New Highly Active Heteroscorpionate-Containing Lutetium Catalysts for the Hydroamination of Aminoalkenes: Isolation and Structural Characterization of a Dipyrrolidinide–Lutetium Complex
Otero, Antonio; Lara-Sánchez, Agustín; Nájera, Carmen; Fernández-Baeza, Juan; Márquez-Segovia, Isabel; Castro-Osma, José Antonio; Martínez, Javier; Sánchez-Barba, Luis F.; Rodríguez, Ana M.; Organometallics 31 (2012) 2244–; doi:10.1021/om2011672

data_4076395
_publ_section_title
;
 New Highly Active Heteroscorpionate-Containing Lutetium Catalysts for the
 Hydroamination of Aminoalkenes: Isolation and Structural Characterization
 of a Dipyrrolidinide--Lutetium Complex
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              2244
_journal_paper_doi               10.1021/om2011672
_journal_volume                  31
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C33 H59 Lu N4 O Si2'
_chemical_formula_sum            'C33 H59 Lu N4 O Si2'
_chemical_formula_weight         758.99
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 114.459(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.9720(6)
_cell_length_b                   19.5503(10)
_cell_length_c                   10.5346(6)
_cell_measurement_reflns_used    3154
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      19.708
_cell_measurement_theta_min      2.366
_cell_volume                     1869.47(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      230(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0481
_diffrn_reflns_av_sigmaI/netI    0.0848
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12069
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    2.733
_exptl_absorpt_correction_T_max  0.7910
_exptl_absorpt_correction_T_min  0.6247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.509
_refine_diff_density_min         -1.564
_refine_diff_density_rms         0.168
_refine_ls_abs_structure_details 'Flack H D (1983), 2975 Friedel pairs'
_refine_ls_abs_structure_Flack   0.016(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         6353
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0637
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0888P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.1572
_reflns_number_gt                5398
_reflns_number_total             6353
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2011672_si_002.cif
_cod_data_source_block           3
_cod_original_cell_volume        1869.47(18)
_cod_original_sg_symbol_H-M      P21
_cod_database_code               4076395