# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Paul Kelly' _publ_contact_author_email P.F.KELLY@LBORO.AC.UK _publ_section_title ; Sulfimidation of thioether groups - a versatile method for modifying and linking thia/oxa crowns ; loop_ _publ_author_name 'Paul Kelly' 'Mark Elsegood' 'Gillian Reid' 'A Slawin' 'Paul M Staniland' # Attachment 'kellycif.cif' data_[2a][BPh4] _database_code_depnum_ccdc_archive 'CCDC 678818' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H20 B 1-, C8 H18 N O3 S 1+' _chemical_formula_sum 'C32 H38 B N O3 S' _chemical_formula_weight 527.50 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.9446(3) _cell_length_b 12.0724(3) _cell_length_c 18.1166(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.060(4) _cell_angle_gamma 90.00 _cell_volume 2803.16(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5205 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 26.22 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.149 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.966 _exptl_absorpt_correction_T_max 0.981 _exptl_absorpt_process_details 'SADABS v2007/2, Sheldrick, G.M., (2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 32677 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0241 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 30.56 _reflns_number_total 8548 _reflns_number_gt 7029 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0621P)^2^+0.7336P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom except NH coords freely refined' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8548 _refine_ls_number_parameters 368 _refine_ls_number_restraints 89 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1206 _refine_ls_wR_factor_gt 0.1125 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.67872(10) 0.51862(14) 0.11149(9) 0.0475(3) Uani 1 1 d . . . H1A H 0.7056(16) 0.5311(17) 0.1562(13) 0.057 Uiso 1 1 d . . . H1B H 0.7043(17) 0.5503(18) 0.0786(12) 0.057 Uiso 1 1 d . . . S1 S 0.55219(2) 0.51729(3) 0.094699(16) 0.02647(8) Uani 1 1 d . . . C1 C 0.52204(13) 0.39573(11) 0.14462(8) 0.0376(3) Uani 1 1 d . . . H1C H 0.5702 0.3900 0.1920 0.045 Uiso 1 1 calc R . . H1D H 0.4499 0.4008 0.1566 0.045 Uiso 1 1 calc R . . C2 C 0.53285(11) 0.29372(11) 0.09694(8) 0.0357(3) Uani 1 1 d . A . H2A H 0.6039 0.2918 0.0826 0.043 Uiso 1 1 calc R . . H2B H 0.5238 0.2263 0.1265 0.043 Uiso 1 1 calc R . . O1 O 0.45867(7) 0.29342(8) 0.03215(6) 0.0380(2) Uani 1 1 d DU . . C3 C 0.36791(19) 0.22689(19) 0.01707(17) 0.0313(7) Uani 0.514(4) 1 d PDU A 1 H3A H 0.3838 0.1502 0.0345 0.038 Uiso 0.514(4) 1 calc PR A 1 H3B H 0.3444 0.2247 -0.0373 0.038 Uiso 0.514(4) 1 calc PR A 1 C4 C 0.28281(19) 0.27446(19) 0.05650(17) 0.0299(6) Uani 0.514(4) 1 d PDU A 1 H4A H 0.3087 0.2882 0.1098 0.036 Uiso 0.514(4) 1 calc PR A 1 H4B H 0.2223 0.2236 0.0529 0.036 Uiso 0.514(4) 1 calc PR A 1 O2 O 0.25288(8) 0.38287(9) 0.01580(8) 0.0521(3) Uani 1 1 d DU . . C3X C 0.36610(19) 0.2442(2) 0.06468(17) 0.0302(7) Uani 0.486(4) 1 d PDU A 2 H3C H 0.3751 0.1634 0.0722 0.036 Uiso 0.486(4) 1 calc PR A 2 H3D H 0.3587 0.2793 0.1131 0.036 Uiso 0.486(4) 1 calc PR A 2 C4X C 0.2726(2) 0.2684(2) 0.00801(17) 0.0307(7) Uani 0.486(4) 1 d PDU A 2 H4C H 0.2874 0.2516 -0.0429 0.037 Uiso 0.486(4) 1 calc PR A 2 H4D H 0.2118 0.2238 0.0180 0.037 Uiso 0.486(4) 1 calc PR A 2 C5 C 0.19415(11) 0.43710(14) 0.06607(9) 0.0413(3) Uani 1 1 d . A . H5A H 0.2040 0.3987 0.1148 0.050 Uiso 1 1 calc R . . H5B H 0.1190 0.4354 0.0461 0.050 Uiso 1 1 calc R . . C6 C 0.23073(10) 0.55387(13) 0.07547(8) 0.0359(3) Uani 1 1 d . . . H6A H 0.2301 0.5897 0.0263 0.043 Uiso 1 1 calc R A . H6B H 0.1847 0.5966 0.1043 0.043 Uiso 1 1 calc R . . O3 O 0.33470(8) 0.55016(9) 0.11463(6) 0.0374(2) Uani 1 1 d . A . C7 C 0.38971(11) 0.65031(11) 0.11206(8) 0.0348(3) Uani 1 1 d . . . H7A H 0.3585 0.7084 0.1405 0.042 Uiso 1 1 calc R A . H7B H 0.3871 0.6755 0.0598 0.042 Uiso 1 1 calc R . . C8 C 0.50108(11) 0.62879(11) 0.14604(7) 0.0327(3) Uani 1 1 d . A . H8A H 0.5038 0.6078 0.1991 0.039 Uiso 1 1 calc R . . H8B H 0.5435 0.6965 0.1433 0.039 Uiso 1 1 calc R . . B1 B 0.51509(10) 0.96022(11) 0.25219(8) 0.0243(2) Uani 1 1 d . . . C9 C 0.43557(9) 0.95119(9) 0.17321(7) 0.0256(2) Uani 1 1 d . . . C10 C 0.46884(10) 0.93155(10) 0.10387(7) 0.0270(2) Uani 1 1 d . . . H10 H 0.5414 0.9230 0.1020 0.032 Uiso 1 1 calc R . . C11 C 0.39991(11) 0.92402(10) 0.03743(8) 0.0330(3) Uani 1 1 d . . . H11 H 0.4261 0.9100 -0.0081 0.040 Uiso 1 1 calc R . . C12 C 0.29367(11) 0.93685(11) 0.03755(9) 0.0380(3) Uani 1 1 d . . . H12 H 0.2465 0.9324 -0.0075 0.046 Uiso 1 1 calc R . . C13 C 0.25748(11) 0.95628(11) 0.10491(9) 0.0389(3) Uani 1 1 d . . . H13 H 0.1848 0.9650 0.1060 0.047 Uiso 1 1 calc R . . C14 C 0.32629(10) 0.96313(11) 0.17055(8) 0.0337(3) Uani 1 1 d . . . H14 H 0.2990 0.9764 0.2158 0.040 Uiso 1 1 calc R . . C15 C 0.49215(9) 1.07495(10) 0.29725(7) 0.0260(2) Uani 1 1 d . . . C16 C 0.43086(11) 1.16267(11) 0.26463(7) 0.0319(3) Uani 1 1 d . . . H16 H 0.3977 1.1546 0.2147 0.038 Uiso 1 1 calc R . . C17 C 0.41635(11) 1.26131(11) 0.30209(8) 0.0359(3) Uani 1 1 d . . . H17 H 0.3736 1.3181 0.2777 0.043 Uiso 1 1 calc R . . C18 C 0.46409(11) 1.27648(11) 0.37462(8) 0.0349(3) Uani 1 1 d . . . H18 H 0.4548 1.3435 0.4004 0.042 Uiso 1 1 calc R . . C19 C 0.52534(11) 1.19259(12) 0.40883(8) 0.0361(3) Uani 1 1 d . . . H19 H 0.5589 1.2018 0.4586 0.043 Uiso 1 1 calc R . . C20 C 0.53833(10) 1.09426(11) 0.37076(8) 0.0318(3) Uani 1 1 d . . . H20 H 0.5805 1.0377 0.3959 0.038 Uiso 1 1 calc R . . C21 C 0.63480(9) 0.96485(9) 0.23160(6) 0.0227(2) Uani 1 1 d . . . C22 C 0.68365(10) 1.06530(10) 0.21744(7) 0.0272(2) Uani 1 1 d . . . H22 H 0.6507 1.1330 0.2273 0.033 Uiso 1 1 calc R . . C23 C 0.77889(10) 1.06916(11) 0.18943(7) 0.0299(3) Uani 1 1 d . . . H23 H 0.8091 1.1387 0.1804 0.036 Uiso 1 1 calc R . . C24 C 0.82921(10) 0.97236(11) 0.17480(7) 0.0303(3) Uani 1 1 d . . . H24 H 0.8933 0.9749 0.1549 0.036 Uiso 1 1 calc R . . C25 C 0.78497(9) 0.87117(11) 0.18958(7) 0.0282(2) Uani 1 1 d . . . H25 H 0.8192 0.8040 0.1804 0.034 Uiso 1 1 calc R . . C26 C 0.69022(9) 0.86856(10) 0.21789(6) 0.0240(2) Uani 1 1 d . . . H26 H 0.6619 0.7987 0.2284 0.029 Uiso 1 1 calc R . . C27 C 0.50213(10) 0.85140(10) 0.30535(7) 0.0270(2) Uani 1 1 d . . . C28 C 0.57731(11) 0.82527(11) 0.36665(7) 0.0317(3) Uani 1 1 d . . . H28 H 0.6382 0.8699 0.3759 0.038 Uiso 1 1 calc R . . C29 C 0.56658(13) 0.73668(12) 0.41448(8) 0.0383(3) Uani 1 1 d . . . H29 H 0.6183 0.7238 0.4562 0.046 Uiso 1 1 calc R . . C30 C 0.48066(14) 0.66757(11) 0.40114(9) 0.0435(4) Uani 1 1 d . . . H30 H 0.4731 0.6068 0.4333 0.052 Uiso 1 1 calc R . . C31 C 0.40615(14) 0.68819(12) 0.34050(9) 0.0431(4) Uani 1 1 d . . . H31 H 0.3476 0.6405 0.3301 0.052 Uiso 1 1 calc R . . C32 C 0.41647(12) 0.77894(11) 0.29433(8) 0.0338(3) Uani 1 1 d . . . H32 H 0.3632 0.7923 0.2536 0.041 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0312(6) 0.0713(10) 0.0406(7) -0.0155(7) 0.0069(5) -0.0049(6) S1 0.03145(15) 0.02803(15) 0.01920(13) -0.00180(10) 0.00103(10) -0.00283(11) C1 0.0547(8) 0.0324(7) 0.0276(6) 0.0073(5) 0.0121(6) 0.0069(6) C2 0.0411(7) 0.0277(6) 0.0390(7) 0.0073(5) 0.0082(6) 0.0097(5) O1 0.0290(5) 0.0234(4) 0.0599(6) -0.0027(4) 0.0002(4) -0.0004(4) C3 0.0342(13) 0.0206(11) 0.0396(17) -0.0023(10) 0.0069(11) -0.0043(9) C4 0.0280(12) 0.0249(11) 0.0372(17) 0.0025(10) 0.0055(10) -0.0033(9) O2 0.0325(5) 0.0272(5) 0.1003(10) -0.0051(6) 0.0222(6) 0.0015(4) C3X 0.0359(14) 0.0216(11) 0.0332(16) 0.0047(10) 0.0059(11) -0.0050(10) C4X 0.0345(13) 0.0267(12) 0.0306(16) -0.0054(10) 0.0035(11) -0.0057(10) C5 0.0282(6) 0.0474(8) 0.0495(8) 0.0067(7) 0.0096(6) -0.0036(6) C6 0.0254(6) 0.0410(7) 0.0413(7) -0.0024(6) 0.0051(5) 0.0052(5) O3 0.0301(5) 0.0367(5) 0.0434(5) 0.0081(4) -0.0012(4) -0.0034(4) C7 0.0382(7) 0.0261(6) 0.0393(7) -0.0063(5) 0.0023(6) 0.0015(5) C8 0.0358(6) 0.0299(6) 0.0312(6) -0.0106(5) 0.0010(5) -0.0044(5) B1 0.0258(6) 0.0216(6) 0.0273(6) -0.0004(5) 0.0097(5) -0.0003(5) C9 0.0264(5) 0.0186(5) 0.0327(6) 0.0007(4) 0.0074(4) -0.0018(4) C10 0.0300(6) 0.0216(5) 0.0297(6) 0.0018(4) 0.0049(5) -0.0008(4) C11 0.0424(7) 0.0236(6) 0.0316(6) 0.0028(5) 0.0002(5) -0.0033(5) C12 0.0391(7) 0.0235(6) 0.0470(8) 0.0022(5) -0.0095(6) -0.0064(5) C13 0.0256(6) 0.0261(6) 0.0631(10) 0.0003(6) -0.0002(6) -0.0045(5) C14 0.0280(6) 0.0276(6) 0.0472(8) -0.0021(5) 0.0114(5) -0.0036(5) C15 0.0275(5) 0.0218(5) 0.0316(6) -0.0009(4) 0.0145(5) -0.0014(4) C16 0.0399(7) 0.0256(6) 0.0318(6) 0.0024(5) 0.0110(5) 0.0029(5) C17 0.0430(7) 0.0232(6) 0.0438(7) 0.0036(5) 0.0143(6) 0.0069(5) C18 0.0373(7) 0.0255(6) 0.0451(7) -0.0080(5) 0.0170(6) 0.0021(5) C19 0.0363(7) 0.0353(7) 0.0375(7) -0.0100(6) 0.0081(5) 0.0043(5) C20 0.0318(6) 0.0293(6) 0.0351(6) -0.0042(5) 0.0075(5) 0.0062(5) C21 0.0250(5) 0.0231(5) 0.0205(5) -0.0014(4) 0.0046(4) -0.0013(4) C22 0.0319(6) 0.0231(5) 0.0279(6) 0.0005(4) 0.0083(5) -0.0012(4) C23 0.0319(6) 0.0301(6) 0.0287(6) 0.0021(5) 0.0075(5) -0.0068(5) C24 0.0236(5) 0.0396(7) 0.0289(6) 0.0007(5) 0.0074(4) -0.0020(5) C25 0.0251(5) 0.0310(6) 0.0289(6) -0.0038(5) 0.0047(4) 0.0027(5) C26 0.0250(5) 0.0235(5) 0.0236(5) -0.0024(4) 0.0037(4) -0.0016(4) C27 0.0354(6) 0.0209(5) 0.0281(6) -0.0023(4) 0.0160(5) 0.0020(4) C28 0.0399(7) 0.0248(6) 0.0337(6) 0.0020(5) 0.0166(5) 0.0056(5) C29 0.0531(8) 0.0309(6) 0.0347(7) 0.0063(5) 0.0199(6) 0.0138(6) C30 0.0710(10) 0.0238(6) 0.0424(8) 0.0064(5) 0.0314(7) 0.0043(6) C31 0.0634(10) 0.0273(6) 0.0436(8) -0.0028(6) 0.0252(7) -0.0120(6) C32 0.0474(8) 0.0259(6) 0.0318(6) -0.0040(5) 0.0178(6) -0.0066(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 N1 S1 1.6235(14) . ? S1 C1 1.7952(14) . ? S1 C8 1.8130(13) . ? C1 C2 1.5219(19) . ? C2 O1 1.4085(17) . ? O1 C3 1.418(2) . ? O1 C3X 1.528(3) . ? C3 C4 1.508(3) . ? C4 O2 1.525(3) . ? O2 C4X 1.416(3) . ? O2 C5 1.4248(19) . ? C3X C4X 1.502(4) . ? C5 C6 1.489(2) . ? C6 O3 1.4314(16) . ? O3 C7 1.4072(17) . ? C7 C8 1.5087(19) . ? B1 C9 1.6449(18) . ? B1 C21 1.6449(17) . ? B1 C27 1.6514(18) . ? B1 C15 1.6555(17) . ? C9 C10 1.4041(17) . ? C9 C14 1.4159(17) . ? C10 C11 1.3971(18) . ? C11 C12 1.384(2) . ? C12 C13 1.387(2) . ? C13 C14 1.385(2) . ? C15 C20 1.4006(18) . ? C15 C16 1.4031(18) . ? C16 C17 1.3962(18) . ? C17 C18 1.384(2) . ? C18 C19 1.379(2) . ? C19 C20 1.3949(18) . ? C21 C26 1.4063(16) . ? C21 C22 1.4077(16) . ? C22 C23 1.3982(17) . ? C23 C24 1.3815(19) . ? C24 C25 1.3910(18) . ? C25 C26 1.3946(16) . ? C27 C32 1.4044(18) . ? C27 C28 1.4060(19) . ? C28 C29 1.3956(18) . ? C29 C30 1.384(2) . ? C30 C31 1.379(2) . ? C31 C32 1.3961(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 S1 C1 101.45(9) . . ? N1 S1 C8 109.13(7) . . ? C1 S1 C8 103.16(7) . . ? C2 C1 S1 109.38(9) . . ? O1 C2 C1 111.64(11) . . ? C2 O1 C3 127.72(16) . . ? C2 O1 C3X 99.18(14) . . ? O1 C3 C4 109.5(2) . . ? C3 C4 O2 104.5(2) . . ? C4X O2 C5 129.17(17) . . ? C5 O2 C4 101.97(15) . . ? C4X C3X O1 105.2(2) . . ? O2 C4X C3X 105.1(2) . . ? O2 C5 C6 108.57(12) . . ? O3 C6 C5 106.79(12) . . ? C7 O3 C6 113.69(11) . . ? O3 C7 C8 107.31(11) . . ? C7 C8 S1 108.36(9) . . ? C9 B1 C21 107.43(9) . . ? C9 B1 C27 110.62(10) . . ? C21 B1 C27 109.59(10) . . ? C9 B1 C15 110.54(10) . . ? C21 B1 C15 108.86(9) . . ? C27 B1 C15 109.76(9) . . ? C10 C9 C14 114.65(12) . . ? C10 C9 B1 123.81(11) . . ? C14 C9 B1 121.55(11) . . ? C11 C10 C9 122.88(12) . . ? C12 C11 C10 120.40(13) . . ? C11 C12 C13 118.58(13) . . ? C14 C13 C12 120.65(13) . . ? C13 C14 C9 122.85(13) . . ? C20 C15 C16 114.56(11) . . ? C20 C15 B1 121.73(11) . . ? C16 C15 B1 123.62(11) . . ? C17 C16 C15 123.07(13) . . ? C18 C17 C16 120.12(13) . . ? C19 C18 C17 118.81(12) . . ? C18 C19 C20 120.29(13) . . ? C19 C20 C15 123.15(12) . . ? C26 C21 C22 115.26(10) . . ? C26 C21 B1 122.15(10) . . ? C22 C21 B1 122.15(10) . . ? C23 C22 C21 122.43(11) . . ? C24 C23 C22 120.33(11) . . ? C23 C24 C25 119.20(11) . . ? C24 C25 C26 119.85(11) . . ? C25 C26 C21 122.88(11) . . ? C32 C27 C28 114.70(12) . . ? C32 C27 B1 123.73(12) . . ? C28 C27 B1 121.57(11) . . ? C29 C28 C27 122.97(14) . . ? C30 C29 C28 120.06(14) . . ? C31 C30 C29 119.03(13) . . ? C30 C31 C32 120.26(14) . . ? C31 C32 C27 122.92(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 S1 C1 C2 -82.41(12) . . . . ? C8 S1 C1 C2 164.60(10) . . . . ? S1 C1 C2 O1 -65.10(14) . . . . ? C1 C2 O1 C3 -105.99(18) . . . . ? C1 C2 O1 C3X -83.58(15) . . . . ? C2 O1 C3 C4 79.0(2) . . . . ? C3X O1 C3 C4 38.0(2) . . . . ? O1 C3 C4 O2 68.9(3) . . . . ? C3 C4 O2 C4X 47.9(2) . . . . ? C3 C4 O2 C5 -165.39(18) . . . . ? C2 O1 C3X C4X 164.32(18) . . . . ? C3 O1 C3X C4X -47.4(2) . . . . ? C5 O2 C4X C3X -85.3(2) . . . . ? C4 O2 C4X C3X -41.5(2) . . . . ? O1 C3X C4X