Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Carl Redshaw' 'Vernon C. Gibson' 'Drew Nienhuis' 'Andrew J. P. White' 'David J. Williams' _publ_contact_author_name 'Dr Carl Redshaw' _publ_contact_author_address ; School of Chemistry and Pharmacy The University of East Anglia Wolfson Materials and Catalysis Cen Norwich Norfolk NR4 7TJ UNITED KINGDOM ; _publ_contact_author_email CARL.REDSHAW@UEA.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Bis(imino)phenoxide Complexes of Aluminium ; data_Compound_1 _database_code_depnum_ccdc_archive 'CCDC 233653' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C35 H47 N2 O Al' _chemical_formula_weight 538.73 _chemical_melting_point ? _chemical_compound_source ? 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' O O 0.0492 0.0322 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/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 8.9160(5) _cell_length_b 23.9904(15) _cell_length_c 15.8501(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.539(5) _cell_angle_gamma 90.00 _cell_volume 3379.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 10.80 _cell_measurement_theta_max 25.00 _exptl_crystal_description plates _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.059 _exptl_crystal_density_method ? _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 0.716 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5367 _diffrn_reflns_av_R_equivalents 0.0679 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 60.00 _reflns_number_total 5006 _reflns_number_observed 3775 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 389 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1027P)^2^+0.4788P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0008(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4617 _refine_ls_number_parameters 361 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0823 _refine_ls_R_factor_obs 0.0605 _refine_ls_wR_factor_all 0.1819 _refine_ls_wR_factor_obs 0.1586 _refine_ls_goodness_of_fit_all 1.046 _refine_ls_goodness_of_fit_obs 1.091 _refine_ls_restrained_S_all 1.092 _refine_ls_restrained_S_obs 1.110 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Al Al 0.50513(9) 0.06643(3) 0.74374(6) 0.0492(3) Uani 1 d . . O1 O 0.4542(2) 0.11739(7) 0.66505(13) 0.0488(5) Uani 1 d . . C1 C 0.3146(3) 0.13629(10) 0.6472(2) 0.0430(6) Uani 1 d . . C2 C 0.1871(3) 0.10229(11) 0.6558(2) 0.0449(6) Uani 1 d . . C3 C 0.0432(3) 0.12408(11) 0.6342(2) 0.0511(7) Uani 1 d . . H3A H -0.0410(3) 0.10108(11) 0.6392(2) 0.061 Uiso 1 calc R . C4 C 0.0209(3) 0.17786(12) 0.6061(2) 0.0551(7) Uani 1 d . . C5 C 0.1473(3) 0.21062(11) 0.5983(2) 0.0507(7) Uani 1 d . . H5A H 0.1343(3) 0.24748(11) 0.5789(2) 0.061 Uiso 1 calc R . C6 C 0.2915(3) 0.19107(10) 0.6178(2) 0.0439(6) Uani 1 d . . C7 C 0.2000(3) 0.04515(11) 0.6829(2) 0.0475(6) Uani 1 d . . H7A H 0.1126(3) 0.02313(11) 0.6764(2) 0.057 Uiso 1 calc R . N7 N 0.3212(3) 0.02152(9) 0.71532(15) 0.0461(5) Uani 1 d . . C8 C 0.4227(3) 0.22765(11) 0.6136(2) 0.0498(7) Uani 1 d . . H8A H 0.5193(3) 0.21204(11) 0.6229(2) 0.060 Uiso 1 calc R . N8 N 0.4115(3) 0.27899(9) 0.5982(2) 0.0523(6) Uani 1 d . . C9 C -0.1357(4) 0.20124(15) 0.5846(3) 0.0843(12) Uani 1 d . . H9A H -0.1571(4) 0.20180(15) 0.5236(3) 0.126 Uiso 1 d R . H9B H -0.1410(4) 0.23886(15) 0.6066(3) 0.126 Uiso 1 d R . H9C H -0.2091(4) 0.17799(15) 0.6099(3) 0.126 Uiso 1 d R . C10 C 0.3189(3) -0.03772(10) 0.7342(2) 0.0472(6) Uani 1 d . . C11 C 0.2734(3) -0.05582(11) 0.8123(2) 0.0474(6) Uani 1 d . . C12 C 0.2805(3) -0.11262(12) 0.8289(2) 0.0562(7) Uani 1 d . . H12A H 0.2507(3) -0.12609(12) 0.8807(2) 0.067 Uiso 1 calc R . C13 C 0.3302(4) -0.14955(12) 0.7709(2) 0.0642(9) Uani 1 d . . H13A H 0.3348(4) -0.18781(12) 0.7836(2) 0.077 Uiso 1 calc R . C14 C 0.3735(4) -0.13070(12) 0.6940(2) 0.0654(8) Uani 1 d . . H14A H 0.4073(4) -0.15634(12) 0.6548(2) 0.078 Uiso 1 calc R . C15 C 0.3676(4) -0.07455(12) 0.6740(2) 0.0560(7) Uani 1 d . . C16 C 0.2125(3) -0.01626(12) 0.8753(2) 0.0545(7) Uani 1 d . . H16A H 0.2344(3) 0.02228(12) 0.8577(2) 0.065 Uiso 1 calc R . C17 C 0.0411(4) -0.0227(2) 0.8747(3) 0.0728(9) Uani 1 d . . H17A H 0.0029(4) 0.0029(2) 0.9153(3) 0.109 Uiso 1 calc R . H17B H 0.0169(4) -0.0606(2) 0.8898(3) 0.109 Uiso 1 calc R . H17C H -0.0049(4) -0.0143(2) 0.8186(3) 0.109 Uiso 1 calc R . C18 C 0.2854(5) -0.0249(2) 0.9649(2) 0.0762(10) Uani 1 d . . H18A H 0.2431(5) 0.0013(2) 1.0031(2) 0.114 Uiso 1 calc R . H18B H 0.3931(5) -0.0189(2) 0.9653(2) 0.114 Uiso 1 calc R . H18C H 0.2665(5) -0.0627(2) 0.9832(2) 0.114 Uiso 1 calc R . C19 C 0.4056(5) -0.05494(14) 0.5866(2) 0.0718(9) Uani 1 d . . H19A H 0.4381(5) -0.01557(14) 0.5922(2) 0.086 Uiso 1 calc R . C20 C 0.5330(7) -0.0871(2) 0.5513(3) 0.107(2) Uani 1 d . . H20A H 0.5510(7) -0.0725(2) 0.4959(3) 0.160 Uiso 1 calc R . H20B H 0.5059(7) -0.1262(2) 0.5463(3) 0.160 Uiso 1 calc R . H20C H 0.6234(7) -0.0832(2) 0.5890(3) 0.160 Uiso 1 calc R . C21 C 0.2625(7) -0.0561(2) 0.5262(3) 0.112(2) Uani 1 d . . H21A H 0.1837(7) -0.0352(2) 0.5508(3) 0.168 Uiso 1 calc R . H21B H 0.2302(7) -0.0944(2) 0.5170(3) 0.168 Uiso 1 calc R . H21C H 0.2832(7) -0.0395(2) 0.4725(3) 0.168 Uiso 1 calc R . C22 C 0.5457(3) 0.31129(11) 0.6008(2) 0.0549(7) Uani 1 d . . C23 C 0.5940(4) 0.33063(13) 0.5242(2) 0.0660(9) Uani 1 d . . C24 C 0.7232(5) 0.3634(2) 0.5276(3) 0.0835(11) Uani 1 d . . H24A H 0.7588(5) 0.3763(2) 0.4770(3) 0.100 Uiso 1 calc R . C25 C 0.7998(4) 0.3772(2) 0.6033(3) 0.0863(12) Uani 1 d . . H25A H 0.8873(4) 0.3991(2) 0.6038(3) 0.104 Uiso 1 calc R . C26 C 0.7492(4) 0.3592(2) 0.6779(3) 0.0796(11) Uani 1 d . . H26A H 0.8026(4) 0.3691(2) 0.7292(3) 0.095 Uiso 1 calc R . C27 C 0.6204(4) 0.32652(12) 0.6793(2) 0.0638(8) Uani 1 d . . C28 C 0.5109(4) 0.31485(15) 0.4405(3) 0.0745(10) Uani 1 d D . H28A H 0.4107(4) 0.30121(15) 0.4539(3) 0.089 Uiso 0.65 calc PR 1 H28B H 0.4473(4) 0.28325(15) 0.4538(3) 0.089 Uiso 0.35 d PR 2 C29 C 0.5833(11) 0.2690(3) 0.4017(6) 0.113(3) Uani 0.65 d PD 1 H29A H 0.5281(11) 0.2597(3) 0.3484(6) 0.169 Uiso 0.65 calc PR 1 H29B H 0.5852(11) 0.2369(3) 0.4391(6) 0.169 Uiso 0.65 calc PR 1 H29C H 0.6855(11) 0.2794(3) 0.3916(6) 0.169 Uiso 0.65 calc PR 1 C30 C 0.4822(9) 0.3656(2) 0.3811(4) 0.077(2) Uani 0.65 d PD 1 H30A H 0.4334(9) 0.3950(2) 0.4110(4) 0.115 Uiso 0.65 calc PR 1 H30B H 0.4179(9) 0.3546(2) 0.3318(4) 0.115 Uiso 0.65 calc PR 1 H30C H 0.5773(9) 0.3792(2) 0.3635(4) 0.115 Uiso 0.65 calc PR 1 C29' C 0.6266(22) 0.2928(8) 0.3726(13) 0.133(8) Uiso 0.35 d PD 2 H29D H 0.6972(22) 0.2666(8) 0.4002(13) 0.199 Uiso 0.35 calc PR 2 H29E H 0.6813(22) 0.3242(8) 0.3517(13) 0.199 Uiso 0.35 calc PR 2 H29F H 0.5700(22) 0.2746(8) 0.3257(13) 0.199 Uiso 0.35 calc PR 2 C30' C 0.4091(22) 0.3528(9) 0.4000(14) 0.145(8) Uiso 0.35 d PD 2 H30D H 0.3655(22) 0.3367(9) 0.3476(14) 0.218 Uiso 0.35 calc PR 2 H30E H 0.4616(22) 0.3870(9) 0.3879(14) 0.218 Uiso 0.35 calc PR 2 H30F H 0.3299(22) 0.3611(9) 0.4367(14) 0.218 Uiso 0.35 calc PR 2 C31 C 0.5651(5) 0.3087(2) 0.7638(3) 0.0765(10) Uani 1 d . . H31A H 0.4629(5) 0.2930(2) 0.7521(3) 0.092 Uiso 1 calc R . C32 C 0.5530(6) 0.3578(2) 0.8248(3) 0.1015(14) Uani 1 d . . H32A H 0.4897(6) 0.3866(2) 0.7976(3) 0.152 Uiso 1 calc R . H32B H 0.6524(6) 0.3729(2) 0.8400(3) 0.152 Uiso 1 calc R . H32C H 0.5090(6) 0.3451(2) 0.8755(3) 0.152 Uiso 1 calc R . C33 C 0.6635(7) 0.2631(2) 0.8049(4) 0.123(2) Uani 1 d . . H33A H 0.6257(7) 0.2526(2) 0.8584(4) 0.185 Uiso 1 calc R . H33B H 0.7659(7) 0.2766(2) 0.8148(4) 0.185 Uiso 1 calc R . H33C H 0.6618(7) 0.2309(2) 0.7678(4) 0.185 Uiso 1 calc R . C34 C 0.4924(5) 0.0999(2) 0.8549(2) 0.0785(10) Uani 1 d . . H34A H 0.3971(5) 0.1193(2) 0.8564(2) 0.118 Uiso 1 calc R . H34B H 0.5743(5) 0.1262(2) 0.8659(2) 0.118 Uiso 1 calc R . H34C H 0.4994(5) 0.0710(2) 0.8978(2) 0.118 Uiso 1 calc R . C35 C 0.6856(4) 0.02495(15) 0.7234(3) 0.0740(10) Uani 1 d . . H35A H 0.6771(4) 0.01063(15) 0.6660(3) 0.111 Uiso 1 calc R . H35B H 0.6975(4) -0.00587(15) 0.7630(3) 0.111 Uiso 1 calc R . H35C H 0.7723(4) 0.04934(15) 0.7311(3) 0.111 Uiso 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 0.0449(4) 0.0394(4) 0.0623(5) 0.0111(4) -0.0020(3) 0.0009(3) O1 0.0420(10) 0.0352(9) 0.0688(12) 0.0124(8) 0.0020(8) 0.0020(7) C1 0.0415(13) 0.0351(13) 0.0521(15) 0.0012(11) 0.0010(11) 0.0026(10) C2 0.0435(14) 0.0344(13) 0.056(2) 0.0040(11) 0.0002(11) -0.0005(10) C3 0.0430(14) 0.0420(15) 0.068(2) 0.0031(13) -0.0003(12) -0.0027(11) C4 0.0441(15) 0.0412(15) 0.079(2) 0.0011(14) -0.0033(13) 0.0063(12) C5 0.054(2) 0.0319(13) 0.066(2) 0.0005(12) -0.0013(13) 0.0062(11) C6 0.0439(13) 0.0304(12) 0.057(2) 0.0009(11) 0.0033(11) 0.0014(10) C7 0.0475(15) 0.0368(13) 0.058(2) 0.0054(11) -0.0007(12) -0.0041(11) N7 0.0511(13) 0.0327(11) 0.0537(13) 0.0068(9) -0.0003(10) -0.0005(9) C8 0.0451(14) 0.0326(14) 0.071(2) 0.0055(12) 0.0018(12) 0.0033(11) N8 0.0483(13) 0.0300(11) 0.078(2) 0.0043(10) -0.0002(11) 0.0014(9) C9 0.048(2) 0.055(2) 0.147(4) 0.009(2) -0.009(2) 0.0113(14) C10 0.0458(14) 0.0330(13) 0.061(2) 0.0071(12) -0.0046(12) -0.0005(11) C11 0.0457(14) 0.0366(13) 0.059(2) 0.0071(12) -0.0013(12) -0.0049(10) C12 0.055(2) 0.044(2) 0.069(2) 0.0136(14) -0.0003(14) -0.0021(12) C13 0.070(2) 0.0345(15) 0.087(2) 0.0150(15) 0.001(2) 0.0029(13) C14 0.080(2) 0.038(2) 0.078(2) 0.0002(14) 0.007(2) 0.0051(14) C15 0.067(2) 0.0384(14) 0.062(2) 0.0040(13) 0.0016(14) 0.0020(13) C16 0.060(2) 0.0436(15) 0.060(2) 0.0068(13) 0.0044(13) -0.0055(12) C17 0.062(2) 0.069(2) 0.089(3) 0.002(2) 0.011(2) 0.007(2) C18 0.082(2) 0.080(2) 0.066(2) 0.001(2) -0.001(2) -0.009(2) C19 0.108(3) 0.048(2) 0.060(2) 0.0032(14) 0.010(2) 0.001(2) C20 0.157(5) 0.079(3) 0.092(3) 0.005(2) 0.054(3) 0.021(3) C21 0.166(5) 