Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Douglas W. Stephan' _publ_contact_author_address ; Dept of Chemistry & Biochemistry University of Windsor Windsor Ontario N9P 3P4 CANADA ; _publ_contact_author_email STEPHAN@UWINDSOR.CA _publ_section_title ; Neutral and Cationic Aluminum-Alkyl and Hydride Complexes of A Sterically Demanding Diimine Ligand ; loop_ _publ_author_name 'Jason D. Masuda' 'Jenny S. J. McCahill' 'Douglas W. Stephan' data_i-Pr2C6H3N(C(Me)NC6H3i-Pr2)2 _database_code_depnum_ccdc_archive 'CCDC 284668' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C40 H57 N3' _chemical_formula_weight 579.89 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n 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' _cell_length_a 12.553(7) _cell_length_b 16.399(9) _cell_length_c 19.071(11) _cell_angle_alpha 90.00 _cell_angle_beta 104.309(11) _cell_angle_gamma 90.00 _cell_volume 3804(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.013 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 0.058 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.037381 _exptl_absorpt_correction_T_max 0.351037 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 16070 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0940 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 23.32 _reflns_number_total 5424 _reflns_number_gt 2263 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0641P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 5424 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1144 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1203 _refine_ls_wR_factor_gt 0.1085 _refine_ls_goodness_of_fit_ref 0.769 _refine_ls_restrained_S_all 0.769 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0524(14) 0.0551(13) 0.0515(13) 0.0050(11) 0.0047(12) -0.0032(11) N2 0.0490(14) 0.0633(14) 0.0570(14) -0.0058(11) 0.0170(13) -0.0110(12) N3 0.0417(13) 0.0616(13) 0.0452(13) 0.0039(11) 0.0065(11) -0.0098(11) C1 0.0596(18) 0.0517(17) 0.0510(16) 0.0060(15) -0.0004(15) -0.0078(15) C2 0.070(2) 0.0613(19) 0.0567(18) -0.0014(16) 0.0127(17) -0.0135(16) C3 0.090(2) 0.082(2) 0.0624(19) 0.0037(18) 0.0187(18) -0.015(2) C4 0.107(3) 0.089(3) 0.068(2) 0.016(2) 0.010(2) -0.021(2) C5 0.103(3) 0.065(2) 0.077(2) 0.0171(19) 0.006(2) 0.0044(19) C6 0.073(2) 0.0597(18) 0.0611(18) 0.0087(17) 0.0045(17) -0.0004(17) C7 0.087(2) 0.075(2) 0.091(2) 0.0019(19) 0.0408(19) 0.002(2) C8 0.161(4) 0.103(3) 0.235(5) -0.078(3) -0.014(4) 0.012(3) C9 0.096(3) 0.138(3) 0.223(4) 0.008(3) 0.064(3) 0.022(3) C10 0.099(3) 0.078(2) 0.082(2) 0.0110(18) 0.017(2) 0.031(2) C11 0.094(3) 0.186(4) 0.169(4) -0.029(3) 0.045(3) -0.024(3) C12 0.113(3) 0.187(4) 0.194(4) -0.110(4) 0.037(3) -0.012(3) C13 0.054(2) 0.0644(18) 0.0574(17) -0.0072(15) 0.0236(16) -0.0087(17) C14 0.065(2) 0.072(2) 0.0631(18) -0.0051(16) 0.0248(17) -0.0110(18) C15 0.100(3) 0.086(2) 0.077(2) -0.0013(17) 0.042(2) -0.019(2) C16 0.079(3) 0.108(3) 0.091(2) -0.015(2) 0.042(2) -0.036(2) C17 0.056(2) 0.115(3) 0.088(2) -0.018(2) 0.0274(19) -0.016(2) C18 0.0480(19) 0.082(2) 0.0695(19) -0.0118(16) 0.0235(17) -0.0073(18) C19 0.081(2) 0.077(2) 0.087(2) 0.0189(18) 0.031(2) 0.0012(18) C20 0.147(4) 0.094(3) 0.125(3) 0.023(2) 0.040(3) 0.016(2) C21 0.132(3) 0.163(4) 0.112(3) -0.038(3) -0.021(3) 0.028(3) C22 0.059(2) 0.097(2) 0.102(2) 0.012(2) 0.018(2) 0.008(2) C23 0.132(4) 0.208(4) 0.116(3) 0.047(3) -0.014(3) -0.027(3) C24 0.267(6) 0.115(3) 0.192(4) 0.015(3) 0.094(4) 0.072(4) C25 0.0538(18) 0.0649(18) 0.0480(17) -0.0027(15) 0.0112(15) -0.0125(16) C26 0.0469(18) 0.092(2) 0.0550(19) 0.0003(16) -0.0001(16) -0.0006(17) C27 0.074(2) 0.122(3) 0.062(2) -0.004(2) -0.003(2) 0.006(2) C28 0.105(3) 0.119(3) 0.067(2) -0.003(2) -0.010(2) -0.006(3) C29 0.118(3) 0.090(2) 0.061(2) -0.0221(18) 0.009(2) -0.013(2) C30 0.078(2) 0.066(2) 0.061(2) -0.0071(16) 0.0098(18) -0.0135(17) C31 0.103(3) 0.066(2) 0.080(2) -0.0179(17) 0.018(2) -0.003(2) C32 0.168(4) 0.070(2) 0.148(3) -0.021(2) 0.024(3) -0.013(2) C33 0.136(3) 0.132(3) 0.138(3) -0.040(3) 0.064(3) 0.006(3) C34 0.070(2) 0.131(3) 0.070(2) -0.011(2) 0.0005(18) 0.035(2) C35 0.117(3) 0.117(3) 0.156(3) -0.020(3) 0.030(3) 0.021(3) C36 0.139(4) 0.219(5) 0.170(4) 0.041(3) 0.100(3) 0.060(4) C37 0.0424(17) 0.0436(14) 0.0524(16) 0.0023(13) 0.0051(15) -0.0010(14) C38 0.0630(18) 0.0575(16) 0.0711(17) -0.0099(14) 0.0197(15) -0.0112(14) C39 0.0478(18) 0.0499(16) 0.0543(17) 0.0012(14) 0.0123(16) -0.0052(14) C40 0.066(2) 0.092(2) 0.0717(18) 0.0054(16) 0.0091(16) -0.0332(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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_ _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) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 23.32 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.158 _refine_diff_density_min -0.190 _refine_diff_density_rms 0.030 #===end data_[i-Pr2C6H3N(C(Me)NC6H3i-Pr2)2)AlI2][AlI4] _database_code_depnum_ccdc_archive 'CCDC 284669' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C42 H61 Al2 I6 N3 O0.50' _chemical_formula_weight 1431.30 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P21212 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 14.196(7) _cell_length_b 35.926(17) _cell_length_c 10.613(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5413(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2728 _exptl_absorpt_coefficient_mu 3.505 _exptl_absorpt_correction_type none _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 21314 _diffrn_reflns_av_R_equivalents 0.1914 _diffrn_reflns_av_sigmaI/netI 0.1413 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 23.22 _reflns_number_total 7706 _reflns_number_gt 5922 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0748P)^2^+106.3021P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.48(8) _refine_ls_number_reflns 