O2 -74.6(3) . . . . ? C4X O2 C5 C6 156.79(18) . . . . ? C4 O2 C5 C6 133.28(15) . . . . ? O2 C5 C6 O3 -68.11(15) . . . . ? C5 C6 O3 C7 165.21(12) . . . . ? C6 O3 C7 C8 -172.30(11) . . . . ? O3 C7 C8 S1 57.13(13) . . . . ? N1 S1 C8 C7 161.99(11) . . . . ? C1 S1 C8 C7 -90.73(11) . . . . ? C21 B1 C9 C10 10.00(15) . . . . ? C27 B1 C9 C10 -109.58(12) . . . . ? C15 B1 C9 C10 128.64(11) . . . . ? C21 B1 C9 C14 -169.91(10) . . . . ? C27 B1 C9 C14 70.51(13) . . . . ? C15 B1 C9 C14 -51.27(14) . . . . ? C14 C9 C10 C11 -0.17(17) . . . . ? B1 C9 C10 C11 179.91(11) . . . . ? C9 C10 C11 C12 0.52(19) . . . . ? C10 C11 C12 C13 -0.55(19) . . . . ? C11 C12 C13 C14 0.3(2) . . . . ? C12 C13 C14 C9 0.1(2) . . . . ? C10 C9 C14 C13 -0.13(18) . . . . ? B1 C9 C14 C13 179.79(12) . . . . ? C9 B1 C15 C20 170.33(11) . . . . ? C21 B1 C15 C20 -71.90(14) . . . . ? C27 B1 C15 C20 48.04(15) . . . . ? C9 B1 C15 C16 -13.45(15) . . . . ? C21 B1 C15 C16 104.32(13) . . . . ? C27 B1 C15 C16 -135.74(12) . . . . ? C20 C15 C16 C17 -0.23(18) . . . . ? B1 C15 C16 C17 -176.70(12) . . . . ? C15 C16 C17 C18 0.5(2) . . . . ? C16 C17 C18 C19 -0.3(2) . . . . ? C17 C18 C19 C20 -0.2(2) . . . . ? C18 C19 C20 C15 0.5(2) . . . . ? C16 C15 C20 C19 -0.28(19) . . . . ? B1 C15 C20 C19 176.26(12) . . . . ? C9 B1 C21 C26 -83.23(13) . . . . ? C27 B1 C21 C26 37.01(15) . . . . ? C15 B1 C21 C26 157.05(11) . . . . ? C9 B1 C21 C22 88.69(13) . . . . ? C27 B1 C21 C22 -151.07(11) . . . . ? C15 B1 C21 C22 -31.03(15) . . . . ? C26 C21 C22 C23 1.99(18) . . . . ? B1 C21 C22 C23 -170.44(11) . . . . ? C21 C22 C23 C24 -0.3(2) . . . . ? C22 C23 C24 C25 -1.20(19) . . . . ? C23 C24 C25 C26 0.84(19) . . . . ? C24 C25 C26 C21 1.02(19) . . . . ? C22 C21 C26 C25 -2.37(17) . . . . ? B1 C21 C26 C25 170.07(11) . . . . ? C9 B1 C27 C32 -16.60(15) . . . . ? C21 B1 C27 C32 -134.87(12) . . . . ? C15 B1 C27 C32 105.64(13) . . . . ? C9 B1 C27 C28 164.18(10) . . . . ? C21 B1 C27 C28 45.91(14) . . . . ? C15 B1 C27 C28 -73.58(13) . . . . ? C32 C27 C28 C29 -2.04(17) . . . . ? B1 C27 C28 C29 177.25(11) . . . . ? C27 C28 C29 C30 2.23(19) . . . . ? C28 C29 C30 C31 -0.4(2) . . . . ? C29 C30 C31 C32 -1.3(2) . . . . ? C30 C31 C32 C27 1.5(2) . . . . ? C28 C27 C32 C31 0.19(18) . . . . ? B1 C27 C32 C31 -179.08(12) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1B O2 0.82(2) 2.04(2) 2.844(2) 170(2) 3_665 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.56 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.524 _refine_diff_density_min -0.303 _refine_diff_density_rms 0.046 #===END data_[3b][BPh4] _database_code_depnum_ccdc_archive 'CCDC 678819' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H68 B2 N2 O4 S2' _chemical_formula_sum 'C60 H68 B2 N2 O4 S2' _chemical_formula_weight 966.90 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.854(3) _cell_length_b 12.341(3) _cell_length_c 16.969(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.861(10) _cell_angle_gamma 90.00 _cell_volume 2547.2(11) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 6847 _cell_measurement_theta_min 1.48 _cell_measurement_theta_max 26.01 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.261 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 0.155 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9389 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14321 _diffrn_reflns_av_R_equivalents 0.1030 _diffrn_reflns_av_sigmaI/netI 0.0822 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 25.35 _reflns_number_total 4600 _reflns_number_gt 3098 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _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. The ammine hydrogen atoms are refined subject to a DFIX constraint. ; _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^)+(0.0964P)^2^+4.7928P] 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 4600 _refine_ls_number_parameters 325 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1302 _refine_ls_R_factor_gt 0.0849 _refine_ls_wR_factor_ref 0.2254 _refine_ls_wR_factor_gt 0.1967 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.037 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.4074(3) 0.0630(3) 0.5727(2) 0.0414(9) Uani 1 1 d D . . H1A H 0.393(4) 0.019(4) 0.5222(19) 0.064(17) Uiso 1 1 d D . . H1B H 0.461(4) 0.061(6) 0.6288(17) 0.10(2) Uiso 1 1 d D . . S1 S 0.39592(10) 0.19042(10) 0.54751(8) 0.0430(4) Uani 1 1 d . . . C2 C 0.2506(4) 0.2081(4) 0.4930(3) 0.0494(13) Uani 1 1 d . . . H2A H 0.2147 0.2341 0.5330 0.059 Uiso 1 1 calc R . . H2B H 0.2412 0.2647 0.4499 0.059 Uiso 1 1 calc R . . C3 C 0.1935(4) 0.1061(4) 0.4519(3) 0.0432(12) Uani 1 1 d . . . H3A H 0.1928 0.0520 0.4948 0.052 Uiso 1 1 calc R . . H3B H 0.1165 0.1225 0.4184 0.052 Uiso 1 1 calc R . . O4 O 0.2507(3) 0.0642(3) 0.4001(2) 0.0449(8) Uani 1 1 d . . . C5 C 0.2149(4) -0.0394(4) 0.3670(3) 0.0449(12) Uani 1 1 d . . . H5A H 0.2396 -0.0515 0.3181 0.054 Uiso 1 1 calc R . . H5B H 0.1335 -0.0403 0.3470 0.054 Uiso 1 1 calc R . . C6 C 0.2548(4) -0.1307(4) 0.4262(3) 0.0388(11) Uani 1 1 d . . . H6A H 0.2241 -0.1248 0.4726 0.047 Uiso 1 1 calc R . . H6B H 0.2310 -0.2006 0.3974 0.047 Uiso 1 1 calc R . . O7 O 0.3745(2) -0.1255(2) 0.45830(19) 0.0413(8) Uani 1 1 d . . . C8 C 0.4216(4) -0.2199(4) 0.4998(3) 0.0469(12) Uani 1 1 d . . . H8A H 0.4030 -0.2818 0.4606 0.056 Uiso 1 1 calc R . . H8B H 0.3913 -0.2348 0.5454 0.056 Uiso 1 1 calc R . . C9 C 0.5453(4) -0.2080(4) 0.5352(3) 0.0463(12) Uani 1 1 d . . . H9A H 0.5771 -0.2733 0.5681 0.056 Uiso 1 1 calc R . . H9B H 0.5638 -0.1445 0.5729 0.056 Uiso 1 1 calc R . . B10 B 0.2496(3) 0.0189(3) 0.7624(3) 0.0217(9) Uani 1 1 d . . . C11 C 0.2453(3) 0.0269(3) 0.8586(2) 0.0203(8) Uani 1 1 d . . . C12 C 0.3359(3) 0.0081(3) 0.9296(2) 0.0253(8) Uani 1 1 d . . . H12A H 0.4056 -0.0030 0.9227 0.030 Uiso 1 1 calc R . . C13 C 0.3294(3) 0.0049(4) 1.0089(3) 0.0331(10) Uani 1 1 d . . . H13A H 0.3938 -0.0084 1.0548 0.040 Uiso 1 1 calc R . . C14 C 0.2298(3) 0.0207(3) 1.0225(3) 0.0318(10) Uani 1 1 d . . . H14A H 0.2250 0.0184 1.0771 0.038 Uiso 1 1 calc R . . C15 C 0.1377(3) 0.0401(3) 0.9544(3) 0.0302(9) Uani 1 1 d . . . H15A H 0.0684 0.0507 0.9621 0.036 Uiso 1 1 calc R . . C16 C 0.1457(3) 0.0442(3) 0.8750(2) 0.0282(9) Uani 1 1 d . . . H16A H 0.0813 0.0593 0.8295 0.034 Uiso 1 1 calc R . . C17 C 0.1707(3) 0.1151(3) 0.7045(2) 0.0254(9) Uani 1 1 d . . . C18 C 0.1766(3) 0.2233(3) 0.7312(3) 0.0333(10) Uani 1 1 d . . . H18A H 0.2260 0.2413 0.7847 0.040 Uiso 1 1 calc R . . C19 C 0.1133(4) 0.3050(4) 0.6829(3) 0.0399(11) Uani 1 1 d . . . H19A H 0.1205 0.3774 0.7031 0.048 Uiso 1 1 calc R . . C20 C 0.0393(4) 0.2812(4) 0.6048(3) 0.0417(12) Uani 1 1 d . . . H20A H -0.0041 0.3368 0.5711 0.050 Uiso 1 1 calc R . . C21 C 0.0300(3) 0.1754(4) 0.5772(3) 0.0371(11) Uani 1 1 d . . . H21A H -0.0209 0.1576 0.5242 0.045 Uiso 1 1 calc R . . C22 C 0.0947(3) 0.0947(3) 0.6265(2) 0.0291(9) Uani 1 1 d . . . H22A H 0.0866 0.0225 0.6060 0.035 Uiso 1 1 calc R . . C23 C 0.3781(3) 0.0334(3) 0.7657(2) 0.0225(8) Uani 1 1 d . . . C24 C 0.4293(3) 0.1327(4) 0.7645(3) 0.0353(10) Uani 1 1 d . . . H24A H 0.3867 0.1969 0.7592 0.042 Uiso 1 1 calc R . . C25 C 0.5388(4) 0.1426(4) 0.7707(3) 0.0428(12) Uani 1 1 d . . . H25A H 0.5700 0.2126 0.7715 0.051 Uiso 1 1 calc R . . C26 C 0.6031(3) 0.0521(4) 0.7756(3) 0.0389(11) Uani 1 1 d . . . H26A H 0.6774 0.0586 0.7770 0.047 Uiso 1 1 calc R . . C27 C 0.5574(3) -0.0482(4) 0.7784(3) 0.0372(11) Uani 1 1 d . . . H27A H 0.6005 -0.1118 0.7826 0.045 Uiso 1 1 calc R . . C28 C 0.4485(3) -0.0564(3) 0.7751(3) 0.0309(9) Uani 1 1 d . . . H28A H 0.4199 -0.1264 0.7794 0.037 Uiso 1 1 calc R . . C29 C 0.2027(3) -0.1003(3) 0.7236(2) 0.0221(8) Uani 1 1 d . . . C30 C 0.2264(3) -0.1443(3) 0.6552(2) 0.0255(9) Uani 1 1 d . . . H30A H 0.2718 -0.1038 0.6315 0.031 Uiso 1 1 calc R . . C31 C 0.1869(3) -0.2438(3) 0.6202(2) 0.0278(9) Uani 1 1 d . . . H31A H 0.2070 -0.2710 0.5747 0.033 Uiso 1 1 calc R . . C32 C 0.1180(3) -0.3036(3) 0.6519(3) 0.0313(9) Uani 1 1 d . . . H32A H 0.0905 -0.3719 0.6285 0.038 Uiso 1 1 calc R . . C33 C 0.0903(3) -0.2623(3) 0.7177(3) 0.0343(10) Uani 1 1 d . . . H33A H 0.0422 -0.3017 0.7395 0.041 Uiso 1 1 calc R . . C34 C 0.1321(3) -0.1634(3) 0.7525(2) 0.0278(9) Uani 1 1 d . . . H34A H 0.1119 -0.1371 0.7981 0.033 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.051(2) 0.042(2) 0.033(2) 0.0059(19) 0.0166(18) 0.0010(18) S1 0.0530(7) 0.0384(7) 0.0444(7) 0.0052(5) 0.0250(6) 0.0045(5) C2 0.050(3) 0.050(3) 0.059(3) 0.012(3) 0.033(3) 0.012(2) C3 0.040(3) 0.049(3) 0.048(3) 0.005(2) 0.024(2) 0.012(2) O4 0.0493(19) 0.048(2) 0.0418(18) 0.0039(16) 0.0211(15) 0.0046(15) C5 0.050(3) 0.055(3) 0.036(3) -0.001(2) 0.022(2) 0.000(2) C6 0.040(2) 0.042(3) 0.038(2) -0.008(2) 0.017(2) -0.008(2) O7 0.0400(17) 0.0385(18) 0.0465(18) 0.0016(15) 0.0158(14) -0.0030(14) C8 0.045(3) 0.042(3) 0.060(3) 0.001(2) 0.026(2) 0.004(2) C9 0.056(3) 0.043(3) 0.049(3) 0.017(2) 0.029(2) 0.013(2) B10 0.022(2) 0.021(2) 0.023(2) 0.0038(18) 0.0080(17) 0.0024(17) C11 0.0239(19) 0.0119(18) 0.0258(19) 0.0017(15) 0.0089(15) 0.0002(14) C12 0.0228(19) 0.028(2) 0.028(2) 0.0026(17) 0.0110(16) 0.0039(15) C13 0.027(2) 0.040(3) 0.031(2) 0.0056(19) 0.0074(17) 0.0081(18) C14 0.035(2) 0.037(2) 0.027(2) 0.0017(19) 0.0157(18) 0.0046(18) C15 0.0223(19) 0.037(2) 0.034(2) -0.0030(19) 0.0128(17) 0.0011(17) C16 0.0233(19) 0.036(2) 0.025(2) 0.0009(18) 0.0073(16) 0.0050(17) C17 0.0226(19) 0.029(2) 0.030(2) 0.0074(17) 0.0147(16) 0.0044(16) C18 0.037(2) 0.029(2) 0.038(2) 0.0050(19) 0.0174(19) 0.0051(18) C19 0.048(3) 0.031(2) 0.052(3) 0.009(2) 0.032(2) 0.010(2) C20 0.045(3) 0.043(3) 0.049(3) 0.028(2) 0.031(2) 0.023(2) C21 0.029(2) 0.053(3) 0.033(2) 0.015(2) 0.0137(18) 0.011(2) C22 0.024(2) 0.034(2) 0.032(2) 0.0087(19) 0.0119(17) 0.0026(17) C23 0.0258(19) 0.024(2) 0.0187(18) 0.0001(16) 0.0079(15) 0.0007(16) C24 0.031(2) 0.030(2) 0.042(2) 0.003(2) 0.0081(19) -0.0056(18) C25 0.036(2) 0.045(3) 0.043(3) 0.016(2) 0.006(2) -0.017(2) C26 0.026(2) 0.064(3) 0.027(2) 0.007(2) 0.0099(17) -0.009(2) C27 0.027(2) 0.048(3) 0.035(2) -0.015(2) 0.0083(18) 0.0029(19) C28 0.025(2) 0.028(2) 0.039(2) -0.0101(19) 0.0093(17) -0.0043(16) C29 0.0173(18) 0.025(2) 0.0221(19) 0.0022(16) 0.0039(15) 0.0015(15) C30 0.0219(19) 0.028(2) 0.0256(19) 0.0047(17) 0.0065(15) -0.0008(16) C31 0.023(2) 0.034(2) 0.024(2) -0.0022(18) 0.0047(16) 0.0037(16) C32 0.024(2) 0.025(2) 0.039(2) -0.0033(19) 0.0031(18) -0.0044(16) C33 0.032(2) 0.030(2) 0.044(3) -0.001(2) 0.0160(19) -0.0093(18) C34 0.027(2) 0.032(2) 0.028(2) -0.0009(18) 0.0122(16) -0.0006(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 S1 1.624(4) . ? N1 H1A 0.980(3) . ? N1 H1B 0.980(3) . ? S1 C2 1.810(5) . ? S1 C9 1.809(5) 3_656 ? C2 C3 1.509(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O4 1.414(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? O4 C5 1.413(6) . ? C5 C6 1.486(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O7 1.458(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O7 C8 1.394(6) . ? C8 C9 1.515(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 S1 1.809(5) 3_656 ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? B10 C23 1.643(5) . ? B10 C29 1.645(6) . ? B10 C11 1.655(5) . ? B10 C17 1.660(5) . ? C11 C12 1.399(5) . ? C11 C16 1.410(5) . ? C12 C13 1.375(6) . ? C12 H12A 0.9500 . ? C13 C14 1.387(5) . ? C13 H13A 0.9500 . ? C14 C15 1.381(6) . ? C14 H14A 0.9500 . ? C15 C16 1.386(5) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 C22 1.392(6) . ? C17 C18 1.405(6) . ? C18 C19 1.386(6) . ? C18 H18A 0.9500 . ? C19 C20 1.390(7) . ? C19 H19A 0.9500 . ? C20 C21 1.380(7) . ? C20 H20A 0.9500 . ? C21 C22 1.390(6) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C24 1.395(5) . ? C23 C28 1.407(5) . ? C24 C25 1.383(6) . ? C24 H24A 0.9500 . ? C25 C26 1.377(7) . ? C25 H25A 0.9500 . ? C26 C27 1.377(6) . ? C26 H26A 0.9500 . ? C27 C28 1.387(6) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C34 1.399(5) . ? C29 C30 1.401(5) . ? C30 C31 1.387(6) . ? C30 H30A 0.9500 . ? C31 C32 1.387(6) . ? C31 H31A 0.9500 . ? C32 C33 1.376(6) . ? C32 H32A 0.9500 . ? C33 C34 1.386(6) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? 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 S1 N1 H1A 109(3) . . ? S1 N1 H1B 105(4) . . ? H1A N1 H1B 135(5) . . ? N1 S1 C2 104.0(2) . . ? N1 S1 C9 107.2(2) . 3_656 ? C2 S1 C9 102.1(2) . 