# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 ata_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_section_title ;Poly{guanidinium} salts: application in the preparation of a coordinatively saturated aluminium cation ; _publ_requested_category FM _publ_contact_author_name 'Martyn Coles' _publ_contact_author_email M.P.COLES@SUSSEX.AC.UK loop_ _publ_author_name 'Martyn Coles' 'Peter B. Hitchcock' 'Sarah H. Oakley' 'Pedro J. Aragon Saez' # Attachment 'Combined cif files.cif' data_(2b)-mar3004 _database_code_depnum_ccdc_archive 'CCDC 617259' _audit_creation_date 2004-03-25T14:22:42-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C15 H27 N6, C24 H20 B' _chemical_formula_sum 'C39 H47 B N6' _chemical_formula_weight 610.64 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2719(3) _cell_length_b 12.4868(3) _cell_length_c 14.3087(5) _cell_angle_alpha 109.992(2) _cell_angle_beta 99.770(1) _cell_angle_gamma 100.197(2) _cell_volume 1644.02(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14160 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.788805E-1 _diffrn_orient_matrix_ub_12 0.135306E-1 _diffrn_orient_matrix_ub_13 0.309328E-1 _diffrn_orient_matrix_ub_21 -0.632599E-1 _diffrn_orient_matrix_ub_22 -0.348496E-1 _diffrn_orient_matrix_ub_23 -0.701973E-1 _diffrn_orient_matrix_ub_31 -0.143696E-1 _diffrn_orient_matrix_ub_32 -0.07978 _diffrn_orient_matrix_ub_33 0.33936E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0512 _diffrn_reflns_av_unetI/netI 0.0374 _diffrn_reflns_number 22790 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _reflns_number_total 5727 _reflns_number_gt 4569 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The H on N1 was refined; other H atoms were riding. The C11 was disordered and the lower occupancy site was left isotropic. 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^)+(0.0520P)^2^+0.5298P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 5727 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1147 _refine_ls_wR_factor_gt 0.1063 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.242 _refine_diff_density_min -0.188 _refine_diff_density_rms 0.035 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' 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 N1 N 0.59431(15) 0.33381(13) 0.16934(11) 0.0376(4) Uani 1 1 d . . . H1X H 0.541(3) 0.247(2) 0.1426(18) 0.077(7) Uiso 1 1 d . . . N2 N 0.62271(13) 0.34359(11) 0.33609(10) 0.0299(3) Uani 1 1 d . . . N3 N 0.65182(14) 0.51636(11) 0.30441(11) 0.0333(3) Uani 1 1 d . . . N4 N 0.42567(15) 0.11340(12) 0.10586(11) 0.0368(3) Uani 1 1 d . . . N5 N 0.44491(13) 0.15985(11) 0.27863(11) 0.0315(3) Uani 1 1 d . . . N6 N 0.24411(14) 0.02977(12) 0.16116(12) 0.0397(4) Uani 1 1 d . . . C1 C 0.62247(15) 0.39842(14) 0.26896(12) 0.0289(4) Uani 1 1 d . . . C2 C 0.63474(19) 0.41164(15) 0.44402(13) 0.0390(4) Uani 1 1 d . . . H2A H 0.662 0.3668 0.4859 0.047 Uiso 1 1 calc R . . H2B H 0.5456 0.4269 0.4536 0.047 Uiso 1 1 calc R . . C3 C 0.7409(2) 0.52705(15) 0.47799(14) 0.0466(5) Uani 1 1 d . . . H3A H 0.7494 0.5746 0.5511 0.056 Uiso 1 1 calc R . . H3B H 0.8308 0.5117 0.4709 0.056 Uiso 1 1 calc R . . C4 C 0.6994(2) 0.59331(15) 0.41312(14) 0.0433(5) Uani 1 1 d . . . H4A H 0.6256 0.6289 0.4356 0.052 Uiso 1 1 calc R . . H4B H 0.7783 0.6579 0.4228 0.052 Uiso 1 1 calc R . . C5 C 0.6389(2) 0.58060(16) 0.23566(15) 0.0443(5) Uani 1 1 d . . . H5A H 0.731 0.6157 0.2316 0.053 Uiso 1 1 calc R . . H5B H 0.5962 0.6456 0.2646 0.053 Uiso 1 1 calc R . . C6 C 0.5544(2) 0.50188(17) 0.12968(15) 0.0495(5) Uani 1 1 d . . . H6A H 0.5648 0.5423 0.0817 0.059 Uiso 1 1 calc R . . H6B H 0.4567 0.4831 0.13 0.059 Uiso 1 1 calc R . . C7 C 0.6012(2) 0.39025(17) 0.09523(14) 0.0490(5) Uani 1 1 d . . . H7A H 0.5426 0.3357 0.027 0.059 Uiso 1 1 calc R . . H7B H 0.6963 0.4087 0.0888 0.059 Uiso 1 1 calc R . . C8 C 0.58932(16) 0.21509(13) 0.30089(13) 0.0308(4) Uani 1 1 d . A . H8A H 0.6217 0.1831 0.2381 0.037 Uiso 1 1 calc R . . H8B H 0.6396 0.1934 0.3543 0.037 Uiso 1 1 calc R . . C9 C 0.37092(16) 0.09884(13) 0.17763(13) 0.0314(4) Uani 1 1 d . A . C13 C 0.18117(19) 0.01824(16) 0.24227(17) 0.0474(5) Uani 1 1 d . A . H13A H 0.191 -0.0555 0.251 0.057 Uiso 1 1 calc R . . H13B H 0.0824 0.0128 0.222 0.057 Uiso 1 1 calc R . . C14 C 0.24515(19) 0.12123(16) 0.34304(16) 0.0446(5) Uani 1 1 d . . . H14A H 0.2193 0.1927 0.3396 0.054 Uiso 1 1 calc R A . H14B H 0.2125 0.1045 0.3991 0.054 Uiso 1 1 calc R . . C15 C 0.39674(18) 0.14061(17) 0.36350(15) 0.0415(4) Uani 1 1 d . A . H15A H 0.4407 0.21 0.428 0.05 Uiso 1 1 calc R . . H15B H 0.4224 0.0711 0.3719 0.05 Uiso 1 1 calc R . . C16 C -0.11742(15) 0.25368(14) 0.58592(12) 0.0281(4) Uani 1 1 d . . . C17 C -0.07731(17) 0.31927(16) 0.52939(13) 0.0349(4) Uani 1 1 d . . . H17 H -0.0601 0.4026 0.56 0.042 Uiso 1 1 calc R . . C18 C -0.06129(18) 0.26895(19) 0.43068(14) 0.0465(5) Uani 1 1 d . . . H18 H -0.0354 0.3176 0.395 0.056 Uiso 1 1 calc R . . C19 C -0.08291(19) 0.1484(2) 0.38424(15) 0.0504(5) Uani 1 1 d . . . H19 H -0.0717 0.1135 0.3168 0.06 Uiso 1 1 calc R . . C20 C -0.12116(19) 0.07947(18) 0.43742(15) 0.0464(5) Uani 1 1 d . . . H20 H -0.1351 -0.0036 0.407 0.056 Uiso 1 1 calc R . . C21 C -0.13930(18) 0.13128(15) 0.53513(13) 0.0374(4) Uani 1 1 d . . . H21 H -0.1679 0.0817 0.5694 0.045 Uiso 1 1 calc R . . C22 C -0.28758(16) 0.24142(13) 0.70827(12) 0.0270(4) Uani 1 1 d . . . C23 C -0.39714(17) 0.18286(14) 0.62144(13) 0.0339(4) Uani 1 1 d . . . H23 H -0.3848 0.1841 0.5575 0.041 Uiso 1 1 calc R . . C24 C -0.52321(18) 0.12303(15) 0.62424(15) 0.0406(4) Uani 1 1 d . . . H24 H -0.5945 0.0848 0.5631 0.049 Uiso 1 1 calc R . . C25 C -0.5450(2) 0.11903(16) 0.71532(16) 0.0446(5) Uani 1 1 d . . . H25 H -0.6301 0.0768 0.7176 0.053 Uiso 1 1 calc R . . C26 C -0.4410(2) 0.17744(17) 0.80318(16) 0.0479(5) Uani 1 1 d . . . H26 H -0.4551 0.1767 0.8669 0.057 Uiso 1 1 calc R . . C27 C -0.31544(19) 0.23749(16) 0.79951(14) 0.0390(4) Uani 1 1 d . . . H27 H -0.2459 0.2774 0.8615 0.047 Uiso 1 1 calc R . . C28 C -0.01509(16) 0.29907(13) 0.78679(12) 0.0266(3) Uani 1 1 d . . . C29 C 0.06123(16) 0.21577(13) 0.76304(13) 0.0280(4) Uani 1 1 d . . . H29 H 0.045 0.1638 0.6935 0.034 Uiso 1 1 calc R . . C30 C 0.16003(17) 0.20562(14) 0.83683(14) 0.0338(4) Uani 1 1 d . . . H30 H 0.2086 0.1469 0.8169 0.041 Uiso 1 1 calc R . . C31 C 0.18823(18) 0.27946(15) 0.93829(14) 0.0388(4) Uani 1 1 d . . . H31 H 0.2563 0.2729 0.9886 0.047 Uiso 1 1 calc R . . C32 C 0.1155(2) 0.36333(17) 0.96547(14) 0.0489(5) Uani 1 1 d . . . H32 H 0.1326 0.4149 1.0352 0.059 Uiso 1 1 calc R . . C33 C 0.0174(2) 0.37223(16) 0.89084(13) 0.0432(5) Uani 1 1 d . . . H33 H -0.0305 0.4314 0.9116 0.052 Uiso 1 1 calc R . . C34 C -0.13259(16) 0.45188(13) 0.73387(11) 0.0260(3) Uani 1 1 d . . . C35 C -0.24639(17) 0.49860(14) 0.73713(12) 0.0311(4) Uani 1 1 d . . . H35 H -0.3344 0.4463 0.7179 0.037 Uiso 1 1 calc R . . C36 C -0.23570(19) 0.61903(15) 0.76749(13) 0.0384(4) Uani 1 1 d . . . H36 H -0.3157 0.6472 0.7691 0.046 Uiso 1 1 calc R . . C37 C -0.1100(2) 0.69764(15) 0.79519(13) 0.0400(4) Uani 1 1 d . . . H37 H -0.1025 0.7799 0.8169 0.048 Uiso 1 1 calc R . . C38 C 0.00476(19) 0.65471(15) 0.79078(14) 0.0400(4) Uani 1 1 d . . . H38 H 0.0921 0.7075 0.8086 0.048 Uiso 1 1 calc R . . C39 C -0.00714(17) 0.53503(14) 0.76053(13) 0.0346(4) Uani 1 1 d . . . H39 H 0.0733 0.5077 0.7576 0.042 Uiso 1 1 calc R . . B B -0.13845(18) 0.31109(15) 0.70287(14) 0.0265(4) Uani 1 1 d . . . C10 C 0.3477(2) 0.05021(17) -0.00106(15) 0.0493(5) Uani 0.635(5) 1 d P A 1 H10C H 0.2897 0.0984 -0.0205 0.059 Uiso 0.635(5) 1 calc PR A 1 H10D H 0.4117 0.0386 -0.046 0.059 Uiso 0.635(5) 1 calc PR A 1 C11 C 0.2615(3) -0.0642(3) -0.0175(3) 0.0518(11) Uani 0.635(5) 1 d P A 1 H11C H 0.3196 -0.1165 -0.0069 0.062 Uiso 0.635(5) 1 calc PR A 1 H11D H 0.2047 -0.1013 -0.089 0.062 Uiso 0.635(5) 1 calc PR A 1 C12 C 0.1688(2) -0.04990(17) 0.05703(17) 0.0558(6) Uani 0.635(5) 1 d P A 1 H12C H 0.0931 -0.0187 0.0333 0.067 Uiso 0.635(5) 1 calc PR A 1 H12D H 0.1286 -0.1279 0.0573 0.067 Uiso 0.635(5) 1 calc PR A 1 C10A C 0.3477(2) 0.05021(17) -0.00106(15) 0.0493(5) Uani 0.365(5) 1 d P A 2 H10A H 0.3847 -0.0179 -0.0323 0.059 Uiso 0.365(5) 1 calc PR A 2 H10B H 0.363 0.1032 -0.0384 0.059 Uiso 0.365(5) 1 calc PR A 2 C11A C 0.1936(5) 0.0052(5) -0.0178(4) 0.0448(17) Uiso 0.365(5) 1 d P A 2 H11A H 0.1498 0.0714 -0.008 0.054 Uiso 0.365(5) 1 calc PR A 2 H11B H 0.1536 -0.0535 -0.0888 0.054 Uiso 0.365(5) 1 calc PR A 2 C12A C 0.1688(2) -0.04990(17) 0.05703(17) 0.0558(6) Uani 0.365(5) 1 d P A 2 H12A H 0.0699 -0.0689 0.0536 0.067 Uiso 0.365(5) 1 calc PR A 2 H12B H 0.198 -0.1243 0.039 0.067 Uiso 0.365(5) 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 N1 0.0409(9) 0.0346(8) 0.0312(8) 0.0096(7) 0.0099(7) 0.0002(7) N2 0.0309(7) 0.0235(7) 0.0309(8) 0.0083(6) 0.0066(6) 0.0019(6) N3 0.0335(8) 0.0255(7) 0.0369(8) 0.0124(6) 0.0043(6) 0.0007(6) N4 0.0379(8) 0.0303(8) 0.0341(8) 0.0072(6) 0.0045(7) 0.0035(6) N5 0.0265(7) 0.0274(7) 0.0374(8) 0.0117(6) 0.0071(6) 0.0016(6) N6 0.0294(8) 0.0260(7) 0.0555(10) 0.0138(7) 0.0019(7) -0.0008(6) C1 0.0214(8) 0.0291(9) 0.0332(10) 0.0107(7) 0.0062(7) 0.0023(6) C2 0.0480(11) 0.0316(9) 0.0327(10) 0.0098(8) 0.0099(8) 0.0036(8) C3 0.0604(13) 0.0319(10) 0.0316(10) 0.0066(8) 0.0006(9) -0.0053(9) C4 0.0512(11) 0.0287(9) 0.0376(11) 0.0052(8) 0.0052(9) 0.0005(8) C5 0.0472(11) 0.0373(10) 0.0474(11) 0.0227(9) 0.0053(9) 0.0012(8) C6 0.0534(12) 0.0486(12) 0.0452(12) 0.0267(10) 0.0034(9) 0.0005(9) C7 0.0545(12) 0.0513(12) 0.0341(11) 0.0164(9) 0.0096(9) -0.0028(9) C8 0.0264(8) 0.0247(8) 0.0387(10) 0.0106(7) 0.0061(7) 0.0049(7) C9 0.0285(9) 0.0179(8) 0.0443(11) 0.0091(7) 0.0047(8) 0.0073(7) C13 0.0335(10) 0.0344(10) 0.0797(15) 0.0270(10) 0.0189(10) 0.0067(8) C14 0.0395(10) 0.0422(11) 0.0625(13) 0.0287(10) 0.0194(9) 0.0118(8) C15 0.0396(10) 0.0408(10) 0.0487(11) 0.0220(9) 0.0145(9) 0.0079(8) C16 0.0238(8) 0.0314(9) 0.0274(9) 0.0090(7) 0.0047(7) 0.0097(7) C17 0.0291(9) 0.0419(10) 0.0300(9) 0.0118(8) 0.0066(7) 0.0045(7) C18 0.0342(10) 0.0701(14) 0.0310(10) 0.0177(10) 0.0102(8) 0.0046(9) C19 0.0316(10) 0.0766(15) 0.0284(10) 0.0011(10) 0.0101(8) 0.0143(10) C20 0.0405(11) 0.0465(11) 0.0390(11) -0.0018(9) 0.0057(9) 0.0191(9) C21 0.0413(10) 0.0346(9) 0.0329(10) 0.0070(8) 0.0083(8) 0.0142(8) C22 0.0323(9) 0.0219(8) 0.0310(9) 0.0106(7) 0.0108(7) 0.0132(7) C23 0.0346(9) 0.0339(9) 0.0347(10) 0.0151(8) 0.0093(8) 0.0074(7) C24 0.0345(10) 0.0346(9) 0.0476(11) 0.0108(8) 0.0121(8) 0.0046(8) C25 0.0414(11) 0.0337(10) 0.0613(13) 0.0151(9) 0.0276(10) 0.0085(8) C26 0.0567(13) 0.0521(12) 0.0474(12) 0.0223(10) 0.0331(10) 0.0188(10) C27 0.0429(10) 0.0415(10) 0.0337(10) 0.0120(8) 0.0153(8) 0.0133(8) C28 0.0292(8) 0.0229(8) 0.0297(9) 0.0105(7) 0.0096(7) 0.0087(6) C29 0.0282(8) 0.0240(8) 0.0333(9) 0.0106(7) 0.0112(7) 0.0072(7) C30 0.0303(9) 0.0293(9) 0.0489(11) 0.0187(8) 0.0133(8) 0.0145(7) C31 0.0368(10) 0.0379(10) 0.0427(11) 0.0190(9) 0.0009(8) 0.0134(8) C32 0.0650(13) 0.0444(11) 0.0314(10) 0.0064(9) -0.0018(9) 0.0293(10) C33 0.0568(12) 0.0394(10) 0.0318(10) 0.0063(8) 0.0023(8) 