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_4115964
_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         'C34 H40 Lu N Si3'
_chemical_formula_sum            'C34 H40 Lu N Si3'
_chemical_formula_weight         721.91
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                78.198(8)
_cell_angle_beta                 67.611(8)
_cell_angle_gamma                63.935(7)
_cell_formula_units_Z            2
_cell_length_a                   11.6187(7)
_cell_length_b                   12.1293(8)
_cell_length_c                   13.9320(11)
_cell_measurement_temperature    293
_cell_volume                     1629.1(2)
_computing_cell_refinement       'IPDS (STOE)'
_computing_data_collection       'IPDS (STOE)'
_computing_data_reduction        'IPDS (STOE)'
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Giaccovazzo)'
_diffrn_measurement_device_type  'IPDS (STOE)'
_diffrn_measurement_method       oscillation
_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  0.0591
_diffrn_reflns_av_sigmaI/netI    0.0637
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9550
_diffrn_reflns_reduction_process
;
 ?
;
_diffrn_reflns_theta_max         25.66
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    3.16
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Decay (STOE)'
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack   none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_hydrogen_treatment    'H-atom refinement: see text '
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         5683
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.916
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          2.229
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/[\
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0769
_reflns_number_gt                4486
_reflns_number_total             5683
_reflns_threshold_expression     >2sigma(i)
_cod_data_source_file            ja992786a_1.cif
_cod_data_source_block           15e
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[\' was changed to
'calc'. New tag '_refine_ls_weighting_details' was created. The value
of the new tag was set to 'w=1/[\'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4115964