# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 188 _publ_requested_journal 'Perkin Transactions 2' loop_ _publ_author_name 'Nassimbeni, Luigi R.' 'Barbour, leonard J.' 'Caira, Mino R.' 'le Roex, Tanya' _publ_contact_author_name 'Prof Luigi R Nassimbeni' _publ_contact_author_address ; Department of Chemistry University of Cape Town Rondebosch 7701 SOUTH AFRICA ; _publ_contact_author_email 'XRAYLUIG@SCIENCE.UCT.AC.ZA' _publ_section_title ; Inclusion compounds with mixed guests: controlled stoichiometries and kinetics of enclathration ; data_c: #H _database_code_CSD 175482 _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-9,10-dihydroxy-9,10-bis(p-tert-butylphenyl)-9,10-dihydroanthracene ; _chemical_name_common none _chemical_melting_point 275-277 _chemical_formula_moiety C34 H36 O2 _chemical_formula_sum 'C34 H36 O2' _chemical_formula_weight 476.63 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 monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.6711(3) _cell_length_b 10.6712(2) _cell_length_c 24.3875(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.4350(10) _cell_angle_gamma 90.00 _cell_volume 4252.43(14) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8950 _cell_measurement_theta_min 0.21 _cell_measurement_theta_max 27.10 _exptl_crystal_description 'clear plates' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.121 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1548 _exptl_absorpt_coefficient_mu 0.068 _exptl_absorpt_correction_type none _exptl_special_details ; Data collected at 173K. ; _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 'Nonius Kappa CCD' _diffrn_measurement_method 'Combination of phi and omega' _diffrn_reflns_number 8950 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 27.17 _reflns_number_total 8950 _reflns_number_gt 6522 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 2000)' _computing_cell_refinement 'Collect (Nonius, 2000)' _computing_data_reduction 'Collect (Nonius, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED, a graphical interface to SHELX (1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1116P)^2^+4.2461P] 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_number_reflns 8950 _refine_ls_number_parameters 489 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1049 _refine_ls_R_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.2214 _refine_ls_wR_factor_gt 0.1953 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.429 _refine_ls_shift/su_mean 0.007 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 0.08349(13) 0.48258(18) 0.10122(7) 0.0409(5) Uani 1 1 d . . . H1 H 0.0930 0.5475 0.1209 0.049 Uiso 1 1 calc R . . C1 C 0.07934(16) 0.5142(2) 0.04342(10) 0.0306(5) Uani 1 1 d . . . C2 C 0.01886(16) 0.6211(2) 0.02627(10) 0.0301(5) Uani 1 1 d . . . C3 C 0.03893(18) 0.7394(2) 0.05056(11) 0.0360(6) Uani 1 1 d . . . H3 H 0.0887 0.7494 0.0770 0.043 Uiso 1 1 calc R . . C4 C -0.01207(19) 0.8411(3) 0.03685(12) 0.0406(7) Uani 1 1 d . . . H4 H 0.0023 0.9201 0.0539 0.049 Uiso 1 1 calc R . . C5 C -0.08436(19) 0.8272(3) -0.00191(12) 0.0407(7) Uani 1 1 d . . . H5 H -0.1196 0.8970 -0.0118 0.049 Uiso 1 1 calc R . . C6 C -0.10521(18) 0.7118(3) -0.02608(11) 0.0377(6) Uani 1 1 d . . . H6 H -0.1552 0.7029 -0.0524 0.045 Uiso 1 1 calc R . . C7 C -0.05395(16) 0.6077(2) -0.01256(10) 0.0312(5) Uani 1 1 d . . . C11 C 0.16300(16) 0.5573(2) 0.03315(10) 0.0318(5) Uani 1 1 d . . . C12 C 0.17081(15) 0.5904(2) -0.02052(10) 0.0304(5) Uani 1 1 d . . . H12 H 0.1262 0.5769 -0.0508 0.036 Uiso 1 1 calc R . . C13 C 0.24220(16) 0.6425(3) -0.03077(11) 0.0354(6) Uani 1 1 d . . . H13 H 0.2450 0.6663 -0.0679 0.042 Uiso 1 1 calc R . . C14 C 0.31003(17) 0.6610(3) 0.01178(13) 0.0455(7) Uani 1 1 d . . . C15 C 0.3024(2) 0.6226(4) 0.06480(14) 0.0655(10) Uani 1 1 d . . . H15 H 0.3480 0.6308 0.0948 0.079 Uiso 1 1 calc R . . C16 C 0.2305(2) 0.5730(4) 0.07539(12) 0.0574(9) Uani 1 1 d . . . H16 H 0.2276 0.5492 0.1125 0.069 Uiso 1 1 calc R . . C17 C 0.3875(2) 0.7234(4) -0.00065(17) 0.0680(11) Uani 1 1 d . . . C18 C 0.4176(3) 0.6507(7) -0.0462(2) 0.113(2) Uani 1 1 d . . . H18A H 0.4231 0.5619 -0.0359 0.169 Uiso 1 1 calc R . . H18B H 0.4708 0.6837 -0.0506 0.169 Uiso 1 1 calc R . . H18C H 0.3781 0.6596 -0.0816 0.169 Uiso 1 1 calc R . . C19 C 0.3660(4) 0.8550(6) -0.0203(5) 0.180(4) Uani 1 1 d . . . H19A H 0.3173 0.8536 -0.0503 0.270 Uiso 1 1 calc R . . H19B H 0.4119 0.8919 -0.0343 0.270 Uiso 1 1 calc R . . H19C H 0.3548 0.9052 0.0110 0.270 Uiso 1 1 calc R . . C20 C 0.4562(3) 0.7246(8) 0.0485(2) 0.124(2) Uani 1 1 d . . . H20A H 0.4400 0.7718 0.0790 0.186 Uiso 1 1 calc R . . H20B H 0.5040 0.7646 0.0381 0.186 Uiso 1 1 calc R . . H20C H 0.4699 0.6384 0.0607 0.186 Uiso 1 1 calc R . . O21 O 0.12736(10) 0.61680(15) 0.20214(7) 0.0280(4) Uani 1 1 d . . . H21 H 0.0867 0.5890 0.2139 0.034 Uiso 1 1 calc R . . C21 C 0.17184(13) 0.7035(2) 0.24257(9) 0.0232(5) Uani 1 1 d . . . C22 C 0.13706(13) 0.6999(2) 0.29598(9) 0.0227(5) Uani 1 1 d . . . C23 C 0.16165(14) 0.6038(2) 0.33465(10) 0.0270(5) Uani 1 1 d . . . H23 H 0.2005 0.5439 0.3276 0.032 Uiso 1 1 calc R . . C24 C 0.13042(15) 0.5947(2) 0.38288(10) 0.0307(5) Uani 1 1 d . . . H24 H 0.1465 0.5274 0.4082 0.037 Uiso 1 1 calc R . . C25 C 0.07548(15) 0.6840(2) 0.39428(10) 0.0303(5) Uani 1 1 d . . . H25 H 0.0553 0.6796 0.4280 0.036 Uiso 1 1 calc R . . C26 C 0.05017(14) 0.7797(2) 0.35633(10) 0.0271(5) Uani 1 1 d . . . H26 H 0.0125 0.8406 0.3642 0.032 Uiso 1 1 calc R . . C27 C 0.07964(13) 0.7874(2) 0.30635(9) 0.0228(5) Uani 1 1 d . . . O28 O 0.02118(10) 0.99650(15) 0.28939(7) 0.0288(4) Uani 1 1 d . . . H28 H 0.0636 1.0367 0.3035 0.035 Uiso 1 1 calc R . . C28 C 0.04379(13) 0.8847(2) 0.26258(9) 0.0232(5) Uani 1 1 d . . . C29 C 0.10232(13) 0.9170(2) 0.22413(10) 0.0241(5) Uani 1 1 d . . . C30 C 0.09146(15) 1.0297(2) 0.19484(11) 0.0309(5) Uani 1 1 d . . . H30 H 0.0505 1.0867 0.2012 0.037 Uiso 1 1 calc R . . C31 C 0.13951(17) 1.0596(3) 0.15672(12) 0.0390(6) Uani 1 1 d . . . H31 H 0.1319 1.1370 0.1372 0.047 Uiso 1 1 calc R . . C32 C 0.19878(17) 0.9763(3) 0.14700(12) 0.0384(6) Uani 1 1 d . . . H32 H 0.2314 0.9959 0.1203 0.046 Uiso 1 1 calc R . . C33 C 0.21050(15) 0.8644(2) 0.17612(11) 0.0317(5) Uani 1 1 d . . . H33 H 0.2518 0.8082 0.1697 0.038 Uiso 1 1 calc R . . C34 C 0.16228(13) 0.8330(2) 0.21502(9) 0.0240(5) Uani 1 1 d . . . C35 C 0.26215(14) 0.6664(2) 0.25563(10) 0.0264(5) Uani 1 1 d . . . C36 C 0.29153(16) 0.5599(2) 0.23360(11) 0.0339(6) Uani 1 1 d . . . H36 H 0.2550 0.5067 0.2092 0.041 Uiso 1 1 calc R . . C37 C 0.37469(18) 0.5308(3) 0.24717(13) 0.0448(7) Uani 1 1 d . . . H37 H 0.3935 0.4577 0.2314 0.054 Uiso 1 1 calc R . . C38 C 0.43145(16) 0.6045(3) 0.28291(14) 0.0468(7) Uani 1 1 d D . . C39 C 0.40019(17) 0.7108(3) 0.30454(14) 0.0461(7) Uani 1 1 d . . . H39 H 0.4364 0.7640 0.3292 0.055 Uiso 1 1 calc R . . C40 C 0.31782(15) 0.7411(3) 0.29112(13) 0.0377(6) Uani 1 1 d . . . H40 H 0.2990 0.8146 0.3065 0.045 Uiso 1 1 calc R . . C41 C 0.52142(19) 0.5695(3) 0.29793(18) 0.0683(11) Uani 1 1 d D . . C42 C 0.5297(5) 0.4381(7) 0.3223(4) 0.0970(13) Uiso 0.603(5) 1 d PD . . C43 C 0.5738(5) 0.6687(8) 0.3277(4) 0.0970(13) Uiso 0.603(5) 1 d PD . . C44 C 0.5489(5) 0.5482(9) 0.2404(3) 0.0970(13) Uiso 0.603(5) 1 d PD . . C48 C -0.03745(13) 0.8347(2) 0.22873(9) 0.0233(5) Uani 1 1 d . . . C49 C -0.10641(14) 0.8289(2) 0.25302(10) 0.0269(5) Uani 1 1 d . . . H49 H -0.1025 0.8540 0.2908 0.032 Uiso 1 1 calc R . . C50 C -0.18010(15) 0.7872(2) 0.22261(11) 0.0301(5) Uani 1 1 d . . . H50 H -0.2261 0.7840 0.2401 0.036 Uiso 1 1 calc R . . C51 C -0.18949(14) 0.7495(2) 0.16682(11) 0.0298(5) Uani 1 1 d . . . C52 C -0.11992(15) 0.7522(2) 0.14348(10) 0.0291(5) Uani 1 1 d . . . H52 H -0.1234 0.7248 0.1060 0.035 Uiso 1 1 calc R . . C53 C -0.04536(14) 0.7942(2) 0.17385(10) 0.0269(5) Uani 1 1 d . . . H53 H 0.0011 0.7951 0.1567 0.032 Uiso 1 1 calc R . . C54 C -0.27301(16) 0.7063(3) 0.13455(13) 0.0430(7) Uani 1 1 d . . . C55 C -0.2761(2) 0.6999(4) 0.07146(14) 0.0556(8) Uani 1 1 d . . . H55A H -0.2662 0.7835 0.0575 0.083 Uiso 1 1 calc R . . H55B H -0.3301 0.6701 0.0525 0.083 Uiso 1 1 calc R . . H55C H -0.2339 0.6420 0.0640 0.083 Uiso 1 1 calc R . . C56 C -0.3400(2) 0.7950(5) 0.14527(19) 0.0775(13) Uani 1 1 d . . . H56A H -0.3386 0.8001 0.1856 0.116 Uiso 1 1 calc R . . H56B H -0.3935 0.7635 0.1262 0.116 Uiso 1 1 calc R . . H56C H -0.3309 0.8785 0.1309 0.116 Uiso 1 1 calc R . . C57 C -0.2877(3) 0.5729(4) 0.15548(18) 0.0756(12) Uani 1 1 d . . . H57A H -0.2446 0.5167 0.1482 0.113 Uiso 1 1 calc R . . H57B H -0.3411 0.5422 0.1357 0.113 Uiso 1 1 calc R . . H57C H -0.2869 0.5755 0.1958 0.113 Uiso 1 1 calc R . . C45 C 0.5417(7) 0.5584(13) 0.3636(3) 0.0970(13) Uiso 0.397(5) 1 d PD . . C46 C 0.5752(6) 0.6762(11) 0.2906(7) 0.0970(13) Uiso 0.397(5) 1 d PD . . C47 C 0.5407(7) 0.4405(9) 0.2850(6) 0.0970(13) Uiso 0.397(5) 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 0.0667(13) 0.0378(10) 0.0209(9) -0.0014(7) 0.0152(9) -0.0102(9) C1 0.0398(14) 0.0344(13) 0.0192(11) 0.0001(9) 0.0097(10) -0.0056(11) C2 0.0359(13) 0.0337(13) 0.0241(11) -0.0019(10) 0.0146(10) -0.0060(10) C3 0.0429(15) 0.0370(14) 0.0311(13) -0.0069(11) 0.0149(11) -0.0092(12) C4 0.0562(18) 0.0326(14) 0.0386(15) -0.0065(11) 0.0226(13) -0.0064(12) C5 0.0550(18) 0.0344(14) 0.0369(15) 0.0016(11) 0.0195(13) 0.0040(12) C6 0.0435(15) 0.0402(15) 0.0315(13) 0.0007(11) 0.0128(12) 0.0001(12) C7 0.0391(14) 0.0343(13) 0.0235(11) -0.0002(10) 0.0143(10) -0.0049(11) C11 0.0346(13) 0.0346(13) 0.0254(12) -0.0006(10) 0.0042(10) -0.0021(11) C12 0.0284(12) 0.0355(13) 0.0260(12) 0.0017(10) 0.0024(10) -0.0021(10) C13 0.0326(13) 0.0420(15) 0.0320(13) 0.0007(11) 0.0075(11) -0.0011(11) C14 0.0323(14) 0.0593(19) 0.0444(16) -0.0128(14) 0.0061(12) -0.0100(13) C15 0.0400(17) 0.111(3) 0.0391(17) -0.0069(18) -0.0070(14) -0.0167(19) C16 0.0462(18) 0.096(3) 0.0266(14) 0.0035(15) -0.0014(13) -0.0119(17) C17 0.0382(18) 0.095(3) 0.072(2) -0.019(2) 0.0149(17) -0.0269(18) C18 0.062(3) 0.192(6) 0.093(3) -0.046(4) 0.037(3) -0.052(3) C19 0.085(4) 0.104(5) 0.355(13) 0.052(6) 0.057(6) -0.044(4) C20 0.055(3) 0.216(7) 0.098(4) -0.048(4) 0.010(3) -0.055(4) O21 0.0304(9) 0.0306(9) 0.0243(8) -0.0053(7) 0.0089(7) -0.0075(7) C21 0.0215(11) 0.0242(11) 0.0239(11) -0.0010(9) 0.0043(9) 0.0003(9) C22 0.0212(11) 0.0225(11) 0.0243(11) -0.0029(9) 0.0045(9) -0.0022(8) C23 0.0263(12) 0.0268(12) 0.0278(12) 0.0005(9) 0.0054(9) 0.0023(9) C24 0.0347(13) 0.0300(13) 0.0263(12) 0.0035(10) 0.0036(10) -0.0008(10) C25 0.0337(13) 0.0365(13) 0.0213(11) -0.0030(10) 0.0072(10) -0.0043(10) C26 0.0254(11) 0.0314(12) 0.0248(11) -0.0044(9) 0.0059(9) 0.0007(9) C27 0.0214(11) 0.0243(11) 0.0218(11) -0.0032(9) 0.0021(8) -0.0027(9) O28 0.0249(8) 0.0243(8) 0.0370(9) -0.0082(7) 0.0055(7) 0.0020(6) C28 0.0226(11) 0.0215(11) 0.0260(11) -0.0038(9) 0.0064(9) 0.0018(9) C29 0.0204(10) 0.0241(11) 0.0265(11) 0.0011(9) 0.0015(9) -0.0015(9) C30 0.0302(12) 0.0261(12) 0.0357(13) 0.0044(10) 0.0043(10) 0.0003(10) C31 0.0422(15) 0.0324(14) 0.0420(15) 0.0136(11) 0.0072(12) -0.0018(11) C32 0.0351(14) 0.0436(15) 0.0387(14) 0.0112(12) 0.0128(11) -0.0054(12) C33 0.0247(12) 0.0368(13) 0.0352(13) 0.0045(11) 0.0098(10) 0.0001(10) C34 0.0204(11) 0.0261(12) 0.0247(11) 0.0007(9) 0.0027(9) -0.0025(9) C35 0.0232(11) 0.0283(12) 0.0294(12) 0.0048(9) 0.0093(9) 0.0045(9) C36 0.0366(14) 0.0329(13) 0.0351(13) 0.0021(11) 0.0142(11) 0.0085(11) C37 0.0413(16) 0.0406(15) 0.0588(18) 0.0104(13) 0.0250(14) 0.0186(13) C38 0.0309(14) 0.0454(17) 0.068(2) 0.0177(15) 0.0183(14) 0.0103(12) C39 0.0255(13) 0.0470(17) 0.064(2) 0.0006(14) 0.0056(13) -0.0009(12) C40 0.0247(12) 0.0367(14) 0.0510(16) -0.0046(12) 0.0059(11) 0.0029(11) C41 0.0318(16) 0.060(2) 0.118(3) 0.033(2) 0.0253(19) 0.0189(15) C48 0.0223(11) 0.0193(11) 0.0277(11) 0.0011(9) 0.0032(9) 0.0031(8) C49 0.0270(12) 0.0275(12) 0.0268(12) -0.0014(9) 0.0069(9) 0.0009(9) C50 0.0227(11) 0.0315(13) 0.0373(13) -0.0024(10) 0.0089(10) -0.0005(9) C51 0.0251(12) 0.0255(12) 0.0378(14) -0.0025(10) 0.0038(10) -0.0009(9) C52 0.0279(12) 0.0308(13) 0.0277(12) -0.0033(10) 0.0033(10) 0.0007(10) C53 0.0238(11) 0.0294(12) 0.0279(12) -0.0019(9) 0.0059(9) -0.0001(9) C54 0.0275(13) 0.0495(17) 0.0501(17) -0.0147(13) 0.0028(12) -0.0077(12) C55 0.0391(16) 0.075(2) 0.0461(18) -0.0111(16) -0.0075(14) -0.0068(15) C56 0.0277(16) 0.113(3) 0.084(3) -0.046(3) -0.0081(16) 0.0073(18) C57 0.075(3) 0.074(3) 0.073(3) -0.004(2) 0.003(2) -0.043(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 1.438(3) . ? C1 C7 1.520(3) 3_565 ? C1 C2 1.526(4) . ? C1 C11 1.536(4) . ? C2 C7 1.391(4) . ? C2 C3 1.406(4) . ? C3 C4 1.378(4) . ? C4 C5 1.384(4) . ? C5 C6 1.379(4) . ? C6 C7 1.401(4) . ? C7 C1 1.520(3) 3_565 ? C11 C16 1.377(4) . ? C11 C12 1.386(3) . ? C12 C13 1.381(4) . ? C13 C14 1.389(4) . ? C14 C15 1.386(5) . ? C14 C17 1.535(4) . ? C15 C16 1.380(5) . ? C17 C20 1.485(6) . ? C17 C19 1.503(8) . ? C17 C18 1.520(6) . ? O21 C21 1.445(3) . ? C21 C22 1.528(3) . ? C21 C35 1.528(3) . ? C21 C34 1.531(3) . ? C22 C27 1.396(3) . ? C22 C23 1.398(3) . ? C23 C24 1.381(3) . ? C24 C25 1.388(4) . ? C25 C26 1.386(3) . ? C26 C27 1.404(3) . ? C27 C28 1.524(3) . ? O28 C28 1.446(3) . ? C28 C29 1.521(3) . ? C28 C48 1.535(3) . ? C29 C30 1.392(3) . ? C29 C34 1.393(3) . ? C30 C31 1.379(4) . ? C31 C32 1.384(4) . ? C32 C33 1.383(4) . ? C33 C34 1.400(3) . ? C35 C36 1.387(3) . ? C35 C40 1.388(4) . ? C36 C37 1.395(4) . ? C37 C38 1.395(5) . ? C38 C39 1.395(4) . ? C38 C41 1.518(4) . ? C39 C40 1.385(4) . ? C41 C47 1.462(8) . ? C41 C43 1.469(7) . ? C41 C46 1.483(8) . ? C41 C42 1.518(7) . ? C41 C45 1.574(8) . ? C41 C44 1.576(7) . ? C42 C47 0.964(14) . ? C42 C45 1.619(15) . ? C43 C46 0.914(14) . ? C43 C45 1.620(16) . ? C44 C47 1.606(16) . ? C44 C46 1.829(16) . ? C48 C53 1.388(3) . ? C48 C49 1.395(3) . ? C49 C50 1.377(3) . ? C50 C51 1.398(4) . ? C51 C52 1.390(3) . ? C51 C54 1.529(3) . ? C52 C53 1.389(3) . ? C54 C56 1.526(5) . ? C54 C55 1.531(5) . ? C54 C57 1.547(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 O1 C1 C7 103.86(19) . 3_565 ? O1 C1 C2 110.18(19) . . ? C7 C1 C2 113.6(2) 3_565 . ? O1 C1 C11 111.2(2) . . ? C7 C1 C11 110.4(2) 3_565 . ? C2 C1 C11 107.7(2) . . ? C7 C2 C3 118.8(2) . . ? C7 C2 C1 123.3(2) . . ? C3 C2 C1 117.8(2) . . ? C4 C3 C2 121.4(3) . . ? C3 C4 C5 119.6(3) . . ? C6 C5 C4 119.9(3) . . ? C5 C6 C7 121.1(3) . . ? C2 C7 C6 119.2(2) . . ? C2 C7 C1 123.0(2) . 3_565 ? C6 C7 C1 117.7(2) . 3_565 ? C16 C11 C12 117.4(2) . . ? C16 C11 C1 123.3(2) . . ? C12 C11 C1 119.2(2) . . ? C13 C12 C11 121.3(2) . . ? C12 C13 C14 121.7(3) . . ? C15 C14 C13 116.3(3) . . ? C15 C14 C17 123.3(3) . . ? C13 C14 C17 120.4(3) . . ? C16 C15 C14 122.1(3) . . ? C11 C16 C15 121.2(3) . . ? C20 C17 C19 110.2(5) . . ? C20 C17 C18 106.3(4) . . ? C19 C17 C18 109.6(6) . . ? C20 C17 C14 112.9(4) . . ? C19 C17 C14 108.2(4) . . ? C18 C17 C14 109.6(3) . . ? O21 C21 C22 109.60(17) . . ? O21 C21 C35 109.12(18) . . ? C22 C21 C35 109.91(18) . . ? O21 C21 C34 106.48(17) . . ? C22 C21 C34 111.88(18) . . ? C35 C21 C34 109.76(18) . . ? C27 C22 C23 119.2(2) . . ? C27 C22 C21 121.8(2) . . ? C23 C22 C21 118.91(19) . . ? C24 C23 C22 121.1(2) . . ? C23 C24 C25 119.8(2) . . ? C26 C25 C24 119.8(2) . . ? C25 C26 C27 120.7(2) . . ? C22 C27 C26 119.2(2) . . ? C22 C27 C28 121.11(19) . . ? C26 C27 C28 119.5(2) . . ? O28 C28 C29 110.40(18) . . ? O28 C28 C27 110.28(18) . . ? C29 C28 C27 112.08(18) . . ? O28 C28 C48 104.38(17) . . ? C29 C28 C48 110.66(18) . . ? C27 C28 C48 108.77(18) . . ? C30 C29 C34 119.9(2) . . ? C30 C29 C28 118.6(2) . . ? C34 C29 C28 121.4(2) . . ? C31 C30 C29 120.8(2) . . ? C30 C31 C32 119.8(2) . . ? C33 C32 C31 120.0(2) . . ? C32 C33 C34 120.9(2) . . ? C29 C34 C33 118.7(2) . . ? C29 C34 C21 121.8(2) . . ? C33 C34 C21 119.3(2) . . ? C36 C35 C40 117.9(2) . . ? C36 C35 C21 122.7(2) . . ? C40 C35 C21 119.4(2) . . ? C35 C36 C37 120.1(3) . . ? C38 C37 C36 122.8(3) . . ? C37 C38 C39 115.9(2) . . ? C37 C38 C41 121.8(3) . . ? C39 C38 C41 122.3(3) . . ? C40 C39 C38 121.8(3) . . ? C39 C40 C35 121.5(3) . . ? C47 C41 C43 130.5(6) . . ? C47 C41 C46 122.2(8) . . ? C43 C41 C46 36.1(6) . . ? C47 C41 C42 37.7(6) . . ? C43 C41 C42 118.2(6) . . ? C46 C41 C42 138.3(6) . . ? C47 C41 C38 115.4(5) . . ? C43 C41 C38 113.8(4) . . ? C46 C41 C38 111.9(5) . . ? C42 C41 C38 109.3(4) . . ? C47 C41 C45 97.9(8) . . ? C43 C41 C45 64.2(7) . . ? C46 C41 C45 99.7(8) . . ? C42 C41 C45 63.1(6) . . ? C38 C41 C45 105.5(5) . . ? C47 C41 C44 63.7(7) . . ? C43 C41 C44 107.1(6) . . ? C46 C41 C44 73.4(7) . . ? C42 C41 C44 101.3(6) . . ? C38 C41 C44 105.5(4) . . ? C45 C41 C44 148.5(6) . . ? C47 C42 C41 68.0(6) . . ? C47 C42 C45 122.9(10) . . ? C41 C42 C45 60.2(4) . . ? C46 C43 C41 72.8(7) . . ? C46 C43 C45 132.5(10) . . ? C41 C43 C45 61.0(5) . . ? C47 C44 C41 54.7(4) . . ? C47 C44 C46 97.1(7) . . ? C41 C44 C46 51.0(4) . . ? C53 C48 C49 117.8(2) . . ? C53 C48 C28 122.1(2) . . ? C49 C48 C28 120.0(2) . . ? C50 C49 C48 120.5(2) . . ? C49 C50 C51 122.2(2) . . ? C52 C51 C50 116.8(2) . . ? C52 C51 C54 123.0(2) . . ? C50 C51 C54 120.2(2) . . ? C51 C52 C53 121.3(2) . . ? C48 C53 C52 121.3(2) . . ? C56 C54 C51 110.3(2) . . ? C56 C54 C55 108.7(3) . . ? C51 C54 C55 112.1(2) . . ? C56 C54 C57 110.2(3) . . ? C51 C54 C57 107.2(3) . . ? C55 C54 C57 108.4(3) . . ? C41 C45 C42 56.7(4) . . ? C41 C45 C43 54.8(4) . . ? C42 C45 C43 104.7(7) . . ? C43 C46 C41 71.2(7) . . ? C43 C46 C44 123.2(10) . . ? C41 C46 C44 55.7(5) . . ? C42 C47 C41 74.3(7) . . ? C42 C47 C44 135.7(9) . . ? C41 C47 C44 61.6(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C7 -114.0(2) . . . . ? C7 C1 C2 C7 2.0(3) 3_565 . . . ? C11 C1 C2 C7 124.6(2) . . . . ? O1 C1 C2 C3 66.9(3) . . . . ? C7 C1 C2 C3 -177.0(2) 3_565 . . . ? C11 C1 C2 C3 -54.5(3) . . . . ? C7 C2 C3 C4 0.3(4) . . . . ? C1 C2 C3 C4 179.3(2) . . . . ? C2 C3 C4 C5 -0.4(4) . . . . ? C3 C4 C5 C6 0.6(4) . . . . ? C4 C5 C6 C7 -0.6(4) . . . . ? C3 C2 C7 C6 -0.3(3) . . . . ? C1 C2 C7 C6 -179.3(2) . . . . ? C3 C2 C7 C1 176.8(2) . . . 