Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'John A. Ripmeester' _publ_contact_author_address ;Steacie Institute for Molecular Sciences National Research Council Canada 100 Sussex Drive Ottawa ON CANADA K1A OR6 ; _publ_contact_author_email John.Ripmeester@nrc-cnrc.gc.ca _publ_contact_author_phone 1-613-993-2011 _publ_contact_author_fax 1-613-998-7833 loop_ _publ_author_name _publ_author_address P.O.Brown ;Steacie Institute for Molecular Sciences National Research Council Canada 100 Sussex Drive Ottawa ON CANADA K1A OR6 ; G.D.Enright ;Steacie Institute for Molecular Sciences National Research Council Canada 100 Sussex Drive Ottawa ON CANADA K1A OR6 ; J.A.Ripmeester ;Steacie Institute for Molecular Sciences National Research Council Canada 100 Sussex Drive Ottawa ON CANADA K1A OR6 ; data_sadf _database_code_depnum_ccdc_archive 'CCDC 292516' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2*(methylpyrogall[4]arene)1*(1,3-bis(3-pyridylmethyl)-2-thiourea)1*(SO4 2-)1*H2O clathrate ; _chemical_name_common ; 2*(methylpyrogall(4)arene)1*(1,3-bis(3-pyridylmethyl)-2- thiourea)1*(SO4 2-)1*H2O clathrate ; _chemical_melting_point ? _chemical_formula_moiety '2(C32 H32 O12), 1(C13 H16 N4 S1), 1(SO4 2-), 1(H2 O)' _chemical_formula_sum 'C77 H82 N4 O29 S2' _chemical_formula_weight 1591.59 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' 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 9.5012(6) _cell_length_b 18.1017(12) _cell_length_c 21.8277(14) _cell_angle_alpha 70.0560(10) _cell_angle_beta 82.3200(10) _cell_angle_gamma 83.1340(10) _cell_volume 3486.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour clear _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 0.173 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9214 _exptl_absorpt_correction_T_max 0.9728 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44480 _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_av_sigmaI/netI 0.1032 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 29.64 _reflns_number_total 19416 _reflns_number_gt 9855 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0413P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap+geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19416 _refine_ls_number_parameters 1376 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1249 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1039 _refine_ls_wR_factor_gt 0.0866 _refine_ls_goodness_of_fit_ref 0.887 _refine_ls_restrained_S_all 0.888 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 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 0.57531(7) 0.76675(4) 0.27872(3) 0.03793(16) Uani 1 1 d . A . O1 O 0.40568(17) 0.43273(10) -0.14359(7) 0.0333(4) Uani 1 1 d . . . O2 O 0.16378(19) 0.43560(9) -0.19566(7) 0.0335(4) Uani 1 1 d . . . O3 O -0.08404(17) 0.40019(10) -0.12294(7) 0.0370(4) Uani 1 1 d . . . O4 O -0.10859(18) 0.24217(9) -0.04342(7) 0.0343(4) Uani 1 1 d . . . O5 O -0.07695(19) 0.07505(10) 0.02263(8) 0.0403(4) Uani 1 1 d . . . O6 O -0.06303(18) 0.01914(9) 0.15195(8) 0.0340(4) Uani 1 1 d . . . O7 O 0.01445(16) -0.05489(9) 0.28405(8) 0.0277(4) Uani 1 1 d . . . O8 O 0.29032(17) -0.12173(9) 0.28441(7) 0.0295(4) Uani 1 1 d . . . O9 O 0.51364(15) -0.03238(9) 0.23578(7) 0.0262(3) Uani 1 1 d . . . O10 O 0.59202(17) 0.05798(9) 0.10437(8) 0.0322(4) Uani 1 1 d . . . O11 O 0.61710(19) 0.12671(10) -0.01976(8) 0.0406(5) Uani 1 1 d . . . O12 O 0.54817(18) 0.29282(9) -0.07731(7) 0.0343(4) Uani 1 1 d . . . O13 O 0.92066(15) 0.93641(9) 0.41010(7) 0.0288(4) Uani 1 1 d . . . O14 O 0.70857(17) 0.97129(9) 0.32773(7) 0.0288(4) Uani 1 1 d . . . O15 O 0.43852(16) 0.93529(10) 0.37409(7) 0.0292(4) Uani 1 1 d . . . O16 O 0.40255(17) 0.77427(9) 0.41861(7) 0.0298(4) Uani 1 1 d . . . O17 O 0.43481(17) 0.61678(9) 0.44821(7) 0.0312(4) Uani 1 1 d . . . O18 O 0.41640(16) 0.51829(9) 0.57405(8) 0.0291(4) Uani 1 1 d . . . O19 O 0.42875(17) 0.41760(10) 0.70526(7) 0.0312(4) Uani 1 1 d . . . O20 O 0.69325(17) 0.34312(9) 0.72655(8) 0.0309(4) Uani 1 1 d . . . O21 O 0.91461(18) 0.42446(9) 0.73887(8) 0.0339(4) Uani 1 1 d . . . O22 O 1.03792(16) 0.53571(9) 0.62691(7) 0.0297(4) Uani 1 1 d . . . O23 O 1.09475(16) 0.62397(9) 0.50613(7) 0.0284(4) Uani 1 1 d . . . O24 O 1.03888(16) 0.78379(9) 0.46583(7) 0.0285(4) Uani 1 1 d . . . N1 N 0.8392(2) 0.55115(12) 0.45224(10) 0.0342(5) Uani 1 1 d . . . N2 N 0.8477(2) 0.76709(13) 0.29551(10) 0.0400(5) Uani 1 1 d . A . N4 N 0.6978(2) 0.96473(13) 0.02254(10) 0.0403(5) Uani 1 1 d . . . O1W O 0.1463(2) 0.70595(12) 0.37486(8) 0.0414(5) Uani 1 1 d . . . C1 C 0.2844(2) 0.41373(11) -0.09998(10) 0.0249(5) Uani 1 1 d . . . C2 C 0.1610(2) 0.41764(12) -0.12905(10) 0.0262(5) Uani 1 1 d . . . C3 C 0.0335(2) 0.39869(12) -0.09084(10) 0.0265(5) Uani 1 1 d . . . C4 C 0.0278(2) 0.37516(12) -0.02259(10) 0.0252(5) Uani 1 1 d . . . C5 C 0.1541(2) 0.37111(11) 0.00471(10) 0.0240(5) Uani 1 1 d . . . C6 C 0.2837(2) 0.39041(11) -0.03218(9) 0.0225(4) Uani 1 1 d . . . C7 C -0.1104(2) 0.35155(13) 0.02165(10) 0.0268(5) Uani 1 1 d . . . C8 C -0.1464(3) 0.40117(15) 0.06683(13) 0.0353(6) Uani 1 1 d . . . C9 C -0.0987(2) 0.21144(13) 0.02303(9) 0.0256(5) Uani 1 1 d . . . C10 C -0.0861(2) 0.13024(13) 0.05365(10) 0.0271(5) Uani 1 1 d . . . C11 C -0.0759(2) 0.10035(12) 0.12101(10) 0.0253(5) Uani 1 1 d . . . C12 C -0.0748(2) 0.14964(12) 0.15741(9) 0.0226(5) Uani 1 1 d . . . C13 C -0.0883(2) 0.23057(13) 0.12496(10) 0.0229(5) Uani 1 1 d . . . C14 C -0.1007(2) 0.26304(12) 0.05792(9) 0.0228(5) Uani 1 1 d . . . C15 C -0.0525(2) 0.11467(13) 0.22978(10) 0.0248(5) Uani 1 1 d . . . C16 C -0.0883(3) 0.17269(16) 0.26697(12) 0.0340(6) Uani 1 1 d . . . C17 C 0.1247(2) -0.00528(12) 0.25991(9) 0.0224(4) Uani 1 1 d . . . C18 C 0.2618(2) -0.04157(12) 0.26115(9) 0.0230(5) Uani 1 1 d . . . C19 C 0.3770(2) 0.00430(12) 0.23902(9) 0.0228(5) Uani 1 1 d . . . C20 C 0.3583(2) 0.08630(12) 0.21929(9) 0.0210(4) Uani 1 1 d . . . C21 C 0.2181(2) 0.12037(12) 0.21740(9) 