Generation of Dimethylsilylene and Allylidene Holmium Complexes from Trimethylsilylated Allyl Ligands
Rosemary E. White; Timothy P. Hanusa; Benjamin E. Kucera; Journal of the American Chemical Society 128 (2006) 9622–9623; doi:10.1021/ja062646i

data_4110767
_publ_contact_author_address
;Department of Chemistry
Vanderbilt University
Box 1822, Station B
Nashville, Tennessee  37235
USA
;
_publ_contact_author_email       t.hanusa@vanderbilt.edu
_publ_contact_author_fax         ' (615)343-1234'
_publ_contact_author_name        'Professor Timothy P. Hanusa'
_publ_contact_author_phone       ' (615)322-4667'
_publ_section_title
;
 Generation of Dimethylsilylene and Allylidene Holmium Complexes from
 Trimethylsilylated Allyl Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9622
_journal_page_last               9623
_journal_paper_doi               10.1021/ja062646i
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C36 H82 Ho2 Si8'
_chemical_formula_sum            'C36 H82 Ho2 Si8'
_chemical_formula_weight         1069.60
_chemical_name_common            05052
_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                84.786(5)
_cell_angle_beta                 75.757(5)
_cell_angle_gamma                69.666(5)
_cell_formula_units_Z            2
_cell_length_a                   11.537(5)
_cell_length_b                   12.043(5)
_cell_length_c                   20.903(5)
_cell_measurement_reflns_used    3659
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.18
_cell_volume                     2639.5(17)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART Platform CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31764
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.00
_exptl_absorpt_coefficient_mu    3.178
_exptl_absorpt_correction_T_max  0.5292
_exptl_absorpt_correction_T_min  0.3375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.544
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         12002
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+1.3288P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0819
_reflns_number_gt                9613
_reflns_number_total             12002
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja062646isi20060626_110515.cif
_cod_data_source_block           05052
_cod_database_code               4110767