data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Redshaw, Carl' _publ_contact_author_email carl.redshaw@uea.ac.uk _publ_section_title ; Synthesis and Characterisation of Alkylaluminium Benzimidazolates and their use in the Ring-Opening Polymerisation of \^I\m-Caprolactone ; loop_ _publ_author_name C.Redshaw W.H.Sun M.Shen W.Huang X.Hao # Attachment '- CIF.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 777730' #TrackingRef '- CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C15H16AlN3 _chemical_formula_sum 'C15 H16 Al N3' _chemical_formula_weight 265.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.530(3) _cell_length_b 13.566(3) _cell_length_c 16.714(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2841.1(10) _cell_formula_units_Z 8 _cell_measurement_temperature 446(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 27.45 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.132 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.9740 _exptl_absorpt_correction_T_max 0.9804 _exptl_special_details ; ? ; _diffrn_ambient_temperature 446(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_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 21861 _diffrn_reflns_av_R_equivalents 0.0691 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 27.45 _reflns_number_total 3240 _reflns_number_gt 3075 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+3.8930P] 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 3240 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0951 _refine_ls_R_factor_gt 0.0890 _refine_ls_wR_factor_ref 0.1909 _refine_ls_wR_factor_gt 0.1877 _refine_ls_goodness_of_fit_ref 1.283 _refine_ls_restrained_S_all 1.283 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.68316(8) 0.18269(7) 0.58606(5) 0.0296(3) Uani 1 1 d . . . N1 N 0.77975(19) 0.12921(17) 0.67122(14) 0.0265(5) Uani 1 1 d . . . N2 N 0.59841(19) 0.22411(18) 0.67392(14) 0.0281(6) Uani 1 1 d . . . N3 N 0.5902(2) 0.23564(18) 0.81102(15) 0.0296(6) Uani 1 1 d . . . C5 C 0.7401(2) 0.1442(2) 0.74645(17) 0.0255(6) Uani 1 1 d . . . C6 C 0.6411(2) 0.2017(2) 0.74710(17) 0.0261(6) Uani 1 1 d . . . C12 C 0.5047(2) 0.2863(2) 0.77686(18) 0.0298(6) Uani 1 1 d . . . C7 C 0.5092(2) 0.2796(2) 0.69249(18) 0.0283(6) Uani 1 1 d . . . C4 C 0.7900(2) 0.1076(2) 0.81367(18) 0.0301(7) Uani 1 1 d . . . H4A H 0.7615 0.1185 0.8643 0.036 Uiso 1 1 calc R . . C8 C 0.4313(3) 0.3222(2) 0.6437(2) 0.0347(7) Uani 1 1 d . . . H8A H 0.4348 0.3174 0.5883 0.042 Uiso 1 1 calc R . . C3 C 0.8833(2) 0.0542(2) 0.80429(18) 0.0317(7) Uani 1 1 d . . . H3B H 0.9183 0.0284 0.8487 0.038 Uiso 1 1 calc R . . C1 C 0.8720(2) 0.0781(2) 0.66224(18) 0.0289(6) Uani 1 1 d . . . C2 C 0.9242(2) 0.0398(2) 0.72824(18) 0.0314(7) Uani 1 1 d . . . H2A H 0.9869 0.0041 0.7215 0.038 Uiso 1 1 calc R . . C10 C 0.3445(3) 0.3795(2) 0.7646(2) 0.0401(8) Uani 1 1 d . . . H10A H 0.2880 0.4134 0.7880 0.048 Uiso 1 1 calc R . . C11 C 0.4216(3) 0.3383(2) 0.8134(2) 0.0349(7) Uani 1 1 d . . . H11A H 0.4184 0.3450 0.8688 0.042 Uiso 1 1 calc R . . C13 C 0.9169(3) 0.0683(3) 0.57979(19) 0.0425(8) Uani 1 1 d . . . H13A H 0.8698 0.0995 0.5422 0.064 Uiso 1 1 calc R . . H13B H 0.9240 -0.0002 0.5666 0.064 Uiso 1 1 calc R . . H13C H 0.9857 0.0994 0.5776 0.064 Uiso 1 1 calc R . . C32 C 0.7357(3) 0.2953(3) 0.5248(2) 0.0431(8) Uani 1 1 d . . . H32A H 0.6831 0.3143 0.4859 0.065 Uiso 1 1 calc R . . H32B H 0.8006 0.2775 0.4980 0.065 Uiso 1 1 calc R . . H32C H 0.7491 0.3495 0.5603 0.065 Uiso 1 1 calc R . . C9 C 0.3488(3) 0.3715(2) 0.6810(2) 0.0398(8) Uani 1 1 d . . . H9A H 0.2952 0.4000 0.6502 0.048 Uiso 1 1 calc R . . C31 C 0.6255(3) 0.0723(3) 0.5254(2) 0.0478(9) Uani 1 1 d . . . H31A H 0.5790 0.0966 0.4843 0.072 Uiso 1 1 calc R . . H31B H 0.5861 0.0298 0.5606 0.072 Uiso 1 1 calc R . . H31C H 0.6830 0.0360 0.5014 0.072 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 0.0335(5) 0.0319(5) 0.0232(4) -0.0008(4) -0.0013(4) -0.0005(4) N1 0.0281(13) 0.0262(12) 0.0253(12) -0.0006(9) 0.0005(10) -0.0002(10) N2 0.0286(13) 0.0299(13) 0.0259(12) 0.0016(10) -0.0028(10) 0.0014(10) N3 0.0299(13) 0.0302(13) 0.0285(13) 0.0001(10) 0.0016(10) 0.0018(11) C5 0.0258(14) 0.0257(13) 0.0251(13) -0.0023(11) 0.0006(11) -0.0035(11) C6 0.0259(14) 0.0289(14) 0.0235(13) -0.0001(11) -0.0004(11) -0.0019(12) C12 0.0280(15) 0.0274(14) 0.0340(16) -0.0007(12) 0.0013(13) -0.0020(12) C7 0.0268(14) 0.0262(14) 0.0319(15) 0.0011(12) -0.0016(12) -0.0036(12) C4 0.0322(16) 0.0327(15) 0.0254(14) -0.0007(12) 0.0002(12) -0.0013(13) C8 0.0334(17) 0.0322(16) 0.0385(17) 0.0026(13) -0.0072(14) -0.0019(13) C3 0.0309(15) 0.0323(15) 0.0321(16) 0.0026(13) -0.0056(13) 0.0013(13) C1 0.0308(15) 0.0264(14) 0.0296(15) 0.0008(12) 0.0033(12) -0.0017(12) C2 0.0289(15) 0.0291(15) 0.0362(16) -0.0010(12) 0.0010(13) 0.0034(13) C10 0.0292(16) 0.0318(16) 0.059(2) -0.0007(15) 0.0075(15) 0.0010(13) C11 0.0325(17) 0.0331(16) 0.0392(17) -0.0004(13) 0.0054(14) -0.0006(13) C13 0.045(2) 0.049(2) 0.0335(17) -0.0027(15) 0.0103(15) 0.0098(16) C32 0.046(2) 0.051(2) 0.0323(17) 0.0126(15) -0.0022(15) -0.0039(16) C9 0.0315(17) 0.0326(16) 0.055(2) 0.0027(15) -0.0053(15) 0.0036(14) C31 0.052(2) 0.048(2) 0.044(2) -0.0135(17) -0.0048(17) -0.0029(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 N2 1.897(3) . ? Al1 C31 1.948(3) . ? Al1 C32 1.953(3) . ? Al1 N1 2.004(3) . ? N1 C1 1.357(4) . ? N1 C5 1.367(4) . ? N2 C6 1.369(4) . ? N2 C7 1.383(4) . ? N3 C6 1.327(4) . ? N3 C12 1.395(4) . ? C5 C4 1.378(4) . ? C5 C6 1.466(4) . ? C12 C11 1.398(4) . ? C12 C7 1.414(4) . ? C7 C8 1.397(4) . ? C4 C3 1.385(4) . ? C4 H4A 0.9300 . ? C8 C9 1.381(5) . ? C8 H8A 0.9300 . ? C3 C2 1.384(4) . ? C3 H3B 0.9300 . ? C1 C2 1.383(4) . ? C1 C13 1.494(4) . ? C2 H2A 0.9300 . ? C10 C11 1.383(5) . ? C10 C9 1.402(5) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C9 H9A 0.9300 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Al1 C31 115.02(15) . . ? N2 Al1 C32 111.27(14) . . ? C31 Al1 C32 116.97(17) . . ? N2 Al1 N1 84.00(11) . . ? C31 Al1 N1 108.37(14) . . ? C32 Al1 N1 116.87(13) . . ? C1 N1 C5 119.2(2) . . ? C1 N1 Al1 128.4(2) . . ? C5 N1 Al1 112.34(19) . . ? C6 N2 C7 103.7(2) . . ? C6 N2 Al1 114.02(19) . . ? C7 N2 Al1 141.9(2) . . ? C6 N3 C12 102.2(2) . . ? N1 C5 C4 122.1(3) . . ? N1 C5 C6 113.2(2) . . ? C4 C5 C6 124.7(3) . . ? N3 C6 N2 117.0(3) . . ? N3 C6 C5 126.7(3) . . ? N2 C6 C5 116.2(2) . . ? N3 C12 C11 129.9(3) . . ? N3 C12 C7 110.2(3) . . ? C11 C12 C7 119.9(3) . . ? N2 C7 C8 131.2(3) . . ? N2 C7 C12 106.9(3) . . ? C8 C7 C12 121.8(3) . . ? C5 C4 C3 118.6(3) . . ? C5 C4 H4A 120.7 . . ? C3 C4 H4A 120.7 . . ? C9 C8 C7 117.4(3) . . ? C9 C8 H8A 121.3 . . ? C7 C8 H8A 121.3 . . ? C2 C3 C4 119.4(3) . . ? C2 C3 H3B 120.3 . . ? C4 C3 H3B 120.3 . . ? N1 C1 C2 120.4(3) . . ? N1 C1 C13 117.9(3) . . ? C2 C1 C13 121.6(3) . . ? C1 C2 C3 120.3(3) . . ? C1 C2 H2A 119.8 . . ? C3 C2 H2A 119.8 . . ? C11 C10 C9 122.0(3) . . ? C11 C10 H10A 119.0 . . ? C9 C10 H10A 119.0 . . ? C10 C11 C12 117.8(3) . . ? C10 C11 H11A 121.1 . . ? C12 C11 H11A 121.1 . . ? C1 C13 H13A 109.5 . . ? C1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Al1 C32 H32A 109.5 . . ? Al1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Al1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C8 C9 C10 121.0(3) . . ? C8 C9 H9A 119.5 . . ? C10 C9 H9A 119.5 . . ? Al1 C31 H31A 109.5 . . ? Al1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Al1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Al1 N1 C1 178.0(3) . . . . ? C31 Al1 N1 C1 63.6(3) . . . . ? C32 Al1 N1 C1 -71.1(3) . . . . ? N2 Al1 N1 C5 1.7(2) . . . . ? C31 Al1 N1 C5 -112.7(2) . . . . ? C32 Al1 N1 C5 112.6(2) . . . . ? C31 Al1 N2 C6 108.8(2) . . . . ? C32 Al1 N2 C6 -115.2(2) . . . . ? N1 Al1 N2 C6 1.3(2) . . . . ? C31 Al1 N2 C7 -80.0(4) . . . . ? C32 Al1 N2 C7 56.0(4) . . . . ? N1 Al1 N2 C7 172.5(3) . . . . ? C1 N1 C5 C4 -1.1(4) . . . . ? Al1 N1 C5 C4 175.6(2) . . . . ? C1 N1 C5 C6 179.1(2) . . . . ? Al1 N1 C5 C6 -4.2(3) . . . . ? C12 N3 C6 N2 -0.2(3) . . . . ? C12 N3 C6 C5 178.3(3) . . . . ? C7 N2 C6 N3 0.2(3) . . . . ? Al1 N2 C6 N3 174.7(2) . . . . ? C7 N2 C6 C5 -178.4(2) . . . . ? Al1 N2 C6 C5 -4.0(3) . . . . ? N1 C5 C6 N3 -173.1(3) . . . . ? C4 C5 C6 N3 7.2(5) . . . . ? N1 C5 C6 N2 5.5(4) . . . . ? C4 C5 C6 N2 -174.3(3) . . . . ? C6 N3 C12 C11 179.7(3) . . . . ? C6 N3 C12 C7 0.1(3) . . . . ? C6 N2 C7 C8 -178.3(3) . . . . ? Al1 N2 C7 C8 9.9(6) . . . . ? C6 N2 C7 C12 -0.1(3) . . . . ? Al1 N2 C7 C12 -171.9(3) . . . . ? N3 C12 C7 N2 0.0(3) . . . . ? C11 C12 C7 N2 -179.7(3) . . . . ? N3 C12 C7 C8 178.4(3) . . . . ? C11 C12 C7 C8 -1.3(5) . . . . ? N1 C5 C4 C3 0.2(4) . . . . ? C6 C5 C4 C3 179.9(3) . . . . ? N2 C7 C8 C9 178.0(3) . . . . ? C12 C7 C8 C9 0.0(4) . . . . ? C5 C4 C3 C2 0.4(4) . . . . ? C5 N1 C1 C2 1.4(4) . . . . ? Al1 N1 C1 C2 -174.7(2) . . . . ? C5 N1 C1 C13 -176.3(3) . . . . ? Al1 N1 C1 C13 7.6(4) . . . . ? N1 C1 C2 C3 -0.8(4) . . . . ? C13 C1 C2 C3 176.8(3) . . . . ? C4 C3 C2 C1 -0.1(5) . . . . ? C9 C10 C11 C12 -1.0(5) . . . . ? N3 C12 C11 C10 -177.9(3) . . . . ? C7 C12 C11 C10 1.7(4) . . . . ? C7 C8 C9 C10 0.7(5) . . . . ? C11 C10 C9 C8 -0.