data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Magdalena, Capo' 'Alvarez, Angel' 'Saa, Jose M.' _publ_contact_author_name 'Dr Capo Magdalena' _publ_contact_author_address ; Chemistry U.I.B. Cra. Valldemossa Km 7.5 07071 Palma Palma de Mallorca SPAIN ; _publ_contact_author_email 'DQUMCC3@CLUST.UIB.ES' _publ_section_title ; Self-assembly of a stereoselective trinuclear sodium/lithium triple helix. ; data_magda _database_code_CSD 183483 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C93 H108 F9 N6 Na3 O21 S3' _chemical_formula_weight 1982.00 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' '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' 'F' 'F' 0.0171 0.0103 '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 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 34.5427(11) _cell_length_b 23.4946(7) _cell_length_c 27.6861(9) _cell_angle_alpha 90.00 _cell_angle_beta 96.9080(10) _cell_angle_gamma 90.00 _cell_volume 22306.0(12) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.180 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8304 _exptl_absorpt_coefficient_mu 0.156 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.5988 _exptl_absorpt_correction_T_max 0.9108 _exptl_absorpt_process_details 'Sadabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omrga scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 112976 _diffrn_reflns_av_R_equivalents 0.0936 _diffrn_reflns_av_sigmaI/netI 0.1410 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 38987 _reflns_number_gt 15007 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'SHELXS-97 (sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 38987 _refine_ls_number_parameters 1916 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.3341 _refine_ls_R_factor_gt 0.1996 _refine_ls_wR_factor_ref 0.5419 _refine_ls_wR_factor_gt 0.4745 _refine_ls_goodness_of_fit_ref 1.544 _refine_ls_restrained_S_all 1.544 _refine_ls_shift/su_max 0.182 _refine_ls_shift/su_mean 0.015 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 C110 C 0.44388(14) 0.54283(19) 0.60550(18) 0.055(3) Uani 1 1 d G . . C111 C 0.41528(17) 0.50110(16) 0.59777(19) 0.046(2) Uani 1 1 d G . . C112 C 0.38129(15) 0.51174(19) 0.5668(2) 0.052(3) Uani 1 1 d G . . C113 C 0.37590(13) 0.5641(2) 0.54365(19) 0.064(3) Uani 1 1 d G . . H113 H 0.3532 0.5712 0.5230 0.077 Uiso 1 1 calc R . . C114 C 0.40449(13) 0.60584(16) 0.55138(15) 0.058(3) Uani 1 1 d G . . C115 C 0.43848(12) 0.59520(16) 0.58230(14) 0.056(3) Uani 1 1 d G . . C116 C 0.46708(15) 0.6369(2) 0.5900(2) 0.063(3) Uani 1 1 d G . . H116 H 0.4898 0.6298 0.6107 0.075 Uiso 1 1 calc R . . C117 C 0.4617(2) 0.6893(2) 0.5668(3) 0.083(4) Uani 1 1 d G . . H117 H 0.4808 0.7172 0.5720 0.100 Uiso 1 1 calc R . . C118 C 0.4277(2) 0.69994(17) 0.5359(2) 0.091(4) Uani 1 1 d G . . H118 H 0.4241 0.7350 0.5204 0.110 Uiso 1 1 calc R . . C119 C 0.39910(19) 0.6582(2) 0.5282(2) 0.084(4) Uani 1 1 d G . . H119 H 0.3764 0.6653 0.5075 0.101 Uiso 1 1 calc R . . O130 O 0.41925(19) 0.4492(3) 0.6216(2) 0.0530(17) Uani 1 1 d . . . C131 C 0.3467(3) 0.4716(4) 0.5658(4) 0.056(3) Uani 1 1 d . . . H13A H 0.3424 0.4633 0.5991 0.067 Uiso 1 1 calc R . . H13B H 0.3237 0.4911 0.5504 0.067 Uiso 1 1 calc R . . N132 N 0.3506(3) 0.4160(4) 0.5397(3) 0.065(2) Uani 1 1 d . . . O133 O 0.3816(2) 0.3843(3) 0.5639(3) 0.070(2) Uani 1 1 d . . . C134 C 0.3589(4) 0.4267(5) 0.4895(4) 0.082(4) Uani 1 1 d . . . H13C H 0.3821 0.4503 0.4910 0.098 Uiso 1 1 calc R . . H13D H 0.3375 0.4485 0.4729 0.098 Uiso 1 1 calc R . . C135 C 0.3651(5) 0.3751(7) 0.4593(5) 0.123(6) Uani 1 1 d . . . H13E H 0.3699 0.3868 0.4274 0.185 Uiso 1 1 calc R . . H13F H 0.3423 0.3515 0.4569 0.185 Uiso 1 1 calc R . . H13G H 0.3871 0.3540 0.4744 0.185 Uiso 1 1 calc R . . C136 C 0.3145(4) 0.3802(6) 0.5421(5) 0.096(4) Uani 1 1 d . . . H13H H 0.3195 0.3425 0.5300 0.116 Uiso 1 1 calc R . . H13I H 0.3106 0.3760 0.5761 0.116 Uiso 1 1 calc R . . C137 C 0.2779(5) 0.4008(8) 0.5156(8) 0.160(8) Uani 1 1 d . . . H13J H 0.2574 0.3743 0.5194 0.240 Uiso 1 1 calc R . . H13K H 0.2809 0.4046 0.4817 0.240 Uiso 1 1 calc R . . H13L H 0.2716 0.4372 0.5283 0.240 Uiso 1 1 calc R . . C120 C 0.48277(11) 0.5264(2) 0.63792(17) 0.045(2) Uani 1 1 d G . . C121 C 0.48171(14) 0.5254(2) 0.68794(18) 0.047(2) Uani 1 1 d G . . C122 C 0.51531(16) 0.5129(2) 0.71901(13) 0.049(3) Uani 1 1 d G . . C123 C 0.54996(14) 0.5014(2) 0.70005(14) 0.052(3) Uani 1 1 d G . . H123 H 0.5724 0.4931 0.7208 0.062 Uiso 1 1 calc R . . C124 C 0.55102(11) 0.50246(16) 0.65002(15) 0.053(3) Uani 1 1 d G . . C125 C 0.51743(12) 0.51495(16) 0.61896(13) 0.051(3) Uani 1 1 d G . . C126 C 0.51848(17) 0.5160(3) 0.56894(13) 0.068(3) Uani 1 1 d G . . H126 H 0.4960 0.5243 0.5482 0.081 Uiso 1 1 calc R . . C127 C 0.5531(2) 0.5045(3) 0.54998(16) 0.097(4) Uani 1 1 d G . . H127 H 0.5538 0.5052 0.5165 0.117 Uiso 1 1 calc R . . C128 C 0.58673(17) 0.4920(3) 0.5810(2) 0.093(4) Uani 1 1 d G . . H128 H 0.6099 0.4843 0.5684 0.111 Uiso 1 1 calc R . . C129 C 0.58567(12) 0.4910(3) 0.6311(2) 0.076(3) Uani 1 1 d G . . H129 H 0.6081 0.4826 0.6518 0.091 Uiso 1 1 calc R . . O140 O 0.44727(19) 0.5294(3) 0.7075(2) 0.0530(17) Uani 1 1 d . . . C141 C 0.5144(3) 0.4976(4) 0.7720(4) 0.060(3) Uani 1 1 d . . . H14A H 0.4951 0.4680 0.7738 0.072 Uiso 1 1 calc R . . H14B H 0.5396 0.4817 0.7844 0.072 Uiso 1 1 calc R . . N142 N 0.5056(3) 0.5451(4) 0.8049(3) 0.063(2) Uani 1 1 d . . . O143 O 0.4673(2) 0.5665(3) 0.7904(2) 0.0609(19) Uani 1 1 d . . . C144 C 0.5058(4) 0.5252(6) 0.8572(4) 0.098(4) Uani 1 1 d . . . H14C H 0.4981 0.5568 0.8764 0.117 Uiso 1 1 calc R . . H14D H 0.4863 0.4956 0.8579 0.117 Uiso 1 1 calc R . . C145 C 0.5437(5) 0.5029(8) 0.8806(6) 0.141(6) Uani 1 1 d . . . H14E H 0.5410 0.4910 0.9132 0.211 Uiso 1 1 calc R . . H14F H 0.5631 0.5323 0.8813 0.211 Uiso 1 1 calc R . . H14G H 0.5515 0.4710 0.8623 0.211 Uiso 1 1 calc R . . C146 C 0.5344(4) 0.5933(5) 0.8013(5) 0.095(4) Uani 1 1 d . . . H14H H 0.5605 0.5788 0.8107 0.114 Uiso 1 1 calc R . . H14I H 0.5329 0.6051 0.7675 0.114 Uiso 1 1 calc R . . C147 C 0.5288(5) 0.6436(6) 0.8310(6) 0.125(6) Uani 1 1 d . . . H14J H 0.5478 0.6720 0.8255 0.188 Uiso 1 1 calc R . . H14K H 0.5319 0.6332 0.8648 0.188 Uiso 1 1 calc R . . H14L H 0.5031 0.6586 0.8221 0.188 Uiso 1 1 calc R . . C210 C 0.47978(12) 0.3423(2) 0.77545(19) 0.051(3) Uani 1 1 d G . . C211 C 0.47489(14) 0.3505(2) 0.72536(19) 0.050(2) Uani 1 1 d G . . C212 C 0.50719(18) 0.3594(2) 0.70083(16) 0.054(3) Uani 1 1 d G . . C213 C 0.54438(16) 0.3601(2) 0.72639(19) 0.068(3) Uani 1 1 d G . . H213 H 0.5660 0.3661 0.7100 0.081 Uiso 1 1 calc R . . C214 C 0.54926(12) 0.35198(17) 0.77648(19) 0.064(3) Uani 1 1 d G . . C215 C 0.51697(13) 0.34307(16) 0.80101(16) 0.058(3) Uani 1 1 d G . . C216 C 0.52185(19) 0.3349(2) 0.85110(16) 0.069(3) Uani 1 1 d G . . H216 H 0.5002 0.3290 0.8675 0.083 Uiso 1 1 calc R . . C217 C 0.5590(2) 0.3357(3) 0.87666(19) 0.084(4) Uani 1 1 d G . . H217 H 0.5623 0.3302 0.9102 0.100 Uiso 1 1 calc R . . C218 C 0.59133(17) 0.3446(3) 0.8521(3) 0.105(5) Uani 1 1 d G . . H218 H 0.6162 0.3451 0.8692 0.126 Uiso 1 1 calc R . . C219 C 0.58645(12) 0.3527(3) 0.8020(3) 0.082(4) Uani 1 1 d G . . H219 H 0.6081 0.3587 0.7856 0.098 Uiso 1 1 calc R . . O230 O 0.4386(2) 0.3534(3) 0.7000(2) 0.0613(19) Uani 1 1 d . . . C231 C 0.5027(3) 0.3765(5) 0.6467(4) 0.069(3) Uani 1 1 d . . . H23A H 0.4845 0.4081 0.6420 0.083 Uiso 1 1 calc R . . H23B H 0.5277 0.3898 0.6387 0.083 Uiso 1 1 calc R . . N232 N 0.4885(3) 0.3296(4) 0.6118(3) 0.073(3) Uani 1 1 d . . . O233 O 0.4521(3) 0.3123(3) 0.6217(3) 0.082(2) Uani 1 1 d . . . C234 C 0.5157(4) 0.2780(6) 0.6182(5) 0.091(4) Uani 1 1 d . . . H23C H 0.5174 0.2653 0.6517 0.109 Uiso 1 1 calc R . . H23D H 0.5042 0.2473 0.5978 0.109 Uiso 1 1 calc R . . C235 C 0.5547(5) 0.2884(7) 0.6062(7) 0.137(6) Uani 1 1 d . . . H23E H 0.5699 0.2543 0.6114 0.205 Uiso 1 1 calc R . . H23F H 0.5666 0.3183 0.6265 0.205 Uiso 1 1 calc R . . H23G H 0.5534 0.2996 0.5727 0.205 Uiso 1 1 calc R . . C236 C 0.4831(5) 0.3554(8) 0.5602(5) 0.116(5) Uani 1 1 d . . . H23H H 0.4645 0.3863 0.5597 0.140 Uiso 1 1 calc R . . H23I H 0.5078 0.3717 0.5538 0.140 Uiso 1 1 calc R . . C237 C 0.4696(6) 0.3152(9) 0.5198(7) 0.155(7) Uani 1 1 d . . . H23J H 0.4679 0.3349 0.4893 0.232 Uiso 1 1 calc R . . H23K H 0.4444 0.3004 0.5244 0.232 Uiso 1 1 calc R . . H23L H 0.4878 0.2843 0.5197 0.232 Uiso 1 1 calc R . . C220 C 0.44281(14) 0.33035(19) 0.79930(18) 0.047(2) Uani 1 1 d G . . C221 C 0.41969(16) 0.37660(16) 0.80848(19) 0.047(2) Uani 1 1 d G . . C222 C 0.38898(15) 0.36949(18) 0.8361(2) 0.051(3) Uani 1 1 d G . . C223 C 0.38138(14) 0.3161(2) 0.85449(19) 0.059(3) Uani 1 1 d G . . H223 H 0.3608 0.3114 0.8729 0.071 Uiso 1 1 calc R . . C224 C 0.40450(12) 0.26989(17) 0.84531(14) 0.057(3) Uani 1 1 d G . . C225 C 0.43522(11) 0.27699(16) 0.81771(13) 0.052(3) Uani 1 1 d G . . C226 C 0.45834(15) 0.2307(2) 0.8085(2) 0.058(3) Uani 1 1 d G . . H226 H 0.4789 0.2355 0.7901 0.070 Uiso 1 1 calc R . . C227 C 0.45075(19) 0.17739(18) 0.8269(2) 0.070(3) Uani 1 1 d G . . H227 H 0.4662 0.1464 0.8208 0.084 Uiso 1 1 calc R . . C228 C 0.4200(2) 0.17029(16) 0.8545(2) 0.077(4) Uani 1 1 d G . . H228 H 0.4150 0.1346 0.8669 0.093 Uiso 1 1 calc R . . C229 C 0.39691(17) 0.21654(19) 0.8637(2) 0.073(3) Uani 1 1 d G . . H229 H 0.3764 0.2118 0.8822 0.087 Uiso 1 1 calc R . . O240 O 0.4256(2) 0.4298(3) 0.7896(2) 0.0582(18) Uani 1 1 d . . . C241 C 0.3590(3) 0.4170(4) 0.8413(4) 0.067(3) Uani 1 1 d . . . H24A H 0.3485 0.4299 0.8091 0.080 Uiso 1 1 calc R . . H24B H 0.3376 0.4012 0.8566 0.080 Uiso 1 1 calc R . . N242 N 0.3753(3) 0.4681(4) 0.8708(4) 0.075(3) Uani 1 1 d . . . O243 O 0.3997(2) 0.4981(3) 0.8434(3) 0.071(2) Uani 1 1 d . . . C244 C 0.3434(4) 0.5067(6) 0.8830(6) 0.102(5) Uani 1 1 d . . . H24C H 0.3281 0.4868 0.9049 0.122 Uiso 1 1 calc R . . H24D H 0.3551 0.5396 0.9002 0.122 Uiso 1 1 calc R . . C245 C 0.3185(5) 0.5255(7) 0.8427(7) 0.137(6) Uani 1 1 d . . . H24E H 0.2994 0.5509 0.8533 0.205 Uiso 1 1 calc R . . H24F H 0.3055 0.4934 0.8264 0.205 Uiso 1 1 calc R . . H24G H 0.3333 0.5451 0.8207 0.205 Uiso 1 1 calc R . . C246 C 0.4002(5) 0.4500(6) 0.9178(5) 0.115(6) Uani 1 1 d . . . H24H H 0.4222 0.4291 0.9078 0.138 Uiso 1 1 calc R . . H24I H 0.4108 0.4848 0.9329 0.138 Uiso 1 1 calc R . . C247 C 0.3867(10) 0.4173(10) 0.9559(8) 0.247(16) Uani 1 1 d . . . H24J H 0.4079 0.4108 0.9811 0.370 Uiso 1 1 calc R . . H24K H 0.3769 0.3814 0.9432 0.370 Uiso 1 1 calc R . . H24L H 0.3663 0.4376 0.9691 0.370 Uiso 1 1 calc R . . C310 C 0.29311(15) 0.4387(2) 0.70935(18) 0.052(3) Uani 1 1 d G . . C311 C 0.31869(14) 0.3940(2) 0.70464(19) 0.048(3) Uani 1 1 d G . . C312 C 0.31688(14) 0.3451(2) 0.7327(2) 0.053(3) Uani 1 1 d G . . C313 C 0.28947(16) 0.34111(17) 0.7654(2) 0.055(3) Uani 1 1 d G . . H313 H 0.2883 0.3085 0.7841 0.066 Uiso 1 1 calc R . . C314 C 0.26389(13) 0.38588(18) 0.77009(15) 0.059(3) Uani 1 1 d G . . C315 C 0.26571(12) 0.43468(16) 0.74208(15) 0.054(3) Uani 1 1 d G . . C316 C 0.24012(16) 0.4795(2) 0.7468(2) 0.075(3) Uani 1 1 d G . . H316 H 0.2413 0.5121 0.7280 0.090 Uiso 1 1 calc R . . C317 C 0.21272(16) 0.4754(3) 0.7795(3) 0.087(4) Uani 1 1 d G . . H317 H 0.1956 0.5054 0.7827 0.105 Uiso 1 1 calc R . . C318 C 0.21090(16) 0.4266(3) 0.8075(2) 0.098(4) Uani 1 1 d G . . H318 H 0.1926 0.4239 0.8294 0.117 Uiso 1 1 calc R . . C319 C 0.23649(17) 0.3818(3) 0.8028(2) 0.076(3) Uani 1 1 d G . . H319 H 0.2353 0.3492 0.8216 0.091 Uiso 1 1 calc R . . O330 O 0.34694(19) 0.3977(3) 0.6734(2) 0.0533(17) Uani 1 1 d . . . C331 C 0.3467(3) 0.2966(4) 0.7309(4) 0.056(3) Uani 1 1 d . . . H33A H 0.3441 0.2705 0.7576 0.067 Uiso 1 1 calc R . . H33B H 0.3727 0.3125 0.7360 0.067 Uiso 1 1 calc R . . N332 N 0.3419(3) 0.2625(3) 0.6824(3) 0.059(2) Uani 1 1 d . . . O333 O 0.3524(2) 0.2972(3) 0.6459(2) 0.065(2) Uani 1 1 d . . . C334 C 0.3721(4) 0.2138(4) 0.6889(4) 0.075(4) Uani 1 1 d . . . H33C H 0.3727 0.1957 0.6575 0.090 Uiso 1 1 calc R . . H33D H 0.3976 0.2306 0.6980 0.090 Uiso 1 1 calc R . . C335 C 0.3666(5) 0.1700(5) 0.7238(5) 0.112(5) Uani 1 1 d . . . H33E H 0.3869 0.1420 0.7238 0.168 Uiso 1 1 calc R . . H33F H 0.3417 0.1521 0.7152 0.168 Uiso 1 1 calc R . . H33G H 0.3675 0.1865 0.7556 0.168 Uiso 1 1 calc R . . C336 C 0.3009(3) 0.2436(5) 0.6695(4) 0.073(3) Uani 1 1 d . . . H33H H 0.2938 0.2189 0.6951 0.087 Uiso 1 1 calc R . . H33I H 0.2840 0.2766 0.6681 0.087 Uiso 1 1 calc R . . C337 C 0.2942(5) 0.2132(6) 0.6229(5) 0.102(5) Uani 1 1 d . . . H33J H 0.2672 0.2026 0.6167 0.154 Uiso 1 1 calc R . . H33K H 0.3101 0.1796 0.6244 0.154 Uiso 1 1 calc R . . H33L H 0.3008 0.2375 0.5973 0.154 Uiso 1 1 calc R . . C320 C 0.29662(16) 0.4904(2) 0.67666(18) 0.053(3) Uani 1 1 d G . . C321 C 0.32782(15) 0.5270(2) 0.68940(19) 0.051(3) Uani 1 1 d G . . C322 C 0.33112(16) 0.5769(2) 0.6633(2) 0.059(3) Uani 1 1 d G . . C323 C 0.30324(18) 0.59036(19) 0.6245(2) 0.076(3) Uani 1 1 d G . . H323 H 0.3055 0.6238 0.6071 0.091 Uiso 1 1 calc R . . C324 C 0.27204(14) 