# Electronic Supplementary Material (ESI) for Dalton Transactions # 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_ip270 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H49 B10 Li N2 O2' _chemical_formula_weight 500.68 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' Li Li -0.0003 0.0001 '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' O O 0.0106 0.0060 '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 10.518(2) _cell_length_b 11.229(2) _cell_length_c 14.087(3) _cell_angle_alpha 103.86(3) _cell_angle_beta 108.18(3) _cell_angle_gamma 96.24(3) _cell_volume 1504.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 24481 _cell_measurement_theta_min 2.08 _cell_measurement_theta_max 29.57 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.105 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540 _exptl_absorpt_coefficient_mu 0.062 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17190 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7418 _reflns_number_gt 5446 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL v4.5' _computing_publication_material 'Bruker SHELXTL v4.5' _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^)+(0.0752P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7418 _refine_ls_number_parameters 479 _refine_ls_number_restraints 170 _refine_ls_R_factor_all 0.0713 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1259 _refine_ls_wR_factor_gt 0.1170 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.28083(9) 0.97902(10) 0.29019(7) 0.0191(2) Uani 1 1 d . A . N2 N 0.15994(11) 1.09162(10) 0.38795(8) 0.0217(2) Uani 1 1 d . . . H2 H 0.0815(18) 1.0740(17) 0.3960(13) 0.040(5) Uiso 1 1 d . . . C1 C 0.04744(11) 0.89102(12) 0.25748(9) 0.0193(2) Uani 1 1 d . . . C2 C 0.05932(11) 0.77387(12) 0.16295(9) 0.0206(2) Uani 1 1 d . A . C3 C 0.17487(11) 0.99441(11) 0.31399(8) 0.0183(2) Uani 1 1 d . . . C4 C 0.41135(11) 1.06794(11) 0.34800(9) 0.0187(2) Uani 1 1 d . . . H4A H 0.4081 1.1197 0.4153 0.022 Uiso 1 1 calc R . . C5 C 0.43982(12) 1.15386(12) 0.28463(10) 0.0229(3) Uani 1 1 d . . . H5A H 0.3674 1.2036 0.2715 0.028 Uiso 1 1 calc R . . H5B H 0.4384 1.1027 0.2164 0.028 Uiso 1 1 calc R . . C6 C 0.57883(13) 1.24203(13) 0.34315(11) 0.0291(3) Uani 1 1 d . . . H6A H 0.5970 1.2945 0.2997 0.035 Uiso 1 1 calc R . . H6B H 0.5773 1.2982 0.4085 0.035 Uiso 1 1 calc R . . C7 C 0.69268(13) 1.16933(14) 0.36901(12) 0.0337(3) Uani 1 1 d . . . H7A H 0.7018 1.1212 0.3035 0.040 Uiso 1 1 calc R . . H7B H 0.7801 1.2288 0.4112 0.040 Uiso 1 1 calc R . . C8 C 0.66426(12) 1.08030(14) 0.42897(11) 0.0309(3) Uani 1 1 d . . . H8A H 0.6676 1.1291 0.4986 0.037 Uiso 1 1 calc R . . H8B H 0.7359 1.0295 0.4394 0.037 Uiso 1 1 calc R . . C9 C 0.52469(12) 0.99374(12) 0.37089(10) 0.0226(3) Uani 1 1 d . . . H9A H 0.5246 0.9388 0.3044 0.027 Uiso 1 1 calc R . . H9B H 0.5071 0.9399 0.4136 0.027 Uiso 1 1 calc R . . C10 C 0.19376(12) 1.22489(12) 0.39511(9) 0.0203(2) Uani 1 1 d . . . H10A H 0.2921 1.2461 0.4033 0.024 Uiso 1 1 calc R . . C11 C 0.10775(14) 1.25555(14) 0.29801(10) 0.0316(3) Uani 1 1 d . . . H11A H 0.1254 1.2074 0.2363 0.038 Uiso 1 1 calc R . . H11B H 0.0097 1.2305 0.2865 0.038 Uiso 1 1 calc R . . C12 C 0.14139(17) 1.39492(16) 0.30984(13) 0.0422(4) Uani 1 1 d . . . H12A H 0.2371 1.4183 0.3145 0.051 Uiso 1 1 calc R . . H12B H 0.0814 1.4132 0.2475 0.051 Uiso 1 1 calc R . . C13 C 0.12209(18) 1.47249(16) 0.40694(14) 0.0446(4) Uani 1 1 d . . . H13A H 0.1495 1.5626 0.4151 0.053 Uiso 1 1 calc R . . H13B H 0.0245 1.4556 0.3992 0.053 Uiso 1 1 calc R . . C14 C 0.20709(16) 1.44129(14) 0.50339(12) 0.0355(3) Uani 1 1 d . . . H14A H 0.1894 1.4894 0.5651 0.043 Uiso 1 1 calc R . . H14B H 0.3052 1.4663 0.5151 0.043 Uiso 1 1 calc R . . C15 C 0.17364(13) 1.30208(12) 0.49180(10) 0.0258(3) Uani 1 1 d . . . H15A H 0.2334 1.2840 0.5543 0.031 Uiso 1 1 calc R . . H15B H 0.0778 1.2785 0.4868 0.031 Uiso 1 1 calc R . . O1 O 0.2862(9) 0.8247(13) 0.0488(6) 0.0314(14) Uani 0.600(12) 1 d PDU A 1 C16 C 0.1847(6) 0.7792(7) -0.0523(5) 0.0397(13) Uani 0.600(12) 1 d PDU A 1 H16A H 0.1455 0.8489 -0.0738 0.048 Uiso 0.600(12) 1 calc PR A 1 H16B H 0.1102 0.7171 -0.0524 0.048 Uiso 0.600(12) 1 calc PR A 1 C17 C 0.2508(4) 0.7206(4) -0.1244(4) 0.0360(10) Uani 0.600(12) 1 d PDU A 1 H17A H 0.2220 0.6284 -0.1461 0.043 Uiso 0.600(12) 1 calc PR A 1 H17B H 0.2256 0.7499 -0.1875 0.043 Uiso 0.600(12) 1 calc PR A 1 C18 C 0.3939(5) 0.7567(7) -0.0692(4) 0.0493(14) Uani 0.600(12) 1 d PDU A 1 H18A H 0.4394 0.7957 -0.1093 0.059 Uiso 0.600(12) 1 calc PR A 1 H18B H 0.4330 0.6827 -0.0581 0.059 Uiso 0.600(12) 1 calc PR A 1 C19 C 0.4151(7) 0.8508(9) 0.0359(5) 0.060(2) Uani 0.600(12) 1 d PDU A 1 H19A H 0.4897 0.8369 0.0930 0.072 Uiso 0.600(12) 1 calc PR A 1 H19B H 0.4362 0.9380 0.0337 0.072 Uiso 0.600(12) 1 calc PR A 1 O1' O 0.3049(13) 0.8401(19) 0.0566(9) 0.029(2) Uani 0.400(12) 1 d PDU A 2 C16' C 0.1986(11) 0.8255(11) -0.0406(9) 0.048(2) Uani 0.400(12) 1 d PDU A 2 H16C H 0.1763 0.9076 -0.0462 0.057 Uiso 0.400(12) 1 calc PR A 2 H16D H 0.1150 0.7696 -0.0469 0.057 Uiso 0.400(12) 1 calc PR A 2 C17' C 0.2515(9) 0.7714(14) -0.1205(7) 0.076(3) Uani 0.400(12) 1 d PDU A 2 H17C H 0.2223 0.6792 -0.1437 0.091 Uiso 0.400(12) 1 calc PR A 2 H17D H 0.2164 0.8031 -0.1815 0.091 Uiso 0.400(12) 1 calc PR A 2 C18' C 0.3948(8) 0.8050(11) -0.0783(6) 0.050(2) Uani 0.400(12) 1 d PDU A 2 H18C H 0.4276 0.8807 -0.0949 0.060 Uiso 0.400(12) 1 calc PR A 2 H18D H 0.4365 0.7361 -0.1060 0.060 Uiso 0.400(12) 1 calc PR A 2 C19' C 0.4299(12) 0.8302(14) 0.0383(9) 0.052(3) Uani 0.400(12) 1 d PDU A 2 H19C H 0.4676 0.7608 0.0615 0.063 Uiso 0.400(12) 1 calc PR A 2 H19D H 0.4982 0.9090 0.0764 0.063 Uiso 0.400(12) 1 calc PR A 2 O2 O 0.3696(12) 0.6896(7) 0.2135(7) 0.031(3) Uani 0.560(13) 1 d PDU A 1 C20 C 0.3015(4) 0.5670(4) 0.1386(4) 0.0330(10) Uani 0.560(13) 1 d PDU A 1 H20A H 0.2104 0.5415 0.1423 0.040 Uiso 0.560(13) 1 calc PR A 1 H20B H 0.2894 0.5700 0.0668 0.040 Uiso 0.560(13) 1 calc PR A 1 C21 C 0.3855(8) 0.4804(6) 0.1654(5) 0.0391(13) Uani 0.560(13) 1 d PDU A 1 H21A H 0.4363 0.4611 0.1169 0.047 Uiso 0.560(13) 1 calc PR A 1 H21B H 0.3292 0.4015 0.1613 0.047 Uiso 0.560(13) 1 calc PR A 1 C22 C 0.4834(13) 0.5417(11) 0.2756(8) 0.038(2) Uani 0.560(13) 1 d PDU A 1 H22A H 0.4796 0.4876 0.3211 0.046 Uiso 0.560(13) 1 calc PR A 1 H22B H 0.5783 0.5614 0.2773 0.046 Uiso 0.560(13) 1 calc PR A 1 C23 C 0.4318(10) 0.6584(10) 0.3076(7) 0.0312(17) Uani 0.560(13) 1 d PDU A 1 H23A H 0.3643 0.6436 0.3413 0.037 Uiso 0.560(13) 1 calc PR A 1 H23B H 0.5080 0.7268 0.3571 0.037 Uiso 0.560(13) 1 calc PR A 1 O2' O 0.3707(15) 0.6869(9) 0.2090(9) 0.029(3) Uani 0.440(13) 1 d PDU A 2 C20' C 0.3530(11) 0.5834(6) 0.1216(3) 0.0451(18) Uani 0.440(13) 1 d PDU A 2 H20C H 0.2543 0.5493 0.0839 0.054 Uiso 0.440(13) 1 calc PR A 2 H20D H 0.3910 0.6126 0.0732 0.054 Uiso 0.440(13) 1 calc PR A 2 C21' C 0.4174(9) 0.4876(9) 0.1509(7) 0.0407(18) Uani 0.440(13) 1 d PDU A 2 H21C H 0.4764 0.4630 0.1098 0.049 Uiso 0.440(13) 1 calc PR A 2 H21D H 0.3488 0.4131 0.1396 0.049 Uiso 0.440(13) 1 calc PR A 2 C22' C 0.5012(15) 0.5416(11) 0.2645(9) 0.029(2) Uani 0.440(13) 1 d PDU A 2 H22C H 0.5996 0.5582 0.2747 0.035 Uiso 0.440(13) 1 calc PR A 2 H22D H 0.4851 0.4832 0.3041 0.035 Uiso 0.440(13) 1 calc PR A 2 C23' C 0.4557(12) 0.6611(13) 0.2999(9) 0.0264(17) Uani 0.440(13) 1 d PDU A 2 H23C H 0.4042 0.6523 0.3467 0.032 Uiso 0.440(13) 1 calc PR A 2 H23D H 0.5359 0.7304 0.3387 0.032 Uiso 0.440(13) 1 calc PR A 2 B3 B -0.03547(13) 0.88355(15) 0.13167(11) 0.0242(3) Uani 1 1 d . . . H3 H 0.0012(15) 0.9544(15) 0.0988(12) 0.031(4) Uiso 1 1 d . . . B4 B -0.11165(14) 0.92632(15) 0.22950(12) 0.0272(3) Uani 1 1 d . . . H4 H -0.1214(15) 1.0249(16) 0.2545(12) 0.032(4) Uiso 1 1 d . . . B5 B -0.05246(15) 0.84311(15) 0.32152(11) 0.0262(3) Uani 1 1 d . . . H5 H -0.0262(15) 0.8926(16) 0.4063(12) 0.034(4) Uiso 1 1 d . . . B6 B 0.05724(14) 0.74930(14) 0.27793(11) 0.0229(3) Uani 1 1 d . . . H6 H 0.1519(16) 0.7381(16) 0.3312(12) 0.039(4) Uiso 1 1 d . . . B7 B -0.20880(14) 0.81798(17) 0.10776(12) 0.0303(3) Uani 1 1 d . . . H7 H -0.2930(16) 0.8430(16) 0.0493(13) 0.038(4) Uiso 1 1 d . . . B8 B -0.09929(14) 0.72353(16) 0.06796(11) 0.0268(3) Uani 1 1 d . . . H8 H -0.1061(16) 0.6883(16) -0.0120(13) 0.036(4) Uiso 1 1 d . . . B9 B -0.04264(15) 0.64062(15) 0.15808(11) 0.0254(3) Uani 1 1 d . . . H9 H -0.0105(16) 0.5512(17) 0.1355(12) 0.037(4) Uiso 1 1 d . . . B10 B -0.11372(15) 0.68153(15) 0.25747(12) 0.0277(3) Uani 1 1 d . . . H10 H -0.1350(16) 0.6154(17) 0.3011(13) 0.039(4) Uiso 1 1 d . . . B11 B -0.21831(15) 0.79142(16) 0.22581(13) 0.0303(3) Uani 1 1 d . . . H11 H -0.3131(17) 0.8018(17) 0.2474(13) 0.042(5) Uiso 1 1 d . . . B12 B -0.21288(15) 0.66590(16) 0.12536(12) 0.0289(3) Uani 1 1 d . . . H12 H -0.2997(15) 0.5879(15) 0.0807(12) 0.030(4) Uiso 1 1 d . . . Li Li 0.2653(2) 0.8175(2) 0.17749(16) 0.0227(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0165(4) 0.0183(5) 0.0191(4) 0.0041(4) 0.0033(4) 0.0013(4) N2 0.0238(5) 0.0168(5) 0.0254(5) 0.0036(4) 0.0122(4) 0.0018(4) C1 0.0169(5) 0.0188(6) 0.0206(5) 0.0032(5) 0.0064(4) 0.0027(4) C2 0.0178(5) 0.0199(6) 0.0201(5) 0.0017(5) 0.0051(4) 0.0011(4) C3 0.0194(5) 0.0162(6) 0.0179(5) 0.0050(4) 0.0049(4) 0.0024(4) C4 0.0172(5) 0.0162(6) 0.0193(5) 0.0019(4) 0.0048(4) 0.0008(4) C5 0.0214(6) 0.0218(7) 0.0264(6) 0.0075(5) 0.0095(5) 0.0033(5) C6 0.0265(6) 0.0219(7) 0.0377(7) 0.0064(6) 0.0131(5) -0.0011(5) C7 0.0208(6) 0.0299(8) 0.0466(8) 0.0070(6) 0.0119(6) -0.0006(5) C8 0.0177(6) 0.0321(8) 0.0355(7) 0.0064(6) 0.0023(5) 0.0037(5) C9 0.0205(6) 0.0190(6) 0.0254(6) 0.0046(5) 0.0056(4) 0.0035(5) C10 0.0205(5) 0.0164(6) 0.0232(5) 0.0056(5) 0.0068(4) 0.0033(4) C11 0.0343(7) 0.0311(8) 0.0263(6) 0.0123(6) 0.0038(5) 0.0054(6) C12 0.0472(9) 0.0375(9) 0.0449(9) 0.0269(8) 0.0088(7) 0.0093(7) C13 0.0485(9) 0.0255(8) 0.0657(11) 0.0212(8) 0.0189(8) 0.0165(7) C14 0.0446(8) 0.0190(7) 0.0417(8) 0.0033(6) 0.0174(6) 0.0069(6) C15 0.0307(6) 0.0191(7) 0.0270(6) 0.0045(5) 0.0107(5) 0.0054(5) O1 0.019(2) 0.047(3) 0.0252(16) 0.0061(14) 0.0090(14) -0.0015(18) C16 0.0235(14) 0.069(4) 0.0240(15) 0.012(2) 0.0039(11) 0.013(2) C17 0.0315(16) 0.037(2) 0.0318(15) 0.0011(14) 0.0097(12) 0.0010(14) C18 0.0343(19) 0.079(4) 0.0378(18) 0.010(2) 0.0192(13) 0.018(2) C19 0.031(3) 0.096(5) 0.032(2) -0.012(2) 0.0181(19) -0.028(3) O1' 0.018(3) 0.046(5) 0.028(3) 0.017(3) 0.009(2) 0.007(4) C16' 0.047(4) 0.069(6) 0.043(4) 0.032(4) 0.018(3) 0.034(4) C17' 0.057(4) 0.129(8) 0.035(3) 0.012(5) 0.007(2) 0.047(5) C18' 0.042(3) 0.067(5) 0.033(3) 0.000(3) 0.020(2) -0.012(3) C19' 0.025(3) 0.094(6) 0.048(4) 0.024(4) 0.020(3) 0.024(4) O2 0.034(4) 0.020(3) 0.028(3) -0.003(2) 0.002(2) 0.004(3) C20 0.0255(17) 0.0265(16) 0.0345(19) -0.0003(13) 0.0004(12) 0.0055(12) C21 0.049(3) 0.0283(19) 0.034(2) -0.0003(14) 0.0100(19) 0.016(2) C22 0.031(4) 0.039(3) 0.042(3) 0.014(2) 0.007(2) 0.008(2) C23 0.044(4) 0.027(2) 0.0269(19) 0.0108(15) 0.013(2) 0.013(2) O2' 0.034(5) 0.028(5) 0.024(4) 0.011(3) 0.001(3) 0.018(3) C20' 0.072(5) 0.031(3) 0.0264(18) -0.0005(16) 0.012(2) 0.022(3) C21' 0.032(3) 0.050(3) 0.038(3) -0.001(2) 0.0146(19) 0.025(2) C22' 0.022(3) 0.018(3) 0.043(4) 0.008(2) 0.004(3) 0.0106(19) C23' 0.023(3) 0.032(3) 0.026(3) 0.011(2) 0.008(2) 0.0077(19) B3 0.0164(6) 0.0298(8) 0.0244(6) 0.0100(6) 0.0032(5) 0.0033(5) B4 0.0186(6) 0.0263(8) 0.0368(8) 0.0070(6) 0.0113(6) 0.0049(5) B5 0.0255(7) 0.0252(8) 0.0264(7) 0.0028(6) 0.0128(5) -0.0021(6) B6 0.0237(6) 0.0189(7) 0.0230(6) 0.0055(5) 0.0054(5) 0.0004(5) B7 0.0161(6) 0.0365(9) 0.0345(8) 0.0103(7) 0.0045(5) 0.0027(6) B8 0.0184(6) 0.0331(9) 0.0214(6) 0.0027(6) 0.0032(5) -0.0026(6) B9 0.0232(6) 0.0201(7) 0.0271(7) 0.0007(6) 0.0078(5) -0.0019(5) B10 0.0283(7) 0.0242(8) 0.0270(7) 0.0034(6) 0.0109(6) -0.0042(6) B11 0.0211(7) 0.0303(9) 0.0363(8) 0.0025(7) 0.0134(6) -0.0014(6) B12 0.0203(6) 0.0309(9) 0.0286(7) 0.0021(6) 0.0072(5) -0.0040(6) Li 0.0201(9) 0.0230(11) 0.0234(10) 0.0035(8) 0.0076(8) 0.0045(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C3 1.2773(16) . ? N1 C4 1.4696(16) . ? N1 Li 2.057(3) . ? N2 C3 1.3771(17) . ? N2 C10 1.4717(16) . ? N2 H2 0.876(18) . ? C1 C3 1.5269(17) . ? C1 C2 1.6793(18) . ? C1 B3 1.6903(18) . ? C1 B6 1.692(2) . ? C1 B5 1.7054(19) . ? C1 B4 1.7087(19) . ? C2 B8 1.7127(19) . ? C2 B6 1.7132(18) . ? C2 B9 1.717(2) . ? C2 B3 1.720(2) . ? C2 Li 2.102(2) . ? C4 C9 1.5244(17) . ? C4 C5 1.5278(17) . ? C4 H4A 1.0000 . ? C5 C6 1.5296(18) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.522(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.516(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.5260(18) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C15 1.5184(18) . ? C10 C11 1.5262(17) . ? C10 H10A 1.0000 . ? C11 C12 1.523(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.520(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.519(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.522(2) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? O1 C16 1.418(8) . ? O1 C19 1.432(8) . ? O1 Li 1.913(9) . ? C16 C17 1.472(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.422(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.534(8) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? O1' C19' 1.427(11) . ? O1' C16' 1.432(11) . ? O1' Li 1.941(14) . ? C16' C17' 1.443(10) . ? C16' H16C 0.9900 . ? C16' H16D 0.9900 . ? C17' C18' 1.407(10) . ? C17' H17C 0.9900 . ? C17' H17D 0.9900 . ? C18' C19' 1.513(11) . ? C18' H18C 0.9900 . ? C18' H18D 0.9900 . ? C19' H19C 0.9900 . ? C19' H19D 0.9900 . ? O2 C23 1.428(9) . ? O2 C20 1.463(8) . ? O2 Li 1.967(9) . ? C20 C21 1.422(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.510(9) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.497(9) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? O2' C20' 1.423(11) . ? O2' C23' 1.430(10) . ? O2' Li 1.983(10) . ? C20' C21' 1.409(9) . ? C20' H20C 0.9900 . ? C20' H20D 0.9900 . ? C21' C22' 1.497(10) . ? C21' H21C 0.9900 . ? C21' H21D 0.9900 . ? C22' C23' 1.499(10) . ? C22' H22C 0.9900 . ? C22' H22D 0.9900 . ? C23' H23C 0.9900 . ? C23' H23D 0.9900 . ? B3 B8 1.753(2) . ? B3 B7 1.785(2) . ? B3 B4 1.797(2) . ? B3 H3 1.103(16) . ? B4 B7 1.761(2) . ? B4 B11 1.764(2) . ? B4 B5 1.773(2) . ? B4 H4 1.105(17) . ? B5 B10 1.766(2) . ? B5 B11 1.771(2) . ? B5 B6 1.793(2) . ? B5 H5 1.120(16) . ? B6 B9 1.753(2) . ? B6 B10 1.780(2) . ? B6 H6 1.084(16) . ? B7 B8 1.775(2) . ? B7 B12 1.781(3) . ? B7 B11 1.789(2) . ? B7 H7 1.118(16) . ? B8 B9 1.746(2) . ? B8 B12 1.785(2) . ? B8 H8 1.077(16) . ? B9 B10 1.775(2) . ? B9 B12 1.777(2) . ? B9 H9 1.101(18) . ? B10 B12 1.782(2) . ? B10 B11 1.785(3) . ? B10 H10 1.117(17) . ? B11 B12 1.762(2) . ? B11 H11 1.139(18) . ? B12 H12 1.096(15) . ? 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 C3 N1 C4 120.88(11) . . ? C3 N1 Li 117.26(10) . . ? C4 N1 Li 121.63(10) . . ? C3 N2 C10 124.76(10) . . ? C3 N2 H2 110.4(12) . . ? C10 N2 H2 110.9(12) . . ? C3 C1 C2 115.33(10) . . ? C3 C1 B3 114.94(10) . . ? C2 C1 B3 61.39(8) . . ? C3 C1 B6 117.28(10) . . ? C2 C1 B6 61.08(8) . . ? B3 C1 B6 113.74(10) . . ? C3 C1 B5 121.70(10) . . ? C2 C1 B5 113.17(10) . . ? B3 C1 B5 115.56(10) . . ? B6 C1 B5 63.70(9) . . ? C3 C1 B4 120.61(11) . . ? C2 C1 B4 113.15(10) . . ? B3 C1 B4 63.81(9) . . ? B6 C1 B4 115.07(10) . . ? B5 C1 B4 62.58(9) . . ? C1 C2 B8 107.05(10) . . ? C1 C2 B6 59.83(8) . . ? B8 C2 B6 111.21(10) . . ? C1 C2 B9 107.17(10) . . ? B8 C2 B9 61.20(9) . . ? B6 C2 B9 61.44(9) . . ? C1 C2 B3 59.62(8) . . ? B8 C2 B3 61.43(9) . . ? B6 C2 B3 111.19(10) . . ? B9 C2 B3 111.21(10) . . ? C1 C2 Li 102.59(10) . . ? B8 C2 Li 139.74(10) . . ? B6 C2 Li 107.02(10) . . ? B9 C2 Li 133.04(11) . . ? B3 C2 Li 115.06(10) . . ? N1 C3 N2 128.54(11) . . ? N1 C3 C1 117.50(11) . . ? N2 C3 C1 113.92(10) . . ? N1 C4 C9 108.38(10) . . ? N1 C4 C5 110.95(9) . . ? C9 C4 C5 109.66(10) . . ? N1 C4 H4A 109.3 . . ? C9 C4 H4A 109.3 . . ? C5 C4 H4A 109.3 . . ? C4 C5 C6 110.62(10) . . ? C4 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? C7 C6 C5 111.27(12) . . ? C7 C6 H6A 109.4 . . ? C5 C6 H6A 109.4 . . ? C7 C6 H6B 109.4 . . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C8 C7 C6 111.35(11) . . ? C8 C7 H7A 109.4 . . ? C6 C7 H7A 109.4 . . ? C8 C7 H7B 109.4 . . ? C6 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? C7 C8 C9 111.28(11) . . ? C7 C8 H8A 109.4 . . ? C9 C8 H8A 109.4 . . ? C7 C8 H8B 109.4 . . ? C9 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C4 C9 C8 111.36(11) . . ? C4 C9 H9A 109.4 . . ? C8 C9 H9A 109.4 . . ? C4 C9 H9B 109.4 . . ? C8 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? N2 C10 C15 108.43(10) . . ? N2 C10 C11 112.28(11) . . ? C15 C10 C11 110.58(11) . . ? N2 C10 H10A 108.5 . . ? C15 C10 H10A 108.5 . . ? C11 C10 H10A 108.5 . . ? C12 C11 C10 110.88(12) . . ? C12 C11 H11A 109.5 . . ? C10 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C13 C12 C11 111.07(13) . . ? C13 C12 H12A 109.4 . . ? C11 C12 H12A 109.4 . . ? C13 C12 H12B 109.4 . . ? C11 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? C14 C13 C12 110.67(13) . . ? C14 C13 H13A 109.5 . . ? C12 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C13 C14 C15 111.30(13) . . ? C13 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? C13 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C10 C15 C14 110.86(11) . . ? C10 C15 H15A 109.5 . . ? C14 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? C16 O1 C19 107.5(6) . . ? C16 O1 Li 126.8(7) . . ? C19 O1 Li 124.2(6) . . ? O1 C16 C17 107.4(5) . . ? O1 C16 H16A 110.2 . . ? C17 C16 H16A 110.2 . . ? O1 C16 H16B 110.2 . . ? C17 C16 H16B 110.2 . . ? H16A C16 H16B 108.5 . . ? C18 C17 C16 106.6(4) . . ? C18 C17 H17A 110.4 . . ? C16 C17 H17A 110.4 . . ? C18 C17 H17B 110.4 . . ? C16 C17 H17B 110.4 . . ? H17A C17 H17B 108.6 . . ? C17 C18 C19 107.1(4) . . ? C17 C18 H18A 110.3 . . ? C19 C18 H18A 110.3 . . ? C17 C18 H18B 110.3 . . ? C19 C18 H18B 110.3 . . ? H18A C18 H18B 108.5 . . ? O1 C19 C18 102.9(6) . . ? O1 C19 H19A 111.2 . . ? C18 C19 H19A 111.2 . . ? O1 C19 H19B 111.2 . . ? C18 C19 H19B 111.2 . . ? H19A C19 H19B 109.1 . . ? C19' O1' C16' 109.0(9) . . ? C19' O1' Li 126.1(9) . . ? C16' O1' Li 121.8(9) . . ? O1' C16' C17' 105.6(8) . . ? O1' C16' H16C 110.6 . . ? C17' C16' H16C 110.6 . . ? O1' C16' H16D 110.6 . . ? C17' C16' H16D 110.6 . . ? H16C C16' H16D 108.8 . . ? C18' C17' C16' 108.1(7) . . ? C18' C17' H17C 110.1 . . ? C16' C17' H17C 110.1 . . ? C18' C17' H17D 110.1 . . ? C16' C17' H17D 110.1 . . ? H17C C17' H17D 108.4 . . ? C17' C18' C19' 105.0(7) . . ? C17' C18' H18C 110.8 . . ? C19' C18' H18C 110.8 . . ? C17' C18' H18D 110.8 . . ? C19' C18' H18D 110.8 . . ? H18C C18' H18D 108.8 . . ? O1' C19' C18' 105.8(8) . . ? O1' C19' H19C 110.6 . . ? C18' C19' H19C 110.6 . . ? O1' C19' H19D 110.6 . . ? C18' C19' H19D 110.6 . . ? H19C C19' H19D 108.7 . . ? C23 O2 C20 102.5(7) . . ? C23 O2 Li 134.8(8) . . ? C20 O2 Li 110.1(5) . . ? C21 C20 O2 107.3(5) . . ? C21 C20 H20A 110.3 . . ? O2 C20 H20A 110.3 . . ? C21 C20 H20B 110.3 . . ? O2 C20 H20B 110.3 . . ? H20A C20 H20B 108.5 . . ? C20 C21 C22 106.8(5) . . ? C20 C21 H21A 110.4 . . ? C22 C21 H21A 110.4 . . ? C20 C21 H21B 110.4 . . ? C22 C21 H21B 110.4 . . ? H21A C21 H21B 108.6 . . ? C23 C22 C21 102.6(7) . . ? C23 C22 H22A 111.2 . . ? C21 C22 H22A 111.2 . . ? C23 C22 H22B 111.2 . . ? C21 C22 H22B 111.2 . . ? H22A C22 H22B 109.2 . . ? O2 C23 C22 105.6(7) . . ? O2 C23 H23A 110.6 . . ? C22 C23 H23A 110.6 . . ? O2 C23 H23B 110.6 . . ? C22 C23 H23B 110.6 . . ? H23A C23 H23B 108.7 . . ? C20' O2' C23' 107.4(7) . . ? C20' O2' Li 115.3(6) . . ? C23' O2' Li 137.0(9) . . ? C21' C20' O2' 112.4(6) . . ? C21' C20' H20C 109.1 . . ? O2' C20' H20C 109.1 . . ? C21' C20' H20D 109.1 . . ? O2' C20' H20D 109.1 . . ? H20C C20' H20D 107.9 . . ? C20' C21' C22' 105.5(7) . . ? C20' C21' H21C 110.6 . . ? C22' C21' H21C 110.6 . . ? C20' C21' H21D 110.6 . . ? C22' C21' H21D 110.6 . . ? H21C C21' H21D 108.8 . . ? C21' C22' C23' 105.8(8) . . ? C21' C22' H22C 110.6 . . ? C23' C22' H22C 110.6 . . ? C21' C22' H22D 110.6 . . ? C23' C22' H22D 110.6 . . ? H22C C22' H22D 108.7 . . ? O2' C23' C22' 107.6(8) . . ? O2' C23' H23C 110.2 . . ? C22' C23' H23C 110.2 . . ? O2' C23' H23D 110.2 . . ? C22' C23' H23D 110.2 . . ? H23C C23' H23D 108.5 . . ? C1 B3 C2 58.99(8) . . ? C1 B3 B8 104.74(11) . . ? C2 B3 B8 59.08(8) . . ? C1 B3 B7 104.26(10) . . ? C2 B3 B7 106.84(11) . . ? B8 B3 B7 60.20(9) . . ? C1 B3 B4 58.59(8) . . ? C2 B3 B4 107.03(10) . . ? B8 B3 B4 107.04(11) . . ? B7 B3 B4 58.92(9) . . ? C1 B3 H3 119.3(8) . . ? C2 B3 H3 120.5(8) . . ? B8 B3 H3 126.7(8) . . ? B7 B3 H3 127.0(8) . . ? B4 B3 H3 120.5(8) . . ? C1 B4 B7 104.50(11) . . ? C1 B4 B11 104.74(11) . . ? B7 B4 B11 60.97(9) . . ? C1 B4 B5 58.62(8) . . ? B7 B4 B5 108.75(12) . . ? B11 B4 B5 60.08(9) . . ? C1 B4 B3 57.60(8) . . ? B7 B4 B3 60.21(9) . . ? B11 B4 B3 108.43(12) . . ? B5 B4 B3 107.18(11) . . ? C1 B4 H4 119.2(8) . . ? B7 B4 H4 125.2(8) . . ? B11 B4 H4 127.9(8) . . ? B5 B4 H4 121.3(8) . . ? B3 B4 H4 117.9(8) . . ? C1 B5 B10 104.53(10) . . ? C1 B5 B11 104.60(10) . . ? B10 B5 B11 60.60(10) . . ? C1 B5 B4 58.80(8) . . ? B10 B5 B4 108.22(11) . . ? B11 B5 B4 59.71(9) . . ? C1 B5 B6 57.79(8) . . ? B10 B5 B6 60.02(9) . . ? B11 B5 B6 107.88(11) . . ? B4 B5 B6 107.15(10) . . ? C1 B5 H5 118.6(8) . . ? B10 B5 H5 127.8(8) . . ? B11 B5 H5 126.5(8) . . ? B4 B5 H5 118.3(9) . . ? B6 B5 H5 120.9(8) . . ? C1 B6 C2 59.09(8) . . ? C1 B6 B9 105.02(10) . . ? C2 B6 B9 59.40(8) . . ? C1 B6 B10 104.49(11) . . ? C2 B6 B10 107.35(10) . . ? B9 B6 B10 60.31(9) . . ? C1 B6 B5 58.51(8) . . ? C2 B6 B5 107.35(10) . . ? B9 B6 B5 107.48(11) . . ? B10 B6 B5 59.25(9) . . ? C1 B6 H6 118.4(9) . . ? C2 B6 H6 117.5(9) . . ? B9 B6 H6 125.5(9) . . ? B10 B6 H6 129.0(9) . . ? B5 B6 H6 122.4(9) . . ? B4 B7 B8 107.65(10) . . ? B4 B7 B12 107.20(11) . . ? B8 B7 B12 60.25(9) . . ? B4 B7 B3 60.87(9) . . ? B8 B7 B3 59.02(9) . . ? B12 B7 B3 107.44(11) . . ? B4 B7 B11 59.59(9) . . ? B8 B7 B11 107.20(12) . . ? B12 B7 B11 59.15(10) . . ? B3 B7 B11 107.86(10) . . ? B4 B7 H7 121.5(9) . . ? B8 B7 H7 121.1(9) . . ? B12 B7 H7 123.7(9) . . ? B3 B7 H7 119.6(8) . . ? B11 B7 H7 124.3(8) . . ? C2 B8 B9 59.54(8) . . ? C2 B8 B3 59.49(8) . . ? B9 B8 B3 108.29(10) . . ? C2 B8 B7 107.62(11) . . ? B9 B8 B7 108.68(11) . . ? B3 B8 B7 60.78(9) . . ? C2 B8 B12 107.32(10) . . ? B9 B8 B12 60.42(9) . . ? B3 B8 B12 108.68(11) . . ? B7 B8 B12 60.06(9) . . ? C2 B8 H8 118.5(8) . . ? B9 B8 H8 121.3(9) . . ? B3 B8 H8 118.5(9) . . ? B7 B8 H8 123.8(9) . . ? B12 B8 H8 125.8(9) . . ? C2 B9 B8 59.27(8) . . ? C2 B9 B6 59.16(8) . . ? B8 B9 B6 107.81(11) . . ? C2 B9 B10 107.41(11) . . ? B8 B9 B10 108.97(12) . . ? B6 B9 B10 60.62(9) . . ? C2 B9 B12 107.46(11) . . ? B8 B9 B12 60.87(9) . . ? B6 B9 B12 108.61(12) . . ? B10 B9 B12 60.22(9) . . ? C2 B9 H9 117.4(9) . . ? B8 B9 H9 121.1(8) . . ? B6 B9 H9 118.2(8) . . ? B10 B9 H9 124.5(9) . . ? B12 B9 H9 126.7(8) . . ? B5 B10 B9 107.67(11) . . ? B5 B10 B6 60.73(9) . . ? B9 B10 B6 59.07(9) . . ? B5 B10 B12 107.32(12) . . ? B9 B10 B12 59.95(9) . . ? B6 B10 B12 107.16(11) . . ? B5 B10 B11 59.82(9) . . ? B9 B10 B11 107.11(11) . . ? B6 B10 B11 107.82(11) . . ? B12 B10 B11 59.22(10) . . ? B5 B10 H10 120.7(9) . . ? B9 B10 H10 122.4(9) . . ? B6 B10 H10 120.6(8) . . ? B12 B10 H10 123.7(8) . . ? B11 B10 H10 122.9(9) . . ? B12 B11 B4 107.93(11) . . ? B12 B11 B5 108.01(12) . . ? B4 B11 B5 60.21(9) . . ? B12 B11 B10 60.32(10) . . ? B4 B11 B10 107.81(10) . . ? B5 B11 B10 59.58(9) . . ? B12 B11 B7 60.21(10) . . ? B4 B11 B7 59.44(9) . . ? B5 B11 B7 107.64(10) . . ? B10 B11 B7 108.04(11) . . ? B12 B11 H11 123.5(9) . . ? B4 B11 H11 119.1(9) . . ? B5 B11 H11 121.3(8) . . ? B10 B11 H11 124.2(9) . . ? B7 B11 H11 120.7(9) . . ? B11 B12 B9 108.01(11) . . ? B11 B12 B7 60.63(10) . . ? B9 B12 B7 107.02(11) . . ? B11 B12 B10 60.47(10) . . ? B9 B12 B10 59.83(9) . . ? B7 B12 B10 108.49(11) . . ? B11 B12 B8 107.92(11) . . ? B9 B12 B8 58.71(9) . . ? B7 B12 B8 59.69(9) . . ? B10 B12 B8 106.94(10) . . ? B11 B12 H12 122.5(8) . . ? B9 B12 H12 120.8(9) . . ? B7 B12 H12 123.0(8) . . ? B10 B12 H12 121.1(8) . . ? B8 B12 H12 122.1(8) . . ? O1 Li O1' 6.7(8) . . ? O1 Li O2 102.6(5) . . ? O1' Li O2 102.6(6) . . ? O1 Li O2' 100.7(6) . . ? O1' Li O2' 100.8(7) . . ? O2 Li O2' 1.9(7) . . ? O1 Li N1 120.5(4) . . ? O1' Li N1 115.8(6) . . ? O2 Li N1 120.5(3) . . ? O2' Li N1 122.2(3) . . ? O1 Li C2 112.4(3) . . ? O1' Li C2 117.9(4) . . ? O2 Li C2 113.6(4) . . ? O2' Li C2 114.2(5) . . ? N1 Li C2 86.99(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 C1 C2 B8 -146.43(10) . . . . ? B3 C1 C2 B8 -40.58(10) . . . . ? B6 C1 C2 B8 105.04(11) . . . . ? B5 C1 C2 B8 66.95(12) . . . . ? B4 C1 C2 B8 -1.83(13) . . . . ? C3 C1 C2 B6 108.53(11) . . . . ? B3 C1 C2 B6 -145.62(10) . . . . ? B5 C1 C2 B6 -38.09(10) . . . . ? B4 C1 C2 B6 -106.87(11) . . . . ? C3 C1 C2 B9 149.21(10) . . . . ? B3 C1 C2 B9 -104.94(10) . . . . ? B6 C1 C2 B9 40.68(9) . . . . ? B5 C1 C2 B9 2.59(13) . . . . ? B4 C1 C2 B9 -66.20(12) . . . . ? C3 C1 C2 B3 -105.86(11) . . . . ? B6 C1 C2 B3 145.62(10) . . . . ? B5 C1 C2 B3 107.53(11) . . . . ? B4 C1 C2 B3 38.74(10) . . . . ? C3 C1 C2 Li 5.99(13) . . . . ? B3 C1 C2 Li 111.84(11) . . . . ? B6 C1 C2 Li -102.54(10) . . . . ? B5 C1 C2 Li -140.63(10) . . . . ? B4 C1 C2 Li 150.59(10) . . . . ? C4 N1 C3 N2 3.49(18) . . . . ? Li N1 C3 N2 178.10(11) . . . . ? C4 N1 C3 C1 -173.98(10) . . . . ? Li N1 C3 C1 0.63(15) . . . . ? C10 N2 C3 N1 53.19(18) . . . . ? C10 N2 C3 C1 -129.27(12) . . . . ? C2 C1 C3 N1 -4.77(15) . . . . ? B3 C1 C3 N1 -73.42(14) . . . . ? B6 C1 C3 N1 64.26(14) . . . . ? B5 C1 C3 N1 138.74(12) . . . . ? B4 C1 C3 N1 -146.54(11) . . . . ? C2 C1 C3 N2 177.40(9) . . . . ? B3 C1 C3 N2 108.75(12) . . . . ? B6 C1 C3 N2 -113.57(12) . . . . ? B5 C1 C3 N2 -39.09(15) . . . . ? B4 C1 C3 N2 35.63(15) . . . . ? C3 N1 C4 C9 135.53(11) . . . . ? Li N1 C4 C9 -38.85(14) . . . . ? C3 N1 C4 C5 -104.03(13) . . . . ? Li N1 C4 C5 81.60(13) . . . . ? N1 C4 C5 C6 -177.38(11) . . . . ? C9 C4 C5 C6 -57.69(14) . . . . ? C4 C5 C6 C7 56.83(15) . . . . ? C5 C6 C7 C8 -54.91(16) . . . . ? C6 C7 C8 C9 54.31(16) . . . . ? N1 C4 C9 C8 178.76(10) . . . . ? C5 C4 C9 C8 57.51(13) . . . . ? C7 C8 C9 C4 -56.11(15) . . . . ? C3 N2 C10 C15 -175.51(11) . . . . ? C3 N2 C10 C11 62.01(16) . . . . ? N2 C10 C11 C12 177.75(12) . . . . ? C15 C10 C11 C12 56.50(16) . . . . ? C10 C11 C12 C13 -56.40(17) . . . . ? C11 C12 C13 C14 56.00(18) . . . . ? C12 C13 C14 C15 -56.09(18) . . . . ? N2 C10 C15 C14 -179.96(11) . . . . ? C11 C10 C15 C14 -56.46(15) . . . . ? C13 C14 C15 C10 56.57(16) . . . . ? C19 O1 C16 C17 27.0(11) . . . . ? Li O1 C16 C17 -139.8(8) . . . . ? O1 C16 C17 C18 -12.4(9) . . . . ? C16 C17 C18 C19 -5.7(9) . . . . ? C16 O1 C19 C18 -29.3(12) . . . . ? Li O1 C19 C18 137.9(9) . . . . ? C17 C18 C19 O1 21.4(10) . . . . ? C19' O1' C16' C17' 16.2(17) . . . . ? Li O1' C16' C17' -144.8(11) . . . . ? O1' C16' C17' C18' -25.8(13) . . . . ? C16' C17' C18' C19' 24.6(11) . . . . ? C16' O1' C19' C18' -1.4(18) . . . . ? Li O1' C19' C18' 158.5(12) . . . . ? C17' C18' C19' O1' -14.2(14) . . . . ? C23 O2 C20 C21 -35.1(10) . . . . ? Li O2 C20 C21 176.8(6) . . . . ? O2 C20 C21 C22 17.0(10) . . . . ? C20 C21 C22 C23 6.8(10) . . . . ? C20 O2 C23 C22 39.1(12) . . . . ? Li O2 C23 C22 174.8(10) . . . . ? C21 C22 C23 O2 -28.7(12) . . . . ? C23' O2' C20' C21' 2.7(16) . . . . ? Li O2' C20' C21' -172.9(8) . . . . ? O2' C20' C21' C22' -9.1(14) . . . . ? C20' C21' C22' C23' 11.6(13) . . . . ? C20' O2' C23' C22' 5.0(17) . . . . ? Li O2' C23' C22' 179.2(15) . . . . ? C21' C22' C23' O2' -10.3(16) . . . . ? C3 C1 B3 C2 106.49(11) . . . . ? B6 C1 B3 C2 -32.68(9) . . . . ? B5 C1 B3 C2 -103.64(11) . . . . ? B4 C1 B3 C2 -140.11(10) . . . . ? C3 C1 B3 B8 145.40(10) . . . . ? C2 C1 B3 B8 38.91(9) . . . . ? B6 C1 B3 B8 6.23(13) . . . . ? B5 C1 B3 B8 -64.73(14) . . . . ? B4 C1 B3 B8 -101.20(11) . . . . ? C3 C1 B3 B7 -152.21(11) . . . . ? C2 C1 B3 B7 101.31(12) . . . . ? B6 C1 B3 B7 68.62(13) . . . . ? B5 C1 B3 B7 -2.34(15) . . . . ? B4 C1 B3 B7 -38.81(10) . . . . ? C3 C1 B3 B4 -113.40(12) . . . . ? C2 C1 B3 B4 140.11(10) . . . . ? B6 C1 B3 B4 107.43(12) . . . . ? B5 C1 B3 B4 36.47(11) . . . . ? B8 C2 B3 C1 134.92(10) . . . . ? B6 C2 B3 C1 31.58(9) . . . . ? B9 C2 B3 C1 98.02(11) . . . . ? Li C2 B3 C1 -90.28(11) . . . . ? C1 C2 B3 B8 -134.92(10) . . . . ? B6 C2 B3 B8 -103.35(11) . . . . ? B9 C2 B3 B8 -36.90(10) . . . . ? Li C2 B3 B8 134.79(11) . . . . ? C1 C2 B3 B7 -96.80(11) . . . . ? B8 C2 B3 B7 38.13(10) . . . . ? B6 C2 B3 B7 -65.22(13) . . . . ? B9 C2 B3 B7 1.23(13) . . . . ? Li C2 B3 B7 172.92(10) . . . . ? C1 C2 B3 B4 -34.92(9) . . . . ? B8 C2 B3 B4 100.00(11) . . . . ? B6 C2 B3 B4 -3.34(13) . . . . ? B9 C2 B3 B4 63.10(12) . . . . ? Li C2 B3 B4 -125.20(11) . . . . ? C3 C1 B4 B7 144.25(11) . . . . ? C2 C1 B4 B7 1.72(14) . . . . ? B3 C1 B4 B7 39.47(10) . . . . ? B6 C1 B4 B7 -65.91(13) . . . . ? B5 C1 B4 B7 -103.36(12) . . . . ? C3 C1 B4 B11 -152.51(11) . . . . ? C2 C1 B4 B11 64.96(13) . . . . ? B3 C1 B4 B11 102.72(12) . . . . ? B6 C1 B4 B11 -2.66(14) . . . . ? B5 C1 B4 B11 -40.12(10) . . . . ? C3 C1 B4 B5 -112.39(12) . . . . ? C2 C1 B4 B5 105.08(11) . . . . ? B3 C1 B4 B5 142.83(11) . . . . ? B6 C1 B4 B5 37.46(11) . . . . ? C3 C1 B4 B3 104.77(12) . . . . ? C2 C1 B4 B3 -37.75(10) . . . . ? B6 C1 B4 B3 -105.38(12) . . . . ? B5 C1 B4 B3 -142.83(11) . . . . ? C2 B3 B4 C1 35.09(9) . . . . ? B8 B3 B4 C1 97.17(11) . . . . ? B7 B3 B4 C1 134.83(12) . . . . ? C1 B3 B4 B7 -134.83(12) . . . . ? C2 B3 B4 B7 -99.74(12) . . . . ? B8 B3 B4 B7 -37.66(10) . . . . ? C1 B3 B4 B11 -96.10(12) . . . . ? C2 B3 B4 B11 -61.01(13) . . . . ? B8 B3 B4 B11 1.07(13) . . . . ? B7 B3 B4 B11 38.73(11) . . . . ? C1 B3 B4 B5 -32.67(9) . . . . ? C2 B3 B4 B5 2.41(13) . . . . ? B8 B3 B4 B5 64.49(12) . . . . ? B7 B3 B4 B5 102.16(12) . . . . ? C3 C1 B5 B10 -146.53(11) . . . . ? C2 C1 B5 B10 -2.30(13) . . . . ? B3 C1 B5 B10 65.81(14) . . . . ? B6 C1 B5 B10 -39.34(10) . . . . ? B4 C1 B5 B10 102.75(12) . . . . ? C3 C1 B5 B11 150.63(11) . . . . ? C2 C1 B5 B11 -65.14(14) . . . . ? B3 C1 B5 B11 2.98(15) . . . . ? B6 C1 B5 B11 -102.17(12) . . . . ? B4 C1 B5 B11 39.91(11) . . . . ? C3 C1 B5 B4 110.72(13) . . . . ? C2 C1 B5 B4 -105.05(11) . . . . ? B3 C1 B5 B4 -36.94(11) . . . . ? B6 C1 B5 B4 -142.09(11) . . . . ? C3 C1 B5 B6 -107.19(12) . . . . ? C2 C1 B5 B6 37.04(9) . . . . ? B3 C1 B5 B6 105.15(12) . . . . ? B4 C1 B5 B6 142.09(11) . . . . ? B7 B4 B5 C1 95.89(11) . . . . ? B11 B4 B5 C1 134.03(11) . . . . ? B3 B4 B5 C1 32.27(9) . . . . ? C1 B4 B5 B10 -96.29(11) . . . . ? B7 B4 B5 B10 -0.39(14) . . . . ? B11 B4 B5 B10 37.74(11) . . . . ? B3 B4 B5 B10 -64.02(13) . . . . ? C1 B4 B5 B11 -134.03(11) . . . . ? B7 B4 B5 B11 -38.13(11) . . . . ? B3 B4 B5 B11 -101.76(12) . . . . ? C1 B4 B5 B6 -32.96(9) . . . . ? B7 B4 B5 B6 62.93(12) . . . . ? B11 B4 B5 B6 101.06(12) . . . . ? B3 B4 B5 B6 -0.70(13) . . . . ? C3 C1 B6 C2 -105.37(11) . . . . ? B3 C1 B6 C2 32.79(9) . . . . ? B5 C1 B6 C2 140.75(10) . . . . ? B4 C1 B6 C2 103.73(11) . . . . ? C3 C1 B6 B9 -144.57(11) . . . . ? C2 C1 B6 B9 -39.19(9) . . . . ? B3 C1 B6 B9 -6.40(13) . . . . ? B5 C1 B6 B9 101.56(11) . . . . ? B4 C1 B6 B9 64.54(13) . . . . ? C3 C1 B6 B10 152.84(10) . . . . ? C2 C1 B6 B10 -101.79(10) . . . . ? B3 C1 B6 B10 -69.00(13) . . . . ? B5 C1 B6 B10 38.97(9) . . . . ? B4 C1 B6 B10 1.94(14) . . . . ? C3 C1 B6 B5 113.87(12) . . . . ? C2 C1 B6 B5 -140.75(10) . . . . ? B3 C1 B6 B5 -107.96(11) . . . . ? B4 C1 B6 B5 -37.02(10) . . . . ? B8 C2 B6 C1 -97.94(12) . . . . ? B9 C2 B6 C1 -134.84(10) . . . . ? B3 C2 B6 C1 -31.50(9) . . . . ? Li C2 B6 C1 94.92(11) . . . . ? C1 C2 B6 B9 134.84(10) . . . . ? B8 C2 B6 B9 36.90(11) . . . . ? B3 C2 B6 B9 103.34(11) . . . . ? Li C2 B6 B9 -130.24(12) . . . . ? C1 C2 B6 B10 96.80(12) . . . . ? B8 C2 B6 B10 -1.14(15) . . . . ? B9 C2 B6 B10 -38.04(11) . . . . ? B3 C2 B6 B10 65.30(13) . . . . ? Li C2 B6 B10 -168.28(11) . . . . ? C1 C2 B6 B5 34.42(9) . . . . ? B8 C2 B6 B5 -63.53(13) . . . . ? B9 C2 B6 B5 -100.42(11) . . . . ? B3 C2 B6 B5 2.92(13) . . . . ? Li C2 B6 B5 129.34(11) . . . . ? B10 B5 B6 C1 134.89(10) . . . . ? B11 B5 B6 C1 96.31(11) . . . . ? B4 B5 B6 C1 33.37(9) . . . . ? C1 B5 B6 C2 -34.66(9) . . . . ? B10 B5 B6 C2 100.23(11) . . . . ? B11 B5 B6 C2 61.65(13) . . . . ? B4 B5 B6 C2 -1.29(13) . . . . ? C1 B5 B6 B9 -97.23(11) . . . . ? B10 B5 B6 B9 37.67(10) . . . . ? B11 B5 B6 B9 -0.92(14) . . . . ? B4 B5 B6 B9 -63.85(13) . . . . ? C1 B5 B6 B10 -134.89(10) . . . . ? B11 B5 B6 B10 -38.59(10) . . . . ? B4 B5 B6 B10 -101.52(11) . . . . ? C1 B4 B7 B8 -0.92(14) . . . . ? B11 B4 B7 B8 -99.96(12) . . . . ? B5 B4 B7 B8 -62.22(13) . . . . ? B3 B4 B7 B8 37.28(10) . . . . ? C1 B4 B7 B12 62.56(13) . . . . ? B11 B4 B7 B12 -36.48(10) . . . . ? B5 B4 B7 B12 1.26(14) . . . . ? B3 B4 B7 B12 100.76(12) . . . . ? C1 B4 B7 B3 -38.20(9) . . . . ? B11 B4 B7 B3 -137.24(12) . . . . ? B5 B4 B7 B3 -99.50(12) . . . . ? C1 B4 B7 B11 99.04(12) . . . . ? B5 B4 B7 B11 37.74(10) . . . . ? B3 B4 B7 B11 137.24(12) . . . . ? C1 B3 B7 B4 38.65(10) . . . . ? C2 B3 B7 B4 100.06(11) . . . . ? B8 B3 B7 B4 137.68(12) . . . . ? C1 B3 B7 B8 -99.03(11) . . . . ? C2 B3 B7 B8 -37.62(10) . . . . ? B4 B3 B7 B8 -137.68(12) . . . . ? C1 B3 B7 B12 -61.71(14) . . . . ? C2 B3 B7 B12 -0.29(14) . . . . ? B8 B3 B7 B12 37.33(10) . . . . ? B4 B3 B7 B12 -100.36(12) . . . . ? C1 B3 B7 B11 0.68(15) . . . . ? C2 B3 B7 B11 62.10(14) . . . . ? B8 B3 B7 B11 99.72(13) . . . . ? B4 B3 B7 B11 -37.96(11) . . . . ? C1 C2 B8 B9 -100.58(10) . . . . ? B6 C2 B8 B9 -37.00(11) . . . . ? B3 C2 B8 B9 -140.30(11) . . . . ? Li C2 B8 B9 123.77(18) . . . . ? C1 C2 B8 B3 39.71(9) . . . . ? B6 C2 B8 B3 103.30(11) . . . . ? B9 C2 B8 B3 140.30(11) . . . . ? Li C2 B8 B3 -95.93(18) . . . . ? C1 C2 B8 B7 1.14(13) . . . . ? B6 C2 B8 B7 64.72(14) . . . . ? B9 C2 B8 B7 101.72(12) . . . . ? B3 C2 B8 B7 -38.58(10) . . . . ? Li C2 B8 B7 -134.51(16) . . . . ? C1 C2 B8 B12 -62.15(13) . . . . ? B6 C2 B8 B12 1.44(15) . . . . ? B9 C2 B8 B12 38.43(11) . . . . ? B3 C2 B8 B12 -101.86(12) . . . . ? Li C2 B8 B12 162.21(15) . . . . ? C1 B3 B8 C2 -38.87(9) . . . . ? B7 B3 B8 C2 -137.08(11) . . . . ? B4 B3 B8 C2 -99.99(10) . . . . ? C1 B3 B8 B9 -3.42(13) . . . . ? C2 B3 B8 B9 35.45(9) . . . . ? B7 B3 B8 B9 -101.63(12) . . . . ? B4 B3 B8 B9 -64.55(13) . . . . ? C1 B3 B8 B7 98.21(11) . . . . ? C2 B3 B8 B7 137.08(11) . . . . ? B4 B3 B8 B7 37.09(10) . . . . ? C1 B3 B8 B12 60.66(12) . . . . ? C2 B3 B8 B12 99.53(11) . . . . ? B7 B3 B8 B12 -37.55(10) . . . . ? B4 B3 B8 B12 -0.46(13) . . . . ? B4 B7 B8 C2 -0.12(15) . . . . ? B12 B7 B8 C2 -100.23(11) . . . . ? B3 B7 B8 C2 37.99(10) . . . . ? B11 B7 B8 C2 -62.89(13) . . . . ? B4 B7 B8 B9 62.87(14) . . . . ? B12 B7 B8 B9 -37.24(10) . . . . ? B3 B7 B8 B9 100.98(11) . . . . ? B11 B7 B8 B9 0.10(13) . . . . ? B4 B7 B8 B3 -38.11(10) . . . . ? B12 B7 B8 B3 -138.22(11) . . . . ? B11 B7 B8 B3 -100.88(11) . . . . ? B4 B7 B8 B12 100.11(12) . . . . ? B3 B7 B8 B12 138.22(11) . . . . ? B11 B7 B8 B12 37.34(10) . . . . ? C1 C2 B9 B8 100.39(11) . . . . ? B6 C2 B9 B8 140.31(11) . . . . ? B3 C2 B9 B8 37.00(10) . . . . ? Li C2 B9 B8 -132.69(14) . . . . ? C1 C2 B9 B6 -39.91(9) . . . . ? B8 C2 B9 B6 -140.31(11) . . . . ? B3 C2 B9 B6 -103.31(11) . . . . ? Li C2 B9 B6 87.01(14) . . . . ? C1 C2 B9 B10 -1.72(13) . . . . ? B8 C2 B9 B10 -102.12(12) . . . . ? B6 C2 B9 B10 38.19(10) . . . . ? B3 C2 B9 B10 -65.12(13) . . . . ? Li C2 B9 B10 125.19(13) . . . . ? C1 C2 B9 B12 61.72(12) . . . . ? B8 C2 B9 B12 -38.67(10) . . . . ? B6 C2 B9 B12 101.64(12) . . . . ? B3 C2 B9 B12 -1.67(13) . . . . ? Li C2 B9 B12 -171.36(12) . . . . ? B3 B8 B9 C2 -35.42(10) . . . . ? B7 B8 B9 C2 -99.89(11) . . . . ? B12 B8 B9 C2 -136.97(11) . . . . ? C2 B8 B9 B6 35.17(10) . . . . ? B3 B8 B9 B6 -0.25(14) . . . . ? B7 B8 B9 B6 -64.72(13) . . . . ? B12 B8 B9 B6 -101.81(12) . . . . ? C2 B8 B9 B10 99.42(11) . . . . ? B3 B8 B9 B10 64.00(13) . . . . ? B7 B8 B9 B10 -0.47(13) . . . . ? B12 B8 B9 B10 -37.56(10) . . . . ? C2 B8 B9 B12 136.97(11) . . . . ? B3 B8 B9 B12 101.55(12) . . . . ? B7 B8 B9 B12 37.08(10) . . . . ? C1 B6 B9 C2 39.04(9) . . . . ? B10 B6 B9 C2 137.39(11) . . . . ? B5 B6 B9 C2 100.19(11) . . . . ? C1 B6 B9 B8 3.83(13) . . . . ? C2 B6 B9 B8 -35.21(10) . . . . ? B10 B6 B9 B8 102.18(12) . . . . ? B5 B6 B9 B8 64.98(13) . . . . ? C1 B6 B9 B10 -98.35(11) . . . . ? C2 B6 B9 B10 -137.39(11) . . . . ? B5 B6 B9 B10 -37.20(10) . . . . ? C1 B6 B9 B12 -60.62(13) . . . . ? C2 B6 B9 B12 -99.66(12) . . . . ? B10 B6 B9 B12 37.73(11) . . . . ? B5 B6 B9 B12 0.53(14) . . . . ? C1 B5 B10 B9 1.10(14) . . . . ? B11 B5 B10 B9 99.90(12) . . . . ? B4 B5 B10 B9 62.55(13) . . . . ? B6 B5 B10 B9 -37.16(10) . . . . ? C1 B5 B10 B6 38.26(9) . . . . ? B11 B5 B10 B6 137.05(11) . . . . ? B4 B5 B10 B6 99.70(11) . . . . ? C1 B5 B10 B12 -62.08(13) . . . . ? B11 B5 B10 B12 36.72(10) . . . . ? B4 B5 B10 B12 -0.63(14) . . . . ? B6 B5 B10 B12 -100.33(11) . . . . ? C1 B5 B10 B11 -98.80(11) . . . . ? B4 B5 B10 B11 -37.35(10) . . . . ? B6 B5 B10 B11 -137.05(11) . . . . ? C2 B9 B10 B5 0.37(14) . . . . ? B8 B9 B10 B5 -62.34(13) . . . . ? B6 B9 B10 B5 37.89(10) . . . . ? B12 B9 B10 B5 -100.18(13) . . . . ? C2 B9 B10 B6 -37.53(10) . . . . ? B8 B9 B10 B6 -100.23(11) . . . . ? B12 B9 B10 B6 -138.07(12) . . . . ? C2 B9 B10 B12 100.54(12) . . . . ? B8 B9 B10 B12 37.84(10) . . . . ? B6 B9 B10 B12 138.07(12) . . . . ? C2 B9 B10 B11 63.36(12) . . . . ? B8 B9 B10 B11 0.66(13) . . . . ? B6 B9 B10 B11 100.89(12) . . . . ? B12 B9 B10 B11 -37.18(10) . . . . ? C1 B6 B10 B5 -38.60(9) . . . . ? C2 B6 B10 B5 -100.24(11) . . . . ? B9 B6 B10 B5 -137.86(11) . . . . ? C1 B6 B10 B9 99.26(11) . . . . ? C2 B6 B10 B9 37.63(10) . . . . ? B5 B6 B10 B9 137.86(11) . . . . ? C1 B6 B10 B12 62.01(13) . . . . ? C2 B6 B10 B12 0.38(15) . . . . ? B9 B6 B10 B12 -37.25(11) . . . . ? B5 B6 B10 B12 100.61(13) . . . . ? C1 B6 B10 B11 -0.39(13) . . . . ? C2 B6 B10 B11 -62.02(13) . . . . ? B9 B6 B10 B11 -99.64(12) . . . . ? B5 B6 B10 B11 38.22(10) . . . . ? C1 B4 B11 B12 -61.51(13) . . . . ? B7 B4 B11 B12 37.12(11) . . . . ? B5 B4 B11 B12 -100.91(13) . . . . ? B3 B4 B11 B12 -1.27(14) . . . . ? C1 B4 B11 B5 39.40(10) . . . . ? B7 B4 B11 B5 138.03(12) . . . . ? B3 B4 B11 B5 99.64(12) . . . . ? C1 B4 B11 B10 2.21(14) . . . . ? B7 B4 B11 B10 100.84(12) . . . . ? B5 B4 B11 B10 -37.19(10) . . . . ? B3 B4 B11 B10 62.45(13) . . . . ? C1 B4 B11 B7 -98.63(12) . . . . ? B5 B4 B11 B7 -138.03(12) . . . . ? B3 B4 B11 B7 -38.39(10) . . . . ? C1 B5 B11 B12 61.30(14) . . . . ? B10 B5 B11 B12 -37.37(11) . . . . ? B4 B5 B11 B12 100.77(12) . . . . ? B6 B5 B11 B12 0.95(15) . . . . ? C1 B5 B11 B4 -39.46(10) . . . . ? B10 B5 B11 B4 -138.14(11) . . . . ? B6 B5 B11 B4 -99.81(11) . . . . ? C1 B5 B11 B10 98.67(11) . . . . ? B4 B5 B11 B10 138.14(11) . . . . ? B6 B5 B11 B10 38.32(10) . . . . ? C1 B5 B11 B7 -2.29(15) . . . . ? B10 B5 B11 B7 -100.96(13) . . . . ? B4 B5 B11 B7 37.17(11) . . . . ? B6 B5 B11 B7 -62.64(14) . . . . ? B5 B10 B11 B12 138.36(11) . . . . ? B9 B10 B11 B12 37.51(10) . . . . ? B6 B10 B11 B12 99.73(12) . . . . ? B5 B10 B11 B4 37.47(10) . . . . ? B9 B10 B11 B4 -63.39(13) . . . . ? B6 B10 B11 B4 -1.16(14) . . . . ? B12 B10 B11 B4 -100.90(12) . . . . ? B9 B10 B11 B5 -100.86(11) . . . . ? B6 B10 B11 B5 -38.63(10) . . . . ? B12 B10 B11 B5 -138.36(11) . . . . ? B5 B10 B11 B7 100.27(11) . . . . ? B9 B10 B11 B7 -0.59(14) . . . . ? B6 B10 B11 B7 61.64(13) . . . . ? B12 B10 B11 B7 -38.10(10) . . . . ? B4 B7 B11 B12 -138.58(11) . . . . ? B8 B7 B11 B12 -37.84(10) . . . . ? B3 B7 B11 B12 -100.04(13) . . . . ? B8 B7 B11 B4 100.75(11) . . . . ? B12 B7 B11 B4 138.58(11) . . . . ? B3 B7 B11 B4 38.54(11) . . . . ? B4 B7 B11 B5 -37.52(11) . . . . ? B8 B7 B11 B5 63.23(14) . . . . ? B12 B7 B11 B5 101.07(13) . . . . ? B3 B7 B11 B5 1.02(16) . . . . ? B4 B7 B11 B10 -100.44(12) . . . . ? B8 B7 B11 B10 0.30(14) . . . . ? B12 B7 B11 B10 38.14(10) . . . . ? B3 B7 B11 B10 -61.90(14) . . . . ? B4 B11 B12 B9 63.02(14) . . . . ? B5 B11 B12 B9 -0.63(15) . . . . ? B10 B11 B12 B9 -37.67(10) . . . . ? B7 B11 B12 B9 99.80(12) . . . . ? B4 B11 B12 B7 -36.78(10) . . . . ? B5 B11 B12 B7 -100.42(12) . . . . ? B10 B11 B12 B7 -137.47(11) . . . . ? B4 B11 B12 B10 100.70(12) . . . . ? B5 B11 B12 B10 37.05(10) . . . . ? B7 B11 B12 B10 137.47(11) . . . . ? B4 B11 B12 B8 0.99(15) . . . . ? B5 B11 B12 B8 -62.66(14) . . . . ? B10 B11 B12 B8 -99.71(11) . . . . ? B7 B11 B12 B8 37.76(10) . . . . ? C2 B9 B12 B11 -62.49(13) . . . . ? B8 B9 B12 B11 -100.43(12) . . . . ? B6 B9 B12 B11 0.05(15) . . . . ? B10 B9 B12 B11 37.96(11) . . . . ? C2 B9 B12 B7 1.42(14) . . . . ? B8 B9 B12 B7 -36.52(11) . . . . ? B6 B9 B12 B7 63.96(13) . . . . ? B10 B9 B12 B7 101.87(12) . . . . ? C2 B9 B12 B10 -100.45(11) . . . . ? B8 B9 B12 B10 -138.39(12) . . . . ? B6 B9 B12 B10 -37.91(10) . . . . ? C2 B9 B12 B8 37.94(10) . . . . ? B6 B9 B12 B8 100.48(12) . . . . ? B10 B9 B12 B8 138.39(12) . . . . ? B4 B7 B12 B11 36.67(10) . . . . ? B8 B7 B12 B11 137.55(10) . . . . ? B3 B7 B12 B11 100.77(12) . . . . ? B4 B7 B12 B9 -64.79(14) . . . . ? B8 B7 B12 B9 36.09(10) . . . . ? B3 B7 B12 B9 -0.69(14) . . . . ? B11 B7 B12 B9 -101.46(12) . . . . ? B4 B7 B12 B10 -1.65(14) . . . . ? B8 B7 B12 B10 99.23(11) . . . . ? B3 B7 B12 B10 62.45(14) . . . . ? B11 B7 B12 B10 -38.32(10) . . . . ? B4 B7 B12 B8 -100.88(11) . . . . ? B3 B7 B12 B8 -36.78(10) . . . . ? B11 B7 B12 B8 -137.55(10) . . . . ? B5 B10 B12 B11 -36.98(10) . . . . ? B9 B10 B12 B11 -137.75(11) . . . . ? B6 B10 B12 B11 -100.89(12) . . . . ? B5 B10 B12 B9 100.77(12) . . . . ? B6 B10 B12 B9 36.86(11) . . . . ? B11 B10 B12 B9 137.75(11) . . . . ? B5 B10 B12 B7 1.41(14) . . . . ? B9 B10 B12 B7 -99.36(12) . . . . ? B6 B10 B12 B7 -62.50(14) . . . . ? B11 B10 B12 B7 38.40(10) . . . . ? B5 B10 B12 B8 64.38(14) . . . . ? B9 B10 B12 B8 -36.39(11) . . . . ? B6 B10 B12 B8 0.47(15) . . . . ? B11 B10 B12 B8 101.37(12) . . . . ? C2 B8 B12 B11 62.55(15) . . . . ? B9 B8 B12 B11 100.58(12) . . . . ? B3 B8 B12 B11 -0.32(14) . . . . ? B7 B8 B12 B11 -38.18(11) . . . . ? C2 B8 B12 B9 -38.03(10) . . . . ? B3 B8 B12 B9 -100.90(11) . . . . ? B7 B8 B12 B9 -138.77(11) . . . . ? C2 B8 B12 B7 100.74(12) . . . . ? B9 B8 B12 B7 138.77(11) . . . . ? B3 B8 B12 B7 37.86(10) . . . . ? C2 B8 B12 B10 -1.15(15) . . . . ? B9 B8 B12 B10 36.88(11) . . . . ? B3 B8 B12 B10 -64.02(14) . . . . ? B7 B8 B12 B10 -101.88(12) . . . . ? C16 O1 Li O1' -161(8) . . . . ? C19 O1 Li O1' 35(6) . . . . ? C16 O1 Li O2 108.0(11) . . . . ? C19 O1 Li O2 -56.7(12) . . . . ? C16 O1 Li O2' 107.5(11) . . . . ? C19 O1 Li O2' -57.1(12) . . . . ? C16 O1 Li N1 -114.7(10) . . . . ? C19 O1 Li N1 80.7(11) . . . . ? C16 O1 Li C2 -14.4(12) . . . . ? C19 O1 Li C2 -179.1(10) . . . . ? C19' O1' Li O1 -123(8) . . . . ? C16' O1' Li O1 34(6) . . . . ? C19' O1' Li O2 -33.0(17) . . . . ? C16' O1' Li O2 124.5(13) . . . . ? C19' O1' Li O2' -33.7(17) . . . . ? C16' O1' Li O2' 123.8(13) . . . . ? C19' O1' Li N1 100.4(16) . . . . ? C16' O1' Li N1 -102.1(13) . . . . ? C19' O1' Li C2 -158.7(13) . . . . ? C16' O1' Li C2 -1.2(16) . . . . ? C23 O2 Li O1 159.0(12) . . . . ? C20 O2 Li O1 -67.6(9) . . . . ? C23 O2 Li O1' 152.1(13) . . . . ? C20 O2 Li O1' -74.4(10) . . . . ? C23 O2 Li O2' 172(24) . . . . ? C20 O2 Li O2' -55(23) . . . . ? C23 O2 Li N1 21.6(14) . . . . ? C20 O2 Li N1 155.1(6) . . . . ? C23 O2 Li C2 -79.4(12) . . . . ? C20 O2 Li C2 54.0(9) . . . . ? C20' O2' Li O1 -40.5(13) . . . . ? C23' O2' Li O1 145.7(17) . . . . ? C20' O2' Li O1' -47.2(13) . . . . ? C23' O2' Li O1' 138.9(17) . . . . ? C20' O2' Li O2 152(25) . . . . ? C23' O2' Li O2 -21(22) . . . . ? C20' O2' Li N1 -177.3(9) . . . . ? C23' O2' Li N1 9(2) . . . . ? C20' O2' Li C2 80.2(13) . . . . ? C23' O2' Li C2 -93.6(17) . . . . ? C3 N1 Li O1 117.0(3) . . . . ? C4 N1 Li O1 -68.4(3) . . . . ? C3 N1 Li O1' 122.3(4) . . . . ? C4 N1 Li O1' -63.1(4) . . . . ? C3 N1 Li O2 -113.1(5) . . . . ? C4 N1 Li O2 61.4(5) . . . . ? C3 N1 Li O2' -114.3(6) . . . . ? C4 N1 Li O2' 60.3(6) . . . . ? C3 N1 Li C2 2.64(12) . . . . ? C4 N1 Li C2 177.21(9) . . . . ? C1 C2 Li O1 -126.3(5) . . . . ? B8 C2 Li O1 10.5(5) . . . . ? B6 C2 Li O1 171.8(5) . . . . ? B9 C2 Li O1 105.2(5) . . . . ? B3 C2 Li O1 -64.2(5) . . . . ? C1 C2 Li O1' -122.1(7) . . . . ? B8 C2 Li O1' 14.7(7) . . . . ? B6 C2 Li O1' 175.9(7) . . . . ? B9 C2 Li O1' 109.4(7) . . . . ? B3 C2 Li O1' -60.0(7) . . . . ? C1 C2 Li O2 117.8(3) . . . . ? B8 C2 Li O2 -105.4(3) . . . . ? B6 C2 Li O2 55.8(3) . . . . ? B9 C2 Li O2 -10.7(4) . . . . ? B3 C2 Li O2 179.9(3) . . . . ? C1 C2 Li O2' 119.8(4) . . . . ? B8 C2 Li O2' -103.4(4) . . . . ? B6 C2 Li O2' 57.8(4) . . . . ? B9 C2 Li O2' -8.7(4) . . . . ? B3 C2 Li O2' -178.1(4) . . . . ? C1 C2 Li N1 -4.36(10) . . . . ? B8 C2 Li N1 132.42(16) . . . . ? B6 C2 Li N1 -66.32(11) . . . . ? B9 C2 Li N1 -132.85(12) . . . . ? B3 C2 Li N1 57.77(11) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.272 _refine_diff_density_min -0.255 _refine_diff_density_rms 0.038 _database_code_depnum_ccdc_archive 'CCDC 963124' ####################################################################### # # 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_magd58 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H34 B10 N2' _chemical_formula_weight 350.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 6.6180(10) _cell_length_b 10.2110(18) _cell_length_c 15.859(3) _cell_angle_alpha 86.218(15) _cell_angle_beta 86.380(14) _cell_angle_gamma 77.332(14) _cell_volume 1042.