Completing the Heterocubane Family [Cp*AlE]4 (E = O, S, Se, and Te) by Selective Oxygenation and Sulfuration of [Cp*Al]4: Density Functional Theory Calculations of [Cp*AlE]4 and Reactivity of [Cp*AlO]4 toward Hydrolysis.
Stelzer, Adrian C.; Hrobárik, Peter; Braun, Thomas; Kaupp, Martin; Braun-Cula, Beatrice; Inorganic chemistry 55 (2016) 4915–4923; doi:10.1021/acs.inorgchem.6b00462

data_4347672
_publ_section_title
;
 Completing the Heterocubane Family [Cp*AlE]4 (E = O, S, Se, and Te) by
 Selective Oxygenation and Sulfuration of [Cp*Al]4: Density Functional
 Theory Calculations of [Cp*AlE]4 and Reactivity of [Cp*AlO]4 toward
 Hydrolysis.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4915
_journal_page_last               4923
_journal_paper_doi               10.1021/acs.inorgchem.6b00462
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C100 H222 Al8 O50 Si8, 2(H2 O)'
_chemical_formula_sum            'C100 H226 Al8 O52 Si8'
_chemical_formula_weight         2701.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 100.622(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.8417(17)
_cell_length_b                   26.294(3)
_cell_length_c                   21.221(3)
_cell_measurement_reflns_used    9613
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.38
_cell_measurement_theta_min      2.48
_cell_volume                     7591.1(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker D8 VENTURE'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1295
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            218855
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.425
_diffrn_reflns_theta_min         2.248
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2916
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.120
_refine_diff_density_max         4.567
_refine_diff_density_min         -2.334
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     817
_refine_ls_number_reflns         18696
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1550
_refine_ls_R_factor_gt           0.1044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1898P)^2^+38.4654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2753
_refine_ls_wR_factor_ref         0.3272
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12263
_reflns_number_total             18696
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00462_si_001.cif
_cod_data_source_block           complex8
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4347672
_shelx_estimated_absorpt_t_min   0.941
_shelx_estimated_absorpt_t_max   0.977
_shelxl_version_number           2013-4
_shelx_res_checksum              85726
_shelx_hkl_checksum              8165