Hydrogenolysis and Protonation of Polymetallic Lutetium Methylidene and Methyl Complexes
Li, Tingting; Nishiura, Masayoshi; Cheng, Jianhua; Zhang, Wenxiong; Li, Yang; Hou, Zhaomin; Organometallics 32 (2013) 4142–; doi:10.1021/om4002999

data_4080966
_publ_section_title
;
 Hydrogenolysis and Protonation of Polymetallic Lutetium Methylidene and
 Methyl Complexes
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4142
_journal_paper_doi               10.1021/om4002999
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C52 H93 Lu4 Si4,C24 B F20'
_chemical_formula_sum            'C76 H93 B F20 Lu4 Si4'
_chemical_formula_weight         2209.55
_chemical_name_common            '[Cp'4Lu4(CH2)3(CH3)][B(C6F5)4]'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 93.665(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.345(8)
_cell_length_b                   27.761(14)
_cell_length_c                   19.677(10)
_cell_measurement_reflns_used    258
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     8365(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0721
_diffrn_reflns_av_sigmaI/netI    0.0843
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            43245
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    4.821
_exptl_absorpt_correction_T_max  0.3787
_exptl_absorpt_correction_T_min  0.2832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       flat
_exptl_crystal_F_000             4296
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.057
_refine_diff_density_min         -1.552
_refine_diff_density_rms         0.208
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     877
_refine_ls_number_reflns         14663
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0816P)^2^+3.9732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1418
_refine_ls_wR_factor_ref         0.1492
_reflns_number_gt                12355
_reflns_number_total             14663
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4002999_si_001.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4080966