Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Bhadbhade, Mohan M.' 'Gonnade, Rajesh G.' 'Puranik, Vedavati G.' 'Shashidhar, Mysore S.' 'Sureshan, Kana M.' _publ_contact_author_name 'Dr Mohan M Bhadbhade' _publ_contact_author_address ; Dr Mohan M Bhadbhade Physical Chemistry Division National Chemical Laboratory Dr Homi Bhabha Road Pashan Pune 411 008 INDIA ; _publ_contact_author_email ? _publ_contact_author_email mohanb@sil.ncl.res.in _publ_contact_author_fax '91 20 5893044' _publ_contact_author_phone '91 20 5893300' data_3 _audit_creation_method 'SHELXL-97' _chemical_name_systematic ; 1,2,3,4,5-penta-o-benzoyl-6-o-tosyl myo-inositol-dichloromethane ; _chemical_name_common 'myo-inositol' _chemical_formula_moiety 'C48.25 H38.50 Cl0.50 O13 S' _chemical_formula_sum 'C48.25 H38.50 Cl0.50 O13 S' _chemical_formula_weight 876.08 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'C2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.771(4) _cell_length_b 11.608(3) _cell_length_c 30.783(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.176(6) _cell_angle_gamma 90.00 _cell_volume 9232(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2268 _cell_measurement_theta_min 1.58 _cell_measurement_theta_max 23.25 _exptl_crystal_description blocks _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.261 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3652 _exptl_absorpt_coefficient_mu 0.162 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 0.97 _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_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22898 _diffrn_reflns_av_R_equivalents 0.0874 _diffrn_reflns_av_sigmaI/netI 0.0966 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 23.25 _reflns_number_total 6618 _reflns_number_gt 2756 _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 'ORTEP32 and PLATON-97' _computing_publication_material 'SHELX-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0732P)^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 0.00021(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6618 _refine_ls_number_parameters 575 _refine_ls_number_restraints 384 _refine_ls_R_factor_all 0.1480 _refine_ls_R_factor_gt 0.0556 _refine_ls_wR_factor_ref 0.1611 _refine_ls_wR_factor_gt 0.1274 _refine_ls_goodness_of_fit_ref 0.874 _refine_ls_restrained_S_all 0.849 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.04734(16) 0.4603(3) 0.23842(15) 0.1618(15) Uani 0.50 d PU . . S1 S 0.17652(5) 0.65583(12) 0.05862(5) 0.0802(4) Uani 1 d U . . O1 O -0.05732(10) 0.7388(2) 0.10358(9) 0.0638(8) Uani 1 d U . . O2 O -0.07042(12) 0.5872(3) 0.14441(12) 0.0918(11) Uani 1 d U . . O3 O 0.04749(9) 0.7907(2) 0.13787(9) 0.0583(7) Uani 1 d U . . O4 O 0.0470(2) 0.7650(3) 0.20883(13) 0.165(2) Uani 1 d U . . O5 O 0.12157(10) 0.6189(2) 0.14492(9) 0.0632(8) Uani 1 d U . . O6 O 0.10728(18) 0.4484(4) 0.16994(17) 0.196(3) Uani 1 d U . . O7 O 0.11994(10) 0.6058(2) 0.05405(10) 0.0700(8) Uani 1 d U . . O8 O 0.21090(13) 0.5711(3) 0.08204(13) 0.1150(13) Uani 1 d U . . O9 O 0.17927(11) 0.7699(3) 0.07603(11) 0.0942(11) Uani 1 d U . . O10 O 0.04085(10) 0.7325(2) -0.00509(9) 0.0611(8) Uani 1 d U . . O11 O 0.01452(13) 0.5799(3) -0.05002(10) 0.0887(10) Uani 1 d U . . O12 O -0.05635(10) 0.7306(2) 0.01283(9) 0.0637(8) Uani 1 d U . . O13 O -0.05515(17) 0.9212(3) 0.00882(15) 0.163(2) Uani 1 d U . . C1 C -0.01848(14) 0.6744(3) 0.08962(13) 0.0526(11) Uani 1 d U . . H1 H -0.0306 0.5954 0.0820 0.063 Uiso 1 calc R . . C2 C 0.03154(15) 0.6727(3) 0.12735(13) 0.0549(11) Uani 1 d U . . H2 H 0.0261 0.6337 0.1540 0.066 Uiso 1 calc R . . C3 C 0.07395(14) 0.6124(3) 0.11111(13) 0.0526(11) Uani 1 d U . . H3 H 0.0645 0.5316 0.1043 0.063 Uiso 1 calc R . . C4 C 0.08214(15) 0.6714(3) 0.06972(14) 0.0542(11) Uani 1 d U . . H4 H 0.0944 0.7504 0.0770 0.065 Uiso 1 calc R . . C5 C 0.03215(15) 0.6718(3) 0.03279(13) 0.0554(11) Uani 1 d U . . H5 H 0.0214 0.5925 0.0242 0.066 Uiso 1 calc R . . C6 C -0.01005(15) 0.7338(3) 0.04852(14) 0.0576(11) Uani 1 d U . . H6 H 0.0002 0.8140 0.0558 0.069 Uiso 1 calc R . . C7 C -0.08129(17) 0.6829(5) 0.13153(17) 0.0692(13) Uani 1 d U . . C8 C -0.12071(17) 0.7568(4) 0.14396(19) 0.0746(14) Uani 1 d U . . C9 C -0.1448(2) 0.8446(5) 0.1160(2) 0.1066(19) Uani 1 d U . . H9 H -0.1367 0.8590 0.0889 0.128 Uiso 1 calc R . . C10 C -0.1819(2) 0.9116(6) 0.1294(3) 0.136(3) Uani 1 d U . . H10 H -0.1992 0.9700 0.1106 0.163 Uiso 1 calc R . . C11 C -0.1927(3) 0.8918(7) 0.1693(4) 0.141(3) Uani 1 d U . . H11 H -0.2167 0.9380 0.1781 0.169 Uiso 1 calc R . . C12 C -0.1689(3) 0.8057(8) 0.1964(3) 0.147(3) Uani 1 d U . . H12 H -0.1768 0.7927 0.2236 0.176 Uiso 1 calc R . . C13 C -0.1321(2) 0.7354(6) 0.1838(2) 0.113(2) Uani 1 d U . . H13 H -0.1160 0.6755 0.2023 0.136 Uiso 1 calc R . . C14 C 0.05399(19) 0.8268(4) 0.17992(17) 0.0794(14) Uani 1 d U . . C15 C 0.06884(16) 0.9496(4) 0.18621(16) 0.0655(12) Uani 1 d U . . C16 C 0.07732(16) 1.0159(4) 0.15172(16) 0.0690(12) Uani 1 d U . . H16 H 0.0754 0.9825 0.1239 0.083 Uiso 1 calc R . . C17 C 0.08861(17) 1.1312(4) 0.15816(18) 0.0791(14) Uani 1 d U . . H17 H 0.0942 1.1756 0.1347 0.095 Uiso 1 calc R . . C18 C 0.09155(19) 1.1803(4) 0.1992(2) 0.0902(16) Uani 1 d U . . H18 H 0.0985 1.2586 0.2035 0.108 Uiso 1 calc R . . C19 C 0.0843(2) 1.1144(5) 0.2337(2) 0.1091(19) Uani 1 d U . . H19 H 0.0868 1.1481 0.2617 0.131 Uiso 1 calc R . . C20 C 0.0732(2) 0.9988(4) 0.22780(17) 0.0959(17) Uani 1 d U . . H20 H 0.0686 0.9543 0.2516 0.115 Uiso 1 calc R . . C21 C 0.1345(2) 0.5287(5) 0.17270(17) 0.0880(16) Uani 1 d U . . C22 C 0.18467(19) 0.5448(4) 0.20631(17) 0.0747(13) Uani 1 d U . . C23 C 0.1985(2) 0.4674(6) 0.2402(2) 0.142(3) Uani 1 d U . . H23 H 0.1760 0.4073 0.2416 0.170 Uiso 1 calc R . . C24 C 0.2448(3) 0.4751(7) 0.2726(2) 0.142(3) Uani 1 d U . . H24 H 0.2534 0.4209 0.2956 0.170 Uiso 1 calc R . . C25 C 0.2772(2) 0.5610(7) 0.2707(2) 0.114(2) Uani 1 d U . . H25 H 0.3081 0.5685 0.2930 0.137 Uiso 1 calc R . . C26 C 0.2651(2) 0.6383(6) 0.2359(2) 0.122(2) Uani 1 d U . . H26 H 0.2883 0.6961 0.2336 0.146 Uiso 1 calc R . . C27 C 0.2175(2) 0.6295(5) 0.20394(19) 0.0984(17) Uani 1 d U . . H27 H 0.2086 0.6832 0.1808 0.118 Uiso 1 calc R . . C28 C 0.17810(17) 0.6575(5) 0.00270(18) 0.0795(14) Uani 1 d U . . C29 C 0.1815(3) 0.5565(6) -0.0181(3) 0.132(2) Uani 1 d U . . H29 H 0.1830 0.4880 -0.0022 0.158 Uiso 1 calc R . . C30 C 0.1828(3) 0.5533(9) -0.0623(4) 0.178(4) Uani 1 d U . . H30 H 0.1840 0.4829 -0.0764 0.214 Uiso 1 calc R . . C31 C 0.1821(3) 0.6535(12) -0.0858(3) 0.150(4) Uani 1 d U . . C32 C 0.1778(2) 0.7550(9) -0.0657(3) 0.142(3) Uani 1 d U . . H32 H 0.1757 0.8233 -0.0819 0.170 Uiso 1 calc R . . C33 C 0.17624(19) 0.7581(6) -0.0202(2) 0.1088(19) Uani 1 d U . . H33 H 0.1740 0.8280 -0.0061 0.131 Uiso 1 calc R . . C34 C 0.1839(3) 0.6626(9) -0.1356(2) 0.233(5) Uani 1 d U . . H34A H 0.1602 0.7210 -0.1505 0.350 Uiso 1 calc R . . H34B H 0.1744 0.5899 -0.1503 0.350 Uiso 1 calc R . . H34C H 0.2184 0.6826 -0.1368 0.350 Uiso 1 calc R . . C35 C 0.02960(16) 0.6783(4) -0.04523(15) 0.0591(11) Uani 1 d U . . C36 C 0.03743(15) 0.7527(4) -0.08162(14) 0.0569(11) Uani 1 d U . . C37 C 0.03738(17) 0.7028(4) -0.12247(17) 0.0785(14) Uani 1 d U . . H37 H 0.0322 0.6239 -0.1266 0.094 Uiso 1 calc R . . C38 C 0.0450(2) 0.7704(5) -0.15701(18) 0.0986(17) Uani 1 d U . . H38 H 0.0447 0.7377 -0.1847 0.118 Uiso 1 calc R . . C39 C 0.0530(2) 0.8876(5) -0.15001(19) 0.0954(17) Uani 1 d U . . H39 H 0.0591 0.9334 -0.1729 0.114 Uiso 1 calc R . . C40 C 0.05213(18) 0.9365(4) -0.11013(19) 0.0841(15) Uani 1 d U . . H40 H 0.0564 1.0157 -0.1063 0.101 Uiso 1 calc R . . C41 C 0.04501(16) 0.8697(4) -0.07555(16) 0.0688(12) Uani 1 d U . . H41 H 0.0453 0.9032 -0.0480 0.083 Uiso 1 calc R . . C42 C -0.0763(2) 0.8317(5) -0.00502(17) 0.0864(15) Uani 1 d U . . C43 C -0.12310(18) 0.8226(4) -0.04084(16) 0.0734(13) Uani 1 d U . . C44 C -0.14187(19) 0.7187(5) -0.05915(17) 0.0884(16) Uani 1 d U . . H44 H -0.1248 0.6508 -0.0481 0.106 Uiso 1 calc R . . C45 C -0.1853(3) 0.7156(6) -0.0934(2) 0.130(2) Uani 1 d U . . H45 H -0.1980 0.6453 -0.1060 0.156 Uiso 1 calc R . . C46 C -0.2113(2) 0.8175(7) -0.1100(2) 0.145(3) Uani 1 d U . . H46 H -0.2416 0.8144 -0.1331 0.174 Uiso 1 calc R . . C47 C -0.1923(3) 0.9207(6) -0.0927(2) 0.128(2) Uani 1 d U . . H47 H -0.2090 0.9887 -0.1042 0.154 Uiso 1 calc R . . C48 C -0.1487(2) 0.9238(5) -0.05824(19) 0.1022(17) Uani 1 d U . . H48 H -0.1356 0.9943 -0.0461 0.123 Uiso 1 calc R . . C49 C 0.0000 0.5375(11) 0.2500 0.086(4) Uani 0.50 d SPU . . H49A H -0.0149 0.5869 0.2245 0.103 Uiso 0.25 calc PR . . H49B H 0.0149 0.5869 0.2755 0.103 Uiso 0.25 calc PR . . 