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 29816 _cell_measurement_theta_min 4.4405 _cell_measurement_theta_max 75.6232 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.117 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 376 _exptl_absorpt_coefficient_mu 0.409 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9602 _exptl_absorpt_correction_T_max 0.9838 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Nova' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3543 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37066 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0091 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.44 _diffrn_reflns_theta_max 75.79 _reflns_number_total 4309 _reflns_number_gt 4244 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XP' _computing_publication_material SHELXL-97 _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^)+(0.0568P)^2^+0.3966P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4309 _refine_ls_number_parameters 252 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1094 _refine_ls_wR_factor_gt 0.1090 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group H1 H 0.457(3) 0.0022(17) 0.3224(11) 0.045(5) Uiso 1 1 d . . . N1 N 0.35611(14) 0.04329(10) 0.29039(6) 0.0229(2) Uani 1 1 d . . . N2 N 0.15358(13) -0.02524(9) 0.18631(5) 0.01843(19) Uani 1 1 d . . . C1 C 0.42712(15) -0.18643(10) 0.24764(6) 0.0158(2) Uani 1 1 d . . . C2 C 0.35945(16) -0.29572(10) 0.19078(6) 0.0183(2) Uani 1 1 d . . . H2 H 0.238(2) -0.2558(14) 0.1575(9) 0.027(3) Uiso 1 1 d . . . C3 C 0.29501(15) -0.04370(10) 0.23989(6) 0.0175(2) Uani 1 1 d . . . C4 C 0.21296(15) 0.15171(10) 0.33444(6) 0.0179(2) Uani 1 1 d . . . H4A H 0.1531 0.2236 0.2915 0.021 Uiso 1 1 calc R . . C5 C 0.03509(16) 0.10228(10) 0.38366(7) 0.0202(2) Uani 1 1 d . . . H5A H -0.0487 0.0689 0.3437 0.024 Uiso 1 1 calc R . . H5B H 0.0927 0.0266 0.4236 0.024 Uiso 1 1 calc R . . C6 C -0.10374(16) 0.21492(11) 0.43283(7) 0.0219(2) Uani 1 1 d . . . H6A H -0.1733 0.2862 0.3925 0.026 Uiso 1 1 calc R . . H6B H -0.2123 0.1788 0.4666 0.026 Uiso 1 1 calc R . . C7 C 0.02155(17) 0.27534(11) 0.49173(7) 0.0229(2) Uani 1 1 d . . . H7A H -0.0703 0.3522 0.5194 0.028 Uiso 1 1 calc R . . H7B H 0.0770 0.2070 0.5365 0.028 Uiso 1 1 calc R . . C8 C 0.20061(17) 0.32302(11) 0.44295(7) 0.0206(2) Uani 1 1 d . . . H8A H 0.2846 0.3557 0.4831 0.025 Uiso 1 1 calc R . . H8B H 0.1443 0.3990 0.4030 0.025 Uiso 1 1 calc R . . C9 C 0.33898(16) 0.21057(11) 0.39380(7) 0.0202(2) Uani 1 1 d . . . H9A H 0.4075 0.1387 0.4340 0.024 Uiso 1 1 calc R . . H9B H 0.4484 0.2463 0.3604 0.024 Uiso 1 1 calc R . . C10 C 0.03777(15) 0.10855(10) 0.15803(6) 0.0167(2) Uani 1 1 d . . . H10A H -0.0165 0.1621 0.2083 0.020 Uiso 1 1 calc R . . C11 C -0.14353(16) 0.09076(10) 0.10797(6) 0.0189(2) Uani 1 1 d . . . H11A H -0.2429 0.0535 0.1465 0.023 Uiso 1 1 calc R . . H11B H -0.0910 0.0255 0.0640 0.023 Uiso 1 1 calc R . . C12 C -0.25623(17) 0.22367(11) 0.06575(7) 0.0213(2) Uani 1 1 d . . . H12A H -0.3648 0.2065 0.0304 0.026 Uiso 1 1 calc R . . H12B H -0.3250 0.2849 0.1099 0.026 Uiso 1 1 calc R . . C13 C -0.10629(18) 0.29102(11) 0.01069(7) 0.0239(2) Uani 1 1 d . . . H13A H -0.0484 0.2341 -0.0370 0.029 Uiso 1 1 calc R . . H13B H -0.1822 0.3788 -0.0132 0.029 Uiso 1 1 calc R . . C14 C 0.07034(17) 0.31255(11) 0.06186(7) 0.0236(2) Uani 1 1 d . . . H14A H 0.0138 0.3763 0.1063 0.028 Uiso 1 1 calc R . . H14B H 0.1687 0.3524 0.0242 0.028 Uiso 1 1 calc R . . C15 C 0.18507(16) 0.17950(11) 0.10307(7) 0.0211(2) Uani 1 1 d . . . H15A H 0.2932 0.1969 0.1385 0.025 Uiso 1 1 calc R . . H15B H 0.2547 0.1197 0.0584 0.025 Uiso 1 1 calc R . . B3 B 0.58117(18) -0.24029(12) 0.15922(7) 0.0181(2) Uani 1 1 d . . . H3 H 0.6016 -0.1759 0.1007 0.022 Uiso 1 1 calc R . . B4 B 0.69022(17) -0.22086(12) 0.25641(7) 0.0176(2) Uani 1 1 d . . . H4 H 0.7843 -0.1433 0.2619 0.021 Uiso 1 1 calc R . . B5 B 0.52094(18) -0.26115(12) 0.34088(7) 0.0178(2) Uani 1 1 d . . . H5 H 0.5047 -0.2095 0.4019 0.021 Uiso 1 1 calc R . . B6 B 0.30428(18) -0.30452(12) 0.29828(7) 0.0189(2) Uani 1 1 d . . . H6 H 0.1452 -0.2815 0.3298 0.023 Uiso 1 1 calc R . . B7 B 0.78367(18) -0.36792(12) 0.19896(7) 0.0190(2) Uani 1 1 d . . . H7 H 0.9418 -0.3890 0.1665 0.023 Uiso 1 1 calc R . . B8 B 0.74679(18) -0.38117(12) 0.31182(7) 0.0179(2) Uani 1 1 d . . . H8 H 0.8811 -0.4112 0.3537 0.021 Uiso 1 1 calc R . . B9 B 0.50803(18) -0.43227(12) 0.33762(7) 0.0190(2) Uani 1 1 d . . . H9 H 0.4847 -0.4955 0.3963 0.023 Uiso 1 1 calc R . . B10 B 0.39750(19) -0.45146(12) 0.24077(8) 0.0206(2) Uani 1 1 d . . . H10 H 0.2993 -0.5265 0.2348 0.025 Uiso 1 1 calc R . . B11 B 0.56706(19) -0.41175(12) 0.15533(7) 0.0199(2) Uani 1 1 d . . . H11 H 0.5793 -0.4610 0.0936 0.024 Uiso 1 1 calc R . . B12 B 0.67092(18) -0.49891(12) 0.24937(7) 0.0192(2) Uani 1 1 d . . . H12 H 0.7553 -0.6068 0.2499 0.023 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 N1 0.0177(4) 0.0230(5) 0.0273(5) -0.0080(4) -0.0060(4) 0.0007(4) N2 0.0186(4) 0.0169(4) 0.0188(4) 0.0010(3) -0.0035(3) -0.0015(3) C1 0.0150(4) 0.0178(5) 0.0140(4) -0.0001(4) -0.0018(4) -0.0025(4) C2 0.0181(5) 0.0185(5) 0.0179(5) -0.0008(4) -0.0030(4) -0.0021(4) C3 0.0155(5) 0.0172(5) 0.0193(5) -0.0018(4) 0.0002(4) -0.0023(4) C4 0.0171(5) 0.0184(5) 0.0179(5) -0.0037(4) -0.0020(4) -0.0020(4) C5 0.0214(5) 0.0207(5) 0.0200(5) -0.0004(4) -0.0038(4) -0.0070(4) C6 0.0197(5) 0.0276(6) 0.0184(5) -0.0001(4) -0.0002(4) -0.0055(4) C7 0.0253(5) 0.0270(6) 0.0162(5) -0.0030(4) -0.0002(4) -0.0048(4) C8 0.0244(5) 0.0202(5) 0.0182(5) -0.0028(4) -0.0034(4) -0.0058(4) C9 0.0187(5) 0.0219(5) 0.0209(5) -0.0030(4) -0.0042(4) -0.0047(4) C10 0.0172(5) 0.0161(5) 0.0158(5) 0.0002(4) -0.0026(4) -0.0012(4) C11 0.0199(5) 0.0186(5) 0.0179(5) 0.0007(4) -0.0040(4) -0.0033(4) C12 0.0211(5) 0.0212(5) 0.0201(5) 0.0013(4) -0.0056(4) -0.0008(4) C13 0.0294(6) 0.0207(5) 0.0188(5) 0.0037(4) -0.0020(4) -0.0002(4) C14 0.0260(6) 0.0191(5) 0.0248(5) 0.0031(4) 0.0018(4) -0.0049(4) C15 0.0184(5) 0.0209(5) 0.0232(5) 0.0014(4) 0.0002(4) -0.0035(4) B3 0.0181(5) 0.0195(5) 0.0151(5) 0.0004(4) 0.0003(4) -0.0013(4) B4 0.0141(5) 0.0192(5) 0.0188(5) 0.0009(4) -0.0020(4) -0.0028(4) B5 0.0170(5) 0.0197(5) 0.0155(5) 0.0030(4) -0.0024(4) -0.0022(4) B6 0.0168(5) 0.0217(6) 0.0179(5) 0.0017(4) -0.0002(4) -0.0049(4) B7 0.0169(5) 0.0196(5) 0.0183(5) 0.0005(4) 0.0005(4) -0.0001(4) B8 0.0162(5) 0.0190(5) 0.0175(5) 0.0013(4) -0.0029(4) -0.0019(4) B9 0.0192(5) 0.0193(5) 0.0182(5) 0.0027(4) -0.0019(4) -0.0041(4) B10 0.0207(6) 0.0189(5) 0.0227(6) 0.0007(4) -0.0045(4) -0.0051(4) B11 0.0220(6) 0.0182(5) 0.0178(5) -0.0013(4) -0.0031(4) 0.0003(4) B12 0.0199(6) 0.0178(5) 0.0187(5) 0.0002(4) -0.0031(4) -0.0014(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C3 1.3734(14) . ? N1 C4 1.4730(13) . ? N1 H1 0.878(18) . ? N2 C3 1.2788(14) . ? N2 C10 1.4691(13) . ? C1 C3 1.5279(14) . ? C1 C2 1.6316(14) . ? C1 B5 1.7068(15) . ? C1 B4 1.7118(15) . ? C1 B6 1.7262(15) . ? C1 B3 1.7274(15) . ? C2 B11 1.6982(16) . ? C2 B10 1.7041(16) . ? C2 B3 1.7200(16) . ? C2 B6 1.7215(16) . ? C2 H2 0.986(14) . ? C4 C9 1.5287(14) . ? C4 C5 1.5305(14) . ? C4 H4A 1.0000 . ? C5 C6 1.5295(15) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.5293(15) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.5255(15) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.5269(15) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.5291(14) . ? C10 C15 1.5343(14) . ? C10 H10A 1.0000 . ? C11 C12 1.5316(14) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.5267(15) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.5263(16) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.5305(15) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? B3 B7 1.7675(16) . ? B3 B11 1.7789(17) . ? B3 B4 1.7832(16) . ? B3 H3 1.1200 . ? B4 B5 1.7773(16) . ? B4 B7 1.7804(17) . ? B4 B8 1.7819(16) . ? B4 H4 1.1200 . ? B5 B8 1.7699(16) . ? B5 B9 1.7723(17) . ? B5 B6 1.7745(16) . ? B5 H5 1.1200 . ? B6 B9 1.7710(17) . ? B6 B10 1.7796(17) . ? B6 H6 1.1200 . ? B7 B11 1.7837(17) . ? B7 B12 1.7907(17) . ? B7 B8 1.7914(17) . ? B7 H7 1.1200 . ? B8 B12 1.7785(17) . ? B8 B9 1.7855(16) . ? B8 H8 1.1200 . ? B9 B10 1.7824(17) . ? B9 B12 1.7881(17) . ? B9 H9 1.1200 . ? B10 B12 1.7792(17) . ? B10 B11 1.7874(17) . ? B10 H10 1.1200 . ? B11 B12 1.7818(17) . ? B11 H11 1.1200 . ? B12 H12 1.1200 . ? 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 C3 N1 C4 124.40(9) . . ? C3 N1 H1 111.9(11) . . ? C4 N1 H1 111.6(11) . . ? C3 N2 C10 123.23(9) . . ? C3 C1 C2 115.61(8) . . ? C3 C1 B5 123.25(8) . . ? C2 C1 B5 110.55(8) . . ? C3 C1 B4 123.22(8) . . ? C2 C1 B4 110.91(8) . . ? B5 C1 B4 62.65(6) . . ? C3 C1 B6 115.25(8) . . ? C2 C1 B6 61.61(6) . . ? B5 C1 B6 62.25(6) . . ? B4 C1 B6 114.52(8) . . ? C3 C1 B3 115.83(8) . . ? C2 C1 B3 61.52(6) . . ? B5 C1 B3 114.22(8) . . ? B4 C1 B3 62.46(6) . . ? B6 C1 B3 114.94(8) . . ? C1 C2 B11 112.12(8) . . ? C1 C2 B10 111.99(8) . . ? B11 C2 B10 63.38(7) . . ? C1 C2 B3 61.98(6) . . ? B11 C2 B3 62.72(7) . . ? B10 C2 B3 115.47(8) . . ? C1 C2 B6 61.90(6) . . ? B11 C2 B6 115.42(8) . . ? B10 C2 B6 62.60(7) . . ? B3 C2 B6 115.58(8) . . ? C1 C2 H2 112.4(8) . . ? B11 C2 H2 124.5(8) . . ? B10 C2 H2 124.0(8) . . ? B3 C2 H2 114.7(8) . . ? B6 C2 H2 113.8(8) . . ? N2 C3 N1 131.59(10) . . ? N2 C3 C1 115.24(9) . . ? N1 C3 C1 113.11(9) . . ? N1 C4 C9 107.78(8) . . ? N1 C4 C5 112.31(9) . . ? C9 C4 C5 110.70(8) . . ? N1 C4 H4A 108.7 . . ? C9 C4 H4A 108.7 . . ? C5 C4 H4A 108.7 . . ? C6 C5 C4 111.15(9) . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5A 109.4 . . ? C6 C5 H5B 109.4 . . ? C4 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C7 C6 C5 111.31(9) . . ? C7 C6 H6A 109.4 . . ? C5 C6 H6A 109.4 . . ? C7 C6 H6B 109.4 . . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C8 C7 C6 111.03(9) . . ? C8 C7 H7A 109.4 . . ? C6 C7 H7A 109.4 . . ? C8 C7 H7B 109.4 . . ? C6 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? C7 C8 C9 111.64(9) . . ? C7 C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? C7 C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? C8 C9 C4 111.05(9) . . ? C8 C9 H9A 109.4 . . ? C4 C9 H9A 109.4 . . ? C8 C9 H9B 109.4 . . ? C4 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? N2 C10 C11 108.29(8) . . ? N2 C10 C15 108.58(8) . . ? C11 C10 C15 111.22(8) . . ? N2 C10 H10A 109.6 . . ? C11 C10 H10A 109.6 . . ? C15 C10 H10A 109.6 . . ? C10 C11 C12 112.01(8) . . ? C10 C11 H11A 109.2 . . ? C12 C11 H11A 109.2 . . ? C10 C11 H11B 109.2 . . ? C12 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? C13 C12 C11 111.35(9) . . ? C13 C12 H12A 109.4 . . ? C11 C12 H12A 109.4 . . ? C13 C12 H12B 109.4 . . ? C11 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? C14 C13 C12 111.06(9) . . ? C14 C13 H13A 109.4 . . ? C12 C13 H13A 109.4 . . ? C14 C13 H13B 109.4 . . ? C12 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? C13 C14 C15 110.85(9) . . ? C13 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C14 C15 C10 111.89(9) . . ? C14 C15 H15A 109.2 . . ? C10 C15 H15A 109.2 . . ? C14 C15 H15B 109.2 . . ? C10 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C2 B3 C1 56.50(6) . . ? C2 B3 B7 104.14(8) . . ? C1 B3 B7 104.52(8) . . ? C2 B3 B11 58.04(6) . . ? C1 B3 B11 103.98(8) . . ? B7 B3 B11 60.39(7) . . ? C2 B3 B4 103.65(8) . . ? C1 B3 B4 58.34(6) . . ? B7 B3 B4 60.19(7) . . ? B11 B3 B4 108.02(8) . . ? C2 B3 H3 125.4 . . ? C1 B3 H3 125.0 . . ? B7 B3 H3 122.8 . . ? B11 B3 H3 122.2 . . ? B4 B3 H3 122.3 . . ? C1 B4 B5 58.54(6) . . ? C1 B4 B7 104.63(8) . . ? B5 B4 B7 107.92(8) . . ? C1 B4 B8 104.43(8) . . ? B5 B4 B8 59.64(7) . . ? B7 B4 B8 60.38(7) . . ? C1 B4 B3 59.20(6) . . ? B5 B4 B3 108.18(8) . . ? B7 B4 B3 59.47(7) . . ? B8 B4 B3 107.94(8) . . ? C1 B4 H4 124.8 . . ? B5 B4 H4 121.6 . . ? B7 B4 H4 122.4 . . ? B8 B4 H4 122.5 . . ? B3 B4 H4 121.4 . . ? C1 B5 B8 105.16(8) . . ? C1 B5 B9 105.38(8) . . ? B8 B5 B9 60.54(7) . . ? C1 B5 B6 59.41(6) . . ? B8 B5 B6 108.62(8) . . ? B9 B5 B6 59.91(7) . . ? C1 B5 B4 58.81(6) . . ? B8 B5 B4 60.31(6) . . ? B9 B5 B4 109.00(8) . . ? B6 B5 B4 109.01(8) . . ? C1 B5 H5 124.4 . . ? B8 B5 H5 122.0 . . ? B9 B5 H5 121.9 . . ? B6 B5 H5 121.0 . . ? B4 B5 H5 120.9 . . ? C2 B6 C1 56.49(6) . . ? C2 B6 B9 104.18(8) . . ? C1 B6 B9 104.61(8) . . ? C2 B6 B5 103.43(8) . . ? C1 B6 B5 58.34(6) . . ? B9 B6 B5 59.98(7) . . ? C2 B6 B10 58.23(6) . . ? C1 B6 B10 104.15(8) . . ? B9 B6 B10 60.27(7) . . ? B5 B6 B10 107.65(8) . . ? C2 B6 H6 125.4 . . ? C1 B6 H6 124.9 . . ? B9 B6 H6 122.8 . . ? B5 B6 H6 122.6 . . ? B10 B6 H6 122.2 . . ? B3 B7 B4 60.35(6) . . ? B3 B7 B11 60.12(7) . . ? B4 B7 B11 107.94(8) . . ? B3 B7 B12 108.05(8) . . ? B4 B7 B12 107.49(8) . . ? B11 B7 B12 59.80(7) . . ? B3 B7 B8 108.21(8) . . ? B4 B7 B8 59.85(6) . . ? B11 B7 B8 107.47(8) . . ? B12 B7 B8 59.54(6) . . ? B3 B7 H7 121.3 . . ? B4 B7 H7 121.8 . . ? B11 B7 H7 121.9 . . ? B12 B7 H7 122.1 . . ? B8 B7 H7 122.0 . . ? B5 B8 B12 107.72(8) . . ? B5 B8 B4 60.05(6) . . ? B12 B8 B4 107.96(8) . . ? B5 B8 B9 59.80(7) . . ? B12 B8 B9 60.23(7) . . ? B4 B8 B9 108.21(8) . . ? B5 B8 B7 107.76(8) . . ? B12 B8 B7 60.21(7) . . ? B4 B8 B7 59.77(6) . . ? B9 B8 B7 108.47(8) . . ? B5 B8 H8 122.0 . . ? B12 B8 H8 121.7 . . ? B4 B8 H8 121.7 . . ? B9 B8 H8 121.4 . . ? B7 B8 H8 121.6 . . ? B6 B9 B5 60.11(6) . . ? B6 B9 B10 60.11(7) . . ? B5 B9 B10 107.63(8) . . ? B6 B9 B8 108.08(8) . . ? B5 B9 B8 59.67(6) . . ? B10 B9 B8 107.62(8) . . ? B6 B9 B12 107.92(8) . . ? B5 B9 B12 107.19(8) . . ? B10 B9 B12 59.77(7) . . ? B8 B9 B12 59.69(7) . . ? B6 B9 H9 121.5 . . ? B5 B9 H9 122.1 . . ? B10 B9 H9 121.9 . . ? B8 B9 H9 121.9 . . ? B12 B9 H9 122.1 . . ? C2 B10 B12 103.92(8) . . ? C2 B10 B6 59.18(6) . . ? B12 B10 B6 107.93(8) . . ? C2 B10 B9 104.41(8) . . ? B12 B10 B9 60.27(7) . . ? B6 B10 B9 59.63(7) . . ? C2 B10 B11 58.15(6) . . ? B12 B10 B11 59.94(7) . . ? B6 B10 B11 108.28(8) . . ? B9 B10 B11 108.25(8) . . ? C2 B10 H10 125.2 . . ? B12 B10 H10 122.6 . . ? B6 B10 H10 121.3 . . ? B9 B10 H10 122.3 . . ? B11 B10 H10 121.4 . . ? C2 B11 B3 59.24(6) . . ? C2 B11 B12 104.06(8) . . ? B3 B11 B12 107.94(8) . . ? C2 B11 B7 104.36(8) . . ? B3 B11 B7 59.49(7) . . ? B12 B11 B7 60.30(7) . . ? C2 B11 B10 58.47(7) . . ? B3 B11 B10 108.56(8) . . ? B12 B11 B10 59.80(7) . . ? B7 B11 B10 108.19(8) . . ? C2 B11 H11 125.1 . . ? B3 B11 H11 121.2 . . ? B12 B11 H11 122.6 . . ? B7 B11 H11 122.5 . . ? B10 B11 H11 121.3 . . ? B8 B12 B10 108.07(8) . . ? B8 B12 B11 108.13(8) . . ? B10 B12 B11 60.26(7) . . ? B8 B12 B9 60.08(7) . . ? B10 B12 B9 59.96(7) . . ? B11 B12 B9 108.25(8) . . ? B8 B12 B7 60.25(7) . . ? B10 B12 B7 108.24(8) . . ? B11 B12 B7 59.90(7) . . ? B9 B12 B7 108.39(8) . . ? B8 B12 H12 121.6 . . ? B10 B12 H12 121.6 . . ? B11 B12 H12 121.6 . . ? B9 B12 H12 121.6 . . ? B7 B12 H12 121.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 C1 C2 B11 145.87(9) . . . . ? B5 C1 C2 B11 -68.13(10) . . . . ? B4 C1 C2 B11 -0.59(11) . . . . ? B6 C1 C2 B11 -107.95(9) . . . . ? B3 C1 C2 B11 39.03(8) . . . . ? C3 C1 C2 B10 -145.08(9) . . . . ? B5 C1 C2 B10 0.93(11) . . . . ? B4 C1 C2 B10 68.47(10) . . . . ? B6 C1 C2 B10 -38.90(8) . . . . ? B3 C1 C2 B10 108.09(9) . . . . ? C3 C1 C2 B3 106.84(9) . . . . ? B5 C1 C2 B3 -107.16(8) . . . . ? B4 C1 C2 B3 -39.62(8) . . . . ? B6 C1 C2 B3 -146.98(8) . . . . ? C3 C1 C2 B6 -106.18(9) . . . . ? B5 C1 C2 B6 39.83(8) . . . . ? B4 C1 C2 B6 107.37(8) . . . . ? B3 C1 C2 B6 146.98(8) . . . . ? C10 N2 C3 N1 9.28(18) . . . . ? C10 N2 C3 C1 -168.01(8) . . . . ? C4 N1 C3 N2 39.41(18) . . . . ? C4 N1 C3 C1 -143.26(10) . . . . ? C2 C1 C3 N2 -3.50(13) . . . . ? B5 C1 C3 N2 -144.74(10) . . . . ? B4 C1 C3 N2 138.40(10) . . . . ? B6 C1 C3 N2 -72.59(11) . . . . ? B3 C1 C3 N2 65.68(12) . . . . ? C2 C1 C3 N1 178.71(8) . . . . ? B5 C1 C3 N1 37.46(13) . . . . ? B4 C1 C3 N1 -39.40(13) . . . . ? B6 C1 C3 N1 109.62(10) . . . . ? B3 C1 C3 N1 -112.12(10) . . . . ? C3 N1 C4 C9 171.58(10) . . . . ? C3 N1 C4 C5 49.39(14) . . . . ? N1 C4 C5 C6 176.70(8) . . . . ? C9 C4 C5 C6 56.18(11) . . . . ? C4 C5 C6 C7 -55.76(11) . . . . ? C5 C6 C7 C8 54.92(12) . . . . ? C6 C7 C8 C9 -55.06(12) . . . . ? C7 C8 C9 C4 55.84(12) . . . . ? N1 C4 C9 C8 -179.26(8) . . . . ? C5 C4 C9 C8 -56.07(11) . . . . ? C3 N2 C10 C11 -169.37(9) . . . . ? C3 N2 C10 C15 69.75(12) . . . . ? N2 C10 C11 C12 -172.32(8) . . . . ? C15 C10 C11 C12 -53.09(11) . . . . ? C10 C11 C12 C13 54.50(12) . . . . ? C11 C12 C13 C14 -56.03(12) . . . . ? C12 C13 C14 C15 56.51(12) . . . . ? C13 C14 C15 C10 -55.62(12) . . . . ? N2 C10 C15 C14 172.84(8) . . . . ? C11 C10 C15 C14 53.79(11) . . . . ? B11 C2 B3 C1 -138.98(8) . . . . ? B10 C2 B3 C1 -102.49(9) . . . . ? B6 C2 B3 C1 -32.20(8) . . . . ? C1 C2 B3 B7 98.24(8) . . . . ? B11 C2 B3 B7 -40.73(7) . . . . ? B10 C2 B3 B7 -4.25(11) . . . . ? B6 C2 B3 B7 66.04(10) . . . . ? C1 C2 B3 B11 138.98(8) . . . . ? B10 C2 B3 B11 36.48(8) . . . . ? B6 C2 B3 B11 106.78(9) . . . . ? C1 C2 B3 B4 36.05(7) . . . . ? B11 C2 B3 B4 -102.93(8) . . . . ? B10 C2 B3 B4 -66.45(10) . . . . ? B6 C2 B3 B4 3.85(11) . . . . ? C3 C1 B3 C2 -106.48(9) . . . . ? B5 C1 B3 C2 101.18(9) . . . . ? B4 C1 B3 C2 137.80(8) . . . . ? B6 C1 B3 C2 31.91(8) . . . . ? C3 C1 B3 B7 155.98(8) . . . . ? C2 C1 B3 B7 -97.54(8) . . . . ? B5 C1 B3 B7 3.64(11) . . . . ? B4 C1 B3 B7 40.26(8) . . . . ? B6 C1 B3 B7 -65.63(10) . . . . ? C3 C1 B3 B11 -141.50(8) . . . . ? C2 C1 B3 B11 -35.02(7) . . . . ? B5 C1 B3 B11 66.16(10) . . . . ? B4 C1 B3 B11 102.77(8) . . . . ? B6 C1 B3 B11 -3.11(10) . . . . ? C3 C1 B3 B4 115.72(9) . . . . ? C2 C1 B3 B4 -137.80(8) . . . . ? B5 C1 B3 B4 -36.61(8) . . . . ? B6 C1 B3 B4 -105.88(9) . . . . ? C3 C1 B4 B5 113.53(10) . . . . ? C2 C1 B4 B5 -103.03(9) . . . . ? B6 C1 B4 B5 -35.69(8) . . . . ? B3 C1 B4 B5 -142.24(8) . . . . ? C3 C1 B4 B7 -144.16(9) . . . . ? C2 C1 B4 B7 -0.72(10) . . . . ? B5 C1 B4 B7 102.31(8) . . . . ? B6 C1 B4 B7 66.62(10) . . . . ? B3 C1 B4 B7 -39.93(7) . . . . ? C3 C1 B4 B8 153.24(9) . . . . ? C2 C1 B4 B8 -63.32(9) . . . . ? B5 C1 B4 B8 39.71(7) . . . . ? B6 C1 B4 B8 4.02(10) . . . . ? B3 C1 B4 B8 -102.53(8) . . . . ? C3 C1 B4 B3 -104.23(10) . . . . ? C2 C1 B4 B3 39.21(8) . . . . ? B5 C1 B4 B3 142.24(8) . . . . ? B6 C1 B4 B3 106.55(9) . . . . ? C2 B3 B4 C1 -35.20(7) . . . . ? B7 B3 B4 C1 -133.86(8) . . . . ? B11 B3 B4 C1 -95.61(9) . . . . ? C2 B3 B4 B5 -1.85(10) . . . . ? C1 B3 B4 B5 33.35(7) . . . . ? B7 B3 B4 B5 -100.51(9) . . . . ? B11 B3 B4 B5 -62.26(10) . . . . ? C2 B3 B4 B7 98.66(8) . . . . ? C1 B3 B4 B7 133.86(8) . . . . ? B11 B3 B4 B7 38.25(8) . . . . ? C2 B3 B4 B8 61.22(9) . . . . ? C1 B3 B4 B8 96.42(8) . . . . ? B7 B3 B4 B8 -37.44(8) . . . . ? B11 B3 B4 B8 0.81(10) . . . . ? C3 C1 B5 B8 -153.67(9) . . . . ? C2 C1 B5 B8 63.41(10) . . . . ? B4 C1 B5 B8 -40.20(7) . . . . ? B6 C1 B5 B8 102.95(9) . . . . ? B3 C1 B5 B8 -3.65(11) . . . . ? C3 C1 B5 B9 143.33(9) . . . . ? C2 C1 B5 B9 0.41(10) . . . . ? B4 C1 B5 B9 -103.20(9) . . . . ? B6 C1 B5 B9 39.95(7) . . . . ? B3 C1 B5 B9 -66.66(10) . . . . ? C3 C1 B5 B6 103.38(10) . . . . ? C2 C1 B5 B6 -39.54(8) . . . . ? B4 C1 B5 B6 -143.15(8) . . . . ? B3 C1 B5 B6 -106.61(9) . . . . ? C3 C1 B5 B4 -113.48(10) . . . . ? C2 C1 B5 B4 103.60(9) . . . . ? B6 C1 B5 B4 143.15(8) . . . . ? B3 C1 B5 B4 36.54(8) . . . . ? B7 B4 B5 C1 -96.50(8) . . . . ? B8 B4 B5 C1 -134.18(8) . . . . ? B3 B4 B5 C1 -33.62(7) . . . . ? C1 B4 B5 B8 134.18(8) . . . . ? B7 B4 B5 B8 37.68(8) . . . . ? B3 B4 B5 B8 100.57(9) . . . . ? C1 B4 B5 B9 96.86(9) . . . . ? B7 B4 B5 B9 0.36(10) . . . . ? B8 B4 B5 B9 -37.33(8) . . . . ? B3 B4 B5 B9 63.24(10) . . . . ? C1 B4 B5 B6 33.10(7) . . . . ? B7 B4 B5 B6 -63.40(10) . . . . ? B8 B4 B5 B6 -101.09(9) . . . . ? B3 B4 B5 B6 -0.52(11) . . . . ? B11 C2 B6 C1 102.64(9) . . . . ? B10 C2 B6 C1 139.02(8) . . . . ? B3 C2 B6 C1 32.23(8) . . . . ? C1 C2 B6 B9 -98.33(8) . . . . ? B11 C2 B6 B9 4.32(11) . . . . ? B10 C2 B6 B9 40.69(8) . . . . ? B3 C2 B6 B9 -66.10(10) . . . . ? C1 C2 B6 B5 -36.37(7) . . . . ? B11 C2 B6 B5 66.27(10) . . . . ? B10 C2 B6 B5 102.64(8) . . . . ? B3 C2 B6 B5 -4.15(11) . . . . ? C1 C2 B6 B10 -139.02(8) . . . . ? B11 C2 B6 B10 -36.37(8) . . . . ? B3 C2 B6 B10 -106.79(9) . . . . ? C3 C1 B6 C2 106.75(9) . . . . ? B5 C1 B6 C2 -137.34(8) . . . . ? B4 C1 B6 C2 -101.50(9) . . . . ? B3 C1 B6 C2 -31.88(8) . . . . ? C3 C1 B6 B9 -155.72(8) . . . . ? C2 C1 B6 B9 97.53(8) . . . . ? B5 C1 B6 B9 -39.81(7) . . . . ? B4 C1 B6 B9 -3.98(11) . . . . ? B3 C1 B6 B9 65.64(10) . . . . ? C3 C1 B6 B5 -115.91(9) . . . . ? C2 C1 B6 B5 137.34(8) . . . . ? B4 C1 B6 B5 35.84(8) . . . . ? B3 C1 B6 B5 105.46(9) . . . . ? C3 C1 B6 B10 141.85(8) . . . . ? C2 C1 B6 B10 35.10(7) . . . . ? B5 C1 B6 B10 -102.24(8) . . . . ? B4 C1 B6 B10 -66.40(10) . . . . ? B3 C1 B6 B10 3.21(10) . . . . ? C1 B5 B6 C2 35.51(7) . . . . ? B8 B5 B6 C2 -61.46(10) . . . . ? B9 B5 B6 C2 -98.80(8) . . . . ? B4 B5 B6 C2 2.65(10) . . . . ? B8 B5 B6 C1 -96.97(8) . . . . ? B9 B5 B6 C1 -134.31(8) . . . . ? B4 B5 B6 C1 -32.87(7) . . . . ? C1 B5 B6 B9 134.31(8) . . . . ? B8 B5 B6 B9 37.34(8) . . . . ? B4 B5 B6 B9 101.44(9) . . . . ? C1 B5 B6 B10 96.03(8) . . . . ? B8 B5 B6 B10 -0.94(10) . . . . ? B9 B5 B6 B10 -38.28(8) . . . . ? B4 B5 B6 B10 63.16(10) . . . . ? C2 B3 B7 B4 -97.83(8) . . . . ? C1 B3 B7 B4 -39.34(7) . . . . ? B11 B3 B7 B4 -137.38(8) . . . . ? C2 B3 B7 B11 39.55(7) . . . . ? C1 B3 B7 B11 98.04(8) . . . . ? B4 B3 B7 B11 137.38(8) . . . . ? C2 B3 B7 B12 2.44(10) . . . . ? C1 B3 B7 B12 60.92(10) . . . . ? B11 B3 B7 B12 -37.12(8) . . . . ? B4 B3 B7 B12 100.26(9) . . . . ? C2 B3 B7 B8 -60.56(10) . . . . ? C1 B3 B7 B8 -2.07(10) . . . . ? B11 B3 B7 B8 -100.11(9) . . . . ? B4 B3 B7 B8 37.27(8) . . . . ? C1 B4 B7 B3 39.79(7) . . . . ? B5 B4 B7 B3 100.94(8) . . . . ? B8 B4 B7 B3 138.30(8) . . . . ? C1 B4 B7 B11 1.69(10) . . . . ? B5 B4 B7 B11 62.84(10) . . . . ? B8 B4 B7 B11 100.19(9) . . . . ? B3 B4 B7 B11 -38.11(8) . . . . ? C1 B4 B7 B12 -61.42(9) . . . . ? B5 B4 B7 B12 -0.27(10) . . . . ? B8 B4 B7 B12 37.08(7) . . . . ? B3 B4 B7 B12 -101.22(9) . . . . ? C1 B4 B7 B8 -98.50(8) . . . . ? B5 B4 B7 B8 -37.35(7) . . . . ? B3 B4 B7 B8 -138.30(8) . . . . ? C1 B5 B8 B12 -61.46(10) . . . . ? B9 B5 B8 B12 37.89(8) . . . . ? B6 B5 B8 B12 0.82(10) . . . . ? B4 B5 B8 B12 -100.93(8) . . . . ? C1 B5 B8 B4 39.46(7) . . . . ? B9 B5 B8 B4 138.82(8) . . . . ? B6 B5 B8 B4 101.75(9) . . . . ? C1 B5 B8 B9 -99.35(8) . . . . ? B6 B5 B8 B9 -37.07(8) . . . . ? B4 B5 B8 B9 -138.82(8) . . . . ? C1 B5 B8 B7 2.09(10) . . . . ? B9 B5 B8 B7 101.45(9) . . . . ? B6 B5 B8 B7 64.38(10) . . . . ? B4 B5 B8 B7 -37.37(8) . . . . ? C1 B4 B8 B5 -39.17(7) . . . . ? B7 B4 B8 B5 -138.01(8) . . . . ? B3 B4 B8 B5 -100.97(8) . . . . ? C1 B4 B8 B12 61.34(10) . . . . ? B5 B4 B8 B12 100.51(9) . . . . ? B7 B4 B8 B12 -37.49(8) . . . . ? B3 B4 B8 B12 -0.46(10) . . . . ? C1 B4 B8 B9 -2.36(10) . . . . ? B5 B4 B8 B9 36.80(8) . . . . ? B7 B4 B8 B9 -101.20(9) . . . . ? B3 B4 B8 B9 -64.17(10) . . . . ? C1 B4 B8 B7 98.84(8) . . . . ? B5 B4 B8 B7 138.01(8) . . . . ? B3 B4 B8 B7 37.03(8) . . . . ? B3 B7 B8 B5 0.01(11) . . . . ? B4 B7 B8 B5 37.50(7) . . . . ? B11 B7 B8 B5 -63.49(10) . . . . ? B12 B7 B8 B5 -100.65(9) . . . . ? B3 B7 B8 B12 100.66(9) . . . . ? B4 B7 B8 B12 138.15(8) . . . . ? B11 B7 B8 B12 37.16(8) . . . . ? B3 B7 B8 B4 -37.49(8) . . . . ? B11 B7 B8 B4 -100.99(8) . . . . ? B12 B7 B8 B4 -138.15(8) . . . . ? B3 B7 B8 B9 63.27(10) . . . . ? B4 B7 B8 B9 100.76(9) . . . . ? B11 B7 B8 B9 -0.24(10) . . . . ? B12 B7 B8 B9 -37.39(8) . . . . ? C2 B6 B9 B5 97.51(8) . . . . ? C1 B6 B9 B5 39.01(7) . . . . ? B10 B6 B9 B5 137.17(8) . . . . ? C2 B6 B9 B10 -39.67(7) . . . . ? C1 B6 B9 B10 -98.16(8) . . . . ? B5 B6 B9 B10 -137.17(8) . . . . ? C2 B6 B9 B8 60.68(10) . . . . ? C1 B6 B9 B8 2.18(10) . . . . ? B5 B6 B9 B8 -36.83(8) . . . . ? B10 B6 B9 B8 100.35(9) . . . . ? C2 B6 B9 B12 -2.43(10) . . . . ? C1 B6 B9 B12 -60.92(10) . . . . ? B5 B6 B9 B12 -99.93(9) . . . . ? B10 B6 B9 B12 37.24(8) . . . . ? C1 B5 B9 B6 -39.71(7) . . . . ? B8 B5 B9 B6 -138.69(8) . . . . ? B4 B5 B9 B6 -101.46(9) . . . . ? C1 B5 B9 B10 -1.51(10) . . . . ? B8 B5 B9 B10 -100.49(9) . . . . ? B6 B5 B9 B10 38.20(8) . . . . ? B4 B5 B9 B10 -63.26(10) . . . . ? C1 B5 B9 B8 98.98(8) . . . . ? B6 B5 B9 B8 138.69(8) . . . . ? B4 B5 B9 B8 37.23(7) . . . . ? C1 B5 B9 B12 61.45(9) . . . . ? B8 B5 B9 B12 -37.53(7) . . . . ? B6 B5 B9 B12 101.16(9) . . . . ? B4 B5 B9 B12 -0.30(10) . . . . ? B5 B8 B9 B6 37.02(8) . . . . ? B12 B8 B9 B6 -100.60(9) . . . . ? B4 B8 B9 B6 0.10(11) . . . . ? B7 B8 B9 B6 -63.22(10) . . . . ? B12 B8 B9 B5 -137.62(8) . . . . ? B4 B8 B9 B5 -36.91(8) . . . . ? B7 B8 B9 B5 -100.23(9) . . . . ? B5 B8 B9 B10 100.50(9) . . . . ? B12 B8 B9 B10 -37.12(8) . . . . ? B4 B8 B9 B10 63.59(10) . . . . ? B7 B8 B9 B10 0.27(10) . . . . ? B5 B8 B9 B12 137.62(8) . . . . ? B4 B8 B9 B12 100.71(9) . . . . ? B7 B8 B9 B12 37.39(8) . . . . ? C1 C2 B10 B12 -64.19(10) . . . . ? B11 C2 B10 B12 40.40(8) . . . . ? B3 C2 B10 B12 4.16(11) . . . . ? B6 C2 B10 B12 -102.79(9) . . . . ? C1 C2 B10 B6 38.60(8) . . . . ? B11 C2 B10 B6 143.19(8) . . . . ? B3 C2 B10 B6 106.96(9) . . . . ? C1 C2 B10 B9 -1.82(11) . . . . ? B11 C2 B10 B9 102.77(9) . . . . ? B3 C2 B10 B9 66.53(10) . . . . ? B6 C2 B10 B9 -40.43(8) . . . . ? C1 C2 B10 B11 -104.59(9) . . . . ? B3 C2 B10 B11 -36.24(8) . . . . ? B6 C2 B10 B11 -143.19(8) . . . . ? C1 B6 B10 C2 -34.33(7) . . . . ? B9 B6 B10 C2 -133.28(8) . . . . ? B5 B6 B10 C2 -95.13(8) . . . . ? C2 B6 B10 B12 95.82(9) . . . . ? C1 B6 B10 B12 61.49(10) . . . . ? B9 B6 B10 B12 -37.46(8) . . . . ? B5 B6 B10 B12 0.69(10) . . . . ? C2 B6 B10 B9 133.28(8) . . . . ? C1 B6 B10 B9 98.95(8) . . . . ? B5 B6 B10 B9 38.15(8) . . . . ? C2 B6 B10 B11 32.41(7) . . . . ? C1 B6 B10 B11 -1.92(10) . . . . ? B9 B6 B10 B11 -100.88(9) . . . . ? B5 B6 B10 B11 -62.73(10) . . . . ? B6 B9 B10 C2 40.20(7) . . . . ? B5 B9 B10 C2 2.00(10) . . . . ? B8 B9 B10 C2 -60.93(10) . . . . ? B12 B9 B10 C2 -98.01(9) . . . . ? B6 B9 B10 B12 138.21(8) . . . . ? B5 B9 B10 B12 100.01(9) . . . . ? B8 B9 B10 B12 37.08(8) . . . . ? B5 B9 B10 B6 -38.20(8) . . . . ? B8 B9 B10 B6 -101.13(9) . . . . ? B12 B9 B10 B6 -138.21(8) . . . . ? B6 B9 B10 B11 100.93(9) . . . . ? B5 B9 B10 B11 62.73(10) . . . . ? B8 B9 B10 B11 -0.20(11) . . . . ? B12 B9 B10 B11 -37.28(8) . . . . ? C1 C2 B11 B3 -38.72(8) . . . . ? B10 C2 B11 B3 -143.10(8) . . . . ? B6 C2 B11 B3 -107.02(9) . . . . ? C1 C2 B11 B12 64.02(10) . . . . ? B10 C2 B11 B12 -40.36(8) . . . . ? B3 C2 B11 B12 102.74(9) . . . . ? B6 C2 B11 B12 -4.28(11) . . . . ? C1 C2 B11 B7 1.61(10) . . . . ? B10 C2 B11 B7 -102.77(9) . . . . ? B3 C2 B11 B7 40.33(7) . . . . ? B6 C2 B11 B7 -66.69(10) . . . . ? C1 C2 B11 B10 104.38(9) . . . . ? B3 C2 B11 B10 143.10(8) . . . . ? B6 C2 B11 B10 36.08(8) . . . . ? C1 B3 B11 C2 34.34(7) . . . . ? B7 B3 B11 C2 133.30(8) . . . . ? B4 B3 B11 C2 95.14(8) . . . . ? C2 B3 B11 B12 -95.99(9) . . . . ? C1 B3 B11 B12 -61.66(10) . . . . ? B7 B3 B11 B12 37.31(8) . . . . ? B4 B3 B11 B12 -0.85(11) . . . . ? C2 B3 B11 B7 -133.30(8) . . . . ? C1 B3 B11 B7 -98.96(8) . . . . ? B4 B3 B11 B7 -38.16(8) . . . . ? C2 B3 B11 B10 -32.67(7) . . . . ? C1 B3 B11 B10 1.66(10) . . . . ? B7 B3 B11 B10 100.62(9) . . . . ? B4 B3 B11 B10 62.47(10) . . . . ? B3 B7 B11 C2 -40.21(7) . . . . ? B4 B7 B11 C2 -2.00(10) . . . . ? B12 B7 B11 C2 98.20(9) . . . . ? B8 B7 B11 C2 61.16(10) . . . . ? B4 B7 B11 B3 38.21(8) . . . . ? B12 B7 B11 B3 138.41(8) . . . . ? B8 B7 B11 B3 101.37(9) . . . . ? B3 B7 B11 B12 -138.41(8) . . . . ? B4 B7 B11 B12 -100.20(9) . . . . ? B8 B7 B11 B12 -37.04(8) . . . . ? B3 B7 B11 B10 -101.25(9) . . . . ? B4 B7 B11 B10 -63.05(10) . . . . ? B12 B7 B11 B10 37.15(8) . . . . ? B8 B7 B11 B10 0.11(10) . . . . ? B12 B10 B11 C2 -133.38(8) . . . . ? B6 B10 B11 C2 -32.81(8) . . . . ? B9 B10 B11 C2 -95.95(9) . . . . ? C2 B10 B11 B3 32.97(8) . . . . ? B12 B10 B11 B3 -100.41(9) . . . . ? B6 B10 B11 B3 0.17(11) . . . . ? B9 B10 B11 B3 -62.98(10) . . . . ? C2 B10 B11 B12 133.38(8) . . . . ? B6 B10 B11 B12 100.57(9) . . . . ? B9 B10 B11 B12 37.43(8) . . . . ? C2 B10 B11 B7 96.01(9) . . . . ? B12 B10 B11 B7 -37.37(8) . . . . ? B6 B10 B11 B7 63.20(10) . . . . ? B9 B10 B11 B7 0.06(11) . . . . ? B5 B8 B12 B10 -0.39(10) . . . . ? B4 B8 B12 B10 -63.82(10) . . . . ? B9 B8 B12 B10 37.31(8) . . . . ? B7 B8 B12 B10 -101.11(9) . . . . ? B5 B8 B12 B11 63.36(10) . . . . ? B4 B8 B12 B11 -0.07(11) . . . . ? B9 B8 B12 B11 101.06(9) . . . . ? B7 B8 B12 B11 -37.36(8) . . . . ? B5 B8 B12 B9 -37.70(7) . . . . ? B4 B8 B12 B9 -101.12(9) . . . . ? B7 B8 B12 B9 -138.42(8) . . . . ? B5 B8 B12 B7 100.72(8) . . . . ? B4 B8 B12 B7 37.30(7) . . . . ? B9 B8 B12 B7 138.42(8) . . . . ? C2 B10 B12 B8 61.48(10) . . . . ? B6 B10 B12 B8 -0.19(11) . . . . ? B9 B10 B12 B8 -37.36(8) . . . . ? B11 B10 B12 B8 100.98(9) . . . . ? C2 B10 B12 B11 -39.50(7) . . . . ? B6 B10 B12 B11 -101.17(9) . . . . ? B9 B10 B12 B11 -138.34(8) . . . . ? C2 B10 B12 B9 98.84(9) . . . . ? B6 B10 B12 B9 37.18(8) . . . . ? B11 B10 B12 B9 138.34(8) . . . . ? C2 B10 B12 B7 -2.29(10) . . . . ? B6 B10 B12 B7 -63.95(10) . . . . ? B9 B10 B12 B7 -101.13(9) . . . . ? B11 B10 B12 B7 37.21(8) . . . . ? C2 B11 B12 B8 -61.19(10) . . . . ? B3 B11 B12 B8 0.57(11) . . . . ? B7 B11 B12 B8 37.52(8) . . . . ? B10 B11 B12 B8 -100.89(9) . . . . ? C2 B11 B12 B10 39.69(8) . . . . ? B3 B11 B12 B10 101.45(9) . . . . ? B7 B11 B12 B10 138.40(8) . . . . ? C2 B11 B12 B9 2.40(11) . . . . ? B3 B11 B12 B9 64.16(10) . . . . ? B7 B11 B12 B9 101.11(9) . . . . ? B10 B11 B12 B9 -37.29(8) . . . . ? C2 B11 B12 B7 -98.71(8) . . . . ? B3 B11 B12 B7 -36.95(8) . . . . ? B10 B11 B12 B7 -138.40(8) . . . . ? B6 B9 B12 B8 100.88(9) . . . . ? B5 B9 B12 B8 37.51(7) . . . . ? B10 B9 B12 B8 138.27(8) . . . . ? B6 B9 B12 B10 -37.39(8) . . . . ? B5 B9 B12 B10 -100.75(9) . . . . ? B8 B9 B12 B10 -138.27(8) . . . . ? B6 B9 B12 B11 0.04(11) . . . . ? B5 B9 B12 B11 -63.33(10) . . . . ? B10 B9 B12 B11 37.42(8) . . . . ? B8 B9 B12 B11 -100.85(9) . . . . ? B6 B9 B12 B7 63.50(10) . . . . ? B5 B9 B12 B7 0.13(10) . . . . ? B10 B9 B12 B7 100.88(9) . . . . ? B8 B9 B12 B7 -37.39(8) . . . . ? B3 B7 B12 B8 -100.93(9) . . . . ? B4 B7 B12 B8 -37.22(7) . . . . ? B11 B7 B12 B8 -138.19(8) . . . . ? B3 B7 B12 B10 -0.11(11) . . . . ? B4 B7 B12 B10 63.60(10) . . . . ? B11 B7 B12 B10 -37.37(8) . . . . ? B8 B7 B12 B10 100.82(9) . . . . ? B3 B7 B12 B11 37.26(8) . . . . ? B4 B7 B12 B11 100.97(9) . . . . ? B8 B7 B12 B11 138.19(8) . . . . ? B3 B7 B12 B9 -63.62(10) . . . . ? B4 B7 B12 B9 0.09(10) . . . . ? B11 B7 B12 B9 -100.88(9) . . . . ? B8 B7 B12 B9 37.31(8) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 75.79 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.380 _refine_diff_density_min -0.267 _refine_diff_density_rms 0.039 _database_code_depnum_ccdc_archive 'CCDC 963125' ####################################################################### # # 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_ip245 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H44 B10 Li2 N2 O4' _chemical_formula_weight 462.52 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' Li Li -0.0003 0.0001 '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' 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 P2(1)2(1)2(1) 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' _cell_length_a 10.182(2) _cell_length_b 13.527(3) _cell_length_c 20.850(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2871.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 28777 _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 29.48 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.070 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 0.064 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(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 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30080 _diffrn_reflns_av_R_equivalents 0.0697 _diffrn_reflns_av_sigmaI/netI 0.0604 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 29.24 _reflns_number_total 7686 _reflns_number_gt 6224 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0516P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.3(8) _refine_ls_number_reflns 7686 _refine_ls_number_parameters 372 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0764 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1092 _refine_ls_wR_factor_gt 0.1037 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.42136(14) 0.10598(10) 0.85286(6) 0.0214(3) Uani 1 1 d . . . N2 N 0.56987(13) 0.09798(10) 0.76056(6) 0.0208(3) Uani 1 1 d . . . C1 C 0.62824(16) 0.02290(11) 0.85929(7) 0.0182(3) Uani 1 1 d . . . C2 C 0.57690(18) -0.02189(13) 0.93050(7) 0.0239(3) Uani 1 1 d . . . C3 C 0.52728(16) 0.08312(11) 0.81974(7) 0.0182(3) Uani 1 1 d . . . C4 C 0.33369(18) 0.18516(14) 0.83105(8) 0.0271(4) Uani 1 1 d . . . H4A H 0.3077(19) 0.1781(14) 0.7856(9) 0.025(5) Uiso 1 1 d . . . C5 C 0.4029(2) 0.28468(15) 0.83705(11) 0.0392(5) Uani 1 1 d . . . H5A H 0.4820 0.2847 0.8103 0.059 Uiso 1 1 calc R . . H5B H 0.4274 0.2959 0.8819 0.059 Uiso 1 1 calc R . . H5C H 0.3436 0.3374 0.8228 0.059 Uiso 1 1 calc R . . C6 C 0.20987(19) 0.18319(17) 0.87146(10) 0.0375(5) Uani 1 1 d . . . H6A H 0.2324 0.1961 0.9164 0.056 Uiso 1 1 calc R . . H6B H 0.1682 0.1181 0.8679 0.056 Uiso 1 1 calc R . . H6C H 0.1490 0.2341 0.8562 0.056 Uiso 1 1 calc R . . C7 C 0.47811(18) 0.12351(13) 0.70899(7) 0.0231(3) Uani 1 1 d . . . H7A H 0.4373(18) 0.1859(14) 0.7154(8) 0.014(4) Uiso 1 1 d . . . C8 C 0.37369(19) 0.04359(15) 0.70136(9) 0.0313(4) Uani 1 1 d . . . H8A H 0.3272 0.0347 0.7421 0.047 Uiso 1 1 calc R . . H8B H 0.4157 -0.0187 0.6890 0.047 Uiso 1 1 calc R . . H8C H 0.3110 0.0635 0.6681 0.047 Uiso 1 1 calc R . . C9 C 0.5551(2) 0.13316(15) 0.64648(8) 0.0328(4) Uani 1 1 d . . . H9A H 0.5964 0.0697 0.6362 0.049 Uiso 1 1 calc R . . H9B H 0.6230 0.1839 0.6514 0.049 Uiso 1 1 calc R . . H9C H 0.4952 0.1520 0.6118 0.049 Uiso 1 1 calc R . . C10 C 0.2206(2) 0.07748(16) 1.03910(9) 0.0370(5) Uani 1 1 d . . . H10A H 0.1588 0.1195 1.0146 0.044 Uiso 1 1 calc R . . H10B H 0.2052 0.0883 1.0854 0.044 Uiso 1 1 calc R . . C11 C 0.2006(2) -0.02886(16) 1.02247(9) 0.0376(5) Uani 1 1 d . . . H11A H 0.2560 -0.0713 1.0501 0.045 Uiso 1 1 calc R . . H11B H 0.1075 -0.0476 1.0289 0.045 Uiso 1 1 calc R . . C12 C 0.3896(2) 0.19951(16) 1.03999(11) 0.0433(5) Uani 1 1 d . . . H12A H 0.3804 0.2082 1.0864 0.065 Uiso 1 1 calc R . . H12B H 0.3327 0.2468 1.0177 0.065 Uiso 1 1 calc R . . H12C H 0.4812 0.2110 1.0276 0.065 Uiso 1 1 calc R . . C13 C 0.2326(2) -0.14151(15) 0.93714(11) 0.0417(5) Uani 1 1 d . . . H13A H 0.1427 -0.1668 0.9412 0.063 Uiso 1 1 calc R . . H13B H 0.2915 -0.1807 0.9642 0.063 Uiso 1 1 calc R . . H13C H 0.2609 -0.1463 0.8923 0.063 Uiso 1 1 calc R . . C14 C 0.9611(2) 0.22036(17) 0.70909(15) 0.0542(7) Uani 1 1 d . . . H14A H 1.0029 0.2095 0.7514 0.065 Uiso 1 1 calc R . . H14B H 0.9979 0.2814 0.6901 0.065 Uiso 1 1 calc R . . C15 C 0.9856(2) 0.13479(18) 0.66632(14) 0.0577(7) Uani 1 1 d . . . H15A H 0.9534 0.1492 0.6225 0.069 Uiso 1 1 calc R . . H15B H 1.0809 0.1206 0.6640 0.069 Uiso 1 1 calc R . . C16 C 0.7811(3) 0.31437(16) 0.74921(11) 0.0452(5) Uani 1 1 d . . . H16A H 0.8206 0.3731 0.7296 0.068 Uiso 1 1 calc R . . H16B H 0.8082 0.3100 0.7942 0.068 Uiso 1 1 calc R . . H16C H 0.6852 0.3192 0.7468 0.068 Uiso 1 1 calc R . . C17 C 0.9529(2) -0.03786(17) 0.66316(10) 0.0457(5) Uani 1 1 d . . . H17A H 1.0480 -0.0476 0.6670 0.069 Uiso 1 1 calc R . . H17B H 0.9286 -0.0361 0.6177 0.069 Uiso 1 1 calc R . . H17C H 0.9070 -0.0925 0.6844 0.069 Uiso 1 1 calc R . . O1 O 0.35272(13) 0.10157(10) 1.02297(6) 0.0312(3) Uani 1 1 d . . . O2 O 0.23629(12) -0.04073(10) 0.95706(6) 0.0292(3) Uani 1 1 d . . . O3 O 0.82342(13) 0.22893(10) 0.71603(6) 0.0319(3) Uani 1 1 d . . . O4 O 0.91741(14) 0.05234(10) 0.69249(6) 0.0363(3) Uani 1 1 d . . . B3 B 0.68423(19) 0.07461(15) 0.92794(9) 0.0234(4) Uani 1 1 d . . . H3 H 0.654(2) 0.1486(17) 0.9420(10) 0.042(6) Uiso 1 1 d . . . B4 B 0.79025(19) 0.05518(15) 0.86078(9) 0.0227(4) Uani 1 1 d . . . H4 H 0.823(2) 0.1215(15) 0.8341(9) 0.031(5) Uiso 1 1 d . . . B5 B 0.73844(19) -0.05463(14) 0.82264(9) 0.0219(4) Uani 1 1 d . . . H5 H 0.738(2) -0.0595(14) 0.7725(9) 0.029(5) Uiso 1 1 d . . . B6 B 0.59976(19) -0.09985(15) 0.86624(9) 0.0242(4) Uani 1 1 d . . . H6 H 0.514(2) -0.1315(14) 0.8408(8) 0.027(5) Uiso 1 1 d . . . B7 B 0.7094(2) -0.02386(18) 0.98118(10) 0.0317(5) Uani 1 1 d . . . H7 H 0.691(2) -0.0116(16) 1.0316(10) 0.040(6) Uiso 1 1 d . . . B8 B 0.8455(2) 0.02506(16) 0.93892(10) 0.0283(4) Uani 1 1 d . . . H8 H 0.925(2) 0.0668(15) 0.9619(9) 0.033(5) Uiso 1 1 d . . . B9 B 0.8775(2) -0.05626(15) 0.87327(10) 0.0266(4) Uani 1 1 d . . . H9 H 0.971(2) -0.0665(14) 0.8535(9) 0.026(5) Uiso 1 1 d . . . B10 B 0.7590(2) -0.15411(15) 0.87656(11) 0.0289(4) Uani 1 1 d . . . H10 H 0.774(2) -0.2284(16) 0.8590(10) 0.038(6) Uiso 1 1 d . . . B11 B 0.6558(2) -0.13213(16) 0.94328(10) 0.0299(5) Uani 1 1 d . . . H11 H 0.604(2) -0.1912(16) 0.9690(10) 0.038(6) Uiso 1 1 d . . . B12 B 0.8274(2) -0.10569(18) 0.94842(11) 0.0330(5) Uani 1 1 d . . . H12 H 0.892(2) -0.1475(17) 0.9809(11) 0.047(6) Uiso 1 1 d . . . Li1 Li 0.3920(3) 0.0404(2) 0.93695(13) 0.0249(6) Uani 1 1 d . . . Li2 Li 0.7534(3) 0.0954(2) 0.73447(14) 0.0312(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0194(7) 0.0220(7) 0.0229(6) 0.0055(5) 0.0026(5) 0.0033(6) N2 0.0190(7) 0.0233(7) 0.0201(6) 0.0020(5) 0.0015(5) -0.0021(6) C1 0.0175(8) 0.0177(8) 0.0194(7) 0.0005(6) 0.0047(6) 0.0001(6) C2 0.0232(9) 0.0264(9) 0.0221(7) 0.0069(6) 0.0039(7) 0.0043(7) C3 0.0182(7) 0.0144(8) 0.0222(7) 0.0009(6) -0.0017(6) -0.0027(6) C4 0.0248(9) 0.0299(10) 0.0267(8) 0.0066(7) 0.0026(7) 0.0099(8) C5 0.0411(12) 0.0249(10) 0.0516(12) 0.0080(8) 0.0046(10) 0.0084(9) C6 0.0254(10) 0.0442(12) 0.0430(11) 0.0132(9) 0.0084(8) 0.0155(9) C7 0.0239(9) 0.0246(9) 0.0209(7) 0.0027(6) 0.0010(6) -0.0007(7) C8 0.0298(10) 0.0345(11) 0.0296(8) -0.0013(7) -0.0064(8) -0.0058(8) C9 0.0372(11) 0.0400(11) 0.0211(8) 0.0018(7) 0.0001(8) -0.0053(9) C10 0.0330(10) 0.0510(13) 0.0271(8) 0.0028(8) 0.0124(8) 0.0087(9) C11 0.0343(11) 0.0461(13) 0.0325(9) 0.0116(9) 0.0108(8) -0.0028(9) C12 0.0492(14) 0.0384(12) 0.0424(11) -0.0134(9) 0.0013(10) 0.0044(10) C13 0.0410(12) 0.0330(11) 0.0510(12) 0.0020(9) 0.0017(10) -0.0059(10) C14 0.0279(12) 0.0346(12) 0.1001(19) 0.0166(12) 0.0134(13) -0.0082(9) C15 0.0436(13) 0.0411(13) 0.0885(18) 0.0230(12) 0.0397(14) 0.0092(11) C16 0.0539(14) 0.0328(12) 0.0491(12) -0.0100(9) 0.0079(11) -0.0060(10) C17 0.0479(14) 0.0437(13) 0.0456(11) -0.0020(10) 0.0047(10) 0.0151(11) O1 0.0289(7) 0.0338(7) 0.0309(6) -0.0049(5) 0.0046(5) 0.0051(6) O2 0.0265(7) 0.0321(7) 0.0290(6) 0.0052(5) 0.0050(5) -0.0024(6) O3 0.0267(7) 0.0297(7) 0.0393(7) -0.0013(5) 0.0082(6) -0.0047(6) O4 0.0322(7) 0.0300(7) 0.0468(8) 0.0033(6) 0.0167(6) 0.0012(6) B3 0.0202(10) 0.0269(11) 0.0232(8) -0.0042(7) -0.0008(7) 0.0040(8) B4 0.0183(9) 0.0223(10) 0.0276(9) -0.0027(7) 0.0022(7) 0.0006(7) B5 0.0201(9) 0.0193(9) 0.0263(8) -0.0034(7) 0.0060(7) 0.0022(7) B6 0.0212(9) 0.0180(9) 0.0332(9) 0.0007(7) 0.0043(8) 0.0004(7) B7 0.0294(11) 0.0398(13) 0.0258(9) 0.0046(9) -0.0019(8) 0.0095(9) B8 0.0222(10) 0.0307(11) 0.0320(9) -0.0022(8) -0.0057(8) 0.0060(9) B9 0.0192(9) 0.0245(10) 0.0361(10) -0.0023(8) 0.0020(8) 0.0044(8) B10 0.0227(10) 0.0189(10) 0.0452(11) 0.0018(8) 0.0046(9) 0.0041(8) B11 0.0221(10) 0.0287(11) 0.0390(11) 0.0138(8) 0.0027(9) 0.0063(9) B12 0.0251(11) 0.0325(12) 0.0415(11) 0.0085(9) -0.0031(9) 0.0075(9) Li1 0.0241(15) 0.0266(15) 0.0239(12) 0.0041(11) 0.0040(11) 0.0034(13) Li2 0.0305(16) 0.0285(16) 0.0346(15) 0.0014(12) 0.0092(13) -0.0024(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C3 1.317(2) . ? N1 C4 1.467(2) . ? N1 Li1 1.988(3) . ? N2 C3 1.3232(19) . ? N2 C7 1.466(2) . ? N2 Li2 1.947(3) . ? C1 C3 1.549(2) . ? C1 C2 1.687(2) . ? C1 B6 1.692(3) . ? C1 B3 1.692(2) . ? C1 B4 1.707(3) . ? C1 B5 1.715(2) . ? C2 B3 1.703(3) . ? C2 B7 1.714(3) . ? C2 B11 1.715(3) . ? C2 B6 1.721(3) . ? C2 Li1 2.067(3) . ? C4 C6 1.517(3) . ? C4 C5 1.525(3) . ? C4 H4A 0.988(19) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.525(3) . ? C7 C9 1.526(2) . ? C7 H7A 0.950(18) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 O1 1.424(2) . ? C10 C11 1.494(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 O2 1.421(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O1 1.422(2) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 O2 1.426(2) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 O3 1.414(3) . ? C14 C15 1.482(4) . ? C14 Li2 2.759(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O4 1.423(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O3 1.414(2) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 O4 1.412(2) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? O1 Li1 2.015(3) . ? O2 Li1 1.973(3) . ? O3 Li2 1.980(3) . ? O4 Li2 1.973(3) . ? B3 B7 1.753(3) . ? B3 B4 1.788(3) . ? B3 B8 1.788(3) . ? B3 H3 1.09(2) . ? B4 B5 1.766(3) . ? B4 B9 1.769(3) . ? B4 B8 1.771(3) . ? B4 Li2 2.715(4) . ? B4 H4 1.11(2) . ? B5 B10 1.766(3) . ? B5 B9 1.766(3) . ? B5 B6 1.787(3) . ? B5 Li2 2.742(4) . ? B5 H5 1.046(19) . ? B6 B11 1.760(3) . ? B6 B10 1.792(3) . ? B6 H6 1.11(2) . ? B7 B11 1.751(3) . ? B7 B8 1.771(3) . ? B7 B12 1.771(3) . ? B7 H7 1.08(2) . ? B8 B9 1.786(3) . ? B8 B12 1.789(3) . ? B8 H8 1.10(2) . ? B9 B12 1.778(3) . ? B9 B10 1.793(3) . ? B9 H9 1.05(2) . ? B10 B11 1.768(3) . ? B10 B12 1.778(3) . ? B10 H10 1.08(2) . ? B11 B12 1.787(3) . ? B11 H11 1.10(2) . ? B12 H12 1.10(2) . ? Li2 H4 2.22(2) . ? Li2 H5 2.25(2) . ? 