# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Li, Wenyi' 'Wu, Wenting' 'Yao, Yingming' 'Zhang, Yong' 'Shen, Qi' _publ_contact_author_name 'Yao, Yingming' _publ_contact_author_email yaoym@suda.edu.cn _publ_section_title ; Manuscript Title: Bimetallic aluminum alkyl complexes as highly active initiators for the polymerization of -caprolactone ; # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_fax 86-512-65880305 _publ_contact_author_phone 86-512-65882806 _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal 'Dalton Transactions ' _publ_requested_category FM _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title_footnote ; ? ; _publ_section_synopsis ; ENTER SYNOPSIS ; #============================================================================== # TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_references ; ENTER OTHER REFERENCES Rigaku/MSC and Rigaku Corporation. (2003). CrystalStructure. Single Crystal Structure Analysis Software. Version 3.5.1. Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #============================================================================== data_complex1 _database_code_depnum_ccdc_archive 'CCDC 836238' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H33 Al N2 O2' _chemical_formula_sum 'C24 H33 Al N2 O2' _chemical_formula_weight 408.50 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 monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.349(3) _cell_length_b 8.789(2) _cell_length_c 12.741(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.768(6) _cell_angle_gamma 90.00 _cell_volume 1134.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5765 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.196 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 440 _exptl_absorpt_coefficient_mu 0.111 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.659 _exptl_absorpt_correction_T_max 0.942 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6588 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 27.45 _reflns_number_total 4427 _reflns_number_gt 3659 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0518P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(16) _refine_ls_number_reflns 4427 _refine_ls_number_parameters 268 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.0991 _refine_ls_wR_factor_gt 0.0919 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.66247(6) 0.33032(7) 0.77666(5) 0.04022(16) Uani 1 1 d . . . O1 O 0.83245(14) 0.3371(2) 0.77656(11) 0.0498(4) Uani 1 1 d . . . O2 O 0.66414(16) 0.45528(17) 0.88795(12) 0.0488(4) Uani 1 1 d . . . N1 N 0.66755(17) 0.1088(2) 0.69967(14) 0.0434(4) Uani 1 1 d . . . N2 N 0.57693(17) 0.1623(2) 0.85543(14) 0.0420(4) Uani 1 1 d . . . C1 C 0.9077(2) 0.2872(3) 0.70987(17) 0.0454(6) Uani 1 1 d . . . C2 C 1.0368(2) 0.3469(3) 0.72338(18) 0.0493(5) Uani 1 1 d . . . C3 C 1.1169(2) 0.3003(3) 0.6552(2) 0.0552(7) Uani 1 1 d . . . H3 H 1.2012 0.3441 0.6627 0.066 Uiso 1 1 calc R . . C4 C 1.0787(3) 0.1919(3) 0.5761(2) 0.0594(7) Uani 1 1 d . . . C5 C 0.9538(2) 0.1296(3) 0.56556(18) 0.0521(6) Uani 1 1 d . . . H5 H 0.9265 0.0539 0.5137 0.062 Uiso 1 1 calc R . . C6 C 0.8677(2) 0.1767(3) 0.63015(17) 0.0458(5) Uani 1 1 d . . . C7 C 0.6982(2) 0.4121(3) 0.99116(17) 0.0439(5) Uani 1 1 d . . . C8 C 0.8002(2) 0.4883(3) 1.06223(19) 0.0503(6) Uani 1 1 d . . . C9 C 0.8307(2) 0.4420(3) 1.16836(19) 0.0540(6) Uani 1 1 d . . . H9 H 0.8987 0.4925 1.2158 0.065 Uiso 1 1 calc R . . C10 C 0.7646(2) 0.3241(3) 1.20744(17) 0.0559(6) Uani 1 1 d . . . C11 C 0.6647(2) 0.2497(3) 1.13611(19) 0.0506(6) Uani 1 1 d . . . H11 H 0.6191 0.1692 1.1608 0.061 Uiso 1 1 calc R . . C12 C 0.6315(2) 0.2927(2) 1.02898(18) 0.0449(5) Uani 1 1 d . . . C13 C 0.7299(2) 0.1110(3) 0.60574(18) 0.0518(6) Uani 1 1 d . . . H13A H 0.6750 0.1711 0.5488 0.062 Uiso 1 1 calc R . . H13B H 0.7337 0.0068 0.5791 0.062 Uiso 1 1 calc R . . C14 C 0.7369(2) 0.0095(3) 0.78590(17) 0.0459(5) Uani 1 1 d . . . H14A H 0.8317 0.0317 0.8012 0.055 Uiso 1 1 calc R . . H14B H 0.7242 -0.0975 0.7648 0.055 Uiso 1 1 calc R . . C15 C 0.6783(2) 0.0411(3) 0.88529(18) 0.0472(6) Uani 1 1 d . . . H15A H 0.6379 -0.0514 0.9071 0.057 Uiso 1 1 calc R . . H15B H 0.7476 0.0750 0.9451 0.057 Uiso 1 1 calc R . . C16 C 0.5286(2) 0.0619(3) 0.67284(19) 0.0524(6) Uani 1 1 d . . . H16A H 0.5219 -0.0471 0.6564 