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.312 _refine_diff_density_min -0.351 _refine_diff_density_rms 0.060 #==End data_2 _database_code_depnum_ccdc_archive 'CCDC 777731' #TrackingRef '- CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H20 Al N3' _chemical_formula_weight 293.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 7.2014(14) _cell_length_b 16.582(3) _cell_length_c 13.370(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.72(3) _cell_angle_gamma 90.00 _cell_volume 1593.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.96 _cell_measurement_theta_max 27.54 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.223 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 0.124 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.9519 _exptl_absorpt_correction_T_max 0.9731 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 12754 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 27.54 _reflns_number_total 3650 _reflns_number_gt 3462 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0947P)^2^+0.9431P] 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 3650 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0784 _refine_ls_R_factor_gt 0.0743 _refine_ls_wR_factor_ref 0.1988 _refine_ls_wR_factor_gt 0.1954 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 1.165 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.04739(10) 0.46300(4) 0.75346(5) 0.0368(2) Uani 1 1 d . . . N2 N -0.0655(3) 0.40382(12) 0.85475(14) 0.0345(4) Uani 1 1 d . . . N1 N -0.0817(3) 0.55636(12) 0.81163(15) 0.0365(4) Uani 1 1 d . . . C5 C -0.1827(3) 0.53572(14) 0.89045(18) 0.0358(5) Uani 1 1 d . . . N3 N -0.2492(3) 0.41147(13) 0.98716(14) 0.0383(5) Uani 1 1 d . . . C32 C 0.3187(3) 0.46802(16) 0.7741(2) 0.0449(6) Uani 1 1 d . . . H32A H 0.3702 0.4963 0.7168 0.054 Uiso 1 1 calc R . . H32B H 0.3530 0.4993 0.8356 0.054 Uiso 1 1 calc R . . C6 C -0.1695(3) 0.44974(14) 0.91449(16) 0.0342(5) Uani 1 1 d . . . C12 C -0.1929(3) 0.33267(15) 0.97492(16) 0.0359(5) Uani 1 1 d . . . C7 C -0.0791(3) 0.32725(14) 0.89268(17) 0.0358(5) Uani 1 1 d . . . C11 C -0.2299(4) 0.26322(17) 1.02959(19) 0.0442(6) Uani 1 1 d . . . H11A H -0.3054 0.2657 1.0852 0.053 Uiso 1 1 calc R . . C8 C -0.0041(3) 0.25444(15) 0.86409(19) 0.0423(6) Uani 1 1 d . . . H8A H 0.0714 0.2512 0.8086 0.051 Uiso 1 1 calc R . . C1 C -0.0792(3) 0.63403(16) 0.7820(2) 0.0432(6) Uani 1 1 d . . . C4 C -0.2833(3) 0.59095(16) 0.9408(2) 0.0437(6) Uani 1 1 d . . . H4A H -0.3544 0.5749 0.9947 0.052 Uiso 1 1 calc R . . C31 C -0.0586(4) 0.43595(18) 0.61778(19) 0.0491(6) Uani 1 1 d . . . H31A H 0.0221 0.4602 0.5687 0.059 Uiso 1 1 calc R . . H31B H -0.0519 0.3767 0.6096 0.059 Uiso 1 1 calc R . . C9 C -0.0431(4) 0.18673(16) 0.9192(2) 0.0480(6) Uani 1 1 d . . . H9A H 0.0066 0.1361 0.9011 0.058 Uiso 1 1 calc R . . C10 C -0.1541(4) 0.19111(16) 1.0008(2) 0.0480(6) Uani 1 1 d . . . H10A H -0.1779 0.1435 1.0373 0.058 Uiso 1 1 calc R . . C3 C -0.2784(4) 0.67088(17) 0.9108(2) 0.0507(7) Uani 1 1 d . . . H3B H -0.3447 0.7108 0.9448 0.061 Uiso 1 1 calc R . . C13 C 0.0359(4) 0.65335(18) 0.6956(2) 0.0564(7) Uani 1 1 d . . . H13A H 0.0929 0.6038 0.6720 0.085 Uiso 1 1 calc R . . H13B H 0.1337 0.6918 0.7174 0.085 Uiso 1 1 calc R . . H13C H -0.0436 0.6771 0.6411 0.085 Uiso 1 1 calc R . . C2 C -0.1760(4) 0.69189(16) 0.8308(2) 0.0495(6) Uani 1 1 d . . . H2A H -0.1725 0.7465 0.8094 0.059 Uiso 1 1 calc R . . C34 C 0.4041(4) 0.38331(17) 0.78380(19) 0.0451(6) Uani 1 1 d . . . H34A H 0.5396 0.3877 0.7945 0.068 Uiso 1 1 calc R . . H34B H 0.3728 0.3527 0.7223 0.068 Uiso 1 1 calc R . . H34C H 0.3543 0.3554 0.8409 0.068 Uiso 1 1 calc R . . C33 C -0.2570(4) 0.4620(2) 0.5902(2) 0.0613(8) Uani 1 1 d . . . H33A H -0.2929 0.4450 0.5214 0.092 Uiso 1 1 calc R . . H33B H -0.2661 0.5208 0.5950 0.092 Uiso 1 1 calc R . . H33C H -0.3405 0.4370 0.6363 0.092 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 0.0331(4) 0.0436(4) 0.0346(4) 0.0057(3) 0.0095(3) -0.0026(3) N2 0.0287(9) 0.0416(10) 0.0338(9) 0.0035(8) 0.0066(7) -0.0007(8) N1 0.0300(9) 0.0428(10) 0.0365(10) 0.0045(8) 0.0010(7) -0.0030(8) C5 0.0268(10) 0.0434(12) 0.0366(11) 0.0018(9) -0.0017(9) -0.0025(9) N3 0.0313(10) 0.0510(12) 0.0330(9) 0.0034(8) 0.0062(8) -0.0032(8) C32 0.0351(12) 0.0518(15) 0.0492(14) 0.0015(11) 0.0133(11) -0.0057(11) C6 0.0263(10) 0.0450(12) 0.0313(11) 0.0015(9) 0.0028(8) -0.0013(9) C12 0.0283(10) 0.0474(13) 0.0320(11) 0.0044(9) 0.0022(8) -0.0028(9) C7 0.0299(11) 0.0435(12) 0.0341(11) 0.0065(9) 0.0025(9) -0.0049(9) C11 0.0369(12) 0.0571(15) 0.0389(12) 0.0108(11) 0.0045(10) -0.0097(11) C8 0.0371(12) 0.0464(13) 0.0441(13) 0.0022(10) 0.0065(10) 0.0016(10) C1 0.0363(12) 0.0428(13) 0.0498(14) 0.0068(10) -0.0035(10) -0.0058(10) C4 0.0345(12) 0.0510(14) 0.0457(13) -0.0028(11) 0.0026(10) -0.0003(11) C31 0.0546(16) 0.0557(16) 0.0381(13) 0.0030(11) 0.0119(11) 0.0001(13) C9 0.0467(15) 0.0406(13) 0.0566(15) 0.0064(11) 0.0029(12) -0.0027(11) C10 0.0477(15) 0.0461(14) 0.0498(14) 0.0129(11) -0.0001(11) -0.0082(12) C3 0.0383(13) 0.0517(15) 0.0610(17) -0.0065(12) -0.0045(12) 0.0068(11) C13 0.0589(17) 0.0472(15) 0.0636(18) 0.0138(13) 0.0091(14) -0.0088(13) C2 0.0448(14) 0.0389(13) 0.0632(17) 0.0050(12) -0.0082(12) -0.0026(11) C34 0.0368(12) 0.0560(15) 0.0427(13) -0.0057(11) 0.0040(10) 0.0014(11) C33 0.0511(17) 0.075(2) 0.0576(18) -0.0016(15) 0.0037(14) -0.0091(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 N2 1.898(2) . ? Al1 C32 1.957(3) . ? Al1 C31 1.974(3) . ? Al1 N1 1.990(2) . ? N2 C6 1.362(3) . ? N2 C7 1.373(3) . ? N1 C1 1.348(3) . ? N1 C5 1.362(3) . ? C5 C4 1.371(3) . ? C5 C6 1.463(3) . ? N3 C6 1.323(3) . ? N3 C12 1.381(3) . ? C32 C34 1.535(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C12 C11 1.399(3) . ? C12 C7 1.416(3) . ? C7 C8 1.386(3) . ? C11 C10 1.380(4) . ? C11 H11A 0.9500 . ? C8 C9 1.382(4) . ? C8 H8A 0.9500 . ? C1 C2 1.375(4) . ? C1 C13 1.499(4) . ? C4 C3 1.386(4) . ? C4 H4A 0.9500 . ? C31 C33 1.515(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C9 C10 1.395(4) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C3 C2 1.382(4) . ? C3 H3B 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C2 H2A 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Al1 C32 113.05(10) . . ? N2 Al1 C31 112.35(11) . . ? C32 Al1 C31 117.52(12) . . ? N2 Al1 N1 83.73(9) . . ? C32 Al1 N1 113.53(11) . . ? C31 Al1 N1 111.93(11) . . ? C6 N2 C7 104.21(18) . . ? C6 N2 Al1 113.99(16) . . ? C7 N2 Al1 141.79(16) . . ? C1 N1 C5 119.0(2) . . ? C1 N1 Al1 127.82(18) . . ? C5 N1 Al1 113.16(16) . . ? N1 C5 C4 122.5(2) . . ? N1 C5 C6 112.6(2) . . ? C4 C5 C6 124.9(2) . . ? C6 N3 C12 102.82(19) . . ? C34 C32 Al1 111.31(18) . . ? C34 C32 H32A 109.4 . . ? Al1 C32 H32A 109.4 . . ? C34 C32 H32B 109.4 . . ? Al1 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? N3 C6 N2 116.4(2) . . ? N3 C6 C5 127.1(2) . . ? N2 C6 C5 116.5(2) . . ? N3 C12 C11 130.5(2) . . ? N3 C12 C7 110.0(2) . . ? C11 C12 C7 119.5(2) . . ? N2 C7 C8 131.7(2) . . ? N2 C7 C12 106.7(2) . . ? C8 C7 C12 121.6(2) . . ? C10 C11 C12 118.4(2) . . ? C10 C11 H11A 120.8 . . ? C12 C11 H11A 120.8 . . ? C9 C8 C7 117.7(2) . . ? C9 C8 H8A 121.2 . . ? C7 C8 H8A 121.2 . . ? N1 C1 C2 120.7(2) . . ? N1 C1 C13 116.7(2) . . ? C2 C1 C13 122.6(2) . . ? C5 C4 C3 118.2(3) . . ? C5 C4 H4A 120.9 . . ? C3 C4 H4A 120.9 . . ? C33 C31 Al1 117.5(2) . . ? C33 C31 H31A 107.9 . . ? Al1 C31 H31A 107.9 . . ? C33 C31 H31B 107.9 . . ? Al1 C31 H31B 107.9 . . ? H31A C31 H31B 107.2 . . ? C8 C9 C10 121.4(3) . . ? C8 C9 H9A 119.3 . . ? C10 C9 H9A 119.3 . . ? C11 C10 C9 121.3(2) . . ? C11 C10 H10A 119.3 . . ? C9 C10 H10A 119.3 . . ? C2 C3 C4 119.3(3) . . ? C2 C3 H3B 120.3 . . ? C4 C3 H3B 120.3 . . ? C1 C13 H13A 109.5 . . ? C1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C1 C2 C3 120.2(3) . . ? C1 C2 H2A 119.9 . . ? C3 C2 H2A 119.9 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C32 Al1 N2 C6 112.08(17) . . . . ? C31 Al1 N2 C6 -112.03(18) . . . . ? N1 Al1 N2 C6 -0.87(16) . . . . ? C32 Al1 N2 C7 -66.6(3) . . . . ? C31 Al1 N2 C7 69.3(3) . . . . ? N1 Al1 N2 C7 -179.5(3) . . . . ? N2 Al1 N1 C1 -180.0(2) . . . . ? C32 Al1 N1 C1 67.6(2) . . . . ? C31 Al1 N1 C1 -68.3(2) . . . . ? N2 Al1 N1 C5 -0.08(16) . . . . ? C32 Al1 N1 C5 -112.52(17) . . . . ? C31 Al1 N1 C5 111.53(17) . . . . ? C1 N1 C5 C4 0.4(3) . . . . ? Al1 N1 C5 C4 -179.52(18) . . . . ? C1 N1 C5 C6 -179.2(2) . . . . ? Al1 N1 C5 C6 0.9(2) . . . . ? N2 Al1 C32 C34 55.3(2) . . . . ? C31 Al1 C32 C34 -78.2(2) . . . . ? N1 Al1 C32 C34 148.48(17) . . . . ? C12 N3 C6 N2 0.2(3) . . . . ? C12 N3 C6 C5 179.3(2) . . . . ? C7 N2 C6 N3 0.0(3) . . . . ? Al1 N2 C6 N3 -179.15(16) . . . . ? C7 N2 C6 C5 -179.22(19) . . . . ? Al1 N2 C6 C5 1.6(3) . . . . ? N1 C5 C6 N3 179.2(2) . . . . ? C4 C5 C6 N3 -0.4(4) . . . . ? N1 C5 C6 N2 -1.7(3) . . . . ? C4 C5 C6 N2 178.8(2) . . . . ? C6 N3 C12 C11 179.2(2) . . . . ? C6 N3 C12 C7 -0.2(2) . . . . ? C6 N2 C7 C8 180.0(3) . . . . ? Al1 N2 C7 C8 -1.3(5) . . . . ? C6 N2 C7 C12 -0.1(2) . . . . ? Al1 N2 C7 C12 178.6(2) . . . . ? N3 C12 C7 N2 0.2(3) . . . . ? C11 C12 C7 N2 -179.3(2) . . . . ? N3 C12 C7 C8 -179.9(2) . . . . ? C11 C12 C7 C8 0.6(4) . . . . ? N3 C12 C11 C10 -179.7(2) . . . . ? C7 C12 C11 C10 -0.3(4) . . . . ? N2 C7 C8 C9 179.4(2) . . . . ? C12 C7 C8 C9 -0.4(4) . . . . ? C5 N1 C1 C2 0.4(4) . . . . ? Al1 N1 C1 C2 -179.70(19) . . . . ? C5 N1 C1 C13 179.3(2) . . . . ? Al1 N1 C1 C13 -0.8(3) . . . . ? N1 C5 C4 C3 -1.2(4) . . . . ? C6 C5 C4 C3 178.3(2) . . . . ? N2 Al1 C31 C33 68.9(2) . . . . ? C32 Al1 C31 C33 -157.3(2) . . . . ? N1 Al1 C31 C33 -23.3(3) . . . . ? C7 C8 C9 C10 0.0(4) . . . . ? C12 C11 C10 C9 -0.1(4) . . . . ? C8 C9 C10 C11 0.2(4) . . . . ? C5 C4 C3 C2 1.1(4) . . . . ? N1 C1 C2 C3 -0.4(4) . . . . ? C13 C1 C2 C3 -179.3(3) . . . . ? C4 C3 C2 C1 -0.