0.0219(4) Uani 1 1 d . . . C22 C 0.0996(2) 0.07607(12) 0.23670(9) 0.0211(4) Uani 1 1 d . . . C23 C 0.4866(2) 0.13593(12) 0.19954(9) 0.0229(5) Uani 1 1 d . . . C24 C 0.4829(3) 0.18898(15) 0.24111(12) 0.0328(6) Uani 1 1 d . . . C25 C 0.5544(2) 0.13800(12) 0.08397(10) 0.0245(5) Uani 1 1 d . . . C26 C 0.5690(2) 0.17483(12) 0.01649(10) 0.0257(5) Uani 1 1 d . . . C27 C 0.5337(2) 0.25504(12) -0.01000(10) 0.0251(5) Uani 1 1 d . . . C28 C 0.4737(2) 0.29848(11) 0.03052(10) 0.0224(4) Uani 1 1 d . . . C29 C 0.4602(2) 0.25938(12) 0.09795(10) 0.0231(5) Uani 1 1 d . . . C30 C 0.5017(2) 0.17972(12) 0.12602(9) 0.0211(4) Uani 1 1 d . . . C31 C 0.4195(2) 0.38460(12) 0.00043(10) 0.0245(5) Uani 1 1 d . . . C32 C 0.3949(3) 0.42952(14) 0.04919(12) 0.0307(5) Uani 1 1 d . . . C33 C 0.7824(2) 0.91922(11) 0.43510(9) 0.0223(4) Uani 1 1 d . . . C34 C 0.6746(2) 0.93673(11) 0.39395(9) 0.0219(4) Uani 1 1 d . . . C35 C 0.5380(2) 0.91649(11) 0.41931(9) 0.0221(4) Uani 1 1 d . . . C36 C 0.5046(2) 0.87868(11) 0.48587(9) 0.0214(4) Uani 1 1 d . . . C37 C 0.6147(2) 0.86288(12) 0.52624(10) 0.0225(5) Uani 1 1 d . . . C38 C 0.7531(2) 0.88266(11) 0.50263(9) 0.0207(4) Uani 1 1 d . . . C39 C 0.3563(2) 0.85168(12) 0.51228(10) 0.0230(5) Uani 1 1 d . . . C40 C 0.2883(3) 0.88372(15) 0.56636(12) 0.0334(6) Uani 1 1 d . . . C41 C 0.3910(2) 0.72727(12) 0.48353(9) 0.0221(4) Uani 1 1 d . . . C42 C 0.4078(2) 0.64603(12) 0.49963(10) 0.0239(5) Uani 1 1 d . . . C43 C 0.3968(2) 0.59841(12) 0.56487(10) 0.0226(4) Uani 1 1 d . . . C44 C 0.3694(2) 0.63125(11) 0.61485(9) 0.0218(4) Uani 1 1 d . . . C45 C 0.3533(2) 0.71305(12) 0.59680(10) 0.0226(4) Uani 1 1 d . . . C46 C 0.3640(2) 0.76253(11) 0.53176(10) 0.0215(4) Uani 1 1 d . . . C47 C 0.3609(2) 0.57863(12) 0.68670(10) 0.0243(5) Uani 1 1 d . . . C48 C 0.2966(3) 0.62127(14) 0.73464(11) 0.0307(5) Uani 1 1 d . . . C49 C 0.5374(2) 0.45846(12) 0.71163(9) 0.0247(5) Uani 1 1 d . . . C50 C 0.6713(2) 0.42064(12) 0.72431(9) 0.0261(5) Uani 1 1 d . . . C51 C 0.7789(2) 0.46234(13) 0.73064(9) 0.0267(5) Uani 1 1 d . . . C52 C 0.7544(2) 0.54232(12) 0.72319(9) 0.0242(5) Uani 1 1 d . . . C53 C 0.6187(2) 0.57851(12) 0.70909(9) 0.0242(5) Uani 1 1 d . . . C54 C 0.5082(2) 0.53822(12) 0.70344(9) 0.0234(5) Uani 1 1 d . . . C55 C 0.8740(2) 0.59008(13) 0.72665(10) 0.0262(5) Uani 1 1 d . . . C56 C 0.8369(3) 0.62881(15) 0.77918(11) 0.0340(6) Uani 1 1 d . . . C57 C 0.9951(2) 0.61509(12) 0.61292(10) 0.0237(5) Uani 1 1 d . . . C58 C 1.0307(2) 0.66178(12) 0.54903(10) 0.0231(5) Uani 1 1 d . . . C59 C 0.9950(2) 0.74272(12) 0.53006(9) 0.0230(5) Uani 1 1 d . . . C60 C 0.9164(2) 0.77723(12) 0.57383(9) 0.0232(5) Uani 1 1 d . . . C61 C 0.8801(2) 0.72764(13) 0.63734(10) 0.0241(5) Uani 1 1 d . . . C62 C 0.9189(2) 0.64655(12) 0.65832(9) 0.0233(5) Uani 1 1 d . . . C63 C 0.8696(2) 0.86561(12) 0.54890(10) 0.0239(5) Uani 1 1 d . . . C64 C 0.8222(3) 0.90190(15) 0.60280(12) 0.0339(6) Uani 1 1 d . . . C65 C 0.8466(3) 0.62047(14) 0.40320(12) 0.0319(5) Uani 1 1 d . . . C66 C 0.7988(2) 0.68998(13) 0.41439(11) 0.0290(5) Uani 1 1 d . . . C67 C 0.7426(2) 0.68535(15) 0.47732(12) 0.0320(5) Uani 1 1 d . . . C68 C 0.7370(3) 0.61369(16) 0.52698(13) 0.0363(6) Uani 1 1 d . . . C69 C 0.7858(3) 0.54626(16) 0.51334(12) 0.0370(6) Uani 1 1 d . . . C70 C 0.8108(3) 0.76949(14) 0.36140(12) 0.0360(6) Uani 1 1 d . . . C71 C 0.7519(3) 0.76944(13) 0.25525(11) 0.0361(6) Uani 1 1 d . . . C73 C 0.7219(3) 0.95292(16) -0.03528(13) 0.0386(6) Uani 1 1 d . . . C74 C 0.7517(2) 0.87714(16) -0.03620(12) 0.0359(6) Uani 1 1 d . . . C75 C 0.7565(2) 0.81562(15) 0.02231(12) 0.0338(6) Uani 1 1 d . A . C76 C 0.7310(3) 0.82975(14) 0.08122(11) 0.0402(6) Uani 1 1 d D . . C77 C 0.7025(3) 0.90644(15) 0.07951(13) 0.0473(7) Uani 1 1 d . A . N3A N 0.8235(14) 0.7825(9) 0.1929(6) 0.036(2) Uani 0.47(3) 1 d PD A -1 H3A H 0.896(7) 0.7997(18) 0.1846(9) 0.044 Uiso 0.47(3) 1 calc PR A -1 C72A C 0.7615(18) 0.7637(6) 0.1448(5) 0.042(3) Uani 0.47(3) 1 d PD A -1 H72A H 0.674(4) 0.7414(12) 0.1647(10) 0.051 Uiso 0.47(3) 1 calc PR A -1 H72B H 0.823(4) 0.724(2) 0.1336(8) 0.051 Uiso 0.47(3) 1 calc PR A -1 N3B N 0.7845(18) 0.7688(11) 0.1947(6) 0.053(4) Uani 0.53(3) 1 d PD A -2 H3B H 0.884(7) 0.7735(11) 0.1795(12) 0.063 Uiso 0.53(3) 1 calc PR A -2 C72B C 0.700(2) 0.7625(6) 0.1470(4) 0.049(3) Uani 0.53(3) 1 d PD A -2 H72C H 0.603(5) 0.7663(6) 0.1617(7) 0.059 Uiso 0.53(3) 1 calc PR A -2 H72D H 0.722(2) 0.7137(19) 0.1409(4) 0.059 Uiso 0.53(3) 1 calc PR A -2 S2A S 0.19095(17) 0.82540(8) 0.15813(5) 0.0241(3) Uani 0.715(3) 1 d PD B -3 O1S O 0.2344(3) 0.74412(15) 0.15637(10) 0.0361(7) Uani 0.715(3) 1 d PD B -3 O2S O 0.3152(2) 0.87054(14) 0.13899(10) 0.0373(7) Uani 0.715(3) 1 d PD B -3 O3S O 0.0781(6) 0.8606(4) 0.1122(3) 0.0331(4) Uani 0.715(3) 1 d PD B -3 O4S O 0.1290(7) 0.8172(4) 0.2272(2) 0.0331(4) Uani 0.715(3) 1 d PD B -3 S2B S 0.1379(4) 0.8029(2) 0.16800(17) 0.0362(8) Uani 0.285(3) 1 d PD B -4 O5S O 0.0928(17) 0.8720(10) 0.1128(7) 0.0331(4) Uani 0.285(3) 1 d PD B -4 O6S O 0.1142(18) 0.8278(11) 0.2224(6) 0.0331(4) Uani 0.285(3) 1 d PD B -4 O7S O 0.0674(6) 0.7318(3) 0.1786(3) 0.0365(17) Uani 0.285(3) 1 d PD B -4 O8S O 0.2973(7) 0.7854(4) 0.1528(3) 0.0393(18) Uani 0.285(3) 1 d PD B -4 H39 H 0.294(2) 0.8738(11) 0.4777(9) 0.016(5) Uiso 1 1 d . . . H15 H -0.119(2) 0.0713(12) 0.2499(9) 0.024(6) Uiso 1 1 d . . . H45 H 0.330(2) 0.7349(11) 0.6316(9) 0.017(5) Uiso 1 1 d . . . H47 H 0.293(2) 0.5384(11) 0.6913(9) 0.019(5) Uiso 1 1 d . . . H55 H 0.959(2) 0.5535(11) 0.7399(8) 0.015(5) Uiso 1 1 d . . . H31 H 0.498(2) 0.4110(11) -0.0360(9) 0.023(5) Uiso 1 1 d . . . H58A H 0.745(3) 0.6639(13) 0.7731(10) 0.038(7) Uiso 1 1 d . . . H61 H 0.826(2) 0.7495(11) 0.6690(9) 0.021(5) Uiso 1 1 d . . . H48C H 0.201(2) 0.6454(12) 0.7246(9) 0.026(6) Uiso 1 1 d . . . H24B H 0.563(3) 0.2224(14) 0.2250(11) 0.039(7) Uiso 1 1 d . . . H29 H 0.422(2) 0.2883(12) 0.1269(10) 0.027(6) Uiso 1 1 d . . . H21 H 0.202(2) 0.1771(12) 0.2015(9) 0.019(5) Uiso 1 1 d . . . H53 H 0.601(2) 0.6341(12) 