3_656 ? C3 C2 S1 113.8(3) . . ? C3 C2 H2A 108.8 . . ? S1 C2 H2A 108.8 . . ? C3 C2 H2B 108.8 . . ? S1 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? O4 C3 C2 108.6(4) . . ? O4 C3 H3A 110.0 . . ? C2 C3 H3A 110.0 . . ? O4 C3 H3B 110.0 . . ? C2 C3 H3B 110.0 . . ? H3A C3 H3B 108.4 . . ? C5 O4 C3 114.2(3) . . ? O4 C5 C6 114.9(4) . . ? O4 C5 H5A 108.6 . . ? C6 C5 H5A 108.6 . . ? O4 C5 H5B 108.6 . . ? C6 C5 H5B 108.6 . . ? H5A C5 H5B 107.5 . . ? O7 C6 C5 108.1(4) . . ? O7 C6 H6A 110.1 . . ? C5 C6 H6A 110.1 . . ? O7 C6 H6B 110.1 . . ? C5 C6 H6B 110.1 . . ? H6A C6 H6B 108.4 . . ? C8 O7 C6 112.7(3) . . ? O7 C8 C9 110.4(4) . . ? O7 C8 H8A 109.6 . . ? C9 C8 H8A 109.6 . . ? O7 C8 H8B 109.6 . . ? C9 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C8 C9 S1 110.6(4) . 3_656 ? C8 C9 H9A 109.5 . . ? S1 C9 H9A 109.5 3_656 . ? C8 C9 H9B 109.5 . . ? S1 C9 H9B 109.5 3_656 . ? H9A C9 H9B 108.1 . . ? C23 B10 C29 110.2(3) . . ? C23 B10 C11 108.3(3) . . ? C29 B10 C11 108.8(3) . . ? C23 B10 C17 111.0(3) . . ? C29 B10 C17 109.2(3) . . ? C11 B10 C17 109.4(3) . . ? C12 C11 C16 114.3(3) . . ? C12 C11 B10 123.8(3) . . ? C16 C11 B10 121.7(3) . . ? C13 C12 C11 123.4(3) . . ? C13 C12 H12A 118.3 . . ? C11 C12 H12A 118.3 . . ? C12 C13 C14 120.7(4) . . ? C12 C13 H13A 119.7 . . ? C14 C13 H13A 119.7 . . ? C15 C14 C13 118.3(4) . . ? C15 C14 H14A 120.9 . . ? C13 C14 H14A 120.9 . . ? C14 C15 C16 120.4(4) . . ? C14 C15 H15A 119.8 . . ? C16 C15 H15A 119.8 . . ? C15 C16 C11 122.9(4) . . ? C15 C16 H16A 118.5 . . ? C11 C16 H16A 118.5 . . ? C22 C17 C18 115.3(4) . . ? C22 C17 B10 122.7(3) . . ? C18 C17 B10 122.0(3) . . ? C19 C18 C17 122.7(4) . . ? C19 C18 H18A 118.6 . . ? C17 C18 H18A 118.6 . . ? C18 C19 C20 120.1(4) . . ? C18 C19 H19A 120.0 . . ? C20 C19 H19A 120.0 . . ? C21 C20 C19 118.8(4) . . ? C21 C20 H20A 120.6 . . ? C19 C20 H20A 120.6 . . ? C20 C21 C22 120.2(4) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? C21 C22 C17 122.9(4) . . ? C21 C22 H22A 118.5 . . ? C17 C22 H22A 118.5 . . ? C24 C23 C28 113.9(3) . . ? C24 C23 B10 124.6(3) . . ? C28 C23 B10 121.4(3) . . ? C25 C24 C23 123.4(4) . . ? C25 C24 H24A 118.3 . . ? C23 C24 H24A 118.3 . . ? C26 C25 C24 120.6(4) . . ? C26 C25 H25A 119.7 . . ? C24 C25 H25A 119.7 . . ? C25 C26 C27 118.5(4) . . ? C25 C26 H26A 120.8 . . ? C27 C26 H26A 120.8 . . ? C26 C27 C28 120.0(4) . . ? C26 C27 H27A 120.0 . . ? C28 C27 H27A 120.0 . . ? C27 C28 C23 123.4(4) . . ? C27 C28 H28A 118.3 . . ? C23 C28 H28A 118.3 . . ? C34 C29 C30 114.5(3) . . ? C34 C29 B10 123.6(3) . . ? C30 C29 B10 121.8(3) . . ? C31 C30 C29 123.3(4) . . ? C31 C30 H30A 118.3 . . ? C29 C30 H30A 118.3 . . ? C32 C31 C30 119.8(4) . . ? C32 C31 H31A 120.1 . . ? C30 C31 H31A 120.1 . . ? C33 C32 C31 118.9(4) . . ? C33 C32 H32A 120.6 . . ? C31 C32 H32A 120.6 . . ? C32 C33 C34 120.4(4) . . ? C32 C33 H33A 119.8 . . ? C34 C33 H33A 119.8 . . ? C33 C34 C29 123.1(4) . . ? C33 C34 H34A 118.4 . . ? C29 C34 H34A 118.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 S1 C2 C3 -26.5(4) . . . . ? C9 S1 C2 C3 84.9(4) 3_656 . . . ? S1 C2 C3 O4 -53.7(5) . . . . ? C2 C3 O4 C5 171.6(4) . . . . ? C3 O4 C5 C6 -77.4(5) . . . . ? O4 C5 C6 O7 -55.6(5) . . . . ? C5 C6 O7 C8 -166.7(4) . . . . ? C6 O7 C8 C9 -177.4(4) . . . . ? O7 C8 C9 S1 -63.4(5) . . . 3_656 ? C23 B10 C11 C12 -21.6(5) . . . . ? C29 B10 C11 C12 98.2(4) . . . . ? C17 B10 C11 C12 -142.6(3) . . . . ? C23 B10 C11 C16 164.2(3) . . . . ? C29 B10 C11 C16 -76.1(4) . . . . ? C17 B10 C11 C16 43.1(5) . . . . ? C16 C11 C12 C13 1.0(6) . . . . ? B10 C11 C12 C13 -173.7(4) . . . . ? C11 C12 C13 C14 -0.1(6) . . . . ? C12 C13 C14 C15 -0.2(6) . . . . ? C13 C14 C15 C16 -0.5(6) . . . . ? C14 C15 C16 C11 1.5(6) . . . . ? C12 C11 C16 C15 -1.6(6) . . . . ? B10 C11 C16 C15 173.1(4) . . . . ? C23 B10 C17 C22 108.4(4) . . . . ? C29 B10 C17 C22 -13.2(5) . . . . ? C11 B10 C17 C22 -132.2(4) . . . . ? C23 B10 C17 C18 -71.4(4) . . . . ? C29 B10 C17 C18 167.0(3) . . . . ? C11 B10 C17 C18 48.0(4) . . . . ? C22 C17 C18 C19 -1.5(6) . . . . ? B10 C17 C18 C19 178.4(3) . . . . ? C17 C18 C19 C20 0.8(6) . . . . ? C18 C19 C20 C21 0.4(6) . . . . ? C19 C20 C21 C22 -0.8(6) . . . . ? C20 C21 C22 C17 0.0(6) . . . . ? C18 C17 C22 C21 1.1(5) . . . . ? B10 C17 C22 C21 -178.7(3) . . . . ? C29 B10 C23 C24 154.7(4) . . . . ? C11 B10 C23 C24 -86.4(4) . . . . ? C17 B10 C23 C24 33.6(5) . . . . ? C29 B10 C23 C28 -29.1(5) . . . . ? C11 B10 C23 C28 89.8(4) . . . . ? C17 B10 C23 C28 -150.1(4) . . . . ? C28 C23 C24 C25 0.9(6) . . . . ? B10 C23 C24 C25 177.4(4) . . . . ? C23 C24 C25 C26 2.3(7) . . . . ? C24 C25 C26 C27 -3.2(7) . . . . ? C25 C26 C27 C28 0.9(6) . . . . ? C26 C27 C28 C23 2.5(6) . . . . ? C24 C23 C28 C27 -3.3(6) . . . . ? B10 C23 C28 C27 -179.9(4) . . . . ? C23 B10 C29 C34 142.0(3) . . . . ? C11 B10 C29 C34 23.4(5) . . . . ? C17 B10 C29 C34 -95.9(4) . . . . ? C23 B10 C29 C30 -41.6(4) . . . . ? C11 B10 C29 C30 -160.2(3) . . . . ? C17 B10 C29 C30 80.5(4) . . . . ? C34 C29 C30 C31 -2.3(5) . . . . ? B10 C29 C30 C31 -179.0(3) . . . . ? C29 C30 C31 C32 1.7(6) . . . . ? C30 C31 C32 C33 0.0(6) . . . . ? C31 C32 C33 C34 -1.0(6) . . . . ? C32 C33 C34 C29 0.4(6) . . . . ? C30 C29 C34 C33 1.2(5) . . . . ? B10 C29 C34 C33 177.9(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O4 0.980(3) 2.34(5) 2.971(5) 121(4) . N1 H1A O7 0.980(3) 2.06(5) 2.972(5) 154(5) . _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.132 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.081 #===END data_[4][BPh4] _database_code_depnum_ccdc_archive 'CCDC 678820' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H44 B N O4 S2' _chemical_formula_sum 'C36 H44 B N O4 S2' _chemical_formula_weight 629.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.7110(11) _cell_length_b 27.872(2) _cell_length_c 11.0118(12) _cell_angle_alpha 90.00 _cell_angle_beta 101.127(3) _cell_angle_gamma 90.00 _cell_volume 3225.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 11130 _cell_measurement_theta_min 1.9394 _cell_measurement_theta_max 25.3491 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.1500 _exptl_crystal_size_mid 0.1500 _exptl_crystal_size_min 0.1500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 0.206 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9751 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20502 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.35 _reflns_number_total 5821 _reflns_number_gt 5155 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _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^)+(0.0424P)^2^+1.8371P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5821 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0926 _refine_ls_wR_factor_gt 0.0885 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.68399(14) 0.16563(5) 0.48769(13) 0.0239(3) Uani 1 1 d . . . S1 S 0.69545(4) 0.107090(14) 0.47452(4) 0.01767(11) Uani 1 1 d . . . C2 C 0.60782(16) 0.08807(7) 0.59073(16) 0.0231(4) Uani 1 1 d . . . H2A H 0.6354 0.1076 0.6662 0.028 Uiso 1 1 calc R . . H2B H 0.5162 0.0944 0.5601 0.028 Uiso 1 1 calc R . . C3 C 0.62516(17) 0.03530(7) 0.62474(17) 0.0261(4) Uani 1 1 d . . . H3A H 0.5612 0.0261 0.6745 0.031 Uiso 1 1 calc R . . H3B H 0.6087 0.0160 0.5479 0.031 Uiso 1 1 calc R . . O4 O 0.74744(11) 0.02404(4) 0.69206(11) 0.0224(3) Uani 1 1 d . . . C5 C 0.77739(17) 0.04245(6) 0.81511(16) 0.0238(4) Uani 1 1 d . . . H5A H 0.7961 0.0156 0.8747 0.029 Uiso 1 1 calc R . . H5B H 0.7037 0.0604 0.8338 0.029 Uiso 1 1 calc R . . C6 C 0.89106(18) 0.07510(6) 0.82802(17) 0.0261(4) Uani 1 1 d . . . H6A H 0.9212 0.0830 0.9165 0.031 Uiso 1 1 calc R . . H6B H 0.9608 0.0584 0.7981 0.031 Uiso 1 1 calc R . . O7 O 0.86021(11) 0.11844(4) 0.75891(11) 0.0231(3) Uani 1 1 d . . . C8 C 0.91753(16) 0.12450(6) 0.65407(16) 0.0221(4) Uani 1 1 d . . . H8A H 1.0089 0.1164 0.6781 0.027 Uiso 1 1 calc R . . H8B H 0.9117 0.1588 0.6302 0.027 Uiso 1 1 calc R . . C9 C 0.85998(15) 0.09462(6) 0.54139(15) 0.0182(3) Uani 1 1 d . . . H9A H 0.8673 0.0603 0.5651 0.022 Uiso 1 1 calc R . . H9B H 0.9114 0.0996 0.4768 0.022 Uiso 1 1 calc R . . S11 S 0.63036(4) 0.192120(14) 0.35429(4) 0.01893(11) Uani 1 1 d . . . C12 C 0.72855(16) 0.24502(6) 0.37980(17) 0.0227(4) Uani 1 1 d . . . H12A H 0.7259 0.2576 0.4633 0.027 Uiso 1 1 calc R . . H12B H 0.8175 0.2355 0.3794 0.027 Uiso 1 1 calc R . . C13 C 0.69261(18) 0.28529(7) 0.28708(17) 0.0267(4) Uani 1 1 d . . . H13A H 0.7616 0.3095 0.3001 0.032 Uiso 1 1 calc R . . H13B H 0.6861 0.2721 0.2026 0.032 Uiso 1 1 calc R . . O14 O 0.57575(12) 0.30856(4) 0.29485(11) 0.0263(3) Uani 1 1 d . . . C15 C 0.57798(18) 0.33558(6) 0.40533(17) 0.0258(4) Uani 1 1 d . . . H15A H 0.5548 0.3693 0.3834 0.031 Uiso 1 1 calc R . . H15B H 0.6652 0.3353 0.4556 0.031 Uiso 1 1 calc R . . C16 C 0.48665(17) 0.31530(6) 0.48086(18) 0.0255(4) Uani 1 1 d . . . H16A H 0.4766 0.3384 0.5465 0.031 Uiso 1 1 calc R . . H16B H 0.4023 0.3106 0.4269 0.031 Uiso 1 1 calc R . . O17 O 0.53111(11) 0.27050(4) 0.53620(11) 0.0225(3) Uani 1 1 d . . . C18 C 0.45606(16) 0.22989(6) 0.49091(17) 0.0231(4) Uani 1 1 d . . . H18A H 0.3653 0.2379 0.4872 0.028 Uiso 1 1 calc R . . H18B H 0.4781 0.2032 0.5505 0.028 Uiso 1 1 calc R . . C19 C 0.47268(16) 0.21292(6) 0.36398(16) 0.0215(4) Uani 1 1 d . . . H19A H 0.4500 0.2397 0.3046 0.026 Uiso 1 1 calc R . . H19B H 0.4116 0.1865 0.3374 0.026 Uiso 1 1 calc R . . B20 B 0.12930(17) 0.12272(7) 0.30481(16) 0.0155(4) Uani 1 1 d . . . C21 C -0.01010(15) 0.10035(6) 0.23935(14) 0.0150(3) Uani 1 1 d . . . C22 C -0.12594(15) 0.12498(6) 0.22179(15) 0.0182(3) Uani 1 1 d . . . H22A H -0.1261 0.1575 0.2480 0.022 Uiso 1 1 calc R . . C23 C -0.24128(16) 0.10388(6) 0.16749(15) 0.0207(4) Uani 1 1 d . . . H23A H -0.3179 0.1218 0.1589 0.025 Uiso 1 1 calc R . . C24 C -0.24469(16) 0.05700(6) 0.12604(15) 0.0204(4) Uani 1 1 d . . . H24A H -0.3230 0.0426 0.0886 0.025 Uiso 1 1 calc R . . C25 C -0.13211(16) 0.03144(6) 0.14002(15) 0.0187(4) Uani 1 1 d . . . H25A H -0.1328 -0.0008 0.1118 0.022 Uiso 1 1 calc R . . C26 C -0.01822(15) 0.05279(6) 0.19519(14) 0.0167(3) Uani 1 1 d . . . H26A H 0.0578 0.0345 0.2036 0.020 Uiso 1 1 calc R . . C27 C 0.17523(15) 0.10007(6) 0.44534(14) 0.0149(3) Uani 1 1 d . . . C28 C 0.14295(15) 0.05367(6) 0.47894(15) 0.0173(3) Uani 1 1 d . . . H28A H 0.0862 0.0351 0.4203 0.021 Uiso 1 1 calc R . . C29 C 0.19060(16) 0.03380(6) 0.59454(15) 0.0203(4) Uani 1 1 d . . . H29A H 0.1665 0.0022 0.6128 0.024 Uiso 1 1 calc R . . C30 C 0.27286(16) 0.05968(6) 0.68322(15) 0.0212(4) Uani 1 1 d . . . H30A H 0.3062 0.0460 0.7618 0.025 Uiso 1 1 calc R . . C31 C 0.30567(16) 0.10589(6) 0.65506(15) 0.0213(4) Uani 1 1 d . . . H31A H 0.3609 0.1244 0.7151 0.026 Uiso 1 1 calc R . . C32 C 0.25748(15) 0.12522(6) 0.53838(15) 0.0183(3) Uani 1 1 d . . . H32A H 0.2816 0.1569 0.5212 0.022 Uiso 1 1 calc R . . C33 C 0.23066(15) 0.10538(5) 0.21785(15) 0.0154(3) Uani 1 1 d . . . C34 C 0.34946(15) 0.08459(6) 0.26297(15) 0.0174(3) Uani 1 1 d . . . H34A H 0.3780 0.0824 0.3500 0.021 Uiso 1 1 calc R . . C35 C 0.42785(16) 0.06701(6) 0.18566(16) 0.0215(4) Uani 1 1 d . . . H35A H 0.5078 0.0532 0.2204 0.026 Uiso 1 1 calc R . . C36 C 0.38913(17) 0.06971(6) 0.05820(16) 0.0225(4) Uani 1 1 d . . . H36A H 0.4411 0.0571 0.0050 0.027 Uiso 1 1 calc R . . C37 C 0.27334(17) 0.09115(6) 0.00957(16) 0.0225(4) Uani 1 1 d . . . H37A H 0.2462 0.0938 -0.0775 0.027 Uiso 1 1 calc R . . C38 C 0.19732(16) 0.10870(6) 0.08810(15) 0.0187(4) Uani 1 1 d . . . H38A H 0.1191 0.1237 0.0527 0.022 Uiso 1 1 calc R . . C39 C 0.12266(14) 0.18156(6) 0.31222(15) 0.0161(3) Uani 1 1 d . . . C40 C 0.16773(16) 0.21256(6) 0.23000(15) 0.0190(4) Uani 1 1 d . . . H40A H 0.2037 0.1990 0.1655 0.023 Uiso 1 1 calc R . . C41 C 0.16221(17) 0.26233(6) 0.23865(16) 0.0239(4) Uani 1 1 d . . . H41A H 0.1943 0.2818 0.1809 0.029 Uiso 1 1 calc R . . C42 C 0.10999(17) 0.28346(6) 0.33132(16) 0.0243(4) Uani 1 1 d . . . H42A H 0.1062 0.3174 0.3378 0.029 Uiso 1 1 calc R . . C43 C 0.06336(16) 0.25432(6) 0.41440(16) 0.0211(4) Uani 1 1 d . . . H43A H 0.0271 0.2683 0.4783 0.025 Uiso 1 1 calc R . . C44 C 0.06964(15) 0.20472(6) 0.40411(15) 0.0189(4) Uani 1 1 d . . . H44A H 0.0366 0.1855 0.4618 0.023 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0286(8) 0.0227(8) 0.0186(7) -0.0021(6) 0.0003(6) 0.0071(6) S1 0.0178(2) 0.0193(2) 0.0158(2) 0.00028(16) 0.00281(16) 0.00112(16) C2 0.0167(8) 0.0324(10) 0.0208(9) 0.0005(7) 0.0050(7) -0.0001(7) C3 0.0238(9) 0.0291(10) 0.0254(10) 0.0015(8) 0.0050(8) -0.0049(8) O4 0.0263(6) 0.0203(6) 0.0209(6) -0.0002(5) 0.0051(5) 0.0012(5) C5 0.0298(10) 0.0235(9) 0.0181(9) 0.0002(7) 0.0049(7) 0.0036(8) C6 0.0302(10) 0.0233(9) 0.0228(10) 0.0024(7) -0.0003(8) 0.0028(8) O7 0.0268(7) 0.0214(6) 0.0209(6) -0.0011(5) 0.0042(5) 0.0020(5) C8 0.0175(8) 0.0254(9) 0.0232(9) -0.0017(7) 0.0034(7) -0.0001(7) C9 0.0151(8) 0.0193(8) 0.0209(9) 0.0012(7) 0.0048(7) 0.0027(7) S11 0.0186(2) 0.0168(2) 0.0207(2) -0.00079(16) 0.00213(17) 0.00220(16) C12 0.0174(8) 0.0232(9) 0.0278(10) -0.0018(7) 0.0052(7) -0.0017(7) C13 0.0289(10) 0.0265(10) 0.0253(10) 