# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H31 Al N2' _chemical_formula_sum 'C27 H31 Al N2' _chemical_formula_weight 410.52 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 Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 14.3480(3) _cell_length_b 18.1039(4) _cell_length_c 9.2139(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2393.35(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used 6709 _cell_measurement_theta_min 3.0482 _cell_measurement_theta_max 32.6037 _exptl_crystal_description tablets _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.139 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 0.100 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.971 _exptl_absorpt_correction_T_max 0.993 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 15.9825 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26614 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0174 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 32.68 _reflns_number_total 4247 _reflns_number_gt 3172 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0848P)^2^+0.4672P] 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_number_reflns 4247 _refine_ls_number_parameters 165 _refine_ls_number_restraints 96 _refine_ls_R_factor_all 0.0736 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1617 _refine_ls_wR_factor_gt 0.1480 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.045 _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 Al Al 0.60492(3) 0.2500 0.63878(5) 0.02969(14) Uani 1 2 d S . . H H 0.5435(13) 0.2500 0.775(2) 0.030(5) Uiso 1 2 d S . . C1 C 0.78568(8) 0.18096(7) 0.65116(12) 0.0328(2) Uani 1 1 d D A . N1 N 0.69315(7) 0.17191(5) 0.65245(11) 0.0329(2) Uani 1 1 d D . . C2 C 0.82802(11) 0.2500 0.64252(17) 0.0328(3) Uani 1 2 d S . . H2A H 0.8937 0.2500 0.6291 0.039 Uiso 1 2 calc SR A . C3 C 0.84878(10) 0.11496(8) 0.66455(18) 0.0510(4) Uani 1 1 d . . . H3A H 0.8415 0.0929 0.7611 0.076 Uiso 1 1 calc R A . H3B H 0.9136 0.1305 0.6510 0.076 Uiso 1 1 calc R . . H3C H 0.8323 0.0785 0.5903 0.076 Uiso 1 1 calc R . . C4 C 0.65553(10) 0.09797(6) 0.6701(2) 0.0363(4) Uani 0.784(6) 1 d PGDU A 1 C5 C 0.64101(10) 0.05194(7) 0.5514(2) 0.0432(5) Uani 0.784(6) 1 d PGDU A 1 C6 C 0.60268(11) -0.01783(6) 0.5714(3) 0.0604(8) Uani 0.784(6) 1 d PGDU A 1 H6A H 0.5928 -0.0493 0.4904 0.073 Uiso 0.784(6) 1 calc PR A 1 C7 C 0.57886(11) -0.04158(8) 0.7100(4) 0.0670(10) Uani 0.784(6) 1 d PGU A 1 H7A H 0.5527 -0.0893 0.7237 0.080 Uiso 0.784(6) 1 calc PR A 1 C8 C 0.59338(11) 0.00444(11) 0.8286(3) 0.0637(9) Uani 0.784(6) 1 d PGDU A 1 H8A H 0.5771 -0.0118 0.9233 0.076 Uiso 0.784(6) 1 calc PR A 1 C9 C 0.63172(11) 0.07422(10) 0.8086(2) 0.0475(5) Uani 0.784(6) 1 d PGDU A 1 C10 C 0.66697(18) 0.07610(13) 0.3981(3) 0.0492(5) Uani 0.784(6) 1 d PDU A 1 H10A H 0.6323 0.1210 0.3729 0.074 Uiso 0.784(6) 1 calc PR A 1 H10B H 0.6512 0.0367 0.3294 0.074 Uiso 0.784(6) 1 calc PR A 1 H10C H 0.7340 0.0862 0.3934 0.074 Uiso 0.784(6) 1 calc PR A 1 C11 C 0.6530(2) 0.1206(2) 0.9412(3) 0.0631(8) Uani 0.784(6) 1 d PDU A 1 H11A H 0.6327 0.0943 1.0286 0.095 Uiso 0.784(6) 1 calc PR A 1 H11B H 0.6199 0.1678 0.9342 0.095 Uiso 0.784(6) 1 calc PR A 1 H11C H 0.7202 0.1297 0.9466 0.095 Uiso 0.784(6) 1 calc PR A 1 C4' C 0.6591(5) 0.1024(3) 0.7054(6) 0.046(2) Uiso 0.216(6) 1 d PGDU A 2 C5' C 0.6349(6) 0.0505(4) 0.6009(6) 0.066(3) Uiso 0.216(6) 1 d PGDU A 2 C6' C 0.5916(5) -0.0150(3) 0.6419(8) 0.0505(19) Uiso 0.216(6) 1 d PGDU A 2 H6'A H 0.5751 -0.0505 0.5704 0.061 Uiso 0.216(6) 1 calc PR A 2 C7' C 0.5726(5) -0.0286(3) 0.7874(9) 0.059(2) Uiso 0.216(6) 1 d PGU A 2 H7'A H 0.5431 -0.0733 0.8154 0.070 Uiso 0.216(6) 1 calc PR A 2 C8' C 0.5969(4) 0.0233(3) 0.8919(7) 0.056(2) Uiso 0.216(6) 1 d PGDU A 2 H8'A H 0.5839 0.0141 0.9914 0.067 Uiso 0.216(6) 1 calc PR A 2 C9' C 0.6401(4) 0.0888(3) 0.8510(6) 0.0289(13) Uiso 0.216(6) 1 d PGDU A 2 C10' C 0.6546(7) 0.0654(6) 0.4440(10) 0.052(3) Uiso 0.216(6) 1 d PDU A 2 H10D H 0.7002 0.0295 0.4080 0.077 Uiso 0.216(6) 1 calc PR A 2 H10E H 0.6797 0.1154 0.4334 0.077 Uiso 0.216(6) 1 calc PR A 2 H10F H 0.5968 0.0610 0.3881 0.077 Uiso 0.216(6) 1 calc PR A 2 C11' C 0.6731(7) 0.1434(5) 0.9630(10) 0.049(2) Uiso 0.216(6) 1 d PDU A 2 H11D H 0.6283 0.1452 1.0432 0.074 Uiso 0.216(6) 1 calc PR A 2 H11E H 0.6784 0.1924 0.9187 0.074 Uiso 0.216(6) 1 calc PR A 2 H11F H 0.7341 0.1280 1.0001 0.074 Uiso 0.216(6) 1 calc PR A 2 C12 C 0.52611(11) 0.2500 0.46195(18) 0.0328(3) Uani 1 2 d S . . C13 C 0.55446(15) 0.2500 0.3159(2) 0.0436(4) Uani 1 2 d S A . H13A H 0.6192 0.2500 0.2946 0.052 Uiso 1 2 calc SR . . C14 C 0.49136(18) 0.2500 0.2016(2) 0.0506(5) Uani 1 2 d S . . H14A H 0.5135 0.2500 0.1044 0.061 Uiso 1 2 calc SR A . C15 C 0.39748(17) 0.2500 0.2282(2) 0.0533(5) Uani 1 2 d S A . H15A H 0.3546 0.2500 0.1497 0.064 Uiso 1 2 calc SR . . C16 C 0.36549(16) 0.2500 0.3689(2) 0.0521(5) Uani 1 2 d S . . H16A H 0.3004 0.2500 0.3882 0.063 Uiso 1 2 calc SR A . C17 C 0.42948(12) 0.2500 0.48360(19) 0.0406(4) Uani 1 2 d S A . H17A H 0.4064 0.2500 0.5802 0.049 Uiso 1 2 calc SR . . 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 Al 0.0239(2) 0.0342(2) 0.0309(2) 0.000 0.00229(16) 0.000 C1 0.0285(5) 0.0418(6) 0.0282(5) -0.0014(4) 0.0007(4) 0.0054(4) N1 0.0278(4) 0.0341(5) 0.0368(5) 0.0008(4) 0.0020(4) 0.0014(3) C2 0.0224(6) 0.0470(8) 0.0289(7) 0.000 0.0014(5) 0.000 C3 0.0371(7) 0.0495(7) 0.0663(9) -0.0059(6) -0.0047(6) 0.0131(6) C4 0.0278(7) 0.0319(8) 0.0493(11) 0.0068(7) -0.0009(7) 0.0025(5) C5 0.0346(8) 0.0296(7) 0.0655(15) -0.0014(7) -0.0086(8) 0.0029(5) C6 0.0482(11) 0.0361(9) 0.097(2) -0.0012(10) -0.0133(12) -0.0002(7) C7 0.0481(10) 0.0435(10) 0.110(3) 0.0279(14) -0.0086(12) -0.0055(8) C8 0.0444(11) 0.0597(14) 0.087(2) 0.0380(16) 0.0032(11) 0.0038(9) C9 0.0420(9) 0.0503(11) 0.0503(12) 0.0118(10) -0.0008(9) 0.0052(8) C10 0.0559(12) 0.0435(10) 0.0482(13) -0.0138(10) -0.0036(11) 0.0054(9) C11 0.0667(17) 0.0751(19) 0.0473(13) 0.0223(13) 0.0087(11) 0.0116(15) C12 0.0342(8) 0.0317(7) 0.0326(7) 0.000 0.0017(6) 0.000 C13 0.0467(10) 0.0441(9) 0.0401(9) 0.000 0.0101(8) 0.000 C14 0.0776(14) 0.0467(10) 0.0274(8) 0.000 0.0061(9) 0.000 C15 0.0663(14) 0.0598(12) 0.0338(9) 0.000 -0.0147(9) 0.000 C16 0.0413(10) 0.0762(14) 0.0388(10) 0.000 -0.0090(8) 0.000 C17 0.0358(8) 0.0585(10) 0.0276(7) 0.000 -0.0020(6) 0.000 _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 Al N1 1.9018(10) 7_565 ? Al N1 1.9018(10) . ? Al C12 1.9833(17) . ? C1 N1 1.3377(14) . ? C1 C2 1.3919(14) . ? C1 C3 1.5043(17) . ? N1 C4' 1.436(4) . ? N1 C4 1.4525(13) . ? C2 C1 1.3919(14) 7_565 ? C4 C5 1.3900 . ? C4 C9 1.3900 . ? C5 C6 1.3900 . ? C5 C10 1.525(3) . ? C6 C7 1.3900 . ? C7 C8 1.3900 . ? C8 C9 1.3900 . ? C9 C11 1.513(3) . ? C4' C5' 1.3900 . ? C4' C9' 1.3900 . ? C5' C6' 1.3900 . ? C5' C10' 1.497(8) . ? C6' C7' 1.3900 . ? C7' C8' 1.3900 . ? C8' C9' 1.3900 . ? C9' C11' 1.505(7) . ? C12 C17 1.401(2) . ? C12 C13 1.406(2) . ? C13 C14 1.389(3) . ? C14 C15 1.369(3) . ? C15 C16 1.376(3) . ? C16 C17 1.400(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 N1 Al N1 96.03(6) 7_565 . ? N1 Al C12 115.72(4) 7_565 . ? N1 Al C12 115.72(4) . . ? N1 C1 C2 122.93(11) . . ? N1 C1 C3 119.95(11) . . ? C2 C1 C3 117.08(11) . . ? C1 N1 C4' 116.6(3) . . ? C1 N1 C4 118.86(11) . . ? C1 N1 Al 124.68(8) . . ? C4' N1 Al 116.6(3) . . ? C4 N1 Al 116.43(8) . . ? C1 C2 C1 127.77(14) 7_565 . ? C5 C4 C9 120.0 . . ? C5 C4 N1 121.36(10) . . ? C9 C4 N1 118.62(10) . . ? C6 C5 C4 120.0 . . ? C6 C5 C10 118.67(11) . . ? C4 C5 C10 121.33(11) . . ? C7 C6 C5 120.0 . . ? C8 C7 C6 120.0 . . ? C7 C8 C9 120.0 . . ? C8 C9 C4 120.0 . . ? C8 C9 C11 118.51(13) . . ? C4 C9 C11 121.34(13) . . ? C5' C4' C9' 120.0 . . ? C5' C4' N1 116.2(3) . . ? C9' C4' N1 123.3(3) . . ? C4' C5' C6' 120.0 . . ? C4' C5' C10' 120.0(5) . . ? C6' C5' C10' 120.0(5) . . ? C7' C6' C5' 120.0 . . ? C8' C7' C6' 120.0 . . ? C7' C8' C9' 120.0 . . ? C8' C9' C4' 120.0 . . ? C8' C9' C11' 120.9(4) . . ? C4' C9' C11' 118.9(4) . . ? C17 C12 C13 115.01(16) . . ? C17 C12 Al 116.58(12) . . ? C13 C12 Al 128.42(13) . . ? C14 C13 C12 122.49(18) . . ? C15 C14 C13 120.39(18) . . ? C14 C15 C16 119.79(19) . . ? C15 C16 C17 119.5(2) . . ? C16 C17 C12 122.80(17) . