Synthesis, Structural Characterization, Catalytic Properties, and Theoretical Study of Compounds Containing an Al-O-M (M = Ti, Hf) Core
Prabhuodeyara M. Gurubasavaraj; Swadhin K. Mandal; Herbert W. Roesky; Rainer B. Oswald; Aritra Pal; Mathias Noltemeyer; Inorganic Chemistry 46 (2007) 1056–1061; doi:10.1021/ic060538r

data_4306830
_publ_section_title
;
Synthesis, Structural Characterization, Catalytic Properties, and
Theoretical Study of Compounds Containing an Al-O-M (M = Ti, Hf) Core
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1056
_journal_page_last               1061
_journal_paper_doi               10.1021/ic060538r
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C41 H57 Al Hf N2 O'
_chemical_formula_weight         799.36
_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                88.28(2)
_cell_angle_beta                 87.17(2)
_cell_angle_gamma                68.47(2)
_cell_formula_units_Z            2
_cell_length_a                   9.921(2)
_cell_length_b                   10.276(2)
_cell_length_c                   19.616(3)
_cell_measurement_temperature    133(2)
_cell_volume                     1857.9(6)
_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_measurement_device_type  IPDS2
_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  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31559
_diffrn_reflns_theta_full        24.81
_diffrn_reflns_theta_max         24.81
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    2.864
_exptl_absorpt_correction_T_max  0.5981
_exptl_absorpt_correction_T_min  0.4803
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.00037(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         6373
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0178
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0166P)^2^+0.8224P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0369
_refine_ls_wR_factor_ref         0.0375
_reflns_number_gt                5808
_reflns_number_total             6373
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060538rsi20060330_035204.cif
_cod_data_source_block           rh
_cod_database_code               4306830