# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H29 B9 N Ta' _chemical_formula_weight 429.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.9980(10) _cell_length_b 17.4118(13) _cell_length_c 18.0236(14) _cell_angle_alpha 90.00 _cell_angle_beta 98.188(2) _cell_angle_gamma 90.00 _cell_volume 4037.5(5) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 318 _cell_measurement_theta_min 15 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.413 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 5.429 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5206 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _diffrn_measurement_method 'PHI & OMEGA SCAN' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 39562 _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 25.25 _reflns_number_total 7254 _reflns_number_gt 6172 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_cell_refinement 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_data_reduction 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SIEMENS SHELXTL' _computing_publication_material 'SIEMENS SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+1.5280P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7254 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0613 _refine_ls_wR_factor_gt 0.0594 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ta1' Ta 0.872830(12) 1.192645(9) 1.228548(10) 0.04398(6) Uani 1 1 d . . . N1' N 0.8551(3) 1.1676(2) 1.3557(2) 0.0576(9) Uani 1 1 d . . . Ta1 Ta 0.719301(12) 0.877013(9) 0.986494(9) 0.03911(6) Uani 1 1 d . . . N1 N 0.6208(3) 0.88298(18) 0.86546(17) 0.0464(8) Uani 1 1 d . . . C1 C 0.5557(3) 0.7909(2) 0.9883(2) 0.0418(9) Uani 1 1 d . . . C2 C 0.6534(3) 0.7384(2) 1.0150(2) 0.0442(9) Uani 1 1 d . . . H2 H 0.6842 0.7018 0.9736 0.053 Uiso 1 1 calc R . . C11 C 0.5008(4) 0.7863(3) 0.9080(2) 0.0555(11) Uani 1 1 d . . . H11A H 0.4751 0.7344 0.8985 0.067 Uiso 1 1 calc R . . H11B H 0.4411 0.8204 0.9029 0.067 Uiso 1 1 calc R . . C12 C 0.5675(4) 0.8072(2) 0.8492(2) 0.0590(12) Uani 1 1 d . . . H12A H 0.6194 0.7676 0.8470 0.071 Uiso 1 1 calc R . . H12B H 0.5245 0.8096 0.8006 0.071 Uiso 1 1 calc R . . C13 C 0.5385(4) 0.9438(3) 0.8559(3) 0.0616(12) Uani 1 1 d . . . H13A H 0.5025 0.9422 0.8056 0.092 Uiso 1 1 calc R . . H13B H 0.5702 0.9933 0.8654 0.092 Uiso 1 1 calc R . . H13C H 0.4902 0.9348 0.8906 0.092 Uiso 1 1 calc R . . C14 C 0.6857(4) 0.8988(3) 0.8045(3) 0.0683(14) Uani 1 1 d . . . H14A H 0.6417 0.9006 0.7570 0.102 Uiso 1 1 calc R . . H14B H 0.7362 0.8586 0.8037 0.102 Uiso 1 1 calc R . . H14C H 0.7206 0.9471 0.8138 0.102 Uiso 1 1 calc R . . C15 C 0.7147(4) 1.0019(2) 0.9748(3) 0.0635(12) Uani 1 1 d . . . H15A H 0.7789 1.0196 0.9602 0.095 Uiso 1 1 calc R . . H15B H 0.7053 1.0248 1.0218 0.095 Uiso 1 1 calc R . . H15C H 0.6581 1.0161 0.9372 0.095 Uiso 1 1 calc R . . C16 C 0.8780(4) 0.9059(3) 1.0384(4) 0.0863(17) Uani 1 1 d . . . H16A H 0.8943 0.9573 1.0248 0.129 Uiso 1 1 calc R . . H16B H 0.9263 0.8708 1.0211 0.129 Uiso 1 1 calc R . . H16C H 0.8827 0.9023 1.0919 0.129 Uiso 1 1 calc R . . C17 C 0.8112(4) 0.8006(3) 0.9250(3) 0.0690(14) Uani 1 1 d . . . H17A H 0.8573 0.8306 0.8995 0.104 Uiso 1 1 calc R . . H17B H 0.7654 0.7715 0.8889 0.104 Uiso 1 1 calc R . . H17C H 0.8510 0.7662 0.9594 0.104 Uiso 1 1 calc R . . B3 B 0.7322(4) 0.7783(3) 1.0854(3) 0.0497(12) Uani 1 1 d . . . H3 H 0.8165 0.7674 1.0940 0.060 Uiso 1 1 calc R . . B4 B 0.6710(4) 0.8651(3) 1.1069(3) 0.0505(12) Uani 1 1 d . . . H4 H 0.7121 0.9151 1.1341 0.061 Uiso 1 1 calc R . . B5 B 0.5599(4) 0.8696(3) 1.0405(2) 0.0428(10) Uani 1 1 d . . . H5 H 0.5233 0.9233 1.0180 0.051 Uiso 1 1 calc R . . B6 B 0.5363(4) 0.7078(3) 1.0379(3) 0.0540(13) Uani 1 1 d . . . H6 H 0.4926 0.6569 1.0150 0.065 Uiso 1 1 calc R . . B7 B 0.6515(4) 0.7005(3) 1.1027(3) 0.0553(13) Uani 1 1 d . . . H7 H 0.6836 0.6444 1.1222 0.066 Uiso 1 1 calc R . . B8 B 0.6592(5) 0.7808(3) 1.1620(3) 0.0575(13) Uani 1 1 d . . . H8 H 0.6958 0.7772 1.2208 0.069 Uiso 1 1 calc R . . B9 B 0.5485(5) 0.8394(3) 1.1332(3) 0.0604(14) Uani 1 1 d . . . H9 H 0.5115 0.8744 1.1729 0.072 Uiso 1 1 calc R . . B10 B 0.4750(4) 0.7941(3) 1.0556(3) 0.0555(13) Uani 1 1 d . . . H10 H 0.3900 0.7998 1.0438 0.067 Uiso 1 1 calc R . . B11 B 0.5372(4) 0.7385(3) 1.1312(3) 0.0585(13) Uani 1 1 d . . . H11 H 0.4936 0.7078 1.1701 0.070 Uiso 1 1 calc R . . B3' B 0.9294(4) 1.3082(3) 1.1675(3) 0.0583(14) Uani 1 1 d . . . H3' H 0.9941 1.2846 1.1414 0.070 Uiso 1 1 calc R . . B4' B 0.7977(4) 1.2858(3) 1.1420(3) 0.0540(13) Uani 1 1 d . . . H4' H 0.7680 1.2477 1.0952 0.065 Uiso 1 1 calc R . . B5' B 0.7425(4) 1.2954(3) 1.2255(3) 0.0476(11) Uani 1 1 d . . . H5' H 0.6755 1.2627 1.2395 0.057 Uiso 1 1 calc R . . B6' B 0.8804(4) 1.4154(3) 1.2762(3) 0.0548(13) Uani 1 1 d . . . H6' H 0.9080 1.4574 1.3202 0.066 Uiso 1 1 calc R . . B7' B 0.9392(5) 1.4060(3) 1.1944(3) 0.0640(15) Uani 1 1 d . . . H7' H 1.0057 1.4418 1.1846 0.077 Uiso 1 1 calc R . . B8' B 0.8433(5) 1.3777(3) 1.1210(3) 0.0688(16) Uani 1 1 d . . . H8' H 0.8462 1.3955 1.0628 0.083 Uiso 1 1 calc R . . B9' B 0.7251(5) 1.3689(3) 1.1576(3) 0.0659(15) Uani 1 1 d . . . H9' H 0.6496 1.3808 1.1236 0.079 Uiso 1 1 calc R . . B10' B 0.7497(4) 1.3920(3) 1.2544(3) 0.0558(13) Uani 1 1 d . . . H10' H 0.6910 1.4186 1.2845 0.067 Uiso 1 1 calc R . . B11' B 0.8126(5) 1.4440(3) 1.1895(3) 0.0654(15) Uani 1 1 d . . . H11' H 0.7949 1.5046 1.1762 0.078 Uiso 1 1 calc R . . C1' C 0.8373(3) 1.3234(2) 1.2913(2) 0.0439(9) Uani 1 1 d . . . C2' C 0.9442(3) 1.3311(2) 1.2592(2) 0.0491(10) Uani 1 1 d . . . H2' H 1.0174 1.3208 1.2966 0.059 Uiso 1 1 calc R . . C11' C 0.8406(4) 1.3081(2) 1.3756(2) 0.0643(13) Uani 1 1 d . . . H11C H 0.7700 1.3053 1.3871 0.077 Uiso 1 1 calc R . . H11D H 0.8747 1.3509 1.4035 0.077 Uiso 1 1 calc R . . C12' C 0.8990(5) 1.2323(3) 1.4020(3) 0.0733(15) Uani 1 1 d . . . H12C H 0.9723 1.2377 1.3979 0.088 Uiso 1 1 calc R . . H12D H 0.8925 1.2227 1.4541 0.088 Uiso 1 1 calc R . . C13' C 0.7442(4) 1.1563(3) 1.3712(4) 0.0881(18) Uani 1 1 d . . . H13D H 0.7445 1.1465 1.4236 0.132 Uiso 1 1 calc R . . H13E H 0.7137 1.1134 1.3426 0.132 Uiso 1 1 calc R . . H13F H 0.7045 1.2017 1.3570 0.132 Uiso 1 1 calc R . . C14' C 0.9076(5) 1.0951(3) 1.3844(3) 0.0901(18) Uani 1 1 d . . . H14D H 0.8983 1.0877 1.4358 0.135 Uiso 1 1 calc R . . H14E H 0.9805 1.0984 1.3809 0.135 Uiso 1 1 calc R . . H14F H 0.8779 1.0525 1.3550 0.135 Uiso 1 1 calc R . . C15' C 0.7517(4) 1.1051(3) 1.2098(3) 0.0762(15) Uani 1 1 d . . . H15D H 0.7777 1.0612 1.1861 0.114 Uiso 1 1 calc R . . H15E H 0.6924 1.1255 1.1781 0.114 Uiso 1 1 calc R . . H15F H 0.7317 1.0901 1.2570 0.114 Uiso 1 1 calc R . . C16' C 0.9199(4) 1.1293(3) 1.1339(3) 0.0800(16) Uani 1 1 d . . . H16D H 0.9161 1.0752 1.1431 0.120 Uiso 1 1 calc R . . H16E H 0.9899 1.1429 1.1282 0.120 Uiso 1 1 calc R . . H16F H 0.8742 1.1421 1.0890 0.120 Uiso 1 1 calc R . . C17' C 1.0351(3) 1.1700(3) 1.2702(3) 0.0660(13) Uani 1 1 d . . . H17D H 1.0556 1.1223 1.2497 0.099 Uiso 1 1 calc R . . H17E H 1.0442 1.1667 1.3239 0.099 Uiso 1 1 calc R . . H17F H 1.0772 1.2109 1.2553 0.099 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ta1' 0.04222(10) 0.03327(9) 0.05753(12) -0.00547(7) 0.01084(8) -0.00013(6) N1' 0.065(2) 0.046(2) 0.063(2) 0.0089(18) 0.014(2) 0.0030(18) Ta1 0.03723(10) 0.03667(9) 0.04318(10) -0.00122(7) 0.00493(7) 0.00033(6) N1 0.060(2) 0.0419(19) 0.0381(18) 0.0001(14) 0.0102(16) -0.0083(15) C1 0.044(2) 0.046(2) 0.035(2) 0.0033(17) 0.0053(17) -0.0052(17) C2 0.058(2) 0.034(2) 0.044(2) 0.0026(17) 0.0173(19) 0.0081(17) C11 0.062(3) 0.063(3) 0.039(2) 0.008(2) -0.003(2) -0.023(2) C12 0.088(4) 0.057(3) 0.031(2) -0.0021(19) 0.003(2) -0.029(2) C13 0.065(3) 0.062(3) 0.054(3) 0.016(2) -0.003(2) 0.009(2) C14 0.096(4) 0.067(3) 0.048(3) 0.003(2) 0.035(3) -0.013(3) C15 0.071(3) 0.045(3) 0.071(3) -0.008(2) -0.002(3) -0.006(2) C16 0.047(3) 0.088(4) 0.115(5) 0.011(3) -0.018(3) -0.013(3) C17 0.060(3) 0.066(3) 0.088(4) 0.010(3) 0.034(3) 0.015(2) B3 0.049(3) 0.053(3) 0.045(3) 0.004(2) 0.001(2) 0.011(2) B4 0.067(3) 0.044(3) 0.038(3) -0.006(2) -0.002(2) 0.007(2) B5 0.045(3) 0.048(3) 0.037(2) -0.0017(19) 0.010(2) 0.011(2) B6 0.070(3) 0.047(3) 0.047(3) 0.011(2) 0.015(3) -0.014(2) B7 0.076(4) 0.049(3) 0.043(3) 0.013(2) 0.012(3) 0.010(2) B8 0.077(4) 0.058(3) 0.035(3) 0.008(2) 0.004(2) 0.009(3) B9 0.075(4) 0.069(4) 0.041(3) 0.003(2) 0.022(3) 0.018(3) B10 0.041(3) 0.077(4) 0.051(3) 0.019(3) 0.016(2) 0.006(2) B11 0.070(3) 0.066(3) 0.043(3) 0.015(2) 0.020(3) 0.001(3) B3' 0.066(3) 0.052(3) 0.062(3) -0.006(2) 0.028(3) -0.009(2) B4' 0.071(3) 0.046(3) 0.045(3) -0.006(2) 0.005(3) 0.000(2) B5' 0.041(3) 0.037(2) 0.066(3) -0.002(2) 0.010(2) 0.0003(19) B6' 0.075(4) 0.029(2) 0.063(3) -0.006(2) 0.018(3) -0.009(2) B7' 0.082(4) 0.041(3) 0.077(4) 0.007(3) 0.038(3) -0.012(3) B8' 0.105(5) 0.050(3) 0.053(3) 0.009(2) 0.019(3) 0.003(3) B9' 0.075(4) 0.052(3) 0.065(4) 0.004(3) -0.008(3) 0.010(3) B10' 0.058(3) 0.037(3) 0.074(4) -0.002(2) 0.014(3) 0.007(2) B11' 0.086(4) 0.040(3) 0.070(4) 0.005(3) 0.011(3) 0.000(3) C1' 0.049(2) 0.032(2) 0.052(2) -0.0039(17) 0.0133(19) 0.0025(17) C2' 0.044(2) 0.039(2) 0.067(3) -0.004(2) 0.013(2) -0.0102(17) C11' 0.100(4) 0.043(3) 0.053(3) -0.003(2) 0.023(3) 0.002(2) C12' 0.108(4) 0.058(3) 0.053(3) 0.002(2) 0.008(3) -0.007(3) C13' 0.089(4) 0.071(4) 0.114(5) 0.016(3) 0.048(4) -0.008(3) C14' 0.119(5) 0.053(3) 0.095(4) 0.022(3) 0.003(4) 0.015(3) C15' 0.060(3) 0.071(3) 0.096(4) -0.002(3) 0.005(3) -0.025(3) C16' 0.082(4) 0.066(3) 0.097(4) -0.038(3) 0.031(3) -0.008(3) C17' 0.041(3) 0.059(3) 0.098(4) -0.004(3) 0.010(2) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1' C17' 2.172(4) . ? Ta1' C15' 2.183(5) . ? Ta1' C16' 2.190(5) . ? Ta1' B4' 2.363(5) . ? Ta1' N1' 2.376(4) . ? Ta1' B3' 2.455(5) . ? Ta1' B5' 2.460(5) . ? Ta1' C1' 2.612(4) . ? Ta1' C2' 2.613(4) . ? N1' C12' 1.469(6) . ? N1' C14' 1.492(6) . ? N1' C13' 1.520(6) . ? Ta1 C15 2.184(4) . ? Ta1 C17 2.192(4) . ? Ta1 C16 2.198(5) . ? Ta1 B4 2.352(5) . ? Ta1 N1 2.369(3) . ? Ta1 B5 2.416(5) . ? Ta1 B3 2.465(5) . ? Ta1 C1 2.607(4) . ? Ta1 C2 2.636(4) . ? N1 C13 1.497(5) . ? N1 C12 1.499(5) . ? N1 C14 1.503(5) . ? C1 C11 1.522(5) . ? C1 C2 1.583(5) . ? C1 B5 1.660(6) . ? C1 B10 1.714(6) . ? C1 B6 1.737(6) . ? C2 B3 1.665(6) . ? C2 B7 1.717(6) . ? C2 B6 1.718(6) . ? C11 C12 1.507(6) . ? B3 B7 1.768(7) . ? B3 B4 1.776(7) . ? B3 B8 1.784(7) . ? B4 B5 1.741(7) . ? B4 B9 1.782(8) . ? B4 B8 1.791(7) . ? B5 B10 1.762(7) . ? B5 B9 1.777(7) . ? B6 B10 1.751(8) . ? B6 B11 1.764(7) . ? B6 B7 1.768(8) . ? B7 B8 1.754(8) . ? B7 B11 1.768(8) . ? B8 B11 1.765(8) . ? B8 B9 1.779(8) . ? B9 B11 1.763(8) . ? B9 B10 1.763(8) . ? B10 B11 1.770(7) . ? B3' C2' 1.683(7) . ? B3' B4' 1.752(8) . ? B3' B7' 1.771(7) . ? B3' B8' 1.776(8) . ? B4' B5' 1.764(7) . ? B4' B8' 1.765(7) . ? B4' B9' 1.772(8) . ? B5' C1' 1.658(6) . ? B5' B10' 1.759(7) . ? B5' B9' 1.763(7) . ? B6' C1' 1.732(6) . ? B6' C2' 1.736(6) . ? B6' B10' 1.736(8) . ? B6' B11' 1.753(8) . ? B6' B7' 1.764(7) . ? B7' C2' 1.747(7) . ? B7' B8' 1.754(9) . ? B7' B11' 1.764(8) . ? B8' B9' 1.762(9) . ? B8' B11' 1.776(8) . ? B9' B11' 1.773(8) . ? B9' B10' 1.775(8) . ? B10' C1' 1.718(6) . ? B10' B11' 1.767(8) . ? C1' C11' 1.537(6) . ? C1' C2' 1.585(5) . ? C11' C12' 1.562(7) . ? 