7706 _refine_ls_number_parameters 483 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1258 _refine_ls_R_factor_gt 0.0980 _refine_ls_wR_factor_ref 0.2556 _refine_ls_wR_factor_gt 0.2286 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 I1 I 0.80438(12) 0.25194(3) 0.32828(15) 0.0531(4) Uani 1 1 d . . . I2 I 0.80211(14) 0.31446(5) 0.65452(14) 0.0665(5) Uani 1 1 d . . . I3 I 0.80575(18) 0.16627(5) 0.0899(2) 0.0860(6) Uani 1 1 d . . . I4 I 0.75694(18) 0.10677(6) -0.2332(2) 0.0902(7) Uani 1 1 d . . . I5 I 0.95005(18) 0.06634(9) 0.0228(3) 0.1220(11) Uani 1 1 d . . . I6 I 0.66699(17) 0.06460(6) 0.1084(3) 0.1015(8) Uani 1 1 d . . . Al1 Al 0.7982(6) 0.10114(19) -0.0005(7) 0.0584(18) Uani 1 1 d . . . Al2 Al 0.8040(4) 0.31486(13) 0.4205(5) 0.0289(11) Uani 1 1 d . . . N1 N 0.7086(12) 0.3482(4) 0.3612(13) 0.035(4) Uani 1 1 d . . . N2 N 0.8116(11) 0.3999(4) 0.3615(11) 0.026(3) Uani 1 1 d . . . N3 N 0.9041(11) 0.3463(4) 0.3587(14) 0.034(4) Uani 1 1 d . . . C1 C 0.7217(13) 0.3843(5) 0.3535(17) 0.033(5) Uani 1 1 d . . . C2 C 0.6437(15) 0.4107(6) 0.336(3) 0.053(6) Uani 1 1 d . . . H2A H 0.5853 0.3973 0.3321 0.080 Uiso 1 1 calc R . . H2B H 0.6529 0.4244 0.2598 0.080 Uiso 1 1 calc R . . H2C H 0.6420 0.4277 0.4064 0.080 Uiso 1 1 calc R . . C3 C 0.8971(13) 0.3816(4) 0.3488(18) 0.027(4) Uani 1 1 d . . . C4 C 0.9821(13) 0.4051(5) 0.333(2) 0.040(5) Uani 1 1 d . . . H4A H 1.0366 0.3895 0.3248 0.060 Uiso 1 1 calc R . . H4B H 0.9892 0.4211 0.4045 0.060 Uiso 1 1 calc R . . H4C H 0.9756 0.4200 0.2579 0.060 Uiso 1 1 calc R . . C5 C 0.6121(13) 0.3334(6) 0.339(3) 0.045(5) Uani 1 1 d . . . C6 C 0.5431(16) 0.3321(6) 0.431(3) 0.054(7) Uani 1 1 d . . . C7 C 0.4566(19) 0.3173(9) 0.405(4) 0.084(9) Uani 1 1 d . . . H7A H 0.4103 0.3162 0.4669 0.101 Uiso 1 1 calc R . . C8 C 0.4388(18) 0.3036(10) 0.281(5) 0.109(15) Uani 1 1 d . . . H8A H 0.3797 0.2944 0.2590 0.130 Uiso 1 1 calc R . . C9 C 0.5084(18) 0.3041(7) 0.197(3) 0.073(9) Uani 1 1 d . . . H9A H 0.4966 0.2926 0.1206 0.087 Uiso 1 1 calc R . . C10 C 0.5983(18) 0.3202(6) 0.212(3) 0.057(7) Uani 1 1 d . . . C11 C 0.5567(19) 0.3464(8) 0.567(2) 0.059(7) Uani 1 1 d . . . H11A H 0.6214 0.3557 0.5746 0.071 Uiso 1 1 calc R . . C12 C 0.490(3) 0.3780(10) 0.598(4) 0.115(14) Uani 1 1 d . . . H12A H 0.4992 0.3980 0.5394 0.172 Uiso 1 1 calc R . . H12B H 0.5032 0.3868 0.6821 0.172 Uiso 1 1 calc R . . H12C H 0.4264 0.3693 0.5938 0.172 Uiso 1 1 calc R . . C13 C 0.544(2) 0.3134(12) 0.661(4) 0.122(14) Uani 1 1 d . . . H13A H 0.5527 0.3222 0.7455 0.183 Uiso 1 1 calc R . . H13B H 0.5903 0.2945 0.6431 0.183 Uiso 1 1 calc R . . H13C H 0.4823 0.3031 0.6520 0.183 Uiso 1 1 calc R . . C14 C 0.666(2) 0.3215(7) 0.112(3) 0.067(7) Uani 1 1 d . . . H14A H 0.7284 0.3211 0.1511 0.080 Uiso 1 1 calc R . . C15 C 0.662(3) 0.3570(10) 0.023(3) 0.114(14) Uani 1 1 d . . . H15A H 0.6649 0.3791 0.0738 0.172 Uiso 1 1 calc R . . H15B H 0.6040 0.3568 -0.0235 0.172 Uiso 1 1 calc R . . H15C H 0.7141 0.3565 -0.0339 0.172 Uiso 1 1 calc R . . C16 C 0.660(3) 0.2869(9) 0.020(3) 0.102(12) Uani 1 1 d . . . H16A H 0.6624 0.2642 0.0679 0.154 Uiso 1 1 calc R . . H16B H 0.7127 0.2875 -0.0374 0.154 Uiso 1 1 calc R . . H16C H 0.6025 0.2879 -0.0270 0.154 Uiso 1 1 calc R . . C17 C 0.9941(14) 0.3270(5) 0.3280(19) 0.037(5) Uani 1 1 d . . . C18 C 1.0621(13) 0.3207(5) 0.421(2) 0.038(5) Uani 1 1 d . . . C19 C 1.1384(16) 0.2994(7) 0.388(2) 0.056(7) Uani 1 1 d . . . H19A H 1.1805 0.2929 0.4514 0.067 Uiso 1 1 calc R . . C20 C 1.1561(17) 0.2876(6) 0.273(3) 0.057(7) Uani 1 1 d . . . H20A H 1.2110 0.2745 0.2551 0.068 Uiso 1 1 calc R . . C21 C 1.0896(18) 0.2954(6) 0.178(3) 0.064(7) Uani 1 1 d . . . H21A H 1.1008 0.2870 0.0965 0.076 Uiso 1 1 calc R . . C22 C 1.0082(14) 0.3150(5) 0.2035(17) 0.033(4) Uani 1 1 d . . . C23 C 1.052(2) 0.3360(11) 0.552(2) 0.083(10) Uani 1 1 d . . . H23A H 0.9913 0.3487 0.5596 0.099 Uiso 1 1 calc R . . C24 C 1.056(3) 0.3033(12) 0.650(3) 0.116(14) Uani 1 1 d . . . H24A H 1.0052 0.2863 0.6337 0.174 Uiso 1 1 calc R . . H24B H 1.0499 0.3131 0.7336 0.174 Uiso 1 1 calc R . . H24C H 1.1150 0.2905 0.6422 0.174 Uiso 1 1 calc R . . C25 C 1.133(2) 0.3650(9) 0.572(2) 0.088(10) Uani 1 1 d . . . H25A H 1.1274 0.3844 0.5106 0.131 Uiso 1 1 calc R . . H25B H 1.1926 0.3530 0.5639 0.131 Uiso 1 1 calc R . . H25C H 1.1275 0.3756 0.6552 0.131 Uiso 1 1 calc R . . C26 C 0.9382(16) 0.3220(7) 0.095(2) 0.053(6) Uani 1 1 d . . . H26A H 0.8769 0.3277 0.1325 0.063 Uiso 1 1 calc R . . C27 C 0.969(2) 0.3559(8) 0.021(3) 0.081(10) Uani 1 1 d . . . H27A H 0.9250 0.3603 -0.0462 0.121 Uiso 1 1 calc R . . H27B H 1.0304 0.3519 -0.0124 0.121 Uiso 1 1 calc R . . H27C H 0.9694 0.3771 0.0764 0.121 Uiso 1 1 calc R . . C28 C 0.923(3) 0.2902(10) 0.004(3) 0.101(12) Uani 1 1 d . . . H28A H 0.8790 0.2974 -0.0597 0.152 Uiso 1 1 calc R . . H28B H 0.8998 0.2690 0.0488 0.152 Uiso 1 1 calc R . . H28C H 0.9824 0.2839 -0.0352 0.152 Uiso 1 1 calc R . . C29 C 0.8148(16) 0.4408(4) 0.3765(18) 0.040(5) Uani 1 1 d . . . C30 C 0.8241(18) 0.4538(5) 0.504(2) 0.052(6) Uani 1 1 d . . . C31 C 0.831(2) 0.4922(7) 0.519(3) 0.088(10) Uani 1 1 d . . . H31A H 0.8363 0.5022 0.5999 0.106 Uiso 1 1 calc R . . C32 C 0.832(2) 0.5156(6) 0.416(3) 0.080(9) Uani 1 1 d . . . H32A H 0.8347 0.5411 0.4293 0.096 Uiso 1 1 calc R . . C33 C 0.8276(18) 0.5032(6) 0.300(2) 0.057(7) Uani 1 1 d . . . H33A H 0.8309 0.5198 0.2326 0.069 Uiso 1 1 calc R . . C34 C 0.8183(14) 0.4646(5) 0.2762(18) 0.035(4) Uani 1 1 d . . . C35 C 0.817(3) 0.4274(7) 0.615(2) 0.079(9) Uani 1 1 d . . . H35A H 0.8088 0.4017 0.5859 0.095 Uiso 1 1 calc R . . C36 C 0.912(3) 0.4317(14) 0.694(3) 0.15(2) Uani 1 1 d . . . H36A H 0.9643 0.4253 0.6414 0.228 Uiso 1 1 calc R . . H36B H 0.9097 0.4155 0.7654 0.228 Uiso 1 1 calc R . . H36C H 0.9178 