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_4306829
_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 N2 O Ti'
_chemical_formula_weight         668.77
_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                90.13(2)
_cell_angle_beta                 90.55(2)
_cell_angle_gamma                114.14(2)
_cell_formula_units_Z            2
_cell_length_a                   9.572(2)
_cell_length_b                   10.422(2)
_cell_length_c                   20.060(3)
_cell_measurement_temperature    100(2)
_cell_volume                     1826.0(7)
_computing_cell_refinement       'Bruker SAINT (V. 7.01A, Siemens 2003)'
_computing_data_collection       'Proteum (Version 1.40, Bruker 2002)'
_computing_data_reduction        'Bruker SAINT (V. 7.01A, Siemens 2003)'
_computing_molecular_graphics    'Bruker AXS SHELXTL (V. 6.12)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.602
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker three circle diffractometer'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_monochromator  'mirror system'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0482
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15952
_diffrn_reflns_theta_full        58.92
_diffrn_reflns_theta_max         58.92
_diffrn_reflns_theta_min         4.41
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.464
_exptl_absorpt_correction_T_max  0.6386
_exptl_absorpt_correction_T_min  0.6386
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         5056
_refine_ls_number_restraints     704
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0603
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+4.3735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1265
_reflns_number_gt                4220
_reflns_number_total             5056
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060538rsi20060330_035143.cif
_cod_data_source_block           temp1
_cod_original_cell_volume        1826.0(6)
_cod_database_code               4306829