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 C3 N1 C4 120.47(13) . . ? C3 N1 Li1 118.74(13) . . ? C4 N1 Li1 120.53(13) . . ? C3 N2 C7 120.72(13) . . ? C3 N2 Li2 124.92(14) . . ? C7 N2 Li2 114.29(13) . . ? C3 C1 C2 116.85(13) . . ? C3 C1 B6 116.61(13) . . ? C2 C1 B6 61.24(10) . . ? C3 C1 B3 117.15(13) . . ? C2 C1 B3 60.55(11) . . ? B6 C1 B3 113.02(13) . . ? C3 C1 B4 121.10(13) . . ? C2 C1 B4 112.05(13) . . ? B6 C1 B4 114.54(13) . . ? B3 C1 B4 63.46(11) . . ? C3 C1 B5 121.22(12) . . ? C2 C1 B5 112.04(12) . . ? B6 C1 B5 63.27(11) . . ? B3 C1 B5 114.16(13) . . ? B4 C1 B5 62.12(11) . . ? C1 C2 B3 59.89(10) . . ? C1 C2 B7 107.72(13) . . ? B3 C2 B7 61.71(12) . . ? C1 C2 B11 107.69(13) . . ? B3 C2 B11 111.75(14) . . ? B7 C2 B11 61.43(13) . . ? C1 C2 B6 59.53(10) . . ? B3 C2 B6 111.01(13) . . ? B7 C2 B6 111.35(14) . . ? B11 C2 B6 61.62(11) . . ? C1 C2 Li1 101.14(12) . . ? B3 C2 Li1 105.92(14) . . ? B7 C2 Li1 133.10(14) . . ? B11 C2 Li1 140.45(15) . . ? B6 C2 Li1 115.06(14) . . ? N1 C3 N2 136.18(15) . . ? N1 C3 C1 112.80(13) . . ? N2 C3 C1 111.02(13) . . ? N1 C4 C6 108.72(14) . . ? N1 C4 C5 109.77(15) . . ? C6 C4 C5 110.73(17) . . ? N1 C4 H4A 112.9(11) . . ? C6 C4 H4A 107.9(12) . . ? C5 C4 H4A 106.7(12) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 110.73(14) . . ? N2 C7 C9 108.62(14) . . ? C8 C7 C9 109.24(14) . . ? N2 C7 H7A 112.6(10) . . ? C8 C7 H7A 109.8(11) . . ? C9 C7 H7A 105.6(10) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O1 C10 C11 107.14(16) . . ? O1 C10 H10A 110.3 . . ? C11 C10 H10A 110.3 . . ? O1 C10 H10B 110.3 . . ? C11 C10 H10B 110.3 . . ? H10A C10 H10B 108.5 . . ? O2 C11 C10 107.26(15) . . ? O2 C11 H11A 110.3 . . ? C10 C11 H11A 110.3 . . ? O2 C11 H11B 110.3 . . ? C10 C11 H11B 110.3 . . ? H11A C11 H11B 108.5 . . ? O1 C12 H12A 109.5 . . ? O1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O2 C13 H13A 109.5 . . ? O2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O3 C14 C15 107.0(2) . . ? O3 C14 Li2 43.18(11) . . ? C15 C14 Li2 76.47(14) . . ? O3 C14 H14A 110.3 . . ? C15 C14 H14A 110.3 . . ? Li2 C14 H14A 93.9 . . ? O3 C14 H14B 110.3 . . ? C15 C14 H14B 110.3 . . ? Li2 C14 H14B 151.4 . . ? H14A C14 H14B 108.6 . . ? O4 C15 C14 107.41(18) . . ? O4 C15 H15A 110.2 . . ? C14 C15 H15A 110.2 . . ? O4 C15 H15B 110.2 . . ? C14 C15 H15B 110.2 . . ? H15A C15 H15B 108.5 . . ? O3 C16 H16A 109.5 . . ? O3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O4 C17 H17A 109.5 . . ? O4 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O4 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C12 O1 C10 113.81(15) . . ? C12 O1 Li1 123.53(15) . . ? C10 O1 Li1 107.66(14) . . ? C11 O2 C13 112.39(15) . . ? C11 O2 Li1 110.30(14) . . ? C13 O2 Li1 119.43(15) . . ? C14 O3 C16 114.78(18) . . ? C14 O3 Li2 107.57(15) . . ? C16 O3 Li2 122.75(15) . . ? C17 O4 C15 112.72(16) . . ? C17 O4 Li2 131.60(16) . . ? C15 O4 Li2 110.61(15) . . ? C1 B3 C2 59.56(10) . . ? C1 B3 B7 105.71(14) . . ? C2 B3 B7 59.44(12) . . ? C1 B3 B4 58.67(10) . . ? C2 B3 B4 107.41(13) . . ? B7 B3 B4 107.22(14) . . ? C1 B3 B8 105.22(13) . . ? C2 B3 B8 107.33(14) . . ? B7 B3 B8 59.99(12) . . ? B4 B3 B8 59.37(11) . . ? C1 B3 H3 121.0(12) . . ? C2 B3 H3 121.2(13) . . ? B7 B3 H3 124.8(11) . . ? B4 B3 H3 121.0(12) . . ? B8 B3 H3 124.6(13) . . ? C1 B4 B5 59.18(10) . . ? C1 B4 B9 105.66(14) . . ? B5 B4 B9 59.96(11) . . ? C1 B4 B8 105.36(14) . . ? B5 B4 B8 108.40(14) . . ? B9 B4 B8 60.59(12) . . ? C1 B4 B3 57.87(10) . . ? B5 B4 B3 107.22(14) . . ? B9 B4 B3 108.25(14) . . ? B8 B4 B3 60.34(11) . . ? C1 B4 Li2 84.27(11) . . ? B5 B4 Li2 71.96(11) . . ? B9 B4 Li2 112.51(13) . . ? B8 B4 Li2 169.16(14) . . ? B3 B4 Li2 130.32(13) . . ? C1 B4 H4 119.2(10) . . ? B5 B4 H4 123.0(10) . . ? B9 B4 H4 127.9(10) . . ? B8 B4 H4 123.6(10) . . ? B3 B4 H4 117.1(10) . . ? Li2 B4 H4 52.5(10) . . ? C1 B5 B4 58.70(10) . . ? C1 B5 B10 105.05(13) . . ? B4 B5 B10 108.60(14) . . ? C1 B5 B9 105.40(13) . . ? B4 B5 B9 60.12(11) . . ? B10 B5 B9 60.99(12) . . ? C1 B5 B6 57.72(10) . . ? B4 B5 B6 107.15(13) . . ? B10 B5 B6 60.59(11) . . ? B9 B5 B6 108.97(14) . . ? C1 B5 Li2 83.26(11) . . ? B4 B5 Li2 70.29(11) . . ? B10 B5 Li2 169.75(14) . . ? B9 B5 Li2 111.42(13) . . ? B6 B5 Li2 129.66(13) . . ? C1 B5 H5 118.5(11) . . ? B4 B5 H5 120.3(11) . . ? B10 B5 H5 126.1(11) . . ? B9 B5 H5 127.0(12) . . ? B6 B5 H5 118.7(11) . . ? Li2 B5 H5 51.5(11) . . ? C1 B6 C2 59.23(10) . . ? C1 B6 B11 105.43(14) . . ? C2 B6 B11 59.02(11) . . ? C1 B6 B5 59.01(10) . . ? C2 B6 B5 107.05(14) . . ? B11 B6 B5 107.03(14) . . ? C1 B6 B10 104.90(14) . . ? C2 B6 B10 106.25(14) . . ? B11 B6 B10 59.70(12) . . ? B5 B6 B10 59.12(11) . . ? C1 B6 H6 118.2(10) . . ? C2 B6 H6 120.1(10) . . ? B11 B6 H6 126.6(10) . . ? B5 B6 H6 120.8(10) . . ? B10 B6 H6 127.8(10) . . ? C2 B7 B11 59.31(12) . . ? C2 B7 B3 58.85(11) . . ? B11 B7 B3 107.72(14) . . ? C2 B7 B8 107.67(13) . . ? B11 B7 B8 109.37(15) . . ? B3 B7 B8 61.01(12) . . ? C2 B7 B12 107.82(15) . . ? B11 B7 B12 60.96(13) . . ? B3 B7 B12 109.27(15) . . ? B8 B7 B12 60.69(12) . . ? C2 B7 H7 117.4(12) . . ? B11 B7 H7 120.9(12) . . ? B3 B7 H7 118.3(12) . . ? B8 B7 H7 124.3(12) . . ? B12 B7 H7 126.1(12) . . ? B7 B8 B4 107.16(15) . . ? B7 B8 B9 107.09(16) . . ? B4 B8 B9 59.65(11) . . ? B7 B8 B3 59.00(12) . . ? B4 B8 B3 60.29(11) . . ? B9 B8 B3 107.47(14) . . ? B7 B8 B12 59.66(13) . . ? B4 B8 B12 107.26(15) . . ? B9 B8 B12 59.65(12) . . ? B3 B8 B12 106.87(16) . . ? B7 B8 H8 123.5(10) . . ? B4 B8 H8 121.2(10) . . ? B9 B8 H8 121.2(11) . . ? B3 B8 H8 122.7(11) . . ? B12 B8 H8 122.4(11) . . ? B5 B9 B4 59.93(11) . . ? B5 B9 B12 107.55(15) . . ? B4 B9 B12 107.83(14) . . ? B5 B9 B8 107.72(14) . . ? B4 B9 B8 59.76(11) . . ? B12 B9 B8 60.27(13) . . ? B5 B9 B10 59.49(12) . . ? B4 B9 B10 107.27(14) . . ? B12 B9 B10 59.71(13) . . ? B8 B9 B10 107.63(15) . . ? B5 B9 H9 119.7(10) . . ? B4 B9 H9 120.8(10) . . ? B12 B9 H9 123.9(10) . . ? B8 B9 H9 123.4(11) . . ? B10 B9 H9 121.9(11) . . ? B5 B10 B11 107.60(14) . . ? B5 B10 B12 107.59(15) . . ? B11 B10 B12 60.51(13) . . ? B5 B10 B6 60.30(11) . . ? B11 B10 B6 59.23(11) . . ? B12 B10 B6 107.75(15) . . ? B5 B10 B9 59.51(11) . . ? B11 B10 B9 107.80(15) . . ? B12 B10 B9 59.74(12) . . ? B6 B10 B9 107.57(14) . . ? B5 B10 H10 120.7(11) . . ? B11 B10 H10 120.5(12) . . ? B12 B10 H10 124.9(11) . . ? B6 B10 H10 118.0(12) . . ? B9 B10 H10 125.3(12) . . ? C2 B11 B7 59.26(12) . . ? C2 B11 B6 59.36(11) . . ? B7 B11 B6 107.78(14) . . ? C2 B11 B10 107.59(13) . . ? B7 B11 B10 108.10(15) . . ? B6 B11 B10 61.07(12) . . ? C2 B11 B12 107.07(15) . . ? B7 B11 B12 60.07(13) . . ? B6 B11 B12 108.80(15) . . ? B10 B11 B12 60.01(13) . . ? C2 B11 H11 118.8(11) . . ? B7 B11 H11 122.6(11) . . ? B6 B11 H11 118.0(11) . . ? B10 B11 H11 123.3(11) . . ? B12 B11 H11 126.1(11) . . ? B7 B12 B10 106.81(15) . . ? B7 B12 B9 107.41(15) . . ? B10 B12 B9 60.54(12) . . ? B7 B12 B11 58.98(13) . . ? B10 B12 B11 59.48(12) . . ? B9 B12 B11 107.62(15) . . ? B7 B12 B8 59.65(13) . . ? B10 B12 B8 108.13(15) . . ? B9 B12 B8 60.08(12) . . ? B11 B12 B8 106.97(15) . . ? B7 B12 H12 119.2(12) . . ? B10 B12 H12 124.3(12) . . ? B9 B12 H12 124.5(12) . . ? B11 B12 H12 121.1(12) . . ? B8 B12 H12 121.1(12) . . ? O2 Li1 N1 123.84(16) . . ? O2 Li1 O1 83.11(12) . . ? N1 Li1 O1 129.15(17) . . ? O2 Li1 C2 121.27(16) . . ? N1 Li1 C2 89.27(12) . . ? O1 Li1 C2 113.95(15) . . ? N2 Li2 O4 160.3(2) . . ? N2 Li2 O3 112.54(17) . . ? O4 Li2 O3 83.02(13) . . ? N2 Li2 B4 82.25(11) . . ? O4 Li2 B4 104.74(14) . . ? O3 Li2 B4 108.75(14) . . ? N2 Li2 B5 76.86(11) . . ? O4 Li2 B5 97.25(13) . . ? O3 Li2 B5 145.64(16) . . ? B4 Li2 B5 37.75(7) . . ? N2 Li2 C14 141.11(17) . . ? O4 Li2 C14 56.43(10) . . ? O3 Li2 C14 29.26(8) . . ? B4 Li2 C14 101.71(13) . . ? B5 Li2 C14 128.67(14) . . ? N2 Li2 H4 92.4(5) . . ? O4 Li2 H4 101.1(5) . . ? O3 Li2 H4 85.5(6) . . ? B4 Li2 H4 23.3(5) . . ? B5 Li2 H4 60.6(5) . . ? C14 Li2 H4 80.7(5) . . ? N2 Li2 H5 81.3(5) . . ? O4 Li2 H5 86.7(5) . . ? O3 Li2 H5 161.0(5) . . ? B4 Li2 H5 58.7(5) . . ? B5 Li2 H5 21.4(5) . . ? C14 Li2 H5 134.0(5) . . ? H4 Li2 H5 80.8(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 C1 C2 B3 -107.55(15) . . . . ? B6 C1 C2 B3 145.30(14) . . . . ? B4 C1 C2 B3 38.52(13) . . . . ? B5 C1 C2 B3 106.17(15) . . . . ? C3 C1 C2 B7 -148.05(14) . . . . ? B6 C1 C2 B7 104.80(15) . . . . ? B3 C1 C2 B7 -40.50(14) . . . . ? B4 C1 C2 B7 -1.99(18) . . . . ? B5 C1 C2 B7 65.66(17) . . . . ? C3 C1 C2 B11 147.10(14) . . . . ? B6 C1 C2 B11 39.95(14) . . . . ? B3 C1 C2 B11 -105.35(15) . . . . ? B4 C1 C2 B11 -66.83(17) . . . . ? B5 C1 C2 B11 0.81(18) . . . . ? C3 C1 C2 B6 107.15(15) . . . . ? B3 C1 C2 B6 -145.30(14) . . . . ? B4 C1 C2 B6 -106.79(15) . . . . ? B5 C1 C2 B6 -39.14(13) . . . . ? C3 C1 C2 Li1 -5.49(17) . . . . ? B6 C1 C2 Li1 -112.64(15) . . . . ? B3 C1 C2 Li1 102.06(14) . . . . ? B4 C1 C2 Li1 140.57(14) . . . . ? B5 C1 C2 Li1 -151.78(14) . . . . ? C4 N1 C3 N2 -18.3(3) . . . . ? Li1 N1 C3 N2 167.49(18) . . . . ? C4 N1 C3 C1 162.18(14) . . . . ? Li1 N1 C3 C1 -12.0(2) . . . . ? C7 N2 C3 N1 -19.5(3) . . . . ? Li2 N2 C3 N1 157.2(2) . . . . ? C7 N2 C3 C1 160.00(14) . . . . ? Li2 N2 C3 C1 -23.3(2) . . . . ? C2 C1 C3 N1 11.49(19) . . . . ? B6 C1 C3 N1 81.03(17) . . . . ? B3 C1 C3 N1 -57.42(18) . . . . ? B4 C1 C3 N1 -131.34(15) . . . . ? B5 C1 C3 N1 154.50(14) . . . . ? C2 C1 C3 N2 -168.13(13) . . . . ? B6 C1 C3 N2 -98.58(16) . . . . ? B3 C1 C3 N2 122.96(15) . . . . ? B4 C1 C3 N2 49.04(18) . . . . ? B5 C1 C3 N2 -25.1(2) . . . . ? C3 N1 C4 C6 170.40(16) . . . . ? Li1 N1 C4 C6 -15.5(2) . . . . ? C3 N1 C4 C5 -68.3(2) . . . . ? Li1 N1 C4 C5 105.72(18) . . . . ? C3 N2 C7 C8 -58.5(2) . . . . ? Li2 N2 C7 C8 124.42(17) . . . . ? C3 N2 C7 C9 -178.48(15) . . . . ? Li2 N2 C7 C9 4.5(2) . . . . ? O1 C10 C11 O2 -54.5(2) . . . . ? O3 C14 C15 O4 -53.2(3) . . . . ? Li2 C14 C15 O4 -22.31(17) . . . . ? C11 C10 O1 C12 -176.13(16) . . . . ? C11 C10 O1 Li1 43.14(18) . . . . ? C10 C11 O2 C13 174.67(17) . . . . ? C10 C11 O2 Li1 38.7(2) . . . . ? C15 C14 O3 C16 -172.68(18) . . . . ? Li2 C14 O3 C16 140.5(2) . . . . ? C15 C14 O3 Li2 46.9(2) . . . . ? C14 C15 O4 C17 -168.6(2) . . . . ? C14 C15 O4 Li2 33.5(3) . . . . ? C3 C1 B3 C2 107.06(15) . . . . ? B6 C1 B3 C2 -32.84(13) . . . . ? B4 C1 B3 C2 -139.82(14) . . . . ? B5 C1 B3 C2 -102.65(14) . . . . ? C3 C1 B3 B7 145.99(14) . . . . ? C2 C1 B3 B7 38.94(13) . . . . ? B6 C1 B3 B7 6.10(18) . . . . ? B4 C1 B3 B7 -100.89(15) . . . . ? B5 C1 B3 B7 -63.72(17) . . . . ? C3 C1 B3 B4 -113.12(15) . . . . ? C2 C1 B3 B4 139.82(14) . . . . ? B6 C1 B3 B4 106.99(15) . . . . ? B5 C1 B3 B4 37.17(14) . . . . ? C3 C1 B3 B8 -151.51(14) . . . . ? C2 C1 B3 B8 101.43(15) . . . . ? B6 C1 B3 B8 68.59(17) . . . . ? B4 C1 B3 B8 -38.39(13) . . . . ? B5 C1 B3 B8 -1.22(18) . . . . ? B7 C2 B3 C1 135.37(14) . . . . ? B11 C2 B3 C1 98.44(14) . . . . ? B6 C2 B3 C1 31.71(13) . . . . ? Li1 C2 B3 C1 -93.84(13) . . . . ? C1 C2 B3 B7 -135.37(14) . . . . ? B11 C2 B3 B7 -36.92(14) . . . . ? B6 C2 B3 B7 -103.66(15) . . . . ? Li1 C2 B3 B7 130.79(14) . . . . ? C1 C2 B3 B4 -35.28(12) . . . . ? B7 C2 B3 B4 100.09(15) . . . . ? B11 C2 B3 B4 63.17(17) . . . . ? B6 C2 B3 B4 -3.57(18) . . . . ? Li1 C2 B3 B4 -129.12(14) . . . . ? C1 C2 B3 B8 -97.80(14) . . . . ? B7 C2 B3 B8 37.57(13) . . . . ? B11 C2 B3 B8 0.65(18) . . . . ? B6 C2 B3 B8 -66.09(16) . . . . ? Li1 C2 B3 B8 168.36(13) . . . . ? C3 C1 B4 B5 -111.46(15) . . . . ? C2 C1 B4 B5 104.11(14) . . . . ? B6 C1 B4 B5 36.79(13) . . . . ? B3 C1 B4 B5 141.42(14) . . . . ? C3 C1 B4 B9 -150.87(14) . . . . ? C2 C1 B4 B9 64.70(16) . . . . ? B6 C1 B4 B9 -2.62(17) . . . . ? B3 C1 B4 B9 102.01(14) . . . . ? B5 C1 B4 B9 -39.41(12) . . . . ? C3 C1 B4 B8 145.99(14) . . . . ? C2 C1 B4 B8 1.56(17) . . . . ? B6 C1 B4 B8 -65.76(16) . . . . ? B3 C1 B4 B8 38.87(13) . . . . ? B5 C1 B4 B8 -102.55(14) . . . . ? C3 C1 B4 B3 107.12(16) . . . . ? C2 C1 B4 B3 -37.31(13) . . . . ? B6 C1 B4 B3 -104.63(15) . . . . ? B5 C1 B4 B3 -141.42(14) . . . . ? C3 C1 B4 Li2 -39.06(14) . . . . ? C2 C1 B4 Li2 176.50(13) . . . . ? B6 C1 B4 Li2 109.18(13) . . . . ? B3 C1 B4 Li2 -146.19(13) . . . . ? B5 C1 B4 Li2 72.39(11) . . . . ? C2 B3 B4 C1 35.66(12) . . . . ? B7 B3 B4 C1 98.23(15) . . . . ? B8 B3 B4 C1 135.86(15) . . . . ? C1 B3 B4 B5 -34.11(12) . . . . ? C2 B3 B4 B5 1.55(18) . . . . ? B7 B3 B4 B5 64.12(17) . . . . ? B8 B3 B4 B5 101.76(15) . . . . ? C1 B3 B4 B9 -97.38(14) . . . . ? C2 B3 B4 B9 -61.72(17) . . . . ? B7 B3 B4 B9 0.85(19) . . . . ? B8 B3 B4 B9 38.48(14) . . . . ? C1 B3 B4 B8 -135.86(15) . . . . ? C2 B3 B4 B8 -100.20(15) . . . . ? B7 B3 B4 B8 -37.63(14) . . . . ? C1 B3 B4 Li2 46.56(17) . . . . ? C2 B3 B4 Li2 82.22(19) . . . . ? B7 B3 B4 Li2 144.79(16) . . . . ? B8 B3 B4 Li2 -177.57(19) . . . . ? C3 C1 B5 B4 111.26(16) . . . . ? C2 C1 B5 B4 -104.13(14) . . . . ? B6 C1 B5 B4 -142.41(14) . . . . ? B3 C1 B5 B4 -37.70(14) . . . . ? C3 C1 B5 B10 -145.85(15) . . . . ? C2 C1 B5 B10 -1.24(18) . . . . ? B6 C1 B5 B10 -39.52(13) . . . . ? B3 C1 B5 B10 65.20(17) . . . . ? B4 C1 B5 B10 102.89(15) . . . . ? C3 C1 B5 B9 150.69(14) . . . . ? C2 C1 B5 B9 -64.70(16) . . . . ? B6 C1 B5 B9 -102.98(14) . . . . ? B3 C1 B5 B9 1.73(18) . . . . ? B4 C1 B5 B9 39.43(13) . . . . ? C3 C1 B5 B6 -106.33(16) . . . . ? C2 C1 B5 B6 38.28(13) . . . . ? B3 C1 B5 B6 104.71(15) . . . . ? B4 C1 B5 B6 142.41(14) . . . . ? C3 C1 B5 Li2 40.26(15) . . . . ? C2 C1 B5 Li2 -175.12(13) . . . . ? B6 C1 B5 Li2 146.59(13) . . . . ? B3 C1 B5 Li2 -108.69(14) . . . . ? B4 C1 B5 Li2 -71.00(11) . . . . ? B9 B4 B5 C1 135.08(14) . . . . ? B8 B4 B5 C1 97.28(14) . . . . ? B3 B4 B5 C1 33.57(12) . . . . ? Li2 B4 B5 C1 -94.12(11) . . . . ? C1 B4 B5 B10 -96.66(14) . . . . ? B9 B4 B5 B10 38.41(14) . . . . ? B8 B4 B5 B10 0.62(19) . . . . ? B3 B4 B5 B10 -63.09(17) . . . . ? Li2 B4 B5 B10 169.21(15) . . . . ? C1 B4 B5 B9 -135.08(14) . . . . ? B8 B4 B5 B9 -37.80(14) . . . . ? B3 B4 B5 B9 -101.51(15) . . . . ? Li2 B4 B5 B9 130.80(13) . . . . ? C1 B4 B5 B6 -32.66(12) . . . . ? B9 B4 B5 B6 102.41(15) . . . . ? B8 B4 B5 B6 64.62(17) . . . . ? B3 B4 B5 B6 0.91(18) . . . . ? Li2 B4 B5 B6 -126.79(14) . . . . ? C1 B4 B5 Li2 94.12(11) . . . . ? B9 B4 B5 Li2 -130.80(13) . . . . ? B8 B4 B5 Li2 -168.60(15) . . . . ? B3 B4 B5 Li2 127.69(14) . . . . ? C3 C1 B6 C2 -107.54(14) . . . . ? B3 C1 B6 C2 32.59(13) . . . . ? B4 C1 B6 C2 102.73(14) . . . . ? B5 C1 B6 C2 139.08(13) . . . . ? C3 C1 B6 B11 -145.74(14) . . . . ? C2 C1 B6 B11 -38.20(13) . . . . ? B3 C1 B6 B11 -5.62(18) . . . . ? B4 C1 B6 B11 64.52(16) . . . . ? B5 C1 B6 B11 100.87(14) . . . . ? C3 C1 B6 B5 113.38(14) . . . . ? C2 C1 B6 B5 -139.08(13) . . . . ? B3 C1 B6 B5 -106.49(15) . . . . ? B4 C1 B6 B5 -36.35(13) . . . . ? C3 C1 B6 B10 152.17(14) . . . . ? C2 C1 B6 B10 -100.29(14) . . . . ? B3 C1 B6 B10 -67.70(16) . . . . ? B4 C1 B6 B10 2.44(18) . . . . ? B5 C1 B6 B10 38.79(13) . . . . ? B3 C2 B6 C1 -31.84(13) . . . . ? B7 C2 B6 C1 -98.58(15) . . . . ? B11 C2 B6 C1 -135.95(15) . . . . ? Li1 C2 B6 C1 88.42(14) . . . . ? C1 C2 B6 B11 135.95(15) . . . . ? B3 C2 B6 B11 104.11(16) . . . . ? B7 C2 B6 B11 37.37(14) . . . . ? Li1 C2 B6 B11 -135.63(16) . . . . ? C1 C2 B6 B5 35.97(12) . . . . ? B3 C2 B6 B5 4.13(18) . . . . ? B7 C2 B6 B5 -62.61(17) . . . . ? B11 C2 B6 B5 -99.98(15) . . . . ? Li1 C2 B6 B5 124.39(15) . . . . ? C1 C2 B6 B10 97.94(14) . . . . ? B3 C2 B6 B10 66.11(16) . . . . ? B7 C2 B6 B10 -0.63(18) . . . . ? B11 C2 B6 B10 -38.00(13) . . . . ? Li1 C2 B6 B10 -173.63(13) . . . . ? B4 B5 B6 C1 33.06(13) . . . . ? B10 B5 B6 C1 135.14(14) . . . . ? B9 B5 B6 C1 96.61(14) . . . . ? Li2 B5 B6 C1 -45.25(16) . . . . ? C1 B5 B6 C2 -36.06(12) . . . . ? B4 B5 B6 C2 -3.01(18) . . . . ? B10 B5 B6 C2 99.07(15) . . . . ? B9 B5 B6 C2 60.55(17) . . . . ? Li2 B5 B6 C2 -81.31(19) . . . . ? C1 B5 B6 B11 -98.09(15) . . . . ? B4 B5 B6 B11 -65.03(17) . . . . ? B10 B5 B6 B11 37.05(14) . . . . ? B9 B5 B6 B11 -1.48(18) . . . . ? Li2 B5 B6 B11 -143.34(16) . . . . ? C1 B5 B6 B10 -135.14(14) . . . . ? B4 B5 B6 B10 -102.08(15) . . . . ? B9 B5 B6 B10 -38.53(14) . . . . ? Li2 B5 B6 B10 179.61(18) . . . . ? C1 C2 B7 B11 -100.91(14) . . . . ? B3 C2 B7 B11 -140.56(15) . . . . ? B6 C2 B7 B11 -37.45(14) . . . . ? Li1 C2 B7 B11 133.9(2) . . . . ? C1 C2 B7 B3 39.65(13) . . . . ? B11 C2 B7 B3 140.56(15) . . . . ? B6 C2 B7 B3 103.11(15) . . . . ? Li1 C2 B7 B3 -85.6(2) . . . . ? C1 C2 B7 B8 1.55(19) . . . . ? B3 C2 B7 B8 -38.09(14) . . . . ? B11 C2 B7 B8 102.46(16) . . . . ? B6 C2 B7 B8 65.02(18) . . . . ? Li1 C2 B7 B8 -123.68(19) . . . . ? C1 C2 B7 B12 -62.52(18) . . . . ? B3 C2 B7 B12 -102.17(16) . . . . ? B11 C2 B7 B12 38.39(15) . . . . ? B6 C2 B7 B12 0.9(2) . . . . ? Li1 C2 B7 B12 172.25(17) . . . . ? C1 B3 B7 C2 -38.99(12) . . . . ? B4 B3 B7 C2 -100.42(14) . . . . ? B8 B3 B7 C2 -137.77(14) . . . . ? C1 B3 B7 B11 -4.00(19) . . . . ? C2 B3 B7 B11 35.00(13) . . . . ? B4 B3 B7 B11 -65.42(18) . . . . ? B8 B3 B7 B11 -102.77(16) . . . . ? C1 B3 B7 B8 98.78(14) . . . . ? C2 B3 B7 B8 137.77(14) . . . . ? B4 B3 B7 B8 37.36(14) . . . . ? C1 B3 B7 B12 60.65(19) . . . . ? C2 B3 B7 B12 99.65(17) . . . . ? B4 B3 B7 B12 -0.8(2) . . . . ? B8 B3 B7 B12 -38.13(15) . . . . ? C2 B7 B8 B4 -0.62(19) . . . . ? B11 B7 B8 B4 62.27(18) . . . . ? B3 B7 B8 B4 -37.75(14) . . . . ? B12 B7 B8 B4 100.31(16) . . . . ? C2 B7 B8 B9 -63.33(18) . . . . ? B11 B7 B8 B9 -0.45(19) . . . . ? B3 B7 B8 B9 -100.47(15) . . . . ? B12 B7 B8 B9 37.59(14) . . . . ? C2 B7 B8 B3 37.13(13) . . . . ? B11 B7 B8 B3 100.02(15) . . . . ? B12 B7 B8 B3 138.06(15) . . . . ? C2 B7 B8 B12 -100.93(17) . . . . ? B11 B7 B8 B12 -38.04(14) . . . . ? B3 B7 B8 B12 -138.06(15) . . . . ? C1 B4 B8 B7 -0.54(18) . . . . ? B5 B4 B8 B7 -62.60(17) . . . . ? B9 B4 B8 B7 -100.11(16) . . . . ? B3 B4 B8 B7 37.17(14) . . . . ? Li2 B4 B8 B7 -152.7(7) . . . . ? C1 B4 B8 B9 99.58(14) . . . . ? B5 B4 B8 B9 37.52(14) . . . . ? B3 B4 B8 B9 137.28(15) . . . . ? Li2 B4 B8 B9 -52.6(8) . . . . ? C1 B4 B8 B3 -37.71(12) . . . . ? B5 B4 B8 B3 -99.77(15) . . . . ? B9 B4 B8 B3 -137.28(15) . . . . ? Li2 B4 B8 B3 170.1(8) . . . . ? C1 B4 B8 B12 62.23(17) . . . . ? B5 B4 B8 B12 0.17(19) . . . . ? B9 B4 B8 B12 -37.35(14) . . . . ? B3 B4 B8 B12 99.94(16) . . . . ? Li2 B4 B8 B12 -89.9(8) . . . . ? C1 B3 B8 B7 -99.60(15) . . . . ? C2 B3 B8 B7 -37.32(13) . . . . ? B4 B3 B8 B7 -137.66(15) . . . . ? C1 B3 B8 B4 38.06(12) . . . . ? C2 B3 B8 B4 100.34(14) . . . . ? B7 B3 B8 B4 137.66(15) . . . . ? C1 B3 B8 B9 0.20(18) . . . . ? C2 B3 B8 B9 62.49(17) . . . . ? B7 B3 B8 B9 99.81(17) . . . . ? B4 B3 B8 B9 -37.86(14) . . . . ? C1 B3 B8 B12 -62.54(17) . . . . ? C2 B3 B8 B12 -0.25(17) . . . . ? B7 B3 B8 B12 37.07(14) . . . . ? B4 B3 B8 B12 -100.59(15) . . . . ? C1 B5 B9 B4 -38.74(12) . . . . ? B10 B5 B9 B4 -137.68(15) . . . . ? B6 B5 B9 B4 -99.33(15) . . . . ? Li2 B5 B9 B4 49.95(13) . . . . ? C1 B5 B9 B12 62.09(17) . . . . ? B4 B5 B9 B12 100.84(16) . . . . ? B10 B5 B9 B12 -36.84(14) . . . . ? B6 B5 B9 B12 1.51(19) . . . . ? Li2 B5 B9 B12 150.79(14) . . . . ? C1 B5 B9 B8 -1.48(18) . . . . ? B4 B5 B9 B8 37.26(14) . . . . ? B10 B5 B9 B8 -100.42(16) . . . . ? B6 B5 B9 B8 -62.07(17) . . . . ? Li2 B5 B9 B8 87.21(16) . . . . ? C1 B5 B9 B10 98.93(14) . . . . ? B4 B5 B9 B10 137.68(15) . . . . ? B6 B5 B9 B10 38.34(13) . . . . ? Li2 B5 B9 B10 -172.37(15) . . . . ? C1 B4 B9 B5 39.04(12) . . . . ? B8 B4 B9 B5 138.12(15) . . . . ? B3 B4 B9 B5 99.76(15) . . . . ? Li2 B4 B9 B5 -51.18(13) . . . . ? C1 B4 B9 B12 -61.32(17) . . . . ? B5 B4 B9 B12 -100.36(16) . . . . ? B8 B4 B9 B12 37.76(15) . . . . ? B3 B4 B9 B12 -0.60(19) . . . . ? Li2 B4 B9 B12 -151.54(14) . . . . ? C1 B4 B9 B8 -99.09(15) . . . . ? B5 B4 B9 B8 -138.12(15) . . . . ? B3 B4 B9 B8 -38.37(14) . . . . ? Li2 B4 B9 B8 170.70(16) . . . . ? C1 B4 B9 B10 1.63(17) . . . . ? B5 B4 B9 B10 -37.41(13) . . . . ? B8 B4 B9 B10 100.71(16) . . . . ? B3 B4 B9 B10 62.35(17) . . . . ? Li2 B4 B9 B10 -88.59(16) . . . . ? B7 B8 B9 B5 62.90(17) . . . . ? B4 B8 B9 B5 -37.33(13) . . . . ? B3 B8 B9 B5 0.81(19) . . . . ? B12 B8 B9 B5 100.50(16) . . . . ? B7 B8 B9 B4 100.23(15) . . . . ? B3 B8 B9 B4 38.15(13) . . . . ? B12 B8 B9 B4 137.83(16) . . . . ? B7 B8 B9 B12 -37.60(14) . . . . ? B4 B8 B9 B12 -137.83(16) . . . . ? B3 B8 B9 B12 -99.68(16) . . . . ? B7 B8 B9 B10 0.13(19) . . . . ? B4 B8 B9 B10 -100.10(15) . . . . ? B3 B8 B9 B10 -61.95(18) . . . . ? B12 B8 B9 B10 37.73(14) . . . . ? C1 B5 B10 B11 1.16(19) . . . . ? B4 B5 B10 B11 62.66(19) . . . . ? B9 B5 B10 B11 100.68(16) . . . . ? B6 B5 B10 B11 -36.98(14) . . . . ? Li2 B5 B10 B11 144.7(7) . . . . ? C1 B5 B10 B12 -62.66(17) . . . . ? B4 B5 B10 B12 -1.16(19) . . . . ? B9 B5 B10 B12 36.86(14) . . . . ? B6 B5 B10 B12 -100.80(16) . . . . ? Li2 B5 B10 B12 80.9(8) . . . . ? C1 B5 B10 B6 38.14(13) . . . . ? B4 B5 B10 B6 99.64(15) . . . . ? B9 B5 B10 B6 137.66(15) . . . . ? Li2 B5 B10 B6 -178.3(8) . . . . ? C1 B5 B10 B9 -99.52(14) . . . . ? B4 B5 B10 B9 -38.02(13) . . . . ? B6 B5 B10 B9 -137.66(15) . . . . ? Li2 B5 B10 B9 44.0(8) . . . . ? C1 B6 B10 B5 -38.74(12) . . . . ? C2 B6 B10 B5 -100.45(15) . . . . ? B11 B6 B10 B5 -138.15(15) . . . . ? C1 B6 B10 B11 99.41(15) . . . . ? C2 B6 B10 B11 37.69(13) . . . . ? B5 B6 B10 B11 138.15(15) . . . . ? C1 B6 B10 B12 61.79(17) . . . . ? C2 B6 B10 B12 0.07(18) . . . . ? B11 B6 B10 B12 -37.62(15) . . . . ? B5 B6 B10 B12 100.53(16) . . . . ? C1 B6 B10 B9 -1.24(18) . . . . ? C2 B6 B10 B9 -62.95(17) . . . . ? B11 B6 B10 B9 -100.64(16) . . . . ? B5 B6 B10 B9 37.50(13) . . . . ? B4 B9 B10 B5 37.61(13) . . . . ? B12 B9 B10 B5 138.55(15) . . . . ? B8 B9 B10 B5 100.57(15) . . . . ? B5 B9 B10 B11 -100.35(15) . . . . ? B4 B9 B10 B11 -62.74(18) . . . . ? B12 B9 B10 B11 38.20(14) . . . . ? B8 B9 B10 B11 0.22(19) . . . . ? B5 B9 B10 B12 -138.55(15) . . . . ? B4 B9 B10 B12 -100.94(15) . . . . ? B8 B9 B10 B12 -37.98(14) . . . . ? B5 B9 B10 B6 -37.85(13) . . . . ? B4 B9 B10 B6 -0.25(19) . . . . ? B12 B9 B10 B6 100.69(16) . . . . ? B8 B9 B10 B6 62.71(18) . . . . ? C1 C2 B11 B7 100.96(15) . . . . ? B3 C2 B11 B7 37.04(14) . . . . ? B6 C2 B11 B7 139.93(15) . . . . ? Li1 C2 B11 B7 -124.2(2) . . . . ? C1 C2 B11 B6 -38.98(13) . . . . ? B3 C2 B11 B6 -102.90(14) . . . . ? B7 C2 B11 B6 -139.93(15) . . . . ? Li1 C2 B11 B6 95.8(2) . . . . ? C1 C2 B11 B10 -0.03(19) . . . . ? B3 C2 B11 B10 -63.95(18) . . . . ? B7 C2 B11 B10 -100.99(17) . . . . ? B6 C2 B11 B10 38.95(14) . . . . ? Li1 C2 B11 B10 134.8(2) . . . . ? C1 C2 B11 B12 63.14(17) . . . . ? B3 C2 B11 B12 -0.78(19) . . . . ? B7 C2 B11 B12 -37.81(14) . . . . ? B6 C2 B11 B12 102.12(16) . . . . ? Li1 C2 B11 B12 -162.03(19) . . . . ? B3 B7 B11 C2 -34.80(13) . . . . ? B8 B7 B11 C2 -99.52(15) . . . . ? B12 B7 B11 C2 -137.45(15) . . . . ? C2 B7 B11 B6 35.56(13) . . . . ? B3 B7 B11 B6 0.8(2) . . . . ? B8 B7 B11 B6 -63.96(18) . . . . ? B12 B7 B11 B6 -101.89(16) . . . . ? C2 B7 B11 B10 100.11(15) . . . . ? B3 B7 B11 B10 65.31(18) . . . . ? B8 B7 B11 B10 0.59(19) . . . . ? B12 B7 B11 B10 -37.33(14) . . . . ? C2 B7 B11 B12 137.45(15) . . . . ? B3 B7 B11 B12 102.64(16) . . . . ? B8 B7 B11 B12 37.92(14) . . . . ? C1 B6 B11 C2 38.30(12) . . . . ? B5 B6 B11 C2 100.00(15) . . . . ? B10 B6 B11 C2 136.79(15) . . . . ? C1 B6 B11 B7 2.78(18) . . . . ? C2 B6 B11 B7 -35.52(14) . . . . ? B5 B6 B11 B7 64.49(18) . . . . ? B10 B6 B11 B7 101.28(16) . . . . ? C1 B6 B11 B10 -98.49(14) . . . . ? C2 B6 B11 B10 -136.79(15) . . . . ? B5 B6 B11 B10 -36.79(13) . . . . ? C1 B6 B11 B12 -60.83(18) . . . . ? C2 B6 B11 B12 -99.13(17) . . . . ? B5 B6 B11 B12 0.87(19) . . . . ? B10 B6 B11 B12 37.66(15) . . . . ? B5 B10 B11 C2 -0.7(2) . . . . ? B12 B10 B11 C2 99.94(17) . . . . ? B6 B10 B11 C2 -38.16(14) . . . . ? B9 B10 B11 C2 62.08(19) . . . . ? B5 B10 B11 B7 -63.29(19) . . . . ? B12 B10 B11 B7 37.36(14) . . . . ? B6 B10 B11 B7 -100.74(15) . . . . ? B9 B10 B11 B7 -0.50(19) . . . . ? B5 B10 B11 B6 37.45(14) . . . . ? B12 B10 B11 B6 138.10(16) . . . . ? B9 B10 B11 B6 100.24(16) . . . . ? B5 B10 B11 B12 -100.65(16) . . . . ? B6 B10 B11 B12 -138.10(16) . . . . ? B9 B10 B11 B12 -37.86(14) . . . . ? C2 B7 B12 B10 -0.9(2) . . . . ? B11 B7 B12 B10 36.80(14) . . . . ? B3 B7 B12 B10 -63.3(2) . . . . ? B8 B7 B12 B10 -101.53(16) . . . . ? C2 B7 B12 B9 62.81(19) . . . . ? B11 B7 B12 B9 100.46(16) . . . . ? B3 B7 B12 B9 0.4(2) . . . . ? B8 B7 B12 B9 -37.86(14) . . . . ? C2 B7 B12 B11 -37.66(14) . . . . ? B3 B7 B12 B11 -100.06(16) . . . . ? B8 B7 B12 B11 -138.32(15) . . . . ? C2 B7 B12 B8 100.67(15) . . . . ? B11 B7 B12 B8 138.32(15) . . . . ? B3 B7 B12 B8 38.26(15) . . . . ? B5 B10 B12 B7 64.10(19) . . . . ? B11 B10 B12 B7 -36.57(14) . . . . ? B6 B10 B12 B7 0.5(2) . . . . ? B9 B10 B12 B7 100.86(17) . . . . ? B5 B10 B12 B9 -36.76(14) . . . . ? B11 B10 B12 B9 -137.43(15) . . . . ? B6 B10 B12 B9 -100.38(15) . . . . ? B5 B10 B12 B11 100.67(16) . . . . ? B6 B10 B12 B11 37.05(14) . . . . ? B9 B10 B12 B11 137.43(15) . . . . ? B5 B10 B12 B8 1.3(2) . . . . ? B11 B10 B12 B8 -99.41(16) . . . . ? B6 B10 B12 B8 -62.36(18) . . . . ? B9 B10 B12 B8 38.02(14) . . . . ? B5 B9 B12 B7 -63.11(19) . . . . ? B4 B9 B12 B7 0.1(2) . . . . ? B8 B9 B12 B7 37.67(15) . . . . ? B10 B9 B12 B7 -99.85(17) . . . . ? B5 B9 B12 B10 36.74(14) . . . . ? B4 B9 B12 B10 99.98(16) . . . . ? B8 B9 B12 B10 137.52(16) . . . . ? B5 B9 B12 B11 -1.0(2) . . . . ? B4 B9 B12 B11 62.29(19) . . . . ? B8 B9 B12 B11 99.82(17) . . . . ? B10 B9 B12 B11 -37.69(15) . . . . ? B5 B9 B12 B8 -100.77(15) . . . . ? B4 B9 B12 B8 -37.54(14) . . . . ? B10 B9 B12 B8 -137.52(16) . . . . ? C2 B11 B12 B7 37.45(13) . . . . ? B6 B11 B12 B7 100.14(16) . . . . ? B10 B11 B12 B7 138.27(15) . . . . ? C2 B11 B12 B10 -100.83(15) . . . . ? B7 B11 B12 B10 -138.27(15) . . . . ? B6 B11 B12 B10 -38.13(14) . . . . ? C2 B11 B12 B9 -62.66(19) . . . . ? B7 B11 B12 B9 -100.10(16) . . . . ? B6 B11 B12 B9 0.0(2) . . . . ? B10 B11 B12 B9 38.17(14) . . . . ? C2 B11 B12 B8 0.58(19) . . . . ? B7 B11 B12 B8 -36.86(14) . . . . ? B6 B11 B12 B8 63.28(19) . . . . ? B10 B11 B12 B8 101.41(16) . . . . ? B4 B8 B12 B7 -100.15(15) . . . . ? B9 B8 B12 B7 -137.49(15) . . . . ? B3 B8 B12 B7 -36.77(13) . . . . ? B7 B8 B12 B10 99.26(16) . . . . ? B4 B8 B12 B10 -0.9(2) . . . . ? B9 B8 B12 B10 -38.23(14) . . . . ? B3 B8 B12 B10 62.49(18) . . . . ? B7 B8 B12 B9 137.49(15) . . . . ? B4 B8 B12 B9 37.34(14) . . . . ? B3 B8 B12 B9 100.72(15) . . . . ? B7 B8 B12 B11 36.57(14) . . . . ? B4 B8 B12 B11 -63.58(18) . . . . ? B9 B8 B12 B11 -100.92(16) . . . . ? B3 B8 B12 B11 -0.21(19) . . . . ? C11 O2 Li1 N1 -145.45(18) . . . . ? C13 O2 Li1 N1 82.1(2) . . . . ? C11 O2 Li1 O1 -12.25(16) . . . . ? C13 O2 Li1 O1 -144.70(15) . . . . ? C11 O2 Li1 C2 101.64(19) . . . . ? C13 O2 Li1 C2 -30.8(2) . . . . ? C3 N1 Li1 O2 -120.61(18) . . . . ? C4 N1 Li1 O2 65.2(2) . . . . ? C3 N1 Li1 O1 128.33(19) . . . . ? C4 N1 Li1 O1 -45.8(3) . . . . ? C3 N1 Li1 C2 7.46(18) . . . . ? C4 N1 Li1 C2 -166.71(14) . . . . ? C12 O1 Li1 O2 -153.97(16) . . . . ? C10 O1 Li1 O2 -17.97(15) . . . . ? C12 O1 Li1 N1 -25.3(3) . . . . ? C10 O1 Li1 N1 110.7(2) . . . . ? C12 O1 Li1 C2 84.8(2) . . . . ? C10 O1 Li1 C2 -139.20(16) . . . . ? C1 C2 Li1 O2 129.69(16) . . . . ? B3 C2 Li1 O2 -168.70(15) . . . . ? B7 C2 Li1 O2 -102.8(2) . . . . ? B11 C2 Li1 O2 -6.8(3) . . . . ? B6 C2 Li1 O2 68.3(2) . . . . ? C1 C2 Li1 N1 -0.39(14) . . . . ? B3 C2 Li1 N1 61.22(14) . . . . ? B7 C2 Li1 N1 127.14(18) . . . . ? B11 C2 Li1 N1 -136.9(2) . . . . ? B6 C2 Li1 N1 -61.80(16) . . . . ? C1 C2 Li1 O1 -133.64(15) . . . . ? B3 C2 Li1 O1 -72.03(17) . . . . ? B7 C2 Li1 O1 -6.1(3) . . . . ? B11 C2 Li1 O1 89.9(3) . . . . ? B6 C2 Li1 O1 164.95(14) . . . . ? C3 N2 Li2 O4 112.9(5) . . . . ? C7 N2 Li2 O4 -70.2(6) . . . . ? C3 N2 Li2 O3 -106.76(19) . . . . ? C7 N2 Li2 O3 70.2(2) . . . . ? C3 N2 Li2 B4 0.39(18) . . . . ? C7 N2 Li2 B4 177.31(12) . . . . ? C3 N2 Li2 B5 38.42(17) . . . . ? C7 N2 Li2 B5 -144.66(13) . . . . ? C3 N2 Li2 C14 -98.7(3) . . . . ? C7 N2 Li2 C14 78.2(3) . . . . ? C17 O4 Li2 N2 -15.4(7) . . . . ? C15 O4 Li2 N2 137.0(5) . . . . ? C17 O4 Li2 O3 -158.99(17) . . . . ? C15 O4 Li2 O3 -6.6(2) . . . . ? C17 O4 Li2 B4 93.4(2) . . . . ? C15 O4 Li2 B4 -114.26(18) . . . . ? C17 O4 Li2 B5 55.6(2) . . . . ? C15 O4 Li2 B5 -152.01(17) . . . . ? C17 O4 Li2 C14 -172.2(2) . . . . ? C15 O4 Li2 C14 -19.83(17) . . . . ? C14 O3 Li2 N2 169.60(19) . . . . ? C16 O3 Li2 N2 33.0(3) . . . . ? C14 O3 Li2 O4 -22.88(19) . . . . ? C16 O3 Li2 O4 -159.48(16) . . . . ? C14 O3 Li2 B4 80.36(19) . . . . ? C16 O3 Li2 B4 -56.2(2) . . . . ? C14 O3 Li2 B5 69.8(3) . . . . ? C16 O3 Li2 B5 -66.8(3) . . . . ? C16 O3 Li2 C14 -136.6(3) . . . . ? C1 B4 Li2 N2 19.11(12) . . . . ? B5 B4 Li2 N2 78.52(13) . . . . ? B9 B4 Li2 N2 123.70(15) . . . . ? B8 B4 Li2 N2 172.2(7) . . . . ? B3 B4 Li2 N2 -19.1(2) . . . . ? C1 B4 Li2 O4 -142.14(15) . . . . ? B5 B4 Li2 O4 -82.73(15) . . . . ? B9 B4 Li2 O4 -37.55(19) . . . . ? B8 B4 Li2 O4 11.0(8) . . . . ? B3 B4 Li2 O4 179.68(16) . . . . ? C1 B4 Li2 O3 130.35(15) . . . . ? B5 B4 Li2 O3 -170.24(17) . . . . ? B9 B4 Li2 O3 -125.06(16) . . . . ? B8 B4 Li2 O3 -76.5(8) . . . . ? B3 B4 Li2 O3 92.2(2) . . . . ? C1 B4 Li2 B5 -59.42(10) . . . . ? B9 B4 Li2 B5 45.18(13) . . . . ? B8 B4 Li2 B5 93.7(8) . . . . ? B3 B4 Li2 B5 -97.59(19) . . . . ? C1 B4 Li2 C14 159.82(13) . . . . ? B5 B4 Li2 C14 -140.76(14) . . . . ? B9 B4 Li2 C14 -95.58(15) . . . . ? B8 B4 Li2 C14 -47.1(8) . . . . ? B3 B4 Li2 C14 121.65(17) . . . . ? C1 B5 Li2 N2 -35.21(11) . . . . ? B4 B5 Li2 N2 -94.32(12) . . . . ? B10 B5 Li2 N2 -180(100) . . . . ? B9 B5 Li2 N2 -139.16(13) . . . . ? B6 B5 Li2 N2 1.99(19) . . . . ? C1 B5 Li2 O4 163.86(14) . . . . ? B4 B5 Li2 O4 104.75(15) . . . . ? B10 B5 Li2 O4 19.2(8) . . . . ? B9 B5 Li2 O4 59.92(17) . . . . ? B6 B5 Li2 O4 -158.94(15) . . . . ? C1 B5 Li2 O3 75.6(3) . . . . ? B4 B5 Li2 O3 16.5(3) . . . . ? B10 B5 Li2 O3 -69.1(9) . . . . ? B9 B5 Li2 O3 -28.3(3) . . . . ? B6 B5 Li2 O3 112.8(3) . . . . ? C1 B5 Li2 B4 59.11(10) . . . . ? B10 B5 Li2 B4 -85.6(8) . . . . ? B9 B5 Li2 B4 -44.83(12) . . . . ? B6 B5 Li2 B4 96.31(18) . . . . ? C1 B5 Li2 C14 111.60(18) . . . . ? B4 B5 Li2 C14 52.49(18) . . . . ? B10 B5 Li2 C14 -33.1(9) . . . . ? B9 B5 Li2 C14 7.7(2) . . . . ? B6 B5 Li2 C14 148.80(17) . . . . ? O3 C14 Li2 N2 -15.4(3) . . . . ? C15 C14 Li2 N2 -149.5(3) . . . . ? O3 C14 Li2 O4 152.4(2) . . . . ? C15 C14 Li2 O4 18.27(14) . . . . ? C15 C14 Li2 O3 -134.1(3) . . . . ? O3 C14 Li2 B4 -107.56(19) . . . . ? C15 C14 Li2 B4 118.30(18) . . . . ? O3 C14 Li2 B5 -137.3(2) . . . . ? C15 C14 Li2 B5 88.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 29.24 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.209 _refine_diff_density_min -0.160 _refine_diff_density_rms 0.038 _database_code_depnum_ccdc_archive 'CCDC 963126' ####################################################################### # # 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_ip187 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H42 B10 N2 Si2' _chemical_formula_weight 414.79 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.616(3) _cell_length_b 9.2632(19) _cell_length_c 19.139(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.97(3) _cell_angle_gamma 90.00 _cell_volume 2567.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 8728 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 29.28 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.073 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 0.144 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'plane graphite' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13083 _diffrn_reflns_av_R_equivalents 0.0842 _diffrn_reflns_av_sigmaI/netI 0.1343 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 26.37 _reflns_number_total 5204 _reflns_number_gt 3066 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0309P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5204 _refine_ls_number_parameters 312 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1222 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.0998 _refine_ls_wR_factor_gt 0.0874 _refine_ls_goodness_of_fit_ref 0.916 _refine_ls_restrained_S_all 0.916 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.57378(5) 1.14216(8) 0.72172(4) 0.01956(19) Uani 1 1 d . . . Si2 Si 0.24652(5) 1.59025(9) 0.56054(5) 0.0245(2) Uani 1 1 d . . . N1 N 0.29343(12) 1.4372(2) 0.61595(12) 0.0192(5) Uani 1 1 d . . . N2 N 0.41506(13) 1.3074(2) 0.59299(12) 0.0181(5) Uani 1 1 d . . . C1 C 0.45797(15) 1.4348(3) 0.70788(14) 0.0177(6) Uani 1 1 d . . . C2 C 0.55230(15) 1.3314(3) 0.75326(14) 0.0169(6) Uani 1 1 d . . . C3 C 0.38461(15) 1.3851(3) 0.63184(14) 0.0146(6) Uani 1 1 d . . . C4 C 0.24056(17) 1.3458(3) 0.65081(16) 0.0288(7) Uani 1 1 d . . . H4 H 0.2873 1.2984 0.6959 0.035 Uiso 1 1 calc R . . C5 C 0.1877(2) 1.2260(4) 0.5990(2) 0.0444(9) Uani 1 1 d . . . H5A H 0.1419 1.2678 0.5532 0.067 Uiso 1 1 calc R . . H5B H 0.1562 1.1672 0.6247 0.067 Uiso 1 1 calc R . . H5C H 0.2306 1.1654 0.5856 0.067 Uiso 1 1 calc R . . C6 C 0.17689(19) 1.4326(4) 0.67905(19) 0.0402(8) Uani 1 1 d . . . H6A H 0.2123 1.5092 0.7129 0.060 Uiso 1 1 calc R . . H6B H 0.1502 1.3686 0.7064 0.060 Uiso 1 1 calc R . . H6C H 0.1272 1.4757 0.6361 0.060 Uiso 1 1 calc R . . C7 C 0.35923(17) 1.2595(3) 0.51581(15) 0.0259(7) Uani 1 1 d . . . H7 H 0.2960 1.3023 0.4993 0.031 Uiso 1 1 calc R . . C8 C 0.40648(19) 1.3090(4) 0.46430(16) 0.0352(8) Uani 1 1 d . . . H8A H 0.4151 1.4138 0.4685 0.053 Uiso 1 1 calc R . . H8B H 0.3683 1.2836 0.4122 0.053 Uiso 1 1 calc R . . H8C H 0.4668 1.2616 0.4787 0.053 Uiso 1 1 calc R . . C9 C 0.35295(19) 1.0951(3) 0.51421(18) 0.0363(8) Uani 1 1 d . . . H9A H 0.4153 1.0540 0.5320 0.054 Uiso 1 1 calc R . . H9B H 0.3183 1.0627 0.4625 0.054 Uiso 1 1 calc R . . H9C H 0.3212 1.0631 0.5470 0.054 Uiso 1 1 calc R . . C10 C 0.4706(2) 1.0275(3) 0.70630(19) 0.0361(8) Uani 1 1 d . . . H10A H 0.4148 1.0807 0.6760 0.054 Uiso 1 1 calc R . . H10B H 0.4675 1.0023 0.7550 0.054 Uiso 1 1 calc R . . H10C H 0.4751 0.9391 0.6797 0.054 Uiso 1 1 calc R . . C11 C 0.61485(19) 1.1522(3) 0.64342(16) 0.0318(7) Uani 1 1 d . . . H11A H 0.6737 1.2043 0.6599 0.048 Uiso 1 1 calc R . . H11B H 0.5692 1.2033 0.6009 0.048 Uiso 1 1 calc R . . H11C H 0.6235 1.0544 0.6277 0.048 Uiso 1 1 calc R . . C12 C 0.67047(19) 1.0621(3) 0.80279(16) 0.0328(8) Uani 1 1 d . . . H12A H 0.6855 0.9664 0.7887 0.049 Uiso 1 1 calc R . . H12B H 0.6519 1.0532 0.8461 0.049 Uiso 1 1 calc R . . H12C H 0.7249 1.1247 0.8160 0.049 Uiso 1 1 calc R . . C13 C 0.12804(18) 1.5512(4) 0.49085(17) 0.0382(9) Uani 1 1 d . . . H13A H 0.1284 1.4592 0.4657 0.057 Uiso 1 1 calc R . . H13B H 0.1087 1.6287 0.4533 0.057 Uiso 1 1 calc R . . H13C H 0.0849 1.5453 0.5170 0.057 Uiso 1 1 calc R . . C14 C 0.2379(2) 1.7509(3) 0.6158(2) 0.0398(9) Uani 1 1 d . . . H14A H 0.1960 1.7296 0.6420 0.060 Uiso 1 1 calc R . . H14B H 0.2139 1.8330 0.5818 0.060 Uiso 1 1 calc R . . H14C H 0.2992 1.7747 0.6529 0.060 Uiso 1 1 calc R . . C15 C 0.32039(19) 1.6388(3) 0.50759(18) 0.0357(8) Uani 1 1 d . . . H15A H 0.3854 1.6246 0.5398 0.053 Uiso 1 1 calc R . . H15B H 0.3101 1.7402 0.4921 0.053 Uiso 1 1 calc R . . H15C H 0.3047 1.5773 0.4629 0.053 Uiso 1 1 calc R . . B3 B 0.4696(2) 1.3556(4) 0.79175(17) 0.0259(8) Uani 1 1 d . . . H13 H 0.4258(17) 1.263(3) 0.7929(14) 0.021(7) Uiso 1 1 d . . . B4 B 0.5895(2) 1.3648(4) 0.84834(17) 0.0270(8) Uani 1 1 d . . . H14 H 0.6187(18) 1.277(3) 0.8832(16) 0.031(8) Uiso 1 1 d . . . B5 B 0.6466(2) 1.4409(3) 0.79408(18) 0.0250(8) Uani 1 1 d . . . H15 H 0.7127(16) 1.399(3) 0.7928(13) 0.018(6) Uiso 1 1 d . . . B6 B 0.56375(19) 1.4807(3) 0.70339(19) 0.0222(8) Uani 1 1 d . . . H16 H 0.5735(17) 1.468(3) 0.6524(15) 0.025(8) Uiso 1 1 d . . . B7 B 0.4872(2) 1.6123(3) 0.7153(2) 0.0296(9) Uani 1 1 d . . . H17 H 0.4495(17) 1.680(3) 0.6678(15) 0.025(7) Uiso 1 1 d . . . B8 B 0.4304(2) 1.5361(4) 0.7699(2) 0.0333(9) Uani 1 1 d . . . H18 H 0.3594(18) 1.561(3) 0.7589(15) 0.034(8) Uiso 1 1 d . . . B9 B 0.5130(2) 1.4950(4) 0.8602(2) 0.0377(10) Uani 1 1 d . . . H19 H 0.4962(18) 1.498(3) 0.9078(17) 0.039(9) Uiso 1 1 d . . . B10 B 0.6230(2) 1.5483(4) 0.8607(2) 0.0367(10) Uani 1 1 d . . . H20 H 0.6768(16) 1.588(3) 0.9077(14) 0.018(7) Uiso 1 1 d . . . B11 B 0.6071(2) 1.6198(4) 0.7707(2) 0.0381(11) Uani 1 1 d . . . H21 H 0.6473(19) 1.705(3) 0.7600(16) 0.033(8) Uiso 1 1 d . . . B12 B 0.5241(2) 1.6528(4) 0.8128(2) 0.0451(12) Uani 1 1 d . . . H22 H 0.5132(19) 1.756(3) 0.8290(17) 0.042(9) Uiso 1 1 d . . . 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 Si1 0.0222(3) 0.0139(4) 0.0217(4) -0.0012(3) 0.0072(3) 0.0022(3) Si2 0.0197(4) 0.0270(4) 0.0245(4) 0.0035(4) 0.0057(3) 0.0044(3) N1 0.0123(9) 0.0252(13) 0.0186(11) 0.0014(10) 0.0040(9) 0.0003(9) N2 0.0163(10) 0.0207(12) 0.0158(12) -0.0021(10) 0.0043(9) -0.0026(9) C1 0.0152(11) 0.0163(14) 0.0195(14) -0.0020(11) 0.0041(11) 0.0053(10) C2 0.0144(11) 0.0159(14) 0.0167(13) 0.0000(11) 0.0018(10) 0.0034(10) C3 0.0147(11) 0.0135(13) 0.0156(13) 0.0003(11) 0.0058(10) -0.0009(10) C4 0.0222(13) 0.0366(18) 0.0296(16) 0.0100(15) 0.0118(12) -0.0022(13) C5 0.0418(19) 0.042(2) 0.062(2) -0.0023(18) 0.0342(18) -0.0132(15) C6 0.0334(16) 0.059(2) 0.0391(18) 0.0005(18) 0.0258(14) -0.0029(16) C7 0.0165(13) 0.0385(18) 0.0191(16) -0.0072(13) 0.0024(12) 0.0010(12) C8 0.0295(15) 0.055(2) 0.0220(16) -0.0017(15) 0.0101(13) 0.0051(14) C9 0.0322(15) 0.0375(19) 0.0336(18) -0.0187(15) 0.0057(13) -0.0086(14) C10 0.0426(17) 0.0215(16) 0.043(2) 0.0015(15) 0.0150(15) -0.0064(13) C11 0.0299(14) 0.0405(18) 0.0246(15) -0.0049(15) 0.0098(12) 0.0115(14) C12 0.0407(16) 0.0236(17) 0.0320(17) 0.0017(14) 0.0114(14) 0.0122(13) C13 0.0254(14) 0.051(2) 0.0314(18) 0.0098(16) 0.0027(13) 0.0061(14) C14 0.0390(18) 0.0342(18) 0.045(2) -0.0005(16) 0.0151(16) 0.0098(14) C15 0.0357(15) 0.0318(17) 0.0411(18) 0.0115(16) 0.0162(14) 0.0028(14) B3 0.0222(14) 0.038(2) 0.0174(16) -0.0023(16) 0.0069(13) 0.0059(15) B4 0.0257(15) 0.0340(19) 0.0150(16) -0.0042(15) 0.0005(13) 0.0112(14) B5 0.0227(15) 0.0180(17) 0.0253(18) -0.0038(14) -0.0014(14) 0.0003(13) B6 0.0154(14) 0.0194(17) 0.0261(19) 0.0030(14) 0.0012(13) -0.0033(12) B7 0.0270(15) 0.0150(17) 0.0323(19) -0.0038(15) -0.0057(15) 0.0030(13) B8 0.0287(17) 0.038(2) 0.0251(19) -0.0148(17) 0.0009(15) 0.0147(16) B9 0.0318(18) 0.051(3) 0.0216(19) -0.0165(18) -0.0002(16) 0.0176(17) B10 0.0293(17) 0.0279(19) 0.036(2) -0.0157(17) -0.0075(16) 0.0083(15) B11 0.0247(16) 0.0182(19) 0.050(2) -0.0070(17) -0.0105(16) -0.0020(14) B12 0.0376(19) 0.030(2) 0.044(2) -0.0231(19) -0.0117(18) 0.0127(17) _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 Si1 C11 1.840(3) . ? Si1 C10 1.859(3) . ? Si1 C12 1.866(3) . ? Si1 C2 1.924(3) . ? Si2 N1 1.758(2) . ? Si2 C15 1.853(3) . ? Si2 C14 1.860(3) . ? Si2 C13 1.867(3) . ? N1 C3 1.425(3) . ? N1 C4 1.502(4) . ? N2 C3 1.249(3) . ? N2 C7 1.475(3) . ? C1 C3 1.547(3) . ? C1 B8 1.690(4) . ? C1 C2 1.698(3) . ? C1 B7 1.698(4) . ? C1 B3 1.712(4) . ? C1 B6 1.739(4) . ? C2 B5 1.717(4) . ? C2 B4 1.719(4) . ? C2 B3 1.724(4) . ? C2 B6 1.727(4) . ? C4 C5 1.511(4) . ? C4 C6 1.526(4) . ? C4 H4 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.507(4) . ? C7 C9 1.526(4) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? B3 B8 1.776(5) . ? B3 B4 1.780(4) . ? B3 B9 1.783(5) . ? B3 H13 1.10(3) . ? B4 B5 1.751(5) . ? B4 B10 1.769(5) . ? B4 B9 1.771(5) . ? B4 H14 1.04(3) . ? B5 B10 1.762(5) . ? B5 B11 1.766(4) . ? B5 B6 1.773(4) . ? B5 H15 1.11(2) . ? B6 B11 1.768(5) . ? B6 B7 1.782(5) . ? B6 H16 1.05(3) . ? B7 B8 1.752(6) . ? B7 B12 1.774(5) . ? B7 B11 1.775(4) . ? B7 H17 1.08(3) . ? B8 B12 1.757(5) . ? B8 B9 1.769(5) . ? B8 H18 1.07(3) . ? B9 B12 1.763(7) . ? B9 B10 1.784(6) . ? B9 H19 1.04(3) . ? B10 B12 1.761(4) . ? B10 B11 1.773(6) . ? B10 H20 1.04(2) . ? B11 B12 1.789(6) . ? B11 H21 1.07(3) . ? B12 H22 1.04(3) . ? 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 C11 Si1 C10 116.43(15) . . ? C11 Si1 C12 106.09(14) . . ? C10 Si1 C12 106.78(15) . . ? C11 Si1 C2 111.37(14) . . ? C10 Si1 C2 109.13(13) . . ? C12 Si1 C2 106.44(12) . . ? N1 Si2 C15 108.76(12) . . ? N1 Si2 C14 113.85(13) . . ? C15 Si2 C14 108.03(17) . . ? N1 Si2 C13 110.65(13) . . ? C15 Si2 C13 108.03(15) . . ? C14 Si2 C13 107.35(15) . . ? C3 N1 C4 112.68(19) . . ? C3 N1 Si2 124.06(18) . . ? C4 N1 Si2 123.26(16) . . ? C3 N2 C7 123.7(2) . . ? C3 C1 B8 122.1(2) . . ? C3 C1 C2 120.6(2) . . ? B8 C1 C2 110.75(19) . . ? C3 C1 B7 116.6(2) . . ? B8 C1 B7 62.2(2) . . ? C2 C1 B7 110.42(18) . . ? C3 C1 B3 122.4(2) . . ? B8 C1 B3 62.9(2) . . ? C2 C1 B3 60.73(16) . . ? B7 C1 B3 113.9(2) . . ? C3 C1 B6 114.1(2) . . ? B8 C1 B6 113.3(2) . . ? C2 C1 B6 60.32(16) . . ? B7 C1 B6 62.44(19) . . ? B3 C1 B6 112.43(19) . . ? C1 C2 B5 109.38(19) . . ? C1 C2 B4 109.0(2) . . ? B5 C2 B4 61.27(19) . . ? C1 C2 B3 60.02(16) . . ? B5 C2 B3 112.4(2) . . ? B4 C2 B3 62.27(18) . . ? C1 C2 B6 61.00(16) . . ? B5 C2 B6 61.95(17) . . ? B4 C2 B6 112.2(2) . . ? B3 C2 B6 112.4(2) . . ? C1 C2 Si1 124.97(15) . . ? B5 C2 Si1 117.42(17) . . ? B4 C2 Si1 117.81(18) . . ? B3 C2 Si1 119.92(19) . . ? B6 C2 Si1 119.3(2) . . ? N2 C3 N1 129.8(2) . . ? N2 C3 C1 114.7(2) . . ? N1 C3 C1 115.4(2) . . ? N1 C4 C5 112.3(3) . . ? N1 C4 C6 113.6(2) . . ? C5 C4 C6 110.5(2) . . ? N1 C4 H4 106.7 . . ? C5 C4 H4 106.7 . . ? C6 C4 H4 106.7 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 108.2(2) . . ? N2 C7 C9 109.3(2) . . ? C8 C7 C9 109.5(3) . . ? N2 C7 H7 109.9 . . ? C8 C7 H7 109.9 . . ? C9 C7 H7 109.9 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si1 C12 H12A 109.5 . . ? Si1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si2 C13 H13A 109.5 . . ? Si2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si2 C14 H14A 109.5 . . ? Si2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si2 C15 H15A 109.5 . . ? Si2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C1 B3 C2 59.25(16) . . ? C1 B3 B8 57.94(19) . . ? C2 B3 B8 105.6(3) . . ? C1 B3 B4 105.6(2) . . ? C2 B3 B4 58.72(17) . . ? B8 B3 B4 106.9(3) . . ? C1 B3 B9 104.9(3) . . ? C2 B3 B9 105.6(2) . . ? B8 B3 B9 59.6(2) . . ? B4 B3 B9 59.61(18) . . ? C1 B3 H13 120.2(13) . . ? C2 B3 H13 118.6(14) . . ? B8 B3 H13 124.9(13) . . ? B4 B3 H13 123.1(13) . . ? B9 B3 H13 128.0(15) . . ? C2 B4 B5 59.33(18) . . ? C2 B4 B10 106.3(3) . . ? B5 B4 B10 60.1(2) . . ? C2 B4 B9 106.3(2) . . ? B5 B4 B9 108.6(3) . . ? B10 B4 B9 60.5(2) . . ? C2 B4 B3 59.01(16) . . ? B5 B4 B3 108.2(2) . . ? B10 B4 B3 108.6(2) . . ? B9 B4 B3 60.29(19) . . ? C2 B4 H14 115.6(16) . . ? B5 B4 H14 119.7(17) . . ? B10 B4 H14 128.8(14) . . ? B9 B4 H14 127.1(17) . . ? B3 B4 H14 117.5(15) . . ? C2 B5 B4 59.40(17) . . ? C2 B5 B10 106.7(3) . . ? B4 B5 B10 60.5(2) . . ? C2 B5 B11 106.25(19) . . ? B4 B5 B11 108.7(3) . . ? B10 B5 B11 60.3(2) . . ? C2 B5 B6 59.29(16) . . ? B4 B5 B6 108.5(2) . . ? B10 B5 B6 108.5(2) . . ? B11 B5 B6 59.96(17) . . ? C2 B5 H15 115.3(12) . . ? B4 B5 H15 123.7(13) . . ? B10 B5 H15 131.4(12) . . ? B11 B5 H15 124.2(13) . . ? B6 B5 H15 113.2(13) . . ? C2 B6 C1 58.68(16) . . ? C2 B6 B11 105.7(2) . . ? C1 B6 B11 104.7(3) . . ? C2 B6 B5 58.75(16) . . ? C1 B6 B5 105.1(2) . . ? B11 B6 B5 59.83(18) . . ? C2 B6 B7 105.3(3) . . ? C1 B6 B7 57.68(17) . . ? B11 B6 B7 59.99(18) . . ? B5 B6 B7 107.2(3) . . ? C2 B6 H16 120.4(15) . . ? C1 B6 H16 119.4(14) . . ? B11 B6 H16 127.6(15) . . ? B5 B6 H16 125.5(14) . . ? B7 B6 H16 122.3(14) . . ? C1 B7 B8 58.64(19) . . ? C1 B7 B12 105.3(3) . . ? B8 B7 B12 59.8(2) . . ? C1 B7 B11 106.1(2) . . ? B8 B7 B11 108.4(3) . . ? B12 B7 B11 60.5(2) . . ? C1 B7 B6 59.88(17) . . ? B8 B7 B6 108.3(2) . . ? B12 B7 B6 108.0(2) . . ? B11 B7 B6 59.63(18) . . ? C1 B7 H17 116.6(13) . . ? B8 B7 H17 119.9(15) . . ? B12 B7 H17 128.6(14) . . ? B11 B7 H17 126.9(14) . . ? B6 B7 H17 118.0(15) . . ? C1 B8 B7 59.11(19) . . ? C1 B8 B12 106.4(3) . . ? B7 B8 B12 60.7(2) . . ? C1 B8 B9 106.4(2) . . ? B7 B8 B9 108.8(3) . . ? B12 B8 B9 60.0(2) . . ? C1 B8 B3 59.12(18) . . ? B7 B8 B3 108.2(2) . . ? B12 B8 B3 108.4(2) . . ? B9 B8 B3 60.39(19) . . ? C1 B8 H18 119.9(15) . . ? B7 B8 H18 120.8(16) . . ? B12 B8 H18 125.2(15) . . ? B9 B8 H18 124.1(16) . . ? B3 B8 H18 119.4(15) . . ? B12 B9 B8 59.7(2) . . ? B12 B9 B4 107.3(3) . . ? B8 B9 B4 107.5(3) . . ? B12 B9 B3 107.8(3) . . ? B8 B9 B3 59.99(19) . . ? B4 B9 B3 60.10(18) . . ? B12 B9 B10 59.5(2) . . ? B8 B9 B10 107.1(3) . . ? B4 B9 B10 59.7(2) . . ? B3 B9 B10 107.7(3) . . ? B12 B9 H19 122.5(18) . . ? B8 B9 H19 121.4(15) . . ? B4 B9 H19 122.2(17) . . ? B3 B9 H19 120.7(17) . . ? B10 B9 H19 123.2(15) . . ? B12 B10 B5 108.3(2) . . ? B12 B10 B4 107.5(2) . . ? B5 B10 B4 59.46(19) . . ? B12 B10 B11 60.8(2) . . ? B5 B10 B11 59.9(2) . . ? B4 B10 B11 107.6(2) . . ? B12 B10 B9 59.6(2) . . ? B5 B10 B9 107.6(2) . . ? B4 B10 B9 59.8(2) . . ? B11 B10 B9 108.3(2) . . ? B12 B10 H20 121.5(14) . . ? B5 B10 H20 120.3(15) . . ? B4 B10 H20 123.9(14) . . ? B11 B10 H20 118.8(15) . . ? B9 B10 H20 124.5(15) . . ? B5 B11 B6 60.21(17) . . ? B5 B11 B10 59.7(2) . . ? B6 B11 B10 108.2(3) . . ? B5 B11 B7 107.8(2) . . ? B6 B11 B7 60.38(17) . . ? B10 B11 B7 107.4(3) . . ? B5 B11 B12 106.9(3) . . ? B6 B11 B12 108.0(2) . . ? B10 B11 B12 59.3(2) . . ? B7 B11 B12 59.7(2) . . ? B5 B11 H21 124.2(15) . . ? B6 B11 H21 119.2(17) . . ? B10 B11 H21 125.4(15) . . ? B7 B11 H21 118.4(14) . . ? B12 B11 H21 122.3(16) . . ? B8 B12 B10 108.7(3) . . ? B8 B12 B9 60.4(2) . . ? B10 B12 B9 60.8(2) . . ? B8 B12 B7 59.5(2) . . ? B10 B12 B7 108.0(3) . . ? B9 B12 B7 108.1(2) . . ? B8 B12 B11 107.6(3) . . ? B10 B12 B11 59.9(2) . . ? B9 B12 B11 108.5(3) . . ? B7 B12 B11 59.8(2) . . ? B8 B12 H22 120.3(16) . . ? B10 B12 H22 124.0(15) . . ? B9 B12 H22 123.4(19) . . ? B7 B12 H22 118.9(17) . . ? B11 B12 H22 121.2(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 Si2 N1 C3 15.0(2) . . . . ? C14 Si2 N1 C3 -105.5(2) . . . . ? C13 Si2 N1 C3 133.5(2) . . . . ? C15 Si2 N1 C4 -164.1(2) . . . . ? C14 Si2 N1 C4 75.4(2) . . . . ? C13 Si2 N1 C4 -45.6(3) . . . . ? C3 C1 C2 B5 142.2(2) . . . . ? B8 C1 C2 B5 -65.6(3) . . . . ? B7 C1 C2 B5 1.4(3) . . . . ? B3 C1 C2 B5 -105.3(2) . . . . ? B6 C1 C2 B5 40.1(2) . . . . ? C3 C1 C2 B4 -152.5(2) . . . . ? B8 C1 C2 B4 -0.3(3) . . . . ? B7 C1 C2 B4 66.7(3) . . . . ? B3 C1 C2 B4 -40.0(2) . . . . ? B6 C1 C2 B4 105.4(2) . . . . ? C3 C1 C2 B3 -112.5(3) . . . . ? B8 C1 C2 B3 39.7(2) . . . . ? B7 C1 C2 B3 106.7(3) . . . . ? B6 C1 C2 B3 145.4(2) . . . . ? C3 C1 C2 B6 102.1(3) . . . . ? B8 C1 C2 B6 -105.7(2) . . . . ? B7 C1 C2 B6 -38.7(2) . . . . ? B3 C1 C2 B6 -145.4(2) . . . . ? C3 C1 C2 Si1 -5.1(3) . . . . ? B8 C1 C2 Si1 147.1(2) . . . . ? B7 C1 C2 Si1 -145.9(2) . . . . ? B3 C1 C2 Si1 107.4(2) . . . . ? B6 C1 C2 Si1 -107.2(2) . . . . ? C11 Si1 C2 C1 78.4(2) . . . . ? C10 Si1 C2 C1 -51.6(3) . . . . ? C12 Si1 C2 C1 -166.4(2) . . . . ? C11 Si1 C2 B5 -66.6(2) . . . . ? C10 Si1 C2 B5 163.5(2) . . . . ? C12 Si1 C2 B5 48.6(2) . . . . ? C11 Si1 C2 B4 -136.8(2) . . . . ? C10 Si1 C2 B4 93.3(2) . . . . ? C12 Si1 C2 B4 -21.6(2) . . . . ? C11 Si1 C2 B3 150.84(17) . . . . ? C10 Si1 C2 B3 20.9(2) . . . . ? C12 Si1 C2 B3 -94.0(2) . . . . ? C11 Si1 C2 B6 5.0(2) . . . . ? C10 Si1 C2 B6 -124.96(18) . . . . ? C12 Si1 C2 B6 120.15(18) . . . . ? C7 N2 C3 N1 4.3(4) . . . . ? C7 N2 C3 C1 -174.0(2) . . . . ? C4 N1 C3 N2 97.1(3) . . . . ? Si2 N1 C3 N2 -82.0(3) . . . . ? C4 N1 C3 C1 -84.6(3) . . . . ? Si2 N1 C3 C1 96.3(2) . . . . ? B8 C1 C3 N2 -178.1(3) . . . . ? C2 C1 C3 N2 -29.1(3) . . . . ? B7 C1 C3 N2 109.4(3) . . . . ? B3 C1 C3 N2 -101.8(3) . . . . ? B6 C1 C3 N2 39.4(3) . . . . ? B8 C1 C3 N1 3.4(4) . . . . ? C2 C1 C3 N1 152.3(2) . . . . ? B7 C1 C3 N1 -69.1(3) . . . . ? B3 C1 C3 N1 79.6(3) . . . . ? B6 C1 C3 N1 -139.1(2) . . . . ? C3 N1 C4 C5 -90.1(3) . . . . ? Si2 N1 C4 C5 89.0(3) . . . . ? C3 N1 C4 C6 143.6(2) . . . . ? Si2 N1 C4 C6 -37.3(3) . . . . ? C3 N2 C7 C8 122.9(3) . . . . ? C3 N2 C7 C9 -117.9(3) . . . . ? C3 C1 B3 C2 109.6(2) . . . . ? B8 C1 B3 C2 -137.9(2) . . . . ? B7 C1 B3 C2 -100.9(2) . . . . ? B6 C1 B3 C2 -32.3(2) . . . . ? C3 C1 B3 B8 -112.5(3) . . . . ? C2 C1 B3 B8 137.9(2) . . . . ? B7 C1 B3 B8 37.0(2) . . . . ? B6 C1 B3 B8 105.7(2) . . . . ? C3 C1 B3 B4 147.1(2) . . . . ? B8 C1 B3 B4 -100.4(3) . . . . ? C2 C1 B3 B4 37.5(2) . . . . ? B7 C1 B3 B4 -63.4(3) . . . . ? B6 C1 B3 B4 5.3(3) . . . . ? C3 C1 B3 B9 -150.9(2) . . . . ? B8 C1 B3 B9 -38.4(2) . . . . ? C2 C1 B3 B9 99.5(2) . . . . ? B7 C1 B3 B9 -1.4(3) . . . . ? B6 C1 B3 B9 67.3(3) . . . . ? B5 C2 B3 C1 100.2(2) . . . . ? B4 C2 B3 C1 136.6(2) . . . . ? B6 C2 B3 C1 32.51(19) . . . . ? Si1 C2 B3 C1 -115.56(19) . . . . ? C1 C2 B3 B8 -36.13(17) . . . . ? B5 C2 B3 B8 64.0(2) . . . . ? B4 C2 B3 B8 100.5(2) . . . . ? B6 C2 B3 B8 -3.6(3) . . . . ? Si1 C2 B3 B8 -151.69(17) . . . . ? C1 C2 B3 B4 -136.6(2) . . . . ? B5 C2 B3 B4 -36.5(2) . . . . ? B6 C2 B3 B4 -104.1(2) . . . . ? Si1 C2 B3 B4 107.8(2) . . . . ? C1 C2 B3 B9 -98.3(2) . . . . ? B5 C2 B3 B9 1.9(3) . . . . ? B4 C2 B3 B9 38.4(2) . . . . ? B6 C2 B3 B9 -65.8(3) . . . . ? Si1 C2 B3 B9 146.2(2) . . . . ? C1 C2 B4 B5 -102.2(2) . . . . ? B3 C2 B4 B5 -141.2(2) . . . . ? B6 C2 B4 B5 -36.7(2) . . . . ? Si1 C2 B4 B5 107.7(2) . . . . ? C1 C2 B4 B10 -63.3(3) . . . . ? B5 C2 B4 B10 39.0(2) . . . . ? B3 C2 B4 B10 -102.2(3) . . . . ? B6 C2 B4 B10 2.3(3) . . . . ? Si1 C2 B4 B10 146.69(19) . . . . ? C1 C2 B4 B9 0.1(3) . . . . ? B5 C2 B4 B9 102.3(3) . . . . ? B3 C2 B4 B9 -38.9(3) . . . . ? B6 C2 B4 B9 65.7(3) . . . . ? Si1 C2 B4 B9 -150.0(2) . . . . ? C1 C2 B4 B3 39.0(2) . . . . ? B5 C2 B4 B3 141.2(2) . . . . ? B6 C2 B4 B3 104.5(2) . . . . ? Si1 C2 B4 B3 -111.1(2) . . . . ? C1 B3 B4 C2 -37.8(2) . . . . ? B8 B3 B4 C2 -98.3(3) . . . . ? B9 B3 B4 C2 -136.1(3) . . . . ? C1 B3 B4 B5 -3.2(3) . . . . ? C2 B3 B4 B5 34.6(2) . . . . ? B8 B3 B4 B5 -63.8(3) . . . . ? B9 B3 B4 B5 -101.5(3) . . . . ? C1 B3 B4 B10 60.5(3) . . . . ? C2 B3 B4 B10 98.2(3) . . . . ? B8 B3 B4 B10 -0.1(3) . . . . ? B9 B3 B4 B10 -37.9(3) . . . . ? C1 B3 B4 B9 98.3(3) . . . . ? C2 B3 B4 B9 136.1(3) . . . . ? B8 B3 B4 B9 37.8(3) . . . . ? C1 C2 B5 B4 101.5(2) . . . . ? B3 C2 B5 B4 36.9(2) . . . . ? B6 C2 B5 B4 141.2(2) . . . . ? Si1 C2 B5 B4 -108.4(2) . . . . ? C1 C2 B5 B10 62.3(3) . . . . ? B4 C2 B5 B10 -39.2(2) . . . . ? B3 C2 B5 B10 -2.3(3) . . . . ? B6 C2 B5 B10 102.0(2) . . . . ? Si1 C2 B5 B10 -147.6(2) . . . . ? C1 C2 B5 B11 -0.9(3) . . . . ? B4 C2 B5 B11 -102.4(3) . . . . ? B3 C2 B5 B11 -65.6(3) . . . . ? B6 C2 B5 B11 38.8(3) . . . . ? Si1 C2 B5 B11 149.2(2) . . . . ? C1 C2 B5 B6 -39.7(2) . . . . ? B4 C2 B5 B6 -141.2(2) . . . . ? B3 C2 B5 B6 -104.3(2) . . . . ? Si1 C2 B5 B6 110.4(2) . . . . ? B10 B4 B5 C2 -135.9(2) . . . . ? B9 B4 B5 C2 -98.4(2) . . . . ? B3 B4 B5 C2 -34.4(2) . . . . ? C2 B4 B5 B10 135.9(2) . . . . ? B9 B4 B5 B10 37.5(2) . . . . ? B3 B4 B5 B10 101.4(3) . . . . ? C2 B4 B5 B11 98.2(2) . . . . ? B10 B4 B5 B11 -37.63(19) . . . . ? B9 B4 B5 B11 -0.1(3) . . . . ? B3 B4 B5 B11 63.8(3) . . . . ? C2 B4 B5 B6 34.6(2) . . . . ? B10 B4 B5 B6 -101.3(2) . . . . ? B9 B4 B5 B6 -63.8(3) . . . . ? B3 B4 B5 B6 0.2(3) . . . . ? B5 C2 B6 C1 -136.5(2) . . . . ? B4 C2 B6 C1 -100.1(2) . . . . ? B3 C2 B6 C1 -32.16(19) . . . . ? Si1 C2 B6 C1 116.12(18) . . . . ? C1 C2 B6 B11 97.9(2) . . . . ? B5 C2 B6 B11 -38.6(2) . . . . ? B4 C2 B6 B11 -2.2(3) . . . . ? B3 C2 B6 B11 65.7(2) . . . . ? Si1 C2 B6 B11 -146.00(19) . . . . ? C1 C2 B6 B5 136.5(2) . . . . ? B4 C2 B6 B5 36.4(2) . . . . ? B3 C2 B6 B5 104.3(2) . . . . ? Si1 C2 B6 B5 -107.4(2) . . . . ? C1 C2 B6 B7 35.38(17) . . . . ? B5 C2 B6 B7 -101.1(2) . . . . ? B4 C2 B6 B7 -64.7(2) . . . . ? B3 C2 B6 B7 3.2(2) . . . . ? Si1 C2 B6 B7 151.50(16) . . . . ? C3 C1 B6 C2 -112.7(2) . . . . ? B8 C1 B6 C2 101.5(2) . . . . ? B7 C1 B6 C2 138.6(2) . . . . ? B3 C1 B6 C2 32.4(2) . . . . ? C3 C1 B6 B11 147.6(2) . . . . ? B8 C1 B6 B11 1.8(3) . . . . ? C2 C1 B6 B11 -99.7(2) . . . . ? B7 C1 B6 B11 38.9(2) . . . . ? B3 C1 B6 B11 -67.3(3) . . . . ? C3 C1 B6 B5 -150.3(2) . . . . ? B8 C1 B6 B5 63.9(3) . . . . ? C2 C1 B6 B5 -37.57(18) . . . . ? B7 C1 B6 B5 101.1(2) . . . . ? B3 C1 B6 B5 -5.1(3) . . . . ? C3 C1 B6 B7 108.7(2) . . . . ? B8 C1 B6 B7 -37.2(2) . . . . ? C2 C1 B6 B7 -138.6(2) . . . . ? B3 C1 B6 B7 -106.2(2) . . . . ? B4 B5 B6 C2 -34.6(2) . . . . ? B10 B5 B6 C2 -98.8(3) . . . . ? B11 B5 B6 C2 -136.0(3) . . . . ? C2 B5 B6 C1 37.53(19) . . . . ? B4 B5 B6 C1 2.9(3) . . . . ? B10 B5 B6 C1 -61.2(3) . . . . ? B11 B5 B6 C1 -98.5(3) . . . . ? C2 B5 B6 B11 136.0(3) . . . . ? B4 B5 B6 B11 101.4(3) . . . . ? B10 B5 B6 B11 37.2(3) . . . . ? C2 B5 B6 B7 97.8(2) . . . . ? B4 B5 B6 B7 63.1(3) . . . . ? B10 B5 B6 B7 -1.0(3) . . . . ? B11 B5 B6 B7 -38.2(2) . . . . ? C3 C1 B7 B8 114.1(2) . . . . ? C2 C1 B7 B8 -103.4(2) . . . . ? B3 C1 B7 B8 -37.3(2) . . . . ? B6 C1 B7 B8 -141.2(2) . . . . ? C3 C1 B7 B12 153.0(2) . . . . ? B8 C1 B7 B12 38.9(2) . . . . ? C2 C1 B7 B12 -64.5(3) . . . . ? B3 C1 B7 B12 1.6(3) . . . . ? B6 C1 B7 B12 -102.2(2) . . . . ? C3 C1 B7 B11 -143.8(3) . . . . ? B8 C1 B7 B11 102.1(3) . . . . ? C2 C1 B7 B11 -1.3(3) . . . . ? B3 C1 B7 B11 64.8(3) . . . . ? B6 C1 B7 B11 -39.1(2) . . . . ? C3 C1 B7 B6 -104.7(3) . . . . ? B8 C1 B7 B6 141.2(2) . . . . ? C2 C1 B7 B6 37.8(2) . . . . ? B3 C1 B7 B6 103.9(2) . . . . ? C2 B6 B7 C1 -35.83(17) . . . . ? B11 B6 B7 C1 -135.4(3) . . . . ? B5 B6 B7 C1 -97.3(2) . . . . ? C2 B6 B7 B8 -1.5(3) . . . . ? C1 B6 B7 B8 34.34(19) . . . . ? B11 B6 B7 B8 -101.1(3) . . . . ? B5 B6 B7 B8 -62.9(3) . . . . ? C2 B6 B7 B12 61.8(3) . . . . ? C1 B6 B7 B12 97.6(3) . . . . ? B11 B6 B7 B12 -37.8(3) . . . . ? B5 B6 B7 B12 0.4(3) . . . . ? C2 B6 B7 B11 99.6(2) . . . . ? C1 