0.100(3) 0.065(3) 0.009(2) -0.021(3) -0.011(3) C22 0.0474(15) 0.0289(13) 0.087(2) 0.0055(13) -0.0013(14) -0.0004(11) C23 0.064(2) 0.045(2) 0.089(2) 0.007(2) 0.004(2) -0.0103(14) C24 0.076(2) 0.061(2) 0.115(3) 0.012(2) 0.015(2) -0.018(2) C25 0.060(2) 0.066(2) 0.131(4) 0.003(2) -0.002(2) -0.019(2) C26 0.064(2) 0.058(2) 0.113(3) 0.000(2) -0.019(2) -0.006(2) C27 0.054(2) 0.042(2) 0.092(2) 0.006(2) -0.013(2) 0.0016(13) C28 0.077(2) 0.061(2) 0.085(2) 0.013(2) 0.004(2) -0.015(2) C29 0.137(7) 0.060(4) 0.135(7) -0.037(5) -0.032(6) 0.030(5) C30 0.101(5) 0.051(3) 0.079(4) 0.009(3) 0.011(3) 0.010(3) C31 0.078(2) 0.065(2) 0.083(2) 0.006(2) -0.017(2) 0.001(2) C32 0.101(3) 0.102(3) 0.098(3) -0.020(3) -0.016(3) -0.006(3) C33 0.140(5) 0.110(4) 0.116(4) 0.040(3) -0.013(3) 0.031(3) C34 0.087(3) 0.079(2) 0.068(2) 0.001(2) -0.001(2) -0.021(2) C35 0.057(2) 0.061(2) 0.103(3) 0.023(2) 0.004(2) 0.011(2) _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 O1 1.779(2) . ? Al C35 1.940(3) . ? Al C34 1.948(4) . ? Al N7 1.984(2) . ? O1 C1 1.334(3) . ? C1 C6 1.404(4) . ? C1 C2 1.415(4) . ? C2 C3 1.402(4) . ? C2 C7 1.438(4) . ? C3 C4 1.374(4) . ? C4 C5 1.388(4) . ? C4 C9 1.518(4) . ? C5 C6 1.381(4) . ? C6 C8 1.468(4) . ? C7 N7 1.290(4) . ? N7 C10 1.453(3) . ? C8 N8 1.258(3) . ? N8 C22 1.424(4) . ? C10 C15 1.395(4) . ? C10 C11 1.403(4) . ? C11 C12 1.388(4) . ? C11 C16 1.509(4) . ? C12 C13 1.375(5) . ? C13 C14 1.383(5) . ? C14 C15 1.384(4) . ? C15 C19 1.526(4) . ? C16 C18 1.529(5) . ? C16 C17 1.535(4) . ? C19 C20 1.516(6) . ? C19 C21 1.534(6) . ? C22 C23 1.398(5) . ? C22 C27 1.412(5) . ? C23 C24 1.391(5) . ? C23 C28 1.516(5) . ? C24 C25 1.373(6) . ? C25 C26 1.368(6) . ? C26 C27 1.392(5) . ? C27 C31 1.525(5) . ? C28 C30' 1.41(2) . ? C28 C29 1.438(7) . ? C28 C30 1.548(6) . ? C28 C29' 1.64(2) . ? C31 C33 1.516(6) . ? C31 C32 1.534(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 O1 Al C35 113.89(14) . . ? O1 Al C34 108.71(15) . . ? C35 Al C34 118.0(2) . . ? O1 Al N7 93.07(9) . . ? C35 Al N7 111.42(14) . . ? C34 Al N7 108.83(14) . . ? C1 O1 Al 124.3(2) . . ? O1 C1 C6 119.9(2) . . ? O1 C1 C2 121.8(2) . . ? C6 C1 C2 118.3(2) . . ? C3 C2 C1 119.2(2) . . ? C3 C2 C7 118.6(2) . . ? C1 C2 C7 122.2(2) . . ? C4 C3 C2 122.4(3) . . ? C3 C4 C5 117.6(3) . . ? C3 C4 C9 121.8(3) . . ? C5 C4 C9 120.6(3) . . ? C6 C5 C4 122.4(3) . . ? C5 C6 C1 120.1(2) . . ? C5 C6 C8 121.2(2) . . ? C1 C6 C8 118.6(2) . . ? N7 C7 C2 125.6(2) . . ? C7 N7 C10 119.1(2) . . ? C7 N7 Al 120.2(2) . . ? C10 N7 Al 120.6(2) . . ? N8 C8 C6 122.9(3) . . ? C8 N8 C22 118.3(2) . . ? C15 C10 C11 122.4(2) . . ? C15 C10 N7 117.9(3) . . ? C11 C10 N7 119.6(2) . . ? C12 C11 C10 117.3(3) . . ? C12 C11 C16 120.4(3) . . ? C10 C11 C16 122.3(2) . . ? C13 C12 C11 121.2(3) . . ? C12 C13 C14 120.4(3) . . ? C13 C14 C15 120.8(3) . . ? C14 C15 C10 117.9(3) . . ? C14 C15 C19 120.0(3) . . ? C10 C15 C19 122.0(3) . . ? C11 C16 C18 112.3(3) . . ? C11 C16 C17 110.0(3) . . ? C18 C16 C17 110.0(3) . . ? C20 C19 C15 113.9(3) . . ? C20 C19 C21 111.8(4) . . ? C15 C19 C21 109.1(4) . . ? C23 C22 C27 121.5(3) . . ? C23 C22 N8 118.1(3) . . ? C27 C22 N8 120.2(3) . . ? C24 C23 C22 117.7(4) . . ? C24 C23 C28 121.4(4) . . ? C22 C23 C28 120.9(3) . . ? C25 C24 C23 121.6(4) . . ? C26 C25 C24 120.2(4) . . ? C25 C26 C27 121.3(4) . . ? C26 C27 C22 117.6(4) . . ? C26 C27 C31 119.8(3) . . ? C22 C27 C31 122.6(3) . . ? C30' C28 C23 119.4(10) . . ? C29 C28 C23 111.1(4) . . ? C29 C28 C30 113.7(6) . . ? C23 C28 C30 112.4(4) . . ? C30' C28 C29' 109.1(11) . . ? C23 C28 C29' 111.5(9) . . ? C33 C31 C27 111.3(4) . . ? C33 C31 C32 110.5(4) . . ? C27 C31 C32 112.5(3) . . ? _refine_diff_density_max 0.319 _refine_diff_density_min -0.218 _refine_diff_density_rms 0.045 #===END data_Compound_2 _database_code_depnum_ccdc_archive 'CCDC 233654' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C38 H56 N2 O Al2' _chemical_formula_weight 610.81 _chemical_melting_point ? _chemical_compound_source ? 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' O O 0.0492 0.0322 '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 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 12.2387(7) _cell_length_b 16.1335(10) _cell_length_c 19.3515(9) _cell_angle_alpha 90.00 _cell_angle_beta 94.321(4) _cell_angle_gamma 90.00 _cell_volume 3810.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 10.73 _cell_measurement_theta_max 28.02 _exptl_crystal_description prisms _exptl_crystal_colour Orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.065 _exptl_crystal_density_method ? _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.897 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5961 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 62.00 _reflns_number_total 5961 _reflns_number_observed 5059 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 238 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1455P)^2^+0.9752P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0016(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5723 _refine_ls_number_parameters 390 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0776 _refine_ls_R_factor_obs 0.0670 _refine_ls_wR_factor_all 0.1938 _refine_ls_wR_factor_obs 0.1801 _refine_ls_goodness_of_fit_all 1.026 _refine_ls_goodness_of_fit_obs 1.055 _refine_ls_restrained_S_all 1.042 _refine_ls_restrained_S_obs 1.055 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Al1 Al 0.82716(5) 0.27931(4) 0.16985(4) 0.0294(2) Uani 1 d . . Al2 Al 0.58430(5) 0.27465(4) 0.21897(4) 0.0273(2) Uani 1 d . . O1 O 0.68743(12) 0.33403(9) 0.17395(8) 0.0247(4) Uani 1 d . . C1 C 0.6564(2) 0.40606(13) 0.13828(11) 0.0230(5) Uani 1 d . . C2 C 0.7094(2) 0.43132(15) 0.08051(12) 0.0258(5) Uani 1 d . . C3 C 0.6735(2) 0.5041(2) 0.04707(12) 0.0291(5) Uani 1 d . . H3A H 0.7089(2) 0.5209(2) 0.00735(12) 0.035 Uiso 1 calc R . C4 C 0.5894(2) 0.55335(14) 0.06815(12) 0.0281(5) Uani 1 d . . C5 C 0.5404(2) 0.52881(14) 0.12673(13) 0.0291(5) Uani 1 d . . H5A H 0.4837(2) 0.56196(14) 0.14328(13) 0.035 Uiso 1 calc R . C6 C 0.5725(2) 0.45571(14) 0.16253(12) 0.0249(5) Uani 1 d . . N7 N 0.8796(2) 0.34734(12) 0.10475(10) 0.0283(4) Uani 1 d . . C7 C 0.8048(2) 0.3867(2) 0.05107(12) 0.0312(5) Uani 1 d . . H7A H 0.8483(2) 0.4297(2) 0.02808(12) 0.037 Uiso 1 calc R . C8 C 0.7625(2) 0.3264(2) -0.0053(2) 0.0459(7) Uani 1 d . . H8A H 0.8246(2) 0.2979(2) -0.0240(2) 0.069 Uiso 1 calc R . H8B H 0.7215(2) 0.3569(2) -0.0426(2) 0.069 Uiso 1 calc R . H8C H 0.7143(2) 0.2855(2) 0.0143(2) 0.069 Uiso 1 calc R . N9 N 0.53276(15) 0.37500(12) 0.26360(10) 0.0259(4) Uani 1 d . . C9 C 0.5260(2) 0.44292(14) 0.22795(13) 0.0281(5) Uani 1 d . . H9A H 0.4873(2) 0.48788(14) 0.24634(13) 0.034 Uiso 1 calc R . C10 C 0.5567(2) 0.6323(2) 0.03004(15) 0.0383(6) Uani 1 d . . H10A H 0.6223(3) 0.6654(6) 0.0234(10) 0.057 Uiso 1 calc R . H10B H 0.5069(14) 0.6642(7) 0.0572(5) 0.057 Uiso 1 calc R . H10C H 0.5197(16) 0.6186(2) -0.0152(5) 0.057 Uiso 1 calc R . C11 C 0.9108(2) 0.2903(2) 0.2601(2) 0.0453(7) Uani 1 d . . H11A H 0.8803(2) 0.2529(2) 0.2936(2) 0.068 Uiso 1 calc R . H11B H 0.9063(2) 0.3476(2) 0.2765(2) 0.068 Uiso 1 calc R . H11C H 0.9877(2) 0.2758(2) 0.2553(2) 0.068 Uiso 1 calc R . C12 C 0.7757(3) 0.1669(2) 0.1412(2) 0.0475(7) Uani 1 d . . H12A H 0.7500(3) 0.1376(2) 0.1813(2) 0.071 Uiso 1 calc R . H12B H 0.8363(3) 0.1359(2) 0.1231(2) 0.071 Uiso 1 calc R . H12C H 0.7155(3) 0.1716(2) 0.1051(2) 0.071 Uiso 1 calc R . C13 C 0.6421(2) 0.2029(2) 0.2943(2) 0.0436(7) Uani 1 d . . H13A H 0.6982(2) 0.2328(2) 0.3233(2) 0.065 Uiso 1 calc R . H13B H 0.6746(2) 0.1533(2) 0.2750(2) 0.065 Uiso 1 calc R . H13C H 0.5825(2) 0.1865(2) 0.3226(2) 0.065 Uiso 1 calc R . C14 C 0.4708(2) 0.2369(2) 0.1503(2) 0.0484(7) Uani 1 d . . H14A H 0.4528(2) 0.2815(2) 0.1170(2) 0.073 Uiso 1 calc R . H14B H 0.4051(2) 0.2217(2) 0.1735(2) 0.073 Uiso 1 calc R . H14C H 0.4972(2) 0.1885(2) 0.1259(2) 0.073 Uiso 1 calc R . C15 C 0.9917(2) 0.3699(2) 0.10343(12) 0.0301(5) Uani 1 d . . C16 C 1.0689(2) 0.3102(2) 0.08491(14) 0.0374(6) Uani 1 d . . C17 C 1.1796(2) 0.3313(2) 0.0885(2) 0.0473(8) Uani 1 d . . H17A H 1.2318(2) 0.2908(2) 0.0775(2) 0.057 Uiso 1 calc R . C18 C 1.2148(2) 0.4094(2) 0.1077(2) 0.0523(8) Uani 1 d . . H18A H 1.2907(2) 0.4224(2) 0.1098(2) 0.063 Uiso 1 calc R . C19 C 1.1399(2) 0.4689(2) 0.12377(15) 0.0458(7) Uani 1 d . . H19A H 1.1647(2) 0.5232(2) 0.13547(15) 0.055 Uiso 1 calc R . C20 C 1.0285(2) 0.4506(2) 0.12318(13) 0.0355(6) Uani 1 d . . C21 C 1.0349(2) 0.2234(2) 0.0616(2) 0.0456(7) Uani 1 d . . H21A H 0.9532(2) 0.2227(2) 0.0541(2) 0.055 Uiso 1 calc R . C22 C 1.0676(4) 0.1611(2) 0.1190(2) 0.0749(12) Uani 1 d . . H22A H 1.0454(4) 0.1053(2) 0.1037(2) 0.112 Uiso 1 calc R . H22B H 1.0311(4) 0.1755(2) 0.1608(2) 0.112 Uiso 1 calc R . H22C H 1.1472(4) 0.1627(2) 0.1293(2) 0.112 Uiso 1 calc R . C23 C 1.0809(4) 0.1981(3) -0.0064(3) 0.0819(13) Uani 1 d . . H23A H 1.0564(4) 0.1418(3) -0.0188(3) 0.123 Uiso 1 calc R . H23B H 1.1611(4) 0.1995(3) -0.0010(3) 0.123 Uiso 1 calc R . H23C H 1.0547(4) 0.2366(3) -0.0431(3) 0.123 Uiso 1 calc R . C24 C 0.9504(2) 0.5164(2) 0.1454(2) 0.0412(6) Uani 1 d . . H24A H 0.8755(2) 0.4913(2) 0.1433(2) 0.049 Uiso 1 calc R . C25 C 0.9456(3) 0.5907(2) 0.0963(2) 0.0629(9) Uani 1 d . . H25A H 0.8944(3) 0.6320(2) 0.1122(2) 0.094 Uiso 1 calc R . H25B H 0.9206(3) 0.5723(2) 0.0495(2) 0.094 Uiso 1 calc R . H25C H 1.0186(3) 0.6153(2) 0.0957(2) 0.094 Uiso 1 calc R . C26 C 0.9788(3) 0.5437(2) 0.2203(2) 0.0640(9) Uani 1 d . . H26A H 0.9268(3) 0.5863(2) 0.2330(2) 0.096 Uiso 1 calc R . H26B H 1.0533(3) 0.5665(2) 0.2246(2) 0.096 Uiso 1 calc R . H26C H 0.9747(3) 0.4959(2) 0.2512(2) 0.096 Uiso 1 calc R . C27 C 0.5012(2) 0.37737(14) 