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_4080967
_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         'C55 H106 Lu4 Si4'
_chemical_formula_sum            'C55 H106 Lu4 Si4'
_chemical_formula_weight         1579.64
_chemical_name_common            Cp'4Lu4HMe7
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 92.6550(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.0700(13)
_cell_length_b                   12.8629(7)
_cell_length_c                   41.788(2)
_cell_measurement_reflns_used    580
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     12387.2(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            34542
_diffrn_reflns_theta_full        26.05
_diffrn_reflns_theta_max         26.05
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    6.428
_exptl_absorpt_correction_T_max  0.5657
_exptl_absorpt_correction_T_min  0.4456
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6208
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.896
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         12154
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0105P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0427
_refine_ls_wR_factor_ref         0.0447
_reflns_number_gt                10111
_reflns_number_total             12154
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4002999_si_001.cif
_cod_data_source_block           5
_cod_original_cell_volume        12387.2(12)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4080967