0.7015(9) 0.021(5) Uiso 1 1 d . . . H64A H 0.800(2) 0.9565(15) 0.5825(11) 0.041(7) Uiso 1 1 d . . . H48B H 0.358(2) 0.6620(12) 0.7365(9) 0.023(6) Uiso 1 1 d . . . H23 H 0.575(2) 0.1001(11) 0.2096(9) 0.017(5) Uiso 1 1 d . . . H5 H 0.152(2) 0.3540(11) 0.0534(10) 0.026(6) Uiso 1 1 d . . . H018 H 0.407(3) 0.4935(14) 0.6129(12) 0.039(8) Uiso 1 1 d . . . H58C H 0.818(2) 0.5866(14) 0.8221(12) 0.042(7) Uiso 1 1 d . . . H010 H 0.571(3) 0.0366(15) 0.1457(13) 0.058(9) Uiso 1 1 d . . . H13 H -0.086(2) 0.2644(12) 0.1508(10) 0.026(6) Uiso 1 1 d . . . H24C H 0.395(3) 0.2230(14) 0.2392(11) 0.045(7) Uiso 1 1 d . . . H63 H 0.954(2) 0.8927(11) 0.5239(9) 0.019(5) Uiso 1 1 d . . . H40C H 0.279(3) 0.9385(16) 0.5489(12) 0.049(8) Uiso 1 1 d . . . H16B H -0.185(3) 0.1941(13) 0.2627(10) 0.038(7) Uiso 1 1 d . . . H7 H -0.190(2) 0.3633(12) -0.0075(10) 0.032(6) Uiso 1 1 d . . . H32A H 0.481(3) 0.4275(13) 0.0719(11) 0.045(7) Uiso 1 1 d . . . H024 H 1.009(3) 0.8321(14) 0.4559(11) 0.040(7) Uiso 1 1 d . . . H58B H 0.919(3) 0.6577(15) 0.7824(12) 0.058(8) Uiso 1 1 d . . . H37 H 0.5915(19) 0.8323(11) 0.5724(9) 0.013(5) Uiso 1 1 d . . . H8A H -0.234(2) 0.3862(12) 0.0934(10) 0.031(6) Uiso 1 1 d . . . H01 H 0.475(3) 0.3959(15) -0.1282(12) 0.052(8) Uiso 1 1 d . . . H8B H -0.073(2) 0.3921(12) 0.0983(10) 0.033(6) Uiso 1 1 d . . . H016 H 0.438(3) 0.7482(15) 0.3940(12) 0.045(8) Uiso 1 1 d . . . H02 H 0.247(3) 0.4352(16) -0.2113(13) 0.058(10) Uiso 1 1 d . . . H24A H 0.494(2) 0.1563(13) 0.2875(11) 0.040(7) Uiso 1 1 d . . . H40B H 0.352(2) 0.8696(12) 0.6024(10) 0.028(6) Uiso 1 1 d . . . H019 H 0.460(3) 0.3736(17) 0.7084(14) 0.070(10) Uiso 1 1 d . . . H011 H 0.623(3) 0.1465(15) -0.0589(13) 0.053(9) Uiso 1 1 d . . . H32B H 0.319(3) 0.4102(14) 0.0854(12) 0.049(7) Uiso 1 1 d . . . H09 H 0.510(3) -0.0798(14) 0.2436(11) 0.039(8) Uiso 1 1 d . . . H64B H 0.733(3) 0.8791(14) 0.6306(12) 0.048(7) Uiso 1 1 d . . . H05 H -0.085(3) 0.0962(16) -0.0177(13) 0.059(9) Uiso 1 1 d . . . H8C H -0.161(2) 0.4587(15) 0.0413(11) 0.048(7) Uiso 1 1 d . . . H48A H 0.284(2) 0.5838(13) 0.7798(11) 0.037(6) Uiso 1 1 d . . . H16A H -0.016(2) 0.2139(13) 0.2538(10) 0.035(7) Uiso 1 1 d . . . H40A H 0.191(3) 0.8662(13) 0.5806(11) 0.042(7) Uiso 1 1 d . . . H32C H 0.365(2) 0.4859(14) 0.0277(10) 0.035(6) Uiso 1 1 d . . . H014 H 0.639(3) 0.9713(14) 0.3078(12) 0.046(8) Uiso 1 1 d . . . H022 H 1.008(3) 0.5088(14) 0.6653(12) 0.045(8) Uiso 1 1 d . . . H017 H 0.459(3) 0.5655(16) 0.4633(13) 0.060(9) Uiso 1 1 d . . . H012 H 0.621(3) 0.2707(18) -0.0997(14) 0.080(10) Uiso 1 1 d . . . H08 H 0.242(3) -0.1432(16) 0.2656(12) 0.056(9) Uiso 1 1 d . . . H07 H -0.026(3) -0.0509(17) 0.2540(14) 0.071(11) Uiso 1 1 d . . . H013 H 0.928(3) 0.9438(14) 0.3698(12) 0.047(8) Uiso 1 1 d . . . H06 H -0.048(3) -0.0024(17) 0.1219(14) 0.070(10) Uiso 1 1 d . . . H64C H 0.897(3) 0.8908(14) 0.6338(12) 0.051(7) Uiso 1 1 d . . . H023 H 1.111(3) 0.6564(17) 0.4689(14) 0.074(11) Uiso 1 1 d . . . H16C H -0.084(3) 0.1448(15) 0.3142(13) 0.056(8) Uiso 1 1 d . . . H020 H 0.714(3) 0.3163(19) 0.7635(15) 0.090(12) Uiso 1 1 d . . . H021 H 0.933(4) 0.419(2) 0.7725(15) 0.088(13) Uiso 1 1 d . . . H015 H 0.402(3) 0.8899(16) 0.3800(13) 0.064(9) Uiso 1 1 d . . . H03 H -0.121(4) 0.354(2) -0.1028(19) 0.135(16) Uiso 1 1 d . . . H69 H 0.781(2) 0.4954(13) 0.5466(10) 0.032(6) Uiso 1 1 d . . . H65 H 0.889(2) 0.6183(12) 0.3618(10) 0.028(6) Uiso 1 1 d . . . H67 H 0.708(2) 0.7332(13) 0.4851(10) 0.034(6) Uiso 1 1 d . . . H1N H 0.873(3) 0.5089(14) 0.4404(11) 0.041(7) Uiso 1 1 d . . . H68 H 0.698(3) 0.6102(14) 0.5667(12) 0.042(7) Uiso 1 1 d . . . H70B H 0.715(2) 0.8019(12) 0.3629(9) 0.030(6) Uiso 1 1 d . . . H70A H 0.885(3) 0.7958(14) 0.3702(11) 0.050(8) Uiso 1 1 d . . . H2N H 0.932(3) 0.7730(17) 0.2787(14) 0.069(11) Uiso 1 1 d . . . H73 H 0.716(2) 0.9994(13) -0.0748(11) 0.038(7) Uiso 1 1 d . . . H74 H 0.769(2) 0.8657(14) -0.0759(11) 0.044(7) Uiso 1 1 d . . . H4N H 0.675(3) 1.0101(16) 0.0243(12) 0.056(9) Uiso 1 1 d . . . H2W H 0.177(4) 0.747(2) 0.3758(16) 0.095(14) Uiso 1 1 d . . . H1W H 0.204(3) 0.6870(16) 0.3450(14) 0.062(9) Uiso 1 1 d . . . H75 H 0.785(2) 0.7619(13) 0.0227(10) 0.030(6) Uiso 1 1 d . . . H77 H 0.684(3) 0.9184(15) 0.1178(13) 0.056(8) Uiso 1 1 d . . . H04 H -0.102(5) 0.207(3) -0.066(2) 0.166(19) Uiso 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 0.0404(4) 0.0296(3) 0.0458(4) -0.0126(3) -0.0136(3) -0.0002(3) O1 0.0306(10) 0.0344(9) 0.0254(8) 0.0003(7) 0.0023(7) -0.0027(8) O2 0.0334(10) 0.0382(10) 0.0209(8) -0.0004(7) -0.0004(7) -0.0027(8) O3 0.0304(10) 0.0390(10) 0.0314(9) 0.0044(8) -0.0098(7) -0.0048(8) O4 0.0553(11) 0.0309(9) 0.0175(7) -0.0056(7) -0.0079(7) -0.0094(8) O5 0.0599(12) 0.0401(10) 0.0263(9) -0.0129(8) -0.0072(8) -0.0156(9) O6 0.0466(11) 0.0252(9) 0.0300(9) -0.0057(7) -0.0089(8) -0.0069(7) O7 0.0233(9) 0.0298(9) 0.0263(8) -0.0040(7) -0.0012(7) -0.0052(7) O8 0.0321(9) 0.0207(8) 0.0336(9) -0.0040(7) -0.0103(7) -0.0006(7) O9 0.0228(8) 0.0214(8) 0.0303(8) -0.0045(7) -0.0029(6) 0.0025(7) O10 0.0412(10) 0.0213(8) 0.0272(9) -0.0045(7) 0.0049(7) 0.0039(7) O11 0.0571(12) 0.0302(9) 0.0291(10) -0.0112(8) 0.0062(8) 0.0092(8) O12 0.0397(10) 0.0318(9) 0.0228(8) -0.0037(7) 0.0049(7) 0.0057(8) O13 0.0255(9) 0.0351(9) 0.0226(8) -0.0047(7) -0.0011(7) -0.0065(7) O14 0.0258(9) 0.0361(9) 0.0196(8) -0.0011(6) -0.0040(7) -0.0058(7) O15 0.0267(9) 0.0316(9) 0.0249(8) -0.0021(7) -0.0069(6) -0.0028(7) O16 0.0407(10) 0.0260(8) 0.0209(8) -0.0063(7) -0.0021(7) -0.0012(7) O17 0.0433(10) 0.0234(9) 0.0276(8) -0.0104(7) -0.0053(7) 0.0026(7) O18 0.0392(10) 0.0200(8) 0.0267(9) -0.0053(7) -0.0056(7) -0.0010(7) O19 0.0352(10) 0.0203(8) 0.0353(9) -0.0050(7) -0.0057(7) -0.0015(7) O20 0.0415(10) 0.0222(8) 0.0272(9) -0.0070(7) -0.0066(7) 0.0051(7) O21 0.0355(10) 0.0327(9) 0.0337(10) -0.0112(8) -0.0134(8) 0.0081(7) O22 0.0369(10) 0.0230(8) 0.0236(8) -0.0038(7) 0.0022(7) 0.0023(7) O23 0.0287(9) 0.0308(9) 0.0234(8) -0.0080(7) 0.0013(7) -0.0008(7) O24 0.0313(9) 0.0261(9) 