Supplementary Material (ESI) for Perkin Transactions This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 188 _publ_requested_journal 'Perkin Transactions 2' loop_ _publ_author_name 'Chakrabarti, P.' 'Das, T.' 'Pal, D.' 'Praveen, T.' 'Samanta, U.' 'Shashidhar, Mysore S.' 'Sureshan, Kana M.' _publ_contact_author_name 'Dr. M. S. Shashidhar' _publ_contact_author_address ; Organic Chemistry Division(Synthesis) National Chemical Laboratory Pune 411 008 India ; _publ_contact_author_email 'shashi@dalton.ncl.res.in' _publ_contact_author_fax '091(20)5893153' _publ_contact_author_phone '091(20)5893153' _publ_section_title ; Silver(I) oxide - Silver halide Mediated Alcoholysis of O-benzoyl-myo-Inositol 1,3,5-orthoformates: Intramolecular Assistance by the Sulfonyl group. ; data_methylether_6 _database_code_CSD 158621 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'racemic 2,6-di-O-benzoyl-4-O-methyl-myo-inositol-1,3,5-orthoformate' ; _chemical_melting_point '502-503 K' _chemical_formula_moiety 'C22 H20 O8' _chemical_formula_sum 'C22 H20 O8' _chemical_formula_weight 412.38 _chemical_compound_source synthesized loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.442(4) _cell_length_b 14.706(6) _cell_length_c 14.775(6) _cell_angle_alpha 118.136(6) _cell_angle_beta 90.390(7) _cell_angle_gamma 90.057(6) _cell_volume 2000.8(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6498 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 26.032 _exptl_crystal_description 'prism' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.349 _exptl_crystal_size_mid 0.291 _exptl_crystal_size_min 0.246 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 0.105 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_correction_T_min 0.639309 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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_device 'Bruker Smart APEX' _diffrn_measurement_method 'Omega Scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14191 _diffrn_reflns_av_R_equivalents 0.0569 _diffrn_reflns_av_sigmaI/netI 0.0568 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.09 _reflns_number_total 7019 _reflns_number_gt 4650 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _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 full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0606P)^2^+0.6806P] 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 0.0008(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7019 _refine_ls_number_parameters 544 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0952 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.1742 _refine_ls_wR_factor_gt 0.1592 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.005 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8630(3) 0.2971(2) 1.0011(2) 0.0566(7) Uani 1 1 d . . . H1 H 0.7834 0.3065 1.0391 0.068 Uiso 1 1 calc R . . C2 C 0.8333(3) 0.2592(2) 0.8884(2) 0.0540(7) Uani 1 1 d . . . H2 H 0.7943 0.1903 0.8586 0.065 Uiso 1 1 calc R . . C3 C 0.9572(3) 0.2554(2) 0.8343(2) 0.0585(8) Uani 1 1 d . . . H3 H 0.9393 0.2370 0.7625 0.070 Uiso 1 1 calc R . . C4 C 1.0463(3) 0.1755(2) 0.8394(3) 0.0679(9) Uani 1 1 d . . . H4 H 1.1277 0.1760 0.8071 0.081 Uiso 1 1 calc R . . C5 C 1.0707(3) 0.2081(2) 0.9523(3) 0.0642(8) Uani 1 1 d . . . H5 H 1.1293 0.1595 0.9588 0.077 Uiso 1 1 calc R . . C6 C 