0.4570 0.7217 0.228 Uiso 1 1 calc R . . C37 C 0.738(4) 0.4382(11) 0.707(3) 0.15(2) Uani 1 1 d . . . H37A H 0.6784 0.4362 0.6653 0.218 Uiso 1 1 calc R . . H37B H 0.7476 0.4634 0.7345 0.218 Uiso 1 1 calc R . . H37C H 0.7395 0.4219 0.7783 0.218 Uiso 1 1 calc R . . C38 C 0.8116(18) 0.4517(5) 0.1384(17) 0.047(5) Uani 1 1 d . . . H38A H 0.8057 0.4245 0.1393 0.056 Uiso 1 1 calc R . . C39 C 0.899(3) 0.4612(9) 0.062(3) 0.088(10) Uani 1 1 d . . . H39A H 0.9541 0.4516 0.1045 0.132 Uiso 1 1 calc R . . H39B H 0.9048 0.4877 0.0544 0.132 Uiso 1 1 calc R . . H39C H 0.8948 0.4502 -0.0200 0.132 Uiso 1 1 calc R . . C40 C 0.724(2) 0.4673(8) 0.069(2) 0.073(9) Uani 1 1 d . . . H40A H 0.7237 0.4583 -0.0158 0.109 Uiso 1 1 calc R . . H40B H 0.7269 0.4940 0.0692 0.109 Uiso 1 1 calc R . . H40C H 0.6682 0.4592 0.1118 0.109 Uiso 1 1 calc R . . C50 C 0.430(4) 0.4779(14) 0.428(12) 0.31(8) Uani 1 1 d . . . H50A H 0.3652 0.4861 0.4185 0.374 Uiso 1 1 calc R . . H50B H 0.4328 0.4512 0.4150 0.374 Uiso 1 1 calc R . . C52 C 0.465(4) 0.4875(10) 0.546(6) 0.17(3) Uani 1 1 d . . . H52A H 0.4135 0.4973 0.5963 0.199 Uiso 1 1 calc R . . H52B H 0.4872 0.4650 0.5871 0.199 Uiso 1 1 calc R . . O1 O 0.5000 0.5000 0.330(6) 0.27(5) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0685(9) 0.0274(6) 0.0634(9) -0.0017(6) 0.0062(9) -0.0054(7) I2 0.0853(11) 0.0810(10) 0.0332(7) 0.0136(7) 0.0028(9) 0.0020(10) I3 0.1109(15) 0.0703(11) 0.0769(12) -0.0407(10) 0.0037(13) -0.0254(12) I4 0.1260(18) 0.0722(11) 0.0724(13) -0.0226(10) -0.0270(13) -0.0020(12) I5 0.0808(15) 0.146(2) 0.139(2) -0.038(2) -0.0197(15) 0.0461(15) I6 0.1012(17) 0.0783(13) 0.125(2) -0.0312(14) 0.0345(14) -0.0226(12) Al1 0.065(4) 0.057(4) 0.053(4) -0.027(3) -0.007(4) -0.002(4) Al2 0.038(3) 0.022(2) 0.027(3) 0.003(2) 0.003(3) 0.000(3) N1 0.057(11) 0.026(8) 0.022(8) 0.003(6) 0.002(8) -0.025(8) N2 0.041(9) 0.029(7) 0.007(6) 0.014(5) -0.002(6) -0.001(7) N3 0.042(9) 0.043(10) 0.015(8) 0.011(7) 0.002(7) 0.004(7) C1 0.040(12) 0.038(11) 0.022(9) 0.011(8) 0.007(8) -0.009(8) C2 0.042(12) 0.039(11) 0.078(17) 0.025(12) 0.012(12) 0.005(10) C3 0.037(10) 0.015(9) 0.030(10) 0.005(7) -0.003(8) 0.009(7) C4 0.035(11) 0.033(10) 0.053(13) 0.001(10) 0.000(10) -0.005(8) C5 0.021(10) 0.039(11) 0.074(16) 0.013(12) -0.012(11) 0.006(8) C6 0.039(13) 0.026(11) 0.10(2) 0.001(11) 0.000(13) 0.024(10) C7 0.041(15) 0.08(2) 0.13(3) 0.01(2) -0.012(17) -0.024(14) C8 0.019(14) 0.12(3) 0.19(4) 0.02(3) -0.05(2) -0.024(15) C9 0.038(15) 0.064(16) 0.12(3) -0.006(16) -0.035(16) -0.020(13) C10 0.072(17) 0.034(12) 0.066(17) -0.012(11) -0.012(13) -0.019(11) C11 0.053(14) 0.079(17) 0.045(15) 0.014(12) 0.010(12) 0.008(13) C12 0.11(3) 0.08(2) 0.16(4) 0.01(2) 0.04(3) 0.01(2) C13 0.07(2) 0.16(4) 0.14(3) 0.03(3) 0.05(2) 0.01(2) C14 0.068(17) 0.074(17) 0.058(16) -0.015(14) -0.025(14) -0.005(13) C15 0.17(4) 0.10(3) 0.07(2) 0.00(2) -0.03(2) -0.04(3) C16 0.14(3) 0.11(3) 0.059(19) -0.040(19) 0.02(2) -0.01(2) C17 0.040(11) 0.039(11) 0.032(11) 0.011(9) -0.002(10) -0.005(9) C18 0.028(10) 0.029(10) 0.056(13) 0.017(9) 0.002(9) -0.011(9) C19 0.043(13) 0.075(16) 0.048(15) 0.025(13) 0.000(11) 0.021(12) C20 0.044(13) 0.038(12) 0.09(2) -0.007(12) 0.007(13) 0.029(10) C21 0.061(16) 0.042(12) 0.09(2) -0.013(13) 0.023(15) 0.018(12) C22 0.041(11) 0.030(10) 0.027(10) 0.002(8) 0.006(8) 0.006(9) C23 0.060(16) 0.15(3) 0.035(15) 0.018(16) -0.016(13) -0.020(18) C24 0.12(3) 0.16(4) 0.07(2) 0.05(2) -0.01(2) 0.02(3) C25 0.12(3) 0.12(3) 0.018(13) 0.001(14) -0.032(15) 0.00(2) C26 0.044(12) 0.082(17) 0.032(12) -0.019(12) 0.005(10) 0.018(12) C27 0.11(2) 0.071(18) 0.064(18) 0.027(15) 0.003(17) 0.055(17) C28 0.14(3) 0.12(3) 0.042(17) -0.009(17) 0.018(19) -0.03(2) C29 0.060(13) 0.018(8) 0.040(11) -0.020(8) 0.015(10) -0.008(9) C30 0.085(18) 0.028(10) 0.043(12) 0.003(9) 0.006(12) -0.001(11) C31 0.13(3) 0.050(15) 0.09(2) -0.028(16) -0.02(2) 0.015(17) C32 0.13(3) 0.025(11) 0.08(2) -0.007(13) 0.02(2) -0.002(14) C33 0.075(17) 0.023(10) 0.075(17) 0.003(11) 0.007(13) -0.019(11) C34 0.037(11) 0.027(9) 0.041(11) 0.009(8) 0.007(9) -0.009(8) C35 0.14(3) 0.055(14) 0.041(14) -0.026(11) -0.018(17) 0.035(17) C36 0.21(5) 0.20(5) 0.05(2) 0.00(3) -0.01(3) 0.09(4) C37 0.27(6) 0.12(3) 0.05(2) 0.03(2) 0.05(3) 0.01(3) C38 0.082(15) 0.034(10) 0.025(10) 0.014(8) 0.008(11) 0.021(11) C39 0.13(3) 0.08(2) 0.055(19) 0.021(15) 0.021(19) -0.009(19) C40 0.09(2) 0.088(19) 0.039(14) 0.027(13) -0.020(13) -0.022(15) C50 0.09(3) 0.05(2) 0.8(3) -0.06(8) -0.05(9) -0.01(2) C52 0.22(9) 0.05(3) 0.22(6) 0.05(3) 0.09(6) 0.06(3) O1 0.33(9) 0.30(9) 0.19(5) 0.000 0.000 0.31(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 I1 Al2 2.463(5) . ? I2 Al2 2.483(5) . ? I3 Al1 2.531(7) . ? I4 Al1 2.546(8) . ? I5 Al1 2.504(8) . ? I6 Al1 2.556(8) . ? Al2 N1 1.915(18) . ? Al2 N3 1.931(16) . ? N1 C1 1.31(2) . ? N1 C5 1.49(3) . ? N2 C3 1.39(2) . ? N2 C1 1.40(2) . ? N2 C29 1.48(2) . ? N3 C3 1.28(2) . ? N3 C17 1.49(3) . ? C1 C2 1.47(3) . ? C3 C4 1.48(3) . ? C5 C6 1.38(3) . ? C5 C10 1.44(4) . ? C6 C7 1.37(4) . ? C6 C11 1.54(4) . ? C7 C8 1.43(5) . ? C8 C9 1.33(5) . ? C9 C10 1.41(3) . ? C10 C14 1.43(4) . ? C11 C12 1.51(4) . ? C11 C13 1.56(4) . ? C14 C16 1.59(4) . ? C14 C15 1.59(4) . ? C17 C18 1.40(3) . ? C17 C22 1.40(3) . ? C18 C19 1.37(3) . ? C18 C23 1.51(4) . ? C19 C20 1.32(4) . ? C20 C21 1.41(4) . ? C21 C22 1.38(3) . ? C22 C26 1.54(3) . ? C23 C25 1.56(4) . ? C23 C24 1.57(4) . ? C26 C27 1.51(4) . ? C26 C28 1.51(4) . ? C29 C34 1.37(3) . ? C29 C30 1.44(3) . ? C30 C31 1.39(3) . ? C30 C35 1.51(3) . ? C31 C32 1.38(4) . ? C32 C33 1.31(4) . ? C33 C34 1.41(3) . ? C34 C38 1.54(3) . ? C35 C37 1.53(5) . ? C35 C36 1.59(5) . ? C38 C39 1.52(4) . ? C38 C40 1.54(3) . ? C50 C52 1.39(11) . ? C50 O1 1.64(10) . ? C52 C52 1.34(10) 2_665 ? O1 C50 1.64(10) 2_665 ? 