0.33435(12) 0.0297(5) Uani 1 d . . C28 C 0.5829(2) 0.3987(2) 0.38611(14) 0.0360(6) Uani 1 d . . C29 C 0.5541(3) 0.3996(2) 0.4539(2) 0.0486(7) Uani 1 d . . H29A H 0.6077(3) 0.4137(2) 0.4901(2) 0.058 Uiso 1 calc R . C30 C 0.4492(3) 0.3803(2) 0.4701(2) 0.0544(8) Uani 1 d . . H30A H 0.4310(3) 0.3813(2) 0.5170(2) 0.065 Uiso 1 calc R . C31 C 0.3707(3) 0.3597(2) 0.4179(2) 0.0506(8) Uani 1 d . . H31A H 0.2986(3) 0.3467(2) 0.4295(2) 0.061 Uiso 1 calc R . C32 C 0.3947(2) 0.3574(2) 0.34900(14) 0.0382(6) Uani 1 d . . C33 C 0.6970(2) 0.4225(2) 0.3675(2) 0.0423(6) Uani 1 d . . H33A H 0.7114(2) 0.3922(2) 0.3240(2) 0.051 Uiso 1 calc R . C34 C 0.7869(3) 0.3984(3) 0.4227(2) 0.0710(11) Uani 1 d . . H34A H 0.8583(3) 0.4154(3) 0.4077(2) 0.107 Uiso 1 calc R . H34B H 0.7863(3) 0.3382(3) 0.4294(2) 0.107 Uiso 1 calc R . H34C H 0.7740(3) 0.4261(3) 0.4664(2) 0.107 Uiso 1 calc R . C35 C 0.7040(3) 0.5158(2) 0.3522(2) 0.0670(10) Uani 1 d . . H35A H 0.7783(3) 0.5295(2) 0.3403(2) 0.101 Uiso 1 calc R . H35B H 0.6867(3) 0.5474(2) 0.3932(2) 0.101 Uiso 1 calc R . H35C H 0.6516(3) 0.5299(2) 0.3132(2) 0.101 Uiso 1 calc R . C36 C 0.3065(2) 0.3341(2) 0.2936(2) 0.0522(8) Uani 1 d . . H36A H 0.3378(2) 0.3405(2) 0.2476(2) 0.063 Uiso 1 calc R . C37 C 0.2076(3) 0.3919(4) 0.2947(2) 0.088(2) Uani 1 d . . H37A H 0.1518(3) 0.3754(4) 0.2583(2) 0.133 Uiso 1 calc R . H37B H 0.2306(3) 0.4490(4) 0.2866(2) 0.133 Uiso 1 calc R . H37C H 0.1769(3) 0.3883(4) 0.3399(2) 0.133 Uiso 1 calc R . C38 C 0.2731(4) 0.2444(3) 0.3010(3) 0.092(2) Uani 1 d . . H38A H 0.2160(4) 0.2305(3) 0.2646(3) 0.138 Uiso 1 calc R . H38B H 0.2449(4) 0.2359(3) 0.3465(3) 0.138 Uiso 1 calc R . H38C H 0.3369(4) 0.2085(3) 0.2966(3) 0.138 Uiso 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 0.0238(4) 0.0241(4) 0.0402(4) 0.0088(3) 0.0018(3) 0.0085(3) Al2 0.0251(4) 0.0195(4) 0.0368(4) 0.0048(3) -0.0011(3) -0.0026(2) O1 0.0202(7) 0.0193(7) 0.0342(8) 0.0089(6) 0.0000(6) 0.0055(6) C1 0.0200(10) 0.0189(10) 0.0291(11) 0.0056(8) -0.0045(8) 0.0014(8) C2 0.0208(10) 0.0271(11) 0.0287(11) 0.0056(9) -0.0047(8) 0.0048(9) C3 0.0250(11) 0.0318(12) 0.0302(11) 0.0097(10) -0.0011(9) 0.0047(9) C4 0.0248(11) 0.0233(11) 0.0355(12) 0.0077(9) -0.0027(9) 0.0043(9) C5 0.0247(11) 0.0227(11) 0.0399(13) 0.0048(9) 0.0027(9) 0.0071(9) C6 0.0215(10) 0.0211(10) 0.0317(11) 0.0040(9) -0.0007(8) 0.0028(8) N7 0.0203(9) 0.0293(10) 0.0350(10) 0.0085(8) 0.0009(8) 0.0097(8) C7 0.0277(12) 0.0344(12) 0.0314(12) 0.0073(10) 0.0009(9) 0.0117(10) C8 0.0440(15) 0.050(2) 0.0426(15) -0.0088(13) -0.0014(12) 0.0136(13) N9 0.0204(9) 0.0249(9) 0.0324(10) 0.0054(8) 0.0017(7) -0.0014(7) C9 0.0211(10) 0.0259(11) 0.0374(12) 0.0038(9) 0.0034(9) 0.0011(8) C10 0.0376(13) 0.0293(13) 0.0475(15) 0.0171(11) 0.0007(11) 0.0100(10) C11 0.0322(13) 0.052(2) 0.050(2) 0.0149(13) -0.0040(11) 0.0069(12) C12 0.051(2) 0.0277(13) 0.065(2) 0.0024(12) 0.0119(14) 0.0067(12) C13 0.0435(15) 0.0329(13) 0.054(2) 0.0185(12) 0.0034(12) 0.0014(11) C14 0.0375(15) 0.046(2) 0.060(2) -0.0070(13) -0.0070(13) -0.0086(12) C15 0.0228(11) 0.0339(13) 0.0337(12) 0.0130(10) 0.0019(9) 0.0079(9) C16 0.0311(13) 0.0432(15) 0.0386(13) 0.0156(11) 0.0064(10) 0.0155(11) C17 0.0257(13) 0.069(2) 0.048(2) 0.0233(15) 0.0093(11) 0.0190(13) C18 0.0230(13) 0.085(2) 0.048(2) 0.027(2) 0.0014(11) 0.0045(14) C19 0.0354(14) 0.059(2) 0.0424(15) 0.0156(13) -0.0039(11) -0.0086(13) C20 0.0296(12) 0.0432(14) 0.0332(12) 0.0094(11) -0.0018(9) 0.0031(11) C21 0.0386(15) 0.0369(15) 0.063(2) 0.0114(13) 0.0153(13) 0.0198(11) C22 0.077(3) 0.049(2) 0.098(3) 0.031(2) 0.002(2) 0.028(2) C23 0.089(3) 0.065(2) 0.097(3) -0.015(2) 0.045(3) 0.015(2) C24 0.0385(14) 0.0360(14) 0.048(2) -0.0014(12) -0.0029(11) 0.0006(11) C25 0.068(2) 0.044(2) 0.077(2) 0.012(2) 0.004(2) 0.015(2) C26 0.068(2) 0.063(2) 0.060(2) -0.014(2) -0.003(2) 0.003(2) C27 0.0318(12) 0.0258(11) 0.0316(12) 0.0065(9) 0.0032(9) 0.0018(9) C28 0.0417(14) 0.0294(12) 0.0366(13) -0.0011(10) 0.0006(11) -0.0009(11) C29 0.058(2) 0.048(2) 0.0383(14) -0.0008(12) -0.0039(12) 0.0007(14) C30 0.071(2) 0.058(2) 0.0357(15) 0.0077(14) 0.0148(14) 0.008(2) C31 0.044(2) 0.061(2) 0.049(2) 0.0162(14) 0.0150(13) 0.0033(14) C32 0.0324(13) 0.0430(15) 0.0400(14) 0.0125(11) 0.0070(11) 0.0011(11) C33 0.0380(14) 0.0397(15) 0.048(2) -0.0066(12) -0.0032(12) -0.0096(11) C34 0.048(2) 0.094(3) 0.068(2) 0.003(2) -0.017(2) -0.010(2) C35 0.065(2) 0.046(2) 0.091(3) -0.006(2) 0.007(2) -0.027(2) C36 0.0280(13) 0.080(2) 0.048(2) 0.017(2) 0.0025(12) -0.0102(14) C37 0.042(2) 0.151(5) 0.071(2) 0.027(3) -0.002(2) 0.026(2) C38 0.078(3) 0.101(4) 0.091(3) 0.021(3) -0.025(2) -0.054(3) _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 N7 1.824(2) . ? Al1 O1 1.931(2) . ? Al1 C11 1.965(3) . ? Al1 C12 1.985(3) . ? Al2 O1 1.854(2) . ? Al2 C14 1.947(3) . ? Al2 C13 1.952(3) . ? Al2 N9 1.961(2) . ? O1 C1 1.390(3) . ? C1 C2 1.395(3) . ? C1 C6 1.410(3) . ? C2 C3 1.395(3) . ? C2 C7 1.519(3) . ? C3 C4 1.385(3) . ? C4 C5 1.380(3) . ? C4 C10 1.511(3) . ? C5 C6 1.409(3) . ? C6 C9 1.442(3) . ? N7 C15 1.421(3) . ? N7 C7 1.476(3) . ? C7 C8 1.523(4) . ? N9 C9 1.294(3) . ? N9 C27 1.451(3) . ? C15 C16 1.414(4) . ? C15 C20 1.421(4) . ? C16 C17 1.392(4) . ? C16 C21 1.520(4) . ? C17 C18 1.373(5) . ? C18 C19 1.379(5) . ? C19 C20 1.394(4) . ? C20 C24 1.514(4) . ? C21 C23 1.526(5) . ? C21 C22 1.528(4) . ? C24 C25 1.527(4) . ? C24 C26 1.529(4) . ? C27 C32 1.393(4) . ? C27 C28 1.404(4) . ? C28 C29 1.385(4) . ? C28 C33 1.517(4) . ? C29 C30 1.380(5) . ? C30 C31 1.381(5) . ? C31 C32 1.387(4) . ? C32 C36 1.510(4) . ? C33 C34 1.525(4) . ? C33 C35 1.537(4) . ? C36 C38 1.514(6) . ? C36 C37 1.530(5) . ? 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 N7 Al1 O1 96.44(8) . . ? N7 Al1 C11 111.89(12) . . ? O1 Al1 C11 109.03(10) . . ? N7 Al1 C12 118.54(12) . . ? O1 Al1 C12 99.56(10) . . ? C11 Al1 C12 117.60(14) . . ? O1 Al2 C14 108.49(12) . . ? O1 Al2 C13 115.87(10) . . ? C14 Al2 C13 121.61(14) . . ? O1 Al2 N9 91.90(8) . . ? C14 Al2 N9 108.79(11) . . ? C13 Al2 N9 105.74(12) . . ? C1 O1 Al2 119.69(13) . . ? C1 O1 Al1 124.85(13) . . ? Al2 O1 Al1 114.80(8) . . ? O1 C1 C2 121.1(2) . . ? O1 C1 C6 119.2(2) . . ? C2 C1 C6 119.7(2) . . ? C1 C2 C3 117.9(2) . . ? C1 C2 C7 125.4(2) . . ? C3 C2 C7 116.7(2) . . ? C4 C3 C2 124.1(2) . . ? C5 C4 C3 117.1(2) . . ? C5 C4 C10 121.8(2) . . ? C3 C4 C10 121.0(2) . . ? C4 C5 C6 121.5(2) . . ? C5 C6 C1 119.7(2) . . ? C5 C6 C9 116.0(2) . . ? C1 C6 C9 123.8(2) . . ? C15 N7 C7 115.2(2) . . ? C15 N7 Al1 123.84(15) . . ? C7 N7 Al1 120.9(2) . . ? N7 C7 C2 113.2(2) . . ? N7 C7 C8 112.9(2) . . ? C2 C7 C8 110.0(2) . . ? C9 N9 C27 118.0(2) . . ? C9 N9 Al2 118.3(2) . . ? C27 N9 Al2 123.68(15) . . ? N9 C9 C6 125.1(2) . . ? C16 C15 C20 119.2(2) . . ? C16 C15 N7 119.7(2) . . ? C20 C15 N7 121.1(2) . . ? C17 C16 C15 119.1(3) . . ? C17 C16 C21 118.9(2) . . ? C15 C16 C21 121.9(2) . . ? C18 C17 C16 121.5(3) . . ? C17 C18 C19 119.9(3) . . ? C18 C19 C20 121.1(3) . . ? C19 C20 C15 119.1(3) . . ? C19 C20 C24 119.2(3) . . ? C15 C20 C24 121.7(2) . . ? C16 C21 C23 113.1(3) . . ? C16 C21 C22 109.9(3) . . ? C23 C21 C22 110.9(3) . . ? C20 C24 C25 111.6(3) . . ? C20 C24 C26 111.6(3) . . ? C25 C24 C26 111.1(3) . . ? C32 C27 C28 122.6(2) . . ? C32 C27 N9 120.4(2) . . ? C28 C27 N9 117.0(2) . . ? C29 C28 C27 117.4(3) . . ? C29 C28 C33 121.8(3) . . ? C27 C28 C33 120.8(2) . . ? C30 C29 C28 121.4(3) . . ? C29 C30 C31 119.7(3) . . ? C30 C31 C32 121.6(3) . . ? C31 C32 C27 117.3(3) . . ? C31 C32 C36 119.9(3) . . ? C27 C32 C36 122.9(2) . . ? C28 C33 C34 113.4(3) . . ? C28 C33 C35 111.1(3) . . ? C34 C33 C35 109.7(3) . . ? C32 C36 C38 110.7(3) . . ? C32 C36 C37 111.2(3) . . ? C38 C36 C37 111.2(4) . . ? _refine_diff_density_max 0.534 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.071 #===END data_Compound_3 _database_code_depnum_ccdc_archive 'CCDC 233655' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C66 H82 N4 O2 Cl Al' _chemical_formula_weight 1025.79 _chemical_melting_point ? _chemical_compound_source ? 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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 '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 Monoclinic _symmetry_space_group_name_H-M Pc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 15.5342(15) _cell_length_b 8.9196(12) _cell_length_c 21.608(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.296(9) _cell_angle_gamma 90.00 _cell_volume 2994.