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_4064116
_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            'C48 H96 Al4'
_chemical_formula_weight         781.17
_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                112.794(3)
_cell_angle_beta                 104.407(3)
_cell_angle_gamma                90.464(3)
_cell_formula_units_Z            1
_cell_length_a                   9.1515(4)
_cell_length_b                   11.5730(5)
_cell_length_c                   14.0031(6)
_cell_measurement_reflns_used    6574
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.56
_cell_measurement_theta_min      1.83
_cell_volume                     1315.16(11)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2005)'
_computing_data_reduction        X-AREA
_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  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21815
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.116
_exptl_absorpt_correction_T_max  0.9597
_exptl_absorpt_correction_T_min  0.7351
_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    0.986
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.973
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         6033
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1116P)^2^+0.1035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1689
_refine_ls_wR_factor_ref         0.1781
_reflns_number_gt                4418
_reflns_number_total             6033
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1011374_si_003.cif
_cod_data_source_block           ks1095
_cod_original_cell_volume        1315.15(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4064116