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.625 _refine_diff_density_min -0.341 _refine_diff_density_rms 0.117 #==End data_4 _database_code_depnum_ccdc_archive 'CCDC 777732' #TrackingRef '- CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H18 Al N3' _chemical_formula_weight 315.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.0651(14) _cell_length_b 12.449(3) _cell_length_c 18.375(4) _cell_angle_alpha 90.00 _cell_angle_beta 89.19(3) _cell_angle_gamma 90.00 _cell_volume 1615.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 25.00 _exptl_crystal_description Plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 0.128 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.9724 _exptl_absorpt_correction_T_max 0.9962 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 10089 _diffrn_reflns_av_R_equivalents 0.1221 _diffrn_reflns_av_sigmaI/netI 0.1020 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2850 _reflns_number_gt 2324 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1035P)^2^+5.9314P] 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 2850 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.1483 _refine_ls_R_factor_gt 0.1260 _refine_ls_wR_factor_ref 0.3101 _refine_ls_wR_factor_gt 0.2970 _refine_ls_goodness_of_fit_ref 1.200 _refine_ls_restrained_S_all 1.200 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.2393(3) 0.59744(14) 0.35026(10) 0.0309(5) Uani 1 1 d . . . N3 N 0.2561(8) 0.3326(4) 0.2166(3) 0.0366(13) Uani 1 1 d . . . N2 N 0.2478(7) 0.4614(4) 0.3057(3) 0.0316(12) Uani 1 1 d . . . N1 N 0.2346(7) 0.6806(4) 0.2573(3) 0.0316(12) Uani 1 1 d . . . C12 C 0.2603(9) 0.3616(5) 0.3392(3) 0.0341(14) Uani 1 1 d . . . C9 C 0.2301(9) 0.6348(5) 0.1874(3) 0.0328(14) Uani 1 1 d . . . C11 C 0.2457(8) 0.4381(5) 0.2328(3) 0.0325(14) Uani 1 1 d . . . C4 C 0.2224(11) 0.7039(6) 0.1247(4) 0.0451(17) Uani 1 1 d . . . C8 C 0.2361(9) 0.5211(5) 0.1753(3) 0.0373(15) Uani 1 1 d . . . C17 C 0.2643(9) 0.2847(5) 0.2841(3) 0.0345(14) Uani 1 1 d . . . C1 C 0.2353(9) 0.7882(5) 0.2634(3) 0.0355(15) Uani 1 1 d . . . C10 C 0.2389(10) 0.8375(5) 0.3378(4) 0.0439(17) Uani 1 1 d . . . H10A H 0.2416 0.7805 0.3745 0.066 Uiso 1 1 calc R . . H10B H 0.1255 0.8817 0.3453 0.066 Uiso 1 1 calc R . . H10C H 0.3520 0.8825 0.3422 0.066 Uiso 1 1 calc R . . C5 C 0.2150(12) 0.6589(6) 0.0540(4) 0.052(2) Uani 1 1 d . . . H5A H 0.2067 0.7051 0.0130 0.063 Uiso 1 1 calc R . . C7 C 0.2284(10) 0.4829(6) 0.1042(3) 0.0417(16) Uani 1 1 d . . . H7A H 0.2291 0.4074 0.0964 0.050 Uiso 1 1 calc R . . C2 C 0.2316(10) 0.8573(5) 0.2030(4) 0.0421(16) Uani 1 1 d . . . H2A H 0.2354 0.9329 0.2101 0.050 Uiso 1 1 calc R . . C32 C 0.4742(10) 0.6208(6) 0.4040(4) 0.0458(18) Uani 1 1 d . . . H32A H 0.4702 0.5791 0.4492 0.069 Uiso 1 1 calc R . . H32B H 0.4870 0.6973 0.4155 0.069 Uiso 1 1 calc R . . H32C H 0.5826 0.5976 0.3741 0.069 Uiso 1 1 calc R . . C31 C -0.0021(10) 0.6138(6) 0.4033(4) 0.0469(18) Uani 1 1 d . . . H31A H 0.0022 0.5730 0.4488 0.070 Uiso 1 1 calc R . . H31B H -0.1053 0.5866 0.3733 0.070 Uiso 1 1 calc R . . H31C H -0.0237 0.6899 0.4142 0.070 Uiso 1 1 calc R . . C16 C 0.2781(10) 0.1747(5) 0.3015(4) 0.0427(16) Uani 1 1 d . . . H16A H 0.2804 0.1210 0.2647 0.051 Uiso 1 1 calc R . . C13 C 0.2702(11) 0.3340(5) 0.4129(4) 0.0438(17) Uani 1 1 d . . . H13A H 0.2695 0.3871 0.4500 0.053 Uiso 1 1 calc R . . C3 C 0.2227(10) 0.8171(6) 0.1351(4) 0.0456(17) Uani 1 1 d . . . H3B H 0.2167 0.8640 0.0944 0.055 Uiso 1 1 calc R . . C6 C 0.2197(12) 0.5512(6) 0.0436(4) 0.053(2) Uani 1 1 d . . . H6A H 0.2171 0.5222 -0.0042 0.064 Uiso 1 1 calc R . . C15 C 0.2883(11) 0.1486(6) 0.3744(4) 0.0503(19) Uani 1 1 d . . . H15A H 0.3006 0.0752 0.3876 0.060 Uiso 1 1 calc R . . C14 C 0.2810(11) 0.2261(6) 0.4292(4) 0.0499(19) Uani 1 1 d . . . H14A H 0.2836 0.2040 0.4787 0.060 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 0.0269(10) 0.0329(10) 0.0327(10) -0.0047(7) 0.0022(7) 0.0000(8) N3 0.037(3) 0.038(3) 0.035(3) -0.004(2) 0.003(2) 0.001(2) N2 0.033(3) 0.028(3) 0.033(3) -0.002(2) 0.001(2) -0.002(2) N1 0.027(3) 0.032(3) 0.036(3) 0.001(2) 0.002(2) 0.004(2) C12 0.035(4) 0.033(3) 0.034(3) -0.003(3) 0.003(3) -0.002(3) C9 0.023(3) 0.041(4) 0.034(3) -0.005(3) 0.001(2) -0.005(3) C11 0.022(3) 0.040(3) 0.036(3) -0.011(3) 0.006(2) -0.001(3) C4 0.057(5) 0.045(4) 0.034(3) 0.002(3) -0.003(3) 0.005(3) C8 0.034(4) 0.040(4) 0.038(3) 0.001(3) 0.002(3) -0.002(3) C17 0.027(3) 0.033(3) 0.043(4) -0.003(3) 0.002(3) 0.000(3) C1 0.024(3) 0.037(4) 0.045(4) -0.002(3) 0.000(3) -0.002(3) C10 0.038(4) 0.034(4) 0.059(4) -0.013(3) 0.000(3) 0.001(3) C5 0.063(5) 0.055(5) 0.038(4) 0.003(3) -0.004(3) 0.002(4) C7 0.043(4) 0.047(4) 0.035(3) -0.005(3) 0.002(3) 0.001(3) C2 0.038(4) 0.034(4) 0.054(4) -0.002(3) 0.003(3) -0.001(3) C32 0.038(4) 0.058(5) 0.041(4) -0.009(3) -0.010(3) 0.000(3) C31 0.038(4) 0.056(5) 0.047(4) -0.009(3) 0.006(3) 0.006(3) C16 0.047(4) 0.038(4) 0.043(4) -0.007(3) 0.006(3) 0.000(3) C13 0.055(5) 0.034(4) 0.041(4) 0.001(3) -0.004(3) -0.004(3) C3 0.043(4) 0.040(4) 0.054(4) 0.012(3) -0.001(3) -0.002(3) C6 0.065(5) 0.063(5) 0.031(3) -0.005(3) 0.003(3) 0.000(4) C15 0.052(5) 0.035(4) 0.064(5) 0.004(3) 0.003(4) -0.003(3) C14 0.060(5) 0.049(4) 0.041(4) 0.003(3) -0.001(3) -0.003(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 N2 1.882(5) . ? Al1 C31 1.963(7) . ? Al1 C32 1.964(6) . ? Al1 N1 1.998(5) . ? N3 C11 1.349(8) . ? N3 C17 1.379(8) . ? N2 C11 1.371(7) . ? N2 C12 1.389(8) . ? N1 C1 1.344(8) . ? N1 C9 1.407(7) . ? C12 C17 1.395(8) . ? C12 C13 1.400(9) . ? C9 C8 1.434(9) . ? C9 C4 1.438(9) . ? C11 C8 1.481(9) . ? C4 C5 1.418(9) . ? C4 C3 1.422(10) . ? C8 C7 1.392(9) . ? C17 C16 1.409(9) . ? C1 C2 1.405(9) . ? C1 C10 1.498(9) . ? C5 C6 1.355(11) . ? C7 C6 1.403(10) . ? C2 C3 1.347(9) . ? C16 C15 1.381(10) . ? C13 C14 1.379(10) . ? C15 C14 1.396(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 N2 Al1 C31 109.3(3) . . ? N2 Al1 C32 109.2(3) . . ? C31 Al1 C32 118.0(3) . . ? N2 Al1 N1 95.5(2) . . ? C31 Al1 N1 110.2(3) . . ? C32 Al1 N1 112.2(3) . . ? C11 N3 C17 103.0(5) . . ? C11 N2 C12 104.2(5) . . ? C11 N2 Al1 127.9(4) . . ? C12 N2 Al1 127.9(4) . . ? C1 N1 C9 118.7(5) . . ? C1 N1 Al1 116.5(4) . . ? C9 N1 Al1 124.9(4) . . ? N2 C12 C17 107.0(5) . . ? N2 C12 C13 130.8(6) . . ? C17 C12 C13 122.2(6) . . ? N1 C9 C8 122.8(5) . . ? N1 C9 C4 119.4(6) . . ? C8 C9 C4 117.9(5) . . ? N3 C11 N2 114.9(5) . . ? N3 C11 C8 121.6(5) . . ? N2 C11 C8 123.5(5) . . ? C5 C4 C3 121.0(6) . . ? C5 C4 C9 120.0(6) . . ? C3 C4 C9 119.1(6) . . ? C7 C8 C9 118.8(6) . . ? C7 C8 C11 115.7(6) . . ? C9 C8 C11 125.4(5) . . ? N3 C17 C12 110.8(5) . . ? N3 C17 C16 129.0(6) . . ? C12 C17 C16 120.2(6) . . ? N1 C1 C2 123.0(6) . . ? N1 C1 C10 118.9(6) . . ? C2 C1 C10 118.1(6) . . ? C6 C5 C4 121.3(7) . . ? C8 C7 C6 122.7(7) . . ? C3 C2 C1 120.4(6) . . ? C15 C16 C17 117.0(6) . . ? C14 C13 C12 117.0(6) . . ? C2 C3 C4 119.5(6) . . ? C5 C6 C7 119.3(6) . . ? C16 C15 C14 122.4(7) . . ? C13 C14 C15 121.2(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C31 Al1 N2 C11 112.2(5) . . . . ? C32 Al1 N2 C11 -117.2(5) . . . . ? N1 Al1 N2 C11 -1.4(5) . . . . ? C31 Al1 N2 C12 -68.7(6) . . . . ? C32 Al1 N2 C12 61.8(6) . . . . ? N1 Al1 N2 C12 177.6(5) . . . . ? N2 Al1 N1 C1 -177.5(5) . . . . ? C31 Al1 N1 C1 69.5(5) . . . . ? C32 Al1 N1 C1 -64.1(5) . . . . ? N2 Al1 N1 C9 2.7(5) . . . . ? C31 Al1 N1 C9 -110.3(5) . . . . ? C32 Al1 N1 C9 116.0(5) . . . . ? C11 N2 C12 C17 -0.2(7) . . . . ? Al1 N2 C12 C17 -179.4(4) . . . . ? C11 N2 C12 C13 179.1(7) . . . . ? Al1 N2 C12 C13 -0.1(10) . . . . ? C1 N1 C9 C8 177.6(6) . . . . ? Al1 N1 C9 C8 -2.6(8) . . . . ? C1 N1 C9 C4 -1.3(9) . . . . ? Al1 N1 C9 C4 178.5(5) . . . . ? C17 N3 C11 N2 0.4(7) . . . . ? C17 N3 C11 C8 179.4(5) . . . . ? C12 N2 C11 N3 -0.2(7) . . . . ? Al1 N2 C11 N3 179.1(4) . . . . ? C12 N2 C11 C8 -179.1(6) . . . . ? Al1 N2 C11 C8 0.1(9) . . . . ? N1 C9 C4 C5 -179.1(6) . . . . ? C8 C9 C4 C5 2.0(10) . . . . ? N1 C9 C4 C3 1.0(10) . . . . ? C8 C9 C4 C3 -177.9(6) . . . . ? N1 C9 C8 C7 179.1(6) . . . . ? C4 C9 C8 C7 -2.0(9) . . . . ? N1 C9 C8 C11 0.7(10) . . . . ? C4 C9 C8 C11 179.6(6) . . . . ? N3 C11 C8 C7 3.3(9) . . . . ? N2 C11 C8 C7 -177.8(6) . . . . ? N3 C11 C8 C9 -178.2(6) . . . . ? N2 C11 C8 C9 0.7(10) . . . . ? C11 N3 C17 C12 -0.5(7) . . . . ? C11 N3 C17 C16 -179.5(7) . . . . ? N2 C12 C17 N3 0.5(7) . . . . ? C13 C12 C17 N3 -178.9(6) . . . . ? N2 C12 C17 C16 179.5(6) . . . . ? C13 C12 C17 C16 0.2(10) . . . . ? C9 N1 C1 C2 0.1(9) . . . . ? Al1 N1 C1 C2 -179.8(5) . . . . ? C9 N1 C1 C10 179.6(5) . . . . ? Al1 N1 C1 C10 -0.2(8) . . . . ? C3 C4 C5 C6 178.2(7) . . . . ? C9 C4 C5 C6 -1.6(12) . . . . ? C9 C8 C7 C6 1.6(10) . . . . ? C11 C8 C7 C6 -179.7(7) . . . . ? N1 C1 C2 C3 1.5(10) . . . . ? C10 C1 C2 C3 -178.1(6) . . . . ? N3 C17 C16 C15 178.5(6) . . . . ? C12 C17 C16 C15 -0.3(10) . . . . ? N2 C12 C13 C14 179.8(7) . . . . ? C17 C12 C13 C14 -1.1(10) . . . . ? C1 C2 C3 C4 -1.7(11) . . . . ? C5 C4 C3 C2 -179.4(7) . . . . ? C9 C4 C3 C2 0.5(11) . . . . ? C4 C5 C6 C7 1.2(12) . . . . ? C8 C7 C6 C5 -1.2(12) . . . . ? C17 C16 C15 C14 1.4(11) . . . . ? C12 C13 C14 C15 2.1(11) . . . . ? C16 C15 C14 C13 -2.4(12) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.535 _refine_diff_density_min -0.447 _refine_diff_density_rms 0.114 #==End data_7 _database_code_depnum_ccdc_archive 'CCDC 777733' #TrackingRef '- CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H30 Al2 Cl2 N6' _chemical_formula_weight 599.