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 31.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.323 _refine_diff_density_min -0.217 _refine_diff_density_rms 0.046 #===END _database_code_depnum_ccdc_archive 'CCDC 953189' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H36 Al N3' _chemical_formula_sum 'C21 H36 Al N3' _chemical_formula_weight 357.51 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 P2(1)/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 18.9383(3) _cell_length_b 13.30838(15) _cell_length_c 18.4372(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.8573(16) _cell_angle_gamma 90.00 _cell_volume 4342.37(11) _cell_formula_units_Z 8 _cell_measurement_temperature 173 _cell_measurement_reflns_used 15414 _cell_measurement_theta_min 2.9696 _cell_measurement_theta_max 32.6582 _exptl_crystal_description blocks _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.094 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 0.102 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.967 _exptl_absorpt_correction_T_max 0.979 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 15.9825 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47993 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0259 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 32.73 _reflns_number_total 14624 _reflns_number_gt 11545 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0675P)^2^+0.9533P] 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_number_reflns 14624 _refine_ls_number_parameters 471 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1326 _refine_ls_wR_factor_gt 0.1233 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 Al1A Al 0.438532(17) 0.43224(2) 0.117049(16) 0.01666(7) Uani 1 1 d . . . H1AA H 0.5197(8) 0.3920(11) 0.1358(8) 0.031(4) Uiso 1 1 d . . . H1AB H 0.3866(8) 0.3843(11) 0.1535(8) 0.031(4) Uiso 1 1 d . . . N1A N 0.46433(5) 0.55027(6) 0.18988(5) 0.01802(15) Uani 1 1 d . . . C2A C 0.44784(6) 0.64575(8) 0.17128(6) 0.02130(19) Uani 1 1 d . . . C3A C 0.40809(6) 0.67699(8) 0.09430(6) 0.0234(2) Uani 1 1 d . . . H3AA H 0.3947 0.7461 0.0873 0.028 Uiso 1 1 calc R . . C4A C 0.38638(6) 0.61850(7) 0.02779(6) 0.01958(18) Uani 1 1 d . . . N5A N 0.39979(5) 0.51946(6) 0.02723(5) 0.01823(15) Uani 1 1 d . . . C6A C 0.38125(7) 0.47192(8) -0.04959(6) 0.0246(2) Uani 1 1 d . . . H6AA H 0.4007 0.5135 -0.0829 0.029 Uiso 1 1 calc R . . H6AB H 0.3258 0.4661 -0.0752 0.029 Uiso 1 1 calc R . . C7A C 0.41705(6) 0.36869(8) -0.03869(6) 0.0240(2) Uani 1 1 d . . . H7AA H 0.3951 0.3291 -0.0870 0.029 Uiso 1 1 calc R . . H7AB H 0.4721 0.3750 -0.0270 0.029 Uiso 1 1 calc R . . N8A N 0.40332(5) 0.31726(6) 0.02558(5) 0.01953(16) Uani 1 1 d . . . C9A C 0.50015(6) 0.52324(7) 0.27071(5) 0.01795(17) Uani 1 1 d . . . C10A C 0.57922(6) 0.51351(8) 0.30353(6) 0.02027(18) Uani 1 1 d . . . C11A C 0.61157(7) 0.48220(8) 0.38078(6) 0.0252(2) Uani 1 1 d . . . H11A H 0.6649 0.4752 0.4036 0.030 Uiso 1 1 calc R . . C12A C 0.56739(7) 0.46122(9) 0.42455(6) 0.0271(2) Uani 1 1 d . . . H12A H 0.5902 0.4396 0.4768 0.033 Uiso 1 1 calc R . . C13A C 0.48972(7) 0.47184(8) 0.39187(6) 0.0263(2) Uani 1 1 d . . . H13A H 0.4598 0.4581 0.4225 0.032 Uiso 1 1 calc R . . C14A C 0.45429(6) 0.50243(8) 0.31467(6) 0.02119(19) Uani 1 1 d . . . C15A C 0.63087(6) 0.53799(9) 0.25907(6) 0.0267(2) Uani 1 1 d . . . H15A H 0.5985 0.5540 0.2043 0.032 Uiso 1 1 calc R . . C16A C 0.68146(7) 0.44867(11) 0.25746(8) 0.0360(3) Uani 1 1 d . . . H16A H 0.6499 0.3902 0.2348 0.054 Uiso 1 1 calc R . . H16B H 0.7149 0.4328 0.3105 0.054 Uiso 1 1 calc R . . H16C H 0.7120 0.4659 0.2260 0.054 Uiso 1 1 calc R . . C17A C 0.67989(9) 0.63063(12) 0.29354(10) 0.0461(3) Uani 1 1 d . . . H17A H 0.6472 0.6874 0.2944 0.069 Uiso 1 1 calc R . . H17B H 0.7099 0.6478 0.2616 0.069 Uiso 1 1 calc R . . H17C H 0.7137 0.6157 0.3466 0.069 Uiso 1 1 calc R . . C18A C 0.36880(7) 0.51325(10) 0.28250(7) 0.0287(2) Uani 1 1 d . . . H18A H 0.3530 0.5258 0.2254 0.034 Uiso 1 1 calc R . . C19A C 0.32922(9) 0.41757(12) 0.29387(9) 0.0448(3) Uani 1 1 d . . . H19A H 0.3461 0.3605 0.2706 0.067 Uiso 1 1 calc R . . H19B H 0.2744 0.4256 0.2688 0.067 Uiso 1 1 calc R . . H19C H 0.3418 0.4054 0.3495 0.067 Uiso 1 1 calc R . . C20A C 0.34223(9) 0.60286(13) 0.31858(9) 0.0462(3) Uani 1 1 d . . . H20A H 0.3673 0.6642 0.3108 0.069 Uiso 1 1 calc R . . H20B H 0.3550 0.5911 0.3743 0.069 Uiso 1 1 calc R . . H20C H 0.2874 0.6105 0.2937 0.069 Uiso 1 1 calc R . . C21A C 0.47186(9) 0.72804(9) 0.23107(7) 0.0354(3) Uani 1 1 d . . . H21A H 0.4653 0.7054 0.2789 0.053 Uiso 1 1 calc R . . H21B H 0.4408 0.7879 0.2112 0.053 Uiso 1 1 calc R . . H21C H 0.5251 0.7444 0.2420 0.053 Uiso 1 1 calc R . . C22A C 0.34709(7) 0.67297(9) -0.04799(6) 0.0288(2) Uani 1 1 d . . . H22A H 0.3785 0.6696 -0.0803 0.043 Uiso 1 1 calc R . . H22B H 0.3393 0.7434 -0.0374 0.043 Uiso 1 1 calc R . . H22C H 0.2981 0.6412 -0.0754 0.043 Uiso 1 1 calc R . . C23A C 0.44730(8) 0.22353(9) 0.04542(7) 0.0333(3) Uani 1 1 d . . . H23A H 0.4284 0.1761 0.0021 0.050 Uiso 1 1 calc R . . H23B H 0.4421 0.1940 0.0919 0.050 Uiso 1 1 calc R . . H23C H 0.5007 0.2381 0.0554 0.050 Uiso 1 1 calc R . . C24A C 0.32281(7) 0.29285(10) 0.00476(7) 0.0317(2) Uani 1 1 d . . . H24A H 0.3085 0.2414 -0.0360 0.048 Uiso 1 1 calc R . . H24B H 0.2925 0.3535 -0.0143 0.048 Uiso 1 1 calc R . . H24C H 0.3138 0.2674 0.0506 0.048 Uiso 1 1 calc R . . Al1B Al 0.075458(19) 0.43619(2) 0.161961(19) 0.02164(7) Uani 1 1 d . . . H1BA H 0.1148(9) 0.3664(13) 0.2283(9) 0.043(4) Uiso 1 1 d . . . H1BB H -0.0084(9) 0.4241(12) 0.1129(9) 0.041(4) Uiso 1 1 d . . . N1B N 0.06104(5) 0.55255(6) 0.22441(5) 0.01961(16) Uani 1 1 d . . . C2B C 0.07621(6) 0.64780(8) 0.21587(6) 0.0242(2) Uani 1 1 d . . . C3B C 0.11722(7) 0.67685(9) 0.16860(7) 0.0297(2) Uani 1 1 d . . . H3BA H 0.1229 0.7470 0.1630 0.036 Uiso 1 1 calc R . . C4B C 0.15020(7) 0.61440(10) 0.12933(7) 0.0297(2) Uani 1 1 d . . . N5B N 0.14320(6) 0.51437(8) 0.12663(6) 0.0277(2) Uani 1 1 d . . . C6B C 0.18518(9) 0.45821(12) 0.08589(10) 0.0452(3) Uani 1 1 d . . . H6BA H 0.2395 0.4756 0.1081 0.054 Uiso 1 1 calc R . . H6BB H 0.1661 0.4764 0.0302 0.054 Uiso 1 1 calc