# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _publ_section_title ;Structural Insights into Mono-Amido Tris-Alkyl Potassium Aluminates ; _publ_contact_author_name R.E.Mulvey _publ_contact_author_email R.E.MULVEY@STRATH.AC.UK loop_ _publ_author_name R.E.Mulvey 'Ben Conway' 'Pablo Garcia-Alvarez' 'A.R. Kennedy' 'Jan Klett' 'Stuart Robertson' # Attachment '- all3.cif' data_jkben8 _database_code_depnum_ccdc_archive 'CCDC 771326' #TrackingRef '- all3.cif' ################################################################### ################## COMPOUND 6 #################################### ################################################################## _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H68 Al K N4' _chemical_formula_weight 550.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna21 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' _cell_length_a 16.505(3) _cell_length_b 11.562(3) _cell_length_c 18.948(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3616.0(14) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 1361 _cell_measurement_theta_min 3.50 _cell_measurement_theta_max 74.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.012 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 1.665 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.77546 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini S' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8896 _diffrn_reflns_av_R_equivalents 0.0896 _diffrn_reflns_av_sigmaI/netI 0.1379 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 6.59 _diffrn_reflns_theta_max 64.98 _reflns_number_total 4713 _reflns_number_gt 2057 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1451P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 4713 _refine_ls_number_parameters 337 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.1589 _refine_ls_R_factor_gt 0.0783 _refine_ls_wR_factor_ref 0.2606 _refine_ls_wR_factor_gt 0.1992 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.940 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group K1 K 0.32988(13) 0.59590(15) 0.09182(11) 0.0490(6) Uani 1 1 d . . . Al1 Al 0.32951(18) 0.8812(2) 0.19546(15) 0.0443(8) Uani 1 1 d . A . C11 C 0.3210(6) 0.8647(7) 0.0890(6) 0.048(2) Uani 1 1 d . A . H11A H 0.3633 0.8090 0.0744 0.058 Uiso 1 1 calc R . . H11B H 0.2681 0.8276 0.0791 0.058 Uiso 1 1 calc R . . C12 C 0.3278(6) 0.9688(9) 0.0399(6) 0.051(3) Uani 1 1 d . . . H12A H 0.3058 1.0377 0.0654 0.061 Uiso 1 1 calc R A . C13 C 0.2793(7) 0.9546(10) -0.0295(6) 0.066(3) Uani 1 1 d . . . H13A H 0.2212 0.9598 -0.0193 0.098 Uiso 1 1 calc R . . H13B H 0.2914 0.8790 -0.0504 0.098 Uiso 1 1 calc R . . H13C H 0.2946 1.0159 -0.0626 0.098 Uiso 1 1 calc R . . C14 C 0.4169(6) 0.9946(8) 0.0208(6) 0.055(3) Uani 1 1 d . . . H14A H 0.4195 1.0642 -0.0086 0.083 Uiso 1 1 calc R . . H14B H 0.4396 0.9289 -0.0053 0.083 Uiso 1 1 calc R . . H14C H 0.4482 1.0069 0.0641 0.083 Uiso 1 1 calc R . . C21 C 0.2379(6) 0.9760(8) 0.2396(5) 0.047(3) Uani 1 1 d . . . H21A H 0.1899 0.9252 0.2441 0.056 Uiso 1 1 calc R A . H21B H 0.2547 0.9979 0.2880 0.056 Uiso 1 1 calc R . . C22 C 0.2116(6) 1.0858(8) 0.2013(6) 0.050(3) Uani 1 1 d . . . H22A H 0.2608 1.1218 0.1797 0.060 Uiso 1 1 calc R . . C23 C 0.1519(7) 1.0556(9) 0.1412(7) 0.071(4) Uani 1 1 d . . . H23A H 0.1756 0.9951 0.1113 0.106 Uiso 1 1 calc R A . H23B H 0.1416 1.1247 0.1126 0.106 Uiso 1 1 calc R . . H23C H 0.1009 1.0278 0.1614 0.106 Uiso 1 1 calc R . . C24 C 0.1716(7) 1.1768(9) 0.2504(6) 0.071(4) Uani 1 1 d . . . H24A H 0.2095 1.1979 0.2881 0.107 Uiso 1 1 calc R A . H24B H 0.1223 1.1440 0.2713 0.107 Uiso 1 1 calc R . . H24C H 0.1576 1.2458 0.2230 0.107 Uiso 1 1 calc R . . C31 C 0.4235(7) 0.9911(8) 0.2146(5) 0.056(3) Uani 1 1 d . . . H31A H 0.4736 0.9488 0.2020 0.068 Uiso 1 1 calc R A . H31B H 0.4183 1.0553 0.1804 0.068 Uiso 1 1 calc R . . C32 C 0.4393(7) 1.0483(9) 0.2889(6) 0.055(3) Uani 1 1 d . . . H32A H 0.4050 1.0062 0.3240 0.066 Uiso 1 1 calc R . . C33 C 0.5294(7) 1.0340(11) 0.3127(6) 0.072(4) Uani 1 1 d . . . H33A H 0.5348 1.0575 0.3622 0.109 Uiso 1 1 calc R A . H33B H 0.5642 1.0827 0.2832 0.109 Uiso 1 1 calc R . . H33C H 0.5456 0.9529 0.3077 0.109 Uiso 1 1 calc R . . C34 C 0.4139(7) 1.1732(10) 0.2905(7) 0.081(4) Uani 1 1 d . . . H34A H 0.3568 1.1794 0.2769 0.121 Uiso 1 1 calc R A . H34B H 0.4473 1.2177 0.2574 0.121 Uiso 1 1 calc R . . H34C H 0.4211 1.2040 0.3383 0.121 Uiso 1 1 calc R . . N41 N 0.3353(5) 0.7177(6) 0.2287(4) 0.046(2) Uani 1 1 d . A . C42 C 0.2607(6) 0.6667(8) 0.2598(5) 0.043(3) Uani 1 1 d . A . C421 C 0.1895(6) 0.6895(8) 0.2083(5) 0.050(3) Uani 1 1 d . . . H42A H 0.1991 0.6479 0.1640 0.076 Uiso 1 1 calc R A . H42B H 0.1856 0.7726 0.1987 0.076 Uiso 1 1 calc R . . H42C H 0.1388 0.6624 0.2295 0.076 Uiso 1 1 calc R . . C422 C 0.2350(7) 0.7180(8) 0.3317(5) 0.058(3) Uani 1 1 d . . . H42D H 0.2731 0.6930 0.3683 0.088 Uiso 1 1 calc R A . H42E H 0.1804 0.6909 0.3436 0.088 Uiso 1 1 calc R . . H42F H 0.2350 0.8027 0.3288 0.088 Uiso 1 1 calc R . . C43 C 0.2661(7) 0.5358(8) 0.2673(6) 0.056(3) Uani 1 1 d . . . H43A H 0.2649 0.5004 0.2198 0.067 Uiso 1 1 calc R A . H43B H 0.2180 0.5078 0.2935 0.067 Uiso 1 1 calc R . . C44 C 0.3430(6) 0.4957(8) 0.3060(6) 0.055(3) Uani 1 1 d . . . H44A H 0.3432 0.5252 0.3550 0.066 Uiso 1 1 calc R . . H44B H 0.3453 0.4102 0.3074 0.066 Uiso 1 1 calc R . . C45 C 0.4154(6) 0.5438(9) 0.2651(6) 0.054(3) Uani 1 1 d . . . H45A H 0.4658 0.5221 0.2902 0.065 Uiso 1 1 calc R A . H45B H 0.4170 0.5070 0.2180 0.065 Uiso 1 1 calc R . . C46 C 0.4139(7) 0.6749(8) 0.2558(6) 0.050(3) Uani 1 1 d . A . C461 C 0.4818(6) 0.7012(9) 0.2013(6) 0.062(3) Uani 1 1 d . . . H46A H 0.4695 0.6621 0.1567 0.093 Uiso 1 1 calc R A . H46B H 0.5338 0.6733 0.2196 0.093 Uiso 1 1 calc R . . H46C H 0.4849 0.7848 0.1934 0.093 Uiso 1 1 calc R . . C462 C 0.4417(6) 0.7310(8) 0.3263(5) 0.056(3) Uani 1 1 d . . . H46D H 0.4043 0.7089 0.3641 0.085 Uiso 1 1 calc R A . H46E H 0.4421 0.8154 0.3213 0.085 Uiso 1 1 calc R . . H46F H 0.4964 0.7041 0.3379 0.085 Uiso 1 1 calc R . . C512 C 0.4197(7) 0.6224(10) -0.0732(6) 0.064(3) Uani 1 1 d . . . H51D H 0.3971 0.6999 -0.0661 0.097 Uiso 1 1 calc R A . H51E H 0.3760 0.5684 -0.0849 0.097 Uiso 1 1 calc R . . H51F H 0.4590 0.6244 -0.1120 0.097 Uiso 1 1 calc R . . N51 N 0.4606(5) 0.5839(7) -0.0077(5) 0.057(2) Uani 1 1 d . . . N52 N 0.3677(5) 0.3722(7) 0.0406(5) 0.052(2) Uani 1 1 d DU A . C513 C 0.4872(7) 0.4636(9) -0.0135(6) 0.065(3) Uani 1 1 d . . . H51G H 0.5195 0.4447 0.0290 0.078 Uiso 1 1 calc R A . H51H H 0.5239 0.4575 -0.0547 0.078 Uiso 1 1 calc R . . C521 C 0.4223(6) 0.3737(8) -0.0213(6) 0.058(3) Uani 1 1 d . A . H52D H 0.3904 0.3892 -0.0645 0.070 Uiso 1 1 d R . . H52E H 0.4479 0.2967 -0.0263 0.070 Uiso 1 1 d R . . C511 C 0.5321(7) 0.6584(9) 0.0055(6) 0.070(4) Uani 1 1 d . . . H51A H 0.5702 0.6489 -0.0338 0.105 Uiso 1 1 d R A . H51B H 0.5583 0.6346 0.0495 0.105 Uiso 1 1 d R . . H51C H 0.5158 0.7397 0.0089 0.105 Uiso 1 1 d R . . N53 N 0.1942(5) 0.4721(8) 0.0372(6) 0.065(3) Uani 1 1 d U A . C523 C 0.4064(7) 0.3165(9) 0.1022(6) 0.065(3) Uani 1 1 d . . . H52A H 0.4566 0.3575 0.1139 0.098 Uiso 1 1 calc R A . H52B H 0.4189 0.2357 0.0909 0.098 Uiso 1 1 calc R . . H52C H 0.3695 0.3193 0.1427 0.098 Uiso 1 1 calc R . . C524 C 0.2923(10) 0.3075(18) 0.0193(13) 0.056(6) Uiso 0.67 1 d PU A 1 H52F H 0.3067 0.2449 -0.0141 0.067 Uiso 0.67 1 calc PR A 1 H52G H 0.2673 0.2718 0.0615 0.067 Uiso 0.67 1 calc PR A 1 C533 C 0.2346(11) 0.3857(16) -0.0139(10) 0.061(5) Uiso 0.67 1 d PU A 1 H53A H 0.1917 0.3392 -0.0369 0.073 Uiso 0.67 1 calc PR A 1 H53B H 0.2629 0.4298 -0.0513 0.073 Uiso 0.67 1 calc PR A 1 C531 C 0.154(2) 0.545(3) -0.013(3) 0.146(19) Uiso 0.67 1 d P A 1 H53C H 0.1773 0.5327 -0.0602 0.220 Uiso 0.67 1 calc PR A 1 H53D H 0.1607 0.6264 0.0003 0.220 Uiso 0.67 1 calc PR A 1 H53E H 0.0960 0.5261 -0.0144 0.220 Uiso 0.67 1 calc PR A 1 C532 C 0.1354(17) 0.422(2) 0.0854(17) 0.059(7) Uiso 0.67 1 d P A 1 H53F H 0.0896 0.3910 0.0584 0.089 Uiso 0.67 1 calc PR A 1 H53G H 0.1160 0.4816 0.1180 0.089 Uiso 0.67 1 calc PR A 1 H53H H 0.1610 0.3593 0.1122 0.089 Uiso 0.67 1 calc PR A 1 C535 C 0.131(5) 0.447(6) 0.094(5) 0.11(3) Uiso 0.33 1 d P A 2 H53I H 0.0880 0.3991 0.0740 0.169 Uiso 0.33 1 calc PR A 2 H53J H 0.1086 0.5197 0.1114 0.169 Uiso 0.33 1 calc PR A 2 H53K H 0.1571 0.4052 0.1331 0.169 Uiso 0.33 1 calc PR A 2 C522 C 0.2864(14) 0.316(4) 0.037(3) 0.071(13) Uiso 0.33 1 d PDU A 2 H52H H 0.2739 0.2918 0.0859 0.085 Uiso 0.33 1 calc PR A 2 H52I H 0.2943 0.2444 0.0095 0.085 Uiso 0.33 1 calc PR A 2 C536 C 0.147(3) 0.569(4) -0.005(3) 0.045(11) Uiso 0.33 1 d P A 2 H53L H 0.1090 0.5317 -0.0384 0.067 Uiso 0.33 1 calc PR A 2 H53M H 0.1854 0.6162 -0.0318 0.067 Uiso 0.33 1 calc PR A 2 H53N H 0.1165 0.6175 0.0276 0.067 Uiso 0.33 1 calc PR A 2 C534 C 0.209(3) 0.370(4) 0.009(3) 0.094(12) Uiso 0.33 1 d PDU A 2 H53O H 0.2132 0.3784 -0.0429 0.113 Uiso 0.33 1 calc PR A 2 H53P H 0.1630 0.3175 0.0191 0.113 Uiso 0.33 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0685(14) 0.0367(9) 0.0419(14) -0.0053(11) 0.0111(14) -0.0006(11) Al1 0.0640(19) 0.0327(12) 0.0364(18) 0.0000(13) 0.0056(18) -0.0006(15) C11 0.067(6) 0.034(4) 0.044(6) -0.002(6) 0.003(6) -0.006(4) C12 0.057(7) 0.052(6) 0.044(7) -0.001(5) 0.002(6) 0.001(5) C13 0.080(8) 0.069(7) 0.047(7) 0.022(6) -0.017(7) -0.010(7) C14 0.078(8) 0.043(6) 0.045(7) -0.005(5) 0.019(6) -0.010(5) C21 0.059(6) 0.046(6) 0.037(6) 0.000(5) -0.003(5) -0.002(5) C22 0.047(6) 0.052(6) 0.052(7) -0.006(6) 0.003(6) 0.001(5) C23 0.077(9) 0.058(6) 0.078(9) 0.011(7) 0.004(7) 0.003(6) C24 0.101(10) 0.044(6) 0.069(8) -0.003(6) 0.010(8) 0.014(7) C31 0.096(9) 0.044(6) 0.030(6) -0.001(5) 0.018(6) 0.002(6) C32 0.069(8) 0.050(6) 0.045(7) -0.004(6) -0.002(6) -0.005(5) C33 0.067(8) 0.092(9) 0.059(8) 0.012(7) -0.020(7) 0.003(7) C34 0.102(10) 0.065(8) 0.076(9) -0.011(7) -0.029(8) 0.009(7) N41 