#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/27/7012770.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_7012770
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         'C18 H33 Al1 N2'
_chemical_formula_structural     'C18 H33 AL N2'
_chemical_formula_sum            'C18 H33 Al N2'
_chemical_formula_weight         304.44
_chemical_name_common            '[Me2Al{C6H4(NHCH2tBu)(NCH2tBu)}]'
_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.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1
_audit_creation_date             2001-04-13T10:58:27-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.773(3)
_cell_angle_beta                 96.342(3)
_cell_angle_gamma                102.991(3)
_cell_formula_units_Z            2
_cell_length_a                   9.6526(5)
_cell_length_b                   9.7157(5)
_cell_length_c                   10.6710(6)
_cell_measurement_reflns_used    5216
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     968.40(9)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0512
_diffrn_reflns_av_unetI/netI     0.0533
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7681
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         3.73
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_T_max  0.9602
_exptl_absorpt_correction_T_min  0.9602
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.044
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         4542
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0650P)²+0.3827P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1307
_reflns_number_gt                3879
_reflns_number_total             4542
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b300957m.txt
_cod_data_source_block           lappert-7
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7012770
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
Al Al 0.34665(4) 0.79462(4) 0.18066(4) 0.02368(13) Uani 1 1 d . . .
N1 N 0.50478(12) 0.82760(13) 0.32643(10) 0.0230(2) Uani 1 1 d . . .
H1 H 0.5434(18) 0.9157(19) 0.3429(16) 0.027(4) Uiso 1 1 d . . .
N2 N 0.25620(12) 0.64484(12) 0.27178(10) 0.0238(2) Uani 1 1 d . . .
C1 C 0.42477(15) 0.77480(14) 0.43283(12) 0.0247(3) Uani 1 1 d . . .
C2 C 0.29517(15) 0.67412(14) 0.39919(12) 0.0241(3) Uani 1 1 d . . .
C3 C 0.22108(17) 0.61647(16) 0.50036(14) 0.0327(3) Uani 1 1 d . . .
H3 H 0.1328 0.5488 0.4834 0.039 Uiso 1 1 calc R . .
C4 C 0.27612(19) 0.65776(18) 0.62432(14) 0.0381(4) Uani 1 1 d . . .
H4 H 0.2246 0.6168 0.6906 0.046 Uiso 1 1 calc R . .
C5 C 0.40371(19) 0.75672(18) 0.65436(14) 0.0372(4) Uani 1 1 d . . .
H5 H 0.4393 0.7839 0.7398 0.045 Uiso 1 1 calc R . .
C6 C 0.47908(17) 0.81581(16) 0.55617(13) 0.0304(3) Uani 1 1 d . . .
H6 H 0.5671 0.8837 0.5742 0.037 Uiso 1 1 calc R . .
C7 C 0.62458(14) 0.75241(15) 0.31372(13) 0.0269(3) Uani 1 1 d . . .
H7B H 0.593 0.6794 0.2446 0.032 Uiso 1 1 calc R . .
H7A H 0.642 0.7035 0.3927 0.032 Uiso 1 1 calc R . .
C8 C 0.76552(15) 0.84962(16) 0.28696(14) 0.0309(3) Uani 1 1 d . . .
C9 C 0.74748(19) 0.9254(2) 0.16354(16) 0.0422(4) Uani 1 1 d . . .
H9C H 0.7149 0.8553 0.0934 0.063 Uiso 1 1 calc R . .
H9B H 0.8394 0.9867 0.1492 0.063 Uiso 1 1 calc R . .
H9A H 0.6766 0.9827 0.1689 0.063 Uiso 1 1 calc R . .
C10 C 0.82485(18) 0.9586(2) 0.39583(17) 0.0443(4) Uani 1 1 d . . .
H10C H 0.7553 1.0161 0.4069 0.066 Uiso 1 1 calc R . .
H10B H 0.9148 1.0198 0.3766 0.066 Uiso 1 1 calc R . .
H10A H 0.8423 0.9097 0.4737 0.066 Uiso 1 1 calc R . .
C11 C 0.87000(19) 0.7527(2) 0.2758(2) 0.0503(5) Uani 1 1 d . . .
H11C H 0.8821 0.7047 0.3551 0.075 Uiso 1 1 calc R . .
H11B H 0.9629 0.8095 0.2583 0.075 Uiso 1 1 calc R . .
H11A H 0.8316 0.6822 0.2068 0.075 Uiso 1 1 calc R . .
C12 C 0.13109(15) 0.53482(15) 0.22546(13) 0.0265(3) Uani 1 1 d . . .
H12B H 0.0872 0.5647 0.1451 0.032 Uiso 1 1 calc R . .
H12A H 0.0603 0.5273 0.2869 0.032 Uiso 1 1 calc R . .