R . . C7B C 0.17479(8) 0.34672(11) 0.09497(9) 0.0389(3) Uani 1 1 d . . . H7BA H 0.1896 0.3088 0.0564 0.047 Uiso 1 1 calc R . . H7BB H 0.2074 0.3246 0.1475 0.047 Uiso 1 1 calc R . . N8B N 0.09543(6) 0.32658(7) 0.08336(5) 0.02671(19) Uani 1 1 d . . . C9B C 0.02560(6) 0.52618(7) 0.27909(6) 0.01917(17) Uani 1 1 d . . . C10B C 0.07177(6) 0.50225(8) 0.35589(6) 0.02299(19) Uani 1 1 d . . . C11B C 0.03719(7) 0.47000(9) 0.40724(6) 0.0286(2) Uani 1 1 d . . . H11B H 0.0677 0.4534 0.4591 0.034 Uiso 1 1 calc R . . C12B C -0.04054(7) 0.46176(9) 0.38421(7) 0.0298(2) Uani 1 1 d . . . H12B H -0.0630 0.4388 0.4197 0.036 Uiso 1 1 calc R . . C13B C -0.08537(6) 0.48722(9) 0.30894(7) 0.0260(2) Uani 1 1 d . . . H13B H -0.1388 0.4827 0.2936 0.031 Uiso 1 1 calc R . . C14B C -0.05365(6) 0.51938(8) 0.25511(6) 0.02030(18) Uani 1 1 d . . . C15B C 0.15719(7) 0.51411(10) 0.38451(7) 0.0315(2) Uani 1 1 d . . . H15B H 0.1717 0.5294 0.3386 0.038 Uiso 1 1 calc R . . C16B C 0.19898(9) 0.41968(12) 0.42281(10) 0.0492(4) Uani 1 1 d . . . H16D H 0.1833 0.3634 0.3863 0.074 Uiso 1 1 calc R . . H16E H 0.1871 0.4045 0.4692 0.074 Uiso 1 1 calc R . . H16F H 0.2535 0.4303 0.4376 0.074 Uiso 1 1 calc R . . C17B C 0.18313(10) 0.60217(14) 0.44155(13) 0.0662(6) Uani 1 1 d . . . H17D H 0.1570 0.6636 0.4169 0.099 Uiso 1 1 calc R . . H17E H 0.2378 0.6114 0.4562 0.099 Uiso 1 1 calc R . . H17F H 0.1712 0.5878 0.4880 0.099 Uiso 1 1 calc R . . C18B C -0.10525(6) 0.54870(8) 0.17381(6) 0.0242(2) Uani 1 1 d . . . H18B H -0.0729 0.5646 0.1427 0.029 Uiso 1 1 calc R . . C19B C -0.15834(7) 0.46279(10) 0.13342(7) 0.0310(2) Uani 1 1 d . . . H19D H -0.1906 0.4841 0.0813 0.046 Uiso 1 1 calc R . . H19E H -0.1899 0.4449 0.1636 0.046 Uiso 1 1 calc R . . H19F H -0.1285 0.4043 0.1295 0.046 Uiso 1 1 calc R . . C20B C -0.15155(9) 0.64251(11) 0.17531(8) 0.0437(3) Uani 1 1 d . . . H20D H -0.1174 0.6975 0.2010 0.066 Uiso 1 1 calc R . . H20E H -0.1852 0.6278 0.2039 0.066 Uiso 1 1 calc R . . H20F H -0.1817 0.6622 0.1220 0.066 Uiso 1 1 calc R . . C21B C 0.05088(9) 0.73086(9) 0.25627(9) 0.0403(3) Uani 1 1 d . . . H21D H 0.0082 0.7665 0.2186 0.060 Uiso 1 1 calc R . . H21E H 0.0927 0.7779 0.2793 0.060 Uiso 1 1 calc R . . H21F H 0.0352 0.7023 0.2972 0.060 Uiso 1 1 calc R . . C22B C 0.19700(10) 0.66504(13) 0.08804(10) 0.0507(4) Uani 1 1 d . . . H22D H 0.2492 0.6409 0.1099 0.076 Uiso 1 1 calc R . . H22E H 0.1961 0.7380 0.0950 0.076 Uiso 1 1 calc R . . H22F H 0.1759 0.6490 0.0326 0.076 Uiso 1 1 calc R . . C23B C 0.08619(10) 0.22256(10) 0.10477(9) 0.0445(3) Uani 1 1 d . . . H23D H 0.0958 0.1765 0.0678 0.067 Uiso 1 1 calc R . . H23E H 0.0345 0.2128 0.1036 0.067 Uiso 1 1 calc R . . H23F H 0.1221 0.2089 0.1572 0.067 Uiso 1 1 calc R . . C24B C 0.04626(9) 0.34381(13) 0.00224(8) 0.0455(3) Uani 1 1 d . . . H24D H 0.0570 0.2933 -0.0311 0.068 Uiso 1 1 calc R . . H24E H 0.0558 0.4110 -0.0140 0.068 Uiso 1 1 calc R . . H24F H -0.0067 0.3386 -0.0022 0.068 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 Al1A 0.02033(14) 0.01532(13) 0.01410(13) 0.00029(10) 0.00585(10) 0.00010(10) N1A 0.0227(4) 0.0169(4) 0.0140(3) -0.0002(3) 0.0061(3) 0.0000(3) C2A 0.0278(5) 0.0175(4) 0.0184(4) -0.0018(3) 0.0079(4) 0.0002(4) C3A 0.0315(5) 0.0161(4) 0.0211(4) 0.0015(3) 0.0073(4) 0.0032(4) C4A 0.0202(4) 0.0193(4) 0.0185(4) 0.0036(3) 0.0059(3) 0.0005(3) N5A 0.0229(4) 0.0174(4) 0.0137(3) 0.0003(3) 0.0057(3) -0.0012(3) C6A 0.0354(6) 0.0218(5) 0.0147(4) -0.0003(3) 0.0067(4) -0.0023(4) C7A 0.0316(5) 0.0242(5) 0.0189(4) -0.0033(4) 0.0125(4) -0.0023(4) N8A 0.0221(4) 0.0176(4) 0.0182(4) -0.0006(3) 0.0065(3) -0.0008(3) C9A 0.0251(4) 0.0150(4) 0.0136(4) -0.0017(3) 0.0067(3) -0.0012(3) C10A 0.0248(5) 0.0189(4) 0.0165(4) -0.0018(3) 0.0067(4) -0.0005(4) C11A 0.0288(5) 0.0256(5) 0.0182(4) -0.0003(4) 0.0046(4) 0.0038(4) C12A 0.0390(6) 0.0258(5) 0.0151(4) 0.0027(4) 0.0078(4) 0.0046(4) C13A 0.0396(6) 0.0243(5) 0.0191(4) 0.0002(4) 0.0156(4) -0.0011(4) C14A 0.0277(5) 0.0197(4) 0.0181(4) -0.0026(3) 0.0106(4) -0.0012(4) C15A 0.0247(5) 0.0340(6) 0.0220(5) -0.0016(4) 0.0090(4) -0.0035(4) C16A 0.0272(5) 0.0493(8) 0.0330(6) -0.0057(5) 0.0126(5) 0.0030(5) C17A 0.0478(8) 0.0432(8) 0.0545(8) -0.0079(7) 0.0269(7) -0.0180(7) C18A 0.0274(5) 0.0376(6) 0.0238(5) -0.0056(4) 0.0124(4) -0.0014(5) C19A 0.0394(7) 0.0532(9) 0.0487(8) -0.0095(7) 0.0242(6) -0.0159(6) C20A 0.0389(7) 0.0510(9) 0.0498(8) -0.0103(7) 0.0172(6) 0.0110(6) C21A 0.0584(8) 0.0192(5) 0.0234(5) -0.0057(4) 0.0079(5) 0.0013(5) C22A 0.0342(6) 0.0240(5) 0.0214(5) 0.0061(4) 0.0017(4) 0.0005(4) C23A 0.0455(7) 0.0205(5) 0.0286(5) -0.0025(4) 0.0069(5) 0.0076(5) C24A 0.0288(5) 0.0325(6) 0.0321(6) -0.0035(5) 0.0088(5) -0.0115(5) Al1B 0.02552(16) 0.02074(15) 0.02191(15) 0.00092(11) 0.01243(12) 0.00108(12) N1B 0.0208(4) 0.0196(4) 0.0191(4) 0.0018(3) 0.0079(3) 0.0001(3) C2B 0.0267(5) 0.0212(5) 0.0238(5) 0.0010(4) 0.0077(4) -0.0013(4) C3B 0.0351(6) 0.0242(5) 0.0314(6) 0.0054(4) 0.0138(5) -0.0051(4) C4B 0.0296(5) 0.0339(6) 0.0276(5) 0.0057(4) 0.0127(4) -0.0051(5) N5B 0.0279(5) 0.0324(5) 0.0279(4) 0.0006(4) 0.0161(4) -0.0012(4) C6B 0.0468(8) 0.0479(8) 0.0571(9) -0.0106(7) 0.0383(7) -0.0076(6) C7B 0.0344(6) 0.0436(7) 0.0446(7) -0.0072(6) 0.0214(6) 0.0068(5) N8B 0.0307(5) 0.0290(5) 0.0221(4) -0.0001(3) 0.0115(4) 0.0038(4) C9B 0.0235(4) 0.0164(4) 0.0187(4) -0.0002(3) 0.0088(3) 0.0012(3) C10B 0.0261(5) 0.0221(5) 0.0194(4) 0.0006(4) 0.0064(4) 0.0022(4) C11B 0.0379(6) 0.0297(5) 0.0185(4) 0.0028(4) 0.0103(4) 0.0025(5) C12B 0.0393(6) 0.0316(6) 0.0244(5) 0.0006(4) 0.0184(5) -0.0025(5) C13B 0.0259(5) 0.0286(5) 0.0267(5) -0.0025(4) 0.0132(4) -0.0022(4) C14B 0.0230(4) 0.0192(4) 0.0195(4) -0.0009(3) 0.0085(4) 0.0009(3) C15B 0.0259(5) 0.0379(6) 0.0265(5) 0.0038(5) 0.0042(4) 0.0032(5) C16B 0.0368(7) 0.0446(8) 0.0548(9) 0.0041(7) 0.0022(6) 0.0127(6) C17B 0.0408(8) 0.0437(9) 0.0907(14) -0.0182(9) -0.0054(9) -0.0058(7) C18B 0.0219(4) 0.0272(5) 0.0224(5) 0.0008(4) 0.0063(4) 0.0026(4) C19B 0.0265(5) 0.0401(6) 0.0247(5) -0.0044(5) 0.0071(4) -0.0041(5) C20B 0.0435(7) 0.0383(7) 0.0378(7) -0.0020(6) 0.0006(6) 0.0174(6) C21B 0.0609(9) 0.0199(5) 0.0500(8) -0.0039(5) 0.0319(7) -0.0026(5) C22B 0.0620(10) 0.0475(8) 0.0590(9) 0.0064(7) 0.0415(8) -0.0136(7) C23B 0.0718(10) 0.0278(6) 0.0449(7) -0.0036(5) 0.0340(7) 0.0019(6) C24B 0.0513(8) 0.0543(9) 0.0250(6) -0.0038(6) 0.0066(6) 0.0104(7) _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 Al1A N5A 1.9398(8) . ? Al1A N1A 2.0104(9) . ? Al1A N8A 2.1976(9) . ? N1A C2A 1.3242(13) . ? N1A C9A 1.4459(12) . ? C2A C3A 1.4117(14) . ? C2A C21A 1.5047(15) . ? C3A C4A 1.3855(14) . ? C4A N5A 1.3431(13) . ? C4A C22A 1.5135(14) . ? N5A C6A 1.4749(12) . ? C6A C7A 1.5134(15) . ? C7A N8A 1.4696(13) . ? N8A C24A 1.4700(14) . ? N8A C23A 1.4718(14) . ? C9A C10A 1.4071(14) . ? C9A C14A 1.4104(13) . ? C10A C11A 1.3986(14) . ? C10A C15A 1.5186(15) . ? C11A C12A 1.3821(16) . ? C12A C13A 1.3840(17) . ? C13A C14A 1.4005(14) . ? C14A C18A 1.5199(16) . ? C15A C16A 1.5336(18) . ? C15A C17A 1.5380(18) . ? C18A C19A 1.5295(19) . ? C18A C20A 1.5349(18) . ? Al1B N5B 1.9359(10) . ? Al1B N1B 2.0055(9) . ? Al1B N8B 2.1821(10) . ? N1B C2B 1.3215(13) . ? N1B C9B 1.4393(13) . ? C2B C3B 1.4121(15) . ? C2B C21B 1.5038(16) . ? C3B C4B 1.3883(18) . ? C4B N5B 1.3370(16) . ? C4B C22B 1.5163(17) . ? N5B C6B 1.4765(16) . ? C6B C7B 1.514(2) . ? C7B N8B 1.4654(16) . ? N8B C23B 1.4670(17) . ? N8B C24B 1.4713(16) . ? C9B C14B 1.4084(14) . ? C9B C10B 1.4105(14) . ? C10B C11B 1.3967(15) . ? C10B C15B 1.5206(16) . ? C11B C12B 1.3836(18) . ? C12B C13B 1.3867(16) . ? C13B C14B 1.3975(14) . ? C14B C18B 1.5202(14) . ? C15B C16B 1.5187(19) . ? C15B C17B 1.534(2) . ? C18B C19B 1.5296(16) . ? C18B C20B 1.5315(17) . ? 