0.063 Uiso 1 1 calc R . . H16B H 0.4815 0.1184 0.6103 0.063 Uiso 1 1 calc R . . C17 C 0.4697(2) 0.0970(3) 0.77141(19) 0.0538(6) Uani 1 1 d . . . H17A H 0.3970 0.1700 0.7526 0.065 Uiso 1 1 calc R . . H17B H 0.4353 0.0037 0.7978 0.065 Uiso 1 1 calc R . . C18 C 0.5254(2) 0.2152(3) 0.94956(19) 0.0514(6) Uani 1 1 d . . . H18A H 0.4918 0.1280 0.9838 0.062 Uiso 1 1 calc R . . H18B H 0.4521 0.2859 0.9259 0.062 Uiso 1 1 calc R . . C19 C 1.0797(2) 0.4631(3) 0.8102(2) 0.0650(7) Uani 1 1 d . . . H19A H 1.1717 0.4886 0.8139 0.097 Uiso 1 1 calc R . . H19B H 1.0689 0.4216 0.8784 0.097 Uiso 1 1 calc R . . H19C H 1.0261 0.5539 0.7941 0.097 Uiso 1 1 calc R . . C20 C 1.1671(3) 0.1457(5) 0.5002(2) 0.0840(10) Uani 1 1 d . . . H20A H 1.1754 0.2300 0.4529 0.126 Uiso 1 1 calc R . . H20B H 1.1288 0.0589 0.4579 0.126 Uiso 1 1 calc R . . H20C H 1.2536 0.1185 0.5412 0.126 Uiso 1 1 calc R . . C21 C 0.8702(3) 0.6162(4) 1.0201(2) 0.0716(8) Uani 1 1 d . . . H21A H 0.8094 0.7001 0.9996 0.107 Uiso 1 1 calc R . . H21B H 0.9030 0.5818 0.9580 0.107 Uiso 1 1 calc R . . H21C H 0.9436 0.6498 1.0753 0.107 Uiso 1 1 calc R . . C22 C 0.7992(3) 0.2790(4) 1.3246(2) 0.0785(9) Uani 1 1 d . . . H22A H 0.7775 0.1727 1.3318 0.118 Uiso 1 1 calc R . . H22B H 0.7493 0.3412 1.3651 0.118 Uiso 1 1 calc R . . H22C H 0.8929 0.2943 1.3517 0.118 Uiso 1 1 calc R . . C23 C 0.5421(3) 0.4368(3) 0.6588(2) 0.0598(7) Uani 1 1 d . . . H23A H 0.5536 0.3956 0.5899 0.072 Uiso 1 1 calc R . . H23B H 0.4505 0.4190 0.6651 0.072 Uiso 1 1 calc R . . C24 C 0.5696(3) 0.6068(3) 0.6622(2) 0.0600(7) Uani 1 1 d . . . H24A H 0.5606 0.6471 0.7312 0.090 Uiso 1 1 calc R . . H24B H 0.5070 0.6570 0.6058 0.090 Uiso 1 1 calc R . . H24C H 0.6586 0.6247 0.6518 0.090 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0415(3) 0.0360(3) 0.0396(3) 0.0027(3) -0.0002(2) -0.0065(3) O1 0.0447(8) 0.0539(9) 0.0491(8) -0.0106(8) 0.0057(6) -0.0161(8) O2 0.0618(10) 0.0397(8) 0.0421(9) 0.0009(7) 0.0043(7) -0.0030(8) N1 0.0401(9) 0.0448(10) 0.0421(10) -0.0015(8) 0.0008(8) -0.0107(9) N2 0.0396(9) 0.0400(10) 0.0444(10) 0.0017(8) 0.0035(8) -0.0045(8) C1 0.0435(11) 0.0502(15) 0.0397(11) 0.0062(9) 0.0018(10) -0.0061(10) C2 0.0430(11) 0.0460(13) 0.0544(13) 0.0107(11) -0.0002(10) -0.0078(11) C3 0.0392(11) 0.0609(17) 0.0644(15) 0.0217(13) 0.0081(11) -0.0036(12) C4 0.0538(14) 0.0705(17) 0.0544(15) 0.0197(13) 0.0121(12) 0.0082(13) C5 0.0544(14) 0.0613(15) 0.0394(12) 0.0087(11) 0.0068(10) 0.0036(12) C6 0.0447(12) 0.0532(13) 0.0366(11) 0.0042(10) 0.0016(10) -0.0044(11) C7 0.0480(12) 0.0422(13) 0.0407(12) -0.0014(9) 0.0074(10) 0.0090(10) C8 0.0503(13) 0.0482(14) 0.0514(14) -0.0107(11) 0.0080(10) 0.0048(11) C9 0.0557(14) 0.0575(15) 0.0456(14) -0.0121(12) 0.0029(11) 0.0137(13) C10 0.0662(14) 0.0587(15) 0.0419(12) -0.0040(13) 0.0088(11) 0.0301(15) C11 0.0585(14) 0.0483(13) 0.0489(13) 0.0078(11) 0.0204(11) 0.0159(12) C12 0.0450(11) 0.0444(13) 0.0463(12) -0.0001(9) 0.0119(10) 0.0098(10) C13 0.0508(12) 0.0587(14) 0.0436(13) -0.0097(11) 0.0042(10) -0.0102(12) C14 0.0493(12) 0.0349(11) 0.0508(13) 0.0000(9) 0.0038(10) -0.0051(10) C15 0.0509(13) 0.0396(12) 0.0501(14) 0.0067(10) 0.0077(11) 0.0012(10) C16 0.0476(13) 0.0498(14) 0.0535(14) -0.0068(11) -0.0044(11) -0.0150(11) C17 0.0402(11) 0.0553(15) 0.0628(15) 0.0003(12) 0.0032(11) -0.0161(12) C18 0.0485(13) 0.0499(14) 0.0581(15) 0.0047(11) 0.0162(11) 0.0017(11) C19 0.0525(14) 0.0605(16) 0.0757(18) 0.0047(14) -0.0015(12) -0.0207(13) C20 0.0689(18) 0.108(3) 0.083(2) 0.0196(19) 0.0338(16) 0.0172(18) C21 0.0833(19) 0.0657(17) 0.0631(17) -0.0166(14) 0.0090(14) -0.0202(17) C22 0.105(2) 0.085(2) 0.0435(14) 0.0008(13) 0.0097(15) 0.0322(18) C23 0.0668(16) 0.0490(14) 0.0535(14) 0.0063(11) -0.0119(12) -0.0069(13) C24 0.0756(17) 0.0494(13) 0.0538(15) 0.0122(12) 0.0104(13) 0.0033(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O1 1.7604(16) . ? Al1 O2 1.7909(17) . ? Al1 C23 1.980(2) . ? Al1 N2 2.0819(19) . ? Al1 N1 2.185(2) . ? O1 C1 1.338(3) . ? O2 C7 1.345(3) . ? N1 C16 1.467(3) . ? N1 C14 1.471(3) . ? N1 C13 1.471(3) . ? N2 C18 1.483(3) . ? N2 C15 1.489(3) . ? N2 C17 1.491(3) . ? C1 C6 1.405(3) . ? C1 C2 1.413(3) . ? C2 C3 1.380(3) . ? C2 C19 1.504(4) . ? C3 C4 1.385(4) . ? C3 H3 0.9400 . ? C4 C5 1.384(4) . ? C4 C20 1.516(4) . ? C5 C6 1.394(3) . ? C5 H5 0.9400 . ? C6 C13 1.512(3) . ? C7 C12 1.395(3) . ? C7 C8 1.411(3) . ? C8 C9 1.385(3) . ? C8 C21 1.496(4) . ? C9 C10 1.389(4) . ? C9 H9 0.9400 . ? C10 C11 1.392(4) . ? C10 C22 1.514(3) . ? C11 C12 1.390(3) . ? C11 H11 0.9400 . ? C12 C18 1.497(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 C15 1.537(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 C17 1.535(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 C24 1.519(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? 