C13 C 0.15935(16) 0.38643(15) 0.20276(14) 0.0289(3) Uani 1 1 d . . .
C14 C 0.0226(2) 0.2916(2) 0.1359(2) 0.0518(5) Uani 1 1 d . . .
H14C H 0.0387 0.1972 0.1198 0.078 Uiso 1 1 calc R . .
H14B H -0.0039 0.3321 0.0556 0.078 Uiso 1 1 calc R . .
H14A H -0.0548 0.2846 0.1893 0.078 Uiso 1 1 calc R . .
C15 C 0.1996(2) 0.32251(19) 0.32726(17) 0.0491(5) Uani 1 1 d . . .
H15C H 0.2138 0.2274 0.3109 0.074 Uiso 1 1 calc R . .
H15B H 0.1226 0.3169 0.381 0.074 Uiso 1 1 calc R . .
H15A H 0.2884 0.382 0.37 0.074 Uiso 1 1 calc R . .
C16 C 0.2796(2) 0.39461(19) 0.12018(19) 0.0480(4) Uani 1 1 d . . .
H16C H 0.3681 0.4542 0.1632 0.072 Uiso 1 1 calc R . .
H16B H 0.2543 0.4354 0.0397 0.072 Uiso 1 1 calc R . .
H16A H 0.2938 0.2994 0.1044 0.072 Uiso 1 1 calc R . .
C17 C 0.40189(18) 0.74932(19) 0.01650(14) 0.0368(4) Uani 1 1 d . . .
H17C H 0.3171 0.7288 -0.0463 0.055 Uiso 1 1 calc R . .
H17B H 0.444 0.6665 0.0231 0.055 Uiso 1 1 calc R . .
H17A H 0.4722 0.83 -0.0095 0.055 Uiso 1 1 calc R . .
C18 C 0.25982(17) 0.95885(16) 0.18501(16) 0.0352(3) Uani 1 1 d . . .
H18C H 0.3277 1.043 0.1618 0.053 Uiso 1 1 calc R . .
H18B H 0.2358 0.9736 0.2703 0.053 Uiso 1 1 calc R . .
H18A H 0.1726 0.9418 0.1251 0.053 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
N2 Al C17 117.64(7) . . ?
N2 Al C18 113.00(6) . . ?
C17 Al C18 115.09(7) . . ?
N2 Al N1 85.62(5) . . ?
C17 Al N1 115.70(6) . . ?
C18 Al N1 105.77(6) . . ?
C1 N1 C7 111.26(10) . . ?
C1 N1 Al 101.62(8) . . ?
C7 N1 Al 115.63(9) . . ?
C2 N2 C12 121.20(11) . . ?
C2 N2 Al 109.83(9) . . ?
C12 N2 Al 126.39(9) . . ?
C6 C1 C2 123.27(13) . . ?
C6 C1 N1 121.48(13) . . ?
C2 C1 N1 115.13(11) . . ?
N2 C2 C1 115.98(12) . . ?
N2 C2 C3 128.08(13) . . ?
C1 C2 C3 115.94(13) . . ?
C4 C3 C2 120.64(14) . . ?
C5 C4 C3 122.07(14) . . ?
C4 C5 C6 118.53(14) . . ?
C1 C6 C5 119.54(15) . . ?
N1 C7 C8 114.32(11) . . ?
C9 C8 C7 111.52(12) . . ?
C9 C8 C10 109.72(14) . . ?
C7 C8 C10 110.87(13) . . ?
C9 C8 C11 109.51(14) . . ?
C7 C8 C11 105.73(13) . . ?
C10 C8 C11 109.40(14) . . ?
N2 C12 C13 115.66(11) . . ?
C15 C13 C16 109.01(15) . . ?
C15 C13 C14 109.04(15) . . ?
C16 C13 C14 109.10(15) . . ?
C15 C13 C12 110.83(12) . . ?
C16 C13 C12 110.58(12) . . ?
C14 C13 C12 108.25(13) . . ?
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
Al N2 1.8655(12) . ?
Al C17 1.9590(15) . ?
Al C18 1.9643(15) . ?
Al N1 2.0234(12) . ?
N1 C1 1.4765(16) . ?
N1 C7 1.5169(17) . ?
N2 C2 1.3782(17) . ?
N2 C12 1.4555(18) . ?
C1 C6 1.3804(19) . ?
C1 C2 1.411(2) . ?
C2 C3 1.4134(18) . ?
C3 C4 1.388(2) . ?
C4 C5 1.384(3) . ?
C5 C6 1.398(2) . ?
C7 C8 1.5296(19) . ?
C8 C9 1.529(2) . ?
C8 C10 1.532(2) . ?
C8 C11 1.539(2) . ?
C12 C13 1.5471(19) . ?
C13 C15 1.523(2) . ?
C13 C16 1.522(2) . ?
C13 C14 1.526(2) . ?
