Supplementary Material (ESI) for Perkin Transactions This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 188 _publ_requested_journal 'Perkin Transactions 2' loop_ _publ_author_name 'Caira, Mino R.' 'Nassimbeni, L. R.' 'Toda, F.' 'Vujovic, Dejana' _publ_contact_author_name 'Prof L R Nassimbeni' _publ_contact_author_address ; Department of Chemistry University of Cape Town Rondebosch 7701 SOUTH AFRICA ; _publ_contact_author_email 'XRAYLUIG@PSIPSY.UCT.AC.ZA' _publ_section_title ; Inclusion by a Diol Host Compound: Structure and Dynamics of Volatile Guest Exchange ; data_c:\dejana\struct~1\t7fur(~2\t7fur _database_code_CSD 166351 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H52 O5' _chemical_formula_weight 901.06 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 ? _symmetry_space_group_name_H-M ? 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' _cell_length_a 21.959(2) _cell_length_b 13.7230(10) _cell_length_c 17.1490(10) _cell_angle_alpha 90.00 _cell_angle_beta 108.216(4) _cell_angle_gamma 90.00 _cell_volume 4908.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.219 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10421 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0580 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.77 _reflns_number_total 6502 _reflns_number_gt 4265 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1889P)^2^+24.5765P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -7(4) _refine_ls_number_reflns 6502 _refine_ls_number_parameters 574 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1567 _refine_ls_R_factor_gt 0.1059 _refine_ls_wR_factor_ref 0.3481 _refine_ls_wR_factor_gt 0.2804 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 7.448 _refine_ls_shift/su_mean 0.619 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 O1A O 0.0827(3) 0.6821(4) 0.1352(4) 0.0353(15) Uani 1 1 d D . . C1A C 0.1056(4) 0.7400(6) 0.2074(5) 0.0324(19) Uani 1 1 d . . . H1A H 0.120(4) 0.674(10) 0.116(8) 0.12(5) Uiso 1 1 d D . . C2A C 0.1248(4) 0.6790(7) 0.2804(6) 0.040(2) Uani 1 1 d . . . C3A C 0.1410(5) 0.6259(8) 0.3384(6) 0.046(3) Uani 1 1 d . . . C4A C 0.1609(6) 0.5709(11) 0.4105(7) 0.067(4) Uani 1 1 d . . . C5A C 0.1805(5) 0.5206(10) 0.4703(6) 0.057(3) Uani 1 1 d . . . O6A O 0.1527(3) 0.3930(6) 0.5462(3) 0.053(2) Uani 1 1 d D . . H6A H 0.1403 0.3608 0.5039 0.064 Uiso 1 1 calc RD . . C6A C 0.2017(5) 0.4555(10) 0.5418(6) 0.054(3) Uani 1 1 d . . . C1AA C 0.1603(4) 0.8042(6) 0.2025(5) 0.037(2) Uani 1 1 d . . . C2AA C 0.2204(7) 0.8036(10) 0.2641(6) 0.069(4) Uani 1 1 d . . . H2AA H 0.2292 0.7618 0.3089 0.083 Uiso 1 1 calc R . . C3AA C 0.2643(6) 0.8663(11) 0.2546(8) 0.080(4) Uani 1 1 d . . . H3AA H 0.3024 0.8719 0.2976 0.095 Uiso 1 1 calc R . . C4AA C 0.2575(7) 0.9230(9) 0.1863(9) 0.076(4) Uani 1 1 d . . . H4AA H 0.2910 0.9624 0.1828 0.092 Uiso 1 1 calc R . . C5AA C 0.2027(6) 0.9210(8) 0.1258(8) 0.058(3) Uani 1 1 d . . . H5AA H 0.1975 0.9589 0.0792 0.069 Uiso 1 1 calc R . . C6AA C 0.1526(6) 0.8619(8) 0.1318(6) 0.051(3) Uani 1 1 d . . . H6AA H 0.1141 0.8605 0.0891 0.061 Uiso 1 1 calc R . . C1AB C 0.0523(4) 0.8055(7) 0.2150(5) 0.038(2) Uiso 1 1 d G . . C2AB C -0.0035(5) 0.8205(9) 0.1501(7) 0.066(3) Uiso 1 1 d G . . H2AB H -0.0121 0.7882 0.1002 0.079 Uiso 1 1 calc R . . C3AB C -0.0488(8) 0.8927(12) 0.1669(10) 0.094(5) Uiso 1 1 d G . . H3AB H -0.0872 0.9086 0.1272 0.113 Uiso 1 1 calc R . . C4AB C -0.0313(6) 0.9343(8) 0.2430(7) 0.068(3) Uiso 1 1 d G . . H4AB H -0.0593 0.9811 0.2512 0.081 Uiso 1 1 calc R . . C5AB C 0.0193(6) 0.9175(9) 0.3057(8) 0.069(3) Uiso 1 1 d G . . H5AB H 0.0250 0.9473 0.3562 0.082 Uiso 1 1 calc R . . C6AB C 0.0632(7) 0.8543(10) 0.2937(8) 0.077(3) Uiso 1 1 d G . . H6AB H 0.1006 0.8419 0.3364 0.092 Uiso 1 1 calc R . . C1AC C 0.2186(5) 0.5241(7) 0.6208(6) 0.043(2) Uani 1 1 d . . . C2AC C 0.2766(6) 0.5645(14) 0.6553(8) 0.097(6) Uani 1 1 d . . . H2AC H 0.3090 0.5516 0.6326 0.116 Uiso 1 1 calc R . . C3AC C 0.2893(7) 0.6225(12) 0.7212(10) 0.084(5) Uani 1 1 d . . . H3AC H 0.3296 0.6511 0.7416 0.100 Uiso 1 1 calc R . . C4AC C 0.2458(6) 0.6399(12) 0.7577(9) 0.077(4) Uani 1 1 d . . . H4AC H 0.2558 0.6807 0.8032 0.092 Uiso 1 1 calc R . . C5AC C 0.1829(7) 0.5969(9) 0.7284(11) 0.080(4) Uani 1 1 d . . . H5AC H 0.1521 0.6050 0.7546 0.097 Uiso 1 1 calc R . . C6AC C 0.1726(6) 0.5423(8) 0.6576(10) 0.072(4) Uani 1 1 d . . . H6AC H 0.1319 0.5164 0.6335 0.087 Uiso 1 1 calc R . . C1AD C 0.2613(5) 0.3984(9) 0.5399(5) 0.049(3) Uani 1 1 d . . . C2AD C 0.2990(7) 0.4268(8) 0.4953(9) 0.070(4) Uani 1 1 d . . . H2AD H 0.2901 