# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2003 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Steve Westcott' 'Mark O. Baerlocher' 'Felix J. Baerlocher' 'Andreas Decken' 'Janet P. Edwards' 'Michael G. Hamilton' 'Xiao-Feng He' 'Alison M. Irving' 'Liliya G. Nikolcheva' 'Christopher M. Vogels' _publ_contact_author_name 'Dr Steve Westcott' _publ_contact_author_address ; Department of Chemistry Mount Allison University 63C York Street Sackville New Brunswick E4L 1G8 CANADA ; _publ_contact_author_email SWESTCOTT@MTA.CA _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Cyclic diamines containing boronate esters ; data_sw_a _database_code_CSD 212668 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H138 B4 N16 O9' _chemical_formula_weight 1703.46 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 P2(1)/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 19.5646(9) _cell_length_b 16.3302(8) _cell_length_c 31.1144(16) _cell_angle_alpha 90.00 _cell_angle_beta 107.5480(10) _cell_angle_gamma 90.00 _cell_volume 9478.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Parallelepip _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.194 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3672 _exptl_absorpt_coefficient_mu 0.077 _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 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 66879 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 27.50 _reflns_number_total 21464 _reflns_number_gt 12175 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1009P)^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 21464 _refine_ls_number_parameters 1667 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1170 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1817 _refine_ls_wR_factor_gt 0.1563 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 B1 B 0.64765(12) 0.75025(15) 0.11165(8) 0.0364(5) Uani 1 1 d . . . O2 O 0.70236(8) 0.81091(9) 0.11040(5) 0.0447(4) Uani 1 1 d . . . C3 C 0.73293(13) 0.78524(17) 0.07583(8) 0.0545(7) Uani 1 1 d . . . C4 C 0.72706(12) 0.69099(16) 0.07767(8) 0.0503(6) Uani 1 1 d . . . O5 O 0.65830(7) 0.68161(9) 0.08519(5) 0.0387(3) Uani 1 1 d . . . C6 C 0.68754(18) 0.8197(2) 0.03062(9) 0.0637(8) Uani 1 1 d . . . C7 C 0.80838(18) 0.8197(3) 0.08685(13) 0.0871(12) Uani 1 1 d . . . C8 C 0.78456(15) 0.6521(3) 0.11687(11) 0.0725(9) Uani 1 1 d . . . C9 C 0.72577(17) 0.6466(2) 0.03446(10) 0.0613(7) Uani 1 1 d . . . C10 C 0.56706(10) 0.78272(12) 0.10158(7) 0.0341(4) Uani 1 1 d . . . C11 C 0.51869(12) 0.80847(14) 0.06112(8) 0.0428(5) Uani 1 1 d . . . C12 C 0.45025(13) 0.83377(15) 0.05930(9) 0.0499(6) Uani 1 1 d . . . C13 C 0.42901(13) 0.83347(15) 0.09802(9) 0.0498(6) Uani 1 1 d . . . C14 C 0.47617(11) 0.80920(13) 0.13883(8) 0.0416(5) Uani 1 1 d . . . C15 C 0.54460(10) 0.78443(12) 0.13992(7) 0.0334(4) Uani 1 1 d . . . C16 C 0.60148(10) 0.75983(12) 0.18248(7) 0.0314(4) Uani 1 1 d . . . N17 N 0.57889(9) 0.69711(10) 0.20823(6) 0.0351(4) Uani 1 1 d . . . C18 C 0.58967(12) 0.62147(13) 0.18541(8) 0.0425(5) Uani 1 1 d . . . C19 C 0.66064(13) 0.63355(14) 0.17547(9) 0.0434(5) Uani 1 1 d . . . N20 N 0.66200(9) 0.72399(11) 0.16621(6) 0.0349(4) Uani 1 1 d . . . C21 C 0.62167(11) 0.69575(14) 0.25607(7) 0.0407(5) Uani 1 1 d . . . C22 C 0.60006(13) 0.76307(15) 0.28285(8) 0.0448(5) Uani 1 1 d . . . N23 N 0.63954(10) 0.75234(13) 0.33039(6) 0.0537(5) Uani 1 1 d . A . C24 C 0.60527(16) 0.73576(16) 0.35652(9) 0.0566(7) Uani 1 1 d . . . C25 C 0.6475(3) 0.7191(4) 0.4059(2) 0.0511(13) Uani 0.75 1 d P A . C26 C 0.7193(2) 0.7327(3) 0.42385(13) 0.0596(10) Uani 0.75 1 d P . . C27 C 0.7516(3) 0.7168(3) 0.46887(14) 0.0740(12) Uani 0.75 1 d P A . C28 C 0.7088(3) 0.6872(2) 0.49284(18) 0.1095(15) Uani 1 1 d . . . C29 C 0.6364(3) 0.6798(4) 0.4769(2) 0.0738(17) Uani 0.75 1 d P A . N30 N 0.6058(2) 0.6926(2) 0.43028(12) 0.0687(9) Uani 0.75 1 d P . . C25A C 0.6115(8) 0.7239(10) 0.4013(5) 0.045(3) Uani 0.25 1 d P A 1 C26A C 0.6757(10) 0.6894(11) 0.4236(5) 0.077(5) Uani 0.25 1 d P A 1 C27A C 0.6746(15) 0.6649(10) 0.4675(5) 0.099(8) Uani 0.25 1 d P A 1 C29A C 0.5748(8) 0.7154(8) 0.4653(4) 0.073(4) Uani 0.25 1 d P A 1 N30A N 0.5584(5) 0.7337(6) 0.4207(3) 0.053(2) Uani 0.25 1 d P A 1 H6A H 0.6376(13) 0.7905(15) 0.0185(8) 0.059(7) Uiso 1 1 d . . . H6B H 0.6783(18) 0.882(2) 0.0292(11) 0.106(11) Uiso 1 1 d . . . H6C H 0.7118(15) 0.8113(17) 0.0060(11) 0.084(9) Uiso 1 1 d . . . H7A H 0.8350(15) 0.8008(18) 0.1168(11) 0.072(10) Uiso 1 1 d . . . H7B H 0.8323(16) 0.7971(18) 0.0649(11) 0.089(9) Uiso 1 1 d . . . H7C H 0.813(3) 0.886(3) 0.0923(17) 0.18(2) Uiso 1 1 d . . . H8A H 0.7923(14) 0.6835(18) 0.1457(10) 0.077(9) Uiso 1 1 d . . . H8B H 0.7700(18) 0.587(2) 0.1242(12) 0.109(12) Uiso 1 1 d . . . H8C H 0.8302(16) 0.6545(17) 0.1115(9) 0.074(8) Uiso 1 1 d . . . H9A H 0.6846(13) 0.6647(14) 0.0088(9) 0.053(7) Uiso 1 1 d . . . H9B H 0.7687(15) 0.6601(17) 0.0257(9) 0.077(9) Uiso 1 1 d . . . H9C H 0.7248(16) 0.578(2) 0.0371(10) 0.099(10) Uiso 1 1 d . . . H11 H 0.5335(12) 0.8105(15) 0.0342(9) 0.059(7) Uiso 1 1 d . . . H12 H 0.4185(12) 0.8485(14) 0.0297(8) 0.053(7) Uiso 1 1 d . . . H13 H 0.3835(12) 0.8457(13) 0.0963(7) 0.044(6) Uiso 1 1 d . . . H14 H 0.4624(12) 0.8073(13) 0.1670(8) 0.049(6) Uiso 1 1 d . . . H16 H 0.6185(9) 0.8076(11) 0.2007(6) 0.021(5) Uiso 1 1 d . . . H20 H 0.7028(13) 0.7485(15) 0.1846(8) 0.054(7) Uiso 1 1 d . . . H19A H 0.7028(12) 0.6165(14) 0.2034(8) 0.051(6) Uiso 1 1 d . . . H19B H 0.6629(11) 0.6045(14) 0.1499(8) 0.047(6) Uiso 1 1 d . . . H18A H 0.5470(11) 0.6157(12) 0.1543(7) 0.036(5) Uiso 1 1 d . . . H18B H 0.5911(11) 0.5737(14) 0.2041(7) 0.039(6) Uiso 1 1 d . . . H21A H 0.6126(11) 0.6410(14) 0.2703(7) 0.046(6) Uiso 1 1 d . . . H21B H 0.6764(11) 0.6977(12) 0.2611(7) 0.040(6) Uiso 1 1 d . . . H22A H 0.5449(12) 0.7606(13) 0.2769(7) 0.046(6) Uiso 1 1 d . . . H22B H 0.6128(12) 0.8155(15) 0.2732(8) 0.054(7) Uiso 1 1 d . . . H24 H 0.5535(15) 0.7369(16) 0.3481(9) 0.069(8) Uiso 1 1 d . . . H26 H 0.7445(15) 0.7549(18) 0.4053(10) 0.079(9) Uiso 1 1 d . . . H27 H 0.797(3) 0.736(3) 0.4774(16) 0.17(2) Uiso 1 1 d . . . H28 H 0.7228(19) 0.667(2) 0.5322(13) 0.122(12) Uiso 1 1 d . . . H29 H 0.6111(19) 0.670(2) 0.4928(12) 0.088(12) Uiso 1 1 d . . . B2 B 0.76276(11) -0.08280(14) 0.23102(8) 0.0312(5) Uani 1 1 d . . . O32 O 0.76449(6) -0.17241(8) 0.23274(5) 0.0343(3) Uani 1 1 d . . . C33 C 0.83071(10) -0.19580(12) 0.26608(7) 0.0357(5) Uani 1 1 d . . . C34 C 0.88144(10) -0.12428(12) 0.26254(7) 0.0351(4) Uani 1 1 d . . . O35 O 0.83389(6) -0.05496(8) 0.25459(4) 0.0335(3) Uani 1 1 d . . . C36 C 0.81858(13) -0.19910(16) 0.31222(8) 0.0433(5) Uani 1 1 d . . . C37 C 0.85367(13) -0.27917(14) 0.25406(10) 0.0480(6) Uani 1 1 d . . . C38 C 0.94287(12) -0.10968(16) 0.30535(8) 0.0433(5) Uani 1 1 d . . . C39 C 0.91062(12) -0.13434(16) 0.22257(9) 0.0433(5) Uani 1 1 d . . . C40 C 0.69772(10) -0.03806(12) 0.24306(7) 0.0334(4) Uani 1 1 d . . . C41 C 0.68709(11) -0.02482(13) 0.28494(8) 0.0385(5) Uani 1 1 d . . . C42 C 0.62445(11) 0.01150(14) 0.28783(9) 0.0431(5) Uani 1 1 d . . . C43 C 0.57136(11) 0.03458(13) 0.24916(9) 0.0444(5) Uani 1 1 d . . . C44 C 0.58071(11) 0.02265(13) 0.20752(9) 0.0423(5) Uani 1 1 d . . . C45 C 0.64388(10) -0.01301(12) 0.20489(7) 0.0338(4) Uani 1 1 d . . . C46 C 0.66029(10) -0.02690(13) 0.16128(7) 0.0372(5) Uani 1 1 d . . . N47 N 0.65832(9) 0.04768(11) 0.13533(6) 0.0421(4) Uani 1 1 d . . . C48 C 0.72985(13) 0.08241(15) 0.15642(9) 0.0464(6) Uani 1 1 d . . . C49 C 0.78036(12) 0.00979(14) 0.16297(8) 0.0424(5) Uani 1 1 d . . . N50 N 0.73819(8) -0.05803(11) 0.17530(6) 0.0338(4) Uani 1 1 d . . . C51 C 0.64308(15) 0.03226(19) 0.08680(8) 0.0556(6) Uani 1 1 d . . . C52 C 0.56342(16) 0.03745(18) 0.06262(10) 0.0639(7) Uani 1 1 d . . . N53 N 0.53988(12) 0.12276(14) 0.05956(7) 0.0596(6) Uani 1 1 d . . . C54 C 0.50003(14) 0.14430(17) 0.08292(9) 0.0558(7) Uani 1 1 d . . . C55 C 0.47280(12) 0.22839(16) 0.08249(8) 0.0540(6) Uani 1 1 d . . . C56 C 0.49186(17) 0.29039(19) 0.05820(11) 0.0693(8) Uani 1 1 d . . . C57 C 0.46232(19) 0.3664(2) 0.05839(13) 0.0837(10) Uani 1 1 d . . . C58 C 0.41456(15) 0.37888(19) 0.08233(11) 0.0714(8) Uani 1 1 d . . . C59 C 0.39893(16) 0.31469(19) 0.10545(10) 0.0677(8) Uani 1 1 d . . . N60 N 0.42686(11) 0.23950(14) 0.10587(8) 0.0634(6) Uani 1 1 d . . . H36A H 0.8623(13) -0.2244(15) 0.3369(8) 0.058(7) Uiso 1 1 d . . . H36B H 0.8102(11) -0.1445(14) 0.3234(7) 0.041(6) Uiso 1 1 d . . . H36C H 0.7752(12) -0.2347(14) 0.3117(7) 0.050(6) Uiso 1 1 d . . . H37A H 0.9018(15) -0.2960(17) 0.2758(10) 0.077(8) Uiso 1 1 d . . . H37B H 0.8160(12) -0.3204(14) 0.2555(7) 0.045(6) Uiso 1 1 d . . . H37C H 0.8568(13) -0.2804(16) 0.2224(9) 0.064(8) Uiso 1 1 d . . . H38A H 0.9729(11) -0.0651(14) 0.3000(7) 0.045(6) Uiso 1 1 d . . . H38B H 0.9712(13) -0.1644(16) 0.3136(8) 0.062(7) Uiso 1 1 d . . . H38C H 0.9228(11) -0.0918(13) 0.3312(7) 0.042(6) Uiso 1 1 d . . . H39A H 0.9497(12) -0.1807(14) 0.2291(7) 0.049(6) Uiso 1 1 d . . . H39B H 0.8727(12) -0.1482(13) 0.1932(8) 0.046(6) Uiso 1 1 d . . . H39C H 0.9302(13) -0.0840(17) 0.2164(8) 0.062(8) Uiso 1 1 d . . . H41 H 0.7234(11) -0.0420(12) 0.3140(7) 0.037(5) Uiso 1 1 d . . . H42 H 0.6181(11) 0.0213(14) 0.3172(8) 0.047(6) Uiso 1 1 d . . . H43 H 0.5269(12) 0.0647(14) 0.2529(7) 0.050(6) Uiso 1 1 d . . . H44 H 0.5440(13) 0.0387(14) 0.1794(9) 0.058(7) Uiso 1 1 d . . . H46 H 0.6301(10) -0.0721(12) 0.1429(6) 0.030(5) Uiso 1 1 d . . . H50 H 0.7393(11) -0.1016(14) 0.1586(7) 0.042(6) Uiso 1 1 d . . . H49A H 0.7939(12) -0.0054(15) 0.1355(9) 0.058(7) Uiso 1 1 d . . . H49B H 0.8231(13) 0.0164(14) 0.1863(8) 0.051(7) Uiso 1 1 d . . . H48A H 0.7411(11) 0.1244(14) 0.1380(8) 0.045(6) Uiso 1 1 d . . . H48B H 0.7309(11) 0.1048(13) 0.1866(8) 0.039(6) Uiso 1 1 d . . . H51A H 0.6705(12) 0.0716(16) 0.0743(8) 0.057(7) Uiso 1 1 d . . . H51B H 0.6623(12) -0.0203(15) 0.0818(8) 0.049(7) Uiso 1 1 d . . . H52A H 0.5546(15) 0.0110(18) 0.0301(11) 0.082(9) Uiso 1 1 d . . . H52B H 0.5365(13) 0.0051(16) 0.0774(9) 0.057(8) Uiso 1 1 d . . . H54 H 0.4831(13) 0.1075(16) 0.0992(9) 0.060(8) Uiso 1 1 d . . . H56 H 0.5254(15) 0.2797(17) 0.0429(9) 0.074(9) Uiso 1 1 d . . . H57 H 0.4765(19) 0.408(2) 0.0400(12) 0.117(13) Uiso 1 1 d . . . H58 H 0.3876(15) 0.4339(18) 0.0799(9) 0.078(9) Uiso 1 1 d . . . H59 H 0.3598(17) 0.3204(19) 0.1197(10) 0.091(10) Uiso 1 1 d . . . B3 B 0.14539(11) 0.92929(13) 0.11538(7) 0.0277(4) Uani 1 1 d . . . O62 O 0.09548(6) 0.98510(8) 0.12744(4) 0.0291(3) Uani 1 1 d . . . C63 C 0.02380(9) 0.96337(12) 0.10107(6) 0.0326(4) Uani 1 1 d . . . C64 C 0.03106(10) 0.87021(13) 0.09247(7) 0.0351(5) Uani 1 1 d . . . O65 O 0.10314(6) 0.86317(8) 0.09023(4) 0.0322(3) Uani 1 1 d . . . C66 C 0.00543(12) 1.01449(16) 0.05834(8) 0.0424(5) Uani 1 1 d . . . C67 C -0.02812(11) 0.98385(17) 0.12703(8) 0.0427(5) Uani 1 1 d . . . C68 C -0.01917(12) 0.83943(18) 0.04806(8) 0.0465(6) Uani 1 1 d . . . C69 C 0.02343(13) 0.81672(15) 0.13094(8) 