0.0232(8) -0.0036(7) -0.0004(6) 0.0008(7) N1 0.0316(12) 0.0298(11) 0.0461(13) -0.0185(10) -0.0089(9) 0.0016(9) N2 0.0321(13) 0.0446(13) 0.0373(12) -0.0090(10) -0.0035(10) 0.0070(10) N4 0.0468(14) 0.0275(12) 0.0482(14) -0.0160(11) -0.0078(10) 0.0043(10) O1W 0.0484(12) 0.0447(12) 0.0286(9) -0.0122(8) 0.0024(8) -0.0008(10) C1 0.0266(12) 0.0163(10) 0.0276(11) -0.0035(9) 0.0029(9) -0.0032(9) C2 0.0336(13) 0.0195(11) 0.0205(10) -0.0006(8) -0.0035(9) -0.0004(9) C3 0.0290(13) 0.0206(11) 0.0254(11) -0.0015(9) -0.0048(9) -0.0005(9) C4 0.0264(12) 0.0191(11) 0.0260(11) -0.0038(9) -0.0015(9) 0.0017(9) C5 0.0306(13) 0.0154(10) 0.0219(11) -0.0030(8) -0.0015(9) 0.0026(9) C6 0.0266(12) 0.0141(10) 0.0240(10) -0.0038(8) -0.0005(9) -0.0011(8) C7 0.0203(12) 0.0290(12) 0.0257(11) -0.0039(9) -0.0022(9) 0.0029(9) C8 0.0347(15) 0.0284(14) 0.0352(14) -0.0063(11) 0.0034(12) 0.0068(11) C9 0.0244(12) 0.0341(13) 0.0181(10) -0.0055(9) -0.0045(8) -0.0081(10) C10 0.0283(13) 0.0322(13) 0.0236(11) -0.0106(10) -0.0035(9) -0.0078(10) C11 0.0233(12) 0.0240(11) 0.0252(11) -0.0018(9) -0.0036(9) -0.0064(9) C12 0.0178(11) 0.0294(12) 0.0193(10) -0.0061(9) -0.0018(8) -0.0031(9) C13 0.0196(11) 0.0262(12) 0.0213(10) -0.0067(9) -0.0017(8) 0.0003(9) C14 0.0161(11) 0.0281(12) 0.0216(10) -0.0049(9) -0.0008(8) -0.0032(9) C15 0.0202(12) 0.0301(12) 0.0206(10) -0.0048(9) -0.0019(9) 0.0011(10) C16 0.0283(14) 0.0466(16) 0.0257(13) -0.0131(11) -0.0053(10) 0.0089(12) C17 0.0227(12) 0.0270(11) 0.0165(10) -0.0050(8) -0.0011(8) -0.0055(9) C18 0.0290(12) 0.0205(11) 0.0180(10) -0.0035(8) -0.0050(8) -0.0015(9) C19 0.0196(11) 0.0273(11) 0.0196(10) -0.0055(9) -0.0054(8) 0.0031(9) C20 0.0231(11) 0.0240(11) 0.0148(9) -0.0051(8) -0.0022(8) -0.0020(9) C21 0.0263(12) 0.0206(11) 0.0175(10) -0.0049(9) -0.0030(8) 0.0006(9) C22 0.0237(11) 0.0255(11) 0.0133(9) -0.0056(8) -0.0035(8) 0.0008(9) C23 0.0214(12) 0.0217(11) 0.0242(11) -0.0054(9) -0.0041(9) -0.0012(9) C24 0.0352(15) 0.0343(14) 0.0296(13) -0.0104(11) -0.0066(11) -0.0024(12) C25 0.0206(11) 0.0202(11) 0.0294(11) -0.0052(9) 0.0005(9) -0.0011(9) C26 0.0236(12) 0.0263(12) 0.0266(11) -0.0109(9) 0.0048(9) -0.0012(9) C27 0.0214(11) 0.0268(12) 0.0228(11) -0.0039(9) 0.0013(9) -0.0023(9) C28 0.0181(11) 0.0199(11) 0.0284(11) -0.0066(9) -0.0025(9) -0.0020(8) C29 0.0208(11) 0.0249(11) 0.0248(11) -0.0102(9) 0.0001(9) -0.0037(9) C30 0.0146(10) 0.0233(11) 0.0245(10) -0.0065(9) 0.0000(8) -0.0039(8) C31 0.0238(12) 0.0232(11) 0.0249(11) -0.0064(9) 0.0008(9) -0.0037(9) C32 0.0360(15) 0.0252(13) 0.0301(13) -0.0080(10) -0.0023(11) -0.0033(11) C33 0.0214(11) 0.0204(11) 0.0249(11) -0.0077(9) 0.0005(9) -0.0035(9) C34 0.0278(12) 0.0178(10) 0.0186(10) -0.0045(8) -0.0015(9) -0.0012(9) C35 0.0254(12) 0.0176(10) 0.0230(10) -0.0064(8) -0.0050(9) 0.0015(9) C36 0.0244(12) 0.0161(10) 0.0228(10) -0.0062(8) -0.0008(9) -0.0001(8) C37 0.0303(13) 0.0175(10) 0.0184(10) -0.0049(8) -0.0002(9) -0.0020(9) C38 0.0247(12) 0.0171(10) 0.0210(10) -0.0070(8) -0.0029(8) -0.0009(8) C39 0.0221(11) 0.0191(11) 0.0236(11) -0.0025(9) -0.0026(9) 0.0021(9) C40 0.0353(15) 0.0268(14) 0.0330(13) -0.0082(11) 0.0055(11) 0.0017(11) C41 0.0181(11) 0.0238(11) 0.0212(10) -0.0027(9) -0.0019(8) -0.0030(9) C42 0.0217(11) 0.0271(12) 0.0237(11) -0.0096(9) -0.0036(9) -0.0001(9) C43 0.0196(11) 0.0185(10) 0.0289(11) -0.0061(9) -0.0042(9) -0.0016(8) C44 0.0170(11) 0.0211(11) 0.0223(10) -0.0010(8) -0.0020(8) -0.0012(8) C45 0.0193(11) 0.0246(11) 0.0236(11) -0.0084(9) 0.0000(8) -0.0011(9) C46 0.0150(10) 0.0195(10) 0.0278(11) -0.0050(9) -0.0021(8) -0.0016(8) C47 0.0248(12) 0.0204(11) 0.0247(11) -0.0041(9) 0.0006(9) -0.0038(9) C48 0.0328(14) 0.0279(13) 0.0267(12) -0.0062(10) 0.0007(10) 0.0029(11) C49 0.0288(12) 0.0243(11) 0.0185(10) -0.0040(9) -0.0012(9) -0.0035(9) C50 0.0363(14) 0.0213(11) 0.0199(10) -0.0069(9) -0.0036(9) 0.0020(10) C51 0.0294(13) 0.0295(12) 0.0176(10) -0.0054(9) -0.0053(9) 0.0081(10) C52 0.0302(12) 0.0259(11) 0.0148(10) -0.0049(8) -0.0011(9) -0.0023(9) C53 0.0312(13) 0.0179(11) 0.0195(10) -0.0029(9) -0.0001(9) 0.0007(9) C54 0.0274(12) 0.0216(11) 0.0167(10) -0.0029(8) 0.0007(8) 0.0011(9) C55 0.0284(13) 0.0279(12) 0.0208(11) -0.0064(9) -0.0041(9) 0.0011(10) C56 0.0438(17) 0.0348(14) 0.0234(12) -0.0103(11) -0.0019(11) -0.0032(13) C57 0.0236(12) 0.0232(11) 0.0246(11) -0.0066(9) -0.0071(9) -0.0012(9) C58 0.0174(11) 0.0284(12) 0.0249(11) -0.0107(9) -0.0030(8) -0.0002(9) C59 0.0216(11) 0.0273(12) 0.0181(10) -0.0038(9) -0.0039(8) -0.0035(9) C60 0.0210(11) 0.0263(11) 0.0236(11) -0.0077(9) -0.0076(9) -0.0025(9) C61 0.0225(12) 0.0300(12) 0.0218(11) -0.0111(9) -0.0042(9) 0.0005(9) C62 0.0229(11) 0.0269(11) 0.0192(10) -0.0056(9) -0.0058(8) -0.0006(9) C63 0.0256(12) 0.0234(11) 0.0224(11) -0.0060(9) -0.0046(9) -0.0034(9) C64 0.0428(16) 0.0313(14) 0.0313(13) -0.0142(11) -0.0107(12) 0.0023(12) C65 0.0305(13) 0.0338(14) 0.0363(13) -0.0171(11) -0.0077(11) 0.0002(10) C66 0.0214(12) 0.0347(13) 0.0375(13) -0.0194(11) -0.0101(10) 0.0023(10) C67 0.0204(12) 0.0415(15) 0.0438(14) -0.0259(12) -0.0076(10) 0.0005(11) C68 0.0260(13) 0.0529(17) 0.0354(14) -0.0207(13) -0.0025(11) -0.0065(12) C69 0.0301(14) 0.0400(15) 0.0406(15) -0.0094(12) -0.0097(11) -0.0073(12) C70 0.0381(15) 0.0321(14) 0.0421(14) -0.0170(11) -0.0110(12) 0.0024(12) C71 0.0437(15) 0.0271(12) 0.0349(13) -0.0102(10) -0.0087(11) 0.0120(11) C73 0.0343(15) 0.0404(15) 0.0411(15) -0.0124(13) -0.0054(11) -0.0047(12) C74 0.0263(13) 0.0512(16) 0.0359(14) -0.0219(13) 0.0014(10) -0.0071(11) C75 0.0287(13) 0.0325(13) 0.0467(15) -0.0231(12) -0.0035(11) 0.0022(11) C76 0.0542(17) 0.0312(13) 0.0369(14) -0.0161(11) -0.0069(12) 0.0068(12) C77 0.067(2) 0.0377(15) 0.0393(15) -0.0198(13) -0.0074(13) 0.0116(14) N3A 0.023(5) 0.055(4) 0.028(3) -0.007(3) 0.005(3) -0.018(4) C72A 0.049(7) 0.029(4) 0.050(5) -0.014(3) 0.004(5) -0.013(5) N3B 0.038(7) 0.076(8) 0.048(5) -0.030(5) -0.015(5) 0.028(5) C72B 0.084(8) 0.037(4) 0.034(4) -0.020(3) -0.032(5) 0.017(5) S2A 0.0310(7) 