0.0317(9) C34 0.0319(9) 0.0264(8) 0.0215(8) 0.0095(7) 0.0071(7) 0.0105(7) C35 0.0343(9) 0.0315(9) 0.0304(9) 0.0133(7) 0.0073(7) 0.0128(7) C36 0.0477(11) 0.0372(10) 0.0390(10) 0.0179(8) 0.0117(8) 0.0248(9) C37 0.0613(13) 0.0255(9) 0.0358(10) 0.0140(8) 0.0098(9) 0.0150(9) C38 0.0452(11) 0.0294(9) 0.0411(11) 0.0141(8) 0.0067(8) 0.0016(8) C39 0.0328(9) 0.0319(9) 0.0393(10) 0.0136(8) 0.0081(8) 0.0095(7) B 0.0299(10) 0.0247(9) 0.0256(10) 0.0081(8) 0.0087(8) 0.0101(7) C10 0.0512(12) 0.0408(11) 0.0423(11) 0.0085(9) -0.0052(9) 0.0095(9) C11 0.053(2) 0.0312(17) 0.047(2) 0.0001(14) -0.0107(15) 0.0028(14) C12 0.0384(11) 0.0394(11) 0.0672(15) 0.0120(10) -0.0109(10) -0.0045(9) C10A 0.0512(12) 0.0408(11) 0.0423(11) 0.0085(9) -0.0052(9) 0.0095(9) C12A 0.0384(11) 0.0394(11) 0.0672(15) 0.0120(10) -0.0109(10) -0.0045(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N1 C1 1.326(2) . ? N1 C7 1.465(2) . ? N2 C1 1.357(2) . ? N2 C2 1.457(2) . ? N2 C8 1.4629(19) . ? N3 C1 1.341(2) . ? N3 C4 1.461(2) . ? N3 C5 1.470(2) . ? N4 C9 1.300(2) . ? N4 C10 1.463(2) . ? N5 C9 1.384(2) . ? N5 C8 1.451(2) . ? N5 C15 1.462(2) . ? N6 C9 1.362(2) . ? N6 C13 1.457(2) . ? N6 C12 1.460(2) . ? C2 C3 1.512(2) . ? C3 C4 1.498(3) . ? C5 C6 1.500(3) . ? C6 C7 1.505(3) . ? C13 C14 1.509(3) . ? C14 C15 1.494(3) . ? C16 C17 1.393(2) . ? C16 C21 1.406(2) . ? C16 B 1.649(2) . ? C17 C18 1.388(2) . ? C18 C19 1.380(3) . ? C19 C20 1.380(3) . ? C20 C21 1.386(3) . ? C22 C27 1.398(2) . ? C22 C23 1.399(2) . ? C22 B 1.650(2) . ? C23 C24 1.390(2) . ? C24 C25 1.375(3) . ? C25 C26 1.377(3) . ? C26 C27 1.391(3) . ? C28 C29 1.396(2) . ? C28 C33 1.399(2) . ? C28 B 1.657(2) . ? C29 C30 1.391(2) . ? C30 C31 1.374(2) . ? C31 C32 1.380(2) . ? C32 C33 1.387(2) . ? C34 C35 1.396(2) . ? C34 C39 1.404(2) . ? C34 B 1.647(2) . ? C35 C36 1.393(2) . ? C36 C37 1.378(3) . ? C37 C38 1.381(3) . ? C38 C39 1.382(2) . ? C10 C11 1.461(4) . ? C11 C12 1.533(4) . ? 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 C1 N1 C7 120.47(15) . . ? C1 N2 C2 119.66(13) . . ? C1 N2 C8 121.54(13) . . ? C2 N2 C8 118.06(13) . . ? C1 N3 C4 124.20(14) . . ? C1 N3 C5 122.27(14) . . ? C4 N3 C5 113.54(13) . . ? C9 N4 C10 118.45(15) . . ? C9 N5 C8 119.59(14) . . ? C9 N5 C15 121.65(14) . . ? C8 N5 C15 115.95(14) . . ? C9 N6 C13 124.45(15) . . ? C9 N6 C12 119.84(16) . . ? C13 N6 C12 115.31(15) . . ? N1 C1 N3 121.35(15) . . ? N1 C1 N2 119.04(14) . . ? N3 C1 N2 119.61(14) . . ? N2 C2 C3 108.96(14) . . ? C4 C3 C2 109.39(16) . . ? N3 C4 C3 111.50(14) . . ? N3 C5 C6 111.96(14) . . ? C5 C6 C7 108.93(16) . . ? N1 C7 C6 110.22(16) . . ? N5 C8 N2 114.31(13) . . ? N4 C9 N6 124.85(16) . . ? N4 C9 N5 118.04(14) . . ? N6 C9 N5 117.08(15) . . ? N6 C13 C14 111.82(14) . . ? C15 C14 C13 108.43(16) . . ? N5 C15 C14 110.31(15) . . ? C17 C16 C21 114.46(15) . . ? C17 C16 B 124.26(14) . . ? C21 C16 B 121.27(14) . . ? C18 C17 C16 123.27(17) . . ? C19 C18 C17 120.19(18) . . ? C18 C19 C20 118.87(17) . . ? C19 C20 C21 120.03(18) . . ? C20 C21 C16 123.16(18) . . ? C27 C22 C23 114.67(15) . . ? C27 C22 B 123.03(15) . . ? C23 C22 B 122.30(14) . . ? C24 C23 C22 123.19(16) . . ? C25 C24 C23 120.14(18) . . ? C24 C25 C26 118.71(17) . . ? C25 C26 C27 120.62(17) . . ? C26 C27 C22 122.64(17) . . ? C29 C28 C33 114.30(14) . . ? C29 C28 B 124.76(14) . . ? C33 C28 B 120.91(13) . . ? C30 C29 C28 122.80(15) . . ? C31 C30 C29 120.81(15) . . ? C30 C31 C32 118.49(16) . . ? C31 C32 C33 119.91(17) . . ? C32 C33 C28 123.68(16) . . ? C35 C34 C39 114.98(14) . . ? C35 C34 B 124.56(14) . . ? C39 C34 B 120.46(13) . . ? C36 C35 C34 122.44(16) . . ? C37 C36 C35 120.52(16) . . ? C36 C37 C38 118.81(15) . . ? C37 C38 C39 120.13(17) . . ? C38 C39 C34 123.08(16) . . ? C34 B C16 110.13(13) . . ? C34 B C22 109.37(12) . . ? C16 B C22 109.64(13) . . ? C34 B C28 108.25(12) . . ? C16 B C28 110.07(12) . . ? C22 B C28 109.36(12) . . ? C11 C10 N4 111.9(2) . . ? C10 C11 C12 110.4(2) . . ? N6 C12 C11 111.51(18) . . ? #===END data_(3b)-jan1205 _database_code_depnum_ccdc_archive 'CCDC 617260' _audit_creation_date 2005-01-19T10:18:03-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C15 H28 N6, C24 H20 B, Cl' _chemical_formula_sum 'C39 H48 B Cl N6' _chemical_formula_weight 647.09 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.8838(3) _cell_length_b 16.0260(3) _cell_length_c 17.2417(4) _cell_angle_alpha 114.855(1) _cell_angle_beta 93.524(1) _cell_angle_gamma 91.947(1) _cell_volume 3466.80(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 31724 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.24 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.148 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.139878E-1 _diffrn_orient_matrix_ub_12 0.326364E-1 _diffrn_orient_matrix_ub_13 0.61444E-1 _diffrn_orient_matrix_ub_21 -0.703991E-1 _diffrn_orient_matrix_ub_22 -0.35289E-2 _diffrn_orient_matrix_ub_23 -0.181229E-1 _diffrn_orient_matrix_ub_31 -0.88655E-2 _diffrn_orient_matrix_ub_32 -0.605987E-1 _diffrn_orient_matrix_ub_33 0.32559E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_unetI/netI 0.054 _diffrn_reflns_number 53243 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 26.03 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 13606 _reflns_number_gt 9575 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; H atoms on N refined; others in riding mode. There are two residual peaks of about 1.3 electrons which make no chemical sense and are assumed to be artefacts. 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^)+(0.0537P)^2^+2.4628P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 13606 _refine_ls_number_parameters 863 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0905 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1403 _refine_ls_wR_factor_gt 0.1235 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.328 _refine_diff_density_min -0.49 _refine_diff_density_rms 0.05 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 B1 B 0.44536(19) 0.79072(17) 0.59751(16) 0.0278(6) Uani 1 1 d . . . Cl1 Cl -0.08162(4) 0.57880(4) 0.39408(4) 0.03352(15) Uani 1 1 d . . . N1 N 0.15773(13) 0.39843(12) 0.35986(12) 0.0289(4) Uani 1 1 d . . . N2 N 0.10032(16) 0.49523(15) 0.30030(14) 0.0348(5) Uani 1 1 d . . . H2X H 0.057(2) 0.5082(19) 0.3299(18) 0.044(8) Uiso 1 1 d . . . N3 N 0.25800(14) 0.45561(13) 0.28750(13) 0.0342(5) Uani 1 1 d . . . N4 N 0.02536(14) 0.28466(13) 0.33067(12) 0.0313(4) Uani 1 1 d . . . N5 N 0.05206(15) 0.23777(14) 0.44065(13) 0.0338(5) Uani 1 1 d . . . H5X H 0.0662(18) 0.2921(18) 0.4763(16) 0.033(7) Uiso 1 1 d . . . N6 N -0.02635(14) 0.13711(13) 0.31162(12) 0.0316(4) Uani 1 1 d . . . C1 C 0.06302(17) 0.37964(15) 0.38268(15) 0.0310(5) Uani 1 1 d . . . H1A H 0.0174 0.4222 0.3749 0.037 Uiso 1 1 calc R . . H1B H 0.0675 0.3914 0.444 0.037 Uiso 1 1 calc R . . C2 C 0.17256(16) 0.45106(15) 0.31691(14) 0.0284(5) Uani 1 1 d . . . C3 C 0.23797(18) 0.35864(17) 0.39078(17) 0.0397(6) Uani 1 1 d . . . H3B H 0.2327 0.2908 0.3581 0.048 Uiso 1 1 calc R . . H3A H 0.2325 0.3729 0.452 0.048 Uiso 1 1 calc R . . C4 C 0.33502(19) 0.39586(18) 0.38093(18) 0.0432(6) Uani 1 1 d . . . H4B H 0.3494 0.4592 0.4261 0.052 Uiso 1 1 calc R . . H4A H 0.3861 0.3568 0.387 0.052 Uiso 1 1 calc R . . C5 C 0.33360(19) 0.39649(19) 0.29402(18) 0.0461(7) Uani 1 1 d . . . H5B H 0.3973 0.4204 0.2863 0.055 Uiso 1 1 calc R . . H5A H 0.3201 0.3331 0.2487 0.055 Uiso 1 1 calc R . . C6 C 0.2851(2) 0.52385(19) 0.25491(19) 0.0480(7) Uani 1 1 d . . . H6B H 0.2921 0.4915 0.1926 0.058 Uiso 1 1 calc R . . H6A H 0.3486 0.5552 0.2835 0.058 Uiso 1 1 calc R . . C7 C 0.2123(2) 0.59472(18) 0.26978(19) 0.0468(7) Uani 1 1 d . . . H7B H 0.2222 0.627 0.2327 0.056 Uiso 1 1 calc R . . H7A H 0.2201 0.6409 0.3303 0.056 Uiso 1 1 calc R . . C8 C 0.1130(2) 0.5476(2) 0.2494(2) 0.0499(7) Uani 1 1 d . . . H8B H 0.064 0.5941 0.2622 0.06 Uiso 1 1 calc R . . H8A H 0.1035 0.5056 0.1876 0.06 Uiso 1 1 calc R . . C9 C 0.01640(16) 0.21973(15) 0.36156(14) 0.0283(5) Uani 1 1 d . . . C10 C -0.0160(2) 0.26628(18) 0.24426(16) 0.0458(7) Uani 1 1 d . . . H10B H 0.0192 0.3058 0.2226 0.055 Uiso 1 1 calc R . . H10A H -0.0847 0.2812 0.2462 0.055 Uiso 1 1 calc R . . C11 C -0.0086(2) 0.16687(18) 0.18505(16) 0.0485(7) Uani 1 1 d . . . H11B H 0.0601 0.1525 0.1801 0.058 Uiso 1 1 calc R . . H11A H -0.0388 0.1538 0.1272 0.058 Uiso 1 1 calc R . . C12 C -0.0601(2) 0.10896(18) 0.22130(16) 0.0469(7) Uani 1 1 d . . . H12B H -0.1306 0.1155 0.2165 0.056 Uiso 1 1 calc R . . H12A H -0.0482 0.0433 0.1878 0.056 Uiso 1 1 calc R . . C13 C -0.04929(18) 0.06765(16) 0.34362(15) 0.0357(6) Uani 1 1 d . . . H13B H -0.0023 0.0193 0.3241 0.043 Uiso 1 1 calc R . . H13A H -0.1146 0.038 0.3191 0.043 Uiso 1 1 calc R . . C14 C -0.0464(2) 0.10909(17) 0.44014(16) 0.0413(6) Uani 1 1 d . . . H14B H -0.0477 0.0595 0.4601 0.05 Uiso 1 1 calc R . . H14A H -0.1036 0.1453 0.4595 0.05 Uiso 1 1 calc R . . C15 C 0.0450(2) 0.17074(16) 0.47730(16) 0.0400(6) Uani 1 1 d . . . H15B H 0.0444 0.2034 0.5404 0.048 Uiso 1 1 calc R . . H15A H 0.1019 0.133 0.4644 0.048 Uiso 1 1 calc R . . C16 C 0.34721(16) 0.72170(15) 0.57692(14) 0.0282(5) Uani 1 1 d . . . C17 C 0.26406(18) 0.73211(16) 0.53271(16) 0.0368(6) Uani 1 1 d . . . H17 H 0.264 0.7817 0.5162 0.044 Uiso 1 1 calc R . . C18 C 0.18196(18) 0.67343(17) 0.51203(17) 0.0422(6) Uani 1 1 d . . . H18 H 0.1273 0.6831 0.4816 0.051 Uiso 1 1 calc R . . C19 C 0.17860(19) 0.60091(17) 0.53513(17) 0.0432(7) Uani 1 1 d . . . H19 H 0.1215 0.5616 0.5225 0.052 Uiso 1 1 calc R . . C20 C 0.2600(2) 0.58644(17) 0.57700(16) 0.0433(7) Uani 1 1 d . . . H20 H 0.2597 0.5359 0.5922 0.052 Uiso 1 1 calc R . . C21 C 0.3425(2) 0.64579(17) 0.59694(16) 0.0390(6) Uani 1 1 d . . . H21 H 0.3978 0.6342 0.6253 0.047 Uiso 1 1 calc R . . C22 C 0.50318(16) 0.80972(14) 0.69154(14) 0.0277(5) Uani 1 1 d . . . C23 C 0.60198(17) 0.83506(15) 0.71123(15) 0.0323(5) Uani 1 1 d . . . H23 H 0.639 0.8364 0.6672 0.039 Uiso 1 1 calc R . . C24 C 0.64895(18) 0.85837(16) 0.79174(16) 0.0369(6) Uani 1 1 d . . . H24 H 0.7163 0.8754 0.8016 0.044 Uiso 1 1 calc R . . C25 C 0.5982(2) 0.85687(17) 0.85742(16) 0.0414(6) Uani 1 1 d . . . H25 H 0.6296 0.8728 0.9128 0.05 Uiso 1 1 calc R . . C26 C 0.5005(2) 0.8315(2) 0.84044(17) 0.0475(7) Uani 1 1 d . . . H26 H 0.4641 0.8295 0.8846 0.057 Uiso 1 1 calc R . . C27 C 0.45455(19) 0.80896(18) 0.75988(16) 0.0398(6) Uani 1 1 d . . . H27 H 0.3871 0.7922 0.7507 0.048 Uiso 1 1 calc R . . C28 C 0.40913(16) 0.89019(15) 0.60412(14) 0.0272(5) Uani 1 1 d . . . C29 C 0.41667(18) 0.92133(16) 0.54050(15) 0.0343(5) Uani 1 1 d . . . H29 H 0.4515 0.8869 0.4927 0.041 Uiso 1 1 calc R . . C30 C 0.37560(19) 1.00064(18) 0.54360(18) 0.0418(6) Uani 1 1 d . . . H30 H 0.3825 1.019 0.4984 0.05 Uiso 1 1 calc R . . C31 C 0.32489(19) 1.05258(17) 0.61231(18) 0.0428(6) Uani 1 1 d . . . H31 H 0.2963 1.1066 0.6147 0.051 Uiso 1 1 calc R . . C32 C 0.31638(18) 1.02486(17) 0.67734(17) 0.0403(6) Uani 1 1 d . . . H32 H 0.2821 1.0602 0.7253 0.048 Uiso 1 1 calc R . . C33 C 0.35753(17) 0.94568(16) 0.67310(15) 0.0341(6) Uani 1 1 d . . . H33 H 0.3506 0.9281 0.7188 0.041 Uiso 1 1 