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 9.949(2) _cell_length_b 11.954(2) _cell_length_c 13.354(3) _cell_angle_alpha 110.54(3) _cell_angle_beta 100.71(3) _cell_angle_gamma 93.27(3) _cell_volume 1448.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.67 _cell_measurement_theta_max 27.48 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 0.317 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.9393 _exptl_absorpt_correction_T_max 0.9393 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 17932 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0506 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6604 _reflns_number_gt 5716 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+1.1173P] 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 6604 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0815 _refine_ls_R_factor_gt 0.0702 _refine_ls_wR_factor_ref 0.1882 _refine_ls_wR_factor_gt 0.1796 _refine_ls_goodness_of_fit_ref 1.172 _refine_ls_restrained_S_all 1.172 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.56746(8) 0.05886(7) 0.25326(7) 0.0408(2) Uani 1 1 d . . . Cl2 Cl 0.91348(9) 0.08224(8) 0.21970(7) 0.0439(2) Uani 1 1 d . . . Al1 Al 0.78119(9) 0.38541(8) 0.71731(7) 0.0284(2) Uani 1 1 d . . . Al2 Al 0.73580(10) 0.17635(8) 0.24728(7) 0.0308(2) Uani 1 1 d . . . N2 N 0.8083(2) 0.3912(2) 0.57885(19) 0.0266(5) Uani 1 1 d . . . N3 N 0.7901(2) 0.2934(2) 0.39692(19) 0.0267(5) Uani 1 1 d . . . N1 N 0.7967(2) 0.2035(2) 0.6327(2) 0.0282(5) Uani 1 1 d . . . N1A N 0.7804(3) 0.5719(2) 0.7898(2) 0.0313(5) Uani 1 1 d . . . N3A N 1.1151(3) 0.5724(2) 0.9492(2) 0.0323(6) Uani 1 1 d . . . N2A N 0.9576(2) 0.4220(2) 0.81486(19) 0.0282(5) Uani 1 1 d . . . C6 C 0.7955(3) 0.2849(2) 0.4956(2) 0.0259(6) Uani 1 1 d . . . C6A C 0.9911(3) 0.5411(3) 0.8830(2) 0.0283(6) Uani 1 1 d . . . C4 C 0.8106(3) 0.0629(3) 0.4565(3) 0.0338(7) Uani 1 1 d . . . H4A H 0.8199 0.0479 0.3835 0.041 Uiso 1 1 calc R . . C7 C 0.8226(3) 0.4785(3) 0.5327(2) 0.0273(6) Uani 1 1 d . . . C11 C 0.8199(3) 0.4823(3) 0.3511(3) 0.0325(6) Uani 1 1 d . . . H11A H 0.8096 0.4422 0.2743 0.039 Uiso 1 1 calc R . . C8 C 0.8554(3) 0.6038(3) 0.5812(3) 0.0325(7) Uani 1 1 d . . . H8A H 0.8698 0.6448 0.6582 0.039 Uiso 1 1 calc R . . C11A C 1.3040(3) 0.4453(3) 0.9635(3) 0.0370(7) Uani 1 1 d . . . H11B H 1.3680 0.5085 1.0190 0.044 Uiso 1 1 calc R . . C5A C 0.8930(3) 0.6233(3) 0.8725(2) 0.0309(6) Uani 1 1 d . . . C12 C 0.8089(3) 0.4181(3) 0.4197(2) 0.0270(6) Uani 1 1 d . . . C5 C 0.7983(3) 0.1774(3) 0.5250(2) 0.0285(6) Uani 1 1 d . . . C9 C 0.8657(3) 0.6649(3) 0.5125(3) 0.0344(7) Uani 1 1 d . . . H9A H 0.8867 0.7502 0.5430 0.041 Uiso 1 1 calc R . . C7A C 1.0768(3) 0.3719(3) 0.8403(2) 0.0297(6) Uani 1 1 d . . . C12A C 1.1727(3) 0.4659(3) 0.9229(3) 0.0312(6) Uani 1 1 d . . . C10 C 0.8465(3) 0.6063(3) 0.4000(3) 0.0349(7) Uani 1 1 d . . . H10A H 0.8518 0.6526 0.3554 0.042 Uiso 1 1 calc R . . C31 C 0.5933(3) 0.3428(3) 0.7388(3) 0.0336(7) Uani 1 1 d . . . H31A H 0.6050 0.3067 0.7957 0.040 Uiso 1 1 calc R . . H31B H 0.5534 0.4186 0.7681 0.040 Uiso 1 1 calc R . . C1 C 0.7937(3) 0.1133(3) 0.6714(3) 0.0334(7) Uani 1 1 d . . . C8A C 1.1133(3) 0.2554(3) 0.7980(3) 0.0346(7) Uani 1 1 d . . . H8AA H 1.0502 0.1913 0.7427 0.041 Uiso 1 1 calc R . . C4A C 0.9126(4) 0.7447(3) 0.9388(3) 0.0386(7) Uani 1 1 d . . . H4AA H 0.9932 0.7788 0.9955 0.046 Uiso 1 1 calc R . . C35 C 0.6813(4) 0.2418(3) 0.1330(3) 0.0379(7) Uani 1 1 d . . . H35A H 0.6131 0.2979 0.1540 0.046 Uiso 1 1 calc R . . H35B H 0.7632 0.2885 0.1274 0.046 Uiso 1 1 calc R . . C13A C 0.5621(4) 0.5858(4) 0.6751(3) 0.0478(9) Uani 1 1 d . . . H13A H 0.5676 0.4998 0.6390 0.072 Uiso 1 1 calc R . . H13B H 0.5629 0.6260 0.6227 0.072 Uiso 1 1 calc R . . H13C H 0.4764 0.5955 0.7017 0.072 Uiso 1 1 calc R . . C2A C 0.6980(4) 0.7623(3) 0.8350(3) 0.0447(8) Uani 1 1 d . . . H2AA H 0.6290 0.8100 0.8209 0.054 Uiso 1 1 calc R . . C1A C 0.6837(3) 0.6412(3) 0.7704(3) 0.0373(7) Uani 1 1 d . . . C2 C 0.7977(4) -0.0043(3) 0.6031(3) 0.0397(8) Uani 1 1 d . . . H2A H 0.7926 -0.0678 0.6301 0.048 Uiso 1 1 calc R . . C13 C 0.7884(4) 0.1398(3) 0.7885(3) 0.0423(8) Uani 1 1 d . . . H13D H 0.7862 0.2263 0.8252 0.063 Uiso 1 1 calc R . . H13E H 0.8702 0.1160 0.8252 0.063 Uiso 1 1 calc R . . H13F H 0.7052 0.0944 0.7918 0.063 Uiso 1 1 calc R . . C9A C 1.2454(4) 0.2377(3) 0.8402(3) 0.0401(8) Uani 1 1 d . . . H9AA H 1.2728 0.1598 0.8129 0.048 Uiso 1 1 calc R . . C10A C 1.3391(3) 0.3312(3) 0.9216(3) 0.0412(8) Uani 1 1 d . . . H10B H 1.4286 0.3156 0.9484 0.049 Uiso 1 1 calc R . . C3 C 0.8090(4) -0.0294(3) 0.4961(3) 0.0385(7) Uani 1 1 d . . . H3A H 0.8156 -0.1092 0.4503 0.046 Uiso 1 1 calc R . . C3A C 0.8125(4) 0.8143(3) 0.9203(3) 0.0461(9) Uani 1 1 d . . . H3AB H 0.8218 0.8972 0.9654 0.055 Uiso 1 1 calc R . . C36 C 0.6194(5) 0.1448(4) 0.0219(3) 0.0552(10) Uani 1 1 d . . . H36A H 0.5931 0.1822 -0.0321 0.083 Uiso 1 1 calc R . . H36B H 0.5376 0.0989 0.0266 0.083 Uiso 1 1 calc R . . H36C H 0.6876 0.0904 -0.0005 0.083 Uiso 1 1 calc R . . C33 C 0.4897(4) 0.2580(4) 0.6400(4) 0.0743(14) Uani 1 1 d . . . H33A H 0.4026 0.2448 0.6610 0.111 Uiso 1 1 calc R . . H33B H 0.5252 0.1810 0.6114 0.111 Uiso 1 1 calc R . . H33C H 0.4738 0.2932 0.5834 0.111 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 Cl1 0.0384(4) 0.0364(4) 0.0431(5) 0.0145(4) 0.0006(3) -0.0017(3) Cl2 0.0453(5) 0.0412(5) 0.0434(5) 0.0096(4) 0.0148(4) 0.0135(4) Al1 0.0291(5) 0.0284(5) 0.0259(5) 0.0076(4) 0.0061(3) 0.0045(3) Al2 0.0350(5) 0.0282(5) 0.0256(5) 0.0068(4) 0.0046(4) 0.0033(4) N2 0.0271(12) 0.0246(12) 0.0272(12) 0.0090(10) 0.0047(9) 0.0057(9) N3 0.0286(12) 0.0238(11) 0.0267(12) 0.0089(10) 0.0047(9) 0.0041(9) N1 0.0297(12) 0.0259(12) 0.0285(13) 0.0096(10) 0.0065(10) 0.0020(9) N1A 0.0330(13) 0.0328(13) 0.0293(13) 0.0108(11) 0.0096(10) 0.0092(10) N3A 0.0328(13) 0.0301(13) 0.0333(14) 0.0111(11) 0.0074(11) 0.0011(10) N2A 0.0314(13) 0.0261(12) 0.0254(12) 0.0080(10) 0.0056(10) 0.0033(10) C6 0.0245(13) 0.0235(13) 0.0254(14) 0.0063(11) 0.0007(10) 0.0031(10) C6A 0.0313(15) 0.0282(14) 0.0267(14) 0.0102(12) 0.0086(11) 0.0051(11) C4 0.0419(17) 0.0296(15) 0.0268(15) 0.0088(12) 0.0023(12) 0.0077(13) C7 0.0287(14) 0.0258(14) 0.0281(14) 0.0105(12) 0.0061(11) 0.0073(11) C11 0.0341(16) 0.0353(16) 0.0279(15) 0.0116(13) 0.0065(12) 0.0060(13) C8 0.0375(16) 0.0265(14) 0.0307(16) 0.0070(12) 0.0073(13) 0.0059(12) C11A 0.0309(16) 0.0403(18) 0.0380(18) 0.0134(14) 0.0060(13) 0.0027(13) C5A 0.0321(15) 0.0318(15) 0.0280(15) 0.0094(12) 0.0079(12) 0.0046(12) C12 0.0251(14) 0.0253(14) 0.0286(15) 0.0081(11) 0.0040(11) 0.0052(11) C5 0.0267(14) 0.0286(14) 0.0277(15) 0.0097(12) 0.0017(11) 0.0027(11) C9 0.0383(17) 0.0242(14) 0.0418(18) 0.0123(13) 0.0104(14) 0.0073(12) C7A 0.0311(15) 0.0327(15) 0.0297(15) 0.0151(13) 0.0092(12) 0.0059(12) C12A 0.0310(15) 0.0310(15) 0.0345(16) 0.0141(13) 0.0096(12) 0.0058(12) C10 0.0379(17) 0.0317(16) 0.0407(18) 0.0193(14) 0.0092(13) 0.0089(13) C31 0.0280(15) 0.0336(16) 0.0364(17) 0.0072(13) 0.0125(12) 0.0031(12) C1 0.0336(16) 0.0329(16) 0.0333(16) 0.0145(13) 0.0033(12) 0.0008(12) C8A 0.0373(17) 0.0319(15) 0.0359(17) 0.0136(13) 0.0092(13) 0.0049(13) C4A 0.0430(18) 0.0322(16) 0.0357(17) 0.0079(14) 0.0066(14) 0.0044(14) C35 0.0478(19) 0.0332(16) 0.0335(17) 0.0127(14) 0.0094(14) 0.0075(14) C13A 0.0384(19) 0.055(2) 0.049(2) 0.0171(18) 0.0077(16) 0.0179(16) C2A 0.044(2) 0.0432(19) 0.048(2) 0.0164(16) 0.0117(16) 0.0183(16) C1A 0.0338(16) 0.0427(18) 0.0390(18) 0.0166(15) 0.0111(13) 0.0134(14) C2 0.049(2) 0.0293(16) 0.0427(19) 0.0182(14) 0.0054(15) 0.0041(14) C13 0.055(2) 0.0377(18) 0.0347(18) 0.0148(15) 0.0105(15) 0.0019(15) C9A 0.0425(18) 0.0363(17) 0.047(2) 0.0179(15) 0.0150(15) 0.0143(14) C10A 0.0321(17) 0.0461(19) 0.050(2) 0.0213(16) 0.0099(14) 0.0124(14) C3 0.050(2) 0.0252(15) 0.0364(17) 0.0091(13) 0.0031(14) 0.0076(13) C3A 0.055(2) 0.0335(17) 0.049(2) 0.0115(16) 0.0144(17) 0.0147(16) C36 0.077(3) 0.051(2) 0.0323(19) 0.0127(17) 0.0057(18) 0.011(2) C33 0.037(2) 0.072(3) 0.085(3) -0.001(3) 0.008(2) -0.004(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 Cl1 Al2 2.1549(14) . ? Cl2 Al2 2.1689(14) . ? Al1 N2A 1.906(3) . ? Al1 N2 1.942(3) . ? Al1 C31 2.007(3) . ? Al1 N1A 2.096(3) . ? Al1 N1 2.099(3) . ? Al2 N3 1.948(3) . ? Al2 C35 1.953(3) . ? N2 C6 1.344(4) . ? N2 C7 1.399(4) . ? N3 C6 1.348(4) . ? N3 C12 1.407(4) . ? N1 C1 1.350(4) . ? N1 C5 1.365(4) . ? N1A C1A 1.352(4) . ? N1A C5A 1.356(4) . ? N3A C6A 1.324(4) . ? N3A C12A 1.385(4) . ? N2A C6A 1.374(4) . ? N2A C7A 1.398(4) . ? C6 C5 1.470(4) . ? C6A C5A 1.447(4) . ? C4 C3 1.381(4) . ? C4 C5 1.381(4) . ? C4 H4A 0.9500 . ? C7 C8 1.398(4) . ? C7 C12 1.402(4) . ? C11 C10 1.380(4) . ? C11 C12 1.399(4) . ? C11 H11A 0.9500 . ? C8 C9 1.372(4) . ? C8 H8A 0.9500 . ? C11A C10A 1.373(5) . ? C11A C12A 1.389(4) . ? C11A H11B 0.9500 . ? C5A C4A 1.390(4) . ? C9 C10 1.387(5) . ? C9 H9A 0.9500 . ? C7A C8A 1.404(4) . ? C7A C12A 1.417(4) . ? C10 H10A 0.9500 . ? C31 C33 1.505(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C1 C2 1.390(5) . ? C1 C13 1.495(5) . ? C8A C9A 1.389(5) . ? C8A H8AA 0.9500 . ? C4A C3A 1.376(5) . ? C4A H4AA 0.9500 . ? C35 C36 1.515(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C13A C1A 1.505(5) . ? C13A H13A 0.9800 . ? C13A H13B 0.9800 . ? C13A H13C 0.9800 . ? C2A C1A 1.385(5) . ? C2A C3A 1.386(5) . ? C2A H2AA 0.9500 . ? C2 C3 1.381(5) . ? C2 H2A 0.9500 . ? C13 H13D 0.9800 . ? C13 H13E 0.9800 . ? C13 H13F 0.9800 . ? C9A C10A 1.397(5) . ? C9A H9AA 0.9500 . ? C10A H10B 0.9500 . ? C3 H3A 0.9500 . ? C3A H3AB 0.9500 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? 