New polynuclear aluminium oxoalkoxides. Crystal structures of [Al5(μ5-O)(μ-OBui)8(OBui)5] and [Al8(μ4-O)2(μ-OH)2(μ-OBui)10(OBui)8]
Isaac Abrahams; Donald C. Bradley; Halina Chudzynska; Majid Motevalli; Robin A. Sinclair; J. Chem. Soc., Dalton Trans.  (2002) 259–266; doi:10.1039/b105876m

data_7010958
_publ_section_title
;
 New polynuclear aluminium oxoalkoxides. Crystal structures of
 [Al5(\m5-O)(\m-OBui)8(OBui)5] and
 [Al8(\m4-O)2(\m-OH)2(\m-OBui)10(OBui)8]
;
_journal_issue                   2
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              259
_journal_page_last               266
_journal_paper_doi               10.1039/b105876m
_journal_year                    2002
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C52 H117 Al5 O14'
_chemical_formula_structural     'C52 H117 AL5 O14'
_chemical_formula_sum            'C52 H117 Al5 O14'
_chemical_formula_weight         1101.36
_space_group_IT_number           103
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      103
_symmetry_space_group_name_Hall  'P 4 -2c'
_symmetry_space_group_name_H-M   'P 4 c c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location
ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta5
_audit_creation_date             2001-10-10T14:29:01-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4930(10)
_cell_length_b                   13.4930(10)
_cell_length_c                   36.699(4)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.27
_cell_measurement_theta_min      2.13
_cell_measurement_wavelength     0.71069
_cell_volume                     6681.5(10)
_computing_cell_refinement
'MADNES REFINE (Pulgrath & Messerschmidt, 1989)'
_computing_data_collection
'MADNES MADONL (Pulgrath & Messerschmidt, 1989)'
_computing_data_reduction
'MADNES ABSURD (Pulgrath & Messerschmidt, 1989)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97(Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0713
_diffrn_reflns_av_sigmaI/netI    0.0643
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            28548
_diffrn_reflns_theta_full        27.17
_diffrn_reflns_theta_max         27.17
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.136
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Walker, N. & Stuart, D (1983) Acta. Cryst. A39, 158-166
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.095
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.21(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         6834
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      0.907
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.558
_refine_ls_shift/su_mean         0.035
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1265
_refine_ls_wR_factor_ref         0.1335
_reflns_number_gt                4449
_reflns_number_total             6834
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b105876m.txt
_cod_data_source_block           altnew
_cod_database_code               7010958
_exptl_absorpt_factor_mur        0.063