Synthesis and Single-Crystal X-ray Diffraction Examination of a Structurally Homologous Series of Tetracoordinate Heteroleptic Anionic Lanthanide Complexes: Ln{N[Si(CH3)2CH2CH2Si(CH3)2]}3(μ-Cl)Li(L)3 [Ln = Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb; (L)3= (THF)3, (Et2O)3, (THF)2(Et2O)]
Oliver Just; William S. Rees; Inorganic Chemistry 40 (2001) 1751–1755; doi:10.1021/ic9912023

data_4319526
_publ_section_title
;
 Synthesis and Single-Crystal X-ray Diffraction Examination of a
 Structurally Homologous Series of Tetracoordinate Heteroleptic Anionic
 Lanthanide Complexes: Ln{N[Si(CH3)2CH2CH2Si(CH3)2]}3(\m-Cl)Li(L)3 [Ln =
 Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb; (L)3= (THF)3, (Et2O)3, (THF)2(Et2O)]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1751
_journal_page_last               1755
_journal_paper_doi               10.1021/ic9912023
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C30 H78 Cl Li N3 O3 Si6 Yb'
_chemical_formula_weight         912.92
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 98.2000(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6763(2)
_cell_length_b                   20.6996(3)
_cell_length_c                   18.7475(2)
_cell_measurement_temperature    173(2)
_cell_volume                     4868.94(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            40080
_diffrn_reflns_theta_full        26.70
_diffrn_reflns_theta_max         26.70
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    2.152
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1908
_refine_diff_density_max         1.605
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       0.00033(8)
_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   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         10279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+6.8373P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0919
_reflns_number_gt                8088
_reflns_number_total             10279
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9912023_9.cif
_cod_data_source_block           just25
_cod_original_cell_volume        4868.95(12)
_cod_database_code               4319526