# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _Journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author 'Victor Barba' _publ_contact_author_email vbarba@ciq.uaem.mx #-------------------------------------------------------------------------- #Publication details loop_ _publ_author_name _publ_author_address 'Victor Barba' ; Centro de Investigaciones Quimicas-UAEM ; 'Herbert Höpfl' ; Centro de Investigaciones Quimicas-UAEM ; 'Norberto Farfan' ; Centro de Investigacion y de Estudios Avanzados-IPN ; 'Rosa Santillan' ; Centro de Investigacion y de estudios Avanzados-IPN ; 'Hiram I. Beltran' ; Instituto Mexicano del Petroleo ; Luis S. Zamudio' ; Instituto mexicano del petroleo ; _publ_contact_author_name 'Victor Barba' data_complex_1a _database_code_depnum_ccdc_archive 'CCDC 230230' _audit_creation_method SHELXL-97 #Chemical and physical data _chemical_name_systematic ; Trimethoxy-[tris-[mu-(3-phenyl-kC)imine-kN]methyl-2-(3,5-di-tert- butyl)phenolate-kO)triboro' ; _chemical_name_common ; Trimethoxy-(tris-(mu-(3-phenyl-kC)imine-kN)methyl-2-(3,5-di- tert-butyl)phenolate-kO)triboro' ; _chemical_melting_point 298 _chemical_formula_moiety ? _chemical_formula_sum 'C70 H92 B3 N3 O7' _chemical_formula_weight 1119.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8178(6) _cell_length_b 13.8784(7) _cell_length_c 23.1363(12) _cell_angle_alpha 79.6780(10) _cell_angle_beta 79.4780(10) _cell_angle_gamma 65.2830(10) _cell_volume 3366.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rectangular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.105 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27636 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0596 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 23.00 _reflns_number_total 9358 _reflns_number_gt 7418 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Cell parameters were determined by least squares refinements on diffractometer angles for 24 automatically centered reflections collected on three sets of 20 frames each. Non-hydrogen atoms were refined anisotropically. Hydrogen atoms were placed in geometrically calculated positionsusing a riding model. Two disordered tBu groups,DFIX and EADP instructions have been used. One THF molecule in the cage. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.0764P)^2^+2.4309P] 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 9358 _refine_ls_number_parameters 807 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0937 _refine_ls_R_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.1784 _refine_ls_wR_factor_gt 0.1680 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.074 _refine_ls_shift/su_mean 0.005 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.5986(4) 0.6948(3) 0.22472(17) 0.0241(9) Uani 1 1 d . . . B31 B 0.7446(4) 0.2605(3) 0.39274(17) 0.0273(10) Uani 1 1 d . . . B61 B 0.8601(4) 0.2496(3) 0.11775(17) 0.0231(9) Uani 1 1 d . . . N1 N 0.5779(2) 0.6296(2) 0.28801(12) 0.0223(6) Uani 1 1 d . . . N31 N 0.7548(2) 0.1981(2) 0.33842(11) 0.0218(6) Uani 1 1 d . . . N61 N 0.7548(2) 0.3727(2) 0.11395(11) 0.0181(6) Uani 1 1 d . . . O1 O 0.4771(2) 0.73434(17) 0.19943(9) 0.0248(5) Uani 1 1 d . . . O2 O 0.6332(2) 0.77719(17) 0.23280(10) 0.0271(6) Uani 1 1 d . . . O31 O 0.6105(2) 0.29654(18) 0.42043(9) 0.0275(6) Uani 1 1 d . . . O32 O 0.8305(2) 0.18103(18) 0.43083(10) 0.0307(6) Uani 1 1 d . . . O61 O 0.79358(19) 0.18263(16) 0.11117(9) 0.0225(5) Uani 1 1 d . . . O62 O 0.9608(2) 0.24104(17) 0.07233(9) 0.0238(5) Uani 1 1 d . . . C1 C 0.3648(3) 0.7530(3) 0.23025(15) 0.0231(8) Uani 1 1 d . . . C2 C 0.3550(3) 0.7156(3) 0.29054(15) 0.0247(8) Uani 1 1 d . . . C3 C 0.2373(3) 0.7318(3) 0.32378(15) 0.0285(8) Uani 1 1 d . . . H3 H 0.2335 0.7058 0.3647 0.034 Uiso 1 1 calc R . . C4 C 0.1283(3) 0.7843(3) 0.29841(16) 0.0298(9) Uani 1 1 d . A . C5 C 0.1418(3) 0.8205(3) 0.23717(16) 0.0300(9) Uani 1 1 d . . . H5 H 0.0669 0.8581 0.2190 0.036 Uiso 1 1 calc R . . C6 C 0.2541(3) 0.8060(3) 0.20142(15) 0.0266(8) Uani 1 1 d . . . C7 C 0.4666(3) 0.6497(3) 0.31580(15) 0.0267(8) Uani 1 1 d . . . H7 H 0.4593 0.6183 0.3556 0.032 Uiso 1 1 calc R . . C8 C 0.6830(3) 0.5455(3) 0.31467(14) 0.0228(8) Uani 1 1 d . . . C9 C 0.6711(3) 0.4524(3) 0.34021(14) 0.0233(8) Uani 1 1 d . . . H9 H 0.5946 0.4456 0.3396 0.028 Uiso 1 1 calc R . . C10 C 0.7676(3) 0.3674(3) 0.36711(14) 0.0236(8) Uani 1 1 d . . . C11 C 0.8788(3) 0.3799(3) 0.36523(15) 0.0288(9) Uani 1 1 d . . . H11 H 0.9472 0.3235 0.3825 0.035 Uiso 1 1 calc R . . C12 C 0.8922(3) 0.4734(3) 0.33847(15) 0.0304(9) Uani 1 1 d . . . H12 H 0.9693 0.4802 0.3375 0.036 Uiso 1 1 calc R . . C13 C 0.7931(3) 0.5567(3) 0.31322(14) 0.0264(8) Uani 1 1 d . . . H13 H 0.8016 0.6208 0.2951 0.032 Uiso 1 1 calc R . . C14 C 0.5484(4) 0.8571(3) 0.26785(17) 0.0383(10) Uani 1 1 d . . . H14A H 0.4710 0.8967 0.2493 0.057 Uiso 1 1 calc R . . H14B H 0.5863 0.9063 0.2713 0.057 Uiso 1 1 calc R . . H14C H 0.5289 0.8239 0.3073 0.057 Uiso 1 1 calc R . . C15 C 0.2603(3) 0.8419(3) 0.13485(16) 0.0362(9) Uani 1 1 d . . . C16 C 0.3306(4) 0.7428(3) 0.10152(17) 0.0462(11) Uani 1 1 d . . . H16A H 0.4146 0.7035 0.1139 0.069 Uiso 1 1 calc R . . H16B H 0.3377 0.7652 0.0588 0.069 Uiso 1 1 calc R . . H16C H 0.2841 0.6966 0.1106 0.069 Uiso 1 1 calc R . . C17 C 0.3270(4) 0.9183(3) 0.11763(18) 0.0456(11) Uani 1 1 d . . . H17A H 0.2833 0.9801 0.1399 0.068 Uiso 1 1 calc R . . H17B H 0.3267 0.9424 0.0751 0.068 Uiso 1 1 calc R . . H17C H 0.4138 0.8814 0.1268 0.068 Uiso 1 1 calc R . . C18 C 0.1292(4) 0.8995(4) 0.11486(18) 0.0543(13) Uani 1 1 d . . . H18A H 0.0849 0.8516 0.1245 0.081 Uiso 1 1 calc R . . H18B H 0.1368 0.9203 0.0720 0.081 Uiso 1 1 calc R . . H18C H 0.0821 0.9634 0.1352 0.081 Uiso 1 1 calc R . . C19 C 0.0000(3) 0.7987(2) 0.33131(13) 0.0342(9) Uani 1 1 d D . . C20A C -0.0636(4) 0.7483(4) 0.3006(2) 0.0460(16) Uani 0.807(7) 1 d PD A 1 H20A H -0.0727 0.7825 0.2598 0.069 Uiso 0.807(7) 1 calc PR A 1 H20B H -0.1466 0.7587 0.3221 0.069 Uiso 0.807(7) 1 calc PR A 1 H20C H -0.0120 0.6718 0.3003 0.069 Uiso 0.807(7) 1 calc PR A 1 C21A C 0.0056(4) 0.7448(4) 0.39559(15) 0.0437(16) Uani 0.807(7) 1 d PD A 1 H21A H 0.0578 0.6683 0.3958 0.066 Uiso 0.807(7) 1 calc PR A 1 H21B H -0.0794 0.7551 0.4143 0.066 Uiso 0.807(7) 1 calc PR A 1 H21C H 0.0419 0.7769 0.4176 0.066 Uiso 0.807(7) 1 calc PR A 1 C22A C -0.0859(5) 0.9180(2) 0.3319(3) 0.0500(17) Uani 0.807(7) 1 d PD A 1 H22A H -0.0526 0.9508 0.3549 0.075 Uiso 0.807(7) 1 calc PR A 1 H22B H -0.1705 0.9256 0.3500 0.075 Uiso 0.807(7) 1 calc PR A 1 H22C H -0.0894 0.9535 0.2913 0.075 Uiso 0.807(7) 1 calc PR A 1 C20B C -0.1096(17) 0.871(3) 0.2956(12) 0.106(9) Uani 0.193(7) 1 d PD A 2 H20D H -0.0962 0.9349 0.2766 0.159 Uiso 0.193(7) 1 calc PR A 2 H20E H -0.1884 0.8916 0.3223 0.159 Uiso 0.193(7) 1 calc PR A 2 H20F H -0.1138 0.8318 0.2653 0.159 Uiso 0.193(7) 1 calc PR A 2 C21B C 0.001(2) 0.6876(9) 0.3556(17) 0.106(9) Uani 0.193(7) 1 d PD A 2 H21D H 0.0233 0.6444 0.3228 0.159 Uiso 0.193(7) 1 calc PR A 2 H21E H -0.0827 0.6954 0.3754 0.159 Uiso 0.193(7) 1 calc PR A 2 H21F H 0.0624 0.6524 0.3839 0.159 Uiso 0.193(7) 1 calc PR A 2 C22B C -0.021(3) 0.878(3) 0.3753(14) 0.106(9) Uani 0.193(7) 1 d PD A 2 H22D H 0.0486 0.8490 0.3992 0.159 Uiso 0.193(7) 1 calc PR A 2 H22E H -0.0999 0.8878 0.4012 0.159 Uiso 0.193(7) 1 calc PR A 2 H22F H -0.0263 0.9463 0.3534 0.159 Uiso 0.193(7) 1 calc PR A 2 C31 C 0.5370(3) 0.2452(3) 0.42081(14) 0.0235(8) Uani 1 1 d . . . C32 C 0.5707(3) 0.1683(3) 0.38209(14) 0.0235(8) Uani 1 1 d . . . C33 C 0.4971(3) 0.1108(3) 0.38351(15) 0.0269(8) Uani 1 1 d . . . H33 H 0.5224 0.0582 0.3572 0.032 Uiso 1 1 calc R . . C34 C 0.3889(3) 0.1285(3) 0.42218(14) 0.0257(8) Uani 1 1 d . B . C35 C 0.3540(3) 0.2123(3) 0.45712(15) 0.0282(8) Uani 1 1 d . . . H35 H 0.2776 0.2280 0.4828 0.034 Uiso 1 1 calc R . . C36 C 0.4203(3) 0.2735(3) 0.45743(15) 0.0278(8) Uani 1 1 d . . . C37 C 0.6757(3) 0.1562(3) 0.33850(14) 0.0238(8) Uani 1 1 d . . . H37 H 0.6886 0.1147 0.3075 0.029 Uiso 1 1 calc R . . C38 C 0.8498(3) 0.1917(3) 0.28833(14) 0.0225(8) Uani 1 1 d . . . C39 C 0.8159(3) 0.2226(3) 0.23214(14) 0.0230(8) Uani 1 1 d . . . H39 H 0.7298 0.2486 0.2269 0.028 Uiso 1 1 calc R . . C40 C 0.9046(3) 0.2170(2) 0.18237(14) 0.0205(8) Uani 1 1 d . . . C41 C 1.0291(3) 0.1775(3) 0.19259(15) 0.0250(8) Uani 1 1 d . . . H41 H 1.0922 0.1711 0.1598 0.030 Uiso 1 1 calc R . . C42 C 1.0641(3) 0.1473(3) 0.24921(16) 0.0322(9) Uani 1 1 d . . . H42 H 1.1501 0.1209 0.2546 0.039 Uiso 1 1 calc R . . C43 C 0.9743(3) 0.1551(3) 0.29802(15) 0.0287(8) Uani 1 1 d . . . H43 H 0.9974 0.1360 0.3370 0.034 Uiso 1 1 calc R . . C44 C 0.8336(4) 0.2081(3) 0.48596(16) 0.0402(10) Uani 1 1 d . . . H44A H 0.8464 0.2746 0.4803 0.060 Uiso 1 1 calc R . . H44B H 0.9026 0.1507 0.5053 0.060 Uiso 1 1 calc R . . H44C H 0.7539 0.2177 0.5109 0.060 Uiso 1 1 calc R . . C45 C 0.3690(3) 0.3680(3) 0.49349(16) 0.0349(9) Uani 1 1 d . . . C46 C 0.3564(4) 0.4699(3) 0.45169(18) 0.0462(11) Uani 1 1 d . . . H46A H 0.3229 0.5309 0.4746 0.069 Uiso 1 1 calc R . . H46B H 0.2993 0.4813 0.4229 0.069 Uiso 1 1 calc R . . H46C H 0.4390 0.4627 0.4307 0.069 Uiso 1 1 calc R . . C47 C 0.4569(4) 0.3511(4) 0.53898(18) 0.0500(11) Uani 1 1 d . . . H47A H 0.4634 0.2869 0.5664 0.075 Uiso 1 1 calc R . . H47B H 0.4233 0.4132 0.5612 0.075 Uiso 1 1 calc R . . H47C H 0.5402 0.3426 0.5185 0.075 Uiso 1 1 calc R . . C48 C 0.2396(4) 0.3852(4) 0.5275(2) 0.0554(13) Uani 1 1 d . . . H48A H 0.2450 0.3215 0.5552 0.083 Uiso 1 1 calc R . . H48B H 0.1802 0.3982 0.4996 0.083 Uiso 1 1 calc R . . H48C H 0.2106 0.4469 0.5496 0.083 Uiso 1 1 calc R . . C49 C 0.3067(3) 0.0668(2) 0.42924(12) 0.0341(9) Uani 1 1 d D . . C50A C 0.1717(3) 0.1434(3) 0.4182(2) 0.0369(14) Uani 0.805(6) 1 d PD B 1 H50A H 0.1375 0.1959 0.4468 0.055 Uiso 0.805(6) 1 calc PR B 1 H50B H 0.1194 0.1026 0.4228 0.055 Uiso 0.805(6) 1 calc PR B 1 H50C H 0.1724 0.1804 0.3779 0.055 Uiso 0.805(6) 1 calc PR B 1 C51A C 0.3011(5) 0.0132(4) 0.49342(14) 0.0355(14) Uani 0.805(6) 1 d PD B 1 H51A H 0.3858 -0.0358 0.5020 0.053 Uiso 0.805(6) 1 calc PR B 1 H51B H 0.2477 -0.0268 0.4984 0.053 Uiso 0.805(6) 1 calc PR B 1 H51C H 0.2660 0.0680 0.5207 0.053 Uiso 0.805(6) 1 calc PR B 1 C52A C 0.3566(5) -0.0195(4) 0.3868(2) 0.0417(15) Uani 0.805(6) 1 d PD B 1 H52A H 0.3586 0.0142 0.3458 0.063 Uiso 0.805(6) 1 calc PR B 1 H52B H 0.3014 -0.0580 0.3931 0.063 Uiso 0.805(6) 1 calc PR B 1 H52C H 0.4416 -0.0698 0.3945 0.063 Uiso 0.805(6) 1 calc PR B 1 C50B C 0.1872(17) 0.093(2) 0.4740(11) 0.084(7) Uani 0.195(6) 1 d PD B 2 H50D H 0.2105 0.0637 0.5140 0.126 Uiso 0.195(6) 1 calc PR B 2 H50E H 0.1342 0.0606 0.4643 0.126 Uiso 0.195(6) 1 calc PR B 2 H50F H 0.1409 0.1703 0.4722 0.126 Uiso 0.195(6) 1 calc PR B 2 C51B C 0.3990(17) -0.0499(6) 0.4423(12) 0.084(7) Uani 0.195(6) 1 d PD B 2 H51D H 0.4746 -0.0645 0.4135 0.126 Uiso 0.195(6) 1 calc PR B 2 H51E H 0.3592 -0.0979 0.4392 0.126 Uiso 0.195(6) 1 calc PR B 2 H51F H 0.4221 -0.0617 0.4823 0.126 Uiso 0.195(6) 1 calc PR B 2 C52B C 0.272(2) 0.078(2) 0.3667(4) 0.084(7) Uani 0.195(6) 1 d PD B 2 H52D H 0.2139 0.1512 0.3560 0.126 Uiso 0.195(6) 1 calc PR B 2 H52E H 0.2312 0.0290 0.3662 0.126 Uiso 0.195(6) 1 calc PR B 2 H52F H 0.3479 0.0594 0.3383 0.126 Uiso 0.195(6) 1 calc PR B 2 C61 C 0.6820(3) 0.2141(3) 0.09322(14) 0.0211(8) Uani 1 1 d . . . C62 C 0.6062(3) 0.3228(2) 0.08285(13) 0.0191(7) Uani 1 1 d . . . C63 C 0.4870(3) 0.3567(3) 0.06399(13) 0.0212(8) Uani 1 1 d . . . H63 H 0.4373 0.4309 0.0566 0.025 Uiso 1 1 calc R . . C64 C 0.4418(3) 0.2843(3) 0.05612(14) 0.0217(8) Uani 1 1 d . . . C65 C 0.5205(3) 0.1754(3) 0.06815(14) 0.0253(8) Uani 1 1 d . . . H65 H 0.4909 0.1242 0.0624 0.030 Uiso 1 1 calc R . . C66 C 0.6370(3) 0.1373(3) 0.08755(14) 0.0232(8) Uani 1 1 d . . . C67 C 0.6473(3) 0.3980(3) 0.09596(13) 0.0210(8) Uani 1 1 d . . . H67 H 0.5926 0.4714 0.0913 0.025 Uiso 1 1 calc R . . C68 C 0.7796(3) 0.4563(2) 0.13108(14) 0.0190(7) Uani 1 1 d . . . C69 C 0.6886(3) 0.5296(2) 0.16625(13) 0.0201(8) Uani 1 1 d . . . H69 H 0.6112 0.5224 0.1795 0.024 Uiso 1 1 calc R . . C70 C 0.7063(3) 0.6132(3) 