B6 B7 B11 135.4(3) . . . . ? B5 B6 B7 B11 38.2(2) . . . . ? C3 C1 B8 B7 -105.5(3) . . . . ? C2 C1 B8 B7 102.8(2) . . . . ? B3 C1 B8 B7 141.5(2) . . . . ? B6 C1 B8 B7 37.3(2) . . . . ? C3 C1 B8 B12 -145.1(2) . . . . ? C2 C1 B8 B12 63.2(3) . . . . ? B7 C1 B8 B12 -39.6(2) . . . . ? B3 C1 B8 B12 101.9(2) . . . . ? B6 C1 B8 B12 -2.4(3) . . . . ? C3 C1 B8 B9 152.0(3) . . . . ? C2 C1 B8 B9 0.4(3) . . . . ? B7 C1 B8 B9 -102.4(3) . . . . ? B3 C1 B8 B9 39.1(2) . . . . ? B6 C1 B8 B9 -65.2(3) . . . . ? C3 C1 B8 B3 112.9(3) . . . . ? C2 C1 B8 B3 -38.7(2) . . . . ? B7 C1 B8 B3 -141.5(2) . . . . ? B6 C1 B8 B3 -104.3(2) . . . . ? B12 B7 B8 C1 -135.5(2) . . . . ? B11 B7 B8 C1 -98.0(2) . . . . ? B6 B7 B8 C1 -34.85(18) . . . . ? C1 B7 B8 B12 135.5(2) . . . . ? B11 B7 B8 B12 37.5(2) . . . . ? B6 B7 B8 B12 100.6(2) . . . . ? C1 B7 B8 B9 98.3(2) . . . . ? B12 B7 B8 B9 -37.2(2) . . . . ? B11 B7 B8 B9 0.2(3) . . . . ? B6 B7 B8 B9 63.4(3) . . . . ? C1 B7 B8 B3 34.20(18) . . . . ? B12 B7 B8 B3 -101.3(2) . . . . ? B11 B7 B8 B3 -63.8(3) . . . . ? B6 B7 B8 B3 -0.6(3) . . . . ? C2 B3 B8 C1 36.72(17) . . . . ? B4 B3 B8 C1 98.1(2) . . . . ? B9 B3 B8 C1 135.9(3) . . . . ? C1 B3 B8 B7 -34.20(19) . . . . ? C2 B3 B8 B7 2.5(3) . . . . ? B4 B3 B8 B7 63.9(3) . . . . ? B9 B3 B8 B7 101.7(3) . . . . ? C1 B3 B8 B12 -98.5(3) . . . . ? C2 B3 B8 B12 -61.8(3) . . . . ? B4 B3 B8 B12 -0.4(4) . . . . ? B9 B3 B8 B12 37.4(3) . . . . ? C1 B3 B8 B9 -135.9(3) . . . . ? C2 B3 B8 B9 -99.2(3) . . . . ? B4 B3 B8 B9 -37.8(3) . . . . ? C1 B8 B9 B12 99.8(3) . . . . ? B7 B8 B9 B12 37.5(3) . . . . ? B3 B8 B9 B12 138.3(3) . . . . ? C1 B8 B9 B4 -0.3(4) . . . . ? B7 B8 B9 B4 -62.6(3) . . . . ? B12 B8 B9 B4 -100.2(3) . . . . ? B3 B8 B9 B4 38.2(3) . . . . ? C1 B8 B9 B3 -38.5(2) . . . . ? B7 B8 B9 B3 -100.8(3) . . . . ? B12 B8 B9 B3 -138.3(3) . . . . ? C1 B8 B9 B10 62.5(3) . . . . ? B7 B8 B9 B10 0.2(3) . . . . ? B12 B8 B9 B10 -37.3(3) . . . . ? B3 B8 B9 B10 101.0(3) . . . . ? C2 B4 B9 B12 -62.7(3) . . . . ? B5 B4 B9 B12 -0.2(3) . . . . ? B10 B4 B9 B12 37.1(2) . . . . ? B3 B4 B9 B12 -101.0(3) . . . . ? C2 B4 B9 B8 0.2(4) . . . . ? B5 B4 B9 B8 62.6(3) . . . . ? B10 B4 B9 B8 99.9(3) . . . . ? B3 B4 B9 B8 -38.1(3) . . . . ? C2 B4 B9 B3 38.3(2) . . . . ? B5 B4 B9 B3 100.7(2) . . . . ? B10 B4 B9 B3 138.1(3) . . . . ? C2 B4 B9 B10 -99.8(3) . . . . ? B5 B4 B9 B10 -37.3(2) . . . . ? B3 B4 B9 B10 -138.1(3) . . . . ? C1 B3 B9 B12 0.5(3) . . . . ? C2 B3 B9 B12 62.2(3) . . . . ? B8 B3 B9 B12 -37.1(2) . . . . ? B4 B3 B9 B12 100.1(3) . . . . ? C1 B3 B9 B8 37.6(2) . . . . ? C2 B3 B9 B8 99.2(3) . . . . ? B4 B3 B9 B8 137.2(3) . . . . ? C1 B3 B9 B4 -99.6(3) . . . . ? C2 B3 B9 B4 -38.0(2) . . . . ? B8 B3 B9 B4 -137.2(3) . . . . ? C1 B3 B9 B10 -62.3(3) . . . . ? C2 B3 B9 B10 -0.7(3) . . . . ? B8 B3 B9 B10 -99.9(3) . . . . ? B4 B3 B9 B10 37.3(2) . . . . ? C2 B5 B10 B12 -61.2(3) . . . . ? B4 B5 B10 B12 -99.9(3) . . . . ? B11 B5 B10 B12 38.3(3) . . . . ? B6 B5 B10 B12 1.3(4) . . . . ? C2 B5 B10 B4 38.73(19) . . . . ? B11 B5 B10 B4 138.3(2) . . . . ? B6 B5 B10 B4 101.2(2) . . . . ? C2 B5 B10 B11 -99.5(2) . . . . ? B4 B5 B10 B11 -138.3(2) . . . . ? B6 B5 B10 B11 -37.1(2) . . . . ? C2 B5 B10 B9 1.8(3) . . . . ? B4 B5 B10 B9 -36.9(2) . . . . ? B11 B5 B10 B9 101.3(3) . . . . ? B6 B5 B10 B9 64.3(3) . . . . ? C2 B4 B10 B12 62.7(3) . . . . ? B5 B4 B10 B12 101.3(3) . . . . ? B9 B4 B10 B12 -37.2(3) . . . . ? B3 B4 B10 B12 0.6(4) . . . . ? C2 B4 B10 B5 -38.61(19) . . . . ? B9 B4 B10 B5 -138.5(2) . . . . ? B3 B4 B10 B5 -100.7(2) . . . . ? C2 B4 B10 B11 -1.4(3) . . . . ? B5 B4 B10 B11 37.2(2) . . . . ? B9 B4 B10 B11 -101.3(3) . . . . ? B3 B4 B10 B11 -63.6(3) . . . . ? C2 B4 B10 B9 99.9(2) . . . . ? B5 B4 B10 B9 138.5(2) . . . . ? B3 B4 B10 B9 37.8(3) . . . . ? B8 B9 B10 B12 37.4(2) . . . . ? B4 B9 B10 B12 138.1(3) . . . . ? B3 B9 B10 B12 100.6(3) . . . . ? B12 B9 B10 B5 -101.3(3) . . . . ? B8 B9 B10 B5 -63.9(3) . . . . ? B4 B9 B10 B5 36.8(2) . . . . ? B3 B9 B10 B5 -0.7(3) . . . . ? B12 B9 B10 B4 -138.1(3) . . . . ? B8 B9 B10 B4 -100.7(3) . . . . ? B3 B9 B10 B4 -37.5(2) . . . . ? B12 B9 B10 B11 -38.0(2) . . . . ? B8 B9 B10 B11 -0.6(3) . . . . ? B4 B9 B10 B11 100.1(3) . . . . ? B3 B9 B10 B11 62.6(3) . . . . ? C2 B5 B11 B6 -38.5(2) . . . . ? B4 B5 B11 B6 -101.0(2) . . . . ? B10 B5 B11 B6 -138.7(3) . . . . ? C2 B5 B11 B10 100.2(3) . . . . ? B4 B5 B11 B10 37.7(2) . . . . ? B6 B5 B11 B10 138.7(3) . . . . ? C2 B5 B11 B7 0.1(4) . . . . ? B4 B5 B11 B7 -62.4(3) . . . . ? B10 B5 B11 B7 -100.1(3) . . . . ? B6 B5 B11 B7 38.6(3) . . . . ? C2 B5 B11 B12 62.9(3) . . . . ? B4 B5 B11 B12 0.4(3) . . . . ? B10 B5 B11 B12 -37.3(2) . . . . ? B6 B5 B11 B12 101.4(2) . . . . ? C2 B6 B11 B5 38.1(2) . . . . ? C1 B6 B11 B5 99.1(3) . . . . ? B7 B6 B11 B5 136.9(3) . . . . ? C2 B6 B11 B10 1.2(3) . . . . ? C1 B6 B11 B10 62.2(3) . . . . ? B5 B6 B11 B10 -36.9(2) . . . . ? B7 B6 B11 B10 100.1(3) . . . . ? C2 B6 B11 B7 -98.9(3) . . . . ? C1 B6 B11 B7 -37.8(2) . . . . ? B5 B6 B11 B7 -136.9(3) . . . . ? C2 B6 B11 B12 -61.5(3) . . . . ? C1 B6 B11 B12 -0.4(3) . . . . ? B5 B6 B11 B12 -99.5(3) . . . . ? B7 B6 B11 B12 37.4(2) . . . . ? B12 B10 B11 B5 -137.6(2) . . . . ? B4 B10 B11 B5 -37.0(2) . . . . ? B9 B10 B11 B5 -100.2(3) . . . . ? B12 B10 B11 B6 -100.5(3) . . . . ? B5 B10 B11 B6 37.1(2) . . . . ? B4 B10 B11 B6 0.1(3) . . . . ? B9 B10 B11 B6 -63.1(3) . . . . ? B12 B10 B11 B7 -36.7(2) . . . . ? B5 B10 B11 B7 100.8(2) . . . . ? B4 B10 B11 B7 63.9(3) . . . . ? B9 B10 B11 B7 0.7(3) . . . . ? B5 B10 B11 B12 137.6(2) . . . . ? B4 B10 B11 B12 100.6(3) . . . . ? B9 B10 B11 B12 37.4(2) . . . . ? C1 B7 B11 B5 0.7(4) . . . . ? B8 B7 B11 B5 62.4(3) . . . . ? B12 B7 B11 B5 99.5(3) . . . . ? B6 B7 B11 B5 -38.5(3) . . . . ? C1 B7 B11 B6 39.2(2) . . . . ? B8 B7 B11 B6 100.9(3) . . . . ? B12 B7 B11 B6 138.0(3) . . . . ? C1 B7 B11 B10 -62.2(3) . . . . ? B8 B7 B11 B10 -0.6(3) . . . . ? B12 B7 B11 B10 36.5(2) . . . . ? B6 B7 B11 B10 -101.4(3) . . . . ? C1 B7 B11 B12 -98.8(3) . . . . ? B8 B7 B11 B12 -37.1(3) . . . . ? B6 B7 B11 B12 -138.0(3) . . . . ? C1 B8 B12 B10 -61.4(3) . . . . ? B7 B8 B12 B10 -100.3(3) . . . . ? B9 B8 B12 B10 38.3(3) . . . . ? B3 B8 B12 B10 0.8(4) . . . . ? C1 B8 B12 B9 -99.8(3) . . . . ? B7 B8 B12 B9 -138.6(3) . . . . ? B3 B8 B12 B9 -37.5(3) . . . . ? C1 B8 B12 B7 38.8(2) . . . . ? B9 B8 B12 B7 138.6(3) . . . . ? B3 B8 B12 B7 101.1(3) . . . . ? C1 B8 B12 B11 1.9(3) . . . . ? B7 B8 B12 B11 -36.9(2) . . . . ? B9 B8 B12 B11 101.7(3) . . . . ? B3 B8 B12 B11 64.2(3) . . . . ? B5 B10 B12 B8 62.0(4) . . . . ? B4 B10 B12 B8 -0.8(4) . . . . ? B11 B10 B12 B8 99.9(3) . . . . ? B9 B10 B12 B8 -38.1(3) . . . . ? B5 B10 B12 B9 100.1(3) . . . . ? B4 B10 B12 B9 37.3(3) . . . . ? B11 B10 B12 B9 138.0(3) . . . . ? B5 B10 B12 B7 -1.0(4) . . . . ? B4 B10 B12 B7 -63.8(4) . . . . ? B11 B10 B12 B7 36.9(3) . . . . ? B9 B10 B12 B7 -101.1(3) . . . . ? B5 B10 B12 B11 -37.9(2) . . . . ? B4 B10 B12 B11 -100.7(3) . . . . ? B9 B10 B12 B11 -138.0(3) . . . . ? B4 B9 B12 B8 100.6(3) . . . . ? B3 B9 B12 B8 37.2(2) . . . . ? B10 B9 B12 B8 137.7(3) . . . . ? B8 B9 B12 B10 -137.7(3) . . . . ? B4 B9 B12 B10 -37.2(2) . . . . ? B3 B9 B12 B10 -100.5(3) . . . . ? B8 B9 B12 B7 -36.8(2) . . . . ? B4 B9 B12 B7 63.8(3) . . . . ? B3 B9 B12 B7 0.4(3) . . . . ? B10 B9 B12 B7 100.9(3) . . . . ? B8 B9 B12 B11 -100.1(3) . . . . ? B4 B9 B12 B11 0.5(3) . . . . ? B3 B9 B12 B11 -62.9(3) . . . . ? B10 B9 B12 B11 37.6(2) . . . . ? C1 B7 B12 B8 -38.4(2) . . . . ? B11 B7 B12 B8 -138.5(3) . . . . ? B6 B7 B12 B8 -101.1(3) . . . . ? C1 B7 B12 B10 63.2(3) . . . . ? B8 B7 B12 B10 101.5(3) . . . . ? B11 B7 B12 B10 -37.0(3) . . . . ? B6 B7 B12 B10 0.4(4) . . . . ? C1 B7 B12 B9 -1.2(3) . . . . ? B8 B7 B12 B9 37.2(2) . . . . ? B11 B7 B12 B9 -101.3(3) . . . . ? B6 B7 B12 B9 -63.9(3) . . . . ? C1 B7 B12 B11 100.1(2) . . . . ? B8 B7 B12 B11 138.5(3) . . . . ? B6 B7 B12 B11 37.4(2) . . . . ? B5 B11 B12 B8 -64.3(3) . . . . ? B6 B11 B12 B8 -0.9(3) . . . . ? B10 B11 B12 B8 -101.8(3) . . . . ? B7 B11 B12 B8 36.8(2) . . . . ? B5 B11 B12 B10 37.5(2) . . . . ? B6 B11 B12 B10 100.9(3) . . . . ? B7 B11 B12 B10 138.6(3) . . . . ? B5 B11 B12 B9 -0.5(3) . . . . ? B6 B11 B12 B9 62.9(3) . . . . ? B10 B11 B12 B9 -38.0(2) . . . . ? B7 B11 B12 B9 100.6(2) . . . . ? B5 B11 B12 B7 -101.1(2) . . . . ? B6 B11 B12 B7 -37.7(2) . . . . ? B10 B11 B12 B7 -138.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.270 _refine_diff_density_min -0.265 _refine_diff_density_rms 0.051 _database_code_depnum_ccdc_archive 'CCDC 963127' ####################################################################### # # 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_ip228 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H70 B10 N6 Sn2' _chemical_formula_weight 872.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 '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' _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 10.334(2) _cell_length_b 12.194(2) _cell_length_c 19.991(4) _cell_angle_alpha 104.60(3) _cell_angle_beta 90.89(3) _cell_angle_gamma 108.06(3) _cell_volume 2305.5(8) _cell_formula_units_Z 2 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 21624 _cell_measurement_theta_min 2.08 _cell_measurement_theta_max 29.53 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 1.111 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(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 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22414 _diffrn_reflns_av_R_equivalents 0.0510 _diffrn_reflns_av_sigmaI/netI 0.0884 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 28.28 _reflns_number_total 11312 _reflns_number_gt 7704 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. 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 _platon_squeeze_void_content 1 0.500 1.000 1.000 205 46 ' ' _platon_squeeze_details A molecule of bezene was removed with SQUEEZE. ; _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^)+(0.0234P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11312 _refine_ls_number_parameters 482 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0850 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.0706 _refine_ls_wR_factor_gt 0.0642 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.05000(3) 1.25856(2) 0.209672(13) 0.02072(7) Uani 1 1 d . . . Sn2 Sn 0.11772(3) 1.10840(2) 0.293094(12) 0.01590(6) Uani 1 1 d . . . N1 N 0.2291(3) 1.2927(2) 0.15830(14) 0.0206(6) Uani 1 1 d . . . N2 N 0.4443(3) 1.4099(3) 0.14422(16) 0.0272(7) Uani 1 1 d . . . N3 N 0.0390(3) 0.9196(2) 0.24562(15) 0.0212(6) Uani 1 1 d . . . N4 N 0.2592(3) 1.0070(2) 0.24110(14) 0.0174(6) Uani 1 1 d . . . N5 N -0.0287(3) 1.1166(2) 0.37840(15) 0.0199(6) Uani 1 1 d . . . N6 N 0.1867(3) 1.1294(2) 0.39901(14) 0.0188(6) Uani 1 1 d . . . C1 C 0.3296(4) 1.4779(3) 0.24936(18) 0.0187(7) Uani 1 1 d . . . C2 C 0.1831(4) 1.4267(3) 0.28284(18) 0.0186(7) Uani 1 1 d . . . C3 C 0.3437(4) 1.3936(3) 0.18029(17) 0.0204(7) Uani 1 1 d . . . C4 C 0.2313(4) 1.2128(3) 0.08942(18) 0.0245(8) Uani 1 1 d . . . H4 H 0.3272 1.2118 0.0846 0.029 Uiso 1 1 calc R . . C5 C 0.1891(6) 1.2600(4) 0.0314(2) 0.0449(12) Uani 1 1 d . . . H5A H 0.2504 1.3416 0.0360 0.067 Uiso 1 1 calc R . . H5B H 0.0949 1.2606 0.0348 0.067 Uiso 1 1 calc R . . H5C H 0.1952 1.2079 -0.0138 0.067 Uiso 1 1 calc R . . C6 C 0.1393(5) 1.0854(3) 0.0834(2) 0.0337(10) Uani 1 1 d . . . H6A H 0.1690 1.0569 0.1207 0.051 Uiso 1 1 calc R . . H6B H 0.1452 1.0330 0.0383 0.051 Uiso 1 1 calc R . . H6C H 0.0445 1.0842 0.0874 0.051 Uiso 1 1 calc R . . C7 C 0.5739(4) 1.5076(3) 0.1594(2) 0.0296(9) Uani 1 1 d . . . H7 H 0.5709 1.5708 0.2018 0.036 Uiso 1 1 calc R . . C8 C 0.6856(5) 1.4583(4) 0.1716(3) 0.0518(13) Uani 1 1 d . . . H8A H 0.6698 1.4258 0.2120 0.078 Uiso 1 1 calc R . . H8B H 0.7741 1.5223 0.1803 0.078 Uiso 1 1 calc R . . H8C H 0.6860 1.3944 0.1306 0.078 Uiso 1 1 calc R . . C9 C 0.5948(5) 1.5595(4) 0.0970(2) 0.0454(12) Uani 1 1 d . . . H9A H 0.5200 1.5902 0.0899 0.068 Uiso 1 1 calc R . . H9B H 0.5959 1.4968 0.0554 0.068 Uiso 1 1 calc R . . H9C H 0.6821 1.6250 0.1055 0.068 Uiso 1 1 calc R . . C10 C 0.1544(4) 0.9073(3) 0.22057(18) 0.0192(7) Uani 1 1 d . . . C11 C 0.1593(4) 0.7919(3) 0.17282(18) 0.0227(8) Uani 1 1 d . . . H11A H 0.1010 0.7241 0.1889 0.027 Uiso 1 1 calc R . . H11B H 0.2543 0.7902 0.1758 0.027 Uiso 1 1 calc R . . C12 C 0.1115(5) 0.7742(3) 0.09703(19) 0.0357(10) Uani 1 1 d . . . H12A H 0.0226 0.7886 0.0946 0.043 Uiso 1 1 calc R . . H12B H 0.1785 0.8336 0.0783 0.043 Uiso 1 1 calc R . . C13 C 0.0956(6) 0.6484(4) 0.0522(2) 0.0490(13) Uani 1 1 d . . . H13A H 0.0245 0.5897 0.0696 0.059 Uiso 1 1 calc R . . H13B H 0.0629 0.6415 0.0040 0.059 Uiso 1 1 calc R . . C14 C 0.2243(6) 0.6162(4) 0.0509(3) 0.0520(13) Uani 1 1 d . . . H14A H 0.2057 0.5340 0.0220 0.078 Uiso 1 1 calc R . . H14B H 0.2574 0.6221 0.0983 0.078 Uiso 1 1 calc R . . H14C H 0.2942 0.6714 0.0317 0.078 Uiso 1 1 calc R . . C15 C -0.0925(4) 0.8251(3) 0.23549(19) 0.0233(8) Uani 1 1 d . . . H15 H -0.0884 0.7550 0.1978 0.028 Uiso 1 1 calc R . . C16 C -0.2038(4) 0.8686(3) 0.2121(2) 0.0337(10) Uani 1 1 d . . . H16A H -0.1813 0.8934 0.1696 0.051 Uiso 1 1 calc R . . H16B H -0.2103 0.9368 0.2487 0.051 Uiso 1 1 calc R . . H16C H -0.2916 0.8036 0.2030 0.051 Uiso 1 1 calc R . . C17 C -0.1196(5) 0.7859(4) 0.3015(2) 0.0378(10) Uani 1 1 d . . . H17A H -0.0452 0.7588 0.3144 0.057 Uiso 1 1 calc R . . H17B H -0.2064 0.7201 0.2938 0.057 Uiso 1 1 calc R . . H17C H -0.1246 0.8535 0.3390 0.057 Uiso 1 1 calc R . . C18 C 0.3900(4) 1.0215(3) 0.21069(18) 0.0192(7) Uani 1 1 d . . . H18 H 0.3707 0.9746 0.1607 0.023 Uiso 1 1 calc R . . C19 C 0.4592(4) 1.1534(3) 0.2143(2) 0.0265(8) Uani 1 1 d . . . H19A H 0.3975 1.1817 0.1906 0.040 Uiso 1 1 calc R . . H19B H 0.5438 1.1627 0.1917 0.040 Uiso 1 1 calc R . . H19C H 0.4806 1.2005 0.2631 0.040 Uiso 1 1 calc R . . C20 C 0.4839(4) 0.9758(3) 0.2469(2) 0.0282(9) Uani 1 1 d . . . H20A H 0.4381 0.8912 0.2443 0.042 Uiso 1 1 calc R . . H20B H 0.5059 1.0224 0.2957 0.042 Uiso 1 1 calc R . . H20C H 0.5684 0.9841 0.2242 0.042 Uiso 1 1 calc R . . C21 C 0.0719(4) 1.1367(3) 0.42628(18) 0.0190(7) Uani 1 1 d . . . C22 C 0.0573(4) 1.1673(3) 0.50297(17) 0.0227(8) Uani 1 1 d . . . H22A H 0.1203 1.1390 0.5267 0.027 Uiso 1 1 calc R . . H22B H -0.0372 1.1240 0.5105 0.027 Uiso 1 1 calc R . . C23 C 0.0880(4) 1.3026(3) 0.53623(19) 0.0255(8) Uani 1 1 d . . . H23A H 0.0395 1.3342 0.5064 0.031 Uiso 1 1 calc R . . H23B H 0.0508 1.3138 0.5819 0.031 Uiso 1 1 calc R . . C24 C 0.2381(4) 1.3754(3) 0.5466(2) 0.0295(9) Uani 1 1 d . . . H24A H 0.2757 1.3669 0.5011 0.035 Uiso 1 1 calc R . . H24B H 0.2878 1.3440 0.5760 0.035 Uiso 1 1 calc R . . C25 C 0.2610(5) 1.5075(3) 0.5810(2) 0.0396(11) Uani 1 1 d . . . H25A H 0.3593 1.5519 0.5874 0.059 Uiso 1 1 calc R . . H25B H 0.2245 1.5161 0.6263 0.059 Uiso 1 1 calc R . . H25C H 0.2141 1.5393 0.5514 0.059 Uiso 1 1 calc R . . C26 C -0.1555(4) 1.1420(3) 0.39546(19) 0.0238(8) Uani 1 1 d . . . H26 H -0.1385 1.1983 0.4431 0.029 Uiso 1 1 calc R . . C27 C -0.1934(4) 1.2036(3) 0.3450(2) 0.0273(8) Uani 1 1 d . . . H27A H -0.1173 1.2761 0.3460 0.041 Uiso 1 1 calc R . . H27B H -0.2749 1.2253 0.3583 0.041 Uiso 1 1 calc R . . H27C H -0.2125 1.1492 0.2980 0.041 Uiso 1 1 calc R . . C28 C -0.2704(4) 1.0280(3) 0.3961(2) 0.0277(8) Uani 1 1 d . . . H28A H -0.2421 0.9906 0.4292 0.042 Uiso 1 1 calc R . . H28B H -0.2902 0.9721 0.3495 0.042 Uiso 1 1 calc R . . H28C H -0.3526 1.0480 0.4099 0.042 Uiso 1 1 calc R . . C29 C 0.3075(3) 1.1258(3) 0.43694(17) 0.0188(7) Uani 1 1 d . . . H29 H 0.2990 1.1522 0.4878 0.023 Uiso 1 1 calc R . . C30 C 0.3125(4) 0.9977(3) 0.4200(2) 0.0274(8) Uani 1 1 d . . . H30A H 0.2277 0.9448 0.4311 0.041 Uiso 1 1 calc R . . H30B H 0.3906 0.9959 0.4477 0.041 Uiso 1 1 calc R . . H30C H 0.3226 0.9703 0.3705 0.041 Uiso 1 1 calc R . . C31 C 0.4369(4) 1.2115(3) 0.4215(2) 0.0256(8) Uani 1 1 d . . . H31A H 0.4304 1.2925 0.4330 0.038 Uiso 1 1 calc R . . H31B H 0.4487 1.1863 0.3720 0.038 Uiso 1 1 calc R . . H31C H 0.5155 1.2111 0.4494 0.038 Uiso 1 1 calc R . . B3 B 0.2038(5) 1.5422(3) 0.2458(2) 0.0243(9) Uani 1 1 d . . . H31 H 0.149(4) 1.522(3) 0.198(2) 0.023(10) Uiso 1 1 d . . . B4 B 0.3795(5) 1.6310(3) 0.2670(2) 0.0245(9) Uani 1 1 d . . . H41 H 0.431(4) 1.674(3) 0.2306(19) 0.020(9) Uiso 1 1 d . . . B5 B 0.4592(4) 1.5590(3) 0.3141(2) 0.0225(9) Uani 1 1 d . . . H51 H 0.560(4) 1.554(3) 0.3058(19) 0.022(10) Uiso 1 1 d . . . B6 B 0.3324(4) 1.4278(3) 0.3218(2) 0.0178(8) Uani 1 1 d . . . H61 H 0.351(4) 1.345(3) 0.3147(18) 0.017(9) Uiso 1 1 d . . . B7 B 0.2528(5) 1.6738(4) 0.3161(2) 0.0281(10) Uani 1 1 d . . . H71 H 0.225(4) 1.743(3) 0.3121(19) 0.022(10) Uiso 1 1 d . . . B8 B 0.4110(5) 1.6845(4) 0.3588(2) 0.0274(10) Uani 1 1 d . . . H81 H 0.485(5) 1.766(4) 0.384(2) 0.040(12) Uiso 1 1 d . . . B9 B 0.3827(5) 1.5580(4) 0.3931(2) 0.0228(9) Uani 1 1 d . . . H91 H 0.431(4) 1.556(3) 0.4360(18) 0.013(9) Uiso 1 1 d . . . B10 B 0.2066(4) 1.4705(4) 0.3713(2) 0.0221(8) Uani 1 1 d . . . H101 H 0.142(4) 1.414(3) 0.3986(18) 0.018(9) Uiso 1 1 d . . . B11 B 0.1278(5) 1.5421(3) 0.3243(2) 0.0247(9) Uani 1 1 d . . . H111 H 0.014(4) 1.524(3) 0.3215(19) 0.024(10) Uiso 1 1 d . . . B12 B 0.2560(5) 1.6292(4) 0.3943(2) 0.0287(10) Uani 1 1 d . . . H121 H 0.234(4) 1.676(4) 0.440(2) 0.041(12) Uiso 1 1 d . . . 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 Sn1 0.01944(16) 0.01839(13) 0.02299(15) 0.00360(11) -0.00325(12) 0.00612(12) Sn2 0.01522(14) 0.01380(12) 0.01758(13) 0.00276(10) 0.00126(11) 0.00436(10) N1 0.0273(17) 0.0168(13) 0.0161(14) 0.0027(11) 0.0001(12) 0.0065(12) N2 0.0301(18) 0.0207(14) 0.0263(17) 0.0033(13) 0.0085(14) 0.0044(13) N3 0.0214(16) 0.0165(13) 0.0223(15) 0.0007(11) 0.0006(12) 0.0053(12) N4 0.0187(15) 0.0158(13) 0.0172(14) 0.0021(11) 0.0002(11) 0.0068(11) N5 0.0138(15) 0.0227(14) 0.0206(15) 0.0022(12) 0.0018(12) 0.0051(12) N6 0.0150(15) 0.0207(14) 0.0195(14) 0.0032(11) 0.0003(12) 0.0060(12) C1 0.0191(18) 0.0157(15) 0.0196(17) 0.0045(13) 0.0008(14) 0.0034(14) C2 0.0179(18) 0.0161(15) 0.0215(17) 0.0051(13) 0.0014(14) 0.0048(14) C3 0.028(2) 0.0157(15) 0.0175(16) 0.0053(13) 0.0009(15) 0.0067(14) C4 0.032(2) 0.0196(16) 0.0197(18) 0.0026(14) -0.0002(16) 0.0081(16) C5 0.074(4) 0.044(2) 0.021(2) 0.0059(18) -0.005(2) 0.027(2) C6 0.043(3) 0.0217(18) 0.027(2) -0.0025(15) -0.0027(18) 0.0051(18) C7 0.033(2) 0.0244(18) 0.027(2) 0.0051(15) 0.0133(17) 0.0032(17) C8 0.035(3) 0.036(2) 0.076(4) 0.008(2) 0.007(3) 0.006(2) C9 0.052(3) 0.039(2) 0.034(2) 0.0088(19) 0.016(2) -0.001(2) C10 0.0215(19) 0.0210(16) 0.0178(16) 0.0069(13) -0.0019(14) 0.0093(14) C11 0.027(2) 0.0189(16) 0.0207(18) 0.0012(13) -0.0026(15) 0.0093(15) C12 0.057(3) 0.030(2) 0.0233(19) -0.0017(16) -0.0058(19) 0.025(2) C13 0.072(4) 0.035(2) 0.034(2) -0.0112(19) -0.010(2) 0.026(2) C14 0.073(4) 0.041(3) 0.046(3) 0.002(2) 0.016(3) 0.031(3) C15 0.0215(19) 0.0166(16) 0.028(2) 0.0020(15) -0.0020(17) 0.0044(14) C16 0.021(2) 0.0280(19) 0.044(2) 0.0010(18) -0.0086(18) 0.0036(17) C17 0.036(3) 0.031(2) 0.048(3) 0.0198(19) 0.013(2) 0.0063(19) C18 0.0171(18) 0.0244(17) 0.0177(17) 0.0047(14) 0.0024(14) 0.0098(14) C19 0.022(2) 0.0306(19) 0.030(2) 0.0113(16) 0.0062(16) 0.0099(16) C20 0.022(2) 0.0293(19) 0.037(2) 0.0074(17) 0.0026(17) 0.0148(16) C21 0.0189(18) 0.0130(14) 0.0224(17) 0.0015(13) 0.0019(14) 0.0037(13) C22 0.0228(19) 0.0250(17) 0.0184(17) 0.0022(14) 0.0040(15) 0.0078(15) C23 0.026(2) 0.0278(18) 0.0214(18) 0.0028(15) 0.0039(15) 0.0097(16) C24 0.028(2) 0.0282(19) 0.029(2) 0.0045(16) 0.0044(17) 0.0074(17) C25 0.037(3) 0.027(2) 0.047(3) 0.0009(18) 0.007(2) 0.0061(18) C26 0.0158(18) 0.0287(18) 0.0245(18) 0.0023(15) 0.0032(15) 0.0078(15) C27 0.0190(19) 0.0256(18) 0.042(2) 0.0131(17) 0.0044(17) 0.0109(15) C28 0.0173(19) 0.037(2) 0.034(2) 0.0167(17) 0.0065(16) 0.0105(16) C29 0.0146(17) 0.0263(17) 0.0157(16) 0.0048(13) 0.0000(13) 0.0075(14) C30 0.031(2) 0.0245(18) 0.030(2) 0.0091(15) 0.0067(17) 0.0119(16) C31 0.0195(19) 0.0252(18) 0.0264(19) 0.0018(15) -0.0016(15) 0.0036(15) B3 0.031(3) 0.0178(19) 0.026(2) 0.0075(16) 0.0029(19) 0.0095(18) B4 0.035(3) 0.0128(17) 0.024(2) 0.0063(15) 0.0034(19) 0.0051(17) B5 0.019(2) 0.0184(18) 0.024(2) 0.0031(16) 0.0018(17) 0.0005(17) B6 0.016(2) 0.0178(18) 0.0181(19) 0.0061(15) -0.0004(15) 0.0021(15) B7 0.034(3) 0.0164(19) 0.032(2) 0.0022(17) 0.004(2) 0.0090(19) B8 0.034(3) 0.0181(18) 0.024(2) -0.0002(16) 0.0062(19) 0.0050(18) B9 0.023(2) 0.0222(19) 0.0177(19) 0.0021(15) -0.0008(17) 0.0021(17) B10 0.023(2) 0.0235(19) 0.0198(19) 0.0030(16) 0.0039(16) 0.0091(17) B11 0.027(2) 0.0201(19) 0.027(2) 0.0011(16) 0.0035(18) 0.0119(17) B12 0.035(3) 0.022(2) 0.023(2) -0.0022(17) 0.0018(19) 0.0077(19) _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 Sn1 N1 2.110(3) . ? Sn1 C2 2.216(3) . ? Sn1 Sn2 2.9869(8) . ? Sn2 N3 2.139(3) . ? Sn2 N6 2.150(3) . ? Sn2 N4 2.295(3) . ? Sn2 N5 2.302(3) . ? Sn2 C10 2.657(3) . ? Sn2 C21 2.667(4) . ? N1 C3 1.384(4) . ? N1 C4 1.478(4) . ? N2 C3 1.268(5) . ? N2 C7 1.457(5) . ? N3 C10 1.337(5) . ? N3 C15 1.455(5) . ? N4 C10 1.318(4) . ? N4 C18 1.469(4) . ? N5 C21 1.323(4) . ? N5 C26 1.463(5) . ? N6 C21 1.332(4) . ? N6 C29 1.468(4) . ? C1 C3 1.539(5) . ? C1 C2 1.669(5) . ? C1 B5 1.710(5) . ? C1 B6 1.712(5) . ? C1 B4 1.715(5) . ? C1 B3 1.723(6) . ? C2 B10 1.704(5) . ? C2 B11 1.708(5) . ? C2 B3 1.709(5) . ? C2 B6 1.714(5) . ? C4 C6 1.523(5) . ? C4 C5 1.530(5) . ? C4 H4 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.500(6) . ? C7 C9 1.526(6) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.505(5) . ? C11 C12 1.527(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.526(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.499(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.515(6) . ? C15 C16 1.519(5) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C20 1.515(5) . ? C18 C19 1.526(5) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.505(5) . ? C22 C23 1.543(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.510(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.524(5) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.513(5) . ? C26 C28 1.526(5) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C31 1.511(5) . ? C29 C30 1.531(5) . ? C29 H29 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? B3 B11 1.766(6) . ? B3 B7 1.773(6) . ? B3 B4 1.782(7) . ? B3 H31 1.04(4) . ? B4 B8 1.773(6) . ? B4 B7 1.777(7) . ? B4 B5 1.781(6) . ? B4 H41 1.06(4) . ? B5 B6 1.770(5) . ? B5 B9 1.779(6) . ? B5 B8 1.784(6) . ? B5 H51 1.07(4) . ? B6 B10 1.773(6) . ? B6 B9 1.774(5) . ? B6 H61 1.06(4) . ? B7 B11 1.768(6) . ? B7 B12 1.783(7) . ? B7 B8 1.786(7) . ? B7 H71 0.99(4) . ? B8 B12 1.770(7) . ? B8 B9 1.788(6) . ? B8 H81 1.05(4) . ? B9 B12 1.778(7) . ? B9 B10 1.783(6) . ? B9 H91 0.99(3) . ? B10 B11 1.772(6) . ? B10 B12 1.774(6) . ? B10 H101 1.07(4) . ? B11 B12 1.779(6) . ? B11 H111 1.13(4) . ? B12 H121 1.01(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Sn1 C2 78.90(12) . . ? N1 Sn1 Sn2 98.28(8) . . ? C2 Sn1 Sn2 92.21(9) . . ? N3 Sn2 N6 106.13(11) . . ? N3 Sn2 N4 59.60(11) . . ? N6 Sn2 N4 97.29(11) . . ? N3 Sn2 N5 97.70(11) . . ? N6 Sn2 N5 59.35(11) . . ? N4 Sn2 N5 143.39(10) . . ? N3 Sn2 C10 29.97(11) . . ? N6 Sn2 C10 105.31(11) . . ? N4 Sn2 C10 29.74(10) . . ? N5 Sn2 C10 123.87(11) . . ? N3 Sn2 C21 105.58(11) . . ? N6 Sn2 C21 29.71(11) . . ? N4 Sn2 C21 123.43(10) . . ? N5 Sn2 C21 29.75(10) . . ? C10 Sn2 C21 119.98(10) . . ? N3 Sn2 Sn1 114.62(8) . . ? N6 Sn2 Sn1 137.56(8) . . ? N4 Sn2 Sn1 112.89(7) . . ? N5 Sn2 Sn1 102.49(8) . . ? C10 Sn2 Sn1 115.78(7) . . ? C21 Sn2 Sn1 121.84(8) . . ? C3 N1 C4 115.1(3) . . ? C3 N1 Sn1 124.9(2) . . ? C4 N1 Sn1 119.6(2) . . ? C3 N2 C7 128.7(3) . . ? C10 N3 C15 126.0(3) . . ? C10 N3 Sn2 97.0(2) . . ? C15 N3 Sn2 136.9(2) . . ? C10 N4 C18 122.2(3) . . ? C10 N4 Sn2 90.5(2) . . ? C18 N4 Sn2 143.7(2) . . ? C21 N5 C26 122.6(3) . . ? C21 N5 Sn2 90.6(2) . . ? C26 N5 Sn2 142.8(2) . . ? C21 N6 C29 125.3(3) . . ? C21 N6 Sn2 97.1(2) . . ? C29 N6 Sn2 137.3(2) . . ? C3 C1 C2 113.8(3) . . ? C3 C1 B5 125.3(3) . . ? C2 C1 B5 110.6(3) . . ? C3 C1 B6 116.4(3) . . ? C2 C1 B6 60.9(2) . . ? B5 C1 B6 62.3(2) . . ? C3 C1 B4 124.6(3) . . ? C2 C1 B4 110.2(3) . . ? B5 C1 B4 62.7(2) . . ? B6 C1 B4 113.6(3) . . ? C3 C1 B3 115.0(3) . . ? C2 C1 B3 60.5(2) . . ? B5 C1 B3 113.9(3) . . ? B6 C1 B3 112.8(3) . . ? B4 C1 B3 62.4(2) . . ? C1 C2 B10 110.8(3) . . ? C1 C2 B11 110.7(3) . . ? B10 C2 B11 62.6(2) . . ? C1 C2 B3 61.3(2) . . ? B10 C2 B3 113.9(3) . . ? B11 C2 B3 62.2(2) . . ? C1 C2 B6 60.8(2) . . ? B10 C2 B6 62.5(2) . . ? B11 C2 B6 113.8(3) . . ? B3 C2 B6 113.4(3) . . ? C1 C2 Sn1 109.7(2) . . ? B10 C2 Sn1 131.0(2) . . ? B11 C2 Sn1 124.1(2) . . ? B3 C2 Sn1 109.1(2) . . ? B6 C2 Sn1 119.0(2) . . ? N2 C3 N1 120.7(3) . . ? N2 C3 C1 126.9(3) . . ? N1 C3 C1 112.4(3) . . ? N1 C4 C6 110.6(3) . . ? N1 C4 C5 110.6(3) . . ? C6 C4 C5 111.0(3) . . ? N1 C4 H4 108.2 . . ? C6 C4 H4 108.2 . . ? C5 C4 H4 108.2 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 108.4(3) . . ? N2 C7 C9 107.6(3) . . ? C8 C7 C9 111.3(4) . . ? N2 C7 H7 109.8 . . ? C8 C7 H7 109.8 . . ? C9 C7 H7 109.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N4 C10 N3 112.5(3) . . ? N4 C10 C11 125.1(3) . . ? N3 C10 C11 122.4(3) . . ? N4 C10 Sn2 59.76(18) . . ? N3 C10 Sn2 53.05(16) . . ? C11 C10 Sn2 172.3(2) . . ? C10 C11 C12 113.5(3) . . ? C10 C11 H11A 108.9 . . ? C12 C11 H11A 108.9 . . ? C10 C11 H11B 108.9 . . ? C12 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? C13 C12 C11 112.2(3) . . ? C13 C12 H12A 109.2 . . ? C11 C12 H12A 109.2 . . ? C13 C12 H12B 109.2 . . ? C11 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C14 C13 C12 114.2(4) . . ? C14 C13 H13A 108.7 . . ? C12 C13 H13A 108.7 . . ? C14 C13 H13B 108.7 . . ? C12 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 C17 109.8(3) . . ? N3 C15 C16 109.5(3) . . ? C17 C15 C16 112.6(4) . . ? N3 C15 H15 108.3 . . ? C17 C15 H15 108.3 . . ? C16 C15 H15 108.3 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N4 C18 C20 111.8(3) . . ? N4 C18 C19 109.3(3) . . ? C20 C18 C19 110.3(3) . . ? N4 C18 H18 108.4 . . ? C20 C18 H18 108.4 . . ? C19 C18 H18 108.4 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N5 C21 N6 112.5(3) . . ? N5 C21 C22 123.0(3) . . ? N6 C21 C22 124.4(3) . . ? N5 C21 Sn2 59.66(18) . . ? N6 C21 Sn2 53.14(17) . . ? C22 C21 Sn2 173.3(2) . . ? C21 C22 C23 113.4(3) . . ? C21 C22 H22A 108.9 . . ? C23 C22 H22A 108.9 . . ? C21 C22 H22B 108.9 . . ? C23 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? C24 C23 C22 114.4(3) . . ? C24 C23 H23A 108.7 . . ? C22 C23 H23A 108.7 . . ? C24 C23 H23B 108.7 . . ? C22 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? C23 C24 C25 111.5(3) . . ? C23 C24 H24A 109.3 . . ? C25 C24 H24A 109.3 . . ? C23 C24 H24B 109.3 . . ? C25 C24 H24B 109.3 . . ? H24A C24 H24B 108.0 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N5 C26 C27 109.5(3) . . ? N5 C26 C28 111.1(3) . . ? C27 C26 C28 111.8(3) . . ? N5 C26 H26 108.1 . . ? C27 C26 H26 108.1 . . ? C28 C26 H26 108.1 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N6 C29 C31 110.9(3) . . ? N6 C29 C30 110.4(3) . . ? C31 C29 C30 111.6(3) . . ? N6 C29 H29 107.9 . . ? C31 C29 H29 107.9 . . ? C30 C29 H29 107.9 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C2 B3 C1 58.2(2) . . ? C2 B3 B11 58.8(2) . . ? C1 B3 B11 105.6(3) . . ? C2 B3 B7 105.3(3) . . ? C1 B3 B7 105.3(3) . . ? B11 B3 B7 60.0(3) . . ? C2 B3 B4 105.3(3) . . ? C1 B3 B4 58.6(2) . . ? B11 B3 B4 107.9(3) . . ? B7 B3 B4 60.0(3) . . ? C2 B3 H31 117(2) . . ? C1 B3 H31 117(2) . . ? B11 B3 H31 124(2) . . ? B7 B3 H31 131(2) . . ? B4 B3 H31 125(2) . . ? C1 B4 B8 105.3(3) . . ? C1 B4 B7 105.4(3) . . ? B8 B4 B7 60.4(3) . . ? C1 B4 B5 58.5(2) . . ? B8 B4 B5 60.3(2) . . ? B7 B4 B5 108.5(3) . . ? C1 B4 B3 59.0(2) . . ? B8 B4 B3 108.0(3) . . ? B7 B4 B3 59.8(3) . . ? B5 B4 B3 107.8(3) . . ? C1 B4 H41 119.9(19) . . ? B8 B4 H41 126.5(19) . . ? B7 B4 H41 124(2) . . ? B5 B4 H41 121(2) . . ? B3 B4 H41 119(2) . . ? C1 B5 B6 58.9(2) . . ? C1 B5 B9 105.5(3) . . ? B6 B5 B9 60.0(2) . . ? C1 B5 B4 58.8(2) . . ? B6 B5 B4 107.6(3) . . ? B9 B5 B4 108.0(3) . . ? C1 B5 B8 105.0(3) . . ? B6 B5 B8 107.7(3) . . ? B9 B5 B8 60.2(2) . . ? B4 B5 B8 59.6(2) . . ? C1 B5 H51 118.2(19) . . ? B6 B5 H51 117.1(19) . . ? B9 B5 H51 125(2) . . ? B4 B5 H51 122(2) . . ? B8 B5 H51 128.9(19) . . ? C1 B6 C2 58.3(2) . . ? C1 B6 B5 58.8(2) . . ? C2 B6 B5 105.8(3) . . ? C1 B6 B10 105.6(3) . . ? C2 B6 B10 58.5(2) . . ? B5 B6 B10 108.4(3) . . ? C1 B6 B9 105.7(3) . . ? C2 B6 B9 105.5(3) . . ? B5 B6 B9 60.3(2) . . ? B10 B6 B9 60.3(2) . . ? C1 B6 H61 116.3(19) . . ? C2 B6 H61 118(2) . . ? B5 B6 H61 123(2) . . ? B10 B6 H61 125(2) . . ? B9 B6 H61 131(2) . . ? B11 B7 B3 59.8(2) . . ? B11 B7 B4 107.9(3) . . ? B3 B7 B4 60.2(3) . . ? B11 B7 B12 60.1(3) . . ? B3 B7 B12 107.6(3) . . ? B4 B7 B12 107.2(3) . . ? B11 B7 B8 107.7(3) . . ? B3 B7 B8 107.8(3) . . ? B4 B7 B8 59.7(3) . . ? B12 B7 B8 59.5(3) . . ? B11 B7 H71 120(2) . . ? B3 B7 H71 119(2) . . ? B4 B7 H71 122(2) . . ? B12 B7 H71 124(2) . . ? B8 B7 H71 125(2) . . ? B12 B8 B4 108.0(3) . . ? B12 B8 B5 107.8(3) . . ? B4 B8 B5 60.1(2) . . ? B12 B8 B7 60.2(3) . . ? B4 B8 B7 59.9(3) . . ? B5 B8 B7 108.0(3) . . ? B12 B8 B9 60.0(3) . . ? B4 B8 B9 108.0(3) . . ? B5 B8 B9 59.8(2) . . ? B7 B8 B9 108.2(3) . . ? B12 B8 H81 121(2) . . ? B4 B8 H81 123(2) . . ? B5 B8 H81 121(2) . . ? B7 B8 H81 123(2) . . ? B9 B8 H81 120(2) . . ? B6 B9 B12 107.4(3) . . ? B6 B9 B5 59.8(2) . . ? B12 B9 B5 107.6(3) . . ? B6 B9 B10 59.8(2) . . ? B12 B9 B10 59.8(2) . . ? B5 B9 B10 107.6(3) . . ? B6 B9 B8 107.4(3) . . ? B12 B9 B8 59.5(3) . . ? B5 B9 B8 60.0(2) . . ? B10 B9 B8 107.2(3) . . ? B6 B9 H91 118.8(19) . . ? B12 B9 H91 123(2) . . ? B5 B9 H91 123(2) . . ? B10 B9 H91 118(2) . . ? B8 B9 H91 126.3(19) . . ? C2 B10 B11 58.8(2) . . ? C2 B10 B6 59.0(2) . . ? B11 B10 B6 107.9(3) . . ? C2 B10 B12 105.3(3) . . ? B11 B10 B12 60.2(2) . . ? B6 B10 B12 107.7(3) . . ? C2 B10 B9 105.6(3) . . ? B11 B10 B9 108.4(3) . . ? B6 B10 B9 59.9(2) . . ? B12 B10 B9 60.0(3) . . ? C2 B10 H101 117.8(19) . . ? B11 B10 H101 117(2) . . ? B6 B10 H101 122.0(19) . . ? B12 B10 H101 125.6(19) . . ? B9 B10 H101 129(2) . . ? C2 B11 B3 58.9(2) . . ? C2 B11 B7 105.6(3) . . ? B3 B11 B7 60.2(2) . . ? C2 B11 B10 58.6(2) . . ? B3 B11 B10 107.9(3) . . ? B7 B11 B10 108.5(3) . . ? C2 B11 B12 105.0(3) . . ? B3 B11 B12 108.1(3) . . ? B7 B11 B12 60.4(3) . . ? B10 B11 B12 59.9(2) . . ? C2 B11 H111 117.0(19) . . ? B3 B11 H111 116.8(19) . . ? B7 B11 H111 126.2(19) . . ? B10 B11 H111 121.0(19) . . ? B12 B11 H111 129.5(19) . . ? B8 B12 B10 108.4(3) . . ? B8 B12 B9 60.5(3) . . ? B10 B12 B9 60.2(2) . . ? B8 B12 B11 108.0(3) . . ? B10 B12 B11 59.8(2) . . ? B9 B12 B11 108.2(3) . . ? B8 B12 B7 60.3(3) . . ? B10 B12 B7 107.7(3) . . ? B9 B12 B7 108.7(3) . . ? B11 B12 B7 59.5(3) . . ? B8 B12 H121 122(2) . . ? B10 B12 H121 121(2) . . ? B9 B12 H121 121(3) . . ? B11 B12 H121 122(3) . . ? B7 B12 H121 123(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Sn1 Sn2 N3 -93.90(12) . . . . ? C2 Sn1 Sn2 N3 -173.00(13) . . . . ? N1 Sn1 Sn2 N6 103.58(14) . . . . ? C2 Sn1 Sn2 N6 24.48(15) . . . . ? N1 Sn1 Sn2 N4 -28.16(10) . . . . ? C2 Sn1 Sn2 N4 -107.25(12) . . . . ? N1 Sn1 Sn2 N5 161.47(10) . . . . ? C2 Sn1 Sn2 N5 82.38(12) . . . . ? N1 Sn1 Sn2 C10 -60.72(12) . . . . ? C2 Sn1 Sn2 C10 -139.82(13) . . . . ? N1 Sn1 Sn2 C21 136.88(11) . . . . ? C2 Sn1 Sn2 C21 57.78(13) . . . . ? C2 Sn1 N1 C3 -4.4(3) . . . . ? Sn2 Sn1 N1 C3 -95.0(3) . . . . ? C2 Sn1 N1 C4 -176.8(3) . . . . ? Sn2 Sn1 N1 C4 92.6(2) . . . . ? N6 Sn2 N3 C10 -92.8(2) . . . . ? N4 Sn2 N3 C10 -3.75(19) . . . . ? N5 Sn2 N3 C10 -153.0(2) . . . . ? C21 Sn2 N3 C10 -123.7(2) . . . . ? Sn1 Sn2 N3 C10 99.4(2) . . . . ? N6 Sn2 N3 C15 90.6(3) . . . . ? N4 Sn2 N3 C15 179.6(4) . . . . ? N5 Sn2 N3 C15 30.3(3) . . . . ? C10 Sn2 N3 C15 -176.6(5) . . . . ? C21 Sn2 N3 C15 59.6(3) . . . . ? Sn1 Sn2 N3 C15 -77.3(3) . . . . ? N3 Sn2 N4 C10 3.77(19) . . . . ? N6 Sn2 N4 C10 108.2(2) . . . . ? N5 Sn2 N4 C10 61.8(3) . . . . ? C21 Sn2 N4 C10 93.0(2) . . . . ? Sn1 Sn2 N4 C10 -102.29(19) . . . . ? N3 Sn2 N4 C18 159.5(4) . . . . ? N6 Sn2 N4 C18 -96.0(4) . . . . ? N5 Sn2 N4 C18 -142.4(3) . . . . ? C10 Sn2 N4 C18 155.7(5) . . . . ? C21 Sn2 N4 C18 -111.3(4) . . . . ? Sn1 Sn2 N4 C18 53.4(4) . . . . ? N3 Sn2 N5 C21 108.0(2) . . . . ? N6 Sn2 N5 C21 3.81(18) . . . . ? N4 Sn2 N5 C21 60.4(3) . . . . ? C10 Sn2 N5 C21 92.2(2) . . . . ? Sn1 Sn2 N5 C21 -134.55(18) . . . . ? N3 Sn2 N5 C26 -97.2(4) . . . . ? N6 Sn2 N5 C26 158.5(4) . . . . ? N4 Sn2 N5 C26 -144.8(3) . . . . ? C10 Sn2 N5 C26 -113.1(4) . . . . ? C21 Sn2 N5 C26 154.7(5) . . . . ? Sn1 Sn2 N5 C26 20.2(4) . . . . ? N3 Sn2 N6 C21 -93.3(2) . . . . ? N4 Sn2 N6 C21 -153.67(19) . . . . ? N5 Sn2 N6 C21 -3.81(18) . . . . ? C10 Sn2 N6 C21 -124.4(2) . . . . ? Sn1 Sn2 N6 C21 70.2(2) . . . . ? N3 Sn2 N6 C29 80.4(3) . . . . ? N4 Sn2 N6 C29 20.0(3) . . . . ? N5 Sn2 N6 C29 169.8(3) . . . . ? C10 Sn2 N6 C29 49.2(3) . . . . ? C21 Sn2 N6 C29 173.6(4) . . . . ? Sn1 Sn2 N6 C29 -116.2(3) . . . . ? C3 C1 C2 B10 147.1(3) . . . . ? B5 C1 C2 B10 0.0(4) . . . . ? B6 C1 C2 B10 38.9(3) . . . . ? B4 C1 C2 B10 -67.4(3) . . . . ? B3 C1 C2 B10 -106.6(3) . . . . ? C3 C1 C2 B11 -145.5(3) . . . . ? B5 C1 C2 B11 67.4(4) . . . . ? B6 C1 C2 B11 106.4(3) . . . . ? B4 C1 C2 B11 0.0(4) . . . . ? B3 C1 C2 B11 -39.1(3) . . . . ? C3 C1 C2 B3 -106.3(3) . . . . ? B5 C1 C2 B3 106.6(3) . . . . ? B6 C1 C2 B3 145.6(3) . . . . ? B4 C1 C2 B3 39.2(3) . . . . ? C3 C1 C2 B6 108.1(3) . . . . ? B5 C1 C2 B6 -39.0(3) . . . . ? B4 C1 C2 B6 -106.4(3) . . . . ? B3 C1 C2 B6 -145.6(3) . . . . ? C3 C1 C2 Sn1 -4.8(3) . . . . ? B5 C1 C2 Sn1 -151.9(2) . . . . ? B6 C1 C2 Sn1 -113.0(2) . . . . ? B4 C1 C2 Sn1 140.7(2) . . . . ? B3 C1 C2 Sn1 101.5(2) . . . . ? N1 Sn1 C2 C1 4.5(2) . . . . ? Sn2 Sn1 C2 C1 102.5(2) . . . . ? N1 Sn1 C2 B10 -139.8(3) . . . . ? Sn2 Sn1 C2 B10 -41.8(3) . . . . ? N1 Sn1 C2 B11 138.7(3) . . . . ? Sn2 Sn1 C2 B11 -123.3(3) . . . . ? N1 Sn1 C2 B3 69.9(2) . . . . ? Sn2 Sn1 C2 B3 167.9(2) . . . . ? N1 Sn1 C2 B6 -62.3(2) . . . . ? Sn2 Sn1 C2 B6 35.7(2) . . . . ? C7 N2 C3 N1 -178.2(3) . . . . ? C7 N2 C3 C1 3.2(6) . . . . ? C4 N1 C3 N2 -3.6(5) . . . . ? Sn1 N1 C3 N2 -176.3(3) . . . . ? C4 N1 C3 C1 175.3(3) . . . . ? Sn1 N1 C3 C1 2.5(4) . . . . ? C2 C1 C3 N2 -179.4(3) . . . . ? B5 C1 C3 N2 -37.9(5) . . . . ? B6 C1 C3 N2 -111.4(4) . . . . ? B4 C1 C3 N2 40.8(6) . . . . ? B3 C1 C3 N2 113.5(4) . . . . ? C2 C1 C3 N1 1.9(4) . . . . ? B5 C1 C3 N1 143.3(3) . . . . ? B6 C1 C3 N1 69.8(4) . . . . ? B4 C1 C3 N1 -137.9(3) . . . . ? B3 C1 C3 N1 -65.3(4) . . . . ? C3 N1 C4 C6 155.3(3) . . . . ? Sn1 N1 C4 C6 -31.5(4) . . . . ? C3 N1 C4 C5 -81.3(4) . . . . ? Sn1 N1 C4 C5 91.9(3) . . . . ? C3 N2 C7 C8 112.5(5) . . . . ? C3 N2 C7 C9 -127.0(4) . . . . ? C18 N4 C10 N3 -168.9(3) . . . . ? Sn2 N4 C10 N3 -5.6(3) . . . . ? C18 N4 C10 C11 9.5(5) . . . . ? Sn2 N4 C10 C11 172.8(3) . . . . ? C18 N4 C10 Sn2 -163.3(3) . . . . ? C15 N3 C10 N4 -176.7(3) . . . . ? Sn2 N3 C10 N4 6.1(3) . . . . ? C15 N3 C10 C11 4.7(5) . . . . ? Sn2 N3 C10 C11 -172.4(3) . . . . ? C15 N3 C10 Sn2 177.2(4) . . . . ? N3 Sn2 C10 N4 -173.5(3) . . . . ? N6 Sn2 C10 N4 -77.6(2) . . . . ? N5 Sn2 C10 N4 -140.72(19) . . . . ? C21 Sn2 C10 N4 -105.8(2) . . . . ? Sn1 Sn2 C10 N4 91.44(19) . . . . ? N6 Sn2 C10 N3 95.8(2) . . . . ? N4 Sn2 C10 N3 173.5(3) . . . . ? N5 Sn2 C10 N3 32.8(2) . . . . ? C21 Sn2 C10 N3 67.7(2) . . . . ? Sn1 Sn2 C10 N3 -95.1(2) . . . . ? N3 Sn2 C10 C11 55.7(19) . . . . ? N6 Sn2 C10 C11 151.5(19) . . . . ? N4 Sn2 C10 C11 -131(2) . . . . ? N5 Sn2 C10 C11 88(2) . . . . ? C21 Sn2 C10 C11 123.4(19) . . . . ? Sn1 Sn2 C10 C11 -39(2) . . . . ? N4 C10 C11 C12 -97.0(4) . . . . ? N3 C10 C11 C12 81.4(5) . . . . ? Sn2 C10 C11 C12 30(2) . . . . ? C10 C11 C12 C13 -170.7(4) . . . . ? C11 C12 C13 C14 -59.5(6) . . . . ? C10 N3 C15 C17 104.7(4) . . . . ? Sn2 N3 C15 C17 -79.4(4) . . . . ? C10 N3 C15 C16 -131.1(4) . . . . ? Sn2 N3 C15 C16 44.7(5) . . . . ? C10 N4 C18 C20 -86.9(4) . . . . ? Sn2 N4 C18 C20 122.2(3) . . . . ? C10 N4 C18 C19 150.6(3) . . . . ? Sn2 N4 C18 C19 -0.3(5) . . . . ? C26 N5 C21 N6 -167.9(3) . . . . ? Sn2 N5 C21 N6 -5.7(3) . . . . ? C26 N5 C21 C22 10.7(5) . . . . ? Sn2 N5 C21 C22 172.8(3) . . . . ? C26 N5 C21 Sn2 -162.2(3) . . . . ? C29 N6 C21 N5 -168.5(3) . . . . ? Sn2 N6 C21 N5 6.2(3) . . . . ? C29 N6 C21 C22 12.9(5) . . . . ? Sn2 N6 C21 C22 -172.3(3) . . . . ? C29 N6 C21 Sn2 -174.7(4) . . . . ? N3 Sn2 C21 N5 -78.0(2) . . . . ? N6 Sn2 C21 N5 -173.4(3) . . . . ? N4 Sn2 C21 N5 -141.57(19) . . . . ? C10 Sn2 C21 N5 -106.7(2) . . . . ? Sn1 Sn2 C21 N5 55.0(2) . . . . ? N3 Sn2 C21 N6 95.4(2) . . . . ? N4 Sn2 C21 N6 31.8(2) . . . . ? N5 Sn2 C21 N6 173.4(3) . . . . ? C10 Sn2 C21 N6 66.7(2) . . . . ? Sn1 Sn2 C21 N6 -131.63(18) . . . . ? N3 Sn2 C21 C22 166(2) . . . . ? N6 Sn2 C21 C22 71(2) . . . . ? N4 Sn2 C21 C22 103(2) . . . . ? N5 Sn2 C21 C22 -116(2) . . . . ? C10 Sn2 C21 C22 138(2) . . . . ? Sn1 Sn2 C21 C22 -61(2) . . . . ? N5 C21 C22 C23 -87.0(4) . . . . ? N6 C21 C22 C23 91.4(4) . . . . ? Sn2 C21 C22 C23 25(2) . . . . ? C21 C22 C23 C24 -75.0(4) . . . . ? C22 C23 C24 C25 -178.8(3) . . . . ? C21 N5 C26 C27 135.8(3) . . . . ? Sn2 N5 C26 C27 -13.8(5) . . . . ? C21 N5 C26 C28 -100.2(4) . . . . ? Sn2 N5 C26 C28 110.2(4) . . . . ? C21 N6 C29 C31 -133.4(3) . . . . ? Sn2 N6 C29 C31 54.3(4) . . . . ? C21 N6 C29 C30 102.4(4) . . . . ? Sn2 N6 C29 C30 -69.9(4) . . . . ? B10 C2 B3 C1 101.5(3) . . . . ? B11 C2 B3 C1 138.1(3) . . . . ? B6 C2 B3 C1 32.5(3) . . . . ? Sn1 C2 B3 C1 -102.6(2) . . . . ? C1 C2 B3 B11 -138.1(3) . . . . ? B10 C2 B3 B11 -36.6(3) . . . . ? B6 C2 B3 B11 -105.6(3) . . . . ? Sn1 C2 B3 B11 119.2(3) . . . . ? C1 C2 B3 B7 -98.7(3) . . . . ? B10 C2 B3 B7 2.8(4) . . . . ? B11 C2 B3 B7 39.4(3) . . . . ? B6 C2 B3 B7 -66.2(4) . . . . ? Sn1 C2 B3 B7 158.7(3) . . . . ? C1 C2 B3 B4 -36.3(3) . . . . ? B10 C2 B3 B4 65.2(4) . . . . ? B11 C2 B3 B4 101.9(3) . . . . ? B6 C2 B3 B4 -3.7(4) . . . . ? Sn1 C2 B3 B4 -138.9(2) . . . . ? C3 C1 B3 C2 104.3(3) . . . . ? B5 C1 B3 C2 -101.0(3) . . . . ? B6 C1 B3 C2 -32.4(3) . . . . ? B4 C1 B3 C2 -138.0(3) . . . . ? C3 C1 B3 B11 140.7(3) . . . . ? C2 C1 B3 B11 36.4(2) . . . . ? B5 C1 B3 B11 -64.6(3) . . . . ? B6 C1 B3 B11 4.0(4) . . . . ? B4 C1 B3 B11 -101.7(3) . . . . ? C3 C1 B3 B7 -156.9(3) . . . . ? C2 C1 B3 B7 98.8(3) . . . . ? B5 C1 B3 B7 -2.2(4) . . . . ? B6 C1 B3 B7 66.4(4) . . . . ? B4 C1 B3 B7 -39.2(3) . . . . ? C3 C1 B3 B4 -117.7(3) . . . . ? C2 C1 B3 B4 138.0(3) . . . . ? B5 C1 B3 B4 37.1(3) . . . . ? B6 C1 B3 B4 105.6(3) . . . . ? C3 C1 B4 B8 -155.3(3) . . . . ? C2 C1 B4 B8 63.7(4) . . . . ? B5 C1 B4 B8 -39.6(3) . . . . ? B6 C1 B4 B8 -2.4(4) . . . . ? B3 C1 B4 B8 102.1(3) . . . . ? C3 C1 B4 B7 141.8(3) . . . . ? C2 C1 B4 B7 0.8(4) . . . . ? B5 C1 B4 B7 -102.5(3) . . . . ? B6 C1 B4 B7 -65.3(4) . . . . ? B3 C1 B4 B7 39.2(3) . . . . ? C3 C1 B4 B5 -115.7(4) . . . . ? C2 C1 B4 B5 103.4(3) . . . . ? B6 C1 B4 B5 37.3(3) . . . . ? B3 C1 B4 B5 141.7(3) . . . . ? C3 C1 B4 B3 102.6(4) . . . . ? C2 C1 B4 B3 -38.3(3) . . . . ? B5 C1 B4 B3 -141.7(3) . . . . ? B6 C1 B4 B3 -104.4(3) . . . . ? C2 B3 B4 C1 36.1(2) . . . . ? B11 B3 B4 C1 97.7(3) . . . . ? B7 B3 B4 C1 135.2(3) . . . . ? C2 B3 B4 B8 -61.3(4) . . . . ? C1 B3 B4 B8 -97.4(3) . . . . ? B11 B3 B4 B8 0.3(4) . . . . ? B7 B3 B4 B8 37.8(3) . . . . ? C2 B3 B4 B7 -99.1(3) . . . . ? C1 B3 B4 B7 -135.2(3) . . . . ? B11 B3 B4 B7 -37.5(3) . . . . ? C2 B3 B4 B5 2.4(4) . . . . ? C1 B3 B4 B5 -33.7(3) . . . . ? B11 B3 B4 B5 64.0(4) . . . . ? B7 B3 B4 B5 101.5(3) . . . . ? C3 C1 B5 B6 -104.1(3) . . . . ? C2 C1 B5 B6 38.4(3) . . . . ? B4 C1 B5 B6 141.2(3) . . . . ? B3 C1 B5 B6 104.2(3) . . . . ? C3 C1 B5 B9 -143.4(3) . . . . ? C2 C1 B5 B9 -0.9(4) . . . . ? B6 C1 B5 B9 -39.3(3) . . . . ? B4 C1 B5 B9 101.9(3) . . . . ? B3 C1 B5 B9 64.9(4) . . . . ? C3 C1 B5 B4 114.7(4) . . . . ? C2 C1 B5 B4 -102.8(3) . . . . ? B6 C1 B5 B4 -141.2(3) . . . . ? B3 C1 B5 B4 -37.0(3) . . . . ? C3 C1 B5 B8 154.0(3) . . . . ? C2 C1 B5 B8 -63.6(3) . . . . ? B6 C1 B5 B8 -101.9(3) . . . . ? B4 C1 B5 B8 39.2(3) . . . . ? B3 C1 B5 B8 2.3(4) . . . . ? B8 B4 B5 C1 134.9(3) . . . . ? B7 B4 B5 C1 97.2(3) . . . . ? B3 B4 B5 C1 33.9(3) . . . . ? C1 B4 B5 B6 -34.3(3) . . . . ? B8 B4 B5 B6 100.6(3) . . . . ? B7 B4 B5 B6 62.9(3) . . . . ? B3 B4 B5 B6 -0.3(4) . . . . ? C1 B4 B5 B9 -97.6(3) . . . . ? B8 B4 B5 B9 37.3(3) . . . . ? B7 B4 B5 B9 -0.4(4) . . . . ? B3 B4 B5 B9 -63.7(3) . . . . ? C1 B4 B5 B8 -134.9(3) . . . . ? B7 B4 B5 B8 -37.7(3) . . . . ? B3 B4 B5 B8 -101.0(3) . . . . ? C3 C1 B6 C2 -103.8(3) . . . . ? B5 C1 B6 C2 138.3(3) . . . . ? B4 C1 B6 C2 100.9(3) . . . . ? B3 C1 B6 C2 32.3(3) . . . . ? C3 C1 B6 B5 117.9(4) . . . . ? C2 C1 B6 B5 -138.3(3) . . . . ? B4 C1 B6 B5 -37.4(3) . . . . ? B3 C1 B6 B5 -106.0(3) . . . . ? C3 C1 B6 B10 -139.7(3) . . . . ? C2 C1 B6 B10 -35.9(2) . . . . ? B5 C1 B6 B10 102.4(3) . . . . ? B4 C1 B6 B10 65.0(4) . . . . ? B3 C1 B6 B10 -3.7(4) . . . . ? C3 C1 B6 B9 157.4(3) . . . . ? C2 C1 B6 B9 -98.8(3) . . . . ? B5 C1 B6 B9 39.5(3) . . . . ? B4 C1 B6 B9 2.1(4) . . . . ? B3 C1 B6 B9 -66.6(4) . . . . ? B10 C2 B6 C1 -138.5(3) . . . . ? B11 C2 B6 C1 -101.4(3) . . . . ? B3 C2 B6 C1 -32.7(3) . . . . ? Sn1 C2 B6 C1 97.6(2) . . . . ? C1 C2 B6 B5 36.2(2) . . . . ? B10 C2 B6 B5 -102.2(3) . . . . ? B11 C2 B6 B5 -65.1(4) . . . . ? B3 C2 B6 B5 3.5(4) . . . . ? Sn1 C2 B6 B5 133.9(2) . . . . ? C1 C2 B6 B10 138.5(3) . . . . ? B11 C2 B6 B10 37.1(3) . . . . ? B3 C2 B6 B10 105.8(3) . . . . ? Sn1 C2 B6 B10 -123.9(3) . . . . ? C1 C2 B6 B9 99.1(3) . . . . ? B10 C2 B6 B9 -39.4(3) . . . . ? B11 C2 B6 B9 -2.3(4) . . . . ? B3 C2 B6 B9 66.4(4) . . . . ? Sn1 C2 B6 B9 -163.3(2) . . . . ? B9 B5 B6 C1 135.2(3) . . . . ? B4 B5 B6 C1 34.2(3) . . . . ? B8 B5 B6 C1 97.1(3) . . . . ? C1 B5 B6 C2 -36.0(2) . . . . ? B9 B5 B6 C2 99.2(3) . . . . ? B4 B5 B6 C2 -1.8(4) . . . . ? B8 B5 B6 C2 61.1(3) . . . . ? C1 B5 B6 B10 -97.5(3) . . . . ? B9 B5 B6 B10 37.7(3) . . . . ? B4 B5 B6 B10 -63.2(4) . . . . ? B8 B5 B6 B10 -0.3(4) . . . . ? C1 B5 B6 B9 -135.2(3) . . . . ? B4 B5 B6 B9 -101.0(3) . . . . ? B8 B5 B6 B9 -38.1(3) . . . . ? C2 B3 B7 B11 -38.9(3) . . . . ? C1 B3 B7 B11 -99.5(3) . . . . ? B4 B3 B7 B11 -138.0(3) . . . . ? C2 B3 B7 B4 99.1(3) . . . . ? C1 B3 B7 B4 38.5(3) . . . . ? B11 B3 B7 B4 138.0(3) . . . . ? C2 B3 B7 B12 -1.1(4) . . . . ? C1 B3 B7 B12 -61.6(4) . . . . ? B11 B3 B7 B12 37.8(3) . . . . ? B4 B3 B7 B12 -100.2(4) . . . . ? C2 B3 B7 B8 61.7(4) . . . . ? C1 B3 B7 B8 1.1(4) . . . . ? B11 B3 B7 B8 100.6(3) . . . . ? B4 B3 B7 B8 -37.4(3) . . . . ? C1 B4 B7 B11 -1.4(4) . . . . ? B8 B4 B7 B11 -100.5(3) . . . . ? B5 B4 B7 B11 -62.8(4) . . . . ? B3 B4 B7 B11 37.4(3) . . . . ? C1 B4 B7 B3 -38.8(3) . . . . ? B8 B4 B7 B3 -137.9(3) . . . . ? B5 B4 B7 B3 -100.2(3) . . . . ? C1 B4 B7 B12 62.0(4) . . . . ? B8 B4 B7 B12 -37.1(3) . . . . ? B5 B4 B7 B12 0.6(4) . . . . ? B3 B4 B7 B12 100.8(3) . . . . ? C1 B4 B7 B8 99.1(3) . . . . ? B5 B4 B7 B8 37.7(3) . . . . ? B3 B4 B7 B8 137.9(3) . . . . ? C1 B4 B8 B12 -61.7(4) . . . . ? B7 B4 B8 B12 37.6(3) . . . . ? B5 B4 B8 B12 -100.5(3) . . . . ? B3 B4 B8 B12 0.1(4) . . . . ? C1 B4 B8 B5 38.8(3) . . . . ? B7 B4 B8 B5 138.1(3) . . . . ? B3 B4 B8 B5 100.6(3) . . . . ? C1 B4 B8 B7 -99.3(3) . . . . ? B5 B4 B8 B7 -138.1(3) . . . . ? B3 B4 B8 B7 -37.5(3) . . . . ? C1 B4 B8 B9 1.7(4) . . . . ? B7 B4 B8 B9 101.0(4) . . . . ? B5 B4 B8 B9 -37.1(3) . . . . ? B3 B4 B8 B9 63.5(4) . . . . ? C1 B5 B8 B12 62.2(4) . . . . ? B6 B5 B8 B12 0.6(4) . . . . ? B9 B5 B8 B12 -37.4(3) . . . . ? B4 B5 B8 B12 101.0(4) . . . . ? C1 B5 B8 B4 -38.8(3) . . . . ? B6 B5 B8 B4 -100.4(3) . . . . ? B9 B5 B8 B4 -138.4(3) . . . . ? C1 B5 B8 B7 -1.4(4) . . . . ? B6 B5 B8 B7 -63.0(4) . . . . ? B9 B5 B8 B7 -101.0(3) . . . . ? B4 B5 B8 B7 37.4(3) . . . . ? C1 B5 B8 B9 99.5(3) . . . . ? B6 B5 B8 B9 38.0(3) . . . . ? B4 B5 B8 B9 138.4(3) . . . . ? B11 B7 B8 B12 -37.2(3) . . . . ? B3 B7 B8 B12 -100.4(3) . . . . ? B4 B7 B8 B12 -138.1(3) . . . . ? B11 B7 B8 B4 100.8(3) . . . . ? B3 B7 B8 B4 37.7(3) . . . . ? B12 B7 B8 B4 138.1(3) . . . . ? B11 B7 B8 B5 63.3(4) . . . . ? B3 B7 B8 B5 0.2(4) . . . . ? B4 B7 B8 B5 -37.5(3) . . . . ? B12 B7 B8 B5 100.6(3) . . . . ? B11 B7 B8 B9 0.1(4) . . . . ? B3 B7 B8 B9 -63.0(4) . . . . ? B4 B7 B8 B9 -100.7(3) . . . . ? B12 B7 B8 B9 37.4(3) . . . . ? C1 B6 B9 B12 61.8(4) . . . . ? C2 B6 B9 B12 1.0(4) . . . . ? B5 B6 B9 B12 100.6(3) . . . . ? B10 B6 B9 B12 -37.5(3) . . . . ? C1 B6 B9 B5 -38.8(3) . . . . ? C2 B6 B9 B5 -99.5(3) . . . . ? B10 B6 B9 B5 -138.1(3) . . . . ? C1 B6 B9 B10 99.3(3) . . . . ? C2 B6 B9 B10 38.5(3) . . . . ? B5 B6 B9 B10 138.1(3) . . . . ? C1 B6 B9 B8 -0.9(4) . . . . ? C2 B6 B9 B8 -61.7(4) . . . . ? B5 B6 B9 B8 37.9(3) . . . . ? B10 B6 B9 B8 -100.2(3) . . . . ? C1 B5 B9 B6 38.8(3) . . . . ? B4 B5 B9 B6 100.4(3) . . . . ? B8 B5 B9 B6 137.4(3) . . . . ? C1 B5 B9 B12 -61.5(3) . . . . ? B6 B5 B9 B12 -100.3(3) . . . . ? B4 B5 B9 B12 0.1(4) . . . . ? B8 B5 B9 B12 37.1(3) . . . . ? C1 B5 B9 B10 1.5(4) . . . . ? B6 B5 B9 B10 -37.3(3) . . . . ? B4 B5 B9 B10 63.1(3) . . . . ? B8 B5 B9 B10 100.1(3) . . . . ? C1 B5 B9 B8 -98.7(3) . . . . ? B6 B5 B9 B8 -137.4(3) . . . . ? B4 B5 B9 B8 -37.0(3) . . . . ? B12 B8 B9 B6 100.3(3) . . . . ? B4 B8 B9 B6 -0.5(4) . . . . ? B5 B8 B9 B6 -37.8(3) . . . . ? B7 B8 B9 B6 62.9(4) . . . . ? B4 B8 B9 B12 -100.9(4) . . . . ? B5 B8 B9 B12 -138.1(3) . . . . ? B7 B8 B9 B12 -37.5(3) . . . . ? B12 B8 B9 B5 138.1(3) . . . . ? B4 B8 B9 B5 37.3(3) . . . . ? B7 B8 B9 B5 100.6(3) . . . . ? B12 B8 B9 B10 37.4(3) . . . . ? B4 B8 B9 B10 -63.5(4) . . . . ? B5 B8 B9 B10 -100.7(3) . . . . ? B7 B8 B9 B10 -0.1(4) . . . . ? C1 C2 B10 B11 103.3(3) . . . . ? B3 C2 B10 B11 36.5(3) . . . . ? B6 C2 B10 B11 141.5(3) . . . . ? Sn1 C2 B10 B11 -112.7(3) . . . . ? C1 C2 B10 B6 -38.2(3) . . . . ? B11 C2 B10 B6 -141.5(3) . . . . ? B3 C2 B10 B6 -105.0(3) . . . . ? Sn1 C2 B10 B6 105.8(3) . . . . ? C1 C2 B10 B12 63.5(4) . . . . ? B11 C2 B10 B12 -39.8(3) . . . . ? B3 C2 B10 B12 -3.3(4) . . . . ? B6 C2 B10 B12 101.7(3) . . . . ? Sn1 C2 B10 B12 -152.5(3) . . . . ? C1 C2 B10 B9 1.0(4) . . . . ? B11 C2 B10 B9 -102.3(3) . . . . ? B3 C2 B10 B9 -65.8(4) . . . . ? B6 C2 B10 B9 39.2(3) . . . . ? Sn1 C2 B10 B9 145.0(3) . . . . ? C1 B6 B10 C2 35.8(2) . . . . ? B5 B6 B10 C2 97.6(3) . . . . ? B9 B6 B10 C2 135.3(3) . . . . ? C1 B6 B10 B11 1.8(3) . . . . ? C2 B6 B10 B11 -34.0(2) . . . . ? B5 B6 B10 B11 63.5(4) . . . . ? B9 B6 B10 B11 101.2(3) . . . . ? C1 B6 B10 B12 -61.8(3) . . . . ? C2 B6 B10 B12 -97.6(3) . . . . ? B5 B6 B10 B12 0.0(4) . . . . ? B9 B6 B10 B12 37.7(3) . . . . ? C1 B6 B10 B9 -99.4(3) . . . . ? C2 B6 B10 B9 -135.3(3) . . . . ? B5 B6 B10 B9 -37.7(3) . . . . ? B6 B9 B10 C2 -38.8(3) . . . . ? B12 B9 B10 C2 99.0(3) . . . . ? B5 B9 B10 C2 -1.5(4) . . . . ? B8 B9 B10 C2 61.7(3) . . . . ? B6 B9 B10 B11 -100.5(3) . . . . ? B12 B9 B10 B11 37.3(3) . . . . ? B5 B9 B10 B11 -63.2(4) . . . . ? B8 B9 B10 B11 0.0(4) . . . . ? B12 B9 B10 B6 137.8(3) . . . . ? B5 B9 B10 B6 37.3(3) . . . . ? B8 B9 B10 B6 100.5(3) . . . . ? B6 B9 B10 B12 -137.8(3) . . . . ? B5 B9 B10 B12 -100.5(3) . . . . ? B8 B9 B10 B12 -37.3(3) . . . . ? C1 C2 B11 B3 38.7(3) . . . . ? B10 C2 B11 B3 142.1(3) . . . . ? B6 C2 B11 B3 105.0(3) . . . . ? Sn1 C2 B11 B3 -95.1(3) . . . . ? C1 C2 B11 B7 -0.9(4) . . . . ? B10 C2 B11 B7 102.4(3) . . . . ? B3 C2 B11 B7 -39.6(3) . . . . ? B6 C2 B11 B7 65.3(4) . . . . ? Sn1 C2 B11 B7 -134.7(3) . . . . ? C1 C2 B11 B10 -103.3(3) . . . . ? B3 C2 B11 B10 -142.1(3) . . . . ? B6 C2 B11 B10 -37.1(3) . . . . ? Sn1 C2 B11 B10 122.8(3) . . . . ? C1 C2 B11 B12 -63.7(4) . . . . ? B10 C2 B11 B12 39.6(3) . . . . ? B3 C2 B11 B12 -102.4(3) . . . . ? B6 C2 B11 B12 2.5(4) . . . . ? Sn1 C2 B11 B12 162.4(2) . . . . ? C1 B3 B11 C2 -36.1(2) . . . . ? B7 B3 B11 C2 -134.9(3) . . . . ? B4 B3 B11 C2 -97.5(3) . . . . ? C2 B3 B11 B7 134.9(3) . . . . ? C1 B3 B11 B7 98.9(3) . . . . ? B4 B3 B11 B7 37.5(3) . . . . ? C2 B3 B11 B10 33.5(3) . . . . ? C1 B3 B11 B10 -2.6(4) . . . . ? B7 B3 B11 B10 -101.5(3) . . . . ? B4 B3 B11 B10 -64.0(3) . . . . ? C2 B3 B11 B12 96.9(3) . . . . ? C1 B3 B11 B12 60.8(3) . . . . ? B7 B3 B11 B12 -38.1(3) . . . . ? B4 B3 B11 B12 -0.6(4) . . . . ? B3 B7 B11 C2 39.0(3) . . . . ? B4 B7 B11 C2 1.4(4) . . . . ? B12 B7 B11 C2 -98.6(3) . . . . ? B8 B7 B11 C2 -61.6(4) . . . . ? B4 B7 B11 B3 -37.6(3) . . . . ? B12 B7 B11 B3 -137.6(3) . . . . ? B8 B7 B11 B3 -100.6(3) . . . . ? B3 B7 B11 B10 100.5(3) . . . . ? B4 B7 B11 B10 62.9(4) . . . . ? B12 B7 B11 B10 -37.1(3) . . . . ? B8 B7 B11 B10 -0.1(4) . . . . ? B3 B7 B11 B12 137.6(3) . . . . ? B4 B7 B11 B12 100.0(4) . . . . ? B8 B7 B11 B12 36.9(3) . . . . ? B6 B10 B11 C2 34.1(3) . . . . ? B12 B10 B11 C2 134.6(3) . . . . ? B9 B10 B11 C2 97.4(3) . . . . ? C2 B10 B11 B3 -33.6(3) . . . . ? B6 B10 B11 B3 0.5(4) . . . . ? B12 B10 B11 B3 101.0(3) . . . . ? B9 B10 B11 B3 63.8(3) . . . . ? C2 B10 B11 B7 -97.4(3) . . . . ? B6 B10 B11 B7 -63.3(3) . . . . ? B12 B10 B11 B7 37.3(3) . . . . ? B9 B10 B11 B7 0.1(4) . . . . ? C2 B10 B11 B12 -134.6(3) . . . . ? B6 B10 B11 B12 -100.5(3) . . . . ? B9 B10 B11 B12 -37.2(3) . . . . ? B4 B8 B12 B10 62.9(4) . . . . ? B5 B8 B12 B10 -0.6(4) . . . . ? B7 B8 B12 B10 100.4(3) . . . . ? B9 B8 B12 B10 -37.9(3) . . . . ? B4 B8 B12 B9 100.8(3) . . . . ? B5 B8 B12 B9 37.3(3) . . . . ? B7 B8 B12 B9 138.2(3) . . . . ? B4 B8 B12 B11 -0.4(4) . . . . ? B5 B8 B12 B11 -63.9(4) . . . . ? B7 B8 B12 B11 37.0(3) . . . . ? B9 B8 B12 B11 -101.2(3) . . . . ? B4 B8 B12 B7 -37.5(3) . . . . ? B5 B8 B12 B7 -101.0(3) . . . . ? B9 B8 B12 B7 -138.2(3) . . . . ? C2 B10 B12 B8 -61.4(4) . . . . ? B11 B10 B12 B8 -100.5(3) . . . . ? B6 B10 B12 B8 0.4(4) . . . . ? B9 B10 B12 B8 38.0(3) . . . . ? C2 B10 B12 B9 -99.4(3) . . . . ? B11 B10 B12 B9 -138.5(3) . . . . ? B6 B10 B12 B9 -37.6(3) . . . . ? C2 B10 B12 B11 39.2(3) . . . . ? B6 B10 B12 B11 100.9(3) . . . . ? B9 B10 B12 B11 138.5(3) . . . . ? C2 B10 B12 B7 2.5(4) . . . . ? B11 B10 B12 B7 -36.7(3) . . . . ? B6 B10 B12 B7 64.2(4) . . . . ? B9 B10 B12 B7 101.8(4) . . . . ? B6 B9 B12 B8 -100.3(3) . . . . ? B5 B9 B12 B8 -37.4(3) . . . . ? B10 B9 B12 B8 -137.8(3) . . . . ? B6 B9 B12 B10 37.5(3) . . . . ? B5 B9 B12 B10 100.5(3) . . . . ? B8 B9 B12 B10 137.8(3) . . . . ? B6 B9 B12 B11 0.4(4) . . . . ? B5 B9 B12 B11 63.4(4) . . . . ? B10 B9 B12 B11 -37.1(3) . . . . ? B8 B9 B12 B11 100.8(3) . . . . ? B6 B9 B12 B7 -62.7(4) . . . . ? B5 B9 B12 B7 0.3(4) . . . . ? B10 B9 B12 B7 -100.2(3) . . . . ? B8 B9 B12 B7 37.7(3) . . . . ? C2 B11 B12 B8 62.3(4) . . . . ? B3 B11 B12 B8 0.6(4) . . . . ? B7 B11 B12 B8 -37.4(3) . . . . ? B10 B11 B12 B8 101.3(3) . . . . ? C2 B11 B12 B10 -39.0(3) . . . . ? B3 B11 B12 B10 -100.6(3) . . . . ? B7 B11 B12 B10 -138.7(3) . . . . ? C2 B11 B12 B9 -1.7(4) . . . . ? B3 B11 B12 B9 -63.4(4) . . . . ? B7 B11 B12 B9 -101.4(4) . . . . ? B10 B11 B12 B9 37.3(3) . . . . ? C2 B11 B12 B7 99.7(3) . . . . ? B3 B11 B12 B7 38.0(3) . . . . ? B10 B11 B12 B7 138.7(3) . . . . ? B11 B7 B12 B8 138.3(3) . . . . ? B3 B7 B12 B8 100.6(3) . . . . ? B4 B7 B12 B8 37.2(3) . . . . ? B11 B7 B12 B10 36.8(3) . . . . ? B3 B7 B12 B10 -0.9(4) . . . . ? B4 B7 B12 B10 -64.3(4) . . . . ? B8 B7 B12 B10 -101.5(3) . . . . ? B11 B7 B12 B9 100.6(3) . . . . ? B3 B7 B12 B9 62.9(4) . . . . ? B4 B7 B12 B9 -0.6(4) . . . . ? B8 B7 B12 B9 -37.7(3) . . . . ? B3 B7 B12 B11 -37.7(3) . . . . ? B4 B7 B12 B11 -101.2(3) . . . . ? B8 B7 B12 B11 -138.