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_4110768
_publ_contact_author_address
;Department of Chemistry
Vanderbilt University
Box 22, 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         'C35 H76 Ho2 O2 Si6'
_chemical_formula_sum            'C35 H76 Ho2 O2 Si6'
_chemical_formula_weight         1027.36
_chemical_name_common            05099
_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                82.540(2)
_cell_angle_beta                 87.940(2)
_cell_angle_gamma                78.290(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5760(11)
_cell_length_b                   11.8757(13)
_cell_length_c                   19.561(2)
_cell_measurement_reflns_used    3802
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.37
_cell_volume                     2385.2(4)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Siemens 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     0.71073
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27613
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.05
_exptl_absorpt_coefficient_mu    3.469
_exptl_absorpt_correction_T_max  0.7084
_exptl_absorpt_correction_T_min  0.4680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.204
_refine_diff_density_min         -1.286
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         10794
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+9.0832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0890
_reflns_number_gt                8571
_reflns_number_total             10794
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja062646isi20060626_110548.cif
_cod_data_source_block           05099
_cod_database_code               4110768