0.18281(14) 0.0210(8) Uani 1 1 d . . . C71 C 0.8223(3) 0.6200(3) 0.16236(14) 0.0249(8) Uani 1 1 d . . . H71 H 0.8377 0.6768 0.1720 0.030 Uiso 1 1 calc R . . C72 C 0.9146(3) 0.5459(3) 0.12851(15) 0.0249(8) Uani 1 1 d . . . H72 H 0.9928 0.5517 0.1159 0.030 Uiso 1 1 calc R . . C73 C 0.8951(3) 0.4633(3) 0.11257(14) 0.0232(8) Uani 1 1 d . . . H73 H 0.9593 0.4122 0.0894 0.028 Uiso 1 1 calc R . . C74 C 0.9360(3) 0.2585(3) 0.01298(14) 0.0309(9) Uani 1 1 d . . . H74A H 0.9115 0.2030 0.0056 0.046 Uiso 1 1 calc R . . H74B H 1.0117 0.2560 -0.0137 0.046 Uiso 1 1 calc R . . H74C H 0.8678 0.3287 0.0059 0.046 Uiso 1 1 calc R . . C75 C 0.7118(3) 0.0172(3) 0.10418(16) 0.0313(9) Uani 1 1 d . . . C76 C 0.7401(4) -0.0034(3) 0.16808(16) 0.0396(10) Uani 1 1 d . . . H76A H 0.7800 -0.0805 0.1796 0.059 Uiso 1 1 calc R . . H76B H 0.6618 0.0272 0.1941 0.059 Uiso 1 1 calc R . . H76C H 0.7968 0.0299 0.1715 0.059 Uiso 1 1 calc R . . C77 C 0.8336(4) -0.0208(3) 0.06227(18) 0.0408(10) Uani 1 1 d . . . H77A H 0.8141 -0.0154 0.0221 0.061 Uiso 1 1 calc R . . H77B H 0.8853 -0.0952 0.0753 0.061 Uiso 1 1 calc R . . H77C H 0.8794 0.0239 0.0625 0.061 Uiso 1 1 calc R . . C78 C 0.6377(4) -0.0488(3) 0.0997(2) 0.0493(12) Uani 1 1 d . . . H78A H 0.6207 -0.0399 0.0587 0.074 Uiso 1 1 calc R . . H78B H 0.5582 -0.0244 0.1257 0.074 Uiso 1 1 calc R . . H78C H 0.6870 -0.1244 0.1118 0.074 Uiso 1 1 calc R . . C79 C 0.3131(3) 0.3146(3) 0.03675(15) 0.0266(8) Uani 1 1 d . . . C80 C 0.2370(3) 0.4340(3) 0.03175(16) 0.0303(9) Uani 1 1 d . . . H80A H 0.2241 0.4594 0.0703 0.045 Uiso 1 1 calc R . . H80B H 0.1555 0.4500 0.0193 0.045 Uiso 1 1 calc R . . H80C H 0.2821 0.4698 0.0025 0.045 Uiso 1 1 calc R . . C81 C 0.3324(4) 0.2763(3) -0.02363(17) 0.0406(10) Uani 1 1 d . . . H81A H 0.2507 0.2921 -0.0358 0.061 Uiso 1 1 calc R . . H81B H 0.3823 0.1991 -0.0210 0.061 Uiso 1 1 calc R . . H81C H 0.3766 0.3130 -0.0528 0.061 Uiso 1 1 calc R . . C82 C 0.2398(3) 0.2611(3) 0.08185(18) 0.0409(10) Uani 1 1 d . . . H82A H 0.2234 0.2891 0.1199 0.061 Uiso 1 1 calc R . . H82B H 0.2889 0.1838 0.0868 0.061 Uiso 1 1 calc R . . H82C H 0.1600 0.2760 0.0679 0.061 Uiso 1 1 calc R . . O91 O 0.4809(4) 0.3389(6) 0.2391(2) 0.137(2) Uani 1 1 d . . . C91 C 0.4133(6) 0.2826(6) 0.2290(3) 0.100(2) Uani 1 1 d . . . H91A H 0.4334 0.2145 0.2554 0.120 Uiso 1 1 calc R . . H91B H 0.4316 0.2670 0.1873 0.120 Uiso 1 1 calc R . . C92 C 0.2804(7) 0.3560(9) 0.2425(5) 0.190(5) Uani 1 1 d . . . H92A H 0.2431 0.3898 0.2052 0.228 Uiso 1 1 calc R . . H92B H 0.2322 0.3154 0.2657 0.228 Uiso 1 1 calc R . . C93 C 0.2738(7) 0.4338(10) 0.2744(5) 0.218(6) Uani 1 1 d . . . H93A H 0.2439 0.4199 0.3166 0.262 Uiso 1 1 calc R . . H93B H 0.2167 0.5054 0.2583 0.262 Uiso 1 1 calc R . . C94 C 0.4022(6) 0.4261(7) 0.2673(5) 0.150(4) Uani 1 1 d . . . H94A H 0.4071 0.4917 0.2440 0.180 Uiso 1 1 calc R . . H94B H 0.4284 0.4195 0.3067 0.180 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.023(2) 0.022(2) 0.027(2) -0.0019(17) -0.0032(17) -0.0082(18) B31 0.023(2) 0.031(2) 0.021(2) -0.0007(18) -0.0010(18) -0.0065(19) B61 0.020(2) 0.021(2) 0.027(2) -0.0097(17) 0.0055(17) -0.0076(18) N1 0.0169(16) 0.0231(16) 0.0239(15) -0.0055(12) 0.0014(13) -0.0053(13) N31 0.0180(15) 0.0203(16) 0.0208(15) -0.0021(12) -0.0016(12) -0.0020(13) N61 0.0160(15) 0.0204(15) 0.0171(14) -0.0034(11) -0.0001(12) -0.0066(12) O1 0.0185(13) 0.0256(13) 0.0250(13) -0.0031(10) 0.0002(10) -0.0049(11) O2 0.0273(13) 0.0236(13) 0.0292(13) -0.0094(11) 0.0035(11) -0.0093(11) O31 0.0284(14) 0.0280(14) 0.0241(13) -0.0053(10) 0.0031(11) -0.0108(12) O32 0.0340(14) 0.0315(14) 0.0237(13) 0.0001(11) -0.0084(11) -0.0096(12) O61 0.0174(13) 0.0196(12) 0.0301(13) -0.0039(10) -0.0064(10) -0.0051(10) O62 0.0210(13) 0.0256(13) 0.0218(13) -0.0080(10) 0.0023(10) -0.0062(10) C1 0.0191(19) 0.0181(18) 0.030(2) -0.0068(15) 0.0016(16) -0.0058(15) C2 0.0212(19) 0.0219(19) 0.027(2) -0.0037(15) -0.0032(16) -0.0046(16) C3 0.025(2) 0.029(2) 0.0260(19) -0.0047(16) 0.0008(16) -0.0067(17) C4 0.024(2) 0.025(2) 0.038(2) -0.0061(17) -0.0028(17) -0.0070(17) C5 0.0174(19) 0.028(2) 0.041(2) -0.0016(17) -0.0087(17) -0.0039(16) C6 0.0198(19) 0.026(2) 0.033(2) -0.0057(16) -0.0038(16) -0.0077(16) C7 0.031(2) 0.024(2) 0.0238(19) -0.0030(15) -0.0011(17) -0.0103(17) C8 0.0200(19) 0.027(2) 0.0193(18) -0.0029(15) -0.0018(14) -0.0069(16) C9 0.0192(19) 0.027(2) 0.0223(18) -0.0033(15) 0.0002(15) -0.0091(16) C10 0.0191(19) 0.030(2) 0.0188(18) -0.0036(15) -0.0007(15) -0.0071(16) C11 0.024(2) 0.028(2) 0.027(2) 0.0020(16) -0.0031(16) -0.0052(17) C12 0.0189(19) 0.040(2) 0.032(2) -0.0004(17) -0.0032(16) -0.0119(18) C13 0.028(2) 0.025(2) 0.0256(19) 0.0007(15) -0.0038(16) -0.0112(17) C14 0.039(2) 0.032(2) 0.042(2) -0.0171(19) 0.0067(19) -0.0132(19) C15 0.024(2) 0.047(2) 0.035(2) 0.0022(19) -0.0076(17) -0.0127(19) C16 0.041(3) 0.068(3) 0.033(2) -0.006(2) -0.0064(19) -0.025(2) C17 0.032(2) 0.049(3) 0.044(2) 0.019(2) -0.0100(19) -0.013(2) C18 0.033(2) 0.084(4) 0.035(2) 0.011(2) -0.0103(19) -0.018(2) C19 0.021(2) 0.035(2) 0.041(2) -0.0067(18) 0.0030(17) -0.0074(18) C20A 0.033(3) 0.051(4) 0.060(4) -0.008(3) 0.000(3) -0.024(3) C21A 0.023(3) 0.058(4) 0.043(3) 0.004(3) 0.005(2) -0.017(3) C22A 0.032(3) 0.032(3) 0.072(4) -0.007(3) 0.013(3) -0.006(2) C20B 0.034(10) 0.15(2) 0.126(19) -0.034(15) 0.025(10) -0.032(12) C21B 0.034(10) 0.15(2) 0.126(19) -0.034(15) 0.025(10) -0.032(12) C22B 0.034(10) 0.15(2) 0.126(19) -0.034(15) 0.025(10) -0.032(12) C31 0.0230(19) 0.0212(19) 0.0237(19) 0.0024(15) -0.0017(15) -0.0086(16) C32 0.0204(19) 0.0216(19) 0.0222(19) 0.0026(15) -0.0036(15) -0.0038(16) C33 0.027(2) 0.024(2) 0.0243(19) -0.0012(15) -0.0089(16) -0.0039(17) C34 0.0228(19) 0.024(2) 0.0238(19) 0.0017(15) -0.0056(16) -0.0038(16) C35 0.0224(19) 0.032(2) 0.0227(19) 0.0024(16) 0.0012(15) -0.0071(17) C36 0.026(2) 0.029(2) 0.0243(19) 0.0020(16) -0.0004(16) -0.0106(17) C37 0.0213(19) 0.0214(19) 0.0250(19) -0.0013(15) -0.0080(15) -0.0032(16) C38 0.0216(19) 0.0206(19) 0.0232(19) -0.0016(15) -0.0025(15) -0.0067(15) C39 0.0181(18) 0.0199(19) 0.029(2) -0.0036(15) -0.0046(16) -0.0044(15) C40 0.0162(18) 0.0151(18) 0.0283(19) -0.0063(14) -0.0024(15) -0.0031(14) C41 0.0193(19) 0.029(2) 0.0254(19) -0.0053(15) 0.0017(15) -0.0090(16) C42 0.0179(19) 0.040(2) 0.036(2) -0.0016(18) -0.0064(17) -0.0078(17) C43 0.024(2) 0.034(2) 0.0245(19) 0.0000(16) -0.0085(16) -0.0079(17) C44 0.044(2) 0.046(3) 0.031(2) -0.0018(19) -0.0105(19) -0.017(2) C45 0.034(2) 0.039(2) 0.032(2) -0.0137(18) 0.0127(17) -0.0181(19) C46 0.043(3) 0.035(2) 0.055(3) -0.018(2) 0.014(2) -0.012(2) C47 0.060(3) 0.057(3) 0.039(2) -0.021(2) 0.010(2) -0.029(2) C48 0.048(3) 0.055(3) 0.065(3) -0.034(2) 0.026(2) -0.025(2) C49 0.028(2) 0.038(2) 0.037(2) 0.0021(18) -0.0074(17) -0.0151(19) C50A 0.022(3) 0.045(3) 0.042(3) -0.008(2) -0.003(2) -0.012(2) C51A 0.042(3) 0.037(3) 0.033(3) 0.001(2) -0.002(2) -0.024(3) C52A 0.038(3) 0.042(3) 0.051(3) -0.016(3) 0.005(2) -0.022(3) C50B 0.071(12) 0.094(14) 0.119(16) -0.004(11) -0.007(11) -0.069(12) C51B 0.071(12) 0.094(14) 0.119(16) -0.004(11) -0.007(11) -0.069(12) C52B 0.071(12) 0.094(14) 0.119(16) -0.004(11) -0.007(11) -0.069(12) C61 0.0199(19) 0.026(2) 0.0175(17) -0.0054(14) 0.0015(14) -0.0090(16) C62 0.0174(18) 0.0194(19) 0.0199(18) -0.0032(14) -0.0018(14) -0.0067(15) C63 0.0185(18) 0.0195(18) 0.0192(18) -0.0019(14) 0.0027(14) -0.0034(15) C64 0.0217(19) 0.025(2) 0.0184(18) -0.0012(15) -0.0003(14) -0.0111(16) C65 0.029(2) 0.027(2) 0.0271(19) -0.0044(15) -0.0012(16) -0.0175(17) C66 0.0216(19) 0.0246(19) 0.0237(18) -0.0022(15) -0.0010(15) -0.0106(16) C67 0.0175(19) 0.0216(19) 0.0181(17) -0.0029(14) 0.0028(14) -0.0039(15) C68 0.0186(18) 0.0148(17) 0.0208(18) -0.0008(14) -0.0042(14) -0.0038(15) C69 0.0140(17) 0.0241(19) 0.0212(18) -0.0024(15) -0.0015(14) -0.0069(15) C70 0.0188(18) 0.0244(19) 0.0202(18) -0.0017(14) -0.0056(14) -0.0081(15) C71 0.024(2) 0.0238(19) 0.029(2) -0.0033(16) -0.0067(16) -0.0098(16) C72 0.0160(18) 0.029(2) 0.031(2) -0.0061(16) 0.0013(15) -0.0102(16) C73 0.0168(18) 0.025(2) 0.0243(19) -0.0070(15) 0.0008(15) -0.0040(15) C74 0.032(2) 0.032(2) 0.0198(19) -0.0062(16) 0.0035(16) -0.0056(17) C75 0.032(2) 0.0196(19) 0.043(2) -0.0016(16) -0.0120(18) -0.0080(17) C76 0.049(3) 0.031(2) 0.042(2) 0.0120(18) -0.021(2) -0.019(2) C77 0.040(2) 0.023(2) 0.053(3) -0.0098(18) -0.017(2) 0.0000(18) C78 0.057(3) 0.026(2) 0.070(3) 0.006(2) -0.032(2) -0.017(2) C79 0.026(2) 0.027(2) 0.029(2) -0.0021(16) -0.0055(16) -0.0118(17) C80 0.0181(19) 0.035(2) 0.036(2) -0.0028(17) -0.0043(16) -0.0087(17) C81 0.034(2) 0.042(2) 0.046(2) -0.0113(19) -0.0174(19) -0.0076(19) C82 0.028(2) 0.036(2) 0.057(3) 0.010(2) -0.0146(19) -0.0135(19) O91 0.062(3) 0.257(7) 0.114(4) -0.088(4) 0.010(3) -0.065(4) C91 0.102(5) 0.124(6) 0.059(4) -0.016(4) -0.009(4) -0.029(5) C92 0.074(5) 0.245(12) 0.282(13) -0.177(11) 0.033(7) -0.057(7) C93 0.080(6) 0.310(14) 0.321(15) -0.241(13) 0.022(7) -0.070(7) C94 0.070(5) 0.146(7) 0.260(11) -0.125(8) 0.017(6) -0.044(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 O2 1.416(4) . ? B1 O1 1.497(4) . ? B1 C70 1.606(5) . ? B1 N1 1.613(5) . ? B31 O32 1.437(4) . ? B31 O31 1.501(5) . ? B31 C10 1.610(5) . ? B31 N31 1.609(5) . ? B61 O62 1.416(4) . ? B61 O61 1.487(4) . ? B61 C40 1.601(5) . ? B61 N61 1.638(5) . ? N1 C7 1.293(4) . ? N1 C8 1.447(4) . ? N31 C37 1.291(4) . ? N31 C38 1.445(4) . ? N61 C67 1.296(4) . ? N61 C68 1.442(4) . ? O1 C1 1.330(4) . ? O2 C14 1.410(4) . ? O31 C31 1.332(4) . ? O32 C44 1.403(4) . ? O61 C61 1.325(4) . ? O62 C74 1.414(4) . ? C1 C2 1.400(5) . ? C1 C6 1.426(5) . ? C2 C3 1.410(5) . ? C2 C7 1.413(5) . ? C3 C4 1.368(5) . ? C4 C5 1.419(5) . ? C4 C19 1.516(5) . ? C5 C6 1.387(5) . ? C6 C15 1.530(5) . ? C8 C13 1.368(5) . ? C8 C9 1.373(5) . ? C9 C10 1.397(5) . ? C10 C11 1.387(5) . ? C11 C12 1.394(5) . ? C12 C13 1.388(5) . ? C15 C17 1.529(5) . ? C15 C18 1.532(5) . ? C15 C16 1.539(6) . ? C19 C22A 1.5390(10) . ? C19 C21A 1.5398(10) . ? C19 C21B 1.5399(11) . ? C19 C20B 1.5400(11) . ? C19 C22B 1.5401(10) . ? C19 C20A 1.5402(10) . ? C31 C32 1.399(5) . ? C31 C36 1.419(5) . ? C32 C33 1.398(5) . ? C32 C37 1.420(5) . ? C33 C34 1.376(5) . ? C34 C35 1.411(5) . ? C34 C49 1.514(5) . ? C35 C36 1.377(5) . ? C36 C45 1.525(5) . ? C38 C39 1.372(4) . ? C38 C43 1.389(5) . ? C39 C40 1.398(5) . ? C40 C41 1.389(4) . ? C41 C42 1.385(5) . ? C42 C43 1.386(5) . ? C45 C47 1.533(5) . ? C45 C48 1.529(5) . ? C45 C46 1.531(5) . ? C49 C52A 1.5382(10) . ? C49 C50B 1.5397(10) . ? C49 C52B 1.5405(10) . ? C49 C51A 1.5402(10) . ? C49 C50A 1.5404(10) . ? C49 C51B 1.5404(10) . ? C61 C62 1.398(4) . ? C61 C66 1.409(5) . ? C62 C63 1.412(4) . ? C62 C67 1.417(4) . ? C63 C64 1.370(4) . ? C64 C65 1.412(5) . ? C64 C79 1.529(5) . ? C65 C66 1.382(5) . ? C66 C75 1.538(5) . ? C68 C69 1.384(4) . ? C68 C73 1.392(4) . ? C69 C70 1.390(4) . ? C70 C71 1.403(4) . ? C71 C72 1.378(5) . ? C72 C73 1.380(5) . ? C75 C76 1.526(5) . ? C75 C77 1.526(5) . ? C75 C78 1.535(5) . ? C79 C80 1.514(5) . ? C79 C82 1.523(5) . ? C79 C81 1.528(5) . ? O91 C94 1.370(8) . ? O91 C91 1.401(8) . ? C91 C92 1.482(9) . ? C92 C93 1.382(10) . ? C93 C94 1.456(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 B1 O1 113.8(3) . . ? O2 B1 C70 110.8(3) . . ? O1 B1 C70 108.6(3) . . ? O2 B1 N1 109.5(3) . . ? O1 B1 N1 105.2(3) . . ? C70 B1 N1 108.7(3) . . ? O32 B31 O31 112.8(3) . . ? O32 B31 C10 118.2(3) . . ? O31 B31 C10 106.2(3) . . ? O32 B31 N31 103.9(3) . . ? O31 B31 N31 106.0(3) . . ? C10 B31 N31 109.1(3) . . ? O62 B61 O61 112.1(3) . . ? O62 B61 C40 112.5(3) . . ? O61 B61 C40 108.1(3) . . ? O62 B61 N61 109.7(3) . . ? O61 B61 N61 105.7(3) . . ? C40 B61 N61 108.5(3) . . ? C7 N1 C8 118.1(3) . . ? C7 N1 B1 120.8(3) . . ? C8 N1 B1 121.0(3) . . ? C37 N31 C38 119.5(3) . . ? C37 N31 B31 120.1(3) . . ? C38 N31 B31 120.3(3) . . ? C67 N61 C68 118.1(3) . . ? C67 N61 B61 121.5(3) . . ? C68 N61 B61 120.4(2) . . ? C1 O1 B1 126.0(3) . . ? C14 O2 B1 118.4(3) . . ? C31 O31 B31 124.4(3) . . ? C44 O32 B31 117.8(3) . . ? C61 O61 B61 128.1(3) . . ? C74 O62 B61 118.1(3) . . ? O1 C1 C2 120.1(3) . . ? O1 C1 C6 120.2(3) . . ? C2 