Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Paul Kelly' _publ_contact_author_address ; Department of Chemistry Loughborough University Loughborough Leicestershire LE11 3TU UNITED KINGDOM ; _publ_contact_author_email P.F.KELLY@LBORO.AC.UK _publ_section_title ; Sulfimidation - a new and versatile strategy for the post ring-closure elaboration of mixed thia/oxa crowns ; loop_ _publ_author_name 'Paul Kelly' 'Mark Elsegood' 'Gillian Reid' 'Paul M. Staniland' data_3 _database_code_depnum_ccdc_archive 'CCDC 630549' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H34 N Na O7 S 2+, (C24 H20 B 1-)2' _chemical_formula_sum 'C62 H74 B2 N Na O7 S' _chemical_formula_weight 1021.89 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' Na Na 0.0362 0.0249 '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 _symmetry_space_group_name_Hall '-P 2ybc' 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 17.7978(11) _cell_length_b 17.6584(11) _cell_length_c 18.0403(12) _cell_angle_alpha 90.00 _cell_angle_beta 100.926(2) _cell_angle_gamma 90.00 _cell_volume 5566.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5265 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 22.49 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.219 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2184 _exptl_absorpt_coefficient_mu 0.120 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.962 _exptl_absorpt_correction_T_max 0.980 _exptl_absorpt_process_details 'SADABS v2.10, Sheldrick, G.M., (2003)' _exptl_special_details ; 'SADABS v2.10 (Sheldrick, 2003)' ; _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 39754 _diffrn_reflns_av_R_equivalents 0.0806 _diffrn_reflns_av_sigmaI/netI 0.0792 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9772 _reflns_number_gt 5168 _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^)+(0.0599P)^2^+2.9690P] 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 9772 _refine_ls_number_parameters 841 _refine_ls_number_restraints 646 _refine_ls_R_factor_all 0.1275 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1624 _refine_ls_wR_factor_gt 0.1248 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.2474(2) 0.7475(2) 0.2683(2) 0.0512(11) Uani 0.772(2) 1 d PDU A 1 S1 S 0.26633(7) 0.66907(8) 0.23002(7) 0.0453(4) Uani 0.772(2) 1 d PDU A 1 C1 C 0.1718(4) 0.6437(4) 0.1795(3) 0.0480(14) Uani 0.772(2) 1 d PDU A 1 H1A H 0.1505 0.6854 0.1452 0.058 Uiso 0.772(2) 1 calc PR A 1 H1B H 0.1748 0.5978 0.1487 0.058 Uiso 0.772(2) 1 calc PR A 1 C2 C 0.1203(3) 0.6289(3) 0.2361(3) 0.0477(12) Uani 0.772(2) 1 d PDU A 1 H2A H 0.1136 0.6761 0.2637 0.057 Uiso 0.772(2) 1 calc PR A 1 H2B H 0.0693 0.6119 0.2094 0.057 Uiso 0.772(2) 1 calc PR A 1 O1 O 0.15361(16) 0.57244(17) 0.28750(18) 0.0398(8) Uani 0.772(2) 1 d PDU A 1 C3 C 0.1025(4) 0.5495(3) 0.3364(4) 0.0520(14) Uani 0.772(2) 1 d PDU A 1 H3A H 0.0553 0.5274 0.3061 0.062 Uiso 0.772(2) 1 calc PR A 1 H3B H 0.0879 0.5940 0.3640 0.062 Uiso 0.772(2) 1 calc PR A 1 C4 C 0.1417(5) 0.4924(5) 0.3910(7) 0.050(2) Uani 0.772(2) 1 d PDU A 1 H4A H 0.1886 0.5145 0.4216 0.060 Uiso 0.772(2) 1 calc PR A 1 H4B H 0.1076 0.4762 0.4254 0.060 Uiso 0.772(2) 1 calc PR A 1 O2 O 0.16068(19) 0.4296(2) 0.34936(19) 0.0383(8) Uani 0.772(2) 1 d PDU A 1 C5 C 0.1942(3) 0.3694(3) 0.3975(3) 0.0461(13) Uani 0.772(2) 1 d PDU A 1 H5A H 0.1570 0.3495 0.4270 0.055 Uiso 0.772(2) 1 calc PR A 1 H5B H 0.2398 0.3879 0.4331 0.055 Uiso 0.772(2) 1 calc PR A 1 C6 C 0.2165(5) 0.3088(4) 0.3480(5) 0.047(2) Uani 0.772(2) 1 d PDU A 1 H6A H 0.2363 0.2640 0.3785 0.057 Uiso 0.772(2) 1 calc PR A 1 H6B H 0.1718 0.2932 0.3097 0.057 Uiso 0.772(2) 1 calc PR A 1 O3 O 0.2748(2) 0.34054(19) 0.3124(2) 0.0405(8) Uani 0.772(2) 1 d PDU A 1 C7 C 0.2952(3) 0.2909(3) 0.2563(3) 0.0506(14) Uani 0.772(2) 1 d PDU A 1 H7A H 0.2516 0.2847 0.2136 0.061 Uiso 0.772(2) 1 calc PR A 1 H7B H 0.3099 0.2404 0.2782 0.061 Uiso 0.772(2) 1 calc PR A 1 C8 C 0.3612(3) 0.3272(4) 0.2300(3) 0.0478(15) Uani 0.772(2) 1 d PDU A 1 H8A H 0.4045 0.3333 0.2730 0.057 Uiso 0.772(2) 1 calc PR A 1 H8B H 0.3784 0.2950 0.1916 0.057 Uiso 0.772(2) 1 calc PR A 1 O4 O 0.3377(2) 0.3996(2) 0.1984(2) 0.0462(9) Uani 0.772(2) 1 d PDU A 1 C9 C 0.3983(4) 0.4358(4) 0.1703(3) 0.0598(15) Uani 0.772(2) 1 d PDU A 1 H9A H 0.4249 0.3983 0.1437 0.072 Uiso 0.772(2) 1 calc PR A 1 H9B H 0.4358 0.4568 0.2129 0.072 Uiso 0.772(2) 1 calc PR A 1 C10 C 0.3669(4) 0.4986(4) 0.1168(5) 0.0556(19) Uani 0.772(2) 1 d PDU A 1 H10A H 0.4070 0.5158 0.0894 0.067 Uiso 0.772(2) 1 calc PR A 1 H10B H 0.3233 0.4792 0.0791 0.067 Uiso 0.772(2) 1 calc PR A 1 O5 O 0.3420(3) 0.5611(2) 0.1559(2) 0.0491(10) Uani 0.772(2) 1 d PDU A 1 C11 C 0.3178(3) 0.6216(3) 0.1044(3) 0.0580(14) Uani 0.772(2) 1 d PDU A 1 H11A H 0.2679 0.6092 0.0722 0.070 Uiso 0.772(2) 1 calc PR A 1 H11B H 0.3556 0.6297 0.0714 0.070 Uiso 0.772(2) 1 calc PR A 1 C12 C 0.3107(8) 0.6926(5) 0.1502(9) 0.063(3) Uani 0.772(2) 1 d PDU A 1 H12A H 0.2793 0.7308 0.1181 0.076 Uiso 0.772(2) 1 calc PR A 1 H12B H 0.3621 0.7146 0.1685 0.076 Uiso 0.772(2) 1 calc PR A 1 N1X N 0.1366(10) 0.6302(10) 0.1587(9) 0.065(5) Uani 0.228(2) 1 d PDU A 2 S1X S 0.2009(2) 0.6315(2) 0.2339(3) 0.0445(14) Uani 0.228(2) 1 d PDU A 2 C1X C 0.1506(9) 0.6686(8) 0.3034(9) 0.053(4) Uani 0.228(2) 1 d PDU A 2 H1C H 0.1872 0.6875 0.3478 0.063 Uiso 0.228(2) 1 calc PR A 2 H1D H 0.1169 0.7109 0.2820 0.063 Uiso 0.228(2) 1 calc PR A 2 C2X C 0.1029(8) 0.6035(8) 0.3264(9) 0.045(3) Uani 0.228(2) 1 d PDU A 2 H2C H 0.0788 0.6190 0.3692 0.053 Uiso 0.228(2) 1 calc PR A 2 H2D H 0.0620 0.5888 0.2836 0.053 Uiso 0.228(2) 1 calc PR A 2 O1X O 0.1545(7) 0.5408(6) 0.3482(8) 0.056(4) Uani 0.228(2) 1 d PDU A 2 C3X C 0.1155(16) 0.4852(15) 0.385(3) 0.059(9) Uani 0.228(2) 1 d PDU A 2 H3C H 0.0707 0.4647 0.3500 0.071 Uiso 0.228(2) 1 calc PR A 2 H3D H 0.0975 0.5080 0.4290 0.071 Uiso 0.228(2) 1 calc PR A 2 C4X C 0.1721(11) 0.4237(10) 0.4111(10) 0.065(5) Uani 0.228(2) 1 d PDU A 2 H4C H 0.2179 0.4453 0.4441 0.078 Uiso 0.228(2) 1 calc PR A 2 H4D H 0.1493 0.3858 0.4408 0.078 Uiso 0.228(2) 1 calc PR A 2 O2X O 0.1936(7) 0.3884(7) 0.3485(7) 0.044(3) Uani 0.228(2) 1 d PDU A 2 C5X C 0.2367(14) 0.3218(13) 0.3694(12) 0.041(6) Uani 0.228(2) 1 d PDU A 2 H5C H 0.2066 0.2857 0.3940 0.049 Uiso 0.228(2) 1 calc PR A 2 H5D H 0.2841 0.3343 0.4056 0.049 Uiso 0.228(2) 1 calc PR A 2 C6X C 0.2562(9) 0.2866(9) 0.2996(9) 0.050(4) Uani 0.228(2) 1 d PDU A 2 H6C H 0.2822 0.2374 0.3118 0.060 Uiso 0.228(2) 1 calc PR A 2 H6D H 0.2094 0.2783 0.2612 0.060 Uiso 0.228(2) 1 calc PR A 2 O3X O 0.3054(6) 0.3385(7) 0.2729(7) 0.041(3) Uani 0.228(2) 1 d PDU A 2 C7X C 0.3280(12) 0.3127(11) 0.2049(10) 0.052(5) Uani 0.228(2) 1 d PDU A 2 H7C H 0.2827 0.3077 0.1639 0.063 Uiso 0.228(2) 1 calc PR A 2 H7D H 0.3533 0.2626 0.2133 0.063 Uiso 0.228(2) 1 calc PR A 2 C8X C 0.3819(10) 0.3695(9) 0.1843(12) 0.060(5) Uani 0.228(2) 1 d PDU A 2 H8C H 0.4262 0.3754 0.2263 0.072 Uiso 0.228(2) 1 calc PR A 2 H8D H 0.4013 0.3520 0.1392 0.072 Uiso 0.228(2) 1 calc PR A 2 O4X O 0.3441(7) 0.4405(7) 0.1686(8) 0.048(3) Uani 0.228(2) 1 d PDU A 2 C9X C 0.3964(12) 0.4922(11) 0.144(2) 0.069(10) Uani 0.228(2) 1 d PDU A 2 H9C H 0.4175 0.4692 0.1027 0.083 Uiso 0.228(2) 1 calc PR A 2 H9D H 0.4395 0.5021 0.1868 0.083 Uiso 0.228(2) 1 calc PR A 2 C10X C 0.3574(13) 0.5656(10) 0.1183(11) 0.052(5) Uani 0.228(2) 1 d PDU A 2 H10C H 0.3935 0.5984 0.0975 0.063 Uiso 0.228(2) 1 calc PR A 2 H10D H 0.3131 0.5553 0.0774 0.063 Uiso 0.228(2) 1 calc PR A 2 O5X O 0.3319(8) 0.6043(7) 0.1777(8) 0.057(4) Uani 0.228(2) 1 d PDU A 2 C11X C 0.309(3) 0.6801(13) 0.164(3) 0.045(6) Uani 0.228(2) 1 d PDU A 2 H11C H 0.2805 0.6835 0.1109 0.054 Uiso 0.228(2) 1 calc PR A 2 H11D H 0.3554 0.7115 0.1672 0.054 Uiso 0.228(2) 1 calc PR A 2 C12X C 0.2578(7) 0.7159(7) 0.2164(8) 0.023(2) Uani 0.228(2) 1 d PDU A 2 H12C H 0.2248 0.7568 0.1906 0.027 Uiso 0.228(2) 1 calc PR A 2 H12D H 0.2890 0.7357 0.2637 0.027 Uiso 0.228(2) 1 calc PR A 2 Na1 Na 0.25284(7) 0.46737(7) 0.26876(7) 0.0411(3) Uani 1 1 d . . . O6 O 0.17024(14) 0.45232(15) 0.15430(13) 0.0550(7) Uani 1 1 d . A . H6 H 0.1891 0.4556 0.1085 0.066 Uiso 1 1 calc R . . C13 C 0.4035(2) 0.4676(2) 0.4011(2) 0.0525(10) Uani 1 1 d . . . H13A H 0.3923 0.4449 0.4475 0.079 Uiso 1 1 calc R A . H13B H 0.4504 0.4979 0.4133 0.079 Uiso 1 1 calc R . . H13C H 0.4106 0.4273 0.3657 0.079 Uiso 1 1 calc R . . O7 O 0.34106(13) 0.51515(13) 0.36744(13) 0.0465(6) Uani 1 1 d . A . H7 H 0.3362 0.5651 0.3854 0.056 Uiso 1 1 calc R . . C14 C 0.0916(2) 0.4382(2) 0.1524(2) 0.0599(11) Uani 1 1 d . . . H14A H 0.0837 0.4256 0.2032 0.090 Uiso 1 1 calc R A . H14B H 0.0748 0.3958 0.1182 0.090 Uiso 1 1 calc R . . H14C H 0.0619 0.4835 0.1342 0.090 Uiso 1 1 calc R . . B1 B 0.4577(2) 0.7544(2) 0.4482(2) 0.0290(8) Uani 1 1 d . . . C15 C 0.39735(18) 0.69467(17) 0.47497(17) 0.0312(8) Uani 1 1 d . . . C16 C 0.31777(18) 0.70291(19) 0.46136(19) 0.0373(8) Uani 1 1 d . . . H16 H 0.2956 0.7448 0.4321 0.045 Uiso 1 1 calc R . . C17 C 0.2696(2) 0.6521(2) 0.4889(2) 0.0463(9) Uani 1 1 d . . . H17 H 0.2158 0.6601 0.4781 0.056 Uiso 1 1 calc R . . C18 C 0.2993(2) 0.5903(2) 0.53179(19) 0.0426(9) Uani 1 1 d . . . H18 H 0.2666 