Rare-Earth Metal Alkyl, Amido, and Cyclopentadienyl Complexes Supported by Imidazolin-2-iminato Ligands: Synthesis, Structural Characterization, and Catalytic Application
Alexandra G. Trambitas; Tarun K. Panda; Jelena Jenter; Peter W. Roesky; Constantin Daniliuc; Cristian G. Hrib; Peter G. Jones; Matthias Tamm; Inorganic Chemistry 49 (2010) 2435–2446; doi:10.1021/ic9024052

data_4315088
_publ_contact_author
;
        Peter G. Jones
        Institut f\"ur Anorganische und Analytische Chemie
        Technische Universit\"at Braunschweig
        Postfach 3329
        38023 Braunschweig
        Germany
;
_publ_contact_author_email       p.jones@tu-bs.de
_publ_contact_author_fax         '049 531 391-5387'
_publ_contact_author_phone       '049 531 391-5382'
_publ_section_title
;
 Rare-Earth Metal Alkyl, Amido, and Cyclopentadienyl Complexes Supported
 by Imidazolin-2-iminato Ligands: Synthesis, Structural Characterization,
 and Catalytic Application
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2435
_journal_page_last               2446
_journal_paper_doi               10.1021/ic9024052
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C47 H88 N5 O2 Si4 Y'
_chemical_formula_weight         956.49
_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                85.783(5)
_cell_angle_beta                 84.522(5)
_cell_angle_gamma                77.737(5)
_cell_formula_units_Z            2
_cell_length_a                   12.2968(16)
_cell_length_b                   13.1799(18)
_cell_length_c                   17.669(2)
_cell_measurement_reflns_used    6779
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     2781.3(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       '\w- and \f-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  0.0537
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            52049
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.16
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.172
_exptl_absorpt_correction_T_max  0.8346
_exptl_absorpt_correction_T_min  0.6314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.154
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment
;
The hydrogens of the C37 methyl group were refined freely. 
The hydrogens of the other methyl groups were refined using a rigid groups, 
other H atoms were included using a riding model. 
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         13782
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0588P)^2^+1.6974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1222
_reflns_number_gt                10176
_reflns_number_total             13782
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9024052_si_002_05.cif
_cod_data_source_block           tarun79
_cod_database_code               4315088