C1 C6 119.6(3) . . ? C1 C2 C3 121.1(3) . . ? C1 C2 C7 118.2(3) . . ? C3 C2 C7 120.2(3) . . ? C4 C3 C2 121.4(3) . . ? C3 C4 C5 115.9(3) . . ? C3 C4 C19 123.5(3) . . ? C5 C4 C19 120.5(3) . . ? C6 C5 C4 126.0(3) . . ? C5 C6 C1 115.9(3) . . ? C5 C6 C15 122.5(3) . . ? C1 C6 C15 121.6(3) . . ? N1 C7 C2 123.9(3) . . ? C13 C8 C9 120.4(3) . . ? C13 C8 N1 121.1(3) . . ? C9 C8 N1 118.4(3) . . ? C8 C9 C10 122.2(3) . . ? C11 C10 C9 116.7(3) . . ? C11 C10 B31 125.6(3) . . ? C9 C10 B31 117.5(3) . . ? C10 C11 C12 121.3(3) . . ? C13 C12 C11 120.1(3) . . ? C8 C13 C12 119.2(3) . . ? C17 C15 C6 111.1(3) . . ? C17 C15 C18 107.7(3) . . ? C6 C15 C18 111.7(3) . . ? C17 C15 C16 109.9(3) . . ? C6 C15 C16 108.9(3) . . ? C18 C15 C16 107.5(3) . . ? C4 C19 C22A 110.8(3) . . ? C4 C19 C21A 113.0(3) . . ? C22A C19 C21A 108.6(4) . . ? C4 C19 C21B 108.4(10) . . ? C22A C19 C21B 140.7(11) . . ? C21A C19 C21B 51.8(15) . . ? C4 C19 C20B 114.0(11) . . ? C22A C19 C20B 49.3(15) . . ? C21A C19 C20B 132.9(11) . . ? C21B C19 C20B 114.5(19) . . ? C4 C19 C22B 103.1(10) . . ? C22A C19 C22B 48.9(15) . . ? C21A C19 C22B 68.1(16) . . ? C21B C19 C22B 119(2) . . ? C20B C19 C22B 97(2) . . ? C4 C19 C20A 110.3(3) . . ? C22A C19 C20A 107.4(4) . . ? C21A C19 C20A 106.5(3) . . ? C21B C19 C20A 59.6(15) . . ? C20B C19 C20A 60.1(16) . . ? C22B C19 C20A 145.0(11) . . ? O31 C31 C32 120.0(3) . . ? O31 C31 C36 120.2(3) . . ? C32 C31 C36 119.7(3) . . ? C33 C32 C31 120.7(3) . . ? C33 C32 C37 120.9(3) . . ? C31 C32 C37 118.2(3) . . ? C34 C33 C32 121.5(3) . . ? C33 C34 C35 115.6(3) . . ? C33 C34 C49 125.5(3) . . ? C35 C34 C49 118.9(3) . . ? C36 C35 C34 126.1(3) . . ? C35 C36 C31 115.9(3) . . ? C35 C36 C45 121.8(3) . . ? C31 C36 C45 122.3(3) . . ? N31 C37 C32 123.9(3) . . ? C39 C38 C43 121.0(3) . . ? C39 C38 N31 119.8(3) . . ? C43 C38 N31 119.2(3) . . ? C38 C39 C40 121.8(3) . . ? C41 C40 C39 116.7(3) . . ? C41 C40 B61 123.7(3) . . ? C39 C40 B61 119.5(3) . . ? C42 C41 C40 122.0(3) . . ? C41 C42 C43 120.4(3) . . ? C42 C43 C38 118.2(3) . . ? C36 C45 C47 110.6(3) . . ? C36 C45 C48 112.7(3) . . ? C47 C45 C48 107.3(3) . . ? C36 C45 C46 109.2(3) . . ? C47 C45 C46 109.4(3) . . ? C48 C45 C46 107.6(3) . . ? C34 C49 C52A 112.1(3) . . ? C34 C49 C50B 121.5(10) . . ? C52A C49 C50B 126.4(10) . . ? C34 C49 C52B 104.8(9) . . ? C52A C49 C52B 52.5(9) . . ? C50B C49 C52B 109.3(15) . . ? C34 C49 C51A 108.9(3) . . ? C52A C49 C51A 109.0(3) . . ? C50B C49 C51A 55.1(12) . . ? C52B C49 C51A 146.1(9) . . ? C34 C49 C50A 110.2(3) . . ? C52A C49 C50A 109.1(3) . . ? C50B C49 C50A 52.4(12) . . ? C52B C49 C50A 63.4(10) . . ? C51A C49 C50A 107.4(3) . . ? C34 C49 C51B 103.1(9) . . ? C52A C49 C51B 53.8(9) . . ? C50B C49 C51B 110.8(15) . . ? C52B C49 C51B 106.3(6) . . ? C51A C49 C51B 62.2(10) . . ? C50A C49 C51B 146.6(9) . . ? O61 C61 C62 120.5(3) . . ? O61 C61 C66 119.6(3) . . ? C62 C61 C66 119.9(3) . . ? C61 C62 C63 120.7(3) . . ? C61 C62 C67 118.6(3) . . ? C63 C62 C67 120.5(3) . . ? C64 C63 C62 121.0(3) . . ? C63 C64 C65 116.4(3) . . ? C63 C64 C79 124.2(3) . . ? C65 C64 C79 119.4(3) . . ? C66 C65 C64 125.3(3) . . ? C65 C66 C61 116.6(3) . . ? C65 C66 C75 121.7(3) . . ? C61 C66 C75 121.7(3) . . ? N61 C67 C62 124.0(3) . . ? C69 C68 C73 119.8(3) . . ? C69 C68 N61 120.0(3) . . ? C73 C68 N61 120.2(3) . . ? C68 C69 C70 122.4(3) . . ? C69 C70 C71 116.6(3) . . ? C69 C70 B1 120.4(3) . . ? C71 C70 B1 123.0(3) . . ? C72 C71 C70 121.3(3) . . ? C73 C72 C71 121.1(3) . . ? C72 C73 C68 118.7(3) . . ? C76 C75 C77 110.3(3) . . ? C76 C75 C78 107.1(3) . . ? C77 C75 C78 108.3(3) . . ? C76 C75 C66 110.0(3) . . ? C77 C75 C66 109.3(3) . . ? C78 C75 C66 111.7(3) . . ? C80 C79 C82 108.2(3) . . ? C80 C79 C81 108.8(3) . . ? C82 C79 C81 109.8(3) . . ? C80 C79 C64 112.0(3) . . ? C82 C79 C64 109.5(3) . . ? C81 C79 C64 108.5(3) . . ? C94 O91 C91 109.9(5) . . ? O91 C91 C92 103.7(6) . . ? C93 C92 C91 109.7(7) . . ? C92 C93 C94 104.3(7) . . ? O91 C94 C93 109.8(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 B1 N1 C7 98.6(3) . . . . ? O1 B1 N1 C7 -24.1(4) . . . . ? C70 B1 N1 C7 -140.3(3) . . . . ? O2 B1 N1 C8 -82.7(4) . . . . ? O1 B1 N1 C8 154.6(3) . . . . ? C70 B1 N1 C8 38.4(4) . . . . ? O32 B31 N31 C37 95.2(3) . . . . ? O31 B31 N31 C37 -23.9(4) . . . . ? C10 B31 N31 C37 -137.9(3) . . . . ? O32 B31 N31 C38 -86.9(3) . . . . ? O31 B31 N31 C38 154.0(3) . . . . ? C10 B31 N31 C38 40.0(4) . . . . ? O62 B61 N61 C67 108.2(3) . . . . ? O61 B61 N61 C67 -12.8(4) . . . . ? C40 B61 N61 C67 -128.6(3) . . . . ? O62 B61 N61 C68 -72.2(4) . . . . ? O61 B61 N61 C68 166.8(2) . . . . ? C40 B61 N61 C68 51.0(4) . . . . ? O2 B1 O1 C1 -93.8(4) . . . . ? C70 B1 O1 C1 142.2(3) . . . . ? N1 B1 O1 C1 26.0(4) . . . . ? O1 B1 O2 C14 56.3(4) . . . . ? C70 B1 O2 C14 179.1(3) . . . . ? N1 B1 O2 C14 -61.1(4) . . . . ? O32 B31 O31 C31 -83.0(4) . . . . ? C10 B31 O31 C31 146.0(3) . . . . ? N31 B31 O31 C31 30.0(4) . . . . ? O31 B31 O32 C44 -59.2(4) . . . . ? C10 B31 O32 C44 65.5(4) . . . . ? N31 B31 O32 C44 -173.5(3) . . . . ? O62 B61 O61 C61 -106.0(3) . . . . ? C40 B61 O61 C61 129.5(3) . . . . ? N61 B61 O61 C61 13.5(4) . . . . ? O61 B61 O62 C74 52.4(4) . . . . ? C40 B61 O62 C74 174.5(3) . . . . ? N61 B61 O62 C74 -64.6(3) . . . . ? B1 O1 C1 C2 -13.2(5) . . . . ? B1 O1 C1 C6 170.3(3) . . . . ? O1 C1 C2 C3 -178.3(3) . . . . ? C6 C1 C2 C3 -1.7(5) . . . . ? O1 C1 C2 C7 -5.9(5) . . . . ? C6 C1 C2 C7 170.7(3) . . . . ? C1 C2 C3 C4 0.3(5) . . . . ? C7 C2 C3 C4 -172.0(3) . . . . ? C2 C3 C4 C5 0.1(5) . . . . ? C2 C3 C4 C19 176.7(3) . . . . ? C3 C4 C5 C6 1.0(5) . . . . ? C19 C4 C5 C6 -175.6(3) . . . . ? C4 C5 C6 C1 -2.4(5) . . . . ? C4 C5 C6 C15 176.2(3) . . . . ? O1 C1 C6 C5 179.1(3) . . . . ? C2 C1 C6 C5 2.6(5) . . . . ? O1 C1 C6 C15 0.6(5) . . . . ? C2 C1 C6 C15 -175.9(3) . . . . ? C8 N1 C7 C2 -168.4(3) . . . . ? B1 N1 C7 C2 10.3(5) . . . . ? C1 C2 C7 N1 6.5(5) . . . . ? C3 C2 C7 N1 178.9(3) . . . . ? C7 N1 C8 C13 -139.6(3) . . . . ? B1 N1 C8 C13 41.7(4) . . . . ? C7 N1 C8 C9 42.2(4) . . . . ? B1 N1 C8 C9 -136.5(3) . . . . ? C13 C8 C9 C10 2.0(5) . . . . ? N1 C8 C9 C10 -179.8(3) . . . . ? C8 C9 C10 C11 -2.0(5) . . . . ? C8 C9 C10 B31 -177.2(3) . . . . ? O32 B31 C10 C11 17.8(5) . . . . ? O31 B31 C10 C11 145.7(3) . . . . ? N31 B31 C10 C11 -100.5(4) . . . . ? O32 B31 C10 C9 -167.5(3) . . . . ? O31 B31 C10 C9 -39.7(4) . . . . ? N31 B31 C10 C9 74.2(4) . . . . ? C9 C10 C11 C12 0.9(5) . . . . ? B31 C10 C11 C12 175.6(3) . . . . ? C10 C11 C12 C13 0.3(5) . . . . ? C9 C8 C13 C12 -0.7(5) . . . . ? N1 C8 C13 C12 -178.9(3) . . . . ? C11 C12 C13 C8 -0.4(5) . . . . ? C5 C6 C15 C17 123.4(4) . . . . ? C1 C6 C15 C17 -58.2(4) . . . . ? C5 C6 C15 C18 3.1(5) . . . . ? C1 C6 C15 C18 -178.4(3) . . . . ? C5 C6 C15 C16 -115.4(4) . . . . ? C1 C6 C15 C16 63.0(4) . . . . ? C3 C4 C19 C22A 120.2(4) . . . . ? C5 C4 C19 C22A -63.5(5) . . . . ? C3 C4 C19 C21A -2.0(5) . . . . ? C5 C4 C19 C21A 174.4(4) . . . . ? C3 C4 C19 C21B -57.5(16) . . . . ? C5 C4 C19 C21B 118.9(16) . . . . ? C3 C4 C19 C20B 173.7(18) . . . . ? C5 C4 C19 C20B -10.0(18) . . . . ? C3 C4 C19 C22B 69.5(17) . . . . ? C5 C4 C19 C22B -114.1(17) . . . . ? C3 C4 C19 C20A -121.0(4) . . . . ? C5 C4 C19 C20A 55.4(4) . . . . ? B31 O31 C31 C32 -16.5(5) . . . . ? B31 O31 C31 C36 168.0(3) . . . . ? O31 C31 C32 C33 177.5(3) . . . . ? C36 C31 C32 C33 -6.9(5) . . . . ? O31 C31 C32 C37 -7.2(5) . . . . ? C36 C31 C32 C37 168.4(3) . . . . ? C31 C32 C33 C34 0.9(5) . . . . ? C37 C32 C33 C34 -174.3(3) . . . . ? C32 C33 C34 C35 3.8(5) . . . . ? C32 C33 C34 C49 -176.7(3) . . . . ? C33 C34 C35 C36 -2.8(5) . . . . ? C49 C34 C35 C36 177.7(3) . . . . ? C34 C35 C36 C31 -2.9(5) . . . . ? C34 C35 C36 C45 175.2(3) . . . . ? O31 C31 C36 C35 -176.8(3) . . . . ? C32 C31 C36 C35 7.7(5) . . . . ? O31 C31 C36 C45 5.1(5) . . . . ? C32 C31 C36 C45 -170.5(3) . . . . ? C38 N31 C37 C32 -172.6(3) . . . . ? B31 N31 C37 C32 5.3(5) . . . . ? C33 C32 C37 N31 -172.5(3) . . . . ? C31 C32 C37 N31 12.2(5) . . . . ? C37 N31 C38 C39 50.9(4) . . . . ? B31 N31 C38 C39 -127.0(3) . . . . ? C37 N31 C38 C43 -129.6(3) . . . . ? B31 N31 C38 C43 52.4(4) . . . . ? C43 C38 C39 C40 1.1(5) . . . . ? N31 C38 C39 C40 -179.4(3) . . . . ? C38 C39 C40 C41 0.6(5) . . . . ? C38 C39 C40 B61 177.5(3) . . . . ? O62 B61 C40 C41 -4.2(5) . . . . ? O61 B61 C40 C41 120.1(3) . . . . ? N61 B61 C40 C41 -125.7(3) . . . . ? O62 B61 C40 C39 179.1(3) . . . . ? O61 B61 C40 C39 -56.6(4) . . . . ? N61 B61 C40 C39 57.6(4) . . . . ? C39 C40 C41 C42 -1.3(5) . . . . ? B61 C40 C41 C42 -178.1(3) . . . . ? C40 C41 C42 C43 0.3(5) . . . . ? C41 C42 C43 C38 1.4(5) . . . . ? C39 C38 C43 C42 -2.1(5) . . . . ? N31 C38 C43 C42 178.5(3) . . . . ? C35 C36 C45 C47 119.9(4) . . . . ? C31 C36 C45 C47 -62.1(4) . . . . ? C35 C36 C45 C48 -0.2(5) . . . . ? C31 C36 C45 C48 177.8(3) . . . . ? C35 C36 C45 C46 -119.7(4) . . . . ? C31 C36 C45 C46 58.3(4) . . . . ? C33 C34 C49 C52A -0.9(5) . . . . ? C35 C34 C49 C52A 178.5(3) . . . . ? C33 C34 C49 C50B 179.9(15) . . . . ? C35 C34 C49 C50B -0.7(15) . . . . ? C33 C34 C49 C52B -56.0(11) . . . . ? C35 C34 C49 C52B 123.5(10) . . . . ? C33 C34 C49 C51A 119.8(4) . . . . ? C35 C34 C49 C51A -60.8(4) . . . . ? C33 C34 C49 C50A -122.6(4) . . . . ? C35 C34 C49 C50A 56.8(4) . . . . ? C33 C34 C49 C51B 55.0(11) . . . . ? C35 C34 C49 C51B -125.5(10) . . . . ? B61 O61 C61 C62 -6.0(5) . . . . ? B61 O61 C61 C66 177.3(3) . . . . ? O61 C61 C62 C63 -179.7(3) . . . . ? C66 C61 C62 C63 -3.0(5) . . . . ? O61 C61 C62 C67 -4.4(5) . . . . ? C66 C61 C62 C67 172.3(3) . . . . ? C61 C62 C63 C64 0.9(5) . . . . ? C67 C62 C63 C64 -174.3(3) . . . . ? C62 C63 C64 C65 0.3(5) . . . . ? C62 C63 C64 C79 179.0(3) . . . . ? C63 C64 C65 C66 0.7(5) . . . . ? C79 C64 C65 C66 -178.1(3) . . . . ? C64 C65 C66 C61 -2.8(5) . . . . ? C64 C65 C66 C75 175.1(3) . . . . ? O61 C61 C66 C65 -179.5(3) . . . . ? C62 C61 C66 C65 3.8(5) . . . . ? O61 C61 C66 C75 2.6(5) . . . . ? C62 C61 C66 C75 -174.1(3) . . . . ? C68 N61 C67 C62 -174.2(3) . . . . ? B61 N61 C67 C62 5.5(5) . . . . ? C61 C62 C67 N61 4.1(5) . . . . ? C63 C62 C67 N61 179.4(3) . . . . ? C67 N61 C68 C69 44.6(4) . . . . ? B61 N61 C68 C69 -135.1(3) . . . . ? C67 N61 C68 C73 -135.7(3) . . . . ? B61 N61 C68 C73 44.6(4) . . . . ? C73 C68 C69 C70 2.0(5) . . . . ? N61 C68 C69 C70 -178.3(3) . . . . ? C68 C69 C70 C71 -0.4(5) . . . . ? C68 C69 C70 B1 -178.8(3) . . . . ? O2 B1 C70 C69 -176.3(3) . . . . ? O1 B1 C70 C69 -50.6(4) . . . . ? N1 B1 C70 C69 63.4(4) . . . . ? O2 B1 C70 C71 5.4(4) . . . . ? O1 B1 C70 C71 131.1(3) . . . . ? N1 B1 C70 C71 -114.9(3) . . . . ? C69 C70 C71 C72 -1.2(5) . . . . ? B1 C70 C71 C72 177.2(3) . . . . ? C70 C71 C72 C73 1.2(5) . . . . ? C71 C72 C73 C68 0.4(5) . . . . ? C69 C68 C73 C72 -1.9(5) . . . . ? N61 C68 C73 C72 178.4(3) . . . . ? C65 C66 C75 C76 -122.0(3) . . . . ? C61 C66 C75 C76 55.8(4) . . . . ? C65 C66 C75 C77 116.7(4) . . . . ? C61 C66 C75 C77 -65.5(4) . . . . ? C65 C66 C75 C78 -3.2(5) . . . . ? C61 C66 C75 C78 174.6(3) . . . . ? C63 C64 C79 C80 -4.4(5) . . . . ? C65 C64 C79 C80 174.3(3) . . . . ? C63 C64 C79 C82 -124.4(4) . . . . ? C65 C64 C79 C82 54.3(4) . . . . ? C63 C64 C79 C81 115.8(4) . . . . ? C65 C64 C79 C81 -65.5(4) . . . . ? C94 O91 C91 C92 11.5(9) . . . . ? O91 C91 C92 C93 -16.5(12) . . . . ? C91 C92 C93 C94 14.6(15) . . . . ? C91 O91 C94 C93 -3.1(12) . . . . ? C92 C93 C94 O91 -7.4(14) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.566 _refine_diff_density_min -0.337 _refine_diff_density_rms 0.052 data_complex_1b _database_code_depnum_ccdc_archive 'CCDC 230231' _audit_creation_method SHELXL-97 #------------------------------------------------------------- #Chemical and physical data _chemical_name_systematic ; Trimethoxy-[tris-[mu-(3-phenyl-kC)imine-kN]methyl-2-(3,5-di-tert- butyl)phenolate-kO)triboro' ; _chemical_name_common ; Trimethoxy-(tris-(mu-(3-phenyl-kC)imine-kN)methyl-2-(3,5-di- tert-butyl)phenolate-kO)triboro' ; _chemical_melting_point '310 C' _chemical_formula_moiety ? _chemical_formula_sum 'C69 H90 B3 N3 O8' _chemical_formula_weight 1121.