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 I5 Al1 I3 112.8(3) . . ? I5 Al1 I4 109.5(3) . . ? I3 Al1 I4 107.7(3) . . ? I5 Al1 I6 109.0(3) . . ? I3 Al1 I6 109.5(3) . . ? I4 Al1 I6 108.2(3) . . ? N1 Al2 N3 92.4(6) . . ? N1 Al2 I1 116.4(5) . . ? N3 Al2 I1 113.6(5) . . ? N1 Al2 I2 109.0(5) . . ? N3 Al2 I2 110.5(5) . . ? I1 Al2 I2 113.10(19) . . ? C1 N1 C5 118.2(16) . . ? C1 N1 Al2 122.6(13) . . ? C5 N1 Al2 118.7(11) . . ? C3 N2 C1 127.3(13) . . ? C3 N2 C29 116.9(15) . . ? C1 N2 C29 115.6(16) . . ? C3 N3 C17 120.8(16) . . ? C3 N3 Al2 123.6(13) . . ? C17 N3 Al2 115.6(12) . . ? N1 C1 N2 121.4(17) . . ? N1 C1 C2 122.6(17) . . ? N2 C1 C2 116.0(16) . . ? N3 C3 N2 122.0(16) . . ? N3 C3 C4 120.8(16) . . ? N2 C3 C4 117.1(14) . . ? C6 C5 C10 124(2) . . ? C6 C5 N1 123(2) . . ? C10 C5 N1 113(2) . . ? C7 C6 C5 121(3) . . ? C7 C6 C11 115(3) . . ? C5 C6 C11 124(2) . . ? C6 C7 C8 119(3) . . ? C9 C8 C7 119(2) . . ? C8 C9 C10 127(3) . . ? C9 C10 C14 122(2) . . ? C9 C10 C5 111(3) . . ? C14 C10 C5 126(2) . . ? C12 C11 C6 112(3) . . ? C12 C11 C13 111(2) . . ? C6 C11 C13 109(3) . . ? C10 C14 C16 114(2) . . ? C10 C14 C15 116(3) . . ? C16 C14 C15 105(2) . . ? C18 C17 C22 121.1(19) . . ? C18 C17 N3 120.9(18) . . ? C22 C17 N3 118.0(17) . . ? C19 C18 C17 117(2) . . ? C19 C18 C23 121(2) . . ? C17 C18 C23 122(2) . . ? C20 C19 C18 124(2) . . ? C19 C20 C21 118(2) . . ? C22 C21 C20 121(2) . . ? C21 C22 C17 117(2) . . ? C21 C22 C26 118(2) . . ? C17 C22 C26 124.3(17) . . ? C18 C23 C25 108(2) . . ? C18 C23 C24 110(3) . . ? C25 C23 C24 113(2) . . ? C27 C26 C28 109(2) . . ? C27 C26 C22 109(2) . . ? C28 C26 C22 116(2) . . ? C34 C29 C30 121.6(15) . . ? C34 C29 N2 122.7(15) . . ? C30 C29 N2 115.4(16) . . ? C31 C30 C29 116(2) . . ? C31 C30 C35 123(2) . . ? C29 C30 C35 121.2(17) . . ? C32 C31 C30 121(3) . . ? C33 C32 C31 123(2) . . ? C32 C33 C34 120(2) . . ? C29 C34 C33 118.7(19) . . ? C29 C34 C38 123.2(15) . . ? C33 C34 C38 118.1(18) . . ? C30 C35 C37 113(2) . . ? C30 C35 C36 107(3) . . ? C37 C35 C36 105(3) . . ? C39 C38 C34 113(2) . . ? C39 C38 C40 108.9(18) . . ? C34 C38 C40 113.0(18) . . ? C52 C50 O1 103(4) . . ? C52 C52 C50 116(4) 2_665 . ? C50 O1 C50 102(8) 2_665 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.22 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.025 _refine_diff_density_min -1.511 _refine_diff_density_rms 0.204 #===end data_(i-Pr2C6H3N(C(=CH2)NC6H3i-Pr2)(C(Me)NC6H3i-Pr2)AlMe2 _database_code_depnum_ccdc_archive 'CCDC 284670' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C42 H62 Al N3' _chemical_formula_weight 635.93 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c 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' _cell_length_a 10.503(6) _cell_length_b 21.773(13) _cell_length_c 18.101(10) _cell_angle_alpha 90.00 _cell_angle_beta 105.680(10) _cell_angle_gamma 90.00 _cell_volume 3985(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.22 _exptl_crystal_density_diffrn 1.060 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.331142 _exptl_absorpt_correction_T_max 0.488980 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 16803 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0864 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 23.28 _reflns_number_total 5698 _reflns_number_gt 3006 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 5698 _refine_ls_number_parameters 423 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0828 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0883 _refine_ls_wR_factor_gt 0.0824 _refine_ls_goodness_of_fit_ref 0.803 _refine_ls_restrained_S_all 0.803 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0544(5) 0.0371(4) 0.0384(4) 0.0007(3) 0.0097(3) -0.0077(3) N1 0.0393(11) 0.0316(11) 0.0337(12) -0.0031(9) 0.0119(9) -0.0013(8) N2 0.0404(11) 0.0295(11) 0.0328(12) 0.0049(9) 0.0069(9) -0.0001(8) N3 0.0377(10) 0.0299(11) 0.0325(12) 0.0010(9) 0.0095(9) 0.0033(8) C1 0.0557(16) 0.0339(13) 0.0336(14) -0.0028(11) 0.0171(13) -0.0034(11) C2 0.0601(17) 0.0443(15) 0.0335(15) -0.0032(12) 0.0108(14) -0.0025(12) C3 0.079(2) 0.0665(19) 0.0425(18) -0.0059(14) 0.0100(15) 0.0032(16) C4 0.105(3) 0.082(2) 0.0468(19) -0.0142(16) 0.0328(19) 0.0041(19) C5 0.074(2) 0.076(2) 0.063(2) -0.0129(17) 0.0367(17) 0.0048(16) C6 0.0601(18) 0.0445(15) 0.0465(17) -0.0043(12) 0.0250(14) 0.0023(12) C7 0.0518(16) 0.0600(17) 0.0405(15) -0.0048(13) 0.0024(12) -0.0001(13) C8 0.0753(19) 0.079(2) 0.088(2) 0.0114(18) -0.0026(16) 0.0115(16) C9 0.0761(19) 0.096(2) 0.080(2) -0.0100(18) 0.0165(16) -0.0265(18) C10 0.0487(16) 0.0691(19) 0.0634(18) -0.0109(14) 0.0191(14) 0.0083(14) C11 0.078(2) 0.086(2) 0.090(2) -0.0009(18) 0.0223(17) 0.0281(17) C12 0.071(2) 0.081(2) 0.173(4) -0.016(2) 0.019(2) -0.0118(18) C13 0.0478(16) 0.0314(13) 0.0360(15) 0.0028(11) 0.0061(12) -0.0009(11) C14 0.0583(16) 0.0395(14) 0.0358(15) 0.0043(12) 0.0098(13) -0.0010(12) C15 0.080(2) 0.0635(18) 0.0438(18) 0.0119(14) 0.0179(15) 0.0001(15) C16 0.089(2) 0.072(2) 0.0406(18) 0.0181(15) -0.0017(17) 0.0132(17) C17 0.0553(16) 0.0644(18) 0.0545(18) 0.0084(15) -0.0020(15) 0.0075(14) C18 0.0492(16) 0.0430(15) 0.0404(16) 0.0060(12) 0.0027(13) 0.0010(12) C19 0.0615(17) 0.0557(17) 0.0434(16) -0.0015(13) 0.0192(13) -0.0105(14) C20 0.078(2) 0.109(2) 0.081(2) -0.0281(19) 0.0379(17) -0.0029(17) C21 0.093(2) 0.076(2) 0.071(2) -0.0039(16) 0.0297(17) -0.0333(17) C22 0.0377(15) 0.0695(18) 0.0571(17) 0.0108(14) 0.0013(13) 0.0007(14) C23 0.0642(18) 0.080(2) 0.106(2) 0.0149(18) 0.0134(17) -0.0111(17) C24 0.0698(19) 0.096(2) 0.090(2) 0.0019(18) 0.0271(17) 0.0130(17) C25 0.0450(15) 0.0269(14) 0.0333(14) 0.0024(10) 0.0097(11) 0.0067(11) C26 0.0493(16) 0.0327(15) 0.0400(15) 0.0016(11) 0.0068(11) 0.0028(12) C27 0.0667(18) 0.0346(17) 0.0602(18) 0.0000(12) 0.0073(14) 0.0008(13) C28 0.084(2) 0.0356(16) 