0.9500(3) 0.2208(2) 1.0154(2) 0.0604(8) Uani 1 1 d . . . H6 H 0.9730 0.2485 1.0880 0.072 Uiso 1 1 calc R . . C7 C 1.0473(3) 0.3809(3) 0.9875(3) 0.0708(9) Uani 1 1 d . . . H7 H 1.0914 0.4478 1.0186 0.085 Uiso 1 1 calc R . . C8 C 0.6225(3) 0.3182(2) 0.8861(2) 0.0600(8) Uani 1 1 d . . . C9 C 0.5429(3) 0.3884(2) 0.8632(2) 0.0595(8) Uani 1 1 d . . . C10 C 0.4123(3) 0.3956(3) 0.8836(3) 0.0798(10) Uani 1 1 d . . . H10 H 0.3765 0.3561 0.9111 0.096 Uiso 1 1 calc R . . C11 C 0.3358(4) 0.4598(4) 0.8640(4) 0.1039(15) Uani 1 1 d . . . H11 H 0.2491 0.4654 0.8798 0.125 Uiso 1 1 calc R . . C12 C 0.3879(5) 0.5162(4) 0.8208(3) 0.1071(16) Uani 1 1 d . . . H12 H 0.3353 0.5585 0.8060 0.129 Uiso 1 1 calc R . . C13 C 0.5169(5) 0.5111(3) 0.7992(3) 0.0941(12) Uani 1 1 d . . . H13 H 0.5511 0.5499 0.7704 0.113 Uiso 1 1 calc R . . C14 C 0.5953(3) 0.4471(3) 0.8210(3) 0.0751(10) Uani 1 1 d . . . H14 H 0.6825 0.4436 0.8075 0.090 Uiso 1 1 calc R . . C15 C 0.8063(3) 0.1086(3) 1.0415(3) 0.0680(9) Uani 1 1 d . . . C16 C 0.7530(3) 0.0017(3) 0.9947(3) 0.0680(9) Uani 1 1 d . . . C17 C 0.6558(4) -0.0201(3) 1.0446(4) 0.0943(13) Uani 1 1 d . . . H17 H 0.6238 0.0317 1.1058 0.113 Uiso 1 1 calc R . . C18 C 0.6058(5) -0.1193(5) 1.0033(6) 0.1240(19) Uani 1 1 d . . . H18 H 0.5400 -0.1333 1.0370 0.149 Uiso 1 1 calc R . . C19 C 0.6512(6) -0.1951(5) 0.9155(6) 0.129(2) Uani 1 1 d . . . H19 H 0.6172 -0.2612 0.8893 0.155 Uiso 1 1 calc R . . C20 C 0.7467(6) -0.1761(3) 0.8642(4) 0.1124(17) Uani 1 1 d . . . H20 H 0.7771 -0.2292 0.8031 0.135 Uiso 1 1 calc R . . C21 C 0.7996(4) -0.0763(3) 0.9036(3) 0.0846(11) Uani 1 1 d . . . H21 H 0.8648 -0.0630 0.8689 0.102 Uiso 1 1 calc R . . C22 C 1.0725(5) -0.0072(3) 0.7583(4) 0.1238(18) Uani 1 1 d . . . H22A H 1.1486 0.0020 0.7274 0.186 Uiso 1 1 calc R . . H22B H 1.0306 -0.0702 0.7112 0.186 Uiso 1 1 calc R . . H22C H 1.0951 -0.0104 0.8198 0.186 Uiso 1 1 calc R . . C1' C 0.3633(3) 0.7028(2) 0.4972(2) 0.0558(7) Uani 1 1 d . . . H1' H 0.2827 0.6942 0.4596 0.067 Uiso 1 1 calc R . . C2' C 0.4515(3) 0.7792(2) 0.4833(2) 0.0605(8) Uani 1 1 d . . . H2' H 0.4722 0.7520 0.4105 0.073 Uiso 1 1 calc R . . C3' C 0.5735(3) 0.7898(2) 0.5446(3) 0.0652(8) Uani 1 1 d . . . H3' H 0.6325 0.8380 0.5378 0.078 Uiso 1 1 calc R . . C4' C 0.5523(3) 0.8226(2) 0.6578(3) 0.0672(9) Uani 1 1 d . . . H4' H 0.6346 0.8206 0.6890 0.081 Uiso 1 1 calc R . . C5' C 0.4614(3) 0.7424(2) 0.6634(2) 0.0602(8) Uani 1 1 d . . . H5' H 0.4457 0.7603 0.7352 0.072 Uiso 1 1 calc R . . C6' C 0.3367(3) 0.7410(2) 0.6102(2) 0.0543(7) Uani 1 1 d . . . H6' H 0.2997 0.8103 0.6407 0.065 Uiso 1 1 calc R . . C7' C 0.5462(3) 0.6166(3) 0.5088(3) 0.0711(9) Uani 1 1 d . . . H7' H 0.5884 0.5493 0.4772 0.085 Uiso 1 1 calc R . . C8' C 0.3076(3) 0.8924(3) 0.4600(3) 0.0644(8) Uani 1 1 d . . . C9' C 0.2563(3) 1.0004(3) 0.5097(3) 0.0665(9) Uani 1 1 d . . . C10' C 0.1565(4) 1.0234(3) 0.4619(4) 0.0908(12) Uani 1 1 d . . . H10' H 0.1222 0.9730 0.4002 0.109 Uiso 1 1 calc R . . C11' C 0.1076(4) 1.1247(4) 0.5082(5) 0.1134(17) Uani 1 1 d . . . H11' H 0.0396 1.1408 0.4773 0.136 Uiso 1 1 calc R . . C12' C 0.1585(6) 1.1985(4) 0.5969(6) 0.125(2) Uani 1 1 d . . . H12' H 0.1261 1.2651 0.6260 0.150 Uiso 1 1 calc R . . C13' C 0.2575(6) 1.1761(3) 0.6444(4) 0.1061(15) Uani 1 1 d . . . H13' H 0.2920 1.2276 0.7053 0.127 Uiso 1 1 calc R . . C14' C 0.3061(4) 1.0775(3) 0.6022(3) 