#------------------------------------------------------------------------------
#$Date: 2025-08-21 12:25:49 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301846 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/67/7006746.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_7006746
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            'C40 H57 N3'
_chemical_formula_weight         579.89
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.309(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.553(7)
_cell_length_b                   16.399(9)
_cell_length_c                   19.071(11)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     3804(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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0940
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16070
_diffrn_reflns_theta_full        23.32
_diffrn_reflns_theta_max         23.32
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.058
_exptl_absorpt_correction_T_max  0.351037
_exptl_absorpt_correction_T_min  0.037381
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_density_diffrn    1.013
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.158
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.030
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.769
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5424
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.769
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0641P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1203
_reflns_number_gt                2263
_reflns_number_total             5424
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b513531a.txt
_cod_data_source_block           i-Pr2C6H3N(C(Me)NC6H3i-Pr2)2
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7006746
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
N1 N 0.82194(17) 0.30854(11) -0.09353(11) 0.0544(6) Uani 1 1 d . . .
N2 N 0.72768(17) 0.20712(12) 0.05699(11) 0.0557(6) Uani 1 1 d . . .
N3 N 0.87734(16) 0.25366(12) 0.02052(10) 0.0503(5) Uani 1 1 d . . .
C1 C 0.8364(2) 0.36068(16) -0.15048(14) 0.0565(7) Uani 1 1 d . . .
C2 C 0.9018(2) 0.33632(16) -0.19713(15) 0.0633(8) Uani 1 1 d . . .
C3 C 0.9086(3) 0.3883(2) -0.25374(15) 0.0782(9) Uani 1 1 d . . .
H3A H 0.9510 0.3732 -0.2853 0.094 Uiso 1 1 calc R . .
C4 C 0.8539(3) 0.4612(2) -0.26367(17) 0.0898(11) Uani 1 1 d . . .
H4A H 0.8608 0.4954 -0.3012 0.108 Uiso 1 1 calc R . .
C5 C 0.7890(3) 0.48447(18) -0.21886(18) 0.0845(10) Uani 1 1 d . . .
H5A H 0.7517 0.5340 -0.2267 0.101 Uiso 1 1 calc R . .
C6 C 0.7782(2) 0.43425(17) -0.16122(15) 0.0668(8) Uani 1 1 d . . .
C7 C 0.9622(2) 0.25531(18) -0.18794(16) 0.0808(9) Uani 1 1 d . . .
H7A H 0.9578 0.2331 -0.1410 0.097 Uiso 1 1 calc R . .
C8 C 0.9070(4) 0.1955(2) -0.2443(2) 0.177(2) Uani 1 1 d . . .
H8A H 0.9462 0.1447 -0.2368 0.266 Uiso 1 1 calc R . .
H8B H 0.9066 0.2164 -0.2914 0.266 Uiso 1 1 calc R . .
H8C H 0.8328 0.1869 -0.2410 0.266 Uiso 1 1 calc R . .
C9 C 1.0834(3) 0.2632(2) -0.1860(2) 0.1481(15) Uani 1 1 d . . .
H9A H 1.1172 0.2103 -0.1793 0.222 Uiso 1 1 calc R . .
H9B H 1.1185 0.2982 -0.1467 0.222 Uiso 1 1 calc R . .
H9C H 1.0912 0.2861 -0.2308 0.222 Uiso 1 1 calc R . .
C10 C 0.7035(3) 0.45873(18) -0.11274(17) 0.0872(10) Uani 1 1 d . . .
H10A H 0.7092 0.4162 -0.0759 0.105 Uiso 1 1 calc R . .
C11 C 0.5835(3) 0.4641(3) -0.1543(2) 0.1475(15) Uani 1 1 d . . .
H11A H 0.5393 0.4788 -0.1217 0.221 Uiso 1 1 calc R . .
H11B H 0.5599 0.4123 -0.1759 0.221 Uiso 1 1 calc R . .
H11C H 0.5756 0.5048 -0.1915 0.221 Uiso 1 1 calc R . .
C12 C 0.7377(3) 0.5383(3) -0.0740(2) 0.1649(19) Uani 1 1 d . . .
H12A H 0.8126 0.5344 -0.0464 0.247 Uiso 1 1 calc R . .
