# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_81128mae _database_code_depnum_ccdc_archive 'CCDC 894126' #TrackingRef '2a.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H49 B N2 O12' _chemical_formula_weight 796.65 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 'P 1 21 / c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.372(5) _cell_length_b 11.078(4) _cell_length_c 19.847(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.849(9) _cell_angle_gamma 90.00 _cell_volume 4002(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 0.096 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9535 _exptl_absorpt_correction_T_max 0.9810 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36795 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.47 _reflns_number_total 9024 _reflns_number_gt 6118 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0598P)^2^+0.2233P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9024 _refine_ls_number_parameters 529 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1250 _refine_ls_wR_factor_gt 0.1115 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 C1 C 0.06897(12) 0.37084(19) 0.32733(11) 0.0439(5) Uani 1 1 d . . . H1 H 0.1171 0.3539 0.3534 0.066 Uiso 1 1 calc R . . H2 H 0.0509 0.4486 0.3417 0.066 Uiso 1 1 calc R . . H3 H 0.0735 0.3739 0.2787 0.066 Uiso 1 1 calc R . . C2 C -0.05276(17) 0.1281(3) 0.45314(12) 0.0760(9) Uani 1 1 d . . . H4 H -0.0406 0.0526 0.4778 0.114 Uiso 1 1 calc R . . H5 H -0.0971 0.1631 0.4676 0.114 Uiso 1 1 calc R . . H6 H -0.0119 0.1851 0.4630 0.114 Uiso 1 1 calc R . . C3 C -0.00733(11) -0.25384(19) 0.37825(11) 0.0417(5) Uani 1 1 d . . . H7 H -0.0113 -0.2844 0.3316 0.063 Uiso 1 1 calc R . . H8 H -0.0399 -0.3004 0.4037 0.063 Uiso 1 1 calc R . . H9 H 0.0435 -0.2620 0.4003 0.063 Uiso 1 1 calc R . . C4 C 0.82741(10) -0.29502(18) -0.00815(11) 0.0414(5) Uani 1 1 d . . . H10 H 0.8195 -0.3165 0.0382 0.062 Uiso 1 1 calc R . . H11 H 0.8653 -0.3475 -0.0226 0.062 Uiso 1 1 calc R . . H12 H 0.7814 -0.3054 -0.0390 0.062 Uiso 1 1 calc R . . C5 C 0.91901(11) 0.0593(2) -0.06097(10) 0.0483(5) Uani 1 1 d . . . H13 H 0.8977 -0.0114 -0.0861 0.072 Uiso 1 1 calc R . . H14 H 0.9722 0.0604 -0.0616 0.072 Uiso 1 1 calc R . . H15 H 0.8972 0.1329 -0.0824 0.072 Uiso 1 1 calc R . . C6 C 0.78014(10) 0.33017(18) 0.06657(10) 0.0388(4) Uani 1 1 d . . . H16 H 0.7327 0.3420 0.0381 0.058 Uiso 1 1 calc R . . H17 H 0.8087 0.4051 0.0680 0.058 Uiso 1 1 calc R . . H18 H 0.7719 0.3083 0.1128 0.058 Uiso 1 1 calc R . . C7 C 0.11295(8) 0.00746(16) 0.28480(8) 0.0276(4) Uani 1 1 d . . . C8 C 0.09762(9) 0.12895(17) 0.29450(9) 0.0317(4) Uani 1 1 d . . . H19 H 0.1270 0.1897 0.2778 0.038 Uiso 1 1 calc R . . C9 C 0.03905(10) 0.16136(17) 0.32888(9) 0.0340(4) Uani 1 1 d . . . C10 C -0.00356(9) 0.07208(18) 0.35449(9) 0.0338(4) Uani 1 1 d . . . C11 C 0.01431(9) -0.04901(18) 0.34754(9) 0.0318(4) Uani 1 1 d . . . C12 C 0.07178(9) -0.08182(17) 0.31238(8) 0.0303(4) Uani 1 1 d . . . H20 H 0.0831 -0.1647 0.3071 0.036 Uiso 1 1 calc R . . C13 C 0.17166(9) -0.03056(16) 0.24543(8) 0.0272(4) Uani 1 1 d . . . C14 C 0.18462(9) -0.14367(17) 0.21931(9) 0.0320(4) Uani 1 1 d . . . H21 H 0.1567 -0.2146 0.2239 0.038 Uiso 1 1 calc R . . C15 C 0.24595(9) -0.13470(16) 0.18509(9) 0.0305(4) Uani 1 1 d . . . H22 H 0.2673 -0.1984 0.1624 0.037 Uiso 1 1 calc R . . C16 C 0.27008(8) -0.01607(15) 0.19028(8) 0.0260(3) Uani 1 1 d . . . C17 C 0.33332(9) 0.04080(15) 0.16858(8) 0.0243(3) Uani 1 1 d . . . C18 C 0.38239(8) -0.01990(16) 0.13297(8) 0.0258(3) Uani 1 1 d . . . H23 H 0.3716 -0.0993 0.1165 0.031 Uiso 1 1 calc R . . C19 C 0.44746(8) 0.03661(15) 0.12160(7) 0.0238(3) Uani 1 1 d . . . C20 C 0.50501(8) -0.02386(15) 0.09333(8) 0.0240(3) Uani 1 1 d . . . C21 C 0.51014(9) -0.14276(16) 0.07274(9) 0.0300(4) Uani 1 1 d . . . H24 H 0.4744 -0.2041 0.0749 0.036 Uiso 1 1 calc R . . C22 C 0.57725(9) -0.15610(16) 0.04833(9) 0.0296(4) Uani 1 1 d . . . H25 H 0.5953 -0.2283 0.0308 0.036 Uiso 1 1 calc R . . C23 C 0.61332(9) -0.04520(15) 0.05417(8) 0.0245(3) Uani 1 1 d . . . C24 C 0.68710(8) -0.01499(15) 0.03813(8) 0.0250(3) Uani 1 1 d . . . C25 C 0.73083(9) -0.10898(16) 0.01836(8) 0.0276(4) Uani 1 1 d . . . H26 H 0.7114 -0.1884 0.0124 0.033 Uiso 1 1 calc R . . C26 C 0.80283(9) -0.08542(17) 0.00743(8) 0.0289(4) Uani 1 1 d . . . C27 C 0.83137(9) 0.03082(17) 0.01433(8) 0.0304(4) Uani 1 1 d . . . C28 C 0.78694(9) 0.12501(16) 0.03255(8) 0.0294(4) Uani 1 1 d . . . C29 C 0.71472(9) 0.10227(16) 0.04426(8) 0.0274(4) Uani 1 1 d . . . H27 H 0.6847 0.1665 0.0563 0.033 Uiso 1 1 calc R . . C30 C 0.37390(8) 0.41531(15) 0.11587(8) 0.0248(3) Uani 1 1 d . . . C31 C 0.41379(9) 0.42783(15) 0.18053(8) 0.0262(3) Uani 1 1 d . . . C32 C 0.43029(9) 0.53978(16) 0.20852(8) 0.0312(4) Uani 1 1 d . . . H28 H 0.4580 0.5481 0.2523 0.037 Uiso 1 1 calc R . . C33 C 0.40470(10) 0.64094(17) 0.17013(9) 0.0341(4) Uani 1 1 d . . . H29 H 0.4154 0.7195 0.1881 0.041 Uiso 1 1 calc R . . C34 C 0.36416(10) 0.62842(16) 0.10656(9) 0.0319(4) Uani 1 1 d . . . H30 H 0.3469 0.6984 0.0817 0.038 Uiso 1 1 calc R . . C35 C 0.34808(9) 0.51412(15) 0.07824(8) 0.0279(4) Uani 1 1 d . . . H31 H 0.3203 0.5053 0.0345 0.033 Uiso 1 1 calc R . . C36 C 0.61498(11) 0.3515(2) 0.16569(10) 0.0428(5) Uani 1 1 d . . . H32 H 0.6609 0.3212 0.1922 0.051 Uiso 1 1 calc R . . H33 H 0.5737 0.3375 0.1920 0.051 Uiso 1 1 calc R . . C37 C 0.62164(12) 0.4841(2) 0.14928(11) 0.0496(5) Uani 1 1 d . . . H34 H 0.6722 0.5044 0.1411 0.059 Uiso 1 1 calc R . . H35 H 0.6082 0.5354 0.1865 0.059 Uiso 1 1 calc R . . C38 C 0.56688(10) 0.49943(17) 0.08462(9) 0.0355(4) Uani 1 1 d . . . H36 H 0.5213 0.5389 0.0948 0.043 Uiso 1 1 calc R . . H37 H 0.5883 0.5484 0.0505 0.043 Uiso 1 1 calc R . . C39 C 0.55146(10) 0.37104(17) 0.05897(9) 0.0319(4) Uani 1 1 d . . . H38 H 0.5000 0.3483 0.0627 0.038 Uiso 1 1 calc R . . H39 H 0.5592 0.3644 0.0107 0.038 Uiso 1 1 calc R . . C40 C 0.27734(11) 0.36392(19) 0.29723(9) 0.0416(5) Uani 1 1 d . . . H40 H 0.3271 0.3497 0.2850 0.050 Uiso 1 1 calc R . . H41 H 0.2763 0.3370 0.3447 0.050 Uiso 1 1 calc R . . C41 C 0.25668(12) 0.4954(2) 0.28912(10) 0.0464(5) Uani 1 1 d . . . H42 H 0.3008 0.5475 0.2971 0.056 Uiso 1 1 calc R . . H43 H 0.2223 0.5188 0.3211 0.056 Uiso 1 1 calc R . . C42 C 0.22004(13) 0.5049(2) 0.21578(11) 0.0481(5) Uani 1 1 d . . . H44 H 0.1720 0.5463 0.2133 0.058 Uiso 1 1 calc R . . H45 H 0.2515 0.5501 0.1878 0.058 Uiso 1 1 calc R . . C43 C 0.21019(10) 0.37535(18) 0.19161(9) 0.0364(4) Uani 1 1 d . . . H46 H 0.1598 0.3626 0.1677 0.044 Uiso 1 1 calc R . . H47 H 0.2458 0.3556 0.1600 0.044 Uiso 1 1 calc R . . O1 O 0.01835(7) 0.27738(13) 0.33934(7) 0.0453(3) Uani 1 1 d . . . O2 O -0.06521(7) 0.10467(14) 0.38285(7) 0.0485(4) Uani 1 1 d . . . O3 O -0.02815(7) -0.12983(13) 0.37715(7) 0.0400(3) Uani 1 1 d . . . O4 O 0.85062(6) -0.17216(12) -0.00960(7) 0.0379(3) Uani 1 1 d . . . O5 O 0.90416(6) 0.05316(13) 0.00820(7) 0.0388(3) Uani 1 1 d . . . O6 O 0.81941(7) 0.23624(12) 0.03882(7) 0.0389(3) Uani 1 1 d . . . O7 O 0.46041(6) 0.15054(10) 0.13907(6) 0.0283(3) Uani 1 1 d . . . O8 O 0.34483(6) 0.15408(11) 0.18701(6) 0.0297(3) Uani 1 1 d . . . O9 O 0.43207(6) 0.31733(11) 0.20796(6) 0.0286(3) Uani 1 1 d . . . O10 O 0.36526(6) 0.29669(10) 0.09911(5) 0.0263(3) Uani 1 1 d . . . O11 O 0.60159(6) 0.29340(12) 0.10071(6) 0.0352(3) Uani 1 1 d . . . O12 O 0.22289(7) 0.30116(12) 0.25132(6) 0.0362(3) Uani 1 1 d . . . N1 N 0.56889(7) 0.03425(12) 0.08188(6) 0.0235(3) Uani 1 1 d . . . H48 H 0.5793 0.1106 0.0910 0.028 Uiso 1 1 calc R . . N2 N 0.22374(7) 0.04678(13) 0.22717(7) 0.0261(3) Uani 1 1 d . . . H49 H 0.2272 0.1241 0.2373 0.031 Uiso 1 1 calc R . . B1 B 0.40080(10) 0.22794(18) 0.15869(9) 0.0269(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0539(12) 0.0318(12) 0.0499(11) -0.0001(9) 0.0215(10) 0.0040(9) C2 0.097(2) 0.086(2) 0.0528(13) 0.0082(13) 0.0405(15) 0.0428(17) C3 0.0353(10) 0.0427(13) 0.0497(11) 0.0071(9) 0.0146(9) -0.0046(8) C4 0.0348(9) 0.0367(12) 0.0538(11) -0.0102(9) 0.0106(9) 0.0060(8) C5 0.0386(10) 0.0595(15) 0.0518(11) 0.0117(10) 0.0243(10) 0.0059(9) C6 0.0323(9) 0.0305(11) 0.0539(11) -0.0022(8) 0.0067(9) -0.0040(8) C7 0.0220(8) 0.0337(10) 0.0279(8) 0.0012(7) 0.0065(7) 0.0010(7) C8 0.0292(8) 0.0355(11) 0.0322(8) 0.0004(7) 0.0102(8) 0.0014(7) C9 0.0333(9) 0.0350(11) 0.0350(9) -0.0001(7) 0.0096(8) 0.0046(8) C10 0.0263(8) 0.0429(12) 0.0342(9) -0.0004(8) 0.0112(8) 0.0031(7) C11 0.0228(8) 0.0419(12) 0.0320(8) 0.0021(8) 0.0081(8) -0.0039(7) C12 0.0257(8) 0.0329(10) 0.0333(8) 0.0009(7) 0.0072(8) 0.0015(7) C13 0.0247(8) 0.0287(10) 0.0293(8) 0.0022(7) 0.0077(7) 0.0010(7) C14 0.0304(8) 0.0281(10) 0.0398(9) 0.0012(7) 0.0127(8) -0.0019(7) C15 0.0284(8) 0.0282(10) 0.0371(9) -0.0020(7) 0.0121(8) 0.0014(7) C16 0.0249(8) 0.0272(9) 0.0267(7) 0.0003(7) 0.0070(7) 0.0031(7) C17 0.0259(8) 0.0245(9) 0.0226(7) 0.0018(6) 0.0028(7) 0.0016(6) C18 0.0255(8) 0.0248(9) 0.0281(7) -0.0019(6) 0.0075(7) -0.0009(6) C19 0.0246(8) 0.0239(9) 0.0231(7) 0.0011(6) 0.0044(7) 0.0016(6) C20 0.0222(7) 0.0254(9) 0.0251(7) 0.0003(6) 0.0064(7) -0.0020(6) C21 0.0275(8) 0.0267(10) 0.0377(9) -0.0030(7) 0.0113(8) -0.0029(7) C22 0.0280(8) 0.0252(10) 0.0374(9) -0.0059(7) 0.0109(8) 0.0009(7) C23 0.0245(8) 0.0257(9) 0.0239(7) 0.0002(6) 0.0050(7) 0.0015(6) C24 0.0238(8) 0.0288(10) 0.0232(7) 0.0012(6) 0.0064(7) 0.0018(6) C25 0.0265(8) 0.0297(10) 0.0273(7) -0.0014(7) 0.0066(7) 0.0009(7) C26 0.0260(8) 0.0348(11) 0.0270(8) 0.0004(7) 0.0079(7) 0.0052(7) C27 0.0218(8) 0.0404(11) 0.0306(8) 0.0018(7) 0.0096(7) -0.0003(7) C28 0.0283(8) 0.0306(10) 0.0305(8) 0.0026(7) 0.0089(8) -0.0015(7) C29 0.0250(8) 0.0290(10) 0.0289(8) 0.0016(7) 0.0060(7) 0.0022(7) C30 0.0271(8) 0.0209(9) 0.0288(7) -0.0043(6) 0.0128(7) -0.0024(6) C31 0.0284(8) 0.0256(9) 0.0268(7) -0.0012(6) 0.0113(7) 0.0002(7) C32 0.0343(9) 0.0305(10) 0.0296(8) -0.0066(7) 0.0073(8) -0.0035(7) C33 0.0429(10) 0.0233(10) 0.0390(9) -0.0086(7) 0.0159(9) -0.0045(8) C34 0.0399(10) 0.0229(10) 0.0351(8) 0.0010(7) 0.0128(8) 0.0008(7) C35 0.0307(8) 0.0267(10) 0.0274(7) 0.0002(7) 0.0080(7) 0.0000(7) C36 0.0391(10) 0.0533(14) 0.0344(9) -0.0012(9) -0.0005(9) 0.0059(9) C37 0.0480(12) 0.0444(14) 0.0537(12) -0.0180(10) -0.0024(11) -0.0005(10) C38 0.0414(10) 0.0313(11) 0.0359(9) -0.0021(7) 0.0125(9) -0.0008(8) C39 0.0331(9) 0.0327(11) 0.0311(8) -0.0018(7) 0.0085(8) -0.0036(7) C40 0.0471(11) 0.0474(13) 0.0316(9) -0.0065(8) 0.0102(9) -0.0046(9) C41 0.0560(12) 0.0408(13) 0.0447(10) -0.0138(9) 0.0148(10) -0.0071(10) C42 0.0546(12) 0.0378(13) 0.0526(11) 0.0013(9) 0.0101(11) 0.0012(10) C43 0.0321(9) 0.0427(12) 0.0356(9) -0.0043(8) 0.0088(8) -0.0024(8) O1 0.0458(8) 0.0358(8) 0.0600(8) 0.0004(6) 0.0282(7) 0.0078(6) O2 0.0367(7) 0.0584(10) 0.0560(8) -0.0047(7) 0.0269(7) 0.0043(6) O3 0.0323(6) 0.0419(9) 0.0502(7) 0.0043(6) 0.0217(6) -0.0024(6) O4 0.0295(6) 0.0375(8) 0.0494(7) -0.0040(6) 0.0156(6) 0.0062(5) O5 0.0249(6) 0.0501(9) 0.0442(7) 0.0014(6) 0.0149(6) -0.0027(5) O6 0.0320(6) 0.0323(8) 0.0554(8) -0.0006(6) 0.0172(6) -0.0060(5) O7 0.0284(6) 0.0227(7) 0.0361(6) -0.0014(5) 0.0126(5) -0.0001(5) O8 0.0307(6) 0.0231(7) 0.0386(6) -0.0010(5) 0.0164(6) 0.0012(5) O9 0.0321(6) 0.0255(7) 0.0284(5) -0.0010(5) 0.0045(5) 0.0017(5) O10 0.0296(6) 0.0208(6) 0.0290(5) -0.0040(4) 0.0066(5) -0.0013(5) O11 0.0326(6) 0.0302(7) 0.0434(7) -0.0041(5) 0.0076(6) 0.0020(5) O12 0.0416(7) 0.0327(8) 0.0369(6) -0.0047(5) 0.0145(6) -0.0046(6) N1 0.0232(6) 0.0215(8) 0.0270(6) -0.0010(5) 0.0072(6) -0.0005(5) N2 0.0265(7) 0.0242(8) 0.0291(6) 0.0005(6) 0.0094(6) 0.0017(5) B1 0.0280(9) 0.0232(10) 0.0310(9) -0.0004(7) 0.0095(8) 0.0011(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.433(2) . ? C1 H1 0.9800 . ? C1 H2 0.9800 . ? C1 H3 0.9800 . ? C2 O2 1.407(3) . ? C2 H4 0.9800 . ? C2 H5 0.9800 . ? C2 H6 0.9800 . ? C3 O3 1.425(2) . ? C3 H7 0.9800 . ? C3 H8 0.9800 . ? C3 H9 0.9800 . ? C4 O4 1.428(2) . ? C4 H10 0.9800 . ? C4 H11 0.9800 . ? C4 H12 0.9800 . ? C5 O5 1.437(2) . ? C5 H13 0.9800 . ? C5 H14 0.9800 . ? C5 H15 0.9800 . ? C6 O6 1.420(2) . ? C6 H16 0.9800 . ? C6 H17 0.9800 . ? C6 H18 0.9800 . ? C7 C8 1.394(3) . ? C7 C12 1.401(2) . ? C7 C13 1.477(2) . ? C8 C9 1.398(2) . ? C8 H19 0.9500 . ? C9 O1 1.364(2) . ? C9 C10 1.399(3) . ? C10 O2 1.380(2) . ? C10 C11 1.392(3) . ? C11 O3 1.371(2) . ? C11 C12 1.391(2) . ? C12 H20 0.9500 . ? C13 N2 1.370(2) . ? C13 C14 1.389(2) . ? C14 C15 1.396(2) . ? C14 H21 0.9500 . ? C15 C16 1.386(3) . ? C15 H22 0.9500 . ? C16 N2 1.384(2) . ? C16 C17 1.438(2) . ? C17 O8 1.316(2) . ? C17 C18 1.392(2) . ? C18 C19 1.395(2) . ? C18 H23 0.9500 . ? C19 O7 1.322(2) . ? C19 C20 1.430(2) . ? C20 N1 1.384(2) . ? C20 C21 1.386(2) . ? C21 C22 1.393(2) . ? C21 H24 0.9500 . ? C22 C23 1.393(2) . ? C22 H25 0.9500 . ? C23 N1 1.366(2) . ? C23 C24 1.473(2) . ? C24 C29 1.394(2) . ? C24 C25 1.403(2) . ? C25 C26 1.394(2) . ? C25 H26 0.9500 . ? C26 O4 1.375(2) . ? C26 C27 1.390(3) . ? C27 O5 1.3816(19) . ? C27 C28 1.402(2) . ? C28 O6 1.367(2) . ? C28 C29 1.401(2) . ? C29 H27 0.9500 . ? C30 O10 1.360(2) . ? C30 C35 1.373(2) . ? C30 C31 1.395(2) . ? C31 O9 1.363(2) . ? C31 C32 1.376(2) . ? C32 C33 1.400(3) . ? C32 H28 0.9500 . ? C33 C34 1.382(3) . ? C33 H29 0.9500 . ? C34 C35 1.400(2) . ? C34 H30 0.9500 . ? C35 H31 0.9500 . ? C36 O11 1.432(2) . ? C36 C37 1.514(3) . ? C36 H32 0.9900 . ? C36 H33 0.9900 . ? C37 C38 1.528(3) . ? C37 H34 0.9900 . ? C37 H35 0.9900 . ? C38 C39 1.524(3) . ? C38 H36 0.9900 . ? C38 H37 0.9900 . ? C39 O11 1.437(2) . ? C39 H38 0.9900 . ? C39 H39 0.9900 . ? C40 O12 1.437(2) . ? C40 C41 1.508(3) . ? C40 H40 0.9900 . ? C40 H41 0.9900 . ? C41 C42 1.522(3) . ? C41 H42 0.9900 . ? C41 H43 0.9900 . ? C42 C43 1.517(3) . ? C42 H44 0.9900 . ? C42 H45 0.9900 . ? C43 O12 1.435(2) . ? C43 H46 0.9900 . ? C43 H47 0.9900 . ? O7 B1 1.484(2) . ? O8 B1 1.484(2) . ? O9 B1 1.454(2) . ? O10 B1 1.481(2) . ? N1 H48 0.8800 . ? N2 H49 0.8800 . ? 