#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/27/7012772.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7012772
loop_
_publ_author_name
'Bezombes, Jean-Philippe'
'Gehrhus, Barbara'
'Hitchcock, Peter B.'
'Lappert, Michael F.'
'Merle, Philippe G.'
_publ_section_title
;
 A comparative study of the behaviour of N-trimethylsilyl and
 N-neopentyl-anilines and 1,2-diaminobenzenes towards trimethylalane;
 X-ray structures of nine Al--N compounds
;
_journal_issue                   9
_journal_name_full               'Dalton Transactions'
_journal_page_first              1821
_journal_paper_doi               10.1039/b300957m
_journal_year                    2003
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C22 H46 Al2 N2'
_chemical_formula_structural     'C22 H46 AL2 N2'
_chemical_formula_sum            'C22 H46 Al2 N2'
_chemical_formula_weight         392.57
_chemical_name_common            '[C6H4{NH(CH2tBu)(AlMe3)}2]'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location
ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta5
_audit_creation_date             2000-03-31T15:06:57-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                98.740(2)
_cell_angle_beta                 99.440(2)
_cell_angle_gamma                97.884(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8445(2)
_cell_length_b                   10.7407(4)
_cell_length_c                   13.0190(4)
_cell_measurement_reflns_used    8407
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     1323.50(7)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0434
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13539
_diffrn_reflns_theta_full        27.85
_diffrn_reflns_theta_max         27.85
_diffrn_reflns_theta_min         3.91
_exptl_absorpt_coefficient_mu    0.118
_exptl_absorpt_correction_T_max  0.9768
_exptl_absorpt_correction_T_min  0.9712
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.985
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         6225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0543P)²+0.6088P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1308
_reflns_number_gt                5143
_reflns_number_total             6225
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b300957m.txt
_cod_data_source_block           lappert-10
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7012772
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.19159(5) 0.23568(4) 0.85936(4) 0.02793(13) Uani 1 1 d . . .
Al2 Al 0.39570(5) -0.33717(4) 0.67484(4) 0.02757(13) Uani 1 1 d . . .
N1 N 0.35274(12) 0.18878(11) 0.78267(9) 0.0236(3) Uani 1 1 d . . .
H1 H 0.3782 0.2576 0.7504 0.028 Uiso 1 1 calc R . .
N2 N 0.20407(13) -0.27385(11) 0.65936(9) 0.0245(3) Uani 1 1 d . . .
H2 H 0.149 -0.3245 0.5985 0.029 Uiso 1 1 calc R . .
C1 C 0.30140(14) 0.08005(13) 0.69741(11) 0.0230(3) Uani 1 1 d . . .
C2 C 0.27696(14) -0.04234(14) 0.71977(11) 0.0236(3) Uani 1 1 d . . .
H2' H 0.2993 -0.0564 0.7904 0.028 Uiso 1 1 calc R . .
C3 C 0.21963(15) -0.14406(13) 0.63816(11) 0.0238(3) Uani 1 1 d . . .
C4 C 0.18583(18) -0.12446(15) 0.53463(12) 0.0317(3) Uani 1 1 d . . .
H4 H 0.1458 -0.1943 0.479 0.038 Uiso 1 1 calc R . .
C5 C 0.2113(2) -0.00158(16) 0.51351(12) 0.0358(4) Uani 1 1 d . . .
H5 H 0.189 0.0124 0.4428 0.043 Uiso 1 1 calc R . .
C6 C 0.26892(17) 0.10107(15) 0.59400(12) 0.0306(3) Uani 1 1 d . . .
H6 H 0.2861 0.1849 0.5788 0.037 Uiso 1 1 calc R . .
C7 C 0.47963(15) 0.18062(15) 0.86144(12) 0.0272(3) Uani 1 1 d . . .
H7A H 0.4657 0.0959 0.883 0.033 Uiso 1 1 calc R . .
H7B H 0.4852 0.2458 0.9252 0.033 Uiso 1 1 calc R . .
C8 C 0.62080(16) 0.19892(15) 0.82521(13) 0.0298(3) Uani 1 1 d . . .
C9 C 0.64426(19) 0.32405(19) 0.78471(17) 0.0455(4) Uani 1 1 d . . .
