Synthesis and temperature-dependent NMR studies of monomeric and dimeric tris(dialkylamido)alanes
Schumann, Erik; Böhme, Uwe; Brendler, Erica; Mertens, Florian; Dalton Transactions  (2022) –; doi:10.1039/D2DT00508E

data_7709941
_publ_section_title
;
 Synthesis and temperature-dependent NMR studies of monomeric and dimeric
 tris(dialkylamido)alanes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00508E
_journal_year                    2022
_chemical_formula_moiety         'C30 H66 Al2 N12'
_chemical_formula_sum            'C30 H66 Al2 N12'
_chemical_formula_weight         648.90
_chemical_melting_point          452
_space_group_crystal_system      tetragonal
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_space_group_name_Hall           '-P 4bc'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
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_audit_update_record
;
2021-07-20 deposited with the CCDC.	2022-03-31 downloaded from the CCDC.
;
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_computing_cell_refinement       'STOE X-AREA'
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_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015)'
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_diffrn_detector                 'image plate (34 cm diameter)'
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_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      ' 243 frames, detector distance = 114 mm'
_diffrn_measurement_device       '2-circle goniometer'
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_diffrn_radiation_monochromator  'plane graphite'
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_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0410
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_diffrn_reflns_Laue_measured_fraction_full 0.997
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_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
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_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            51858
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.912
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
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_exptl_absorpt_correction_T_max  0.8483
_exptl_absorpt_correction_T_min  0.2999
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-RED; Stoe, 2009'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.187
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0448P)^2^+1.3866P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0963
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3931
_reflns_number_total             4556
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00508e2.cif
_cod_data_source_block           ES107sq_1
_cod_original_cell_volume        3971.9(3)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               7709941
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.953
_shelx_estimated_absorpt_t_max   0.979
_shelx_res_checksum              69898
_shelx_hkl_checksum              48266
_shelx_fab_checksum              22836