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 N2A Al1 N2 107.75(11) . . ? N2A Al1 C31 130.52(13) . . ? N2 Al1 C31 121.71(13) . . ? N2A Al1 N1A 82.56(11) . . ? N2 Al1 N1A 94.22(11) . . ? C31 Al1 N1A 94.35(12) . . ? N2A Al1 N1 96.31(11) . . ? N2 Al1 N1 79.56(10) . . ? C31 Al1 N1 91.59(12) . . ? N1A Al1 N1 173.05(11) . . ? N3 Al2 C35 116.11(13) . . ? N3 Al2 Cl1 103.41(9) . . ? C35 Al2 Cl1 111.21(12) . . ? N3 Al2 Cl2 105.26(9) . . ? C35 Al2 Cl2 109.68(12) . . ? Cl1 Al2 Cl2 110.89(5) . . ? C6 N2 C7 105.2(2) . . ? C6 N2 Al1 116.60(19) . . ? C7 N2 Al1 137.6(2) . . ? C6 N3 C12 104.4(2) . . ? C6 N3 Al2 133.0(2) . . ? C12 N3 Al2 121.66(19) . . ? C1 N1 C5 119.4(3) . . ? C1 N1 Al1 127.0(2) . . ? C5 N1 Al1 113.34(19) . . ? C1A N1A C5A 119.0(3) . . ? C1A N1A Al1 130.0(2) . . ? C5A N1A Al1 110.9(2) . . ? C6A N3A C12A 103.4(3) . . ? C6A N2A C7A 103.1(2) . . ? C6A N2A Al1 114.2(2) . . ? C7A N2A Al1 142.6(2) . . ? N2 C6 N3 114.5(2) . . ? N2 C6 C5 116.3(3) . . ? N3 C6 C5 129.1(3) . . ? N3A C6A N2A 116.7(3) . . ? N3A C6A C5A 125.1(3) . . ? N2A C6A C5A 118.1(3) . . ? C3 C4 C5 118.7(3) . . ? C3 C4 H4A 120.7 . . ? C5 C4 H4A 120.7 . . ? C8 C7 N2 131.1(3) . . ? C8 C7 C12 121.1(3) . . ? N2 C7 C12 107.6(2) . . ? C10 C11 C12 117.1(3) . . ? C10 C11 H11A 121.5 . . ? C12 C11 H11A 121.5 . . ? C9 C8 C7 117.0(3) . . ? C9 C8 H8A 121.5 . . ? C7 C8 H8A 121.5 . . ? C10A C11A C12A 118.4(3) . . ? C10A C11A H11B 120.8 . . ? C12A C11A H11B 120.8 . . ? N1A C5A C4A 122.5(3) . . ? N1A C5A C6A 113.9(3) . . ? C4A C5A C6A 123.6(3) . . ? C11 C12 C7 120.8(3) . . ? C11 C12 N3 131.0(3) . . ? C7 C12 N3 108.1(2) . . ? N1 C5 C4 121.8(3) . . ? N1 C5 C6 112.3(3) . . ? C4 C5 C6 125.8(3) . . ? C8 C9 C10 122.2(3) . . ? C8 C9 H9A 118.9 . . ? C10 C9 H9A 118.9 . . ? N2A C7A C8A 132.6(3) . . ? N2A C7A C12A 107.1(3) . . ? C8A C7A C12A 120.2(3) . . ? N3A C12A C11A 129.2(3) . . ? N3A C12A C7A 109.8(3) . . ? C11A C12A C7A 121.0(3) . . ? C11 C10 C9 121.6(3) . . ? C11 C10 H10A 119.2 . . ? C9 C10 H10A 119.2 . . ? C33 C31 Al1 117.4(3) . . ? C33 C31 H31A 108.0 . . ? Al1 C31 H31A 108.0 . . ? C33 C31 H31B 108.0 . . ? Al1 C31 H31B 108.0 . . ? H31A C31 H31B 107.2 . . ? N1 C1 C2 120.3(3) . . ? N1 C1 C13 120.2(3) . . ? C2 C1 C13 119.6(3) . . ? C9A C8A C7A 117.3(3) . . ? C9A C8A H8AA 121.3 . . ? C7A C8A H8AA 121.3 . . ? C3A C4A C5A 118.4(3) . . ? C3A C4A H4AA 120.8 . . ? C5A C4A H4AA 120.8 . . ? C36 C35 Al2 112.7(2) . . ? C36 C35 H35A 109.0 . . ? Al2 C35 H35A 109.0 . . ? C36 C35 H35B 109.0 . . ? Al2 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? C1A C13A H13A 109.5 . . ? C1A C13A H13B 109.5 . . ? H13A C13A H13B 109.5 . . ? C1A C13A H13C 109.5 . . ? H13A C13A H13C 109.5 . . ? H13B C13A H13C 109.5 . . ? C1A C2A C3A 120.2(3) . . ? C1A C2A H2AA 119.9 . . ? C3A C2A H2AA 119.9 . . ? N1A C1A C2A 120.7(3) . . ? N1A C1A C13A 119.1(3) . . ? C2A C1A C13A 120.2(3) . . ? C3 C2 C1 120.3(3) . . ? C3 C2 H2A 119.9 . . ? C1 C2 H2A 119.9 . . ? C1 C13 H13D 109.5 . . ? C1 C13 H13E 109.5 . . ? H13D C13 H13E 109.5 . . ? C1 C13 H13F 109.5 . . ? H13D C13 H13F 109.5 . . ? H13E C13 H13F 109.5 . . ? C8A C9A C10A 121.9(3) . . ? C8A C9A H9AA 119.0 . . ? C10A C9A H9AA 119.0 . . ? C11A C10A C9A 121.1(3) . . ? C11A C10A H10B 119.5 . . ? C9A C10A H10B 119.5 . . ? C2 C3 C4 119.3(3) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C4A C3A C2A 119.3(3) . . ? C4A C3A H3AB 120.3 . . ? C2A C3A H3AB 120.3 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2A Al1 N2 C6 106.0(2) . . . . ? C31 Al1 N2 C6 -72.7(2) . . . . ? N1A Al1 N2 C6 -170.4(2) . . . . ? N1 Al1 N2 C6 12.7(2) . . . . ? N2A Al1 N2 C7 -84.0(3) . . . . ? C31 Al1 N2 C7 97.3(3) . . . . ? N1A Al1 N2 C7 -0.4(3) . . . . ? N1 Al1 N2 C7 -177.3(3) . . . . ? C35 Al2 N3 C6 158.0(3) . . . . ? Cl1 Al2 N3 C6 36.0(3) . . . . ? Cl2 Al2 N3 C6 -80.5(3) . . . . ? C35 Al2 N3 C12 -9.2(3) . . . . ? Cl1 Al2 N3 C12 -131.3(2) . . . . ? Cl2 Al2 N3 C12 112.3(2) . . . . ? N2A Al1 N1 C1 70.5(3) . . . . ? N2 Al1 N1 C1 177.5(3) . . . . ? C31 Al1 N1 C1 -60.6(3) . . . . ? N1A Al1 N1 C1 150.8(8) . . . . ? N2A Al1 N1 C5 -115.2(2) . . . . ? N2 Al1 N1 C5 -8.2(2) . . . . ? C31 Al1 N1 C5 113.8(2) . . . . ? N1A Al1 N1 C5 -34.9(10) . . . . ? N2A Al1 N1A C1A 179.4(3) . . . . ? N2 Al1 N1A C1A 72.0(3) . . . . ? C31 Al1 N1A C1A -50.3(3) . . . . ? N1 Al1 N1A C1A 98.3(9) . . . . ? N2A Al1 N1A C5A -5.2(2) . . . . ? N2 Al1 N1A C5A -112.6(2) . . . . ? C31 Al1 N1A C5A 125.1(2) . . . . ? N1 Al1 N1A C5A -86.3(9) . . . . ? N2 Al1 N2A C6A 95.2(2) . . . . ? C31 Al1 N2A C6A -86.2(2) . . . . ? N1A Al1 N2A C6A 3.2(2) . . . . ? N1 Al1 N2A C6A 176.3(2) . . . . ? N2 Al1 N2A C7A -78.8(3) . . . . ? C31 Al1 N2A C7A 99.8(3) . . . . ? N1A Al1 N2A C7A -170.9(3) . . . . ? N1 Al1 N2A C7A 2.2(3) . . . . ? C7 N2 C6 N3 -4.5(3) . . . . ? Al1 N2 C6 N3 168.49(19) . . . . ? C7 N2 C6 C5 171.7(2) . . . . ? Al1 N2 C6 C5 -15.2(3) . . . . ? C12 N3 C6 N2 3.5(3) . . . . ? Al2 N3 C6 N2 -165.3(2) . . . . ? C12 N3 C6 C5 -172.2(3) . . . . ? Al2 N3 C6 C5 19.0(5) . . . . ? C12A N3A C6A N2A 1.1(3) . . . . ? C12A N3A C6A C5A -175.0(3) . . . . ? C7A N2A C6A N3A -1.0(3) . . . . ? Al1 N2A C6A N3A -177.2(2) . . . . ? C7A N2A C6A C5A 175.5(3) . . . . ? Al1 N2A C6A C5A -0.8(3) . . . . ? C6 N2 C7 C8 -171.5(3) . . . . ? Al1 N2 C7 C8 17.8(5) . . . . ? C6 N2 C7 C12 3.6(3) . . . . ? Al1 N2 C7 C12 -167.1(2) . . . . ? N2 C7 C8 C9 178.1(3) . . . . ? C12 C7 C8 C9 3.5(4) . . . . ? C1A N1A C5A C4A 0.4(5) . . . . ? Al1 N1A C5A C4A -175.6(2) . . . . ? C1A N1A C5A C6A -178.1(3) . . . . ? Al1 N1A C5A C6A 6.0(3) . . . . ? N3A C6A C5A N1A 172.3(3) . . . . ? N2A C6A C5A N1A -3.8(4) . . . . ? N3A C6A C5A C4A -6.1(5) . . . . ? N2A C6A C5A C4A 177.8(3) . . . . ? C10 C11 C12 C7 0.8(4) . . . . ? C10 C11 C12 N3 -176.2(3) . . . . ? C8 C7 C12 C11 -3.6(4) . . . . ? N2 C7 C12 C11 -179.3(3) . . . . ? C8 C7 C12 N3 174.0(3) . . . . ? N2 C7 C12 N3 -1.7(3) . . . . ? C6 N3 C12 C11 176.4(3) . . . . ? Al2 N3 C12 C11 -13.2(4) . . . . ? C6 N3 C12 C7 -1.0(3) . . . . ? Al2 N3 C12 C7 169.47(19) . . . . ? C1 N1 C5 C4 -6.4(4) . . . . ? Al1 N1 C5 C4 178.8(2) . . . . ? C1 N1 C5 C6 177.6(3) . . . . ? Al1 N1 C5 C6 2.8(3) . . . . ? C3 C4 C5 N1 5.7(5) . . . . ? C3 C4 C5 C6 -178.8(3) . . . . ? N2 C6 C5 N1 7.6(4) . . . . ? N3 C6 C5 N1 -176.8(3) . . . . ? N2 C6 C5 C4 -168.3(3) . . . . ? N3 C6 C5 C4 7.4(5) . . . . ? C7 C8 C9 C10 -0.8(5) . . . . ? C6A N2A C7A C8A -177.4(3) . . . . ? Al1 N2A C7A C8A -3.0(6) . . . . ? C6A N2A C7A C12A 0.3(3) . . . . ? Al1 N2A C7A C12A 174.8(3) . . . . ? C6A N3A C12A C11A 177.3(3) . . . . ? C6A N3A C12A C7A -0.8(3) . . . . ? C10A C11A C12A N3A -177.9(3) . . . . ? C10A C11A C12A C7A 0.1(5) . . . . ? N2A C7A C12A N3A 0.3(3) . . . . ? C8A C7A C12A N3A 178.4(3) . . . . ? N2A C7A C12A C11A -178.0(3) . . . . ? C8A C7A C12A C11A 0.1(5) . . . . ? C12 C11 C10 C9 1.9(5) . . . . ? C8 C9 C10 C11 -2.0(5) . . . . ? N2A Al1 C31 C33 -147.9(3) . . . . ? N2 Al1 C31 C33 30.5(4) . . . . ? N1A Al1 C31 C33 128.2(3) . . . . ? N1 Al1 C31 C33 -48.2(3) . . . . ? C5 N1 C1 C2 2.5(4) . . . . ? Al1 N1 C1 C2 176.5(2) . . . . ? C5 N1 C1 C13 -178.5(3) . . . . ? Al1 N1 C1 C13 -4.5(4) . . . . ? N2A C7A C8A C9A 177.4(3) . . . . ? C12A C7A C8A C9A -0.1(4) . . . . ? N1A C5A C4A C3A 1.0(5) . . . . ? C6A C5A C4A C3A 179.3(3) . . . . ? N3 Al2 C35 C36 -170.9(2) . . . . ? Cl1 Al2 C35 C36 -53.1(3) . . . . ? Cl2 Al2 C35 C36 70.0(3) . . . . ? C5A N1A C1A C2A -1.1(5) . . . . ? Al1 N1A C1A C2A 174.0(3) . . . . ? C5A N1A C1A C13A 177.0(3) . . . . ? Al1 N1A C1A C13A -7.9(5) . . . . ? C3A C2A C1A N1A 0.5(5) . . . . ? C3A C2A C1A C13A -177.7(3) . . . . ? N1 C1 C2 C3 2.0(5) . . . . ? C13 C1 C2 C3 -177.0(3) . . . . ? C7A C8A C9A C10A 0.1(5) . . . . ? C12A C11A C10A C9A -0.1(5) . . . . ? C8A C9A C10A C11A 0.0(5) . . . . ? C1 C2 C3 C4 -2.6(5) . . . . ? C5 C4 C3 C2 -1.1(5) . . . . ? C5A C4A C3A C2A -1.6(5) . . . . ? C1A C2A C3A C4A 0.