calc R . . C34 C 0.51814(16) 0.74259(15) 0.52056(14) 0.0281(5) Uani 1 1 d . . . C35 C 0.60105(17) 0.79006(17) 0.51240(15) 0.0326(5) Uani 1 1 d . . . H35 H 0.6103 0.8545 0.5468 0.039 Uiso 1 1 calc R . . C36 C 0.67029(18) 0.74674(19) 0.45600(16) 0.0394(6) Uani 1 1 d . . . H36 H 0.7261 0.7815 0.4538 0.047 Uiso 1 1 calc R . . C37 C 0.6582(2) 0.65383(19) 0.40343(16) 0.0429(7) Uani 1 1 d . . . H37 H 0.706 0.6237 0.366 0.051 Uiso 1 1 calc R . . C38 C 0.5757(2) 0.60550(18) 0.40615(16) 0.0421(6) Uani 1 1 d . . . H38 H 0.565 0.5419 0.3687 0.051 Uiso 1 1 calc R . . C39 C 0.50759(18) 0.64911(16) 0.46343(14) 0.0329(5) Uani 1 1 d . . . H39 H 0.4513 0.6139 0.4638 0.04 Uiso 1 1 calc R . . B1B B 0.89830(19) 0.19193(17) -0.09091(16) 0.0281(6) Uani 1 1 d . A 1 Cl1B Cl 0.42011(5) 0.40605(5) 0.07272(5) 0.0511(2) Uani 1 1 d . B 1 N1B N 0.50858(15) 0.71135(14) 0.19244(14) 0.0399(5) Uani 1 1 d . C 1 N2B N 0.51958(17) 0.76058(15) 0.08446(13) 0.0384(5) Uani 1 1 d . C 1 H2Y H 0.541(2) 0.7100(19) 0.0508(18) 0.047(8) Uiso 1 1 d . D 1 N3B N 0.45443(14) 0.85243(14) 0.20912(12) 0.0365(5) Uani 1 1 d . C 1 N4B N 0.64940(14) 0.62262(13) 0.17116(13) 0.0360(5) Uani 1 1 d . C 1 N5B N 0.62662(17) 0.47304(13) 0.15786(14) 0.0345(5) Uani 1 1 d . C 1 H5Y H 0.571(2) 0.4694(19) 0.1378(18) 0.045(9) Uiso 1 1 d . E 1 N6B N 0.78095(14) 0.54197(13) 0.18649(12) 0.0336(5) Uani 1 1 d . C 1 C1B C 0.5473(2) 0.62439(18) 0.1439(2) 0.0489(7) Uani 1 1 d . C 1 H1B1 H 0.5413 0.6116 0.0824 0.059 Uiso 1 1 calc R C 1 H1B2 H 0.5089 0.5751 0.1508 0.059 Uiso 1 1 calc R C 1 C2B C 0.49406(16) 0.77490(15) 0.16165(14) 0.0287(5) Uani 1 1 d . C 1 C3B C 0.4822(2) 0.7324(3) 0.2821(2) 0.0652(9) Uani 1 1 d . C 1 H3B2 H 0.4702 0.6741 0.2879 0.078 Uiso 1 1 calc R C 1 H3B1 H 0.5366 0.7686 0.3241 0.078 Uiso 1 1 calc R C 1 C4B C 0.3952(2) 0.7849(3) 0.2999(2) 0.0699(10) Uani 1 1 d . C 1 H4B2 H 0.3401 0.7481 0.2593 0.084 Uiso 1 1 calc R C 1 H4B1 H 0.3783 0.7992 0.3589 0.084 Uiso 1 1 calc R C 1 C5B C 0.4148(2) 0.8705(3) 0.29058(18) 0.0647(9) Uani 1 1 d . C 1 H5B2 H 0.3541 0.9021 0.2939 0.078 Uiso 1 1 calc R C 1 H5B1 H 0.4613 0.912 0.3383 0.078 Uiso 1 1 calc R C 1 C6B C 0.4425(2) 0.92673(18) 0.1811(2) 0.0537(8) Uani 1 1 d . C 1 H6B2 H 0.4572 0.9871 0.2308 0.064 Uiso 1 1 calc R C 1 H6B1 H 0.3744 0.9243 0.159 0.064 Uiso 1 1 calc R C 1 C7B C 0.5083(2) 0.9182(2) 0.1119(2) 0.0618(9) Uani 1 1 d . C 1 H7B2 H 0.4904 0.961 0.0864 0.074 Uiso 1 1 calc R C 1 H7B1 H 0.5761 0.9346 0.137 0.074 Uiso 1 1 calc R C 1 C8B C 0.4992(2) 0.82259(19) 0.04504(19) 0.0489(7) Uani 1 1 d . C 1 H8B2 H 0.4329 0.808 0.0162 0.059 Uiso 1 1 calc R C 1 H8B1 H 0.5453 0.8153 0.0014 0.059 Uiso 1 1 calc R C 1 C9B C 0.68634(17) 0.54504(16) 0.17064(14) 0.0302(5) Uani 1 1 d . C 1 C10B C 0.71585(19) 0.69608(18) 0.17082(19) 0.0455(7) Uani 1 1 d . C 1 H10D H 0.683 0.7544 0.1892 0.055 Uiso 1 1 calc R C 1 H10C H 0.7353 0.6794 0.1121 0.055 Uiso 1 1 calc R C 1 C11B C 0.80349(19) 0.70852(18) 0.23078(17) 0.0425(6) Uani 1 1 d . C 1 H11D H 0.7844 0.7279 0.29 0.051 Uiso 1 1 calc R C 1 H11C H 0.8491 0.757 0.2302 0.051 Uiso 1 1 calc R C 1 C12B C 0.85145(18) 0.61897(19) 0.20286(17) 0.0436(6) Uani 1 1 d . C 1 H12D H 0.8838 0.6074 0.15 0.052 Uiso 1 1 calc R C 1 H12C H 0.9015 0.6233 0.2481 0.052 Uiso 1 1 calc R C 1 C13B C 0.82115(19) 0.45450(18) 0.17441(17) 0.0433(6) Uani 1 1 d . C 1 H13D H 0.8854 0.4664 0.2068 0.052 Uiso 1 1 calc R C 1 H13C H 0.8295 0.4177 0.1129 0.052 Uiso 1 1 calc R C 1 C14B C 0.7544(2) 0.40193(19) 0.20545(18) 0.0485(7) Uani 1 1 d . C 1 H14D H 0.7799 0.3414 0.1946 0.058 Uiso 1 1 calc R C 1 H14C H 0.7506 0.4364 0.268 0.058 Uiso 1 1 calc R C 1 C15B C 0.6558(2) 0.38776(17) 0.16031(19) 0.0461(7) Uani 1 1 d . C 1 H15D H 0.6559 0.3393 0.1011 0.055 Uiso 1 1 calc R C 1 H15C H 0.6089 0.3669 0.1905 0.055 Uiso 1 1 calc R C 1 C16B C 0.85036(16) 0.13557(15) -0.04051(14) 0.0279(5) Uani 1 1 d . A 1 C17B C 0.87973(19) 0.04822(16) -0.05373(16) 0.0375(6) Uani 1 1 d . A 1 H17B H 0.9273 0.0226 -0.093 0.045 Uiso 1 1 calc R A 1 C18B C 0.8435(2) -0.00304(17) -0.01301(17) 0.0428(6) Uani 1 1 d . A 1 H18B H 0.8652 -0.0626 -0.0254 0.051 Uiso 1 1 calc R A 1 C19B C 0.77612(19) 0.03274(19) 0.04537(17) 0.0431(6) Uani 1 1 d . A 1 H19B H 0.7494 -0.0023 0.0726 0.052 Uiso 1 1 calc R A 1 C20B C 0.7478(2) 0.1201(2) 0.06389(18) 0.0480(7) Uani 1 1 d . A 1 H20B H 0.7032 0.1466 0.1058 0.058 Uiso 1 1 calc R A 1 C21B C 0.78445(18) 0.16968(18) 0.02143(16) 0.0395(6) Uani 1 1 d . A 1 H21B H 0.7635 0.2297 0.0353 0.047 Uiso 1 1 calc R A 1 C22B C 0.85307(17) 0.29231(15) -0.06881(13) 0.0287(5) Uani 1 1 d . A 1 C23B C 0.91059(18) 0.37234(16) -0.05212(15) 0.0336(5) Uani 1 1 d . A 1 H23B H 0.9789 0.3695 -0.0499 0.04 Uiso 1 1 calc R A 1 C24B C 0.8721(2) 0.45596(16) -0.03871(15) 0.0389(6) Uani 1 1 d . A 1 H24B H 0.9142 0.5082 -0.0283 0.047 Uiso 1 1 calc R A 1 C25B C 0.7740(2) 0.46373(17) -0.04029(15) 0.0389(6) Uani 1 1 d . A 1 H25B H 0.7477 0.5211 -0.0297 0.047 Uiso 1 1 calc R A 1 C26B C 0.71414(19) 0.38594(17) -0.05776(15) 0.0386(6) Uani 1 1 d . A 1 H26B H 0.646 0.3898 -0.0594 0.046 Uiso 1 1 calc R A 1 C27B C 0.75285(17) 0.30265(16) -0.07283(15) 0.0332(5) Uani 1 1 d . A 1 H27B H 0.7099 0.2501 -0.0865 0.04 Uiso 1 1 calc R A 1 C28B C 1.01438(16) 0.20677(15) -0.05877(14) 0.0297(5) Uani 1 1 d . A 1 C29B C 1.08785(17) 0.16384(16) -0.11000(16) 0.0337(5) Uani 1 1 d . A 1 H29B H 1.0713 0.1248 -0.1689 0.04 Uiso 1 1 calc R A 1 C30B C 1.18451(18) 0.17590(18) -0.07836(19) 0.0423(6) Uani 1 1 d . A 1 H30B H 1.2322 0.1448 -0.1154 0.051 Uiso 1 1 calc R A 1 C31B C 1.21112(19) 0.23288(19) 0.00659(19) 0.0460(7) Uani 1 1 d . A 1 H31B H 1.2771 0.242 0.0283 0.055 Uiso 1 1 calc R A 1 C32B C 1.1407(2) 0.27629(19) 0.05933(18) 0.0467(7) Uani 1 1 d . A 1 H32B H 1.1579 0.3157 0.118 0.056 Uiso 1 1 calc R A 1 C33B C 1.04481(18) 0.26275(17) 0.02727(16) 0.0387(6) Uani 1 1 d . A 1 H33B H 0.9975 0.2928 0.0653 0.046 Uiso 1 1 calc R A 1 C34B C 0.87875(16) 0.13573(16) -0.19605(14) 0.0303(5) Uani 1 1 d . A 1 C35B C 0.9101(2) 0.17666(18) -0.24848(16) 0.0438(6) Uani 1 1 d . A 1 H35B H 0.9472 0.2339 -0.2222 0.053 Uiso 1 1 calc R A 1 C36B C 0.8898(2) 0.1379(2) -0.33641(17) 0.0520(7) Uani 1 1 d . A 1 H36B H 0.9125 0.1687 -0.369 0.062 Uiso 1 1 calc R A 1 C37B C 0.8366(2) 0.0544(2) -0.37711(17) 0.0511(8) Uani 1 1 d . A 1 H37B H 0.8216 0.0277 -0.4375 0.061 Uiso 1 1 calc R A 1 C38B C 0.80573(19) 0.0106(2) -0.32833(17) 0.0501(7) Uani 1 1 d . A 1 H38B H 0.7698 -0.0472 -0.3554 0.06 Uiso 1 1 calc R A 1 C39B C 0.82685(17) 0.05069(17) -0.23958(15) 0.0375(6) Uani 1 1 d . A 1 H39B H 0.8051 0.0189 -0.2076 0.045 Uiso 1 1 calc R A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.0292(14) 0.0282(13) 0.0277(13) 0.0139(11) 0.0013(11) -0.0018(11) Cl1 0.0340(3) 0.0343(3) 0.0288(3) 0.0096(2) 0.0059(2) 0.0028(2) N1 0.0308(11) 0.0281(10) 0.0301(10) 0.0141(9) 0.0048(8) 0.0036(8) N2 0.0320(12) 0.0449(12) 0.0408(12) 0.0290(10) 0.0141(10) 0.0101(10) N3 0.0320(11) 0.0354(11) 0.0384(11) 0.0172(9) 0.0122(9) 0.0055(9) N4 0.0393(12) 0.0288(10) 0.0266(10) 0.0134(8) -0.0008(8) -0.0019(9) N5 0.0474(13) 0.0263(11) 0.0283(11) 0.0129(9) -0.0008(9) -0.0012(9) N6 0.0370(11) 0.0300(10) 0.0271(10) 0.0119(9) 0.0002(8) -0.0014(9) C1 0.0395(14) 0.0272(12) 0.0292(12) 0.0139(10) 0.0086(10) 0.0052(10) C2 0.0307(13) 0.0287(12) 0.0245(11) 0.0097(10) 0.0042(10) 0.0021(10) C3 0.0420(15) 0.0377(14) 0.0433(15) 0.0211(12) -0.0014(12) 0.0080(12) C4 0.0363(15) 0.0397(14) 0.0534(17) 0.0198(13) -0.0007(12) 0.0082(12) C5 0.0370(15) 0.0436(15) 0.0586(18) 0.0204(14) 0.0145(13) 0.0132(12) C6 0.0416(16) 0.0536(17) 0.0597(18) 0.0326(15) 0.0203(13) 0.0028(13) C7 0.0554(18) 0.0444(15) 0.0520(17) 0.0295(14) 0.0183(14) 0.0055(13) C8 0.0447(16) 0.0667(19) 0.0637(19) 0.0506(16) 0.0148(14) 0.0106(14) C9 0.0283(12) 0.0300(12) 0.0276(12) 0.0127(10) 0.0049(10) 0.0044(10) C10 0.0586(18) 0.0459(15) 0.0368(14) 0.0241(13) -0.0123(13) -0.0067(13) C11 0.0661(19) 0.0479(16) 0.0280(13) 0.0151(12) -0.0055(13) -0.0124(14) C12 0.0619(19) 0.0411(15) 0.0323(14) 0.0125(12) -0.0048(13) -0.0122(13) C13 0.0370(14) 0.0304(13) 0.0412(14) 0.0172(11) 0.0025(11) -0.0029(10) C14 0.0548(17) 0.0332(13) 0.0428(15) 0.0213(12) 0.0149(13) 0.0025(12) C15 0.0605(18) 0.0313(13) 0.0324(13) 0.0178(11) 0.0032(12) 0.0015(12) C16 0.0313(13) 0.0272(12) 0.0251(11) 0.0099(10) 0.0054(10) 0.0018(10) C17 0.0368(14) 0.0276(12) 0.0440(15) 0.0136(11) 0.0015(11) 0.0007(10) C18 0.0297(14) 0.0341(14) 0.0481(16) 0.0035(12) 0.0003(12) 0.0020(11) C19 0.0375(15) 0.0345(14) 0.0419(15) 0.0003(12) 0.0140(12) -0.0097(11) C20 0.0611(19) 0.0327(13) 0.0360(14) 0.0142(12) 0.0134(13) -0.0095(12) C21 0.0488(16) 0.0359(13) 0.0337(13) 0.0170(11) 0.0017(12) -0.0042(12) C22 0.0333(13) 0.0214(11) 0.0302(12) 0.0127(10) 0.0019(10) 0.0022(9) C23 0.0363(14) 0.0299(12) 0.0327(13) 0.0153(10) 0.0029(10) 0.0011(10) C24 0.0334(14) 0.0336(13) 0.0429(15) 0.0172(12) -0.0063(11) -0.0025(11) C25 0.0486(16) 0.0430(15) 0.0338(14) 0.0194(12) -0.0084(12) -0.0004(12) C26 0.0483(17) 0.0684(19) 0.0341(14) 0.0308(14) 0.0001(12) -0.0033(14) C27 0.0340(14) 0.0542(16) 0.0364(14) 0.0251(13) 0.0003(11) -0.0022(12) C28 0.0249(12) 0.0283(12) 0.0275(12) 0.0120(10) -0.0033(9) -0.0050(9) C29 0.0367(14) 0.0367(13) 0.0331(13) 0.0185(11) 0.0009(11) 0.0023(11) C30 0.0418(15) 0.0451(15) 0.0496(16) 0.0311(13) 0.0020(12) 0.0034(12) C31 0.0386(15) 0.0330(14) 0.0616(18) 0.0255(13) -0.0026(13) 0.0051(11) C32 0.0375(15) 0.0327(13) 0.0447(15) 0.0103(12) 0.0042(12) 0.0044(11) C33 0.0383(14) 0.0314(13) 0.0333(13) 0.0144(11) 0.0039(11) 0.0004(11) C34 0.0284(12) 0.0324(12) 0.0284(12) 0.0182(10) -0.0017(9) 0.0027(10) C35 0.0345(14) 0.0361(13) 0.0321(13) 0.0196(11) 0.0008(10) 0.0011(10) C36 0.0303(14) 0.0603(17) 0.0390(14) 0.0319(14) 0.0044(11) 0.0054(12) C37 0.0430(16) 0.0581(18) 0.0353(14) 0.0250(13) 0.0118(12) 0.0200(13) C38 0.0531(17) 0.0390(14) 0.0346(14) 0.0147(12) 0.0082(12) 0.0123(13) C39 0.0367(14) 0.0339(13) 0.0309(13) 0.0162(11) 0.0032(10) 0.0033(10) B1B 0.0302(14) 0.0274(13) 0.0253(13) 0.0100(11) 0.0032(11) -0.0003(11) Cl1B 0.0347(4) 0.0418(4) 0.0547(4) -0.0018(3) 0.0105(3) 0.0005(3) N1B 0.0388(12) 0.0433(12) 0.0489(13) 0.0311(11) -0.0009(10) 0.0005(10) N2B 0.0575(15) 0.0313(11) 0.0317(11) 0.0165(10) 0.0118(10) 0.0178(10) N3B 0.0318(11) 0.0362(11) 0.0315(11) 0.0045(9) 0.0018(9) 0.0039(9) N4B 0.0341(12) 0.0338(11) 0.0476(12) 0.0263(10) -0.0054(9) -0.0044(9) N5B 0.0331(13) 0.0282(11) 0.0437(13) 0.0171(10) 0.0006(10) 0.0035(9) N6B 0.0307(11) 0.0382(11) 0.0316(11) 0.0147(9) 0.0008(9) 0.0035(9) C1B 0.0461(17) 0.0381(15) 0.0680(19) 0.0321(14) -0.0209(14) -0.0094(12) C2B 0.0273(12) 0.0291(12) 0.0304(12) 0.0143(10) -0.0033(10) -0.0027(10) C3B 0.064(2) 0.096(3) 0.060(2) 0.059(2) -0.0015(16) -0.0063(19) C4B 0.051(2) 0.111(3) 0.0374(17) 0.0232(18) 0.0055(14) -0.0129(19) C5B 0.0496(19) 0.092(3) 0.0357(16) 0.0091(16) 0.0086(14) 0.0112(17) C6B 0.0439(17) 0.0289(14) 0.073(2) 0.0078(14) -0.0052(15) 0.0097(12) C7B 0.067(2) 0.0440(17) 0.088(2) 0.0429(18) -0.0042(18) -0.0002(15) C8B 0.0538(18) 0.0546(17) 0.0554(17) 0.0390(15) 0.0083(14) 0.0092(14) C9B 0.0373(14) 0.0332(13) 0.0216(11) 0.0125(10) 