0.55380(18) 0.61180(16) 0.070(3) Uani 1 1 d G . . C325 C 0.26873(13) 0.50382(17) 0.63786(16) 0.058(3) Uani 1 1 d G . . C326 C 0.23754(16) 0.4673(2) 0.6251(2) 0.083(4) Uani 1 1 d G . . H326 H 0.2353 0.4338 0.6426 0.100 Uiso 1 1 calc R . . C327 C 0.20965(16) 0.4807(3) 0.5863(3) 0.100(5) Uani 1 1 d G . . H327 H 0.1888 0.4562 0.5778 0.120 Uiso 1 1 calc R . . C328 C 0.21296(18) 0.5306(3) 0.5603(2) 0.102(5) Uani 1 1 d G . . H328 H 0.1943 0.5396 0.5343 0.122 Uiso 1 1 calc R . . C329 C 0.24415(19) 0.5672(3) 0.5730(2) 0.083(4) Uani 1 1 d G . . H329 H 0.2464 0.6006 0.5556 0.100 Uiso 1 1 calc R . . O340 O 0.3570(2) 0.5126(3) 0.7242(2) 0.0575(18) Uani 1 1 d . . . C341 C 0.3686(4) 0.6138(5) 0.6691(4) 0.077(4) Uani 1 1 d . . . H34A H 0.3909 0.5896 0.6661 0.093 Uiso 1 1 calc R . . H34B H 0.3670 0.6416 0.6430 0.093 Uiso 1 1 calc R . . N342 N 0.3751(3) 0.6451(4) 0.7180(4) 0.079(3) Uani 1 1 d . . . O343 O 0.3838(3) 0.6039(3) 0.7561(3) 0.080(2) Uani 1 1 d . . . C344 C 0.4128(6) 0.6796(7) 0.7150(6) 0.137(8) Uani 1 1 d . . . H34C H 0.4322 0.6544 0.7039 0.164 Uiso 1 1 calc R . . H34D H 0.4073 0.7090 0.6905 0.164 Uiso 1 1 calc R . . C345 C 0.4278(9) 0.7033(9) 0.7544(16) 0.34(3) Uani 1 1 d . . . H34E H 0.4507 0.7241 0.7485 0.505 Uiso 1 1 calc R . . H34F H 0.4347 0.6747 0.7786 0.505 Uiso 1 1 calc R . . H34G H 0.4092 0.7290 0.7656 0.505 Uiso 1 1 calc R . . C346 C 0.3397(5) 0.6780(6) 0.7280(6) 0.129(6) Uani 1 1 d . . . H34H H 0.3442 0.6950 0.7601 0.155 Uiso 1 1 calc R . . H34I H 0.3175 0.6525 0.7274 0.155 Uiso 1 1 calc R . . C347 C 0.3308(7) 0.7242(7) 0.6902(8) 0.208(13) Uani 1 1 d . . . H34J H 0.3082 0.7451 0.6970 0.312 Uiso 1 1 calc R . . H34K H 0.3258 0.7072 0.6585 0.312 Uiso 1 1 calc R . . H34L H 0.3527 0.7495 0.6910 0.312 Uiso 1 1 calc R . . Na1 Na 0.39153(17) 0.2897(2) 0.58365(19) 0.0971(16) Uani 1 1 d . . . Na2 Na 0.40551(9) 0.44589(13) 0.70393(11) 0.0363(8) Uani 1 1 d . . . Na3 Na 0.41586(16) 0.59352(19) 0.83576(18) 0.0875(15) Uani 1 1 d . . . S30 S 0.4506(2) 0.6261(3) 0.9592(3) 0.239(4) Uiso 1 1 d G . . O33 O 0.4241(4) 0.5849(7) 0.9726(5) 0.50(2) Uiso 1 1 d G . . O32 O 0.4394(5) 0.6804(5) 0.9742(4) 0.279(10) Uiso 1 1 d G . . O31 O 0.4505(3) 0.6255(5) 0.9083(3) 0.183(5) Uiso 1 1 d G . . C30 C 0.5006(3) 0.6092(7) 0.9893(4) 0.73(7) Uiso 1 1 d G . . F31 F 0.5006(4) 0.6097(7) 1.0395(4) 0.266(7) Uiso 1 1 d G . . F32 F 0.5078(6) 0.5621(8) 0.9782(4) 0.337(11) Uiso 1 1 d G . . F33 F 0.5203(7) 0.6570(8) 0.9760(5) 0.472(18) Uiso 1 1 d G . . O301 O 0.3696(5) 0.6603(7) 0.8656(6) 0.219(7) Uiso 1 1 d . . . O2 O 0.3726(7) 0.2265(10) 0.5276(8) 0.280(9) Uiso 1 1 d . . . O5 O 0.3934(7) 0.3621(9) 0.6301(8) 0.264(9) Uiso 1 1 d . . . C410 C 0.05198(16) 0.00239(19) 0.62811(19) 0.054(3) Uani 1 1 d G . . C411 C 0.07425(18) 0.04868(16) 0.6167(2) 0.047(2) Uani 1 1 d G . . C412 C 0.10376(17) 0.0413(2) 0.5873(2) 0.059(3) Uani 1 1 d G . . C413 C 0.11100(15) -0.0124(2) 0.5693(2) 0.065(3) Uani 1 1 d G . . H413 H 0.1307 -0.0173 0.5496 0.079 Uiso 1 1 calc R . . C414 C 0.08873(14) -0.05866(18) 0.58066(15) 0.060(3) Uani 1 1 d G . . C415 C 0.05922(13) -0.05128(17) 0.61007(15) 0.056(3) Uani 1 1 d G . . C416 C 0.03695(17) -0.0976(2) 0.6214(2) 0.075(3) Uani 1 1 d G . . H416 H 0.0172 -0.0926 0.6411 0.090 Uiso 1 1 calc R . . C417 C 0.0442(2) -0.15124(18) 0.6034(3) 0.096(4) Uani 1 1 d G . . H417 H 0.0293 -0.1822 0.6110 0.115 Uiso 1 1 calc R . . C418 C 0.0737(2) -0.15863(17) 0.5740(3) 0.097(5) Uani 1 1 d G . . H418 H 0.0785 -0.1945 0.5619 0.116 Uiso 1 1 calc R . . C419 C 0.0960(2) -0.1123(2) 0.5626(2) 0.080(4) Uani 1 1 d G . . H419 H 0.1157 -0.1173 0.5429 0.096 Uiso 1 1 calc R . . O430 O 0.06892(19) 0.0999(3) 0.6374(2) 0.0553(18) Uani 1 1 d . . . C431 C 0.1307(3) 0.0901(4) 0.5781(4) 0.062(3) Uani 1 1 d . . . H43A H 0.1515 0.0752 0.5611 0.075 Uiso 1 1 calc R . . H43B H 0.1425 0.1044 0.6093 0.075 Uiso 1 1 calc R . . N432 N 0.1116(3) 0.1401(4) 0.5487(3) 0.066(3) Uani 1 1 d . . . O433 O 0.0878(2) 0.1689(3) 0.5774(3) 0.067(2) Uani 1 1 d . . . C434 C 0.0863(4) 0.1185(6) 0.5041(4) 0.086(4) Uani 1 1 d . . . H43C H 0.1024 0.0972 0.4841 0.103 Uiso 1 1 calc R . . H43D H 0.0669 0.0927 0.5142 0.103 Uiso 1 1 calc R . . C435 C 0.0662(5) 0.1654(8) 0.4744(5) 0.135(7) Uani 1 1 d . . . H43E H 0.0505 0.1495 0.4467 0.202 Uiso 1 1 calc R . . H43F H 0.0853 0.1906 0.4635 0.202 Uiso 1 1 calc R . . H43G H 0.0498 0.1863 0.4938 0.202 Uiso 1 1 calc R . . C436 C 0.1410(6) 0.1785(7) 0.5333(7) 0.130(6) Uani 1 1 d D . . H43H H 0.1269 0.2140 0.5271 0.156 Uiso 1 1 calc R . . H43I H 0.1451 0.1641 0.5014 0.156 Uiso 1 1 calc R . . C437 C 0.1812(6) 0.1977(12) 0.5543(14) 0.34(2) Uani 1 1 d D . . H43J H 0.1913 0.2238 0.5323 0.512 Uiso 1 1 calc R . . H43K H 0.1981 0.1653 0.5592 0.512 Uiso 1 1 calc R . . H43L H 0.1797 0.2163 0.5849 0.512 Uiso 1 1 calc R . . C420 C 0.01666(13) 0.0149(2) 0.6555(2) 0.056(3) Uani 1 1 d G . . C421 C 0.02205(15) 0.0183(2) 0.7060(2) 0.052(3) Uani 1 1 d G . . C422 C -0.00963(19) 0.0283(2) 0.73138(16) 0.053(3) Uani 1 1 d G . . C423 C -0.04670(16) 0.0349(2) 0.7063(2) 0.063(3) Uani 1 1 d G . . H423 H -0.0679 0.0416 0.7233 0.075 Uiso 1 1 calc R . . C424 C -0.05209(12) 0.03143(17) 0.6558(2) 0.071(3) Uani 1 1 d G . . C425 C -0.02041(14) 0.02142(16) 0.63042(16) 0.060(3) Uani 1 1 d G . . C426 C -0.0258(2) 0.0180(3) 0.57993(16) 0.074(3) Uani 1 1 d G . . H426 H -0.0046 0.0113 0.5629 0.089 Uiso 1 1 calc R . . C427 C -0.0629(3) 0.0245(3) 0.5548(2) 0.114(5) Uani 1 1 d G . . H427 H -0.0665 0.0222 0.5211 0.137 Uiso 1 1 calc R . . C428 C -0.0946(2) 0.0345(3) 0.5802(3) 0.122(6) Uani 1 1 d G . . H428 H -0.1194 0.0389 0.5634 0.147 Uiso 1 1 calc R . . C429 C -0.08916(13) 0.0380(3) 0.6307(3) 0.092(4) Uani 1 1 d G . . H429 H -0.1104 0.0447 0.6477 0.110 Uiso 1 1 calc R . . O440 O 0.05900(18) 0.0181(2) 0.7307(2) 0.0510(17) Uani 1 1 d . . . C441 C -0.0032(3) 0.0449(4) 0.7856(4) 0.066(3) Uani 1 1 d . . . H44A H -0.0276 0.0587 0.7951 0.079 Uiso 1 1 calc R . . H44B H 0.0154 0.0760 0.7897 0.079 Uiso 1 1 calc R . . N442 N 0.0120(3) -0.0044(4) 0.8202(3) 0.068(3) Uani 1 1 d . . . O443 O 0.0500(2) -0.0178(3) 0.8113(3) 0.068(2) Uani 1 1 d . . . C444 C -0.0138(4) -0.0566(5) 0.8101(6) 0.112(6) Uani 1 1 d . . . H44C H -0.0394 -0.0483 0.8194 0.134 Uiso 1 1 calc R . . H44D H -0.0169 -0.0642 0.7754 0.134 Uiso 1 1 calc R . . C445 C 0.0016(6) -0.1085(8) 0.8363(9) 0.191(10) Uani 1 1 d . . . H44E H -0.0161 -0.1395 0.8285 0.286 Uiso 1 1 calc R . . H44F H 0.0044 -0.1016 0.8707 0.286 Uiso 1 1 calc R . . H44G H 0.0266 -0.1179 0.8264 0.286 Uiso 1 1 calc R . . C446 C 0.0154(4) 0.0177(8) 0.8721(4) 0.112(6) Uani 1 1 d . . . H44H H 0.0264 -0.0123 0.8935 0.135 Uiso 1 1 calc R . . H44I H 0.0339 0.0490 0.8748 0.135 Uiso 1 1 calc R . . C447 C -0.0208(5) 0.0376(8) 0.8900(6) 0.134(6) Uani 1 1 d . . . H44J H -0.0152 0.0495 0.9233 0.202 Uiso 1 1 calc R . . H44K H -0.0395 0.0072 0.8878 0.202 Uiso 1 1 calc R . . H44L H -0.0313 0.0691 0.8705 0.202 Uiso 1 1 calc R . . C510 C 0.20749(14) 0.10982(19) 0.72363(18) 0.050(3) Uani 1 1 d G . . C511 C 0.18218(13) 0.1560(2) 0.71811(19) 0.046(2) Uani 1 1 d G . . C512 C 0.19128(15) 0.2058(2) 0.7441(2) 0.049(3) Uani 1 1 d G . . C513 C 0.22569(16) 0.20944(17) 0.7756(2) 0.056(3) Uani 1 1 d G . . H513 H 0.2318 0.2428 0.7930 0.067 Uiso 1 1 calc R . . C514 C 0.25100(12) 0.16327(17) 0.78115(14) 0.056(3) Uani 1 1 d G . . C515 C 0.24190(12) 0.11346(16) 0.75515(14) 0.052(3) Uani 1 1 d G . . C516 C 0.26720(16) 0.06729(19) 0.7607(2) 0.071(3) Uani 1 1 d G . . H516 H 0.2611 0.0340 0.7433 0.085 Uiso 1 1 calc R . . C517 C 0.30161(15) 0.0709(3) 0.7922(2) 0.087(4) Uani 1 1 d G . . H517 H 0.3185 0.0400 0.7959 0.104 Uiso 1 1 calc R . . C518 C 0.31072(14) 0.1207(3) 0.8182(2) 0.093(4) Uani 1 1 d G . . H518 H 0.3337 0.1232 0.8393 0.111 Uiso 1 1 calc R . . C519 C 0.28541(15) 0.1669(3) 0.8127(2) 0.079(4) Uani 1 1 d G . . H519 H 0.2915 0.2002 0.8301 0.095 Uiso 1 1 calc R . . O530 O 0.14695(19) 0.1516(2) 0.6902(2) 0.0521(17) Uani 1 1 d . . . C531 C 0.1625(3) 0.2539(4) 0.7440(4) 0.064(3) Uani 1 1 d . . . H53A H 0.1724 0.2810 0.7689 0.076 Uiso 1 1 calc R . . H53B H 0.1382 0.2388 0.7529 0.076 Uiso 1 1 calc R . . N532 N 0.1536(3) 0.2862(4) 0.6953(3) 0.075(3) Uani 1 1 d D . . O533 O 0.1327(2) 0.2509(3) 0.6618(2) 0.0574(18) Uani 1 1 d . . . C534 C 0.1944(5) 0.2982(6) 0.6763(5) 0.110(5) Uani 1 1 d . . . H53C H 0.2105 0.3207 0.7002 0.132 Uiso 1 1 calc R . . H53D H 0.2076 0.2624 0.6723 0.132 Uiso 1 1 calc R . . C535 C 0.1890(5) 0.3299(7) 0.6277(6) 0.142(7) Uani 1 1 d . . . H53E H 0.2140 0.3360 0.6166 0.212 Uiso 1 1 calc R . . H53F H 0.1767 0.3660 0.6318 0.212 Uiso 1 1 calc R . . H53G H 0.1729 0.3077 0.6040 0.212 Uiso 1 1 calc R . . C536 C 0.1264(6) 0.3367(6) 0.7046(6) 0.264(19) Uani 1 1 d D . . H53H H 0.1266 0.3606 0.6760 0.316 Uiso 1 1 calc R . . H53I H 0.1006 0.3198 0.7016 0.316 Uiso 1 1 calc R . . C537 C 0.1260(11) 0.3787(9) 0.7458(7) 0.52(6) Uani 1 1 d D . . H53J H 0.1074 0.4084 0.7364 0.778 Uiso 1 1 calc R . . H53K H 0.1515 0.3951 0.7534 0.778 Uiso 1 1 calc R . . H53L H 0.1187 0.3595 0.7740 0.778 Uiso 1 1 calc R . . C520 C 0.19591(16) 0.05507(19) 0.69422(18) 0.047(2) Uani 1 1 d G . . C521 C 0.17016(16) 0.0186(2) 0.71377(17) 0.051(3) Uani 1 1 d G . . C522 C 0.16218(15) -0.0347(2) 0.6932(2) 0.057(3) Uani 1 1 d G . . C523 C 0.17994(17) -0.05158(18) 0.6531(2) 0.060(3) Uani 1 1 d G . . H523 H 0.1746 -0.0873 0.6393 0.072 Uiso 1 1 calc R . . C524 C 0.20569(13) -0.01515(18) 0.63353(15) 0.062(3) Uani 1 1 d G . . C525 C 0.21367(12) 0.03817(17) 0.65409(15) 0.057(3) Uani 1 1 d G . . C526 C 0.23942(16) 0.0746(2) 0.6345(2) 0.073(3) Uani 1 1 d G . . H526 H 0.2448 0.1103 0.6483 0.088 Uiso 1 1 calc R . . C527 C 0.25718(18) 0.0577(3) 0.5944(2) 0.099(5) Uani 1 1 d G . . H527 H 0.2744 0.0821 0.5813 0.119 Uiso 1 1 calc R . . C528 C 0.24920(19) 0.0044(3) 0.5739(2) 0.100(4) Uani 1 1 d G . . H528 H 0.2611 -0.0069 0.5470 0.120 Uiso 1 1 calc R . . C529 C 0.22346(19) -0.0321(3) 0.59340(19) 0.085(4) Uani 1 1 d G . . H529 H 0.2181 -0.0677 0.5796 0.102 Uiso 1 1 calc R . . O540 O 0.14948(19) 0.0375(3) 0.7502(2) 0.0538(17) Uani 1 1 d . . . C541 C 0.1300(3) -0.0736(4) 0.7080(4) 0.052(3) Uiso 1 1 d . . . H54A H 0.1057 -0.0525 0.7044 0.063 Uiso 1 1 calc R . . H54B H 0.1269 -0.1054 0.6855 0.063 Uiso 1 1 calc R . . N542 N 0.1364(3) -0.0964(4) 0.7577(3) 0.067(3) Uani 1 1 d . . . O543 O 0.1374(2) -0.0526(3) 0.7932(3) 0.065(2) Uani 1 1 d . . . C544 C 0.1748(4) -0.1300(5) 0.7672(5) 0.081(4) Uani 1 1 d . . . H54C H 0.1747 -0.1591 0.7423 0.097 Uiso 1 1 calc R . . H54D H 0.1961 -0.1043 0.7634 0.097 Uiso 1 1 calc R . . C545 C 0.1827(5) -0.1579(7) 0.8154(6) 0.124(6) Uani 1 1 d . . . H54E H 0.2071 -0.1780 0.8173 0.186 Uiso 1 1 calc R . . H54F H 0.1621 -0.1841 0.8196 0.186 Uiso 1 1 calc R . . H54G H 0.1842 -0.1295 0.8405 0.186 Uiso 1 1 calc R . . C546 C 0.1001(4) -0.1339(5) 0.7665(5) 0.085(4) Uani 1 1 d . . . H54H H 0.1023 -0.1441 0.8007 0.102 Uiso 1 1 calc R . . H54I H 0.0767 -0.1109 0.7594 0.102 Uiso 1 1 calc R . . C547 C 0.0953(5) -0.1844(6) 0.7386(5) 0.122(6) Uani 1 1 d . . . H54J H 0.0726 -0.2043 0.7462 0.183 Uiso 1 1 calc R . . H54K H 0.1178 -0.2082 0.7460 0.183 Uiso 1 1 calc R . . H54L H 0.0923 -0.1749 0.7046 0.183 Uiso 1 1 calc R . . C610 C 0.03459(11) 0.2002(2) 0.79866(18) 0.043(2) Uani 1 1 d G . . C611 C 0.02884(15) 0.1935(2) 0.74843(18) 0.055(3) Uani 1 1 d G . . C612 C -0.00839(17) 0.1834(2) 0.72496(14) 0.048(3) Uani 1 1 d G . . C613 C -0.03988(14) 0.1800(2) 0.75172(17) 0.057(3) Uani 1 1 d G . . H613 H -0.0648 0.1732 0.7360 0.069 Uiso 1 1 calc R . . C614 C -0.03413(11) 0.18668(14) 0.80195(17) 0.054(3) Uani 1 1 d G . . C615 C 0.00310(12) 0.19681(14) 0.82542(14) 0.051(3) Uani 1 1 d G . . C616 C 0.00885(17) 0.2035(2) 0.87565(15) 0.061(3) Uani 1 1 d G . . H616 H 0.0338 0.2103 0.8914 0.073 Uiso 1 1 calc R . . C617 C -0.0226(2) 0.2001(2) 0.90241(16) 0.070(3) Uani 1 1 d G . . H617 H -0.0188 0.2046 0.9360 0.084 Uiso 1 1 calc R . . C618 C -0.05987(18) 0.1900(2) 0.8789(2) 0.075(3) Uani 1 1 d G . . H618 H -0.0809 0.1877 0.8968 0.090 Uiso 1 1 calc R . . C619 C -0.06562(13) 0.1833(2) 0.8287(2) 0.072(3) Uani 1 1 d G . . H619 H -0.0905 0.1765 0.8130 0.087 Uiso 1 1 calc R . . O630 O 0.06015(19) 0.1943(3) 0.7213(2) 0.0531(17) Uani 1 1 d . . . C631 C -0.0150(3) 0.1629(4) 0.6718(4) 0.053(3) Uani 1 1 d . . . H63A H -0.0410 0.1468 0.6653 0.064 Uiso 1 1 calc R . . H63B H 0.0036 0.1330 0.6673 0.064 Uiso 1 1 calc R . . N632 N -0.0105(3) 0.2112(3) 0.6352(3) 0.059(2) Uani 1 1 d . . . O633 O 0.0264(2) 0.2332(3) 0.6428(2) 0.066(2) Uani 1 1 d . . . C634 C -0.0390(4) 0.2571(4) 0.6398(4) 0.074(3) Uani 1 1 d . . . H63C H -0.0349 0.2868 0.6166 0.089 Uiso 1 1 calc R . . H63D H -0.0338 0.2733 0.6721 0.089 Uiso 1 1 calc R . . C635 C -0.0824(4) 0.2385(6) 0.6313(6) 0.109(5) Uani 1 1 d . . . H63E H -0.0988 0.2705 0.6360 0.164 Uiso 1 1 calc R . . H63F H -0.0869 0.2090 0.6539 0.164 Uiso 1 1 calc R . . H63G H -0.0884 0.2245 0.5987 0.164 Uiso 1 1 calc R . . C636 C -0.0168(4) 0.1827(5) 0.5848(4) 0.077(4) Uani 1 1 d . . . H63H H 0.0037 0.1548 0.5829 0.092 Uiso 1 1 calc R . . H63I H -0.0414 0.1624 0.5817 0.092 Uiso 1 1 calc R . . C637 C -0.0170(5) 0.2232(6) 0.5425(5) 0.106(5) Uani 1 1 d . . . H63J H -0.0210 0.2022 0.5125 0.159 Uiso 1 1 calc R . . H63K H 0.0075 0.2428 0.5446 0.159 Uiso 1 1 calc R . . H63L H -0.0377 0.2503 0.5434 0.159 Uiso 1 1 calc R . . C620 C 0.07596(13) 0.21645(19) 0.82118(19) 0.052(3) Uani 1 1 d G . . C621 C 0.10233(17) 0.17172(16) 0.82876(19) 0.048(2) Uani 1 1 d G . . C622 C 0.13969(16) 0.18150(19) 0.8520(2) 0.058(3) Uani 1 1 d G . . C623 C 0.15068(13) 0.2360(2) 0.86763(19) 0.056(3) Uani 1 1 d G . . H623 H 0.1757 0.2425 0.8832 0.067 Uiso 1 1 calc R . . C624 C 0.12431(12) 0.28073(17) 0.86006(14) 0.054(3) Uani 1 1 d G . . C625 C 0.08695(12) 0.27096(17) 0.83683(14) 0.053(3) Uani 1 1 d G . . C626 C 0.06058(15) 0.3157(2) 0.8292(2) 0.065(3) Uani 1 1 d G . . H626 H 0.0356 0.3091 0.8137 0.078 Uiso 1 1 calc R . . C627 C 0.0716(2) 0.37019(19) 0.8449(2) 0.086(4) Uani 1 1 d G . . H627 H 0.0539 0.4001 0.8398 0.103 Uiso 1 1 calc R . . C628 C 0.1089(2) 0.37996(17) 0.8681(2) 0.085(4) Uani 1 1 d G . . H628 H 0.1163 0.4164 0.8786 0.102 Uiso 1 1 calc R . . C629 C 0.13530(17) 0.33523(19) 0.8757(2) 0.066(3) Uani 1 1 d G . . H629 H 0.1603 0.3418 0.8912 0.079 Uiso 1 1 calc R . . O640 O 0.09310(19) 0.1192(2) 0.8099(2) 0.0522(17) Uani 1 1 d . . . C641 C 0.1721(3) 0.1356(4) 0.8560(4) 0.057(3) Uani 1 1 d . . . H64A H 0.1747 0.1207 0.8238 0.069 Uiso 1 1 calc R . . H64B H 0.1968 0.1530 0.8685 0.069 Uiso 1 1 calc R . . N642 N 0.1633(3) 0.0870(4) 0.8892(3) 0.068(3) Uani 1 1 d . . . O643 O 0.1323(2) 0.0543(3) 0.8662(3) 0.066(2) Uani 1 1 d . . . C644 C 0.1506(5) 0.1074(5) 0.9357(4) 0.096(5) Uani 1 1 d . . . H64C H 0.1266 0.1285 0.9273 0.115 Uiso 1 1 calc R . . H64D H 0.1440 0.0739 0.9535 0.115 Uiso 1 1 calc R . . C645 C 0.1763(5) 0.1432(8) 0.9702(6) 0.139(6) Uani 1 1 d . . . H64E H 0.1629 0.1528 0.9976 0.208 Uiso 1 1 calc R . . H64F H 0.1829 0.1774 0.9542 0.208 Uiso 1 1 calc R . . H64G H 0.1997 0.1225 0.9813 0.208 Uiso 1 1 calc R . . C646 C 0.1972(4) 0.0475(6) 0.8994(7) 0.122(6) Uani 1 1 d . . . H64H H 0.2183 0.0680 0.9180 0.146 Uiso 1 1 calc R . . H64I H 0.1897 0.0166 0.9196 0.146 Uiso 1 1 calc R . . C647 C 0.2112(7) 0.0241(8) 0.8586(6) 0.164(10) Uani 1 1 d . . . H64J H 0.2323 -0.0015 0.8688 0.246 Uiso 1 1 calc R . . H64K H 0.2204 0.0540 0.8392 0.246 Uiso 1 1 calc R . . H64L H 0.1906 0.0037 0.8396 0.246 Uiso 1 1 calc R . . Na4 Na 0.07867(13) 0.25895(17) 0.60436(16) 0.0721(12) Uani 1 1 d . . . Na5 Na 0.09609(11) 0.10318(14) 0.72406(13) 0.0522(10) Uani 1 1 d . . . Na6 Na 0.10838(13) -0.03506(17) 0.85991(15) 0.0688(12) Uani 1 1 d . . . S40 S 0.08800(12) 0.37351(19) 0.55384(15) 0.1166(14) Uani 1 1 d G . . O43 O 0.1014(3) 0.3194(2) 0.5413(3) 0.169(5) Uani 1 1 d G . . O42 O 0.1184(2) 0.4136(3) 0.5537(3) 0.178(6) Uani 1 1 d G . . O41 O 0.0758(2) 0.3712(4) 0.60066(18) 0.160(5) Uani 1 1 d G . . C40 C 0.04607(18) 0.3952(4) 0.5086(3) 0.188(11) Uani 1 1 d G . . F41 F 0.0581(3) 0.3975(5) 0.4625(2) 0.213(7) Uani 1 1 d G . . F43 F 0.0188(3) 0.3547(4) 0.5108(3) 0.238(7) Uani 1 1 d G . . F42 F 0.0361(4) 0.4474(3) 0.5224(3) 0.217(7) Uani 1 1 d G . . S60 S 0.12257(15) -0.11540(19) 0.94519(16) 0.1368(18) Uani 1 1 d G . . O62 O 0.0989(2) -0.1241(2) 0.9006(2) 0.155(4) Uiso 1 1 d G . . O61 O 0.1459(2) -0.0665(2) 0.9418(2) 0.186(6) Uiso 1 1 d G . . O63 O 0.14678(19) -0.1633(2) 0.9558(2) 0.285(10) Uiso 1 1 d G . . C60 C 0.0928(3) -0.1001(5) 0.9909(3) 0.220(11) Uiso 1 1 d G . . F61 F 0.0675(4) -0.0549(5) 0.9787(4) 0.355(11) Uiso 1 1 d G . . F62 F 0.0714(4) -0.1498(5) 0.9945(4) 0.294(8) Uiso 1 1 d G . . F63 F 0.1149(4) -0.0891(6) 1.0352(3) 0.286(8) Uiso 1 1 d G . . S10 S 0.2787(2) 0.2300(3) 0.4298(2) 0.135(2) Uiso 0.839(9) 1 d PG . . O11 O 0.3183(2) 0.2440(5) 0.4429(3) 0.196(7) Uiso 0.839(9) 1 d PG . . O12 O 0.2668(8) 0.2328(10) 0.3798(7) 0.377(18) Uiso 0.839(9) 1 d PG . . O13 O 0.2548(8) 0.2764(5) 0.4511(10) 0.42(2) Uiso 0.839(9) 1 d PG . . C10 C 0.2692(4) 0.1640(5) 0.4577(5) 0.265(18) Uiso 0.839(9) 1 d PG . . F13 F 0.2917(6) 0.1232(7) 0.4374(7) 0.376(15) Uiso 0.839(9) 1 d PG . . F11 F 0.2799(6) 0.1661(8) 0.5077(5) 0.291(10) Uiso 0.839(9) 1 d PG . . F12 F 0.2300(4) 0.1496(7) 0.4481(6) 0.267(9) Uiso 0.839(9) 1 d PG . . S20 S 0.6644(3) 0.3814(5) 0.6988(4) 0.252(5) Uiso 0.767(7) 1 d PG . . O21 O 0.6421(5) 0.4256(7) 0.7162(7) 0.246(11) Uiso 0.767(7) 1 d PG . . O22 O 0.6434(5) 0.3298(6) 0.6985(8) 0.290(14) Uiso 0.767(7) 1 d PG . . O23 O 0.6720(6) 0.3943(9) 0.6510(5) 0.313(15) Uiso 0.767(7) 1 d PG . . C20 C 0.7114(5) 0.3741(11) 0.7391(8) 0.54(6) Uiso 0.767(7) 1 d PG . . F21 F 0.7333(5) 0.3305(13) 0.7218(12) 0.48(2) Uiso 0.767(7) 1 d PG . . F22 F 0.7274(4) 0.4150(13) 0.7017(12) 0.390(17) Uiso 0.767(7) 1 d PG . . F23 F 0.7019(4) 0.3769(15) 0.7664(12) 0.48(3) Uiso 0.767(7) 1 d PG . . S50 S -0.1672(3) 0.1560(6) 0.7099(5) 0.213(6) Uiso 0.593(7) 1 d PG . . O51 O -0.1539(4) 0.1994(9) 0.7430(9) 0.35(2) Uiso 0.593(7) 1 d PG . . O52 O -0.1523(4) 0.1031(7) 0.7277(10) 0.32(2) Uiso 0.593(7) 1 d PG . . O53 O -0.1544(4) 0.1672(13) 0.6644(5) 0.58(5) Uiso 0.593(7) 1 d PG . . C50 C -0.2164(6) 0.1606(12) 0.7148(10) 0.35(4) Uiso 0.593(7) 1 d PG . . F51 F -0.2268(11) 0.1251(12) 0.7513(10) 0.311(16) Uiso 0.593(7) 1 d PG . . F52 F -0.2380(11) 0.2107(11) 0.7141(12) 0.328(17) Uiso 0.593(7) 1 d PG . . F53 F -0.2241(15) 0.1334(17) 0.6700(11) 0.42(3) Uiso 0.593(7) 1 d PG . . N60 N 0.1849(13) 0.8637(18) 0.4848(16) 0.224(18) Uiso 0.50 1 d PD . . C61 C 0.1786(14) 0.820(2) 0.466(3) 0.29(3) Uiso 0.50 1 d PD . . C62 C 0.1851(14) 0.7673(18) 0.4387(17) 0.191(18) Uiso 0.50 1 d PD . . N70 N 0.1743(6) 0.0459(9) 0.4676(7) 0.189(7) Uiso 1 1 d D . . C71 C 0.1952(7) 0.0204(10) 0.4475(9) 0.181(9) Uiso 1 1 d D . . C72 C 0.2271(12) -0.009(2) 0.4263(18) 0.43(3) Uiso 1 1 d D . . N81 N 0.3239(14) 0.537(2) 0.1770(18) 0.26(2) Uiso 0.50 1 d PD . . C83 C 0.3497(11) 0.5051(16) 0.1783(12) 0.128(11) Uiso 0.50 1 d PD . . C84 C 0.3736(19) 0.456(3) 0.166(3) 0.32(4) Uiso 0.50 1 d PD . . N91 N 0.1031(10) 0.9849(14) 0.2082(13) 0.347(18) Uiso 1 1 d D . . C93 C 0.1229(8) 0.9700(11) 0.1803(10) 0.194(9) Uiso 1 1 d D . . C94 C 0.1445(10) 0.9346(14) 0.1484(12) 0.262(14) Uiso 1 1 d 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 C110 0.060(7) 0.062(7) 0.044(6) -0.006(5) 0.015(5) -0.013(6) C111 0.056(7) 0.048(6) 0.035(5) 0.008(5) 0.010(5) 0.010(5) C112 0.065(7) 0.045(6) 0.045(6) 0.003(5) 0.009(5) -0.007(5) C113 0.071(8) 0.066(7) 0.055(7) 0.002(6) 0.003(6) -0.003(6) C114 0.092(9) 0.040(6) 0.043(6) 0.013(5) 0.010(6) -0.001(6) C115 0.072(8) 0.037(6) 0.058(7) 0.013(5) 0.008(6) -0.011(5) C116 0.088(9) 0.039(6) 0.063(7) -0.005(5) 0.014(6) -0.019(6) C117 0.096(10) 0.064(8) 0.089(10) 0.011(7) 0.007(8) -0.022(7) C118 0.124(13) 0.042(7) 0.114(11) 0.023(7) 0.038(10) -0.004(8) C119 0.095(10) 0.067(8) 0.090(9) 0.017(7) 0.006(8) 0.015(7) O130 0.060(4) 0.047(4) 0.052(4) 0.007(3) 0.005(3) -0.007(3) C131 0.055(7) 0.054(6) 0.057(7) -0.006(5) -0.001(5) -0.006(5) N132 0.073(7) 0.058(6) 0.061(6) -0.002(5) 0.004(5) -0.024(5) O133 0.087(6) 0.059(5) 0.063(5) -0.001(4) -0.003(4) 0.000(4) C134 0.128(12) 0.075(8) 0.041(7) 0.005(6) 0.006(7) -0.006(8) C135 0.160(16) 0.129(13) 0.081(10) -0.016(10) 0.021(10) -0.040(12) C136 0.092(11) 0.083(9) 0.111(11) -0.004(8) -0.002(9) -0.032(8) C137 0.096(14) 0.146(16) 0.22(2) 0.004(15) -0.029(14) -0.021(12) C120 0.057(7) 0.035(5) 0.041(6) 0.000(4) 0.002(5) -0.012(5) C121 0.055(7) 0.045(6) 0.042(6) -0.003(5) 0.009(5) -0.010(5) C122 0.067(7) 0.053(6) 0.026(5) -0.006(4) 0.003(5) -0.015(5) C123 0.046(6) 0.053(6) 0.057(7) -0.010(5) 0.004(5) -0.009(5) C124 0.046(6) 0.070(7) 0.045(6) -0.009(5) 0.014(5) -0.011(5) C125 0.051(7) 0.071(7) 0.034(6) -0.008(5) 0.021(5) -0.014(5) C126 0.055(7) 0.084(8) 0.065(8) -0.002(6) 0.010(6) -0.013(6) C127 0.098(11) 0.146(13) 0.051(8) -0.003(8) 0.018(8) -0.017(10) C128 0.062(9) 0.141(12) 0.080(9) 0.017(9) 0.031(7) 0.004(8) C129 0.060(8) 0.092(9) 0.077(9) 0.007(7) 0.017(6) -0.024(7) O140 0.060(5) 0.054(4) 0.047(4) -0.001(3) 0.014(3) -0.006(3) C141 0.067(7) 0.041(6) 0.072(8) 0.002(5) 0.007(6) 0.000(5) N142 0.076(7) 0.058(6) 0.055(6) -0.007(5) 0.003(5) -0.014(5) O143 0.067(5) 0.063(4) 0.054(4) -0.009(3) 0.010(4) -0.002(4) C144 0.123(13) 0.114(11) 0.051(8) -0.008(7) -0.008(8) 0.013(9) C145 0.137(16) 0.153(16) 0.126(14) -0.002(12) -0.011(12) 0.001(13) C146 0.088(10) 0.083(9) 0.122(12) -0.028(8) 0.046(8) -0.047(8) C147 0.117(13) 0.101(11) 0.163(15) -0.071(11) 0.040(11) -0.042(10) C210 0.047(6) 0.039(6) 0.069(7) 0.004(5) 0.013(5) 0.006(5) C211 0.051(7) 0.050(6) 0.051(6) 0.006(5) 0.017(5) -0.002(5) C212 0.074(8) 0.042(6) 0.051(6) 0.004(5) 0.026(6) -0.006(5) C213 0.049(7) 0.052(7) 0.106(10) 0.002(7) 0.024(7) -0.004(5) C214 0.046(7) 0.059(7) 0.088(9) 0.015(6) 0.011(6) -0.002(5) C215 0.061(8) 0.049(6) 0.062(7) 0.003(5) 0.002(6) 0.004(5) C216 0.066(8) 0.062(7) 0.076(8) 0.009(6) -0.001(6) -0.002(6) C217 0.085(10) 0.077(8) 0.087(9) 0.009(7) 0.003(8) 0.000(7) C218 0.057(9) 0.104(11) 0.148(15) -0.032(10) -0.016(9) -0.003(8) C219 0.069(9) 0.088(9) 0.088(10) -0.005(8) 0.004(7) -0.007(7) O230 0.047(4) 0.073(5) 0.066(5) 0.016(4) 0.011(4) -0.003(4) C231 0.067(8) 0.057(7) 0.088(9) -0.010(6) 0.031(6) -0.012(6) N232 0.078(7) 0.078(7) 0.069(7) 0.019(6) 0.036(5) 0.005(6) O233 0.089(6) 0.093(6) 0.068(5) 0.003(4) 0.028(5) -0.016(5) C234 0.104(12) 0.085(9) 0.088(10) -0.007(7) 0.022(8) 0.024(9) C235 0.105(14) 0.142(15) 0.164(16) -0.020(12) 0.019(12) 0.050(12) C236 0.113(13) 0.152(15) 0.085(11) 0.012(11) 0.020(9) 0.004(11) C237 0.131(16) 0.22(2) 0.121(15) -0.025(15) 0.034(12) -0.004(15) C220 0.047(6) 0.054(6) 0.042(6) 0.001(5) 0.009(5) -0.001(5) C221 0.048(6) 0.050(6) 0.043(6) 0.005(5) 0.008(5) -0.013(5) C222 0.053(7) 0.053(6) 0.048(6) -0.012(5) 0.008(5) 0.002(5) C223 0.065(7) 0.045(6) 0.072(7) 0.014(5) 0.029(6) -0.008(6) C224 0.050(7) 0.058(7) 0.062(7) 0.018(6) 0.005(5) -0.012(5) C225 0.056(7) 0.045(6) 0.052(6) 0.011(5) -0.003(5) 0.006(5) C226 0.056(7) 0.049(6) 0.069(7) 0.009(6) 0.002(5) 0.003(5) C227 0.069(8) 0.058(7) 0.080(8) 0.010(6) -0.005(7) 0.024(6) C228 0.085(10) 0.055(7) 0.090(9) 0.013(7) 0.008(7) -0.002(7) C229 0.082(9) 0.064(8) 0.072(8) 0.013(6) 0.012(7) -0.006(7) O240 0.067(5) 0.043(4) 0.066(5) 0.011(3) 0.012(4) -0.005(3) C241 0.076(8) 0.064(7) 0.062(7) -0.022(6) 0.018(6) -0.028(6) N242 0.076(7) 0.065(6) 0.089(8) -0.019(6) 0.031(6) -0.005(6) O243 0.079(6) 0.062(5) 0.079(5) -0.006(4) 0.033(4) -0.019(4) C244 0.084(11) 0.092(10) 0.136(14) -0.033(10) 0.042(10) 0.014(8) C245 0.131(16) 0.114(13) 0.160(17) -0.036(12) 0.000(13) 0.030(12) C246 0.190(18) 0.088(10) 0.068(10) 0.004(8) 0.016(11) -0.013(10) C247 0.48(5) 0.151(19) 0.130(18) -0.007(15) 0.10(2) -0.01(2) C310 0.053(7) 0.039(6) 0.060(7) -0.005(5) -0.008(5) -0.004(5) C311 0.054(7) 0.041(6) 0.046(6) 0.002(5) -0.006(5) -0.012(5) C312 0.043(6) 0.052(6) 0.061(7) -0.012(5) -0.002(5) -0.010(5) C313 0.064(7) 0.041(6) 0.058(7) 0.007(5) 0.004(6) -0.013(5) C314 0.057(7) 0.052(7) 0.072(8) -0.006(6) 0.022(6) -0.010(6) C315 0.046(6) 0.058(7) 0.060(7) -0.008(5) 0.011(5) -0.001(5) C316 0.056(7) 0.075(8) 0.099(9) 0.001(7) 0.031(7) 0.004(6) C317 0.088(10) 0.068(8) 0.110(11) 0.011(8) 0.028(8) 0.009(7) C318 0.074(10) 0.107(11) 0.120(12) -0.012(10) 0.044(8) -0.011(8) C319 0.086(9) 0.065(8) 0.082(9) 0.000(6) 0.034(7) -0.005(7) O330 0.046(4) 0.055(4) 0.061(4) 0.001(3) 0.012(3) -0.007(3) C331 0.061(7) 0.044(6) 0.064(7) 0.001(5) 0.006(5) 0.000(5) N332 0.074(7) 0.039(5) 0.065(6) 0.001(4) 0.016(5) 0.006(5) O333 0.088(6) 0.050(4) 0.057(5) 0.010(4) 0.013(4) -0.015(4) C334 0.100(10) 0.045(7) 0.087(9) -0.012(6) 0.036(7) 0.012(6) C335 0.200(18) 0.045(7) 0.096(10) 0.014(7) 0.041(11) 0.021(9) C336 0.067(8) 0.061(7) 0.088(9) -0.019(7) 0.001(6) -0.022(6) C337 0.125(13) 0.085(10) 0.098(11) 0.003(8) 0.016(9) -0.024(9) C320 0.055(7) 0.046(6) 0.060(7) -0.002(5) 0.015(5) 0.001(5) C321 0.074(8) 0.031(5) 0.049(6) 0.005(5) 0.015(6) 0.009(5) C322 0.066(8) 0.051(6) 0.060(7) -0.003(5) 0.013(6) -0.009(6) C323 0.100(10) 0.056(7) 0.078(9) 0.017(6) 0.030(8) 0.007(7) C324 0.082(9) 0.046(7) 0.081(8) 0.015(6) 0.007(7) 0.008(6) C325 0.048(7) 0.062(7) 0.063(7) -0.003(6) 0.005(5) -0.004(6) C326 0.085(10) 0.076(8) 0.084(9) 0.013(7) -0.004(7) 0.015(7) C327 0.072(9) 0.102(11) 0.119(12) 0.024(9) -0.016(8) -0.007(8) C328 0.084(11) 0.103(11) 0.110(11) 0.015(9) -0.022(9) 0.023(9) C329 0.090(10) 0.063(8) 0.097(10) 0.013(7) 0.014(8) 0.020(7) O340 0.058(5) 0.047(4) 0.068(5) 0.005(3) 0.009(4) 0.003(3) C341 0.096(10) 0.059(7) 0.081(9) 0.020(7) 0.024(7) -0.004(7) N342 0.090(8) 0.055(6) 0.089(8) -0.010(6) -0.001(6) -0.014(6) O343 0.105(7) 0.060(5) 0.076(5) -0.003(4) 0.015(5) -0.012(4) C344 0.20(2) 0.081(11) 0.118(13) 0.000(9) -0.028(12) -0.095(12) C345 0.26(4) 0.078(16) 0.64(8) 0.15(3) -0.05(4) -0.063(18) C346 0.146(16) 0.084(10) 0.150(15) -0.033(10) -0.008(12) 0.057(11) C347 0.25(3) 0.084(12) 0.26(3) -0.034(14) -0.09(2) 0.087(15) Na1 