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 O1 C1 H1 109.5 . . ? O1 C1 H2 109.5 . . ? H1 C1 H2 109.5 . . ? O1 C1 H3 109.5 . . ? H1 C1 H3 109.5 . . ? H2 C1 H3 109.5 . . ? O2 C2 H4 109.5 . . ? O2 C2 H5 109.5 . . ? H4 C2 H5 109.5 . . ? O2 C2 H6 109.5 . . ? H4 C2 H6 109.5 . . ? H5 C2 H6 109.5 . . ? O3 C3 H7 109.5 . . ? O3 C3 H8 109.5 . . ? H7 C3 H8 109.5 . . ? O3 C3 H9 109.5 . . ? H7 C3 H9 109.5 . . ? H8 C3 H9 109.5 . . ? O4 C4 H10 109.5 . . ? O4 C4 H11 109.5 . . ? H10 C4 H11 109.5 . . ? O4 C4 H12 109.5 . . ? H10 C4 H12 109.5 . . ? H11 C4 H12 109.5 . . ? O5 C5 H13 109.5 . . ? O5 C5 H14 109.5 . . ? H13 C5 H14 109.5 . . ? O5 C5 H15 109.5 . . ? H13 C5 H15 109.5 . . ? H14 C5 H15 109.5 . . ? O6 C6 H16 109.5 . . ? O6 C6 H17 109.5 . . ? H16 C6 H17 109.5 . . ? O6 C6 H18 109.5 . . ? H16 C6 H18 109.5 . . ? H17 C6 H18 109.5 . . ? C8 C7 C12 119.85(14) . . ? C8 C7 C13 121.62(15) . . ? C12 C7 C13 118.53(16) . . ? C7 C8 C9 119.94(16) . . ? C7 C8 H19 120.0 . . ? C9 C8 H19 120.0 . . ? O1 C9 C8 124.45(17) . . ? O1 C9 C10 115.41(15) . . ? C8 C9 C10 120.14(17) . . ? O2 C10 C11 120.68(16) . . ? O2 C10 C9 119.63(17) . . ? C11 C10 C9 119.58(15) . . ? O3 C11 C10 115.52(14) . . ? O3 C11 C12 124.03(17) . . ? C10 C11 C12 120.45(16) . . ? C11 C12 C7 119.93(17) . . ? C11 C12 H20 120.0 . . ? C7 C12 H20 120.0 . . ? N2 C13 C14 107.70(13) . . ? N2 C13 C7 123.28(15) . . ? C14 C13 C7 129.01(15) . . ? C13 C14 C15 107.95(16) . . ? C13 C14 H21 126.0 . . ? C15 C14 H21 126.0 . . ? C16 C15 C14 107.59(15) . . ? C16 C15 H22 126.2 . . ? C14 C15 H22 126.2 . . ? N2 C16 C15 107.62(13) . . ? N2 C16 C17 121.23(15) . . ? C15 C16 C17 130.99(14) . . ? O8 C17 C18 120.73(14) . . ? O8 C17 C16 116.10(13) . . ? C18 C17 C16 123.10(15) . . ? C17 C18 C19 119.61(16) . . ? C17 C18 H23 120.2 . . ? C19 C18 H23 120.2 . . ? O7 C19 C18 120.91(14) . . ? O7 C19 C20 115.73(13) . . ? C18 C19 C20 123.32(15) . . ? N1 C20 C21 107.47(13) . . ? N1 C20 C19 122.38(15) . . ? C21 C20 C19 130.14(14) . . ? C20 C21 C22 107.60(15) . . ? C20 C21 H24 126.2 . . ? C22 C21 H24 126.2 . . ? C21 C22 C23 108.13(15) . . ? C21 C22 H25 125.9 . . ? C23 C22 H25 125.9 . . ? N1 C23 C22 107.34(13) . . ? N1 C23 C24 123.98(15) . . ? C22 C23 C24 128.60(14) . . ? C29 C24 C25 120.02(14) . . ? C29 C24 C23 121.85(14) . . ? C25 C24 C23 118.09(15) . . ? C26 C25 C24 119.75(16) . . ? C26 C25 H26 120.1 . . ? C24 C25 H26 120.1 . . ? O4 C26 C27 115.26(14) . . ? O4 C26 C25 123.98(16) . . ? C27 C26 C25 120.75(15) . . ? O5 C27 C26 120.92(15) . . ? O5 C27 C28 119.60(16) . . ? C26 C27 C28 119.32(15) . . ? O6 C28 C29 123.93(15) . . ? O6 C28 C27 115.60(14) . . ? C29 C28 C27 120.46(16) . . ? C24 C29 C28 119.66(15) . . ? C24 C29 H27 120.2 . . ? C28 C29 H27 120.2 . . ? O10 C30 C35 128.14(15) . . ? O10 C30 C31 110.50(14) . . ? C35 C30 C31 121.36(16) . . ? O9 C31 C32 128.29(16) . . ? O9 C31 C30 110.36(14) . . ? C32 C31 C30 121.34(16) . . ? C31 C32 C33 117.57(16) . . ? C31 C32 H28 121.2 . . ? C33 C32 H28 121.2 . . ? C34 C33 C32 121.05(17) . . ? C34 C33 H29 119.5 . . ? C32 C33 H29 119.5 . . ? C33 C34 C35 121.00(17) . . ? C33 C34 H30 119.5 . . ? C35 C34 H30 119.5 . . ? C30 C35 C34 117.67(16) . . ? C30 C35 H31 121.2 . . ? C34 C35 H31 121.2 . . ? O11 C36 C37 104.56(16) . . ? O11 C36 H32 110.8 . . ? C37 C36 H32 110.8 . . ? O11 C36 H33 110.8 . . ? C37 C36 H33 110.8 . . ? H32 C36 H33 108.9 . . ? C36 C37 C38 103.01(16) . . ? C36 C37 H34 111.2 . . ? C38 C37 H34 111.2 . . ? C36 C37 H35 111.2 . . ? C38 C37 H35 111.2 . . ? H34 C37 H35 109.1 . . ? C39 C38 C37 104.36(16) . . ? C39 C38 H36 110.9 . . ? C37 C38 H36 110.9 . . ? C39 C38 H37 110.9 . . ? C37 C38 H37 110.9 . . ? H36 C38 H37 108.9 . . ? O11 C39 C38 106.90(14) . . ? O11 C39 H38 110.3 . . ? C38 C39 H38 110.3 . . ? O11 C39 H39 110.3 . . ? C38 C39 H39 110.3 . . ? H38 C39 H39 108.6 . . ? O12 C40 C41 104.85(16) . . ? O12 C40 H40 110.8 . . ? C41 C40 H40 110.8 . . ? O12 C40 H41 110.8 . . ? C41 C40 H41 110.8 . . ? H40 C40 H41 108.9 . . ? C40 C41 C42 103.96(16) . . ? C40 C41 H42 111.0 . . ? C42 C41 H42 111.0 . . ? C40 C41 H43 111.0 . . ? C42 C41 H43 111.0 . . ? H42 C41 H43 109.0 . . ? C43 C42 C41 104.76(17) . . ? C43 C42 H44 110.8 . . ? C41 C42 H44 110.8 . . ? C43 C42 H45 110.8 . . ? C41 C42 H45 110.8 . . ? H44 C42 H45 108.9 . . ? O12 C43 C42 106.38(15) . . ? O12 C43 H46 110.5 . . ? C42 C43 H46 110.5 . . ? O12 C43 H47 110.5 . . ? C42 C43 H47 110.5 . . ? H46 C43 H47 108.6 . . ? C9 O1 C1 117.03(14) . . ? C10 O2 C2 114.92(17) . . ? C11 O3 C3 117.93(13) . . ? C26 O4 C4 117.31(13) . . ? C27 O5 C5 113.87(14) . . ? C28 O6 C6 117.22(13) . . ? C19 O7 B1 120.50(13) . . ? C17 O8 B1 120.92(12) . . ? C31 O9 B1 106.86(13) . . ? C30 O10 B1 106.12(13) . . ? C36 O11 C39 105.55(13) . . ? C43 O12 C40 105.49(14) . . ? C23 N1 C20 109.45(14) . . ? C23 N1 H48 125.3 . . ? C20 N1 H48 125.3 . . ? C13 N2 C16 109.13(14) . . ? C13 N2 H49 125.4 . . ? C16 N2 H49 125.4 . . ? O9 B1 O10 106.11(14) . . ? O9 B1 O8 110.58(13) . . ? O10 B1 O8 109.47(14) . . ? O9 B1 O7 109.39(14) . . ? O10 B1 O7 110.38(13) . . ? O8 B1 O7 110.81(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 C7 C8 C9 -3.0(3) . . . . ? C13 C7 C8 C9 176.52(16) . . . . ? C7 C8 C9 O1 -178.12(17) . . . . ? C7 C8 C9 C10 1.0(3) . . . . ? O1 C9 C10 O2 5.0(3) . . . . ? C8 C9 C10 O2 -174.13(16) . . . . ? O1 C9 C10 C11 -178.64(16) . . . . ? C8 C9 C10 C11 2.2(3) . . . . ? O2 C10 C11 O3 -6.9(2) . . . . ? C9 C10 C11 O3 176.84(16) . . . . ? O2 C10 C11 C12 173.00(16) . . . . ? C9 C10 C11 C12 -3.3(3) . . . . ? O3 C11 C12 C7 -178.92(16) . . . . ? C10 C11 C12 C7 1.2(3) . . . . ? C8 C7 C12 C11 2.0(2) . . . . ? C13 C7 C12 C11 -177.60(15) . . . . ? C8 C7 C13 N2 13.0(3) . . . . ? C12 C7 C13 N2 -167.43(15) . . . . ? C8 C7 C13 C14 -165.59(18) . . . . ? C12 C7 C13 C14 14.0(3) . . . . ? N2 C13 C14 C15 0.44(19) . . . . ? C7 C13 C14 C15 179.20(17) . . . . ? C13 C14 C15 C16 -0.2(2) . . . . ? C14 C15 C16 N2 -0.2(2) . . . . ? C14 C15 C16 C17 175.26(17) . . . . ? N2 C16 C17 O8 1.3(2) . . . . ? C15 C16 C17 O8 -173.60(17) . . . . ? N2 C16 C17 C18 178.26(14) . . . . ? C15 C16 C17 C18 3.4(3) . . . . ? O8 C17 C18 C19 5.3(2) . . . . ? C16 C17 C18 C19 -171.51(15) . . . . ? C17 C18 C19 O7 -5.8(2) . . . . ? C17 C18 C19 C20 171.80(15) . . . . ? O7 C19 C20 N1 -2.9(2) . . . . ? C18 C19 C20 N1 179.38(15) . . . . ? O7 C19 C20 C21 177.07(16) . . . . ? C18 C19 C20 C21 -0.6(3) . . . . ? N1 C20 C21 C22 -0.39(19) . . . . ? C19 C20 C21 C22 179.59(16) . . . . ? C20 C21 C22 C23 0.2(2) . . . . ? C21 C22 C23 N1 0.15(19) . . . . ? C21 C22 C23 C24 176.93(16) . . . . ? N1 C23 C24 C29 -6.3(2) . . . . ? C22 C23 C24 C29 177.46(17) . . . . ? N1 C23 C24 C25 171.65(15) . . . . ? C22 C23 C24 C25 -4.6(2) . . . . ? C29 C24 C25 C26 2.5(2) . . . . ? C23 C24 C25 C26 -175.48(14) . . . . ? C24 C25 C26 O4 177.56(15) . . . . ? C24 C25 C26 C27 -1.5(2) . . . . ? O4 C26 C27 O5 -3.7(2) . . . . ? C25 C26 C27 O5 175.45(15) . . . . ? O4 C26 C27 C28 -179.12(14) . . . . ? C25 C26 C27 C28 0.0(3) . . . . ? O5 C27 C28 O6 4.0(2) . . . . ? C26 C27 C28 O6 179.46(15) . . . . ? O5 C27 C28 C29 -174.95(15) . . . . ? C26 C27 C28 C29 0.5(2) . . . . ? C25 C24 C29 C28 -1.9(2) . . . . ? C23 C24 C29 C28 175.96(14) . . . . ? O6 C28 C29 C24 -178.44(16) . . . . ? C27 C28 C29 C24 0.4(2) . . . . ? O10 C30 C31 O9 -0.26(17) . . . . ? C35 C30 C31 O9 178.88(13) . . . . ? O10 C30 C31 C32 179.35(13) . . . . ? C35 C30 C31 C32 -1.5(2) . . . . ? O9 C31 C32 C33 -179.61(14) . . . . ? C30 C31 C32 C33 0.9(2) . . . . ? C31 C32 C33 C34 0.2(2) . . . . ? C32 C33 C34 C35 -0.7(3) . . . . ? O10 C30 C35 C34 179.98(14) . . . . ? C31 C30 C35 C34 1.0(2) . . . . ? C33 C34 C35 C30 0.1(2) . . . . ? O11 C36 C37 C38 34.69(19) . . . . ? C36 C37 C38 C39 -16.15(19) . . . . ? C37 C38 C39 O11 -7.47(18) . . . . ? O12 C40 C41 C42 -29.89(19) . . . . ? C40 C41 C42 C43 9.9(2) . . . . ? C41 C42 C43 O12 13.4(2) . . . . ? C8 C9 O1 C1 -13.9(3) . . . . ? C10 C9 O1 C1 166.98(17) . . . . ? C11 C10 O2 C2 93.9(2) . . . . ? C9 C10 O2 C2 -89.9(2) . . . . ? C10 C11 O3 C3 -173.16(17) . . . . ? C12 C11 O3 C3 6.9(3) . . . . ? C27 C26 O4 C4 171.62(16) . . . . ? C25 C26 O4 C4 -7.5(2) . . . . ? C26 C27 O5 C5 79.7(2) . . . . ? C28 C27 O5 C5 -104.91(19) . . . . ? C29 C28 O6 C6 7.7(2) . . . . ? C27 C28 O6 C6 -171.16(15) . . . . ? C18 C19 O7 B1 -11.9(2) . . . . ? C20 C19 O7 B1 170.35(14) . . . . ? C18 C17 O8 B1 12.8(2) . . . . ? C16 C17 O8 B1 -170.14(14) . . . . ? C32 C31 O9 B1 179.17(15) . . . . ? C30 C31 O9 B1 -1.26(16) . . . . ? C35 C30 O10 B1 -177.44(15) . . . . ? C31 C30 O10 B1 1.62(16) . . . . ? C37 C36 O11 C39 -40.60(18) . . . . ? C38 C39 O11 C36 29.90(17) . . . . ? C42 C43 O12 C40 -32.88(18) . . . . ? C41 C40 O12 C43 39.39(17) . . . . ? C22 C23 N1 C20 -0.40(18) . . . . ? C24 C23 N1 C20 -177.36(14) . . . . ? C21 C20 N1 C23 0.50(17) . . . . ? C19 C20 N1 C23 -179.48(14) . . . . ? C14 C13 N2 C16 -0.55(18) . . . . ? C7 C13 N2 C16 -179.40(14) . . . . ? C15 C16 N2 C13 0.45(19) . . . . ? C17 C16 N2 C13 -175.52(14) . . . . ? C31 O9 B1 O10 2.18(15) . . . . ? C31 O9 B1 O8 -116.44(14) . . . . ? C31 O9 B1 O7 121.25(13) . . . . ? C30 O10 B1 O9 -2.32(15) . . . . ? C30 O10 B1 O8 117.03(13) . . . . ? C30 O10 B1 O7 -120.73(14) . . . . ? C17 O8 B1 O9 -149.16(14) . . . . ? C17 O8 B1 O10 94.29(17) . . . . ? C17 O8 B1 O7 -27.7(2) . . . . ? C19 O7 B1 O9 149.29(14) . . . . ? C19 O7 B1 O10 -94.32(17) . . . . ? C19 O7 B1 O8 27.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.209 _refine_diff_density_min -0.256 _refine_diff_density_rms 0.051 data_0119ma _database_code_depnum_ccdc_archive 'CCDC 894127' #TrackingRef '2a-TBACl.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H69 B Cl N3 O10' _chemical_formula_weight 930.