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 N5A Al1A N1A 91.76(4) . . ? N5A Al1A N8A 80.93(3) . . ? N1A Al1A N8A 172.64(4) . . ? C2A N1A C9A 119.11(8) . . ? C2A N1A Al1A 126.72(7) . . ? C9A N1A Al1A 114.04(6) . . ? N1A C2A C3A 122.35(9) . . ? N1A C2A C21A 121.79(9) . . ? C3A C2A C21A 115.85(9) . . ? C4A C3A C2A 127.47(9) . . ? N5A C4A C3A 124.11(9) . . ? N5A C4A C22A 119.67(9) . . ? C3A C4A C22A 116.19(9) . . ? C4A N5A C6A 116.57(8) . . ? C4A N5A Al1A 126.57(7) . . ? C6A N5A Al1A 116.84(7) . . ? N5A C6A C7A 108.64(8) . . ? N8A C7A C6A 109.29(8) . . ? C7A N8A C24A 110.93(9) . . ? C7A N8A C23A 110.38(9) . . ? C24A N8A C23A 108.68(9) . . ? C7A N8A Al1A 101.65(6) . . ? C24A N8A Al1A 110.94(7) . . ? C23A N8A Al1A 114.15(7) . . ? C10A C9A C14A 120.90(9) . . ? C10A C9A N1A 120.20(8) . . ? C14A C9A N1A 118.83(9) . . ? C11A C10A C9A 118.59(9) . . ? C11A C10A C15A 118.74(10) . . ? C9A C10A C15A 122.65(9) . . ? C12A C11A C10A 121.20(10) . . ? C11A C12A C13A 119.71(10) . . ? C12A C13A C14A 121.50(10) . . ? C13A C14A C9A 118.09(10) . . ? C13A C14A C18A 118.85(9) . . ? C9A C14A C18A 123.05(9) . . ? C10A C15A C16A 111.78(10) . . ? C10A C15A C17A 111.04(10) . . ? C16A C15A C17A 109.88(11) . . ? C14A C18A C19A 111.94(11) . . ? C14A C18A C20A 111.87(10) . . ? C19A C18A C20A 109.58(11) . . ? N5B Al1B N1B 91.16(4) . . ? N5B Al1B N8B 81.00(4) . . ? N1B Al1B N8B 171.38(4) . . ? C2B N1B C9B 119.52(9) . . ? C2B N1B Al1B 126.32(7) . . ? C9B N1B Al1B 113.99(6) . . ? N1B C2B C3B 121.80(10) . . ? N1B C2B C21B 121.66(10) . . ? C3B C2B C21B 116.54(10) . . ? C4B C3B C2B 127.33(11) . . ? N5B C4B C3B 123.94(10) . . ? N5B C4B C22B 119.46(12) . . ? C3B C4B C22B 116.60(12) . . ? C4B N5B C6B 117.30(10) . . ? C4B N5B Al1B 126.26(8) . . ? C6B N5B Al1B 116.13(8) . . ? N5B C6B C7B 108.98(10) . . ? N8B C7B C6B 109.27(11) . . ? C7B N8B C23B 110.35(11) . . ? C7B N8B C24B 111.40(11) . . ? C23B N8B C24B 109.12(11) . . ? C7B N8B Al1B 101.07(7) . . ? C23B N8B Al1B 112.75(7) . . ? C24B N8B Al1B 111.98(8) . . ? C14B C9B C10B 120.74(9) . . ? C14B C9B N1B 120.42(9) . . ? C10B C9B N1B 118.76(9) . . ? C11B C10B C9B 118.50(10) . . ? C11B C10B C15B 119.62(10) . . ? C9B C10B C15B 121.85(10) . . ? C12B C11B C10B 121.39(10) . . ? C11B C12B C13B 119.55(10) . . ? C12B C13B C14B 121.38(10) . . ? C13B C14B C9B 118.44(9) . . ? C13B C14B C18B 119.40(9) . . ? C9B C14B C18B 122.14(9) . . ? C16B C15B C10B 112.92(11) . . ? C16B C15B C17B 109.07(12) . . ? C10B C15B C17B 111.02(11) . . ? C14B C18B C19B 111.63(9) . . ? C14B C18B C20B 111.26(9) . . ? C19B C18B C20B 109.68(10) . . ? _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.385 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.049 _database_code_depnum_ccdc_archive 'CCDC 954263' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H36 Al N3' _chemical_formula_sum 'C23 H36 Al N3' _chemical_formula_weight 381.53 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2933(4) _cell_length_b 10.1234(4) _cell_length_c 14.4114(5) _cell_angle_alpha 103.226(3) _cell_angle_beta 103.546(3) _cell_angle_gamma 94.966(3) _cell_volume 1132.45(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 4757 _cell_measurement_theta_min 3.3267 _cell_measurement_theta_max 32.6457 _exptl_crystal_description blocks _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.119 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 416 _exptl_absorpt_coefficient_mu 0.102 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.962 _exptl_absorpt_correction_T_max 0.988 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 15.9825 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12644 _diffrn_reflns_av_R_equivalents 0.0166 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 32.72 _reflns_number_total 7386 _reflns_number_gt 5995 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0713P)^2^+0.1873P] 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_number_reflns 7386 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0571 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1352 _refine_ls_wR_factor_gt 0.1281 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 Al Al 0.46190(4) 0.46753(3) 0.20567(2) 0.02195(9) Uani 1 1 d . . . H H 0.5870(19) 0.3983(15) 0.1563(11) 0.033(4) Uiso 1 1 d . . . N1 N 0.48295(12) 0.65320(9) 0.24150(7) 0.02311(17) Uani 1 1 d . . . C2 C 0.41737(16) 0.69503(11) 0.32890(9) 0.0296(2) Uani 1 1 d . . . H2A H 0.2975 0.7049 0.3079 0.036 Uiso 1 1 calc R . . H2B H 0.4799 0.7846 0.3712 0.036 Uiso 1 1 calc R . . C3 C 0.43741(16) 0.58602(11) 0.38647(8) 0.0287(2) Uani 1 1 d . . . H3A H 0.5541 0.5988 0.4278 0.034 Uiso 1 1 calc R . . H3B H 0.3612 0.5937 0.4304 0.034 Uiso 1 1 calc R . . N4 N 0.39640(12) 0.44947(9) 0.31489(6) 0.02288(17) Uani 1 1 d . . . C5 C 0.57065(13) 0.75979(10) 0.21572(7) 0.02185(19) Uani 1 1 d . . . C6 C 0.74733(14) 0.78045(11) 0.24079(8) 0.0260(2) Uani 1 1 d . . . C7 C 0.83288(16) 0.88659(12) 0.21576(9) 0.0317(2) Uani 1 1 d . . . H7A H 0.9520 0.8998 0.2333 0.038 Uiso 1 1 calc R . . C8 C 0.74896(18) 0.97339(12) 0.16600(9) 0.0336(3) Uani 1 1 d . . . C9 C 0.57521(18) 0.95206(12) 0.14180(10) 0.0348(3) Uani 1 1 d . . . H9A H 0.5157 1.0098 0.1071 0.042 Uiso 1 1 calc R . . C10 C 0.48455(15) 0.84870(11) 0.16658(9) 0.0286(2) Uani 1 1 d . . . C11 C 0.84525(16) 0.68999(14) 0.29531(12) 0.0401(3) Uani 1 1 d . . . H11A H 0.9654 0.7239 0.3115 0.060 Uiso 1 1 calc R . . H11B H 0.8223 0.5958 0.2535 0.060 Uiso 1 1 calc R . . H11C H 0.8116 0.6915 0.3563 0.060 Uiso 1 1 calc R . . C12 C 0.8452(2) 1.08802(15) 0.14072(12) 0.0490(4) Uani 1 1 d . . . H12A H 0.8814 1.0509 0.0812 0.073 Uiso 1 1 calc R . . H12B H 0.9436 1.1303 0.1958 0.073 Uiso 1 1 calc R . . H12C H 0.7728 1.1572 0.1288 0.073 Uiso 1 1 calc R . . C13 C 0.29570(18) 0.83483(16) 0.14208(13) 0.0447(3) Uani 1 1 d . . . H13A H 0.2479 0.7375 0.1182 0.067 Uiso 1 1 calc R . . H13B H 0.2555 0.8819 0.0907 0.067 Uiso 1 1 calc R . . H13C H 0.2611 0.8761 0.2014 0.067 Uiso 1 1 calc R . . C14 C 0.34707(13) 0.33713(10) 0.35039(7) 0.02095(18) Uani 1 1 d . . . C15 C 0.19318(13) 0.32393(11) 0.37645(8) 0.0240(2) Uani 1 1 d . . . C16 C 0.14759(14) 0.21106(12) 0.41014(9) 0.0272(2) Uani 1 1 d . . . H16A H 0.0443 0.2036 0.4277 0.033 Uiso 1 1 calc R . . C17 C 0.24805(14) 0.10916(11) 0.41893(8) 0.0272(2) Uani 1 1 d . . . C18 C 0.39823(14) 0.12266(11) 0.39230(9) 0.0271(2) Uani 1 1 d . . . H18A H 0.4675 0.0531 0.3962 0.033 Uiso 1 1 calc R . . C19 C 0.45053(13) 0.23495(11) 0.36011(8) 0.0237(2) Uani 1 1 d . . . C20 C 0.07577(16) 0.42945(14) 0.36958(10) 0.0352(3) Uani 1 1 d . . . H20A H -0.0396 0.3828 0.3394 0.053 Uiso 1 1 calc R . . H20B H 0.1068 0.4878 0.3290 0.053 Uiso 1 1 calc R . . H20C