Heteroleptic Complexes of Lanthanum(III) and Neodymium(III) with Oxygen- or Nitrogen-Functionalized Tris(triorganosilyl)methyl Ligands
Bowman, Lyndsey J.; Izod, Keith; Clegg, William; Harrington, Ross W.; Organometallics 25 (2006) 2999–; doi:10.1021/om060072k

data_4075155
_publ_section_title
;
 Heteroleptic Complexes of Lanthanum(III) and Neodymium(III) with Oxygen-
 or Nitrogen-Functionalized Tris(triorganosilyl)methyl Ligands
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2999
_journal_paper_doi               10.1021/om060072k
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C20 H53 I La N O2 Si5'
_chemical_formula_sum            'C20 H53 I La N O2 Si5'
_chemical_formula_weight         745.89
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_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                   27.3564(6)
_cell_length_b                   27.3564(6)
_cell_length_c                   9.1519(4)
_cell_measurement_reflns_used    7454
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      23.6
_cell_measurement_theta_min      2.23
_cell_volume                     6849.0(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX2 CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6768
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_av_sigmaI/netI    0.0437
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            56296
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        5
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.339
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3008
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         7014
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0304P)^2^+10.2793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0812
_reflns_number_gt                5282
_reflns_number_total             7014
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om060072ksi20060308_062842.cif
_cod_data_source_block           sse0167_ki201_compound9
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               4075155