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1540(2) _cell_length_b 19.3011(4) _cell_length_c 21.6869(4) _cell_angle_alpha 88.2974(9) _cell_angle_beta 78.0546(10) _cell_angle_gamma 82.5905(10) _cell_volume 4935.68(16) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.252 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1992 _exptl_absorpt_coefficient_mu 1.173 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.5917 _exptl_absorpt_correction_T_max 0.7199 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52386 _diffrn_reflns_av_R_equivalents 0.1075 _diffrn_reflns_av_sigmaI/netI 0.1320 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 68.25 _reflns_number_total 17410 _reflns_number_gt 9420 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1311P)^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 17410 _refine_ls_number_parameters 1211 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1282 _refine_ls_R_factor_gt 0.0837 _refine_ls_wR_factor_ref 0.2618 _refine_ls_wR_factor_gt 0.2251 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.005 _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 Cl2 Cl 0.70523(10) 0.18589(5) 0.33485(5) 0.0451(3) Uani 1 1 d . . . O1 O 0.7257(2) 0.47841(14) 0.17949(13) 0.0430(7) Uani 1 1 d . . . O2 O 0.3134(2) 0.03297(13) 0.14130(13) 0.0405(7) Uani 1 1 d . . . O3 O 0.6850(3) 0.22949(14) 0.64995(12) 0.0448(8) Uani 1 1 d . . . O17 O 0.6356(3) -0.03076(14) 0.19242(13) 0.0433(7) Uani 1 1 d . . . O4 O 0.3594(3) 0.10774(14) 0.23211(12) 0.0426(7) Uani 1 1 d . . . O18 O 0.3997(2) 0.54450(13) 0.12273(13) 0.0417(7) Uani 1 1 d . . . O5 O 0.7510(3) 0.43026(14) 0.06242(13) 0.0466(8) Uani 1 1 d . . . O6 O 0.3211(2) 0.08344(14) 0.02468(12) 0.0405(7) Uani 1 1 d . . . N2 N 0.6612(3) 0.15440(16) 0.19455(15) 0.0370(8) Uani 1 1 d . . . H32 H 0.6691 0.1647 0.2325 0.044 Uiso 1 1 calc R . . N3 N 0.3780(3) 0.35907(15) 0.13766(15) 0.0337(8) Uani 1 1 d . . . H33 H 0.3596 0.3493 0.1781 0.040 Uiso 1 1 calc R . . N4 N 0.3220(3) 0.47537(17) 0.35428(15) 0.0374(8) Uani 1 1 d . . . H34 H 0.3082 0.4361 0.3395 0.045 Uiso 1 1 calc R . . O7 O 0.2951(3) 0.27611(15) 0.60204(13) 0.0473(8) Uani 1 1 d . . . O8 O 0.6297(3) 0.40656(14) 0.27925(13) 0.0464(8) Uani 1 1 d . . . O19 O 0.6520(3) -0.08795(14) 0.29290(13) 0.0469(8) Uani 1 1 d . . . O9 O 0.7885(3) -0.12087(14) 0.19632(13) 0.0463(8) Uani 1 1 d . . . O20 O 0.3566(3) 0.60144(14) 0.22653(13) 0.0450(8) Uani 1 1 d . . . O10 O 0.2449(3) 0.63561(15) 0.14704(14) 0.0489(8) Uani 1 1 d . . . O11 O 0.4309(3) 0.66471(15) 0.13368(14) 0.0487(8) Uani 1 1 d . . . C52 C 0.3777(3) 0.2385(2) 0.10312(18) 0.0333(9) Uani 1 1 d . . . O12 O 0.6044(3) -0.15204(15) 0.21145(14) 0.0502(8) Uani 1 1 d . . . O13 O 0.7051(3) 0.09235(15) 0.68197(14) 0.0587(9) Uani 1 1 d . . . C55 C 0.4242(4) 0.4169(2) 0.04779(19) 0.0406(11) Uani 1 1 d . . . H35 H 0.4411 0.4530 0.0179 0.049 Uiso 1 1 calc R . . O14 O 0.6574(3) 0.26951(15) 0.53567(14) 0.0681(11) Uani 1 1 d . . . N5 N 0.6681(3) 0.03757(17) 0.41124(15) 0.0403(9) Uani 1 1 d . . . H36 H 0.6789 0.0779 0.3924 0.048 Uiso 1 1 calc R . . O15 O 0.2920(3) 0.40940(15) 0.63578(14) 0.0596(10) Uani 1 1 d . . . C59 C 0.3365(4) 0.5360(2) 0.3194(2) 0.0393(10) Uani 1 1 d . . . C60 C 0.6349(4) 0.3050(2) 0.2144(2) 0.0391(10) Uani 1 1 d . . . H1 H 0.6058 0.2777 0.2498 0.047 Uiso 1 1 calc R . . C61 C 0.3412(3) 0.1279(2) 0.06773(18) 0.0354(10) Uani 1 1 d . . . C62 C 0.3950(3) 0.3120(2) 0.09058(18) 0.0330(9) Uani 1 1 d . . . C63 C 0.3598(3) 0.1970(2) 0.05550(18) 0.0351(10) Uani 1 1 d . . . H37 H 0.3604 0.2159 0.0145 0.042 Uiso 1 1 calc R . . C64 C 0.6610(3) 0.2759(2) 0.15476(19) 0.0365(10) Uani 1 1 d . . . C65 C 0.3939(3) 0.4250(2) 0.11301(19) 0.0347(10) Uani 1 1 d . . . C66 C 0.6556(4) 0.0283(2) 0.21487(19) 0.0371(10) Uani 1 1 d . . . C67 C 0.3790(3) 0.2103(2) 0.16364(18) 0.0350(10) Uani 1 1 d . . . H38 H 0.3915 0.2383 0.1962 0.042 Uiso 1 1 calc R . . C68 C 0.6552(3) 0.2009(2) 0.14706(19) 0.0368(10) Uani 1 1 d . . . C69 C 0.6530(4) 0.0880(2) 0.17433(19) 0.0379(10) Uani 1 1 d . . . C70 C 0.6416(4) 0.0942(2) 0.11212(19) 0.0408(11) Uani 1 1 d . . . H2 H 0.6341 0.0576 0.0856 0.049 Uiso 1 1 calc R . . C71 C 0.6627(4) -0.0265(2) 0.3156(2) 0.0393(10) Uani 1 1 d . . . O16 O 0.3132(4) 0.24093(17) 0.48482(15) 0.0882(14) Uani 1 1 d . . . C73 C 0.3771(4) 0.4848(2) 0.15189(19) 0.0366(10) Uani 1 1 d . . . C74 C 0.3083(4) 0.3273(2) 0.55734(19) 0.0383(10) Uani 1 1 d . . . C75 C 0.3453(4) 0.4823(2) 0.21674(19) 0.0397(11) Uani 1 1 d . . . H39 H 0.3243 0.4401 0.2366 0.048 Uiso 1 1 calc R . . C76 C 0.6590(4) -0.0238(2) 0.3810(2) 0.0433(11) Uani 1 1 d . . . C77 C 0.4253(3) 0.3469(2) 0.03421(19) 0.0378(10) Uani 1 1 d . . . H40 H 0.4437 0.3266 -0.0066 0.045 Uiso 1 1 calc R . . C78 C 0.3067(4) 0.3965(2) 0.57268(19) 0.0430(11) Uani 1 1 d . . . C79 C 0.6741(4) 0.0310(2) 0.2756(2) 0.0414(11) Uani 1 1 d . . . H3 H 0.6947 0.0724 0.2900 0.050 Uiso 1 1 calc R . . C80 C 0.6987(4) 0.3164(2) 0.1021(2) 0.0382(10) Uani 1 1 d . . . H4 H 0.7137 0.2970 0.0610 0.046 Uiso 1 1 calc R . . C81 C 0.3435(4) 0.5397(2) 0.2530(2) 0.0400(10) Uani 1 1 d . . . C82 C 0.3407(4) 0.0995(2) 0.12760(19) 0.0359(10) Uani 1 1 d . . . C83 C 0.3818(4) 0.1472(2) 0.28187(19) 0.0426(11) Uani 1 1 d . . . H41 H 0.4554 0.1645 0.2683 0.064 Uiso 1 1 calc R . . H42 H 0.3831 0.1174 0.3191 0.064 Uiso 1 1 calc R . . H43 H 0.3222 0.1869 0.2923 0.064 Uiso 1 1 calc R . . C84 C 0.6771(4) 0.1787(2) 0.60817(19) 0.0406(11) Uani 1 1 d . . . C85 C 0.6432(3) 0.1650(2) 0.0959(2) 0.0409(10) Uani 1 1 d . . . H5 H 0.6369 0.1847 0.0560 0.049 Uiso 1 1 calc R . . C86 C 0.7142(4) 0.3855(2) 0.1105(2) 0.0404(10) Uani 1 1 d . . . C87 C 0.3527(4) 0.5538(2) 0.4192(2) 0.0537(13) Uani 1 1 d . . . H44 H 0.3631 0.5754 0.4560 0.064 Uiso 1 1 calc R . . C88 C 0.2524(4) 0.6988(2) 0.1179(2) 0.0453(11) Uani 1 1 d . . . C89 C 0.6648(4) 0.0801(2) 0.51945(19) 0.0398(10) Uani 1 1 d . . . C90 C 0.6578(4) 0.0255(2) 0.4743(2) 0.0448(11) Uani 1 1 d . . . C91 C 0.6851(4) 0.1083(2) 0.6236(2) 0.0441(11) Uani 1 1 d . . . C92 C 0.3614(3) 0.1401(2) 0.17516(18) 0.0352(10) Uani 1 1 d . . . C93 C 0.8758(4) -0.2106(2) 0.1163(2) 0.0516(12) Uani 1 1 d . . . H6 H 0.9491 -0.1958 0.1083 0.062 Uiso 1 1 calc R . . C94 C 0.3323(4) 0.4852(2) 0.4147(2) 0.0415(11) Uani 1 1 d . . . C95 C 0.6651(4) 0.1992(2) 0.5475(2) 0.0446(11) Uani 1 1 d . . . C96 C 0.3228(4) 0.4300(2) 0.46369(19) 0.0418(11) Uani 1 1 d . . . C97 C 0.3891(5) 0.7811(2) 0.0850(2) 0.0542(13) Uani 1 1 d . . . H45 H 0.4626 0.7945 0.0817 0.065 Uiso 1 1 calc R . . C98 C 0.6510(4) 0.3740(2) 0.22275(19) 0.0377(10) Uani 1 1 d . . . C99 C 0.3162(4) 0.4480(2) 0.5258(2) 0.0441(11) Uani 1 1 d . . . H46 H 0.3182 0.4951 0.5365 0.053 Uiso 1 1 calc R . . C100 C 0.6390(5) -0.0435(2) 0.4847(2) 0.0594(15) Uani 1 1 d . . . H7 H 0.6273 -0.0663 0.5245 0.071 Uiso 1 1 calc R . . C101 C 0.3199(4) 0.1100(2) -0.03766(19) 0.0430(11) Uani 1 1 d . . . H47 H 0.2626 0.1510 -0.0355 0.065 Uiso 1 1 calc R . . H48 H 0.3016 0.0738 -0.0633 0.065 Uiso 1 1 calc R . . H49 H 0.3946 0.1233 -0.0568 0.065 Uiso 1 1 calc R . . C102 C 0.6942(4) 0.4138(2) 0.1707(2) 0.0404(10) Uani 1 1 d . . . C103 C 0.3552(4) 0.5853(2) 0.3609(2) 0.0485(12) Uani 1 1 d . . . H50 H 0.3675 0.6323 0.3507 0.058 Uiso 1 1 calc R . . C104 C 0.7874(4) -0.1772(2) 0.1602(2) 0.0455(12) Uani 1 1 d . . . C105 C 0.3611(4) 0.7174(2) 0.1113(2) 0.0456(11) Uani 1 1 d . . . C106 C 0.7476(5) -0.2897(2) 0.0975(2) 0.0532(13) Uani 1 1 d . . . H8 H 0.7363 -0.3301 0.0768 0.064 Uiso 1 1 calc R . . C107 C 0.6580(5) -0.2549(2) 0.1403(2) 0.0567(14) Uani 1 1 d . . . H9 H 0.5849 -0.2699 0.1487 0.068 Uiso 1 1 calc R . . C108 C 0.6401(4) -0.0736(2) 0.4278(2) 0.0525(13) Uani 1 1 d . . . H10 H 0.6296 -0.1206 0.4217 0.063 Uiso 1 1 calc R . . C109 C 0.5755(4) 0.3680(2) 0.3319(2) 0.0507(12) Uani 1 1 d . . . H11 H 0.5061 0.3535 0.3229 0.076 Uiso 1 1 calc R . . H12 H 0.5564 0.3975 0.3695 0.076 Uiso 1 1 calc R . . H13 H 0.6270 0.3265 0.3392 0.076 Uiso 1 1 calc R . . C110 C 0.3150(4) 0.3103(2) 0.4953(2) 0.0522(13) Uani 1 1 d . . . C111 C 0.6593(4) 0.1502(2) 0.5030(2) 0.0450(12) Uani 1 1 d . . . H14 H 0.6516 0.1646 0.4617 0.054 Uiso 1 1 calc R . . C112 C 0.1689(5) 0.7412(2) 0.0946(2) 0.0552(13) Uani 1 1 d . . . H51 H 0.0955 0.7277 0.0973 0.066 Uiso 1 1 calc R . . C113 C 0.3204(4) 0.3608(2) 0.4480(2) 0.0491(12) Uani 1 1 d . . . H52 H 0.3223 0.3483 0.4057 0.059 Uiso 1 1 calc R . . C114 C 0.8530(5) -0.2664(2) 0.0845(2) 0.0566(13) Uani 1 1 d . . . H15 H 0.9112 -0.2894 0.0530 0.068 Uiso 1 1 calc R . . C115 C 0.6768(4) 0.0597(2) 0.5799(2) 0.0493(12) Uani 1 1 d . . . H16 H 0.6793 0.0117 0.5913 0.059 Uiso 1 1 calc R . . C116 C 0.4062(4) -0.0209(2) 0.1198(2) 0.0469(12) Uani 1 1 d . . . H53 H 0.4303 -0.0178 0.0739 0.070 Uiso 1 1 calc R . . H54 H 0.3815 -0.0668 0.1311 0.070 Uiso 1 1 calc R . . H55 H 0.4697 -0.0148 0.1396 0.070 Uiso 1 1 calc R . . C117 C 0.6798(4) -0.1974(2) 0.1704(2) 0.0467(12) Uani 1 1 d . . . C118 C 0.7610(4) 0.4069(2) -0.0003(2) 0.0527(13) Uani 1 1 d . . . H17 H 0.8240 0.3691 -0.0101 0.079 Uiso 1 1 calc R . . H18 H 0.7755 0.4458 -0.0297 0.079 Uiso 1 1 calc R . . H19 H 0.6905 0.3897 -0.0044 0.079 Uiso 1 1 calc R . . B1 B 0.3594(5) 0.6107(3) 0.1582(3) 0.0463(13) Uani 1 1 d . . . C120 C 0.1974(5) 0.8043(3) 0.0672(2) 0.0627(15) Uani 1 1 d . . . H56 H 0.1425 0.8343 0.0504 0.075 Uiso 1 1 calc R . . B2 B 0.6699(5) -0.0978(3) 0.2243(2) 0.0451(13) Uani 1 1 d . . . C122 C 0.3029(5) 0.8241(3) 0.0637(2) 0.0597(14) Uani 1 1 d . . . H57 H 0.3178 0.8685 0.0464 0.072 Uiso 1 1 calc R . . C123 C 0.6098(4) 0.2302(2) 0.7116(2) 0.0515(13) Uani 1 1 d . . . H20 H 0.5407 0.2106 0.7083 0.077 Uiso 1 1 calc R . . H21 H 0.5897 0.2783 0.7269 0.077 Uiso 1 1 calc R . . H22 H 0.6481 0.2021 0.7412 0.077 Uiso 1 1 calc R . . C124 C 0.3167(5) 0.4750(2) 0.6542(2) 0.0607(14) Uani 1 1 d . . . H58 H 0.3944 0.4818 0.6336 0.091 Uiso 1 1 calc R . . H59 H 0.3094 0.4758 0.7000 0.091 Uiso 1 1 calc R . . H60 H 0.2635 0.5126 0.6416 0.091 Uiso 1 1 calc R . . C125 C 0.6453(4) 0.5360(2) 0.1712(2) 0.0528(13) Uani 1 1 d . . . H23 H 0.6272 0.5335 0.1294 0.079 Uiso 1 1 calc R . . H24 H 0.6768 0.5795 0.1749 0.079 Uiso 1 1 calc R . . H25 H 0.5762 0.5347 0.2037 0.079 Uiso 1 1 calc R . . C126 C 0.3824(4) 0.2630(3) 0.6388(2) 0.0610(14) Uani 1 1 d . . . H61 H 0.4567 0.2662 0.6114 0.092 Uiso 1 1 calc R . . H62 H 0.3812 0.2161 0.6574 0.092 Uiso 1 1 calc R . . H63 H 0.3686 0.2977 0.6724 0.092 Uiso 1 1 calc R . . C127 C 0.6778(5) 0.0262(2) 0.7078(2) 0.0674(16) Uani 1 1 d . . . H26 H 0.5983 0.0222 0.7077 0.101 Uiso 1 1 calc R . . H27 H 0.6898 0.0224 0.7512 0.101 Uiso 1 1 calc R . . H28 H 0.7266 -0.0114 0.6823 0.101 Uiso 1 1 calc R . . N1 N 0.0060(3) 0.25827(18) 0.21456(17) 0.0444(9) Uani 1 1 d . . . C3 C 0.0841(4) 0.3005(2) 0.1696(2) 0.0453(11) Uani 1 1 d . . . H67 H 0.1216 0.3284 0.1948 0.054 Uiso 1 1 calc R . . H68 H 0.1440 0.2677 0.1438 0.054 Uiso 1 1 calc R . . C156 C 0.1208(4) 0.3833(2) 0.0797(2) 0.0534(13) Uani 1 1 d . . . H69 H 0.1610 0.4109 0.1036 0.064 Uiso 1 1 calc R . . H70 H 0.1768 0.3464 0.0564 0.064 Uiso 1 1 calc R . . C7 C 0.0301(4) 0.3493(2) 0.1258(2) 0.0467(11) Uani 1 1 d . . . H71 H -0.0242 0.3860 0.1506 0.056 Uiso 1 1 calc R . . H72 H -0.0122 0.3230 0.1021 0.056 Uiso 1 1 calc R . . C9 C 0.0690(4) 0.4309(2) 0.0329(2) 0.0558(13) Uani 1 1 d . . . H73 H 0.0282 0.4038 0.0096 0.084 Uiso 1 1 calc R . . H74 H 0.1295 0.4507 0.0032 0.084 Uiso 1 1 calc R . . H75 H 0.0163 0.4689 0.0557 0.084 Uiso 1 1 calc R . . C132 C 0.3288(9) 0.2205(3) 0.4213(3) 0.160(4) Uani 1 1 d . . . H64 H 0.2669 0.2443 0.4029 0.240 Uiso 1 1 calc R . . H65 H 0.3289 0.1698 0.4192 0.240 Uiso 1 1 calc R . . H66 H 0.4013 0.2332 0.3977 0.240 Uiso 1 1 calc R . . C131 C 0.6393(7) 0.2921(3) 0.4746(2) 0.106(3) Uani 1 1 d . . . H29 H 0.7097 0.2808 0.4432 0.158 Uiso 1 1 calc R . . H30 H 0.6166 0.3427 0.4750 0.158 Uiso 1 1 calc R . . H31 H 0.5794 0.2683 0.4637 0.158 Uiso 1 1 calc R . . C1 C 0.0812(4) 0.2106(2) 0.2501(2) 0.0515(12) Uani 1 1 d . . . H76 H 0.1234 0.2402 0.2709 0.062 Uiso 1 1 calc R . . H77 H 0.1377 0.1812 0.2189 0.062 Uiso 1 1 calc R . . C133 C -0.0840(4) 0.3052(2) 0.2593(2) 0.0474(12) Uani 1 1 d . . . H78 H -0.1297 0.3352 0.2336 0.057 Uiso 1 1 calc R . . H79 H -0.1352 0.2751 0.2857 0.057 Uiso 1 1 calc R . . C134 C -0.0446(4) 0.3523(2) 0.3030(2) 0.0564(13) Uani 1 1 d . . . H80 H -0.1020 0.3569 0.3428 0.068 Uiso 1 1 calc R . . H81 H 0.0266 0.3285 0.3131 0.068 Uiso 1 1 calc R . . C140 C 0.0168(4) 0.1706(3) 0.1260(2) 0.0568(13) Uani 1 1 d . . . H82 H 0.0710 0.1370 0.1436 0.068 Uiso 1 1 calc R . . H83 H 0.0609 0.2000 0.0945 0.068 Uiso 1 1 calc R . . C142 C 0.0131(4) 0.0872(3) 0.0384(2) 0.0635(14) Uani 1 1 d . . . H84 H 0.0516 0.1181 0.0067 0.095 Uiso 1 1 calc R . . H85 H -0.0369 0.0620 0.0196 0.095 Uiso 1 1 calc R . . H86 H 0.0696 0.0536 0.0532 0.095 Uiso 1 1 calc R . . C146 C -0.0570(4) 0.1306(3) 0.0938(3) 0.0641(15) Uani 1 1 d . . . H87 H -0.0978 0.0994 0.1250 0.077 Uiso 1 1 calc R . . H88 H -0.1142 0.1643 0.0787 0.077 Uiso 1 1 calc R . . C191 C -0.0566(4) 0.2162(2) 0.1783(2) 0.0467(12) Uani 1 1 d . . . H89 H -0.1016 0.1860 0.2086 0.056 Uiso 1 1 calc R . . H90 H -0.1106 0.2490 0.1598 0.056 Uiso 1 1 calc R . . C207 C 0.0963(4) 0.3741(2) 0.7822(2) 0.0533(13) Uani 1 1 d . . . H91 H 0.1343 0.4006 0.7459 0.064 Uiso 1 1 calc R . . H92 H 0.1551 0.3409 0.7965 0.064 Uiso 1 1 calc R . . C208 C 0.0688(4) 0.2810(3) 0.7106(2) 0.0544(13) Uani 1 1 d . . . H93 H 0.1223 0.3042 0.6783 0.065 Uiso 1 1 calc R . . H94 H 0.1141 0.2433 0.7298 0.065 Uiso 1 1 calc R . . C209 C 0.0127(4) 0.3337(3) 0.7610(2) 0.0555(13) Uani 1 1 d . . . H95 H -0.0438 0.3668 0.7446 0.067 Uiso 1 1 calc R . . H96 H -0.0281 0.3092 0.7977 0.067 Uiso 1 1 calc R . . C210 C 0.0407(4) 0.4247(3) 0.8353(2) 0.0630(14) Uani 1 1 d . . . H97 H -0.0194 0.4567 0.8220 0.095 Uiso 1 1 calc R . . H98 H 0.0977 0.4515 0.8457 0.095 Uiso 1 1 calc R . . H99 H 0.0082 0.3984 0.8725 0.095 Uiso 1 1 calc R . . C203 C -0.1179(5) 0.1020(3) 0.7906(3) 0.0688(16) Uani 1 1 d . . . H100 H -0.1415 0.0776 0.7569 0.083 Uiso 1 1 calc R . . H101 H -0.1866 0.1281 0.8165 0.083 Uiso 1 1 calc R . . C204 C -0.0922(4) 0.2100(3) 0.7240(2) 0.0564(13) Uani 1 1 d . . . H102 H -0.1410 0.2444 0.7540 0.068 Uiso 1 1 calc R . . H103 H -0.1417 0.1893 0.7006 0.068 Uiso 1 1 calc R . . C205 C -0.0641(6) 0.0483(3) 0.8319(3) 0.093(2) Uani 1 1 d . . . H104 H 0.0059 0.0237 0.8069 0.139 Uiso 1 1 calc R . . H105 H -0.1170 0.0145 0.8479 0.139 Uiso 1 1 calc R . . H106 H -0.0464 0.0719 0.8673 0.139 Uiso 