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.780 _refine_diff_density_min -1.245 _refine_diff_density_rms 0.103 _database_code_depnum_ccdc_archive 'CCDC 963128' ####################################################################### # # 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_ip210 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H29 B10 N2 P' _chemical_formula_weight 376.47 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C2 /c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 35.600(7) _cell_length_b 6.6979(13) _cell_length_c 24.238(5) _cell_angle_alpha 90.00 _cell_angle_beta 131.32(3) _cell_angle_gamma 90.00 _cell_volume 4340.6(15) _cell_formula_units_Z 8 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 23799 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 29.49 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.152 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 0.130 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(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 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23273 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_h_max 48 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 29.22 _reflns_number_total 5833 _reflns_number_gt 4846 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+1.3829P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5833 _refine_ls_number_parameters 369 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.0973 _refine_ls_wR_factor_gt 0.0922 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P P 0.070829(11) 0.01413(5) 0.205292(18) 0.01658(8) Uani 1 1 d . . . N1 N 0.12105(4) 0.09089(16) 0.29274(6) 0.0177(2) Uani 1 1 d . . . N2 N 0.20310(4) 0.20100(17) 0.37627(6) 0.0214(2) Uani 1 1 d . . . C1 C 0.16033(4) 0.15392(17) 0.24327(6) 0.0146(2) Uani 1 1 d . . . C2 C 0.10419(4) 0.07673(17) 0.17317(7) 0.0153(2) Uani 1 1 d . . . C3 C 0.16561(4) 0.15776(18) 0.31074(7) 0.0168(2) Uani 1 1 d . . . C4 C 0.12558(5) 0.0150(2) 0.35473(7) 0.0224(3) Uani 1 1 d . . . H4A H 0.1483(6) 0.108(2) 0.3958(9) 0.022(4) Uiso 1 1 d . . . C5 C 0.07534(6) 0.0183(3) 0.33544(10) 0.0332(3) Uani 1 1 d . . . H5C H 0.0800(7) -0.028(3) 0.3779(12) 0.042(5) Uiso 1 1 d . . . H5B H 0.0606(7) 0.146(3) 0.3213(11) 0.037(5) Uiso 1 1 d . . . H5A H 0.0512(8) -0.075(3) 0.2953(12) 0.049(6) Uiso 1 1 d . . . C6 C 0.14859(7) -0.1910(2) 0.37741(10) 0.0341(3) Uani 1 1 d . . . H6C H 0.1820(7) -0.189(3) 0.3921(11) 0.042(5) Uiso 1 1 d . . . H6B H 0.1277(7) -0.282(3) 0.3383(11) 0.036(5) Uiso 1 1 d . . . H6A H 0.1529(7) -0.238(3) 0.4206(11) 0.045(5) Uiso 1 1 d . . . C7 C 0.25158(5) 0.2644(2) 0.40105(7) 0.0224(3) Uani 1 1 d . . . H7A H 0.2520(6) 0.273(2) 0.3626(10) 0.027(4) Uiso 1 1 d . . . C8 C 0.29055(6) 0.1114(3) 0.45617(10) 0.0367(4) Uani 1 1 d . . . H8C H 0.2924(7) 0.107(3) 0.4980(12) 0.049(6) Uiso 1 1 d . . . H8B H 0.3230(8) 0.150(3) 0.4732(11) 0.046(5) Uiso 1 1 d . . . H8A H 0.2825(8) -0.023(3) 0.4333(12) 0.051(6) Uiso 1 1 d . . . C9 C 0.26357(6) 0.4695(3) 0.43577(10) 0.0324(3) Uani 1 1 d . . . H9C H 0.2967(7) 0.511(3) 0.4548(11) 0.038(5) Uiso 1 1 d . . . H9B H 0.2639(7) 0.465(3) 0.4764(11) 0.036(5) Uiso 1 1 d . . . H9A H 0.2399(8) 0.562(3) 0.4006(12) 0.050(6) Uiso 1 1 d . . . C10 C 0.02566(4) 0.21785(18) 0.16558(7) 0.0184(2) Uani 1 1 d . . . C11 C 0.03206(5) 0.3942(2) 0.20125(8) 0.0243(3) Uani 1 1 d . . . H11A H 0.0628(7) 0.418(3) 0.2507(10) 0.033(5) Uiso 1 1 d . . . C12 C -0.00592(6) 0.5347(2) 0.16591(9) 0.0294(3) Uani 1 1 d . . . H12A H -0.0008(7) 0.656(3) 0.1920(10) 0.036(5) Uiso 1 1 d . . . C13 C -0.05029(6) 0.5015(2) 0.09466(9) 0.0311(3) Uani 1 1 d . . . H13A H -0.0766(7) 0.603(3) 0.0702(11) 0.044(5) Uiso 1 1 d . . . C14 C -0.05694(5) 0.3259(2) 0.05905(8) 0.0287(3) Uani 1 1 d . . . H14A H -0.0869(7) 0.303(3) 0.0104(11) 0.038(5) Uiso 1 1 d . . . C15 C -0.01935(5) 0.1840(2) 0.09443(7) 0.0224(3) Uani 1 1 d . . . H15A H -0.0232(6) 0.057(3) 0.0707(10) 0.030(4) Uiso 1 1 d . . . B3 B 0.15301(5) -0.0882(2) 0.21157(8) 0.0178(3) Uani 1 1 d . . . H3 H 0.1562(6) -0.204(2) 0.2457(9) 0.024(4) Uiso 1 1 d . . . B4 B 0.20336(5) 0.0651(2) 0.23862(8) 0.0181(3) Uani 1 1 d . . . H4 H 0.2394(6) 0.028(2) 0.2885(9) 0.022(4) Uiso 1 1 d . . . B5 B 0.18239(5) 0.3185(2) 0.21646(8) 0.0175(3) Uani 1 1 d . . . H5 H 0.2058(6) 0.434(2) 0.2521(9) 0.021(4) Uiso 1 1 d . . . B6 B 0.11883(5) 0.3254(2) 0.17585(8) 0.0174(3) Uani 1 1 d . . . H6 H 0.1037(6) 0.434(2) 0.1887(9) 0.018(4) Uiso 1 1 d . . . B7 B 0.08283(5) 0.1833(2) 0.09325(8) 0.0203(3) Uani 1 1 d . . . H7 H 0.0429(6) 0.215(2) 0.0521(9) 0.024(4) Uiso 1 1 d . . . B8 B 0.13360(5) 0.3354(2) 0.11965(8) 0.0203(3) Uani 1 1 d . . . H8 H 0.1276(6) 0.473(2) 0.0920(9) 0.023(4) Uiso 1 1 d . . . B9 B 0.18578(5) 0.1758(2) 0.15817(8) 0.0201(3) Uani 1 1 d . . . H9 H 0.2141(6) 0.211(2) 0.1546(9) 0.024(4) Uiso 1 1 d . . . B10 B 0.16762(5) -0.0746(2) 0.15544(9) 0.0208(3) Uani 1 1 d . . . H10 H 0.1828(6) -0.202(2) 0.1503(9) 0.026(4) Uiso 1 1 d . . . B11 B 0.10386(5) -0.0692(2) 0.11519(8) 0.0200(3) Uani 1 1 d . . . H11 H 0.0773(6) -0.187(2) 0.0882(9) 0.026(4) Uiso 1 1 d . . . B12 B 0.12441(5) 0.0937(2) 0.08184(8) 0.0216(3) Uani 1 1 d . . . H12 H 0.1108(6) 0.076(2) 0.0269(9) 0.025(4) Uiso 1 1 d . . . 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 P 0.01309(14) 0.01796(15) 0.01797(15) -0.00226(12) 0.00994(12) -0.00278(11) N1 0.0138(4) 0.0240(5) 0.0158(5) -0.0010(4) 0.0100(4) -0.0030(4) N2 0.0152(5) 0.0317(6) 0.0173(5) -0.0031(4) 0.0107(4) -0.0044(4) C1 0.0118(5) 0.0155(5) 0.0151(5) -0.0025(4) 0.0082(4) -0.0016(4) C2 0.0126(5) 0.0165(5) 0.0149(5) -0.0026(4) 0.0082(4) -0.0020(4) C3 0.0143(5) 0.0194(5) 0.0179(6) -0.0011(4) 0.0112(5) -0.0003(4) C4 0.0218(6) 0.0294(6) 0.0197(6) -0.0015(5) 0.0152(5) -0.0045(5) C5 0.0284(7) 0.0492(9) 0.0329(8) 0.0013(7) 0.0249(7) -0.0040(7) C6 0.0397(9) 0.0326(8) 0.0324(8) 0.0084(7) 0.0248(7) 0.0034(7) C7 0.0142(5) 0.0362(7) 0.0160(6) -0.0041(5) 0.0096(5) -0.0061(5) C8 0.0200(7) 0.0490(10) 0.0350(9) 0.0066(8) 0.0156(6) 0.0022(6) C9 0.0281(7) 0.0401(8) 0.0316(8) -0.0106(7) 0.0208(7) -0.0119(6) C10 0.0143(5) 0.0218(6) 0.0207(6) -0.0014(5) 0.0122(5) -0.0008(4) C11 0.0194(6) 0.0256(6) 0.0260(7) -0.0070(5) 0.0141(5) -0.0041(5) C12 0.0312(7) 0.0231(6) 0.0375(8) -0.0048(6) 0.0242(7) 0.0000(5) C13 0.0289(7) 0.0305(7) 0.0346(8) 0.0072(6) 0.0212(6) 0.0100(6) C14 0.0212(6) 0.0380(8) 0.0201(7) 0.0030(6) 0.0107(6) 0.0052(5) C15 0.0187(6) 0.0277(6) 0.0201(6) -0.0026(5) 0.0125(5) -0.0005(5) B3 0.0178(6) 0.0152(6) 0.0219(7) -0.0023(5) 0.0137(6) -0.0003(5) B4 0.0162(6) 0.0192(6) 0.0212(7) -0.0022(5) 0.0133(6) -0.0004(5) B5 0.0177(6) 0.0171(6) 0.0196(7) -0.0020(5) 0.0131(6) -0.0025(5) B6 0.0167(6) 0.0158(6) 0.0189(6) -0.0004(5) 0.0114(5) -0.0002(5) B7 0.0193(6) 0.0228(7) 0.0166(6) -0.0011(5) 0.0109(6) -0.0019(5) B8 0.0223(7) 0.0201(6) 0.0191(7) -0.0005(5) 0.0139(6) -0.0025(5) B9 0.0211(7) 0.0218(6) 0.0214(7) -0.0048(5) 0.0157(6) -0.0045(5) B10 0.0223(7) 0.0194(6) 0.0257(7) -0.0057(5) 0.0180(6) -0.0034(5) B11 0.0207(6) 0.0209(6) 0.0199(7) -0.0069(5) 0.0141(6) -0.0042(5) B12 0.0230(7) 0.0250(7) 0.0192(7) -0.0051(6) 0.0149(6) -0.0053(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P N1 1.7174(14) . ? P C10 1.8249(13) . ? P C2 1.8475(12) . ? N1 C3 1.4123(15) . ? N1 C4 1.4905(17) . ? N2 C3 1.2605(17) . ? N2 C7 1.4668(16) . ? C1 C3 1.5179(17) . ? C1 C2 1.6322(18) . ? C1 B5 1.7112(18) . ? C1 B4 1.7149(17) . ? C1 B6 1.7276(19) . ? C1 B3 1.7386(18) . ? C2 B7 1.702(2) . ? C2 B11 1.7054(18) . ? C2 B3 1.7235(18) . ? C2 B6 1.7337(18) . ? C4 C6 1.511(2) . ? C4 C5 1.5211(19) . ? C4 H4A 0.986(17) . ? C5 H5C 0.98(2) . ? C5 H5B 0.941(19) . ? C5 H5A 0.98(2) . ? C6 H6C 0.99(2) . ? C6 H6B 0.94(2) . ? C6 H6A 1.00(2) . ? C7 C9 1.517(2) . ? C7 C8 1.521(2) . ? C7 H7A 0.943(18) . ? C8 H8C 0.97(2) . ? C8 H8B 0.97(2) . ? C8 H8A 0.99(2) . ? C9 H9C 0.980(19) . ? C9 H9B 0.98(2) . ? C9 H9A 0.93(2) . ? C10 C11 1.3906(18) . ? C10 C15 1.3943(19) . ? C11 C12 1.385(2) . ? C11 H11A 0.963(19) . ? C12 C13 1.387(2) . ? C12 H12A 0.970(19) . ? C13 C14 1.384(2) . ? C13 H13A 0.98(2) . ? C14 C15 1.3837(19) . ? C14 H14A 0.944(19) . ? C15 H15A 0.986(18) . ? B3 B10 1.751(2) . ? B3 B11 1.771(2) . ? B3 B4 1.773(2) . ? B3 H3 1.084(16) . ? B4 B9 1.770(2) . ? B4 B10 1.781(2) . ? B4 B5 1.788(2) . ? B4 H4 1.058(16) . ? B5 B9 1.775(2) . ? B5 B6 1.775(2) . ? B5 B8 1.776(2) . ? B5 H5 1.045(16) . ? B6 B8 1.755(2) . ? B6 B7 1.780(2) . ? B6 H6 1.067(15) . ? B7 B12 1.780(2) . ? B7 B11 1.782(2) . ? B7 B8 1.785(2) . ? B7 H7 1.091(16) . ? B8 B12 1.781(2) . ? B8 B9 1.782(2) . ? B8 H8 1.078(16) . ? B9 B12 1.778(2) . ? B9 B10 1.783(2) . ? B9 H9 1.093(16) . ? B10 B11 1.784(2) . ? B10 B12 1.787(2) . ? B10 H10 1.060(16) . ? B11 B12 1.777(2) . ? B11 H11 1.063(16) . ? B12 H12 1.081(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 N1 P C10 105.30(6) . . ? N1 P C2 90.99(5) . . ? C10 P C2 101.29(6) . . ? C3 N1 C4 116.43(11) . . ? C3 N1 P 121.18(9) . . ? C4 N1 P 118.27(8) . . ? C3 N2 C7 124.26(11) . . ? C3 C1 C2 108.80(9) . . ? C3 C1 B5 129.54(10) . . ? C2 C1 B5 111.25(10) . . ? C3 C1 B4 126.58(10) . . ? C2 C1 B4 110.78(9) . . ? B5 C1 B4 62.91(8) . . ? C3 C1 B6 115.35(10) . . ? C2 C1 B6 62.05(8) . . ? B5 C1 B6 62.15(8) . . ? B4 C1 B6 114.31(10) . . ? C3 C1 B3 111.57(9) . . ? C2 C1 B3 61.40(7) . . ? B5 C1 B3 113.93(9) . . ? B4 C1 B3 61.79(8) . . ? B6 C1 B3 114.65(10) . . ? C1 C2 B7 111.83(10) . . ? C1 C2 B11 112.13(9) . . ? B7 C2 B11 63.09(8) . . ? C1 C2 B3 62.34(8) . . ? B7 C2 B3 114.64(10) . . ? B11 C2 B3 62.20(9) . . ? C1 C2 B6 61.67(7) . . ? B7 C2 B6 62.41(8) . . ? B11 C2 B6 114.81(10) . . ? B3 C2 B6 115.11(9) . . ? C1 C2 P 108.62(8) . . ? B7 C2 P 130.28(9) . . ? B11 C2 P 124.10(8) . . ? B3 C2 P 109.06(8) . . ? B6 C2 P 117.60(8) . . ? N2 C3 N1 120.05(11) . . ? N2 C3 C1 129.54(11) . . ? N1 C3 C1 110.31(10) . . ? N1 C4 C6 110.50(11) . . ? N1 C4 C5 111.25(12) . . ? C6 C4 C5 111.72(13) . . ? N1 C4 H4A 105.8(9) . . ? C6 C4 H4A 108.9(9) . . ? C5 C4 H4A 108.5(9) . . ? C4 C5 H5C 108.9(11) . . ? C4 C5 H5B 112.7(11) . . ? H5C C5 H5B 109.6(16) . . ? C4 C5 H5A 112.1(12) . . ? H5C C5 H5A 105.8(17) . . ? H5B C5 H5A 107.5(17) . . ? C4 C6 H6C 110.6(11) . . ? C4 C6 H6B 110.2(11) . . ? H6C C6 H6B 109.3(16) . . ? C4 C6 H6A 109.8(11) . . ? H6C C6 H6A 108.0(16) . . ? H6B C6 H6A 108.9(16) . . ? N2 C7 C9 108.25(11) . . ? N2 C7 C8 107.99(12) . . ? C9 C7 C8 111.31(13) . . ? N2 C7 H7A 113.2(10) . . ? C9 C7 H7A 108.1(10) . . ? C8 C7 H7A 108.0(10) . . ? C7 C8 H8C 109.1(12) . . ? C7 C8 H8B 109.5(12) . . ? H8C C8 H8B 108.7(17) . . ? C7 C8 H8A 111.0(13) . . ? H8C C8 H8A 110.6(18) . . ? H8B C8 H8A 107.8(17) . . ? C7 C9 H9C 109.2(11) . . ? C7 C9 H9B 110.1(11) . . ? H9C C9 H9B 108.8(16) . . ? C7 C9 H9A 110.0(13) . . ? H9C C9 H9A 108.7(17) . . ? H9B C9 H9A 110.0(17) . . ? C11 C10 C15 119.33(12) . . ? C11 C10 P 125.55(10) . . ? C15 C10 P 115.06(10) . . ? C12 C11 C10 120.01(13) . . ? C12 C11 H11A 120.1(11) . . ? C10 C11 H11A 119.9(11) . . ? C11 C12 C13 120.36(14) . . ? C11 C12 H12A 118.6(11) . . ? C13 C12 H12A 121.0(11) . . ? C14 C13 C12 119.86(13) . . ? C14 C13 H13A 120.7(12) . . ? C12 C13 H13A 119.5(12) . . ? C13 C14 C15 120.01(14) . . ? C13 C14 H14A 120.4(11) . . ? C15 C14 H14A 119.6(11) . . ? C14 C15 C10 120.41(13) . . ? C14 C15 H15A 121.8(10) . . ? C10 C15 H15A 117.8(10) . . ? C2 B3 C1 56.26(7) . . ? C2 B3 B10 104.96(10) . . ? C1 B3 B10 105.08(9) . . ? C2 B3 B11 58.40(8) . . ? C1 B3 B11 104.19(9) . . ? B10 B3 B11 60.85(9) . . ? C2 B3 B4 103.97(9) . . ? C1 B3 B4 58.45(7) . . ? B10 B3 B4 60.70(8) . . ? B11 B3 B4 108.85(11) . . ? C2 B3 H3 115.6(8) . . ? C1 B3 H3 115.0(9) . . ? B10 B3 H3 133.9(8) . . ? B11 B3 H3 124.9(8) . . ? B4 B3 H3 124.1(8) . . ? C1 B4 B9 104.22(10) . . ? C1 B4 B3 59.76(7) . . ? B9 B4 B3 107.42(11) . . ? C1 B4 B10 104.79(10) . . ? B9 B4 B10 60.27(9) . . ? B3 B4 B10 59.02(8) . . ? C1 B4 B5 58.44(7) . . ? B9 B4 B5 59.84(8) . . ? B3 B4 B5 108.60(9) . . ? B10 B4 B5 108.31(11) . . ? C1 B4 H4 117.8(9) . . ? B9 B4 H4 129.6(9) . . ? B3 B4 H4 116.9(8) . . ? B10 B4 H4 126.3(9) . . ? B5 B4 H4 121.1(8) . . ? C1 B5 B9 104.17(9) . . ? C1 B5 B6 59.38(7) . . ? B9 B5 B6 107.72(10) . . ? C1 B5 B8 104.41(9) . . ? B9 B5 B8 60.25(8) . . ? B6 B5 B8 59.25(9) . . ? C1 B5 B4 58.65(7) . . ? B9 B5 B4 59.57(8) . . ? B6 B5 B4 108.53(9) . . ? B8 B5 B4 107.91(10) . . ? C1 B5 H5 118.6(9) . . ? B9 B5 H5 128.5(9) . . ? B6 B5 H5 117.8(8) . . ? B8 B5 H5 126.5(9) . . ? B4 B5 H5 120.7(9) . . ? C1 B6 C2 56.27(7) . . ? C1 B6 B8 104.60(9) . . ? C2 B6 B8 104.14(9) . . ? C1 B6 B5 58.47(8) . . ? C2 B6 B5 103.73(9) . . ? B8 B6 B5 60.40(9) . . ? C1 B6 B7 103.84(10) . . ? C2 B6 B7 57.91(8) . . ? B8 B6 B7 60.65(8) . . ? B5 B6 B7 108.51(10) . . ? C1 B6 H6 117.3(9) . . ? C2 B6 H6 118.0(8) . . ? B8 B6 H6 131.8(8) . . ? B5 B6 H6 124.0(8) . . ? B7 B6 H6 124.5(8) . . ? C2 B7 B6 59.68(8) . . ? C2 B7 B12 104.07(10) . . ? B6 B7 B12 107.46(10) . . ? C2 B7 B11 58.56(8) . . ? B6 B7 B11 108.85(10) . . ? B12 B7 B11 59.85(8) . . ? C2 B7 B8 104.22(10) . . ? B6 B7 B8 58.99(8) . . ? B12 B7 B8 59.95(8) . . ? B11 B7 B8 107.94(10) . . ? C2 B7 H7 117.1(9) . . ? B6 B7 H7 117.5(8) . . ? B12 B7 H7 129.7(9) . . ? B11 B7 H7 119.6(8) . . ? B8 B7 H7 128.2(8) . . ? B6 B8 B5 60.34(8) . . ? B6 B8 B12 108.50(10) . . ? B5 B8 B12 108.00(10) . . ? B6 B8 B9 108.26(10) . . ? B5 B8 B9 59.84(8) . . ? B12 B8 B9 59.86(8) . . ? B6 B8 B7 60.36(8) . . ? B5 B8 B7 108.23(10) . . ? B12 B8 B7 59.89(8) . . ? B9 B8 B7 107.70(10) . . ? B6 B8 H8 118.5(9) . . ? B5 B8 H8 119.8(9) . . ? B12 B8 H8 124.5(9) . . ? B9 B8 H8 123.4(8) . . ? B7 B8 H8 121.9(8) . . ? B4 B9 B5 60.59(8) . . ? B4 B9 B12 108.33(10) . . ? B5 B9 B12 108.20(10) . . ? B4 B9 B8 108.44(10) . . ? B5 B9 B8 59.91(9) . . ? B12 B9 B8 60.04(9) . . ? B4 B9 B10 60.17(9) . . ? B5 B9 B10 108.82(10) . . ? B12 B9 B10 60.27(9) . . ? B8 B9 B10 108.53(10) . . ? B4 B9 H9 120.2(9) . . ? B5 B9 H9 119.9(9) . . ? B12 B9 H9 123.3(9) . . ? B8 B9 H9 121.8(8) . . ? B10 B9 H9 122.0(8) . . ? B3 B10 B4 60.28(8) . . ? B3 B10 B9 107.85(10) . . ? B4 B10 B9 59.56(8) . . ? B3 B10 B11 60.14(9) . . ? B4 B10 B11 107.96(10) . . ? B9 B10 B11 107.49(10) . . ? B3 B10 B12 107.86(10) . . ? B4 B10 B12 107.42(10) . . ? B9 B10 B12 59.74(9) . . ? B11 B10 B12 59.70(9) . . ? B3 B10 H10 119.0(9) . . ? B4 B10 H10 121.1(9) . . ? B9 B10 H10 124.2(9) . . ? B11 B10 H10 121.0(9) . . ? B12 B10 H10 124.1(9) . . ? C2 B11 B3 59.40(8) . . ? C2 B11 B12 104.02(10) . . ? B3 B11 B12 107.41(10) . . ? C2 B11 B7 58.35(8) . . ? B3 B11 B7 108.43(10) . . ? B12 B11 B7 60.01(8) . . ? C2 B11 B10 104.31(10) . . ? B3 B11 B10 59.01(9) . . ? B12 B11 B10 60.26(9) . . ? B7 B11 B10 108.34(10) . . ? C2 B11 H11 117.0(9) . . ? B3 B11 H11 117.5(9) . . ? B12 B11 H11 129.9(9) . . ? B7 B11 H11 119.7(9) . . ? B10 B11 H11 127.8(9) . . ? B11 B12 B9 107.97(11) . . ? B11 B12 B7 60.14(8) . . ? B9 B12 B7 108.10(10) . . ? B11 B12 B8 108.34(10) . . ? B9 B12 B8 60.09(8) . . ? B7 B12 B8 60.17(8) . . ? B11 B12 B10 60.05(8) . . ? B9 B12 B10 60.00(9) . . ? B7 B12 B10 108.28(10) . . ? B8 B12 B10 108.36(11) . . ? B11 B12 H12 120.7(9) . . ? B9 B12 H12 123.9(9) . . ? B7 B12 H12 119.0(9) . . ? B8 B12 H12 120.8(9) . . ? B10 B12 H12 123.5(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 P N1 C3 -104.62(10) . . . . ? C2 P N1 C3 -2.63(10) . . . . ? C10 P N1 C4 99.01(10) . . . . ? C2 P N1 C4 -159.00(10) . . . . ? C3 C1 C2 B7 147.84(10) . . . . ? B5 C1 C2 B7 -0.82(13) . . . . ? B4 C1 C2 B7 -68.79(12) . . . . ? B6 C1 C2 B7 38.49(9) . . . . ? B3 C1 C2 B7 -107.29(11) . . . . ? C3 C1 C2 B11 -143.47(10) . . . . ? B5 C1 C2 B11 67.87(12) . . . . ? B4 C1 C2 B11 -0.10(13) . . . . ? B6 C1 C2 B11 107.18(11) . . . . ? B3 C1 C2 B11 -38.60(10) . . . . ? C3 C1 C2 B3 -104.87(10) . . . . ? B5 C1 C2 B3 106.48(10) . . . . ? B4 C1 C2 B3 38.50(9) . . . . ? B6 C1 C2 B3 145.78(10) . . . . ? C3 C1 C2 B6 109.35(10) . . . . ? B5 C1 C2 B6 -39.31(9) . . . . ? B4 C1 C2 B6 -107.28(10) . . . . ? B3 C1 C2 B6 -145.78(10) . . . . ? C3 C1 C2 P -2.60(11) . . . . ? B5 C1 C2 P -151.26(8) . . . . ? B4 C1 C2 P 140.77(8) . . . . ? B6 C1 C2 P -111.95(9) . . . . ? B3 C1 C2 P 102.27(9) . . . . ? N1 P C2 C1 2.80(8) . . . . ? C10 P C2 C1 108.61(8) . . . . ? N1 P C2 B7 -140.31(11) . . . . ? C10 P C2 B7 -34.50(12) . . . . ? N1 P C2 B11 137.89(10) . . . . ? C10 P C2 B11 -116.30(11) . . . . ? N1 P C2 B3 69.10(9) . . . . ? C10 P C2 B3 174.92(8) . . . . ? N1 P C2 B6 -64.32(9) . . . . ? C10 P C2 B6 41.49(10) . . . . ? C7 N2 C3 N1 177.62(11) . . . . ? C7 N2 C3 C1 1.6(2) . . . . ? C4 N1 C3 N2 -18.58(17) . . . . ? P N1 C3 N2 -175.37(10) . . . . ? C4 N1 C3 C1 158.17(10) . . . . ? P N1 C3 C1 1.38(14) . . . . ? C2 C1 C3 N2 177.30(13) . . . . ? B5 C1 C3 N2 -41.7(2) . . . . ? B4 C1 C3 N2 41.3(2) . . . . ? B6 C1 C3 N2 -115.44(14) . . . . ? B3 C1 C3 N2 111.45(14) . . . . ? C2 C1 C3 N1 0.95(13) . . . . ? B5 C1 C3 N1 141.99(11) . . . . ? B4 C1 C3 N1 -135.05(11) . . . . ? B6 C1 C3 N1 68.21(13) . . . . ? B3 C1 C3 N1 -64.90(12) . . . . ? C3 N1 C4 C6 -75.70(14) . . . . ? P N1 C4 C6 81.79(13) . . . . ? C3 N1 C4 C5 159.61(12) . . . . ? P N1 C4 C5 -42.90(15) . . . . ? C3 N2 C7 C9 121.20(15) . . . . ? C3 N2 C7 C8 -118.17(15) . . . . ? N1 P C10 C11 -0.74(13) . . . . ? C2 P C10 C11 -94.92(12) . . . . ? N1 P C10 C15 -177.99(9) . . . . ? C2 P C10 C15 87.84(10) . . . . ? C15 C10 C11 C12 -0.5(2) . . . . ? P C10 C11 C12 -177.62(11) . . . . ? C10 C11 C12 C13 -0.6(2) . . . . ? C11 C12 C13 C14 0.9(2) . . . . ? C12 C13 C14 C15 -0.1(2) . . . . ? C13 C14 C15 C10 -1.0(2) . . . . ? C11 C10 C15 C14 1.3(2) . . . . ? P C10 C15 C14 178.70(11) . . . . ? B7 C2 B3 C1 102.79(11) . . . . ? B11 C2 B3 C1 139.20(10) . . . . ? B6 C2 B3 C1 33.14(10) . . . . ? P C2 B3 C1 -101.56(9) . . . . ? C1 C2 B3 B10 -98.35(10) . . . . ? B7 C2 B3 B10 4.44(13) . . . . ? B11 C2 B3 B10 40.85(9) . . . . ? B6 C2 B3 B10 -65.22(12) . . . . ? P C2 B3 B10 160.09(8) . . . . ? C1 C2 B3 B11 -139.20(10) . . . . ? B7 C2 B3 B11 -36.42(10) . . . . ? B6 C2 B3 B11 -106.07(11) . . . . ? P C2 B3 B11 119.24(9) . . . . ? C1 C2 B3 B4 -35.45(9) . . . . ? B7 C2 B3 B4 67.34(12) . . . . ? B11 C2 B3 B4 103.76(11) . . . . ? B6 C2 B3 B4 -2.31(13) . . . . ? P C2 B3 B4 -137.01(8) . . . . ? C3 C1 B3 C2 100.33(10) . . . . ? B5 C1 B3 C2 -102.11(11) . . . . ? B4 C1 B3 C2 -138.67(10) . . . . ? B6 C1 B3 C2 -33.13(9) . . . . ? C3 C1 B3 B10 -161.53(10) . . . . ? C2 C1 B3 B10 98.14(11) . . . . ? B5 C1 B3 B10 -3.97(13) . . . . ? B4 C1 B3 B10 -40.53(10) . . . . ? B6 C1 B3 B10 65.01(12) . . . . ? C3 C1 B3 B11 135.35(10) . . . . ? C2 C1 B3 B11 35.03(9) . . . . ? B5 C1 B3 B11 -67.08(12) . . . . ? B4 C1 B3 B11 -103.64(11) . . . . ? B6 C1 B3 B11 1.90(12) . . . . ? C3 C1 B3 B4 -121.01(11) . . . . ? C2 C1 B3 B4 138.67(10) . . . . ? B5 C1 B3 B4 36.56(10) . . . . ? B6 C1 B3 B4 105.53(11) . . . . ? C3 C1 B4 B9 -160.92(11) . . . . ? C2 C1 B4 B9 63.78(12) . . . . ? B5 C1 B4 B9 -40.19(9) . . . . ? B6 C1 B4 B9 -3.98(12) . . . . ? B3 C1 B4 B9 102.11(11) . . . . ? C3 C1 B4 B3 96.97(13) . . . . ? C2 C1 B4 B3 -38.33(9) . . . . ? B5 C1 B4 B3 -142.30(10) . . . . ? B6 C1 B4 B3 -106.09(11) . . . . ? C3 C1 B4 B10 136.61(12) . . . . ? C2 C1 B4 B10 1.31(12) . . . . ? B5 C1 B4 B10 -102.66(11) . . . . ? B6 C1 B4 B10 -66.45(12) . . . . ? B3 C1 B4 B10 39.64(9) . . . . ? C3 C1 B4 B5 -120.73(13) . . . . ? C2 C1 B4 B5 103.97(10) . . . . ? B6 C1 B4 B5 36.22(10) . . . . ? B3 C1 B4 B5 142.30(10) . . . . ? C2 B3 B4 C1 34.47(9) . . . . ? B10 B3 B4 C1 133.99(10) . . . . ? B11 B3 B4 C1 95.41(10) . . . . ? C2 B3 B4 B9 -62.15(12) . . . . ? C1 B3 B4 B9 -96.61(10) . . . . ? B10 B3 B4 B9 37.38(10) . . . . ? B11 B3 B4 B9 -1.20(13) . . . . ? C2 B3 B4 B10 -99.52(11) . . . . ? C1 B3 B4 B10 -133.99(10) . . . . ? B11 B3 B4 B10 -38.58(9) . . . . ? C2 B3 B4 B5 1.12(13) . . . . ? C1 B3 B4 B5 -33.35(9) . . . . ? B10 B3 B4 B5 100.64(11) . . . . ? B11 B3 B4 B5 62.06(12) . . . . ? C3 C1 B5 B9 156.52(11) . . . . ? C2 C1 B5 B9 -63.17(11) . . . . ? B4 C1 B5 B9 40.05(9) . . . . ? B6 C1 B5 B9 -102.44(11) . . . . ? B3 C1 B5 B9 3.92(13) . . . . ? C3 C1 B5 B6 -101.05(13) . . . . ? C2 C1 B5 B6 39.27(9) . . . . ? B4 C1 B5 B6 142.48(10) . . . . ? B3 C1 B5 B6 106.36(11) . . . . ? C3 C1 B5 B8 -141.10(12) . . . . ? C2 C1 B5 B8 -0.79(12) . . . . ? B4 C1 B5 B8 102.43(10) . . . . ? B6 C1 B5 B8 -40.05(9) . . . . ? B3 C1 B5 B8 66.31(12) . . . . ? C3 C1 B5 B4 116.47(13) . . . . ? C2 C1 B5 B4 -103.22(10) . . . . ? B6 C1 B5 B4 -142.48(10) . . . . ? B3 C1 B5 B4 -36.13(10) . . . . ? B9 B4 B5 C1 133.66(10) . . . . ? B3 B4 B5 C1 33.88(9) . . . . ? B10 B4 B5 C1 96.44(10) . . . . ? C1 B4 B5 B9 -133.66(10) . . . . ? B3 B4 B5 B9 -99.78(11) . . . . ? B10 B4 B5 B9 -37.21(9) . . . . ? C1 B4 B5 B6 -33.56(9) . . . . ? B9 B4 B5 B6 100.10(11) . . . . ? B3 B4 B5 B6 0.32(13) . . . . ? B10 B4 B5 B6 62.89(12) . . . . ? C1 B4 B5 B8 -96.28(10) . . . . ? B9 B4 B5 B8 37.38(9) . . . . ? B3 B4 B5 B8 -62.40(13) . . . . ? B10 B4 B5 B8 0.16(12) . . . . ? C3 C1 B6 C2 -98.77(10) . . . . ? B5 C1 B6 C2 138.10(10) . . . . ? B4 C1 B6 C2 101.60(10) . . . . ? B3 C1 B6 C2 32.90(9) . . . . ? C3 C1 B6 B8 163.79(10) . . . . ? C2 C1 B6 B8 -97.44(10) . . . . ? B5 C1 B6 B8 40.66(9) . . . . ? B4 C1 B6 B8 4.15(12) . . . . ? B3 C1 B6 B8 -64.54(12) . . . . ? C3 C1 B6 B5 123.13(11) . . . . ? C2 C1 B6 B5 -138.10(10) . . . . ? B4 C1 B6 B5 -36.51(9) . . . . ? B3 C1 B6 B5 -105.20(11) . . . . ? C3 C1 B6 B7 -133.44(10) . . . . ? C2 C1 B6 B7 -34.67(9) . . . . ? B5 C1 B6 B7 103.43(10) . . . . ? B4 C1 B6 B7 66.93(12) . . . . ? B3 C1 B6 B7 -1.77(12) . . . . ? B7 C2 B6 C1 -139.31(10) . . . . ? B11 C2 B6 C1 -102.84(11) . . . . ? B3 C2 B6 C1 -33.37(10) . . . . ? P C2 B6 C1 97.33(9) . . . . ? C1 C2 B6 B8 98.30(10) . . . . ? B7 C2 B6 B8 -41.01(9) . . . . ? B11 C2 B6 B8 -4.54(13) . . . . ? B3 C2 B6 B8 64.93(13) . . . . ? P C2 B6 B8 -164.37(8) . . . . ? C1 C2 B6 B5 35.87(9) . . . . ? B7 C2 B6 B5 -103.44(11) . . . . ? B11 C2 B6 B5 -66.97(13) . . . . ? B3 C2 B6 B5 2.50(13) . . . . ? P C2 B6 B5 133.20(9) . . . . ? C1 C2 B6 B7 139.31(10) . . . . ? B11 C2 B6 B7 36.47(10) . . . . ? B3 C2 B6 B7 105.94(12) . . . . ? P C2 B6 B7 -123.36(10) . . . . ? B9 B5 B6 C1 96.29(10) . . . . ? B8 B5 B6 C1 133.52(10) . . . . ? B4 B5 B6 C1 33.26(9) . . . . ? C1 B5 B6 C2 -34.87(8) . . . . ? B9 B5 B6 C2 61.42(12) . . . . ? B8 B5 B6 C2 98.65(10) . . . . ? B4 B5 B6 C2 -1.60(13) . . . . ? C1 B5 B6 B8 -133.52(10) . . . . ? B9 B5 B6 B8 -37.23(9) . . . . ? B4 B5 B6 B8 -100.25(11) . . . . ? C1 B5 B6 B7 -95.20(10) . . . . ? B9 B5 B6 B7 1.08(13) . . . . ? B8 B5 B6 B7 38.31(9) . . . . ? B4 B5 B6 B7 -61.94(12) . . . . ? C1 C2 B7 B6 -38.18(9) . . . . ? B11 C2 B7 B6 -142.76(10) . . . . ? B3 C2 B7 B6 -106.69(10) . . . . ? P C2 B7 B6 104.03(11) . . . . ? C1 C2 B7 B12 64.04(12) . . . . ? B11 C2 B7 B12 -40.54(9) . . . . ? B3 C2 B7 B12 -4.46(13) . . . . ? B6 C2 B7 B12 102.22(10) . . . . ? P C2 B7 B12 -153.75(9) . . . . ? C1 C2 B7 B11 104.58(10) . . . . ? B3 C2 B7 B11 36.08(10) . . . . ? B6 C2 B7 B11 142.76(10) . . . . ? P C2 B7 B11 -113.21(11) . . . . ? C1 C2 B7 B8 2.02(12) . . . . ? B11 C2 B7 B8 -102.56(10) . . . . ? B3 C2 B7 B8 -66.48(12) . . . . ? B6 C2 B7 B8 40.20(9) . . . . ? P C2 B7 B8 144.23(10) . . . . ? C1 B6 B7 C2 33.95(8) . . . . ? B8 B6 B7 C2 133.11(10) . . . . ? B5 B6 B7 C2 94.91(10) . . . . ? C1 B6 B7 B12 -62.44(12) . . . . ? C2 B6 B7 B12 -96.39(11) . . . . ? B8 B6 B7 B12 36.72(10) . . . . ? B5 B6 B7 B12 -1.48(13) . . . . ? C1 B6 B7 B11 0.89(12) . . . . ? C2 B6 B7 B11 -33.06(9) . . . . ? B8 B6 B7 B11 100.05(11) . . . . ? B5 B6 B7 B11 61.85(12) . . . . ? C1 B6 B7 B8 -99.16(10) . . . . ? C2 B6 B7 B8 -133.11(10) . . . . ? B5 B6 B7 B8 -38.20(9) . . . . ? C1 B6 B8 B5 -39.70(9) . . . . ? C2 B6 B8 B5 -97.96(10) . . . . ? B7 B6 B8 B5 -137.59(10) . . . . ? C1 B6 B8 B12 60.93(12) . . . . ? C2 B6 B8 B12 2.67(13) . . . . ? B5 B6 B8 B12 100.63(11) . . . . ? B7 B6 B8 B12 -36.95(10) . . . . ? C1 B6 B8 B9 -2.51(12) . . . . ? C2 B6 B8 B9 -60.77(12) . . . . ? B5 B6 B8 B9 37.19(9) . . . . ? B7 B6 B8 B9 -100.40(11) . . . . ? C1 B6 B8 B7 97.89(10) . . . . ? C2 B6 B8 B7 39.63(9) . . . . ? B5 B6 B8 B7 137.59(10) . . . . ? C1 B5 B8 B6 40.12(9) . . . . ? B9 B5 B8 B6 138.41(10) . . . . ? B4 B5 B8 B6 101.33(10) . . . . ? C1 B5 B8 B12 -61.36(12) . . . . ? B9 B5 B8 B12 36.93(9) . . . . ? B6 B5 B8 B12 -101.48(10) . . . . ? B4 B5 B8 B12 -0.15(13) . . . . ? C1 B5 B8 B9 -98.29(10) . . . . ? B6 B5 B8 B9 -138.41(10) . . . . ? B4 B5 B8 B9 -37.08(9) . . . . ? C1 B5 B8 B7 2.00(12) . . . . ? B9 B5 B8 B7 100.30(11) . . . . ? B6 B5 B8 B7 -38.11(9) . . . . ? B4 B5 B8 B7 63.22(12) . . . . ? C2 B7 B8 B6 -40.55(9) . . . . ? B12 B7 B8 B6 -138.77(11) . . . . ? B11 B7 B8 B6 -101.64(11) . . . . ? C2 B7 B8 B5 -2.44(13) . . . . ? B6 B7 B8 B5 38.11(9) . . . . ? B12 B7 B8 B5 -100.67(11) . . . . ? B11 B7 B8 B5 -63.53(12) . . . . ? C2 B7 B8 B12 98.22(11) . . . . ? B6 B7 B8 B12 138.77(11) . . . . ? B11 B7 B8 B12 37.14(10) . . . . ? C2 B7 B8 B9 60.81(12) . . . . ? B6 B7 B8 B9 101.36(11) . . . . ? B12 B7 B8 B9 -37.42(10) . . . . ? B11 B7 B8 B9 -0.28(13) . . . . ? C1 B4 B9 B5 39.49(8) . . . . ? B3 B4 B9 B5 101.78(10) . . . . ? B10 B4 B9 B5 138.61(10) . . . . ? C1 B4 B9 B12 -61.51(12) . . . . ? B3 B4 B9 B12 0.78(13) . . . . ? B10 B4 B9 B12 37.61(9) . . . . ? B5 B4 B9 B12 -101.00(11) . . . . ? C1 B4 B9 B8 2.13(12) . . . . ? B3 B4 B9 B8 64.42(12) . . . . ? B10 B4 B9 B8 101.25(11) . . . . ? B5 B4 B9 B8 -37.36(9) . . . . ? C1 B4 B9 B10 -99.12(10) . . . . ? B3 B4 B9 B10 -36.82(9) . . . . ? B5 B4 B9 B10 -138.61(10) . . . . ? C1 B5 B9 B4 -39.58(9) . . . . ? B6 B5 B9 B4 -101.50(10) . . . . ? B8 B5 B9 B4 -138.29(10) . . . . ? C1 B5 B9 B12 61.65(12) . . . . ? B6 B5 B9 B12 -0.26(13) . . . . ? B8 B5 B9 B12 -37.06(10) . . . . ? B4 B5 B9 B12 101.23(11) . . . . ? C1 B5 B9 B8 98.71(10) . . . . ? B6 B5 B9 B8 36.79(9) . . . . ? B4 B5 B9 B8 138.29(10) . . . . ? C1 B5 B9 B10 -2.28(13) . . . . ? B6 B5 B9 B10 -64.19(13) . . . . ? B8 B5 B9 B10 -100.99(11) . . . . ? B4 B5 B9 B10 37.30(10) . . . . ? B6 B8 B9 B4 0.25(13) . . . . ? B5 B8 B9 B4 37.66(9) . . . . ? B12 B8 B9 B4 -100.98(11) . . . . ? B7 B8 B9 B4 -63.55(12) . . . . ? B6 B8 B9 B5 -37.41(9) . . . . ? B12 B8 B9 B5 -138.64(10) . . . . ? B7 B8 B9 B5 -101.21(11) . . . . ? B6 B8 B9 B12 101.24(11) . . . . ? B5 B8 B9 B12 138.64(10) . . . . ? B7 B8 B9 B12 37.43(10) . . . . ? B6 B8 B9 B10 64.07(13) . . . . ? B5 B8 B9 B10 101.48(11) . . . . ? B12 B8 B9 B10 -37.16(10) . . . . ? B7 B8 B9 B10 0.27(14) . . . . ? C2 B3 B10 B4 97.85(10) . . . . ? C1 B3 B10 B4 39.42(9) . . . . ? B11 B3 B10 B4 137.49(10) . . . . ? C2 B3 B10 B9 60.68(12) . . . . ? C1 B3 B10 B9 2.25(13) . . . . ? B11 B3 B10 B9 100.32(11) . . . . ? B4 B3 B10 B9 -37.17(10) . . . . ? C2 B3 B10 B11 -39.64(9) . . . . ? C1 B3 B10 B11 -98.07(10) . . . . ? B4 B3 B10 B11 -137.49(10) . . . . ? C2 B3 B10 B12 -2.41(12) . . . . ? C1 B3 B10 B12 -60.85(12) . . . . ? B11 B3 B10 B12 37.22(9) . . . . ? B4 B3 B10 B12 -100.26(11) . . . . ? C1 B4 B10 B3 -40.00(9) . . . . ? B9 B4 B10 B3 -138.16(10) . . . . ? B5 B4 B10 B3 -101.13(10) . . . . ? C1 B4 B10 B9 98.16(10) . . . . ? B3 B4 B10 B9 138.16(10) . . . . ? B5 B4 B10 B9 37.03(9) . . . . ? C1 B4 B10 B11 -1.97(13) . . . . ? B9 B4 B10 B11 -100.13(11) . . . . ? B3 B4 B10 B11 38.03(9) . . . . ? B5 B4 B10 B11 -63.10(12) . . . . ? C1 B4 B10 B12 61.01(12) . . . . ? B9 B4 B10 B12 -37.15(9) . . . . ? B3 B4 B10 B12 101.02(10) . . . . ? B5 B4 B10 B12 -0.12(12) . . . . ? B4 B9 B10 B3 37.48(10) . . . . ? B5 B9 B10 B3 0.00(14) . . . . ? B12 B9 B10 B3 -100.67(11) . . . . ? B8 B9 B10 B3 -63.61(13) . . . . ? B5 B9 B10 B4 -37.48(10) . . . . ? B12 B9 B10 B4 -138.16(10) . . . . ? B8 B9 B10 B4 -101.10(11) . . . . ? B4 B9 B10 B11 100.94(11) . . . . ? B5 B9 B10 B11 63.46(13) . . . . ? B12 B9 B10 B11 -37.22(10) . . . . ? B8 B9 B10 B11 -0.15(14) . . . . ? B4 B9 B10 B12 138.16(10) . . . . ? B5 B9 B10 B12 100.68(11) . . . . ? B8 B9 B10 B12 37.06(10) . . . . ? C1 C2 B11 B3 38.66(9) . . . . ? B7 C2 B11 B3 142.76(10) . . . . ? B6 C2 B11 B3 106.55(10) . . . . ? P C2 B11 B3 -95.10(10) . . . . ? C1 C2 B11 B12 -63.50(12) . . . . ? B7 C2 B11 B12 40.61(9) . . . . ? B3 C2 B11 B12 -102.16(10) . . . . ? B6 C2 B11 B12 4.39(13) . . . . ? P C2 B11 B12 162.74(9) . . . . ? C1 C2 B11 B7 -104.11(11) . . . . ? B3 C2 B11 B7 -142.76(10) . . . . ? B6 C2 B11 B7 -36.21(10) . . . . ? P C2 B11 B7 122.14(11) . . . . ? C1 C2 B11 B10 -1.14(13) . . . . ? B7 C2 B11 B10 102.96(11) . . . . ? B3 C2 B11 B10 -39.80(9) . . . . ? B6 C2 B11 B10 66.75(12) . . . . ? P C2 B11 B10 -134.90(9) . . . . ? C1 B3 B11 C2 -34.08(8) . . . . ? B10 B3 B11 C2 -133.65(10) . . . . ? B4 B3 B11 C2 -95.13(10) . . . . ? C2 B3 B11 B12 96.29(10) . . . . ? C1 B3 B11 B12 62.21(11) . . . . ? B10 B3 B11 B12 -37.36(9) . . . . ? B4 B3 B11 B12 1.16(13) . . . . ? C2 B3 B11 B7 32.88(9) . . . . ? C1 B3 B11 B7 -1.20(12) . . . . ? B10 B3 B11 B7 -100.77(11) . . . . ? B4 B3 B11 B7 -62.25(12) . . . . ? C2 B3 B11 B10 133.65(10) . . . . ? C1 B3 B11 B10 99.57(10) . . . . ? B4 B3 B11 B10 38.52(9) . . . . ? B6 B7 B11 C2 33.50(9) . . . . ? B12 B7 B11 C2 133.19(10) . . . . ? B8 B7 B11 C2 96.01(11) . . . . ? C2 B7 B11 B3 -33.30(9) . . . . ? B6 B7 B11 B3 0.20(13) . . . . ? B12 B7 B11 B3 99.89(11) . . . . ? B8 B7 B11 B3 62.71(13) . . . . ? C2 B7 B11 B12 -133.19(10) . . . . ? B6 B7 B11 B12 -99.69(11) . . . . ? B8 B7 B11 B12 -37.18(10) . . . . ? C2 B7 B11 B10 -95.83(11) . . . . ? B6 B7 B11 B10 -62.32(13) . . . . ? B12 B7 B11 B10 37.36(10) . . . . ? B8 B7 B11 B10 0.18(13) . . . . ? B3 B10 B11 C2 40.00(9) . . . . ? B4 B10 B11 C2 1.91(13) . . . . ? B9 B10 B11 C2 -60.94(13) . . . . ? B12 B10 B11 C2 -98.18(10) . . . . ? B4 B10 B11 B3 -38.09(10) . . . . ? B9 B10 B11 B3 -100.94(11) . . . . ? B12 B10 B11 B3 -138.17(10) . . . . ? B3 B10 B11 B12 138.17(10) . . . . ? B4 B10 B11 B12 100.08(11) . . . . ? B9 B10 B11 B12 37.23(10) . . . . ? B3 B10 B11 B7 100.92(11) . . . . ? B4 B10 B11 B7 62.83(13) . . . . ? B9 B10 B11 B7 -0.02(14) . . . . ? B12 B10 B11 B7 -37.25(10) . . . . ? C2 B11 B12 B9 61.20(12) . . . . ? B3 B11 B12 B9 -0.66(13) . . . . ? B7 B11 B12 B9 100.97(11) . . . . ? B10 B11 B12 B9 -37.47(10) . . . . ? C2 B11 B12 B7 -39.77(9) . . . . ? B3 B11 B12 B7 -101.63(11) . . . . ? B10 B11 B12 B7 -138.44(10) . . . . ? C2 B11 B12 B8 -2.40(13) . . . . ? B3 B11 B12 B8 -64.26(12) . . . . ? B7 B11 B12 B8 37.37(10) . . . . ? B10 B11 B12 B8 -101.06(11) . . . . ? C2 B11 B12 B10 98.67(11) . . . . ? B3 B11 B12 B10 36.81(9) . . . . ? B7 B11 B12 B10 138.44(10) . . . . ? B4 B9 B12 B11 -0.08(13) . . . . ? B5 B9 B12 B11 -64.25(13) . . . . ? B8 B9 B12 B11 -101.24(11) . . . . ? B10 B9 B12 B11 37.49(10) . . . . ? B4 B9 B12 B7 63.52(13) . . . . ? B5 B9 B12 B7 -0.65(14) . . . . ? B8 B9 B12 B7 -37.65(10) . . . . ? B10 B9 B12 B7 101.08(11) . . . . ? B4 B9 B12 B8 101.17(11) . . . . ? B5 B9 B12 B8 37.00(10) . . . . ? B10 B9 B12 B8 138.73(10) . . . . ? B4 B9 B12 B10 -37.57(9) . . . . ? B5 B9 B12 B10 -101.74(11) . . . . ? B8 B9 B12 B10 -138.73(10) . . . . ? C2 B7 B12 B11 39.89(9) . . . . ? B6 B7 B12 B11 102.07(11) . . . . ? B8 B7 B12 B11 138.38(11) . . . . ? C2 B7 B12 B9 -60.87(12) . . . . ? B6 B7 B12 B9 1.31(13) . . . . ? B11 B7 B12 B9 -100.76(11) . . . . ? B8 B7 B12 B9 37.62(10) . . . . ? C2 B7 B12 B8 -98.49(11) . . . . ? B6 B7 B12 B8 -36.31(10) . . . . ? B11 B7 B12 B8 -138.38(11) . . . . ? C2 B7 B12 B10 2.64(12) . . . . ? B6 B7 B12 B10 64.81(12) . . . . ? B11 B7 B12 B10 -37.25(10) . . . . ? B8 B7 B12 B10 101.12(11) . . . . ? B6 B8 B12 B11 -0.20(14) . . . . ? B5 B8 B12 B11 63.70(13) . . . . ? B9 B8 B12 B11 100.62(11) . . . . ? B7 B8 B12 B11 -37.36(10) . . . . ? B6 B8 B12 B9 -100.83(11) . . . . ? B5 B8 B12 B9 -36.92(10) . . . . ? B7 B8 B12 B9 -137.99(11) . . . . ? B6 B8 B12 B7 37.16(10) . . . . ? B5 B8 B12 B7 101.06(11) . . . . ? B9 B8 B12 B7 137.99(11) . . . . ? B6 B8 B12 B10 -63.83(12) . . . . ? B5 B8 B12 B10 0.08(13) . . . . ? B9 B8 B12 B10 37.00(10) . . . . ? B7 B8 B12 B10 -100.99(11) . . . . ? B3 B10 B12 B11 -37.42(9) . . . . ? B4 B10 B12 B11 -101.01(11) . . . . ? B9 B10 B12 B11 -138.07(10) . . . . ? B3 B10 B12 B9 100.65(11) . . . . ? B4 B10 B12 B9 37.07(9) . . . . ? B11 B10 B12 B9 138.07(10) . . . . ? B3 B10 B12 B7 -0.13(13) . . . . ? B4 B10 B12 B7 -63.71(12) . . . . ? B9 B10 B12 B7 -100.78(11) . . . . ? B11 B10 B12 B7 37.29(9) . . . . ? B3 B10 B12 B8 63.61(12) . . . . ? B4 B10 B12 B8 0.03(13) . . . . ? B9 B10 B12 B8 -37.04(9) . . . . ? B11 B10 B12 B8 101.03(11) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 29.22 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.367 _refine_diff_density_min -0.271 _refine_diff_density_rms 0.043 _database_code_depnum_ccdc_archive 'CCDC 963129' ####################################################################### # # 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_magd57 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H42 B10 N2 Si' _chemical_formula_weight 530.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 11.8346(15) _cell_length_b 32.995(5) _cell_length_c 9.2931(11) _cell_angle_alpha 90.00 _cell_angle_beta 123.079(17) _cell_angle_gamma 90.00 _cell_volume 3040.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 43025 _cell_measurement_theta_min 4.6515 _cell_measurement_theta_max 75.7424 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.160 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.814 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9158 _exptl_absorpt_correction_T_max 0.9604 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Nova' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3543 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57605 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0127 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 4.66 _diffrn_reflns_theta_max 75.93 _reflns_number_total 6195 _reflns_number_gt 6165 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XP' _computing_publication_material SHELXL-97 _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^)+(0.0520P)^2^+1.0410P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.006(13) _refine_ls_number_reflns 6195 _refine_ls_number_parameters 361 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0276 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0735 _refine_ls_wR_factor_gt 0.0734 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 Si Si 0.98052(3) 0.876267(9) 0.96454(4) 0.01285(7) Uani 1 1 d . . . C1 C 0.73072(11) 0.90656(3) 0.68981(15) 0.0145(2) Uani 1 1 d . . . C2 C 0.88960(11) 0.90168(3) 0.74613(15) 0.0136(2) Uani 1 1 d . . . C3 C 0.71086(12) 0.88552(4) 0.82158(15) 0.0151(2) Uani 1 1 d . . . C4 C 0.81432(12) 0.83618(3) 1.05732(15) 0.0155(2) Uani 1 1 d . . . H4A H 0.7388 0.8456 1.0678 0.019 Uiso 1 1 calc R . . C5 C 0.94063(12) 0.83256(4) 1.23858(15) 0.0180(2) Uani 1 1 d . . . H5A H 0.9611 0.8591 1.2973 0.022 Uiso 1 1 calc R . . H5B H 1.0184 0.8246 1.2321 0.022 Uiso 1 1 calc R . . C6 C 0.91871(13) 0.80076(4) 1.34143(16) 0.0202(2) Uani 1 1 d . . . H6A H 1.0023 0.7979 1.4569 0.024 Uiso 1 1 calc R . . H6B H 0.8460 0.8100 1.3562 0.024 Uiso 1 1 calc R . . C7 C 0.88066(14) 0.75964(4) 1.25102(17) 0.0226(3) Uani 1 1 d . . . H7A H 0.9564 0.7493 1.2447 0.027 Uiso 1 1 calc R . . H7B H 0.8640 0.7400 1.3182 0.027 Uiso 1 1 calc R . . C8 C 0.75450(15) 0.76317(4) 1.06992(18) 0.0259(3) Uani 1 1 d . . . H8A H 0.6766 0.7708 1.0767 0.031 Uiso 1 1 calc R . . H8B H 0.7347 0.7366 1.0115 0.031 Uiso 1 1 calc R . . C9 C 0.77407(13) 0.79502(4) 0.96577(16) 0.0209(3) Uani 1 1 d . . . H9A H 0.6892 0.7980 0.8517 0.025 Uiso 1 1 calc R . . H9B H 0.8450 0.7858 0.9477 0.025 Uiso 1 1 calc R . . C10 C 0.47594(12) 0.90240(4) 0.69818(17) 0.0195(2) Uani 1 1 d . . . H10A H 0.4835 0.9170 0.6095 0.023 Uiso 1 1 calc R . . C11 C 0.36567(13) 0.87001(4) 0.61155(17) 0.0229(3) Uani 1 1 d . . . H11A H 0.2819 0.8826 0.5166 0.027 Uiso 1 1 calc R . . H11B H 0.3939 0.8490 0.5613 0.027 Uiso 1 1 calc R . . C12 C 0.33608(13) 0.84983(4) 0.73548(19) 0.0258(3) Uani 1 1 d . . . H12A H 0.2596 0.8308 0.6713 0.031 Uiso 1 1 calc R . . H12B H 0.4159 0.8341 0.8222 0.031 Uiso 1 1 calc R . . C13 C 0.30168(15) 0.88128(4) 0.8255(2) 0.0278(3) Uani 1 1 d . . . H13A H 0.2864 0.8676 0.9084 0.033 Uiso 1 1 calc R . . H13B H 0.2175 0.8955 0.7398 0.033 Uiso 1 1 calc R . . C14 C 0.41553(14) 0.91202(4) 0.92001(17) 0.0230(3) Uani 1 1 d . . . H14A H 0.4981 0.8981 1.0114 0.028 Uiso 1 1 calc R . . H14B H 0.3903 0.9326 0.9750 0.028 Uiso 1 1 calc R . . C15 C 0.44409(12) 0.93276(4) 0.79629(17) 0.0212(3) Uani 1 1 d . . . H15A H 0.5214 0.9515 0.8617 0.025 Uiso 1 1 calc R . . H15B H 0.3646 0.9491 0.7129 0.025 Uiso 1 1 calc R . . C16 C 1.08367(12) 0.83126(4) 0.98298(16) 0.0161(2) Uani 1 1 d . . . C17 C 1.20494(13) 0.82370(4) 1.13954(17) 0.0219(3) Uani 1 1 d . . . H17 H 1.2341 0.8419 1.2327 0.026 Uiso 1 1 calc R . . C18 C 1.28367(15) 0.78995(5) 1.16116(19) 0.0291(3) Uani 1 1 d . . . H18 H 1.3652 0.7851 1.2687 0.035 Uiso 1 1 calc R . . C19 C 1.24272(16) 0.76347(4) 1.0256(2) 0.0293(3) Uani 1 1 d . . . H19 H 1.2961 0.7404 1.0401 0.035 Uiso 1 1 calc R . . C20 C 1.12372(14) 0.77062(4) 0.86851(19) 0.0262(3) Uani 1 1 d . . . H20 H 1.0959 0.7526 0.7752 0.031 Uiso 1 1 calc R . . C21 C 1.04526(13) 0.80423(4) 0.84782(17) 0.0209(2) Uani 1 1 d . . . H21 H 0.9640 0.8089 0.7398 0.025 Uiso 1 1 calc R . . C22 C 1.09004(11) 0.91435(4) 1.13121(15) 0.0157(2) Uani 1 1 d . . . C23 C 1.20995(12) 0.92705(4) 1.14838(16) 0.0184(2) Uani 1 1 d . . . H23 H 1.2389 0.9143 1.0823 0.022 Uiso 1 1 calc R . . C24 C 1.28693(13) 0.95812(4) 1.26072(18) 0.0215(3) Uani 1 1 d . . . H24 H 1.3669 0.9668 1.2693 0.026 Uiso 1 1 calc R . . C25 C 1.24679(13) 0.97647(4) 1.36062(17) 0.0224(3) Uani 1 1 d . . . H25 H 1.2998 0.9976 1.4380 0.027 Uiso 1 1 calc R . . C26 C 1.12948(13) 0.96400(4) 1.34731(16) 0.0200(2) Uani 1 1 d . . . H26 H 1.1030 0.9762 1.4170 0.024 Uiso 1 1 calc R . . C27 C 1.05075(12) 0.93360(4) 1.23177(15) 0.0164(2) Uani 1 1 d . . . H27 H 0.9691 0.9258 1.2208 0.020 Uiso 1 1 calc R . . N1 N 0.83046(10) 0.86615(3) 0.95046(13) 0.01510(19) Uani 1 1 d . . . N2 N 0.60449(11) 0.88271(3) 0.82150(14) 0.0186(2) Uani 1 1 d . . . B3 B 0.83385(13) 0.94916(4) 0.75980(17) 0.0152(2) Uani 1 1 d . . . H3 H 0.8688 0.9657 0.8825 0.018 Uiso 1 1 calc R . . B4 B 0.66362(13) 0.95140(4) 0.58228(17) 0.0161(3) Uani 1 1 d . . . H4 H 0.5862 0.9696 0.5878 0.019 Uiso 1 1 calc R . . B5 B 0.62163(13) 0.90398(4) 0.47055(18) 0.0175(3) Uani 1 1 d . . . H5 H 0.5169 0.8913 0.4028 0.021 Uiso 1 1 calc R . . B6 B 0.76643(14) 0.87223(4) 0.58026(18) 0.0159(3) Uani 1 1 d . . . H6 H 0.7576 0.8386 0.5864 0.019 Uiso 1 1 calc R . . B7 B 0.89826(14) 0.89502(4) 0.57035(18) 0.0169(3) Uani 1 1 d . . . H7 H 0.9765 0.8763 0.5686 0.020 Uiso 1 1 calc R . . B8 B 0.93978(14) 0.94209(4) 0.68103(18) 0.0167(2) Uani 1 1 d . . . H8 H 1.0453 0.9542 0.7519 0.020 Uiso 1 1 calc R . . B9 B 0.79511(14) 0.97432(4) 0.57115(18) 0.0169(3) Uani 1 1 d . . . H9 H 0.8044 1.0080 0.5676 0.020 Uiso 1 1 calc R . . B10 B 0.66402(14) 0.94662(4) 0.39129(17) 0.0175(3) Uani 1 1 d . . . H10 H 0.5869 0.9622 0.2690 0.021 Uiso 1 1 calc R . . B11 B 0.72799(14) 0.89742(4) 0.39124(18) 0.0181(3) Uani 1 1 d . . . H11 H 0.6933 0.8805 0.2695 0.022 Uiso 1 1 calc R . . B12 B 0.83474(14) 0.94100(4) 0.45256(18) 0.0182(3) Uani 1 1 d . . . H12 H 0.8700 0.9529 0.3706 0.022 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 Si 0.01235(13) 0.01373(14) 0.01300(14) -0.00037(11) 0.00726(11) 0.00078(11) C1 0.0128(5) 0.0155(5) 0.0150(6) 0.0006(4) 0.0074(4) 0.0012(4) C2 0.0137(5) 0.0141(5) 0.0139(5) -0.0017(4) 0.0080(4) -0.0006(4) C3 0.0159(5) 0.0149(5) 0.0145(6) 0.0015(4) 0.0083(5) 0.0007(4) C4 0.0154(5) 0.0161(6) 0.0165(6) 0.0026(4) 0.0096(5) 0.0010(4) C5 0.0209(6) 0.0171(5) 0.0155(6) 0.0007(4) 0.0095(5) -0.0005(4) C6 0.0238(6) 0.0196(6) 0.0178(6) 0.0038(5) 0.0116(5) 0.0024(5) C7 0.0291(6) 0.0172(6) 0.0218(6) 0.0050(5) 0.0139(5) 0.0023(5) C8 0.0295(6) 0.0202(6) 0.0245(7) 0.0020(5) 0.0124(6) -0.0065(5) C9 0.0224(6) 0.0194(6) 0.0176(6) 0.0010(5) 0.0088(5) -0.0040(5) C10 0.0155(5) 0.0237(6) 0.0204(6) 0.0076(5) 0.0105(5) 0.0045(5) C11 0.0182(6) 0.0268(6) 0.0195(6) -0.0044(5) 0.0076(5) 0.0033(5) C12 0.0207(6) 0.0204(6) 0.0352(8) -0.0021(5) 0.0146(6) -0.0050(5) C13 0.0249(7) 0.0310(7) 0.0374(8) 0.0018(6) 0.0232(6) -0.0011(6) C14 0.0223(6) 0.0274(6) 0.0203(6) -0.0026(5) 0.0123(5) 0.0038(5) C15 0.0163(5) 0.0170(6) 0.0260(7) 0.0023(5) 0.0088(5) 0.0009(4) C16 0.0157(5) 0.0163(5) 0.0192(6) 0.0034(4) 0.0113(5) 0.0016(4) C17 0.0217(6) 0.0247(6) 0.0186(6) 0.0017(5) 0.0107(5) 0.0059(5) C18 0.0274(7) 0.0326(7) 0.0239(7) 0.0077(6) 0.0119(6) 0.0144(6) C19 0.0346(7) 0.0245(7) 0.0338(8) 0.0070(6) 0.0219(6) 0.0149(6) C20 0.0312(7) 0.0208(6) 0.0300(7) -0.0035(5) 0.0188(6) 0.0052(5) C21 0.0189(6) 0.0205(6) 0.0215(6) -0.0013(5) 0.0099(5) 0.0019(5) C22 0.0138(5) 0.0162(5) 0.0144(5) 0.0019(4) 0.0059(4) 0.0018(4) C23 0.0154(5) 0.0216(6) 0.0188(6) 0.0010(5) 0.0097(5) 0.0007(4) C24 0.0155(5) 0.0202(6) 0.0233(6) 0.0031(5) 0.0070(5) -0.0012(4) C25 0.0220(6) 0.0163(6) 0.0200(6) -0.0010(5) 0.0056(5) -0.0021(5) C26 0.0239(6) 0.0161(5) 0.0171(6) -0.0011(4) 0.0093(5) 0.0030(5) C27 0.0168(5) 0.0154(5) 0.0160(6) 0.0012(4) 0.0083(5) 0.0017(4) N1 0.0138(4) 0.0165(4) 0.0153(5) 0.0022(4) 0.0081(4) 0.0022(4) N2 0.0153(5) 0.0218(5) 0.0201(5) 0.0055(4) 0.0105(4) 0.0029(4) B3 0.0170(6) 0.0134(6) 0.0158(6) 0.0005(5) 0.0094(5) 0.0017(5) B4 0.0181(6) 0.0158(6) 0.0153(6) 0.0023(5) 0.0097(5) 0.0028(5) B5 0.0161(6) 0.0189(6) 0.0150(6) 0.0009(5) 0.0069(5) 0.0018(5) B6 0.0152(6) 0.0165(6) 0.0147(6) -0.0014(5) 0.0073(5) 0.0003(5) B7 0.0183(6) 0.0188(6) 0.0154(6) -0.0004(5) 0.0104(5) 0.0006(5) B8 0.0185(6) 0.0164(6) 0.0180(6) 0.0003(5) 0.0118(5) -0.0006(5) B9 0.0199(6) 0.0153(6) 0.0177(6) 0.0013(5) 0.0115(5) 0.0003(5) B10 0.0200(6) 0.0183(6) 0.0153(6) 0.0019(5) 0.0105(5) 0.0018(5) B11 0.0198(6) 0.0191(6) 0.0143(6) -0.0005(5) 0.0086(5) 0.0020(5) B12 0.0210(6) 0.0201(6) 0.0163(6) 0.0020(5) 0.0118(5) 0.0014(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si N1 1.7404(10) . ? Si C22 1.8618(13) . ? Si C16 1.8698(12) . ? Si C2 1.8964(13) . ? C1 C3 1.5332(16) . ? C1 C2 1.6616(15) . ? C1 B4 1.7183(17) . ? C1 B5 1.7188(18) . ? C1 B6 1.7227(18) . ? C1 B3 1.7383(17) . ? C2 B8 1.6998(17) . ? C2 B7 1.7059(18) . ? C2 B6 1.7299(18) . ? C2 B3 1.7311(17) . ? C3 N2 1.2619(16) . ? C3 N1 1.4128(15) . ? C4 N1 1.4858(15) . ? C4 C5 1.5289(17) . ? C4 C9 1.5339(17) . ? C4 H4A 1.0000 . ? C5 C6 1.5336(16) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.5285(18) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.5272(19) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.5294(17) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N2 1.4652(16) . ? C10 C11 1.5320(19) . ? C10 C15 1.5337(18) . ? C10 H10A 1.0000 . ? C11 C12 1.527(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.5214(19) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.524(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.5260(19) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C21 1.3988(18) . ? C16 C17 1.3998(18) . ? C17 C18 1.3944(19) . ? C17 H17 0.9500 . ? C18 C19 1.385(2) . ? C18 H18 0.9500 . ? C19 C20 1.388(2) . ? C19 H19 0.9500 . ? C20 C21 1.3908(18) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.4027(17) . ? C22 C23 1.4029(17) . ? C23 C24 1.3902(18) . ? C23 H23 0.9500 . ? C24 C25 1.391(2) . ? C24 H24 0.9500 . ? C25 C26 1.387(2) . ? C25 H25 0.9500 . ? C26 C27 1.3909(18) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? B3 B9 1.7594(19) . ? B3 B4 1.777(2) . ? B3 B8 1.7787(19) . ? B3 H3 1.1200 . ? B4 B9 1.7831(19) . ? B4 B10 1.7845(19) . ? B4 B5 1.7918(19) . ? B4 H4 1.1200 . ? B5 B6 1.7794(19) . ? B5 B10 1.782(2) . ? B5 B11 1.785(2) . ? B5 H5 1.1200 . ? B6 B11 1.764(2) . ? B6 B7 1.7790(19) . ? B6 H6 1.1200 . ? B7 B8 1.7777(19) . ? B7 B12 1.780(2) . ? B7 B11 1.782(2) . ? B7 H7 1.1200 . ? B8 B12 1.781(2) . ? B8 B9 1.7878(19) . ? B8 H8 1.1200 . ? B9 B10 1.790(2) . ? B9 B12 1.791(2) . ? B9 H9 1.1200 . ? B10 B12 1.785(2) . ? B10 B11 1.791(2) . ? B10 H10 1.1200 . ? B11 B12 1.790(2) . ? B11 H11 1.1200 . ? B12 H12 1.1200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Si C22 114.23(5) . . ? N1 Si C16 116.29(5) . . ? C22 Si C16 109.66(6) . . ? N1 Si C2 92.56(5) . . ? C22 Si C2 108.83(5) . . ? C16 Si C2 114.20(5) . . ? C3 C1 C2 110.18(9) . . ? C3 C1 B4 129.10(10) . . ? C2 C1 B4 110.55(9) . . ? C3 C1 B5 125.52(10) . . ? C2 C1 B5 110.93(9) . . ? B4 C1 B5 62.84(8) . . ? C3 C1 B6 111.61(9) . . ? C2 C1 B6 61.45(7) . . ? B4 C1 B6 114.03(9) . . ? B5 C1 B6 62.27(8) . . ? C3 C1 B3 116.72(10) . . ? C2 C1 B3 61.17(7) . . ? B4 C1 B3 61.87(8) . . ? B5 C1 B3 113.79(9) . . ? B6 C1 B3 113.84(9) . . ? C1 C2 B8 111.53(9) . . ? C1 C2 B7 111.09(9) . . ? B8 C2 B7 62.93(8) . . ? C1 C2 B6 61.02(7) . . ? B8 C2 B6 114.31(10) . . ? B7 C2 B6 62.36(8) . . ? C1 C2 B3 61.60(7) . . ? B8 C2 B3 62.45(8) . . ? B7 C2 B3 114.29(9) . . ? B6 C2 B3 113.84(9) . . ? C1 C2 Si 105.28(7) . . ? B8 C2 Si 128.57(8) . . ? B7 C2 Si 132.25(8) . . ? B6 C2 Si 114.54(8) . . ? B3 C2 Si 109.75(8) . . ? N2 C3 N1 120.32(11) . . ? N2 C3 C1 128.36(11) . . ? N1 C3 C1 111.25(10) . . ? N1 C4 C5 112.54(10) . . ? N1 C4 C9 109.44(10) . . ? C5 C4 C9 111.27(10) . . ? N1 C4 H4A 107.8 . . ? C5 C4 H4A 107.8 . . ? C9 C4 H4A 107.8 . . ? C4 C5 C6 110.12(10) . . ? C4 C5 H5A 109.6 . . ? C6 C5 H5A 109.6 . . ? C4 C5 H5B 109.6 . . ? C6 C5 H5B 109.6 . . ? H5A C5 H5B 108.2 . . ? C7 C6 C5 111.34(10) . . ? C7 C6 H6A 109.4 . . ? C5 C6 H6A 109.4 . . ? C7 C6 H6B 109.4 . . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C8 C7 C6 110.83(10) . . ? C8 C7 H7A 109.5 . . ? C6 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? C7 C8 C9 110.80(11) . . ? C7 C8 H8A 109.5 . . ? C9 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C8 C9 C4 111.45(11) . . ? C8 C9 H9A 109.3 . . ? C4 C9 H9A 109.3 . . ? C8 C9 H9B 109.3 . . ? C4 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? N2 C10 C11 108.94(10) . . ? N2 C10 C15 108.16(10) . . ? C11 C10 C15 110.66(10) . . ? N2 C10 H10A 109.7 . . ? C11 C10 H10A 109.7 . . ? C15 C10 H10A 109.7 . . ? C12 C11 C10 112.83(11) . . ? C12 C11 H11A 109.0 . . ? C10 C11 H11A 109.0 . . ? C12 C11 H11B 109.0 . . ? C10 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C13 C12 C11 110.96(11) . . ? C13 C12 H12A 109.4 . . ? C11 C12 H12A 109.4 . . ? C13 C12 H12B 109.4 . . ? C11 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? C12 C13 C14 110.67(11) . . ? C12 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C13 C14 C15 110.73(11) . . ? C13 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C14 C15 C10 112.48(10) . . ? C14 C15 H15A 109.1 . . ? C10 C15 H15A 109.1 . . ? C14 C15 H15B 109.1 . . ? C10 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? C21 C16 C17 117.78(11) . . ? C21 C16 Si 123.24(9) . . ? C17 C16 Si 118.98(10) . . ? C18 C17 C16 121.16(13) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C19 C18 C17 119.88(13) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 119.99(12) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C19 C20 C21 119.91(13) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C20 C21 C16 121.27(12) . . ? C20 C21 H21 119.4 . . ? C16 C21 H21 119.4 . . ? C27 C22 C23 118.13(11) . . ? C27 C22 Si 121.77(9) . . ? C23 C22 Si 119.86(10) . . ? C24 C23 C22 120.89(12) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C25 119.97(12) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C26 C25 C24 120.07(12) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C27 119.92(12) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 C22 120.99(11) . . ? C26 C27 H27 119.5 . . ? C22 C27 H27 119.5 . . ? C3 N1 C4 115.66(9) . . ? C3 N1 Si 119.08(8) . . ? C4 N1 Si 125.14(8) . . ? C3 N2 C10 125.27(11) . . ? C2 B3 C1 57.23(7) . . ? C2 B3 B9 104.85(9) . . ? C1 B3 B9 105.12(9) . . ? C2 B3 B4 104.71(9) . . ? C1 B3 B4 58.51(7) . . ? B9 B3 B4 60.56(8) . . ? C2 B3 B8 57.91(7) . . ? C1 B3 B8 104.40(9) . . ? B9 B3 B8 60.70(8) . . ? B4 B3 B8 108.66(10) . . ? C2 B3 H3 124.9 . . ? C1 B3 H3 124.6 . . ? B9 B3 H3 122.4 . . ? B4 B3 H3 121.8 . . ? B8 B3 H3 122.1 . . ? C1 B4 B3 59.62(7) . . ? C1 B4 B9 104.95(9) . . ? B3 B4 B9 59.23(8) . . ? C1 B4 B10 104.53(9) . . ? B3 B4 B10 107.61(10) . . ? B9 B4 B10 60.24(8) . . ? C1 B4 B5 58.59(7) . . ? B3 B4 B5 108.47(9) . . ? B9 B4 B5 108.15(9) . . ? B10 B4 B5 59.79(8) . . ? C1 B4 H4 124.5 . . ? B3 B4 H4 121.4 . . ? B9 B4 H4 122.4 . . ? B10 B4 H4 122.6 . . ? B5 B4 H4 121.4 . . ? C1 B5 B6 58.97(7) . . ? C1 B5 B10 104.60(9) . . ? B6 B5 B10 107.53(9) . . ? C1 B5 B11 104.64(9) . . ? B6 B5 B11 59.32(8) . . ? B10 B5 B11 60.28(8) . . ? C1 B5 B4 58.56(7) . . ? B6 B5 B4 107.84(9) . . ? B10 B5 B4 59.90(8) . . ? B11 B5 B4 108.06(10) . . ? C1 B5 H5 124.7 . . ? B6 B5 H5 121.8 . . ? B10 B5 H5 122.4 . . ? B11 B5 H5 122.4 . . ? B4 B5 H5 121.5 . . ? C1 B6 C2 57.54(7) . . ? C1 B6 B11 105.40(9) . . ? C2 B6 B11 104.87(9) . . ? C1 B6 B7 104.93(9) . . ? C2 B6 B7 58.16(7) . . ? B11 B6 B7 60.40(8) . . ? C1 B6 B5 58.76(7) . . ? C2 B6 B5 105.04(9) . . ? B11 B6 B5 60.51(8) . . ? B7 B6 B5 108.60(10) . . ? C1 B6 H6 124.2 . . ? C2 B6 H6 124.6 . . ? B11 B6 H6 122.5 . . ? B7 B6 H6 122.0 . . ? B5 B6 H6 121.7 . . ? C2 B7 B8 58.37(7) . . ? C2 B7 B6 59.48(7) . . ? B8 B7 B6 108.22(9) . . ? C2 B7 B12 104.67(9) . . ? B8 B7 B12 60.10(8) . . ? B6 B7 B12 107.71(9) . . ? C2 B7 B11 105.10(9) . . ? B8 B7 B11 108.43(9) . . ? B6 B7 B11 59.38(8) . . ? B12 B7 B11 60.32(8) . . ? C2 B7 H7 124.5 . . ? B8 B7 H7 121.4 . . ? B6 B7 H7 121.5 . . ? B12 B7 H7 122.4 . . ? B11 B7 H7 122.2 . . ? C2 B8 B7 58.70(7) . . ? C2 B8 B3 59.64(7) . . ? B7 B8 B3 108.56(9) . . ? C2 B8 B12 104.85(10) . . ? B7 B8 B12 60.00(8) . . ? B3 B8 B12 107.64(10) . . ? C2 B8 B9 104.96(9) . . ? B7 B8 B9 108.24(10) . . ? B3 B8 B9 59.12(7) . . ? B12 B8 B9 60.23(8) . . ? C2 B8 H8 124.3 . . ? B7 B8 H8 121.2 . . ? B3 B8 H8 121.5 . . ? B12 B8 H8 122.5 . . ? B9 B8 H8 122.5 . . ? B3 B9 B4 60.21(8) . . ? B3 B9 B8 60.18(8) . . ? B4 B9 B8 107.99(9) . . ? B3 B9 B10 108.13(10) . . ? B4 B9 B10 59.92(8) . . ? B8 B9 B10 107.54(10) . . ? B3 B9 B12 108.07(9) . . ? B4 B9 B12 107.78(9) . . ? B8 B9 B12 59.71(8) . . ? B10 B9 B12 59.78(8) . . ? B3 B9 H9 121.4 . . ? B4 B9 H9 121.7 . . ? B8 B9 H9 121.9 . . ? B10 B9 H9 121.9 . . ? B12 B9 H9 121.9 . . ? B5 B10 B4 60.31(8) . . ? B5 B10 B12 108.13(9) . . ? B4 B10 B12 108.00(10) . . ? B5 B10 B9 108.24(9) . . ? B4 B10 B9 59.84(8) . . ? B12 B10 B9 60.13(8) . . ? B5 B10 B11 59.94(8) . . ? B4 B10 B11 108.12(9) . . ? B12 B10 B11 60.06(8) . . ? B9 B10 B11 108.17(9) . . ? B5 B10 H10 121.5 . . ? B4 B10 H10 121.7 . . ? B12 B10 H10 121.7 . . ? B9 B10 H10 121.6 . . ? B11 B10 H10 121.7 . . ? B6 B11 B7 60.22(8) . . ? B6 B11 B5 60.18(8) . . ? B7 B11 B5 108.20(10) . . ? B6 B11 B12 107.94(10) . . ? B7 B11 B12 59.77(8) . . ? B5 B11 B12 107.78(10) . . ? B6 B11 B10 107.83(10) . . ? B7 B11 B10 107.62(10) . . ? B5 B11 B10 59.79(8) . . ? B12 B11 B10 59.78(8) . . ? B6 B11 H11 121.6 . . ? B7 B11 H11 121.7 . . ? B5 B11 H11 121.7 . . ? B12 B11 H11 121.9 . . ? B10 B11 H11 122.0 . . ? B7 B12 B8 59.90(8) . . ? B7 B12 B10 108.02(9) . . ? B8 B12 B10 108.07(10) . . ? B7 B12 B11 59.91(8) . . ? B8 B12 B11 107.94(9) . . ? B10 B12 B11 60.16(8) . . ? B7 B12 B9 108.02(9) . . ? B8 B12 B9 60.06(8) . . ? B10 B12 B9 60.10(8) . . ? B11 B12 B9 108.23(9) . . ? B7 B12 H12 121.8 . . ? B8 B12 H12 121.8 . . ? B10 B12 H12 121.6 . . ? B11 B12 H12 121.7 . . ? B9 B12 H12 121.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 C1 C2 B8 -149.01(10) . . . . ? B4 C1 C2 B8 -0.22(13) . . . . ? B5 C1 C2 B8 67.54(12) . . . . ? B6 C1 C2 B8 106.70(10) . . . . ? B3 C1 C2 B8 -38.86(9) . . . . ? C3 C1 C2 B7 142.84(10) . . . . ? B4 C1 C2 B7 -68.37(11) . . . . ? B5 C1 C2 B7 -0.62(12) . . . . ? B6 C1 C2 B7 38.55(9) . . . . ? B3 C1 C2 B7 -107.02(10) . . . . ? C3 C1 C2 B6 104.29(10) . . . . ? B4 C1 C2 B6 -106.92(10) . . . . ? B5 C1 C2 B6 -39.16(9) . . . . ? B3 C1 C2 B6 -145.57(9) . . . . ? C3 C1 C2 B3 -110.15(10) . . . . ? B4 C1 C2 B3 38.65(9) . . . . ? B5 C1 C2 B3 106.40(10) . . . . ? B6 C1 C2 B3 145.57(9) . . . . ? C3 C1 C2 Si -5.64(10) . . . . ? B4 C1 C2 Si 143.15(8) . . . . ? B5 C1 C2 Si -149.09(8) . . . . ? B6 C1 C2 Si -109.93(8) . . . . ? B3 C1 C2 Si 104.51(8) . . . . ? N1 Si C2 C1 9.77(7) . . . . ? C22 Si C2 C1 -106.93(7) . . . . ? C16 Si C2 C1 130.18(7) . . . . ? N1 Si C2 B8 144.55(10) . . . . ? C22 Si C2 B8 27.85(11) . . . . ? C16 Si C2 B8 -95.04(10) . . . . ? N1 Si C2 B7 -129.01(11) . . . . ? C22 Si C2 B7 114.29(11) . . . . ? C16 Si C2 B7 -8.59(12) . . . . ? N1 Si C2 B6 -54.92(9) . . . . ? C22 Si C2 B6 -171.62(8) . . . . ? C16 Si C2 B6 65.49(9) . . . . ? N1 Si C2 B3 74.57(8) . . . . ? C22 Si C2 B3 -42.13(9) . . . . ? C16 Si C2 B3 -165.02(7) . . . . ? C2 C1 C3 N2 -179.67(12) . . . . ? B4 C1 C3 N2 39.0(2) . . . . ? B5 C1 C3 N2 -42.78(19) . . . . ? B6 C1 C3 N2 -113.38(14) . . . . ? B3 C1 C3 N2 113.30(14) . . . . ? C2 C1 C3 N1 -2.70(13) . . . . ? B4 C1 C3 N1 -144.01(11) . . . . ? B5 C1 C3 N1 134.19(11) . . . . ? B6 C1 C3 N1 63.59(12) . . . . ? B3 C1 C3 N1 -69.73(12) . . . . ? N1 C4 C5 C6 -179.07(9) . . . . ? C9 C4 C5 C6 -55.81(13) . . . . ? C4 C5 C6 C7 56.80(14) . . . . ? C5 C6 C7 C8 -57.16(14) . . . . ? C6 C7 C8 C9 55.96(15) . . . . ? C7 C8 C9 C4 -55.37(15) . . . . ? N1 C4 C9 C8 -179.30(10) . . . . ? C5 C4 C9 C8 55.68(14) . . . . ? N2 C10 C11 C12 66.93(14) . . . . ? C15 C10 C11 C12 -51.87(14) . . . . ? C10 C11 C12 C13 54.73(14) . . . . ? C11 C12 C13 C14 -56.97(15) . . . . ? C12 C13 C14 C15 57.59(15) . . . . ? C13 C14 C15 C10 -55.81(14) . . . . ? N2 C10 C15 C14 -66.86(13) . . . . ? C11 C10 C15 C14 52.41(14) . . . . ? N1 Si C16 C21 70.46(12) . . . . ? C22 Si C16 C21 -158.04(10) . . . . ? C2 Si C16 C21 -35.61(12) . . . . ? N1 Si C16 C17 -108.94(10) . . . . ? C22 Si C16 C17 22.57(11) . . . . ? C2 Si C16 C17 145.00(10) . . . . ? C21 C16 C17 C18 -1.15(19) . . . . ? Si C16 C17 C18 178.28(11) . . . . ? C16 C17 C18 C19 0.7(2) . . . . ? C17 C18 C19 C20 0.2(2) . . . . ? C18 C19 C20 C21 -0.4(2) . . . . ? C19 C20 C21 C16 -0.1(2) . . . . ? C17 C16 C21 C20 0.87(19) . . . . ? Si C16 C21 C20 -178.53(11) . . . . ? N1 Si C22 C27 -1.68(12) . . . . ? C16 Si C22 C27 -134.26(10) . . . . ? C2 Si C22 C27 100.17(10) . . . . ? N1 Si C22 C23 -176.06(9) . . . . ? C16 Si C22 C23 51.36(11) . . . . ? C2 Si C22 C23 -74.21(11) . . . . ? C27 C22 C23 C24 -0.60(18) . . . . ? Si C22 C23 C24 173.98(10) . . . . ? C22 C23 C24 C25 1.35(19) . . . . ? C23 C24 C25 C26 -0.48(19) . . . . ? C24 C25 C26 C27 -1.13(19) . . . . ? C25 C26 C27 C22 1.89(18) . . . . ? C23 C22 C27 C26 -1.01(17) . . . . ? Si C22 C27 C26 -175.49(9) . . . . ? N2 C3 N1 C4 12.67(16) . . . . ? C1 C3 N1 C4 -164.57(10) . . . . ? N2 C3 N1 Si -171.20(10) . . . . ? C1 C3 N1 Si 11.56(13) . . . . ? C5 C4 N1 C3 -150.99(10) . . . . ? C9 C4 N1 C3 84.74(12) . . . . ? C5 C4 N1 Si 33.14(14) . . . . ? C9 C4 N1 Si -91.13(12) . . . . ? C22 Si N1 C3 98.73(10) . . . . ? C16 Si N1 C3 -131.93(9) . . . . ? C2 Si N1 C3 -13.26(9) . . . . ? C22 Si N1 C4 -85.54(10) . . . . ? C16 Si N1 C4 43.80(11) . . . . ? C2 Si N1 C4 162.48(10) . . . . ? N1 C3 N2 C10 178.02(11) . . . . ? C1 C3 N2 C10 -5.3(2) . . . . ? C11 C10 N2 C3 123.61(13) . . . . ? C15 C10 N2 C3 -116.04(14) . . . . ? B8 C2 B3 C1 138.83(10) . . . . ? B7 C2 B3 C1 101.82(10) . . . . ? B6 C2 B3 C1 32.74(9) . . . . ? Si C2 B3 C1 -97.13(8) . . . . ? C1 C2 B3 B9 -98.63(10) . . . . ? B8 C2 B3 B9 40.19(9) . . . . ? B7 C2 B3 B9 3.19(12) . . . . ? B6 C2 B3 B9 -65.90(12) . . . . ? Si C2 B3 B9 164.23(7) . . . . ? C1 C2 B3 B4 -35.77(8) . . . . ? B8 C2 B3 B4 103.05(10) . . . . ? B7 C2 B3 B4 66.05(11) . . . . ? B6 C2 B3 B4 -3.04(12) . . . . ? Si C2 B3 B4 -132.91(8) . . . . ? C1 C2 B3 B8 -138.83(10) . . . . ? B7 C2 B3 B8 -37.00(9) . . . . ? B6 C2 B3 B8 -106.09(11) . . . . ? Si C2 B3 B8 124.04(9) . . . . ? C3 C1 B3 C2 99.43(11) . . . . ? B4 C1 B3 C2 -138.46(9) . . . . ? B5 C1 B3 C2 -101.72(10) . . . . ? B6 C1 B3 C2 -32.89(9) . . . . ? C3 C1 B3 B9 -162.42(9) . . . . ? C2 C1 B3 B9 98.16(10) . . . . ? B4 C1 B3 B9 -40.31(9) . . . . ? B5 C1 B3 B9 -3.56(12) . . . . ? B6 C1 B3 B9 65.27(11) . . . . ? C3 C1 B3 B4 -122.11(11) . . . . ? C2 C1 B3 B4 138.46(9) . . . . ? B5 C1 B3 B4 36.75(9) . . . . ? B6 C1 B3 B4 105.58(10) . . . . ? C3 C1 B3 B8 134.59(10) . . . . ? C2 C1 B3 B8 35.16(8) . . . . ? B4 C1 B3 B8 -103.30(10) . . . . ? B5 C1 B3 B8 -66.55(11) . . . . ? B6 C1 B3 B8 2.27(12) . . . . ? C3 C1 B4 B3 102.85(13) . . . . ? C2 C1 B4 B3 -38.34(9) . . . . ? B5 C1 B4 B3 -142.02(10) . . . . ? B6 C1 B4 B3 -105.28(10) . . . . ? C3 C1 B4 B9 142.48(11) . . . . ? C2 C1 B4 B9 1.28(12) . . . . ? B5 C1 B4 B9 -102.40(10) . . . . ? B6 C1 B4 B9 -65.65(12) . . . . ? B3 C1 B4 B9 39.63(9) . . . . ? C3 C1 B4 B10 -155.01(11) . . . . ? C2 C1 B4 B10 63.80(11) . . . . ? B5 C1 B4 B10 -39.88(9) . . . . ? B6 C1 B4 B10 -3.14(12) . . . . ? B3 C1 B4 B10 102.14(10) . . . . ? C3 C1 B4 B5 -115.12(13) . . . . ? C2 C1 B4 B5 103.68(10) . . . . ? B6 C1 B4 B5 36.75(9) . . . . ? B3 C1 B4 B5 142.02(10) . . . . ? C2 B3 B4 C1 35.20(8) . . . . ? B9 B3 B4 C1 134.18(10) . . . . ? B8 B3 B4 C1 95.79(10) . . . . ? C2 B3 B4 B9 -98.98(10) . . . . ? C1 B3 B4 B9 -134.18(10) . . . . ? B8 B3 B4 B9 -38.39(9) . . . . ? C2 B3 B4 B10 -61.64(11) . . . . ? C1 B3 B4 B10 -96.84(10) . . . . ? B9 B3 B4 B10 37.34(9) . . . . ? B8 B3 B4 B10 -1.05(12) . . . . ? C2 B3 B4 B5 1.58(12) . . . . ? C1 B3 B4 B5 -33.62(8) . . . . ? B9 B3 B4 B5 100.56(10) . . . . ? B8 B3 B4 B5 62.17(11) . . . . ? C3 C1 B5 B6 -97.81(12) . . . . ? C2 C1 B5 B6 38.81(9) . . . . ? B4 C1 B5 B6 141.88(10) . . . . ? B3 C1 B5 B6 105.50(10) . . . . ? C3 C1 B5 B10 160.26(10) . . . . ? C2 C1 B5 B10 -63.11(11) . . . . ? B4 C1 B5 B10 39.95(9) . . . . ? B6 C1 B5 B10 -101.92(10) . . . . ? B3 C1 B5 B10 3.58(12) . . . . ? C3 C1 B5 B11 -137.22(11) . . . . ? C2 C1 B5 B11 -0.60(12) . . . . ? B4 C1 B5 B11 102.47(10) . . . . ? B6 C1 B5 B11 -39.41(9) . . . . ? B3 C1 B5 B11 66.10(12) . . . . ? C3 C1 B5 B4 120.31(12) . . . . ? C2 C1 B5 B4 -103.07(10) . . . . ? B6 C1 B5 B4 -141.88(10) . . . . ? B3 C1 B5 B4 -36.37(9) . . . . ? B3 B4 B5 C1 34.03(8) . . . . ? B9 B4 B5 C1 96.77(10) . . . . ? B10 B4 B5 C1 134.09(9) . . . . ? C1 B4 B5 B6 -33.76(9) . . . . ? B3 B4 B5 B6 0.27(12) . . . . ? B9 B4 B5 B6 63.01(12) . . . . ? B10 B4 B5 B6 100.33(10) . . . . ? C1 B4 B5 B10 -134.09(9) . . . . ? B3 B4 B5 B10 -100.06(10) . . . . ? B9 B4 B5 B10 -37.32(9) . . . . ? C1 B4 B5 B11 -96.45(10) . . . . ? B3 B4 B5 B11 -62.42(11) . . . . ? B9 B4 B5 B11 0.32(12) . . . . ? B10 B4 B5 B11 37.64(9) . . . . ? C3 C1 B6 C2 -101.94(10) . . . . ? B4 C1 B6 C2 101.24(10) . . . . ? B5 C1 B6 C2 138.21(9) . . . . ? B3 C1 B6 C2 32.79(9) . . . . ? C3 C1 B6 B11 160.00(10) . . . . ? C2 C1 B6 B11 -98.06(10) . . . . ? B4 C1 B6 B11 3.18(12) . . . . ? B5 C1 B6 B11 40.15(9) . . . . ? B3 C1 B6 B11 -65.27(11) . . . . ? C3 C1 B6 B7 -137.18(10) . . . . ? C2 C1 B6 B7 -35.24(8) . . . . ? B4 C1 B6 B7 66.00(12) . . . . ? B5 C1 B6 B7 102.97(10) . . . . ? B3 C1 B6 B7 -2.45(12) . . . . ? C3 C1 B6 B5 119.85(11) . . . . ? C2 C1 B6 B5 -138.21(9) . . . . ? B4 C1 B6 B5 -36.97(9) . . . . ? B3 C1 B6 B5 -105.42(10) . . . . ? B8 C2 B6 C1 -102.13(10) . . . . ? B7 C2 B6 C1 -138.98(10) . . . . ? B3 C2 B6 C1 -32.94(9) . . . . ? Si C2 B6 C1 94.49(8) . . . . ? C1 C2 B6 B11 99.02(10) . . . . ? B8 C2 B6 B11 -3.11(13) . . . . ? B7 C2 B6 B11 -39.96(9) . . . . ? B3 C2 B6 B11 66.08(12) . . . . ? Si C2 B6 B11 -166.49(7) . . . . ? C1 C2 B6 B7 138.98(10) . . . . ? B8 C2 B6 B7 36.85(9) . . . . ? B3 C2 B6 B7 106.04(11) . . . . ? Si C2 B6 B7 -126.53(9) . . . . ? C1 C2 B6 B5 36.16(8) . . . . ? B8 C2 B6 B5 -65.97(12) . . . . ? B7 C2 B6 B5 -102.82(10) . . . . ? B3 C2 B6 B5 3.21(13) . . . . ? Si C2 B6 B5 130.64(8) . . . . ? B10 B5 B6 C1 96.80(10) . . . . ? B11 B5 B6 C1 134.42(10) . . . . ? B4 B5 B6 C1 33.60(9) . . . . ? C1 B5 B6 C2 -35.61(8) . . . . ? B10 B5 B6 C2 61.20(11) . . . . ? B11 B5 B6 C2 98.82(10) . . . . ? B4 B5 B6 C2 -2.01(12) . . . . ? C1 B5 B6 B11 -134.42(10) . . . . ? B10 B5 B6 B11 -37.62(9) . . . . ? B4 B5 B6 B11 -100.82(10) . . . . ? C1 B5 B6 B7 -96.53(10) . . . . ? B10 B5 B6 B7 0.27(13) . . . . ? B11 B5 B6 B7 37.89(9) . . . . ? B4 B5 B6 B7 -62.93(12) . . . . ? C1 C2 B7 B8 104.16(10) . . . . ? B6 C2 B7 B8 142.14(10) . . . . ? B3 C2 B7 B8 36.82(9) . . . . ? Si C2 B7 B8 -118.79(12) . . . . ? C1 C2 B7 B6 -37.98(9) . . . . ? B8 C2 B7 B6 -142.14(10) . . . . ? B3 C2 B7 B6 -105.32(10) . . . . ? Si C2 B7 B6 99.07(11) . . . . ? C1 C2 B7 B12 64.19(11) . . . . ? B8 C2 B7 B12 -39.97(9) . . . . ? B6 C2 B7 B12 102.17(10) . . . . ? B3 C2 B7 B12 -3.15(12) . . . . ? Si C2 B7 B12 -158.76(9) . . . . ? C1 C2 B7 B11 1.55(12) . . . . ? B8 C2 B7 B11 -102.61(10) . . . . ? B6 C2 B7 B11 39.52(9) . . . . ? B3 C2 B7 B11 -65.80(12) . . . . ? Si C2 B7 B11 138.59(10) . . . . ? C1 B6 B7 C2 34.97(8) . . . . ? B11 B6 B7 C2 134.44(10) . . . . ? B5 B6 B7 C2 96.50(10) . . . . ? C1 B6 B7 B8 1.59(12) . . . . ? C2 B6 B7 B8 -33.38(9) . . . . ? B11 B6 B7 B8 101.06(10) . . . . ? B5 B6 B7 B8 63.12(12) . . . . ? C1 B6 B7 B12 -61.94(11) . . . . ? C2 B6 B7 B12 -96.91(10) . . . . ? B11 B6 B7 B12 37.53(9) . . . . ? B5 B6 B7 B12 -0.41(13) . . . . ? C1 B6 B7 B11 -99.48(10) . . . . ? C2 B6 B7 B11 -134.44(10) . . . . ? B5 B6 B7 B11 -37.94(9) . . . . ? C1 C2 B8 B7 -103.47(10) . . . . ? B6 C2 B8 B7 -36.63(9) . . . . ? B3 C2 B8 B7 -141.97(9) . . . . ? Si C2 B8 B7 123.93(11) . . . . ? C1 C2 B8 B3 38.50(9) . . . . ? B7 C2 B8 B3 141.97(9) . . . . ? B6 C2 B8 B3 105.34(10) . . . . ? Si C2 B8 B3 -94.10(10) . . . . ? C1 C2 B8 B12 -63.51(11) . . . . ? B7 C2 B8 B12 39.96(9) . . . . ? B6 C2 B8 B12 3.33(12) . . . . ? B3 C2 B8 B12 -102.01(10) . . . . ? Si C2 B8 B12 163.89(8) . . . . ? C1 C2 B8 B9 -0.95(12) . . . . ? B7 C2 B8 B9 102.52(10) . . . . ? B6 C2 B8 B9 65.89(12) . . . . ? B3 C2 B8 B9 -39.45(9) . . . . ? Si C2 B8 B9 -133.55(9) . . . . ? B6 B7 B8 C2 33.82(9) . . . . ? B12 B7 B8 C2 134.20(10) . . . . ? B11 B7 B8 C2 96.73(10) . . . . ? C2 B7 B8 B3 -34.11(9) . . . . ? B6 B7 B8 B3 -0.28(13) . . . . ? B12 B7 B8 B3 100.10(10) . . . . ? B11 B7 B8 B3 62.62(12) . . . . ? C2 B7 B8 B12 -134.20(10) . . . . ? B6 B7 B8 B12 -100.38(10) . . . . ? B11 B7 B8 B12 -37.48(9) . . . . ? C2 B7 B8 B9 -96.76(10) . . . . ? B6 B7 B8 B9 -62.93(12) . . . . ? B12 B7 B8 B9 37.45(9) . . . . ? B11 B7 B8 B9 -0.03(12) . . . . ? C1 B3 B8 C2 -34.86(8) . . . . ? B9 B3 B8 C2 -134.33(10) . . . . ? B4 B3 B8 C2 -96.01(10) . . . . ? C2 B3 B8 B7 33.73(9) . . . . ? C1 B3 B8 B7 -1.13(12) . . . . ? B9 B3 B8 B7 -100.60(11) . . . . ? B4 B3 B8 B7 -62.28(12) . . . . ? C2 B3 B8 B12 97.20(10) . . . . ? C1 B3 B8 B12 62.34(11) . . . . ? B9 B3 B8 B12 -37.13(9) . . . . ? B4 B3 B8 B12 1.19(12) . . . . ? C2 B3 B8 B9 134.33(10) . . . . ? C1 B3 B8 B9 99.48(10) . . . . ? B4 B3 B8 B9 38.32(9) . . . . ? C2 B3 B9 B4 98.74(10) . . . . ? C1 B3 B9 B4 39.30(8) . . . . ? B8 B3 B9 B4 137.57(10) . . . . ? C2 B3 B9 B8 -38.83(8) . . . . ? C1 B3 B9 B8 -98.27(10) . . . . ? B4 B3 B9 B8 -137.57(10) . . . . ? C2 B3 B9 B10 61.42(11) . . . . ? C1 B3 B9 B10 1.98(12) . . . . ? B4 B3 B9 B10 -37.33(9) . . . . ? B8 B3 B9 B10 100.25(10) . . . . ? C2 B3 B9 B12 -1.82(12) . . . . ? C1 B3 B9 B12 -61.26(11) . . . . ? B4 B3 B9 B12 -100.56(10) . . . . ? B8 B3 B9 B12 37.01(9) . . . . ? C1 B4 B9 B3 -39.81(9) . . . . ? B10 B4 B9 B3 -138.24(10) . . . . ? B5 B4 B9 B3 -101.12(10) . . . . ? C1 B4 B9 B8 -1.83(12) . . . . ? B3 B4 B9 B8 37.98(9) . . . . ? B10 B4 B9 B8 -100.26(11) . . . . ? B5 B4 B9 B8 -63.14(12) . . . . ? C1 B4 B9 B10 98.43(10) . . . . ? B3 B4 B9 B10 138.24(10) . . . . ? B5 B4 B9 B10 37.12(9) . . . . ? C1 B4 B9 B12 61.24(11) . . . . ? B3 B4 B9 B12 101.06(10) . . . . ? B10 B4 B9 B12 -37.19(9) . . . . ? B5 B4 B9 B12 -0.07(12) . . . . ? C2 B8 B9 B3 39.71(9) . . . . ? B7 B8 B9 B3 101.14(10) . . . . ? B12 B8 B9 B3 138.49(10) . . . . ? C2 B8 B9 B4 1.71(12) . . . . ? B7 B8 B9 B4 63.15(12) . . . . ? B3 B8 B9 B4 -37.99(9) . . . . ? B12 B8 B9 B4 100.50(10) . . . . ? C2 B8 B9 B10 -61.54(11) . . . . ? B7 B8 B9 B10 -0.10(12) . . . . ? B3 B8 B9 B10 -101.25(10) . . . . ? B12 B8 B9 B10 37.24(9) . . . . ? C2 B8 B9 B12 -98.78(10) . . . . ? B7 B8 B9 B12 -37.35(9) . . . . ? B3 B8 B9 B12 -138.49(10) . . . . ? C1 B5 B10 B4 -39.29(8) . . . . ? B6 B5 B10 B4 -100.85(10) . . . . ? B11 B5 B10 B4 -138.04(10) . . . . ? C1 B5 B10 B12 61.52(11) . . . . ? B6 B5 B10 B12 -0.04(13) . . . . ? B11 B5 B10 B12 -37.23(9) . . . . ? B4 B5 B10 B12 100.81(10) . . . . ? C1 B5 B10 B9 -2.13(12) . . . . ? B6 B5 B10 B9 -63.68(12) . . . . ? B11 B5 B10 B9 -100.87(10) . . . . ? B4 B5 B10 B9 37.17(9) . . . . ? C1 B5 B10 B11 98.75(9) . . . . ? B6 B5 B10 B11 37.19(9) . . . . ? B4 B5 B10 B11 138.04(10) . . . . ? C1 B4 B10 B5 39.29(8) . . . . ? B3 B4 B10 B5 101.53(10) . . . . ? B9 B4 B10 B5 138.42(10) . . . . ? C1 B4 B10 B12 -61.73(11) . . . . ? B3 B4 B10 B12 0.50(12) . . . . ? B9 B4 B10 B12 37.40(9) . . . . ? B5 B4 B10 B12 -101.03(10) . . . . ? C1 B4 B10 B9 -99.13(10) . . . . ? B3 B4 B10 B9 -36.90(9) . . . . ? B5 B4 B10 B9 -138.42(10) . . . . ? C1 B4 B10 B11 1.79(12) . . . . ? B3 B4 B10 B11 64.02(12) . . . . ? B9 B4 B10 B11 100.92(10) . . . . ? B5 B4 B10 B11 -37.51(9) . . . . ? B3 B9 B10 B5 0.08(12) . . . . ? B4 B9 B10 B5 -37.37(9) . . . . ? B8 B9 B10 B5 63.65(11) . . . . ? B12 B9 B10 B5 100.86(10) . . . . ? B3 B9 B10 B4 37.46(9) . . . . ? B8 B9 B10 B4 101.02(10) . . . . ? B12 B9 B10 B4 138.23(10) . . . . ? B3 B9 B10 B12 -100.78(10) . . . . ? B4 B9 B10 B12 -138.23(10) . . . . ? B8 B9 B10 B12 -37.22(9) . . . . ? B3 B9 B10 B11 -63.37(12) . . . . ? B4 B9 B10 B11 -100.83(10) . . . . ? B8 B9 B10 B11 0.19(12) . . . . ? B12 B9 B10 B11 37.41(9) . . . . ? C1 B6 B11 B7 98.67(10) . . . . ? C2 B6 B11 B7 38.87(9) . . . . ? B5 B6 B11 B7 137.97(10) . . . . ? C1 B6 B11 B5 -39.30(9) . . . . ? C2 B6 B11 B5 -99.11(10) . . . . ? B7 B6 B11 B5 -137.97(10) . . . . ? C1 B6 B11 B12 61.33(11) . . . . ? C2 B6 B11 B12 1.52(12) . . . . ? B7 B6 B11 B12 -37.35(9) . . . . ? B5 B6 B11 B12 100.63(10) . . . . ? C1 B6 B11 B10 -1.83(12) . . . . ? C2 B6 B11 B10 -61.63(11) . . . . ? B7 B6 B11 B10 -100.50(10) . . . . ? B5 B6 B11 B10 37.47(9) . . . . ? C2 B7 B11 B6 -39.57(9) . . . . ? B8 B7 B11 B6 -100.71(10) . . . . ? B12 B7 B11 B6 -138.09(10) . . . . ? C2 B7 B11 B5 -1.88(12) . . . . ? B8 B7 B11 B5 -63.02(12) . . . . ? B6 B7 B11 B5 37.69(9) . . . . ? B12 B7 B11 B5 -100.40(10) . . . . ? C2 B7 B11 B12 98.52(10) . . . . ? B8 B7 B11 B12 37.38(9) . . . . ? B6 B7 B11 B12 138.09(10) . . . . ? C2 B7 B11 B10 61.29(11) . . . . ? B8 B7 B11 B10 0.15(12) . . . . ? B6 B7 B11 B10 100.86(10) . . . . ? B12 B7 B11 B10 -37.23(9) . . . . ? C1 B5 B11 B6 39.24(9) . . . . ? B10 B5 B11 B6 137.92(10) . . . . ? B4 B5 B11 B6 100.44(10) . . . . ? C1 B5 B11 B7 1.53(12) . . . . ? B6 B5 B11 B7 -37.71(9) . . . . ? B10 B5 B11 B7 100.21(10) . . . . ? B4 B5 B11 B7 62.73(12) . . . . ? C1 B5 B11 B12 -61.65(11) . . . . ? B6 B5 B11 B12 -100.89(10) . . . . ? B10 B5 B11 B12 37.02(9) . . . . ? B4 B5 B11 B12 -0.45(12) . . . . ? C1 B5 B11 B10 -98.68(10) . . . . ? B6 B5 B11 B10 -137.92(10) . . . . ? B4 B5 B11 B10 -37.48(9) . . . . ? B5 B10 B11 B6 -37.65(9) . . . . ? B4 B10 B11 B6 0.02(13) . . . . ? B12 B10 B11 B6 100.78(11) . . . . ? B9 B10 B11 B6 63.35(12) . . . . ? B5 B10 B11 B7 -101.20(10) . . . . ? B4 B10 B11 B7 -63.53(12) . . . . ? B12 B10 B11 B7 37.23(9) . . . . ? B9 B10 B11 B7 -0.21(13) . . . . ? B4 B10 B11 B5 37.67(9) . . . . ? B12 B10 B11 B5 138.43(10) . . . . ? B9 B10 B11 B5 100.99(10) . . . . ? B5 B10 B11 B12 -138.43(10) . . . . ? B4 B10 B11 B12 -100.76(10) . . . . ? B9 B10 B11 B12 -37.44(9) . . . . ? C2 B7 B12 B8 39.12(8) . . . . ? B6 B7 B12 B8 101.25(10) . . . . ? B11 B7 B12 B8 138.36(10) . . . . ? C2 B7 B12 B10 -61.75(12) . . . . ? B8 B7 B12 B10 -100.86(10) . . . . ? B6 B7 B12 B10 0.38(13) . . . . ? B11 B7 B12 B10 37.50(9) . . . . ? C2 B7 B12 B11 -99.25(10) . . . . ? B8 B7 B12 B11 -138.36(10) . . . . ? B6 B7 B12 B11 -37.12(9) . . . . ? C2 B7 B12 B9 1.80(12) . . . . ? B8 B7 B12 B9 -37.32(9) . . . . ? B6 B7 B12 B9 63.93(12) . . . . ? B11 B7 B12 B9 101.05(10) . . . . ? C2 B8 B12 B7 -39.32(8) . . . . ? B3 B8 B12 B7 -101.65(10) . . . . ? B9 B8 B12 B7 -138.30(9) . . . . ? C2 B8 B12 B10 61.46(11) . . . . ? B7 B8 B12 B10 100.78(10) . . . . ? B3 B8 B12 B10 -0.87(13) . . . . ? B9 B8 B12 B10 -37.52(9) . . . . ? C2 B8 B12 B11 -2.15(12) . . . . ? B7 B8 B12 B11 37.17(9) . . . . ? B3 B8 B12 B11 -64.48(11) . . . . ? B9 B8 B12 B11 -101.12(10) . . . . ? C2 B8 B12 B9 98.97(9) . . . . ? B7 B8 B12 B9 138.30(9) . . . . ? B3 B8 B12 B9 36.64(9) . . . . ? B5 B10 B12 B7 -0.21(13) . . . . ? B4 B10 B12 B7 63.58(12) . . . . ? B9 B10 B12 B7 100.85(10) . . . . ? B11 B10 B12 B7 -37.39(9) . . . . ? B5 B10 B12 B8 -63.56(12) . . . . ? B4 B10 B12 B8 0.23(13) . . . . ? B9 B10 B12 B8 37.50(9) . . . . ? B11 B10 B12 B8 -100.73(10) . . . . ? B5 B10 B12 B11 37.18(9) . . . . ? B4 B10 B12 B11 100.97(10) . . . . ? B9 B10 B12 B11 138.23(10) . . . . ? B5 B10 B12 B9 -101.06(10) . . . . ? B4 B10 B12 B9 -37.27(9) . . . . ? B11 B10 B12 B9 -138.23(10) . . . . ? B6 B11 B12 B7 37.54(9) . . . . ? B5 B11 B12 B7 101.11(10) . . . . ? B10 B11 B12 B7 138.14(10) . . . . ? B6 B11 B12 B8 0.38(12) . . . . ? B7 B11 B12 B8 -37.17(9) . . . . ? B5 B11 B12 B8 63.94(12) . . . . ? B10 B11 B12 B8 100.97(10) . . . . ? B6 B11 B12 B10 -100.59(10) . . . . ? B7 B11 B12 B10 -138.14(10) . . . . ? B5 B11 B12 B10 -37.02(9) . . . . ? B6 B11 B12 B9 -63.15(12) . . . . ? B7 B11 B12 B9 -100.70(10) . . . . ? B5 B11 B12 B9 0.41(12) . . . . ? B10 B11 B12 B9 37.44(9) . . . . ? B3 B9 B12 B7 0.03(13) . . . . ? B4 B9 B12 B7 -63.60(12) . . . . ? B8 B9 B12 B7 37.25(9) . . . . ? B10 B9 B12 B7 -100.85(10) . . . . ? B3 B9 B12 B8 -37.22(9) . . . . ? B4 B9 B12 B8 -100.85(10) . . . . ? B10 B9 B12 B8 -138.10(10) . . . . ? B3 B9 B12 B10 100.88(10) . . . . ? B4 B9 B12 B10 37.25(9) . . . . ? B8 B9 B12 B10 138.10(10) . . . . ? B3 B9 B12 B11 63.41(12) . . . . ? B4 B9 B12 B11 -0.22(12) . . . . ? B8 B9 B12 B11 100.63(10) . . . . ? B10 B9 B12 B11 -37.46(9) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 75.93 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.219 _refine_diff_density_min -0.241 _refine_diff_density_rms 0.032 _database_code_depnum_ccdc_archive 'CCDC 963130' ####################################################################### # # 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_magd45 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H50 B10 N2 O Ti' _chemical_formula_weight 598.68 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pmc21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, z' 'x, -y, z+1/2' _cell_length_a 12.608(3) _cell_length_b 10.454(2) _cell_length_c 24.129(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3180.3(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 22409 _cell_measurement_theta_min 3.4961 _cell_measurement_theta_max 76.0713 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 2.466 _exptl_absorpt_correction_T_min 0.71948 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Nova' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3543 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54885 _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 76.17 _reflns_number_total 6908 _reflns_number_gt 6625 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XP' _computing_publication_material SHELXL-97 _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^)+(0.0764P)^2^+2.5060P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.51(2) _refine_ls_number_reflns 6908 _refine_ls_number_parameters 424 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1257 _refine_ls_wR_factor_gt 0.1237 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.0000 0.84249(5) 0.14334(2) 0.01339(14) Uani 1 2 d S . . N1 N 0.0000 0.7855(3) 0.06368(13) 0.0129(6) Uani 1 2 d S . . N2 N 0.0000 0.6560(3) -0.01445(13) 0.0156(6) Uani 1 2 d S . . C1 C 0.0000 0.5608(3) 0.08155(15) 0.0129(6) Uani 1 2 d S . . C2 C 0.0000 0.6190(3) 0.14734(15) 0.0123(6) Uani 1 2 d S . . C3 C 0.0000 0.6680(3) 0.03832(16) 0.0137(7) Uani 1 2 d S . . C4 C 0.0000 0.9027(3) 0.02920(14) 0.0140(7) Uani 1 2 d S . . H4A H 0.0000 0.9754 0.0561 0.017 Uiso 1 2 calc SR . . C5 C 0.10064(19) 0.9209(2) -0.00602(11) 0.0165(5) Uani 1 1 d . . . H5A H 0.1641 0.9139 0.0179 0.020 Uiso 1 1 calc R . . H5B H 0.1046 0.8528 -0.0345 0.020 Uiso 1 1 calc R . . C6 C 0.0992(2) 1.0523(2) -0.03432(11) 0.0192(5) Uani 1 1 d . . . H6A H 0.1010 1.1203 -0.0058 0.023 Uiso 1 1 calc R . . H6B H 0.1629 1.0615 -0.0579 0.023 Uiso 1 1 calc R . . C7 C 0.0000 1.0677(4) -0.06975(17) 0.0215(8) Uani 1 2 d S . . H7A H 0.0000 1.1534 -0.0872 0.026 Uiso 1 2 calc SR . . H7B H 0.0000 1.0027 -0.0996 0.026 Uiso 1 2 calc SR . . C8 C 0.0000 0.5381(3) -0.04630(15) 0.0164(7) Uani 1 2 d S . . H8A H 0.0000 0.4630 -0.0206 0.020 Uiso 1 2 calc SR . . C9 C 0.0996(2) 0.5352(3) -0.08262(13) 0.0256(6) Uani 1 1 d . . . H9A H 0.1026 0.6137 -0.1055 0.031 Uiso 1 1 calc R . . H9B H 0.1634 0.5334 -0.0587 0.031 Uiso 1 1 calc R . . C10 C 0.0996(3) 0.4177(3) -0.12041(13) 0.0304(7) Uani 1 1 d . . . H10A H 0.1630 0.4204 -0.1446 0.036 Uiso 1 1 calc R . . H10B H 0.1041 0.3395 -0.0974 0.036 Uiso 1 1 calc R . . C11 C 0.0000 0.4118(5) -0.15626(19) 0.0374(11) Uani 1 2 d S . . H11A H 0.0000 0.3314 -0.1779 0.045 Uiso 1 2 calc SR . . H11B H 0.0000 0.4843 -0.1827 0.045 Uiso 1 2 calc SR . . C12 C 0.1127(2) 1.0068(3) 0.18644(12) 0.0210(5) Uani 1 1 d . . . H12A H 0.0852 1.0837 0.1993 0.025 Uiso 1 1 d R . . C13 C 0.1237(2) 0.8938(3) 0.21749(11) 0.0211(5) Uani 1 1 d . . . H13A H 0.1029 0.8820 0.2541 0.025 Uiso 1 1 d R . . C14 C 0.1719(2) 0.8015(2) 0.18299(11) 0.0184(5) Uani 1 1 d . . . H14A H 0.1897 0.7185 0.1933 0.022 Uiso 1 1 d R . . C15 C 0.1887(2) 0.8565(2) 0.13021(11) 0.0170(5) Uani 1 1 d . . . H15A H 0.2193 0.8165 0.0997 0.020 Uiso 1 1 d R . . C16 C 0.1506(2) 0.9828(2) 0.13226(11) 0.0202(5) Uani 1 1 d . . . H16A H 0.1504 1.0409 0.1031 0.024 Uiso 1 1 d R . . B3 B -0.1127(2) 0.5472(3) 0.12009(12) 0.0144(5) Uani 1 1 d . . . H3 H -0.1858 0.6014 0.1118 0.017 Uiso 1 1 d R . . B4 B -0.0709(2) 0.4210(3) 0.07579(12) 0.0157(5) Uani 1 1 d . . . H4 H -0.1171 0.3925 0.0392 0.019 Uiso 1 1 d R . . B5 B -0.1145(2) 0.3868(3) 0.14444(13) 0.0160(5) Uani 1 1 d . . . H5 H -0.1888 0.3354 0.1526 0.019 Uiso 1 1 d R . . B6 B 0.0000 0.3093(4) 0.11643(17) 0.0163(8) Uani 1 2 d S . . H6 H 0.0000 0.2069 0.1060 0.020 Uiso 1 2 d SR . . B7 B 0.0699(2) 0.5123(3) 0.18858(12) 0.0159(5) Uani 1 1 d . . . H7 H 0.1155 0.5424 0.2252 0.019 Uiso 1 1 d R . . B8 B 0.0000 0.3650(4) 0.18701(18) 0.0169(8) Uani 1 2 d S . . H8 H 0.0000 0.2985 0.2224 0.020 Uiso 1 2 d SR . . Ti2 Ti 0.5000 0.22693(6) 0.01872(2) 0.01337(14) Uani 1 2 d S . . N3 N 0.5000 0.2877(3) 0.09811(13) 0.0147(6) Uani 1 2 d S . . N4 N 0.5000 0.4216(3) 0.17463(14) 0.0194(6) Uani 1 2 d S . . C21 C 0.5000 0.5117(3) 0.07714(15) 0.0141(7) Uani 1 2 d S . . C22 C 0.5000 0.4496(3) 0.01240(15) 0.0138(6) Uani 1 2 d S . . C23 C 0.5000 0.4065(3) 0.12165(16) 0.0152(7) Uani 1 2 d S . . C24 C 0.5000 0.1733(3) 0.13402(15) 0.0157(7) Uani 1 2 d S . . H24A H 0.5000 0.0985 0.1082 0.019 Uiso 1 2 calc SR . . C25 C 0.3994(2) 0.1581(2) 0.16949(11) 0.0177(5) Uani 1 1 d . . . H25A H 0.3949 0.2297 0.1962 0.021 Uiso 1 1 calc R . . H25B H 0.3361 0.1617 0.1453 0.021 Uiso 1 1 calc R . . C26 C 0.4002(2) 0.0312(3) 0.20105(12) 0.0224(6) Uani 1 1 d . . . H26A H 0.3978 -0.0406 0.1743 0.027 Uiso 1 1 calc R . . H26B H 0.3365 0.0258 0.2249 0.027 Uiso 1 1 calc R . . C27 C 0.5000 0.0194(4) 0.23701(17) 0.0216(8) Uani 1 2 d S . . H27A H 0.5000 -0.0644 0.2562 0.026 Uiso 1 2 calc SR . . H27B H 0.5000 0.0875 0.2655 0.026 Uiso 1 2 calc SR . . C28 C 0.5000 0.5415(3) 0.20517(16) 0.0180(7) Uani 1 2 d S . . H28A H 0.5000 0.6146 0.1784 0.022 Uiso 1 2 calc SR . . C29 C 0.4007(2) 0.5477(3) 0.24070(13) 0.0259(6) Uani 1 1 d . . . H29A H 0.3981 0.4723 0.2655 0.031 Uiso 1 1 calc R . . H29B H 0.3372 0.5456 0.2166 0.031 Uiso 1 1 calc R . . C30 C 0.4000(3) 0.6707(3) 0.27553(14) 0.0312(7) Uani 1 1 d . . . H30A H 0.3946 0.7456 0.2506 0.037 Uiso 1 1 calc R . . H30B H 0.3370 0.6706 0.3000 0.037 Uiso 1 1 calc R . . C31 C 0.5000 0.6828(4) 0.31082(18) 0.0342(10) Uani 1 2 d S . . H31A H 0.5000 0.6153 0.3396 0.041 Uiso 1 2 calc SR . . H31B H 0.5000 0.7668 0.3298 0.041 Uiso 1 2 calc SR . . C32 C 0.65060(19) 0.0870(2) 0.03162(11) 0.0162(5) Uani 1 1 d . . . H32A H 0.6504 0.0307 0.0615 0.019 Uiso 1 1 d R . . C33 C 0.6128(2) 0.0607(2) -0.02234(12) 0.0192(5) Uani 1 1 d . . . H33A H 0.5845 -0.0166 -0.0340 0.023 Uiso 1 1 d R . . C34 C 0.6245(2) 0.1715(2) -0.05466(11) 0.0196(5) Uani 1 1 d . . . H34A H 0.6047 0.1811 -0.0916 0.023 Uiso 1 1 d R . . C35 C 0.6726(2) 0.2662(2) -0.02080(11) 0.0173(5) Uani 1 1 d . . . H35A H 0.6900 0.3489 -0.0318 0.021 Uiso 1 1 d R . . C36 C 0.6890(2) 0.2143(2) 0.03228(11) 0.0175(5) Uani 1 1 d . . . H36A H 0.7197 0.2559 0.0623 0.021 Uiso 1 1 d R . . B23 B 0.3874(2) 0.5227(3) 0.03845(12) 0.0156(5) Uani 1 1 d . . . H23 H 0.3143 0.4690 0.0472 0.019 Uiso 1 1 d R . . B24 B 0.4293(2) 0.6506(3) 0.08190(13) 0.0168(5) Uani 1 1 d . . . H24 H 0.3836 0.6807 0.1185 0.020 Uiso 1 1 d R . . B25 B 0.4306(2) 0.5539(3) -0.03013(12) 0.0167(5) Uani 1 1 d . . . H25 H 0.3852 0.5219 -0.0665 0.020 Uiso 1 1 d R . . B26 B 0.3857(2) 0.6812(3) 0.01301(13) 0.0187(6) Uani 1 1 d . . . H26 H 0.3112 0.7321 0.0048 0.022 Uiso 1 1 d R . . B27 B 0.5000 0.7611(4) 0.03951(19) 0.0189(8) Uani 1 2 d S . . H27 H 0.5000 0.8644 0.0483 0.023 Uiso 1 2 d SR . . B28 B 0.5000 0.7022(4) -0.02983(19) 0.0198(8) Uani 1 2 d S . . H28 H 0.5000 0.7671 -0.0657 0.024 Uiso 1 2 d SR . . O1 O 0.2107(3) 0.2645(4) 0.29402(15) 0.0737(10) Uani 1 1 d . . . C41 C 0.3099(3) 0.2536(4) 0.33029(14) 0.0407(8) Uani 1 1 d . . . H41A H 0.3749 0.2532 0.3073 0.049 Uiso 1 1 calc R . . H41B H 0.3140 0.3256 0.3569 0.049 Uiso 1 1 calc R . . C42 C 0.2970(4) 0.1281(5) 0.36028(19) 0.0624(13) Uani 1 1 d . . . H42A H 0.3623 0.0762 0.3571 0.075 Uiso 1 1 calc R . . H42B H 0.2821 0.1430 0.4001 0.075 Uiso 1 1 calc R . . C43 C 0.2056(3) 0.0609(4) 0.33334(13) 0.0421(8) Uani 1 1 d . . . H43A H 0.2299 0.0082 0.3017 0.051 Uiso 1 1 calc R . . H43B H 0.1680 0.0055 0.3602 0.051 Uiso 1 1 calc R . . C44 C 0.1418(4) 0.1590(4) 0.3157(2) 0.0522(10) Uani 1 1 d . . . H44A H 0.0981 0.1908 0.3469 0.063 Uiso 1 1 calc R . . H44B H 0.0936 0.1284 0.2862 0.063 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 Ti1 0.0091(3) 0.0109(3) 0.0202(3) -0.0015(2) 0.000 0.000 N1 0.0114(13) 0.0098(13) 0.0176(15) 0.0020(11) 0.000 0.000 N2 0.0160(14) 0.0113(13) 0.0195(15) -0.0013(11) 0.000 0.000 C1 0.0115(15) 0.0107(15) 0.0164(16) -0.0014(13) 0.000 0.000 C2 0.0100(14) 0.0116(14) 0.0152(15) -0.0009(14) 0.000 0.000 C3 0.0088(15) 0.0128(16) 0.0193(17) 0.0003(13) 0.000 0.000 C4 0.0134(15) 0.0129(15) 0.0158(18) 0.0025(12) 0.000 0.000 C5 0.0127(11) 0.0156(11) 0.0211(12) 0.0022(10) 0.0021(9) -0.0009(9) C6 0.0144(12) 0.0176(11) 0.0255(13) 0.0054(10) 0.0008(10) -0.0026(9) C7 0.0196(19) 0.0188(17) 0.0262(19) 0.0092(15) 0.000 0.000 C8 0.0191(18) 0.0131(15) 0.0169(17) -0.0015(13) 0.000 0.000 C9 0.0243(15) 0.0220(13) 0.0304(15) -0.0044(11) 0.0088(12) -0.0033(11) C10 0.0308(16) 0.0259(15) 0.0345(16) -0.0101(12) 0.0122(13) -0.0035(12) C11 0.059(3) 0.030(2) 0.023(2) -0.0055(18) 0.000 0.000 C12 0.0144(12) 0.0170(11) 0.0315(14) -0.0069(11) -0.0049(11) -0.0009(10) C13 0.0190(13) 0.0224(13) 0.0220(13) -0.0038(10) -0.0047(10) -0.0041(10) C14 0.0132(11) 0.0162(11) 0.0259(13) -0.0005(11) -0.0057(10) -0.0026(10) C15 0.0094(11) 0.0156(11) 0.0259(14) -0.0018(9) -0.0022(10) -0.0021(9) C16 0.0136(11) 0.0163(11) 0.0308(15) 0.0002(10) -0.0034(10) -0.0030(10) B3 0.0100(12) 0.0161(13) 0.0171(12) -0.0006(10) 0.0001(10) -0.0014(10) B4 0.0154(12) 0.0122(12) 0.0196(13) -0.0002(10) 0.0016(10) -0.0017(10) B5 0.0149(12) 0.0131(12) 0.0200(12) -0.0015(11) 0.0021(12) -0.0027(10) B6 0.0160(18) 0.0135(17) 0.0194(19) -0.0003(16) 0.000 0.000 B7 0.0137(13) 0.0135(12) 0.0203(13) -0.0001(10) 0.0004(10) 0.0004(10) B8 0.018(2) 0.0152(17) 0.0176(19) 0.0007(16) 0.000 0.000 Ti2 0.0092(3) 0.0102(3) 0.0207(3) -0.0004(2) 0.000 0.000 N3 0.0119(14) 0.0123(14) 0.0199(15) -0.0008(12) 0.000 0.000 N4 0.0230(16) 0.0138(14) 0.0213(16) -0.0008(13) 0.000 0.000 C21 0.0111(16) 0.0124(15) 0.0188(16) -0.0021(13) 0.000 0.000 C22 0.0125(15) 0.0125(14) 0.0163(16) -0.0005(13) 0.000 0.000 C23 0.0092(15) 0.0142(16) 0.0222(17) 0.0004(14) 0.000 0.000 C24 0.0147(16) 0.0097(14) 0.023(2) -0.0014(13) 0.000 0.000 C25 0.0117(11) 0.0179(12) 0.0236(13) 0.0025(10) 0.0005(10) 0.0023(9) C26 0.0156(13) 0.0202(13) 0.0313(15) 0.0031(11) 0.0008(11) -0.0024(10) C27 0.0182(18) 0.0201(18) 0.0263(19) 0.0069(15) 0.000 0.000 C28 0.0202(19) 0.0128(16) 0.0212(18) -0.0003(14) 0.000 0.000 C29 0.0247(15) 0.0222(13) 0.0309(15) -0.0043(11) 0.0064(12) -0.0045(11) C30 0.0312(16) 0.0244(14) 0.0378(17) -0.0088(13) 0.0138(14) -0.0023(11) C31 0.059(3) 0.025(2) 0.0192(19) -0.0030(16) 0.000 0.000 C32 0.0112(11) 0.0138(11) 0.0237(13) 0.0016(9) 0.0025(9) 0.0040(9) C33 0.0119(11) 0.0153(11) 0.0303(14) -0.0053(10) 0.0021(10) 0.0024(9) C34 0.0161(12) 0.0220(13) 0.0206(12) -0.0016(10) 0.0005(10) 0.0021(10) C35 0.0129(11) 0.0148(11) 0.0240(13) -0.0006(10) 0.0059(10) 0.0021(9) C36 0.0118(11) 0.0166(12) 0.0239(14) -0.0005(9) -0.0001(10) 0.0021(9) B23 0.0132(12) 0.0131(12) 0.0203(13) -0.0002(11) -0.0023(11) 0.0020(10) B24 0.0143(12) 0.0113(12) 0.0246(14) -0.0017(10) -0.0003(11) 0.0009(10) B25 0.0133(13) 0.0146(12) 0.0222(13) 0.0021(11) -0.0015(11) 0.0017(10) B26 0.0178(13) 0.0143(12) 0.0239(14) 0.0011(11) -0.0029(12) 0.0014(11) B27 0.0179(19) 0.0112(17) 0.027(2) 0.0045(16) 0.000 0.000 B28 0.021(2) 0.0128(17) 0.026(2) 0.0027(17) 0.000 0.000 O1 0.076(2) 0.085(2) 0.060(2) -0.0003(18) -0.0078(18) 0.015(2) C41 0.044(2) 0.0499(19) 0.0284(15) 0.0043(14) 0.0008(14) 0.0035(17) C42 0.050(2) 0.089(3) 0.048(2) 0.035(2) 0.0052(19) 0.004(2) C43 0.061(2) 0.0417(18) 0.0238(14) 0.0041(13) 0.0030(15) -0.0058(17) C44 0.047(2) 0.044(2) 0.065(3) -0.0085(18) -0.019(2) -0.0062(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 N1 2.012(3) . ? Ti1 C2 2.339(3) . ? Ti1 C15 2.405(3) 3 ? Ti1 C15 2.405(3) . ? Ti1 C14 2.408(3) 3 ? Ti1 C14 2.408(3) . ? Ti1 C16 2.414(3) . ? Ti1 C16 2.414(3) 3 ? Ti1 C13 2.433(3) . ? Ti1 C13 2.433(3) 3 ? Ti1 C12 2.460(3) . ? Ti1 C12 2.460(3) 3 ? N1 C3 1.372(4) . ? N1 C4 1.481(4) . ? N2 C3 1.280(5) . ? N2 C8 1.452(4) . ? C1 C3 1.531(5) . ? C1 C2 1.700(5) . ? C1 B3 1.704(3) 3 ? C1 B3 1.704(3) . ? C1 B4 1.719(4) . ? C1 B4 1.719(4) 3 ? C2 B7 1.736(4) 3 ? C2 B7 1.736(4) . ? C2 B3 1.736(3) . ? C2 B3 1.736(3) 3 ? C4 C5 1.539(3) . ? C4 C5 1.539(3) 3 ? C4 H4A 1.0000 . ? C5 C6 1.534(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.523(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C6 1.523(3) 3 ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.532(3) 3 ? C8 C9 1.532(3) . ? C8 H8A 1.0000 . ? C9 C10 1.529(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.527(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C10 1.527(4) 3 ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.405(4) . ? C12 C16 1.414(4) . ? C12 H12A 0.9300 . ? C13 C14 1.412(4) . ? C13 H13A 0.9301 . ? C14 C15 1.413(4) . ? C14 H14A 0.9301 . ? C15 C16 1.407(3) . ? C15 H15A 0.9300 . ? C16 H16A 0.9298 . ? B3 B7 1.777(4) 3 ? B3 B5 1.777(4) . ? B3 B4 1.778(4) . ? B3 H3 1.0999 . ? B4 B6 1.767(5) . ? B4 B5 1.781(4) . ? B4 B4 1.787(6) 3 ? B4 H4 1.1001 . ? B5 B7 1.780(4) 3 ? B5 B8 1.786(4) . ? B5 B6 1.788(4) . ? B5 H5 1.0972 . ? B6 B4 1.767(5) 3 ? B6 B5 1.788(4) 3 ? B6 B8 1.800(6) . ? B6 H6 1.1000 . ? B7 B7 1.763(6) 3 ? B7 B8 1.775(5) . ? B7 B3 1.777(4) 3 ? B7 B5 1.780(4) 3 ? B7 H7 1.1000 . ? B8 B7 1.775(5) 3 ? B8 B5 1.786(4) 3 ? B8 H8 1.1000 . ? Ti2 N3 2.018(3) . ? Ti2 C22 2.333(3) . ? Ti2 C36 2.409(3) . ? Ti2 C36 2.409(3) 3_655 ? Ti2 C35 2.411(3) 3_655 ? Ti2 C35 2.411(3) . ? Ti2 C32 2.417(2) 3_655 ? Ti2 C32 2.417(2) . ? Ti2 C34 2.436(3) . ? Ti2 C34 2.436(3) 3_655 ? Ti2 C33 2.455(3) 3_655 ? Ti2 C33 2.455(3) . ? N3 C23 1.365(5) . ? N3 C24 1.478(4) . ? N4 C23 1.288(5) . ? N4 C28 1.453(5) . ? C21 C23 1.536(5) . ? C21 C22 1.692(5) . ? C21 B23 1.703(4) . ? C21 B23 1.703(4) 3_655 ? C21 B24 1.708(4) 3_655 ? C21 B24 1.708(4) . ? C22 B23 1.730(3) 3_655 ? C22 B23 1.730(3) . ? C22 B25 1.734(4) 3_655 ? C22 B25 1.734(4) . ? C24 C25 1.538(3) 3_655 ? C24 C25 1.538(3) . ? C24 H24A 1.0000 . ? C25 C26 1.530(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.533(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C26 1.533(3) 3_655 ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.519(3) 3_655 ? C28 C29 1.519(3) . ? C28 H28A 1.0000 . ? C29 C30 1.536(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.527(4) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C30 1.527(4) 3_655 ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.413(4) . ? C32 C36 1.417(3) . ? C32 H32A 0.9299 . ? C33 C34 1.404(4) . ? C33 H33A 0.9267 . ? C34 C35 1.420(4) . ? C34 H34A 0.9303 . ? C35 C36 1.406(4) . ? C35 H35A 0.9301 . ? C36 H36A 0.9301 . ? B23 B26 1.768(4) . ? B23 B25 1.772(4) . ? B23 B24 1.779(4) . ? B23 H23 1.0999 . ? B24 B26 1.780(4) . ? B24 B27 1.782(5) . ? B24 B24 1.783(6) 3_655 ? B24 H24 1.1000 . ? B25 B25 1.751(6) 3_655 ? B25 B28 1.780(5) . ? B25 B26 1.782(4) . ? B25 H25 1.1000 . ? B26 B27 1.785(4) . ? B26 B28 1.787(4) . ? B26 H26 1.0971 . ? B27 B24 1.782(5) 3_655 ? B27 B28 1.783(7) . ? B27 B26 1.785(4) 3_655 ? B27 H27 1.1001 . ? B28 B25 1.780(5) 3_655 ? B28 B26 1.787(4) 3_655 ? B28 H28 1.1001 . ? O1 C44 1.499(6) . ? O1 C41 1.530(5) . ? C41 C42 1.507(6) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.497(6) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.371(6) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ti1 C2 75.13(12) . . ? N1 Ti1 C15 83.81(7) . 3 ? C2 Ti1 C15 93.79(6) . 3 ? N1 Ti1 C15 83.81(7) . . ? C2 Ti1 C15 93.79(6) . . ? C15 Ti1 C15 163.31(13) 3 . ? N1 Ti1 C14 109.08(7) . 3 ? C2 Ti1 C14 78.80(7) . 3 ? C15 Ti1 C14 34.16(9) 3 3 ? C15 Ti1 C14 162.53(10) . 3 ? N1 Ti1 C14 109.08(7) . . ? C2 Ti1 C14 78.80(7) . . ? C15 Ti1 C14 162.53(10) 3 . ? C15 Ti1 C14 34.16(9) . . ? C14 Ti1 C14 128.37(14) 3 . ? N1 Ti1 C16 94.26(8) . . ? C2 Ti1 C16 127.72(6) . . ? C15 Ti1 C16 136.59(9) 3 . ? C15 Ti1 C16 33.95(8) . . ? C14 Ti1 C16 149.33(9) 3 . ? C14 Ti1 C16 56.25(9) . . ? N1 Ti1 C16 94.26(8) . 3 ? C2 Ti1 C16 127.72(6) . 3 ? C15 Ti1 C16 33.95(8) 3 3 ? C15 Ti1 C16 136.59(9) . 3 ? C14 Ti1 C16 56.25(9) 3 3 ? C14 Ti1 C16 149.33(9) . 3 ? C16 Ti1 C16 103.69(13) . 3 ? N1 Ti1 C13 140.13(7) . . ? C2 Ti1 C13 100.95(10) . . ? C15 Ti1 C13 135.86(10) 3 . ? C15 Ti1 C13 56.58(9) . . ? C14 Ti1 C13 108.91(10) 3 . ? C14 Ti1 C13 33.91(9) . . ? C16 Ti1 C13 56.18(9) . . ? C16 Ti1 C13 116.83(10) 3 . ? N1 Ti1 C13 140.13(7) . 3 ? C2 Ti1 C13 100.95(10) . 3 ? C15 Ti1 C13 56.58(9) 3 3 ? C15 Ti1 C13 135.86(10) . 3 ? C14 Ti1 C13 33.91(9) 3 3 ? C14 Ti1 C13 108.91(10) . 3 ? C16 Ti1 C13 116.83(10) . 3 ? C16 Ti1 C13 56.18(9) 3 3 ? C13 Ti1 C13 79.72(14) . 3 ? N1 Ti1 C12 127.64(9) . . ? C2 Ti1 C12 132.86(9) . . ? C15 Ti1 C12 125.79(9) 3 . ? C15 Ti1 C12 56.06(9) . . ? C14 Ti1 C12 118.44(10) 3 . ? C14 Ti1 C12 55.69(9) . . ? C16 Ti1 C12 33.72(9) . . ? C16 Ti1 C12 94.40(9) 3 . ? C13 Ti1 C12 33.37(9) . . ? C13 Ti1 C12 84.57(10) 3 . ? N1 Ti1 C12 127.64(9) . 3 ? C2 Ti1 C12 132.86(9) . 3 ? C15 Ti1 C12 56.06(9) 3 3 ? C15 Ti1 C12 125.79(9) . 3 ? C14 Ti1 C12 55.69(9) 3 3 ? C14 Ti1 C12 118.44(10) . 3 ? C16 Ti1 C12 94.40(9) . 3 ? C16 Ti1 C12 33.72(9) 3 3 ? C13 Ti1 C12 84.57(10) . 3 ? C13 Ti1 C12 33.37(9) 3 3 ? C12 Ti1 C12 70.57(13) . 3 ? C3 N1 C4 119.3(3) . . ? C3 N1 Ti1 133.7(3) . . ? C4 N1 Ti1 107.0(2) . . ? C3 N2 C8 127.6(3) . . ? C3 C1 C2 112.0(3) . . ? C3 C1 B3 115.63(16) . 3 ? C2 C1 B3 61.33(14) . 3 ? C3 C1 B3 115.63(16) . . ? C2 C1 B3 61.33(14) . . ? B3 C1 B3 113.0(3) 3 . ? C3 C1 B4 124.6(2) . . ? C2 C1 B4 112.3(2) . . ? B3 C1 B4 114.0(2) 3 . ? B3 C1 B4 62.60(15) . . ? C3 C1 B4 124.6(2) . 3 ? C2 C1 B4 112.3(2) . 3 ? B3 C1 B4 62.60(15) 3 3 ? B3 C1 B4 114.0(2) . 3 ? B4 C1 B4 62.7(2) . 3 ? C1 C2 B7 107.8(2) . 3 ? C1 C2 B7 107.8(2) . . ? B7 C2 B7 61.1(2) 3 . ? C1 C2 B3 59.45(14) . . ? B7 C2 B3 61.56(15) 3 . ? B7 C2 B3 110.8(2) . . ? C1 C2 B3 59.45(14) . 3 ? B7 C2 B3 110.8(2) 3 3 ? B7 C2 B3 61.56(15) . 3 ? B3 C2 B3 109.9(3) . 3 ? C1 C2 Ti1 108.6(2) . . ? B7 C2 Ti1 131.75(17) 3 . ? B7 C2 Ti1 131.75(17) . . ? B3 C2 Ti1 114.58(15) . . ? B3 C2 Ti1 114.58(15) 3 . ? N2 C3 N1 122.2(3) . . ? N2 C3 C1 127.3(3) . . ? N1 C3 C1 110.6(3) . . ? N1 C4 C5 114.37(17) . . ? N1 C4 C5 114.37(17) . 3 ? C5 C4 C5 111.1(3) . 3 ? N1 C4 H4A 105.3 . . ? C5 C4 H4A 105.3 . . ? C5 C4 H4A 105.3 3 . ? C6 C5 C4 110.3(2) . . ? C6 C5 H5A 109.6 . . ? C4 C5 H5A 109.6 . . ? C6 C5 H5B 109.6 . . ? C4 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? C7 C6 C5 110.8(2) . . ? C7 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C6 C7 C6 110.3(3) 3 . ? C6 C7 H7A 109.6 3 . ? C6 C7 H7A 109.6 . . ? C6 C7 H7B 109.6 3 . ? C6 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? N2 C8 C9 108.7(2) . 3 ? N2 C8 C9 108.7(2) . . ? C9 C8 C9 110.2(3) 3 . ? N2 C8 H8A 109.8 . . ? C9 C8 H8A 109.8 3 . ? C9 C8 H8A 109.8 . . ? C10 C9 C8 111.0(3) . . ? C10 C9 H9A 109.4 . . ? C8 C9 H9A 109.4 . . ? C10 C9 H9B 109.4 . . ? C8 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C11 C10 C9 111.8(3) . . ? C11 C10 H10A 109.3 . . ? C9 C10 H10A 109.3 . . ? C11 C10 H10B 109.3 . . ? C9 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? C10 C11 C10 110.8(4) . 