Neutral and cationic trimethylsilylmethyl complexes of the rare earth metals supported by a crown ether: synthesis and structural characterization
Arndt, Stefan; Zeimentz, Peter M.; Spaniol, Thomas P.; Okuda, Jun; Honda, Masaru; Tatsumi, Kazuyuki; Dalton Transactions  (2003) 3622–; doi:10.1039/b305964b

data_7013263
_publ_section_title
;
 Neutral and cationic trimethylsilylmethyl complexes of the rare earth
 metals supported by a crown ether: synthesis and structural
 characterization
;
_journal_issue                   18
_journal_name_full               'Dalton Transactions'
_journal_page_first              3622
_journal_paper_doi               10.1039/b305964b
_journal_year                    2003
_chemical_formula_sum            'C20 H49 O4 Si3 Y'
_chemical_formula_weight         526.77
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 98.057(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7710(10)
_cell_length_b                   16.2169(8)
_cell_length_c                   19.1370(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.0
_cell_measurement_theta_min      6.6
_cell_volume                     3002.4(4)
_computing_cell_refinement       'REIND (Enraf nonius)'
_computing_data_collection       'CAD4 (Enraf nonius)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'CAD4 (Enraf-nonius)'
_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  0.1474
_diffrn_reflns_av_sigmaI/netI    0.3341
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            12264
_diffrn_reflns_theta_full        28.06
_diffrn_reflns_theta_max         28.06
_diffrn_reflns_theta_min         3.06
_diffrn_standards_decay_%        28
_diffrn_standards_interval_count 151
_diffrn_standards_interval_time  53
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.081
_exptl_absorpt_correction_T_max  0.8105
_exptl_absorpt_correction_T_min  0.5191
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   psi-scans
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         7122
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.2752
_refine_ls_R_factor_gt           0.0810
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1849
_reflns_number_gt                2478
_reflns_number_total             7122
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b305964b.txt
_cod_data_source_block           mh1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7013263