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 Cl1 0.190(4) 0.106(3) 0.223(4) -0.020(3) 0.115(3) 0.022(2) S1 0.0664(9) 0.0862(10) 0.0902(10) 0.0073(9) 0.0241(7) 0.0057(8) O1 0.0619(19) 0.0570(18) 0.075(2) 0.0014(16) 0.0227(16) 0.0045(15) O2 0.100(3) 0.071(2) 0.118(3) 0.019(2) 0.054(2) 0.008(2) O3 0.0709(19) 0.0508(18) 0.053(2) -0.0063(14) 0.0149(14) -0.0069(14) O4 0.351(7) 0.084(3) 0.075(3) -0.015(2) 0.081(4) -0.073(3) O5 0.060(2) 0.0566(19) 0.067(2) 0.0016(16) 0.0060(16) -0.0016(14) O6 0.147(4) 0.135(4) 0.228(5) 0.112(4) -0.089(4) -0.079(3) O7 0.069(2) 0.0574(18) 0.091(2) -0.0102(16) 0.0358(17) -0.0040(15) O8 0.096(3) 0.120(3) 0.128(3) 0.039(3) 0.028(2) 0.040(2) O9 0.079(2) 0.084(2) 0.122(3) -0.022(2) 0.032(2) -0.0201(18) O10 0.086(2) 0.0507(17) 0.0489(19) -0.0032(16) 0.0218(15) -0.0135(15) O11 0.148(3) 0.053(2) 0.070(2) -0.0113(17) 0.039(2) -0.027(2) O12 0.062(2) 0.0567(19) 0.063(2) 0.0001(16) 0.0009(16) -0.0021(15) O13 0.178(4) 0.062(3) 0.178(4) -0.021(3) -0.077(3) 0.020(3) C1 0.057(3) 0.048(2) 0.055(3) -0.005(2) 0.018(2) 0.000(2) C2 0.062(3) 0.046(3) 0.059(3) -0.004(2) 0.021(2) -0.010(2) C3 0.046(3) 0.049(3) 0.059(3) 0.000(2) 0.007(2) -0.003(2) C4 0.060(3) 0.043(2) 0.063(3) -0.001(2) 0.021(2) 0.001(2) C5 0.073(3) 0.044(2) 0.049(3) -0.002(2) 0.016(2) -0.009(2) C6 0.061(3) 0.052(3) 0.057(3) -0.005(2) 0.011(2) -0.003(2) C7 0.066(3) 0.068(3) 0.077(4) -0.001(3) 0.025(3) 0.000(3) C8 0.061(3) 0.077(4) 0.089(4) -0.011(3) 0.026(3) -0.003(3) C9 0.076(4) 0.093(4) 0.160(6) 0.013(4) 0.048(4) 0.008(3) C10 0.086(5) 0.105(5) 0.231(10) 0.017(6) 0.067(6) 0.011(4) C11 0.079(5) 0.125(7) 0.224(11) -0.040(7) 0.047(6) 0.013(4) C12 0.101(5) 0.226(9) 0.126(6) -0.060(6) 0.053(5) 0.016(6) C13 0.093(4) 0.159(6) 0.091(5) -0.018(4) 0.031(4) 0.019(4) C14 0.121(4) 0.071(4) 0.047(3) -0.003(3) 0.021(3) -0.011(3) C15 0.081(3) 0.058(3) 0.057(3) -0.008(3) 0.017(2) -0.006(2) C16 0.077(3) 0.064(3) 0.064(3) -0.006(3) 0.014(3) -0.004(3) C17 0.096(4) 0.062(4) 0.082(4) 0.003(3) 0.027(3) -0.009(3) C18 0.108(4) 0.059(3) 0.107(5) -0.009(4) 0.033(3) -0.008(3) C19 0.159(6) 0.080(4) 0.100(5) -0.037(4) 0.056(4) -0.018(4) C20 0.157(5) 0.069(4) 0.070(4) -0.014(3) 0.044(3) -0.014(3) C21 0.074(4) 0.082(4) 0.089(4) 0.028(3) -0.013(3) -0.008(3) C22 0.066(4) 0.072(3) 0.079(4) 0.009(3) 0.005(3) -0.001(3) C23 0.103(5) 0.151(6) 0.140(6) 0.071(5) -0.026(4) -0.035(4) C24 0.101(5) 0.175(7) 0.126(6) 0.074(5) -0.013(4) -0.009(5) C25 0.093(5) 0.141(6) 0.089(5) 0.002(4) -0.009(4) 0.000(5) C26 0.096(5) 0.117(5) 0.134(6) -0.003(5) -0.003(4) -0.019(4) C27 0.079(4) 0.090(4) 0.108(5) 0.008(3) -0.006(4) -0.007(3) C28 0.068(3) 0.086(4) 0.092(4) 0.008(4) 0.034(3) 0.002(3) C29 0.181(7) 0.122(6) 0.117(6) -0.011(5) 0.083(5) -0.006(5) C30 0.216(9) 0.185(10) 0.162(10) -0.046(8) 0.100(8) -0.039(7) C31 0.083(5) 0.263(13) 0.113(7) -0.025(8) 0.042(4) 0.013(7) C32 0.098(5) 0.215(10) 0.129(7) 0.081(7) 0.059(5) 0.026(5) C33 0.095(4) 0.124(6) 0.117(6) 0.024(5) 0.044(4) 0.022(4) C34 0.154(7) 0.467(16) 0.095(6) 0.014(8) 0.061(5) 0.016(8) C35 0.075(3) 0.049(3) 0.053(3) -0.003(3) 0.017(2) -0.005(2) C36 0.066(3) 0.055(3) 0.051(3) 0.001(2) 0.017(2) -0.001(2) C37 0.103(4) 0.068(3) 0.071(4) 0.002(3) 0.034(3) -0.007(3) C38 0.139(5) 0.092(4) 0.076(4) 0.001(3) 0.048(3) -0.013(4) C39 0.127(5) 0.092(5) 0.081(4) 0.029(3) 0.053(3) -0.005(3) C40 0.110(4) 0.065(3) 0.086(4) 0.010(3) 0.040(3) -0.004(3) C41 0.082(3) 0.063(3) 0.066(3) 0.001(3) 0.026(3) -0.003(2) C42 0.100(4) 0.054(3) 0.087(4) -0.010(3) -0.007(3) 0.009(3) C43 0.077(3) 0.069(3) 0.068(3) -0.006(3) 0.009(3) 0.007(3) C44 0.076(4) 0.084(4) 0.086(4) 0.008(3) -0.012(3) -0.013(3) C45 0.111(5) 0.101(5) 0.147(6) 0.017(4) -0.023(5) -0.020(4) C46 0.100(5) 0.138(7) 0.155(7) 0.040(6) -0.042(4) -0.022(5) C47 0.089(5) 0.123(6) 0.147(6) 0.025(5) -0.018(4) 0.015(4) C48 0.096(4) 0.087(4) 0.109(5) 0.002(3) 0.002(4) 0.025(3) C49 0.132(12) 0.068(9) 0.073(10) 0.000 0.056(9) 0.000 _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 Cl1 C49 1.665(7) . ? S1 O8 1.410(3) . ? S1 O9 1.423(3) . ? S1 O7 1.594(3) . ? S1 C28 1.733(5) . ? O1 C7 1.365(5) . ? O1 C1 1.435(4) . ? O2 C7 1.189(5) . ? O3 C14 1.328(5) . ? O3 C2 1.446(4) . ? O4 C14 1.195(5) . ? O5 C21 1.338(5) . ? O5 C3 1.421(4) . ? O6 C21 1.174(5) . ? O7 C4 1.446(4) . ? O10 C35 1.348(4) . ? O10 C5 1.433(4) . ? O11 C35 1.207(4) . ? O12 C42 1.346(5) . ? O12 C6 1.426(4) . ? O13 C42 1.207(5) . ? C1 C6 1.508(5) . ? C1 C2 1.526(5) . ? C2 C3 1.525(5) . ? C3 C4 1.512(5) . ? C4 C5 1.512(5) . ? C5 C6 1.521(5) . ? C7 C8 1.486(6) . ? C8 C13 1.362(6) . ? C8 C9 1.380(6) . ? C9 C10 1.405(8) . ? C10 C11 1.354(9) . ? C11 C12 1.350(9) . ? C12 C13 1.409(8) . ? C14 C15 1.479(6) . ? C15 C16 1.378(5) . ? C15 C20 1.379(6) . ? C16 C17 1.374(6) . ? C17 C18 1.369(6) . ? C18 C19 1.365(7) . ? C19 C20 1.377(6) . ? C21 C22 1.476(6) . ? C22 C27 1.334(6) . ? C22 C23 1.352(6) . ? C23 C24 1.377(7) . ? C24 C25 1.334(7) . ? C25 C26 1.369(7) . ? C26 C27 1.395(7) . ? C28 C29 1.350(7) . ? C28 C33 1.359(7) . ? C29 C30 1.371(10) . ? C30 C31 1.366(11) . ? C31 C32 1.349(10) . ? C31 C34 1.550(10) . ? C32 C33 1.411(8) . ? C35 C36 1.472(5) . ? C36 C41 1.379(5) . ? C36 C37 1.384(5) . ? C37 C38 1.378(6) . ? C38 C39 1.386(6) . ? C39 C40 1.358(6) . ? C40 C41 1.370(6) . ? C42 C43 1.440(6) . ? C43 C44 1.369(6) . ? C43 C48 1.394(6) . ? C44 C45 1.350(7) . ? C45 C46 1.398(8) . ? C46 C47 1.356(8) . ? C47 C48 1.356(7) . ? C49 Cl1 1.665(7) 2 ? 