0.0439(5) Uani 1 1 d . . . C70 C 0.20317(9) 0.96617(11) 0.09323(6) 0.0279(4) Uani 1 1 d . . . C71 C 0.19260(10) 0.99660(12) 0.04983(7) 0.0346(4) Uani 1 1 d . . . C72 C 0.24915(12) 1.02975(14) 0.03747(8) 0.0429(5) Uani 1 1 d . . . C73 C 0.31704(12) 1.03278(15) 0.06829(8) 0.0452(5) Uani 1 1 d . . . C74 C 0.32913(11) 1.00238(13) 0.11125(7) 0.0360(5) Uani 1 1 d . . . C75 C 0.27220(9) 0.96853(11) 0.12312(6) 0.0279(4) Uani 1 1 d . . . C76 C 0.27809(9) 0.93515(12) 0.16902(6) 0.0273(4) Uani 1 1 d . . . N77 N 0.32839(8) 0.86726(10) 0.18295(5) 0.0333(4) Uani 1 1 d . . . C78 C 0.28448(11) 0.79576(13) 0.16383(8) 0.0382(5) Uani 1 1 d . . . C79 C 0.21387(11) 0.81057(12) 0.17281(8) 0.0361(5) Uani 1 1 d . . . N80 N 0.20314(8) 0.90100(9) 0.16537(5) 0.0270(3) Uani 1 1 d . . . C81 C 0.35877(11) 0.86050(14) 0.23209(7) 0.0390(5) Uani 1 1 d . . . C82 C 0.42250(12) 0.91638(16) 0.24878(7) 0.0445(5) Uani 1 1 d . . . N83 N 0.45567(9) 0.90575(12) 0.29754(6) 0.0442(4) Uani 1 1 d . . . C84 C 0.47217(11) 0.97055(17) 0.31989(8) 0.0453(6) Uani 1 1 d . . . C85 C 0.50940(12) 0.97171(19) 0.36867(8) 0.0583(7) Uani 1 1 d . . . C86 C 0.52285(15) 0.9008(3) 0.39479(10) 0.0803(10) Uani 1 1 d . . . C87 C 0.5571(2) 0.9101(6) 0.43979(15) 0.144(2) Uani 1 1 d . . . C88 C 0.5777(3) 0.9855(7) 0.45759(17) 0.192(4) Uani 1 1 d . . . C89 C 0.5635(3) 1.0505(5) 0.42966(18) 0.139(2) Uani 1 1 d . . . N90 N 0.52870(14) 1.04723(19) 0.38507(8) 0.0885(9) Uani 1 1 d . . . H66A H -0.0436(14) 1.0065(16) 0.0394(9) 0.066(8) Uiso 1 1 d . . . H66B H 0.0383(11) 0.9975(12) 0.0395(7) 0.037(6) Uiso 1 1 d . . . H66C H 0.0092(11) 1.0749(15) 0.0671(7) 0.048(6) Uiso 1 1 d . . . H67A H -0.0792(13) 0.9660(14) 0.1094(8) 0.052(6) Uiso 1 1 d . . . H67B H -0.0148(12) 0.9581(14) 0.1567(9) 0.050(7) Uiso 1 1 d . . . H67C H -0.0294(12) 1.0452(16) 0.1320(8) 0.051(7) Uiso 1 1 d . . . H68A H -0.0139(13) 0.7779(17) 0.0475(8) 0.062(8) Uiso 1 1 d . . . H68B H -0.0693(13) 0.8498(14) 0.0467(8) 0.050(6) Uiso 1 1 d . . . H68C H -0.0109(12) 0.8640(15) 0.0208(9) 0.056(7) Uiso 1 1 d . . . H69A H 0.0539(10) 0.8377(12) 0.1618(7) 0.033(5) Uiso 1 1 d . . . H69B H 0.0361(11) 0.7535(15) 0.1256(7) 0.052(6) Uiso 1 1 d . . . H69C H -0.0269(14) 0.8166(15) 0.1346(9) 0.067(8) Uiso 1 1 d . . . H71 H 0.1412(11) 0.9928(13) 0.0260(7) 0.040(6) Uiso 1 1 d . . . H72 H 0.2417(11) 1.0514(13) 0.0069(8) 0.043(6) Uiso 1 1 d . . . H73 H 0.3545(13) 1.0538(15) 0.0585(8) 0.061(7) Uiso 1 1 d . . . H74 H 0.3750(13) 1.0029(14) 0.1323(8) 0.053(7) Uiso 1 1 d . . . H76 H 0.2884(10) 0.9792(12) 0.1919(7) 0.033(5) Uiso 1 1 d . . . H78A H 0.2798(10) 0.7968(12) 0.1322(8) 0.036(6) Uiso 1 1 d . . . H78B H 0.3089(13) 0.7449(16) 0.1789(8) 0.059(7) Uiso 1 1 d . . . H79A H 0.1745(11) 0.7806(13) 0.1516(7) 0.041(6) Uiso 1 1 d . . . H79B H 0.2189(11) 0.7990(13) 0.2045(8) 0.041(6) Uiso 1 1 d . . . H80 H 0.1885(10) 0.9277(12) 0.1890(7) 0.032(5) Uiso 1 1 d . . . H81A H 0.3230(11) 0.8734(13) 0.2495(7) 0.044(6) Uiso 1 1 d . . . H81B H 0.3781(11) 0.8012(13) 0.2389(7) 0.041(6) Uiso 1 1 d . . . H82A H 0.4048(11) 0.9798(14) 0.2407(7) 0.044(6) Uiso 1 1 d . . . H82B H 0.4609(13) 0.9025(15) 0.2336(8) 0.062(7) Uiso 1 1 d . . . H84 H 0.4644(15) 1.0282(19) 0.3075(10) 0.081(9) Uiso 1 1 d . . . H86 H 0.5049(17) 0.845(2) 0.3815(11) 0.089(11) Uiso 1 1 d . . . H87 H 0.564(3) 0.860(3) 0.4548(18) 0.15(2) Uiso 1 1 d . . . H88 H 0.605(3) 1.000(3) 0.4886(18) 0.167(18) Uiso 1 1 d . . . H89 H 0.569(2) 1.112(3) 0.4365(14) 0.127(15) Uiso 1 1 d . . . B4 B 0.20024(11) 0.10335(13) 0.23406(7) 0.0295(5) Uani 1 1 d . . . O92 O 0.19295(7) 0.01374(8) 0.23532(4) 0.0311(3) Uani 1 1 d . . . C93 C 0.16635(10) -0.00624(12) 0.27258(6) 0.0323(4) Uani 1 1 d . . . C94 C 0.12299(10) 0.07200(12) 0.27640(7) 0.0336(4) Uani 1 1 d . . . O95 O 0.16572(7) 0.13586(8) 0.26510(4) 0.0316(3) Uani 1 1 d . . . C96 C 0.12244(14) -0.08427(14) 0.26136(8) 0.0430(5) Uani 1 1 d . . . C97 C 0.23037(13) -0.01931(16) 0.31430(8) 0.0446(5) Uani 1 1 d . . . C98 C 0.04871(11) 0.07371(15) 0.24214(8) 0.0407(5) Uani 1 1 d . . . C99 C 0.11673(14) 0.08839(16) 0.32297(8) 0.0431(5) Uani 1 1 d . . . C100 C 0.27830(10) 0.13792(11) 0.23686(7) 0.0316(4) Uani 1 1 d . . . C101 C 0.33959(10) 0.14530(13) 0.27414(8) 0.0385(5) Uani 1 1 d . . . C102 C 0.40389(11) 0.17287(13) 0.26857(9) 0.0457(6) Uani 1 1 d . . . C103 C 0.40815(11) 0.19088(14) 0.22593(9) 0.0477(6) Uani 1 1 d . . . C104 C 0.34824(11) 0.18390(13) 0.18849(9) 0.0416(5) Uani 1 1 d . . . C105 C 0.28403(10) 0.15886(11) 0.19493(7) 0.0325(4) Uani 1 1 d . . . C106 C 0.21565(10) 0.15004(12) 0.15672(7) 0.0321(4) Uani 1 1 d . . . N107 N 0.19347(9) 0.22446(10) 0.13083(5) 0.0340(4) Uani 1 1 d . . . C108 C 0.15577(12) 0.26950(13) 0.15771(8) 0.0362(5) Uani 1 1 d . . . C109 C 0.11138(11) 0.20418(13) 0.17203(8) 0.0355(5) Uani 1 1 d . . . N110 N 0.15829(8) 0.12986(10) 0.17956(6) 0.0296(3) Uani 1 1 d . . . C111 C 0.14894(12) 0.21150(14) 0.08373(7) 0.0395(5) Uani 1 1 d . . . C112 C 0.17042(13) 0.26957(14) 0.05215(8) 0.0417(5) Uani 1 1 d . . . N113 N 0.15338(9) 0.35405(11) 0.05953(6) 0.0411(4) Uani 1 1 d . . . C114 C 0.20174(12) 0.40682(14) 0.06344(7) 0.0402(5) Uani 1 1 d . . . C115 C 0.18931(12) 0.49506(14) 0.06933(7) 0.0435(5) Uani 1 1 d . . . C116 C 0.12997(16) 0.52314(17) 0.07978(9) 0.0567(6) Uani 1 1 d . . . C117 C 0.1207(2) 0.60679(18) 0.08302(10) 0.0683(8) Uani 1 1 d . . . C118 C 0.16984(19) 0.65882(18) 0.07514(9) 0.0699(8) Uani 1 1 d . . . C119 C 0.22853(19) 0.62605(18) 0.06623(11) 0.0713(8) Uani 1 1 d . . . N120 N 0.23974(11) 0.54484(13) 0.06333(7) 0.0611(6) Uani 1 1 d . . . H96A H 0.0986(12) -0.0979(14) 0.2869(8) 0.051(6) Uiso 1 1 d . . . H96B H 0.1543(11) -0.1296(14) 0.2586(7) 0.043(6) Uiso 1 1 d . . . H96C H 0.0818(12) -0.0752(13) 0.2292(8) 0.050(6) Uiso 1 1 d . . . H97A H 0.2129(12) -0.0377(15) 0.3382(9) 0.057(7) Uiso 1 1 d . . . H97B H 0.2600(11) 0.0329(13) 0.3256(7) 0.038(6) Uiso 1 1 d . . . H97C H 0.2634(14) -0.0606(16) 0.3083(8) 0.064(7) Uiso 1 1 d . . . H98A H 0.0548(11) 0.0624(13) 0.2109(8) 0.039(6) Uiso 1 1 d . . . H98B H 0.0278(12) 0.1330(16) 0.2408(8) 0.056(7) Uiso 1 1 d . . . H98C H 0.0164(12) 0.0357(14) 0.2487(7) 0.046(6) Uiso 1 1 d . . . H99A H 0.0876(12) 0.1392(15) 0.3226(7) 0.047(6) Uiso 1 1 d . . . H99B H 0.0953(12) 0.0455(15) 0.3324(8) 0.053(7) Uiso 1 1 d . . . H99C H 0.1631(12) 0.0955(13) 0.3438(7) 0.039(6) Uiso 1 1 d . . . H101 H 0.3377(11) 0.1316(13) 0.3052(8) 0.042(6) Uiso 1 1 d . . . H102 H 0.4469(12) 0.1765(13) 0.2970(8) 0.048(6) Uiso 1 1 d . . . H103 H 0.4539(13) 0.2107(14) 0.2220(8) 0.057(7) Uiso 1 1 d . . . H104 H 0.3515(12) 0.1975(14) 0.1573(9) 0.057(7) Uiso 1 1 d . . . H106 H 0.2174(9) 0.1042(12) 0.1359(6) 0.024(5) Uiso 1 1 d . . . H110 H 0.1340(10) 0.0874(13) 0.1652(7) 0.031(5) Uiso 1 1 d . . . H109 H 0.1024(11) 0.2169(13) 0.2009(8) 0.040(6) Uiso 1 1 d . . . H108 H 0.1935(11) 0.2905(12) 0.1848(7) 0.035(5) Uiso 1 1 d . . . H111 H 0.1602(11) 0.1535(14) 0.0754(7) 0.042(6) Uiso 1 1 d . . . H112 H 0.2240(13) 0.2633(14) 0.0547(8) 0.056(7) Uiso 1 1 d . . . H114 H 0.2498(13) 0.3914(14) 0.0625(8) 0.051(6) Uiso 1 1 d . . . H116 H 0.0964(14) 0.4846(18) 0.0814(9) 0.069(9) Uiso 1 1 d . . . H117 H 0.0818(18) 0.626(2) 0.0913(11) 0.100(12) Uiso 1 1 d . . . H118 H 0.1604(15) 0.7213(19) 0.0760(9) 0.083(9) Uiso 1 1 d . . . H119 H 0.2638(17) 0.658(2) 0.0589(11) 0.096(11) Uiso 1 1 d . . . H129 H 0.0686(11) 0.1917(12) 0.1465(7) 0.037(6) Uiso 1 1 d . . . H128 H 0.1270(11) 0.3119(14) 0.1400(7) 0.046(6) Uiso 1 1 d . . . H131 H 0.0975(13) 0.2186(15) 0.0801(8) 0.058(7) Uiso 1 1 d . . . H132 H 0.1405(11) 0.2517(13) 0.0197(8) 0.047(6) Uiso 1 1 d . . . C201 C 0.5410(4) 0.3989(3) -0.0601(2) 0.214(4) Uani 1 1 d . . . H20A H 0.5480 0.3707 -0.0863 0.321 Uiso 1 1 calc R . . H20B H 0.5307 0.4568 -0.0673 0.321 Uiso 1 1 calc R . . H20C H 0.5008 0.3739 -0.0523 0.321 Uiso 1 1 calc R . . C202 C 0.5974(4) 0.3927(4) -0.0269(2) 0.157(2) Uani 1 1 d . . . H20D H 0.6361 0.4222 -0.0349 0.189 Uiso 1 1 calc R . . H20J H 0.6110 0.3341 -0.0238 0.189 Uiso 1 1 calc R . . O203 O 0.5968(3) 0.4188(4) 0.01235(15) 0.216(3) Uani 1 1 d . . . C204 C 0.6535(3) 0.4119(4) 0.0449(3) 0.197(4) Uani 1 1 d . . . H20E H 0.6952 0.4309 0.0358 0.236 Uiso 1 1 calc R . . H20F H 0.6615 0.3538 0.0543 0.236 Uiso 1 1 calc R . . C205 C 0.6453(7) 0.4648(7) 0.0845(2) 0.386(10) Uani 1 1 d . . . H20G H 0.6870 0.4565 0.1111 0.579 Uiso 1 1 calc R . . H20H H 0.6016 0.4487 0.0915 0.579 Uiso 1 1 calc R . . H20I H 0.6422 0.5228 0.0759 0.579 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 B1 0.0391(12) 0.0383(13) 0.0348(13) -0.0058(10) 0.0159(10) -0.0092(10) O2 0.0477(8) 0.0528(10) 0.0426(9) -0.0139(7) 0.0271(7) -0.0214(7) C3 0.0529(13) 0.0735(18) 0.0489(15) -0.0226(13) 0.0331(12) -0.0289(12) C4 0.0396(11) 0.0724(17) 0.0469(14) -0.0167(12) 0.0251(11) -0.0073(11) O5 0.0370(7) 0.0424(8) 0.0410(8) -0.0095(7) 0.0181(6) -0.0050(6) C6 0.093(2) 0.0630(19) 0.0503(16) -0.0076(14) 0.0447(16) -0.0261(16) C7 0.0655(19) 0.139(3) 0.076(2) -0.049(2) 0.0489(19) -0.052(2) C8 0.0424(14) 0.123(3) 0.0559(18) -0.0107(19) 0.0199(13) 0.0151(16) C9 0.0618(17) 0.079(2) 0.0520(17) -0.0209(15) 0.0311(15) -0.0042(15) C10 0.0415(10) 0.0250(10) 0.0377(12) -0.0011(8) 0.0147(9) -0.0050(8) C11 0.0503(13) 0.0382(13) 0.0406(13) 0.0036(10) 0.0147(11) -0.0015(10) C12 0.0509(13) 0.0473(14) 0.0470(15) 0.0035(11) 0.0077(12) 0.0070(11) C13 0.0403(12) 0.0465(14) 0.0630(17) 0.0007(12) 0.0162(12) 0.0117(10) C14 0.0434(11) 0.0375(12) 0.0482(14) -0.0002(10) 0.0200(11) 0.0054(9) C15 0.0360(10) 0.0259(10) 0.0401(12) -0.0011(9) 0.0143(9) -0.0036(8) C16 0.0337(9) 0.0283(11) 0.0364(11) -0.0035(9) 0.0169(9) -0.0048(8) N17 0.0387(9) 0.0319(9) 0.0373(10) 0.0006(7) 0.0156(8) -0.0059(7) C18 0.0502(13) 0.0306(12) 0.0488(14) 0.0016(10) 0.0181(11) -0.0057(9) C19 0.0516(13) 0.0358(12) 0.0461(14) 0.0009(11) 0.0199(12) 0.0054(10) N20 0.0341(9) 0.0366(10) 0.0372(10) -0.0045(8) 0.0158(8) -0.0059(7) C21 0.0394(11) 0.0468(14) 0.0391(13) 0.0071(10) 0.0166(10) 0.0000(9) C22 0.0520(13) 0.0468(15) 0.0385(13) 0.0004(11) 0.0178(11) -0.0031(11) N23 0.0556(11) 0.0695(14) 0.0395(11) -0.0003(10) 0.0199(10) 0.0046(10) C24 0.0729(18) 0.0536(16) 0.0515(16) -0.0096(12) 0.0310(14) -0.0173(13) C25 0.064(4) 0.050(3) 0.044(3) -0.011(2) 0.024(3) -0.005(3) C26 0.072(3) 0.061(2) 0.047(2) -0.0094(18) 0.019(2) -0.009(2) C27 0.099(3) 0.066(3) 0.050(2) -0.007(2) 0.012(2) -0.011(2) C28 0.188(5) 0.052(2) 0.083(3) -0.001(2) 0.034(4) -0.009(3) C29 0.089(4) 0.051(3) 0.089(5) 0.005(3) 0.038(4) -0.019(3) N30 0.091(3) 0.074(2) 0.051(2) 0.0013(18) 0.038(2) -0.020(2) C25A 0.071(9) 0.038(6) 0.029(6) -0.001(5) 0.020(8) 0.006(8) C26A 0.074(11) 0.102(13) 0.046(9) 0.017(8) 0.002(7) 0.035(9) C27A 0.17(2) 0.055(9) 0.029(7) -0.008(6) -0.043(10) 0.008(11) C29A 0.111(11) 0.067(8) 0.035(6) -0.003(5) 0.014(6) -0.037(7) N30A 0.069(6) 0.051(5) 0.046(5) 0.000(4) 0.030(5) -0.012(4) B2 0.0309(10) 0.0290(12) 0.0336(12) -0.0003(9) 0.0095(9) -0.0007(9) O32 0.0296(6) 0.0309(7) 0.0395(8) 0.0010(6) 