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 Al1 O2 97.55(8) . . ? O1 Al1 C23 117.24(11) . . ? O2 Al1 C23 102.32(10) . . ? O1 Al1 N2 123.21(8) . . ? O2 Al1 N2 89.41(8) . . ? C23 Al1 N2 115.93(10) . . ? O1 Al1 N1 85.10(7) . . ? O2 Al1 N1 154.76(8) . . ? C23 Al1 N1 98.62(9) . . ? N2 Al1 N1 68.66(7) . . ? C1 O1 Al1 134.46(13) . . ? C7 O2 Al1 124.03(14) . . ? C16 N1 C14 108.22(17) . . ? C16 N1 C13 112.67(17) . . ? C14 N1 C13 112.78(19) . . ? C16 N1 Al1 104.06(14) . . ? C14 N1 Al1 104.26(13) . . ? C13 N1 Al1 114.12(15) . . ? C18 N2 C15 111.61(17) . . ? C18 N2 C17 111.32(17) . . ? C15 N2 C17 106.89(18) . . ? C18 N2 Al1 115.22(14) . . ? C15 N2 Al1 106.49(13) . . ? C17 N2 Al1 104.74(14) . . ? O1 C1 C6 124.17(19) . . ? O1 C1 C2 117.3(2) . . ? C6 C1 C2 118.5(2) . . ? C3 C2 C1 119.2(2) . . ? C3 C2 C19 122.6(2) . . ? C1 C2 C19 118.1(2) . . ? C2 C3 C4 122.9(2) . . ? C2 C3 H3 118.6 . . ? C4 C3 H3 118.6 . . ? C5 C4 C3 117.7(2) . . ? C5 C4 C20 120.3(3) . . ? C3 C4 C20 121.9(3) . . ? C4 C5 C6 121.5(3) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 120.2(2) . . ? C5 C6 C13 117.1(2) . . ? C1 C6 C13 122.6(2) . . ? O2 C7 C12 120.0(2) . . ? O2 C7 C8 120.4(2) . . ? C12 C7 C8 119.5(2) . . ? C9 C8 C7 118.6(2) . . ? C9 C8 C21 122.7(2) . . ? C7 C8 C21 118.7(2) . . ? C8 C9 C10 122.6(2) . . ? C8 C9 H9 118.7 . . ? C10 C9 H9 118.7 . . ? C9 C10 C11 118.1(2) . . ? C9 C10 C22 120.9(2) . . ? C11 C10 C22 121.0(3) . . ? C12 C11 C10 121.0(2) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C11 C12 C7 120.2(2) . . ? C11 C12 C18 122.7(2) . . ? C7 C12 C18 117.1(2) . . ? N1 C13 C6 112.93(18) . . ? N1 C13 H13A 109.0 . . ? C6 C13 H13A 109.0 . . ? N1 C13 H13B 109.0 . . ? C6 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? N1 C14 C15 107.08(18) . . ? N1 C14 H14A 110.3 . . ? C15 C14 H14A 110.3 . . ? N1 C14 H14B 110.3 . . ? C15 C14 H14B 110.3 . . ? H14A C14 H14B 108.6 . . ? N2 C15 C14 107.14(17) . . ? N2 C15 H15A 110.3 . . ? C14 C15 H15A 110.3 . . ? N2 C15 H15B 110.3 . . ? C14 C15 H15B 110.3 . . ? H15A C15 H15B 108.5 . . ? N1 C16 C17 106.67(17) . . ? N1 C16 H16A 110.4 . . ? C17 C16 H16A 110.4 . . ? N1 C16 H16B 110.4 . . ? C17 C16 H16B 110.4 . . ? H16A C16 H16B 108.6 . . ? N2 C17 C16 107.64(17) . . ? N2 C17 H17A 110.2 . . ? C16 C17 H17A 110.2 . . ? N2 C17 H17B 110.2 . . ? C16 C17 H17B 110.2 . . ? H17A C17 H17B 108.5 . . ? N2 C18 C12 110.76(18) . . ? N2 C18 H18A 109.5 . . ? C12 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? C12 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? C2 C19 H19A 109.5 . . ? C2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C4 C20 H20A 109.5 . . ? C4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C8 C21 H21A 109.5 . . ? C8 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C8 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C10 C22 H22A 109.5 . . ? C10 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C10 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 Al1 110.99(17) . . ? C24 C23 H23A 109.4 . . ? Al1 C23 H23A 109.4 . . ? C24 C23 H23B 109.4 . . ? Al1 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.154 _refine_diff_density_min -0.171 _refine_diff_density_rms 0.035 #============================================================================== data_complex2 _database_code_depnum_ccdc_archive 'CCDC 836239' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H48 Al2 N2 O2' _chemical_formula_sum 'C30 H48 Al2 N2 O2' _chemical_formula_weight 522.66 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' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1586(16) _cell_length_b 9.0924(19) _cell_length_c 20.628(4) _cell_angle_alpha 90.850(6) _cell_angle_beta 90.895(6) _cell_angle_gamma 95.683(6) _cell_volume 1522.