0.0006(8) 0.0066(8) -0.0041(8) O14 0.0308(7) 0.0216(6) 0.0245(7) 0.0005(5) 0.0001(5) 0.0005(5) C15 0.0307(10) 0.0176(9) 0.0268(10) -0.0002(7) -0.0005(8) -0.0003(8) C16 0.0249(9) 0.0175(9) 0.0324(10) -0.0012(7) 0.0009(8) 0.0039(7) O17 0.0227(6) 0.0175(6) 0.0261(7) 0.0001(5) 0.0023(5) 0.0000(5) C18 0.0196(9) 0.0182(9) 0.0323(10) -0.0012(7) 0.0067(8) -0.0012(7) C19 0.0153(8) 0.0187(8) 0.0289(10) -0.0017(7) 0.0002(7) -0.0001(7) B20 0.0155(9) 0.0180(9) 0.0131(9) -0.0001(7) 0.0034(7) -0.0001(7) C21 0.0157(8) 0.0200(8) 0.0100(7) 0.0028(6) 0.0043(6) -0.0008(7) C22 0.0191(8) 0.0206(8) 0.0154(8) -0.0018(7) 0.0049(7) 0.0015(7) C23 0.0152(8) 0.0297(10) 0.0171(9) 0.0019(7) 0.0031(7) 0.0042(7) C24 0.0161(8) 0.0305(9) 0.0140(8) 0.0006(7) 0.0011(6) -0.0057(7) C25 0.0232(9) 0.0185(8) 0.0142(8) 0.0008(6) 0.0034(7) -0.0039(7) C26 0.0168(8) 0.0190(8) 0.0145(8) 0.0020(6) 0.0036(6) -0.0002(7) C27 0.0124(7) 0.0195(8) 0.0144(8) -0.0021(6) 0.0067(6) 0.0020(6) C28 0.0188(8) 0.0181(8) 0.0152(8) -0.0033(6) 0.0038(6) 0.0006(7) C29 0.0268(9) 0.0172(8) 0.0182(9) 0.0010(7) 0.0074(7) 0.0031(7) C30 0.0240(9) 0.0284(9) 0.0115(8) 0.0024(7) 0.0037(7) 0.0075(8) C31 0.0187(9) 0.0291(9) 0.0153(8) -0.0034(7) 0.0015(7) -0.0016(7) C32 0.0167(8) 0.0211(8) 0.0177(8) 0.0002(7) 0.0051(7) -0.0031(7) C33 0.0166(8) 0.0137(8) 0.0164(8) -0.0008(6) 0.0044(6) -0.0049(6) C34 0.0168(8) 0.0185(8) 0.0171(8) -0.0001(6) 0.0034(7) -0.0033(7) C35 0.0157(8) 0.0223(9) 0.0275(10) 0.0013(7) 0.0070(7) -0.0007(7) C36 0.0228(9) 0.0243(9) 0.0241(9) -0.0033(7) 0.0133(7) -0.0032(7) C37 0.0255(9) 0.0267(9) 0.0165(9) -0.0031(7) 0.0071(7) -0.0074(8) C38 0.0176(8) 0.0211(9) 0.0172(8) 0.0002(7) 0.0027(7) -0.0018(7) C39 0.0114(8) 0.0200(8) 0.0149(8) 0.0005(6) -0.0028(6) -0.0009(6) C40 0.0196(8) 0.0219(9) 0.0139(8) 0.0016(7) -0.0005(7) 0.0002(7) C41 0.0275(9) 0.0217(9) 0.0200(9) 0.0055(7) -0.0017(7) -0.0030(8) C42 0.0268(9) 0.0176(8) 0.0238(9) -0.0006(7) -0.0070(7) 0.0015(7) C43 0.0180(8) 0.0225(9) 0.0207(9) -0.0057(7) -0.0017(7) 0.0013(7) C44 0.0165(8) 0.0212(9) 0.0187(9) -0.0006(7) 0.0025(7) -0.0011(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 S1 1.6447(15) . ? N1 S11 1.6454(15) . ? S1 C2 1.8064(17) . ? S1 C9 1.8077(17) . ? C2 C3 1.520(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O4 1.410(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? O4 C5 1.426(2) . ? C5 C6 1.505(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O7 1.432(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O7 C8 1.418(2) . ? C8 C9 1.522(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? S11 C12 1.8014(17) . ? S11 C19 1.8081(17) . ? C12 C13 1.516(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 O14 1.427(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? O14 C15 1.427(2) . ? C15 C16 1.511(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O17 1.430(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? O17 C18 1.422(2) . ? C18 C19 1.518(2) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? B20 C39 1.644(2) . ? B20 C21 1.650(2) . ? B20 C33 1.652(2) . ? B20 C27 1.656(2) . ? C21 C22 1.398(2) . ? C21 C26 1.409(2) . ? C22 C23 1.394(2) . ? C22 H22A 0.9500 . ? C23 C24 1.382(2) . ? C23 H23A 0.9500 . ? C24 C25 1.383(2) . ? C24 H24A 0.9500 . ? C25 C26 1.388(2) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 C32 1.403(2) . ? C27 C28 1.406(2) . ? C28 C29 1.392(2) . ? C28 H28A 0.9500 . ? C29 C30 1.385(2) . ? C29 H29A 0.9500 . ? C30 C31 1.386(2) . ? C30 H30A 0.9500 . ? C31 C32 1.397(2) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C34 1.399(2) . ? C33 C38 1.407(2) . ? C34 C35 1.395(2) . ? C34 H34A 0.9500 . ? C35 C36 1.387(3) . ? C35 H35A 0.9500 . ? C36 C37 1.388(3) . ? C36 H36A 0.9500 . ? C37 C38 1.386(2) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C40 1.403(2) . ? C39 C44 1.409(2) . ? C40 C41 1.393(2) . ? C40 H40A 0.9500 . ? C41 C42 1.386(3) . ? C41 H41A 0.9500 . ? C42 C43 1.387(3) . ? C42 H42A 0.9500 . ? C43 C44 1.390(2) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? 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 S1 N1 S11 112.68(8) . . ? N1 S1 C2 99.83(8) . . ? N1 S1 C9 103.78(8) . . ? C2 S1 C9 104.71(8) . . ? C3 C2 S1 113.76(12) . . ? C3 C2 H2A 108.8 . . ? S1 C2 H2A 108.8 . . ? C3 C2 H2B 108.8 . . ? S1 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? O4 C3 C2 113.69(14) . . ? O4 C3 H3A 108.8 . . ? C2 C3 H3A 108.8 . . ? O4 C3 H3B 108.8 . . ? C2 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C3 O4 C5 115.79(13) . . ? O4 C5 C6 109.69(14) . . ? O4 C5 H5A 109.7 . . ? C6 C5 H5A 109.7 . . ? O4 C5 H5B 109.7 . . ? C6 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? O7 C6 C5 111.13(15) . . ? O7 C6 H6A 109.4 . . ? C5 C6 H6A 109.4 . . ? O7 C6 H6B 109.4 . . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C8 O7 C6 116.19(13) . . ? O7 C8 C9 115.31(14) . . ? O7 C8 H8A 108.4 . . ? C9 C8 H8A 108.4 . . ? O7 C8 H8B 108.4 . . ? C9 C8 H8B 108.4 . . ? H8A C8 H8B 107.5 . . ? C8 C9 S1 115.87(12) . . ? C8 C9 H9A 108.3 . . ? S1 C9 H9A 108.3 . . ? C8 C9 H9B 108.3 . . ? S1 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? N1 S11 C12 97.78(8) . . ? N1 S11 C19 105.08(8) . . ? C12 S11 C19 104.61(8) . . ? C13 C12 S11 115.86(13) . . ? C13 C12 H12A 108.3 . . ? S11 C12 H12A 108.3 . . ? C13 C12 H12B 108.3 . . ? S11 C12 H12B 108.3 . . ? H12A C12 H12B 107.4 . . ? O14 C13 C12 114.07(15) . . ? O14 C13 H13A 108.7 . . ? C12 C13 H13A 108.7 . . ? O14 C13 H13B 108.7 . . ? C12 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? C13 O14 C15 114.86(14) . . ? O14 C15 C16 111.46(14) . . ? O14 C15 H15A 109.3 . . ? C16 C15 H15A 109.3 . . ? O14 C15 H15B 109.3 . . ? C16 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? O17 C16 C15 111.31(14) . . ? O17 C16 H16A 109.4 . . ? C15 C16 H16A 109.4 . . ? O17 C16 H16B 109.4 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C18 O17 C16 115.24(13) . . ? O17 C18 C19 114.34(14) . . ? O17 C18 H18A 108.7 . . ? C19 C18 H18A 108.7 . . ? O17 C18 H18B 108.7 . . ? C19 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? C18 C19 S11 115.54(12) . . ? C18 C19 H19A 108.4 . . ? S11 C19 H19A 108.4 . . ? C18 C19 H19B 108.4 . . ? S11 C19 H19B 108.4 . . ? H19A C19 H19B 107.5 . . ? C39 B20 C21 110.75(13) . . ? C39 B20 C33 111.10(13) . . ? C21 B20 C33 106.06(12) . . ? C39 B20 C27 109.99(13) . . ? C21 B20 C27 110.18(13) . . ? C33 B20 C27 108.67(13) . . ? C22 C21 C26 114.84(14) . . ? C22 C21 B20 125.38(14) . . ? C26 C21 B20 119.78(14) . . ? C23 C22 C21 122.78(16) . . ? C23 C22 H22A 118.6 . . ? C21 C22 H22A 118.6 . . ? C24 C23 C22 120.33(15) . . ? C24 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? C23 C24 C25 118.89(15) . . ? C23 C24 H24A 120.6 . . ? C25 C24 H24A 120.6 . . ? C24 C25 C26 120.12(16) . . ? C24 C25 H25A 119.9 . . ? C26 C25 H25A 119.9 . . ? C25 C26 C21 123.03(15) . . ? C25 C26 H26A 118.5 . . ? C21 C26 H26A 118.5 . . ? C32 C27 C28 114.76(15) . . ? C32 C27 B20 121.56(14) . . ? C28 C27 B20 123.55(14) . . ? C29 C28 C27 122.77(15) . . ? C29 C28 H28A 118.6 . . ? C27 C28 H28A 118.6 . . ? C30 C29 C28 120.58(16) . . ? C30 C29 H29A 119.7 . . ? C28 C29 H29A 119.7 . . ? C29 C30 C31 118.72(15) . . ? C29 C30 H30A 120.6 . . ? C31 C30 H30A 120.6 . . ? C30 C31 C32 119.97(15) . . ? C30 C31 H31A 120.0 . . ? C32 C31 H31A 120.0 . . ? C31 C32 C27 123.19(16) . . ? C31 C32 H32A 118.4 . . ? C27 C32 H32A 118.4 . . ? C34 C33 C38 115.01(14) . . ? C34 C33 B20 124.72(14) . . ? C38 C33 B20 120.18(14) . . ? C35 C34 C33 122.83(15) . . ? C35 C34 H34A 118.6 . . ? C33 C34 H34A 118.6 . . ? C36 C35 C34 120.06(16) . . ? C36 C35 H35A 120.0 . . ? C34 C35 H35A 120.0 . . ? C35 C36 C37 118.97(15) . . ? C35 C36 H36A 120.5 . . ? C37 C36 H36A 120.5 . . ? C38 C37 C36 120.00(16) . . ? C38 C37 H37A 120.0 . . ? C36 C37 H37A 120.0 . . ? C37 C38 C33 123.07(16) . . ? C37 C38 H38A 118.5 . . ? C33 C38 H38A 118.5 . . ? C40 C39 C44 114.71(15) . . ? C40 C39 B20 123.96(14) . . ? C44 C39 B20 121.33(14) . . ? C41 C40 C39 123.01(16) . . ? C41 C40 H40A 118.5 . . ? C39 C40 H40A 118.5 . . ? C42 C41 C40 120.14(16) . . ? C42 C41 H41A 119.9 . . ? C40 C41 H41A 119.9 . . ? C41 C42 C43 119.00(16) . . ? C41 C42 H42A 120.5 . . ? C43 C42 H42A 120.5 . . ? C42 C43 C44 119.97(16) . . ? C42 C43 H43A 120.0 . . ? C44 C43 H43A 120.0 . . ? C43 C44 C39 123.16(16) . . ? C43 C44 H44A 118.4 . . ? C39 C44 H44A 118.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S11 N1 S1 C2 -127.92(10) . . . . ? S11 N1 S1 C9 124.15(9) . . . . ? N1 S1 C2 C3 -166.50(13) . . . . ? C9 S1 C2 C3 -59.31(14) . . . . ? S1 C2 C3 O4 70.41(18) . . . . ? C2 C3 O4 C5 69.07(19) . . . . ? C3 O4 C5 C6 -119.77(16) . . . . ? O4 C5 C6 O7 69.38(18) . . . . ? C5 C6 O7 C8 -111.41(16) . . . . ? C6 O7 C8 C9 75.63(18) . . . . ? O7 C8 C9 S1 62.70(18) . . . . ? N1 S1 C9 C8 37.52(14) . . . . ? C2 S1 C9 C8 -66.74(14) . . . . ? S1 N1 S11 C12 -142.19(9) . . . . ? S1 N1 S11 C19 110.32(10) . . . . ? N1 S11 C12 C13 -168.57(13) . . . . ? C19 S11 C12 C13 -60.69(15) . . . . ? S11 C12 C13 O14 69.41(18) . . . . ? C12 C13 O14 C15 67.64(19) . . . . ? C13 O14 C15 C16 -116.58(16) . . . . ? O14 C15 C16 O17 71.09(19) . . . . ? C15 C16 O17 C18 -113.22(16) . . . . ? C16 O17 C18 C19 75.43(18) . . . . ? O17 C18 C19 S11 63.01(18) . . . . ? N1 S11 C19 C18 35.25(14) . . . . ? C12 S11 C19 C18 -67.17(14) . . . . ? C39 B20 C21 C22 -15.8(2) . . . . ? C33 B20 C21 C22 -136.46(15) . . . . ? C27 B20 C21 C22 106.11(17) . . . . ? C39 B20 C21 C26 163.76(14) . . . . ? C33 B20 C21 C26 43.11(18) . . . . ? C27 B20 C21 C26 -74.32(17) . . . . ? C26 C21 C22 C23 1.5(2) . . . . ? B20 C21 C22 C23 -178.95(15) . . . . ? C21 C22 C23 C24 -1.2(2) . . . . ? C22 C23 C24 C25 0.3(2) . . . . ? C23 C24 C25 C26 0.2(2) . . . . ? C24 C25 C26 C21 0.1(2) . . . . ? C22 C21 C26 C25 -0.9(2) . . . . ? B20 C21 C26 C25 179.50(14) . . . . ? C39 B20 C27 C32 -31.0(2) . . . . ? C21 B20 C27 C32 -153.38(14) . . . . ? C33 B20 C27 C32 90.82(17) . . . . ? C39 B20 C27 C28 153.34(14) . . . . ? C21 B20 C27 C28 31.0(2) . . . . ? C33 B20 C27 C28 -84.84(18) . . . . ? C32 C27 C28 C29 -1.2(2) . . . . ? B20 C27 C28 C29 174.76(15) . . . . ? C27 C28 C29 C30 0.4(2) . . . . ? C28 C29 C30 C31 0.7(2) . . . . ? C29 C30 C31 C32 -1.0(2) . . . . ? C30 C31 C32 C27 0.2(3) . . . . ? C28 C27 C32 C31 0.9(2) . . . . ? B20 C27 C32 C31 -175.16(15) . . . . ? C39 B20 C33 C34 107.87(17) . . . . ? C21 B20 C33 C34 -131.70(15) . . . . ? C27 B20 C33 C34 -13.3(2) . . . . ? C39 B20 C33 C38 -75.56(18) . . . . ? C21 B20 C33 C38 44.87(19) . . . . ? C27 B20 C33 C38 163.30(14) . . . . ? C38 C33 C34 C35 -1.9(2) . . . . ? B20 C33 C34 C35 174.80(15) . . . . ? C33 C34 C35 C36 0.0(3) . . . . ? C34 C35 C36 C37 1.6(2) . . . . ? C35 C36 C37 C38 -1.1(3) . . . . ? C36 C37 C38 C33 -1.0(3) . . . . ? C34 C33 C38 C37 2.4(2) . . . . ? B20 C33 C38 C37 -174.47(15) . . . . ? C21 B20 C39 C40 -100.99(17) . . . . ? C33 B20 C39 C40 16.6(2) . . . . ? C27 B20 C39 C40 136.98(15) . . . . ? C21 B20 C39 C44 78.91(18) . . . . ? C33 B20 C39 C44 -163.48(14) . . . . ? C27 B20 C39 C44 -43.11(19) . . . . ? C44 C39 C40 C41 0.7(2) . . . . ? B20 C39 C40 C41 -179.40(15) . . . . ? C39 C40 C41 C42 -0.2(3) . . . . ? C40 C41 C42 C43 -0.2(3) . . . . ? C41 C42 C43 C44 0.1(2) . . . . ? C42 C43 C44 C39 0.4(3) . . . . ? C40 C39 C44 C43 -0.8(2) . . . . ? B20 C39 C44 C43 179.32(15) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.294 _refine_diff_density_min -0.315 _refine_diff_density_rms 0.047 #===END data_[5][BPh4] _database_code_depnum_ccdc_archive 'CCDC 678821' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H53 B Cl3 N O6 S2' _chemical_formula_sum 'C41 H53 B Cl3 N O6 S2' _chemical_formula_weight 837.12 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.046(3) _cell_length_b 11.934(2) _cell_length_c 25.163(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.981(6) _cell_angle_gamma 90.00 _cell_volume 4166.5(16) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 8570 _cell_measurement_theta_min 1.8925 _cell_measurement_theta_max 25.3491 _exptl_crystal_description needle _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.1300 _exptl_crystal_size_mid 0.0300 _exptl_crystal_size_min 0.0300 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 0.367 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9820 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22437 _diffrn_reflns_av_R_equivalents 0.0567 _diffrn_reflns_av_sigmaI/netI 0.0649 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.38 _reflns_number_total 6919 _reflns_number_gt 4955 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _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. O4 was refined as partial occupancies with the hydrogen atom