0.4852 0.4663 0.084 Uiso 1 1 calc R . . C3AD C 0.3494(8) 0.3725(10) 0.4917(10) 0.097(5) Uani 1 1 d . . . H3AD H 0.3730 0.3947 0.4587 0.116 Uiso 1 1 calc R . . C4AD C 0.3687(6) 0.2833(10) 0.5351(7) 0.062(3) Uani 1 1 d . . . H4AD H 0.4048 0.2484 0.5343 0.074 Uiso 1 1 calc R . . C5AD C 0.3265(7) 0.2526(17) 0.5808(10) 0.107(8) Uani 1 1 d . . . H5AD H 0.3355 0.1955 0.6114 0.128 Uiso 1 1 calc R . . C6AD C 0.2744(5) 0.3055(10) 0.5795(8) 0.079(4) Uani 1 1 d . . . H6AD H 0.2461 0.2808 0.6051 0.095 Uiso 1 1 calc R . . O1B O -0.0074(3) 0.6079(6) 0.0048(4) 0.060(2) Uani 1 1 d D . . H1B H 0.0022 0.6419 0.0461 0.072 Uiso 1 1 calc RD . . C1B C -0.0602(5) 0.5410(8) 0.0057(5) 0.053(3) Uani 1 1 d . . . C2B C -0.0350(6) 0.4807(11) 0.0803(6) 0.066(4) Uani 1 1 d . . . C3B C -0.0165(5) 0.4322(9) 0.1414(6) 0.048(3) Uani 1 1 d . . . C4B C 0.0044(5) 0.3734(10) 0.2077(6) 0.049(3) Uani 1 1 d . . . C5B C 0.0210(5) 0.3250(8) 0.2710(5) 0.043(3) Uani 1 1 d . . . O6B O 0.0630(3) 0.3171(4) 0.4157(3) 0.0310(14) Uani 1 1 d D . . H6B H 0.0340 0.3530 0.4188 0.037 Uiso 1 1 calc RD . . C6B C 0.0408(4) 0.2588(6) 0.3429(5) 0.0315(19) Uani 1 1 d . . . C1BA C -0.0732(5) 0.4837(8) -0.0695(5) 0.049(3) Uani 1 1 d . . . C2BA C -0.0264(6) 0.4599(9) -0.1046(8) 0.067(3) Uani 1 1 d . . . H2BA H 0.0145 0.4865 -0.0842 0.081 Uiso 1 1 calc R . . C3BA C -0.0407(7) 0.3974(11) -0.1689(11) 0.090(5) Uani 1 1 d . . . H3BA H -0.0071 0.3811 -0.1887 0.108 Uiso 1 1 calc R . . C4BA C -0.0970(6) 0.3567(7) -0.2070(7) 0.061(3) Uani 1 1 d . . . H4BA H -0.1030 0.3153 -0.2518 0.073 Uiso 1 1 calc R . . C5BA C -0.1459(6) 0.3800(13) -0.1758(7) 0.084(5) Uani 1 1 d . . . H5BA H -0.1872 0.3571 -0.2018 0.100 Uiso 1 1 calc R . . C6BA C -0.1336(6) 0.4394(14) -0.1031(8) 0.086(5) Uani 1 1 d . . . H6BA H -0.1654 0.4485 -0.0786 0.103 Uiso 1 1 calc R . . C1BB C -0.1169(5) 0.6059(9) 0.0114(6) 0.055(3) Uani 1 1 d . . . C2BB C -0.1324(6) 0.6879(13) -0.0332(6) 0.073(5) Uani 1 1 d . . . H2BB H -0.1084 0.7072 -0.0666 0.087 Uiso 1 1 calc R . . C3BB C -0.1834(5) 0.7433(11) -0.0297(6) 0.068(3) Uani 1 1 d . . . H3BB H -0.1929 0.8009 -0.0596 0.081 Uiso 1 1 calc R . . C4BB C -0.2184(7) 0.7167(16) 0.0146(9) 0.087(5) Uani 1 1 d . . . H4BB H -0.2522 0.7565 0.0165 0.104 Uiso 1 1 calc R . . C5BB C -0.2079(7) 0.6357(14) 0.0569(10) 0.093(5) Uani 1 1 d . . . H5BB H -0.2350 0.6172 0.0865 0.112 Uiso 1 1 calc R . . C6BB C -0.1549(8) 0.5762(12) 0.0572(8) 0.087(5) Uani 1 1 d . . . H6BB H -0.1462 0.5189 0.0876 0.104 Uiso 1 1 calc R . . C1BC C -0.0180(5) 0.1970(7) 0.3498(6) 0.038(2) Uani 1 1 d . . . C2BC C -0.0086(5) 0.1385(7) 0.4152(7) 0.050(3) Uani 1 1 d . . . H2BC H 0.0312 0.1377 0.4555 0.060 Uiso 1 1 calc R . . C3BC C -0.0575(6) 0.0789(8) 0.4239(8) 0.064(4) Uani 1 1 d . . . H3BC H -0.0503 0.0384 0.4694 0.077 Uiso 1 1 calc R . . C4BC C -0.1186(6) 0.0808(9) 0.3621(7) 0.063(3) Uani 1 1 d . . . H4BC H -0.1517 0.0424 0.3682 0.075 Uiso 1 1 calc R . . C5BC C -0.1289(6) 0.1371(12) 0.2955(7) 0.076(4) Uani 1 1 d . . . H5BC H -0.1685 0.1393 0.2548 0.091 Uiso 1 1 calc R . . C6BC C -0.0755(5) 0.1940(10) 0.2905(6) 0.057(3) Uani 1 1 d . . . H6BC H -0.0807 0.2310 0.2435 0.068 Uiso 1 1 calc R . . C1BD C 0.0960(5) 0.1923(8) 0.3418(6) 0.050(3) Uiso 1 1 d G . . C2BD C 0.1487(6) 0.1810(12) 0.4116(8) 0.072(3) Uiso 1 1 d G . . H2BD H 0.1497 0.2175 0.4577 0.086 Uiso 1 1 calc R . . C3BD C 0.2009(6) 0.1183(9) 0.4179(8) 0.072(3) Uiso 1 1 d G . . H3BD H 0.2362 0.1149 0.4650 0.087 Uiso 1 1 calc R . . C4BD C 0.1963(7) 0.0639(10) 0.3511(8) 0.077(3) Uiso 1 1 d G . . H4BD H 0.2292 0.0203 0.3534 0.092 Uiso 1 1 calc R . . C5BD C 0.1471(7) 0.0688(11) 0.2817(10) 0.090(4) Uiso 1 1 d G . . H5BD H 0.1459 0.0295 0.2370 0.108 Uiso 1 1 calc R . . C6BD C 0.0935(7) 0.1395(10) 0.2775(8) 0.077(4) Uiso 1 1 d G . . H6BD H 0.0591 0.1455 0.2295 0.092 Uiso 1 1 calc R . . O1G O 0.1385(7) 0.1334(10) 0.0465(8) 0.129(4) Uiso 1 1 d G . . C2G C 0.1233(15) 0.228(2) 0.067(3) 0.152(8) Uiso 1 1 d G . . H2G H 0.1513 0.2687 0.1058 0.183 Uiso 1 1 calc R . . C3G C 0.0677(9) 0.2501(11) 0.0277(13) 0.119(5) Uiso 1 1 d G . . H3G H 0.0518 0.3116 0.0334 0.143 Uiso 1 1 calc R . . C4G C 0.0311(14) 0.187(2) -0.0222(17) 0.167(11) Uiso 1 1 d G . . H4G H -0.0118 0.1873 -0.0540 0.200 Uiso 1 1 calc R . . C5G C 0.0848(12) 0.1106(19) -0.0091(15) 0.157(8) Uiso 1 1 d G . . H5G H 0.0794 0.0528 -0.0387 0.188 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1A 0.033(3) 0.031(3) 0.038(3) -0.013(3) 0.005(3) 0.003(3) C1A 0.026(4) 0.035(4) 0.041(5) -0.012(4) 0.016(4) 0.003(4) C2A 0.038(5) 0.047(5) 0.042(6) -0.009(5) 0.021(5) 0.008(4) C3A 