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7903(18) _cell_length_b 13.840(2) _cell_length_c 23.415(4) _cell_angle_alpha 79.863(3) _cell_angle_beta 79.457(3) _cell_angle_gamma 65.716(3) _cell_volume 3402.3(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max .32 _exptl_crystal_size_mid .24 _exptl_crystal_size_min .22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.095 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 0.070 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13387 _diffrn_reflns_av_R_equivalents 0.0812 _diffrn_reflns_av_sigmaI/netI 0.2010 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 22.50 _reflns_number_total 8502 _reflns_number_gt 4534 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.1016P)^2^+6.2144P] 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 8502 _refine_ls_number_parameters 692 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.2059 _refine_ls_R_factor_gt 0.1286 _refine_ls_wR_factor_ref 0.3146 _refine_ls_wR_factor_gt 0.2706 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 1.2949(5) 0.1849(4) 0.1119(2) 0.0179(14) Uani 1 1 d . . . O2 O 0.9794(5) 0.7372(5) 0.2000(2) 0.0217(15) Uani 1 1 d . . . O3 O 1.1097(5) 0.3016(4) 0.4179(2) 0.0192(15) Uani 1 1 d . . . O5 O 1.1359(5) 0.7820(5) 0.2316(3) 0.0251(16) Uani 1 1 d . . . O4 O 1.4614(5) 0.2450(5) 0.0742(2) 0.0169(14) Uani 1 1 d . . . N2 N 1.0788(6) 0.6355(6) 0.2873(3) 0.0191(18) Uani 1 1 d . . . N3 N 1.2558(6) 0.2014(5) 0.3375(3) 0.0147(17) Uani 1 1 d . . . O6 O 1.3295(5) 0.1877(5) 0.4282(2) 0.0222(15) Uani 1 1 d . . . N1 N 1.2576(6) 0.3744(6) 0.1146(3) 0.0162(18) Uani 1 1 d . . . C1 C 1.1823(8) 0.2168(8) 0.0936(4) 0.0231(8) Uani 1 1 d . . . C8 C 1.2798(8) 0.4594(8) 0.1315(4) 0.0231(8) Uani 1 1 d . . . C2 C 0.9896(7) 0.3574(7) 0.0638(4) 0.020(2) Uani 1 1 d . . . H2 H 0.9406 0.4299 0.0573 0.024 Uiso 1 1 calc R . . C27 C 1.0724(8) 0.1681(7) 0.3819(4) 0.019(2) Uani 1 1 d . . . C14 C 0.8548(7) 0.7240(7) 0.2916(4) 0.018(2) Uani 1 1 d . . . C3 C 1.0250(8) 0.1764(7) 0.0652(4) 0.021(2) Uani 1 1 d . . . H3 H 0.9966 0.1265 0.0581 0.025 Uiso 1 1 calc R . . C9 C 1.2085(7) 0.6167(7) 0.1830(4) 0.014(2) Uani 1 1 d . . . C10 C 1.3952(7) 0.4680(7) 0.1126(4) 0.017(2) Uani 1 1 d . . . H10 H 1.4575 0.4184 0.0899 0.020 Uiso 1 1 calc R . . C28 C 1.0398(8) 0.2457(7) 0.4200(4) 0.016(2) Uani 1 1 d . . . C34 C 1.4047(8) 0.2200(7) 0.1833(4) 0.0231(8) Uani 1 1 d . . . C7 C 1.1498(8) 0.3997(7) 0.0971(4) 0.021(2) Uani 1 1 d . . . H7 H 1.0960 0.4713 0.0933 0.025 Uiso 1 1 calc R . . C4 C 0.9466(8) 0.2849(8) 0.0545(4) 0.022(2) Uani 1 1 d . . . C29 C 0.8915(8) 0.1263(8) 0.4223(4) 0.0231(8) Uani 1 1 d . . . C15 C 0.8663(8) 0.7591(7) 0.2307(4) 0.019(2) Uani 1 1 d . . . C40 C 1.2186(8) 0.0184(7) 0.0986(4) 0.025(2) Uani 1 1 d . . . C5 C 1.1095(8) 0.3230(8) 0.0833(4) 0.0231(8) Uani 1 1 d . . . C30 C 1.0006(8) 0.1081(7) 0.3848(4) 0.028(2) Uani 1 1 d . . . H30 H 1.0274 0.0542 0.3607 0.033 Uiso 1 1 calc R . . C20 C 0.9672(8) 0.6568(7) 0.3158(4) 0.025(2) Uani 1 1 d . . . H20 H 0.9605 0.6263 0.3543 0.030 Uiso 1 1 calc R . . C21 C 1.1844(7) 0.5509(7) 0.3138(4) 0.014(2) Uani 1 1 d . . . C59 C 0.8119(8) 0.0616(7) 0.4295(4) 0.018(2) Uani 1 1 d . . . C46 C 0.8185(7) 0.3148(7) 0.0340(4) 0.020(2) Uani 1 1 d . . . C31 C 0.9213(8) 0.2739(7) 0.4555(4) 0.024(2) Uani 1 1 d . . . C33 C 1.1789(8) 0.1557(7) 0.3380(4) 0.0231(8) Uani 1 1 d . . . H33 H 1.1932 0.1132 0.3087 0.028 Uiso 1 1 calc R . . C16 C 0.7554(8) 0.8142(7) 0.2037(4) 0.027(2) Uani 1 1 d . . . C35 C 1.3165(8) 0.2239(7) 0.2320(4) 0.021(2) Uani 1 1 d . . . H35 H 1.2329 0.2457 0.2267 0.025 Uiso 1 1 calc R . . C36 C 1.5623(8) 0.1599(7) 0.2491(4) 0.0231(8) Uani 1 1 d . . . H36 H 1.6456 0.1393 0.2545 0.028 Uiso 1 1 calc R . . B1 B 1.3630(9) 0.2500(9) 0.1194(5) 0.0212(19) Uani 1 1 d . . . C11 C 1.1899(8) 0.5334(7) 0.1669(4) 0.0231(8) Uani 1 1 d . . . H11 H 1.1141 0.5263 0.1804 0.028 Uiso 1 1 calc R . . C37 C 1.3491(7) 0.1967(7) 0.2875(4) 0.013(2) Uani 1 1 d . . . C22 C 1.2662(7) 0.3721(7) 0.3653(4) 0.014(2) Uani 1 1 d . . . C23 C 1.1708(8) 0.4570(7) 0.3383(4) 0.017(2) Uani 1 1 d . . . H23 H 1.0962 0.4502 0.3367 0.020 Uiso 1 1 calc R . . C38 C 1.4734(8) 0.1641(7) 0.2972(4) 0.027(2) Uani 1 1 d . . . H38 H 1.4959 0.1458 0.3349 0.033 Uiso 1 1 calc R . . C6 C 1.1413(8) 0.1375(7) 0.0854(4) 0.019(2) Uani 1 1 d . . . C24 C 1.2941(8) 0.5650(7) 0.3134(4) 0.018(2) Uani 1 1 d . . . H24 H 1.3022 0.6286 0.2974 0.021 Uiso 1 1 calc R . . C32 C 0.8565(8) 0.2104(7) 0.4558(4) 0.024(2) Uani 1 1 d . . . H32 H 0.7820 0.2251 0.4809 0.029 Uiso 1 1 calc R . . C12 C 1.3226(8) 0.6253(7) 0.1623(4) 0.018(2) Uani 1 1 d . . . H12 H 1.3370 0.6816 0.1715 0.022 Uiso 1 1 calc R . . C13 C 1.4163(7) 0.5509(7) 0.1280(3) 0.016(2) Uani 1 1 d . . . H13 H 1.4928 0.5571 0.1155 0.019 Uiso 1 1 calc R . . C25 C 1.3766(8) 0.3881(7) 0.3640(4) 0.023(2) Uani 1 1 d . . . H25 H 1.4426 0.3340 0.3815 0.027 Uiso 1 1 calc R . . C48 C 1.4400(8) 0.2591(7) 0.0161(4) 0.028(2) Uani 1 1 d . . . H48A H 1.4104 0.2071 0.0101 0.042 Uiso 1 1 calc R . . H48B H 1.5167 0.2506 -0.0091 0.042 Uiso 1 1 calc R . . H48C H 1.3781 0.3294 0.0073 0.042 Uiso 1 1 calc R . . C17 C 0.6443(9) 0.8302(8) 0.2406(4) 0.033(3) Uani 1 1 d . . . H17 H 0.5708 0.8692 0.2236 0.039 Uiso 1 1 calc R . . C18 C 0.6296(8) 0.7953(8) 0.2994(4) 0.025(2) Uani 1 1 d . . . C19 C 0.7395(8) 0.7412(7) 0.3245(4) 0.024(2) Uani 1 1 d . . . H19 H 0.7359 0.7160 0.3640 0.028 Uiso 1 1 calc R . . C63 C 1.3329(9) 0.2153(8) 0.4830(4) 0.032(3) Uani 1 1 d . . . H63A H 1.3295 0.2867 0.4784 0.048 Uiso 1 1 calc R . . H63B H 1.4091 0.1668 0.4982 0.048 Uiso 1 1 calc R . . H63C H 1.2623 0.2111 0.5096 0.048 Uiso 1 1 calc R . . C26 C 1.3919(7) 0.4795(7) 0.3381(4) 0.019(2) Uani 1 1 d . . . H26 H 1.4685 0.4846 0.3370 0.023 Uiso 1 1 calc R . . C39 C 1.5291(7) 0.1857(7) 0.1932(4) 0.021(2) Uani 1 1 d . . . H39 H 1.5910 0.1801 0.1615 0.025 Uiso 1 1 calc R . . C55 C 0.8538(9) 0.4725(8) 0.4495(5) 0.043(3) Uani 1 1 d . . . H55A H 0.8191 0.5329 0.4714 0.064 Uiso 1 1 calc R . . H55B H 0.7987 0.4813 0.4217 0.064 Uiso 1 1 calc R . . H55C H 0.9343 0.4672 0.4292 0.064 Uiso 1 1 calc R . . C44 C 0.7415(7) 0.4352(7) 0.0315(4) 0.025(2) Uani 1 1 d . . . H44A H 0.7282 0.4573 0.0696 0.037 Uiso 1 1 calc R . . H44B H 0.6620 0.4517 0.0187 0.037 Uiso 1 1 calc R . . H44C H 0.7860 0.4722 0.0045 0.037 Uiso 1 1 calc R . . C43 C 1.2448(9) -0.0056(7) 0.1633(4) 0.034(3) Uani 1 1 d . . . H43A H 1.2951 0.0309 0.1689 0.051 Uiso 1 1 calc R . . H43B H 1.2887 -0.0810 0.1726 0.051 Uiso 1 1 calc R . . H43C H 1.1668 0.0186 0.1884 0.051 Uiso 1 1 calc R . . C41 C 1.3424(8) -0.0155(8) 0.0583(4) 0.036(3) Uani 1 1 d . . . H41A H 1.3266 -0.0126 0.0191 0.054 Uiso 1 1 calc R . . H41B H 1.3957 -0.0871 0.0715 0.054 Uiso 1 1 calc R . . H41C H 1.3830 0.0317 0.0590 0.054 Uiso 1 1 calc R . . C45 C 0.8391(9) 0.2786(8) -0.0264(4) 0.039(3) Uani 1 1 d . . . H45A H 0.8838 0.3150 -0.0538 0.058 Uiso 1 1 calc R . . H45B H 0.7595 0.2950 -0.0390 0.058 Uiso 1 1 calc R . . H45C H 0.8871 0.2031 -0.0245 0.058 Uiso 1 1 calc R . . C47 C 0.7453(8) 0.2582(8) 0.0785(4) 0.032(3) Uani 1 1 d . . . H47A H 0.7918 0.1825 0.0807 0.048 Uiso 1 1 calc R . . H47B H 0.6652 0.2757 0.0662 0.048 Uiso 1 1 calc R . . H47C H 0.7334 0.2814 0.1162 0.048 Uiso 1 1 calc R . . B2 B 1.1012(9) 0.6997(8) 0.2240(5) 0.019(3) Uani 1 1 d . . . C56 C 0.7395(9) 0.3845(8) 0.5244(5) 0.044(3) Uani 1 1 d . . . H56A H 0.7090 0.4446 0.5463 0.067 Uiso 1 1 calc R . . H56B H 0.7461 0.3213 0.5507 0.067 Uiso 1 1 calc R . . H56C H 0.6823 0.3961 0.4971 0.067 Uiso 1 1 calc R . . C49 C 0.7594(9) 0.8492(9) 0.1383(4) 0.041(3) Uani 1 1 d . . . C57 C 0.9573(9) 0.3565(9) 0.5348(4) 0.042(3) Uani 1 1 d . . . H57A H 1.0333 0.3614 0.5141 0.062 Uiso 1 1 calc R . . H57B H 0.9764 0.2879 0.5572 0.062 Uiso 1 1 calc R . . H57C H 0.9179 0.4113 0.5605 0.062 Uiso 1 1 calc R . . C60 C 0.8059(10) 0.0086(9) 0.4928(4) 0.044(3) Uani 1 1 d . . . H60A H 0.7599 -0.0361 0.4969 0.066 Uiso 1 1 calc R . . H60B H 0.7647 0.0626 0.5189 0.066 Uiso 1 1 calc R . . H60C H 0.8894 -0.0339 0.5022 0.066 Uiso 1 1 calc R . . B3 B 1.2437(9) 0.2648(9) 0.3908(5) 0.0212(19) Uani 1 1 d . . . C54 C 1.0540(9) 0.8613(8) 0.2661(4) 0.033(3) Uani 1 1 d . . . H54A H 0.9754 0.8963 0.2504 0.050 Uiso 1 1 calc R . . H54B H 1.0896 0.9124 0.2663 0.050 Uiso 1 1 calc R . . H54C H 1.0407 0.8297 0.3053 0.050 Uiso 1 1 calc R . . C53 C 0.5011(9) 0.8137(8) 0.3351(5) 0.036(3) Uani 1 1 d . . . C58 C 0.8687(9) 0.3709(9) 0.4912(4) 0.034(3) Uani 1 1 d . . . C61 C 0.6766(8) 0.1364(9) 0.4184(5) 0.046(3) Uani 1 1 d . . . H61A H 0.6779 0.1767 0.3806 0.069 Uiso 1 1 calc R . . H61B H 0.6398 0.1843 0.4479 0.069 Uiso 1 1 calc R . . H61C H 0.6279 0.0947 0.4197 0.069 Uiso 1 1 calc R . . C50 C 0.8280(9) 0.9218(9) 0.1205(5) 0.052(3) Uani 1 1 d . . . H50A H 0.7886 0.9823 0.1423 0.078 Uiso 1 1 calc R . . H50B H 0.8261 0.9456 0.0795 0.078 Uiso 1 1 calc R . . H50C H 0.9135 0.8841 0.1283 0.078 Uiso 1 1 calc R . . C62 C 0.8614(10) -0.0236(9) 0.3896(5) 0.053(3) Uani 1 1 d . . . H62A H 0.8559 0.0084 0.3499 0.079 Uiso 1 1 calc R . . H62B H 0.8129 -0.0668 0.3988 0.079 Uiso 1 1 calc R . . H62C H 0.9475 -0.0674 0.3946 0.079 Uiso 1 1 calc R . . C51 C 0.8281(9) 0.7488(10) 0.1055(4) 0.052(4) Uani 1 1 d . . . H51A H 0.9093 0.7089 0.1182 0.078 Uiso 1 1 calc R . . H51B H 0.8374 0.7702 0.0642 0.078 Uiso 1 1 calc R . . H51C H 0.7801 0.7052 0.1138 0.078 Uiso 1 1 calc R . . C42 C 1.1486(10) -0.0493(8) 0.0911(6) 0.056(4) Uani 1 1 d . . . H42A H 1.0742 -0.0336 0.1188 0.084 Uiso 1 1 calc R . . H42B H 1.2016 -0.1235 0.0977 0.084 Uiso 1 1 calc R . . H42C H 1.1259 -0.0333 0.0522 0.084 Uiso 1 1 calc R . . C52 C 0.6291(9) 0.9051(10) 0.1194(5) 0.058(4) Uani 1 1 d . . . H52A H 0.5865 0.8573 0.1285 0.087 Uiso 1 1 calc R . . H52B H 0.6358 0.9265 0.0781 0.087 Uiso 1 1 calc R . . H52C H 0.5827 0.9670 0.1398 0.087 Uiso 1 1 calc R . . C71 C 0.5032(12) 0.7307(12) 0.3815(8) 0.159(11) Uani 1 1 d . . . H71A H 0.4260 0.7539 0.4072 0.239 Uiso 1 1 calc R . . H71B H 0.5721 0.7143 0.4029 0.239 Uiso 1 1 calc R . . H71C H 0.5129 0.6681 0.3654 0.239 Uiso 1 1 calc R . . C72 C 0.4755(8) 0.9059(7) 0.3738(4) 0.0231(8) Uani 1 1 d . . . H72A H 0.3925 0.9261 0.3946 0.035 Uiso 1 1 calc R . . H72B H 0.4829 0.9666 0.3489 0.035 Uiso 1 1 calc R . . H72C H 0.5357 0.8808 0.4012 0.035 Uiso 1 1 calc R . . C73 C 0.4037(13) 0.852(3) 0.3019(8) 0.31(2) Uani 1 1 d . . . H73A H 0.3269 0.8891 0.3254 0.463 Uiso 1 1 calc R . . H73B H 0.3976 0.7935 0.2877 0.463 Uiso 1 1 calc R . . H73C H 0.4187 0.9000 0.2694 0.463 Uiso 1 1 calc R . . C83 C 0.8992(14) 0.2233(13) 0.2320(7) 0.115(6) Uiso 1 1 d D . . H83A H 0.9578 0.2335 0.1997 0.173 Uiso 1 1 calc R . . H83B H 0.8617 0.1796 0.2221 0.173 Uiso 1 1 calc R . . H83C H 0.9422 0.1888 0.2657 0.173 Uiso 1 1 calc R . . C81 C 0.8054(17) 0.4220(11) 0.2405(17) 0.37(2) Uiso 1 1 d D . . O7 O 0.8960(18) 0.4293(17) 0.2526(12) 0.334(13) Uiso 1 1 d D . . O8 O 0.8023(18) 0.3259(11) 0.2448(11) 0.342(13) Uiso 1 1 d D . . C82 C 0.6950(17) 0.5240(12) 0.2283(12) 0.248(14) Uiso 1 1 d D . . H82A H 0.6682 0.5633 0.2616 0.372 Uiso 1 1 calc R . . H82B H 0.6276 0.5081 0.2207 0.372 Uiso 1 1 calc R . . H82C H 0.7186 0.5660 0.1948 0.372 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 O1 0.016(3) 0.016(4) 0.024(4) -0.002(3) -0.008(3) -0.006(3) O2 0.017(3) 0.027(4) 0.018(4) 0.000(3) 0.001(3) -0.008(3) O3 0.018(3) 0.016(4) 0.020(4) 0.001(3) -0.004(3) -0.003(3) O5 0.025(4) 0.022(4) 0.027(4) -0.013(3) 0.009(3) -0.009(3) O4 0.013(3) 0.023(4) 0.009(3) -0.006(3) 0.001(3) -0.001(3) N2 0.017(4) 0.016(5) 0.021(4) -0.001(4) 0.000(4) -0.004(4) N3 0.015(4) 0.011(4) 0.013(4) -0.002(3) -0.004(3) 0.001(4) O6 0.022(3) 0.025(4) 0.017(4) 0.000(3) -0.009(3) -0.004(3) N1 0.012(4) 0.023(5) 0.014(4) -0.013(4) 0.010(3) -0.008(4) C1 0.0171(17) 0.030(2) 0.0161(18) -0.0006(15) -0.0040(13) -0.0035(16) C8 0.0171(17) 0.030(2) 0.0161(18) -0.0006(15) -0.0040(13) -0.0035(16) C2 0.012(5) 0.016(6) 0.025(6) 0.004(4) -0.008(4) 0.000(5) C27 0.017(5) 0.027(6) 0.009(5) -0.002(4) -0.001(4) -0.006(5) C14 0.011(5) 0.024(6) 0.020(6) -0.001(4) -0.007(4) -0.005(5) C3 0.026(5) 0.024(6) 