0.0248(6) 0.0164(4) -0.0070(4) -0.0035(5) 0.0001(5) O1S 0.0511(19) 0.0285(14) 0.0270(12) -0.0095(11) -0.0049(11) 0.0057(13) O2S 0.0386(15) 0.0480(16) 0.0252(12) -0.0091(10) -0.0001(10) -0.0156(11) O3S 0.0367(13) 0.0362(18) 0.0256(7) -0.0087(8) -0.0056(7) -0.0013(7) O4S 0.0367(13) 0.0362(18) 0.0256(7) -0.0087(8) -0.0056(7) -0.0013(7) S2B 0.031(2) 0.042(2) 0.0351(15) -0.0119(14) -0.0034(13) -0.0018(13) O5S 0.0367(13) 0.0362(18) 0.0256(7) -0.0087(8) -0.0056(7) -0.0013(7) O6S 0.0367(13) 0.0362(18) 0.0256(7) -0.0087(8) -0.0056(7) -0.0013(7) O7S 0.041(4) 0.028(3) 0.039(3) -0.010(3) 0.000(3) -0.003(3) O8S 0.030(4) 0.050(5) 0.045(4) -0.030(3) -0.002(3) 0.009(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 C71 1.689(3) . ? O1 C1 1.390(2) . ? O1 H01 0.89(3) . ? O2 C2 1.375(2) . ? O2 H02 0.82(3) . ? O3 C3 1.389(3) . ? O3 H03 0.89(4) . ? O4 C9 1.377(2) . ? O4 H04 0.93(5) . ? O5 C10 1.375(3) . ? O5 H05 0.84(3) . ? O6 C11 1.391(2) . ? O6 H06 0.86(3) . ? O7 C17 1.391(2) . ? O7 H07 0.78(3) . ? O8 C18 1.370(2) . ? O8 H08 0.86(3) . ? O9 C19 1.391(2) . ? O9 H09 0.82(2) . ? O10 C25 1.380(2) . ? O10 H010 0.86(3) . ? O11 C26 1.368(2) . ? O11 H011 0.80(3) . ? O12 C27 1.389(2) . ? O12 H012 0.92(3) . ? O13 C33 1.383(2) . ? O13 H013 0.84(2) . ? O14 C34 1.375(2) . ? O14 H014 0.84(2) . ? O15 C35 1.388(2) . ? O15 H015 0.89(3) . ? O16 C41 1.379(2) . ? O16 H016 0.84(3) . ? O17 C42 1.379(2) . ? O17 H017 0.89(3) . ? O18 C43 1.388(2) . ? O18 H018 0.81(2) . ? O19 C49 1.386(3) . ? O19 H019 0.80(3) . ? O20 C50 1.379(2) . ? O20 H020 0.82(3) . ? O21 C51 1.390(2) . ? O21 H021 0.75(3) . ? O22 C57 1.385(2) . ? O22 H022 0.84(2) . ? O23 C58 1.379(2) . ? O23 H023 0.83(3) . ? O24 C59 1.378(2) . ? O24 H024 0.85(2) . ? N1 C69 1.339(3) . ? N1 C65 1.345(3) . ? N1 H1N 0.90(2) . ? N2 C71 1.335(3) . ? N2 C70 1.448(3) . ? N2 H2N 0.84(3) . ? N4 C77 1.331(3) . ? N4 C73 1.337(3) . ? N4 H4N 0.84(3) . ? O1W H2W 0.84(4) . ? O1W H1W 0.93(3) . ? C1 C2 1.389(3) . ? C1 C6 1.393(3) . ? C2 C3 1.384(3) . ? C3 C4 1.398(3) . ? C4 C5 1.393(3) . ? C4 C7 1.534(3) . ? C5 C6 1.390(3) . ? C5 H5 0.999(19) . ? C6 C31 1.531(3) . ? C7 C14 1.524(3) . ? C7 C8 1.529(3) . ? C7 H7 1.01(2) . ? C8 H8A 0.96(2) . ? C8 H8B 1.00(2) . ? C8 H8C 1.00(2) . ? C9 C14 1.389(3) . ? C9 C10 1.390(3) . ? C10 C11 1.395(3) . ? C11 C12 1.384(3) . ? C12 C13 1.391(3) . ? C12 C15 1.522(3) . ? C13 C14 1.394(3) . ? C13 H13 0.97(2) . ? C15 C16 1.517(3) . ? C15 C22 1.531(3) . ? C15 H15 1.01(2) . ? C16 H16B 0.96(2) . ? C16 H16A 1.02(2) . ? C16 H16C 0.98(3) . ? C17 C22 1.386(3) . ? C17 C18 1.387(3) . ? C18 C19 1.386(3) . ? C19 C20 1.393(3) . ? C20 C21 1.399(3) . ? C20 C23 1.529(3) . ? C21 C22 1.395(3) . ? C21 H21 0.965(19) . ? C23 C30 1.524(3) . ? C23 C24 1.525(3) . ? C23 H23 1.001(19) . ? C24 H24B 0.98(2) . ? C24 H24C 0.98(2) . ? C24 H24A 1.00(2) . ? C25 C30 1.387(3) . ? C25 C26 1.390(3) . ? C26 C27 1.385(3) . ? C27 C28 1.399(3) . ? C28 C29 1.394(3) . ? C28 C31 1.525(3) . ? C29 C30 1.392(3) . ? C29 H29 0.96(2) . ? C31 C32 1.525(3) . ? C31 H31 1.04(2) . ? C32 H32A 1.00(2) . ? C32 H32B 0.99(3) . ? C32 H32C 0.99(2) . ? C33 C34 1.389(3) . ? C33 C38 1.399(3) . ? C34 C35 1.382(3) . ? C35 C36 1.389(3) . ? C36 C37 1.398(3) . ? C36 C39 1.520(3) . ? C37 C38 1.389(3) . ? C37 H37 0.980(18) . ? C38 C63 1.531(3) . ? C39 C46 1.517(3) . ? C39 C40 1.523(3) . ? C39 H39 0.969(18) . ? C40 H40C 0.93(3) . ? C40 H40B 1.00(2) . ? C40 H40A 0.99(2) . ? C41 C42 1.385(3) . ? C41 C46 1.389(3) . ? C42 C43 1.388(3) . ? C43 C44 1.393(3) . ? C44 C45 1.391(3) . ? C44 C47 1.529(3) . ? C45 C46 1.394(3) . ? C45 H45 0.961(19) . ? C47 C48 1.527(3) . ? C47 C54 1.529(3) . ? C47 H47 1.00(2) . ? C48 H48C 0.98(2) . ? C48 H48B 1.01(2) . ? C48 H48A 0.99(2) . ? C49 C50 1.386(3) . ? C49 C54 1.391(3) . ? C50 C51 1.388(3) . ? C51 C52 1.395(3) . ? C52 C53 1.397(3) . ? C52 C55 1.532(3) . ? C53 C54 1.389(3) . ? C53 H53 0.96(2) . ? C55 C56 1.520(3) . ? C55 C62 1.531(3) . ? C55 H55 0.992(19) . ? C56 H58A 1.01(2) . ? C56 H58C 1.00(2) . ? C56 H58B 1.01(3) . ? C57 C58 1.383(3) . ? C57 C62 1.387(3) . ? C58 C59 1.392(3) . ? C59 C60 1.402(3) . ? C60 C61 1.394(3) . ? C60 C63 1.534(3) . ? C61 C62 1.399(3) . ? C61 H61 0.97(2) . ? C63 C64 1.528(3) . ? C63 H63 0.99(2) . ? C64 H64A 0.95(2) . ? C64 H64B 1.02(3) . ? C64 H64C 1.00(3) . ? C65 C66 1.376(3) . ? C65 H65 0.95(2) . ? C66 C67 1.384(3) . ? C66 C70 1.513(3) . ? C67 C68 1.379(3) . ? C67 H67 0.95(2) . ? C68 C69 1.367(3) . ? C68 H68 0.88(2) . ? C69 H69 0.96(2) . ? C70 H70B 1.02(2) . ? C70 H70A 0.97(3) . ? C71 N3B 1.320(12) . ? C71 N3A 1.393(13) . ? C73 C74 1.374(3) . ? C73 H73 0.98(2) . ? C74 C75 1.381(3) . ? C74 H74 0.95(2) . ? C75 C76 1.380(3) . ? C75 H75 0.97(2) . ? C76 C77 1.371(3) . ? C76 C72A 1.527(8) . ? C76 C72B 1.552(7) . ? C77 H77 0.92(3) . ? N3A C72A 1.421(8) . ? N3A H3A 0.7648 . ? C72A H72A 0.9530 . ? C72A H72B 0.9530 . ? N3B C72B 1.438(8) . ? N3B H3B 0.9621 . ? C72B H72C 0.9341 . ? C72B H72D 0.9341 . ? S2A O2S 1.449(3) . ? S2A O1S 1.492(3) . ? S2A O3S 1.499(7) . ? S2A O4S 1.508(5) . ? S2B O6S 1.390(16) . ? S2B O7S 1.456(7) . ? S2B O5S 1.476(18) . ? S2B O8S 1.525(7) . ? 