0.052(6) 0.054(6) 0.029(5) 0.012(5) 0.007(5) -0.022(5) C4A 0.052(7) 0.105(10) 0.048(6) 0.013(7) 0.021(6) -0.036(7) C5A 0.042(6) 0.089(9) 0.036(5) 0.020(6) 0.005(5) -0.030(6) O6A 0.052(4) 0.086(5) 0.022(3) 0.003(3) 0.011(3) -0.037(4) C6A 0.040(5) 0.090(8) 0.034(5) 0.011(6) 0.016(5) -0.020(6) C1AA 0.042(5) 0.027(4) 0.044(5) -0.015(4) 0.020(4) -0.014(4) C2AA 0.099(10) 0.080(8) 0.032(6) -0.012(6) 0.024(6) -0.036(7) C3AA 0.070(8) 0.103(10) 0.068(8) -0.025(7) 0.025(7) -0.057(8) C4AA 0.088(10) 0.073(8) 0.095(11) -0.032(8) 0.069(9) -0.047(7) C5AA 0.075(8) 0.044(6) 0.069(7) -0.017(5) 0.043(7) -0.010(6) C6AA 0.060(7) 0.044(6) 0.054(6) 0.007(5) 0.024(6) 0.004(5) C1AC 0.040(5) 0.045(5) 0.038(5) 0.012(4) 0.004(5) -0.010(4) C2AC 0.057(8) 0.177(17) 0.060(8) -0.051(10) 0.025(7) -0.042(10) C3AC 0.057(8) 0.113(12) 0.077(10) -0.022(9) 0.015(8) -0.051(8) C4AC 0.066(8) 0.088(11) 0.060(8) -0.017(8) -0.004(7) 0.002(7) C5AC 0.088(9) 0.046(7) 0.118(11) -0.008(8) 0.047(9) 0.001(7) C6AC 0.059(8) 0.037(6) 0.131(13) -0.033(7) 0.045(9) -0.015(6) C1AD 0.043(6) 0.080(8) 0.019(4) 0.003(5) 0.002(4) -0.031(6) C2AD 0.093(9) 0.042(6) 0.094(9) -0.005(6) 0.057(8) -0.016(6) C3AD 0.130(12) 0.062(8) 0.143(13) 0.019(8) 0.107(12) -0.040(8) C4AD 0.053(7) 0.084(8) 0.051(6) 0.017(6) 0.021(6) -0.019(6) C5AD 0.043(7) 0.17(2) 0.091(11) 0.064(12) -0.005(7) -0.044(10) C6AD 0.027(6) 0.124(10) 0.083(8) 0.060(8) 0.012(6) -0.012(6) O1B 0.049(5) 0.081(5) 0.048(4) 0.004(4) 0.013(4) -0.046(4) C1B 0.050(6) 0.075(7) 0.025(4) 0.012(5) 0.000(4) -0.052(6) C2B 0.051(7) 0.111(10) 0.033(6) -0.005(6) 0.011(5) -0.043(7) C3B 0.038(6) 0.083(8) 0.020(4) 0.001(5) 0.006(4) -0.024(5) C4B 0.039(6) 0.085(8) 0.028(5) -0.008(5) 0.019(5) -0.011(6) C5B 0.038(6) 0.059(6) 0.028(5) -0.002(4) 0.006(4) -0.037(5) O6B 0.025(3) 0.036(3) 0.033(3) -0.001(3) 0.010(3) -0.001(2) C6B 0.044(5) 0.028(4) 0.025(4) -0.005(4) 0.015(4) -0.005(4) C1BA 0.042(6) 0.066(7) 0.034(5) 0.020(5) 0.005(4) -0.021(5) C2BA 0.045(7) 0.060(7) 0.092(9) 0.008(7) 0.014(7) -0.011(6) C3BA 0.069(9) 0.072(8) 0.155(14) -0.045(10) 0.072(9) -0.034(7) C4BA 0.085(10) 0.033(5) 0.077(8) 0.004(5) 0.044(7) -0.008(5) C5BA 0.054(8) 0.139(14) 0.043(6) -0.034(8) -0.005(6) -0.009(8) C6BA 0.050(8) 0.147(15) 0.065(8) -0.033(9) 0.023(7) -0.056(9) C1BB 0.043(6) 0.075(7) 0.040(6) 0.010(6) 0.006(5) -0.027(6) C2BB 0.047(7) 0.141(14) 0.025(5) 0.038(7) 0.003(5) -0.014(8) C3BB 0.039(6) 0.113(9) 0.047(6) 0.047(6) 0.009(5) 0.009(6) C4BB 0.063(8) 0.127(15) 0.069(9) 0.012(10) 0.018(8) -0.007(9) C5BB 0.082(10) 0.128(14) 0.083(10) 0.021(11) 0.046(9) 0.032(10) C6BB 0.100(11) 0.106(12) 0.084(9) 0.023(9) 0.071(9) -0.016(10) C1BC 0.054(7) 0.039(5) 0.035(5) -0.009(4) 0.033(5) -0.002(5) C2BC 0.046(6) 0.035(5) 0.080(8) -0.008(6) 0.037(6) -0.004(5) C3BC 0.088(10) 0.035(6) 0.092(9) 0.005(5) 0.062(9) -0.014(6) C4BC 0.069(7) 0.068(8) 0.067(7) -0.037(6) 0.044(7) -0.037(6) C5BC 0.058(7) 0.139(12) 0.046(7) -0.031(8) 0.036(6) -0.057(8) C6BC 0.036(5) 0.098(9) 0.043(6) -0.020(6) 0.022(5) -0.034(6) _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 O1A C1A 1.425(10) . ? C1A C2A 1.454(14) . ? C1A C1AA 1.513(12) . ? C1A C1AB 1.512(12) . ? C2A C3A 1.194(13) . ? C3A C4A 1.397(15) . ? C4A C5A 1.199(15) . ? C5A C6A 1.471(15) . ? O6A C6A 1.394(12) . ? C6A C1AD 1.535(17) . ? C6A C1AC 1.594(15) . ? C1AA C2AA 1.409(16) . ? C1AA C6AA 1.415(14) . ? C2AA C3AA 1.340(17) . ? C3AA C4AA 1.374(19) . ? C4AA C5AA 1.322(19) . ? C5AA C6AA 1.395(16) . ? C1AB C2AB 1.3900 . ? C1AB C6AB 1.459(16) . ? C2AB C3AB 1.493(19) . ? C3AB C4AB 1.364(19) . ? C4AB C5AB 1.302(17) . ? C5AB C6AB 1.359(18) . ? C1AC C2AC 1.345(17) . ? C1AC C6AC 1.372(16) . ? C2AC C3AC 1.34(2) . ? C3AC C4AC 1.32(2) . ? C4AC C5AC 1.44(2) . ? C5AC C6AC 1.382(19) . ? C1AD C2AD 1.349(15) . ? C1AD C6AD 1.430(16) . ? C2AD C3AD 1.35(2) . ? C3AD C4AD 1.426(19) . ? C4AD C5AD 1.451(18) . ? C5AD C6AD 1.35(2) . ? O1B C1B 1.483(10) . ? C1B C1BA 1.461(15) . ? C1B C2B 1.478(15) . ? C1B C1BB 1.557(18) . ? C2B C3B 1.199(15) . ? C3B C4B 1.353(15) . ? C4B C5B 1.226(14) . ? C5B C6B 1.484(13) . ? O6B C6B 1.433(10) . ? C6B C1BD 1.521(13) . ? C6B C1BC 1.579(13) . ? C1BA C2BA 1.383(17) . ? C1BA C6BA 1.408(15) . ? C2BA C3BA 1.355(19) . ? C3BA C4BA 1.328(19) . ? C4BA C5BA 1.380(17) . ? C5BA C6BA 1.443(18) . ? C1BB C2BB 1.344(18) . ? C1BB C6BB 1.375(17) . ? C2BB C3BB 1.369(18) . ? C3BB C4BB 1.290(18) . ? C4BB C5BB 1.31(2) . ? C5BB C6BB 1.42(2) . ? C1BC C2BC 1.343(15) . ? C1BC C6BC 1.351(14) . ? C2BC C3BC 1.394(14) . ? C3BC C4BC 1.427(19) . ? C4BC C5BC 1.338(19) . ? C5BC C6BC 1.435(15) . ? C1BD C2BD 1.3900 . ? C1BD C6BD 1.307(17) . ? C2BD C3BD 1.410(17) . ? C3BD C4BD 1.343(17) . ? C4BD C5BD 1.336(19) . ? C5BD C6BD 1.509(19) . ? O1G C2G 1.4200 . ? O1G C5G 1.30(3) . ? C2G C3G 1.23(3) . ? C3G C4G 1.31(3) . ? C4G C5G 1.54(3) . ? 