0.5557 0.5507 0.051 Uiso 1 1 calc R . . C19 C 0.3774(2) 0.58033(19) 0.54633(18) 0.0405(9) Uani 1 1 d . . . H19 H 0.3993 0.5387 0.5762 0.049 Uiso 1 1 calc R . . C20 C 0.4243(2) 0.63078(18) 0.51763(18) 0.0367(8) Uani 1 1 d . . . H20 H 0.4778 0.6214 0.5275 0.044 Uiso 1 1 calc R . . C21 C 0.41626(17) 0.80821(17) 0.37695(17) 0.0300(7) Uani 1 1 d . . . C22 C 0.43465(18) 0.80674(18) 0.30473(17) 0.0326(8) Uani 1 1 d . . . H22 H 0.4710 0.7706 0.2946 0.039 Uiso 1 1 calc R . . C23 C 0.40205(19) 0.85587(19) 0.24714(19) 0.0384(8) Uani 1 1 d . . . H23 H 0.4162 0.8525 0.1991 0.046 Uiso 1 1 calc R . . C24 C 0.3494(2) 0.90920(19) 0.25945(19) 0.0397(9) Uani 1 1 d . . . H24 H 0.3271 0.9427 0.2202 0.048 Uiso 1 1 calc R . . C25 C 0.32943(19) 0.91326(18) 0.32993(19) 0.0381(8) Uani 1 1 d . . . H25 H 0.2930 0.9496 0.3393 0.046 Uiso 1 1 calc R . . C26 C 0.36254(18) 0.86442(18) 0.38663(18) 0.0341(8) Uani 1 1 d . . . H26 H 0.3484 0.8689 0.4347 0.041 Uiso 1 1 calc R . . C27 C 0.52666(18) 0.70398(17) 0.42226(17) 0.0292(7) Uani 1 1 d . . . C28 C 0.5090(2) 0.64462(18) 0.36947(18) 0.0354(8) Uani 1 1 d . . . H28 H 0.4568 0.6338 0.3497 0.042 Uiso 1 1 calc R . . C29 C 0.5650(2) 0.60145(18) 0.34522(19) 0.0404(9) Uani 1 1 d . . . H29 H 0.5505 0.5616 0.3100 0.048 Uiso 1 1 calc R . . C30 C 0.6415(2) 0.61611(19) 0.3721(2) 0.0421(9) Uani 1 1 d . . . H30 H 0.6800 0.5875 0.3548 0.051 Uiso 1 1 calc R . . C31 C 0.6612(2) 0.67286(19) 0.42440(19) 0.0406(9) Uani 1 1 d . . . H31 H 0.7136 0.6832 0.4440 0.049 Uiso 1 1 calc R . . C32 C 0.60424(18) 0.71529(18) 0.44876(18) 0.0347(8) Uani 1 1 d . . . H32 H 0.6194 0.7538 0.4853 0.042 Uiso 1 1 calc R . . C33 C 0.49428(17) 0.80932(17) 0.51940(17) 0.0307(8) Uani 1 1 d . . . C34 C 0.52258(18) 0.88151(18) 0.50813(18) 0.0335(8) Uani 1 1 d . . . H34 H 0.5170 0.9000 0.4579 0.040 Uiso 1 1 calc R . . C35 C 0.55828(18) 0.92721(19) 0.56664(19) 0.0374(8) Uani 1 1 d . . . H35 H 0.5773 0.9754 0.5559 0.045 Uiso 1 1 calc R . . C36 C 0.56644(19) 0.90323(19) 0.64056(19) 0.0390(9) Uani 1 1 d . . . H36 H 0.5909 0.9344 0.6810 0.047 Uiso 1 1 calc R . . C37 C 0.5381(2) 0.8326(2) 0.65433(19) 0.0446(9) Uani 1 1 d . . . H37 H 0.5424 0.8153 0.7048 0.054 Uiso 1 1 calc R . . C38 C 0.50347(19) 0.78685(19) 0.59511(17) 0.0368(8) Uani 1 1 d . . . H38 H 0.4853 0.7384 0.6063 0.044 Uiso 1 1 calc R . . B2 B -0.0146(2) 0.7559(2) 0.5137(2) 0.0329(9) Uani 1 1 d . . . C39 C -0.04153(17) 0.69061(18) 0.44787(18) 0.0320(8) Uani 1 1 d . . . C40 C -0.06355(19) 0.70993(19) 0.37114(19) 0.0401(9) Uani 1 1 d . . . H40 H -0.0589 0.7612 0.3567 0.048 Uiso 1 1 calc R . . C41 C -0.0919(2) 0.6572(2) 0.31552(19) 0.0438(9) Uani 1 1 d . . . H41 H -0.1065 0.6727 0.2644 0.053 Uiso 1 1 calc R . . C42 C -0.0986(2) 0.5820(2) 0.3352(2) 0.0460(9) Uani 1 1 d . . . H42 H -0.1191 0.5457 0.2980 0.055 Uiso 1 1 calc R . . C43 C -0.0753(2) 0.5606(2) 0.4094(2) 0.0440(9) Uani 1 1 d . . . H43 H -0.0785 0.5089 0.4231 0.053 Uiso 1 1 calc R . . C44 C -0.04711(19) 0.61386(18) 0.46415(19) 0.0377(8) Uani 1 1 d . . . H44 H -0.0310 0.5974 0.5148 0.045 Uiso 1 1 calc R . . C45 C 0.04519(17) 0.81547(18) 0.48497(17) 0.0300(7) Uani 1 1 d . . . C46 C 0.05160(18) 0.89209(18) 0.50604(18) 0.0339(8) Uani 1 1 d . . . H46 H 0.0186 0.9114 0.5372 0.041 Uiso 1 1 calc R . . C47 C 0.10420(19) 0.9409(2) 0.48326(19) 0.0391(9) Uani 1 1 d . . . H47 H 0.1061 0.9924 0.4985 0.047 Uiso 1 1 calc R . . C48 C 0.15385(19) 0.9148(2) 0.43849(19) 0.0416(9) Uani 1 1 d . . . H48 H 0.1903 0.9477 0.4233 0.050 Uiso 1 1 calc R . . C49 C 0.14916(19) 0.84005(19) 0.41651(19) 0.0392(9) Uani 1 1 d . . . H49 H 0.1828 0.8210 0.3859 0.047 Uiso 1 1 calc R . . C50 C 0.09565(19) 0.79231(19) 0.43872(18) 0.0371(8) Uani 1 1 d . . . H50 H 0.0932 0.7413 0.4216 0.044 Uiso 1 1 calc R . . C51 C -0.09105(18) 0.80175(17) 0.52899(18) 0.0320(8) Uani 1 1 d . . . C52 C -0.08913(19) 0.84728(18) 0.59338(18) 0.0360(8) Uani 1 1 d . . . H52 H -0.0427 0.8504 0.6293 0.043 Uiso 1 1 calc R . . C53 C -0.1520(2) 0.88791(19) 0.6068(2) 0.0408(9) Uani 1 1 d . . . H53 H -0.1480 0.9178 0.6512 0.049 Uiso 1 1 calc R . . C54 C -0.2204(2) 0.88509(19) 0.5559(2) 0.0431(9) Uani 1 1 d . . . H54 H -0.2637 0.9124 0.5651 0.052 Uiso 1 1 calc R . . C55 C -0.22480(19) 0.84206(19) 0.4915(2) 0.0406(9) Uani 1 1 d . . . H55 H -0.2712 0.8403 0.4554 0.049 Uiso 1 1 calc R . . C56 C -0.16152(18) 0.80127(18) 0.47911(19) 0.0365(8) Uani 1 1 d . . . H56 H -0.1664 0.7716 0.4345 0.044 Uiso 1 1 calc R . . C57 C 0.03124(18) 0.71235(17) 0.58981(18) 0.0318(8) Uani 1 1 d . . . C58 C 0.00280(19) 0.69955(19) 0.65627(18) 0.0374(8) Uani 1 1 d . . . H58 H -0.0458 0.7198 0.6599 0.045 Uiso 1 1 calc R . . C59 C 0.0429(2) 0.6585(2) 0.7171(2) 0.0434(9) Uani 1 1 d . . . H59 H 0.0219 0.6527 0.7615 0.052 Uiso 1 1 calc R . . C60 C 0.1124(2) 0.62627(19) 0.71372(19) 0.0422(9) Uani 1 1 d . . . H60 H 0.1394 0.5977 0.7549 0.051 Uiso 1 1 calc R . . C61 C 0.1421(2) 0.63641(19) 0.64870(19) 0.0409(9) Uani 1 1 d . . . H61 H 0.1898 0.6141 0.6448 0.049 Uiso 1 1 calc R . . C62 C 0.10266(19) 0.67895(18) 0.58952(19) 0.0373(8) Uani 1 1 d . . . H62 H 0.1252 0.6859 0.5463 0.045 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 0.046(2) 0.048(2) 0.060(3) -0.001(2) 0.011(2) -0.002(2) S1 0.0452(8) 0.0533(9) 0.0368(7) -0.0011(6) 0.0065(6) -0.0036(6) C1 0.057(4) 0.047(4) 0.029(3) 0.009(3) -0.020(2) -0.012(3) C2 0.032(2) 0.040(3) 0.066(3) 0.010(2) -0.007(2) 0.004(2) O1 0.0324(18) 0.0417(19) 0.046(2) 0.0086(15) 0.0100(15) 0.0019(14) C3 0.056(4) 0.036(3) 0.074(4) -0.005(2) 0.037(3) -0.001(3) C4 0.068(6) 0.042(3) 0.051(4) -0.006(2) 0.036(5) -0.015(3) O2 0.042(2) 0.036(2) 0.037(2) 0.0007(15) 0.0106(16) -0.0047(16) C5 0.044(3) 0.051(3) 0.044(3) 0.014(3) 0.013(3) -0.003(2) C6 0.052(4) 0.034(4) 0.056(5) 0.011(3) 0.012(4) -0.010(3) O3 0.040(2) 0.036(2) 0.047(2) -0.0019(17) 0.0115(16) -0.0007(16) C7 0.052(4) 0.039(3) 0.060(4) -0.012(3) 0.010(3) -0.001(3) C8 0.049(4) 0.044(3) 0.052(4) -0.012(3) 0.014(3) 0.009(3) O4 0.040(2) 0.053(2) 0.048(2) -0.0012(18) 0.0142(17) 0.0018(19) C9 0.052(4) 0.076(4) 0.058(4) 0.004(3) 0.028(3) 0.007(3) C10 0.058(5) 0.067(4) 0.049(4) -0.006(2) 0.030(4) -0.003(3) O5 0.055(3) 0.059(2) 0.037(3) -0.0072(19) 0.019(2) -0.007(2) C11 0.082(4) 0.057(3) 0.040(3) -0.005(2) 0.021(3) -0.023(3) C12 0.091(6) 0.055(4) 0.051(7) -0.010(4) 0.029(5) -0.029(4) N1X 0.081(13) 0.038(9) 0.068(9) -0.019(8) -0.009(7) -0.016(8) S1X 0.040(3) 0.036(2) 0.061(3) -0.008(2) 0.015(2) -0.0098(19) C1X 0.054(11) 0.045(7) 0.064(10) -0.003(7) 0.026(7) -0.003(7) C2X 0.037(9) 0.048(8) 0.049(10) -0.012(7) 0.007(6) -0.009(5) O1X 0.050(8) 0.046(6) 0.075(10) -0.010(6) 0.020(8) 0.001(6) C3X 0.060(19) 0.054(12) 0.067(17) -0.002(11) 0.025(15) 0.007(10) C4X 0.074(13) 0.066(11) 0.065(13) 0.006(8) 0.034(11) 0.021(9) O2X 0.054(9) 0.034(7) 0.044(8) 0.002(5) 0.008(6) -0.001(5) C5X 0.048(15) 0.019(9) 0.055(14) 0.001(8) 0.007(10) -0.015(9) C6X 0.045(11) 0.047(11) 0.054(10) 0.002(8) 0.002(8) 0.008(7) O3X 0.030(7) 0.044(8) 0.047(7) -0.010(6) 0.000(5) 0.006(6) C7X 0.062(15) 0.043(8) 0.051(12) -0.019(9) 0.008(10) -0.002(10) C8X 0.049(12) 0.063(9) 0.072(13) 0.000(10) 0.020(9) 0.009(7) O4X 0.036(8) 0.051(7) 0.063(10) -0.013(7) 0.021(7) 0.000(5) C9X 0.034(15) 0.044(8) 0.14(3) -0.022(11) 0.056(15) 0.004(8) C10X 0.056(14) 0.044(8) 0.059(14) -0.026(7) 0.015(11) -0.004(8) O5X 0.072(9) 0.035(6) 0.080(10) -0.007(7) 0.052(8) 0.010(6) C11X 0.067(16) 0.031(8) 0.044(17) -0.001(9) 0.030(11) 0.002(9) C12X 0.030(4) 0.010(3) 0.025(4) 0.004(3) -0.002(3) 0.010(2) Na1 0.0424(8) 0.0422(8) 0.0375(8) 0.0028(6) 0.0047(6) -0.0002(6) O6 0.0448(16) 0.0820(19) 0.0366(15) -0.0043(14) 0.0033(12) 0.0056(14) C13 0.044(2) 0.047(2) 0.061(3) -0.005(2) -0.004(2) 0.0035(19) O7 0.0415(15) 0.0432(15) 0.0504(16) -0.0106(12) -0.0021(12) 0.0059(12) C14 0.063(3) 0.055(3) 0.057(3) 0.001(2) -0.001(2) -0.017(2) B1 0.028(2) 0.033(2) 0.025(2) -0.0012(16) 0.0045(16) -0.0019(17) C15 0.035(2) 0.0348(19) 0.0230(17) -0.0018(15) 0.0038(14) 0.0014(15) C16 0.032(2) 0.044(2) 0.038(2) 0.0023(17) 0.0104(16) 0.0030(16) C17 0.034(2) 0.059(3) 0.050(2) 0.000(2) 0.0160(18) -0.0016(18) C18 0.045(2) 0.050(2) 0.036(2) -0.0041(18) 0.0170(18) -0.0153(18) C19 0.050(2) 0.039(2) 0.033(2) 0.0029(16) 0.0107(17) -0.0084(18) C20 0.038(2) 0.037(2) 0.033(2) 0.0029(16) 0.0039(16) -0.0023(16) C21 0.0297(18) 0.0308(18) 0.0289(18) -0.0019(15) 0.0045(14) -0.0083(15) C22 0.0313(19) 0.0363(19) 0.0288(19) 0.0020(15) 0.0024(15) -0.0039(15) C23 0.042(2) 0.044(2) 0.0284(19) 0.0032(16) 0.0033(16) -0.0080(17) C24 0.044(2) 0.036(2) 0.036(2) 0.0105(16) 0.0001(17) -0.0048(17) C25 0.033(2) 0.037(2) 0.042(2) 0.0039(17) 0.0012(16) 0.0031(16) C26 0.039(2) 0.037(2) 0.0261(18) -0.0033(15) 0.0046(15) -0.0022(16) C27 0.0317(19) 0.0315(18) 0.0247(17) 0.0042(14) 0.0058(14) -0.0015(14) C28 0.044(2) 0.0341(19) 0.0290(19) 0.0007(15) 0.0085(16) -0.0002(16) C29 0.061(3) 0.0295(19) 0.032(2) 0.0001(15) 0.0137(18) 0.0012(18) C30 0.047(2) 0.038(2) 0.044(2) 0.0049(18) 0.0154(18) 0.0056(18) C31 0.036(2) 0.042(2) 0.043(2) 0.0088(18) 0.0071(17) 0.0010(17) C32 0.036(2) 0.036(2) 0.0321(19) 0.0036(15) 0.0070(16) -0.0013(16) C33 0.0288(18) 0.0326(19) 0.0316(19) -0.0010(15) 