# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_NH015_a
_database_code_depnum_ccdc_archive 'CCDC 2338876'
loop_
_audit_author_name
_audit_author_address
'Martin Wilken'
;Ruhr University Bochum
Germany
;
_audit_update_record             
;
2024-03-08 deposited with the CCDC.	2024-04-11 downloaded from the CCDC.
;
#

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        Bis(3-dimethylaminopropylalan)
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H28 Al2 N2'
_chemical_formula_sum            'C10 H28 Al2 N2'
_chemical_formula_weight         230.30
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

#

_cell_length_a                   7.0931(5)
_cell_length_b                   7.1791(6)
_cell_length_c                   7.9448(6)
_cell_angle_alpha                65.927(7)
_cell_angle_beta                 79.774(6)
_cell_angle_gamma                85.949(6)
_cell_volume                     363.51(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2589
_cell_measurement_theta_min      6.1470
_cell_measurement_theta_max      72.5870
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.052
_exptl_crystal_F_000             128
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.297
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.185
_exptl_absorpt_coefficient_mu    1.569
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.86950
_exptl_absorpt_correction_T_max  1.00000
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4409
_diffrn_reflns_number            4027
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_av_R_equivalents  0.0146
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         6.184
_diffrn_reflns_theta_max         73.010
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1414
_reflns_number_gt                1351
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0320P)²+0.1181P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1414
_refine_ls_number_parameters     101
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0237
_refine_ls_wR_factor_ref         0.0643
_refine_ls_wR_factor_gt          0.0633
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.23071(12) 0.65966(13) 0.67511(12) 0.0143(2) Uani 1 1 d . . . . .
C1 C 0.30576(16) 0.86387(17) 0.89659(16) 0.0188(2) Uani 1 1 d . . . . .
H1A H 0.385(2) 0.975(2) 0.881(2) 0.028 Uiso 1 1 d . U . . .
H1B H 0.252(2) 0.803(2) 1.027(2) 0.028 Uiso 1 1 d . U . . .
C2 C 0.14388(17) 0.94053(17) 0.77905(16) 0.0191(2) Uani 1 1 d . . . . .
H1I H 0.036(2) 0.996(2) 0.838(2) 0.029 Uiso 1 1 d . U . . .
H1F H 0.192(2) 1.051(2) 0.657(2) 0.029 Uiso 1 1 d . U . . .
Al1 Al 0.44590(4) 0.64400(5) 0.83557(4) 0.01446(12) Uani 1 1 d . . . . .
C3 C 0.06881(15) 0.76435(17) 0.74925(16) 0.0170(2) Uani 1 1 d . . . . .
H1JJ H 0.007(2) 0.660(2) 0.871(2) 0.026 Uiso 1 1 d . U . . .
H1D H -0.024(2) 0.804(2) 0.667(2) 0.026 Uiso 1 1 d . U . . .
C4 C 0.29683(16) 0.78463(18) 0.47442(15) 0.0202(2) Uani 1 1 d . . . . .
H4A H 0.192356 0.805558 0.406642 0.030 Uiso 1 1 calc R U . . .
H4B H 0.398916 0.715177 0.426818 0.030 Uiso 1 1 calc R U . . .
H4C H 0.342061 0.914165 0.459725 0.030 Uiso 1 1 calc R U . . .
C5 C 0.16554(17) 0.45928(17) 0.69548(17) 0.0199(2) Uani 1 1 d . . . . .
H1H H 0.051(2) 0.472(2) 0.644(2) 0.030 Uiso 1 1 d . U . . .
H1C H 0.140(2) 0.367(2) 0.827(2) 0.030 Uiso 1 1 d . U . . .
H1 H 0.261(2) 0.400(2) 0.635(2) 0.030 Uiso 1 1 d . U . . .
H2 H 0.392(2) 0.417(2) 0.9786(19) 0.024(3) Uiso 1 1 d . . . . .
H3 H 0.619(2) 0.665(2) 0.682(2) 0.030(4) Uiso 1 1 d . . . . .

#


#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C5 1.4788(13) . ?
N1 C4 1.4813(14) . ?
N1 C3 1.4932(13) . ?
N1 Al1 2.1254(9) . ?
C1 C2 1.5380(15) . ?
C1 Al1 1.9864(12) . ?
C1 H1A 0.966(16) . ?
C1 H1B 0.957(15) . ?
C2 C3 1.5243(15) . ?
C2 H1I 0.972(15) . ?
C2 H1F 0.989(16) . ?
Al1 Al1 2.7877(7) 2_667 ?
Al1 H2 1.588(14) . ?
Al1 H3 1.536(14) . ?
C3 H1JJ 0.995(15) . ?
C3 H1D 0.960(15) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H1H 0.955(16) . ?
C5 H1C 0.972(15) . ?
C5 H1 0.942(16) . ?