0.0062(6) -0.0012(5) C33 0.0298(9) 0.0336(11) 0.0411(12) 0.0032(9) 0.0069(9) 0.0015(8) C34 0.0309(9) 0.0329(11) 0.0406(12) 0.0002(9) 0.0097(9) 0.0016(8) O35 0.0303(6) 0.0293(7) 0.0387(8) -0.0003(6) 0.0070(6) -0.0011(5) C36 0.0435(12) 0.0442(14) 0.0414(13) 0.0064(11) 0.0118(10) -0.0029(10) C37 0.0457(13) 0.0354(13) 0.0606(17) 0.0015(11) 0.0127(12) 0.0054(10) C38 0.0351(11) 0.0433(14) 0.0471(14) 0.0019(11) 0.0057(10) -0.0016(10) C39 0.0374(11) 0.0454(14) 0.0499(15) -0.0014(11) 0.0173(11) -0.0014(10) C40 0.0316(9) 0.0282(10) 0.0397(12) -0.0007(9) 0.0097(9) -0.0051(8) C41 0.0358(10) 0.0387(12) 0.0415(13) -0.0026(10) 0.0123(10) -0.0036(9) C42 0.0421(11) 0.0408(13) 0.0528(15) -0.0025(11) 0.0239(11) -0.0050(9) C43 0.0347(11) 0.0343(12) 0.0685(17) 0.0017(11) 0.0220(11) -0.0013(9) C44 0.0337(10) 0.0340(12) 0.0564(15) 0.0044(10) 0.0095(11) -0.0014(9) C45 0.0317(9) 0.0250(10) 0.0419(12) 0.0006(9) 0.0070(9) -0.0038(8) C46 0.0346(10) 0.0287(11) 0.0430(12) -0.0008(9) 0.0038(9) -0.0024(8) N47 0.0501(10) 0.0356(10) 0.0352(10) 0.0047(8) 0.0047(8) 0.0004(8) C48 0.0564(14) 0.0369(13) 0.0440(14) 0.0051(11) 0.0121(11) -0.0103(10) C49 0.0440(12) 0.0443(13) 0.0386(13) 0.0047(10) 0.0118(11) -0.0104(10) N50 0.0349(8) 0.0308(10) 0.0355(10) -0.0013(8) 0.0101(7) -0.0031(7) C51 0.0684(17) 0.0555(17) 0.0380(14) 0.0044(12) 0.0085(12) 0.0061(14) C52 0.0694(17) 0.0589(18) 0.0493(17) 0.0034(14) -0.0035(14) -0.0067(14) N53 0.0621(13) 0.0594(14) 0.0442(12) 0.0125(10) -0.0039(11) 0.0006(10) C54 0.0497(14) 0.0583(17) 0.0463(15) 0.0127(13) -0.0051(12) -0.0150(12) C55 0.0426(12) 0.0605(17) 0.0462(14) 0.0102(12) -0.0060(11) -0.0095(11) C56 0.0662(17) 0.0594(19) 0.083(2) 0.0146(16) 0.0232(17) -0.0047(14) C57 0.083(2) 0.059(2) 0.111(3) 0.0253(19) 0.031(2) -0.0073(16) C58 0.0570(16) 0.0561(19) 0.090(2) 0.0172(16) 0.0057(16) -0.0031(14) C59 0.0558(16) 0.072(2) 0.0654(19) 0.0130(15) 0.0038(14) 0.0008(14) N60 0.0559(12) 0.0618(15) 0.0659(15) 0.0168(12) 0.0087(11) -0.0007(11) B3 0.0278(10) 0.0290(11) 0.0252(11) -0.0008(9) 0.0061(8) -0.0023(8) O62 0.0239(6) 0.0345(7) 0.0264(7) -0.0037(6) 0.0040(5) -0.0007(5) C63 0.0228(8) 0.0440(12) 0.0284(10) -0.0025(9) 0.0037(8) -0.0026(8) C64 0.0270(9) 0.0458(12) 0.0317(11) -0.0049(9) 0.0077(8) -0.0092(8) O65 0.0305(6) 0.0333(8) 0.0325(7) -0.0061(6) 0.0089(6) -0.0068(5) C66 0.0345(11) 0.0546(16) 0.0331(12) 0.0025(11) 0.0029(10) 0.0010(10) C67 0.0295(10) 0.0591(16) 0.0396(14) -0.0062(12) 0.0107(10) -0.0013(10) C68 0.0359(12) 0.0617(17) 0.0388(14) -0.0128(12) 0.0066(10) -0.0155(11) C69 0.0429(12) 0.0478(15) 0.0423(14) -0.0006(11) 0.0148(11) -0.0123(10) C70 0.0315(9) 0.0238(10) 0.0280(10) -0.0024(8) 0.0083(8) -0.0009(7) C71 0.0358(10) 0.0356(11) 0.0305(11) -0.0001(9) 0.0073(9) -0.0037(8) C72 0.0477(12) 0.0498(14) 0.0335(12) 0.0086(10) 0.0155(10) -0.0051(10) C73 0.0387(11) 0.0529(14) 0.0475(14) 0.0104(11) 0.0181(10) -0.0075(10) C74 0.0308(10) 0.0349(12) 0.0422(13) 0.0011(9) 0.0108(9) -0.0033(8) C75 0.0288(9) 0.0239(10) 0.0311(10) -0.0015(8) 0.0091(8) 0.0005(7) C76 0.0233(8) 0.0270(10) 0.0302(10) -0.0015(8) 0.0062(7) -0.0013(7) N77 0.0295(8) 0.0359(10) 0.0313(9) 0.0037(7) 0.0044(7) 0.0058(7) C78 0.0438(11) 0.0288(11) 0.0398(13) 0.0024(10) 0.0092(10) 0.0062(9) C79 0.0390(11) 0.0262(11) 0.0394(13) 0.0058(9) 0.0061(10) -0.0021(8) N80 0.0271(7) 0.0254(8) 0.0280(9) 0.0007(7) 0.0075(7) -0.0012(6) C81 0.0343(10) 0.0463(13) 0.0325(12) 0.0093(10) 0.0043(9) 0.0012(9) C82 0.0390(11) 0.0578(16) 0.0330(12) -0.0006(11) 0.0054(10) -0.0071(10) N83 0.0341(9) 0.0598(13) 0.0346(10) -0.0011(9) 0.0043(8) -0.0041(8) C84 0.0346(11) 0.0648(17) 0.0376(13) -0.0034(12) 0.0123(9) -0.0083(11) C85 0.0396(12) 0.097(2) 0.0377(14) -0.0135(14) 0.0104(11) -0.0201(13) C86 0.0519(15) 0.135(3) 0.0444(17) 0.021(2) 0.0003(13) -0.0045(18) C87 0.091(3) 0.268(8) 0.050(3) 0.040(4) -0.012(2) -0.019(4) C88 0.137(4) 0.382(12) 0.036(3) -0.016(5) -0.007(3) -0.098(6) C89 0.115(3) 0.232(7) 0.068(3) -0.075(4) 0.026(3) -0.097(4) N90 0.0793(16) 0.133(2) 0.0583(16) -0.0401(16) 0.0280(13) -0.0531(17) B4 0.0322(10) 0.0266(11) 0.0273(11) -0.0020(9) 0.0053(9) 0.0006(8) O92 0.0384(7) 0.0266(7) 0.0288(7) -0.0011(6) 0.0106(6) 0.0004(5) C93 0.0389(10) 0.0312(11) 0.0265(10) 0.0003(8) 0.0092(8) -0.0020(8) C94 0.0379(10) 0.0307(11) 0.0333(11) -0.0022(8) 0.0123(9) -0.0044(8) O95 0.0352(7) 0.0272(7) 0.0336(7) -0.0037(6) 0.0123(6) -0.0028(5) C96 0.0584(14) 0.0329(12) 0.0404(13) -0.0014(10) 0.0190(12) -0.0053(10) C97 0.0525(13) 0.0445(14) 0.0327(12) 0.0024(11) 0.0063(11) 0.0070(11) C98 0.0349(11) 0.0402(13) 0.0470(14) -0.0010(11) 0.0125(10) -0.0037(9) C99 0.0529(14) 0.0399(14) 0.0409(13) -0.0044(11) 0.0209(12) -0.0039(11) C100 0.0323(9) 0.0232(10) 0.0381(11) -0.0045(8) 0.0089(8) 0.0020(7) C101 0.0352(10) 0.0344(12) 0.0423(13) -0.0077(10) 0.0065(9) 0.0036(8) C102 0.0302(10) 0.0375(13) 0.0631(16) -0.0121(11) 0.0049(11) 0.0014(9) C103 0.0341(11) 0.0372(13) 0.0735(18) -0.0035(12) 0.0188(12) -0.0028(9) C104 0.0390(11) 0.0327(12) 0.0570(15) 0.0014(10) 0.0203(11) 0.0004(9) C105 0.0340(10) 0.0227(10) 0.0417(12) -0.0028(8) 0.0125(9) 0.0009(8) C106 0.0408(10) 0.0249(10) 0.0339(11) -0.0025(8) 0.0160(9) -0.0003(8) N107 0.0445(9) 0.0270(9) 0.0307(9) -0.0015(7) 0.0117(7) -0.0009(7) C108 0.0453(11) 0.0263(11) 0.0360(12) -0.0006(9) 0.0105(10) 0.0049(9) C109 0.0399(11) 0.0325(11) 0.0347(12) 0.0021(9) 0.0120(10) 0.0078(9) N110 0.0322(8) 0.0247(9) 0.0317(9) -0.0018(7) 0.0094(7) -0.0007(7) C111 0.0480(12) 0.0340(12) 0.0355(12) -0.0038(9) 0.0110(10) -0.0030(9) C112 0.0530(13) 0.0373(12) 0.0340(12) 0.0008(10) 0.0117(10) 0.0054(10) N113 0.0463(10) 0.0363(10) 0.0381(10) 0.0061(8) 0.0087(8) 0.0045(8) C114 0.0445(12) 0.0439(13) 0.0283(11) 0.0035(9) 0.0053(9) 0.0015(10) C115 0.0557(13) 0.0424(13) 0.0251(11) 0.0031(9) 0.0011(10) -0.0020(10) C116 0.0742(17) 0.0470(16) 0.0504(16) 0.0017(12) 0.0210(14) 0.0048(13) C117 0.095(2) 0.0524(18) 0.0593(18) -0.0023(14) 0.0255(17) 0.0141(16) C118 0.106(2) 0.0418(17) 0.0471(16) -0.0030(13) 0.0004(16) 0.0024(16) C119 0.088(2) 0.0468(18) 0.067(2) 0.0018(14) 0.0051(17) -0.0156(16) N120 0.0657(13) 0.0474(13) 0.0610(14) 0.0026(10) 0.0055(11) -0.0111(10) C201 0.312(9) 0.064(3) 0.208(7) 0.015(4) -0.008(7) -0.057(4) C202 0.192(6) 0.152(5) 0.128(5) 0.044(4) 0.049(4) 0.038(4) O203 0.202(4) 0.354(7) 0.100(3) -0.078(4) 0.057(3) -0.125(5) C204 0.113(4) 0.184(6) 0.248(9) 0.088(6) -0.013(5) -0.012(4) C205 0.63(2) 0.392(14) 0.089(4) -0.057(6) 0.043(8) -0.383(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 O5 1.442(3) . ? B1 O2 1.468(3) . ? B1 C10 1.602(3) . ? B1 N20 1.691(3) . ? O2 C3 1.442(3) . ? C3 C7 1.519(3) . ? C3 C6 1.526(4) . ? C3 C4 1.546(4) . ? C4 O5 1.442(2) . ? C4 C9 1.521(3) . ? C4 C8 1.526(4) . ? C6 H6A 1.05(3) . ? C6 H6B 1.03(4) . ? C6 H6C 1.03(3) . ? C7 H7A 0.97(3) . ? C7 H7B 1.01(3) . ? C7 H7C 1.10(5) . ? C8 H8A 1.00(3) . ? C8 H8B 1.14(4) . ? C8 H8C 0.96(3) . ? C9 H9A 0.99(3) . ? C9 H9B 0.98(3) . ? C9 H9C 1.12(3) . ? C10 C15 1.391(3) . ? C10 C11 1.392(3) . ? C11 C12 1.386(3) . ? C11 H11 0.97(3) . ? C12 C13 1.388(3) . ? C12 H12 0.97(2) . ? C13 C14 1.384(3) . ? C13 H13 0.90(2) . ? C14 C15 1.389(3) . ? C14 H14 0.99(2) . ? C15 C16 1.505(3) . ? C16 N17 1.449(2) . ? C16 N20 1.537(2) . ? C16 H16 0.962(18) . ? N17 C18 1.471(3) . ? N17 C21 1.472(3) . ? C18 C19 1.524(3) . ? C18 H18A 1.08(2) . ? C18 H18B 0.97(2) . ? C19 N20 1.507(3) . ? C19 H19A 1.04(2) . ? C19 H19B 0.94(2) . ? N20 H20 0.92(2) . ? C21 C22 1.515(3) . ? C21 H21A 1.04(2) . ? C21 H21B 1.03(2) . ? C22 N23 1.458(3) . ? C22 H22A 1.04(2) . ? C22 H22B 0.96(2) . ? N23 C24 1.230(3) . ? C24 C25A 1.374(16) . ? C24 C25 1.532(7) . ? C24 H24 0.97(3) . ? C25 C25A 0.679(12) . ? C25 C26A 0.813(13) . ? C25 N30 1.342(7) . ? C25 C26 1.366(7) . ? C25 N30A 1.948(11) . ? C25 C27A 2.031(17) . ? C26 C26A 1.108(19) . ? C26 C27 1.377(6) . ? C26 C25A 2.018(16) . ? C26 H26 0.94(3) . ? C27 C28 1.366(7) . ? C27 C27A 1.72(3) . ? C27 C26A 1.768(18) . ? C27 H27 0.90(5) . ? C28 C27A 0.941(16) . ? C28 C29 1.358(8) . ? C28 H28 1.22(4) . ? C29 C27A 0.91(3) . ? C29 C29A 1.288(17) . ? C29 N30 1.408(7) . ? C29 C26A 2.032(18) . ? C29 H29 0.82(3) . ? N30 C25A 1.072(16) . ? N30 N30A 1.111(10) . ? N30 C26A 1.443(18) . ? N30 C29A 1.447(14) . ? N30 C27A 1.55(2) . ? C25A N30A 1.360(17) . ? C25A C26A 1.361(19) . ? C26A C27A 1.43(2) . ? C29A N30A 1.359(14) . ? C29A H29 1.19(4) . ? B2 O35 1.437(2) . ? B2 O32 1.464(3) . ? B2 C40 1.606(3) . ? B2 N50 1.702(3) . ? O32 C33 1.446(2) . ? C33 C37 1.515(3) . ? C33 C36 1.525(3) . ? C33 C34 1.558(3) . ? C34 O35 1.439(2) . ? C34 C38 1.520(3) . ? C34 C39 1.526(3) . ? C36 H36A 1.05(2) . ? C36 H36B 0.99(2) . ? C36 H36C 1.02(2) . ? C37 H37A 1.02(3) . ? C37 H37B 1.01(2) . ? C37 H37C 1.01(3) . ? C38 H38A 0.98(2) . ? C38 H38B 1.04(3) . ? C38 H38C 1.04(2) . ? C39 H39A 1.05(2) . ? C39 H39B 1.01(2) . ? C39 H39C 0.95(3) . ? C40 C45 1.390(3) . ? C40 C41 1.397(3) . ? C41 C42 1.389(3) . ? C41 H41 1.01(2) . ? C42 C43 1.384(3) . ? C42 H42 0.97(2) . ? C43 C44 1.376(3) . ? C43 H43 1.04(2) . ? C44 C45 1.391(3) . ? C44 H44 0.99(3) . ? C45 C46 1.503(3) . ? C46 N47 1.455(3) . ? C46 N50 1.540(2) . ? C46 H46 1.01(2) . ? N47 C48 1.469(3) . ? N47 C51 1.470(3) . ? C48 C49 1.518(3) . ? C48 H48A 0.96(2) . ? C48 H48B 1.00(2) . ? C49 N50 1.498(3) . ? C49 H49A 1.00(3) . ? C49 H49B 0.93(2) . ? N50 H50 0.89(2) . ? C51 C52 1.515(4) . ? C51 H51A 0.99(3) . ? C51 H51B 0.97(2) . ? C52 N53 1.461(4) . ? C52 H52A 1.07(3) . ? C52 H52B 0.96(3) . ? N53 C54 1.265(4) . ? C54 C55 1.471(4) . ? C54 H54 0.91(3) . ? C55 N60 1.328(3) . ? C55 C56 1.380(4) . ? C56 C57 1.370(4) . ? C56 H56 0.94(3) . ? C57 C58 1.375(5) . ? C57 H57 0.98(4) . ? C58 C59 1.357(4) . ? C58 H58 1.03(3) . ? C59 N60 1.342(4) . ? C59 H59 1.00(3) . ? B3 O65 1.439(2) . ? B3 O62 1.465(2) . ? B3 C70 1.608(3) . ? B3 N80 1.688(3) . ? O62 C63 1.439(2) . ? C63 C67 1.514(3) . ? C63 C66 1.518(3) . ? C63 C64 1.559(3) . ? C64 O65 1.437(2) . ? C64 C68 1.520(3) . ? C64 C69 1.525(3) . ? C66 H66A 0.97(3) . ? C66 H66B 1.03(2) . ? C66 H66C 1.02(2) . ? C67 H67A 1.03(2) . ? C67 H67B 0.98(2) . ? C67 H67C 1.02(2) . ? C68 H68A 1.01(3) . ? C68 H68B 0.98(2) . ? C68 H68C 0.99(3) . ? C69 H69A 1.02(2) . ? C69 H69B 1.09(2) . ? C69 H69C 1.03(3) . ? C70 C75 1.390(2) . ? C70 C71 1.395(3) . ? C71 C72 1.386(3) . ? C71 H71 1.06(2) . ? C72 C73 1.385(3) . ? C72 H72 0.98(2) . ? C73 C74 1.378(3) . ? C73 H73 0.94(3) . ? C74 C75 1.389(3) . ? C74 H74 0.94(2) . ? C75 C76 1.500(3) . ? C76 N77 1.459(2) . ? C76 N80 1.541(2) . ? C76 H76 0.99(2) . ? N77 C78 1.465(3) . ? N77 C81 1.468(3) . ? C78 C79 1.509(3) . ? C78 H78A 0.96(2) . ? C78 H78B 1.00(3) . ? C79 N80 1.500(2) . ? C79 H79A 0.98(2) . ? C79 H79B 0.98(2) . ? N80 H80 0.97(2) . ? C81 C82 1.505(3) . ? C81 H81A 1.03(2) . ? C81 H81B 1.04(2) . ? C82 N83 1.469(3) . ? C82 H82A 1.10(2) . ? C82 H82B 1.02(2) . ? N83 C84 1.254(3) . ? C84 C85 1.472(3) . ? C84 H84 1.01(3) . ? C85 N90 1.345(4) . ? C85 C86 1.393(4) . ? C86 C87 1.367(6) . ? C86 H86 1.01(3) . ? C87 