H12B H 0.6911 0.5496 -0.0421 0.247 Uiso 1 1 calc R . .
H12C H 0.7311 0.5814 -0.1088 0.247 Uiso 1 1 calc R . .
C13 C 0.6347(2) 0.15560(16) 0.05467(14) 0.0567(7) Uani 1 1 d . . .
C14 C 0.6513(2) 0.08719(18) 0.10009(15) 0.0650(8) Uani 1 1 d . . .
C15 C 0.5582(3) 0.04114(19) 0.10304(17) 0.0843(9) Uani 1 1 d . . .
H15A H 0.5665 -0.0051 0.1321 0.101 Uiso 1 1 calc R . .
C16 C 0.4550(3) 0.0631(2) 0.0637(2) 0.0890(10) Uani 1 1 d . . .
H16A H 0.3944 0.0318 0.0665 0.107 Uiso 1 1 calc R . .
C17 C 0.4414(2) 0.1309(2) 0.02071(17) 0.0849(9) Uani 1 1 d . . .
H17A H 0.3710 0.1449 -0.0054 0.102 Uiso 1 1 calc R . .
C18 C 0.5297(2) 0.17949(17) 0.01465(15) 0.0649(8) Uani 1 1 d . . .
C19 C 0.7647(3) 0.06521(17) 0.14517(16) 0.0796(9) Uani 1 1 d . . .
H19A H 0.8181 0.0889 0.1213 0.095 Uiso 1 1 calc R . .
C20 C 0.7872(3) -0.02591(19) 0.15205(18) 0.1211(13) Uani 1 1 d . . .
H20A H 0.7768 -0.0494 0.1047 0.182 Uiso 1 1 calc R . .
H20B H 0.7374 -0.0509 0.1765 0.182 Uiso 1 1 calc R . .
H20C H 0.8615 -0.0350 0.1792 0.182 Uiso 1 1 calc R . .
C21 C 0.7850(3) 0.1040(2) 0.22058(19) 0.1446(16) Uani 1 1 d . . .
H21A H 0.7734 0.1618 0.2158 0.217 Uiso 1 1 calc R . .
H21B H 0.8593 0.0935 0.2471 0.217 Uiso 1 1 calc R . .
H21C H 0.7351 0.0810 0.2461 0.217 Uiso 1 1 calc R . .
C22 C 0.5110(2) 0.2561(2) -0.03128(17) 0.0862(9) Uani 1 1 d . . .
H22A H 0.5822 0.2721 -0.0395 0.103 Uiso 1 1 calc R . .
C23 C 0.4326(3) 0.2434(3) -0.1050(2) 0.1598(17) Uani 1 1 d . . .
H23A H 0.4249 0.2935 -0.1319 0.240 Uiso 1 1 calc R . .
H23B H 0.3621 0.2268 -0.0989 0.240 Uiso 1 1 calc R . .
H23C H 0.4612 0.2019 -0.1308 0.240 Uiso 1 1 calc R . .
C24 C 0.4726(4) 0.3252(2) 0.0089(2) 0.185(2) Uani 1 1 d . . .
H24A H 0.5236 0.3325 0.0551 0.277 Uiso 1 1 calc R . .
H24B H 0.4013 0.3125 0.0159 0.277 Uiso 1 1 calc R . .
H24C H 0.4684 0.3746 -0.0187 0.277 Uiso 1 1 calc R . .
C25 C 0.9455(2) 0.25828(16) 0.09437(13) 0.0558(7) Uani 1 1 d . . .
C26 C 1.0308(2) 0.20032(18) 0.11573(15) 0.0670(8) Uani 1 1 d . . .
C27 C 1.0967(3) 0.2052(2) 0.18560(17) 0.0894(10) Uani 1 1 d . . .
H27A H 1.1529 0.1674 0.2010 0.107 Uiso 1 1 calc R . .
C28 C 1.0805(3) 0.2645(2) 0.23215(18) 0.1029(12) Uani 1 1 d . . .
H28A H 1.1262 0.2668 0.2786 0.123 Uiso 1 1 calc R . .
C29 C 0.9976(3) 0.3208(2) 0.21140(17) 0.0921(11) Uani 1 1 d . . .