0.0082(15) 0.0036(15) C34 0.038(2) 0.0356(19) 0.0283(19) 0.0007(15) 0.0092(15) -0.0018(16) C35 0.038(2) 0.035(2) 0.039(2) -0.0014(16) 0.0081(17) -0.0027(16) C36 0.045(2) 0.041(2) 0.029(2) -0.0058(16) 0.0031(16) -0.0045(17) C37 0.056(2) 0.050(2) 0.0267(19) 0.0006(17) 0.0032(17) -0.0063(19) C38 0.047(2) 0.0354(19) 0.0276(19) 0.0017(15) 0.0055(16) -0.0062(16) B2 0.032(2) 0.038(2) 0.028(2) 0.0013(17) 0.0041(17) 0.0006(18) C39 0.0280(18) 0.039(2) 0.0294(19) 0.0020(15) 0.0057(14) 0.0030(15) C40 0.044(2) 0.036(2) 0.039(2) 0.0016(17) 0.0050(17) 0.0021(16) C41 0.053(2) 0.046(2) 0.030(2) -0.0025(18) 0.0000(17) 0.0045(18) C42 0.048(2) 0.043(2) 0.045(2) -0.0062(18) 0.0015(18) -0.0043(18) C43 0.048(2) 0.037(2) 0.047(2) -0.0003(18) 0.0084(19) -0.0052(17) C44 0.040(2) 0.040(2) 0.033(2) 0.0055(17) 0.0066(16) -0.0020(16) C45 0.0300(18) 0.0337(19) 0.0243(18) 0.0028(14) 0.0005(14) 0.0020(15) C46 0.0302(19) 0.039(2) 0.0330(19) 0.0006(16) 0.0082(15) -0.0012(16) C47 0.037(2) 0.040(2) 0.038(2) -0.0040(17) 0.0046(17) -0.0071(17) C48 0.036(2) 0.045(2) 0.045(2) 0.0099(18) 0.0081(17) -0.0045(17) C49 0.035(2) 0.043(2) 0.042(2) 0.0111(17) 0.0140(17) 0.0062(17) C50 0.040(2) 0.0353(19) 0.036(2) 0.0034(16) 0.0089(17) 0.0036(16) C51 0.0343(19) 0.0314(18) 0.0309(19) 0.0036(15) 0.0079(15) -0.0049(15) C52 0.0327(19) 0.040(2) 0.035(2) 0.0037(16) 0.0073(16) -0.0030(16) C53 0.046(2) 0.038(2) 0.042(2) 0.0029(17) 0.0166(18) 0.0017(17) C54 0.038(2) 0.037(2) 0.057(3) 0.0109(19) 0.0162(19) 0.0049(17) C55 0.031(2) 0.040(2) 0.048(2) 0.0058(18) -0.0006(17) -0.0016(16) C56 0.035(2) 0.037(2) 0.037(2) 0.0051(16) 0.0032(16) -0.0013(16) C57 0.0304(19) 0.0308(18) 0.0330(19) -0.0015(15) 0.0031(15) -0.0055(15) C58 0.035(2) 0.044(2) 0.033(2) 0.0052(17) 0.0053(16) -0.0024(16) C59 0.045(2) 0.051(2) 0.034(2) 0.0059(18) 0.0071(17) -0.0028(19) C60 0.050(2) 0.041(2) 0.032(2) 0.0062(16) -0.0046(17) 0.0007(18) C61 0.036(2) 0.046(2) 0.038(2) -0.0002(17) -0.0019(17) 0.0097(17) C62 0.039(2) 0.040(2) 0.033(2) 0.0033(16) 0.0078(16) 0.0037(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 1.611(4) . ? S1 C1 1.812(6) . ? S1 C12 1.817(8) . ? C1 C2 1.519(8) . ? C2 O1 1.413(5) . ? O1 C3 1.441(6) . ? O1 Na1 2.627(3) . ? C3 C4 1.487(11) . ? C4 O2 1.414(10) . ? O2 C5 1.430(6) . ? O2 Na1 2.480(4) . ? C5 C6 1.494(9) . ? C6 O3 1.434(9) . ? O3 C7 1.437(6) . ? O3 Na1 2.381(4) . ? C7 C8 1.493(8) . ? C8 O4 1.429(7) . ? O4 C9 1.427(7) . ? O4 Na1 2.460(4) . ? C9 C10 1.506(9) . ? C10 O5 1.425(9) . ? O5 C11 1.428(7) . ? C11 C12 1.520(12) . ? N1X S1X 1.602(13) . ? S1X C1X 1.797(12) . ? S1X C12X 1.861(12) . ? C1X C2X 1.532(15) . ? C2X O1X 1.444(15) . ? O1X C3X 1.441(18) . ? O1X Na1 2.784(12) . ? C3X C4X 1.49(2) . ? C4X O2X 1.405(17) . ? O2X C5X 1.415(19) . ? O2X Na1 2.389(12) . ? C5X C6X 1.50(2) . ? C6X O3X 1.414(16) . ? O3X C7X 1.434(17) . ? O3X Na1 2.457(12) . ? C7X C8X 1.485(18) . ? C8X O4X 1.425(16) . ? O4X C9X 1.429(18) . ? O4X Na1 2.691(12) . ? C9X C10X 1.504(19) . ? C10X O5X 1.415(16) . ? O5X C11X 1.408(18) . ? C11X C12X 1.57(2) . ? Na1 O7 2.299(3) . ? Na1 O6 2.312(3) . ? O6 C14 1.415(4) . ? C13 O7 1.434(4) . ? B1 C15 1.642(5) . ? B1 C33 1.642(5) . ? B1 C27 1.654(5) . ? B1 C21 1.655(5) . ? C15 C20 1.398(4) . ? C15 C16 1.398(4) . ? C16 C17 1.396(5) . ? C17 C18 1.383(5) . ? C18 C19 1.377(5) . ? C19 C20 1.387(4) . ? C21 C22 1.402(4) . ? C21 C26 1.412(4) . ? C22 C23 1.393(4) . ? C23 C24 1.376(5) . ? C24 C25 1.385(5) . ? C25 C26 1.382(4) . ? C27 C32 1.387(4) . ? C27 C28 1.411(4) . ? C28 C29 1.389(4) . ? C29 C30 1.381(5) . ? C30 C31 1.375(5) . ? C31 C32 1.397(4) . ? C33 C34 1.400(4) . ? C33 C38 1.402(4) . ? C34 C35 1.384(4) . ? C35 C36 1.380(4) . ? C36 C37 1.385(5) . ? C37 C38 1.387(4) . ? B2 C45 1.648(5) . ? B2 C57 1.648(5) . ? B2 C51 1.650(5) . ? B2 C39 1.660(5) . ? C39 C44 1.394(4) . ? C39 C40 1.407(4) . ? C40 C41 1.391(5) . ? C41 C42 1.386(5) . ? C42 C43 1.376(5) . ? C43 C44 1.387(5) . ? C45 C50 1.398(4) . ? C45 C46 1.404(4) . ? C46 C47 1.391(4) . ? C47 C48 1.384(5) . ? C48 C49 1.376(5) . ? C49 C50 1.387(4) . ? C51 C56 1.398(4) . ? C51 C52 1.408(4) . ? C52 C53 1.389(4) . ? C53 C54 1.379(5) . ? C54 C55 1.379(5) . ? C55 C56 1.390(5) . ? C57 C62 1.402(4) . ? C57 C58 1.405(4) . ? C58 C59 1.394(5) . ? C59 C60 1.374(5) . ? C60 C61 1.387(5) . ? C61 C62 1.383(4) . ? 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 100.3(3) . . ? N1 S1 C12 107.5(3) . . ? C1 S1 C12 99.2(6) . . ? C2 C1 S1 109.0(4) . . ? O1 C2 C1 109.4(4) . . ? C2 O1 C3 111.4(4) . . ? C2 O1 Na1 128.5(3) . . ? C3 O1 Na1 113.5(3) . . ? O1 C3 C4 108.9(6) . . ? O2 C4 C3 108.0(8) . . ? C4 O2 C5 112.0(5) . . ? C4 O2 Na1 110.6(3) . . ? C5 O2 Na1 108.0(3) . . ? O2 C5 C6 107.3(6) . . ? O3 C6 C5 106.5(6) . . ? C6 O3 C7 112.3(5) . . ? C6 O3 Na1 115.4(4) . . ? C7 O3 Na1 112.8(3) . . ? O3 C7 C8 106.3(5) . . ? O4 C8 C7 108.8(5) . . ? C9 O4 C8 111.1(4) . . ? C9 O4 Na1 123.0(4) . . ? C8 O4 Na1 113.0(3) . . ? O4 C9 C10 110.2(6) . . ? O5 C10 C9 111.4(6) . . ? C10 O5 C11 109.9(5) . . ? O5 C11 C12 108.0(7) . . ? C11 C12 S1 109.6(5) . . ? N1X S1X C1X 103.0(9) . . ? N1X S1X C12X 101.1(8) . . ? C1X S1X C12X 100.8(6) . . ? C2X C1X S1X 106.9(10) . . ? O1X C2X C1X 107.0(11) . . ? C3X O1X C2X 108.1(13) . . ? C3X O1X Na1 109.1(14) . . ? C2X O1X Na1 130.3(10) . . ? O1X C3X C4X 106.5(17) . . ? O2X C4X C3X 110(2) . . ? C4X O2X C5X 111.8(14) . . ? C4X O2X Na1 116.3(11) . . ? C5X O2X Na1 111.5(12) . . ? O2X C5X C6X 108.7(17) . . ? O3X C6X C5X 106.0(17) . . ? C6X O3X C7X 112.2(13) . . ? C6X O3X Na1 110.7(10) . . ? C7X O3X Na1 115.8(11) . . ? O3X C7X C8X 107.4(14) . . ? O4X C8X C7X 110.0(16) . . ? C8X O4X C9X 108.1(13) . . ? C8X O4X Na1 110.1(11) . . ? C9X O4X Na1 127.1(13) . . ? O4X C9X C10X 110.9(16) . . ? O5X C10X C9X 112.0(19) . . ? C11X O5X C10X 116.5(17) . . ? O5X C11X C12X 117.2(18) . . ? C11X C12X S1X 100.2(13) . . ? O7 Na1 O6 163.54(11) . . ? O7 Na1 O3 92.53(11) . . ? O6 Na1 O3 102.93(12) . . ? O7 Na1 O2X 93.6(3) . . ? O6 Na1 O2X 101.1(3) . . ? O3 Na1 O2X 46.8(3) . . ? O7 Na1 O3X 96.7(3) . . ? O6 Na1 O3X 95.4(3) . . ? O3 Na1 O3X 23.3(2) . . ? O2X Na1 O3X 69.5(4) . . ? O7 Na1 O4 100.48(11) . . ? O6 Na1 O4 80.33(11) . . ? O3 Na1 O4 68.57(13) . . ? O2X Na1 O4 114.3(3) . . ? O3X Na1 O4 45.3(3) . . ? O7 Na1 O2 94.30(11) . . ? O6 Na1 O2 96.52(11) . . ? O3 Na1 O2 68.82(13) . . ? O2X Na1 O2 22.1(3) . . ? O3X Na1 O2 91.4(3) . . ? O4 Na1 O2 135.29(14) . . ? O7 Na1 O1 91.05(10) . . ? O6 Na1 O1 82.35(10) . . ? O3 Na1 O1 133.92(12) . . ? O2X Na1 O1 87.2(3) . . ? O3X Na1 O1 155.8(3) . . ? O4 Na1 O1 154.63(13) . . ? O2 Na1 O1 65.09(11) . . ? O7 Na1 O4X 100.0(3) . . ? O6 Na1 O4X 75.1(3) . . ? O3 Na1 O4X 88.5(3) . . ? O2X Na1 O4X 133.9(4) . . ? O3X Na1 O4X 65.3(4) . . ? O4 Na1 O4X 20.0(2) . . ? O2 Na1 O4X 153.7(3) . . ? O1 Na1 O4X 135.8(3) . . ? O7 Na1 O1X 80.4(3) . . ? O6 Na1 O1X 99.1(3) . . ? O3 Na1 O1X 110.3(3) . . ? O2X Na1 O1X 64.5(4) . . ? O3X Na1 O1X 133.6(4) . . ? O4 Na1 O1X 178.6(3) . . ? O2 Na1 O1X 43.4(3) . . ? O1 Na1 O1X 26.0(3) . . ? O4X Na1 O1X 161.1(4) . . ? C14 O6 Na1 120.1(2) . . ? C13 O7 Na1 118.3(2) . . ? C15 B1 C33 109.5(2) . . ? C15 B1 C27 107.4(3) . . ? C33 B1 C27 109.5(3) . . ? C15 B1 C21 112.2(3) . . ? C33 B1 C21 108.7(3) . . ? C27 B1 C21 109.5(2) . . ? C20 C15 C16 114.3(3) . . ? C20 C15 B1 120.3(3) . . ? C16 C15 B1 125.4(3) . . ? C17 C16 C15 122.7(3) . . ? C18 C17 C16 120.7(3) . . ? C19 C18 C17 118.2(3) . . ? C18 C19 C20 120.3(3) . . ? C19 C20 C15 123.8(3) . . ? C22 C21 C26 114.3(3) . . ? C22 C21 B1 124.2(3) . . ? C26 C21 B1 121.3(3) . . ? C23 C22 C21 122.9(3) . . ? C24 C23 C22 120.4(3) . . ? C23 C24 C25 119.0(3) . . ? C26 C25 C24 120.0(3) . . ? C25 C26 C21 123.4(3) . . ? C32 C27 C28 114.8(3) . . ? C32 C27 B1 124.6(3) . . ? C28 C27 B1 120.6(3) . . ? C29 C28 C27 122.6(3) . . ? C30 C29 C28 120.3(3) . . ? C31 C30 C29 118.9(3) . . ? C30 C31 C32 120.1(3) . . ? C27 C32 C31 123.3(3) . . ? C34 C33 C38 114.9(3) . . ? C34 C33 B1 121.6(3) . . ? C38 C33 B1 123.4(3) . . ? C35 C34 C33 123.1(3) . . ? C36 C35 C34 120.5(3) . . ? C35 C36 C37 118.3(3) . . ? C36 C37 C38 120.7(3) . . ? C37 C38 C33 122.6(3) . . ? C45 B2 C57 108.2(3) . . ? C45 B2 C51 110.0(3) . . ? C57 B2 C51 112.6(3) . . ? C45 B2 C39 109.5(3) . . ? C57 B2 C39 107.6(3) . . ? C51 B2 C39 109.0(3) . . ? C44 C39 C40 115.2(3) . . ? C44 C39 B2 123.2(3) . . ? C40 C39 B2 121.6(3) . . ? C41 C40 C39 122.9(3) . . ? C42 C41 C40 119.5(3) . . ? C43 C42 C41 119.2(3) . . ? C42 C43 C44 120.5(3) . . ? C43 C44 C39 122.6(3) . . ? C50 C45 C46 114.5(3) . . ? C50 C45 B2 121.8(3) . . ? C46 C45 B2 123.6(3) . . ? C47 C46 C45 122.8(3) . . ? C48 C47 C46 120.4(3) . . ? C49 C48 C47 118.5(3) . . ? C48 C49 C50 120.5(3) . . ? C49 C50 C45 123.3(3) . . ? C56 C51 C52 114.4(3) . . ? C56 C51 B2 123.8(3) . . ? C52 C51 B2 121.7(3) . . ? C53 C52 C51 123.0(3) . . ? C54 C53 C52 120.3(3) . . ? C55 C54 C53 118.9(3) . . ? C54 C55 C56 120.2(3) . . ? C55 C56 C51 123.3(3) . . ? C62 C57 C58 114.1(3) . . ? C62 C57 B2 120.0(3) . . ? C58 C57 B2 125.7(3) . . ? C59 C58 C57 122.8(3) . . ? C60 C59 C58 120.7(3) . . ? C59 C60 C61 118.4(3) . . ? C62 C61 C60 120.2(3) . . ? C61 C62 C57 123.6(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 