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6103 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.140 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 0.123 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.786 _exptl_absorpt_correction_T_max 0.938 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14219 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5604 _reflns_number_gt 4266 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0799P)^2^+0.8723P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5604 _refine_ls_number_parameters 341 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0851 _refine_ls_R_factor_gt 0.0652 _refine_ls_wR_factor_ref 0.1839 _refine_ls_wR_factor_gt 0.1713 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.33911(10) 0.24040(9) 0.92647(4) 0.0394(2) Uani 1 1 d . . . Al2 Al 0.84096(13) 0.72818(12) 0.57355(5) 0.0584(3) Uani 1 1 d D . . O1 O 0.2297(3) 0.2491(2) 0.85266(10) 0.0471(5) Uani 1 1 d . . . O2 O 0.7216(3) 0.6947(2) 0.64276(10) 0.0529(6) Uani 1 1 d . A . N1 N 0.4278(3) 0.4639(2) 0.93441(10) 0.0354(5) Uani 1 1 d . . . N2 N 0.9311(3) 0.5234(3) 0.56522(12) 0.0485(6) Uani 1 1 d . . . C1 C 0.1430(3) 0.3649(3) 0.83961(13) 0.0420(7) Uani 1 1 d . . . C2 C -0.0203(4) 0.3397(4) 0.81616(14) 0.0474(7) Uani 1 1 d . . . C3 C -0.1037(4) 0.4619(4) 0.80491(14) 0.0522(8) Uani 1 1 d . . . H3 H -0.2133 0.4464 0.7895 0.063 Uiso 1 1 calc R . . C4 C -0.0349(4) 0.6064(4) 0.81502(14) 0.0519(8) Uani 1 1 d . . . C5 C 0.1288(4) 0.6276(4) 0.83652(14) 0.0483(7) Uani 1 1 d . . . H5 H 0.1795 0.7242 0.8430 0.058 Uiso 1 1 calc R . . C6 C 0.2180(3) 0.5081(3) 0.84859(13) 0.0405(6) Uani 1 1 d . . . C7 C 0.3972(3) 0.5273(3) 0.86814(13) 0.0407(6) Uani 1 1 d . . . H7A H 0.4361 0.6328 0.8687 0.049 Uiso 1 1 calc R . . H7B H 0.4608 0.4781 0.8358 0.049 Uiso 1 1 calc R . . C8 C 0.6094(3) 0.4870(3) 0.94805(13) 0.0383(6) Uani 1 1 d . . . H8A H 0.6482 0.5910 0.9412 0.046 Uiso 1 1 calc R . . H8B H 0.6663 0.4269 0.9175 0.046 Uiso 1 1 calc R . . C9 C 0.6523(3) 0.4464(3) 1.01625(13) 0.0379(6) Uani 1 1 d . . . H9A H 0.6175 0.3414 1.0225 0.045 Uiso 1 1 calc R . . H9B H 0.7721 0.4615 1.0227 0.045 Uiso 1 1 calc R . . C10 C -0.0951(4) 0.1833(4) 0.80498(17) 0.0626(9) Uani 1 1 d . . . H10A H -0.2063 0.1839 0.7877 0.094 Uiso 1 1 calc R . . H10B H -0.0980 0.1312 0.8457 0.094 Uiso 1 1 calc R . . H10C H -0.0293 0.1339 0.7743 0.094 Uiso 1 1 calc R . . C11 C -0.1313(5) 0.7380(5) 0.80335(19) 0.0748(11) Uani 1 1 d . . . H11A H -0.1387 0.7554 0.7572 0.112 Uiso 1 1 calc R . . H11B H -0.0757 0.8248 0.8250 0.112 Uiso 1 1 calc R . . H11C H -0.2413 0.7181 0.8204 0.112 Uiso 1 1 calc R . . C12 C 0.1860(4) 0.1765(3) 0.99540(16) 0.0500(8) Uani 1 1 d . . . H12A H 0.1518 0.0711 0.9881 0.060 Uiso 1 1 calc R . . H12B H 0.2481 0.1855 1.0366 0.060 Uiso 1 1 calc R . . C13 C 0.0293(4) 0.2544(4) 1.00447(18) 0.0606(9) Uani 1 1 d . . . H13A H 0.0579 0.3511 1.0243 0.091 Uiso 1 1 calc R . . H13B H -0.0456 0.1958 1.0322 0.091 Uiso 1 1 calc R . . H13C H -0.0235 0.2654 0.9626 0.091 Uiso 1 1 calc R . . C14 C 0.5274(4) 0.1266(4) 0.91166(19) 0.0589(9) Uani 1 1 d . . . H14A H 0.6023 0.1792 0.8812 0.071 Uiso 1 1 calc R . . H14B H 0.5878 0.1181 0.9526 0.071 Uiso 1 1 calc R . . C15 C 0.4728(5) -0.0270(4) 0.8846(2) 0.0700(10) Uani 1 1 d . . . H15A H 0.4081 -0.0829 0.9166 0.105 Uiso 1 1 calc R . . H15B H 0.5689 -0.0771 0.8743 0.105 Uiso 1 1 calc R . . H15C H 0.4064 -0.0190 0.8456 0.105 Uiso 1 1 calc R . . C16 C 0.6451(4) 0.5609(4) 0.65772(13) 0.0462(7) Uani 1 1 d . . . C17 C 0.4845(4) 0.5491(4) 0.68224(14) 0.0495(8) Uani 1 1 d . A . C18 C 0.4113(4) 0.4108(4) 0.69623(15) 0.0568(9) Uani 1 1 d . . . H18 H 0.3043 0.4025 0.7129 0.068 Uiso 1 1 calc R A . C19 C 0.4885(5) 0.2823(4) 0.68682(15) 0.0587(9) Uani 1 1 d . A . C20 C 0.6486(4) 0.2977(4) 0.66403(15) 0.0556(8) Uani 1 1 d . . . H20 H 0.7047 0.2132 0.6581 0.067 Uiso 1 1 calc R A . C21 C 0.7266(4) 0.4349(4) 0.64995(14) 0.0484(7) Uani 1 1 d . A . C22 C 0.9055(4) 0.4558(4) 0.63112(14) 0.0523(8) Uani 1 1 d . . . H22A H 0.9672 0.5194 0.6637 0.063 Uiso 1 1 calc R A . H22B H 0.9501 0.3596 0.6313 0.063 Uiso 1 1 calc R . . C23 C 1.1122(4) 0.5342(4) 0.55273(15) 0.0510(8) Uani 1 1 d . . . H23A H 1.1528 0.4379 0.5601 0.061 Uiso 1 1 calc R A . H23B H 1.1697 0.6057 0.5834 0.061 Uiso 1 1 calc R . . C24 C 1.1509(4) 0.5816(4) 0.48435(14) 0.0507(8) Uani 1 1 d . . . H24A H 1.1149 0.6800 0.4777 0.061 Uiso 1 1 calc R . . H24B H 1.2704 0.5885 0.4785 0.061 Uiso 1 1 calc R . . C25 C 0.4028(4) 0.6876(4) 0.69464(17) 0.0646(9) Uani 1 1 d . . . H25A H 0.2900 0.6616 0.7076 0.097 Uiso 1 1 calc R A . H25B H 0.4034 0.7451 0.6554 0.097 Uiso 1 1 calc R . . H25C H 0.4623 0.7456 0.7289 0.097 Uiso 1 1 calc R . . C26 C 0.4041(6) 0.1301(5) 0.7014(2) 0.0815(12) Uani 1 1 d . . . H26A H 0.3506 0.0871 0.6623 0.122 Uiso 1 1 calc R A . H26B H 0.3225 0.1389 0.7346 0.122 Uiso 1 1 calc R . . H26C H 0.4854 0.0672 0.7166 0.122 Uiso 1 1 calc R . . C27 C 1.0270(6) 0.8739(4) 0.5967(3) 0.0935(15) Uani 1 1 d . A . H27A H 1.0938 0.8349 0.6311 0.112 Uiso 1 1 calc R . . H27B H 1.0967 0.8927 0.5588 0.112 Uiso 1 1 calc R . . C28 C 0.9642(6) 1.0178(5) 0.6199(3) 0.0986(15) Uani 1 1 d . . . H28A H 0.8869 1.0495 0.5880 0.148 Uiso 1 1 calc R A . H28B H 1.0562 1.0932 0.6254 0.148 Uiso 1 1 calc R . . H28C H 0.9095 1.0021 0.6610 0.148 Uiso 1 1 calc R . . C29 C 0.7309(12) 0.8050(10) 0.5010(5) 0.068(2) Uani 0.50 1 d PD A 1 H29A H 0.7197 0.9102 0.5084 0.081 Uiso 0.50 1 calc PR A 1 H29B H 0.7955 0.7948 0.4618 0.081 Uiso 0.50 1 calc PR A 1 C29' C 0.6784(13) 0.7379(10) 0.5009(5) 0.068(2) Uani 0.50 1 d PD A 2 H29C H 0.7391 0.7579 0.4608 0.081 Uiso 0.50 1 calc PR A 2 H29D H 0.6157 0.6407 0.4956 0.081 Uiso 0.50 1 calc PR A 2 C30 C 0.5655(11) 0.7228(11) 0.4921(4) 0.0800(17) Uani 0.50 1 d PD A 1 H30A H 0.5775 0.6208 0.4802 0.120 Uiso 0.50 1 calc PR A 1 H30B H 0.5054 0.7679 0.4581 0.120 Uiso 0.50 1 calc PR A 1 H30C H 0.5057 0.7258 0.5323 0.120 Uiso 0.50 1 calc PR A 1 C30' C 0.5556(10) 0.8553(10) 0.5091(4) 0.0800(17) Uani 0.50 1 d PD A 2 H30D H 0.4965 0.8386 0.5492 0.120 Uiso 0.50 1 calc PR A 2 H30E H 0.4779 0.8479 0.4728 0.120 Uiso 0.50 1 calc PR A 2 H30F H 0.6152 0.9530 0.5104 0.120 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0367(5) 0.0371(5) 0.0443(5) -0.0041(4) 0.0021(4) 0.0037(4) Al2 0.0642(7) 0.0627(7) 0.0519(6) 0.0111(5) 0.0192(5) 0.0191(5) O1 0.0516(12) 0.0420(11) 0.0471(11) -0.0072(9) -0.0044(9) 0.0030(9) O2 0.0563(13) 0.0532(13) 0.0495(12) 0.0005(10) 0.0139(10) 0.0051(11) N1 0.0343(11) 0.0379(12) 0.0339(12) -0.0029(9) 0.0027(9) 0.0030(10) N2 0.0461(14) 0.0606(16) 0.0395(13) 0.0050(12) 0.0088(11) 0.0068(12) C1 0.0423(15) 0.0522(17) 0.0306(14) -0.0063(12) -0.0001(12) 0.0021(14) C2 0.0443(16) 0.062(2) 0.0336(15) -0.0039(13) -0.0003(12) -0.0026(15) C3 0.0426(16) 0.078(2) 0.0362(16) -0.0035(15) -0.0031(13) 0.0056(16) C4 0.0561(19) 0.070(2) 0.0319(15) -0.0004(14) -0.0016(13) 0.0203(17) C5 0.0545(18) 0.0542(18) 0.0366(15) -0.0019(13) -0.0036(13) 0.0089(15) C6 0.0404(15) 0.0494(17) 0.0310(14) -0.0014(12) -0.0003(11) 0.0020(13) C7 0.0438(16) 0.0416(15) 0.0358(14) 0.0005(12) 0.0009(12) -0.0004(13) C8 0.0311(13) 0.0405(15) 0.0423(15) -0.0023(12) 0.0044(11) -0.0018(11) C9 0.0332(14) 0.0376(15) 0.0424(15) -0.0041(12) 0.0027(12) 0.0020(12) C10 0.0529(19) 0.074(2) 0.056(2) -0.0088(17) -0.0049(16) -0.0149(17) C11 0.079(3) 0.089(3) 0.062(2) -0.005(2) -0.016(2) 0.038(2) C12 0.0554(18) 0.0382(16) 0.0546(18) -0.0004(14) 0.0062(15) -0.0053(14) C13 0.0472(18) 0.069(2) 0.064(2) 0.0003(17) 0.0161(16) -0.0024(16) C14 0.0513(18) 0.0491(19) 0.077(2) -0.0165(17) -0.0003(17) 0.0127(15) C15 0.082(3) 0.050(2) 0.080(3) -0.0151(18) -0.009(2) 0.0227(19) C16 0.0499(17) 0.0597(19) 0.0292(14) -0.0009(13) 0.0050(12) 0.0067(15) C17 0.0479(17) 0.066(2) 0.0351(15) -0.0012(14) 0.0072(13) 0.0053(15) C18 0.0492(18) 0.083(3) 0.0375(16) -0.0002(16) 0.0098(14) 0.0014(18) C19 0.071(2) 0.063(2) 0.0399(17) 0.0008(15) 0.0096(16) -0.0033(18) C20 0.066(2) 0.063(2) 0.0384(16) 0.0042(15) 0.0094(15) 0.0089(17) C21 0.0524(18) 0.062(2) 0.0321(14) 0.0031(13) 0.0063(13) 0.0112(16) C22 0.0521(18) 0.067(2) 0.0394(16) 0.0090(15) 0.0080(14) 0.0136(16) C23 0.0421(16) 0.067(2) 0.0438(16) -0.0026(15) 0.0068(13) 0.0044(15) C24 0.0439(16) 0.062(2) 0.0469(17) 0.0004(15) 0.0097(14) 0.0069(15) C25 0.057(2) 0.084(3) 0.055(2) -0.0054(18) 0.0130(16) 0.0166(19) C26 0.092(3) 0.073(3) 0.075(3) 0.005(2) 0.020(2) -0.015(2) C27 0.087(3) 0.058(2) 0.138(4) 0.003(3) 0.052(3) 0.007(2) C28 0.101(3) 0.070(3) 0.125(4) -0.010(3) 0.028(3) 0.010(3) C29 0.083(6) 0.061(6) 0.065(3) 0.031(5) 0.026(4) 0.024(5) C29' 0.083(6) 0.061(6) 0.065(3) 0.031(5) 0.026(4) 0.024(5) C30 0.079(4) 0.098(5) 0.067(4) -0.006(3) -0.007(3) 0.031(4) C30' 0.079(4) 0.098(5) 0.067(4) -0.006(3) -0.007(3) 0.031(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 