C88 1.360(10) . ? C87 H87 0.93(5) . ? C88 C89 1.346(10) . ? C88 H88 0.98(5) . ? C89 N90 1.350(6) . ? C89 H89 1.02(4) . ? B4 O95 1.437(3) . ? B4 O92 1.472(2) . ? B4 C100 1.606(3) . ? B4 N110 1.702(3) . ? O92 C93 1.444(2) . ? C93 C96 1.517(3) . ? C93 C97 1.523(3) . ? C93 C94 1.558(3) . ? C94 O95 1.445(2) . ? C94 C99 1.514(3) . ? C94 C98 1.521(3) . ? C96 H96A 1.06(2) . ? C96 H96B 0.99(2) . ? C96 H96C 1.08(2) . ? C97 H97A 0.96(3) . ? C97 H97B 1.03(2) . ? C97 H97C 0.99(3) . ? C98 H98A 1.03(2) . ? C98 H98B 1.05(2) . ? C98 H98C 0.95(2) . ? C99 H99A 1.00(2) . ? C99 H99B 0.91(3) . ? C99 H99C 0.95(2) . ? C100 C105 1.385(3) . ? C100 C101 1.400(3) . ? C101 C102 1.395(3) . ? C101 H101 1.00(2) . ? C102 C103 1.386(4) . ? C102 H102 1.02(2) . ? C103 C104 1.386(3) . ? C103 H103 0.99(2) . ? C104 C105 1.392(3) . ? C104 H104 1.02(2) . ? C105 C106 1.505(3) . ? C106 N107 1.450(2) . ? C106 N110 1.534(2) . ? C106 H106 0.997(19) . ? N107 C108 1.468(3) . ? N107 C111 1.477(3) . ? C108 C109 1.524(3) . ? C108 H108 1.00(2) . ? C108 H128 0.96(2) . ? C109 N110 1.497(2) . ? C109 H109 0.99(2) . ? C109 H129 0.99(2) . ? N110 H110 0.88(2) . ? C111 C112 1.513(3) . ? C111 H111 1.02(2) . ? C111 H131 0.99(2) . ? C112 N113 1.454(3) . ? C112 H112 1.03(2) . ? C112 H132 1.04(2) . ? N113 C114 1.258(3) . ? C114 C115 1.482(3) . ? C114 H114 0.98(2) . ? C115 N120 1.334(3) . ? C115 C116 1.375(4) . ? C116 C117 1.386(4) . ? C116 H116 0.92(3) . ? C117 C118 1.360(4) . ? C117 H117 0.93(3) . ? C118 C119 1.369(5) . ? C118 H118 1.04(3) . ? C119 N120 1.352(4) . ? C119 H119 0.95(3) . ? C201 C202 1.267(7) . ? C201 H20A 0.9800 . ? C201 H20B 0.9800 . ? C201 H20C 0.9800 . ? C202 O203 1.298(7) . ? C202 H20D 0.9900 . ? C202 H20J 0.9900 . ? O203 C204 1.261(6) . ? C204 C205 1.553(12) . ? C204 H20E 0.9900 . ? C204 H20F 0.9900 . ? C205 H20G 0.9800 . ? C205 H20H 0.9800 . ? C205 H20I 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 B1 O2 106.10(16) . . ? O5 B1 C10 116.65(17) . . ? O2 B1 C10 117.00(18) . . ? O5 B1 N20 111.54(17) . . ? O2 B1 N20 107.23(16) . . ? C10 B1 N20 97.82(15) . . ? C3 O2 B1 107.06(16) . . ? O2 C3 C7 108.5(2) . . ? O2 C3 C6 108.9(2) . . ? C7 C3 C6 109.1(3) . . ? O2 C3 C4 102.11(17) . . ? C7 C3 C4 116.0(3) . . ? C6 C3 C4 111.8(2) . . ? O5 C4 C9 108.98(19) . . ? O5 C4 C8 109.0(2) . . ? C9 C4 C8 108.7(2) . . ? O5 C4 C3 101.26(17) . . ? C9 C4 C3 115.1(2) . . ? C8 C4 C3 113.5(2) . . ? C4 O5 B1 108.22(15) . . ? C3 C6 H6A 112.6(13) . . ? C3 C6 H6B 116.6(19) . . ? H6A C6 H6B 107(2) . . ? C3 C6 H6C 111.5(17) . . ? H6A C6 H6C 105(2) . . ? H6B C6 H6C 102(2) . . ? C3 C7 H7A 107.6(17) . . ? C3 C7 H7B 109.3(17) . . ? H7A C7 H7B 108(2) . . ? C3 C7 H7C 115(3) . . ? H7A C7 H7C 100(3) . . ? H7B C7 H7C 116(3) . . ? C4 C8 H8A 112.2(16) . . ? C4 C8 H8B 112.3(17) . . ? H8A C8 H8B 106(2) . . ? C4 C8 H8C 110.2(17) . . ? H8A C8 H8C 104(2) . . ? H8B C8 H8C 112(2) . . ? C4 C9 H9A 111.3(14) . . ? C4 C9 H9B 110.5(17) . . ? H9A C9 H9B 105(2) . . ? C4 C9 H9C 114.0(16) . . ? H9A C9 H9C 109(2) . . ? H9B C9 H9C 106(2) . . ? C15 C10 C11 117.71(19) . . ? C15 C10 B1 112.69(18) . . ? C11 C10 B1 129.60(19) . . ? C12 C11 C10 120.8(2) . . ? C12 C11 H11 119.5(14) . . ? C10 C11 H11 119.7(14) . . ? C11 C12 C13 120.1(2) . . ? C11 C12 H12 116.5(14) . . ? C13 C12 H12 123.3(14) . . ? C14 C13 C12 120.4(2) . . ? C14 C13 H13 119.6(14) . . ? C12 C13 H13 119.8(14) . . ? C13 C14 C15 118.5(2) . . ? C13 C14 H14 122.4(13) . . ? C15 C14 H14 119.1(13) . . ? C14 C15 C10 122.4(2) . . ? C14 C15 C16 123.42(19) . . ? C10 C15 C16 114.11(17) . . ? N17 C16 C15 114.03(16) . . ? N17 C16 N20 107.85(15) . . ? C15 C16 N20 104.51(15) . . ? N17 C16 H16 110.9(11) . . ? C15 C16 H16 109.5(11) . . ? N20 C16 H16 109.8(10) . . ? C16 N17 C18 102.39(16) . . ? C16 N17 C21 113.24(16) . . ? C18 N17 C21 110.78(17) . . ? N17 C18 C19 105.15(17) . . ? N17 C18 H18A 108.9(11) . . ? C19 C18 H18A 109.6(11) . . ? N17 C18 H18B 111.6(12) . . ? C19 C18 H18B 111.3(12) . . ? H18A C18 H18B 110.1(16) . . ? N20 C19 C18 103.61(17) . . ? N20 C19 H19A 111.5(13) . . ? C18 C19 H19A 109.8(12) . . ? N20 C19 H19B 108.9(14) . . ? C18 C19 H19B 112.6(14) . . ? H19A C19 H19B 110.2(19) . . ? C19 N20 C16 104.52(15) . . ? C19 N20 B1 115.70(17) . . ? C16 N20 B1 108.85(15) . . ? C19 N20 H20 111.6(15) . . ? C16 N20 H20 103.8(15) . . ? B1 N20 H20 111.4(15) . . ? N17 C21 C22 112.17(18) . . ? N17 C21 H21A 109.0(12) . . ? C22 C21 H21A 106.2(12) . . ? N17 C21 H21B 113.5(12) . . ? C22 C21 H21B 110.0(12) . . ? H21A C21 H21B 105.4(16) . . ? N23 C22 C21 108.68(19) . . ? N23 C22 H22A 112.4(12) . . ? C21 C22 H22A 108.7(12) . . ? N23 C22 H22B 108.3(14) . . ? C21 C22 H22B 109.4(14) . . ? H22A C22 H22B 109.4(18) . . ? C24 N23 C22 118.0(2) . . ? N23 C24 C25A 143.3(7) . . ? N23 C24 C25 117.7(3) . . ? C25A C24 C25 26.3(5) . . ? N23 C24 H24 123.5(16) . . ? C25A C24 H24 92.5(17) . . ? C25 C24 H24 118.6(16) . . ? C25A C25 C26A 131(3) . . ? C25A C25 N30 52.4(17) . . ? C26A C25 N30 79.9(16) . . ? C25A C25 C26 160.2(19) . . ? C26A C25 C26 54.2(15) . . ? N30 C25 C26 123.1(6) . . ? C25A C25 C24 63.7(17) . . ? C26A C25 C24 146.9(13) . . ? N30 C25 C24 112.9(5) . . ? C26 C25 C24 124.0(5) . . ? C25A C25 N30A 24.7(16) . . ? C26A C25 N30A 112.5(16) . . ? N30 C25 N30A 33.5(3) . . ? C26 C25 N30A 140.1(5) . . ? C24 C25 N30A 88.0(4) . . ? C25A C25 C27A 102(2) . . ? C26A C25 C27A 33.7(15) . . ? N30 C25 C27A 49.9(9) . . ? C26 C25 C27A 74.9(9) . . ? C24 C25 C27A 158.6(8) . . ? N30A C25 C27A 80.0(9) . . ? C26A C26 C25 36.5(8) . . ? C26A C26 C27 90.1(9) . . ? C25 C26 C27 119.1(5) . . ? C26A C26 C25A 39.5(9) . . ? C25 C26 C25A 6.6(6) . . ? C27 C26 C25A 116.8(6) . . ? C26A C26 H26 142(2) . . ? C25 C26 H26 118.5(18) . . ? C27 C26 H26 122.4(18) . . ? C25A C26 H26 120.0(18) . . ? C28 C27 C26 117.0(5) . . ? C28 C27 C27A 33.1(5) . . ? C26 C27 C27A 86.4(6) . . ? C28 C27 C26A 80.8(7) . . ? C26 C27 C26A 38.8(6) . . ? C27A C27 C26A 48.3(8) . . ? C28 C27 H27 132(3) . . ? C26 C27 H27 110(3) . . ? C27A C27 H27 163(3) . . ? C26A C27 H27 147(3) . . ? C27A C28 C29 42.2(16) . . ? C27A C28 C27 94.4(19) . . ? C29 C28 C27 125.2(5) . . ? C27A C28 H28 129(2) . . ? C29 C28 H28 103.7(17) . . ? C27 C28 H28 131.0(18) . . ? C27A C29 C29A 144.7(14) . . ? C27A C29 C28 43.7(11) . . ? C29A C29 C28 147.9(7) . . ? C27A C29 N30 81.0(12) . . ? C29A C29 N30 64.8(6) . . ? C28 C29 N30 115.8(5) . . ? C27A C29 C26A 38.0(11) . . ? C29A C29 C26A 106.8(8) . . ? C28 C29 C26A 71.4(6) . . ? N30 C29 C26A 45.2(5) . . ? C27A C29 H29 148(3) . . ? C29A C29 H29 65(3) . . ? C28 C29 H29 124(3) . . ? N30 C29 H29 121(3) . . ? C26A C29 H29 164(3) . . ? C25A N30 N30A 77.0(10) . . ? C25A N30 C25 30.1(7) . . ? N30A N30 C25 104.7(6) . . ? C25A N30 C29 145.0(10) . . ? N30A N30 C29 115.2(6) . . ? C25 N30 C29 119.3(5) . . ? C25A N30 C26A 63.5(8) . . ? N30A N30 C26A 137.2(9) . . ? C25 N30 C26A 33.7(6) . . ? C29 N30 C26A 90.9(7) . . ? C25A N30 C29A 133.2(11) . . ? N30A N30 C29A 62.6(8) . . ? C25 N30 C29A 143.8(6) . . ? C29 N30 C29A 53.6(6) . . ? C26A N30 C29A 138.4(9) . . ? C25A N30 C27A 118.7(14) . . ? N30A N30 C27A 147.3(9) . . ? C25 N30 C27A 88.8(11) . . ? C29 N30 C27A 35.5(8) . . ? C26A N30 C27A 56.8(12) . . ? C29A N30 C27A 88.8(11) . . ? C25 C25A N30 97(2) . . ? C25 C25A N30A 143(2) . . ? N30 C25A N30A 52.8(8) . . ? C25 C25A C26A 26.7(17) . . ? N30 C25A C26A 71.6(11) . . ? N30A C25A C26A 122.1(14) . . ? C25 C25A C24 90.0(19) . . ? N30 C25A C24 156.9(16) . . ? N30A C25A C24 126.0(12) . . ? C26A C25A C24 111.3(13) . . ? C25 C25A C26 13.3(13) . . ? N30 C25A C26 95.9(11) . . ? N30A C25A C26 134.1(11) . . ? C26A C25A C26 31.2(10) . . ? C24 C25A C26 96.1(8) . . ? C25 C26A C26 89.3(19) . . ? C25 C26A C25A 22.0(13) . . ? C26 C26A C25A 109.2(16) . . ? C25 C26A C27A 128(2) . . ? C26 C26A C27A 114.0(17) . . ? C25A C26A C27A 109.1(17) . . ? C25 C26A N30 66.4(13) . . ? C26 C26A N30 137.6(15) . . ? C25A C26A N30 44.9(8) . . ? C27A C26A N30 65.5(14) . . ? C25 C26A C27 128.7(19) . . ? C26 C26A C27 51.1(7) . . ? C25A C26A C27 136.6(15) . . ? C27A C26A C27 64.0(12) . . ? N30 C26A C27 118.8(10) . . ? C25 C26A C29 104.8(15) . . ? C26 C26A C29 121.7(12) . . ? C25A C26A C29 86.1(10) . . ? C27A C26A C29 23.2(10) . . ? N30 C26A C29 43.8(5) . . ? C27 C26A C29 78.7(6) . . ? C29 C27A C28 94.1(18) . . ? C29 C27A C26A 118.7(18) . . ? C28 C27A C26A 119(3) . . ? C29 C27A N30 63.5(14) . . ? C28 C27A N30 138.6(16) . . ? C26A C27A N30 57.7(8) . . ? C29 C27A C27 131.0(17) . . ? C28 C27A C27 52.5(16) . . ? C26A C27A C27 67.7(14) . . ? N30 C27A C27 115.6(12) . . ? C29 C27A C25 100.4(14) . . ? C28 C27A C25 122.7(19) . . ? C26A C27A C25 18.4(7) . . ? N30 C27A C25 41.4(4) . . ? C27 C27A C25 77.7(9) . . ? C29 C29A N30A 107.4(11) . . ? C29 C29A N30 61.7(8) . . ? N30A C29A N30 46.5(6) . . ? C29 C29A H29 38.1(18) . . ? N30A C29A H29 141(2) . . ? N30 C29A H29 95(2) . . ? N30 N30A C29A 70.9(9) . . ? N30 N30A C25A 50.2(8) . . ? C29A N30A C25A 116.8(12) . . ? N30 N30A C25 41.8(4) . . ? C29A N30A C25 105.2(9) . . ? C25A N30A C25 12.0(8) . . ? O35 B2 O32 106.81(15) . . ? O35 B2 C40 116.77(17) . . ? O32 B2 C40 117.20(16) . . ? O35 B2 N50 112.16(15) . . ? O32 B2 N50 105.73(15) . . ? C40 B2 N50 97.41(14) . . ? C33 O32 B2 107.22(14) . . ? O32 C33 C37 109.18(17) . . ? O32 C33 C36 108.94(16) . . ? C37 C33 C36 110.02(19) . . ? O32 C33 C34 101.74(15) . . ? C37 C33 C34 114.43(17) . . ? C36 C33 C34 112.11(18) . . ? O35 C34 C38 109.08(17) . . ? O35 C34 C39 109.03(17) . . ? C38 C34 C39 109.87(18) . . ? O35 C34 C33 102.08(14) . . ? C38 C34 C33 114.08(18) . . ? C39 C34 C33 112.32(18) . . ? B2 O35 C34 108.39(14) . . ? C33 C36 H36A 112.3(13) . . ? C33 C36 H36B 112.9(13) . . ? H36A C36 H36B 106.5(18) . . ? C33 C36 H36C 111.5(13) . . ? H36A C36 H36C 106.1(18) . . ? H36B C36 H36C 107.0(17) . . ? C33 C37 H37A 111.3(16) . . ? C33 C37 H37B 108.2(12) . . ? H37A C37 H37B 109(2) . . ? C33 C37 H37C 111.7(15) . . ? H37A C37 H37C 109(2) . . ? H37B C37 H37C 107.0(19) . . ? C34 C38 H38A 108.9(13) . . ? C34 C38 H38B 107.6(14) . . ? H38A C38 H38B 112.2(18) . . ? C34 C38 H38C 109.9(11) . . ? H38A C38 H38C 108.0(17) . . ? H38B C38 H38C 110.3(18) . . ? C34 C39 H39A 110.4(12) . . ? C34 C39 H39B 114.0(12) . . ? H39A C39 H39B 107.8(17) . . ? C34 C39 H39C 110.0(15) . . ? H39A C39 H39C 110.4(19) . . ? H39B C39 H39C 104.0(19) . . ? C45 C40 C41 117.61(18) . . ? C45 C40 B2 112.60(17) . . ? C41 C40 B2 129.72(18) . . ? C42 C41 C40 120.6(2) . . ? C42 C41 H41 117.4(12) . . ? C40 C41 H41 122.0(11) . . ? C43 C42 C41 120.4(2) . . ? C43 C42 H42 119.8(13) . . ? C41 C42 H42 119.8(13) . . ? C44 C43 C42 120.1(2) . . ? C44 C43 H43 121.8(12) . . ? C42 C43 H43 117.9(12) . . ? C43 C44 C45 119.2(2) . . ? C43 C44 H44 122.1(14) . . ? C45 C44 H44 118.7(14) . . ? C40 C45 C44 122.1(2) . . ? C40 C45 C46 114.43(17) . . ? C44 C45 C46 123.50(19) . . ? N47 C46 C45 113.41(17) . . ? N47 C46 N50 106.98(16) . . ? C45 C46 N50 104.87(16) . . ? N47 C46 H46 112.6(11) . . ? C45 C46 H46 112.0(11) . . ? N50 C46 H46 106.3(11) . . ? C46 N47 