3 ? C10 C11 H11A 109.5 . . ? C10 C11 H11A 109.5 3 . ? C10 C11 H11B 109.5 . . ? C10 C11 H11B 109.5 3 . ? H11A C11 H11B 108.1 . . ? C13 C12 C16 108.1(2) . . ? C13 C12 Ti1 72.29(15) . . ? C16 C12 Ti1 71.38(14) . . ? C13 C12 H12A 125.8 . . ? C16 C12 H12A 126.0 . . ? Ti1 C12 H12A 122.0 . . ? C12 C13 C14 107.6(2) . . ? C12 C13 Ti1 74.34(16) . . ? C14 C13 Ti1 72.04(15) . . ? C12 C13 H13A 126.2 . . ? C14 C13 H13A 126.2 . . ? Ti1 C13 H13A 119.3 . . ? C13 C14 C15 108.5(2) . . ? C13 C14 Ti1 74.04(15) . . ? C15 C14 Ti1 72.82(15) . . ? C13 C14 H14A 125.7 . . ? C15 C14 H14A 125.7 . . ? Ti1 C14 H14A 119.3 . . ? C16 C15 C14 107.4(2) . . ? C16 C15 Ti1 73.38(15) . . ? C14 C15 Ti1 73.02(15) . . ? C16 C15 H15A 126.2 . . ? C14 C15 H15A 126.4 . . ? Ti1 C15 H15A 119.1 . . ? C15 C16 C12 108.3(2) . . ? C15 C16 Ti1 72.67(15) . . ? C12 C16 Ti1 74.90(15) . . ? C15 C16 H16A 126.0 . . ? C12 C16 H16A 125.7 . . ? Ti1 C16 H16A 118.6 . . ? C1 B3 C2 59.22(17) . . ? C1 B3 B7 105.8(2) . 3 ? C2 B3 B7 59.21(17) . 3 ? C1 B3 B5 105.6(2) . . ? C2 B3 B5 107.0(2) . . ? B7 B3 B5 60.14(16) 3 . ? C1 B3 B4 59.11(17) . . ? C2 B3 B4 107.8(2) . . ? B7 B3 B4 108.4(2) 3 . ? B5 B3 B4 60.14(16) . . ? C1 B3 H3 123.8 . . ? C2 B3 H3 122.2 . . ? B7 B3 H3 122.0 3 . ? B5 B3 H3 122.4 . . ? B4 B3 H3 121.4 . . ? C1 B4 B6 104.7(2) . . ? C1 B4 B3 58.30(15) . . ? B6 B4 B3 107.9(2) . . ? C1 B4 B5 104.8(2) . . ? B6 B4 B5 60.52(16) . . ? B3 B4 B5 59.89(16) . . ? C1 B4 B4 58.67(11) . 3 ? B6 B4 B4 59.62(11) . 3 ? B3 B4 B4 107.25(12) . 3 ? B5 B4 B4 107.98(13) . 3 ? C1 B4 H4 124.8 . . ? B6 B4 H4 122.3 . . ? B3 B4 H4 121.8 . . ? B5 B4 H4 122.0 . . ? B4 B4 H4 122.0 3 . ? B3 B5 B7 59.92(15) . 3 ? B3 B5 B4 59.97(16) . . ? B7 B5 B4 108.13(19) 3 . ? B3 B5 B8 107.5(2) . . ? B7 B5 B8 59.68(19) 3 . ? B4 B5 B8 108.1(2) . . ? B3 B5 B6 107.0(2) . . ? B7 B5 B6 107.8(2) 3 . ? B4 B5 B6 59.35(19) . . ? B8 B5 B6 60.45(19) . . ? B3 B5 H5 122.2 . . ? B7 B5 H5 121.5 3 . ? B4 B5 H5 121.9 . . ? B8 B5 H5 121.6 . . ? B6 B5 H5 122.3 . . ? B4 B6 B4 60.8(2) . 3 ? B4 B6 B5 108.6(2) . 3 ? B4 B6 B5 60.13(17) 3 3 ? B4 B6 B5 60.13(17) . . ? B4 B6 B5 108.6(2) 3 . ? B5 B6 B5 107.7(3) 3 . ? B4 B6 B8 108.1(2) . . ? B4 B6 B8 108.1(2) 3 . ? B5 B6 B8 59.72(16) 3 . ? B5 B6 B8 59.72(16) . . ? B4 B6 H6 121.1 . . ? B4 B6 H6 121.1 3 . ? B5 B6 H6 121.9 3 . ? B5 B6 H6 121.9 . . ? B8 B6 H6 122.1 . . ? C2 B7 B7 59.47(11) . 3 ? C2 B7 B8 107.0(2) . . ? B7 B7 B8 60.21(11) 3 . ? C2 B7 B3 59.24(15) . 3 ? B7 B7 B3 107.67(13) 3 3 ? B8 B7 B3 108.0(2) . 3 ? C2 B7 B5 106.9(2) . 3 ? B7 B7 B5 108.40(13) 3 3 ? B8 B7 B5 60.33(17) . 3 ? B3 B7 B5 59.94(16) 3 3 ? C2 B7 H7 122.8 . . ? B7 B7 H7 121.5 3 . ? B8 B7 H7 121.7 . . ? B3 B7 H7 122.0 3 . ? B5 B7 H7 121.8 3 . ? B7 B8 B7 59.6(2) . 3 ? B7 B8 B5 107.6(2) . . ? B7 B8 B5 59.99(16) 3 . ? B7 B8 B5 59.99(16) . 3 ? B7 B8 B5 107.6(2) 3 3 ? B5 B8 B5 107.8(3) . 3 ? B7 B8 B6 107.5(2) . . ? B7 B8 B6 107.5(2) 3 . ? B5 B8 B6 59.83(16) . . ? B5 B8 B6 59.83(16) 3 . ? B7 B8 H8 122.1 . . ? B7 B8 H8 122.1 3 . ? B5 B8 H8 121.8 . . ? B5 B8 H8 121.8 3 . ? B6 B8 H8 122.0 . . ? N3 Ti2 C22 75.39(13) . . ? N3 Ti2 C36 83.59(7) . . ? C22 Ti2 C36 93.64(6) . . ? N3 Ti2 C36 83.59(7) . 3_655 ? C22 Ti2 C36 93.64(6) . 3_655 ? C36 Ti2 C36 163.16(13) . 3_655 ? N3 Ti2 C35 108.77(7) . 3_655 ? C22 Ti2 C35 78.71(7) . 3_655 ? C36 Ti2 C35 162.91(9) . 3_655 ? C36 Ti2 C35 33.93(9) 3_655 3_655 ? N3 Ti2 C35 108.77(7) . . ? C22 Ti2 C35 78.71(7) . . ? C36 Ti2 C35 33.93(9) . . ? C36 Ti2 C35 162.91(9) 3_655 . ? C35 Ti2 C35 128.98(13) 3_655 . ? N3 Ti2 C32 93.92(8) . 3_655 ? C22 Ti2 C32 127.76(6) . 3_655 ? C36 Ti2 C32 136.59(9) . 3_655 ? C36 Ti2 C32 34.14(8) 3_655 3_655 ? C35 Ti2 C32 56.29(8) 3_655 3_655 ? C35 Ti2 C32 149.65(9) . 3_655 ? N3 Ti2 C32 93.92(8) . . ? C22 Ti2 C32 127.76(6) . . ? C36 Ti2 C32 34.14(8) . . ? C36 Ti2 C32 136.59(9) 3_655 . ? C35 Ti2 C32 149.65(9) 3_655 . ? C35 Ti2 C32 56.29(8) . . ? C32 Ti2 C32 103.54(12) 3_655 . ? N3 Ti2 C34 139.88(7) . . ? C22 Ti2 C34 100.95(9) . . ? C36 Ti2 C34 56.51(9) . . ? C36 Ti2 C34 136.31(9) 3_655 . ? C35 Ti2 C34 109.55(10) 3_655 . ? C35 Ti2 C34 34.05(9) . . ? C32 Ti2 C34 117.11(9) 3_655 . ? C32 Ti2 C34 56.18(9) . . ? N3 Ti2 C34 139.88(7) . 3_655 ? C22 Ti2 C34 100.95(9) . 3_655 ? C36 Ti2 C34 136.31(9) . 3_655 ? C36 Ti2 C34 56.51(9) 3_655 3_655 ? C35 Ti2 C34 34.05(9) 3_655 3_655 ? C35 Ti2 C34 109.55(10) . 3_655 ? C32 Ti2 C34 56.18(9) 3_655 3_655 ? C32 Ti2 C34 117.11(9) . 3_655 ? C34 Ti2 C34 80.24(13) . 3_655 ? N3 Ti2 C33 127.30(9) . 3_655 ? C22 Ti2 C33 132.85(9) . 3_655 ? C36 Ti2 C33 126.11(9) . 3_655 ? C36 Ti2 C33 56.14(9) 3_655 3_655 ? C35 Ti2 C33 55.80(8) 3_655 3_655 ? C35 Ti2 C33 118.95(9) . 3_655 ? C32 Ti2 C33 33.71(9) 3_655 3_655 ? C32 Ti2 C33 94.51(9) . 3_655 ? C34 Ti2 C33 84.93(9) . 3_655 ? C34 Ti2 C33 33.36(9) 3_655 3_655 ? N3 Ti2 C33 127.30(9) . . ? C22 Ti2 C33 132.85(9) . . ? C36 Ti2 C33 56.14(9) . . ? C36 Ti2 C33 126.11(9) 3_655 . ? C35 Ti2 C33 118.95(9) 3_655 . ? C35 Ti2 C33 55.80(8) . . ? C32 Ti2 C33 94.51(9) 3_655 . ? C32 Ti2 C33 33.71(9) . . ? C34 Ti2 C33 33.36(9) . . ? C34 Ti2 C33 84.93(9) 3_655 . ? C33 Ti2 C33 70.83(13) 3_655 . ? C23 N3 C24 119.5(3) . . ? C23 N3 Ti2 132.9(3) . . ? C24 N3 Ti2 107.5(2) . . ? C23 N4 C28 127.5(3) . . ? C23 C21 C22 111.8(3) . . ? C23 C21 B23 115.57(17) . . ? C22 C21 B23 61.29(15) . . ? C23 C21 B23 115.57(17) . 3_655 ? C22 C21 B23 61.29(15) . 3_655 ? B23 C21 B23 112.9(3) . 3_655 ? C23 C21 B24 124.1(2) . 3_655 ? C22 C21 B24 112.8(2) . 3_655 ? B23 C21 B24 114.5(2) . 3_655 ? B23 C21 B24 62.88(16) 3_655 3_655 ? C23 C21 B24 124.1(2) . . ? C22 C21 B24 112.8(2) . . ? B23 C21 B24 62.88(16) . . ? B23 C21 B24 114.5(2) 3_655 . ? B24 C21 B24 62.9(2) 3_655 . ? C21 C22 B23 59.68(15) . 3_655 ? C21 C22 B23 59.68(15) . . ? B23 C22 B23 110.3(3) 3_655 . ? C21 C22 B25 107.8(2) . 3_655 ? B23 C22 B25 61.53(16) 3_655 3_655 ? B23 C22 B25 110.6(2) . 3_655 ? C21 C22 B25 107.8(2) . . ? B23 C22 B25 110.6(2) 3_655 . ? B23 C22 B25 61.53(16) . . ? B25 C22 B25 60.6(2) 3_655 . ? C21 C22 Ti2 108.8(2) . . ? B23 C22 Ti2 114.64(15) 3_655 . ? B23 C22 Ti2 114.64(15) . . ? B25 C22 Ti2 131.76(18) 3_655 . ? B25 C22 Ti2 131.76(18) . . ? N4 C23 N3 121.6(3) . . ? N4 C23 C21 127.3(3) . . ? N3 C23 C21 111.1(3) . . ? N3 C24 C25 114.20(17) . 3_655 ? N3 C24 C25 114.20(17) . . ? C25 C24 C25 111.1(3) 3_655 . ? N3 C24 H24A 105.5 . . ? C25 C24 H24A 105.5 3_655 . ? C25 C24 H24A 105.5 . . ? C26 C25 C24 111.2(2) . . ? C26 C25 H25A 109.4 . . ? C24 C25 H25A 109.4 . . ? C26 C25 H25B 109.4 . . ? C24 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? C25 C26 C27 110.9(2) . . ? C25 C26 H26A 109.5 . . ? C27 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C27 C26 H26B 109.5 . . ? H26A C26 H26B 108.0 . . ? C26 C27 C26 110.3(3) . 3_655 ? C26 C27 H27A 109.6 . . ? C26 C27 H27A 109.6 3_655 . ? C26 C27 H27B 109.6 . . ? C26 C27 H27B 109.6 3_655 . ? H27A C27 H27B 108.1 . . ? N4 C28 C29 108.8(2) . 3_655 ? N4 C28 C29 108.8(2) . . ? C29 C28 C29 111.0(3) 3_655 . ? N4 C28 H28A 109.4 . . ? C29 C28 H28A 109.4 3_655 . ? C29 C28 H28A 109.4 . . ? C28 C29 C30 110.5(3) . . ? C28 C29 H29A 109.6 . . ? C30 C29 H29A 109.6 . . ? C28 C29 H29B 109.6 . . ? C30 C29 H29B 109.6 . . ? H29A C29 H29B 108.1 . . ? C31 C30 C29 111.7(3) . . ? C31 C30 H30A 109.3 . . ? C29 C30 H30A 109.3 . . ? C31 C30 H30B 109.3 . . ? C29 C30 H30B 109.3 . . ? H30A C30 H30B 107.9 . . ? C30 C31 C30 111.3(4) . 3_655 ? C30 C31 H31A 109.4 . . ? C30 C31 H31A 109.4 3_655 . ? C30 C31 H31B 109.4 . . ? C30 C31 H31B 109.4 3_655 . ? H31A C31 H31B 108.0 . . ? C33 C32 C36 108.0(2) . . ? C33 C32 Ti2 74.61(14) . . ? C36 C32 Ti2 72.61(15) . . ? C33 C32 H32A 126.1 . . ? C36 C32 H32A 125.9 . . ? Ti2 C32 H32A 118.7 . . ? C34 C33 C32 108.4(2) . . ? C34 C33 Ti2 72.59(15) . . ? C32 C33 Ti2 71.68(14) . . ? C34 C33 H33A 126.1 . . ? C32 C33 H33A 125.4 . . ? Ti2 C33 H33A 121.1 . . ? C33 C34 C35 107.5(2) . . ? C33 C34 Ti2 74.05(16) . . ? C35 C34 Ti2 71.99(15) . . ? C33 C34 H34A 126.3 . . ? C35 C34 H34A 126.2 . . ? Ti2 C34 H34A 119.8 . . ? C36 C35 C34 108.5(2) . . ? C36 C35 Ti2 72.96(15) . . ? C34 C35 Ti2 73.96(15) . . ? C36 C35 H35A 125.6 . . ? C34 C35 H35A 125.8 . . ? Ti2 C35 H35A 118.9 . . ? C35 C36 C32 107.6(2) . . ? C35 C36 Ti2 73.11(15) . . ? C32 C36 Ti2 73.26(15) . . ? C35 C36 H36A 126.2 . . ? C32 C36 H36A 126.2 . . ? Ti2 C36 H36A 119.5 . . ? C21 B23 C22 59.03(18) . . ? C21 B23 B26 105.3(2) . . ? C22 B23 B26 107.3(2) . . ? C21 B23 B25 105.6(2) . . ? C22 B23 B25 59.34(17) . . ? B26 B23 B25 60.47(17) . . ? C21 B23 B24 58.69(17) . . ? C22 B23 B24 107.6(2) . . ? B26 B23 B24 60.24(16) . . ? B25 B23 B24 108.7(2) . . ? C21 B23 H23 124.0 . . ? C22 B23 H23 122.1 . . ? B26 B23 H23 122.3 . . ? B25 B23 H23 122.0 . . ? B24 B23 H23 121.3 . . ? C21 B24 B23 58.43(15) . . ? C21 B24 B26 104.6(2) . . ? B23 B24 B26 59.55(16) . . ? C21 B24 B27 104.6(2) . . ? B23 B24 B27 107.3(2) . . ? B26 B24 B27 60.13(18) . . ? C21 B24 B24 58.54(11) . 3_655 ? B23 B24 B24 107.27(13) . 3_655 ? B26 B24 B24 108.00(14) . 3_655 ? B27 B24 B24 59.99(11) . 3_655 ? C21 B24 H24 124.8 . . ? B23 B24 H24 122.2 . . ? B26 B24 H24 122.4 . . ? B27 B24 H24 122.4 . . ? B24 B24 H24 121.6 3_655 . ? C22 B25 B25 59.69(11) . 3_655 ? C22 B25 B23 59.13(16) . . ? B25 B25 B23 107.89(13) 3_655 . ? C22 B25 B28 107.3(2) . . ? B25 B25 B28 60.55(11) 3_655 . ? B23 B25 B28 107.9(2) . . ? C22 B25 B26 106.5(2) . . ? B25 B25 B26 108.53(13) 3_655 . ? B23 B25 B26 59.64(16) . . ? B28 B25 B26 60.22(18) . . ? C22 B25 H25 122.9 . . ? B25 B25 H25 121.3 3_655 . ? B23 B25 H25 122.0 . . ? B28 B25 H25 121.6 . . ? B26 B25 H25 121.9 . . ? B23 B26 B24 60.20(17) . . ? B23 B26 B25 59.89(16) . . ? B24 B26 B25 108.2(2) . . ? B23 B26 B27 107.7(2) . . ? B24 B26 B27 60.00(19) . . ? B25 B26 B27 107.6(2) . . ? B23 B26 B28 107.8(2) . . ? B24 B26 B28 108.2(2) . . ? B25 B26 B28 59.83(19) . . ? B27 B26 B28 59.9(2) . . ? B23 B26 H26 121.9 . . ? B24 B26 H26 121.4 . . ? B25 B26 H26 121.9 . . ? B27 B26 H26 121.9 . . ? B28 B26 H26 121.8 . . ? B24 B27 B24 60.0(2) 3_655 . ? B24 B27 B28 108.3(2) 3_655 . ? B24 B27 B28 108.3(2) . . ? B24 B27 B26 107.8(2) 3_655 . ? B24 B27 B26 59.87(16) . . ? B28 B27 B26 60.13(17) . . ? B24 B27 B26 59.87(16) 3_655 3_655 ? B24 B27 B26 107.8(2) . 3_655 ? B28 B27 B26 60.13(17) . 3_655 ? B26 B27 B26 107.8(3) . 3_655 ? B24 B27 H27 121.7 3_655 . ? B24 B27 H27 121.7 . . ? B28 B27 H27 121.3 . . ? B26 B27 H27 121.9 . . ? B26 B27 H27 121.9 3_655 . ? B25 B28 B25 58.9(2) . 3_655 ? B25 B28 B27 107.7(3) . . ? B25 B28 B27 107.7(3) 3_655 . ? B25 B28 B26 107.0(3) . 3_655 ? B25 B28 B26 59.94(16) 3_655 3_655 ? B27 B28 B26 59.97(17) . 3_655 ? B25 B28 B26 59.94(16) . . ? B25 B28 B26 107.0(3) 3_655 . ? B27 B28 B26 59.97(17) . . ? B26 B28 B26 107.5(3) 3_655 . ? B25 B28 H28 122.3 . . ? B25 B28 H28 122.3 3_655 . ? B27 B28 H28 121.7 . . ? B26 B28 H28 122.1 3_655 . ? B26 B28 H28 122.1 . . ? C44 O1 C41 102.7(3) . . ? C42 C41 O1 104.5(3) . . ? C42 C41 H41A 110.8 . . ? O1 C41 H41A 110.8 . . ? C42 C41 H41B 110.8 . . ? O1 C41 H41B 110.8 . . ? H41A C41 H41B 108.9 . . ? C43 C42 C41 106.5(3) . . ? C43 C42 H42A 110.4 . . ? C41 C42 H42A 110.4 . . ? C43 C42 H42B 110.4 . . ? C41 C42 H42B 110.4 . . ? H42A C42 H42B 108.6 . . ? C44 C43 C42 103.6(3) . . ? C44 C43 H43A 111.0 . . ? C42 C43 H43A 111.0 . . ? C44 C43 H43B 111.0 . . ? C42 C43 H43B 111.0 . . ? H43A C43 H43B 109.0 . . ? C43 C44 O1 108.5(4) . . ? C43 C44 H44A 110.0 . . ? O1 C44 H44A 110.0 . . ? C43 C44 H44B 110.0 . . ? O1 C44 H44B 110.0 . . ? H44A C44 H44B 108.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Ti1 N1 C3 0.0 . . . . ? C15 Ti1 N1 C3 -95.60(6) 3 . . . ? C15 Ti1 N1 C3 95.60(6) . . . . ? C14 Ti1 N1 C3 -72.27(7) 3 . . . ? C14 Ti1 N1 C3 72.27(7) . . . . ? C16 Ti1 N1 C3 127.95(6) . . . . ? C16 Ti1 N1 C3 -127.95(6) 3 . . . ? C13 Ti1 N1 C3 89.36(15) . . . . ? C13 Ti1 N1 C3 -89.36(15) 3 . . . ? C12 Ti1 N1 C3 133.16(10) . . . . ? C12 Ti1 N1 C3 -133.16(10) 3 . . . ? C2 Ti1 N1 C4 180.0 . . . . ? C15 Ti1 N1 C4 84.40(6) 3 . . . ? C15 Ti1 N1 C4 -84.40(6) . . . . ? C14 Ti1 N1 C4 107.73(7) 3 . . . ? C14 Ti1 N1 C4 -107.73(7) . . . . ? C16 Ti1 N1 C4 -52.05(6) . . . . ? C16 Ti1 N1 C4 52.05(6) 3 . . . ? C13 Ti1 N1 C4 -90.64(15) . . . . ? C13 Ti1 N1 C4 90.64(15) 3 . . . ? C12 Ti1 N1 C4 -46.84(10) . . . . ? C12 Ti1 N1 C4 46.84(10) 3 . . . ? C3 C1 C2 B7 147.76(13) . . . 3 ? B3 C1 C2 B7 -104.1(2) 3 . . 3 ? B3 C1 C2 B7 39.63(17) . . . 3 ? B4 C1 C2 B7 2.0(2) . . . 3 ? B4 C1 C2 B7 -66.44(17) 3 . . 3 ? C3 C1 C2 B7 -147.76(13) . . . . ? B3 C1 C2 B7 -39.63(17) 3 . . . ? B3 C1 C2 B7 104.1(2) . . . . ? B4 C1 C2 B7 66.44(17) . . . . ? B4 C1 C2 B7 -2.0(2) 3 . . . ? C3 C1 C2 B3 108.13(14) . . . . ? B3 C1 C2 B3 -143.7(3) 3 . . . ? B4 C1 C2 B3 -37.68(17) . . . . ? B4 C1 C2 B3 -106.1(2) 3 . . . ? C3 C1 C2 B3 -108.13(14) . . . 3 ? B3 C1 C2 B3 143.7(3) . . . 3 ? B4 C1 C2 B3 106.1(2) . . . 3 ? B4 C1 C2 B3 37.68(17) 3 . . 3 ? C3 C1 C2 Ti1 0.0 . . . . ? B3 C1 C2 Ti1 108.13(14) 3 . . . ? B3 C1 C2 Ti1 -108.13(14) . . . . ? B4 C1 C2 Ti1 -145.81(14) . . . . ? B4 C1 C2 Ti1 145.81(14) 3 . . . ? N1 Ti1 C2 C1 0.0 . . . . ? C15 Ti1 C2 C1 82.56(7) 3 . . . ? C15 Ti1 C2 C1 -82.56(7) . . . . ? C14 Ti1 C2 C1 113.41(7) 3 . . . ? C14 Ti1 C2 C1 -113.41(7) . . . . ? C16 Ti1 C2 C1 -83.79(11) . . . . ? C16 Ti1 C2 C1 83.79(11) 3 . . . ? C13 Ti1 C2 C1 -139.24(7) . . . . ? C13 Ti1 C2 C1 139.24(7) 3 . . . ? C12 Ti1 C2 C1 -128.00(12) . . . . ? C12 Ti1 C2 C1 128.00(12) 3 . . . ? N1 Ti1 C2 B7 -137.1(2) . . . 3 ? C15 Ti1 C2 B7 -54.5(2) 3 . . 3 ? C15 Ti1 C2 B7 140.3(2) . . . 3 ? C14 Ti1 C2 B7 -23.7(2) 3 . . 3 ? C14 Ti1 C2 B7 109.5(2) . . . 3 ? C16 Ti1 C2 B7 139.12(18) . . . 3 ? C16 Ti1 C2 B7 -53.3(3) 3 . . 3 ? C13 Ti1 C2 B7 83.7(2) . . . 3 ? C13 Ti1 C2 B7 2.2(2) 3 . . 3 ? C12 Ti1 C2 B7 94.91(18) . . . 3 ? C12 Ti1 C2 B7 -9.1(3) 3 . . 3 ? N1 Ti1 C2 B7 137.1(2) . . . . ? C15 Ti1 C2 B7 -140.3(2) 3 . . . ? C15 Ti1 C2 B7 54.5(2) . . . . ? C14 Ti1 C2 B7 -109.5(2) 3 . . . ? C14 Ti1 C2 B7 23.7(2) . . . . ? C16 Ti1 C2 B7 53.3(3) . . . . ? C16 Ti1 C2 B7 -139.12(18) 3 . . . ? C13 Ti1 C2 B7 -2.2(2) . . . . ? C13 Ti1 C2 B7 -83.7(2) 3 . . . ? C12 Ti1 C2 B7 9.1(3) . . . . ? C12 Ti1 C2 B7 -94.91(18) 3 . . . ? N1 Ti1 C2 B3 -64.17(19) . . . . ? C15 Ti1 C2 B3 18.4(2) 3 . . . ? C15 Ti1 C2 B3 -146.7(2) . . . . ? C14 Ti1 C2 B3 49.24(19) 3 . . . ? C14 Ti1 C2 B3 -177.6(2) . . . . ? C16 Ti1 C2 B3 -147.96(16) . . . . ? C16 Ti1 C2 B3 19.6(3) 3 . . . ? C13 Ti1 C2 B3 156.59(19) . . . . ? C13 Ti1 C2 B3 75.1(2) 3 . . . ? C12 Ti1 C2 B3 167.84(17) . . . . ? C12 Ti1 C2 B3 63.8(3) 3 . . . ? N1 Ti1 C2 B3 64.17(19) . . . 3 ? C15 Ti1 C2 B3 146.7(2) 3 . . 3 ? C15 Ti1 C2 B3 -18.4(2) . . . 3 ? C14 Ti1 C2 B3 177.6(2) 3 . . 3 ? C14 Ti1 C2 B3 -49.24(19) . . . 3 ? C16 Ti1 C2 B3 -19.6(3) . . . 3 ? C16 Ti1 C2 B3 147.96(16) 3 . . 3 ? C13 Ti1 C2 B3 -75.1(2) . . . 3 ? C13 Ti1 C2 B3 -156.59(19) 3 . . 3 ? C12 Ti1 C2 B3 -63.8(3) . . . 3 ? C12 Ti1 C2 B3 -167.84(17) 3 . . 3 ? C8 N2 C3 N1 180.0 . . . . ? C8 N2 C3 C1 0.0 . . . . ? C4 N1 C3 N2 0.0 . . . . ? Ti1 N1 C3 N2 180.0 . . . . ? C4 N1 C3 C1 180.0 . . . . ? Ti1 N1 C3 C1 0.0 . . . . ? C2 C1 C3 N2 180.0 . . . . ? B3 C1 C3 N2 112.4(2) 3 . . . ? B3 C1 C3 N2 -112.4(2) . . . . ? B4 C1 C3 N2 -39.2(2) . . . . ? B4 C1 C3 N2 39.2(2) 3 . . . ? C2 C1 C3 N1 0.0 . . . . ? B3 C1 C3 N1 -67.6(2) 3 . . . ? B3 C1 C3 N1 67.6(2) . . . . ? B4 C1 C3 N1 140.8(2) . . . . ? B4 C1 C3 N1 -140.8(2) 3 . . . ? C3 N1 C4 C5 -64.8(2) . . . . ? Ti1 N1 C4 C5 115.2(2) . . . . ? C3 N1 C4 C5 64.8(2) . . . 3 ? Ti1 N1 C4 C5 -115.2(2) . . . 3 ? N1 C4 C5 C6 -172.9(2) . . . . ? C5 C4 C5 C6 55.9(3) 3 . . . ? C4 C5 C6 C7 -57.1(3) . . . . ? C5 C6 C7 C6 58.5(4) . . . 3 ? C3 N2 C8 C9 120.1(2) . . . 3 ? C3 N2 C8 C9 -120.1(2) . . . . ? N2 C8 C9 C10 -175.7(3) . . . . ? C9 C8 C9 C10 -56.8(4) 3 . . . ? C8 C9 C10 C11 56.2(4) . . . . ? C9 C10 C11 C10 -54.7(5) . . . 3 ? N1 Ti1 C12 C13 -126.25(17) . . . . ? C2 Ti1 C12 C13 -20.4(2) . . . . ? C15 Ti1 C12 C13 120.92(17) 3 . . . ? C15 Ti1 C12 C13 -79.33(18) . . . . ? C14 Ti1 C12 C13 81.24(18) 3 . . . ? C14 Ti1 C12 C13 -37.77(16) . . . . ? C16 Ti1 C12 C13 -116.9(2) . . . . ? C16 Ti1 C12 C13 134.93(17) 3 . . . ? C13 Ti1 C12 C13 79.5(2) 3 . . . ? C12 Ti1 C12 C13 110.68(16) 3 . . . ? N1 Ti1 C12 C16 -9.38(19) . . . . ? C2 Ti1 C12 C16 96.50(19) . . . . ? C15 Ti1 C12 C16 -122.22(16) 3 . . . ? C15 Ti1 C12 C16 37.54(14) . . . . ? C14 Ti1 C12 C16 -161.89(15) 3 . . . ? C14 Ti1 C12 C16 79.09(17) . . . . ? C16 Ti1 C12 C16 -108.20(19) 3 . . . ? C13 Ti1 C12 C16 116.9(2) . . . . ? C13 Ti1 C12 C16 -163.59(16) 3 . . . ? C12 Ti1 C12 C16 -132.46(13) 3 . . . ? C16 C12 C13 C14 2.0(3) . . . . ? Ti1 C12 C13 C14 64.85(18) . . . . ? C16 C12 C13 Ti1 -62.80(18) . . . . ? N1 Ti1 C13 C12 85.1(2) . . . . ? C2 Ti1 C13 C12 164.94(17) . . . . ? C15 Ti1 C13 C12 -87.8(2) 3 . . . ? C15 Ti1 C13 C12 77.63(17) . . . . ? C14 Ti1 C13 C12 -113.28(17) 3 . . . ? C14 Ti1 C13 C12 114.9(2) . . . . ? C16 Ti1 C13 C12 36.59(16) . . . . ? C16 Ti1 C13 C12 -52.28(19) 3 . . . ? C13 Ti1 C13 C12 -95.76(17) 3 . . . ? C12 Ti1 C13 C12 -62.41(18) 3 . . . ? N1 Ti1 C13 C14 -29.9(2) . . . . ? C2 Ti1 C13 C14 50.01(17) . . . . ? C15 Ti1 C13 C14 157.24(16) 3 . . . ? C15 Ti1 C13 C14 -37.30(15) . . . . ? C14 Ti1 C13 C14 131.80(19) 3 . . . ? C16 Ti1 C13 C14 -78.34(17) . . . . ? C16 Ti1 C13 C14 -167.21(15) 3 . . . ? C13 Ti1 C13 C14 149.31(13) 3 . . . ? C12 Ti1 C13 C14 -114.9(2) . . . . ? C12 Ti1 C13 C14 -177.33(17) 3 . . . ? C12 C13 C14 C15 -1.2(3) . . . . ? Ti1 C13 C14 C15 65.18(18) . . . . ? C12 C13 C14 Ti1 -66.38(19) . . . . ? N1 Ti1 C14 C13 160.27(16) . . . . ? C2 Ti1 C14 C13 -129.93(18) . . . . ? C15 Ti1 C14 C13 -63.8(4) 3 . . . ? C15 Ti1 C14 C13 115.7(2) . . . . ? C14 Ti1 C14 C13 -64.1(2) 3 . . . ? C16 Ti1 C14 C13 78.12(17) . . . . ? C16 Ti1 C14 C13 22.8(3) 3 . . . ? C13 Ti1 C14 C13 -32.06(15) 3 . . . ? C12 Ti1 C14 C13 37.15(16) . . . . ? C12 Ti1 C14 C13 3.02(19) 3 . . . ? N1 Ti1 C14 C15 44.53(17) . . . . ? C2 Ti1 C14 C15 114.34(17) . . . . ? C15 Ti1 C14 C15 -179.5(3) 3 . . . ? C14 Ti1 C14 C15 -179.84(12) 3 . . . ? C16 Ti1 C14 C15 -37.62(14) . . . . ? C16 Ti1 C14 C15 -92.9(2) 3 . . . ? C13 Ti1 C14 C15 -115.7(2) . . . . ? C13 Ti1 C14 C15 -147.79(15) 3 . . . ? C12 Ti1 C14 C15 -78.58(16) . . . . ? C12 Ti1 C14 C15 -112.71(16) 3 . . . ? C13 C14 C15 C16 -0.1(3) . . . . ? Ti1 C14 C15 C16 65.86(18) . . . . ? C13 C14 C15 Ti1 -65.98(18) . . . . ? N1 Ti1 C15 C16 107.15(17) . . . . ? C2 Ti1 C15 C16 -178.27(17) . . . . ? C15 Ti1 C15 C16 64.8(5) 3 . . . ? C14 Ti1 C15 C16 -114.2(3) 3 . . . ? C14 Ti1 C15 C16 -114.7(2) . . . . ? C16 Ti1 C15 C16 17.49(17) 3 . . . ? C13 Ti1 C15 C16 -77.64(17) . . . . ? C13 Ti1 C15 C16 -68.3(2) 3 . . . ? C12 Ti1 C15 C16 -37.28(16) . . . . ? C12 Ti1 C15 C16 -25.6(2) 3 . . . ? N1 Ti1 C15 C14 -138.19(17) . . . . ? C2 Ti1 C15 C14 -63.60(17) . . . . ? C15 Ti1 C15 C14 179.5(4) 3 . . . ? C14 Ti1 C15 C14 0.4(3) 3 . . . ? C16 Ti1 C15 C14 114.7(2) . . . . ? C16 Ti1 C15 C14 132.15(16) 3 . . . ? C13 Ti1 C15 C14 37.02(15) . . . . ? C13 Ti1 C15 C14 46.4(2) 3 . . . ? C12 Ti1 C15 C14 77.39(16) . . . . ? C12 Ti1 C15 C14 89.04(17) 3 . . . ? C14 C15 C16 C12 1.4(3) . . . . ? Ti1 C15 C16 C12 67.01(18) . . . . ? C14 C15 C16 Ti1 -65.61(17) . . . . ? C13 C12 C16 C15 -2.1(3) . . . . ? Ti1 C12 C16 C15 -65.53(18) . . . . ? C13 C12 C16 Ti1 63.39(19) . . . . ? N1 Ti1 C16 C15 -72.29(16) . . . . ? C2 Ti1 C16 C15 2.2(2) . . . . ? C15 Ti1 C16 C15 -157.8(2) 3 . . . ? C14 Ti1 C16 C15 147.54(19) 3 . . . ? C14 Ti1 C16 C15 37.86(15) . . . . ? C16 Ti1 C16 C15 -167.73(12) 3 . . . ? C13 Ti1 C16 C15 78.94(17) . . . . ? C13 Ti1 C16 C15 133.53(16) 3 . . . ? C12 Ti1 C16 C15 115.1(2) . . . . ? C12 Ti1 C16 C15 159.40(16) 3 . . . ? N1 Ti1 C16 C12 172.56(16) . . . . ? C2 Ti1 C16 C12 -112.96(19) . . . . ? C15 Ti1 C16 C12 87.07(19) 3 . . . ? C15 Ti1 C16 C12 -115.1(2) . . . . ? C14 Ti1 C16 C12 32.4(3) 3 . . . ? C14 Ti1 C16 C12 -77.29(17) . . . . ? C16 Ti1 C16 C12 77.12(18) 3 . . . ? C13 Ti1 C16 C12 -36.21(15) . . . . ? C13 Ti1 C16 C12 18.38(18) 3 . . . ? C12 Ti1 C16 C12 44.25(15) 3 . . . ? C3 C1 B3 C2 -102.2(3) . . . . ? B3 C1 B3 C2 34.3(3) 3 . . . ? B4 C1 B3 C2 140.4(2) . . . . ? B4 C1 B3 C2 103.3(2) 3 . . . ? C3 C1 B3 B7 -140.2(2) . . . 3 ? C2 C1 B3 B7 -38.1(2) . . . 3 ? B3 C1 B3 B7 -3.8(3) 3 . . 3 ? B4 C1 B3 B7 102.4(2) . . . 3 ? B4 C1 B3 B7 65.2(3) 3 . . 3 ? C3 C1 B3 B5 157.1(2) . . . . ? C2 C1 B3 B5 -100.8(2) . . . . ? B3 C1 B3 B5 -66.5(3) 3 . . . ? B4 C1 B3 B5 39.64(19) . . . . ? B4 C1 B3 B5 2.5(3) 3 . . . ? C3 C1 B3 B4 117.4(3) . . . . ? C2 C1 B3 B4 -140.4(2) . . . . ? B3 C1 B3 B4 -106.1(3) 3 . . . ? B4 C1 B3 B4 -37.13(19) 3 . . . ? B7 C2 B3 C1 -136.3(2) 3 . . . ? B7 C2 B3 C1 -98.9(2) . . . . ? B3 C2 B3 C1 -32.8(3) 3 . . . ? Ti1 C2 B3 C1 97.9(2) . . . . ? C1 C2 B3 B7 136.3(2) . . . 3 ? B7 C2 B3 B7 37.38(19) . . . 3 ? B3 C2 B3 B7 103.5(3) 3 . . 3 ? Ti1 C2 B3 B7 -125.8(2) . . . 3 ? C1 C2 B3 B5 98.4(2) . . . . ? B7 C2 B3 B5 -37.93(19) 3 . . . ? B7 C2 B3 B5 -0.5(3) . . . . ? B3 C2 B3 B5 65.6(3) 3 . . . ? Ti1 C2 B3 B5 -163.73(17) . . . . ? C1 C2 B3 B4 35.0(2) . . . . ? B7 C2 B3 B4 -101.3(2) 3 . . . ? B7 C2 B3 B4 -63.9(3) . . . . ? B3 C2 B3 B4 2.2(3) 3 . . . ? Ti1 C2 B3 B4 132.92(18) . . . . ? C3 C1 B4 B6 154.3(2) . . . . ? C2 C1 B4 B6 -65.0(2) . . . . ? B3 C1 B4 B6 2.4(3) 3 . . . ? B3 C1 B4 B6 -102.2(2) . . . . ? B4 C1 B4 B6 39.5(2) 3 . . . ? C3 C1 B4 B3 -103.6(2) . . . . ? C2 C1 B4 B3 37.16(16) . . . . ? B3 C1 B4 B3 104.5(3) 3 . . . ? B4 C1 B4 B3 141.63(17) 3 . . . ? C3 C1 B4 B5 -142.9(2) . . . . ? C2 C1 B4 B5 -2.2(2) . . . . ? B3 C1 B4 B5 65.2(2) 3 . . . ? B3 C1 B4 B5 -39.34(18) . . . . ? B4 C1 B4 B5 102.29(17) 3 . . . ? C3 C1 B4 B4 114.8(3) . . . 3 ? C2 C1 B4 B4 -104.46(18) . . . 3 ? B3 C1 B4 B4 -37.11(14) 3 . . 3 ? B3 C1 B4 B4 -141.63(17) . . . 3 ? C2 B3 B4 C1 -35.1(2) . . . . ? B7 B3 B4 C1 -97.7(2) 3 . . . ? B5 B3 B4 C1 -134.9(2) . . . . ? C1 B3 B4 B6 96.6(2) . . . . ? C2 B3 B4 B6 61.5(2) . . . . ? B7 B3 B4 B6 -1.1(2) 3 . . . ? B5 B3 B4 B6 -38.31(17) . . . . ? C1 B3 B4 B5 134.9(2) . . . . ? C2 B3 B4 B5 99.8(2) . . . . ? B7 B3 B4 B5 37.18(18) 3 . . . ? C1 B3 B4 B4 33.73(15) . . . 3 ? C2 B3 B4 B4 -1.4(2) . . . 3 ? B7 B3 B4 B4 -63.98(17) 3 . . 3 ? B5 B3 B4 B4 -101.17(13) . . . 3 ? C1 B3 B5 B7 99.5(2) . . . 3 ? C2 B3 B5 B7 37.51(19) . . . 3 ? B4 B3 B5 B7 138.62(19) . . . 3 ? C1 B3 B5 B4 -39.15(19) . . . . ? C2 B3 B5 B4 -101.1(2) . . . . ? B7 B3 B5 B4 -138.62(19) 3 . . . ? C1 B3 B5 B8 62.0(3) . . . . ? C2 B3 B5 B8 0.1(3) . . . . ? B7 B3 B5 B8 -37.4(2) 3 . . . ? B4 B3 B5 B8 101.2(2) . . . . ? C1 B3 B5 B6 -1.6(3) . . . . ? C2 B3 B5 B6 -63.5(3) . . . . ? B7 B3 B5 B6 -101.0(2) 3 . . . ? B4 B3 B5 B6 37.6(2) . . . . ? C1 B4 B5 B3 38.57(17) . . . . ? B6 B4 B5 B3 137.3(2) . . . . ? B4 B4 B5 B3 99.91(13) 3 . . . ? C1 B4 B5 B7 1.6(2) . . . 3 ? B6 B4 B5 B7 100.3(2) . . . 3 ? B3 B4 B5 B7 -37.01(18) . . . 3 ? B4 B4 B5 B7 62.90(17) 3 . . 3 ? C1 B4 B5 B8 -61.6(2) . . . . ? B6 B4 B5 B8 37.2(2) . . . . ? B3 B4 B5 B8 -100.2(2) . . . . ? B4 B4 B5 B8 -0.2(2) 3 . . . ? C1 B4 B5 B6 -98.8(2) . . . . ? B3 B4 B5 B6 -137.3(2) . . . . ? B4 B4 B5 B6 -37.42(15) 3 . . . ? C1 B4 B6 B4 -39.0(2) . . . 3 ? B3 B4 B6 B4 -99.91(17) . . . 3 ? B5 B4 B6 B4 -137.94(17) . . . 3 ? C1 B4 B6 B5 -1.2(3) . . . 3 ? B3 B4 B6 B5 -62.1(3) . . . 3 ? B5 B4 B6 B5 -100.1(3) . . . 3 ? B4 B4 B6 B5 37.79(14) 3 . . 3 ? C1 B4 B6 B5 98.9(2) . . . . ? B3 B4 B6 B5 38.03(18) . . . . ? B4 B4 B6 B5 137.94(17) 3 . . . ? C1 B4 B6 B8 62.1(2) . . . . ? B3 B4 B6 B8 1.2(2) . . . . ? B5 B4 B6 B8 -36.87(16) . . . . ? B4 B4 B6 B8 101.07(17) 3 . . . ? B3 B5 B6 B4 -37.8(2) . . . . ? B7 B5 B6 B4 -101.0(2) 3 . . . ? B8 B5 B6 B4 -138.7(2) . . . . ? B3 B5 B6 B4 0.2(3) . . . 3 ? B7 B5 B6 B4 -62.9(3) 3 . . 3 ? B4 B5 B6 B4 38.07(19) . . . 3 ? B8 B5 B6 B4 -100.6(2) . . . 3 ? B3 B5 B6 B5 63.8(3) . . . 3 ? B7 B5 B6 B5 0.7(4) 3 . . 3 ? B4 B5 B6 B5 101.7(3) . . . 3 ? B8 B5 B6 B5 -37.0(3) . . . 3 ? B3 B5 B6 B8 100.8(2) . . . . ? B7 B5 B6 B8 37.7(2) 3 . . . ? B4 B5 B6 B8 138.7(2) . . . . ? C1 C2 B7 B7 -100.91(15) . . . 3 ? B3 C2 B7 B7 -37.59(14) . . . 3 ? B3 C2 B7 B7 -139.57(16) 3 . . 3 ? Ti1 C2 B7 B7 121.8(2) . . . 3 ? C1 C2 B7 B8 -62.5(2) . . . . ? B7 C2 B7 B8 38.4(2) 3 . . . ? B3 C2 B7 B8 0.8(3) . . . . ? B3 C2 B7 B8 -101.2(2) 3 . . . ? Ti1 C2 B7 B8 160.14(18) . . . . ? C1 C2 B7 B3 38.66(16) . . . 3 ? B7 C2 B7 B3 139.57(16) 3 . . 3 ? B3 C2 B7 B3 102.0(3) . . . 3 ? Ti1 C2 B7 B3 -98.7(2) . . . 3 ? C1 C2 B7 B5 0.9(2) . . . 3 ? B7 C2 B7 B5 101.76(17) 3 . . 3 ? B3 C2 B7 B5 64.2(2) . . . 3 ? B3 C2 B7 B5 -37.81(18) 3 . . 3 ? Ti1 C2 B7 B5 -136.5(2) . . . 3 ? C2 B7 B8 B7 -38.0(2) . . . 3 ? B3 B7 B8 B7 -100.46(17) 3 . . 3 ? B5 B7 B8 B7 -138.13(18) 3 . . 3 ? C2 B7 B8 B5 -0.7(3) . . . . ? B7 B7 B8 B5 37.33(14) 3 . . . ? B3 B7 B8 B5 -63.1(3) 3 . . . ? B5 B7 B8 B5 -100.8(3) 3 . . . ? C2 B7 B8 B5 100.1(2) . . . 3 ? B7 B7 B8 B5 138.13(18) 3 . . 3 ? B3 B7 B8 B5 37.67(19) 3 . . 3 ? C2 B7 B8 B6 62.4(2) . . . . ? B7 B7 B8 B6 100.40(17) 3 . . . ? B3 B7 B8 B6 -0.1(2) 3 . . . ? B5 B7 B8 B6 -37.73(17) 3 . . . ? B3 B5 B8 B7 0.4(3) . . . . ? B7 B5 B8 B7 -37.1(2) 3 . . . ? B4 B5 B8 B7 63.7(3) . . . . ? B6 B5 B8 B7 100.4(3) . . . . ? B3 B5 B8 B7 37.53(19) . . . 3 ? B4 B5 B8 B7 100.8(2) . . . 3 ? B6 B5 B8 B7 137.5(2) . . . 3 ? B3 B5 B8 B5 -62.9(3) . . . 3 ? B7 B5 B8 B5 -100.5(3) 3 . . 3 ? B4 B5 B8 B5 0.4(3) . . . 3 ? B6 B5 B8 B5 37.1(3) . . . 3 ? B3 B5 B8 B6 -100.0(2) . . . . ? B7 B5 B8 B6 -137.5(2) 3 . . . ? B4 B5 B8 B6 -36.7(2) . . . . ? B4 B6 B8 B7 -63.54(17) . . . . ? B4 B6 B8 B7 0.8(2) 3 . . . ? B5 B6 B8 B7 37.80(17) 3 . . . ? B5 B6 B8 B7 -100.6(2) . . . . ? B4 B6 B8 B7 -0.8(2) . . . 3 ? B4 B6 B8 B7 63.54(17) 3 . . 3 ? B5 B6 B8 B7 100.6(2) 3 . . 3 ? B5 B6 B8 B7 -37.80(17) . . . 3 ? B4 B6 B8 B5 37.05(17) . . . . ? B4 B6 B8 B5 101.3(2) 3 . . . ? B5 B6 B8 B5 138.4(3) 3 . . . ? B4 B6 B8 B5 -101.3(2) . . . 3 ? B4 B6 B8 B5 -37.05(17) 3 . . 3 ? B5 B6 B8 B5 -138.4(3) . . . 3 ? C22 Ti2 N3 C23 0.0 . . . . ? C36 Ti2 N3 C23 95.47(6) . . . . ? C36 Ti2 N3 C23 -95.47(6) 3_655 . . . ? C35 Ti2 N3 C23 -72.41(7) 3_655 . . . ? C35 Ti2 N3 C23 72.41(7) . . . . ? C32 Ti2 N3 C23 -128.06(6) 3_655 . . . ? C32 Ti2 N3 C23 128.06(6) . . . . ? C34 Ti2 N3 C23 89.73(15) . . . . ? C34 Ti2 N3 C23 -89.73(15) 3_655 . . . ? C33 Ti2 N3 C23 -133.24(9) 3_655 . . . ? C33 Ti2 N3 C23 133.24(9) . . . . ? C22 Ti2 N3 C24 180.0 . . . . ? C36 Ti2 N3 C24 -84.53(6) . . . . ? C36 Ti2 N3 C24 84.53(6) 3_655 . . . ? C35 Ti2 N3 C24 107.59(7) 3_655 . . . ? C35 Ti2 N3 C24 -107.59(7) . . . . ? C32 Ti2 N3 C24 51.94(6) 3_655 . . . ? C32 Ti2 N3 C24 -51.94(6) . . . . ? C34 Ti2 N3 C24 -90.27(15) . . . . ? C34 Ti2 N3 C24 90.27(15) 3_655 . . . ? C33 Ti2 N3 C24 46.76(9) 3_655 . . . ? C33 Ti2 N3 C24 -46.76(9) . . . . ? C23 C21 C22 B23 -108.12(14) . . . 3_655 ? B23 C21 C22 B23 143.8(3) . . . 3_655 ? B24 C21 C22 B23 37.38(18) 3_655 . . 3_655 ? B24 C21 C22 B23 106.4(2) . . . 3_655 ? C23 C21 C22 B23 108.12(14) . . . . ? B23 C21 C22 B23 -143.8(3) 3_655 . . . ? B24 C21 C22 B23 -106.4(2) 3_655 . . . ? B24 C21 C22 B23 -37.38(18) . . . . ? C23 C21 C22 B25 -147.99(13) . . . 3_655 ? B23 C21 C22 B25 103.9(2) . . . 3_655 ? B23 C21 C22 B25 -39.87(17) 3_655 . . 3_655 ? B24 C21 C22 B25 -2.5(2) 3_655 . . 3_655 ? B24 C21 C22 B25 66.50(17) . . . 3_655 ? C23 C21 C22 B25 147.99(13) . . . . ? B23 C21 C22 B25 39.87(17) . . . . ? B23 C21 C22 B25 -103.9(2) 3_655 . . . ? B24 C21 C22 B25 -66.50(17) 3_655 . . . ? B24 C21 C22 B25 2.5(2) . . . . ? C23 C21 C22 Ti2 0.0 . . . . ? B23 C21 C22 Ti2 -108.12(14) . . . . ? B23 C21 C22 Ti2 108.12(14) 3_655 . . . ? B24 C21 C22 Ti2 145.50(15) 3_655 . . . ? B24 C21 C22 Ti2 -145.50(15) . . . . ? N3 Ti2 C22 C21 0.0 . . . . ? C36 Ti2 C22 C21 -82.40(7) . . . . ? C36 Ti2 C22 C21 82.40(7) 3_655 . . . ? C35 Ti2 C22 C21 113.03(7) 3_655 . . . ? C35 Ti2 C22 C21 -113.03(7) . . . . ? C32 Ti2 C22 C21 83.54(11) 3_655 . . . ? C32 Ti2 C22 C21 -83.54(11) . . . . ? C34 Ti2 C22 C21 -138.98(7) . . . . ? C34 Ti2 C22 C21 138.98(7) 3_655 . . . ? C33 Ti2 C22 C21 127.77(11) 3_655 . . . ? C33 Ti2 C22 C21 -127.77(11) . . . . ? N3 Ti2 C22 B23 64.50(19) . . . 3_655 ? C36 Ti2 C22 B23 -17.9(2) . . . 3_655 ? C36 Ti2 C22 B23 146.9(2) 3_655 . . 3_655 ? C35 Ti2 C22 B23 177.5(2) 3_655 . . 3_655 ? C35 Ti2 C22 B23 -48.53(19) . . . 3_655 ? C32 Ti2 C22 B23 148.04(16) 3_655 . . 3_655 ? C32 Ti2 C22 B23 -19.0(3) . . . 3_655 ? C34 Ti2 C22 B23 -74.5(2) . . . 3_655 ? C34 Ti2 C22 B23 -156.52(19) 3_655 . . 3_655 ? C33 Ti2 C22 B23 -167.74(17) 3_655 . . 3_655 ? C33 Ti2 C22 B23 -63.3(3) . . . 3_655 ? N3 Ti2 C22 B23 -64.50(19) . . . . ? C36 Ti2 C22 B23 -146.9(2) . . . . ? C36 Ti2 C22 B23 17.9(2) 3_655 . . . ? C35 Ti2 C22 B23 48.53(19) 3_655 . . . ? C35 Ti2 C22 B23 -177.5(2) . . . . ? C32 Ti2 C22 B23 19.0(3) 3_655 . . . ? C32 Ti2 C22 B23 -148.04(16) . . . . ? C34 Ti2 C22 B23 156.52(19) . . . . ? C34 Ti2 C22 B23 74.5(2) 3_655 . . . ? C33 Ti2 C22 B23 63.3(3) 3_655 . . . ? C33 Ti2 C22 B23 167.74(17) . . . . ? N3 Ti2 C22 B25 137.4(2) . . . 3_655 ? C36 Ti2 C22 B25 55.0(2) . . . 3_655 ? C36 Ti2 C22 B25 -140.2(2) 3_655 . . 3_655 ? C35 Ti2 C22 B25 -109.6(2) 3_655 . . 3_655 ? C35 Ti2 C22 B25 24.4(2) . . . 3_655 ? C32 Ti2 C22 B25 -139.04(18) 3_655 . . 3_655 ? C32 Ti2 C22 B25 53.9(3) . . . 3_655 ? C34 Ti2 C22 B25 -1.6(2) . . . 3_655 ? C34 Ti2 C22 B25 -83.6(2) 3_655 . . 3_655 ? C33 Ti2 C22 B25 -94.81(19) 3_655 . . 3_655 ? C33 Ti2 C22 B25 9.7(3) . . . 3_655 ? N3 Ti2 C22 B25 -137.4(2) . . . . ? C36 Ti2 C22 B25 140.2(2) . . . . ? C36 Ti2 C22 B25 -55.0(2) 3_655 . . . ? C35 Ti2 C22 B25 -24.4(2) 3_655 . . . ? C35 Ti2 C22 B25 109.6(2) . . . . ? C32 Ti2 C22 B25 -53.9(3) 3_655 . . . ? C32 Ti2 C22 B25 139.04(18) . . . . ? C34 Ti2 C22 B25 83.6(2) . . . . ? C34 Ti2 C22 B25 1.6(2) 3_655 . . . ? C33 Ti2 C22 B25 -9.7(3) 3_655 . . . ? C33 Ti2 C22 B25 94.81(19) . . . . ? C28 N4 C23 N3 180.0 . . . . ? C28 N4 C23 C21 0.000(1) . . . . ? C24 N3 C23 N4 0.0 . . . . ? Ti2 N3 C23 N4 180.0 . . . . ? C24 N3 C23 C21 180.0 . . . . ? Ti2 N3 C23 C21 0.0 . . . . ? C22 C21 C23 N4 180.0 . . . . ? B23 C21 C23 N4 -112.5(2) . . . . ? B23 C21 C23 N4 112.5(2) 3_655 . . . ? B24 C21 C23 N4 39.1(2) 3_655 . . . ? B24 C21 C23 N4 -39.1(2) . . . . ? C22 C21 C23 N3 0.0 . . . . ? B23 C21 C23 N3 67.5(2) . . . . ? B23 C21 C23 N3 -67.5(2) 3_655 . . . ? B24 C21 C23 N3 -140.9(2) 3_655 . . . ? B24 C21 C23 N3 140.9(2) . . . . ? C23 N3 C24 C25 -64.7(2) . . . 3_655 ? Ti2 N3 C24 C25 115.3(2) . . . 3_655 ? C23 N3 C24 C25 64.7(2) . . . . ? Ti2 N3 C24 C25 -115.3(2) . . . . ? N3 C24 C25 C26 174.3(2) . . . . ? C25 C24 C25 C26 -54.8(4) 3_655 . . . ? C24 C25 C26 C27 56.4(3) . . . . ? C25 C26 C27 C26 -57.6(4) . . . 3_655 ? C23 N4 C28 C29 -119.4(2) . . . 3_655 ? C23 N4 C28 C29 119.4(2) . . . . ? N4 C28 C29 C30 177.7(3) . . . . ? C29 C28 C29 C30 57.9(4) 3_655 . . . ? C28 C29 C30 C31 -55.6(4) . . . . ? C29 C30 C31 C30 53.6(5) . . . 3_655 ? N3 Ti2 C32 C33 172.57(16) . . . . ? C22 Ti2 C32 C33 -112.90(18) . . . . ? C36 Ti2 C32 C33 -114.9(2) . . . . ? C36 Ti2 C32 C33 87.76(19) 3_655 . . . ? C35 Ti2 C32 C33 33.5(3) 3_655 . . . ? C35 Ti2 C32 C33 -77.43(16) . . . . ? C32 Ti2 C32 C33 77.58(17) 3_655 . . . ? C34 Ti2 C32 C33 -36.18(15) . . . . ? C34 Ti2 C32 C33 18.90(18) 3_655 . . . ? C33 Ti2 C32 C33 44.64(14) 3_655 . . . ? N3 Ti2 C32 C36 -72.51(16) . . . . ? C22 Ti2 C32 C36 2.0(2) . . . . ? C36 Ti2 C32 C36 -157.3(2) 3_655 . . . ? C35 Ti2 C32 C36 148.43(18) 3_655 . . . ? C35 Ti2 C32 C36 37.49(15) . . . . ? C32 Ti2 C32 C36 -167.50(12) 3_655 . . . ? C34 Ti2 C32 C36 78.74(16) . . . . ? C34 Ti2 C32 C36 133.83(15) 3_655 . . . ? C33 Ti2 C32 C36 159.56(16) 3_655 . . . ? C33 Ti2 C32 C36 114.9(2) . . . . ? C36 C32 C33 C34 -1.7(3) . . . . ? Ti2 C32 C33 C34 63.75(18) . . . . ? C36 C32 C33 Ti2 -65.47(18) . . . . ? N3 Ti2 C33 C34 -126.23(17) . . . . ? C22 Ti2 C33 C34 -20.3(2) . . . . ? C36 Ti2 C33 C34 -79.10(17) . . . . ? C36 Ti2 C33 C34 121.31(17) 3_655 . . . ? C35 Ti2 C33 C34 81.69(18) 3_655 . . . ? C35 Ti2 C33 C34 -37.87(16) . . . . ? C32 Ti2 C33 C34 135.35(17) 3_655 . . . ? C32 Ti2 C33 C34 -116.9(2) . . . . ? C34 Ti2 C33 C34 79.93(19) 3_655 . . . ? C33 Ti2 C33 C34 110.97(15) 3_655 . . . ? N3 Ti2 C33 C32 -9.33(19) . . . . ? C22 Ti2 C33 C32 96.58(18) . . . . ? C36 Ti2 C33 C32 37.80(14) . . . . ? C36 Ti2 C33 C32 -121.79(16) 3_655 . . . ? C35 Ti2 C33 C32 -161.41(14) 3_655 . . . ? C35 Ti2 C33 C32 79.03(16) . . . . ? C32 Ti2 C33 C32 -107.75(18) 3_655 . . . ? C34 Ti2 C33 C32 116.9(2) . . . . ? C34 Ti2 C33 C32 -163.17(16) 3_655 . . . ? C33 Ti2 C33 C32 -132.14(13) 3_655 . . . ? C32 C33 C34 C35 1.5(3) . . . . ? Ti2 C33 C34 C35 64.70(18) . . . . ? C32 C33 C34 Ti2 -63.16(18) . . . . ? N3 Ti2 C34 C33 84.7(2) . . . . ? C22 Ti2 C34 C33 164.98(16) . . . . ? C36 Ti2 C34 C33 77.87(17) . . . . ? C36 Ti2 C34 C33 -87.79(19) 3_655 . . . ? C35 Ti2 C34 C33 -113.24(16) 3_655 . . . ? C35 Ti2 C34 C33 114.9(2) . . . . ? C32 Ti2 C34 C33 -51.91(19) 3_655 . . . ? C32 Ti2 C34 C33 36.57(15) . . . . ? C34 Ti2 C34 C33 -95.64(16) 3_655 . . . ? C33 Ti2 C34 C33 -62.31(17) 3_655 . . . ? N3 Ti2 C34 C35 -30.2(2) . . . . ? C22 Ti2 C34 C35 50.03(16) . . . . ? C36 Ti2 C34 C35 -37.08(14) . . . . ? C36 Ti2 C34 C35 157.26(15) 3_655 . . . ? C35 Ti2 C34 C35 131.82(18) 3_655 . . . ? C32 Ti2 C34 C35 -166.85(14) 3_655 . . . ? C32 Ti2 C34 C35 -78.37(16) . . . . ? C34 Ti2 C34 C35 149.42(12) 3_655 . . . ? C33 Ti2 C34 C35 -177.26(16) 3_655 . . . ? C33 Ti2 C34 C35 -114.9(2) . . . . ? C33 C34 C35 C36 -0.8(3) . . . . ? Ti2 C34 C35 C36 65.29(18) . . . . ? C33 C34 C35 Ti2 -66.07(19) . . . . ? N3 Ti2 C35 C36 44.23(17) . . . . ? C22 Ti2 C35 C36 114.38(16) . . . . ? C36 Ti2 C35 C36 179.0(3) 3_655 . . . ? C35 Ti2 C35 C36 179.65(12) 3_655 . . . ? C32 Ti2 C35 C36 -92.1(2) 3_655 . . . ? C32 Ti2 C35 C36 -37.73(14) . . . . ? C34 Ti2 C35 C36 -115.7(2) . . . . ? C34 Ti2 C35 C36 -147.88(15) 3_655 . . . ? C33 Ti2 C35 C36 -112.61(16) 3_655 . . . ? C33 Ti2 C35 C36 -78.65(16) . . . . ? N3 Ti2 C35 C34 159.96(16) . . . . ? C22 Ti2 C35 C34 -129.89(18) . . . . ? C36 Ti2 C35 C34 115.7(2) . . . . ? C36 Ti2 C35 C34 -65.3(4) 3_655 . . . ? C35 Ti2 C35 C34 -64.6(2) 3_655 . . . ? C32 Ti2 C35 C34 23.6(3) 3_655 . . . ? C32 Ti2 C35 C34 78.00(16) . . . . ? C34 Ti2 C35 C34 -32.15(14) 3_655 . . . ? C33 Ti2 C35 C34 3.12(18) 3_655 . . . ? C33 Ti2 C35 C34 37.08(15) . . . . ? C34 C35 C36 C32 -0.3(3) . . . . ? Ti2 C35 C36 C32 65.67(18) . . . . ? C34 C35 C36 Ti2 -65.95(18) . . . . ? C33 C32 C36 C35 1.2(3) . . . . ? Ti2 C32 C36 C35 -65.57(18) . . . . ? C33 C32 C36 Ti2 66.80(18) . . . . ? N3 Ti2 C36 C35 -138.35(17) . . . . ? C22 Ti2 C36 C35 -63.51(16) . . . . ? C36 Ti2 C36 C35 -179.0(4) 3_655 . . . ? C35 Ti2 C36 C35 -0.9(3) 3_655 . . . ? C32 Ti2 C36 C35 132.72(15) 3_655 . . . ? C32 Ti2 C36 C35 114.9(2) . . . . ? C34 Ti2 C36 C35 37.22(14) . . . . ? C34 Ti2 C36 C35 46.5(2) 3_655 . . . ? C33 Ti2 C36 C35 89.36(17) 3_655 . . . ? C33 Ti2 C36 C35 77.57(16) . . . . ? N3 Ti2 C36 C32 106.76(17) . . . . ? C22 Ti2 C36 C32 -178.40(17) . . . . ? C36 Ti2 C36 C32 66.1(5) 3_655 . . . ? C35 Ti2 C36 C32 -115.8(3) 3_655 . . . ? C35 Ti2 C36 C32 -114.9(2) . . . . ? C32 Ti2 C36 C32 17.83(17) 3_655 . . . ? C34 Ti2 C36 C32 -77.67(16) . . . . ? C34 Ti2 C36 C32 -68.39(19) 3_655 . . . ? C33 Ti2 C36 C32 -25.53(19) 3_655 . . . ? C33 Ti2 C36 C32 -37.32(15) . . . . ? C23 C21 B23 C22 -101.9(3) . . . . ? B23 C21 B23 C22 34.3(3) 3_655 . . . ? B24 C21 B23 C22 103.7(3) 3_655 . . . ? B24 C21 B23 C22 141.1(2) . . . . ? C23 C21 B23 B26 156.7(3) . . . . ? C22 C21 B23 B26 -101.3(2) . . . . ? B23 C21 B23 B26 -67.0(3) 3_655 . . . ? B24 C21 B23 B26 2.4(3) 3_655 . . . ? B24 C21 B23 B26 39.7(2) . . . . ? C23 C21 B23 B25 -140.3(2) . . . . ? C22 C21 B23 B25 -38.3(2) . . . . ? B23 C21 B23 B25 -4.1(3) 3_655 . . . ? B24 C21 B23 B25 65.4(3) 3_655 . . . ? B24 C21 B23 B25 102.7(2) . . . . ? C23 C21 B23 B24 117.0(3) . . . . ? C22 C21 B23 B24 -141.1(2) . . . . ? B23 C21 B23 B24 -106.8(3) 3_655 . . . ? B24 C21 B23 B24 -37.3(2) 3_655 . . . ? B23 C22 B23 C21 -33.0(3) 3_655 . . . ? B25 C22 B23 C21 -99.1(2) 3_655 . . . ? B25 C22 B23 C21 -136.0(2) . . . . ? Ti2 C22 B23 C21 98.2(2) . . . . ? C21 C22 B23 B26 97.8(2) . . . . ? B23 C22 B23 B26 64.8(3) 3_655 . . . ? B25 C22 B23 B26 -1.3(3) 3_655 . . . ? B25 C22 B23 B26 -38.2(2) . . . . ? Ti2 C22 B23 B26 -164.02(18) . . . . ? C21 C22 B23 B25 136.0(2) . . . . ? B23 C22 B23 B25 103.1(3) 3_655 . . . ? B25 C22 B23 B25 36.91(19) 3_655 . . . ? Ti2 C22 B23 B25 -125.8(2) . . . . ? C21 C22 B23 B24 34.3(2) . . . . ? B23 C22 B23 B24 1.3(4) 3_655 . . . ? B25 C22 B23 B24 -64.8(3) 3_655 . . . ? B25 C22 B23 B24 -101.7(2) . . . . ? Ti2 C22 B23 B24 132.49(18) . . . . ? C23 C21 B24 B23 -103.8(2) . . . . ? C22 C21 B24 B23 36.75(17) . . . . ? B23 C21 B24 B23 104.4(3) 3_655 . . . ? B24 C21 B24 B23 141.68(18) 3_655 . . . ? C23 C21 B24 B26 -143.1(2) . . . . ? C22 C21 B24 B26 -2.5(2) . . . . ? B23 C21 B24 B26 -39.25(19) . . . . ? B23 C21 B24 B26 65.1(3) 3_655 . . . ? B24 C21 B24 B26 102.43(17) 3_655 . . . ? C23 C21 B24 B27 154.6(2) . . . . ? C22 C21 B24 B27 -64.9(2) . . . . ? B23 C21 B24 B27 -101.6(2) . . . . ? B23 C21 B24 B27 2.8(3) 3_655 . . . ? B24 C21 B24 B27 40.1(2) 3_655 . . . ? C23 C21 B24 B24 114.5(3) . . . 3_655 ? C22 C21 B24 B24 -104.94(19) . . . 3_655 ? B23 C21 B24 B24 -141.68(18) . . . 3_655 ? B23 C21 B24 B24 -37.33(15) 3_655 . . 3_655 ? C22 B23 B24 C21 -34.4(2) . . . . ? B26 B23 B24 C21 -134.7(2) . . . . ? B25 B23 B24 C21 -97.2(2) . . . . ? C21 B23 B24 B26 134.7(2) . . . . ? C22 B23 B24 B26 100.3(2) . . . . ? B25 B23 B24 B26 37.53(19) . . . . ? C21 B23 B24 B27 96.8(2) . . . . ? C22 B23 B24 B27 62.3(2) . . . . ? B26 B23 B24 B27 -37.97(18) . . . . ? B25 B23 B24 B27 -0.4(2) . . . . ? C21 B23 B24 B24 33.63(15) . . . 3_655 ? C22 B23 B24 B24 -0.8(2) . . . 3_655 ? B26 B23 B24 B24 -101.11(15) . . . 3_655 ? B25 B23 B24 B24 -63.58(18) . . . 3_655 ? C21 C22 B25 B25 100.80(16) . . . 3_655 ? B23 C22 B25 B25 37.28(14) 3_655 . . 3_655 ? B23 C22 B25 B25 139.82(17) . . . 3_655 ? Ti2 C22 B25 B25 -121.5(2) . . . 3_655 ? C21 C22 B25 B23 -39.02(16) . . . . ? B23 C22 B25 B23 -102.5(3) 3_655 . . . ? B25 C22 B25 B23 -139.82(17) 3_655 . . . ? Ti2 C22 B25 B23 98.7(2) . . . . ? C21 C22 B25 B28 61.9(2) . . . . ? B23 C22 B25 B28 -1.6(3) 3_655 . . . ? B23 C22 B25 B28 100.9(2) . . . . ? B25 C22 B25 B28 -38.9(2) 3_655 . . . ? Ti2 C22 B25 B28 -160.37(19) . . . . ? C21 C22 B25 B26 -1.3(2) . . . . ? B23 C22 B25 B26 -64.9(2) 3_655 . . . ? B23 C22 B25 B26 37.67(19) . . . . ? B25 C22 B25 B26 -102.15(17) 3_655 . . . ? Ti2 C22 B25 B26 136.4(2) . . . . ? C21 B23 B25 C22 38.2(2) . . . . ? B26 B23 B25 C22 137.2(2) . . . . ? B24 B23 B25 C22 99.8(2) . . . . ? C21 B23 B25 B25 2.4(2) . . . 3_655 ? C22 B23 B25 B25 -35.82(14) . . . 3_655 ? B26 B23 B25 B25 101.41(14) . . . 3_655 ? B24 B23 B25 B25 63.98(17) . . . 3_655 ? C21 B23 B25 B28 -61.6(2) . . . . ? C22 B23 B25 B28 -99.8(2) . . . . ? B26 B23 B25 B28 37.43(18) . . . . ? B24 B23 B25 B28 0.0(2) . . . . ? C21 B23 B25 B26 -99.1(2) . . . . ? C22 B23 B25 B26 -137.2(2) . . . . ? B24 B23 B25 B26 -37.43(18) . . . . ? C21 B23 B26 B24 -39.0(2) . . . . ? C22 B23 B26 B24 -100.7(2) . . . . ? B25 B23 B26 B24 -138.5(2) . . . . ? C21 B23 B26 B25 99.5(2) . . . . ? C22 B23 B26 B25 37.7(2) . . . . ? B24 B23 B26 B25 138.5(2) . . . . ? C21 B23 B26 B27 -1.0(3) . . . . ? C22 B23 B26 B27 -62.7(3) . . . . ? B25 B23 B26 B27 -100.5(2) . . . . ? B24 B23 B26 B27 38.0(2) . . . . ? C21 B23 B26 B28 62.2(3) . . . . ? C22 B23 B26 B28 0.5(3) . . . . ? B25 B23 B26 B28 -37.2(2) . . . . ? B24 B23 B26 B28 101.2(2) . . . . ? C21 B24 B26 B23 38.70(18) . . . . ? B27 B24 B26 B23 137.4(2) . . . . ? B24 B24 B26 B23 99.85(14) 3_655 . . . ? C21 B24 B26 B25 1.5(2) . . . . ? B23 B24 B26 B25 -37.15(18) . . . . ? B27 B24 B26 B25 100.2(2) . . . . ? B24 B24 B26 B25 62.70(18) 3_655 . . . ? C21 B24 B26 B27 -98.7(2) . . . . ? B23 B24 B26 B27 -137.4(2) . . . . ? B24 B24 B26 B27 -37.52(16) 3_655 . . . ? C21 B24 B26 B28 -61.8(3) . . . . ? B23 B24 B26 B28 -100.5(2) . . . . ? B27 B24 B26 B28 36.9(2) . . . . ? B24 B24 B26 B28 -0.7(2) 3_655 . . . ? C22 B25 B26 B23 -37.44(18) . . . . ? B25 B25 B26 B23 -100.32(14) 3_655 . . . ? B28 B25 B26 B23 -138.2(2) . . . . ? C22 B25 B26 B24 -0.2(2) . . . . ? B25 B25 B26 B24 -63.03(19) 3_655 . . . ? B23 B25 B26 B24 37.29(19) . . . . ? B28 B25 B26 B24 -100.9(2) . . . . ? C22 B25 B26 B27 63.2(3) . . . . ? B25 B25 B26 B27 0.4(2) 3_655 . . . ? B23 B25 B26 B27 100.7(2) . . . . ? B28 B25 B26 B27 -37.5(2) . . . . ? C22 B25 B26 B28 100.8(2) . . . . ? B25 B25 B26 B28 37.90(17) 3_655 . . . ? B23 B25 B26 B28 138.2(2) . . . . ? C21 B24 B27 B24 -39.4(2) . . . 3_655 ? B23 B24 B27 B24 -100.32(18) . . . 3_655 ? B26 B24 B27 B24 -138.02(19) . . . 3_655 ? C21 B24 B27 B28 61.7(2) . . . . ? B23 B24 B27 B28 0.7(2) . . . . ? B26 B24 B27 B28 -36.99(17) . . . . ? B24 B24 B27 B28 101.03(17) 3_655 . . . ? C21 B24 B27 B26 98.7(2) . . . . ? B23 B24 B27 B26 37.71(19) . . . . ? B24 B24 B27 B26 138.02(19) 3_655 . . . ? C21 B24 B27 B26 -1.9(3) . . . 3_655 ? B23 B24 B27 B26 -62.9(3) . . . 3_655 ? B26 B24 B27 B26 -100.6(3) . . . 3_655 ? B24 B24 B27 B26 37.42(15) 3_655 . . 3_655 ? B23 B26 B27 B24 -0.6(3) . . . 3_655 ? B24 B26 B27 B24 37.5(2) . . . 3_655 ? B25 B26 B27 B24 -63.8(3) . . . 3_655 ? B28 B26 B27 B24 -101.3(3) . . . 3_655 ? B23 B26 B27 B24 -38.1(2) . . . . ? B25 B26 B27 B24 -101.3(2) . . . . ? B28 B26 B27 B24 -138.8(2) . . . . ? B23 B26 B27 B28 100.7(2) . . . . ? B24 B26 B27 B28 138.8(2) . . . . ? B25 B26 B27 B28 37.5(2) . . . . ? B23 B26 B27 B26 62.6(3) . . . 3_655 ? B24 B26 B27 B26 100.7(3) . . . 3_655 ? B25 B26 B27 B26 -0.6(4) . . . 3_655 ? B28 B26 B27 B26 -38.1(3) . . . 3_655 ? C22 B25 B28 B25 38.5(2) . . . 3_655 ? B23 B25 B28 B25 100.85(18) . . . 3_655 ? B26 B25 B28 B25 138.02(19) . . . 3_655 ? C22 B25 B28 B27 -61.9(2) . . . . ? B25 B25 B28 B27 -100.40(18) 3_655 . . . ? B23 B25 B28 B27 0.4(2) . . . . ? B26 B25 B28 B27 37.62(17) . . . . ? C22 B25 B28 B26 1.3(3) . . . 3_655 ? B25 B25 B28 B26 -37.25(14) 3_655 . . 3_655 ? B23 B25 B28 B26 63.6(3) . . . 3_655 ? B26 B25 B28 B26 100.8(3) . . . 3_655 ? C22 B25 B28 B26 -99.5(2) . . . . ? B25 B25 B28 B26 -138.02(19) 3_655 . . . ? B23 B25 B28 B26 -37.2(2) . . . . ? B24 B27 B28 B25 62.87(17) 3_655 . . . ? B24 B27 B28 B25 -0.7(2) . . . . ? B26 B27 B28 B25 -37.60(17) . . . . ? B26 B27 B28 B25 99.8(2) 3_655 . . . ? B24 B27 B28 B25 0.7(2) 3_655 . . 3_655 ? B24 B27 B28 B25 -62.87(17) . . . 3_655 ? B26 B27 B28 B25 -99.8(2) . . . 3_655 ? B26 B27 B28 B25 37.60(17) 3_655 . . 3_655 ? B24 B27 B28 B26 -36.88(18) 3_655 . . 3_655 ? B24 B27 B28 B26 -100.5(2) . . . 3_655 ? B26 B27 B28 B26 -137.4(3) . . . 3_655 ? B24 B27 B28 B26 100.5(2) 3_655 . . . ? B24 B27 B28 B26 36.88(18) . . . . ? B26 B27 B28 B26 137.4(3) 3_655 . . . ? B23 B26 B28 B25 37.3(2) . . . . ? B24 B26 B28 B25 100.9(2) . . . . ? B27 B26 B28 B25 137.8(2) . . . . ? B23 B26 B28 B25 0.5(3) . . . 3_655 ? B24 B26 B28 B25 64.1(3) . . . 3_655 ? B25 B26 B28 B25 -36.8(2) . . . 3_655 ? B27 B26 B28 B25 101.0(3) . . . 3_655 ? B23 B26 B28 B27 -100.6(3) . . . . ? B24 B26 B28 B27 -36.9(2) . . . . ? B25 B26 B28 B27 -137.8(2) . . . . ? B23 B26 B28 B26 -62.6(3) . . . 3_655 ? B24 B26 B28 B26 1.0(4) . . . 3_655 ? B25 B26 B28 B26 -99.9(3) . . . 3_655 ? B27 B26 B28 B26 38.0(3) . . . 3_655 ? C44 O1 C41 C42 11.3(4) . . . . ? O1 C41 C42 C43 10.6(5) . . . . ? C41 C42 C43 C44 -30.6(5) . . . . ? C42 C43 C44 O1 39.2(4) . . . . ? C41 O1 C44 C43 -32.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 76.17 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.639 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.056 _database_code_depnum_ccdc_archive 'CCDC 963131' ####################################################################### # # 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_magd52 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H42 B10 N2 Zr' _chemical_formula_weight 569.