0.114(4) 0.083(3) 0.097(4) -0.007(3) 0.024(3) -0.018(3) Na2 0.0353(19) 0.0356(18) 0.0394(19) 0.0061(15) 0.0101(15) -0.0067(15) Na3 0.107(4) 0.064(3) 0.096(4) -0.010(3) 0.030(3) -0.011(3) C410 0.061(7) 0.050(6) 0.047(6) 0.011(5) -0.006(5) -0.004(5) C411 0.063(7) 0.033(5) 0.046(6) 0.002(5) 0.003(5) -0.001(5) C412 0.068(8) 0.047(6) 0.057(7) 0.014(5) -0.007(6) -0.006(6) C413 0.077(8) 0.067(8) 0.050(7) -0.016(6) 0.000(6) -0.008(6) C414 0.084(9) 0.046(6) 0.046(6) -0.009(5) -0.005(6) 0.001(6) C415 0.079(8) 0.034(6) 0.052(7) -0.006(5) -0.007(6) -0.005(5) C416 0.085(9) 0.051(7) 0.086(9) -0.001(6) 0.000(7) 0.005(6) C417 0.120(13) 0.052(8) 0.112(11) -0.012(7) 0.004(9) -0.013(8) C418 0.122(13) 0.060(8) 0.103(11) -0.031(8) -0.011(9) 0.015(8) C419 0.096(10) 0.066(8) 0.075(8) -0.014(7) -0.002(7) -0.007(7) O430 0.063(5) 0.046(4) 0.056(4) -0.006(3) 0.004(3) -0.006(3) C431 0.068(8) 0.057(7) 0.062(7) 0.000(6) 0.008(6) -0.011(6) N432 0.076(7) 0.054(6) 0.069(6) 0.009(5) 0.011(5) -0.005(5) O433 0.088(6) 0.055(4) 0.059(5) 0.001(4) 0.012(4) -0.004(4) C434 0.109(11) 0.102(10) 0.049(7) -0.001(7) 0.016(7) 0.008(8) C435 0.148(15) 0.195(17) 0.060(9) 0.034(10) 0.007(9) 0.084(13) C436 0.114(14) 0.095(11) 0.185(17) 0.065(11) 0.036(13) 0.007(11) C437 0.17(3) 0.27(4) 0.58(7) 0.16(4) 0.03(4) 0.10(3) C420 0.087(9) 0.031(5) 0.048(6) 0.005(5) -0.005(6) -0.013(5) C421 0.057(7) 0.029(5) 0.068(7) 0.015(5) 0.001(6) -0.011(5) C422 0.053(7) 0.039(6) 0.069(7) 0.005(5) 0.011(6) -0.006(5) C423 0.054(7) 0.053(6) 0.079(8) 0.007(6) -0.001(6) -0.003(5) C424 0.051(8) 0.054(7) 0.103(10) 0.011(7) -0.016(7) -0.009(6) C425 0.062(8) 0.046(6) 0.062(7) 0.007(5) -0.028(6) -0.002(5) C426 0.067(8) 0.058(7) 0.093(9) 0.001(7) -0.013(7) -0.012(6) C427 0.119(14) 0.096(11) 0.117(13) -0.009(9) -0.027(11) -0.030(10) C428 0.111(14) 0.096(11) 0.142(16) 0.004(11) -0.056(12) -0.009(10) C429 0.069(9) 0.073(8) 0.126(12) 0.007(8) -0.020(8) -0.011(7) O440 0.043(4) 0.048(4) 0.059(4) 0.000(3) -0.005(3) -0.004(3) C441 0.084(9) 0.038(6) 0.076(8) 0.018(5) 0.011(6) 0.017(6) N442 0.068(7) 0.064(6) 0.073(7) 0.012(5) 0.019(5) 0.014(5) O443 0.052(5) 0.072(5) 0.079(5) 0.015(4) 0.008(4) 0.006(4) C444 0.071(9) 0.073(9) 0.192(16) 0.073(10) 0.016(10) -0.004(7) C445 0.124(16) 0.170(18) 0.28(3) 0.136(19) 0.028(17) 0.010(14) C446 0.089(11) 0.191(16) 0.060(9) 0.049(10) 0.022(7) 0.044(11) C447 0.139(16) 0.153(15) 0.113(13) -0.009(11) 0.021(11) 0.047(12) C510 0.055(7) 0.037(5) 0.059(7) 0.012(5) 0.021(5) -0.002(5) C511 0.041(6) 0.055(6) 0.041(6) 0.008(5) 0.006(5) -0.008(5) C512 0.063(7) 0.033(5) 0.050(6) -0.003(5) 0.004(5) -0.006(5) C513 0.084(8) 0.029(5) 0.056(7) 0.007(5) 0.010(6) -0.016(5) C514 0.052(7) 0.061(7) 0.053(6) -0.006(5) -0.006(5) -0.013(6) C515 0.048(6) 0.051(6) 0.054(6) 0.004(5) -0.004(5) -0.003(5) C516 0.068(8) 0.067(8) 0.073(8) 0.004(6) -0.009(6) -0.005(6) C517 0.069(9) 0.074(9) 0.115(11) -0.004(8) -0.001(8) 0.001(7) C518 0.070(9) 0.106(11) 0.096(10) -0.005(9) -0.016(7) -0.017(8) C519 0.074(9) 0.071(8) 0.087(9) -0.022(7) -0.006(7) -0.005(7) O530 0.058(5) 0.045(4) 0.051(4) 0.001(3) 0.000(3) -0.009(3) C531 0.092(9) 0.048(6) 0.049(7) 0.000(5) -0.002(6) -0.009(6) N532 0.112(9) 0.051(6) 0.059(6) 0.001(5) -0.007(6) 0.006(6) O533 0.074(5) 0.042(4) 0.054(4) -0.005(3) -0.003(4) -0.006(3) C534 0.119(13) 0.100(11) 0.100(11) 0.031(9) -0.023(9) -0.063(10) C535 0.178(18) 0.121(13) 0.110(13) 0.034(10) -0.051(12) -0.063(12) C536 0.52(5) 0.037(8) 0.165(17) -0.009(10) -0.23(2) 0.070(16) C537 0.54(8) 0.22(4) 0.67(10) 0.26(5) -0.43(8) -0.17(4) C520 0.052(6) 0.038(5) 0.050(6) -0.003(5) 0.006(5) -0.012(5) C521 0.058(7) 0.035(5) 0.055(7) -0.004(5) -0.009(5) 0.008(5) C522 0.061(7) 0.046(6) 0.062(7) 0.009(5) 0.000(6) 0.001(5) C523 0.074(8) 0.050(6) 0.056(7) -0.015(5) 0.009(6) 0.001(6) C524 0.073(8) 0.062(7) 0.054(7) -0.012(6) 0.018(6) 0.002(6) C525 0.056(7) 0.057(7) 0.059(7) -0.001(6) 0.009(5) 0.008(6) C526 0.072(8) 0.078(8) 0.072(8) -0.009(7) 0.017(7) -0.011(7) C527 0.118(12) 0.104(11) 0.083(10) -0.014(8) 0.045(9) -0.034(9) C528 0.083(10) 0.130(13) 0.090(10) -0.010(10) 0.030(8) -0.002(9) C529 0.104(11) 0.081(9) 0.073(9) -0.016(7) 0.016(8) -0.008(8) O540 0.057(4) 0.046(4) 0.060(4) -0.012(3) 0.014(3) -0.003(3) N542 0.074(7) 0.045(5) 0.079(7) -0.003(5) 0.005(5) -0.004(5) O543 0.077(5) 0.046(4) 0.072(5) -0.001(4) 0.002(4) -0.013(4) C544 0.080(9) 0.075(8) 0.087(9) 0.006(7) 0.004(7) 0.010(7) C545 0.133(15) 0.115(12) 0.115(13) 0.026(10) -0.017(10) 0.034(10) C546 0.107(11) 0.058(8) 0.086(9) 0.021(7) -0.006(8) -0.026(7) C547 0.176(17) 0.079(10) 0.113(12) -0.003(9) 0.024(11) -0.071(10) C610 0.055(7) 0.027(5) 0.045(6) -0.001(4) -0.004(5) 0.006(4) C611 0.059(7) 0.028(5) 0.073(8) 0.010(5) -0.008(6) 0.006(5) C612 0.060(7) 0.028(5) 0.054(6) 0.003(4) -0.003(5) 0.002(5) C613 0.049(7) 0.034(5) 0.086(8) 0.007(5) -0.002(6) 0.001(5) C614 0.056(7) 0.035(5) 0.071(8) 0.014(5) 0.007(6) 0.006(5) C615 0.058(7) 0.038(6) 0.058(7) 0.006(5) 0.009(6) 0.000(5) C616 0.064(8) 0.054(6) 0.067(8) 0.012(6) 0.014(6) 0.004(5) C617 0.090(10) 0.064(7) 0.056(7) -0.009(6) 0.013(7) 0.004(7) C618 0.075(9) 0.062(7) 0.094(10) 0.009(7) 0.038(8) -0.002(6) C619 0.063(8) 0.067(8) 0.091(9) 0.017(7) 0.023(7) 0.012(6) O630 0.052(4) 0.056(4) 0.052(4) -0.002(3) 0.009(3) -0.001(3) C631 0.051(6) 0.037(5) 0.069(7) 0.000(5) 0.001(5) -0.002(5) N632 0.068(6) 0.053(5) 0.052(5) -0.008(4) -0.011(4) -0.005(5) O633 0.079(6) 0.059(4) 0.057(5) 0.007(4) -0.006(4) -0.012(4) C634 0.092(10) 0.044(6) 0.084(9) 0.009(6) -0.001(7) 0.017(6) C635 0.090(12) 0.108(11) 0.128(13) 0.001(9) 0.012(9) 0.036(9) C636 0.089(9) 0.074(8) 0.068(8) -0.006(7) 0.009(7) 0.023(7) C637 0.122(13) 0.118(12) 0.076(10) -0.006(9) 0.007(8) 0.006(10) C620 0.051(7) 0.059(7) 0.048(6) 0.013(5) 0.017(5) 0.008(5) C621 0.056(7) 0.053(6) 0.035(5) 0.002(5) 0.004(5) -0.009(5) C622 0.058(7) 0.065(7) 0.051(6) 0.011(5) 0.003(5) -0.006(6) C623 0.054(7) 0.063(7) 0.049(6) -0.001(5) -0.002(5) -0.021(6) C624 0.068(8) 0.043(6) 0.051(6) -0.011(5) 0.004(5) -0.012(6) C625 0.070(8) 0.035(6) 0.057(7) -0.006(5) 0.017(6) -0.001(5) C626 0.081(8) 0.055(7) 0.062(7) -0.011(6) 0.026(6) -0.012(6) C627 0.086(10) 0.065(8) 0.114(11) -0.002(8) 0.040(8) 0.006(7) C628 0.102(11) 0.064(8) 0.096(10) -0.044(7) 0.042(8) -0.033(8) C629 0.062(8) 0.064(7) 0.072(8) 0.002(6) 0.012(6) -0.004(6) O640 0.062(5) 0.037(4) 0.054(4) -0.005(3) -0.008(3) -0.005(3) C641 0.058(7) 0.048(6) 0.067(7) 0.011(5) 0.012(5) 0.006(5) N642 0.057(6) 0.082(7) 0.061(6) 0.001(5) -0.012(5) 0.000(5) O643 0.066(5) 0.060(4) 0.070(5) 0.007(4) -0.005(4) -0.002(4) C644 0.150(14) 0.086(9) 0.045(8) 0.017(7) -0.016(8) -0.024(9) C645 0.148(17) 0.163(16) 0.100(12) 0.007(11) -0.004(11) -0.034(13) C646 0.087(11) 0.080(10) 0.185(18) 0.042(11) -0.042(11) 0.011(8) C647 0.28(3) 0.123(15) 0.098(13) 0.002(11) 0.056(15) 0.072(16) Na4 0.085(3) 0.052(2) 0.078(3) 0.011(2) 0.005(2) -0.007(2) Na5 0.057(2) 0.043(2) 0.055(2) 0.0026(18) 0.0011(19) -0.0032(18) Na6 0.078(3) 0.065(3) 0.063(3) 0.012(2) 0.006(2) -0.005(2) S40 0.104(3) 0.121(3) 0.124(4) 0.040(3) 0.010(3) -0.004(3) O43 0.234(16) 0.106(9) 0.185(13) 0.001(8) 0.092(11) 0.015(9) O42 0.134(11) 0.168(11) 0.227(15) 0.007(10) 0.005(10) -0.087(10) O41 0.155(11) 0.247(14) 0.089(8) 0.029(8) 0.055(8) 0.023(10) C40 0.19(3) 0.125(18) 0.23(3) 0.073(19) -0.04(2) -0.005(17) F41 0.177(12) 0.338(19) 0.121(9) 0.042(10) 0.006(8) 0.037(12) F43 0.181(14) 0.31(2) 0.209(13) 0.037(13) -0.017(10) -0.080(13) F42 0.282(17) 0.178(11) 0.186(12) 0.017(9) 0.008(11) 0.112(12) S60 0.177(5) 0.107(3) 0.121(4) 0.030(3) -0.004(3) 0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C110 C111 1.3900 . ? C110 C115 1.3900 . ? C110 C120 1.572(6) . ? C111 O130 1.384(7) . ? C111 C112 1.3900 . ? C112 C113 1.3900 . ? C112 C131 1.521(10) . ? C113 C114 1.3900 . ? C114 C115 1.3900 . ? C114 C119 1.3900 . ? C115 C116 1.3900 . ? C116 C117 1.3900 . ? C117 C118 1.3900 . ? C118 C119 1.3900 . ? O130 Na2 2.385(7) . ? C131 N132 1.506(12) . ? N132 O133 1.406(11) . ? N132 C134 1.474(13) . ? N132 C136 1.514(15) . ? O133 Na1 2.305(9) . ? C134 C135 1.503(17) . ? C136 C137 1.464(19) . ? C120 C121 1.3900 . ? C120 C125 1.3900 . ? C121 O140 1.368(7) . ? C121 C122 1.3900 . ? C122 C123 1.3900 . ? C122 C141 1.516(11) . ? C123 C124 1.3900 . ? C124 C125 1.3900 . ? C124 C129 1.3900 . ? C125 C126 1.3900 . ? C126 C127 1.3900 . ? C127 C128 1.3900 . ? C128 C129 1.3900 . ? O140 Na2 2.430(7) . ? C141 N142 1.495(12) . ? N142 O143 1.424(11) . ? N142 C144 1.520(14) . ? N142 C146 1.519(13) . ? O143 Na3 2.382(9) . ? C144 C145 1.483(19) . ? C146 C147 1.466(16) . ? C210 C211 1.3900 . ? C210 C215 1.3900 . ? C210 C220 1.532(6) . ? C211 O230 1.363(8) . ? C211 C212 1.3900 . ? C212 C213 1.3900 . ? C212 C231 1.542(12) . ? C213 C214 1.3900 . ? C214 C215 1.3900 . ? C214 C219 1.3900 . ? C215 C216 1.3900 . ? C216 C217 1.3900 . ? C217 C218 1.3900 . ? C218 C219 1.3900 . ? O230 Na2 2.464(8) . ? C231 N232 1.507(14) . ? N232 O233 1.382(11) . ? N232 C234 1.530(15) . ? N232 C236 1.542(16) . ? O233 Na1 2.289(10) . ? C234 C235 1.45(2) . ? C236 C237 1.50(2) . ? C220 C221 1.3900 . ? C220 C225 1.3900 . ? C221 O240 1.380(7) . ? C221 C222 1.3900 . ? C222 C223 1.3900 . ? C222 C241 1.541(12) . ? C223 C224 1.3900 . ? C224 C225 1.3900 . ? C224 C229 1.3900 . ? C225 C226 1.3900 . ? C226 C227 1.3900 . ? C227 C228 1.3900 . ? C228 C229 1.3900 . ? O240 Na2 2.419(7) . ? C241 N242 1.522(12) . ? N242 O243 1.392(11) . ? N242 C244 1.496(15) . ? N242 C246 1.532(17) . ? O243 Na3 2.325(8) . ? C244 C245 1.398(19) . ? C246 C247 1.43(2) . ? C310 C311 1.3900 . ? C310 C315 1.3900 . ? C310 C320 1.528(6) . ? C311 O330 1.383(8) . ? C311 C312 1.3900 . ? C312 C313 1.3900 . ? C312 C331 1.541(10) . ? C313 C314 1.3900 . ? C314 C315 1.3900 . ? C314 C319 1.3900 . ? C315 C316 1.3900 . ? C316 C317 1.3900 . ? C317 C318 1.3900 . ? C318 C319 1.3900 . ? O330 Na2 2.383(7) . ? C331 N332 1.557(12) . ? N332 O333 1.380(10) . ? N332 C336 1.486(13) . ? N332 C334 1.544(13) . ? O333 Na1 2.320(9) . ? C334 C335 1.439(15) . ? C336 C337 1.468(15) . ? C320 C321 1.3900 . ? C320 C325 1.3900 . ? C321 O340 1.350(8) . ? C321 C322 1.3900 . ? C322 C323 1.3900 . ? C322 C341 1.550(13) . ? C323 C324 1.3900 . ? C324 C325 1.3900 . ? C324 C329 1.3900 . ? C325 C326 1.3900 . ? C326 C327 1.3900 . ? C327 C328 1.3900 . ? C328 C329 1.3900 . ? O340 Na2 2.409(7) . ? C341 N342 1.532(14) . ? N342 O343 1.435(11) . ? N342 C346 1.500(17) . ? N342 C344 1.548(19) . ? O343 Na3 2.359(10) . ? C344 C345 1.28(4) . ? C346 C347 1.51(2) . ? Na1 O5 2.13(2) . ? Na1 O2 2.19(2) . ? Na2 O5 2.83(2) . ? Na3 O31 2.335(10) . ? Na3 O301 2.452(19) . ? S30 O33 1.4110 . ? S30 O31 1.4113 . ? S30 O32 1.4116 . ? S30 C30 1.8671 . ? C30 F32 1.18(2) . ? C30 F33 1.38(3) . ? C30 F31 1.3908 . ? C410 C411 1.3900 . ? C410 C415 1.3900 . ? C410 C420 1.540(7) . ? C411 O430 1.355(7) . ? C411 C412 1.3900 . ? C412 C413 1.3900 . ? C412 C431 1.517(11) . ? C413 C414 1.3900 . ? C414 C415 1.3900 . ? C414 C419 1.3900 . ? C415 C416 1.3900 . ? C416 C417 1.3900 . ? C417 C418 1.3900 . ? C418 C419 1.3900 . ? O430 Na5 2.470(7) . ? C431 N432 1.533(13) . ? N432 O433 1.388(11) . ? N432 C436 1.462(17) . ? N432 C434 1.510(14) . ? O433 Na4 2.278(8) . ? C434 C435 1.498(17) . ? C436 C437 1.506(5) . ? C420 C421 1.3900 . ? C420 C425 1.3900 . ? C421 O440 1.374(7) . ? C421 C422 1.3900 . ? C422 C423 1.3900 . ? C422 C441 1.542(11) . ? C423 C424 1.3900 . ? C424 C425 1.3900 . ? C424 C429 1.3900 . ? C425 C426 1.3900 . ? C426 C427 1.3900 . ? C427 C428 1.3900 . ? C428 C429 1.3900 . ? O440 Na5 2.393(7) . ? C441 N442 1.553(12) . ? N442 O443 1.402(11) . ? N442 C446 1.519(16) . ? N442 C444 1.521(15) . ? O443 Na6 2.320(8) . ? C444 C445 1.484(18) . ? C446 C447 1.477(18) . ? C510 C511 1.3900 . ? C510 C515 1.3900 . ? C510 C520 1.549(6) . ? C511 O530 1.365(7) . ? C511 C512 1.3900 . ? C512 C513 1.3900 . ? C512 C531 1.505(11) . ? C513 C514 1.3900 . ? C514 C515 1.3900 . ? C514 C519 1.3900 . ? C515 C516 1.3900 . ? C516 C517 1.3900 . ? C517 C518 1.3900 . ? C518 C519 1.3900 . ? O530 Na5 2.378(7) . ? C531 N532 1.546(12) . ? N532 O533 1.381(10) . ? N532 C536 1.554(5) . ? N532 C534 1.586(17) . ? O533 Na4 2.310(8) . ? C534 C535 1.530(18) . ? C536 C537 1.511(5) . ? C520 C521 1.3900 . ? C520 C525 1.3900 . ? C521 O540 1.377(7) . ? C521 C522 1.3900 . ? C522 C523 1.3900 . ? C522 C541 1.533(10) . ? C523 C524 1.3900 . ? C524 C525 1.3900 . ? C524 C529 1.3900 . ? C525 C526 1.3900 . ? C526 C527 1.3900 . ? C527 C528 1.3900 . ? C528 C529 1.3900 . ? O540 Na5 2.446(7) . ? C541 N542 1.467(12) . ? N542 O543 1.421(10) . ? N542 C544 1.537(14) . ? N542 C546 1.577(14) . ? O543 Na6 2.243(9) . ? C544 C545 1.481(17) . ? C546 C547 1.415(16) . ? C610 C611 1.3900 . ? C610 C615 1.3900 . ? C610 C620 1.537(6) . ? C611 O630 1.388(8) . ? C611 C612 1.3900 . ? C612 C613 1.3900 . ? C612 C631 1.538(10) . ? C613 C614 1.3900 . ? C614 C615 1.3900 . ? C614 C619 1.3900 . ? C615 C616 1.3900 . ? C616 C617 1.3900 . ? C617 C618 1.3900 . ? C618 C619 1.3900 . ? O630 