0.056(5) 0.043(4) 0.038(5) 0.015(4) -0.001(4) 0.003(4) C42 0.058(7) 0.048(6) 0.025(6) -0.010(5) 0.002(5) 0.008(5) C421 0.062(7) 0.046(5) 0.043(7) 0.002(5) -0.001(6) -0.003(5) C422 0.083(8) 0.040(6) 0.052(7) 0.007(6) 0.003(6) 0.002(5) C43 0.072(8) 0.049(6) 0.045(7) -0.004(6) -0.009(6) -0.004(6) C44 0.083(8) 0.037(5) 0.045(7) -0.006(5) -0.003(7) -0.006(6) C45 0.059(7) 0.057(6) 0.045(7) -0.007(6) -0.002(6) 0.005(6) C46 0.063(7) 0.036(5) 0.052(7) -0.002(5) -0.003(6) -0.003(5) C461 0.067(7) 0.050(6) 0.070(8) -0.001(6) 0.015(7) -0.002(5) C462 0.080(8) 0.037(6) 0.053(7) 0.010(5) -0.016(6) -0.004(5) C512 0.070(7) 0.071(8) 0.053(8) 0.029(6) 0.003(6) 0.000(6) N51 0.068(6) 0.043(5) 0.059(6) -0.002(4) 0.008(5) -0.012(4) N52 0.058(5) 0.050(5) 0.048(6) -0.016(5) -0.002(5) 0.003(4) C513 0.092(9) 0.054(7) 0.049(8) -0.015(6) 0.020(7) -0.005(6) C521 0.083(8) 0.045(6) 0.046(7) -0.017(6) -0.001(7) -0.001(6) C511 0.094(9) 0.053(7) 0.062(8) -0.003(6) 0.025(7) -0.008(7) N53 0.063(6) 0.062(6) 0.070(7) -0.031(6) -0.005(5) 0.005(5) C523 0.074(8) 0.068(7) 0.054(8) -0.006(7) 0.006(7) 0.000(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 N52 2.832(8) . ? K1 N53 2.852(9) . ? K1 N51 2.869(9) . ? K1 N41 2.952(8) . ? K1 C11 3.111(8) . ? K1 C42 3.480(9) . ? K1 C533 3.520(19) . ? K1 C46 3.522(11) . ? K1 Al1 3.839(3) . ? Al1 N41 1.995(8) . ? Al1 C11 2.031(11) . ? Al1 C31 2.038(11) . ? Al1 C21 2.047(10) . ? C11 C12 1.526(13) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C14 1.543(12) . ? C12 C13 1.547(14) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C21 C22 1.525(13) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.546(15) . ? C22 C24 1.552(14) . ? C22 H22A 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C31 C32 1.578(13) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C34 1.504(14) . ? C32 C33 1.562(13) . ? C32 H32A 1.0000 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? N41 C46 1.480(12) . ? N41 C42 1.487(12) . ? C42 C43 1.523(13) . ? C42 C422 1.545(12) . ? C42 C421 1.551(13) . ? C421 H42A 0.9800 . ? C421 H42B 0.9800 . ? C421 H42C 0.9800 . ? C422 H42D 0.9800 . ? C422 H42E 0.9800 . ? C422 H42F 0.9800 . ? C43 C44 1.537(13) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.529(14) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.527(13) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C461 1.552(14) . ? C46 C462 1.555(13) . ? C461 H46A 0.9800 . ? C461 H46B 0.9800 . ? C461 H46C 0.9800 . ? C462 H46D 0.9800 . ? C462 H46E 0.9800 . ? C462 H46F 0.9800 . ? C512 N51 1.481(13) . ? C512 H51D 0.9800 . ? C512 H51E 0.9800 . ? C512 H51F 0.9800 . ? N51 C513 1.462(12) . ? N51 C511 1.482(13) . ? N52 C521 1.479(12) . ? N52 C523 1.480(13) . ? N52 C522 1.489(10) . ? N52 C524 1.507(18) . ? C513 C521 1.500(13) . ? C513 H51G 0.9900 . ? C513 H51H 0.9900 . ? C521 H52D 0.9900 . ? C521 H52E 0.9900 . ? C511 H51A 0.9800 . ? C511 H51B 0.9800 . ? C511 H51C 0.9800 . ? N53 C534 1.32(5) . ? N53 C531 1.44(4) . ? N53 C532 1.45(3) . ? N53 C535 1.52(8) . ? N53 C533 1.54(2) . ? N53 C536 1.58(5) . ? C523 H52A 0.9800 . ? C523 H52B 0.9800 . ? C523 H52C 0.9800 . ? C524 C533 1.46(2) . ? C524 H52F 0.9900 . ? C524 H52G 0.9900 . ? C533 H53A 0.9900 . ? C533 H53B 0.9900 . ? C531 H53C 0.9800 . ? C531 H53D 0.9800 . ? C531 H53E 0.9800 . ? C532 H53F 0.9800 . ? C532 H53G 0.9800 . ? C532 H53H 0.9800 . ? C535 H53I 0.9800 . ? C535 H53J 0.9800 . ? C535 H53K 0.9800 . ? C522 C534 1.517(10) . ? C522 H52H 0.9900 . ? C522 H52I 0.9900 . ? C536 H53L 0.9800 . ? C536 H53M 0.9800 . ? C536 H53N 0.9800 . ? C534 H53O 0.9900 . ? C534 H53P 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 N52 K1 N53 65.8(2) . . ? N52 K1 N51 64.2(2) . . ? N53 K1 N51 109.1(3) . . ? N52 K1 N41 136.9(2) . . ? N53 K1 N41 125.6(3) . . ? N51 K1 N41 125.3(3) . . ? N52 K1 C11 156.4(3) . . ? N53 K1 C11 117.3(3) . . ? N51 K1 C11 94.2(3) . . ? N41 K1 C11 62.6(2) . . ? N52 K1 C42 126.9(2) . . ? N53 K1 C42 101.1(3) . . ? N51 K1 C42 149.3(3) . . ? N41 K1 C42 25.1(2) . . ? C11 K1 C42 76.4(3) . . ? N52 K1 C533 43.4(3) . . ? N53 K1 C533 25.4(3) . . ? N51 K1 C533 85.9(4) . . ? N41 K1 C533 147.4(4) . . ? C11 K1 C533 131.2(3) . . ? C42 K1 C533 122.4(4) . . ? N52 K1 C46 116.9(2) . . ? N53 K1 C46 139.4(3) . . ? N51 K1 C46 107.2(3) . . ? N41 K1 C46 24.5(2) . . ? C11 K1 C46 77.0(3) . . ? C42 K1 C46 42.4(2) . . ? C533 K1 C46 149.0(3) . . ? N52 K1 Al1 163.8(2) . . ? N53 K1 Al1 128.0(2) . . ? N51 K1 Al1 112.27(18) . . ? N41 K1 Al1 30.78(15) . . ? C11 K1 Al1 31.8(2) . . ? C42 K1 Al1 47.88(17) . . ? C533 K1 Al1 152.1(3) . . ? C46 K1 Al1 47.67(17) . . ? N41 Al1 C11 103.1(3) . . ? N41 Al1 C31 119.9(4) . . ? C11 Al1 C31 106.8(4) . . ? N41 Al1 C21 114.5(4) . . ? C11 Al1 C21 113.9(4) . . ? C31 Al1 C21 99.0(4) . . ? N41 Al1 K1 49.2(2) . . ? C11 Al1 K1 53.9(2) . . ? C31 Al1 K1 128.7(3) . . ? C21 Al1 K1 132.1(3) . . ? C12 C11 Al1 121.8(7) . . ? C12 C11 K1 142.6(7) . . ? Al1 C11 K1 94.2(3) . . ? C12 C11 H11A 106.9 . . ? Al1 C11 H11A 106.9 . . ? K1 C11 H11A 47.3 . . ? C12 C11 H11B 106.9 . . ? Al1 C11 H11B 106.9 . . ? K1 C11 H11B 67.2 . . ? H11A C11 H11B 106.7 . . ? C11 C12 C14 111.4(8) . . ? C11 C12 C13 113.3(8) . . ? C14 C12 C13 108.3(8) . . ? C11 C12 H12A 107.9 . . ? C14 C12 H12A 107.9 . . ? C13 C12 H12A 107.9 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C22 C21 Al1 117.5(7) . . ? C22 C21 H21A 107.9 . . ? Al1 C21 H21A 107.9 . . ? C22 C21 H21B 107.9 . . ? Al1 C21 H21B 107.9 . . ? H21A C21 H21B 107.2 . . ? C21 C22 C23 110.1(8) . . ? C21 C22 C24 113.6(9) . . ? C23 C22 C24 108.9(8) . . ? C21 C22 H22A 108.0 . . ? C23 C22 H22A 108.0 . . ? C24 C22 H22A 108.0 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C32 C31 Al1 123.1(7) . . ? C32 C31 H31A 106.5 . . ? Al1 C31 H31A 106.5 . . ? C32 C31 H31B 106.5 . . ? Al1 C31 H31B 106.5 . . ? H31A C31 H31B 106.5 . . ? C34 C32 C33 111.2(9) . . ? C34 C32 C31 112.0(9) . . ? C33 C32 C31 111.8(9) . . ? C34 C32 H32A 107.2 . . ? C33 C32 H32A 107.2 . . ? C31 C32 H32A 107.2 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 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 . . ? C46 N41 C42 117.1(7) . . ? C46 N41 Al1 117.9(6) . . ? C42 N41 Al1 117.5(6) . . ? C46 N41 K1 99.9(6) . . ? C42 N41 K1 97.7(5) . . ? Al1 N41 K1 100.0(3) . . ? N41 C42 C43 112.5(8) . . ? N41 C42 C422 115.2(8) . . ? C43 C42 C422 108.4(8) . . ? N41 C42 C421 108.0(8) . . ? C43 C42 C421 105.8(8) . . ? C422 C42 C421 106.4(8) . . ? N41 C42 K1 57.2(4) . . ? C43 C42 K1 80.3(6) . . ? C422 C42 K1 170.7(6) . . ? C421 C42 K1 73.3(5) . . ? C42 C421 H42A 109.5 . . ? C42 C421 H42B 109.5 . . ? H42A C421 H42B 109.5 . . ? C42 C421 H42C 109.5 . . ? H42A C421 H42C 109.5 . . ? H42B C421 H42C 109.5 . . ? C42 C422 H42D 109.5 . . ? C42 C422 H42E 109.5 . . ? H42D C422 H42E 109.5 . . ? C42 C422 H42F 109.5 . . ? H42D C422 H42F 109.5 . . ? H42E C422 H42F 109.5 . . ? C42 C43 C44 113.1(8) . . ? C42 C43 H43A 109.0 . . ? C44 C43 H43A 109.0 . . ? C42 C43 H43B 109.0 . . ? C44 C43 H43B 109.0 . . ? H43A C43 H43B 107.8 . . ? C45 C44 C43 107.1(9) . . ? C45 C44 H44A 110.3 . . ? C43 C44 H44A 110.3 . . ? C45 C44 H44B 110.3 . . ? C43 C44 H44B 110.3 . . ? H44A C44 H44B 108.5 . . ? C46 C45 C44 114.0(9) . . ? C46 C45 H45A 108.7 . . ? C44 C45 H45A 108.7 . . ? C46 C45 H45B 108.7 . . ? C44 C45 H45B 108.7 . . ? H45A C45 H45B 107.6 . . ? N41 C46 C45 112.7(9) . . ? N41 C46 C461 109.7(9) . . ? C45 C46 C461 105.1(8) . . ? N41 C46 C462 114.7(8) . . ? C45 C46 C462 108.0(8) . . ? C461 C46 C462 106.0(8) . . ? N41 C46 K1 55.7(5) . . ? C45 C46 K1 81.5(6) . . ? C461 C46 K1 75.5(6) . . ? C462 C46 K1 169.3(7) . . ? C46 C461 H46A 109.5 . . ? C46 C461 H46B 109.5 . . ? H46A C461 H46B 109.5 . . ? C46 C461 H46C 109.5 . . ? H46A C461 H46C 109.5 . . ? H46B C461 H46C 109.5 . . ? C46 C462 H46D 109.5 . . ? C46 C462 H46E 109.5 . . ? H46D C462 H46E 109.5 . . ? C46 C462 H46F 109.5 . . ? H46D C462 H46F 109.5 . . ? H46E C462 H46F 109.5 . . ? N51 C512 H51D 109.5 . . ? N51 C512 H51E 109.5 . . ? H51D C512 H51E 109.5 . . ? N51 C512 H51F 109.5 . . ? H51D C512 H51F 109.5 . . ? H51E C512 H51F 109.5 . . ? C513 N51 C512 111.1(9) . . ? C513 N51 C511 109.1(9) . . ? C512 N51 C511 109.2(8) . . ? C513 N51 K1 108.7(6) . . ? C512 N51 K1 101.1(6) . . ? C511 N51 K1 117.4(6) . . ? C521 N52 C523 111.5(8) . . ? C521 N52 C522 121(2) . . ? C523 N52 C522 104(2) . . ? C521 N52 C524 107.3(11) . . ? C523 N52 C524 110.6(11) . . ? C522 N52 C524 14(3) . . ? C521 N52 K1 113.3(6) . . ? C523 N52 K1 102.8(6) . . ? C522 N52 K1 102(2) . . ? C524 N52 K1 111.3(10) . . ? N51 C513 C521 116.9(9) . . ? N51 C513 H51G 108.1 . . ? C521 C513 H51G 108.1 . . ? N51 C513 H51H 108.1 . . ? C521 C513 H51H 108.1 . . ? H51G C513 H51H 107.3 . . ? N52 C521 C513 111.5(8) . . ? N52 C521 H52D 109.5 . . ? C513 C521 H52D 109.6 . . ? N52 C521 H52E 109.0 . . ? C513 C521 H52E 109.1 . . ? H52D C521 H52E 108.0 . . ? N51 C511 H51A 108.5 . . ? N51 C511 H51B 109.4 . . ? H51A C511 H51B 109.5 . . ? N51 C511 H51C 110.5 . . ? H51A C511 H51C 109.5 . . ? H51B C511 H51C 109.5 . . ? C534 N53 C531 110(3) . . ? C534 N53 C532 91(3) . . ? C531 N53 C532 110(2) . . ? C534 N53 C535 104(4) . . ? C531 N53 C535 106(4) . . ? C532 N53 C535 13(3) . . ? C534 N53 C533 24(2) . . ? C531 N53 C533 99.3(19) . . ? C532 N53 C533 115.1(15) . . ? C535 N53 C533 128(3) . . ? C534 N53 C536 121(3) . . ? C531 N53 C536 11(3) . . ? C532 N53 C536 106(2) . . ? C535 N53 C536 99(4) . . ? C533 N53 C536 110(2) . . ? C534 N53 K1 116.8(19) . . ? C531 N53 K1 108.1(16) . . ? C532 N53 K1 119.8(14) . . ? C535 N53 K1 112(3) . . ? C533 N53 K1 102.3(8) . . ? C536 N53 K1 102.7(15) . . ? N52 C523 H52A 109.5 . . ? N52 C523 H52B 109.5 . . ? H52A C523 H52B 109.5 . . ? N52 C523 H52C 109.5 . . ? H52A C523 H52C 109.5 . . ? H52B C523 H52C 109.5 . . ? C533 C524 N52 110.3(15) . . ? C533 C524 H52F 109.6 . . ? N52 C524 H52F 109.6 . . ? C533 C524 H52G 109.6 . . ? N52 C524 H52G 109.6 . . ? H52F C524 H52G 108.1 . . ? C524 C533 N53 114.4(16) . . ? C524 C533 K1 83.7(12) . . ? N53 C533 K1 52.3(7) . . ? C524 C533 H53A 108.7 . . ? N53 C533 H53A 108.7 . . ? K1 C533 H53A 160.9 . . ? C524 C533 H53B 108.7 . . ? N53 C533 H53B 108.7 . . ? K1 C533 H53B 80.8 . . ? H53A C533 H53B 107.6 . . ? N53 C531 H53C 109.5 . . ? N53 C531 H53D 109.5 . . ? N53 C531 H53E 109.5 . . ? N53 C532 H53F 109.5 . . ? N53 C532 H53G 109.5 . . ? N53 C532 H53H 109.5 . . ? N53 C535 H53I 109.5 . . ? N53 C535 H53J 109.5 . . ? H53I C535 H53J 109.5 . . ? N53 C535 H53K 109.5 . . ? H53I C535 H53K 109.5 . . ? H53J C535 H53K 109.5 . . ? N52 C522 C534 127(4) . . ? N52 C522 H52H 105.6 . . ? C534 C522 H52H 105.6 . . ? N52 C522 H52I 105.6 . . ? C534 C522 H52I 105.6 . . ? H52H C522 H52I 106.1 . . ? N53 C536 H53L 109.5 . . ? N53 C536 H53M 109.5 . . ? H53L C536 H53M 109.5 . . ? N53 C536 H53N 109.5 . . ? H53L C536 H53N 109.5 . . ? H53M C536 H53N 109.5 . . ? N53 C534 C522 112(4) . . ? N53 C534 H53O 109.2 . . ? C522 C534 H53O 109.2 . . ? N53 C534 H53P 109.2 . . ? C522 C534 H53P 109.2 . . ? H53O C534 H53P 107.9 . . ? 