0.0823(11) Uani 1 1 d . . . H14' H 0.3722 1.0624 0.6353 0.099 Uiso 1 1 calc R . . C15' C 0.1250(3) 0.6840(2) 0.6138(2) 0.0594(8) Uani 1 1 d . . . C16' C 0.0443(3) 0.6130(2) 0.6360(2) 0.0592(8) Uani 1 1 d . . . C17' C 0.0950(3) 0.5541(3) 0.6768(3) 0.0769(10) Uani 1 1 d . . . H17' H 0.1826 0.5563 0.6895 0.092 Uiso 1 1 calc R . . C18' C 0.0161(4) 0.4912(3) 0.6996(3) 0.0939(12) Uani 1 1 d . . . H18' H 0.0505 0.4518 0.7278 0.113 Uiso 1 1 calc R . . C19' C -0.1116(5) 0.4881(4) 0.6799(3) 0.1012(15) Uani 1 1 d . . . H19' H -0.1646 0.4465 0.6954 0.121 Uiso 1 1 calc R . . C20' C -0.1633(4) 0.5445(4) 0.6380(4) 0.1026(14) Uani 1 1 d . . . H20' H -0.2507 0.5401 0.6239 0.123 Uiso 1 1 calc R . . C21' C -0.0870(3) 0.6084(3) 0.6162(3) 0.0798(10) Uani 1 1 d . . . H21' H -0.1228 0.6479 0.5887 0.096 Uiso 1 1 calc R . . C22' C 0.5873(5) 1.0035(3) 0.7372(4) 0.1211(18) Uani 1 1 d . . . H22D H 0.6654 0.9913 0.7643 0.182 Uiso 1 1 calc R . . H22E H 0.5510 1.0677 0.7866 0.182 Uiso 1 1 calc R . . H22F H 0.6049 1.0065 0.6751 0.182 Uiso 1 1 calc R . . O1 O 0.9327(2) 0.39336(15) 1.04193(17) 0.0651(6) Uani 1 1 d . . . O2 O 0.74854(18) 0.32980(15) 0.87491(16) 0.0575(5) Uani 1 1 d . . . O3 O 1.0218(2) 0.35439(17) 0.88468(19) 0.0692(6) Uani 1 1 d . . . O4 O 0.9881(3) 0.07755(17) 0.78295(18) 0.0831(7) Uani 1 1 d . . . O5 O 1.1293(2) 0.31017(18) 0.9968(2) 0.0775(7) Uani 1 1 d . . . O6 O 0.8901(2) 0.12062(15) 0.97847(16) 0.0651(6) Uani 1 1 d . . . O7 O 0.5805(2) 0.25590(18) 0.9099(2) 0.0892(8) Uani 1 1 d . . . O8 O 0.7792(3) 0.1769(2) 1.1241(2) 0.1041(9) Uani 1 1 d . . . O1' O 0.4310(2) 0.60630(15) 0.45574(17) 0.0666(6) Uani 1 1 d . . . O2' O 0.3929(2) 0.87991(15) 0.52146(16) 0.0662(6) Uani 1 1 d . . . O3' O 0.6296(2) 0.68798(18) 0.4995(2) 0.0757(7) Uani 1 1 d . . . O4' O 0.4981(3) 0.92109(17) 0.71594(17) 0.0824(7) Uani 1 1 d . . . O5' O 0.5236(2) 0.64366(17) 0.61167(19) 0.0684(6) Uani 1 1 d . . . O6' O 0.25103(18) 0.67044(15) 0.62368(16) 0.0567(5) Uani 1 1 d . . . O7' O 0.2775(3) 0.8257(2) 0.3772(2) 0.1008(9) Uani 1 1 d . . . O8' O 0.0849(2) 0.74557(18) 0.5888(2) 0.0874(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0602(19) 0.0428(16) 0.066(2) 0.0254(15) 0.0093(15) 0.0019(13) C2 0.0565(18) 0.0397(15) 0.068(2) 0.0271(14) 0.0031(14) 0.0029(13) C3 0.066(2) 0.0511(18) 0.0631(19) 0.0307(15) 0.0079(15) 0.0072(15) C4 0.072(2) 0.061(2) 0.077(2) 0.0379(18) 0.0206(17) 0.0188(17) C5 0.066(2) 0.0514(18) 0.081(2) 0.0359(17) 0.0030(17) 0.0126(15) C6 0.079(2) 0.0459(17) 0.0597(19) 0.0276(15) 0.0044(16) 0.0064(15) C7 0.060(2) 0.058(2) 0.099(3) 0.042(2) -0.0104(19) -0.0058(16) C8 0.0538(19) 0.0451(17) 0.066(2) 0.0136(15) 0.0015(15) -0.0072(14) C9 0.0507(18) 0.0513(17) 0.0562(18) 0.0086(15) -0.0045(14) -0.0001(14) C10 0.054(2) 0.075(2) 0.082(2) 0.014(2) -0.0017(18) -0.0020(18) C11 0.055(2) 0.117(4) 0.097(3) 0.016(3) -0.005(2) 0.021(2) C12 0.096(4) 0.116(4) 0.078(3) 0.019(3) -0.012(2) 0.053(3) C13 0.109(3) 0.095(3) 0.079(3) 0.042(2) 0.004(2) 0.031(3) C14 0.066(2) 0.081(2) 0.082(2) 0.043(2) 0.0099(18) 0.0160(18) C15 0.088(2) 0.060(2) 0.062(2) 0.0328(18) 0.0116(18) 0.0056(18) C16 0.077(2) 0.061(2) 0.081(2) 0.046(2) -0.0108(18) -0.0029(17) C17 0.078(3) 0.085(3) 0.138(4) 0.068(3) 0.009(3) 0.001(2) C18 0.096(4) 0.103(4) 0.204(6) 0.098(4) -0.012(4) -0.025(3) C19 0.131(5) 0.089(4) 0.194(7) 0.089(4) -0.076(5) -0.047(3) C20 