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_4085473
_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         'C32 H59 N1 Si6'
_chemical_formula_sum            'C32 H59 N Si6'
_chemical_formula_weight         626.34
_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   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                101.382(3)
_cell_angle_beta                 91.531(2)
_cell_angle_gamma                113.170(3)
_cell_formula_units_Z            2
_cell_length_a                   9.9961(3)
_cell_length_b                   12.1873(4)
_cell_length_c                   17.8179(5)
_cell_measurement_reflns_used    11145
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      4
_cell_volume                     1943.18(12)
_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 0.983
_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  0.021
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19323
_diffrn_reflns_theta_full        73.466
_diffrn_reflns_theta_max         76.527
_diffrn_reflns_theta_min         4.051
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.152
_exptl_absorpt_correction_T_max  0.65
_exptl_absorpt_correction_T_min  0.65
_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_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.49
_refine_diff_density_min         -1.62
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1106
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         7260
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.0005426
_refine_ls_shift/su_mean         0.0000307
_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: 
 -0.317 -19.0 -8.89 -7.24 -5.93 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0286
_refine_ls_wR_factor_gt          0.0278
_refine_ls_wR_factor_ref         0.0276
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                7467
_reflns_number_total             8062
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.88
_oxford_diffrn_Wilson_scale      0.03
_oxford_refine_ls_r_factor_ref   0.0434
_oxford_refine_ls_scale          6.015(5)
_oxford_reflns_number_all        8033
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_cod_data_source_file            om501252m_si_002.cif
_cod_data_source_block           10
_cod_depositor_comments
'Adding full bibliography for 4085469--4085474.cif.'
_cod_original_cell_volume        1943.17(12)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C32 H59 N1 Si6'
_cod_database_code               4085473
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
END                                                                             
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_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.001000 = SI(3) TO C(27) 
U(IJ) .0, 0.001000 = SI(3) TO C(28) 
U(IJ) .0, 0.001000 = SI(3) TO C(29) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;