0.0053(10) 0.0036(11) C10B 0.0442(16) 0.0426(15) 0.0599(18) 0.0334(14) -0.0012(13) -0.0085(12) C11B 0.0424(16) 0.0437(15) 0.0446(15) 0.0233(13) 0.0004(12) -0.0108(12) C12B 0.0327(14) 0.0577(17) 0.0414(15) 0.0231(13) -0.0008(11) -0.0057(12) C13B 0.0419(16) 0.0435(15) 0.0355(14) 0.0077(12) 0.0002(12) 0.0123(12) C14B 0.0613(19) 0.0404(15) 0.0454(16) 0.0190(13) 0.0018(14) 0.0178(14) C15B 0.0479(17) 0.0302(13) 0.0623(18) 0.0211(13) 0.0064(14) 0.0073(12) C16B 0.0271(12) 0.0304(12) 0.0236(11) 0.0097(10) -0.0018(9) -0.0017(10) C17B 0.0441(15) 0.0271(12) 0.0403(14) 0.0122(11) 0.0109(12) 0.0026(11) C18B 0.0531(17) 0.0320(13) 0.0439(15) 0.0175(12) 0.0009(13) -0.0032(12) C19B 0.0423(16) 0.0513(16) 0.0446(15) 0.0308(14) -0.0014(12) -0.0109(13) C20B 0.0417(16) 0.070(2) 0.0452(16) 0.0346(15) 0.0143(13) 0.0095(14) C21B 0.0417(15) 0.0453(15) 0.0387(14) 0.0232(12) 0.0099(12) 0.0116(12) C22B 0.0341(13) 0.0303(12) 0.0205(11) 0.0100(10) 0.0007(9) -0.0009(10) C23B 0.0349(13) 0.0322(13) 0.0325(13) 0.0131(11) 0.0006(10) -0.0020(10) C24B 0.0497(17) 0.0283(13) 0.0360(14) 0.0126(11) -0.0039(12) -0.0065(11) C25B 0.0514(17) 0.0323(13) 0.0312(13) 0.0124(11) -0.0039(11) 0.0072(12) C26B 0.0352(14) 0.0451(15) 0.0348(14) 0.0169(12) -0.0044(11) 0.0080(12) C27B 0.0338(14) 0.0336(13) 0.0312(13) 0.0140(11) -0.0037(10) -0.0034(10) C28B 0.0312(13) 0.0285(12) 0.0317(12) 0.0153(10) 0.0023(10) -0.0009(10) C29B 0.0384(14) 0.0310(12) 0.0379(13) 0.0201(11) 0.0078(11) 0.0006(10) C30B 0.0325(14) 0.0452(15) 0.0653(19) 0.0377(15) 0.0133(13) 0.0055(12) C31B 0.0308(14) 0.0505(16) 0.069(2) 0.0401(16) -0.0073(13) -0.0069(12) C32B 0.0456(17) 0.0462(16) 0.0465(16) 0.0206(13) -0.0124(13) -0.0084(13) C33B 0.0363(14) 0.0435(15) 0.0330(13) 0.0135(12) -0.0002(11) 0.0015(11) C34B 0.0290(13) 0.0327(12) 0.0268(12) 0.0097(10) 0.0050(10) 0.0047(10) C35B 0.0595(18) 0.0406(15) 0.0293(13) 0.0126(12) 0.0068(12) 0.0030(13) C36B 0.070(2) 0.0590(19) 0.0322(14) 0.0224(14) 0.0108(14) 0.0172(16) C37B 0.0444(17) 0.075(2) 0.0238(13) 0.0096(14) 0.0020(12) 0.0178(15) C38B 0.0306(14) 0.0609(18) 0.0361(15) -0.0011(14) 0.0010(12) -0.0025(13) C39B 0.0292(13) 0.0435(14) 0.0304(13) 0.0067(11) 0.0041(10) -0.0018(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 B1 C16 1.648(3) . ? B1 C28 1.648(3) . ? B1 C34 1.653(3) . ? B1 C22 1.666(3) . ? N1 C2 1.354(3) . ? N1 C1 1.453(3) . ? N1 C3 1.481(3) . ? N2 C2 1.331(3) . ? N2 C8 1.460(3) . ? N2 H2X 0.79(3) . ? N3 C2 1.330(3) . ? N3 C5 1.468(3) . ? N3 C6 1.472(3) . ? N4 C9 1.359(3) . ? N4 C1 1.461(3) . ? N4 C10 1.467(3) . ? N5 C9 1.328(3) . ? N5 C15 1.461(3) . ? N5 H5X 0.84(3) . ? N6 C9 1.331(3) . ? N6 C12 1.467(3) . ? N6 C13 1.469(3) . ? C1 H1A 0.99 . ? C1 H1B 0.99 . ? C3 C4 1.503(4) . ? C3 H3B 0.99 . ? C3 H3A 0.99 . ? C4 C5 1.502(4) . ? C4 H4B 0.99 . ? C4 H4A 0.99 . ? C5 H5B 0.99 . ? C5 H5A 0.99 . ? C6 C7 1.497(4) . ? C6 H6B 0.99 . ? C6 H6A 0.99 . ? C7 C8 1.498(4) . ? C7 H7B 0.99 . ? C7 H7A 0.99 . ? C8 H8B 0.99 . ? C8 H8A 0.99 . ? C10 C11 1.499(4) . ? C10 H10B 0.99 . ? C10 H10A 0.99 . ? C11 C12 1.503(4) . ? C11 H11B 0.99 . ? C11 H11A 0.99 . ? C12 H12B 0.99 . ? C12 H12A 0.99 . ? C13 C14 1.508(3) . ? C13 H13B 0.99 . ? C13 H13A 0.99 . ? C14 C15 1.510(4) . ? C14 H14B 0.99 . ? C14 H14A 0.99 . ? C15 H15B 0.99 . ? C15 H15A 0.99 . ? C16 C17 1.398(3) . ? C16 C21 1.398(3) . ? C17 C18 1.381(3) . ? C17 H17 0.95 . ? C18 C19 1.378(4) . ? C18 H18 0.95 . ? C19 C20 1.382(4) . ? C19 H19 0.95 . ? C20 C21 1.392(4) . ? C20 H20 0.95 . ? C21 H21 0.95 . ? C22 C23 1.397(3) . ? C22 C27 1.398(3) . ? C23 C24 1.388(3) . ? C23 H23 0.95 . ? C24 C25 1.378(4) . ? C24 H24 0.95 . ? C25 C26 1.381(4) . ? C25 H25 0.95 . ? C26 C27 1.385(3) . ? C26 H26 0.95 . ? C27 H27 0.95 . ? C28 C29 1.391(3) . ? C28 C33 1.406(3) . ? C29 C30 1.393(3) . ? C29 H29 0.95 . ? C30 C31 1.380(4) . ? C30 H30 0.95 . ? C31 C32 1.378(4) . ? C31 H31 0.95 . ? C32 C33 1.385(3) . ? C32 H32 0.95 . ? C33 H33 0.95 . ? C34 C39 1.401(3) . ? C34 C35 1.405(3) . ? C35 C36 1.394(3) . ? C35 H35 0.95 . ? C36 C37 1.377(4) . ? C36 H36 0.95 . ? C37 C38 1.376(4) . ? C37 H37 0.95 . ? C38 C39 1.392(3) . ? C38 H38 0.95 . ? C39 H39 0.95 . ? B1B C16B 1.644(3) . ? B1B C22B 1.646(3) . ? B1B C28B 1.647(3) . ? B1B C34B 1.650(3) . ? N1B C2B 1.347(3) . ? N1B C1B 1.434(3) . ? N1B C3B 1.509(4) . ? N2B C2B 1.325(3) . ? N2B C8B 1.447(3) . ? N2B H2Y 0.85(3) . ? N3B C2B 1.328(3) . ? N3B C5B 1.457(3) . ? N3B C6B 1.472(4) . ? N4B C9B 1.358(3) . ? N4B C1B 1.470(3) . ? N4B C10B 1.473(3) . ? N5B C9B 1.329(3) . ? N5B C15B 1.455(3) . ? N5B H5Y 0.81(3) . ? N6B C9B 1.332(3) . ? N6B C13B 1.464(3) . ? N6B C12B 1.467(3) . ? C1B H1B1 0.99 . ? C1B H1B2 0.99 . ? C3B C4B 1.470(5) . ? C3B H3B2 0.99 . ? C3B H3B1 0.99 . ? C4B C5B 1.467(5) . ? C4B H4B2 0.99 . ? C4B H4B1 0.99 . ? C5B H5B2 0.99 . ? C5B H5B1 0.99 . ? C6B C7B 1.511(4) . ? C6B H6B2 0.99 . ? C6B H6B1 0.99 . ? C7B C8B 1.475(4) . ? C7B H7B2 0.99 . ? C7B H7B1 0.99 . ? C8B H8B2 0.99 . ? C8B H8B1 0.99 . ? C10B C11B 1.498(4) . ? C10B H10D 0.99 . ? C10B H10C 0.99 . ? C11B C12B 1.503(4) . ? C11B H11D 0.99 . ? C11B H11C 0.99 . ? C12B H12D 0.99 . ? C12B H12C 0.99 . ? C13B C14B 1.498(4) . ? C13B H13D 0.99 . ? C13B H13C 0.99 . ? C14B C15B 1.493(4) . ? C14B H14D 0.99 . ? C14B H14C 0.99 . ? C15B H15D 0.99 . ? C15B H15C 0.99 . ? C16B C21B 1.393(3) . ? C16B C17B 1.400(3) . ? C17B C18B 1.386(3) . ? C17B H17B 0.95 . ? C18B C19B 1.373(4) . ? C18B H18B 0.95 . ? C19B C20B 1.376(4) . ? C19B H19B 0.95 . ? C20B C21B 1.390(4) . ? C20B H20B 0.95 . ? C21B H21B 0.95 . ? C22B C23B 1.399(3) . ? C22B C27B 1.408(3) . ? C23B C24B 1.392(3) . ? C23B H23B 0.95 . ? C24B C25B 1.372(4) . ? C24B H24B 0.95 . ? C25B C26B 1.385(4) . ? C25B H25B 0.95 . ? C26B C27B 1.383(3) . ? C26B H26B 0.95 . ? C27B H27B 0.95 . ? C28B C29B 1.393(3) . ? C28B C33B 1.401(3) . ? C29B C30B 1.393(4) . ? C29B H29B 0.95 . ? C30B C31B 1.379(4) . ? C30B H30B 0.95 . ? C31B C32B 1.375(4) . ? C31B H31B 0.95 . ? C32B C33B 1.383(4) . ? C32B H32B 0.95 . ? C33B H33B 0.95 . ? C34B C39B 1.395(3) . ? C34B C35B 1.402(3) . ? C35B C36B 1.381(4) . ? C35B H35B 0.95 . ? C36B C37B 1.381(4) . ? C36B H36B 0.95 . ? C37B C38B 1.380(4) . ? C37B H37B 0.95 . ? C38B C39B 1.395(3) . ? C38B H38B 0.95 . ? C39B H39B 0.95 . ? 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 C16 B1 C28 106.56(18) . . ? C16 B1 C34 108.66(18) . . ? C28 B1 C34 113.34(18) . . ? C16 B1 C22 111.58(18) . . ? C28 B1 C22 107.56(17) . . ? C34 B1 C22 109.16(18) . . ? C2 N1 C1 123.09(19) . . ? C2 N1 C3 122.39(19) . . ? C1 N1 C3 114.47(18) . . ? C2 N2 C8 121.1(2) . . ? C2 N2 H2X 120(2) . . ? C8 N2 H2X 116(2) . . ? C2 N3 C5 119.9(2) . . ? C2 N3 C6 123.1(2) . . ? C5 N3 C6 116.8(2) . . ? C9 N4 C1 123.82(19) . . ? C9 N4 C10 120.63(19) . . ? C1 N4 C10 115.00(18) . . ? C9 N5 C15 122.7(2) . . ? C9 N5 H5X 120.4(17) . . ? C15 N5 H5X 114.9(17) . . ? C9 N6 C12 123.4(2) . . ? C9 N6 C13 122.75(19) . . ? C12 N6 C13 113.78(19) . . ? N1 C1 N4 112.09(18) . . ? N1 C1 H1A 109.2 . . ? N4 C1 H1A 109.2 . . ? N1 C1 H1B 109.2 . . ? N4 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? N3 C2 N2 119.4(2) . . ? N3 C2 N1 120.3(2) . . ? N2 C2 N1 120.2(2) . . ? N1 C3 C4 111.8(2) . . ? N1 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? N1 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? H3B C3 H3A 107.9 . . ? C5 C4 C3 109.0(2) . . ? C5 C4 H4B 109.9 . . ? C3 C4 H4B 109.9 . . ? C5 C4 H4A 109.9 . . ? C3 C4 H4A 109.9 . . ? H4B C4 H4A 108.3 . . ? N3 C5 C4 108.5(2) . . ? N3 C5 H5B 110 . . ? C4 C5 H5B 110 . . ? N3 C5 H5A 110 . . ? C4 C5 H5A 110 . . ? H5B C5 H5A 108.4 . . ? N3 C6 C7 112.7(2) . . ? N3 C6 H6B 109.1 . . ? C7 C6 H6B 109.1 . . ? N3 C6 H6A 109.1 . . ? C7 C6 H6A 109.1 . . ? H6B C6 H6A 107.8 . . ? C6 C7 C8 108.8(2) . . ? C6 C7 H7B 109.9 . . ? C8 C7 H7B 109.9 . . ? C6 C7 H7A 109.9 . . ? C8 C7 H7A 109.9 . . ? H7B C7 H7A 108.3 . . ? N2 C8 C7 110.0(2) . . ? N2 C8 H8B 109.7 . . ? C7 C8 H8B 109.7 . . ? N2 C8 H8A 109.7 . . ? C7 C8 H8A 109.7 . . ? H8B C8 H8A 108.2 . . ? N5 C9 N6 120.0(2) . . ? N5 C9 N4 120.2(2) . . ? N6 C9 N4 119.8(2) . . ? N4 C10 C11 110.0(2) . . ? N4 C10 H10B 109.7 . . ? C11 C10 H10B 109.7 . . ? N4 C10 H10A 109.7 . . ? C11 C10 H10A 109.7 . . ? H10B C10 H10A 108.2 . . ? C10 C11 C12 108.2(2) . . ? C10 C11 H11B 110.1 . . ? C12 C11 H11B 110.1 . . ? C10 C11 H11A 110.1 . . ? C12 C11 H11A 110.1 . . ? H11B C11 H11A 108.4 . . ? N6 C12 C11 110.9(2) . . ? N6 C12 H12B 109.5 . . ? C11 C12 H12B 109.5 . . ? N6 C12 H12A 109.5 . . ? C11 C12 H12A 109.5 . . ? H12B C12 H12A 108.1 . . ? N6 C13 C14 112.02(19) . . ? N6 C13 H13B 109.2 . . ? C14 C13 H13B 109.2 . . ? N6 C13 H13A 109.2 . . ? C14 C13 H13A 109.2 . . ? H13B C13 H13A 107.9 . . ? C13 C14 C15 109.0(2) . . ? C13 C14 H14B 109.9 . . ? C15 C14 H14B 109.9 . . ? C13 C14 H14A 109.9 . . ? C15 C14 H14A 109.9 . . ? H14B C14 H14A 108.3 . . ? N5 C15 C14 109.9(2) . . ? N5 C15 H15B 109.7 . . ? C14 C15 H15B 109.7 . . ? N5 C15 H15A 109.7 . . ? C14 C15 H15A 109.7 . . ? H15B C15 H15A 108.2 . . ? C17 C16 C21 115.2(2) . . ? C17 C16 B1 121.6(2) . . ? C21 C16 B1 123.2(2) . . ? C18 C17 C16 122.8(2) . . ? C18 C17 H17 118.6 . . ? C16 C17 H17 118.6 . . ? C19 C18 C17 120.6(3) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C20 118.7(2) . . ? C18 C19 H19 120.7 . . ? C20 C19 H19 120.7 . . ? C19 C20 C21 120.1(2) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C16 122.6(3) . . ? C20 C21 H21 118.7 . . ? C16 C21 H21 118.7 . . ? C23 C22 C27 114.4(2) . . ? C23 C22 B1 123.3(2) . . ? C27 C22 B1 122.1(2) . . ? C24 C23 C22 123.5(2) . . ? C24 C23 H23 118.3 . . ? C22 C23 H23 118.3 . . ? C25 C24 C23 120.3(2) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 118.1(2) . . ? C24 C25 H25 121 . . ? C26 C25 H25 121 . . ? C25 C26 C27 121.0(2) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C26 C27 C22 122.8(2) . . ? C26 C27 H27 118.6 . . ? C22 C27 H27 118.6 . . ? C29 C28 C33 114.9(2) . . ? C29 C28 B1 124.5(2) . . ? C33 C28 B1 120.3(2) . . ? C28 C29 C30 123.1(2) . . ? C28 C29 H29 118.5 . . ? C30 C29 H29 118.5 . . ? C31 C30 C29 120.0(2) . . ? C31 C30 H30 120 . . ? C29 C30 H30 120 . . ? C32 C31 C30 118.9(2) . . ? C32 C31 H31 120.5 . . ? C30 C31 H31 120.5 . . ? C31 C32 C33 120.3(2) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C32 C33 C28 122.8(2) . . ? C32 C33 H33 118.6 . . ? C28 C33 H33 118.6 . . ? C39 C34 C35 114.4(2) . . ? C39 C34 B1 122.8(2) . . ? C35 C34 B1 122.5(2) . . ? C36 C35 C34 122.9(2) . . ? C36 C35 H35 118.5 . . ? C34 C35 H35 118.5 . . ? C37 C36 C35 120.3(2) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C38 C37 C36 118.8(2) . . ? C38 C37 H37 120.6 . . ? C36 C37 H37 120.6 . . ? C37 C38 C39 120.5(2) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C38 C39 C34 123.0(2) . . ? C38 C39 H39 118.5 . . ? C34 C39 H39 118.5 . . ? C16B B1B C22B 113.52(18) . . ? C16B B1B C28B 104.78(18) . . ? C22B B1B C28B 110.07(18) . . ? C16B B1B C34B 112.29(18) . . ? C22B B1B C34B 104.22(18) . . ? C28B B1B C34B 112.16(18) . . ? C2B N1B C1B 123.2(2) . . ? C2B N1B C3B 118.4(2) . . ? C1B N1B C3B 118.4(2) . . ? C2B N2B C8B 123.0(2) . . ? C2B N2B H2Y 122.3(19) . . ? C8B N2B H2Y 113.9(19) . . ? C2B N3B C5B 