C48 102.31(16) . . ? C46 N47 C51 112.94(19) . . ? C48 N47 C51 113.3(2) . . ? N47 C48 C49 104.62(18) . . ? N47 C48 H48A 111.6(13) . . ? C49 C48 H48A 112.4(13) . . ? N47 C48 H48B 107.9(12) . . ? C49 C48 H48B 109.3(12) . . ? H48A C48 H48B 110.7(18) . . ? N50 C49 C48 103.03(18) . . ? N50 C49 H49A 110.1(14) . . ? C48 C49 H49A 114.1(14) . . ? N50 C49 H49B 108.6(14) . . ? C48 C49 H49B 114.1(14) . . ? H49A C49 H49B 107(2) . . ? C49 N50 C46 104.94(16) . . ? C49 N50 B2 115.35(16) . . ? C46 N50 B2 108.58(15) . . ? C49 N50 H50 109.4(14) . . ? C46 N50 H50 107.2(14) . . ? B2 N50 H50 110.9(14) . . ? N47 C51 C52 111.1(2) . . ? N47 C51 H51A 109.1(14) . . ? C52 C51 H51A 111.5(14) . . ? N47 C51 H51B 110.5(14) . . ? C52 C51 H51B 111.1(13) . . ? H51A C51 H51B 103(2) . . ? N53 C52 C51 110.0(2) . . ? N53 C52 H52A 111.5(16) . . ? C51 C52 H52A 107.3(16) . . ? N53 C52 H52B 110.5(16) . . ? C51 C52 H52B 111.3(15) . . ? H52A C52 H52B 106(2) . . ? C54 N53 C52 117.7(3) . . ? N53 C54 C55 122.6(3) . . ? N53 C54 H54 121.8(17) . . ? C55 C54 H54 115.5(17) . . ? N60 C55 C56 122.6(3) . . ? N60 C55 C54 115.2(2) . . ? C56 C55 C54 122.2(3) . . ? C57 C56 C55 118.6(3) . . ? C57 C56 H56 122.2(18) . . ? C55 C56 H56 119.2(18) . . ? C56 C57 C58 119.5(3) . . ? C56 C57 H57 115(2) . . ? C58 C57 H57 125(2) . . ? C59 C58 C57 118.1(3) . . ? C59 C58 H58 121.3(16) . . ? C57 C58 H58 120.2(16) . . ? N60 C59 C58 123.8(3) . . ? N60 C59 H59 116.5(18) . . ? C58 C59 H59 119.2(18) . . ? C55 N60 C59 117.4(2) . . ? O65 B3 O62 106.75(14) . . ? O65 B3 C70 114.25(16) . . ? O62 B3 C70 119.06(16) . . ? O65 B3 N80 114.26(15) . . ? O62 B3 N80 104.28(14) . . ? C70 B3 N80 97.80(13) . . ? C63 O62 B3 108.09(14) . . ? O62 C63 C67 109.67(16) . . ? O62 C63 C66 107.24(16) . . ? C67 C63 C66 109.03(18) . . ? O62 C63 C64 102.42(14) . . ? C67 C63 C64 114.70(18) . . ? C66 C63 C64 113.33(17) . . ? O65 C64 C68 107.72(17) . . ? O65 C64 C69 108.78(17) . . ? C68 C64 C69 109.56(18) . . ? O65 C64 C63 103.18(14) . . ? C68 C64 C63 114.31(18) . . ? C69 C64 C63 112.88(17) . . ? C64 O65 B3 108.95(14) . . ? C63 C66 H66A 112.8(15) . . ? C63 C66 H66B 109.0(11) . . ? H66A C66 H66B 106.8(18) . . ? C63 C66 H66C 108.6(13) . . ? H66A C66 H66C 105.8(19) . . ? H66B C66 H66C 113.9(17) . . ? C63 C67 H67A 110.7(13) . . ? C63 C67 H67B 112.2(13) . . ? H67A C67 H67B 108.8(19) . . ? C63 C67 H67C 110.5(13) . . ? H67A C67 H67C 107.3(18) . . ? H67B C67 H67C 107.1(19) . . ? C64 C68 H68A 107.7(14) . . ? C64 C68 H68B 110.2(13) . . ? H68A C68 H68B 106.0(19) . . ? C64 C68 H68C 114.5(14) . . ? H68A C68 H68C 110(2) . . ? H68B C68 H68C 108.1(19) . . ? C64 C69 H69A 112.2(11) . . ? C64 C69 H69B 110.0(12) . . ? H69A C69 H69B 111.5(16) . . ? C64 C69 H69C 114.4(14) . . ? H69A C69 H69C 101.7(18) . . ? H69B C69 H69C 106.7(18) . . ? C75 C70 C71 117.92(17) . . ? C75 C70 B3 112.98(16) . . ? C71 C70 B3 129.08(16) . . ? C72 C71 C70 120.68(18) . . ? C72 C71 H71 119.9(11) . . ? C70 C71 H71 119.4(11) . . ? C73 C72 C71 120.1(2) . . ? C73 C72 H72 119.2(12) . . ? C71 C72 H72 120.8(12) . . ? C74 C73 C72 120.5(2) . . ? C74 C73 H73 121.6(15) . . ? C72 C73 H73 117.9(15) . . ? C73 C74 C75 118.97(19) . . ? C73 C74 H74 121.5(15) . . ? C75 C74 H74 119.5(15) . . ? C74 C75 C70 121.88(18) . . ? C74 C75 C76 124.05(17) . . ? C70 C75 C76 114.01(15) . . ? N77 C76 C75 114.22(15) . . ? N77 C76 N80 106.78(14) . . ? C75 C76 N80 105.26(14) . . ? N77 C76 H76 111.5(11) . . ? C75 C76 H76 111.2(12) . . ? N80 C76 H76 107.4(11) . . ? C76 N77 C78 102.98(14) . . ? C76 N77 C81 113.05(16) . . ? C78 N77 C81 111.50(17) . . ? N77 C78 C79 104.74(17) . . ? N77 C78 H78A 105.3(12) . . ? C79 C78 H78A 112.2(12) . . ? N77 C78 H78B 109.4(14) . . ? C79 C78 H78B 112.4(14) . . ? H78A C78 H78B 112.3(19) . . ? N80 C79 C78 102.86(16) . . ? N80 C79 H79A 110.0(12) . . ? C78 C79 H79A 111.9(12) . . ? N80 C79 H79B 108.2(13) . . ? C78 C79 H79B 109.6(12) . . ? H79A C79 H79B 113.6(18) . . ? C79 N80 C76 105.03(14) . . ? C79 N80 B3 115.81(15) . . ? C76 N80 B3 109.06(13) . . ? C79 N80 H80 112.6(12) . . ? C76 N80 H80 105.9(11) . . ? B3 N80 H80 108.0(11) . . ? N77 C81 C82 110.29(17) . . ? N77 C81 H81A 114.0(12) . . ? C82 C81 H81A 108.6(12) . . ? N77 C81 H81B 107.0(12) . . ? C82 C81 H81B 106.4(11) . . ? H81A C81 H81B 110.3(16) . . ? N83 C82 C81 110.28(18) . . ? N83 C82 H82A 111.1(11) . . ? C81 C82 H82A 108.8(11) . . ? N83 C82 H82B 107.0(14) . . ? C81 C82 H82B 110.7(14) . . ? H82A C82 H82B 109.1(18) . . ? C84 N83 C82 115.6(2) . . ? N83 C84 C85 123.2(3) . . ? N83 C84 H84 126.1(17) . . ? C85 C84 H84 110.6(17) . . ? N90 C85 C86 124.0(3) . . ? N90 C85 C84 113.5(3) . . ? C86 C85 C84 122.6(3) . . ? C87 C86 C85 117.0(5) . . ? C87 C86 H86 121.4(19) . . ? C85 C86 H86 121.6(19) . . ? C88 C87 C86 120.7(6) . . ? C88 C87 H87 128(3) . . ? C86 C87 H87 111(4) . . ? C89 C88 C87 118.2(5) . . ? C89 C88 H88 113(3) . . ? C87 C88 H88 129(3) . . ? C88 C89 N90 125.1(6) . . ? C88 C89 H89 130(3) . . ? N90 C89 H89 104(3) . . ? C85 N90 C89 115.0(4) . . ? O95 B4 O92 106.29(16) . . ? O95 B4 C100 117.76(16) . . ? O92 B4 C100 116.50(16) . . ? O95 B4 N110 113.12(15) . . ? O92 B4 N110 104.95(14) . . ? C100 B4 N110 97.44(15) . . ? C93 O92 B4 107.90(14) . . ? O92 C93 C96 108.73(16) . . ? O92 C93 C97 108.25(17) . . ? C96 C93 C97 109.98(18) . . ? O92 C93 C94 102.25(14) . . ? C96 C93 C94 115.00(17) . . ? C97 C93 C94 112.13(17) . . ? O95 C94 C99 108.97(16) . . ? O95 C94 C98 108.47(16) . . ? C99 C94 C98 109.36(18) . . ? O95 C94 C93 101.83(14) . . ? C99 C94 C93 114.89(18) . . ? C98 C94 C93 112.87(16) . . ? B4 O95 C94 108.70(14) . . ? C93 C96 H96A 110.5(12) . . ? C93 C96 H96B 108.7(12) . . ? H96A C96 H96B 109.8(18) . . ? C93 C96 H96C 107.8(12) . . ? H96A C96 H96C 110.7(17) . . ? H96B C96 H96C 109.3(17) . . ? C93 C97 H97A 108.2(14) . . ? C93 C97 H97B 114.0(12) . . ? H97A C97 H97B 106.9(19) . . ? C93 C97 H97C 110.6(15) . . ? H97A C97 H97C 110(2) . . ? H97B C97 H97C 107.2(18) . . ? C94 C98 H98A 107.5(11) . . ? C94 C98 H98B 108.9(13) . . ? H98A C98 H98B 106.4(17) . . ? C94 C98 H98C 113.2(13) . . ? H98A C98 H98C 111.1(18) . . ? H98B C98 H98C 109.6(18) . . ? C94 C99 H99A 110.1(13) . . ? C94 C99 H99B 110.6(15) . . ? H99A C99 H99B 108.9(19) . . ? C94 C99 H99C 109.9(13) . . ? H99A C99 H99C 109.1(18) . . ? H99B C99 H99C 108(2) . . ? C105 C100 C101 117.83(18) . . ? C105 C100 B4 112.41(16) . . ? C101 C100 B4 129.66(19) . . ? C102 C101 C100 120.3(2) . . ? C102 C101 H101 119.2(12) . . ? C100 C101 H101 120.5(12) . . ? C103 C102 C101 120.3(2) . . ? C103 C102 H102 122.9(12) . . ? C101 C102 H102 116.7(12) . . ? C104 C103 C102 120.5(2) . . ? C104 C103 H103 119.3(14) . . ? C102 C103 H103 120.2(14) . . ? C103 C104 C105 118.3(2) . . ? C103 C104 H104 120.3(14) . . ? C105 C104 H104 121.4(14) . . ? C100 C105 C104 122.75(19) . . ? C100 C105 C106 114.54(16) . . ? C104 C105 C106 122.69(19) . . ? N107 C106 C105 113.86(16) . . ? N107 C106 N110 107.40(15) . . ? C105 C106 N110 104.76(15) . . ? N107 C106 H106 109.4(11) . . ? C105 C106 H106 112.9(10) . . ? N110 C106 H106 108.2(10) . . ? C106 N107 C108 102.77(15) . . ? C106 N107 C111 114.78(16) . . ? C108 N107 C111 112.93(17) . . ? N107 C108 C109 104.14(16) . . ? N107 C108 H108 106.3(11) . . ? C109 C108 H108 109.6(12) . . ? N107 C108 H128 110.2(13) . . ? C109 C108 H128 112.8(13) . . ? H108 C108 H128 113.2(18) . . ? N110 C109 C108 103.69(16) . . ? N110 C109 H109 107.3(12) . . ? C108 C109 H109 113.0(12) . . ? N110 C109 H129 106.9(12) . . ? C108 C109 H129 109.3(12) . . ? H109 C109 H129 115.8(17) . . ? C109 N110 C106 104.65(15) . . ? C109 N110 B4 116.80(15) . . ? C106 N110 B4 108.41(14) . . ? C109 N110 H110 110.2(13) . . ? C106 N110 H110 107.0(13) . . ? B4 N110 H110 109.2(13) . . ? N107 C111 C112 110.99(18) . . ? N107 C111 H111 106.0(12) . . ? C112 C111 H111 107.0(12) . . ? N107 C111 H131 111.9(14) . . ? C112 C111 H131 109.1(14) . . ? H111 C111 H131 111.8(18) . . ? N113 C112 C111 111.75(18) . . ? N113 C112 H112 110.9(13) . . ? C111 C112 H112 111.2(13) . . ? N113 C112 H132 109.2(12) . . ? C111 C112 H132 105.6(12) . . ? H112 C112 H132 107.9(17) . . ? C114 N113 C112 117.63(19) . . ? N113 C114 C115 122.1(2) . . ? N113 C114 H114 121.3(14) . . ? C115 C114 H114 116.6(13) . . ? N120 C115 C116 122.9(2) . . ? N120 C115 C114 114.8(2) . . ? C116 C115 C114 122.4(2) . . ? C115 C116 C117 119.0(3) . . ? C115 C116 H116 116.9(17) . . ? C117 C116 H116 123.8(18) . . ? C118 C117 C116 119.2(3) . . ? C118 C117 H117 121(2) . . ? C116 C117 H117 120(2) . . ? C117 C118 C119 118.3(3) . . ? C117 C118 H118 118.0(16) . . ? C119 C118 H118 123.7(16) . . ? N120 C119 C118 124.1(3) . . ? N120 C119 H119 112(2) . . ? C118 C119 H119 123(2) . . ? C115 N120 C119 116.5(3) . . ? C202 C201 H20A 109.5 . . ? C202 C201 H20B 109.5 . . ? H20A C201 H20B 109.5 . . ? C202 C201 H20C 109.5 . . ? H20A C201 H20C 109.5 . . ? H20B C201 H20C 109.5 . . ? C201 C202 O203 119.2(7) . . ? C201 C202 H20D 107.5 . . ? O203 C202 H20D 107.5 . . ? C201 C202 H20J 107.5 . . ? O203 C202 H20J 107.5 . . ? H20D C202 H20J 107.0 . . ? C204 O203 C202 118.1(7) . . ? O203 C204 C205 108.1(7) . . ? O203 C204 H20E 110.1 . . ? C205 C204 H20E 110.1 . . ? O203 C204 H20F 110.1 . . ? C205 C204 H20F 110.1 . . ? H20E C204 H20F 108.4 . . ? C204 C205 H20G 109.5 . . ? C204 C205 H20H 109.5 . . ? H20G C205 H20H 109.5 . . ? C204 C205 H20I 109.5 . . ? H20G C205 H20I 109.5 . . ? H20H C205 H20I 109.5 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.770 _refine_diff_density_min -0.794 _refine_diff_density_rms 0.050 data_sw_b _database_code_CSD 212669 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H27 B N2 O2' _chemical_formula_weight 302.22 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 Tetragonal _symmetry_space_group_name_H-M P-42(1)c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 12.5263(6) _cell_length_b 12.5263(6) _cell_length_c 21.7284(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3409.4(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.178 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 0.076 _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 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37188 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 32.49 _reflns_number_total 6166 _reflns_number_gt 4903 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0855P)^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 0.9(8) _refine_ls_number_reflns 6166 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1266 _refine_ls_wR_factor_gt 0.1166 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _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 B B 0.18280(10) 0.51203(10) 0.10597(7) 0.0222(2) Uani 1 1 d . . . O2 O 0.12153(7) 0.42568(7) 0.13546(5) 0.02504(18) Uani 1 1 d . . . C3 C 0.18864(10) 0.37934(11) 0.18200(6) 0.0279(2) Uani 1 1 d . . . C4 C 0.25629(11) 0.47699(11) 0.20245(6) 0.0288(3) Uani 1 1 d . . . O5 O 0.27114(7) 0.53460(7) 0.14589(4) 0.02515(18) Uani 1 1 d . . . C6 C 0.11983(14) 0.32993(14) 0.23201(8) 0.0394(3) Uani 