0.0656(19) 0.0003(14) 0.0036(16) 0.0171(16) C29 0.0555(18) 0.0531(19) 0.0645(19) 0.0005(14) 0.0057(14) 0.0251(15) C30 0.0415(15) 0.0472(16) 0.0388(15) -0.0014(12) 0.0084(11) 0.0098(12) C31 0.0447(15) 0.0404(15) 0.0772(19) 0.0023(14) 0.0110(14) -0.0013(12) C32 0.0637(18) 0.069(2) 0.098(2) -0.0066(17) -0.0183(16) -0.0045(15) C33 0.0674(19) 0.086(2) 0.131(3) 0.001(2) 0.0452(19) -0.0118(16) C34 0.0448(15) 0.0659(18) 0.0637(18) -0.0005(14) 0.0194(14) 0.0103(13) C35 0.0550(18) 0.132(3) 0.071(2) 0.0025(19) 0.0024(16) -0.0033(18) C36 0.068(2) 0.158(3) 0.078(2) 0.024(2) 0.0279(17) -0.007(2) C37 0.087(2) 0.0390(19) 0.0375(18) 0.0053(16) 0.0167(15) 0.0119(15) C38 0.0335(13) 0.0384(15) 0.0350(15) 0.0031(12) 0.0085(10) 0.0008(11) C39 0.0599(16) 0.0477(15) 0.0443(16) 0.0029(12) 0.0176(13) 0.0021(12) C40 0.0338(13) 0.0377(15) 0.0356(15) 0.0018(12) 0.0092(10) 0.0033(11) C41 0.113(2) 0.0469(17) 0.068(2) 0.0029(14) 0.0214(17) 0.0054(16) C42 0.0620(17) 0.096(2) 0.0469(16) 0.0063(15) 0.0074(13) -0.0395(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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) . ? 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) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.179 _refine_diff_density_min -0.193 _refine_diff_density_rms 0.029 #===end data_[(i-Pr2C6H3N(C(=CH2)NC6H3i-Pr2)(C(Me)NC6H3i-Pr2)AlH][B(C6F5)4] _database_code_depnum_ccdc_archive 'CCDC 284671' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C64 H57 Al B F20 N3' _chemical_formula_weight 1285.92 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 16.0619(19) _cell_length_b 18.950(2) _cell_length_c 20.586(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6266.0(13) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_diffrn 1.363 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2640 _exptl_absorpt_coefficient_mu 0.134 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.491051 _exptl_absorpt_correction_T_max 1.000000 _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 60173 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11040 _reflns_number_gt 7826 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+3.1891P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.2(3) _refine_ls_number_reflns 11040 _refine_ls_number_parameters 818 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0842 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1553 _refine_ls_wR_factor_gt 0.1372 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 0.30802(10) 0.22035(8) 0.03875(10) 0.0879(5) Uani 1 1 d . . . B1 B 0.0546(3) 0.7490(3) 0.0981(2) 0.0585(11) Uani 1 1 d . . . F1 F 0.0584(2) 0.79498(15) 0.23191(13) 0.0916(8) Uani 1 1 d . . . F2 F 0.1788(3) 0.8644(2) 0.29326(19) 0.1498(16) Uani 1 1 d . . . F3 F 0.3183(3) 0.9050(2) 0.2279(2) 0.1622(18) Uani 1 1 d . . . F4 F 0.3310(2) 0.8761(2) 0.0992(2) 0.1310(13) Uani 1 1 d . . . F5 F 0.20945(18) 0.81351(16) 0.03566(16) 0.0958(9) Uani 1 1 d . . . F6 F 0.04639(19) 0.87138(13) 0.01632(13) 0.0836(8) Uani 1 1 d . . . F7 F 0.0247(3) 0.87718(17) -0.11101(15) 0.1172(11) Uani 1 1 d . . . F8 F 0.0151(3) 0.7562(2) -0.18254(14) 0.1265(12) Uani 1 1 d . . . F9 F 0.0282(2) 0.62953(16) -0.12156(13) 0.0953(9) Uani 1 1 d . . . F10 F 0.05152(18) 0.62173(12) 0.00484(12) 0.0784(7) Uani 1 1 d . . . F11 F -0.09303(16) 0.66227(13) 0.08157(13) 0.0759(7) Uani 1 1 d . . . F12 F -0.25093(17) 0.69938(17) 0.09617(14) 0.0965(9) Uani 1 1 d . . . F13 F -0.29130(19) 0.8339(2) 0.13122(18) 0.1238(13) Uani 1 1 d . . . F14 F -0.1686(2) 0.92861(17) 0.15290(19) 0.1173(12) Uani 1 1 d . . . F15 F -0.01121(18) 0.89239(13) 0.14380(15) 0.0902(8) Uani 1 1 d . . . F16 F -0.03009(17) 0.66032(14) 0.20625(12) 0.0802(7) Uani 1 1 d . . . F17 F 0.0375(2) 0.55053(16) 0.26497(14) 0.1016(10) Uani 1 1 d . . . F18 F 0.1910(2) 0.50372(16) 0.23120(15) 0.1074(10) Uani 1 1 d . . . F19 F 0.27138(19) 0.56475(17) 0.12998(16) 0.1023(9) Uani 1 1 d . . . F20 F 0.20362(17) 0.67170(14) 0.06617(14) 0.0855(8) Uani 1 1 d . . . C1 C 0.4968(3) 0.21794(19) 0.0514(2) 0.0700(14) Uani 1 1 d . . . C2 C 0.5697(3) 0.2454(3) 0.0410(3) 0.0888(15) Uani 1 1 d . . . H2A H 0.5741 0.2918 0.0265 0.107 Uiso 1 1 calc R . . H2B H 0.6175 0.2188 0.0480 0.107 Uiso 1 1 calc R . . C3 C 0.4153(2) 0.1012(2) 0.07102(19) 0.0544(9) Uani 1 1 d . . . C4 C 0.4237(3) 0.0253(2) 0.0877(3) 0.0790(13) Uani 1 1 d . . . H4A H 0.3761 0.0000 0.0717 0.118 Uiso 1 1 calc R . . H4B H 0.4270 0.0201 0.1340 0.118 Uiso 1 1 calc R . . H4C H 0.4733 0.0067 0.0681 0.118 Uiso 1 1 calc R . . C5 C 0.4243(2) 0.32755(19) 0.0313(2) 0.0568(10) Uani 1 1 d . . . C6 C 0.4216(3) 0.3733(2) 0.0851(2) 0.0639(10) Uani 1 1 d . . . C7 C 0.4247(3) 0.4450(2) 0.0720(3) 0.0781(13) Uani 1 1 d . . . H7A H 0.4234 0.4767 0.1065 0.094 Uiso 1 1 calc R . . C8 C 0.4295(3) 0.4701(2) 0.0103(3) 0.0841(15) Uani 1 1 d . . . H8A H 0.4313 0.5186 0.0032 0.101 Uiso 1 1 calc R . . C9 C 0.4318(3) 0.4250(3) -0.0411(3) 0.0869(15) Uani 1 1 d . . . H9A H 0.4344 0.4434 -0.0830 0.104 Uiso 1 1 calc R . . C10 C 0.4302(3) 0.3519(2) -0.0326(2) 0.0721(12) Uani 1 1 d . . . C11 C 0.4182(3) 0.3480(3) 0.1548(2) 0.0813(14) Uani 1 1 d . . . H11A H 0.4135 0.2965 0.1542 0.098 Uiso 1 1 calc R . . C12 C 0.5001(4) 0.3670(4) 0.1906(3) 0.120(2) Uani 1 1 d . . . H12A H 0.5459 0.3428 0.1704 0.179 Uiso 1 1 calc R . . H12B H 0.4961 0.3530 0.2353 0.179 Uiso 1 1 calc R . . H12C H 0.5092 0.4170 0.1882 0.179 Uiso 1 1 calc R . . C13 C 0.3429(4) 0.3769(3) 0.1911(3) 0.116(2) Uani 1 1 d . . . H13A H 0.2929 0.3576 0.1727 0.173 Uiso 1 1 calc R . . H13B H 0.3418 0.4274 0.1874 0.173 Uiso 1 1 calc R . . H13C H 0.3464 0.3639 0.2361 0.173 Uiso 1 1 calc R . . C14 C 0.4332(4) 0.3032(3) -0.0913(2) 0.0918(16) Uani 1 1 d . . . H14A H 0.4290 0.2545 -0.0757 0.110 Uiso 1 1 calc R . . C15 C 0.3594(5) 0.3171(4) -0.1366(3) 