0.170(5) 0.063(3) 0.099(3) 0.034(2) -0.057(3) -0.014(3) C21 0.126(3) 0.062(2) 0.068(2) 0.033(2) -0.022(2) -0.007(2) C22 0.174(5) 0.071(3) 0.126(4) 0.045(3) 0.051(4) 0.054(3) C1' 0.0629(19) 0.0427(16) 0.0614(19) 0.0242(14) -0.0077(15) -0.0096(14) C2' 0.082(2) 0.0430(16) 0.0575(18) 0.0245(14) -0.0033(16) -0.0081(15) C3' 0.069(2) 0.0529(19) 0.082(2) 0.0386(17) -0.0017(17) -0.0134(15) C4' 0.077(2) 0.058(2) 0.074(2) 0.0367(18) -0.0235(17) -0.0243(16) C5' 0.069(2) 0.0541(18) 0.0633(19) 0.0325(16) -0.0080(16) -0.0097(15) C6' 0.0613(18) 0.0373(15) 0.0647(19) 0.0243(14) -0.0010(14) -0.0056(13) C7' 0.061(2) 0.056(2) 0.102(3) 0.042(2) 0.0058(19) -0.0027(16) C8' 0.085(2) 0.058(2) 0.058(2) 0.0335(18) -0.0061(17) -0.0099(17) C9' 0.076(2) 0.062(2) 0.075(2) 0.0434(19) 0.0084(18) -0.0050(17) C10' 0.081(3) 0.084(3) 0.125(4) 0.064(3) 0.000(2) -0.006(2) C11' 0.083(3) 0.105(4) 0.187(6) 0.098(4) 0.029(3) 0.028(3) C12' 0.126(5) 0.075(3) 0.169(6) 0.053(4) 0.071(4) 0.017(3) C13' 0.148(5) 0.063(3) 0.097(3) 0.029(2) 0.041(3) 0.001(3) C14' 0.116(3) 0.061(2) 0.069(2) 0.0304(19) 0.017(2) -0.001(2) C15' 0.0579(19) 0.0477(17) 0.0617(19) 0.0168(15) 0.0006(15) 0.0085(14) C16' 0.0514(18) 0.0520(18) 0.0560(18) 0.0105(15) 0.0061(14) 0.0000(14) C17' 0.064(2) 0.088(3) 0.086(3) 0.047(2) -0.0097(18) -0.0223(19) C18' 0.098(3) 0.095(3) 0.096(3) 0.051(2) -0.004(2) -0.033(2) C19' 0.094(3) 0.106(4) 0.080(3) 0.024(3) 0.017(2) -0.043(3) C20' 0.056(2) 0.114(4) 0.102(3) 0.021(3) 0.009(2) -0.023(2) C21' 0.052(2) 0.076(2) 0.086(3) 0.017(2) 0.0056(18) 0.0048(18) C22' 0.185(5) 0.070(3) 0.107(3) 0.041(2) -0.047(3) -0.062(3) O1 0.0705(14) 0.0429(11) 0.0765(15) 0.0236(11) -0.0044(11) 0.0012(10) O2 0.0478(12) 0.0498(11) 0.0795(14) 0.0343(11) 0.0003(10) -0.0002(9) O3 0.0640(14) 0.0627(14) 0.0975(18) 0.0515(13) 0.0045(12) -0.0006(11) O4 0.119(2) 0.0520(14) 0.0722(15) 0.0242(12) 0.0181(14) 0.0237(13) O5 0.0644(14) 0.0688(15) 0.1096(19) 0.0507(14) -0.0104(13) 0.0007(11) O6 0.0926(16) 0.0470(12) 0.0607(13) 0.0295(10) 0.0094(11) 0.0025(11) O7 0.0772(17) 0.0636(15) 0.134(2) 0.0519(16) 0.0142(15) -0.0141(12) O8 0.145(3) 0.0756(18) 0.0820(19) 0.0287(16) 0.0402(18) -0.0054(17) O1' 0.0733(15) 0.0434(12) 0.0770(15) 0.0233(11) 0.0056(12) -0.0056(10) O2' 0.0937(16) 0.0473(12) 0.0623(13) 0.0299(11) -0.0106(12) -0.0085(11) O3' 0.0652(14) 0.0665(15) 0.1036(18) 0.0469(14) 0.0106(12) -0.0061(11) O4' 0.123(2) 0.0506(13) 0.0651(14) 0.0204(11) -0.0157(13) -0.0293(13) O5' 0.0655(14) 0.0606(14) 0.0947(18) 0.0495(13) -0.0034(12) -0.0035(11) O6' 0.0496(12) 0.0484(11) 0.0774(14) 0.0342(11) 0.0016(10) -0.0023(9) O7' 0.142(3) 0.0713(17) 0.0742(18) 0.0228(15) -0.0366(17) 0.0018(16) O8' 0.0773(17) 0.0666(16) 0.123(2) 0.0486(16) -0.0088(15) 0.0141(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.444(3) . ? C1 C2 1.515(4) . ? C1 C6 1.533(4) . ? C2 O2 1.448(3) . ? C2 C3 1.512(4) . ? C3 O3 1.449(4) . ? C3 C4 1.528(4) . ? C4 O4 1.413(4) . ? C4 C5 1.522(5) . ? C5 O5 1.456(4) . ? C5 C6 1.532(4) . ? C6 O6 1.447(4) . ? C7 O5 1.403(4) . ? C7 O3 1.403(4) . ? C7 O1 1.409(4) . ? C8 O7 1.210(4) . ? C8 O2 1.348(4) . ? C8 C9 1.483(4) . ? C9 C10 1.393(4) . ? C9 C14 1.394(5) . ? C10 C11 1.367(6) . ? C11 C12 1.376(7) . ? C12 C13 1.380(6) . ? C13 C14 1.395(5) . ? C15 O8 1.195(4) . ? C15 O6 1.353(4) . ? C15 C16 1.492(5) . ? C16 C17 1.382(5) . ? C16 C21 1.385(5) . ? C17 C18 