# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name 'John D. Kennedy' 'Neil J. Bullen' 'Andreas Franken' 'Colin A. Kilner' _publ_contact_author_name 'Prof John D Kennedy' _publ_contact_author_address ; Department of Chemistry University of Leeds Leeds LS2 9JT Leeds W Yorkshire LS2 9JT UNITED KINGDOM ; _publ_contact_author_email JOHNK@CHEM.LEEDS.AC.UK _publ_section_title ; Polyhedral monocarbaborane chemistry. Routes to neutral, monoanionic and dianionic carbo-carbaborane-rods. ; data_afx53b _database_code_CSD 184236 _publ_section_title ; Polyhedral monocarbaborane chemistry. Routes to neutral, monoanionic and dianionic carbo-carbaborane-rods. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H48 B11 N' _chemical_formula_weight 529.59 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 24.8134(2) _cell_length_b 14.0073(2) _cell_length_c 19.492 _cell_angle_alpha 90.00 _cell_angle_beta 107.1260(5) _cell_angle_gamma 90.00 _cell_volume 6474.44(11) _cell_formula_units_Z 8 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.087 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 0.056 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9828 _exptl_absorpt_correction_T_max 0.9916 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 15 degree phi range. ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63091 _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12649 _reflns_number_gt 9593 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3 for Windows (Farrugia, 1997) XSeed (Barbour, 2001) ; _computing_publication_material 'WC (Thornton-Pett, 2000)' _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^)+(0.1341P)^2^+6.6312P] 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 SHELXL _refine_ls_extinction_coef 0.0060(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12649 _refine_ls_number_parameters 752 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1164 _refine_ls_R_factor_gt 0.0936 _refine_ls_wR_factor_ref 0.2749 _refine_ls_wR_factor_gt 0.2537 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.010 _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 C1 C 0.17974(11) 0.22509(18) 0.51935(14) 0.0323(6) Uani 1 1 d . . . C13 C 0.21915(11) 0.20506(19) 0.59332(15) 0.0351(6) Uani 1 1 d . . . C14 C 0.26985(12) 0.1560(2) 0.60190(15) 0.0397(6) Uani 1 1 d . . . H14 H 0.2809 0.1395 0.5607 0.048 Uiso 1 1 calc R . . C15 C 0.30432(13) 0.1309(2) 0.66939(16) 0.0417(7) Uani 1 1 d . . . H15 H 0.3384 0.0975 0.6735 0.050 Uiso 1 1 calc R . . C16 C 0.28981(12) 0.1538(2) 0.73117(15) 0.0399(6) Uani 1 1 d . . . C17 C 0.23972(13) 0.2043(2) 0.72289(16) 0.0412(7) Uani 1 1 d . . . H17 H 0.2293 0.2222 0.7643 0.049 Uiso 1 1 calc R . . C18 C 0.20472(12) 0.2292(2) 0.65508(15) 0.0378(6) Uani 1 1 d . . . H18 H 0.1707 0.2629 0.6509 0.045 Uiso 1 1 calc R . . C19 C 0.32769(15) 0.1229(2) 0.80275(17) 0.0502(8) Uani 1 1 d . . . C20 C 0.38586(18) 0.1103(3) 0.8163(2) 0.0734(11) Uani 1 1 d . . . H20 H 0.4022 0.1207 0.7786 0.088 Uiso 1 1 calc R . . C21 C 0.4203(2) 0.0831(4) 0.8834(2) 0.0836(13) Uani 1 1 d . . . H21 H 0.4598 0.0756 0.8915 0.100 Uiso 1 1 calc R . . C22 C 0.39643(19) 0.0672(3) 0.9381(2) 0.0670(10) Uani 1 1 d . . . C23 C 0.3413(2) 0.0799(4) 0.9270(2) 0.0878(14) Uani 1 1 d . . . H23 H 0.3255 0.0700 0.9653 0.105 Uiso 1 1 calc R . . C24 C 0.30690(18) 0.1074(4) 0.8603(2) 0.0785(13) Uani 1 1 d . . . H24 H 0.2677 0.1159 0.8538 0.094 Uiso 1 1 calc R . . C25 C 0.4348(2) 0.0381(4) 1.0126(2) 0.0921(15) Uani 1 1 d . . . H25A H 0.4182 0.0603 1.0496 0.138 Uiso 1 1 calc R . . H25B H 0.4721 0.0670 1.0206 0.138 Uiso 1 1 calc R . . H25C H 0.4385 -0.0316 1.0151 0.138 Uiso 1 1 calc R . . C26 C 0.05041(12) 0.27281(18) 0.27914(15) 0.0354(6) Uani 1 1 d . . . C27 C -0.00288(12) 0.31406(19) 0.27006(16) 0.0388(6) Uani 1 1 d . . . H27 H -0.0140 0.3298 0.3113 0.047 Uiso 1 1 calc R . . C28 C -0.03984(13) 0.3325(2) 0.20229(17) 0.0449(7) Uani 1 1 d . . . H28 H -0.0754 0.3608 0.1982 0.054 Uiso 1 1 calc R . . C29 C -0.02550(14) 0.3103(2) 0.14110(17) 0.0473(7) Uani 1 1 d . . . C30 C 0.02654(15) 0.2697(2) 0.14809(16) 0.0487(8) Uani 1 1 d . . . H30 H 0.0371 0.2540 0.1064 0.058 Uiso 1 1 calc R . . C31 C 0.06416(13) 0.2513(2) 0.21658(15) 0.0414(7) Uani 1 1 d . . . H31 H 0.0998 0.2236 0.2202 0.050 Uiso 1 1 calc R . . C32 C -0.06783(17) 0.3327(3) 0.06816(19) 0.0633(10) Uani 1 1 d . . . H32A H -0.0539 0.3070 0.0298 0.095 Uiso 1 1 calc R . . H32B H -0.0725 0.4020 0.0625 0.095 Uiso 1 1 calc R . . H32C H -0.1042 0.3034 0.0655 0.095 Uiso 1 1 calc R . . C33 C 0.31781(12) 0.8112(2) 0.50322(16) 0.0388(6) Uani 1 1 d . . . C45 C 0.28092(13) 0.8311(2) 0.42832(16) 0.0403(6) Uani 1 1 d . . . C46 C 0.29395(13) 0.7957(2) 0.36830(16) 0.0431(7) Uani 1 1 d . . . H46 H 0.3268 0.7576 0.3747 0.052 Uiso 1 1 calc R . . C47 C 0.25995(13) 0.8150(2) 0.29937(16) 0.0446(7) Uani 1 1 d . . . H47 H 0.2697 0.7890 0.2596 0.054 Uiso 1 1 calc R . . C48 C 0.21159(14) 0.8717(2) 0.28685(17) 0.0455(7) Uani 1 1 d . . . C49 C 0.19819(15) 0.9068(2) 0.34781(18) 0.0518(8) Uani 1 1 d . . . H49 H 0.1654 0.9448 0.3415 0.062 Uiso 1 1 calc R . . C50 C 0.23204(14) 0.8869(2) 0.41655(17) 0.0497(8) Uani 1 1 d . . . H50 H 0.2220 0.9114 0.4565 0.060 Uiso 1 1 calc R . . C51 C 0.17420(15) 0.8885(2) 0.21283(18) 0.0517(8) Uani 1 1 d . . . C52 C 0.17876(16) 0.8328(3) 0.15518(19) 0.0577(9) Uani 1 1 d . . . H52 H 0.2075 0.7858 0.1627 0.069 Uiso 1 1 calc R . . C53 C 0.14152(17) 0.8457(3) 0.0872(2) 0.0624(10) Uani 1 1 d . . . H53 H 0.1458 0.8072 0.0490 0.075 Uiso 1 1 calc R . . C54 C 0.09880(17) 0.9118(3) 0.07266(19) 0.0630(10) Uani 1 1 d . . . C55 C 0.09523(18) 0.9703(3) 0.1293(2) 0.0661(10) Uani 1 1 d . . . H55 H 0.0671 1.0186 0.1208 0.079 Uiso 1 1 calc R . . C56 C 0.13214(17) 0.9588(3) 0.1979(2) 0.0624(9) Uani 1 1 d . . . H56 H 0.1288 0.9994 0.2354 0.075 Uiso 1 1 calc R . . C57 C 0.05819(19) 0.9204(3) -0.0001(2) 0.0756(12) Uani 1 1 d . . . H57A H 0.0743 0.8911 -0.0353 0.113 Uiso 1 1 calc R . . H57B H 0.0505 0.9881 -0.0119 0.113 Uiso 1 1 calc R . . H57C H 0.0230 0.8879 -0.0013 0.113 Uiso 1 1 calc R . . C58 C 0.43881(14) 0.7529(2) 0.74628(18) 0.0509(8) Uani 1 1 d . . . C59 C 0.42798(16) 0.7857(3) 0.80728(19) 0.0626(10) Uani 1 1 d . . . H59 H 0.3941 0.8199 0.8033 0.075 Uiso 1 1 calc R . . C60 C 0.46653(19) 0.7696(3) 0.8762(2) 0.0734(12) Uani 1 1 d . . . H60 H 0.4583 0.7930 0.9178 0.088 Uiso 1 1 calc R . . C61 C 0.51658(17) 0.7192(3) 0.8831(2) 0.0672(11) Uani 1 1 d . . . C62 C 0.52661(16) 0.6850(3) 0.8240(2) 0.0669(11) Uani 1 1 d . . . H62 H 0.5601 0.6495 0.8284 0.080 Uiso 1 1 calc R . . C63 C 0.48909(14) 0.7002(3) 0.7563(2) 0.0569(9) Uani 1 1 d . . . H63 H 0.4975 0.6745 0.7155 0.068 Uiso 1 1 calc R . . C64 C 0.5594(2) 0.7022(4) 0.9560(2) 0.0873(14) Uani 1 1 d . . . H64A H 0.5731 0.6363 0.9587 0.131 Uiso 1 1 calc R . . H64B H 0.5414 0.7130 0.9939 0.131 Uiso 1 1 calc R . . H64C H 0.5911 0.7463 0.9624 0.131 Uiso 1 1 calc R . . C65 C 0.07089(12) 0.61636(19) 0.15292(14) 0.0347(6) Uani 1 1 d . . . H65A H 0.0412 0.6515 0.1671 0.042 Uiso 1 1 calc R . . H65B H 0.0934 0.6639 0.1357 0.042 Uiso 1 1 calc R . . C66 C 0.04272(13) 0.5498(2) 0.09129(15) 0.0433(7) Uani 1 1 d . . . H66A H 0.0714 0.5213 0.0722 0.065 Uiso 1 1 calc R . . H66B H 0.0158 0.5860 0.0533 0.065 Uiso 1 1 calc R . . H66C H 0.0227 0.4993 0.1086 0.065 Uiso 1 1 calc R . . C67 C 0.15097(11) 0.50085(19) 0.19900(16) 0.0370(6) Uani 1 1 d . . . H67A H 0.1750 0.4707 0.2434 0.044 Uiso 1 1 calc R . . H67B H 0.1296 0.4493 0.1679 0.044 Uiso 1 1 calc R . . C68 C 0.18855(13) 0.5485(2) 0.16093(19) 0.0496(8) Uani 1 1 d . . . H68A H 0.1653 0.5804 0.1176 0.074 Uiso 1 1 calc R . . H68B H 0.2123 0.5003 0.1476 0.074 Uiso 1 1 calc R . . H68C H 0.2125 0.5956 0.1929 0.074 Uiso 1 1 calc R . . C69 C 0.13941(12) 0.64504(19) 0.26986(16) 0.0386(6) Uani 1 1 d . . . H69A H 0.1626 0.6823 0.2458 0.046 Uiso 1 1 calc R . . H69B H 0.1108 0.6888 0.2785 0.046 Uiso 1 1 calc R . . C70 C 0.17705(14) 0.6114(2) 0.34152(18) 0.0512(8) Uani 1 1 d . . . H70A H 0.1550 0.5728 0.3655 0.077 Uiso 1 1 calc R . . H70B H 0.1927 0.6668 0.3715 0.077 Uiso 1 1 calc R . . H70C H 0.2079 0.5729 0.3342 0.077 Uiso 1 1 calc R . . C71 C 0.07443(11) 0.50473(18) 0.25425(14) 0.0328(6) Uani 1 1 d . . . H71A H 0.0542 0.4563 0.2190 0.039 Uiso 1 1 calc R . . H71B H 0.1006 0.4702 0.2949 0.039 Uiso 1 1 calc R . . C72 C 0.03181(12) 0.5571(2) 0.28186(16) 0.0387(6) Uani 1 1 d . . . H72A H 0.0510 0.6064 0.3160 0.058 Uiso 1 1 calc