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_4075158
_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         'C30 H76 I2 Nd2 O6 Si6'
_chemical_formula_sum            'C30 H76 I2 Nd2 O6 Si6'
_chemical_formula_weight         1243.73
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                68.672(14)
_cell_angle_beta                 72.213(13)
_cell_angle_gamma                87.620(18)
_cell_formula_units_Z            1
_cell_length_a                   9.406(3)
_cell_length_b                   12.4259(14)
_cell_length_c                   13.660(2)
_cell_measurement_reflns_used    851
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.50
_cell_volume                     1411.8(6)
_computing_cell_refinement       EvalCCD
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        EvalCCD
_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      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            38418
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         4.05
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.068
_exptl_absorpt_correction_T_max  0.508
_exptl_absorpt_correction_T_min  0.330
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       slab
_exptl_crystal_F_000             614
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.608
_refine_diff_density_min         -1.678
_refine_diff_density_rms         0.165
_refine_ls_extinction_coef       0.0079(13)
_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   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         6450
_refine_ls_number_restraints     339
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1088P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1596
_refine_ls_wR_factor_ref         0.1757
_reflns_number_gt                4606
_reflns_number_total             6450
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om060072ksi20060308_062842.cif
_cod_data_source_block           ki208a_compound11
_cod_original_cell_volume        1411.7(5)
_cod_database_code               4075158