Isocyanide insertion and cyclization reactions to form indolines using pincer-type complexes of scandium.
Wicker, Benjamin F.; Pink, Maren; Mindiola, Daniel J.; Dalton transactions (Cambridge, England : 2003) 40 (2011) 9020–9025; doi:10.1039/c1dt10287g

data_7016354
_publ_section_title
;
 Isocyanide insertion and cyclization reactions to form indolines using
 pincer-type complexes of scandium.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9020
_journal_page_last               9025
_journal_paper_doi               10.1039/c1dt10287g
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C74 H97 N6 P2 Sc, 2.5(C5 H12)'
_chemical_formula_sum            'C86.5 H127 N6 P2 Sc'
_chemical_formula_weight         1357.84
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                86.436(2)
_cell_angle_beta                 70.6750(10)
_cell_angle_gamma                65.6990(10)
_cell_formula_units_Z            2
_cell_length_a                   14.4984(8)
_cell_length_b                   15.6478(9)
_cell_length_c                   20.5567(12)
_cell_measurement_reflns_used    1859
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.57
_cell_measurement_theta_min      1.43
_cell_volume                     3996.1(4)
_computing_cell_refinement       'Bruker APEX 2 (2009)'
_computing_data_collection       'Bruker APEX 2 (2009)'
_computing_data_reduction        'Bruker APEX 2 (2009)'
_computing_molecular_graphics    'Diamond 3.2d (2010)'
_computing_publication_material  'WinGX (2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  kappa
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0456
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            81527
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         1.43
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker APEX II Kappa Duo'
_exptl_absorpt_coefficient_mu    0.179
_exptl_absorpt_correction_T_max  0.9737
_exptl_absorpt_correction_T_min  0.9651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (R. Blessing, 1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1478
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.865
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     903
_refine_ls_number_reflns         22328
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1600
_refine_ls_wR_factor_ref         0.1791
_reflns_number_gt                16314
_reflns_number_total             22328
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10287g.txt
_cod_data_source_block           10052
_cod_original_formula_sum        'C86.50 H127 N6 P2 Sc'
_cod_database_code               7016354