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 26 _cell_measurement_theta_min 10.60 _cell_measurement_theta_max 24.90 _exptl_crystal_description blocks _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.138 _exptl_crystal_density_method ? _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 1.052 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4586 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0538 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 59.97 _reflns_number_total 4480 _reflns_number_observed 3870 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 109 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1092P)^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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0013(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.06(3) _refine_ls_number_reflns 4371 _refine_ls_number_parameters 668 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0752 _refine_ls_R_factor_obs 0.0616 _refine_ls_wR_factor_all 0.1592 _refine_ls_wR_factor_obs 0.1463 _refine_ls_goodness_of_fit_all 1.049 _refine_ls_goodness_of_fit_obs 1.075 _refine_ls_restrained_S_all 1.077 _refine_ls_restrained_S_obs 1.075 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Al Al 0.89358(10) -0.1860(2) 0.70930(6) 0.0242(4) Uani 1 d . . Cl Cl 0.90782(10) 0.0222(2) 0.65894(7) 0.0396(4) Uani 1 d . . O1 O 0.9584(3) -0.1573(5) 0.7781(2) 0.0290(9) Uani 1 d . . C1 C 0.9490(4) -0.0647(6) 0.8263(2) 0.0240(12) Uani 1 d . . C2 C 0.8671(4) -0.0057(6) 0.8406(2) 0.0252(11) Uani 1 d . . C3 C 0.8575(4) 0.0900(6) 0.8921(2) 0.0288(13) Uani 1 d . . H3A H 0.8022(4) 0.1292(6) 0.9014(2) 0.035 Uiso 1 calc R . C4 C 0.9260(4) 0.1277(7) 0.9292(2) 0.0301(13) Uani 1 d . . C5 C 1.0060(4) 0.0658(7) 0.9160(2) 0.0297(13) Uani 1 d . . H5A H 1.0534(4) 0.0902(7) 0.9420(2) 0.036 Uiso 1 calc R . C6 C 1.0199(4) -0.0311(6) 0.8659(2) 0.0261(12) Uani 1 d . . C7 C 0.7920(4) -0.0529(6) 0.8088(2) 0.0302(13) Uani 1 d . . H7A H 0.7386(4) -0.0173(6) 0.8241(2) 0.036 Uiso 1 calc R . N7 N 0.7888(3) -0.1412(5) 0.7602(2) 0.0291(11) Uani 1 d . . C8 C 1.1050(4) -0.0963(7) 0.8564(2) 0.0333(14) Uani 1 d . . H8A H 1.1144(4) -0.1633(7) 0.8230(2) 0.040 Uiso 1 calc R . N8 N 1.1664(4) -0.0636(7) 0.8927(2) 0.0447(14) Uani 1 d . . C9 C 0.9139(5) 0.2271(9) 0.9864(3) 0.048(2) Uani 1 d . . H9A H 0.9600(5) 0.3021(9) 0.9882(3) 0.072 Uiso 1 d R . H9B H 0.9160(5) 0.1649(9) 1.0238(3) 0.072 Uiso 1 d R . H9C H 0.8581(5) 0.2778(9) 0.9838(3) 0.072 Uiso 1 d R . C10 C 0.7025(4) -0.1978(7) 0.7471(2) 0.0325(13) Uani 1 d . . C11 C 0.6856(5) -0.3428(8) 0.7670(3) 0.0382(15) Uani 1 d . . C12 C 0.6021(5) -0.3951(10) 0.7593(3) 0.055(2) Uani 1 d . . H12A H 0.5874(5) -0.4927(10) 0.7733(3) 0.067 Uiso 1 calc R . C13 C 0.5397(5) -0.3059(11) 0.7311(4) 0.059(2) Uani 1 d . . H13A H 0.4828(5) -0.3430(11) 0.7261(4) 0.070 Uiso 1 calc R . C14 C 0.5599(5) -0.1654(10) 0.7107(3) 0.051(2) Uani 1 d . . H14A H 0.5163(5) -0.1073(10) 0.6911(3) 0.062 Uiso 1 calc R . C15 C 0.6410(4) -0.1047(8) 0.7173(3) 0.039(2) Uani 1 d . . C16 C 0.7527(6) -0.4377(8) 0.7993(3) 0.051(2) Uani 1 d . . H16A H 0.8097(6) -0.3889(8) 0.7922(3) 0.062 Uiso 1 calc R . C17 C 0.7368(8) -0.4371(12) 0.8700(4) 0.084(3) Uani 1 d . . H17A H 0.7805(8) -0.4988(12) 0.8906(4) 0.125 Uiso 1 calc R . H17B H 0.6795(8) -0.4779(12) 0.8785(4) 0.125 Uiso 1 calc R . H17C H 0.7403(8) -0.3341(12) 0.8856(4) 0.125 Uiso 1 calc R . C18 C 0.7590(7) -0.5968(10) 0.7748(4) 0.069(2) Uani 1 d . . H18A H 0.8036(7) -0.6512(10) 0.7978(4) 0.103 Uiso 1 calc R . H18B H 0.7739(7) -0.5943(10) 0.7308(4) 0.103 Uiso 1 calc R . H18C H 0.7035(7) -0.6474(10) 0.7799(4) 0.103 Uiso 1 calc R . C19 C 0.6619(5) 0.0491(8) 0.6935(3) 0.043(2) Uani 1 d . . H19A H 0.7170(5) 0.0827(8) 0.7132(3) 0.052 Uiso 1 calc R . C20 C 0.6754(6) 0.0420(10) 0.6221(3) 0.059(2) Uani 1 d . . H20A H 0.6890(6) 0.1424(10) 0.6065(3) 0.088 Uiso 1 calc R . H20B H 0.6226(6) 0.0056(10) 0.6021(3) 0.088 Uiso 1 calc R . H20C H 0.7230(6) -0.0263(10) 0.6128(3) 0.088 Uiso 1 calc R . C21 C 0.5931(6) 0.1641(10) 0.7078(4) 0.067(2) Uani 1 d . . H21A H 0.6104(6) 0.2617(10) 0.6911(4) 0.100 Uiso 1 calc R . H21B H 0.5859(6) 0.1718(10) 0.7527(4) 0.100 Uiso 1 calc R . H21C H 0.5386(6) 0.1331(10) 0.6887(4) 0.100 Uiso 1 calc R . C22 C 1.2484(5) -0.1372(10) 0.8867(3) 0.049(2) Uani 1 d . . C23 C 1.3134(5) -0.0685(12) 0.8526(3) 0.065(3) Uani 1 d . . C24 C 1.3915(6) -0.1386(15) 0.8493(4) 0.074(3) Uani 1 d . . H24A H 1.4362(6) -0.0936(15) 0.8259(4) 0.089 Uiso 1 calc R . C25 C 1.4071(7) -0.2691(18) 0.8783(5) 0.096(5) Uani 1 d . . H25A H 1.4623(7) -0.3142(18) 0.8756(5) 0.116 Uiso 1 calc R . C26 C 1.3433(8) -0.3373(14) 0.9115(4) 0.081(3) Uani 1 d . . H26A H 1.3546(8) -0.4306(14) 0.9312(4) 0.097 Uiso 1 calc R . C27 C 1.2629(5) -0.2727(11) 0.9171(3) 0.058(2) Uani 1 d . . C28 C 1.2964(6) 0.0844(14) 0.8244(4) 0.074(3) Uani 1 d . . H28A H 1.2365(6) 0.0851(14) 0.8072(4) 0.088 Uiso 1 calc R . C29 C 1.3033(11) 0.2050(14) 0.8723(6) 0.109(4) Uani 1 d . . H29A H 1.2921(11) 0.3027(14) 0.8530(6) 0.164 Uiso 1 calc R . H29B H 1.3614(11) 0.2045(14) 0.8903(6) 0.164 Uiso 1 calc R . H29C H 1.2610(11) 0.1869(14) 0.9049(6) 0.164 Uiso 1 calc R . C30 C 1.3593(12) 0.1181(21) 0.7712(6) 0.134(6) Uani 1 d . . H30A H 1.3548(12) 0.0392(21) 0.7398(6) 0.201 Uiso 1 calc R . H30B H 1.4182(12) 0.1215(21) 0.7875(6) 0.201 Uiso 1 calc R . H30C H 1.3448(12) 0.2150(21) 0.7526(6) 0.201 Uiso 1 calc R . C31 C 1.1920(7) -0.3414(11) 0.9569(4) 0.071(3) Uani 1 d . . H31A H 1.1362(7) -0.3305(11) 0.9341(4) 0.085 Uiso 1 calc R . C32 C 1.2040(11) -0.5053(14) 0.9723(6) 0.110(5) Uani 1 d . . H32A H 1.2083(11) -0.5634(14) 0.9340(6) 0.165 Uiso 1 calc R . H32B H 1.1546(11) -0.5407(14) 0.9963(6) 0.165 Uiso 1 calc R . H32C H 1.2568(11) -0.5181(14) 0.9968(6) 0.165 Uiso 1 calc R . C33 C 1.1855(10) -0.2529(15) 1.0171(5) 0.107(4) Uani 1 d . . H33A H 1.1777(10) -0.1463(15) 1.0077(5) 0.160 Uiso 1 calc R . H33B H 1.2384(10) -0.2665(15) 1.0414(5) 0.160 Uiso 1 calc R . H33C H 1.1362(10) -0.2891(15) 1.0409(5) 0.160 Uiso 1 calc R . O41 O 0.8212(3) -0.2917(5) 0.6606(2) 0.0306(9) Uani 1 d . . C41 C 0.8278(4) -0.4030(6) 0.6205(2) 0.0233(11) Uani 1 d . . C42 C 0.9052(4) -0.4824(7) 0.6128(2) 0.0295(12) Uani 1 d . . C43 C 0.9110(4) -0.6060(7) 0.5735(3) 0.0344(14) Uani 1 d . . H43A H 0.9639(4) -0.6589(7) 0.5708(3) 0.041 Uiso 1 calc R . C44 C 0.8415(4) -0.6534(7) 0.5383(3) 0.0352(14) Uani 1 d . . C45 C 0.7664(4) -0.5702(7) 0.5438(2) 0.0296(13) Uani 1 d . . H45A H 0.7185(4) -0.5991(7) 0.5191(2) 0.036 Uiso 1 calc R . C46 C 0.7563(4) -0.4481(7) 0.5827(2) 0.0266(12) Uani 1 d . . C47 C 0.9808(4) -0.4411(7) 0.6471(2) 0.0297(13) Uani 1 d . . H47A H 1.0305(4) -0.5010(7) 0.6406(2) 0.036 Uiso 1 calc R . N47 N 0.9892(3) -0.3314(6) 0.6861(2) 0.0266(10) Uani 1 d . . C48 C 0.6753(4) -0.3664(7) 0.5842(2) 0.0298(13) Uani 1 d . . H48A H 0.6636(4) -0.3003(7) 0.6175(2) 0.036 Uiso 1 calc R . N48 N 0.6197(4) -0.3828(6) 0.5409(2) 0.0381(12) Uani 1 d . . C49 C 0.8472(5) -0.7906(9) 0.4992(3) 0.051(2) Uani 1 d . . H49A H 0.9001(5) -0.8452(9) 0.5094(3) 0.076 Uiso 1 d R . H49B H 0.8479(5) -0.7619(9) 0.4555(3) 0.076 Uiso 1 d R . H49C H 0.7973(5) -0.8549(9) 0.5071(3) 0.076 Uiso 1 d R . C50 C 1.0735(4) -0.3357(6) 0.7157(2) 0.0276(12) Uani 1 d . . C51 C 1.0879(5) -0.4419(7) 0.7631(3) 0.0371(15) Uani 1 d . . C52 C 1.1703(5) -0.4556(9) 0.7854(3) 0.050(2) Uani 1 d . . H52A H 1.1817(5) -0.5267(9) 0.8171(3) 0.060 Uiso 1 calc R . C53 C 1.2369(5) -0.3699(10) 0.7633(3) 0.053(2) Uani 1 d . . H53A H 1.2935(5) -0.3839(10) 0.7790(3) 0.063 Uiso 1 calc R . C54 C 1.2215(5) -0.2642(9) 0.7184(3) 0.049(2) Uani 1 d . . H54A H 1.2678(5) -0.2047(9) 0.7037(3) 0.058 Uiso 1 calc R . C55 C 1.1391(5) -0.2426(8) 0.6941(3) 0.0381(15) Uani 1 d . . C56 C 1.0158(5) -0.5383(8) 0.7877(3) 0.047(2) Uani 1 d . . H56A H 0.9617(5) -0.5046(8) 0.7665(3) 0.056 Uiso 1 calc R . C57 C 1.0261(8) -0.6977(10) 0.7736(5) 0.076(3) Uani 1 d . . H57A H 0.9775(8) -0.7538(10) 0.7908(5) 0.115 Uiso 1 calc R . H57B H 1.0799(8) -0.7342(10) 0.7921(5) 0.115 Uiso 1 calc R . H57C H 1.0278(8) -0.7117(10) 0.7287(5) 0.115 Uiso 1 calc R . C58 C 1.0024(7) -0.5128(12) 0.8589(4) 0.072(3) Uani 1 d . . H58A H 0.9957(7) -0.4054(12) 0.8671(4) 0.109 Uiso 1 calc R . H58B H 1.0525(7) -0.5509(12) 0.8817(4) 0.109 Uiso 1 calc R . H58C H 0.9506(7) -0.5662(12) 0.8724(4) 0.109 Uiso 1 calc R . C59 C 1.1228(5) -0.1257(10) 0.6445(3) 0.052(2) Uani 1 d . . H59A H 1.0598(5) -0.1027(10) 0.6451(3) 0.062 Uiso 1 calc R . C60 C 1.1692(11) 0.0180(13) 0.6571(5) 0.101(4) Uani 1 d . . H60A H 1.1567(11) 0.0898(13) 0.6239(5) 0.151 Uiso 1 calc R . H60B H 1.2313(11) -0.0010(13) 0.6590(5) 0.151 Uiso 1 calc R . H60C H 1.1500(11) 0.0593(13) 0.6967(5) 0.151 Uiso 1 calc R . C61 C 1.1429(7) -0.1916(13) 0.5798(4) 0.072(3) Uani 1 d . . H61A H 1.1109(7) -0.2853(13) 0.5741(4) 0.108 Uiso 1 calc R . H61B H 1.2048(7) -0.2115(13) 0.5767(4) 0.108 Uiso 1 calc R . H61C H 1.1258(7) -0.1196(13) 0.5478(4) 0.108 Uiso 1 calc R . C62 C 0.5412(4) -0.3036(7) 0.5431(2) 0.0341(14) Uani 1 d . . C63 C 0.5330(4) -0.1670(8) 0.5101(3) 0.0391(15) Uani 1 d . . C64 C 0.4551(5) -0.0910(8) 0.5128(3) 0.048(2) Uani 1 d . . H64A H 0.4484(5) 0.0013(8) 0.4914(3) 0.057 Uiso 1 calc R . C65 C 0.3874(5) -0.1484(10) 0.5463(4) 0.058(2) Uani 1 d . . H65A H 0.3357(5) -0.0922(10) 0.5500(4) 0.069 Uiso 1 calc R . C66 C 0.3938(5) -0.2853(9) 0.5744(3) 0.046(2) Uani 1 d . . H66A H 0.3449(5) -0.3257(9) 0.5947(3) 0.055 Uiso 1 calc R . C67 C 0.4697(5) -0.3664(8) 0.5739(3) 0.0395(15) Uani 1 d . . C68 C 0.6056(5) -0.1145(8) 0.4680(3) 0.043(2) Uani 1 d . . H68A H 0.6615(5) -0.1418(8) 0.4881(3) 0.052 Uiso 1 calc R . C69 C 0.5977(6) -0.2039(12) 0.4070(4) 0.070(3) Uani 1 d . . H69A H 0.5971(6) -0.3115(12) 0.4162(4) 0.105 Uiso 1 calc R . H69B H 0.6469(6) -0.1808(12) 0.3804(4) 0.105 Uiso 1 calc R . H69C H 0.5442(6) -0.1762(12) 0.3857(4) 0.105 Uiso 1 calc R . C70 C 0.6067(6) 0.0520(10) 0.4551(3) 0.058(2) Uani 1 d . . H70A H 0.6550(6) 0.0759(10) 0.4279(3) 0.087 Uiso 1 calc R . H70B H 0.6132(6) 0.1068(10) 0.4942(3) 0.087 Uiso 1 calc R . H70C H 0.5526(6) 0.0814(10) 0.4350(3) 0.087 Uiso 1 calc R . C71 C 0.4758(5) -0.5207(8) 0.6025(3) 0.043(2) Uani 1 d . . H71A H 0.5280(5) -0.5209(8) 0.6298(3) 0.051 Uiso 1 calc R . C72 C 0.4010(6) -0.5670(10) 0.6420(4) 0.063(2) Uani 1 d . . H72A H 0.4111(6) -0.6681(10) 0.6583(4) 0.094 Uiso 1 calc R . H72B H 0.3481(6) -0.5666(10) 0.6170(4) 0.094 Uiso 1 calc R . H72C H 0.3949(6) -0.4965(10) 0.6765(4) 0.094 Uiso 1 calc R . C73 C 0.4902(6) -0.6420(9) 0.5523(4) 0.061(2) Uani 1 d . . H73A H 0.5388(6) -0.6130(9) 0.5262(4) 0.091 Uiso 1 calc R . H73B H 0.4382(6) -0.6513(9) 0.5267(4) 0.091 Uiso 1 calc R . H73C H 0.5026(6) -0.7383(9) 0.5723(4) 0.091 Uiso 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 0.0305(9) 0.0285(8) 0.0135(6) -0.0017(6) -0.0004(6) 0.0039(7) Cl 0.0463(9) 0.0383(8) 0.0342(7) 0.0095(6) 0.0020(6) 0.0016(7) O1 0.032(2) 0.039(2) 0.015(2) -0.0118(15) 0.001(2) 0.003(2) C1 