1 1 calc R . . N8 N -0.0092(3) 0.2480(2) 0.67780(17) 0.0538(11) Uani 1 1 d . . . C206 C -0.0374(5) 0.1530(3) 0.7610(2) 0.0667(15) Uani 1 1 d . . . H107 H -0.0090 0.1745 0.7945 0.080 Uiso 1 1 calc R . . H108 H 0.0285 0.1272 0.7326 0.080 Uiso 1 1 calc R . . C212 C -0.0773(5) 0.3033(3) 0.6446(3) 0.0706(17) Uani 1 1 d . . . H109 H -0.1271 0.2802 0.6232 0.085 Uiso 1 1 calc R . . H110 H -0.1264 0.3354 0.6766 0.085 Uiso 1 1 calc R . . Cl1 Cl 0.27284(9) 0.33229(5) 0.29101(5) 0.0409(3) Uani 1 1 d . . . C240 C -0.0045(7) 0.3457(4) 0.5965(3) 0.105(2) Uani 1 1 d . . . H111 H 0.0257 0.3804 0.6190 0.126 Uiso 1 1 calc R . . H112 H 0.0609 0.3140 0.5737 0.126 Uiso 1 1 calc R . . C243 C 0.0230(6) 0.1623(3) 0.2999(3) 0.0981(16) Uani 1 1 d U . . H113 H 0.0616 0.1598 0.3360 0.118 Uiso 1 1 calc R . . H114 H -0.0562 0.1837 0.3153 0.118 Uiso 1 1 calc R . . C247 C 0.0654(5) 0.1962(3) 0.6291(2) 0.0679(16) Uani 1 1 d . . . H115 H 0.1191 0.2219 0.5993 0.082 Uiso 1 1 calc R . . H116 H 0.1104 0.1612 0.6512 0.082 Uiso 1 1 calc R . . C248 C -0.0022(5) 0.1580(3) 0.5916(3) 0.0856(19) Uani 1 1 d . . . H117 H -0.0470 0.1262 0.6201 0.103 Uiso 1 1 calc R . . H118 H -0.0557 0.1925 0.5744 0.103 Uiso 1 1 calc R . . C257 C -0.0239(5) 0.4248(3) 0.2797(3) 0.0731(16) Uani 1 1 d . . . H119 H -0.0911 0.4473 0.2644 0.088 Uiso 1 1 calc R . . H120 H 0.0415 0.4212 0.2437 0.088 Uiso 1 1 calc R . . C258 C -0.0005(5) 0.4706(3) 0.3299(3) 0.0831(19) Uani 1 1 d . . . H121 H -0.0685 0.4792 0.3633 0.125 Uiso 1 1 calc R . . H122 H 0.0198 0.5152 0.3110 0.125 Uiso 1 1 calc R . . H123 H 0.0623 0.4470 0.3477 0.125 Uiso 1 1 calc R . . C259 C 0.0209(6) 0.0913(3) 0.2794(3) 0.1006(16) Uani 1 1 d U . . H124 H 0.0957 0.0738 0.2533 0.121 Uiso 1 1 calc R . . H125 H -0.0366 0.0916 0.2530 0.121 Uiso 1 1 calc R . . C260 C -0.0087(6) 0.0393(3) 0.3394(3) 0.126(3) Uani 1 1 d . . . H126 H 0.0561 0.0309 0.3602 0.189 Uiso 1 1 calc R . . H127 H -0.0247 -0.0052 0.3247 0.189 Uiso 1 1 calc R . . H128 H -0.0753 0.0609 0.3692 0.189 Uiso 1 1 calc R . . C261 C 0.0723(7) 0.1176(5) 0.5398(4) 0.168(4) Uani 1 1 d . . . H129 H 0.1155 0.0777 0.5577 0.202 Uiso 1 1 calc R . . H130 H 0.1276 0.1475 0.5167 0.202 Uiso 1 1 calc R . . C262 C -0.0604(9) 0.3808(6) 0.5525(5) 0.174(4) Uani 1 1 d U . . H131 H -0.1032 0.3464 0.5380 0.209 Uiso 1 1 calc R . . H132 H -0.1177 0.4165 0.5766 0.209 Uiso 1 1 calc R . . C263 C 0.0119(10) 0.0906(6) 0.4947(5) 0.229(6) Uani 1 1 d . . . H133 H -0.0438 0.0614 0.5172 0.343 Uiso 1 1 calc R . . H134 H 0.0666 0.0626 0.4624 0.343 Uiso 1 1 calc R . . H135 H -0.0269 0.1298 0.4746 0.343 Uiso 1 1 calc R . . C264 C -0.0105(12) 0.4145(7) 0.4985(7) 0.264(7) Uani 1 1 d U . . H136 H 0.0676 0.4202 0.5007 0.396 Uiso 1 1 calc R . . H137 H -0.0536 0.4606 0.4953 0.396 Uiso 1 1 calc R . . H138 H -0.0103 0.3867 0.4615 0.396 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 Cl2 0.0649(8) 0.0351(6) 0.0383(6) 0.0039(4) -0.0142(5) -0.0132(5) O1 0.050(2) 0.0325(16) 0.0530(18) 0.0056(14) -0.0234(15) -0.0115(14) O2 0.0520(19) 0.0297(15) 0.0419(17) 0.0025(13) -0.0104(14) -0.0122(14) O3 0.065(2) 0.0421(17) 0.0307(16) 0.0017(13) -0.0105(14) -0.0203(15) O17 0.060(2) 0.0344(16) 0.0410(17) 0.0027(13) -0.0191(14) -0.0129(14) O4 0.066(2) 0.0344(16) 0.0309(15) 0.0029(12) -0.0148(14) -0.0108(14) O18 0.061(2) 0.0308(16) 0.0387(16) 0.0044(13) -0.0176(14) -0.0134(14) O5 0.067(2) 0.0399(17) 0.0382(17) 0.0095(13) -0.0165(15) -0.0187(15) O6 0.057(2) 0.0335(16) 0.0350(16) 0.0006(12) -0.0155(14) -0.0111(14) N2 0.053(2) 0.0346(19) 0.0276(18) 0.0028(15) -0.0135(16) -0.0121(16) N3 0.042(2) 0.0289(18) 0.0324(18) 0.0025(14) -0.0106(15) -0.0073(15) N4 0.049(2) 0.0317(19) 0.0330(19) -0.0026(15) -0.0107(16) -0.0077(16) O7 0.062(2) 0.0516(19) 0.0344(16) 0.0064(14) -0.0140(15) -0.0237(16) O8 0.064(2) 0.0425(17) 0.0357(17) -0.0009(14) -0.0135(15) -0.0122(15) O19 0.071(2) 0.0365(17) 0.0389(17) 0.0020(13) -0.0194(15) -0.0157(15) O9 0.058(2) 0.0388(17) 0.0479(18) -0.0034(14) -0.0193(16) -0.0118(15) O20 0.064(2) 0.0304(16) 0.0445(18) 0.0030(13) -0.0182(15) -0.0112(14) O10 0.053(2) 0.0400(18) 0.0546(19) 0.0048(15) -0.0111(16) -0.0096(15) O11 0.056(2) 0.0386(18) 0.0525(19) 0.0035(15) -0.0100(16) -0.0117(15) C52 0.038(2) 0.031(2) 0.031(2) -0.0020(17) -0.0042(18) -0.0078(18) O12 0.065(2) 0.0418(18) 0.0483(19) 0.0028(15) -0.0160(16) -0.0167(16) O13 0.103(3) 0.0434(19) 0.0434(19) 0.0127(15) -0.0362(18) -0.0269(18) C55 0.051(3) 0.035(2) 0.040(2) 0.0067(19) -0.013(2) -0.016(2) O14 0.138(3) 0.0331(18) 0.0356(18) 0.0047(14) -0.0212(19) -0.0159(19) N5 0.057(2) 0.034(2) 0.035(2) 0.0039(15) -0.0149(17) -0.0136(17) O15 0.102(3) 0.0428(19) 0.0348(18) -0.0025(14) -0.0120(17) -0.0165(18) C59 0.049(3) 0.029(2) 0.042(3) 0.0003(19) -0.013(2) -0.0058(19) C60 0.046(3) 0.035(2) 0.040(2) 0.0094(19) -0.015(2) -0.011(2) C61 0.044(3) 0.032(2) 0.033(2) -0.0054(18) -0.0106(19) -0.0090(19) C62 0.033(2) 0.032(2) 0.035(2) -0.0032(18) -0.0092(18) -0.0047(18) C63 0.041(3) 0.036(2) 0.029(2) -0.0002(18) -0.0083(18) -0.0065(19) C64 0.039(3) 0.036(2) 0.039(2) 0.0047(19) -0.0171(19) -0.0087(19) C65 0.039(3) 0.029(2) 0.038(2) 0.0027(18) -0.0118(19) -0.0089(18) C66 0.042(3) 0.034(2) 0.038(2) -0.0017(19) -0.0117(19) -0.0071(19) C67 0.037(2) 0.033(2) 0.035(2) -0.0040(18) -0.0047(18) -0.0082(18) C68 0.041(3) 0.039(2) 0.034(2) 0.0036(19) -0.0118(19) -0.0114(19) C69 0.042(3) 0.036(2) 0.037(2) -0.0015(19) -0.0090(19) -0.0099(19) C70 0.047(3) 0.042(3) 0.035(2) 0.0043(19) -0.012(2) -0.012(2) C71 0.046(3) 0.037(2) 0.039(2) 0.0005(19) -0.016(2) -0.012(2) O16 0.203(5) 0.0372(19) 0.0341(19) 0.0060(15) -0.034(2) -0.035(2) C73 0.043(3) 0.031(2) 0.041(2) 0.0045(18) -0.014(2) -0.0121(19) C74 0.045(3) 0.037(2) 0.034(2) 0.0035(19) -0.0091(19) -0.010(2) C75 0.051(3) 0.028(2) 0.041(2) 0.0020(18) -0.007(2) -0.0131(19) C76 0.062(3) 0.033(2) 0.040(3) 0.0026(19) -0.018(2) -0.014(2) C77 0.047(3) 0.037(2) 0.032(2) 0.0001(18) -0.0069(19) -0.013(2) C78 0.051(3) 0.049(3) 0.030(2) -0.006(2) -0.009(2) -0.009(2) C79 0.049(3) 0.035(2) 0.045(3) 0.004(2) -0.019(2) -0.010(2) C80 0.046(3) 0.034(2) 0.038(2) 0.0047(19) -0.016(2) -0.010(2) C81 0.046(3) 0.033(2) 0.043(3) 0.0018(19) -0.010(2) -0.009(2) C82 0.047(3) 0.028(2) 0.034(2) 0.0042(18) -0.0091(19) -0.0106(19) C83 0.057(3) 0.040(2) 0.034(2) -0.0012(19) -0.015(2) -0.010(2) C84 0.056(3) 0.036(2) 0.034(2) -0.0013(19) -0.009(2) -0.018(2) C85 0.039(3) 0.046(3) 0.039(2) 0.008(2) -0.011(2) -0.008(2) C86 0.040(3) 0.042(3) 0.042(3) 0.009(2) -0.015(2) -0.011(2) C87 0.084(4) 0.038(3) 0.044(3) 0.000(2) -0.016(3) -0.018(2) C88 0.058(3) 0.036(2) 0.041(3) 0.000(2) -0.009(2) -0.004(2) C89 0.054(3) 0.037(2) 0.034(2) 0.0026(19) -0.016(2) -0.013(2) C90 0.068(3) 0.038(2) 0.035(2) 0.0060(19) -0.020(2) -0.013(2) C91 0.060(3) 0.046(3) 0.032(2) 0.008(2) -0.015(2) -0.020(2) C92 0.041(3) 0.032(2) 0.032(2) 0.0044(17) -0.0046(18) -0.0068(18) C93 0.060(3) 0.046(3) 0.053(3) 0.000(2) -0.024(3) -0.003(2) C94 0.055(3) 0.036(2) 0.036(2) -0.0027(19) -0.013(2) -0.007(2) C95 0.062(3) 0.033(2) 0.040(3) 0.004(2) -0.011(2) -0.012(2) C96 0.052(3) 0.037(2) 0.036(2) -0.0006(19) -0.006(2) -0.009(2) C97 0.079(4) 0.038(3) 0.044(3) 0.003(2) -0.007(3) -0.011(3) C98 0.037(3) 0.040(2) 0.038(2) -0.0001(19) -0.0146(19) -0.0024(19) C99 0.061(3) 0.036(2) 0.038(3) -0.0044(19) -0.016(2) -0.008(2) C100 0.108(5) 0.042(3) 0.036(3) 0.009(2) -0.023(3) -0.027(3) C101 0.058(3) 0.034(2) 0.040(2) -0.0005(19) -0.015(2) -0.011(2) C102 0.043(3) 0.034(2) 0.050(3) 0.003(2) -0.020(2) -0.008(2) C103 0.064(3) 0.035(2) 0.046(3) -0.002(2) -0.006(2) -0.013(2) C104 0.063(3) 0.034(2) 0.045(3) 0.004(2) -0.020(2) -0.015(2) C105 0.056(3) 0.043(3) 0.039(3) 0.002(2) -0.012(2) -0.009(2) C106 0.083(4) 0.036(3) 0.043(3) -0.002(2) -0.021(3) -0.003(3) C107 0.082(4) 0.045(3) 0.053(3) 0.014(2) -0.028(3) -0.025(3) C108 0.084(4) 0.041(3) 0.039(3) 0.004(2) -0.020(2) -0.023(3) C109 0.073(4) 0.039(3) 0.038(3) 0.000(2) -0.007(2) -0.007(2) C110 0.082(4) 0.035(3) 0.043(3) -0.001(2) -0.013(2) -0.016(2) C111 0.068(3) 0.037(3) 0.033(2) 0.0056(19) -0.016(2) -0.012(2) C112 0.067(4) 0.051(3) 0.047(3) 0.001(2) -0.017(3) -0.001(3) C113 0.076(4) 0.041(3) 0.034(2) -0.002(2) -0.017(2) -0.012(2) C114 0.076(4) 0.042(3) 0.054(3) -0.004(2) -0.022(3) 0.003(3) C115 0.077(4) 0.036(3) 0.040(3) 0.008(2) -0.019(2) -0.020(2) C116 0.062(3) 0.031(2) 0.050(3) 0.002(2) -0.016(2) -0.006(2) C117 0.079(4) 0.028(2) 0.037(2) 0.0056(19) -0.021(2) -0.011(2) C118 0.077(4) 0.047(3) 0.037(3) 0.007(2) -0.009(2) -0.024(3) B1 0.053(4) 0.037(3) 0.053(3) 0.004(2) -0.016(3) -0.014(3) C120 0.085(4) 0.047(3) 0.057(3) 0.005(2) -0.021(3) -0.001(3) B2 0.060(4) 0.041(3) 0.041(3) 0.003(2) -0.020(3) -0.016(3) C122 0.095(5) 0.041(3) 0.043(3) 0.004(2) -0.015(3) -0.009(3) C123 0.069(4) 0.050(3) 0.037(3) 0.005(2) -0.008(2) -0.015(2) C124 0.096(4) 0.051(3) 0.042(3) -0.007(2) -0.022(3) -0.017(3) C125 0.062(3) 0.038(3) 0.063(3) 0.005(2) -0.024(3) -0.007(2) C126 0.073(4) 0.052(3) 0.062(3) 0.011(3) -0.025(3) -0.007(3) C127 0.117(5) 0.052(3) 0.043(3) 0.019(2) -0.031(3) -0.028(3) N1 0.042(2) 0.044(2) 0.051(2) 0.0065(18) -0.0150(18) -0.0129(18) C3 0.042(3) 0.044(3) 0.052(3) 0.004(2) -0.010(2) -0.011(2) C156 0.051(3) 0.053(3) 0.060(3) 0.011(2) -0.017(2) -0.013(2) C7 0.040(3) 0.051(3) 0.053(3) 0.003(2) -0.017(2) -0.008(2) C9 0.058(3) 0.054(3) 0.057(3) 0.003(2) -0.014(3) -0.010(2) C132 0.411(14) 0.036(3) 0.048(4) 0.001(3) -0.067(6) -0.047(6) C131 0.250(9) 0.044(3) 0.034(3) 0.007(2) -0.052(4) -0.020(4) C1 0.045(3) 0.051(3) 0.060(3) 0.009(2) -0.018(2) -0.002(2) C133 0.037(3) 0.048(3) 0.056(3) 0.002(2) -0.009(2) -0.002(2) C134 0.060(3) 0.052(3) 0.058(3) -0.001(3) -0.017(3) -0.006(3) C140 0.050(3) 0.056(3) 0.067(3) 0.002(3) -0.017(3) -0.011(2) C142 0.068(4) 0.056(3) 0.069(4) -0.010(3) -0.020(3) -0.004(3) C146 0.056(4) 0.065(3) 0.078(4) -0.016(3) -0.025(3) -0.011(3) C191 0.039(3) 0.046(3) 0.058(3) -0.003(2) -0.012(2) -0.014(2) C207 0.063(4) 0.058(3) 0.044(3) 0.004(2) -0.015(2) -0.021(3) C208 0.059(3) 0.072(3) 0.043(3) 0.000(2) -0.025(2) -0.026(3) C209 0.053(3) 0.068(3) 0.049(3) 0.005(3) -0.015(2) -0.017(3) C210 0.071(4) 0.055(3) 0.065(3) -0.006(3) -0.013(3) -0.017(3) C203 0.080(4) 0.076(4) 0.060(3) 0.009(3) -0.026(3) -0.026(3) C204 0.055(3) 0.069(3) 0.049(3) 0.009(3) -0.014(2) -0.021(3) C205 0.111(6) 0.091(5) 0.091(5) 0.027(4) -0.046(4) -0.032(4) N8 0.060(3) 0.068(3) 0.042(2) 0.005(2) -0.020(2) -0.025(2) C206 0.071(4) 0.080(4) 0.059(3) 0.002(3) -0.026(3) -0.027(3) C212 0.096(5) 0.069(4) 0.063(4) 0.018(3) -0.044(3) -0.031(3) Cl1 0.0540(7) 0.0338(6) 0.0380(6) 0.0007(4) -0.0119(5) -0.0129(5) C240 0.166(7) 0.099(5) 0.066(4) 0.032(4) -0.038(4) -0.066(5) C243 0.100(2) 0.096(2) 0.099(2) 0.0012(14) -0.0175(14) -0.0151(14) C247 0.074(4) 0.072(4) 0.061(3) -0.015(3) -0.010(3) -0.023(3) C248 0.096(5) 0.095(5) 0.076(4) -0.023(4) -0.026(4) -0.031(4) C257 0.091(5) 0.057(3) 0.069(4) -0.009(3) -0.015(3) 0.000(3) C258 0.083(5) 0.065(4) 0.108(5) -0.027(4) -0.038(4) 0.004(3) C259 0.1011(18) 0.0989(18) 0.1007(18) 0.0004(10) -0.0178(10) -0.0139(10) C260 0.137(7) 0.071(5) 0.138(7) 0.034(4) 0.034(5) -0.005(4) C261 0.117(7) 0.226(10) 0.171(9) -0.144(8) -0.014(6) -0.047(7) C262 0.174(4) 0.175(4) 0.174(4) 0.0026(10) -0.0351(13) -0.0218(11) C263 0.232(13) 0.286(14) 0.181(11) -0.100(11) -0.021(9) -0.097(11) C264 0.264(7) 0.264(7) 0.264(7) -0.0001(10) -0.0539(17) -0.0326(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C102 1.381(5) . ? O1 C125 1.415(5) . ? O2 C82 1.376(4) . ? O2 C116 1.442(5) . ? O3 C84 1.379(4) . ? O3 C123 1.454(5) . ? O17 C66 1.322(4) . ? O17 B2 1.501(6) . ? O4 C92 1.365(4) . ? O4 C83 1.430(4) . ? O18 C73 1.330(4) . ? O18 B1 1.485(6) . ? O5 C86 1.373(4) . ? O5 C118 1.422(5) . ? O6 C61 1.366(4) . ? O6 C101 1.434(5) . ? N2 C68 1.353(5) . ? N2 C69 1.389(5) . ? N2 H32 0.8800 . ? N3 C62 1.353(5) . ? N3 C65 1.387(4) . ? N3 H33 0.8800 . ? N4 C94 1.362(5) . ? N4 C59 1.385(5) . ? N4 H34 0.8800 . ? O7 C74 1.364(4) . ? O7 C126 1.447(5) . ? O8 C98 1.355(5) . ? O8 C109 1.434(5) . ? O19 C71 1.330(5) . ? O19 B2 1.473(6) . ? O9 C104 1.362(5) . ? O9 B2 1.460(6) . ? O20 C81 1.321(4) . ? O20 B1 1.481(6) . ? O10 C88 1.363(5) . ? O10 B1 1.478(6) . ? O11 C105 1.382(5) . ? O11 B1 1.460(6) . ? C52 C63 1.394(5) . ? C52 C67 1.408(5) . ? C52 C62 1.470(5) . ? O12 C117 1.378(5) . ? O12 B2 1.460(6) . ? O13 C91 1.357(5) . ? O13 C127 1.431(5) . ? C55 C77 1.389(5) . ? C55 C65 1.394(5) . ? C55 H35 0.9500 . ? O14 C95 1.369(5) . ? O14 C131 1.433(5) . ? N5 C90 1.363(5) . ? N5 C76 1.397(5) . ? N5 H36 0.8800 . ? O15 C78 1.369(5) . ? O15 C124 1.425(5) . ? C59 C103 1.399(6) . ? C59 C81 1.423(6) . ? C60 C64 1.384(5) . ? C60 C98 1.393(5) . ? C60 H1 0.9500 . ? C61 C63 1.388(5) . ? C61 C82 