H9A H 0.6362 0.3946 0.8395 0.068 Uiso 1 1 calc R . .
H9B H 0.574 0.3209 0.7212 0.068 Uiso 1 1 calc R . .
H9C H 0.7377 0.3374 0.7673 0.068 Uiso 1 1 calc R . .
C10 C 0.73191(19) 0.2051(2) 0.92426(16) 0.0473(5) Uani 1 1 d . . .
H10A H 0.7176 0.1247 0.951 0.071 Uiso 1 1 calc R . .
H10B H 0.7241 0.276 0.9788 0.071 Uiso 1 1 calc R . .
H10C H 0.825 0.2185 0.9062 0.071 Uiso 1 1 calc R . .
C11 C 0.6336(2) 0.0880(2) 0.74080(18) 0.0536(6) Uani 1 1 d . . .
H11A H 0.6182 0.0078 0.7676 0.08 Uiso 1 1 calc R . .
H11B H 0.7273 0.1009 0.7236 0.08 Uiso 1 1 calc R . .
H11C H 0.5637 0.0842 0.677 0.08 Uiso 1 1 calc R . .
C12 C 0.1641(2) 0.10170(18) 0.94556(15) 0.0430(4) Uani 1 1 d . . .
H12A H 0.2449 0.113 1.0032 0.064 Uiso 1 1 calc R . .
H12B H 0.1543 0.0175 0.9011 0.064 Uiso 1 1 calc R . .
H12C H 0.0795 0.1079 0.9752 0.064 Uiso 1 1 calc R . .
C13 C 0.04011(18) 0.2306(2) 0.73812(15) 0.0428(4) Uani 1 1 d . . .
H13A H 0.0643 0.3009 0.7009 0.064 Uiso 1 1 calc R . .
H13B H -0.0469 0.2395 0.7637 0.064 Uiso 1 1 calc R . .
H13C H 0.0278 0.149 0.6896 0.064 Uiso 1 1 calc R . .
C14 C 0.2710(2) 0.40910(16) 0.93898(14) 0.0402(4) Uani 1 1 d . . .
H14A H 0.2805 0.4683 0.8893 0.06 Uiso 1 1 calc R . .
H14B H 0.363 0.408 0.9809 0.06 Uiso 1 1 calc R . .
H14C H 0.2089 0.437 0.9863 0.06 Uiso 1 1 calc R . .
C15 C 0.13159(16) -0.30030(15) 0.74812(12) 0.0278(3) Uani 1 1 d . . .
H15A H 0.1626 -0.2267 0.8071 0.033 Uiso 1 1 calc R . .
H15B H 0.1631 -0.3758 0.7736 0.033 Uiso 1 1 calc R . .
C16 C -0.02886(17) -0.32483(16) 0.72315(15) 0.0358(4) Uani 1 1 d . . .
C17 C -0.0870(2) -0.2066(2) 0.6965(2) 0.0685(7) Uani 1 1 d . . .
H17A H -0.051 -0.1346 0.755 0.103 Uiso 1 1 calc R . .
H17B H -0.1892 -0.2237 0.6856 0.103 Uiso 1 1 calc R . .
H17C H -0.0582 -0.1854 0.6318 0.103 Uiso 1 1 calc R . .
C18 C -0.0751(2) -0.3582(2) 0.82371(18) 0.0539(5) Uani 1 1 d . . .
H18A H -0.0414 -0.2856 0.882 0.081 Uiso 1 1 calc R . .
H18B H -0.0362 -0.433 0.8419 0.081 Uiso 1 1 calc R . .
H18C H -0.1773 -0.3774 0.8116 0.081 Uiso 1 1 calc R . .
C19 C -0.0826(2) -0.4386(2) 0.63368(18) 0.0593(6) Uani 1 1 d . . .
H19A H -0.0443 -0.5134 0.6526 0.089 Uiso 1 1 calc R . .
H19B H -0.0532 -0.4188 0.5688 0.089 Uiso 1 1 calc R . .
H19C H -0.1848 -0.4569 0.6221 0.089 Uiso 1 1 calc R . .
C20 C 0.3309(2) -0.52388(16) 0.65047(15) 0.0404(4) Uani 1 1 d . . .
H20A H 0.2917 -0.5465 0.711 0.061 Uiso 1 1 calc R . .