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 O1A C1A C2A 110.9(7) . . ? O1A C1A C1AA 110.2(7) . . ? C2A C1A C1AA 111.2(8) . . ? O1A C1A C1AB 109.5(7) . . ? C2A C1A C1AB 107.0(7) . . ? C1AA C1A C1AB 107.9(7) . . ? C3A C2A C1A 177.4(10) . . ? C2A C3A C4A 175.2(11) . . ? C5A C4A C3A 175.8(15) . . ? C4A C5A C6A 176.9(12) . . ? O6A C6A C5A 111.8(8) . . ? O6A C6A C1AD 111.3(10) . . ? C5A C6A C1AD 109.9(9) . . ? O6A C6A C1AC 107.2(8) . . ? C5A C6A C1AC 106.2(10) . . ? C1AD C6A C1AC 110.2(8) . . ? C2AA C1AA C6AA 118.5(10) . . ? C2AA C1AA C1A 121.9(9) . . ? C6AA C1AA C1A 119.4(9) . . ? C3AA C2AA C1AA 116.5(12) . . ? C4AA C3AA C2AA 125.2(13) . . ? C5AA C4AA C3AA 119.1(11) . . ? C4AA C5AA C6AA 120.0(12) . . ? C5AA C6AA C1AA 120.3(11) . . ? C2AB C1AB C6AB 121.3(10) . . ? C2AB C1AB C1A 122.2(9) . . ? C6AB C1AB C1A 116.5(8) . . ? C1AB C2AB C3AB 114.7(11) . . ? C4AB C3AB C2AB 117.2(14) . . ? C5AB C4AB C3AB 128.9(13) . . ? C4AB C5AB C6AB 116.8(13) . . ? C5AB C6AB C1AB 121.0(12) . . ? C2AC C1AC C6AC 117.0(11) . . ? C2AC C1AC C6A 123.6(11) . . ? C6AC C1AC C6A 119.3(9) . . ? C3AC C2AC C1AC 122.4(13) . . ? C4AC C3AC C2AC 121.1(12) . . ? C3AC C4AC C5AC 121.3(13) . . ? C6AC C5AC C4AC 114.0(13) . . ? C1AC C6AC C5AC 124.0(12) . . ? C2AD C1AD C6AD 117.3(11) . . ? C2AD C1AD C6A 122.9(11) . . ? C6AD C1AD C6A 119.4(9) . . ? C1AD C2AD C3AD 121.5(12) . . ? C2AD C3AD C4AD 124.3(11) . . ? C3AD C4AD C5AD 113.3(14) . . ? C6AD C5AD C4AD 121.2(15) . . ? C5AD C6AD C1AD 122.0(11) . . ? C1BA C1B C2B 112.2(10) . . ? C1BA C1B O1B 105.1(8) . . ? C2B C1B O1B 105.9(8) . . ? C1BA C1B C1BB 115.1(8) . . ? C2B C1B C1BB 110.9(9) . . ? O1B C1B C1BB 106.8(9) . . ? C3B C2B C1B 177.7(13) . . ? C2B C3B C4B 176.9(13) . . ? C5B C4B C3B 174.9(12) . . ? C4B C5B C6B 175.0(11) . . ? O6B C6B C5B 108.2(7) . . ? O6B C6B C1BD 107.0(7) . . ? C5B C6B C1BD 112.6(8) . . ? O6B C6B C1BC 107.3(6) . . ? C5B C6B C1BC 110.8(7) . . ? C1BD C6B C1BC 110.6(7) . . ? C2BA C1BA C6BA 117.0(11) . . ? C2BA C1BA C1B 123.0(9) . . ? C6BA C1BA C1B 119.5(11) . . ? C3BA C2BA C1BA 119.3(11) . . ? C4BA C3BA C2BA 127.6(13) . . ? C3BA C4BA C5BA 115.4(12) . . ? C4BA C5BA C6BA 120.5(12) . . ? C1BA C6BA C5BA 119.7(13) . . ? C2BB C1BB C6BB 118.8(13) . . ? C2BB C1BB C1B 120.6(10) . . ? C6BB C1BB C1B 120.4(11) . . ? C1BB C2BB C3BB 120.4(11) . . ? C4BB C3BB C2BB 120.9(14) . . ? C3BB C4BB C5BB 122.2(17) . . ? C4BB C5BB C6BB 119.5(15) . . ? C1BB C6BB C5BB 118.1(15) . . ? C2BC C1BC C6BC 118.2(10) . . ? C2BC C1BC C6B 117.9(9) . . ? C6BC C1BC C6B 123.7(9) . . ? C1BC C2BC C3BC 121.3(12) . . ? C2BC C3BC C4BC 119.1(11) . . ? C5BC C4BC C3BC 120.9(11) . . ? C4BC C5BC C6BC 116.2(12) . . ? C1BC C6BC C5BC 124.2(11) . . ? C2BD C1BD C6BD 117.9(12) . . ? C2BD C1BD C6B 120.5(9) . . ? C6BD C1BD C6B 121.4(10) . . ? C3BD C2BD C1BD 124.9(12) . . ? C2BD C3BD C4BD 115.5(12) . . ? C3BD C4BD C5BD 123.8(14) . . ? C6BD C5BD C4BD 118.4(14) . . ? C5BD C6BD C1BD 119.3(13) . . ? C2G O1G C5G 100.0(18) . . ? C3G C2G O1G 110.6(19) . . ? C4G C3G C2G 120(2) . . ? C3G C4G C5G 94(2) . . ? C4G C5G O1G 115(2) . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 25.77 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 0.910 _refine_diff_density_min -0.685 _refine_diff_density_rms 0.087 data_c:\dejana\struct~1\t7furs\t7furs _database_code_CSD 166352 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H30 O4' _chemical_formula_weight 550.62 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.3054(2) _cell_length_b 15.3908(4) _cell_length_c 11.4520(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.8920(10) _cell_angle_gamma 90.00 _cell_volume 1458.54(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.254 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 580 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4981 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0538 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.92 _reflns_number_total 3002 _reflns_number_gt 1887 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0804P)^2^+0.4573P] 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 3002 _refine_ls_number_parameters 189 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1043 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1679 _refine_ls_wR_factor_gt 0.1437 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 1.377 _refine_ls_shift/su_mean 0.278 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 0.34400(17) 0.04715(10) 0.16148(12) 0.0311(4) Uani 1 1 d D . . C1A C 0.1080(2) -0.01557(13) 0.24073(17) 0.0260(5) Uani 1 1 d . . . C1B C 0.3433(2) -0.10787(13) 0.18578(17) 0.0257(5) Uani 1 1 d . . . C2 C 0.3781(2) -0.01098(13) 0.35389(18) 0.0277(5) Uani 1 1 d . . . C3 C 0.4553(2) -0.00385(13) 0.44656(18) 0.0275(5) Uani 1 1 d . . . C1 C 0.2918(2) -0.02103(13) 0.23577(17) 0.0252(5) Uani 1 1 d . . . C2A C 0.0384(3) 0.02055(15) 0.33486(18) 0.0337(5) Uani 1 1 d . . . H2A H 0.1035 0.0379 0.4009 0.040 Uiso 1 1 calc R . . C6A C 0.0094(3) -0.04234(15) 0.14345(18) 0.0323(5) Uani 1 1 d . . . H6A H 0.0548 -0.0673 0.0800 0.039 Uiso 1 1 calc R . . C2B C 0.3176(3) -0.18379(15) 0.2464(2) 0.0370(6) Uani 1 1 d . . . H2B H 0.2685 -0.1814 0.3164 0.044 Uiso 1 1 calc R . . C5A C -0.1565(3) -0.03198(16) 0.1406(2) 0.0377(6) Uani 1 1 d . . . H5A H -0.2219 -0.0500 0.0751 0.045 Uiso 1 1 calc R . . C6B C 0.4152(3) -0.11233(15) 0.0812(2) 0.0346(5) Uani 1 1 d . . . H6B H 0.4323 -0.0619 0.0393 0.041 Uiso 1 1 calc R . . C4A C -0.2251(3) 0.00482(16) 0.2339(2) 0.0385(6) Uani 1 1 d . . . H4A H -0.3366 0.0120 0.2313 0.046 Uiso 1 1 calc R . . C3A C -0.1279(3) 0.03111(16) 0.3315(2) 0.0414(6) Uani 1 1 d . . . H3A H -0.1739 0.0558 0.3949 0.050 Uiso 1 1 calc R . . C5B C 0.4618(3) -0.19254(17) 0.0390(2) 0.0464(7) Uani 1 1 d . . . H5B H 0.5103 -0.1954 -0.0312 0.056 Uiso 1 1 calc R . . C4B C 0.4370(3) -0.26719(17) 0.0997(2) 0.0502(7) Uani 1 1 d . . . H4B H 0.4687 -0.3205 0.0711 0.060 Uiso 1 1 calc R . . C3B C 0.3644(3) -0.26299(16) 0.2040(2) 0.0477(7) Uani 1 1 d . . . H3B H 0.3470 -0.3136 0.2455 0.057 Uiso 1 1 calc R . . H1 H 0.285(3) 0.0964(17) 0.174(3) 0.078(10) Uiso 1 1 d D . . O1G O -0.1605(3) -0.30265(18) -0.0338(2) 0.0951(8) Uiso 1 1 d . . . C4G C -0.0214(4) -0.2056(2) -0.1229(3) 0.0643(8) Uani 1 1 d . . . H4G H 0.0564 -0.1642 -0.1368 0.077 Uiso 1 1 calc R . . C3G C -0.1465(4) -0.2311(2) -0.2003(2) 0.0659(9) Uani 1 1 d . . . H3G H -0.1708 -0.2106 -0.2762 0.079 Uiso 1 1 calc R . . C5G C -0.0302(4) -0.2493(2) -0.0261(3) 0.0692(9) Uani 1 1 d . . . H5G H 0.0433 -0.2445 0.0396 0.083 Uiso 1 1 calc R . . C2G C -0.2268(4) -0.2915(2) -0.1452(4) 0.0770(11) Uani 1 1 d . . . H2G H -0.3160 -0.3219 -0.1785 0.092 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0309(9) 0.0312(9) 0.0319(8) 0.0051(7) 0.0061(7) -0.0008(7) C1A 0.0239(11) 0.0288(11) 0.0252(11) 0.0037(9) 0.0006(9) -0.0003(8) C1B 0.0198(10) 0.0304(11) 0.0260(11) -0.0019(9) -0.0033(9) -0.0005(8) C2 0.0238(11) 0.0300(11) 0.0294(12) -0.0031(9) 0.0019(10) -0.0005(9) C3 0.0237(11) 0.0288(12) 0.0299(11) -0.0024(9) 0.0016(9) -0.0020(8) C1 0.0254(11) 0.0291(11) 0.0214(10) 0.0002(8) 0.0030(9) -0.0026(8) C2A 0.0296(12) 0.0458(14) 0.0255(11) -0.0010(10) 0.0007(9) 0.0034(10) C6A 0.0265(12) 0.0439(13) 0.0263(11) -0.0055(10) 0.0008(9) -0.0016(9) C2B 0.0438(14) 0.0343(13) 0.0327(12) -0.0002(10) 0.0021(11) -0.0036(10) C5A 0.0268(13) 0.0474(15) 0.0376(13) -0.0002(11) -0.0041(10) -0.0033(10) C6B 0.0352(13) 0.0366(13) 0.0321(12) -0.0028(10) 0.0043(10) -0.0003(10) C4A 0.0239(12) 0.0476(15) 0.0442(14) 0.0087(11) 0.0050(11) 0.0003(10) C3A 0.0338(14) 0.0592(16) 0.0325(12) 0.0007(11) 0.0103(11) 0.0072(11) C5B 0.0468(15) 0.0510(16) 0.0424(14) -0.0155(12) 0.0097(12) 0.0046(12) C4B 0.0531(16) 0.0366(15) 0.0595(17) -0.0174(13) -0.0027(14) 0.0074(12) C3B 0.0556(16) 0.0320(14) 0.0535(16) 0.0006(12) -0.0060(14) -0.0026(11) C4G 0.0586(19) 0.0535(19) 0.083(2) 0.0034(17) 0.0204(18) 0.0037(14) C3G 0.069(2) 0.094(3) 0.0337(15) -0.0099(16) 0.0006(15) 0.0232(19) C5G 0.067(2) 0.063(2) 0.072(2) -0.0084(17) -0.0230(17) 0.0076(16) C2G 0.055(2) 0.061(2) 0.113(3) -0.042(2) -0.004(2) 0.0011(16) _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 C1 1.441(2) . ? C1A C2A 1.383(3) . ? C1A C6A 1.388(3) . ? C1A C1 1.535(3) . ? C1B C2B 1.385(3) . ? C1B C6B 1.384(3) . ? C1B C1 1.529(3) . ? C2 C3 1.197(3) . ? C2 C1 1.484(3) . ? C3 C3 1.381(4) 3_656 ? C2A C3A 1.388(3) . ? C6A C5A 1.384(3) . ? C2B C3B 1.380(3) . ? C5A C4A 1.375(3) . ? C6B C5B 1.393(3) . ? C4A C3A 1.383(3) . ? C5B C4B 1.368(4) . ? C4B C3B 1.385(4) . ? O1G C5G 1.355(4) . ? O1G C2G 1.356(4) . ? C4G C5G 1.304(4) . ? C4G C3G 1.365(4) . ? C3G C2G 1.334(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2A C1A C6A 119.19(19) . . ? C2A C1A C1 122.30(18) . . ? C6A C1A C1 118.36(18) . . ? C2B C1B C6B 119.2(2) . . ? C2B C1B C1 119.31(19) . . ? C6B C1B C1 121.47(19) . . ? C3 C2 C1 176.5(2) . . ? C2 C3 C3 179.7(3) . 