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_4319521
_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 H72 Cl Li N3 O3 Si6 Tb'
_chemical_formula_weight         892.76
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 93.6350(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.6729(4)
_cell_length_b                   17.4492(2)
_cell_length_c                   21.2795(3)
_cell_measurement_temperature    173(2)
_cell_volume                     9513.4(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_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  0.0426
_diffrn_reflns_av_sigmaI/netI    0.0502
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            49251
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.79
_exptl_absorpt_coefficient_mu    1.723
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_F_000             3728
_refine_diff_density_max         2.468
_refine_diff_density_min         -1.271
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.064
_refine_ls_goodness_of_fit_obs   1.178
_refine_ls_matrix_type           full
_refine_ls_number_parameters     876
_refine_ls_number_reflns         16727
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_restrained_S_obs      1.178
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_obs          0.0506
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1525
_refine_ls_wR_factor_obs         0.1367
_reflns_number_observed          11288
_reflns_number_total             16763
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9912023_4.cif
_cod_data_source_block           just40
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4319521