
_oxford_refine_ls_scale          3.5326(19)
_oxford_reflns_number_all        4740
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title 'ADS_310 in P2(1)/c'
_cod_data_source_file            om501252m_si_002.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 4085469--4085474.cif.'
_cod_original_cell_volume        2282.05(4)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4085471