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_4065943
_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            'C30 H47 Al Hf'
_chemical_formula_weight         613.15
_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                69.7766(19)
_cell_angle_beta                 78.672(2)
_cell_angle_gamma                79.446(2)
_cell_formula_units_Z            4
_cell_length_a                   10.1020(3)
_cell_length_b                   17.5528(4)
_cell_length_c                   18.3908(4)
_cell_measurement_reflns_used    55772
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.23
_cell_measurement_theta_min      1.98
_cell_volume                     2976.74(14)
_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    'SIR2004 (Burla, 2005)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45795
_diffrn_reflns_theta_full        26.82
_diffrn_reflns_theta_max         26.82
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    3.548
_exptl_absorpt_correction_T_max  0.5788
_exptl_absorpt_correction_T_min  0.3795
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-SHAPE and X-RED32 (Stoe & Cie, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.221
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         12631
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0226
_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^)+(0.0325P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0509
_reflns_number_gt                10417
_reflns_number_total             12631
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100208g_si_002.cif
_cod_data_source_block           compound_3
_cod_original_cell_volume        2976.74(13)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4065943