3_565 ? C1 C2 C7 C1 -2.2(4) . . . 3_565 ? C5 C6 C7 C2 0.5(4) . . . . ? C5 C6 C7 C1 -176.8(2) . . . 3_565 ? O1 C1 C11 C16 -5.1(4) . . . . ? C7 C1 C11 C16 -119.8(3) 3_565 . . . ? C2 C1 C11 C16 115.7(3) . . . . ? O1 C1 C11 C12 179.3(2) . . . . ? C7 C1 C11 C12 64.6(3) 3_565 . . . ? C2 C1 C11 C12 -59.9(3) . . . . ? C16 C11 C12 C13 -3.0(4) . . . . ? C1 C11 C12 C13 172.9(2) . . . . ? C11 C12 C13 C14 1.8(4) . . . . ? C12 C13 C14 C15 0.9(5) . . . . ? C12 C13 C14 C17 -177.8(3) . . . . ? C13 C14 C15 C16 -2.3(6) . . . . ? C17 C14 C15 C16 176.4(4) . . . . ? C12 C11 C16 C15 1.6(5) . . . . ? C1 C11 C16 C15 -174.1(3) . . . . ? C14 C15 C16 C11 1.1(6) . . . . ? C15 C14 C17 C20 6.7(6) . . . . ? C13 C14 C17 C20 -174.6(4) . . . . ? C15 C14 C17 C19 -115.5(6) . . . . ? C13 C14 C17 C19 63.2(6) . . . . ? C15 C14 C17 C18 125.0(5) . . . . ? C13 C14 C17 C18 -56.3(5) . . . . ? O21 C21 C22 C27 -97.0(2) . . . . ? C35 C21 C22 C27 143.1(2) . . . . ? C34 C21 C22 C27 20.9(3) . . . . ? O21 C21 C22 C23 81.0(2) . . . . ? C35 C21 C22 C23 -38.9(3) . . . . ? C34 C21 C22 C23 -161.1(2) . . . . ? C27 C22 C23 C24 -0.3(3) . . . . ? C21 C22 C23 C24 -178.4(2) . . . . ? C22 C23 C24 C25 -1.9(4) . . . . ? C23 C24 C25 C26 2.1(4) . . . . ? C24 C25 C26 C27 -0.1(4) . . . . ? C23 C22 C27 C26 2.3(3) . . . . ? C21 C22 C27 C26 -179.7(2) . . . . ? C23 C22 C27 C28 -173.0(2) . . . . ? C21 C22 C27 C28 5.0(3) . . . . ? C25 C26 C27 C22 -2.1(3) . . . . ? C25 C26 C27 C28 173.3(2) . . . . ? C22 C27 C28 O28 -151.3(2) . . . . ? C26 C27 C28 O28 33.4(3) . . . . ? C22 C27 C28 C29 -27.9(3) . . . . ? C26 C27 C28 C29 156.8(2) . . . . ? C22 C27 C28 C48 94.8(2) . . . . ? C26 C27 C28 C48 -80.5(2) . . . . ? O28 C28 C29 C30 -36.0(3) . . . . ? C27 C28 C29 C30 -159.3(2) . . . . ? C48 C28 C29 C30 79.1(3) . . . . ? O28 C28 C29 C34 148.4(2) . . . . ? C27 C28 C29 C34 25.0(3) . . . . ? C48 C28 C29 C34 -96.6(2) . . . . ? C34 C29 C30 C31 0.0(4) . . . . ? C28 C29 C30 C31 -175.7(2) . . . . ? C29 C30 C31 C32 0.6(4) . . . . ? C30 C31 C32 C33 -1.0(4) . . . . ? C31 C32 C33 C34 0.9(4) . . . . ? C30 C29 C34 C33 -0.1(3) . . . . ? C28 C29 C34 C33 175.5(2) . . . . ? C30 C29 C34 C21 -174.9(2) . . . . ? C28 C29 C34 C21 0.7(3) . . . . ? C32 C33 C34 C29 -0.4(4) . . . . ? C32 C33 C34 C21 174.6(2) . . . . ? O21 C21 C34 C29 95.9(2) . . . . ? C22 C21 C34 C29 -23.8(3) . . . . ? C35 C21 C34 C29 -146.1(2) . . . . ? O21 C21 C34 C33 -78.8(2) . . . . ? C22 C21 C34 C33 161.4(2) . . . . ? C35 C21 C34 C33 39.1(3) . . . . ? O21 C21 C35 C36 -4.1(3) . . . . ? C22 C21 C35 C36 116.1(2) . . . . ? C34 C21 C35 C36 -120.4(2) . . . . ? O21 C21 C35 C40 176.2(2) . . . . ? C22 C21 C35 C40 -63.6(3) . . . . ? C34 C21 C35 C40 59.8(3) . . . . ? C40 C35 C36 C37 -0.1(4) . . . . ? C21 C35 C36 C37 -179.9(2) . . . . ? C35 C36 C37 C38 0.4(4) . . . . ? C36 C37 C38 C39 -0.2(4) . . . . ? C36 C37 C38 C41 178.8(3) . . . . ? C37 C38 C39 C40 -0.1(5) . . . . ? C41 C38 C39 C40 -179.2(3) . . . . ? C38 C39 C40 C35 0.4(5) . . . . ? C36 C35 C40 C39 -0.2(4) . . . . ? C21 C35 C40 C39 179.5(3) . . . . ? C37 C38 C41 C47 -15.3(8) . . . . ? C39 C38 C41 C47 163.7(7) . . . . ? C37 C38 C41 C43 169.7(5) . . . . ? C39 C38 C41 C43 -11.3(6) . . . . ? C37 C38 C41 C46 130.5(7) . . . . ? C39 C38 C41 C46 -50.5(8) . . . . ? C37 C38 C41 C42 -55.7(6) . . . . ? C39 C38 C41 C42 123.3(5) . . . . ? C37 C38 C41 C45 -122.1(6) . . . . ? C39 C38 C41 C45 56.9(6) . . . . ? C37 C38 C41 C44 52.6(5) . . . . ? C39 C38 C41 C44 -128.5(5) . . . . ? C43 C41 C42 C47 -120.8(10) . . . . ? C46 C41 C42 C47 -81.8(15) . . . . ? C38 C41 C42 C47 106.8(10) . . . . ? C45 C41 C42 C47 -155.2(11) . . . . ? C44 C41 C42 C47 -4.2(10) . . . . ? C47 C41 C42 C45 155.2(11) . . . . ? C43 C41 C42 C45 34.3(8) . . . . ? C46 C41 C42 C45 73.3(13) . . . . ? C38 C41 C42 C45 -98.0(6) . . . . ? C44 C41 C42 C45 150.9(6) . . . . ? C47 C41 C43 C46 90.9(14) . . . . ? C42 C41 C43 C46 134.6(11) . . . . ? C38 C41 C43 C46 -95.0(10) . . . . ? C45 C41 C43 C46 168.6(12) . . . . ? C44 C41 C43 C46 21.2(11) . . . . ? C47 C41 C43 C45 -77.7(11) . . . . ? C46 C41 C43 C45 -168.6(12) . . . . ? C42 C41 C43 C45 -34.0(7) . . . . ? C38 C41 C43 C45 96.3(6) . . . . ? C44 C41 C43 C45 -147.4(6) . . . . ? C43 C41 C44 C47 127.3(7) . . . . ? C46 C41 C44 C47 140.2(8) . . . . ? C42 C41 C44 C47 2.9(7) . . . . ? C38 C41 C44 C47 -111.1(6) . . . . ? C45 C41 C44 C47 59.0(14) . . . . ? C47 C41 C44 C46 -140.2(8) . . . . ? C43 C41 C44 C46 -12.8(7) . . . . ? C42 C41 C44 C46 -137.3(7) . . . . ? C38 C41 C44 C46 108.8(6) . . . . ? C45 C41 C44 C46 -81.2(13) . . . . ? O28 C28 C48 C53 134.8(2) . . . . ? C29 C28 C48 C53 16.0(3) . . . . ? C27 C28 C48 C53 -107.5(2) . . . . ? O28 C28 C48 C49 -45.2(3) . . . . ? C29 C28 C48 C49 -164.0(2) . . . . ? C27 C28 C48 C49 72.5(2) . . . . ? C53 C48 C49 C50 -1.7(3) . . . . ? C28 C48 C49 C50 178.4(2) . . . . ? C48 C49 C50 C51 -0.1(4) . . . . ? C49 C50 C51 C52 1.9(4) . . . . ? C49 C50 C51 C54 -178.8(2) . . . . ? C50 C51 C52 C53 -1.9(4) . . . . ? C54 C51 C52 C53 178.9(2) . . . . ? C49 C48 C53 C52 1.7(3) . . . . ? C28 C48 C53 C52 -178.4(2) . . . . ? C51 C52 C53 C48 0.1(4) . . . . ? C52 C51 C54 C56 -136.1(3) . . . . ? C50 C51 C54 C56 44.7(4) . . . . ? C52 C51 C54 C55 -14.8(4) . . . . ? C50 C51 C54 C55 166.0(3) . . . . ? C52 C51 C54 C57 103.9(3) . . . . ? C50 C51 C54 C57 -75.2(3) . . . . ? C47 C41 C45 C42 -15.0(7) . . . . ? C43 C41 C45 C42 -146.5(7) . . . . ? C46 C41 C45 C42 -139.7(7) . . . . ? C38 C41 C45 C42 104.2(5) . . . . ? C44 C41 C45 C42 -65.9(13) . . . . ? C47 C41 C45 C43 131.5(7) . . . . ? C46 C41 C45 C43 6.8(7) . . . . ? C42 C41 C45 C43 146.5(7) . . . . ? C38 C41 C45 C43 -109.4(5) . . . . ? C44 C41 C45 C43 80.6(13) . . . . ? C47 C42 C45 C41 27.7(11) . . . . ? C47 C42 C45 C43 -0.1(14) . . . . ? C41 C42 C45 C43 -27.8(5) . . . . ? C46 C43 C45 C41 -14.8(14) . . . . ? C46 C43 C45 C42 13.7(18) . . . . ? C41 C43 C45 C42 28.5(5) . . . . ? C45 C43 C46 C41 13.6(13) . . . . ? C41 C43 C46 C44 -20.9(9) . . . . ? C45 C43 C46 C44 -7(2) . . . . ? C47 C41 C46 C43 -116.1(12) . . . . ? C42 C41 C46 C43 -70.5(15) . . . . ? C38 C41 C46 C43 100.7(10) . . . . ? C45 C41 C46 C43 -10.4(11) . . . . ? C44 C41 C46 C43 -158.8(11) . . . . ? C47 C41 C46 C44 42.7(9) . . . . ? C43 C41 C46 C44 158.8(11) . . . . ? C42 C41 C46 C44 88.4(11) . . . . ? C38 C41 C46 C44 -100.4(5) . . . . ? C45 C41 C46 C44 148.5(6) . . . . ? C47 C44 C46 C43 -7.7(14) . . . . ? C41 C44 C46 C43 24.1(11) . . . . ? C47 C44 C46 C41 -31.8(6) . . . . ? C45 C42 C47 C41 -25.7(10) . . . . ? C41 C42 C47 C44 5.8(14) . . . . ? C45 C42 C47 C44 -20(2) . . . . ? C43 C41 C47 C42 84.8(12) . . . . ? C46 C41 C47 C42 128.9(11) . . . . ? C38 C41 C47 C42 -89.1(10) . . . . ? C45 C41 C47 C42 22.2(10) . . . . ? C44 C41 C47 C42 175.4(11) . . . . ? C43 C41 C47 C44 -90.5(9) . . . . ? C46 C41 C47 C44 -46.5(10) . . . . ? C42 C41 C47 C44 -175.4(11) . . . . ? C38 C41 C47 C44 95.5(6) . . . . ? C45 C41 C47 C44 -153.2(6) . . . . ? C41 C44 C47 C42 -6.4(15) . . . . ? C46 C44 C47 C42 23.7(18) . . . . ? C46 C44 C47 C41 30.1(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O21 0.84 2.09 2.816(2) 145.1 . _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 27.17 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 0.809 _refine_diff_density_min -0.570 _refine_diff_density_rms 0.061 #========================================================END data_c:_H.4A _database_code_CSD 175483 _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-9,10-dihydroxy-9,10-bis(p-tert-butylphenyl)-9,10-dihydroanthracene. 4(N,N-dimethylformamide) clathrate ; _chemical_name_common none _chemical_melting_point 278-280 _chemical_formula_moiety 'C34 H36 O2.4(C3 H7 N O)' _chemical_formula_sum 'C46 H64 N4 O6' _chemical_formula_weight 769.01 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' _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 9.0806(3) _cell_length_b 8.9414(4) _cell_length_c 14.9350(10) _cell_angle_alpha 74.477(2) _cell_angle_beta 88.693(2) _cell_angle_gamma 110.189(3) _cell_volume 1087.67(9) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4771 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 27.49 _exptl_crystal_description 'clear elongated plates' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.174 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 416 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type none _exptl_special_details ; Unstable without mother liquor under atmospheric conditions. Crystal coated with Paratone oil and data collected at 173K. ; _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 'Nonius Kappa CCD' _diffrn_measurement_method 'Combination of phi and omega' _diffrn_reflns_number 6935 _diffrn_reflns_av_R_equivalents 0.0167 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4771 _reflns_number_gt 3093 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 2000)' _computing_cell_refinement 'Collect (Nonius, 2000)' _computing_data_reduction 'Collect (Nonius, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED, a graphical interface to SHELX (1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0859P)^2^+0.4724P] 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_number_reflns 4771 _refine_ls_number_parameters 259 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0991 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1811 _refine_ls_wR_factor_gt 0.1497 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.056 _refine_ls_shift/su_mean 0.004 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 -0.26297(17) -0.17006(17) -0.06293(9) 0.0341(4) Uani 1 1 d . . . H1 H -0.2220 -0.0971 -0.1144 0.041 Uiso 1 1 calc R . . C1 C -0.1559(2) -0.1460(2) 0.00501(12) 0.0251(4) Uani 1 1 d . . . C2 C 0.0060(2) -0.1377(2) -0.03121(12) 0.0263(4) Uani 1 1 d . . . C3 C 0.0099(3) -0.2730(2) -0.06146(14) 0.0336(5) Uani 1 1 d . . . H3 H -0.0863 -0.3611 -0.0606 0.040 Uiso 1 1 calc R . . C4 C 0.1510(3) -0.2790(3) -0.09216(15) 0.0400(5) Uani 1 1 d . . . H4 H 0.1518 -0.3702 -0.1131 0.048 Uiso 1 1 calc R . . C5 C 0.2917(3) -0.1526(3) -0.09261(15) 0.0414(6) Uani 1 1 d . . . H5 H 0.3895 -0.1575 -0.1127 0.050 Uiso 1 1 calc R . . C6 C 0.2892(3) -0.0190(3) -0.06363(15) 0.0355(5) Uani 1 1 d . . . H6 H 0.3861 0.0681 -0.0643 0.043 Uiso 1 1 calc R . . C7 C 0.1462(2) -0.0097(2) -0.03319(12) 0.0270(4) Uani 1 1 d . . . C11 C -0.2273(2) -0.2982(2) 0.09190(12) 0.0239(4) Uani 1 1 d . . . C12 C -0.1438(2) -0.3133(2) 0.16859(13) 0.0303(4) Uani 1 1 d . . . H12 H -0.0421 -0.2318 0.1658 0.036 Uiso 1 1 calc R . . C13 C -0.2077(2) -0.4462(2) 0.24911(13) 0.0312(4) Uani 1 1 d . . . H13 H -0.1486 -0.4534 0.3007 0.037 Uiso 1 1 calc R . . C14 C -0.3558(2) -0.5693(2) 0.25664(13) 0.0271(4) Uani 1 1 d . . . C15 C -0.4370(2) -0.5544(2) 0.17916(13) 0.0282(4) Uani 1 1 d . . . H15 H -0.5378 -0.6369 0.1814 0.034 Uiso 1 1 calc R . . C16 C -0.3736(2) -0.4204(2) 0.09778(13) 0.0275(4) Uani 1 1 d . . . H16 H -0.4320 -0.4133 0.0458 0.033 Uiso 1 1 calc R . . C17 C -0.4196(3) -0.7149(2) 0.34750(14) 0.0348(5) Uani 1 1 d . . . C18 C -0.5886(3) -0.8273(3) 0.34642(19) 0.0575(7) Uani 1 1 d . . . H18A H -0.6234 -0.9203 0.4043 0.086 Uiso 1 1 calc R . . H18B H -0.5934 -0.8709 0.2925 0.086 Uiso 1 1 calc R . . H18C H -0.6581 -0.7633 0.3417 0.086 Uiso 1 1 calc R . . C19 C -0.3137(3) -0.8179(3) 0.35822(18) 0.0543(7) Uani 1 1 d . . . H19A H -0.2045 -0.7466 0.3593 0.081 Uiso 1 1 calc R . . H19B H -0.3181 -0.8641 0.3053 0.081 Uiso 1 1 calc R . . H19C H -0.3507 -0.9091 0.4169 0.081 Uiso 1 1 calc R . . C20 C -0.4157(4) -0.6481(3) 0.43266(16) 0.0543(7) Uani 1 1 d . . . H20A H -0.4802 -0.5786 0.4254 0.081 Uiso 1 1 calc R . . H20B H -0.3064 -0.5814 0.4369 0.081 Uiso 1 1 calc R . . H20C H -0.4580 -0.7419 0.4899 0.081 Uiso 1 1 calc R . . O21 O -0.1505(2) 0.0436(2) -0.23885(11) 0.0550(5) Uani 1 1 d . . . C22 C -0.0410(4) 0.0425(3) -0.28702(18) 0.0536(7) Uani 1 1 d . . . H22 H 0.0106 -0.0316 -0.2600 0.064 Uiso 1 1 calc R . . N23 N 0.0110(3) 0.1378(3) -0.37478(14) 0.0521(6) Uani 1 1 d . . . C24 C -0.0615(3) 0.2535(3) -0.42033(17) 0.0535(7) Uani 1 1 d . . . H24A H -0.0082 0.3125 -0.4844 0.080 Uiso 1 1 calc R . . H24B H -0.0519 0.3342 -0.3854 0.080 Uiso 1 1 calc R . . H24C H -0.1735 0.1924 -0.4221 0.080 Uiso 1 1 calc R . . C25 C 0.1494(6) 0.1420(6) -0.4274(3) 0.131(2) Uani 1 1 d . . . H25A H 0.1667 0.2197 -0.4903 0.197 Uiso 1 1 calc R . . H25B H 0.1328 0.0303 -0.4321 0.197 Uiso 1 1 calc R . . H25C H 0.2422 0.1789 -0.3952 0.197 Uiso 1 1 calc R . . O26 O -0.1318(3) -0.3854(4) -0.36646(16) 0.1034(9) Uani 1 1 d . . . C27 C -0.1498(4) -0.4635(4) -0.2849(2) 0.0672(8) Uani 1 1 d . . . H27 H -0.0729 -0.4183 -0.2477 0.081 Uiso 1 1 calc R . . N28 N -0.2664(3) -0.6063(3) -0.24209(14) 0.0488(5) Uani 1 1 d . . . C29 C -0.3936(4) -0.6887(4) -0.2878(2) 0.0713(9) Uani 1 1 d . . . H29A H -0.4940 -0.6940 -0.2589 0.107 Uiso 1 1 calc R . . H29B H -0.3971 -0.8019 -0.2814 0.107 Uiso 1 1 calc R . . H29C H -0.3765 -0.6263 -0.3544 0.107 Uiso 1 1 calc R . . C30 C -0.2706(3) -0.6870(4) -0.14405(18) 0.0564(7) Uani 1 1 d . . . H30A H -0.1732 -0.6274 -0.1217 0.085 Uiso 1 1 calc R . . H30B H -0.2796 -0.8025 -0.1354 0.085 Uiso 1 1 calc R . . H30C H -0.3620 -0.6858 -0.1084 0.085 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 0.0366(8) 0.0341(8) 0.0258(7) -0.0056(6) -0.0073(6) 0.0083(6) C1 0.0291(11) 0.0225(9) 0.0204(8) -0.0039(7) -0.0001(7) 0.0075(8) C2 0.0334(11) 0.0230(9) 0.0204(8) -0.0035(7) 0.0013(7) 0.0101(8) C3 0.0422(13) 0.0256(10) 0.0307(10) -0.0085(8) 0.0033(9) 0.0098(9) C4 0.0544(15) 0.0303(11) 0.0377(11) -0.0094(9) 0.0088(10) 0.0197(11) C5 0.0421(13) 0.0381(12) 0.0437(12) -0.0056(9) 0.0125(10) 0.0203(11) C6 0.0334(12) 0.0277(10) 0.0395(11) -0.0038(8) 0.0058(9) 0.0094(9) C7 0.0338(11) 0.0224(9) 0.0233(9) -0.0028(7) 0.0011(8) 0.0115(8) C11 0.0253(10) 0.0227(9) 0.0233(9) -0.0073(7) -0.0003(7) 0.0079(8) C12 0.0268(11) 0.0272(10) 0.0296(10) -0.0053(8) -0.0024(8) 0.0034(8) C13 0.0311(11) 0.0333(11) 0.0254(9) -0.0047(8) -0.0054(8) 0.0100(9) C14 0.0276(10) 0.0229(9) 0.0283(9) -0.0051(7) 0.0021(8) 0.0082(8) C15 0.0229(10) 0.0235(9) 0.0329(10) -0.0077(8) -0.0002(8) 0.0029(8) C16 0.0277(11) 0.0281(10) 0.0263(9) -0.0085(8) -0.0051(8) 0.0092(8) C17 0.0362(12) 0.0294(10) 0.0309(10) -0.0010(8) 0.0017(9) 0.0088(9) C18 0.0468(16) 0.0450(14) 0.0520(15) 0.0077(11) 0.0003(12) -0.0010(12) C19 0.0646(18) 0.0455(14) 0.0459(14) 0.0060(11) 0.0048(12) 0.0271(13) C20 0.0684(18) 0.0486(14) 0.0346(12) -0.0044(10) 0.0067(12) 0.0144(13) O21 0.0538(11) 0.0623(11) 0.0329(9) -0.0085(8) -0.0076(8) 0.0058(9) C22 0.0681(19) 0.0470(14) 0.0427(13) -0.0067(11) -0.0057(13) 0.0224(13) N23 0.0704(15) 0.0455(11) 0.0384(11) -0.0003(9) 0.0078(10) 0.0285(11) C24 0.0628(18) 0.0587(16) 0.0376(13) -0.0050(11) -0.0067(12) 0.0272(14) C25 0.166(4) 0.146(4) 0.093(3) 0.034(3) 0.056(3) 0.127(4) O26 0.120(2) 0.114(2) 0.0592(14) 0.0272(13) 0.0256(13) 0.0643(18) C27 0.0633(19) 0.0692(19) 0.0632(18) 0.0013(15) 0.0123(15) 0.0340(16) N28 0.0496(13) 0.0526(12) 0.0437(11) -0.0061(9) 0.0003(10) 0.0246(10) C29 0.076(2) 0.096(2) 0.0679(19) -0.0383(18) -0.0245(17) 0.0506(19) C30 0.0503(16) 0.0708(18) 0.0467(14) -0.0061(12) -0.0030(12) 0.0289(14) _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 1.428(2) . ? C1 C2 1.525(3) . ? C1 C7 1.534(2) 2 ? C1 C11 1.537(2) . ? C2 C7 1.381(3) . ? C2 C3 1.410(3) . ? C3 C4 1.374(3) . ? C4 C5 1.382(3) . ? C5 C6 1.382(3) . ? C6 C7 1.403(3) . ? C7 C1 1.534(2) 2 ? C11 C16 1.382(3) . ? C11 C12 1.390(3) . ? C12 C13 1.386(3) . ? C13 C14 1.392(3) . ? C14 C15 1.387(3) . ? C14 C17 1.539(3) . ? C15 C16 1.399(3) . ? C17 C18 1.521(3) . ? C17 C19 1.529(3) . ? C17 C20 1.539(3) . ? O21 C22 1.218(3) . ? C22 N23 1.328(3) . ? N23 C24 1.442(3) . ? N23 C25 1.450(4) . ? O26 C27 1.206(4) . ? C27 N28 1.327(4) . ? N28 C29 1.436(4) . ? N28 C30 1.442(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 O1 C1 C2 110.81(14) . . ? O1 C1 C7 110.06(15) . 2 ? C2 C1 C7 112.20(15) . 2 ? O1 C1 C11 106.34(14) . . ? C2 C1 C11 109.29(14) . . ? C7 C1 C11 107.92(14) 2 . ? C7 C2 C3 119.22(18) . . ? C7 C2 C1 123.95(15) . . ? C3 C2 C1 116.80(17) . . ? C4 C3 C2 120.9(2) . . ? C3 C4 C5 120.05(18) . . ? C4 C5 C6 119.56(19) . . ? C5 C6 C7 121.2(2) . . ? C2 C7 C6 119.11(17) . . ? C2 C7 C1 123.74(16) . 2 ? C6 C7 C1 117.15(17) . 