R . . H72B H 0.0132 0.5119 0.3059 0.058 Uiso 1 1 calc R . . H72C H 0.0035 0.5870 0.2416 0.058 Uiso 1 1 calc R . . C73 C 0.41384(13) 0.5219(2) 0.84094(16) 0.0426(7) Uani 1 1 d . . . H73A H 0.4309 0.5666 0.8139 0.051 Uiso 1 1 calc R . . H73B H 0.3854 0.5580 0.8570 0.051 Uiso 1 1 calc R . . C74 C 0.45921(14) 0.4880(3) 0.90616(18) 0.0554(8) Uani 1 1 d . . . H74A H 0.4888 0.4555 0.8911 0.083 Uiso 1 1 calc R . . H74B H 0.4429 0.4435 0.9334 0.083 Uiso 1 1 calc R . . H74C H 0.4754 0.5428 0.9364 0.083 Uiso 1 1 calc R . . C75 C 0.42498(16) 0.3868(2) 0.76165(17) 0.0526(8) Uani 1 1 d . . . H75A H 0.4524 0.3547 0.8025 0.063 Uiso 1 1 calc R . . H75B H 0.4038 0.3364 0.7292 0.063 Uiso 1 1 calc R . . C76 C 0.45728(16) 0.4450(3) 0.72152(18) 0.0547(9) Uani 1 1 d . . . H76A H 0.4786 0.4953 0.7530 0.082 Uiso 1 1 calc R . . H76B H 0.4308 0.4740 0.6791 0.082 Uiso 1 1 calc R . . H76C H 0.4834 0.4034 0.7064 0.082 Uiso 1 1 calc R . . C77 C 0.35547(16) 0.3733(2) 0.82824(18) 0.0549(8) Uani 1 1 d . . . H77A H 0.3352 0.3250 0.7930 0.066 Uiso 1 1 calc R . . H77B H 0.3851 0.3395 0.8657 0.066 Uiso 1 1 calc R . . C78 C 0.31431(17) 0.4167(3) 0.8630(2) 0.0677(10) Uani 1 1 d . . . H78A H 0.2820 0.4429 0.8258 0.101 Uiso 1 1 calc R . . H78B H 0.3330 0.4679 0.8956 0.101 Uiso 1 1 calc R . . H78C H 0.3012 0.3675 0.8901 0.101 Uiso 1 1 calc R . . C79 C 0.34010(14) 0.4946(2) 0.72947(17) 0.0494(8) Uani 1 1 d . . . H79A H 0.3131 0.5276 0.7500 0.059 Uiso 1 1 calc R . . H79B H 0.3597 0.5440 0.7095 0.059 Uiso 1 1 calc R . . C80 C 0.3072(2) 0.4312(3) 0.6688(2) 0.0766(13) Uani 1 1 d . . . H80A H 0.2852 0.3850 0.6871 0.115 Uiso 1 1 calc R . . H80B H 0.3335 0.3971 0.6485 0.115 Uiso 1 1 calc R . . H80C H 0.2817 0.4704 0.6315 0.115 Uiso 1 1 calc R . . B2 B 0.12142(13) 0.2970(2) 0.50876(17) 0.0340(6) Uani 1 1 d . . . H2 H 0.1109 0.3345 0.5540 0.041 Uiso 1 1 calc R . . B3 B 0.17897(13) 0.3348(2) 0.47843(17) 0.0360(7) Uani 1 1 d . . . H3 H 0.2063 0.3967 0.5035 0.043 Uiso 1 1 calc R . . B4 B 0.20680(13) 0.2316(2) 0.44746(17) 0.0370(7) Uani 1 1 d . . . H4 H 0.2528 0.2258 0.4522 0.044 Uiso 1 1 calc R . . B5 B 0.16738(14) 0.1307(2) 0.45966(17) 0.0360(7) Uani 1 1 d . . . H5 H 0.1872 0.0586 0.4726 0.043 Uiso 1 1 calc R . . B6 B 0.11447(13) 0.1712(2) 0.49729(17) 0.0353(7) Uani 1 1 d . . . H6 H 0.0994 0.1255 0.5351 0.042 Uiso 1 1 calc R . . B7 B 0.06841(13) 0.2484(2) 0.43508(17) 0.0351(7) Uani 1 1 d . . . H7 H 0.0226 0.2540 0.4311 0.042 Uiso 1 1 calc R . . B8 B 0.10827(13) 0.3493(2) 0.42262(17) 0.0343(6) Uani 1 1 d . . . H8 H 0.0886 0.4217 0.4101 0.041 Uiso 1 1 calc R . . B9 B 0.16138(13) 0.3089(2) 0.38507(17) 0.0353(7) Uani 1 1 d . . . H9 H 0.1769 0.3548 0.3478 0.042 Uiso 1 1 calc R . . B10 B 0.15475(14) 0.1831(2) 0.37367(17) 0.0367(7) Uani 1 1 d . . . H10 H 0.1660 0.1457 0.3290 0.044 Uiso 1 1 calc R . . B11 B 0.09710(14) 0.1447(2) 0.40443(17) 0.0363(7) Uani 1 1 d . . . H11 H 0.0702 0.0820 0.3802 0.044 Uiso 1 1 calc R . . B12 B 0.09278(13) 0.2556(2) 0.35706(16) 0.0330(6) Uani 1 1 d . . . B34 B 0.33149(16) 0.9046(2) 0.56304(19) 0.0465(8) Uani 1 1 d . . . H34 H 0.3146 0.9786 0.5494 0.056 Uiso 1 1 calc R . . B35 B 0.28751(15) 0.8093(3) 0.57193(19) 0.0447(8) Uani 1 1 d . . . H35 H 0.2414 0.8204 0.5644 0.054 Uiso 1 1 calc R . . B36 B 0.31272(16) 0.7032(3) 0.5427(2) 0.0460(8) Uani 1 1 d . . . H36 H 0.2835 0.6444 0.5158 0.055 Uiso 1 1 calc R . . B37 B 0.37334(17) 0.7328(3) 0.5169(2) 0.0498(9) Uani 1 1 d . . . H37 H 0.3842 0.6931 0.4729 0.060 Uiso 1 1 calc R . . B38 B 0.38501(15) 0.8575(3) 0.5288(2) 0.0488(9) Uani 1 1 d . . . H38 H 0.4036 0.9001 0.4927 0.059 Uiso 1 1 calc R . . B39 B 0.39993(17) 0.8834(3) 0.6221(2) 0.0521(9) Uani 1 1 d . . . H39 H 0.4285 0.9433 0.6483 0.063 Uiso 1 1 calc R . . B40 B 0.33952(16) 0.8530(3) 0.64838(19) 0.0468(8) Uani 1 1 d . . . H40 H 0.3282 0.8928 0.6920 0.056 Uiso 1 1 calc R . . B41 B 0.32802(15) 0.7280(3) 0.63589(19) 0.0444(8) Uani 1 1 d . . . H41 H 0.3091 0.6850 0.6714 0.053 Uiso 1 1 calc R . . B42 B 0.38123(16) 0.6811(3) 0.6017(2) 0.0473(8) Uani 1 1 d . . . H42 H 0.3976 0.6067 0.6144 0.057 Uiso 1 1 calc R . . B43 B 0.42567(16) 0.7763(3) 0.5929(2) 0.0530(9) Uani 1 1 d . . . H43 H 0.4717 0.7655 0.5998 0.064 Uiso 1 1 calc R . . B44 B 0.39852(15) 0.7727(3) 0.66789(19) 0.0437(8) Uani 1 1 d . . . N1 N 0.38390(10) 0.44285(16) 0.79039(12) 0.0387(5) Uani 1 1 d . . . N2 N 0.10908(9) 0.56701(15) 0.21894(12) 0.0326(5) 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 C1 0.0328(13) 0.0277(13) 0.0381(14) -0.0007(10) 0.0130(11) -0.0001(10) C13 0.0357(14) 0.0300(13) 0.0393(14) 0.0000(11) 0.0105(11) -0.0021(11) C14 0.0392(15) 0.0386(15) 0.0400(15) 0.0007(12) 0.0098(12) 0.0031(12) C15 0.0395(15) 0.0383(15) 0.0444(16) 0.0003(12) 0.0078(13) 0.0011(12) C16 0.0411(15) 0.0347(14) 0.0400(15) 0.0033(12) 0.0060(12) -0.0086(12) C17 0.0456(16) 0.0407(16) 0.0388(15) -0.0012(12) 0.0148(13) -0.0094(13) C18 0.0353(14) 0.0376(15) 0.0402(15) -0.0029(12) 0.0108(12) -0.0041(12) C19 0.0569(19) 0.0464(18) 0.0484(18) 0.0003(14) 0.0171(15) -0.0053(15) C20 0.072(3) 0.090(3) 0.058(2) 0.017(2) 0.019(2) 0.014(2) C21 0.075(3) 0.098(3) 0.069(3) 0.020(2) 0.008(2) 0.019(3) C22 0.083(3) 0.061(2) 0.057(2) 0.0015(18) 0.020(2) -0.014(2) C23 0.083(3) 0.120(4) 0.054(2) -0.001(2) 0.010(2) -0.003(3) C24 0.062(2) 0.117(4) 0.055(2) 0.004(2) 0.0140(19) 0.001(2) C25 0.107(4) 0.098(4) 0.061(3) 0.018(2) 0.009(2) -0.007(3) C26 0.0381(14) 0.0251(12) 0.0417(15) 0.0024(11) 0.0100(12) -0.0060(11) C27 0.0384(14) 0.0297(13) 0.0455(16) 0.0037(11) 0.0077(12) -0.0067(11) C28 0.0411(16) 0.0317(14) 0.0545(18) 0.0079(13) 0.0027(14) -0.0051(12) C29 0.0510(18) 0.0356(15) 0.0472(17) 0.0061(13) 0.0019(14) -0.0099(13) C30 0.071(2) 0.0377(16) 0.0375(16) -0.0020(12) 0.0170(15) -0.0155(15) C31 0.0502(17) 0.0326(14) 0.0412(16) 0.0001(12) 0.0132(13) -0.0088(12) C32 0.067(2) 0.066(2) 0.053(2) 0.0012(17) 0.0111(17) -0.0047(19) C33 0.0417(15) 0.0336(14) 0.0436(15) -0.0033(12) 0.0162(12) 0.0017(12) C45 0.0442(16) 0.0330(14) 0.0429(15) -0.0032(12) 0.0119(13) -0.0017(12) C46 0.0446(16) 0.0429(16) 0.0470(17) -0.0021(13) 0.0213(14) -0.0034(13) C47 0.0481(17) 0.0465(17) 0.0444(16) -0.0032(13) 0.0218(14) -0.0084(14) C48 0.0525(18) 0.0357(15) 0.0453(16) -0.0013(12) 0.0098(14) -0.0092(13) C49 0.0537(19) 0.0451(17) 0.0517(18) -0.0065(14) 0.0078(15) 0.0079(15) C50 0.0538(18) 0.0462(17) 0.0464(17) -0.0092(14) 0.0108(14) 0.0085(14) C51 0.0569(19) 0.0456(17) 0.0534(19) -0.0011(15) 0.0174(16) -0.0081(15) C52 0.063(2) 0.055(2) 0.055(2) -0.0037(16) 0.0160(17) -0.0109(17) C53 0.071(2) 0.060(2) 0.053(2) -0.0045(17) 0.0139(18) -0.0170(19) C54 0.069(2) 0.068(2) 0.052(2) 0.0113(18) 0.0173(18) -0.021(2) C55 0.071(2) 0.063(2) 0.064(2) 0.0200(19) 0.0178(19) 0.0029(19) C56 0.075(2) 0.054(2) 0.058(2) 0.0080(17) 0.0196(19) 0.0034(18) C57 0.080(3) 0.076(3) 0.064(2) 0.016(2) 0.011(2) -0.007(2) C58 0.0455(17) 0.0540(19) 0.0511(18) 0.0133(15) 0.0113(15) -0.0136(15) C59 0.0498(19) 0.085(3) 0.051(2) 0.0074(18) 0.0106(16) -0.0189(19) C60 0.079(3) 0.092(3) 0.049(2) 0.005(2) 0.0198(19) -0.032(2) C61 0.054(2) 0.066(2) 0.070(3) 0.020(2) 0.0011(19) -0.0198(19) C62 0.053(2) 0.065(2) 0.074(3) 0.024(2) 0.0044(19) -0.0116(18) C63 0.0467(18) 0.0522(19) 0.065(2) 0.0187(16) 0.0055(16) -0.0102(15) C64 0.086(3) 0.094(3) 0.070(3) 0.010(2) 0.004(2) -0.011(3) C65 0.0395(14) 0.0293(13) 0.0368(14) 0.0054(11) 0.0138(12) 0.0049(11) C66 0.0472(16) 0.0421(16) 0.0388(15) -0.0012(12) 0.0100(13) 0.0118(13) C67 0.0353(14) 0.0301(13) 0.0482(16) 0.0020(12) 0.0161(12) 0.0058(11) C68 0.0448(17) 0.0431(17) 0.070(2) 0.0043(15) 0.0308(16) 0.0048(13) C69 0.0395(15) 0.0284(13) 0.0484(16) -0.0031(12) 0.0136(13) -0.0041(11) C70 0.0475(17) 0.0468(18) 0.0527(18) -0.0049(14) 0.0047(14) -0.0051(14) C71 0.0356(13) 0.0246(12) 0.0394(14) 0.0035(10) 0.0132(11) 0.0000(10) C72 0.0421(15) 0.0328(14) 0.0445(15) 0.0038(12) 0.0177(13) 0.0036(12) C73 0.0462(16) 0.0371(15) 0.0457(16) -0.0079(12) 0.0157(13) -0.0062(13) C74 0.0498(18) 0.064(2) 0.0495(18) -0.0134(16) 0.0096(15) -0.0013(16) C75 0.071(2) 0.0389(16) 0.0461(17) -0.0045(13) 0.0147(16) 0.0129(15) C76 0.068(2) 0.0528(19) 0.0485(18) 0.0038(15) 0.0256(16) 0.0224(17) C77 0.069(2) 0.0392(17) 0.0514(18) 0.0020(14) 0.0103(16) -0.0147(16) C78 0.065(2) 0.068(2) 0.078(3) 0.004(2) 0.034(2) -0.0200(19) C79 0.0505(18) 0.0436(17) 0.0502(18) 0.0054(14) 0.0085(14) 0.0002(14) C80 0.088(3) 0.067(2) 0.053(2) 0.0037(18) -0.014(2) -0.021(2) B2 0.0364(16) 0.0268(14) 