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_4072968
_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 O4 Si6 Tm'
_chemical_formula_sum            'C25 H63 O4 Si6 Tm'
_chemical_formula_weight         765.22
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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            4
_cell_length_a                   23.6067(15)
_cell_length_b                   9.6827(6)
_cell_length_c                   16.0840(10)
_cell_measurement_reflns_used    25353
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.49
_cell_measurement_theta_min      2.27
_cell_volume                     3676.4(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_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      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'thin-slice \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  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25600
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.73
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.635
_exptl_absorpt_correction_T_max  0.726
_exptl_absorpt_correction_T_min  0.486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.376
_refine_diff_density_min         -3.393
_refine_diff_density_rms         0.154
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.047(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.372
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         6438
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.372
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0000P)^2^+16.2559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0907
_reflns_number_gt                6053
_reflns_number_total             6438
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om0611711si20061222_060252.cif
_cod_data_source_block           ki218_compound9
_cod_database_code               4072968