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 O8 S1 O9 119.6(2) . . ? O8 S1 O7 105.6(2) . . ? O9 S1 O7 109.04(17) . . ? O8 S1 C28 109.5(2) . . ? O9 S1 C28 110.6(3) . . ? O7 S1 C28 100.7(2) . . ? C7 O1 C1 116.0(3) . . ? C14 O3 C2 118.2(3) . . ? C21 O5 C3 117.4(3) . . ? C4 O7 S1 120.7(2) . . ? C35 O10 C5 118.2(3) . . ? C42 O12 C6 117.6(3) . . ? O1 C1 C6 107.0(3) . . ? O1 C1 C2 109.8(3) . . ? C6 C1 C2 110.5(3) . . ? O3 C2 C3 107.8(3) . . ? O3 C2 C1 107.9(3) . . ? C3 C2 C1 109.7(3) . . ? O5 C3 C4 107.0(3) . . ? O5 C3 C2 109.7(3) . . ? C4 C3 C2 110.7(3) . . ? O7 C4 C3 108.1(3) . . ? O7 C4 C5 108.0(3) . . ? C3 C4 C5 109.8(3) . . ? O10 C5 C4 108.2(3) . . ? O10 C5 C6 108.6(3) . . ? C4 C5 C6 110.3(3) . . ? O12 C6 C1 110.1(3) . . ? O12 C6 C5 108.1(3) . . ? C1 C6 C5 109.7(3) . . ? O2 C7 O1 122.7(4) . . ? O2 C7 C8 125.6(5) . . ? O1 C7 C8 111.7(4) . . ? C13 C8 C9 121.2(5) . . ? C13 C8 C7 117.9(5) . . ? C9 C8 C7 120.9(5) . . ? C8 C9 C10 118.5(6) . . ? C11 C10 C9 120.5(7) . . ? C12 C11 C10 120.5(8) . . ? C11 C12 C13 120.7(8) . . ? C8 C13 C12 118.6(6) . . ? O4 C14 O3 122.0(5) . . ? O4 C14 C15 124.8(5) . . ? O3 C14 C15 113.2(4) . . ? C16 C15 C20 119.5(4) . . ? C16 C15 C14 122.1(4) . . ? C20 C15 C14 118.4(5) . . ? C17 C16 C15 120.5(4) . . ? C18 C17 C16 119.7(5) . . ? C19 C18 C17 120.0(5) . . ? C18 C19 C20 120.9(5) . . ? C19 C20 C15 119.3(5) . . ? O6 C21 O5 121.5(5) . . ? O6 C21 C22 125.8(5) . . ? O5 C21 C22 112.6(5) . . ? C27 C22 C23 118.8(5) . . ? C27 C22 C21 123.1(5) . . ? C23 C22 C21 118.1(5) . . ? C22 C23 C24 121.9(6) . . ? C25 C24 C23 119.3(6) . . ? C24 C25 C26 120.0(6) . . ? C25 C26 C27 119.4(6) . . ? C22 C27 C26 120.5(6) . . ? C29 C28 C33 119.8(6) . . ? C29 C28 S1 119.0(5) . . ? C33 C28 S1 121.2(5) . . ? C28 C29 C30 121.1(7) . . ? C31 C30 C29 120.1(9) . . ? C32 C31 C30 119.5(9) . . ? C32 C31 C34 115.0(11) . . ? C30 C31 C34 125.5(11) . . ? C31 C32 C33 120.3(8) . . ? C28 C33 C32 119.1(7) . . ? O11 C35 O10 122.7(4) . . ? O11 C35 C36 124.8(4) . . ? O10 C35 C36 112.5(4) . . ? C41 C36 C37 120.0(4) . . ? C41 C36 C35 121.3(4) . . ? C37 C36 C35 118.7(4) . . ? C38 C37 C36 119.9(5) . . ? C37 C38 C39 119.1(5) . . ? C40 C39 C38 120.8(5) . . ? C39 C40 C41 120.3(5) . . ? C40 C41 C36 119.8(4) . . ? O13 C42 O12 120.5(5) . . ? O13 C42 C43 124.6(5) . . ? O12 C42 C43 114.9(5) . . ? C44 C43 C48 119.6(5) . . ? C44 C43 C42 122.1(5) . . ? C48 C43 C42 118.3(5) . . ? C45 C44 C43 119.5(5) . . ? C44 C45 C46 120.5(6) . . ? C47 C46 C45 120.2(6) . . ? C46 C47 C48 119.2(6) . . ? C47 C48 C43 120.9(6) . . ? Cl1 C49 Cl1 114.9(8) . 2 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O8 S1 O7 C4 125.4(3) . . . . ? O9 S1 O7 C4 -4.4(3) . . . . ? C28 S1 O7 C4 -120.7(3) . . . . ? C7 O1 C1 C6 161.7(3) . . . . ? C7 O1 C1 C2 -78.3(4) . . . . ? C14 O3 C2 C3 -118.5(4) . . . . ? C14 O3 C2 C1 123.1(4) . . . . ? O1 C1 C2 O3 -58.3(4) . . . . ? C6 C1 C2 O3 59.5(4) . . . . ? O1 C1 C2 C3 -175.5(3) . . . . ? C6 C1 C2 C3 -57.7(4) . . . . ? C21 O5 C3 C4 -144.0(4) . . . . ? C21 O5 C3 C2 95.8(4) . . . . ? O3 C2 C3 O5 58.1(4) . . . . ? C1 C2 C3 O5 175.4(3) . . . . ? O3 C2 C3 C4 -59.8(4) . . . . ? C1 C2 C3 C4 57.4(4) . . . . ? S1 O7 C4 C3 -109.7(3) . . . . ? S1 O7 C4 C5 131.4(3) . . . . ? O5 C3 C4 O7 64.5(4) . . . . ? C2 C3 C4 O7 -175.9(3) . . . . ? O5 C3 C4 C5 -177.8(3) . . . . ? C2 C3 C4 C5 -58.3(4) . . . . ? C35 O10 C5 C4 125.1(3) . . . . ? C35 O10 C5 C6 -115.2(4) . . . . ? O7 C4 C5 O10 -64.7(4) . . . . ? C3 C4 C5 O10 177.6(3) . . . . ? O7 C4 C5 C6 176.7(3) . . . . ? C3 C4 C5 C6 58.9(4) . . . . ? C42 O12 C6 C1 122.8(4) . . . . ? C42 O12 C6 C5 -117.4(4) . . . . ? O1 C1 C6 O12 -63.0(4) . . . . ? C2 C1 C6 O12 177.5(3) . . . . ? O1 C1 C6 C5 178.2(3) . . . . ? C2 C1 C6 C5 58.7(4) . . . . ? O10 C5 C6 O12 62.2(4) . . . . ? C4 C5 C6 O12 -179.3(3) . . . . ? O10 C5 C6 C1 -177.7(3) . . . . ? C4 C5 C6 C1 -59.3(4) . . . . ? C1 O1 C7 O2 1.2(6) . . . . ? C1 O1 C7 C8 180.0(3) . . . . ? O2 C7 C8 C13 25.2(8) . . . . ? O1 C7 C8 C13 -153.5(4) . . . . ? O2 C7 C8 C9 -154.9(5) . . . . ? O1 C7 C8 C9 26.4(6) . . . . ? C13 C8 C9 C10 -0.3(8) . . . . ? C7 C8 C9 C10 179.8(5) . . . . ? C8 C9 C10 C11 1.5(10) . . . . ? C9 C10 C11 C12 -1.6(12) . . . . ? C10 C11 C12 C13 0.5(12) . . . . ? C9 C8 C13 C12 -0.8(8) . . . . ? C7 C8 C13 C12 179.1(5) . . . . ? C11 C12 C13 C8 0.7(10) . . . . ? C2 O3 C14 O4 -0.1(7) . . . . ? C2 O3 C14 C15 -178.4(3) . . . . ? O4 C14 C15 C16 178.7(5) . . . . ? O3 C14 C15 