0.0402(16) -0.0015(12) 0.0135(13) 0.0016(12) B3 0.0368(16) 0.0307(15) 0.0395(16) 0.0000(12) 0.0099(13) -0.0036(12) B4 0.0341(15) 0.0414(17) 0.0371(16) 0.0010(13) 0.0128(13) 0.0017(13) B5 0.0417(17) 0.0288(15) 0.0371(16) -0.0031(12) 0.0108(13) 0.0059(13) B6 0.0366(16) 0.0294(15) 0.0406(16) 0.0001(12) 0.0126(13) -0.0021(12) B7 0.0326(15) 0.0333(15) 0.0402(16) 0.0014(12) 0.0120(13) -0.0003(12) B8 0.0367(15) 0.0262(14) 0.0401(16) 0.0019(12) 0.0117(13) 0.0009(12) B9 0.0331(15) 0.0351(16) 0.0385(16) 0.0024(13) 0.0115(13) -0.0012(12) B10 0.0405(17) 0.0324(15) 0.0379(16) -0.0006(12) 0.0125(13) 0.0050(13) B11 0.0414(17) 0.0278(14) 0.0384(16) 0.0006(12) 0.0098(13) -0.0029(12) B12 0.0349(15) 0.0277(14) 0.0376(16) 0.0000(12) 0.0125(13) -0.0017(12) B34 0.054(2) 0.0332(17) 0.0472(19) -0.0045(14) 0.0077(16) 0.0026(15) B35 0.0378(17) 0.050(2) 0.0472(19) -0.0022(15) 0.0134(15) 0.0040(15) B36 0.054(2) 0.0371(17) 0.0480(19) -0.0014(15) 0.0166(16) -0.0014(15) B37 0.057(2) 0.050(2) 0.049(2) 0.0097(16) 0.0246(17) 0.0180(17) B38 0.0417(18) 0.053(2) 0.053(2) 0.0134(17) 0.0154(16) -0.0008(16) B39 0.049(2) 0.049(2) 0.053(2) 0.0101(17) 0.0059(17) -0.0109(16) B40 0.0478(19) 0.048(2) 0.0443(19) -0.0042(15) 0.0132(15) 0.0071(16) B41 0.0389(17) 0.051(2) 0.0469(19) 0.0013(15) 0.0178(15) -0.0023(15) B42 0.055(2) 0.0419(18) 0.051(2) 0.0084(15) 0.0233(17) 0.0080(16) B43 0.0394(18) 0.066(2) 0.057(2) 0.0204(19) 0.0205(17) 0.0078(17) B44 0.0397(17) 0.0441(18) 0.0490(19) 0.0066(15) 0.0154(15) -0.0030(15) N1 0.0475(14) 0.0288(11) 0.0378(12) -0.0025(9) 0.0095(10) -0.0026(10) N2 0.0328(11) 0.0251(11) 0.0407(12) 0.0019(9) 0.0120(10) 0.0016(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 C1 C13 1.511(4) . ? C1 B6 1.723(4) . ? C1 B2 1.725(4) . ? C1 B4 1.725(4) . ? C1 B5 1.728(4) . ? C1 B3 1.729(4) . ? C13 C18 1.395(4) . ? C13 C14 1.400(4) . ? C14 C15 1.387(4) . ? C15 C16 1.392(4) . ? C16 C17 1.398(4) . ? C16 C19 1.498(4) . ? C17 C18 1.395(4) . ? C19 C24 1.383(5) . ? C19 C20 1.400(5) . ? C20 C21 1.387(5) . ? C21 C22 1.383(6) . ? C22 C23 1.332(6) . ? C22 C25 1.538(6) . ? C23 C24 1.384(6) . ? C26 C31 1.393(4) . ? C26 C27 1.405(4) . ? C26 B12 1.591(4) . ? C27 C28 1.393(4) . ? C28 C29 1.377(5) . ? C29 C30 1.381(5) . ? C29 C32 1.531(5) . ? C30 C31 1.409(4) . ? C33 C45 1.504(4) . ? C33 B35 1.718(4) . ? C33 B36 1.718(4) . ? C33 B34 1.719(4) . ? C33 B37 1.720(4) . ? C33 B38 1.720(5) . ? C45 C46 1.394(4) . ? C45 C50 1.404(4) . ? C46 C47 1.387(4) . ? C47 C48 1.399(5) . ? C48 C49 1.414(5) . ? C48 C51 1.486(5) . ? C49 C50 1.384(5) . ? C51 C52 1.400(5) . ? C51 C56 1.402(5) . ? C52 C53 1.387(5) . ? C53 C54 1.373(6) . ? C54 C55 1.399(6) . ? C54 C57 1.483(5) . ? C55 C56 1.389(5) . ? C58 C59 1.373(5) . ? C58 C63 1.413(5) . ? C58 B44 1.585(5) . ? C59 C60 1.420(5) . ? C60 C61 1.400(6) . ? C61 C62 1.338(6) . ? C61 C64 1.522(6) . ? C62 C63 1.389(5) . ? C65 C66 1.518(4) . ? C65 N2 1.521(3) . ? C67 C68 1.507(4) . ? C67 N2 1.526(3) . ? C69 C70 1.509(4) . ? C69 N2 1.519(3) . ? C71 C72 1.510(4) . ? C71 N2 1.524(3) . ? C73 C74 1.506(5) . ? C73 N1 1.523(4) . ? C75 C76 1.513(5) . ? C75 N1 1.519(4) . ? C77 C78 1.510(5) . ? C77 N1 1.516(4) . ? C79 C80 1.511(5) . ? C79 N1 1.535(4) . ? B2 B8 1.772(4) . ? B2 B7 1.773(4) . ? B2 B6 1.779(4) . ? B2 B3 1.780(4) . ? B3 B9 1.779(4) . ? B3 B8 1.783(4) . ? B3 B4 1.783(4) . ? B4 B10 1.762(4) . ? B4 B9 1.765(4) . ? B4 B5 1.774(5) . ? B5 B11 1.770(5) . ? B5 B10 1.771(4) . ? B5 B6 1.775(4) . ? B6 B7 1.769(4) . ? B6 B11 1.772(4) . ? B7 B8 1.783(4) . ? B7 B11 1.795(4) . ? B7 B12 1.797(4) . ? B8 B9 1.778(4) . ? B8 B12 1.793(4) . ? B9 B10 1.778(4) . ? B9 B12 1.790(4) . ? B10 B11 1.789(5) . ? B10 B12 1.791(4) . ? B11 B12 1.794(4) . ? B34 B35 1.765(5) . ? B34 B40 1.771(5) . ? B34 B39 1.774(5) . ? B34 B38 1.780(5) . ? B35 B41 1.768(5) . ? B35 B40 1.768(5) . ? B35 B36 1.771(5) . ? B36 B37 1.770(5) . ? B36 B42 1.776(5) . ? B36 B41 1.777(5) . ? B37 B42 1.762(5) . ? B37 B43 1.767(6) . ? B37 B38 1.773(6) . ? B38 B43 1.769(5) . ? B38 B39 1.784(6) . ? B39 B40 1.773(5) . ? B39 B43 1.787(6) . ? B39 B44 1.794(5) . ? B40 B41 1.779(5) . ? B40 B44 1.796(5) . ? B41 B42 1.772(5) . ? B41 B44 1.788(5) . ? B42 B43 1.770(5) . ? B42 B44 1.780(5) . ? B43 B44 1.780(5) . ? 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 C13 C1 B6 117.0(2) . . ? C13 C1 B2 120.5(2) . . ? B6 C1 B2 62.12(17) . . ? C13 C1 B4 119.2(2) . . ? B6 C1 B4 112.5(2) . . ? B2 C1 B4 112.7(2) . . ? C13 C1 B5 115.9(2) . . ? B6 C1 B5 61.91(17) . . ? B2 C1 B5 112.9(2) . . ? B4 C1 B5 61.82(18) . . ? C13 C1 B3 121.4(2) . . ? B6 C1 B3 113.1(2) . . ? B2 C1 B3 62.02(17) . . ? B4 C1 B3 62.14(18) . . ? B5 C1 B3 113.2(2) . . ? C18 C13 C14 117.8(3) . . ? C18 C13 C1 121.3(2) . . ? C14 C13 C1 120.8(2) . . ? C15 C14 C13 121.3(3) . . ? C14 C15 C16 121.2(3) . . ? C15 C16 C17 117.7(3) . . ? C15 C16 C19 119.2(3) . . ? C17 C16 C19 123.1(3) . . ? C18 C17 C16 121.3(3) . . ? C13 C18 C17 120.7(3) . . ? C24 C19 C20 115.9(3) . . ? C24 C19 C16 121.3(3) . . ? C20 C19 C16 122.8(3) . . ? C21 C20 C19 121.9(4) . . ? C22 C21 C20 119.0(4) . . ? C23 C22 C21 120.4(4) . . ? C23 C22 C25 120.6(4) . . ? C21 C22 C25 119.0(4) . . ? C22 C23 C24 120.6(4) . . ? C19 C24 C23 122.1(4) . . ? C31 C26 C27 116.3(3) . . ? C31 C26 B12 122.7(3) . . ? C27 C26 B12 121.0(3) . . ? C28 C27 C26 121.9(3) . . ? C29 C28 C27 120.9(3) . . ? C28 C29 C30 118.7(3) . . ? C28 C29 C32 118.5(3) . . ? C30 C29 C32 122.8(3) . . ? C29 C30 C31 120.5(3) . . ? C26 C31 C30 121.7(3) . . ? C45 C33 B35 118.6(2) . . ? C45 C33 B36 119.6(2) . . ? B35 C33 B36 62.0(2) . . ? C45 C33 B34 117.3(2) . . ? B35 C33 B34 61.8(2) . . ? B36 C33 B34 113.1(2) . . ? C45 C33 B37 120.0(2) . . ? B35 C33 B37 112.6(2) . . ? B36 C33 B37 62.0(2) . . ? B34 C33 B37 113.1(3) . . ? C45 C33 B38 118.2(2) . . ? B35 C33 B38 112.9(2) . . ? B36 C33 B38 113.3(2) . . ? B34 C33 B38 62.3(2) . . ? B37 C33 B38 62.1(2) . . ? C46 C45 C50 117.6(3) . . ? C46 C45 C33 121.6(3) . . ? C50 C45 C33 120.8(3) . . ? C47 C46 C45 121.2(3) . . ? C46 C47 C48 121.7(3) . . ? C47 C48 C49 116.9(3) . . ? C47 C48 C51 121.2(3) . . ? C49 C48 C51 121.8(3) . . ? C50 C49 C48 121.2(3) . . ? C49 C50 C45 121.3(3) . . ? C52 C51 C56 117.1(3) . . ? C52 C51 C48 121.1(3) . . ? C56 C51 C48 121.8(3) . . ? C53 C52 C51 120.4(4) . . ? C54 C53 C52 122.8(4) . . ? C53 C54 C55 117.2(4) . . ? C53 C54 C57 121.2(4) . . ? C55 C54 C57 121.6(4) . . ? C56 C55 C54 121.0(4) . . ? C55 C56 C51 121.4(4) . . ? C59 C58 C63 116.4(3) . . ? C59 C58 B44 123.2(3) . . ? C63 C58 B44 120.3(3) . . ? C58 C59 C60 121.2(4) . . ? C61 C60 C59 120.2(4) . . ? C62 C61 C60 118.9(4) . . ? C62 C61 C64 119.5(4) . . ? C60 C61 C64 121.6(4) . . ? C61 C62 C63 121.3(4) . . ? C62 C63 C58 122.0(4) . . ? C66 C65 N2 114.7(2) . . ? C68 C67 N2 115.0(2) . . ? C70 C69 N2 115.7(2) . . ? C72 C71 N2 115.5(2) . . ? C74 C73 N1 114.7(3) . . ? C76 C75 N1 115.3(3) . . ? C78 C77 N1 115.7(3) . . ? C80 C79 N1 115.1(3) . . ? C1 B2 B8 105.6(2) . . ? C1 B2 B7 105.6(2) . . ? B8 B2 B7 60.38(17) . . ? C1 B2 B6 58.88(16) . . ? B8 B2 B6 107.9(2) . . ? B7 B2 B6 59.75(17) . . ? C1 B2 B3 59.11(16) . . ? B8 B2 B3 60.26(17) . . ? B7 B2 B3 108.8(2) . . ? B6 B2 B3 108.1(2) . . ? C1 B3 B9 104.8(2) . . ? C1 B3 B2 58.87(16) . . ? B9 B3 B2 107.4(2) . . ? C1 B3 B8 104.9(2) . . ? B9 B3 B8 59.89(17) . . ? B2 B3 B8 59.65(17) . . ? C1 B3 B4 58.82(17) . . ? B9 B3 B4 59.40(17) . . ? B2 B3 B4 107.4(2) . . ? B8 B3 B4 107.2(2) . . ? C1 B4 B10 106.0(2) . . ? C1 B4 B9 105.6(2) . . ? B10 B4 B9 60.55(18) . . ? C1 B4 B5 59.15(16) . . ? B10 B4 B5 60.12(18) . . ? B9 B4 B5 108.4(2) . . ? C1 B4 B3 59.04(16) . . ? B10 B4 B3 109.0(2) . . ? B9 B4 B3 60.20(18) . . ? B5 B4 B3 108.5(2) . . ? C1 B5 B11 105.8(2) . . ? C1 B5 B10 105.5(2) . . ? B11 B5 B10 60.69(18) . . ? C1 B5 B4 59.03(17) . . ? B11 B5 B4 108.3(2) . . ? B10 B5 B4 59.61(18) . . ? C1 B5 B6 58.92(16) . . ? B11 B5 B6 59.99(18) . . ? B10 B5 B6 108.2(2) . . ? B4 B5 B6 107.8(2) . . ? C1 B6 B7 105.8(2) . . ? C1 B6 B11 105.9(2) . . ? B7 B6 B11 60.91(18) . . ? C1 B6 B5 59.18(16) . . ? B7 B6 B5 108.6(2) . . ? B11 B6 B5 59.88(18) . . ? C1 B6 B2 59.00(16) . . ? B7 B6 B2 59.96(17) . . ? B11 B6 B2 108.7(2) . . ? B5 B6 B2 108.2(2) . . ? B6 B7 B2 60.28(17) . . ? B6 B7 B8 107.8(2) . . ? B2 B7 B8 59.78(17) . . ? B6 B7 B11 59.62(17) . . ? B2 B7 B11 107.9(2) . . ? B8 B7 B11 107.8(2) . . ? B6 B7 B12 107.7(2) . . ? B2 B7 B12 108.0(2) . . ? B8 B7 B12 60.09(17) . . ? B11 B7 B12 59.93(17) . . ? B2 B8 B9 107.8(2) . . ? B2 B8 B7 