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.526 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.124 #==End data_8 _database_code_depnum_ccdc_archive 'CCDC 777734' #TrackingRef '- CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H25 Al2 Cl2 N3' _chemical_formula_weight 420.28 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 36.391(7) _cell_length_b 7.5279(15) _cell_length_c 17.176(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.05(3) _cell_angle_gamma 90.00 _cell_volume 4361.2(15) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.21 _cell_measurement_theta_max 27.48 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.280 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 0.386 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.8392 _exptl_absorpt_correction_T_max 0.9164 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 16729 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4962 _reflns_number_gt 4733 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1162P)^2^+14.5349P] 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 4962 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0856 _refine_ls_R_factor_gt 0.0817 _refine_ls_wR_factor_ref 0.2231 _refine_ls_wR_factor_gt 0.2163 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.09112(3) 0.56948(13) 0.31090(6) 0.0336(3) Uani 1 1 d . . . Cl2 Cl 0.19203(3) -0.04407(14) 0.35405(7) 0.0590(3) Uani 1 1 d . . . Cl1 Cl 0.22753(3) 0.14641(17) 0.20562(7) 0.0572(3) Uani 1 1 d . . . Al2 Al 0.17817(3) 0.02184(14) 0.22348(7) 0.0422(3) Uani 1 1 d . . . N2 N 0.09927(7) 0.4150(4) 0.22955(16) 0.0316(5) Uani 1 1 d . . . N3 N 0.13871(7) 0.2098(3) 0.20364(16) 0.0296(5) Uani 1 1 d . . . N1 N 0.14838(7) 0.5206(3) 0.37445(16) 0.0297(5) Uani 1 1 d . . . C5 C 0.16525(8) 0.4124(4) 0.33314(18) 0.0289(6) Uani 1 1 d . . . C7 C 0.07697(8) 0.3315(4) 0.15507(19) 0.0311(6) Uani 1 1 d . . . C12 C 0.10091(8) 0.2045(4) 0.13771(18) 0.0299(6) Uani 1 1 d . . . C4 C 0.20587(9) 0.3859(4) 0.3636(2) 0.0335(6) Uani 1 1 d . . . H4A H 0.2178 0.3170 0.3331 0.040 Uiso 1 1 calc R . . C3 C 0.22890(9) 0.4633(5) 0.4405(2) 0.0372(7) Uani 1 1 d . . . H3A H 0.2568 0.4453 0.4631 0.045 Uiso 1 1 calc R . . C6 C 0.13557(8) 0.3402(4) 0.25485(18) 0.0289(6) Uani 1 1 d . . . C2 C 0.21149(10) 0.5649(4) 0.4832(2) 0.0366(7) Uani 1 1 d . . . H2A H 0.2270 0.6142 0.5363 0.044 Uiso 1 1 calc R . . C11 C 0.08613(9) 0.1019(4) 0.0644(2) 0.0351(6) Uani 1 1 d . . . H11A H 0.1022 0.0165 0.0515 0.042 Uiso 1 1 calc R . . C1 C 0.17078(9) 0.5952(4) 0.44812(19) 0.0334(6) Uani 1 1 d . . . C9 C 0.02295(10) 0.2545(5) 0.0299(2) 0.0409(7) Uani 1 1 d . . . H9A H -0.0038 0.2682 -0.0075 0.049 Uiso 1 1 calc R . . C13 C 0.15034(11) 0.7142(5) 0.4887(2) 0.0466(8) Uani 1 1 d . . . H13A H 0.1219 0.7176 0.4544 0.070 Uiso 1 1 calc R . . H13B H 0.1614 0.8343 0.4936 0.070 Uiso 1 1 calc R . . H13C H 0.1543 0.6687 0.5448 0.070 Uiso 1 1 calc R . . C8 C 0.03721(9) 0.3584(5) 0.1018(2) 0.0379(7) Uani 1 1 d . . . H8A H 0.0209 0.4434 0.1144 0.046 Uiso 1 1 calc R . . C10 C 0.04694(10) 0.1299(5) 0.0111(2) 0.0393(7) Uani 1 1 d . . . H10A H 0.0362 0.0628 -0.0392 0.047 Uiso 1 1 calc R . . C31 C 0.05762(10) 0.4449(6) 0.3613(3) 0.0500(10) Uani 1 1 d . . . H31A H 0.0595 0.5104 0.4126 0.060 Uiso 1 1 calc R . . H31B H 0.0298 0.4535 0.3214 0.060 Uiso 1 1 calc R . . C32 C 0.07958(11) 0.8183(5) 0.2753(3) 0.0500(9) Uani 1 1 d . . . H32A H 0.0768 0.8867 0.3220 0.060 Uiso 1 1 calc R . . H32B H 0.1025 0.8678 0.2648 0.060 Uiso 1 1 calc R . . C35 C 0.15897(16) -0.1979(7) 0.1593(4) 0.0815(17) Uani 1 1 d . . . H35A H 0.1686 -0.2991 0.1985 0.098 Uiso 1 1 calc R . . H35B H 0.1297 -0.1982 0.1394 0.098 Uiso 1 1 calc R . . C36 C 0.1696(2) -0.2309(12) 0.0882(5) 0.116(3) Uani 1 1 d . . . H36A H 0.1580 -0.3439 0.0621 0.174 Uiso 1 1 calc R . . H36B H 0.1985 -0.2368 0.1066 0.174 Uiso 1 1 calc R . . H36C H 0.1595 -0.1346 0.0473 0.174 Uiso 1 1 calc R . . C34 C 0.04358(15) 0.8441(7) 0.1995(4) 0.0779(16) Uani 1 1 d . . . H34A H 0.0400 0.9709 0.1858 0.117 Uiso 1 1 calc R . . H34B H 0.0205 0.7992 0.2097 0.117 Uiso 1 1 calc R . . H34C H 0.0462 0.7792 0.1524 0.117 Uiso 1 1 calc R . . C33 C 0.0656(2) 0.2701(11) 0.3824(6) 0.132(3) Uani 1 1 d . . . H33A H 0.0468 0.2251 0.4064 0.198 Uiso 1 1 calc R . . H33B H 0.0927 0.2585 0.4239 0.198 Uiso 1 1 calc R . . H33C H 0.0629 0.2013 0.3321 0.198 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 0.0257(4) 0.0360(5) 0.0401(5) -0.0035(4) 0.0136(4) 0.0033(4) Cl2 0.0401(5) 0.0544(6) 0.0681(6) 0.0274(5) 0.0039(4) -0.0013(4) Cl1 0.0383(5) 0.0817(7) 0.0587(6) -0.0074(5) 0.0264(4) 0.0079(4) Al2 0.0310(5) 0.0357(5) 0.0532(6) -0.0082(4) 0.0082(4) 0.0065(4) N2 0.0240(11) 0.0352(13) 0.0341(13) -0.0017(10) 0.0090(10) 0.0034(10) N3 0.0232(11) 0.0329(13) 0.0324(12) -0.0004(10) 0.0100(9) 0.0011(9) N1 0.0278(11) 0.0297(12) 0.0324(12) 0.0003(10) 0.0121(10) 0.0008(9) C5 0.0265(13) 0.0301(14) 0.0312(13) 0.0016(11) 0.0119(11) -0.0001(11) C7 0.0243(13) 0.0347(15) 0.0326(14) 0.0024(12) 0.0085(11) -0.0006(11) C12 0.0260(13) 0.0310(14) 0.0320(14) 0.0011(11) 0.0102(11) -0.0033(11) C4 0.0253(13) 0.0382(16) 0.0370(15) -0.0028(12) 0.0119(12) 0.0009(12) C3 0.0263(14) 0.0421(17) 0.0394(16) 0.0004(14) 0.0081(12) 0.0001(12) C6 0.0226(13) 0.0340(14) 0.0310(13) 0.0017(11) 0.0112(11) 0.0009(11) C2 0.0340(15) 0.0381(16) 0.0327(15) -0.0004(13) 0.0067(12) -0.0027(13) C11 0.0346(15) 0.0351(15) 0.0359(15) -0.0025(13) 0.0137(13) -0.0030(13) C1 0.0342(15) 0.0333(15) 0.0331(14) -0.0014(12) 0.0133(12) -0.0025(12) C9 0.0294(15) 0.0460(18) 0.0383(16) 0.0038(14) 0.0026(12) -0.0031(13) C13 0.0463(19) 0.051(2) 0.0428(18) -0.0131(16) 0.0167(15) 0.0010(16) C8 0.0269(14) 0.0421(17) 0.0408(16) 0.0032(14) 0.0080(13) 0.0043(12) C10 0.0396(17) 0.0411(17) 0.0330(15) -0.0017(13) 0.0088(13) -0.0082(14) C31 0.0295(16) 0.074(3) 0.054(2) -0.0154(19) 0.0248(15) -0.0105(17) C32 0.0390(18) 0.0354(18) 0.069(2) -0.0030(17) 0.0125(17) 0.0083(14) C35 0.069(3) 0.059(3) 0.100(4) -0.026(3) 0.012(3) 0.020(2) C36 0.113(6) 0.111(6) 0.141(7) -0.036(5) 0.067(5) -0.009(5) C34 0.057(3) 0.062(3) 0.088(4) 0.027(3) -0.004(2) -0.008(2) C33 0.124(6) 0.112(6) 0.213(10) 0.060(6) 0.124(7) 0.013(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 N2 1.925(3) . ? Al1 C32 1.966(4) . ? Al1 C31 1.976(4) . ? Al1 N1 1.990(3) . ? Cl2 Al2 2.1635(17) . ? Cl1 Al2 2.1479(16) . ? Al2 N3 1.953(3) . ? Al2 C35 1.965(5) . ? N2 C6 1.349(4) . ? N2 C7 1.382(4) . ? N3 C6 1.351(4) . ? N3 C12 1.417(4) . ? N1 C1 1.344(4) . ? N1 C5 1.368(4) . ? C5 C4 1.385(4) . ? C5 C6 1.476(4) . ? C7 C12 1.399(4) . ? C7 C8 1.406(4) . ? C12 C11 1.402(4) . ? C4 C3 1.397(4) . ? C4 H4A 0.9500 . ? C3 C2 1.369(5) . ? C3 H3A 0.9500 . ? C2 C1 1.393(4) . ? C2 H2A 0.9500 . ? C11 C10 1.391(5) . ? C11 H11A 0.9500 . ? C1 C13 1.494(5) . ? C9 C8 1.388(5) . ? C9 C10 1.399(5) . ? C9 H9A 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C8 H8A 0.9500 . ? C10 H10A 0.9500 . ? C31 C33 1.367(9) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C34 1.473(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C35 C36 1.434(9) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Al1 C32 115.05(16) . . ? N2 Al1 C31 108.65(15) . . ? C32 Al1 C31 119.54(18) . . ? N2 Al1 N1 82.61(11) . . ? C32 Al1 N1 113.83(14) . . ? C31 Al1 N1 111.28(15) . . ? N3 Al2 C35 115.39(18) . . ? N3 Al2 Cl1 104.96(10) . . ? C35 Al2 Cl1 115.3(2) . . ? N3 Al2 Cl2 102.54(10) . . ? C35 Al2 Cl2 106.5(2) . . ? Cl1 Al2 Cl2 111.48(7) . . ? C6 N2 C7 105.8(2) . . ? C6 N2 Al1 114.7(2) . . ? C7 N2 Al1 138.6(2) . . ? C6 N3 C12 104.3(2) . . ? C6 N3 Al2 130.5(2) . . ? C12 N3 Al2 123.3(2) . . ? C1 N1 C5 120.4(3) . . ? C1 N1 Al1 125.4(2) . . ? C5 N1 Al1 114.0(2) . . ? N1 C5 C4 120.8(3) . . ? N1 C5 C6 112.0(2) . . ? C4 C5 C6 127.1(3) . . ? N2 C7 C12 108.2(2) . . ? N2 C7 C8 129.8(3) . . ? C12 C7 C8 122.1(3) . . ? C7 C12 C11 120.6(3) . . ? C7 C12 N3 107.8(3) . . ? C11 C12 N3 131.6(3) . . ? C5 C4 C3 118.3(3) . . ? C5 C4 H4A 120.8 . . ? C3 C4 H4A 120.8 . . ? C2 C3 C4 120.3(3) . . ? C2 C3 H3A 119.8 . . ? C4 C3 H3A 119.8 . . ? N2 C6 N3 113.9(3) . . ? N2 C6 C5 115.7(3) . . ? N3 C6 C5 130.4(3) . . ? C3 C2 C1 119.4(3) . . ? C3 C2 H2A 120.3 . . ? C1 C2 H2A 120.3 . . ? C10 C11 C12 117.4(3) . . ? C10 C11 H11A 121.3 . . ? C12 C11 H11A 121.3 . . ? N1 C1 C2 120.6(3) . . ? N1 C1 C13 117.3(3) . . ? C2 C1 C13 122.1(3) . . ? C8 C9 C10 121.7(3) . . ? C8 C9 H9A 119.1 . . ? C10 C9 H9A 119.1 . . ? C1 C13 H13A 109.5 . . ? C1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C9 C8 C7 116.6(3) . . ? C9 C8 H8A 121.7 . . ? C7 C8 H8A 121.7 . . ? C11 C10 C9 121.6(3) . . ? C11 C10 H10A 119.2 . . ? C9 C10 H10A 119.2 . . ? C33 C31 Al1 118.0(3) . . ? C33 C31 H31A 107.8 . . ? Al1 C31 H31A 107.8 . . ? C33 C31 H31B 107.8 . . ? Al1 C31 H31B 107.8 . . ? H31A C31 H31B 107.1 . . ? C34 C32 Al1 114.6(3) . . ? C34 C32 H32A 108.6 . . ? Al1 C32 H32A 108.6 . . ? C34 C32 H32B 108.6 . . ? Al1 C32 H32B 108.6 . . ? H32A C32 H32B 107.6 . . ? C36 C35 Al2 118.1(5) . . ? C36 C35 H35A 107.8 . . ? Al2 C35 H35A 107.8 . . ? C36 C35 H35B 107.8 . . ? Al2 C35 H35B 107.8 . . ? H35A C35 H35B 107.1 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C32 