S1 C1 C2 -64.5(4) . . . . ? C12 S1 C1 C2 -174.3(4) . . . . ? S1 C1 C2 O1 -56.1(5) . . . . ? C1 C2 O1 C3 -172.7(4) . . . . ? C1 C2 O1 Na1 -23.5(5) . . . . ? C2 O1 C3 C4 -177.8(6) . . . . ? Na1 O1 C3 C4 28.1(7) . . . . ? O1 C3 C4 O2 -60.2(8) . . . . ? C3 C4 O2 C5 -176.1(5) . . . . ? C3 C4 O2 Na1 63.4(7) . . . . ? C4 O2 C5 C6 -176.3(6) . . . . ? Na1 O2 C5 C6 -54.3(5) . . . . ? O2 C5 C6 O3 64.6(6) . . . . ? C5 C6 O3 C7 -173.2(5) . . . . ? C5 C6 O3 Na1 -42.1(7) . . . . ? C6 O3 C7 C8 -174.3(5) . . . . ? Na1 O3 C7 C8 53.3(5) . . . . ? O3 C7 C8 O4 -60.4(6) . . . . ? C7 C8 O4 C9 -178.2(5) . . . . ? C7 C8 O4 Na1 38.9(5) . . . . ? C8 O4 C9 C10 162.4(5) . . . . ? Na1 O4 C9 C10 -59.0(6) . . . . ? O4 C9 C10 O5 71.2(7) . . . . ? C9 C10 O5 C11 175.8(5) . . . . ? C10 O5 C11 C12 -166.2(6) . . . . ? O5 C11 C12 S1 -41.8(10) . . . . ? N1 S1 C12 C11 -170.7(7) . . . . ? C1 S1 C12 C11 -66.8(9) . . . . ? N1X S1X C1X C2X 78.2(13) . . . . ? C12X S1X C1X C2X -177.7(11) . . . . ? S1X C1X C2X O1X 53.1(15) . . . . ? C1X C2X O1X C3X 168(2) . . . . ? C1X C2X O1X Na1 -55.5(16) . . . . ? C2X O1X C3X C4X -177(2) . . . . ? Na1 O1X C3X C4X 37(3) . . . . ? O1X C3X C4X O2X -64(3) . . . . ? C3X C4X O2X C5X -170(2) . . . . ? C3X C4X O2X Na1 61(2) . . . . ? C4X O2X C5X C6X 179.0(17) . . . . ? Na1 O2X C5X C6X -49(2) . . . . ? O2X C5X C6X O3X 66(2) . . . . ? C5X C6X O3X C7X -179.0(16) . . . . ? C5X C6X O3X Na1 -47.9(15) . . . . ? C6X O3X C7X C8X -177.5(15) . . . . ? Na1 O3X C7X C8X 54.1(19) . . . . ? O3X C7X C8X O4X -63(2) . . . . ? C7X C8X O4X C9X -176(2) . . . . ? C7X C8X O4X Na1 40.8(17) . . . . ? C8X O4X C9X C10X 173(2) . . . . ? Na1 O4X C9X C10X -52(3) . . . . ? O4X C9X C10X O5X 64(3) . . . . ? C9X C10X O5X C11X 167(3) . . . . ? C10X O5X C11X C12X 162(3) . . . . ? O5X C11X C12X S1X -34(4) . . . . ? N1X S1X C12X C11X -81(2) . . . . ? C1X S1X C12X C11X 173(2) . . . . ? C6 O3 Na1 O7 104.3(4) . . . . ? C7 O3 Na1 O7 -124.8(3) . . . . ? C6 O3 Na1 O6 -81.4(4) . . . . ? C7 O3 Na1 O6 49.5(3) . . . . ? C6 O3 Na1 O2X 11.7(6) . . . . ? C7 O3 Na1 O2X 142.6(5) . . . . ? C6 O3 Na1 O3X -154.6(9) . . . . ? C7 O3 Na1 O3X -23.7(7) . . . . ? C6 O3 Na1 O4 -155.4(4) . . . . ? C7 O3 Na1 O4 -24.5(3) . . . . ? C6 O3 Na1 O2 10.7(4) . . . . ? C7 O3 Na1 O2 141.6(3) . . . . ? C6 O3 Na1 O1 10.4(5) . . . . ? C7 O3 Na1 O1 141.3(3) . . . . ? C6 O3 Na1 O4X -155.7(5) . . . . ? C7 O3 Na1 O4X -24.8(4) . . . . ? C6 O3 Na1 O1X 23.6(5) . . . . ? C7 O3 Na1 O1X 154.4(4) . . . . ? C4X O2X Na1 O7 50.9(12) . . . . ? C5X O2X Na1 O7 -78.8(12) . . . . ? C4X O2X Na1 O6 -121.6(12) . . . . ? C5X O2X Na1 O6 108.7(11) . . . . ? C4X O2X Na1 O3 141.0(14) . . . . ? C5X O2X Na1 O3 11.3(10) . . . . ? C4X O2X Na1 O3X 146.7(13) . . . . ? C5X O2X Na1 O3X 17.0(11) . . . . ? C4X O2X Na1 O4 154.1(11) . . . . ? C5X O2X Na1 O4 24.4(12) . . . . ? C4X O2X Na1 O2 -41.7(11) . . . . ? C5X O2X Na1 O2 -171.4(17) . . . . ? C4X O2X Na1 O1 -39.9(12) . . . . ? C5X O2X Na1 O1 -169.7(12) . . . . ? C4X O2X Na1 O4X 158.5(11) . . . . ? C5X O2X Na1 O4X 28.8(14) . . . . ? C4X O2X Na1 O1X -26.7(12) . . . . ? C5X O2X Na1 O1X -156.5(13) . . . . ? C4X O2X Na1 S1X -37.7(13) . . . . ? C5X O2X Na1 S1X -167.5(11) . . . . ? C6X O3X Na1 O7 109.4(10) . . . . ? C7X O3X Na1 O7 -121.5(11) . . . . ? C6X O3X Na1 O6 -81.8(10) . . . . ? C7X O3X Na1 O6 47.4(11) . . . . ? C6X O3X Na1 O3 28.6(8) . . . . ? C7X O3X Na1 O3 157.7(16) . . . . ? C6X O3X Na1 O2X 18.0(10) . . . . ? C7X O3X Na1 O2X 147.2(12) . . . . ? C6X O3X Na1 O4 -152.5(12) . . . . ? C7X O3X Na1 O4 -23.3(10) . . . . ? C6X O3X Na1 O2 14.9(10) . . . . ? C7X O3X Na1 O2 144.0(11) . . . . ? C6X O3X Na1 O1 1.6(15) . . . . ? C7X O3X Na1 O1 130.8(10) . . . . ? C6X O3X Na1 O4X -152.6(11) . . . . ? C7X O3X Na1 O4X -23.5(11) . . . . ? C6X O3X Na1 O1X 26.2(12) . . . . ? C7X O3X Na1 O1X 155.4(10) . . . . ? C9 O4 Na1 O7 -57.9(4) . . . . ? C8 O4 Na1 O7 80.0(3) . . . . ? C9 O4 Na1 O6 105.4(4) . . . . ? C8 O4 Na1 O6 -116.7(3) . . . . ? C9 O4 Na1 O3 -146.5(4) . . . . ? C8 O4 Na1 O3 -8.6(3) . . . . ? C9 O4 Na1 O2X -156.7(5) . . . . ? C8 O4 Na1 O2X -18.8(5) . . . . ? C9 O4 Na1 O3X -146.9(6) . . . . ? C8 O4 Na1 O3X -9.1(5) . . . . ? C9 O4 Na1 O2 -165.0(4) . . . . ? C8 O4 Na1 O2 -27.2(4) . . . . ? C9 O4 Na1 O1 57.8(5) . . . . ? C8 O4 Na1 O1 -164.3(3) . . . . ? C9 O4 Na1 O4X 32.6(9) . . . . ? C8 O4 Na1 O4X 170.5(11) . . . . ? C4 O2 Na1 O7 55.6(5) . . . . ? C5 O2 Na1 O7 -67.3(3) . . . . ? C4 O2 Na1 O6 -112.0(5) . . . . ? C5 O2 Na1 O6 125.1(3) . . . . ? C4 O2 Na1 O3 146.6(5) . . . . ? C5 O2 Na1 O3 23.7(3) . . . . ? C4 O2 Na1 O2X 144.5(10) . . . . ? C5 O2 Na1 O2X 21.6(8) . . . . ? C4 O2 Na1 O3X 152.4(6) . . . . ? C5 O2 Na1 O3X 29.5(4) . . . . ? C4 O2 Na1 O4 165.2(5) . . . . ? C5 O2 Na1 O4 42.3(4) . . . . ? C4 O2 Na1 O1 -33.6(5) . . . . ? C5 O2 Na1 O1 -156.5(3) . . . . ? C4 O2 Na1 O4X 178.7(8) . . . . ? C5 O2 Na1 O4X 55.8(8) . . . . ? C4 O2 Na1 O1X -15.7(6) . . . . ? C5 O2 Na1 O1X -138.5(6) . . . . ? C2 O1 Na1 O7 118.9(3) . . . . ? C3 O1 Na1 O7 -92.5(3) . . . . ? C2 O1 Na1 O6 -46.0(3) . . . . ? C3 O1 Na1 O6 102.6(3) . . . . ? C2 O1 Na1 O3 -146.6(3) . . . . ? C3 O1 Na1 O3 2.0(4) . . . . ? C2 O1 Na1 O2X -147.6(4) . . . . ? C3 O1 Na1 O2X 1.1(4) . . . . ? C2 O1 Na1 O3X -132.2(8) . . . . ? C3 O1 Na1 O3X 16.4(8) . . . . ? C2 O1 Na1 O4 1.3(5) . . . . ? C3 O1 Na1 O4 149.9(4) . . . . ? C2 O1 Na1 O2 -146.9(3) . . . . ? C3 O1 Na1 O2 1.8(3) . . . . ? C2 O1 Na1 O4X 13.3(6) . . . . ? C3 O1 Na1 O4X 162.0(5) . . . . ? C2 O1 Na1 O1X -175.7(7) . . . . ? C3 O1 Na1 O1X -27.1(7) . . . . ? C8X O4X Na1 O7 82.7(11) . . . . ? C9X O4X Na1 O7 -51.2(17) . . . . ? C8X O4X Na1 O6 -113.4(11) . . . . ? C9X O4X Na1 O6 112.7(17) . . . . ? C8X O4X Na1 O3 -9.7(10) . . . . ? C9X O4X Na1 O3 -143.5(17) . . . . ? C8X O4X Na1 O2X -22.3(13) . . . . ? C9X O4X Na1 O2X -156.2(16) . . . . ? C8X O4X Na1 O3X -10.1(10) . . . . ? C9X O4X Na1 O3X -144.0(18) . . . . ? C8X O4X Na1 O4 -10.5(9) . . . . ? C9X O4X Na1 O4 -144(2) . . . . ? C8X O4X Na1 O2 -39.4(14) . . . . ? C9X O4X Na1 O2 -173.2(15) . . . . ? C8X O4X Na1 O1 -175.3(9) . . . . ? C9X O4X Na1 O1 50.8(19) . . . . ? C8X O4X Na1 O1X 172.4(12) . . . . ? C9X O4X Na1 O1X 39(2) . . . . ? C3X O1X Na1 O7 -106(2) . . . . ? C2X O1X Na1 O7 117.1(12) . . . . ? C3X O1X Na1 O6 90(2) . . . . ? C2X O1X Na1 O6 -46.2(12) . . . . ? C3X O1X Na1 O3 -17(2) . . . . ? C2X O1X Na1 O3 -153.7(11) . . . . ? C3X O1X Na1 O2X -8(2) . . . . ? C2X O1X Na1 O2X -144.2(13) . . . . ? C3X O1X Na1 O3X -16(2) . . . . ? C2X O1X Na1 O3X -152.8(11) . . . . ? C3X O1X Na1 O2 0(2) . . . . ? C2X O1X Na1 O2 -136.1(14) . . . . ? C3X O1X Na1 O1 141(2) . . . . ? C2X O1X Na1 O1 4.3(9) . . . . ? C3X O1X Na1 O4X 161(2) . . . . ? C2X O1X Na1 O4X 24(2) . . . . ? O7 Na1 O6 C14 -122.1(4) . . . . ? O3 Na1 O6 C14 78.4(3) . . . . ? O2X Na1 O6 C14 30.5(4) . . . . ? O3X Na1 O6 C14 100.7(4) . . . . ? O4 Na1 O6 C14 143.6(3) . . . . ? O2 Na1 O6 C14 8.7(3) . . . . ? O1 Na1 O6 C14 -55.1(3) . . . . ? O4X Na1 O6 C14 163.3(4) . . . . ? O1X Na1 O6 C14 -35.1(4) . . . . ? O6 Na1 O7 C13 -132.1(4) . . . . ? O3 Na1 O7 C13 27.9(3) . . . . ? O2X Na1 O7 C13 74.7(4) . . . . ? O3X Na1 O7 C13 4.9(4) . . . . ? O4 Na1 O7 C13 -40.8(3) . . . . ? O2 Na1 O7 C13 96.8(3) . . . . ? O1 Na1 O7 C13 161.9(2) . . . . ? O4X Na1 O7 C13 -61.1(4) . . . . ? O1X Na1 O7 C13 138.1(3) . . . . ? C33 B1 C15 C20 -78.2(4) . . . . ? C27 B1 C15 C20 40.6(4) . . . . ? C21 B1 C15 C20 161.0(3) . . . . ? C33 B1 C15 C16 99.0(4) . . . . ? C27 B1 C15 C16 -142.1(3) . . . . ? C21 B1 C15 C16 -21.7(4) . . . . ? C20 C15 C16 C17 0.8(5) . . . . ? B1 C15 C16 C17 -176.6(3) . . . . ? C15 C16 C17 C18 0.1(5) . . . . ? C16 C17 C18 C19 -0.1(5) . . . . ? C17 C18 C19 C20 -0.8(5) . . . . ? C18 C19 C20 C15 1.8(5) . . . . ? C16 C15 C20 C19 -1.7(5) . . . . ? B1 C15 C20 C19 175.8(3) . . . . ? C15 B1 C21 C22 -115.5(3) . . . . ? C33 B1 C21 C22 123.3(3) . . . . ? C27 B1 C21 C22 3.7(4) . . . . ? C15 B1 C21 C26 69.5(4) . . . . ? C33 B1 C21 C26 -51.7(4) . . . . ? C27 B1 C21 C26 -171.3(3) . . . . ? C26 C21 C22 C23 -0.8(4) . . . . ? B1 C21 C22 C23 -176.1(3) . . . . ? C21 C22 C23 C24 0.2(5) . . . . ? C22 C23 C24 C25 0.0(5) . . . . ? C23 C24 C25 C26 0.3(5) . . . . ? C24 C25 C26 C21 -0.9(5) . . . . ? C22 C21 C26 C25 1.1(5) . . . . ? B1 C21 C26 C25 176.6(3) . . . . ? C15 B1 C27 C32 -128.1(3) . . . . ? C33 B1 C27 C32 -9.3(4) . . . . ? C21 B1 C27 C32 109.8(3) . . . . ? C15 B1 C27 C28 52.0(4) . . . . ? C33 B1 C27 C28 170.9(3) . . . . ? C21 B1 C27 C28 -70.0(3) . . . . ? C32 C27 C28 C29 -0.7(4) . . . . ? B1 C27 C28 C29 179.1(3) . . . . ? C27 C28 C29 C30 -0.7(5) . . . . ? C28 C29 C30 C31 1.5(5) . . . . ? C29 C30 C31 C32 -0.8(5) . . . . ? C28 C27 C32 C31 1.4(4) . . . . ? B1 C27 C32 C31 -178.5(3) . . . . ? C30 C31 C32 C27 -0.6(5) . . . . ? C15 B1 C33 C34 -154.8(3) . . . . ? C27 B1 C33 C34 87.7(3) . . . . ? C21 B1 C33 C34 -32.0(4) . . . . ? C15 B1 C33 C38 28.7(4) . . . . ? C27 B1 C33 C38 -88.8(4) . . . . ? C21 B1 C33 C38 151.5(3) . . . . ? C38 C33 C34 C35 1.1(5) . . . . ? B1 C33 C34 C35 -175.6(3) . . . . ? C33 C34 C35 C36 -1.1(5) . . . . ? C34 C35 C36 C37 0.0(5) . . . . ? C35 C36 C37 C38 0.9(5) . . . . ? C36 C37 C38 C33 -0.9(5) . . . . ? C34 