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_7010959
_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         'C72 H164 Al8 O22'
_chemical_formula_structural     'C72 H164 AL8 O22'
_chemical_formula_sum            'C72 H164 Al8 O22'
_chemical_formula_weight         1597.87
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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             2001-06-12T17:21:27-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 99.81(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.282(5)
_cell_length_b                   19.276(8)
_cell_length_c                   18.192(4)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.4425
_cell_measurement_theta_min      10.1385
_cell_measurement_wavelength     0.71073
_cell_volume                     10118(5)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_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      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
x-axis points to radiation source
the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.2244E-2
_diffrn_orient_matrix_UB_12      0.15304E-1
_diffrn_orient_matrix_UB_13      0.51774E-1
_diffrn_orient_matrix_UB_21      0.25811E-1
_diffrn_orient_matrix_UB_22      0.33671E-1
_diffrn_orient_matrix_UB_23      -0.1048E-2
_diffrn_orient_matrix_UB_31      -0.23006E-1
_diffrn_orient_matrix_UB_32      0.36433E-1
_diffrn_orient_matrix_UB_33      -0.02068
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_sigmaI/netI    0.1315
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9062
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1.62
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        5
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.137
_exptl_absorpt_correction_T_max  0.9995
_exptl_absorpt_correction_T_min  0.9569
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
Number of psi-scan sets used was   3
Theta correction was applied.
Averaged transmission function was used.
No Fourier smoothing was applied.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.049
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.00005(6)
_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   0.948
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         8876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.1997
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.321
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+2.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1517
_refine_ls_wR_factor_ref         0.2009
_reflns_number_gt                3822
_reflns_number_total             8876
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b105876m.txt
_cod_data_source_block           alumh
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7010959
_exptl_absorpt_factor_mur        0
_exptl_absorpt_correction_t_ave  0.9744
_diffrn_standards_decay_corr_max 1.088
_diffrn_standards_decay_corr_min 0.97