H 0.0840 0.4862 0.4359 0.053 Uiso 1 1 calc R . . C21 C 0.19884(18) -0.00850(13) 0.45970(11) 0.0375(3) Uani 1 1 d . . . H21A H 0.2634 -0.0827 0.4423 0.056 Uiso 1 1 calc R . . H21B H 0.0788 -0.0423 0.4315 0.056 Uiso 1 1 calc R . . H21C H 0.2223 0.0231 0.5317 0.056 Uiso 1 1 calc R . . C22 C 0.62219(15) 0.24985(14) 0.34188(11) 0.0351(3) Uani 1 1 d . . . H22A H 0.6848 0.1807 0.3651 0.053 Uiso 1 1 calc R . . H22B H 0.6825 0.3417 0.3777 0.053 Uiso 1 1 calc R . . H22C H 0.6107 0.2368 0.2710 0.053 Uiso 1 1 calc R . . N30 N 0.25869(13) 0.37933(10) 0.09187(7) 0.0293(2) Uani 1 1 d . . . C32 C 0.28103(19) 0.41518(16) 0.00102(9) 0.0408(3) Uani 1 1 d . . . H32A H 0.1826 0.3726 -0.0540 0.061 Uiso 1 1 calc R . . H32B H 0.3814 0.3815 -0.0145 0.061 Uiso 1 1 calc R . . H32C H 0.2938 0.5151 0.0116 0.061 Uiso 1 1 calc R . . C31 C 0.10231(17) 0.42284(16) 0.11242(10) 0.0416(3) Uani 1 1 d . . . H31A H 0.0070 0.3777 0.0560 0.062 Uiso 1 1 calc R . . H31B H 0.1096 0.5226 0.1233 0.062 Uiso 1 1 calc R . . H31C H 0.0865 0.3971 0.1716 0.062 Uiso 1 1 calc R . . C33 C 0.2459(2) 0.22833(13) 0.07664(11) 0.0454(3) Uani 1 1 d . . . H33A H 0.1478 0.1833 0.0221 0.068 Uiso 1 1 calc R . . H33B H 0.2341 0.2043 0.1371 0.068 Uiso 1 1 calc R . . H33C H 0.3474 0.1977 0.0607 0.068 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 Al 0.02521(16) 0.02059(15) 0.02066(15) 0.00373(11) 0.00944(12) 0.00140(11) N1 0.0270(4) 0.0200(4) 0.0230(4) 0.0042(3) 0.0100(3) 0.0011(3) C2 0.0377(6) 0.0233(5) 0.0295(5) 0.0025(4) 0.0165(5) 0.0033(4) C3 0.0372(6) 0.0265(5) 0.0207(5) 0.0016(4) 0.0105(4) -0.0014(4) N4 0.0286(4) 0.0207(4) 0.0197(4) 0.0041(3) 0.0091(3) 0.0011(3) C5 0.0253(5) 0.0195(4) 0.0199(4) 0.0034(3) 0.0065(4) 0.0019(3) C6 0.0254(5) 0.0235(5) 0.0276(5) 0.0045(4) 0.0066(4) 0.0014(4) C7 0.0305(6) 0.0285(5) 0.0341(6) 0.0029(4) 0.0126(5) -0.0037(4) C8 0.0475(7) 0.0237(5) 0.0307(6) 0.0048(4) 0.0180(5) -0.0036(5) C9 0.0469(7) 0.0263(5) 0.0336(6) 0.0134(5) 0.0097(5) 0.0049(5) C10 0.0307(5) 0.0258(5) 0.0298(5) 0.0094(4) 0.0063(4) 0.0048(4) C11 0.0264(6) 0.0362(6) 0.0552(8) 0.0170(6) 0.0009(5) 0.0038(5) C12 0.0693(10) 0.0333(7) 0.0485(8) 0.0112(6) 0.0289(8) -0.0096(6) C13 0.0324(6) 0.0439(7) 0.0582(9) 0.0235(7) 0.0015(6) 0.0089(5) C14 0.0209(4) 0.0242(4) 0.0176(4) 0.0048(3) 0.0058(3) 0.0017(3) C15 0.0217(5) 0.0291(5) 0.0243(5) 0.0092(4) 0.0087(4) 0.0056(4) C16 0.0228(5) 0.0320(5) 0.0296(5) 0.0107(4) 0.0102(4) 0.0023(4) C17 0.0282(5) 0.0265(5) 0.0273(5) 0.0085(4) 0.0079(4) 0.0002(4) C18 0.0279(5) 0.0258(5) 0.0300(5) 0.0088(4) 0.0095(4) 0.0070(4) C19 0.0208(4) 0.0278(5) 0.0236(5) 0.0068(4) 0.0077(4) 0.0038(4) C20 0.0325(6) 0.0407(6) 0.0440(7) 0.0193(5) 0.0203(5) 0.0165(5) C21 0.0405(7) 0.0320(6) 0.0472(7) 0.0181(5) 0.0181(6) 0.0034(5) C22 0.0255(5) 0.0429(7) 0.0453(7) 0.0181(6) 0.0170(5) 0.0107(5) N30 0.0343(5) 0.0286(5) 0.0219(4) 0.0019(3) 0.0088(4) -0.0034(4) C32 0.0473(8) 0.0512(8) 0.0226(5) 0.0089(5) 0.0098(5) -0.0004(6) C31 0.0291(6) 0.0561(8) 0.0328(6) 0.0032(6) 0.0062(5) -0.0017(5) C33 0.0597(9) 0.0277(6) 0.0400(7) -0.0011(5) 0.0112(6) -0.0096(6) _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 Al N1 1.8130(9) . ? Al N4 1.8224(9) . ? Al N30 2.0253(10) . ? N1 C5 1.4162(13) . ? N1 C2 1.4759(14) . ? C2 C3 1.5232(16) . ? C3 N4 1.4807(14) . ? N4 C14 1.4164(13) . ? C5 C6 1.4091(15) . ? C5 C10 1.4098(15) . ? C6 C7 1.3976(15) . ? C6 C11 1.5082(17) . ? C7 C8 1.3897(19) . ? C8 C9 1.386(2) . ? C8 C12 1.5116(17) . ? C9 C10 1.3958(16) . ? C10 C13 1.5092(18) . ? C14 C19 1.4105(14) . ? C14 C15 1.4161(14) . ? C15 C16 1.3963(15) . ? C15 C20 1.5107(15) . ? C16 C17 1.3904(16) . ? C17 C18 1.3913(16) . ? C17 C21 1.5097(16) . ? C18 C19 1.3949(15) . ? C19 C22 1.5082(15) . ? N30 C31 1.4774(17) . ? N30 C32 1.4831(16) . ? N30 C33 1.4844(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Al N4 93.27(4) . . ? N1 Al N30 113.26(5) . . ? N4 Al N30 104.21(4) . . ? C5 N1 C2 116.09(8) . . ? C5 N1 Al 134.14(7) . . ? C2 N1 Al 108.66(7) . . ? N1 C2 C3 108.78(9) . . ? N4 C3 C2 108.31(9) . . ? C14 N4 C3 116.51(8) . . ? C14 N4 Al 134.91(7) . . ? C3 N4 Al 107.42(6) . . ? C6 C5 C10 118.64(10) . . ? C6 C5 N1 120.13(9) . . ? C10 C5 N1 121.22(10) . . ? C7 C6 C5 119.74(10) . . ? C7 C6 C11 119.61(11) . . ? C5 C6 C11 120.65(10) . . ? C8 C7 C6 122.00(11) . . ? C9 C8 C7 117.71(10) . . ? C9 C8 C12 121.56(13) . . ? C7 C8 C12 120.73(13) . . ? C8 C9 C10 122.29(11) . . ? C9 C10 C5 119.60(11) . . ? C9 C10 C13 119.68(11) . . ? C5 C10 C13 120.71(10) . . ? C19 C14 C15 118.37(9) . . ? C19 C14 N4 120.46(9) . . ? C15 C14 N4 121.17(9) . . ? C16 C15 C14 119.66(10) . . ? C16 C15 C20 118.43(10) . . ? C14 C15 C20 121.91(10) . . ? C17 C16 C15 122.32(10) . . ? C16 C17 C18 117.49(10) . . ? C16 C17 C21 121.07(11) . . ? C18 C17 C21 121.40(11) . . ? C17 C18 C19 122.21(10) . . ? C18 C19 C14 119.92(9) . . ? C18 C19 C22 119.34(10) . . ? C14 C19 C22 120.64(10) . . ? C31 N30 C32 109.67(11) . . ? C31 N30 C33 108.67(11) . . ? C32 N30 C33 109.14(11) . . ? C31 N30 Al 111.88(8) . . ? C32 N30 Al 109.47(8) . . ? C33 N30 Al 107.95(9) . . ? _diffrn_measured_fraction_theta_max 0.884 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.547 _refine_diff_density_min -0.207 _refine_diff_density_rms 0.047 _database_code_depnum_ccdc_archive 'CCDC 954264' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H78 Al2 N4, 2(C7 H8)' _chemical_formula_sum 'C66 H94 Al2 N4' _chemical_formula_weight 997.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5586(4) _cell_length_b 11.9034(3) _cell_length_c 22.9284(7) _cell_angle_alpha 91.033(2) _cell_angle_beta 96.291(3) _cell_angle_gamma 108.695(2) _cell_volume 2965.47(16) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 15542 _cell_measurement_theta_min 1.9240 _cell_measurement_theta_max 72.3080 _exptl_crystal_description 'tabular needles' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.117 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 0.750 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.863 _exptl_absorpt_correction_T_max 0.959 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur PX Ultra' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 8.2556 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22901 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 72.42 _reflns_number_total 11459 _reflns_number_gt 10035 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0539P)^2^+0.5951P] 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 SHELXL _refine_ls_extinction_coef 0.00050(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11459 _refine_ls_number_parameters 666 _refine_ls_number_restraints 85 _refine_ls_R_factor_all 0.0440 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.1032 _refine_ls_wR_factor_gt 0.0984 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.047 _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 Al1 Al 0.43920(3) 0.68192(3) 0.369230(14) 0.02075(9) Uani 1 1 d . . . H1 H 0.4725(15) 0.5995(15) 0.4092(7) 0.038(4) Uiso 1 1 d . . . Al2 Al 0.56651(3) 0.72507(3) 0.271516(14) 0.02106(9) Uani 1 1 d . . . H2 H 0.6918(15) 0.7199(14) 0.2816(7) 0.037(4) Uiso 1 1 d . . . N1 N 0.56209(8) 0.82591(8) 0.33972(4) 0.02025(19) Uani 1 1 d . . . C2 