2 ? C16 C11 C12 118.19(17) . . ? C16 C11 C1 122.51(17) . . ? C12 C11 C1 119.29(16) . . ? C13 C12 C11 120.53(18) . . ? C12 C13 C14 122.03(18) . . ? C15 C14 C13 116.94(17) . . ? C15 C14 C17 123.45(17) . . ? C13 C14 C17 119.59(18) . . ? C14 C15 C16 121.40(17) . . ? C11 C16 C15 120.90(18) . . ? C18 C17 C19 108.9(2) . . ? C18 C17 C20 108.3(2) . . ? C19 C17 C20 108.8(2) . . ? C18 C17 C14 112.04(18) . . ? C19 C17 C14 108.45(17) . . ? C20 C17 C14 110.29(17) . . ? O21 C22 N23 124.5(2) . . ? C22 N23 C24 120.8(2) . . ? C22 N23 C25 122.7(2) . . ? C24 N23 C25 116.3(2) . . ? O26 C27 N28 126.4(4) . . ? C27 N28 C29 123.6(3) . . ? C27 N28 C30 120.1(3) . . ? C29 N28 C30 116.3(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C7 127.10(18) . . . . ? C7 C1 C2 C7 3.6(3) 2 . . . ? C11 C1 C2 C7 -116.03(19) . . . . ? O1 C1 C2 C3 -54.9(2) . . . . ? C7 C1 C2 C3 -178.33(16) 2 . . . ? C11 C1 C2 C3 62.0(2) . . . . ? C7 C2 C3 C4 0.4(3) . . . . ? C1 C2 C3 C4 -177.75(18) . . . . ? C2 C3 C4 C5 0.8(3) . . . . ? C3 C4 C5 C6 -1.2(3) . . . . ? C4 C5 C6 C7 0.4(3) . . . . ? C3 C2 C7 C6 -1.2(3) . . . . ? C1 C2 C7 C6 176.82(17) . . . . ? C3 C2 C7 C1 177.97(17) . . . 2 ? C1 C2 C7 C1 -4.0(3) . . . 2 ? C5 C6 C7 C2 0.8(3) . . . . ? C5 C6 C7 C1 -178.37(18) . . . 2 ? O1 C1 C11 C16 -4.4(2) . . . . ? C2 C1 C11 C16 -124.11(18) . . . . ? C7 C1 C11 C16 113.62(19) 2 . . . ? O1 C1 C11 C12 176.76(16) . . . . ? C2 C1 C11 C12 57.1(2) . . . . ? C7 C1 C11 C12 -65.2(2) 2 . . . ? C16 C11 C12 C13 -1.1(3) . . . . ? C1 C11 C12 C13 177.77(17) . . . . ? C11 C12 C13 C14 0.3(3) . . . . ? C12 C13 C14 C15 0.7(3) . . . . ? C12 C13 C14 C17 179.32(18) . . . . ? C13 C14 C15 C16 -0.9(3) . . . . ? C17 C14 C15 C16 -179.48(17) . . . . ? C12 C11 C16 C15 0.9(3) . . . . ? C1 C11 C16 C15 -177.95(16) . . . . ? C14 C15 C16 C11 0.1(3) . . . . ? C15 C14 C17 C18 -6.9(3) . . . . ? C13 C14 C17 C18 174.5(2) . . . . ? C15 C14 C17 C19 113.2(2) . . . . ? C13 C14 C17 C19 -65.3(2) . . . . ? C15 C14 C17 C20 -127.7(2) . . . . ? C13 C14 C17 C20 53.7(3) . . . . ? O21 C22 N23 C24 0.1(4) . . . . ? O21 C22 N23 C25 175.1(4) . . . . ? O26 C27 N28 C29 -1.5(4) . . . . ? O26 C27 N28 C30 178.9(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O21 0.84 1.89 2.728(2) 171.2 . _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.269 _refine_diff_density_min -0.250 _refine_diff_density_rms 0.049 #========================================================END data_c:_H.3A.B _database_code_CSD 175484 _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-9,10-dihydroxy-9,10-bis(p-tert-butylphenyl)-9,10-dihydroanthracene. 3(N,N-dimethylformamide). 1(dimethyl sulfoxide) clathrate ; _chemical_name_common none _chemical_melting_point 279-281 _chemical_formula_moiety 'C34 H36 O2. 3(C3 H7 N O). 1(C2 H6 O S)' _chemical_formula_sum 'C45 H63 N3 O6 S' _chemical_formula_weight 774.04 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 9.0858(2) _cell_length_b 9.0547(2) _cell_length_c 14.7684(4) _cell_angle_alpha 107.1440(10) _cell_angle_beta 91.5270(10) _cell_angle_gamma 70.236(2) _cell_volume 1089.00(4) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6059 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 29.58 _exptl_crystal_description 'clear elongated plates' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.180 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 418 _exptl_absorpt_coefficient_mu 0.123 _exptl_absorpt_correction_type none _exptl_special_details ; Unstable without mother liquor under atmospheric conditions. Crystal coated with Paratone oil and data collected at 173K. ; _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 'Nonius Kappa CCD' _diffrn_measurement_method 'Combination of phi and omega' _diffrn_reflns_number 11163 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 29.62 _reflns_number_total 6059 _reflns_number_gt 4429 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 2000)' _computing_cell_refinement 'Collect (Nonius, 2000)' _computing_data_reduction 'Collect (Nonius, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED, a graphical interface to SHELX (1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 6059 _refine_ls_number_parameters 287 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1420 _refine_ls_R_factor_gt 0.1166 _refine_ls_wR_factor_ref 0.4104 _refine_ls_wR_factor_gt 0.3845 _refine_ls_goodness_of_fit_ref 1.651 _refine_ls_restrained_S_all 1.651 _refine_ls_shift/su_max 0.125 _refine_ls_shift/su_mean 0.019 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 0.25930(19) -0.1587(2) 0.07169(12) 0.0386(5) Uani 1 1 d . . . H1 H 0.2184 -0.0836 0.1225 0.046 Uiso 1 1 calc R . . C1 C 0.1545(2) -0.1415(2) -0.00177(16) 0.0302(5) Uani 1 1 d . . . C2 C -0.0053(2) -0.1361(2) 0.03020(16) 0.0325(5) Uani 1 1 d . . . C3 C -0.0111(3) -0.2684(3) 0.05977(19) 0.0409(6) Uani 1 1 d . . . H3 H 0.0839 -0.3545 0.0604 0.049 Uiso 1 1 calc R . . C4 C -0.1515(3) -0.2763(3) 0.0879(2) 0.0490(7) Uani 1 1 d . . . H4 H -0.1524 -0.3660 0.1084 0.059 Uiso 1 1 calc R . . C5 C -0.2901(3) -0.1527(3) 0.0859(2) 0.0501(7) Uani 1 1 d . . . H5 H -0.3872 -0.1583 0.1040 0.060 Uiso 1 1 calc R . . C6 C -0.2877(3) -0.0201(3) 0.0574(2) 0.0411(6) Uani 1 1 d . . . H6 H -0.3835 0.0649 0.0566 0.049 Uiso 1 1 calc R . . C7 C -0.1455(2) -0.0103(2) 0.02992(16) 0.0320(5) Uani 1 1 d . . . C11 C 0.2255(2) -0.2936(2) -0.08786(16) 0.0311(5) Uani 1 1 d . . . C12 C 0.3717(2) -0.4127(3) -0.08979(17) 0.0338(5) Uani 1 1 d . . . H12 H 0.4301 -0.4009 -0.0354 0.041 Uiso 1 1 calc R . . C13 C 0.4335(3) -0.5477(3) -0.16923(18) 0.0361(5) Uani 1 1 d . . . H13 H 0.5332 -0.6268 -0.1679 0.043 Uiso 1 1 calc R . . C14 C 0.3536(3) -0.5710(3) -0.25111(17) 0.0360(5) Uani 1 1 d . . . C15 C 0.2054(3) -0.4522(3) -0.24789(19) 0.0410(6) Uani 1 1 d . . . H15 H 0.1466 -0.4646 -0.3020 0.049 Uiso 1 1 calc R . . C16 C 0.1421(3) -0.3177(3) -0.16857(18) 0.0389(6) Uani 1 1 d . . . H16 H 0.0407 -0.2407 -0.1689 0.047 Uiso 1 1 calc R . . C17 C 0.4163(3) -0.7203(3) -0.3405(2) 0.0459(6) Uani 1 1 d . . . C18 C 0.5842(4) -0.8267(4) -0.3333(3) 0.0710(10) Uani 1 1 d . . . H18A H 0.6537 -0.7632 -0.3298 0.107 Uiso 1 1 calc R . . H18B H 0.6178 -0.9243 -0.3894 0.107 Uiso 1 1 calc R . . H18C H 0.5889 -0.8611 -0.2759 0.107 Uiso 1 1 calc R . . C19 C 0.4130(5) -0.6640(4) -0.4279(2) 0.0667(9) Uani 1 1 d . . . H19A H 0.3061 -0.5934 -0.4328 0.100 Uiso 1 1 calc R . . H19B H 0.4463 -0.7603 -0.4847 0.100 Uiso 1 1 calc R . . H19C H 0.4843 -0.6019 -0.4225 0.100 Uiso 1 1 calc R . . C20 C 0.3081(5) -0.8226(4) -0.3529(3) 0.0695(10) Uani 1 1 d . . . H20A H 0.3057 -0.8572 -0.2962 0.104 Uiso 1 1 calc R . . H20B H 0.3478 -0.9202 -0.4087 0.104 Uiso 1 1 calc R . . H20C H 0.2018 -0.7558 -0.3618 0.104 Uiso 1 1 calc R . . O21 O 0.1446(5) 0.0508(5) 0.2399(2) 0.0794(11) Uani 0.75 1 d P . . C22 C 0.0266(9) 0.0508(7) 0.2872(4) 0.0885(19) Uani 0.75 1 d P . . N23 N -0.0237(6) 0.1447(5) 0.3760(3) 0.0771(12) Uani 0.75 1 d P . . C24 C 0.0560(7) 0.2536(6) 0.4252(4) 0.0734(14) Uani 0.75 1 d P . . C25 C -0.1938(13) 0.1812(12) 0.4172(8) 0.144(4) Uani 0.75 1 d P . . O26 O 0.2454(7) 0.1404(7) 0.2140(4) 0.0803(15) Uani 0.50 1 d P . . S27 S 0.3360(2) 0.2384(3) 0.19143(16) 0.0754(6) Uani 0.50 1 d P . . C28 C 0.2096(12) 0.4303(14) 0.1970(14) 0.110(5) Uani 0.50 1 d P . . C29 C 0.4171(8) 0.2997(7) 0.2920(4) 0.133(2) Uani 1.25 1 d P . . O30 O 0.1282(9) 0.6151(8) 0.3637(4) 0.146(3) Uani 0.75 1 d P . . C31 C 0.1509(9) 0.5365(10) 0.2827(5) 0.098(2) Uani 0.75 1 d P . . N32 N 0.2720(5) 0.3892(6) 0.2449(3) 0.0637(10) Uani 0.75 1 d P . . C33 C 0.2740(8) 0.3182(9) 0.1449(4) 0.0794(14) Uani 0.75 1 d P . . 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 0.0289(8) 0.0365(9) 0.0449(10) 0.0147(7) -0.0030(7) -0.0024(6) C1 0.0234(10) 0.0245(9) 0.0417(12) 0.0147(8) 0.0002(8) -0.0027(7) C2 0.0280(10) 0.0251(10) 0.0422(12) 0.0134(9) 0.0058(8) -0.0030(8) C3 0.0372(12) 0.0292(11) 0.0561(15) 0.0201(10) 0.0079(10) -0.0043(9) C4 0.0502(15) 0.0344(12) 0.0664(17) 0.0219(12) 0.0146(12) -0.0125(11) C5 0.0401(13) 0.0389(13) 0.0733(19) 0.0183(13) 0.0179(13) -0.0134(11) C6 0.0258(10) 0.0328(11) 0.0624(16) 0.0162(11) 0.0096(10) -0.0047(8) C7 0.0272(10) 0.0246(9) 0.0426(12) 0.0120(8) 0.0051(8) -0.0049(8) C11 0.0208(9) 0.0242(9) 0.0475(12) 0.0165(9) 0.0017(8) -0.0017(7) C12 0.0241(10) 0.0298(10) 0.0444(12) 0.0167(9) -0.0002(8) -0.0006(8) C13 0.0242(10) 0.0283(10) 0.0515(13) 0.0158(10) 0.0027(9) -0.0003(8) C14 0.0295(11) 0.0280(10) 0.0474(13) 0.0119(9) 0.0051(9) -0.0051(8) C15 0.0285(11) 0.0364(12) 0.0513(14) 0.0111(10) -0.0052(10) -0.0050(9) C16 0.0244(10) 0.0323(11) 0.0506(14) 0.0128(10) -0.0007(9) 0.0022(8) C17 0.0410(13) 0.0330(12) 0.0524(15) 0.0049(11) 0.0069(11) -0.0048(10) C18 0.0544(19) 0.0493(17) 0.074(2) -0.0014(15) 0.0084(16) 0.0099(14) C19 0.080(2) 0.0522(17) 0.0524(17) 0.0105(14) 0.0110(16) -0.0074(16) C20 0.081(2) 0.0516(17) 0.069(2) -0.0014(15) 0.0101(18) -0.0308(17) O21 0.075(2) 0.075(2) 0.0516(18) 0.0030(16) -0.0071(17) 0.0066(18) C22 0.102(5) 0.064(3) 0.063(3) -0.009(2) -0.022(3) -0.009(3) N23 0.105(3) 0.056(2) 0.077(3) 0.016(2) -0.021(2) -0.040(2) C24 0.075(3) 0.066(3) 0.063(3) -0.007(2) -0.010(2) -0.027(2) C25 0.154(8) 0.133(7) 0.153(8) -0.006(6) 0.035(6) -0.099(7) O26 0.078(4) 0.072(3) 0.086(4) 0.014(3) -0.008(3) -0.030(3) S27 0.0630(11) 0.0766(13) 0.0828(13) 0.0215(11) 0.0021(10) -0.0211(10) C28 0.061(6) 0.073(6) 0.203(15) 0.066(9) 0.016(8) -0.007(5) C29 0.175(6) 0.164(5) 0.119(4) 0.070(4) -0.050(4) -0.112(5) O30 0.176(6) 0.158(5) 0.086(3) -0.031(3) 0.040(4) -0.091(5) C31 0.088(4) 0.104(5) 0.091(4) 0.000(4) 0.017(3) -0.045(4) N32 0.058(2) 0.060(2) 0.065(2) 0.0052(19) 0.0015(19) -0.021(2) C33 0.072(3) 0.088(4) 0.080(4) 0.031(3) -0.012(3) -0.026(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 O1 C1 1.433(3) . ? C1 C2 1.519(3) . ? C1 C7 1.525(3) 2 ? C1 C11 1.530(3) . ? C2 C7 1.393(3) . ? C2 C3 1.407(3) . ? C3 C4 1.382(3) . ? C4 C5 1.380(4) . ? C5 C6 1.391(3) . ? C6 C7 1.404(3) . ? C7 C1 1.525(3) 2 ? C11 C12 1.394(3) . ? C11 C16 1.397(3) . ? C12 C13 1.382(3) . ? C13 C14 1.393(4) . ? C14 C15 1.402(3) . ? C14 C17 1.537(3) . ? C15 C16 1.381(4) . ? C17 C19 1.516(4) . ? C17 C18 1.525(4) . ? C17 C20 1.538(5) . ? O21 C22 1.295(8) . ? O21 O26 1.532(8) . ? C22 N23 1.328(7) . ? N23 C24 1.434(6) . ? N23 C25 1.566(11) . ? O26 S27 1.503(6) . ? S27 C33 1.144(6) . ? S27 N32 1.295(5) . ? S27 C29 1.671(5) . ? S27 C28 1.708(10) . ? C28 N32 0.976(15) . ? C28 C33 1.062(14) . ? C28 C31 1.335(18) . ? C29 N32 1.562(8) . ? O30 C31 1.181(8) . ? C31 N32 1.379(9) . ? N32 C33 1.425(8) . ? 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 110.14(17) . . ? O1 C1 C7 109.85(18) . 2 ? C2 C1 C7 112.50(16) . 2 ? O1 C1 C11 106.75(16) . . ? C2 C1 C11 109.20(17) . . ? C7 C1 C11 108.20(17) 2 . ? C7 C2 C3 118.5(2) . . ? C7 C2 C1 123.88(17) . . ? C3 C2 C1 117.59(18) . . ? C4 C3 C2 121.7(2) . . ? C5 C4 C3 119.5(2) . . ? C4 C5 C6 120.0(2) . . ? C5 C6 C7 120.8(2) . . ? C2 C7 C6 119.44(19) . . ? C2 C7 C1 123.56(18) . 2 ? C6 C7 C1 117.00(18) . 2 ? C12 C11 C16 117.5(2) . . ? C12 C11 C1 122.8(2) . . ? C16 C11 C1 119.76(18) . . ? C13 C12 C11 121.3(2) . . ? C12 C13 C14 121.8(2) . . ? C13 C14 C15 116.4(2) . . ? C13 C14 C17 123.7(2) . . ? C15 C14 C17 119.8(2) . . ? C16 C15 C14 122.1(2) . . ? C15 C16 C11 120.8(2) . . ? C19 C17 C18 108.5(3) . . ? C19 C17 C14 110.4(2) . . ? C18 C17 C14 111.7(2) . . ? C19 C17 C20 108.1(3) . . ? C18 C17 C20 109.8(3) . . ? C14 C17 C20 108.2(2) . . ? C22 O21 O26 151.2(4) . . ? O21 C22 N23 124.3(5) . . ? C22 N23 C24 119.4(5) . . ? C22 N23 C25 121.0(6) . . ? C24 N23 C25 116.9(5) . . ? S27 O26 O21 176.4(5) . . ? C33 S27 N32 71.2(4) . . ? C33 S27 O26 114.0(4) . . ? N32 S27 O26 107.3(3) . . ? C33 S27 C29 126.2(4) . . ? N32 S27 C29 62.1(3) . . ? O26 S27 C29 104.2(3) . . ? C33 S27 C28 37.5(7) . . ? N32 S27 C28 34.6(6) . . ? O26 S27 C28 109.2(4) . . ? C29 S27 C28 95.5(7) . . ? N32 C28 C33 88.6(9) . . ? N32 C28 C31 71.4(14) . . ? C33 C28 C31 158.9(15) . . ? N32 C28 S27 48.9(5) . . ? C33 C28 S27 41.0(5) . . ? C31 C28 S27 118.0(12) . . ? N32 C29 S27 47.1(2) . . ? O30 C31 C28 166.6(10) . . ? O30 C31 N32 125.1(8) . . ? C28 C31 N32 42.1(6) . . ? C28 N32 S27 96.5(10) . . ? C28 N32 C31 66.5(10) . . ? S27 N32 C31 155.7(5) . . ? C28 N32 C33 48.2(9) . . ? S27 N32 C33 49.5(3) . . ? C31 N32 C33 114.4(6) . . ? C28 N32 C29 159.8(9) . . ? S27 N32 C29 70.8(3) . . ? C31 N32 C29 130.1(5) . . ? C33 N32 C29 115.1(5) . . ? C28 C33 S27 101.4(10) . . ? C28 C33 N32 43.2(9) . . ? S27 C33 N32 59.4(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C7 125.6(2) . . . . ? C7 C1 C2 C7 2.7(4) 2 . . . ? C11 C1 C2 C7 -117.5(2) . . . . ? O1 C1 C2 C3 -55.8(3) . . . . ? C7 C1 C2 C3 -178.8(2) 2 . . . ? C11 C1 C2 C3 61.1(3) . . . . ? C7 C2 C3 C4 0.2(4) . . . . ? C1 C2 C3 C4 -178.4(2) . . . . ? C2 C3 C4 C5 0.8(5) . . . . ? C3 C4 C5 C6 -1.1(5) . . . . ? C4 C5 C6 C7 0.4(5) . . . . ? C3 C2 C7 C6 -1.0(4) . . . . ? C1 C2 C7 C6 177.6(2) . . . . ? C3 C2 C7 C1 178.5(2) . . . 2 ? C1 C2 C7 C1 -3.0(4) . . . 2 ? C5 C6 C7 C2 0.7(4) . . . . ? C5 C6 C7 C1 -178.8(2) . . . 2 ? O1 C1 C11 C12 -4.6(3) . . . . ? C2 C1 C11 C12 -123.7(2) . . . . ? C7 C1 C11 C12 113.5(2) 2 . . . ? O1 C1 C11 C16 174.84(18) . . . . ? C2 C1 C11 C16 55.8(2) . . . . ? C7 C1 C11 C16 -67.0(2) 2 . . . ? C16 C11 C12 C13 1.4(3) . . . . ? C1 C11 C12 C13 -179.12(19) . . . . ? C11 C12 C13 C14 0.3(3) . . . . ? C12 C13 C14 C15 -1.5(3) . . . . ? C12 C13 C14 C17 -179.0(2) . . . . ? C13 C14 C15 C16 0.9(4) . . . . ? C17 C14 C15 C16 178.6(2) . . . . ? C14 C15 C16 C11 0.8(4) . . . . ? C12 C11 C16 C15 -1.9(3) . . . . ? C1 C11 C16 C15 178.5(2) . . . . ? C13 C14 C17 C19 -128.2(3) . . . . ? C15 C14 C17 C19 54.3(3) . . . . ? C13 C14 C17 C18 -7.4(4) . . . . ? C15 C14 C17 C18 175.1(3) . . . . ? C13 C14 C17 C20 113.7(3) . . . . ? C15 C14 C17 C20 -63.8(3) . . . . ? O26 O21 C22 N23 -35.8(12) . . . . ? O21 C22 N23 C24 -0.6(8) . . . . ? O21 C22 N23 C25 160.2(7) . . . . ? C22 O21 O26 S27 -16(8) . . . . ? O21 O26 S27 C33 -58(7) . . . . ? O21 O26 S27 N32 18(7) . . . . ? O21 O26 S27 C29 83(7) . . . . ? O21 O26 S27 C28 -18(7) . . . . ? C33 S27 C28 N32 -162.4(12) . . . . ? O26 S27 C28 N32 92.8(7) . . . . ? C29 S27 C28 N32 -14.3(7) . . . . ? N32 S27 C28 C33 162.4(12) . . . . ? O26 S27 C28 C33 -104.7(7) . . . . ? C29 S27 C28 C33 148.1(7) . . . . ? C33 S27 C28 C31 178.1(14) . . . . ? N32 S27 C28 C31 -19.5(6) . . . . ? O26 S27 C28 C31 73.4(10) . . . . ? C29 S27 C28 C31 -33.8(8) . . . . ? C33 S27 C29 N32 32.7(5) . . . . ? O26 S27 C29 N32 -102.3(4) . . . . ? C28 S27 C29 N32 9.2(5) . . . . ? N32 C28 C31 O30 20(4) . . . . ? C33 C28 C31 O30 39(6) . . . . ? S27 C28 C31 O30 35(4) . . . . ? C33 C28 C31 N32 19(3) . . . . ? S27 C28 C31 N32 15.4(4) . . . . ? C33 C28 N32 S27 -11.4(8) . . . . ? C31 C28 N32 S27 161.9(4) . . . . ? C33 C28 N32 C31 -173.3(9) . . . . ? S27 C28 N32 C31 -161.9(4) . . . . ? C31 C28 N32 C33 173.3(9) . . . . ? S27 C28 N32 C33 11.4(8) . . . . ? C33 C28 N32 C29 38(3) . . . . ? C31 C28 N32 C29 -148(2) . . . . ? S27 C28 N32 C29 50(3) . . . . ? C33 S27 N32 C28 11.2(8) . . . . ? O26 S27 N32 C28 -98.9(7) . . . . ? C29 S27 N32 C28 163.8(8) . . . . ? C33 S27 N32 C31 55.0(13) . . . . ? O26 S27 N32 C31 -55.1(13) . . . . ? C29 S27 N32 C31 -152.4(13) . . . . ? C28 S27 N32 C31 43.8(12) . . . . ? O26 S27 N32 C33 -110.1(4) . . . . ? C29 S27 N32 C33 152.6(4) . . . . ? C28 S27 N32 C33 -11.2(7) . . . . ? C33 S27 N32 C29 -152.6(4) . . . . ? O26 S27 N32 C29 97.3(4) . . . . ? C28 S27 N32 C29 -163.8(8) . . . . ? O30 C31 N32 C28 -174.5(10) . . . . ? O30 C31 N32 S27 136.9(11) . . . . ? C28 C31 N32 S27 -48.6(13) . . . . ? O30 C31 N32 C33 -180.0(7) . . . . ? C28 C31 N32 C33 -5.5(7) . . . . ? O30 C31 N32 C29 -8.2(10) . . . . ? C28 C31 N32 C29 166.3(10) . . . . ? S27 C29 N32 C28 -53(3) . . . . ? S27 C29 N32 C31 165.6(6) . . . . ? S27 C29 N32 C33 -22.7(4) . . . . ? N32 C28 C33 S27 13.1(9) . . . . ? C31 C28 C33 S27 -5(3) . . . . ? C31 C28 C33 N32 -18(3) . . . . ? S27 C28 C33 N32 -13.1(9) . . . . ? N32 S27 C33 C28 -10.4(7) . . . . ? O26 S27 C33 C28 90.7(8) . . . . ? C29 S27 C33 C28 -40.7(9) . . . . ? O26 S27 C33 N32 101.1(4) . . . . ? C29 S27 C33 N32 -30.3(5) . . . . ? C28 S27 C33 N32 10.4(7) . . . . ? S27 N32 C33 C28 165.0(10) . . . . ? C31 N32 C33 C28 6.7(9) . . . . ? C29 N32 C33 C28 -166.3(10) . . . . ? C28 N32 C33 S27 -165.0(10) . . . . ? C31 N32 C33 S27 -158.3(5) . . . . ? C29 N32 C33 S27 28.7(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O21 0.84 1.79 2.623(4) 170.6 . O1 H1 O26 0.84 2.17 2.863(6) 139.8 . _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 29.62 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.929 _refine_diff_density_min -0.880 _refine_diff_density_rms 0.098 #========================================================END data_c:_H.2A.2B _database_code_CSD 175485 _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-9,10-dihydroxy-9,10-bis(p-tert-butylphenyl)-9,10-dihydroanthracene. 2(N,N-dimethylformamide). 2(dimethyl sulfoxide) clathrate ; _chemical_name_common none _chemical_melting_point 276-278 _chemical_formula_moiety 'C34 H36 O2. 2(C3 H7 N O). 2(C2 H6 O S)' _chemical_formula_sum 'C44 H62 N2 O6 S2' _chemical_formula_weight 779.