Al1 N2 C6 118.3(2) . . . . ? C31 Al1 N2 C6 -104.7(3) . . . . ? N1 Al1 N2 C6 5.4(2) . . . . ? C32 Al1 N2 C7 -75.1(4) . . . . ? C31 Al1 N2 C7 62.0(4) . . . . ? N1 Al1 N2 C7 172.0(3) . . . . ? C35 Al2 N3 C6 150.7(3) . . . . ? Cl1 Al2 N3 C6 -81.2(3) . . . . ? Cl2 Al2 N3 C6 35.4(3) . . . . ? C35 Al2 N3 C12 -10.8(3) . . . . ? Cl1 Al2 N3 C12 117.2(2) . . . . ? Cl2 Al2 N3 C12 -126.2(2) . . . . ? N2 Al1 N1 C1 175.6(3) . . . . ? C32 Al1 N1 C1 61.5(3) . . . . ? C31 Al1 N1 C1 -77.2(3) . . . . ? N2 Al1 N1 C5 1.1(2) . . . . ? C32 Al1 N1 C5 -113.0(2) . . . . ? C31 Al1 N1 C5 108.3(2) . . . . ? C1 N1 C5 C4 -3.8(4) . . . . ? Al1 N1 C5 C4 171.0(2) . . . . ? C1 N1 C5 C6 178.5(3) . . . . ? Al1 N1 C5 C6 -6.7(3) . . . . ? C6 N2 C7 C12 0.7(3) . . . . ? Al1 N2 C7 C12 -166.8(3) . . . . ? C6 N2 C7 C8 -179.7(3) . . . . ? Al1 N2 C7 C8 12.9(6) . . . . ? N2 C7 C12 C11 -178.5(3) . . . . ? C8 C7 C12 C11 1.8(5) . . . . ? N2 C7 C12 N3 0.4(3) . . . . ? C8 C7 C12 N3 -179.3(3) . . . . ? C6 N3 C12 C7 -1.3(3) . . . . ? Al2 N3 C12 C7 164.3(2) . . . . ? C6 N3 C12 C11 177.5(3) . . . . ? Al2 N3 C12 C11 -16.9(5) . . . . ? N1 C5 C4 C3 4.1(5) . . . . ? C6 C5 C4 C3 -178.6(3) . . . . ? C5 C4 C3 C2 -1.1(5) . . . . ? C7 N2 C6 N3 -1.6(3) . . . . ? Al1 N2 C6 N3 169.3(2) . . . . ? C7 N2 C6 C5 178.5(2) . . . . ? Al1 N2 C6 C5 -10.6(3) . . . . ? C12 N3 C6 N2 1.9(3) . . . . ? Al2 N3 C6 N2 -162.3(2) . . . . ? C12 N3 C6 C5 -178.3(3) . . . . ? Al2 N3 C6 C5 17.6(5) . . . . ? N1 C5 C6 N2 11.4(4) . . . . ? C4 C5 C6 N2 -166.1(3) . . . . ? N1 C5 C6 N3 -168.5(3) . . . . ? C4 C5 C6 N3 14.0(5) . . . . ? C4 C3 C2 C1 -2.1(5) . . . . ? C7 C12 C11 C10 -1.0(5) . . . . ? N3 C12 C11 C10 -179.6(3) . . . . ? C5 N1 C1 C2 0.5(5) . . . . ? Al1 N1 C1 C2 -173.6(2) . . . . ? C5 N1 C1 C13 179.0(3) . . . . ? Al1 N1 C1 C13 4.8(4) . . . . ? C3 C2 C1 N1 2.4(5) . . . . ? C3 C2 C1 C13 -176.0(3) . . . . ? C10 C9 C8 C7 -0.3(5) . . . . ? N2 C7 C8 C9 179.3(3) . . . . ? C12 C7 C8 C9 -1.1(5) . . . . ? C12 C11 C10 C9 -0.5(5) . . . . ? C8 C9 C10 C11 1.1(5) . . . . ? N2 Al1 C31 C33 42.8(6) . . . . ? C32 Al1 C31 C33 177.6(6) . . . . ? N1 Al1 C31 C33 -46.4(6) . . . . ? N2 Al1 C32 C34 60.2(4) . . . . ? C31 Al1 C32 C34 -72.0(4) . . . . ? N1 Al1 C32 C34 153.1(4) . . . . ? N3 Al2 C35 C36 103.8(5) . . . . ? Cl1 Al2 C35 C36 -18.9(6) . . . . ? Cl2 Al2 C35 C36 -143.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.336 _refine_diff_density_min -0.908 _refine_diff_density_rms 0.170 #==End data_1a _database_code_depnum_ccdc_archive 'CCDC 777735' #TrackingRef '- CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H37 Al2 N3' _chemical_formula_weight 457.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 15.890(3) _cell_length_b 7.4374(15) _cell_length_c 22.421(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.00(3) _cell_angle_gamma 90.00 _cell_volume 2609.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.46 _cell_measurement_theta_max 27.47 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 0.130 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.9619 _exptl_absorpt_correction_T_max 0.9871 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 20662 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5936 _reflns_number_gt 5040 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0730P)^2^+2.9160P] 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 5936 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.1270 _refine_ls_R_factor_gt 0.1071 _refine_ls_wR_factor_ref 0.2392 _refine_ls_wR_factor_gt 0.2244 _refine_ls_goodness_of_fit_ref 1.305 _refine_ls_restrained_S_all 1.305 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.70583(7) 0.45859(15) 0.04406(5) 0.0296(3) Uani 1 1 d . . . N1 N 0.77197(19) 0.6369(4) 0.00357(14) 0.0304(7) Uani 1 1 d . . . C1 C 0.7418(3) 0.6739(6) -0.05515(18) 0.0375(9) Uani 1 1 d . . . C44 C 1.1893(11) 0.2961(16) 0.2582(11) 0.105(7) Uani 0.76(4) 1 d P A 1 H44A H 1.2125 0.1742 0.2650 0.158 Uiso 0.76(4) 1 calc PR A 1 H44B H 1.1855 0.3519 0.2972 0.158 Uiso 0.76(4) 1 calc PR A 1 H44C H 1.2270 0.3679 0.2374 0.158 Uiso 0.76(4) 1 calc PR A 1 C44' C 1.149(3) 0.274(5) 0.2857(14) 0.071(11) Uani 0.24(4) 1 d P A 2 H44D H 1.1749 0.1551 0.2928 0.107 Uiso 0.24(4) 1 calc PR A 2 H44E H 1.1077 0.2928 0.3131 0.107 Uiso 0.24(4) 1 calc PR A 2 H44F H 1.1934 0.3667 0.2932 0.107 Uiso 0.24(4) 1 calc PR A 2 Al2 Al 1.04564(7) 0.52533(17) 0.20230(5) 0.0344(3) Uani 1 1 d . A . N2 N 0.79051(18) 0.4410(4) 0.11524(13) 0.0285(7) Uani 1 1 d . . . C2 C 0.7713(3) 0.8180(6) -0.0854(2) 0.0443(10) Uani 1 1 d . . . H2A H 0.7505 0.8366 -0.1273 0.053 Uiso 1 1 calc R . . N3 N 0.91881(19) 0.4788(4) 0.17591(13) 0.0293(7) Uani 1 1 d . . . C3 C 0.8302(3) 0.9318(6) -0.0544(2) 0.0425(10) Uani 1 1 d . . . H3A H 0.8503 1.0309 -0.0747 0.051 Uiso 1 1 calc R . . C4 C 0.8616(2) 0.9031(6) 0.00781(19) 0.0362(9) Uani 1 1 d . . . C5 C 0.9178(3) 1.0281(6) 0.0422(2) 0.0433(11) Uani 1 1 d . . . H5A H 0.9369 1.1303 0.0229 0.052 Uiso 1 1 calc R . . C6 C 0.9442(3) 1.0026(5) 0.1022(2) 0.0413(10) Uani 1 1 d . . . H6A H 0.9774 1.0918 0.1259 0.050 Uiso 1 1 calc R . . C7 C 0.9222(2) 0.8431(5) 0.12949(19) 0.0354(9) Uani 1 1 d . . . H7A H 0.9425 0.8252 0.1715 0.043 Uiso 1 1 calc R . . C8 C 0.8723(2) 0.7120(5) 0.09762(17) 0.0313(8) Uani 1 1 d . . . C9 C 0.8343(2) 0.7474(5) 0.03553(18) 0.0304(8) Uani 1 1 d . . . C10 C 0.6729(3) 0.5562(7) -0.0891(2) 0.0504(12) Uani 1 1 d . . . H10A H 0.6589 0.4611 -0.0622 0.076 Uiso 1 1 calc R . . H10B H 0.6931 0.5019 -0.1239 0.076 Uiso 1 1 calc R . . H10C H 0.6219 0.6287 -0.1033 0.076 Uiso 1 1 calc R . . C11 C 0.8613(2) 0.5420(5) 0.12912(16) 0.0277(8) Uani 1 1 d . . . C12 C 0.7996(2) 0.3035(5) 0.15825(16) 0.0299(8) Uani 1 1 d . . . C13 C 0.7442(3) 0.1668(5) 0.16739(18) 0.0359(9) Uani 1 1 d . . . H13A H 0.6904 0.1525 0.1417 0.043 Uiso 1 1 calc R . . C14 C 0.7701(3) 0.0519(6) 0.21533(19) 0.0407(10) Uani 1 1 d . . . H14A H 0.7343 -0.0452 0.2223 0.049 Uiso 1 1 calc R . . C15 C 0.8491(3) 0.0767(6) 0.25407(19) 0.0425(10) Uani 1 1 d . . . H15A H 0.8652 -0.0037 0.2870 0.051 Uiso 1 1 calc R . . C16 C 0.9036(3) 0.2143(6) 0.24539(18) 0.0369(9) Uani 1 1 d . . . H16A H 0.9563 0.2314 0.2722 0.044 Uiso 1 1 calc R . . C17 C 0.8792(2) 0.3275(5) 0.19612(16) 0.0296(8) Uani 1 1 d . . . C31 C 0.6056(2) 0.5879(6) 0.06133(19) 0.0367(9) Uani 1 1 d . . . H31A H 0.5647 0.6048 0.0230 0.044 Uiso 1 1 calc R . . H31B H 0.5770 0.5137 0.0886 0.044 Uiso 1 1 calc R . . C32 C 0.6977(3) 0.2204(5) 0.00548(19) 0.0387(10) Uani 1 1 d . . . H32A H 0.7332 0.2219 -0.0267 0.046 Uiso 1 1 calc R . . H32B H 0.7234 0.1315 0.0362 0.046 Uiso 1 1 calc R . . C33 C 1.0544(3) 0.6865(7) 0.2741(2) 0.0483(11) Uani 1 1 d . . . H33A H 1.1147 0.6872 0.2949 0.058 Uiso 1 1 calc R . . H33B H 1.0403 0.8103 0.2594 0.058 Uiso 1 1 calc R . . C35 C 1.0950(3) 0.6301(6) 0.13448(19) 0.0413(10) Uani 1 1 d . . . H35A H 1.0812 0.7600 0.1323 0.050 Uiso 1 1 calc R . . H35B H 1.1580 0.6197 0.1449 0.050 Uiso 1 1 calc R . . C41 C 0.6272(3) 0.7715(6) 0.0907(2) 0.0444(10) Uani 1 1 d . . . H41A H 0.5747 0.8295 0.0983 0.067 Uiso 1 1 calc R . . H41B H 0.6541 0.8470 0.0635 0.067 Uiso 1 1 calc R . . H41C H 0.6666 0.7558 0.1291 0.067 Uiso 1 1 calc R . . C42 C 0.6080(3) 0.1528(7) -0.0227(2) 0.0590(14) Uani 1 1 d . . . H42A H 0.6126 0.0334 -0.0404 0.088 Uiso 1 1 calc R . . H42B H 0.5821 0.2364 -0.0545 0.088 Uiso 1 1 calc R . . H42C H 0.5723 0.1455 0.0087 0.088 Uiso 1 1 calc R . . C43 C 0.9992(4) 0.6421(10) 0.3202(3) 0.081(2) Uani 1 1 d . . . H43A H 1.0088 0.7308 0.3530 0.121 Uiso 1 1 calc R . . H43B H 1.0138 0.5220 0.3368 0.121 Uiso 1 1 calc R . . H43C H 0.9390 0.6444 0.3008 0.121 Uiso 1 1 calc R . . C45 C 1.0672(3) 0.5508(7) 0.0713(2) 0.0502(12) Uani 1 1 d . . . H45A H 1.0959 0.6150 0.0423 0.075 Uiso 1 1 calc R . . H45B H 1.0052 0.5633 0.0593 0.075 Uiso 1 1 calc R . . H45C H 1.0827 0.4232 0.0717 0.075 Uiso 1 1 calc R . . C34 C 1.1028(3) 0.2873(7) 0.2204(2) 0.0534(12) Uani 1 1 d . . . H34A H 1.0660 0.2110 0.2413 0.064 Uiso 1 1 calc R A 1 H34B H 1.1075 0.2278 0.1816 0.064 Uiso 1 1 calc R A 1 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 0.0247(5) 0.0299(6) 0.0320(6) -0.0026(5) -0.0008(4) 0.0026(4) N1 0.0234(15) 0.0353(17) 0.0324(18) 0.0017(14) 0.0043(12) 0.0080(13) C1 0.035(2) 0.042(2) 0.034(2) 0.0043(18) 0.0022(16) 0.0114(18) C44 0.067(8) 0.106(8) 0.121(14) -0.015(7) -0.046(9) 0.036(6) C44' 0.06(2) 0.088(19) 0.066(18) 0.015(14) 0.007(14) 0.048(16) Al2 0.0261(6) 0.0456(7) 0.0295(7) -0.0021(5) -0.0009(5) -0.0032(5) N2 0.0247(15) 0.0304(16) 0.0293(17) -0.0021(13) 0.0015(12) -0.0031(12) C2 0.048(3) 0.047(3) 0.037(2) 0.011(2) 0.0061(19) 0.012(2) N3 0.0268(15) 0.0354(17) 0.0244(16) -0.0005(13) 0.0007(12) 0.0001(13) C3 0.043(2) 0.039(2) 0.049(3) 0.014(2) 0.018(2) 0.0110(19) C4 0.0282(19) 0.035(2) 0.048(2) 0.0073(18) 0.0149(17) 0.0079(16) C5 0.039(2) 0.030(2) 0.065(3) 0.006(2) 0.021(2) 0.0007(18) C6 0.033(2) 0.032(2) 0.059(3) -0.0062(19) 0.0091(19) -0.0021(17) C7 0.0275(18) 0.036(2) 0.043(2) -0.0057(17) 0.0074(16) 0.0011(16) C8 0.0244(17) 0.036(2) 0.035(2) -0.0033(16) 0.0089(15) 0.0008(15) C9 0.0254(18) 0.0290(19) 0.038(2) 0.0004(16) 0.0086(15) 0.0071(15) C10 0.045(3) 0.064(3) 0.036(2) 