Rare-Earth Metal Tris(trimethylsilylmethyl) Anionic Complexes Bearing One 1-Phenyl-2,3,4,5-tetrapropylcyclopentadienyl Ligand: Synthesis, Structural Characterization, and Application
Ling Xu; Zitao Wang; Wen-Xiong Zhang; Zhenfeng Xi; Inorganic Chemistry 51 (2012) 11941–11948; doi:10.1021/ic3018369

data_4330954
_publ_section_title
;
 Rare-Earth Metal Tris(trimethylsilylmethyl) Anionic Complexes Bearing One
 1-Phenyl-2,3,4,5-tetrapropylcyclopentadienyl Ligand: Synthesis,
 Structural Characterization, and Application
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11941
_journal_page_last               11948
_journal_paper_doi               10.1021/ic3018369
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C57 H63 Lu O5'
_chemical_formula_weight         1003.04
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 105.18(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.627(3)
_cell_length_b                   16.234(3)
_cell_length_c                   23.257(5)
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.55
_cell_volume                     4965.4(19)
_computing_cell_refinement       Rapid-AUTO
_computing_data_collection       'Rapid-AUTO (Rigaku,2000)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC,2000)'
_computing_molecular_graphics    'Siemens SHELXTL V4.2,(Sheldrick,1990)'
_computing_publication_material  SHELXL-97,(Sheldrick,1997)
_computing_structure_refinement  SHELXL-97,(Sheldrick,1997)
_computing_structure_solution    SHELXS-97,(Sheldrick,1997)
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku RAXIS RAPID IP'
_diffrn_measurement_method       \W
_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  0.0955
_diffrn_reflns_av_sigmaI/netI    0.2636
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            11360
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.035
_exptl_absorpt_correction_T_max  0.9051
_exptl_absorpt_correction_T_min  0.8224
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
                                  HIGASHI, T. (1995). Abscor-empirical
                                  Absorption Correction based on Fourier
                                  Series Approximation.
                                  Rigaku Corporation,Tokyo,Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       block
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.568
_refine_diff_density_min         -1.363
_refine_diff_density_rms         0.218
_refine_ls_extinction_coef       0.00694(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         11360
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1261
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0190P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.1440
_reflns_number_gt                4513
_reflns_number_total             11360
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3018369_si_002_6.cif
_cod_data_source_block           2-Lu
_cod_original_cell_volume        4965.4(17)
_cod_database_code               4330954