C 0.48193(10) 0.90466(10) 0.33112(5) 0.0219(2) Uani 1 1 d . . . H2A H 0.5345 0.9882 0.3292 0.026 Uiso 1 1 calc R . . H2B H 0.4273 0.8806 0.2935 0.026 Uiso 1 1 calc R . . C3 C 0.40486(10) 0.89486(10) 0.38128(5) 0.0233(2) Uani 1 1 d . . . H3A H 0.4579 0.9318 0.4180 0.028 Uiso 1 1 calc R . . H3B H 0.3435 0.9361 0.3726 0.028 Uiso 1 1 calc R . . N4 N 0.34263(9) 0.76800(8) 0.38788(4) 0.0232(2) Uani 1 1 d . . . C5 C 0.68657(10) 0.89908(10) 0.36586(5) 0.0219(2) Uani 1 1 d . . . C6 C 0.76223(11) 0.98005(10) 0.33014(5) 0.0249(2) Uani 1 1 d . . . C7 C 0.88013(12) 1.05012(12) 0.35394(6) 0.0331(3) Uani 1 1 d . . . H7A H 0.9306 1.1043 0.3299 0.040 Uiso 1 1 calc R . . C8 C 0.92544(13) 1.04305(14) 0.41123(7) 0.0405(3) Uani 1 1 d . . . H8A H 1.0066 1.0905 0.4264 0.049 Uiso 1 1 calc R . . C9 C 0.85111(12) 0.96605(13) 0.44612(6) 0.0360(3) Uani 1 1 d . . . H9A H 0.8823 0.9609 0.4857 0.043 Uiso 1 1 calc R . . C10 C 0.73099(11) 0.89495(10) 0.42524(5) 0.0256(2) Uani 1 1 d . . . C11 C 0.72470(11) 1.00034(11) 0.26645(5) 0.0276(3) Uani 1 1 d . . . H11A H 0.6400 0.9441 0.2540 0.033 Uiso 1 1 calc R . . C12 C 0.81103(14) 0.97677(14) 0.22544(6) 0.0401(3) Uani 1 1 d . . . H12A H 0.8131 0.8956 0.2293 0.060 Uiso 1 1 calc R . . H12B H 0.8940 1.0332 0.2359 0.060 Uiso 1 1 calc R . . H12C H 0.7813 0.9864 0.1847 0.060 Uiso 1 1 calc R . . C13 C 0.72143(13) 1.12784(12) 0.26015(7) 0.0382(3) Uani 1 1 d . . . H13A H 0.6661 1.1431 0.2865 0.057 Uiso 1 1 calc R . . H13B H 0.6916 1.1372 0.2194 0.057 Uiso 1 1 calc R . . H13C H 0.8045 1.1843 0.2706 0.057 Uiso 1 1 calc R . . C14 C 0.65732(11) 0.82091(11) 0.46989(5) 0.0274(2) Uani 1 1 d . . . H14A H 0.5700 0.7870 0.4514 0.033 Uiso 1 1 calc R . . C15 C 0.65861(15) 0.89671(15) 0.52473(6) 0.0449(4) Uani 1 1 d . . . H15A H 0.6294 0.9628 0.5132 0.067 Uiso 1 1 calc R . . H15B H 0.7427 0.9281 0.5449 0.067 Uiso 1 1 calc R . . H15C H 0.6046 0.8478 0.5512 0.067 Uiso 1 1 calc R . . C16 C 0.70232(14) 0.71750(14) 0.48655(8) 0.0440(4) Uani 1 1 d . . . H16A H 0.7008 0.6699 0.4510 0.066 Uiso 1 1 calc R . . H16B H 0.6485 0.6678 0.5129 0.066 Uiso 1 1 calc R . . H16C H 0.7866 0.7481 0.5065 0.066 Uiso 1 1 calc R . . C17 C 0.22769(11) 0.73926(10) 0.41159(5) 0.0253(2) Uani 1 1 d . . . C18 C 0.21949(12) 0.71078(11) 0.47083(6) 0.0286(3) Uani 1 1 d . . . C19 C 0.10333(13) 0.66968(13) 0.49011(6) 0.0370(3) Uani 1 1 d . . . H19A H 0.0968 0.6463 0.5293 0.044 Uiso 1 1 calc R . . C20 C -0.00183(13) 0.66231(14) 0.45348(7) 0.0425(3) Uani 1 1 d . . . H20A H -0.0802 0.6314 0.4669 0.051 Uiso 1 1 calc R . . C21 C 0.00726(13) 0.70029(13) 0.39690(7) 0.0389(3) Uani 1 1 d . . . H21A H -0.0650 0.6997 0.3726 0.047 Uiso 1 1 calc R . . C22 C 0.12056(11) 0.73939(11) 0.37500(6) 0.0295(3) Uani 1 1 d . . . C23 C 0.33271(12) 0.72838(11) 0.51504(6) 0.0309(3) Uani 1 1 d . . . H23A H 0.4060 0.7742 0.4960 0.037 Uiso 1 1 calc R . . C24 C 0.32965(16) 0.80219(14) 0.56993(7) 0.0429(3) Uani 1 1 d . . . H24A H 0.3175 0.8768 0.5583 0.064 Uiso 1 1 calc R . . H24B H 0.4077 0.8196 0.5955 0.064 Uiso 1 1 calc R . . H24C H 0.2618 0.7574 0.5911 0.064 Uiso 1 1 calc R . . C25 C 0.35242(16) 0.61258(14) 0.53373(7) 0.0440(3) Uani 1 1 d . . . H25A H 0.3545 0.5649 0.4988 0.066 Uiso 1 1 calc R . . H25B H 0.2848 0.5679 0.5551 0.066 Uiso 1 1 calc R . . H25C H 0.4306 0.6307 0.5593 0.066 Uiso 1 1 calc R . . C26 C 0.12642(12) 0.78694(12) 0.31387(6) 0.0318(3) Uani 1 1 d . . . H26A H 0.2125 0.8039 0.3043 0.038 Uiso 1 1 calc R . . C27 C 0.04029(14) 0.69980(14) 0.26582(7) 0.0427(3) Uani 1 1 d . . . H27A H 0.0582 0.6247 0.2664 0.064 Uiso 1 1 calc R . . H27B H 0.0527 0.7335 0.2274 0.064 Uiso 1 1 calc R . . H27C H -0.0453 0.6853 0.2729 0.064 Uiso 1 1 calc R . . C28 C 0.09769(15) 0.90402(14) 0.31301(8) 0.0452(4) Uani 1 1 d . . . H28A H 0.1529 0.9601 0.3437 0.068 Uiso 1 1 calc R . . H28B H 0.0121 0.8891 0.3202 0.068 Uiso 1 1 calc R . . H28C H 0.1097 0.9377 0.2746 0.068 Uiso 1 1 calc R . . N31 N 0.41571(9) 0.59464(8) 0.29196(4) 0.02124(19) Uani 1 1 d . . . C32 C 0.32045(11) 0.60900(10) 0.24425(5) 0.0247(2) Uani 1 1 d . . . H32A H 0.2488 0.5352 0.2389 0.030 Uiso 1 1 calc R . . H32B H 0.2915 0.6746 0.2564 0.030 Uiso 1 1 calc R . . C33 C 0.37369(12) 0.63544(10) 0.18665(5) 0.0275(2) Uani 1 1 d . . . H33A H 0.3882 0.5644 0.1701 0.033 Uiso 1 1 calc R . . H33B H 0.3160 0.6583 0.1579 0.033 Uiso 1 1 calc R . . N34 N 0.49010(9) 0.73351(8) 0.19895(4) 0.0249(2) Uani 1 1 d . . . C35 C 0.39330(11) 0.46701(10) 0.30021(5) 0.0227(2) Uani 1 1 d . . . C36 C 0.28362(11) 0.40106(10) 0.32320(5) 0.0260(2) Uani 1 1 d . . . C37 C 0.26307(13) 0.28114(11) 0.33290(6) 0.0314(3) Uani 1 1 d . . . H37A H 0.1895 0.2367 0.3479 0.038 Uiso 1 1 calc R . . C38 C 0.34675(13) 0.22551(11) 0.32135(6) 0.0336(3) Uani 1 1 d . . . H38A H 0.3323 0.1444 0.3293 0.040 Uiso 1 1 calc R . . C39 C 0.45111(13) 0.28902(11) 0.29814(6) 0.0308(3) Uani 1 1 d . . . H39A H 0.5085 0.2506 0.2901 0.037 Uiso 1 1 calc R . . C40 C 0.47585(11) 0.40869(10) 0.28594(5) 0.0255(2) Uani 1 1 d . . . C41 C 0.18241(11) 0.45007(11) 0.33750(6) 0.0289(3) Uani 1 1 d . . . H41A H 0.2109 0.5375 0.3323 0.035 Uiso 1 1 calc R . . C42 C 0.15297(14) 0.42982(12) 0.40089(6) 0.0375(3) Uani 1 1 d . . . H42A H 0.2281 0.4656 0.4282 0.056 Uiso 1 1 calc R . . H42B H 0.1209 0.3443 0.4063 0.056 Uiso 1 1 calc R . . H42C H 0.0911 0.4666 0.4087 0.056 Uiso 1 1 calc R . . C43 C 0.06357(13) 0.39293(13) 0.29545(7) 0.0407(3) Uani 1 1 d . . . H43A H 0.0810 0.4054 0.2548 0.061 Uiso 1 1 calc R . . H43B H 0.0018 0.4294 0.3037 0.061 Uiso 1 1 calc R . . H43C H 0.0322 0.3075 0.3011 0.061 Uiso 1 1 calc R . . C44 C 0.59163(12) 0.46448(11) 0.25746(6) 0.0309(3) Uani 1 1 d . . . H44A H 0.5911 0.5446 0.2453 0.037 Uiso 1 1 calc R . . C45 C 0.59622(18) 0.39282(14) 0.20215(8) 0.0497(4) Uani 1 1 d . . . H45A H 0.5220 0.3824 0.1746 0.075 Uiso 1 1 calc R . . H45B H 0.6005 0.3148 0.2129 0.075 Uiso 1 1 calc R . . H45C H 0.6691 0.4353 0.1835 0.075 Uiso 1 1 calc R . . C46 C 0.70598(14) 0.48294(16) 0.30136(9) 0.0532(4) Uani 1 1 d . . . H46A H 0.7008 0.5289 0.3363 0.080 Uiso 1 1 calc R . . H46B H 0.7793 0.5262 0.2833 0.080 Uiso 1 1 calc R . . H46C H 0.7113 0.4056 0.3127 0.080 Uiso 1 1 calc R . . C47 C 0.52689(11) 0.80291(10) 0.14997(5) 0.0260(2) Uani 1 1 d . . . C48 C 0.61312(12) 0.78231(11) 0.11568(6) 0.0312(3) Uani 1 1 d . . . C49 C 0.65253(14) 0.85749(13) 0.07065(6) 0.0376(3) Uani 1 1 d . . . H49A H 0.7119 0.8450 0.0480 0.045 Uiso 1 1 calc R . . C50 C 0.60712(15) 0.94925(13) 0.05837(6) 0.0401(3) Uani 1 1 d . . . H50A H 0.6375 1.0016 0.0287 0.048 Uiso 1 1 calc R . . C51 C 0.51675(14) 0.96469(12) 0.08957(6) 0.0363(3) Uani 1 1 d . . . H51A H 0.4831 1.0260 0.0798 0.044 Uiso 1 1 calc R . . C52 C 0.47416(12) 0.89240(11) 0.13485(5) 0.0286(3) Uani 1 1 d . . . C53 C 0.65721(15) 0.67578(13) 0.12363(6) 0.0402(3) Uani 1 1 d . . . H53A H 0.6296 0.6396 0.1609 0.048 Uiso 1 1 calc R . . C54 C 0.59603(17) 0.58257(15) 0.07309(8) 0.0527(4) Uani 1 1 d . . . H54A H 0.5065 0.5631 0.0703 0.079 Uiso 1 1 calc R . . H54B H 0.6180 0.5107 0.0805 0.079 Uiso 1 1 calc R . . H54C H 0.6244 0.6143 0.0361 0.079 Uiso 1 1 calc R . . C55 C 0.79670(18) 0.70667(18) 0.12886(8) 0.0560(4) Uani 1 1 d . . . H55A H 0.8348 0.7658 0.1615 0.084 Uiso 