H20B H 0.4099 -0.5686 0.6423 0.061 Uiso 1 1 calc R . .
H20C H 0.2591 -0.549 0.5861 0.061 Uiso 1 1 calc R . .
C21 C 0.4890(2) -0.26346(19) 0.82119(14) 0.0427(4) Uani 1 1 d . . .
H21A H 0.4379 -0.3015 0.8704 0.064 Uiso 1 1 calc R . .
H21B H 0.4909 -0.1709 0.8334 0.064 Uiso 1 1 calc R . .
H21C H 0.5848 -0.2813 0.8327 0.064 Uiso 1 1 calc R . .
C22 C 0.4775(2) -0.2771(2) 0.55973(16) 0.0462(5) Uani 1 1 d . . .
H22A H 0.4211 -0.3211 0.4915 0.069 Uiso 1 1 calc R . .
H22B H 0.573 -0.2954 0.5648 0.069 Uiso 1 1 calc R . .
H22C H 0.4793 -0.1849 0.5655 0.069 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C12 Al1 C13 116.19(9) . . ?
C12 Al1 C14 115.78(8) . . ?
C13 Al1 C14 114.30(9) . . ?
C12 Al1 N1 104.05(7) . . ?
C13 Al1 N1 101.43(7) . . ?
C14 Al1 N1 102.10(7) . . ?
C22 Al2 C21 117.87(9) . . ?
C22 Al2 C20 114.20(9) . . ?
C21 Al2 C20 114.11(8) . . ?
C22 Al2 N2 103.44(7) . . ?
C21 Al2 N2 104.32(7) . . ?
C20 Al2 N2 99.84(7) . . ?
C1 N1 C7 117.07(11) . . ?
C1 N1 Al1 110.42(9) . . ?
C7 N1 Al1 110.75(9) . . ?
C3 N2 C15 117.34(11) . . ?
C3 N2 Al2 110.34(9) . . ?
C15 N2 Al2 111.05(9) . . ?
C2 C1 C6 120.47(13) . . ?
C2 C1 N1 120.22(12) . . ?
C6 C1 N1 119.19(13) . . ?
C3 C2 C1 119.47(13) . . ?
C2 C3 C4 120.71(13) . . ?
C2 C3 N2 119.90(12) . . ?
C4 C3 N2 119.24(13) . . ?
C5 C4 C3 119.12(14) . . ?
C6 C5 C4 120.94(14) . . ?
C5 C6 C1 119.28(14) . . ?
N1 C7 C8 116.90(12) . . ?
C9 C8 C11 110.07(16) . . ?
C9 C8 C10 108.88(14) . . ?
C11 C8 C10 109.08(16) . . ?
C9 C8 C7 110.61(13) . . ?
C11 C8 C7 112.32(13) . . ?
C10 C8 C7 105.74(13) . . ?
N2 C15 C16 116.67(13) . . ?
C19 C16 C17 110.9(2) . . ?
C19 C16 C18 108.57(16) . . ?
C17 C16 C18 109.31(18) . . ?
C19 C16 C15 110.39(15) . . ?
C17 C16 C15 111.64(15) . . ?
C18 C16 C15 105.86(15) . . ?
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
Al1 C12 1.9714(19) . ?
Al1 C13 1.9744(19) . ?
Al1 C14 1.9756(18) . ?
Al1 N1 2.0864(13) . ?
Al2 C22 1.9641(19) . ?
Al2 C21 1.9670(18) . ?
Al2 C20 1.9794(18) . ?
Al2 N2 2.0811(13) . ?
N1 C1 1.4532(17) . ?
N1 C7 1.5022(18) . ?
N2 C3 1.4544(18) . ?
N2 C15 1.4967(19) . ?
C1 C2 1.387(2) . ?
C1 C6 1.392(2) . ?
C2 C3 1.386(2) . ?
C3 C4 1.389(2) . ?
C4 C5 1.387(2) . ?
C5 C6 1.385(2) . ?
C7 C8 1.537(2) . ?
C8 C9 1.519(2) . ?
C8 C11 1.527(2) . ?
C8 C10 1.535(2) . ?
C15 C16 1.537(2) . ?
C16 C19 1.522(3) . ?
C16 C17 1.526(3) . ?
C16 C18 1.531(3) . ?