C16 -3.0(6) . . . . ? O4 C14 C15 C20 -2.6(8) . . . . ? O3 C14 C15 C20 175.6(4) . . . . ? C20 C15 C16 C17 -1.8(7) . . . . ? C14 C15 C16 C17 176.8(4) . . . . ? C15 C16 C17 C18 0.1(7) . . . . ? C16 C17 C18 C19 1.3(7) . . . . ? C17 C18 C19 C20 -1.0(8) . . . . ? C18 C19 C20 C15 -0.7(8) . . . . ? C16 C15 C20 C19 2.1(7) . . . . ? C14 C15 C20 C19 -176.6(5) . . . . ? C3 O5 C21 O6 -1.5(8) . . . . ? C3 O5 C21 C22 179.9(4) . . . . ? O6 C21 C22 C27 169.9(7) . . . . ? O5 C21 C22 C27 -11.5(7) . . . . ? O6 C21 C22 C23 -7.9(10) . . . . ? O5 C21 C22 C23 170.7(5) . . . . ? C27 C22 C23 C24 1.3(10) . . . . ? C21 C22 C23 C24 179.2(6) . . . . ? C22 C23 C24 C25 -0.1(12) . . . . ? C23 C24 C25 C26 -2.1(11) . . . . ? C24 C25 C26 C27 3.2(10) . . . . ? C23 C22 C27 C26 -0.2(9) . . . . ? C21 C22 C27 C26 -178.0(5) . . . . ? C25 C26 C27 C22 -2.0(9) . . . . ? O8 S1 C28 C29 39.1(5) . . . . ? O9 S1 C28 C29 172.9(4) . . . . ? O7 S1 C28 C29 -71.9(5) . . . . ? O8 S1 C28 C33 -140.6(4) . . . . ? O9 S1 C28 C33 -6.8(5) . . . . ? O7 S1 C28 C33 108.4(4) . . . . ? C33 C28 C29 C30 -0.5(10) . . . . ? S1 C28 C29 C30 179.8(6) . . . . ? C28 C29 C30 C31 2.0(12) . . . . ? C29 C30 C31 C32 -3.2(13) . . . . ? C29 C30 C31 C34 179.4(7) . . . . ? C30 C31 C32 C33 2.9(12) . . . . ? C34 C31 C32 C33 -179.4(5) . . . . ? C29 C28 C33 C32 0.2(8) . . . . ? S1 C28 C33 C32 179.9(4) . . . . ? C31 C32 C33 C28 -1.4(9) . . . . ? C5 O10 C35 O11 -2.9(6) . . . . ? C5 O10 C35 C36 176.6(3) . . . . ? O11 C35 C36 C41 167.3(4) . . . . ? O10 C35 C36 C41 -12.2(5) . . . . ? O11 C35 C36 C37 -13.1(6) . . . . ? O10 C35 C36 C37 167.4(4) . . . . ? C41 C36 C37 C38 0.0(7) . . . . ? C35 C36 C37 C38 -179.6(4) . . . . ? C36 C37 C38 C39 0.6(7) . . . . ? C37 C38 C39 C40 -1.7(8) . . . . ? C38 C39 C40 C41 2.2(8) . . . . ? C39 C40 C41 C36 -1.6(7) . . . . ? C37 C36 C41 C40 0.4(6) . . . . ? C35 C36 C41 C40 -179.9(4) . . . . ? C6 O12 C42 O13 0.5(7) . . . . ? C6 O12 C42 C43 -179.9(4) . . . . ? O13 C42 C43 C44 171.4(6) . . . . ? O12 C42 C43 C44 -8.2(7) . . . . ? O13 C42 C43 C48 -6.1(8) . . . . ? O12 C42 C43 C48 174.2(4) . . . . ? C48 C43 C44 C45 -0.9(8) . . . . ? C42 C43 C44 C45 -178.5(5) . . . . ? C43 C44 C45 C46 -0.4(10) . . . . ? C44 C45 C46 C47 1.7(11) . . . . ? C45 C46 C47 C48 -1.7(11) . . . . ? C46 C47 C48 C43 0.4(10) . . . . ? C44 C43 C48 C47 0.9(8) . . . . ? C42 C43 C48 C47 178.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.297 _refine_diff_density_min -0.223 _refine_diff_density_rms 0.040 data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; '1,2,3,4,5-penta-o-benzoyl-6-o-tosyl myo-inositol-dibromomethane' ; _chemical_name_common 'myo-inositol' _chemical_formula_moiety 'C48.5 H39 Br O13 S' _chemical_formula_sum 'C48.5 H39 Br O13 S' _chemical_formula_weight 941.77 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' 'Br' 'Br' -0.2901 2.4595 '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 'C2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.9267(17) _cell_length_b 11.7160(8) _cell_length_c 30.874(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.9980(10) _cell_angle_gamma 90.00 _cell_volume 9362.7(11) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2348 _cell_measurement_theta_min 1.55 _cell_measurement_theta_max 23.26 _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max '0.24' _exptl_crystal_size_mid '0.22' _exptl_crystal_size_min '0.16' _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3880 _exptl_absorpt_coefficient_mu 0.986 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26695 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 23.26 _reflns_number_total 6718 _reflns_number_gt 4006 _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 'ORTEP32 and PLATON-97' _computing_publication_material 'SHELX-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.1420P)^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 6718 _refine_ls_number_parameters 573 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1014 _refine_ls_R_factor_gt 0.0664 _refine_ls_wR_factor_ref 0.2329 _refine_ls_wR_factor_gt 0.2172 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.039 _refine_ls_shift/su_mean 0.003 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.05180(4) 0.53897(8) 0.23637(4) 0.1312(5) Uani 1 d . . . S1 S 0.17596(5) 0.34945(14) 0.05819(5) 0.0638(4) Uani 1 d . . . O1 O -0.05609(12) 0.2605(3) 0.10225(11) 0.0486(8) Uani 1 d . . . O2 O -0.06942(14) 0.4095(4) 0.14319(13) 0.0695(10) Uani 1 d . . . O3 O 0.04934(12) 0.2141(2) 0.13745(9) 0.0438(8) Uani 1 d . . . O4 O 0.0379(2) 0.2310(4) 0.20573(14) 0.116(2) Uani 1 d . . . O5 O 0.12163(12) 0.3864(3) 0.14491(11) 