0.015(5) -0.001(5) -0.005(4) -0.013(5) C9 0.015(5) 0.010(5) 0.018(5) -0.001(4) -0.008(4) -0.004(4) C10 0.006(4) 0.017(6) 0.018(5) -0.009(4) 0.004(4) 0.004(4) C28 0.015(5) 0.006(5) 0.017(5) 0.000(4) -0.001(4) 0.003(4) C34 0.0171(17) 0.030(2) 0.0161(18) -0.0006(15) -0.0040(13) -0.0035(16) C7 0.021(5) 0.026(6) 0.019(5) -0.013(5) 0.007(4) -0.014(5) C4 0.023(5) 0.036(7) 0.017(5) -0.005(5) -0.004(4) -0.020(6) C29 0.0171(17) 0.030(2) 0.0161(18) -0.0006(15) -0.0040(13) -0.0035(16) C15 0.021(6) 0.003(5) 0.030(6) -0.002(4) 0.002(5) -0.004(5) C40 0.028(6) 0.016(6) 0.025(6) -0.006(5) -0.014(5) 0.002(5) C5 0.0171(17) 0.030(2) 0.0161(18) -0.0006(15) -0.0040(13) -0.0035(16) C30 0.039(6) 0.017(6) 0.023(6) -0.002(5) 0.001(5) -0.008(5) C20 0.024(6) 0.022(6) 0.026(6) -0.009(5) 0.007(5) -0.008(5) C21 0.010(5) 0.011(5) 0.014(5) -0.004(4) -0.002(4) 0.003(4) C59 0.016(5) 0.021(6) 0.024(6) -0.006(5) -0.011(4) -0.008(5) C46 0.011(5) 0.015(6) 0.030(6) -0.010(5) 0.003(4) -0.001(5) C31 0.024(5) 0.025(6) 0.023(6) -0.011(5) 0.007(4) -0.010(5) C33 0.0171(17) 0.030(2) 0.0161(18) -0.0006(15) -0.0040(13) -0.0035(16) C16 0.015(5) 0.014(6) 0.040(7) 0.001(5) 0.000(5) 0.003(5) C35 0.019(5) 0.017(6) 0.029(6) -0.010(5) 0.003(4) -0.008(5) C36 0.0171(17) 0.030(2) 0.0161(18) -0.0006(15) -0.0040(13) -0.0035(16) B1 0.009(4) 0.024(5) 0.028(5) -0.005(4) -0.009(3) -0.001(4) C11 0.0171(17) 0.030(2) 0.0161(18) -0.0006(15) -0.0040(13) -0.0035(16) C37 0.007(4) 0.016(5) 0.010(5) -0.007(4) 0.000(4) 0.005(4) C22 0.007(4) 0.017(5) 0.011(5) -0.009(4) -0.005(4) 0.007(4) C23 0.010(5) 0.023(6) 0.016(5) -0.005(4) 0.001(4) -0.005(5) C38 0.023(5) 0.031(6) 0.022(6) 0.008(5) -0.012(4) -0.005(5) C6 0.015(5) 0.008(5) 0.027(6) -0.004(4) -0.009(4) 0.005(4) C24 0.021(5) 0.019(6) 0.014(5) -0.002(4) -0.006(4) -0.007(5) C32 0.017(5) 0.033(6) 0.016(5) 0.002(5) -0.002(4) -0.005(5) C12 0.023(5) 0.020(6) 0.020(5) -0.003(4) -0.014(4) -0.011(5) C13 0.011(5) 0.019(6) 0.017(5) -0.011(4) 0.000(4) -0.003(5) C25 0.022(5) 0.018(6) 0.022(6) 0.000(5) -0.005(4) -0.002(5) C48 0.025(5) 0.016(6) 0.027(6) -0.010(5) 0.007(5) 0.005(5) C17 0.026(6) 0.039(7) 0.031(7) 0.007(5) -0.008(5) -0.013(6) C18 0.010(5) 0.030(6) 0.032(6) -0.012(5) 0.000(4) -0.003(5) C19 0.020(5) 0.019(6) 0.025(6) -0.010(5) 0.004(4) -0.001(5) C63 0.034(6) 0.032(7) 0.034(7) 0.003(5) -0.018(5) -0.013(6) C26 0.007(5) 0.031(6) 0.020(5) -0.002(5) 0.000(4) -0.007(5) C39 0.015(5) 0.039(6) 0.009(5) -0.008(5) 0.006(4) -0.013(5) C55 0.028(6) 0.021(6) 0.071(8) -0.020(6) 0.017(6) -0.005(5) C44 0.010(5) 0.034(7) 0.027(6) -0.002(5) -0.013(4) -0.002(5) C43 0.039(6) 0.016(6) 0.044(7) -0.001(5) -0.011(5) -0.005(5) C41 0.026(6) 0.027(7) 0.042(7) -0.012(5) -0.013(5) 0.010(5) C45 0.027(6) 0.038(7) 0.055(8) -0.013(6) -0.020(5) -0.008(6) C47 0.020(5) 0.037(7) 0.041(7) 0.003(5) -0.006(5) -0.015(5) B2 0.017(6) 0.012(6) 0.031(7) -0.010(5) 0.004(5) -0.008(5) C56 0.047(7) 0.037(7) 0.055(8) -0.033(6) 0.019(6) -0.023(6) C49 0.020(6) 0.066(9) 0.031(7) 0.012(6) -0.016(5) -0.014(6) C57 0.042(7) 0.049(8) 0.037(7) -0.022(6) 0.011(5) -0.022(6) C60 0.066(8) 0.061(8) 0.025(6) -0.011(6) 0.001(6) -0.044(7) B3 0.009(4) 0.024(5) 0.028(5) -0.005(4) -0.009(3) -0.001(4) C54 0.039(6) 0.034(7) 0.041(7) -0.015(6) 0.004(5) -0.027(6) C53 0.021(6) 0.030(7) 0.043(7) -0.009(6) 0.011(5) 0.000(5) C58 0.040(6) 0.055(8) 0.024(6) -0.016(6) 0.014(5) -0.037(6) C61 0.028(6) 0.049(8) 0.059(8) 0.003(6) -0.013(6) -0.013(6) C50 0.036(7) 0.064(9) 0.043(8) 0.024(7) -0.027(6) -0.010(7) C62 0.054(7) 0.070(9) 0.054(8) -0.029(7) 0.013(6) -0.044(7) C51 0.024(6) 0.107(11) 0.027(6) -0.015(7) -0.013(5) -0.022(7) C42 0.057(8) 0.019(7) 0.101(11) 0.000(7) -0.037(7) -0.016(6) C52 0.022(6) 0.115(12) 0.032(7) 0.021(7) -0.021(5) -0.024(7) C71 0.038(8) 0.091(13) 0.25(2) 0.101(14) 0.049(11) -0.006(9) C72 0.0171(17) 0.030(2) 0.0161(18) -0.0006(15) -0.0040(13) -0.0035(16) C73 0.030(9) 0.74(6) 0.069(13) 0.07(2) 0.005(9) -0.12(2) _geom_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. 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. Cell parameters were determined by least squares refinements on diffractometer angles for 24 automatically centered reflections collected on three sets of 20 frames each. Non-hydrogen atoms were refined anisotropically, except C81, C82, C83, O7 and O8 atoms, (for solvent molecule) which were refined only isotropically. Hydrogen atoms were placed in geometrically calculated positionsusing a riding model. For the disordered groups, DFIX and EADP instructions have been used. The thermal parameters of the atoms C5, C29,C33, C72,C82 and B3 werefied using EADP intruction. ; 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 C1 1.342(10) . ? O1 B1 1.480(11) . ? O2 C15 1.333(9) . ? O2 B2 1.494(11) . ? O3 C28 1.332(9) . ? O3 B3 1.497(11) . ? O5 C54 1.394(10) . ? O5 B2 1.405(11) . ? O4 C48 1.395(10) . ? O4 B1 1.408(11) . ? N2 C20 1.301(10) . ? N2 C21 1.460(10) . ? N2 B2 1.626(12) . ? N3 C33 1.299(10) . ? N3 C37 1.444(10) . ? N3 B3 1.601(12) . ? O6 C63 1.413(10) . ? O6 B3 1.427(12) . ? N1 C7 1.296(10) . ? N1 C8 1.436(11) . ? N1 B1 1.656(13) . ? C1 C5 1.367(12) . ? C1 C6 1.422(12) . ? C8 C11 1.395(12) . ? C8 C10 1.399(11) . ? C2 C4 1.358(12) . ? C2 C5 1.429(11) . ? C27 C30 1.396(12) . ? C27 C28 1.404(11) . ? C27 C33 1.440(11) . ? C14 C19 1.383(11) . ? C14 C20 1.421(12) . ? C14 C15 1.423(12) . ? C3 C6 1.391(12) . ? C3 C4 1.409(12) . ? C9 C11 1.382(12) . ? C9 C12 1.390(10) . ? C9 B2 1.610(12) . ? C10 C13 1.385(11) . ? C28 C31 1.427(11) . ? C34 C35 1.387(11) . ? C34 C39 1.395(11) . ? C34 B1 1.591(13) . ? C7 C5 1.432(12) . ? C4 C46 1.538(12) . ? C29 C30 1.374(12) . ? C29 C32 1.395(12) . ? C29 C59 1.515(11) . ? C15 C16 1.415(12) . ? C40 C41 1.526(12) . ? C40 C6 1.527(12) . ? C40 C42 1.528(12) . ? C40 C43 1.554(12) . ? C21 C24 1.383(11) . ? C21 C23 1.385(11) . ? C59 C62 1.491(13) . ? C59 C60 1.538(12) . ? C59 C61 1.543(12) . ? C46 C45 1.527(12) . ? C46 C44 1.532(12) . ? C46 C47 1.544(11) . ? C31 C32 1.380(12) . ? C31 C58 1.551(12) . ? C16 C17 1.387(12) . ? C16 C49 1.520(13) . ? C35 C37 1.367(11) . ? C36 C39 1.377(11) . ? C36 C38 1.382(11) . ? C37 C38 1.395(11) . ? C22 C23 1.399(11) . ? C22 C25 1.401(11) . ? C22 B3 1.609(13) . ? C24 C26 1.395(11) . ? C12 C13 1.399(11) . ? C25 C26 1.371(12) . ? C17 C18 1.381(13) . ? C18 C19 1.383(12) . ? C18 C53 1.534(12) . ? C55 C58 1.529(13) . ? C56 C58 1.531(12) . ? C49 C50 1.496(14) . ? C49 C52 1.518(12) . ? C49 C51 1.549(15) . ? C57 C58 1.524(13) . ? C53 C73 1.373(18) . ? C53 C71 1.431(15) . ? C53 C72 1.590(13) . ? C83 O8 1.4503(11) . ? C81 O7 1.2003(11) . ? C81 O8 1.3303(11) . ? C81 C82 1.5003(11) . ? 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 O1 B1 129.0(7) . . ? C15 O2 B2 126.6(7) . . ? C28 O3 B3 122.6(7) . . ? C54 O5 B2 119.2(7) . . ? C48 O4 B1 119.7(7) . . ? C20 N2 C21 117.9(7) . . ? C20 N2 B2 121.6(8) . . ? C21 N2 B2 120.6(6) . . ? C33 N3 C37 118.8(7) . . ? C33 N3 B3 120.2(7) . . ? C37 N3 B3 121.0(7) . . ? C63 O6 B3 118.4(7) . . ? C7 N1 C8 116.5(7) . . ? C7 N1 B1 122.0(7) . . ? C8 N1 B1 121.4(7) . . ? O1 C1 C5 120.5(8) . . ? O1 C1 C6 118.3(8) . . ? C5 C1 C6 121.2(8) . . ? C11 C8 C10 118.6(8) . . ? C11 C8 N1 121.9(7) . . ? C10 C8 N1 119.5(8) . . ? C4 C2 C5 120.4(9) . . ? C30 C27 C28 121.0(8) . . ? C30 C27 C33 121.1(8) . . ? C28 C27 C33 117.9(8) . . ? C19 C14 C20 120.3(8) . . ? C19 C14 C15 122.1(8) . . ? C20 C14 C15 117.0(8) . . ? C6 C3 C4 125.4(8) . . ? C11 C9 C12 117.3(8) . . ? C11 C9 B2 120.7(7) . . ? C12 C9 B2 122.0(7) . . ? C13 C10 C8 119.6(8) . . ? O3 C28 C27 121.0(7) . . ? O3 C28 C31 120.1(8) . . ? C27 C28 C31 118.3(8) . . ? C35 C34 C39 117.1(8) . . ? C35 C34 B1 120.2(8) . . ? C39 C34 B1 122.7(8) . . ? N1 C7 C5 123.3(9) . . ? C2 C4 C3 117.1(8) . . ? C2 C4 C46 123.9(9) . . ? C3 C4 C46 119.0(8) . . ? C30 C29 C32 115.3(9) . . ? C30 C29 C59 124.7(9) . . ? C32 C29 C59 120.0(7) . . ? O2 C15 C16 121.4(8) . . ? O2 C15 C14 120.3(8) . . ? C16 C15 C14 118.3(8) . . ? C41 C40 C6 110.6(8) . . ? C41 C40 C42 108.5(8) . . ? C6 C40 C42 111.9(8) . . ? C41 C40 C43 109.7(8) . . ? C6 C40 C43 109.1(7) . . ? C42 C40 C43 107.0(8) . . ? C1 C5 C2 120.7(9) . . ? C1 C5 C7 119.1(8) . . ? C2 C5 C7 119.9(9) . . ? C29 C30 C27 122.0(9) . . ? N2 C20 C14 123.9(9) . . ? C24 C21 C23 121.9(8) . . ? C24 C21 N2 120.4(7) . . ? C23 C21 N2 117.7(7) . . ? C62 C59 C29 113.0(7) . . ? C62 C59 C60 108.3(8) . . ? C29 C59 C60 109.3(7) . . ? C62 C59 C61 109.3(8) . . ? C29 C59 C61 109.5(8) . . ? C60 C59 C61 107.3(8) . . ? C45 C46 C44 109.9(8) . . ? C45 C46 C4 109.1(7) . . ? C44 C46 C4 111.1(7) . . ? C45 C46 C47 110.4(7) . . ? C44 C46 C47 108.0(7) . . ? C4 C46 C47 108.4(8) . . ? C32 C31 C28 116.2(8) . . ? C32 C31 C58 122.2(7) . . ? C28 C31 C58 121.6(8) . . ? N3 C33 C27 122.9(9) . . ? C17 C16 C15 115.5(9) . . ? C17 C16 C49 122.8(9) . . ? C15 C16 C49 121.7(8) . . ? C37 C35 C34 121.8(8) . . ? C39 C36 C38 120.9(8) . . ? O4 B1 O1 112.6(8) . . ? O4 B1 C34 114.1(7) . . ? O1 B1 C34 109.6(8) . . ? O4 B1 N1 107.1(7) . . ? O1 B1 N1 104.7(6) . . ? C34 B1 N1 108.2(7) . . ? C9 C11 C8 122.9(8) . . ? C35 C37 C38 120.8(8) . . ? C35 C37 N3 120.9(7) . . ? C38 C37 N3 118.3(8) . . ? C23 C22 C25 115.1(8) . . ? C23 C22 B3 118.4(7) . . ? C25 C22 B3 126.3(8) . . ? C21 C23 C22 121.9(8) . . ? C36 C38 C37 118.0(9) . . ? C3 C6 C1 115.1(8) . . ? C3 C6 C40 122.5(8) . . ? C1 C6 C40 122.4(8) . . ? C21 C24 C26 117.0(8) . . ? C31 C32 C29 126.6(8) . . ? C9 C12 C13 121.4(7) . . ? C10 C13 C12 120.1(7) . . ? C26 C25 C22 123.2(9) . . ? C18 C17 C16 127.8(9) . . ? C17 C18 C19 115.4(8) . . ? C17 C18 C53 123.1(9) . . ? C19 C18 C53 121.5(9) . . ? C18 C19 C14 120.8(9) . . ? C25 C26 C24 120.8(8) . . ? C36 C39 C34 121.4(8) . . ? O5 B2 O2 114.4(8) . . ? O5 B2 C9 111.3(7) . . ? O2 B2 C9 108.8(7) . . ? O5 B2 N2 109.5(7) . . ? O2 B2 N2 103.9(6) . . ? C9 B2 N2 108.6(7) . . ? C50 C49 C52 109.1(9) . . ? C50 C49 C16 110.8(9) . . ? C52 C49 C16 112.1(8) . . ? C50 C49 C51 109.1(9) . . ? C52 C49 C51 107.1(9) . . ? C16 C49 C51 108.6(9) . . ? O6 B3 O3 113.7(8) . . ? O6 B3 N3 103.9(8) . . ? O3 B3 N3 106.9(7) . . ? O6 B3 C22 117.6(7) . . ? O3 B3 C22 105.3(7) . . ? N3 B3 C22 109.0(7) . . ? C73 C53 C71 117.5(15) . . ? C73 C53 C18 114.0(10) . . ? C71 C53 C18 113.6(9) . . ? C73 C53 C72 105.6(15) . . ? C71 C53 C72 98.4(11) . . ? C18 C53 C72 105.3(8) . . ? C57 C58 C55 109.4(8) . . ? C57 C58 C56 108.9(8) . . ? C55 C58 C56 107.8(9) . . ? C57 C58 C31 110.4(8) . . ? C55 C58 C31 109.4(7) . . ? C56 C58 C31 111.0(7) . . ? O7 C81 O8 119.1(8) . . ? O7 C81 C82 117.1(7) . . ? O8 C81 C82 123.4(7) . . ? C81 O8 C83 132(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag B1 O1 C1 C5 -5.2(13) . . . . ? B1 O1 C1 C6 174.9(8) . . . . ? C7 N1 C8 C11 45.3(12) . . . . ? B1 N1 C8 C11 -132.9(8) . . . . ? C7 N1 C8 C10 -135.6(8) . . . . ? B1 N1 C8 C10 46.1(11) . . . . ? C11 C8 C10 C13 -1.9(13) . . . . ? N1 C8 C10 C13 179.0(8) . . . . ? B3 O3 C28 C27 -20.2(12) . . . . ? B3 O3 C28 C31 168.3(8) . . . . ? C30 C27 C28 O3 178.7(8) . . . . ? C33 C27 C28 O3 -4.1(13) . . . . ? C30 C27 C28 C31 -9.7(13) . . . . ? C33 C27 C28 C31 167.5(8) . . . . ? C8 N1 C7 C5 -174.9(8) . . . . ? B1 N1 C7 C5 3.3(12) . . . . ? C5 C2 C4 C3 0.1(13) . . . . ? C5 C2 C4 C46 179.5(8) . . . . ? C6 C3 C4 C2 1.3(14) . . . . ? C6 C3 C4 C46 -178.1(8) . . . . ? B2 O2 C15 C16 167.0(8) . . . . ? B2 O2 C15 C14 -15.2(12) . . . . ? C19 C14 C15 O2 -177.2(8) . . . . ? C20 C14 C15 O2 -6.1(12) . . . . ? C19 C14 C15 C16 0.7(13) . . . . ? C20 C14 C15 C16 171.8(8) . . . . ? O1 C1 C5 C2 179.9(8) . . . . ? C6 C1 C5 C2 -0.1(14) . . . . ? O1 C1 C5 C7 -5.4(13) . . . . ? C6 C1 C5 C7 174.6(8) . . . . ? C4 C2 C5 C1 -0.7(13) . . . . ? C4 C2 C5 C7 -175.3(8) . . . . ? N1 C7 C5 C1 5.8(13) . . . . ? N1 C7 C5 C2 -179.5(8) . . . . ? C32 C29 C30 C27 1.6(13) . . . . ? C59 C29 C30 C27 -177.4(8) . . . . ? C28 C27 C30 C29 3.9(14) . . . . ? C33 C27 C30 C29 -173.2(9) . . . . ? C21 N2 C20 C14 -169.4(8) . . . . ? B2 N2 C20 C14 10.3(13) . . . . ? C19 C14 C20 N2 178.8(9) . . . . ? C15 C14 C20 N2 7.5(13) . . . . ? C20 N2 C21 C24 -136.2(8) . . . . ? B2 N2 C21 C24 44.2(11) . . . . ? C20 N2 C21 C23 