#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/27/7012771.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_7012771
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         'C32 H52 Al2 Cl2 N4'
_chemical_formula_structural     'C32 H52 Al2 Cl2 N4'
_chemical_formula_sum            'C32 H52 Al2 Cl2 N4'
_chemical_formula_weight         617.64
_chemical_name_common            '[{(C6H4(NCH2tBu)2)AlCl}2]''
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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             2000-03-22T16:07:16-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 106.504(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0101(7)
_cell_length_b                   14.8750(9)
_cell_length_c                   20.3163(10)
_cell_measurement_reflns_used    22330
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.986
_cell_measurement_theta_min      4.529
_cell_measurement_wavelength     0.71073
_cell_volume                     3480.0(3)
_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 0.945
_diffrn_measured_fraction_theta_max 0.945
_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  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0514
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9892
_diffrn_reflns_theta_full        22.98
_diffrn_reflns_theta_max         22.98
_diffrn_reflns_theta_min         5.17
_exptl_absorpt_coefficient_mu    0.264
_exptl_absorpt_correction_T_max  0.9251
_exptl_absorpt_correction_T_min  0.9251
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.04
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         4566
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0447
_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)+(0.0347P)²+2.1748P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1138
_reflns_number_gt                3780
_reflns_number_total             4566
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b300957m.txt
_cod_data_source_block           lappert-9
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7012771
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.34556(6) 0.33458(5) 0.06914(4) 0.0304(2) Uani 1 1 d . . .
Al2 Al 0.34065(6) 0.23887(5) 0.18241(4) 0.0322(2) Uani 1 1 d . . .
Cl1 Cl 0.30960(6) 0.46988(5) 0.04017(4) 0.0484(2) Uani 1 1 d . . .
Cl2 Cl 0.23616(6) 0.24246(5) 0.24982(4) 0.0469(2) Uani 1 1 d . . .
N1 N 0.38795(18) 0.24967(14) 0.01697(11) 0.0326(5) Uani 1 1 d . . .
N2 N 0.23455(17) 0.25343(14) 0.08907(11) 0.0323(5) Uani 1 1 d . . .
N3 N 0.43545(17) 0.33616(14) 0.16715(11) 0.0308(5) Uani 1 1 d . . .
N4 N 0.45821(18) 0.15977(14) 0.18988(11) 0.0343(5) Uani 1 1 d . . .
C1 C 0.3316(2) 0.16799(18) 0.01921(13) 0.0356(6) Uani 1 1 d . . .
C2 C 0.2453(2) 0.16884(18) 0.05427(13) 0.0345(6) Uani 1 1 d . . .
C3 C 0.1851(3) 0.09180(19) 0.06105(15) 0.0445(7) Uani 1 1 d . . .
H3 H 0.1287 0.0938 0.0857 0.053 Uiso 1 1 calc R . .
C4 C 0.2066(3) 0.0118(2) 0.03207(17) 0.0532(8) Uani 1 1 d . . .
H4 H 0.1639 -0.0408 0.0356 0.064 Uiso 1 1 calc R . .
C5 C 0.2906(3) 0.0094(2) -0.00184(17) 0.0563(9) Uani 1 1 d . . .
H5 H 0.3062 -0.0456 -0.0213 0.068 Uiso 1 1 calc R . .
C6 C 0.3530(3) 0.0856(2) -0.00832(15) 0.0457(7) Uani 1 1 d . . .
H6 H 0.411 0.0819 -0.0317 0.055 Uiso 1 1 calc R . .
C7 C 0.4840(2) 0.2537(2) -0.01455(14) 0.0407(7) Uani 1 1 d . . .
H7A H 0.5207 0.1936 -0.0103 0.049 Uiso 1 1 calc R . .
H7B H 0.5429 0.2962 0.0125 0.049 Uiso 1 1 calc R . .
C8 C 0.4536(3) 0.2821(2) -0.09016(15) 0.0483(8) Uani 1 1 d . . .
C9 C 0.5659(3) 0.2762(3) -0.11156(19) 0.0697(11) Uani 1 1 d . . .
H9A H 0.5947 0.2142 -0.1061 0.105 Uiso 1 1 calc R . .
H9B H 0.6244 0.3162 -0.0826 0.105 Uiso 1 1 calc R . .
H9C H 0.5503 0.2943 -0.1597 0.105 Uiso 1 1 calc R . .
C10 C 0.4082(3) 0.3786(2) -0.09878(18) 0.0608(9) Uani 1 1 d . . .