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 9.1425(3) _cell_length_b 9.1730(3) _cell_length_c 14.273(1) _cell_angle_alpha 71.356(1) _cell_angle_beta 81.229(1) _cell_angle_gamma 69.938(1) _cell_volume 1064.13(9) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4625 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'clear elongated plates' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.216 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 420 _exptl_absorpt_coefficient_mu 0.173 _exptl_absorpt_correction_type none _exptl_special_details ; Unstable without mother liquor under atmospheric conditions. Crystal coated with Paratone oil and data collected at 173K. ; _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 'Nonius Kappa CCD' _diffrn_measurement_method 'Combination of phi and omega' _diffrn_reflns_number 5770 _diffrn_reflns_av_R_equivalents 0.0145 _diffrn_reflns_av_sigmaI/netI 0.0481 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4625 _reflns_number_gt 3420 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 2000)' _computing_cell_refinement 'Collect (Nonius, 2000)' _computing_data_reduction 'Collect (Nonius, 2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED, a graphical interface to SHELX (1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1491P)^2^+2.4558P] 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_number_reflns 4625 _refine_ls_number_parameters 249 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1179 _refine_ls_R_factor_gt 0.0902 _refine_ls_wR_factor_ref 0.2706 _refine_ls_wR_factor_gt 0.2445 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.159 _refine_ls_shift/su_mean 0.005 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.2575(3) -0.2283(3) 0.08250(16) 0.0233(5) Uani 1 1 d . . . H1 H 0.2444 -0.1735 0.1220 0.028 Uiso 1 1 calc R . . C1 C 0.1550(3) -0.1376(4) 0.0027(2) 0.0182(6) Uani 1 1 d . . . C2 C -0.0035(4) -0.1654(4) 0.0318(2) 0.0188(6) Uani 1 1 d . . . C3 C -0.0063(4) -0.3256(4) 0.0626(3) 0.0269(8) Uani 1 1 d . . . H3 H 0.0895 -0.4114 0.0669 0.032 Uiso 1 1 calc R . . C4 C -0.1444(5) -0.3626(4) 0.0870(3) 0.0309(8) Uani 1 1 d . . . H4 H -0.1435 -0.4721 0.1078 0.037 Uiso 1 1 calc R . . C5 C -0.2855(4) -0.2361(4) 0.0807(3) 0.0301(8) Uani 1 1 d . . . H5 H -0.3815 -0.2590 0.0960 0.036 Uiso 1 1 calc R . . C6 C -0.2842(4) -0.0783(4) 0.0522(2) 0.0236(7) Uani 1 1 d . . . H6 H -0.3802 0.0069 0.0491 0.028 Uiso 1 1 calc R . . C7 C -0.1438(4) -0.0405(4) 0.0274(2) 0.0184(6) Uani 1 1 d . . . C11 C 0.2272(3) -0.2052(4) -0.0852(2) 0.0173(6) Uani 1 1 d . . . C12 C 0.1448(4) -0.1500(4) -0.1713(2) 0.0216(7) Uani 1 1 d . . . H12 H 0.0443 -0.0716 -0.1745 0.026 Uiso 1 1 calc R . . C13 C 0.2080(4) -0.2083(4) -0.2521(2) 0.0230(7) Uani 1 1 d . . . H13 H 0.1501 -0.1684 -0.3099 0.028 Uiso 1 1 calc R . . C14 C 0.3556(4) -0.3251(4) -0.2498(2) 0.0206(7) Uani 1 1 d . . . C15 C 0.4354(4) -0.3801(4) -0.1638(2) 0.0208(7) Uani 1 1 d . . . H15 H 0.5351 -0.4601 -0.1600 0.025 Uiso 1 1 calc R . . C16 C 0.3732(4) -0.3209(4) -0.0823(2) 0.0209(7) Uani 1 1 d . . . H16 H 0.4312 -0.3603 -0.0246 0.025 Uiso 1 1 calc R . . C17 C 0.4188(4) -0.3878(4) -0.3404(2) 0.0263(8) Uani 1 1 d . . . C18 C 0.3156(6) -0.4810(6) -0.3525(3) 0.0426(10) Uani 1 1 d . . . H18A H 0.3202 -0.5737 -0.2936 0.064 Uiso 1 1 calc R . . H18B H 0.3529 -0.5197 -0.4110 0.064 Uiso 1 1 calc R . . H18C H 0.2077 -0.4091 -0.3606 0.064 Uiso 1 1 calc R . . C19 C 0.5874(5) -0.5005(5) -0.3296(3) 0.0433(11) Uani 1 1 d . . . H19A H 0.6537 -0.4428 -0.3198 0.065 Uiso 1 1 calc R . . H19B H 0.6241 -0.5351 -0.3896 0.065 Uiso 1 1 calc R . . H19C H 0.5923 -0.5958 -0.2724 0.065 Uiso 1 1 calc R . . C20 C 0.4125(5) -0.2453(5) -0.4338(3) 0.0348(9) Uani 1 1 d . . . H20A H 0.3051 -0.1723 -0.4420 0.052 Uiso 1 1 calc R . . H20B H 0.4484 -0.2863 -0.4916 0.052 Uiso 1 1 calc R . . H20C H 0.4800 -0.1862 -0.4276 0.052 Uiso 1 1 calc R . . O21 O 0.2421(3) -0.0645(3) 0.2165(2) 0.0360(6) Uani 1 1 d . . . S22 S 0.33702(11) 0.04975(12) 0.19115(7) 0.0329(3) Uani 1 1 d . . . C23 C 0.4556(6) -0.0076(6) 0.2916(4) 0.0556(13) Uani 1 1 d . . . H23A H 0.3898 -0.0039 0.3523 0.083 Uiso 1 1 calc R . . H23B H 0.5161 0.0672 0.2792 0.083 Uiso 1 1 calc R . . H23C H 0.5268 -0.1180 0.2990 0.083 Uiso 1 1 calc R . . C24 C 0.2074(6) 0.2345(6) 0.2058(6) 0.0718(19) Uani 1 1 d . . . H24A H 0.1268 0.2787 0.1572 0.108 Uiso 1 1 calc R . . H24B H 0.2648 0.3115 0.1957 0.108 Uiso 1 1 calc R . . H24C H 0.1584 0.2163 0.2728 0.108 Uiso 1 1 calc R . . O25 O 0.1974(9) 0.1956(9) -0.5501(6) 0.050 Uiso 0.432(6) 1 d P . . C26 C 0.1841(10) 0.2791(16) -0.4730(6) 0.127(4) Uani 1 1 d . . . N27 N 0.0668(7) 0.2369(6) -0.4112(3) 0.0645(13) Uani 1 1 d . . . C28 C 0.0252(8) 0.2875(9) -0.3202(4) 0.0747(18) Uani 1 1 d . . . H28A H 0.1162 0.2422 -0.2794 0.112 Uiso 1 1 calc R . . H28B H -0.0598 0.2479 -0.2832 0.112 Uiso 1 1 calc R . . H28C H -0.0084 0.4060 -0.3375 0.112 Uiso 1 1 calc R . . C29 C -0.0456(9) 0.1840(9) -0.4374(6) 0.085(2) Uani 1 1 d . . . O30 O -0.0003(7) 0.1457(7) -0.5193(4) 0.050 Uiso 0.568(6) 1 d P . . 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 0.0269(12) 0.0205(12) 0.0177(11) -0.0072(9) -0.0041(9) 0.0015(9) C1 0.0186(14) 0.0153(14) 0.0151(14) -0.0052(11) -0.0001(11) 0.0021(11) C2 0.0233(15) 0.0142(14) 0.0167(14) -0.0057(11) 0.0041(11) -0.0045(12) C3 0.0302(17) 0.0181(16) 0.0284(18) -0.0074(13) 0.0056(14) -0.0048(13) C4 0.043(2) 0.0197(17) 0.0299(18) -0.0069(14) 0.0089(16) -0.0138(15) C5 0.0315(18) 0.0307(19) 0.0298(18) -0.0091(15) 0.0081(14) -0.0153(15) C6 0.0227(16) 0.0241(17) 0.0240(16) -0.0102(13) 0.0046(12) -0.0068(13) C7 0.0219(15) 0.0177(15) 0.0142(14) -0.0069(11) 0.0013(11) -0.0033(12) C11 0.0193(14) 0.0137(14) 0.0177(14) -0.0063(11) 0.0022(11) -0.0035(11) C12 0.0175(14) 0.0231(16) 0.0213(16) -0.0094(13) -0.0001(12) -0.0003(12) C13 0.0219(15) 0.0269(17) 0.0176(15) -0.0088(13) -0.0007(12) -0.0026(13) C14 0.0243(15) 0.0181(15) 0.0192(15) -0.0081(12) 0.0054(12) -0.0064(12) C15 0.0190(14) 0.0168(15) 0.0226(16) -0.0080(12) 0.0036(12) -0.0004(12) C16 0.0209(15) 0.0191(15) 0.0176(15) -0.0053(12) -0.0027(12) 0.0007(12) C17 0.0318(18) 0.0254(17) 0.0204(16) -0.0127(13) 0.0059(13) -0.0048(14) C18 0.063(3) 0.045(2) 0.035(2) -0.0252(19) 0.011(2) -0.028(2) C19 0.044(2) 0.041(2) 0.031(2) -0.0199(18) 0.0075(17) 0.0070(19) C20 0.044(2) 0.035(2) 0.0236(18) -0.0116(15) 0.0094(15) -0.0117(17) O21 0.0417(15) 0.0342(15) 0.0386(15) -0.0174(12) -0.0041(12) -0.0128(12) S22 0.0291(5) 0.0399(6) 0.0289(5) -0.0093(4) -0.0009(4) -0.0107(4) C23 0.067(3) 0.045(3) 0.061(3) -0.004(2) -0.033(3) -0.023(2) C24 0.044(3) 0.033(3) 0.138(6) -0.027(3) -0.015(3) -0.006(2) C26 0.081(5) 0.243(13) 0.075(5) -0.066(7) 0.031(4) -0.067(7) N27 0.101(4) 0.056(3) 0.046(2) -0.013(2) 0.011(2) -0.044(3) C28 0.071(4) 0.099(5) 0.051(3) -0.014(3) 0.003(3) -0.032(4) C29 0.087(5) 0.089(5) 0.094(5) -0.032(4) -0.028(4) -0.034(4) _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 1.432(4) . ? C1 C7 1.522(5) 2 ? C1 C2 1.530(4) . ? C1 C11 1.536(4) . ? C2 C7 1.390(4) . ? C2 C3 1.401(5) . ? C3 C4 1.383(5) . ? C4 C5 1.400(5) . ? C5 C6 1.376(5) . ? C6 C7 1.408(5) . ? C7 C1 1.522(5) 2 ? C11 C16 1.388(4) . ? C11 C12 1.398(4) . ? C12 C13 1.389(4) . ? C13 C14 1.403(4) . ? C14 C15 1.385(5) . ? C14 C17 1.534(4) . ? C15 C16 1.401(4) . ? C17 C18 1.532(6) . ? C17 C19 1.532(5) . ? C17 C20 1.532(5) . ? O21 S22 1.506(3) . ? S22 C24 1.759(5) . ? S22 C23 1.762(5) . ? O25 C26 1.499(12) . ? C26 N27 1.362(9) . ? N27 C29 1.417(8) . ? N27 C28 1.469(7) . ? C29 O30 1.294(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C7 110.4(3) . 2 ? O1 C1 C2 109.6(2) . . ? C7 C1 C2 113.0(2) 2 . ? O1 C1 C11 106.9(2) . . ? C7 C1 C11 108.6(2) 2 . ? C2 C1 C11 108.1(3) . . ? C7 C2 C3 118.8(3) . . ? C7 C2 C1 123.5(3) . . ? C3 C2 C1 117.7(3) . . ? C4 C3 C2 121.9(3) . . ? C3 C4 C5 119.0(3) . . ? C6 C5 C4 119.6(3) . . ? C5 C6 C7 121.4(3) . . ? C2 C7 C6 119.2(3) . . ? C2 C7 C1 123.5(3) . 2 ? C6 C7 C1 117.3(3) . 2 ? C16 C11 C12 118.3(3) . . ? C16 C11 C1 121.9(3) . . ? C12 C11 C1 119.8(3) . . ? C13 C12 C11 120.9(3) . . ? C12 C13 C14 121.2(3) . . ? C15 C14 C13 117.4(3) . . ? C15 C14 C17 123.5(3) . . ? C13 C14 C17 119.2(3) . . ? C14 C15 C16 121.8(3) . . ? C11 C16 C15 120.5(3) . . ? C18 C17 C19 109.0(3) . . ? C18 C17 C20 108.7(3) . . ? C19 C17 C20 108.5(3) . . ? C18 C17 C14 108.4(3) . . ? C19 C17 C14 112.1(3) . . ? C20 C17 C14 110.1(3) . . ? O21 S22 C24 105.7(2) . . ? O21 S22 C23 107.0(2) . . ? C24 S22 C23 99.6(3) . . ? N27 C26 O25 102.0(8) . . ? C26 N27 C29 125.0(6) . . ? C26 N27 C28 118.6(6) . . ? C29 N27 C28 114.4(5) . . ? O30 C29 N27 109.8(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C7 126.1(3) . . . . ? C7 C1 C2 C7 2.4(5) 2 . . . ? C11 C1 C2 C7 -117.7(3) . . . . ? O1 C1 C2 C3 -55.2(4) . . . . ? C7 C1 C2 C3 -178.8(3) 2 . . . ? C11 C1 C2 C3 61.0(4) . . . . ? C7 C2 C3 C4 1.2(5) . . . . ? C1 C2 C3 C4 -177.6(3) . . . . ? C2 C3 C4 C5 0.0(5) . . . . ? C3 C4 C5 C6 -1.1(6) . . . . ? C4 C5 C6 C7 1.1(5) . . . . ? C3 C2 C7 C6 -1.2(5) . . . . ? C1 C2 C7 C6 177.5(3) . . . . ? C3 C2 C7 C1 178.6(3) . . . 2 ? C1 C2 C7 C1 -2.7(5) . . . 2 ? C5 C6 C7 C2 0.1(5) . . . . ? C5 C6 C7 C1 -179.7(3) . . . 2 ? O1 C1 C11 C16 -6.0(4) . . . . ? C7 C1 C11 C16 113.2(3) 2 . . . ? C2 C1 C11 C16 -123.9(3) . . . . ? O1 C1 C11 C12 173.9(3) . . . . ? C7 C1 C11 C12 -66.9(4) 2 . . . ? C2 C1 C11 C12 56.0(4) . . . . ? C16 C11 C12 C13 -0.6(5) . . . . ? C1 C11 C12 C13 179.5(3) . . . . ? C11 C12 C13 C14 0.5(5) . . . . ? C12 C13 C14 C15 0.2(5) . . . . ? C12 C13 C14 C17 178.9(3) . . . . ? C13 C14 C15 C16 -0.8(5) . . . . ? C17 C14 C15 C16 -179.3(3) . . . . ? C12 C11 C16 C15 0.0(5) . . . . ? C1 C11 C16 C15 179.9(3) . . . . ? C14 C15 C16 C11 0.6(5) . . . . ? C15 C14 C17 C18 112.9(4) . . . . ? C13 C14 C17 C18 -65.7(4) . . . . ? C15 C14 C17 C19 -7.5(5) . . . . ? C13 C14 C17 C19 174.0(3) . . . . ? C15 C14 C17 C20 -128.3(4) . . . . ? C13 C14 C17 C20 53.1(4) . . . . ? O25 C26 N27 C29 -21.0(11) . . . . ? O25 C26 N27 C28 175.8(6) . . . . ? C26 N27 C29 O30 14.8(11) . . . . ? C28 N27 C29 O30 178.5(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O21 0.84 1.91 2.747(4) 172.5 . _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 0.909 _refine_diff_density_min -2.245 _refine_diff_density_rms 0.103 #========================================================END data_c:_H.A.3B _database_code_CSD 175486 _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-9,10-dihydroxy-9,10-bis(p-tert-butylphenyl)-9,10-dihydroanthracene. 1(N,N-dimethylformamide). 3(dimethyl sulfoxide) clathrate. ; _chemical_name_common none _chemical_melting_point 280.5 _chemical_formula_moiety 'C34 H36 O2. 1(C3 H7 N O). 3(C2 H6 O S)' _chemical_formula_sum 'C43 H61 N O6 S3' _chemical_formula_weight 784.11 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 9.0460(2) _cell_length_b 9.1291(2) _cell_length_c 14.4090(10) _cell_angle_alpha 72.5590(10) _cell_angle_beta 80.1320(10) _cell_angle_gamma 71.486(2) _cell_volume 1072.64(8) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3710 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 25.02 _exptl_crystal_description 'clear elongated plates' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 422 _exptl_absorpt_coefficient_mu 0.218 _exptl_absorpt_correction_type none _exptl_special_details ; Unstable without mother liqour under atmospheric conditions. Crystal coated with Paratone oil and data collected at 173K. ; _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 'Nonius Kappa CCD' _diffrn_measurement_method 'Combination of phi and omega' _diffrn_reflns_number 5799 _diffrn_reflns_av_R_equivalents 0.0164 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3694 _reflns_number_gt 3060 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 2000)' _computing_cell_refinement 'Collect (Nonius, 2000)' _computing_data_reduction 'Collect (Nonius, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED, a graphical interface to SHELX (1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1034P)^2^+2.5429P] 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_number_reflns 3694 _refine_ls_number_parameters 257 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0961 _refine_ls_R_factor_gt 0.0816 _refine_ls_wR_factor_ref 0.2228 _refine_ls_wR_factor_gt 0.2087 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 1.563 _refine_ls_shift/su_mean 0.069 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 -0.2512(3) 0.2215(3) -0.08235(16) 0.0254(5) Uani 1 1 d . . . H1 H -0.2245 0.1730 -0.1264 0.030 Uiso 1 1 calc R . . C1 C -0.1539(4) 0.1360(4) -0.0032(2) 0.0203(7) Uani 1 1 d . . . C2 C 0.0076(4) 0.1640(4) -0.0316(2) 0.0198(7) Uani 1 1 d . . . C3 C 0.0140(4) 0.3233(4) -0.0617(2) 0.0285(8) Uani 1 1 d . . . H3 H -0.0807 0.4078 -0.0666 0.034 Uiso 1 1 calc R . . C4 C 0.1547(4) 0.3594(4) -0.0843(3) 0.0327(8) Uani 1 1 d . . . H4 H 0.1567 0.4679 -0.1043 0.039 Uiso 1 1 calc R . . C5 C 0.2936(4) 0.2368(4) -0.0779(3) 0.0313(8) Uani 1 1 d . . . H5 H 0.3911 0.2610 -0.0928 0.038 Uiso 1 1 calc R . . C6 C 0.2895(4) 0.0793(4) -0.0496(2) 0.0271(7) Uani 1 1 d . . . H6 H 0.3848 -0.0043 -0.0462 0.033 Uiso 1 1 calc R . . C7 C 0.1466(4) 0.0412(4) -0.0260(2) 0.0194(7) Uani 1 1 d . . . C11 C -0.2307(4) 0.2065(4) 0.0830(2) 0.0193(6) Uani 1 1 d . . . C12 C -0.1549(4) 0.1545(4) 0.1682(2) 0.0260(7) Uani 1 1 d . . . H12 H -0.0567 0.0750 0.1722 0.031 Uiso 1 1 calc R . . C13 C -0.2207(4) 0.2171(4) 0.2474(2) 0.0286(8) Uani 1 1 d . . . H13 H -0.1665 0.1795 0.3047 0.034 Uiso 1 1 calc R . . C14 C -0.3652(4) 0.3345(4) 0.2447(2) 0.0264(7) Uani 1 1 d . . . C15 C -0.4396(4) 0.3863(4) 0.1592(2) 0.0259(7) Uani 1 1 d . . . H15 H -0.5371 0.4670 0.1546 0.031 Uiso 1 1 calc R . . C16 C -0.3741(4) 0.3223(4) 0.0797(2) 0.0236(7) Uani 1 1 d . . . H16 H -0.4286 0.3587 0.0225 0.028 Uiso 1 1 calc R . . C17 C -0.4312(5) 0.4022(5) 0.3336(3) 0.0373(9) Uani 1 1 d . . . C18 C -0.4398(6) 0.2652(6) 0.4253(3) 0.0557(13) Uani 1 1 d . . . H18A H -0.3366 0.1868 0.4330 0.083 Uiso 1 1 calc R . . H18B H -0.5157 0.2133 0.4189 0.083 Uiso 1 1 calc R . . H18C H -0.4726 0.3081 0.4827 0.083 Uiso 1 1 calc R . . C19 C -0.5938(6) 0.5190(7) 0.3213(4) 0.0665(15) Uani 1 1 d . . . H19A H -0.6318 0.5573 0.3801 0.100 Uiso 1 1 calc R . . H19B H -0.6651 0.4649 0.3110 0.100 Uiso 1 1 calc R . . H19C H -0.5893 0.6101 0.2648 0.100 Uiso 1 1 calc R . . C20 C -0.3192(6) 0.4901(6) 0.3470(3) 0.0553(13) Uani 1 1 d . . . H20A H -0.2142 0.4154 0.3555 0.083 Uiso 1 1 calc R . . H20B H -0.3571 0.5312 0.4048 0.083 Uiso 1 1 calc R . . H20C H -0.3153 0.5794 0.2892 0.083 Uiso 1 1 calc R . . O21 O -0.2188(3) 0.0586(3) -0.2208(2) 0.0421(7) Uani 1 1 d . . . S22 S -0.32514(11) -0.04838(13) -0.19398(7) 0.0412(3) Uani 1 1 d . . . C23 C -0.2045(6) -0.2396(6) -0.2003(5) 0.0739(17) Uani 1 1 d . . . H23A H -0.1520 -0.2336 -0.2662 0.111 Uiso 1 1 calc R . . H23B H -0.2685 -0.3139 -0.1855 0.111 Uiso 1 1 calc R . . H23C H -0.1260 -0.2778 -0.1528 0.111 Uiso 1 1 calc R . . C24 C -0.4344(7) 0.0008(6) -0.2947(4) 0.0665(15) Uani 1 1 d . . . H24A H -0.4971 0.1131 -0.3069 0.100 Uiso 1 1 calc R . . H24B H -0.5038 -0.0680 -0.2807 0.100 Uiso 1 1 calc R . . H24C H -0.3630 -0.0154 -0.3525 0.100 Uiso 1 1 calc R . . O25 O 0.0523(15) 0.2702(16) 0.6781(8) 0.1174(18) Uiso 0.50 1 d PD . . C26 C 0.1302(18) 0.206(2) 0.6154(10) 0.1174(18) Uiso 0.50 1 d PD . . N27 N 0.0907(17) 0.200(2) 0.5289(9) 0.1174(18) Uiso 0.50 1 d PD . . C28 C -0.0613(16) 0.200(2) 0.5554(11) 0.1174(18) Uiso 0.50 1 d PD . . C29 C 0.110(2) 0.237(2) 0.4220(8) 0.1174(18) Uiso 0.50 1 d PD . . S30 S 0.1329(15) 0.2537(14) 0.5739(9) 0.1174(18) Uiso 0.23 1 d PD . . S31 S 0.0972(7) 0.1384(6) 0.5418(5) 0.081(2) Uani 0.25 1 d PD . . C32 C 0.165(3) 0.231(3) 0.4392(9) 0.1174(18) Uiso 0.25 1 d PD . . C33 C -0.0639(16) 0.291(3) 0.534(2) 0.1174(18) Uiso 0.25 1 d PD . . O34 O 0.143(3) 0.314(5) 0.498(3) 0.1174(18) Uiso 0.15 1 d PD . . S35 S -0.015(2) 0.335(2) 0.5435(12) 0.1174(18) Uiso 0.15 1 d PD . . C36 C -0.048(6) 0.136(4) 0.574(3) 0.1174(18) Uiso 0.15 1 d PD . . C37 C -0.019(4) 0.356(5) 0.6598(17) 0.1174(18) Uiso 0.25 1 d PD . . C39 C 0.136(13) 0.346(14) 0.500(9) 0.1174(18) Uiso 0.10 1 d P . . O38 O 0.215(8) 0.174(8) 0.576(5) 0.1174(18) Uiso 0.10 1 d P . . 