Reaction of LAlH2 with tert-Butyl Hydrogenperoxide under C-H Bond Activation and Substitution Leads to the Formation of a Pentacoordinated tert-Butylperoxo Aluminum Compound
S. Shravan Kumar; Sanjay Singh; Herbert W. Roesky; Jörg Magull; Inorganic Chemistry 44 (2005) 1199–1201; doi:10.1021/ic048336n

data_4308639
_publ_contact_author_address
;
Institut f\"ur Anorganische Chemie der Universit\"at G\"ottingen, 
Tammannstrasse 4, D-37077 G\"ottingen, Germany
;
_publ_contact_author_name        'Herbert W . Roesky'
_publ_section_title
;
Reaction of LAlH2 with tert-Butyl Hydrogenperoxide under C-H Bond
Activation and Substitution Leads to the Formation of a
Pentacoordinated tert-Butylperoxo Aluminum Compound
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1199
_journal_page_last               1201
_journal_paper_doi               10.1021/ic048336n
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C66 H103 Al3 N4 O9'
_chemical_formula_weight         1177.46
_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                89.609(4)
_cell_angle_beta                 80.735(5)
_cell_angle_gamma                67.620(5)
_cell_formula_units_Z            2
_cell_length_a                   13.6221(9)
_cell_length_b                   14.5119(8)
_cell_length_c                   18.5448(10)
_cell_measurement_temperature    133(2)
_cell_volume                     3339.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0974
_diffrn_reflns_av_sigmaI/netI    0.0610
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            49160
_diffrn_reflns_theta_full        24.81
_diffrn_reflns_theta_max         24.81
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    0.113
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1276
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     776
_refine_ls_number_reflns         11423
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0848P)^2^+0.9085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1561
_reflns_number_gt                8124
_reflns_number_total             11423
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048336nsi20041124_052632.cif
_cod_data_source_block           Compound_2
_cod_original_cell_volume        3339.7(3)
_cod_database_code               4308639