1.393(5) . ? C62 C77 1.384(5) . ? C63 H37 0.9500 . ? C64 C80 1.395(5) . ? C64 C68 1.475(5) . ? C65 C73 1.417(5) . ? C66 C79 1.383(5) . ? C66 C69 1.430(5) . ? C67 C92 1.405(5) . ? C67 H38 0.9500 . ? C68 C85 1.368(5) . ? C69 C70 1.385(5) . ? C70 C85 1.402(5) . ? C70 H2 0.9500 . ? C71 C79 1.390(5) . ? C71 C76 1.414(6) . ? O16 C110 1.368(5) . ? O16 C132 1.412(6) . ? C73 C75 1.380(5) . ? C74 C110 1.377(6) . ? C74 C78 1.382(6) . ? C75 C81 1.373(5) . ? C75 H39 0.9500 . ? C76 C108 1.381(5) . ? C77 H40 0.9500 . ? C78 C99 1.399(6) . ? C79 H3 0.9500 . ? C80 C86 1.393(5) . ? C80 H4 0.9500 . ? C82 C92 1.396(5) . ? C83 H41 0.9800 . ? C83 H42 0.9800 . ? C83 H43 0.9800 . ? C84 C91 1.387(6) . ? C84 C95 1.394(6) . ? C85 H5 0.9500 . ? C86 C102 1.392(6) . ? C87 C103 1.384(6) . ? C87 C94 1.389(6) . ? C87 H44 0.9500 . ? C88 C112 1.387(6) . ? C88 C105 1.391(6) . ? C89 C111 1.386(5) . ? C89 C115 1.388(6) . ? C89 C90 1.481(5) . ? C90 C100 1.383(6) . ? C91 C115 1.380(6) . ? C93 C104 1.382(6) . ? C93 C114 1.384(6) . ? C93 H6 0.9500 . ? C94 C96 1.481(5) . ? C95 C111 1.388(6) . ? C96 C99 1.384(5) . ? C96 C113 1.393(5) . ? C97 C105 1.392(6) . ? C97 C122 1.398(7) . ? C97 H45 0.9500 . ? C98 C102 1.396(5) . ? C99 H46 0.9500 . ? C100 C108 1.377(6) . ? C100 H7 0.9500 . ? C101 H47 0.9800 . ? C101 H48 0.9800 . ? C101 H49 0.9800 . ? C103 H50 0.9500 . ? C104 C117 1.385(6) . ? C106 C114 1.384(7) . ? C106 C107 1.389(7) . ? C106 H8 0.9500 . ? C107 C117 1.385(6) . ? C107 H9 0.9500 . ? C108 H10 0.9500 . ? C109 H11 0.9800 . ? C109 H12 0.9800 . ? C109 H13 0.9800 . ? C110 C113 1.392(6) . ? C111 H14 0.9500 . ? C112 C120 1.393(6) . ? C112 H51 0.9500 . ? C113 H52 0.9500 . ? C114 H15 0.9500 . ? C115 H16 0.9500 . ? C116 H53 0.9800 . ? C116 H54 0.9800 . ? C116 H55 0.9800 . ? C118 H17 0.9800 . ? C118 H18 0.9800 . ? C118 H19 0.9800 . ? C120 C122 1.371(7) . ? C120 H56 0.9500 . ? C122 H57 0.9500 . ? C123 H20 0.9800 . ? C123 H21 0.9800 . ? C123 H22 0.9800 . ? C124 H58 0.9800 . ? C124 H59 0.9800 . ? C124 H60 0.9800 . ? C125 H23 0.9800 . ? C125 H24 0.9800 . ? C125 H25 0.9800 . ? C126 H61 0.9800 . ? C126 H62 0.9800 . ? C126 H63 0.9800 . ? C127 H26 0.9800 . ? C127 H27 0.9800 . ? C127 H28 0.9800 . ? N1 C3 1.511(5) . ? N1 C191 1.517(5) . ? N1 C1 1.519(5) . ? N1 C133 1.522(5) . ? C3 C7 1.506(6) . ? C3 H67 0.9900 . ? C3 H68 0.9900 . ? C156 C9 1.528(6) . ? C156 C7 1.528(6) . ? C156 H69 0.9900 . ? C156 H70 0.9900 . ? C7 H71 0.9900 . ? C7 H72 0.9900 . ? C9 H73 0.9800 . ? C9 H74 0.9800 . ? C9 H75 0.9800 . ? C132 H64 0.9800 . ? C132 H65 0.9800 . ? C132 H66 0.9800 . ? C131 H29 0.9800 . ? C131 H30 0.9800 . ? C131 H31 0.9800 . ? C1 C243 1.526(7) . ? C1 H76 0.9900 . ? C1 H77 0.9900 . ? C133 C134 1.518(6) . ? C133 H78 0.9900 . ? C133 H79 0.9900 . ? C134 C257 1.506(7) . ? C134 H80 0.9900 . ? C134 H81 0.9900 . ? C140 C191 1.516(6) . ? C140 C146 1.535(6) . ? C140 H82 0.9900 . ? C140 H83 0.9900 . ? C142 C146 1.524(7) . ? C142 H84 0.9800 . ? C142 H85 0.9800 . ? C142 H86 0.9800 . ? C146 H87 0.9900 . ? C146 H88 0.9900 . ? C191 H89 0.9900 . ? C191 H90 0.9900 . ? C207 C209 1.506(6) . ? C207 C210 1.519(6) . ? C207 H91 0.9900 . ? C207 H92 0.9900 . ? C208 N8 1.508(5) . ? C208 C209 1.509(6) . ? C208 H93 0.9900 . ? C208 H94 0.9900 . ? C209 H95 0.9900 . ? C209 H96 0.9900 . ? C210 H97 0.9800 . ? C210 H98 0.9800 . ? C210 H99 0.9800 . ? C203 C206 1.513(7) . ? C203 C205 1.522(7) . ? C203 H100 0.9900 . ? C203 H101 0.9900 . ? C204 C206 1.509(7) . ? C204 N8 1.513(5) . ? C204 H102 0.9900 . ? C204 H103 0.9900 . ? C205 H104 0.9800 . ? C205 H105 0.9800 . ? C205 H106 0.9800 . ? N8 C212 1.522(6) . ? N8 C247 1.540(6) . ? C206 H107 0.9900 . ? C206 H108 0.9900 . ? C212 C240 1.515(7) . ? C212 H109 0.9900 . ? C212 H110 0.9900 . ? C240 C262 1.393(10) . ? C240 H111 0.9900 . ? C240 H112 0.9900 . ? C243 C259 1.458(8) . ? C243 H113 0.9900 . ? C243 H114 0.9900 . ? C247 C248 1.532(7) . ? C247 H115 0.9900 . ? C247 H116 0.9900 . ? C248 C261 1.461(9) . ? C248 H117 0.9900 . ? C248 H118 0.9900 . ? C257 C258 1.515(7) . ? C257 H119 0.9900 . ? C257 H120 0.9900 . ? C258 H121 0.9800 . ? C258 H122 0.9800 . ? C258 H123 0.9800 . ? C259 C260 1.628(8) . ? C259 H124 0.9900 . ? C259 H125 0.9900 . ? C260 H126 0.9800 . ? C260 H127 0.9800 . ? C260 H128 0.9800 . ? C261 C263 1.483(11) . ? C261 H129 0.9900 . ? C261 H130 0.9900 . ? C262 C264 1.386(14) . ? C262 H131 0.9900 . ? C262 H132 0.9900 . ? C263 H133 0.9800 . ? C263 H134 0.9800 . ? C263 H135 0.9800 . ? C264 H136 0.9800 . ? C264 H137 0.9800 . ? C264 H138 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 C102 O1 C125 114.9(3) . . ? C82 O2 C116 113.5(3) . . ? C84 O3 C123 117.2(3) . . ? C66 O17 B2 118.1(3) . . ? C92 O4 C83 117.4(3) . . ? C73 O18 B1 118.3(3) . . ? C86 O5 C118 117.3(3) . . ? C61 O6 C101 117.5(3) . . ? C68 N2 C69 109.8(3) . . ? C68 N2 H32 125.1 . . ? C69 N2 H32 125.1 . . ? C62 N3 C65 110.2(3) . . ? C62 N3 H33 124.9 . . ? C65 N3 H33 124.9 . . ? C94 N4 C59 110.3(3) . . ? C94 N4 H34 124.8 . . ? C59 N4 H34 124.8 . . ? C74 O7 C126 116.4(3) . . ? C98 O8 C109 115.5(3) . . ? C71 O19 B2 119.8(3) . . ? C104 O9 B2 105.6(3) . . ? C81 O20 B1 119.8(3) . . ? C88 O10 B1 106.1(3) . . ? C105 O11 B1 105.9(4) . . ? C63 C52 C67 120.2(4) . . ? C63 C52 C62 120.3(4) . . ? C67 C52 C62 119.6(4) . . ? C117 O12 B2 105.3(4) . . ? C91 O13 C127 117.1(3) . . ? C77 C55 C65 108.0(4) . . ? C77 C55 H35 126.0 . . ? C65 C55 H35 126.0 . . ? C95 O14 C131 116.9(4) . . ? C90 N5 C76 109.7(3) . . ? C90 N5 H36 125.2 . . ? C76 N5 H36 125.2 . . ? C78 O15 C124 117.9(3) . . ? N4 C59 C103 106.0(4) . . ? N4 C59 C81 123.4(4) . . ? C103 C59 C81 130.2(4) . . ? C64 C60 C98 120.3(4) . . ? C64 C60 H1 119.8 . . ? C98 C60 H1 119.8 . . ? O6 C61 C63 124.7(4) . . ? O6 C61 C82 115.0(3) . . ? C63 C61 C82 120.3(4) . . ? N3 C62 C77 107.7(3) . . ? N3 C62 C52 121.8(3) . . ? C77 C62 C52 130.5(4) . . ? C61 C63 C52 120.2(4) . . ? C61 C63 H37 119.9 . . ? C52 C63 H37 119.9 . . ? C60 C64 C80 120.3(4) . . ? C60 C64 C68 119.9(4) . . ? C80 C64 C68 119.7(4) . . ? N3 C65 C55 106.1(3) . . ? N3 C65 C73 122.1(4) . . ? C55 C65 C73 131.8(4) . . ? O17 C66 C79 120.3(4) . . ? O17 C66 C69 116.7(4) . . ? C79 C66 C69 123.0(4) . . ? C92 C67 C52 119.0(4) . . ? C92 C67 H38 120.5 . . ? C52 C67 H38 120.5 . . ? N2 C68 C85 107.6(4) . . ? N2 C68 C64 122.1(4) . . ? C85 C68 C64 130.3(4) . . ? C70 C69 N2 107.1(4) . . ? C70 C69 C66 130.7(4) . . ? N2 C69 C66 122.2(4) . . ? C69 C70 C85 106.8(4) . . ? C69 C70 H2 126.6 . . ? C85 C70 H2 126.6 . . ? O19 C71 C79 120.0(4) . . ? O19 C71 C76 116.3(4) . . ? C79 C71 C76 123.7(4) . . ? C110 O16 C132 116.5(4) . . ? O18 C73 C75 120.4(4) . . ? O18 C73 C65 116.2(4) . . ? C75 C73 C65 123.3(4) . . ? O7 C74 C110 118.8(4) . . ? O7 C74 C78 122.2(4) . . ? C110 C74 C78 118.8(4) . . ? C81 C75 C73 121.3(4) . . ? C81 C75 H39 119.4 . . ? C73 C75 H39 119.4 . . ? C108 C76 N5 106.2(4) . . ? C108 C76 C71 131.2(4) . . ? N5 C76 C71 122.4(4) . . ? C62 C77 C55 107.9(4) . . ? C62 C77 H40 126.0 . . ? C55 C77 H40 126.0 . . ? O15 C78 C74 115.0(4) . . ? O15 C78 C99 124.3(4) . . ? C74 C78 C99 120.7(4) . . ? C66 C79 C71 120.7(4) . . ? C66 C79 H3 119.7 . . ? C71 C79 H3 119.7 . . ? C86 C80 C64 119.3(4) . . ? C86 C80 H4 120.4 . . ? C64 C80 H4 120.4 . . ? O20 C81 C75 120.5(4) . . ? O20 C81 C59 116.2(4) . . ? C75 C81 C59 123.1(4) . . ? O2 C82 C61 120.5(4) . . ? O2 C82 C92 119.5(3) . . ? C61 C82 C92 119.9(3) . . ? O4 C83 H41 109.5 . . ? O4 C83 H42 109.5 . . ? H41 C83 H42 109.5 . . ? O4 C83 H43 109.5 . . ? H41 C83 H43 109.5 . . ? H42 C83 H43 109.5 . . ? O3 C84 C91 122.5(4) . . ? O3 C84 C95 118.4(4) . . ? C91 C84 C95 119.1(4) . . ? C68 C85 C70 108.8(4) . . ? C68 C85 H5 125.6 . . ? C70 C85 H5 125.6 . . ? O5 C86 C102 114.8(4) . . ? O5 C86 C80 124.6(4) . . ? C102 C86 C80 120.6(4) . . ? C103 C87 C94 108.2(4) . . ? C103 C87 H44 125.9 . . ? C94 C87 H44 125.9 . . ? O10 C88 C112 128.0(4) . . ? O10 C88 C105 110.7(4) . . ? C112 C88 C105 121.3(4) . . ? C111 C89 C115 119.6(4) . . ? C111 C89 C90 121.9(4) . . ? C115 C89 C90 118.4(4) . . ? N5 C90 C100 107.0(4) . . ? N5 C90 C89 122.9(4) . . ? C100 C90 C89 130.1(4) . . ? O13 C91 C115 124.6(4) . . ? O13 C91 C84 115.4(4) . . ? C115 C91 C84 120.0(4) . . ? O4 C92 C82 115.6(3) . . ? O4 C92 C67 124.0(4) . . ? C82 C92 C67 120.4(4) . . ? C104 C93 C114 117.1(5) . . ? C104 C93 H6 121.5 . . ? C114 C93 H6 121.5 . . ? N4 C94 C87 107.3(4) . . ? N4 C94 C96 123.6(4) . . ? C87 C94 C96 129.1(4) . . ? O14 C95 C111 123.2(4) . . ? O14 C95 C84 115.9(4) . . ? C111 C95 C84 120.9(4) . . ? C99 C96 C113 120.0(4) . . ? C99 C96 C94 119.1(4) . . ? C113 C96 C94 120.9(4) . . ? C105 C97 C122 116.1(5) . . ? C105 C97 H45 121.9 . . ? C122 C97 H45 121.9 . . ? O8 C98 C60 124.6(4) . . ? O8 C98 C102 115.7(4) . . ? C60 C98 C102 119.7(4) . . ? C96 C99 C78 119.7(4) . . ? C96 C99 H46 120.1 . . ? C78 C99 H46 120.1 . . ? C108 C100 C90 108.7(4) . . ? C108 C100 H7 125.7 . . ? C90 C100 H7 125.7 . . ? O6 C101 H47 109.5 . . ? O6 C101 H48 109.5 . . ? H47 C101 H48 109.5 . . ? O6 C101 H49 109.5 . . ? H47 C101 H49 109.5 . . ? H48 C101 H49 109.5 . . ? O1 C102 C86 120.4(4) . . ? O1 C102 C98 119.8(4) . . ? C86 C102 C98 119.6(4) . . ? C87 C103 C59 108.2(4) . . ? C87 C103 H50 125.9 . . ? C59 C103 H50 125.9 . . ? O9 C104 C93 127.9(4) . . ? O9 C104 C117 110.7(4) . . ? C93 C104 C117 121.4(4) . . ? O11 C105 C88 110.5(4) . . ? O11 C105 C97 127.8(4) . . ? C88 C105 C97 121.8(5) . . ? C114 C106 C107 121.0(5) . . ? C114 C106 H8 119.5 . . ? C107 C106 H8 119.5 . . ? C117 C107 C106 117.1(5) . . ? C117 C107 H9 121.4 . . ? C106 C107 H9 121.4 . . ? C100 C108 C76 108.4(4) . . ? C100 C108 H10 125.8 . . ? C76 C108 H10 125.8 . . ? O8 C109 H11 109.5 . . ? O8 C109 H12 109.5 . . ? H11 C109 H12 109.5 . . ? O8 C109 H13 109.5 . . ? H11 C109 H13 109.5 . . ? H12 C109 H13 109.5 . . ? O16 C110 C74 114.8(4) . . ? O16 C110 C113 123.5(4) . . ? C74 C110 C113 121.7(4) . . ? C89 C111 C95 119.5(4) . . ? C89 C111 H14 120.3 . . ? C95 C111 H14 120.3 . . ? C88 C112 C120 117.0(5) . . ? C88 C112 H51 121.5 . . ? C120 C112 H51 121.5 . . ? C110 C113 C96 119.0(4) . . ? C110 C113 H52 120.5 . . ? C96 C113 H52 120.5 . . ? C93 C114 C106 121.8(5) . . ? C93 C114 H15 119.1 . . ? C106 C114 H15 119.1 . . ? C91 C115 C89 120.9(4) . . ? C91 C115 H16 119.6 . . ? C89 C115 H16 119.6 . . ? O2 C116 H53 109.5 . . ? O2 C116 H54 109.5 . . ? H53 C116 H54 109.5 . . ? O2 C116 H55 109.5 . . ? H53 C116 H55 109.5 . . ? H54 C116 H55 109.5 . . ? O12 C117 C107 128.2(5) . . ? O12 C117 C104 110.4(4) . . ? C107 C117 C104 121.5(5) . . ? O5 C118 H17 109.5 . . ? O5 C118 H18 109.5 . . ? H17 C118 H18 109.5 . . ? O5 C118 H19 109.5 . . ? H17 C118 H19 109.5 . . ? H18 C118 H19 109.5 . . ? O11 B1 O10 106.7(4) . . ? O11 B1 O20 109.2(4) . . ? O10 B1 O20 110.6(4) . . ? O11 B1 O18 110.8(4) . . ? O10 B1 O18 107.3(4) . . ? O20 B1 O18 112.1(4) . . ? C122 C120 C112 121.6(5) . . ? C122 C120 H56 119.2 . . ? C112 C120 H56 119.2 . . ? O12 B2 O9 107.0(4) . . ? O12 B2 O19 109.3(4) . . ? O9 B2 O19 112.0(4) . . ? O12 B2 O17 110.2(4) . . ? O9 B2 O17 107.5(4) . . ? O19 B2 O17 110.7(4) . . ? C120 C122 C97 122.1(5) . . ? C120 C122 H57 118.9 . . ? C97 C122 H57 118.9 . . ? O3 C123 H20 109.5 . . ? O3 C123 H21 109.5 . . ? H20 C123 H21 109.5 . . ? O3 C123 H22 109.5 . . ? H20 C123 H22 109.5 . . ? H21 C123 H22 109.5 . . ? O15 C124 H58 109.5 . . ? O15 C124 H59 109.5 . . ? H58 C124 H59 109.5 . . ? O15 C124 H60 109.5 . . ? H58 C124 H60 109.5 . . ? H59 C124 H60 109.5 . . ? O1 C125 H23 109.5 . . ? O1 C125 H24 109.5 . . ? H23 C125 H24 109.5 . . ? O1 C125 H25 109.5 . . ? H23 C125 H25 109.5 . . ? H24 C125 H25 109.5 . . ? O7 C126 H61 109.5 . . ? O7 C126 H62 109.5 . . ? H61 C126 H62 109.5 . . ? O7 C126 H63 109.5 . . ? H61 C126 H63 109.5 . . ? H62 C126 H63 109.5 . . ? O13 C127 H26 109.5 . . ? O13 C127 H27 109.5 . . ? H26 C127 H27 109.5 . . ? O13 C127 H28 109.5 . . ? H26 C127 H28 109.5 . . ? H27 C127 H28 109.5 . . ? C3 N1 C191 110.3(3) . . ? C3 N1 C1 106.2(3) . . ? C191 N1 C1 111.0(3) . . ? C3 N1 C133 111.4(3) . . ? C191 N1 C133 106.6(3) . . ? C1 N1 C133 111.5(3) . . ? C7 C3 N1 116.5(4) . . ? C7 C3 H67 108.2 . . ? N1 C3 H67 108.2 . . ? C7 C3 H68 108.2 . . ? N1 C3 H68 108.2 . . ? H67 C3 H68 107.3 . . ? C9 C156 C7 111.5(4) . . ? C9 C156 H69 109.3 . . ? C7 C156 H69 109.3 . . ? C9 C156 H70 109.3 . . ? C7 C156 H70 109.3 . . ? H69 C156 H70 108.0 . . ? C3 C7 C156 110.2(4) . . ? C3 C7 H71 109.6 . . ? C156 C7 H71 109.6 . . ? C3 C7 H72 109.6 . . ? C156 C7 H72 109.6 . . ? H71 C7 H72 108.1 . . ? C156 C9 H73 109.5 . . ? C156 C9 H74 109.5 . . ? H73 C9 H74 109.5 . . ? C156 C9 H75 109.5 . . ? H73 C9 H75 109.5 . . ? H74 C9 H75 109.5 . . ? O16 C132 H64 109.5 . . ? O16 C132 H65 109.5 . . ? H64 C132 H65 109.5 . . ? O16 C132 H66 109.5 . . ? H64 C132 H66 109.5 . . ? H65 C132 H66 109.5 . . ? O14 C131 H29 109.5 . . ? O14 C131 H30 109.5 . . ? H29 C131 H30 109.5 . . ? O14 C131 H31 109.5 . . ? H29 C131 H31 109.5 . . ? H30 C131 H31 109.5 . . ? N1 C1 C243 117.2(4) . . ? N1 C1 H76 108.0 . . ? C243 C1 H76 108.0 . . ? N1 C1 H77 108.0 . . ? C243 C1 H77 108.0 . . ? H76 C1 H77 107.3 . . ? C134 C133 N1 117.9(4) . . ? C134 C133 H78 107.8 . . ? N1 C133 H78 107.8 . . ? C134 C133 H79 107.8 . . ? N1 C133 H79 107.8 . . ? H78 C133 H79 107.2 . . ? C257 C134 C133 117.5(4) . . ? C257 C134 H80 107.9 . . ? C133 C134 H80 107.9 . . ? C257 C134 H81 107.9 . . ? C133 C134 H81 107.9 . . ? H80 C134 H81 107.2 . . ? C191 C140 C146 110.4(4) . . ? C191 C140 H82 109.6 . . ? C146 C140 H82 109.6 . . ? C191 C140 H83 109.6 . . ? C146 C140 H83 109.6 . . ? H82 C140 H83 108.1 . . ? C146 C142 H84 109.5 . . ? C146 C142 H85 109.5 . . ? H84 C142 H85 109.5 . . ? C146 C142 H86 109.5 . . ? H84 C142 H86 109.5 . . ? H85 C142 H86 109.5 . . ? C142 C146 C140 112.0(4) . . ? C142 C146 H87 109.2 . . ? C140 C146 H87 109.2 . . ? C142 C146 H88 109.2 . . ? C140 C146 H88 109.2 . . ? H87 C146 H88 107.9 . . ? C140 C191 N1 115.8(4) . . ? C140 C191 H89 108.3 . . ? N1 C191 H89 108.3 . . ? C140 C191 H90 108.3 . . ? N1 C191 H90 108.3 . . ? H89 C191 H90 107.4 . . ? C209 C207 C210 112.7(4) . . ? C209 C207 H91 109.1 . . ? C210 C207 H91 109.1 . . ? C209 C207 H92 109.1 . . ? C210 C207 H92 109.1 . . ? H91 C207 H92 107.8 . . ? N8 C208 C209 116.2(4) . . ? N8 C208 H93 108.2 . . ? C209 C208 H93 108.2 . . ? N8 C208 H94 108.2 . . ? C209 C208 H94 108.2 . . ? H93 C208 H94 107.4 . . ? C207 C209 C208 112.6(4) . . ? C207 C209 H95 109.1 . . ? C208 C209 H95 109.1 . . ? C207 C209 H96 109.1 . . ? C208 C209 H96 109.1 . . ? H95 C209 H96 107.8 . . ? C207 C210 H97 109.5 . . ? C207 C210 H98 109.5 . . ? H97 C210 H98 109.5 . . ? C207 C210 H99 109.5 . . ? H97 C210 H99 109.5 . . ? H98 C210 H99 109.5 . . ? C206 C203 C205 112.0(5) . . ? C206 C203 H100 109.2 . . ? C205 C203 H100 109.2 . . ? C206 C203 H101 109.2 . . ? C205 C203 H101 109.2 . . ? H100 C203 H101 107.9 . . ? C206 C204 N8 114.3(4) . . ? C206 C204 H102 108.7 . . ? N8 C204 H102 108.7 . . ? C206 C204 H103 108.7 . . ? N8 C204 H103 108.7 . . ? H102 C204 H103 107.6 . . ? C203 C205 H104 109.5 . . ? C203 C205 H105 109.5 . . ? H104 C205 H105 109.5 . . ? C203 C205 H106 109.5 . . ? H104 C205 H106 109.5 . . ? H105 C205 H106 109.5 . . ? C208 N8 C204 111.4(3) . . ? C208 N8 C212 110.6(4) . . ? C204 N8 C212 107.8(4) . . ? C208 N8 C247 107.3(4) . . ? C204 N8 C247 110.0(4) . . ? C212 N8 C247 109.7(4) . . ? C204 C206 C203 112.7(5) . . ? C204 C206 H107 109.0 . . ? C203 C206 H107 109.0 . . ? C204 C206 H108 109.0 . . ? C203 C206 H108 109.0 . . ? H107 C206 H108 107.8 . . ? C240 C212 N8 113.7(5) . . ? C240 C212 H109 108.8 . . ? N8 C212 H109 108.8 . . ? C240 C212 H110 108.8 . . ? N8 C212 H110 108.8 . . ? H109 C212 H110 107.7 . . ? C262 C240 C212 114.8(8) . . ? C262 C240 H111 108.6 . . ? C212 C240 H111 108.6 . . ? C262 C240 H112 108.6 . . ? C212 C240 H112 108.6 . . ? H111 C240 H112 107.6 . . ? C259 C243 C1 115.8(6) . . ? C259 C243 H113 108.3 . . ? C1 C243 H113 108.3 . . ? C259 C243 H114 108.3 . . ? C1 C243 H114 108.3 . . ? H113 C243 H114 107.4 . . ? C248 C247 N8 113.7(5) . . ? C248 C247 H115 108.8 . . ? N8 C247 H115 108.8 . . ? C248 C247 H116 108.8 . . ? N8 C247 H116 108.8 . . ? H115 C247 H116 107.7 . . ? C261 C248 C247 111.5(6) . . ? C261 C248 H117 109.3 . . ? C247 C248 H117 109.3 . . ? C261 C248 H118 109.3 . . ? C247 C248 H118 109.3 . . ? H117 C248 H118 108.0 . . ? C134 C257 C258 113.2(5) . . ? C134 C257 H119 108.9 . . ? C258 C257 H119 108.9 . . ? C134 C257 H120 108.9 . . ? C258 C257 H120 108.9 . . ? H119 C257 H120 107.7 . . ? C257 C258 H121 109.5 . . ? C257 C258 H122 109.5 . . ? H121 C258 H122 109.5 . . ? C257 C258 H123 109.5 . . ? H121 C258 H123 109.5 . . ? H122 C258 H123 109.5 . . ? C243 C259 C260 111.3(6) . . ? C243 C259 H124 109.4 . . ? C260 C259 H124 109.4 . . ? C243 C259 H125 109.4 . . ? C260 C259 H125 109.4 . . ? H124 C259 H125 108.0 . . ? C259 C260 H126 109.5 . . ? C259 C260 H127 109.5 . . ? H126 C260 H127 109.5 . . ? C259 C260 H128 109.5 . . ? H126 C260 H128 109.5 . . ? H127 C260 H128 109.5 . . ? C248 C261 C263 114.0(8) . . ? C248 C261 H129 108.8 . . ? C263 C261 H129 108.8 . . ? C248 C261 H130 108.8 . . ? C263 C261 H130 108.8 . . ? H129 C261 H130 107.7 . . ? C264 C262 C240 126.3(11) . . ? C264 C262 H131 105.7 . . ? C240 C262 H131 105.7 . . ? C264 C262 H132 105.7 . . ? C240 C262 H132 105.7 . . ? H131 C262 H132 106.2 . . ? C261 C263 H133 109.5 . . ? C261 C263 H134 109.5 . . ? H133 C263 H134 109.5 . . ? C261 C263 H135 109.5 . . ? H133 C263 H135 109.5 . . ? H134 C263 H135 109.5 . . ? C262 C264 H136 109.5 . . ? C262 C264 H137 109.5 . . ? H136 C264 H137 109.5 . . ? C262 C264 H138 109.5 . . ? H136 C264 H138 109.5 . . ? H137 C264 H138 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C94 N4 C59 C103 -0.7(5) . . . . ? C94 N4 C59 C81 172.6(4) . . . . ? C101 O6 C61 C63 0.4(6) . . . . ? C101 O6 C61 C82 179.6(4) . . . . ? C65 N3 C62 C77 1.5(4) . . . . ? C65 N3 C62 C52 -176.6(3) . . . . ? C63 C52 C62 N3 159.4(4) . . . . ? C67 C52 C62 N3 -20.5(6) . . . . ? C63 C52 C62 C77 -18.3(7) . . . . ? C67 C52 C62 C77 161.8(4) . . . . ? O6 C61 C63 C52 178.8(4) . . . . ? C82 C61 C63 C52 -0.3(6) . . . . ? C67 C52 C63 C61 1.2(6) . . . . ? C62 C52 C63 C61 -178.7(4) . . . . ? C98 C60 C64 C80 -3.0(6) . . . . ? C98 C60 C64 C68 173.5(4) . . . . ? C62 N3 C65 C55 -1.2(5) . . . . ? C62 N3 C65 C73 177.6(4) . . . . ? C77 C55 C65 N3 0.4(5) . . . . ? C77 C55 C65 C73 -178.2(4) . . . . ? B2 O17 C66 C79 -19.5(6) . . . . ? B2 O17 C66 C69 162.6(4) . . . . ? C63 C52 C67 C92 -0.4(6) . . . . ? C62 C52 C67 C92 179.5(3) . . . . ? C69 N2 C68 C85 0.0(5) . . . . ? C69 N2 C68 C64 179.7(4) . . . . ? C60 C64 C68 N2 -21.7(6) . . . . ? C80 C64 C68 N2 154.9(4) . . . . ? C60 C64 C68 C85 157.9(4) . . . . ? C80 C64 C68 C85 -25.5(7) . . . . ? C68 N2 C69 C70 0.0(5) . . . . ? C68 N2 C69 C66 -179.4(4) . . . . ? O17 C66 C69 C70 -5.9(7) . . . . ? C79 C66 C69 C70 176.3(4) . . . . ? O17 C66 C69 N2 173.3(4) . . . . ? C79 C66 C69 N2 -4.4(7) . . . . ? N2 C69 C70 C85 0.0(5) . . . . ? C66 C69 C70 C85 179.3(4) . . . . ? B2 O19 C71 C79 9.5(6) . . . . ? B2 O19 C71 C76 -171.9(4) . . . . ? B1 O18 C73 C75 -17.0(6) . . . . ? B1 O18 C73 C65 166.3(4) . . . . ? N3 C65 C73 O18 177.3(3) . . . . ? C55 C65 C73 O18 -4.3(7) . . . . ? N3 C65 C73 C75 0.7(7) . . . . ? C55 C65 C73 C75 179.1(5) . . . . ? C126 O7 C74 C110 120.8(5) . . . . ? C126 O7 C74 C78 -64.1(6) . . . . ? O18 C73 C75 C81 -4.5(7) . . . . ? C65 C73 C75 C81 172.0(4) . . . . ? C90 N5 C76 C108 1.4(5) . . . . ? C90 N5 C76 C71 177.8(4) . . . . ? O19 C71 C76 C108 -3.9(8) . . . . ? C79 C71 C76 C108 174.6(5) . . . . ? O19 C71 C76 N5 -179.4(4) . . . . ? C79 C71 C76 N5 -0.9(7) . . . . ? N3 C62 C77 C55 -1.3(5) . . . . ? C52 C62 C77 C55 176.7(4) . . . . ? C65 C55 C77 C62 0.5(5) . . . . ? C124 O15 C78 C74 165.0(4) . . . . ? C124 O15 C78 C99 -16.9(7) . . . . ? O7 C74 C78 O15 0.6(6) . . . . ? C110 C74 C78 O15 175.7(4) . . . . ? O7 C74 C78 C99 -177.6(4) . . . . ? C110 C74 C78 C99 -2.4(7) . . . . ? O17 C66 C79 C71 -5.3(6) . . . . ? C69 C66 C79 C71 172.4(4) . . . . ? O19 C71 C79 C66 10.9(6) . . . . ? C76 C71 C79 C66 -167.6(4) . . . . ? C60 C64 C80 C86 2.6(6) . . . . ? C68 C64 C80 C86 -174.0(4) . . . . ? B1 O20 C81 C75 7.4(6) . . . . ? B1 O20 C81 C59 -177.2(4) . . . . ? C73 C75 C81 O20 9.6(7) . . . . ? C73 C75 C81 C59 -165.4(4) . . . . ? N4 C59 C81 O20 179.6(4) . . . . ? C103 C59 C81 O20 -8.9(7) . . . . ? N4 C59 C81 C75 -5.2(7) . . . . ? C103 C59 C81 C75 166.3(5) . . . . ? C116 O2 C82 C61 80.6(5) . . . . ? C116 O2 C82 C92 -103.1(4) . . . . ? O6 C61 C82 O2 -4.4(6) . . . . ? C63 C61 C82 O2 174.8(4) . . . . ? O6 C61 C82 C92 179.4(4) . . . . ? C63 C61 C82 C92 -1.4(6) . . . . ? C123 O3 C84 C91 -53.3(6) . . . . ? C123 O3 C84 C95 129.2(4) . . . . ? N2 C68 C85 C70 0.0(5) . . . . ? C64 C68 C85 C70 -179.7(4) . . . . ? C69 C70 C85 C68 0.0(5) . . . . ? C118 O5 C86 C102 -173.3(4) . . . . ? C118 O5 C86 C80 7.8(6) . . . . ? C64 C80 C86 O5 179.9(4) . . . . ? C64 C80 C86 C102 1.1(6) . . . . ? B1 O10 C88 C112 176.1(5) . . . . ? B1 O10 C88 C105 -1.9(5) . . . . ? C76 N5 C90 C100 -1.5(5) . . . . ? C76 N5 C90 C89 179.4(4) . . . . ? C111 C89 C90 N5 13.4(7) . . . . ? C115 C89 C90 N5 -166.8(4) . . . . ? C111 C89 C90 C100 -165.5(5) . . . . ? C115 C89 C90 C100 14.3(8) . . . . ? C127 O13 C91 C115 -22.3(7) . . . . ? C127 O13 C91 C84 160.1(4) . . . . ? O3 C84 C91 O13 -2.2(6) . . . . ? C95 C84 C91 O13 175.3(4) . . . . ? O3 C84 C91 C115 -179.9(4) . . . . ? C95 C84 C91 C115 -2.4(7) . . . . ? C83 O4 C92 C82 179.2(4) . . . . ? C83 O4 C92 C67 -3.0(6) . . . . ? O2 C82 C92 O4 3.9(6) . . . . ? C61 C82 C92 O4 -179.8(4) . . . . ? O2 C82 C92 C67 -174.1(4) . . . . ? C61 C82 C92 C67 2.2(6) . . . . ? C52 C67 C92 O4 -179.1(4) . . . . ? C52 C67 C92 C82 -1.3(6) . . . . ? C59 N4 C94 C87 0.6(5) . . . . ? C59 N4 C94 C96 -179.1(4) . . . . ? C103 C87 C94 N4 -0.3(5) . . . . ? C103 C87 C94 C96 179.4(4) . . . . ? C131 O14 C95 C111 1.8(7) . . . . ? C131 O14 C95 C84 -177.0(5) . . . . ? O3 C84 C95 O14 -2.6(6) . . . . ? C91 C84 C95 O14 179.8(4) . . . . ? O3 C84 C95 C111 178.6(4) . . . . ? C91 C84 C95 C111 0.9(7) . . . . ? N4 C94 C96 C99 -169.7(4) . . . . ? C87 C94 C96 C99 10.7(7) . . . . ? N4 C94 C96 C113 10.2(7) . . . . ? C87 C94 C96 C113 -169.4(5) . . . . ? C109 O8 C98 C60 -6.9(6) . . . . ? C109 O8 C98 C102 174.4(4) . . . . ? C64 C60 C98 O8 -178.9(4) . . . . ? C64 C60 C98 C102 -0.3(6) . . . . ? C113 C96 C99 C78 -0.2(7) . . . . ? C94 C96 C99 C78 179.7(4) . . . . ? O15 C78 C99 C96 -175.5(4) . . . . ? C74 C78 C99 C96 2.6(7) . . . . ? N5 C90 C100 C108 1.1(6) . . . . ? C89 C90 C100 C108 -179.9(5) . . . . ? C125 O1 C102 C86 85.3(5) . . . . ? C125 O1 C102 C98 -100.2(5) . . . . ? O5 C86 C102 O1 -8.8(6) . . . . ? C80 C86 C102 O1 170.2(4) . . . . ? O5 C86 C102 C98 176.8(4) . . . . ? C80 C86 C102 C98 -4.3(6) . . . . ? O8 C98 C102 O1 8.1(6) . . . . ? C60 C98 C102 O1 -170.6(4) . . . . ? O8 C98 C102 C86 -177.4(4) . . . . ? C60 C98 C102 C86 3.9(6) . . . . ? C94 C87 C103 C59 -0.2(6) . . . . ? N4 C59 C103 C87 0.5(5) . . . . ? C81 C59 C103 C87 -172.1(5) . . . . ? B2 O9 C104 C93 168.4(5) . . . . ? B2 O9 C104 C117 -8.6(5) . . . . ? C114 C93 C104 O9 -178.8(4) . . . . ? C114 C93 C104 C117 -2.1(7) . . . . ? B1 O11 C105 C88 -2.3(5) . . . . ? B1 O11 C105 C97 178.0(5) . . . . ? O10 C88 C105 O11 2.8(5) . . . . ? C112 C88 C105 O11 -175.4(4) . . . . ? O10 C88 C105 C97 -177.5(4) . . . . ? C112 C88 C105 C97 4.3(7) . . . . ? C122 C97 C105 O11 177.6(4) . . . . ? C122 C97 C105 C88 -2.1(7) . . . . ? C114 C106 C107 C117 -1.6(7) . . . . ? C90 C100 C108 C76 -0.3(6) . . . . ? N5 C76 C108 C100 -0.7(6) . . . . ? C71 C76 C108 C100 -176.7(5) . . . . ? C132 O16 C110 C74 -175.3(6) . . . . ? C132 O16 C110 C113 6.3(9) . . . . ? O7 C74 C110 O16 -3.1(7) . . . . ? C78 C74 C110 O16 -178.4(4) . . . . ? O7 C74 C110 C113 175.4(4) . . . . ? C78 C74 C110 C113 0.0(7) . . . . ? C115 C89 C111 C95 -0.5(7) . . . . ? C90 C89 C111 C95 179.3(4) . . . . ? O14 C95 C111 C89 -178.3(4) . . . . ? C84 C95 C111 C89 0.5(7) . . . . ? O10 C88 C112 C120 179.3(4) . . . . ? C105 C88 C112 C120 -2.9(7) . . . . ? O16 C110 C113 C96 -179.4(5) . . . . ? C74 C110 C113 C96 2.2(8) . . . . ? C99 C96 C113 C110 -2.1(7) . . . . ? C94 C96 C113 C110 178.0(4) . . . . ? C104 C93 C114 C106 -2.3(7) . . . . ? C107 C106 C114 C93 4.2(7) . . . . ? O13 C91 C115 C89 -175.0(4) . . . . ? C84 C91 C115 C89 2.5(7) . . . . ? C111 C89 C115 C91 -1.0(7) . . . . ? C90 C89 C115 C91 179.2(4) . . . . ? B2 O12 C117 C107 -175.0(4) . . . . ? B2 O12 C117 C104 3.5(5) . . . . ? C106 C107 C117 O12 175.6(4) . . . . ? C106 C107 C117 C104 -2.7(7) . . . . ? O9 C104 C117 O12 3.3(5) . . . . ? C93 C104 C117 O12 -174.0(4) . . . . ? O9 C104 C117 C107 -178.1(4) . . . . ? C93 C104 C117 C107 4.7(7) . . . . ? C105 O11 B1 O10 1.1(5) . . . . ? C105 O11 B1 O20 -118.4(4) . . . . ? C105 O11 B1 O18 117.6(4) . . . . ? C88 O10 B1 O11 0.5(5) . . . . ? C88 O10 B1 O20 119.1(4) . . . . ? C88 O10 B1 O18 -118.4(4) . . . . ? C81 O20 B1 O11 -149.8(4) . . . . ? C81 O20 B1 O10 93.1(4) . . . . ? C81 O20 B1 O18 -26.6(6) . . . . ? C73 O18 B1 O11 153.6(4) . . . . ? C73 O18 B1 O10 -90.3(4) . . . . ? C73 O18 B1 O20 31.3(6) . . . . ? C88 C112 C120 C122 -0.6(7) . . . . ? C117 O12 B2 O9 -8.6(4) . . . . ? C117 O12 B2 O19 -130.0(4) . . . . ? C117 O12 B2 O17 108.0(4) . . . . ? C104 O9 B2 O12 10.5(4) . . . . ? C104 O9 B2 O19 130.3(4) . . . . ? C104 O9 B2 O17 -107.9(4) . . . . ? C71 O19 B2 O12 -153.0(4) . . . . ? C71 O19 B2 O9 88.6(5) . . . . ? C71 O19 B2 O17 -31.4(6) . . . . ? C66 O17 B2 O12 