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 0.0299(12) 0.0212(12) 0.0217(12) -0.0072(9) -0.0060(9) 0.0008(9) C1 0.0213(15) 0.0170(15) 0.0188(15) -0.0048(12) 0.0002(12) -0.0010(12) C2 0.0264(16) 0.0164(14) 0.0173(15) -0.0080(12) 0.0027(12) -0.0059(12) C3 0.0328(18) 0.0195(16) 0.0281(18) -0.0061(13) 0.0064(14) -0.0053(14) C4 0.042(2) 0.0217(17) 0.0351(19) -0.0088(15) 0.0079(16) -0.0148(16) C5 0.0325(19) 0.0335(19) 0.0323(19) -0.0112(15) 0.0072(14) -0.0182(16) C6 0.0241(17) 0.0287(18) 0.0291(17) -0.0119(14) 0.0033(13) -0.0070(14) C7 0.0237(16) 0.0186(15) 0.0174(15) -0.0089(12) 0.0013(11) -0.0057(12) C11 0.0211(15) 0.0158(15) 0.0213(16) -0.0072(12) 0.0021(12) -0.0055(12) C12 0.0248(17) 0.0239(17) 0.0260(17) -0.0095(14) 0.0009(13) -0.0013(13) C13 0.0330(19) 0.0314(19) 0.0218(17) -0.0099(14) -0.0012(13) -0.0076(15) C14 0.0338(18) 0.0214(16) 0.0254(17) -0.0115(13) 0.0083(14) -0.0102(14) C15 0.0240(16) 0.0187(16) 0.0328(18) -0.0122(14) 0.0061(13) -0.0024(13) C16 0.0250(16) 0.0175(15) 0.0258(17) -0.0064(13) -0.0017(13) -0.0021(12) C17 0.050(2) 0.034(2) 0.0280(19) -0.0187(16) 0.0113(16) -0.0096(17) C18 0.080(3) 0.051(3) 0.033(2) -0.020(2) 0.023(2) -0.020(2) C19 0.068(3) 0.067(3) 0.054(3) -0.042(3) 0.009(2) 0.012(3) C20 0.085(4) 0.056(3) 0.042(2) -0.031(2) 0.008(2) -0.034(3) O21 0.0462(16) 0.0373(15) 0.0488(17) -0.0187(13) -0.0122(13) -0.0088(12) S22 0.0348(6) 0.0493(6) 0.0394(6) -0.0149(5) -0.0015(4) -0.0095(4) C23 0.050(3) 0.036(3) 0.137(5) -0.020(3) -0.015(3) -0.012(2) C24 0.080(4) 0.058(3) 0.074(4) -0.009(3) -0.038(3) -0.027(3) S31 0.045(3) 0.043(3) 0.105(5) 0.011(3) 0.010(3) 0.019(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 1.435(4) . ? C1 C2 1.528(4) . ? C1 C11 1.529(4) . ? C1 C7 1.528(4) 2 ? C2 C7 1.389(4) . ? C2 C3 1.405(5) . ? C3 C4 1.377(5) . ? C4 C5 1.387(5) . ? C5 C6 1.383(5) . ? C6 C7 1.404(5) . ? C7 C1 1.528(4) 2 ? C11 C16 1.387(4) . ? C11 C12 1.391(5) . ? C12 C13 1.387(5) . ? C13 C14 1.401(5) . ? C14 C15 1.388(5) . ? C14 C17 1.536(4) . ? C15 C16 1.398(5) . ? C17 C19 1.521(6) . ? C17 C18 1.534(6) . ? C17 C20 1.543(6) . ? O21 S22 1.508(3) . ? S22 C24 1.761(5) . ? S22 C23 1.760(5) . ? O25 C26 1.220(9) . ? C26 N27 1.377(8) . ? N27 C28 1.363(9) . ? N27 C29 1.466(8) . ? S30 C39 1.15(12) . ? S30 O38 0.86(7) . ? S30 S31 1.409(9) . ? S30 C37 1.89(3) . ? S30 C32 1.976(10) . ? S31 C32 1.596(10) . ? S31 C33 1.658(10) . ? C32 C39 1.49(12) . ? O34 S35 1.446(10) . ? S35 C37 1.736(10) . ? S35 C36 1.847(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 109.6(2) . . ? O1 C1 C11 106.9(2) . . ? C2 C1 C11 108.5(2) . . ? O1 C1 C7 110.2(2) . 2 ? C2 C1 C7 112.7(2) . 2 ? C11 C1 C7 108.8(2) . 2 ? C7 C2 C3 118.9(3) . . ? C7 C2 C1 123.7(3) . . ? C3 C2 C1 117.4(3) . . ? C4 C3 C2 121.4(3) . . ? C3 C4 C5 119.8(3) . . ? C6 C5 C4 119.7(3) . . ? C5 C6 C7 121.0(3) . . ? C2 C7 C6 119.3(3) . . ? C2 C7 C1 123.5(3) . 2 ? C6 C7 C1 117.2(3) . 2 ? C16 C11 C12 118.1(3) . . ? C16 C11 C1 122.4(3) . . ? C12 C11 C1 119.5(3) . . ? C13 C12 C11 120.9(3) . . ? C12 C13 C14 121.5(3) . . ? C15 C14 C13 117.2(3) . . ? C15 C14 C17 123.4(3) . . ? C13 C14 C17 119.3(3) . . ? C14 C15 C16 121.4(3) . . ? C11 C16 C15 120.9(3) . . ? C19 C17 C18 108.4(4) . . ? C19 C17 C14 112.4(3) . . ? C18 C17 C14 109.8(3) . . ? C19 C17 C20 108.9(4) . . ? C18 C17 C20 109.2(4) . . ? C14 C17 C20 108.0(3) . . ? O21 S22 C24 106.9(2) . . ? O21 S22 C23 105.9(2) . . ? C24 S22 C23 99.9(3) . . ? O25 C26 N27 130.9(12) . . ? C28 N27 C26 99.3(7) . . ? C28 N27 C29 106.4(8) . . ? C26 N27 C29 150.3(12) . . ? C39 S30 O38 110(7) . . ? C39 S30 S31 98(6) . . ? O38 S30 S31 72(4) . . ? C39 S30 C37 108(6) . . ? O38 S30 C37 139(5) . . ? S31 S30 C37 117.4(12) . . ? C39 S30 C32 49(6) . . ? O38 S30 C32 78(5) . . ? S31 S30 C32 53.1(5) . . ? C37 S30 C32 141.3(16) . . ? S30 S31 C32 82.0(7) . . ? S30 S31 C33 74.2(6) . . ? C32 S31 C33 89.2(7) . . ? C39 C32 S31 77(4) . . ? C39 C32 S30 35(5) . . ? S31 C32 S30 44.9(4) . . ? O34 S35 C37 109.1(10) . . ? O34 S35 C36 105.2(9) . . ? C37 S35 C36 100.4(7) . . ? S35 C37 S30 44.5(8) . . ? S30 C39 C32 96(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C7 -126.6(3) . . . . ? C11 C1 C2 C7 117.0(3) . . . . ? C7 C1 C2 C7 -3.5(4) 2 . . . ? O1 C1 C2 C3 55.6(4) . . . . ? C11 C1 C2 C3 -60.8(3) . . . . ? C7 C1 C2 C3 178.7(3) 2 . . . ? C7 C2 C3 C4 -0.9(5) . . . . ? C1 C2 C3 C4 177.0(3) . . . . ? C2 C3 C4 C5 0.3(5) . . . . ? C3 C4 C5 C6 0.6(5) . . . . ? C4 C5 C6 C7 -0.9(5) . . . . ? C3 C2 C7 C6 0.7(4) . . . . ? C1 C2 C7 C6 -177.1(3) . . . . ? C3 C2 C7 C1 -178.3(3) . . . 2 ? C1 C2 C7 C1 3.9(5) . . . 2 ? C5 C6 C7 C2 0.2(5) . . . . ? C5 C6 C7 C1 179.3(3) . . . 2 ? O1 C1 C11 C16 4.5(4) . . . . ? C2 C1 C11 C16 122.6(3) . . . . ? C7 C1 C11 C16 -114.4(3) 2 . . . ? O1 C1 C11 C12 -175.1(3) . . . . ? C2 C1 C11 C12 -57.0(4) . . . . ? C7 C1 C11 C12 66.0(4) 2 . . . ? C16 C11 C12 C13 -0.2(5) . . . . ? C1 C11 C12 C13 179.4(3) . . . . ? C11 C12 C13 C14 0.0(5) . . . . ? C12 C13 C14 C15 -0.4(5) . . . . ? C12 C13 C14 C17 -178.7(3) . . . . ? C13 C14 C15 C16 0.9(5) . . . . ? C17 C14 C15 C16 179.2(3) . . . . ? C12 C11 C16 C15 0.8(5) . . . . ? C1 C11 C16 C15 -178.8(3) . . . . ? C14 C15 C16 C11 -1.2(5) . . . . ? C15 C14 C17 C19 5.9(5) . . . . ? C13 C14 C17 C19 -175.8(4) . . . . ? C15 C14 C17 C18 126.8(4) . . . . ? C13 C14 C17 C18 -55.0(5) . . . . ? C15 C14 C17 C20 -114.3(4) . . . . ? C13 C14 C17 C20 64.0(4) . . . . ? O25 C26 N27 C28 -33(3) . . . . ? O25 C26 N27 C29 117(3) . . . . ? C39 S30 S31 C32 21(6) . . . . ? O38 S30 S31 C32 -88(5) . . . . ? C37 S30 S31 C32 135.2(19) . . . . ? C39 S30 S31 C33 -71(6) . . . . ? O38 S30 S31 C33 -179(5) . . . . ? C37 S30 S31 C33 43.7(19) . . . . ? C32 S30 S31 C33 -91.5(7) . . . . ? S30 S31 C32 C39 -16(5) . . . . ? C33 S31 C32 C39 58(5) . . . . ? C33 S31 C32 S30 74.1(6) . . . . ? O38 S30 C32 C39 -131(9) . . . . ? S31 S30 C32 C39 152(8) . . . . ? C37 S30 C32 C39 63(8) . . . . ? C39 S30 C32 S31 -152(8) . . . . ? O38 S30 C32 S31 77(5) . . . . ? C37 S30 C32 S31 -89(2) . . . . ? O34 S35 C37 S30 -27.7(18) . . . . ? C36 S35 C37 S30 82.5(18) . . . . ? C39 S30 C37 S35 51(7) . . . . ? O38 S30 C37 S35 -152(7) . . . . ? S31 S30 C37 S35 -57.6(13) . . . . ? C32 S30 C37 S35 7(2) . . . . ? O38 S30 C39 C32 52(8) . . . . ? S31 S30 C39 C32 -22(6) . . . . ? C37 S30 C39 C32 -144(4) . . . . ? S31 C32 C39 S30 20(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O21 0.84 1.93 2.753(3) 165.0 . _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.360 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.081 #========================================================END data_c: H.4B _database_code_CSD 175487 _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-9,10-dihydroxy-9,10-bis(p-tert-butylphenyl)-9,10-dihydroanthracene. 4(dimethyl sulfoxide) clathrate ; _chemical_name_common none _chemical_melting_point 278-280 _chemical_formula_moiety 'C34 H36 O2.4(C2 H6 O S)' _chemical_formula_sum 'C42 H60 O6 S4' _chemical_formula_weight 789.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0359(3) _cell_length_b 9.1353(3) _cell_length_c 14.4126(6) _cell_angle_alpha 72.9810(10) _cell_angle_beta 80.0860(10) _cell_angle_gamma 71.631(2) _cell_volume 1075.44(7) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4370 _cell_measurement_theta_min 0.21 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'clear plates' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.218 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 424 _exptl_absorpt_coefficient_mu 0.264 _exptl_absorpt_correction_type none _exptl_special_details ; Unstable without mother liquor under atmospheric conditions. Crystal coated with Paratone oil and data collected at 173K ; _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 'Nonius Kappa CCD' _diffrn_measurement_method 'Combination of phi and omega' _diffrn_reflns_number 6220 _diffrn_reflns_av_R_equivalents 0.0184 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4370 _reflns_number_gt 3683 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 2000)' _computing_cell_refinement 'Collect (Nonius, 2000)' _computing_data_reduction 'Collect (Nonius, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED, a graphical interface to SHELX (1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1723P)^2^+1.1734P] 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_number_reflns 4370 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1003 _refine_ls_R_factor_gt 0.0893 _refine_ls_wR_factor_ref 0.2690 _refine_ls_wR_factor_gt 0.2546 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.806 _refine_ls_shift/su_mean 0.103 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 0.2503(2) -0.2198(2) 0.08247(14) 0.0326(5) Uani 1 1 d . . . H1 H 0.2407 -0.1606 0.1193 0.039 Uiso 1 1 calc R . . C1 C 0.1537(3) -0.1353(3) 0.00402(18) 0.0258(5) Uani 1 1 d . . . C2 C -0.0081(3) -0.1631(3) 0.03164(19) 0.0267(5) Uani 1 1 d . . . C3 C -0.0146(3) -0.3226(3) 0.0619(2) 0.0352(6) Uani 1 1 d . . . H3 H 0.0800 -0.4068 0.0672 0.042 Uiso 1 1 calc R . . C4 C -0.1560(4) -0.3580(4) 0.0840(2) 0.0412(7) Uani 1 1 d . . . H4 H -0.1585 -0.4660 0.1038 0.049 Uiso 1 1 calc R . . C5 C -0.2953(4) -0.2353(4) 0.0773(2) 0.0395(7) Uani 1 1 d . . . H5 H -0.3931 -0.2590 0.0919 0.047 Uiso 1 1 calc R . . C6 C -0.2901(3) -0.0792(3) 0.0492(2) 0.0335(6) Uani 1 1 d . . . H6 H -0.3854 0.0042 0.0457 0.040 Uiso 1 1 calc R . . C7 C -0.1471(3) -0.0405(3) 0.02560(18) 0.0263(5) Uani 1 1 d . . . C11 C 0.2309(3) -0.2072(3) -0.08237(19) 0.0262(5) Uani 1 1 d . . . C12 C 0.3746(3) -0.3229(3) -0.0786(2) 0.0307(6) Uani 1 1 d . . . H12 H 0.4288 -0.3582 -0.0217 0.037 Uiso 1 1 calc R . . C13 C 0.4403(3) -0.3880(3) -0.1586(2) 0.0333(6) Uani 1 1 d . . . H13 H 0.5376 -0.4685 -0.1540 0.040 Uiso 1 1 calc R . . C14 C 0.3666(3) -0.3376(3) -0.2438(2) 0.0329(6) Uani 1 1 d . . . C15 C 0.2221(3) -0.2195(4) -0.2467(2) 0.0364(6) Uani 1 1 d . . . H15 H 0.1688 -0.1821 -0.3042 0.044 Uiso 1 1 calc R . . C16 C 0.1555(3) -0.1563(3) -0.1676(2) 0.0329(6) Uani 1 1 d . . . H16 H 0.0572 -0.0773 -0.1716 0.039 Uiso 1 1 calc R . . C17 C 0.4314(4) -0.4066(4) -0.3322(2) 0.0440(8) Uani 1 1 d . . . C18 C 0.3214(6) -0.4937(5) -0.3463(3) 0.0628(11) Uani 1 1 d . . . H18A H 0.2167 -0.4192 -0.3557 0.094 Uiso 1 1 calc R . . H18B H 0.3158 -0.5817 -0.2886 0.094 Uiso 1 1 calc R . . H18C H 0.3609 -0.5361 -0.4037 0.094 Uiso 1 1 calc R . . C19 C 0.4431(6) -0.2716(5) -0.4240(3) 0.0632(11) Uani 1 1 d . . . H19A H 0.4830 -0.3165 -0.4804 0.095 Uiso 1 1 calc R . . H19B H 0.5146 -0.2160 -0.4154 0.095 Uiso 1 1 calc R . . H19C H 0.3392 -0.1960 -0.4347 0.095 Uiso 1 1 calc R . . C20 C 0.5944(6) -0.5233(6) -0.3201(3) 0.0765(15) Uani 1 1 d . . . H20A H 0.6289 -0.5687 -0.3766 0.115 Uiso 1 1 calc R . . H20B H 0.5912 -0.6092 -0.2608 0.115 Uiso 1 1 calc R . . H20C H 0.6677 -0.4671 -0.3151 0.115 Uiso 1 1 calc R . . O21 O 0.2147(3) -0.0566(3) 0.22277(19) 0.0485(6) Uani 1 1 d . . . S22 S 0.32340(10) 0.04812(11) 0.19493(7) 0.0450(4) Uani 0.933(5) 1 d P . . S23 S 0.245(5) 0.039(6) 0.296(3) 0.153(16) Uiso 0.067(5) 1 d P . . C24 C 0.2026(6) 0.2404(5) 0.2002(5) 0.0828(17) Uani 1 1 d . . . C25 C 0.4316(6) 0.0012(6) 0.2966(4) 0.0758(14) Uani 1 1 d . . . O26 O 0.1356(11) 0.2440(13) -0.4262(8) 0.083(3) Uiso 0.424(7) 1 d P . . S27 S 0.1022(5) 0.1504(6) -0.4544(4) 0.121(2) Uani 0.424(7) 1 d P . . C28 C 0.118(2) 0.239(3) -0.5679(16) 0.119(6) Uiso 0.424(7) 1 d P . . C29 C -0.030(6) 0.118(5) -0.439(3) 0.377(19) Uiso 1 1 d . . . O30 O 0.129(2) 0.309(3) -0.4999(16) 0.213(7) Uiso 0.576(7) 1 d P . . S31 S -0.0492(18) 0.271(3) -0.4577(9) 0.365(12) Uani 0.576(7) 1 d P . . C32 C 0.0565(16) 0.2676(17) -0.3277(11) 0.112(4) Uiso 0.576(7) 1 d P . . 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 0.0340(10) 0.0303(9) 0.0308(10) -0.0111(8) -0.0066(8) -0.0005(7) C1 0.0245(11) 0.0242(11) 0.0266(12) -0.0091(10) -0.0001(9) -0.0026(9) C2 0.0301(12) 0.0232(11) 0.0263(12) -0.0086(9) 0.0029(9) -0.0074(9) C3 0.0394(14) 0.0227(12) 0.0388(15) -0.0079(11) 0.0049(11) -0.0066(10) C4 0.0479(17) 0.0304(13) 0.0463(18) -0.0123(13) 0.0092(13) -0.0171(12) C5 0.0383(15) 0.0420(16) 0.0431(17) -0.0142(13) 0.0072(12) -0.0206(12) C6 0.0294(13) 0.0348(13) 0.0364(15) -0.0129(11) 0.0034(10) -0.0089(10) C7 0.0277(12) 0.0258(12) 0.0260(12) -0.0102(10) 0.0010(9) -0.0069(9) C11 0.0247(11) 0.0240(11) 0.0288(13) -0.0098(10) 0.0012(9) -0.0044(9) C12 0.0274(12) 0.0279(12) 0.0349(14) -0.0116(11) -0.0022(10) -0.0020(9) C13 0.0310(13) 0.0267(12) 0.0399(15) -0.0151(11) 0.0028(11) -0.0021(10) C14 0.0381(14) 0.0291(12) 0.0325(14) -0.0122(11) 0.0042(11) -0.0107(10) C15 0.0366(14) 0.0408(15) 0.0311(14) -0.0143(12) -0.0020(11) -0.0057(11) C16 0.0295(12) 0.0350(13) 0.0308(14) -0.0122(11) -0.0011(10) -0.0017(10) C17 0.0514(18) 0.0418(16) 0.0391(16) -0.0234(14) 0.0072(13) -0.0075(13) C18 0.088(3) 0.066(2) 0.049(2) -0.035(2) 0.0080(19) -0.032(2) C19 0.084(3) 0.063(2) 0.0395(19) -0.0233(18) 0.0223(18) -0.022(2) C20 0.074(3) 0.081(3) 0.062(3) -0.048(2) 0.002(2) 0.018(2) O21 0.0497(13) 0.0463(13) 0.0575(15) -0.0215(11) -0.0118(11) -0.0129(10) S22 0.0361(5) 0.0543(6) 0.0458(6) -0.0172(4) -0.0016(3) -0.0111(4) C24 0.058(2) 0.040(2) 0.151(5) -0.022(3) -0.019(3) -0.0120(17) C25 0.085(3) 0.067(3) 0.090(3) -0.013(2) -0.047(3) -0.027(2) S27 0.067(2) 0.100(3) 0.151(5) -0.013(3) 0.017(2) 0.008(2) S31 0.264(13) 0.46(2) 0.236(11) -0.109(13) -0.068(9) 0.135(15) _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 1.428(3) . ? C1 C7 1.521(3) 2 ? C1 C2 1.528(3) . ? C1 C11 1.536(3) . ? C2 C7 1.390(3) . ? C2 C3 1.410(4) . ? C3 C4 1.379(4) . ? C4 C5 1.392(4) . ? C5 C6 1.377(4) . ? C6 C7 1.406(4) . ? C7 C1 1.521(3) 2 ? C11 C12 1.390(3) . ? C11 C16 1.395(4) . ? C12 C13 1.405(4) . ? C13 C14 1.387(4) . ? C14 C15 1.406(4) . ? C14 C17 1.530(4) . ? C15 C16 1.388(4) . ? C17 C18 1.525(5) . ? C17 C20 1.525(5) . ? C17 C19 1.537(6) . ? O21 S22 1.508(3) . ? O21 S23 1.65(4) . ? S22 S23 1.50(5) . ? S22 C24 1.767(4) . ? S22 C25 1.775(4) . ? S23 C25 1.61(5) . ? S23 C24 1.92(5) . ? O26 O30 1.06(2) . ? O26 S27 1.181(10) . ? O26 C32 1.519(17) . ? O26 S31 1.73(2) . ? S27 S31 1.457(11) . ? S27 C29 1.29(4) . ? S27 O30 1.48(2) . ? S27 C28 1.60(2) . ? C28 O30 1.35(2) . ? C28 S31 2.01(3) . ? C29 S31 1.30(4) . ? O30 S31 1.73(3) . ? S31 C32 2.24(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 O1 C1 C7 110.63(19) . 2 ? O1 C1 C2 109.9(2) . . ? C7 C1 C2 112.89(19) 2 . ? O1 C1 C11 106.67(18) . . ? C7 C1 C11 108.5(2) 2 . ? C2 C1 C11 108.01(19) . . ? C7 C2 C3 119.1(2) . . ? C7 C2 C1 123.5(2) . . ? C3 C2 C1 117.3(2) . . ? C4 C3 C2 121.0(3) . . ? C3 C4 C5 119.9(3) . . ? C6 C5 C4 119.5(3) . . ? C5 C6 C7 121.4(3) . . ? C2 C7 C6 119.0(2) . . ? C2 C7 C1 123.5(2) . 2 ? C6 C7 C1 117.5(2) . 2 ? C12 C11 C16 118.3(2) . . ? C12 C11 C1 122.1(2) . . ? C16 C11 C1 119.6(2) . . ? C11 C12 C13 120.5(2) . . ? C14 C13 C12 121.7(2) . . ? C13 C14 C15 117.1(2) . . ? C13 C14 C17 123.8(3) . . ? C15 C14 C17 119.1(3) . . ? C16 C15 C14 121.5(3) . . ? C15 C16 C11 120.9(2) . . ? C18 C17 C20 108.7(3) . . ? C18 C17 C14 109.0(3) . . ? C20 C17 C14 112.2(3) . . ? C18 C17 C19 109.2(3) . . ? C20 C17 C19 107.6(3) . . ? C14 C17 C19 110.0(3) . . ? S22 O21 S23 56.2(17) . . ? O21 S22 S23 66.9(17) . . ? O21 S22 C24 105.14(19) . . ? S23 S22 C24 71.4(18) . . ? O21 S22 C25 106.6(2) . . ? S23 S22 C25 58.4(18) . . ? C24 S22 C25 99.9(3) . . ? S22 S23 C25 69(2) . . ? S22 S23 O21 56.9(16) . . ? C25 S23 O21 108(3) . . ? S22 S23 C24 60.9(17) . . ? C25 S23 C24 100(2) . . ? O21 S23 C24 93(2) . . ? S22 C24 S23 47.7(14) . . ? S23 C25 S22 52.1(17) . . ? O30 O26 S27 83.0(13) . . ? O30 O26 C32 137.4(16) . . ? S27 O26 C32 115.7(10) . . ? O30 O26 S31 72.1(13) . . ? S27 O26 S31 56.3(8) . . ? C32 O26 S31 86.7(8) . . ? O26 S27 S31 81.2(11) . . ? O26 S27 C29 127.5(18) . . ? S31 S27 C29 56.2(15) . . ? O26 S27 O30 44.9(8) . . ? S31 S27 O30 72.0(12) . . ? C29 S27 O30 127(2) . . ? O26 S27 C28 96.2(10) . . ? S31 S27 C28 82.1(10) . . ? C29 S27 C28 106(2) . . ? O30 S27 C28 51.8(9) . . ? O30 C28 S27 59.6(14) . . ? O30 C28 S31 57.9(13) . . ? S27 C28 S31 45.8(7) . . ? S31 C29 S27 69(2) . . ? O26 O30 C28 120(2) . . ? O26 O30 S27 52.1(11) . . ? C28 O30 S27 68.6(14) . . ? O26 O30 S31 72.3(14) . . ? C28 O30 S31 80.6(14) . . ? S27 O30 S31 53.3(9) . . ? C29 S31 S27 55.2(19) . . ? C29 S31 O30 109(3) . . ? S27 S31 O30 54.8(9) . . ? C29 S31 O26 93(2) . . ? S27 S31 O26 42.4(6) . . ? O30 S31 O26 35.5(8) . . ? C29 S31 C28 86(2) . . ? S27 S31 C28 52.1(8) . . ? O30 S31 C28 41.5(8) . . ? O26 S31 C28 67.4(9) . . ? C29 S31 C32 97.4(19) . . ? S27 S31 C32 73.4(7) . . ? O30 S31 C32 73.4(11) . . ? O26 S31 C32 42.7(6) . . ? C28 S31 C32 110.1(11) . . ? O26 C32 S31 50.6(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C7 127.1(2) . . . . ? C7 C1 C2 C7 3.1(4) 2 . . . ? C11 C1 C2 C7 -116.9(3) . . . . ? O1 C1 C2 C3 -54.9(3) . . . . ? C7 C1 C2 C3 -178.9(2) 2 . . . ? C11 C1 C2 C3 61.2(3) . . . . ? C7 C2 C3 C4 1.0(4) . . . . ? C1 C2 C3 C4 -177.1(3) . . . . ? C2 C3 C4 C5 -0.5(5) . . . . ? C3 C4 C5 C6 -0.5(5) . . . . ? C4 C5 C6 C7 1.0(5) . . . . ? C3 C2 C7 C6 -0.5(4) . . . . ? C1 C2 C7 C6 177.5(2) . . . . ? C3 C2 C7 C1 178.6(2) . . . 2 ? C1 C2 C7 C1 -3.4(4) . . . 2 ? C5 C6 C7 C2 -0.5(4) . . . . ? C5 C6 C7 C1 -179.7(2) . . . 