Self-reducing precursors for aluminium metal thin films: evaluation of stable aluminium hydrides for vapor phase aluminium deposition.
Huster, Niklas; Mullins, Rita; Nolan, Michael; Devi, Anjana; Dalton transactions (Cambridge, England : 2003) 53 (2024) 7711–7720; doi:10.1039/d4dt00709c

data_7715721
_publ_section_title
;
 Self-reducing precursors for aluminium metal thin films: evaluation of
 stable aluminium hydrides for vapor phase aluminium deposition.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7711
_journal_page_last               7720
_journal_paper_doi               10.1039/d4dt00709c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C10 H28 Al2 N2'
_chemical_formula_sum            'C10 H28 Al2 N2'
_chemical_formula_weight         230.30
_chemical_name_systematic        Bis(3-dimethylaminopropylalan)
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Hygroscopic,Heat-sensitive,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-17
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-03-08 deposited with the CCDC.	2024-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                65.927(7)
_cell_angle_beta                 79.774(6)
_cell_angle_gamma                85.949(6)
_cell_formula_units_Z            1
_cell_length_a                   7.0931(5)
_cell_length_b                   7.1791(6)
_cell_length_c                   7.9448(6)
_cell_measurement_reflns_used    2589
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.5870
_cell_measurement_theta_min      6.1470
_cell_volume                     363.51(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4409
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -124.00 -79.00   1.00    1.00    --  -41.47 -99.00-150.00   45
  2  \w      2.00  99.00   1.00    1.00    --   41.47-125.00 120.00   97
  3  \w      2.00  99.00   1.00    1.00    --   41.47-125.00 -30.00   97
  4  \w     15.00 118.00   1.00    1.00    --   41.47  37.00-150.00  103
  5  \w     15.00 118.00   1.00    1.00    --   41.47  37.00 -60.00  103
  6  \w     17.00 158.00   1.00    1.00    --  106.28   0.00 -90.00  141
  7  \w     22.00 109.00   1.00    1.00    --  106.28 -94.00-180.00   87
  8  \w     32.00 134.00   1.00    1.00    --  106.28 -45.00-180.00  102
  9  \w     76.00 158.00   1.00    1.00    --  106.28  61.00 -90.00   82
 10  \w     28.00 112.00   1.00    1.00    --  106.28-111.00 -60.00   84
 11  \w     22.00 109.00   1.00    1.00    --  106.28 -94.00   0.00   87
 12  \w     28.00 112.00   1.00    1.00    --  106.28-111.00 120.00   84
 13  \w     32.00 135.00   1.00    1.00    --  106.28 -50.00 -68.00  103
 14  \w     79.00 158.00   1.00    1.00    --  106.28 111.00 -30.00   79
 15  \w     32.00 134.00   1.00    1.00    --  106.28 -45.00  60.00  102
 16  \w   -115.00 -12.00   1.00    1.00    --  -41.47 -57.00  30.00  103
 17  \w   -120.00  -8.00   1.00    1.00    --  -41.47 -77.00 120.00  112
 18  \w    -71.00  32.00   1.00    1.00    --  -41.47  57.00-150.00  103
 19  \w      8.00 120.00   1.00    1.00    --   41.47  77.00 -30.00  112
 20  \w     76.00 158.00   1.00    1.00    --  106.28  30.00  90.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1115591000
_diffrn_orient_matrix_UB_12      -0.1747523000
_diffrn_orient_matrix_UB_13      0.1312918000
_diffrn_orient_matrix_UB_21      -0.1470401000
_diffrn_orient_matrix_UB_22      -0.1549485000
_diffrn_orient_matrix_UB_23      0.0123528000
_diffrn_orient_matrix_UB_31      0.1210026000
_diffrn_orient_matrix_UB_32      -0.0263308000
_diffrn_orient_matrix_UB_33      -0.1701490000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0146
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4027
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.010
_diffrn_reflns_theta_min         6.184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.569
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.052
_exptl_crystal_description       block
_exptl_crystal_F_000             128
_exptl_crystal_recrystallization_method Sublimation
_exptl_crystal_size_max          0.297
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.185
_refine_diff_density_max         0.247
_refine_diff_density_min         -0.157
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0237
_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^)+(0.0320P)^2^+0.1181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0633
_refine_ls_wR_factor_ref         0.0643
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1351
_reflns_number_total             1414
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00709c2.cif
_cod_data_source_block           NH015_a
_cod_depositor_comments          'Adding full bibliography for 7715721.cif.'
_cod_database_code               7715721
_shelx_shelxl_version_number     2019/3
_cell_oxdiff_length_a            7.0931(5)
_cell_oxdiff_length_b            7.1791(5)
_cell_oxdiff_length_c            7.9448(6)
_cell_oxdiff_angle_alpha         65.927(7)
_cell_oxdiff_angle_beta          79.774(6)
_cell_oxdiff_angle_gamma         85.949(6)
_cell_oxdiff_volume              363.51(5)
_cell_oxdiff_measurement_reflns_used 2589
_oxdiff_exptl_absorpt_empirical_full_min 0.834
_oxdiff_exptl_absorpt_empirical_full_max 1.156
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_ac3_digest_frames
;
01bd3f15fd55006159368959fe5d399d5b00029f18d
;
_diffrn_oxdiff_ac3_digest_hkl
;
0174bcd3803dae0ea7a42f269a5617a59630b1
;
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         'Al C5 H14 N'
_chemical_oxdiff_usercomment     'eventuell dimer'
_shelx_res_checksum              80062