1.388(6) . ? C18 C19 1.340(8) . ? C19 C20 1.362(8) . ? C20 C21 1.410(6) . ? C22 O4 1.429(4) . ? C1' O1' 1.442(3) . ? C1' C6' 1.518(4) . ? C1' C2' 1.539(4) . ? C2' O2' 1.451(3) . ? C2' C3' 1.522(4) . ? C3' O3' 1.447(4) . ? C3' C4' 1.525(5) . ? C4' O4' 1.410(4) . ? C4' C5' 1.545(4) . ? C5' O5' 1.441(4) . ? C5' C6' 1.511(4) . ? C6' O6' 1.454(3) . ? C7' O5' 1.400(4) . ? C7' O1' 1.400(4) . ? C7' O3' 1.419(4) . ? C8' O7' 1.192(4) . ? C8' O2' 1.342(4) . ? C8' C9' 1.501(5) . ? C9' C10' 1.385(5) . ? C9' C14' 1.397(5) . ? C10' C11' 1.411(6) . ? C11' C12' 1.352(8) . ? C12' C13' 1.370(7) . ? C13' C14' 1.379(5) . ? C15' O8' 1.204(3) . ? C15' O6' 1.349(4) . ? C15' C16' 1.494(4) . ? C16' C17' 1.372(5) . ? C16' C21' 1.394(4) . ? C17' C18' 1.395(5) . ? C18' C19' 1.359(6) . ? C19' C20' 1.358(6) . ? C20' C21' 1.382(6) . ? C22' O4' 1.438(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 109.8(2) . . ? O1 C1 C6 106.5(2) . . ? C2 C1 C6 110.7(2) . . ? O2 C2 C3 107.6(2) . . ? O2 C2 C1 110.8(2) . . ? C3 C2 C1 108.3(3) . . ? O3 C3 C2 110.3(2) . . ? O3 C3 C4 107.7(3) . . ? C2 C3 C4 109.6(2) . . ? O4 C4 C5 115.0(3) . . ? O4 C4 C3 107.8(3) . . ? C5 C4 C3 107.4(3) . . ? O5 C5 C4 106.7(2) . . ? O5 C5 C6 105.4(2) . . ? C4 C5 C6 114.8(3) . . ? O6 C6 C5 108.4(2) . . ? O6 C6 C1 112.0(3) . . ? C5 C6 C1 107.0(2) . . ? O5 C7 O3 112.2(3) . . ? O5 C7 O1 111.6(3) . . ? O3 C7 O1 110.9(3) . . ? O7 C8 O2 123.3(3) . . ? O7 C8 C9 124.6(3) . . ? O2 C8 C9 112.2(3) . . ? C10 C9 C14 119.0(3) . . ? C10 C9 C8 119.3(3) . . ? C14 C9 C8 121.7(3) . . ? C11 C10 C9 121.0(4) . . ? C10 C11 C12 119.6(4) . . ? C11 C12 C13 121.2(4) . . ? C12 C13 C14 119.2(4) . . ? C9 C14 C13 120.0(3) . . ? O8 C15 O6 122.8(3) . . ? O8 C15 C16 125.3(3) . . ? O6 C15 C16 111.9(3) . . ? C17 C16 C21 119.3(4) . . ? C17 C16 C15 118.9(4) . . ? C21 C16 C15 121.8(3) . . ? C16 C17 C18 120.0(5) . . ? C19 C18 C17 120.9(5) . . ? C18 C19 C20 120.6(5) . . ? C19 C20 C21 120.1(5) . . ? C16 C21 C20 119.1(4) . . ? O1' C1' C6' 110.0(2) . . ? O1' C1' C2' 106.3(2) . . ? C6' C1' C2' 110.3(2) . . ? O2' C2' C3' 108.9(2) . . ? O2' C2' C1' 111.6(3) . . ? C3' C2' C1' 107.2(2) . . ? O3' C3' C2' 105.8(3) . . ? O3' C3' C4' 106.9(2) . . ? C2' C3' C4' 114.5(3) . . ? O4' C4' C3' 115.7(3) . . ? O4' C4' C5' 108.0(3) . . ? C3' C4' C5' 107.3(2) . . ? O5' C5' C6' 110.6(2) . . ? O5' C5' C4' 107.2(3) . . ? C6' C5' C4' 108.8(2) . . ? O6' C6' C5' 107.0(2) . . ? O6' C6' C1' 110.5(2) . . ? C5' C6' C1' 108.4(3) . . ? O5' C7' O1' 110.9(3) . . ? O5' C7' O3' 111.6(3) . . ? O1' C7' O3' 111.1(3) . . ? O7' C8' O2' 123.6(3) . . ? O7' C8' C9' 125.4(3) . . ? O2' C8' C9' 111.0(3) . . ? C10' C9' C14' 119.4(4) . . ? C10' C9' C8' 118.5(3) . . ? C14' C9' C8' 122.1(3) . . ? C9' C10' C11' 118.9(5) . . ? C12' C11' C10' 120.7(5) . . ? C11' C12' C13' 120.6(5) . . ? C12' C13' C14' 120.2(5) . . ? C13' C14' C9' 120.2(4) . . ? O8' C15' O6' 122.8(3) . . ? O8' C15' C16' 125.2(3) . . ? O6' C15' C16' 111.9(3) . . ? C17' C16' C21' 119.4(3) . . ? C17' C16' C15' 122.1(3) . . ? C21' C16' C15' 118.6(3) . . ? C16' C17' C18' 120.5(4) . . ? C19' C18' C17' 119.2(4) . . ? C20' C19' C18' 121.2(4) . . ? C19' C20' C21' 120.5(4) . . ? C20' C21' C16' 119.3(4) . . ? C7 O1 C1 110.5(2) . . ? C8 O2 C2 116.1(2) . . ? C7 O3 C3 109.8(2) . . ? C4 O4 C22 114.3(3) . . ? C7 O5 C5 110.8(2) . . ? C15 O6 C6 117.4(2) . . ? C7' O1' C1' 