0.036(3) 0.025(3) 0.012(2) -0.004(2) 0.005(2) -0.001(2) C2 0.025(3) 0.029(3) 0.021(2) -0.002(2) 0.001(2) 0.004(2) C3 0.040(4) 0.031(3) 0.016(2) -0.003(2) 0.001(2) 0.003(3) C4 0.042(4) 0.035(3) 0.013(2) -0.008(2) 0.003(2) 0.004(3) C5 0.034(3) 0.036(3) 0.019(2) -0.005(2) -0.002(2) -0.003(3) C6 0.033(3) 0.028(3) 0.017(2) 0.001(2) -0.002(2) -0.001(2) C7 0.037(4) 0.033(3) 0.021(2) -0.004(2) 0.001(2) 0.006(3) N7 0.034(3) 0.037(3) 0.016(2) -0.005(2) 0.000(2) -0.001(2) C8 0.039(4) 0.043(3) 0.018(2) 0.000(2) 0.000(2) 0.008(3) N8 0.033(3) 0.069(4) 0.032(3) -0.017(2) -0.006(2) 0.008(3) C9 0.057(5) 0.061(4) 0.026(3) -0.025(3) -0.001(3) 0.007(4) C10 0.035(4) 0.043(3) 0.020(2) -0.014(2) 0.005(2) -0.006(3) C11 0.041(4) 0.050(4) 0.024(3) -0.011(2) 0.007(3) -0.013(3) C12 0.051(5) 0.070(5) 0.045(4) -0.013(3) 0.007(3) -0.027(4) C13 0.038(4) 0.081(6) 0.056(4) -0.030(4) 0.008(4) -0.016(4) C14 0.029(4) 0.077(5) 0.048(4) -0.031(4) 0.001(3) 0.006(4) C15 0.033(4) 0.051(4) 0.033(3) -0.018(3) 0.002(3) 0.007(3) C16 0.071(5) 0.050(4) 0.033(3) 0.005(3) 0.000(3) -0.017(4) C17 0.135(10) 0.085(6) 0.030(4) 0.005(4) -0.006(5) -0.016(6) C18 0.088(7) 0.062(5) 0.055(4) 0.004(4) -0.006(4) -0.011(5) C19 0.047(4) 0.051(4) 0.033(3) -0.012(3) -0.015(3) 0.009(3) C20 0.074(6) 0.066(5) 0.036(4) 0.000(3) -0.005(4) -0.001(4) C21 0.069(6) 0.058(5) 0.074(5) -0.019(4) -0.026(5) 0.022(4) C22 0.039(4) 0.080(5) 0.028(3) -0.021(3) -0.009(3) 0.012(4) C23 0.040(5) 0.117(8) 0.037(3) -0.023(4) -0.007(3) 0.000(5) C24 0.034(5) 0.135(9) 0.052(4) -0.036(6) -0.009(4) 0.008(5) C25 0.051(6) 0.162(12) 0.077(7) -0.063(8) -0.033(6) 0.051(8) C26 0.080(8) 0.108(8) 0.055(5) -0.041(5) -0.032(5) 0.044(7) C27 0.050(5) 0.088(6) 0.037(4) -0.025(4) -0.019(3) 0.022(4) C28 0.042(5) 0.122(9) 0.057(5) 0.006(5) -0.002(4) -0.011(5) C29 0.140(13) 0.084(8) 0.103(9) 0.004(7) -0.017(8) 0.038(8) C30 0.158(15) 0.166(15) 0.078(7) 0.013(9) 0.039(9) -0.045(13) C31 0.083(7) 0.088(6) 0.042(4) -0.008(4) -0.016(4) 0.015(5) C32 0.152(14) 0.089(8) 0.088(8) 0.011(6) -0.027(8) 0.026(9) C33 0.138(12) 0.119(9) 0.063(6) -0.019(6) 0.034(7) -0.012(9) O41 0.034(2) 0.037(2) 0.020(2) -0.008(2) 0.000(2) 0.003(2) C41 0.031(3) 0.024(3) 0.015(2) 0.000(2) 0.003(2) -0.002(2) C42 0.033(3) 0.037(3) 0.019(2) -0.005(2) -0.003(2) 0.004(3) C43 0.037(4) 0.037(3) 0.029(3) -0.007(2) -0.003(3) 0.011(3) C44 0.043(4) 0.039(3) 0.023(3) -0.007(2) 0.000(2) 0.002(3) C45 0.033(3) 0.036(3) 0.020(2) -0.001(2) -0.005(2) -0.001(3) C46 0.030(3) 0.034(3) 0.015(2) -0.002(2) -0.001(2) -0.001(2) C47 0.032(3) 0.037(3) 0.020(2) -0.001(2) 0.002(2) 0.007(3) N47 0.030(3) 0.036(2) 0.015(2) -0.003(2) -0.004(2) 0.000(2) C48 0.030(3) 0.038(3) 0.022(2) 0.001(2) 0.001(2) 0.003(3) N48 0.036(3) 0.053(3) 0.025(2) -0.012(2) -0.007(2) 0.007(3) C49 0.053(5) 0.055(4) 0.044(4) -0.024(3) -0.010(3) 0.012(4) C50 0.025(3) 0.033(3) 0.025(2) -0.008(2) 0.000(2) 0.005(2) C51 0.045(4) 0.040(3) 0.026(3) -0.006(2) -0.008(3) 0.008(3) C52 0.057(5) 0.061(4) 0.033(3) -0.009(3) -0.016(3) 0.019(4) C53 0.029(4) 0.086(6) 0.042(4) -0.023(4) -0.010(3) 0.017(4) C54 0.035(4) 0.066(4) 0.045(4) -0.019(3) 0.006(3) 0.004(3) C55 0.040(4) 0.047(3) 0.028(3) -0.003(3) 0.006(3) 0.002(3) C56 0.055(5) 0.050(4) 0.036(3) 0.009(3) -0.008(3) -0.003(4) C57 0.108(9) 0.049(5) 0.072(6) 0.013(4) -0.010(5) -0.005(5) C58 0.094(7) 0.085(6) 0.038(4) 0.017(4) 0.010(4) -0.009(6) C59 0.045(4) 0.070(5) 0.041(4) 0.013(3) 0.013(3) 0.004(4) C60 0.161(13) 0.078(7) 0.064(6) 0.004(5) 0.014(7) -0.025(8) C61 0.069(6) 0.113(7) 0.033(4) 0.009(4) 0.007(4) -0.010(6) C62 0.032(4) 0.044(3) 0.026(3) -0.009(2) -0.007(2) 0.008(3) C63 0.035(4) 0.054(4) 0.028(3) -0.007(3) 0.002(3) 0.001(3) C64 0.040(4) 0.051(4) 0.053(4) 0.006(3) -0.002(3) 0.007(3) C65 0.030(4) 0.067(5) 0.076(5) 0.002(4) 0.007(4) 0.010(4) C66 0.027(4) 0.061(4) 0.049(4) -0.001(3) 0.009(3) 0.006(3) C67 0.036(4) 0.052(4) 0.030(3) -0.010(3) -0.004(3) 0.002(3) C68 0.035(4) 0.052(4) 0.042(3) -0.005(3) 0.001(3) -0.002(3) C69 0.069(6) 0.089(6) 0.052(4) -0.025(4) 0.029(4) -0.016(5) C70 0.065(5) 0.068(5) 0.041(4) 0.002(3) 0.008(3) 0.000(4) C71 0.034(4) 0.059(4) 0.036(3) -0.004(3) -0.002(3) 0.003(3) C72 0.064(6) 0.066(5) 0.059(5) 0.004(4) 0.013(4) -0.011(4) C73 0.079(6) 0.053(4) 0.050(4) -0.008(3) -0.017(4) 0.009(4) _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 O41 1.803(4) . ? Al O1 1.809(4) . ? Al N7 2.009(5) . ? Al N47 2.036(5) . ? Al Cl 2.164(2) . ? O1 C1 1.338(6) . ? C1 C2 1.413(8) . ? C1 C6 1.423(8) . ? C2 C3 1.412(7) . ? C2 C7 1.415(9) . ? C3 C4 1.370(9) . ? C4 C5 1.390(9) . ? C4 C9 1.534(7) . ? C5 C6 1.403(8) . ? C6 C8 1.460(9) . ? C7 N7 1.314(7) . ? N7 C10 1.459(8) . ? C8 N8 1.265(9) . ? N8 C22 1.439(9) . ? C10 C11 1.389(9) . ? C10 C15 1.417(10) . ? C11 C12 1.388(11) . ? C11 C16 1.510(11) . ? C12 C13 1.390(13) . ? C13 C14 1.366(13) . ? C14 C15 1.379(10) . ? C15 C19 1.502(11) . ? C16 C18 1.518(12) . ? C16 C17 1.549(10) . ? C19 C21 1.513(11) . ? C19 C20 1.560(9) . ? C22 C27 1.393(13) . ? C22 C23 1.395(13) . ? C23 C24 1.367(13) . ? C23 C28 1.52(2) . ? C24 C25 1.34(2) . ? C25 C26 1.37(2) . ? C26 C27 1.382(13) . ? C27 C31 1.529(14) . ? C28 C29 1.50(2) . ? C28 C30 1.54(2) . ? C31 C32 1.510(15) . ? C31 C33 1.526(13) . ? O41 C41 1.321(7) . ? C41 C42 1.407(8) . ? C41 C46 1.433(8) . ? C42 C43 1.395(8) . ? C42 C47 1.434(8) . ? C43 C44 1.383(9) . ? C44 C45 1.388(9) . ? C44 C49 1.490(9) . ? C45 C46 1.386(8) . ? C46 C48 1.454(9) . ? C47 N47 1.297(8) . ? N47 C50 1.456(8) . ? C48 N48 1.278(8) . ? N48 C62 1.411(8) . ? C50 C55 1.396(9) . ? C50 C51 1.412(9) . ? C51 C52 1.371(10) . ? C51 C56 1.511(11) . ? C52 C53 1.374(12) . ? C53 C54 1.372(12) . ? C54 C55 1.396(10) . ? C55 C59 1.515(10) . ? C56 C57 1.462(12) . ? C56 C58 1.572(10) . ? C59 C60 1.495(15) . ? C59 C61 1.550(11) . ? C62 C67 1.413(10) . ? C62 C63 1.417(10) . ? C63 C64 1.389(10) . ? C63 C68 1.527(10) . ? C64 C65 1.378(12) . ? C65 C66 1.366(12) . ? C66 C67 1.383(10) . ? C67 C71 1.511(10) . ? C68 C70 1.511(11) . ? C68 C69 1.544(10) . ? C71 C72 1.504(11) . ? C71 C73 1.549(10) . ? 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 O41 Al O1 153.7(2) . . ? O41 Al N7 85.4(2) . . ? O1 Al N7 88.3(2) . . ? O41 Al N47 88.7(2) . . ? O1 Al N47 83.6(2) . . ? N7 Al N47 148.8(2) . . ? O41 Al Cl 102.72(15) . . ? O1 Al Cl 103.5(2) . . ? N7 Al Cl 100.9(2) . . ? N47 Al Cl 110.3(2) . . ? C1 O1 Al 131.7(4) . . ? O1 C1 C2 120.1(5) . . ? O1 C1 C6 120.7(5) . . ? C2 C1 C6 119.1(5) . . ? C3 C2 C1 119.7(5) . . ? C3 C2 C7 118.3(5) . . ? C1 C2 C7 121.6(5) . . ? C4 C3 C2 121.7(6) . . ? C3 C4 C5 118.3(5) . . ? C3 C4 C9 121.0(6) . . ? C5 C4 C9 120.6(6) . . ? C4 C5 C6 123.0(5) . . ? C5 C6 C1 118.1(5) . . ? C5 C6 C8 119.8(5) . . ? C1 C6 C8 122.1(5) . . ? N7 C7 C2 126.5(6) . . ? C7 N7 C10 113.2(5) . . ? C7 N7 Al 122.0(4) . . ? C10 N7 Al 124.8(3) . . ? N8 C8 C6 120.1(5) . . ? C8 N8 C22 120.2(5) . . ? C11 C10 C15 123.9(6) . . ? C11 C10 N7 115.9(6) . . ? C15 C10 N7 120.1(6) . . ? C12 C11 C10 117.0(7) . . ? C12 C11 C16 120.6(7) . . ? C10 C11 C16 122.3(6) . . ? C11 C12 C13 120.6(8) . . ? C14 C13 C12 120.4(7) . . ? C13 C14 C15 122.5(8) . . ? C14 C15 C10 115.5(7) . . ? C14 C15 C19 121.5(7) . . ? C10 C15 C19 123.0(6) . . ? C11 C16 C18 114.1(7) . . ? C11 C16 C17 109.9(8) . . ? C18 C16 C17 111.0(7) . . ? C15 C19 C21 113.3(7) . . ? C15 C19 C20 109.4(6) . . ? C21 C19 C20 109.1(7) . . ? C27 C22 C23 121.0(8) . . ? C27 C22 N8 119.6(7) . . ? C23 C22 N8 119.4(8) . . ? C24 C23 C22 118.1(10) . . ? C24 C23 C28 122.9(10) . . ? C22 C23 C28 118.8(8) . . ? C25 C24 C23 122.0(11) . . ? C24 C25 C26 120.1(9) . . ? C25 C26 C27 121.1(11) . . ? C26 C27 C22 117.7(10) . . ? C26 C27 C31 122.4(10) . . ? C22 C27 C31 119.9(7) . . ? C29 C28 C23 110.9(8) . . ? C29 C28 C30 109.4(12) . . ? C23 C28 C30 111.4(11) . . ? C32 C31 C33 108.7(9) . . ? C32 C31 C27 115.1(10) . . ? C33 C31 C27 108.9(9) . . ? C41 O41 Al 136.5(4) . . ? O41 C41 C42 121.7(5) . . ? O41 C41 C46 121.4(5) . . ? C42 C41 C46 116.9(5) . . ? C43 C42 C41 121.8(6) . . ? C43 C42 C47 117.6(5) . . ? C41 C42 C47 120.5(5) . . ? C44 C43 C42 121.6(6) . . ? C43 C44 C45 116.3(5) . . ? C43 C44 C49 120.9(6) . . ? C45 C44 C49 122.7(6) . . ? C46 C45 C44 124.8(6) . . ? C45 C46 C41 118.4(5) . . ? C45 C46 C48 120.5(5) . . ? C41 C46 C48 121.1(5) . . ? N47 C47 C42 127.5(6) . . ? C47 N47 C50 110.7(5) . . ? C47 N47 Al 124.7(4) . . ? C50 N47 Al 124.3(3) . . ? N48 C48 C46 120.6(5) . . ? C48 N48 C62 119.9(5) . . ? C55 C50 C51 121.9(6) . . ? C55 C50 N47 119.6(5) . . ? C51 C50 N47 118.3(5) . . ? C52 C51 C50 117.3(7) . . ? C52 C51 C56 121.2(6) . . ? C50 C51 C56 121.5(6) . . ? C51 C52 C53 122.1(7) . . ? C54 C53 C52 120.0(7) . . ? C53 C54 C55 121.1(7) . . ? C54 C55 C50 117.5(6) . . ? C54 C55 C59 120.7(7) . . ? C50 C55 C59 121.7(6) . . ? C57 C56 C51 113.5(8) . . ? C57 C56 C58 111.0(7) . . ? C51 C56 C58 111.4(6) . . ? C60 C59 C55 112.5(8) . . ? C60 C59 C61 112.9(8) . . ? C55 C59 C61 110.1(7) . . ? N48 C62 C67 120.0(6) . . ? N48 C62 C63 119.2(6) . . ? C67 C62 C63 120.6(6) . . ? C64 C63 C62 118.3(6) . . ? C64 C63 C68 121.5(6) . . ? C62 C63 C68 120.0(6) . . ? C65 C64 C63 120.5(7) . . ? C66 C65 C64 120.7(7) . . ? C65 C66 C67 121.7(7) . . ? C66 C67 C62 117.9(6) . . ? C66 C67 C71 121.7(7) . . ? C62 C67 C71 120.4(6) . . ? C70 C68 C63 114.8(6) . . ? C70 C68 C69 110.6(7) . . ? C63 C68 C69 107.1(6) . . ? C72 C71 C67 115.8(6) . . ? C72 C71 C73 108.7(7) . . ? C67 C71 C73 111.0(6) . . ? _refine_diff_density_max 0.400 _refine_diff_density_min -0.511 _refine_diff_density_rms 0.069 #===END data_Compound_4 _database_code_depnum_ccdc_archive 'CCDC 233656' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C41 H59 N2 O Al' _chemical_formula_weight 622.88 _chemical_melting_point ? _chemical_compound_source ? 