157.5(4) . . . . ? C66 O17 B2 O9 -86.2(4) . . . . ? C66 O17 B2 O19 36.4(6) . . . . ? C112 C120 C122 C97 2.9(8) . . . . ? C105 C97 C122 C120 -1.5(7) . . . . ? C191 N1 C3 C7 56.2(5) . . . . ? C1 N1 C3 C7 176.5(4) . . . . ? C133 N1 C3 C7 -62.0(5) . . . . ? N1 C3 C7 C156 -175.1(4) . . . . ? C9 C156 C7 C3 177.7(4) . . . . ? C3 N1 C1 C243 179.1(4) . . . . ? C191 N1 C1 C243 -61.0(5) . . . . ? C133 N1 C1 C243 57.6(5) . . . . ? C3 N1 C133 C134 -61.1(5) . . . . ? C191 N1 C133 C134 178.5(4) . . . . ? C1 N1 C133 C134 57.3(5) . . . . ? N1 C133 C134 C257 91.0(5) . . . . ? C191 C140 C146 C142 176.7(4) . . . . ? C146 C140 C191 N1 179.4(4) . . . . ? C3 N1 C191 C140 53.1(5) . . . . ? C1 N1 C191 C140 -64.3(5) . . . . ? C133 N1 C191 C140 174.2(4) . . . . ? C210 C207 C209 C208 -177.1(4) . . . . ? N8 C208 C209 C207 -168.8(4) . . . . ? C209 C208 N8 C204 -59.2(5) . . . . ? C209 C208 N8 C212 60.7(5) . . . . ? C209 C208 N8 C247 -179.7(4) . . . . ? C206 C204 N8 C208 -58.5(5) . . . . ? C206 C204 N8 C212 180.0(4) . . . . ? C206 C204 N8 C247 60.4(5) . . . . ? N8 C204 C206 C203 -161.9(4) . . . . ? C205 C203 C206 C204 -175.5(5) . . . . ? C208 N8 C212 C240 58.0(6) . . . . ? C204 N8 C212 C240 -179.9(5) . . . . ? C247 N8 C212 C240 -60.1(5) . . . . ? N8 C212 C240 C262 161.2(7) . . . . ? N1 C1 C243 C259 96.1(6) . . . . ? C208 N8 C247 C248 179.9(4) . . . . ? C204 N8 C247 C248 58.6(6) . . . . ? C212 N8 C247 C248 -59.9(6) . . . . ? N8 C247 C248 C261 171.4(6) . . . . ? C133 C134 C257 C258 172.2(4) . . . . ? C1 C243 C259 C260 163.5(5) . . . . ? C247 C248 C261 C263 -169.0(8) . . . . ? C212 C240 C262 C264 -169.9(11) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H32 Cl2 0.88 2.41 3.284(3) 175.1 . N3 H33 Cl1 0.88 2.49 3.357(3) 169.6 . N4 H34 Cl1 0.88 2.42 3.295(3) 175.6 . N5 H36 Cl2 0.88 2.42 3.299(3) 176.4 . _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 68.25 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 1.285 _refine_diff_density_min -0.624 _refine_diff_density_rms 0.077 data_21129ma _database_code_depnum_ccdc_archive 'CCDC 921412' #TrackingRef '3a.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H39 B N2 O8, C4 H8 O2, O' _chemical_formula_sum 'C45 H47 B N2 O11' _chemical_formula_weight 801.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2288(2) _cell_length_b 12.3482(3) _cell_length_c 16.4083(3) _cell_angle_alpha 71.0113(13) _cell_angle_beta 70.5677(11) _cell_angle_gamma 80.8212(12) _cell_volume 2025.39(7) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 11986 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 68.23 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 846 _exptl_absorpt_coefficient_mu 0.771 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8611 _exptl_absorpt_correction_T_max 0.9625 _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20067 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0665 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 64.00 _reflns_number_total 6583 _reflns_number_gt 4308 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0665P)^2^+1.0860P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6583 _refine_ls_number_parameters 540 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0843 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1588 _refine_ls_wR_factor_gt 0.1264 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 1.0449(2) 0.58570(19) -0.30862(16) 0.0278(6) Uani 1 1 d . . . H1 H 1.0728 0.5294 -0.2691 0.033 Uiso 1 1 calc R . . N2 N 1.3774(2) 0.3553(2) -0.68789(16) 0.0286(6) Uani 1 1 d . . . H46 H 1.4199 0.2996 -0.6580 0.034 Uiso 1 1 calc R . . O1 O 1.19699(18) 0.42563(16) -0.38048(13) 0.0306(5) Uani 1 1 d . . . O2 O 1.32337(18) 0.35521(16) -0.50922(13) 0.0316(5) Uani 1 1 d . . . O3 O 1.06659(19) 0.63233(17) -0.00835(14) 0.0352(5) Uani 1 1 d . . . O4 O 0.87388(19) 0.77583(16) 0.03879(13) 0.0332(5) Uani 1 1 d . . . O5 O 0.72723(18) 0.87970(17) -0.06777(14) 0.0346(5) Uani 1 1 d . . . O6 O 1.75020(18) 0.10710(17) -0.85661(13) 0.0347(5) Uani 1 1 d . . . O7 O 1.71505(19) 0.14142(17) -1.01471(14) 0.0358(5) Uani 1 1 d . . . O8 O 1.53162(18) 0.29049(17) -1.06605(13) 0.0335(5) Uani 1 1 d . . . O9 O 1.52350(18) 0.18124(16) -0.58733(14) 0.0335(5) Uani 1 1 d . . . O10 O 1.65058(19) 0.16079(19) -0.50264(15) 0.0413(6) Uani 1 1 d . . . O11 O 1.1760(2) 0.41419(18) -0.19469(15) 0.0479(6) Uani 1 1 d . . . C1 C 0.9761(3) 0.6820(2) -0.2919(2) 0.0278(7) Uani 1 1 d . . . C2 C 0.9490(3) 0.7476(3) -0.3707(2) 0.0323(7) Uani 1 1 d . . . H2 H 0.9010 0.8189 -0.3783 0.039 Uiso 1 1 calc R . . C3 C 1.0037(3) 0.6918(2) -0.4368(2) 0.0323(7) Uani 1 1 d . . . H3 H 1.0004 0.7180 -0.4973 0.039 Uiso 1 1 calc R . . C4 C 1.0638(3) 0.5905(2) -0.39764(19) 0.0270(7) Uani 1 1 d . . . C5 C 1.1407(3) 0.5037(2) -0.4345(2) 0.0276(7) Uani 1 1 d . . . C6 C 1.1622(3) 0.5026(2) -0.52252(19) 0.0283(7) Uani 1 1 d . . . H6 H 1.1122 0.5521 -0.5580 0.034 Uiso 1 1 calc R . . C7 C 1.2570(3) 0.4290(2) -0.55893(19) 0.0266(7) Uani 1 1 d . . . C8 C 1.2903(3) 0.4336(2) -0.65141(19) 0.0279(7) Uani 1 1 d . . . C9 C 1.2453(3) 0.5061(2) -0.7204(2) 0.0302(7) Uani 1 1 d . . . H9 H 1.1844 0.5685 -0.7156 0.036 Uiso 1 1 calc R . . C10 C 1.3041(3) 0.4722(2) -0.7978(2) 0.0302(7) Uani 1 1 d . . . H10 H 1.2904 0.5072 -0.8550 0.036 Uiso 1 1 calc R . . C11 C 1.3871(3) 0.3776(2) -0.77710(19) 0.0280(7) Uani 1 1 d . . . C12 C 0.9488(3) 0.7056(2) -0.2055(2) 0.0274(7) Uani 1 1 d . . . C13 C 1.0242(3) 0.6533(2) -0.14926(19) 0.0273(7) Uani 1 1 d . . . H13 H 1.0920 0.6002 -0.1658 0.033 Uiso 1 1 calc R . . C14 C 0.9992(3) 0.6796(2) -0.0688(2) 0.0284(7) Uani 1 1 d . . . C15 C 0.8995(3) 0.7563(2) -0.04437(19) 0.0281(7) Uani 1 1 d . . . C16 C 0.8243(3) 0.8082(2) -0.0999(2) 0.0293(7) Uani 1 1 d . . . C17 C 0.8487(3) 0.7832(2) -0.1814(2) 0.0293(7) Uani 1 1 d . . . H17 H 0.7976 0.8187 -0.2200 0.035 Uiso 1 1 calc R . . C18 C 1.1759(3) 0.5591(3) -0.0338(2) 0.0370(8) Uani 1 1 d . . . H18 H 1.1510 0.4950 -0.0463 0.055 Uiso 1 1 calc R . . H18A H 1.2139 0.5293 0.0155 0.055 Uiso 1 1 calc R . . H18B H 1.2375 0.6028 -0.0881 0.055 Uiso 1 1 calc R . . C19 C 0.9048(3) 0.8883(3) 0.0325(2) 0.0426(8) Uani 1 1 d . . . H19 H 0.9917 0.9027 -0.0068 0.064 Uiso 1 1 calc R . . H19A H 0.8975 0.8916 0.0928 0.064 Uiso 1 1 calc R . . H19B H 0.8463 0.9467 0.0071 0.064 Uiso 1 1 calc R . . C20 C 0.6597(3) 0.9511(3) -0.1278(2) 0.0375(8) Uani 1 1 d . . . H20 H 0.7198 0.9934 -0.1838 0.056 Uiso 1 1 calc R . . H20A H 0.6015 1.0055 -0.0991 0.056 Uiso 1 1 calc R . . H20B H 0.6116 0.9034 -0.1416 0.056 Uiso 1 1 calc R . . C21 C 1.4728(3) 0.3132(2) -0.83684(19) 0.0271(7) Uani 1 1 d . . . C22 C 1.5690(3) 0.2361(2) -0.8121(2) 0.0292(7) Uani 1 1 d . . . H22 H 1.5780 0.2207 -0.7538 0.035 Uiso 1 1 calc R . . C23 C 1.6514(3) 0.1818(2) -0.87321(19) 0.0276(7) Uani 1 1 d . . . C24 C 1.6368(3) 0.2018(2) -0.9579(2) 0.0288(7) Uani 1 1 d . . . C25 C 1.5401(3) 0.2779(2) -0.98203(19) 0.0291(7) Uani 1 1 d . . . C26 C 1.4588(3) 0.3345(2) -0.92209(19) 0.0284(7) Uani 1 1 d . . . H26 H 1.3939 0.3874 -0.9392 0.034 Uiso 1 1 calc R . . C27 C 1.7744(3) 0.0893(3) -0.7727(2) 0.0375(8) Uani 1 1 d . . . H27 H 1.7906 0.1627 -0.7685 0.056 Uiso 1 1 calc R . . H27A H 1.8486 0.0359 -0.7697 0.056 Uiso 1 1 calc R . . H27B H 1.7008 0.0570 -0.7224 0.056 Uiso 1 1 calc R . . C28 C 1.8071(3) 0.2094(3) -1.0911(2) 0.0432(8) Uani 1 1 d . . . H28 H 1.7641 0.2641 -1.1322 0.065 Uiso 1 1 calc R . . H28A H 1.8674 0.1590 -1.1230 0.065 Uiso 1 1 calc R . . H28B H 1.8523 0.2513 -1.0702 0.065 Uiso 1 1 calc R . . C29 C 1.4308(3) 0.3658(3) -1.0923(2) 0.0341(7) Uani 1 1 d . . . H29 H 1.3494 0.3354 -1.0521 0.051 Uiso 1 1 calc R . . H29A H 1.4379 0.3712 -1.1547 0.051 Uiso 1 1 calc R . . H29B H 1.4365 0.4421 -1.0883 0.051 Uiso 1 1 calc R . . C30 C 1.1573(3) 0.2290(3) -0.3847(2) 0.0322(7) Uani 1 1 d . . . C31 C 1.0335(3) 0.2334(3) -0.3263(2) 0.0394(8) Uani 1 1 d . . . H31 H 1.0084 0.2921 -0.2972 0.047 Uiso 1 1 calc R . . C32 C 0.9473(3) 0.1546(3) -0.3101(2) 0.0430(8) Uani 1 1 d . . . H32 H 0.8637 0.1613 -0.2717 0.052 Uiso 1 1 calc R . . C33 C 0.9817(3) 0.0659(3) -0.3493(2) 0.0427(8) Uani 1 1 d . . . H33 H 0.9225 0.0114 -0.3373 0.051 Uiso 1 1 calc R . . C34 C 1.1032(3) 0.0576(3) -0.4062(2) 0.0402(8) Uani 1 1 d . . . H34 H 1.1282 -0.0032 -0.4330 0.048 Uiso 1 1 calc R . . C35 C 1.1888(3) 0.1385(3) -0.4240(2) 0.0370(8) Uani 1 1 d . . . H35 H 1.2714 0.1324 -0.4641 0.044 Uiso 1 1 calc R . . C36 C 1.3655(3) 0.2753(3) -0.3554(2) 0.0357(7) Uani 1 1 d . . . C37 C 1.3433(3) 0.1889(3) -0.2727(2) 0.0354(7) Uani 1 1 d . . . H37 H 1.2685 0.1484 -0.2511 0.043 Uiso 1 1 calc R . . C38 C 1.4256(3) 0.1599(3) -0.2211(2) 0.0393(8) Uani 1 1 d . . . H38 H 1.4065 0.1014 -0.1649 0.047 Uiso 1 1 calc R . . C39 C 1.5355(3) 0.2168(3) -0.2522(2) 0.0389(8) Uani 1 1 d . . . H39 H 1.5923 0.1982 -0.2171 0.047 Uiso 1 1 calc R . . C40 C 1.5629(3) 0.3009(3) -0.3345(2) 0.0440(9) Uani 1 1 d . . . H40 H 1.6400 0.3384 -0.3570 0.053 Uiso 1 1 calc R . . C41 C 1.4783(3) 0.3306(3) -0.3840(2) 0.0388(8) Uani 1 1 d . . . H41 H 1.4972 0.3905 -0.4394 0.047 Uiso 1 1 calc R . . C42 C 1.6616(4) 0.3293(3) -0.6238(3) 0.0604(11) Uani 1 1 d . . . H42 H 1.7377 0.3174 -0.6719 0.091 Uiso 1 1 calc R . . H42A H 1.6845 0.3614 -0.5841 0.091 Uiso 1 1 calc R . . H42B H 1.6008 0.3825 -0.6506 0.091 Uiso 1 1 calc R . . C43 C 1.6037(3) 0.2176(3) -0.5704(2) 0.0345(7) Uani 1 1 d . . . C44 C 1.5922(3) 0.0552(3) -0.4429(2) 0.0405(8) Uani 1 1 d . . . H44 H 1.5940 0.0031 -0.4782 0.049 Uiso 1 1 calc R . . H44A H 1.5029 0.0719 -0.4106 0.049 Uiso 1 1 calc R . . C45 C 1.6652(3) 0.0000(3) -0.3765(2) 0.0511(9) Uani 1 1 d . . . H45 H 1.7529 -0.0176 -0.4090 0.077 Uiso 1 1 calc R . . H45A H 1.6266 -0.0710 -0.3346 0.077 Uiso 1 1 calc R . . H45B H 1.6637 0.0527 -0.3425 0.077 Uiso 1 1 calc R . . B1 B 1.2610(3) 0.3190(3) -0.4074(2) 0.0318(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0285(13) 0.0284(13) 0.0259(14) -0.0086(11) -0.0081(11) 0.0015(10) N2 0.0282(13) 0.0293(13) 0.0281(14) -0.0096(11) -0.0086(11) 0.0015(10) O1 0.0332(11) 0.0305(11) 0.0284(12) -0.0117(9) -0.0093(9) 0.0046(9) O2 0.0325(11) 0.0342(11) 0.0282(12) -0.0113(9) -0.0100(9) 0.0045(9) O3 0.0380(12) 0.0379(12) 0.0336(12) -0.0157(10) -0.0158(10) 0.0085(9) O4 0.0407(12) 0.0306(11) 0.0293(12) -0.0132(9) -0.0092(10) 0.0015(9) O5 0.0357(12) 0.0353(12) 0.0322(12) -0.0148(10) -0.0107(10) 0.0114(9) O6 0.0342(12) 0.0407(12) 0.0298(12) -0.0142(10) -0.0135(10) 0.0129(9) O7 0.0388(12) 0.0363(12) 0.0306(12) -0.0154(10) -0.0076(10) 0.0088(10) O8 0.0338(11) 0.0409(12) 0.0278(12) -0.0142(10) -0.0122(9) 0.0077(9) O9 0.0317(11) 0.0369(12) 0.0362(13) -0.0146(10) -0.0134(10) 0.0012(9) O10 0.0360(12) 0.0515(14) 0.0420(14) -0.0142(11) -0.0178(11) -0.0036(10) O11 0.0675(16) 0.0407(13) 0.0362(13) -0.0169(11) -0.0190(12) 0.0144(11) C1 0.0267(15) 0.0276(16) 0.0292(17) -0.0104(13) -0.0069(13) -0.0011(12) C2 0.0330(17) 0.0307(16) 0.0334(18) -0.0118(14) -0.0110(14) 0.0046(13) C3 0.0330(17) 0.0340(17) 0.0298(17) -0.0102(14) -0.0109(14) 0.0033(13) C4 0.0264(15) 0.0299(16) 0.0273(17) -0.0134(13) -0.0064(13) -0.0020(12) C5 0.0255(15) 0.0271(15) 0.0280(17) -0.0069(13) -0.0053(13) -0.0041(12) C6 0.0269(16) 0.0327(16) 0.0271(16) -0.0119(13) -0.0094(13) 0.0029(12) C7 0.0239(15) 0.0253(15) 0.0294(17) -0.0072(13) -0.0056(13) -0.0051(12) C8 0.0264(15) 0.0323(16) 0.0249(16) -0.0127(13) -0.0040(13) -0.0003(12) C9 0.0307(16) 0.0291(16) 0.0300(17) -0.0108(13) -0.0080(14) 0.0030(13) C10 0.0310(16) 0.0344(17) 0.0234(16) -0.0089(13) -0.0077(13) 0.0034(13) C11 0.0274(16) 0.0327(16) 0.0251(16) -0.0111(13) -0.0058(13) -0.0046(13) C12 0.0278(15) 0.0261(15) 0.0289(17) -0.0113(13) -0.0064(13) -0.0007(12) C13 0.0286(16) 0.0280(15) 0.0240(16) -0.0096(13) -0.0049(13) 0.0001(12) C14 0.0287(16) 0.0276(16) 0.0309(17) -0.0083(13) -0.0127(14) 0.0008(12) C15 0.0335(16) 0.0289(16) 0.0248(16) -0.0144(13) -0.0074(13) 0.0007(13) C16 0.0268(15) 0.0252(15) 0.0346(18) -0.0115(13) -0.0066(13) 0.0024(12) C17 0.0325(16) 0.0268(16) 0.0297(17) -0.0088(13) -0.0107(14) -0.0004(13) C18 0.0323(17) 0.0387(18) 0.044(2) -0.0160(15) -0.0173(15) 0.0090(14) C19 0.055(2) 0.0361(18) 0.047(2) -0.0221(16) -0.0207(17) 0.0006(16) C20 0.0407(19) 0.0345(17) 0.0368(19) -0.0096(15) -0.0157(16) 0.0060(14) C21 0.0239(15) 0.0295(16) 0.0277(17) -0.0120(13) -0.0035(13) -0.0024(12) C22 0.0288(16) 0.0317(16) 0.0278(17) -0.0102(13) -0.0081(13) -0.0012(13) C23 0.0250(15) 0.0291(16) 0.0274(17) -0.0085(13) -0.0074(13) 0.0010(12) C24 0.0237(15) 0.0313(16) 0.0312(17) -0.0155(13) -0.0038(13) 0.0027(12) C25 0.0281(16) 0.0342(17) 0.0252(16) -0.0104(13) -0.0053(13) -0.0048(13) C26 0.0274(16) 0.0304(16) 0.0268(17) -0.0100(13) -0.0065(13) 0.0003(12) C27 0.0395(18) 0.0405(18) 