111.1(2) . . ? C8' O2' C2' 117.3(2) . . ? C7' O3' C3' 110.9(2) . . ? C4' O4' C22' 112.9(3) . . ? C7' O5' C5' 110.8(2) . . ? C15' O6' C6' 115.8(2) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.182 _refine_diff_density_min -0.170 _refine_diff_density_rms 0.043 #===END data_mesylate_8 _database_code_CSD 158622 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'racemic 2,6-di-O-benzoyl-4-O-methanesulfonyl-myo-inositol-1,3,5-orthoformate' ; _chemical_melting_point '434-435 K' _chemical_formula_moiety 'C22 H20 O10 S' _chemical_formula_sum 'C22 H20 O10 S' _chemical_formula_weight 476.44 _chemical_compound_source synthesized 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.860(3) _cell_length_b 11.530(4) _cell_length_c 12.079(4) _cell_angle_alpha 109.205(5) _cell_angle_beta 105.285(5) _cell_angle_gamma 102.015(5) _cell_volume 1063.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6921 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 27.78 _exptl_crystal_description 'Prism ' _exptl_crystal_colour 'Colourless' _exptl_crystal_size_max 0.506 _exptl_crystal_size_mid 0.438 _exptl_crystal_size_min 0.131 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 0.211 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_correction_T_min 0.774924 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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_device 'Bruker Smart APEX' _diffrn_measurement_method 'Omega Scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11503 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 27.78 _reflns_number_total 4533 _reflns_number_gt 3863 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _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 full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0897P)^2^+0.2684P] 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 0.003(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4533 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0594 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1564 _refine_ls_wR_factor_gt 0.1495 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.29427(6) 0.58066(4) 0.48624(5) 0.05283(19) Uani 1 1 d . . . O1 O 0.81687(17) 0.98926(14) 0.94983(12) 0.0589(4) Uani 1 1 d . . . O2 O 0.87318(15) 0.74132(13) 0.86472(11) 0.0462(3) Uani 1 1 d . . . O3 O 0.59874(17) 0.81360(17) 0.90981(13) 0.0622(4) Uani 1 1 d . . . O4 O 0.45157(15) 0.70671(13) 0.56689(12) 0.0495(3) Uani 1 1 d . . . O5 O 0.5481(2) 0.98397(17) 0.86023(14) 0.0688(5) Uani 1 1 d . . . O6 O 0.73320(18) 0.90748(13) 0.61857(13) 0.0545(3) Uani 1 1 d . . . O7 O 1.0469(2) 0.74292(18) 0.75887(15) 0.0667(4) Uani 1 1 d . . . O8 O 0.7328(4) 1.0792(2) 0.5719(2) 0.1094(8) Uani 1 1 d . . . O9 O 0.3194(2) 0.52376(17) 0.37240(17) 0.0793(5) Uani 1 1 d . . . O10 O 0.2729(2) 0.50927(17) 0.56040(19) 0.0798(5) Uani 1 1 d . . . C1 C 0.8294(2) 0.92973(17) 0.82913(17) 0.0472(4) Uani 1 1 d . . . H1 H 0.9444 0.9600 0.8352 0.057 Uiso 1 1 calc R . . C2 C 0.7697(2) 0.78226(17) 0.78232(16) 0.0415(4) Uani 1 1 d . . . H2 H 0.7675 0.7415 0.6965 0.050 Uiso 1 1 calc R . . C3 C 0.5970(2) 0.74156(19) 0.78625(17) 0.0482(4) Uani 1 1 d . . . H3 H 0.5581 0.6481 0.7645 0.058 Uiso 1 1 calc R . . C4 C 0.4757(2) 0.77766(19) 0.69756(17) 0.0483(4) Uani 1 1 d . . . H4 H 0.3689 0.7580 0.7085 0.058 Uiso 1 1 calc R . . C5 C 0.5432(3) 0.9227(2) 0.73354(18) 