Reductive Reactivity of the Organolanthanide Hydrides, [(C5Me5)2LnH]x, Leads to an sa-Allyl Cyclopentadienyl (η5-C5Me4CH2-C5Me4CH2-η3)2- and Trianionic Cyclooctatetraenyl (C8H7)3- Ligands
William J. Evans; Benjamin M. Schmiege; Sara E. Lorenz; Kevin A. Miller; Timothy M. Champagne; Joseph W. Ziller; Antonio G. DiPasquale; Arnold L. Rheingold; Journal of the American Chemical Society 130 (2008) 8555–8563; doi:10.1021/ja8011726

data_4107955
_publ_section_title
;
 Reductive Reactivity of the Organolanthanide Hydrides, [(C5Me5)2LnH]x,
 Leads to an sa-Allyl Cyclopentadienyl (\h5-C5Me4CH2-C5Me4CH2-\h3)2- and
 Trianionic Cyclooctatetraenyl (C8H7)3- Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8555
_journal_page_last               8563
_journal_paper_doi               10.1021/ja8011726
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C66 H86 S2 Y2'
_chemical_formula_weight         1121.29
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                69.574(2)
_cell_angle_beta                 76.507(2)
_cell_angle_gamma                83.370(2)
_cell_formula_units_Z            1
_cell_length_a                   10.3399(11)
_cell_length_b                   10.4821(11)
_cell_length_c                   14.6925(16)
_cell_measurement_temperature    163(2)
_cell_volume                     1450.1(3)
_computing_cell_refinement       'Bruker SMART/SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0342
_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       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16112
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        '< 1.0'
_diffrn_standards_interval_count 'initial 50 frames recollected'
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    2.102
_exptl_absorpt_correction_T_max  0.6435
_exptl_absorpt_correction_T_min  0.5528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         7023
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+1.6406P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.0982
_reflns_number_gt                6248
_reflns_number_total             7023
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8011726-file008.cif
_cod_data_source_block           bms3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4107955