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 C1 O1 H01 107.4(16) . . ? C2 O2 H02 108.4(19) . . ? C3 O3 H03 106(3) . . ? C9 O4 H04 117(3) . . ? C10 O5 H05 111.7(19) . . ? C11 O6 H06 107.4(19) . . ? C17 O7 H07 106(2) . . ? C18 O8 H08 109.2(18) . . ? C19 O9 H09 110.6(17) . . ? C25 O10 H010 111.7(18) . . ? C26 O11 H011 117.2(19) . . ? C27 O12 H012 114.5(18) . . ? C33 O13 H013 107.9(17) . . ? C34 O14 H014 109.4(17) . . ? C35 O15 H015 105.0(17) . . ? C41 O16 H016 111.5(17) . . ? C42 O17 H017 109.6(17) . . ? C43 O18 H018 109.7(17) . . ? C49 O19 H019 108(2) . . ? C50 O20 H020 108(2) . . ? C51 O21 H021 110(3) . . ? C57 O22 H022 112.0(17) . . ? C58 O23 H023 110(2) . . ? C59 O24 H024 111.2(16) . . ? C69 N1 C65 122.3(2) . . ? C69 N1 H1N 123.3(15) . . ? C65 N1 H1N 114.3(15) . . ? C71 N2 C70 123.8(2) . . ? C71 N2 H2N 116(2) . . ? C70 N2 H2N 119(2) . . ? C77 N4 C73 123.0(2) . . ? C77 N4 H4N 116.6(18) . . ? C73 N4 H4N 120.3(18) . . ? H2W O1W H1W 110(3) . . ? C2 C1 O1 114.71(18) . . ? C2 C1 C6 121.35(19) . . ? O1 C1 C6 123.92(19) . . ? O2 C2 C3 118.34(19) . . ? O2 C2 C1 121.2(2) . . ? C3 C2 C1 120.32(19) . . ? C2 C3 O3 117.25(18) . . ? C2 C3 C4 120.30(19) . . ? O3 C3 C4 122.36(19) . . ? C5 C4 C3 117.64(19) . . ? C5 C4 C7 120.32(18) . . ? C3 C4 C7 122.00(19) . . ? C6 C5 C4 123.60(19) . . ? C6 C5 H5 117.8(12) . . ? C4 C5 H5 118.6(12) . . ? C5 C6 C1 116.78(19) . . ? C5 C6 C31 121.42(18) . . ? C1 C6 C31 121.79(18) . . ? C14 C7 C8 113.67(18) . . ? C14 C7 C4 110.16(17) . . ? C8 C7 C4 110.7(2) . . ? C14 C7 H7 107.0(12) . . ? C8 C7 H7 107.5(12) . . ? C4 C7 H7 107.5(12) . . ? C7 C8 H8A 109.3(13) . . ? C7 C8 H8B 112.6(13) . . ? H8A C8 H8B 105.7(18) . . ? C7 C8 H8C 111.5(14) . . ? H8A C8 H8C 107.1(19) . . ? H8B C8 H8C 110.2(18) . . ? O4 C9 C14 118.71(18) . . ? O4 C9 C10 119.83(19) . . ? C14 C9 C10 121.46(18) . . ? O5 C10 C9 125.36(18) . . ? O5 C10 C11 115.70(19) . . ? C9 C10 C11 118.90(19) . . ? C12 C11 O6 119.28(18) . . ? C12 C11 C10 121.51(19) . . ? O6 C11 C10 119.19(19) . . ? C11 C12 C13 117.79(18) . . ? C11 C12 C15 119.84(18) . . ? C13 C12 C15 122.31(19) . . ? C12 C13 C14 122.6(2) . . ? C12 C13 H13 117.1(12) . . ? C14 C13 H13 120.3(12) . . ? C9 C14 C13 117.69(19) . . ? C9 C14 C7 119.36(17) . . ? C13 C14 C7 122.91(19) . . ? C16 C15 C12 114.02(18) . . ? C16 C15 C22 112.33(18) . . ? C12 C15 C22 109.04(16) . . ? C16 C15 H15 107.0(11) . . ? C12 C15 H15 106.9(11) . . ? C22 C15 H15 107.2(11) . . ? C15 C16 H16B 109.8(14) . . ? C15 C16 H16A 111.5(13) . . ? H16B C16 H16A 114.3(19) . . ? C15 C16 H16C 109.8(15) . . ? H16B C16 H16C 105.1(19) . . ? H16A C16 H16C 106.1(19) . . ? C22 C17 C18 121.53(19) . . ? C22 C17 O7 122.10(18) . . ? C18 C17 O7 116.36(18) . . ? O8 C18 C19 117.52(18) . . ? O8 C18 C17 122.99(19) . . ? C19 C18 C17 119.48(18) . . ? C18 C19 O9 119.20(18) . . ? C18 C19 C20 121.34(19) . . ? O9 C19 C20 119.46(19) . . ? C19 C20 C21 117.06(19) . . ? C19 C20 C23 120.76(18) . . ? C21 C20 C23 122.17(18) . . ? C22 C21 C20 123.00(19) . . ? C22 C21 H21 118.2(12) . . ? C20 C21 H21 118.8(12) . . ? C17 C22 C21 117.36(19) . . ? C17 C22 C15 120.62(19) . . ? C21 C22 C15 121.95(18) . . ? C30 C23 C24 113.92(18) . . ? C30 C23 C20 110.92(16) . . ? C24 C23 C20 111.44(18) . . ? C30 C23 H23 106.7(10) . . ? C24 C23 H23 104.5(11) . . ? C20 C23 H23 109.0(11) . . ? C23 C24 H24B 109.0(13) . . ? C23 C24 H24C 112.1(14) . . ? H24B C24 H24C 108.4(19) . . ? C23 C24 H24A 109.9(13) . . ? H24B C24 H24A 108.2(18) . . ? H24C C24 H24A 109.2(18) . . ? O10 C25 C30 124.01(18) . . ? O10 C25 C26 114.68(18) . . ? C30 C25 C26 121.28(18) . . ? O11 C26 C27 124.24(18) . . ? O11 C26 C25 115.66(18) . . ? C27 C26 C25 120.09(19) . . ? C26 C27 O12 120.83(18) . . ? C26 C27 C28 120.32(18) . . ? O12 C27 C28 118.71(18) . . ? C29 C28 C27 117.75(18) . . ? C29 C28 C31 122.20(18) . . ? C27 C28 C31 119.99(17) . . ? C30 C29 C28 122.96(19) . . ? C30 C29 H29 117.7(12) . . ? C28 C29 H29 119.3(12) . . ? C25 C30 C29 117.42(18) . . ? C25 C30 C23 118.89(17) . . ? C29 C30 C23 123.64(18) . . ? C32 C31 C28 113.47(17) . . ? C32 C31 C6 110.52(18) . . ? C28 C31 C6 110.24(17) . . ? C32 C31 H31 108.0(11) . . ? C28 C31 H31 106.5(11) . . ? C6 C31 H31 107.9(11) . . ? C31 C32 H32A 113.7(14) . . ? C31 C32 H32B 114.6(14) . . ? H32A C32 H32B 104.1(19) . . ? C31 C32 H32C 111.6(12) . . ? H32A C32 H32C 106.9(18) . . ? H32B C32 H32C 105.2(19) . . ? O13 C33 C34 120.76(17) . . ? O13 C33 C38 118.78(18) . . ? C34 C33 C38 120.46(19) . . ? O14 C34 C35 121.26(18) . . ? O14 C34 C33 118.54(18) . . ? C35 C34 C33 120.14(18) . . ? C34 C35 O15 115.75(17) . . ? C34 C35 C36 121.41(18) . . ? O15 C35 C36 122.83(19) . . ? C35 C36 C37 117.20(19) . . ? C35 C36 C39 120.68(18) . . ? C37 C36 C39 122.03(18) . . ? C38 C37 C36 123.07(18) . . ? C38 C37 H37 120.5(11) . . ? C36 C37 H37 116.2(11) . . ? C37 C38 C33 117.71(18) . . ? C37 C38 C63 121.21(17) . . ? C33 C38 C63 121.08(18) . . ? C46 C39 C36 108.59(16) . . ? C46 C39 C40 114.06(18) . . ? C36 C39 C40 112.67(19) . . ? C46 C39 H39 108.2(11) . . ? C36 C39 H39 108.8(11) . . ? C40 C39 H39 104.2(11) . . ? C39 C40 H40C 108.2(15) . . ? C39 C40 H40B 110.2(12) . . ? H40C C40 H40B 106.9(19) . . ? C39 C40 H40A 109.5(14) . . ? H40C C40 H40A 107(2) . . ? H40B C40 H40A 114.8(18) . . ? O16 C41 C42 119.73(18) . . ? O16 C41 C46 119.17(18) . . ? C42 C41 C46 121.09(18) . . ? O17 C42 C41 116.67(18) . . ? O17 C42 C43 123.32(19) . . ? C41 C42 C43 120.00(19) . . ? C42 C43 O18 114.02(18) . . ? C42 C43 C44 120.84(18) . . ? O18 C43 C44 125.14(18) . . ? C45 C44 C43 117.53(18) . . ? C45 C44 C47 121.78(18) . . ? C43 C44 C47 120.68(18) . . ? C44 C45 C46 123.06(19) . . ? C44 C45 H45 116.7(11) . . ? C46 C45 H45 120.2(11) . . ? C41 C46 C45 117.47(18) . . ? C41 C46 C39 119.48(17) . . ? C45 C46 C39 122.94(18) . . ? C48 C47 C54 111.44(18) . . ? C48 C47 C44 114.04(17) . . ? C54 C47 C44 109.57(16) . . ? C48 C47 H47 105.2(11) . . ? C54 C47 H47 110.2(11) . . ? C44 C47 H47 106.1(10) . . ? C47 C48 H48C 111.0(12) . . ? C47 C48 H48B 113.3(12) . . ? H48C C48 H48B 110.0(17) . . ? C47 C48 H48A 111.0(13) . . ? H48C C48 H48A 105.1(17) . . ? H48B C48 H48A 106.1(17) . . ? C50 C49 O19 120.40(19) . . ? C50 C49 C54 121.6(2) . . ? O19 C49 C54 117.97(19) . . ? O20 C50 C49 117.5(2) . . ? O20 C50 C51 122.74(19) . . ? C49 C50 C51 119.72(19) . . ? C50 C51 O21 118.49(19) . . ? C50 C51 C52 120.71(19) . . ? O21 C51 C52 120.6(2) . . ? C51 C52 C53 117.7(2) . . ? C51 C52 C55 121.31(19) . . ? C53 C52 C55 120.91(19) . . ? C54 C53 C52 123.0(2) . . ? C54 C53 H53 117.8(12) . . ? C52 C53 H53 119.1(12) . . ? C53 C54 C49 117.23(19) . . ? C53 C54 C47 122.67(18) . . ? C49 C54 C47 120.07(19) . . ? C56 C55 C62 114.68(19) . . ? C56 C55 C52 112.12(19) . . ? C62 C55 C52 110.01(16) . . ? C56 C55 H55 105.5(11) . . ? C62 C55 H55 105.5(11) . . ? C52 C55 H55 108.6(11) . . ? C55 C56 H58A 112.6(13) . . ? C55 C56 H58C 