59.85(17) . . ? B9 B8 B7 108.2(2) . . ? B2 B8 B3 60.09(17) . . ? B9 B8 B3 59.96(18) . . ? B7 B8 B3 108.2(2) . . ? B2 B8 B12 108.3(2) . . ? B9 B8 B12 60.18(17) . . ? B7 B8 B12 60.36(17) . . ? B3 B8 B12 108.5(2) . . ? B4 B9 B10 59.64(18) . . ? B4 B9 B8 108.2(2) . . ? B10 B9 B8 108.3(2) . . ? B4 B9 B3 60.40(18) . . ? B10 B9 B3 108.4(2) . . ? B8 B9 B3 60.15(18) . . ? B4 B9 B12 108.1(2) . . ? B10 B9 B12 60.27(17) . . ? B8 B9 B12 60.31(17) . . ? B3 B9 B12 108.8(2) . . ? B4 B10 B5 60.27(18) . . ? B4 B10 B9 59.81(18) . . ? B5 B10 B9 107.9(2) . . ? B4 B10 B11 108.0(2) . . ? B5 B10 B11 59.64(18) . . ? B9 B10 B11 108.0(2) . . ? B4 B10 B12 108.2(2) . . ? B5 B10 B12 108.0(2) . . ? B9 B10 B12 60.21(17) . . ? B11 B10 B12 60.16(17) . . ? B5 B11 B6 60.13(17) . . ? B5 B11 B10 59.68(18) . . ? B6 B11 B10 107.5(2) . . ? B5 B11 B12 107.9(2) . . ? B6 B11 B12 107.7(2) . . ? B10 B11 B12 59.99(17) . . ? B5 B11 B7 107.7(2) . . ? B6 B11 B7 59.47(17) . . ? B10 B11 B7 107.6(2) . . ? B12 B11 B7 60.10(17) . . ? C26 B12 B9 122.0(2) . . ? C26 B12 B10 123.3(2) . . ? B9 B12 B10 59.53(17) . . ? C26 B12 B8 120.8(2) . . ? B9 B12 B8 59.50(17) . . ? B10 B12 B8 107.1(2) . . ? C26 B12 B11 123.0(2) . . ? B9 B12 B11 107.3(2) . . ? B10 B12 B11 59.85(18) . . ? B8 B12 B11 107.4(2) . . ? C26 B12 B7 121.6(2) . . ? B9 B12 B7 107.0(2) . . ? B10 B12 B7 107.4(2) . . ? B8 B12 B7 59.54(17) . . ? B11 B12 B7 59.97(17) . . ? C33 B34 B35 59.09(19) . . ? C33 B34 B40 105.7(2) . . ? B35 B34 B40 60.0(2) . . ? C33 B34 B39 105.8(3) . . ? B35 B34 B39 108.1(3) . . ? B40 B34 B39 60.0(2) . . ? C33 B34 B38 58.9(2) . . ? B35 B34 B38 107.9(2) . . ? B40 B34 B38 108.1(2) . . ? B39 B34 B38 60.3(2) . . ? C33 B35 B34 59.14(19) . . ? C33 B35 B41 105.7(2) . . ? B34 B35 B41 108.5(2) . . ? C33 B35 B40 105.9(2) . . ? B34 B35 B40 60.2(2) . . ? B41 B35 B40 60.4(2) . . ? C33 B35 B36 58.98(19) . . ? B34 B35 B36 108.4(2) . . ? B41 B35 B36 60.3(2) . . ? B40 B35 B36 108.8(3) . . ? C33 B36 B37 59.05(19) . . ? C33 B36 B35 58.98(19) . . ? B37 B36 B35 107.7(3) . . ? C33 B36 B42 105.1(3) . . ? B37 B36 B42 59.6(2) . . ? B35 B36 B42 107.4(3) . . ? C33 B36 B41 105.3(2) . . ? B37 B36 B41 107.5(3) . . ? B35 B36 B41 59.8(2) . . ? B42 B36 B41 59.8(2) . . ? C33 B37 B42 105.7(2) . . ? C33 B37 B43 105.5(3) . . ? B42 B37 B43 60.2(2) . . ? C33 B37 B36 58.97(19) . . ? B42 B37 B36 60.4(2) . . ? B43 B37 B36 108.6(3) . . ? C33 B37 B38 58.99(19) . . ? B42 B37 B38 108.3(3) . . ? B43 B37 B38 60.0(2) . . ? B36 B37 B38 108.3(3) . . ? C33 B38 B43 105.4(3) . . ? C33 B38 B37 58.9(2) . . ? B43 B38 B37 59.8(2) . . ? C33 B38 B34 58.80(18) . . ? B43 B38 B34 107.8(3) . . ? B37 B38 B34 107.7(3) . . ? C33 B38 B39 105.3(2) . . ? B43 B38 B39 60.4(2) . . ? B37 B38 B39 108.1(3) . . ? B34 B38 B39 59.7(2) . . ? B40 B39 B34 59.9(2) . . ? B40 B39 B38 107.8(3) . . ? B34 B39 B38 60.0(2) . . ? B40 B39 B43 107.6(3) . . ? B34 B39 B43 107.3(3) . . ? B38 B39 B43 59.4(2) . . ? B40 B39 B44 60.5(2) . . ? B34 B39 B44 108.2(3) . . ? B38 B39 B44 107.6(3) . . ? B43 B39 B44 59.6(2) . . ? B35 B40 B34 59.8(2) . . ? B35 B40 B39 108.0(3) . . ? B34 B40 B39 60.1(2) . . ? B35 B40 B41 59.8(2) . . ? B34 B40 B41 107.7(2) . . ? B39 B40 B41 108.2(3) . . ? B35 B40 B44 108.0(3) . . ? B34 B40 B44 108.3(3) . . ? B39 B40 B44 60.4(2) . . ? B41 B40 B44 60.0(2) . . ? B35 B41 B42 107.8(2) . . ? B35 B41 B36 59.9(2) . . ? B42 B41 B36 60.1(2) . . ? B35 B41 B40 59.8(2) . . ? B42 B41 B40 108.0(3) . . ? B36 B41 B40 108.0(3) . . ? B35 B41 B44 108.4(3) . . ? B42 B41 B44 60.0(2) . . ? B36 B41 B44 108.5(2) . . ? B40 B41 B44 60.5(2) . . ? B37 B42 B43 60.0(2) . . ? B37 B42 B41 108.1(3) . . ? B43 B42 B41 108.1(3) . . ? B37 B42 B36 60.0(2) . . ? B43 B42 B36 108.1(3) . . ? B41 B42 B36 60.1(2) . . ? B37 B42 B44 108.7(3) . . ? B43 B42 B44 60.2(2) . . ? B41 B42 B44 60.5(2) . . ? B36 B42 B44 108.9(3) . . ? B37 B43 B38 60.2(2) . . ? B37 B43 B42 59.7(2) . . ? B38 B43 B42 108.1(3) . . ? B37 B43 B44 108.5(3) . . ? B38 B43 B44 108.9(3) . . ? B42 B43 B44 60.2(2) . . ? B37 B43 B39 108.3(3) . . ? B38 B43 B39 60.2(2) . . ? B42 B43 B39 108.1(3) . . ? B44 B43 B39 60.4(2) . . ? C58 B44 B42 121.5(3) . . ? C58 B44 B43 120.8(3) . . ? B42 B44 B43 59.6(2) . . ? C58 B44 B41 123.3(3) . . ? B42 B44 B41 59.5(2) . . ? B43 B44 B41 106.9(3) . . ? C58 B44 B39 122.1(3) . . ? B42 B44 B39 107.3(3) . . ? B43 B44 B39 60.0(2) . . ? B41 B44 B39 106.8(3) . . ? C58 B44 B40 123.9(3) . . ? B42 B44 B40 106.9(3) . . ? B43 B44 B40 106.9(3) . . ? B41 B44 B40 59.5(2) . . ? B39 B44 B40 59.2(2) . . ? C77 N1 C75 107.8(2) . . ? C77 N1 C73 111.1(2) . . ? C75 N1 C73 111.3(2) . . ? C77 N1 C79 110.8(2) . . ? C75 N1 C79 111.0(2) . . ? C73 N1 C79 104.9(2) . . ? C69 N2 C65 106.9(2) . . ? C69 N2 C71 110.7(2) . . ? C65 N2 C71 110.4(2) . . ? C69 N2 C67 111.1(2) . . ? C65 N2 C67 111.2(2) . . ? C71 N2 C67 106.53(19) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.871 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.070 data_njb79 _database_code_CSD 204007 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H24 B9 N' _chemical_formula_weight 363.68 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.9181(2) _cell_length_b 10.8545(3) _cell_length_c 19.3643(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.2720(10) _cell_angle_gamma 90.00 _cell_volume 2067.91(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.168 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.060 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9821 _exptl_absorpt_correction_T_max 0.9862 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 15 degree phi range. ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18031 _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_sigmaI/netI 0.0390 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4053 _reflns_number_gt 3363 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3 for Windows (Farrugia, 1997) XSeed (Barbour, 2001) ; _computing_publication_material 'WC (Thornton-Pett, 2000)' _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^)+(0.0628P)^2^+0.3676P] 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 SHELXL _refine_ls_extinction_coef 0.017(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4053 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1183 _refine_ls_wR_factor_gt 0.1106 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 N60 N 0.61664(10) 0.35458(9) 0.23839(5) 0.0317(3) Uani 1 1 d . . . C1 C 0.29402(13) 0.27873(11) 0.33836(6) 0.0326(3) Uani 1 1 d . . . C11 C 0.15135(13) 0.23620(11) 0.32046(6) 0.0332(3) Uani 1 1 d . . . C12 C 0.06527(13) 0.23177(12) 0.37210(7) 0.0363(3) Uani 1 1 d . . . C13 C -0.06610(13) 0.18774(13) 0.35710(7) 0.0397(3) Uani 1 1 d . . . C14 C -0.11313(14) 0.14550(13) 0.29110(7) 0.0421(3) Uani 1 1 d . . . C15 C -0.02856(14) 0.15001(14) 0.23933(7) 0.0428(3) Uani 1 1 d . . . C16 C 0.10239(14) 0.19634(12) 0.25358(7) 0.0383(3) Uani 1 1 d . . . C61 C 0.55023(14) 0.31916(13) 0.17653(7) 0.0411(3) Uani 1 1 d . . . C62 C 0.60755(15) 0.32916(14) 0.11555(7) 0.0429(3) Uani 1 1 d . . . C63 C 0.73779(13) 0.37620(12) 0.11644(6) 0.0348(3) Uani 1 1 d . . . C64 C 0.80428(13) 0.41400(12) 0.18024(7) 0.0359(3) Uani 1 1 d . . . C65 C 0.74271(13) 0.40268(12) 0.23969(7) 0.0343(3) Uani 1 1 d . . . C66 C 0.80433(14) 0.38645(14) 0.05067(7) 0.0400(3) Uani 1 1 d . . . C67 C 0.93885(13) 0.31860(12) 0.05568(6) 0.0347(3) Uani 1 1 d . . . C68 C 0.94240(16) 0.19059(13) 0.05080(7) 0.0422(3) Uani 1 1 d . . . C69 C 1.06542(17) 0.12887(15) 0.05710(7) 0.0490(4) Uani 1 1 d . . . C70 C 1.18703(16) 0.19289(16) 0.06722(7) 0.0492(4) Uani 1 1 d . . . C71 C 1.18480(15) 0.32005(15) 0.07182(7) 0.0466(4) Uani 1 1 d . . . C72 C 1.06124(14) 0.38217(13) 0.06645(7) 0.0392(3) Uani 1 1 d . . . B2 B 0.42621(14) 0.22025(13) 0.31020(7) 0.0317(3) Uani 1 1 d . . . B3 B 0.37227(15) 0.38273(13) 0.29921(7) 0.0336(3) Uani 1 1 d . . . B4 B 0.34534(15) 0.38878(14) 0.39137(8) 0.0362(3) Uani 1 1 d . . . B5 B 0.39914(15) 0.22698(13) 0.40221(7) 0.0338(3) Uani 1 1 d . . . B6 B 0.54930(14) 0.34190(13) 0.30611(7) 0.0322(3) Uani 1 1 d . . . B7 B 0.49363(16) 0.46058(14) 0.36280(8) 0.0373(3) Uani 1 1 d . . . B8 B 0.51192(15) 0.35025(14) 0.43547(7) 0.0370(3) Uani 1 1 d . . . B9 B 0.56964(15) 0.23036(14) 0.37793(7) 0.0345(3) Uani 1 1 d . . . B10 B 0.63652(16) 0.37525(14) 0.38480(7) 0.0366(3) Uani 1 1 d . . . H2 H 0.4149(13) 0.1429(14) 0.2710(7) 0.039(4) Uiso 1 1 d . . . H3 H 0.3188(13) 0.4261(13) 0.2519(7) 0.036(3) Uiso 1 1 d . . . H4 