Lewis-Base Stabilization of the Parent Al(I) Hydride under Ambient Conditions.
Mellerup, Soren K.; Cui, Yunshu; Fantuzzi, Felipe; Schmid, Paul; Goettel, James T.; Bélanger-Chabot, Guillaume; Arrowsmith, Merle; Krummenacher, Ivo; Ye, Qing; Engel, Volker; Engels, Bernd; Braunschweig, Holger; Journal of the American Chemical Society 141 (2019) 16954–16960; doi:10.1021/jacs.9b09128

data_4127947
_publ_section_title
;
 Lewis-Base Stabilization of the Parent Al(I) Hydride under Ambient
 Conditions.
;
_journal_issue                   42
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16954
_journal_page_last               16960
_journal_paper_doi               10.1021/jacs.9b09128
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C49 H84 Al N2 Na Si'
_chemical_formula_sum            'C49 H84 Al N2 Na Si'
_chemical_formula_weight         779.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 100.226(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.647(4)
_cell_length_b                   27.147(7)
_cell_length_c                   13.569(4)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.72
_cell_measurement_theta_min      2.45
_cell_volume                     4947(2)
_computing_cell_refinement       'Saint+ ver. V8.37A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.37A (Bruker AXS)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CMOS area detector (Photon II)'
_diffrn_detector_area_resol_mean 7.5
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1061
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            106433
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_min         2.139
_diffrn_source                   'microfocus sealed tube (Incoatec ImS)'
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_T_max  0.7406
_exptl_absorpt_correction_T_min  0.7054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SadAbs 2016/2 (Bruker AXS)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.046
_exptl_crystal_description       Block
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.197
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         5042
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+5.9118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1117
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4063
_reflns_number_total             5042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b09128_si_004.cif
_cod_data_source_block           (cAAC)2AlHNa(tBu2MeSi)
_cod_database_code               4127947
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.986
_shelx_estimated_absorpt_t_max   0.992
_shelx_res_checksum              65121
_shelx_hkl_checksum              63032