124.0(2) . . ? C2B N3B C6B 122.1(2) . . ? C5B N3B C6B 113.7(2) . . ? C9B N4B C1B 121.7(2) . . ? C9B N4B C10B 119.0(2) . . ? C1B N4B C10B 116.23(19) . . ? C9B N5B C15B 125.1(2) . . ? C9B N5B H5Y 120(2) . . ? C15B N5B H5Y 113(2) . . ? C9B N6B C13B 119.9(2) . . ? C9B N6B C12B 123.3(2) . . ? C13B N6B C12B 116.0(2) . . ? N1B C1B N4B 112.3(2) . . ? N1B C1B H1B1 109.2 . . ? N4B C1B H1B1 109.2 . . ? N1B C1B H1B2 109.2 . . ? N4B C1B H1B2 109.2 . . ? H1B1 C1B H1B2 107.9 . . ? N2B C2B N3B 119.9(2) . . ? N2B C2B N1B 120.3(2) . . ? N3B C2B N1B 119.8(2) . . ? C4B C3B N1B 110.0(2) . . ? C4B C3B H3B2 109.7 . . ? N1B C3B H3B2 109.7 . . ? C4B C3B H3B1 109.7 . . ? N1B C3B H3B1 109.7 . . ? H3B2 C3B H3B1 108.2 . . ? C5B C4B C3B 108.6(3) . . ? C5B C4B H4B2 110 . . ? C3B C4B H4B2 110 . . ? C5B C4B H4B1 110 . . ? C3B C4B H4B1 110 . . ? H4B2 C4B H4B1 108.4 . . ? N3B C5B C4B 111.3(3) . . ? N3B C5B H5B2 109.4 . . ? C4B C5B H5B2 109.4 . . ? N3B C5B H5B1 109.4 . . ? C4B C5B H5B1 109.4 . . ? H5B2 C5B H5B1 108 . . ? N3B C6B C7B 111.3(2) . . ? N3B C6B H6B2 109.4 . . ? C7B C6B H6B2 109.4 . . ? N3B C6B H6B1 109.4 . . ? C7B C6B H6B1 109.4 . . ? H6B2 C6B H6B1 108 . . ? C8B C7B C6B 109.4(2) . . ? C8B C7B H7B2 109.8 . . ? C6B C7B H7B2 109.8 . . ? C8B C7B H7B1 109.8 . . ? C6B C7B H7B1 109.8 . . ? H7B2 C7B H7B1 108.3 . . ? N2B C8B C7B 109.0(2) . . ? N2B C8B H8B2 109.9 . . ? C7B C8B H8B2 109.9 . . ? N2B C8B H8B1 109.9 . . ? C7B C8B H8B1 109.9 . . ? H8B2 C8B H8B1 108.3 . . ? N5B C9B N6B 119.9(2) . . ? N5B C9B N4B 119.3(2) . . ? N6B C9B N4B 120.7(2) . . ? N4B C10B C11B 109.2(2) . . ? N4B C10B H10D 109.8 . . ? C11B C10B H10D 109.8 . . ? N4B C10B H10C 109.8 . . ? C11B C10B H10C 109.8 . . ? H10D C10B H10C 108.3 . . ? C10B C11B C12B 109.2(2) . . ? C10B C11B H11D 109.8 . . ? C12B C11B H11D 109.8 . . ? C10B C11B H11C 109.8 . . ? C12B C11B H11C 109.8 . . ? H11D C11B H11C 108.3 . . ? N6B C12B C11B 111.2(2) . . ? N6B C12B H12D 109.4 . . ? C11B C12B H12D 109.4 . . ? N6B C12B H12C 109.4 . . ? C11B C12B H12C 109.4 . . ? H12D C12B H12C 108 . . ? N6B C13B C14B 109.6(2) . . ? N6B C13B H13D 109.8 . . ? C14B C13B H13D 109.8 . . ? N6B C13B H13C 109.8 . . ? C14B C13B H13C 109.8 . . ? H13D C13B H13C 108.2 . . ? C15B C14B C13B 110.2(2) . . ? C15B C14B H14D 109.6 . . ? C13B C14B H14D 109.6 . . ? C15B C14B H14C 109.6 . . ? C13B C14B H14C 109.6 . . ? H14D C14B H14C 108.1 . . ? N5B C15B C14B 110.4(2) . . ? N5B C15B H15D 109.6 . . ? C14B C15B H15D 109.6 . . ? N5B C15B H15C 109.6 . . ? C14B C15B H15C 109.6 . . ? H15D C15B H15C 108.1 . . ? C21B C16B C17B 113.9(2) . . ? C21B C16B B1B 125.4(2) . . ? C17B C16B B1B 120.5(2) . . ? C18B C17B C16B 123.9(2) . . ? C18B C17B H17B 118 . . ? C16B C17B H17B 118 . . ? C19B C18B C17B 119.6(2) . . ? C19B C18B H18B 120.2 . . ? C17B C18B H18B 120.2 . . ? C18B C19B C20B 119.0(2) . . ? C18B C19B H19B 120.5 . . ? C20B C19B H19B 120.5 . . ? C19B C20B C21B 120.2(2) . . ? C19B C20B H20B 119.9 . . ? C21B C20B H20B 119.9 . . ? C20B C21B C16B 123.2(2) . . ? C20B C21B H21B 118.4 . . ? C16B C21B H21B 118.4 . . ? C23B C22B C27B 114.5(2) . . ? C23B C22B B1B 122.8(2) . . ? C27B C22B B1B 122.5(2) . . ? C24B C23B C22B 122.9(2) . . ? C24B C23B H23B 118.6 . . ? C22B C23B H23B 118.6 . . ? C25B C24B C23B 120.7(2) . . ? C25B C24B H24B 119.7 . . ? C23B C24B H24B 119.7 . . ? C24B C25B C26B 118.5(2) . . ? C24B C25B H25B 120.8 . . ? C26B C25B H25B 120.8 . . ? C27B C26B C25B 120.5(2) . . ? C27B C26B H26B 119.7 . . ? C25B C26B H26B 119.7 . . ? C26B C27B C22B 122.9(2) . . ? C26B C27B H27B 118.5 . . ? C22B C27B H27B 118.5 . . ? C29B C28B C33B 115.0(2) . . ? C29B C28B B1B 125.1(2) . . ? C33B C28B B1B 119.8(2) . . ? C30B C29B C28B 122.7(2) . . ? C30B C29B H29B 118.7 . . ? C28B C29B H29B 118.7 . . ? C31B C30B C29B 120.2(2) . . ? C31B C30B H30B 119.9 . . ? C29B C30B H30B 119.9 . . ? C32B C31B C30B 118.9(2) . . ? C32B C31B H31B 120.5 . . ? C30B C31B H31B 120.5 . . ? C31B C32B C33B 120.2(3) . . ? C31B C32B H32B 119.9 . . ? C33B C32B H32B 119.9 . . ? C32B C33B C28B 122.9(2) . . ? C32B C33B H33B 118.5 . . ? C28B C33B H33B 118.5 . . ? C39B C34B C35B 114.9(2) . . ? C39B C34B B1B 125.4(2) . . ? C35B C34B B1B 119.5(2) . . ? C36B C35B C34B 123.3(3) . . ? C36B C35B H35B 118.4 . . ? C34B C35B H35B 118.4 . . ? C37B C36B C35B 120.1(3) . . ? C37B C36B H36B 119.9 . . ? C35B C36B H36B 119.9 . . ? C38B C37B C36B 118.7(2) . . ? C38B C37B H37B 120.7 . . ? C36B C37B H37B 120.7 . . ? C37B C38B C39B 120.5(3) . . ? C37B C38B H38B 119.8 . . ? C39B C38B H38B 119.8 . . ? C38B C39B C34B 122.5(3) . . ? C38B C39B H39B 118.8 . . ? C34B C39B H39B 118.8 . . ? data_jul2105 _database_code_depnum_ccdc_archive 'CCDC 617261' _audit_creation_date 2005-07-26T10:51:27-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C17 H21 Al N6, C24 H20 B, C4 H8 O' _chemical_formula_sum 'C45 H60 Al B N6 O' _chemical_formula_weight 738.78 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8106(2) _cell_length_b 19.9865(4) _cell_length_c 21.7023(3) _cell_angle_alpha 66.307(1) _cell_angle_beta 87.632(1) _cell_angle_gamma 74.326(1) _cell_volume 4122.18(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 32810 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.19 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.953058E-1 _diffrn_orient_matrix_ub_12 -0.172724E-1 _diffrn_orient_matrix_ub_13 0.110623E-1 _diffrn_orient_matrix_ub_21 -0.130727E-1 _diffrn_orient_matrix_ub_22 -0.290071E-1 _diffrn_orient_matrix_ub_23 0.483434E-1 _diffrn_orient_matrix_ub_31 0.54984E-2 _diffrn_orient_matrix_ub_32 -0.457613E-1 _diffrn_orient_matrix_ub_33 -0.93499E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_unetI/netI 0.0526 _diffrn_reflns_number 55294 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 25.97 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 16005 _reflns_number_gt 11181 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The THF solvate molecules were included with SADI restraints. 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^)+(0.0762P)^2^+3.3637P] 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_number_reflns 16005 _refine_ls_number_parameters 973 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0949 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.167 _refine_ls_wR_factor_gt 0.1455 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.963 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.703 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.046 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al Al 0.86558(9) 0.84455(4) 0.04071(4) 0.0421(2) Uani 1 1 d . . . B B 0.4513(2) 0.69437(14) 0.29220(12) 0.0250(5) Uani 1 1 d . . . N1 N 0.80526(18) 0.83596(11) 0.18942(10) 0.0306(4) Uani 1 1 d . . . N2 N 0.96615(18) 0.83627(11) 0.11493(9) 0.0304(4) Uani 1 1 d . . . N3 N 0.96976(18) 0.88795(11) 0.19446(9) 0.0293(4) Uani 1 1 d . . . N4 N 0.85968(18) 0.71019(10) 0.18558(9) 0.0286(4) Uani 1 1 d . . . N5 N 0.8542(2) 0.74229(12) 0.06957(10) 0.0389(5) Uani 1 1 d . . . N6 N 0.9346(2) 0.61563(11) 0.14742(10) 0.0386(5) Uani 1 1 d . . . C1 C 0.9156(2) 0.85367(12) 0.16535(11) 0.0263(5) Uani 1 1 d . . . C2 C 1.0999(2) 0.84071(14) 0.10505(12) 0.0374(6) Uani 1 1 d . . . H2A H 1.1285 0.8328 0.064 0.045 Uiso 1 1 calc R . . H2B H 1.1577 0.8005 0.1441 0.045 Uiso 1 1 calc R . . C3 C 1.1060(3) 0.91803(14) 0.09799(12) 0.0386(6) Uani 1 1 d . . . H3A H 1.1936 0.9237 0.0877 0.046 Uiso 1 1 calc R . . H3B H 1.044 0.9585 0.0609 0.046 Uiso 1 1 calc R . . C4 C 1.0725(2) 0.92387(15) 0.16399(12) 0.0373(6) Uani 1 1 d . . . H4A H 1.1505 0.8991 0.1958 0.045 Uiso 1 1 calc R . . H4B H 1.0442 0.9782 0.1565 0.045 Uiso 1 1 calc R . . C5 C 0.9322(3) 0.89628(16) 0.25707(13) 0.0395(6) Uani 1 1 d . . . H5A H 0.9038 0.9511 0.2478 0.047 Uiso 1 1 calc R . . H5B H 1.0083 0.8723 0.2901 0.047 Uiso 1 1 calc R . . C6 C 0.8252(3) 0.86085(16) 0.28768(13) 0.0435(6) Uani 1 1 d . . . H6A H 0.8618 0.8059 0.3156 0.052 Uiso 1 1 calc R . . H6B H 0.7791 0.885 0.3171 0.052 Uiso 1 1 calc R . . C7 C 0.7335(2) 0.87190(15) 0.23218(13) 0.0374(6) Uani 1 1 d . . . H7A H 0.6632 0.8485 0.2515 0.045 Uiso 1 1 calc R . . H7B H 0.6948 0.9268 0.205 0.045 Uiso 1 1 calc R . . C8 C 0.7600(2) 0.77743(13) 0.17998(12) 0.0316(5) Uani 1 1 d . . . H8A H 0.6976 0.7621 0.2139 0.038 Uiso 1 1 calc R . . H8B H 0.7134 0.8002 0.1348 0.038 Uiso 1 1 calc R . . C9 C 0.8845(2) 0.68997(13) 0.13256(11) 0.0313(5) Uani 1 1 d . . . C10 C 0.9336(2) 0.66698(14) 0.25148(11) 0.0347(5) Uani 1 1 d . . . H10A H 0.8733 0.6613 0.2876 0.042 Uiso 1 1 calc R . . H10B H 0.9907 0.6958 0.257 0.042 Uiso 1 1 calc R . . C11 C 1.0144(2) 0.58906(14) 0.25914(13) 0.0385(6) Uani 1 1 d . . . H11A H 1.1006 0.5917 0.243 0.046 Uiso 1 1 calc R . . H11B H 1.0255 0.5532 0.3073 0.046 Uiso 1 1 calc R . . C12 C 0.9471(3) 0.56177(14) 0.21826(13) 0.0398(6) Uani 1 1 d . . . H12A H 0.9976 0.5104 0.223 0.048 Uiso 1 1 calc R . . H12B H 0.8608 0.559 0.2344 0.048 Uiso 1 1 calc R . . C13 C 0.9944(3) 0.58656(17) 0.09790(15) 0.0511(7) Uani 1 1 d . . . H13A H 0.9473 0.5528 0.0926 0.061 Uiso 1 1 calc R . . H13B H 1.0846 0.5562 0.1144 0.061 Uiso 1 1 calc R . . C14 C 0.9927(3) 0.65087(18) 0.03076(14) 0.0561(8) Uani 1 1 d . . . H14A H 1.004 0.632 -0.0055 0.067 Uiso 1 1 calc R . . H14B H 1.0638 0.6732 0.031 0.067 Uiso 1 1 calc R . . C15 C 0.8646(3) 0.71012(17) 0.01833(13) 0.0502(8) Uani 1 1 d . . . H15A H 0.8576 0.7511 -0.0274 0.06 Uiso 1 1 calc R . . H15B H 0.7935 0.6867 0.0211 0.06 Uiso 1 1 calc R . . C16 C 0.7033(3) 0.92477(17) 0.02746(17) 0.0679(10) Uani 1 1 d . . . H16A H 0.6498 0.93 -0.0104 0.102 Uiso 1 1 calc R . . H16B H 0.7225 0.9731 0.0177 0.102 Uiso 1 1 calc R . . H16C H 0.6571 0.9111 0.0685 0.102 Uiso 1 1 calc R . . C17 C 0.9645(4) 0.86484(19) -0.03958(14) 0.0736(11) Uani 1 1 d . . . H17A H 0.9124 0.869 -0.0775 0.11 Uiso 1 1 calc R . . H17B H 1.0435 0.8231 -0.0303 0.11 Uiso 1 1 calc R . . H17C H 0.9869 0.9126 -0.051 0.11 Uiso 1 1 calc R . . C18 C 0.3485(2) 0.66455(12) 0.34821(10) 0.0251(5) Uani 1 1 d . . . C19 C 0.2155(2) 0.69915(14) 0.33628(12) 0.0334(5) Uani 1 1 d . . . H19 H 0.1841 0.7428 0.2956 0.04 Uiso 1 1 calc R . . C20 C 0.1276(2) 0.67231(15) 0.38149(12) 0.0390(6) Uani 1 1 d . . . H20 H 0.038 0.697 0.3709 0.047 Uiso 1 1 calc R . . C21 C 0.1699(2) 0.60980(15) 0.44197(12) 0.0368(6) Uani 1 1 d . . . H21 H 0.1102 0.5915 0.4732 0.044 Uiso 1 1 calc R . . C22 C 0.3000(2) 0.57464(14) 0.45604(11) 0.0326(5) Uani 1 1 d . . . H22 H 0.3308 0.5318 0.4974 0.039 Uiso 1 1 calc R . . C23 C 0.3864(2) 0.60167(13) 0.41002(11) 0.0275(5) Uani 1 1 d . . . H23 H 0.4756 0.5763 0.421 0.033 Uiso 1 1 calc R . . C24 C 0.4140(2) 0.78810(12) 0.25907(11) 0.0253(5) Uani 1 1 d . . . C25 C 0.3728(2) 0.82979(13) 0.29862(12) 0.0318(5) Uani 1 1 d . . . H25 H 0.3584 0.8033 0.3444 0.038 Uiso 1 1 calc R . . C26 C 0.3521(2) 0.90832(14) 0.27366(13) 0.0379(6) Uani 1 1 d . . . H26 H 0.3239 0.9342 0.3023 0.046 Uiso 1 1 calc R . . C27 C 0.3727(2) 0.94838(14) 0.20744(13) 0.0390(6) Uani 1 1 d . . . H27 H 0.3604 1.0017 0.1903 0.047 Uiso 1 1 calc R . . C28 C 0.4112(2) 0.91008(13) 0.16626(12) 0.0351(6) Uani 1 1 d . . . H28 H 0.4248 0.9373 0.1204 