Na5 2.471(7) . ? C631 N632 1.543(12) . ? N632 O633 1.368(10) . ? N632 C634 1.474(13) . ? N632 C636 1.539(13) . ? O633 Na4 2.287(9) . ? C634 C635 1.552(17) . ? C636 C637 1.509(17) . ? C620 C621 1.3900 . ? C620 C625 1.3900 . ? C621 O640 1.361(7) . ? C621 C622 1.3900 . ? C622 C623 1.3900 . ? C622 C641 1.549(10) . ? C623 C624 1.3900 . ? C624 C625 1.3900 . ? C624 C629 1.3900 . ? C625 C626 1.3900 . ? C626 C627 1.3900 . ? C627 C628 1.3900 . ? C628 C629 1.3900 . ? O640 Na5 2.422(7) . ? C641 N642 1.521(13) . ? N642 O643 1.405(10) . ? N642 C644 1.487(15) . ? N642 C646 1.495(16) . ? O643 Na6 2.255(8) . ? C644 C645 1.486(18) . ? C646 C647 1.39(2) . ? Na4 O43 2.451(9) . ? Na4 O41 2.640(10) . ? Na4 S40 3.068(6) . ? Na6 O62 2.416(6) . ? Na6 O61 2.580(6) . ? Na6 S60 3.017(5) . ? S40 O42 1.4109 . ? S40 O43 1.4111 . ? S40 O41 1.4112 . ? S40 C40 1.8677 . ? C40 F42 1.342(13) . ? C40 F43 1.345(13) . ? C40 F41 1.3909 . ? S60 O63 1.4111 . ? S60 O62 1.4114 . ? S60 O61 1.4115 . ? S60 C60 1.760(9) . ? C60 F63 1.3907 . ? C60 F61 1.3910 . ? C60 F62 1.3912 . ? S10 O12 1.397(19) . ? S10 O11 1.4112 . ? S10 O13 1.53(2) . ? S10 C10 1.780(13) . ? C10 F12 1.3908 . ? C10 F11 1.3909 . ? C10 F13 1.3917 . ? S20 O22 1.4113 . ? S20 O21 1.4113 . ? S20 O23 1.4115 . ? S20 C20 1.8663 . ? S20 F23 2.15(3) . ? C20 F23 0.86(4) . ? C20 F21 1.3916 . ? C20 F22 1.56(4) . ? S50 O53 1.4102 . ? S50 O51 1.4110 . ? S50 O52 1.4113 . ? S50 C50 1.72(2) . ? C50 F52 1.3909 . ? C50 F53 1.3912 . ? C50 F51 1.3915 . ? N60 C61 1.155(10) . ? C61 C62 1.485(10) . ? N70 C71 1.135(8) . ? C71 C72 1.480(8) . ? N81 C83 1.157(10) . ? C83 C84 1.477(9) . ? N91 C93 1.147(9) . ? C93 C94 1.478(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C111 C110 C115 120.0 . . ? C111 C110 C120 117.2(3) . . ? C115 C110 C120 122.6(3) . . ? O130 C111 C112 118.7(4) . . ? O130 C111 C110 121.3(4) . . ? C112 C111 C110 120.0 . . ? C111 C112 C113 120.0 . . ? C111 C112 C131 120.3(5) . . ? C113 C112 C131 118.6(5) . . ? C114 C113 C112 120.0 . . ? C115 C114 C113 120.0 . . ? C115 C114 C119 120.0 . . ? C113 C114 C119 120.0 . . ? C116 C115 C114 120.0 . . ? C116 C115 C110 120.0 . . ? C114 C115 C110 120.0 . . ? C117 C116 C115 120.0 . . ? C116 C117 C118 120.0 . . ? C117 C118 C119 120.0 . . ? C118 C119 C114 120.0 . . ? C111 O130 Na2 117.7(4) . . ? N132 C131 C112 115.5(8) . . ? O133 N132 C134 108.4(9) . . ? O133 N132 C131 109.8(7) . . ? C134 N132 C131 110.1(8) . . ? O133 N132 C136 105.6(8) . . ? C134 N132 C136 113.1(9) . . ? C131 N132 C136 109.8(9) . . ? N132 O133 Na1 135.0(6) . . ? N132 C134 C135 116.4(10) . . ? C137 C136 N132 117.3(12) . . ? C121 C120 C125 120.0 . . ? C121 C120 C110 116.8(3) . . ? C125 C120 C110 123.2(3) . . ? O140 C121 C122 118.1(4) . . ? O140 C121 C120 121.4(4) . . ? C122 C121 C120 120.0 . . ? C121 C122 C123 120.0 . . ? C121 C122 C141 122.5(5) . . ? C123 C122 C141 116.0(5) . . ? C122 C123 C124 120.0 . . ? C125 C124 C123 120.0 . . ? C125 C124 C129 120.0 . . ? C123 C124 C129 120.0 . . ? C126 C125 C124 120.0 . . ? C126 C125 C120 120.0 . . ? C124 C125 C120 120.0 . . ? C125 C126 C127 120.0 . . ? C128 C127 C126 120.0 . . ? C127 C128 C129 120.0 . . ? C128 C129 C124 120.0 . . ? C121 O140 Na2 117.9(4) . . ? N142 C141 C122 116.2(7) . . ? O143 N142 C141 110.1(7) . . ? O143 N142 C144 106.0(9) . . ? C141 N142 C144 111.7(9) . . ? O143 N142 C146 108.1(9) . . ? C141 N142 C146 109.4(9) . . ? C144 N142 C146 111.3(10) . . ? N142 O143 Na3 132.1(5) . . ? C145 C144 N142 115.4(13) . . ? C147 C146 N142 115.6(11) . . ? C211 C210 C215 120.0 . . ? C211 C210 C220 116.6(3) . . ? C215 C210 C220 123.4(3) . . ? O230 C211 C212 118.9(5) . . ? O230 C211 C210 121.0(5) . . ? C212 C211 C210 120.0 . . ? C211 C212 C213 120.0 . . ? C211 C212 C231 121.4(6) . . ? C213 C212 C231 118.1(6) . . ? C214 C213 C212 120.0 . . ? C215 C214 C213 120.0 . . ? C215 C214 C219 120.0 . . ? C213 C214 C219 120.0 . . ? C216 C215 C214 120.0 . . ? C216 C215 C210 120.0 . . ? C214 C215 C210 120.0 . . ? C217 C216 C215 120.0 . . ? C216 C217 C218 120.0 . . ? C219 C218 C217 120.0 . . ? C218 C219 C214 120.0 . . ? C211 O230 Na2 115.1(5) . . ? N232 C231 C212 114.8(8) . . ? O233 N232 C231 108.7(8) . . ? O233 N232 C234 107.8(9) . . ? C231 N232 C234 111.0(10) . . ? O233 N232 C236 106.7(10) . . ? C231 N232 C236 107.4(10) . . ? C234 N232 C236 115.0(10) . . ? N232 O233 Na1 141.3(6) . . ? C235 C234 N232 114.5(12) . . ? C237 C236 N232 115.9(14) . . ? C221 C220 C225 120.0 . . ? C221 C220 C210 117.5(3) . . ? C225 C220 C210 121.8(3) . . ? O240 C221 C220 121.7(4) . . ? O240 C221 C222 118.3(4) . . ? C220 C221 C222 120.0 . . ? C223 C222 C221 120.0 . . ? C223 C222 C241 117.4(5) . . ? C221 C222 C241 122.0(5) . . ? C222 C223 C224 120.0 . . ? C225 C224 C223 120.0 . . ? C225 C224 C229 120.0 . . ? C223 C224 C229 120.0 . . ? C226 C225 C224 120.0 . . ? C226 C225 C220 120.0 . . ? C224 C225 C220 120.0 . . ? C227 C226 C225 120.0 . . ? C226 C227 C228 120.0 . . ? C229 C228 C227 120.0 . . ? C228 C229 C224 120.0 . . ? C221 O240 Na2 118.3(4) . . ? N242 C241 C222 114.4(8) . . ? O243 N242 C244 109.1(9) . . ? O243 N242 C241 108.4(8) . . ? C244 N242 C241 111.4(10) . . ? O243 N242 C246 106.9(10) . . ? C244 N242 C246 109.3(11) . . ? C241 N242 C246 111.7(9) . . ? N242 O243 Na3 134.8(6) . . ? C245 C244 N242 114.3(13) . . ? C247 C246 N242 125.3(19) . . ? C311 C310 C315 120.0 . . ? C311 C310 C320 116.7(4) . . ? C315 C310 C320 123.3(4) . . ? O330 C311 C312 119.0(4) . . ? O330 C311 C310 121.0(4) . . ? C312 C311 C310 120.0 . . ? C311 C312 C313 120.0 . . ? C311 C312 C331 121.2(5) . . ? C313 C312 C331 118.6(5) . . ? C312 C313 C314 120.0 . . ? C315 C314 C313 120.0 . . ? C315 C314 C319 120.0 . . ? C313 C314 C319 120.0 . . ? C316 C315 C314 120.0 . . ? C316 C315 C310 120.0 . . ? C314 C315 C310 120.0 . . ? C315 C316 C317 120.0 . . ? C318 C317 C316 120.0 . . ? C319 C318 C317 120.0 . . ? C318 C319 C314 120.0 . . ? C311 O330 Na2 116.2(4) . . ? C312 C331 N332 113.9(7) . . ? O333 N332 C336 109.2(8) . . ? O333 N332 C334 106.9(8) . . ? C336 N332 C334 114.6(8) . . ? O333 N332 C331 108.6(7) . . ? C336 N332 C331 111.1(8) . . ? C334 N332 C331 106.3(8) . . ? N332 O333 Na1 136.5(6) . . ? C335 C334 N332 117.9(11) . . ? C337 C336 N332 113.8(11) . . ? C321 C320 C325 120.0 . . ? C321 C320 C310 117.1(3) . . ? C325 C320 C310 122.7(3) . . ? O340 C321 C320 121.1(4) . . ? O340 C321 C322 118.7(4) . . ? C320 C321 C322 120.0 . . ? C323 C322 C321 120.0 . . ? C323 C322 C341 116.5(6) . . ? C321 C322 C341 122.6(6) . . ? C324 C323 C322 120.0 . . ? C323 C324 C325 120.0 . . ? C323 C324 C329 120.0 . . ? C325 C324 C329 120.0 . . ? C326 C325 C324 120.0 . . ? C326 C325 C320 120.0 . . ? C324 C325 C320 120.0 . . ? C327 C326 C325 120.0 . . ? C326 C327 C328 120.0 . . ? C329 C328 C327 120.0 . . ? C328 C329 C324 120.0 . . ? C321 O340 Na2 118.5(5) . . ? N342 C341 C322 112.9(9) . . ? O343 N342 C346 108.5(11) . . ? O343 N342 C341 108.7(8) . . ? C346 N342 C341 112.0(10) . . ? O343 N342 C344 106.8(10) . . ? C346 N342 C344 116.7(12) . . ? C341 N342 C344 103.7(10) . . ? N342 O343 Na3 142.2(6) . . ? C345 C344 N342 116(2) . . ? N342 C346 C347 110.1(16) . . ? O5 Na1 O2 162.7(9) . . ? O5 Na1 O233 64.9(7) . . ? O2 Na1 O233 131.5(7) . . ? O5 Na1 O133 50.6(6) . . ? O2 Na1 O133 117.5(7) . . ? O233 Na1 O133 89.2(3) . . ? O5 Na1 O333 57.9(6) . . ? O2 Na1 O333 115.3(7) . . ? O233 Na1 O333 102.8(3) . . ? O133 Na1 O333 91.1(3) . . ? O330 Na2 O130 86.2(2) . . ? O330 Na2 O340 78.9(2) . . ? O130 Na2 O340 115.1(2) . . ? O330 Na2 O240 113.9(2) . . ? O130 Na2 O240 151.2(3) . . ? O340 Na2 O240 89.9(2) . . ? O330 Na2 O140 150.7(3) . . ? O130 Na2 O140 80.0(2) . . ? O340 Na2 O140 83.7(2) . . ? O240 Na2 O140 89.3(2) . . ? O330 Na2 O230 86.8(2) . . ? O130 Na2 O230 80.8(2) . . ? O340 Na2 O230 157.4(3) . . ? O240 Na2 O230 80.0(2) . . ? O140 Na2 O230 116.0(3) . . ? O330 Na2 O5 50.8(5) . . ? O130 Na2 O5 50.4(5) . . ? O340 Na2 O5 125.0(5) . . ? O240 Na2 O5 126.8(5) . . ? O140 Na2 O5 128.7(5) . . ? O230 Na2 O5 52.0(5) . . ? O243 Na3 O31 109.7(4) . . ? O243 Na3 O343 95.4(3) . . ? O31 Na3 O343 154.8(4) . . ? O243 Na3 O143 89.6(3) . . ? O31 Na3 O143 101.6(4) . . ? O343 Na3 O143 80.3(3) . . ? O243 Na3 O301 114.3(5) . . ? O31 Na3 O301 78.0(5) . . ? O343 Na3 O301 89.9(5) . . ? O143 Na3 O301 154.9(5) . . ? O33 S30 O31 109.5 . . ? O33 S30 O32 109.5 . . ? O31 S30 O32 109.5 . . ? O33 S30 C30 109.5 . . ? O31 S30 C30 109.5 . . ? O32 S30 C30 109.5 . . ? S30 O31 Na3 143.3(7) . . ? F32 C30 F33 124.3(19) . . ? F32 C30 F31 107.0(11) . . ? F33 C30 F31 108.5(9) . . ? F32 C30 S30 107.2(11) . . ? F33 C30 S30 99.7(11) . . ? F31 C30 S30 109.4 . . ? Na1 O5 Na2 169.2(11) . . ? C411 C410 C415 120.0 . . ? C411 C410 C420 117.1(3) . . ? C415 C410 C420 122.5(3) . . ? O430 C411 C412 120.3(5) . . ? O430 C411 C410 119.5(5) . . ? C412 C411 C410 120.0 . . ? C411 C412 C413 120.0 . . ? C411 C412 C431 120.8(6) . . ? C413 C412 C431 119.0(6) . . ? C414 C413 C412 120.0 . . ? C413 C414 C415 120.0 . . ? C413 C414 C419 120.0 . . ? C415 C414 C419 120.0 . . ? C416 C415 C414 120.0 . . ? C416 C415 C410 120.0 . . ? C414 C415 C410 120.0 . . ? C415 C416 C417 120.0 . . ? C416 C417 C418 120.0 . . ? C419 C418 C417 120.0 . . ? C418 C419 C414 120.0 . . ? C411 O430 Na5 112.5(4) . . ? C412 C431 N432 115.8(8) . . ? O433 N432 C436 110.3(10) . . ? O433 N432 C434 108.0(9) . . ? C436 N432 C434 108.8(11) . . ? O433 N432 C431 108.4(8) . . ? C436 N432 C431 111.0(10) . . ? C434 N432 C431 110.2(8) . . ? N432 O433 Na4 139.0(6) . . ? C435 C434 N432 112.8(11) . . ? N432 C436 C437 135(2) . . ? C421 C420 C425 120.0 . . ? C421 C420 C410 119.2(4) . . ? C425 C420 C410 120.8(4) . . ? O440 C421 C420 120.3(5) . . ? O440 C421 C422 119.3(5) . . ? C420 C421 C422 120.0 . . ? C421 C422 C423 120.0 . . ? C421 C422 C441 120.3(6) . . ? C423 C422 C441 118.4(6) . . ? C424 C423 C422 120.0 . . ? C425 C424 C423 120.0 . . ? C425 C424 C429 120.0 . . ? C423 C424 C429 120.0 . . ? C426 C425 C424 120.0 . . ? C426 C425 C420 120.0 . . ? C424 C425 C420 120.0 . . ? C427 C426 C425 120.0 . . ? C428 C427 C426 120.0 . . ? C427 C428 C429 120.0 . . ? C428 C429 C424 120.0 . . ? C421 O440 Na5 115.7(4) . . ? C422 C441 N442 114.2(7) . . ? O443 N442 C446 105.8(9) . . ? O443 N442 C444 109.2(9) . . ? C446 N442 C444 115.3(11) . . ? O443 N442 C441 108.3(8) . . ? C446 N442 C441 108.1(9) . . ? C444 N442 C441 110.0(9) . . ? N442 O443 Na6 134.9(6) . . ? C445 C444 N442 113.9(13) . . ? C447 C446 N442 116.9(12) . . ? C511 C510 C515 120.0 . . ? C511 C510 C520 118.1(3) . . ? C515 C510 C520 121.9(3) . . ? O530 C511 C512 119.2(4) . . ? O530 C511 C510 120.6(4) . . ? C512 C511 C510 120.0 . . ? C511 C512 C513 120.0 . . ? C511 C512 C531 121.5(5) . . ? C513 C512 C531 118.0(5) . . ? C514 C513 C512 120.0 . . ? C515 C514 C513 120.0 . . ? C515 C514 C519 120.0 . . ? C513 C514 C519 120.0 . . ? C516 C515 C514 120.0 . . ? C516 C515 C510 120.0 . . ? C514 C515 C510 120.0 . . ? C517 C516 C515 120.0 . . ? C516 C517 C518 120.0 . . ? C519 C518 C517 120.0 . . ? C518 C519 C514 120.0 . . ? C511 O530 Na5 117.6(4) . . ? C512 C531 N532 115.7(8) . . ? O533 N532 C531 108.8(8) . . ? O533 N532 C536 107.0(9) . . ? C531 N532 C536 106.9(9) . . ? O533 N532 C534 107.3(8) . . ? C531 N532 C534 106.5(9) . . ? C536 N532 C534 119.9(12) . . ? N532 O533 Na4 136.6(5) . . ? C535 C534 N532 111.0(12) . . ? C537 C536 N532 133.2(16) . . ? C521 C520 C525 120.0 . . ? C521 C520 C510 116.3(4) . . ? C525 C520 C510 123.1(4) . . ? O540 C521 C520 120.0(4) . . ? O540 C521 C522 119.7(4) . . ? C520 C521 C522 120.0 . . ? C523 C522 C521 120.0 . . ? C523 C522 C541 116.6(5) . . ? C521 C522 C541 122.9(5) . . ? C524 C523 C522 120.0 . . ? C525 C524 C523 120.0 . . ? C525 C524 C529 120.0 . . ? C523 C524 C529 120.0 . . ? C526 C525 C524 120.0 . . ? C526 C525 C520 120.0 . . ? C524 C525 C520 120.0 . . ? C525 C526 C527 120.0 . . ? C528 C527 C526 120.0 . . ? C527 C528 C529 120.0 . . ? C528 C529 C524 120.0 . . ? C521 O540 Na5 115.2(4) . . ? N542 C541 C522 115.8(7) . . ? O543 N542 C541 111.9(7) . . ? O543 N542 C544 107.8(8) . . ? C541 N542 C544 112.2(9) . . ? O543 N542 C546 104.5(8) . . ? C541 N542 C546 108.4(8) . . ? C544 N542 C546 111.8(9) . . ? N542 O543 Na6 136.7(6) . . ? C545 C544 N542 116.4(11) . . ? C547 C546 N542 115.3(12) . . ? C611 C610 C615 120.0 . . ? C611 C610 C620 116.6(3) . . ? C615 C610 C620 123.2(3) . . ? O630 C611 C612 119.1(4) . . ? O630 C611 C610 120.8(4) . . ? C612 C611 C610 120.0 . . ? C611 C612 C613 120.0 . . ? C611 C612 C631 121.6(5) . . ? C613 C612 C631 117.1(5) . . ? C614 C613 C612 120.0 . . ? C613 C614 C615 120.0 . . ? C613 C614 C619 120.0 . . ? C615 C614 C619 120.0 . . ? C616 C615 C614 120.0 . . ? C616 C615 C610 120.0 . . ? C614 C615 C610 120.0 . . ? C615 C616 C617 120.0 . . ? C618 C617 C616 120.0 . . ? C617 C618 C619 120.0 . . ? C618 C619 C614 120.0 . . ? C611 O630 Na5 113.2(4) . . ? C612 C631 N632 112.5(7) . . ? O633 N632 C634 109.1(8) . . ? O633 N632 C636 109.4(9) . . ? C634 N632 C636 112.0(8) . . ? O633 N632 C631 109.9(7) . . ? C634 N632 C631 111.2(9) . . ? C636 