0.0530(5) Uani 1 1 d . . . H5 H 0.4693 0.9484 0.6771 0.064 Uiso 1 1 calc R . . C6 C 0.7198(3) 0.96934(18) 0.73768(19) 0.0523(4) Uani 1 1 d . . . H6 H 0.7579 1.0638 0.7655 0.063 Uiso 1 1 calc R . . C7 C 0.6546(3) 0.9479(2) 0.9431(2) 0.0648(6) Uani 1 1 d . . . H7 H 0.6526 0.9913 1.0272 0.078 Uiso 1 1 calc R . . C8 C 1.0107(2) 0.72554(17) 0.84257(17) 0.0459(4) Uani 1 1 d . . . C9 C 1.1100(2) 0.68629(17) 0.93504(17) 0.0460(4) Uani 1 1 d . . . C10 C 1.2491(3) 0.6585(3) 0.9207(3) 0.0811(8) Uani 1 1 d . . . H10 H 1.2769 0.6611 0.8523 0.097 Uiso 1 1 calc R . . C11 C 1.3477(4) 0.6266(4) 1.0081(4) 0.1017(11) Uani 1 1 d . . . H11 H 1.4422 0.6086 0.9984 0.122 Uiso 1 1 calc R . . C12 C 1.3081(3) 0.6211(3) 1.1081(3) 0.0812(8) Uani 1 1 d . . . H12 H 1.3750 0.5996 1.1664 0.097 Uiso 1 1 calc R . . C13 C 1.1697(4) 0.6473(3) 1.1222(2) 0.0812(8) Uani 1 1 d . . . H13 H 1.1417 0.6432 1.1901 0.097 Uiso 1 1 calc R . . C14 C 1.0706(3) 0.6799(3) 1.0359(2) 0.0677(6) Uani 1 1 d . . . H14 H 0.9763 0.6977 1.0463 0.081 Uiso 1 1 calc R . . C15 C 0.7415(3) 0.9719(2) 0.5450(2) 0.0627(6) Uani 1 1 d . . . C16 C 0.7585(3) 0.8915(3) 0.4277(2) 0.0673(6) Uani 1 1 d . . . C17 C 0.7337(3) 0.7593(3) 0.3930(2) 0.0722(6) Uani 1 1 d . . . H17 H 0.7086 0.7209 0.4454 0.087 Uiso 1 1 calc R . . C18 C 0.7457(4) 0.6838(4) 0.2813(3) 0.0971(10) Uani 1 1 d . . . H18 H 0.7310 0.5960 0.2605 0.117 Uiso 1 1 calc R . . C19 C 0.7787(5) 0.7371(6) 0.2034(4) 0.1253(16) Uani 1 1 d . . . H19 H 0.7823 0.6851 0.1275 0.150 Uiso 1 1 calc R . . C20 C 0.8073(4) 0.8689(6) 0.2348(4) 0.1296(19) Uani 1 1 d . . . H20 H 0.8334 0.9047 0.1808 0.156 Uiso 1 1 calc R . . C21 C 0.7970(3) 0.9499(4) 0.3491(3) 0.1015(12) Uani 1 1 d . . . H21 H 0.8152 1.0382 0.3706 0.122 Uiso 1 1 calc R . . C22 C 0.1297(3) 0.6411(2) 0.4593(2) 0.0655(6) Uani 1 1 d . . . H22A H 0.1538 0.7048 0.4260 0.098 Uiso 1 1 calc R . . H22B H 0.1136 0.6805 0.5369 0.098 Uiso 1 1 calc R . . H22C H 0.0309 0.5714 0.4001 0.098 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0483(3) 0.0404(3) 0.0536(3) 0.0156(2) 0.0036(2) 0.00731(19) O1 0.0496(8) 0.0588(8) 0.0444(7) 0.0025(6) 0.0049(6) 0.0164(6) O2 0.0422(7) 0.0540(7) 0.0432(7) 0.0213(6) 0.0131(5) 0.0176(5) O3 0.0476(8) 0.0916(11) 0.0452(7) 0.0271(7) 0.0176(6) 0.0185(7) O4 0.0417(7) 0.0493(7) 0.0422(7) 0.0110(6) 0.0082(5) 0.0061(5) O5 0.0617(9) 0.0812(11) 0.0499(8) 0.0065(7) 0.0122(7) 0.0397(8) O6 0.0649(8) 0.0461(7) 0.0557(8) 0.0266(6) 0.0206(7) 0.0159(6) O7 0.0648(9) 0.0978(12) 0.0640(9) 0.0465(9) 0.0347(8) 0.0408(9) O8 0.158(2) 0.0729(12) 0.1276(18) 0.0685(13) 0.0526(17) 0.0489(14) O9 0.0791(11) 0.0598(9) 0.0658(10) -0.0003(8) 0.0158(9) 0.0129(8) O10 0.0723(11) 0.0615(9) 0.0971(13) 0.0475(9) 0.0074(9) 0.0097(8) C1 0.0401(9) 0.0425(9) 0.0471(10) 0.0115(7) 0.0097(7) 0.0088(7) C2 0.0391(8) 0.0442(9) 0.0378(8) 0.0157(7) 0.0102(7) 0.0127(7) C3 0.0401(9) 0.0543(10) 0.0450(9) 0.0208(8) 0.0115(7) 0.0088(7) C4 0.0364(8) 0.0582(11) 0.0409(9) 0.0154(8) 0.0090(7) 0.0112(7) C5 0.0524(10) 0.0533(11) 0.0455(10) 0.0124(8) 0.0097(8) 0.0244(9) C6 0.0552(11) 0.0366(9) 0.0535(10) 0.0135(8) 0.0101(8) 0.0117(8) C7 0.0551(12) 0.0827(16) 0.0431(10) 0.0090(10) 0.0128(9) 0.0296(11) C8 0.0440(9) 0.0457(9) 0.0451(9) 0.0157(7) 0.0150(8) 0.0145(7) C9 0.0449(9) 0.0404(9) 0.0463(9) 0.0144(7) 0.0115(7) 0.0127(7) C10 0.0627(14) 0.123(2) 0.0957(19) 0.0699(18) 