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 N52 K1 Al1 N41 -48.2(8) . . . . ? N53 K1 Al1 N41 97.5(4) . . . . ? N51 K1 Al1 N41 -122.2(4) . . . . ? C11 K1 Al1 N41 178.6(5) . . . . ? C42 K1 Al1 N41 29.7(4) . . . . ? C533 K1 Al1 N41 110.4(8) . . . . ? C46 K1 Al1 N41 -28.7(4) . . . . ? N52 K1 Al1 C11 133.3(8) . . . . ? N53 K1 Al1 C11 -81.0(5) . . . . ? N51 K1 Al1 C11 59.3(4) . . . . ? N41 K1 Al1 C11 -178.6(5) . . . . ? C42 K1 Al1 C11 -148.9(4) . . . . ? C533 K1 Al1 C11 -68.2(8) . . . . ? C46 K1 Al1 C11 152.7(4) . . . . ? N52 K1 Al1 C31 50.6(8) . . . . ? N53 K1 Al1 C31 -163.7(5) . . . . ? N51 K1 Al1 C31 -23.4(4) . . . . ? N41 K1 Al1 C31 98.7(5) . . . . ? C11 K1 Al1 C31 -82.7(5) . . . . ? C42 K1 Al1 C31 128.4(5) . . . . ? C533 K1 Al1 C31 -150.9(8) . . . . ? C46 K1 Al1 C31 70.0(5) . . . . ? N52 K1 Al1 C21 -135.7(8) . . . . ? N53 K1 Al1 C21 10.0(5) . . . . ? N51 K1 Al1 C21 150.3(4) . . . . ? N41 K1 Al1 C21 -87.6(5) . . . . ? C11 K1 Al1 C21 91.0(5) . . . . ? C42 K1 Al1 C21 -57.9(4) . . . . ? C533 K1 Al1 C21 22.8(8) . . . . ? C46 K1 Al1 C21 -116.3(5) . . . . ? N41 Al1 C11 C12 -170.6(8) . . . . ? C31 Al1 C11 C12 -43.5(9) . . . . ? C21 Al1 C11 C12 64.7(9) . . . . ? K1 Al1 C11 C12 -169.5(10) . . . . ? N41 Al1 C11 K1 -1.1(4) . . . . ? C31 Al1 C11 K1 126.1(4) . . . . ? C21 Al1 C11 K1 -125.8(4) . . . . ? N52 K1 C11 C12 15.7(15) . . . . ? N53 K1 C11 C12 -75.9(11) . . . . ? N51 K1 C11 C12 38.2(11) . . . . ? N41 K1 C11 C12 166.1(12) . . . . ? C42 K1 C11 C12 -171.5(11) . . . . ? C533 K1 C11 C12 -50.0(12) . . . . ? C46 K1 C11 C12 144.9(11) . . . . ? Al1 K1 C11 C12 165.3(13) . . . . ? N52 K1 C11 Al1 -149.5(5) . . . . ? N53 K1 C11 Al1 118.9(4) . . . . ? N51 K1 C11 Al1 -127.1(4) . . . . ? N41 K1 C11 Al1 0.8(3) . . . . ? C42 K1 C11 Al1 23.2(3) . . . . ? C533 K1 C11 Al1 144.7(5) . . . . ? C46 K1 C11 Al1 -20.4(3) . . . . ? Al1 C11 C12 C14 86.9(10) . . . . ? K1 C11 C12 C14 -75.8(13) . . . . ? Al1 C11 C12 C13 -150.7(8) . . . . ? K1 C11 C12 C13 46.7(15) . . . . ? N41 Al1 C21 C22 -160.5(7) . . . . ? C11 Al1 C21 C22 -42.2(9) . . . . ? C31 Al1 C21 C22 70.7(8) . . . . ? K1 Al1 C21 C22 -104.3(7) . . . . ? Al1 C21 C22 C23 82.4(10) . . . . ? Al1 C21 C22 C24 -155.2(7) . . . . ? N41 Al1 C31 C32 -76.9(9) . . . . ? C11 Al1 C31 C32 166.5(8) . . . . ? C21 Al1 C31 C32 48.1(9) . . . . ? K1 Al1 C31 C32 -136.6(7) . . . . ? Al1 C31 C32 C34 -103.8(10) . . . . ? Al1 C31 C32 C33 130.7(9) . . . . ? C11 Al1 N41 C46 108.1(7) . . . . ? C31 Al1 N41 C46 -10.3(8) . . . . ? C21 Al1 N41 C46 -127.6(7) . . . . ? K1 Al1 N41 C46 106.9(7) . . . . ? C11 Al1 N41 C42 -103.0(7) . . . . ? C31 Al1 N41 C42 138.6(7) . . . . ? C21 Al1 N41 C42 21.3(8) . . . . ? K1 Al1 N41 C42 -104.2(7) . . . . ? C11 Al1 N41 K1 1.2(4) . . . . ? C31 Al1 N41 K1 -117.2(4) . . . . ? C21 Al1 N41 K1 125.5(4) . . . . ? N52 K1 N41 C46 41.4(7) . . . . ? N53 K1 N41 C46 133.0(6) . . . . ? N51 K1 N41 C46 -47.2(6) . . . . ? C11 K1 N41 C46 -121.7(6) . . . . ? C42 K1 N41 C46 119.4(8) . . . . ? C533 K1 N41 C46 113.7(8) . . . . ? Al1 K1 N41 C46 -120.9(7) . . . . ? N52 K1 N41 C42 -77.9(6) . . . . ? N53 K1 N41 C42 13.6(6) . . . . ? N51 K1 N41 C42 -166.5(5) . . . . ? C11 K1 N41 C42 118.9(6) . . . . ? C533 K1 N41 C42 -5.6(9) . . . . ? C46 K1 N41 C42 -119.4(8) . . . . ? Al1 K1 N41 C42 119.8(7) . . . . ? N52 K1 N41 Al1 162.3(3) . . . . ? N53 K1 N41 Al1 -106.1(4) . . . . ? N51 K1 N41 Al1 73.7(4) . . . . ? C11 K1 N41 Al1 -0.8(3) . . . . ? C42 K1 N41 Al1 -119.8(7) . . . . ? C533 K1 N41 Al1 -125.4(6) . . . . ? C46 K1 N41 Al1 120.9(7) . . . . ? C46 N41 C42 C43 -44.2(11) . . . . ? Al1 N41 C42 C43 166.7(7) . . . . ? K1 N41 C42 C43 61.1(8) . . . . ? C46 N41 C42 C422 80.7(10) . . . . ? Al1 N41 C42 C422 -68.4(9) . . . . ? K1 N41 C42 C422 -174.0(7) . . . . ? C46 N41 C42 C421 -160.6(8) . . . . ? Al1 N41 C42 C421 50.3(9) . . . . ? K1 N41 C42 C421 -55.3(7) . . . . ? C46 N41 C42 K1 -105.3(7) . . . . ? Al1 N41 C42 K1 105.5(6) . . . . ? N52 K1 C42 N41 123.3(5) . . . . ? N53 K1 C42 N41 -168.7(5) . . . . ? N51 K1 C42 N41 21.8(8) . . . . ? C11 K1 C42 N41 -53.1(5) . . . . ? C533 K1 C42 N41 176.4(5) . . . . ? C46 K1 C42 N41 32.4(5) . . . . ? Al1 K1 C42 N41 -36.8(4) . . . . ? N52 K1 C42 C43 -1.5(7) . . . . ? N53 K1 C42 C43 66.4(6) . . . . ? N51 K1 C42 C43 -103.0(7) . . . . ? N41 K1 C42 C43 -124.8(8) . . . . ? C11 K1 C42 C43 -177.9(6) . . . . ? C533 K1 C42 C43 51.6(7) . . . . ? C46 K1 C42 C43 -92.5(6) . . . . ? Al1 K1 C42 C43 -161.6(7) . . . . ? N52 K1 C42 C422 159(4) . . . . ? N53 K1 C42 C422 -133(4) . . . . ? N51 K1 C42 C422 58(4) . . . . ? N41 K1 C42 C422 36(4) . . . . ? C11 K1 C42 C422 -17(4) . . . . ? C533 K1 C42 C422 -147(4) . . . . ? C46 K1 C42 C422 69(4) . . . . ? Al1 K1 C42 C422 -1(4) . . . . ? N52 K1 C42 C421 -111.4(5) . . . . ? N53 K1 C42 C421 -43.4(5) . . . . ? N51 K1 C42 C421 147.2(5) . . . . ? N41 K1 C42 C421 125.3(8) . . . . ? C11 K1 C42 C421 72.2(5) . . . . ? C533 K1 C42 C421 -58.2(6) . . . . ? C46 K1 C42 C421 157.7(7) . . . . ? Al1 K1 C42 C421 88.5(5) . . . . ? N41 C42 C43 C44 51.8(11) . . . . ? C422 C42 C43 C44 -76.7(11) . . . . ? C421 C42 C43 C44 169.6(9) . . . . ? K1 C42 C43 C44 100.2(8) . . . . ? C42 C43 C44 C45 -57.0(11) . . . . ? C43 C44 C45 C46 55.9(11) . . . . ? C42 N41 C46 C45 42.8(12) . . . . ? Al1 N41 C46 C45 -168.2(7) . . . . ? K1 N41 C46 C45 -61.2(9) . . . . ? C42 N41 C46 C461 159.5(8) . . . . ? Al1 N41 C46 C461 -51.5(10) . . . . ? K1 N41 C46 C461 55.5(8) . . . . ? C42 N41 C46 C462 -81.4(10) . . . . ? Al1 N41 C46 C462 67.6(10) . . . . ? K1 N41 C46 C462 174.6(7) . . . . ? C42 N41 C46 K1 104.0(7) . . . . ? Al1 N41 C46 K1 -107.0(6) . . . . ? C44 C45 C46 N41 -49.6(12) . . . . ? C44 C45 C46 C461 -169.0(9) . . . . ? C44 C45 C46 C462 78.2(11) . . . . ? C44 C45 C46 K1 -96.7(8) . . . . ? N52 K1 C46 N41 -149.5(5) . . . . ? N53 K1 C46 N41 -66.1(7) . . . . ? N51 K1 C46 N41 141.2(5) . . . . ? C11 K1 C46 N41 50.8(5) . . . . ? C42 K1 C46 N41 -33.2(5) . . . . ? C533 K1 C46 N41 -107.1(8) . . . . ? Al1 K1 C46 N41 36.4(5) . . . . ? N52 K1 C46 C45 -24.3(7) . . . . ? N53 K1 C46 C45 59.1(7) . . . . ? N51 K1 C46 C45 -93.6(6) . . . . ? N41 K1 C46 C45 125.2(9) . . . . ? C11 K1 C46 C45 176.0(6) . . . . ? C42 K1 C46 C45 92.0(6) . . . . ? C533 K1 C46 C45 18.1(10) . . . . ? Al1 K1 C46 C45 161.6(7) . . . . ? N52 K1 C46 C461 83.7(6) . . . . ? N53 K1 C46 C461 167.2(5) . . . . ? N51 K1 C46 C461 14.4(6) . . . . ? N41 K1 C46 C461 -126.8(8) . . . . ? C11 K1 C46 C461 -75.9(5) . . . . ? C42 K1 C46 C461 -160.0(7) . . . . ? C533 K1 C46 C461 126.2(8) . . . . ? Al1 K1 C46 C461 -90.3(5) . . . . ? N52 K1 C46 C462 -177(4) . . . . ? N53 K1 C46 C462 -93(4) . . . . ? N51 K1 C46 C462 114(4) . . . . ? N41 K1 C46 C462 -27(4) . . . . ? C11 K1 C46 C462 24(4) . . . . ? C42 K1 C46 C462 -61(4) . . . . ? C533 K1 C46 C462 -134(4) . . . . ? Al1 K1 C46 C462 9(4) . . . . ? N52 K1 N51 C513 -15.8(7) . . . . ? N53 K1 N51 C513 -65.3(8) . . . . ? N41 K1 N51 C513 114.9(7) . . . . ? C11 K1 N51 C513 174.0(7) . . . . ? C42 K1 N51 C513 103.8(7) . . . . ? C533 K1 N51 C513 -55.0(7) . . . . ? C46 K1 N51 C513 96.3(7) . . . . ? Al1 K1 N51 C513 146.9(6) . . . . ? N52 K1 N51 C512 101.2(6) . . . . ? N53 K1 N51 C512 51.7(6) . . . . ? N41 K1 N51 C512 -128.1(6) . . . . ? C11 K1 N51 C512 -69.0(6) . . . . ? C42 K1 N51 C512 -139.3(6) . . . . ? C533 K1 N51 C512 62.0(6) . . . . ? C46 K1 N51 C512 -146.7(6) . . . . ? Al1 K1 N51 C512 -96.1(6) . . . . ? N52 K1 N51 C511 -140.1(8) . . . . ? N53 K1 N51 C511 170.4(7) . . . . ? N41 K1 N51 C511 -9.5(8) . . . . ? C11 K1 N51 C511 49.6(7) . . . . ? C42 K1 N51 C511 -20.6(10) . . . . ? C533 K1 N51 C511 -179.3(8) . . . . ? C46 K1 N51 C511 -28.0(8) . . . . ? Al1 K1 N51 C511 22.6(8) . . . . ? N53 K1 N52 C521 115.4(7) . . . . ? N51 K1 N52 C521 -12.7(6) . . . . ? N41 K1 N52 C521 -127.7(6) . . . . ? C11 K1 N52 C521 12.3(11) . . . . ? C42 K1 N52 C521 -158.9(6) . . . . ? C533 K1 N52 C521 100.7(8) . . . . ? C46 K1 N52 C521 -109.8(7) . . . . ? Al1 K1 N52 C521 -93.7(9) . . . . ? N53 K1 N52 C523 -124.1(7) . . . . ? N51 K1 N52 C523 107.9(6) . . . . ? N41 K1 N52 C523 -7.1(8) . . . . ? C11 K1 N52 C523 132.8(7) . . . . ? C42 K1 N52 C523 -38.3(7) . . . . ? C533 K1 N52 C523 -138.8(8) . . . . ? C46 K1 N52 C523 10.8(7) . . . . ? Al1 K1 N52 C523 26.8(11) . . . . ? N53 K1 N52 C522 -17(2) . . . . ? N51 K1 N52 C522 -145(2) . . . . ? N41 K1 N52 C522 100(2) . . . . ? C11 K1 N52 C522 -120(2) . . . . ? C42 K1 N52 C522 69(2) . . . . ? C533 K1 N52 C522 -31(2) . . . . ? C46 K1 N52 C522 118(2) . . . . ? Al1 K1 N52 C522 134(2) . . . . ? N53 K1 N52 C524 -5.6(10) . . . . ? N51 K1 N52 C524 -133.7(11) . . . . ? N41 K1 N52 C524 111.3(10) . . . . ? C11 K1 N52 C524 -108.7(12) . . . . ? C42 K1 N52 C524 80.1(11) . . . . ? C533 K1 N52 C524 -20.3(11) . . . . ? C46 K1 N52 C524 129.2(10) . . . . ? Al1 K1 N52 C524 145.2(10) . . . . ? C512 N51 C513 C521 -64.3(12) . . . . ? C511 