0.125(2) Uani 1 1 d . . . H15A H 0.3086 0.3042 -0.1150 0.188 Uiso 1 1 calc R . . H15B H 0.3655 0.2895 -0.1754 0.188 Uiso 1 1 calc R . . H15C H 0.3577 0.3662 -0.1477 0.188 Uiso 1 1 calc R . . C16 C 0.5168(5) 0.3106(3) -0.1285(3) 0.113(2) Uani 1 1 d . . . H16A H 0.5183 0.2772 -0.1636 0.170 Uiso 1 1 calc R . . H16B H 0.5622 0.3016 -0.0994 0.170 Uiso 1 1 calc R . . H16C H 0.5215 0.3576 -0.1456 0.170 Uiso 1 1 calc R . . C17 C 0.5646(3) 0.1003(2) 0.0556(3) 0.0714(12) Uani 1 1 d . . . C18 C 0.6087(3) 0.0878(3) 0.1127(3) 0.0850(15) Uani 1 1 d . . . C19 C 0.6819(4) 0.0491(3) 0.1060(4) 0.115(2) Uani 1 1 d . . . H19A H 0.7140 0.0399 0.1426 0.138 Uiso 1 1 calc R . . C20 C 0.7074(4) 0.0246(4) 0.0481(4) 0.122(2) Uani 1 1 d . . . H20A H 0.7550 -0.0032 0.0458 0.146 Uiso 1 1 calc R . . C21 C 0.6632(4) 0.0406(3) -0.0093(4) 0.109(2) Uani 1 1 d . . . H21A H 0.6834 0.0255 -0.0493 0.131 Uiso 1 1 calc R . . C22 C 0.5894(3) 0.0790(3) -0.0061(3) 0.0811(14) Uani 1 1 d . . . C23 C 0.5815(4) 0.1129(4) 0.1789(3) 0.112(2) Uani 1 1 d . . . H23A H 0.5269 0.1356 0.1747 0.135 Uiso 1 1 calc R . . C24 C 0.5744(5) 0.0521(5) 0.2275(4) 0.159(3) Uani 1 1 d . . . H24A H 0.5324 0.0196 0.2131 0.238 Uiso 1 1 calc R . . H24B H 0.5594 0.0704 0.2694 0.238 Uiso 1 1 calc R . . H24C H 0.6269 0.0281 0.2305 0.238 Uiso 1 1 calc R . . C25 C 0.6432(5) 0.1667(4) 0.2074(3) 0.136(3) Uani 1 1 d . . . H25A H 0.6430 0.2087 0.1812 0.204 Uiso 1 1 calc R . . H25B H 0.6981 0.1467 0.2077 0.204 Uiso 1 1 calc R . . H25C H 0.6270 0.1783 0.2510 0.204 Uiso 1 1 calc R . . C26 C 0.5398(3) 0.0941(3) -0.0675(3) 0.0891(15) Uani 1 1 d . . . H26A H 0.4997 0.1314 -0.0572 0.107 Uiso 1 1 calc R . . C27 C 0.4901(4) 0.0292(3) -0.0892(3) 0.111(2) Uani 1 1 d . . . H27A H 0.4654 0.0382 -0.1308 0.166 Uiso 1 1 calc R . . H27B H 0.4472 0.0195 -0.0580 0.166 Uiso 1 1 calc R . . H27C H 0.5267 -0.0107 -0.0923 0.166 Uiso 1 1 calc R . . C28 C 0.5936(5) 0.1206(4) -0.1234(4) 0.127(2) Uani 1 1 d . . . H28A H 0.5588 0.1320 -0.1598 0.191 Uiso 1 1 calc R . . H28B H 0.6324 0.0844 -0.1357 0.191 Uiso 1 1 calc R . . H28C H 0.6236 0.1619 -0.1099 0.191 Uiso 1 1 calc R . . C29 C 0.2689(2) 0.0895(2) 0.0899(2) 0.0647(11) Uani 1 1 d . . . C30 C 0.2244(2) 0.0507(2) 0.0436(2) 0.0709(12) Uani 1 1 d . . . C31 C 0.1553(3) 0.0136(3) 0.0654(3) 0.0946(17) Uani 1 1 d . . . H31A H 0.1242 -0.0129 0.0362 0.114 Uiso 1 1 calc R . . C32 C 0.1324(3) 0.0155(3) 0.1295(3) 0.0998(18) Uani 1 1 d . . . H32A H 0.0859 -0.0097 0.1431 0.120 Uiso 1 1 calc R . . C33 C 0.1764(4) 0.0537(3) 0.1735(3) 0.0994(18) Uani 1 1 d . . . H33A H 0.1597 0.0539 0.2167 0.119 Uiso 1 1 calc R . . C34 C 0.2465(3) 0.0928(3) 0.1550(2) 0.0759(13) Uani 1 1 d . . . C35 C 0.2467(3) 0.0466(3) -0.0284(3) 0.0836(14) Uani 1 1 d . . . H35A H 0.2970 0.0749 -0.0352 0.100 Uiso 1 1 calc R . . C36 C 0.1808(4) 0.0751(4) -0.0718(3) 0.127(2) Uani 1 1 d . . . H36A H 0.1769 0.1253 -0.0662 0.191 Uiso 1 1 calc R . . H36B H 0.1284 0.0537 -0.0611 0.191 Uiso 1 1 calc R . . H36C H 0.1945 0.0647 -0.1162 0.191 Uiso 1 1 calc R . . C37 C 0.2669(4) -0.0303(3) -0.0484(3) 0.1074(19) Uani 1 1 d . . . H37A H 0.2951 -0.0303 -0.0896 0.161 Uiso 1 1 calc R . . H37B H 0.2161 -0.0567 -0.0520 0.161 Uiso 1 1 calc R . . H37C H 0.3019 -0.0515 -0.0162 0.161 Uiso 1 1 calc R . . C38 C 0.2932(4) 0.1349(3) 0.2050(3) 0.0954(17) Uani 1 1 d . . . H38A H 0.3398 0.1581 0.1828 0.115 Uiso 1 1 calc R . . C39 C 0.2401(5) 0.1920(4) 0.2347(3) 0.138(3) Uani 1 1 d . . . H39A H 0.2182 0.2216 0.2009 0.207 Uiso 1 1 calc R . . H39B H 0.2734 0.2200 0.2637 0.207 Uiso 1 1 calc R . . H39C H 0.1950 0.1710 0.2583 0.207 Uiso 1 1 calc R . . C40 C 0.3292(5) 0.0892(5) 0.2571(4) 0.150(3) Uani 1 1 d . . . H40A H 0.3681 0.0567 0.2382 0.225 Uiso 1 1 calc R . . H40B H 0.2853 0.0634 0.2780 0.225 Uiso 1 1 calc R . . H40C H 0.3573 0.1181 0.2884 0.225 Uiso 1 1 calc R . . C41 C 0.1256(3) 0.8009(2) 0.1301(2) 0.0659(11) Uani 1 1 d . . . C42 C 0.1241(3) 0.8160(2) 0.1962(2) 0.0738(12) Uani 1 1 d . . . C43 C 0.1866(5) 0.8497(3) 0.2284(3) 0.1019(19) Uani 1 1 d . . . C44 C 0.2567(4) 0.8706(3) 0.1961(4) 0.112(2) Uani 1 1 d . . . C45 C 0.2619(3) 0.8575(3) 0.1307(4) 0.0944(17) Uani 1 1 d . . . C46 C 0.1984(3) 0.8243(2) 0.0998(3) 0.0725(12) Uani 1 1 d . . . C47 C 0.0513(2) 0.7467(2) 0.01764(19) 0.0581(10) Uani 1 1 d . . . C48 C 0.0433(3) 0.8094(2) -0.0164(2) 0.0662(11) Uani 1 1 d . . . C49 C 0.0319(3) 0.8136(3) -0.0819(2) 0.0795(13) Uani 1 1 d . . . C50 C 0.0273(3) 0.7534(3) -0.1179(2) 0.0853(14) Uani 1 1 d . . . C51 C 0.0343(3) 0.6891(3) -0.0872(2) 0.0703(12) Uani 1 1 d . . . C52 C 0.0463(3) 0.6871(2) -0.0206(2) 0.0630(10) Uani 1 1 d . . . C53 C -0.0430(3) 0.7741(2) 0.11422(18) 0.0577(10) Uani 1 1 d . . . C54 C -0.1078(3) 0.7288(2) 0.10096(19) 0.0569(10) Uani 1 1 d . . . C55 C -0.1913(3) 0.7459(3) 0.1068(2) 0.0707(12) Uani 1 1 d . . . C56 C -0.2111(3) 0.8140(3) 0.1248(2) 0.0806(14) Uani 1 1 d . . . C57 C -0.1495(3) 0.8618(3) 0.1375(2) 0.0803(14) Uani 1 1 d . . . C58 C -0.0676(3) 0.8414(2) 0.1310(2) 0.0681(11) Uani 1 1 d . . . C59 C 0.0827(3) 0.6729(2) 0.13228(19) 0.0564(9) Uani 1 1 d . . . C60 C 0.0450(3) 0.6389(2) 0.1834(2) 0.0629(10) Uani 1 1 d . . . C61 C 0.0794(3) 0.5813(2) 0.2161(2) 0.0722(12) Uani 1 1 d . . . C62 C 0.1559(3) 0.5576(2) 0.1988(2) 0.0766(13) Uani 1 1 d . . . C63 C 0.1969(3) 0.5883(3) 0.1482(2) 0.0748(13) Uani 1 1 d . . . C64 C 0.1591(3) 0.6441(2) 0.1166(2) 0.0670(11) Uani 1 1 d . . . N1 N 0.4195(2) 0.25155(15) 0.04304(16) 0.0554(8) Uani 1 1 d . . . N2 N 0.48546(18) 0.13926(16) 0.05899(16) 0.0563(8) Uani 1 1 d . . . N3 N 0.3416(2) 0.13107(18) 0.06895(16) 0.0592(8) Uani 1 1 d . . . H1 H 0.248(2) 0.2538(18) 0.0621(16) 0.050 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0725(9) 0.0611(8) 0.1300(14) 0.0025(9) 0.0110(9) 0.0003(7) B1 0.065(3) 0.053(2) 