Synthesis and Structural Characterization of a Terminal Hydroxide Containing Alumoxane via Hydrolysis of Aluminum Hydrides
Ying Peng; Guangcai Bai; Hongjun Fan; Denis Vidovic; Herbert W. Roesky; Jörg Magull; Inorganic Chemistry 43 (2004) 1217–1219; doi:10.1021/ic0351803

data_4310618
_publ_section_title
;
 Synthesis and Structural Characterization of a Terminal Hydroxide
 Containing Alumoxane via Hydrolysis of Aluminum Hydrides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1217
_journal_page_last               1219
_journal_paper_doi               10.1021/ic0351803
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C68 H104 Al2 N5 O3'
_chemical_formula_weight         1093.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.01(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.128(3)
_cell_length_b                   21.500(4)
_cell_length_c                   22.083(4)
_cell_measurement_temperature    133(2)
_cell_volume                     6642(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.1377
_diffrn_reflns_av_sigmaI/netI    0.1515
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            39741
_diffrn_reflns_theta_full        24.87
_diffrn_reflns_theta_max         24.87
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.090
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2388
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.722
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     770
_refine_ls_number_reflns         11408
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.722
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0231P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.1035
_reflns_number_gt                5592
_reflns_number_total             11408
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0351803si20040109_080143.cif
_cod_data_source_block           p254
_cod_database_code               4310618