1 1 calc R . . H55B H 0.8261 0.7393 0.0922 0.084 Uiso 1 1 calc R . . H55C H 0.8189 0.6349 0.1361 0.084 Uiso 1 1 calc R . . C56 C 0.36821(12) 0.90808(11) 0.16452(6) 0.0312(3) Uani 1 1 d . . . H56A H 0.3523 0.8513 0.1966 0.037 Uiso 1 1 calc R . . C57 C 0.39631(15) 1.03318(13) 0.19227(7) 0.0418(3) Uani 1 1 d . . . H57A H 0.4713 1.0530 0.2203 0.063 Uiso 1 1 calc R . . H57B H 0.3274 1.0363 0.2129 0.063 Uiso 1 1 calc R . . H57C H 0.4083 1.0904 0.1615 0.063 Uiso 1 1 calc R . . C58 C 0.25076(15) 0.87658(15) 0.12089(7) 0.0464(4) Uani 1 1 d . . . H58A H 0.2327 0.7962 0.1033 0.070 Uiso 1 1 calc R . . H58B H 0.2625 0.9334 0.0899 0.070 Uiso 1 1 calc R . . H58C H 0.1819 0.8799 0.1415 0.070 Uiso 1 1 calc R . . C60 C -0.0516(2) 0.1430(3) 0.00898(10) 0.0800(7) Uani 1 1 d . . . H60A H -0.1063 0.1911 0.0095 0.120 Uiso 1 1 calc R . . H60B H -0.0993 0.0590 0.0111 0.120 Uiso 1 1 calc R . . H60C H -0.0132 0.1541 -0.0275 0.120 Uiso 1 1 calc R . . C61 C 0.04692(16) 0.18129(17) 0.06093(7) 0.0514(4) Uani 1 1 d . . . C62 C 0.02490(19) 0.1398(2) 0.11570(9) 0.0749(7) Uani 1 1 d . . . H62A H -0.0529 0.0841 0.1205 0.090 Uiso 1 1 calc R . . C63 C 0.1139(2) 0.1776(2) 0.16376(9) 0.0710(6) Uani 1 1 d . . . H63A H 0.0966 0.1475 0.2011 0.085 Uiso 1 1 calc R . . C64 C 0.22534(18) 0.25709(18) 0.15810(8) 0.0568(4) Uani 1 1 d . . . H64A H 0.2860 0.2835 0.1913 0.068 Uiso 1 1 calc R . . C65 C 0.24972(19) 0.29899(18) 0.10398(9) 0.0622(5) Uani 1 1 d . . . H65A H 0.3280 0.3541 0.0995 0.075 Uiso 1 1 calc R . . C66 C 0.16066(18) 0.26129(18) 0.05589(8) 0.0550(4) Uani 1 1 d . . . H66A H 0.1786 0.2914 0.0186 0.066 Uiso 1 1 calc R . . C70 C 1.0207(3) 0.5077(3) 0.11843(13) 0.0690(8) Uani 0.767(4) 1 d PDU A 1 H70A H 1.0764 0.4605 0.1199 0.103 Uiso 0.767(4) 1 calc PR A 1 H70B H 1.0080 0.5268 0.1585 0.103 Uiso 0.767(4) 1 calc PR A 1 H70C H 1.0569 0.5815 0.0991 0.103 Uiso 0.767(4) 1 calc PR A 1 C71 C 0.89934(14) 0.43794(16) 0.08437(8) 0.0451(6) Uani 0.767(4) 1 d PGDU A 1 C72 C 0.86098(18) 0.46775(16) 0.02893(8) 0.0524(8) Uani 0.767(4) 1 d PGDU A 1 H72A H 0.9115 0.5351 0.0116 0.063 Uiso 0.767(4) 1 calc PR A 1 C73 C 0.7487(2) 0.3990(3) -0.00120(8) 0.0744(9) Uani 0.767(4) 1 d PGU A 1 H73A H 0.7225 0.4194 -0.0391 0.089 Uiso 0.767(4) 1 calc PR A 1 C74 C 0.67488(14) 0.3005(2) 0.02411(14) 0.0918(16) Uani 0.767(4) 1 d PGU A 1 H74A H 0.5982 0.2536 0.0035 0.110 Uiso 0.767(4) 1 calc PR A 1 C75 C 0.7132(2) 0.27073(15) 0.07955(14) 0.0861(14) Uani 0.767(4) 1 d PGU A 1 H75A H 0.6628 0.2034 0.0968 0.103 Uiso 0.767(4) 1 calc PR A 1 C76 C 0.8255(3) 0.33943(18) 0.10968(8) 0.0683(9) Uani 0.767(4) 1 d PGDU A 1 H76A H 0.8517 0.3191 0.1476 0.082 Uiso 0.767(4) 1 calc PR A 1 C70' C 0.9557(14) 0.4294(15) 0.1438(6) 0.123(5) Uiso 0.233(4) 1 d PDU A 2 H70D H 0.9735 0.3578 0.1564 0.184 Uiso 0.233(4) 1 calc PR A 2 H70E H 0.9253 0.4630 0.1759 0.184 Uiso 0.233(4) 1 calc PR A 2 H70F H 1.0309 0.4880 0.1335 0.184 Uiso 0.233(4) 1 calc PR A 2 C71' C 0.8611(6) 0.3984(8) 0.0920(3) 0.053(2) Uiso 0.233(4) 1 d PGDU A 2 C72' C 0.8779(5) 0.4683(6) 0.0437(4) 0.049(2) Uiso 0.233(4) 1 d PGDU A 2 H72B H 0.9489 0.5365 0.0445 0.059 Uiso 0.233(4) 1 calc PR A 2 C73' C 0.7906(7) 0.4385(6) -0.0057(3) 0.061(3) Uiso 0.233(4) 1 d PGU A 2 H73B H 0.8021 0.4863 -0.0387 0.073 Uiso 0.233(4) 1 calc PR A 2 C74' C 0.6866(6) 0.3388(6) -0.0068(3) 0.046(2) Uiso 0.233(4) 1 d PGU A 2 H74B H 0.6270 0.3184 -0.0406 0.055 Uiso 0.233(4) 1 calc PR A 2 C75' C 0.6698(5) 0.2689(5) 0.0414(4) 0.045(2) Uiso 0.233(4) 1 d PGU A 2 H75B H 0.5987 0.2007 0.0407 0.054 Uiso 0.233(4) 1 calc PR A 2 C76' C 0.7571(7) 0.2987(7) 0.0908(3) 0.052(2) Uiso 0.233(4) 1 d PGDU A 2 H76B H 0.7456 0.2509 0.1238 0.063 Uiso 0.233(4) 1 calc PR A 2 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 0.02124(17) 0.01910(16) 0.02187(16) 0.00092(12) 0.00356(12) 0.00619(12) Al2 0.02108(17) 0.01934(16) 0.02219(17) 0.00010(12) 0.00387(12) 0.00542(12) N1 0.0192(4) 0.0187(4) 0.0224(4) 0.0001(3) 0.0021(4) 0.0058(4) C2 0.0206(5) 0.0202(5) 0.0255(5) 0.0019(4) 0.0015(4) 0.0077(4) C3 0.0213(5) 0.0209(5) 0.0277(6) -0.0006(4) 0.0030(4) 0.0071(4) N4 0.0217(5) 0.0212(5) 0.0266(5) 0.0012(4) 0.0059(4) 0.0060(4) C5 0.0193(5) 0.0208(5) 0.0256(6) -0.0017(4) 0.0015(4) 0.0074(4) C6 0.0221(5) 0.0228(5) 0.0291(6) 0.0004(4) 0.0023(5) 0.0067(4) C7 0.0236(6) 0.0322(6) 0.0376(7) 0.0047(5) 0.0014(5) 0.0015(5) C8 0.0229(6) 0.0465(8) 0.0412(8) 0.0044(6) -0.0064(6) -0.0007(6) C9 0.0270(6) 0.0435(7) 0.0313(7) 0.0035(6) -0.0067(5) 0.0060(6) C10 0.0244(6) 0.0265(6) 0.0266(6) 0.0001(4) 0.0006(5) 0.0099(5) C11 0.0244(6) 0.0260(6) 0.0279(6) 0.0034(5) 0.0033(5) 0.0019(5) C12 0.0355(7) 0.0453(8) 0.0345(7) 0.0007(6) 0.0124(6) 0.0038(6) C13 0.0346(7) 0.0298(6) 0.0454(8) 0.0111(6) -0.0009(6) 0.0053(5) C14 0.0263(6) 0.0318(6) 0.0232(6) 0.0010(5) -0.0005(5) 0.0095(5) C15 0.0412(8) 0.0569(9) 0.0303(7) -0.0101(6) 0.0051(6) 0.0077(7) C16 0.0389(8) 0.0417(8) 0.0531(9) 0.0160(7) -0.0004(7) 0.0164(6) C17 0.0240(6) 0.0219(5) 0.0308(6) 0.0007(4) 0.0075(5) 0.0071(4) C18 0.0295(6) 0.0262(6) 0.0314(6) 0.0013(5) 0.0098(5) 0.0086(5) C19 0.0353(7) 0.0396(7) 0.0369(7) 0.0047(6) 0.0158(6) 0.0093(6) C20 0.0288(7) 0.0482(8) 0.0510(9) 0.0034(7) 0.0184(6) 0.0087(6) C21 0.0232(6) 0.0463(8) 0.0472(8) 0.0019(6) 0.0065(6) 0.0107(6) C22 0.0241(6) 0.0292(6) 0.0357(7) 0.0002(5) 0.0059(5) 0.0088(5) C23 0.0328(6) 0.0323(6) 0.0272(6) 0.0033(5) 0.0084(5) 0.0082(5) C24 0.0523(9) 0.0404(8) 0.0368(7) -0.0060(6) 0.0035(7) 0.0172(7) C25 0.0543(9) 0.0392(8) 0.0406(8) -0.0001(6) -0.0014(7) 0.0202(7) C26 0.0234(6) 0.0352(7) 0.0369(7) 0.0049(5) 0.0023(5) 0.0097(5) C27 0.0356(7) 0.0453(8) 0.0412(8) 0.0030(6) -0.0031(6) 0.0071(6) C28 0.0401(8) 0.0412(8) 0.0579(9) 0.0095(7) 0.0037(7) 0.0187(6) N31 0.0213(5) 0.0185(4) 0.0229(5) 0.0010(3) 0.0024(4) 0.0052(4) C32 0.0228(5) 0.0232(5) 0.0264(6) 0.0017(4) 0.0009(5) 0.0056(4) C33 0.0299(6) 0.0233(5) 0.0251(6) 0.0005(4) 0.0009(5) 0.0040(5) N34 0.0278(5) 0.0219(5) 0.0221(5) 0.0011(4) 0.0036(4) 0.0038(4) C35 0.0260(6) 0.0180(5) 0.0214(5) -0.0006(4) 0.0004(4) 0.0044(4) C36 0.0284(6) 0.0224(5) 0.0243(6) -0.0003(4) 0.0021(5) 0.0046(5) C37 0.0349(7) 0.0218(6) 0.0339(7) 0.0030(5) 0.0075(5) 0.0028(5) C38 0.0430(7) 0.0206(6) 0.0359(7) 0.0037(5) 0.0052(6) 0.0083(5) C39 0.0372(7) 0.0233(6) 0.0334(6) 0.0005(5) 0.0035(5) 0.0123(5) C40 0.0273(6) 0.0222(5) 0.0256(6) -0.0014(4) 0.0007(5) 0.0070(5) C41 0.0261(6) 0.0237(6) 0.0350(7) 0.0040(5) 0.0073(5) 0.0040(5) C42 0.0409(7) 0.0326(7) 0.0404(7) 0.0064(6) 0.0172(6) 0.0098(6) C43 0.0282(7) 0.0350(7) 0.0515(9) 0.0065(6) 0.0009(6) 0.0010(6) C44 0.0304(6) 0.0239(6) 0.0409(7) 0.0029(5) 0.0086(5) 0.0107(5) C45 0.0652(10) 0.0340(7) 0.0590(10) 0.0037(7) 0.0324(8) 0.0203(7) C46 0.0304(7) 0.0478(9) 0.0767(12) 0.0176(8) 0.0014(8) 0.0072(6) C47 0.0285(6) 0.0240(5) 0.0218(5) 0.0011(4) 0.0014(5) 0.0041(5) C48 0.0352(7) 0.0323(6) 0.0253(6) 0.0020(5) 0.0052(5) 0.0096(5) C49 0.0400(7) 0.0438(7) 0.0285(6) 0.0060(6) 0.0107(6) 0.0105(6) C50 0.0468(8) 0.0397(7) 0.0299(7) 0.0126(6) 0.0080(6) 0.0069(6) C51 0.0433(8) 0.0309(6) 0.0328(7) 0.0078(5) 0.0009(6) 0.0106(6) C52 0.0308(6) 0.0260(6) 0.0257(6) 0.0003(5) -0.0009(5) 0.0063(5) C53 0.0556(9) 0.0437(8) 0.0317(7) 0.0076(6) 0.0174(6) 