0.058(3) 0.002(2) 0.003(2) -0.010(2) F1 0.114(2) 0.095(2) 0.0654(16) -0.0077(14) -0.0052(16) -0.0093(18) F2 0.197(4) 0.139(3) 0.113(3) -0.030(2) -0.064(3) -0.026(3) F3 0.142(3) 0.135(3) 0.210(5) -0.011(3) -0.091(3) -0.044(3) F4 0.084(2) 0.115(3) 0.194(4) 0.028(3) -0.012(2) -0.0378(19) F5 0.0867(19) 0.102(2) 0.099(2) 0.0179(18) 0.0096(16) -0.0279(16) F6 0.109(2) 0.0583(15) 0.0835(17) 0.0057(13) -0.0109(16) -0.0039(14) F7 0.166(3) 0.097(2) 0.088(2) 0.0331(18) -0.009(2) 0.009(2) F8 0.184(4) 0.136(3) 0.0595(17) 0.0078(17) -0.0171(19) 0.003(3) F9 0.110(2) 0.104(2) 0.0720(17) -0.0261(16) -0.0003(16) -0.0034(18) F10 0.105(2) 0.0557(14) 0.0741(15) -0.0060(12) 0.0040(14) 0.0010(13) F11 0.0789(16) 0.0633(15) 0.0856(17) -0.0158(13) 0.0003(13) -0.0154(12) F12 0.0712(16) 0.120(2) 0.099(2) -0.0172(18) -0.0051(15) -0.0245(17) F13 0.0670(19) 0.161(3) 0.143(3) -0.034(3) -0.0061(19) 0.026(2) F14 0.106(2) 0.089(2) 0.157(3) -0.040(2) -0.004(2) 0.0352(18) F15 0.0932(19) 0.0557(14) 0.122(2) -0.0203(15) -0.0032(16) -0.0020(14) F16 0.0901(18) 0.0831(17) 0.0674(15) 0.0052(13) 0.0131(14) 0.0034(14) F17 0.141(3) 0.089(2) 0.0743(17) 0.0229(15) 0.0160(18) -0.0037(19) F18 0.147(3) 0.0825(19) 0.092(2) 0.0153(16) -0.026(2) 0.0230(19) F19 0.081(2) 0.112(2) 0.114(2) 0.0050(19) -0.0077(17) 0.0283(17) F20 0.0745(16) 0.0873(18) 0.0948(19) 0.0128(15) 0.0113(15) 0.0062(14) C1 0.112(4) 0.0330(19) 0.065(3) 0.0205(18) 0.053(3) 0.034(2) C2 0.085(4) 0.056(3) 0.125(4) -0.007(3) -0.019(3) 0.008(3) C3 0.051(2) 0.049(2) 0.063(2) -0.0003(18) 0.0011(18) -0.0032(18) C4 0.077(3) 0.049(2) 0.112(4) 0.004(2) 0.011(3) -0.005(2) C5 0.061(2) 0.044(2) 0.065(2) 0.0035(18) -0.0062(19) 0.0008(18) C6 0.067(3) 0.052(2) 0.073(3) -0.007(2) -0.002(2) 0.003(2) C7 0.092(3) 0.043(2) 0.100(4) -0.014(2) -0.003(3) -0.002(2) C8 0.089(4) 0.044(2) 0.120(4) 0.006(3) -0.007(3) 0.001(2) C9 0.095(4) 0.072(3) 0.093(4) 0.024(3) -0.002(3) 0.012(3) C10 0.084(3) 0.061(3) 0.070(3) 0.004(2) -0.005(2) -0.002(2) C11 0.102(4) 0.074(3) 0.067(3) -0.014(2) 0.009(3) -0.006(3) C12 0.129(5) 0.152(6) 0.078(4) 0.002(4) -0.009(4) -0.006(5) C13 0.133(5) 0.107(5) 0.107(4) -0.029(4) 0.029(4) -0.021(4) C14 0.126(5) 0.077(3) 0.073(3) 0.001(3) -0.004(3) 0.012(3) C15 0.152(6) 0.134(6) 0.089(4) 0.001(4) -0.029(4) 0.006(5) C16 0.154(6) 0.104(4) 0.081(4) 0.008(3) 0.010(4) 0.003(4) C17 0.047(2) 0.066(3) 0.101(4) -0.011(3) 0.006(2) 0.001(2) C18 0.051(3) 0.087(3) 0.117(4) 0.005(3) -0.014(3) 0.009(2) C19 0.073(4) 0.115(5) 0.156(6) -0.020(4) -0.024(4) 0.029(3) C20 0.061(3) 0.121(5) 0.183(7) -0.050(5) -0.012(4) 0.026(3) C21 0.079(4) 0.111(5) 0.138(5) -0.049(4) 0.018(4) 0.019(3) C22 0.063(3) 0.076(3) 0.105(4) -0.023(3) 0.007(3) 0.003(2) C23 0.090(4) 0.156(6) 0.090(4) 0.012(4) -0.008(3) 0.035(4) C24 0.143(7) 0.203(9) 0.130(6) 0.061(6) -0.016(5) 0.015(6) C25 0.124(5) 0.171(7) 0.112(5) -0.037(5) -0.011(4) 0.002(5) C26 0.089(3) 0.079(3) 0.099(4) -0.026(3) 0.023(3) 0.010(3) C27 0.104(4) 0.125(5) 0.103(4) -0.027(4) 0.007(3) -0.024(4) C28 0.148(6) 0.100(5) 0.133(6) -0.021(4) 0.035(5) -0.022(4) C29 0.046(2) 0.065(3) 0.083(3) -0.006(2) 0.004(2) -0.0031(19) C30 0.046(2) 0.073(3) 0.094(3) -0.011(3) 0.000(2) 0.004(2) C31 0.063(3) 0.089(4) 0.131(5) -0.025(3) 0.000(3) -0.019(3) C32 0.064(3) 0.102(4) 0.134(5) -0.017(4) 0.024(3) -0.024(3) C33 0.088(4) 0.109(4) 0.101(4) -0.012(3) 0.032(3) -0.026(3) C34 0.056(2) 0.089(3) 0.083(3) -0.004(3) 0.014(2) -0.012(2) C35 0.065(3) 0.091(4) 0.094(4) -0.016(3) -0.012(3) -0.001(3) C36 0.110(5) 0.171(7) 0.100(4) -0.022(4) -0.026(4) 0.017(5) C37 0.127(5) 0.084(4) 0.111(4) -0.037(3) 0.006(4) -0.002(3) C38 0.094(4) 0.118(4) 0.074(3) -0.021(3) 0.019(3) -0.028(3) C39 0.149(6) 0.146(6) 0.118(5) -0.047(5) 0.029(5) -0.021(5) C40 0.163(7) 0.183(8) 0.104(5) -0.020(5) -0.034(5) -0.018(6) C41 0.065(3) 0.060(3) 0.073(3) 0.007(2) -0.007(2) -0.004(2) C42 0.078(3) 0.065(3) 0.078(3) -0.001(2) -0.012(3) -0.006(2) C43 0.120(5) 0.083(4) 0.103(5) -0.012(3) -0.043(4) -0.013(4) C44 0.111(5) 0.085(4) 0.140(6) 0.012(4) -0.072(5) -0.018(4) C45 0.066(3) 0.075(3) 0.143(6) 0.021(4) -0.023(4) -0.020(3) C46 0.073(3) 0.055(3) 0.089(4) 0.010(2) -0.004(3) -0.008(2) C47 0.052(2) 0.058(2) 0.064(2) 0.001(2) 0.0014(18) -0.0068(19) C48 0.071(3) 0.059(3) 0.068(3) 0.000(2) 0.001(2) -0.007(2) C49 0.088(3) 0.082(3) 0.068(3) 0.017(3) -0.009(2) -0.002(3) C50 0.101(4) 0.100(4) 0.055(3) 0.003(3) -0.003(3) -0.009(3) C51 0.069(3) 0.078(3) 0.064(3) -0.010(3) -0.003(2) -0.009(2) C52 0.059(2) 0.062(3) 0.068(3) -0.003(2) 0.001(2) -0.007(2) C53 0.067(3) 0.052(2) 0.053(2) 0.0008(18) 0.0009(19) -0.0067(19) C54 0.061(3) 0.055(2) 0.054(2) -0.0052(18) -0.0021(19) -0.0064(19) C55 0.070(3) 0.086(3) 0.056(2) -0.009(2) -0.004(2) -0.014(3) C56 0.058(3) 0.109(4) 0.075(3) -0.004(3) -0.001(2) 0.009(3) C57 0.076(3) 0.080(3) 0.085(3) -0.020(3) -0.015(3) 0.019(3) C58 0.073(3) 0.058(3) 0.074(3) -0.010(2) 0.004(2) -0.006(2) C59 0.061(2) 0.049(2) 0.059(2) -0.0071(18) 0.0013(19) -0.0030(18) C60 0.078(3) 0.055(2) 0.056(2) -0.008(2) -0.002(2) 0.001(2) C61 0.101(4) 0.060(3) 0.055(2) 0.001(2) -0.004(2) -0.004(3) C62 0.093(4) 0.062(3) 0.075(3) 0.000(2) -0.016(3) 0.012(3) C63 0.077(3) 0.068(3) 0.080(3) -0.005(2) -0.016(3) 0.008(3) C64 0.076(3) 0.063(3) 0.063(3) -0.003(2) -0.001(2) -0.008(2) N1 0.0624(19) 0.0376(15) 0.066(2) -0.0008(14) -0.0026(16) -0.0039(15) N2 0.0459(17) 0.0516(18) 0.071(2) -0.0041(16) 0.0023(15) -0.0023(14) N3 0.0487(18) 0.065(2) 0.064(2) -0.0043(17) 0.0033(15) 0.0018(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N3 1.881(4) . ? Al1 N1 1.888(4) . ? B1 C41 1.643(6) . ? B1 C47 1.658(6) . ? B1 C59 1.668(6) . ? B1 C53 1.670(6) . ? F1 C42 1.346(5) . ? F2 C43 1.371(7) . ? F3 C44 1.353(6) . ? F4 C45 1.333(7) . ? F5 C46 1.347(6) . ? F6 C48 1.354(5) . ? F7 C49 1.350(5) . ? F8 C50 1.346(5) . ? F9 