0.042 Uiso 1 1 calc R . . C29 C 0.4304(2) 0.83159(13) 0.19159(11) 0.0293(5) Uani 1 1 d . . . H29 H 0.4555 0.8066 0.1621 0.035 Uiso 1 1 calc R . . C30 C 0.4475(2) 0.66532(12) 0.23133(11) 0.0266(5) Uani 1 1 d . . . C31 C 0.3359(2) 0.65536(13) 0.20992(11) 0.0316(5) Uani 1 1 d . . . H31 H 0.2618 0.6605 0.2345 0.038 Uiso 1 1 calc R . . C32 C 0.3285(3) 0.63829(14) 0.15424(13) 0.0402(6) Uani 1 1 d . . . H32 H 0.2501 0.6327 0.1415 0.048 Uiso 1 1 calc R . . C33 C 0.4339(3) 0.62939(15) 0.11746(12) 0.0416(6) Uani 1 1 d . . . H33 H 0.4291 0.6178 0.0794 0.05 Uiso 1 1 calc R . . C34 C 0.5473(3) 0.63769(15) 0.13727(12) 0.0404(6) Uani 1 1 d . . . H34 H 0.6215 0.6311 0.113 0.048 Uiso 1 1 calc R . . C35 C 0.5522(2) 0.65550(13) 0.19239(11) 0.0317(5) Uani 1 1 d . . . H35 H 0.6308 0.6614 0.2045 0.038 Uiso 1 1 calc R . . C36 C 0.5957(2) 0.65987(12) 0.33313(10) 0.0255(5) Uani 1 1 d . . . C37 C 0.6426(2) 0.69747(14) 0.36543(11) 0.0301(5) Uani 1 1 d . . . H37 H 0.5953 0.7478 0.3583 0.036 Uiso 1 1 calc R . . C38 C 0.7561(2) 0.66367(15) 0.40756(11) 0.0359(6) Uani 1 1 d . . . H38 H 0.7843 0.6911 0.4285 0.043 Uiso 1 1 calc R . . C39 C 0.8279(2) 0.59055(15) 0.41904(12) 0.0365(6) Uani 1 1 d . . . H39 H 0.9047 0.5672 0.4481 0.044 Uiso 1 1 calc R . . C40 C 0.7857(2) 0.55206(14) 0.38745(12) 0.0348(6) Uani 1 1 d . . . H40 H 0.8342 0.5019 0.3946 0.042 Uiso 1 1 calc R . . C41 C 0.6727(2) 0.58630(13) 0.34531(11) 0.0297(5) Uani 1 1 d . . . H41 H 0.6466 0.5587 0.3239 0.036 Uiso 1 1 calc R . . Al1B Al 0.57776(7) 0.17199(4) 0.45651(4) 0.03280(18) Uani 1 1 d . A 1 B1B B 0.0197(2) 0.30282(15) 0.20580(13) 0.0276(5) Uani 1 1 d . B 1 N1B N 0.6401(2) 0.16844(12) 0.30880(10) 0.0360(5) Uani 1 1 d . A 1 N2B N 0.48308(18) 0.17086(11) 0.38472(9) 0.0308(4) Uani 1 1 d . A 1 N3B N 0.4851(2) 0.10547(12) 0.31592(11) 0.0398(5) Uani 1 1 d . A 1 N4B N 0.58933(19) 0.29731(10) 0.30576(9) 0.0307(4) Uani 1 1 d . A 1 N5B N 0.58648(19) 0.27545(11) 0.42014(10) 0.0323(4) Uani 1 1 d . A 1 N6B N 0.5182(2) 0.39905(11) 0.33555(10) 0.0365(5) Uani 1 1 d . A 1 C1B C 0.5352(2) 0.14769(13) 0.33760(11) 0.0308(5) Uani 1 1 d . A 1 C2B C 0.7148(3) 0.13580(18) 0.26433(16) 0.0532(8) Uani 1 1 d . A 1 H2B1 H 0.8078 0.1213 0.278 0.064 Uiso 1 1 calc R A 1 H2B2 H 0.6997 0.1748 0.2173 0.064 Uiso 1 1 calc R A 1 C3B C 0.6796(3) 0.06817(19) 0.26692(18) 0.0624(9) Uani 1 1 d . A 1 H3B1 H 0.715 0.0244 0.3101 0.075 Uiso 1 1 calc R A 1 H3B2 H 0.7165 0.0547 0.2296 0.075 Uiso 1 1 calc R A 1 C4B C 0.5372(3) 0.08514(18) 0.26086(15) 0.0517(7) Uani 1 1 d . A 1 H4B1 H 0.5019 0.1277 0.217 0.062 Uiso 1 1 calc R A 1 H4B2 H 0.5126 0.04 0.263 0.062 Uiso 1 1 calc R A 1 C5B C 0.3831(3) 0.07069(15) 0.34948(14) 0.0446(7) Uani 1 1 d . A 1 H5B1 H 0.4135 0.0151 0.3625 0.053 Uiso 1 1 calc R A 1 H5B2 H 0.3063 0.0912 0.3173 0.053 Uiso 1 1 calc R A 1 C6B C 0.3456(3) 0.08567(15) 0.41141(13) 0.0432(6) Uani 1 1 d . A 1 H6B1 H 0.4064 0.0487 0.4506 0.052 Uiso 1 1 calc R A 1 H6B2 H 0.2578 0.0806 0.4221 0.052 Uiso 1 1 calc R A 1 C7B C 0.3498(2) 0.16555(14) 0.39643(13) 0.0371(6) Uani 1 1 d . A 1 H7B1 H 0.2918 0.202 0.3559 0.045 Uiso 1 1 calc R A 1 H7B2 H 0.3199 0.1787 0.4349 0.045 Uiso 1 1 calc R A 1 C8B C 0.6862(2) 0.22743(14) 0.31719(13) 0.0351(6) Uani 1 1 d . A 1 H8B1 H 0.7265 0.2065 0.3636 0.042 Uiso 1 1 calc R A 1 H8B2 H 0.754 0.2389 0.2857 0.042 Uiso 1 1 calc R A 1 C9B C 0.5629(2) 0.32358(13) 0.35552(12) 0.0307(5) Uani 1 1 d . A 1 C10B C 0.5282(3) 0.33957(14) 0.23664(12) 0.0400(6) Uani 1 1 d . A 1 H10C H 0.4716 0.3119 0.2285 0.048 Uiso 1 1 calc R A 1 H10D H 0.5958 0.3419 0.2043 0.048 Uiso 1 1 calc R A 1 C11B C 0.4496(3) 0.41947(14) 0.22389(13) 0.0409(6) Uani 1 1 d . A 1 H11C H 0.4435 0.4526 0.1752 0.049 Uiso 1 1 calc R A 1 H11D H 0.3613 0.4195 0.238 0.049 Uiso 1 1 calc R A 1 C12B C 0.5151(3) 0.44855(14) 0.26394(13) 0.0413(6) Uani 1 1 d . A 1 H12C H 0.6038 0.4478 0.2503 0.05 Uiso 1 1 calc R A 1 H12D H 0.467 0.5015 0.2556 0.05 Uiso 1 1 calc R A 1 C13B C 0.4563(3) 0.43494(15) 0.38031(13) 0.0432(6) Uani 1 1 d . A 1 H13C H 0.3674 0.4656 0.3615 0.052 Uiso 1 1 calc R A 1 H13D H 0.5044 0.4696 0.3829 0.052 Uiso 1 1 calc R A 1 C14B C 0.4527(3) 0.37594(15) 0.45023(13) 0.0409(6) Uani 1 1 d . A 1 H14C H 0.3786 0.3552 0.4518 0.049 Uiso 1 1 calc R A 1 H14D H 0.4429 0.3992 0.4834 0.049 Uiso 1 1 calc R A 1 C15B C 0.5774(3) 0.31287(15) 0.46730(13) 0.0393(6) Uani 1 1 d . A 1 H15C H 0.6515 0.3341 0.4637 0.047 Uiso 1 1 calc R A 1 H15D H 0.5798 0.2752 0.5142 0.047 Uiso 1 1 calc R A 1 C16B C 0.4734(3) 0.15691(16) 0.53540(13) 0.0490(7) Uani 1 1 d . A 1 H16D H 0.5216 0.1576 0.5723 0.073 Uiso 1 1 calc R A 1 H16E H 0.4543 0.1078 0.55 0.073 Uiso 1 1 calc R A 1 H16F H 0.3927 0.1978 0.523 0.073 Uiso 1 1 calc R A 1 C17B C 0.7442(3) 0.09313(15) 0.47589(15) 0.0488(7) Uani 1 1 d . A 1 H17D H 0.7942 0.093 0.5126 0.073 Uiso 1 1 calc R A 1 H17E H 0.7923 0.104 0.4354 0.073 Uiso 1 1 calc R A 1 H17F H 0.7287 0.0432 0.4893 0.073 Uiso 1 1 calc R A 1 C18B C 0.0236(2) 0.33716(12) 0.26274(11) 0.0278(5) Uani 1 1 d . B 1 C19B C -0.0828(2) 0.35244(13) 0.29939(12) 0.0341(5) Uani 1 1 d . B 1 H19B H -0.162 0.3464 0.2881 0.041 Uiso 1 1 calc R B 1 C20B C -0.0778(3) 0.37582(14) 0.35117(12) 0.0402(6) Uani 1 1 d . B 1 H20B H -0.1527 0.3857 0.3742 0.048 Uiso 1 1 calc R B 1 C21B C 0.0360(3) 0.38471(14) 0.36934(12) 0.0404(6) Uani 1 1 d . B 1 H21B H 0.0405 0.4001 0.4051 0.048 Uiso 1 1 calc R B 1 C22B C 0.1428(3) 0.37077(14) 0.33453(12) 0.0391(6) Uani 1 1 d . B 1 H22B H 0.2216 0.3767 0.3463 0.047 Uiso 1 1 calc R B 1 C23B C 0.1358(2) 0.34803(13) 0.28223(11) 0.0323(5) Uani 1 1 d . B 1 H23B H 0.2106 0.3395 0.2588 0.039 Uiso 1 1 calc R B 1 C24B C 0.1327(2) 0.32441(13) 0.15386(11) 0.0296(5) Uani 1 1 d . B 1 C25B C 0.1116(2) 0.39522(14) 0.09921(12) 0.0369(6) Uani 1 1 d . B 1 H25B H 0.0277 0.4296 0.0902 0.044 Uiso 1 1 calc R B 1 C26B C 0.2067(3) 0.41780(17) 0.05743(14) 0.0466(7) Uani 1 1 d . B 1 H26B H 0.1879 0.4669 0.0215 0.056 Uiso 1 1 calc R B 1 C27B C 0.3286(3) 0.36859(18) 0.06839(13) 0.0465(7) Uani 1 1 d . B 1 H27B H 0.3941 0.3831 0.0397 0.056 Uiso 1 1 calc R B 1 C28B C 0.3544(3) 0.29829(18) 0.12136(14) 0.0474(7) Uani 1 1 d . B 1 H28B H 0.4383 0.2641 0.1294 0.057 Uiso 1 1 calc R B 1 C29B C 0.2582(2) 0.27705(16) 0.16327(12) 0.0392(6) Uani 1 1 d . B 1 H29B H 0.2787 0.2283 0.1998 0.047 Uiso 1 1 calc R B 1 C30B C -0.1202(2) 0.34172(13) 0.16028(11) 0.0286(5) Uani 1 1 d . B 1 C31B C -0.1918(2) 0.41728(13) 0.14562(12) 0.0342(5) Uani 1 1 d . B 1 H31B H -0.1636 0.4445 0.1668 0.041 Uiso 1 1 calc R B 1 C32B C -0.3019(2) 0.45374(15) 0.10149(13) 0.0407(6) Uani 1 1 d . B 1 H32B H -0.3467 0.505 0.0928 0.049 Uiso 1 1 calc R B 1 C33B C -0.3464(2) 0.41588(16) 0.07027(13) 0.0444(7) Uani 1 1 d . B 1 H33B H -0.4212 0.4408 0.0397 0.053 Uiso 1 1 calc R B 1 C34B C -0.2812(2) 0.34164(16) 0.08394(12) 0.0425(6) Uani 1 1 d . B 1 H34B H -0.3118 0.3148 0.0631 0.051 Uiso 1 1 calc R B 1 C35B C -0.1702(2) 0.30517(14) 0.12819(12) 0.0342(5) Uani 1 1 d . B 1 H35B H -0.1271 0.2537 0.1368 0.041 Uiso 1 1 calc R B 1 C36B C 0.0439(2) 0.21009(13) 0.24417(11) 0.0281(5) Uani 1 1 d . B 1 C37B C 0.0783(2) 0.16297(14) 0.20909(12) 0.0350(5) Uani 1 1 d . B 1 H37B H 0.0942 0.1852 0.1629 0.042 Uiso 1 1 calc R B 1 C38B C 0.0902(2) 0.08551(14) 0.23852(14) 0.0409(6) Uani 1 1 d . B 1 H38B H 0.1128 0.0562 0.2124 0.049 Uiso 1 1 calc R B 1 C39B C 0.0690(2) 0.05102(15) 0.30594(14) 0.0431(6) Uani 1 1 d . B 1 H39B H 0.0763 -0.0019 0.3265 0.052 Uiso 1 1 calc R B 1 C40B C 0.0371(2) 0.09488(14) 0.34295(13) 0.0380(6) Uani 1 1 d . B 1 H40B H 0.023 0.0719 0.3894 0.046 Uiso 1 1 calc R B 1 C41B C 0.0255(2) 0.17241(13) 0.31246(12) 0.0312(5) Uani 1 1 d . B 1 H41B H 0.0041 0.2011 0.3391 0.037 Uiso 1 1 calc R B 1 O1S O 0.9715(3) 0.89008(14) 0.40247(11) 0.0765(7) Uani 1 1 d D C 1 C1S C 1.0906(3) 0.8351(2) 0.42812(15) 0.0600(8) Uani 1 1 d D C 1 H1S1 H 1.1566 0.8594 0.4321 0.072 Uiso 1 1 calc R C 1 H1S2 H 1.1196 0.8091 0.3976 0.072 Uiso 1 1 calc R C 1 C2S C 1.0718(3) 0.77897(18) 0.49627(15) 0.0560(8) Uani 1 1 d D C 1 H2S1 H 1.0892 0.7274 0.497 0.067 Uiso 1 1 calc R C 1 H2S2 H 1.1291 0.777 0.5317 0.067 Uiso 1 1 calc R C 1 C3S C 0.9337(4) 0.8086(2) 0.50625(19) 0.0995(16) Uani 1 1 d D C 1 H3S1 H 0.8814 0.778 0.4995 0.119 Uiso 1 1 calc R C 1 H3S2 H 0.9242 0.8072 0.5523 0.119 Uiso 1 1 calc R C 1 C4S C 0.8941(4) 0.8854(2) 0.45658(19) 0.0883(13) Uani 1 1 d D C 1 H4S1 H 0.8023 0.8991 0.4411 0.106 Uiso 1 1 calc R C 1 H4S2 H 0.9047 0.9208 0.476 0.106 Uiso 1 1 calc R C 1 O2S O 0.6037(4) 0.0912(2) 0.11639(16) 0.1368(14) Uani 1 1 d D D 1 C5S C 0.4856(5) 0.1194(3) 0.07902(19) 0.119(2) Uani 1 1 d D D 1 H5S2 H 0.4166 0.1384 0.1042 0.143 Uiso 1 1 calc R D 1 H5S1 H 0.4644 0.0787 0.0702 0.143 Uiso 1 1 calc R D 1 C6S C 0.4955(5) 0.1819(3) 0.0147(2) 0.1097(17) Uani 1 1 d D D 1 H6S1 H 0.4458 0.1827 -0.023 0.132 Uiso 1 1 calc R D 1 H6S2 H 0.4648 0.2318 0.0177 0.132 Uiso 1 1 calc R D 1 C7S C 0.6277(6) 0.1639(4) 0.0068(3) 0.186(4) Uani 1 1 d D D 1 H8S2 H 0.6544 0.2112 -0.0149 0.224 Uiso 1 1 calc R D 1 H8S1 H 0.6466 0.1362 -0.0229 0.224 Uiso 1 1 calc R D 1 C8S C 0.7021(5) 0.1160(4) 0.0731(3) 0.146(2) Uani 1 1 d D D 1 H7S2 H 0.7695 0.0723 0.0712 0.175 Uiso 1 1 calc R D 1 H7S1 H 0.7427 0.146 0.0886 0.175 Uiso 1 1 calc R D 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al 0.0684(6) 0.0340(4) 0.0265(4) -0.0072(3) -0.0027(4) -0.0252(4) B 0.0255(13) 0.0224(13) 0.0269(13) -0.0089(10) 0.0027(10) -0.0082(10) N1 0.0292(10) 0.0325(11) 0.0364(11) -0.0182(9) 0.0057(8) -0.0123(9) N2 0.0354(11) 0.0296(11) 0.0290(10) -0.0112(8) 0.0060(8) -0.0154(9) N3 0.0325(11) 0.0306(11) 0.0271(10) -0.0119(8) -0.0002(8) -0.0119(9) N4 0.0336(11) 0.0277(10) 0.0266(10) -0.0107(8) 0.0041(8) -0.0126(8) N5 0.0611(14) 0.0365(12) 0.0281(11) -0.0142(9) 0.0020(9) -0.0257(11) N6 0.0533(14) 0.0311(12) 0.0372(12) -0.0171(9) 0.0116(10) -0.0169(10) C1 0.0296(12) 0.0195(11) 0.0264(11) -0.0062(9) -0.0022(9) -0.0055(9) C2 0.0359(14) 0.0400(15) 0.0342(13) -0.0121(11) 0.0093(11) -0.0131(11) C3 0.0404(15) 0.0405(15) 0.0334(13) -0.0071(11) 0.0020(11) -0.0208(12) C4 0.0419(15) 0.0362(14) 0.0361(13) -0.0098(11) -0.0021(11) -0.0215(12) C5 0.0411(15) 0.0459(16) 0.0402(14) -0.0263(12) 0.0019(11) -0.0117(12) C6 0.0489(16) 0.0459(16) 0.0403(15) -0.0241(13) 0.0068(12) -0.0104(13) C7 0.0315(13) 0.0392(14) 0.0478(15) -0.0249(12) 0.0089(11) -0.0092(11) C8 0.0305(13) 0.0301(13) 0.0358(13) -0.0133(10) 0.0007(10) -0.0108(10) C9 0.0391(14) 0.0311(13) 0.0298(12) -0.0122(10) 0.0067(10) -0.0201(11) C10 0.0415(14) 0.0349(14) 0.0252(12) -0.0080(10) 0.0032(10) -0.0133(11) C11 0.0373(14) 0.0335(14) 0.0391(14) -0.0085(11) 0.0052(11) -0.0112(11) C12 0.0464(15) 0.0266(13) 0.0432(14) -0.0099(11) 0.0089(12) -0.0130(11) C13 0.0652(19) 0.0487(17) 0.0578(18) -0.0360(15) 0.0201(15) -0.0242(15) C14 0.081(2) 0.069(2) 0.0454(16) -0.0388(16) 0.0267(15) -0.0424(19) C15 0.084(2) 0.0527(18) 0.0312(14) -0.0219(13) 0.0073(14) -0.0380(17) C16 0.082(2) 0.0428(18) 0.061(2) -0.0019(15) -0.0312(17) -0.0148(17) C17 0.143(4) 0.062(2) 0.0321(15) -0.0160(15) 0.0216(18) -0.059(2) C18 0.0265(12) 0.0249(12) 0.0262(11) -0.0118(9) 0.0013(9) -0.0084(9) C19 