H10A H 0.3362 0.3822 -0.0852 0.091 Uiso 1 1 calc R . .
H10B H 0.3927 0.3968 -0.1469 0.091 Uiso 1 1 calc R . .
H10C H 0.4664 0.4188 -0.0697 0.091 Uiso 1 1 calc R . .
C11 C 0.3605(3) 0.2206(3) -0.13651(16) 0.0619(10) Uani 1 1 d . . .
H11A H 0.3882 0.1584 -0.1318 0.093 Uiso 1 1 calc R . .
H11B H 0.3453 0.2397 -0.1844 0.093 Uiso 1 1 calc R . .
H11C H 0.2887 0.2248 -0.1228 0.093 Uiso 1 1 calc R . .
C12 C 0.1135(2) 0.2848(2) 0.08529(14) 0.0375(7) Uani 1 1 d . . .
H12A H 0.1206 0.3436 0.109 0.045 Uiso 1 1 calc R . .
H12B H 0.0808 0.242 0.1122 0.045 Uiso 1 1 calc R . .
C13 C 0.0232(2) 0.2958(2) 0.01406(14) 0.0395(7) Uani 1 1 d . . .
C14 C 0.0776(2) 0.3207(2) -0.04262(15) 0.0481(8) Uani 1 1 d . . .
H14A H 0.1246 0.3752 -0.0295 0.072 Uiso 1 1 calc R . .
H14B H 0.0162 0.3317 -0.0853 0.072 Uiso 1 1 calc R . .
H14C H 0.1271 0.2713 -0.0495 0.072 Uiso 1 1 calc R . .
C15 C -0.0575(3) 0.3720(2) 0.02199(18) 0.0589(9) Uani 1 1 d . . .
H15A H -0.0123 0.4273 0.0353 0.088 Uiso 1 1 calc R . .
H15B H -0.0948 0.356 0.0575 0.088 Uiso 1 1 calc R . .
H15C H -0.1171 0.3815 -0.0217 0.088 Uiso 1 1 calc R . .
C16 C -0.0505(3) 0.2108(2) -0.00706(18) 0.0568(9) Uani 1 1 d . . .
H16A H -0.0856 0.1943 0.0293 0.085 Uiso 1 1 calc R . .
H16B H -0.0012 0.1614 -0.0143 0.085 Uiso 1 1 calc R . .
H16C H -0.1119 0.2222 -0.0497 0.085 Uiso 1 1 calc R . .
C17 C 0.5471(2) 0.29596(18) 0.16698(13) 0.0327(6) Uani 1 1 d . . .
C18 C 0.5547(2) 0.20203(18) 0.17727(13) 0.0345(6) Uani 1 1 d . . .
C19 C 0.6557(2) 0.1593(2) 0.17168(15) 0.0431(7) Uani 1 1 d . . .
H19 H 0.6643 0.0963 0.1786 0.052 Uiso 1 1 calc R . .
C20 C 0.7427(3) 0.2082(2) 0.15624(16) 0.0490(8) Uani 1 1 d . . .
H20 H 0.8105 0.1781 0.1527 0.059 Uiso 1 1 calc R . .
C21 C 0.7334(2) 0.2997(2) 0.14591(15) 0.0471(8) Uani 1 1 d . . .
H21 H 0.7946 0.3324 0.1359 0.057 Uiso 1 1 calc R . .
C22 C 0.6339(2) 0.3438(2) 0.15026(14) 0.0391(7) Uani 1 1 d . . .
H22 H 0.6254 0.4066 0.1418 0.047 Uiso 1 1 calc R . .
C23 C 0.4410(2) 0.42529(18) 0.20327(13) 0.0360(6) Uani 1 1 d . . .
H23A H 0.3604 0.443 0.2007 0.043 Uiso 1 1 calc R . .
H23B H 0.4709 0.4703 0.1766 0.043 Uiso 1 1 calc R . .
C24 C 0.5144(2) 0.4336(2) 0.27952(14) 0.0414(7) Uani 1 1 d . . .
C25 C 0.6409(3) 0.4583(2) 0.28644(16) 0.0546(8) Uani 1 1 d . . .
H25A H 0.6779 0.4095 0.268 0.082 Uiso 1 1 calc R . .
H25B H 0.6823 0.4675 0.335 0.082 Uiso 1 1 calc R . .
H25C H 0.6434 0.5137 0.2608 0.082 Uiso 1 1 calc R . .