C33 C38 C37 -0.1(5) . . . . ? B1 C33 C38 C37 176.6(3) . . . . ? C45 B2 C39 C44 137.3(3) . . . . ? C57 B2 C39 C44 19.9(4) . . . . ? C51 B2 C39 C44 -102.4(3) . . . . ? C45 B2 C39 C40 -45.4(4) . . . . ? C57 B2 C39 C40 -162.8(3) . . . . ? C51 B2 C39 C40 74.9(4) . . . . ? C44 C39 C40 C41 2.5(5) . . . . ? B2 C39 C40 C41 -175.0(3) . . . . ? C39 C40 C41 C42 -0.5(5) . . . . ? C40 C41 C42 C43 -1.6(5) . . . . ? C41 C42 C43 C44 1.6(5) . . . . ? C42 C43 C44 C39 0.6(5) . . . . ? C40 C39 C44 C43 -2.6(5) . . . . ? B2 C39 C44 C43 174.9(3) . . . . ? C57 B2 C45 C50 84.5(3) . . . . ? C51 B2 C45 C50 -152.2(3) . . . . ? C39 B2 C45 C50 -32.4(4) . . . . ? C57 B2 C45 C46 -93.6(3) . . . . ? C51 B2 C45 C46 29.7(4) . . . . ? C39 B2 C45 C46 149.5(3) . . . . ? C50 C45 C46 C47 -0.4(5) . . . . ? B2 C45 C46 C47 177.8(3) . . . . ? C45 C46 C47 C48 -0.7(5) . . . . ? C46 C47 C48 C49 0.8(5) . . . . ? C47 C48 C49 C50 0.2(5) . . . . ? C48 C49 C50 C45 -1.4(5) . . . . ? C46 C45 C50 C49 1.5(5) . . . . ? B2 C45 C50 C49 -176.8(3) . . . . ? C45 B2 C51 C56 102.2(3) . . . . ? C57 B2 C51 C56 -137.1(3) . . . . ? C39 B2 C51 C56 -17.8(4) . . . . ? C45 B2 C51 C52 -75.5(4) . . . . ? C57 B2 C51 C52 45.3(4) . . . . ? C39 B2 C51 C52 164.5(3) . . . . ? C56 C51 C52 C53 0.5(5) . . . . ? B2 C51 C52 C53 178.4(3) . . . . ? C51 C52 C53 C54 -0.2(5) . . . . ? C52 C53 C54 C55 -0.7(5) . . . . ? C53 C54 C55 C56 1.2(5) . . . . ? C54 C55 C56 C51 -0.8(5) . . . . ? C52 C51 C56 C55 0.0(5) . . . . ? B2 C51 C56 C55 -177.9(3) . . . . ? C45 B2 C57 C62 -50.0(4) . . . . ? C51 B2 C57 C62 -171.8(3) . . . . ? C39 B2 C57 C62 68.2(4) . . . . ? C45 B2 C57 C58 135.2(3) . . . . ? C51 B2 C57 C58 13.4(4) . . . . ? C39 B2 C57 C58 -106.6(3) . . . . ? C62 C57 C58 C59 1.2(5) . . . . ? B2 C57 C58 C59 176.3(3) . . . . ? C57 C58 C59 C60 -1.9(5) . . . . ? C58 C59 C60 C61 0.8(5) . . . . ? C59 C60 C61 C62 0.9(5) . . . . ? C60 C61 C62 C57 -1.6(5) . . . . ? C58 C57 C62 C61 0.5(5) . . . . ? B2 C57 C62 C61 -174.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.659 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.050 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 630550' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H48 N Na O10 S2 2+, (C24 H20 B 1-)2, 2(C D Cl3)' _chemical_formula_sum 'C74 H88 B2 Cl6 D2 N Na O10 S2' _chemical_formula_weight 1476.91 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' Na Na 0.0362 0.0249 '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 13.6709(6) _cell_length_b 14.2510(7) _cell_length_c 22.0061(10) _cell_angle_alpha 95.678(2) _cell_angle_beta 98.668(2) _cell_angle_gamma 114.616(2) _cell_volume 3790.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10083 _cell_measurement_theta_min 2.254 _cell_measurement_theta_max 27.392 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.294 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 0.344 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.872 _exptl_absorpt_correction_T_max 0.895 _exptl_absorpt_process_details 'SADABS v2.10, Sheldrick, G.M., (2003)' _exptl_special_details ; 'SADABS v2.10 (Sheldrick, 2003)' ; _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 33152 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 28.98 _reflns_number_total 17365 _reflns_number_gt 10786 _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^)+(0.1152P)^2^+4.5092P] 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 17365 _refine_ls_number_parameters 865 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1170 _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.2376 _refine_ls_wR_factor_gt 0.1948 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na1 Na 1.08753(10) 0.30043(10) 0.23609(6) 0.0361(3) Uani 1 1 d . . . N1 N 0.7023(3) 0.1635(3) 0.26647(16) 0.0566(9) Uani 1 1 d . . . S1 S 0.65966(8) 0.05250(9) 0.21768(4) 0.0512(3) Uani 1 1 d . . . C1 C 0.5478(4) -0.0323(5) 0.2501(2) 0.0778(15) Uani 1 1 d . . . H1A H 0.4946 -0.0024 0.2526 0.093 Uiso 1 1 calc R . . H1B H 0.5088 -0.1023 0.2230 0.093 Uiso 1 1 calc R . . C2 C 0.5943(5) -0.0421(5) 0.3144(2) 0.0865(18) Uani 1 1 d . . . H2A H 0.6260 0.0263 0.3431 0.104 Uiso 1 1 calc R . . H2B H 0.5359 -0.0942 0.3314 0.104 Uiso 1 1 calc R . . O1 O 0.6764(3) -0.0748(3) 0.30773(14) 0.0799(11) Uani 1 1 d . . . C3 C 0.7380(5) -0.0779(4) 0.3648(2) 0.093(2) Uani 1 1 d . . . H3A H 0.6915 -0.1359 0.3841 0.111 Uiso 1 1 calc R . . H3B H 0.7639 -0.0111 0.3944 0.111 Uiso 1 1 calc R . . C4 C 0.8335(5) -0.0941(4) 0.3512(3) 0.090(2) Uani 1 1 d . . . H4A H 0.8693 -0.1109 0.3883 0.108 Uiso 1 1 calc R . . H4B H 0.8083 -0.1536 0.3161 0.108 Uiso 1 1 calc R . . O2 O 0.9097(3) -0.0013(2) 0.33512(14) 0.0637(8) Uani 1 1 d . . . C5 C 0.9983(5) -0.0132(4) 0.3172(2) 0.0736(15) Uani 1 1 d . . . H5A H 0.9707 -0.0710 0.2808 0.088 Uiso 1 1 calc R . . H5B H 1.0380 -0.0316 0.3519 0.088 Uiso 1 1 calc R . . C6 C 1.0751(4) 0.0866(4) 0.3003(2) 0.0609(11) Uani 1 1 d . . . H6A H 1.1037 0.1433 0.3374 0.073 Uiso 1 1 calc R . . H6B H 1.1386 0.0776 0.2891 0.073 Uiso 1 1 calc R . . O3 O 1.0247(2) 0.1178(2) 0.24956(12) 0.0476(6) Uani 1 1 d . . . C7 C 1.0108(4) 0.0587(4) 0.18980(19) 0.0596(11) Uani 1 1 d . . . H7A H 0.9840 -0.0167 0.1921 0.071 Uiso 1 1 calc R . . H7B H 1.0819 0.0829 0.1763 0.071 Uiso 1 1 calc R . . C8 C 0.9287(4) 0.0750(3) 0.14449(19) 0.0568(11) Uani 1 1 d . . . H8A H 0.9157 0.0339 0.1027 0.068 Uiso 1 1 calc R . . H8B H 0.8578 0.0511 0.1583 0.068 Uiso 1 1 calc R . . O4 O 0.9704(2) 0.1834(2) 0.14155(11) 0.0465(6) Uani 1 1 d . . . C9 C 0.9156(3) 0.2064(4) 0.08862(16) 0.0518(10) Uani 1 1 d . . . H9A H 0.8868 0.1460 0.0538 0.062 Uiso 1 1 calc R . . H9B H 0.9696 0.2679 0.0751 0.062 Uiso 1 1 calc R . . C10 C 0.8229(3) 0.2290(3) 0.10176(19) 0.0550(10) Uani 1 1 d . . . H10A H 0.8499 0.2868 0.1380 0.066 Uiso 1 1 calc R . . H10B H 0.7923 0.2511 0.0652 0.066 Uiso 1 1 calc R . . O5 O 0.7410(2) 0.1388(2) 0.11449(12) 0.0501(6) Uani 1 1 d . . . C11 C 0.6465(3) 0.1540(4) 0.1225(2) 0.0605(11) Uani 1 1 d . . . H11A H 0.6058 0.1563 0.0819 0.073 Uiso 1 1 calc R . . H11B H 0.6687 0.2207 0.1514 0.073 Uiso 1 1 calc R . . C12 C 0.5770(3) 0.0634(4) 0.1490(2) 0.0633(12) Uani 1 1 d . . . H12A H 0.5472 -0.0018 0.1176 0.076 Uiso 1 1 calc R . . H12B H 0.5143 0.0738 0.1602 0.076 Uiso 1 1 calc R . . S2 S 0.83795(7) 0.23174(7) 0.28146(4) 0.0392(2) Uani 1 1 d . . . C13 C 0.8787(3) 0.2200(3) 0.36096(16) 0.0435(8) Uani 1 1 d . . . H13A H 0.8199 0.2164 0.3833 0.052 Uiso 1 1 calc R . . H13B H 0.8843 0.1529 0.3607 0.052 Uiso 1 1 calc R . . C14 C 0.9861(3) 0.3076(3) 0.39723(15) 0.0394(7) Uani 1 1 d . . . H14A H 0.9796 0.3744 0.4022 0.047 Uiso 1 1 calc R . . H14B H 1.0044 0.2926 0.4393 0.047 Uiso 1 1 calc R . . O6 O 1.07059(18) 0.31656(18) 0.36458(10) 0.0375(5) Uani 1 1 d . . . C15 C 1.1759(3) 0.3963(3) 0.39959(16) 0.0424(8) Uani 1 1 d . . . H15A H 1.1806 0.3951 0.4448 0.051 Uiso 1 1 calc R . . H15B H 1.1841 0.4664 0.3924 0.051 Uiso 1 1 calc R . . C16 C 1.2657(3) 0.3755(3) 0.37883(15) 0.0410(8) Uani 1 1 d . . . H16A H 1.3383 0.4279 0.4037 0.049 Uiso 1 1 calc R . . H16B H 1.2568 0.3049 0.3853 0.049 Uiso 1 1 calc R . . O7 O 1.26009(18) 0.38192(19) 0.31471(10) 0.0395(5) Uani 1 1 d . . . C17 C 1.3525(3) 0.3765(3) 0.29440(17) 0.0455(8) Uani 1 1 d . . . H17A H 1.3501 0.3064 0.2963 0.055 Uiso 1 1 calc R . . H17B H 1.4220 0.4301 0.3218 0.055 Uiso 1 1 calc R . . C18 C 1.3470(3) 0.3959(3) 0.22843(17) 0.0505(9) Uani 1 1 d . . . H18A H 1.3470 0.4649 0.2263 0.061 Uiso 1 1 calc R . . H18B H 1.4115 0.3956 0.2133 0.061 Uiso 1 1 calc R . . O8 O 1.2485(2) 0.3146(2) 0.19124(11) 0.0487(6) Uani 1 1 d . . . C19 C 1.2271(4) 0.3265(4) 0.12796(17) 0.0603(11) Uani 1 1 d . . . H19A H 1.1645 0.2614 0.1038 0.072 Uiso 1 1 calc R . . H19B H 1.2924 0.3364 0.1102 0.072 Uiso 1 1 calc R . . C20 C 1.2008(4) 0.4177(4) 0.12088(19) 0.0644(12) Uani 1 1 d . . . H20A H 1.2693 0.4843 0.1317 0.077 Uiso 1 1 calc R . . H20B H 1.1641 0.4107 0.0772 0.077 Uiso 1 1 calc R . . O9 O 1.1293(2) 0.4176(2) 0.16226(13) 0.0553(7) Uani 1 1 d . . . C21 C 1.0918(4) 0.4955(3) 0.1586(2) 0.0596(11) Uani 1 1 d . . . H21A H 1.0270 0.4709 0.1238 0.072 Uiso 1 1 calc R . . H21B H 1.1504 0.5601 0.1507 0.072 Uiso 1 1 calc R . . C22 C 1.0612(4) 0.5182(3) 0.2191(2) 0.0710(13) Uani 1 1 d . . . H22A H 1.1282 0.5507 0.2529 0.085 Uiso 1 1 calc R . . H22B H 1.0293 0.5689 0.2156 0.085 Uiso 1 1 calc R . . O10 O 0.9852(3) 0.42697(19) 0.23424(13) 0.0546(7) Uani 1 1 d . . . C23 C 0.9511(4) 0.4481(3) 0.28988(18) 0.0564(11) Uani 1 1 d . . . H23A H 0.9441 0.5146 0.2916 0.068 Uiso 1 1 calc R . . H23B H 1.0067 0.4555 0.3268 0.068 Uiso 1 1 calc R . . C24 C 0.8426(4) 0.3599(3) 0.29072(18) 0.0525(10) Uani 1 1 d . . . H24A H 0.7862 0.3602 0.2569 0.063 Uiso 1 1 calc R . . H24B H 0.8223 0.3734 0.3309 0.063 Uiso 1 1 calc R . . B1 B 0.7496(3) 0.5833(3) 0.38777(15) 0.0290(7) Uani 1 1 d . . . C25 C 0.7437(2) 0.4811(2) 0.41946(13) 0.0289(6) Uani 1 1 d . . . C26 C 0.6441(3) 0.3908(3) 0.41348(16) 0.0389(7) Uani 1 1 d . . . H26 H 0.5785 0.3892 0.3906 0.047 Uiso 1 1 calc R . . C27 C 0.6373(3) 0.3041(3) 0.43936(19) 0.0446(8) Uani 1 1 d . . . H27 H 0.5681 0.2448 0.4334 0.054 Uiso 1 1 calc R . . C28 C 