0.0290(13) 0.0347(13) 0.0292(12) -0.0078(10) 0.0009(10) -0.0056(10) C20 0.0231(12) 0.0521(16) 0.0380(14) -0.0162(12) 0.0025(10) -0.0081(11) C21 0.0320(14) 0.0475(16) 0.0335(13) -0.0142(12) 0.0105(10) -0.0196(12) C22 0.0360(14) 0.0324(13) 0.0269(12) -0.0079(10) 0.0036(10) -0.0121(11) C23 0.0260(12) 0.0285(12) 0.0287(12) -0.0126(10) 0.0032(9) -0.0072(10) C24 0.0203(11) 0.0246(12) 0.0297(12) -0.0092(9) -0.0002(9) -0.0064(9) C25 0.0317(13) 0.0313(13) 0.0316(12) -0.0131(10) -0.0013(10) -0.0063(10) C26 0.0356(14) 0.0310(14) 0.0489(15) -0.0207(12) -0.0034(11) -0.0038(11) C27 0.0333(14) 0.0229(12) 0.0560(16) -0.0107(12) -0.0045(12) -0.0072(10) C28 0.0305(13) 0.0296(13) 0.0367(13) -0.0035(11) -0.0008(10) -0.0100(10) C29 0.0255(12) 0.0298(12) 0.0308(12) -0.0103(10) 0.0007(9) -0.0079(10) C30 0.0309(12) 0.0186(11) 0.0258(11) -0.0043(9) 0.0007(9) -0.0070(9) C31 0.0315(13) 0.0313(13) 0.0311(12) -0.0118(10) -0.0004(10) -0.0082(10) C32 0.0426(15) 0.0390(15) 0.0405(14) -0.0177(12) -0.0068(12) -0.0098(12) C33 0.0586(18) 0.0388(15) 0.0290(13) -0.0168(11) -0.0004(12) -0.0109(13) C34 0.0486(16) 0.0394(15) 0.0374(14) -0.0189(12) 0.0140(12) -0.0153(12) C35 0.0354(13) 0.0295(13) 0.0351(13) -0.0148(10) 0.0071(10) -0.0147(10) C36 0.0231(11) 0.0282(12) 0.0240(11) -0.0075(9) 0.0068(9) -0.0110(9) C37 0.0271(12) 0.0340(13) 0.0293(12) -0.0123(10) 0.0052(9) -0.0098(10) C38 0.0335(13) 0.0485(16) 0.0288(12) -0.0152(11) 0.0036(10) -0.0173(12) C39 0.0240(12) 0.0441(15) 0.0300(12) -0.0035(11) -0.0005(10) -0.0093(11) C40 0.0261(12) 0.0319(13) 0.0350(13) -0.0038(11) 0.0063(10) -0.0062(10) C41 0.0268(12) 0.0295(13) 0.0321(12) -0.0102(10) 0.0061(9) -0.0108(10) Al1B 0.0387(4) 0.0294(4) 0.0317(4) -0.0117(3) 0.0010(3) -0.0124(3) B1B 0.0278(14) 0.0276(14) 0.0270(13) -0.0104(11) 0.0027(10) -0.0081(11) N1B 0.0378(12) 0.0360(12) 0.0446(12) -0.0258(10) 0.0118(9) -0.0130(9) N2B 0.0302(11) 0.0303(11) 0.0341(11) -0.0137(9) 0.0048(8) -0.0112(9) N3B 0.0467(13) 0.0384(12) 0.0434(12) -0.0223(10) -0.0003(10) -0.0166(10) N4B 0.0353(11) 0.0268(10) 0.0327(10) -0.0135(9) 0.0076(8) -0.0112(9) N5B 0.0380(11) 0.0298(11) 0.0338(11) -0.0160(9) 0.0017(9) -0.0116(9) N6B 0.0478(13) 0.0273(11) 0.0361(11) -0.0145(9) 0.0101(9) -0.0116(9) C1B 0.0336(13) 0.0243(12) 0.0337(12) -0.0119(10) -0.0033(10) -0.0056(10) C2B 0.0470(17) 0.063(2) 0.072(2) -0.0502(17) 0.0218(15) -0.0170(15) C3B 0.060(2) 0.065(2) 0.073(2) -0.0488(18) -0.0031(16) -0.0014(16) C4B 0.0542(18) 0.0598(19) 0.0593(18) -0.0407(16) 0.0012(14) -0.0179(15) C5B 0.0465(16) 0.0333(14) 0.0535(16) -0.0130(12) -0.0090(13) -0.0158(12) C6B 0.0410(15) 0.0416(15) 0.0419(15) -0.0051(12) -0.0040(12) -0.0209(12) C7B 0.0304(13) 0.0397(15) 0.0388(14) -0.0126(11) 0.0013(10) -0.0110(11) C8B 0.0347(13) 0.0354(14) 0.0424(14) -0.0212(11) 0.0120(11) -0.0141(11) C9B 0.0308(13) 0.0305(13) 0.0372(13) -0.0169(11) 0.0077(10) -0.0142(10) C10B 0.0535(16) 0.0385(15) 0.0311(13) -0.0152(11) 0.0079(11) -0.0169(13) C11B 0.0454(15) 0.0379(15) 0.0342(13) -0.0089(11) 0.0074(11) -0.0129(12) C12B 0.0503(16) 0.0286(13) 0.0416(14) -0.0094(11) 0.0089(12) -0.0140(12) C13B 0.0503(16) 0.0344(14) 0.0521(16) -0.0254(13) 0.0121(13) -0.0120(12) C14B 0.0485(16) 0.0464(16) 0.0403(14) -0.0278(13) 0.0099(12) -0.0175(13) C15B 0.0502(16) 0.0412(15) 0.0375(14) -0.0235(12) 0.0026(11) -0.0183(13) C16B 0.0651(19) 0.0470(17) 0.0356(14) -0.0130(13) 0.0031(13) -0.0224(15) C17B 0.0483(17) 0.0366(15) 0.0535(17) -0.0105(13) -0.0072(13) -0.0099(13) C18B 0.0318(12) 0.0211(11) 0.0280(12) -0.0078(9) 0.0022(9) -0.0070(10) C19B 0.0393(14) 0.0291(13) 0.0356(13) -0.0133(11) 0.0070(11) -0.0124(11) C20B 0.0498(16) 0.0347(14) 0.0386(14) -0.0182(12) 0.0157(12) -0.0124(12) C21B 0.0568(17) 0.0364(14) 0.0305(13) -0.0173(11) 0.0021(12) -0.0110(13) C22B 0.0446(15) 0.0349(14) 0.0373(14) -0.0146(11) -0.0064(11) -0.0088(12) C23B 0.0341(13) 0.0320(13) 0.0321(12) -0.0143(10) 0.0031(10) -0.0091(11) C24B 0.0311(13) 0.0374(14) 0.0284(12) -0.0184(10) 0.0038(9) -0.0145(11) C25B 0.0391(14) 0.0370(14) 0.0404(14) -0.0187(12) 0.0109(11) -0.0163(12) C26B 0.0551(18) 0.0476(17) 0.0457(16) -0.0194(13) 0.0165(13) -0.0288(14) C27B 0.0439(16) 0.070(2) 0.0412(15) -0.0274(15) 0.0165(12) -0.0350(15) C28B 0.0292(14) 0.073(2) 0.0453(16) -0.0288(15) 0.0070(12) -0.0147(14) C29B 0.0331(14) 0.0491(16) 0.0332(13) -0.0153(12) 0.0036(10) -0.0105(12) C30B 0.0277(12) 0.0307(13) 0.0259(11) -0.0074(10) 0.0072(9) -0.0129(10) C31B 0.0310(13) 0.0309(13) 0.0374(13) -0.0091(11) 0.0046(10) -0.0113(11) C32B 0.0326(14) 0.0329(14) 0.0415(14) -0.0016(11) 0.0050(11) -0.0068(11) C33B 0.0312(14) 0.0480(17) 0.0379(14) -0.0021(12) -0.0039(11) -0.0089(12) C34B 0.0393(15) 0.0552(18) 0.0351(14) -0.0158(13) -0.0004(11) -0.0196(13) C35B 0.0315(13) 0.0369(14) 0.0318(12) -0.0115(11) 0.0030(10) -0.0095(11) C36B 0.0243(12) 0.0291(12) 0.0311(12) -0.0128(10) 0.0000(9) -0.0064(10) C37B 0.0349(13) 0.0331(14) 0.0371(13) -0.0162(11) 0.0000(10) -0.0062(11) C38B 0.0415(15) 0.0313(14) 0.0521(16) -0.0224(12) -0.0032(12) -0.0040(11) C39B 0.0391(15) 0.0259(13) 0.0585(17) -0.0118(12) -0.0033(12) -0.0074(11) C40B 0.0365(14) 0.0326(14) 0.0393(14) -0.0071(11) 0.0035(11) -0.0126(11) C41B 0.0276(12) 0.0307(13) 0.0350(13) -0.0131(10) 0.0016(10) -0.0076(10) O1S 0.0899(19) 0.0720(16) 0.0454(13) -0.0062(11) 0.0122(12) -0.0163(14) C1S 0.062(2) 0.085(2) 0.0455(17) -0.0310(17) 0.0144(15) -0.0341(19) C2S 0.0513(18) 0.063(2) 0.0501(17) -0.0199(15) 0.0061(14) -0.0160(15) C3S 0.061(2) 0.107(3) 0.066(2) 0.010(2) 0.0211(19) 0.003(2) C4S 0.088(3) 0.084(3) 0.068(2) -0.029(2) 0.008(2) 0.013(2) O2S 0.148(3) 0.184(4) 0.0660(19) -0.024(2) 0.002(2) -0.069(3) C5S 0.163(5) 0.169(5) 0.048(2) -0.018(3) -0.004(3) -0.120(4) C6S 0.128(4) 0.128(4) 0.076(3) -0.017(3) 0.014(3) -0.078(4) C7S 0.117(5) 0.182(6) 0.118(5) 0.032(4) 0.062(4) 0.027(4) C8S 0.104(4) 0.197(6) 0.092(4) -0.018(4) 0.023(3) -0.040(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al N2 1.907(2) . ? Al N5 1.920(2) . ? Al C17 1.964(3) . ? Al C16 1.970(4) . ? B C30 1.649(3) . ? B C24 1.650(3) . ? B C18 1.653(3) . ? B C36 1.655(3) . ? N1 C1 1.360(3) . ? N1 C7 1.468(3) . ? N1 C8 1.469(3) . ? N2 C1 1.331(3) . ? N2 C2 1.474(3) . ? N3 C1 1.344(3) . ? N3 C5 1.463(3) . ? N3 C4 1.475(3) . ? N4 C9 1.360(3) . ? N4 C8 1.442(3) . ? N4 C10 1.469(3) . ? N5 C9 1.331(3) . ? N5 C15 1.479(3) . ? N6 C9 1.341(3) . ? N6 C12 1.466(3) . ? N6 C13 1.467(3) . ? C2 C3 1.510(3) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 C4 1.505(3) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 C6 1.510(4) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 C7 1.500(4) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C10 C11 1.511(3) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C11 C12 1.507(4) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C14 1.503(4) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 C15 1.510(4) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 C23 1.400(3) . ? C18 C19 1.401(3) . ? C19 C20 1.389(3) . ? C19 H19 0.95 . ? C20 C21 1.384(3) . ? C20 H20 0.95 . ? C21 C22 1.377(3) . ? C21 H21 0.95 . ? C22 C23 1.386(3) . ? C22 H22 0.95 . ? C23 H23 0.95 . ? C24 C29 1.404(3) . ? C24 C25 1.404(3) . ? C25 C26 1.394(3) . ? C25 H25 0.95 . ? C26 C27 1.379(4) . ? C26 H26 0.95 . ? C27 C28 1.380(4) . ? C27 H27 0.95 . ? C28 C29 1.395(3) . ? C28 H28 0.95 . ? C29 H29 0.95 . ? C30 C31 1.400(3) . ? C30 C35 1.404(3) . ? C31 C32 1.392(3) . ? C31 H31 0.95 . ? C32 C33 1.377(4) . ? C32 H32 0.95 . ? C33 C34 1.388(4) . ? C33 H33 0.95 . ? C34 C35 1.385(3) . ? C34 H34 0.95 . ? C35 H35 0.95 . ? C36 C41 1.404(3) . ? C36 C37 1.405(3) . ? C37 C38 1.395(3) . ? C37 H37 0.95 . ? C38 C39 1.382(4) . ? C38 H38 0.95 . ? C39 C40 1.381(4) . ? C39 H39 0.95 . ? C40 C41 1.391(3) . ? C40 H40 0.95 . ? C41 H41 0.95 . ? Al1B N2B 1.910(2) . ? Al1B N5B 1.922(2) . ? Al1B C17B 1.974(3) . ? Al1B C16B 1.976(3) . ? B1B C18B 1.643(3) . ? B1B C36B 1.647(3) . ? B1B C24B 1.652(3) . ? B1B C30B 1.655(3) . ? N1B C1B 1.354(3) . ? N1B C2B 1.472(3) . ? N1B C8B 1.473(3) . ? N2B C1B 1.330(3) . ? N2B C7B 1.477(3) . ? N3B C1B 1.347(3) . ? N3B C4B 1.456(3) . ? N3B C5B 1.473(3) . ? N4B C9B 1.369(3) . ? N4B C8B 1.436(3) . ? N4B C10B 1.470(3) . ? N5B C9B 1.330(3) . ? N5B C15B 1.478(3) . ? N6B C9B 1.340(3) . ? N6B C12B 1.465(3) . ? N6B C13B 1.467(3) . ? C2B C3B 1.480(4) . ? C2B H2B1 0.99 . ? C2B H2B2 0.99 . ? C3B C4B 1.483(4) . ? C3B H3B1 0.99 . ? C3B H3B2 0.99 . ? C4B H4B1 0.99 . ? C4B H4B2 0.99 . ? C5B C6B 1.508(4) . ? C5B H5B1 0.99 . ? C5B H5B2 0.99 . ? C6B C7B 1.509(4) . ? C6B H6B1 0.99 . ? C6B H6B2 0.99 . ? C7B H7B1 0.99 . ? C7B H7B2 0.99 . ? C8B H8B1 0.99 . ? C8B H8B2 0.99 . ? C10B C11B 1.510(4) . ? C10B H10C 0.99 . ? C10B H10D 0.99 . ? C11B C12B 1.508(4) . ? C11B H11C 0.99 . ? C11B H11D 0.99 . ? C12B H12C 0.99 . ? C12B H12D 0.99 . ? C13B C14B 1.509(4) . ? C13B H13C 0.99 . ? C13B H13D 0.99 . ? C14B C15B 1.514(4) . ? C14B H14C 0.99 . ? C14B H14D 0.99 . ? C15B H15C 0.99 . ? C15B H15D 0.99 . ? C16B H16D 0.98 . ? C16B H16E 0.98 . ? C16B H16F 0.98 . ? C17B H17D 0.98 . ? C17B H17E 0.98 . ? C17B H17F 0.98 . ? C18B C23B 1.399(3) . ? C18B C19B 1.407(3) . ? C19B C20B 1.387(3) . ? C19B H19B 0.95 . ? C20B C21B 1.384(4) . ? C20B H20B 0.95 . ? C21B C22B 1.380(4) . ? C21B H21B 0.95 . ? C22B C23B 1.393(3) . ? C22B H22B 0.95 . ? C23B H23B 0.95 . ? C24B C29B 1.397(3) . ? C24B C25B 1.400(3) . ? C25B C26B 1.389(3) . ? C25B H25B 0.95 . ? C26B C27B 1.378(4) . ? C26B H26B 0.95 . ? C27B C28B 1.375(4) . ? C27B H27B 0.95 . ? C28B C29B 1.393(4) . ? C28B H28B 0.95 . ? C29B H29B 0.95 . ? C30B C35B 1.402(3) . ? C30B C31B 1.408(3) . ? C31B C32B 1.389(3) . ? C31B H31B 0.95 . ? C32B C33B 1.378(4) . ? C32B H32B 0.95 . ? C33B C34B 1.373(4) . ? C33B H33B 0.95 . ? C34B C35B 1.398(3) . ? C34B H34B 0.95 . ? C35B H35B 0.95 . ? C36B C41B 1.401(3) . ? C36B C37B 1.403(3) . ? C37B C38B 1.388(3) . ? C37B H37B 0.95 . ? C38B C39B 1.384(4) . ? C38B H38B 0.95 . ? C39B C40B 1.383(4) . ? C39B H39B 0.95 . ? C40B C41B 1.390(3) . ? C40B H40B 0.95 . ? C41B H41B 0.95 . ? O1S C4S 1.400(4) . ? O1S C1S 1.406(4) . ? C1S C2S 1.501(4) . ? C1S H1S1 0.99 . ? C1S H1S2 0.99 . ? C2S C3S 1.492(4) . ? C2S H2S1 0.99 . ? C2S H2S2 0.99 . ? C3S C4S 1.433(5) . ? C3S H3S1 0.99 . ? C3S H3S2 0.99 . ? C4S H4S1 0.99 . ? C4S H4S2 0.99 . ? O2S C5S 1.391(5) . ? O2S C8S 1.445(5) . ? C5S C6S 1.476(5) . ? C5S H5S2 0.99 . ? C5S H5S1 0.99 . ? C6S C7S 1.397(6) . ? C6S H6S1 0.99 . ? C6S H6S2 0.99 . ? C7S C8S 1.486(7) . ? C7S H8S2 0.99 . ? C7S H8S1 0.99 . ? C8S H7S2 0.99 . ? C8S H7S1 0.99 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Al N5 101.45(9) . . ? N2 Al C17 109.81(13) . . ? N5 Al C17 106.74(12) . . ? N2 Al C16 107.96(12) . . ? N5 Al C16 117.21(13) . . ? C17 Al C16 112.96(16) . . ? C30 B C24 108.92(17) . . ? C30 B C18 110.20(17) . . ? C24 B C18 110.15(18) . . ? C30 B C36 111.58(18) . . ? C24 B C36 108.98(17) . . ? C18 B C36 106.99(17) . . ? C1 N1 C7 118.58(19) . . ? C1 N1 C8 123.30(18) . . ? C7 N1 C8 117.87(18) . . ? C1 N2 C2 113.82(19) . . ? C1 N2 Al 123.55(16) . . ? C2 N2 Al 118.27(15) . . ? C1 N3 C5 124.89(19) . . ? C1 N3 C4 122.23(19) . . ? C5 