1 1 d . . . C7 C 0.25877(12) 0.29356(12) 0.15303(8) 0.0373(3) Uani 1 1 d . . . C8 C 0.19450(15) 0.54910(14) 0.24748(8) 0.0404(3) Uani 1 1 d . . . C9 C 0.36474(13) 0.45079(15) 0.22919(9) 0.0432(4) Uani 1 1 d . . . C10 C 0.20849(10) 0.49793(9) 0.03391(6) 0.0244(2) Uani 1 1 d . . . C11 C 0.14348(10) 0.56166(9) -0.00311(6) 0.0244(2) Uani 1 1 d . . . C12 C 0.14647(13) 0.55622(11) -0.06751(7) 0.0330(3) Uani 1 1 d . . . C13 C 0.22071(15) 0.48834(12) -0.09504(7) 0.0383(3) Uani 1 1 d . . . C14 C 0.29050(15) 0.42930(12) -0.05947(8) 0.0394(3) Uani 1 1 d . . . C15 C 0.28367(12) 0.43220(11) 0.00460(7) 0.0317(3) Uani 1 1 d . . . C16 C 0.08027(10) 0.64271(9) 0.03199(6) 0.0241(2) Uani 1 1 d . . . N17 N 0.11989(10) 0.75067(8) 0.02157(5) 0.0270(2) Uani 1 1 d . . . C18 C 0.10995(11) 0.80739(9) 0.08097(6) 0.0267(2) Uani 1 1 d . . . C19 C 0.13655(11) 0.72004(10) 0.12813(6) 0.0269(2) Uani 1 1 d . . . N20 N 0.09813(8) 0.61785(8) 0.10014(5) 0.02231(19) Uani 1 1 d . . . C21 C 0.18887(14) 0.89979(11) 0.08404(8) 0.0364(3) Uani 1 1 d . . . C22 C -0.00445(13) 0.84631(12) 0.08857(8) 0.0369(3) Uani 1 1 d . . . H6A H 0.0615(17) 0.3759(17) 0.2459(10) 0.047(6) Uiso 1 1 d . . . H6B H 0.1658(18) 0.3064(18) 0.2664(10) 0.052(6) Uiso 1 1 d . . . H6C H 0.0821(19) 0.264(2) 0.2200(11) 0.056(6) Uiso 1 1 d . . . H7A H 0.3078(19) 0.3291(18) 0.1221(10) 0.051(6) Uiso 1 1 d . . . H7B H 0.2108(17) 0.2338(17) 0.1318(10) 0.049(5) Uiso 1 1 d . . . H7C H 0.3004(15) 0.2578(15) 0.1858(9) 0.037(5) Uiso 1 1 d . . . H8A H 0.2325(19) 0.6162(19) 0.2495(11) 0.056(6) Uiso 1 1 d . . . H8B H 0.1853(16) 0.5121(17) 0.2882(10) 0.041(5) Uiso 1 1 d . . . H8C H 0.1162(19) 0.5386(18) 0.2391(10) 0.049(6) Uiso 1 1 d . . . H9A H 0.4122(18) 0.4201(17) 0.1964(10) 0.050(6) Uiso 1 1 d . . . H9B H 0.3583(16) 0.4008(16) 0.2697(9) 0.041(5) Uiso 1 1 d . . . H9C H 0.3757(19) 0.521(2) 0.2499(11) 0.053(6) Uiso 1 1 d . . . H12 H 0.0969(14) 0.6020(14) -0.0909(8) 0.027(4) Uiso 1 1 d . . . H13 H 0.2144(18) 0.4867(18) -0.1391(11) 0.053(6) Uiso 1 1 d . . . H14 H 0.3456(17) 0.3807(18) -0.0768(10) 0.047(5) Uiso 1 1 d . . . H15 H 0.3394(12) 0.3863(13) 0.0258(8) 0.021(4) Uiso 1 1 d . . . H16 H 0.0049(15) 0.6403(14) 0.0244(8) 0.031(4) Uiso 1 1 d . . . H17 H 0.1908(12) 0.7437(12) 0.0118(7) 0.020(4) Uiso 1 1 d . . . H19A H 0.1003(14) 0.7296(14) 0.1648(8) 0.030(4) Uiso 1 1 d . . . H19B H 0.2172(15) 0.7112(15) 0.1339(9) 0.034(4) Uiso 1 1 d . . . H20 H 0.0390(19) 0.6050(18) 0.1163(10) 0.048(6) Uiso 1 1 d . . . H21A H 0.1810(17) 0.9365(17) 0.1232(10) 0.045(5) Uiso 1 1 d . . . H21B H 0.1814(19) 0.9474(18) 0.0503(12) 0.056(6) Uiso 1 1 d . . . H21C H 0.262(2) 0.871(2) 0.0847(12) 0.073(8) Uiso 1 1 d . . . H22A H -0.0257(17) 0.8996(17) 0.0564(10) 0.049(6) Uiso 1 1 d . . . H22B H -0.0154(19) 0.8826(19) 0.1298(11) 0.057(6) Uiso 1 1 d . . . H22C H -0.0533(15) 0.7933(16) 0.0895(9) 0.034(5) 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 B 0.0197(5) 0.0212(5) 0.0255(6) 0.0034(5) 0.0005(5) 0.0008(4) O2 0.0200(3) 0.0235(4) 0.0316(4) 0.0086(3) -0.0011(3) 0.0001(3) C3 0.0240(5) 0.0289(5) 0.0308(6) 0.0071(5) -0.0011(5) 0.0018(4) C4 0.0310(6) 0.0301(6) 0.0253(6) 0.0026(5) -0.0052(5) -0.0002(5) O5 0.0204(4) 0.0290(4) 0.0261(4) 0.0045(3) -0.0012(3) -0.0022(3) C6 0.0402(8) 0.0415(8) 0.0365(8) 0.0150(6) 0.0028(6) -0.0023(6) C7 0.0355(7) 0.0304(6) 0.0459(9) 0.0058(6) 0.0003(6) 0.0070(5) C8 0.0475(9) 0.0424(8) 0.0314(7) -0.0029(6) 0.0016(6) 0.0031(7) C9 0.0334(7) 0.0500(9) 0.0462(9) 0.0070(8) -0.0136(7) 0.0014(6) C10 0.0277(5) 0.0206(4) 0.0248(5) 0.0005(4) 0.0013(4) -0.0020(4) C11 0.0283(5) 0.0221(5) 0.0229(5) 0.0014(4) -0.0007(4) -0.0040(4) C12 0.0461(8) 0.0297(6) 0.0233(6) 0.0009(5) -0.0027(5) -0.0078(6) C13 0.0591(9) 0.0308(6) 0.0251(7) -0.0058(5) 0.0063(6) -0.0094(6) C14 0.0537(9) 0.0286(6) 0.0357(8) -0.0072(6) 0.0129(7) -0.0016(6) C15 0.0373(6) 0.0246(5) 0.0331(7) -0.0026(5) 0.0055(6) 0.0021(5) C16 0.0253(5) 0.0234(5) 0.0237(5) 0.0027(4) -0.0037(4) 0.0010(4) N17 0.0330(5) 0.0221(4) 0.0258(5) 0.0042(4) -0.0007(4) 0.0010(4) C18 0.0318(6) 0.0206(5) 0.0277(6) 0.0029(4) -0.0025(5) 0.0026(4) C19 0.0334(6) 0.0213(5) 0.0260(6) 0.0015(4) -0.0035(5) 0.0005(5) N20 0.0223(4) 0.0205(4) 0.0241(5) 0.0023(4) 0.0009(4) 0.0003(3) C21 0.0455(8) 0.0243(6) 0.0393(8) 0.0043(5) -0.0049(6) -0.0052(5) C22 0.0378(7) 0.0312(6) 0.0416(8) 0.0000(6) -0.0022(6) 0.0093(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 B O5 1.4341(16) . ? B O2 1.4731(15) . ? B C10 1.6082(19) . ? B N20 1.7023(16) . ? O2 C3 1.4373(15) . ? C3 C6 1.519(2) . ? C3 C7 1.5240(19) . ? C3 C4 1.5530(19) . ? C4 O5 1.4373(16) . ? C4 C9 1.514(2) . ? C4 C8 1.540(2) . ? C10 C11 1.3954(17) . ? C10 C15 1.4037(18) . ? C11 C12 1.4015(18) . ? C11 C16 1.4965(17) . ? C12 C13 1.395(2) . ? C13 C14 1.381(3) . ? C14 C15 1.395(2) . ? C16 N17 1.4582(16) . ? C16 N20 1.5297(17) . ? N17 C18 1.4786(17) . ? C18 C22 1.523(2) . ? C18 C21 1.5235(19) . ? C18 C19 1.5357(17) . ? C19 N20 1.4968(16) . ? 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 O5 B O2 106.48(10) . . ? O5 B C10 117.14(10) . . ? O2 B C10 116.56(10) . . ? O5 B N20 111.85(10) . . ? O2 B N20 106.23(9) . . ? C10 B N20 97.92(9) . . ? C3 O2 B 107.32(9) . . ? O2 C3 C6 109.63(11) . . ? O2 C3 C7 109.35(12) . . ? C6 C3 C7 109.59(12) . . ? O2 C3 C4 101.68(10) . . ? C6 C3 C4 115.21(12) . . ? C7 C3 C4 111.04(11) . . ? O5 C4 C9 108.72(12) . . ? O5 C4 C8 108.29(11) . . ? C9 C4 C8 109.53(13) . . ? O5 C4 C3 102.79(10) . . ? C9 C4 C3 115.39(12) . . ? C8 C4 C3 111.68(12) . . ? B O5 C4 108.56(9) . . ? C11 C10 C15 117.75(12) . . ? C11 C10 B 112.44(10) . . ? C15 C10 B 129.81(12) . . ? C10 C11 C12 122.15(13) . . ? C10 C11 C16 113.77(11) . . ? C12 C11 C16 123.78(12) . . ? C13 C12 C11 118.39(14) . . ? C14 C13 C12 120.56(14) . . ? C13 C14 C15 120.36(15) . . ? C14 C15 C10 120.60(14) . . ? N17 C16 C11 111.72(10) . . ? N17 C16 N20 106.82(10) . . ? C11 C16 N20 106.14(9) . . ? C16 N17 C18 106.35(10) . . ? N17 C18 C22 109.13(11) . . ? N17 C18 C21 110.40(12) . . ? C22 C18 C21 111.27(11) . . ? N17 C18 C19 102.82(9) . . ? C22 C18 C19 111.10(12) . . ? C21 C18 C19 111.80(12) . . ? N20 C19 C18 105.57(10) . . ? C19 N20 C16 105.44(9) . . ? C19 N20 B 115.81(9) . . ? C16 N20 B 108.76(9) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 32.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.542 _refine_diff_density_min -0.164 _refine_diff_density_rms 0.054 data_sw_c _database_code_CSD 212670 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H33 B N2 O3' _chemical_formula_weight 396.32 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5447(12) _cell_length_b 10.5484(13) _cell_length_c 10.9073(13) _cell_angle_alpha 95.987(2) _cell_angle_beta 92.320(2) _cell_angle_gamma 91.666(2) _cell_volume 1090.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelepi _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.207 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 428 _exptl_absorpt_coefficient_mu 0.079 _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 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5524 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3592 _reflns_number_gt 3226 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0673P)^2^+0.1226P] 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 3592 _refine_ls_number_parameters 394 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.1126 _refine_ls_wR_factor_gt 0.1099 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _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 B1 B 0.14222(14) 0.00272(13) 0.79509(13) 0.0267(3) Uani 1 1 d . . . O2 O 0.14992(9) -0.10526(8) 0.86201(8) 0.0290(2) Uani 1 1 d . . . C3 C 0.18754(14) -0.21213(12) 0.78036(13) 0.0347(3) Uani 1 1 d . . . C4 C 0.27562(14) -0.14864(12) 0.68707(13) 0.0352(3) Uani 1 1 d . . . O5 O 0.20572(9) -0.03132(8) 0.67827(8) 0.0308(2) Uani 1 1 d . . . C6 C 0.05484(17) -0.27871(14) 0.72174(17) 0.0450(4) Uani 1 1 d . . . C7 C 0.26522(19) -0.30225(15) 0.85567(17) 0.0479(4) Uani 1 1 d . . . C8 C 0.2771(2) -0.22004(17) 0.55999(16) 0.0507(4) Uani 1 1 d . . . C9 C 0.42473(15) -0.11528(16) 0.73594(16) 0.0434(4) Uani 1 1 d . . . C10 C 0.18578(12) 0.13684(11) 0.87056(11) 0.0269(3) Uani 1 1 d . . . C11 C 0.30149(13) 0.17086(12) 0.94891(12) 0.0310(3) Uani 1 1 d . . . C12 C 0.31765(14) 0.29204(13) 1.00908(13) 0.0359(3) Uani 1 1 d . . . C13 C 0.21756(15) 0.38151(13) 0.99276(13) 0.0370(3) Uani 1 1 d . . . C14 C 0.10110(14) 0.35005(12) 0.91599(13) 0.0335(3) Uani 1 1 d . . . C15 C 0.08733(13) 0.22828(11) 0.85519(11) 0.0275(3) Uani 1 1 d . . . C16 C -0.03166(12) 0.17892(11) 0.76678(12) 0.0266(3) Uani 1 1 d . . . N17 N -0.17133(10) 0.20656(10) 0.80787(10) 0.0304(3) Uani 1 1 d . . . C18 C -0.24381(13) 0.09109(12) 0.83552(13) 0.0323(3) Uani 1 1 d . . . C19 C -0.12680(13) 0.00116(12) 0.84771(12) 0.0303(3) Uani 1 1 d . . . N20 N -0.02401(10) 0.03810(9) 0.75914(10) 0.0256(2) Uani 1 1 d . . . C21 C -0.24402(13) 0.30764(12) 0.76953(12) 0.0306(3) Uani 1 1 d . . . C22 C -0.17859(15) 0.40380(12) 0.71299(13) 0.0350(3) Uani 1 1 d . . . C23 C -0.25426(17) 0.50305(14) 0.67579(15) 0.0427(4) Uani 1 1 d . . . C24 C -0.39504(17) 0.51063(14) 0.69573(16) 0.0488(4) Uani 1 1 d . . . C25 C -0.45929(16) 0.41820(15) 0.75434(15) 0.0464(4) Uani 1 1 d . . . C26 C -0.38663(14) 0.31689(14) 0.79077(14) 0.0382(3) Uani 1 1 d . . . C27 C 0.2568(3) 0.2726(3) 0.56081(18) 0.0893(9) Uani 1 1 d . . . C28 C 0.26448(17) 0.16111(19) 0.46753(16) 0.0530(4) Uani 1 1 d . . . O29 O 0.14876(11) 0.07547(10) 0.47089(9) 0.0446(3) Uani 1 1 d . . . H6A H 0.0073(19) -0.2227(17) 0.6651(16) 0.052(4) Uiso 1 1 d . . . H6B H -0.006(2) -0.3005(17) 0.7906(19) 0.062(5) Uiso 1 1 d . . . H6C H 0.0792(18) -0.3601(17) 0.6695(16) 0.050(4) Uiso 1 1 d . . . H7A H 0.2970(18) -0.3734(17) 0.8034(16) 0.049(4) Uiso 1 1 d . . . H7C H 0.200(2) -0.3357(18) 0.9133(19) 0.065(5) Uiso 1 1 d . . . H7B H 0.350(2) -0.2616(16) 0.9014(17) 0.054(5) Uiso 1 1 d . . . H8A H 0.182(2) -0.2335(17) 0.5243(17) 0.055(5) Uiso 1 1 d . . . H8C H 0.334(2) -0.1722(17) 0.5061(18) 0.056(5) Uiso 1 1 d . . . H8B H 0.3153(19) -0.3073(18) 0.5658(17) 0.055(5) Uiso 1 1 d . . . H9A H 0.4826(18) -0.1912(16) 0.7342(16) 0.048(4) Uiso 1 1 d . . . H9B H 0.4641(19) -0.0567(17) 0.6850(17) 0.054(5) Uiso 1 1 d . . . H9C H 0.4254(17) -0.0717(15) 0.8215(17) 0.044(4) Uiso 1 1 d . . . H11 H 0.3703(16) 0.1083(14) 0.9636(13) 0.032(3) Uiso 1 1 d . . . H12 H 0.3975(17) 0.3153(14) 1.0616(15) 0.040(4) Uiso 1 1 d . . . H13 H 0.2272(17) 0.4652(16) 1.0367(16) 0.047(4) Uiso 1 1 d . . . H14 H 0.0334(16) 0.4148(14) 0.9070(14) 0.037(4) Uiso 1 1 d . . . H16 H -0.0176(13) 0.2067(12) 0.6851(12) 0.022(3) Uiso 1 1 d . . . H18A H -0.2909(16) 0.1049(14) 0.9105(15) 0.037(4) Uiso 1 1 d . . . H18B H -0.3111(15) 0.0596(13) 0.7674(14) 0.031(3) Uiso 1 1 d . . . H19A H -0.0835(15) 0.0148(13) 0.9287(14) 0.030(3) Uiso 1 1 d . . . H19B H -0.1520(15) -0.0884(14) 0.8285(14) 0.034(4) Uiso 1 1 d . . . H20 H -0.0521(15) 0.0045(13) 