H 0.2661(14) 0.4413(14) 0.4163(7) 0.043(4) Uiso 1 1 d . . . H5 H 0.3643(13) 0.1488(13) 0.4379(7) 0.038(4) Uiso 1 1 d . . . H7 H 0.5002(15) 0.5646(15) 0.3616(7) 0.051(4) Uiso 1 1 d . . . H8 H 0.5344(13) 0.3633(12) 0.4958(7) 0.031(3) Uiso 1 1 d . . . H9 H 0.6359(14) 0.1436(14) 0.3889(7) 0.044(4) Uiso 1 1 d . . . H10 H 0.7434(15) 0.4051(14) 0.3977(7) 0.044(4) Uiso 1 1 d . . . H12 H 0.0988(14) 0.2607(13) 0.4192(8) 0.038(4) Uiso 1 1 d . . . H13 H -0.1262(15) 0.1855(14) 0.3935(8) 0.047(4) Uiso 1 1 d . . . H14 H -0.2071(16) 0.1154(14) 0.2808(7) 0.047(4) Uiso 1 1 d . . . H15 H -0.0596(15) 0.1229(15) 0.1927(8) 0.052(4) Uiso 1 1 d . . . H16 H 0.1629(15) 0.2008(13) 0.2170(8) 0.040(4) Uiso 1 1 d . . . H61 H 0.4581(16) 0.2859(14) 0.1782(8) 0.043(4) Uiso 1 1 d . . . H62 H 0.5534(16) 0.3040(15) 0.0726(9) 0.052(4) Uiso 1 1 d . . . H64 H 0.8960(15) 0.4474(15) 0.1849(7) 0.045(4) Uiso 1 1 d . . . H65 H 0.7890(14) 0.4262(14) 0.2862(7) 0.041(4) Uiso 1 1 d . . . H66A H 0.7410(15) 0.3533(15) 0.0107(8) 0.045(4) Uiso 1 1 d . . . H66B H 0.8205(14) 0.4749(15) 0.0429(7) 0.044(4) Uiso 1 1 d . . . H68 H 0.8561(16) 0.1469(15) 0.0432(8) 0.049(4) Uiso 1 1 d . . . H69 H 1.0651(17) 0.0372(18) 0.0542(8) 0.063(5) Uiso 1 1 d . . . H70 H 1.2802(17) 0.1486(16) 0.0706(9) 0.059(5) Uiso 1 1 d . . . H71 H 1.2739(17) 0.3715(16) 0.0801(8) 0.059(5) Uiso 1 1 d . . . H72 H 1.0597(15) 0.4713(16) 0.0693(8) 0.049(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 N60 0.0347(6) 0.0283(5) 0.0336(5) -0.0006(4) 0.0110(4) -0.0018(4) C1 0.0341(7) 0.0320(6) 0.0336(6) 0.0005(5) 0.0114(5) 0.0013(5) C11 0.0323(6) 0.0320(7) 0.0362(6) 0.0034(5) 0.0079(5) 0.0027(5) C12 0.0350(7) 0.0394(7) 0.0358(7) 0.0015(5) 0.0093(5) 0.0013(5) C13 0.0335(7) 0.0421(8) 0.0450(7) 0.0063(6) 0.0109(6) 0.0011(6) C14 0.0338(7) 0.0402(8) 0.0514(8) 0.0069(6) 0.0026(6) -0.0004(6) C15 0.0439(8) 0.0448(8) 0.0385(7) 0.0011(6) -0.0001(6) 0.0020(6) C16 0.0396(7) 0.0407(7) 0.0357(7) 0.0041(5) 0.0094(6) 0.0029(6) C61 0.0396(7) 0.0475(8) 0.0375(7) -0.0039(6) 0.0106(6) -0.0101(6) C62 0.0442(8) 0.0513(8) 0.0345(7) -0.0051(6) 0.0099(6) -0.0077(6) C63 0.0400(7) 0.0303(6) 0.0362(6) 0.0036(5) 0.0126(5) 0.0041(5) C64 0.0350(7) 0.0353(7) 0.0392(7) 0.0018(5) 0.0114(5) -0.0014(5) C65 0.0343(7) 0.0332(7) 0.0365(7) -0.0002(5) 0.0088(5) -0.0026(5) C66 0.0426(8) 0.0445(8) 0.0351(7) 0.0065(6) 0.0137(6) 0.0050(6) C67 0.0418(7) 0.0379(7) 0.0262(6) 0.0024(5) 0.0114(5) 0.0031(5) C68 0.0507(8) 0.0400(8) 0.0364(7) -0.0010(5) 0.0078(6) -0.0005(6) C69 0.0658(10) 0.0413(8) 0.0398(7) -0.0019(6) 0.0060(7) 0.0132(7) C70 0.0513(9) 0.0611(10) 0.0358(7) 0.0024(6) 0.0077(6) 0.0186(7) C71 0.0414(8) 0.0616(10) 0.0372(7) 0.0045(6) 0.0071(6) 0.0000(7) C72 0.0463(8) 0.0389(8) 0.0340(6) 0.0022(5) 0.0116(6) 0.0001(6) B2 0.0326(7) 0.0296(7) 0.0344(7) 0.0004(6) 0.0098(6) -0.0006(6) B3 0.0365(7) 0.0300(7) 0.0363(7) 0.0005(6) 0.0117(6) 0.0014(6) B4 0.0402(8) 0.0331(8) 0.0375(7) -0.0016(6) 0.0138(6) 0.0005(6) B5 0.0357(8) 0.0332(7) 0.0340(7) 0.0003(6) 0.0102(6) -0.0011(6) B6 0.0343(7) 0.0300(7) 0.0344(7) -0.0003(5) 0.0119(6) -0.0016(5) B7 0.0451(8) 0.0303(7) 0.0387(7) -0.0036(6) 0.0148(6) -0.0033(6) B8 0.0420(8) 0.0367(8) 0.0339(7) -0.0024(6) 0.0106(6) -0.0044(6) B9 0.0336(7) 0.0358(8) 0.0351(7) 0.0022(6) 0.0082(6) -0.0007(6) B10 0.0390(8) 0.0370(8) 0.0352(7) -0.0024(6) 0.0100(6) -0.0052(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N60 C61 1.3480(17) . ? N60 C65 1.3523(16) . ? N60 B6 1.5511(16) . ? C1 C11 1.4870(17) . ? C1 B2 1.6125(17) . ? C1 B3 1.6125(18) . ? C1 B5 1.6140(19) . ? C1 B4 1.6149(19) . ? C11 C16 1.3932(18) . ? C11 C12 1.3955(17) . ? C12 C13 1.3837(19) . ? C12 H12 0.982(15) . ? C13 C14 1.382(2) . ? C13 H13 0.980(15) . ? C14 C15 1.387(2) . ? C14 H14 0.984(15) . ? C15 C16 1.388(2) . ? C15 H15 0.962(16) . ? C16 H16 0.986(15) . ? C61 C62 1.3781(19) . ? C61 H61 0.987(15) . ? C62 C63 1.3871(19) . ? C62 H62 0.971(17) . ? C63 C64 1.3868(18) . ? C63 C66 1.5108(17) . ? C64 C65 1.3753(17) . ? C64 H64 0.972(15) . ? C65 H65 0.992(14) . ? C66 C67 1.5163(18) . ? C66 H66A 1.000(15) . ? C66 H66B 0.988(16) . ? C67 C72 1.3889(19) . ? C67 C68 1.393(2) . ? C68 C69 1.384(2) . ? C68 H68 0.973(16) . ? C69 C70 1.384(2) . ? C69 H69 0.997(19) . ? C70 C71 1.383(2) . ? C70 H70 1.036(17) . ? C71 C72 1.391(2) . ? C71 H71 1.041(17) . ? C72 H72 0.970(17) . ? B2 B6 1.807(2) . ? B2 B9 1.812(2) . ? B2 B5 1.8366(19) . ? B2 B3 1.847(2) . ? B2 H2 1.128(14) . ? B3 B6 1.799(2) . ? B3 B7 1.818(2) . ? B3 B4 1.839(2) . ? B3 H3 1.104(13) . ? B4 B8 1.810(2) . ? B4 B7 1.812(2) . ? B4 B5 1.840(2) . ? B4 H4 1.128(14) . ? B5 B8 1.809(2) . ? B5 B9 1.812(2) . ? B5 H5 1.173(14) . ? B6 B10 1.694(2) . ? B6 B7 1.823(2) . ? B6 B9 1.836(2) . ? B7 B10 1.701(2) . ? B7 B8 1.839(2) . ? B7 H7 1.132(17) . ? B8 B10 1.694(2) . ? B8 B9 1.850(2) . ? B8 H8 1.170(13) . ? B9 B10 1.706(2) . ? B9 H9 1.153(15) . ? B10 H10 1.106(14) . ? 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 C61 N60 C65 118.25(10) . . ? C61 N60 B6 120.78(10) . . ? C65 N60 B6 120.97(10) . . ? C11 C1 B2 126.12(11) . . ? C11 C1 B3 127.46(11) . . ? B2 C1 B3 69.90(8) . . ? C11 C1 B5 125.02(10) . . ? B2 C1 B5 69.39(9) . . ? B3 C1 B5 107.52(10) . . ? C11 C1 B4 126.29(10) . . ? B2 C1 B4 107.56(10) . . ? B3 C1 B4 69.47(9) . . ? B5 C1 B4 69.47(9) . . ? C16 C11 C12 118.85(12) . . ? C16 C11 C1 121.49(11) . . ? C12 C11 C1 119.62(11) . . ? C13 C12 C11 120.44(12) . . ? C13 C12 H12 120.3(8) . . ? C11 C12 H12 119.2(8) . . ? C14 C13 C12 120.49(12) . . ? C14 C13 H13 119.5(9) . . ? C12 C13 H13 120.0(9) . . ? C13 C14 C15 119.50(13) . . ? C13 C14 H14 119.8(8) . . ? C15 C14 H14 120.6(8) . . ? C14 C15 C16 120.37(13) . . ? C14 C15 H15 121.1(9) . . ? C16 C15 H15 118.5(9) . . ? C15 C16 C11 120.32(12) . . ? C15 C16 H16 120.9(9) . . ? C11 C16 H16 118.7(9) . . ? N60 C61 C62 122.06(12) . . ? N60 C61 H61 115.1(9) . . ? C62 C61 H61 122.8(9) . . ? C61 C62 C63 120.19(13) . . ? C61 C62 H62 117.9(9) . . ? C63 C62 H62 121.9(9) . . ? C64 C63 C62 117.20(11) . . ? C64 C63 C66 121.33(12) . . ? C62 C63 C66 121.47(12) . . ? C65 C64 C63 120.52(12) . . ? C65 C64 H64 117.7(8) . . ? C63 C64 H64 121.8(8) . . ? N60 C65 C64 121.76(12) . . ? N60 C65 H65 115.9(8) . . ? C64 C65 H65 122.3(8) . . ? C63 C66 C67 112.65(11) . . ? C63 C66 H66A 109.1(8) . . ? C67 C66 H66A 109.6(9) . . ? C63 C66 H66B 107.2(8) . . ? C67 C66 H66B 108.9(9) . . ? H66A C66 H66B 109.3(12) . . ? C72 C67 C68 118.46(13) . . ? C72 C67 C66 120.90(12) . . ? C68 C67 C66 120.63(12) . . ? C69 C68 C67 120.42(14) . . ? C69 C68 H68 121.8(9) . . ? C67 C68 H68 117.8(9) . . ? C68 C69 C70 120.81(14) . . ? C68 C69 H69 118.8(10) . . ? C70 C69 H69 120.4(10) . . ? C71 C70 C69 119.29(14) . . ? C71 C70 H70 118.7(10) . . ? C69 C70 H70 122.0(10) . . ? C70 C71 C72 119.99(14) . . ? C70 C71 H71 121.7(9) . . ? C72 C71 H71 118.3(9) . . ? C67 C72 C71 121.02(14) . . ? C67 C72 H72 119.0(9) . . ? C71 C72 H72 120.0(9) . . ? C1 B2 B6 108.06(10) . . ? C1 B2 B9 109.20(10) . . ? B6 B2 B9 60.96(8) . . ? C1 B2 B5 55.34(8) . . ? B6 B2 B5 101.31(9) . . ? B9 B2 B5 59.55(8) . . ? C1 B2 B3 55.05(7) . . ? B6 B2 B3 58.99(8) . . ? B9 B2 B3 102.41(10) . . ? B5 B2 B3 89.88(9) . . ? C1 B2 H2 120.3(7) . . ? B6 B2 H2 121.7(7) . . ? B9 B2 H2 122.3(7) . . ? B5 B2 H2 131.9(7) . . ? B3 B2 H2 129.1(7) . . ? C1 B3 B6 108.41(10) . . ? C1 B3 B7 108.89(10) . . ? B6 B3 B7 60.52(8) . . ? C1 B3 B4 55.33(8) . . ? B6 B3 B4 101.36(10) . . ? B7 B3 B4 59.40(8) . . ? C1 B3 B2 55.05(7) . . ? B6 B3 B2 59.38(8) . . ? B7 B3 B2 102.03(10) . . ? B4 B3 B2 89.88(9) . . ? C1 B3 H3 118.7(7) . . ? B6 B3 H3 121.9(7) . . ? B7 B3 H3 124.8(7) . . ? B4 B3 H3 132.5(7) . . ? B2 B3 H3 127.2(7) . . ? C1 B4 B8 108.93(10) . . ? C1 B4 B7 109.07(10) . . ? B8 B4 B7 61.03(8) . . ? C1 B4 B3 55.21(8) . . ? B8 B4 B3 102.33(9) . . ? B7 B4 B3 59.72(8) . . ? C1 B4 B5 55.24(8) . . ? B8 B4 B5 59.43(8) . . ? B7 B4 B5 102.15(10) . . ? B3 B4 B5 90.05(9) . . ? C1 B4 H4 117.7(7) . . ? B8 B4 H4 124.0(7) . . ? B7 B4 H4 123.4(7) . . ? B3 B4 H4 128.9(7) . . ? B5 B4 H4 129.9(7) . . ? C1 B5 B8 109.00(11) . . ? C1 B5 B9 109.13(10) . . ? B8 B5 B9 61.46(8) . . ? C1 B5 B2 55.27(7) . . ? B8 B5 B2 102.42(9) . . ? B9 B5 B2 59.55(8) . . ? C1 B5 B4 55.29(8) . . ? B8 B5 B4 59.47(8) . . ? B9 B5 B4 102.58(10) . . ? B2 B5 B4 90.19(9) . . ? C1 B5 H5 119.5(7) . . ? B8 B5 H5 122.7(7) . . ? B9 B5 H5 121.4(7) . . ? B2 B5 H5 129.2(7) . . ? B4 B5 H5 130.9(7) . . ? N60 B6 B10 121.08(11) . . ? N60 B6 B3 115.84(10) . . ? B10 