Cationic Methyl Complexes of the Rare-Earth Metals: An Experimental and Computational Study on Synthesis, Structure, and Reactivity
Mathias U. Kramer; Dominique Robert; Stefan Arndt; Peter M. Zeimentz; Thomas P. Spaniol; Ahmed Yahia; Laurent Maron; Odile Eisenstein; Jun Okuda; Inorganic Chemistry 47 (2008) 9265–9278; doi:10.1021/ic801259n

data_4306458
_publ_contact_author_address
;
        Institute for Inorganic Chemistry
        RWTH Aachen University
        Landoltweg 1
        D-52074 Aachen
        Germany
;
_publ_contact_author_email       jun.okuda@ac.rwth-aachen.de
_publ_contact_author_fax         '0049 241 8092644'
_publ_contact_author_name        'Jun Okuda'
_publ_contact_author_phone       '0049 241 8094645'
_publ_section_title
;
Cationic Methyl Complexes of the Rare-Earth Metals: An Experimental and
Computational Study on Synthesis, Structure, and Reactivity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9265
_journal_page_last               9278
_journal_paper_doi               10.1021/ic801259n
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C29 H71 Li3 O5 Y2'
_chemical_formula_weight         698.50
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           41
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'A 2 -2ab'
_symmetry_space_group_name_H-M   'A b a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.681(3)
_cell_length_b                   16.058(3)
_cell_length_c                   16.549(5)
_cell_measurement_reflns_used    2398
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      21.27
_cell_measurement_theta_min      2.19
_cell_volume                     4167.1(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.853
_diffrn_measured_fraction_theta_max 0.853
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega 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  0.0679
_diffrn_reflns_av_sigmaI/netI    0.1073
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13801
_diffrn_reflns_theta_full        29.08
_diffrn_reflns_theta_max         29.08
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    2.798
_exptl_absorpt_correction_T_max  0.4338
_exptl_absorpt_correction_T_min  0.2030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.600
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.002(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         4639
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1185
_refine_ls_R_factor_gt           0.0519
_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^)+(0.0528P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1241
_reflns_number_gt                2730
_reflns_number_total             4639
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801259n_si_002_02.cif
_cod_data_source_block           1'-Y
_cod_database_code               4306458