0.0499(8) Uani 1 d . . . O6 O 0.11549(17) 0.5717(4) 0.15857(16) 0.0963(15) Uani 1 d . . . O7 O 0.11905(13) 0.3970(3) 0.05296(12) 0.0574(9) Uani 1 d . . . O8 O 0.20984(16) 0.4350(4) 0.08138(16) 0.0970(15) Uani 1 d . . . O9 O 0.17949(15) 0.2371(4) 0.07605(15) 0.0811(12) Uani 1 d . . . O10 O 0.04038(13) 0.2684(3) -0.00587(10) 0.0489(8) Uani 1 d . . . O11 O 0.01475(17) 0.4194(3) -0.05110(11) 0.0717(11) Uani 1 d . . . O12 O -0.05620(12) 0.2678(3) 0.01176(10) 0.0505(9) Uani 1 d . . . O13 O -0.0543(2) 0.0773(4) 0.00929(19) 0.140(3) Uani 1 d . . . C1 C -0.01751(17) 0.3249(4) 0.08895(14) 0.0400(11) Uani 1 d . . . H1 H -0.0301 0.4027 0.0811 0.048 Uiso 1 calc R . . C2 C 0.03227(16) 0.3292(4) 0.12582(15) 0.0397(11) Uani 1 d . . . H2 H 0.0270 0.3685 0.1522 0.048 Uiso 1 calc R . . C3 C 0.07345(16) 0.3899(4) 0.10961(14) 0.0407(11) Uani 1 d . . . H3 H 0.0632 0.4695 0.1024 0.049 Uiso 1 calc R . . C4 C 0.08172(16) 0.3325(4) 0.06907(15) 0.0418(11) Uani 1 d . . . H4 H 0.0944 0.2546 0.0767 0.050 Uiso 1 calc R . . C5 C 0.03202(18) 0.3297(4) 0.03210(15) 0.0438(11) Uani 1 d . . . H5 H 0.0205 0.4076 0.0231 0.053 Uiso 1 calc R . . C6 C -0.00944(17) 0.2665(4) 0.04769(14) 0.0432(12) Uani 1 d . . . H6 H 0.0015 0.1874 0.0551 0.052 Uiso 1 calc R . . C7 C -0.07992(19) 0.3146(5) 0.13002(18) 0.0533(13) Uani 1 d . . . C8 C -0.1190(2) 0.2406(5) 0.1418(2) 0.0659(16) Uani 1 d . . . C9 C -0.1432(2) 0.1550(6) 0.1152(3) 0.094(2) Uani 1 d . . . H9 H -0.1354 0.1402 0.0883 0.113 Uiso 1 calc R . . C10 C -0.1794(3) 0.0890(7) 0.1276(5) 0.136(4) Uani 1 d . . . H10 H -0.1967 0.0318 0.1084 0.163 Uiso 1 calc R . . C11 C -0.1900(4) 0.1067(11) 0.1673(5) 0.147(5) Uani 1 d . . . H11 H -0.2139 0.0610 0.1758 0.176 Uiso 1 calc R . . C12 C -0.1657(3) 0.1907(12) 0.1945(4) 0.155(5) Uani 1 d . . . H12 H -0.1726 0.2021 0.2220 0.186 Uiso 1 calc R . . C13 C -0.1302(2) 0.2613(8) 0.1820(2) 0.106(3) Uani 1 d . . . H13 H -0.1145 0.3212 0.2005 0.128 Uiso 1 calc R . . C14 C 0.0504(2) 0.1742(5) 0.17850(17) 0.0576(14) Uani 1 d . . . C15 C 0.06691(19) 0.0535(4) 0.18457(16) 0.0489(12) Uani 1 d . . . C16 C 0.0694(2) 0.0033(5) 0.22519(19) 0.0716(16) Uani 1 d . . . H16 H 0.0625 0.0460 0.2483 0.086 Uiso 1 calc R . . C17 C 0.0822(3) -0.1114(6) 0.2319(2) 0.088(2) Uani 1 d . . . H17 H 0.0843 -0.1454 0.2595 0.106 Uiso 1 calc R . . C18 C 0.0918(2) -0.1744(5) 0.1978(2) 0.0735(17) Uani 1 d . . . H18 H 0.0999 -0.2515 0.2022 0.088 Uiso 1 calc R . . C19 C 0.0895(2) -0.1248(5) 0.1575(2) 0.0629(15) Uani 1 d . . . H19 H 0.0963 -0.1678 0.1345 0.075 Uiso 1 calc R . . C20 C 0.07703(19) -0.0103(4) 0.15073(18) 0.0542(13) Uani 1 d . . . H20 H 0.0755 0.0235 0.1231 0.065 Uiso 1 calc R . . C21 C 0.1388(2) 0.4854(5) 0.16738(17) 0.0528(13) Uani 1 d . . . C22 C 0.18697(19) 0.4704(5) 0.20273(18) 0.0559(14) Uani 1 d . . . C23 C 0.2031(3) 0.5518(7) 0.2339(3) 0.116(3) Uani 1 d . . . H23 H 0.1835 0.6179 0.2318 0.140 Uiso 1 calc R . . C24 C 0.2479(3) 0.5421(9) 0.2693(3) 0.123(3) Uani 1 d . . . H24 H 0.2566 0.5986 0.2913 0.147 Uiso 1 calc R . . C25 C 0.2773(3) 0.4531(8) 0.2713(3) 0.106(3) Uani 1 d . . . H25 H 0.3068 0.4448 0.2954 0.127 Uiso 1 calc R . . C26 C 0.2649(3) 0.3697(7) 0.2376(3) 0.123(3) Uani 1 d . . . H26 H 0.2873 0.3094 0.2374 0.147 Uiso 1 calc R . . C27 C 0.2185(3) 0.3792(6) 0.2044(2) 0.097(2) Uani 1 d . . . H27 H 0.2087 0.3219 0.1828 0.117 Uiso 1 calc R . . C28 C 0.1775(2) 0.3465(6) 0.0020(2) 0.0707(16) Uani 1 d . . . C29 C 0.1790(4) 0.4473(8) -0.0202(3) 0.121(3) Uani 1 d . . . H29 H 0.1789 0.5168 -0.0057 0.146 Uiso 1 calc R . . C30 C 0.1808(4) 0.4438(12) -0.0653(4) 0.156(5) Uani 1 d . . . H30 H 0.1817 0.5115 -0.0808 0.187 Uiso 1 calc R . . C31 C 0.1813(3) 0.3405(15) -0.0868(3) 0.134(4) Uani 1 d . . . C32 C 0.1787(3) 0.2448(11) -0.0638(4) 0.130(4) Uani 1 d . . . H32 H 0.1779 0.1752 -0.0785 0.156 Uiso 1 calc R . . C33 C 0.1771(3) 0.2441(7) -0.0203(3) 0.094(2) Uani 1 d . . . H33 H 0.1758 0.1754 -0.0055 0.113 Uiso 1 calc R . . C34 C 0.1831(4) 0.3353(13) -0.1353(3) 0.187(5) Uani 1 d . . . H34C H 0.1816 0.2534 -0.1449 0.176 Uiso 1 d . . . H34A H 0.1503 0.3740 -0.1565 0.176 Uiso 1 d . . . H34B H 0.2134 0.3734 -0.1407 0.176 Uiso 1 d . . . C35 C 0.02960(18) 0.3227(4) -0.04606(15) 0.0449(12) Uani 1 d . . . C36 C 0.03758(18) 0.2480(4) -0.08181(16) 0.0469(12) Uani 1 d . . . C37 C 0.0369(2) 0.2967(5) -0.12311(17) 0.0635(15) Uani 1 d . . . H37 H 0.0308 0.3744 -0.1280 0.076 Uiso 1 calc R . . C38 C 0.0456(3) 0.2281(6) -0.15685(19) 0.0782(18) Uani 1 d . . . H38 H 0.0466 0.2600 -0.1842 0.094 Uiso 1 calc R . . C39 C 0.0527(2) 0.1121(6) -0.1497(2) 0.0764(18) Uani 1 d . . . H39 H 0.0580 0.0662 -0.1726 0.092 Uiso 