2 ? O1 C1 C11 C12 -4.7(3) . . . . ? C7 C1 C11 C12 114.5(3) 2 . . . ? C2 C1 C11 C12 -122.9(3) . . . . ? O1 C1 C11 C16 175.0(2) . . . . ? C7 C1 C11 C16 -65.8(3) 2 . . . ? C2 C1 C11 C16 56.9(3) . . . . ? C16 C11 C12 C13 -0.9(4) . . . . ? C1 C11 C12 C13 178.8(2) . . . . ? C11 C12 C13 C14 1.3(4) . . . . ? C12 C13 C14 C15 -0.7(4) . . . . ? C12 C13 C14 C17 -178.8(3) . . . . ? C13 C14 C15 C16 -0.2(4) . . . . ? C17 C14 C15 C16 178.0(3) . . . . ? C14 C15 C16 C11 0.6(5) . . . . ? C12 C11 C16 C15 0.0(4) . . . . ? C1 C11 C16 C15 -179.7(3) . . . . ? C13 C14 C17 C18 114.1(4) . . . . ? C15 C14 C17 C18 -64.0(4) . . . . ? C13 C14 C17 C20 -6.3(5) . . . . ? C15 C14 C17 C20 175.5(4) . . . . ? C13 C14 C17 C19 -126.1(3) . . . . ? C15 C14 C17 C19 55.7(4) . . . . ? S23 O21 S22 C24 -62(2) . . . . ? S23 O21 S22 C25 43.8(19) . . . . ? O21 S22 S23 C25 128.8(17) . . . . ? C24 S22 S23 C25 -114.8(15) . . . . ? C24 S22 S23 O21 116.3(12) . . . . ? C25 S22 S23 O21 -128.8(17) . . . . ? O21 S22 S23 C24 -116.3(12) . . . . ? C25 S22 S23 C24 114.8(15) . . . . ? S22 O21 S23 C25 -49.9(19) . . . . ? S22 O21 S23 C24 51.7(13) . . . . ? O21 S22 C24 S23 58.6(18) . . . . ? C25 S22 C24 S23 -51.7(18) . . . . ? C25 S23 C24 S22 59.6(17) . . . . ? O21 S23 C24 S22 -48.8(13) . . . . ? O21 S23 C25 S22 43.2(16) . . . . ? C24 S23 C25 S22 -53.6(15) . . . . ? O21 S22 C25 S23 -48(2) . . . . ? C24 S22 C25 S23 61(2) . . . . ? O30 O26 S27 S31 -73.2(13) . . . . ? C32 O26 S27 S31 66.6(11) . . . . ? O30 O26 S27 C29 -107(3) . . . . ? C32 O26 S27 C29 32(3) . . . . ? S31 O26 S27 C29 -34(2) . . . . ? C32 O26 S27 O30 139.7(18) . . . . ? S31 O26 S27 O30 73.2(13) . . . . ? O30 O26 S27 C28 7.8(16) . . . . ? C32 O26 S27 C28 147.6(11) . . . . ? S31 O26 S27 C28 81.0(11) . . . . ? O26 S27 C28 O30 -7.0(14) . . . . ? S31 S27 C28 O30 73.2(14) . . . . ? C29 S27 C28 O30 125(2) . . . . ? O26 S27 C28 S31 -80.2(12) . . . . ? C29 S27 C28 S31 51.5(16) . . . . ? O30 S27 C28 S31 -73.2(14) . . . . ? O26 S27 C29 S31 42(3) . . . . ? O30 S27 C29 S31 -15(3) . . . . ? C28 S27 C29 S31 -69.0(17) . . . . ? S27 O26 O30 C28 -11(2) . . . . ? C32 O26 O30 C28 -131(2) . . . . ? S31 O26 O30 C28 -68(2) . . . . ? C32 O26 O30 S27 -121(2) . . . . ? S31 O26 O30 S27 -56.8(8) . . . . ? S27 O26 O30 S31 56.8(8) . . . . ? C32 O26 O30 S31 -64(2) . . . . ? S27 C28 O30 O26 9.1(19) . . . . ? S31 C28 O30 O26 63(2) . . . . ? S31 C28 O30 S27 54.1(8) . . . . ? S27 C28 O30 S31 -54.1(8) . . . . ? S31 S27 O30 O26 95.8(14) . . . . ? C29 S27 O30 O26 109(2) . . . . ? C28 S27 O30 O26 -170(2) . . . . ? O26 S27 O30 C28 170(2) . . . . ? S31 S27 O30 C28 -94.2(13) . . . . ? C29 S27 O30 C28 -81(3) . . . . ? O26 S27 O30 S31 -95.8(14) . . . . ? C29 S27 O30 S31 13(3) . . . . ? C28 S27 O30 S31 94.2(13) . . . . ? S27 C29 S31 O30 11(2) . . . . ? S27 C29 S31 O26 -21.2(14) . . . . ? S27 C29 S31 C28 45.9(13) . . . . ? S27 C29 S31 C32 -63.8(15) . . . . ? O26 S27 S31 C29 -148(2) . . . . ? O30 S27 S31 C29 167(2) . . . . ? C28 S27 S31 C29 115(2) . . . . ? O26 S27 S31 O30 45.2(9) . . . . ? C29 S27 S31 O30 -167(2) . . . . ? C28 S27 S31 O30 -52.3(10) . . . . ? C29 S27 S31 O26 148(2) . . . . ? O30 S27 S31 O26 -45.2(9) . . . . ? C28 S27 S31 O26 -97.5(10) . . . . ? O26 S27 S31 C28 97.5(10) . . . . ? C29 S27 S31 C28 -115(2) . . . . ? O30 S27 S31 C28 52.3(10) . . . . ? O26 S27 S31 C32 -35.9(8) . . . . ? C29 S27 S31 C32 112(2) . . . . ? O30 S27 S31 C32 -81.2(11) . . . . ? C28 S27 S31 C32 -133.4(10) . . . . ? O26 O30 S31 C29 -67(2) . . . . ? C28 O30 S31 C29 59(3) . . . . ? S27 O30 S31 C29 -11(2) . . . . ? O26 O30 S31 S27 -55.5(11) . . . . ? C28 O30 S31 S27 70.3(13) . . . . ? C28 O30 S31 O26 126(2) . . . . ? S27 O30 S31 O26 55.5(11) . . . . ? O26 O30 S31 C28 -126(2) . . . . ? S27 O30 S31 C28 -70.3(13) . . . . ? O26 O30 S31 C32 25.6(11) . . . . ? C28 O30 S31 C32 151.4(15) . . . . ? S27 O30 S31 C32 81.1(8) . . . . ? O30 O26 S31 C29 120(2) . . . . ? S27 O26 S31 C29 26.1(19) . . . . ? C32 O26 S31 C29 -98(2) . . . . ? O30 O26 S31 S27 93.5(14) . . . . ? C32 O26 S31 S27 -124.1(11) . . . . ? S27 O26 S31 O30 -93.5(14) . . . . ? C32 O26 S31 O30 142.5(17) . . . . ? O30 O26 S31 C28 35.6(14) . . . . ? S27 O26 S31 C28 -57.9(8) . . . . ? C32 O26 S31 C28 178.0(11) . . . . ? O30 O26 S31 C32 -142.5(17) . . . . ? S27 O26 S31 C32 124.1(11) . . . . ? O30 C28 S31 C29 -126(3) . . . . ? S27 C28 S31 C29 -48.4(19) . . . . ? O30 C28 S31 S27 -77.1(15) . . . . ? S27 C28 S31 O30 77.1(15) . . . . ? O30 C28 S31 O26 -30.7(13) . . . . ? S27 C28 S31 O26 46.4(6) . . . . ? O30 C28 S31 C32 -29.3(16) . . . . ? S27 C28 S31 C32 47.8(9) . . . . ? O30 O26 C32 S31 59(2) . . . . ? S27 O26 C32 S31 -49.9(10) . . . . ? C29 S31 C32 O26 86(2) . . . . ? S27 S31 C32 O26 35.7(8) . . . . ? O30 S31 C32 O26 -21.7(9) . . . . ? C28 S31 C32 O26 -1.9(11) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O21 0.84 1.94 2.766(3) 169.8 . _diffrn_measured_fraction_theta_max 0.887 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.887 _refine_diff_density_max 0.750 _refine_diff_density_min -0.710 _refine_diff_density_rms 0.077 #========================================================END data_c: H.4C _database_code_CSD 175488 _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-9,10-dihydroxy-9,10-bis(p-tert-butylphenyl)-9,10-dihydroanthracene. 4(acetone) clathrate ; _chemical_name_common none _chemical_melting_point 286-288 _chemical_formula_moiety 'C34 H36 O2.4(C3 H6 O)' _chemical_formula_sum 'C46 H60 O6' _chemical_formula_weight 708.94 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 monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.9057(2) _cell_length_b 26.9049(6) _cell_length_c 9.1615(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.5900(10) _cell_angle_gamma 90.00 _cell_volume 2080.62(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3933 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 25.70 _exptl_crystal_description 'clear elongated plates' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.132 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type none _exptl_special_details ; Unstable without mother liquor under atmospheric conditions. Crystal coated with Paratone oil and data collected at 173K. ; _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 'Nonius Kappa CCD' _diffrn_measurement_method 'combinaton of phi and omega' _diffrn_reflns_number 11359 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0593 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 25.70 _reflns_number_total 3911 _reflns_number_gt 2328 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 2000)' _computing_cell_refinement 'Collect (Nonius, 2000)' _computing_data_reduction 'Collect (Nonius, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED, a graphical interface to SHELX (1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1382P)^2^+0.5206P] 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_number_reflns 3911 _refine_ls_number_parameters 267 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1126 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.2069 _refine_ls_wR_factor_gt 0.1679 _refine_ls_goodness_of_fit_ref 0.917 _refine_ls_restrained_S_all 0.917 _refine_ls_shift/su_max 0.597 _refine_ls_shift/su_mean 0.049 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 -0.26417(17) 0.95768(6) 0.31034(18) 0.0329(4) Uani 1 1 d . . . H1 H -0.2320 0.9327 0.3666 0.040 Uiso 1 1 calc R . . C1 C -0.1549(2) 0.99825(8) 0.3647(3) 0.0262(5) Uani 1 1 d . . . C2 C -0.1468(3) 1.01184(9) 0.5289(3) 0.0273(5) Uani 1 1 d . . . C3 C -0.2892(3) 1.02257(9) 0.5562(3) 0.0336(6) Uani 1 1 d . . . H3 H -0.3861 1.0200 0.4740 0.040 Uiso 1 1 calc R . . C4 C -0.2919(3) 1.03670(10) 0.6995(3) 0.0378(6) Uani 1 1 d . . . H4 H -0.3898 1.0441 0.7155 0.045 Uiso 1 1 calc R . . C5 C -0.1518(3) 1.04008(10) 0.8203(3) 0.0388(6) Uani 1 1 d . . . H5 H -0.1528 1.0498 0.9197 0.047 Uiso 1 1 calc R . . C6 C -0.0109(3) 1.02932(9) 0.7957(3) 0.0341(6) Uani 1 1 d . . . H6 H 0.0850 1.0316 0.8792 0.041 Uiso 1 1 calc R . . C7 C -0.0052(2) 1.01505(8) 0.6501(2) 0.0265(5) Uani 1 1 d . . . C11 C -0.2220(2) 1.04268(8) 0.2594(3) 0.0250(5) Uani 1 1 d . . . C12 C -0.3664(3) 1.04132(9) 0.1424(3) 0.0284(6) Uani 1 1 d . . . H12 H -0.4294 1.0121 0.1264 0.034 Uiso 1 1 calc R . . C13 C -0.4195(3) 1.08261(9) 0.0482(3) 0.0305(6) Uani 1 1 d . . . H13 H -0.5181 1.0807 -0.0320 0.037 Uiso 1 1 calc R . . C14 C -0.3326(3) 1.12656(9) 0.0681(3) 0.0294(6) Uani 1 1 d . . . C15 C -0.1885(3) 1.12701(9) 0.1865(3) 0.0360(6) Uani 1 1 d . . . H15 H -0.1255 1.1562 0.2040 0.043 Uiso 1 1 calc R . . C16 C -0.1348(3) 1.08593(9) 0.2795(3) 0.0345(6) Uani 1 1 d . . . H16 H -0.0356 1.0876 0.3589 0.041 Uiso 1 1 calc R . . C17 C -0.3876(3) 1.17177(9) -0.0347(3) 0.0393(7) Uani 1 1 d . . . C18 C -0.4128(17) 1.1581(4) -0.2099(12) 0.068(3) Uani 0.29 1 d P . . C19 C -0.5527(6) 1.16663(17) -0.1439(6) 0.0598(13) Uani 0.71 1 d P . . C20 C -0.5675(18) 1.1871(7) -0.042(2) 0.107(6) Uani 0.29 1 d P . . C21 C -0.3760(6) 1.21834(15) 0.0672(5) 0.0566(12) Uani 0.71 1 d P . . C22 C -0.2749(16) 1.2176(4) -0.0001(17) 0.080(4) Uani 0.29 1 d P . . C23 C -0.2709(6) 1.17791(18) -0.1290(5) 0.0601(12) Uani 0.71 1 d P . . O24 O -0.1735(2) 0.86404(7) 0.4590(2) 0.0475(5) Uani 1 1 d . . . C25 C -0.0970(3) 0.82928(11) 0.4373(3) 0.0477(7) Uani 1 1 d . . . C26 C 0.0082(5) 0.83479(16) 0.3428(6) 0.0976(14) Uani 1 1 d . . . H26A H 0.0044 0.8692 0.3068 0.146 Uiso 1 1 calc R . . H26B H -0.0268 0.8124 0.2540 0.146 Uiso 1 1 calc R . . H26C H 0.1169 0.8264 0.4048 0.146 Uiso 1 1 calc R . . C27 C -0.1021(5) 0.77951(11) 0.5080(4) 0.0728(10) Uani 1 1 d . . . H27A H -0.1604 0.7821 0.5820 0.109 Uiso 1 1 calc R . . H27B H 0.0062 0.7682 0.5611 0.109 Uiso 1 1 calc R . . H27C H -0.1553 0.7557 0.4272 0.109 Uiso 1 1 calc R . . O28 O -0.7268(5) 1.18454(12) 0.2216(4) 0.1377(15) Uani 1 1 d . . . C29 C -0.6803(5) 1.14322(14) 0.2599(4) 0.0691(10) Uani 1 1 d . . . C30 C -0.7681(4) 1.09839(16) 0.1829(5) 0.0850(12) Uani 1 1 d . . . H30A H -0.8624 1.1086 0.0991 0.127 Uiso 1 1 calc R . . H30B H -0.8002 1.0787 0.2579 0.127 Uiso 1 1 calc R . . H30C H -0.6995 1.0783 0.1411 0.127 Uiso 1 1 calc R . . C31 C -0.5328(5) 1.13502(15) 0.3863(5) 0.0798(11) Uani 1 1 d . . . H31A H -0.4518 1.1220 0.3449 0.120 Uiso 1 1 calc R . . H31B H -0.5515 1.1110 0.4590 0.120 Uiso 1 1 calc R . . H31C H -0.4965 1.1665 0.4394 0.120 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 0.0328(9) 0.0273(10) 0.0337(10) 0.0019(7) 0.0036(7) -0.0055(7) C1 0.0240(11) 0.0266(13) 0.0258(13) -0.0016(10) 0.0046(10) -0.0033(9) C2 0.0300(12) 0.0259(13) 0.0270(13) 0.0052(10) 0.0104(10) 0.0013(10) C3 0.0286(12) 0.0400(15) 0.0322(14) 0.0048(11) 0.0098(10) 0.0013(11) C4 0.0370(14) 0.0420(16) 0.0398(16) 0.0047(12) 0.0200(12) 0.0070(11) C5 0.0487(15) 0.0411(16) 0.0311(14) -0.0004(12) 0.0191(12) 0.0070(12) C6 0.0374(13) 0.0360(15) 0.0267(13) -0.0007(11) 0.0071(11) 0.0036(11) C7 0.0285(12) 0.0277(13) 0.0232(12) 0.0021(10) 0.0078(10) -0.0008(9) C11 0.0253(11) 0.0280(13) 0.0219(12) -0.0013(10) 0.0078(9) -0.0003(9) C12 0.0280(12) 0.0276(13) 0.0275(13) -0.0012(10) 0.0058(10) -0.0025(10) C13 0.0297(12) 0.0339(14) 0.0254(12) -0.0020(10) 0.0054(10) 0.0011(10) C14 0.0334(13) 0.0296(14) 0.0266(13) -0.0013(10) 0.0114(10) 0.0018(10) C15 0.0360(13) 0.0293(14) 0.0379(15) -0.0016(11) 0.0052(11) -0.0078(11) C16 0.0279(12) 0.0360(15) 0.0329(14) 0.0029(11) 0.0002(10) -0.0039(11) C17 0.0483(15) 0.0324(15) 0.0340(15) 0.0032(11) 0.0084(12) 0.0002(12) C18 0.121(11) 0.054(7) 0.033(6) 0.016(5) 0.029(7) 0.008(7) C19 0.056(3) 0.051(3) 0.057(3) 0.020(2) -0.004(2) 0.005(2) C20 0.103(10) 0.136(13) 0.119(12) 0.086(11) 0.088(10) 0.102(10) C21 0.079(3) 0.027(2) 0.055(3) -0.0019(19) 0.009(3) 0.005(2) C22 0.089(9) 0.033(7) 0.097(10) 0.024(7) -0.001(8) -0.023(6) C23 0.076(3) 0.056(3) 0.057(3) 0.019(2) 0.033(3) 0.000(2) O24 0.0476(11) 0.0340(11) 0.0532(12) -0.0022(9) 0.0049(9) -0.0002(9) C25 0.0501(16) 0.0383(17) 0.0462(17) -0.0065(13) 0.0034(14) -0.0034(13) C26 0.120(3) 0.069(3) 0.132(4) 0.006(3) 0.080(3) 0.013(2) C27 0.098(3) 0.0347(19) 0.084(3) 0.0020(17) 0.027(2) 0.0046(17) O28 0.237(4) 0.070(2) 0.110(3) 0.0405(19) 0.061(3) 0.062(2) C29 0.097(3) 0.057(2) 0.068(2) 0.0154(19) 0.046(2) 0.015(2) C30 0.075(2) 0.090(3) 0.102(3) -0.011(2) 0.045(2) -0.008(2) C31 0.085(3) 0.084(3) 0.074(3) -0.004(2) 0.030(2) 0.006(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 1.441(3) . ? C1 C7 1.517(3) 3_576 ? C1 C11 1.533(3) . ? C1 C2 1.527(3) . ? C2 C7 1.392(3) . ? C2 C3 1.399(3) . ? C3 C4 1.374(4) . ? C4 C5 1.382(4) . ? C5 C6 1.375(3) . ? C6 C7 1.405(3) . ? C7 C1 1.517(3) 3_576 ? C11 C16 1.378(3) . ? C11 C12 1.387(3) . ? C12 C13 1.394(3) . ? C13 C14 1.393(3) . ? C14 C15 1.391(3) . ? C14 C17 1.521(3) . ? C15 C16 1.384(3) . ? C17 C19 1.498(5) . ? C17 C22 1.556(11) . ? C17 C21 1.546(5) . ? C17 C23 1.557(5) . ? C17 C18 1.591(11) . ? C17 C20 1.636(11) . ? C18 C23 1.354(14) . ? C18 C19 1.566(14) . ? C19 C20 1.129(18) . ? C20 C21 1.88(2) . ? C21 C22 1.243(16) . ? C22 C23 1.600(17) . ? O24 C25 1.211(3) . ? C25 C26 1.471(5) . ? C25 C27 1.494(4) . ? O28 C29 1.199(4) . ? C29 C31 1.465(5) . ? C29 C30 1.487(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 O1 C1 C7 109.92(18) . 3_576 ? O1 C1 C11 106.74(17) . . ? C7 C1 C11 108.47(18) 3_576 . ? O1 C1 C2 109.65(17) . . ? C7 C1 C2 113.19(18) 3_576 . ? C11 C1 C2 108.65(18) . . ? C7 C2 C3 119.2(2) . . ? C7 C2 C1 123.12(19) . . ? C3 C2 C1 117.7(2) . . ? C4 C3 C2 121.4(2) . . ? C3 C4 C5 119.8(2) . . ? C6 C5 C4 119.6(2) . . ? C5 C6 C7 121.6(2) . . ? C2 C7 C6 118.5(2) . . ? C2 C7 C1 123.5(2) . 3_576 ? C6 C7 C1 117.93(19) . 3_576 ? C16 C11 C12 118.0(2) . . ? C16 C11 C1 118.96(19) . . ? C12 C11 C1 123.0(2) . . ? C11 C12 C13 120.3(2) . . ? C14 C13 C12 122.1(2) . . ? C15 C14 C13 116.4(2) . . ? C15 C14 C17 120.7(2) . . ? C13 C14 C17 122.8(2) . . ? C16 C15 C14 121.7(2) . . ? C11 C16 C15 121.5(2) . . ? C19 C17 C14 113.2(2) . . ? C19 C17 C22 129.9(5) . . ? C14 C17 C22 116.6(5) . . ? C19 C17 C21 109.9(3) . . ? C14 C17 C21 109.1(2) . . ? C22 C17 C21 47.2(6) . . ? C19 C17 C23 109.1(3) . . ? C14 C17 C23 106.7(2) . . ? C22 C17 C23 61.8(7) . . ? C21 C17 C23 108.7(3) . . ? C19 C17 C18 60.8(6) . . ? C14 C17 C18 110.7(5) . . ? C22 C17 C18 105.2(8) . . ? C21 C17 C18 139.2(5) . . ? C23 C17 C18 50.9(5) . . ? C19 C17 C20 41.9(7) . . ? C14 C17 C20 110.2(5) . . ? C22 C17 C20 111.6(10) . . ? C21 C17 C20 72.3(9) . . ? C23 C17 C20 140.3(5) . . ? C18 C17 C20 101.3(9) . . ? C23 C18 C19 116.8(8) . . ? C23 C18 C17 63.3(5) . . ? C19 C18 C17 56.7(4) . . ? C20 C19 C17 75.6(9) . . ? C20 C19 C18 135.1(11) . . ? C17 C19 C18 62.5(5) . . ? C19 C20 C17 62.5(5) . . ? C19 C20 C21 109.5(9) . . ? C17 C20 C21 51.7(5) . . ? C22 C21 C17 66.8(6) . . ? C22 C21 C20 114.0(8) . . ? C17 C21 C20 56.1(5) . . ? C21 C22 C17 65.9(6) . . ? C21 C22 C23 124.6(8) . . ? C17 C22 C23 59.1(5) . . ? C18 C23 C17 65.8(5) . . ? C18 C23 C22 115.4(8) . . ? C17 C23 C22 59.1(5) . . ? O24 C25 C26 121.1(3) . . ? O24 C25 C27 121.7(3) . . ? C26 C25 C27 117.2(3) . . ? O28 C29 C31 120.7(4) . . ? O28 C29 C30 122.2(4) . . ? C31 C29 C30 117.1(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C7 127.4(2) . . . . ? C7 C1 C2 C7 4.3(3) 3_576 . . . ? C11 C1 C2 C7 -116.3(2) . . . . ? O1 C1 C2 C3 -54.1(3) . . . . ? C7 C1 C2 C3 -177.2(2) 3_576 . . . ? C11 C1 C2 C3 62.2(3) . . . . ? C7 C2 C3 C4 0.7(4) . . . . ? C1 C2 C3 C4 -177.8(2) . . . . ? C2 C3 C4 C5 -0.6(4) . . . . ? C3 C4 C5 C6 0.1(4) . . . . ? C4 C5 C6 C7 0.2(4) . . . . ? C3 C2 C7 C6 -0.4(3) . . . . ? C1 C2 C7 C6 178.1(2) . . . . ? C3 C2 C7 C1 176.8(2) . . . 3_576 ? C1 C2 C7 C1 -4.7(4) . . . 3_576 ? C5 C6 C7 C2 -0.1(4) . . . . ? C5 C6 C7 C1 -177.4(2) . . . 3_576 ? O1 C1 C11 C16 -175.71(19) . . . . ? C7 C1 C11 C16 -57.3(3) 3_576 . . . ? C2 C1 C11 C16 66.1(3) . . . . ? O1 C1 C11 C12 3.3(3) . . . . ? C7 C1 C11 C12 121.7(2) 3_576 . . . ? C2 C1 C11 C12 -114.9(2) . . . . ? C16 C11 C12 C13 0.4(3) . . . . ? C1 C11 C12 C13 -178.6(2) . . . . ? C11 C12 C13 C14 -0.8(3) . . . . ? C12 C13 C14 C15 0.5(3) . . . . ? C12 C13 C14 C17 179.2(2) . . . . ? C13 C14 C15 C16 0.0(3) . . . . ? C17 C14 C15 C16 -178.7(2) . . . . ? C12 C11 C16 C15 0.1(4) . . . . ? C1 C11 C16 C15 179.2(2) . . . . ? C14 C15 C16 C11 -0.3(4) . . . . ? C15 C14 C17 C19 -173.5(3) . . . . ? C13 C14 C17 C19 7.9(4) . . . . ? C15 C14 C17 C22 0.1(8) . . . . ? C13 C14 C17 C22 -178.5(8) . . . . ? C15 C14 C17 C21 -50.9(4) . . . . ? C13 C14 C17 C21 130.5(3) . . . . ? C15 C14 C17 C23 66.5(3) . . . . ? C13 C14 C17 C23 -112.1(3) . . . . ? C15 C14 C17 C18 120.4(6) . . . . ? C13 C14 C17 C18 -58.2(6) . . . . ? C15 C14 C17 C20 -128.4(9) . . . . ? C13 C14 C17 C20 53.0(9) . . . . ? C19 C17 C18 C23 159.2(6) . . . . ? C14 C17 C18 C23 -95.1(5) . . . . ? C22 C17 C18 C23 31.7(7) . . . . ? C21 C17 C18 C23 72.1(9) . . . . ? C20 C17 C18 C23 148.0(7) . . . . ? C14 C17 C18 C19 105.7(4) . . . . ? C22 C17 C18 C19 -127.5(6) . . . . ? C21 C17 C18 C19 -87.1(8) . . . . ? C23 C17 C18 C19 -159.2(6) . . . . ? C20 C17 C18 C19 -11.2(7) . . . . ? C14 C17 C19 C20 94.9(8) . . . . ? C22 C17 C19 C20 -77.7(12) . . . . ? C21 C17 C19 C20 -27.4(9) . . . . ? C23 C17 C19 C20 -146.5(8) . . . . ? C18 C17 C19 C20 -163.5(10) . . . . ? C14 C17 C19 C18 -101.7(5) . . . . ? C22 C17 C19 C18 85.8(10) . . . . ? C21 C17 C19 C18 136.1(6) . . . . ? C23 C17 C19 C18 17.0(5) . . . . ? C20 C17 C19 C18 163.5(10) . . . . ? C23 C18 C19 C20 2.1(16) . . . . ? C17 C18 C19 C20 23.0(12) . . . . ? C23 C18 C19 C17 -20.8(6) . . . . ? C18 C19 C20 C17 -20.9(11) . . . . ? C17 C19 C20 C21 22.2(5) . . . . ? C18 C19 C20 C21 1.3(15) . . . . ? C14 C17 C20 C19 -102.6(6) . . . . ? C22 C17 C20 C19 126.2(9) . . . . ? C21 C17 C20 C19 153.0(8) . . . . ? C23 C17 C20 C19 54.8(15) . . . . ? C18 C17 C20 C19 14.7(9) . . . . ? C19 C17 C20 C21 -153.0(8) . . . . ? C14 C17 C20 C21 104.4(4) . . . . ? C22 C17 C20 C21 -26.7(7) . . . . ? C23 C17 C20 C21 -98.2(11) . . . . ? C18 C17 C20 C21 -138.3(5) . . . . ? C19 C17 C21 C22 -126.4(7) . . . . ? C14 C17 C21 C22 108.9(6) . . . . ? C23 C17 C21 C22 -7.2(7) . . . . ? C18 C17 C21 C22 -58.4(11) . . . . ? C20 C17 C21 C22 -145.3(8) . . . . ? C19 C17 C21 C20 18.8(5) . . . . ? C14 C17 C21 C20 -105.8(5) . . . . ? C22 C17 C21 C20 145.3(8) . . . . ? C23 C17 C21 C20 138.1(5) . . . . ? C18 C17 C21 C20 86.8(10) . . . . ? C19 C20 C21 C22 9.7(12) . . . . ? C17 C20 C21 C22 35.0(7) . . . . ? C19 C20 C21 C17 -25.3(7) . . . . ? C20 C21 C22 C17 -31.2(6) . . . . ? C17 C21 C22 C23 8.0(7) . . . . ? C20 C21 C22 C23 -23.1(13) . . . . ? C19 C17 C22 C21 80.3(8) . . . . ? C14 C17 C22 C21 -92.1(6) . . . . ? C23 C17 C22 C21 172.3(7) . . . . ? C18 C17 C22 C21 144.8(6) . . . . ? C20 C17 C22 C21 35.7(9) . . . . ? C19 C17 C22 C23 -92.0(8) . . . . ? C14 C17 C22 C23 95.6(5) . . . . ? C21 C17 C22 C23 -172.3(7) . . . . ? C18 C17 C22 C23 -27.5(6) . . . . ? C20 C17 C22 C23 -136.6(7) . . . . ? C19 C18 C23 C17 19.4(5) . . . . ? C19 C18 C23 C22 -13.7(11) . . . . ? C17 C18 C23 C22 -33.1(6) . . . . ? C19 C17 C23 C18 -19.2(6) . . . . ? C14 C17 C23 C18 103.4(6) . . . . ? C22 C17 C23 C18 -144.9(8) . . . . ? C21 C17 C23 C18 -139.0(6) . . . . ? C20 C17 C23 C18 -54.4(14) . . . . ? C19 C17 C23 C22 125.8(6) . . . . ? C14 C17 C23 C22 -111.7(5) . . . . ? C21 C17 C23 C22 6.0(6) . . . . ? C18 C17 C23 C22 144.9(8) . . . . ? C20 C17 C23 C22 90.5(14) . . . . ? C21 C22 C23 C18 26.9(13) . . . . ? C17 C22 C23 C18 35.5(7) . . . . ? C21 C22 C23 C17 -8.5(8) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O24 0.84 2.03 2.855(2) 167.5 . _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.70 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.378 _refine_diff_density_min -0.215 _refine_diff_density_rms 0.054 #========================================================END data_c:_H.2A.2C _database_code_CSD 175489 _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-9,10-dihydroxy-9,10-bis(p-tert-butylphenyl)-9,10-dihydroanthracene. 