Al1 O1 1.760(2) . ? Al1 C14 1.961(3) . ? Al1 C12 1.964(3) . ? Al1 N1 2.092(2) . ? Al2 O2 1.754(2) . ? Al2 C29 1.910(10) . ? Al2 C27 1.961(5) . ? Al2 C29' 1.995(11) . ? Al2 N2 2.074(3) . ? O1 C1 1.353(4) . ? O2 C16 1.353(4) . ? N1 C9 1.493(3) 2_667 ? N1 C8 1.497(3) . ? N1 C7 1.518(3) . ? N2 C24 1.493(4) 2_766 ? N2 C23 1.497(4) . ? N2 C22 1.509(4) . ? C1 C6 1.391(4) . ? C1 C2 1.406(4) . ? C2 C3 1.380(5) . ? C2 C10 1.504(5) . ? C3 C4 1.389(5) . ? C3 H3 0.9400 . ? C4 C5 1.395(4) . ? C4 C11 1.516(5) . ? C5 C6 1.390(4) . ? C5 H5 0.9400 . ? C6 C7 1.503(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C9 1.505(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 N1 1.493(3) 2_667 ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C12 C13 1.534(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 C15 1.519(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 C21 1.390(4) . ? C16 C17 1.406(4) . ? C17 C18 1.374(5) . ? C17 C25 1.503(5) . ? C18 C19 1.393(5) . ? C18 H18 0.9400 . ? C19 C20 1.390(5) . ? C19 C26 1.520(5) . ? C20 C21 1.380(5) . ? C20 H20 0.9400 . ? C21 C22 1.510(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 C24 1.510(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N2 1.493(4) 2_766 ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 C28 1.525(6) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 C30 1.483(11) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29' C30' 1.544(11) . ? C29' H29C 0.9800 . ? C29' H29D 0.9800 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C30' H30D 0.9700 . ? C30' H30E 0.9700 . ? C30' H30F 0.9700 . ? 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 Al1 C14 108.29(13) . . ? O1 Al1 C12 109.64(13) . . ? C14 Al1 C12 118.11(16) . . ? O1 Al1 N1 97.73(10) . . ? C14 Al1 N1 107.95(13) . . ? C12 Al1 N1 113.12(11) . . ? O2 Al2 C29 115.8(3) . . ? O2 Al2 C27 108.29(17) . . ? C29 Al2 C27 106.6(3) . . ? O2 Al2 C29' 105.1(3) . . ? C29 Al2 C29' 20.8(3) . . ? C27 Al2 C29' 127.4(3) . . ? O2 Al2 N2 98.42(11) . . ? C29 Al2 N2 119.4(3) . . ? C27 Al2 N2 107.66(15) . . ? C29' Al2 N2 106.3(3) . . ? C1 O1 Al1 121.02(17) . . ? C16 O2 Al2 124.03(18) . . ? C9 N1 C8 106.7(2) 2_667 . ? C9 N1 C7 108.0(2) 2_667 . ? C8 N1 C7 107.4(2) . . ? C9 N1 Al1 116.24(17) 2_667 . ? C8 N1 Al1 112.88(16) . . ? C7 N1 Al1 105.17(16) . . ? C24 N2 C23 107.0(2) 2_766 . ? C24 N2 C22 108.2(2) 2_766 . ? C23 N2 C22 107.1(2) . . ? C24 N2 Al2 116.60(19) 2_766 . ? C23 N2 Al2 113.0(2) . . ? C22 N2 Al2 104.49(18) . . ? O1 C1 C6 119.3(3) . . ? O1 C1 C2 119.9(3) . . ? C6 C1 C2 120.7(3) . . ? C3 C2 C1 117.4(3) . . ? C3 C2 C10 123.5(3) . . ? C1 C2 C10 119.1(3) . . ? C2 C3 C4 123.6(3) . . ? C2 C3 H3 118.2 . . ? C4 C3 H3 118.2 . . ? C3 C4 C5 117.5(3) . . ? C3 C4 C11 122.2(3) . . ? C5 C4 C11 120.3(3) . . ? C6 C5 C4 121.0(3) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C1 119.7(3) . . ? C5 C6 C7 122.3(3) . . ? C1 C6 C7 118.0(3) . . ? C6 C7 N1 112.2(2) . . ? C6 C7 H7A 109.2 . . ? N1 C7 H7A 109.2 . . ? C6 C7 H7B 109.2 . . ? N1 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? N1 C8 C9 112.1(2) . . ? N1 C8 H8A 109.2 . . ? C9 C8 H8A 109.2 . . ? N1 C8 H8B 109.2 . . ? C9 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? N1 C9 C8 112.1(2) 2_667 . ? N1 C9 H9A 109.2 2_667 . ? C8 C9 H9A 109.2 . . ? N1 C9 H9B 109.2 2_667 . ? C8 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C2 C10 H10A 109.5 . . ? C2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C4 C11 H11A 109.5 . . ? C4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 Al1 119.5(2) . . ? C13 C12 H12A 107.4 . . ? Al1 C12 H12A 107.4 . . ? C13 C12 H12B 107.4 . . ? Al1 C12 H12B 107.4 . . ? H12A C12 H12B 107.0 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 Al1 111.5(2) . . ? C15 C14 H14A 109.3 . . ? Al1 C14 H14A 109.3 . . ? C15 C14 H14B 109.3 . . ? Al1 C14 H14B 109.3 . . ? H14A C14 H14B 108.0 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O2 C16 C21 119.9(3) . . ? O2 C16 C17 120.3(3) . . ? C21 C16 C17 119.8(3) . . ? C18 C17 C16 118.3(3) . . ? C18 C17 C25 122.7(3) . . ? C16 C17 C25 119.0(3) . . ? C17 C18 C19 123.0(3) . . ? C17 C18 H18 118.5 . . ? C19 C18 H18 118.5 . . ? C20 C19 C18 117.5(3) . . ? C20 C19 C26 120.4(3) . . ? C18 C19 C26 122.2(3) . . ? C21 C20 C19 121.2(3) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C20 C21 C16 