#

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C5 N1 C4 108.73(9) . . ?
C5 N1 C3 109.58(8) . . ?
C4 N1 C3 109.83(8) . . ?
C5 N1 Al1 114.54(7) . . ?
C4 N1 Al1 110.66(7) . . ?
C3 N1 Al1 103.35(6) . . ?
C2 C1 Al1 108.40(7) . . ?
C2 C1 H1A 111.2(9) . . ?
Al1 C1 H1A 114.7(9) . . ?
C2 C1 H1B 109.8(9) . . ?
Al1 C1 H1B 106.5(9) . . ?
H1A C1 H1B 106.1(12) . . ?
C3 C2 C1 109.52(9) . . ?
C3 C2 H1I 107.4(9) . . ?
C1 C2 H1I 113.0(9) . . ?
C3 C2 H1F 109.9(9) . . ?
C1 C2 H1F 110.1(9) . . ?
H1I C2 H1F 106.8(12) . . ?
C1 Al1 N1 87.37(4) . . ?
C1 Al1 Al1 107.35(4) . 2_667 ?
N1 Al1 Al1 135.04(3) . 2_667 ?
C1 Al1 H2 116.3(5) . . ?
N1 Al1 H2 93.4(5) . . ?
Al1 Al1 H2 41.8(5) 2_667 . ?
C1 Al1 H3 128.0(5) . . ?
N1 Al1 H3 97.0(5) . . ?
Al1 Al1 H3 105.3(5) 2_667 . ?
H2 Al1 H3 115.1(7) . . ?
N1 C3 C2 110.26(9) . . ?
N1 C3 H1JJ 106.5(8) . . ?
C2 C3 H1JJ 110.1(8) . . ?
N1 C3 H1D 108.5(8) . . ?
C2 C3 H1D 114.2(9) . . ?
H1JJ C3 H1D 106.9(12) . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C5 H1H 111.1(9) . . ?
N1 C5 H1C 110.4(9) . . ?
H1H C5 H1C 108.1(12) . . ?
N1 C5 H1 110.4(9) . . ?
H1H C5 H1 108.9(12) . . ?
H1C C5 H1 107.8(12) . . ?

#

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Al1 C1 C2 C3 32.72(11) . . . . ?
C5 N1 C3 C2 164.59(9) . . . . ?
C4 N1 C3 C2 -76.04(11) . . . . ?
Al1 N1 C3 C2 42.07(9) . . . . ?
C1 C2 C3 N1 -51.70(12) . . . . ?

#

_refine_diff_density_max         0.247
_refine_diff_density_min         -0.157
_refine_diff_density_rms         0.038
######### additional information out of the cif_od #######  
_audit_creation_date             2020-07-17
_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_ambient_environment      N~2~
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_reflns_av_sigmaI/netI    0.0190
_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_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -124.00 -79.00   1.00    1.00    --  -41.47 -99.00-150.00   45
  2  ω      2.00  99.00   1.00    1.00    --   41.47-125.00 120.00   97
  3  ω      2.00  99.00   1.00    1.00    --   41.47-125.00 -30.00   97
  4  ω     15.00 118.00   1.00    1.00    --   41.47  37.00-150.00  103
  5  ω     15.00 118.00   1.00    1.00    --   41.47  37.00 -60.00  103
  6  ω     17.00 158.00   1.00    1.00    --  106.28   0.00 -90.00  141
  7  ω     22.00 109.00   1.00    1.00    --  106.28 -94.00-180.00   87
  8  ω     32.00 134.00   1.00    1.00    --  106.28 -45.00-180.00  102
  9  ω     76.00 158.00   1.00    1.00    --  106.28  61.00 -90.00   82
 10  ω     28.00 112.00   1.00    1.00    --  106.28-111.00 -60.00   84
 11  ω     22.00 109.00   1.00    1.00    --  106.28 -94.00   0.00   87
 12  ω     28.00 112.00   1.00    1.00    --  106.28-111.00 120.00   84
 13  ω     32.00 135.00   1.00    1.00    --  106.28 -50.00 -68.00  103
 14  ω     79.00 158.00   1.00    1.00    --  106.28 111.00 -30.00   79
 15  ω     32.00 134.00   1.00    1.00    --  106.28 -45.00  60.00  102
 16  ω   -115.00 -12.00   1.00    1.00    --  -41.47 -57.00  30.00  103
 17  ω   -120.00  -8.00   1.00    1.00    --  -41.47 -77.00 120.00  112
 18  ω    -71.00  32.00   1.00    1.00    --  -41.47  57.00-150.00  103
 19  ω      8.00 120.00   1.00    1.00    --   41.47  77.00 -30.00  112
 20  ω     76.00 158.00   1.00    1.00    --  106.28  30.00  90.00   82
;
_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'







_exptl_crystal_recrystallization_method Sublimation
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Hygroscopic,Heat-sensitive,Oxygen-sensitive