44.6(11) . . . . ? B2 N2 C21 C23 -135.1(8) . . . . ? C30 C29 C59 C62 -2.0(13) . . . . ? C32 C29 C59 C62 178.9(9) . . . . ? C30 C29 C59 C60 118.6(10) . . . . ? C32 C29 C59 C60 -60.5(11) . . . . ? C30 C29 C59 C61 -124.1(10) . . . . ? C32 C29 C59 C61 56.9(11) . . . . ? C2 C4 C46 C45 115.5(10) . . . . ? C3 C4 C46 C45 -65.1(11) . . . . ? C2 C4 C46 C44 -5.8(12) . . . . ? C3 C4 C46 C44 173.6(8) . . . . ? C2 C4 C46 C47 -124.3(9) . . . . ? C3 C4 C46 C47 55.1(10) . . . . ? O3 C28 C31 C32 -178.8(8) . . . . ? C27 C28 C31 C32 9.6(13) . . . . ? O3 C28 C31 C58 1.7(13) . . . . ? C27 C28 C31 C58 -170.0(8) . . . . ? C37 N3 C33 C27 -171.4(8) . . . . ? B3 N3 C33 C27 6.7(13) . . . . ? C30 C27 C33 N3 -172.5(8) . . . . ? C28 C27 C33 N3 10.3(13) . . . . ? O2 C15 C16 C17 179.0(8) . . . . ? C14 C15 C16 C17 1.1(13) . . . . ? O2 C15 C16 C49 1.2(14) . . . . ? C14 C15 C16 C49 -176.7(9) . . . . ? C39 C34 C35 C37 0.7(14) . . . . ? B1 C34 C35 C37 178.7(8) . . . . ? C48 O4 B1 O1 47.9(11) . . . . ? C48 O4 B1 C34 173.7(7) . . . . ? C48 O4 B1 N1 -66.6(9) . . . . ? C1 O1 B1 O4 -103.8(10) . . . . ? C1 O1 B1 C34 128.1(8) . . . . ? C1 O1 B1 N1 12.3(11) . . . . ? C35 C34 B1 O4 178.5(8) . . . . ? C39 C34 B1 O4 -3.6(14) . . . . ? C35 C34 B1 O1 -54.2(11) . . . . ? C39 C34 B1 O1 123.7(9) . . . . ? C35 C34 B1 N1 59.4(10) . . . . ? C39 C34 B1 N1 -122.7(9) . . . . ? C7 N1 B1 O4 108.8(8) . . . . ? C8 N1 B1 O4 -73.1(9) . . . . ? C7 N1 B1 O1 -11.0(11) . . . . ? C8 N1 B1 O1 167.1(7) . . . . ? C7 N1 B1 C34 -127.7(8) . . . . ? C8 N1 B1 C34 50.4(10) . . . . ? C12 C9 C11 C8 -0.1(13) . . . . ? B2 C9 C11 C8 180.0(8) . . . . ? C10 C8 C11 C9 1.9(13) . . . . ? N1 C8 C11 C9 -179.0(8) . . . . ? C34 C35 C37 C38 0.3(14) . . . . ? C34 C35 C37 N3 180.0(8) . . . . ? C33 N3 C37 C35 50.2(11) . . . . ? B3 N3 C37 C35 -127.9(9) . . . . ? C33 N3 C37 C38 -130.2(9) . . . . ? B3 N3 C37 C38 51.8(12) . . . . ? C24 C21 C23 C22 1.7(13) . . . . ? N2 C21 C23 C22 -179.1(7) . . . . ? C25 C22 C23 C21 -2.0(12) . . . . ? B3 C22 C23 C21 -178.2(8) . . . . ? C39 C36 C38 C37 -0.8(14) . . . . ? C35 C37 C38 C36 -0.3(14) . . . . ? N3 C37 C38 C36 -179.9(8) . . . . ? C4 C3 C6 C1 -2.0(13) . . . . ? C4 C3 C6 C40 177.1(8) . . . . ? O1 C1 C6 C3 -178.7(8) . . . . ? C5 C1 C6 C3 1.4(13) . . . . ? O1 C1 C6 C40 2.2(13) . . . . ? C5 C1 C6 C40 -177.8(8) . . . . ? C41 C40 C6 C3 117.0(10) . . . . ? C42 C40 C6 C3 -4.1(13) . . . . ? C43 C40 C6 C3 -122.3(9) . . . . ? C41 C40 C6 C1 -63.9(11) . . . . ? C42 C40 C6 C1 175.0(9) . . . . ? C43 C40 C6 C1 56.8(11) . . . . ? C23 C21 C24 C26 0.9(12) . . . . ? N2 C21 C24 C26 -178.3(7) . . . . ? C28 C31 C32 C29 -4.3(14) . . . . ? C58 C31 C32 C29 175.3(9) . . . . ? C30 C29 C32 C31 -1.3(14) . . . . ? C59 C29 C32 C31 177.8(9) . . . . ? C11 C9 C12 C13 -1.7(12) . . . . ? B2 C9 C12 C13 178.2(8) . . . . ? C8 C10 C13 C12 0.2(13) . . . . ? C9 C12 C13 C10 1.7(13) . . . . ? C23 C22 C25 C26 -0.3(12) . . . . ? B3 C22 C25 C26 175.6(8) . . . . ? C15 C16 C17 C18 -2.9(16) . . . . ? C49 C16 C17 C18 174.9(10) . . . . ? C16 C17 C18 C19 2.5(16) . . . . ? C16 C17 C18 C53 -177.1(10) . . . . ? C17 C18 C19 C14 -0.4(14) . . . . ? C53 C18 C19 C14 179.2(9) . . . . ? C20 C14 C19 C18 -171.9(8) . . . . ? C15 C14 C19 C18 -1.1(14) . . . . ? C22 C25 C26 C24 2.8(13) . . . . ? C21 C24 C26 C25 -3.1(13) . . . . ? C38 C36 C39 C34 1.9(15) . . . . ? C35 C34 C39 C36 -1.8(14) . . . . ? B1 C34 C39 C36 -179.7(9) . . . . ? C54 O5 B2 O2 56.3(11) . . . . ? C54 O5 B2 C9 -179.9(7) . . . . ? C54 O5 B2 N2 -59.8(10) . . . . ? C15 O2 B2 O5 -90.8(10) . . . . ? C15 O2 B2 C9 144.1(8) . . . . ? C15 O2 B2 N2 28.5(11) . . . . ? C11 C9 B2 O5 -175.9(8) . . . . ? C12 C9 B2 O5 4.2(12) . . . . ? C11 C9 B2 O2 -49.0(11) . . . . ? C12 C9 B2 O2 131.1(8) . . . . ? C11 C9 B2 N2 63.5(10) . . . . ? C12 C9 B2 N2 -116.4(8) . . . . ? C20 N2 B2 O5 97.1(9) . . . . ? C21 N2 B2 O5 -83.3(9) . . . . ? C20 N2 B2 O2 -25.5(10) . . . . ? C21 N2 B2 O2 154.1(7) . . . . ? C20 N2 B2 C9 -141.2(8) . . . . ? C21 N2 B2 C9 38.4(10) . . . . ? C17 C16 C49 C50 123.6(10) . . . . ? C15 C16 C49 C50 -58.8(13) . . . . ? C17 C16 C49 C52 1.5(15) . . . . ? C15 C16 C49 C52 179.1(10) . . . . ? C17 C16 C49 C51 -116.6(10) . . . . ? C15 C16 C49 C51 61.0(11) . . . . ? C63 O6 B3 O3 -58.1(10) . . . . ? C63 O6 B3 N3 -173.9(6) . . . . ? C63 O6 B3 C22 65.6(10) . . . . ? C28 O3 B3 O6 -80.9(10) . . . . ? C28 O3 B3 N3 33.1(11) . . . . ? C28 O3 B3 C22 149.0(7) . . . . ? C33 N3 B3 O6 94.4(9) . . . . ? C37 N3 B3 O6 -87.6(9) . . . . ? C33 N3 B3 O3 -26.1(11) . . . . ? C37 N3 B3 O3 151.9(7) . . . . ? C33 N3 B3 C22 -139.5(8) . . . . ? C37 N3 B3 C22 38.6(10) . . . . ? C23 C22 B3 O6 -167.7(8) . . . . ? C25 C22 B3 O6 16.5(13) . . . . ? C23 C22 B3 O3 -39.9(10) . . . . ? C25 C22 B3 O3 144.3(8) . . . . ? C23 C22 B3 N3 74.5(9) . . . . ? C25 C22 B3 N3 -101.3(9) . . . . ? C17 C18 C53 C73 10(2) . . . . ? C19 C18 C53 C73 -169.3(18) . . . . ? C17 C18 C53 C71 148.4(14) . . . . ? C19 C18 C53 C71 -31.1(16) . . . . ? C17 C18 C53 C72 -105.1(11) . . . . ? C19 C18 C53 C72 75.4(11) . . . . ? C32 C31 C58 C57 120.2(9) . . . . ? C28 C31 C58 C57 -60.2(11) . . . . ? C32 C31 C58 C55 -119.4(9) . . . . ? C28 C31 C58 C55 60.1(12) . . . . ? C32 C31 C58 C56 -0.6(13) . . . . ? C28 C31 C58 C56 179.0(9) . . . . ? O7 C81 O8 C83 -38(6) . . . . ? C82 C81 O8 C83 150(3) . . . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.833 _refine_diff_density_min -1.601 _refine_diff_density_rms 0.078 data_complex1c _database_code_depnum_ccdc_archive 'CCDC 230232' _audit_creation_method SHELXL-97 #Chemical and physical data _chemical_name_systematic ; Trimethoxy-[tris-[mu-(3-phenyl-kC)imine-kN]methyl-2-(3,5-di-tert- butyl)phenolate-kO)triboro' ; _chemical_name_common ; Trimethoxy-(tris-(mu-(3-phenyl-kC)imine-kN)methyl-2-(3,5-di- tert-butyl)phenolate-kO)triboro' ; _chemical_melting_point 282 _chemical_formula_moiety ? _chemical_formula_sum 'C96 H111 B3 N3 O6' _chemical_formula_weight 1435.31 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 Cubic _symmetry_space_group_name_H-M Pa-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' _cell_length_a 25.8615(7) _cell_length_b 25.8615(7) _cell_length_c 25.8615(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17296.6(8) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description hexagon _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.102 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6168 _exptl_absorpt_coefficient_mu 0.067 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 102023 _diffrn_reflns_av_R_equivalents 0.1122 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 22.99 _reflns_number_total 4019 _reflns_number_gt 3791 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Cell parameters were determined by least squares refinements on diffractometer angles for 24 automatically centered reflections collected on three sets of 20 frames each. Non-hydrogen atoms were refined anisotropically. Hydrogen atoms were placed in geometrically calculated positionsusing a riding model. One disordered tBu group,DFIX and EADP instructions have been used. ; _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^)+(0.0472P)^2^+53.9293P] 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 4019 _refine_ls_number_parameters 369 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1171 _refine_ls_R_factor_gt 0.1111 _refine_ls_wR_factor_ref 0.2234 _refine_ls_wR_factor_gt 0.2200 _refine_ls_goodness_of_fit_ref 1.260 _refine_ls_restrained_S_all 1.260 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.0236(2) 0.8343(2) 0.2844(2) 0.0266(12) Uani 1 1 d . . . N1 N 0.04681(14) 0.78951(15) 0.32231(14) 0.0249(9) Uani 1 1 d . . . O1 O 0.04127(11) 0.81971(11) 0.23172(11) 0.0241(7) Uani 1 1 d . . . O2 O -0.03126(11) 0.83559(11) 0.28987(12) 0.0280(8) Uani 1 1 d . . . C1 C 0.05184(17) 0.77173(17) 0.21500(18) 0.0255(11) Uani 1 1 d . . . C2 C 0.05876(18) 0.73177(17) 0.25069(18) 0.0268(11) Uani 1 1 d . . . C3 C 0.07127(18) 0.68173(18) 0.23396(19) 0.0316(12) Uani 1 1 d . . . H3 H 0.0751 0.6549 0.2587 0.038 Uiso 1 1 calc R . . C4 C 0.07797(18) 0.67085(18) 0.18279(19) 0.0296(11) Uani 1 1 d . A . C5 C 0.07130(18) 0.71234(17) 0.14810(18) 0.0271(11) Uani 1 1 d . . . H5 H 0.0760 0.7053 0.1123 0.033 Uiso 1 1 calc R . . C6 C 0.05845(17) 0.76243(17) 0.16185(18) 0.0266(11) Uani 1 1 d . . . C7 C 0.05857(17) 0.74412(18) 0.30448(18) 0.0270(11) Uani 1 1 d . . . H7 H 0.0675 0.7178 0.3285 0.032 Uiso 1 1 calc R . . C8 C 0.05450(17) 0.79988(17) 0.37627(17) 0.0239(11) Uani 1 1 d . . . C9 C 0.10179(17) 0.78842(16) 0.39910(17) 0.0222(10) Uani 1 1 d . . . H9 H 0.1285 0.7735 0.3787 0.027 Uiso 1 1 calc R . . C10 C 0.11090(17) 0.79841(16) 0.45129(17) 0.0234(10) Uani 1 1 d . . . C11 C 0.07091(18) 0.82094(18) 0.47919(18) 0.0299(12) Uani 1 1 d . . . H11 H 0.0759 0.8285 0.5148 0.036 Uiso 1 1 calc R . . C12 C 0.02405(19) 0.8326(2) 0.45647(19) 0.0357(13) Uani 1 1 d . . . H12 H -0.0028 0.8475 0.4767 0.043 Uiso 1 1 calc R . . C13 C 0.01569(18) 0.82269(19) 0.40453(18) 0.0321(12) Uani 1 1 d . . . H13 H -0.0163 0.8315 0.3887 0.039 Uiso 1 1 calc R . . C14 C -0.0610(2) 0.7925(2) 0.2735(2) 0.0430(14) Uani 1 1 d . . . H14A H -0.0517 0.7835 0.2379 0.065 Uiso 1 1 calc R . . H14B H -0.0978 0.8013 0.2751 0.065 Uiso 1 1 calc R . . H14C H -0.0541 0.7630 0.2962 0.065 Uiso 1 1 calc R . . C15 C 0.05378(18) 0.80652(17) 0.12201(18) 0.0275(11) Uani 1 1 d . . . C16 C 0.0969(2) 0.84643(19) 0.1322(2) 0.0386(13) Uani 1 1 d . . . H16A H 0.0933 0.8603 0.1673 0.058 Uiso 1 1 calc R . . H16B H 0.0942 0.8747 0.1071 0.058 Uiso 1 1 calc R . . H16C H 0.1307 0.8297 0.1286 0.058 Uiso 1 1 calc R . . C17 C 0.00052(19) 0.83226(18) 0.12594(18) 0.0315(12) Uani 1 1 d . . . H17A H -0.0265 0.8065 0.1191 0.047 Uiso 1 1 calc R . . H17B H -0.0019 0.8602 0.1004 0.047 Uiso 1 1 calc R . . H17C H -0.0041 0.8465 0.1608 0.047 Uiso 1 1 calc R . . C18 C 0.05962(19) 0.78672(18) 0.06696(18) 0.0300(12) Uani 1 1 d . . . H18A H 0.0934 0.7699 0.0631 0.045 Uiso 1 1 calc R . . H18B H 0.0571 0.8158 0.0428 0.045 Uiso 1 1 calc R . . H18C H 0.0321 0.7617 0.0595 0.045 Uiso 1 1 calc R . . C19 C 0.09010(18) 0.61733(18) 0.16243(17) 0.0410(14) Uani 1 1 d D . . C20A C 0.0475(3) 0.5987(3) 0.1252(3) 0.039(2) Uani 0.647(10) 1 d PD A 1 H20A H 0.0561 0.5640 0.1125 0.059 Uiso 0.647(10) 1 calc PR A 1 H20B H 0.0450 0.6225 0.0959 0.059 Uiso 0.647(10) 1 calc PR A 1 H20C H 0.0143 0.5976 0.1435 0.059 Uiso 0.647(10) 1 calc PR A 1 C21A C 0.0952(5) 0.5760(3) 0.2050(3) 0.049(3) Uani 0.647(10) 1 d PD A 1 H21A H 0.1032 0.5425 0.1891 0.073 Uiso 0.647(10) 1 calc PR A 1 H21B H 0.0626 0.5734 0.2241 0.073 Uiso 0.647(10) 1 calc PR A 1 H21C H 0.1231 0.5857 0.2287 0.073 Uiso 0.647(10) 1 calc PR A 1 C22A C 0.1400(2) 0.6189(3) 0.1300(3) 0.036(2) Uani 0.647(10) 1 d PD A 1 H22A H 0.1478 0.5841 0.1172 0.054 Uiso 0.647(10) 1 calc PR A 1 H22B H 0.1687 0.6311 0.1516 0.054 Uiso 0.647(10) 1 calc PR A 1 H22C H 0.1353 0.6424 0.1007 0.054 Uiso 0.647(10) 1 calc PR A 1 C20B C 0.1424(4) 0.6054(7) 0.1884(7) 0.112(13) Uani 0.353(10) 1 d PD A 2 H20D H 0.1541 0.5709 0.1779 0.169 Uiso 0.353(10) 1 calc PR A 2 H20E H 0.1383 0.6065 0.2261 0.169 Uiso 0.353(10) 1 calc PR A 2 H20F H 0.1679 0.6313 0.1777 0.169 Uiso 0.353(10) 1 calc PR A 2 C21B C 0.0598(8) 0.5763(5) 0.1931(6) 0.046(5) Uani 0.353(10) 1 d PD A 2 H21D H 0.0681 0.5418 0.1797 0.069 Uiso 0.353(10) 1 calc PR A 2 H21E H 0.0226 0.5826 0.1894 0.069 Uiso 0.353(10) 1 calc PR A 2 H21F H 0.0693 0.5783 0.2297 0.069 Uiso 0.353(10) 1 calc PR A 2 C22B C 0.1087(9) 0.6142(7) 0.1060(3) 0.069(7) Uani 0.353(10) 1 d PD A 2 H22D H 0.1154 0.5780 0.0969 0.103 Uiso 0.353(10) 1 calc PR A 2 H22E H 0.1406 0.6343 0.1021 0.103 Uiso 0.353(10) 1 calc PR A 2 H22F H 0.0820 0.6282 0.0831 0.103 Uiso 0.353(10) 1 calc PR A 2 C31 C 0.1947(2) 0.7544(2) 0.2317(2) 0.0545(16) Uani 1 1 d . . . H31 H 0.1659 0.7480 0.2098 0.065 Uiso 1 1 calc R . . C32 C 0.2048(2) 0.7224(3) 0.2733(2) 0.0554(16) Uani 1 1 d . . . H32 H 0.1829 0.6935 0.2798 0.066 Uiso 1 1 calc R . . C41 C 0.4672(3) 0.5532(3) 0.2118(3) 0.077(2) Uani 1 1 d . . . H41 H 0.4696 0.5203 0.2279 0.092 Uiso 1 1 calc R . . C42 