120.3(3) . . ? C20 C21 C22 122.0(3) . . ? C16 C21 C22 117.5(3) . . ? N2 C22 C21 113.2(2) . . ? N2 C22 H22A 108.9 . . ? C21 C22 H22A 108.9 . . ? N2 C22 H22B 108.9 . . ? C21 C22 H22B 108.9 . . ? H22A C22 H22B 107.8 . . ? N2 C23 C24 111.9(3) . . ? N2 C23 H23A 109.2 . . ? C24 C23 H23A 109.2 . . ? N2 C23 H23B 109.2 . . ? C24 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? N2 C24 C23 112.3(3) 2_766 . ? N2 C24 H24A 109.1 2_766 . ? C23 C24 H24A 109.1 . . ? N2 C24 H24B 109.1 2_766 . ? C23 C24 H24B 109.1 . . ? H24A C24 H24B 107.9 . . ? C17 C25 H25A 109.5 . . ? C17 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C17 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C19 C26 H26A 109.5 . . ? C19 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C19 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 Al2 110.1(3) . . ? C28 C27 H27A 109.6 . . ? Al2 C27 H27A 109.6 . . ? C28 C27 H27B 109.6 . . ? Al2 C27 H27B 109.6 . . ? H27A C27 H27B 108.2 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 Al2 109.4(6) . . ? C30 C29 H29A 109.8 . . ? Al2 C29 H29A 109.8 . . ? C30 C29 H29B 109.8 . . ? Al2 C29 H29B 109.8 . . ? H29A C29 H29B 108.2 . . ? C30' C29' Al2 115.4(7) . . ? C30' C29' H29C 108.4 . . ? Al2 C29' H29C 108.4 . . ? C30' C29' H29D 108.4 . . ? Al2 C29' H29D 108.4 . . ? H29C C29' H29D 107.5 . . ? C29' C30' H30D 109.5 . . ? C29' C30' H30E 109.5 . . ? H30D C30' H30E 109.5 . . ? C29' C30' H30F 109.5 . . ? H30D C30' H30F 109.5 . . ? H30E C30' H30F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.326 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.082 #============================================================================== data_complex3 _database_code_depnum_ccdc_archive 'CCDC 836240' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H20 Al N O' _chemical_formula_sum 'C13 H20 Al N O' _chemical_formula_weight 233.28 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 7.5977(10) _cell_length_b 21.372(3) _cell_length_c 8.0416(11) _cell_angle_alpha 90.00 _cell_angle_beta 91.022(4) _cell_angle_gamma 90.00 _cell_volume 1305.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5507 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.80 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.187 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504 _exptl_absorpt_coefficient_mu 0.136 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.727 _exptl_absorpt_correction_T_max 0.978 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7358 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2965 _reflns_number_gt 2261 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0793P)^2^+0.0802P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2965 _refine_ls_number_parameters 150 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0683 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1401 _refine_ls_wR_factor_gt 0.1286 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.24604(7) 0.54177(2) 0.73933(6) 0.03304(19) Uani 1 1 d . . . O1 O 0.18378(16) 0.57476(5) 0.54533(14) 0.0352(3) Uani 1 1 d . . . N1 N -0.00630(18) 0.52972(6) 0.83255(16) 0.0280(3) Uani 1 1 d . . . C1 C 0.0743(2) 0.62494(8) 0.5541(2) 0.0318(4) Uani 1 1 d . . . C2 C 0.1185(3) 0.68215(9) 0.4812(2) 0.0375(4) Uani 1 1 d . . . C3 C 0.0018(3) 0.73180(8) 0.5004(2) 0.0413(5) Uani 1 1 d . . . H3 H 0.0307 0.7706 0.4529 0.050 Uiso 1 1 calc R . . C4 C -0.1545(3) 0.72719(9) 0.5858(2) 0.0398(4) Uani 1 1 d . . . C5 C -0.1971(2) 0.66893(8) 0.6524(2) 0.0362(4) Uani 1 1 d . . . H5 H -0.3036 0.6640 0.7085 0.043 Uiso 1 1 calc R . . C6 C -0.0839(2) 0.61797(8) 0.6369(2) 0.0306(4) Uani 1 1 d . . . C7 C -0.1312(2) 0.55378(8) 0.6987(2) 0.0321(4) Uani 1 1 d . . . H7A H -0.1315 0.5245 0.6048 0.039 Uiso 1 1 calc R . . H7B H -0.2506 0.5549 0.7427 0.039 Uiso 1 1 calc R . . C8 C -0.0405(2) 0.56451(7) 0.9890(2) 0.0300(4) Uani 1 1 d . . . H8A H -0.1672 0.5640 1.0100 0.036 Uiso 1 1 calc R . . H8B H -0.0047 0.6082 0.9752 0.036 Uiso 1 1 calc R . . C9 C 0.0565(2) 0.53706(7) 1.1371(2) 0.0310(4) Uani 1 1 d . . . H9A H 0.1835 0.5395 1.1186 0.037 Uiso 1 1 calc R . . H9B H 0.0307 0.5619 1.2361 0.037 Uiso 1 1 calc R . . C10 C 0.2876(3) 0.68884(10) 0.3886(3) 0.0545(6) Uani 1 1 d . . . H10A H 0.3866 0.6836 0.4652 0.082 Uiso 1 1 calc R . . H10B H 0.2927 0.7300 0.3383 0.082 Uiso 1 1 calc R . . H10C