B6 B3 113.37(10) . . ? N60 B6 B2 117.88(10) . . ? B10 B6 B2 112.81(10) . . ? B3 B6 B2 61.63(8) . . ? N60 B6 B7 129.94(10) . . ? B10 B6 B7 57.73(8) . . ? B3 B6 B7 60.23(8) . . ? B2 B6 B7 103.42(9) . . ? N60 B6 B9 132.94(11) . . ? B10 B6 B9 57.63(8) . . ? B3 B6 B9 103.37(9) . . ? B2 B6 B9 59.66(8) . . ? B7 B6 B9 91.28(9) . . ? B10 B7 B4 111.84(11) . . ? B10 B7 B3 112.07(10) . . ? B4 B7 B3 60.88(8) . . ? B10 B7 B6 57.31(8) . . ? B4 B7 B6 101.50(10) . . ? B3 B7 B6 59.24(8) . . ? B10 B7 B8 57.02(8) . . ? B4 B7 B8 59.44(8) . . ? B3 B7 B8 102.02(10) . . ? B6 B7 B8 89.58(9) . . ? B10 B7 H7 120.0(8) . . ? B4 B7 H7 119.1(7) . . ? B3 B7 H7 119.0(8) . . ? B6 B7 H7 132.1(7) . . ? B8 B7 H7 131.7(7) . . ? B10 B8 B5 112.07(10) . . ? B10 B8 B4 112.27(11) . . ? B5 B8 B4 61.10(8) . . ? B10 B8 B7 57.40(8) . . ? B5 B8 B7 102.27(10) . . ? B4 B8 B7 59.53(8) . . ? B10 B8 B9 57.32(8) . . ? B5 B8 B9 59.34(8) . . ? B4 B8 B9 102.23(10) . . ? B7 B8 B9 90.30(9) . . ? B10 B8 H8 119.9(6) . . ? B5 B8 H8 118.4(6) . . ? B4 B8 H8 119.3(6) . . ? B7 B8 H8 132.3(7) . . ? B9 B8 H8 130.7(6) . . ? B10 B9 B5 111.40(11) . . ? B10 B9 B2 111.98(11) . . ? B5 B9 B2 60.90(8) . . ? B10 B9 B6 57.00(8) . . ? B5 B9 B6 101.15(10) . . ? B2 B9 B6 59.38(8) . . ? B10 B9 B8 56.73(8) . . ? B5 B9 B8 59.20(8) . . ? B2 B9 B8 101.77(10) . . ? B6 B9 B8 88.84(9) . . ? B10 B9 H9 122.1(7) . . ? B5 B9 H9 117.7(7) . . ? B2 B9 H9 117.4(7) . . ? B6 B9 H9 133.1(7) . . ? B8 B9 H9 132.6(7) . . ? B6 B10 B8 99.20(10) . . ? B6 B10 B7 64.95(9) . . ? B8 B10 B7 65.58(9) . . ? B6 B10 B9 65.37(9) . . ? B8 B10 B9 65.95(9) . . ? B7 B10 B9 100.31(10) . . ? B6 B10 H10 129.1(7) . . ? B8 B10 H10 131.7(7) . . ? B7 B10 H10 129.9(8) . . ? B9 B10 H10 129.8(8) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.209 _refine_diff_density_min -0.170 _refine_diff_density_rms 0.045 data_c:\windows\desktop\andy\struct~1\conh28~1\sx _database_code_CSD 204008 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H72 B18 N4 O2' _chemical_formula_weight 811.58 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.25280(10) _cell_length_b 24.5742(3) _cell_length_c 14.40150(10) _cell_angle_alpha 90.00 _cell_angle_beta 102.9230(10) _cell_angle_gamma 90.00 _cell_volume 4916.38(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.096 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 0.061 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9821 _exptl_absorpt_correction_T_max 0.9958 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 15 degree phi range. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 67006 _diffrn_reflns_av_R_equivalents 0.0674 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9637 _reflns_number_gt 7882 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3 for Windows (Farrugia, 1997) XSeed (Barbour, 2001) ; _computing_publication_material 'WC (Thornton-Pett, 2000)' _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^)+(0.1102P)^2^+1.9052P] 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 SHELXL _refine_ls_extinction_coef 0.0151(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9637 _refine_ls_number_parameters 576 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0773 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.1882 _refine_ls_wR_factor_gt 0.1691 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.069 _refine_ls_shift/su_mean 0.008 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 O1 O 0.08103(12) 0.26200(7) 0.04559(15) 0.0726(5) Uani 1 1 d . . . O2 O 0.44321(9) 0.47593(5) 0.08459(10) 0.0478(3) Uani 1 1 d . . . N1 N 0.19883(12) 0.23362(7) -0.02444(12) 0.0443(4) Uani 1 1 d . . . N2 N 0.30919(12) 0.52077(6) 0.10183(12) 0.0436(4) Uani 1 1 d . . . N3 N 0.13850(10) 0.71135(6) 0.81735(11) 0.0405(4) Uani 1 1 d . . . N4 N 0.62921(11) 0.55839(7) 0.31970(12) 0.0475(4) Uani 1 1 d . . . C1A C 0.44170(13) 0.74000(8) 0.10439(13) 0.0406(4) Uani 1 1 d . . . C1B C 0.06604(12) 0.02911(7) -0.19149(12) 0.0362(4) Uani 1 1 d . . . C2A C 0.40846(13) 0.68273(8) 0.10512(13) 0.0402(4) Uani 1 1 d . . . C2B C 0.09707(12) 0.08255(7) -0.14649(13) 0.0372(4) Uani 1 1 d . . . C3A C 0.43490(14) 0.64427(8) 0.04451(14) 0.0449(4) Uani 1 1 d . . . H3A H 0.4746 0.6551 0.0029 0.054 Uiso 1 1 calc R . . C3B C 0.06844(13) 0.10102(7) -0.06585(13) 0.0388(4) Uani 1 1 d . . . H3B H 0.0268 0.0791 -0.0385 0.047 Uiso 1 1 calc R . . C4A C 0.40473(14) 0.59065(8) 0.04341(14) 0.0444(4) Uani 1 1 d . . . H4A H 0.4242 0.5650 0.0021 0.053 Uiso 1 1 calc R . . C4B C 0.09927(13) 0.15082(7) -0.02426(13) 0.0395(4) Uani 1 1 d . . . H4B H 0.0791 0.1626 0.0310 0.047 Uiso 1 1 calc R . . C5A C 0.34551(13) 0.57475(7) 0.10343(14) 0.0408(4) Uani 1 1 d . . . C5B C 0.15993(13) 0.18325(7) -0.06423(13) 0.0394(4) Uani 1 1 d . . . C6 C 0.35894(13) 0.47490(7) 0.08971(13) 0.0389(4) Uani 1 1 d . . . C6A C 0.31844(13) 0.61255(8) 0.16453(14) 0.0429(4) Uani 1 1 d . . . H6A H 0.2782 0.6018 0.2057 0.051 Uiso 1 1 calc R . . C6B C 0.18802(14) 0.16560(8) -0.14521(14) 0.0470(5) Uani 1 1 d . . . H6B H 0.2287 0.1878 -0.1732 0.056 Uiso 1 1 calc R . . C7 C 0.30409(13) 0.42242(7) 0.08050(12) 0.0368(4) Uani 1 1 d . . . C7A C 0.35025(13) 0.66582(8) 0.16529(14) 0.0428(4) Uani 1 1 d . . . H7A H 0.3320 0.6913 0.2077 0.051 Uiso 1 1 calc R . . C7B C 0.15737(14) 0.11606(8) -0.18546(15) 0.0461(5) Uani 1 1 d . . . H7B H 0.1776 0.1045 -0.2408 0.055 Uiso 1 1 calc R . . C8 C 0.20446(13) 0.41945(8) 0.06214(13) 0.0419(4) Uani 1 1 d . . . H8 H 0.1674 0.4518 0.0597 0.050 Uiso 1 1 calc R . . C9 C 0.15904(14) 0.36955(8) 0.04734(14) 0.0447(4) Uani 1 1 d . . . H9 H 0.0909 0.3677 0.0366 0.054 Uiso 1 1 calc R . . C10 C 0.21206(13) 0.32204(7) 0.04796(13) 0.0399(4) Uani 1 1 d . . . C11 C 0.31239(14) 0.32481(8) 0.06846(14) 0.0438(4) Uani 1 1 d . . . H11 H 0.3495 0.2925 0.0706 0.053 Uiso 1 1 calc R . . C12 C 0.35750(14) 0.37462(8) 0.08564(14) 0.0426(4) Uani 1 1 d . . . H12 H 0.4258 0.3763 0.1012 0.051 Uiso 1 1 calc R . . C13 C 0.15786(14) 0.26983(8) 0.02446(14) 0.0443(4) Uani 1 1 d . . . C14 C 0.67725(16) 0.55622(9) 0.42486(15) 0.0546(5) Uani 1 1 d . . . H14A H 0.7403 0.5748 0.4345 0.066 Uiso 1 1 calc R . . H14B H 0.6372 0.5769 0.4606 0.066 Uiso 1 1 calc R . . C15 C 0.69320(18) 0.49982(11) 0.46688(19) 0.0714(7) Uani 1 1 d . . . H15A H 0.6315 0.4806 0.4567 0.107 Uiso 1 1 calc R . . H15B H 0.7213 0.5025 0.5353 0.107 Uiso 1 1 calc R . . H15C H 0.7372 0.4798 0.4358 0.107 Uiso 1 1 calc R . . C16 C 0.69602(16) 0.53332(12) 0.26327(17) 0.0643(6) Uani 1 1 d . . . H16A H 0.7043 0.4943 0.2800 0.077 Uiso 1 1 calc R . . H16B H 0.7599 0.5509 0.2827 0.077 Uiso 1 1 calc R . . C17 C 0.66161(18) 0.53832(16) 0.15540(19) 0.0872(10) Uani 1 1 d . . . H17A H 0.5969 0.5228 0.1355 0.131 Uiso 1 1 calc R . . H17B H 0.7059 0.5186 0.1242 0.131 Uiso 1 1 calc R . . H17C H 0.6600 0.5768 0.1372 0.131 Uiso 1 1 calc R . . C18 C 0.53579(14) 0.52619(9) 0.29903(15) 0.0520(5) Uani 1 1 d . . . H18A H 0.5049 0.5304 0.2307 0.062 Uiso 1 1 calc R . . H18B H 0.5516 0.4872 0.3104 0.062 Uiso 1 1 calc R . . C19 C 0.46369(16) 0.54195(11) 0.35678(16) 0.0605(6) Uani 1 1 d . . . H19A H 0.4909 0.5347 0.4243 0.091 Uiso 1 1 calc R . . H19B H 0.4047 0.5206 0.3355 0.091 Uiso 1 1 calc R . . H19C H 0.4487 0.5808 0.3479 0.091 Uiso 1 1 calc R . . C20 C 0.60617(18) 0.61709(10) 0.29198(17) 0.0621(6) Uani 1 1 d . . . H20A H 0.5653 0.6320 0.3332 0.075 Uiso 1 1 calc R . . H20B H 0.5680 0.6180 0.2255 0.075 Uiso 1 1 calc R . . C21 C 0.6928(2) 0.65388(12) 0.2993(2) 0.0860(9) Uani 1 1 d . . . H21A H 0.7311 0.6536 0.3649 0.129 Uiso 1 1 calc R . . H21B H 0.6711 0.6911 0.2816 0.129 Uiso 1 1 calc R . . H21C H 0.7322 0.6408 0.2562 0.129 Uiso 1 1 calc R . . C22 C 0.08404(15) 0.67425(8) 0.87137(16) 0.0489(5) Uani 1 1 d . . . H22A H 0.0320 0.6956 0.8896 0.059 Uiso 1 1 calc R . . H22B H 0.0533 0.6450 0.8279 0.059 Uiso 1 1 calc R . . C23 C 0.14412(19) 0.64855(11) 0.95956(18) 0.0678(6) Uani 1 1 d . . . H23A H 0.1903 0.6233 0.9417 0.102 Uiso 1 1 calc R . . H23B H 0.1023 0.6286 0.9933 0.102 Uiso 1 1 calc R . . H23C H 0.1790 0.6769 1.0012 0.102 Uiso 1 1 calc R . . C24 C 0.18312(14) 0.75943(8) 0.87778(14) 0.0452(4) Uani 1 1 d . . . H24A H 0.2317 0.7454 0.9327 0.054 Uiso 1 1 calc R . . H24B H 0.2174 0.7822 0.8393 0.054 Uiso 1 1 calc R . . C25 C 0.11389(15) 0.79520(8) 0.91514(15) 0.0491(5) Uani 1 1 d . . . H25A H 0.0661 0.8102 0.8616 0.074 Uiso 1 1 calc R . . H25B H 0.1494 0.8250 0.9525 0.074 Uiso 1 1 calc R . . H25C H 0.0812 0.7736 0.9557 0.074 Uiso 