C 0.4425(3) 0.5926(3) 0.2353(3) 0.074(2) Uani 1 1 d . . . H42 H 0.4292 0.5880 0.2692 0.089 Uiso 1 1 calc R . . C43 C 0.4363(3) 0.6399(3) 0.2107(3) 0.078(2) Uani 1 1 d . . . H43 H 0.4176 0.6670 0.2271 0.094 Uiso 1 1 calc R . . C44 C 0.4574(3) 0.6475(3) 0.1623(3) 0.078(2) Uani 1 1 d . . . H44 H 0.4539 0.6799 0.1454 0.094 Uiso 1 1 calc R . . C45 C 0.4832(3) 0.6077(3) 0.1388(3) 0.082(2) Uani 1 1 d . . . H45 H 0.4973 0.6121 0.1051 0.099 Uiso 1 1 calc R . . C46 C 0.4888(3) 0.5613(4) 0.1643(3) 0.091(3) Uani 1 1 d . . . H46 H 0.5081 0.5344 0.1485 0.110 Uiso 1 1 calc R . . C51 C 0.5429(2) 0.5160(2) 0.0266(2) 0.0533(16) Uani 1 1 d . . . H51 H 0.5729 0.5269 0.0448 0.064 Uiso 1 1 calc R . . C71 C 0.9691(4) 0.4691(4) 0.0309(4) 0.101(7) Uani 1 3 d S . . C72 C 1.0073(7) 0.4683(7) 0.0404(7) 0.040(4) Uani 0.33 1 d P . . C73 C 0.9497(6) 0.5139(6) -0.0139(6) 0.036(4) Uani 0.33 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.028(3) 0.027(3) 0.025(3) 0.005(2) -0.003(2) -0.001(2) N1 0.019(2) 0.031(2) 0.024(2) 0.0045(18) 0.0010(16) -0.0031(17) O1 0.0287(17) 0.0189(17) 0.0246(17) -0.0022(13) -0.0016(14) 0.0014(14) O2 0.0214(17) 0.0242(17) 0.038(2) -0.0001(15) -0.0058(14) -0.0017(14) C1 0.022(2) 0.026(3) 0.029(3) -0.001(2) -0.004(2) -0.004(2) C2 0.028(3) 0.025(3) 0.027(3) 0.000(2) 0.000(2) -0.003(2) C3 0.033(3) 0.025(3) 0.037(3) 0.007(2) 0.005(2) 0.003(2) C4 0.031(3) 0.025(3) 0.033(3) 0.003(2) 0.007(2) -0.001(2) C5 0.028(3) 0.027(3) 0.027(3) -0.006(2) 0.003(2) -0.001(2) C6 0.025(3) 0.025(3) 0.030(3) 0.000(2) -0.003(2) -0.003(2) C7 0.026(3) 0.024(3) 0.031(3) 0.006(2) -0.002(2) 0.001(2) C8 0.024(3) 0.025(3) 0.023(2) 0.005(2) -0.002(2) -0.001(2) C9 0.023(2) 0.019(2) 0.024(3) 0.0041(19) 0.005(2) 0.0009(19) C10 0.030(3) 0.017(2) 0.023(3) 0.0066(19) 0.008(2) -0.005(2) C11 0.037(3) 0.029(3) 0.023(3) 0.007(2) 0.004(2) 0.004(2) C12 0.032(3) 0.048(3) 0.027(3) 0.008(2) 0.010(2) 0.017(2) C13 0.024(3) 0.042(3) 0.030(3) 0.014(2) 0.002(2) 0.006(2) C14 0.030(3) 0.035(3) 0.064(4) 0.001(3) -0.003(3) -0.001(2) C15 0.028(3) 0.026(3) 0.028(3) 0.000(2) -0.002(2) -0.001(2) C16 0.053(3) 0.029(3) 0.034(3) 0.007(2) -0.002(3) -0.010(3) C17 0.041(3) 0.028(3) 0.026(3) -0.003(2) -0.007(2) 0.007(2) C18 0.035(3) 0.026(3) 0.029(3) 0.000(2) 0.000(2) 0.003(2) C19 0.050(3) 0.026(3) 0.047(3) 0.004(2) 0.022(3) 0.006(3) C20A 0.040(5) 0.020(4) 0.058(6) -0.005(4) 0.002(4) -0.005(4) C21A 0.065(8) 0.029(5) 0.051(6) 0.011(4) 0.027(6) 0.011(5) C22A 0.047(6) 0.030(5) 0.031(5) -0.001(4) 0.007(4) 0.013(4) C20B 0.24(4) 0.020(10) 0.077(16) -0.013(10) 0.09(2) 0.006(15) C21B 0.080(14) 0.021(8) 0.037(10) -0.006(7) 0.009(11) 0.001(10) C22B 0.093(17) 0.052(12) 0.061(13) -0.014(10) -0.033(12) 0.023(11) C31 0.045(4) 0.060(4) 0.059(4) 0.009(3) -0.009(3) -0.003(3) C32 0.051(4) 0.061(4) 0.054(4) 0.010(3) 0.001(3) -0.015(3) C41 0.069(5) 0.082(5) 0.079(5) 0.015(4) 0.001(4) 0.022(4) C42 0.084(5) 0.074(5) 0.065(5) 0.002(4) -0.001(4) 0.004(4) C43 0.098(6) 0.065(5) 0.072(5) 0.002(4) 0.015(4) -0.003(4) C44 0.091(6) 0.078(5) 0.067(5) 0.000(4) -0.002(4) -0.005(5) C45 0.085(6) 0.099(6) 0.063(5) 0.004(5) -0.003(4) 0.019(5) C46 0.072(5) 0.114(7) 0.088(6) 0.007(5) 0.001(5) 0.048(5) C51 0.049(4) 0.059(4) 0.052(4) 0.011(3) -0.016(3) -0.016(3) C71 0.101(7) 0.101(7) 0.101(7) 0.033(7) 0.033(7) -0.033(7) C72 0.057(13) 0.039(11) 0.023(9) -0.002(7) 0.007(10) -0.029(10) C73 0.042(10) 0.026(8) 0.038(10) 0.007(7) -0.006(8) 0.000(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 B1 O2 1.426(6) . ? B1 O1 1.487(6) . ? B1 C10 1.601(7) 7_564 ? B1 N1 1.631(6) . ? N1 C7 1.297(6) . ? N1 C8 1.435(6) . ? O1 C1 1.342(5) . ? O2 C14 1.419(6) . ? C1 C2 1.397(6) . ? C1 C6 1.406(6) . ? C2 C3 1.402(7) . ? C2 C7 1.427(7) . ? C3 C4 1.364(7) . ? C4 C5 1.409(6) . ? C4 C19 1.514(7) . ? C5 C6 1.384(6) . ? C6 C15 1.542(6) . ? C8 C13 1.375(6) . ? C8 C9 1.390(6) . ? C9 C10 1.394(6) . ? C10 C11 1.389(6) . ? C10 B1 1.601(7) 10_655 ? C11 C12 1.380(7) . ? C12 C13 1.384(7) . ? C15 C18 1.521(6) . ? C15 C17 1.533(7) . ? C15 C16 1.543(7) . ? C19 C21A 1.5393(10) . ? C19 C22B 1.5395(11) . ? C19 C22A 1.5395(10) . ? C19 C21B 1.5397(10) . ? C19 C20B 1.5403(11) . ? C19 C20A 1.5410(10) . ? C31 C32 1.362(8) 7_564 ? C31 C32 1.384(8) . ? C32 C31 1.362(8) 10_655 ? C41 C42 1.349(10) . ? C41 C46 1.365(10) . ? C42 C43 1.388(10) . ? C43 C44 1.379(10) . ? C44 C45 1.369(10) . ? C45 C46 1.376(11) . ? C51 C51 1.370(6) 19_656 ? C51 C51 1.370(6) 22_565 ? C71 C72 1.017(17) . ? C71 C72 1.017(17) 8_645 ? C71 C72 1.017(17) 11_556 ? C71 C73 1.713(18) 11_556 ? C71 C73 1.713(18) 8_645 ? C71 C73 1.713(18) . ? C72 C73 1.22(2) 11_556 ? C72 C73 1.38(2) 13_765 ? C72 C73 1.49(2) 8_645 ? C72 C72 1.61(3) 8_645 ? C72 C72 1.61(3) 11_556 ? C73 C72 1.22(2) 8_645 ? C73 C72 1.38(2) 13_765 ? C73 C72 1.49(2) 11_556 ? C73 C73 1.51(2) 23_764 ? C73 C73 1.51(2) 20_675 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 B1 O1 113.7(4) . . ? O2 B1 C10 111.1(4) . 7_564 ? O1 B1 C10 107.9(4) . 7_564 ? O2 B1 N1 108.9(4) . . ? O1 B1 N1 104.9(4) . . ? C10 B1 N1 110.1(4) 7_564 . ? C7 N1 C8 118.8(4) . . ? C7 N1 B1 121.0(4) . . ? C8 N1 B1 120.1(4) . . ? C1 O1 B1 126.3(4) . . ? C14 O2 B1 119.4(4) . . ? O1 C1 C2 119.8(4) . . ? O1 C1 C6 119.9(4) . . ? C2 C1 C6 120.2(4) . . ? C1 C2 C3 120.5(4) . . ? C1 C2 C7 118.6(4) . . ? C3 C2 C7 120.5(4) . . ? C4 C3 C2 121.3(4) . . ? C3 C4 C5 116.4(4) . . ? C3 C4 C19 123.5(4) . . ? C5 C4 C19 120.0(4) . . ? C6 C5 C4 125.3(4) . . ? C5 C6 C1 116.2(4) . . ? C5 C6 C15 122.6(4) . . ? C1 C6 C15 121.2(4) . . ? N1 C7 C2 123.3(4) . . ? C13 C8 C9 120.5(4) . . ? C13 C8 N1 119.8(4) . . ? C9 C8 N1 119.7(4) . . ? C8 C9 C10 121.4(4) . . ? C11 C10 C9 117.1(4) . . ? C11 C10 B1 122.9(4) . 10_655 ? C9 C10 B1 120.0(4) . 10_655 ? C12 C11 C10 121.6(5) . . ? C11 C12 C13 120.7(5) . . ? C8 C13 C12 118.8(4) . . ? C18 C15 C17 107.3(4) . . ? C18 C15 C6 111.7(4) . . ? C17 C15 C6 110.3(4) . . ? C18 C15 C16 108.2(4) . . ? C17 C15 C16 110.4(4) . . ? C6 C15 C16 108.9(4) . . ? C4 C19 C21A 113.8(5) . . ? C4 C19 C22B 116.3(8) . . ? C21A C19 C22B 127.9(9) . . ? C4 C19 C22A 109.8(4) . . ? C21A C19 C22A 109.6(6) . . ? C22B C19 C22A 39.0(8) . . ? C4 C19 C21B 110.2(7) . . ? C21A C19 C21B 36.6(7) . . ? C22B C19 C21B 127.7(11) . . ? C22A C19 C21B 136.5(9) . . ? C4 C19 C20B 102.3(7) . . ? C21A C19 C20B 58.3(9) . . ? C22B C19 C20B 97.4(11) . . ? C22A C19 C20B 60.4(8) . . ? C21B C19 C20B 94.8(11) . . ? C4 C19 C20A 110.8(4) . . ? C21A C19 C20A 106.9(6) . . ? C22B C19 C20A 67.3(9) . . ? C22A C19 C20A 105.5(5) . . ? C21B C19 C20A 75.0(9) . . ? C20B C19 C20A 146.9(8) . . ? C32 C31 C32 119.2(7) 7_564 . ? C31 C32 C31 120.8(7) 10_655 . ? C42 C41 C46 118.9(8) . . ? C41 C42 C43 120.9(7) . . ? C44 C43 C42 119.7(8) . . ? C45 C44 C43 119.3(8) . . ? C44 C45 C46 119.6(8) . . ? C41 C46 C45 121.5(8) . . ? C51 C51 C51 119.995(13) 19_656 22_565 ? C72 C71 C72 104.5(19) . 8_645 ? C72 C71 C72 104.5(19) . 11_556 ? C72 C71 C72 104.5(19) 8_645 11_556 ? C72 C71 C73 44.6(13) . 11_556 ? C72 C71 C73 60.1(13) 8_645 11_556 ? C72 C71 C73 118(2) 11_556 11_556 ? C72 C71 C73 60.1(13) . 8_645 ? C72 C71 C73 118(2) 8_645 8_645 ? C72 C71 C73 44.6(13) 11_556 8_645 ? C73 C71 C73 86.5(11) 11_556 8_645 ? C72 C71 C73 118(2) . . ? C72 C71 C73 44.6(13) 8_645 . ? C72 C71 C73 60.1(13) 11_556 . ? C73 C71 C73 86.5(11) 11_556 . ? C73 C71 C73 86.5(11) 8_645 . ? C71 C72 C73 100(2) . 11_556 ? C71 C72 C73 131(2) . 13_765 ? C73 C72 C73 70.7(10) 11_556 13_765 ? C71 C72 C73 83.7(15) . 8_645 ? C73 C72 C73 119.5(19) 11_556 8_645 ? C73 C72 C73 63.2(9) 13_765 8_645 ? C71 C72 C72 37.8(9) . 8_645 ? C73 C72 C72 62.0(16) 11_556 8_645 ? C73 C72 C72 109.8(11) 13_765 8_645 ? C73 C72 C72 99.1(11) 8_645 8_645 ? C71 C72 C72 37.7(9) . 11_556 ? C73 C72 C72 112.6(15) 11_556 11_556 ? C73 C72 C72 99.9(11) 13_765 11_556 ? C73 C72 C72 46.1(11) 8_645 11_556 ? C72 C72 C72 60.000(3) 8_645 11_556 ? C72 C73 C72 110.9(18) 8_645 13_765 ? C72 C73 C72 71.9(18) 8_645 11_556 ? C72 C73 C72 96.4(16) 13_765 11_556 ? C72 C73 C73 113.8(11) 8_645 23_764 ? C72 C73 C73 49.6(12) 13_765 23_764 ? C72 C73 C73 54.8(8) 11_556 23_764 ? C72 C73 C73 59.7(10) 8_645 20_675 ? C72 C73 C73 62.0(12) 13_765 20_675 ? C72 C73 C73 109.3(10) 11_556 20_675 ? C73 C73 C73 101.9(13) 23_764 20_675 ? C72 C73 C71 35.8(10) 8_645 . ? C72 C73 C71 108.9(12) 13_765 . ? C72 C73 C71 36.2(8) 11_556 . ? C73 C73 C71 85.2(7) 23_764 . ? C73 C73 C71 85.2(7) 20_675 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.619 _refine_diff_density_min -0.580 _refine_diff_density_rms 0.056 data_complex1d _database_code_depnum_ccdc_archive 'CCDC 230233' _audit_creation_method SHELXL-97 #--------------------------------------------------------------------------- #Chemical and physical data _chemical_name_systematic ; Trimethoxy-[tris-[mu-(3-phenyl-kC)imine-kN]methyl-2-(3,5-di-tert- butyl)phenolate-kO)triboro' ; _chemical_name_common ; Trimethoxy-(tris-(mu-(3-phenyl-kC)imine-kN)methyl-2-(3,5-di- tert-butyl)phenolate-kO)triboro' ; _chemical_melting_point ' 271 C ' _chemical_formula_moiety ? _chemical_formula_sum 'C77.33 H96 B2.67 N2.67 O10.67' _chemical_formula_weight 1262.39 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M Pa-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' _cell_length_a 25.6586(13) _cell_length_b 25.6586(13) _cell_length_c 25.6586(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 16892.7(15) _cell_formula_units_Z 9 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prims _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.117 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6096 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 133329 _diffrn_reflns_av_R_equivalents 0.0768 _diffrn_reflns_av_sigmaI/netI 0.0192 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 22.99 _reflns_number_total 3926 _reflns_number_gt 3895 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Cell parameters were determined by least squares refinements on diffractometer angles for 24 automatically centered reflections collected on three sets of 20 frames each. Non-hydrogen atoms were refined anisotropically. Hydrogen atoms were placed in geometrically calculated positionsusing a riding model. THF molecules are disordered and located at special positions (C3 axis) in the crystal lattice, leading to high R values; However, our interest in this structure has been mainly focused on the confirmation of the molecular structure and the conformation of the molecule, but not in the disscusion of particular bond lengths or bond angles. ; _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^)+(0.0609P)^2^+69.5827P] 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 3926 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1079 _refine_ls_R_factor_gt 0.1072 _refine_ls_wR_factor_ref 0.2338 _refine_ls_wR_factor_gt 0.2334 _refine_ls_goodness_of_fit_ref 1.229 _refine_ls_restrained_S_all 1.229 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.97875(19) 0.66558(19) 0.28616(19) 0.0167(11) Uani 1 1 d . . . N1 N 0.95483(13) 0.70983(14) 0.32486(13) 0.0151(8) Uani 1 1 d . . . O1 O 0.95943(11) 0.67952(10) 0.23340(11) 0.0152(7) Uani 1 1 d . . . O2 O 1.03432(11) 0.66632(11) 0.29039(11) 0.0177(7) Uani 1 1 d . . . O10 O 0.0236(3) 0.8125(2) 0.3847(2) 0.0930(19) Uani 1 1 d . . . O11 O 0.7884(17) 0.7337(14) 0.3065(8) 0.217(15) Uani 0.67 1 d P . . O12 O 0.9748(5) 0.5252(5) 0.4748(5) 0.237(11) Uani 1 3 d S . . C1 C 0.92508(18) 0.81771(17) 0.23704(17) 0.0214(11) Uani 1 1 d . . . H1 H 0.9206 0.8439 0.2617 0.026 Uiso 1 1 calc R . . C2 C 0.91790(18) 0.82864(17) 0.18529(17) 0.0207(10) Uani 1 1 d . . . C3 C 0.94117(17) 0.75499(17) 0.30731(17) 0.0180(10) Uani 1 1 d . . . H3 H 0.9322 0.7808 0.3312 0.022 Uiso 1 1 calc R . . C4 C 0.92460(17) 0.78698(17) 0.14996(17) 0.0198(10) Uani 1 1 d . . . H4 H 0.9189 0.7939 0.1148 0.024 Uiso 1 1 calc R . . C5 C 0.94691(16) 0.72737(16) 0.21715(17) 0.0157(10) Uani 1 1 d . . . C6 C 0.93913(17) 0.76726(16) 0.25329(17) 0.0182(10) Uani 1 1 d . . . C7 C 0.93902(16) 0.73678(16) 0.16327(16) 0.0156(10) Uani 1 1 d . . . C8 C 0.98739(16) 0.67687(16) 0.40842(17) 