positions on C3 and C5 being calculated from the major component only. Various different crytslas fronm several different preparations were tried - the best result is described. ; _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^)+(0.1309P)^2^+15.6815P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0081(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6919 _refine_ls_number_parameters 498 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1380 _refine_ls_R_factor_gt 0.1066 _refine_ls_wR_factor_ref 0.2964 _refine_ls_wR_factor_gt 0.2626 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.2830(4) 0.7746(5) 0.0894(2) 0.0406(13) Uani 1 1 d . A 1 S1 S 0.19675(12) 0.73603(16) 0.12245(7) 0.0465(5) Uani 1 1 d . A 1 C2 C 0.0974(6) 0.8277(9) 0.0911(5) 0.097(4) Uani 1 1 d . A 1 H2A H 0.1184 0.9067 0.0959 0.117 Uiso 1 1 calc R A 1 H2B H 0.0846 0.8122 0.0520 0.117 Uiso 1 1 calc R A 1 C3 C 0.0099(6) 0.8136(7) 0.1127(3) 0.060(2) Uani 1 1 d . A 1 H3A H -0.0265 0.7506 0.0937 0.072 Uiso 1 1 calc R A 1 H3B H -0.0296 0.8821 0.1048 0.072 Uiso 1 1 calc R A 1 O4A O 0.0209(5) 0.7921(6) 0.1705(3) 0.0470(17) Uani 0.70 1 d P A 1 C5 C -0.0561(6) 0.7299(8) 0.1832(6) 0.107(5) Uani 1 1 d . A 1 H5A H -0.0840 0.7735 0.2105 0.128 Uiso 1 1 calc R A 1 H5B H -0.1054 0.7285 0.1505 0.128 Uiso 1 1 calc R A 1 C6 C -0.0470(7) 0.6254(9) 0.2012(5) 0.103(4) Uani 1 1 d . A 1 H6A H -0.0560 0.5732 0.1702 0.123 Uiso 1 1 calc R A 1 H6B H -0.0979 0.6097 0.2233 0.123 Uiso 1 1 calc R A 1 O7 O 0.0470(5) 0.6059(5) 0.2333(3) 0.0823(19) Uani 1 1 d . A 1 C8 C 0.0724(6) 0.4952(7) 0.2364(4) 0.062(2) Uani 1 1 d . A 1 H8A H 0.0140 0.4505 0.2393 0.074 Uiso 1 1 calc R A 1 H8B H 0.1182 0.4836 0.2700 0.074 Uiso 1 1 calc R A 1 C9 C 0.1144(9) 0.4524(9) 0.1932(6) 0.109(4) Uani 1 1 d . A 1 H9A H 0.1312 0.3727 0.2007 0.130 Uiso 1 1 calc R A 1 H9B H 0.0658 0.4549 0.1602 0.130 Uiso 1 1 calc R A 1 O10 O 0.1975(4) 0.5092(5) 0.1832(2) 0.0705(17) Uani 1 1 d . A 1 C11 C 0.2145(7) 0.5143(8) 0.1279(4) 0.078(3) Uani 1 1 d . A 1 H11A H 0.1970 0.4411 0.1105 0.094 Uiso 1 1 calc R A 1 H11B H 0.2843 0.5261 0.1278 0.094 Uiso 1 1 calc R A 1 C12 C 0.1608(8) 0.6027(8) 0.0959(3) 0.077(3) Uani 1 1 d . A 1 H12A H 0.0909 0.5925 0.0961 0.092 Uiso 1 1 calc R A 1 H12B H 0.1726 0.5978 0.0582 0.092 Uiso 1 1 calc R A 1 S21 S 0.38159(11) 0.80410(14) 0.13135(6) 0.0383(5) Uani 1 1 d . A 1 C22 C 0.4689(5) 0.7570(7) 0.0924(3) 0.0538(19) Uani 1 1 d . A 1 H22A H 0.4511 0.7832 0.0549 0.065 Uiso 1 1 calc R A 1 H22B H 0.5325 0.7894 0.1070 0.065 Uiso 1 1 calc R A 1 C23 C 0.4757(5) 0.6305(7) 0.0932(3) 0.055(2) Uani 1 1 d . A 1 H23A H 0.4138 0.5990 0.0751 0.066 Uiso 1 1 calc R A 1 H23B H 0.5266 0.6071 0.0724 0.066 Uiso 1 1 calc R A 1 O24 O 0.4965(4) 0.5855(4) 0.1455(2) 0.0627(15) Uani 1 1 d . A 1 C25 C 0.5963(8) 0.5957(8) 0.1699(6) 0.133(6) Uani 1 1 d . A 1 H25A H 0.6329 0.6346 0.1448 0.160 Uiso 1 1 calc R A 1 H25B H 0.6245 0.5202 0.1771 0.160 Uiso 1 1 calc R A 1 C26 C 0.6045(12) 0.6600(8) 0.2214(5) 0.165(8) Uani 1 1 d . A 1 H26A H 0.5532 0.6369 0.2420 0.199 Uiso 1 1 calc R A 1 H26B H 0.6678 0.6461 0.2437 0.199 Uiso 1 1 calc R A 1 O27 O 0.5945(4) 0.7757(4) 0.2073(2) 0.0677(17) Uani 1 1 d . A 1 C28 C 0.5933(8) 0.8388(9) 0.2550(4) 0.090(4) Uani 1 1 d . A 1 H28A H 0.6559 0.8306 0.2790 0.108 Uiso 1 1 calc R A 1 H28B H 0.5420 0.8104 0.2742 0.108 Uiso 1 1 calc R A 1 C29 C 0.5757(6) 0.9591(8) 0.2412(4) 0.071(3) Uani 1 1 d . A 1 H29A H 0.5809 1.0041 0.2746 0.085 Uiso 1 1 calc R A 1 H29B H 0.6249 0.9864 0.2200 0.085 Uiso 1 1 calc R A 1 O30 O 0.4810(4) 0.9723(5) 0.2103(2) 0.0629(15) Uani 1 1 d . A 1 C31 C 0.4820(6) 1.0011(7) 0.1558(3) 0.059(2) Uani 1 1 d . A 1 H31A H 0.5395 0.9687 0.1433 0.071 Uiso 1 1 calc R A 1 H31B H 0.4840 1.0835 0.1518 0.071 Uiso 1 1 calc R A 1 C32 C 0.3931(6) 0.9554(6) 0.1241(3) 0.056(2) Uani 1 1 d . A 1 H32A H 0.3926 0.9733 0.0856 0.067 Uiso 1 1 calc R A 1 H32B H 0.3366 0.9924 0.1356 0.067 Uiso 1 1 calc R A 1 B40 B 0.2595(5) 0.2703(6) 0.5196(3) 0.0340(16) Uani 1 1 d . B 1 C41 C 0.3746(4) 0.2704(5) 0.5445(2) 0.0348(14) Uani 1 1 d . B 1 C42 C 0.4405(4) 0.3470(5) 0.5281(2) 0.0293(13) Uani 1 1 d . B 1 H42A H 0.4173 0.4016 0.5018 0.035 Uiso 1 1 calc R B 1 C43 C 0.5389(4) 0.3459(5) 0.5490(2) 0.0328(13) Uani 1 1 d . B 1 H43A H 0.5811 0.3995 0.5372 0.039 Uiso 1 1 calc R B 1 C44 C 0.5744(4) 0.2665(5) 0.5870(2) 0.0351(14) Uani 1 1 d . B 1 H44A H 0.6412 0.2643 0.6009 0.042 Uiso 1 1 calc R B 1 C45 C 0.5125(4) 0.1909(5) 0.6044(3) 0.0384(15) Uani 1 1 d . B 1 H45A H 0.5363 0.1365 0.6307 0.046 Uiso 1 1 calc R B 1 C46 C 0.4145(5) 0.1939(6) 0.5836(3) 0.0400(15) Uani 1 1 d . B 1 H46A H 0.3730 0.1412 0.5966 0.048 Uiso 1 1 calc R B 1 C47 C 0.2272(5) 0.1444(5) 0.4965(2) 0.0356(14) Uani 1 1 d . B 1 C48 C 0.1309(4) 0.1074(5) 0.4867(2) 0.0386(15) Uani 1 1 d . B 1 H48A H 0.0822 0.1552 0.4963 0.046 Uiso 1 1 calc R B 1 C49 C 0.1034(5) 0.0032(6) 0.4636(3) 0.0449(17) Uani 1 1 d . B 1 H49A H 0.0372 -0.0170 0.4565 0.054 Uiso 1 1 calc R B 1 C50 C 0.1729(5) -0.0702(5) 0.4510(3) 0.0448(17) Uani 1 1 d . B 1 H50A H 0.1549 -0.1413 0.4356 0.054 Uiso 1 1 calc R B 1 C51 C 0.2685(5) -0.0391(6) 0.4609(3) 0.0482(17) Uani 1 1 d . B 1 H51A H 0.3168 -0.0885 0.4522 0.058 Uiso 1 1 calc R B 1 C52 C 0.2939(5) 0.0639(6) 0.4836(3) 0.0444(16) Uani 1 1 d . B 1 H52A H 0.3605 0.0820 0.4912 0.053 Uiso 1 1 calc R B 1 C53 C 0.1919(4) 0.3091(5) 0.5644(3) 0.0399(16) Uani 1 1 d . B 1 C54 C 0.0962(4) 0.3444(6) 0.5485(3) 0.0475(18) Uani 1 1 d . B 1 H54A H 0.0722 0.3498 0.5111 0.057 Uiso 1 1 calc R B 1 C55 C 0.0347(5) 0.3720(7) 0.5853(4) 0.063(2) Uani 1 1 d . B 1 H55A H -0.0299 0.3937 0.5726 0.076 Uiso 1 1 calc R B 1 C56 C 0.0670(6) 0.3680(6) 0.6397(4) 0.060(2) Uani 1 1 d . B 1 H56A H 0.0253 0.3856 0.6648 0.072 Uiso 1 1 calc R B 1 C57 C 0.1616(5) 0.3377(6) 0.6568(3) 0.0497(18) Uani 1 1 d . B 1 H57A H 0.1863 0.3374 0.6942 0.060 Uiso 1 1 calc R B 1 C58 C 0.2221(5) 0.3073(6) 0.6194(3) 0.0443(17) Uani 1 1 d . B 1 H58A H 0.2863 0.2846 0.6325 0.053 Uiso 1 1 calc R B 1 C59 C 0.2427(4) 0.3581(6) 0.4687(3) 0.0443(17) Uani 1 1 d . B 1 C60 C 0.2244(4) 0.4737(6) 0.4751(3) 0.0486(19) Uani 1 1 d . B 1 H60A H 0.2130 0.5000 0.5092 0.058 Uiso 1 1 calc R B 1 C61 C 0.2227(4) 0.5506(6) 0.4327(5) 0.066(3) Uani 1 1 d . B 1 H61A H 0.2113 0.6277 0.4388 0.079 Uiso 1 1 calc R B 1 C62 C 0.2373(6) 0.5155(8) 0.3820(4) 0.068(3) Uani 1 1 d . B 1 H62A H 0.2345 0.5673 0.3532 0.081 Uiso 1 1 calc R B 1 C63 C 0.2557(5) 0.4051(8) 0.3747(3) 0.060(2) Uani 1 1 d . B 1 H63A H 0.2664 0.3801 0.3403 0.072 Uiso 1 1 calc R B 1 C64 C 0.2593(4) 0.3272(6) 0.4169(3) 0.0442(17) Uani 1 1 d . B 1 H64A H 0.2734 0.2511 0.4102 0.053 Uiso 1 1 calc R B 1 C71 C 0.2079(4) 0.7959(5) 0.2603(2) 0.0357(14) Uani 1 1 d . C 1 H71A H 0.1628 0.7460 0.2364 0.043 Uiso 1 1 calc R C 1 Cl1 Cl 0.21403(15) 0.92700(14) 0.22838(7) 0.0542(5) Uani 1 1 d . C 1 Cl2 Cl 0.32052(14) 0.73399(19) 0.27194(7) 0.0627(6) Uani 1 1 d . C 1 Cl3 Cl 0.16248(15) 0.81578(18) 0.32128(7) 0.0591(6) Uani 1 1 d . C 1 O4B O 0.0089(11) 0.7174(14) 0.1329(7) 0.048(4) Uani 0.30 1 d P D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.038(3) 0.043(3) 0.037(3) 0.006(2) -0.004(2) -0.008(2) S1 0.0406(10) 0.0557(12) 0.0393(10) -0.0020(8) -0.0058(7) -0.0087(8) C2 0.046(5) 0.098(8) 0.140(10) 0.058(7) -0.012(6) -0.004(5) C3 0.072(6) 0.039(5) 0.060(5) -0.006(4) -0.019(4) 0.014(4) O4A 0.042(4) 0.059(5) 0.038(4) 0.008(3) -0.002(3) 0.003(3) C5 0.033(5) 0.064(7) 0.229(14) 0.051(7) 0.040(6) 0.002(4) C6 0.068(7) 0.088(8) 0.158(11) 0.052(8) 0.038(7) 0.014(6) O7 0.075(4) 0.065(4) 0.106(5) 0.023(4) 0.011(4) -0.007(3) C8 0.061(5) 0.047(5) 0.080(6) 0.011(4) 0.019(4) -0.007(4) C9 0.119(10) 0.070(7) 0.162(12) -0.025(7) 0.096(9) -0.029(6) O10 0.049(3) 0.096(5) 0.069(4) 0.023(3) 0.016(3) 0.003(3) C11 0.075(6) 0.051(6) 0.119(8) -0.014(5) 0.049(6) 0.012(4) C12 0.118(8) 0.065(6) 0.050(5) -0.021(4) 0.022(5) -0.043(6) S21 0.0405(9) 0.0392(10) 0.0331(9) 0.0090(6) -0.0007(6) -0.0064(7) C22 0.049(4) 0.065(5) 0.050(4) 0.009(4) 0.016(3) -0.005(4) C23 0.042(4) 0.074(6) 0.053(5) -0.019(4) 0.018(3) -0.006(4) O24 0.071(4) 0.041(3) 0.068(4) -0.006(2) -0.015(3) -0.008(2) C25 0.104(8) 0.035(5) 0.219(14) -0.011(7) -0.102(9) 0.006(5) C26 0.258(17) 0.038(6) 0.144(11) 0.044(6) -0.143(12) -0.061(8) O27 0.085(4) 0.036(3) 0.071(4) 0.016(3) -0.024(3) -0.029(3) C28 0.096(7) 0.108(9) 0.055(6) 0.021(5) -0.024(5) -0.054(6) C29 0.060(5) 0.090(7) 0.063(5) -0.018(5) 0.010(4) -0.032(5) O30 0.070(4) 0.081(4) 0.043(3) -0.013(3) 0.025(3) -0.025(3) C31 0.068(5) 0.054(5) 0.060(5) -0.006(4) 0.023(4) -0.017(4) C32 0.063(5) 0.043(5) 0.064(5) 0.015(4) 0.017(4) -0.005(3) B40 0.025(3) 0.031(4) 0.045(4) 0.000(3) 0.002(3) 0.005(3) C41 0.034(3) 0.035(4) 0.036(3) -0.001(3) 0.008(3) 0.003(3) C42 0.030(3) 0.028(3) 0.030(3) 0.004(2) 0.006(2) 0.002(2) C43 0.034(3) 0.038(4) 0.028(3) -0.001(2) 0.008(2) 0.001(3) C44 0.033(3) 0.043(4) 0.028(3) 0.001(3) 0.004(2) 0.006(3) C45 0.035(3) 0.037(4) 0.042(4) 0.011(3) 0.001(3) 0.005(3) C46 0.038(4) 0.037(4) 0.046(4) 0.012(3) 0.013(3) 0.000(3) C47 0.043(4) 0.035(4) 0.029(3) 0.002(3) 0.006(3) 0.007(3) C48 0.036(3) 0.034(4) 0.041(4) 0.000(3) -0.011(3) 0.006(3) C49 0.054(4) 0.041(4) 0.035(4) -0.001(3) -0.007(3) 0.006(3) C50 0.067(5) 0.027(4) 0.038(4) -0.001(3) -0.001(3) 0.001(3) C51 0.059(5) 0.035(4) 0.055(4) -0.006(3) 0.021(3) 0.007(3) C52 0.050(4) 0.037(4) 0.049(4) -0.004(3) 0.019(3) 0.006(3) C53 0.030(3) 0.023(4) 0.068(5) -0.006(3) 0.013(3) -0.005(2) C54 0.028(3) 0.038(4) 0.076(5) -0.008(3) 0.007(3) 0.004(3) C55 0.030(4) 0.051(5) 0.114(8) -0.030(5) 0.026(4) -0.004(3) C56 0.051(5) 0.048(5) 0.089(7) -0.029(4) 0.034(4) -0.014(4) C57 0.054(5) 0.035(4) 0.066(5) -0.018(3) 0.025(4) -0.010(3) C58 0.038(4) 0.038(4) 0.058(5) -0.012(3) 0.013(3) -0.007(3) C59 0.021(3) 0.048(5) 0.061(5) 0.012(3) 0.001(3) -0.001(3) C60 0.023(3) 0.030(4) 0.090(6) 0.009(3) 0.002(3) -0.004(3) C61 0.018(3) 0.037(5) 0.137(9) 0.029(5) -0.008(4) -0.001(3) C62 0.043(4) 0.062(6) 0.087(7) 0.033(5) -0.028(4) -0.018(4) C63 0.038(4) 0.079(7) 0.056(5) 0.018(4) -0.015(3) -0.020(4) C64 0.031(3) 0.041(4) 0.057(4) 0.020(3) -0.004(3) -0.004(3) C71 0.038(3) 0.034(4) 0.034(3) 0.002(3) 0.003(3) 0.004(3) Cl1 0.0845(14) 0.0328(10) 0.0495(11) 0.0042(7) 0.0231(9) 0.0030(8) Cl2 0.0552(12) 0.0829(15) 0.0476(11) -0.0035(9) 0.0006(8) 0.0311(10) Cl3 0.0694(13) 0.0718(14) 0.0401(10) 0.0114(8) 0.0206(9) 0.0229(10) O4B 0.037(9) 0.055(11) 0.057(11) 0.029(9) 0.023(7) 0.017(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 N1 S1 1.639(6) . ? N1 S21 1.643(5) . ? S1 C12 1.768(8) . ? S1 C2 1.849(9) . ? C2 C3 1.430(13) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O4A 1.460(10) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? O4A C5 1.389(10) . ? C5 C6 1.326(13) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O7 1.455(12) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O7 C8 1.367(10) . ? C8 C9 1.410(12) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O10 1.407(11) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? O10 C11 1.448(11) . ? C11 C12 1.464(13) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? S21 C22 1.776(8) . ? S21 C32 1.824(7) . ? C22 C23 1.513(11) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 O24 1.410(9) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? O24 C25 1.445(10) . ? C25 C26 1.493(19) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O27 1.428(10) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? O27 C28 1.419(12) . ? C28 C29 1.489(14) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O30 1.440(10) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? O30 C31 1.416(9) . ? C31 C32 1.478(11) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? B40 C41 1.640(9) . ? B40 C59 1.643(10) . ? B40 C53 1.647(10) . ? B40 C47 1.649(9) . ? C41 C46 1.393(9) . ? C41 C42 1.408(8) . ? C42 C43 1.400(8) . ? C42 H42A 0.9500 . ? C43 C44 1.382(8) . ? C43 H43A 0.9500 . ? C44 C45 1.371(9) . ? C44 H44A 0.9500 . ? C45 C46 1.394(8) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C47 C48 1.408(9) . ? C47 C52 1.414(9) . ? C48 C49 1.402(9) . ? C48 H48A 0.9500 . ? C49 C50 1.384(10) . ? C49 H49A 0.9500 . ? C50 C51 1.378(10) . ? C50 H50A 0.9500 . ? C51 C52 1.379(10) . ? C51 H51A 0.9500 . ? C52 H52A 0.9500 . ? C53 C58 1.383(10) . ? C53 C54 1.406(9) . ? C54 C55 1.402(10) . ? C54 H54A 0.9500 . ? C55 C56 1.373(12) . ? C55 H55A 0.9500 . ? C56 C57 1.380(11) . ? C56 H56A 0.9500 . ? C57 C58 1.411(9) . ? C57 H57A 0.9500 . ? C58 H58A 0.9500 . ? C59 C64 1.410(10) . ? C59 C60 1.417(10) . ? C60 C61 1.405(11) . ? C60 H60A 0.9500 . ? C61 C62 1.388(13) . ? C61 H61A 0.9500 . ? C62 C63 1.362(13) . ? C62 H62A 0.9500 . ? C63 C64 1.405(10) . ? C63 H63A 0.9500 . ? C64 H64A 0.9500 . ? C71 Cl2 1.729(6) . ? C71 Cl3 1.766(6) . ? C71 Cl1 1.767(6) . ? C71 H71A 1.0000 . ? 