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_4115968
_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_formula_sum            'C75 H88 N2 Si6 Y2'
_chemical_formula_weight         1363.86
_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                72.396(5)
_cell_angle_beta                 75.824(6)
_cell_angle_gamma                69.896(5)
_cell_formula_units_Z            1
_cell_length_a                   11.1193(6)
_cell_length_b                   11.9449(5)
_cell_length_c                   14.8399(8)
_cell_measurement_temperature    193
_cell_volume                     1742.24(17)
_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-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR97 (Giaccovazzo)'
_diffrn_ambient_temperature      193
_diffrn_measurement_device       '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  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21813
_diffrn_reflns_reduction_process
;
 ?
;
_diffrn_reflns_theta_max         24.66
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    1.80
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_F_000             714
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.978
_refine_diff_density_min         -0.454
_refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.973
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5393
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_obs          0.0358
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef F^2^
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0666P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0944
_refine_ls_wR_factor_obs         0.0944
_reflns_number_observed          4525
_reflns_number_total             5536
_reflns_observed_criterion       >2sigma(i)
_cod_data_source_file            ja992786a_5.cif
_cod_data_source_block           15b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0666P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'.
New tag '_refine_ls_weighting_details' was created. The value of the
new tag was set to 'w=1/[s^2^(Fo^2^)+( 0.0666P)^2^+0.0000P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1742.2(2)
_cod_original_formula_sum        ' C75 H88 N2 Si6 Y2'
_cod_database_code               4115968