An N,N'-Diamidocarbene: Studies in C-H Insertion, Reversible Carbonylation, and Transition-Metal Coordination Chemistry
Todd W. Hudnall; Christopher W. Bielawski; Journal of the American Chemical Society 131 (2009) 16039–16041; doi:10.1021/ja907481w

data_4105333
_publ_section_title
;
 An N,N'-Diamidocarbene: Studies in C-H Insertion, Reversible
 Carbonylation, and Transition-Metal Coordination Chemistry
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16039
_journal_page_last               16041
_journal_paper_doi               10.1021/ja907481w
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         1,3-{Dipp}4,6-{Oxo}-5-{Me2}-2CO-HMDS
_chemical_formula_sum            'C37 H58 N3 Na O3 Si2'
_chemical_formula_weight         672.03
_chemical_name_common            6-KetoDipp-Ketene
_chemical_name_systematic
; 
 ? 
;
_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                82.83(3)
_cell_angle_beta                 87.57(3)
_cell_angle_gamma                79.23(3)
_cell_formula_units_Z            2
_cell_length_a                   10.617(2)
_cell_length_b                   11.695(2)
_cell_length_c                   16.402(3)
_cell_measurement_temperature    150(2)
_cell_volume                     1984.7(7)
_computing_cell_refinement       'Collect software, Nonius B.V. 1998'
_computing_data_collection       'Collect software, Nonius B.V. 1998'
_computing_data_reduction
'DENZO and Scalepack (Otwinoski and Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '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  0.1483
_diffrn_reflns_av_sigmaI/netI    0.3061
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11477
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.136
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         6771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.2894
_refine_ls_R_factor_gt           0.1038
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0041P)^2^+3.5539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1437
_refine_ls_wR_factor_ref         0.2015
_reflns_number_gt                2414
_reflns_number_total             6771
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja907481w_si_002_3.cif
_cod_data_source_block           3NaHMDS
_cod_database_code               4105333