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 S1 N1 S21 110.5(3) . . ? N1 S1 C12 104.6(4) . . ? N1 S1 C2 100.7(4) . . ? C12 S1 C2 102.6(5) . . ? C3 C2 S1 113.9(7) . . ? C3 C2 H2A 108.8 . . ? S1 C2 H2A 108.8 . . ? C3 C2 H2B 108.8 . . ? S1 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C2 C3 O4A 115.8(7) . . ? C2 C3 H3A 108.3 . . ? O4A C3 H3A 108.3 . . ? C2 C3 H3B 108.3 . . ? O4A C3 H3B 108.3 . . ? H3A C3 H3B 107.4 . . ? C5 O4A C3 110.9(8) . . ? C6 C5 O4A 122.9(8) . . ? C6 C5 H5A 106.6 . . ? O4A C5 H5A 106.6 . . ? C6 C5 H5B 106.6 . . ? O4A C5 H5B 106.6 . . ? H5A C5 H5B 106.6 . . ? C5 C6 O7 111.8(10) . . ? C5 C6 H6A 109.3 . . ? O7 C6 H6A 109.3 . . ? C5 C6 H6B 109.3 . . ? O7 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? C8 O7 C6 113.1(8) . . ? O7 C8 C9 116.3(8) . . ? O7 C8 H8A 108.2 . . ? C9 C8 H8A 108.2 . . ? O7 C8 H8B 108.2 . . ? C9 C8 H8B 108.2 . . ? H8A C8 H8B 107.4 . . ? O10 C9 C8 115.0(9) . . ? O10 C9 H9A 108.5 . . ? C8 C9 H9A 108.5 . . ? O10 C9 H9B 108.5 . . ? C8 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? C9 O10 C11 117.3(8) . . ? O10 C11 C12 114.2(7) . . ? O10 C11 H11A 108.7 . . ? C12 C11 H11A 108.7 . . ? O10 C11 H11B 108.7 . . ? C12 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? C11 C12 S1 110.4(7) . . ? C11 C12 H12A 109.6 . . ? S1 C12 H12A 109.6 . . ? C11 C12 H12B 109.6 . . ? S1 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? N1 S21 C22 99.4(3) . . ? N1 S21 C32 103.1(3) . . ? C22 S21 C32 100.3(4) . . ? C23 C22 S21 110.9(5) . . ? C23 C22 H22A 109.5 . . ? S21 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? S21 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? O24 C23 C22 113.3(6) . . ? O24 C23 H23A 108.9 . . ? C22 C23 H23A 108.9 . . ? O24 C23 H23B 108.9 . . ? C22 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? C23 O24 C25 114.2(8) . . ? O24 C25 C26 110.5(12) . . ? O24 C25 H25A 109.6 . . ? C26 C25 H25A 109.6 . . ? O24 C25 H25B 109.6 . . ? C26 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? O27 C26 C25 106.9(9) . . ? O27 C26 H26A 110.3 . . ? C25 C26 H26A 110.3 . . ? O27 C26 H26B 110.3 . . ? C25 C26 H26B 110.3 . . ? H26A C26 H26B 108.6 . . ? C28 O27 C26 108.5(8) . . ? O27 C28 C29 109.7(7) . . ? O27 C28 H28A 109.7 . . ? C29 C28 H28A 109.7 . . ? O27 C28 H28B 109.7 . . ? C29 C28 H28B 109.7 . . ? H28A C28 H28B 108.2 . . ? O30 C29 C28 109.7(7) . . ? O30 C29 H29A 109.7 . . ? C28 C29 H29A 109.7 . . ? O30 C29 H29B 109.7 . . ? C28 C29 H29B 109.7 . . ? H29A C29 H29B 108.2 . . ? C31 O30 C29 113.6(6) . . ? O30 C31 C32 107.3(6) . . ? O30 C31 H31A 110.2 . . ? C32 C31 H31A 110.2 . . ? O30 C31 H31B 110.2 . . ? C32 C31 H31B 110.2 . . ? H31A C31 H31B 108.5 . . ? C31 C32 S21 113.1(6) . . ? C31 C32 H32A 109.0 . . ? S21 C32 H32A 109.0 . . ? C31 C32 H32B 109.0 . . ? S21 C32 H32B 109.0 . . ? H32A C32 H32B 107.8 . . ? C41 B40 C59 108.1(5) . . ? C41 B40 C53 112.2(5) . . ? C59 B40 C53 109.0(5) . . ? C41 B40 C47 109.6(5) . . ? C59 B40 C47 107.9(5) . . ? C53 B40 C47 110.0(5) . . ? C46 C41 C42 114.9(5) . . ? C46 C41 B40 122.2(6) . . ? C42 C41 B40 122.9(5) . . ? C43 C42 C41 122.7(5) . . ? C43 C42 H42A 118.7 . . ? C41 C42 H42A 118.7 . . ? C44 C43 C42 119.6(6) . . ? C44 C43 H43A 120.2 . . ? C42 C43 H43A 120.2 . . ? C45 C44 C43 119.6(6) . . ? C45 C44 H44A 120.2 . . ? C43 C44 H44A 120.2 . . ? C44 C45 C46 120.1(6) . . ? C44 C45 H45A 119.9 . . ? C46 C45 H45A 119.9 . . ? C41 C46 C45 123.1(6) . . ? C41 C46 H46A 118.4 . . ? C45 C46 H46A 118.4 . . ? C48 C47 C52 113.6(6) . . ? C48 C47 B40 123.4(5) . . ? C52 C47 B40 123.0(6) . . ? C49 C48 C47 123.1(6) . . ? C49 C48 H48A 118.5 . . ? C47 C48 H48A 118.5 . . ? C50 C49 C48 119.9(7) . . ? C50 C49 H49A 120.1 . . ? C48 C49 H49A 120.1 . . ? C51 C50 C49 119.4(6) . . ? C51 C50 H50A 120.3 . . ? C49 C50 H50A 120.3 . . ? C50 C51 C52 119.8(6) . . ? C50 C51 H51A 120.1 . . ? C52 C51 H51A 120.1 . . ? C51 C52 C47 124.2(7) . . ? C51 C52 H52A 117.9 . . ? C47 C52 H52A 117.9 . . ? C58 C53 C54 114.8(6) . . ? C58 C53 B40 124.1(6) . . ? C54 C53 B40 121.1(6) . . ? C55 C54 C53 122.9(7) . . ? C55 C54 H54A 118.6 . . ? C53 C54 H54A 118.6 . . ? C56 C55 C54 120.6(7) . . ? C56 C55 H55A 119.7 . . ? C54 C55 H55A 119.7 . . ? C55 C56 C57 118.2(7) . . ? C55 C56 H56A 120.9 . . ? C57 C56 H56A 120.9 . . ? C56 C57 C58 120.7(7) . . ? C56 C57 H57A 119.6 . . ? C58 C57 H57A 119.6 . . ? C53 C58 C57 122.8(7) . . ? C53 C58 H58A 118.6 . . ? C57 C58 H58A 118.6 . . ? C64 C59 C60 114.8(6) . . ? C64 C59 B40 122.0(6) . . ? C60 C59 B40 122.6(7) . . ? C61 C60 C59 122.1(8) . . ? C61 C60 H60A 118.9 . . ? C59 C60 H60A 118.9 . . ? C62 C61 C60 120.9(8) . . ? C62 C61 H61A 119.6 . . ? C60 C61 H61A 119.6 . . ? C63 C62 C61 118.3(8) . . ? C63 C62 H62A 120.8 . . ? C61 C62 H62A 120.8 . . ? C62 C63 C64 121.6(9) . . ? C62 C63 H63A 119.2 . . ? C64 C63 H63A 119.2 . . ? C63 C64 C59 122.2(7) . . ? C63 C64 H64A 118.9 . . ? C59 C64 H64A 118.9 . . ? Cl2 C71 Cl3 110.8(3) . . ? Cl2 C71 Cl1 110.3(4) . . ? Cl3 C71 Cl1 109.0(3) . . ? Cl2 C71 H71A 108.9 . . ? Cl3 C71 H71A 108.9 . . ? Cl1 C71 H71A 108.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S21 N1 S1 C12 -124.2(5) . . . . ? S21 N1 S1 C2 129.6(5) . . . . ? N1 S1 C2 C3 -179.4(8) . . . . ? C12 S1 C2 C3 72.9(9) . . . . ? S1 C2 C3 O4A 36.7(11) . . . . ? C2 C3 O4A C5 -151.8(9) . . . . ? C3 O4A C5 C6 112.5(15) . . . . ? O4A C5 C6 O7 32(2) . . . . ? C5 C6 O7 C8 -158.2(11) . . . . ? C6 O7 C8 C9 83.7(11) . . . . ? O7 C8 C9 O10 56.6(14) . . . . ? C8 C9 O10 C11 -147.9(10) . . . . ? C9 O10 C11 C12 82.1(11) . . . . ? O10 C11 C12 S1 63.0(10) . . . . ? N1 S1 C12 C11 92.2(7) . . . . ? C2 S1 C12 C11 -163.0(7) . . . . ? S1 N1 S21 C22 145.6(4) . . . . ? S1 N1 S21 C32 -111.4(4) . . . . ? N1 S21 C22 C23 -76.2(6) . . . . ? C32 S21 C22 C23 178.5(6) . . . . ? S21 C22 C23 O24 -56.4(8) . . . . ? C22 C23 O24 C25 -77.2(8) . . . . ? C23 O24 C25 C26 121.6(10) . . . . ? O24 C25 C26 O27 -78.7(13) . . . . ? C25 C26 O27 C28 174.9(10) . . . . ? C26 O27 C28 C29 -175.8(9) . . . . ? O27 C28 C29 O30 64.6(10) . . . . ? C28 C29 O30 C31 -110.3(8) . . . . ? C29 O30 C31 C32 150.7(7) . . . . ? O30 C31 C32 S21 -57.7(8) . . . . ? N1 S21 C32 C31 -176.0(6) . . . . ? C22 S21 C32 C31 -73.8(6) . . . . ? C59 B40 C41 C46 -171.3(6) . . . . ? C53 B40 C41 C46 68.5(8) . . . . ? C47 B40 C41 C46 -54.0(8) . . . . ? C59 B40 C41 C42 8.4(8) . . . . ? C53 B40 C41 C42 -111.8(7) . . . . ? C47 B40 C41 C42 125.7(6) . . . . ? C46 C41 C42 C43 0.5(9) . . . . ? B40 C41 C42 C43 -179.2(5) . . . . ? C41 C42 C43 C44 0.6(9) . . . . ? C42 C43 C44 C45 -1.1(9) . . . . ? C43 C44 C45 C46 0.5(10) . . . . ? C42 C41 C46 C45 -1.2(10) . . . . ? B40 C41 C46 C45 178.5(6) . . . . ? C44 C45 C46 C41 0.8(10) . . . . ? C41 B40 C47 C48 161.3(6) . . . . ? C59 B40 C47 C48 -81.2(7) . . . . ? C53 B40 C47 C48 37.6(8) . . . . ? C41 B40 C47 C52 -19.7(8) . . . . ? C59 B40 C47 C52 97.8(7) . . . . ? C53 B40 C47 C52 -143.4(6) . . . . ? C52 C47 C48 C49 -3.6(9) . . . . ? B40 C47 C48 C49 175.5(6) . . . . ? C47 C48 C49 C50 2.4(10) . . . . ? C48 C49 C50 C51 -0.7(10) . . . . ? C49 C50 C51 C52 0.5(10) . . . . ? C50 C51 C52 C47 -2.1(11) . . . . ? C48 C47 C52 C51 3.5(10) . . . . ? B40 C47 C52 C51 -175.6(6) . . . . ? C41 B40 C53 C58 -19.4(8) . . . . ? C59 B40 C53 C58 -139.1(6) . . . . ? C47 B40 C53 C58 102.8(7) . . . . ? C41 B40 C53 C54 162.2(6) . . . . ? C59 B40 C53 C54 42.6(8) . . . . ? C47 B40 C53 C54 -75.5(7) . . . . ? C58 C53 C54 C55 -2.2(10) . . . . ? B40 C53 C54 C55 176.3(6) . . . . ? C53 C54 C55 C56 1.6(11) . . . . ? C54 C55 C56 C57 0.9(11) . . . . ? C55 C56 C57 C58 -2.6(11) . . . . ? C54 C53 C58 C57 0.4(9) . . . . ? B40 C53 C58 C57 -178.0(6) . . . . ? C56 C57 C58 C53 2.0(10) . . . . ? C41 B40 C59 C64 82.4(7) . . . . ? C53 B40 C59 C64 -155.4(6) . . . . ? C47 B40 C59 C64 -36.0(8) . . . . ? C41 B40 C59 C60 -88.2(7) . . . . ? C53 B40 C59 C60 34.0(8) . . . . ? C47 B40 C59 C60 153.4(5) . . . . ? C64 C59 C60 C61 0.3(9) . . . . ? B40 C59 C60 C61 171.5(6) . . . . ? C59 C60 C61 C62 1.2(10) . . . . ? C60 C61 C62 C63 -1.6(10) . . . . ? C61 C62 C63 C64 0.5(11) . . . . ? C62 C63 C64 C59 1.0(10) . . . . ? C60 C59 C64 C63 -1.4(9) . . . . ? B40 C59 C64 C63 -172.6(6) . . . . ? _diffrn_measured_fraction_theta_max 0.903 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 0.889 _refine_diff_density_min -0.846 _refine_diff_density_rms 0.108 #===END data_[6][BPh4] _database_code_depnum_ccdc_archive 'CCDC 678822' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H20 B 1-, C12 H24 N O4 S 1+' _chemical_formula_sum 'C36 H44 B N O4 S2' _chemical_formula_weight 629.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6347(5) _cell_length_b 14.3378(7) _cell_length_c 22.9147(11) _cell_angle_alpha 78.764(2) _cell_angle_beta 81.805(2) _cell_angle_gamma 71.051(2) _cell_volume 3229.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9006 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 28.66 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.295 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 0.206 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.878 _exptl_absorpt_correction_T_max 0.976 _exptl_absorpt_process_details 'SADABS v2.10, Sheldrick, G.M., (2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 28453 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 0.91 _diffrn_reflns_theta_max 28.90 _reflns_number_total 14816 _reflns_number_gt 10459 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0605P)^2^+0.9348P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14816 _refine_ls_number_parameters 793 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0740 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1268 _refine_ls_wR_factor_gt 0.1103 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.32936(16) 0.87788(13) 0.40752(7) 0.0261(4) Uani 1 1 d . . . S1 S 0.40784(5) 0.85319(4) 0.34234(2) 0.02527(12) Uani 1 1 d . . . C1 C 0.4125(2) 0.72594(15) 0.34200(10) 0.0303(5) Uani 1 1 d . . . H1A H 0.4267 0.6866 0.3824 0.036 Uiso 1 1 calc R . . H1B H 0.3264 0.7253 0.3306 0.036 Uiso 1 1 calc R . . C2 C 0.5247(2) 0.68017(17) 0.29791(10) 0.0335(5) Uani 1 1 d . . . H2A H 0.5280 0.6102 0.2983 0.040 Uiso 1 1 calc R . . H2B H 0.5059 0.7172 0.2573 0.040 Uiso 1 1 calc R . . O1 O 0.65038(15) 0.68130(11) 0.31043(7) 0.0340(4) Uani 1 1 d . . . C3 C 0.7080(2) 0.60877(16) 0.35962(10) 0.0337(5) Uani 1 1 d . . . H3A H 0.7943 0.5637 0.3453 0.040 Uiso 1 1 calc R . . H3B H 0.6480 0.5679 0.3761 0.040 Uiso 1 1 calc R . . C4 C 0.7300(2) 0.65706(17) 0.40790(10) 0.0335(5) Uani 1 1 d . . . H4A H 0.7801 0.6053 0.4387 0.040 Uiso 1 1 calc R . . H4B H 0.7835 0.7026 0.3910 0.040 Uiso 1 1 calc R . . O2 O 0.60558(14) 0.71161(11) 0.43425(6) 0.0306(3) Uani 1 1 d . . . C5 C 0.6212(2) 0.75232(16) 0.48368(9) 0.0308(5) Uani 1 1 d . . . H5A H 0.6849 0.7913 0.4719 0.037 Uiso 1 1 calc R . . H5B H 0.6559 0.6981 0.5168 0.037 Uiso 1 1 calc R . . C6 C 0.4859(2) 0.81893(16) 0.50320(9) 0.0302(5) Uani 1 1 d . . . H6A H 0.4928 0.8487 0.5377 0.036 Uiso 1 1 calc R . . H6B H 0.4232 0.7792 0.5158 0.036 Uiso 1 1 calc R . . S2 S 0.42421(5) 0.91665(4) 0.44198(2) 0.02442(12) Uani 1 1 d . . . C7 C 0.3007(2) 1.00480(16) 0.48278(10) 0.0324(5) Uani 1 1 d . . . H7A H 0.2344 0.9732 0.5053 0.039 Uiso 1 1 calc R . . H7B H 0.3440 1.0243 0.5119 0.039 Uiso 1 1 calc R . . C8 C 0.2311(2) 1.09606(17) 0.44124(10) 0.0337(5) Uani 1 1 d . . . H8A H 0.1861 1.0774 0.4124 0.040 Uiso 1 1 calc R . . H8B H 0.1627 1.1437 0.4642 0.040 Uiso 1 1 calc R . . O3 O 0.32852(15) 1.14105(11) 0.41029(7) 0.0341(4) Uani 1 1 d . . . C9 C 0.2842(2) 1.20819(17) 0.35655(11) 0.0391(6) Uani 1 1 d . . . H9A H 0.3200 1.2653 0.3513 0.047 Uiso 1 1 calc R . . H9B H 0.1855 1.2348 0.3603 0.047 Uiso 1 1 calc R . . C10 C 0.3287(2) 1.15725(17) 0.30291(10) 0.0373(5) Uani 1 1 d . . . H10A H 0.2923 1.2034 0.2669 0.045 Uiso 1 1 calc R . . H10B H 0.4273 1.1354 0.2965 0.045 Uiso 1 1 calc R . . O4 O 0.28004(16) 1.07280(11) 0.31382(7) 0.0384(4) Uani 1 1 d . . . C11 C 0.3022(3) 1.02183(17) 0.26492(10) 0.0386(6) Uani 1 1 d . . . H11A H 0.3931 1.0154 0.2451 0.046 Uiso 1 1 calc R . . H11B H 0.2366 1.0587 0.2354 0.046 Uiso 1 1 calc R . . C12 C 0.2870(2) 0.91965(16) 0.28897(10) 0.0344(5) Uani 1 1 d . . . H12A H 0.3005 0.8815 0.2557 0.041 Uiso 1 1 calc R . . H12B H 0.1958 0.9268 0.3084 0.041 Uiso 1 1 calc R . . N2 N 0.69280(16) 0.09136(13) 0.10960(7) 0.0257(4) Uani 1 1 d . . . S3 S 0.57176(5) 0.08071(4) 0.07607(2) 0.02480(12) Uani 1 1 d . . . C13 C 0.6702(2) 0.01057(16) 0.01925(9) 0.0293(5) Uani 1 1 d . . . H13A H 0.6123 0.0106 -0.0109 0.035 Uiso 1 1 calc R . . H13B H 0.7385 0.0419 -0.0011 0.035 Uiso 1 