108.1(13) . . ? H58A C56 H58C 104.8(18) . . ? C55 C56 H58B 111.1(15) . . ? H58A C56 H58B 112(2) . . ? H58C C56 H58B 107.9(19) . . ? C58 C57 O22 115.02(18) . . ? C58 C57 C62 121.47(19) . . ? O22 C57 C62 123.50(18) . . ? O23 C58 C57 117.06(18) . . ? O23 C58 C59 123.15(18) . . ? C57 C58 C59 119.70(18) . . ? O24 C59 C58 114.84(18) . . ? O24 C59 C60 124.17(18) . . ? C58 C59 C60 120.97(18) . . ? C61 C60 C59 117.29(18) . . ? C61 C60 C63 123.78(18) . . ? C59 C60 C63 118.87(17) . . ? C60 C61 C62 122.9(2) . . ? C60 C61 H61 119.5(11) . . ? C62 C61 H61 117.6(11) . . ? C57 C62 C61 117.60(18) . . ? C57 C62 C55 118.30(18) . . ? C61 C62 C55 123.97(19) . . ? C64 C63 C38 110.20(18) . . ? C64 C63 C60 114.52(18) . . ? C38 C63 C60 110.96(17) . . ? C64 C63 H63 105.8(11) . . ? C38 C63 H63 108.3(11) . . ? C60 C63 H63 106.8(11) . . ? C63 C64 H64A 107.9(14) . . ? C63 C64 H64B 112.0(14) . . ? H64A C64 H64B 107(2) . . ? C63 C64 H64C 111.1(14) . . ? H64A C64 H64C 113(2) . . ? H64B C64 H64C 106.1(19) . . ? N1 C65 C66 120.5(2) . . ? N1 C65 H65 116.4(13) . . ? C66 C65 H65 123.0(13) . . ? C65 C66 C67 117.5(2) . . ? C65 C66 C70 122.3(2) . . ? C67 C66 C70 120.2(2) . . ? C68 C67 C66 121.0(2) . . ? C68 C67 H67 121.3(13) . . ? C66 C67 H67 117.7(13) . . ? C69 C68 C67 119.3(2) . . ? C69 C68 H68 119.3(16) . . ? C67 C68 H68 121.3(16) . . ? N1 C69 C68 119.4(2) . . ? N1 C69 H69 119.4(13) . . ? C68 C69 H69 121.2(13) . . ? N2 C70 C66 115.3(2) . . ? N2 C70 H70B 108.6(11) . . ? C66 C70 H70B 108.0(12) . . ? N2 C70 H70A 106.4(14) . . ? C66 C70 H70A 108.7(14) . . ? H70B C70 H70A 109.7(19) . . ? N3B C71 N2 124.2(7) . . ? N3B C71 N3A 19.2(8) . . ? N2 C71 N3A 107.5(5) . . ? N3B C71 S1 112.6(8) . . ? N2 C71 S1 123.01(19) . . ? N3A C71 S1 129.1(5) . . ? N4 C73 C74 118.7(2) . . ? N4 C73 H73 117.5(13) . . ? C74 C73 H73 123.8(13) . . ? C73 C74 C75 119.3(2) . . ? C73 C74 H74 121.9(14) . . ? C75 C74 H74 118.8(14) . . ? C76 C75 C74 120.6(2) . . ? C76 C75 H75 118.8(12) . . ? C74 C75 H75 120.5(12) . . ? C77 C76 C75 117.9(2) . . ? C77 C76 C72A 121.1(5) . . ? C75 C76 C72A 120.0(6) . . ? C77 C76 C72B 118.9(5) . . ? C75 C76 C72B 121.8(5) . . ? C72A C76 C72B 21.8(5) . . ? N4 C77 C76 120.5(2) . . ? N4 C77 H77 118.9(16) . . ? C76 C77 H77 120.6(16) . . ? C71 N3A C72A 119.9(8) . . ? C71 N3A H3A 120.0 . . ? N3A C72A C76 118.4(10) . . ? C76 C72A H72A 107.7 . . ? C76 C72A H72B 107.7 . . ? C71 N3B C72B 132.4(10) . . ? C71 N3B H3B 113.8 . . ? C72B N3B H3B 113.8 . . ? N3B C72B C76 109.3(8) . . ? N3B C72B H72C 109.8 . . ? C76 C72B H72C 109.8 . . ? N3B C72B H72D 109.8 . . ? C76 C72B H72D 109.8 . . ? H72C C72B H72D 108.3 . . ? O2S S2A O1S 108.79(19) . . ? O2S S2A O3S 111.9(2) . . ? O1S S2A O3S 107.6(2) . . ? O2S S2A O4S 111.8(4) . . ? O1S S2A O4S 106.9(3) . . ? O3S S2A O4S 109.6(3) . . ? O6S S2B O7S 111.9(10) . . ? O6S S2B O5S 105.1(9) . . ? O7S S2B O5S 115.2(5) . . ? O6S S2B O8S 109.8(8) . . ? O7S S2B O8S 108.2(4) . . ? O5S S2B O8S 106.5(7) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 29.64 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.288 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.053 # Attachment 'POB58.cif' data_POB58 _database_code_depnum_ccdc_archive 'CCDC 292517' _audit_creation_method SHELXL-97 _chemical_name_systematic rctt-methylpyrogall[4]arene _chemical_name_common rctt-methylpyrogall(4)arene _chemical_melting_point ? _chemical_formula_moiety 'C32 H32 O12' _chemical_formula_sum 'C16 H16 O6' _chemical_formula_weight 304.29 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' _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 8.8592(17) _cell_length_b 9.3271(18) _cell_length_c 9.4416(18) _cell_angle_alpha 106.968(4) _cell_angle_beta 104.650(4) _cell_angle_gamma 104.616(4) _cell_volume 675.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 320 _exptl_absorpt_coefficient_mu 0.115 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.9773 _exptl_absorpt_correction_T_max 0.9908 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7490 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 29.59 _reflns_number_total 3722 _reflns_number_gt 2656 _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 full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0782P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3722 _refine_ls_number_parameters 273 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0706 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.1286 _refine_ls_wR_factor_gt 0.1174 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O -0.36771(14) 0.68238(15) 0.32328(15) 0.0219(2) Uani 1 1 d D . . O2 O -0.15371(15) 0.52606(14) 0.40331(14) 0.0265(3) Uani 1 1 d . . . O3 O 0.13857(14) 0.58104(15) 0.34933(14) 0.0264(3) Uani 1 1 d . . . O4 O 0.42130(15) 1.09558(15) 0.44990(13) 0.0227(3) Uani 1 1 d D . . O5 O 0.52426(15) 1.37376(14) 0.39440(14) 0.0258(3) Uani 1 1 d . . . O6 O 0.44893(15) 1.36993(15) 0.09860(15) 0.0264(3) Uani 1 1 d D . . C7 C -0.11548(18) 0.63341(18) 0.33349(17) 0.0189(3) Uani 1 1 d . . . C8 C -0.17871(17) 0.82048(18) 0.21724(16) 0.0181(3) Uani 1 1 d . . . C9 C 0.29843(17) 0.93964(18) 0.16744(17) 0.0177(3) Uani 1 1 d . . . C10 C 0.31541(17) 1.08236(18) -0.01311(17) 0.0178(3) Uani 1 1 d . . . C11 C -0.22050(17) 0.71405(18) 0.29038(16) 0.0178(3) Uani 1 1 d . . . C12 C 0.26826(17) 0.94201(18) 0.01538(17) 0.0186(3) Uani 1 1 d . . . C13 C 0.23952(18) 0.78518(18) 0.19405(17) 0.0179(3) Uani 1 1 d . . . C14 C 0.43238(18) 1.22764(18) 0.27004(17) 0.0195(3) Uani 1 1 d . . . C15 C 0.38160(17) 1.08548(18) 0.29440(16) 0.0185(3) Uani 1 1 d . . . C16 C 0.03437(18) 0.66020(18) 0.30563(16) 0.0191(3) Uani 1 1 d . . . C17 C 0.07982(17) 0.76582(17) 0.23241(16) 0.0176(3) Uani 1 1 d . . . C18 C -0.28817(18) 0.91689(18) 0.17854(17) 0.0186(3) Uani 1 1 d . . . C19 C -0.02891(18) 0.84356(18) 0.18927(17) 0.0190(3) Uani 1 1 d . . . C20 C 0.39655(18) 1.22700(18) 0.11767(17) 0.0192(3) Uani 1 1 d . . . C21 C 0.2158(2) 0.63652(19) 0.0554(2) 0.0242(3) Uani 