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_4105978
_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            'C42 H81 Lu3 Si3'
_chemical_formula_weight         1195.25
_chemical_name_common            '[Cp'LuMe2]3'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   9.1108(7)
_cell_length_b                   18.1931(14)
_cell_length_c                   29.074(2)
_cell_measurement_temperature    173(2)
_cell_volume                     4819.1(6)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            25208
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    6.197
_exptl_absorpt_correction_T_max  0.5761
_exptl_absorpt_correction_T_min  0.4566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.115
_refine_diff_density_min         -1.036
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.003(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         8473
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0209P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0495
_reflns_number_gt                7968
_reflns_number_total             8473
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja200540b_si_003.cif
_cod_data_source_block           7310zwx
_cod_database_code               4105978