N51 C513 C521 175.3(9) . . . . ? K1 N51 C513 C521 46.2(11) . . . . ? C523 N52 C521 C513 -75.3(11) . . . . ? C522 N52 C521 C513 162(2) . . . . ? C524 N52 C521 C513 163.3(11) . . . . ? K1 N52 C521 C513 40.1(10) . . . . ? N51 C513 C521 N52 -61.4(13) . . . . ? N52 K1 N53 C534 -4(3) . . . . ? N51 K1 N53 C534 45(3) . . . . ? N41 K1 N53 C534 -135(3) . . . . ? C11 K1 N53 C534 150(3) . . . . ? C42 K1 N53 C534 -129(3) . . . . ? C533 K1 N53 C534 20(3) . . . . ? C46 K1 N53 C534 -108(3) . . . . ? Al1 K1 N53 C534 -174(3) . . . . ? N52 K1 N53 C531 -128(2) . . . . ? N51 K1 N53 C531 -80(2) . . . . ? N41 K1 N53 C531 100(2) . . . . ? C11 K1 N53 C531 26(2) . . . . ? C42 K1 N53 C531 106(2) . . . . ? C533 K1 N53 C531 -104(2) . . . . ? C46 K1 N53 C531 128(2) . . . . ? Al1 K1 N53 C531 62(2) . . . . ? N52 K1 N53 C532 104.7(14) . . . . ? N51 K1 N53 C532 153.4(14) . . . . ? N41 K1 N53 C532 -26.8(14) . . . . ? C11 K1 N53 C532 -101.3(14) . . . . ? C42 K1 N53 C532 -20.9(14) . . . . ? C533 K1 N53 C532 128.7(17) . . . . ? C46 K1 N53 C532 0.9(15) . . . . ? Al1 K1 N53 C532 -65.4(14) . . . . ? N52 K1 N53 C535 116(3) . . . . ? N51 K1 N53 C535 165(3) . . . . ? N41 K1 N53 C535 -16(3) . . . . ? C11 K1 N53 C535 -90(3) . . . . ? C42 K1 N53 C535 -10(3) . . . . ? C533 K1 N53 C535 140(3) . . . . ? C46 K1 N53 C535 12(3) . . . . ? Al1 K1 N53 C535 -54(3) . . . . ? N52 K1 N53 C533 -24.0(8) . . . . ? N51 K1 N53 C533 24.6(9) . . . . ? N41 K1 N53 C533 -155.5(8) . . . . ? C11 K1 N53 C533 130.0(8) . . . . ? C42 K1 N53 C533 -149.7(8) . . . . ? C46 K1 N53 C533 -127.8(8) . . . . ? Al1 K1 N53 C533 165.9(8) . . . . ? N52 K1 N53 C536 -139(2) . . . . ? N51 K1 N53 C536 -90(2) . . . . ? N41 K1 N53 C536 90(2) . . . . ? C11 K1 N53 C536 15(2) . . . . ? C42 K1 N53 C536 96(2) . . . . ? C533 K1 N53 C536 -115(2) . . . . ? C46 K1 N53 C536 118(2) . . . . ? Al1 K1 N53 C536 51(2) . . . . ? C521 N52 C524 C533 -86.5(17) . . . . ? C523 N52 C524 C533 151.6(15) . . . . ? C522 N52 C524 C533 89(10) . . . . ? K1 N52 C524 C533 37.9(19) . . . . ? N52 C524 C533 N53 -71(2) . . . . ? N52 C524 C533 K1 -27.6(14) . . . . ? C534 N53 C533 C524 -70(5) . . . . ? C531 N53 C533 C524 171(2) . . . . ? C532 N53 C533 C524 -72(2) . . . . ? C535 N53 C533 C524 -71(5) . . . . ? C536 N53 C533 C524 168.6(19) . . . . ? K1 N53 C533 C524 59.9(15) . . . . ? C534 N53 C533 K1 -130(5) . . . . ? C531 N53 C533 K1 111.0(18) . . . . ? C532 N53 C533 K1 -131.6(17) . . . . ? C535 N53 C533 K1 -131(5) . . . . ? C536 N53 C533 K1 108.8(17) . . . . ? N52 K1 C533 C524 19.7(10) . . . . ? N53 K1 C533 C524 -127.6(16) . . . . ? N51 K1 C533 C524 75.7(11) . . . . ? N41 K1 C533 C524 -88.8(12) . . . . ? C11 K1 C533 C524 167.6(10) . . . . ? C42 K1 C533 C524 -91.6(11) . . . . ? C46 K1 C533 C524 -41.5(15) . . . . ? Al1 K1 C533 C524 -151.8(9) . . . . ? N52 K1 C533 N53 147.3(11) . . . . ? N51 K1 C533 N53 -156.7(9) . . . . ? N41 K1 C533 N53 38.8(12) . . . . ? C11 K1 C533 N53 -64.8(10) . . . . ? C42 K1 C533 N53 36.0(10) . . . . ? C46 K1 C533 N53 86.1(10) . . . . ? Al1 K1 C533 N53 -24.2(13) . . . . ? C521 N52 C522 C534 -83(6) . . . . ? C523 N52 C522 C534 150(5) . . . . ? C524 N52 C522 C534 -88(11) . . . . ? K1 N52 C522 C534 44(6) . . . . ? C531 N53 C534 C522 147(4) . . . . ? C532 N53 C534 C522 -101(4) . . . . ? C535 N53 C534 C522 -100(5) . . . . ? C533 N53 C534 C522 80(6) . . . . ? C536 N53 C534 C522 150(3) . . . . ? K1 N53 C534 C522 24(5) . . . . ? N52 C522 C534 N53 -51(7) . . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 64.98 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.647 _refine_diff_density_min -0.861 _refine_diff_density_rms 0.089 #===END ################################################################### ################## COMPOUND 7##################################### ################################################################## data_srbc902 _database_code_depnum_ccdc_archive 'CCDC 771327' #TrackingRef '- all3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H64 Al K N4' _chemical_formula_sum 'C28 H64 Al K N4' _chemical_formula_weight 522.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 11.3887(5) _cell_length_b 18.1965(8) _cell_length_c 16.9006(8) _cell_angle_alpha 90.00 _cell_angle_beta 105.222(5) _cell_angle_gamma 90.00 _cell_volume 3379.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9916 _cell_measurement_theta_min 4.0155 _cell_measurement_theta_max 71.5931 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.028 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 0.204 _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Oxford Diffraction Gemini S' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18993 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 25.97 _reflns_number_total 6485 _reflns_number_gt 4992 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _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^)+(0.0884P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.056(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6485 _refine_ls_number_parameters 336 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1268 _refine_ls_wR_factor_gt 0.1234 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group K1 K 0.11211(3) 0.08439(2) 0.27953(2) 0.03147(14) Uani 1 1 d . . . Al1 Al 0.35594(4) 0.01404(3) 0.23235(3) 0.02357(15) Uani 1 1 d . B . N1 N 0.23647(12) -0.04774(8) 0.25672(8) 0.0260(3) Uani 1 1 d . . . N2 N -0.09574(14) 0.11504(10) 0.14516(10) 0.0403(4) Uani 1 1 d . . . N3 N -0.10653(13) 0.12197(9) 0.32060(9) 0.0355(4) Uani 1 1 d . . . N4 N 0.13042(14) 0.13866(9) 0.44648(9) 0.0333(4) Uani 1 1 d . . . C10 C 0.26612(16) -0.08475(10) 0.33706(10) 0.0303(4) Uani 1 1 d . . . H10A H 0.3137 -0.0484 0.3773 0.036 Uiso 1 1 calc R . . C11 C 0.15101(18) -0.10186(12) 0.36540(11) 0.0393(5) Uani 1 1 d . . . H11A H 0.1738 -0.1315 0.4163 0.047 Uiso 1 1 calc R . . H11B H 0.1148 -0.0553 0.3780 0.047 Uiso 1 1 calc R . . C12 C 0.05667(19) -0.14378(12) 0.30005(12) 0.0444(5) Uani 1 1 d . . . H12A H -0.0185 -0.1503 0.3182 0.053 Uiso 1 1 calc R . . H12B H 0.0886 -0.1931 0.2922 0.053 Uiso 1 1 calc R . . C13 C 0.02757(17) -0.10137(11) 0.21887(12) 0.0392(5) Uani 1 1 d . . . H13A H -0.0144 -0.0550 0.2252 0.047 Uiso 1 1 calc R . . H13B H -0.0284 -0.1310 0.1759 0.047 Uiso 1 1 calc R . . C14 C 0.14330(16) -0.08359(10) 0.19140(10) 0.0304(4) Uani 1 1 d . . . H14A H 0.1184 -0.0464 0.1465 0.036 Uiso 1 1 calc R . . C15 C 0.34677(19) -0.15355(11) 0.34495(12) 0.0410(5) Uani 1 1 d . . . H15A H 0.4161 -0.1432 0.3225 0.061 Uiso 1 1 calc R . . H15B H 0.2991 -0.1942 0.3145 0.061 Uiso 1 1 calc R . . H15C H 0.3765 -0.1671 0.4029 0.061 Uiso 1 1 calc R . . C16 C 0.18545(18) -0.15150(11) 0.15225(12) 0.0403(5) Uani 1 1 d . . . H16A H 0.2620 -0.1404 0.1386 0.060 Uiso 1 1 calc R . . H16B H 0.1233 -0.1648 0.1022 0.060 Uiso 1 1 calc R . . H16C H 0.1979 -0.1926 0.1910 0.060 Uiso 1 1 calc R . . C20 C -0.20978(18) 0.12186(14) 0.16933(13) 0.0492(5) Uani 1 1 d . . . H20A H -0.2451 0.0722 0.1702 0.059 Uiso 1 1 calc R . . H20B H -0.2679 0.1511 0.1272 0.059 Uiso 1 1 calc R . . C21 C -0.19636(18) 0.15763(13) 0.25251(12) 0.0458(5) Uani 1 1 d . . . H21A H -0.1725 0.2096 0.2492 0.055 Uiso 1 1 calc R . . H21B H -0.2765 0.1572 0.2650 0.055 Uiso 1 1 calc R . . C22 C -0.09180(18) 0.16603(12) 0.39530(12) 0.0433(5) Uani 1 1 d . . . H22A H -0.1682 0.1637 0.4127 0.052 Uiso 1 1 calc R . . H22B H -0.0785 0.2179 0.3824 0.052 Uiso 1 1 calc R . . C23 C 0.01265(18) 0.14154(12) 0.46628(12) 0.0422(5) Uani 1 1 d . . . H23A H 0.0191 0.1757 0.5128 0.051 Uiso 1 1 calc R . . H23B H -0.0061 0.0922 0.4843 0.051 Uiso 1 1 calc R . . C24 C -0.1171(2) 0.06891(15) 0.07134(13) 0.0589(6) Uani 1 1 d . . . H24A H -0.0411 0.0639 0.0548 0.088 Uiso 1 1 calc R . . H24B H -0.1791 0.0919 0.0268 0.088 Uiso 1 1 calc R . . H24C H -0.1452 0.0202 0.0831 0.088 Uiso 1 1 calc R . . C25 C -0.0506(2) 0.18676(13) 0.12912(15) 0.0561(6) Uani 1 1 d . . . H25A H -0.0353 0.2169 0.1789 0.084 Uiso 1 1 calc R . . H25B H -0.1113 0.2110 0.0849 0.084 Uiso 1 1 calc R . . H25C H 0.0253 0.1807 0.1128 0.084 Uiso 1 1 calc R . . C26 C -0.14310(18) 0.04721(12) 0.33342(13) 0.0440(5) Uani 1 1 d . . . H26A H -0.0824 0.0250 0.3793 0.066 Uiso 1 1 calc R . . H26B H -0.1492 0.0182 0.2836 0.066 Uiso 1 1 calc R . . H26C H -0.2223 0.0481 0.3460 0.066 Uiso 1 1 calc R . . C27 C 0.16955(19) 0.21132(12) 0.42912(14) 0.0459(5) Uani 1 1 d . . . H27A H 0.2503 0.2081 0.4190 0.069 Uiso 1 1 calc R . . H27B H 0.1733 0.2436 0.4761 0.069 Uiso 1 1 calc R . . H27C H 0.1115 0.2313 0.3805 0.069 Uiso 1 1 calc R . . C28 C 0.2215(2) 0.10666(15) 0.51548(13) 0.0560(6) Uani 1 1 d . . . H28A H 0.3002 0.1044 0.5022 0.084 Uiso 1 1 calc R . . H28B H 0.1963 0.0569 0.5261 0.084 Uiso 1 1 calc R . . H28C H 0.2291 0.1372 0.5644 0.084 Uiso 1 1 calc R . . C30 C 0.38878(15) 0.09404(10) 0.32059(10) 0.0273(4) Uani 1 1 d . . . H30A H 0.3491 0.1398 0.2950 0.033 Uiso 1 1 calc R . . H30B H 0.3477 0.0793 0.3630 0.033 Uiso 1 1 calc R . . C31 C 0.52183(15) 0.11257(10) 0.36429(10) 0.0280(4) Uani 1 1 d . . . H31A H 0.5711 0.1054 0.3238 0.034 Uiso 1 1 calc R . . C32 C 0.57096(17) 0.06005(11) 0.43531(11) 0.0373(4) Uani 1 1 d . . . H32A H 0.6580 0.0691 0.4585 0.056 Uiso 1 1 calc R . . H32B H 0.5588 0.0093 0.4155 0.056 Uiso 1 1 calc R . . H32C H 0.5277 0.0679 0.4777 0.056 Uiso 1 1 calc R . . C33 C 0.53977(18) 0.19162(11) 0.39436(13) 0.0422(5) Uani 1 1 d . . . H33A H 0.6258 0.1998 0.4220 0.063 Uiso 1 1 calc R . . H33B H 0.4904 0.2008 0.4329 0.063 Uiso 1 1 calc R . . H33C H 0.5146 0.2251 0.3476 0.063 Uiso 1 1 calc R . . C40 C 0.51870(15) -0.03170(10) 0.23450(11) 0.0319(4) Uani 1 1 d . . . H40A H 0.5687 0.0083 0.2205 0.038 Uiso 1 1 calc R . . H40B H 0.5568 -0.0445 0.2925 0.038 Uiso 1 1 calc R . . C41 C 0.53757(17) -0.09858(10) 0.18394(11) 0.0331(4) Uani 1 1 d . . . H41A H 0.4889 -0.1401 0.1976 0.040 Uiso 1 1 calc R . . C42 C 0.4923(2) -0.08441(12) 0.09188(12) 0.0448(5) Uani 1 