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 C17' Ta1' C15' 124.8(2) . . ? C17' Ta1' C16' 79.2(2) . . ? C15' Ta1' C16' 78.6(2) . . ? C17' Ta1' B4' 130.0(2) . . ? C15' Ta1' B4' 99.0(2) . . ? C16' Ta1' B4' 88.1(2) . . ? C17' Ta1' N1' 81.73(17) . . ? C15' Ta1' N1' 81.62(18) . . ? C16' Ta1' N1' 137.28(18) . . ? B4' Ta1' N1' 132.46(15) . . ? C17' Ta1' B3' 88.0(2) . . ? C15' Ta1' B3' 139.3(2) . . ? C16' Ta1' B3' 85.93(19) . . ? B4' Ta1' B3' 42.60(19) . . ? N1' Ta1' B3' 131.22(16) . . ? C17' Ta1' B5' 140.53(17) . . ? C15' Ta1' B5' 91.46(19) . . ? C16' Ta1' B5' 128.1(2) . . ? B4' Ta1' B5' 42.85(17) . . ? N1' Ta1' B5' 89.70(15) . . ? B3' Ta1' B5' 69.08(18) . . ? C17' Ta1' C1' 103.39(16) . . ? C15' Ta1' C1' 120.50(18) . . ? C16' Ta1' C1' 149.59(18) . . ? B4' Ta1' C1' 66.79(15) . . ? N1' Ta1' C1' 72.24(12) . . ? B3' Ta1' C1' 64.08(15) . . ? B5' Ta1' C1' 38.01(14) . . ? C17' Ta1' C2' 78.26(16) . . ? C15' Ta1' C2' 154.59(18) . . ? C16' Ta1' C2' 119.93(17) . . ? B4' Ta1' C2' 66.87(16) . . ? N1' Ta1' C2' 92.63(13) . . ? B3' Ta1' C2' 38.64(16) . . ? B5' Ta1' C2' 63.66(14) . . ? C1' Ta1' C2' 35.32(12) . . ? C12' N1' C14' 109.4(4) . . ? C12' N1' C13' 107.3(4) . . ? C14' N1' C13' 103.1(4) . . ? C12' N1' Ta1' 108.9(3) . . ? C14' N1' Ta1' 112.8(3) . . ? C13' N1' Ta1' 115.2(3) . . ? C15 Ta1 C17 124.37(18) . . ? C15 Ta1 C16 79.9(2) . . ? C17 Ta1 C16 78.9(2) . . ? C15 Ta1 B4 99.77(17) . . ? C17 Ta1 B4 130.51(18) . . ? C16 Ta1 B4 89.2(2) . . ? C15 Ta1 N1 82.17(14) . . ? C17 Ta1 N1 79.78(17) . . ? C16 Ta1 N1 137.12(18) . . ? B4 Ta1 N1 132.30(15) . . ? C15 Ta1 B5 94.52(17) . . ? C17 Ta1 B5 137.09(17) . . ? C16 Ta1 B5 130.4(2) . . ? B4 Ta1 B5 42.81(17) . . ? N1 Ta1 B5 89.51(14) . . ? C15 Ta1 B3 139.64(17) . . ? C17 Ta1 B3 87.53(18) . . ? C16 Ta1 B3 83.6(2) . . ? B4 Ta1 B3 43.19(16) . . ? N1 Ta1 B3 131.98(14) . . ? B5 Ta1 B3 69.22(16) . . ? C15 Ta1 C1 124.27(16) . . ? C17 Ta1 C1 99.28(16) . . ? C16 Ta1 C1 147.58(18) . . ? B4 Ta1 C1 67.19(15) . . ? N1 Ta1 C1 72.66(11) . . ? B5 Ta1 C1 38.37(14) . . ? B3 Ta1 C1 63.97(15) . . ? C15 Ta1 C2 157.69(16) . . ? C17 Ta1 C2 76.02(15) . . ? C16 Ta1 C2 115.96(18) . . ? B4 Ta1 C2 66.59(15) . . ? N1 Ta1 C2 94.12(12) . . ? B5 Ta1 C2 63.36(14) . . ? B3 Ta1 C2 37.91(15) . . ? C1 Ta1 C2 35.14(12) . . ? C13 N1 C12 107.3(4) . . ? C13 N1 C14 104.6(3) . . ? C12 N1 C14 108.0(3) . . ? C13 N1 Ta1 114.8(2) . . ? C12 N1 Ta1 108.4(2) . . ? C14 N1 Ta1 113.3(3) . . ? C11 C1 C2 120.4(4) . . ? C11 C1 B5 123.7(3) . . ? C2 C1 B5 110.2(3) . . ? C11 C1 B10 115.1(4) . . ? C2 C1 B10 110.4(3) . . ? B5 C1 B10 62.9(3) . . ? C11 C1 B6 111.3(3) . . ? C2 C1 B6 62.1(3) . . ? B5 C1 B6 113.1(3) . . ? B10 C1 B6 61.0(3) . . ? C11 C1 Ta1 106.9(2) . . ? C2 C1 Ta1 73.5(2) . . ? B5 C1 Ta1 64.6(2) . . ? B10 C1 Ta1 124.9(3) . . ? B6 C1 Ta1 131.6(3) . . ? C1 C2 B3 111.8(3) . . ? C1 C2 B7 112.7(3) . . ? B3 C2 B7 63.0(3) . . ? C1 C2 B6 63.4(3) . . ? B3 C2 B6 114.6(3) . . ? B7 C2 B6 62.0(3) . . ? C1 C2 Ta1 71.41(19) . . ? B3 C2 Ta1 65.5(2) . . ? B7 C2 Ta1 125.4(3) . . ? B6 C2 Ta1 130.9(3) . . ? C12 C11 C1 114.7(4) . . ? N1 C12 C11 111.8(3) . . ? C2 B3 B7 59.9(3) . . ? C2 B3 B4 106.0(3) . . ? B7 B3 B4 108.5(4) . . ? C2 B3 B8 105.2(4) . . ? B7 B3 B8 59.2(3) . . ? B4 B3 B8 60.4(3) . . ? C2 B3 Ta1 76.6(2) . . ? B7 B3 Ta1 132.9(3) . . ? B4 B3 Ta1 65.0(2) . . ? B8 B3 Ta1 123.6(3) . . ? B5 B4 B3 104.0(3) . . ? B5 B4 B9 60.6(3) . . ? B3 B4 B9 106.8(4) . . ? B5 B4 B8 106.8(4) . . ? B3 B4 B8 60.0(3) . . ? B9 B4 B8 59.7(3) . . ? B5 B4 Ta1 70.5(2) . . ? B3 B4 Ta1 71.8(2) . . ? B9 B4 Ta1 129.3(3) . . ? B8 B4 Ta1 129.7(3) . . ? C1 B5 B4 108.0(3) . . ? C1 B5 B10 60.0(3) . . ? B4 B5 B10 109.7(3) . . ? C1 B5 B9 106.7(3) . . ? B4 B5 B9 60.9(3) . . ? B10 B5 B9 59.8(3) . . ? C1 B5 Ta1 77.0(2) . . ? B4 B5 Ta1 66.7(2) . . ? B10 B5 Ta1 133.9(3) . . ? B9 B5 Ta1 125.9(3) . . ? C2 B6 C1 54.5(2) . . ? C2 B6 B10 102.7(3) . . ? C1 B6 B10 58.8(3) . . ? C2 B6 B11 104.4(4) . . ? C1 B6 B11 104.9(3) . . ? B10 B6 B11 60.5(3) . . ? C2 B6 B7 59.0(3) . . ? C1 B6 B7 103.2(3) . . ? B10 B6 B7 107.8(4) . . ? B11 B6 B7 60.1(3) . . ? C2 B7 B8 104.3(3) . . ? C2 B7 B6 59.1(3) . . ? B8 B7 B6 108.3(4) . . ? C2 B7 B3 57.1(3) . . ? B8 B7 B3 60.9(3) . . ? B6 B7 B3 107.2(3) . . ? C2 B7 B11 104.3(3) . . ? B8 B7 B11 60.1(3) . . ? B6 B7 B11 59.8(3) . . ? B3 B7 B11 108.0(4) . . ? B7 B8 B11 60.3(3) . . ? B7 B8 B9 107.8(4) . . ? B11 B8 B9 59.7(3) . . ? B7 B8 B3 60.0(3) . . ? B11 B8 B3 107.5(4) . . ? B9 B8 B3 106.6(3) . . ? B7 B8 B4 108.5(3) . . ? B11 B8 B4 108.2(4) . . ? B9 B8 B4 59.9(3) . . ? B3 B8 B4 59.6(3) . . ? B11 B9 B10 60.3(3) . . ? B11 B9 B5 107.1(4) . . ? B10 B9 B5 59.7(3) . . ? B11 B9 B8 59.8(3) . . ? B10 B9 B8 107.4(4) . . ? B5 B9 B8 105.8(4) . . ? B11 B9 B4 108.7(4) . . ? B10 B9 B4 107.8(3) . . ? B5 B9 B4 58.6(3) . . ? B8 B9 B4 60.4(3) . . ? C1 B10 B6 60.2(3) . . ? C1 B10 B5 57.0(2) . . ? B6 B10 B5 107.6(3) . . ? C1 B10 B9 105.0(3) . . ? B6 B10 B9 108.7(4) . . ? B5 B10 B9 60.5(3) . . ? C1 B10 B11 105.6(3) . . ? B6 B10 B11 60.1(3) . . ? B5 B10 B11 107.5(4) . . ? B9 B10 B11 59.9(3) . . ? B9 B11 B6 108.1(3) . . ? B9 B11 B8 60.6(3) . . ? B6 B11 B8 108.1(4) . . ? B9 B11 B7 107.9(4) . . ? B6 B11 B7 60.1(3) . . ? B8 B11 B7 59.5(3) . . ? B9 B11 B10 59.9(3) . . ? B6 B11 B10 59.4(3) . . ? B8 B11 B10 107.8(4) . . ? B7 B11 B10 106.9(3) . . ? C2' B3' B4' 106.3(3) . . ? C2' B3' B7' 60.7(3) . . ? B4' B3' B7' 108.3(4) . . ? C2' B3' B8' 106.1(4) . . ? B4' B3' B8' 60.0(3) . . ? B7' B3' B8' 59.3(3) . . ? C2' B3' Ta1' 75.8(2) . . ? B4' B3' Ta1' 65.9(2) . . ? B7' B3' Ta1' 132.9(3) . . ? B8' B3' Ta1' 124.1(3) . . ? B3' B4' B5' 104.8(3) . . ? B3' B4' B8' 60.7(3) . . ? B5' B4' B8' 106.6(4) . . ? B3' B4' B9' 107.4(4) . . ? B5' B4' B9' 59.8(3) . . ? B8' B4' B9' 59.7(3) . . ? B3' B4' Ta1' 71.5(3) . . ? B5' B4' Ta1' 71.5(2) . . ? B8' B4' Ta1' 130.1(4) . . ? B9' B4' Ta1' 129.5(3) . . ? C1' B5' B10' 60.3(3) . . ? C1' B5' B9' 107.0(3) . . ? B10' B5' B9' 60.5(3) . . ? C1' B5' B4' 106.7(3) . . ? B10' B5' B4' 109.4(4) . . ? B9' B5' B4' 60.3(3) . . ? C1' B5' Ta1' 76.0(2) . . ? B10' B5' Ta1' 132.9(3) . . ? B9' B5' Ta1' 124.3(3) . . ? B4' B5' Ta1' 65.7(2) . . ? C1' B6' C2' 54.4(2) . . ? C1' B6' B10' 59.4(3) . . ? C2' B6' B10' 103.7(3) . . ? C1' B6' B11' 105.7(4) . . ? C2' B6' B11' 105.9(4) . . ? B10' B6' B11' 60.9(3) . . ? C1' B6' B7' 103.5(3) . . ? C2' B6' B7' 59.9(3) . . ? B10' B6' B7' 108.4(4) . . ? B11' B6' B7' 60.2(3) . . ? C2' B7' B8' 104.4(4) . . ? C2' B7' B6' 59.3(3) . . ? B8' B7' B6' 108.1(4) . . ? C2' B7' B11' 105.0(4) . . ? B8' B7' B11' 60.6(3) . . ? B6' B7' B11' 59.6(3) . . ? C2' B7' B3' 57.2(3) . . ? B8' B7' B3' 60.5(3) . . ? B6' B7' B3' 107.1(3) . . ? B11' B7' B3' 108.4(4) . . ? B7' B8' B9' 107.9(4) . . ? B7' B8' B4' 108.5(4) . . ? B9' B8' B4' 60.3(3) . . ? B7' B8' B11' 60.0(3) . . ? B9' B8' B11' 60.2(3) . . ? B4' B8' B11' 108.9(4) . . ? B7' B8' B3' 60.2(3) . . ? B9' B8' B3' 106.8(4) . . ? B4' B8' B3' 59.3(3) . . ? B11' B8' B3' 107.7(4) . . ? B8' B9' B5' 106.8(4) . . ? B8' B9' B4' 59.9(3) . . ? B5' B9' B4' 59.9(3) . . ? B8' B9' B11' 60.3(3) . . ? B5' B9' B11' 107.2(4) . . ? B4' B9' B11' 108.8(4) . . ? B8' B9' B10' 107.6(4) . . ? B5' B9' B10' 59.6(3) . . ? B4' B9' B10' 108.3(4) . . ? B11' B9' B10' 59.8(3) . . ? C1' B10' B6' 60.2(3) . . ? C1' B10' B5' 56.9(3) . . ? B6' B10' B5' 107.5(3) . . ? C1' B10' B11' 105.6(4) . . ? B6' B10' B11' 60.0(3) . . ? B5' B10' B11' 107.7(4) . . ? C1' B10' B9' 103.9(3) . . ? B6' B10' B9' 108.0(4) . . ? B5' B10' B9' 59.8(3) . . ? B11' B10' B9' 60.1(3) . . ? B6' B11' B7' 60.2(3) . . ? B6' B11' B10' 59.1(3) . . ? B7' B11' B10' 107.0(4) . . ? B6' B11' B9' 107.4(4) . . ? B7' B11' B9' 106.9(4) . . ? B10' B11' B9' 60.2(3) . . ? B6' B11' B8' 107.5(4) . . ? B7' B11' B8' 59.4(3) . . ? B10' B11' B8' 107.3(4) . . ? B9' B11' B8' 59.5(3) . . ? C11' C1' C2' 118.3(4) . . ? C11' C1' B5' 124.8(4) . . ? C2' C1' B5' 111.3(3) . . ? C11' C1' B10' 115.3(3) . . ? C2' C1' B10' 111.5(3) . . ? B5' C1' B10' 62.8(3) . . ? C11' C1' B6' 110.6(3) . . ? C2' C1' B6' 62.9(3) . . ? B5' C1' B6' 112.5(3) . . ? B10' C1' B6' 60.4(3) . . ? C11' C1' Ta1' 107.2(2) . . ? C2' C1' Ta1' 72.36(19) . . ? B5' C1' Ta1' 66.00(19) . . ? B10' C1' Ta1' 125.9(3) . . ? B6' C1' Ta1' 131.1(3) . . ? C1' C2' B3' 110.8(3) . . ? C1' C2' B6' 62.7(3) . . ? B3' C2' B6' 112.5(4) . . ? C1' C2' B7' 110.9(3) . . ? B3' C2' B7' 62.1(3) . . ? B6' C2' B7' 60.8(3) . . ? C1' C2' Ta1' 72.32(19) . . ? B3' C2' Ta1' 65.6(2) . . ? B6' C2' Ta1' 130.8(3) . . ? B7' C2' Ta1' 124.7(3) . . ? C1' C11' C12' 113.0(4) . . ? N1' C12' C11' 110.1(4) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.902 _refine_diff_density_min -0.817 _refine_diff_density_rms 0.081 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.499 0.000 0.500 395.5 103.0 2 0.499 0.500 0.000 395.6 102.9 _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 943870' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H42 B9 N2 O Ta' _chemical_formula_weight 616.