1 1 calc R . . C26 C 0.06563(14) 0.73037(9) 0.73007(14) 0.0482(5) Uani 1 1 d . . . H26A H 0.0364 0.6980 0.6940 0.058 Uiso 1 1 calc R . . H26B H 0.0136 0.7502 0.7513 0.058 Uiso 1 1 calc R . . C27 C 0.10539(17) 0.76683(10) 0.66346(16) 0.0575(5) Uani 1 1 d . . . H27A H 0.1320 0.7999 0.6974 0.086 Uiso 1 1 calc R . . H27B H 0.0537 0.7766 0.6089 0.086 Uiso 1 1 calc R . . H27C H 0.1563 0.7476 0.6410 0.086 Uiso 1 1 calc R . . C28 C 0.22166(14) 0.68110(8) 0.78983(16) 0.0490(5) Uani 1 1 d . . . H28A H 0.2558 0.7065 0.7554 0.059 Uiso 1 1 calc R . . H28B H 0.2677 0.6696 0.8487 0.059 Uiso 1 1 calc R . . C29 C 0.19141(19) 0.63148(11) 0.7281(2) 0.0731(7) Uani 1 1 d . . . H29A H 0.1622 0.6047 0.7634 0.110 Uiso 1 1 calc R . . H29B H 0.2480 0.6154 0.7106 0.110 Uiso 1 1 calc R . . H29C H 0.1445 0.6422 0.6703 0.110 Uiso 1 1 calc R . . B2A B 0.37552(16) 0.79365(9) 0.09866(17) 0.0444(5) Uani 1 1 d . . . H2A H 0.2965 0.7908 0.0959 0.053 Uiso 1 1 calc R . . B2B B 0.13357(15) -0.01091(8) -0.23669(15) 0.0388(4) Uani 1 1 d . . . H2B H 0.2107 -0.0008 -0.2341 0.047 Uiso 1 1 calc R . . B3A B 0.47966(16) 0.77839(10) 0.19585(17) 0.0463(5) Uani 1 1 d . . . H3A1 H 0.4840 0.7634 0.2701 0.056 Uiso 1 1 calc R . . B3B B 0.07258(15) -0.02986(9) -0.14101(16) 0.0410(5) Uani 1 1 d . . . H3B1 H 0.1010 -0.0350 -0.0625 0.049 Uiso 1 1 calc R . . B4A B 0.55012(16) 0.75995(9) 0.10747(16) 0.0431(5) Uani 1 1 d . . . H4A1 H 0.6106 0.7303 0.1117 0.052 Uiso 1 1 calc R . . B4B B -0.03866(14) 0.00148(8) -0.20753(16) 0.0400(5) Uani 1 1 d . . . H4B1 H -0.0989 0.0214 -0.1820 0.048 Uiso 1 1 calc R . . B5A B 0.44546(15) 0.77501(9) 0.01032(16) 0.0425(5) Uani 1 1 d . . . H5A H 0.4224 0.7573 -0.0629 0.051 Uiso 1 1 calc R . . B5B B 0.02171(15) 0.02041(8) -0.30365(15) 0.0392(4) Uani 1 1 d . . . H5B H 0.0094 0.0554 -0.3547 0.047 Uiso 1 1 calc R . . B6A B 0.44600(18) 0.84823(10) 0.16259(19) 0.0532(6) Uani 1 1 d . . . H6A1 H 0.4152 0.8748 0.2116 0.064 Uiso 1 1 calc R . . B6B B 0.09706(16) -0.08026(9) -0.22451(17) 0.0439(5) Uani 1 1 d . . . H6B1 H 0.1526 -0.1125 -0.2002 0.053 Uiso 1 1 calc R . . B7A B 0.56937(17) 0.82437(10) 0.16944(18) 0.0507(6) Uani 1 1 d . . . H7A1 H 0.6375 0.8318 0.2241 0.061 Uiso 1 1 calc R . . B7B B -0.02517(16) -0.07153(9) -0.20402(18) 0.0454(5) Uani 1 1 d . . . H7B1 H -0.0677 -0.0969 -0.1635 0.055 Uiso 1 1 calc R . . B8A B 0.54555(17) 0.82155(9) 0.03874(17) 0.0466(5) Uani 1 1 d . . . H8A H 0.5947 0.8267 -0.0114 0.056 Uiso 1 1 calc R . . B8B B -0.06099(16) -0.03593(9) -0.31869(17) 0.0448(5) Uani 1 1 d . . . H8B H -0.1324 -0.0326 -0.3701 0.054 Uiso 1 1 calc R . . B9A B 0.42151(18) 0.84551(10) 0.0316(2) 0.0524(6) Uani 1 1 d . . . H9A H 0.3712 0.8697 -0.0242 0.063 Uiso 1 1 calc R . . B9B B 0.06097(16) -0.04482(9) -0.33918(16) 0.0428(5) Uani 1 1 d . . . H9B H 0.0874 -0.0487 -0.4065 0.051 Uiso 1 1 calc R . . B10A B 0.51980(19) 0.87707(10) 0.0987(2) 0.0568(6) Uani 1 1 d . . . H10A H 0.5446 0.9202 0.0968 0.068 Uiso 1 1 calc R . . B10B B -0.00391(17) -0.09701(9) -0.30695(18) 0.0488(5) Uani 1 1 d . . . H10B H -0.0262 -0.1368 -0.3432 0.059 Uiso 1 1 calc R . . H3 H 0.2550(17) 0.5182(9) 0.1211(15) 0.050(6) Uiso 1 1 d . . . H4 H 0.2490(18) 0.2447(10) -0.0471(17) 0.062(7) 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 O1 0.0548(9) 0.0533(9) 0.1220(15) -0.0331(9) 0.0457(10) -0.0162(7) O2 0.0391(7) 0.0444(8) 0.0620(9) -0.0073(6) 0.0159(6) -0.0051(6) N1 0.0413(9) 0.0410(9) 0.0536(10) -0.0112(7) 0.0171(7) -0.0091(7) N2 0.0406(9) 0.0372(8) 0.0573(10) -0.0010(7) 0.0201(8) -0.0033(6) N3 0.0337(8) 0.0418(9) 0.0460(9) -0.0032(7) 0.0089(6) -0.0035(6) N4 0.0392(8) 0.0549(10) 0.0458(9) -0.0058(7) 0.0040(7) 0.0038(7) C1A 0.0391(10) 0.0407(10) 0.0442(10) -0.0002(8) 0.0143(8) -0.0029(7) C1B 0.0336(9) 0.0362(9) 0.0397(9) -0.0028(7) 0.0101(7) -0.0012(7) C2A 0.0372(9) 0.0390(10) 0.0459(10) 0.0024(8) 0.0126(8) -0.0009(7) C2B 0.0326(8) 0.0386(9) 0.0405(9) -0.0033(7) 0.0084(7) -0.0013(7) C3A 0.0456(10) 0.0455(11) 0.0483(11) 0.0000(8) 0.0208(8) -0.0038(8) C3B 0.0368(9) 0.0396(9) 0.0417(9) -0.0013(7) 0.0123(7) -0.0025(7) C4A 0.0465(10) 0.0434(10) 0.0471(10) -0.0028(8) 0.0185(8) -0.0009(8) C4B 0.0398(9) 0.0413(10) 0.0385(9) -0.0042(7) 0.0114(7) -0.0008(7) C5A 0.0384(9) 0.0361(9) 0.0492(10) 0.0014(8) 0.0130(8) -0.0003(7) C5B 0.0341(9) 0.0388(10) 0.0452(10) -0.0076(8) 0.0084(7) -0.0032(7) C6 0.0389(10) 0.0413(10) 0.0376(9) -0.0031(7) 0.0110(7) -0.0032(7) C6A 0.0392(10) 0.0426(10) 0.0515(11) 0.0023(8) 0.0199(8) 0.0018(8) C6B 0.0441(10) 0.0474(11) 0.0544(11) -0.0086(9) 0.0215(9) -0.0118(8) C7 0.0399(9) 0.0386(9) 0.0326(8) -0.0025(7) 0.0097(7) -0.0037(7) C7A 0.0417(10) 0.0399(10) 0.0505(11) 0.0000(8) 0.0185(8) 0.0034(8) C7B 0.0456(10) 0.0479(11) 0.0497(11) -0.0114(9) 0.0212(9) -0.0100(8) C8 0.0403(10) 0.0386(10) 0.0475(10) -0.0045(8) 0.0110(8) 0.0016(7) C9 0.0356(9) 0.0447(10) 0.0544(11) -0.0090(9) 0.0117(8) -0.0036(8) C10 0.0408(10) 0.0405(10) 0.0393(9) -0.0062(7) 0.0110(7) -0.0042(7) C11 0.0419(10) 0.0405(10) 0.0489(11) -0.0059(8) 0.0099(8) 0.0010(8) C12 0.0368(9) 0.0436(10) 0.0468(10) -0.0065(8) 0.0078(8) -0.0017(7) C13 0.0393(10) 0.0409(10) 0.0542(11) -0.0089(8) 0.0136(8) -0.0043(8) C14 0.0511(12) 0.0576(13) 0.0492(11) -0.0045(10) -0.0017(9) 0.0020(10) C15 0.0609(15) 0.0716(16) 0.0724(16) 0.0141(13) -0.0048(12) 0.0060(12) C16 0.0391(11) 0.0869(18) 0.0679(15) -0.0195(13) 0.0137(10) -0.0018(11) C17 0.0474(13) 0.154(3) 0.0639(15) -0.0331(17) 0.0196(12) -0.0137(16) C18 0.0398(10) 0.0627(13) 0.0514(12) -0.0068(10) 0.0057(9) -0.0006(9) C19 0.0487(12) 0.0800(16) 0.0536(12) 0.0017(11) 0.0130(10) 0.0082(11) C20 0.0660(14) 0.0579(14) 0.0554(13) 0.0056(10) -0.0015(11) 0.0034(11) C21 0.097(2) 0.0694(18) 0.0779(18) 0.0175(14) -0.0097(15) -0.0200(15) C22 0.0434(10) 0.0431(11) 0.0634(12) 0.0012(9) 0.0185(9) -0.0052(8) C23 0.0687(15) 0.0680(16) 0.0690(15) 0.0180(12) 0.0205(12) -0.0002(12) C24 0.0411(10) 0.0465(11) 0.0464(10) -0.0049(8) 0.0066(8) -0.0085(8) C25 0.0573(12) 0.0418(11) 0.0499(11) -0.0027(8) 0.0157(9) -0.0044(9) C26 0.0406(10) 0.0538(12) 0.0471(11) -0.0056(9) 0.0031(8) 0.0013(8) C27 0.0633(14) 0.0605(13) 0.0500(12) 0.0030(10) 0.0153(10) 0.0116(11) C28 0.0387(10) 0.0474(11) 0.0634(13) -0.0022(9) 0.0163(9) 0.0012(8) C29 0.0598(14) 0.0600(15) 0.107(2) -0.0283(14) 0.0338(14) -0.0021(11) B2A 0.0397(11) 0.0422(12) 0.0539(13) -0.0008(9) 0.0163(9) -0.0030(9) B2B 0.0366(10) 0.0377(10) 0.0431(11) -0.0003(8) 0.0111(8) 0.0017(8) B3A 0.0423(12) 0.0527(13) 0.0467(12) -0.0036(10) 0.0157(9) -0.0072(10) B3B 0.0374(11) 0.0425(11) 0.0439(11) 0.0029(9) 0.0105(9) -0.0016(8) B4A 0.0381(11) 0.0469(12) 0.0458(11) -0.0009(9) 0.0123(9) -0.0037(9) B4B 0.0335(10) 0.0373(11) 0.0498(12) -0.0032(9) 0.0107(8) -0.0009(8) B5A 0.0413(11) 0.0430(11) 0.0449(11) 0.0022(9) 0.0131(9) -0.0038(9) B5B 0.0390(10) 0.0361(10) 0.0419(11) -0.0031(8) 0.0078(8) 0.0017(8) B6A 0.0503(13) 0.0465(13) 0.0683(15) -0.0119(11) 0.0247(11) -0.0077(10) B6B 0.0421(11) 0.0360(11) 0.0556(13) 0.0026(9) 0.0151(10) 0.0014(8) B7A 0.0439(12) 0.0582(14) 0.0535(13) -0.0111(11) 0.0185(10) -0.0117(10) B7B 0.0409(11) 0.0365(11) 0.0603(13) 0.0001(9) 0.0145(10) -0.0041(9) B8A 0.0443(12) 0.0456(12) 0.0524(13) 0.0007(10) 0.0159(10) -0.0071(9) B8B 0.0377(11) 0.0426(12) 0.0520(12) -0.0078(9) 0.0059(9) -0.0012(9) B9A 0.0493(13) 0.0430(12) 0.0679(15) 0.0041(11) 0.0197(11) -0.0014(10) B9B 0.0450(11) 0.0376(11) 0.0460(12) -0.0054(9) 0.0105(9) 0.0005(9) B10A 0.0563(14) 0.0440(13) 0.0759(17) -0.0061(12) 0.0274(13) -0.0100(10) B10B 0.0463(12) 0.0380(11) 0.0625(14) -0.0085(10) 0.0127(10) -0.0030(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 O1 C13 1.216(2) . ? O2 C6 1.220(2) . ? N1 C13 1.346(2) . ? N1 C5B 1.423(2) . ? N2 C6 1.364(2) . ? N2 C5A 1.422(2) . ? N3 C26 1.514(2) . ? N3 C24 1.520(2) . ? N3 C22 1.520(2) . ? N3 C28 1.525(2) . ? N4 C20 1.513(3) . ? N4 C16 1.514(3) . ? N4 C14 1.517(3) . ? N4 C18 1.520(3) . ? C1A C2A 1.486(3) . ? C1A B3A 1.612(3) . ? C1A B2A 1.613(3) . ? C1A B4A 1.612(3) . ? C1A B5A 1.616(3) . ? C1B C2B 1.487(2) . ? C1B B4B 1.608(3) . ? C1B B2B 1.612(3) . ? C1B B5B 1.612(3) . ? C1B B3B 1.615(3) . ? C2A C7A 1.390(3) . ? C2A C3A 1.394(3) . ? C2B C3B 1.390(2) . ? C2B C7B 1.396(3) . ? C3A C4A 1.385(3) . ? C3B C4B 1.390(3) . ? C4A C5A 1.392(3) . ? C4B C5B 1.392(3) . ? C5A C6A 1.392(3) . ? C5B C6B 1.385(3) . ? C6 C7 1.498(2) . ? C6A C7A 1.384(3) . ? C6B C7B 1.377(3) . ? C7 C8 1.387(3) . ? C7 C12 1.393(3) . ? C8 C9 1.381(3) . ? C9 C10 1.390(3) . ? C10 