1 d . . . H42A H 0.4056 -0.0718 0.0780 0.067 Uiso 1 1 calc R . . H42B H 0.5040 -0.1287 0.0619 0.067 Uiso 1 1 calc R . . H42C H 0.5382 -0.0436 0.0767 0.067 Uiso 1 1 calc R . . C43 C 0.67035(18) -0.12276(12) 0.20495(13) 0.0442(5) Uani 1 1 d . . . H43A H 0.6973 -0.1357 0.2632 0.066 Uiso 1 1 calc R . . H43B H 0.7206 -0.0825 0.1935 0.066 Uiso 1 1 calc R . . H43C H 0.6785 -0.1656 0.1717 0.066 Uiso 1 1 calc R . . C50 C 0.27056(17) 0.06364(10) 0.12474(10) 0.0330(4) Uani 1 1 d . . . H50A H 0.2797 0.0315 0.0795 0.040 Uiso 1 1 calc R A 1 H50B H 0.1826 0.0660 0.1216 0.040 Uiso 1 1 calc R A 1 C51 C 0.3129(2) 0.14210(15) 0.10863(15) 0.0366(8) Uani 0.810(6) 1 d P B 1 H51A H 0.2896 0.1760 0.1486 0.044 Uiso 0.810(6) 1 calc PR B 1 C52 C 0.2499(3) 0.1696(2) 0.0227(2) 0.0488(9) Uani 0.810(6) 1 d P B 1 H52A H 0.2717 0.2212 0.0174 0.073 Uiso 0.810(6) 1 calc PR B 1 H52B H 0.1615 0.1656 0.0135 0.073 Uiso 0.810(6) 1 calc PR B 1 H52C H 0.2758 0.1399 -0.0180 0.073 Uiso 0.810(6) 1 calc PR B 1 C53 C 0.4509(3) 0.14745(17) 0.12309(16) 0.0397(7) Uani 0.810(6) 1 d P B 1 H53A H 0.4726 0.1971 0.1094 0.059 Uiso 0.810(6) 1 calc PR B 1 H53B H 0.4779 0.1116 0.0883 0.059 Uiso 0.810(6) 1 calc PR B 1 H53C H 0.4906 0.1371 0.1808 0.059 Uiso 0.810(6) 1 calc PR B 1 C51A C 0.3308(9) 0.1091(6) 0.0744(6) 0.032(3) Uiso 0.190(6) 1 d P B 2 H51B H 0.3885 0.0762 0.0556 0.039 Uiso 0.190(6) 1 calc PR B 2 C52A C 0.2447(14) 0.1415(9) -0.0023(9) 0.049(4) Uiso 0.190(6) 1 d P B 2 H52D H 0.1739 0.1629 0.0118 0.074 Uiso 0.190(6) 1 calc PR B 2 H52E H 0.2178 0.1026 -0.0432 0.074 Uiso 0.190(6) 1 calc PR B 2 H52F H 0.2871 0.1798 -0.0249 0.074 Uiso 0.190(6) 1 calc PR B 2 C53A C 0.4068(15) 0.1678(9) 0.1277(9) 0.050(4) Uiso 0.190(6) 1 d P B 2 H53D H 0.3530 0.2043 0.1425 0.075 Uiso 0.190(6) 1 calc PR B 2 H53E H 0.4586 0.1919 0.0975 0.075 Uiso 0.190(6) 1 calc PR B 2 H53F H 0.4578 0.1452 0.1776 0.075 Uiso 0.190(6) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0230(2) 0.0353(2) 0.0364(2) -0.00492(16) 0.00829(15) 0.00324(16) Al1 0.0226(3) 0.0253(3) 0.0241(2) -0.00095(19) 0.00847(18) -0.0001(2) N1 0.0257(7) 0.0274(7) 0.0254(7) 0.0000(6) 0.0074(5) -0.0023(6) N2 0.0293(8) 0.0493(10) 0.0415(8) 0.0063(8) 0.0076(7) -0.0009(8) N3 0.0262(8) 0.0400(9) 0.0422(8) 0.0028(7) 0.0124(6) 0.0018(7) N4 0.0322(8) 0.0364(9) 0.0334(8) 0.0042(6) 0.0121(6) 0.0024(7) C10 0.0319(9) 0.0327(9) 0.0274(8) 0.0012(7) 0.0100(7) -0.0023(8) C11 0.0412(11) 0.0442(12) 0.0374(10) 0.0034(8) 0.0189(8) -0.0012(9) C12 0.0405(11) 0.0465(12) 0.0523(12) 0.0006(10) 0.0230(9) -0.0083(10) C13 0.0305(10) 0.0399(11) 0.0474(11) -0.0070(9) 0.0106(8) -0.0058(9) C14 0.0272(9) 0.0321(9) 0.0307(8) -0.0001(7) 0.0054(7) -0.0038(8) C15 0.0432(11) 0.0402(11) 0.0411(10) 0.0098(9) 0.0136(8) 0.0052(9) C16 0.0421(11) 0.0408(11) 0.0410(10) -0.0104(9) 0.0163(9) -0.0099(9) C20 0.0259(10) 0.0687(15) 0.0506(12) 0.0114(11) 0.0059(9) -0.0017(10) C21 0.0276(10) 0.0573(14) 0.0539(12) 0.0102(10) 0.0135(9) 0.0081(9) C22 0.0325(11) 0.0484(12) 0.0542(12) -0.0027(10) 0.0202(9) 0.0049(9) C23 0.0414(11) 0.0514(12) 0.0400(10) -0.0001(9) 0.0217(9) 0.0024(10) C24 0.0485(14) 0.0820(19) 0.0405(11) -0.0012(12) 0.0016(9) -0.0012(13) C25 0.0430(13) 0.0584(15) 0.0691(15) 0.0170(12) 0.0188(11) -0.0015(11) C26 0.0334(10) 0.0450(12) 0.0572(12) 0.0040(10) 0.0184(9) -0.0008(9) C27 0.0430(12) 0.0423(12) 0.0530(12) -0.0002(10) 0.0137(10) -0.0036(10) C28 0.0500(14) 0.0753(17) 0.0434(11) 0.0167(11) 0.0137(10) 0.0168(12) C30 0.0225(8) 0.0299(9) 0.0302(8) -0.0012(7) 0.0080(7) 0.0013(7) C31 0.0242(9) 0.0288(9) 0.0318(8) -0.0023(7) 0.0088(7) 0.0000(7) C32 0.0353(10) 0.0427(11) 0.0314(9) -0.0015(8) 0.0044(7) 0.0042(9) C33 0.0323(10) 0.0343(11) 0.0580(12) -0.0099(9) 0.0085(9) -0.0028(9) C40 0.0268(9) 0.0335(10) 0.0377(9) -0.0051(8) 0.0125(7) -0.0007(8) C41 0.0327(10) 0.0319(10) 0.0389(9) -0.0050(8) 0.0166(8) -0.0043(8) C42 0.0492(12) 0.0512(13) 0.0383(10) -0.0067(9) 0.0194(9) 0.0022(10) C43 0.0396(12) 0.0384(11) 0.0568(12) -0.0087(10) 0.0167(10) 0.0071(9) C50 0.0337(10) 0.0362(10) 0.0299(8) 0.0018(7) 0.0096(7) 0.0003(8) C51 0.0397(15) 0.0373(15) 0.0345(13) 0.0068(11) 0.0130(10) 0.0051(11) C52 0.0444(16) 0.055(2) 0.0479(18) 0.0244(17) 0.0131(13) 0.0058(15) C53 0.0391(16) 0.0390(15) 0.0430(14) 0.0094(11) 0.0146(12) -0.0024(13) _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 K1 N3 2.8386(15) . ? K1 N1 2.8675(15) . ? K1 N2 2.8720(16) . ? K1 N4 2.9446(15) . ? K1 C30 3.0483(17) . ? K1 Al1 3.3389(6) . ? Al1 N1 1.8918(14) . ? Al1 C40 2.0236(17) . ? Al1 C50 2.0344(18) . ? Al1 C30 2.0470(17) . ? N1 C14 1.468(2) . ? N1 C10 1.473(2) . ? N2 C25 1.454(3) . ? N2 C20 1.465(2) . ? N2 C24 1.470(3) . ? N3 C26 1.456(3) . ? N3 C22 1.467(2) . ? N3 C21 1.474(2) . ? N4 C27 1.450(2) . ? N4 C28 1.463(3) . ? N4 C23 1.466(2) . ? C10 C15 1.538(3) . ? C10 C11 1.541(2) . ? C10 H10A 1.0000 . ? C11 C12 1.527(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.533(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.542(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C16 1.537(3) . ? C14 H14A 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C20 C21 1.520(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.518(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C30 C31 1.539(2) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.521(2) . ? C31 C33 1.521(2) . ? C31 H31A 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C40 C41 1.534(2) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C43 1.525(3) . ? C41 C42 1.527(3) . ? C41 H41A 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C50 C51A 1.479(10) . ? C50 C51 1.554(3) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.526(3) . ? C51 C53 1.528(4) . ? C51 H51A 1.0000 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C51A C53A 1.513(18) . ? C51A C52A 1.524(18) . ? C51A H51B 1.0000 . ? C52A H52D 0.9800 . ? C52A H52E 0.9800 . ? C52A H52F 0.9800 . ? C53A H53D 0.9800 . ? C53A H53E 0.9800 . ? C53A H53F 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 N3 K1 N1 136.96(4) . . ? N3 K1 N2 63.44(4) . . ? N1 K1 N2 112.96(5) . . ? N3 K1 N4 62.02(4) . . ? N1 K1 N4 119.79(4) . . ? N2 K1 N4 121.93(5) . . ? N3 K1 C30 148.33(5) . . ? N1 K1 C30 63.99(4) . . ? N2 K1 C30 139.19(5) . . ? N4 K1 C30 87.34(4) . . ? N3 K1 Al1 171.39(4) . . ? N1 K1 Al1 34.44(3) . . ? N2 K1 Al1 116.75(4) . . ? N4 K1 Al1 120.22(3) . . ? C30 K1 Al1 37.03(3) . . ? N1 Al1 C40 117.35(7) . . ? N1 Al1 C50 104.83(7) . . ? C40 Al1 C50 114.78(7) . . ? N1 Al1 C30 105.56(6) . . ? C40 Al1 C30 106.75(7) . . ? C50 Al1 C30 106.79(7) . . ? N1 Al1 K1 59.01(4) . . ? C40 Al1 K1 165.64(5) . . ? C50 Al1 K1 79.11(5) . . ? C30 Al1 K1 63.75(5) . . ? C14 N1 C10 115.81(13) . . ? C14 N1 Al1 121.30(10) . . ? C10 N1 Al1 117.93(11) . . ? C14 N1 K1 100.88(10) . . ? C10 N1 K1 105.14(9) . . ? Al1 N1 K1 86.55(5) . . ? C25 N2 C20 111.02(18) . . ? C25 N2 C24 110.00(17) . . ? C20 N2 C24 108.90(16) . . ? C25 N2 K1 93.63(12) . . ? C20 N2 K1 113.75(11) . . ? C24 N2 K1 118.57(13) . . ? C26 N3 C22 110.80(15) . . ? C26 N3 C21 111.13(16) . . ? C22 N3 C21 109.28(15) . . ? C26 N3 K1 96.60(11) . . ? C22 N3 K1 115.63(11) . . ? C21 N3 K1 112.86(10) . . ? C27 N4 C28 109.46(17) . . ? C27 N4 C23 111.21(16) . . ? C28 N4 C23 109.40(15) . . ? C27 N4 K1 93.44(11) . . ? C28 N4 K1 119.16(12) . . ? C23 N4 K1 113.07(11) . . ? N1 C10 C15 116.05(14) . . ? N1 C10 C11 111.77(14) . . ? C15 C10 C11 110.25(15) . . ? N1 C10 H10A 106.0 . . ? C15 C10 H10A 106.0 . . ? C11 C10 H10A 106.0 . . ? C12 C11 C10 111.75(15) . . ? C12 C11 H11A 109.3 . . ? C10 C11 H11A 109.3 . . ? C12 C11 H11B 109.3 . . ? C10 C11 H11B 109.3 . . ? H11A C11 H11B 107.9 . . ? C11 C12 C13 109.97(16) . . ? C11 C12 H12A 109.7 . . ? C13 C12 H12A 109.7 . . ? C11 C12 H12B 109.7 . . ? C13 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? C12 C13 C14 111.97(16) . . ? C12 C13 H13A 109.2 . . ? C14 C13 H13A 109.2 . . ? C12 C13 H13B 109.2 . . ? C14 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? N1 C14 C16 115.80(15) . . ? N1 C14 C13 111.90(14) . . ? C16 C14 C13 110.44(15) . . ? N1 C14 H14A 106.0 . . ? C16 C14 H14A 106.0 . . ? C13 C14 H14A 106.0 . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C20 C21 114.38(17) . . ? N2 C20 H20A 108.7 . . ? C21 C20 H20A 108.7 . . ? N2 C20 H20B 108.7 . . ? C21 C20 H20B 108.7 . . ? H20A C20 H20B 107.6 . . ? N3 C21 C20 114.46(17) . . ? N3 C21 H21A 108.6 . . ? C20 C21 H21A 108.6 . . ? N3 C21 H21B 108.6 . . ? C20 C21 H21B 108.6 . . ? H21A C21 H21B 107.6 . . ? N3 C22 C23 114.10(16) . . ? N3 C22 H22A 108.7 . . ? C23 C22 H22A 108.7 . . ? N3 C22 H22B 108.7 . . ? C23 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? N4 C23 C22 113.85(15) . . ? N4 C23 H23A 108.8 . . ? C22 C23 H23A 108.8 . . ? N4 C23 H23B 108.8 . . ? C22 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? N2 C24 H24A 109.5 . . ? N2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N2 C25 H25A 109.5 . . ? N2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N3 C26 H26A 109.5 . . ? N3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N4 C27 H27A 109.5 . . ? N4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N4 C28 H28A 109.5 . . ? N4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C31 C30 Al1 118.30(11) . . ? C31 C30 K1 161.93(11) . . ? Al1 C30 K1 79.22(5) . . ? C31 C30 H30A 107.7 . . ? Al1 C30 H30A 107.7 . . ? K1 C30 H30A 67.8 . . ? C31 C30 H30B 107.7 . . ? Al1 C30 H30B 107.7 . . ? K1 C30 H30B 59.5 . . ? H30A C30 H30B 107.1 . . ? C32 C31 C33 109.94(15) . . ? C32 C31 C30 110.67(14) . . ? C33 C31 C30 113.36(14) . . ? C32 C31 H31A 107.5 . . ? C33 C31 H31A 107.5 . . ? C30 C31 H31A 107.5 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 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 . . ? C41 C40 Al1 125.31(13) . . ? C41 C40 H40A 106.0 . . ? Al1 C40 H40A 106.0 . . ? C41 C40 H40B 106.0 . . ? Al1 C40 H40B 106.0 . . ? H40A C40 H40B 106.3 . . ? C43 C41 C42 