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.7587(18) _cell_length_b 18.933(3) _cell_length_c 19.809(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5534.9(13) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2464 _exptl_absorpt_coefficient_mu 3.989 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2983 _exptl_absorpt_correction_T_max 0.5026 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40396 _diffrn_reflns_av_R_equivalents 0.0895 _diffrn_reflns_av_sigmaI/netI 0.0522 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.24 _reflns_number_total 5010 _reflns_number_gt 3700 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5010 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0745 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1830 _refine_ls_wR_factor_gt 0.1389 _refine_ls_goodness_of_fit_ref 1.299 _refine_ls_restrained_S_all 1.299 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ta1 Ta 0.72299(2) 0.025532(15) 0.837068(15) 0.03621(19) Uani 1 1 d . . . O1 O 0.8077(4) -0.0499(3) 0.8960(3) 0.0571(15) Uani 1 1 d . . . C1 C 0.6626(6) -0.0276(4) 0.7278(5) 0.048(2) Uani 1 1 d . . . C2 C 0.6527(5) 0.0563(4) 0.7257(4) 0.0466(19) Uani 1 1 d . . . H2 H 0.5892 0.0805 0.7433 0.056 Uiso 1 1 calc R . . C11 C 0.5808(5) -0.0709(4) 0.7507(4) 0.051(2) Uani 1 1 d . . . H11A H 0.5271 -0.0420 0.7452 0.062 Uiso 1 1 calc R . . H11B H 0.5748 -0.1110 0.7206 0.062 Uiso 1 1 calc R . . C12 C 0.5822(6) -0.0983(5) 0.8225(5) 0.058(2) Uani 1 1 d . . . H12A H 0.5221 -0.1151 0.8341 0.069 Uiso 1 1 calc R . . H12B H 0.6232 -0.1383 0.8249 0.069 Uiso 1 1 calc R . . C13 C 0.5952(7) -0.0686(6) 0.9417(5) 0.077(3) Uani 1 1 d . . . H13A H 0.5427 -0.0986 0.9424 0.116 Uiso 1 1 calc R . . H13B H 0.5855 -0.0289 0.9709 0.116 Uiso 1 1 calc R . . H13C H 0.6470 -0.0948 0.9570 0.116 Uiso 1 1 calc R . . C14 C 0.5790(7) 0.0278(4) 0.8606(5) 0.054(2) Uani 1 1 d . . . H14A H 0.5615 0.0551 0.9000 0.064 Uiso 1 1 calc R . . H14B H 0.5382 0.0337 0.8227 0.064 Uiso 1 1 calc R . . C15 C 0.7911(5) 0.1480(4) 0.9353(4) 0.0426(18) Uani 1 1 d . . . C16 C 0.7345(6) 0.1737(5) 0.9876(4) 0.052(2) Uani 1 1 d . . . C17 C 0.7656(7) 0.2263(5) 1.0297(5) 0.067(3) Uani 1 1 d . . . H17A H 0.7285 0.2428 1.0642 0.081 Uiso 1 1 calc R . . C18 C 0.8513(9) 0.2550(5) 1.0213(5) 0.078(3) Uani 1 1 d . . . H18A H 0.8713 0.2904 1.0502 0.094 Uiso 1 1 calc R . . C19 C 0.9061(7) 0.2317(5) 0.9712(5) 0.068(3) Uani 1 1 d . . . H19A H 0.9634 0.2515 0.9661 0.081 Uiso 1 1 calc R . . C20 C 0.8776(6) 0.1777(4) 0.9265(4) 0.049(2) Uani 1 1 d . . . C21 C 0.9407(6) 0.1559(5) 0.8716(5) 0.062(2) Uani 1 1 d . . . H21A H 0.9128 0.1195 0.8449 0.093 Uiso 1 1 calc R . . H21B H 0.9958 0.1382 0.8910 0.093 Uiso 1 1 calc R . . H21C H 0.9540 0.1958 0.8434 0.093 Uiso 1 1 calc R . . C22 C 0.6422(7) 0.1442(5) 0.9987(5) 0.070(3) Uani 1 1 d . . . H22A H 0.6141 0.1679 1.0360 0.106 Uiso 1 1 calc R . . H22B H 0.6468 0.0946 1.0084 0.106 Uiso 1 1 calc R . . H22C H 0.6064 0.1509 0.9587 0.106 Uiso 1 1 calc R . . C23 C 0.7473(6) 0.1848(4) 0.7618(4) 0.053(2) Uani 1 1 d . . . H23A H 0.7724 0.1862 0.8076 0.064 Uiso 1 1 calc R . . C24 C 0.6526(8) 0.2138(5) 0.7662(6) 0.093(4) Uani 1 1 d . . . H24A H 0.6549 0.2620 0.7812 0.139 Uiso 1 1 calc R . . H24B H 0.6180 0.1863 0.7977 0.139 Uiso 1 1 calc R . . H24C H 0.6245 0.2117 0.7226 0.139 Uiso 1 1 calc R . . C25 C 0.8068(10) 0.2326(5) 0.7185(5) 0.089(4) Uani 1 1 d . . . H25A H 0.8024 0.2803 0.7346 0.134 Uiso 1 1 calc R . . H25B H 0.7869 0.2305 0.6724 0.134 Uiso 1 1 calc R . . H25C H 0.8686 0.2170 0.7213 0.134 Uiso 1 1 calc R . . C26 C 0.8052(9) -0.1260(6) 0.9026(7) 0.090(4) Uani 1 1 d . . . H26A H 0.7598 -0.1400 0.9354 0.108 Uiso 1 1 calc R . . H26B H 0.7908 -0.1478 0.8596 0.108 Uiso 1 1 calc R . . C27 C 0.8927(9) -0.1467(7) 0.9244(9) 0.130(6) Uani 1 1 d . . . H27A H 0.9299 -0.1592 0.8858 0.156 Uiso 1 1 calc R . . H27B H 0.8883 -0.1876 0.9538 0.156 Uiso 1 1 calc R . . C28 C 0.9331(7) -0.0875(6) 0.9608(6) 0.077(3) Uani 1 1 d . . . H28A H 0.9979 -0.0852 0.9528 0.093 Uiso 1 1 calc R . . H28B H 0.9225 -0.0916 1.0090 0.093 Uiso 1 1 calc R . . C29 C 0.8861(6) -0.0235(4) 0.9325(5) 0.060(2) Uani 1 1 d . . . H29A H 0.8674 0.0080 0.9686 0.072 Uiso 1 1 calc R . . H29B H 0.9262 0.0021 0.9024 0.072 Uiso 1 1 calc R . . N1 N 0.6110(5) -0.0440(4) 0.8734(4) 0.0538(18) Uani 1 1 d . . . N2 N 0.7598(5) 0.0938(4) 0.8946(3) 0.0434(15) Uani 1 1 d . . . B3 B 0.7503(7) 0.1017(5) 0.7375(5) 0.045(2) Uani 1 1 d . . . B4 B 0.8324(6) 0.0313(4) 0.7457(5) 0.045(2) Uani 1 1 d . . . H4 H 0.8968 0.0384 0.7728 0.054 Uiso 1 1 calc R . . B5 B 0.7709(6) -0.0484(6) 0.7410(5) 0.043(2) Uani 1 1 d . . . H5 H 0.7919 -0.0969 0.7673 0.052 Uiso 1 1 calc R . . B6 B 0.6441(8) 0.0109(6) 0.6505(5) 0.051(2) Uani 1 1 d . . . H6 H 0.5817 0.0055 0.6206 0.061 Uiso 1 1 calc R . . B7 B 0.7041(8) 0.0911(6) 0.6543(5) 0.051(3) Uani 1 1 d . . . H7 H 0.6813 0.1377 0.6257 0.062 Uiso 1 1 calc R . . B8 B 0.8182(8) 0.0725(6) 0.6667(4) 0.050(2) Uani 1 1 d . . . H8 H 0.8716 0.1066 0.6458 0.060 Uiso 1 1 calc R . . B9 B 0.8312(8) -0.0212(5) 0.6709(5) 0.047(2) Uani 1 1 d . . . H9 H 0.8926 -0.0488 0.6537 0.056 Uiso 1 1 calc R . . B10 B 0.7216(7) -0.0599(7) 0.6596(5) 0.053(3) Uani 1 1 d . . . H10 H 0.7107 -0.1116 0.6356 0.063 Uiso 1 1 calc R . . B11 B 0.7518(9) 0.0176(6) 0.6119(6) 0.059(3) Uani 1 1 d . . . H11 H 0.7615 0.0161 0.5569 0.071 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ta1 0.0353(3) 0.0275(3) 0.0458(3) -0.00062(12) -0.00155(12) 0.00047(11) O1 0.064(4) 0.042(3) 0.065(4) 0.011(3) -0.019(3) 0.003(3) C1 0.040(4) 0.028(4) 0.075(6) -0.009(4) -0.009(4) 0.000(3) C2 0.049(5) 0.037(4) 0.054(5) -0.003(4) -0.005(4) 0.009(4) C11 0.042(4) 0.041(4) 0.071(5) -0.019(4) -0.005(4) 0.002(4) C12 0.046(5) 0.033(4) 0.094(7) 0.004(4) -0.005(4) -0.011(4) C13 0.087(7) 0.070(7) 0.075(7) 0.009(6) 0.012(5) -0.030(6) C14 0.058(6) 0.039(5) 0.064(5) -0.003(4) 0.031(5) -0.005(4) C15 0.061(5) 0.025(4) 0.042(4) 0.001(3) -0.008(3) 0.003(3) C16 0.074(6) 0.038(5) 0.044(4) 0.002(4) -0.005(4) 0.005(4) C17 0.116(8) 0.037(6) 0.048(6) -0.007(4) -0.004(5) 0.000(6) C18 0.134(10) 0.038(5) 0.062(6) -0.009(5) -0.026(6) -0.015(6) C19 0.081(7) 0.051(6) 0.070(6) 0.001(5) -0.024(5) -0.015(5) C20 0.059(5) 0.039(4) 0.050(5) 0.006(4) -0.017(4) 0.004(4) C21 0.056(5) 0.056(5) 0.074(6) 0.001(5) -0.009(5) -0.010(4) C22 0.091(8) 0.047(5) 0.073(7) -0.014(5) 0.022(5) 0.009(5) C23 0.076(5) 0.029(4) 0.054(5) 0.002(4) -0.010(4) -0.001(4) C24 0.100(8) 0.039(5) 0.140(11) -0.025(6) -0.012(7) 0.012(6) C25 0.162(11) 0.038(5) 0.068(7) 0.006(5) -0.004(7) -0.030(7) C26 0.112(9) 0.047(6) 0.112(9) 0.002(6) -0.033(8) 0.022(6) C27 0.100(10) 0.064(8) 0.227(18) 0.031(10) -0.064(11) 0.008(8) C28 0.068(6) 0.072(7) 0.093(7) 0.027(6) -0.021(5) 0.007(6) C29 0.049(5) 0.057(6) 0.076(7) 0.009(5) -0.018(5) -0.003(4) N1 0.051(4) 0.037(4) 0.074(5) 0.002(3) 0.006(4) -0.013(3) N2 0.052(4) 0.036(4) 0.042(4) -0.001(3) 0.002(3) 0.005(3) B3 0.053(5) 0.034(5) 0.047(5) 0.001(4) 0.002(4) 0.005(4) B4 0.039(5) 0.035(5) 0.061(6) -0.003(4) -0.004(4) -0.006(4) B5 0.043(5) 0.037(5) 0.050(6) 0.000(4) 0.004(4) 0.010(4) B6 0.056(7) 0.049(6) 0.048(6) 0.002(4) -0.012(4) 0.011(5) B7 0.060(6) 0.040(6) 0.055(6) 0.002(4) -0.007(4) 0.003(5) B8 0.059(7) 0.042(6) 0.049(5) -0.002(4) -0.003(4) -0.005(5) B9 0.044(6) 0.042(6) 0.053(6) -0.012(4) 0.000(4) 0.004(4) B10 0.051(7) 0.051(7) 0.056(7) -0.009(4) -0.003(4) 0.006(5) B11 0.079(7) 0.061(7) 0.037(6) -0.010(5) -0.006(5) 0.003(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1 N2 1.806(7) . ? Ta1 C14 2.176(9) . ? Ta1 O1 2.229(6) . ? Ta1 N1 2.232(7) . ? Ta1 B4 2.427(10) . ? Ta1 B5 2.466(10) . ? Ta1 B3 2.477(10) . ? Ta1 C2 2.506(8) . ? Ta1 C1 2.548(9) . ? O1 C26 1.446(12) . ? O1 C29 1.454(11) . ? C1 C11 1.528(12) . ? C1 C2 1.596(10) . ? C1 B5 1.666(13) . ? C1 B10 1.721(13) . ? C1 B6 1.717(13) . ? C2 B3 1.694(13) . ? C2 B6 1.725(13) . ? C2 B7 1.736(13) . ? C11 C12 1.513(12) . ? C12 N1 1.503(11) . ? C13 N1 1.449(12) . ? C14 N1 1.461(10) . ? C15 N2 1.385(10) . ? C15 C20 1.406(11) . ? C15 C16 1.417(12) . ? C16 C17 1.377(12) . ? C16 C22 1.489(13) . ? C17 C18 1.387(14) . ? C18 C19 1.353(14) . ? C19 C20 1.417(12) . ? C20 C21 1.490(12) . ? C23 C24 1.505(13) . ? C23 C25 1.524(13) . ? C23 B3 1.644(12) . ? C26 C27 1.417(15) . ? C27 C28 1.462(16) . ? C28 C29 1.505(12) . ? B3 B7 1.795(14) . ? B3 B8 1.810(14) . ? B3 B4 1.808(13) . ? B4 B8 1.762(14) . ? B4 B5 1.764(13) . ? B4 B9 1.784(13) . ? B5 B9 1.728(14) . ? B5 B10 1.783(14) . ? B6 B7 1.760(16) . ? B6 B11 1.768(17) . ? B6 B10 1.771(15) . ? B7 B8 1.738(16) . ? B7 B11 1.771(16) . ? B8 B9 1.787(16) . ? B8 B11 1.793(15) . ? B9 B10 1.790(17) . ? B9 B11 1.811(15) . ? B10 B11 1.802(17) . ? 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 Ta1 C14 98.3(3) . . ? N2 Ta1 O1 87.7(3) . . ? C14 Ta1 O1 116.6(3) . . ? N2 Ta1 N1 116.2(3) . . ? C14 Ta1 N1 38.7(3) . . ? O1 Ta1 N1 82.4(3) . . ? N2 Ta1 B4 103.8(3) . . ? C14 Ta1 B4 143.9(4) . . ? O1 Ta1 B4 92.7(3) . . ? N1 Ta1 B4 139.4(3) . . ? N2 Ta1 B5 143.8(3) . . ? C14 Ta1 B5 117.2(3) . . ? O1 Ta1 B5 83.1(3) . . ? N1 Ta1 B5 97.3(3) . . ? B4 Ta1 B5 42.2(3) . . ? N2 Ta1 B3 92.1(3) . . ? C14 Ta1 B3 108.6(4) . . ? O1 Ta1 B3 134.4(3) . . ? N1 Ta1 B3 136.1(3) . . ? B4 Ta1 B3 43.3(3) . . ? B5 Ta1 B3 70.7(4) . . ? N2 Ta1 C2 120.9(3) . . ? C14 Ta1 C2 77.3(4) . . ? O1 Ta1 C2 147.4(2) . . ? N1 Ta1 C2 96.6(3) . . ? B4 Ta1 C2 67.0(3) . . ? B5 Ta1 C2 64.6(3) . . ? B3 Ta1 C2 39.7(3) . . ? N2 Ta1 C1 157.5(3) . . ? C14 Ta1 C1 81.3(4) . . ? O1 Ta1 C1 112.8(2) . . ? N1 Ta1 C1 77.4(3) . . ? B4 Ta1 C1 67.5(3) . . ? B5 Ta1 C1 38.8(3) . . ? B3 Ta1 C1 67.1(3) . . ? C2 Ta1 C1 36.8(2) . . ? C26 O1 C29 108.6(7) . . ? C26 O1 Ta1 132.2(6) . . ? C29 O1 Ta1 119.1(5) . . ? C11 C1 C2 118.0(7) . . ? C11 C1 B5 125.7(7) . . ? C2 C1 B5 109.1(6) . . ? C11 C1 B10 116.3(7) . . ? C2 C1 B10 112.3(7) . . ? B5 C1 B10 63.5(6) . . ? C11 C1 B6 111.6(7) . . ? C2 C1 B6 62.6(5) . . ? B5 C1 B6 113.1(7) . . ? B10 C1 B6 62.0(6) . . ? C11 C1 Ta1 103.6(6) . . ? C2 C1 Ta1 70.2(4) . . ? B5 C1 Ta1 67.9(4) . . ? B10 C1 Ta1 129.1(5) . . ? B6 C1 Ta1 130.2(5) . . ? C1 C2 B3 115.1(6) . . ? C1 C2 B6 62.1(6) . . ? B3 C2 B6 115.7(7) . . ? C1 C2 B7 111.0(7) . . ? B3 C2 B7 63.1(6) . . ? B6 C2 B7 61.1(6) . . ? C1 C2 Ta1 73.0(4) . . ? B3 C2 Ta1 69.2(4) . . ? B6 C2 Ta1 132.4(5) . . ? B7 C2 Ta1 128.7(6) . . ? C12 C11 C1 116.9(7) . . ? N1 C12 C11 113.5(7) . . ? N1 C14 Ta1 72.7(5) . . ? N2 C15 C20 121.8(7) . . ? N2 C15 C16 119.0(7) . . ? C20 C15 C16 119.2(7) . . ? C17 C16 C15 119.7(9) . . ? C17 C16 C22 119.1(9) . . ? C15 C16 C22 121.2(8) . . ? C16 C17 C18 120.9(10) . . ? C19 C18 C17 120.4(9) . . ? C18 C19 C20 121.0(9) . . ? C15 C20 C19 118.7(8) . . ? C15 C20 C21 123.1(7) . . ? C19 C20 C21 118.1(8) . . ? C24 C23 C25 110.5(8) . . ? C24 C23 B3 113.1(8) . . ? C25 C23 B3 112.8(8) . . ? C27 C26 O1 106.3(11) . . ? C26 C27 C28 108.1(11) . . ? C27 C28 C29 104.2(8) . . ? O1 C29 C28 106.0(7) . . ? C13 N1 C14 114.2(8) . . ? C13 N1 C12 111.1(7) . . ? C14 N1 C12 115.4(7) . . ? C13 N1 Ta1 127.6(6) . . ? C14 N1 Ta1 68.6(4) . . ? C12 N1 Ta1 113.4(5) . . ? C15 N2 Ta1 176.3(6) . . ? C23 B3 C2 120.2(8) . . ? C23 B3 B7 111.4(7) . . ? C2 B3 B7 59.6(6) . . ? C23 B3 B8 122.2(8) . . ? C2 B3 B8 102.0(7) . . ? B7 B3 B8 57.6(6) . . ? C23 B3 B4 134.1(8) . . ? C2 B3 B4 102.0(6) . . ? B7 B3 B4 104.8(7) . . ? B8 B3 B4 58.3(5) . . ? C23 B3 Ta1 108.6(6) . . ? C2 B3 Ta1 71.1(4) . . ? B7 B3 Ta1 127.2(6) . . ? B8 B3 Ta1 122.0(6) . . ? B4 B3 Ta1 66.9(4) . . ? B8 B4 B5 105.7(7) . . ? B8 B4 B9 60.5(6) . . ? B5 B4 B9 58.3(5) . . ? B8 B4 B3 60.9(6) . . ? B5 B4 B3 106.3(7) . . ? B9 B4 B3 109.3(7) . . ? B8 B4 Ta1 127.1(6) . . ? B5 B4 Ta1 70.0(4) . . ? B9 B4 Ta1 126.0(6) . . ? B3 B4 Ta1 69.8(4) . . ? C1 B5 B9 107.4(7) . . ? C1 B5 B4 107.5(7) . . ? B9 B5 B4 61.4(6) . . ? C1 B5 B10 59.7(5) . . ? B9 B5 B10 61.3(6) . . ? B4 B5 B10 111.3(8) . . ? C1 B5 Ta1 73.3(4) . . ? B9 B5 Ta1 126.8(6) . . ? B4 B5 