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -0.1862 2.2449 '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 10.4438(4) _cell_length_b 10.7747(4) _cell_length_c 13.2968(6) _cell_angle_alpha 107.827(4) _cell_angle_beta 96.672(4) _cell_angle_gamma 93.456(3) _cell_volume 1407.49(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 21413 _cell_measurement_theta_min 3.5243 _cell_measurement_theta_max 75.9889 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.345 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 3.316 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7546 _exptl_absorpt_correction_T_max 0.9071 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Nova' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3543 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33562 _diffrn_reflns_av_R_equivalents 0.0896 _diffrn_reflns_av_sigmaI/netI 0.0447 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 76.18 _reflns_number_total 5822 _reflns_number_gt 5523 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XP' _computing_publication_material SHELXL-97 _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^)+(0.0622P)^2^+0.6735P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5822 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0967 _refine_ls_wR_factor_gt 0.0946 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr Zr 0.701413(15) 0.798212(15) 0.674323(12) 0.01524(8) Uani 1 1 d . . . N1 N 0.79248(17) 0.98689(17) 0.74650(14) 0.0164(3) Uani 1 1 d . . . N2 N 0.93908(18) 1.17217(18) 0.80734(14) 0.0187(4) Uani 1 1 d . . . C1 C 1.0106(2) 0.9469(2) 0.72626(16) 0.0161(4) Uani 1 1 d . . . C2 C 0.9329(2) 0.7918(2) 0.66797(17) 0.0173(4) Uani 1 1 d . . . C3 C 0.9162(2) 1.0487(2) 0.76513(16) 0.0169(4) Uani 1 1 d . . . C4 C 0.6822(2) 1.0599(2) 0.77695(16) 0.0173(4) Uani 1 1 d . . . H4A H 0.6054 0.9925 0.7530 0.021 Uiso 1 1 calc R . . C5 C 0.6513(2) 1.1607(2) 0.71945(17) 0.0196(4) Uani 1 1 d . . . H5A H 0.7220 1.2331 0.7419 0.023 Uiso 1 1 calc R . . H5B H 0.6458 1.1185 0.6414 0.023 Uiso 1 1 calc R . . C6 C 0.5230(2) 1.2160(2) 0.74511(18) 0.0226(5) Uani 1 1 d . . . H6A H 0.4511 1.1450 0.7167 0.027 Uiso 1 1 calc R . . H6B H 0.5070 1.2837 0.7101 0.027 Uiso 1 1 calc R . . C7 C 0.5265(2) 1.2763(3) 0.86589(19) 0.0263(5) Uani 1 1 d . . . H7A H 0.5934 1.3523 0.8931 0.032 Uiso 1 1 calc R . . H7B H 0.4416 1.3082 0.8810 0.032 Uiso 1 1 calc R . . C8 C 0.5566(2) 1.1769(2) 0.92367(18) 0.0240(5) Uani 1 1 d . . . H8A H 0.4852 1.1051 0.9018 0.029 Uiso 1 1 calc R . . H8B H 0.5624 1.2200 1.0016 0.029 Uiso 1 1 calc R . . C9 C 0.6844(2) 1.1196(2) 0.89841(17) 0.0198(4) Uani 1 1 d . . . H9A H 0.6983 1.0511 0.9329 0.024 Uiso 1 1 calc R . . H9B H 0.7571 1.1896 0.9278 0.024 Uiso 1 1 calc R . . C10 C 1.0642(2) 1.2489(2) 0.83076(17) 0.0176(4) Uani 1 1 d . . . H10 H 1.1351 1.1897 0.8224 0.021 Uiso 1 1 calc R . . C11 C 1.0778(2) 1.3402(2) 0.94646(17) 0.0199(4) Uani 1 1 d . . . H11A H 1.0029 1.3927 0.9552 0.024 Uiso 1 1 calc R . . H11B H 1.0768 1.2869 0.9952 0.024 Uiso 1 1 calc R . . C12 C 1.2033(2) 1.4325(2) 0.97707(17) 0.0218(4) Uani 1 1 d . . . H12A H 1.2784 1.3809 0.9782 0.026 Uiso 1 1 calc R . . H12B H 1.2049 1.4947 1.0497 0.026 Uiso 1 1 calc R . . C13 C 1.2149(2) 1.5093(2) 0.89819(18) 0.0227(5) Uani 1 1 d . . . H13A H 1.1485 1.5722 0.9062 0.027 Uiso 1 1 calc R . . H13B H 1.3011 1.5602 0.9154 0.027 Uiso 1 1 calc R . . C14 C 1.1973(2) 1.4194(2) 0.78246(18) 0.0202(4) Uani 1 1 d . . . H14A H 1.2704 1.3646 0.7716 0.024 Uiso 1 1 calc R . . H14B H 1.1981 1.4733 0.7341 0.024 Uiso 1 1 calc R . . C15 C 1.0696(2) 1.3309(2) 0.75500(17) 0.0199(4) Uani 1 1 d . . . H15A H 1.0616 1.2720 0.6805 0.024 Uiso 1 1 calc R . . H15B H 0.9961 1.3853 0.7607 0.024 Uiso 1 1 calc R . . C16 C 0.6655(2) 0.8616(2) 0.50513(17) 0.0198(4) Uani 1 1 d . . . H16 H 0.7122 0.9394 0.5038 0.024 Uiso 1 1 calc R . . C17 C 0.7068(2) 0.7352(2) 0.47459(16) 0.0200(4) Uani 1 1 d . . . H17 H 0.7862 0.7126 0.4491 0.024 Uiso 1 1 calc R . . C18 C 0.6084(2) 0.6471(2) 0.48863(17) 0.0200(4) Uani 1 1 d . . . H18 H 0.6109 0.5554 0.4747 0.024 Uiso 1 1 calc R . . C19 C 0.5065(2) 0.7201(2) 0.52703(17) 0.0201(4) Uani 1 1 d . . . H19 H 0.4278 0.6862 0.5426 0.024 Uiso 1 1 calc R . . C20 C 0.5425(2) 0.8526(2) 0.53808(16) 0.0189(4) Uani 1 1 d . . . H20 H 0.4924 0.9236 0.5634 0.023 Uiso 1 1 calc R . . C21 C 0.7554(2) 0.6585(2) 0.79336(18) 0.0220(5) Uani 1 1 d . . . H21 H 0.8403 0.6318 0.7977 0.026 Uiso 1 1 calc R . . C22 C 0.6467(2) 0.5878(2) 0.71994(19) 0.0237(5) Uani 1 1 d . . . H22 H 0.6458 0.5054 0.6666 0.028 Uiso 1 1 calc R . . C23 C 0.5401(2) 0.6617(2) 0.74035(19) 0.0251(5) Uani 1 1 d . . . H23 H 0.4543 0.6374 0.7034 0.030 Uiso 1 1 calc R . . C24 C 0.5832(2) 0.7783(2) 0.82551(18) 0.0235(5) Uani 1 1 d . . . H24 H 0.5318 0.8466 0.8550 0.028 Uiso 1 1 calc R . . C25 C 0.7161(2) 0.7751(2) 0.85883(18) 0.0212(4) Uani 1 1 d . . . H25 H 0.7696 0.8402 0.9155 0.025 Uiso 1 1 calc R . . B3 B 1.0268(2) 0.8339(2) 0.79284(19) 0.0176(4) Uani 1 1 d . . . H3 H 0.9836 0.8391 0.8671 0.021 Uiso 1 1 calc R . . B4 B 1.0375(2) 0.6833(2) 0.6930(2) 0.0192(5) Uani 1 1 d . . . H4 H 1.0028 0.5870 0.7014 0.023 Uiso 1 1 calc R . . B5 B 1.0185(2) 0.7100(2) 0.5683(2) 0.0193(5) Uani 1 1 d . . . H5 H 0.9713 0.6319 0.4940 0.023 Uiso 1 1 calc R . . B6 B 0.9968(2) 0.8776(2) 0.59057(19) 0.0173(4) Uani 1 1 d . . . H6 H 0.9337 0.9116 0.5322 0.021 Uiso 1 1 calc R . . B7 B 1.1605(2) 0.9457(2) 0.79308(19) 0.0184(5) Uani 1 1 d . . . H7 H 1.2063 1.0240 0.8678 0.022 Uiso 1 1 calc R . . B8 B 1.1812(2) 0.7776(2) 0.7713(2) 0.0191(5) Uani 1 1 d . . . H8 H 1.2414 0.7443 0.8317 0.023 Uiso 1 1 calc R . . B9 B 1.1766(2) 0.7012(3) 0.6314(2) 0.0206(5) Uani 1 1 d . . . H9 H 1.2346 0.6175 0.5992 0.025 Uiso 1 1 calc R . . B10 B 1.1507(2) 0.8221(2) 0.5662(2) 0.0197(5) Uani 1 1 d . . . H10A H 1.1906 0.8184 0.4908 0.024 Uiso 1 1 calc R . . B11 B 1.1421(2) 0.9732(2) 0.66680(19) 0.0178(5) Uani 1 1 d . . . H11 H 1.1758 1.0695 0.6581 0.021 Uiso 1 1 calc R . . B12 B 1.2519(2) 0.8634(2) 0.6924(2) 0.0189(5) Uani 1 1 d . . . H12 H 1.3593 0.8866 0.7003 0.023 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 Zr 0.01397(11) 0.01931(12) 0.01136(12) 0.00551(8) -0.00327(7) -0.00056(7) N1 0.0144(8) 0.0189(8) 0.0138(8) 0.0044(7) -0.0027(6) 0.0003(7) N2 0.0173(9) 0.0211(9) 0.0165(9) 0.0061(7) -0.0032(7) 0.0009(7) C1 0.0160(10) 0.0175(9) 0.0136(9) 0.0051(8) -0.0022(8) -0.0002(8) C2 0.0180(10) 0.0182(9) 0.0143(9) 0.0054(8) -0.0037(8) -0.0004(8) C3 0.0162(10) 0.0217(10) 0.0130(9) 0.0070(8) -0.0016(8) 0.0023(8) C4 0.0158(10) 0.0210(10) 0.0132(10) 0.0043(8) -0.0027(8) 0.0010(8) C5 0.0176(10) 0.0230(10) 0.0161(10) 0.0051(8) -0.0025(8) 0.0017(8) C6 0.0192(11) 0.0277(11) 0.0177(11) 0.0047(9) -0.0050(8) 0.0051(9) C7 0.0214(11) 0.0349(12) 0.0190(11) 0.0035(9) -0.0011(9) 0.0092(10) C8 0.0188(11) 0.0336(12) 0.0156(10) 0.0035(9) -0.0006(8) 0.0008(9) C9 0.0196(10) 0.0244(10) 0.0133(10) 0.0048(8) -0.0027(8) 0.0012(8) C10 0.0159(10) 0.0184(10) 0.0154(10) 0.0034(8) -0.0029(8) -0.0006(8) C11 0.0205(11) 0.0216(10) 0.0151(10) 0.0044(8) -0.0020(8) -0.0003(8) C12 0.0220(11) 0.0255(11) 0.0150(10) 0.0056(8) -0.0050(8) -0.0026(9) C13 0.0250(11) 0.0221(10) 0.0185(11) 0.0056(9) -0.0017(9) -0.0047(9) C14 0.0199(11) 0.0231(10) 0.0179(10) 0.0091(8) -0.0021(8) 0.0005(8) C15 0.0199(10) 0.0233(10) 0.0142(10) 0.0053(8) -0.0038(8) -0.0003(8) C16 0.0194(10) 0.0248(11) 0.0126(10) 0.0061(8) -0.0057(8) -0.0025(8) C17 0.0192(10) 0.0281(11) 0.0102(9) 0.0048(8) -0.0035(8) 0.0013(9) C18 0.0219(11) 0.0210(10) 0.0129(10) 0.0023(8) -0.0047(8) -0.0014(9) C19 0.0156(10) 0.0273(11) 0.0143(10) 0.0058(8) -0.0058(8) -0.0018(8) C20 0.0189(10) 0.0245(10) 0.0108(9) 0.0046(8) -0.0054(8) 0.0030(8) C21 0.0213(11) 0.0280(11) 0.0200(11) 0.0137(9) 0.0004(9) 0.0011(9) C22 0.0279(12) 0.0230(11) 0.0204(11) 0.0109(9) -0.0028(9) -0.0050(9) C23 0.0204(11) 0.0349(12) 0.0211(11) 0.0153(10) -0.0046(9) -0.0068(9) C24 0.0227(11) 0.0330(12) 0.0186(11) 0.0138(9) 0.0030(9) 0.0018(9) C25 0.0220(11) 0.0282(11) 0.0146(10) 0.0109(9) -0.0022(8) -0.0017(9) B3 0.0158(11) 0.0213(11) 0.0157(11) 0.0081(9) -0.0036(9) 0.0008(9) B4 0.0166(11) 0.0199(11) 0.0206(12) 0.0074(9) -0.0018(9) 0.0012(9) B5 0.0197(12) 0.0191(11) 0.0182(11) 0.0056(9) -0.0005(9) 0.0020(9) B6 0.0168(11) 0.0199(11) 0.0138(11) 0.0050(9) -0.0016(9) 0.0007(9) B7 0.0146(11) 0.0236(12) 0.0166(11) 0.0081(9) -0.0035(9) 0.0012(9) B8 0.0170(11) 0.0208(11) 0.0192(12) 0.0084(9) -0.0035(9) 0.0010(9) B9 0.0162(11) 0.0220(11) 0.0228(12) 0.0070(10) -0.0009(9) 0.0016(9) B10 0.0182(11) 0.0216(11) 0.0172(11) 0.0046(9) -0.0002(9) -0.0006(9) B11 0.0153(11) 0.0215(11) 0.0159(11) 0.0063(9) -0.0012(9) -0.0003(9) B12 0.0171(11) 0.0215(11) 0.0179(11) 0.0079(9) -0.0026(9) 0.0018(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr N1 2.0782(18) . ? Zr C2 2.433(2) . ? Zr C25 2.529(2) . ? Zr C24 2.534(2) . ? Zr C21 2.538(2) . ? Zr C16 2.539(2) . ? Zr C20 2.540(2) . ? Zr C17 2.540(2) . ? Zr C18 2.546(2) . ? Zr C19 2.558(2) . ? Zr C22 2.570(2) . ? Zr C23 2.571(2) . ? N1 C3 1.377(3) . ? N1 C4 1.460(3) . ? N2 C3 1.271(3) . ? N2 C10 1.451(3) . ? C1 C3 1.531(3) . ? C1 B7 1.711(3) . ? C1 B11 1.713(3) . ? C1 B6 1.713(3) . ? C1 B3 1.716(3) . ? C1 C2 1.717(3) . ? C2 B4 1.726(3) . ? C2 B5 1.729(3) . ? C2 B6 1.740(3) . ? C2 B3 1.741(3) . ? C4 C5 1.537(3) . ? C4 C9 1.542(3) . ? C4 H4A 1.0000 . ? C5 C6 1.531(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.532(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.524(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.533(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C15 1.533(3) . ? C10 C11 1.537(3) . ? C10 H10 1.0000 . ? C11 C12 1.530(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.532(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.530(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.530(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.407(3) . ? C16 C20 1.412(3) . ? C16 H16 0.9500 . ? C17 C18 1.424(3) . ? C17 H17 0.9500 . ? C18 C19 1.412(3) . ? C18 H18 0.9500 . ? C19 C20 1.413(3) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C25 1.407(3) . ? C21 C22 1.416(3) . ? C21 H21 0.9500 . ? C22 C23 1.412(4) . ? C22 H22 0.9500 . ? C23 C24 1.416(4) . ? C23 H23 0.9500 . ? C24 C25 1.414(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? B3 B4 1.774(4) . ? B3 B8 1.780(3) . ? B3 B7 1.787(3) . ? B3 H3 1.1200 . ? B4 B5 1.759(4) . ? B4 B9 1.776(4) . ? B4 B8 1.782(3) . ? B4 H4 1.1200 . ? B5 B6 1.772(3) . ? B5 B9 1.784(4) . ? B5 B10 1.787(4) . ? B5 H5 1.1200 . ? B6 B10 1.779(4) . ? B6 B11 1.790(3) . ? B6 H6 1.1200 . ? B7 B8 1.775(3) . ? B7 B12 1.778(4) . ? B7 B11 1.783(3) . ? B7 H7 1.1200 . ? B8 B9 1.782(4) . ? B8 B12 1.787(4) . ? B8 H8 1.1200 . ? B9 B12 1.774(4) . ? B9 B10 1.789(4) . ? B9 H9 1.1200 . ? B10 B11 1.777(3) . ? B10 B12 1.790(4) . ? B10 H10A 1.1200 . ? B11 B12 1.774(3) . ? B11 H11 1.1200 . ? B12 H12 1.1200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zr C2 71.57(7) . . ? N1 Zr C25 87.30(7) . . ? C2 Zr C25 93.95(7) . . ? N1 Zr C24 98.64(8) . . ? C2 Zr C24 126.35(7) . . ? C25 Zr C24 32.42(7) . . ? N1 Zr C21 109.59(7) . . ? C2 Zr C21 79.65(7) . . ? C25 Zr C21 32.23(8) . . ? C24 Zr C21 53.45(8) . . ? N1 Zr C16 85.97(7) . . ? C2 Zr C16 92.47(7) . . ? C25 Zr C16 168.75(8) . . ? C24 Zr C16 140.50(8) . . ? C21 Zr C16 158.85(8) . . ? N1 Zr C20 96.69(7) . . ? C2 Zr C20 124.76(7) . . ? C25 Zr C20 140.40(7) . . ? C24 Zr C20 108.55(7) . . ? C21 Zr C20 149.44(7) . . ? C16 Zr C20 32.29(7) . . ? N1 Zr C17 108.84(7) . . ? C2 Zr C17 79.01(7) . . ? C25 Zr C17 158.86(8) . . ? C24 Zr C17 148.06(8) . . ? C21 Zr C17 126.70(8) . . ? C16 Zr C17 32.17(7) . . ? C20 Zr C17 53.36(7) . . ? N1 Zr C18 139.04(7) . . ? C2 Zr C18 101.21(7) . . ? C25 Zr C18 133.65(8) . . ? C24 Zr C18 116.07(8) . . ? C21 Zr C18 108.45(8) . . ? C16 Zr C18 53.53(7) . . ? C20 Zr C18 53.33(7) . . ? C17 Zr C18 32.51(7) . . ? N1 Zr C19 128.63(7) . . ? C2 Zr C19 131.40(7) . . ? C25 Zr C19 126.33(7) . . ? C24 Zr C19 96.63(7) . . ? C21 Zr C19 118.80(8) . . ? C16 Zr C19 53.41(7) . . ? C20 Zr C19 32.17(7) . . ? C17 Zr C19 53.43(7) . . ? C18 Zr C19 32.12(7) . . ? N1 Zr C22 139.92(7) . . ? C2 Zr C22 100.79(7) . . ? C25 Zr C22 53.35(8) . . ? C24 Zr C22 53.30(8) . . ? C21 Zr C22 32.18(7) . . ? C16 Zr C22 134.10(7) . . ? C20 Zr C22 117.93(7) . . ? C17 Zr C22 107.99(8) . . ? C18 Zr C22 80.72(8) . . ? C19 Zr C22 86.63(7) . . ? N1 Zr C23 130.69(7) . . ? C2 Zr C23 131.22(7) . . ? C25 Zr C23 53.30(7) . . ? C24 Zr C23 32.20(8) . . ? C21 Zr C23 53.07(7) . . ? C16 Zr C23 126.82(7) . . ? C20 Zr C23 97.94(7) . . ? C17 Zr C23 117.64(8) . . ? C18 Zr C23 85.13(8) . . ? C19 Zr C23 73.66(7) . . ? C22 Zr C23 31.88(8) . . ? C3 N1 C4 121.46(18) . . ? C3 N1 Zr 137.30(15) . . ? C4 N1 Zr 101.19(13) . . ? C3 N2 C10 126.88(19) . . ? C3 C1 B7 124.68(17) . . ? C3 C1 B11 124.29(17) . . ? B7 C1 B11 62.77(14) . . ? C3 C1 B6 115.23(17) . . ? B7 C1 B6 114.38(17) . . ? B11 C1 B6 63.01(13) . . ? C3 C1 B3 115.77(17) . . ? B7 C1 B3 62.88(14) . . ? B11 C1 B3 114.33(17) . . ? B6 C1 B3 112.74(16) . . ? C3 C1 C2 112.26(17) . . ? B7 C1 C2 112.09(16) . . ? B11 C1 C2 112.18(16) . . ? B6 C1 C2 60.96(13) . . ? B3 C1 C2 60.96(13) . . ? C1 C2 B4 107.39(16) . . ? C1 C2 B5 107.46(16) . . ? B4 C2 B5 61.21(14) . . ? C1 C2 B6 59.42(12) . . ? B4 C2 B6 110.81(17) . . ? B5 C2 B6 61.43(13) . . ? C1 C2 B3 59.49(12) . . ? B4 C2 B3 61.55(14) . . ? B5 C2 B3 111.15(17) . . ? B6 C2 B3 110.22(16) . . ? C1 C2 Zr 109.44(12) . . ? B4 C2 Zr 131.12(14) . . ? B5 C2 Zr 131.67(14) . . ? B6 C2 Zr 115.19(13) . . ? B3 C2 Zr 114.06(13) . . ? N2 C3 N1 121.5(2) . . ? N2 C3 C1 129.2(2) . . ? N1 C3 C1 109.34(18) . . ? N1 C4 C5 115.60(17) . . ? N1 C4 C9 114.27(17) . . ? C5 C4 C9 111.15(18) . . ? N1 C4 Zr 47.58(9) . . ? C5 C4 Zr 124.29(13) . . ? C9 C4 Zr 124.16(14) . . ? N1 C4 H4A 104.8 . . ? C5 C4 H4A 104.8 . . ? C9 C4 H4A 104.8 . . ? Zr C4 H4A 57.3 . . ? C6 C5 C4 110.87(18) . . ? C6 C5 H5A 109.5 . . ? C4 C5 H5A 109.5 . . ? C6 C5 H5B 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? C5 C6 C7 110.58(18) . . ? C5 C6 H6A 109.5 . . ? C7 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C8 C7 C6 111.4(2) . . ? C8 C7 H7A 109.4 . . ? C6 C7 H7A 109.4 . . ? C8 C7 H7B 109.4 . . ? C6 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? C7 C8 C9 111.27(19) . . ? C7 C8 H8A 109.4 . . ? C9 C8 H8A 109.4 . . ? C7 C8 H8B 109.4 . . ? C9 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C8 C9 C4 110.80(17) . . ? C8 C9 H9A 109.5 . . ? C4 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? N2 C10 C15 109.44(17) . . ? N2 C10 C11 107.55(18) . . ? C15 C10 C11 109.56(18) . . ? N2 C10 H10 110.1 . . ? C15 C10 H10 110.1 . . ? C11 C10 H10 110.1 . . ? C12 C11 C10 111.81(18) . . ? C12 C11 H11A 109.3 . . ? C10 C11 H11A 109.3 . . ? C12 C11 H11B 109.3 . . ? C10 C11 H11B 109.3 . . ? H11A C11 H11B 107.9 . . ? C11 C12 C13 111.31(18) . . ? C11 C12 H12A 109.4 . . ? C13 C12 H12A 109.4 . . ? C11 C12 H12B 109.4 . . ? C13 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? C14 C13 C12 112.18(18) . . ? C14 C13 H13A 109.2 . . ? C12 C13 H13A 109.2 . . ? C14 C13 H13B 109.2 . . ? C12 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? C13 C14 C15 110.98(19) . . ? C13 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? C13 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C14 C15 C10 110.61(18) . . ? C14 C15 H15A 109.5 . . ? C10 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? C17 C16 C20 108.0(2) . . ? C17 C16 Zr 73.97(12) . . ? C20 C16 Zr 73.89(12) . . ? C17 C16 H16 126.0 . . ? C20 C16 H16 126.0 . . ? Zr C16 H16 118.1 . . ? C16 C17 C18 108.0(2) . . ? C16 C17 Zr 73.86(12) . . ? C18 C17 Zr 73.97(12) . . ? C16 C17 H17 126.0 . . ? C18 C17 H17 126.0 . . ? Zr C17 H17 118.1 . . ? C19 C18 C17 107.9(2) . . ? C19 C18 Zr 74.43(12) . . ? C17 C18 Zr 73.52(12) . . ? C19 C18 H18 126.1 . . ? C17 C18 H18 126.1 . . ? Zr C18 H18 118.0 . . ? C18 C19 C20 107.8(2) . . ? C18 C19 Zr 73.46(12) . . ? C20 C19 Zr 73.18(12) . . ? C18 C19 H19 126.1 . . ? C20 C19 H19 126.1 . . ? Zr C19 H19 119.2 . . ? C16 C20 C19 108.4(2) . . ? C16 C20 Zr 73.82(12) . . ? C19 C20 Zr 74.65(12) . . ? C16 C20 H20 125.8 . . ? C19 C20 H20 125.8 . . ? Zr C20 H20 117.7 . . ? C25 C21 C22 108.4(2) . . ? C25 C21 Zr 73.52(13) . . ? C22 C21 Zr 75.13(13) . . ? C25 C21 H21 125.8 . . ? C22 C21 H21 125.8 . . ? Zr C21 H21 117.5 . . ? C23 C22 C21 107.6(2) . . ? C23 C22 Zr 74.12(13) . . ? C21 C22 Zr 72.69(13) . . ? C23 C22 H22 126.2 . . ? C21 C22 H22 126.2 . . ? Zr C22 H22 118.9 . . ? C22 C23 C24 108.1(2) . . ? C22 C23 Zr 73.99(13) . . ? C24 C23 Zr 72.46(13) . . ? C22 C23 H23 126.0 . . ? C24 C23 H23 126.0 . . ? Zr C23 H23 119.4 . . ? C25 C24 C23 107.9(2) . . ? C25 C24 Zr 73.59(13) . . ? C23 C24 Zr 75.34(13) . . ? C25 C24 H24 126.1 . . ? C23 C24 H24 126.1 . . ? Zr C24 H24 117.1 . . ? C21 C25 C24 108.0(2) . . ? C21 C25 Zr 74.24(13) . . ? C24 C25 Zr 73.99(13) . . ? C21 C25 H25 126.0 . . ? C24 C25 H25 126.0 . . ? Zr C25 H25 117.7 . . ? C1 B3 C2 59.55(12) . . ? C1 B3 B4 105.31(16) . . ? C2 B3 B4 58.81(13) . . ? C1 B3 B8 104.81(16) . . ? C2 B3 B8 106.73(17) . . ? B4 B3 B8 60.18(14) . . ? C1 B3 B7 58.43(13) . . ? C2 B3 B7 107.37(16) . . ? B4 B3 B7 107.78(17) . . ? B8 B3 B7 59.69(14) . . ? C1 B3 H3 124.1 . . ? C2 B3 H3 122.2 . . ? B4 B3 H3 122.4 . . ? B8 B3 H3 122.7 . . ? B7 B3 H3 121.9 . . ? C2 B4 B5 59.47(13) . . ? C2 B4 B3 59.64(13) . . ? B5 B4 B3 108.20(17) . . ? C2 B4 B9 107.31(17) . . ? B5 B4 B9 60.62(14) . . ? B3 B4 B9 108.15(17) . . ? C2 B4 B8 107.29(17) . . ? B5 B4 B8 108.77(17) . . ? B3 B4 B8 60.07(14) . . ? B9 B4 B8 60.11(14) . . ? C2 B4 H4 122.6 . . ? B5 B4 H4 121.2 . . ? B3 B4 H4 121.7 . . ? B9 B4 H4 121.6 . . ? B8 B4 H4 121.6 . . ? C2 B5 B4 59.31(13) . . ? C2 B5 B6 59.58(13) . . ? B4 B5 B6 107.80(17) . . ? C2 B5 B9 106.84(17) . . ? B4 B5 B9 60.17(14) . . ? B6 B5 B9 107.82(17) . . ? C2 B5 B10 107.16(17) . . ? B4 B5 B10 108.37(18) . . ? B6 B5 B10 59.99(14) . . ? B9 B5 B10 60.12(14) . . ? C2 B5 H5 122.8 . . ? B4 B5 H5 121.6 . . ? B6 B5 H5 121.8 . . ? B9 B5 H5 121.9 . . ? B10 B5 H5 121.6 . . ? C1 B6 C2 59.62(12) . . ? C1 B6 B5 105.71(16) . . ? C2 B6 B5 58.99(13) . . ? C1 B6 B10 105.07(17) . . ? C2 B6 B10 107.05(17) . . ? B5 B6 B10 60.44(14) . . ? C1 B6 B11 58.49(13) . . ? C2 B6 B11 107.47(16) . . ? B5 B6 B11 108.08(17) . . ? B10 B6 B11 59.71(14) . . ? C1 B6 H6 123.9 . . ? C2 B6 H6 122.1 . . ? B5 B6 H6 122.1 . . ? B10 B6 H6 122.5 . . ? B11 B6 H6 121.8 . . ? C1 B7 B8 105.21(17) . . ? C1 B7 B12 104.90(17) . . ? B8 B7 B12 60.38(14) . . ? C1 B7 B11 58.67(13) . . ? B8 B7 B11 108.14(17) . . ? B12 B7 B11 59.78(14) . . ? C1 B7 B3 58.69(13) . . ? B8 B7 B3 59.95(14) . . ? B12 B7 B3 107.90(17) . . ? B11 B7 B3 107.58(17) . . ? C1 B7 H7 124.5 . . ? B8 B7 H7 122.0 . . ? B12 B7 H7 122.3 . . ? B11 B7 H7 121.7 . . ? B3 B7 H7 121.7 . . ? B7 B8 B3 60.36(14) . . ? B7 B8 B4 107.98(17) . . ? B3 B8 B4 59.75(14) . . ? B7 B8 B9 107.75(17) . . ? B3 B8 B9 107.65(17) . . ? B4 B8 B9 59.79(14) . . ? B7 B8 B12 59.88(14) . . ? B3 B8 B12 107.84(17) . . ? B4 B8 B12 107.39(17) . . ? B9 B8 B12 59.62(14) . . ? B7 B8 H8 121.6 . . ? B3 B8 H8 121.7 . . ? B4 B8 H8 122.0 . . ? B9 B8 H8 122.0 . . ? B12 B8 H8 122.1 . . ? B12 B9 B4 108.17(17) . . ? B12 B9 B8 60.31(14) . . ? B4 B9 B8 60.09(14) . . ? B12 B9 B5 108.17(17) . . ? B4 B9 B5 59.21(14) . . ? B8 B9 B5 107.63(18) . . ? B12 B9 B10 60.31(14) . . ? B4 B9 B10 107.52(17) . . ? B8 B9 B10 108.36(17) . . ? B5 B9 B10 60.02(14) . . ? B12 B9 H9 121.3 . . ? B4 B9 H9 122.1 . . ? B8 B9 H9 121.5 . . ? B5 B9 H9 122.1 . . ? B10 B9 H9 121.6 . . ? B11 B10 B6 60.46(14) . . ? B11 B10 B5 107.99(17) . . ? B6 B10 B5 59.58(14) . . ? B11 B10 B9 107.38(17) . . ? B6 B10 B9 107.30(17) . . ? B5 B10 B9 59.86(14) . . ? B11 B10 B12 59.67(14) . . ? B6 B10 B12 107.59(17) . . ? B5 B10 B12 107.35(17) . . ? B9 B10 B12 59.44(14) . . ? B11 B10 H10A 121.7 . . ? B6 B10 H10A 121.9 . . ? B5 B10 H10A 121.9 . . ? B9 B10 H10A 122.3 . . ? B12 B10 H10A 122.2 . . ? C1 B11 B12 104.95(17) . . ? C1 B11 B10 105.18(16) . . ? B12 B11 B10 60.53(14) . . ? C1 B11 B7 58.56(13) . . ? B12 B11 B7 59.96(14) . . ? B10 B11 B7 108.37(17) . . ? C1 B11 B6 58.50(13) . . ? B12 B11 B6 107.78(17) . . ? B10 B11 B6 59.83(14) . . ? B7 B11 B6 107.29(17) . . ? C1 B11 H11 124.6 . . ? B12 B11 H11 122.2 . . ? B10 B11 H11 121.9 . . ? B7 B11 H11 121.7 . . ? B6 B11 H11 122.0 . . ? B9 B12 B11 108.15(17) . . ? B9 B12 B7 107.99(17) . . ? B11 B12 B7 60.26(14) . . ? B9 B12 B8 60.06(14) . . ? B11 B12 B8 108.02(17) . . ? B7 B12 B8 59.74(14) . . ? B9 B12 B10 60.26(14) . . ? B11 B12 B10 59.80(14) . . ? B7 B12 B10 108.03(17) . . ? B8 B12 B10 108.12(17) . . ? B9 B12 H12 121.6 . . ? B11 B12 H12 121.7 . . ? B7 B12 H12 121.7 . . ? B8 B12 H12 121.8 . . ? B10 B12 H12 121.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Zr N1 C3 2.8(2) . . . . ? C25 Zr N1 C3 97.8(2) . . . . ? C24 Zr N1 C3 128.3(2) . . . . ? C21 Zr N1 C3 74.1(2) . . . . ? C16 Zr N1 C3 -91.2(2) . . . . ? C20 Zr N1 C3 -121.7(2) . . . . ? C17 Zr N1 C3 -68.2(2) . . . . ? C18 Zr N1 C3 -83.2(2) . . . . ? C19 Zr N1 C3 -126.0(2) . . . . ? C22 Zr N1 C3 87.6(2) . . . . ? C23 Zr N1 C3 131.8(2) . . . . ? C2 Zr N1 C4 -179.94(14) . . . . ? C25 Zr N1 C4 -84.87(13) . . . . ? C24 Zr N1 C4 -54.40(13) . . . . ? C21 Zr N1 C4 -108.57(13) . . . . ? C16 Zr N1 C4 86.11(13) . . . . ? C20 Zr N1 C4 55.59(13) . . . . ? C17 Zr N1 C4 109.09(12) . . . . ? C18 Zr N1 C4 94.15(15) . . . . ? C19 Zr N1 C4 51.31(15) . . . . ? C22 Zr N1 C4 -95.08(15) . . . . ? C23 Zr N1 C4 -50.93(16) . . . . ? C3 C1 C2 B4 -148.26(17) . . . . ? B7 C1 C2 B4 -2.2(2) . . . . ? B11 C1 C2 B4 66.2(2) . . . . ? B6 C1 C2 B4 104.32(18) . . . . ? B3 C1 C2 B4 -40.19(16) . . . . ? C3 C1 C2 B5 147.24(17) . . . . ? B7 C1 C2 B5 -66.7(2) . . . . ? B11 C1 C2 B5 1.7(2) . . . . ? B6 C1 C2 B5 39.82(16) . . . . ? B3 C1 C2 B5 -104.69(17) . . . . ? C3 C1 C2 B6 107.43(18) . . . . ? B7 C1 C2 B6 -106.51(18) . . . . ? B11 C1 C2 B6 -38.09(16) . . . . ? B3 C1 C2 B6 -144.51(17) . . . . ? C3 C1 C2 B3 -108.07(18) . . . . ? B7 C1 C2 B3 37.99(16) . . . . ? B11 C1 C2 B3 106.41(18) . . . . ? B6 C1 C2 B3 144.51(17) . . . . ? C3 C1 C2 Zr -0.98(19) . . . . ? B7 C1 C2 Zr 145.08(13) . . . . ? B11 C1 C2 Zr -146.50(14) . . . . ? B6 C1 C2 Zr -108.40(14) . . . . ? B3 C1 C2 Zr 107.09(14) . . . . ? N1 Zr C2 C1 -0.45(12) . . . . ? C25 Zr C2 C1 -86.28(13) . . . . ? C24 Zr C2 C1 -87.65(14) . . . . ? C21 Zr C2 C1 -115.29(13) . . . . ? C16 Zr C2 C1 84.48(13) . . . . ? C20 Zr C2 C1 84.86(14) . . . . ? C17 Zr C2 C1 113.85(13) . . . . ? C18 Zr C2 C1 137.75(12) . . . . ? C19 Zr C2 C1 125.24(13) . . . . ? C22 Zr C2 C1 -139.70(12) . . . . ? C23 Zr C2 C1 -128.89(13) . . . . ? N1 Zr C2 B4 136.34(19) . . . . ? C25 Zr C2 B4 50.51(19) . . . . ? C24 Zr C2 B4 49.1(2) . . . . ? C21 Zr C2 B4 21.50(18) . . . . ? C16 Zr C2 B4 -138.74(18) . . . . ? C20 Zr C2 B4 -138.35(17) . . . . ? C17 Zr C2 B4 -109.37(19) . . . . ? C18 Zr C2 B4 -85.47(18) . . . . ? C19 Zr C2 B4 -97.97(19) . . . . ? C22 Zr C2 B4 -2.91(19) . . . . ? C23 Zr C2 B4 7.9(2) . . . . ? N1 Zr C2 B5 -138.19(19) . . . . ? C25 Zr C2 B5 135.99(18) . . . . ? C24 Zr C2 B5 134.61(17) . . . . ? C21 Zr C2 B5 106.97(19) . . . . ? C16 Zr C2 B5 -53.26(18) . . . . ? C20 Zr C2 B5 -52.9(2) . . . . ? C17 Zr C2 B5 -23.89(18) . . . . ? C18 Zr C2 B5 0.01(19) . . . . ? C19 Zr C2 B5 -12.5(2) . . . . ? C22 Zr C2 B5 82.57(18) . . . . ? C23 Zr C2 B5 93.38(19) . . . . ? N1 Zr C2 B6 -64.97(14) . . . . ? C25 Zr C2 B6 -150.80(14) . . . . ? C24 Zr C2 B6 -152.18(13) . . . . ? C21 Zr C2 B6 -179.81(15) . . . . ? C16 Zr C2 B6 19.95(14) . . . . ? C20 Zr C2 B6 20.34(17) . . . . ? C17 Zr C2 B6 49.33(14) . . . . ? C18 Zr C2 B6 73.23(14) . . . . ? C19 Zr C2 B6 60.72(17) . . . . ? C22 Zr C2 B6 155.78(14) . . . . ? C23 Zr C2 B6 166.59(13) . . . . ? N1 Zr C2 B3 63.95(14) . . . . ? C25 Zr C2 B3 -21.87(14) . . . . ? C24 Zr C2 B3 -23.25(17) . . . . ? C21 Zr C2 B3 -50.88(14) . . . . ? C16 Zr C2 B3 148.88(14) . . . . ? C20 Zr C2 B3 149.27(13) . . . . ? C17 Zr C2 B3 178.25(15) . . . . ? C18 Zr C2 B3 -157.85(13) . . . . ? C19 Zr C2 B3 -170.35(12) . . . . ? C22 Zr C2 B3 -75.29(14) . . . . ? C23 Zr C2 B3 -64.48(17) . . . . ? C10 N2 C3 N1 -179.78(19) . . . . ? C10 N2 C3 C1 -0.7(4) . . . . ? C4 N1 C3 N2 -1.6(3) . . . . ? Zr N1 C3 N2 175.26(16) . . . . ? C4 N1 C3 C1 179.14(17) . . . . ? Zr N1 C3 C1 -4.0(3) . . . . ? B7 C1 C3 N2 42.3(3) . . . . ? B11 C1 C3 N2 -36.1(3) . . . . ? B6 C1 C3 N2 -109.5(2) . . . . ? B3 C1 C3 N2 115.9(2) . . . . ? C2 C1 C3 N2 -176.7(2) . . . . ? B7 C1 C3 N1 -138.58(19) . . . . ? B11 C1 C3 N1 143.05(19) . . . . ? B6 C1 C3 N1 69.7(2) . . . . ? B3 C1 C3 N1 -64.9(2) . . . . ? C2 C1 C3 N1 2.4(2) . . . . ? C3 N1 C4 C5 63.8(3) . . . . ? Zr N1 C4 C5 -114.11(16) . . . . ? C3 N1 C4 C9 -67.2(3) . . . . ? Zr N1 C4 C9 114.98(16) . . . . ? C3 N1 C4 Zr 177.9(2) . . . . ? C2 Zr C4 N1 0.06(13) . . . . ? C25 Zr C4 N1 92.99(13) . . . . ? C24 Zr C4 N1 125.34(13) . . . . ? C21 Zr C4 N1 84.71(13) . . . . ? C16 Zr C4 N1 -91.24(13) . . . . ? C20 Zr C4 N1 -123.40(13) . . . . ? C17 Zr C4 N1 -83.79(13) . . . . ? C18 Zr C4 N1 -118.23(13) . . . . ? C19 Zr C4 N1 -140.56(12) . . . . ? C22 Zr C4 N1 118.48(14) . . . . ? C23 Zr C4 N1 141.75(12) . . . . ? N1 Zr C4 C5 94.9(2) . . . . ? C2 Zr C4 C5 94.96(17) . . . . ? C25 Zr C4 C5 -172.11(17) . . . . ? C24 Zr C4 C5 -139.76(17) . . . . ? C21 Zr C4 C5 179.60(16) . . . . ? C16 Zr C4 C5 3.66(17) . . . . ? C20 Zr C4 C5 -28.51(16) . . . . ? C17 Zr C4 C5 11.10(19) . . . . ? C18 Zr C4 C5 -23.3(2) . . . . ? C19 Zr C4 C5 -45.66(18) . . . . ? C22 Zr C4 C5 -146.62(16) . . . . ? C23 Zr C4 C5 -123.36(17) . . . . ? N1 Zr C4 C9 -93.0(2) . . . . ? C2 Zr C4 C9 -92.97(17) . . . . ? C25 Zr C4 C9 -0.04(17) . . . . ? C24 Zr C4 C9 32.31(17) . . . . ? C21 Zr C4 C9 -8.33(19) . . . . ? C16 Zr C4 C9 175.73(17) . . . . ? C20 Zr C4 C9 143.57(17) . . . . ? C17 Zr C4 C9 -176.83(16) . . . . ? C18 Zr C4 C9 148.74(15) . . . . ? C19 Zr C4 C9 126.41(16) . . . . ? C22 Zr C4 C9 25.4(2) . . . . ? C23 Zr C4 C9 48.72(18) . . . . ? N1 C4 C5 C6 171.54(17) . . . . ? C9 C4 C5 C6 -56.1(2) . . . . ? Zr C4 C5 C6 116.89(17) . . . . ? C4 C5 C6 C7 56.5(3) . . . . ? C5 C6 C7 C8 -56.8(3) . . . . ? C6 C7 C8 C9 56.3(3) . . . . ? C7 C8 C9 C4 -55.2(3) . . . . ? N1 C4 C9 C8 -171.76(18) . . . . ? C5 C4 C9 C8 55.2(2) . . . . ? Zr C4 C9 C8 -117.79(18) . . . . ? C3 N2 C10 C15 109.9(2) . . . . ? C3 N2 C10 C11 -131.2(2) . . . . ? N2 C10 C11 C12 -176.16(18) . . . . ? C15 C10 C11 C12 -57.3(2) . . . . ? C10 C11 C12 C13 54.2(3) . . . . ? C11 C12 C13 C14 -52.4(3) . . . . ? C12 C13 C14 C15 54.3(3) . . . . ? C13 C14 C15 C10 -57.6(2) . . . . ? N2 C10 C15 C14 176.41(18) . . . . ? C11 C10 C15 C14 58.7(2) . . . . ? N1 Zr C16 C17 136.05(14) . . . . ? C2 Zr C16 C17 64.73(14) . . . . ? C25 Zr C16 C17 -170.5(3) . . . . ? C24 Zr C16 C17 -125.25(15) . . . . ? C21 Zr C16 C17 -2.5(3) . . . . ? C20 Zr C16 C17 -114.68(19) . . . . ? C18 Zr C16 C17 -37.41(13) . . . . ? C19 Zr C16 C17 -77.68(14) . . . . ? C22 Zr C16 C17 -42.88(18) . . . . ? C23 Zr C16 C17 -84.16(16) . . . . ? N1 Zr C16 C20 -109.27(13) . . . . ? C2 Zr C16 C20 179.41(13) . . . . ? C25 Zr C16 C20 -55.8(4) . . . . ? C24 Zr C16 C20 -10.58(19) . . . . ? C21 Zr C16 C20 112.2(2) . . . . ? C17 Zr C16 C20 114.68(19) . . . . ? C18 Zr C16 C20 77.27(14) . . . . ? C19 Zr C16 C20 37.00(13) . . . . ? C22 Zr C16 C20 71.79(16) . . . . ? C23 Zr C16 C20 30.52(17) . . . . ? C20 C16 C17 C18 0.1(2) . . . . ? Zr C16 C17 C18 66.67(15) . . . . ? C20 C16 C17 Zr -66.61(15) . . . . ? N1 Zr C17 C16 -47.01(15) . . . . ? C2 Zr C17 C16 -113.02(14) . . . . ? C25 Zr C17 C16 174.89(18) . . . . ? C24 Zr C17 C16 100.90(18) . . . . ? C21 Zr C17 C16 178.87(13) . . . . ? C20 Zr C17 C16 37.23(13) . . . . ? C18 Zr C17 C16 114.65(19) . . . . ? C19 Zr C17 C16 77.61(14) . . . . ? C22 Zr C17 C16 149.08(13) . . . . ? C23 Zr C17 C16 115.98(14) . . . . ? N1 Zr C17 C18 -161.67(13) . . . . ? C2 Zr C17 C18 132.32(14) . . . . ? C25 Zr C17 C18 60.2(3) . . . . ? C24 Zr C17 C18 -13.8(2) . . . . ? C21 Zr C17 C18 64.22(16) . . . . ? C16 Zr C17 C18 -114.65(19) . . . . ? C20 Zr C17 C18 -77.42(14) . . . . ? C19 Zr C17 C18 -37.04(13) . . . . ? C22 Zr C17 C18 34.43(15) . . . . ? C23 Zr C17 C18 1.33(16) . . . . ? C16 C17 C18 C19 0.5(2) . . . . ? Zr C17 C18 C19 67.08(15) . . . . ? C16 C17 C18 Zr -66.60(15) . . . . ? N1 Zr C18 C19 -87.48(16) . . . . ? C2 Zr C18 C19 -162.21(13) . . . . ? C25 Zr C18 C19 91.16(16) . . . . ? C24 Zr C18 C19 57.47(15) . . . . ? C21 Zr C18 C19 115.08(14) . . . . ? C16 Zr C18 C19 -77.49(15) . . . . ? C20 Zr C18 C19 -36.97(13) . . . . ? C17 Zr C18 C19 -114.5(2) . . . . ? C22 Zr C18 C19 98.53(14) . . . . ? C23 Zr C18 C19 66.69(14) . . . . ? N1 Zr C18 C17 27.01(19) . . . . ? C2 Zr C18 C17 -47.73(14) . . . . ? C25 Zr C18 C17 -154.36(13) . . . . ? C24 Zr C18 C17 171.95(13) . . . . ? C21 Zr C18 C17 -130.44(13) . . . . ? C16 Zr C18 C17 37.00(13) . . . . ? C20 Zr C18 C17 77.51(14) . . . . ? C19 Zr C18 C17 114.5(2) . . . . ? C22 Zr C18 C17 -146.99(14) . . . . ? C23 Zr C18 C17 -178.82(14) . . . . ? C17 C18 C19 C20 -0.8(2) . . . . ? Zr C18 C19 C20 65.64(15) . . . . ? C17 C18 C19 Zr -66.47(15) . . . . ? N1 Zr C19 C18 123.04(14) . . . . ? C2 Zr C19 C18 23.54(17) . . . . ? C25 Zr C19 C18 -116.11(14) . . . . ? C24 Zr C19 C18 -130.32(14) . . . . ? C21 Zr C19 C18 -78.66(15) . . . . ? C16 Zr C19 C18 77.89(14) . . . . ? C20 Zr C19 C18 115.04(19) . . . . ? C17 Zr C19 C18 37.52(13) . . . . ? C22 Zr C19 C18 -77.88(14) . . . . ? C23 Zr C19 C18 -107.52(15) . . . . ? N1 Zr C19 C20 8.00(17) . . . . ? C2 Zr C19 C20 -91.49(15) . . . . ? C25 Zr C19 C20 128.85(13) . . . . ? C24 Zr C19 C20 114.64(13) . . . . ? C21 Zr C19 C20 166.30(12) . . . . ? C16 Zr C19 C20 -37.15(13) . . . . ? C17 Zr C19 C20 -77.52(14) . . . . ? C18 Zr C19 C20 -115.04(19) . . . . ? C22 Zr C19 C20 167.09(14) . . . . ? C23 Zr C19 C20 137.45(14) . . . . ? C17 C16 C20 C19 -0.6(2) . . . . ? Zr C16 C20 C19 -67.24(15) . . . . ? C17 C16 C20 Zr 66.67(15) . . . . ? C18 C19 C20 C16 0.9(2) . . . . ? Zr C19 C20 C16 66.69(15) . . . . ? C18 C19 C20 Zr -65.82(15) . . . . ? N1 Zr C20 C16 71.46(13) . . . . ? C2 Zr C20 C16 -0.72(16) . . . . ? C25 Zr C20 C16 165.33(13) . . . . ? C24 Zr C20 C16 172.93(13) . . . . ? C21 Zr C20 C16 -138.92(16) . . . . ? C17 Zr C20 C16 -37.08(13) . . . . ? C18 Zr C20 C16 -77.92(14) . . . . ? C19 Zr C20 C16 -114.83(19) . . . . ? C22 Zr C20 C16 -129.45(13) . . . . ? C23 Zr C20 C16 -155.76(13) . . . . ? N1 Zr C20 C19 -173.71(13) . . . . ? C2 Zr C20 C19 114.11(13) . . . . ? C25 Zr C20 C19 -79.84(17) . . . . ? C24 Zr C20 C19 -72.24(14) . . . . ? C21 Zr C20 C19 -24.1(2) . . . . ? C16 Zr C20 C19 114.83(19) . . . . ? C17 Zr C20 C19 77.75(14) . . . . ? C18 Zr C20 C19 36.91(13) . . . . ? C22 Zr C20 C19 -14.63(16) . . . . ? C23 Zr C20 C19 -40.94(14) . . . . ? N1 Zr C21 C25 48.85(15) . . . . ? C2 Zr C21 C25 114.88(14) . . . . ? C24 Zr C21 C25 -37.40(13) . . . . ? C16 Zr C21 C25 -175.64(17) . . . . ? C20 Zr C21 C25 -98.94(18) . . . . ? C17 Zr C21 C25 -177.31(13) . . . . ? C18 Zr C21 C25 -146.63(13) . . . . ? C19 Zr C21 C25 -113.30(14) . . . . ? C22 Zr C21 C25 -114.8(2) . . . . ? C23 Zr C21 C25 -77.90(15) . . . . ? N1 Zr C21 C22 163.62(14) . . . . ? C2 Zr C21 C22 -130.34(15) . . . . ? C25 Zr C21 C22 114.8(2) . . . . ? C24 Zr C21 C22 77.37(15) . . . . ? C16 Zr C21 C22 -60.9(3) . . . . ? C20 Zr C21 C22 15.8(2) . . . . ? C17 Zr C21 C22 -62.54(17) . . . . ? C18 Zr C21 C22 -31.86(16) . . . . ? C19 Zr C21 C22 1.47(17) . . . . ? C23 Zr C21 C22 36.88(14) . . . . ? C25 C21 C22 C23 0.1(3) . . . . ? Zr C21 C22 C23 -66.43(16) . . . . ? C25 C21 C22 Zr 66.57(15) . . . . ? N1 Zr C22 C23 90.38(17) . . . . ? C2 Zr C22 C23 164.51(13) . . . . ? C25 Zr C22 C23 77.62(15) . . . . ? C24 Zr C22 C23 36.88(14) . . . . ? C21 Zr C22 C23 114.8(2) . . . . ? C16 Zr C22 C23 -91.27(16) . . . . ? C20 Zr C22 C23 -56.21(16) . . . . ? C17 Zr C22 C23 -113.66(14) . . . . ? C18 Zr C22 C23 -95.73(14) . . . . ? C19 Zr C22 C23 -63.95(14) . . . . ? N1 Zr C22 C21 -24.4(2) . . . . ? C2 Zr C22 C21 49.75(15) . . . . ? C25 Zr C22 C21 -37.13(14) . . . . ? C24 Zr C22 C21 -77.87(15) . . . . ? C16 Zr C22 C21 153.97(13) . . . . ? C20 Zr C22 C21 -170.97(13) . . . . ? C17 Zr C22 C21 131.58(14) . . . . ? C18 Zr C22 C21 149.51(15) . . . . ? C19 Zr C22 C21 -178.71(15) . . . . ? C23 Zr C22 C21 -114.8(2) . . . . ? C21 C22 C23 C24 0.5(3) . . . . ? Zr C22 C23 C24 -64.94(16) . . . . ? C21 C22 C23 Zr 65.48(15) . . . . ? N1 Zr C23 C22 -121.88(14) . . . . ? C2 Zr C23 C22 -20.41(18) . . . . ? C25 Zr C23 C22 -77.81(15) . . . . ? C24 Zr C23 C22 -115.4(2) . . . . ? C21 Zr C23 C22 -37.23(13) . . . . ? C16 Zr C23 C22 116.25(14) . . . . ? C20 Zr C23 C22 132.15(14) . . . . ? C17 Zr C23 C22 79.53(15) . . . . ? C18 Zr C23 C22 80.24(14) . . . . ? C19 Zr C23 C22 110.83(15) . . . . ? N1 Zr C23 C24 -6.44(18) . . . . ? C2 Zr C23 C24 95.03(16) . . . . ? C25 Zr C23 C24 37.63(14) . . . . ? C21 Zr C23 C24 78.21(15) . . . . ? C16 Zr C23 C24 -128.31(14) . . . . ? C20 Zr C23 C24 -112.41(14) . . . . ? C17 Zr C23 C24 -165.03(13) . . . . ? C18 Zr C23 C24 -164.32(15) . . . . ? C19 Zr C23 C24 -133.73(15) . . . . ? C22 Zr C23 C24 115.4(2) . . . . ? C22 C23 C24 C25 -1.0(3) . . . . ? Zr C23 C24 C25 -66.96(15) . . . . ? C22 C23 C24 Zr 65.95(16) . . . . ? N1 Zr C24 C25 -70.86(15) . . . . ? C2 Zr C24 C25 2.57(18) . . . . ? C21 Zr C24 C25 37.18(14) . . . . ? C16 Zr C24 C25 -165.02(13) . . . . ? C20 Zr C24 C25 -170.95(14) . . . . ? C17 Zr C24 C25 139.71(16) . . . . ? C18 Zr C24 C25 131.53(14) . . . . ? C19 Zr C24 C25 158.35(14) . . . . ? C22 Zr C24 C25 77.58(15) . . . . ? C23 Zr C24 C25 114.1(2) . . . . ? N1 Zr C24 C23 175.06(14) . . . . ? C2 Zr C24 C23 -111.51(15) . . . . ? C25 Zr C24 C23 -114.1(2) . . . . ? C21 Zr C24 C23 -76.91(15) . . . . ? C16 Zr C24 C23 80.90(18) . . . . ? C20 Zr C24 C23 74.97(15) . . . . ? C17 Zr C24 C23 25.6(2) . . . . ? C18 Zr C24 C23 17.45(17) . . . . ? C19 Zr C24 C23 44.27(15) . . . . ? C22 Zr C24 C23 -36.50(14) . . . . ? C22 C21 C25 C24 -0.8(3) . . . . ? Zr C21 C25 C24 66.87(15) . . . . ? C22 C21 C25 Zr -67.64(16) . . . . ? C23 C24 C25 C21 1.1(3) . . . . ? Zr C24 C25 C21 -67.04(15) . . . . ? C23 C24 C25 Zr 68.14(16) . . . . ? N1 Zr C25 C21 -134.75(14) . . . . ? C2 Zr C25 C21 -63.45(14) . . . . ? C24 Zr C25 C21 114.5(2) . . . . ? C16 Zr C25 C21 171.9(3) . . . . ? C20 Zr C25 C21 128.00(14) . . . . ? C17 Zr C25 C21 6.0(3) . . . . ? C18 Zr C25 C21 46.14(18) . . . . ? C19 Zr C25 C21 87.42(15) . . . . ? C22 Zr C25 C21 37.06(14) . . . . ? C23 Zr C25 C21 77.12(15) . . . . ? N1 Zr C25 C24 110.77(15) . . . . ? C2 Zr C25 C24 -177.93(14) . . . . ? C21 Zr C25 C24 -114.5(2) . . . . ? C16 Zr C25 C24 57.4(4) . . . . ? C20 Zr C25 C24 13.5(2) . . . . ? C17 Zr C25 C24 -108.5(2) . . . . ? C18 Zr C25 C24 -68.34(17) . . . . ? C19 Zr C25 C24 -27.06(17) . . . . ? C22 Zr C25 C24 -77.42(15) . . . . ? C23 Zr C25 C24 -37.36(14) . . . . ? C3 C1 B3 C2 102.30(19) . . . . ? B7 C1 B3 C2 -140.14(17) . . . . ? B11 C1 B3 C2 -102.87(18) . . . . ? B6 C1 B3 C2 -33.39(16) . . . . ? C3 C1 B3 B4 140.70(18) . . . . ? B7 C1 B3 B4 -101.74(18) . . . . ? B11 C1 B3 B4 -64.5(2) . . . . ? B6 C1 B3 B4 5.0(2) . . . . ? C2 C1 B3 B4 38.40(15) . . . . ? C3 C1 B3 B8 -156.75(17) . . . . ? B7 C1 B3 B8 -39.19(16) . . . . ? B11 C1 B3 B8 -1.9(2) . . . . ? B6 C1 B3 B8 67.6(2) . . . . ? C2 C1 B3 B8 100.95(17) . . . . ? C3 C1 B3 B7 -117.6(2) . . . . ? B11 C1 B3 B7 37.27(17) . . . . ? B6 C1 B3 B7 106.75(19) . . . . ? C2 C1 B3 B7 140.14(17) . . . . ? B4 C2 B3 C1 135.54(17) . . . . ? B5 C2 B3 C1 98.36(17) . . . . ? B6 C2 B3 C1 32.19(15) . . . . ? Zr C2 B3 C1 -99.21(14) . . . . ? C1 C2 B3 B4 -135.54(17) . . . . ? B5 C2 B3 B4 -37.18(16) . . . . ? B6 C2 B3 B4 -103.36(18) . . . . ? Zr C2 B3 B4 125.25(15) . . . . ? C1 C2 B3 B8 -97.64(17) . . . . ? B4 C2 B3 B8 37.91(16) . . . . ? B5 C2 B3 B8 0.7(2) . . . . ? B6 C2 B3 B8 -65.4(2) . . . . ? Zr C2 B3 B8 163.16(13) . . . . ? C1 C2 B3 B7 -34.90(15) . . . . ? B4 C2 B3 B7 100.64(18) . . . . ? B5 C2 B3 B7 63.5(2) . . . . ? B6 C2 B3 B7 -2.7(2) . . . . ? Zr C2 B3 B7 -134.11(14) . . . . ? C1 C2 B4 B5 -100.76(17) . . . . ? B6 C2 B4 B5 -37.58(16) . . . . ? B3 C2 B4 B5 -139.98(17) . . . . ? Zr C2 B4 B5 121.82(19) . . . . ? C1 C2 B4 B3 39.22(15) . . . . ? B5 C2 B4 B3 139.98(17) . . . . ? B6 C2 B4 B3 102.39(18) . . . . ? Zr C2 B4 B3 -98.20(18) . . . . ? C1 C2 B4 B9 -62.1(2) . . . . ? B5 C2 B4 B9 38.70(16) . . . . ? B6 C2 B4 B9 1.1(2) . . . . ? B3 C2 B4 B9 -101.27(18) . . . . ? Zr C2 B4 B9 160.53(15) . . . . ? C1 C2 B4 B8 1.2(2) . . . . ? B5 C2 B4 B8 101.98(18) . . . . ? B6 C2 B4 B8 64.4(2) . . . . ? B3 C2 B4 B8 -37.99(16) . . . . ? Zr C2 B4 B8 -136.19(16) . . . . ? C1 B3 B4 C2 -38.75(15) . . . . ? B8 B3 B4 C2 -137.30(17) . . . . ? B7 B3 B4 C2 -99.92(17) . . . . ? C1 B3 B4 B5 -3.1(2) . . . . ? C2 B3 B4 B5 35.67(16) . . . . ? B8 B3 B4 B5 -101.62(19) . . . . ? B7 B3 B4 B5 -64.3(2) . . . . ? C1 B3 B4 B9 61.1(2) . . . . ? C2 B3 B4 B9 99.84(18) . . . . ? B8 B3 B4 B9 -37.46(16) . . . . ? B7 B3 B4 B9 -0.1(2) . . . . ? C1 B3 B4 B8 98.54(17) . . . . ? C2 B3 B4 B8 137.30(17) . . . . ? B7 B3 B4 B8 37.37(16) . . . . ? C1 C2 B5 B4 100.64(17) . . . . ? B6 C2 B5 B4 139.52(17) . . . . ? B3 C2 B5 B4 37.32(16) . . . . ? Zr C2 B5 B4 -121.03(19) . . . . ? C1 C2 B5 B6 -38.88(15) . . . . ? B4 C2 B5 B6 -139.52(17) . . . . ? B3 C2 B5 B6 -102.20(18) . . . . ? Zr C2 B5 B6 99.45(18) . . . . ? C1 C2 B5 B9 62.3(2) . . . . ? B4 C2 B5 B9 -38.38(16) . . . . ? B6 C2 B5 B9 101.14(18) . . . . ? B3 C2 B5 B9 -1.1(2) . . . . ? Zr C2 B5 B9 -159.41(15) . . . . ? C1 C2 B5 B10 -0.9(2) . . . . ? B4 C2 B5 B10 -101.55(19) . . . . ? B6 C2 B5 B10 37.97(16) . . . . ? B3 C2 B5 B10 -64.2(2) . . . . ? Zr C2 B5 B10 137.42(16) . . . . ? B3 B4 B5 C2 -35.74(16) . . . . ? B9 B4 B5 C2 -136.76(18) . . . . ? B8 B4 B5 C2 -99.44(18) . . . . ? C2 B4 B5 B6 36.01(16) . . . . ? B3 B4 B5 B6 0.3(2) . . . . ? B9 B4 B5 B6 -100.75(19) . . . . ? B8 B4 B5 B6 -63.4(2) . . . . ? C2 B4 B5 B9 136.76(18) . . . . ? B3 B4 B5 B9 101.02(19) . . . . ? B8 B4 B5 B9 37.32(17) . . . . ? C2 B4 B5 B10 99.46(18) . . . . ? B3 B4 B5 B10 63.7(2) . . . . ? B9 B4 B5 B10 -37.30(16) . . . . ? B8 B4 B5 B10 0.0(2) . . . . ? C3 C1 B6 C2 -102.55(19) . . . . ? B7 C1 B6 C2 102.74(18) . . . . ? B11 C1 B6 C2 140.13(17) . . . . ? B3 C1 B6 C2 33.40(16) . . . . ? C3 C1 B6 B5 -140.81(18) . . . . ? B7 C1 B6 B5 64.5(2) . . . . ? B11 C1 B6 B5 101.87(18) . . . . ? B3 C1 B6 B5 -4.9(2) . . . . ? C2 C1 B6 B5 -38.26(15) . . . . ? C3 C1 B6 B10 156.26(18) . . . . ? B7 C1 B6 B10 1.6(2) . . . . ? B11 C1 B6 B10 38.94(16) . . . . ? B3 C1 B6 B10 -67.8(2) . . . . ? C2 C1 B6 B10 -101.19(17) . . . . ? C3 C1 B6 B11 117.3(2) . . . . ? B7 C1 B6 B11 -37.39(17) . . . . ? B3 C1 B6 B11 -106.73(18) . . . . ? C2 C1 B6 B11 -140.13(17) . . . . ? B4 C2 B6 C1 -98.44(17) . . . . ? B5 C2 B6 C1 -135.93(17) . . . . ? B3 C2 B6 C1 -32.21(16) . . . . ? Zr C2 B6 C1 98.59(14) . . . . ? C1 C2 B6 B5 135.93(17) . . . . ? B4 C2 B6 B5 37.49(17) . . . . ? B3 C2 B6 B5 103.72(18) . . . . ? Zr C2 B6 B5 -125.48(15) . . . . ? C1 C2 B6 B10 97.79(17) . . . . ? B4 C2 B6 B10 -0.7(2) . . . . ? B5 C2 B6 B10 -38.14(16) . . . . ? B3 C2 B6 B10 65.6(2) . . . . ? Zr C2 B6 B10 -163.62(13) . . . . ? C1 C2 B6 B11 34.96(15) . . . . ? B4 C2 B6 B11 -63.5(2) . . . . ? B5 C2 B6 B11 -100.97(18) . . . . ? B3 C2 B6 B11 2.7(2) . . . . ? Zr C2 B6 B11 133.55(14) . . . . ? C2 B5 B6 C1 38.56(15) . . . . ? B4 B5 B6 C1 2.7(2) . . . . ? B9 B5 B6 C1 -60.9(2) . . . . ? B10 B5 B6 C1 -98.69(18) . . . . ? B4 B5 B6 C2 -35.90(16) . . . . ? B9 B5 B6 C2 -99.44(18) . . . . ? B10 B5 B6 C2 -137.25(17) . . . . ? C2 B5 B6 B10 137.25(17) . . . . ? B4 B5 B6 B10 101.35(19) . . . . ? B9 B5 B6 B10 37.81(16) . . . . ? C2 B5 B6 B11 99.92(17) . . . . ? B4 B5 B6 B11 64.0(2) . . . . ? B9 B5 B6 B11 0.5(2) . . . . ? B10 B5 B6 B11 -37.33(16) . . . . ? C3 C1 B7 B8 143.26(19) . . . . ? B11 C1 B7 B8 -102.25(18) . . . . ? B6 C1 B7 B8 -64.8(2) . . . . ? B3 C1 B7 B8 39.40(16) . . . . ? C2 C1 B7 B8 2.2(2) . . . . ? C3 C1 B7 B12 -153.98(19) . . . . ? B11 C1 B7 B12 -39.49(16) . . . . ? B6 C1 B7 B12 -2.0(2) . . . . ? B3 C1 B7 B12 102.15(18) . . . . ? C2 C1 B7 B12 64.9(2) . . . . ? C3 C1 B7 B11 -114.5(2) . . . . ? B6 C1 B7 B11 37.48(17) . . . . ? B3 C1 B7 B11 141.65(17) . . . . ? C2 C1 B7 B11 104.44(17) . . . . ? C3 C1 B7 B3 103.9(2) . . . . ? B11 C1 B7 B3 -141.65(17) . . . . ? B6 C1 B7 B3 -104.17(18) . . . . ? C2 C1 B7 B3 -37.21(16) . . . . ? C2 B3 B7 C1 35.37(15) . . . . ? B4 B3 B7 C1 97.37(18) . . . . ? B8 B3 B7 C1 134.96(17) . . . . ? C1 B3 B7 B8 -134.96(17) . . . . ? C2 B3 B7 B8 -99.59(18) . . . . ? B4 B3 B7 B8 -37.59(16) . . . . ? C1 B3 B7 B12 -96.87(18) . . . . ? C2 B3 B7 B12 -61.5(2) . . . . ? B4 B3 B7 B12 0.5(2) . . . . ? B8 B3 B7 B12 38.09(16) . . . . ? C1 B3 B7 B11 -33.78(15) . . . . ? C2 B3 B7 B11 1.6(2) . . . . ? B4 B3 B7 B11 63.6(2) . . . . ? B8 B3 B7 B11 101.18(18) . . . . ? C1 B7 B8 B3 -38.79(15) . . . . ? B12 B7 B8 B3 -137.53(17) . . . . ? B11 B7 B8 B3 -100.24(18) . . . . ? C1 B7 B8 B4 -1.3(2) . . . . ? B12 B7 B8 B4 -100.08(18) . . . . ? B11 B7 B8 B4 -62.8(2) . . . . ? B3 B7 B8 B4 37.45(16) . . . . ? C1 B7 B8 B9 61.8(2) . . . . ? B12 B7 B8 B9 -36.92(16) . . . . ? B11 B7 B8 B9 0.4(2) . . . . ? B3 B7 B8 B9 100.61(18) . . . . ? C1 B7 B8 B12 98.74(18) . . . . ? B11 B7 B8 B12 37.29(16) . . . . ? B3 B7 B8 B12 137.53(17) . . . . ? C1 B3 B8 B7 38.58(15) . . . . ? C2 B3 B8 B7 100.68(17) . . . . ? B4 B3 B8 B7 137.97(18) . . . . ? C1 B3 B8 B4 -99.39(17) . . . . ? C2 B3 B8 B4 -37.29(15) . . . . ? B7 B3 B8 B4 -137.97(18) . . . . ? C1 B3 B8 B9 -62.2(2) . . . . ? C2 B3 B8 B9 -0.1(2) . . . . ? B4 B3 B8 B9 37.19(16) . . . . ? B7 B3 B8 B9 -100.78(18) . . . . ? C1 B3 B8 B12 0.7(2) . . . . ? C2 B3 B8 B12 62.8(2) . . . . ? B4 B3 B8 B12 100.12(18) . . . . ? B7 B3 B8 B12 -37.85(16) . . . . ? C2 B4 B8 B7 0.1(2) . . . . ? B5 B4 B8 B7 62.9(2) . . . . ? B3 B4 B8 B7 -37.72(16) . . . . ? B9 B4 B8 B7 100.48(19) . . . . ? C2 B4 B8 B3 37.80(15) . . . . ? B5 B4 B8 B3 100.66(18) . . . . ? B9 B4 B8 B3 138.20(18) . . . . ? C2 B4 B8 B9 -100.40(18) . . . . ? B5 B4 B8 B9 -37.54(17) . . . . ? B3 B4 B8 B9 -138.20(18) . . . . ? C2 B4 B8 B12 -63.1(2) . . . . ? B5 B4 B8 B12 -0.2(2) . . . . ? B3 B4 B8 B12 -100.90(18) . . . . ? B9 B4 B8 B12 37.30(16) . . . . ? C2 B4 B9 B12 62.6(2) . . . . ? B5 B4 B9 B12 100.74(19) . . . . ? B3 B4 B9 B12 -0.4(2) . . . . ? B8 B4 B9 B12 -37.80(16) . . . . ? C2 B4 B9 B8 100.37(18) . . . . ? B5 B4 B9 B8 138.55(18) . . . . ? B3 B4 B9 B8 37.43(16) . . . . ? C2 B4 B9 B5 -38.18(16) . . . . ? B3 B4 B9 B5 -101.11(18) . . . . ? B8 B4 B9 B5 -138.55(18) . . . . ? C2 B4 B9 B10 -1.1(2) . . . . ? B5 B4 B9 B10 37.04(16) . . . . ? B3 B4 B9 B10 -64.1(2) . . . . ? B8 B4 B9 B10 -101.50(18) . . . . ? B7 B8 B9 B12 37.03(16) . . . . ? B3 B8 B9 B12 100.73(18) . . . . ? B4 B8 B9 B12 137.91(18) . . . . ? B7 B8 B9 B4 -100.87(18) . . . . ? B3 B8 B9 B4 -37.17(16) . . . . ? B12 B8 B9 B4 -137.91(18) . . . . ? B7 B8 B9 B5 -64.2(2) . . . . ? B3 B8 B9 B5 -0.5(2) . . . . ? B4 B8 B9 B5 36.64(16) . . . . ? B12 B8 B9 B5 -101.27(19) . . . . ? B7 B8 B9 B10 -0.8(2) . . . . ? B3 B8 B9 B10 62.9(2) . . . . ? B4 B8 B9 B10 100.08(19) . . . . ? B12 B8 B9 B10 -37.82(17) . . . . ? C2 B5 B9 B12 -62.8(2) . . . . ? B4 B5 B9 B12 -100.75(19) . . . . ? B6 B5 B9 B12 0.0(2) . . . . ? B10 B5 B9 B12 37.70(16) . . . . ? C2 B5 B9 B4 37.99(16) . . . . ? B6 B5 B9 B4 100.71(18) . . . . ? B10 B5 B9 B4 138.45(18) . . . . ? C2 B5 B9 B8 1.0(2) . . . . ? B4 B5 B9 B8 -37.02(16) . . . . ? B6 B5 B9 B8 63.7(2) . . . . ? B10 B5 B9 B8 101.43(18) . . . . ? C2 B5 B9 B10 -100.46(18) . . . . ? B4 B5 B9 B10 -138.45(18) . . . . ? B6 B5 B9 B10 -37.75(16) . . . . ? C1 B6 B10 B11 -38.35(15) . . . . ? C2 B6 B10 B11 -100.63(17) . . . . ? B5 B6 B10 B11 -138.12(18) . . . . ? C1 B6 B10 B5 99.76(17) . . . . ? C2 B6 B10 B5 37.48(15) . . . . ? B11 B6 B10 B5 138.12(18) . . . . ? C1 B6 B10 B9 62.2(2) . . . . ? C2 B6 B10 B9 -0.1(2) . . . . ? B5 B6 B10 B9 -37.56(16) . . . . ? B11 B6 B10 B9 100.55(19) . . . . ? C1 B6 B10 B12 -0.4(2) . . . . ? C2 B6 B10 B12 -62.7(2) . . . . ? B5 B6 B10 B12 -100.18(18) . . . . ? B11 B6 B10 B12 37.94(16) . . . . ? C2 B5 B10 B11 -0.1(2) . . . . ? B4 B5 B10 B11 -62.7(2) . . . . ? B6 B5 B10 B11 37.64(16) . . . . ? B9 B5 B10 B11 -100.06(19) . . . . ? C2 B5 B10 B6 -37.78(16) . . . . ? B4 B5 B10 B6 -100.38(18) . . . . ? B9 B5 B10 B6 -137.70(18) . . . . ? C2 B5 B10 B9 99.92(18) . . . . ? B4 B5 B10 B9 37.32(16) . . . . ? B6 B5 B10 B9 137.70(18) . . . . ? C2 B5 B10 B12 62.8(2) . . . . ? B4 B5 B10 B12 0.2(2) . . . . ? B6 B5 B10 B12 100.58(18) . . . . ? B9 B5 B10 B12 -37.12(16) . . . . ? B12 B9 B10 B11 -36.92(16) . . . . ? B4 B9 B10 B11 64.4(2) . . . . ? B8 B9 B10 B11 0.9(2) . . . . ? B5 B9 B10 B11 101.10(18) . . . . ? B12 B9 B10 B6 -100.58(18) . . . . ? B4 B9 B10 B6 0.7(2) . . . . ? B8 B9 B10 B6 -62.8(2) . . . . ? B5 B9 B10 B6 37.44(16) . . . . ? B12 B9 B10 B5 -138.02(18) . . . . ? B4 B9 B10 B5 -36.69(16) . . . . ? B8 B9 B10 B5 -100.19(19) . . . . ? B4 B9 B10 B12 101.33(18) . . . . ? B8 B9 B10 B12 37.83(17) . . . . ? B5 B9 B10 B12 138.02(18) . . . . ? C3 C1 B11 B12 154.66(19) . . . . ? B7 C1 B11 B12 39.59(16) . . . . ? B6 C1 B11 B12 -101.95(18) . . . . ? B3 C1 B11 B12 2.3(2) . . . . ? C2 C1 B11 B12 -64.7(2) . . . . ? C3 C1 B11 B10 -142.41(19) . . . . ? B7 C1 B11 B10 102.52(18) . . . . ? B6 C1 B11 B10 -39.02(16) . . . . ? B3 C1 B11 B10 65.2(2) . . . . ? C2 C1 B11 B10 -1.8(2) . . . . ? C3 C1 B11 B7 115.1(2) . . . . ? B6 C1 B11 B7 -141.54(17) . . . . ? B3 C1 B11 B7 -37.31(17) . . . . ? C2 C1 B11 B7 -104.29(18) . . . . ? C3 C1 B11 B6 -103.4(2) . . . . ? B7 C1 B11 B6 141.54(17) . . . . ? B3 C1 B11 B6 104.23(18) . . . . ? C2 C1 B11 B6 37.25(15) . . . . ? B6 B10 B11 C1 38.38(15) . . . . ? B5 B10 B11 C1 1.1(2) . . . . ? B9 B10 B11 C1 -62.0(2) . . . . ? B12 B10 B11 C1 -98.85(18) . . . . ? B6 B10 B11 B12 137.23(18) . . . . ? B5 B10 B11 B12 99.98(19) . . . . ? B9 B10 B11 B12 36.82(16) . . . . ? B6 B10 B11 B7 99.74(18) . . . . ? B5 B10 B11 B7 62.5(2) . . . . ? B9 B10 B11 B7 -0.7(2) . . . . ? B12 B10 B11 B7 -37.49(16) . . . . ? B5 B10 B11 B6 -37.25(16) . . . . ? B9 B10 B11 B6 -100.41(18) . . . . ? B12 B10 B11 B6 -137.23(18) . . . . ? B8 B7 B11 C1 97.11(18) . . . . ? B12 B7 B11 C1 134.66(17) . . . . ? B3 B7 B11 C1 33.79(15) . . . . ? C1 B7 B11 B12 -134.66(17) . . . . ? B8 B7 B11 B12 -37.55(16) . . . . ? B3 B7 B11 B12 -100.87(19) . . . . ? C1 B7 B11 B10 -96.92(18) . . . . ? B8 B7 B11 B10 0.2(2) . . . . ? B12 B7 B11 B10 37.75(16) . . . . ? B3 B7 B11 B10 -63.1(2) . . . . ? C1 B7 B11 B6 -33.74(15) . . . . ? B8 B7 B11 B6 63.4(2) . . . . ? B12 B7 B11 B6 100.92(18) . . . . ? B3 B7 B11 B6 0.0(2) . . . . ? C2 B6 B11 C1 -35.44(15) . . . . ? B5 B6 B11 C1 -97.70(18) . . . . ? B10 B6 B11 C1 -135.35(18) . . . . ? C1 B6 B11 B12 96.97(18) . . . . ? C2 B6 B11 B12 61.5(2) . . . . ? B5 B6 B11 B12 -0.7(2) . . . . ? B10 B6 B11 B12 -38.38(16) . . . . ? C1 B6 B11 B10 135.35(18) . . . . ? C2 B6 B11 B10 99.91(18) . . . . ? B5 B6 B11 B10 37.65(16) . . . . ? C1 B6 B11 B7 33.76(15) . . . . ? C2 B6 B11 B7 -1.7(2) . . . . ? B5 B6 B11 B7 -63.9(2) . . . . ? B10 B6 B11 B7 -101.59(18) . . . . ? B4 B9 B12 B11 -63.1(2) . . . . ? B8 B9 B12 B11 -100.77(19) . . . . ? B5 B9 B12 B11 -0.4(2) . . . . ? B10 B9 B12 B11 37.16(16) . . . . ? B4 B9 B12 B7 0.7(2) . . . . ? B8 B9 B12 B7 -37.03(16) . . . . ? B5 B9 B12 B7 63.3(2) . . . . ? B10 B9 B12 B7 100.90(18) . . . . ? B4 B9 B12 B8 37.70(17) . . . . ? B5 B9 B12 B8 100.36(19) . . . . ? B10 B9 B12 B8 137.93(18) . . . . ? B4 B9 B12 B10 -100.23(19) . . . . ? B8 B9 B12 B10 -137.93(18) . . . . ? B5 B9 B12 B10 -37.57(16) . . . . ? C1 B11 B12 B9 61.9(2) . . . . ? B10 B11 B12 B9 -37.36(16) . . . . ? B7 B11 B12 B9 100.78(19) . . . . ? B6 B11 B12 B9 0.7(2) . . . . ? C1 B11 B12 B7 -38.91(15) . . . . ? B10 B11 B12 B7 -138.14(18) . . . . ? B6 B11 B12 B7 -100.08(18) . . . . ? C1 B11 B12 B8 -1.7(2) . . . . ? B10 B11 B12 B8 -100.90(19) . . . . ? B7 B11 B12 B8 37.24(16) . . . . ? B6 B11 B12 B8 -62.8(2) . . . . ? C1 B11 B12 B10 99.23(17) . . . . ? B7 B11 B12 B10 138.14(18) . . . . ? B6 B11 B12 B10 38.06(16) . . . . ? C1 B7 B12 B9 -62.1(2) . . . . ? B8 B7 B12 B9 37.17(16) . . . . ? B11 B7 B12 B9 -101.05(19) . . . . ? B3 B7 B12 B9 -0.7(2) . . . . ? C1 B7 B12 B11 38.95(15) . . . . ? B8 B7 B12 B11 138.22(18) . . . . ? B3 B7 B12 B11 100.32(18) . . . . ? C1 B7 B12 B8 -99.26(18) . . . . ? B11 B7 B12 B8 -138.22(18) . . . . ? B3 B7 B12 B8 -37.89(16) . . . . ? C1 B7 B12 B10 1.6(2) . . . . ? B8 B7 B12 B10 100.88(19) . . . . ? B11 B7 B12 B10 -37.34(16) . . . . ? B3 B7 B12 B10 63.0(2) . . . . ? B7 B8 B12 B9 -138.46(18) . . . . ? B3 B8 B12 B9 -100.40(18) . . . . ? B4 B8 B12 B9 -37.38(16) . . . . ? B7 B8 B12 B11 -37.47(16) . . . . ? B3 B8 B12 B11 0.6(2) . . . . ? B4 B8 B12 B11 63.6(2) . . . . ? B9 B8 B12 B11 100.99(19) . . . . ? B3 B8 B12 B7 38.06(16) . . . . ? B4 B8 B12 B7 101.08(18) . . . . ? B9 B8 B12 B7 138.46(18) . . . . ? B7 B8 B12 B10 -100.72(18) . . . . ? B3 B8 B12 B10 -62.7(2) . . . . ? B4 B8 B12 B10 0.4(2) . . . . ? B9 B8 B12 B10 37.74(17) . . . . ? B11 B10 B12 B9 138.38(18) . . . . ? B6 B10 B12 B9 100.08(18) . . . . ? B5 B10 B12 B9 37.31(16) . . . . ? B6 B10 B12 B11 -38.30(16) . . . . ? B5 B10 B12 B11 -101.08(18) . . . . ? B9 B10 B12 B11 -138.38(18) . . . . ? B11 B10 B12 B7 37.54(16) . . . . ? B6 B10 B12 B7 -0.8(2) . . . . ? B5 B10 B12 B7 -63.5(2) . . . . ? B9 B10 B12 B7 -100.84(19) . . . . ? B11 B10 B12 B8 100.73(19) . . . . ? B6 B10 B12 B8 62.4(2) . . . . ? B5 B10 B12 B8 -0.3(2) . . . . ? B9 B10 B12 B8 -37.65(17) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 76.18 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.435 _refine_diff_density_min -0.784 _refine_diff_density_rms 0.094 #============================================================================= # end of cif data for "magd52" #============================================================================= #============================================================================= # end of cif file #============================================================================= _database_code_depnum_ccdc_archive 'CCDC 963132'