109.57(15) . . ? C43 C41 C40 112.00(15) . . ? C42 C41 C40 111.99(16) . . ? C43 C41 H41A 107.7 . . ? C42 C41 H41A 107.7 . . ? C40 C41 H41A 107.7 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C51A C50 C51 34.2(4) . . ? C51A C50 Al1 125.3(4) . . ? C51 C50 Al1 117.82(13) . . ? C51A C50 H50A 74.1 . . ? C51 C50 H50A 107.9 . . ? Al1 C50 H50A 107.9 . . ? C51A C50 H50B 124.1 . . ? C51 C50 H50B 107.9 . . ? Al1 C50 H50B 107.9 . . ? H50A C50 H50B 107.2 . . ? C52 C51 C53 109.8(2) . . ? C52 C51 C50 112.2(2) . . ? C53 C51 C50 112.6(2) . . ? C52 C51 H51A 107.3 . . ? C53 C51 H51A 107.3 . . ? C50 C51 H51A 107.3 . . ? C50 C51A C53A 109.3(9) . . ? C50 C51A C52A 114.4(9) . . ? C53A C51A C52A 111.9(10) . . ? C50 C51A H51B 106.9 . . ? C53A C51A H51B 106.9 . . ? C52A C51A H51B 106.9 . . ? C51A C52A H52D 109.5 . . ? C51A C52A H52E 109.5 . . ? H52D C52A H52E 109.5 . . ? C51A C52A H52F 109.5 . . ? H52D C52A H52F 109.5 . . ? H52E C52A H52F 109.5 . . ? C51A C53A H53D 109.5 . . ? C51A C53A H53E 109.5 . . ? H53D C53A H53E 109.5 . . ? C51A C53A H53F 109.5 . . ? H53D C53A H53F 109.5 . . ? H53E C53A H53F 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 N3 K1 Al1 N1 -3.1(2) . . . . ? N2 K1 Al1 N1 -92.15(6) . . . . ? N4 K1 Al1 N1 99.63(6) . . . . ? C30 K1 Al1 N1 130.18(7) . . . . ? N3 K1 Al1 C40 -82.4(3) . . . . ? N1 K1 Al1 C40 -79.3(2) . . . . ? N2 K1 Al1 C40 -171.5(2) . . . . ? N4 K1 Al1 C40 20.3(2) . . . . ? C30 K1 Al1 C40 50.9(2) . . . . ? N3 K1 Al1 C50 111.7(2) . . . . ? N1 K1 Al1 C50 114.81(7) . . . . ? N2 K1 Al1 C50 22.66(7) . . . . ? N4 K1 Al1 C50 -145.56(7) . . . . ? C30 K1 Al1 C50 -115.01(8) . . . . ? N3 K1 Al1 C30 -133.3(2) . . . . ? N1 K1 Al1 C30 -130.18(7) . . . . ? N2 K1 Al1 C30 137.67(7) . . . . ? N4 K1 Al1 C30 -30.56(7) . . . . ? C40 Al1 N1 C14 -95.28(14) . . . . ? C50 Al1 N1 C14 33.40(14) . . . . ? C30 Al1 N1 C14 145.98(13) . . . . ? K1 Al1 N1 C14 100.64(13) . . . . ? C40 Al1 N1 C10 58.76(14) . . . . ? C50 Al1 N1 C10 -172.55(12) . . . . ? C30 Al1 N1 C10 -59.98(13) . . . . ? K1 Al1 N1 C10 -105.31(12) . . . . ? C40 Al1 N1 K1 164.08(6) . . . . ? C50 Al1 N1 K1 -67.24(6) . . . . ? C30 Al1 N1 K1 45.34(6) . . . . ? N3 K1 N1 C14 58.10(11) . . . . ? N2 K1 N1 C14 -16.96(10) . . . . ? N4 K1 N1 C14 137.78(9) . . . . ? C30 K1 N1 C14 -152.02(10) . . . . ? Al1 K1 N1 C14 -121.23(11) . . . . ? N3 K1 N1 C10 -62.66(12) . . . . ? N2 K1 N1 C10 -137.71(10) . . . . ? N4 K1 N1 C10 17.03(11) . . . . ? C30 K1 N1 C10 87.22(10) . . . . ? Al1 K1 N1 C10 118.02(11) . . . . ? N3 K1 N1 Al1 179.32(5) . . . . ? N2 K1 N1 Al1 104.27(5) . . . . ? N4 K1 N1 Al1 -100.99(5) . . . . ? C30 K1 N1 Al1 -30.80(5) . . . . ? N3 K1 N2 C25 105.17(13) . . . . ? N1 K1 N2 C25 -122.34(12) . . . . ? N4 K1 N2 C25 83.54(12) . . . . ? C30 K1 N2 C25 -46.11(15) . . . . ? Al1 K1 N2 C25 -84.47(12) . . . . ? N3 K1 N2 C20 -9.71(14) . . . . ? N1 K1 N2 C20 122.79(14) . . . . ? N4 K1 N2 C20 -31.34(16) . . . . ? C30 K1 N2 C20 -160.98(13) . . . . ? Al1 K1 N2 C20 160.66(13) . . . . ? N3 K1 N2 C24 -139.70(16) . . . . ? N1 K1 N2 C24 -7.20(15) . . . . ? N4 K1 N2 C24 -161.33(14) . . . . ? C30 K1 N2 C24 69.02(17) . . . . ? Al1 K1 N2 C24 30.66(15) . . . . ? N1 K1 N3 C26 3.24(14) . . . . ? N2 K1 N3 C26 99.19(12) . . . . ? N4 K1 N3 C26 -101.56(12) . . . . ? C30 K1 N3 C26 -117.55(13) . . . . ? Al1 K1 N3 C26 5.8(3) . . . . ? N1 K1 N3 C22 120.11(13) . . . . ? N2 K1 N3 C22 -143.94(14) . . . . ? N4 K1 N3 C22 15.31(12) . . . . ? C30 K1 N3 C22 -0.68(18) . . . . ? Al1 K1 N3 C22 122.7(2) . . . . ? N1 K1 N3 C21 -113.03(13) . . . . ? N2 K1 N3 C21 -17.08(13) . . . . ? N4 K1 N3 C21 142.17(15) . . . . ? C30 K1 N3 C21 126.17(14) . . . . ? Al1 K1 N3 C21 -110.5(2) . . . . ? N3 K1 N4 C27 -102.71(12) . . . . ? N1 K1 N4 C27 126.79(11) . . . . ? N2 K1 N4 C27 -80.79(12) . . . . ? C30 K1 N4 C27 68.96(11) . . . . ? Al1 K1 N4 C27 86.81(11) . . . . ? N3 K1 N4 C28 142.72(16) . . . . ? N1 K1 N4 C28 12.23(16) . . . . ? N2 K1 N4 C28 164.65(14) . . . . ? C30 K1 N4 C28 -45.60(15) . . . . ? Al1 K1 N4 C28 -27.75(16) . . . . ? N3 K1 N4 C23 12.10(12) . . . . ? N1 K1 N4 C23 -118.40(12) . . . . ? N2 K1 N4 C23 34.03(14) . . . . ? C30 K1 N4 C23 -176.23(13) . . . . ? Al1 K1 N4 C23 -158.38(11) . . . . ? C14 N1 C10 C15 76.38(19) . . . . ? Al1 N1 C10 C15 -79.08(17) . . . . ? K1 N1 C10 C15 -173.25(13) . . . . ? C14 N1 C10 C11 -51.22(19) . . . . ? Al1 N1 C10 C11 153.32(12) . . . . ? K1 N1 C10 C11 59.14(15) . . . . ? N1 C10 C11 C12 52.7(2) . . . . ? C15 C10 C11 C12 -78.0(2) . . . . ? C10 C11 C12 C13 -54.7(2) . . . . ? C11 C12 C13 C14 54.2(2) . . . . ? C10 N1 C14 C16 -77.01(18) . . . . ? Al1 N1 C14 C16 77.55(18) . . . . ? K1 N1 C14 C16 170.14(12) . . . . ? C10 N1 C14 C13 50.7(2) . . . . ? Al1 N1 C14 C13 -154.69(12) . . . . ? K1 N1 C14 C13 -62.11(15) . . . . ? C12 C13 C14 N1 -51.8(2) . . . . ? C12 C13 C14 C16 78.80(19) . . . . ? C25 N2 C20 C21 -68.3(2) . . . . ? C24 N2 C20 C21 170.47(19) . . . . ? K1 N2 C20 C21 35.8(2) . . . . ? C26 N3 C21 C20 -63.8(2) . . . . ? C22 N3 C21 C20 173.64(16) . . . . ? K1 N3 C21 C20 43.5(2) . . . . ? N2 C20 C21 N3 -55.1(3) . . . . ? C26 N3 C22 C23 66.4(2) . . . . ? C21 N3 C22 C23 -170.81(16) . . . . ? K1 N3 C22 C23 -42.2(2) . . . . ? C27 N4 C23 C22 65.4(2) . . . . ? C28 N4 C23 C22 -173.60(19) . . . . ? K1 N4 C23 C22 -38.2(2) . . . . ? N3 C22 C23 N4 55.2(2) . . . . ? N1 Al1 C30 C31 132.44(12) . . . . ? C40 Al1 C30 C31 6.86(15) . . . . ? C50 Al1 C30 C31 -116.36(13) . . . . ? K1 Al1 C30 C31 175.28(14) . . . . ? N1 Al1 C30 K1 -42.83(6) . . . . ? C40 Al1 C30 K1 -168.41(6) . . . . ? C50 Al1 C30 K1 68.36(6) . . . . ? N3 K1 C30 C31 1.5(4) . . . . ? N1 K1 C30 C31 -137.7(4) . . . . ? N2 K1 C30 C31 126.6(4) . . . . ? N4 K1 C30 C31 -12.6(4) . . . . ? Al1 K1 C30 C31 -166.5(4) . . . . ? N3 K1 C30 Al1 168.01(7) . . . . ? N1 K1 C30 Al1 28.74(4) . . . . ? N2 K1 C30 Al1 -66.95(9) . . . . ? N4 K1 C30 Al1 153.91(6) . . . . ? Al1 C30 C31 C32 -84.41(15) . . . . ? K1 C30 C31 C32 80.5(4) . . . . ? Al1 C30 C31 C33 151.54(13) . . . . ? K1 C30 C31 C33 -43.6(4) . . . . ? N1 Al1 C40 C41 56.35(17) . . . . ? C50 Al1 C40 C41 -67.44(17) . . . . ? C30 Al1 C40 C41 174.46(14) . . . . ? K1 Al1 C40 C41 127.9(2) . . . . ? Al1 C40 C41 C43 -175.44(13) . . . . ? Al1 C40 C41 C42 61.0(2) . . . . ? N1 Al1 C50 C51A -170.8(6) . . . . ? C40 Al1 C50 C51A -40.6(6) . . . . ? C30 Al1 C50 C51A 77.5(6) . . . . ? K1 Al1 C50 C51A 135.6(6) . . . . ? N1 Al1 C50 C51 149.81(15) . . . . ? C40 Al1 C50 C51 -79.98(16) . . . . ? C30 Al1 C50 C51 38.10(17) . . . . ? K1 Al1 C50 C51 96.20(15) . . . . ? C51A C50 C51 C52 61.9(7) . . . . ? Al1 C50 C51 C52 174.57(17) . . . . ? C51A C50 C51 C53 -62.6(7) . . . . ? Al1 C50 C51 C53 50.1(3) . . . . ? C51 C50 C51A C53A 36.6(9) . . . . ? Al1 C50 C51A C53A -52.0(12) . . . . ? C51 C50 C51A C52A -89.8(11) . . . . ? Al1 C50 C51A C52A -178.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.482 _refine_diff_density_min -0.328 _refine_diff_density_rms 0.085 #===END ################################################################### ################## COMPOUND 8 ##################################### ################################################################## data_pgaben17 _database_code_depnum_ccdc_archive 'CCDC 771328' #TrackingRef '- all3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H68 Al K N4 Si2' _chemical_formula_weight 571.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' 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' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.5276(6) _cell_length_b 18.4028(8) _cell_length_c 17.3602(9) _cell_angle_alpha 90.00 _cell_angle_beta 93.669(5) _cell_angle_gamma 90.00 _cell_volume 3675.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9261 _cell_measurement_theta_min 2.4450 _cell_measurement_theta_max 30.7248 _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.032 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 0.254 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.96303 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Oxford Diffraction Gemini S' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 49892 _diffrn_reflns_av_R_equivalents 0.0786 _diffrn_reflns_av_sigmaI/netI 0.1145 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 29.00 _reflns_number_total 9769 _reflns_number_gt 5330 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0176(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9769 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0843 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.0984 _refine_ls_wR_factor_gt 0.0887 _refine_ls_goodness_of_fit_ref 0.796 _refine_ls_restrained_S_all 0.796 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.25912(5) 0.31670(3) 0.64442(3) 0.01972(13) Uani 1 1 d . . . K1 K 0.49957(4) 0.19612(2) 0.61705(2) 0.02424(11) Uani 1 1 d . . . Si1 Si 0.23926(5) 0.15377(3) 0.70205(3) 0.02217(13) Uani 1 1 d . . . Si2 Si 0.17857(5) 0.18392(3) 0.53623(3) 0.02177(13) Uani 1 1 d . . . N1 N 0.24014(13) 0.21227(7) 0.62449(8) 0.0194(3) Uani 1 1 d . . . N2 N 0.66534(14) 0.14652(8) 0.74061(9) 0.0281(4) Uani 1 1 d . . . N3 N 0.68323(14) 0.10737(8) 0.57019(9) 0.0260(4) Uani 1 1 d . . . N4 N 0.63925(14) 0.25793(8) 0.50675(9) 0.0284(4) Uani 1 1 d . . . C1 C 0.42441(16) 0.33564(9) 0.69053(10) 0.0222(4) Uani 1 1 d . . . H1A H 0.4481 0.2934 0.7232 0.027 Uiso 1 1 calc R . . H1B H 0.4767 0.3371 0.6475 0.027 Uiso 1 1 calc R . . C2 C 0.44652(17) 0.40503(9) 0.73939(10) 0.0263(4) Uani 1 1 d . . . H2 H 0.3960 0.4444 0.7160 0.032 Uiso 1 1 calc R . . C3 C 0.41359(19) 0.39415(11) 0.82168(11) 0.0353(5) Uani 1 1 d . . . H3A H 0.4617 0.3555 0.8460 0.053 Uiso 1 1 calc R . . H3B H 0.3315 0.3804 0.8216 0.053 Uiso 1 1 calc R . . H3C H 0.4263 0.4395 0.8507 0.053 Uiso 1 1 calc R . . C4 C 0.5727(2) 0.43070(12) 0.73952(13) 0.0445(6) Uani 1 1 d . . . H4A H 0.5824 0.4749 0.7707 0.067 Uiso 1 1 calc R . . H4B H 0.5921 0.4410 0.6865 0.067 Uiso 1 1 calc R . . H4C