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_4076396
_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_formula_moiety         'C55 H65 N6 Lu, 2.5(C7 H8)'
_chemical_formula_sum            'C72.5 H85 Lu N6'
_chemical_formula_weight         1215.44
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.575(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.199(2)
_cell_length_b                   25.257(3)
_cell_length_c                   15.9042(19)
_cell_measurement_reflns_used    1712
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      16.309
_cell_measurement_theta_min      2.405
_cell_volume                     6085.9(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT, SADABS, XPREP'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      230(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.1400
_diffrn_reflns_av_sigmaI/netI    0.2422
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            49098
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    1.670
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.6678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2532
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.762
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.859
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         10525
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.859
_refine_ls_R_factor_all          0.1170
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1764P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1228
_refine_ls_wR_factor_ref         0.1560
_reflns_number_gt                5753
_reflns_number_total             10525
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2011672_si_002.cif
_cod_data_source_block           13
_cod_original_cell_volume        6086.1(13)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4076396