0.0180(10) Uani 1 1 d . . . H8 H 1.0194 0.6692 0.3932 0.022 Uiso 1 1 calc R . . C9 C 0.97865(17) 0.66671(18) 0.46060(17) 0.0208(10) Uani 1 1 d . . . H9 H 1.0051 0.6523 0.4807 0.025 Uiso 1 1 calc R . . C10 C 0.93100(17) 0.67770(16) 0.48317(16) 0.0166(10) Uani 1 1 d . . . H10 H 0.9261 0.6704 0.5183 0.020 Uiso 1 1 calc R . . C11 C 0.89980(16) 0.70927(16) 0.40216(16) 0.0147(9) Uani 1 1 d . . . H11 H 0.8733 0.7234 0.3818 0.018 Uiso 1 1 calc R . . C12 C 0.94764(16) 0.69865(16) 0.37947(16) 0.0145(9) Uani 1 1 d . . . C13 C 0.89024(16) 0.69930(15) 0.45493(16) 0.0130(9) Uani 1 1 d . . . C14 C 0.90057(19) 0.65261(18) 0.13325(18) 0.0278(11) Uani 1 1 d . . . H14A H 0.9043 0.6384 0.1677 0.042 Uiso 1 1 calc R . . H14B H 0.9029 0.6250 0.1081 0.042 Uiso 1 1 calc R . . H14C H 0.8673 0.6694 0.1302 0.042 Uiso 1 1 calc R . . C15 C 0.99783(18) 0.66601(18) 0.12681(17) 0.0227(11) Uani 1 1 d . . . H15A H 1.0016 0.6500 0.1604 0.034 Uiso 1 1 calc R . . H15B H 1.0247 0.6916 0.1221 0.034 Uiso 1 1 calc R . . H15C H 1.0006 0.6399 0.1002 0.034 Uiso 1 1 calc R . . C16 C 0.93820(18) 0.71271(17) 0.06733(17) 0.0213(10) Uani 1 1 d . . . H16A H 0.9418 0.6842 0.0434 0.032 Uiso 1 1 calc R . . H16B H 0.9647 0.7382 0.0604 0.032 Uiso 1 1 calc R . . H16C H 0.9045 0.7283 0.0632 0.032 Uiso 1 1 calc R . . C17 C 0.94414(17) 0.69258(16) 0.12328(17) 0.0175(10) Uani 1 1 d . . . C18 C 0.9456(3) 0.9020(2) 0.1270(2) 0.0478(16) Uani 1 1 d . . . H18A H 0.9375 0.9366 0.1153 0.072 Uiso 1 1 calc R . . H18B H 0.9470 0.8789 0.0976 0.072 Uiso 1 1 calc R . . H18C H 0.9788 0.9021 0.1443 0.072 Uiso 1 1 calc R . . C19 C 0.8992(3) 0.9222(2) 0.2084(2) 0.0559(19) Uani 1 1 d . . . H19A H 0.8901 0.9556 0.1941 0.084 Uiso 1 1 calc R . . H19B H 0.9323 0.9247 0.2258 0.084 Uiso 1 1 calc R . . H19C H 0.8730 0.9116 0.2329 0.084 Uiso 1 1 calc R . . C20 C 0.8521(2) 0.8805(2) 0.1355(2) 0.0431(15) Uani 1 1 d . . . H20A H 0.8242 0.8716 0.1589 0.065 Uiso 1 1 calc R . . H20B H 0.8547 0.8545 0.1088 0.065 Uiso 1 1 calc R . . H20C H 0.8451 0.9138 0.1199 0.065 Uiso 1 1 calc R . . C21 C 0.9028(2) 0.88311(18) 0.16558(18) 0.0289(12) Uani 1 1 d . . . C22 C 1.06193(18) 0.70941(19) 0.2702(2) 0.0291(12) Uani 1 1 d . . . H22A H 1.0544 0.7131 0.2338 0.044 Uiso 1 1 calc R . . H22B H 1.0987 0.7040 0.2749 0.044 Uiso 1 1 calc R . . H22C H 1.0515 0.7405 0.2883 0.044 Uiso 1 1 calc R . . C30 C 0.0008(3) 0.8245(3) 0.4335(3) 0.079(2) Uani 1 1 d . . . H30A H -0.0211 0.7963 0.4458 0.095 Uiso 1 1 calc R . . H30B H -0.0196 0.8563 0.4318 0.095 Uiso 1 1 calc R . . C31 C 0.0917(5) 0.7876(5) 0.4502(3) 0.135(5) Uani 1 1 d . . . H31A H 0.1274 0.7975 0.4581 0.162 Uiso 1 1 calc R . . H31B H 0.0843 0.7534 0.4646 0.162 Uiso 1 1 calc R . . C32 C 0.0797(5) 0.7910(5) 0.3932(4) 0.118(4) Uani 1 1 d . . . H32A H 0.0826 0.7567 0.3776 0.141 Uiso 1 1 calc R . . H32B H 0.1047 0.8138 0.3763 0.141 Uiso 1 1 calc R . . C33 C 0.0496(5) 0.8316(5) 0.4692(4) 0.135(5) Uani 1 1 d . . . H33A H 0.0404 0.8263 0.5055 0.162 Uiso 1 1 calc R . . H33B H 0.0640 0.8663 0.4653 0.162 Uiso 1 1 calc R . . C34 C 0.7646(11) 0.7761(8) 0.2986(8) 0.136(7) Uani 0.67 1 d P . . C35 C 0.7714(9) 0.7781(11) 0.2427(11) 0.157(9) Uani 0.67 1 d P . . C36 C 0.9712(7) 0.9629(7) 0.5175(7) 0.158(5) Uani 1 1 d . . . C38 C 0.9618(15) 0.5228(19) 0.5234(7) 0.29(2) Uani 0.67 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.014(3) 0.018(3) 0.018(3) 0.001(2) -0.001(2) 0.000(2) N1 0.0110(18) 0.020(2) 0.0143(19) 0.0010(16) -0.0004(15) -0.0029(15) O1 0.0183(16) 0.0131(15) 0.0143(15) 0.0004(12) -0.0005(12) 0.0023(12) O2 0.0152(15) 0.0180(16) 0.0199(16) 0.0021(13) 0.0030(13) -0.0013(13) O10 0.112(5) 0.106(5) 0.062(4) 0.009(3) -0.015(3) -0.029(4) O11 0.216(17) 0.31(4) 0.123(13) -0.073(16) -0.073(11) 0.15(3) O12 0.237(11) 0.237(11) 0.237(11) 0.048(11) -0.048(11) 0.048(11) C1 0.032(3) 0.014(2) 0.019(2) -0.0041(19) -0.005(2) 0.004(2) C2 0.025(2) 0.015(2) 0.022(2) -0.0005(19) -0.005(2) -0.0007(19) C3 0.024(2) 0.015(2) 0.016(2) -0.0014(18) -0.0010(19) -0.0002(19) C4 0.023(2) 0.021(2) 0.015(2) 0.0026(19) -0.0048(19) -0.002(2) C5 0.011(2) 0.016(2) 0.020(2) 0.0013(19) 0.0006(18) -0.0010(18) C6 0.021(2) 0.019(2) 0.016(2) 0.0011(19) -0.0026(18) -0.0018(19) C7 0.015(2) 0.016(2) 0.015(2) -0.0006(18) 0.0008(18) -0.0048(18) C8 0.013(2) 0.019(2) 0.022(2) -0.0044(19) 0.0009(19) 0.0050(18) C9 0.020(2) 0.027(3) 0.015(2) 0.003(2) -0.0048(19) 0.005(2) C10 0.024(2) 0.016(2) 0.010(2) -0.0015(18) -0.0047(19) 0.0016(19) C11 0.014(2) 0.014(2) 0.016(2) 0.0011(18) -0.0057(18) 0.0038(18) C12 0.020(2) 0.012(2) 0.012(2) -0.0010(17) 0.0011(18) -0.0019(18) C13 0.020(2) 0.006(2) 0.012(2) -0.0022(16) -0.0034(18) -0.0040(17) C14 0.038(3) 0.023(3) 0.022(3) -0.006(2) -0.002(2) -0.008(2) C15 0.029(3) 0.022(2) 0.017(2) -0.0006(19) -0.002(2) 0.006(2) C16 0.026(3) 0.020(2) 0.018(2) -0.0018(19) -0.002(2) 0.004(2) C17 0.022(2) 0.014(2) 0.016(2) -0.0004(18) -0.0015(19) -0.0014(19) C18 0.072(4) 0.023(3) 0.048(4) 0.008(3) -0.006(3) 0.001(3) C19 0.105(6) 0.021(3) 0.042(3) 0.000(3) -0.029(4) 0.020(3) C20 0.062(4) 0.023(3) 0.045(3) 0.000(2) -0.022(3) 0.013(3) C21 0.049(3) 0.016(2) 0.022(3) 0.001(2) -0.011(2) 0.001(2) C22 0.020(3) 0.029(3) 0.038(3) 0.009(2) 0.003(2) -0.005(2) C30 0.093(6) 0.084(6) 0.061(5) -0.028(4) 0.004(4) -0.018(5) C31 0.212(14) 0.140(10) 0.054(5) -0.013(6) 0.006(7) -0.062(10) C32 0.147(11) 0.131(9) 0.076(7) -0.007(6) 0.017(7) -0.022(8) C33 0.157(11) 0.165(11) 0.083(7) -0.063(8) 0.037(7) -0.056(9) C34 0.17(2) 0.105(14) 0.128(17) -0.015(13) -0.025(17) 0.040(14) C35 0.17(2) 0.15(2) 0.15(2) 0.051(17) 0.05(2) 0.000(18) C36 0.133(13) 0.210(15) 0.131(12) 0.032(11) -0.043(9) -0.036(10) C38 0.31(4) 0.49(6) 0.066(12) -0.05(2) -0.057(19) 0.26(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 O2 1.430(6) . ? B1 O1 1.486(6) . ? B1 C13 1.601(6) 6_566 ? B1 N1 1.629(6) . ? N1 C3 1.292(6) . ? N1 C12 1.442(5) . ? O1 C5 1.336(5) . ? O2 C22 1.411(5) . ? O10 C30 1.416(9) . ? O10 C32 1.557(13) . ? O11 C34 1.26(2) . ? O11 O11 1.26(3) 6_566 ? O11 O11 1.26(3) 12_664 ? O12 C38 1.29(2) 6_566 ? O12 C38 1.29(2) 12_664 ? O12 C38 1.29(2) . ? C1 C2 1.370(6) . ? C1 C6 1.407(6) . ? C2 C4 1.412(6) . ? C2 C21 1.536(6) . ? C3 C6 1.422(6) . ? C4 C7 1.383(6) . ? C5 C6 1.395(6) . ? C5 C7 1.418(6) . ? C7 C17 1.535(6) . ? C8 C12 1.380(6) . ? C8 C9 1.382(6) . ? C9 C10 1.382(6) . ? C10 C13 1.388(6) . ? C11 C12 1.386(6) . ? C11 C13 1.400(6) . ? C13 B1 1.601(6) 12_664 ? C14 C17 1.538(6) . ? C15 C17 1.540(6) . ? C16 C17 1.533(6) . ? C18 C21 1.556(8) . ? C19 C21 1.491(7) . ? C20 C21 1.514(7) . ? C30 C33 1.561(13) . ? C31 C32 1.498(13) . ? C31 C33 1.636(16) . ? C34 C35 1.39(3) 12_664 ? C34 C35 1.45(3) . ? C35 C34 1.39(3) 6_566 ? C35 C35 1.56(4) 6_566 ? C35 C35 1.56(4) 12_664 ? C36 C36 1.306(13) 22_575 ? C36 C36 1.306(13) 19_657 ? C38 C38 1.61(4) 18_755 ? C38 C38 1.61(4) 24_657 ? C38 C38 2.02(4) 12_664 ? C38 C38 2.02(4) 6_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 B1 O1 113.5(4) . . ? O2 B1 C13 112.0(4) . 6_566 ? O1 B1 C13 107.5(3) . 6_566 ? O2 B1 N1 108.7(3) . . ? O1 B1 N1 105.2(3) . . ? C13 B1 N1 109.7(3) 6_566 . ? C3 N1 C12 118.8(4) . . ? C3 N1 B1 121.0(3) . . ? C12 N1 B1 120.1(3) . . ? C5 O1 B1 125.9(3) . . ? C22 O2 B1 118.9(3) . . ? C30 O10 C32 109.5(6) . . ? C34 O11 O11 116(2) . 6_566 ? C34 O11 O11 115(3) . 12_664 ? O11 O11 O11 60.000(9) 6_566 12_664 ? C38 O12 C38 103(2) 6_566 12_664 ? C38 O12 C38 103(2) 6_566 . ? C38 O12 C38 103(2) 12_664 . ? C2 C1 C6 120.7(4) . . ? C1 C2 C4 116.8(4) . . ? C1 C2 C21 122.7(4) . . ? C4 C2 C21 120.5(4) . . ? N1 C3 C6 123.3(4) . . ? C7 C4 C2 125.4(4) . . ? O1 C5 C6 120.1(4) . . ? O1 C5 C7 119.7(4) . . ? C6 C5 C7 120.2(4) . . ? C5 C6 C1 121.0(4) . . ? C5 C6 C3 118.7(4) . . ? C1 C6 C3 120.1(4) . . ? C4 C7 C5 115.9(4) . . ? C4 C7 C17 123.1(4) . . ? C5 C7 C17 120.9(4) . . ? C12 C8 C9 118.5(4) . . ? C10 C9 C8 120.7(4) . . ? C9 C10 C13 122.0(4) . . ? C12 C11 C13 121.7(4) . . ? C8 C12 C11 120.5(4) . . ? C8 C12 N1 120.6(4) . . ? C11 C12 N1 118.9(4) . . ? C10 C13 C11 116.5(4) . . ? C10 C13 B1 124.6(4) . 12_664 ? C11 C13 B1 118.9(4) . 12_664 ? C16 C17 C7 111.6(3) . . ? C16 C17 C14 107.9(4) . . ? C7 C17 C14 108.6(4) . . ? C16 C17 C15 107.0(4) . . ? C7 C17 C15 111.4(3) . . ? C14 C17 C15 110.2(4) . . ? C19 C21 C20 110.6(5) . . ? C19 C21 C2 112.6(4) . . ? C20 C21 C2 110.2(4) . . ? C19 C21 C18 107.6(5) . . ? C20 C21 C18 107.3(4) . . ? C2 C21 C18 108.3(4) . . ? O10 C30 C33 102.3(7) . . ? C32 C31 C33 96.6(10) . . ? C31 C32 O10 110.4(9) . . ? C30 C33 C31 106.0(7) . . ? O11 C34 C35 99(3) . 12_664 ? O11 C34 C35 97(2) . . ? C35 C34 C35 67(2) 12_664 . ? C34 C35 C34 112(2) 6_566 . ? C34 C35 C35 58(2) 6_566 6_566 ? C34 C35 C35 104.7(15) . 6_566 ? C34 C35 C35 107.7(19) 6_566 12_664 ? C34 C35 C35 54.7(17) . 12_664 ? C35 C35 C35 60.000(4) 6_566 12_664 ? C36 C36 C36 115.8(11) 22_575 19_657 ? O12 C38 C38 88.5(12) . 18_755 ? O12 C38 C38 88.5(12) . 24_657 ? C38 C38 C38 78(2) 18_755 24_657 ? O12 C38 C38 38.7(10) . 12_664 ? C38 C38 C38 51.2(10) 18_755 12_664 ? C38 C38 C38 90.000(5) 24_657 12_664 ? O12 C38 C38 38.7(10) . 6_566 ? C38 C38 C38 90.000(10) 18_755 6_566 ? C38 C38 C38 51.2(10) 24_657 6_566 ? C38 C38 C38 60.000(3) 12_664 6_566 ? 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 O2 B1 N1 C3 98.5(4) . . . . ? O1 B1 N1 C3 -23.4(5) . . . . ? C13 B1 N1 C3 -138.7(4) 6_566 . . . ? O2 B1 N1 C12 -82.7(4) . . . . ? O1 B1 N1 C12 155.4(3) . . . . ? C13 B1 N1 C12 40.1(5) 6_566 . . . ? O2 B1 O1 C5 -91.3(5) . . . . ? C13 B1 O1 C5 144.2(4) 6_566 . . . ? N1 B1 O1 C5 27.3(5) . . . . ? O1 B1 O2 C22 47.0(5) . . . . ? C13 B1 O2 C22 168.9(4) 6_566 . . . ? N1 B1 O2 C22 -69.7(5) . . . . ? C6 C1 C2 C4 0.8(7) . . . . ? C6 C1 C2 C21 -179.7(4) . . . . ? C12 N1 C3 C6 -170.1(4) . . . . ? B1 N1 C3 C6 8.7(6) . . . . ? C1 C2 C4 C7 -1.7(7) . . . . ? C21 C2 C4 C7 178.8(4) . . . . ? B1 O1 C5 C6 -15.7(6) . . . . ? B1 O1 C5 C7 167.4(4) . . . . ? O1 C5 C6 C1 -178.9(4) . . . . ? C7 C5 C6 C1 -2.1(6) . . . . ? O1 C5 C6 C3 -4.4(6) . . . . ? C7 C5 C6 C3 172.4(4) . . . . ? C2 C1 C6 C5 1.0(7) . . . . ? C2 C1 C6 C3 -173.4(4) . . . . ? N1 C3 C6 C5 6.9(7) . . . . ? N1 C3 C6 C1 -178.5(4) . . . . ? C2 C4 C7 C5 0.7(7) . . . . ? C2 C4 C7 C17 178.1(4) . . . . ? O1 C5 C7 C4 178.1(4) . . . . ? C6 C5 C7 C4 1.2(6) . . . . ? O1 C5 C7 C17 0.6(6) . . . . ? C6 C5 C7 C17 -176.3(4) . . . . ? C12 C8 C9 C10 0.5(7) . . . . ? C8 C9 C10 C13 -0.2(7) . . . . ? C9 C8 C12 C11 -1.0(6) . . . . ? C9 C8 C12 N1 -179.8(4) . . . . ? C13 C11 C12 C8 1.1(6) . . . . ? C13 C11 C12 N1 180.0(4) . . . . ? C3 N1 C12 C8 -132.2(4) . . . . ? B1 N1 C12 C8 49.0(5) . . . . ? C3 N1 C12 C11 49.0(5) . . . . ? B1 N1 C12 C11 -129.8(4) . . . . ? C9 C10 C13 C11 0.2(6) . . . . ? C9 C10 C13 B1 -179.0(4) . . . 12_664 ? C12 C11 C13 C10 -0.7(6) . . . . ? C12 C11 C13 B1 178.6(4) . . . 12_664 ? C4 C7 C17 C16 7.2(6) . . . . ? C5 C7 C17 C16 -175.5(4) . . . . ? C4 C7 C17 C14 -111.7(5) . . . . ? C5 C7 C17 C14 65.6(5) . . . . ? C4 C7 C17 C15 126.8(4) . . . . ? C5 C7 C17 C15 -55.9(5) . . . . ? C1 C2 C21 C19 2.4(7) . . . . ? C4 C2 C21 C19 -178.1(5) . . . . ? C1 C2 C21 C20 -121.6(5) . . . . ? C4 C2 C21 C20 57.8(6) . . . . ? C1 C2 C21 C18 121.3(5) . . . . ? C4 C2 C21 C18 -59.2(6) . . . . ? C32 O10 C30 C33 22.0(10) . . . . ? C33 C31 C32 O10 -23.6(11) . . . . ? C30 O10 C32 C31 2.1(11) . . . . ? O10 C30 C33 C31 -37.6(10) . . . . ? C32 C31 C33 C30 37.0(11) . . . . ? O11 O11 C34 C35 67(6) 6_566 . . 12_664 ? O11 O11 C34 C35 0(6) 12_664 . . 12_664 ? O11 O11 C34 C35 -1(6) 6_566 . . . ? O11 O11 C34 C35 -68(6) 12_664 . . . ? O11 C34 C35 C34 0(3) . . . 6_566 ? C35 C34 C35 C34 -96(2) 12_664 . . 6_566 ? O11 C34 C35 C35 62(3) . . . 6_566 ? C35 C34 C35 C35 -35.1(10) 12_664 . . 6_566 ? O11 C34 C35 C35 97(3) . . . 12_664 ? C38 O12 C38 C38 -91.8(15) 6_566 . . 18_755 ? C38 O12 C38 C38 14(2) 12_664 . . 18_755 ? C38 O12 C38 C38 -14(2) 6_566 . . 24_657 ? C38 O12 C38 C38 91.8(15) 12_664 . . 24_657 ? C38 O12 C38 C38 -106(3) 6_566 . . 12_664 ? C38 O12 C38 C38 106(3) 12_664 . . 6_566 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.668 _refine_diff_density_min -0.483 _refine_diff_density_rms 0.069