0.0346(19) -0.0123(15) -0.0159(15) 0.0051(14) C28 0.0381(19) 0.051(2) 0.036(2) -0.0196(16) -0.0026(16) 0.0061(16) C29 0.0306(17) 0.0398(18) 0.0324(18) -0.0126(14) -0.0116(14) 0.0057(14) C30 0.0329(17) 0.0354(17) 0.0271(17) -0.0092(14) -0.0097(14) 0.0027(13) C31 0.0377(18) 0.0450(19) 0.0345(19) -0.0153(16) -0.0065(15) -0.0016(15) C32 0.0359(18) 0.061(2) 0.0328(19) -0.0174(17) -0.0044(15) -0.0091(16) C33 0.045(2) 0.043(2) 0.041(2) -0.0108(16) -0.0130(16) -0.0079(16) C34 0.044(2) 0.0395(19) 0.0376(19) -0.0140(15) -0.0113(16) -0.0012(15) C35 0.0333(17) 0.0419(19) 0.0379(19) -0.0170(15) -0.0106(15) 0.0030(14) C36 0.0362(18) 0.0341(17) 0.0358(19) -0.0156(15) -0.0066(15) 0.0027(14) C37 0.0342(17) 0.0333(17) 0.0385(19) -0.0119(15) -0.0106(15) 0.0015(14) C38 0.0397(19) 0.0406(19) 0.039(2) -0.0137(15) -0.0146(16) 0.0059(15) C39 0.0429(19) 0.0411(19) 0.042(2) -0.0192(16) -0.0196(16) 0.0026(15) C40 0.0402(19) 0.043(2) 0.053(2) -0.0162(18) -0.0189(17) -0.0005(15) C41 0.0360(18) 0.0387(18) 0.040(2) -0.0102(15) -0.0107(16) -0.0017(14) C42 0.059(2) 0.073(3) 0.049(2) -0.003(2) -0.017(2) -0.031(2) C43 0.0281(16) 0.0465(19) 0.0321(18) -0.0149(15) -0.0101(14) -0.0018(14) C44 0.044(2) 0.0374(18) 0.044(2) -0.0177(16) -0.0174(17) 0.0077(15) C45 0.056(2) 0.055(2) 0.049(2) -0.0205(19) -0.0279(19) 0.0136(18) B1 0.035(2) 0.037(2) 0.0234(19) -0.0133(16) -0.0064(16) 0.0037(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 N1 C1 1.366(3) . ? N1 C4 1.387(3) . ? N1 H1 0.8800 . ? N2 C11 1.368(4) . ? N2 C8 1.391(3) . ? N2 H46 0.8800 . ? O1 C5 1.318(3) . ? O1 B1 1.520(4) . ? O2 C7 1.325(3) . ? O2 B1 1.522(4) . ? O3 C14 1.371(3) . ? O3 C18 1.431(3) . ? O4 C15 1.390(3) . ? O4 C19 1.448(3) . ? O5 C16 1.364(3) . ? O5 C20 1.428(3) . ? O6 C23 1.367(3) . ? O6 C27 1.432(3) . ? O7 C24 1.377(3) . ? O7 C28 1.440(4) . ? O8 C25 1.370(3) . ? O8 C29 1.435(3) . ? O9 C43 1.211(3) . ? O10 C43 1.330(4) . ? O10 C44 1.450(4) . ? C1 C2 1.386(4) . ? C1 C12 1.463(4) . ? C2 C3 1.391(4) . ? C2 H2 0.9500 . ? C3 C4 1.389(4) . ? C3 H3 0.9500 . ? C4 C5 1.429(4) . ? C5 C6 1.386(4) . ? C6 C7 1.392(4) . ? C6 H6 0.9500 . ? C7 C8 1.421(4) . ? C8 C9 1.384(4) . ? C9 C10 1.387(4) . ? C9 H9 0.9500 . ? C10 C11 1.397(4) . ? C10 H10 0.9500 . ? C11 C21 1.468(4) . ? C12 C13 1.394(4) . ? C12 C17 1.395(4) . ? C13 C14 1.389(4) . ? C13 H13 0.9500 . ? C14 C15 1.386(4) . ? C15 C16 1.383(4) . ? C16 C17 1.399(4) . ? C17 H17 0.9500 . ? C18 H18 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 H19 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C20 H20 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 C26 1.395(4) . ? C21 C22 1.396(4) . ? C22 C23 1.390(4) . ? C22 H22 0.9500 . ? C23 C24 1.390(4) . ? C24 C25 1.392(4) . ? C25 C26 1.391(4) . ? C26 H26 0.9500 . ? C27 H27 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 H28 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 H29 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 C31 1.406(4) . ? C30 C35 1.407(4) . ? C30 B1 1.608(5) . ? C31 C32 1.384(4) . ? C31 H31 0.9500 . ? C32 C33 1.385(4) . ? C32 H32 0.9500 . ? C33 C34 1.383(4) . ? C33 H33 0.9500 . ? C34 C35 1.391(4) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.399(4) . ? C36 C41 1.401(4) . ? C36 B1 1.600(5) . ? C37 C38 1.384(4) . ? C37 H37 0.9500 . ? C38 C39 1.380(4) . ? C38 H38 0.9500 . ? C39 C40 1.383(5) . ? C39 H39 0.9500 . ? C40 C41 1.380(4) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C43 1.488(4) . ? C42 H42 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C44 C45 1.503(4) . ? C44 H44 0.9900 . ? C44 H44A 0.9900 . ? C45 H45 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 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 C1 N1 C4 109.3(2) . . ? C1 N1 H1 125.3 . . ? C4 N1 H1 125.3 . . ? C11 N2 C8 110.0(2) . . ? C11 N2 H46 125.0 . . ? C8 N2 H46 125.0 . . ? C5 O1 B1 118.8(2) . . ? C7 O2 B1 116.7(2) . . ? C14 O3 C18 117.5(2) . . ? C15 O4 C19 114.0(2) . . ? C16 O5 C20 118.1(2) . . ? C23 O6 C27 117.4(2) . . ? C24 O7 C28 114.1(2) . . ? C25 O8 C29 117.2(2) . . ? C43 O10 C44 116.3(2) . . ? N1 C1 C2 107.3(2) . . ? N1 C1 C12 122.1(3) . . ? C2 C1 C12 130.6(3) . . ? C1 C2 C3 108.7(3) . . ? C1 C2 H2 125.6 . . ? C3 C2 H2 125.6 . . ? C4 C3 C2 107.1(3) . . ? C4 C3 H3 126.4 . . ? C2 C3 H3 126.4 . . ? N1 C4 C3 107.5(2) . . ? N1 C4 C5 120.7(3) . . ? C3 C4 C5 131.6(3) . . ? O1 C5 C6 120.9(3) . . ? O1 C5 C4 115.5(3) . . ? C6 C5 C4 123.6(3) . . ? C5 C6 C7 120.0(3) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? O2 C7 C6 120.9(3) . . ? O2 C7 C8 117.4(3) . . ? C6 C7 C8 121.6(3) . . ? C9 C8 N2 106.6(2) . . ? C9 C8 C7 130.6(3) . . ? N2 C8 C7 122.7(3) . . ? C8 C9 C10 108.4(3) . . ? C8 C9 H9 125.8 . . ? C10 C9 H9 125.8 . . ? C9 C10 C11 108.2(3) . . ? C9 C10 H10 125.9 . . ? C11 C10 H10 125.9 . . ? N2 C11 C10 106.8(2) . . ? N2 C11 C21 124.4(3) . . ? C10 C11 C21 128.7(3) . . ? C13 C12 C17 120.6(3) . . ? C13 C12 C1 120.2(3) . . ? C17 C12 C1 119.2(3) . . ? C14 C13 C12 119.4(3) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? O3 C14 C15 115.7(3) . . ? O3 C14 C13 124.1(3) . . ? C15 C14 C13 120.3(3) . . ? C16 C15 C14 120.5(3) . . ? C16 C15 O4 121.0(3) . . ? C14 C15 O4 118.4(3) . . ? O5 C16 C15 115.3(3) . . ? O5 C16 C17 124.7(3) . . ? C15 C16 C17 119.9(3) . . ? C12 C17 C16 119.3(3) . . ? C12 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? O3 C18 H18 109.5 . . ? O3 C18 H18A 109.5 . . ? H18 C18 H18A 109.5 . . ? O3 C18 H18B 109.5 . . ? H18 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O4 C19 H19 109.5 . . ? O4 C19 H19A 109.5 . . ? H19 C19 H19A 109.5 . . ? O4 C19 H19B 109.5 . . ? H19 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O5 C20 H20 109.5 . . ? O5 C20 H20A 109.5 . . ? H20 C20 H20A 109.5 . . ? O5 C20 H20B 109.5 . . ? H20 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C26 C21 C22 120.0(3) . . ? C26 C21 C11 117.8(3) . . ? C22 C21 C11 122.2(3) . . ? C23 C22 C21 119.7(3) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? O6 C23 C22 124.4(3) . . ? O6 C23 C24 115.2(2) . . ? C22 C23 C24 120.4(3) . . ? O7 C24 C23 119.0(2) . . ? O7 C24 C25 121.2(3) . . ? C23 C24 C25 119.7(3) . . ? O8 C25 C26 124.1(3) . . ? O8 C25 C24 115.6(2) . . ? C26 C25 C24 120.3(3) . . ? C25 C26 C21 119.8(3) . . ? C25 C26 H26 120.1 . . ? C21 C26 H26 120.1 . . ? O6 C27 H27 109.5 . . ? O6 C27 H27A 109.5 . . ? H27 C27 H27A 109.5 . . ? O6 C27 H27B 109.5 . . ? H27 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O7 C28 H28 109.5 . . ? O7 C28 H28A 109.5 . . ? H28 C28 H28A 109.5 . . ? O7 C28 H28B 109.5 . . ? H28 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O8 C29 H29 109.5 . . ? O8 C29 H29A 109.5 . . ? H29 C29 H29A 109.5 . . ? O8 C29 H29B 109.5 . . ? H29 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C31 C30 C35 116.0(3) . . ? C31 C30 B1 124.1(3) . . ? C35 C30 B1 119.9(3) . . ? C32 C31 C30 121.7(3) . . ? C32 C31 H31 119.1 . . ? C30 C31 H31 119.1 . . ? C31 C32 C33 120.7(3) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C34 C33 C32 119.2(3) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C33 C34 C35 119.9(3) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C34 C35 C30 122.3(3) . . ? C34 C35 H35 118.8 . . ? C30 C35 H35 118.8 . . ? C37 C36 C41 115.7(3) . . ? C37 C36 B1 122.0(3) . . ? C41 C36 B1 121.8(3) . . ? C38 C37 C36 122.9(3) . . ? C38 C37 H37 118.5 . . ? C36 C37 H37 118.5 . . ? C39 C38 C37 119.3(3) . . ? C39 C38 H38 120.4 . . ? C37 C38 H38 120.4 . . ? C38 C39 C40 119.8(3) . . ? C38 C39 H39 120.1 . . ? C40 C39 H39 120.1 . . ? C41 C40 C39 120.0(3) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 C36 122.2(3) . . ? C40 C41 H41 118.9 . . ? C36 C41 H41 118.9 . . ? C43 C42 H42 109.5 . . ? C43 C42 H42A 109.5 . . ? H42 C42 H42A 109.5 . . ? C43 C42 H42B 109.5 . . ? H42 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? O9 C43 O10 123.4(3) . . ? O9 C43 C42 123.7(3) . . ? O10 C43 C42 112.9(3) . . ? O10 C44 C45 107.9(3) . . ? O10 C44 H44 110.1 . . ? C45 C44 H44 110.1 . . ? O10 C44 H44A 110.1 . . ? C45 C44 H44A 110.1 . . ? H44 C44 H44A 108.4 . . ? C44 C45 H45 109.5 . . ? C44 C45 H45A 109.5 . . ? H45 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? O1 B1 O2 107.8(2) . . ? O1 B1 C36 104.6(2) . . ? O2 B1 C36 110.7(2) . . ? O1 B1 C30 110.1(2) . . ? O2 B1 C30 107.8(2) . . ? C36 B1 C30 115.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 N1 C1 C2 1.2(3) . . . . ? C4 N1 C1 C12 -175.5(2) . . . . ? N1 C1 C2 C3 -1.1(3) . . . . ? C12 C1 C2 C3 175.2(3) . . . . ? C1 C2 C3 C4 0.5(3) . . . . ? C1 N1 C4 C3 -0.9(3) . . . . ? C1 N1 C4 C5 175.6(2) . . . . ? C2 C3 C4 N1 0.2(3) . . . . ? C2 C3 C4 C5 -175.8(3) . . . . ? B1 O1 C5 C6 -14.1(4) . . . . ? B1 O1 C5 C4 169.2(2) . . . . ? N1 C4 C5 O1 -4.2(4) . . . . ? C3 C4 C5 O1 171.3(3) . . . . ? N1 C4 C5 C6 179.2(3) . . . . ? C3 C4 C5 C6 -5.3(5) . . . . ? O1 C5 C6 C7 -9.1(4) . . . . ? C4 C5 C6 C7 167.3(3) . . . . ? B1 O2 C7 C6 24.4(4) . . . . ? B1 O2 C7 C8 -158.4(2) . . . . ? C5 C6 C7 O2 3.5(4) . . . . ? C5 C6 C7 C8 -173.6(3) . . . . ? C11 N2 C8 C9 0.0(3) . . . . ? C11 N2 C8 C7 177.7(2) . . . . ? O2 C7 C8 C9 -174.8(3) . . . . ? C6 C7 C8 C9 2.3(5) . . . . ? O2 C7 C8 N2 8.1(4) . . . . ? C6 C7 C8 N2 -174.7(3) . . . . ? N2 C8 C9 C10 0.1(3) . . . . ? C7 C8 C9 C10 -177.3(3) . . . . ? C8 C9 C10 C11 -0.2(3) . . . . ? C8 N2 C11 C10 -0.1(3) . . . . ? C8 N2 C11 C21 178.4(2) . . . . ? C9 C10 C11 N2 0.2(3) . . . . ? C9 C10 C11 C21 -178.3(3) . . . . ? N1 C1 C12 C13 21.5(4) . . . . ? C2 C1 C12 C13 -154.3(3) . . . . ? N1 C1 C12 C17 -160.2(3) . . . . ? C2 C1 C12 C17 24.0(5) . . . . ? C17 C12 C13 C14 -0.3(4) . . . . ? C1 C12 C13 C14 177.9(2) . . . . ? C18 O3 C14 C15 -175.6(2) . . . . ? C18 O3 C14 C13 5.6(4) . . . . ? C12 C13 C14 O3 179.3(3) . . . . ? C12 C13 C14 C15 0.6(4) . . . . ? O3 C14 C15 C16 -179.3(3) . . . . ? C13 C14 C15 C16 -0.4(4) . . . . ? O3 C14 C15 O4 -2.1(4) . . . . ? C13 C14 C15 O4 176.8(2) . . . . ? C19 O4 C15 C16 -73.4(3) . . . . ? C19 O4 C15 C14 109.4(3) . . . . ? C20 O5 C16 C15 169.2(3) . . . . ? C20 O5 C16 C17 -12.5(4) . . . . ? C14 C15 C16 O5 178.4(2) . . . . ? O4 C15 C16 O5 1.2(4) . . . . ? C14 C15 C16 C17 0.0(4) . . . . ? O4 C15 C16 C17 -177.2(2) . . . . ? C13 C12 C17 C16 -0.1(4) . . . . ? C1 C12 C17 C16 -178.4(3) . . . . ? O5 C16 C17 C12 -178.0(3) . . . . ? C15 C16 C17 C12 0.2(4) . . . . ? N2 C11 C21 C26 170.5(2) . . . . ? C10 C11 C21 C26 -11.3(4) . . . . ? N2 C11 C21 C22 -11.9(4) . . . . ? C10 C11 C21 C22 166.4(3) . . . . ? C26 C21 C22 C23 0.8(4) . . . . ? C11 C21 C22 C23 -176.7(3) . . . . ? C27 O6 C23 C22 -3.9(4) . . . . ? C27 O6 C23 C24 176.0(3) . . . . ? C21 C22 C23 O6 178.4(3) . . . . ? C21 C22 C23 C24 -1.5(4) . . . . ? C28 O7 C24 C23 -108.7(3) . . . . ? C28 O7 C24 C25 74.4(3) . . . . ? O6 C23 C24 O7 4.1(4) . . . . ? C22 C23 C24 O7 -176.0(2) . . . . ? O6 C23 C24 C25 -179.0(2) . . . . ? C22 C23 C24 C25 0.9(4) . . . . ? C29 O8 C25 C26 -0.9(4) . . . . ? C29 O8 C25 C24 178.3(2) . . . . ? O7 C24 C25 O8 -1.9(4) . . . . ? C23 C24 C25 O8 -178.8(2) . . . . ? O7 C24 C25 C26 177.3(3) . . . . ? C23 C24 C25 C26 0.4(4) . . . . ? O8 C25 C26 C21 178.0(3) . . . . ? C24 C25 C26 C21 -1.1(4) . . . . ? C22 C21 C26 C25 0.5(4) . . . . ? C11 C21 C26 C25 178.2(3) . . . . ? C35 C30 C31 C32 -1.3(5) . . . . ? B1 C30 C31 C32 179.1(3) . . . . ? C30 C31 C32 C33 1.9(5) . . . . ? C31 C32 C33 C34 -0.9(5) . . . . ? C32 C33 C34 C35 -0.6(5) . . . . ? C33 C34 C35 C30 1.2(5) . . . . ? C31 C30 C35 C34 -0.2(5) . . . . ? B1 C30 C35 C34 179.4(3) . . . . ? C41 C36 C37 C38 0.9(4) . . . . ? B1 C36 C37 C38 -171.6(3) . . . . ? C36 C37 C38 C39 -0.9(5) . . . . ? C37 C38 C39 C40 -0.7(5) . . . . ? C38 C39 C40 C41 2.2(5) . . . . ? C39 C40 C41 C36 -2.3(5) . . . . ? C37 C36 C41 C40 0.7(5) . . . . ? B1 C36 C41 C40 173.2(3) . . . . ? C44 O10 C43 O9 -5.6(4) . . . . ? C44 O10 C43 C42 175.3(3) . . . . ? C43 O10 C44 C45 175.4(3) . . . . ? C5 O1 B1 O2 37.9(3) . . . . ? C5 O1 B1 C36 155.7(2) . . . . ? C5 O1 B1 C30 -79.4(3) . . . . ? C7 O2 B1 O1 -42.7(3) . . . . ? C7 O2 B1 C36 -156.5(2) . . . . ? C7 O2 B1 C30 76.0(3) . . . . ? C37 C36 B1 O1 96.8(3) . . . . ? C41 C36 B1 O1 -75.2(3) . . . . ? C37 C36 B1 O2 -147.4(3) . . . . ? C41 C36 B1 O2 40.6(4) . . . . ? C37 C36 B1 C30 -24.5(4) . . . . ? C41 C36 B1 C30 163.5(3) . . . . ? C31 C30 B1 O1 -16.6(4) . . . . ? C35 C30 B1 O1 163.8(3) . . . . ? C31 C30 B1 O2 -133.9(3) . . . . ? C35 C30 B1 O2 46.5(4) . . . . ? C31 C30 B1 C36 101.6(3) . . . . ? C35 C30 B1 C36 -78.0(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O11 0.88 2.04 2.900(3) 167.0 . N2 H46 O9 0.88 2.02 2.899(3) 175.4 . _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 64.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.445 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.058