#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:58:42 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179771 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/67/7006748.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_7006748
loop_
_publ_author_name
'Masuda, Jason D.'
'Stephan, Douglas W.'
_publ_section_title
;
 Neutral and cationic aluminium complexes of a sterically demanding
 N-imidoylamidine ligand.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2089
_journal_page_last               2097
_journal_paper_doi               10.1039/b513531a
_journal_year                    2006
_chemical_formula_sum            'C42 H62 Al N3'
_chemical_formula_weight         635.93
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.680(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.503(6)
_cell_length_b                   21.773(13)
_cell_length_c                   18.101(10)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     3985(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_sigmaI/netI    0.0864
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16803
_diffrn_reflns_theta_full        23.28
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.488980
_exptl_absorpt_correction_T_min  0.331142
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_density_diffrn    1.060
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.179
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.029
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.803
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         5698
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.803
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0469P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0883
_reflns_number_gt                3006
_reflns_number_total             5698
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b513531a.txt
_cod_data_source_block
(i-Pr2C6H3N(C(=CH2)NC6H3i-Pr2)(C(Me)NC6H3i-Pr2)AlMe2
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7006748
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.29755(7) 0.41387(3) 0.26533(4) 0.0439(2) Uani 1 1 d . . .
N1 N 0.26763(15) 0.35798(8) 0.34203(9) 0.0345(4) Uani 1 1 d . . .
N2 N 0.21032(15) 0.36155(7) 0.18374(9) 0.0348(4) Uani 1 1 d . . .
N3 N 0.25282(15) 0.27014(7) 0.26106(10) 0.0334(4) Uani 1 1 d . . .
C1 C 0.2653(2) 0.38143(9) 0.41775(12) 0.0401(6) Uani 1 1 d . . .
C2 C 0.3822(2) 0.38522(10) 0.47768(13) 0.0463(6) Uani 1 1 d . . .
C3 C 0.3743(3) 0.40604(11) 0.54927(14) 0.0638(7) Uani 1 1 d . . .
H3A H 0.4509 0.4087 0.5896 0.077 Uiso 1 1 calc R . .
C4 C 0.2549(3) 0.42274(12) 0.56109(16) 0.0756(8) Uani 1 1 d . . .
H4A H 0.2509 0.4361 0.6092 0.091 Uiso 1 1 calc R . .
C5 C 0.1415(3) 0.41966(11) 0.50144(16) 0.0673(8) Uani 1 1 d . . .
H5A H 0.0617 0.4314 0.5102 0.081 Uiso 1 1 calc R . .
C6 C 0.1418(2) 0.39953(10) 0.42840(13) 0.0483(6) Uani 1 1 d . . .
C7 C 0.5184(2) 0.36634(11) 0.46984(13) 0.0528(6) Uani 1 1 d . . .
H7A H 0.5086 0.3543 0.4164 0.063 Uiso 1 1 calc R . .
C8 C 0.5757(3) 0.31154(12) 0.52151(16) 0.0857(9) Uani 1 1 d . . .
H8A H 0.5160 0.2774 0.5088 0.129 Uiso 1 1 calc R . .
H8B H 0.5874 0.3227 0.5742 0.129 Uiso 1 1 calc R . .
H8C H 0.6596 0.3003 0.5138 0.129 Uiso 1 1 calc R . .
C9 C 0.6170(2) 0.42013(12) 0.48901(15) 0.0848(9) Uani 1 1 d . . .
H9A H 0.5824 0.4544 0.4564 0.127 Uiso 1 1 calc R . .
H9B H 0.6998 0.4077 0.4809 0.127 Uiso 1 1 calc R . .
H9C H 0.6302 0.4318 0.5417 0.127 Uiso 1 1 calc R . .
C10 C 0.0138(2) 0.39546(11) 0.36602(14) 0.0597(7) Uani 1 1 d . . .
H10A H 0.0360 0.3936 0.3168 0.072 Uiso 1 1 calc R . .
C11 C -0.0749(3) 0.45196(12) 0.36378(16) 0.0849(9) Uani 1 1 d . . .
H11A H -0.0268 0.4885 0.3586 0.127 Uiso 1 1 calc R . .
H11B H -0.1016 0.4540 0.4104 0.127 Uiso 1 1 calc R . .
H11C H -0.1518 0.4487 0.3209 0.127 Uiso 1 1 calc R . .
C12 C -0.0635(3) 0.33746(13) 0.3728(2) 0.1111(12) Uani 1 1 d . . .
H12A H -0.0084 0.3021 0.3737 0.167 Uiso 1 1 calc R . .
H12B H -0.1401 0.3348 0.3297 0.167 Uiso 1 1 calc R . .