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' O O 0.0106 0.0060 '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 9.5331(14) _cell_length_b 17.296(2) _cell_length_c 23.950(3) _cell_angle_alpha 92.317(11) _cell_angle_beta 91.800(10) _cell_angle_gamma 94.951(10) _cell_volume 3928.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 29 _cell_measurement_theta_min 4.80 _cell_measurement_theta_max 12.52 _exptl_crystal_description rhombs _exptl_crystal_colour Orange/red _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.053 _exptl_crystal_density_method ? _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5.33 _diffrn_reflns_number 10969 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0762 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 22.50 _reflns_number_total 10226 _reflns_number_observed 6399 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1193 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0957P)^2^+0.4940P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0002(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9033 _refine_ls_number_parameters 872 _refine_ls_number_restraints 205 _refine_ls_R_factor_all 0.1188 _refine_ls_R_factor_obs 0.0667 _refine_ls_wR_factor_all 0.1970 _refine_ls_wR_factor_obs 0.1591 _refine_ls_goodness_of_fit_all 1.041 _refine_ls_goodness_of_fit_obs 1.127 _refine_ls_restrained_S_all 1.147 _refine_ls_restrained_S_obs 1.229 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Al Al 0.61767(15) 0.54169(8) 0.25996(6) 0.0430(4) Uani 1 d D . O1 O 0.5751(3) 0.5945(2) 0.32119(12) 0.0454(8) Uani 1 d . . C1 C 0.4533(4) 0.6122(2) 0.3408(2) 0.0325(9) Uani 1 d . . C2 C 0.3242(5) 0.5919(2) 0.3110(2) 0.0344(9) Uani 1 d . . C3 C 0.1989(5) 0.6117(3) 0.3349(2) 0.0456(11) Uani 1 d . . H3A H 0.1121(5) 0.5974(3) 0.3150(2) 0.055 Uiso 1 calc R . C4 C 0.1964(5) 0.6509(3) 0.3860(2) 0.0502(12) Uani 1 d . . C5 C 0.3236(5) 0.6705(3) 0.4140(2) 0.0434(11) Uani 1 d . . H5A H 0.3235(5) 0.6975(3) 0.4493(2) 0.052 Uiso 1 calc R . C6 C 0.4522(5) 0.6527(2) 0.3934(2) 0.0338(9) Uani 1 d . . C7 C 0.3167(5) 0.5517(2) 0.2573(2) 0.0369(10) Uani 1 d . . H7A H 0.2255(5) 0.5412(2) 0.2401(2) 0.044 Uiso 1 calc R . N7 N 0.4206(4) 0.5280(2) 0.22977(14) 0.0362(8) Uani 1 d . . C8 C 0.5855(5) 0.6732(2) 0.4245(2) 0.0386(10) Uani 1 d . . H8A H 0.6680(5) 0.6526(2) 0.4112(2) 0.046 Uiso 1 calc R . N8 N 0.5967(4) 0.7175(2) 0.46872(14) 0.0408(9) Uani 1 d . . C9 C 0.0582(6) 0.6706(5) 0.4113(3) 0.085(2) Uani 1 d . . H9A H -0.0211(6) 0.6446(5) 0.3889(3) 0.127 Uiso 1 d R . H9B H 0.0525(6) 0.7269(5) 0.4118(3) 0.127 Uiso 1 d R . H9C H 0.0545(6) 0.6529(5) 0.4497(3) 0.127 Uiso 1 d R . C10 C 0.6617(11) 0.4343(5) 0.2790(5) 0.057(2) Uani 0.60 d PD 1 H10A H 0.5934(11) 0.4156(5) 0.3068(5) 0.069 Uiso 0.60 calc PR 1 H10B H 0.6431(11) 0.4005(5) 0.2448(5) 0.069 Uiso 0.60 calc PR 1 C11 C 0.8107(11) 0.4209(6) 0.3022(4) 0.074(3) Uani 0.60 d PD 1 H11A H 0.8934(11) 0.4394(6) 0.2801(4) 0.089 Uiso 0.60 calc PR 1 C12 C 0.7904(22) 0.3290(8) 0.3154(9) 0.133(8) Uani 0.60 d PDU 1 H12A H 0.8792(22) 0.3127(8) 0.3307(9) 0.199 Uiso 0.60 calc PR 1 H12B H 0.7630(22) 0.2985(8) 0.2808(9) 0.199 Uiso 0.60 calc PR 1 H12C H 0.7167(22) 0.3205(8) 0.3427(9) 0.199 Uiso 0.60 calc PR 1 C13 C 0.7993(22) 0.4579(11) 0.3647(6) 0.129(7) Uani 0.60 d PDU 1 H13A H 0.8880(22) 0.4540(11) 0.3858(6) 0.193 Uiso 0.60 calc PR 1 H13B H 0.7221(22) 0.4295(11) 0.3834(6) 0.193 Uiso 0.60 calc PR 1 H13C H 0.7809(22) 0.5126(11) 0.3628(6) 0.193 Uiso 0.60 calc PR 1 C10A C 0.7142(19) 0.4505(9) 0.2645(6) 0.065(6) Uiso 0.40 d PD 2 H10C H 0.6683(19) 0.4111(9) 0.2372(6) 0.078 Uiso 0.40 calc PR 2 H10D H 0.8117(19) 0.4630(9) 0.2525(6) 0.078 Uiso 0.40 calc PR 2 C11A C 0.7231(20) 0.4118(9) 0.3232(7) 0.095(6) Uiso 0.40 d PD 2 H11B H 0.6353(20) 0.3987(9) 0.3439(7) 0.114 Uiso 0.40 calc PR 2 C12A C 0.8306(26) 0.3408(11) 0.3060(10) 0.088(7) Uiso 0.40 d PD 2 H12D H 0.8474(26) 0.3103(11) 0.3388(10) 0.133 Uiso 0.40 calc PR 2 H12E H 0.9206(26) 0.3648(11) 0.2936(10) 0.133 Uiso 0.40 calc PR 2 H12F H 0.7854(26) 0.3067(11) 0.2758(10) 0.133 Uiso 0.40 calc PR 2 C13A C 0.8533(20) 0.4717(11) 0.3530(8) 0.070(6) Uiso 0.40 d PD 2 H13D H 0.8734(20) 0.4557(11) 0.3910(8) 0.106 Uiso 0.40 calc PR 2 H13E H 0.8250(20) 0.5248(11) 0.3545(8) 0.106 Uiso 0.40 calc PR 2 H13F H 0.9379(20) 0.4696(11) 0.3310(8) 0.106 Uiso 0.40 calc PR 2 C14 C 0.7667(13) 0.5908(7) 0.2173(6) 0.049(4) Uani 0.50 d PD 1 H14A H 0.8563(13) 0.5720(7) 0.2307(6) 0.059 Uiso 0.50 calc PR 1 H14B H 0.7507(13) 0.5716(7) 0.1779(6) 0.059 Uiso 0.50 calc PR 1 C15 C 0.7889(12) 0.6821(6) 0.2173(4) 0.051(3) Uani 0.50 d PD 1 H15A H 0.7142(12) 0.7139(6) 0.2027(4) 0.062 Uiso 0.50 calc PR 1 C16 C 0.8705(23) 0.7037(15) 0.2761(7) 0.078(8) Uani 0.50 d PD 1 H16A H 0.8901(23) 0.7602(15) 0.2807(7) 0.117 Uiso 0.50 calc PR 1 H16B H 0.9594(23) 0.6792(15) 0.2772(7) 0.117 Uiso 0.50 calc PR 1 H16C H 0.8119(23) 0.6849(15) 0.3065(7) 0.117 Uiso 0.50 calc PR 1 C17 C 0.9512(16) 0.6752(11) 0.1826(7) 0.101(5) Uani 0.50 d PDU 1 H17A H 0.9942(16) 0.7275(11) 0.1762(7) 0.152 Uiso 0.50 calc PR 1 H17B H 0.9327(16) 0.6465(11) 0.1466(7) 0.152 Uiso 0.50 calc PR 1 H17C H 1.0155(16) 0.6479(11) 0.2059(7) 0.152 Uiso 0.50 calc PR 1 C14A C 0.7135(14) 0.6147(9) 0.2068(6) 0.058(4) Uani 0.50 d PD 2 H14C H 0.7189(14) 0.5871(9) 0.1700(6) 0.070 Uiso 0.50 calc PR 2 H14D H 0.6556(14) 0.6588(9) 0.2015(6) 0.070 Uiso 0.50 calc PR 2 C15A C 0.8632(13) 0.6465(8) 0.2272(5) 0.072(3) Uani 0.50 d PD 2 H15B H 0.9366(13) 0.6108(8) 0.2368(5) 0.086 Uiso 0.50 calc PR 2 C16A C 0.8252(22) 0.7172(13) 0.2715(8) 0.067(6) Uani 0.50 d PD 2 H16D H 0.9126(22) 0.7434(13) 0.2882(8) 0.100 Uiso 0.50 calc PR 2 H16E H 0.7671(22) 0.6953(13) 0.3010(8) 0.100 Uiso 0.50 calc PR 2 H16F H 0.7734(22) 0.7547(13) 0.2515(8) 0.100 Uiso 0.50 calc PR 2 C17A C 0.8890(17) 0.7134(8) 0.1757(6) 0.081(4) Uani 0.50 d PDU 2 H17D H 0.9826(17) 0.7413(8) 0.1813(6) 0.121 Uiso 0.50 calc PR 2 H17E H 0.8170(17) 0.7505(8) 0.1779(6) 0.121 Uiso 0.50 calc PR 2 H17F H 0.8821(17) 0.6863(8) 0.1389(6) 0.121 Uiso 0.50 calc PR 2 C18 C 0.3876(5) 0.4844(2) 0.1773(2) 0.0380(10) Uani 1 d . . C19 C 0.3972(6) 0.5226(3) 0.1265(2) 0.0533(13) Uani 1 d . . C20 C 0.3712(7) 0.4780(3) 0.0776(2) 0.065(2) Uani 1 d . . H20A H 0.3766(7) 0.5024(3) 0.0428(2) 0.078 Uiso 1 calc R . C21 C 0.3381(7) 0.3999(4) 0.0778(2) 0.071(2) Uani 1 d . . H21A H 0.3227(7) 0.3705(4) 0.0434(2) 0.085 Uiso 1 calc R . C22 C 0.3267(7) 0.3629(3) 0.1279(2) 0.071(2) Uani 1 d . . H22A H 0.3009(7) 0.3085(3) 0.1274(2) 0.085 Uiso 1 calc R . C23 C 0.3523(6) 0.4039(3) 0.1786(2) 0.0498(12) Uani 1 d . . C24 C 0.4259(10) 0.6098(3) 0.1255(2) 0.092(3) Uani 1 d . . H24A H 0.4765(10) 0.6283(3) 0.1614(2) 0.110 Uiso 1 calc R . C25 C 0.2868(12) 0.6468(5) 0.1227(4) 0.140(4) Uani 1 d U . H25A H 0.3054(12) 0.7034(5) 0.1220(4) 0.209 Uiso 1 calc R . H25B H 0.2326(12) 0.6334(5) 0.1556(4) 0.209 Uiso 1 calc R . H25C H 0.2329(12) 0.6275(5) 0.0887(4) 0.209 Uiso 1 calc R . C26 C 0.5189(12) 0.6366(4) 0.0771(3) 0.124(3) Uani 1 d U . H26A H 0.5337(12) 0.6934(4) 0.0787(3) 0.186 Uiso 1 calc R . H26B H 0.4720(12) 0.6187(4) 0.0413(3) 0.186 Uiso 1 calc R . H26C H 0.6101(12) 0.6147(4) 0.0805(3) 0.186 Uiso 1 calc R . C27 C 0.3378(7) 0.3620(3) 0.2326(2) 0.069(2) Uani 1 d . . H27A H 0.3874(7) 0.3964(3) 0.2630(2) 0.083 Uiso 1 calc R . C28 C 0.1835(10) 0.3485(5) 0.2478(3) 0.119(3) Uani 1 d . . H28A H 0.1770(10) 0.3214(5) 0.2828(3) 0.178 Uiso 1 calc R . H28B H 0.1310(10) 0.3169(5) 0.2179(3) 0.178 Uiso 1 calc R . H28C H 0.1435(10) 0.3986(5) 0.2523(3) 0.178 Uiso 1 calc R . C29 C 0.4069(10) 0.2855(3) 0.2310(3) 0.100(3) Uani 1 d U . H29A H 0.3948(10) 0.2606(3) 0.2667(3) 0.149 Uiso 1 calc R . H29B H 0.5076(10) 0.2958(3) 0.2244(3) 0.149 Uiso 1 calc R . H29C H 0.3625(10) 0.2511(3) 0.2007(3) 0.149 Uiso 1 calc R . C30 C 0.7316(5) 0.7298(3) 0.4969(2) 0.0422(11) Uani 1 d . . C31 C 0.7760(6) 0.6731(3) 0.5324(2) 0.0496(12) Uani 1 d . . C32 C 0.9032(7) 0.6893(3) 0.5615(2) 0.0643(15) Uani 1 d . . H32A H 0.9354(7) 0.6522(3) 0.5860(2) 0.077 Uiso 1 calc R . C33 C 0.9842(6) 0.7583(4) 0.5558(2) 0.066(2) Uani 1 d . . H33A H 1.0722(6) 0.7678(4) 0.5757(2) 0.079 Uiso 1 calc R . C34 C 0.9377(6) 0.8137(3) 0.5212(2) 0.0547(13) Uani 1 d . . H34A H 0.9945(6) 0.8610(3) 0.5175(2) 0.066 Uiso 1 calc R . C35 C 0.8113(5) 0.8015(3) 0.4922(2) 0.0429(11) Uani 1 d . . C36 C 0.6865(7) 0.5972(3) 0.5398(2) 0.068(2) Uani 1 d . . H36A H 0.5941(7) 0.6004(3) 0.5195(2) 0.081 Uiso 1 calc R . C37 C 0.6567(12) 0.5835(5) 0.6007(4) 0.130(4) Uani 1 d U . H37A H 0.6139(12) 0.6283(5) 0.6171(4) 0.195 Uiso 1 calc R . H37B H 0.7451(12) 0.5767(5) 0.6212(4) 0.195 Uiso 1 calc R . H37C H 0.5920(12) 0.5367(5) 0.6031(4) 0.195 Uiso 1 calc R . C38 C 0.7516(12) 0.5287(4) 0.5155(4) 0.138(4) Uani 1 d U . H38A H 0.7713(12) 0.5370(4) 0.4762(4) 0.207 Uiso 1 calc R . H38B H 0.6866(12) 0.4820(4) 0.5182(4) 0.207 Uiso 1 calc R . H38C H 0.8397(12) 0.5221(4) 0.5363(4) 0.207 Uiso 1 calc R . C39 C 0.7566(6) 0.8617(3) 0.4540(2) 0.0516(12) Uani 1 d . . H39A H 0.6520(6) 0.8592(3) 0.4570(2) 0.062 Uiso 1 calc R . C40 C 0.8160(7) 0.9451(3) 0.4705(3) 0.070(2) Uani 1 d . . H40A H 0.7963(7) 0.9569(3) 0.5096(3) 0.105 Uiso 1 calc R . H40B H 0.7717(7) 0.9814(3) 0.4466(3) 0.105 Uiso 1 calc R . H40C H 0.9181(7) 0.9501(3) 0.4657(3) 0.105 Uiso 1 calc R . C41 C 0.7879(8) 0.8439(3) 0.3931(2) 0.077(2) Uani 1 d . . H41A H 0.7516(8) 0.8835(3) 0.3697(2) 0.116 Uiso 1 calc R . H41B H 0.7422(8) 0.7927(3) 0.3812(2) 0.116 Uiso 1 calc R . H41C H 0.8899(8) 0.8440(3) 0.3891(2) 0.116 Uiso 1 calc R . Al' Al 0.34168(14) 0.97287(8) 0.76533(6) 0.0418(4) Uani 1 d . . O1' O 0.3712(3) 0.8947(2) 0.80990(12) 0.0400(7) Uani 1 d . . C1' C 0.4924(4) 