1 calc R . . C40 C 0.0521(2) 0.0636(5) -0.1095(2) 0.0654(15) Uani 1 d . . . H40 H 0.0565 -0.0147 -0.1052 0.078 Uiso 1 calc R . . C41 C 0.04503(19) 0.1313(4) -0.07592(17) 0.0545(13) Uani 1 d . . . H41 H 0.0452 0.0986 -0.0484 0.065 Uiso 1 calc R . . C42 C -0.0759(2) 0.1650(5) -0.00500(19) 0.0667(15) Uani 1 d . . . C43 C -0.1237(2) 0.1728(5) -0.04163(17) 0.0583(14) Uani 1 d . . . C44 C -0.1486(3) 0.0720(6) -0.0571(2) 0.085(2) Uani 1 d . . . H44 H -0.1349 0.0031 -0.0442 0.102 Uiso 1 calc R . . C45 C -0.1936(3) 0.0728(7) -0.0917(3) 0.111(3) Uani 1 d . . . H45 H -0.2105 0.0047 -0.1020 0.133 Uiso 1 calc R . . C46 C -0.2134(3) 0.1736(9) -0.1106(3) 0.119(3) Uani 1 d . . . H46 H -0.2437 0.1747 -0.1340 0.142 Uiso 1 calc R . . C47 C -0.1880(3) 0.2749(7) -0.0947(3) 0.100(2) Uani 1 d . . . H47 H -0.2016 0.3437 -0.1078 0.120 Uiso 1 calc R . . C48 C -0.1436(2) 0.2749(5) -0.06049(19) 0.0681(16) Uani 1 d . . . H48 H -0.1270 0.3432 -0.0500 0.082 Uiso 1 calc R . . C49 C 0.0000 0.4517(8) 0.2500 0.088(3) Uani 1 d S . . H49A H -0.0156 0.4029 0.2245 0.106 Uiso 0.50 calc PR . . H49B H 0.0156 0.4029 0.2755 0.106 Uiso 0.50 calc PR . . 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 Br1 0.1694(9) 0.0959(7) 0.1605(9) -0.0048(5) 0.0996(8) -0.0324(6) S1 0.0524(8) 0.0712(10) 0.0705(10) -0.0035(8) 0.0215(7) -0.0040(7) O1 0.0506(19) 0.0422(19) 0.055(2) 0.0025(16) 0.0169(16) -0.0040(15) O2 0.078(3) 0.062(3) 0.080(3) -0.013(2) 0.040(2) -0.005(2) O3 0.061(2) 0.0371(18) 0.0353(18) 0.0050(14) 0.0157(15) 0.0056(15) O4 0.242(6) 0.063(3) 0.064(3) 0.014(2) 0.079(3) 0.052(3) O5 0.050(2) 0.039(2) 0.057(2) -0.0007(16) 0.0075(16) 0.0011(15) O6 0.088(3) 0.056(3) 0.120(4) -0.029(2) -0.014(3) 0.013(2) O7 0.060(2) 0.048(2) 0.073(2) 0.0083(17) 0.0326(18) 0.0013(16) O8 0.068(3) 0.116(4) 0.106(3) -0.034(3) 0.021(2) -0.034(3) O9 0.065(2) 0.083(3) 0.100(3) 0.026(2) 0.028(2) 0.024(2) O10 0.071(2) 0.0375(18) 0.0389(19) 0.0033(15) 0.0171(16) 0.0134(16) O11 0.128(3) 0.041(2) 0.052(2) 0.0100(17) 0.034(2) 0.025(2) O12 0.057(2) 0.041(2) 0.0470(19) -0.0001(15) 0.0038(16) -0.0016(16) O13 0.163(5) 0.046(3) 0.144(5) 0.021(3) -0.070(4) -0.016(3) C1 0.046(3) 0.033(3) 0.042(3) 0.006(2) 0.014(2) 0.003(2) C2 0.046(3) 0.033(3) 0.039(3) 0.002(2) 0.010(2) 0.009(2) C3 0.039(3) 0.035(3) 0.043(3) 0.003(2) 0.003(2) 0.003(2) C4 0.046(3) 0.034(3) 0.048(3) 0.005(2) 0.017(2) 0.000(2) C5 0.058(3) 0.035(3) 0.041(3) 0.003(2) 0.017(2) 0.008(2) C6 0.047(3) 0.039(3) 0.040(3) 0.005(2) 0.006(2) 0.005(2) C7 0.051(3) 0.052(4) 0.058(3) 0.005(3) 0.018(3) 0.004(3) C8 0.044(3) 0.071(4) 0.085(4) 0.016(3) 0.021(3) 0.003(3) C9 0.064(4) 0.071(4) 0.159(7) -0.010(5) 0.051(4) -0.009(4) C10 0.069(5) 0.078(5) 0.267(14) -0.003(7) 0.057(7) -0.013(4) C11 0.071(6) 0.152(10) 0.220(14) 0.093(10) 0.046(8) 0.002(6) C12 0.077(6) 0.265(15) 0.124(8) 0.088(9) 0.032(5) -0.015(7) C13 0.069(4) 0.173(8) 0.082(5) 0.025(5) 0.029(4) -0.023(5) C14 0.083(4) 0.051(3) 0.042(3) 0.005(3) 0.022(3) 0.007(3) C15 0.063(3) 0.040(3) 0.044(3) 0.005(2) 0.014(2) 0.002(2) C16 0.113(5) 0.053(4) 0.051(3) 0.007(3) 0.028(3) 0.006(3) C17 0.135(6) 0.066(4) 0.072(4) 0.029(4) 0.040(4) 0.017(4) C18 0.093(4) 0.041(3) 0.092(5) 0.010(3) 0.033(4) 0.010(3) C19 0.072(4) 0.050(4) 0.069(4) -0.006(3) 0.023(3) 0.003(3) C20 0.062(3) 0.049(3) 0.051(3) 0.008(3) 0.015(3) 0.004(3) C21 0.055(3) 0.048(3) 0.057(3) -0.003(3) 0.018(3) 0.000(3) C22 0.051(3) 0.058(4) 0.055(3) -0.005(3) 0.010(3) -0.006(3) C23 0.076(5) 0.123(7) 0.126(6) -0.055(5) -0.012(5) 0.023(4) C24 0.067(5) 0.155(9) 0.123(7) -0.067(6) -0.013(5) 0.004(5) C25 0.081(5) 0.117(7) 0.090(6) 0.010(5) -0.027(4) -0.005(5) C26 0.088(5) 0.110(7) 0.135(7) -0.002(6) -0.028(5) 0.022(5) C27 0.086(5) 0.075(5) 0.104(5) -0.015(4) -0.018(4) 0.006(4) C28 0.053(3) 0.086(5) 0.081(4) 0.003(4) 0.032(3) -0.002(3) C29 0.169(8) 0.108(7) 0.110(6) 0.021(5) 0.078(6) 0.015(6) C30 0.151(9) 0.222(14) 0.123(9) 0.069(9) 0.087(7) 0.042(9) C31 0.071(5) 0.259(16) 0.082(6) -0.022(8) 0.037(4) -0.014(7) C32 0.102(6) 0.186(11) 0.119(8) -0.073(7) 0.060(6) -0.031(7) C33 0.095(5) 0.098(6) 0.102(6) -0.029(4) 0.049(4) -0.017(4) C34 0.114(7) 0.370(18) 0.096(6) -0.012(9) 0.059(5) -0.027(9) C35 0.061(3) 0.036(3) 0.038(3) 0.005(2) 0.014(2) 0.006(2) C36 0.053(3) 0.041(3) 0.047(3) 0.003(2) 0.014(2) 0.004(2) C37 0.090(4) 0.052(3) 0.052(3) 0.008(3) 0.027(3) 0.005(3) C38 0.113(5) 0.082(5) 0.051(4) -0.001(3) 0.041(3) 0.008(4) C39 0.093(5) 0.077(5) 0.068(4) -0.021(4) 0.038(3) 0.003(4) C40 0.082(4) 0.049(3) 0.070(4) -0.011(3) 0.029(3) 0.009(3) C41 0.067(3) 0.045(3) 0.053(3) 0.003(2) 0.019(3) 0.004(2) C42 0.083(4) 0.051(4) 0.060(4) 0.007(3) 