Ta1 67.7(5) . . ? B10 B5 Ta1 130.6(6) . . ? C1 B6 C2 55.2(5) . . ? C1 B6 B7 104.4(7) . . ? C2 B6 B7 59.7(6) . . ? C1 B6 B11 105.9(7) . . ? C2 B6 B11 105.7(7) . . ? B7 B6 B11 60.3(6) . . ? C1 B6 B10 59.1(5) . . ? C2 B6 B10 104.0(7) . . ? B7 B6 B10 108.9(8) . . ? B11 B6 B10 61.2(6) . . ? B8 B7 C2 103.4(7) . . ? B8 B7 B6 108.5(8) . . ? C2 B7 B6 59.1(6) . . ? B8 B7 B11 61.4(7) . . ? C2 B7 B11 105.2(8) . . ? B6 B7 B11 60.1(7) . . ? B8 B7 B3 61.6(6) . . ? C2 B7 B3 57.3(5) . . ? B6 B7 B3 109.1(7) . . ? B11 B7 B3 111.8(8) . . ? B7 B8 B4 109.3(8) . . ? B7 B8 B9 108.2(8) . . ? B4 B8 B9 60.4(5) . . ? B7 B8 B11 60.2(6) . . ? B4 B8 B11 110.3(7) . . ? B9 B8 B11 60.8(6) . . ? B7 B8 B3 60.8(6) . . ? B4 B8 B3 60.8(5) . . ? B9 B8 B3 109.0(7) . . ? B11 B8 B3 110.1(8) . . ? B5 B9 B4 60.3(5) . . ? B5 B9 B8 106.2(7) . . ? B4 B9 B8 59.1(5) . . ? B5 B9 B10 60.9(6) . . ? B4 B9 B10 110.0(7) . . ? B8 B9 B10 107.6(8) . . ? B5 B9 B11 107.8(8) . . ? B4 B9 B11 108.4(7) . . ? B8 B9 B11 59.8(6) . . ? B10 B9 B11 60.0(7) . . ? C1 B10 B6 58.9(6) . . ? C1 B10 B5 56.8(5) . . ? B6 B10 B5 105.2(7) . . ? C1 B10 B9 102.3(7) . . ? B6 B10 B9 106.6(9) . . ? B5 B10 B9 57.8(5) . . ? C1 B10 B11 104.3(8) . . ? B6 B10 B11 59.3(7) . . ? B5 B10 B11 105.9(8) . . ? B9 B10 B11 60.6(6) . . ? B6 B11 B7 59.6(7) . . ? B6 B11 B8 105.7(8) . . ? B7 B11 B8 58.4(6) . . ? B6 B11 B10 59.5(6) . . ? B7 B11 B10 107.1(8) . . ? B8 B11 B10 106.9(7) . . ? B6 B11 B9 105.8(8) . . ? B7 B11 B9 105.7(7) . . ? B8 B11 B9 59.4(6) . . ? B10 B11 B9 59.4(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.419 _refine_diff_density_min -2.184 _refine_diff_density_rms 0.186 _database_code_depnum_ccdc_archive 'CCDC 943871' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30.50 H51 B9 N3 Ta' _chemical_formula_weight 737.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8958(7) _cell_length_b 10.8119(9) _cell_length_c 18.1883(14) _cell_angle_alpha 92.057(2) _cell_angle_beta 100.2410(10) _cell_angle_gamma 90.5130(10) _cell_volume 1720.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 363 _cell_measurement_theta_min 15 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 746 _exptl_absorpt_coefficient_mu 3.221 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5920 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _diffrn_measurement_method 'PHI & OMEGA SCAN' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24003 _diffrn_reflns_av_R_equivalents 0.0680 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.25 _reflns_number_total 6161 _reflns_number_gt 5803 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_cell_refinement 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_data_reduction 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SIEMENS SHELXTL' _computing_publication_material 'SIEMENS SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+0.9875P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6161 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0920 _refine_ls_wR_factor_gt 0.0874 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ta1 Ta 0.974275(14) 0.714005(12) 0.748773(8) 0.03221(8) Uani 1 1 d . . . N1 N 1.2283(4) 0.6753(3) 0.7839(2) 0.0423(8) Uani 1 1 d . . . N2 N 0.9422(4) 0.7963(3) 0.8314(2) 0.0406(8) Uani 1 1 d . . . N3 N 1.0611(4) 0.8558(3) 0.68570(19) 0.0371(8) Uani 1 1 d . . . C1 C 0.9991(5) 0.4785(4) 0.7476(3) 0.0418(9) Uani 1 1 d . . . C2 C 0.9592(5) 0.5114(4) 0.6623(2) 0.0417(9) Uani 1 1 d . . . H2 H 1.0517 0.5275 0.6307 0.050 Uiso 1 1 calc R . . C11 C 1.1619(5) 0.4540(4) 0.7845(3) 0.0530(11) Uani 1 1 d . . . H11A H 1.1614 0.3854 0.8174 0.064 Uiso 1 1 calc R . . H11B H 1.2197 0.4290 0.7461 0.064 Uiso 1 1 calc R . . C12 C 1.2414(5) 0.5622(4) 0.8285(3) 0.0517(12) Uani 1 1 d . . . H12A H 1.1972 0.5773 0.8730 0.062 Uiso 1 1 calc R . . H12B H 1.3485 0.5435 0.8443 0.062 Uiso 1 1 calc R . . C13 C 1.3130(5) 0.6544(5) 0.7199(3) 0.0587(13) Uani 1 1 d . . . H13A H 1.4185 0.6392 0.7392 0.088 Uiso 1 1 calc R . . H13B H 1.3053 0.7264 0.6902 0.088 Uiso 1 1 calc R . . H13C H 1.2691 0.5842 0.6895 0.088 Uiso 1 1 calc R . . C14 C 1.3116(6) 0.7770(5) 0.8315(4) 0.0648(15) Uani 1 1 d . . . H14A H 1.4174 0.7563 0.8447 0.097 Uiso 1 1 calc R . . H14B H 1.2687 0.7885 0.8761 0.097 Uiso 1 1 calc R . . H14C H 1.3026 0.8520 0.8045 0.097 Uiso 1 1 calc R . . C15 C 0.7618(5) 0.6750(5) 0.5648(3) 0.0537(11) Uani 1 1 d . . . H15A H 0.8283 0.7488 0.5738 0.064 Uiso 1 1 calc R . . C16 C 0.5984(6) 0.7202(7) 0.5536(4) 0.0787(18) Uani 1 1 d . . . H16A H 0.5782 0.7677 0.5094 0.118 Uiso 1 1 calc R . . H16B H 0.5844 0.7711 0.5962 0.118 Uiso 1 1 calc R . . H16C H 0.5293 0.6504 0.5482 0.118 Uiso 1 1 calc R . . C17 C 0.7896(9) 0.6124(7) 0.4910(3) 0.0803(18) Uani 1 1 d . . . H17A H 0.7624 0.6680 0.4510 0.120 Uiso 1 1 calc R . . H17B H 0.7280 0.5382 0.4806 0.120 Uiso 1 1 calc R . . H17C H 0.8955 0.5918 0.4954 0.120 Uiso 1 1 calc R . . C18 C 0.8800(5) 0.8459(4) 0.8908(3) 0.0459(10) Uani 1 1 d . . . C19 C 0.7591(6) 0.9283(5) 0.8771(3) 0.0558(12) Uani 1 1 d . . . C20 C 0.6963(8) 0.9764(6) 0.9372(4) 0.0792(18) Uani 1 1 d . . . H20A H 0.6130 1.0286 0.9282 0.095 Uiso 1 1 calc R . . C21 C 0.7557(9) 0.9479(6) 1.0089(4) 0.083(2) Uani 1 1 d . . . H21A H 0.7156 0.9833 1.0484 0.100 Uiso 1 1 calc R . . C22 C 0.8749(8) 0.8668(6) 1.0229(3) 0.0776(17) Uani 1 1 d . . . H22A H 0.9133 0.8470 1.0719 0.093 Uiso 1 1 calc R . . C23 C 0.9380(7) 0.8149(5) 0.9660(3) 0.0586(13) Uani 1 1 d . . . C24 C 1.0641(8) 0.7251(7) 0.9841(3) 0.0787(18) Uani 1 1 d . . . H24A H 1.0873 0.7162 1.0372 0.118 Uiso 1 1 calc R . . H24B H 1.1532 0.7550 0.9669 0.118 Uiso 1 1 calc R . . H24C H 1.0330 0.6463 0.9599 0.118 Uiso 1 1 calc R . . C25 C 0.6956(7) 0.9656(7) 0.8003(4) 0.0767(18) Uani 1 1 d . . . H25A H 0.7500 0.9250 0.7655 0.115 Uiso 1 1 calc R . . H25B H 0.7063 1.0537 0.7975 0.115 Uiso 1 1 calc R . . H25C H 0.5894 0.9424 0.7883 0.115 Uiso 1 1 calc R . . C26 C 1.1695(5) 0.9409(4) 0.6625(2) 0.0400(9) Uani 1 1 d . . . C27 C 1.2210(6) 1.0447(4) 0.7097(3) 0.0486(11) Uani 1 1 d . . . C28 C 1.3315(6) 1.1203(5) 0.6895(3) 0.0589(13) Uani 1 1 d . . . H28A H 1.3685 1.1888 0.7199 0.071 Uiso 1 1 calc R . . C29 C 1.3871(6) 1.0959(5) 0.6252(3) 0.0649(15) Uani 1 1 d . . . H29A H 1.4623 1.1474 0.6128 0.078 Uiso 1 1 calc R . . C30 C 1.3333(6) 0.9961(5) 0.5787(3) 0.0586(13) Uani 1 1 d . . . H30A H 1.3713 0.9819 0.5347 0.070 Uiso 1 1 calc R . . C31 C 1.2228(6) 0.9160(4) 0.5963(3) 0.0502(11) Uani 1 1 d . . . C32 C 1.1623(8) 0.8106(6) 0.5435(3) 0.0751(18) Uani 1 1 d . . . H32A H 1.2158 0.8081 0.5021 0.113 Uiso 1 1 calc R . . H32B H 1.0553 0.8216 0.5255 0.113 Uiso 1 1 calc R . . H32C H 1.1769 0.7343 0.5691 0.113 Uiso 1 1 calc R . . C33 C 1.1558(8) 1.0759(5) 0.7794(3) 0.0646(14) Uani 1 1 d . . . H33A H 1.2054 1.1494 0.8039 0.097 Uiso 1 1 calc R . . H33B H 1.1727 1.0085 0.8126 0.097 Uiso 1 1 calc R . . H33C H 1.0482 1.0897 0.7659 0.097 Uiso 1 1 calc R . . C34 C 0.9173(5) 0.8655(4) 0.6762(2) 0.0441(10) Uani 1 1 d . . . C35 C 0.8279(7) 0.9669(5) 0.6367(3) 0.0662(14) Uani 1 1 d . . . H35A H 0.8867 1.0048 0.6039 0.099 Uiso 1 1 calc R . . H35B H 0.8049 1.0277 0.6726 0.099 Uiso 1 1 calc R . . H35C H 0.7345 0.9334 0.6079 0.099 Uiso 1 1 calc R . . C36 C 0.492(2) 0.7138(15) 0.0675(13) 0.124(8) Uani 0.50 1 d P . . H36A H 0.5718 0.7637 0.0540 0.187 Uiso 0.50 1 calc PR . . H36B H 0.5106 0.7045 0.1206 0.187 Uiso 0.50 1 calc PR . . H36C H 0.3955 0.7533 0.0527 0.187 Uiso 0.50 1 calc PR . . C37 C 0.4888(10) 0.6115(11) 0.0356(5) 0.110(3) Uani 1 1 d . . . C38 C 0.3911(9) 0.5134(12) 0.0408(5) 0.108(3) Uani 1 1 d . . . H38A H 0.3162 0.5250 0.0700 0.129 Uiso 1 1 calc R . . C39 C 0.3979(11) 0.4047(13) 0.0070(6) 0.126(4) Uani 1 1 d . . . H39 H 0.3293 0.3411 0.0114 0.151 Uiso 1 1 calc R . . B3 B 0.7995(5) 0.5946(5) 0.6390(3) 0.0423(11) Uani 1 1 d . . . B4 B 0.7288(5) 0.6073(5) 0.7264(3) 0.0459(11) Uani 1 1 d . . . H4 H 0.6549 0.6836 0.7384 0.055 Uiso 1 1 calc R . . B5 B 0.8637(7) 0.5296(5) 0.7935(3) 0.0461(13) Uani 1 1 d . . . H5 H 0.8863 0.5522 0.8540 0.055 Uiso 1 1 calc R . . B6 B 0.9314(7) 0.3593(5) 0.6839(4) 0.0572(14) Uani 1 1 d . . . H6 H 0.9988 0.2798 0.6700 0.069 Uiso 1 1 calc R . . B7 B 0.8025(7) 0.4309(6) 0.6164(3) 0.0579(14) Uani 1 1 d . . . H7 H 0.7849 0.3971 0.5577 0.069 Uiso 1 1 calc R . . B8 B 0.6519(6) 0.4897(5) 0.6576(3) 0.0538(13) Uani 1 1 d . . . H8 H 0.5341 0.4942 0.6265 0.065 Uiso 1 1 calc R . . B9 B 0.6928(7) 0.4536(6) 0.7531(4) 0.0552(14) Uani 1 1 d . . . H9 H 0.6009 0.4355 0.7848 0.066 Uiso 1 1 calc R . . B10 B 0.8667(7) 0.3735(5) 0.7688(4) 0.0545(13) Uani 1 1 d . . . H10 H 0.8914 0.3029 0.8112 0.065 Uiso 1 1 calc R . . B11 B 0.7381(8) 0.3455(6) 0.6850(5) 0.0719(19) Uani 1 1 d . . . H11 H 0.6765 0.2565 0.6721 0.086 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ta1 0.02639(11) 0.03473(12) 0.03499(12) -0.00071(7) 0.00433(7) 0.00276(7) N1 0.0294(17) 0.0410(19) 0.054(2) 0.0022(16) 0.0018(15) 0.0022(14) N2 0.0357(18) 0.0405(19) 0.045(2) -0.0019(15) 0.0046(15) 0.0059(15) N3 0.0421(19) 0.0317(17) 0.0383(19) 0.0019(14) 0.0093(15) 0.0021(14) C1 0.037(2) 0.038(2) 0.050(2) 0.0020(18) 0.0071(18) 0.0032(17) C2 0.042(2) 0.041(2) 0.043(2) -0.0055(18) 0.0095(18) 0.0002(18) C11 0.047(3) 0.043(2) 0.067(3) 0.008(2) 0.005(2) 0.011(2) C12 0.036(2) 0.050(3) 0.066(3) 0.015(2) -0.002(2) 0.0069(19) C13 0.033(2) 0.068(3) 0.079(4) 0.009(3) 0.020(2) 0.008(2) C14 0.037(2) 0.055(3) 0.093(4) 0.007(3) -0.014(3) -0.005(2) C15 0.046(3) 0.066(3) 0.045(3) 0.001(2) -0.003(2) 0.002(2) C16 0.053(3) 0.100(5) 0.083(4) 0.029(4) 0.008(3) 0.019(3) C17 0.102(5) 0.091(5) 0.045(3) -0.003(3) 0.004(3) 0.008(4) C18 0.047(2) 0.046(2) 0.045(2) -0.0122(19) 0.0142(19) -0.0063(19) C19 0.056(3) 0.051(3) 0.063(3) -0.010(2) 0.019(2) 0.003(2) C20 0.083(4) 0.073(4) 0.090(5) -0.014(3) 0.040(4) 0.014(3) C21 0.112(5) 0.077(4) 0.070(4) -0.019(3) 0.048(4) 0.000(4) C22 0.097(5) 0.088(4) 0.051(3) -0.014(3) 0.024(3) -0.003(4) C23 0.066(3) 0.064(3) 0.045(3) -0.012(2) 0.011(2) -0.012(3) C24 0.082(4) 0.110(5) 0.040(3) 0.005(3) -0.001(3) 0.019(4) C25 0.062(4) 0.084(4) 0.085(4) 0.007(3) 0.016(3) 0.037(3) C26 0.040(2) 0.037(2) 0.042(2) 0.0064(18) 0.0065(18) -0.0022(17) C27 0.055(3) 0.039(2) 0.050(3) 0.006(2) 0.000(2) 0.001(2) C28 0.064(3) 0.044(3) 0.063(3) 0.004(2) -0.004(3) -0.015(2) C29 0.059(3) 0.069(3) 0.065(3) 0.019(3) 0.003(3) -0.019(3) C30 0.053(3) 0.068(3) 0.059(3) 0.015(3) 0.017(2) -0.007(2) C31 0.052(3) 0.051(3) 0.048(3) 0.001(2) 0.008(2) -0.006(2) C32 0.090(5) 0.081(4) 0.058(3) -0.015(3) 0.028(3) -0.023(3) C33 0.080(4) 0.056(3) 0.056(3) -0.003(3) 0.007(3) -0.002(3) C34 0.045(2) 0.049(2) 0.037(2) 0.0006(19) 0.0023(18) 0.0057(19) C35 0.069(4) 0.058(3) 0.069(4) 0.012(3) 0.001(3) 0.014(3) C36 0.110(13) 