0.8868(2) 0.8366(2) 0.0334(9) Uani 1 d . . C2' C 0.6229(4) 0.9141(2) 0.8154(2) 0.0315(9) Uani 1 d . . C3' C 0.7500(5) 0.9017(2) 0.8441(2) 0.0375(10) Uani 1 d . . H3'A H 0.8371(5) 0.9200(2) 0.8290(2) 0.045 Uiso 1 calc R . C4' C 0.7509(5) 0.8637(2) 0.8935(2) 0.0405(10) Uani 1 d . . C5' C 0.6220(5) 0.8376(2) 0.9141(2) 0.0399(10) Uani 1 d . . H5'A H 0.6214(5) 0.8117(2) 0.9484(2) 0.048 Uiso 1 calc R . C6' C 0.4935(5) 0.8472(2) 0.8875(2) 0.0369(10) Uani 1 d . . C7' C 0.6340(4) 0.9507(2) 0.7622(2) 0.0306(9) Uani 1 d . . H7'A H 0.7256(4) 0.9591(2) 0.7479(2) 0.037 Uiso 1 calc R . N7' N 0.5309(3) 0.9727(2) 0.73244(13) 0.0316(8) Uani 1 d . . C8' C 0.3604(5) 0.8180(3) 0.9113(2) 0.0427(11) Uani 1 d . . H8'A H 0.2738(5) 0.8291(3) 0.8939(2) 0.051 Uiso 1 calc R . N8' N 0.3590(4) 0.7779(2) 0.95510(15) 0.0434(9) Uani 1 d . . C9' C 0.8883(6) 0.8503(3) 0.9238(2) 0.0591(14) Uani 1 d . . H9'1 H 0.8863(6) 0.7959(3) 0.9340(2) 0.089 Uiso 1 d R . H9'2 H 0.9002(6) 0.8841(3) 0.9578(2) 0.089 Uiso 1 d R . H9'3 H 0.9670(6) 0.8622(3) 0.8994(2) 0.089 Uiso 1 d R . C10' C 0.3397(6) 1.0689(3) 0.8135(3) 0.067(2) Uani 1 d . . H10E H 0.4375(6) 1.0930(3) 0.8185(3) 0.080 Uiso 1 calc R . H10F H 0.2844(6) 1.1058(3) 0.7936(3) 0.080 Uiso 1 calc R . C11' C 0.2790(6) 1.0581(3) 0.8713(2) 0.0622(14) Uani 1 d . . H11C H 0.3314(6) 1.0179(3) 0.8899(2) 0.075 Uiso 1 calc R . C12' C 0.2974(8) 1.1319(5) 0.9091(3) 0.099(2) Uani 1 d . . H12G H 0.3972(8) 1.1513(5) 0.9118(3) 0.148 Uiso 1 calc R . H12H H 0.2646(8) 1.1202(5) 0.9465(3) 0.148 Uiso 1 calc R . H12I H 0.2422(8) 1.1715(5) 0.8933(3) 0.148 Uiso 1 calc R . C13' C 0.1267(6) 1.0280(4) 0.8670(3) 0.073(2) Uani 1 d . . H13G H 0.1156(6) 0.9807(4) 0.8428(3) 0.110 Uiso 1 calc R . H13H H 0.0713(6) 1.0674(4) 0.8511(3) 0.110 Uiso 1 calc R . H13I H 0.0936(6) 1.0162(4) 0.9043(3) 0.110 Uiso 1 calc R . C14' C 0.2042(6) 0.9536(4) 0.7029(2) 0.073(2) Uani 1 d . . H14E H 0.2195(6) 0.9979(4) 0.6782(2) 0.087 Uiso 1 calc R . H14F H 0.2307(6) 0.9072(4) 0.6816(2) 0.087 Uiso 1 calc R . C15' C 0.0473(5) 0.9415(3) 0.7107(2) 0.0551(13) Uani 1 d . . H15C H 0.0232(5) 0.9794(3) 0.7408(2) 0.066 Uiso 1 calc R . C16' C 0.0065(7) 0.8609(3) 0.7300(3) 0.077(2) Uani 1 d . . H16G H -0.0955(7) 0.8542(3) 0.7348(3) 0.115 Uiso 1 calc R . H16H H 0.0557(7) 0.8537(3) 0.7658(3) 0.115 Uiso 1 calc R . H16I H 0.0330(7) 0.8223(3) 0.7021(3) 0.115 Uiso 1 calc R . C17' C -0.0370(6) 0.9575(4) 0.6579(2) 0.071(2) Uani 1 d . . H17G H -0.0087(6) 1.0101(4) 0.6462(2) 0.106 Uiso 1 calc R . H17H H -0.1378(6) 0.9531(4) 0.6655(2) 0.106 Uiso 1 calc R . H17I H -0.0188(6) 0.9197(4) 0.6280(2) 0.106 Uiso 1 calc R . C18' C 0.5628(4) 1.0059(2) 0.6789(2) 0.0332(9) Uani 1 d . . C19' C 0.5376(5) 0.9584(3) 0.6304(2) 0.0379(10) Uani 1 d . . C20' C 0.5667(5) 0.9911(3) 0.5795(2) 0.0480(12) Uani 1 d . . H20B H 0.5514(5) 0.9600(3) 0.5459(2) 0.058 Uiso 1 calc R . C21' C 0.6176(6) 1.0679(3) 0.5772(2) 0.0561(13) Uani 1 d . . H21B H 0.6358(6) 1.0894(3) 0.5419(2) 0.067 Uiso 1 calc R . C22' C 0.6424(5) 1.1139(3) 0.6254(2) 0.0491(12) Uani 1 d . . H22B H 0.6777(5) 1.1667(3) 0.6232(2) 0.059 Uiso 1 calc R . C23' C 0.6160(5) 1.0835(2) 0.6777(2) 0.0401(10) Uani 1 d . . C24' C 0.4914(5) 0.8720(3) 0.6321(2) 0.0423(11) Uani 1 d . . H24B H 0.4423(5) 0.8634(3) 0.6679(2) 0.051 Uiso 1 calc R . C25' C 0.6191(6) 0.8242(3) 0.6322(2) 0.0573(13) Uani 1 d . . H25D H 0.5873(6) 0.7689(3) 0.6334(2) 0.086 Uiso 1 calc R . H25E H 0.6803(6) 0.8398(3) 0.6651(2) 0.086 Uiso 1 calc R . H25F H 0.6716(6) 0.8334(3) 0.5983(2) 0.086 Uiso 1 calc R . C26' C 0.3890(7) 0.8416(3) 0.5838(2) 0.069(2) Uani 1 d . . H26D H 0.3636(7) 0.7860(3) 0.5874(2) 0.103 Uiso 1 calc R . H26E H 0.4343(7) 0.8500(3) 0.5481(2) 0.103 Uiso 1 calc R . H26F H 0.3039(7) 0.8695(3) 0.5851(2) 0.103 Uiso 1 calc R . C27' C 0.6485(6) 1.1356(3) 0.7301(2) 0.0497(12) Uani 1 d . . H27B H 0.6183(6) 1.1050(3) 0.7629(2) 0.060 Uiso 1 calc R . C28' C 0.8087(7) 1.1566(5) 0.7372(3) 0.090(2) Uani 1 d . . H28D H 0.8573(7) 1.1089(5) 0.7371(3) 0.134 Uiso 1 calc R . H28E H 0.8297(7) 1.1862(5) 0.7726(3) 0.134 Uiso 1 calc R . H28F H 0.8411(7) 1.1881(5) 0.7062(3) 0.134 Uiso 1 calc R . C29' C 0.5673(9) 1.2061(3) 0.7298(3) 0.088(2) Uani 1 d . . H29D H 0.5908(9) 1.2382(3) 0.7640(3) 0.132 Uiso 1 calc R . H29E H 0.4661(9) 1.1900(3) 0.7279(3) 0.132 Uiso 1 calc R . H29F H 0.5920(9) 1.2363(3) 0.6972(3) 0.132 Uiso 1 calc R . C30' C 0.2270(5) 0.7545(2) 0.9783(2) 0.0401(11) Uani 1 d . . C31' C 0.1835(5) 0.7990(3) 1.0236(2) 0.0411(11) Uani 1 d . . C32' C 0.0583(5) 0.7744(3) 1.0478(2) 0.0486(12) Uani 1 d . . H32B H 0.0261(5) 0.8043(3) 1.0782(2) 0.058 Uiso 1 calc R . C33' C -0.0200(5) 0.7080(3) 1.0289(2) 0.0560(13) Uani 1 d . . H33B H -0.1061(5) 0.6925(3) 1.0459(2) 0.067 Uiso 1 calc R . C34' C 0.0263(6) 0.6632(3) 0.9852(2) 0.0583(14) Uani 1 d . . H34B H -0.0277(6) 0.6166(3) 0.9729(2) 0.070 Uiso 1 calc R . C35' C 0.1496(6) 0.6852(3) 0.9591(2) 0.0509(12) Uani 1 d . . C36' C 0.2716(6) 0.8728(3) 1.0443(2) 0.0498(12) Uani 1 d . . H36B H 0.3709(6) 0.8671(3) 1.0336(2) 0.060 Uiso 1 calc R . C37' C 0.2730(7) 0.8869(4) 1.1077(2) 0.071(2) Uani 1 d . . H37D H 0.3314(7) 0.9350(4) 1.1182(2) 0.107 Uiso 1 calc R . H37E H 0.3120(7) 0.8433(4) 1.1259(2) 0.107 Uiso 1 calc R . H37F H 0.1766(7) 0.8914(4) 1.1197(2) 0.107 Uiso 1 calc R . C38' C 0.2238(8) 0.9441(3) 1.0157(2) 0.072(2) Uani 1 d . . H38D H 0.2823(8) 0.9906(3) 1.0299(2) 0.109 Uiso 1 calc R . H38E H 0.1250(8) 0.9499(3) 1.0238(2) 0.109 Uiso 1 calc R . H38F H 0.2334(8) 0.9375(3) 0.9753(2) 0.109 Uiso 1 calc R . C39' C 0.1997(7) 0.6359(3) 0.9107(3) 0.076(2) Uani 1 d D . H39B H 0.3011(7) 0.6540(3) 0.9062(3) 0.092 Uiso 0.70 calc PR 1 H39C H 0.2515(7) 0.6719(3) 0.8879(3) 0.092 Uiso 0.30 d PR 2 C40' C 0.1970(14) 0.5503(5) 0.9268(4) 0.095(3) Uani 0.70 d PD 1 H40D H 0.2475(14) 0.5474(5) 0.9629(4) 0.143 Uiso 0.70 calc PR 1 H40E H 0.2426(14) 0.5204(5) 0.8981(4) 0.143 Uiso 0.70 calc PR 1 H40F H 0.0991(14) 0.5288(5) 0.9298(4) 0.143 Uiso 0.70 calc PR 1 C41' C 0.1295(16) 0.6477(7) 0.8590(3) 0.114(5) Uani 0.70 d PD 1 H41D H 0.1657(16) 0.6147(7) 0.8295(3) 0.171 Uiso 0.70 calc PR 1 H41E H 0.1462(16) 0.7024(7) 0.8497(3) 0.171 Uiso 0.70 calc PR 1 H41F H 0.0281(16) 0.6343(7) 0.8620(3) 0.171 Uiso 0.70 calc PR 1 C40B C 0.3074(26) 0.5855(17) 0.9215(12) 0.111(9) Uiso 0.30 d PD 2 H40G H 0.3284(26) 0.5577(17) 0.8867(12) 0.166 Uiso 0.30 calc PR 2 H40H H 0.2750(26) 0.5479(17) 0.9489(12) 0.166 Uiso 0.30 calc PR 2 H40I H 0.3926(26) 0.6161(17) 0.9364(12) 0.166 Uiso 0.30 calc PR 2 C41B C 0.0721(24) 0.5877(17) 0.8756(12) 0.105(8) Uiso 0.30 d PD 2 H41G H -0.0024(24) 0.6219(17) 0.8679(12) 0.158 Uiso 0.30 calc PR 2 H41H H 0.0344(24) 0.5442(17) 0.8972(12) 0.158 Uiso 0.30 calc PR 2 H41I H 0.1066(24) 0.5677(17) 0.8402(12) 0.158 Uiso 0.30 calc PR 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 Al 0.0400(8) 0.0456(8) 0.0426(8) -0.0086(6) 0.0029(6) 0.0038(6) O1 0.042(2) 0.051(2) 0.042(2) -0.0115(14) 0.0011(14) 0.0033(15) C1 0.039(2) 0.024(2) 0.035(2) 0.005(2) 0.000(2) 0.004(2) C2 0.044(3) 0.026(2) 0.034(2) 0.001(2) 0.001(2) 0.007(2) C3 0.042(3) 0.050(3) 0.045(3) -0.001(2) -0.006(2) 0.004(2) C4 0.047(3) 0.058(3) 0.048(3) -0.001(2) 0.006(2) 0.012(2) C5 0.061(3) 0.038(2) 0.032(2) 0.001(2) 0.005(2) 0.010(2) C6 0.045(3) 0.024(2) 0.032(2) 0.002(2) 0.003(2) 0.002(2) C7 0.039(2) 0.033(2) 0.038(2) 0.003(2) -0.004(2) 0.005(2) N7 0.049(2) 0.029(2) 0.030(2) -0.0015(14) 0.000(2) 0.008(2) C8 0.053(3) 0.030(2) 0.032(2) 0.003(2) 0.001(2) 0.001(2) N8 0.052(2) 0.034(2) 0.035(2) -0.002(2) -0.002(2) -0.001(2) C9 0.060(4) 0.135(6) 0.063(4) -0.024(4) 0.010(3) 0.033(4) C10 0.050(6) 0.053(5) 0.070(6) 0.002(5) -0.005(5) 0.015(5) C11 0.076(7) 0.066(6) 0.084(7) 0.028(5) 0.004(6) 0.018(5) C12 0.142(12) 0.105(9) 0.158(11) 0.061(8) -0.015(9) 0.028(8) C13 0.172(16) 0.141(13) 0.081(9) 0.008(9) -0.026(11) 0.063(12) C14 0.039(8) 0.077(9) 0.033(7) -0.003(5) 0.003(6) 0.008(7) C15 0.050(6) 0.060(7) 0.044(6) 0.012(5) -0.009(5) -0.004(6) C16 0.053(15) 0.106(17) 0.069(10) -0.013(10) -0.002(8) -0.019(11) C17 0.098(9) 0.116(10) 0.086(8) -0.007(8) 0.025(7) -0.023(8) C14A 0.047(8) 0.086(11) 0.037(7) -0.003(7) 0.004(6) -0.014(8) C15A 0.055(8) 0.082(9) 0.076(9) 0.004(7) 0.000(7) -0.008(8) C16A 0.042(12) 0.068(10) 0.087(13) 0.002(8) 0.009(8) -0.015(9) C17A 0.093(10) 0.076(8) 0.070(8) 0.014(7) 0.007(7) -0.017(8) C18 0.043(3) 0.039(2) 0.032(2) -0.004(2) -0.004(2) 0.011(2) C19 0.073(4) 0.049(3) 0.040(3) 0.007(2) -0.007(2) 0.016(3) C20 0.097(4) 0.068(4) 0.031(3) 0.001(2) -0.006(3) 0.014(3) C21 0.099(5) 0.071(4) 0.036(3) -0.017(3) -0.006(3) -0.009(3) C22 0.106(5) 0.047(3) 0.054(3) -0.012(3) -0.001(3) -0.018(3) C23 0.069(3) 0.041(3) 0.037(3) -0.005(2) 0.001(2) -0.004(2) C24 0.184(8) 0.045(3) 0.049(3) 0.015(3) -0.013(4) 0.018(4) C25 0.211(8) 0.099(5) 0.120(6) 0.017(5) -0.020(6) 0.085(6) C26 0.228(10) 0.070(4) 0.069(4) 0.027(4) 0.005(5) -0.023(5) C27 0.115(5) 0.041(3) 0.047(3) 0.000(2) 0.004(3) -0.022(3) C28 0.147(8) 0.120(7) 0.077(5) 0.009(4) 0.028(5) -0.065(6) C29 0.187(8) 0.041(3) 0.066(4) -0.001(3) -0.022(5) -0.005(4) C30 0.052(3) 0.045(3) 0.029(2) -0.004(2) 0.003(2) 0.003(2) C31 0.064(3) 0.044(3) 0.039(3) 0.002(2) -0.004(2) 0.001(2) C32 0.082(4) 0.059(3) 0.052(3) 0.007(3) -0.013(3) 0.006(3) C33 0.059(3) 0.082(4) 0.053(3) -0.010(3) -0.017(3) 0.002(3) C34 0.056(3) 0.054(3) 0.052(3) -0.005(2) 0.003(3) -0.006(2) C35 0.049(3) 0.042(3) 0.036(2) -0.006(2) 0.000(2) -0.001(2) C36 0.090(4) 0.051(3) 0.061(3) 0.020(3) -0.016(3) -0.003(3) C37 0.205(10) 0.073(5) 0.109(6) 0.008(4) 0.059(6) -0.021(6) C38 0.211(10) 0.067(5) 0.131(7) -0.017(5) 0.057(7) -0.023(6) C39 0.058(3) 0.036(3) 0.060(3) 0.004(2) 0.002(2) -0.001(2) C40 0.084(4) 0.041(3) 0.083(4) -0.002(3) 