C11 1.396(3) . ? C10 C13 1.497(3) . ? C11 C12 1.379(3) . ? C14 C15 1.509(3) . ? C16 C17 1.526(4) . ? C18 C19 1.510(3) . ? C20 C21 1.515(4) . ? C22 C23 1.503(3) . ? C24 C25 1.508(3) . ? C26 C27 1.512(3) . ? C28 C29 1.514(3) . ? B2A B6A 1.800(3) . ? B2A B9A 1.809(3) . ? B2A B3A 1.837(3) . ? B2A B5A 1.841(3) . ? B2B B6B 1.802(3) . ? B2B B9B 1.806(3) . ? B2B B5B 1.838(3) . ? B2B B3B 1.846(3) . ? B3A B7A 1.809(3) . ? B3A B6A 1.817(4) . ? B3A B4A 1.845(3) . ? B3B B7B 1.802(3) . ? B3B B6B 1.814(3) . ? B3B B4B 1.829(3) . ? B4A B8A 1.802(3) . ? B4A B7A 1.808(3) . ? B4A B5A 1.840(3) . ? B4B B7B 1.804(3) . ? B4B B8B 1.811(3) . ? B4B B5B 1.845(3) . ? B5A B8A 1.803(3) . ? B5A B9A 1.805(3) . ? B5B B8B 1.800(3) . ? B5B B9B 1.809(3) . ? B6A B10A 1.699(3) . ? B6A B7A 1.835(3) . ? B6A B9A 1.842(4) . ? B6B B10B 1.699(3) . ? B6B B9B 1.836(3) . ? B6B B7B 1.843(3) . ? B7A B10A 1.701(4) . ? B7A B8A 1.838(3) . ? B7B B10B 1.698(3) . ? B7B B8B 1.838(3) . ? B8A B10A 1.698(3) . ? B8A B9A 1.844(3) . ? B8B B10B 1.698(3) . ? B8B B9B 1.840(3) . ? B9A B10A 1.701(4) . ? B9B B10B 1.705(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 C13 N1 C5B 127.58(16) . . ? C6 N2 C5A 125.12(16) . . ? C26 N3 C24 110.91(15) . . ? C26 N3 C22 106.02(14) . . ? C24 N3 C22 111.68(15) . . ? C26 N3 C28 111.31(15) . . ? C24 N3 C28 106.13(14) . . ? C22 N3 C28 110.87(15) . . ? C20 N4 C16 111.82(19) . . ? C20 N4 C14 108.65(16) . . ? C16 N4 C14 108.90(16) . . ? C20 N4 C18 108.40(16) . . ? C16 N4 C18 108.16(16) . . ? C14 N4 C18 110.93(17) . . ? C2A C1A B3A 126.72(17) . . ? C2A C1A B2A 126.24(16) . . ? B3A C1A B2A 69.45(14) . . ? C2A C1A B4A 126.37(16) . . ? B3A C1A B4A 69.82(13) . . ? B2A C1A B4A 107.39(15) . . ? C2A C1A B5A 125.50(16) . . ? B3A C1A B5A 107.78(16) . . ? B2A C1A B5A 69.54(14) . . ? B4A C1A B5A 69.50(13) . . ? C2B C1B B4B 127.68(15) . . ? C2B C1B B2B 124.65(15) . . ? B4B C1B B2B 107.64(14) . . ? C2B C1B B5B 124.45(15) . . ? B4B C1B B5B 69.93(13) . . ? B2B C1B B5B 69.51(12) . . ? C2B C1B B3B 127.93(16) . . ? B4B C1B B3B 69.14(13) . . ? B2B C1B B3B 69.79(13) . . ? B5B C1B B3B 107.60(15) . . ? C7A C2A C3A 118.03(17) . . ? C7A C2A C1A 121.55(17) . . ? C3A C2A C1A 120.42(16) . . ? C3B C2B C7B 117.74(17) . . ? C3B C2B C1B 122.55(16) . . ? C7B C2B C1B 119.71(16) . . ? C4A C3A C2A 121.69(17) . . ? C4B C3B C2B 121.59(16) . . ? C5A C4A C3A 119.32(17) . . ? C3B C4B C5B 119.46(16) . . ? C4A C5A C6A 119.82(17) . . ? C4A C5A N2 121.38(17) . . ? C6A C5A N2 118.77(16) . . ? C6B C5B C4B 119.50(17) . . ? C6B C5B N1 116.85(16) . . ? C4B C5B N1 123.61(17) . . ? O2 C6 N2 122.52(17) . . ? O2 C6 C7 120.92(16) . . ? N2 C6 C7 116.54(16) . . ? C7A C6A C5A 119.96(17) . . ? C7B C6B C5B 120.49(17) . . ? C8 C7 C12 119.33(17) . . ? C8 C7 C6 123.63(17) . . ? C12 C7 C6 116.93(16) . . ? C6A C7A C2A 121.17(17) . . ? C6B C7B C2B 121.22(17) . . ? C9 C8 C7 120.06(17) . . ? C8 C9 C10 120.64(17) . . ? C9 C10 C11 119.37(17) . . ? C9 C10 C13 117.79(16) . . ? C11 C10 C13 122.83(17) . . ? C12 C11 C10 119.72(17) . . ? C11 C12 C7 120.78(17) . . ? O1 C13 N1 123.13(18) . . ? O1 C13 C10 121.83(17) . . ? N1 C13 C10 114.99(16) . . ? C15 C14 N4 115.25(19) . . ? N4 C16 C17 114.6(2) . . ? C19 C18 N4 115.65(18) . . ? N4 C20 C21 115.2(2) . . ? C23 C22 N3 115.16(17) . . ? C25 C24 N3 115.72(15) . . ? C27 C26 N3 115.12(17) . . ? C29 C28 N3 114.18(17) . . ? C1A B2A B6A 109.25(17) . . ? C1A B2A B9A 109.01(15) . . ? B6A B2A B9A 61.37(14) . . ? C1A B2A B3A 55.27(12) . . ? B6A B2A B3A 59.93(14) . . ? B9A B2A B3A 102.90(15) . . ? C1A B2A B5A 55.32(12) . . ? B6A B2A B5A 102.26(15) . . ? B9A B2A B5A 59.28(12) . . ? B3A B2A B5A 90.32(14) . . ? C1B B2B B6B 109.04(14) . . ? C1B B2B B9B 109.08(15) . . ? B6B B2B B9B 61.18(12) . . ? C1B B2B B5B 55.24(11) . . ? B6B B2B B5B 102.22(14) . . ? B9B B2B B5B 59.54(11) . . ? C1B B2B B3B 55.18(11) . . ? B6B B2B B3B 59.62(12) . . ? B9B B2B B3B 102.37(14) . . ? B5B B2B B3B 89.95(13) . . ? C1A B3A B7A 108.52(16) . . ? C1A B3A B6A 108.47(17) . . ? B7A B3A B6A 60.80(13) . . ? C1A B3A B2A 55.29(12) . . ? B7A B3A B2A 101.59(16) . . ? B6A B3A B2A 59.04(13) . . ? C1A B3A B4A 55.10(12) . . ? B7A B3A B4A 59.28(12) . . ? B6A B3A B4A 101.68(16) . . ? B2A B3A B4A 89.79(14) . . ? C1B B3B B7B 108.85(15) . . ? C1B B3B B6B 108.34(15) . . ? B7B B3B B6B 61.30(12) . . ? C1B B3B B4B 55.27(11) . . ? B7B B3B B4B 59.57(12) . . ? B6B B3B B4B 102.30(15) . . ? C1B B3B B2B 55.03(11) . . ? B7B B3B B2B 101.98(15) . . ? B6B B3B B2B 58.99(12) . . ? B4B B3B B2B 90.04(13) . . ? C1A B4A B8A 108.88(16) . . ? C1A B4A B7A 108.58(16) . . ? B8A B4A B7A 61.21(13) . . ? C1A B4A B5A 55.33(11) . . ? B8A B4A B5A 59.32(12) . . ? B7A B4A B5A 101.94(16) . . ? C1A B4A B3A 55.08(12) . . ? B8A B4A B3A 102.37(16) . . ? B7A B4A B3A 59.36(12) . . ? B5A B4A B3A 90.08(14) . . ? C1B B4B B7B 109.04(15) . . ? C1B B4B B8B 108.37(15) . . ? B7B B4B B8B 61.10(13) . . ? C1B B4B B3B 55.59(11) . . ? B7B B4B B3B 59.47(12) . . ? B8B B4B B3B 102.11(14) . . ? C1B B4B B5B 55.11(11) . . ? B7B B4B B5B 101.96(14) . . ? B8B B4B B5B 58.96(12) . . ? B3B B4B B5B 90.24(13) . . ? C1A B5A B8A 108.69(16) . . ? C1A B5A B9A 109.03(16) . . ? B8A B5A B9A 61.48(13) . . ? C1A B5A B4A 55.16(12) . . ? B8A B5A B4A 59.28(12) . . ? B9A B5A B4A 102.48(16) . . ? C1A B5A B2A 55.15(12) . . ? B8A B5A B2A 102.04(15) . . ? B9A B5A B2A 59.46(13) . . ? B4A B5A B2A 89.82(14) . . ? C1B B5B B8B 108.79(15) . . ? C1B B5B B9B 108.92(15) . . ? B8B B5B B9B 61.31(12) . . ? C1B B5B B2B 55.25(11) . . ? B8B B5B B2B 102.06(14) . . ? B9B B5B B2B 59.36(11) . . ? C1B B5B B4B 54.95(11) . . ? B8B B5B B4B 59.58(12) . . ? B9B B5B B4B 102.37(14) . . ? B2B B5B B4B 89.77(13) . . ? B10A B6A B2A 112.08(18) . . ? B10A B6A B3A 112.19(17) . . ? B2A B6A B3A 61.03(13) . . ? B10A B6A B7A 57.36(15) . . ? B2A B6A B7A 102.00(16) . . ? B3A B6A B7A 59.39(13) . . ? B10A B6A B9A 57.24(15) . . ? B2A B6A B9A 59.53(13) . . ? B3A B6A B9A 102.37(16) . . ? B7A B6A B9A 90.19(15) . . ? B10B B6B B2B 112.28(16) . . ? B10B B6B B3B 111.74(16) . . ? B2B B6B B3B 61.40(12) . . ? B10B B6B B9B 57.52(13) . . ? B2B B6B B9B 59.52(12) . . ? B3B B6B B9B 102.46(14) . . ? B10B B6B B7B 57.10(13) . . ? B2B B6B B7B 102.09(14) . . ? B3B B6B B7B 59.04(12) . . ? B9B B6B B7B 90.23(14) . . ? B10A B7A B4A 111.98(18) . . ? B10A B7A B3A 112.52(18) . . ? B4A B7A B3A 61.35(13) . . ? B10A B7A B6A 57.30(14) . . ? B4A B7A B6A 102.44(15) . . ? B3A B7A B6A 59.81(13) . . ? B10A B7A B8A 57.21(14) . . ? B4A B7A B8A 59.24(12) . . ? B3A B7A B8A 102.38(16) . . ? B6A B7A B8A 90.10(16) . . ? B10B B7B B3B 112.35(16) . . ? B10B B7B B4B 112.39(17) . . ? B3B B7B B4B 60.95(12) . . ? B10B B7B B8B 57.23(13) . . ? B3B B7B B8B 102.13(14) . . ? B4B B7B B8B 59.65(12) . . ? B10B B7B B6B 57.16(13) . . ? B3B B7B B6B 59.66(12) . . ? B4B B7B B6B 102.11(14) . . ? B8B B7B B6B 89.66(14) . . ? B10A B8A B4A 112.39(17) . . ? B10A B8A B5A 112.03(17) . . ? B4A B8A B5A 61.40(12) . . ? B10A B8A B7A 57.33(15) . . ? B4A B8A B7A 59.56(13) . . ? B5A B8A B7A 102.24(15) . . ? B10A B8A B9A 57.21(14) . . ? B4A B8A B9A 102.44(15) . . ? B5A B8A B9A 59.32(13) . . ? B7A B8A B9A 90.03(15) . . ? B10B B8B B5B 112.44(16) . . ? B10B B8B B4B 112.02(17) . . ? B5B B8B B4B 61.46(12) . . ? B10B B8B B9B 57.45(12) . . ? B5B B8B B9B 59.60(12) . . ? B4B B8B B9B 102.49(14) . . ? B10B B8B B7B 57.24(13) . . ? B5B B8B B7B 102.43(15) . . ? B4B B8B B7B 59.25(12) . . ? B9B B8B B7B 90.28(14) . . ? B10A B9A B5A 111.78(18) . . ? B10A B9A B2A 111.61(19) . . ? B5A B9A B2A 61.25(12) . . ? B10A B9A B6A 57.16(14) . . ? B5A B9A B6A 102.04(17) . . ? B2A B9A B6A 59.10(13) . . ? B10A B9A B8A 57.07(14) . . ? B5A B9A B8A 59.19(12) . . ? B2A B9A B8A 101.69(16) . . ? B6A B9A B8A 89.68(16) . . ? B10B B9B B2B 111.78(16) . . ? B10B B9B B5B 111.63(16) . . ? B2B B9B B5B 61.11(12) . . ? B10B B9B B8B 57.07(13) . . ? B2B B9B B8B 101.73(14) . . ? B5B B9B B8B 59.09(12) . . ? B10B B9B B6B 57.20(13) . . ? B2B B9B B6B 59.30(12) . . ? B5B B9B B6B 102.01(14) . . ? B8B B9B B6B 89.82(14) . . ? B9A B10A B6A 65.60(15) . . ? B9A B10A B8A 65.72(15) . . ? B6A B10A B8A 99.82(17) . . ? B9A B10A B7A 99.93(17) . . ? B6A B10A B7A 65.33(15) . . ? B8A B10A B7A 65.46(15) . . ? B7B B10B B8B 65.53(14) . . ? B7B B10B B6B 65.74(14) . . ? B8B B10B B6B 99.65(16) . . ? B7B B10B B9B 100.02(16) . . ? B8B B10B B9B 65.47(13) . . ? B6B B10B B9B 65.28(13) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.086 _refine_diff_density_min -0.281 _refine_diff_density_rms 0.097