0.068(9) 0.17(2) 0.010(11) -0.039(13) 0.001(9) C37 0.081(5) 0.145(9) 0.093(6) 0.037(6) -0.019(5) 0.003(5) C38 0.059(4) 0.177(10) 0.085(6) 0.058(6) -0.002(4) -0.011(6) C39 0.089(7) 0.183(11) 0.102(7) 0.054(7) -0.002(5) -0.026(7) B3 0.032(2) 0.050(3) 0.042(3) 0.000(2) 0.0016(19) 0.001(2) B4 0.026(2) 0.057(3) 0.054(3) 0.000(2) 0.005(2) -0.001(2) B5 0.047(3) 0.047(3) 0.046(3) 0.004(2) 0.013(2) -0.008(2) B6 0.059(3) 0.037(3) 0.074(4) -0.012(3) 0.010(3) 0.002(2) B7 0.065(4) 0.054(3) 0.050(3) -0.013(3) 0.003(3) -0.005(3) B8 0.038(3) 0.058(3) 0.061(3) -0.008(3) -0.001(2) -0.010(2) B9 0.045(3) 0.056(3) 0.068(4) 0.001(3) 0.020(3) -0.013(2) B10 0.056(3) 0.043(3) 0.062(3) 0.006(3) 0.006(3) -0.008(2) B11 0.058(4) 0.054(4) 0.098(5) -0.008(4) 0.003(4) -0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1 N2 1.787(4) . ? Ta1 C34 2.147(4) . ? Ta1 N3 2.163(3) . ? Ta1 N1 2.283(3) . ? Ta1 B4 2.423(5) . ? Ta1 B5 2.444(5) . ? Ta1 C1 2.557(4) . ? Ta1 B3 2.597(5) . ? Ta1 C2 2.639(4) . ? N1 C14 1.481(6) . ? N1 C12 1.485(6) . ? N1 C13 1.507(6) . ? N2 C18 1.393(5) . ? N3 C34 1.265(6) . ? N3 C26 1.454(5) . ? C1 C11 1.514(6) . ? C1 C2 1.583(6) . ? C1 B5 1.671(7) . ? C1 B10 1.731(7) . ? C1 B6 1.731(7) . ? C2 B3 1.685(6) . ? C2 B7 1.706(7) . ? C2 B6 1.731(7) . ? C11 C12 1.493(7) . ? C15 C16 1.519(7) . ? C15 C17 1.542(8) . ? C15 B3 1.619(7) . ? C18 C19 1.396(7) . ? C18 C23 1.426(7) . ? C19 C20 1.400(7) . ? C19 C25 1.483(8) . ? C20 C21 1.364(10) . ? C21 C22 1.376(10) . ? C22 C23 1.368(8) . ? C23 C24 1.490(8) . ? C26 C31 1.389(6) . ? C26 C27 1.411(7) . ? C27 C28 1.380(7) . ? C27 C33 1.514(8) . ? C28 C29 1.366(8) . ? C29 C30 1.375(8) . ? C30 C31 1.390(7) . ? C31 C32 1.495(8) . ? C34 C35 1.491(7) . ? C36 C37 1.229(19) . ? C37 C38 1.382(14) . ? C37 C39 1.384(14) 2_665 ? C38 C39 1.314(15) . ? C39 C37 1.384(14) 2_665 ? B3 B7 1.804(8) . ? B3 B4 1.810(7) . ? B3 B8 1.812(7) . ? B4 B9 1.790(8) . ? B4 B5 1.792(8) . ? B4 B8 1.794(8) . ? B5 B10 1.733(8) . ? B5 B9 1.750(8) . ? B6 B11 1.728(9) . ? B6 B7 1.734(9) . ? B6 B10 1.743(9) . ? B7 B11 1.751(10) . ? B7 B8 1.760(9) . ? B8 B9 1.770(9) . ? B8 B11 1.791(9) . ? B9 B10 1.763(9) . ? B9 B11 1.774(10) . ? B10 B11 1.750(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ta1 C34 95.24(16) . . ? N2 Ta1 N3 103.37(15) . . ? C34 Ta1 N3 34.14(15) . . ? N2 Ta1 N1 99.09(15) . . ? C34 Ta1 N1 116.40(15) . . ? N3 Ta1 N1 82.31(13) . . ? N2 Ta1 B4 94.82(17) . . ? C34 Ta1 B4 98.82(18) . . ? N3 Ta1 B4 129.91(16) . . ? N1 Ta1 B4 140.43(16) . . ? N2 Ta1 B5 88.44(18) . . ? C34 Ta1 B5 142.00(19) . . ? N3 Ta1 B5 167.47(18) . . ? N1 Ta1 B5 100.19(17) . . ? B4 Ta1 B5 43.20(19) . . ? N2 Ta1 C1 120.10(15) . . ? C34 Ta1 C1 142.16(16) . . ? N3 Ta1 C1 132.64(14) . . ? N1 Ta1 C1 73.63(13) . . ? B4 Ta1 C1 67.35(16) . . ? B5 Ta1 C1 38.95(17) . . ? N2 Ta1 B3 134.42(15) . . ? C34 Ta1 B3 81.39(16) . . ? N3 Ta1 B3 98.66(15) . . ? N1 Ta1 B3 123.25(14) . . ? B4 Ta1 B3 42.10(17) . . ? B5 Ta1 B3 69.62(19) . . ? C1 Ta1 B3 64.65(15) . . ? N2 Ta1 C2 151.79(15) . . ? C34 Ta1 C2 106.76(15) . . ? N3 Ta1 C2 104.75(13) . . ? N1 Ta1 C2 86.92(13) . . ? B4 Ta1 C2 65.01(16) . . ? B5 Ta1 C2 63.36(17) . . ? C1 Ta1 C2 35.44(14) . . ? B3 Ta1 C2 37.54(14) . . ? C14 N1 C12 107.7(4) . . ? C14 N1 C13 105.9(4) . . ? C12 N1 C13 108.2(4) . . ? C14 N1 Ta1 112.7(3) . . ? C12 N1 Ta1 107.5(2) . . ? C13 N1 Ta1 114.5(3) . . ? C18 N2 Ta1 165.2(3) . . ? C34 N3 C26 127.3(4) . . ? C34 N3 Ta1 72.2(3) . . ? C26 N3 Ta1 159.0(3) . . ? C11 C1 C2 121.1(4) . . ? C11 C1 B5 124.1(4) . . ? C2 C1 B5 110.5(4) . . ? C11 C1 B10 113.9(4) . . ? C2 C1 B10 110.3(4) . . ? B5 C1 B10 61.2(3) . . ? C11 C1 B6 110.1(4) . . ? C2 C1 B6 62.8(3) . . ? B5 C1 B6 111.5(4) . . ? B10 C1 B6 60.5(3) . . ? C11 C1 Ta1 105.8(3) . . ? C2 C1 Ta1 75.1(2) . . ? B5 C1 Ta1 66.9(2) . . ? B10 C1 Ta1 126.2(3) . . ? B6 C1 Ta1 134.4(3) . . ? C1 C2 B3 114.9(3) . . ? C1 C2 B7 111.9(4) . . ? B3 C2 B7 64.3(3) . . ? C1 C2 B6 62.8(3) . . ? B3 C2 B6 115.8(4) . . ? B7 C2 B6 60.6(3) . . ? C1 C2 Ta1 69.5(2) . . ? B3 C2 Ta1 69.9(2) . . ? B7 C2 Ta1 129.4(3) . . ? B6 C2 Ta1 129.2(3) . . ? C12 C11 C1 114.2(4) . . ? N1 C12 C11 111.4(4) . . ? C16 C15 C17 108.6(5) . . ? C16 C15 B3 110.7(4) . . ? C17 C15 B3 116.8(5) . . ? N2 C18 C19 119.8(4) . . ? N2 C18 C23 121.3(4) . . ? C19 C18 C23 119.0(4) . . ? C18 C19 C20 119.3(5) . . ? C18 C19 C25 121.5(4) . . ? C20 C19 C25 119.3(5) . . ? C21 C20 C19 120.8(6) . . ? C20 C21 C22 120.2(5) . . ? C23 C22 C21 121.3(6) . . ? C22 C23 C18 119.4(6) . . ? C22 C23 C24 119.0(5) . . ? C18 C23 C24 121.6(5) . . ? C31 C26 C27 122.1(4) . . ? C31 C26 N3 119.5(4) . . ? C27 C26 N3 118.4(4) . . ? C28 C27 C26 117.8(5) . . ? C28 C27 C33 120.2(5) . . ? C26 C27 C33 121.9(4) . . ? C29 C28 C27 120.8(5) . . ? C28 C29 C30 120.8(5) . . ? C29 C30 C31 121.1(5) . . ? C26 C31 C30 117.4(4) . . ? C26 C31 C32 122.5(4) . . ? C30 C31 C32 120.1(5) . . ? N3 C34 C35 125.3(5) . . ? N3 C34 Ta1 73.6(2) . . ? C35 C34 Ta1 160.0(4) . . ? C36 C37 C38 127.1(16) . . ? C36 C37 C39 114.0(15) . 2_665 ? C38 C37 C39 118.8(11) . 2_665 ? C39 C38 C37 123.8(10) . . ? C38 C39 C37 117.3(10) . 2_665 ? C15 B3 C2 124.2(4) . . ? C15 B3 B7 111.9(4) . . ? C2 B3 B7 58.4(3) . . ? C15 B3 B4 130.6(4) . . ? C2 B3 B4 102.4(3) . . ? B7 B3 B4 105.5(4) . . ? C15 B3 B8 117.5(4) . . ? C2 B3 B8 102.5(4) . . ? B7 B3 B8 58.2(3) . . ? B4 B3 B8 59.4(3) . . ? C15 B3 Ta1 112.5(3) . . ? C2 B3 Ta1 72.6(2) . . ? B7 B3 Ta1 126.6(3) . . ? B4 B3 Ta1 63.8(2) . . ? B8 B3 Ta1 120.2(3) . . ? B9 B4 B5 58.5(3) . . ? B9 B4 B8 59.2(3) . . ? B5 B4 B8 105.2(4) . . ? B9 B4 B3 107.5(4) . . ? B5 B4 B3 106.2(4) . . ? B8 B4 B3 60.4(3) . . ? B9 B4 Ta1 125.9(3) . . ? B5 B4 Ta1 69.0(2) . . ? B8 B4 Ta1 130.7(3) . . ? B3 B4 Ta1 74.1(2) . . ? C1 B5 B10 61.1(3) . . ? C1 B5 B9 107.3(4) . . ? B10 B5 B9 60.8(3) . . ? C1 B5 B4 105.9(4) . . ? B10 B5 B4 110.1(4) . . ? B9 B5 B4 60.7(3) . . ? C1 B5 Ta1 74.2(2) . . ? B10 B5 Ta1 133.1(4) . . ? B9 B5 Ta1 126.8(4) . . ? B4 B5 Ta1 67.8(2) . . ? B11 B6 C2 105.1(4) . . ? B11 B6 C1 106.1(4) . . ? C2 B6 C1 54.4(3) . . ? B11 B6 B7 60.8(4) . . ? C2 B6 B7 59.0(3) . . ? C1 B6 B7 103.8(4) . . ? B11 B6 B10 60.6(4) . . ? C2 B6 B10 103.2(4) . . ? C1 B6 B10 59.8(3) . . ? B7 B6 B10 108.5(4) . . ? C2 B7 B6 60.4(3) . . ? C2 B7 B11 105.2(4) . . ? B6 B7 B11 59.5(4) . . ? C2 B7 B8 103.8(4) . . ? B6 B7 B8 109.0(5) . . ? B11 B7 B8 61.4(4) . . ? C2 B7 B3 57.3(3) . . ? B6 B7 B3 109.8(4) . . ? B11 B7 B3 110.7(4) . . ? B8 B7 B3 61.1(3) . . ? B7 B8 B9 106.7(4) . . ? B7 B8 B11 59.1(4) . . ? B9 B8 B11 59.7(4) . . ? B7 B8 B4 108.1(4) . . ? B9 B8 B4 60.3(3) . . ? B11 B8 B4 108.4(4) . . ? B7 B8 B3 60.6(3) . . ? B9 B8 B3 108.3(4) . . ? B11 B8 B3 108.4(4) . . ? B4 B8 B3 60.3(3) . . ? B5 B9 B10 59.1(3) . . ? B5 B9 B8 108.0(4) . . ? B10 B9 B8 108.0(4) . . ? B5 B9 B11 106.8(4) . . ? B10 B9 B11 59.3(4) . . ? B8 B9 B11 60.7(4) . . ? B5 B9 B4 60.8(3) . . ? B10 B9 B4 108.8(4) . . ? B8 B9 B4 60.5(3) . . ? B11 B9 B4 109.4(4) . . ? C1 B10 B5 57.7(3) . . ? C1 B10 B6 59.8(3) . . ? B5 B10 B6 108.0(4) . . ? C1 B10 B11 105.1(4) . . ? B5 B10 B11 108.6(5) . . ? B6 B10 B11 59.3(4) . . ? C1 B10 B9 104.1(4) . . ? B5 B10 B9 60.1(3) . . ? B6 B10 B9 107.8(4) . . ? B11 B10 B9 60.6(4) . . ? B6 B11 B10 60.1(4) . . ? B6 B11 B7 59.8(4) . . ? B10 B11 B7 107.4(4) . . ? B6 B11 B9 108.0(4) . . ? B10 B11 B9 60.0(4) . . ? B7 B11 B9 106.9(5) . . ? B6 B11 B8 107.8(5) . . ? B10 B11 B8 107.7(4) . . ? B7 B11 B8 59.6(4) . . ? B9 B11 B8 59.5(4) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.678 _refine_diff_density_min -0.781 _refine_diff_density_rms 0.118 _database_code_depnum_ccdc_archive 'CCDC 943872' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H59 B9 N3 O0.25 Ta' _chemical_formula_weight 780.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.280(2) _cell_length_b 20.1642(18) _cell_length_c 20.6296(19) _cell_angle_alpha 90.00 _cell_angle_beta 111.047(2) _cell_angle_gamma 90.00 _cell_volume 8649.6(14) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 464 _cell_measurement_theta_min 15 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.198 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3184 _exptl_absorpt_coefficient_mu 2.566 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5141 _exptl_absorpt_correction_T_max 0.7387 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKE KAPPA APEXII DUO DIFFRACTOMETER' _diffrn_measurement_method 'PHI & OMEGA SCAN' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 78279 _diffrn_reflns_av_R_equivalents 0.1031 _diffrn_reflns_av_sigmaI/netI 0.0838 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 25.25 _reflns_number_total 15568 _reflns_number_gt 9596 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_cell_refinement 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_data_reduction 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SIEMENS SHELXTL' _computing_publication_material 'SIEMENS SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0913P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15568 _refine_ls_number_parameters 856 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.0875 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1701 _refine_ls_wR_factor_gt 0.1538 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ta1' Ta 0.516825(13) 0.784144(16) 0.820119(16) 0.03798(11) Uani 1 1 d . . . Ta1 Ta -0.017400(13) 0.785175(16) 0.294701(15) 0.03831(12) Uani 1 1 d . . . N1' N 0.5616(3) 0.7110(3) 0.9085(4) 0.0498(17) Uani 1 1 d . . . N2' N 0.5189(2) 0.8572(3) 0.8689(3) 0.0381(14) Uani 1 1 d . . . N3' N 0.4284(3) 0.7345(3) 0.8119(4) 0.0469(16) Uani 1 1 d . . . N1 N -0.0604(3) 0.7104(3) 0.3489(4) 0.0473(17) Uani 1 1 d . . . N2 N -0.0216(2) 0.8578(3) 0.3435(3) 0.0359(13) Uani 1 1 d . . . N3 N 0.0748(3) 0.7366(3) 0.3533(3) 0.0424(15) Uani 1 1 d . . . B3' B 0.5059(5) 0.7718(5) 0.6968(5) 0.049(2) Uani 1 1 d . . . H3' H 0.4534 0.7669 0.6719 0.059 Uiso 1 1 calc R . . B4' B 0.5475(5) 0.8470(5) 0.7350(5) 0.051(2) Uani 1 1 d . . . H4' H 0.5238 0.8950 0.7337 0.061 Uiso 1 1 calc R . . B5' B 0.6158(4) 0.8193(5) 0.8019(5) 0.047(2) Uani 1 1 d . . . H5' H 0.6389 0.8475 0.8502 0.056 Uiso 1 1 calc R . . B6' B 0.6261(5) 0.7048(5) 0.7267(6) 0.058(3) Uani 1 1 d . . . H6' H 0.6512 0.6585 0.7240 0.069 Uiso 1 1 calc R . . B7' B 0.5546(5) 0.7295(6) 0.6591(6) 0.058(3) Uani 1 1 d . . . H7' H 0.5334 0.6994 0.6119 0.069 Uiso 1 1 calc R . . B8' B 0.5525(5) 0.8156(6) 0.6571(5) 0.061(3) Uani 1 1 d . . . H8' H 0.5297 0.8414 0.6073 0.073 Uiso 1 1 calc R . . B9' B 0.6228(5) 0.8490(5) 0.7256(5) 0.060(3) Uani 1 1 d . . . H9' H 0.6460 0.8962 0.7216 0.072 Uiso 1 1 calc R . . B10' B 0.6675(6) 0.7786(6) 0.7699(7) 0.072(3) Uani 1 1 d . . . H10' H 0.7202 0.7800 0.7956 0.087 Uiso 1 1 calc R . . B11' B 0.6288(6) 0.7755(6) 0.6771(6) 0.068(3) Uani 1 1 d . . . H11' H 0.6562 0.7758 0.6421 0.082 Uiso 1 1 calc R . . C1' C 0.6166(4) 0.7377(5) 0.8016(4) 0.050(2) Uani 1 1 d . . . C2' C 0.5535(5) 0.7105(4) 0.7385(5) 0.059(3) Uani 1 1 d . . . H2' H 0.5327 0.6620 0.7433 0.071 Uiso 1 1 calc R . . C11' C 0.6501(4) 0.6960(5) 0.8643(5) 0.064(3) Uani 1 1 d . . . H11A H 0.6962 0.7007 0.8763 0.077 Uiso 1 1 calc R . . H11B H 0.6393 0.6498 0.8524 0.077 Uiso 1 1 calc R . . C12' C 0.6338(4) 0.7128(4) 0.9269(5) 0.059(2) Uani 1 1 d . . . H12A H 0.6499 0.7567 0.9435 0.070 Uiso 1 1 calc R . . H12B H 0.6542 0.6813 0.9638 0.070 Uiso 1 1 calc R . . C13' C 0.5396(4) 0.6399(4) 0.8910(5) 0.066(3) Uani 1 1 d . . . H13A H 0.5603 0.6122 0.9306 0.099 Uiso 1 1 calc R . . H13B H 0.5506 0.6251 0.8526 0.099 Uiso 1 1 calc R . . H13C H 0.4938 0.6375 0.8789 0.099 Uiso 1 1 calc R . . C14' C 0.5494(5) 0.7313(5) 0.9717(5) 0.073(3) Uani 1 1 d . . . H14A H 0.5687 0.6998 1.0082 0.110 Uiso 1 1 calc R . . H14B H 0.5039 0.7330 0.9617 0.110 Uiso 1 1 calc R . . H14C H 0.5678 0.7744 0.9863 0.110 Uiso 1 1 calc R . . C15' C 0.5247(3) 0.9234(4) 0.8946(4) 0.0399(17) Uani 1 1 d . . . C16' C 0.4747(4) 0.9690(4) 0.8637(5) 0.057(2) Uani 1 1 d . . . C17' C 0.4815(5) 1.0337(5) 0.8896(6) 0.071(3) Uani 1 1 d . . . H17A H 0.4489 1.0643 0.8692 0.085 Uiso 1 1 calc R . . C18' C 0.5345(5) 1.0534(5) 0.9440(6) 0.077(3) Uani 1 1 d . . . H18A H 0.5377 1.0963 0.9617 0.092 Uiso 1 1 calc R . . C19' C 0.5829(4) 1.0085(5) 0.9720(5) 0.065(2) Uani 1 1 d . . . H19A H 0.6192 1.0220 1.0089 0.078 Uiso 1 1 calc R . . C20' C 0.5806(4) 0.9437(4) 0.9479(4) 0.048(2) Uani 1 1 d . . . C21' C 0.6364(4) 0.8981(5) 0.9813(4) 0.057(2) Uani 1 1 d . . . H21A H 0.6264 0.8560 0.9558 0.069 Uiso 1 1 calc R . . C22' C 0.6465(5) 0.8826(6) 1.0574(5) 0.089(3) Uani 1 1 d . . . H22A H 0.6072 0.8661 1.0604 0.134 Uiso 1 1 calc R . . H22B H 0.6591 0.9223 1.0846 0.134 Uiso 1 1 calc R . . H22C H 0.6797 0.8498 1.0748 0.134 Uiso 1 1 calc R . . C23' C 0.6990(4) 0.9237(6) 0.9764(7) 0.105(4) Uani 1 1 d . . . H23A H 0.6928 0.9328 0.9288 0.158 Uiso 1 1 calc R . . H23B H 0.7320 0.8908 0.9943 0.158 Uiso 1 1 calc R . . H23C H 0.7117 0.9637 1.0032 0.158 Uiso 1 1 calc R . . C24' C 0.4136(4) 0.9500(5) 0.8044(5) 0.071(3) Uani 1 1 d . . . H24A H 0.4174 0.9026 0.7963 0.085 Uiso 1 1 calc R . . C25' C 0.3541(5) 0.9576(8) 0.8241(7) 0.128(5) Uani 1 1 d . . . H25A H 0.3597 0.9325 0.8654 0.192 Uiso 1 1 calc R . . H25B H 0.3170 0.9416 0.7868 0.192 Uiso 1 1 calc R . . H25C H 0.3481 1.0035 0.8324 0.192 Uiso 1 1 calc R . . C26' C 0.4065(6) 0.9844(10) 0.7369(7) 0.185(9) Uani 1 1 d . . . H26A H 0.4448 0.9778 0.7265 0.277 Uiso 1 1 calc R . . H26B H 0.3999 1.0310 0.7411 0.277 Uiso 1 1 calc R . . H26C H 0.3703 0.9662 0.7001 0.277 Uiso 1 1 calc R . . C27' C 0.3813(3) 0.6872(4) 0.8226(4) 0.0439(18) Uani 1 1 d . . . C28' C 0.3562(4) 0.7027(4) 0.8740(5) 0.049(2) Uani 1 1 d . . . C29' C 0.3139(4) 0.6569(5) 0.8842(6) 0.070(3) Uani 1 1 d . . . H29A H 0.2970 0.6645 0.9187 0.083 Uiso 1 1 calc R . . C30' C 0.2970(4) 0.6019(5) 0.8454(6) 0.078(3) Uani 1 1 d . . . H30A H 0.2668 0.5734 0.8519 0.094 Uiso 1 1 calc R . . C31' C 0.3226(4) 0.5868(5) 0.7970(5) 0.066(3) Uani 1 1 d . . . H31A H 0.3116 0.5471 0.7726 0.080 Uiso 1 1 calc R . . C32' C 0.3658(4) 0.6303(4) 0.7830(5) 0.056(2) Uani 1 1 d . . . C33' C 0.3940(4) 0.6128(5) 0.7284(5) 0.061(2) Uani 1 1 d . . . H33A H 0.4279 0.6447 0.7309 0.073 Uiso 1 1 calc R . . C34' C 0.4240(5) 0.5408(6) 0.7416(6) 0.095(4) Uani 1 1 d . . . H34A H 0.4574 0.5391 0.7866 0.143 Uiso 1 1 calc R . . H34B H 0.4416 0.5304 0.7066 0.143 Uiso 1 1 calc R . . H34C H 0.3911 0.5092 0.7395 0.143 Uiso 1 1 calc R . . C35' C 0.3411(6) 0.6158(7) 0.6548(5) 0.110(4) Uani 1 1 d . . . H35A H 0.3229 0.6595 0.6466 0.165 Uiso 1 1 calc R . . H35B H 0.3081 0.5841 0.6518 0.165 Uiso 1 1 calc R . . H35C H 0.3597 0.6056 0.6206 0.165 Uiso 1 1 calc R . . C36' C 0.3713(4) 0.7663(5) 0.9172(5) 0.061(3) Uani 1 1 d . . . H36A H 0.4070 0.7887 0.9092 0.073 Uiso 1 1 calc R . . C37' C 0.3905(5) 0.7544(8) 0.9953(6) 0.100(4) Uani 1 1 d . . . H37A H 0.4273 0.7256 1.0110 0.150 Uiso 1 1 calc R . . H37B H 0.3553 0.7341 1.0044 0.150 Uiso 1 1 calc R . . H37C H 0.4009 0.7959 1.0194 0.150 Uiso 1 1 calc R . . C38' C 0.3128(6) 0.8125(6) 0.8931(8) 0.109(4) Uani 1 1 d . . . H38A H 0.3007 0.8210 0.8442 0.163 Uiso 1 1 calc R . . H38B H 0.3234 0.8536 0.9181 0.163 Uiso 1 1 calc R . . H38C H 0.2775 0.7920 0.9018 0.163 Uiso 1 1 calc R . . C39' C 0.4170(4) 0.7784(4) 0.7666(4) 0.047(2) Uani 1 1 d . . . C40' C 0.3543(4) 0.7953(4) 0.7131(5) 0.066(3) Uani 1 1 d . . . H40A H 0.3213 0.7682 0.7194 0.099 Uiso 1 1 calc R . . H40B H 0.3559 0.7874 0.6679 0.099 Uiso 1 1 calc R . . H40C H 0.3449 0.8412 0.7173 0.099 Uiso 1 1 calc R . . C1 C -0.1153(4) 0.7383(5) 0.1983(4) 0.052(2) Uani 1 1 d . . . C2 C -0.1165(4) 0.8175(6) 0.1998(5) 0.069(3) Uani 1 1 d . . . H2 H -0.1406 0.8446 0.2299 0.083 Uiso 1 1 calc R . . C11 C -0.1508(4) 0.6940(5) 0.2353(4) 0.059(2) Uani 1 1 d . . . H11C H -0.1968 0.6997 0.2123 0.071 Uiso 1 1 calc R . . H11D H -0.1408 0.6478 0.2305 0.071 Uiso 1 1 calc R . . C12 C -0.1326(4) 0.7099(4) 0.3125(5) 0.057(2) Uani 1 1 d . . . H12C H -0.1499 0.7530 0.3176 0.068 Uiso 1 1 calc R . . H12D H -0.1513 0.6771 0.3339 0.068 Uiso 1 1 calc R . . C13 C -0.0379(4) 0.6391(4) 0.3474(5) 0.065(3) Uani 1 1 d . . . H13D H -0.0579 0.6108 0.3711 0.098 Uiso 1 1 calc R . . H13E H 0.0080 0.6370 0.3701 0.098 Uiso 1 1 calc R . . H13F H -0.0495 0.6248 0.3001 0.098 Uiso 1 1 calc R . . C14 C -0.0446(5) 0.7289(5) 0.4217(5) 0.075(3) Uani 1 1 d . . . H14D H -0.0630 0.6972 0.4439 0.112 Uiso 1 1 calc R . . H14E H -0.0617 0.7721 0.4243 0.112 Uiso 1 1 calc R . . H14F H 0.0013 0.7295 0.4448 0.112 Uiso 1 1 calc R . . C15 C -0.0275(3) 0.9209(4) 0.3675(4) 0.0415(18) Uani 1 1 d . . . C16 C 0.0231(4) 0.9677(4) 0.3845(4) 0.049(2) Uani 1 1 d . . . C17 C 0.0173(4) 1.0282(5) 0.4097(5) 0.064(3) Uani 1 1 d . . . H17B H 0.0519 1.0575 0.4212 0.077 Uiso 1 1 calc R . . C18 C -0.0381(4) 1.0476(5) 0.4188(5) 0.064(2) Uani 1 1 d . . . H18B H -0.0407 1.0893 0.4366 0.076 Uiso 1 1 calc R . . C19 C -0.0890(5) 1.0058(5) 0.4017(5) 0.064(2) Uani 1 1 d . . . H19B H -0.1269 1.0197 0.4067 0.077 Uiso 1 1 calc R . . C20 C -0.0853(3) 0.9408(4) 0.3762(4) 0.0454(19) Uani 1 1 d . . . C21 C -0.1430(4) 0.8945(5) 0.3587(5) 0.063(2) Uani 1 1 d . . . H21B H -0.1333 0.8531 0.3396 0.076 Uiso 1 1 calc R . . C22 C -0.1578(5) 0.8787(6) 0.4254(6) 0.099(4) Uani 1 1 d . . . H22D H -0.1210 0.8578 0.4591 0.148 Uiso 1 1 calc R . . H22E H -0.1941 0.8495 0.4139 0.148 Uiso 1 1 calc R . . H22F H -0.1672 0.9192 0.4444 0.148 Uiso 1 1 calc R . . C23 C -0.2029(4) 0.9276(6) 0.3038(7) 0.107(4) Uani 1 1 d . . . H23D H -0.1941 0.9369 0.2625 0.160 Uiso 1 1 calc R . . H23E H -0.2125 0.9683 0.3223 0.160 Uiso 1 1 calc R . . H23F H -0.2391 0.8982 0.2929 0.160 Uiso 1 1 calc R . . C24 C 0.0849(4) 0.9500(5) 0.3730(5) 0.068(3) Uani 1 1 d . . . H24B H 0.0849 0.9027 0.3623 0.081 Uiso 1 1 calc R . . C25 C 0.1441(4) 0.9662(7) 0.4373(6) 0.122(5) Uani 1 1 d . . . H25D H 0.1415 0.9428 0.4767 0.183 Uiso 1 1 calc R . . H25E H 0.1457 1.0130 0.4460 0.183 Uiso 1 1 calc R . . H25F H 0.1823 0.9529 0.4293 0.183 Uiso 1 1 calc R . . C26 C 0.0947(6) 0.9911(8) 0.3144(7) 0.133(6) Uani 1 1 d . . . H26D H 0.0594 0.9835 0.2717 0.200 Uiso 1 1 calc R . . H26E H 0.1341 0.9779 0.3090 0.200 Uiso 1 1 calc R . . H26F H 0.0968 1.0373 0.3259 0.200 Uiso 1 1 calc R . . C27 C 0.1229(4) 0.6907(4) 0.3991(4) 0.049(2) Uani 1 1 d . . . C28 C 0.1508(4) 0.7067(5) 0.4698(5) 0.056(2) Uani 1 1 d . . . C29 C 0.1947(5) 0.6618(5) 0.5117(5) 0.075(3) Uani 1 1 d . . . H29B H 0.2148 0.6703 0.5589 0.090 Uiso 1 1 calc R . . C30 C 0.2087(5) 0.6056(5) 0.4843(6) 0.077(3) Uani 1 1 d . . . H30B H 0.2370 0.5751 0.5135 0.093 Uiso 1 1 calc R . . C31 C 0.1826(4) 0.5926(5) 0.4158(5) 0.067(3) Uani 1 1 d . . . H31B H 0.1954 0.5549 0.3983 0.080 Uiso 1 1 calc R . . C32 C 0.1374(4) 0.6339(4) 0.3711(5) 0.054(2) Uani 1 1 d . . . C33 C 0.1074(4) 0.6153(5) 0.2943(5) 0.064(2) Uani 1 1 d . . . H33B H 0.0718 0.6459 0.2720 0.077 Uiso 1 1 calc R . . C34 C 0.0809(5) 0.5462(6) 0.2847(6) 0.096(4) Uani 1 1 d . . . H34D H 0.0499 0.5421 0.3070 0.145 Uiso 1 1 calc R . . H34E H 0.1152 0.5152 0.3049 0.145 Uiso 1 1 calc R . . H34F H 0.0605 0.5370 0.2360 0.145 Uiso 1 1 calc R . . C35 C 0.1549(5) 0.6226(6) 0.2595(6) 0.092(4) Uani 1 1 d . . . H35D H 0.1711 0.6672 0.2653 0.137 Uiso 1 1 calc R . . H35E H 0.1346 0.6130 0.2109 0.137 Uiso 1 1 calc R . . H35F H 0.1899 0.5923 0.2798 0.137 Uiso 1 1 calc R . . C36 C 0.1379(5) 0.7702(5) 0.5019(6) 0.073(3) Uani 1 1 d . . . H36B H 0.1033 0.7943 0.4665 0.088 Uiso 1 1 calc R . . C37 C 0.1150(6) 0.7534(8) 0.5636(6) 0.118(5) Uani 1 1 d . . . H37D H 0.0770 0.7264 0.5469 0.177 Uiso 1 1 calc R . . H37E H 0.1055 0.7938 0.5827 0.177 Uiso 1 1 calc R . . H37F H 0.1483 0.7298 0.5989 0.177 Uiso 1 1 calc R . . C38 C 0.1984(7) 0.8129(7) 0.5237(8) 0.120(5) Uani 1 1 d . . . H38D H 0.2105 0.8209 0.4841 0.181 Uiso 1 1 calc R . . H38E H 0.2327 0.7902 0.5588 0.181 Uiso 1 1 calc R . . H38F H 0.1902 0.8544 0.5417 0.181 Uiso 1 1 calc R . . C39 C 0.0837(4) 0.7840(4) 0.3184(5) 0.048(2) Uani 1 1 d . . . C40 C 0.1456(4) 0.8051(5) 0.3119(6) 0.067(3) Uani 1 1 d . . . H40D H 0.1803 0.7793 0.3429 0.101 Uiso 1 1 calc R . . H40E H 0.1530 0.8512 0.3236 0.101 Uiso 1 1 calc R . . H40F H 0.1433 0.7982 0.2650 0.101 Uiso 1 1 calc R . . B3 B -0.0479(5) 0.8468(5) 0.1877(5) 0.054(2) Uani 1 1 d . . . H3 H -0.0247 0.8948 0.2065 0.065 Uiso 1 1 calc R . . B4 B -0.0057(5) 0.7746(5) 0.1796(5) 0.051(3) Uani 1 1 d . . . H4 H 0.0468 0.7713 0.1941 0.061 Uiso 1 1 calc R . . B5 B -0.0516(5) 0.7095(4) 0.1870(5) 0.044(2) Uani 1 1 d . . . H5 H -0.0295 0.6618 0.2085 0.053 Uiso 1 1 calc R . . B6 B -0.1665(5) 0.7777(5) 0.1271(5) 0.060(3) Uani 1 1 d . . . H6 H -0.2192 0.7786 0.1113 0.072 Uiso 1 1 calc R . . B7 B -0.1238(5) 0.8456(6) 0.1177(6) 0.067(3) Uani 1 1 d . . . H7 H -0.1483 0.8920 0.0950 0.081 Uiso 1 1 calc R . . B8 B -0.0532(5) 0.8173(6) 0.1034(5) 0.065(3) Uani 1 1 d . . . H8 H -0.0308 0.8440 0.0716 0.078 Uiso 1 1 calc R . . B9 B -0.0563(5) 0.7313(6) 0.1028(5) 0.062(3) Uani 1 1 d . . . H9 H -0.0365 0.7017 0.0704 0.074 Uiso 1 1 calc R . . B10 B -0.1259(5) 0.7052(6) 0.1177(6) 0.061(3) Uani 1 1 d . . . H10 H -0.1508 0.6586 0.0964 0.074 Uiso 1 1 calc R . . B11 B -0.1292(6) 0.7765(6) 0.0657(6) 0.069(3) Uani 1 1 d . . . H11 H -0.1568 0.7774 0.0095 0.083 Uiso 1 1 calc R . . O1 O 0.8474(7) 0.9523(7) 0.9368(7) 0.111(7) Uani 0.50 1 d PD . . C41 C 0.8025(7) 0.9396(8) 0.8667(9) 0.069(5) Uani 0.50 1 d PDU . . H41A H 0.7585 0.9452 0.8641 0.083 Uiso 0.50 1 calc PR . . H41B H 0.8078 0.8949 0.8522 0.083 Uiso 0.50 1 calc PR . . C44 C 0.8908(7) 1.0069(8) 0.9466(8) 0.063(5) Uani 0.50 1 d PDU . . H44A H 0.9352 0.9922 0.9643 0.075 Uiso 0.50 1 calc PR . . H44B H 0.8846 1.0396 0.9780 0.075 Uiso 0.50 1 calc PR . . C42 C 0.8196(8) 0.9908(8) 0.8216(8) 0.076(5) Uani 0.50 1 d PDU . . H42A H 0.7821 1.0170 0.7957 0.092 Uiso 0.50 1 calc PR . . H42B H 0.8356 0.9691 0.7891 0.092 Uiso 0.50 1 calc PR . . C43 C 0.8719(8) 1.0348(8) 0.8722(8) 0.070(5) Uani 0.50 1 d PDU . . H43A H 0.8559 1.0798 0.8707 0.084 Uiso 0.50 1 calc PR . . H43B H 0.9093 1.0359 0.8586 0.084 Uiso 0.50 1 calc PR . . 