0.007(3) -0.004(3) C41 0.123(6) 0.049(3) 0.058(3) 0.011(3) 0.000(3) -0.006(3) Al' 0.0329(7) 0.0527(8) 0.0425(7) 0.0214(6) 0.0064(6) 0.0087(6) O1' 0.036(2) 0.045(2) 0.040(2) 0.0162(13) 0.0079(14) 0.0025(13) C1' 0.038(2) 0.029(2) 0.034(2) 0.002(2) 0.003(2) 0.005(2) C2' 0.038(2) 0.024(2) 0.033(2) 0.003(2) 0.003(2) 0.002(2) C3' 0.042(2) 0.032(2) 0.039(2) 0.003(2) 0.000(2) 0.005(2) C4' 0.047(3) 0.034(2) 0.040(2) 0.004(2) -0.010(2) 0.003(2) C5' 0.058(3) 0.030(2) 0.033(2) 0.007(2) 0.002(2) 0.005(2) C6' 0.046(3) 0.032(2) 0.035(2) 0.011(2) 0.008(2) 0.011(2) C7' 0.029(2) 0.029(2) 0.035(2) 0.006(2) 0.003(2) 0.001(2) N7' 0.032(2) 0.032(2) 0.031(2) 0.0065(14) 0.0033(15) 0.0004(15) C8' 0.055(3) 0.042(2) 0.034(2) 0.012(2) 0.009(2) 0.014(2) N8' 0.054(2) 0.045(2) 0.033(2) 0.010(2) 0.013(2) 0.009(2) C9' 0.053(3) 0.067(3) 0.058(3) 0.021(3) -0.012(2) 0.001(3) C10' 0.064(4) 0.051(3) 0.091(4) 0.019(3) 0.030(3) 0.014(3) C11' 0.066(4) 0.060(3) 0.062(3) 0.000(3) 0.014(3) 0.018(3) C12' 0.080(5) 0.100(5) 0.114(6) -0.039(5) 0.012(4) 0.012(4) C13' 0.066(4) 0.088(4) 0.066(4) 0.002(3) 0.028(3) -0.002(3) C14' 0.044(3) 0.114(5) 0.061(3) 0.028(3) -0.004(3) 0.005(3) C15' 0.046(3) 0.071(3) 0.048(3) 0.007(2) 0.002(2) 0.002(2) C16' 0.089(5) 0.060(4) 0.082(4) 0.008(3) 0.006(4) 0.005(3) C17' 0.051(3) 0.097(5) 0.064(4) 0.009(3) -0.006(3) 0.004(3) C18' 0.031(2) 0.039(2) 0.030(2) 0.013(2) 0.000(2) 0.001(2) C19' 0.038(2) 0.040(2) 0.035(2) 0.006(2) 0.001(2) 0.002(2) C20' 0.057(3) 0.052(3) 0.033(2) 0.005(2) 0.004(2) -0.005(2) C21' 0.074(4) 0.059(3) 0.036(3) 0.020(2) 0.002(2) 0.001(3) C22' 0.065(3) 0.038(3) 0.044(3) 0.016(2) 0.004(2) 0.002(2) C23' 0.047(3) 0.038(2) 0.036(2) 0.008(2) 0.003(2) 0.002(2) C24' 0.048(3) 0.042(3) 0.035(2) 0.001(2) 0.003(2) -0.005(2) C25' 0.068(3) 0.042(3) 0.063(3) 0.003(2) 0.011(3) 0.009(2) C26' 0.080(4) 0.061(3) 0.061(3) 0.001(3) -0.007(3) -0.017(3) C27' 0.070(3) 0.039(3) 0.038(2) 0.004(2) 0.009(2) -0.010(2) C28' 0.080(5) 0.113(6) 0.064(4) -0.016(4) 0.000(3) -0.042(4) C29' 0.162(7) 0.041(3) 0.065(4) 0.006(3) 0.022(4) 0.020(4) C30' 0.054(3) 0.038(2) 0.032(2) 0.014(2) 0.009(2) 0.012(2) C31' 0.050(3) 0.044(2) 0.032(2) 0.011(2) 0.006(2) 0.014(2) C32' 0.050(3) 0.060(3) 0.038(2) 0.004(2) 0.008(2) 0.012(2) C33' 0.046(3) 0.071(4) 0.052(3) 0.019(3) 0.012(2) 0.005(3) C34' 0.068(4) 0.048(3) 0.059(3) 0.007(2) 0.009(3) -0.003(3) C35' 0.066(3) 0.042(3) 0.047(3) 0.009(2) 0.014(2) 0.012(2) C36' 0.055(3) 0.050(3) 0.045(3) -0.002(2) 0.005(2) 0.009(2) C37' 0.091(4) 0.071(4) 0.052(3) -0.008(3) -0.007(3) 0.012(3) C38' 0.111(5) 0.045(3) 0.062(3) 0.009(3) -0.001(3) 0.007(3) C39' 0.094(5) 0.057(3) 0.077(4) -0.018(3) 0.025(4) 0.004(3) C40' 0.145(10) 0.061(6) 0.081(7) -0.026(5) -0.014(7) 0.036(6) C41' 0.214(15) 0.102(8) 0.029(4) -0.004(5) 0.016(6) 0.037(9) _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 O1 1.773(3) . ? Al C10A 1.899(14) . ? Al C14 1.934(11) . ? Al N7 1.983(4) . ? Al C10 2.006(9) . ? Al C14A 2.013(12) . ? O1 C1 1.322(5) . ? C1 C2 1.414(6) . ? C1 C6 1.417(6) . ? C2 C3 1.403(6) . ? C2 C7 1.433(6) . ? C3 C4 1.378(7) . ? C4 C5 1.376(7) . ? C4 C9 1.526(7) . ? C5 C6 1.390(6) . ? C6 C8 1.462(6) . ? C7 N7 1.293(6) . ? N7 C18 1.451(5) . ? C8 N8 1.278(6) . ? N8 C30 1.428(6) . ? C10 C11 1.549(12) . ? C11 C13 1.613(15) . ? C11 C12 1.630(14) . ? C10A C11A 1.58(2) . ? C11A C13A 1.67(2) . ? C11A C12A 1.71(2) . ? C14 C15 1.574(14) . ? C15 C16 1.60(2) . ? C15 C17 1.79(2) . ? C14A C15A 1.542(14) . ? C15A C16A 1.66(2) . ? C15A C17A 1.734(15) . ? C18 C23 1.406(7) . ? C18 C19 1.410(6) . ? C19 C20 1.381(7) . ? C19 C24 1.510(8) . ? C20 C21 1.361(8) . ? C21 C22 1.385(8) . ? C22 C23 1.386(7) . ? C23 C27 1.513(7) . ? C24 C25 1.522(12) . ? C24 C26 1.543(11) . ? C27 C28 1.527(11) . ? C27 C29 1.527(9) . ? C30 C35 1.407(7) . ? C30 C31 1.407(7) . ? C31 C32 1.381(8) . ? C31 C36 1.523(7) . ? C32 C33 1.378(8) . ? C33 C34 1.385(8) . ? C34 C35 1.367(7) . ? C35 C39 1.528(7) . ? C36 C38 1.491(10) . ? C36 C37 1.517(10) . ? C39 C41 1.524(8) . ? C39 C40 1.534(7) . ? Al' O1' 1.791(3) . ? Al' C14' 1.955(6) . ? Al' C10' 1.985(6) . ? Al' N7' 1.991(4) . ? O1' C1' 1.323(5) . ? C1' C2' 1.409(6) . ? C1' C6' 1.423(6) . ? C2' C3' 1.411(6) . ? C2' C7' 1.449(6) . ? C3' C4' 1.375(6) . ? C4' C5' 1.386(7) . ? C4' C9' 1.518(7) . ? C5' C6' 1.389(6) . ? C6' C8' 1.465(6) . ? C7' N7' 1.289(5) . ? N7' C18' 1.455(5) . ? C8' N8' 1.281(6) . ? N8' C30' 1.425(6) . ? C10' C11' 1.530(8) . ? C11' C13' 1.498(8) . ? C11' C12' 1.529(8) . ? C14' C15' 1.511(7) . ? C15' C16' 1.510(8) . ? C15' C17' 1.525(7) . ? C18' C23' 1.394(6) . ? C18' C19' 1.399(6) . ? C19' C20' 1.389(6) . ? C19' C24' 1.523(6) . ? C20' C21' 1.378(7) . ? C21' C22' 1.379(7) . ? C22' C23' 1.400(6) . ? C23' C27' 1.522(6) . ? C24' C25' 1.529(7) . ? C24' C26' 1.536(7) . ? C27' C29' 1.501(8) . ? C27' C28' 1.542(8) . ? C30' C31' 1.398(6) . ? C30' C35' 1.404(7) . ? C31' C32' 1.386(7) . ? C31' C36' 1.522(7) . ? C32' C33' 1.368(8) . ? C33' C34' 1.382(8) . ? C34' C35' 1.381(7) . ? C35' C39' 1.525(7) . ? C36' C37' 1.528(7) . ? C36' C38' 1.530(7) . ? C39' C41' 1.421(11) . ? C39' C40B 1.43(2) . ? C39' C40' 1.543(10) . ? C39' C41B 1.61(2) . ? 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 O1 Al C10A 121.0(5) . . ? O1 Al C14 115.5(4) . . ? O1 Al N7 94.16(15) . . ? C10A Al N7 116.7(6) . . ? C14 Al N7 121.0(4) . . ? O1 Al C10 110.0(4) . . ? C14 Al C10 110.4(5) . . ? N7 Al C10 104.3(3) . . ? O1 Al C14A 109.6(5) . . ? C10A Al C14A 110.2(7) . . ? N7 Al C14A 103.0(4) . . ? C1 O1 Al 131.9(3) . . ? O1 C1 C2 122.0(4) . . ? O1 C1 C6 118.9(4) . . ? C2 C1 C6 119.1(4) . . ? C3 C2 C1 118.7(4) . . ? C3 C2 C7 118.9(4) . . ? C1 C2 C7 122.4(4) . . ? C4 C3 C2 122.8(4) . . ? C5 C4 C3 117.3(4) . . ? C5 C4 C9 121.2(5) . . ? C3 C4 C9 121.5(5) . . ? C4 C5 C6 123.5(4) . . ? C5 C6 C1 118.6(4) . . ? C5 C6 C8 122.3(4) . . ? C1 C6 C8 119.1(4) . . ? N7 C7 C2 127.0(4) . . ? C7 N7 C18 117.7(4) . . ? C7 N7 Al 122.2(3) . . ? C18 N7 Al 119.9(3) . . ? N8 C8 C6 123.3(4) . . ? C8 N8 C30 117.8(4) . . ? C11 C10 Al 119.6(7) . . ? C10 C11 C13 98.8(9) . . ? C10 C11 C12 101.1(10) . . ? C13 C11 C12 99.4(10) . . ? C11A C10A Al 117.8(11) . . ? C10A C11A C13A 98.3(12) . . ? C10A C11A C12A 98.7(13) . . ? C13A C11A C12A 94.2(12) . . ? C15 C14 Al 119.6(8) . . ? C14 C15 C16 102.5(12) . . ? C14 C15 C17 89.8(9) . . ? C16 C15 C17 91.7(10) . . ? C15A C14A Al 113.2(9) . . ? C14A C15A C16A 100.2(11) . . ? C14A C15A C17A 96.2(10) . . ? C16A C15A C17A 89.7(11) . . ? C23 C18 C19 121.7(4) . . ? C23 C18 N7 118.6(4) . . ? C19 C18 N7 119.7(4) . . ? C20 C19 C18 117.5(5) . . ? C20 C19 C24 121.0(5) . . ? C18 C19 C24 121.4(4) . . ? C21 C20 C19 121.8(5) . . ? C20 C21 C22 120.4(5) . . ? C21 C22 C23 121.0(5) . . ? C22 C23 C18 117.6(5) . . ? C22 C23 C27 119.8(5) . . ? C18 C23 C27 122.6(4) . . ? C19 C24 C25 109.4(7) . . ? C19 C24 C26 113.4(6) . . ? C25 C24 C26 110.3(6) . . ? C23 C27 C28 111.1(6) . . ? C23 C27 C29 112.5(5) . . ? C28 C27 C29 110.6(6) . . ? C35 C30 C31 121.5(4) . . ? C35 C30 N8 118.8(4) . . ? C31 C30 N8 119.4(4) . . ? C32 C31 C30 117.6(5) . . ? C32 C31 C36 120.6(5) . . ? C30 C31 C36 121.7(5) . . ? C33 C32 C31 121.2(5) . . ? C32 C33 C34 120.2(5) . . ? C35 C34 C33 121.1(5) . . ? C34 C35 C30 118.2(4) . . ? C34 C35 C39 122.3(4) . . ? C30 C35 C39 119.4(4) . . ? C38 C36 C37 108.8(6) . . ? C38 C36 C31 112.4(6) . . ? C37 C36 C31 112.5(5) . . ? C41 C39 C35 111.4(4) . . ? C41 C39 C40 109.0(4) . . ? C35 C39 C40 113.1(4) . . ? O1' Al' C14' 118.5(2) . . ? O1' Al' C10' 107.6(2) . . ? C14' Al' C10' 119.4(3) . . ? O1' Al' N7' 93.48(14) . . ? C14' Al' N7' 106.3(2) . . ? C10' Al' N7' 108.0(2) . . ? C1' O1' Al' 124.0(3) . . ? O1' C1' C2' 122.3(4) . . ? O1' C1' C6' 119.7(4) . . ? C2' C1' C6' 118.0(4) . . ? C1' C2' C3' 120.4(4) . . ? C1' C2' C7' 122.3(4) . . ? C3' C2' C7' 117.1(4) . . ? C4' C3' C2' 121.6(4) . . ? C3' C4' C5' 117.6(4) . . ? C3' C4' C9' 121.1(4) . . ? C5' C4' C9' 121.3(4) . . ? C4' C5' C6' 123.5(4) . . ? C5' C6' C1' 119.0(4) . . ? C5' C6' C8' 121.0(4) . . ? C1' C6' C8' 120.0(4) . . ? N7' C7' C2' 126.0(4) . . ? C7' N7' C18' 117.8(3) . . ? C7' N7' Al' 119.0(3) . . ? C18' N7' Al' 122.7(3) . . ? N8' C8' C6' 121.1(4) . . ? C8' N8' C30' 118.9(4) . . ? C11' C10' Al' 115.8(4) . . ? C13' C11' C12' 109.9(5) . . ? C13' C11' C10' 111.3(5) . . ? C12' C11' C10' 113.3(5) . . ? C15' C14' Al' 123.1(4) . . ? C16' C15' C14' 110.8(5) . . ? C16' C15' C17' 111.1(5) . . ? C14' C15' C17' 112.0(4) . . ? C23' C18' C19' 122.4(4) . . ? C23' C18' N7' 119.2(4) . . ? C19' C18' N7' 118.3(4) . . ? C20' C19' C18' 117.7(4) . . ? C20' C19' C24' 119.8(4) . . ? C18' C19' C24' 122.3(4) . . ? C21' C20' C19' 120.9(4) . . ? C20' C21' C22' 120.7(4) . . ? C21' C22' C23' 120.6(4) . . ? C18' C23' C22' 117.7(4) . . ? C18' C23' C27' 123.4(4) . . ? C22' C23' C27' 119.0(4) . . ? C19' C24' C25' 110.7(4) . . ? C19' C24' C26' 113.6(4) . . ? C25' C24' C26' 109.0(4) . . ? C29' C27' C23' 111.8(5) . . ? C29' C27' C28' 112.3(5) . . ? C23' C27' C28' 109.9(4) . . ? C31' C30' C35' 121.4(4) . . ? C31' C30' N8' 117.9(4) . . ? C35' C30' N8' 120.5(4) . . ? C32' C31' C30' 118.0(4) . . ? C32' C31' C36' 121.9(4) . . ? C30' C31' C36' 120.1(4) . . ? C33' C32' C31' 121.4(5) . . ? C32' C33' C34' 120.1(5) . . ? C35' C34' C33' 121.1(5) . . ? C34' C35' C30' 118.0(4) . . ? C34' C35' C39' 120.9(5) . . ? C30' C35' C39' 121.1(5) . . ? C31' C36' C37' 113.7(4) . . ? C31' C36' C38' 111.3(4) . . ? C37' C36' C38' 109.5(4) . . ? C41' C39' C35' 113.0(6) . . ? C40B C39' C35' 118.7(13) . . ? C41' C39' C40' 114.8(7) . . ? C35' C39' C40' 109.8(6) . . ? C40B C39' C41B 108.9(15) . . ? C35' C39' C41B 112.8(11) . . ? _refine_diff_density_max 0.429 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.047 #===END