0.7299(3) 0.3031(3) 0.47372(17) 0.0420(8) Uani 1 1 d . . . H28 H 0.7251 0.2436 0.4915 0.050 Uiso 1 1 calc R . . C29 C 0.8301(3) 0.3904(3) 0.48169(15) 0.0372(7) Uani 1 1 d . . . H29 H 0.8947 0.3916 0.5056 0.045 Uiso 1 1 calc R . . C30 C 0.8361(2) 0.4769(2) 0.45461(13) 0.0305(6) Uani 1 1 d . . . H30 H 0.9058 0.5355 0.4602 0.037 Uiso 1 1 calc R . . C31 C 0.8621(2) 0.6884(2) 0.42469(13) 0.0288(6) Uani 1 1 d . . . C32 C 0.9676(3) 0.7069(2) 0.41498(14) 0.0323(6) Uani 1 1 d . . . H32 H 0.9741 0.6567 0.3862 0.039 Uiso 1 1 calc R . . C33 C 1.0623(3) 0.7949(3) 0.44543(15) 0.0388(7) Uani 1 1 d . . . H33 H 1.1316 0.8037 0.4372 0.047 Uiso 1 1 calc R . . C34 C 1.0568(3) 0.8701(3) 0.48783(15) 0.0433(8) Uani 1 1 d . . . H34 H 1.1215 0.9313 0.5081 0.052 Uiso 1 1 calc R . . C35 C 0.9555(3) 0.8544(3) 0.50005(16) 0.0428(8) Uani 1 1 d . . . H35 H 0.9504 0.9043 0.5298 0.051 Uiso 1 1 calc R . . C36 C 0.8612(3) 0.7660(2) 0.46905(14) 0.0350(7) Uani 1 1 d . . . H36 H 0.7926 0.7575 0.4783 0.042 Uiso 1 1 calc R . . C37 C 0.6421(2) 0.6044(2) 0.39494(14) 0.0320(6) Uani 1 1 d . . . C38 C 0.5999(3) 0.5948(3) 0.44911(16) 0.0384(7) Uani 1 1 d . . . H38 H 0.6302 0.5688 0.4813 0.046 Uiso 1 1 calc R . . C39 C 0.5156(3) 0.6215(3) 0.45820(19) 0.0457(8) Uani 1 1 d . . . H39 H 0.4912 0.6157 0.4964 0.055 Uiso 1 1 calc R . . C40 C 0.4679(3) 0.6562(3) 0.4121(2) 0.0512(10) Uani 1 1 d . . . H40 H 0.4103 0.6746 0.4180 0.061 Uiso 1 1 calc R . . C41 C 0.5046(3) 0.6642(3) 0.3568(2) 0.0531(10) Uani 1 1 d . . . H41 H 0.4708 0.6865 0.3240 0.064 Uiso 1 1 calc R . . C42 C 0.5909(3) 0.6399(3) 0.34889(17) 0.0412(8) Uani 1 1 d . . . H42 H 0.6160 0.6476 0.3109 0.049 Uiso 1 1 calc R . . C43 C 0.7470(3) 0.5591(3) 0.31236(14) 0.0332(7) Uani 1 1 d . . . C44 C 0.8157(3) 0.6311(3) 0.28049(15) 0.0414(8) Uani 1 1 d . . . H44 H 0.8682 0.6978 0.3035 0.050 Uiso 1 1 calc R . . C45 C 0.8108(3) 0.6092(4) 0.21653(17) 0.0539(10) Uani 1 1 d . . . H45 H 0.8601 0.6599 0.1971 0.065 Uiso 1 1 calc R . . C46 C 0.7337(4) 0.5135(4) 0.18162(17) 0.0616(12) Uani 1 1 d . . . H46 H 0.7310 0.4970 0.1383 0.074 Uiso 1 1 calc R . . C47 C 0.6604(4) 0.4419(4) 0.21067(17) 0.0577(11) Uani 1 1 d . . . H47 H 0.6048 0.3772 0.1869 0.069 Uiso 1 1 calc R . . C48 C 0.6685(3) 0.4651(3) 0.27443(15) 0.0420(8) Uani 1 1 d . . . H48 H 0.6181 0.4144 0.2934 0.050 Uiso 1 1 calc R . . B2 B 0.8212(3) 0.1685(3) 0.88937(17) 0.0313(7) Uani 1 1 d . . . C49 C 0.9492(3) 0.1909(2) 0.91768(14) 0.0320(6) Uani 1 1 d . . . C50 C 1.0391(3) 0.2834(3) 0.91334(15) 0.0350(7) Uani 1 1 d . . . H50 H 1.0251 0.3330 0.8923 0.042 Uiso 1 1 calc R . . C51 C 1.1476(3) 0.3059(3) 0.93829(15) 0.0394(7) Uani 1 1 d . . . H51 H 1.2057 0.3697 0.9343 0.047 Uiso 1 1 calc R . . C52 C 1.1710(3) 0.2347(3) 0.96920(15) 0.0416(8) Uani 1 1 d . . . H52 H 1.2450 0.2497 0.9867 0.050 Uiso 1 1 calc R . . C53 C 1.0856(3) 0.1423(3) 0.97413(15) 0.0418(8) Uani 1 1 d . . . H53 H 1.1003 0.0932 0.9954 0.050 Uiso 1 1 calc R . . C54 C 0.9775(3) 0.1209(3) 0.94800(15) 0.0358(7) Uani 1 1 d . . . H54 H 0.9202 0.0556 0.9508 0.043 Uiso 1 1 calc R . . C55 C 0.7394(3) 0.0447(2) 0.88885(16) 0.0360(7) Uani 1 1 d . . . C56 C 0.7086(3) -0.0345(3) 0.83737(19) 0.0464(8) Uani 1 1 d . . . H56 H 0.7294 -0.0159 0.7994 0.056 Uiso 1 1 calc R . . C57 C 0.6480(4) -0.1403(3) 0.8397(2) 0.0630(12) Uani 1 1 d . . . H57 H 0.6292 -0.1921 0.8038 0.076 Uiso 1 1 calc R . . C58 C 0.6156(4) -0.1701(3) 0.8934(2) 0.0621(12) Uani 1 1 d . . . H58 H 0.5742 -0.2421 0.8947 0.075 Uiso 1 1 calc R . . C59 C 0.6432(3) -0.0954(3) 0.9451(2) 0.0528(10) Uani 1 1 d . . . H59 H 0.6216 -0.1153 0.9827 0.063 Uiso 1 1 calc R . . C60 C 0.7031(3) 0.0104(3) 0.94247(18) 0.0448(8) Uani 1 1 d . . . H60 H 0.7200 0.0613 0.9786 0.054 Uiso 1 1 calc R . . C61 C 0.7852(3) 0.2462(2) 0.93174(14) 0.0306(6) Uani 1 1 d . . . C62 C 0.6745(3) 0.2189(3) 0.93243(16) 0.0387(7) Uani 1 1 d . . . H62 H 0.6206 0.1523 0.9099 0.046 Uiso 1 1 calc R . . C63 C 0.6393(3) 0.2838(3) 0.96429(16) 0.0426(8) Uani 1 1 d . . . H63 H 0.5630 0.2611 0.9633 0.051 Uiso 1 1 calc R . . C64 C 0.7147(3) 0.3811(3) 0.99751(16) 0.0429(8) Uani 1 1 d . . . H64 H 0.6911 0.4264 1.0190 0.051 Uiso 1 1 calc R . . C65 C 0.8248(3) 0.4115(3) 0.99886(16) 0.0414(8) Uani 1 1 d . . . H65 H 0.8778 0.4782 1.0217 0.050 Uiso 1 1 calc R . . C66 C 0.8592(3) 0.3448(2) 0.96683(14) 0.0338(7) Uani 1 1 d . . . H66 H 0.9358 0.3673 0.9690 0.041 Uiso 1 1 calc R . . C67 C 0.8109(2) 0.1920(2) 0.81701(14) 0.0311(6) Uani 1 1 d . . . C68 C 0.7309(3) 0.2209(3) 0.78944(15) 0.0373(7) Uani 1 1 d . . . H68 H 0.6825 0.2300 0.8137 0.045 Uiso 1 1 calc R . . C69 C 0.7191(3) 0.2370(3) 0.72782(17) 0.0438(8) Uani 1 1 d . . . H69 H 0.6623 0.2548 0.7108 0.053 Uiso 1 1 calc R . . C70 C 0.7893(3) 0.2273(3) 0.69142(16) 0.0415(8) Uani 1 1 d . . . H70 H 0.7825 0.2398 0.6497 0.050 Uiso 1 1 calc R . . C71 C 0.8697(3) 0.1991(3) 0.71668(15) 0.0398(7) Uani 1 1 d . . . H71 H 0.9187 0.1919 0.6923 0.048 Uiso 1 1 calc R . . C72 C 0.8789(3) 0.1812(3) 0.77791(15) 0.0371(7) Uani 1 1 d . . . H72 H 0.9340 0.1606 0.7939 0.044 Uiso 1 1 calc R . . C73 C 0.5926(5) 0.6756(5) 0.1538(3) 0.108(2) Uani 1 1 d . . . H73 H 0.6408 0.6549 0.1828 0.129 Uiso 1 1 calc R . . Cl1 Cl 0.48489(12) 0.67360(12) 0.18831(7) 0.0857(4) Uani 1 1 d . . . Cl3 Cl 0.54357(16) 0.58782(17) 0.08209(9) 0.1236(7) Uani 1 1 d . . . C74 C 0.6825(4) 0.9709(4) 0.6026(2) 0.0664(12) Uani 1 1 d . . . H74 H 0.7558 1.0316 0.6208 0.080 Uiso 1 1 calc R . . Cl4 Cl 0.62636(13) 0.91665(14) 0.66357(6) 0.0955(5) Uani 1 1 d . . . Cl5 Cl 0.70273(13) 0.87990(11) 0.55449(7) 0.0868(4) Uani 1 1 d . . . Cl6 Cl 0.59846(15) 1.01755(14) 0.56064(8) 0.1127(6) Uani 1 1 d . . . Cl2 Cl 0.67040(17) 0.80114(17) 0.14155(11) 0.1375(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.0357(7) 0.0434(7) 0.0272(6) 0.0046(5) 0.0021(5) 0.0171(6) N1 0.0393(17) 0.081(2) 0.0460(18) -0.0038(17) 0.0078(14) 0.0269(17) S1 0.0356(5) 0.0710(7) 0.0368(5) 0.0051(4) 0.0052(4) 0.0154(4) C1 0.046(2) 0.099(4) 0.057(3) 0.009(3) 0.014(2) 0.002(2) C2 0.066(3) 0.100(4) 0.051(3) 0.016(3) 0.016(2) -0.006(3) O1 0.074(2) 0.085(2) 0.0446(17) 0.0170(16) -0.0012(16) 0.0032(19) C3 0.094(4) 0.073(3) 0.048(3) 0.028(2) -0.009(3) -0.019(3) C4 0.111(5) 0.044(3) 0.070(3) 0.027(2) -0.025(3) 0.002(3) O2 0.085(2) 0.0367(14) 0.0545(17) 0.0120(12) -0.0079(15) 0.0189(15) C5 0.102(4) 0.057(3) 0.063(3) 0.003(2) -0.022(3) 0.051(3) C6 0.065(3) 0.062(3) 0.061(3) 0.001(2) -0.010(2) 0.043(2) O3 0.0535(15) 0.0485(14) 0.0435(14) -0.0037(11) -0.0012(11) 0.0315(12) C7 0.071(3) 0.065(3) 0.052(2) -0.0122(19) 0.001(2) 0.047(2) C8 0.063(3) 0.057(2) 0.047(2) -0.0141(18) -0.0061(18) 0.034(2) O4 0.0425(13) 0.0546(15) 0.0334(12) 0.0019(11) -0.0019(10) 0.0174(12) C9 0.045(2) 0.074(3) 0.0255(16) 0.0101(17) 0.0023(14) 0.0169(19) C10 0.050(2) 0.060(2) 0.044(2) 0.0150(18) -0.0034(17) 0.0167(19) O5 0.0475(14) 0.0550(16) 0.0488(15) 0.0114(12) 0.0074(12) 0.0240(13) C11 0.049(2) 0.090(3) 0.051(2) 0.015(2) 0.0013(18) 0.041(2) C12 0.039(2) 0.100(4) 0.047(2) 0.008(2) 0.0011(17) 0.030(2) S2 0.0380(4) 0.0496(5) 0.0344(4) 0.0037(4) 0.0074(3) 0.0244(4) C13 0.0417(19) 0.051(2) 0.0386(18) 0.0130(16) 0.0105(15) 0.0191(16) C14 0.0443(19) 0.047(2) 0.0312(16) 0.0076(14) 0.0083(14) 0.0241(16) O6 0.0381(12) 0.0416(13) 0.0300(11) 0.0004(9) 0.0031(9) 0.0174(10) C15 0.0453(19) 0.0433(19) 0.0295(16) -0.0031(14) 0.0009(14) 0.0154(16) C16 0.0384(18) 0.0471(19) 0.0283(16) 0.0027(14) -0.0024(13) 0.0141(15) O7 0.0356(12) 0.0516(14) 0.0279(11) 0.0052(10) 0.0011(9) 0.0181(11) C17 0.0353(18) 0.058(2) 0.0421(19) 0.0077(17) 0.0035(15) 0.0216(17) C18 0.0366(18) 0.069(3) 0.042(2) 0.0089(18) 0.0075(15) 0.0190(18) O8 0.0428(14) 0.0701(18) 0.0314(12) 0.0060(12) 0.0071(10) 0.0239(13) C19 0.053(2) 0.099(3) 0.0304(18) 0.011(2) 0.0142(17) 0.032(2) C20 0.051(2) 0.096(4) 0.040(2) 0.027(2) 0.0111(18) 0.021(2) O9 0.0581(16) 0.0586(17) 0.0518(16) 0.0267(13) 0.0172(13) 0.0227(14) C21 0.074(3) 0.044(2) 0.054(2) 0.0232(19) 0.006(2) 0.020(2) C22 0.089(3) 0.039(2) 0.082(3) 0.024(2) 0.013(3) 0.024(2) O10 0.085(2) 0.0339(13) 0.0490(15) 0.0096(11) 0.0165(14) 0.0285(14) C23 0.094(3) 0.044(2) 0.044(2) 0.0015(17) 0.005(2) 0.047(2) C24 0.071(3) 0.063(3) 0.040(2) 0.0012(17) 0.0031(18) 0.050(2) B1 0.0288(16) 0.0351(18) 0.0239(15) -0.0008(13) -0.0007(13) 0.0180(14) C25 0.0297(14) 0.0349(16) 0.0234(13) -0.0026(11) 0.0024(11) 0.0183(13) C26 0.0304(16) 0.0417(18) 0.0428(18) -0.0003(14) 0.0016(13) 0.0179(14) C27 0.0358(18) 0.0351(18) 0.061(2) 0.0054(16) 0.0130(16) 0.0136(15) C28 0.0459(19) 0.0381(18) 0.051(2) 0.0121(15) 0.0160(16) 0.0240(16) C29 0.0385(17) 0.0451(19) 0.0366(17) 0.0080(14) 0.0059(14) 0.0270(15) C30 0.0298(15) 0.0348(16) 0.0272(14) 0.0011(12) 0.0039(12) 0.0161(13) C31 0.0356(15) 0.0327(15) 0.0204(13) 0.0055(11) 0.0003(11) 0.0189(13) C32 0.0336(16) 0.0364(16) 0.0265(14) 0.0050(12) 0.0023(12) 0.0166(13) C33 0.0352(17) 0.0474(19) 0.0302(16) 0.0147(14) 0.0033(13) 0.0143(15) C34 0.051(2) 0.0347(17) 0.0292(16) 0.0051(13) -0.0053(15) 0.0090(15) C35 0.059(2) 0.0340(17) 0.0324(17) 0.0006(13) 0.0029(15) 0.0212(16) C36 0.0451(18) 0.0337(16) 0.0294(15) 0.0049(12) 0.0058(13) 0.0212(14) C37 0.0311(15) 0.0364(16) 