1 1 d . . . C22 C -0.2148(2) 1.0837(2) 0.30895(19) 0.0251(3) Uani 1 1 d . . . H13 H 0.319(2) 0.789(2) 0.287(2) 0.017(4) Uiso 1 1 d . . . H12 H 0.208(2) 0.839(2) -0.077(2) 0.022(4) Uiso 1 1 d . . . H21B H 0.307(3) 0.642(2) 0.029(2) 0.029(5) Uiso 1 1 d . . . H22A H -0.104(3) 1.136(2) 0.310(2) 0.030(5) Uiso 1 1 d . . . H19 H 0.006(2) 0.917(2) 0.138(2) 0.025(5) Uiso 1 1 d . . . H21C H 0.193(2) 0.545(2) 0.082(2) 0.029(5) Uiso 1 1 d . . . H22C H -0.209(2) 1.076(2) 0.410(2) 0.033(5) Uiso 1 1 d . . . H21A H 0.120(2) 0.612(2) -0.038(2) 0.030(5) Uiso 1 1 d . . . H18 H -0.397(2) 0.860(2) 0.176(2) 0.024(5) Uiso 1 1 d . . . H22B H -0.286(2) 1.147(2) 0.287(2) 0.032(5) Uiso 1 1 d . . . H03 H 0.099(3) 0.525(3) 0.398(3) 0.066(8) Uiso 1 1 d . . . H02 H -0.257(3) 0.500(3) 0.389(3) 0.050(7) Uiso 1 1 d . . . H05 H 0.557(3) 1.360(3) 0.466(3) 0.053(8) Uiso 1 1 d . . . H4A H 0.401(5) 1.155(4) 0.503(4) 0.029(5) Uiso 0.56(3) 1 d PD . . H4B H 0.456(5) 1.037(5) 0.469(5) 0.029(5) Uiso 0.44(3) 1 d PD . . H1A H -0.431(4) 0.600(3) 0.273(4) 0.029(5) Uiso 0.55(3) 1 d PD . . H1B H -0.375(6) 0.739(5) 0.393(4) 0.029(5) Uiso 0.45(3) 1 d PD . . H6A H 0.489(5) 1.436(4) 0.182(3) 0.029(5) Uiso 0.51(3) 1 d PD . . H6B H 0.393(4) 1.354(5) 0.015(3) 0.029(5) Uiso 0.49(3) 1 d PD . . 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 O1 0.0216(5) 0.0202(6) 0.0247(6) 0.0089(5) 0.0111(5) 0.0056(5) O2 0.0249(6) 0.0305(7) 0.0352(6) 0.0244(6) 0.0138(5) 0.0104(5) O3 0.0267(6) 0.0308(7) 0.0350(7) 0.0235(6) 0.0143(5) 0.0151(5) O4 0.0312(6) 0.0238(6) 0.0160(5) 0.0084(5) 0.0086(4) 0.0129(5) O5 0.0336(6) 0.0164(6) 0.0205(6) 0.0045(5) 0.0080(5) 0.0020(5) O6 0.0340(6) 0.0181(6) 0.0242(6) 0.0100(5) 0.0075(5) 0.0050(5) C7 0.0217(7) 0.0169(7) 0.0174(7) 0.0081(6) 0.0066(5) 0.0043(5) C8 0.0195(6) 0.0163(7) 0.0178(7) 0.0068(6) 0.0053(5) 0.0057(5) C9 0.0166(6) 0.0184(7) 0.0215(7) 0.0099(6) 0.0083(5) 0.0072(5) C10 0.0163(6) 0.0196(7) 0.0194(7) 0.0088(6) 0.0068(5) 0.0070(5) C11 0.0193(7) 0.0160(7) 0.0168(6) 0.0056(6) 0.0072(5) 0.0040(5) C12 0.0183(6) 0.0177(7) 0.0193(7) 0.0072(6) 0.0060(5) 0.0061(6) C13 0.0185(6) 0.0160(7) 0.0202(7) 0.0092(6) 0.0062(5) 0.0055(5) C14 0.0210(7) 0.0165(7) 0.0192(7) 0.0054(6) 0.0065(5) 0.0057(6) C15 0.0182(6) 0.0208(7) 0.0171(7) 0.0082(6) 0.0061(5) 0.0071(6) C16 0.0211(7) 0.0180(7) 0.0179(7) 0.0084(6) 0.0047(5) 0.0068(6) C17 0.0179(7) 0.0169(7) 0.0173(7) 0.0070(6) 0.0061(5) 0.0046(5) C18 0.0192(7) 0.0188(7) 0.0196(7) 0.0087(6) 0.0077(5) 0.0070(6) C19 0.0206(7) 0.0182(7) 0.0205(7) 0.0105(6) 0.0080(5) 0.0064(6) C20 0.0199(7) 0.0181(7) 0.0227(7) 0.0102(6) 0.0091(5) 0.0072(6) C21 0.0276(8) 0.0180(8) 0.0302(8) 0.0096(7) 0.0150(7) 0.0079(6) C22 0.0331(9) 0.0228(8) 0.0211(8) 0.0087(7) 0.0098(6) 0.0122(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C11 1.3959(18) . ? O1 H1A 0.75(2) . ? O1 H1B 0.74(2) . ? O2 C7 1.3707(17) . ? O2 H02 0.85(3) . ? O3 C16 1.3772(18) . ? O3 H03 0.86(3) . ? O4 C15 1.3891(17) . ? O4 H4A 0.73(2) . ? O4 H4B 0.73(2) . ? O5 C14 1.3861(18) . ? O5 H05 0.73(3) . ? O6 C20 1.3767(18) . ? O6 H6A 0.76(2) . ? O6 H6B 0.76(2) . ? C7 C11 1.392(2) . ? C7 C16 1.393(2) . ? C8 C11 1.3940(19) . ? C8 C19 1.394(2) . ? C8 C18 1.528(2) . ? C9 C15 1.388(2) . ? C9 C12 1.400(2) . ? C9 C13 1.5196(19) . ? C10 C12 1.3953(19) . ? C10 C20 1.397(2) . ? C10 C18 1.5214(19) 2_575 ? C12 H12 0.989(18) . ? C13 C17 1.528(2) . ? C13 C21 1.528(2) . ? C13 H13 0.964(17) . ? C14 C20 1.391(2) . ? C14 C15 1.394(2) . ? C16 C17 1.3959(19) . ? C17 C19 1.395(2) . ? C18 C10 1.5214(19) 2_575 ? C18 C22 1.525(2) . ? C18 H18 0.970(19) . ? C19 H19 0.986(19) . ? C21 H21B 0.90(2) . ? C21 H21C 0.95(2) . ? C21 H21A 0.98(2) . ? C22 H22A 0.98(2) . ? C22 H22C 0.96(2) . ? C22 H22B 0.99(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 C11 O1 H1A 114(3) . . ? C11 O1 H1B 121(4) . . ? H1A O1 H1B 124(5) . . ? C7 O2 H02 108.1(16) . . ? C16 O3 H03 109.6(19) . . ? C15 O4 H4A 117(3) . . ? C15 O4 H4B 117(4) . . ? H4A O4 H4B 127(5) . . ? C14 O5 H05 109(2) . . ? C20 O6 H6A 107(3) . . ? C20 O6 H6B 105(3) . . ? H6A O6 H6B 140(4) . . ? O2 C7 C11 122.34(13) . . ? O2 C7 C16 117.61(13) . . ? C11 C7 C16 120.05(13) . . ? C11 C8 C19 117.96(13) . . ? C11 C8 C18 120.99(13) . . ? C19 C8 C18 120.93(12) . . ? C15 C9 C12 117.24(13) . . ? C15 C9 C13 120.82(12) . . ? C12 C9 C13 121.92(13) . . ? C12 C10 C20 117.75(13) . . ? C12 C10 C18 122.91(13) . 2_575 ? C20 C10 C18 119.30(12) . 2_575 ? C7 C11 C8 120.72(13) . . ? C7 C11 O1 116.88(12) . . ? C8 C11 O1 122.40(13) . . ? C10 C12 C9 123.32(14) . . ? C10 C12 H12 118.3(10) . . ? C9 C12 H12 118.4(10) . . ? C9 C13 C17 111.60(12) . . ? C9 C13 C21 113.10(12) . . ? C17 C13 C21 110.11(12) . . ? C9 C13 H13 109.9(10) . . ? C17 C13 H13 103.8(10) . . ? C21 C13 H13 107.8(10) . . ? O5 C14 C20 117.19(13) . . ? O5 C14 C15 122.11(13) . . ? C20 C14 C15 120.67(13) . . ? C9 C15 O4 121.70(13) . . ? C9 C15 C14 120.87(13) . . ? O4 C15 C14 117.41(13) . . ? O3 C16 C7 119.94(13) . . ? O3 C16 C17 119.39(13) . . ? C7 C16 C17 120.67(13) . . ? C19 C17 C16 117.87(13) . . ? C19 C17 C13 122.46(12) . . ? C16 C17 C13 119.58(13) . . ? C10 C18 C22 113.82(12) 2_575 . ? C10 C18 C8 112.05(12) 2_575 . ? C22 C18 C8 108.94(12) . . ? C10 C18 H18 105.4(10) 2_575 . ? C22 C18 H18 109.9(11) . . ? C8 C18 H18 106.3(11) . . ? C8 C19 C17 122.72(13) . . ? C8 C19 H19 121.1(11) . . ? C17 C19 H19 116.2(11) . . ? O6 C20 C14 118.90(13) . . ? O6 C20 C10 120.93(13) . . ? C14 C20 C10 120.11(13) . . ? C13 C21 H21B 113.6(13) . . ? C13 C21 H21C 110.2(12) . . ? H21B C21 H21C 105.1(16) . . ? C13 C21 H21A 112.3(12) . . ? H21B C21 H21A 109.7(16) . . ? H21C C21 H21A 105.4(16) . . ? C18 C22 H22A 108.0(12) . . ? C18 C22 H22C 110.1(12) . . ? H22A C22 H22C 110.8(16) . . ? C18 C22 H22B 110.0(11) . . ? H22A C22 H22B 109.3(16) . . ? H22C C22 H22B 108.7(16) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 29.59 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.401 _refine_diff_density_min -0.219 _refine_diff_density_rms 0.059