N632 C631 105.2(8) . . ? N632 O633 Na4 143.3(6) . . ? N632 C634 C635 115.0(9) . . ? C637 C636 N632 114.6(10) . . ? C621 C620 C625 120.0 . . ? C621 C620 C610 115.7(3) . . ? C625 C620 C610 124.1(3) . . ? O640 C621 C620 120.5(4) . . ? O640 C621 C622 119.2(4) . . ? C620 C621 C622 120.0 . . ? C623 C622 C621 120.0 . . ? C623 C622 C641 116.8(5) . . ? C621 C622 C641 122.8(5) . . ? C622 C623 C624 120.0 . . ? C625 C624 C623 120.0 . . ? C625 C624 C629 120.0 . . ? C623 C624 C629 120.0 . . ? C626 C625 C624 120.0 . . ? C626 C625 C620 120.0 . . ? C624 C625 C620 120.0 . . ? C627 C626 C625 120.0 . . ? C626 C627 C628 120.0 . . ? C629 C628 C627 120.0 . . ? C628 C629 C624 120.0 . . ? C621 O640 Na5 118.8(4) . . ? N642 C641 C622 111.6(8) . . ? O643 N642 C644 106.3(9) . . ? O643 N642 C646 106.4(9) . . ? C644 N642 C646 110.0(11) . . ? O643 N642 C641 109.6(7) . . ? C644 N642 C641 112.5(9) . . ? C646 N642 C641 111.7(10) . . ? N642 O643 Na6 142.7(6) . . ? C645 C644 N642 121.6(13) . . ? C647 C646 N642 115.7(15) . . ? O433 Na4 O633 93.1(3) . . ? O433 Na4 O533 91.0(3) . . ? O633 Na4 O533 106.0(3) . . ? O433 Na4 O43 103.7(3) . . ? O633 Na4 O43 145.5(3) . . ? O533 Na4 O43 103.6(3) . . ? O433 Na4 O41 157.1(3) . . ? O633 Na4 O41 104.7(3) . . ? O533 Na4 O41 97.6(3) . . ? O43 Na4 O41 53.67(12) . . ? O433 Na4 S40 129.8(3) . . ? O633 Na4 S40 125.2(3) . . ? O533 Na4 S40 105.4(2) . . ? O43 Na4 S40 26.76(7) . . ? O41 Na4 S40 27.33(6) . . ? O530 Na5 O440 149.1(3) . . ? O530 Na5 O640 115.7(2) . . ? O440 Na5 O640 88.2(2) . . ? O530 Na5 O540 81.5(2) . . ? O440 Na5 O540 80.9(2) . . ? O640 Na5 O540 85.9(2) . . ? O530 Na5 O430 81.0(2) . . ? O440 Na5 O430 84.5(2) . . ? O640 Na5 O430 154.5(3) . . ? O540 Na5 O430 116.9(3) . . ? O530 Na5 O630 88.0(2) . . ? O440 Na5 O630 117.0(3) . . ? O640 Na5 O630 79.3(2) . . ? O540 Na5 O630 156.0(3) . . ? O430 Na5 O630 82.3(2) . . ? O543 Na6 O643 92.2(3) . . ? O543 Na6 O443 89.9(3) . . ? O643 Na6 O443 99.6(3) . . ? O543 Na6 O62 108.9(3) . . ? O643 Na6 O62 147.0(3) . . ? O443 Na6 O62 105.4(3) . . ? O543 Na6 O61 116.3(3) . . ? O643 Na6 O61 93.3(2) . . ? O443 Na6 O61 150.3(3) . . ? O62 Na6 O61 54.83(12) . . ? O543 Na6 S60 118.8(3) . . ? O643 Na6 S60 119.9(3) . . ? O443 Na6 S60 127.7(3) . . ? O62 Na6 S60 27.36(6) . . ? O61 Na6 S60 27.84(6) . . ? O42 S40 O43 109.5 . . ? O42 S40 O41 109.5 . . ? O43 S40 O41 109.5 . . ? O42 S40 C40 109.5 . . ? O43 S40 C40 109.5 . . ? O41 S40 C40 109.5 . . ? O42 S40 Na4 134.9(3) . . ? O43 S40 Na4 51.5(3) . . ? O41 S40 Na4 59.2(3) . . ? C40 S40 Na4 115.5(3) . . ? S40 O43 Na4 101.8(4) . . ? S40 O41 Na4 93.5(3) . . ? F42 C40 F43 115.4(10) . . ? F42 C40 F41 110.0(6) . . ? F43 C40 F41 110.9(7) . . ? F42 C40 S40 105.3(6) . . ? F43 C40 S40 105.4(5) . . ? F41 C40 S40 109.5 . . ? O63 S60 O62 109.5 . . ? O63 S60 O61 109.5 . . ? O62 S60 O61 109.5 . . ? O63 S60 C60 113.3(4) . . ? O62 S60 C60 109.4(6) . . ? O61 S60 C60 105.6(5) . . ? O63 S60 Na6 134.26(12) . . ? O62 S60 Na6 51.88(12) . . ? O61 S60 Na6 58.61(12) . . ? C60 S60 Na6 112.4(4) . . ? S60 O62 Na6 100.76(15) . . ? S60 O61 Na6 93.55(14) . . ? F63 C60 F61 109.5 . . ? F63 C60 F62 109.4 . . ? F61 C60 F62 109.5 . . ? F63 C60 S60 111.5(5) . . ? F61 C60 S60 112.8(3) . . ? F62 C60 S60 104.0(4) . . ? O12 S10 O11 113.9(11) . . ? O12 S10 O13 103.9(12) . . ? O11 S10 O13 106.7(11) . . ? O12 S10 C10 115.1(12) . . ? O11 S10 C10 108.3(8) . . ? O13 S10 C10 108.5(11) . . ? F12 C10 F11 109.5 . . ? F12 C10 F13 109.5 . . ? F11 C10 F13 109.4 . . ? F12 C10 S10 110.7(7) . . ? F11 C10 S10 111.1(7) . . ? F13 C10 S10 106.5(7) . . ? O22 S20 O21 109.5 . . ? O22 S20 O23 109.5 . . ? O21 S20 O23 109.4 . . ? O22 S20 C20 109.5 . . ? O21 S20 C20 109.5 . . ? O23 S20 C20 109.5 . . ? O22 S20 F23 102.6(12) . . ? O21 S20 F23 91.9(13) . . ? O23 S20 F23 131.7(10) . . ? C20 S20 F23 23.5(10) . . ? F23 C20 F21 130(3) . . ? F23 C20 F22 137(4) . . ? F21 C20 F22 88.5(16) . . ? F23 C20 S20 96.9(17) . . ? F21 C20 S20 109.5 . . ? F22 C20 S20 84.2(10) . . ? C20 F23 S20 59.7(16) . . ? O53 S50 O51 109.5 . . ? O53 S50 O52 109.5 . . ? O51 S50 O52 109.5 . . ? O53 S50 C50 118.4(11) . . ? O51 S50 C50 98.8(11) . . ? O52 S50 C50 110.5(11) . . ? F52 C50 F53 109.5 . . ? F52 C50 F51 109.5 . . ? F53 C50 F51 109.4 . . ? F52 C50 S50 126(2) . . ? F53 C50 S50 89(2) . . ? F51 C50 S50 111(2) . . ? N60 C61 C62 160(4) . . ? N70 C71 C72 171(4) . . ? N81 C83 C84 160(4) . . ? N91 C93 C94 164(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.933 _refine_diff_density_min -1.150 _refine_diff_density_rms 0.192 data_och207m _database_code_CSD 183484 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C93 H108 F9 Li3 N6 O21 S3' _chemical_formula_weight 1933.85 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' 'Li' 'Li' -0.0003 0.0001 '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' 'F' 'F' 0.0171 0.0103 '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 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 15.331(10) _cell_length_b 27.404(16) _cell_length_c 23.137(14) _cell_angle_alpha 90.00 _cell_angle_beta 98.033(16) _cell_angle_gamma 90.00 _cell_volume 9625(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 43 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4056 _exptl_absorpt_coefficient_mu 0.166 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.5357 _exptl_absorpt_correction_T_max 0.7758 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60845 _diffrn_reflns_av_R_equivalents 0.3816 _diffrn_reflns_av_sigmaI/netI 0.4941 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 28.43 _reflns_number_total 22498 _reflns_number_gt 5127 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXL-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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0111(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 22498 _refine_ls_number_parameters 1038 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.3720 _refine_ls_R_factor_gt 0.1553 _refine_ls_wR_factor_ref 0.4896 _refine_ls_wR_factor_gt 0.3680 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0.004 _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 S1 S 0.08195(19) 0.85985(11) 0.00350(13) 0.0576(8) Uani 1 1 d D . . O1S O 0.0831(6) 0.8470(3) -0.0572(3) 0.076(2) Uani 1 1 d D . . O2S O 0.0272(5) 0.8297(2) 0.0335(3) 0.061(2) Uani 1 1 d D . . O3S O 0.1667(5) 0.8710(3) 0.0366(3) 0.072(2) Uani 1 1 d D . . C1S C 0.0257(7) 0.9176(5) -0.0002(4) 0.070(4) Uani 1 1 d D . . F1S F -0.0576(5) 0.9139(3) -0.0247(3) 0.095(3) Uani 1 1 d D . . F2S F 0.0642(5) 0.9511(3) -0.0304(3) 0.087(2) Uani 1 1 d D . . F3S F 0.0248(5) 0.9377(2) 0.0523(3) 0.081(2) Uani 1 1 d D . . O5S O 0.7885(5) -0.0089(2) 0.2962(4) 0.095(3) Uiso 1 1 d D . . S2S S 0.8515(3) -0.04143(19) 0.3276(2) 0.0608(19) Uiso 0.527(7) 1 d PGD A 1 O4S O 0.9025(5) -0.0210(3) 0.3795(3) 0.084(5) Uiso 0.527(7) 1 d PGD A 1 O6S O 0.8971(5) -0.0761(3) 0.2953(3) 0.097(7) Uiso 0.527(7) 1 d PGD A 1 C2S C 0.7708(4) -0.0785(2) 0.3552(2) 0.065(7) Uiso 0.527(7) 1 d PGD A 1 F4S F 0.7154(4) -0.0529(3) 0.3823(4) 0.062(3) Uiso 0.527(7) 1 d PGD A 1 F5S F 0.8066(6) -0.1121(2) 0.3939(4) 0.077(4) Uiso 0.527(7) 1 d PGD A 1 F6S F 0.7216(5) -0.1041(3) 0.3136(3) 0.104(5) Uiso 0.527(7) 1 d PGD A 1 S2SA S 0.7879(4) -0.05967(18) 0.3096(2) 0.063(2) Uiso 0.473(7) 1 d PGD A 2 O4SA O 0.7446(5) -0.0946(4) 0.2672(3) 0.071(5) Uiso 0.473(7) 1 d PGD A 2 O6SA O 0.7894(6) -0.0732(4) 0.3703(2) 0.085(6) Uiso 0.473(7) 1 d PGD A 2 C2SA C 0.9020(4) -0.0630(4) 0.3002(4) 0.036(6) Uiso 0.473(7) 1 d PGD A 2 F4SA F 0.9166(6) -0.0487(5) 0.2481(5) 0.115(6) Uiso 0.473(7) 1 d PGD A 2 F5SA F 0.9274(12) -0.1088(4) 0.3068(7) 0.120(7) Uiso 0.473(7) 1 d PGD A 2 F6SA F 0.9469(11) -0.0395(5) 0.3441(6) 0.115(6) Uiso 0.473(7) 1 d PGD A 2 S3 S 0.17751(18) 0.36583(10) 0.10297(10) 0.0439(7) Uani 1 1 d D . . O7S O 0.2527(5) 0.3478(3) 0.1408(3) 0.067(2) Uani 1 1 d D . . O8S O 0.1845(7) 0.3561(3) 0.0429(3) 0.080(3) Uani 1 1 d D . . O9S O 0.0955(5) 0.3560(3) 0.1221(4) 0.081(3) Uani 1 1 d D . . C3S C 0.1910(7) 0.4308(4) 0.1090(4) 0.059(3) Uani 1 1 d D . . F8S F 0.1237(6) 0.4538(3) 0.0797(6) 0.158(5) Uani 1 1 d D . . F7S F 0.2598(5) 0.4476(2) 0.0880(3) 0.076(2) Uani 1 1 d D . . F9S F 0.1961(8) 0.4468(3) 0.1624(4) 0.148(5) Uani 1 1 d D . . Li1 Li 0.5005(11) 0.1616(6) 0.2200(6) 0.044(4) Uani 1 1 d . . . Li2 Li 0.3151(11) 0.2911(6) 0.1638(7) 0.050(4) Uani 1 1 d . . . Li3 Li 0.6920(16) 0.0387(6) 0.2736(8) 0.075(7) Uani 1 1 d . A . C1 C 0.2416(4) 0.00105(17) 0.0535(2) 0.060(3) Uani 1 1 d G . . H1 H 0.1859 -0.0080 0.0639 0.072 Uiso 1 1 calc R . . C2 C 0.2845(5) -0.02985(16) 0.0191(2) 0.067(4) Uani 1 1 d G . . H2 H 0.2583 -0.0600 0.0059 0.080 Uiso 1 1 calc R . . C3 C 0.3659(5) -0.01668(18) 0.0040(2) 0.063(3) Uani 1 1 d G . . H3 H 0.3953 -0.0378 -0.0195 0.076 Uiso 1 1 calc R . . C4 C 0.4044(3) 0.02740(19) 0.0233(2) 0.056(3) Uani 1 1 d G . . H4 H 0.4600 0.0364 0.0130 0.067 Uiso 1 1 calc R . . C5 C 0.3614(3) 0.05830(15) 0.05773(16) 0.050(3) Uani 1 1 d G . . C6 C 0.2800(3) 0.04512(15) 0.07285(16) 0.048(3) Uani 1 1 d G . . C7 C 0.2370(3) 0.07602(19) 0.1073(2) 0.055(3) Uani 1 1 d G . . H7 H 0.1814 0.0670 0.1176 0.066 Uiso 1 1 calc R . . C8 C 0.2755(4) 0.12010(18) 0.1266(2) 0.051(3) Uani 1 1 d G . . C9 C 0.3569(4) 0.13328(15) 0.1115(2) 0.047(3) Uani 1 1 d G . . C10 C 0.3998(3) 0.10238(17) 0.0770(2) 0.050(3) Uani 1 1 d G . . C11 C 0.4905(3) 0.12160(19) 0.06284(16) 0.050(3) Uani 1 1 d G . . C12 C 0.5614(4) 0.12158(19) 0.10742(14) 0.046(3) Uani 1 1 d G . . C13 C 0.6446(3) 0.1352(2) 0.09582(17) 0.049(3) Uani 1 1 d G . . C14 C 0.6568(3) 0.1488(2) 0.03965(19) 0.047(3) Uani 1 1 d G . . H14 H 0.7137 0.1581 0.0317 0.057 Uiso 1 1 calc R . . C15 C 0.5859(3) 0.14885(13) -0.00492(14) 0.046(3) Uani 1 1 d G . . C16 C 0.5028(3) 0.13524(13) 0.00667(14) 0.047(3) Uani 1 1 d G . . C17 C 0.4318(3) 0.1353(2) -0.03790(18) 0.049(3) Uani 1 1 d G . . H17 H 0.3750 0.1260 -0.0300 0.059 Uiso 1 1 calc R . . C18 C 0.4441(4) 0.1489(2) -0.09407(16) 0.056(3) Uani 1 1 d G . . H18 H 0.3956 0.1489 -0.1245 0.067 Uiso 1 1 calc R . . C19 C 0.5273(4) 0.1625(2) -0.10567(14) 0.062(3) Uani 1 1 d G . . H19 H 0.5356 0.1718 -0.1441 0.074 Uiso 1 1 calc R . . C20 C 0.5982(3) 0.1625(2) -0.06110(16) 0.056(3) Uani 1 1 d G . . H20 H 0.6550 0.1718 -0.0690 0.068 Uiso 1 1 calc R . . C21 C 0.2283(8) 0.1492(4) 0.1700(4) 0.055(3) Uani 1 1 d . . . H21A H 0.1785 0.1295 0.1802 0.066 Uiso 1 1 calc R . . H21B H 0.2698 0.1543 0.2062 0.066 Uiso 1 1 calc R . . C22 C 0.1559(10) 0.2253(4) 0.1925(5) 0.087(5) Uani 1 1 d D . . H22A H 0.1342 0.2573 0.1763 0.105 Uiso 1 1 calc R . . H22B H 0.2028 0.2317 0.2255 0.105 Uiso 1 1 calc R . . C23 C 0.0805(11) 0.1986(5) 0.2151(8) 0.158(10) Uani 1 1 d D . . H23A H 0.0580 0.2185 0.2449 0.237 Uiso 1 1 calc R . . H23B H 0.1019 0.1673 0.2321 0.237 Uiso 1 1 calc R . . H23C H 0.0332 0.1927 0.1827 0.237 Uiso 1 1 calc R . . C24 C 0.1309(7) 0.1922(4) 0.0921(4) 0.047(3) Uani 1 1 d . . . H24A H 0.1624 0.1760 0.0629 0.056 Uiso 1 1 calc R . . H24B H 0.0824 0.1704 0.0998 0.056 Uiso 1 1 calc R . . C25 C 0.0922(7) 0.2388(4) 0.0667(4) 0.052(3) Uani 1 1 d . . . H25A H 0.0523 0.2318 0.0308 0.079 Uiso 1 1 calc R . . H25B H 0.1395 0.2604 0.0578 0.079 Uiso 1 1 calc R . . H25C H 0.0594 0.2548 0.0949 0.079 Uiso 1 1 calc R . . C26 C 0.7222(7) 0.1459(4) 0.1454(4) 0.055(3) Uani 1 1 d . . . H26A H 0.7685 0.1641 0.1288 0.065 Uiso 1 1 calc R . . H26B H 0.7005 0.1668 0.1752 0.065 Uiso 1 1 calc R . . C27 C 0.7909(8) 0.0680(4) 0.1297(4) 0.060(3) Uani 1 1 d . . . H27A H 0.8290 0.0870 0.1069 0.072 Uiso 1 1 calc R . . H27B H 0.7384 0.0576 0.1026 0.072 Uiso 1 1 calc R . . C28 C 0.8411(11) 0.0226(5) 0.1538(6) 0.092(5) Uani 1 1 d . . . H28A H 0.8581 0.0033 0.1215 0.138 Uiso 1 1 calc R . . H28B H 0.8034 0.0029 0.1756 0.138 Uiso 1 1 calc R . . H28C H 0.8941 0.0324 0.1799 0.138 Uiso 1 1 calc R . . C29 C 0.8294(9) 0.1134(5) 0.2246(5) 0.086(5) Uani 1 1 d D . . H29A H 0.8484 0.0834 0.2466 0.104 Uiso 1 1 calc R . . H29B H 0.8015 0.1350 0.2511 0.104 Uiso 1 1 calc R . . C30 C 0.9107(10) 0.1391(6) 0.2082(6) 0.116(6) Uani 1 1 d D . . H30A H 0.9514 0.1464 0.2437 0.174 Uiso 1 1 calc R . . H30B H 0.8930 0.1695 0.1875 0.174 Uiso 1 1 calc R . . H30C H 0.9400 0.1177 0.1829 0.174 Uiso 1 1 calc R . . C31 C 0.6865(4) 0.3143(3) 0.4360(3) 0.102(6) Uani 1 1 d G . . H31 H 0.6833 0.3076 0.4760 0.122 Uiso 1 1 calc R . . C32 C 0.7024(5) 0.3615(2) 0.4184(4) 0.106(6) Uani 1 1 d G . . H32 H 0.7101 0.3872 0.4463 0.127 Uiso 1 1 calc R . . C33 C 0.7072(5) 0.37129(19) 0.3600(4) 0.097(5) Uani 1 1 d G . . H33 H 0.7181 0.4036 0.3479 0.116 Uiso 1 1 calc R . . C34 C 0.6960(4) 0.33377(19) 0.3192(3) 0.071(4) Uani 1 1 d G . . H34 H 0.6993 0.3404 0.2792 0.085 Uiso 1 1 calc R . . C35 C 0.6801(3) 0.28650(18) 0.3368(2) 0.058(3) Uani 1 1 d G . . C36 C 0.6754(3) 0.2767(2) 0.3952(2) 0.074(4) Uani 1 1 d G . . C37 C 0.6594(4) 0.2295(2) 0.4129(2) 0.062(3) Uani 1 1 d G . . H37 H 0.6562 0.2228 0.4528 0.074 Uiso 1 1 calc R . . C38 C 0.6483(4) 0.1920(2) 0.3721(3) 