1 calc R . . C14 C 0.7368(2) -0.09465(16) 0.04733(10) 0.0313(5) Uani 1 1 d . . . H14A H 0.7923 -0.1339 0.0167 0.038 Uiso 1 1 calc R . . H14B H 0.7948 -0.0954 0.0777 0.038 Uiso 1 1 calc R . . O5 O 0.63369(14) -0.13578(11) 0.07441(7) 0.0319(3) Uani 1 1 d . . . C15 C 0.6782(2) -0.22763(16) 0.11467(11) 0.0348(5) Uani 1 1 d . . . H15A H 0.7426 -0.2780 0.0922 0.042 Uiso 1 1 calc R . . H15B H 0.6008 -0.2520 0.1300 0.042 Uiso 1 1 calc R . . C16 C 0.7433(2) -0.21998(16) 0.16703(10) 0.0337(5) Uani 1 1 d . . . H16A H 0.7613 -0.2837 0.1953 0.040 Uiso 1 1 calc R . . H16B H 0.8294 -0.2068 0.1530 0.040 Uiso 1 1 calc R . . O6 O 0.65667(14) -0.14072(11) 0.19627(7) 0.0327(3) Uani 1 1 d . . . C17 C 0.7208(2) -0.11726(16) 0.23958(10) 0.0322(5) Uani 1 1 d . . . H17A H 0.7890 -0.1784 0.2565 0.039 Uiso 1 1 calc R . . H17B H 0.6541 -0.0936 0.2725 0.039 Uiso 1 1 calc R . . C18 C 0.7873(2) -0.03705(15) 0.21256(9) 0.0289(5) Uani 1 1 d . . . H18A H 0.8560 -0.0610 0.1803 0.035 Uiso 1 1 calc R . . H18B H 0.8317 -0.0231 0.2436 0.035 Uiso 1 1 calc R . . S4 S 0.66278(5) 0.07634(4) 0.18265(2) 0.02397(12) Uani 1 1 d . . . C19 C 0.7311(2) 0.16742(16) 0.19851(9) 0.0302(5) Uani 1 1 d . . . H19A H 0.7351 0.1603 0.2421 0.036 Uiso 1 1 calc R . . H19B H 0.8228 0.1568 0.1790 0.036 Uiso 1 1 calc R . . C20 C 0.6438(2) 0.27037(16) 0.17537(10) 0.0336(5) Uani 1 1 d . . . H20A H 0.6727 0.3219 0.1879 0.040 Uiso 1 1 calc R . . H20B H 0.6482 0.2813 0.1312 0.040 Uiso 1 1 calc R . . O7 O 0.51182(16) 0.27503(11) 0.20034(7) 0.0366(4) Uani 1 1 d . . . C21 C 0.4086(2) 0.36041(17) 0.17576(11) 0.0394(6) Uani 1 1 d . . . H21A H 0.4318 0.4215 0.1769 0.047 Uiso 1 1 calc R . . H21B H 0.3242 0.3638 0.2011 0.047 Uiso 1 1 calc R . . C22 C 0.3868(2) 0.35895(17) 0.11283(11) 0.0381(5) Uani 1 1 d . . . H22A H 0.3126 0.4184 0.0989 0.046 Uiso 1 1 calc R . . H22B H 0.4683 0.3608 0.0863 0.046 Uiso 1 1 calc R . . O8 O 0.35548(16) 0.26993(11) 0.11056(7) 0.0385(4) Uani 1 1 d . . . C23 C 0.3640(2) 0.25152(18) 0.05129(11) 0.0380(5) Uani 1 1 d . . . H23A H 0.3298 0.3158 0.0247 0.046 Uiso 1 1 calc R . . H23B H 0.3069 0.2097 0.0498 0.046 Uiso 1 1 calc R . . C24 C 0.5061(2) 0.19918(16) 0.02878(9) 0.0318(5) Uani 1 1 d . . . H24A H 0.5629 0.2420 0.0284 0.038 Uiso 1 1 calc R . . H24B H 0.5078 0.1879 -0.0126 0.038 Uiso 1 1 calc R . . B1 B 0.1997(2) 0.71502(16) 0.12290(10) 0.0216(4) Uani 1 1 d . . . C25 C 0.11941(19) 0.69477(14) 0.07232(9) 0.0222(4) Uani 1 1 d . . . C26 C 0.1369(2) 0.73599(15) 0.01194(9) 0.0274(4) Uani 1 1 d . . . H26 H 0.1891 0.7804 0.0017 0.033 Uiso 1 1 calc R . . C27 C 0.0815(2) 0.71488(16) -0.03346(9) 0.0317(5) Uani 1 1 d . . . H27 H 0.0976 0.7437 -0.0737 0.038 Uiso 1 1 calc R . . C28 C 0.0031(2) 0.65215(17) -0.02024(10) 0.0366(5) Uani 1 1 d . . . H28 H -0.0352 0.6375 -0.0510 0.044 Uiso 1 1 calc R . . C29 C -0.0188(2) 0.61089(17) 0.03894(10) 0.0347(5) Uani 1 1 d . . . H29 H -0.0725 0.5676 0.0489 0.042 Uiso 1 1 calc R . . C30 C 0.0377(2) 0.63274(15) 0.08360(9) 0.0276(4) Uani 1 1 d . . . H30 H 0.0201 0.6042 0.1237 0.033 Uiso 1 1 calc R . . C31 C 0.35623(19) 0.64247(14) 0.11818(8) 0.0214(4) Uani 1 1 d . . . C32 C 0.4233(2) 0.60280(14) 0.06698(9) 0.0248(4) Uani 1 1 d . . . H32 H 0.3754 0.6156 0.0328 0.030 Uiso 1 1 calc R . . C33 C 0.5570(2) 0.54554(15) 0.06396(9) 0.0294(5) Uani 1 1 d . . . H33 H 0.5981 0.5208 0.0281 0.035 Uiso 1 1 calc R . . C34 C 0.6304(2) 0.52424(15) 0.11264(10) 0.0285(5) Uani 1 1 d . . . H34 H 0.7218 0.4854 0.1106 0.034 Uiso 1 1 calc R . . C35 C 0.5677(2) 0.56092(15) 0.16460(9) 0.0268(4) Uani 1 1 d . . . H35 H 0.6164 0.5470 0.1986 0.032 Uiso 1 1 calc R . . C36 C 0.4341(2) 0.61793(14) 0.16709(9) 0.0248(4) Uani 1 1 d . . . H36 H 0.3934 0.6414 0.2034 0.030 Uiso 1 1 calc R . . C37 C 0.13708(18) 0.68858(15) 0.19206(9) 0.0238(4) Uani 1 1 d . . . C38 C 0.1357(2) 0.59084(16) 0.21634(9) 0.0288(5) Uani 1 1 d . . . H38 H 0.1666 0.5410 0.1913 0.035 Uiso 1 1 calc R . . C39 C 0.0911(2) 0.56395(19) 0.27523(10) 0.0365(5) Uani 1 1 d . . . H39 H 0.0889 0.4976 0.2893 0.044 Uiso 1 1 calc R . . C40 C 0.0500(2) 0.6339(2) 0.31342(10) 0.0411(6) Uani 1 1 d . . . H40 H 0.0213 0.6156 0.3540 0.049 Uiso 1 1 calc R . . C41 C 0.0510(2) 0.7300(2) 0.29219(10) 0.0390(6) Uani 1 1 d . . . H41 H 0.0232 0.7784 0.3182 0.047 Uiso 1 1 calc R . . C42 C 0.09280(19) 0.75701(17) 0.23234(9) 0.0296(5) Uani 1 1 d . . . H42 H 0.0911 0.8243 0.2185 0.036 Uiso 1 1 calc R . . C43 C 0.19264(19) 0.83334(14) 0.11215(8) 0.0219(4) Uani 1 1 d . . . C44 C 0.2911(2) 0.86629(15) 0.12894(9) 0.0261(4) Uani 1 1 d . . . H44 H 0.3715 0.8178 0.1414 0.031 Uiso 1 1 calc R . . C45 C 0.2763(2) 0.96654(16) 0.12811(9) 0.0305(5) Uani 1 1 d . . . H45 H 0.3457 0.9851 0.1399 0.037 Uiso 1 1 calc R . . C46 C 0.1604(2) 1.03937(16) 0.11003(9) 0.0320(5) Uani 1 1 d . . . H46 H 0.1487 1.1079 0.1103 0.038 Uiso 1 1 calc R . . C47 C 0.0615(2) 1.01051(16) 0.09154(10) 0.0323(5) Uani 1 1 d . . . H47 H -0.0178 1.0595 0.0783 0.039 Uiso 1 1 calc R . . C48 C 0.0791(2) 0.90996(15) 0.09248(9) 0.0280(4) Uani 1 1 d . . . H48 H 0.0108 0.8921 0.0791 0.034 Uiso 1 1 calc R . . B2 B 0.7886(2) 0.28232(16) 0.36225(10) 0.0206(4) Uani 1 1 d . . . C49 C 0.86032(19) 0.31288(14) 0.29539(9) 0.0231(4) Uani 1 1 d . . . C50 C 0.8301(2) 0.41218(15) 0.26707(9) 0.0258(4) Uani 1 1 d . . . H50 H 0.7595 0.4611 0.2848 0.031 Uiso 1 1 calc R . . C51 C 0.8983(2) 0.44313(16) 0.21419(9) 0.0304(5) Uani 1 1 d . . . H51 H 0.8751 0.5118 0.1972 0.037 Uiso 1 1 calc R . . C52 C 0.9995(2) 0.37407(17) 0.18641(9) 0.0331(5) Uani 1 1 d . . . H52 H 1.0470 0.3946 0.1505 0.040 Uiso 1 1 calc R . . C53 C 1.0306(2) 0.27482(18) 0.21171(10) 0.0358(5) Uani 1 1 d . . . H53 H 1.0990 0.2263 0.1927 0.043 Uiso 1 1 calc R . . C54 C 0.9622(2) 0.24489(16) 0.26510(9) 0.0305(5) Uani 1 1 d . . . H54 H 0.9856 0.1759 0.2815 0.037 Uiso 1 1 calc R . . C55 C 0.79054(19) 0.16489(14) 0.36973(9) 0.0229(4) Uani 1 1 d . . . C56 C 0.6828(2) 0.13519(15) 0.35941(8) 0.0248(4) Uani 1 1 d . . . H56 H 0.6008 0.1852 0.3507 0.030 Uiso 1 1 calc R . . C57 C 0.6914(2) 0.03584(16) 0.36144(9) 0.0307(5) Uani 1 1 d . . . H57 H 0.6162 0.0195 0.3539 0.037 Uiso 1 1 calc R . . C58 C 0.8084(2) -0.03927(16) 0.37427(10) 0.0350(5) Uani 1 1 d . . . H58 H 0.8145 -0.1072 0.3754 0.042 Uiso 1 1 calc R . . C59 C 0.9169(2) -0.01389(16) 0.38549(10) 0.0363(5) Uani 1 1 d . . . H59 H 0.9982 -0.0645 0.3945 0.044 Uiso 1 1 calc R . . C60 C 0.9062(2) 0.08594(16) 0.38353(10) 0.0311(5) Uani 1 1 d . . . H60 H 0.9814 0.1014 0.3920 0.037 Uiso 1 1 calc R . . C61 C 0.87196(18) 0.29673(14) 0.41342(9) 0.0227(4) Uani 1 1 d . . . C62 C 0.8586(2) 0.25172(16) 0.47329(9) 0.0282(4) Uani 1 1 d . . . H62 H 0.8116 0.2038 0.4829 0.034 Uiso 1 1 calc R . . C63 C 0.9112(2) 0.27421(17) 0.51905(10) 0.0356(5) Uani 1 1 d . . . H63 H 0.8974 0.2435 0.5591 0.043 Uiso 1 1 calc R . . C64 C 0.9835(2) 0.34117(18) 0.50638(10) 0.0386(6) Uani 1 1 d . . . H64 H 1.0190 0.3573 0.5375 0.046 Uiso 1 1 calc R . . C65 C 1.0038(2) 0.38472(17) 0.44748(10) 0.0347(5) Uani 1 1 d . . . H65 H 1.0556 0.4295 0.4380 0.042 Uiso 1 1 calc R . . C66 C 0.9483(2) 0.36260(15) 0.40266(9) 0.0270(4) Uani 1 1 d . . . H66 H 0.9628 0.3936 0.3628 0.032 Uiso 1 1 calc R . . C67 C 0.63431(19) 0.35695(14) 0.36995(9) 0.0222(4) Uani 1 1 d . . . C68 C 0.5776(2) 0.40041(15) 0.42127(9) 0.0263(4) Uani 1 1 d . . . H68 H 0.6314 0.3869 0.4535 0.032 Uiso 1 1 calc R . . C69 C 0.4464(2) 0.46225(16) 0.42732(10) 0.0325(5) Uani 1 1 d . . . H69 H 0.4127 0.4893 0.4631 0.039 Uiso 1 1 calc R . . C70 C 0.3653(2) 0.48430(16) 0.38113(11) 0.0341(5) Uani 1 1 d . . . H70 H 0.2759 0.5267 0.3847 0.041 Uiso 1 1 calc R . . C71 C 0.4168(2) 0.44345(16) 0.32972(10) 0.0320(5) Uani 1 1 d . . . H71 H 0.3624 0.4577 0.2977 0.038 Uiso 1 1 calc R . . C72 C 0.5480(2) 0.38152(15) 0.32460(9) 0.0281(4) Uani 1 1 d . . . H72 H 0.5806 0.3546 0.2887 0.034 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0263(9) 0.0316(10) 0.0237(9) -0.0078(7) -0.0006(7) -0.0119(7) S1 0.0281(3) 0.0260(3) 0.0233(2) -0.0068(2) -0.0012(2) -0.0092(2) C1 0.0339(12) 0.0270(11) 0.0337(12) -0.0090(9) -0.0023(9) -0.0121(9) C2 0.0367(12) 0.0340(12) 0.0327(12) -0.0132(10) -0.0025(10) -0.0103(10) O1 0.0338(8) 0.0339(9) 0.0346(8) -0.0071(7) -0.0019(7) -0.0105(7) C3 0.0326(12) 0.0264(11) 0.0407(13) -0.0086(10) -0.0012(10) -0.0058(9) C4 0.0282(11) 0.0312(12) 0.0389(13) -0.0079(10) -0.0051(9) -0.0037(9) O2 0.0284(8) 0.0331(8) 0.0311(8) -0.0102(7) -0.0034(6) -0.0073(6) C5 0.0323(12) 0.0334(12) 0.0277(11) -0.0036(9) -0.0071(9) -0.0105(9) C6 0.0326(12) 0.0365(12) 0.0220(10) -0.0029(9) -0.0017(9) -0.0127(10) S2 0.0252(3) 0.0277(3) 0.0226(2) -0.0071(2) 0.00077(19) -0.0106(2) C7 0.0331(12) 0.0378(13) 0.0307(11) -0.0167(10) 0.0060(9) -0.0137(10) C8 0.0254(11) 0.0377(13) 0.0393(13) -0.0162(10) 0.0025(9) -0.0078(9) O3 0.0326(8) 0.0355(9) 0.0372(9) -0.0080(7) -0.0048(7) -0.0123(7) C9 0.0370(13) 0.0269(12) 0.0527(15) -0.0037(11) -0.0134(11) -0.0063(10) C10 0.0424(13) 0.0302(12) 0.0399(13) 0.0044(10) -0.0105(11) -0.0149(10) O4 0.0522(10) 0.0322(9) 0.0334(9) -0.0064(7) -0.0048(7) -0.0152(8) C11 0.0492(14) 0.0348(13) 0.0268(11) -0.0029(10) -0.0088(10) -0.0048(11) C12 0.0383(13) 0.0347(13) 0.0302(12) -0.0078(10) -0.0107(10) -0.0066(10) N2 0.0270(9) 0.0336(10) 0.0202(8) -0.0053(7) -0.0014(7) -0.0142(8) S3 0.0265(3) 0.0270(3) 0.0238(2) -0.0049(2) -0.0012(2) -0.0119(2) C13 0.0338(12) 0.0343(12) 0.0254(10) -0.0112(9) 0.0020(9) -0.0162(10) C14 0.0302(11) 0.0354(12) 0.0330(12) -0.0129(10) 0.0037(9) -0.0146(10) O5 0.0282(8) 0.0312(8) 0.0406(9) -0.0072(7) -0.0030(7) -0.0138(7) C15 0.0321(12) 0.0243(11) 0.0488(14) -0.0077(10) -0.0003(10) -0.0098(9) C16 0.0305(12) 0.0240(11) 0.0416(13) -0.0037(10) 0.0024(10) -0.0050(9) O6 0.0303(8) 0.0257(8) 0.0397(9) -0.0047(7) -0.0029(7) -0.0056(6) C17 0.0340(12) 0.0276(12) 0.0306(11) 0.0022(9) -0.0042(9) -0.0071(9) C18 0.0291(11) 0.0291(11) 0.0262(11) -0.0030(9) -0.0027(9) -0.0063(9) S4 0.0274(3) 0.0243(3) 0.0202(2) -0.00379(19) -0.00020(19) -0.0086(2) C19 0.0408(13) 0.0350(12) 0.0214(10) -0.0063(9) -0.0031(9) -0.0193(10) C20 0.0483(14) 0.0274(12) 0.0291(11) -0.0064(9) 0.0021(10) -0.0182(10) O7 0.0453(9) 0.0267(8) 0.0342(9) -0.0045(7) 0.0075(7) -0.0108(7) C21 0.0472(14) 0.0238(12) 0.0438(14) -0.0072(10) 0.0057(11) -0.0091(10) C22 0.0415(13) 0.0256(12) 0.0462(14) -0.0044(10) 0.0011(11) -0.0117(10) O8 0.0399(9) 0.0312(9) 0.0466(10) -0.0080(7) 0.0057(7) -0.0164(7) C23 0.0323(12) 0.0341(13) 0.0502(15) -0.0047(11) -0.0099(11) -0.0121(10) C24 0.0376(12) 0.0325(12) 0.0257(11) 0.0003(9) -0.0078(9) -0.0118(10) B1 0.0212(11) 0.0214(11) 0.0211(11) -0.0021(9) -0.0014(9) -0.0060(9) C25 0.0227(10) 0.0192(10) 0.0231(10) -0.0032(8) -0.0017(8) -0.0045(8) C26 0.0262(11) 0.0268(11) 0.0282(11) -0.0025(9) -0.0025(8) -0.0075(9) C27 0.0355(12) 0.0333(12) 0.0221(10) -0.0040(9) -0.0057(9) -0.0036(10) C28 0.0402(13) 0.0363(13) 0.0364(13) -0.0163(10) -0.0117(10) -0.0062(10) C29 0.0386(13) 0.0318(12) 0.0405(13) -0.0114(10) -0.0057(10) -0.0158(10) C30 0.0307(11) 0.0266(11) 0.0271(11) -0.0051(9) -0.0022(9) -0.0104(9) C31 0.0246(10) 0.0161(9) 0.0233(10) -0.0009(8) -0.0011(8) -0.0077(8) C32 0.0277(10) 0.0233(10) 0.0223(10) -0.0027(8) -0.0017(8) -0.0072(8) C33 0.0334(12) 0.0229(11) 0.0296(11) -0.0058(9) 0.0039(9) -0.0072(9) C34 0.0233(10) 0.0203(10) 0.0384(12) -0.0019(9) 0.0005(9) -0.0048(8) C35 0.0261(10) 0.0236(10) 0.0297(11) -0.0015(9) -0.0061(9) -0.0066(8) C36 0.0263(10) 0.0234(10) 0.0248(10) -0.0047(8) -0.0011(8) -0.0078(8) C37 0.0157(9) 0.0299(11) 0.0247(10) -0.0035(8) -0.0026(8) -0.0056(8) C38 0.0256(11) 0.0314(12) 0.0275(11) -0.0010(9) -0.0028(9) -0.0081(9) C39 0.0263(11) 0.0462(14) 0.0321(12) 0.0099(10) -0.0055(9) -0.0125(10) C40 0.0236(11) 0.0673(18) 0.0231(11) 0.0028(11) 0.0005(9) -0.0081(11) C41 0.0264(11) 0.0583(16) 0.0284(12) -0.0157(11) -0.0007(9) -0.0030(11) C42 0.0220(10) 0.0357(12) 0.0288(11) -0.0085(9) -0.0024(8) -0.0036(9) C43 0.0228(10) 0.0214(10) 0.0201(9) -0.0038(8) 0.0018(8) -0.0061(8) C44 0.0268(10) 0.0277(11) 0.0245(10) -0.0058(8) -0.0014(8) -0.0086(9) C45 0.0385(12) 0.0342(12) 0.0248(11) -0.0082(9) 0.0016(9) -0.0190(10) C46 0.0452(13) 0.0218(11) 0.0299(11) -0.0092(9) 0.0098(10) -0.0139(10) C47 0.0305(11) 0.0231(11) 0.0356(12) -0.0031(9) 0.0057(9) -0.0023(9) C48 0.0240(10) 0.0270(11) 0.0317(11) -0.0044(9) 0.0014(9) -0.0078(9) B2 0.0197(10) 0.0198(11) 0.0218(11) -0.0027(9) -0.0037(8) -0.0050(8) C49 0.0243(10) 0.0236(10) 0.0224(10) -0.0039(8) -0.0063(8) -0.0068(8) C50 0.0260(10) 0.0249(11) 0.0263(10) -0.0059(8) -0.0027(8) -0.0060(8) C51 0.0356(12) 0.0272(11) 0.0281(11) 0.0016(9) -0.0058(9) -0.0114(9) C52 0.0322(12) 0.0446(14) 0.0225(10) -0.0033(10) -0.0004(9) -0.0136(10) C53 0.0344(12) 0.0392(13) 0.0287(11) -0.0106(10) 