C51 1.336(5) . ? F10 C52 1.348(5) . ? F11 C54 1.344(4) . ? F12 C55 1.320(5) . ? F13 C56 1.349(5) . ? F14 C57 1.340(6) . ? F15 C58 1.351(5) . ? F16 C60 1.357(5) . ? F17 C61 1.344(5) . ? F18 C62 1.345(5) . ? F19 C63 1.330(6) . ? F20 C64 1.364(5) . ? C1 C2 1.300(7) . ? C1 N1 1.405(5) . ? C1 N2 1.510(5) . ? C3 N3 1.313(5) . ? C3 N2 1.360(5) . ? C3 C4 1.485(6) . ? C5 C10 1.396(6) . ? C5 C6 1.407(6) . ? C5 N1 1.462(5) . ? C6 C7 1.386(6) . ? C6 C11 1.515(7) . ? C7 C8 1.359(7) . ? C8 C9 1.361(7) . ? C9 C10 1.397(7) . ? C10 C14 1.522(7) . ? C11 C13 1.523(8) . ? C11 C12 1.550(8) . ? C14 C15 1.531(8) . ? C14 C16 1.551(8) . ? C17 C22 1.390(7) . ? C17 C18 1.392(7) . ? C17 N2 1.472(5) . ? C18 C19 1.393(7) . ? C18 C23 1.508(8) . ? C19 C20 1.342(9) . ? C20 C21 1.411(10) . ? C21 C22 1.392(8) . ? C22 C26 1.522(8) . ? C23 C24 1.532(9) . ? C23 C25 1.538(9) . ? C26 C28 1.524(8) . ? C26 C27 1.532(8) . ? C29 C34 1.387(6) . ? C29 C30 1.399(6) . ? C29 N3 1.474(5) . ? C30 C31 1.388(7) . ? C30 C35 1.527(7) . ? C31 C32 1.370(8) . ? C32 C33 1.357(8) . ? C33 C34 1.402(7) . ? C34 C38 1.504(7) . ? C35 C36 1.487(8) . ? C35 C37 1.549(7) . ? C38 C40 1.494(9) . ? C38 C39 1.507(9) . ? C41 C42 1.391(6) . ? C41 C46 1.398(6) . ? C42 C43 1.362(7) . ? C43 C44 1.366(9) . ? C44 C45 1.371(9) . ? C45 C46 1.357(7) . ? C47 C52 1.378(6) . ? C47 C48 1.386(6) . ? C48 C49 1.363(6) . ? C49 C50 1.364(7) . ? C50 C51 1.376(7) . ? C51 C52 1.386(6) . ? C53 C54 1.377(5) . ? C53 C58 1.379(6) . ? C54 C55 1.385(6) . ? C55 C56 1.380(7) . ? C56 C57 1.366(7) . ? C57 C58 1.378(7) . ? C59 C60 1.374(6) . ? C59 C64 1.382(6) . ? C60 C61 1.397(6) . ? C61 C62 1.355(7) . ? C62 C63 1.363(7) . ? C63 C64 1.382(6) . ? 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 N3 Al1 N1 89.68(15) . . ? C41 B1 C47 116.0(3) . . ? C41 B1 C59 99.3(3) . . ? C47 B1 C59 114.0(3) . . ? C41 B1 C53 113.7(3) . . ? C47 B1 C53 100.2(3) . . ? C59 B1 C53 114.6(3) . . ? C2 C1 N1 126.4(4) . . ? C2 C1 N2 121.4(4) . . ? N1 C1 N2 110.7(4) . . ? N3 C3 N2 120.9(3) . . ? N3 C3 C4 120.4(4) . . ? N2 C3 C4 118.7(4) . . ? C10 C5 C6 122.7(4) . . ? C10 C5 N1 119.0(4) . . ? C6 C5 N1 118.3(4) . . ? C7 C6 C5 116.7(4) . . ? C7 C6 C11 119.7(4) . . ? C5 C6 C11 123.6(4) . . ? C8 C7 C6 121.8(5) . . ? C7 C8 C9 120.5(4) . . ? C8 C9 C10 121.7(5) . . ? C5 C10 C9 116.6(4) . . ? C5 C10 C14 123.4(4) . . ? C9 C10 C14 120.1(5) . . ? C6 C11 C13 112.3(5) . . ? C6 C11 C12 110.2(4) . . ? C13 C11 C12 111.0(4) . . ? C10 C14 C15 110.8(5) . . ? C10 C14 C16 111.4(5) . . ? C15 C14 C16 110.8(5) . . ? C22 C17 C18 125.2(4) . . ? C22 C17 N2 115.9(4) . . ? C18 C17 N2 119.0(4) . . ? C17 C18 C19 115.8(6) . . ? C17 C18 C23 124.2(4) . . ? C19 C18 C23 120.1(5) . . ? C20 C19 C18 121.9(6) . . ? C19 C20 C21 121.0(5) . . ? C22 C21 C20 120.0(6) . . ? C17 C22 C21 116.1(5) . . ? C17 C22 C26 123.7(4) . . ? C21 C22 C26 120.3(5) . . ? C18 C23 C24 112.0(6) . . ? C18 C23 C25 111.6(5) . . ? C24 C23 C25 107.3(6) . . ? C22 C26 C28 113.1(5) . . ? C22 C26 C27 111.3(5) . . ? C28 C26 C27 109.9(5) . . ? C34 C29 C30 123.3(4) . . ? C34 C29 N3 117.6(4) . . ? C30 C29 N3 119.0(4) . . ? C31 C30 C29 117.0(5) . . ? C31 C30 C35 118.4(5) . . ? C29 C30 C35 124.7(4) . . ? C32 C31 C30 120.9(5) . . ? C33 C32 C31 121.1(5) . . ? C32 C33 C34 121.3(5) . . ? C29 C34 C33 116.5(5) . . ? C29 C34 C38 123.8(4) . . ? C33 C34 C38 119.7(5) . . ? C36 C35 C30 113.4(5) . . ? C36 C35 C37 109.3(5) . . ? C30 C35 C37 110.9(5) . . ? C40 C38 C34 112.2(5) . . ? C40 C38 C39 110.2(6) . . ? C34 C38 C39 112.1(5) . . ? C42 C41 C46 112.7(4) . . ? C42 C41 B1 120.2(4) . . ? C46 C41 B1 126.3(4) . . ? F1 C42 C43 116.8(5) . . ? F1 C42 C41 119.1(4) . . ? C43 C42 C41 124.0(5) . . ? C42 C43 C44 120.5(6) . . ? C42 C43 F2 120.1(7) . . ? C44 C43 F2 119.4(6) . . ? F3 C44 C43 120.5(7) . . ? F3 C44 C45 121.2(7) . . ? C43 C44 C45 118.3(5) . . ? F4 C45 C46 121.3(6) . . ? F4 C45 C44 118.7(6) . . ? C46 C45 C44 119.9(6) . . ? F5 C46 C45 115.5(5) . . ? F5 C46 C41 119.9(4) . . ? C45 C46 C41 124.5(5) . . ? C52 C47 C48 114.1(4) . . ? C52 C47 B1 126.5(4) . . ? C48 C47 B1 119.0(4) . . ? F6 C48 C49 116.5(4) . . ? F6 C48 C47 119.3(4) . . ? C49 C48 C47 124.2(4) . . ? F7 C49 C48 120.2(5) . . ? F7 C49 C50 120.0(4) . . ? C48 C49 C50 119.8(5) . . ? F8 C50 C49 120.8(5) . . ? F8 C50 C51 120.0(5) . . ? C49 C50 C51 119.1(4) . . ? F9 C51 C50 119.9(4) . . ? F9 C51 C52 120.7(4) . . ? C50 C51 C52 119.3(4) . . ? F10 C52 C47 121.8(4) . . ? F10 C52 C51 114.7(4) . . ? C47 C52 C51 123.5(4) . . ? C54 C53 C58 114.1(4) . . ? C54 C53 B1 119.6(3) . . ? C58 C53 B1 125.6(4) . . ? F11 C54 C53 120.6(4) . . ? F11 C54 C55 114.6(4) . . ? C53 C54 C55 124.8(4) . . ? F12 C55 C56 120.2(4) . . ? F12 C55 C54 122.1(4) . . ? C56 C55 C54 117.7(4) . . ? F13 C56 C57 119.2(5) . . ? F13 C56 C55 120.4(5) . . ? C57 C56 C55 120.4(4) . . ? F14 C57 C56 120.4(5) . . ? F14 C57 C58 120.5(5) . . ? C56 C57 C58 119.1(4) . . ? F15 C58 C57 114.8(4) . . ? F15 C58 C53 121.2(4) . . ? C57 C58 C53 123.9(4) . . ? C60 C59 C64 112.7(4) . . ? C60 C59 B1 127.5(4) . . ? C64 C59 B1 118.9(4) . . ? F16 C60 C59 121.1(4) . . ? F16 C60 C61 114.7(4) . . ? C59 C60 C61 124.1(4) . . ? F17 C61 C62 120.5(4) . . ? F17 C61 C60 120.1(5) . . ? C62 C61 C60 119.4(4) . . ? F18 C62 C61 120.1(5) . . ? F18 C62 C63 120.0(5) . . ? C61 C62 C63 119.9(5) . . ? F19 C63 C62 120.5(4) . . ? F19 C63 C64 121.3(5) . . ? C62 C63 C64 118.2(5) . . ? F20 C64 C59 119.5(4) . . ? F20 C64 C63 114.9(4) . . ? C59 C64 C63 125.6(4) . . ? C1 N1 C5 114.9(3) . . ? C1 N1 Al1 134.5(3) . . ? C5 N1 Al1 110.5(2) . . ? C3 N2 C17 117.3(3) . . ? C3 N2 C1 129.9(3) . . ? C17 N2 C1 112.8(3) . . ? C3 N3 C29 118.4(3) . . ? C3 N3 Al1 131.0(3) . . ? C29 N3 Al1 110.5(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.284 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.039 #===end