C2-Symmetric ansa-Lanthanidocene Complexes. Synthesis via Silylamine Elimination and β-SiH Agostic Rigidity
Jörg Eppinger; Michael Spiegler; Wolfgang Hieringer; Wolfgang A. Herrmann; Reiner Anwander; Journal of the American Chemical Society 122 (2000) 3080–3096; doi:10.1021/ja992786a

data_4115967
_publ_contact_author_address
;
       Anorganisch-chemisches Institut der
       Technischen Universit\"at M\"unchen
       Lichtenbergstrasse 4
       D-85747 Garching bei M\"unchen
;
_publ_contact_author_email       reiner.anwander@ch.tum.de
_publ_contact_author_fax         '089 289 13473'
_publ_contact_author_name
;
 Reiner Anwander
;
_publ_contact_author_phone       '089 289 14378'
_publ_section_title
;
 C2-Symmetric ansa-Lanthanidocene Complexes. Synthesis via Silylamine
 Elimination and \b-SiH Agostic Rigidity
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3080
_journal_page_last               3096
_journal_paper_doi               10.1021/ja992786a
_journal_volume                  122
_journal_year                    2000
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C26 H36 Lu N Si3'
_chemical_formula_sum            'C26 H36 Lu N Si3'
_chemical_formula_weight         621.80
_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'
_cell_angle_alpha                90
_cell_angle_beta                 108.145(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0153(4)
_cell_length_b                   11.8938(5)
_cell_length_c                   15.7695(5)
_cell_measurement_temperature    273
_cell_volume                     2676.21(16)
_computing_cell_refinement       'Scalepack (HKL)'
_computing_data_collection       'Collect (Nonius)'
_computing_data_reduction        'Nprocess (Nonius)'
_computing_molecular_graphics    'PLATON (SPEK, 1990)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Giaccovazza)'
_diffrn_ambient_temperature      273
_diffrn_measurement_device_type  'Kappa CCD / MACH3 (Nonius)'
_diffrn_measurement_method       phi-scans/omega-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'FR 591 rotating anode (Nonius)'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0165
_diffrn_reflns_av_sigmaI/netI    0.0277
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4071
_diffrn_reflns_reduction_process
;
 ?
;
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         4.92
_exptl_absorpt_coefficient_mu    3.84
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Scalepack (Nonius)'
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack   none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    'H-atom refinement: see text '
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         2203
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0206
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_wR_factor_gt          0.0469
_refine_ls_wR_factor_ref         0.0474
_reflns_number_gt                2085
_reflns_number_total             2203
_reflns_threshold_expression     >2sigma(i)
_cod_data_source_file            ja992786a_4.cif
_cod_data_source_block           13e
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4115967