0.0040(9) -0.0041(10) C54 0.0324(12) 0.0258(11) 0.0299(11) -0.0047(9) -0.0018(9) -0.0042(9) C55 0.0233(10) 0.0227(10) 0.0223(10) -0.0048(8) 0.0012(8) -0.0071(8) C56 0.0280(11) 0.0258(11) 0.0202(10) -0.0052(8) 0.0002(8) -0.0077(8) C57 0.0408(13) 0.0330(12) 0.0239(10) -0.0081(9) 0.0028(9) -0.0193(10) C58 0.0516(14) 0.0222(11) 0.0301(11) -0.0081(9) 0.0101(10) -0.0130(10) C59 0.0339(12) 0.0239(11) 0.0405(13) -0.0024(10) 0.0061(10) -0.0002(9) C60 0.0255(11) 0.0276(11) 0.0373(12) -0.0020(9) -0.0010(9) -0.0067(9) C61 0.0185(9) 0.0217(10) 0.0262(10) -0.0042(8) -0.0027(8) -0.0034(8) C62 0.0245(10) 0.0312(11) 0.0272(11) 0.0002(9) -0.0048(8) -0.0082(9) C63 0.0335(12) 0.0423(14) 0.0257(11) -0.0022(10) -0.0072(9) -0.0043(10) C64 0.0394(13) 0.0448(14) 0.0343(12) -0.0141(11) -0.0140(10) -0.0075(11) C65 0.0327(12) 0.0355(13) 0.0413(13) -0.0091(10) -0.0091(10) -0.0133(10) C66 0.0270(11) 0.0256(11) 0.0274(11) -0.0040(8) -0.0048(8) -0.0057(8) C67 0.0232(10) 0.0167(9) 0.0266(10) -0.0025(8) -0.0035(8) -0.0060(8) C68 0.0271(11) 0.0243(11) 0.0282(11) -0.0054(8) -0.0031(8) -0.0076(8) C69 0.0316(12) 0.0278(12) 0.0339(12) -0.0077(9) 0.0043(9) -0.0046(9) C70 0.0221(11) 0.0253(11) 0.0481(14) -0.0008(10) -0.0026(10) -0.0011(9) C71 0.0256(11) 0.0286(12) 0.0398(13) 0.0001(10) -0.0104(9) -0.0053(9) C72 0.0270(11) 0.0266(11) 0.0301(11) -0.0048(9) -0.0055(9) -0.0059(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 S1 1.6465(17) . ? N1 S2 1.6469(17) . ? S1 C12 1.804(2) . ? S1 C1 1.811(2) . ? C1 C2 1.511(3) . ? C2 O1 1.412(3) . ? O1 C3 1.433(3) . ? C3 C4 1.495(3) . ? C4 O2 1.418(2) . ? O2 C5 1.423(2) . ? C5 C6 1.507(3) . ? C6 S2 1.806(2) . ? S2 C7 1.797(2) . ? C7 C8 1.501(3) . ? C8 O3 1.428(3) . ? O3 C9 1.440(3) . ? C9 C10 1.492(3) . ? C10 O4 1.431(3) . ? O4 C11 1.406(3) . ? C11 C12 1.514(3) . ? N2 S4 1.6439(16) . ? N2 S3 1.6510(16) . ? S3 C13 1.800(2) . ? S3 C24 1.810(2) . ? C13 C14 1.500(3) . ? C14 O5 1.421(2) . ? O5 C15 1.434(3) . ? C15 C16 1.506(3) . ? C16 O6 1.425(2) . ? O6 C17 1.427(3) . ? C17 C18 1.527(3) . ? C18 S4 1.815(2) . ? S4 C19 1.801(2) . ? C19 C20 1.506(3) . ? C20 O7 1.424(3) . ? O7 C21 1.434(3) . ? C21 C22 1.498(3) . ? C22 O8 1.432(3) . ? O8 C23 1.418(3) . ? C23 C24 1.518(3) . ? B1 C43 1.644(3) . ? B1 C37 1.652(3) . ? B1 C25 1.653(3) . ? B1 C31 1.653(3) . ? C25 C30 1.400(3) . ? C25 C26 1.406(3) . ? C26 C27 1.391(3) . ? C27 C28 1.380(3) . ? C28 C29 1.389(3) . ? C29 C30 1.389(3) . ? C31 C32 1.402(3) . ? C31 C36 1.410(3) . ? C32 C33 1.391(3) . ? C33 C34 1.382(3) . ? C34 C35 1.389(3) . ? C35 C36 1.390(3) . ? C37 C42 1.402(3) . ? C37 C38 1.407(3) . ? C38 C39 1.389(3) . ? C39 C40 1.382(3) . ? C40 C41 1.372(4) . ? C41 C42 1.400(3) . ? C43 C48 1.403(3) . ? C43 C44 1.405(3) . ? C44 C45 1.391(3) . ? C45 C46 1.387(3) . ? C46 C47 1.390(3) . ? C47 C48 1.388(3) . ? B2 C61 1.647(3) . ? B2 C67 1.649(3) . ? B2 C55 1.653(3) . ? B2 C49 1.656(3) . ? C49 C50 1.398(3) . ? C49 C54 1.403(3) . ? C50 C51 1.393(3) . ? C51 C52 1.379(3) . ? C52 C53 1.378(3) . ? C53 C54 1.398(3) . ? C55 C60 1.401(3) . ? C55 C56 1.408(3) . ? C56 C57 1.389(3) . ? C57 C58 1.380(3) . ? C58 C59 1.386(3) . ? C59 C60 1.391(3) . ? C61 C66 1.401(3) . ? C61 C62 1.406(3) . ? C62 C63 1.390(3) . ? C63 C64 1.380(3) . ? C64 C65 1.391(3) . ? C65 C66 1.388(3) . ? C67 C72 1.402(3) . ? C67 C68 1.405(3) . ? C68 C69 1.393(3) . ? C69 C70 1.385(3) . ? C70 C71 1.381(3) . ? C71 C72 1.392(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 N1 S2 107.97(10) . . ? N1 S1 C12 104.78(10) . . ? N1 S1 C1 103.95(9) . . ? C12 S1 C1 100.39(10) . . ? C2 C1 S1 109.17(15) . . ? O1 C2 C1 112.99(17) . . ? C2 O1 C3 115.21(17) . . ? O1 C3 C4 111.67(18) . . ? O2 C4 C3 109.96(17) . . ? C4 O2 C5 111.95(16) . . ? O2 C5 C6 107.48(17) . . ? C5 C6 S2 109.38(14) . . ? N1 S2 C7 101.20(10) . . ? N1 S2 C6 106.86(10) . . ? C7 S2 C6 99.56(10) . . ? C8 C7 S2 110.80(15) . . ? O3 C8 C7 108.24(17) . . ? C8 O3 C9 113.14(17) . . ? O3 C9 C10 111.59(18) . . ? O4 C10 C9 107.16(19) . . ? C11 O4 C10 114.43(18) . . ? O4 C11 C12 107.14(18) . . ? C11 C12 S1 109.72(16) . . ? S4 N2 S3 112.22(10) . . ? N2 S3 C13 99.45(9) . . ? N2 S3 C24 106.52(10) . . ? C13 S3 C24 98.36(10) . . ? C14 C13 S3 109.43(14) . . ? O5 C14 C13 106.92(17) . . ? C14 O5 C15 114.36(16) . . ? O5 C15 C16 114.49(17) . . ? O6 C16 C15 109.09(17) . . ? C16 O6 C17 112.20(16) . . ? O6 C17 C18 111.78(17) . . ? C17 C18 S4 109.72(14) . . ? N2 S4 C19 99.26(9) . . ? N2 S4 C18 107.09(9) . . ? C19 S4 C18 99.43(10) . . ? C20 C19 S4 108.96(15) . . ? O7 C20 C19 106.08(17) . . ? C20 O7 C21 115.25(17) . . ? O7 C21 C22 113.58(18) . . ? O8 C22 C21 109.23(19) . . ? C23 O8 C22 112.36(17) . . ? O8 C23 C24 112.11(18) . . ? C23 C24 S3 110.48(16) . . ? C43 B1 C37 106.97(15) . . ? C43 B1 C25 110.08(16) . . ? C37 B1 C25 113.24(16) . . ? C43 B1 C31 110.77(16) . . ? C37 B1 C31 106.88(15) . . ? C25 B1 C31 108.86(15) . . ? C30 C25 C26 114.55(18) . . ? C30 C25 B1 125.00(17) . . ? C26 C25 B1 120.33(17) . . ? C27 C26 C25 123.1(2) . . ? C28 C27 C26 120.2(2) . . ? C27 C28 C29 118.7(2) . . ? C30 C29 C28 120.2(2) . . ? C29 C30 C25 123.2(2) . . ? C32 C31 C36 114.72(18) . . ? C32 C31 B1 124.66(17) . . ? C36 C31 B1 120.60(17) . . ? C33 C32 C31 122.91(19) . . ? C34 C33 C32 120.62(19) . . ? C33 C34 C35 118.52(19) . . ? C34 C35 C36 120.32(19) . . ? C35 C36 C31 122.89(18) . . ? C42 C37 C38 114.87(19) . . ? C42 C37 B1 123.89(18) . . ? C38 C37 B1 121.01(17) . . ? C39 C38 C37 123.0(2) . . ? C40 C39 C38 119.9(2) . . ? C41 C40 C39 119.4(2) . . ? C40 C41 C42 120.3(2) . . ? C41 C42 C37 122.5(2) . . ? C48 C43 C44 114.67(18) . . ? C48 C43 B1 121.90(17) . . ? C44 C43 B1 122.95(17) . . ? C45 C44 C43 123.1(2) . . ? C46 C45 C44 120.1(2) . . ? C45 C46 C47 118.92(19) . . ? C48 C47 C46 119.8(2) . . ? C47 C48 C43 123.4(2) . . ? C61 B2 C67 107.78(15) . . ? C61 B2 C55 110.76(16) . . ? C67 B2 C55 110.67(15) . . ? C61 B2 C49 108.84(15) . . ? C67 B2 C49 110.31(15) . . ? C55 B2 C49 108.47(15) . . ? C50 C49 C54 114.73(18) . . ? C50 C49 B2 121.20(17) . . ? C54 C49 B2 123.86(17) . . ? C51 C50 C49 123.36(19) . . ? C52 C51 C50 120.0(2) . . ? C53 C52 C51 118.8(2) . . ? C52 C53 C54 120.6(2) . . ? C53 C54 C49 122.5(2) . . ? C60 C55 C56 114.52(18) . . ? C60 C55 B2 121.06(17) . . ? C56 C55 B2 124.30(17) . . ? C57 C56 C55 122.78(19) . . ? C58 C57 C56 120.6(2) . . ? C57 C58 C59 118.8(2) . . ? C58 C59 C60 119.8(2) . . ? C59 C60 C55 123.5(2) . . ? C66 C61 C62 114.90(18) . . ? C66 C61 B2 123.17(17) . . ? C62 C61 B2 121.54(17) . . ? C63 C62 C61 122.9(2) . . ? C64 C63 C62 120.0(2) . . ? C63 C64 C65 119.2(2) . . ? C66 C65 C64 119.8(2) . . ? C65 C66 C61 123.1(2) . . ? C72 C67 C68 114.38(18) . . ? C72 C67 B2 121.52(17) . . ? C68 C67 B2 124.09(17) . . ? C69 C68 C67 123.33(19) . . ? C70 C69 C68 120.0(2) . . ? C71 C70 C69 118.7(2) . . ? C70 C71 C72 120.4(2) . . ? C71 C72 C67 123.1(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 S2 N1 S1 C12 -129.15(11) . . . . ? S2 N1 S1 C1 125.92(11) . . . . ? N1 S1 C1 C2 -157.84(15) . . . . ? C12 S1 C1 C2 93.93(17) . . . . ? S1 C1 C2 O1 57.7(2) . . . . ? C1 C2 O1 C3 75.4(2) . . . . ? C2 O1 C3 C4 -119.5(2) . . . . ? O1 C3 C4 O2 66.5(2) . . . . ? C3 C4 O2 C5 175.29(18) . . . . ? C4 O2 C5 C6 172.98(17) . . . . ? O2 C5 C6 S2 -59.5(2) . . . . ? S1 N1 S2 C7 146.82(11) . . . . ? S1 N1 S2 C6 -109.47(11) . . . . ? C5 C6 S2 N1 94.53(16) . . . . ? C5 C6 S2 C7 -160.59(15) . . . . ? N1 S2 C7 C8 -70.18(17) . . . . ? C6 S2 C7 C8 -179.64(16) . . . . ? S2 C7 C8 O3 -60.2(2) . . . . ? C7 C8 O3 C9 160.97(17) . . . . ? C8 O3 C9 C10 -94.8(2) . . . . ? O3 C9 C10 O4 56.2(2) . . . . ? C9 C10 O4 C11 174.05(18) . . . . ? C10 O4 C11 C12 162.14(18) . . . . ? O4 C11 C12 S1 -60.3(2) . . . . ? N1 S1 C12 C11 92.91(17) . . . . ? C1 S1 C12 C11 -159.53(16) . . . . ? S4 N2 S3 C13 -139.23(11) . . . . ? S4 N2 S3 C24 119.05(11) . . . . ? N2 S3 C13 C14 72.21(16) . . . . ? C24 S3 C13 C14 -179.38(15) . . . . ? S3 C13 C14 O5 60.72(19) . . . . ? C13 C14 O5 C15 -166.60(16) . . . . ? C14 O5 C15 C16 60.7(2) . . . . ? O5 C15 C16 O6 52.6(2) . . . . ? C15 C16 O6 C17 -169.53(17) . . . . ? C16 O6 C17 C18 90.4(2) . . . . ? O6 C17 C18 S4 60.1(2) . . . . ? S3 N2 S4 C19 -142.94(11) . . . . ? S3 N2 S4 C18 114.13(11) . . . . ? C17 C18 S4 N2 -111.61(15) . . . . ? C17 C18 S4 C19 145.58(15) . . . . ? N2 S4 C19 C20 69.20(16) . . . . ? C18 S4 C19 C20 178.40(15) . . . . ? S4 C19 C20 O7 53.12(19) . . . . ? C19 C20 O7 C21 -169.29(17) . . . . ? C20 O7 C21 C22 69.7(2) . . . . ? O7 C21 C22 O8 57.6(3) . . . . ? C21 C22 O8 C23 -166.24(18) . . . . ? C22 O8 C23 C24 83.0(2) . . . . ? O8 C23 C24 S3 59.4(2) . . . . ? N2 S3 C24 C23 -113.26(16) . . . . ? C13 S3 C24 C23 144.22(16) . . . . ? C43 B1 C25 C30 -139.88(19) . . . . ? C37 B1 C25 C30 -20.2(3) . . . . ? C31 B1 C25 C30 98.5(2) . . . . ? C43 B1 C25 C26 44.3(2) . . . . ? C37 B1 C25 C26 163.99(17) . . . . ? C31 B1 C25 C26 -77.3(2) . . . . ? C30 C25 C26 C27 -1.9(3) . . . . ? B1 C25 C26 C27 174.30(18) . . . . ? C25 C26 C27 C28 1.1(3) . . . . ? C26 C27 C28 C29 -0.1(3) . . . . ? C27 C28 C29 C30 0.0(3) . . . . ? C28 C29 C30 C25 -0.9(3) . . . . ? C26 C25 C30 C29 1.8(3) . . . . ? B1 C25 C30 C29 -174.23(19) . . . . ? C43 B1 C31 C32 -97.5(2) . . . . ? C37 B1 C31 C32 146.34(18) . . . . ? C25 B1 C31 C32 23.7(3) . . . . ? C43 B1 C31 C36 80.9(2) . . . . ? C37 B1 C31 C36 -35.3(2) . . . . ? C25 B1 C31 C36 -157.90(17) . . . . ? C36 C31 C32 C33 -1.4(3) . . . . ? B1 C31 C32 C33 177.11(18) . . . . ? C31 C32 C33 C34 0.6(3) . . . . ? C32 C33 C34 C35 0.3(3) . . . . ? C33 C34 C35 C36 -0.2(3) . . . . ? C34 C35 C36 C31 -0.8(3) . . . . ? C32 C31 C36 C35 1.5(3) . . . . ? B1 C31 C36 C35 -177.08(18) . . . . ? C43 B1 C37 C42 -2.2(2) . . . . ? C25 B1 C37 C42 -123.6(2) . . . . ? C31 B1 C37 C42 116.5(2) . . . . ? C43 B1 C37 C38 -176.48(17) . . . . ? C25 B1 C37 C38 62.1(2) . . . . ? C31 B1 C37 C38 -57.8(2) . . . . ? C42 C37 C38 C39 1.4(3) . . . . ? B1 C37 C38 C39 176.21(18) . . . . ? C37 C38 C39 C40 -2.3(3) . . . . ? C38 C39 C40 C41 1.4(3) . . . . ? C39 C40 C41 C42 0.3(3) . . . . ? C40 C41 C42 C37 -1.1(3) . . . . ? C38 C37 C42 C41 0.3(3) . . . . ? B1 C37 C42 C41 -174.31(18) . . . . ? C37 B1 C43 C48 -87.4(2) . . . . ? C25 B1 C43 C48 36.0(2) . . . . ? C31 B1 C43 C48 156.44(18) . . . . ? C37 B1 C43 C44 84.2(2) . . . . ? C25 B1 C43 C44 -152.38(18) . . . . ? C31 B1 C43 C44 -31.9(2) . . . . ? C48 C43 C44 C45 2.0(3) . . . . ? B1 C43 C44 C45 -170.21(18) . . . . ? C43 C44 C45 C46 -0.1(3) . . . . ? C44 C45 C46 C47 -1.5(3) . . . . ? C45 C46 C47 C48 1.2(3) . . . . ? C46 C47 C48 C43 0.9(3) . . . . ? C44 C43 C48 C47 -2.4(3) . . . . ? B1 C43 C48 C47 169.92(19) . . . . ? C61 B2 C49 C50 -84.3(2) . . . . ? C67 B2 C49 C50 33.8(2) . . . . ? C55 B2 C49 C50 155.13(17) . . . . ? C61 B2 C49 C54 90.1(2) . . . . ? C67 B2 C49 C54 -151.83(19) . . . . ? C55 B2 C49 C54 -30.5(2) . . . . ? C54 C49 C50 C51 -2.4(3) . . . . ? B2 C49 C50 C51 172.44(18) . . . . ? C49 C50 C51 C52 1.4(3) . . . . ? C50 C51 C52 C53 0.5(3) . . . . ? C51 C52 C53 C54 -1.1(3) . . . . ? C52 C53 C54 C49 -0.1(3) . . . . ? C50 C49 C54 C53 1.8(3) . . . . ? B2 C49 C54 C53 -172.97(19) . . . . ? C61 B2 C55 C60 -40.5(2) . . . . ? C67 B2 C55 C60 -159.94(18) . . . . ? C49 B2 C55 C60 78.9(2) . . . . ? C61 B2 C55 C56 143.76(18) . . . . ? C67 B2 C55 C56 24.3(3) . . . . ? C49 B2 C55 C56 -96.9(2) . . . . ? C60 C55 C56 C57 -1.3(3) . . . . ? B2 C55 C56 C57 174.67(18) . . . . ? C55 C56 C57 C58 0.3(3) . . . . ? C56 C57 C58 C59 0.4(3) . . . . ? C57 C58 C59 C60 -0.1(3) . . . . ? C58 C59 C60 C55 -1.0(3) . . . . ? C56 C55 C60 C59 1.7(3) . . . . ? B2 C55 C60 C59 -174.5(2) . . . . ? C67 B2 C61 C66 -94.4(2) . . . . ? C55 B2 C61 C66 144.40(18) . . . . ? C49 B2 C61 C66 25.2(2) . . . . ? C67 B2 C61 C62 78.1(2) . . . . ? C55 B2 C61 C62 -43.1(2) . . . . ? C49 B2 C61 C62 -162.28(17) . . . . ? C66 C61 C62 C63 3.1(3) . . . . ? B2 C61 C62 C63 -170.01(19) . . . . ? C61 C62 C63 C64 -1.9(3) . . . . ? C62 C63 C64 C65 -0.6(3) . . . . ? C63 C64 C65 C66 1.8(3) . . . . ? C64 C65 C66 C61 -0.5(3) . . . . ? C62 C61 C66 C65 -1.8(3) . . . . ? B2 C61 C66 C65 171.12(19) . . . . ? C61 B2 C67 C72 163.46(18) . . . . ? C55 B2 C67 C72 -75.3(2) . . . . ? C49 B2 C67 C72 44.8(2) . . . . ? C61 B2 C67 C68 -17.0(2) . . . . ? C55 B2 C67 C68 104.2(2) . . . . ? C49 B2 C67 C68 -135.70(19) . . . . ? C72 C67 C68 C69 0.4(3) . . . . ? B2 C67 C68 C69 -179.12(19) . . . . ? C67 C68 C69 C70 -0.5(3) . . . . ? C68 C69 C70 C71 0.4(3) . . . . ? C69 C70 C71 C72 -0.1(3) . . . . ? C70 C71 C72 C67 0.1(3) . . . . ? C68 C67 C72 C71 -0.2(3) . . . . ? B2 C67 C72 C71 179.37(18) . . . . ? _diffrn_measured_fraction_theta_max 0.870 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.570 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.062 #===END