3_656 ? O1 C1 C2 108.42(16) . . ? O1 C1 C1B 107.92(16) . . ? C2 C1 C1B 107.67(16) . . ? O1 C1 C1A 109.40(16) . . ? C2 C1 C1A 111.43(16) . . ? C1B C1 C1A 111.87(16) . . ? C1A C2A C3A 120.5(2) . . ? C5A C6A C1A 120.2(2) . . ? C3B C2B C1B 120.6(2) . . ? C4A C5A C6A 120.5(2) . . ? C1B C6B C5B 119.8(2) . . ? C5A C4A C3A 119.8(2) . . ? C4A C3A C2A 119.9(2) . . ? C4B C5B C6B 120.6(2) . . ? C5B C4B C3B 119.7(2) . . ? C2B C3B C4B 120.1(2) . . ? C5G O1G C2G 104.0(3) . . ? C5G C4G C3G 108.0(3) . . ? C2G C3G C4G 106.1(3) . . ? C4G C5G O1G 111.1(3) . . ? C3G C2G O1G 110.7(3) . . ? _diffrn_measured_fraction_theta_max 0.861 _diffrn_reflns_theta_full 27.92 _diffrn_measured_fraction_theta_full 0.861 _refine_diff_density_max 0.236 _refine_diff_density_min -0.721 _refine_diff_density_rms 0.057 data_c:\dejana\struct~1\t7thf\t7thf _database_code_CSD 166353 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H30 O4' _chemical_formula_weight 550.62 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.2907(4) _cell_length_b 16.0716(9) _cell_length_c 11.4225(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.061(3) _cell_angle_gamma 90.00 _cell_volume 1519.82(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 580 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5754 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3412 _reflns_number_gt 2524 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1443P)^2^+1.7956P] 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 3412 _refine_ls_number_parameters 175 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1137 _refine_ls_R_factor_gt 0.0887 _refine_ls_wR_factor_ref 0.2722 _refine_ls_wR_factor_gt 0.2466 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 1.799 _refine_ls_shift/su_mean 0.475 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 0.8623(2) 0.04221(13) 0.16043(16) 0.0322(5) Uani 1 1 d D . . C1 C 0.8013(3) -0.01982(16) 0.2361(2) 0.0260(5) Uani 1 1 d . . . C2 C 0.8845(3) -0.01144(16) 0.3537(2) 0.0275(5) Uani 1 1 d . . . C3 C 0.9579(3) -0.00435(16) 0.4470(2) 0.0282(6) Uani 1 1 d . . . C1A C 0.6180(3) -0.00871(16) 0.2429(2) 0.0275(5) Uani 1 1 d . . . C6A C 0.5176(3) -0.03377(19) 0.1478(2) 0.0374(7) Uani 1 1 d . . . H6A H 0.5612 -0.0606 0.0846 0.045 Uiso 1 1 calc R . . C1B C 0.8421(3) -0.10515(17) 0.1869(2) 0.0295(6) Uani 1 1 d . . . C2A C 0.5499(3) 0.0299(2) 0.3366(2) 0.0382(7) Uani 1 1 d . . . H2A H 0.6153 0.0464 0.4011 0.046 Uiso 1 1 calc R . . C3A C 0.3844(4) 0.0443(2) 0.3349(3) 0.0476(8) Uani 1 1 d . . . H3A H 0.3398 0.0702 0.3984 0.057 Uiso 1 1 calc R . . C2B C 0.9109(3) -0.11396(19) 0.0794(2) 0.0371(6) Uani 1 1 d . . . H2B H 0.9372 -0.0671 0.0366 0.044 Uiso 1 1 calc R . . C5A C 0.3523(3) -0.0188(2) 0.1470(3) 0.0455(8) Uani 1 1 d . . . H5A H 0.2861 -0.0355 0.0830 0.055 Uiso 1 1 calc R . . C6B C 0.8055(4) -0.17624(19) 0.2488(3) 0.0447(7) Uani 1 1 d . . . H6B H 0.7636 -0.1703 0.3223 0.054 Uiso 1 1 calc R . . C3B C 0.9404(4) -0.1926(2) 0.0361(3) 0.0511(8) Uani 1 1 d . . . H3B H 0.9858 -0.1979 -0.0362 0.061 Uiso 1 1 calc R . . C4A C 0.2861(3) 0.0203(2) 0.2398(3) 0.0462(8) Uani 1 1 d . . . H4A H 0.1756 0.0307 0.2384 0.055 Uiso 1 1 calc R . . C4B C 0.9045(5) -0.2624(2) 0.0970(4) 0.0576(10) Uani 1 1 d . . . H4B H 0.9286 -0.3148 0.0683 0.069 Uiso 1 1 calc R . . C5B C 0.8282(3) -0.25343(12) 0.2073(2) 0.0591(10) Uani 1 1 d . . . H5B H 0.7956 -0.2999 0.2484 0.071 Uiso 1 1 calc R . . O1GB O 0.7053(3) 0.19342(12) 0.1813(2) 0.0523(12) Uiso 0.781(11) 1 d PR A 1 O1GA O 0.7493(3) 0.19522(12) 0.1400(2) 0.037(3) Uiso 0.219(11) 1 d PR A . C2GB C 0.7316(3) 0.27860(12) 0.2039(2) 0.0684(16) Uiso 0.845(14) 1 d PR A 1 H2G1 H 0.8443 0.2888 0.2268 0.082 Uiso 0.845(14) 1 calc PR A 1 H2G2 H 0.6658 0.2974 0.2664 0.082 Uiso 0.845(14) 1 calc PR A 1 C2GA C 0.7872(19) 0.2788(9) 0.1721(14) 0.025(5) Uiso 0.155(14) 1 d P . . H2G3 H 0.9003 0.2912 0.1627 0.030 Uiso 0.155(14) 1 calc PR A 1 H2G4 H 0.7610 0.2904 0.2523 0.030 Uiso 0.155(14) 1 calc PR A 1 C3G C 0.6840(7) 0.3242(4) 0.0893(5) 0.0880(15) Uiso 1 1 d . A 1 C5GB C 0.5535(10) 0.1939(5) 0.1218(8) 0.058(3) Uiso 0.496(16) 1 d P A 1 H5G1 H 0.4689 0.2057 0.1748 0.070 Uiso 0.496(16) 1 calc PR A 1 H5G2 H 0.5312 0.1409 0.0836 0.070 Uiso 0.496(16) 1 calc PR A 1 C5GA C 0.6081(13) 0.1924(6) 0.0573(10) 0.075(4) Uiso 0.504(16) 1 d P . . H5G3 H 0.6333 0.1607 -0.0116 0.090 Uiso 0.504(16) 1 calc PR A 1 H5G4 H 0.5188 0.1654 0.0936 0.090 Uiso 0.504(16) 1 calc PR A 1 C4G C 0.5682(8) 0.2668(4) 0.0276(5) 0.0963(16) Uiso 1 1 d . A 1 H1 H 0.846(5) 0.0998(17) 0.178(3) 0.069(12) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0306(10) 0.0346(11) 