H12C H -0.0905 0.3390 0.4194 0.167 Uiso 1 1 calc R . .
C13 C 0.1440(2) 0.38513(9) 0.10726(12) 0.0394(6) Uani 1 1 d . . .
C14 C 0.2172(2) 0.40595(10) 0.05702(13) 0.0451(6) Uani 1 1 d . . .
C15 C 0.1482(3) 0.42663(11) -0.01563(14) 0.0622(7) Uani 1 1 d . . .
H15A H 0.1953 0.4397 -0.0495 0.075 Uiso 1 1 calc R . .
C16 C 0.0117(3) 0.42831(11) -0.03873(15) 0.0708(8) Uani 1 1 d . . .
H16A H -0.0323 0.4425 -0.0874 0.085 Uiso 1 1 calc R . .
C17 C -0.0587(2) 0.40886(11) 0.01088(15) 0.0614(7) Uani 1 1 d . . .
H17A H -0.1506 0.4102 -0.0047 0.074 Uiso 1 1 calc R . .
C18 C 0.0047(2) 0.38707(10) 0.08425(13) 0.0460(6) Uani 1 1 d . . .
C19 C 0.3672(2) 0.40756(10) 0.07867(13) 0.0525(6) Uani 1 1 d . . .
H19A H 0.3992 0.3897 0.1301 0.063 Uiso 1 1 calc R . .
C20 C 0.4259(2) 0.36974(13) 0.02450(15) 0.0860(9) Uani 1 1 d . . .
H20A H 0.3949 0.3282 0.0230 0.129 Uiso 1 1 calc R . .
H20B H 0.5206 0.3703 0.0426 0.129 Uiso 1 1 calc R . .
H20C H 0.3988 0.3871 -0.0261 0.129 Uiso 1 1 calc R . .
C21 C 0.4167(3) 0.47449(11) 0.08309(15) 0.0786(9) Uani 1 1 d . . .
H21A H 0.3804 0.4972 0.1180 0.118 Uiso 1 1 calc R . .
H21B H 0.3890 0.4929 0.0331 0.118 Uiso 1 1 calc R . .
H21C H 0.5115 0.4750 0.1009 0.118 Uiso 1 1 calc R . .
C22 C -0.0807(2) 0.36600(11) 0.13562(14) 0.0570(7) Uani 1 1 d . . .
H22A H -0.0217 0.3526 0.1847 0.068 Uiso 1 1 calc R . .
C23 C -0.1681(2) 0.31176(12) 0.10046(16) 0.0852(9) Uani 1 1 d . . .
H23A H -0.1137 0.2787 0.0915 0.128 Uiso 1 1 calc R . .
H23B H -0.2280 0.3241 0.0527 0.128 Uiso 1 1 calc R . .
H23C H -0.2175 0.2984 0.1350 0.128 Uiso 1 1 calc R . .
C24 C -0.1663(2) 0.41899(12) 0.15193(16) 0.0840(9) Uani 1 1 d . . .
H24A H -0.1103 0.4526 0.1749 0.126 Uiso 1 1 calc R . .
H24B H -0.2155 0.4051 0.1864 0.126 Uiso 1 1 calc R . .
H24C H -0.2264 0.4323 0.1047 0.126 Uiso 1 1 calc R . .
C25 C 0.2763(2) 0.20347(9) 0.26395(11) 0.0353(5) Uani 1 1 d . . .
C26 C 0.1683(2) 0.16272(10) 0.24962(12) 0.0417(6) Uani 1 1 d . . .
C27 C 0.1958(3) 0.10040(10) 0.25805(13) 0.0558(7) Uani 1 1 d . . .
H27A H 0.1261 0.0727 0.2504 0.067 Uiso 1 1 calc R . .
C28 C 0.3234(3) 0.07851(11) 0.27733(13) 0.0650(7) Uani 1 1 d . . .
H28A H 0.3391 0.0365 0.2821 0.078 Uiso 1 1 calc R . .
C29 C 0.4279(2) 0.11902(12) 0.28961(13) 0.0597(7) Uani 1 1 d . . .
H29A H 0.5138 0.1038 0.3020 0.072 Uiso 1 1 calc R . .
C30 C 0.4074(2) 0.18237(10) 0.28391(12) 0.0430(6) Uani 1 1 d . . .
C31 C 0.0244(2) 0.18364(10) 0.22542(14) 0.0552(7) Uani 1 1 d . . .
H31A H 0.0230 0.2284 0.2196 0.066 Uiso 1 1 calc R . .
C32 C -0.0487(2) 0.15517(12) 0.14766(16) 0.0845(9) Uani 1 1 d . . .
H32A H -0.0042 0.1663 0.1097 0.127 Uiso 1 1 calc R . .