0.007(2) -0.0086(19) 0.001(2) C11 0.0211(16) 0.0318(19) 0.0300(19) -0.0017(15) 0.0041(14) 0.0031(14) C12 0.0276(18) 0.033(2) 0.029(2) -0.0045(15) 0.0031(14) 0.0006(15) C13 0.032(2) 0.039(2) 0.037(2) -0.0047(17) 0.0062(16) -0.0068(17) C14 0.050(2) 0.036(2) 0.038(2) 0.0010(18) 0.0120(19) -0.0069(19) C15 0.053(3) 0.042(2) 0.032(2) 0.0099(18) 0.0043(19) -0.001(2) C16 0.036(2) 0.044(2) 0.029(2) 0.0013(17) 0.0012(16) 0.0010(18) C17 0.0288(18) 0.034(2) 0.0257(19) -0.0013(15) 0.0035(14) -0.0018(15) C31 0.0280(19) 0.038(2) 0.043(2) -0.0033(18) 0.0035(16) 0.0050(16) C32 0.039(2) 0.033(2) 0.040(2) -0.0056(17) -0.0052(17) 0.0096(17) C33 0.037(2) 0.064(3) 0.041(3) -0.006(2) 0.0011(18) -0.011(2) C35 0.028(2) 0.051(3) 0.046(3) 0.003(2) 0.0069(17) -0.0024(18) C41 0.042(2) 0.042(2) 0.051(3) -0.006(2) 0.010(2) 0.0059(19) C42 0.052(3) 0.041(3) 0.073(4) -0.008(2) -0.020(2) -0.002(2) C43 0.084(4) 0.105(5) 0.061(4) -0.036(3) 0.034(3) -0.038(4) C45 0.045(2) 0.069(3) 0.037(2) 0.005(2) 0.0072(19) 0.019(2) C34 0.040(2) 0.060(3) 0.058(3) 0.014(2) 0.004(2) 0.008(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 Al1 N2 1.905(3) . ? Al1 C31 1.956(4) . ? Al1 C32 1.966(4) . ? Al1 N1 2.005(3) . ? N1 C1 1.349(5) . ? N1 C9 1.386(5) . ? C1 C2 1.392(6) . ? C1 C10 1.501(6) . ? C44 C34 1.486(10) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C44' C34 1.52(3) . ? C44' H44D 0.9800 . ? C44' H44E 0.9800 . ? C44' H44F 0.9800 . ? Al2 C35 1.987(4) . ? Al2 C33 1.993(5) . ? Al2 C34 1.999(5) . ? Al2 N3 2.029(3) . ? N2 C11 1.343(4) . ? N2 C12 1.395(5) . ? C2 C3 1.359(6) . ? C2 H2A 0.9500 . ? N3 C11 1.350(4) . ? N3 C17 1.403(5) . ? C3 C4 1.414(6) . ? C3 H3A 0.9500 . ? C4 C9 1.418(5) . ? C4 C5 1.420(6) . ? C5 C6 1.352(6) . ? C5 H5A 0.9500 . ? C6 C7 1.406(6) . ? C6 H6A 0.9500 . ? C7 C8 1.376(5) . ? C7 H7A 0.9500 . ? C8 C9 1.443(5) . ? C8 C11 1.473(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C12 C13 1.384(5) . ? C12 C17 1.407(5) . ? C13 C14 1.379(6) . ? C13 H13A 0.9500 . ? C14 C15 1.409(6) . ? C14 H14A 0.9500 . ? C15 C16 1.377(6) . ? C15 H15A 0.9500 . ? C16 C17 1.389(5) . ? C16 H16A 0.9500 . ? C31 C41 1.529(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C42 1.539(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C43 1.503(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C35 C45 1.528(6) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Al1 C31 110.43(16) . . ? N2 Al1 C32 106.83(15) . . ? C31 Al1 C32 122.45(18) . . ? N2 Al1 N1 94.31(13) . . ? C31 Al1 N1 105.86(16) . . ? C32 Al1 N1 113.37(17) . . ? C1 N1 C9 119.0(3) . . ? C1 N1 Al1 116.8(3) . . ? C9 N1 Al1 122.8(3) . . ? N1 C1 C2 122.7(4) . . ? N1 C1 C10 118.7(4) . . ? C2 C1 C10 118.7(4) . . ? C34 C44 H44A 109.5 . . ? C34 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C34 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C34 C44' H44D 109.5 . . ? C34 C44' H44E 109.5 . . ? H44D C44' H44E 109.5 . . ? C34 C44' H44F 109.5 . . ? H44D C44' H44F 109.5 . . ? H44E C44' H44F 109.5 . . ? C35 Al2 C33 113.6(2) . . ? C35 Al2 C34 106.1(2) . . ? C33 Al2 C34 113.8(2) . . ? C35 Al2 N3 110.35(15) . . ? C33 Al2 N3 105.33(16) . . ? C34 Al2 N3 107.55(18) . . ? C11 N2 C12 105.5(3) . . ? C11 N2 Al1 126.6(3) . . ? C12 N2 Al1 127.1(2) . . ? C3 C2 C1 119.4(4) . . ? C3 C2 H2A 120.3 . . ? C1 C2 H2A 120.3 . . ? C11 N3 C17 104.4(3) . . ? C11 N3 Al2 132.2(3) . . ? C17 N3 Al2 121.4(2) . . ? C2 C3 C4 120.3(4) . . ? C2 C3 H3A 119.9 . . ? C4 C3 H3A 119.9 . . ? C3 C4 C9 118.2(4) . . ? C3 C4 C5 121.2(4) . . ? C9 C4 C5 120.6(4) . . ? C6 C5 C4 120.4(4) . . ? C6 C5 H5A 119.8 . . ? C4 C5 H5A 119.8 . . ? C5 C6 C7 119.6(4) . . ? C5 C6 H6A 120.2 . . ? C7 C6 H6A 120.2 . . ? C8 C7 C6 122.5(4) . . ? C8 C7 H7A 118.8 . . ? C6 C7 H7A 118.8 . . ? C7 C8 C9 118.6(4) . . ? C7 C8 C11 117.7(4) . . ? C9 C8 C11 123.7(3) . . ? N1 C9 C4 120.2(4) . . ? N1 C9 C8 122.2(3) . . ? C4 C9 C8 117.6(4) . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 N3 114.3(3) . . ? N2 C11 C8 122.2(3) . . ? N3 C11 C8 123.4(3) . . ? C13 C12 N2 130.5(3) . . ? C13 C12 C17 122.1(4) . . ? N2 C12 C17 107.4(3) . . ? C14 C13 C12 117.3(4) . . ? C14 C13 H13A 121.3 . . ? C12 C13 H13A 121.3 . . ? C13 C14 C15 120.9(4) . . ? C13 C14 H14A 119.5 . . ? C15 C14 H14A 119.5 . . ? C16 C15 C14 121.7(4) . . ? C16 C15 H15A 119.2 . . ? C14 C15 H15A 119.2 . . ? C15 C16 C17 117.8(4) . . ? C15 C16 H16A 121.1 . . ? C17 C16 H16A 121.1 . . ? C16 C17 N3 131.6(3) . . ? C16 C17 C12 120.1(4) . . ? N3 C17 C12 108.3(3) . . ? C41 C31 Al1 113.2(3) . . ? C41 C31 H31A 108.9 . . ? Al1 C31 H31A 108.9 . . ? C41 C31 H31B 108.9 . . ? Al1 C31 H31B 108.9 . . ? H31A C31 H31B 107.7 . . ? C42 C32 Al1 117.4(3) . . ? C42 C32 H32A 107.9 . . ? Al1 C32 H32A 107.9 . . ? C42 C32 H32B 107.9 . . ? Al1 C32 H32B 107.9 . . ? H32A C32 H32B 107.2 . . ? C43 C33 Al2 117.1(3) . . ? C43 C33 H33A 108.0 . . ? Al2 C33 H33A 108.0 . . ? C43 C33 H33B 108.0 . . ? Al2 C33 H33B 108.0 . . ? H33A C33 H33B 107.3 . . ? C45 C35 Al2 118.0(3) . . ? C45 C35 H35A 107.8 . . ? Al2 C35 H35A 107.8 . . ? C45 C35 H35B 107.8 . . ? Al2 C35 H35B 107.8 . . ? H35A C35 H35B 107.1 . . ? C31 C41 H41A 109.5 . . ? C31 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C31 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C32 C42 H42A 109.5 . . ? C32 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C32 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C33 C43 H43A 109.5 . . ? C33 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C33 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C35 C45 H45A 109.5 . . ? C35 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C35 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C34 C44' 38.0(12) . . ? C44 C34 Al2 114.8(5) . . ? C44' C34 Al2 112.1(11) . . ? C44 C34 H34A 108.6 . . ? C44' C34 H34A 74.4 . . ? Al2 C34 H34A 108.6 . . ? C44 C34 H34B 108.6 . . ? C44' C34 H34B 136.1 . . ? Al2 C34 H34B 108.6 . . ? H34A C34 H34B 107.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Al1 N1 C1 170.4(3) . . . . ? C31 Al1 N1 C1 -76.9(3) . . . . ? C32 Al1 N1 C1 60.0(3) . . . . ? N2 Al1 N1 C9 -23.3(3) . . . . ? C31 Al1 N1 C9 89.4(3) . . . . ? C32 Al1 N1 C9 -133.7(3) . . . . ? C9 N1 C1 C2 0.7(6) . . . . ? Al1 N1 C1 C2 167.5(3) . . . . ? C9 N1 C1 C10 -178.6(4) . . . . ? Al1 N1 C1 C10 -11.8(5) . . . . ? C31 Al1 N2 C11 -101.4(3) . . . . ? C32 Al1 N2 C11 123.3(3) . . . . ? N1 Al1 N2 C11 7.3(3) . . . . ? C31 Al1 N2 C12 90.2(3) . . . . ? C32 Al1 N2 C12 -45.1(3) . . . . ? N1 Al1 N2 C12 -161.1(3) . . . . ? N1 C1 C2 C3 -3.0(6) . . . . ? C10 C1 C2 C3 176.3(4) . . . . ? C35 Al2 N3 C11 -18.1(4) . . . . ? C33 Al2 N3 C11 104.9(4) . . . . ? C34 Al2 N3 C11 -133.4(4) . . . . ? C35 Al2 N3 C17 143.1(3) . . . . ? C33 Al2 N3 C17 -93.9(3) . . . . ? C34 Al2 N3 C17 27.8(3) . . . . ? C1 C2 C3 C4 0.5(6) . . . . ? C2 C3 C4 C9 4.0(6) . . . . ? C2 C3 C4 C5 -174.8(4) . . . . ? C3 C4 C5 C6 177.0(4) . . . . ? C9 C4 C5 C6 -1.7(6) . . . . ? C4 C5 C6 C7 5.8(6) . . . . ? C5 C6 C7 C8 -1.8(6) . . . . ? C6 C7 C8 C9 -6.4(6) . . . . ? C6 C7 C8 C11 173.3(3) . . . . ? C1 N1 C9 C4 4.0(5) . . . . ? Al1 N1 C9 C4 -162.0(3) . . . . ? C1 N1 C9 C8 -177.2(3) . . . . ? Al1 N1 C9 C8 16.7(5) . . . . ? C3 C4 C9 N1 -6.2(5) . . . . ? C5 C4 C9 N1 172.5(3) . . . . ? C3 C4 C9 C8 174.9(3) . . . . ? C5 C4 C9 C8 -6.3(5) . . . . ? C7 C8 C9 N1 -168.7(3) . . . . ? C11 C8 C9 N1 11.7(5) . . . . ? C7 C8 C9 C4 10.1(5) . . . . ? C11 C8 C9 C4 -169.5(3) . . . . ? C12 N2 C11 N3 3.1(4) . . . . ? Al1 N2 C11 N3 -167.3(2) . . . . ? C12 N2 C11 C8 -173.9(3) . . . . ? Al1 N2 C11 C8 15.7(5) . . . . ? C17 N3 C11 N2 -3.3(4) . . . . ? Al2 N3 C11 N2 160.2(3) . . . . ? C17 N3 C11 C8 173.7(3) . . . . ? Al2 N3 C11 C8 -22.8(5) . . . . ? C7 C8 C11 N2 150.6(4) . . . . ? C9 C8 C11 N2 -29.8(5) . . . . ? C7 C8 C11 N3 -26.2(5) . . . . ? C9 C8 C11 N3 153.5(3) . . . . ? C11 N2 C12 C13 176.5(4) . . . . ? Al1 N2 C12 C13 -13.2(6) . . . . ? C11 N2 C12 C17 -1.5(4) . . . . ? Al1 N2 C12 C17 168.8(3) . . . . ? N2 C12 C13 C14 -178.2(4) . . . . ? C17 C12 C13 C14 -0.4(6) . . . . ? C12 C13 C14 C15 1.5(6) . . . . ? C13 C14 C15 C16 -0.7(7) . . . . ? C14 C15 C16 C17 -1.3(6) . . . . ? C15 C16 C17 N3 178.6(4) . . . . ? C15 C16 C17 C12 2.3(6) . . . . ? C11 N3 C17 C16 -174.6(4) . . . . ? Al2 N3 C17 C16 19.7(6) . . . . ? C11 N3 C17 C12 2.1(4) . . . . ? Al2 N3 C17 C12 -163.6(2) . . . . ? C13 C12 C17 C16 -1.5(6) . . . . ? N2 C12 C17 C16 176.8(3) . . . . ? C13 C12 C17 N3 -178.6(3) . . . . ? N2 C12 C17 N3 -0.4(4) . . . . ? N2 Al1 C31 C41 53.6(3) . . . . ? C32 Al1 C31 C41 -179.3(3) . . . . ? N1 Al1 C31 C41 -47.3(3) . . . . ? N2 Al1 C32 C42 140.7(3) . . . . ? C31 Al1 C32 C42 12.0(4) . . . . ? N1 Al1 C32 C42 -116.8(4) . . . . ? C35 Al2 C33 C43 164.1(4) . . . . ? C34 Al2 C33 C43 -74.4(5) . . . . ? N3 Al2 C33 C43 43.2(5) . . . . ? C33 Al2 C35 C45 -160.4(3) . . . . ? C34 Al2 C35 C45 73.9(4) . . . . ? N3 Al2 C35 C45 -42.3(4) . . . . ? C35 Al2 C34 C44 80.4(13) . . . . ? C33 Al2 C34 C44 -45.2(13) . . . . ? N3 Al2 C34 C44 -161.5(13) . . . . ? C35 Al2 C34 C44' 122(2) . . . . ? C33 Al2 C34 C44' -4(2) . . . . ? N3 Al2 C34 C44' -120(2) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.507 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.120 #==End