0.0315(10) 0.0056(8) 0.0013(7) -0.0053(8) C1 0.0242(11) 0.0314(13) 0.0221(11) 0.0016(9) -0.0028(9) -0.0029(9) C2 0.0219(11) 0.0315(13) 0.0288(13) -0.0024(10) -0.0013(9) -0.0004(9) C3 0.0232(11) 0.0329(13) 0.0283(13) -0.0032(10) -0.0009(9) -0.0004(9) C1A 0.0245(12) 0.0317(13) 0.0258(12) 0.0037(10) -0.0032(9) -0.0024(9) C6A 0.0284(13) 0.0528(17) 0.0302(13) -0.0011(12) -0.0055(10) -0.0035(12) C1B 0.0259(12) 0.0345(14) 0.0272(12) -0.0033(10) -0.0060(9) -0.0008(10) C2A 0.0323(14) 0.0495(17) 0.0326(14) -0.0038(12) -0.0012(10) 0.0033(12) C3A 0.0333(15) 0.063(2) 0.0472(17) 0.0006(15) 0.0083(13) 0.0094(14) C2B 0.0380(14) 0.0431(16) 0.0303(13) -0.0033(11) 0.0043(11) -0.0002(12) C5A 0.0270(14) 0.066(2) 0.0419(16) 0.0052(14) -0.0110(11) -0.0058(13) C6B 0.063(2) 0.0358(16) 0.0359(15) -0.0003(12) 0.0060(13) -0.0045(13) C3B 0.0531(19) 0.059(2) 0.0413(17) -0.0188(15) 0.0039(14) 0.0018(15) C4A 0.0231(13) 0.061(2) 0.0546(18) 0.0150(15) 0.0008(12) 0.0020(12) C4B 0.062(2) 0.0421(19) 0.068(2) -0.0252(17) -0.0048(17) 0.0042(16) C5B 0.082(3) 0.0353(17) 0.060(2) -0.0008(15) 0.0005(18) -0.0071(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.429(3) . ? C1 C2 1.483(3) . ? C1 C1B 1.527(4) . ? C1 C1A 1.537(3) . ? C2 C3 1.204(3) . ? C3 C3 1.373(5) 3_756 ? C1A C2A 1.383(4) . ? C1A C6A 1.393(3) . ? C6A C5A 1.391(4) . ? C1B C6B 1.386(4) . ? C1B C2B 1.388(4) . ? C2A C3A 1.390(4) . ? C3A C4A 1.378(5) . ? C2B C3B 1.384(4) . ? C5A C4A 1.372(5) . ? C6B C5B 1.345(4) . ? C3B C4B 1.360(6) . ? C4B C5B 1.446(5) . ? O1GB C5GB 1.398(8) . ? O1GB C2GB 1.4078 . ? O1GA C2GA 1.422(15) . ? O1GA C5GA 1.465(10) . ? C2GB C3G 1.533(6) . ? C2GA C3G 1.440(16) . ? C3G C4G 1.482(8) . ? C5GB C4G 1.601(11) . ? C5GA C4G 1.282(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 108.78(19) . . ? O1 C1 C1B 108.2(2) . . ? C2 C1 C1B 108.3(2) . . ? O1 C1 C1A 109.43(19) . . ? C2 C1 C1A 110.9(2) . . ? C1B C1 C1A 111.2(2) . . ? C3 C2 C1 177.3(2) . . ? C2 C3 C3 179.5(4) . 3_756 ? C2A C1A C6A 118.8(2) . . ? C2A C1A C1 122.5(2) . . ? C6A C1A C1 118.6(2) . . ? C5A C6A C1A 120.2(3) . . ? C6B C1B C2B 118.6(3) . . ? C6B C1B C1 119.6(2) . . ? C2B C1B C1 121.8(2) . . ? C1A C2A C3A 120.5(3) . . ? C4A C3A C2A 120.4(3) . . ? C3B C2B C1B 119.8(3) . . ? C4A C5A C6A 120.6(3) . . ? C5B C6B C1B 122.8(3) . . ? C4B C3B C2B 121.5(3) . . ? C5A C4A C3A 119.5(3) . . ? C3B C4B C5B 118.8(3) . . ? C6B C5B C4B 118.3(3) . . ? C5GB O1GB C2GB 102.2(4) . . ? C2GA O1GA C5GA 110.7(7) . . ? O1GB C2GB C3G 106.1(2) . . ? O1GA C2GA C3G 101.1(9) . . ? C2GA C3G C4G 110.2(8) . . ? C2GA C3G C2GB 23.1(7) . . ? C4G C3G C2GB 103.9(4) . . ? O1GB C5GB C4G 103.4(6) . . ? C4G C5GA O1GA 109.1(7) . . ? C5GA C4G C3G 107.6(7) . . ? C5GA C4G C5GB 33.5(6) . . ? C3G C4G C5GB 101.9(5) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.721 _refine_diff_density_min -0.593 _refine_diff_density_rms 0.074 data_c:\dejana\struct~1\thesis~1\t7thios\t7thios _database_code_CSD 166354 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H28 O2 S2.53' _chemical_formula_weight 573.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.2043(2) _cell_length_b 16.0186(5) _cell_length_c 11.4831(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.521(2) _cell_angle_gamma 90.00 _cell_volume 1504.43(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.266 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 601 _exptl_absorpt_coefficient_mu 0.245 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6644 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 24.71 _reflns_number_total 2545 _reflns_number_gt 1981 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1373P)^2^+2.1491P] 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 0.008(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2545 _refine_ls_number_parameters 190 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0932 _refine_ls_R_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.2286 _refine_ls_wR_factor_gt 0.2118 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 1.523 _refine_ls_shift/su_mean 0.399 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 0.1487(3) 0.53485(15) 0.33938(19) 0.0281(6) Uani 1 1 d D . . C2 C 0.1190(4) 0.4827(2) 0.1456(3) 0.0253(8) Uani 1 1 d . . . C1 C 0.2053(4) 0.4712(2) 0.2630(3) 0.0236(8) Uani 1 1 d . . . C1A C 0.3906(4) 0.4790(2) 0.2596(3) 0.0231(8) Uani 1 1 d . . . C3 C 0.0433(4) 0.4936(2) 0.0530(3) 0.0257(8) Uani 1 1 d . . . C2A C 0.4630(4) 0.5139(2) 0.1657(3) 0.0280(8) Uani 1 1 d . . . H2A H 0.3987 0.5283 0.0984 0.034 Uiso 1 1 calc R . . C6A C 0.4897(4) 0.4565(2) 0.3579(3) 