0.0299(15) -0.0005(12) 0.0029(12) 0.0185(13) C38 0.0401(18) 0.0440(19) 0.0346(17) 0.0017(14) 0.0078(14) 0.0229(15) C39 0.0414(19) 0.045(2) 0.053(2) 0.0014(16) 0.0181(16) 0.0206(16) C40 0.0365(18) 0.050(2) 0.075(3) 0.0029(19) 0.0153(18) 0.0278(17) C41 0.048(2) 0.060(2) 0.063(3) 0.012(2) 0.0040(19) 0.038(2) C42 0.0406(18) 0.052(2) 0.0404(18) 0.0094(15) 0.0060(14) 0.0303(16) C43 0.0357(16) 0.0472(18) 0.0255(14) 0.0016(13) 0.0011(12) 0.0295(15) C44 0.0424(18) 0.066(2) 0.0251(15) 0.0081(15) 0.0047(13) 0.0337(18) C45 0.057(2) 0.091(3) 0.0301(18) 0.0144(19) 0.0101(16) 0.047(2) C46 0.085(3) 0.104(4) 0.0216(17) 0.004(2) 0.0025(19) 0.071(3) C47 0.075(3) 0.072(3) 0.0318(19) -0.0130(18) -0.0125(18) 0.051(2) C48 0.0478(19) 0.053(2) 0.0297(16) -0.0042(14) -0.0022(14) 0.0322(17) B2 0.0296(17) 0.0284(17) 0.0335(18) 0.0014(14) 0.0024(14) 0.0127(14) C49 0.0357(16) 0.0349(16) 0.0254(14) -0.0002(12) 0.0026(12) 0.0181(13) C50 0.0357(16) 0.0375(17) 0.0320(16) 0.0045(13) 0.0042(13) 0.0174(14) C51 0.0342(17) 0.049(2) 0.0349(17) 0.0038(14) 0.0067(13) 0.0187(15) C52 0.0390(18) 0.061(2) 0.0293(16) 0.0007(15) 0.0019(13) 0.0298(17) C53 0.053(2) 0.049(2) 0.0326(17) 0.0045(15) 0.0034(15) 0.0347(18) C54 0.0401(17) 0.0373(17) 0.0328(16) 0.0035(13) 0.0047(13) 0.0211(14) C55 0.0307(16) 0.0316(16) 0.0408(18) 0.0017(13) -0.0036(13) 0.0137(13) C56 0.044(2) 0.0359(18) 0.055(2) -0.0029(16) 0.0063(16) 0.0182(16) C57 0.060(3) 0.036(2) 0.081(3) -0.012(2) 0.002(2) 0.0192(19) C58 0.051(2) 0.033(2) 0.093(4) 0.014(2) 0.003(2) 0.0129(17) C59 0.0382(19) 0.045(2) 0.064(2) 0.0198(19) -0.0018(17) 0.0095(16) C60 0.0396(18) 0.0357(18) 0.046(2) 0.0061(15) -0.0055(15) 0.0090(15) C61 0.0353(16) 0.0308(15) 0.0260(14) 0.0053(12) 0.0039(12) 0.0154(13) C62 0.0346(17) 0.0386(18) 0.0383(18) 0.0001(14) 0.0022(14) 0.0150(14) C63 0.0376(18) 0.054(2) 0.0395(18) 0.0078(16) 0.0072(14) 0.0238(16) C64 0.054(2) 0.050(2) 0.0326(17) 0.0007(15) 0.0081(15) 0.0320(18) C65 0.051(2) 0.0360(18) 0.0333(17) 0.0000(14) 0.0066(15) 0.0179(16) C66 0.0352(16) 0.0349(16) 0.0298(15) 0.0064(13) 0.0067(13) 0.0138(14) C67 0.0305(15) 0.0279(15) 0.0304(15) -0.0009(12) -0.0009(12) 0.0121(12) C68 0.0369(17) 0.0405(18) 0.0376(17) 0.0031(14) 0.0045(14) 0.0218(15) C69 0.0436(19) 0.051(2) 0.0407(19) 0.0061(16) -0.0016(15) 0.0286(17) C70 0.049(2) 0.0447(19) 0.0298(16) 0.0024(14) 0.0004(14) 0.0236(16) C71 0.0441(18) 0.0442(19) 0.0316(16) 0.0003(14) 0.0050(14) 0.0223(16) C72 0.0384(17) 0.0418(18) 0.0322(16) -0.0015(13) -0.0002(13) 0.0232(15) C73 0.097(4) 0.105(5) 0.115(5) -0.029(4) -0.044(4) 0.072(4) Cl1 0.0830(9) 0.0996(10) 0.0765(8) 0.0304(8) 0.0146(7) 0.0395(8) Cl3 0.1137(13) 0.1391(15) 0.1200(14) -0.0391(11) -0.0304(10) 0.0894(12) C74 0.060(3) 0.058(3) 0.065(3) -0.008(2) -0.014(2) 0.023(2) Cl4 0.0939(10) 0.1239(13) 0.0599(8) -0.0051(8) 0.0037(7) 0.0482(9) Cl5 0.1053(11) 0.0739(8) 0.0817(9) 0.0027(7) 0.0239(8) 0.0410(8) Cl6 0.1151(12) 0.0977(11) 0.1076(12) -0.0089(9) -0.0496(10) 0.0602(10) Cl2 0.1112(14) 0.1203(15) 0.1609(19) -0.0110(13) 0.0833(14) 0.0213(11) _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 Na1 O4 2.400(3) . ? Na1 O9 2.404(3) . ? Na1 O3 2.443(3) . ? Na1 O7 2.449(2) . ? Na1 O8 2.486(3) . ? Na1 O10 2.704(3) . ? Na1 O6 2.866(2) . ? N1 S1 1.643(4) . ? N1 S2 1.656(3) . ? S1 C12 1.807(4) . ? S1 C1 1.808(5) . ? C1 C2 1.505(7) . ? C2 O1 1.404(7) . ? O1 C3 1.419(6) . ? C3 C4 1.485(9) . ? C4 O2 1.420(6) . ? O2 C5 1.397(6) . ? C5 C6 1.498(7) . ? C6 O3 1.429(5) . ? O3 C7 1.431(4) . ? C7 C8 1.495(6) . ? C8 O4 1.418(5) . ? O4 C9 1.429(4) . ? C9 C10 1.492(6) . ? C10 O5 1.397(5) . ? O5 C11 1.429(5) . ? C11 C12 1.485(7) . ? S2 C24 1.790(4) . ? S2 C13 1.800(4) . ? C13 C14 1.509(5) . ? C14 O6 1.418(4) . ? O6 C15 1.444(4) . ? C15 C16 1.500(5) . ? C16 O7 1.416(4) . ? O7 C17 1.431(4) . ? C17 C18 1.501(5) . ? C18 O8 1.416(4) . ? O8 C19 1.421(4) . ? C19 C20 1.502(7) . ? C20 O9 1.433(5) . ? O9 C21 1.407(5) . ? C21 C22 1.498(7) . ? C22 O10 1.395(5) . ? O10 C23 1.422(5) . ? C23 C24 1.496(6) . ? B1 C37 1.644(4) . ? B1 C31 1.653(4) . ? B1 C43 1.653(4) . ? B1 C25 1.653(5) . ? C25 C30 1.406(4) . ? C25 C26 1.408(5) . ? C26 C27 1.384(5) . ? C27 C28 1.381(5) . ? C28 C29 1.386(5) . ? C29 C30 1.398(4) . ? C31 C36 1.406(4) . ? C31 C32 1.409(4) . ? C32 C33 1.385(5) . ? C33 C34 1.384(5) . ? C34 C35 1.381(5) . ? C35 C36 1.388(5) . ? C37 C38 1.395(4) . ? C37 C42 1.398(4) . ? C38 C39 1.390(5) . ? C39 C40 1.366(6) . ? C40 C41 1.382(6) . ? C41 C42 1.391(5) . ? C43 C48 1.398(5) . ? C43 C44 1.401(5) . ? C44 C45 1.396(5) . ? C45 C46 1.383(7) . ? C46 C47 1.387(7) . ? C47 C48 1.386(5) . ? B2 C55 1.647(5) . ? B2 C49 1.648(5) . ? B2 C61 1.651(5) . ? B2 C67 1.657(5) . ? C49 C50 1.402(5) . ? C49 C54 1.403(4) . ? C50 C51 1.388(4) . ? C51 C52 1.391(5) . ? C52 C53 1.376(5) . ? C53 C54 1.393(5) . ? C55 C56 1.393(5) . ? C55 C60 1.402(5) . ? C56 C57 1.397(6) . ? C57 C58 1.368(7) . ? C58 C59 1.366(6) . ? C59 C60 1.396(5) . ? C61 C66 1.400(4) . ? C61 C62 1.400(4) . ? C62 C63 1.387(5) . ? C63 C64 1.380(5) . ? C64 C65 1.376(5) . ? C65 C66 1.401(5) . ? C67 C68 1.400(4) . ? C67 C72 1.401(5) . ? C68 C69 1.394(5) . ? C69 C70 1.379(5) . ? C70 C71 1.381(5) . ? C71 C72 1.393(5) . ? C73 Cl2 1.733(8) . ? C73 Cl1 1.746(7) . ? C73 Cl3 1.761(6) . ? C74 Cl5 1.730(5) . ? C74 Cl4 1.735(6) . ? C74 Cl6 1.747(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Na1 O9 79.47(10) . . ? O4 Na1 O3 69.20(9) . . ? O9 Na1 O3 144.94(11) . . ? O4 Na1 O7 152.62(10) . . ? O9 Na1 O7 100.90(10) . . ? O3 Na1 O7 99.94(9) . . ? O4 Na1 O8 88.20(9) . . ? O9 Na1 O8 65.93(10) . . ? O3 Na1 O8 96.96(10) . . ? O7 Na1 O8 67.69(8) . . ? O4 Na1 O10 94.74(10) . . ? O9 Na1 O10 64.66(10) . . ? O3 Na1 O10 131.57(10) . . ? O7 Na1 O10 110.30(10) . . ? O8 Na1 O10 128.97(10) . . ? O4 Na1 O6 134.02(9) . . ? O9 Na1 O6 136.13(10) . . ? O3 Na1 O6 78.74(8) . . ? O7 Na1 O6 62.97(7) . . ? O8 Na1 O6 128.66(8) . . ? O10 Na1 O6 82.42(8) . . ? S1 N1 S2 112.30(19) . . ? N1 S1 C12 105.5(2) . . ? N1 S1 C1 100.3(2) . . ? C12 S1 C1 97.5(2) . . ? C2 C1 S1 108.8(3) . . ? O1 C2 C1 106.4(4) . . ? C2 O1 C3 114.6(5) . . ? O1 C3 C4 108.1(5) . . ? O2 C4 C3 109.1(4) . . ? C5 O2 C4 112.3(4) . . ? O2 C5 C6 109.9(3) . . ? O3 C6 C5 113.3(3) . . ? C6 O3 C7 113.5(3) . . ? C6 O3 Na1 122.9(2) . . ? C7 O3 Na1 106.3(2) . . ? O3 C7 C8 107.7(3) . . ? O4 C8 C7 108.7(3) . . ? C8 O4 C9 114.2(3) . . ? C8 O4 Na1 115.4(2) . . ? C9 O4 Na1 128.5(2) . . ? O4 C9 C10 112.9(3) . . ? O5 C10 C9 109.3(4) . . ? C10 O5 C11 111.3(3) . . ? O5 C11 C12 106.2(4) . . ? C11 C12 S1 109.0(3) . . ? N1 S2 C24 97.5(2) . . ? N1 S2 C13 103.00(17) . . ? C24 S2 C13 102.17(18) . . ? C14 C13 S2 115.3(2) . . ? O6 C14 C13 109.2(3) . . ? C14 O6 C15 110.7(2) . . ? C14 O6 Na1 135.61(18) . . ? C15 O6 Na1 106.22(18) . . ? O6 C15 C16 109.0(3) . . ? O7 C16 C15 108.9(3) . . ? C16 O7 C17 111.2(2) . . ? C16 O7 Na1 123.26(19) . . ? C17 O7 Na1 114.92(19) . . ? O7 C17 C18 107.8(3) . . ? O8 C18 C17 107.5(3) . . ? C18 O8 C19 114.2(3) . . ? C18 O8 Na1 110.6(2) . . ? C19 O8 Na1 108.1(2) . . ? O8 C19 C20 112.7(3) . . ? O9 C20 C19 107.5(3) . . ? C21 O9 C20 114.5(3) . . ? C21 O9 Na1 123.3(2) . . ? C20 O9 Na1 122.0(3) . . ? O9 C21 C22 109.0(3) . . ? O10 C22 C21 111.4(4) . . ? C22 O10 C23 112.0(3) . . ? C22 O10 Na1 103.5(3) . . ? C23 O10 Na1 116.4(2) . . ? O10 C23 C24 109.3(3) . . ? C23 C24 S2 115.6(3) . . ? C37 B1 C31 108.5(2) . . ? C37 B1 C43 107.8(2) . . ? C31 B1 C43 111.8(3) . . ? C37 B1 C25 110.1(3) . . ? C31 B1 C25 109.0(2) . . ? C43 B1 C25 109.6(2) . . ? C30 C25 C26 114.4(3) . . ? C30 C25 B1 123.5(3) . . ? C26 C25 B1 122.1(3) . . ? C27 C26 C25 123.1(3) . . ? C28 C27 C26 120.8(3) . . ? C27 C28 C29 118.6(3) . . ? C28 C29 C30 120.0(3) . . ? C29 C30 C25 123.0(3) . . ? C36 C31 C32 114.2(3) . . ? C36 C31 B1 123.2(3) . . ? C32 C31 B1 122.6(3) . . ? C33 C32 C31 123.1(3) . . ? C34 C33 C32 120.4(3) . . ? C35 C34 C33 118.7(3) . . ? C34 C35 C36 120.2(3) . . ? C35 C36 C31 123.3(3) . . ? C38 C37 C42 115.1(3) . . ? C38 C37 B1 122.4(3) . . ? C42 C37 B1 122.4(3) . . ? C39 C38 C37 123.1(3) . . ? C40 C39 C38 120.0(3) . . ? C39 C40 C41 119.1(3) . . ? C40 C41 C42 120.3(3) . . ? C41 C42 C37 122.3(3) . . ? C48 C43 C44 114.7(3) . . ? C48 C43 B1 121.0(3) . . ? C44 C43 B1 124.2(3) . . ? C45 C44 C43 123.1(4) . . ? C46 C45 C44 119.7(4) . . ? C45 C46 C47 119.1(3) . . ? C48 C47 C46 119.8(4) . . ? C47 C48 C43 123.5(4) . . ? C55 B2 C49 108.8(2) . . ? C55 B2 C61 110.2(3) . . ? C49 B2 C61 110.8(2) . . ? C55 B2 C67 109.5(2) . . ? C49 B2 C67 109.1(3) . . ? C61 B2 C67 108.4(2) . . ? C50 C49 C54 114.6(3) . . ? C50 C49 B2 121.9(3) . . ? C54 C49 B2 123.6(3) . . ? C51 C50 C49 123.2(3) . . ? C50 C51 C52 119.9(3) . . ? C53 C52 C51 119.1(3) . . ? C52 C53 C54 120.0(3) . . ? C53 C54 C49 123.2(3) . . ? C56 C55 C60 115.1(3) . . ? C56 C55 B2 123.0(3) . . ? C60 C55 B2 121.7(3) . . ? C55 C56 C57 122.2(4) . . ? C58 C57 C56 120.6(4) . . ? C59 C58 C57 119.5(4) . . ? C58 C59 C60 119.8(4) . . ? C59 C60 C55 122.9(4) . . ? C66 C61 C62 114.6(3) . . ? C66 C61 B2 124.2(3) . . ? C62 C61 B2 121.1(3) . . ? C63 C62 C61 123.5(3) . . ? C64 C63 C62 120.2(3) . . ? C65 C64 C63 118.7(3) . . ? C64 C65 C66 120.5(3) . . ? C61 C66 C65 