0.051(3) Uani 1 1 d G . . C39 C 0.6530(4) 0.20170(19) 0.3137(2) 0.052(3) Uani 1 1 d G . . C40 C 0.6689(4) 0.2490(2) 0.29602(18) 0.052(3) Uani 1 1 d G . . C41 C 0.6837(3) 0.2556(2) 0.23202(19) 0.051(3) Uani 1 1 d G . . C42 C 0.6092(3) 0.2513(2) 0.1906(2) 0.046(3) Uani 1 1 d G . . C43 C 0.6147(3) 0.2604(2) 0.1321(2) 0.050(3) Uani 1 1 d G . . C44 C 0.6947(3) 0.2739(2) 0.11507(18) 0.061(3) Uani 1 1 d G . . H44 H 0.6985 0.2801 0.0751 0.073 Uiso 1 1 calc R . . C45 C 0.7692(3) 0.27814(14) 0.15648(19) 0.054(3) Uani 1 1 d G . . C46 C 0.7638(3) 0.26900(14) 0.21496(18) 0.056(3) Uani 1 1 d G . . C47 C 0.8383(3) 0.2733(2) 0.2564(2) 0.069(4) Uani 1 1 d G . . H47 H 0.8345 0.2670 0.2963 0.083 Uiso 1 1 calc R . . C48 C 0.9183(3) 0.2867(2) 0.2393(3) 0.081(4) Uani 1 1 d G . . H48 H 0.9693 0.2896 0.2676 0.097 Uiso 1 1 calc R . . C49 C 0.9238(3) 0.2958(2) 0.1808(3) 0.078(4) Uani 1 1 d G . . H49 H 0.9785 0.3050 0.1692 0.094 Uiso 1 1 calc R . . C50 C 0.8493(3) 0.2916(2) 0.1394(3) 0.067(3) Uani 1 1 d G . . H50 H 0.8531 0.2978 0.0995 0.080 Uiso 1 1 calc R . . C51 C 0.6209(9) 0.1433(4) 0.3924(4) 0.070(4) Uani 1 1 d . . . H51A H 0.5633 0.1347 0.3698 0.084 Uiso 1 1 calc R . . H51B H 0.6122 0.1462 0.4339 0.084 Uiso 1 1 calc R . . C52 C 0.6841(11) 0.0635(7) 0.4217(6) 0.145(10) Uani 1 1 d D . . H52A H 0.6937 0.0733 0.4633 0.174 Uiso 1 1 calc R . . H52B H 0.7287 0.0390 0.4146 0.174 Uiso 1 1 calc R . . C53 C 0.5908(12) 0.0448(4) 0.4033(6) 0.091(5) Uani 1 1 d D . . H53A H 0.5810 0.0156 0.4260 0.136 Uiso 1 1 calc R . . H53B H 0.5829 0.0366 0.3616 0.136 Uiso 1 1 calc R . . H53C H 0.5484 0.0701 0.4104 0.136 Uiso 1 1 calc R . . C54 C 0.7808(11) 0.1221(6) 0.4121(6) 0.130(8) Uani 1 1 d D . . H54A H 0.7974 0.1487 0.3869 0.156 Uiso 1 1 calc R . . H54B H 0.7805 0.1352 0.4520 0.156 Uiso 1 1 calc R . . C55 C 0.8470(18) 0.0801(10) 0.4135(8) 0.31(2) Uani 1 1 d D . . H55A H 0.9060 0.0919 0.4289 0.464 Uiso 1 1 calc R . . H55B H 0.8473 0.0675 0.3738 0.464 Uiso 1 1 calc R . . H55C H 0.8302 0.0539 0.4385 0.464 Uiso 1 1 calc R . . C56 C 0.5366(7) 0.2507(4) 0.0837(4) 0.048(3) Uani 1 1 d . . . H56A H 0.5123 0.2179 0.0896 0.057 Uiso 1 1 calc R . . H56B H 0.5585 0.2508 0.0454 0.057 Uiso 1 1 calc R . . C57 C 0.4990(7) 0.3386(3) 0.0742(4) 0.045(3) Uani 1 1 d . . . H57A H 0.5229 0.3395 0.0366 0.054 Uiso 1 1 calc R . . H57B H 0.5484 0.3448 0.1058 0.054 Uiso 1 1 calc R . . C58 C 0.4307(7) 0.3793(4) 0.0745(4) 0.055(3) Uani 1 1 d . . . H58A H 0.4585 0.4109 0.0693 0.083 Uiso 1 1 calc R . . H58B H 0.4074 0.3790 0.1119 0.083 Uiso 1 1 calc R . . H58C H 0.3825 0.3740 0.0426 0.083 Uiso 1 1 calc R . . C59 C 0.3867(7) 0.2752(4) 0.0372(4) 0.052(3) Uani 1 1 d . . . H59A H 0.3380 0.2985 0.0394 0.062 Uiso 1 1 calc R . . H59B H 0.3655 0.2424 0.0467 0.062 Uiso 1 1 calc R . . C60 C 0.4070(8) 0.2745(5) -0.0246(4) 0.063(3) Uani 1 1 d . . . H60A H 0.3541 0.2650 -0.0510 0.095 Uiso 1 1 calc R . . H60B H 0.4542 0.2509 -0.0278 0.095 Uiso 1 1 calc R . . H60C H 0.4260 0.3070 -0.0351 0.095 Uiso 1 1 calc R . . C61 C 0.1405(5) 0.0194(2) 0.2513(3) 0.088(5) Uani 1 1 d G . . H61 H 0.1246 -0.0081 0.2272 0.105 Uiso 1 1 calc R . . C62 C 0.0783(4) 0.0414(3) 0.2811(3) 0.086(5) Uani 1 1 d G . . H62 H 0.0200 0.0290 0.2773 0.103 Uiso 1 1 calc R . . C63 C 0.1015(4) 0.0817(3) 0.3164(3) 0.082(4) Uani 1 1 d G . . H63 H 0.0590 0.0968 0.3368 0.098 Uiso 1 1 calc R . . C64 C 0.1869(4) 0.1000(2) 0.3219(2) 0.066(3) Uani 1 1 d G . . H64 H 0.2027 0.1275 0.3461 0.079 Uiso 1 1 calc R . . C65 C 0.2490(4) 0.07794(16) 0.29215(18) 0.067(4) Uani 1 1 d G . . C66 C 0.2258(4) 0.03765(16) 0.25683(19) 0.079(4) Uani 1 1 d G . . C67 C 0.2880(5) 0.01561(19) 0.2270(2) 0.078(4) Uani 1 1 d G . . H67 H 0.2721 -0.0119 0.2029 0.094 Uiso 1 1 calc R . . C68 C 0.3733(5) 0.0339(2) 0.2325(2) 0.066(4) Uani 1 1 d G . . C69 C 0.3965(4) 0.0742(2) 0.2679(3) 0.058(3) Uani 1 1 d G . . C70 C 0.3344(4) 0.09620(19) 0.2977(2) 0.058(3) Uani 1 1 d G . . C71 C 0.3679(4) 0.13686(18) 0.34149(14) 0.051(3) Uani 1 1 d G . . C72 C 0.3898(4) 0.1814(2) 0.31858(15) 0.042(2) Uani 1 1 d G . . C73 C 0.4189(4) 0.21965(17) 0.3558(2) 0.039(2) Uani 1 1 d G . . C74 C 0.4260(4) 0.21343(15) 0.41586(19) 0.052(3) Uani 1 1 d G . . H74 H 0.4458 0.2396 0.4413 0.062 Uiso 1 1 calc R . . C75 C 0.4040(3) 0.16892(15) 0.43877(14) 0.056(3) Uani 1 1 d G . . C76 C 0.3749(3) 0.13064(15) 0.40159(15) 0.054(3) Uani 1 1 d G . . C77 C 0.3530(5) 0.08613(16) 0.4245(2) 0.072(4) Uani 1 1 d G . . H77 H 0.3331 0.0600 0.3991 0.086 Uiso 1 1 calc R . . C78 C 0.3601(5) 0.0799(2) 0.4846(2) 0.085(5) Uani 1 1 d G . . H78 H 0.3450 0.0495 0.5003 0.102 Uiso 1 1 calc R . . C79 C 0.3891(5) 0.1182(2) 0.52178(16) 0.095(5) Uani 1 1 d G . . H79 H 0.3940 0.1139 0.5629 0.114 Uiso 1 1 calc R . . C80 C 0.4111(5) 0.1627(2) 0.49887(14) 0.067(4) Uani 1 1 d G . . H80 H 0.4309 0.1889 0.5243 0.080 Uiso 1 1 calc R . . C81 C 0.4363(9) 0.0106(4) 0.1952(4) 0.070(4) Uani 1 1 d . . . H81A H 0.4029 -0.0130 0.1683 0.084 Uiso 1 1 calc R . . H81B H 0.4585 0.0364 0.1710 0.084 Uiso 1 1 calc R . . C82 C 0.5622(11) -0.0468(4) 0.1888(5) 0.089(5) Uani 1 1 d . . . H82A H 0.5234 -0.0742 0.1740 0.107 Uiso 1 1 calc R . . H82B H 0.6157 -0.0608 0.2117 0.107 Uiso 1 1 calc R . . C83 C 0.5896(12) -0.0182(5) 0.1355(5) 0.108(6) Uani 1 1 d . . . H83A H 0.6196 -0.0403 0.1115 0.161 Uiso 1 1 calc R . . H83B H 0.6293 0.0086 0.1496 0.161 Uiso 1 1 calc R . . H83C H 0.5368 -0.0048 0.1119 0.161 Uiso 1 1 calc R . . C84 C 0.4945(11) -0.0474(4) 0.2773(4) 0.092(5) Uani 1 1 d D . . H84A H 0.4595 -0.0289 0.3027 0.111 Uiso 1 1 calc R . . H84B H 0.5502 -0.0575 0.3013 0.111 Uiso 1 1 calc R . . C85 C 0.4434(13) -0.0926(6) 0.2540(8) 0.163(9) Uani 1 1 d D . . H85A H 0.4295 -0.1124 0.2868 0.245 Uiso 1 1 calc R . . H85B H 0.4792 -0.1118 0.2304 0.245 Uiso 1 1 calc R . . H85C H 0.3886 -0.0826 0.2299 0.245 Uiso 1 1 calc R . . C86 C 0.4533(7) 0.2679(4) 0.3321(4) 0.048(3) Uani 1 1 d . . . H86A H 0.4823 0.2871 0.3657 0.058 Uiso 1 1 calc R . . H86B H 0.4990 0.2597 0.3075 0.058 Uiso 1 1 calc R . . C87 C 0.4307(8) 0.3445(4) 0.2755(5) 0.057(3) Uani 1 1 d . . . H87A H 0.4804 0.3333 0.2558 0.069 Uiso 1 1 calc R . . H87B H 0.3881 0.3612 0.2459 0.069 Uiso 1 1 calc R . . C88 C 0.4657(9) 0.3814(4) 0.3220(5) 0.072(4) Uani 1 1 d . . . H88A H 0.4935 0.4085 0.3038 0.107 Uiso 1 1 calc R . . H88B H 0.5092 0.3657 0.3511 0.107 Uiso 1 1 calc R . . H88C H 0.4169 0.3939 0.3409 0.107 Uiso 1 1 calc R . . C89 C 0.3133(7) 0.3126(4) 0.3312(4) 0.049(3) Uani 1 1 d . . . H89A H 0.3391 0.3284 0.3681 0.058 Uiso 1 1 calc R . . H89B H 0.2846 0.2820 0.3413 0.058 Uiso 1 1 calc R . . C90 C 0.2436(8) 0.3461(5) 0.2996(5) 0.069(4) Uani 1 1 d . . . H90A H 0.1988 0.3529 0.3249 0.104 Uiso 1 1 calc R . . H90B H 0.2159 0.3303 0.2637 0.104 Uiso 1 1 calc R . . H90C H 0.2710 0.3768 0.2899 0.104 Uiso 1 1 calc R . . N1 N 0.1934(5) 0.1983(3) 0.1474(3) 0.041(2) Uani 1 1 d . . . N2 N 0.7620(6) 0.1000(3) 0.1745(3) 0.050(2) Uani 1 1 d . A . N3 N 0.6852(8) 0.1015(4) 0.3870(3) 0.084(4) Uani 1 1 d . A . N4 N 0.4621(5) 0.2888(3) 0.0825(3) 0.044(2) Uani 1 1 d . . . N5 N 0.5147(7) -0.0156(3) 0.2290(3) 0.065(3) Uani 1 1 d D A . N6 N 0.3859(5) 0.3000(3) 0.2972(3) 0.043(2) Uani 1 1 d . . . O1 O 0.3970(4) 0.1743(2) 0.1373(2) 0.0471(18) Uani 1 1 d . . . O2 O 0.5513(5) 0.1121(2) 0.1641(2) 0.0504(19) Uani 1 1 d . . . O3 O 0.6304(5) 0.1648(2) 0.2731(3) 0.055(2) Uani 1 1 d . . . O4 O 0.5294(4) 0.2366(2) 0.2051(3) 0.0465(17) Uani 1 1 d . . . O5 O 0.4809(5) 0.0940(3) 0.2692(3) 0.059(2) Uani 1 1 d . . . O6 O 0.3950(4) 0.1872(2) 0.2604(2) 0.0487(18) Uani 1 1 d . . . O7 O 0.2647(4) 0.2279(3) 0.1357(3) 0.056(2) Uani 1 1 d . . . O8 O 0.6986(6) 0.0751(3) 0.2004(3) 0.062(2) Uani 1 1 d . . . O9 O 0.6893(5) 0.0919(3) 0.3288(2) 0.056(2) Uani 1 1 d . . . O10 O 0.4300(4) 0.2877(3) 0.1373(3) 0.0505(18) Uani 1 1 d . . . O11 O 0.5735(6) 0.0207(3) 0.2562(3) 0.066(2) Uani 1 1 d . . . O12 O 0.3482(4) 0.2739(2) 0.2473(3) 0.0473(18) 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 S1 0.0507(19) 0.048(2) 0.0658(17) -0.0001(15) -0.0217(13) -0.0052(14) O1S 0.082(7) 0.073(6) 0.069(5) -0.002(4) -0.004(4) -0.011(5) O2S 0.075(6) 0.031(4) 0.072(5) 0.000(4) -0.011(4) -0.013(4) O3S 0.059(5) 0.072(6) 0.073(5) 0.018(4) -0.031(4) -0.005(4) C1S 0.064(9) 0.055(9) 0.078(8) -0.011(7) -0.041(7) -0.003(7) F1S 0.065(5) 0.071(5) 0.131(6) -0.002(5) -0.049(4) 0.012(4) F2S 0.101(6) 0.048(5) 0.100(5) 0.018(4) -0.030(4) -0.005(4) F3S 0.086(5) 0.057(5) 0.092(5) -0.016(4) -0.015(4) 0.012(4) S3 0.0474(17) 0.0386(17) 0.0414(13) -0.0038(11) -0.0092(11) 0.0029(12) O7S 0.065(6) 0.068(6) 0.059(4) 0.021(4) -0.022(4) 0.005(4) O8S 0.148(9) 0.053(5) 0.034(3) -0.009(4) -0.001(4) -0.011(5) O9S 0.048(6) 0.071(6) 0.130(7) -0.011(5) 0.027(5) -0.017(4) C3S 0.055(8) 0.038(8) 0.083(8) -0.022(6) 0.002(6) -0.006(6) F8S 0.073(7) 0.049(5) 0.334(16) 0.013(7) -0.034(8) 0.014(5) F7S 0.074(5) 0.050(4) 0.106(5) 0.003(4) 0.022(4) -0.007(4) F9S 0.227(12) 0.108(8) 0.132(7) -0.082(6) 0.103(8) -0.090(8) Li1 0.048(10) 0.039(10) 0.036(8) -0.010(7) -0.022(7) -0.001(8) Li2 0.040(10) 0.044(11) 0.059(10) 0.017(8) -0.017(8) -0.007(8) Li3 0.124(19) 0.022(10) 0.066(12) -0.016(9) -0.034(11) 0.008(11) C1 0.074(9) 0.052(8) 0.048(6) 0.003(6) -0.012(6) -0.009(6) C2 0.110(11) 0.026(7) 0.053(6) -0.005(5) -0.026(7) -0.017(7) C3 0.084(9) 0.060(9) 0.040(5) 0.000(5) -0.016(6) -0.026(7) C4 0.084(9) 0.030(7) 0.046(6) 0.004(5) -0.024(5) -0.011(6) C5 0.079(8) 0.025(6) 0.040(5) -0.004(4) -0.019(5) -0.008(6) C6 0.066(8) 0.033(7) 0.037(5) 0.004(5) -0.019(5) -0.015(5) C7 0.070(8) 0.033(7) 0.051(6) 0.010(5) -0.026(5) -0.009(6) C8 0.055(7) 0.049(7) 0.040(5) 0.014(5) -0.021(5) -0.013(5) C9 0.065(7) 0.027(6) 0.039(5) 0.009(4) -0.023(5) -0.016(5) C10 0.068(8) 0.036(7) 0.039(5) 0.007(5) -0.012(5) 0.003(6) C11 0.076(8) 0.025(6) 0.043(5) 0.001(4) -0.016(5) -0.011(5) C12 0.070(8) 0.031(6) 0.030(5) 0.002(4) -0.023(5) 0.002(5) C13 0.069(8) 0.031(6) 0.038(5) 0.005(4) -0.027(5) -0.005(5) C14 0.064(7) 0.035(6) 0.038(5) 0.007(4) -0.014(5) 0.000(5) C15 0.057(7) 0.042(7) 0.032(5) 0.007(4) -0.017(4) -0.008(5) C16 0.068(7) 0.044(7) 0.025(4) 0.005(4) -0.015(4) -0.011(6) C17 0.068(7) 0.036(6) 0.036(5) -0.001(4) -0.020(5) -0.009(5) C18 0.068(8) 0.057(8) 0.031(5) 0.003(5) -0.031(5) -0.008(6) C19 0.079(9) 0.058(8) 0.039(5) 0.012(5) -0.022(5) -0.021(7) C20 0.055(7) 0.062(8) 0.046(5) 0.007(5) -0.016(5) -0.016(6) C21 0.071(8) 0.048(7) 0.039(5) 0.015(5) -0.017(5) -0.013(6) C22 0.162(15) 0.050(8) 0.060(7) -0.011(6) 0.049(9) -0.024(9) C23 0.24(2) 0.087(12) 0.184(18) 0.055(13) 0.153(19) 0.054(14) C24 0.051(7) 0.045(7) 0.035(5) -0.011(4) -0.024(4) -0.002(5) C25 0.045(7) 0.056(8) 0.048(6) -0.002(5) -0.019(5) 0.007(5) C26 0.067(8) 0.033(7) 0.052(6) 0.007(5) -0.028(5) -0.007(5) C27 0.097(10) 0.030(7) 0.046(6) 0.010(5) -0.012(6) 0.013(6) C28 0.144(14) 0.053(9) 0.072(8) 0.009(7) -0.010(8) 0.027(9) C29 0.100(12) 0.078(10) 0.064(8) -0.005(7) -0.052(8) 0.016(9) C30 0.107(14) 0.151(17) 0.076(9) 0.009(10) -0.035(9) 0.032(13) C31 0.055(9) 0.110(13) 0.137(12) -0.097(11) 0.007(8) -0.015(8) C32 0.042(8) 0.119(14) 0.158(15) -0.105(12) 0.023(9) -0.019(8) C33 0.052(9) 0.079(10) 0.165(15) -0.085(11) 0.032(9) -0.027(7) C34 0.049(8) 0.057(9) 0.105(9) -0.045(7) 0.000(6) -0.004(6) C35 0.035(6) 0.056(8) 0.078(8) -0.033(6) -0.014(5) 0.005(5) C36 0.025(6) 0.105(11) 0.087(9) -0.059(8) -0.011(6) 0.001(6) C37 0.045(7) 0.077(9) 0.057(6) -0.037(7) -0.011(5) 0.005(6) C38 0.040(6) 0.063(8) 0.041(5) -0.017(5) -0.020(4) 0.016(5) C39 0.045(7) 0.058(8) 0.045(5) -0.015(5) -0.022(5) 0.026(5) C40 0.049(7) 0.043(7) 0.054(6) -0.013(5) -0.032(5) 0.015(5) C41 0.057(7) 0.027(6) 0.058(6) -0.007(5) -0.031(5) 0.005(5) C42 0.054(7) 0.033(7) 0.045(5) 0.007(4) -0.019(5) -0.003(5) C43 0.051(7) 0.033(6) 0.061(6) 0.007(5) -0.016(5) 0.001(5) C44 0.046(7) 0.044(8) 0.087(8) 0.013(6) -0.009(6) 0.012(5) C45 0.034(7) 0.050(8) 0.072(7) 0.006(6) -0.016(5) 0.004(5) C46 0.023(6) 0.040(7) 0.097(9) -0.011(6) -0.024(5) -0.006(5) C47 0.055(8) 0.074(9) 0.072(7) -0.032(7) -0.015(6) 0.016(6) C48 0.033(8) 0.096(11) 0.106(10) -0.037(9) -0.019(7) 0.008(7) C49 0.039(8) 0.080(10) 0.113(11) -0.033(9) 0.002(7) -0.006(6) C50 0.033(7) 0.050(8) 0.111(10) -0.001(7) -0.013(6) -0.002(5) C51 0.092(10) 0.072(9) 0.037(5) -0.017(6) -0.020(6) 0.045(8) C52 0.23(3) 0.140(18) 0.060(9) 0.032(11) 0.005(13) 0.109(19) C53 0.166(16) 0.021(7) 0.071(8) 0.010(6) -0.034(9) 0.008(8) C54 0.152(16) 0.139(16) 0.076(9) -0.057(10) -0.067(10) 0.096(13) C55 0.35(4) 0.43(4) 0.106(14) -0.13(2) -0.116(17) 0.35(4) C56 0.043(6) 0.039(7) 0.055(6) 0.005(5) -0.016(5) 0.004(5) C57 0.058(7) 0.025(6) 0.049(5) 0.013(4) -0.005(5) 0.000(5) C58 0.053(7) 0.048(7) 0.060(6) 0.006(5) -0.009(5) 0.007(5) C59 0.037(6) 0.054(7) 0.057(6) 0.009(5) -0.020(5) -0.007(5) C60 0.064(8) 0.077(9) 0.042(5) -0.016(6) -0.017(5) 0.002(6) C61 0.090(11) 0.070(10) 0.084(9) 0.019(8) -0.059(8) -0.027(8) C62 0.068(10) 0.062(10) 0.113(11) 0.023(9) -0.040(8) -0.019(8) C63 0.102(12) 0.045(8) 0.088(9) 0.023(7) -0.021(8) -0.010(8) C64 