0.0296(8) Uani 1 1 d . . . H6A H 0.4432 0.4324 0.4211 0.036 Uiso 1 1 calc R . . C1B C 0.1574(4) 0.3872(2) 0.3114(3) 0.0249(8) Uani 1 1 d . . . C3A C 0.6303(4) 0.5273(2) 0.1715(3) 0.0330(9) Uani 1 1 d . . . H3A H 0.6775 0.5511 0.1084 0.040 Uiso 1 1 calc R . . C4A C 0.7264(4) 0.5057(2) 0.2698(3) 0.0333(9) Uani 1 1 d . . . H4A H 0.8385 0.5155 0.2737 0.040 Uiso 1 1 calc R . . C5A C 0.6564(4) 0.4693(2) 0.3632(3) 0.0339(9) Uani 1 1 d . . . H5A H 0.7216 0.4536 0.4295 0.041 Uiso 1 1 calc R . . C5B C 0.0384(5) 0.3019(3) 0.4556(4) 0.0475(11) Uani 1 1 d . . . H5B H -0.0094 0.2979 0.5262 0.057 Uiso 1 1 calc R . . C2B C 0.1942(5) 0.3143(2) 0.2518(3) 0.0350(9) Uani 1 1 d . . . H2B H 0.2475 0.3179 0.1834 0.042 Uiso 1 1 calc R . . C6B C 0.0797(4) 0.3799(2) 0.4143(3) 0.0349(9) Uani 1 1 d . . . H6B H 0.0553 0.4276 0.4557 0.042 Uiso 1 1 calc R . . C3B C 0.1524(5) 0.2371(2) 0.2934(4) 0.0455(11) Uani 1 1 d . . . H3B H 0.1811 0.1891 0.2544 0.055 Uiso 1 1 calc R . . C4B C 0.06689(16) 0.23056(7) 0.39403(10) 0.0503(12) Uani 1 1 d . . . H4B H 0.0302 0.1790 0.4186 0.060 Uiso 1 1 calc R . . S1G S 0.65392(16) 0.28740(7) 0.73565(10) 0.0346(6) Uani 0.599(3) 1 d PR . . S3G S 0.66912(16) 0.18618(7) 0.55815(10) 0.0415(9) Uani 0.401(3) 1 d PR . . C5G C 0.51700(16) 0.30939(7) 0.62795(10) 0.0513(12) Uani 1 1 d R . . H5G H 0.395(6) 0.371(3) 0.613(4) 0.062 Uiso 1 1 d . . . C4G C 0.5323(6) 0.2544(3) 0.5340(4) 0.0515(12) Uani 1 1 d . . . H4G H 0.4675 0.2579 0.4640 0.062 Uiso 1 1 calc R . . C2G C 0.7317(6) 0.2089(3) 0.6763(5) 0.0595(14) Uani 1 1 d . . . H2G H 0.8149 0.1782 0.7159 0.071 Uiso 1 1 calc R . . H1 H 0.195(6) 0.587(2) 0.310(4) 0.070(15) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0270(13) 0.0307(14) 0.0266(13) -0.0036(10) 0.0013(10) 0.0041(10) C2 0.0226(17) 0.0286(19) 0.0245(17) 0.0024(14) 0.0000(14) 0.0000(14) C1 0.0208(17) 0.0299(18) 0.0196(16) -0.0014(13) -0.0015(13) 0.0035(13) C1A 0.0233(17) 0.0238(17) 0.0220(16) -0.0027(12) 0.0000(13) 0.0018(13) C3 0.0214(17) 0.0311(18) 0.0244(17) 0.0001(14) 0.0010(13) -0.0002(14) C2A 0.0276(19) 0.0316(19) 0.0245(17) -0.0001(14) 0.0009(14) -0.0013(15) C6A 0.0249(18) 0.038(2) 0.0253(17) 0.0026(15) -0.0006(14) 0.0013(15) C1B 0.0201(16) 0.0309(19) 0.0224(16) 0.0027(14) -0.0069(13) 0.0013(14) C3A 0.030(2) 0.038(2) 0.0321(19) -0.0035(16) 0.0099(16) -0.0043(16) C4A 0.0208(18) 0.044(2) 0.035(2) -0.0073(16) 0.0024(15) 0.0007(16) C5A 0.0238(18) 0.043(2) 0.034(2) -0.0015(16) -0.0054(15) 0.0034(16) C5B 0.048(3) 0.052(3) 0.042(2) 0.017(2) 0.0021(19) -0.010(2) C2B 0.036(2) 0.034(2) 0.035(2) 0.0001(15) 0.0003(16) 0.0036(16) C6B 0.0312(19) 0.041(2) 0.0327(19) 0.0043(16) 0.0003(16) -0.0017(16) C3B 0.050(3) 0.028(2) 0.056(3) 0.0025(18) -0.007(2) -0.0002(18) C4B 0.048(3) 0.038(2) 0.062(3) 0.020(2) -0.009(2) -0.0077(19) S1G 0.0529(11) 0.0267(9) 0.0240(8) 0.0003(6) 0.0024(6) -0.0016(7) S3G 0.0547(17) 0.0339(14) 0.0352(14) -0.0046(10) -0.0008(11) 0.0025(11) C5G 0.056(3) 0.049(3) 0.051(3) 0.007(2) 0.014(2) 0.003(2) C4G 0.054(3) 0.065(3) 0.034(2) -0.003(2) -0.0066(19) -0.008(2) C2G 0.051(3) 0.047(3) 0.078(3) 0.024(2) -0.012(2) -0.005(2) _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 C1 1.446(4) . ? C2 C3 1.201(5) . ? C2 C1 1.484(4) . ? C1 C1B 1.520(5) . ? C1 C1A 1.529(4) . ? C1A C6A 1.385(5) . ? C1A C2A 1.389(5) . ? C3 C3 1.376(6) 3_565 ? C2A C3A 1.386(5) . ? C6A C5A 1.380(5) . ? C1B C6B 1.391(5) . ? C1B C2B 1.399(5) . ? C3A C4A 1.369(5) . ? C4A C5A 1.386(5) . ? C5B C4B 1.374(5) . ? C5B C6B 1.388(5) . ? C2B C3B 1.378(5) . ? C3B C4B 1.402(5) . ? S1G C2G 1.588(6) . ? S1G C5G 1.6421 . ? S3G C2G 1.459(5) . ? S3G C4G 1.575(5) . ? C5G C4G 1.406(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 C2 C1 177.1(3) . . ? O1 C1 C2 108.1(3) . . ? O1 C1 C1B 107.3(2) . . ? C2 C1 C1B 108.9(3) . . ? O1 C1 C1A 109.0(3) . . ? C2 C1 C1A 111.8(3) . . ? C1B C1 C1A 111.6(3) . . ? C6A C1A C2A 118.6(3) . . ? C6A C1A C1 118.6(3) . . ? C2A C1A C1 122.6(3) . . ? C2 C3 C3 179.7(5) . 3_565 ? C3A C2A C1A 120.5(3) . . ? C5A C6A C1A 120.9(3) . . ? C6B C1B C2B 118.6(3) . . ? C6B C1B C1 122.3(3) . . ? C2B C1B C1 119.2(3) . . ? C4A C3A C2A 120.3(3) . . ? C3A C4A C5A 119.8(3) . . ? C6A C5A C4A 119.9(3) . . ? C4B C5B C6B 121.2(4) . . ? C3B C2B C1B 120.6(3) . . ? C5B C6B C1B 120.4(4) . . ? C2B C3B C4B 120.5(3) . . ? C5B C4B C3B 118.6(3) . . ? C2G S1G C5G 96.95(18) . . ? C2G S3G C4G 100.6(3) . . ? C4G C5G S1G 110.2(2) . . ? C5G C4G S3G 113.9(3) . . ? S3G C2G S1G 118.2(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.143 _refine_diff_density_min -0.599 _refine_diff_density_rms 0.078