0.008(3) -0.013(3) C43 0.058(3) 0.059(4) 0.053(3) 0.000(3) 0.008(3) -0.012(3) C44 0.086(5) 0.073(4) 0.082(4) -0.003(3) -0.002(4) -0.029(4) C45 0.094(5) 0.088(6) 0.127(7) -0.025(5) -0.009(5) -0.032(5) C46 0.083(5) 0.125(8) 0.117(7) -0.026(6) -0.024(5) -0.002(5) C47 0.077(5) 0.092(6) 0.109(6) -0.005(4) -0.012(4) 0.012(4) C48 0.059(4) 0.071(4) 0.067(4) -0.002(3) 0.006(3) 0.004(3) C49 0.103(7) 0.076(6) 0.091(7) 0.000 0.036(6) 0.000 _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 Br1 C49 1.868(5) . ? S1 O8 1.411(4) . ? S1 O9 1.420(4) . ? S1 O7 1.597(4) . ? S1 C28 1.748(6) . ? O1 C7 1.361(6) . ? O1 C1 1.433(5) . ? O2 C7 1.191(6) . ? O3 C14 1.343(6) . ? O3 C2 1.438(5) . ? O4 C14 1.191(6) . ? O5 C21 1.366(6) . ? O5 C3 1.447(5) . ? O6 C21 1.181(6) . ? O7 C4 1.451(5) . ? O10 C35 1.353(5) . ? O10 C5 1.444(5) . ? O11 C35 1.197(5) . ? O12 C42 1.360(6) . ? O12 C6 1.430(5) . ? O13 C42 1.203(7) . ? C1 C2 1.501(6) . ? C1 C6 1.514(6) . ? C2 C3 1.514(6) . ? C3 C4 1.491(6) . ? C4 C5 1.501(6) . ? C5 C6 1.524(6) . ? C7 C8 1.485(7) . ? C8 C9 1.345(9) . ? C8 C13 1.378(9) . ? C9 C10 1.378(11) . ? C10 C11 1.351(15) . ? C11 C12 1.340(15) . ? C12 C13 1.394(11) . ? C14 C15 1.478(7) . ? C15 C16 1.370(7) . ? C15 C20 1.372(7) . ? C16 C17 1.389(8) . ? C17 C18 1.364(8) . ? C18 C19 1.360(8) . ? C19 C20 1.385(7) . ? C21 C22 1.458(7) . ? C22 C23 1.339(8) . ? C22 C27 1.357(8) . ? C23 C24 1.390(10) . ? C24 C25 1.302(10) . ? C25 C26 1.400(11) . ? C26 C27 1.385(9) . ? C28 C29 1.372(10) . ? C28 C33 1.382(9) . ? C29 C30 1.407(13) . ? C30 C31 1.381(15) . ? C31 C32 1.339(14) . ? C31 C34 1.513(13) . ? C32 C33 1.358(12) . ? C35 C36 1.470(7) . ? C36 C41 1.387(7) . ? C36 C37 1.393(7) . ? C37 C38 1.385(8) . ? C38 C39 1.382(8) . ? C39 C40 1.369(8) . ? C40 C41 1.360(7) . ? C42 C43 1.464(8) . ? C43 C48 1.374(7) . ? C43 C44 1.377(8) . ? C44 C45 1.378(9) . ? C45 C46 1.359(10) . ? C46 C47 1.389(10) . ? C47 C48 1.360(8) . ? C49 Br1 1.868(5) 2 ? 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 O8 S1 O9 119.8(3) . . ? O8 S1 O7 105.7(2) . . ? O9 S1 O7 108.8(2) . . ? O8 S1 C28 109.2(3) . . ? O9 S1 C28 110.5(3) . . ? O7 S1 C28 101.0(2) . . ? C7 O1 C1 116.1(4) . . ? C14 O3 C2 119.0(4) . . ? C21 O5 C3 117.8(4) . . ? C4 O7 S1 121.3(3) . . ? C35 O10 C5 118.0(3) . . ? C42 O12 C6 116.9(4) . . ? O1 C1 C2 111.5(3) . . ? O1 C1 C6 106.7(3) . . ? C2 C1 C6 110.4(4) . . ? O3 C2 C1 108.4(3) . . ? O3 C2 C3 108.1(3) . . ? C1 C2 C3 110.3(3) . . ? O5 C3 C4 108.0(3) . . ? O5 C3 C2 108.9(3) . . ? C4 C3 C2 111.0(4) . . ? O7 C4 C3 109.3(3) . . ? O7 C4 C5 107.9(4) . . ? C3 C4 C5 109.9(4) . . ? O10 C5 C4 108.8(4) . . ? O10 C5 C6 107.9(4) . . ? C4 C5 C6 110.3(4) . . ? O12 C6 C1 110.4(4) . . ? O12 C6 C5 108.3(3) . . ? C1 C6 C5 109.5(4) . . ? O2 C7 O1 122.8(5) . . ? O2 C7 C8 125.4(5) . . ? O1 C7 C8 111.8(5) . . ? C9 C8 C13 119.4(6) . . ? C9 C8 C7 122.9(6) . . ? C13 C8 C7 117.7(6) . . ? C8 C9 C10 120.7(9) . . ? C11 C10 C9 120.5(10) . . ? C12 C11 C10 119.5(10) . . ? C11 C12 C13 121.1(11) . . ? C8 C13 C12 118.7(9) . . ? O4 C14 O3 122.3(5) . . ? O4 C14 C15 125.3(5) . . ? O3 C14 C15 112.3(4) . . ? C16 C15 C20 119.5(5) . . ? C16 C15 C14 117.7(5) . . ? C20 C15 C14 122.7(4) . . ? C15 C16 C17 119.9(5) . . ? C18 C17 C16 120.1(6) . . ? C19 C18 C17 120.2(5) . . ? C18 C19 C20 120.0(5) . . ? C15 C20 C19 120.3(5) . . ? O6 C21 O5 121.8(5) . . ? O6 C21 C22 125.6(5) . . ? O5 C21 C22 112.6(5) . . ? C23 C22 C27 117.3(6) . . ? C23 C22 C21 119.8(5) . . ? C27 C22 C21 122.8(5) . . ? C22 C23 C24 123.1(7) . . ? C25 C24 C23 119.2(7) . . ? C24 C25 C26 120.4(7) . . ? C27 C26 C25 118.5(7) . . ? C22 C27 C26 121.2(7) . . ? C29 C28 C33 119.8(7) . . ? C29 C28 S1 119.5(6) . . ? C33 C28 S1 120.8(5) . . ? C28 C29 C30 118.9(9) . . ? C31 C30 C29 120.4(10) . . ? C32 C31 C30 118.2(9) . . ? C32 C31 C34 120.7(14) . . ? C30 C31 C34 121.1(14) . . ? C31 C32 C33 123.3(10) . . ? C32 C33 C28 119.3(8) . . ? O11 C35 O10 122.9(4) . . ? O11 C35 C36 125.4(4) . . ? O10 C35 C36 111.7(4) . . ? C41 C36 C37 119.3(5) . . ? C41 C36 C35 122.3(4) . . ? C37 C36 C35 118.4(4) . . ? C38 C37 C36 119.2(5) . . ? C39 C38 C37 119.7(5) . . ? C40 C39 C38 121.2(5) . . ? C41 C40 C39 119.2(5) . . ? C40 C41 C36 121.4(5) . . ? O13 C42 O12 121.2(5) . . ? O13 C42 C43 124.8(5) . . ? O12 C42 C43 114.0(5) . . ? C48 C43 C44 120.3(5) . . ? C48 C43 C42 122.7(5) . . ? C44 C43 C42 117.0(5) . . ? C43 C44 C45 120.2(7) . . ? C46 C45 C44 119.7(7) . . ? C45 C46 C47 119.7(7) . . ? C48 C47 C46 121.0(7) . . ? C47 C48 C43 119.1(6) . . ? Br1 C49 Br1 113.7(5) 2 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.709 _refine_diff_density_min -1.161 _refine_diff_density_rms 0.066