122.6(3) . . ? C68 C67 C72 114.7(3) . . ? C68 C67 B2 122.5(3) . . ? C72 C67 B2 122.8(3) . . ? C69 C68 C67 122.7(3) . . ? C70 C69 C68 120.5(3) . . ? C69 C70 C71 118.8(3) . . ? C70 C71 C72 120.0(3) . . ? C71 C72 C67 123.2(3) . . ? Cl2 C73 Cl1 109.9(3) . . ? Cl2 C73 Cl3 109.1(5) . . ? Cl1 C73 Cl3 111.6(3) . . ? Cl5 C74 Cl4 110.3(3) . . ? Cl5 C74 Cl6 111.2(3) . . ? Cl4 C74 Cl6 110.5(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S2 N1 S1 C12 -116.3(2) . . . . ? S2 N1 S1 C1 142.8(3) . . . . ? N1 S1 C1 C2 -64.5(5) . . . . ? C12 S1 C1 C2 -171.8(5) . . . . ? S1 C1 C2 O1 -53.9(5) . . . . ? C1 C2 O1 C3 173.7(4) . . . . ? C2 O1 C3 C4 -169.6(4) . . . . ? O1 C3 C4 O2 70.9(5) . . . . ? C3 C4 O2 C5 -175.6(4) . . . . ? C4 O2 C5 C6 179.5(4) . . . . ? O2 C5 C6 O3 -60.5(5) . . . . ? C5 C6 O3 C7 -76.6(5) . . . . ? C5 C6 O3 Na1 153.0(3) . . . . ? O4 Na1 O3 C6 164.2(3) . . . . ? O9 Na1 O3 C6 136.1(3) . . . . ? O7 Na1 O3 C6 10.3(3) . . . . ? O8 Na1 O3 C6 78.8(3) . . . . ? O10 Na1 O3 C6 -118.4(3) . . . . ? O6 Na1 O3 C6 -49.3(3) . . . . ? O4 Na1 O3 C7 30.9(2) . . . . ? O9 Na1 O3 C7 2.8(3) . . . . ? O7 Na1 O3 C7 -122.9(2) . . . . ? O8 Na1 O3 C7 -54.5(2) . . . . ? O10 Na1 O3 C7 108.3(2) . . . . ? O6 Na1 O3 C7 177.4(2) . . . . ? C6 O3 C7 C8 162.9(4) . . . . ? Na1 O3 C7 C8 -58.9(4) . . . . ? O3 C7 C8 O4 60.8(5) . . . . ? C7 C8 O4 C9 163.9(3) . . . . ? C7 C8 O4 Na1 -30.7(4) . . . . ? O9 Na1 O4 C8 164.4(3) . . . . ? O3 Na1 O4 C8 0.4(2) . . . . ? O7 Na1 O4 C8 71.0(3) . . . . ? O8 Na1 O4 C8 98.6(3) . . . . ? O10 Na1 O4 C8 -132.5(3) . . . . ? O6 Na1 O4 C8 -48.5(3) . . . . ? O9 Na1 O4 C9 -32.6(3) . . . . ? O3 Na1 O4 C9 163.4(3) . . . . ? O7 Na1 O4 C9 -126.0(3) . . . . ? O8 Na1 O4 C9 -98.5(3) . . . . ? O10 Na1 O4 C9 30.5(3) . . . . ? O6 Na1 O4 C9 114.5(3) . . . . ? C8 O4 C9 C10 92.5(4) . . . . ? Na1 O4 C9 C10 -70.7(4) . . . . ? O4 C9 C10 O5 -64.9(4) . . . . ? C9 C10 O5 C11 -175.4(3) . . . . ? C10 O5 C11 C12 -168.0(3) . . . . ? O5 C11 C12 S1 52.9(4) . . . . ? N1 S1 C12 C11 60.5(4) . . . . ? C1 S1 C12 C11 163.5(4) . . . . ? S1 N1 S2 C24 146.8(2) . . . . ? S1 N1 S2 C13 -108.8(2) . . . . ? N1 S2 C13 C14 -154.6(3) . . . . ? C24 S2 C13 C14 -53.9(3) . . . . ? S2 C13 C14 O6 -55.9(4) . . . . ? C13 C14 O6 C15 -177.1(3) . . . . ? C13 C14 O6 Na1 38.6(4) . . . . ? O4 Na1 O6 C14 -42.0(3) . . . . ? O9 Na1 O6 C14 87.7(3) . . . . ? O3 Na1 O6 C14 -87.9(3) . . . . ? O7 Na1 O6 C14 164.7(3) . . . . ? O8 Na1 O6 C14 -177.8(3) . . . . ? O10 Na1 O6 C14 47.3(3) . . . . ? O4 Na1 O6 C15 172.7(2) . . . . ? O9 Na1 O6 C15 -57.7(2) . . . . ? O3 Na1 O6 C15 126.8(2) . . . . ? O7 Na1 O6 C15 19.38(19) . . . . ? O8 Na1 O6 C15 36.8(2) . . . . ? O10 Na1 O6 C15 -98.1(2) . . . . ? C14 O6 C15 C16 157.5(3) . . . . ? Na1 O6 C15 C16 -47.7(3) . . . . ? O6 C15 C16 O7 61.9(4) . . . . ? C15 C16 O7 C17 172.4(3) . . . . ? C15 C16 O7 Na1 -45.0(4) . . . . ? O4 Na1 O7 C16 -121.5(3) . . . . ? O9 Na1 O7 C16 150.4(2) . . . . ? O3 Na1 O7 C16 -57.9(3) . . . . ? O8 Na1 O7 C16 -151.4(3) . . . . ? O10 Na1 O7 C16 83.6(3) . . . . ? O6 Na1 O7 C16 13.9(2) . . . . ? O4 Na1 O7 C17 20.0(4) . . . . ? O9 Na1 O7 C17 -68.2(2) . . . . ? O3 Na1 O7 C17 83.5(2) . . . . ? O8 Na1 O7 C17 -10.0(2) . . . . ? O10 Na1 O7 C17 -135.0(2) . . . . ? O6 Na1 O7 C17 155.3(2) . . . . ? C16 O7 C17 C18 -173.7(3) . . . . ? Na1 O7 C17 C18 40.3(4) . . . . ? O7 C17 C18 O8 -62.1(4) . . . . ? C17 C18 O8 C19 175.4(3) . . . . ? C17 C18 O8 Na1 53.1(3) . . . . ? O4 Na1 O8 C18 169.6(2) . . . . ? O9 Na1 O8 C18 90.4(2) . . . . ? O3 Na1 O8 C18 -121.6(2) . . . . ? O7 Na1 O8 C18 -23.7(2) . . . . ? O10 Na1 O8 C18 75.0(3) . . . . ? O6 Na1 O8 C18 -40.5(3) . . . . ? O4 Na1 O8 C19 43.8(3) . . . . ? O9 Na1 O8 C19 -35.4(3) . . . . ? O3 Na1 O8 C19 112.6(3) . . . . ? O7 Na1 O8 C19 -149.5(3) . . . . ? O10 Na1 O8 C19 -50.8(3) . . . . ? O6 Na1 O8 C19 -166.3(2) . . . . ? C18 O8 C19 C20 -68.2(4) . . . . ? Na1 O8 C19 C20 55.4(4) . . . . ? O8 C19 C20 O9 -42.0(5) . . . . ? C19 C20 O9 C21 -176.6(3) . . . . ? C19 C20 O9 Na1 7.2(4) . . . . ? O4 Na1 O9 C21 106.4(3) . . . . ? O3 Na1 O9 C21 133.1(3) . . . . ? O7 Na1 O9 C21 -101.5(3) . . . . ? O8 Na1 O9 C21 -160.8(3) . . . . ? O10 Na1 O9 C21 6.0(3) . . . . ? O6 Na1 O9 C21 -39.3(3) . . . . ? O4 Na1 O9 C20 -77.7(3) . . . . ? O3 Na1 O9 C20 -51.1(4) . . . . ? O7 Na1 O9 C20 74.4(3) . . . . ? O8 Na1 O9 C20 15.0(3) . . . . ? O10 Na1 O9 C20 -178.1(3) . . . . ? O6 Na1 O9 C20 136.5(3) . . . . ? C20 O9 C21 C22 -155.9(4) . . . . ? Na1 O9 C21 C22 20.2(5) . . . . ? O9 C21 C22 O10 -54.6(5) . . . . ? C21 C22 O10 C23 -177.0(4) . . . . ? C21 C22 O10 Na1 56.8(4) . . . . ? O4 Na1 O10 C22 -108.4(3) . . . . ? O9 Na1 O10 C22 -32.4(3) . . . . ? O3 Na1 O10 C22 -174.7(3) . . . . ? O7 Na1 O10 C22 60.3(3) . . . . ? O8 Na1 O10 C22 -16.9(3) . . . . ? O6 Na1 O10 C22 117.8(3) . . . . ? O4 Na1 O10 C23 128.3(3) . . . . ? O9 Na1 O10 C23 -155.7(3) . . . . ? O3 Na1 O10 C23 62.0(3) . . . . ? O7 Na1 O10 C23 -63.0(3) . . . . ? O8 Na1 O10 C23 -140.2(3) . . . . ? O6 Na1 O10 C23 -5.6(3) . . . . ? C22 O10 C23 C24 158.2(3) . . . . ? Na1 O10 C23 C24 -82.9(3) . . . . ? O10 C23 C24 S2 54.6(4) . . . . ? N1 S2 C24 C23 -165.7(3) . . . . ? C13 S2 C24 C23 89.2(3) . . . . ? C37 B1 C25 C30 -140.2(3) . . . . ? C31 B1 C25 C30 -21.3(4) . . . . ? C43 B1 C25 C30 101.4(3) . . . . ? C37 B1 C25 C26 39.4(4) . . . . ? C31 B1 C25 C26 158.3(3) . . . . ? C43 B1 C25 C26 -79.0(3) . . . . ? C30 C25 C26 C27 -0.7(5) . . . . ? B1 C25 C26 C27 179.7(3) . . . . ? C25 C26 C27 C28 0.9(6) . . . . ? C26 C27 C28 C29 -0.1(5) . . . . ? C27 C28 C29 C30 -0.7(5) . . . . ? C28 C29 C30 C25 0.9(5) . . . . ? C26 C25 C30 C29 -0.2(4) . . . . ? B1 C25 C30 C29 179.4(3) . . . . ? C37 B1 C31 C36 17.1(4) . . . . ? C43 B1 C31 C36 135.9(3) . . . . ? C25 B1 C31 C36 -102.8(3) . . . . ? C37 B1 C31 C32 -163.9(3) . . . . ? C43 B1 C31 C32 -45.1(4) . . . . ? C25 B1 C31 C32 76.3(3) . . . . ? C36 C31 C32 C33 -1.2(4) . . . . ? B1 C31 C32 C33 179.7(3) . . . . ? C31 C32 C33 C34 0.1(5) . . . . ? C32 C33 C34 C35 1.4(5) . . . . ? C33 C34 C35 C36 -1.5(5) . . . . ? C34 C35 C36 C31 0.3(5) . . . . ? C32 C31 C36 C35 1.0(4) . . . . ? B1 C31 C36 C35 -179.9(3) . . . . ? C31 B1 C37 C38 -79.2(4) . . . . ? C43 B1 C37 C38 159.5(3) . . . . ? C25 B1 C37 C38 40.0(4) . . . . ? C31 B1 C37 C42 96.5(3) . . . . ? C43 B1 C37 C42 -24.8(4) . . . . ? C25 B1 C37 C42 -144.3(3) . . . . ? C42 C37 C38 C39 -2.1(5) . . . . ? B1 C37 C38 C39 173.9(3) . . . . ? C37 C38 C39 C40 2.0(6) . . . . ? C38 C39 C40 C41 0.0(6) . . . . ? C39 C40 C41 C42 -1.7(6) . . . . ? C40 C41 C42 C37 1.5(6) . . . . ? C38 C37 C42 C41 0.3(5) . . . . ? B1 C37 C42 C41 -175.7(3) . . . . ? C37 B1 C43 C48 -71.2(3) . . . . ? C31 B1 C43 C48 169.6(3) . . . . ? C25 B1 C43 C48 48.6(4) . . . . ? C37 B1 C43 C44 104.4(3) . . . . ? C31 B1 C43 C44 -14.8(4) . . . . ? C25 B1 C43 C44 -135.8(3) . . . . ? C48 C43 C44 C45 -3.2(5) . . . . ? B1 C43 C44 C45 -179.0(3) . . . . ? C43 C44 C45 C46 1.4(5) . . . . ? C44 C45 C46 C47 1.9(6) . . . . ? C45 C46 C47 C48 -2.9(6) . . . . ? C46 C47 C48 C43 0.9(5) . . . . ? C44 C43 C48 C47 2.1(5) . . . . ? B1 C43 C48 C47 178.0(3) . . . . ? C55 B2 C49 C50 168.1(3) . . . . ? C61 B2 C49 C50 -70.6(4) . . . . ? C67 B2 C49 C50 48.7(4) . . . . ? C55 B2 C49 C54 -12.2(4) . . . . ? C61 B2 C49 C54 109.1(3) . . . . ? C67 B2 C49 C54 -131.7(3) . . . . ? C54 C49 C50 C51 -1.6(5) . . . . ? B2 C49 C50 C51 178.1(3) . . . . ? C49 C50 C51 C52 0.2(5) . . . . ? C50 C51 C52 C53 0.4(5) . . . . ? C51 C52 C53 C54 0.4(5) . . . . ? C52 C53 C54 C49 -2.0(5) . . . . ? C50 C49 C54 C53 2.5(5) . . . . ? B2 C49 C54 C53 -177.2(3) . . . . ? C49 B2 C55 C56 -92.5(4) . . . . ? C61 B2 C55 C56 145.9(3) . . . . ? C67 B2 C55 C56 26.7(4) . . . . ? C49 B2 C55 C60 82.2(4) . . . . ? C61 B2 C55 C60 -39.5(4) . . . . ? C67 B2 C55 C60 -158.6(3) . . . . ? C60 C55 C56 C57 -1.4(5) . . . . ? B2 C55 C56 C57 173.6(3) . . . . ? C55 C56 C57 C58 0.6(6) . . . . ? C56 C57 C58 C59 -0.2(7) . . . . ? C57 C58 C59 C60 0.6(6) . . . . ? C58 C59 C60 C55 -1.5(6) . . . . ? C56 C55 C60 C59 1.8(5) . . . . ? B2 C55 C60 C59 -173.2(3) . . . . ? C55 B2 C61 C66 147.3(3) . . . . ? C49 B2 C61 C66 26.8(4) . . . . ? C67 B2 C61 C66 -92.9(3) . . . . ? C55 B2 C61 C62 -35.9(4) . . . . ? C49 B2 C61 C62 -156.4(3) . . . . ? C67 B2 C61 C62 83.9(3) . . . . ? C66 C61 C62 C63 0.9(5) . . . . ? B2 C61 C62 C63 -176.2(3) . . . . ? C61 C62 C63 C64 0.2(5) . . . . ? C62 C63 C64 C65 -0.7(5) . . . . ? C63 C64 C65 C66 0.3(5) . . . . ? C62 C61 C66 C65 -1.4(4) . . . . ? B2 C61 C66 C65 175.6(3) . . . . ? C64 C65 C66 C61 0.9(5) . . . . ? C55 B2 C67 C68 87.0(3) . . . . ? C49 B2 C67 C68 -153.9(3) . . . . ? C61 B2 C67 C68 -33.2(4) . . . . ? C55 B2 C67 C72 -90.7(3) . . . . ? C49 B2 C67 C72 28.3(4) . . . . ? C61 B2 C67 C72 149.0(3) . . . . ? C72 C67 C68 C69 0.4(5) . . . . ? B2 C67 C68 C69 -177.5(3) . . . . ? C67 C68 C69 C70 -1.6(5) . . . . ? C68 C69 C70 C71 1.5(5) . . . . ? C69 C70 C71 C72 -0.1(5) . . . . ? C70 C71 C72 C67 -1.2(5) . . . . ? C68 C67 C72 C71 1.0(5) . . . . ? B2 C67 C72 C71 178.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.863 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.921 _refine_diff_density_min -1.045 _refine_diff_density_rms 0.079 #===END