Intramolecular Alkylation of α-Diimine Ligands Giving Amido—Imino and Diamido Scandium and Yttrium Complexes as Catalysts for Intramolecular Hydroamination/Cyclization
Kaneko, Hiroshi; Tsurugi, Hayato; Panda, Tarun K.; Mashima, Kazushi; Organometallics 29 (2010) 3463–; doi:10.1021/om1002667

data_4066067
_publ_section_title
;
 Intramolecular Alkylation of \a-Diimine Ligands Giving Amido---Imino and
 Diamido Scandium and Yttrium Complexes as Catalysts for Intramolecular
 Hydroamination/Cyclization
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3463
_journal_paper_doi               10.1021/om1002667
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C34 H61 N2 O Sc Si3'
_chemical_formula_sum            'C34 H61 N2 O Sc Si3'
_chemical_formula_weight         643.08
_chemical_name_common            3a
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.5070(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   40.5881(7)
_cell_length_b                   11.1135(2)
_cell_length_c                   17.4976(4)
_cell_measurement_reflns_used    77239
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      3.1
_cell_volume                     7784.3(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_molecular_graphics    Ortep-32
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            101799
_diffrn_reflns_theta_full        30.47
_diffrn_reflns_theta_max         30.47
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.307
_exptl_absorpt_correction_T_max  0.9848
_exptl_absorpt_correction_T_min  0.8565
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.097
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.340
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         11799
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.340
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0499P)^2^+12.5288P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1600
_refine_ls_wR_factor_ref         0.1624
_reflns_number_gt                10600
_reflns_number_total             11799
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1002667_si_001.cif
_cod_data_source_block           Sccomplex3a
_cod_database_code               4066067