Ln4(CH2)4 Cubane-Type Rare-Earth Methylidene Complexes Consisting of "(C5Me4SiMe3)LnCH2" Units (Ln = Tm, Lu)
Wen-Xiong Zhang; Zitao Wang; Masayoshi Nishiura; Zhenfeng Xi; Zhaomin Hou; Journal of the American Chemical Society 133 (2011) 5712–5715; doi:10.1021/ja200540b

data_4105981
_publ_section_title
;
 Ln4(CH2)4 Cubane-Type Rare-Earth Methylidene Complexes Consisting of
 "(C5Me4SiMe3)LnCH2" Units (Ln = Tm, Lu)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5712
_journal_page_last               5715
_journal_paper_doi               10.1021/ja200540b
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C64 H104 Lu4 Si4'
_chemical_formula_weight         1685.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 115.768(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.3484(13)
_cell_length_b                   23.487(3)
_cell_length_c                   13.4630(14)
_cell_measurement_temperature    173(2)
_cell_volume                     3516.4(7)
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            18173
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    5.667
_exptl_absorpt_correction_T_max  0.2812
_exptl_absorpt_correction_T_min  0.2102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         5.068
_refine_diff_density_min         -2.341
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         6296
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0639
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+65.4158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.1561
_reflns_number_gt                5155
_reflns_number_total             6296
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja200540b_si_006.cif
_cod_data_source_block           4-Lu
_cod_original_cell_volume        3516.3(6)
_cod_database_code               4105981