C26 C 0.5162(4) 0.3487(3) 0.32083(18) 0.0752(12) Uani 1 1 d . . .
H26A H 0.5504 0.2996 0.3008 0.113 Uiso 1 1 calc R . .
H26B H 0.4367 0.3326 0.3201 0.113 Uiso 1 1 calc R . .
H26C H 0.5628 0.3587 0.3684 0.113 Uiso 1 1 calc R . .
C27 C 0.4622(3) 0.5114(3) 0.3088(2) 0.0881(15) Uani 1 1 d . . .
H27A H 0.4618 0.5653 0.281 0.132 Uiso 1 1 calc R . .
H27B H 0.5088 0.5228 0.3561 0.132 Uiso 1 1 calc R . .
H27C H 0.3825 0.4965 0.3082 0.132 Uiso 1 1 calc R . .
C28 C 0.4538(2) 0.06119(18) 0.19237(14) 0.0394(7) Uani 1 1 d . . .
H28A H 0.5052 0.037 0.1662 0.047 Uiso 1 1 calc R . .
H28B H 0.3736 0.042 0.1682 0.047 Uiso 1 1 calc R . .
C29 C 0.4886(2) 0.01701(19) 0.26405(14) 0.0392(7) Uani 1 1 d . . .
C30 C 0.6096(2) 0.0455(2) 0.30701(16) 0.0470(7) Uani 1 1 d . . .
H30A H 0.6111 0.1106 0.3143 0.07 Uiso 1 1 calc R . .
H30B H 0.6667 0.0294 0.2828 0.07 Uiso 1 1 calc R . .
H30C H 0.6288 0.0146 0.3515 0.07 Uiso 1 1 calc R . .
C31 C 0.4852(3) -0.0847(2) 0.25283(18) 0.0586(9) Uani 1 1 d . . .
H31A H 0.5419 -0.1014 0.2285 0.088 Uiso 1 1 calc R . .
H31B H 0.4073 -0.1026 0.2255 0.088 Uiso 1 1 calc R . .
H31C H 0.5044 -0.1154 0.2973 0.088 Uiso 1 1 calc R . .
C32 C 0.3996(3) 0.0412(2) 0.30248(16) 0.0502(8) Uani 1 1 d . . .
H32A H 0.4007 0.1063 0.3101 0.075 Uiso 1 1 calc R . .
H32B H 0.4194 0.01 0.3468 0.075 Uiso 1 1 calc R . .
H32C H 0.3219 0.0228 0.2751 0.075 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'
Cl Cl 0.1484 0.1585 '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
N1 Al1 N2 90.71(10) . . ?
N1 Al1 N3 115.69(10) . . ?
N2 Al1 N3 90.47(9) . . ?
N1 Al1 Cl1 124.87(8) . . ?
N2 Al1 Cl1 123.95(8) . . ?
N3 Al1 Cl1 106.25(7) . . ?
N1 Al1 Al2 101.96(8) . . ?
N2 Al1 Al2 46.47(7) . . ?
N3 Al1 Al2 44.87(6) . . ?
Cl1 Al1 Al2 133.16(4) . . ?
N4 Al2 N3 91.10(9) . . ?
N4 Al2 N2 115.28(10) . . ?
N3 Al2 N2 90.74(9) . . ?
N4 Al2 Cl2 123.83(8) . . ?
N3 Al2 Cl2 125.20(7) . . ?
N2 Al2 Cl2 106.32(7) . . ?
N4 Al2 Al1 101.95(7) . . ?
N3 Al2 Al1 46.59(7) . . ?
N2 Al2 Al1 45.01(6) . . ?
Cl2 Al2 Al1 134.21(4) . . ?
C1 N1 C7 119.8(2) . . ?
C1 N1 Al1 111.58(17) . . ?
C7 N1 Al1 127.68(18) . . ?
C2 N2 C12 117.2(2) . . ?
C2 N2 Al1 105.98(15) . . ?
C12 N2 Al1 120.69(17) . . ?
C2 N2 Al2 104.35(15) . . ?
C12 N2 Al2 115.66(16) . . ?
Al1 N2 Al2 88.52(9) . . ?
C17 N3 C23 116.41(19) . . ?
C17 N3 Al2 106.09(16) . . ?
C23 N3 Al2 122.03(16) . . ?
C17 N3 Al1 103.32(15) . . ?
C23 N3 Al1 115.89(16) . . ?
Al2 N3 Al1 88.53(9) . . ?
