Reactions of Five-Membered Metallacyclocumulenes Cp2M(η4-t-Bu-C4-t-Bu) (M = Ti, Zr) with Diisobutylaluminum Hydride
Burlakov, Vladimir V.; Kaleta, Katharina; Beweries, Torsten; Arndt, Perdita; Baumann, Wolfgang; Spannenberg, Anke; Shur, Vladimir B.; Rosenthal, Uwe; Organometallics 30 (2011) 1157–; doi:10.1021/om1011374

data_4064115
_publ_section_title
;
 Reactions of Five-Membered Metallacyclocumulenes Cp2M(\h4-t-Bu-C4-t-Bu)
 (M = Ti, Zr) with Diisobutylaluminum Hydride
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1157
_journal_paper_doi               10.1021/om1011374
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C33 H50 Al O Ti'
_chemical_formula_weight         537.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_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                 106.406(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.4074(6)
_cell_length_b                   9.9765(2)
_cell_length_c                   20.8968(7)
_cell_measurement_reflns_used    6009
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.29
_cell_measurement_theta_min      2.01
_cell_volume                     3081.31(18)
_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_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0609
_diffrn_reflns_av_sigmaI/netI    0.0666
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            49369
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.329
_exptl_absorpt_correction_T_max  0.9700
_exptl_absorpt_correction_T_min  0.8709
_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    1.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.852
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         7071
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      0.853
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0997
_reflns_number_gt                4258
_reflns_number_total             7071
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1011374_si_002.cif
_cod_data_source_block           ks1107
_cod_original_cell_volume        3081.30(17)
_cod_original_sg_symbol_H-M      P2/c
_cod_database_code               4064115