Evidence for the Existence of Terminal Scandium Imidos: Mechanistic Studies Involving Imido-Scandium Bond Formation and C-H Activation Reactions
Benjamin F. Wicker; Hongjun Fan; Anne K. Hickey; Marco G. Crestani; Jennifer Scott; Maren Pink; Daniel J. Mindiola; Journal of the American Chemical Society 134 (2012) 20081–20096; doi:10.1021/ja307279r

data_4118981
_publ_section_title
;
 Evidence for the Existence of Terminal Scandium Imidos: Mechanistic
 Studies Involving Imido-Scandium Bond Formation and C-H Activation
 Reactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              20081
_journal_page_last               20096
_journal_paper_doi               10.1021/ja307279r
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C44 H64 N3 P2 Sc'
_chemical_formula_weight         741.88
_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                81.190(6)
_cell_angle_beta                 70.859(4)
_cell_angle_gamma                74.747(5)
_cell_formula_units_Z            2
_cell_length_a                   10.151(3)
_cell_length_b                   14.758(4)
_cell_length_c                   15.422(5)
_cell_measurement_reflns_used    3390
_cell_measurement_temperature    150(2)
_cell_measurement_theta_min      2.18
_cell_volume                     2100.1(11)
_computing_cell_refinement       'APEX II v2010.11.3 (Bruker, 2010)'
_computing_data_collection       'APEX II v2010.11.3 (Bruker, 2010)'
_computing_data_reduction        'APEX II v2010.11.3 (Bruker, 2010)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2010)'
_computing_publication_material  'SHELXTL (Bruker, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2010)'
_computing_structure_solution    'SIR-2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 83.33
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
'0.30 degree frames measured for 5 seconds each'
_diffrn_measurement_device       'APEX Kappa Duo'
_diffrn_measurement_device_type  Kappa
_diffrn_measurement_method       'omega and phi 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  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0736
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19974
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    0.284
_exptl_absorpt_correction_T_max  0.9859
_exptl_absorpt_correction_T_min  0.9586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         7369
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+0.4207P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1148
_reflns_number_gt                4861
_reflns_number_total             7369
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja307279r_si_002.cif
_cod_data_source_block           11043
_cod_original_cell_volume        2100.0(10)
_cod_database_code               4118981