0.6852(14) 0.028(3) Uiso 1 1 d . . . H22 H -0.0776(18) 0.4033(14) 0.6985(14) 0.040(4) Uiso 1 1 d . . . H23 H -0.2091(18) 0.5655(17) 0.6342(16) 0.048(4) Uiso 1 1 d . . . H24 H -0.446(2) 0.5828(18) 0.6734(18) 0.061(5) Uiso 1 1 d . . . H25 H -0.557(2) 0.4208(18) 0.7712(18) 0.063(5) Uiso 1 1 d . . . H26 H -0.4331(18) 0.2528(16) 0.8331(15) 0.043(4) Uiso 1 1 d . . . H27A H 0.262(3) 0.242(2) 0.638(3) 0.092(7) Uiso 1 1 d . . . H27B H 0.161(5) 0.325(5) 0.543(5) 0.22(2) Uiso 1 1 d . . . H27C H 0.333(3) 0.331(3) 0.550(3) 0.106(8) Uiso 1 1 d . . . H28A H 0.2642(18) 0.1899(16) 0.3849(17) 0.050(4) Uiso 1 1 d . . . H28B H 0.353(3) 0.115(2) 0.478(2) 0.086(7) Uiso 1 1 d . . . H29 H 0.159(2) 0.0311(19) 0.540(2) 0.069(6) 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 B1 0.0223(7) 0.0312(7) 0.0268(7) 0.0043(6) -0.0016(5) 0.0014(5) O2 0.0311(5) 0.0284(4) 0.0277(5) 0.0030(3) -0.0002(4) 0.0047(3) C3 0.0357(7) 0.0284(6) 0.0388(8) -0.0012(5) -0.0034(6) 0.0049(5) C4 0.0340(7) 0.0365(7) 0.0340(7) -0.0034(5) -0.0011(6) 0.0097(5) O5 0.0322(5) 0.0331(5) 0.0271(5) 0.0020(4) 0.0016(4) 0.0049(4) C6 0.0441(8) 0.0331(7) 0.0555(10) -0.0026(7) -0.0065(7) -0.0011(6) C7 0.0526(10) 0.0370(8) 0.0548(10) 0.0062(7) -0.0030(8) 0.0145(7) C8 0.0555(11) 0.0542(9) 0.0398(9) -0.0110(7) 0.0016(8) 0.0141(8) C9 0.0311(8) 0.0512(9) 0.0474(9) 0.0007(7) 0.0021(6) 0.0076(6) C10 0.0258(6) 0.0310(6) 0.0245(6) 0.0050(5) 0.0022(5) 0.0005(5) C11 0.0277(6) 0.0345(7) 0.0309(7) 0.0041(5) -0.0020(5) 0.0017(5) C12 0.0322(7) 0.0407(7) 0.0331(7) 0.0002(6) -0.0063(6) -0.0041(6) C13 0.0397(8) 0.0320(7) 0.0372(8) -0.0036(6) -0.0042(6) -0.0021(6) C14 0.0329(7) 0.0293(6) 0.0375(7) 0.0002(5) -0.0015(6) 0.0034(5) C15 0.0267(6) 0.0299(6) 0.0262(6) 0.0042(5) 0.0016(5) -0.0005(5) C16 0.0257(6) 0.0272(6) 0.0270(7) 0.0038(5) -0.0007(5) 0.0026(5) N17 0.0229(5) 0.0321(5) 0.0364(6) 0.0037(4) 0.0001(4) 0.0031(4) C18 0.0272(7) 0.0369(7) 0.0328(7) 0.0034(5) 0.0009(6) -0.0003(5) C19 0.0288(7) 0.0326(7) 0.0297(7) 0.0052(5) 0.0009(5) -0.0008(5) N20 0.0254(5) 0.0274(5) 0.0233(6) 0.0015(4) -0.0027(4) 0.0005(4) C21 0.0299(7) 0.0316(6) 0.0281(7) -0.0047(5) -0.0059(5) 0.0047(5) C22 0.0347(8) 0.0323(7) 0.0365(7) -0.0014(5) -0.0068(6) 0.0039(5) C23 0.0494(9) 0.0318(7) 0.0452(9) 0.0010(6) -0.0120(7) 0.0049(6) C24 0.0497(9) 0.0380(8) 0.0560(10) -0.0045(7) -0.0181(7) 0.0160(7) C25 0.0346(8) 0.0469(8) 0.0541(9) -0.0098(7) -0.0112(7) 0.0127(6) C26 0.0302(7) 0.0404(7) 0.0417(8) -0.0055(6) -0.0044(6) 0.0061(6) C27 0.130(2) 0.0977(16) 0.0356(10) 0.0094(10) -0.0060(11) -0.0755(17) C28 0.0394(9) 0.0814(12) 0.0399(9) 0.0192(8) -0.0010(7) -0.0079(8) O29 0.0515(6) 0.0501(6) 0.0317(6) 0.0084(5) -0.0094(4) -0.0083(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 B1 O2 1.4176(16) . ? B1 O5 1.4490(16) . ? B1 C10 1.5960(18) . ? B1 N20 1.6808(16) . ? O2 C3 1.4258(15) . ? C3 C7 1.5109(19) . ? C3 C6 1.515(2) . ? C3 C4 1.539(2) . ? C4 O5 1.4330(15) . ? C4 C8 1.508(2) . ? C4 C9 1.518(2) . ? C6 H6A 1.002(18) . ? C6 H6B 1.01(2) . ? C6 H6C 1.018(18) . ? C7 H7A 0.958(18) . ? C7 H7C 0.99(2) . ? C7 H7B 0.994(19) . ? C8 H8A 0.969(19) . ? C8 H8C 0.98(2) . ? C8 H8B 1.007(18) . ? C9 H9A 0.985(17) . ? C9 H9B 0.953(19) . ? C9 H9C 0.996(18) . ? C10 C15 1.3839(17) . ? C10 C11 1.3840(18) . ? C11 C12 1.3761(19) . ? C11 H11 0.965(15) . ? C12 C13 1.3815(19) . ? C12 H12 0.945(17) . ? C13 C14 1.3755(19) . ? C13 H13 0.959(18) . ? C14 C15 1.3829(18) . ? C14 H14 0.963(15) . ? C15 C16 1.5044(17) . ? C16 N17 1.4515(16) . ? C16 N20 1.4831(15) . ? C16 H16 0.980(13) . ? N17 C21 1.3805(16) . ? N17 C18 1.4483(17) . ? C18 C19 1.4970(18) . ? C18 H18A 0.949(16) . ? C18 H18B 0.986(15) . ? C19 N20 1.4767(16) . ? C19 H19A 0.955(15) . ? C19 H19B 0.968(15) . ? N20 H20 0.875(16) . ? C21 C22 1.387(2) . ? C21 C26 1.3944(19) . ? C22 C23 1.3752(19) . ? C22 H22 0.983(17) . ? C23 C24 1.373(2) . ? C23 H23 0.942(18) . ? C24 C25 1.365(3) . ? C24 H24 0.964(19) . ? C25 C26 1.375(2) . ? C25 H25 0.96(2) . ? C26 H26 0.965(17) . ? C27 C28 1.478(3) . ? C27 H27A 0.93(3) . ? C27 H27B 1.10(5) . ? C27 H27C 0.96(3) . ? C28 O29 1.411(2) . ? C28 H28A 0.981(19) . ? C28 H28B 0.99(2) . ? O29 H29 0.93(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 O2 B1 O5 106.80(10) . . ? O2 B1 C10 116.06(10) . . ? O5 B1 C10 118.56(10) . . ? O2 B1 N20 112.40(10) . . ? O5 B1 N20 105.64(9) . . ? C10 B1 N20 96.60(9) . . ? B1 O2 C3 108.66(10) . . ? O2 C3 C7 107.94(11) . . ? O2 C3 C6 108.78(11) . . ? C7 C3 C6 109.35(12) . . ? O2 C3 C4 102.14(10) . . ? C7 C3 C4 115.36(12) . . ? C6 C3 C4 112.79(12) . . ? O5 C4 C8 108.61(12) . . ? O5 C4 C9 107.53(11) . . ? C8 C4 C9 109.95(13) . . ? O5 C4 C3 102.09(10) . . ? C8 C4 C3 115.54(13) . . ? C9 C4 C3 112.50(12) . . ? C4 O5 B1 107.56(9) . . ? C3 C6 H6A 109.9(10) . . ? C3 C6 H6B 107.6(11) . . ? H6A C6 H6B 112.6(15) . . ? C3 C6 H6C 109.8(10) . . ? H6A C6 H6C 107.2(14) . . ? H6B C6 H6C 109.7(14) . . ? C3 C7 H7A 110.6(10) . . ? C3 C7 H7C 108.4(11) . . ? H7A C7 H7C 107.7(15) . . ? C3 C7 H7B 112.9(10) . . ? H7A C7 H7B 106.6(14) . . ? H7C C7 H7B 110.5(16) . . ? C4 C8 H8A 110.5(11) . . ? C4 C8 H8C 110.2(11) . . ? H8A C8 H8C 109.7(15) . . ? C4 C8 H8B 109.7(11) . . ? H8A C8 H8B 106.3(15) . . ? H8C C8 H8B 110.4(15) . . ? C4 C9 H9A 111.9(10) . . ? C4 C9 H9B 107.6(11) . . ? H9A C9 H9B 109.3(14) . . ? C4 C9 H9C 110.7(9) . . ? H9A C9 H9C 109.8(14) . . ? H9B C9 H9C 107.5(14) . . ? C15 C10 C11 117.89(11) . . ? C15 C10 B1 112.32(10) . . ? C11 C10 B1 129.75(11) . . ? C12 C11 C10 120.76(12) . . ? C12 C11 H11 119.5(9) . . ? C10 C11 H11 119.7(9) . . ? C11 C12 C13 120.30(12) . . ? C11 C12 H12 120.5(9) . . ? C13 C12 H12 119.2(9) . . ? C14 C13 C12 120.17(12) . . ? C14 C13 H13 119.4(10) . . ? C12 C13 H13 120.4(10) . . ? C13 C14 C15 118.76(12) . . ? C13 C14 H14 117.9(9) . . ? C15 C14 H14 123.4(9) . . ? C14 C15 C10 122.12(12) . . ? C14 C15 C16 125.64(11) . . ? C10 C15 C16 112.24(10) . . ? N17 C16 N20 105.07(9) . . ? N17 C16 C15 115.55(10) . . ? N20 C16 C15 104.75(9) . . ? N17 C16 H16 111.4(7) . . ? N20 C16 H16 109.2(7) . . ? C15 C16 H16 110.3(8) . . ? C21 N17 C18 121.27(10) . . ? C21 N17 C16 121.55(11) . . ? C18 N17 C16 110.54(10) . . ? N17 C18 C19 102.80(10) . . ? N17 C18 H18A 111.1(9) . . ? C19 C18 H18A 110.8(9) . . ? N17 C18 H18B 110.4(8) . . ? C19 C18 H18B 111.4(8) . . ? H18A C18 H18B 110.1(12) . . ? N20 C19 C18 104.39(10) . . ? N20 C19 H19A 108.2(8) . . ? C18 C19 H19A 110.2(8) . . ? N20 C19 H19B 108.8(9) . . ? C18 C19 H19B 115.7(9) . . ? H19A C19 H19B 109.3(12) . . ? C19 N20 C16 103.88(9) . . ? C19 N20 B1 114.21(9) . . ? C16 N20 B1 107.95(9) . . ? C19 N20 H20 108.5(9) . . ? C16 N20 H20 109.7(9) . . ? B1 N20 H20 112.2(9) . . ? N17 C21 C22 121.95(12) . . ? N17 C21 C26 119.84(12) . . ? C22 C21 C26 118.18(13) . . ? C23 C22 C21 120.42(14) . . ? C23 C22 H22 118.2(9) . . ? C21 C22 H22 121.4(9) . . ? C24 C23 C22 121.00(16) . . ? C24 C23 H23 119.6(10) . . ? C22 C23 H23 119.4(11) . . ? C25 C24 C23 118.89(14) . . ? C25 C24 H24 120.4(11) . . ? C23 C24 H24 120.6(11) . . ? C24 C25 C26 121.30(15) . . ? C24 C25 H25 121.4(11) . . ? C26 C25 H25 117.3(11) . . ? C25 C26 C21 120.17(15) . . ? C25 C26 H26 120.4(10) . . ? C21 C26 H26 119.4(10) . . ? C28 C27 H27A 107.2(15) . . ? C28 C27 H27B 110(3) . . ? H27A C27 H27B 114(3) . . ? C28 C27 H27C 108.3(17) . . ? H27A C27 H27C 112(2) . . ? H27B C27 H27C 105(3) . . ? O29 C28 C27 111.71(16) . . ? O29 C28 H28A 107.8(10) . . ? C27 C28 H28A 109.5(10) . . ? O29 C28 H28B 109.4(14) . . ? C27 C28 H28B 111.9(14) . . ? H28A C28 H28B 106.5(16) . . ? C28 O29 H29 109.3(13) . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 0.295 _refine_diff_density_min -0.223 _refine_diff_density_rms 0.039 data_sw_d _database_code_CSD 212671 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H54 B2 N4 O5' _chemical_formula_weight 620.43 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0250(16) _cell_length_b 10.9140(17) _cell_length_c 17.365(3) _cell_angle_alpha 106.609(2) _cell_angle_beta 105.779(2) _cell_angle_gamma 93.244(2) _cell_volume 1733.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Parallelepi _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.175 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.189 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 0.078 _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 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8934 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 24.99 _reflns_number_total 5738 _reflns_number_gt 3782 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0885P)^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 5738 _refine_ls_number_parameters 622 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0822 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1399 _refine_ls_wR_factor_gt 0.1320 _refine_ls_goodness_of_fit_ref 0.919 _refine_ls_restrained_S_all 0.919 _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 B1 B 0.0977(3) 0.4208(3) 0.36439(14) 0.0292(6) Uani 1 1 d . . . O2 O 0.13660(15) 0.34777(14) 0.29056(8) 0.0312(4) Uani 1 1 d . . . C3 C 0.2229(2) 0.2543(2) 0.31284(13) 0.0326(5) Uani 1 1 d . . . C4 C 0.1710(2) 0.2271(2) 0.38429(13) 0.0324(5) Uani 1 1 d . . . O5 O 0.13445(16) 0.35027(14) 0.42426(8) 0.0308(4) Uani 1 1 d . . . C6 C 0.2005(3) 0.1375(3) 0.23559(15) 0.0422(6) Uani 1 1 d . . . C7 C 0.3755(3) 0.3169(3) 0.34396(17) 0.0432(6) Uani 1 1 d . . . C8 C 0.0410(3) 0.1255(3) 0.35086(16) 0.0430(7) Uani 1 1 d . . . C9 C 0.2831(3) 0.1919(3) 0.45014(16) 0.0434(7) Uani 1 1 d . . . C10 C 0.1469(2) 0.5743(2) 0.40262(12) 0.0293(5) Uani 1 1 d . . . C11 C 0.0372(2) 0.6451(2) 0.38712(12) 0.0313(5) Uani 1 1 d . . . C12 C 0.0565(3) 0.7789(3) 0.41532(15) 0.0440(7) Uani 1 1 d . . . C13 C 0.1887(3) 0.8454(3) 0.46205(17) 0.0494(7) Uani 1 1 d . . . C14 C 0.3000(3) 0.7771(3) 0.47936(15) 0.0435(6) Uani 1 1 d . . . C15 C 0.2798(3) 0.6439(2) 0.44934(13) 0.0353(6) Uani 1 1 d . . . C16 C -0.1025(2) 0.5627(2) 0.34112(13) 0.0333(6) Uani 1 1 d . . . N17 N -0.2044(2) 0.5842(2) 0.38746(12) 0.0387(5) Uani 1 1 d . . . C18 C -0.2830(3) 0.4572(3) 0.36621(15) 0.0426(7) Uani 1 1 d . . . C19 C -0.1737(3) 0.3668(3) 0.36546(16) 0.0388(6) Uani 1 1 d . . . N20 N -0.07567(19) 0.42270(18) 0.32838(11) 0.0307(5) Uani 1 1 d . . . B21 B 0.8853(3) 0.4065(3) 0.10047(14) 0.0299(6) Uani 1 1 d . . . O22 O 0.82517(15) 0.33635(14) 0.14688(8) 0.0324(4) Uani 1 1 d . . . C23 C 0.7175(2) 0.2343(2) 0.08716(13) 0.0345(6) Uani 1 1 d . . . C24 C 0.7687(2) 0.2023(2) 0.00741(13) 0.0338(6) Uani 1 1 d . . . O25 O 0.83301(16) 0.32719(14) 0.01317(8) 0.0324(4) Uani 1 1 d . . . C26 C 0.5779(3) 0.2858(3) 0.07400(17) 0.0447(7) Uani 1 1 d . . . C27 C 0.7103(4) 0.1238(3) 0.12361(19) 0.0484(7) Uani 1 1 d . . . C28 C 0.8767(3) 0.1103(3) 0.00983(18) 0.0457(7) Uani 1 1 d . . . C29 C 0.6513(3) 0.1510(3) -0.07579(15) 0.0465(7) Uani 1 1 d . . . C30 C 0.8720(2) 0.5575(2) 0.11888(12) 0.0298(5) Uani 1 1 d . . . C31 C 1.0000(2) 0.6369(2) 0.16039(12) 0.0323(5) Uani 1 1 d . . . C32 C 