0.0263(7) C54 0.0570(10) 0.0413(8) 0.0617(11) -0.0055(7) 0.0151(8) 0.0168(7) C55 0.0597(11) 0.0677(11) 0.0507(9) -0.0106(8) -0.0018(8) 0.0383(9) C56 0.0328(7) 0.0305(6) 0.0303(6) 0.0009(5) -0.0008(5) 0.0118(5) C57 0.0445(8) 0.0357(7) 0.0465(8) -0.0040(6) 0.0000(7) 0.0171(6) C58 0.0369(8) 0.0544(9) 0.0454(8) -0.0033(7) -0.0070(7) 0.0155(7) C60 0.0564(12) 0.123(2) 0.0505(11) -0.0088(12) -0.0104(9) 0.0219(13) C61 0.0423(9) 0.0710(11) 0.0398(8) -0.0030(8) 0.0002(7) 0.0188(8) C62 0.0439(10) 0.1092(18) 0.0532(11) 0.0139(11) 0.0066(9) -0.0012(11) C63 0.0607(12) 0.1021(16) 0.0417(10) 0.0160(10) 0.0052(9) 0.0142(11) C64 0.0554(10) 0.0654(11) 0.0444(9) -0.0036(8) -0.0098(8) 0.0178(9) C65 0.0527(10) 0.0607(11) 0.0585(11) 0.0029(9) 0.0006(9) 0.0002(9) C66 0.0575(10) 0.0635(11) 0.0417(9) 0.0067(8) 0.0082(8) 0.0155(8) C70 0.0646(17) 0.0825(19) 0.0576(15) -0.0173(13) -0.0079(13) 0.0268(14) C71 0.0517(13) 0.0401(12) 0.0460(13) -0.0035(9) 0.0181(10) 0.0148(11) C72 0.0460(13) 0.0669(16) 0.0452(16) -0.0075(11) 0.0029(12) 0.0208(11) C73 0.0489(18) 0.097(2) 0.0747(19) -0.0382(17) -0.0042(14) 0.026(2) C74 0.0605(19) 0.075(2) 0.125(4) -0.055(3) 0.020(2) 0.0019(16) C75 0.070(2) 0.0562(17) 0.116(3) -0.0252(18) 0.028(2) -0.0055(15) C76 0.079(2) 0.0441(13) 0.0804(19) -0.0015(13) 0.0356(17) 0.0104(14) _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 N4 1.8167(10) . ? Al1 N31 1.9848(10) . ? Al1 N1 2.0261(10) . ? Al1 Al2 2.7800(5) . ? Al2 N34 1.8163(11) . ? Al2 N1 1.9692(10) . ? Al2 N31 2.0345(10) . ? N1 C5 1.4755(14) . ? N1 C2 1.5164(14) . ? C2 C3 1.5141(16) . ? C3 N4 1.4685(14) . ? N4 C17 1.4321(15) . ? C5 C10 1.4089(16) . ? C5 C6 1.4176(17) . ? C6 C7 1.3937(17) . ? C6 C11 1.5233(17) . ? C7 C8 1.374(2) . ? C8 C9 1.375(2) . ? C9 C10 1.3999(18) . ? C10 C14 1.5140(17) . ? C11 C12 1.5278(19) . ? C11 C13 1.5392(18) . ? C14 C16 1.5216(18) . ? C14 C15 1.5303(19) . ? C17 C18 1.4118(18) . ? C17 C22 1.4180(18) . ? C18 C19 1.3980(18) . ? C18 C23 1.5199(19) . ? C19 C20 1.377(2) . ? C20 C21 1.385(2) . ? C21 C22 1.3948(19) . ? C22 C26 1.5214(19) . ? C23 C25 1.5286(19) . ? C23 C24 1.5320(19) . ? C26 C27 1.529(2) . ? C26 C28 1.533(2) . ? N31 C35 1.4764(14) . ? N31 C32 1.5171(15) . ? C32 C33 1.5135(17) . ? C33 N34 1.4665(15) . ? N34 C47 1.4274(15) . ? C35 C40 1.4085(17) . ? C35 C36 1.4229(17) . ? C36 C37 1.3962(17) . ? C36 C41 1.5268(18) . ? C37 C38 1.380(2) . ? C38 C39 1.371(2) . ? C39 C40 1.4000(17) . ? C40 C44 1.5152(18) . ? C41 C42 1.5346(19) . ? C41 C43 1.5382(19) . ? C44 C46 1.524(2) . ? C44 C45 1.531(2) . ? C47 C48 1.4119(18) . ? C47 C52 1.4177(18) . ? C48 C49 1.3961(19) . ? C48 C53 1.5175(19) . ? C49 C50 1.376(2) . ? C50 C51 1.385(2) . ? C51 C52 1.3903(19) . ? C52 C56 1.5237(19) . ? C53 C55 1.525(3) . ? C53 C54 1.531(2) . ? C56 C57 1.5292(19) . ? C56 C58 1.5320(19) . ? C60 C61 1.508(3) . ? C61 C66 1.372(3) . ? C61 C62 1.378(3) . ? C62 C63 1.382(3) . ? C63 C64 1.354(3) . ? C64 C65 1.370(3) . ? C65 C66 1.384(3) . ? C70 C71 1.502(3) . ? C71 C72 1.3900 . ? C71 C76 1.3900 . ? C72 C73 1.3900 . ? C73 C74 1.3900 . ? C74 C75 1.3900 . ? C75 C76 1.3900 . ? C70' C71' 1.477(11) . ? C71' C72' 1.3900 . ? C71' C76' 1.3900 . ? C72' C73' 1.3900 . ? C73' C74' 1.3900 . ? C74' C75' 1.3900 . ? C75' C76' 1.3900 . ? 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 N4 Al1 N31 123.02(5) . . ? N4 Al1 N1 91.90(4) . . ? N31 Al1 N1 90.68(4) . . ? N4 Al1 Al2 122.05(3) . . ? N31 Al1 Al2 46.98(3) . . ? N1 Al1 Al2 45.07(3) . . ? N34 Al2 N1 122.45(4) . . ? N34 Al2 N31 91.55(4) . . ? N1 Al2 N31 90.88(4) . . ? N34 Al2 Al1 121.63(4) . . ? N1 Al2 Al1 46.76(3) . . ? N31 Al2 Al1 45.50(3) . . ? C5 N1 C2 108.87(8) . . ? C5 N1 Al2 112.02(7) . . ? C2 N1 Al2 117.35(7) . . ? C5 N1 Al1 130.70(7) . . ? C2 N1 Al1 99.09(6) . . ? Al2 N1 Al1 88.17(4) . . ? C3 C2 N1 110.39(9) . . ? N4 C3 C2 107.54(9) . . ? C17 N4 C3 115.73(9) . . ? C17 N4 Al1 133.78(8) . . ? C3 N4 Al1 110.23(7) . . ? C10 C5 C6 118.96(10) . . ? C10 C5 N1 122.67(10) . . ? C6 C5 N1 118.32(10) . . ? C7 C6 C5 119.30(11) . . ? C7 C6 C11 115.46(11) . . ? C5 C6 C11 125.23(10) . . ? C8 C7 C6 121.85(12) . . ? C7 C8 C9 118.77(12) . . ? C8 C9 C10 122.19(12) . . ? C9 C10 C5 118.84(11) . . ? C9 C10 C14 116.14(11) . . ? C5 C10 C14 125.00(11) . . ? C6 C11 C12 111.90(11) . . ? C6 C11 C13 110.87(11) . . ? C12 C11 C13 109.36(11) . . ? C10 C14 C16 111.66(11) . . ? C10 C14 C15 111.49(11) . . ? C16 C14 C15 110.55(12) . . ? C18 C17 C22 119.53(11) . . ? C18 C17 N4 120.97(11) . . ? C22 C17 N4 119.50(11) . . ? C19 C18 C17 118.84(12) . . ? C19 C18 C23 118.78(12) . . ? C17 C18 C23 122.32(11) . . ? C20 C19 C18 121.43(13) . . ? C19 C20 C21 119.63(13) . . ? C20 C21 C22 121.19(13) . . ? C21 C22 C17 118.92(12) . . ? C21 C22 C26 119.03(12) . . ? C17 C22 C26 121.96(11) . . ? C18 C23 C25 113.96(11) . . ? C18 C23 C24 111.41(11) . . ? C25 C23 C24 109.07(12) . . ? C22 C26 C27 113.66(11) . . ? C22 C26 C28 110.29(12) . . ? C27 C26 C28 109.29(12) . . ? C35 N31 C32 109.35(8) . . ? C35 N31 Al1 110.07(7) . . ? C32 N31 Al1 118.70(7) . . ? C35 N31 Al2 131.46(8) . . ? C32 N31 Al2 99.40(6) . . ? Al1 N31 Al2 87.52(4) . . ? C33 C32 N31 111.01(10) . . ? N34 C33 C32 107.27(9) . . ? C47 N34 C33 114.75(9) . . ? C47 N34 Al2 133.72(8) . . ? C33 N34 Al2 110.81(8) . . ? C40 C35 C36 119.20(10) . . ? C40 C35 N31 122.49(10) . . ? C36 C35 N31 118.31(10) . . ? C37 C36 C35 118.91(12) . . ? C37 C36 C41 115.85(11) . . ? C35 C36 C41 125.22(10) . . ? C38 C37 C36 121.75(12) . . ? C39 C38 C37 119.00(11) . . ? C38 C39 C40 122.16(12) . . ? C39 C40 C35 118.87(11) . . ? C39 C40 C44 115.73(11) . . ? C35 C40 C44 125.40(10) . . ? C36 C41 C42 112.37(11) . . ? C36 C41 C43 110.85(11) . . ? C42 C41 C43 108.62(11) . . ? C40 C44 C46 110.79(12) . . ? C40 C44 C45 112.35(11) . . ? C46 C44 C45 111.05(13) . . ? C48 C47 C52 119.49(11) . . ? C48 C47 N34 121.06(11) . . ? C52 C47 N34 119.43(11) . . ? C49 C48 C47 119.02(12) . . ? C49 C48 C53 119.09(12) . . ? C47 C48 C53 121.75(11) . . ? C50 C49 C48 121.35(14) . . ? C49 C50 C51 119.54(13) . . ? C50 C51 C52 121.45(13) . . ? C51 C52 C47 118.85(12) . . ? C51 C52 C56 118.89(12) . . ? C47 C52 C56 122.19(11) . . ? C48 C53 C55 113.84(13) . . ? C48 C53 C54 109.74(13) . . ? C55 C53 C54 110.19(13) . . ? C52 C56 C57 113.23(12) . . ? C52 C56 C58 110.59(11) . . ? C57 C56 C58 109.64(12) . . ? C66 C61 C62 117.44(17) . . ? C66 C61 C60 121.36(18) . . ? C62 C61 C60 121.17(18) . . ? C61 C62 C63 121.25(19) . . ? C64 C63 C62 120.56(19) . . ? C63 C64 C65 119.26(17) . . ? C64 C65 C66 120.20(18) . . ? C61 C66 C65 121.29(17) . . ? C72 C71 C76 120.0 . . ? C72 C71 C70 122.24(19) . . ? C76 C71 C70 117.75(19) . . ? C71 C72 C73 120.0 . . ? C74 C73 C72 120.0 . . ? C75 C74 C73 120.0 . . ? C74 C75 C76 120.0 . . ? C75 C76 C71 120.0 . . ? C72' C71' C76' 120.0 . . ? C72' C71' C70' 119.6(6) . . ? C76' C71' C70' 120.4(6) . . ? C71' C72' C73' 120.0 . . ? C72' C73' C74' 120.0 . . ? C75' C74' C73' 120.0 . . ? C74' C75' C76' 120.0 . . ? C75' C76' C71' 120.0 . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 72.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.268 _refine_diff_density_min -0.251 _refine_diff_density_rms 0.037 #===END _database_code_depnum_ccdc_archive 'CCDC 954265'