H 0.2928 0.6572 0.3024 0.082 Uiso 1 1 calc R . . C11 C -0.2743(3) 0.78258(10) 0.6095(3) 0.0565(6) Uani 1 1 d . . . H11A H -0.2197 0.8117 0.6872 0.085 Uiso 1 1 calc R . . H11B H -0.3857 0.7684 0.6530 0.085 Uiso 1 1 calc R . . H11C H -0.2945 0.8033 0.5034 0.085 Uiso 1 1 calc R . . C12 C 0.3633(3) 0.60591(11) 0.8758(3) 0.0506(5) Uani 1 1 d . . . H12A H 0.4217 0.6356 0.8041 0.076 Uiso 1 1 calc R . . H12B H 0.4496 0.5863 0.9492 0.076 Uiso 1 1 calc R . . H12C H 0.2767 0.6276 0.9416 0.076 Uiso 1 1 calc R . . C13 C 0.3605(3) 0.46083(10) 0.7056(3) 0.0476(5) Uani 1 1 d . . . H13A H 0.2739 0.4306 0.6665 0.071 Uiso 1 1 calc R . . H13B H 0.4124 0.4465 0.8099 0.071 Uiso 1 1 calc R . . H13C H 0.4518 0.4652 0.6236 0.071 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0337(3) 0.0354(3) 0.0302(3) 0.0042(2) 0.0039(2) 0.0009(2) O1 0.0427(7) 0.0333(6) 0.0297(6) 0.0036(5) 0.0073(5) 0.0050(6) N1 0.0336(8) 0.0249(7) 0.0256(7) 0.0023(5) 0.0019(6) -0.0012(6) C1 0.0392(10) 0.0328(9) 0.0235(8) 0.0014(7) 0.0011(7) 0.0014(7) C2 0.0421(10) 0.0359(9) 0.0346(9) 0.0062(8) 0.0044(8) -0.0035(8) C3 0.0503(11) 0.0291(9) 0.0448(10) 0.0092(8) 0.0043(9) -0.0035(8) C4 0.0464(11) 0.0343(9) 0.0387(10) 0.0052(8) -0.0009(9) 0.0048(8) C5 0.0362(10) 0.0387(9) 0.0339(9) 0.0054(7) 0.0019(8) 0.0008(8) C6 0.0354(9) 0.0312(8) 0.0252(8) 0.0040(7) -0.0015(7) -0.0015(7) C7 0.0340(9) 0.0333(9) 0.0290(8) 0.0045(7) -0.0011(7) -0.0037(7) C8 0.0373(9) 0.0240(8) 0.0288(8) 0.0002(7) 0.0055(7) -0.0004(7) C9 0.0400(10) 0.0250(8) 0.0282(8) 0.0009(6) 0.0030(7) -0.0041(7) C10 0.0538(13) 0.0485(11) 0.0619(14) 0.0154(11) 0.0209(11) -0.0026(10) C11 0.0603(14) 0.0414(11) 0.0681(14) 0.0122(11) 0.0099(12) 0.0129(10) C12 0.0432(12) 0.0642(14) 0.0446(11) 0.0011(10) 0.0022(9) -0.0172(10) C13 0.0497(12) 0.0472(12) 0.0461(11) 0.0111(9) 0.0106(10) 0.0131(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 Al1 O1 1.7687(13) . ? Al1 C13 1.957(2) . ? Al1 C12 1.960(2) . ? Al1 N1 2.0868(15) . ? O1 C1 1.360(2) . ? N1 C8 1.488(2) . ? N1 C9 1.499(2) 3_567 ? N1 C7 1.512(2) . ? C1 C6 1.393(3) . ? C1 C2 1.399(2) . ? C2 C3 1.393(3) . ? C2 C10 1.504(3) . ? C3 C4 1.386(3) . ? C3 H3 0.9400 . ? C4 C5 1.396(3) . ? C4 C11 1.508(3) . ? C5 C6 1.395(2) . ? C5 H5 0.9400 . ? C6 C7 1.504(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C9 1.508(2) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 N1 1.499(2) 3_567 ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? 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 Al1 C13 110.03(8) . . ? O1 Al1 C12 109.07(8) . . ? C13 Al1 C12 119.81(10) . . ? O1 Al1 N1 97.65(6) . . ? C13 Al1 N1 110.73(8) . . ? C12 Al1 N1 107.25(8) . . ? C1 O1 Al1 115.03(10) . . ? C8 N1 C9 106.80(12) . 3_567 ? C8 N1 C7 108.36(13) . . ? C9 N1 C7 106.35(12) 3_567 . ? C8 N1 Al1 114.69(10) . . ? C9 N1 Al1 114.47(11) 3_567 . ? C7 N1 Al1 105.73(10) . . ? O1 C1 C6 118.32(15) . . ? O1 C1 C2 121.04(16) . . ? C6 C1 C2 120.63(16) . . ? C3 C2 C1 117.46(17) . . ? C3 C2 C10 122.25(17) . . ? C1 C2 C10 120.28(17) . . ? C4 C3 C2 123.60(17) . . ? C4 C3 H3 118.2 . . ? C2 C3 H3 118.2 . . ? C3 C4 C5 117.39(17) . . ? C3 C4 C11 122.11(18) . . ? C5 C4 C11 120.49(19) . . ? C6 C5 C4 121.01(18) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C1 119.85(16) . . ? C5 C6 C7 122.11(16) . . ? C1 C6 C7 117.94(15) . . ? C6 C7 N1 113.23(13) . . ? C6 C7 H7A 108.9 . . ? N1 C7 H7A 108.9 . . ? C6 C7 H7B 108.9 . . ? N1 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? N1 C8 C9 112.51(13) . . ? N1 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? N1 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? N1 C9 C8 112.13(13) 3_567 . ? N1 C9 H9A 109.2 3_567 . ? C8 C9 H9A 109.2 . . ? N1 C9 H9B 109.2 3_567 . ? C8 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C2 C10 H10A 109.5 . . ? C2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C4 C11 H11A 109.5 . . ? C4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Al1 C12 H12A 109.5 . . ? Al1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Al1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Al1 C13 H13A 109.5 . . ? Al1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Al1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.251 _refine_diff_density_min -0.211 _refine_diff_density_rms 0.047 #===================================================End OF CIF