H 0.6243 0.3926 0.7615 0.067 Uiso 1 1 calc R . . C5 C 0.26063(17) 0.37213(9) 0.54344(10) 0.0247(4) Uani 1 1 d . . . H5A H 0.2989 0.3413 0.5058 0.030 Uiso 1 1 calc R . . H5B H 0.1791 0.3794 0.5234 0.030 Uiso 1 1 calc R . . C6 C 0.32152(18) 0.44686(9) 0.54633(10) 0.0266(4) Uani 1 1 d . . . H6 H 0.3980 0.4412 0.5763 0.032 Uiso 1 1 calc R . . C7 C 0.34505(19) 0.47596(10) 0.46605(11) 0.0341(5) Uani 1 1 d . . . H7A H 0.2711 0.4834 0.4361 0.051 Uiso 1 1 calc R . . H7B H 0.3923 0.4408 0.4395 0.051 Uiso 1 1 calc R . . H7C H 0.3869 0.5222 0.4713 0.051 Uiso 1 1 calc R . . C8 C 0.2504(2) 0.50316(10) 0.58748(12) 0.0377(5) Uani 1 1 d . . . H8A H 0.1773 0.5122 0.5571 0.057 Uiso 1 1 calc R . . H8B H 0.2947 0.5485 0.5931 0.057 Uiso 1 1 calc R . . H8C H 0.2337 0.4849 0.6386 0.057 Uiso 1 1 calc R . . C9 C 0.14068(16) 0.34757(10) 0.71815(11) 0.0254(4) Uani 1 1 d . . . H9A H 0.1519 0.3156 0.7639 0.030 Uiso 1 1 calc R . . H9B H 0.1628 0.3972 0.7357 0.030 Uiso 1 1 calc R . . C10 C 0.00903(17) 0.34950(10) 0.69672(12) 0.0309(5) Uani 1 1 d . . . H10 H -0.0137 0.3013 0.6738 0.037 Uiso 1 1 calc R . . C11 C -0.02272(19) 0.40770(11) 0.63645(12) 0.0381(5) Uani 1 1 d . . . H11A H -0.1072 0.4083 0.6254 0.057 Uiso 1 1 calc R . . H11B H 0.0156 0.3969 0.5890 0.057 Uiso 1 1 calc R . . H11C H 0.0031 0.4553 0.6562 0.057 Uiso 1 1 calc R . . C12 C -0.0610(2) 0.36098(12) 0.76709(14) 0.0491(6) Uani 1 1 d . . . H12A H -0.0393 0.4075 0.7914 0.074 Uiso 1 1 calc R . . H12B H -0.0446 0.3215 0.8041 0.074 Uiso 1 1 calc R . . H12C H -0.1441 0.3613 0.7511 0.074 Uiso 1 1 calc R . . C13 C 0.32515(18) 0.18855(10) 0.78981(10) 0.0273(4) Uani 1 1 d . . . H13A H 0.4073 0.1924 0.7789 0.041 Uiso 1 1 calc R . . H13B H 0.3171 0.1549 0.8329 0.041 Uiso 1 1 calc R . . H13C H 0.2959 0.2365 0.8035 0.041 Uiso 1 1 calc R . . C14 C 0.31254(19) 0.06404(10) 0.68257(11) 0.0325(5) Uani 1 1 d . . . H14A H 0.2549 0.0299 0.6597 0.049 Uiso 1 1 calc R . . H14B H 0.3468 0.0440 0.7312 0.049 Uiso 1 1 calc R . . H14C H 0.3738 0.0718 0.6468 0.049 Uiso 1 1 calc R . . C15 C 0.09029(17) 0.13447(11) 0.73372(12) 0.0351(5) Uani 1 1 d . . . H15A H 0.0554 0.1796 0.7513 0.053 Uiso 1 1 calc R . . H15B H 0.0955 0.0992 0.7761 0.053 Uiso 1 1 calc R . . H15C H 0.0419 0.1145 0.6903 0.053 Uiso 1 1 calc R . . C16 C 0.29222(18) 0.17532(10) 0.46396(11) 0.0333(5) Uani 1 1 d . . . H16A H 0.3339 0.2215 0.4605 0.050 Uiso 1 1 calc R . . H16B H 0.2549 0.1631 0.4133 0.050 Uiso 1 1 calc R . . H16C H 0.3472 0.1369 0.4803 0.050 Uiso 1 1 calc R . . C17 C 0.05876(17) 0.24457(10) 0.49591(11) 0.0302(5) Uani 1 1 d . . . H17A H 0.0091 0.2585 0.5372 0.045 Uiso 1 1 calc R . . H17B H 0.0122 0.2186 0.4555 0.045 Uiso 1 1 calc R . . H17C H 0.0924 0.2883 0.4740 0.045 Uiso 1 1 calc R . . C18 C 0.10697(19) 0.09168(10) 0.53517(12) 0.0337(5) Uani 1 1 d . . . H18A H 0.1631 0.0553 0.5553 0.051 Uiso 1 1 calc R . . H18B H 0.0802 0.0791 0.4821 0.051 Uiso 1 1 calc R . . H18C H 0.0404 0.0928 0.5676 0.051 Uiso 1 1 calc R . . C19 C 0.57214(19) 0.30127(11) 0.44896(13) 0.0421(6) Uani 1 1 d . . . H19A H 0.5256 0.3372 0.4750 0.063 Uiso 1 1 calc R . . H19B H 0.5206 0.2693 0.4172 0.063 Uiso 1 1 calc R . . H19C H 0.6253 0.3263 0.4160 0.063 Uiso 1 1 calc R . . C20 C 0.7186(2) 0.30598(11) 0.55241(13) 0.0419(6) Uani 1 1 d . . . H20A H 0.7753 0.3269 0.5190 0.063 Uiso 1 1 calc R . . H20B H 0.7593 0.2780 0.5939 0.063 Uiso 1 1 calc R . . H20C H 0.6740 0.3451 0.5748 0.063 Uiso 1 1 calc R . . C21 C 0.70379(19) 0.20146(10) 0.46806(11) 0.0335(5) Uani 1 1 d . . . H21A H 0.7632 0.2251 0.4378 0.040 Uiso 1 1 calc R . . H21B H 0.6494 0.1753 0.4314 0.040 Uiso 1 1 calc R . . C22 C 0.76349(18) 0.14669(10) 0.52259(11) 0.0308(5) Uani 1 1 d . . . H22A H 0.8055 0.1111 0.4920 0.037 Uiso 1 1 calc R . . H22B H 0.8218 0.1724 0.5570 0.037 Uiso 1 1 calc R . . C23 C 0.6181(2) 0.05261(11) 0.52411(13) 0.0435(6) Uani 1 1 d . . . H23A H 0.6722 0.0165 0.5054 0.065 Uiso 1 1 calc R . . H23B H 0.5761 0.0761 0.4800 0.065 Uiso 1 1 calc R . . H23C H 0.5625 0.0285 0.5560 0.065 Uiso 1 1 calc R . . C24 C 0.74772(18) 0.07298(10) 0.63631(11) 0.0321(5) Uani 1 1 d . . . H24A H 0.8227 0.0544 0.6196 0.039 Uiso 1 1 calc R . . H24B H 0.7026 0.0310 0.6538 0.039 Uiso 1 1 calc R . . C25 C 0.77092(18) 0.12443(11) 0.70272(12) 0.0351(5) Uani 1 1 d . . . H25A H 0.8255 0.1010 0.7415 0.042 Uiso 1 1 calc R . . H25B H 0.8094 0.1685 0.6838 0.042 Uiso 1 1 calc R . . C26 C 0.6966(2) 0.20740(12) 0.79212(13) 0.0522(7) Uani 1 1 d . . . H26A H 0.6274 0.2242 0.8168 0.078 Uiso 1 1 calc R . . H26B H 0.7279 0.2472 0.7622 0.078 Uiso 1 1 calc R . . H26C H 0.7555 0.1915 0.8318 0.078 Uiso 1 1 calc R . . C27 C 0.6223(2) 0.08643(12) 0.78598(13) 0.0497(6) Uani 1 1 d . . . H27A H 0.6851 0.0684 0.8217 0.075 Uiso 1 1 calc R . . H27B H 0.5951 0.0471 0.7513 0.075 Uiso 1 1 calc R . . H27C H 0.5578 0.1035 0.8154 0.075 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 0.0216(3) 0.0165(3) 0.0208(3) -0.0006(2) -0.0005(2) -0.0003(2) K1 0.0222(2) 0.0241(2) 0.0265(2) -0.00020(17) 0.00182(17) 0.00197(17) Si1 0.0236(3) 0.0194(3) 0.0234(3) 0.0018(2) 0.0001(2) -0.0015(2) Si2 0.0236(3) 0.0192(3) 0.0221(3) -0.0018(2) -0.0019(2) -0.0016(2) N1 0.0194(9) 0.0171(7) 0.0214(8) -0.0007(6) -0.0003(6) -0.0009(6) N2 0.0286(10) 0.0289(9) 0.0263(9) 0.0005(7) -0.0011(7) 0.0013(7) N3 0.0271(10) 0.0210(8) 0.0297(9) 0.0002(7) 0.0004(7) 0.0003(7) N4 0.0291(10) 0.0256(8) 0.0310(9) 0.0063(7) 0.0045(8) 0.0027(7) C1 0.0269(11) 0.0184(9) 0.0211(10) 0.0009(7) 0.0002(8) -0.0002(8) C2 0.0318(12) 0.0202(9) 0.0261(11) -0.0015(8) -0.0052(9) -0.0020(8) C3 0.0450(15) 0.0329(11) 0.0273(11) -0.0061(9) -0.0042(10) 0.0016(10) C4 0.0431(15) 0.0416(13) 0.0483(14) -0.0133(11) -0.0023(11) -0.0161(11) C5 0.0263(11) 0.0200(9) 0.0272(11) -0.0013(8) -0.0026(8) 0.0000(8) C6 0.0339(12) 0.0210(9) 0.0243(10) 0.0035(8) -0.0043(9) -0.0035(8) C7 0.0440(14) 0.0265(10) 0.0314(12) 0.0066(9) -0.0017(10) -0.0034(9) C8 0.0536(16) 0.0223(10) 0.0371(13) -0.0008(9) 0.0015(11) -0.0030(10) C9 0.0278(12) 0.0200(9) 0.0282(10) -0.0013(8) 0.0001(9) 0.0008(8) C10 0.0247(12) 0.0250(10) 0.0433(13) -0.0028(9) 0.0036(9) 0.0015(9) C11 0.0287(13) 0.0365(12) 0.0483(14) -0.0037(10) -0.0037(10) 0.0079(10) C12 0.0358(15) 0.0538(15) 0.0596(16) 0.0099(12) 0.0176(12) 0.0098(11) C13 0.0328(12) 0.0249(10) 0.0240(10) 0.0042(8) 0.0004(8) -0.0009(9) C14 0.0399(14) 0.0235(10) 0.0333(12) 0.0024(9) -0.0036(10) 0.0012(9) C15 0.0317(13) 0.0390(12) 0.0348(12) 0.0044(9) 0.0032(10) -0.0064(10) C16 0.0406(14) 0.0346(11) 0.0245(11) -0.0065(9) 0.0021(10) -0.0015(9) C17 0.0315(13) 0.0262(10) 0.0315(11) -0.0043(8) -0.0087(9) -0.0008(9) C18 0.0406(14) 0.0257(10) 0.0337(12) -0.0037(9) -0.0057(10) -0.0037(9) C19 0.0344(14) 0.0398(12) 0.0519(14) 0.0176(11) 0.0001(11) 0.0005(10) C20 0.0459(15) 0.0338(12) 0.0458(14) 0.0014(10) 0.0013(11) 0.0002(10) C21 0.0361(13) 0.0372(12) 0.0281(11) 0.0035(9) 0.0088(9) 0.0012(10) C22 0.0293(12) 0.0321(11) 0.0320(11) -0.0001(9) 0.0094(9) 0.0055(9) C23 0.0501(16) 0.0313(12) 0.0484(14) -0.0073(10) -0.0027(12) -0.0043(10) C24 0.0319(13) 0.0260(10) 0.0386(12) 0.0054(9) 0.0037(10) 0.0078(9) C25 0.0289(13) 0.0381(12) 0.0377(13) 0.0081(10) -0.0039(10) 0.0024(9) C26 0.0534(17) 0.0551(15) 0.0463(15) -0.0153(12) -0.0104(12) 0.0026(13) C27 0.0407(16) 0.0600(15) 0.0484(15) 0.0235(12) 0.0024(12) 0.0028(12) _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 N1 1.9626(14) . ? Al1 C9 2.0122(19) . ? Al1 C5 2.0292(18) . ? Al1 C1 2.0489(19) . ? Al1 K1 3.6058(7) . ? K1 N4 2.8192(16) . ? K1 N3 2.8341(16) . ? K1 N2 2.9260(16) . ? K1 N1 3.0164(15) . ? K1 Si1 3.5151(7) . ? K1 Si2 3.8791(7) . ? Si1 N1 1.7245(15) . ? Si1 C15 1.870(2) . ? Si1 C13 1.8756(18) . ? Si1 C14 1.8951(19) . ? Si2 N1 1.7274(14) . ? Si2 C17 1.8759(19) . ? Si2 C16 1.878(2) . ? Si2 C18 1.8871(19) . ? N2 C27 1.463(2) . ? N2 C26 1.464(2) . ? N2 C25 1.477(2) . ? N3 C23 1.463(2) . ? N3 C22 1.470(2) . ? N3 C24 1.470(2) . ? N4 C19 1.463(2) . ? N4 C21 1.466(2) . ? N4 C20 1.467(3) . ? C1 C2 1.545(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.515(3) . ? C2 C4 1.529(3) . ? C2 H2 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.543(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C8 1.527(3) . ? C6 C7 1.533(2) . ? C6 H6 1.0000 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.540(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C12 1.521(3) . ? C10 C11 1.525(3) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.517(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.503(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 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 N1 Al1 C9 108.42(7) . . ? N1 Al1 C5 110.30(7) . . ? C9 Al1 C5 116.83(8) . . ? N1 Al1 C1 109.01(7) . . ? C9 Al1 C1 110.81(8) . . ? C5 Al1 C1 101.12(8) . . ? N1 Al1 K1 56.78(5) . . ? C9 Al1 K1 144.70(6) . . ? C5 Al1 K1 98.42(6) . . ? C1 Al1 K1 56.81(5) . . ? N4 K1 N3 64.40(4) . . ? N4 K1 N2 104.43(5) . . ? N3 K1 N2 64.27(4) . . ? N4 K1 N1 126.89(4) . . ? N3 K1 N1 146.09(4) . . ? N2 K1 N1 127.02(4) . . ? N4 K1 Si1 156.15(4) . . ? N3 K1 Si1 131.77(3) . . ? N2 K1 Si1 99.10(3) . . ? N1 K1 Si1 29.37(3) . . ? N4 K1 Al1 108.57(3) . . ? N3 K1 Al1 170.81(4) . . ? N2 K1 Al1 124.54(3) . . ? N1 K1 Al1 32.98(3) . . ? Si1 K1 Al1 52.918(13) . . ? N4 K1 Si2 110.53(4) . . ? N3 K1 Si2 125.14(3) . . ? N2 K1 Si2 144.12(3) . . ? N1 K1 Si2 25.27(3) . . ? Si1 K1 Si2 47.062(13) . . ? Al1 K1 Si2 50.186(12) . . ? N1 Si1 C15 113.54(8) . . ? N1 Si1 C13 113.09(8) . . ? C15 Si1 C13 105.84(9) . . ? N1 Si1 C14 112.31(8) . . ? C15 Si1 C14 108.37(9) . . ? C13 Si1 C14 102.96(9) . . ? N1 Si1 K1 59.07(5) . . ? C15 Si1 K1 171.89(7) . . ? C13 Si1 K1 81.08(6) . . ? C14 Si1 K1 73.50(7) . . ? N1 Si2 C17 113.71(8) . . ? N1 Si2 C16 110.70(8) . . ? C17 Si2 C16 109.23(9) . . ? N1 Si2 C18 115.78(8) . . ? C17 Si2 C18 102.73(9) . . ? C16 Si2 C18 103.95(9) . . ? N1 Si2 K1 48.20(5) . . ? C17 Si2 K1 139.73(6) . . ? C16 Si2 K1 