C18 N4 C28 119.5(2) . . ?
C18 N4 Al2 110.98(17) . . ?
C28 N4 Al2 128.07(18) . . ?
N1 C1 C6 127.0(3) . . ?
N1 C1 C2 116.1(2) . . ?
C6 C1 C2 116.9(3) . . ?
C3 C2 C1 121.4(3) . . ?
C3 C2 N2 122.9(2) . . ?
C1 C2 N2 115.3(2) . . ?
C2 C3 C4 120.3(3) . . ?
C5 C4 C3 119.2(3) . . ?
C4 C5 C6 121.4(3) . . ?
C5 C6 C1 120.8(3) . . ?
N1 C7 C8 117.0(2) . . ?
C10 C8 C9 109.6(3) . . ?
C10 C8 C7 110.4(3) . . ?
C9 C8 C7 106.9(3) . . ?
C10 C8 C11 108.3(3) . . ?
C9 C8 C11 109.7(3) . . ?
C7 C8 C11 112.0(3) . . ?
N2 C12 C13 119.3(2) . . ?
C14 C13 C15 108.7(3) . . ?
C14 C13 C16 109.1(3) . . ?
C15 C13 C16 107.9(2) . . ?
C14 C13 C12 113.2(2) . . ?
C15 C13 C12 106.0(2) . . ?
C16 C13 C12 111.7(2) . . ?
C22 C17 C18 121.7(2) . . ?
C22 C17 N3 122.9(2) . . ?
C18 C17 N3 115.0(2) . . ?
C19 C18 N4 126.1(3) . . ?
C19 C18 C17 117.2(2) . . ?
N4 C18 C17 116.6(2) . . ?
C20 C19 C18 120.5(3) . . ?
C21 C20 C19 121.4(3) . . ?
C20 C21 C22 119.4(3) . . ?
C17 C22 C21 119.7(3) . . ?
N3 C23 C24 119.3(2) . . ?
C26 C24 C27 111.3(3) . . ?
C26 C24 C25 107.0(3) . . ?
C27 C24 C25 106.9(3) . . ?
C26 C24 C23 113.7(2) . . ?
C27 C24 C23 105.7(2) . . ?
C25 C24 C23 112.2(2) . . ?
N4 C28 C29 117.1(2) . . ?
C30 C29 C31 109.9(2) . . ?
C30 C29 C32 109.4(2) . . ?
C31 C29 C32 108.4(3) . . ?
C30 C29 C28 112.3(2) . . ?
C31 C29 C28 107.0(2) . . ?
C32 C29 C28 109.8(2) . . ?
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 N1 1.812(2) . ?
Al1 N2 1.925(2) . ?
Al1 N3 1.977(2) . ?
Al1 Cl1 2.1069(10) . ?
Al1 Al2 2.7208(11) . ?
Al2 N4 1.811(2) . ?
Al2 N3 1.920(2) . ?
Al2 N2 1.973(2) . ?
Al2 Cl2 2.1047(10) . ?
N1 C1 1.398(3) . ?
N1 C7 1.471(3) . ?
N2 C2 1.467(3) . ?
N2 C12 1.507(3) . ?
N3 C17 1.470(3) . ?
N3 C23 1.508(3) . ?
N4 C18 1.405(3) . ?
N4 C28 1.469(3) . ?
C1 C6 1.401(4) . ?
C1 C2 1.415(4) . ?
C2 C3 1.383(4) . ?
C3 C4 1.384(4) . ?
C4 C5 1.374(5) . ?
C5 C6 1.385(4) . ?
C7 C8 1.534(4) . ?
C8 C10 1.529(5) . ?
C8 C9 1.532(4) . ?
C8 C11 1.541(4) . ?
C12 C13 1.551(4) . ?
C13 C14 1.522(4) . ?
C13 C15 1.530(4) . ?
C13 C16 1.533(4) . ?
C17 C22 1.381(4) . ?
C17 C18 1.412(4) . ?
C18 C19 1.402(4) . ?
C19 C20 1.381(4) . ?
C20 C21 1.376(4) . ?
C21 C22 1.388(4) . ?
C23 C24 1.554(4) . ?
C24 C26 1.513(5) . ?
C24 C27 1.516(4) . ?
C24 C25 1.530(4) . ?
C28 C29 1.543(4) . ?
C29 C30 1.527(4) . ?
C29 C31 1.529(4) . ?
C29 C32 1.535(4) . ?