0.073(9) 0.053(8) 0.061(7) 0.021(6) -0.026(6) -0.023(7) C65 0.098(11) 0.033(7) 0.054(7) 0.019(5) -0.043(6) -0.023(7) C66 0.121(13) 0.040(8) 0.059(7) 0.017(6) -0.050(7) -0.013(8) C67 0.132(13) 0.032(7) 0.053(7) 0.009(6) -0.050(7) 0.001(8) C68 0.110(11) 0.041(7) 0.035(5) 0.004(5) -0.032(6) -0.003(7) C69 0.098(10) 0.026(6) 0.040(5) 0.000(5) -0.029(6) -0.009(6) C70 0.104(10) 0.020(6) 0.040(5) 0.009(5) -0.026(6) 0.003(6) C71 0.062(7) 0.038(7) 0.043(5) 0.011(5) -0.025(5) -0.004(5) C72 0.054(7) 0.034(6) 0.031(4) 0.001(4) -0.015(4) -0.001(5) C73 0.038(6) 0.034(6) 0.041(5) 0.003(4) -0.007(4) 0.003(4) C74 0.055(7) 0.057(8) 0.038(5) 0.002(5) -0.014(5) -0.001(6) C75 0.088(9) 0.032(7) 0.040(5) 0.013(5) -0.016(5) -0.008(6) C76 0.085(9) 0.031(6) 0.036(5) 0.015(5) -0.024(5) -0.005(6) C77 0.110(11) 0.052(8) 0.044(6) 0.000(6) -0.022(6) -0.010(7) C78 0.159(14) 0.048(8) 0.040(6) 0.007(6) -0.013(7) -0.018(8) C79 0.173(16) 0.061(9) 0.042(6) 0.017(6) -0.023(8) -0.020(10) C80 0.110(10) 0.040(7) 0.040(5) 0.005(5) -0.027(6) -0.006(7) C81 0.129(11) 0.037(7) 0.031(5) 0.002(5) -0.036(6) -0.017(7) C82 0.171(15) 0.041(8) 0.048(7) -0.004(6) -0.008(8) -0.009(9) C83 0.22(2) 0.046(9) 0.046(7) -0.008(6) -0.009(9) -0.008(10) C84 0.167(16) 0.044(8) 0.063(8) -0.015(7) 0.005(9) -0.033(9) C85 0.15(2) 0.19(2) 0.144(16) 0.042(17) -0.004(14) -0.041(17) C86 0.050(7) 0.042(7) 0.045(5) 0.002(5) -0.021(5) 0.006(5) C87 0.062(8) 0.039(7) 0.065(7) 0.020(6) -0.013(5) -0.004(6) C88 0.077(10) 0.031(7) 0.100(9) -0.003(7) -0.008(7) -0.007(6) C89 0.042(7) 0.044(7) 0.057(6) 0.008(5) -0.003(5) 0.007(5) C90 0.051(8) 0.086(10) 0.068(7) 0.021(7) 0.001(6) 0.015(6) N1 0.047(5) 0.041(5) 0.033(4) 0.001(4) -0.003(4) -0.012(4) N2 0.072(7) 0.024(5) 0.046(5) 0.004(4) -0.020(4) 0.007(5) N3 0.144(11) 0.073(8) 0.028(4) -0.009(5) -0.015(5) 0.063(7) N4 0.044(5) 0.043(6) 0.041(4) 0.009(4) -0.010(4) 0.000(4) N5 0.144(10) 0.019(5) 0.026(4) -0.002(4) -0.011(5) -0.011(5) N6 0.050(5) 0.033(5) 0.041(4) -0.006(4) -0.019(4) 0.006(4) O1 0.058(5) 0.035(4) 0.041(3) -0.001(3) -0.020(3) -0.014(3) O2 0.081(5) 0.031(4) 0.032(3) 0.004(3) -0.019(3) -0.008(4) O3 0.080(6) 0.037(4) 0.039(3) -0.015(3) -0.022(3) 0.011(4) O4 0.047(4) 0.038(4) 0.049(4) 0.003(3) -0.014(3) -0.006(3) O5 0.084(6) 0.046(5) 0.041(4) 0.001(3) -0.013(4) -0.016(4) O6 0.060(5) 0.047(5) 0.032(3) 0.005(3) -0.019(3) -0.010(4) O7 0.042(4) 0.051(5) 0.067(4) 0.022(4) -0.020(3) -0.014(4) O8 0.106(7) 0.037(5) 0.038(4) 0.001(3) -0.014(4) 0.009(4) O9 0.080(6) 0.054(5) 0.029(3) -0.006(3) -0.013(3) 0.023(4) O10 0.047(5) 0.055(5) 0.046(4) 0.010(3) -0.009(3) -0.001(3) O11 0.116(7) 0.036(5) 0.038(4) -0.009(3) -0.016(4) -0.002(4) O12 0.053(5) 0.035(4) 0.047(4) 0.004(3) -0.017(3) -0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O2S 1.425(7) . ? S1 O3S 1.446(7) . ? S1 O1S 1.449(7) . ? S1 C1S 1.798(13) . ? C1S F1S 1.327(10) . ? C1S F3S 1.335(10) . ? C1S F2S 1.339(10) . ? O5S S2SA 1.427(5) . ? O5S S2S 1.436(5) . ? O5S Li3 1.98(2) . ? S2S O6S 1.4476 . ? S2S O4S 1.4522 . ? S2S C2S 1.7866 . ? C2S F4S 1.3259 . ? C2S F6S 1.336(5) . ? C2S F5S 1.3465 . ? S2SA O6SA 1.4482 . ? S2SA O4SA 1.4637 . ? S2SA C2SA 1.7955 . ? C2SA F6SA 1.315(5) . ? C2SA F5SA 1.316(5) . ? C2SA F4SA 1.3166 . ? S3 O9S 1.417(7) . ? S3 O8S 1.434(6) . ? S3 O7S 1.435(7) . ? S3 C3S 1.796(12) . ? O7S Li2 1.862(19) . ? C3S F9S 1.303(10) . ? C3S F7S 1.305(10) . ? C3S F8S 1.313(11) . ? Li1 O6 2.098(18) . ? Li1 O2 2.099(17) . ? Li1 O4 2.140(18) . ? Li1 O3 2.190(16) . ? Li1 O5 2.218(18) . ? Li1 O1 2.335(15) . ? Li2 O10 1.948(19) . ? Li2 O7 1.971(19) . ? Li2 O12 1.984(17) . ? Li3 O11 1.87(3) . ? Li3 O9 1.945(19) . ? Li3 O8 1.98(2) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C5 C6 1.3900 . ? C5 C10 1.3900 . ? C6 C7 1.3900 . ? C7 C8 1.3900 . ? C8 C9 1.3900 . ? C8 C21 1.540(12) . ? C9 O1 1.377(7) . ? C9 C10 1.3900 . ? C10 C11 1.564(6) . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 O2 1.366(7) . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C13 C26 1.560(10) . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C15 C20 1.3900 . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C18 C19 1.3900 . ? C19 C20 1.3900 . ? C21 N1 1.513(13) . ? C22 N1 1.461(13) . ? C22 C23 1.521(5) . ? C24 C25 1.494(14) . ? C24 N1 1.497(11) . ? C26 N2 1.514(12) . ? C27 N2 1.473(12) . ? C27 C28 1.528(16) . ? C29 N2 1.486(13) . ? C29 C30 1.524(5) . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C35 C40 1.3900 . ? C36 C37 1.3900 . ? C37 C38 1.3900 . ? C38 C39 1.3900 . ? C38 C51 1.492(14) . ? C39 O3 1.389(7) . ? C39 C40 1.3900 . ? C40 C41 1.540(6) . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C42 O4 1.373(8) . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C43 C56 1.544(10) . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C45 C50 1.3900 . ? C46 C47 1.3900 . ? C47 C48 1.3900 . ? C48 C49 1.3900 . ? C49 C50 1.3900 . ? C51 N3 1.529(14) . ? C52 N3 1.315(17) . ? C52 C53 1.524(5) . ? C54 C55 1.532(5) . ? C54 N3 1.60(2) . ? C56 N4 1.545(12) . ? C57 N4 1.501(12) . ? C57 C58 1.529(14) . ? C59 N4 1.495(12) . ? C59 C60 1.503(13) . ? C61 C62 1.3900 . ? C61 C66 1.3900 . ? C62 C63 1.3900 . ? C63 C64 1.3900 . ? C64 C65 1.3900 . ? C65 C66 1.3900 . ? C65 C70 1.3900 . ? C66 C67 1.3900 . ? C67 C68 1.3900 . ? C68 C69 1.3900 . ? C68 C81 1.523(14) . ? C69 C70 1.3900 . ? C69 O5 1.399(9) . ? C70 C71 1.545(6) . ? C71 C72 1.3900 . ? C71 C76 1.3900 . ? C72 O6 1.369(6) . ? C72 C73 1.3900 . ? C73 C74 1.3900 . ? C73 C86 1.552(11) . ? C74 C75 1.3900 . ? C75 C76 1.3900 . ? C75 C80 1.3900 . ? C76 C77 1.3900 . ? C77 C78 1.3900 . ? C78 C79 1.3900 . ? C79 C80 1.3900 . ? C81 N5 1.520(15) . ? C82 N5 1.522(15) . ? C82 C83 1.567(16) . ? C84 N5 1.484(5) . ? C84 C85 1.523(5) . ? C86 N6 1.504(11) . ? C87 C88 1.518(15) . ? C87 N6 1.519(13) . ? C89 N6 1.490(12) . ? C89 C90 1.516(14) . ? N1 O7 1.418(9) . ? N2 O8 1.390(11) . ? N3 O9 1.381(9) . ? N4 O10 1.422(9) . ? N5 O11 1.428(11) . ? N6 O12 1.410(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2S S1 O3S 114.3(5) . . ? O2S S1 O1S 114.8(5) . . ? O3S S1 O1S 115.6(5) . . ? O2S S1 C1S 102.8(5) . . ? O3S S1 C1S 103.2(5) . . ? O1S S1 C1S 103.8(5) . . ? F1S C1S F3S 106.7(10) . . ? F1S C1S F2S 107.3(9) . . ? F3S C1S F2S 104.7(9) . . ? F1S C1S S1 112.3(8) . . ? F3S C1S S1 112.7(7) . . ? F2S C1S S1 112.7(8) . . ? S2SA O5S S2S 46.1(3) . . ? S2SA O5S Li3 132.1(9) . . ? S2S O5S Li3 164.8(9) . . ? O5S S2S O6S 119.2(5) . . ? O5S S2S O4S 115.2(6) . . ? O6S S2S O4S 115.9 . . ? O5S S2S C2S 94.8(5) . . ? O6S S2S C2S 102.7 . . ? O4S S2S C2S 104.1 . . ? F4S C2S F6S 106.5(6) . . ? F4S C2S F5S 106.0 . . ? F6S C2S F5S 104.9(6) . . ? F4S C2S S2S 112.9 . . ? F6S C2S S2S 112.9(4) . . ? F5S C2S S2S 112.9 . . ? O5S S2SA O6SA 117.4(6) . . ? O5S S2SA O4SA 120.5(7) . . ? O6SA S2SA O4SA 115.3 . . ? O5S S2SA C2SA 89.3(5) . . ? O6SA S2SA C2SA 102.8 . . ? O4SA S2SA C2SA 104.0 . . ? F6SA C2SA F5SA 105.2(4) . . ? F6SA C2SA F4SA 115.1(9) . . ? F5SA C2SA F4SA 107.8(10) . . ? F6SA C2SA S2SA 107.1(10) . . ? F5SA C2SA S2SA 108.2(10) . . ? F4SA C2SA S2SA 112.9 . . ? O9S S3 O8S 117.2(6) . . ? O9S S3 O7S 114.6(5) . . ? O8S S3 O7S 111.4(5) . . ? O9S S3 C3S 105.2(5) . . ? O8S S3 C3S 103.7(5) . . ? O7S S3 C3S 102.7(5) . . ? S3 O7S Li2 143.0(8) . . ? F9S C3S F7S 106.8(9) . . ? F9S C3S F8S 105.5(11) . . ? F7S C3S F8S 104.9(10) . . ? F9S C3S S3 113.5(8) . . ? F7S C3S S3 114.2(7) . . ? F8S C3S S3 111.2(7) . . ? O6 Li1 O2 150.0(9) . . ? O6 Li1 O4 86.6(7) . . ? O2 Li1 O4 114.8(8) . . ? O6 Li1 O3 115.7(7) . . ? O2 Li1 O3 89.2(7) . . ? O4 Li1 O3 81.9(6) . . ? O6 Li1 O5 83.2(7) . . ? O2 Li1 O5 82.2(6) . . ? O4 Li1 O5 158.6(7) . . ? O3 Li1 O5 85.6(6) . . ? O6 Li1 O1 80.6(6) . . ? O2 Li1 O1 81.9(5) . . ? O4 Li1 O1 81.8(6) . . ? O3 Li1 O1 156.1(9) . . ? O5 Li1 O1 114.8(7) . . ? O7S Li2 O10 113.7(9) . . ? O7S Li2 O7 118.5(9) . . ? O10 Li2 O7 100.5(9) . . ? O7S Li2 O12 121.9(10) . . ? O10 Li2 O12 100.2(8) . . ? O7 Li2 O12 98.4(8) . . ? O11 Li3 O9 103.2(12) . . ? O11 Li3 O8 96.4(9) . . ? O9 Li3 O8 101.1(9) . . ? O11 Li3 O5S 123.4(10) . . ? O9 Li3 O5S 113.8(10) . . ? O8 Li3 O5S 115.6(13) . . ? C2 C1 C6 120.0 . . ? C3 C2 C1 120.0 . . ? C4 C3 C2 120.0 . . ? C3 C4 C5 120.0 . . ? C6 C5 C4 120.0 . . ? C6 C5 C10 120.0 . . ? C4 C5 C10 120.0 . . ? C7 C6 C5 120.0 . . ? C7 C6 C1 120.0 . . ? C5 C6 C1 120.0 . . ? C8 C7 C6 120.0 . . ? C7 C8 C9 120.0 . . ? C7 C8 C21 116.3(5) . . ? C9 C8 C21 123.4(5) . . ? O1 C9 C10 121.8(5) . . ? O1 C9 C8 117.7(5) . . ? C10 C9 C8 120.0 . . ? C9 C10 C5 120.0 . . ? C9 C10 C11 114.9(3) . . ? C5 C10 C11 125.1(3) . . ? C12 C11 C16 120.0 . . ? C12 C11 C10 118.0(3) . . ? C16 C11 C10 121.8(3) . . ? O2 C12 C13 117.8(4) . . ? O2 C12 C11 122.0(4) . . ? C13 C12 C11 120.0 . . ? C12 C13 C14 120.0 . . ? C12 C13 C26 122.3(5) . . ? C14 C13 C26 116.6(5) . . ? C15 C14 C13 120.0 . . ? C14 C15 C16 120.0 . . ? C14 C15 C20 120.0 . . ? C16 C15 C20 120.0 . . ? C17 C16 C15 120.0 . . ? C17 C16 C11 120.0 . . ? C15 C16 C11 120.0 . . ? C18 C17 C16 120.0 . . ? C17 C18 C19 120.0 . . ? C20 C19 C18 120.0 . . ? C19 C20 C15 120.0 . . ? N1 C21 C8 114.3(7) . . ? N1 C22 C23 113.2(10) . . ? C25 C24 N1 114.4(8) . . ? N2 C26 C13 113.0(7) . . ? N2 C27 C28 114.4(8) . . ? N2 C29 C30 115.0(11) . . ? C32 C31 C36 120.0 . . ? C31 C32 C33 120.0 . . ? C34 C33 C32 120.0 . . ? C35 C34 C33 120.0 . . ? C34 C35 C36 120.0 . . ? C34 C35 C40 120.0 . . ? C36 C35 C40 120.0 . . ? C37 C36 C35 120.0 . . ? C37 C36 C31 120.0 . . ? C35 C36 C31 120.0 . . ? C38 C37 C36 120.0 . . ? C39 C38 C37 120.0 . . ? C39 C38 C51 122.2(5) . . ? C37 C38 C51 117.4(5) . . ? O3 C39 C38 118.4(5) . . ? O3 C39 C40 121.1(4) . . ? C38 C39 C40 120.0 . . ? C39 C40 C35 120.0 . . ? C39 C40 C41 116.6(4) . . ? C35 C40 C41 123.0(4) . . ? C42 C41 C46 120.0 . . ? C42 C41 C40 115.8(4) . . ? C46 C41 C40 124.0(4) . . ? O4 C42 C43 117.9(4) . . ? O4 C42 C41 122.1(4) . . ? C43 C42 C41 120.0 . . ? C42 C43 C44 120.0 . . ? C42 C43 C56 122.0(5) . . ? C44 C43 C56 117.7(5) . . ? C45 C44 C43 120.0 . . ? C44 C45 C46 120.0 . . ? C44 C45 C50 120.0 . . ? C46 C45 C50 120.0 . . ? C47 C46 C45 120.0 . . ? C47 C46 C41 120.0 . . ? C45 C46 C41 120.0 . . ? C46 C47 C48 120.0 . . ? C49 C48 C47 120.0 . . ? C50 C49 C48 120.0 . . ? C49 C50 C45 120.0 . . ? C38 C51 N3 115.5(10) . . ? N3 C52 C53 100.8(12) . . ? C55 C54 N3 108.2(16) . . ? C43 C56 N4 113.1(7) . . ? N4 C57 C58 113.0(9) . . ? N4 C59 C60 115.3(9) . . ? C62 C61 C66 120.0 . . ? C63 C62 C61 120.0 . . ? C62 C63 C64 120.0 . . ? C65 C64 C63 120.0 . . ? C64 C65 C66 120.0 . . ? C64 C65 C70 120.0 . . ? C66 C65 C70 120.0 . . ? C67 C66 C65 120.0 . . ? C67 C66 C61 120.0 . . ? C65 C66 C61 120.0 . . ? C68 C67 C66 120.0 . . ? C67 C68 C69 120.0 . . ? C67 C68 C81 117.4(6) . . ? C69 C68 C81 122.4(6) . . ? C70 C69 C68 120.0 . . ? C70 C69 O5 121.1(5) . . ? C68 C69 O5 118.8(5) . . ? C69 C70 C65 120.0 . . ? C69 C70 C71 116.8(4) . . ? C65 C70 C71 122.8(4) . . ? C72 C71 C76 120.0 . . ? C72 C71 C70 117.3(3) . . ? C76 C71 C70 122.7(3) . . ? O6 C72 C71 121.9(4) . . ? O6 C72 C73 117.6(4) . . ? C71 C72 C73 120.0 . . ? C74 C73 C72 120.0 . . ? C74 C73 C86 118.3(4) . . ? C72 C73 C86 121.4(5) . . ? C75 C74 C73 120.0 . . ? C76 C75 C74 120.0 . . ? C76 C75 C80 120.0 . . ? C74 C75 C80 120.0 . . ? C77 C76 C75 120.0 . . ? C77 C76 C71 120.0 . . ? C75 C76 C71 120.0 . . ? C78 C77 C76 120.0 . . ? C77 C78 C79 120.0 . . ? C80 C79 C78 120.0 . . ? C79 C80 C75 120.0 . . ? N5 C81 C68 115.0(7) . . ? N5 C82 C83 113.8(9) . . ? N5 C84 C85 111.2(10) . . ? N6 C86 C73 116.5(8) . . ? C88 C87 N6 115.7(9) . . ? N6 C89 C90 114.5(8) . . ? O7 N1 C22 103.7(7) . . ? O7 N1 C24 108.6(7) . . ? C22 N1 C24 113.4(9) . . ? O7 N1 C21 109.2(7) . . ? C22 N1 C21 111.2(8) . . ? C24 N1 C21 110.4(7) . . ? O8 N2 C27 107.9(8) . . ? O8 N2 C29 103.8(8) . . ? C27 N2 C29 116.9(10) . . ? O8 N2 C26 109.6(8) . . ? C27 N2 C26 108.9(7) . . ? C29 N2 C26 109.6(8) . . ? C52 N3 O9 116.8(11) . . ? C52 N3 C51 118.7(11) . . ? O9 N3 C51 109.9(7) . . ? C52 N3 C54 98.4(11) . . ? O9 N3 C54 104.9(10) . . ? C51 N3 C54 105.8(9) . . ? O10 N4 C59 106.9(7) . . ? O10 N4 C57 108.5(7) . . ? C59 N4 C57 114.0(7) . . ? O10 N4 C56 108.4(7) . . ? C59 N4 C56 109.9(8) . . ? C57 N4 C56 109.0(8) . . ? O11 N5 C84 105.2(7) . . ? O11 N5 C81 107.6(7) . . ? C84 N5 C81 115.6(11) . . ? O11 N5 C82 109.6(10) . . ? C84 N5 C82 107.4(8) . . ? C81 N5 C82 111.2(8) . . ? O12 N6 C89 107.3(7) . . ? O12 N6 C86 108.4(7) . . ? C89 N6 C86 111.1(7) . . ? O12 N6 C87 106.9(7) . . ? C89 N6 C87 113.2(8) . . ? C86 N6 C87 109.8(8) . . ? C9 O1 Li1 116.5(6) . . ? C12 O2 Li1 124.7(6) . . ? C39 O3 Li1 122.0(6) . . ? C42 O4 Li1 122.2(7) . . ? C69 O5 Li1 120.3(6) . . ? C72 O6 Li1 123.6(6) . . ? N1 O7 Li2 135.8(8) . . ? N2 O8 Li3 137.5(9) . . ? N3 O9 Li3 142.2(9) . . ? N4 O10 Li2 136.1(7) . . ? N5 O11 Li3 144.2(9) . . ? N6 O12 Li2 134.0(7) . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 28.43 _diffrn_measured_fraction_theta_full 0.929 _refine_diff_density_max 1.627 _refine_diff_density_min -0.601 _refine_diff_density_rms 0.156