63.66(6) . . ? C18 Si2 K1 117.52(7) . . ? Si1 N1 Si2 118.78(8) . . ? Si1 N1 Al1 118.67(8) . . ? Si2 N1 Al1 119.14(8) . . ? Si1 N1 K1 91.56(6) . . ? Si2 N1 K1 106.53(6) . . ? Al1 N1 K1 90.25(5) . . ? C27 N2 C26 109.18(17) . . ? C27 N2 C25 110.45(16) . . ? C26 N2 C25 107.75(16) . . ? C27 N2 K1 113.73(12) . . ? C26 N2 K1 109.43(12) . . ? C25 N2 K1 106.11(11) . . ? C23 N3 C22 110.54(16) . . ? C23 N3 C24 110.27(15) . . ? C22 N3 C24 110.23(15) . . ? C23 N3 K1 100.80(12) . . ? C22 N3 K1 112.73(10) . . ? C24 N3 K1 111.94(11) . . ? C19 N4 C21 109.50(16) . . ? C19 N4 C20 109.00(15) . . ? C21 N4 C20 110.97(16) . . ? C19 N4 K1 112.68(12) . . ? C21 N4 K1 110.73(11) . . ? C20 N4 K1 103.85(12) . . ? C2 C1 Al1 118.14(13) . . ? C2 C1 H1A 107.8 . . ? Al1 C1 H1A 107.8 . . ? C2 C1 H1B 107.8 . . ? Al1 C1 H1B 107.8 . . ? H1A C1 H1B 107.1 . . ? C3 C2 C4 109.58(16) . . ? C3 C2 C1 111.47(15) . . ? C4 C2 C1 112.31(16) . . ? C3 C2 H2 107.8 . . ? C4 C2 H2 107.8 . . ? C1 C2 H2 107.8 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 Al1 116.68(12) . . ? C6 C5 H5A 108.1 . . ? Al1 C5 H5A 108.1 . . ? C6 C5 H5B 108.1 . . ? Al1 C5 H5B 108.1 . . ? H5A C5 H5B 107.3 . . ? C8 C6 C7 108.65(15) . . ? C8 C6 C5 111.30(16) . . ? C7 C6 C5 112.84(15) . . ? C8 C6 H6 108.0 . . ? C7 C6 H6 108.0 . . ? C5 C6 H6 108.0 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 Al1 123.45(13) . . ? C10 C9 H9A 106.5 . . ? Al1 C9 H9A 106.5 . . ? C10 C9 H9B 106.5 . . ? Al1 C9 H9B 106.5 . . ? H9A C9 H9B 106.5 . . ? C12 C10 C11 109.69(16) . . ? C12 C10 C9 111.98(17) . . ? C11 C10 C9 111.81(16) . . ? C12 C10 H10 107.7 . . ? C11 C10 H10 107.7 . . ? C9 C10 H10 107.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N4 C19 H19A 109.5 . . ? N4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N4 C20 H20A 109.5 . . ? N4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N4 C21 C22 114.10(16) . . ? N4 C21 H21A 108.7 . . ? C22 C21 H21A 108.7 . . ? N4 C21 H21B 108.7 . . ? C22 C21 H21B 108.7 . . ? H21A C21 H21B 107.6 . . ? N3 C22 C21 113.65(16) . . ? N3 C22 H22A 108.8 . . ? C21 C22 H22A 108.8 . . ? N3 C22 H22B 108.8 . . ? C21 C22 H22B 108.8 . . ? H22A C22 H22B 107.7 . . ? N3 C23 H23A 109.5 . . ? N3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N3 C24 C25 112.59(15) . . ? N3 C24 H24A 109.1 . . ? C25 C24 H24A 109.1 . . ? N3 C24 H24B 109.1 . . ? C25 C24 H24B 109.1 . . ? H24A C24 H24B 107.8 . . ? N2 C25 C24 113.82(17) . . ? N2 C25 H25A 108.8 . . ? C24 C25 H25A 108.8 . . ? N2 C25 H25B 108.8 . . ? C24 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? N2 C26 H26A 109.5 . . ? N2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N2 C27 H27A 109.5 . . ? N2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 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 N1 Al1 K1 N4 130.21(6) . . . . ? C9 Al1 K1 N4 -155.53(10) . . . . ? C5 Al1 K1 N4 21.40(7) . . . . ? C1 Al1 K1 N4 -76.43(7) . . . . ? N1 Al1 K1 N3 91.2(2) . . . . ? C9 Al1 K1 N3 165.5(2) . . . . ? C5 Al1 K1 N3 -17.6(2) . . . . ? C1 Al1 K1 N3 -115.4(2) . . . . ? N1 Al1 K1 N2 -106.40(6) . . . . ? C9 Al1 K1 N2 -32.14(11) . . . . ? C5 Al1 K1 N2 144.79(6) . . . . ? C1 Al1 K1 N2 46.96(7) . . . . ? C9 Al1 K1 N1 74.26(11) . . . . ? C5 Al1 K1 N1 -108.81(7) . . . . ? C1 Al1 K1 N1 153.36(8) . . . . ? N1 Al1 K1 Si1 -32.63(5) . . . . ? C9 Al1 K1 Si1 41.63(10) . . . . ? C5 Al1 K1 Si1 -141.44(6) . . . . ? C1 Al1 K1 Si1 120.73(6) . . . . ? N1 Al1 K1 Si2 28.58(5) . . . . ? C9 Al1 K1 Si2 102.84(10) . . . . ? C5 Al1 K1 Si2 -80.23(5) . . . . ? C1 Al1 K1 Si2 -178.06(6) . . . . ? N4 K1 Si1 N1 -7.00(10) . . . . ? N3 K1 Si1 N1 -132.99(7) . . . . ? N2 K1 Si1 N1 163.54(6) . . . . ? Al1 K1 Si1 N1 36.76(5) . . . . ? Si2 K1 Si1 N1 -30.09(5) . . . . ? N4 K1 Si1 C15 18.2(5) . . . . ? N3 K1 Si1 C15 -107.8(5) . . . . ? N2 K1 Si1 C15 -171.3(5) . . . . ? N1 K1 Si1 C15 25.2(5) . . . . ? Al1 K1 Si1 C15 61.9(5) . . . . ? Si2 K1 Si1 C15 -4.9(5) . . . . ? N4 K1 Si1 C13 -130.83(10) . . . . ? N3 K1 Si1 C13 103.18(7) . . . . ? N2 K1 Si1 C13 39.70(7) . . . . ? N1 K1 Si1 C13 -123.83(8) . . . . ? Al1 K1 Si1 C13 -87.07(6) . . . . ? Si2 K1 Si1 C13 -153.93(6) . . . . ? N4 K1 Si1 C14 122.72(11) . . . . ? N3 K1 Si1 C14 -3.27(8) . . . . ? N2 K1 Si1 C14 -66.75(7) . . . . ? N1 K1 Si1 C14 129.72(8) . . . . ? Al1 K1 Si1 C14 166.48(7) . . . . ? Si2 K1 Si1 C14 99.62(6) . . . . ? N4 K1 Si2 N1 -135.08(7) . . . . ? N3 K1 Si2 N1 152.41(7) . . . . ? N2 K1 Si2 N1 58.56(8) . . . . ? Si1 K1 Si2 N1 35.17(6) . . . . ? Al1 K1 Si2 N1 -37.58(6) . . . . ? N4 K1 Si2 C17 -57.84(11) . . . . ? N3 K1 Si2 C17 -130.34(11) . . . . ? N2 K1 Si2 C17 135.80(11) . . . . ? N1 K1 Si2 C17 77.24(12) . . . . ? Si1 K1 Si2 C17 112.41(10) . . . . ? Al1 K1 Si2 C17 39.67(10) . . . . ? N4 K1 Si2 C16 31.25(8) . . . . ? N3 K1 Si2 C16 -41.25(8) . . . . ? N2 K1 Si2 C16 -135.11(9) . . . . ? N1 K1 Si2 C16 166.33(9) . . . . ? Si1 K1 Si2 C16 -158.50(7) . . . . ? Al1 K1 Si2 C16 128.75(7) . . . . ? N4 K1 Si2 C18 123.86(8) . . . . ? N3 K1 Si2 C18 51.35(8) . . . . ? N2 K1 Si2 C18 -42.51(9) . . . . ? N1 K1 Si2 C18 -101.07(10) . . . . ? Si1 K1 Si2 C18 -65.89(7) . . . . ? Al1 K1 Si2 C18 -138.64(8) . . . . ? C15 Si1 N1 Si2 -66.39(12) . . . . ? C13 Si1 N1 Si2 172.99(9) . . . . ? C14 Si1 N1 Si2 56.99(12) . . . . ? K1 Si1 N1 Si2 109.86(10) . . . . ? C15 Si1 N1 Al1 92.61(11) . . . . ? C13 Si1 N1 Al1 -28.01(12) . . . . ? C14 Si1 N1 Al1 -144.00(9) . . . . ? K1 Si1 N1 Al1 -91.14(8) . . . . ? C15 Si1 N1 K1 -176.25(7) . . . . ? C13 Si1 N1 K1 63.13(8) . . . . ? C14 Si1 N1 K1 -52.86(8) . . . . ? C17 Si2 N1 Si1 122.24(10) . . . . ? C16 Si2 N1 Si1 -114.36(10) . . . . ? C18 Si2 N1 Si1 3.60(14) . . . . ? K1 Si2 N1 Si1 -101.27(10) . . . . ? C17 Si2 N1 Al1 -36.66(12) . . . . ? C16 Si2 N1 Al1 86.74(11) . . . . ? C18 Si2 N1 Al1 -155.31(9) . . . . ? K1 Si2 N1 Al1 99.82(9) . . . . ? C17 Si2 N1 K1 -136.48(8) . . . . ? C16 Si2 N1 K1 -13.08(9) . . . . ? C18 Si2 N1 K1 104.87(9) . . . . ? C9 Al1 N1 Si1 -52.19(11) . . . . ? C5 Al1 N1 Si1 178.72(9) . . . . ? C1 Al1 N1 Si1 68.54(11) . . . . ? K1 Al1 N1 Si1 91.92(9) . . . . ? C9 Al1 N1 Si2 106.73(10) . . . . ? C5 Al1 N1 Si2 -22.36(12) . . . . ? C1 Al1 N1 Si2 -132.54(9) . . . . ? K1 Al1 N1 Si2 -109.16(9) . . . . ? C9 Al1 N1 K1 -144.11(6) . . . . ? C5 Al1 N1 K1 86.80(7) . . . . ? C1 Al1 N1 K1 -23.38(7) . . . . ? N4 K1 N1 Si1 176.47(5) . . . . ? N3 K1 N1 Si1 77.95(9) . . . . ? N2 K1 N1 Si1 -20.52(8) . . . . ? Al1 K1 N1 Si1 -118.69(8) . . . . ? Si2 K1 N1 Si1 120.70(9) . . . . ? N4 K1 N1 Si2 55.77(8) . . . . ? N3 K1 N1 Si2 -42.75(11) . . . . ? N2 K1 N1 Si2 -141.22(6) . . . . ? Si1 K1 N1 Si2 -120.70(9) . . . . ? Al1 K1 N1 Si2 120.61(8) . . . . ? N4 K1 N1 Al1 -64.84(7) . . . . ? N3 K1 N1 Al1 -163.36(6) . . . . ? N2 K1 N1 Al1 98.17(6) . . . . ? Si1 K1 N1 Al1 118.69(8) . . . . ? Si2 K1 N1 Al1 -120.61(8) . . . . ? N4 K1 N2 C27 -154.27(14) . . . . ? N3 K1 N2 C27 -102.53(14) . . . . ? N1 K1 N2 C27 39.69(15) . . . . ? Si1 K1 N2 C27 29.67(14) . . . . ? Al1 K1 N2 C27 80.54(14) . . . . ? Si2 K1 N2 C27 12.55(16) . . . . ? N4 K1 N2 C26 83.34(14) . . . . ? N3 K1 N2 C26 135.08(14) . . . . ? N1 K1 N2 C26 -82.69(14) . . . . ? Si1 K1 N2 C26 -92.72(13) . . . . ? Al1 K1 N2 C26 -41.85(15) . . . . ? Si2 K1 N2 C26 -109.84(13) . . . . ? N4 K1 N2 C25 -32.66(12) . . . . ? N3 K1 N2 C25 19.08(11) . . . . ? N1 K1 N2 C25 161.31(10) . . . . ? Si1 K1 N2 C25 151.28(11) . . . . ? Al1 K1 N2 C25 -157.85(10) . . . . ? Si2 K1 N2 C25 134.16(10) . . . . ? N4 K1 N3 C23 -108.60(12) . . . . ? N2 K1 N3 C23 128.87(12) . . . . ? N1 K1 N3 C23 10.10(15) . . . . ? Si1 K1 N3 C23 50.12(13) . . . . ? Al1 K1 N3 C23 -67.2(3) . . . . ? Si2 K1 N3 C23 -10.65(13) . . . . ? N4 K1 N3 C22 9.25(11) . . . . ? N2 K1 N3 C22 -113.28(13) . . . . ? N1 K1 N3 C22 127.95(12) . . . . ? Si1 K1 N3 C22 167.98(10) . . . . ? Al1 K1 N3 C22 50.7(3) . . . . ? Si2 K1 N3 C22 107.20(12) . . . . ? N4 K1 N3 C24 134.19(13) . . . . ? N2 K1 N3 C24 11.67(11) . . . . ? N1 K1 N3 C24 -107.10(13) . . . . ? Si1 K1 N3 C24 -67.08(13) . . . . ? Al1 K1 N3 C24 175.62(17) . . . . ? Si2 K1 N3 C24 -127.85(11) . . . . ? N3 K1 N4 C19 142.01(14) . . . . ? N2 K1 N4 C19 -166.34(13) . . . . ? N1 K1 N4 C19 -0.27(15) . . . . ? Si1 K1 N4 C19 4.01(19) . . . . ? Al1 K1 N4 C19 -31.59(13) . . . . ? Si2 K1 N4 C19 21.87(13) . . . . ? N3 K1 N4 C21 18.98(12) . . . . ? N2 K1 N4 C21 70.64(13) . . . . ? N1 K1 N4 C21 -123.30(12) . . . . ? Si1 K1 N4 C21 -119.02(12) . . . . ? Al1 K1 N4 C21 -154.61(11) . . . . ? Si2 K1 N4 C21 -101.16(12) . . . . ? N3 K1 N4 C20 -100.18(12) . . . . ? N2 K1 N4 C20 -48.53(12) . . . . ? N1 K1 N4 C20 117.54(11) . . . . ? Si1 K1 N4 C20 121.82(12) . . . . ? Al1 K1 N4 C20 86.22(11) . . . . ? Si2 K1 N4 C20 139.68(11) . . . . ? N1 Al1 C1 C2 -156.59(12) . . . . ? C9 Al1 C1 C2 -37.34(15) . . . . ? C5 Al1 C1 C2 87.19(14) . . . . ? K1 Al1 C1 C2 -179.97(15) . . . . ? Al1 C1 C2 C3 82.34(18) . . . . ? Al1 C1 C2 C4 -154.25(14) . . . . ? N1 Al1 C5 C6 -156.39(13) . . . . ? C9 Al1 C5 C6 79.22(16) . . . . ? C1 Al1 C5 C6 -41.13(15) . . . . ? K1 Al1 C5 C6 -98.79(14) . . . . ? Al1 C5 C6 C8 -71.75(19) . . . . ? Al1 C5 C6 C7 165.79(14) . . . . ? N1 Al1 C9 C10 -68.41(16) . . . . ? C5 Al1 C9 C10 56.93(17) . . . . ? C1 Al1 C9 C10 171.98(14) . . . . ? K1 Al1 C9 C10 -126.48(13) . . . . ? Al1 C9 C10 C12 169.22(14) . . . . ? Al1 C9 C10 C11 -67.2(2) . . . . ? C19 N4 C21 C22 -172.03(17) . . . . ? C20 N4 C21 C22 67.6(2) . . . . ? K1 N4 C21 C22 -47.18(19) . . . . ? C23 N3 C22 C21 75.1(2) . . . . ? C24 N3 C22 C21 -162.74(16) . . . . ? K1 N3 C22 C21 -36.86(19) . . . . ? N4 C21 C22 N3 59.2(2) . . . . ? C23 N3 C24 C25 -154.25(18) . . . . ? C22 N3 C24 C25 83.4(2) . . . . ? K1 N3 C24 C25 -42.89(19) . . . . ? C27 N2 C25 C24 72.8(2) . . . . ? C26 N2 C25 C24 -168.07(17) . . . . ? K1 N2 C25 C24 -50.94(17) . . . . ? N3 C24 C25 N2 68.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.537 _refine_diff_density_min -0.566 _refine_diff_density_rms 0.084 #===END