H32B H -0.1379 0.1701 0.1324 0.127 Uiso 1 1 calc R . .
H32C H -0.0494 0.1113 0.1524 0.127 Uiso 1 1 calc R . .
C33 C -0.0482(2) 0.16708(13) 0.28593(17) 0.0912(10) Uani 1 1 d . . .
H33A H -0.0032 0.1854 0.3342 0.137 Uiso 1 1 calc R . .
H33B H -0.0495 0.1233 0.2916 0.137 Uiso 1 1 calc R . .
H33C H -0.1373 0.1822 0.2698 0.137 Uiso 1 1 calc R . .
C34 C 0.5243(2) 0.22648(11) 0.29986(14) 0.0572(7) Uani 1 1 d . . .
H34A H 0.4930 0.2663 0.3130 0.069 Uiso 1 1 calc R . .
C35 C 0.6391(2) 0.20632(14) 0.36798(15) 0.0889(9) Uani 1 1 d . . .
H35A H 0.6075 0.2015 0.4127 0.133 Uiso 1 1 calc R . .
H35B H 0.7073 0.2370 0.3777 0.133 Uiso 1 1 calc R . .
H35C H 0.6741 0.1680 0.3561 0.133 Uiso 1 1 calc R . .
C36 C 0.5739(3) 0.23589(15) 0.22832(16) 0.0999(11) Uani 1 1 d . . .
H36A H 0.5018 0.2490 0.1863 0.150 Uiso 1 1 calc R . .
H36B H 0.6088 0.1979 0.2152 0.150 Uiso 1 1 calc R . .
H36C H 0.6420 0.2666 0.2387 0.150 Uiso 1 1 calc R . .
C37 C 0.2129(3) 0.26111(13) 0.12366(16) 0.0544(7) Uani 1 1 d . . .
H37A H 0.231(2) 0.2205(10) 0.1281(12) 0.056(7) Uiso 1 1 d . . .
H37B H 0.195(2) 0.2809(10) 0.0779(12) 0.056(7) Uiso 1 1 d . . .
C38 C 0.22528(18) 0.29902(10) 0.18686(12) 0.0358(5) Uani 1 1 d . . .
C39 C 0.2552(2) 0.25519(10) 0.39539(12) 0.0499(6) Uani 1 1 d . . .
H39A H 0.2587 0.2785 0.4409 0.075 Uiso 1 1 calc R . .
H39B H 0.3303 0.2283 0.4047 0.075 Uiso 1 1 calc R . .
H39C H 0.1754 0.2313 0.3818 0.075 Uiso 1 1 calc R . .
C40 C 0.25718(19) 0.29740(10) 0.33214(12) 0.0358(5) Uani 1 1 d . . .
C41 C 0.2075(3) 0.49317(10) 0.26297(15) 0.0768(8) Uani 1 1 d . . .
H41A H 0.1146 0.4864 0.2559 0.115 Uiso 1 1 calc R . .
H41B H 0.2203 0.5175 0.2214 0.115 Uiso 1 1 calc R . .
H41C H 0.2435 0.5144 0.3105 0.115 Uiso 1 1 calc R . .
C42 C 0.4919(2) 0.42152(11) 0.28012(13) 0.0697(8) Uani 1 1 d . . .
H42A H 0.5300 0.3814 0.2809 0.105 Uiso 1 1 calc R . .
H42B H 0.5311 0.4420 0.3279 0.105 Uiso 1 1 calc R . .
H42C H 0.5084 0.4449 0.2387 0.105 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 0.0000 0.0000 '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'
Al Al 0.0645 0.0514 '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 Al1 N1 92.47(8) . . ?
N2 Al1 C41 112.54(10) . . ?
N1 Al1 C41 113.45(10) . . ?
N2 Al1 C42 114.65(9) . . ?
N1 Al1 C42 108.38(9) . . ?
C41 Al1 C42 113.54(11) . . ?
C40 N1 C1 116.63(17) . . ?
C40 N1 Al1 123.36(14) . . ?
C1 N1 Al1 119.86(14) . . ?
C38 N2 C13 114.04(17) . . ?
C38 N2 Al1 122.67(14) . . ?
C13 N2 Al1 122.18(13) . . ?
C40 N3 C38 128.16(17) . . ?
C40 N3 C25 114.85(16) . . ?
C38 N3 C25 116.97(16) . . ?
C2 C1 C6 121.3(2) . . ?
C2 C1 N1 120.65(19) . . ?
C6 C1 N1 118.04(19) . . ?
C3 C2 C1 118.5(2) . . ?
C3 C2 C7 117.7(2) . . ?
C1 C2 C7 123.8(2) . . ?
