Synthesis and Structures of Ln(II) and Ln(III) Dialkyls Derived from LnI2(Ln = Nd, Tm, Yb)
Bowman, Lyndsey J.; Izod, Keith; Clegg, William; Harrington, Ross W.; Organometallics 26 (2007) 2646–; doi:10.1021/om0611711

data_4072969
_publ_section_title
;
 Synthesis and Structures of Ln(II) and Ln(III) Dialkyls Derived from
 LnI2(Ln = Nd, Tm, Yb)
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2646
_journal_paper_doi               10.1021/om0611711
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C25 H63 Nd O4 Si6'
_chemical_formula_sum            'C25 H63 Nd O4 Si6'
_chemical_formula_weight         740.53
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 107.460(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.6513(7)
_cell_length_b                   16.9051(12)
_cell_length_c                   12.0511(9)
_cell_measurement_reflns_used    4762
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      21.9
_cell_measurement_theta_min      2.40
_cell_volume                     1875.6(2)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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     0.6751
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1109
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20957
_diffrn_reflns_theta_full        28.80
_diffrn_reflns_theta_max         28.80
_diffrn_reflns_theta_min         2.39
_diffrn_standards_decay_%        10
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.601
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             778
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.081
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.119(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         20957
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1155
_refine_ls_wR_factor_ref         0.1299
_reflns_number_gt                15758
_reflns_number_total             20957
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om0611711si20061222_060252.cif
_cod_data_source_block           ki221_compound10
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4072969