Covalent Lanthanide Chemistry Near the Limit of Weak Bonding: Observation of (CpSiMe3)3Ce-ECp* and a Comprehensive Density Functional Theory Analysis of Cp3Ln-ECp (E = Al, Ga)
Jamin L. Krinsky; Stefan G. Minasian; John Arnold; Inorganic Chemistry 50 (2011) 345–357; doi:10.1021/ic102028d

data_4324168
_publ_section_title
;
 Covalent Lanthanide Chemistry Near the Limit of Weak Bonding: Observation
 of (CpSiMe3)3Ce-ECp* and a Comprehensive Density Functional Theory
 Analysis of Cp3Ln-ECp (E = Al, Ga)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              345
_journal_page_last               357
_journal_paper_doi               10.1021/ic102028d
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C24 H39 Ce Si3'
_chemical_formula_sum            'C24 H39 Ce Si3'
_chemical_formula_weight         551.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   8.3780(5)
_cell_length_b                   22.2086(15)
_cell_length_c                   29.1454(18)
_cell_measurement_reflns_used    14194
_cell_measurement_temperature    453(2)
_cell_measurement_theta_max      25.295
_cell_measurement_theta_min      2.691
_cell_volume                     5422.9(6)
_computing_cell_refinement       'Bruker SAINT v7.07'
_computing_data_collection       'Bruker SMART v5.631'
_computing_data_reduction        'Bruker SAINT v7.07'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      453(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '\w 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  0.0809
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            55419
_diffrn_reflns_theta_full        25.33
_diffrn_reflns_theta_max         25.33
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    1.819
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.803
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2264
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.203
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4941
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0308P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0737
_reflns_number_gt                3511
_reflns_number_total             4941
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102028d_si_002.cif
_cod_data_source_block           sgm625m
_cod_database_code               4324168