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 Ta1' 0.03473(18) 0.0401(2) 0.0393(2) 0.00275(14) 0.01352(14) 0.00398(14) Ta1 0.03406(18) 0.0419(2) 0.0379(2) 0.00213(14) 0.01167(14) -0.00315(14) N1' 0.043(4) 0.056(5) 0.046(4) 0.011(3) 0.011(3) 0.000(3) N2' 0.027(3) 0.052(4) 0.035(3) 0.002(3) 0.010(2) 0.003(3) N3' 0.041(4) 0.045(4) 0.056(4) -0.003(3) 0.020(3) -0.004(3) N1 0.045(4) 0.045(4) 0.050(4) 0.008(3) 0.015(3) -0.004(3) N2 0.027(3) 0.044(4) 0.035(3) 0.003(3) 0.008(2) 0.000(3) N3 0.033(3) 0.047(4) 0.038(4) -0.008(3) 0.001(3) 0.003(3) B3' 0.059(6) 0.059(7) 0.040(5) 0.001(4) 0.032(5) -0.004(5) B4' 0.061(6) 0.052(6) 0.049(6) 0.007(5) 0.029(5) 0.011(5) B5' 0.039(5) 0.063(7) 0.041(5) -0.011(5) 0.017(4) -0.010(5) B6' 0.062(6) 0.053(7) 0.074(8) -0.011(5) 0.044(6) 0.001(5) B7' 0.058(6) 0.070(8) 0.049(6) -0.006(5) 0.024(5) 0.000(5) B8' 0.077(7) 0.069(8) 0.049(6) -0.001(5) 0.037(5) -0.008(6) B9' 0.086(7) 0.047(6) 0.064(7) -0.003(5) 0.047(6) -0.009(6) B10' 0.055(6) 0.098(10) 0.076(8) -0.014(7) 0.037(6) -0.007(6) B11' 0.065(7) 0.083(9) 0.073(8) -0.011(6) 0.044(6) -0.007(6) C1' 0.034(4) 0.065(6) 0.055(5) 0.004(4) 0.020(4) 0.002(4) C2' 0.070(6) 0.047(6) 0.078(7) -0.017(5) 0.048(5) -0.002(4) C11' 0.043(5) 0.074(7) 0.075(7) 0.018(5) 0.020(5) 0.019(5) C12' 0.045(5) 0.073(7) 0.042(5) 0.014(4) -0.004(4) 0.009(4) C13' 0.058(5) 0.052(6) 0.092(7) 0.028(5) 0.032(5) 0.010(5) C14' 0.070(6) 0.100(9) 0.056(6) 0.023(5) 0.030(5) 0.009(6) C15' 0.044(4) 0.031(4) 0.050(5) 0.001(3) 0.024(4) 0.003(4) C16' 0.062(5) 0.051(6) 0.066(6) 0.004(4) 0.032(5) 0.000(5) C17' 0.077(7) 0.041(6) 0.097(8) 0.008(5) 0.034(6) 0.020(5) C18' 0.091(7) 0.041(6) 0.095(8) -0.012(5) 0.030(6) -0.010(6) C19' 0.067(6) 0.058(6) 0.060(6) -0.003(5) 0.010(5) -0.013(5) C20' 0.051(5) 0.050(5) 0.046(5) -0.002(4) 0.021(4) -0.002(4) C21' 0.049(5) 0.072(7) 0.048(5) -0.006(4) 0.013(4) -0.011(5) C22' 0.107(8) 0.089(8) 0.068(7) 0.014(6) 0.027(6) 0.033(7) C23' 0.046(5) 0.139(12) 0.132(10) -0.007(9) 0.032(6) -0.020(7) C24' 0.067(6) 0.059(6) 0.074(7) -0.007(5) 0.009(5) 0.017(5) C25' 0.082(8) 0.175(15) 0.128(12) -0.053(10) 0.039(8) -0.049(9) C26' 0.087(9) 0.32(3) 0.099(11) 0.085(14) -0.029(8) -0.033(12) C27' 0.032(4) 0.032(4) 0.063(5) 0.005(4) 0.010(4) -0.002(3) C28' 0.035(4) 0.049(6) 0.063(6) 0.005(4) 0.018(4) 0.000(4) C29' 0.046(5) 0.068(7) 0.101(8) 0.004(6) 0.035(5) -0.008(5) C30' 0.055(6) 0.068(7) 0.115(9) 0.015(6) 0.036(6) -0.019(5) C31' 0.058(5) 0.057(6) 0.087(7) -0.007(5) 0.030(5) -0.022(5) C32' 0.033(4) 0.046(6) 0.075(6) 0.002(4) 0.001(4) 0.002(4) C33' 0.055(5) 0.067(7) 0.059(6) -0.009(5) 0.019(4) -0.006(5) C34' 0.105(9) 0.088(9) 0.104(9) -0.018(7) 0.051(7) 0.020(7) C35' 0.118(10) 0.145(12) 0.059(7) -0.009(7) 0.021(7) 0.024(9) C36' 0.043(5) 0.066(6) 0.079(7) -0.022(5) 0.028(5) -0.003(4) C37' 0.087(8) 0.155(12) 0.070(8) -0.015(8) 0.040(6) -0.034(8) C38' 0.089(9) 0.084(9) 0.161(13) -0.029(9) 0.053(9) 0.009(7) C39' 0.064(5) 0.035(5) 0.037(5) 0.004(4) 0.012(4) 0.016(4) C40' 0.061(6) 0.064(7) 0.061(6) 0.011(5) 0.007(5) -0.011(5) C1 0.041(4) 0.059(6) 0.053(5) -0.002(4) 0.015(4) -0.002(4) C2 0.052(5) 0.089(8) 0.060(6) -0.003(5) 0.013(4) 0.006(5) C11 0.039(4) 0.075(7) 0.055(6) -0.004(5) 0.007(4) -0.014(4) C12 0.053(5) 0.056(6) 0.069(6) 0.009(4) 0.031(5) -0.001(4) C13 0.061(5) 0.060(6) 0.086(7) 0.016(5) 0.039(5) -0.008(5) C14 0.098(8) 0.097(8) 0.044(5) -0.013(5) 0.043(5) -0.034(6) C15 0.041(4) 0.051(5) 0.033(4) 0.003(4) 0.014(3) -0.004(4) C16 0.055(5) 0.046(5) 0.050(5) -0.003(4) 0.022(4) 0.001(4) C17 0.061(6) 0.066(7) 0.063(6) -0.018(5) 0.019(5) -0.016(5) C18 0.069(6) 0.054(6) 0.065(6) -0.016(5) 0.021(5) -0.002(5) C19 0.068(6) 0.063(6) 0.067(6) 0.008(5) 0.031(5) 0.022(5) C20 0.045(4) 0.048(5) 0.044(5) 0.000(4) 0.017(4) -0.003(4) C21 0.048(5) 0.066(6) 0.083(7) 0.000(5) 0.034(5) -0.002(4) C22 0.089(8) 0.120(10) 0.109(9) -0.007(8) 0.063(7) -0.040(7) C23 0.049(6) 0.110(10) 0.135(11) 0.018(8) 0.001(6) -0.010(6) C24 0.050(5) 0.068(7) 0.091(7) -0.022(5) 0.033(5) -0.015(5) C25 0.042(6) 0.191(16) 0.107(10) -0.017(9) -0.005(6) 0.019(7) C26 0.095(9) 0.207(17) 0.123(11) 0.052(11) 0.068(8) 0.018(10) C27 0.035(4) 0.052(5) 0.050(5) 0.007(4) 0.005(4) 0.007(4) C28 0.044(5) 0.072(7) 0.048(5) -0.004(4) 0.010(4) 0.002(4) C29 0.065(6) 0.083(8) 0.061(6) 0.002(6) 0.004(5) 0.021(6) C30 0.059(6) 0.071(8) 0.077(8) 0.014(6) -0.005(5) 0.014(5) C31 0.051(5) 0.051(6) 0.080(7) -0.003(5) 0.003(5) 0.011(4) C32 0.047(4) 0.038(5) 0.070(6) -0.016(4) 0.012(4) -0.004(4) C33 0.065(6) 0.054(6) 0.065(6) -0.013(5) 0.013(5) 0.001(5) C34 0.101(9) 0.093(9) 0.089(8) -0.034(7) 0.027(7) -0.022(7) C35 0.107(9) 0.092(9) 0.083(8) -0.035(6) 0.043(7) -0.020(7) C36 0.071(7) 0.068(7) 0.067(7) -0.014(5) 0.009(5) 0.014(5) C37 0.107(10) 0.174(14) 0.070(8) -0.022(9) 0.027(7) 0.044(10) C38 0.131(12) 0.092(10) 0.125(12) -0.038(9) 0.028(9) -0.011(9) C39 0.038(4) 0.043(5) 0.061(6) 0.000(4) 0.013(4) -0.013(4) C40 0.047(5) 0.071(7) 0.089(8) 0.000(5) 0.029(5) -0.008(5) B3 0.056(6) 0.051(7) 0.054(6) -0.002(5) 0.018(5) -0.001(5) B4 0.049(5) 0.071(8) 0.037(5) -0.006(4) 0.019(4) -0.001(5) B5 0.053(5) 0.028(5) 0.046(5) -0.001(4) 0.011(4) 0.009(4) B6 0.045(5) 0.071(8) 0.048(6) 0.002(5) -0.001(4) 0.010(5) B7 0.067(7) 0.070(8) 0.054(7) 0.010(6) 0.010(5) 0.022(6) B8 0.067(7) 0.088(9) 0.041(6) 0.010(6) 0.020(5) 0.012(6) B9 0.059(6) 0.077(8) 0.043(6) -0.010(5) 0.012(5) -0.003(6) B10 0.060(6) 0.065(8) 0.048(6) -0.018(5) 0.006(5) -0.007(5) B11 0.071(7) 0.083(9) 0.047(6) -0.005(6) 0.012(5) 0.013(6) O1 0.165(15) 0.106(12) 0.124(13) 0.058(10) 0.127(13) 0.102(12) C41 0.055(8) 0.064(9) 0.099(9) -0.028(7) 0.040(7) 0.024(7) C44 0.055(7) 0.065(9) 0.078(9) -0.027(7) 0.037(7) 0.023(7) C42 0.080(9) 0.095(10) 0.055(8) 0.004(7) 0.025(7) 0.066(7) C43 0.076(8) 0.058(9) 0.100(9) 0.005(7) 0.062(7) 0.038(7) _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 Ta1' N2' 1.775(6) . ? Ta1' C39' 2.101(9) . ? Ta1' N3' 2.161(6) . ? Ta1' N1' 2.278(6) . ? Ta1' B4' 2.453(9) . ? Ta1' B5' 2.470(8) . ? Ta1' B3' 2.480(8) . ? Ta1' C1' 2.564(8) . ? Ta1' C2' 2.587(8) . ? Ta1 N2 1.799(6) . ? Ta1 C39 2.127(8) . ? Ta1 N3 2.204(6) . ? Ta1 N1 2.283(6) . ? Ta1 B3 2.408(10) . ? Ta1 C2 2.455(9) . ? Ta1 B4 2.489(9) . ? Ta1 C1 2.547(8) . ? Ta1 B5 2.575(9) . ? N1' C14' 1.484(11) . ? N1' C12' 1.514(10) . ? N1' C13' 1.515(10) . ? N2' C15' 1.425(9) . ? N3' C39' 1.245(9) . ? N3' C27' 1.493(10) . ? N1 C14 1.462(10) . ? N1 C12 1.510(11) . ? N1 C13 1.527(10) . ? N2 C15 1.389(9) . ? N3 C39 1.253(10) . ? N3 C27 1.473(10) . ? B3' C2' 1.655(14) . ? B3' B7' 1.766(13) . ? B3' B8' 1.772(13) . ? B3' B4' 1.804(15) . ? B4' B5' 1.738(14) . ? B4' B9' 1.757(13) . ? B4' B8' 1.768(13) . ? B5' C1' 1.646(14) . ? B5' B10' 1.730(13) . ? B5' B9' 1.744(13) . ? B6' C2' 1.724(12) . ? B6' C1' 1.763(13) . ? B6' B11' 1.770(16) . ? B6' B7' 1.771(16) . ? B6' B10' 1.808(16) . ? B7' C2' 1.693(14) . ? B7' B8' 1.736(16) . ? B7' B11' 1.814(15) . ? B8' B11' 1.792(16) . ? B8' B9' 1.821(16) . ? B9' B10' 1.785(17) . ? B9' B11' 1.819(15) . ? B10' C1' 1.712(13) . ? B10' B11' 1.796(18) . ? C1' C11' 1.498(12) . ? C1' C2' 1.631(13) . ? C11' C12' 1.502(13) . ? C15' C20' 1.395(10) . ? C15' C16' 1.408(11) . ? C16' C17' 1.399(12) . ? C16' C24' 1.515(12) . ? C17' C18' 1.365(13) . ? C18' C19' 1.366(13) . ? C19' C20' 1.393(12) . ? C20' C21' 1.499(11) . ? C21' C23' 1.525(11) . ? C21' C22' 1.536(12) . ? C24' C26' 1.513(16) . ? C24' C25' 1.528(14) . ? C27' C32' 1.378(11) . ? C27' C28' 1.402(11) . ? C28' C29' 1.388(11) . ? C28' C36' 1.528(12) . ? C29' C30' 1.341(14) . ? C30' C31' 1.351(13) . ? C31' C32' 1.405(11) . ? C32' C33' 1.517(12) . ? C33' C35' 1.553(13) . ? C33' C34' 1.579(14) . ? C36' C37' 1.530(14) . ? C36' C38' 1.534(14) . ? C39' C40' 1.475(12) . ? C1 C11 1.562(12) . ? C1 C2 1.599(14) . ? C1 B5 1.626(12) . ? C1 B6 1.701(13) . ? C1 B10 1.728(13) . ? C2 B6 1.714(14) . ? C2 B7 1.737(14) . ? C2 B3 1.738(13) . ? C11 C12 1.530(12) . ? C15 C16 1.413(10) . ? C15 C20 1.419(10) . ? C16 C17 1.350(11) . ? C16 C24 1.523(11) . ? C17 C18 1.371(12) . ? C18 C19 1.353(12) . ? C19 C20 1.426(12) . ? C20 C21 1.525(11) . ? C21 C23 1.558(13) . ? C21 C22 1.558(13) . ? C24 C25 1.532(13) . ? C24 C26 1.544(14) . ? C27 C32 1.372(11) . ? C27 C28 1.402(12) . ? C28 C29 1.385(12) . ? C28 C36 1.517(12) . ? C29 C30 1.352(13) . ? C30 C31 1.347(13) . ? C31 C32 1.375(11) . ? C32 C33 1.530(12) . ? C33 C35 1.485(13) . ? C33 C34 1.499(13) . ? C36 C38 1.526(16) . ? C36 C37 1.568(16) . ? C39 C40 1.495(11) . ? B3 B4 1.773(14) . ? B3 B7 1.787(14) . ? B3 B8 1.802(14) . ? B4 B5 1.703(14) . ? B4 B8 1.771(14) . ? B4 B9 1.806(14) . ? B5 B9 1.757(14) . ? B5 B10 1.758(14) . ? B6 B7 1.716(16) . ? B6 B11 1.747(16) . ? B6 B10 1.767(15) . ? B7 B11 1.736(16) . ? B7 B8 1.795(15) . ? B8 B9 1.734(17) . ? B8 B11 1.788(17) . ? B9 B10 1.765(15) . ? B9 B11 1.777(16) . ? B10 B11 1.779(16) . ? O1 C44 1.433(9) . ? O1 C41 1.455(9) . ? C41 C42 1.526(10) . ? C44 C43 1.544(10) . ? C42 C43 1.538(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2' Ta1' C39' 98.7(3) . . ? N2' Ta1' N3' 105.4(2) . . ? C39' Ta1' N3' 33.9(3) . . ? N2' Ta1' N1' 99.7(3) . . ? C39' Ta1' N1' 117.5(3) . . ? N3' Ta1' N1' 83.6(2) . . ? N2' Ta1' B4' 91.2(3) . . ? C39' Ta1' B4' 99.6(3) . . ? N3' Ta1' B4' 131.6(3) . . ? N1' Ta1' B4' 138.8(3) . . ? N2' Ta1' B5' 90.3(3) . . ? C39' Ta1' B5' 140.4(3) . . ? N3' Ta1' B5' 163.6(3) . . ? N1' Ta1' B5' 98.6(3) . . ? B4' Ta1' B5' 41.3(3) . . ? N2' Ta1' B3' 129.7(3) . . ? C39' Ta1' B3' 76.1(3) . . ? N3' Ta1' B3' 97.0(3) . . ? N1' Ta1' B3' 127.5(3) . . ? B4' Ta1' B3' 42.9(3) . . ? B5' Ta1' B3' 68.7(3) . . ? N2' Ta1' C1' 122.7(3) . . ? C39' Ta1' C1' 135.4(3) . . ? N3' Ta1' C1' 129.3(3) . . ? N1' Ta1' C1' 74.2(3) . . ? B4' Ta1' C1' 66.6(3) . . ? B5' Ta1' C1' 38.1(3) . . ? B3' Ta1' C1' 65.3(3) . . ? N2' Ta1' C2' 153.6(3) . . ? C39' Ta1' C2' 98.5(3) . . ? N3' Ta1' C2' 100.1(3) . . ? N1' Ta1' C2' 89.9(3) . . ? B4' Ta1' C2' 66.2(3) . . ? B5' Ta1' C2' 63.8(3) . . ? B3' Ta1' C2' 38.1(3) . . ? C1' Ta1' C2' 36.9(3) . . ? N2 Ta1 C39 98.3(3) . . ? N2 Ta1 N3 106.3(2) . . ? C39 Ta1 N3 33.6(3) . . ? N2 Ta1 N1 98.5(2) . . ? C39 Ta1 N1 118.4(3) . . ? N3 Ta1 N1 