C4 C3 C2 121.0(2) . . ?
C5 C4 C3 119.8(2) . . ?
C4 C5 C6 122.4(2) . . ?
C5 C6 C1 117.0(2) . . ?
C5 C6 C10 120.0(2) . . ?
C1 C6 C10 123.0(2) . . ?
C2 C7 C8 112.0(2) . . ?
C2 C7 C9 111.3(2) . . ?
C8 C7 C9 109.0(2) . . ?
C6 C10 C12 112.0(2) . . ?
C6 C10 C11 112.6(2) . . ?
C12 C10 C11 109.4(2) . . ?
C18 C13 C14 120.1(2) . . ?
C18 C13 N2 118.71(18) . . ?
C14 C13 N2 121.21(19) . . ?
C15 C14 C13 118.4(2) . . ?
C15 C14 C19 118.3(2) . . ?
C13 C14 C19 123.2(2) . . ?
C16 C15 C14 121.8(2) . . ?
C17 C16 C15 119.4(2) . . ?
C16 C17 C18 121.5(2) . . ?
C17 C18 C13 118.7(2) . . ?
C17 C18 C22 118.2(2) . . ?
C13 C18 C22 123.0(2) . . ?
C14 C19 C20 113.0(2) . . ?
C14 C19 C21 110.3(2) . . ?
C20 C19 C21 110.7(2) . . ?
C23 C22 C18 111.4(2) . . ?
C23 C22 C24 110.1(2) . . ?
C18 C22 C24 111.2(2) . . ?
C30 C25 C26 121.79(19) . . ?
C30 C25 N3 118.44(18) . . ?
C26 C25 N3 119.73(18) . . ?
C27 C26 C25 117.5(2) . . ?
C27 C26 C31 119.0(2) . . ?
C25 C26 C31 123.46(19) . . ?
C28 C27 C26 121.8(2) . . ?
C27 C28 C29 119.9(2) . . ?
C28 C29 C30 121.3(2) . . ?
C29 C30 C25 117.6(2) . . ?
C29 C30 C34 120.6(2) . . ?
C25 C30 C34 121.8(2) . . ?
C26 C31 C33 111.7(2) . . ?
C26 C31 C32 110.64(19) . . ?
C33 C31 C32 109.7(2) . . ?
C30 C34 C36 111.4(2) . . ?
C30 C34 C35 112.9(2) . . ?
C36 C34 C35 110.1(2) . . ?
N2 C38 C37 125.0(2) . . ?
N2 C38 N3 117.67(19) . . ?
C37 C38 N3 117.4(2) . . ?
N1 C40 N3 121.48(18) . . ?
N1 C40 C39 122.1(2) . . ?
N3 C40 C39 116.37(19) . . ?
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 N2 1.8939(19) . ?
Al1 N1 1.9348(18) . ?
Al1 C41 1.964(3) . ?
Al1 C42 1.993(3) . ?
N1 C40 1.332(3) . ?
N1 C1 1.469(2) . ?
N2 C38 1.370(3) . ?
N2 C13 1.464(3) . ?
N3 C40 1.406(2) . ?
N3 C38 1.440(3) . ?
N3 C25 1.471(3) . ?
C1 C2 1.404(3) . ?
C1 C6 1.418(3) . ?
C2 C3 1.396(3) . ?
C2 C7 1.532(3) . ?
C3 C4 1.377(3) . ?
C4 C5 1.376(3) . ?
C5 C6 1.394(3) . ?
C6 C10 1.506(3) . ?
C7 C8 1.535(3) . ?
C7 C9 1.539(3) . ?
C10 C12 1.524(3) . ?
C10 C11 1.538(3) . ?
C13 C18 1.409(3) . ?
C13 C14 1.414(3) . ?
C14 C15 1.394(3) . ?
C14 C19 1.518(3) . ?
C15 C16 1.381(3) . ?
C16 C17 1.375(3) . ?
C17 C18 1.398(3) . ?
C18 C22 1.527(3) . ?
C19 C20 1.531(3) . ?
C19 C21 1.542(3) . ?
C22 C23 1.525(3) . ?
C22 C24 1.539(3) . ?
C25 C30 1.403(3) . ?
C25 C26 1.408(3) . ?
C26 C27 1.387(3) . ?
C26 C31 1.525(3) . ?
C27 C28 1.375(3) . ?
C28 C29 1.379(3) . ?
C29 C30 1.396(3) . ?
C30 C34 1.523(3) . ?
C31 C33 1.537(3) . ?
C31 C32 1.540(3) . ?
C34 C36 1.535(3) . ?
C34 C35 1.537(3) . ?
C37 C38 1.388(3) . ?
C39 C40 1.473(3) . ?