0.0390(14) 0.0498(16) C11 0.0675(17) 0.154(3) 0.126(3) 0.089(3) 0.0374(18) 0.063(2) C12 0.0734(16) 0.0814(17) 0.0797(17) 0.0418(14) 0.0010(13) 0.0269(13) C13 0.101(2) 0.0947(19) 0.0592(14) 0.0414(13) 0.0238(13) 0.0434(16) C14 0.0763(15) 0.0842(16) 0.0604(13) 0.0362(12) 0.0300(11) 0.0430(13) C15 0.0550(11) 0.0635(13) 0.0792(15) 0.0477(12) 0.0171(10) 0.0163(10) C16 0.0465(11) 0.1054(19) 0.0720(14) 0.0616(14) 0.0207(10) 0.0268(11) C17 0.0740(15) 0.0968(19) 0.0606(13) 0.0418(13) 0.0279(12) 0.0363(14) C18 0.089(2) 0.142(3) 0.0681(16) 0.0387(18) 0.0367(16) 0.049(2) C19 0.085(2) 0.225(6) 0.085(2) 0.076(3) 0.0465(19) 0.047(3) C20 0.0691(19) 0.265(6) 0.111(3) 0.138(4) 0.0471(19) 0.045(3) C21 0.0584(15) 0.170(3) 0.128(3) 0.119(3) 0.0370(16) 0.0375(18) C22 0.0464(11) 0.0686(13) 0.0723(14) 0.0348(11) 0.0035(10) 0.0135(10) _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 O9 1.4139(19) . ? S1 O10 1.4231(18) . ? S1 O4 1.5853(13) . ? S1 C22 1.744(2) . ? O1 C7 1.389(3) . ? O1 C1 1.438(2) . ? O2 C8 1.349(2) . ? O2 C2 1.436(2) . ? O3 C7 1.404(3) . ? O3 C3 1.444(2) . ? O4 C4 1.451(2) . ? O5 C7 1.416(3) . ? O5 C5 1.443(2) . ? O6 C15 1.339(2) . ? O6 C6 1.429(2) . ? O7 C8 1.201(2) . ? O8 C15 1.196(3) . ? C1 C6 1.524(3) . ? C1 C2 1.525(3) . ? C2 C3 1.522(2) . ? C3 C4 1.533(3) . ? C4 C5 1.521(3) . ? C5 C6 1.527(3) . ? C8 C9 1.486(3) . ? C9 C14 1.372(3) . ? C9 C10 1.376(3) . ? C10 C11 1.385(4) . ? C11 C12 1.360(4) . ? C12 C13 1.361(4) . ? C13 C14 1.383(3) . ? C15 C16 1.482(4) . ? C16 C17 1.392(4) . ? C16 C21 1.404(3) . ? C17 C18 1.390(4) . ? C18 C19 1.340(6) . ? C19 C20 1.388(7) . ? C20 C21 1.429(6) . ? 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 O9 S1 O10 120.51(12) . . ? O9 S1 O4 104.06(10) . . ? O10 S1 O4 109.04(9) . . ? O9 S1 C22 109.66(12) . . ? O10 S1 C22 108.28(12) . . ? O4 S1 C22 104.04(10) . . ? C7 O1 C1 110.71(14) . . ? C8 O2 C2 116.13(14) . . ? C7 O3 C3 111.34(15) . . ? C4 O4 S1 117.75(11) . . ? C7 O5 C5 110.92(14) . . ? C15 O6 C6 119.73(17) . . ? O1 C1 C6 107.76(15) . . ? O1 C1 C2 110.47(15) . . ? C6 C1 C2 109.18(15) . . ? O2 C2 C3 107.11(14) . . ? O2 C2 C1 110.64(14) . . ? C3 C2 C1 107.67(15) . . ? O3 C3 C2 109.76(14) . . ? O3 C3 C4 104.90(15) . . ? C2 C3 C4 110.98(15) . . ? O4 C4 C5 109.80(15) . . ? O4 C4 C3 112.08(15) . . ? C5 C4 C3 108.33(15) . . ? O5 C5 C4 105.33(17) . . ? O5 C5 C6 106.46(16) . . ? C4 C5 C6 114.23(15) . . ? O6 C6 C1 106.43(15) . . ? O6 C6 C5 111.71(15) . . ? C1 C6 C5 107.84(17) . . ? O1 C7 O3 111.11(17) . . ? O1 C7 O5 111.6(2) . . ? O3 C7 O5 111.25(18) . . ? O7 C8 O2 123.35(17) . . ? O7 C8 C9 125.18(17) . . ? O2 C8 C9 111.47(15) . . ? C14 C9 C10 118.8(2) . . ? C14 C9 C8 122.52(17) . . ? C10 C9 C8 118.66(19) . . ? C9 C10 C11 120.0(2) . . ? C12 C11 C10 120.8(2) . . ? C11 C12 C13 119.5(2) . . ? C12 C13 C14 120.3(3) . . ? C9 C14 C13 120.6(2) . . ? O8 C15 O6 123.1(2) . . ? O8 C15 C16 125.9(2) . . ? O6 C15 C16 110.99(19) . . ? C17 C16 C21 119.6(3) . . ? C17 C16 C15 121.45(19) . . ? C21 C16 C15 119.0(3) . . ? C18 C17 C16 121.2(3) . . ? C19 C18 C17 120.2(4) . . ? C18 C19 C20 120.9(4) . . ? C19 C20 C21 120.6(3) . . ? C16 C21 C20 117.5(4) . . ? _diffrn_measured_fraction_theta_max 0.906 _diffrn_reflns_theta_full 27.78 _diffrn_measured_fraction_theta_full 0.906 _refine_diff_density_max 0.381 _refine_diff_density_min -0.440 _refine_diff_density_rms 0.060 #===END