H29A H 0.9880 0.3605 0.2441 0.110 Uiso 1 1 calc R . .
C30 C 0.9269(3) 0.31914(17) 0.14129(15) 0.0697(8) Uani 1 1 d . . .
C31 C 0.8350(3) 0.38102(17) 0.12082(16) 0.0840(9) Uani 1 1 d . . .
H31A H 0.7967 0.3715 0.0701 0.101 Uiso 1 1 calc R . .
C32 C 0.8783(3) 0.46962(18) 0.12718(19) 0.1312(14) Uani 1 1 d . . .
H32A H 0.9295 0.4762 0.0976 0.197 Uiso 1 1 calc R . .
H32B H 0.9144 0.4811 0.1767 0.197 Uiso 1 1 calc R . .
H32C H 0.8178 0.5066 0.1112 0.197 Uiso 1 1 calc R . .
C33 C 0.7509(3) 0.3706(2) 0.1666(2) 0.1296(13) Uani 1 1 d . . .
H33A H 0.7226 0.3159 0.1614 0.194 Uiso 1 1 calc R . .
H33B H 0.6915 0.4085 0.1505 0.194 Uiso 1 1 calc R . .
H33C H 0.7859 0.3809 0.2165 0.194 Uiso 1 1 calc R . .
C34 C 1.0523(3) 0.1340(2) 0.06513(16) 0.0932(10) Uani 1 1 d . . .
H34A H 0.9917 0.1345 0.0214 0.112 Uiso 1 1 calc R . .
C35 C 1.0577(3) 0.0490(2) 0.0989(2) 0.1307(14) Uani 1 1 d . . .
H35A H 0.9901 0.0379 0.1120 0.196 Uiso 1 1 calc R . .
H35B H 1.1177 0.0468 0.1413 0.196 Uiso 1 1 calc R . .
H35C H 1.0687 0.0091 0.0645 0.196 Uiso 1 1 calc R . .
C36 C 1.1594(3) 0.1512(3) 0.0427(2) 0.1652(18) Uani 1 1 d . . .
H36A H 1.1557 0.2043 0.0211 0.248 Uiso 1 1 calc R . .
H36B H 1.1692 0.1109 0.0083 0.248 Uiso 1 1 calc R . .
H36C H 1.2203 0.1491 0.0845 0.248 Uiso 1 1 calc R . .
C37 C 0.7807(2) 0.20363(13) 0.00839(13) 0.0473(6) Uani 1 1 d . . .
C38 C 0.7574(2) 0.14735(14) -0.05594(12) 0.0633(7) Uani 1 1 d . . .
H38B H 0.6911 0.1174 -0.0576 0.095 Uiso 1 1 calc R . .
H38C H 0.8175 0.1100 -0.0518 0.095 Uiso 1 1 calc R . .
H38D H 0.7486 0.1788 -0.0995 0.095 Uiso 1 1 calc R . .
C39 C 0.8940(2) 0.30585(14) -0.03353(14) 0.0507(7) Uani 1 1 d . . .
C40 C 0.9984(2) 0.35610(16) -0.01545(14) 0.0779(9) Uani 1 1 d . . .
H40B H 1.0015 0.3896 -0.0562 0.117 Uiso 1 1 calc R . .
H40C H 1.0609 0.3204 -0.0042 0.117 Uiso 1 1 calc R . .
H40D H 0.9989 0.3902 0.0256 0.117 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'
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
C39 N1 C1 120.6(2) . . ?
C37 N2 C13 121.4(2) . . ?
C39 N3 C37 120.44(19) . . ?
C39 N3 C25 121.5(2) . . ?
C37 N3 C25 117.13(19) . . ?
C6 C1 C2 121.1(3) . . ?
C6 C1 N1 117.9(3) . . ?
C2 C1 N1 120.9(2) . . ?
C3 C2 C1 118.2(3) . . ?
C3 C2 C7 120.0(3) . . ?
C1 C2 C7 121.8(2) . . ?
C4 C3 C2 121.1(3) . . ?
C3 C4 C5 120.7(3) . . ?
C4 C5 C6 120.7(3) . . ?
C1 C6 C5 118.2(3) . . ?
C1 C6 C10 121.0(3) . . ?
C5 C6 C10 120.8(3) . . ?