1.0125(3) 0.7706(2) 0.18061(14) 0.0414(6) Uani 1 1 d . . . C33 C 0.8940(3) 0.8269(3) 0.15835(15) 0.0470(7) Uani 1 1 d . . . C34 C 0.7641(3) 0.7498(3) 0.11712(14) 0.0407(6) Uani 1 1 d . . . C35 C 0.7534(3) 0.6173(2) 0.09831(13) 0.0344(6) Uani 1 1 d . . . C36 C 1.1210(2) 0.5649(2) 0.17925(13) 0.0317(5) Uani 1 1 d . . . N37 N 1.2305(2) 0.5873(2) 0.14337(12) 0.0373(5) Uani 1 1 d . . . C38 C 1.2790(3) 0.4630(3) 0.11942(15) 0.0392(6) Uani 1 1 d . . . C39 C 1.1467(3) 0.3652(3) 0.08449(15) 0.0371(6) Uani 1 1 d . . . N40 N 1.06053(19) 0.42045(18) 0.14078(10) 0.0303(5) Uani 1 1 d . . . O41 O 0.4841(3) 0.9818(2) 0.31997(15) 0.0840(7) Uani 1 1 d . . . C42 C 0.4560(5) 0.8689(5) 0.3375(3) 0.0905(13) Uani 1 1 d . . . C43 C 0.5448(7) 0.7788(4) 0.3042(3) 0.122(2) Uani 1 1 d . . . C44 C 0.6713(6) 0.8686(7) 0.3157(3) 0.1144(19) Uani 1 1 d . . . C45 C 0.6114(5) 0.9799(5) 0.2993(2) 0.0994(17) Uani 1 1 d . . . H6A H 0.255(2) 0.067(2) 0.2506(14) 0.042(7) Uiso 1 1 d . . . H6B H 0.234(3) 0.159(3) 0.1911(18) 0.063(8) Uiso 1 1 d . . . H6C H 0.097(3) 0.099(2) 0.2092(16) 0.052(8) Uiso 1 1 d . . . H7A H 0.439(2) 0.250(2) 0.3510(14) 0.039(6) Uiso 1 1 d . . . H7B H 0.395(3) 0.351(2) 0.2987(16) 0.057(7) Uiso 1 1 d . . . H7C H 0.399(3) 0.395(2) 0.3992(16) 0.050(7) Uiso 1 1 d . . . H8A H 0.067(2) 0.040(2) 0.3336(14) 0.042(7) Uiso 1 1 d . . . H8B H -0.031(3) 0.145(2) 0.3066(16) 0.055(8) Uiso 1 1 d . . . H8C H -0.003(2) 0.130(2) 0.3994(15) 0.046(7) Uiso 1 1 d . . . H9A H 0.316(3) 0.111(3) 0.4249(16) 0.054(8) Uiso 1 1 d . . . H9B H 0.366(3) 0.269(3) 0.4812(16) 0.052(7) Uiso 1 1 d . . . H9C H 0.244(2) 0.172(2) 0.4944(15) 0.046(7) Uiso 1 1 d . . . H12 H -0.020(3) 0.824(2) 0.4077(14) 0.039(7) Uiso 1 1 d . . . H13 H 0.204(3) 0.939(3) 0.4854(15) 0.048(7) Uiso 1 1 d . . . H14 H 0.395(3) 0.824(2) 0.5081(15) 0.048(7) Uiso 1 1 d . . . H15 H 0.362(2) 0.598(2) 0.4609(13) 0.028(6) Uiso 1 1 d . . . H16 H -0.142(2) 0.5700(19) 0.2848(13) 0.029(6) Uiso 1 1 d . . . H17 H -0.155(3) 0.613(2) 0.4474(16) 0.046(7) Uiso 1 1 d . . . H18A H -0.351(3) 0.435(2) 0.3100(16) 0.049(7) Uiso 1 1 d . . . H18B H -0.332(3) 0.455(2) 0.4071(16) 0.051(7) Uiso 1 1 d . . . H19A H -0.206(3) 0.274(3) 0.3330(15) 0.049(7) Uiso 1 1 d . . . H19B H -0.116(2) 0.370(2) 0.4241(15) 0.037(6) Uiso 1 1 d . . . H20 H -0.102(2) 0.386(2) 0.2708(16) 0.040(6) Uiso 1 1 d . . . H26A H 0.494(3) 0.215(3) 0.0398(16) 0.054(7) Uiso 1 1 d . . . H26B H 0.573(3) 0.354(3) 0.0449(17) 0.061(8) Uiso 1 1 d . . . H26C H 0.563(3) 0.324(2) 0.1277(17) 0.055(8) Uiso 1 1 d . . . H27A H 0.647(3) 0.044(3) 0.0832(17) 0.061(8) Uiso 1 1 d . . . H27B H 0.805(3) 0.100(3) 0.1407(17) 0.063(9) Uiso 1 1 d . . . H27C H 0.667(3) 0.151(3) 0.1688(19) 0.069(9) Uiso 1 1 d . . . H28A H 0.828(3) 0.016(3) -0.0033(15) 0.052(7) Uiso 1 1 d . . . H28B H 0.917(3) 0.111(2) -0.0349(17) 0.056(8) Uiso 1 1 d . . . H28C H 0.952(3) 0.139(3) 0.0626(19) 0.064(9) Uiso 1 1 d . . . H29A H 0.596(3) 0.066(3) -0.0823(16) 0.057(8) Uiso 1 1 d . . . H29B H 0.694(3) 0.131(2) -0.1211(16) 0.048(7) Uiso 1 1 d . . . H29C H 0.580(2) 0.220(2) -0.0831(13) 0.037(6) Uiso 1 1 d . . . H32 H 1.109(3) 0.824(2) 0.2078(14) 0.040(7) Uiso 1 1 d . . . H33 H 0.899(2) 0.920(2) 0.1705(14) 0.043(7) Uiso 1 1 d . . . H34 H 0.681(2) 0.790(2) 0.1047(13) 0.035(6) Uiso 1 1 d . . . H35 H 0.663(2) 0.565(2) 0.0726(13) 0.032(6) Uiso 1 1 d . . . H36 H 1.165(2) 0.582(2) 0.2434(14) 0.032(6) Uiso 1 1 d . . . H37 H 1.196(2) 0.613(2) 0.0976(14) 0.035(6) Uiso 1 1 d . . . H38A H 1.336(3) 0.461(2) 0.0809(15) 0.047(7) Uiso 1 1 d . . . H38B H 1.338(2) 0.446(2) 0.1675(15) 0.042(6) Uiso 1 1 d . . . H39A H 1.095(2) 0.361(2) 0.0258(14) 0.031(6) Uiso 1 1 d . . . H39B H 1.156(2) 0.275(2) 0.0840(12) 0.029(6) Uiso 1 1 d . . . H40 H 1.081(3) 0.384(2) 0.1865(16) 0.052(7) Uiso 1 1 d . . . H42A H 0.370(5) 0.837(5) 0.315(3) 0.14(2) Uiso 1 1 d . . . H42B H 0.486(4) 0.892(4) 0.407(3) 0.133(15) Uiso 1 1 d . . . H43A H 0.525(4) 0.736(4) 0.244(3) 0.120(15) Uiso 1 1 d . . . H43B H 0.554(5) 0.723(5) 0.338(3) 0.144(17) Uiso 1 1 d . . . H44A H 0.737(5) 0.834(5) 0.280(3) 0.17(2) Uiso 1 1 d . . . H44B H 0.744(5) 0.897(4) 0.384(3) 0.162(18) Uiso 1 1 d . . . H45A H 0.593(4) 0.975(4) 0.243(3) 0.116(13) Uiso 1 1 d . . . H45B H 0.670(5) 1.067(4) 0.333(3) 0.141(17) 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 B1 0.0327(15) 0.0391(16) 0.0201(11) 0.0144(11) 0.0088(11) 0.0086(12) O2 0.0359(9) 0.0362(9) 0.0245(7) 0.0127(7) 0.0095(7) 0.0112(7) C3 0.0357(14) 0.0354(14) 0.0286(11) 0.0130(10) 0.0085(10) 0.0109(11) C4 0.0414(14) 0.0306(13) 0.0240(10) 0.0105(10) 0.0058(10) 0.0060(11) O5 0.0413(10) 0.0317(9) 0.0210(7) 0.0123(6) 0.0075(7) 0.0073(7) C6 0.0529(19) 0.0450(17) 0.0301(12) 0.0114(12) 0.0134(13) 0.0167(14) C7 0.0399(16) 0.0535(18) 0.0421(15) 0.0222(14) 0.0125(12) 0.0144(14) C8 0.0574(19) 0.0372(17) 0.0353(13) 0.0116(12) 0.0160(13) 0.0032(14) C9 0.0603(19) 0.0429(17) 0.0322(13) 0.0189(12) 0.0124(13) 0.0190(15) C10 0.0346(14) 0.0371(13) 0.0198(10) 0.0142(9) 0.0087(10) 0.0049(11) C11 0.0389(14) 0.0366(14) 0.0233(10) 0.0139(10) 0.0119(10) 0.0081(11) C12 0.0524(19) 0.0401(17) 0.0444(14) 0.0184(12) 0.0156(14) 0.0142(15) C13 0.063(2) 0.0317(16) 0.0508(16) 0.0117(13) 0.0154(15) 0.0030(15) C14 0.0472(17) 0.0405(17) 0.0387(13) 0.0117(12) 0.0094(13) -0.0048(14) C15 0.0390(15) 0.0385(15) 0.0302(12) 0.0144(11) 0.0098(11) 0.0047(12) C16 0.0392(15) 0.0423(15) 0.0226(11) 0.0137(10) 0.0112(10) 0.0124(11) N17 0.0365(12) 0.0546(14) 0.0274(10) 0.0146(10) 0.0101(9) 0.0144(10) C18 0.0344(15) 0.067(2) 0.0277(12) 0.0177(12) 0.0090(12) 0.0064(14) C19 0.0348(15) 0.0472(17) 0.0370(13) 0.0156(12) 0.0134(11) 0.0020(12) N20 0.0340(11) 0.0387(12) 0.0196(9) 0.0095(8) 0.0079(8) 0.0050(9) B21 0.0332(15) 0.0396(16) 0.0183(11) 0.0115(11) 0.0073(11) 0.0062(12) O22 0.0350(9) 0.0367(9) 0.0236(7) 0.0110(7) 0.0051(7) -0.0009(7) C23 0.0331(14) 0.0393(14) 0.0286(11) 0.0125(10) 0.0044(10) 0.0005(11) C24 0.0391(14) 0.0329(14) 0.0245(11) 0.0070(10) 0.0047(10) 0.0011(11) O25 0.0399(10) 0.0355(9) 0.0205(7) 0.0099(6) 0.0060(7) 0.0036(7) C26 0.0373(16) 0.0590(19) 0.0354(14) 0.0138(14) 0.0090(12) 0.0035(14) C27 0.055(2) 0.0461(18) 0.0448(15) 0.0211(14) 0.0112(15) -0.0029(16) C28 0.0531(19) 0.0379(17) 0.0454(16) 0.0114(13) 0.0151(15) 0.0080(14) C29 0.0519(18) 0.0532(19) 0.0255(12) 0.0068(12) 0.0056(12) -0.0031(16) C30 0.0348(14) 0.0384(14) 0.0186(10) 0.0117(9) 0.0095(10) 0.0042(11) C31 0.0404(15) 0.0375(14) 0.0201(10) 0.0107(10) 0.0093(10) 0.0047(12) C32 0.0475(17) 0.0382(16) 0.0332(12) 0.0089(11) 0.0068(12) 0.0046(13) C33 0.063(2) 0.0329(16) 0.0416(14) 0.0096(12) 0.0116(14) 0.0117(14) C34 0.0482(17) 0.0415(17) 0.0334(13) 0.0121(11) 0.0110(12) 0.0185(14) C35 0.0379(15) 0.0413(16) 0.0239(11) 0.0102(10) 0.0090(11) 0.0081(12) C36 0.0338(14) 0.0373(14) 0.0242(11) 0.0146(10) 0.0047(10) 0.0005(11) N37 0.0365(12) 0.0494(14) 0.0296(10) 0.0211(10) 0.0071(9) 0.0026(10) C38 0.0357(15) 0.0583(18) 0.0311(12) 0.0230(12) 0.0115(12) 0.0112(13) C39 0.0395(15) 0.0454(17) 0.0322(13) 0.0151(11) 0.0160(11) 0.0119(12) N40 0.0362(12) 0.0366(12) 0.0215(9) 0.0134(8) 0.0094(8) 0.0067(9) O41 0.0924(19) 0.0702(16) 0.0957(17) 0.0332(14) 0.0264(15) 0.0324(14) C42 0.067(3) 0.108(4) 0.116(4) 0.067(3) 0.026(3) 0.008(3) C43 0.138(5) 0.055(3) 0.102(3) 0.010(2) -0.065(3) 0.026(3) C44 0.093(4) 0.202(6) 0.054(2) 0.034(3) 0.028(2) 0.070(4) C45 0.100(4) 0.139(4) 0.047(2) 0.039(2) 0.002(2) -0.044(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 O5 1.446(3) . ? B1 O2 1.468(3) . ? B1 C10 1.607(3) . ? B1 N20 1.683(3) . ? O2 C3 1.443(3) . ? C3 C6 1.517(3) . ? C3 C7 1.523(4) . ? C3 C4 1.562(3) . ? C4 O5 1.443(3) . ? C4 C9 1.523(3) . ? C4 C8 1.524(3) . ? C10 C11 1.390(3) . ? C10 C15 1.398(3) . ? C11 C12 1.384(3) . ? C11 C16 1.499(3) . ? C12 C13 1.382(4) . ? C13 C14 1.390(4) . ? C14 C15 1.379(3) . ? C16 N17 1.453(3) . ? C16 N20 1.531(3) . ? N17 C18 1.451(3) . ? C18 C19 1.515(4) . ? C19 N20 1.501(3) . ? B21 O25 1.445(3) . ? B21 O22 1.471(3) . ? B21 C30 1.607(3) . ? B21 N40 1.685(3) . ? O22 C23 1.441(3) . ? C23 C27 1.520(3) . ? C23 C26 1.521(3) . ? C23 C24 1.560(3) . ? C24 O25 1.439(3) . ? C24 C28 1.519(4) . ? C24 C29 1.524(3) . ? C30 C31 1.389(3) . ? C30 C35 1.399(3) . ? C31 C32 1.390(3) . ? C31 C36 1.495(3) . ? C32 C33 1.380(4) . ? C33 C34 1.393(4) . ? C34 C35 1.379(3) . ? C36 N37 1.443(3) . ? C36 N40 1.539(3) . ? N37 C38 1.453(3) . ? C38 C39 1.516(4) . ? C39 N40 1.499(3) . ? O41 C42 1.383(5) . ? O41 C45 1.415(5) . ? C42 C43 1.466(7) . ? C43 C44 1.489(7) . ? C44 C45 1.451(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 B1 O2 105.53(18) . . ? O5 B1 C10 115.19(17) . . ? O2 B1 C10 118.98(17) . . ? O5 B1 N20 113.55(17) . . ? O2 B1 N20 105.16(16) . . ? C10 B1 N20 98.10(17) . . ? C3 O2 B1 109.05(15) . . ? O2 C3 C6 109.36(18) . . ? O2 C3 C7 108.18(19) . . ? C6 C3 C7 109.5(2) . . ? O2 C3 C4 102.16(16) . . ? C6 C3 C4 114.6(2) . . ? C7 C3 C4 112.68(18) . . ? O5 C4 C9 108.26(18) . . ? O5 C4 C8 108.8(2) . . ? C9 C4 C8 109.6(2) . . ? O5 C4 C3 102.57(16) . . ? C9 C4 C3 114.1(2) . . ? C8 C4 C3 113.09(18) . . ? C4 O5 B1 109.74(15) . . ? C11 C10 C15 117.2(2) . . ? C11 C10 B1 113.0(2) . . ? C15 C10 B1 129.8(2) . . ? C12 C11 C10 122.4(2) . . ? C12 C11 C16 124.1(2) . . ? C10 C11 C16 113.5(2) . . ? C13 C12 C11 119.4(3) . . ? C12 C13 C14 119.5(3) . . ? C15 C14 C13 120.5(3) . . ? C14 C15 C10 121.1(2) . . ? N17 C16 C11 114.07(18) . . ? N17 C16 N20 107.18(17) . . ? C11 C16 N20 106.08(18) . . ? C18 N17 C16 104.47(19) . . ? N17 C18 C19 104.5(2) . . ? N20 C19 C18 103.12(19) . . ? C19 N20 C16 104.77(17) . . ? C19 N20 B1 119.89(16) . . ? C16 N20 B1 109.06(17) . . ? O25 B21 O22 105.29(18) . . ? O25 B21 C30 115.92(17) . . ? O22 B21 C30 117.76(18) . . ? O25 B21 N40 113.24(17) . . ? O22 B21 N40 105.99(16) . . ? C30 B21 N40 98.35(17) . . ? C23 O22 B21 108.69(15) . . ? O22 C23 C27 108.52(19) . . ? O22 C23 C26 108.6(2) . . ? C27 C23 C26 109.1(2) . . ? O22 C23 C24 102.23(17) . . ? C27 C23 C24 114.6(2) . . ? C26 C23 C24 113.26(18) . . ? O25 C24 C28 109.7(2) . . ? O25 C24 C29 108.36(18) . . ? C28 C24 C29 109.5(2) . . ? O25 C24 C23 102.03(17) . . ? C28 C24 C23 112.53(19) . . ? C29 C24 C23 114.3(2) . . ? C24 O25 B21 109.74(15) . . ? C31 C30 C35 117.4(2) . . ? C31 C30 B21 112.9(2) . . ? C35 C30 B21 129.6(2) . . ? C30 C31 C32 122.3(2) . . ? C30 C31 C36 113.8(2) . . ? C32 C31 C36 123.9(2) . . ? C33 C32 C31 119.0(3) . . ? C32 C33 C34 120.0(3) . . ? C35 C34 C33 120.2(3) . . ? C34 C35 C30 121.1(2) . . ? N37 C36 C31 115.03(17) . . ? N37 C36 N40 107.44(17) . . ? C31 C36 N40 106.09(18) . . ? C36 N37 C38 104.73(18) . . ? N37 C38 C39 104.5(2) . . ? N40 C39 C38 103.12(19) . . ? C39 N40 C36 104.47(17) . . ? C39 N40 B21 119.92(16) . . ? C36 N40 B21 108.70(16) . . ? C42 O41 C45 108.2(3) . . ? O41 C42 C43 107.0(4) . . ? C42 C43 C44 101.6(4) . . ? C45 C44 C43 102.3(4) . . ? O41 C45 C44 107.4(3) . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 0.360 _refine_diff_density_min -0.271 _refine_diff_density_rms 0.076