84.9(2) . . ? N2 Ta1 B3 92.2(3) . . ? C39 Ta1 B3 98.3(3) . . ? N3 Ta1 B3 129.2(3) . . ? N1 Ta1 B3 139.4(3) . . ? N2 Ta1 C2 91.0(3) . . ? C39 Ta1 C2 139.6(3) . . ? N3 Ta1 C2 161.8(3) . . ? N1 Ta1 C2 98.6(3) . . ? B3 Ta1 C2 41.9(3) . . ? N2 Ta1 B4 130.4(3) . . ? C39 Ta1 B4 75.7(3) . . ? N3 Ta1 B4 95.1(3) . . ? N1 Ta1 B4 128.1(3) . . ? B3 Ta1 B4 42.4(3) . . ? C2 Ta1 B4 68.6(3) . . ? N2 Ta1 C1 122.5(3) . . ? C39 Ta1 C1 135.6(3) . . ? N3 Ta1 C1 129.1(3) . . ? N1 Ta1 C1 75.2(3) . . ? B3 Ta1 C1 66.1(3) . . ? C2 Ta1 C1 37.2(3) . . ? B4 Ta1 C1 65.0(3) . . ? N2 Ta1 B5 155.1(3) . . ? C39 Ta1 B5 98.8(3) . . ? N3 Ta1 B5 98.0(3) . . ? N1 Ta1 B5 89.2(3) . . ? B3 Ta1 B5 67.4(3) . . ? C2 Ta1 B5 64.3(3) . . ? B4 Ta1 B5 39.3(3) . . ? C1 Ta1 B5 37.0(3) . . ? C14' N1' C12' 106.6(7) . . ? C14' N1' C13' 108.9(7) . . ? C12' N1' C13' 107.9(6) . . ? C14' N1' Ta1' 111.0(5) . . ? C12' N1' Ta1' 107.8(5) . . ? C13' N1' Ta1' 114.3(5) . . ? C15' N2' Ta1' 165.6(5) . . ? C39' N3' C27' 126.9(7) . . ? C39' N3' Ta1' 70.4(5) . . ? C27' N3' Ta1' 162.5(5) . . ? C14 N1 C12 109.5(7) . . ? C14 N1 C13 107.5(7) . . ? C12 N1 C13 106.5(6) . . ? C14 N1 Ta1 110.2(5) . . ? C12 N1 Ta1 108.6(5) . . ? C13 N1 Ta1 114.3(5) . . ? C15 N2 Ta1 167.5(5) . . ? C39 N3 C27 128.3(7) . . ? C39 N3 Ta1 69.8(5) . . ? C27 N3 Ta1 161.9(5) . . ? C2' B3' B7' 59.2(6) . . ? C2' B3' B8' 104.0(7) . . ? B7' B3' B8' 58.8(6) . . ? C2' B3' B4' 105.6(8) . . ? B7' B3' B4' 107.3(7) . . ? B8' B3' B4' 59.3(5) . . ? C2' B3' Ta1' 74.5(5) . . ? B7' B3' Ta1' 130.6(6) . . ? B8' B3' Ta1' 124.5(6) . . ? B4' B3' Ta1' 67.8(4) . . ? B5' B4' B9' 59.8(5) . . ? B5' B4' B8' 106.6(7) . . ? B9' B4' B8' 62.2(6) . . ? B5' B4' B3' 104.1(7) . . ? B9' B4' B3' 109.4(7) . . ? B8' B4' B3' 59.5(5) . . ? B5' B4' Ta1' 69.8(4) . . ? B9' B4' Ta1' 127.9(6) . . ? B8' B4' Ta1' 126.2(6) . . ? B3' B4' Ta1' 69.3(4) . . ? C1' B5' B10' 60.9(6) . . ? C1' B5' B4' 109.0(7) . . ? B10' B5' B4' 111.2(7) . . ? C1' B5' B9' 109.5(7) . . ? B10' B5' B9' 61.9(6) . . ? B4' B5' B9' 60.6(6) . . ? C1' B5' Ta1' 74.0(4) . . ? B10' B5' Ta1' 132.5(7) . . ? B4' B5' Ta1' 68.8(4) . . ? B9' B5' Ta1' 127.6(6) . . ? C2' B6' C1' 55.8(5) . . ? C2' B6' B11' 104.9(7) . . ? C1' B6' B11' 104.1(7) . . ? C2' B6' B7' 57.9(6) . . ? C1' B6' B7' 103.2(7) . . ? B11' B6' B7' 61.6(7) . . ? C2' B6' B10' 102.4(7) . . ? C1' B6' B10' 57.3(5) . . ? B11' B6' B10' 60.2(7) . . ? B7' B6' B10' 108.2(8) . . ? C2' B7' B8' 103.9(7) . . ? C2' B7' B3' 57.1(5) . . ? B8' B7' B3' 60.8(6) . . ? C2' B7' B6' 59.7(6) . . ? B8' B7' B6' 108.0(8) . . ? B3' B7' B6' 108.0(7) . . ? C2' B7' B11' 104.3(8) . . ? B8' B7' B11' 60.6(6) . . ? B3' B7' B11' 108.8(8) . . ? B6' B7' B11' 59.1(6) . . ? B7' B8' B4' 110.3(7) . . ? B7' B8' B3' 60.4(6) . . ? B4' B8' B3' 61.3(5) . . ? B7' B8' B11' 61.8(6) . . ? B4' B8' B11' 108.4(8) . . ? B3' B8' B11' 109.5(8) . . ? B7' B8' B9' 110.0(8) . . ? B4' B8' B9' 58.6(5) . . ? B3' B8' B9' 108.0(7) . . ? B11' B8' B9' 60.5(6) . . ? B5' B9' B4' 59.5(5) . . ? B5' B9' B10' 58.7(6) . . ? B4' B9' B10' 107.7(7) . . ? B5' B9' B11' 105.4(7) . . ? B4' B9' B11' 107.7(7) . . ? B10' B9' B11' 59.7(6) . . ? B5' B9' B8' 104.1(7) . . ? B4' B9' B8' 59.2(6) . . ? B10' B9' B8' 105.7(8) . . ? B11' B9' B8' 59.0(6) . . ? C1' B10' B5' 57.1(6) . . ? C1' B10' B9' 104.7(7) . . ? B5' B10' B9' 59.5(6) . . ? C1' B10' B11' 105.1(8) . . ? B5' B10' B11' 107.0(8) . . ? B9' B10' B11' 61.1(7) . . ? C1' B10' B6' 60.0(6) . . ? B5' B10' B6' 106.6(7) . . ? B9' B10' B6' 108.1(9) . . ? B11' B10' B6' 58.8(7) . . ? B6' B11' B8' 105.6(7) . . ? B6' B11' B10' 61.0(7) . . ? B8' B11' B10' 106.4(7) . . ? B6' B11' B7' 59.2(6) . . ? B8' B11' B7' 57.6(6) . . ? B10' B11' B7' 106.8(7) . . ? B6' B11' B9' 108.3(8) . . ? B8' B11' B9' 60.5(6) . . ? B10' B11' B9' 59.2(6) . . ? B7' B11' B9' 106.7(7) . . ? C11' C1' C2' 121.3(8) . . ? C11' C1' B5' 124.2(8) . . ? C2' C1' B5' 109.4(6) . . ? C11' C1' B10' 114.0(7) . . ? C2' C1' B10' 110.9(7) . . ? B5' C1' B10' 62.0(6) . . ? C11' C1' B6' 111.4(7) . . ? C2' C1' B6' 60.9(5) . . ? B5' C1' B6' 112.7(6) . . ? B10' C1' B6' 62.7(6) . . ? C11' C1' Ta1' 105.5(5) . . ? C2' C1' Ta1' 72.3(4) . . ? B5' C1' Ta1' 67.8(4) . . ? B10' C1' Ta1' 127.6(6) . . ? B6' C1' Ta1' 130.6(6) . . ? C1' C2' B3' 111.8(7) . . ? C1' C2' B7' 112.8(7) . . ? B3' C2' B7' 63.6(6) . . ? C1' C2' B6' 63.3(6) . . ? B3' C2' B6' 115.7(7) . . ? B7' C2' B6' 62.4(6) . . ? C1' C2' Ta1' 70.8(4) . . ? B3' C2' Ta1' 67.5(4) . . ? B7' C2' Ta1' 128.1(6) . . ? B6' C2' Ta1' 131.4(6) . . ? C1' C11' C12' 114.5(7) . . ? C11' C12' N1' 110.0(7) . . ? C20' C15' C16' 120.2(8) . . ? C20' C15' N2' 120.2(7) . . ? C16' C15' N2' 119.5(7) . . ? C17' C16' C15' 118.5(8) . . ? C17' C16' C24' 119.1(8) . . ? C15' C16' C24' 122.4(8) . . ? C18' C17' C16' 122.0(9) . . ? C17' C18' C19' 118.2(9) . . ? C18' C19' C20' 123.3(9) . . ? C19' C20' C15' 117.6(8) . . ? C19' C20' C21' 119.6(8) . . ? C15' C20' C21' 122.7(8) . . ? C20' C21' C23' 112.9(8) . . ? C20' C21' C22' 112.8(7) . . ? C23' C21' C22' 109.5(8) . . ? C26' C24' C16' 113.3(9) . . ? C26' C24' C25' 112.6(10) . . ? C16' C24' C25' 112.0(9) . . ? C32' C27' C28' 123.4(7) . . ? C32' C27' N3' 119.0(7) . . ? C28' C27' N3' 117.6(7) . . ? C29' C28' C27' 116.3(8) . . ? C29' C28' C36' 119.3(8) . . ? C27' C28' C36' 124.3(7) . . ? C30' C29' C28' 121.4(9) . . ? C29' C30' C31' 121.7(9) . . ? C30' C31' C32' 120.8(9) . . ? C27' C32' C31' 116.3(9) . . ? C27' C32' C33' 123.4(8) . . ? C31' C32' C33' 120.2(8) . . ? C32' C33' C35' 110.2(8) . . ? C32' C33' C34' 110.4(8) . . ? C35' C33' C34' 109.2(9) . . ? C28' C36' C37' 113.7(9) . . ? C28' C36' C38' 109.7(8) . . ? C37' C36' C38' 108.7(9) . . ? N3' C39' C40' 127.5(8) . . ? N3' C39' Ta1' 75.6(5) . . ? C40' C39' Ta1' 156.8(7) . . ? C11 C1 C2 123.2(7) . . ? C11 C1 B5 119.2(8) . . ? C2 C1 B5 112.4(7) . . ? C11 C1 B6 112.9(7) . . ? C2 C1 B6 62.5(6) . . ? B5 C1 B6 113.1(7) . . ? C11 C1 B10 109.4(7) . . ? C2 C1 B10 114.0(7) . . ? B5 C1 B10 63.2(6) . . ? B6 C1 B10 62.1(6) . . ? C11 C1 Ta1 105.8(5) . . ? C2 C1 Ta1 68.3(4) . . ? B5 C1 Ta1 72.4(4) . . ? B6 C1 Ta1 128.4(6) . . ? B10 C1 Ta1 132.6(6) . . ? C1 C2 B6 61.7(6) . . ? C1 C2 B7 107.6(7) . . ? B6 C2 B7 59.6(6) . . ? C1 C2 B3 108.3(7) . . ? B6 C2 B3 111.2(7) . . ? B7 C2 B3 61.9(6) . . ? C1 C2 Ta1 74.5(4) . . ? B6 C2 Ta1 133.6(7) . . ? B7 C2 Ta1 127.3(6) . . ? B3 C2 Ta1 67.6(4) . . ? C12 C11 C1 113.4(7) . . ? N1 C12 C11 110.9(7) . . ? N2 C15 C16 122.0(6) . . ? N2 C15 C20 120.7(7) . . ? C16 C15 C20 117.3(7) . . ? C17 C16 C15 121.4(7) . . ? C17 C16 C24 119.1(8) . . ? C15 C16 C24 119.4(7) . . ? C16 C17 C18 121.6(8) . . ? C19 C18 C17 120.0(9) . . ? C18 C19 C20 120.9(8) . . ? C15 C20 C19 118.8(7) . . ? C15 C20 C21 121.5(7) . . ? C19 C20 C21 119.7(7) . . ? C20 C21 C23 109.8(8) . . ? C20 C21 C22 110.1(8) . . ? C23 C21 C22 109.4(8) . . ? C16 C24 C25 111.2(8) . . ? C16 C24 C26 112.8(9) . . ? C25 C24 C26 104.1(9) . . ? C32 C27 C28 123.1(8) . . ? C32 C27 N3 118.8(7) . . ? C28 C27 N3 118.1(7) . . ? C29 C28 C27 116.7(8) . . ? C29 C28 C36 118.9(9) . . ? C27 C28 C36 124.4(8) . . ? C30 C29 C28 120.3(10) . . ? C31 C30 C29 121.6(9) . . ? C30 C31 C32 121.5(9) . . ? C27 C32 C31 116.8(8) . . ? C27 C32 C33 124.0(8) . . ? C31 C32 C33 119.2(8) . . ? C35 C33 C34 110.2(8) . . ? C35 C33 C32 110.8(8) . . ? C34 C33 C32 111.7(8) . . ? C28 C36 C38 108.6(9) . . ? C28 C36 C37 109.9(10) . . ? C38 C36 C37 113.2(10) . . ? N3 C39 C40 127.5(8) . . ? N3 C39 Ta1 76.6(5) . . ? C40 C39 Ta1 155.7(7) . . ? C2 B3 B4 105.0(7) . . ? C2 B3 B7 59.0(6) . . ? B4 B3 B7 107.0(7) . . ? C2 B3 B8 105.7(7) . . ? B4 B3 B8 59.4(6) . . ? B7 B3 B8 60.0(6) . . ? C2 B3 Ta1 70.5(5) . . ? B4 B3 Ta1 71.2(4) . . ? B7 B3 Ta1 127.4(6) . . ? B8 B3 Ta1 127.8(7) . . ? B5 B4 B8 105.5(7) . . ? B5 B4 B3 105.6(7) . . ? B8 B4 B3 61.1(6) . . ? B5 B4 B9 60.0(6) . . ? B8 B4 B9 58.0(6) . . ? B3 B4 B9 107.1(7) . . ? B5 B4 Ta1 73.1(5) . . ? B8 B4 Ta1 124.8(6) . . ? B3 B4 Ta1 66.4(4) . . ? B9 B4 Ta1 129.2(6) . . ? C1 B5 B4 108.7(7) . . ? C1 B5 B9 107.9(7) . . ? B4 B5 B9 62.9(6) . . ? C1 B5 B10 61.3(6) . . ? B4 B5 B10 112.7(7) . . ? B9 B5 B10 60.3(6) . . ? C1 B5 Ta1 70.6(4) . . ? B4 B5 Ta1 67.6(4) . . ? B9 B5 Ta1 126.8(6) . . ? B10 B5 Ta1 129.1(6) . . ? C1 B6 C2 55.9(6) . . ? C1 B6 B7 104.1(7) . . ? C2 B6 B7 60.9(6) . . ? C1 B6 B11 105.8(7) . . ? C2 B6 B11 108.2(8) . . ? B7 B6 B11 60.2(7) . . ? C1 B6 B10 59.7(6) . . ? C2 B6 B10 106.6(7) . . ? B7 B6 B10 108.7(8) . . ? B11 B6 B10 60.8(7) . . ? B6 B7 B11 60.8(7) . . ? B6 B7 C2 59.5(6) . . ? B11 B7 C2 107.7(8) . . ? B6 B7 B3 108.8(8) . . ? B11 B7 B3 110.2(8) . . ? C2 B7 B3 59.1(5) . . ? B6 B7 B8 108.6(8) . . ? B11 B7 B8 60.8(7) . . ? C2 B7 B8 106.0(7) . . ? B3 B7 B8 60.4(6) . . ? B9 B8 B4 62.0(6) . . ? B9 B8 B11 60.6(7) . . ? B4 B8 B11 109.5(8) . . ? B9 B8 B7 106.5(8) . . ? B4 B8 B7 106.8(7) . . ? B11 B8 B7 57.9(6) . . ? B9 B8 B3 109.1(7) . . ? B4 B8 B3 59.5(5) . . ? B11 B8 B3 107.2(7) . . ? B7 B8 B3 59.6(6) . . ? B8 B9 B5 104.7(7) . . ? B8 B9 B10 109.4(8) . . ? B5 B9 B10 59.9(6) . . ? B8 B9 B11 61.2(7) . . ? B5 B9 B11 106.0(8) . . ? B10 B9 B11 60.3(7) . . ? B8 B9 B4 60.0(6) . . ? B5 B9 B4 57.1(5) . . ? B10 B9 B4 107.6(7) . . ? B11 B9 B4 108.4(8) . . ? C1 B10 B5 55.6(5) . . ? C1 B10 B9 103.2(7) . . ? B5 B10 B9 59.8(6) . . ? C1 B10 B6 58.2(6) . . ? B5 B10 B6 103.9(7) . . ? B9 B10 B6 106.8(8) . . ? C1 B10 B11 103.3(7) . . ? B5 B10 B11 105.8(8) . . ? B9 B10 B11 60.2(7) . . ? B6 B10 B11 59.0(6) . . ? B7 B11 B6 59.0(6) . . ? B7 B11 B9 107.2(8) . . ? B6 B11 B9 107.1(8) . . ? B7 B11 B10 107.3(8) . . ? B6 B11 B10 60.1(6) . . ? B9 B11 B10 59.5(6) . . ? B7 B11 B8 61.2(6) . . ? B6 B11 B8 107.5(8) . . ? B9 B11 B8 58.2(7) . . ? B10 B11 B8 106.3(8) . . ? C44 O1 C41 117.6(12) . . ? O1 C41 C42 104.8(13) . . ? O1 C44 C43 102.2(12) . . ? C41 C42 C43 105.8(13) . . ? C42 C43 C44 109.5(13) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.888 _refine_diff_density_min -0.847 _refine_diff_density_rms 0.141 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.993 -0.057 0.074 43.4 0.9 2 0.777 -0.034 0.145 23.7 -1.2 3 0.500 0.000 0.500 582.1 42.8 4 0.223 0.034 0.855 23.5 -2.2 5 0.007 0.057 0.926 43.7 1.2 6 0.779 0.207 0.798 35.3 0.1 7 0.251 0.188 0.797 12.0 0.3 8 0.226 0.216 0.082 24.0 -0.5 9 0.779 0.293 0.298 35.4 0.0 10 0.226 0.284 0.582 24.0 -0.5 11 0.500 0.500 1.000 582.1 43.1 12 0.251 0.312 0.297 11.8 -0.2 13 1.007 0.443 0.426 43.3 1.0 14 0.223 0.466 0.355 23.7 -1.6 15 0.993 0.557 0.574 43.7 1.7 16 0.777 0.534 0.645 23.6 -1.3 17 0.221 0.707 0.702 35.2 -0.3 18 0.749 0.688 0.703 11.9 -0.1 19 0.774 0.716 0.418 24.0 -0.2 20 0.221 0.793 0.202 35.5 -0.4 21 0.774 0.784 0.918 24.0 -0.5 22 0.749 0.812 0.203 11.8 -0.5 _platon_squeeze_details ; ; #===END _database_code_depnum_ccdc_archive 'CCDC 943873'