Reactions of the Five-Membered Hafnacyclocumulene Cp2Hf(η4-t-Bu-C4-t-Bu) with the Lewis Acids Tris(pentafluorophenyl)borane and Diisobutylaluminum Hydride
Burlakov, Vladimir V.; Beweries, Torsten; Kaleta, Katharina; Bogdanov, Vyacheslav S.; Arndt, Perdita; Baumann, Wolfgang; Spannenberg, Anke; Shur, Vladimir B.; Rosenthal, Uwe; Organometallics 29 (2010) 2367–; doi:10.1021/om100208g

data_4065942
_publ_section_title
;
 Reactions of the Five-Membered Hafnacyclocumulene Cp2Hf(\h4-t-Bu-C4-t-Bu)
 with the Lewis Acids Tris(pentafluorophenyl)borane and Diisobutylaluminum
 Hydride
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2367
_journal_paper_doi               10.1021/om100208g
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C68 H56 B D6 F15 Hf2'
_chemical_formula_weight         1531.97
_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                83.164(3)
_cell_angle_beta                 76.599(3)
_cell_angle_gamma                89.156(3)
_cell_formula_units_Z            2
_cell_length_a                   10.1365(3)
_cell_length_b                   15.8667(5)
_cell_length_c                   19.3646(6)
_cell_measurement_reflns_used    53055
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      1.59
_cell_volume                     3007.86(17)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2005)'
_computing_data_reduction        X-AREA
_computing_molecular_graphics    'XP in SHELXTL'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38900
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    3.537
_exptl_absorpt_correction_T_max  0.6270
_exptl_absorpt_correction_T_min  0.4165
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-SHAPE and X-RED32 (Stoe & Cie, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1508
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.941
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     773
_refine_ls_number_reflns         11168
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0245
_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^)+(0.0196P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0433
_refine_ls_wR_factor_ref         0.0452
_reflns_number_gt                8536
_reflns_number_total             11168
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100208g_si_002.cif
_cod_data_source_block           compound_2
_cod_original_cell_volume        3007.86(16)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C68 H56 D6 B F15 Hf2'
_cod_database_code               4065942