N3 C4 112.84(18) . . ? C9 N4 C8 121.66(19) . . ? C9 N4 C10 122.96(19) . . ? C8 N4 C10 115.35(18) . . ? C9 N5 C15 113.8(2) . . ? C9 N5 Al 123.81(16) . . ? C15 N5 Al 117.77(16) . . ? C9 N6 C12 118.41(19) . . ? C9 N6 C13 123.0(2) . . ? C12 N6 C13 117.9(2) . . ? N2 C1 N3 122.6(2) . . ? N2 C1 N1 119.54(19) . . ? N3 C1 N1 117.81(19) . . ? N2 C2 C3 108.9(2) . . ? N2 C2 H2A 109.9 . . ? C3 C2 H2A 109.9 . . ? N2 C2 H2B 109.9 . . ? C3 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C4 C3 C2 107.32(19) . . ? C4 C3 H3A 110.3 . . ? C2 C3 H3A 110.3 . . ? C4 C3 H3B 110.3 . . ? C2 C3 H3B 110.3 . . ? H3A C3 H3B 108.5 . . ? N3 C4 C3 112.30(19) . . ? N3 C4 H4A 109.1 . . ? C3 C4 H4A 109.1 . . ? N3 C4 H4B 109.1 . . ? C3 C4 H4B 109.1 . . ? H4A C4 H4B 107.9 . . ? N3 C5 C6 113.0(2) . . ? N3 C5 H5A 109 . . ? C6 C5 H5A 109 . . ? N3 C5 H5B 109 . . ? C6 C5 H5B 109 . . ? H5A C5 H5B 107.8 . . ? C7 C6 C5 109.2(2) . . ? C7 C6 H6A 109.8 . . ? C5 C6 H6A 109.8 . . ? C7 C6 H6B 109.8 . . ? C5 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? N1 C7 C6 108.3(2) . . ? N1 C7 H7A 110 . . ? C6 C7 H7A 110 . . ? N1 C7 H7B 110 . . ? C6 C7 H7B 110 . . ? H7A C7 H7B 108.4 . . ? N4 C8 N1 115.13(19) . . ? N4 C8 H8A 108.5 . . ? N1 C8 H8A 108.5 . . ? N4 C8 H8B 108.5 . . ? N1 C8 H8B 108.5 . . ? H8A C8 H8B 107.5 . . ? N5 C9 N6 122.9(2) . . ? N5 C9 N4 120.3(2) . . ? N6 C9 N4 116.7(2) . . ? N4 C10 C11 112.36(19) . . ? N4 C10 H10A 109.1 . . ? C11 C10 H10A 109.1 . . ? N4 C10 H10B 109.1 . . ? C11 C10 H10B 109.1 . . ? H10A C10 H10B 107.9 . . ? C12 C11 C10 108.6(2) . . ? C12 C11 H11A 110 . . ? C10 C11 H11A 110 . . ? C12 C11 H11B 110 . . ? C10 C11 H11B 110 . . ? H11A C11 H11B 108.4 . . ? N6 C12 C11 108.1(2) . . ? N6 C12 H12A 110.1 . . ? C11 C12 H12A 110.1 . . ? N6 C12 H12B 110.1 . . ? C11 C12 H12B 110.1 . . ? H12A C12 H12B 108.4 . . ? N6 C13 C14 110.8(2) . . ? N6 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? N6 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C13 C14 C15 108.1(2) . . ? C13 C14 H14A 110.1 . . ? C15 C14 H14A 110.1 . . ? C13 C14 H14B 110.1 . . ? C15 C14 H14B 110.1 . . ? H14A C14 H14B 108.4 . . ? N5 C15 C14 109.3(2) . . ? N5 C15 H15A 109.8 . . ? C14 C15 H15A 109.8 . . ? N5 C15 H15B 109.8 . . ? C14 C15 H15B 109.8 . . ? H15A C15 H15B 108.3 . . ? Al C16 H16A 109.5 . . ? Al C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Al C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Al C17 H17A 109.5 . . ? Al C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Al C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 114.7(2) . . ? C23 C18 B 123.01(19) . . ? C19 C18 B 122.22(19) . . ? C20 C19 C18 122.8(2) . . ? C20 C19 H19 118.6 . . ? C18 C19 H19 118.6 . . ? C21 C20 C19 120.3(2) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C22 C21 C20 118.8(2) . . ? C22 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? C21 C22 C23 120.1(2) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C18 123.2(2) . . ? C22 C23 H23 118.4 . . ? C18 C23 H23 118.4 . . ? C29 C24 C25 115.0(2) . . ? C29 C24 B 123.27(19) . . ? C25 C24 B 121.53(19) . . ? C26 C25 C24 123.0(2) . . ? C26 C25 H25 118.5 . . ? C24 C25 H25 118.5 . . ? C27 C26 C25 119.9(2) . . ? C27 C26 H26 120 . . ? C25 C26 H26 120 . . ? C26 C27 C28 119.3(2) . . ? C26 C27 H27 120.4 . . ? C28 C27 H27 120.4 . . ? C27 C28 C29 120.3(2) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C28 C29 C24 122.5(2) . . ? C28 C29 H29 118.8 . . ? C24 C29 H29 118.8 . . ? C31 C30 C35 114.2(2) . . ? C31 C30 B 122.9(2) . . ? C35 C30 B 122.6(2) . . ? C32 C31 C30 123.1(2) . . ? C32 C31 H31 118.5 . . ? C30 C31 H31 118.5 . . ? C33 C32 C31 120.6(2) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 C34 118.5(2) . . ? C32 C33 H33 120.8 . . ? C34 C33 H33 120.8 . . ? C35 C34 C33 120.0(2) . . ? C35 C34 H34 120 . . ? C33 C34 H34 120 . . ? C34 C35 C30 123.6(2) . . ? C34 C35 H35 118.2 . . ? C30 C35 H35 118.2 . . ? C41 C36 C37 115.0(2) . . ? C41 C36 B 121.76(19) . . ? C37 C36 B 122.7(2) . . ? C38 C37 C36 122.5(2) . . ? C38 C37 H37 118.7 . . ? C36 C37 H37 118.7 . . ? C39 C38 C37 120.5(2) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C40 C39 C38 118.7(2) . . ? C40 C39 H39 120.6 . . ? C38 C39 H39 120.6 . . ? C39 C40 C41 120.4(2) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C40 C41 C36 122.8(2) . . ? C40 C41 H41 118.6 . . ? C36 C41 H41 118.6 . . ? N2B Al1B N5B 101.73(9) . . ? N2B Al1B C17B 108.36(11) . . ? N5B Al1B C17B 116.01(11) . . ? N2B Al1B C16B 109.23(11) . . ? N5B Al1B C16B 107.74(11) . . ? C17B Al1B C16B 113.06(13) . . ? C18B B1B C36B 108.99(18) . . ? C18B B1B C24B 108.26(18) . . ? C36B B1B C24B 111.26(19) . . ? C18B B1B C30B 111.30(19) . . ? C36B B1B C30B 109.57(18) . . ? C24B B1B C30B 107.46(18) . . ? C1B N1B C2B 122.7(2) . . ? C1B N1B C8B 123.01(19) . . ? C2B N1B C8B 114.3(2) . . ? C1B N2B C7B 113.89(19) . . ? C1B N2B Al1B 124.99(16) . . ? C7B N2B Al1B 116.65(15) . . ? C1B N3B C4B 121.6(2) . . ? C1B N3B C5B 123.1(2) . . ? C4B N3B C5B 115.0(2) . . ? C9B N4B C8B 121.2(2) . . ? C9B N4B C10B 123.4(2) . . ? C8B N4B C10B 115.27(19) . . ? C9B N5B C15B 113.98(19) . . ? C9B N5B Al1B 125.53(15) . . ? C15B N5B Al1B 117.56(15) . . ? C9B N6B C12B 119.2(2) . . ? C9B N6B C13B 123.1(2) . . ? C12B N6B C13B 117.2(2) . . ? N2B C1B N3B 122.1(2) . . ? N2B C1B N1B 119.6(2) . . ? N3B C1B N1B 118.3(2) . . ? N1B C2B C3B 112.0(2) . . ? N1B C2B H2B1 109.2 . . ? C3B C2B H2B1 109.2 . . ? N1B C2B H2B2 109.2 . . ? C3B C2B H2B2 109.2 . . ? H2B1 C2B H2B2 107.9 . . ? C2B C3B C4B 109.3(3) . . ? C2B C3B H3B1 109.8 . . ? C4B C3B H3B1 109.8 . . ? C2B C3B H3B2 109.8 . . ? C4B C3B H3B2 109.8 . . ? H3B1 C3B H3B2 108.3 . . ? N3B C4B C3B 108.8(2) . . ? N3B C4B H4B1 109.9 . . ? C3B C4B H4B1 109.9 . . ? N3B C4B H4B2 109.9 . . ? C3B C4B H4B2 109.9 . . ? H4B1 C4B H4B2 108.3 . . ? N3B C5B C6B 112.3(2) . . ? N3B C5B H5B1 109.1 . . ? C6B C5B H5B1 109.1 . . ? N3B C5B H5B2 109.1 . . ? C6B C5B H5B2 109.1 . . ? H5B1 C5B H5B2 107.9 . . ? C5B C6B C7B 107.5(2) . . ? C5B C6B H6B1 110.2 . . ? C7B C6B H6B1 110.2 . . ? C5B C6B H6B2 110.2 . . ? C7B C6B H6B2 110.2 . . ? H6B1 C6B H6B2 108.5 . . ? N2B C7B C6B 109.5(2) . . ? N2B C7B H7B1 109.8 . . ? C6B C7B H7B1 109.8 . . ? N2B C7B H7B2 109.8 . . ? C6B C7B H7B2 109.8 . . ? H7B1 C7B H7B2 108.2 . . ? N4B C8B N1B 115.4(2) . . ? N4B C8B H8B1 108.4 . . ? N1B C8B H8B1 108.4 . . ? N4B C8B H8B2 108.4 . . ? N1B C8B H8B2 108.4 . . ? H8B1 C8B H8B2 107.5 . . ? N5B C9B N6B 122.9(2) . . ? N5B C9B N4B 120.4(2) . . ? N6B C9B N4B 116.7(2) . . ? N4B C10B C11B 112.5(2) . . ? N4B C10B H10C 109.1 . . ? C11B C10B H10C 109.1 . . ? N4B C10B H10D 109.1 . . ? C11B C10B H10D 109.1 . . ? H10C C10B H10D 107.8 . . ? C12B C11B C10B 108.2(2) . . ? C12B C11B H11C 110.1 . . ? C10B C11B H11C 110.1 . . ? C12B C11B H11D 110.1 . . ? C10B C11B H11D 110.1 . . ? H11C C11B H11D 108.4 . . ? N6B C12B C11B 107.9(2) . . ? N6B C12B H12C 110.1 . . ? C11B C12B H12C 110.1 . . ? N6B C12B H12D 110.1 . . ? C11B C12B H12D 110.1 . . ? H12C C12B H12D 108.4 . . ? N6B C13B C14B 111.0(2) . . ? N6B C13B H13C 109.4 . . ? C14B C13B H13C 109.4 . . ? N6B C13B H13D 109.4 . . ? C14B C13B H13D 109.4 . . ? H13C C13B H13D 108 . . ? C13B C14B C15B 108.4(2) . . ? C13B C14B H14C 110 . . ? C15B C14B H14C 110 . . ? C13B C14B H14D 110 . . ? C15B C14B H14D 110 . . ? H14C C14B H14D 108.4 . . ? N5B C15B C14B 109.4(2) . . ? N5B C15B H15C 109.8 . . ? C14B C15B H15C 109.8 . . ? N5B C15B H15D 109.8 . . ? C14B C15B H15D 109.8 . . ? H15C C15B H15D 108.3 . . ? Al1B C16B H16D 109.5 . . ? Al1B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? Al1B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? Al1B C17B H17D 109.5 . . ? Al1B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? Al1B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? C23B C18B C19B 114.6(2) . . ? C23B C18B B1B 122.6(2) . . ? C19B C18B B1B 122.6(2) . . ? C20B C19B C18B 123.2(2) . . ? C20B C19B H19B 118.4 . . ? C18B C19B H19B 118.4 . . ? C21B C20B C19B 120.1(2) . . ? C21B C20B H20B 120 . . ? C19B C20B H20B 120 . . ? C22B C21B C20B 118.8(2) . . ? C22B C21B H21B 120.6 . . ? C20B C21B H21B 120.6 . . ? C21B C22B C23B 120.4(2) . . ? C21B C22B H22B 119.8 . . ? C23B C22B H22B 119.8 . . ? C22B C23B C18B 122.9(2) . . ? C22B C23B H23B 118.5 . . ? C18B C23B H23B 118.5 . . ? C29B C24B C25B 114.6(2) . . ? C29B C24B B1B 123.5(2) . . ? C25B C24B B1B 121.6(2) . . ? C26B C25B C24B 123.5(3) . . ? C26B C25B H25B 118.3 . . ? C24B C25B H25B 118.3 . . ? C27B C26B C25B 119.6(3) . . ? C27B C26B H26B 120.2 . . ? C25B C26B H26B 120.2 . . ? C28B C27B C26B 119.3(2) . . ? C28B C27B H27B 120.4 . . ? C26B C27B H27B 120.4 . . ? C27B C28B C29B 120.3(3) . . ? C27B C28B H28B 119.8 . . ? C29B C28B H28B 119.8 . . ? C28B C29B C24B 122.7(3) . . ? C28B C29B H29B 118.6 . . ? C24B C29B H29B 118.6 . . ? C35B C30B C31B 114.9(2) . . ? C35B C30B B1B 122.9(2) . . ? C31B C30B B1B 121.9(2) . . ? C32B C31B C30B 122.8(2) . . ? C32B C31B H31B 118.6 . . ? C30B C31B H31B 118.6 . . ? C33B C32B C31B 120.2(2) . . ? C33B C32B H32B 119.9 . . ? C31B C32B H32B 119.9 . . ? C34B C33B C32B 119.1(2) . . ? C34B C33B H33B 120.5 . . ? C32B C33B H33B 120.5 . . ? C33B C34B C35B 120.6(2) . . ? C33B C34B H34B 119.7 . . ? C35B C34B H34B 119.7 . . ? C34B C35B C30B 122.4(2) . . ? C34B C35B H35B 118.8 . . ? C30B C35B H35B 118.8 . . ? C41B C36B C37B 114.6(2) . . ? C41B C36B B1B 123.6(2) . . ? C37B C36B B1B 121.7(2) . . ? C38B C37B C36B 123.3(2) . . ? C38B C37B H37B 118.3 . . ? C36B C37B H37B 118.3 . . ? C39B C38B C37B 119.9(2) . . ? C39B C38B H38B 120 . . ? C37B C38B H38B 120 . . ? C40B C39B C38B 118.9(2) . . ? C40B C39B H39B 120.6 . . ? C38B C39B H39B 120.6 . . ? C39B C40B C41B 120.3(2) . . ? C39B C40B H40B 119.9 . . ? C41B C40B H40B 119.9 . . ? C40B C41B C36B 122.9(2) . . ? C40B C41B H41B 118.5 . . ? C36B C41B H41B 118.5 . . ? C4S O1S C1S 107.8(2) . . ? O1S C1S C2S 107.5(2) . . ? O1S C1S H1S1 110.2 . . ? C2S C1S H1S1 110.2 . . ? O1S C1S H1S2 110.2 . . ? C2S C1S H1S2 110.2 . . ? H1S1 C1S H1S2 108.5 . . ? C3S C2S C1S 104.0(3) . . ? C3S C2S H2S1 111 . . ? C1S C2S H2S1 111 . . ? C3S C2S H2S2 111 . . ? C1S C2S H2S2 111 . . ? H2S1 C2S H2S2 109 . . ? C4S C3S C2S 105.4(3) . . ? C4S C3S H3S1 110.7 . . ? C2S C3S H3S1 110.7 . . ? C4S C3S H3S2 110.7 . . ? C2S C3S H3S2 110.7 . . ? H3S1 C3S H3S2 108.8 . . ? O1S C4S C3S 107.6(3) . . ? O1S C4S H4S1 110.2 . . ? C3S C4S H4S1 110.2 . . ? O1S C4S H4S2 110.2 . . ? C3S C4S H4S2 110.2 . . ? H4S1 C4S H4S2 108.5 . . ? C5S O2S C8S 110.0(4) . . ? O2S C5S C6S 107.9(4) . . ? O2S C5S H5S2 110.1 . . ? C6S C5S H5S2 110.1 . . ? O2S C5S H5S1 110.1 . . ? C6S C5S H5S1 110.1 . . ? H5S2 C5S H5S1 108.4 . . ? C7S C6S C5S 102.5(5) . . ? C7S C6S H6S1 111.3 . . ? C5S C6S H6S1 111.3 . . ? C7S C6S H6S2 111.3 . . ? C5S C6S H6S2 111.3 . . ? H6S1 C6S H6S2 109.2 . . ? C6S C7S C8S 110.8(4) . . ? C6S C7S H8S2 109.5 . . ? C8S C7S H8S2 109.5 . . ? C6S C7S H8S1 109.5 . . ? C8S C7S H8S1 109.5 . . ? H8S2 C7S H8S1 108.1 . . ? O2S C8S C7S 102.3(4) . . ? O2S C8S H7S2 111.3 . . ? C7S C8S H7S2 111.3 . . ? O2S C8S H7S1 111.3 . . ? C7S C8S H7S1 111.3 . . ? H7S2 C8S H7S1 109.2 . . ? #===END