C8 C7 C9 110.9(3) . . ?
C8 C7 C2 111.2(3) . . ?
C9 C7 C2 113.4(3) . . ?
C12 C10 C11 109.3(3) . . ?
C12 C10 C6 112.5(3) . . ?
C11 C10 C6 112.2(3) . . ?
C14 C13 C18 122.3(3) . . ?
C14 C13 N2 117.2(3) . . ?
C18 C13 N2 120.0(2) . . ?
C13 C14 C15 117.2(3) . . ?
C13 C14 C19 121.1(3) . . ?
C15 C14 C19 121.6(3) . . ?
C16 C15 C14 121.2(3) . . ?
C17 C16 C15 120.1(3) . . ?
C16 C17 C18 122.1(3) . . ?
C17 C18 C13 117.0(3) . . ?
C17 C18 C22 120.7(3) . . ?
C13 C18 C22 122.3(3) . . ?
C14 C19 C20 114.3(3) . . ?
C14 C19 C21 110.4(3) . . ?
C20 C19 C21 110.0(3) . . ?
C24 C22 C18 110.5(3) . . ?
C24 C22 C23 110.9(3) . . ?
C18 C22 C23 113.2(3) . . ?
C30 C25 C26 122.0(3) . . ?
C30 C25 N3 120.3(3) . . ?
C26 C25 N3 117.7(2) . . ?
C27 C26 C25 117.9(3) . . ?
C27 C26 C34 119.5(3) . . ?
C25 C26 C34 122.6(2) . . ?
C28 C27 C26 121.1(3) . . ?
C27 C28 C29 121.0(3) . . ?
C28 C29 C30 121.0(3) . . ?
C25 C30 C29 117.0(3) . . ?
C25 C30 C31 123.4(3) . . ?
C29 C30 C31 119.5(3) . . ?
C30 C31 C33 111.5(3) . . ?
C30 C31 C32 112.3(3) . . ?
C33 C31 C32 109.7(3) . . ?
C26 C34 C35 112.4(3) . . ?
C26 C34 C36 110.5(3) . . ?
C35 C34 C36 109.5(3) . . ?
N2 C37 N3 115.6(2) . . ?
N2 C37 C38 126.2(2) . . ?
N3 C37 C38 117.9(2) . . ?
N1 C39 N3 118.9(2) . . ?
N1 C39 C40 124.7(2) . . ?
N3 C39 C40 116.4(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
N1 C39 1.272(3) . ?
N1 C1 1.429(3) . ?
N2 C37 1.269(3) . ?
N2 C13 1.433(3) . ?
N3 C39 1.395(3) . ?
N3 C37 1.435(3) . ?
N3 C25 1.458(3) . ?
C1 C6 1.399(3) . ?
C1 C2 1.409(3) . ?
C2 C3 1.395(3) . ?
C2 C7 1.518(4) . ?
C3 C4 1.368(4) . ?
C4 C5 1.373(4) . ?
C5 C6 1.407(4) . ?
C6 C10 1.524(4) . ?
C7 C8 1.494(4) . ?
C7 C9 1.518(4) . ?
C10 C12 1.508(4) . ?
C10 C11 1.522(4) . ?
C13 C14 1.401(3) . ?
C13 C18 1.406(3) . ?
C14 C15 1.404(4) . ?
C14 C19 1.513(4) . ?
C15 C16 1.375(4) . ?
C16 C17 1.367(4) . ?
C17 C18 1.393(4) . ?
C18 C22 1.517(4) . ?
C19 C20 1.520(4) . ?
C19 C21 1.535(4) . ?
C22 C24 1.513(4) . ?
C22 C23 1.518(4) . ?
C25 C30 1.398(3) . ?
C25 C26 1.415(3) . ?
C26 C27 1.386(3) . ?
C26 C34 1.522(4) . ?
C27 C28 1.366(4) . ?
C28 C29 1.373(4) . ?
C29 C30 1.411(4) . ?
C30 C31 1.513(4) . ?
C31 C33 1.537(4) . ?
C31 C32 1.546(4) . ?
C34 C35 1.529(4) . ?
C34 C36 1.534(5) . ?
C37 C38 1.505(3) . ?
C39 C40 1.514(3) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 21175611
2 PubChem 102186281