2(N,N-dimethylformamide). 2(acetone) clathrate ; _chemical_name_common none _chemical_melting_point 292 _chemical_formula_moiety 'C34 H36 O2. 2(C3 H7 N O). 2(C3 H6 O)' _chemical_formula_sum 'C46 H62 N2 O6' _chemical_formula_weight 738.98 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' _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 8.99320(10) _cell_length_b 9.16740(10) _cell_length_c 14.3817(2) _cell_angle_alpha 108.3260(10) _cell_angle_beta 92.8080(10) _cell_angle_gamma 70.8860(10) _cell_volume 1061.57(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4641 _cell_measurement_theta_min 1.49 _cell_measurement_theta_max 27.50 _exptl_crystal_description 'clear plates' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.156 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 400 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type none _exptl_special_details ; Unstable without mother liquor under atmospheric conditions. Crystal coated with Paratone oil and data collected at 173K. ; _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 'Nonius Kappa CCD' _diffrn_measurement_method 'Combination of phi and omega' _diffrn_reflns_number 7598 _diffrn_reflns_av_R_equivalents 0.0160 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4651 _reflns_number_gt 3708 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 2000)' _computing_cell_refinement 'Collect (Nonius, 2000)' _computing_data_reduction 'Collect (Nonius, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics none _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1340P)^2^+0.8628P] 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_number_reflns 4651 _refine_ls_number_parameters 266 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1000 _refine_ls_R_factor_gt 0.0828 _refine_ls_wR_factor_ref 0.2551 _refine_ls_wR_factor_gt 0.2396 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.277 _refine_ls_shift/su_mean 0.026 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 -0.25492(18) 0.15116(18) -0.08133(11) 0.0301(4) Uani 1 1 d . . . H1 H -0.2122 0.0766 -0.1331 0.036 Uiso 1 1 calc R . . C1 C -0.1538(2) 0.1365(2) -0.00242(14) 0.0227(4) Uani 1 1 d . . . C2 C 0.0093(2) 0.1349(2) -0.02874(14) 0.0237(4) Uani 1 1 d . . . C3 C 0.0167(3) 0.2667(3) -0.05670(16) 0.0309(5) Uani 1 1 d . . . H3 H -0.0781 0.3501 -0.0595 0.037 Uiso 1 1 calc R . . C4 C 0.1591(3) 0.2766(3) -0.08002(18) 0.0360(5) Uani 1 1 d . . . H4 H 0.1622 0.3655 -0.0995 0.043 Uiso 1 1 calc R . . C5 C 0.2982(3) 0.1558(3) -0.07483(19) 0.0372(6) Uani 1 1 d . . . H5 H 0.3968 0.1626 -0.0901 0.045 Uiso 1 1 calc R . . C6 C 0.2928(3) 0.0263(3) -0.04752(17) 0.0316(5) Uani 1 1 d . . . H6 H 0.3883 -0.0559 -0.0442 0.038 Uiso 1 1 calc R . . C7 C 0.1483(2) 0.0138(2) -0.02453(14) 0.0241(4) Uani 1 1 d . . . C11 C -0.2280(2) 0.2879(2) 0.08572(14) 0.0237(4) Uani 1 1 d . . . C12 C -0.1480(3) 0.3118(3) 0.17152(17) 0.0324(5) Uani 1 1 d . . . H12 H -0.0489 0.2342 0.1744 0.039 Uiso 1 1 calc R . . C19 C -0.5702(19) 0.7167(17) 0.3843(11) 0.083(5) Uani 0.28 1 d P . . C23 C -0.4506(16) 0.8742(10) 0.3142(8) 0.058(3) Uani 0.28 1 d P . . C31 C -0.0500(15) -0.2407(15) -0.4491(9) 0.072(3) Uiso 0.33 1 d P . . C13 C -0.2111(3) 0.4473(3) 0.25300(17) 0.0355(5) Uani 1 1 d . . . H13 H -0.1539 0.4610 0.3107 0.043 Uiso 1 1 calc R . . C14 C -0.3567(3) 0.5641(3) 0.25201(16) 0.0314(5) Uani 1 1 d . . . C15 C -0.4347(3) 0.5404(3) 0.16580(17) 0.0315(5) Uani 1 1 d . . . H15 H -0.5329 0.6189 0.1624 0.038 Uiso 1 1 calc R . . C16 C -0.3720(2) 0.4030(3) 0.08353(16) 0.0278(5) Uani 1 1 d . . . H16 H -0.4289 0.3890 0.0258 0.033 Uiso 1 1 calc R . . C17 C -0.4236(3) 0.7135(3) 0.34301(18) 0.0416(6) Uani 1 1 d . . . C18 C -0.5997(6) 0.8084(6) 0.3308(3) 0.0698(16) Uani 0.72 1 d P . . C20 C -0.4249(6) 0.6569(5) 0.4330(3) 0.0515(10) Uani 0.72 1 d P . . C21 C -0.2945(16) 0.7290(15) 0.4277(8) 0.069(4) Uani 0.28 1 d P . . C22 C -0.3237(8) 0.8194(6) 0.3553(4) 0.0755(17) Uani 0.72 1 d P . . O24 O -0.1694(3) -0.1080(4) -0.2609(2) 0.0407(6) Uiso 0.67 1 d P . . C25 C -0.0968(5) -0.1683(5) -0.3406(3) 0.0438(9) Uiso 0.67 1 d P . . N26 N 0.0200(4) -0.1288(4) -0.3733(2) 0.0668(8) Uiso 1 1 d . . . C27 C 0.0481(8) 0.0187(8) -0.3002(5) 0.0762(16) Uiso 0.67 1 d P . . C28 C 0.1061(10) -0.2063(10) -0.4599(6) 0.092(2) Uiso 0.67 1 d P . . O29 O -0.1345(9) -0.0388(10) -0.2609(6) 0.0655(18) Uiso 0.33 1 d P . . C30 C -0.0081(12) -0.0616(12) -0.2947(7) 0.055(2) Uiso 0.33 1 d P . . C32 C 0.2046(14) -0.1924(15) -0.4269(9) 0.067(3) Uiso 0.33 1 d P . . O33 O -0.2090(4) 0.5256(4) -0.3604(2) 0.0965(10) Uani 1 1 d . . . C34 C -0.2777(5) 0.6053(4) -0.2804(2) 0.0604(8) Uani 1 1 d . . . C35 C -0.4345(6) 0.7335(6) -0.2723(4) 0.0880(13) Uani 1 1 d . . . H35A H -0.4651 0.7384 -0.3379 0.132 Uiso 1 1 calc R . . H35B H -0.4279 0.8392 -0.2318 0.132 Uiso 1 1 calc R . . H35C H -0.5134 0.7073 -0.2419 0.132 Uiso 1 1 calc R . . C36 C -0.2111(5) 0.5769(7) -0.1894(3) 0.0816(13) Uani 1 1 d . . . H36A H -0.1094 0.4891 -0.2053 0.122 Uiso 1 1 calc R . . H36B H -0.2837 0.5462 -0.1566 0.122 Uiso 1 1 calc R . . H36C H -0.1961 0.6767 -0.1456 0.122 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 0.0293(8) 0.0278(8) 0.0252(8) 0.0050(6) -0.0049(6) -0.0029(6) C1 0.0218(9) 0.0207(9) 0.0227(9) 0.0056(7) -0.0010(7) -0.0042(7) C2 0.0272(10) 0.0203(9) 0.0205(9) 0.0037(7) 0.0022(7) -0.0059(8) C3 0.0357(12) 0.0235(10) 0.0316(11) 0.0090(8) 0.0042(9) -0.0059(8) C4 0.0449(13) 0.0271(11) 0.0379(12) 0.0087(9) 0.0079(10) -0.0141(10) C5 0.0347(12) 0.0351(12) 0.0426(13) 0.0076(10) 0.0095(10) -0.0155(10) C6 0.0254(11) 0.0280(11) 0.0374(12) 0.0053(9) 0.0039(9) -0.0075(8) C7 0.0253(10) 0.0201(9) 0.0230(9) 0.0031(7) 0.0014(7) -0.0057(8) C11 0.0239(10) 0.0190(9) 0.0254(10) 0.0066(7) 0.0023(8) -0.0032(7) C12 0.0279(11) 0.0277(11) 0.0301(11) 0.0037(9) -0.0013(8) 0.0007(8) C19 0.088(10) 0.058(7) 0.083(9) -0.025(7) 0.065(8) -0.034(7) C23 0.091(8) 0.016(4) 0.044(5) 0.001(4) -0.010(5) 0.001(4) C13 0.0379(13) 0.0315(12) 0.0270(11) 0.0035(9) -0.0025(9) -0.0041(9) C14 0.0397(12) 0.0206(10) 0.0285(11) 0.0052(8) 0.0090(9) -0.0039(9) C15 0.0307(11) 0.0235(10) 0.0337(11) 0.0106(9) 0.0065(9) 0.0023(8) C16 0.0263(10) 0.0248(10) 0.0282(10) 0.0085(8) 0.0014(8) -0.0026(8) C17 0.0564(16) 0.0261(11) 0.0297(12) 0.0019(9) 0.0107(11) -0.0019(10) C18 0.078(3) 0.046(2) 0.036(2) -0.0036(18) 0.007(2) 0.029(2) C20 0.072(3) 0.041(2) 0.0270(17) 0.0053(15) 0.0116(17) -0.0021(19) C21 0.075(8) 0.051(6) 0.041(6) -0.013(5) -0.019(5) 0.002(6) C22 0.126(5) 0.042(2) 0.056(3) -0.012(2) 0.024(3) -0.046(3) O33 0.131(3) 0.0742(18) 0.0585(17) -0.0022(14) 0.0208(17) -0.0195(18) C34 0.080(2) 0.0505(17) 0.0526(18) 0.0086(14) 0.0087(16) -0.0291(16) C35 0.093(3) 0.078(3) 0.095(3) 0.040(2) 0.018(2) -0.016(2) C36 0.078(3) 0.125(4) 0.072(2) 0.043(3) -0.014(2) -0.062(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 O1 C1 1.431(2) . ? C1 C2 1.527(3) . ? C1 C7 1.530(3) 2 ? C1 C11 1.533(3) . ? C2 C7 1.387(3) . ? C2 C3 1.410(3) . ? C3 C4 1.378(3) . ? C4 C5 1.390(4) . ? C5 C6 1.379(3) . ? C6 C7 1.404(3) . ? C7 C1 1.530(3) 2 ? C11 C16 1.383(3) . ? C11 C12 1.391(3) . ? C12 C13 1.388(3) . ? C19 C18 1.269(19) . ? C19 C20 1.48(2) . ? C19 C17 1.461(12) . ? C23 C22 1.284(13) . ? C23 C17 1.594(10) . ? C23 C18 1.694(15) . ? C31 N26 1.513(13) . ? C31 C25 1.510(13) . ? C31 C28 1.562(14) . ? C13 C14 1.397(3) . ? C14 C15 1.386(3) . ? C14 C17 1.537(3) . ? C15 C16 1.402(3) . ? C17 C22 1.493(6) . ? C17 C20 1.540(5) . ? C17 C18 1.569(5) . ? C17 C21 1.646(11) . ? C20 C21 1.538(16) . ? C21 C22 1.489(15) . ? O24 O29 0.794(8) . ? O24 C25 1.218(5) . ? O24 C30 1.767(10) . ? C25 O29 1.326(9) . ? C25 N26 1.364(5) . ? C25 C30 1.443(11) . ? N26 C30 1.099(10) . ? N26 C28 1.354(8) . ? N26 C27 1.517(7) . ? N26 C32 1.703(12) . ? C27 C30 1.043(11) . ? C28 C32 1.010(12) . ? O29 C30 1.186(12) . ? O33 C34 1.219(4) . ? C34 C36 1.475(5) . ? C34 C35 1.493(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 110.42(16) . . ? O1 C1 C7 109.89(16) . 2 ? C2 C1 C7 112.80(16) . 2 ? O1 C1 C11 106.58(15) . . ? C2 C1 C11 108.50(16) . . ? C7 C1 C11 108.42(16) 2 . ? C7 C2 C3 119.09(19) . . ? C7 C2 C1 123.71(18) . . ? C3 C2 C1 117.19(18) . . ? C4 C3 C2 121.1(2) . . ? C3 C4 C5 119.6(2) . . ? C6 C5 C4 119.9(2) . . ? C5 C6 C7 121.1(2) . . ? C2 C7 C6 119.20(19) . . ? C2 C7 C1 123.43(18) . 2 ? C6 C7 C1 117.35(18) . 2 ? C16 C11 C12 118.29(19) . . ? C16 C11 C1 122.63(18) . . ? C12 C11 C1 119.08(17) . . ? C13 C12 C11 120.9(2) . . ? C18 C19 C20 129.7(10) . . ? C18 C19 C17 69.8(7) . . ? C20 C19 C17 63.3(7) . . ? C22 C23 C17 61.4(5) . . ? C22 C23 C18 114.9(8) . . ? C17 C23 C18 56.9(5) . . ? N26 C31 C25 53.6(5) . . ? N26 C31 C28 52.2(5) . . ? C25 C31 C28 104.6(8) . . ? C12 C13 C14 121.4(2) . . ? C15 C14 C13 117.27(19) . . ? C15 C14 C17 122.3(2) . . ? C13 C14 C17 120.4(2) . . ? C14 C15 C16 121.5(2) . . ? C11 C16 C15 120.6(2) . . ? C19 C17 C22 139.6(5) . . ? C19 C17 C20 58.9(8) . . ? C22 C17 C20 112.1(3) . . ? C19 C17 C14 112.2(5) . . ? C22 C17 C14 107.9(3) . . ? C20 C17 C14 109.3(2) . . ? C19 C17 C18 49.4(8) . . ? C22 C17 C18 110.7(4) . . ? C20 C17 C18 106.2(3) . . ? C14 C17 C18 110.6(2) . . ? C19 C17 C23 110.4(9) . . ? C22 C17 C23 49.0(5) . . ? C20 C17 C23 141.2(4) . . ? C14 C17 C23 109.0(4) . . ? C18 C17 C23 64.8(6) . . ? C19 C17 C21 110.6(10) . . ? C22 C17 C21 56.4(6) . . ? C20 C17 C21 57.6(6) . . ? C14 C17 C21 112.3(4) . . ? C18 C17 C21 137.1(4) . . ? C23 C17 C21 101.8(7) . . ? C19 C18 C17 60.9(6) . . ? C19 C18 C23 115.0(9) . . ? C17 C18 C23 58.3(4) . . ? C19 C20 C17 57.9(5) . . ? C19 C20 C21 116.0(7) . . ? C17 C20 C21 64.7(5) . . ? C22 C21 C20 112.5(8) . . ? C22 C21 C17 56.6(5) . . ? C20 C21 C17 57.7(5) . . ? C23 C22 C21 130.1(9) . . ? C23 C22 C17 69.6(6) . . ? C21 C22 C17 67.0(6) . . ? O29 O24 C25 79.4(6) . . ? O29 O24 C30 33.3(7) . . ? C25 O24 C30 54.1(4) . . ? O24 C25 O29 36.1(4) . . ? O24 C25 N26 128.5(4) . . ? O29 C25 N26 93.8(5) . . ? O24 C25 C30 82.8(5) . . ? O29 C25 C30 50.5(5) . . ? N26 C25 C30 46.0(4) . . ? O24 C25 C31 164.7(6) . . ? O29 C25 C31 148.6(7) . . ? N26 C25 C31 63.3(5) . . ? C30 C25 C31 109.2(7) . . ? C30 N26 C28 159.1(7) . . ? C30 N26 C25 70.8(6) . . ? C28 N26 C25 126.9(5) . . ? C30 N26 C27 43.4(6) . . ? C28 N26 C27 120.7(5) . . ? C25 N26 C27 112.4(4) . . ? C30 N26 C31 133.7(8) . . ? C28 N26 C31 65.7(6) . . ? C25 N26 C31 63.1(5) . . ? C27 N26 C31 164.1(6) . . ? C30 N26 C32 122.7(7) . . ? C28 N26 C32 36.4(5) . . ? C25 N26 C32 148.1(5) . . ? C27 N26 C32 91.1(5) . . ? C31 N26 C32 99.6(6) . . ? C30 C27 N26 46.4(6) . . ? C32 C28 N26 90.9(9) . . ? C32 C28 C31 145.1(11) . . ? N26 C28 C31 62.0(6) . . ? O24 O29 C30 125.2(10) . . ? O24 O29 C25 64.6(6) . . ? C30 O29 C25 69.9(7) . . ? C27 C30 N26 90.1(9) . . ? C27 C30 O29 131.7(11) . . ? N26 C30 O29 118.4(10) . . ? C27 C30 C25 148.5(10) . . ? N26 C30 C25 63.2(6) . . ? O29 C30 C25 59.6(6) . . ? C27 C30 O24 153.2(9) . . ? N26 C30 O24 106.1(7) . . ? O29 C30 O24 21.5(5) . . ? C25 C30 O24 43.1(3) . . ? C28 C32 N26 52.7(7) . . ? O33 C34 C36 121.6(4) . . ? O33 C34 C35 120.4(4) . . ? C36 C34 C35 118.0(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C7 -126.1(2) . . . . ? C7 C1 C2 C7 -2.7(3) 2 . . . ? C11 C1 C2 C7 117.5(2) . . . . ? O1 C1 C2 C3 55.3(2) . . . . ? C7 C1 C2 C3 178.71(17) 2 . . . ? C11 C1 C2 C3 -61.1(2) . . . . ? C7 C2 C3 C4 0.2(3) . . . . ? C1 C2 C3 C4 178.9(2) . . . . ? C2 C3 C4 C5 -0.8(4) . . . . ? C3 C4 C5 C6 0.7(4) . . . . ? C4 C5 C6 C7 -0.1(4) . . . . ? C3 C2 C7 C6 0.5(3) . . . . ? C1 C2 C7 C6 -178.12(18) . . . . ? C3 C2 C7 C1 -178.45(18) . . . 2 ? C1 C2 C7 C1 3.0(3) . . . 2 ? C5 C6 C7 C2 -0.5(3) . . . . ? C5 C6 C7 C1 178.5(2) . . . 2 ? O1 C1 C11 C16 4.3(3) . . . . ? C2 C1 C11 C16 123.2(2) . . . . ? C7 C1 C11 C16 -113.9(2) 2 . . . ? O1 C1 C11 C12 -175.45(18) . . . . ? C2 C1 C11 C12 -56.5(2) . . . . ? C7 C1 C11 C12 66.3(2) 2 . . . ? C16 C11 C12 C13 0.1(3) . . . . ? C1 C11 C12 C13 179.9(2) . . . . ? C11 C12 C13 C14 0.2(4) . . . . ? C12 C13 C14 C15 -1.0(4) . . . . ? C12 C13 C14 C17 -179.7(2) . . . . ? C13 C14 C15 C16 1.4(3) . . . . ? C17 C14 C15 C16 -179.9(2) . . . . ? C12 C11 C16 C15 0.3(3) . . . . ? C1 C11 C16 C15 -179.50(19) . . . . ? C14 C15 C16 C11 -1.1(3) . . . . ? C18 C19 C17 C22 73.3(14) . . . . ? C20 C19 C17 C22 -88.3(12) . . . . ? C18 C19 C17 C20 161.6(8) . . . . ? C18 C19 C17 C14 -98.6(5) . . . . ? C20 C19 C17 C14 99.8(5) . . . . ? C20 C19 C17 C18 -161.6(8) . . . . ? C18 C19 C17 C23 23.2(8) . . . . ? C20 C19 C17 C23 -138.3(5) . . . . ? C18 C19 C17 C21 135.1(7) . . . . ? C20 C19 C17 C21 -26.4(7) . . . . ? C15 C14 C17 C19 65.0(9) . . . . ? C13 C14 C17 C19 -116.3(9) . . . . ? C15 C14 C17 C22 -109.5(4) . . . . ? C13 C14 C17 C22 69.2(4) . . . . ? C15 C14 C17 C20 128.3(3) . . . . ? C13 C14 C17 C20 -53.0(4) . . . . ? C15 C14 C17 C18 11.7(4) . . . . ? C13 C14 C17 C18 -169.6(3) . . . . ? C15 C14 C17 C23 -57.6(6) . . . . ? C13 C14 C17 C23 121.0(6) . . . . ? C15 C14 C17 C21 -169.7(6) . . . . ? C13 C14 C17 C21 9.0(7) . . . . ? C22 C23 C17 C19 138.8(8) . . . . ? C18 C23 C17 C19 -19.3(8) . . . . ? C18 C23 C17 C22 -158.1(6) . . . . ? C22 C23 C17 C20 73.5(10) . . . . ? C18 C23 C17 C20 -84.6(8) . . . . ? C22 C23 C17 C14 -97.5(5) . . . . ? C18 C23 C17 C14 104.4(3) . . . . ? C22 C23 C17 C18 158.1(6) . . . . ? C22 C23 C17 C21 21.4(7) . . . . ? C18 C23 C17 C21 -136.8(5) . . . . ? C20 C19 C18 C17 21.6(8) . . . . ? C20 C19 C18 C23 -1.0(13) . . . . ? C17 C19 C18 C23 -22.5(7) . . . . ? C22 C17 C18 C19 -138.4(7) . . . . ? C20 C17 C18 C19 -16.4(7) . . . . ? C14 C17 C18 C19 102.1(7) . . . . ? C23 C17 C18 C19 -155.9(8) . . . . ? C21 C17 C18 C19 -75.9(12) . . . . ? C19 C17 C18 C23 155.9(8) . . . . ? C22 C17 C18 C23 17.5(5) . . . . ? C20 C17 C18 C23 139.5(5) . . . . ? C14 C17 C18 C23 -102.0(5) . . . . ? C21 C17 C18 C23 80.0(10) . . . . ? C22 C23 C18 C19 2.0(10) . . . . ? C17 C23 C18 C19 23.2(7) . . . . ? C22 C23 C18 C17 -21.1(5) . . . . ? C18 C19 C20 C17 -22.7(8) . . . . ? C18 C19 C20 C21 7.0(14) . . . . ? C17 C19 C20 C21 29.8(7) . . . . ? C22 C17 C20 C19 135.6(6) . . . . ? C14 C17 C20 C19 -104.8(6) . . . . ? C18 C17 C20 C19 14.5(6) . . . . ? C23 C17 C20 C19 84.2(11) . . . . ? C21 C17 C20 C19 150.4(7) . . . . ? C19 C17 C20 C21 -150.4(7) . . . . ? C22 C17 C20 C21 -14.8(5) . . . . ? C14 C17 C20 C21 104.8(5) . . . . ? C18 C17 C20 C21 -135.9(5) . . . . ? C23 C17 C20 C21 -66.2(10) . . . . ? C19 C20 C21 C22 -12.8(10) . . . . ? C17 C20 C21 C22 14.9(5) . . . . ? C19 C20 C21 C17 -27.7(6) . . . . ? C19 C17 C21 C22 -136.6(7) . . . . ? C20 C17 C21 C22 -163.5(6) . . . . ? C14 C17 C21 C22 97.2(4) . . . . ? C18 C17 C21 C22 -84.8(9) . . . . ? C23 C17 C21 C22 -19.3(6) . . . . ? C19 C17 C21 C20 26.8(7) . . . . ? C22 C17 C21 C20 163.5(6) . . . . ? C14 C17 C21 C20 -99.3(4) . . . . ? C18 C17 C21 C20 78.7(8) . . . . ? C23 C17 C21 C20 144.2(5) . . . . ? C17 C23 C22 C21 -31.0(8) . . . . ? C18 C23 C22 C21 -10.9(11) . . . . ? C18 C23 C22 C17 20.1(5) . . . . ? C20 C21 C22 C23 16.5(12) . . . . ? C17 C21 C22 C23 31.6(8) . . . . ? C20 C21 C22 C17 -15.1(5) . . . . ? C19 C17 C22 C23 -72.1(15) . . . . ? C20 C17 C22 C23 -139.6(6) . . . . ? C14 C17 C22 C23 100.0(6) . . . . ? C18 C17 C22 C23 -21.1(6) . . . . ? C21 C17 C22 C23 -154.7(8) . . . . ? C19 C17 C22 C21 82.5(14) . . . . ? C20 C17 C22 C21 15.0(6) . . . . ? C14 C17 C22 C21 -105.4(5) . . . . ? C18 C17 C22 C21 133.5(5) . . . . ? C23 C17 C22 C21 154.7(8) . . . . ? C30 O24 C25 O29 -23.9(7) . . . . ? O29 O24 C25 N26 18.3(8) . . . . ? C30 O24 C25 N26 -5.5(5) . . . . ? O29 O24 C25 C30 23.9(7) . . . . ? O29 O24 C25 C31 -118(2) . . . . ? C30 O24 C25 C31 -142(2) . . . . ? N26 C31 C25 O24 143(2) . . . . ? C28 C31 C25 O24 155.1(19) . . . . ? N26 C31 C25 O29 46.8(13) . . . . ? C28 C31 C25 O29 58.8(15) . . . . ? C28 C31 C25 N26 12.0(5) . . . . ? N26 C31 C25 C30 3.1(6) . . . . ? C28 C31 C25 C30 15.0(10) . . . . ? O24 C25 N26 C30 7.6(7) . . . . ? O29 C25 N26 C30 18.3(7) . . . . ? C31 C25 N26 C30 176.0(8) . . . . ? O24 C25 N26 C28 174.9(5) . . . . ? O29 C25 N26 C28 -174.4(6) . . . . ? C30 C25 N26 C28 167.2(8) . . . . ? C31 C25 N26 C28 -16.8(7) . . . . ? O24 C25 N26 C27 -5.2(6) . . . . ? O29 C25 N26 C27 5.5(5) . . . . ? C30 C25 N26 C27 -12.8(6) . . . . ? C31 C25 N26 C27 163.2(6) . . . . ? O24 C25 N26 C31 -168.3(7) . . . . ? O29 C25 N26 C31 -157.6(7) . . . . ? C30 C25 N26 C31 -176.0(8) . . . . ? O24 C25 N26 C32 129.2(9) . . . . ? O29 C25 N26 C32 139.9(10) . . . . ? C30 C25 N26 C32 121.6(11) . . . . ? C31 C25 N26 C32 -62.4(11) . . . . ? C25 C31 N26 C30 -5.3(11) . . . . ? C28 C31 N26 C30 -170.6(10) . . . . ? C25 C31 N26 C28 165.3(6) . . . . ? C28 C31 N26 C25 -165.3(6) . . . . ? C25 C31 N26 C27 -77(2) . . . . ? C28 C31 N26 C27 118(2) . . . . ? C25 C31 N26 C32 151.6(5) . . . . ? C28 C31 N26 C32 -13.7(6) . . . . ? C28 N26 C27 C30 -162.3(9) . . . . ? C25 N26 C27 C30 17.7(9) . . . . ? C31 N26 C27 C30 88(2) . . . . ? C32 N26 C27 C30 -140.1(9) . . . . ? C30 N26 C28 C32 4(2) . . . . ? C25 N26 C28 C32 -140.4(8) . . . . ? C27 N26 C28 C32 39.6(10) . . . . ? C31 N26 C28 C32 -156.8(10) . . . . ? C30 N26 C28 C31 161(2) . . . . ? C25 N26 C28 C31 16.4(7) . . . . ? C27 N26 C28 C31 -163.5(7) . . . . ? C32 N26 C28 C31 156.8(10) . . . . ? N26 C31 C28 C32 43.3(18) . . . . ? C25 C31 C28 C32 31(2) . . . . ? C25 C31 C28 N26 -12.2(5) . . . . ? C25 O24 O29 C30 -36.7(10) . . . . ? C30 O24 O29 C25 36.7(10) . . . . ? N26 C25 O29 O24 -165.7(6) . . . . ? C30 C25 O29 O24 -148.7(9) . . . . ? C31 C25 O29 O24 153.6(12) . . . . ? O24 C25 O29 C30 148.7(9) . . . . ? N26 C25 O29 C30 -17.0(6) . . . . ? C31 C25 O29 C30 -57.8(14) . . . . ? N26 C27 C30 O29 -129.7(16) . . . . ? N26 C27 C30 C25 -30.6(14) . . . . ? N26 C27 C30 O24 -128(2) . . . . ? C28 N26 C30 C27 47(2) . . . . ? C25 N26 C30 C27 -162.7(8) . . . . ? C31 N26 C30 C27 -157.7(8) . . . . ? C32 N26 C30 C27 49.7(10) . . . . ? C28 N26 C30 O29 -173.8(14) . . . . ? C25 N26 C30 O29 -23.5(9) . . . . ? C27 N26 C30 O29 139.2(14) . . . . ? C31 N26 C30 O29 -18.5(16) . . . . ? C32 N26 C30 O29 -171.1(8) . . . . ? C28 N26 C30 C25 -150.3(18) . . . . ? C27 N26 C30 C25 162.7(8) . . . . ? C31 N26 C30 C25 5.0(10) . . . . ? C32 N26 C30 C25 -147.6(6) . . . . ? C28 N26 C30 O24 -154.6(16) . . . . ? C25 N26 C30 O24 -4.3(4) . . . . ? C27 N26 C30 O24 158.4(11) . . . . ? C31 N26 C30 O24 0.7(13) . . . . ? C32 N26 C30 O24 -151.9(6) . . . . ? O24 O29 C30 C27 178.4(12) . . . . ? C25 O29 C30 C27 143.3(14) . . . . ? O24 O29 C30 N26 59.4(16) . . . . ? C25 O29 C30 N26 24.4(9) . . . . ? O24 O29 C30 C25 35.1(10) . . . . ? C25 O29 C30 O24 -35.1(10) . . . . ? O24 C25 C30 C27 -139.2(19) . . . . ? O29 C25 C30 C27 -121(2) . . . . ? N26 C25 C30 C27 34.8(16) . . . . ? C31 C25 C30 C27 31(2) . . . . ? O24 C25 C30 N26 -174.0(6) . . . . ? O29 C25 C30 N26 -156.0(9) . . . . ? C31 C25 C30 N26 -3.8(8) . . . . ? O24 C25 C30 O29 -18.0(6) . . . . ? N26 C25 C30 O29 156.0(9) . . . . ? C31 C25 C30 O29 152.2(8) . . . . ? O29 C25 C30 O24 18.0(6) . . . . ? N26 C25 C30 O24 174.0(6) . . . . ? C31 C25 C30 O24 170.2(7) . . . . ? O29 O24 C30 C27 -2.7(19) . . . . ? C25 O24 C30 C27 131(2) . . . . ? O29 O24 C30 N26 -127.9(15) . . . . ? C25 O24 C30 N26 5.6(5) . . . . ? C25 O24 C30 O29 133.5(13) . . . . ? O29 O24 C30 C25 -133.5(13) . . . . ? C31 C28 C32 N26 -37.3(16) . . . . ? C30 N26 C32 C28 -178.4(10) . . . . ? C25 N26 C32 C28 74.6(13) . . . . ? C27 N26 C32 C28 -146.8(9) . . . . ? C31 N26 C32 C28 21.3(10) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O24 0.84 2.02 2.836(3) 164.2 . O1 H1 O29 0.84 1.84 2.662(8) 163.9 . _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 0.678 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.093 #========================================================END data_c:_H.2B.2C _database_code_CSD 175490 _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-9,10-dihydroxy-9,10-bis(p-tert-butylphenyl)-9,10-dihydroanthracene. 2(dimethyl sulfoxide). 2(acetone) clathrate ; _chemical_name_common none _chemical_melting_point 289-290 _chemical_formula_moiety 'C34 H36 O2. 2(C2 H6 O S). 2(C3 H6 O)' _chemical_formula_sum 'C44 H60 O6 S2' _chemical_formula_weight 749.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9424(18) _cell_length_b 9.1788(18) _cell_length_c 14.345(3) _cell_angle_alpha 72.25(3) _cell_angle_beta 79.80(3) _cell_angle_gamma 71.09(3) _cell_volume 1056.9(4) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4985 _cell_measurement_theta_min 2.89 _cell_measurement_theta_max 28.29 _exptl_crystal_description clear plates _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 404 _exptl_absorpt_coefficient_mu 0.171 _exptl_absorpt_correction_type none _exptl_special_details ; Unstable without mother liquor under atmospheric conditions. Crystal coated with Paratone oil and data collected at 173K. ; _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 'Nonius Kappa CCD' _diffrn_measurement_method 'Combination of phi and omega' _diffrn_reflns_number 7063 _diffrn_reflns_av_R_equivalents 0.0166 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 28.29 _reflns_number_total 4985 _reflns_number_gt 4006 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 2000)' _computing_cell_refinement 'Collect (Nonius, 2000)' _computing_data_reduction 'Collect (Nonius, 2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics none _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1367P)^2^+0.9278P] 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_number_reflns 4985 _refine_ls_number_parameters 237 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0935 _refine_ls_R_factor_gt 0.0793 _refine_ls_wR_factor_ref 0.2332 _refine_ls_wR_factor_gt 0.2195 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.084 _refine_ls_shift/su_mean 0.006 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 -0.25558(18) 0.22208(18) -0.08176(11) 0.0225(3) Uani 1 1 d . . . H1 H -0.2318 0.1722 -0.1251 0.027 Uiso 1 1 calc R . . C1 C -0.1563(2) 0.1353(2) -0.00266(14) 0.0176(4) Uani 1 1 d . . . C2 C -0.1481(2) -0.0411(2) 0.02585(14) 0.0183(4) Uani 1 1 d . . . C3 C -0.2922(3) -0.0794(3) 0.04977(16) 0.0237(4) Uani 1 1 d . . . H3 H -0.3890 0.0041 0.0469 0.028 Uiso 1 1 calc R . . C4 C -0.2963(3) -0.2363(3) 0.07744(18) 0.0289(5) Uani 1 1 d . . . H4 H -0.3951 -0.2600 0.0920 0.035 Uiso 1 1 calc R . . C5 C -0.1550(3) -0.3591(3) 0.08387(18) 0.0299(5) Uani 1 1 d . . . H5 H -0.1566 -0.4673 0.1040 0.036 Uiso 1 1 calc R . . C6 C -0.0117(3) -0.3228(3) 0.06068(17) 0.0256(5) Uani 1 1 d . . . H6 H 0.0847 -0.4072 0.0650 0.031 Uiso 1 1 calc R . . C7 C -0.0060(2) -0.1637(2) 0.03093(14) 0.0187(4) Uani 1 1 d . . . C11 C -0.2347(2) 0.2043(2) 0.08452(14) 0.0178(4) Uani 1 1 d . . . C12 C -0.3798(2) 0.3216(2) 0.08122(16) 0.0215(4) Uani 1 1 d . . . H12 H -0.4348 0.3597 0.0236 0.026 Uiso 1 1 calc R . . C13 C -0.4459(3) 0.3842(3) 0.16192(17) 0.0244(5) Uani 1 1 d . . . H13 H -0.5441 0.4660 0.1573 0.029 Uiso 1 1 calc R . . C14 C -0.3718(3) 0.3297(3) 0.24830(16) 0.0241(5) Uani 1 1 d . . . C15 C -0.2251(3) 0.2106(3) 0.25033(16) 0.0267(5) Uani 1 1 d . . . H15 H -0.1705 0.1710 0.3081 0.032 Uiso 1 1 calc R . . C16 C -0.1584(3) 0.1498(3) 0.17062(16) 0.0238(4) Uani 1 1 d . . . H16 H -0.0591 0.0697 0.1745 0.029 Uiso 1 1 calc R . . C17 C -0.4384(3) 0.3958(3) 0.33810(18) 0.0358(6) Uani 1 1 d . . . C18 C -0.6058(5) 0.5116(6) 0.3260(3) 0.0719(12) Uani 1 1 d . . . H18A H -0.6772 0.4557 0.3177 0.108 Uiso 1 1 calc R . . H18B H -0.6031 0.6014 0.2680 0.108 Uiso 1 1 calc R . . H18C H -0.6440 0.5516 0.3844 0.108 Uiso 1 1 calc R . . C19 C -0.4435(6) 0.2605(4) 0.4295(2) 0.0629(11) Uani 1 1 d . . . H19C H -0.5133 0.2023 0.4221 0.094 Uiso 1 1 calc R . . H19A H -0.4842 0.3039 0.4866 0.094 Uiso 1 1 calc R . . H19B H -0.3364 0.1875 0.4391 0.094 Uiso 1 1 calc R . . C20 C -0.3297(6) 0.4869(5) 0.3495(3) 0.0611(10) Uani 1 1 d . . . H20A H -0.3683 0.5271 0.4079 0.092 Uiso 1 1 calc R . . H20B H -0.3295 0.5769 0.2913 0.092 Uiso 1 1 calc R . . H20C H -0.2216 0.4151 0.3568 0.092 Uiso 1 1 calc R . . O21 O -0.2186(2) 0.0639(2) -0.22413(15) 0.0403(5) Uani 1 1 d . . . S22 S -0.32514(8) -0.04349(9) -0.19577(5) 0.0400(2) Uani 1 1 d . . . C23 C -0.2020(4) -0.2327(4) -0.2012(4) 0.0658(11) Uani 1 1 d . . . H23A H -0.1484 -0.2271 -0.2674 0.099 Uiso 1 1 calc R . . H23B H -0.2658 -0.3074 -0.1856 0.099 Uiso 1 1 calc R . . H23C H -0.1226 -0.2699 -0.1535 0.099 Uiso 1 1 calc R . . C24 C -0.4369(5) 0.0060(5) -0.2968(3) 0.0615(10) Uani 1 1 d . . . H24A H -0.5095 0.1142 -0.3046 0.092 Uiso 1 1 calc R . . H24B H -0.4980 -0.0702 -0.2852 0.092 Uiso 1 1 calc R . . H24C H -0.3650 0.0015 -0.3566 0.092 Uiso 1 1 calc R . . C25 C -1.2506(18) 0.8461(18) 0.4338(11) 0.086(4) Uiso 0.38 1 d P . . C26 C -1.1177(12) 0.7917(12) 0.4120(7) 0.052(2) Uiso 0.38 1 d P . . C27 C -1.0553(10) 0.7196(10) 0.3186(6) 0.0439(17) Uiso 0.38 1 d P . . C28 C -0.9707(14) 0.8168(14) 0.4477(9) 0.066(3) Uiso 0.38 1 d P . . C29 C -0.9250(15) 0.7290(16) 0.3426(10) 0.073(3) Uiso 0.38 1 d P . . C30 C -1.045(2) 0.684(2) 0.4176(13) 0.099(4) Uiso 0.38 1 d P . . C31 C -1.0909(14) 0.8266(15) 0.4495(9) 0.065(3) Uiso 0.38 1 d P . . C32 C -1.061(3) 0.561(4) 0.479(2) 0.153(9) Uiso 0.38 1 d P . . 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 0.0246(7) 0.0211(7) 0.0188(7) -0.0076(6) -0.0061(6) 0.0017(6) C1 0.0183(9) 0.0146(8) 0.0171(9) -0.0054(7) -0.0012(7) -0.0003(7) C2 0.0208(9) 0.0165(9) 0.0180(9) -0.0078(7) 0.0006(7) -0.0040(7) C3 0.0203(10) 0.0252(10) 0.0268(10) -0.0103(8) 0.0020(8) -0.0069(8) C4 0.0285(11) 0.0307(12) 0.0314(12) -0.0109(9) 0.0050(9) -0.0154(9) C5 0.0366(12) 0.0216(10) 0.0332(12) -0.0086(9) 0.0064(9) -0.0141(9) C6 0.0298(11) 0.0164(9) 0.0285(11) -0.0071(8) 0.0033(8) -0.0058(8) C7 0.0214(9) 0.0165(9) 0.0179(9) -0.0069(7) 0.0014(7) -0.0045(7) C11 0.0182(9) 0.0159(9) 0.0194(9) -0.0070(7) 0.0005(7) -0.0038(7) C12 0.0217(10) 0.0169(9) 0.0236(10) -0.0080(8) -0.0016(7) -0.0002(7) C13 0.0251(10) 0.0178(9) 0.0275(11) -0.0104(8) 0.0036(8) -0.0013(8) C14 0.0319(11) 0.0199(10) 0.0213(10) -0.0102(8) 0.0060(8) -0.0084(8) C15 0.0300(11) 0.0288(11) 0.0213(10) -0.0099(8) -0.0029(8) -0.0050(9) C16 0.0228(10) 0.0246(10) 0.0211(10) -0.0083(8) -0.0021(8) -0.0010(8) C17 0.0519(15) 0.0319(12) 0.0242(11) -0.0179(10) 0.0084(10) -0.0090(11) C18 0.070(2) 0.076(3) 0.055(2) -0.043(2) 0.0045(18) 0.016(2) C19 0.101(3) 0.0472(18) 0.0324(15) -0.0161(13) 0.0236(17) -0.0213(19) C20 0.092(3) 0.061(2) 0.0465(18) -0.0340(16) 0.0078(17) -0.032(2) O21 0.0416(10) 0.0399(10) 0.0458(11) -0.0191(9) -0.0091(8) -0.0103(8) S22 0.0330(4) 0.0507(4) 0.0368(4) -0.0142(3) -0.0016(3) -0.0111(3) C23 0.0457(18) 0.0370(16) 0.113(3) -0.0109(19) -0.0156(19) -0.0131(14) C24 0.068(2) 0.055(2) 0.072(2) -0.0050(17) -0.0364(19) -0.0252(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 1.434(2) . ? C1 C7 1.520(3) 2 ? C1 C2 1.524(3) . ? C1 C11 1.530(3) . ? C2 C7 1.394(3) . ? C2 C3 1.401(3) . ? C3 C4 1.383(3) . ? C4 C5 1.389(4) . ? C5 C6 1.387(3) . ? C6 C7 1.407(3) . ? C7 C1 1.520(3) 2 ? C11 C12 1.389(3) . ? C11 C16 1.393(3) . ? C12 C13 1.401(3) . ? C13 C14 1.387(3) . ? C14 C15 1.407(3) . ? C14 C17 1.534(3) . ? C15 C16 1.381(3) . ? C17 C19 1.512(4) . ? C17 C20 1.529(5) . ? C17 C18 1.533(5) . ? O21 S22 1.507(2) . ? S22 C23 1.746(4) . ? S22 C24 1.767(4) . ? C25 C26 1.157(17) . ? C25 C31 1.43(2) . ? C25 C30 1.98(2) . ? C26 C31 0.807(13) . ? C26 C30 0.980(19) . ? C26 C28 1.597(16) . ? C26 C27 1.606(13) . ? C26 C29 1.841(16) . ? C26 C32 1.98(3) . ? C27 C29 1.307(15) . ? C27 C30 1.37(2) . ? C28 C31 1.046(15) . ? C28 C30 1.75(2) . ? C28 C29 1.843(18) . ? C29 C30 1.44(2) . ? C30 C32 1.24(3) . ? C30 C31 1.43(2) . ? C32 C32 1.36(5) 2_366 ? 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 C7 109.77(16) . 2 ? O1 C1 C2 110.15(16) . . ? C7 C1 C2 112.97(16) 2 . ? O1 C1 C11 106.58(15) . . ? C7 C1 C11 108.26(16) 2 . ? C2 C1 C11 108.89(16) . . ? C7 C2 C3 119.31(19) . . ? C7 C2 C1 123.33(18) . . ? C3 C2 C1 117.35(18) . . ? C4 C3 C2 121.4(2) . . ? C3 C4 C5 119.6(2) . . ? C6 C5 C4 119.6(2) . . ? C5 C6 C7 121.3(2) . . ? C2 C7 C6 118.78(19) . . ? C2 C7 C1 123.61(17) . 2 ? C6 C7 C1 117.58(18) . 2 ? C12 C11 C16 118.07(18) . . ? C12 C11 C1 122.48(18) . . ? C16 C11 C1 119.45(17) . . ? C11 C12 C13 120.7(2) . . ? C14 C13 C12 121.71(19) . . ? C13 C14 C15 116.75(19) . . ? C13 C14 C17 123.6(2) . . ? C15 C14 C17 119.6(2) . . ? C16 C15 C14 121.8(2) . . ? C15 C16 C11 120.96(19) . . ? C19 C17 C20 109.6(3) . . ? C19 C17 C18 108.8(3) . . ? C20 C17 C18 108.2(3) . . ? C19 C17 C14 110.2(2) . . ? C20 C17 C14 108.2(2) . . ? C18 C17 C14 111.8(2) . . ? O21 S22 C23 105.78(15) . . ? O21 S22 C24 106.53(16) . . ? C23 S22 C24 100.5(2) . . ? C26 C25 C31 34.3(7) . . ? C26 C25 C30 20.0(8) . . ? C31 C25 C30 46.1(9) . . ? C31 C26 C30 105.9(18) . . ? C31 C26 C25 91.7(15) . . ? C30 C26 C25 136.2(17) . . ? C31 C26 C28 35.1(11) . . ? C30 C26 C28 81.7(14) . . ? C25 C26 C28 126.4(12) . . ? C31 C26 C27 143.1(14) . . ? C30 C26 C27 58.1(12) . . ? C25 C26 C27 123.4(11) . . ? C28 C26 C27 108.3(8) . . ? C31 C26 C29 99.4(13) . . ? C30 C26 C29 51.1(13) . . ? C25 C26 C29 164.0(12) . . ? C28 C26 C29 64.4(7) . . ? C27 C26 C29 43.9(6) . . ? C31 C26 C32 101.5(15) . . ? C30 C26 C32 30.6(13) . . ? C25 C26 C32 107.5(13) . . ? C28 C26 C32 93.5(10) . . ? C27 C26 C32 80.0(10) . . ? C29 C26 C32 81.6(10) . . ? C29 C27 C30 65.2(10) . . ? C29 C27 C26 77.6(8) . . ? C30 C27 C26 37.4(8) . . ? C31 C28 C26 26.4(8) . . ? C31 C28 C30 54.8(10) . . ? C26 C28 C30 33.7(7) . . ? C31 C28 C29 90.6(11) . . ? C26 C28 C29 64.2(7) . . ? C30 C28 C29 47.3(8) . . ? C27 C29 C30 59.5(10) . . ? C27 C29 C26 58.5(7) . . ? C30 C29 C26 31.9(8) . . ? C27 C29 C28 109.8(9) . . ? C30 C29 C28 62.9(10) . . ? C26 C29 C28 51.4(6) . . ? C26 C30 C32 126(2) . . ? C26 C30 C27 84.6(15) . . ? C32 C30 C27 126(2) . . ? C26 C30 C31 32.9(9) . . ? C32 C30 C31 117(2) . . ? C27 C30 C31 110.8(15) . . ? C26 C30 C29 97.0(17) . . ? C32 C30 C29 137(2) . . ? C27 C30 C29 55.3(9) . . ? C31 C30 C29 95.6(14) . . ? C26 C30 C28 64.6(13) . . ? C32 C30 C28 121(2) . . ? C27 C30 C28 112.1(13) . . ? C31 C30 C28 36.7(7) . . ? C29 C30 C28 69.8(10) . . ? C26 C30 C25 23.8(10) . . ? C32 C30 C25 103.6(17) . . ? C27 C30 C25 91.6(11) . . ? C31 C30 C25 46.1(9) . . ? C29 C30 C25 119.3(14) . . ? C28 C30 C25 82.4(10) . . ? C26 C31 C28 118.5(17) . . ? C26 C31 C25 54.0(12) . . ? C28 C31 C25 170.0(15) . . ? C26 C31 C30 41.2(12) . . ? C28 C31 C30 88.5(12) . . ? C25 C31 C30 87.9(12) . . ? C30 C32 C32 124(4) . 2_366 ? C30 C32 C26 23.7(11) . . ? C32 C32 C26 141(3) 2_366 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C7 126.7(2) . . . . ? C7 C1 C2 C7 3.5(3) 2 . . . ? C11 C1 C2 C7 -116.8(2) . . . . ? O1 C1 C2 C3 -54.6(2) . . . . ? C7 C1 C2 C3 -177.77(17) 2 . . . ? C11 C1 C2 C3 61.9(2) . . . . ? C7 C2 C3 C4 -0.6(3) . . . . ? C1 C2 C3 C4 -179.3(2) . . . . ? C2 C3 C4 C5 1.4(4) . . . . ? C3 C4 C5 C6 -1.2(4) . . . . ? C4 C5 C6 C7 0.2(4) . . . . ? C3 C2 C7 C6 -0.4(3) . . . . ? C1 C2 C7 C6 178.26(18) . . . . ? C3 C2 C7 C1 177.42(18) . . . 2 ? C1 C2 C7 C1 -3.9(3) . . . 2 ? C5 C6 C7 C2 0.6(3) . . . . ? C5 C6 C7 C1 -177.4(2) . . . 2 ? O1 C1 C11 C12 3.6(3) . . . . ? C7 C1 C11 C12 121.6(2) 2 . . . ? C2 C1 C11 C12 -115.2(2) . . . . ? O1 C1 C11 C16 -175.72(18) . . . . ? C7 C1 C11 C16 -57.7(2) 2 . . . ? C2 C1 C11 C16 65.5(2) . . . . ? C16 C11 C12 C13 0.8(3) . . . . ? C1 C11 C12 C13 -178.56(19) . . . . ? C11 C12 C13 C14 -1.4(3) . . . . ? C12 C13 C14 C15 1.2(3) . . . . ? C12 C13 C14 C17 179.3(2) . . . . ? C13 C14 C15 C16 -0.4(3) . . . . ? C17 C14 C15 C16 -178.5(2) . . . . ? C14 C15 C16 C11 -0.2(4) . . . . ? C12 C11 C16 C15 0.0(3) . . . . ? C1 C11 C16 C15 179.4(2) . . . . ? C13 C14 C17 C19 128.9(3) . . . . ? C15 C14 C17 C19 -53.1(4) . . . . ? C13 C14 C17 C20 -111.3(3) . . . . ? C15 C14 C17 C20 66.7(3) . . . . ? C13 C14 C17 C18 7.7(4) . . . . ? C15 C14 C17 C18 -174.3(3) . . . . ? C30 C25 C26 C31 -115(3) . . . . ? C31 C25 C26 C30 115(3) . . . . ? C31 C25 C26 C28 -5.6(12) . . . . ? C30 C25 C26 C28 -121(3) . . . . ? C31 C25 C26 C27 -168.0(19) . . . . ? C30 C25 C26 C27 77(2) . . . . ? C31 C25 C26 C29 -134(5) . . . . ? C30 C25 C26 C29 110(5) . . . . ? C31 C25 C26 C32 102.6(16) . . . . ? C30 C25 C26 C32 -13(2) . . . . ? C31 C26 C27 C29 8(2) . . . . ? C30 C26 C27 C29 -65.2(15) . . . . ? C25 C26 C27 C29 167.3(14) . . . . ? C28 C26 C27 C29 2.2(9) . . . . ? C32 C26 C27 C29 -88.2(11) . . . . ? C31 C26 C27 C30 73(3) . . . . ? C25 C26 C27 C30 -127(2) . . . . ? C28 C26 C27 C30 67.4(15) . . . . ? C29 C26 C27 C30 65.2(15) . . . . ? C32 C26 C27 C30 -23.0(15) . . . . ? C30 C26 C28 C31 -133(2) . . . . ? C25 C26 C28 C31 10(2) . . . . ? C27 C26 C28 C31 174(2) . . . . ? C29 C26 C28 C31 176(2) . . . . ? C32 C26 C28 C31 -105(2) . . . . ? C31 C26 C28 C30 133(2) . . . . ? C25 C26 C28 C30 143(2) . . . . ? C27 C26 C28 C30 -52.3(12) . . . . ? C29 C26 C28 C30 -50.7(13) . . . . ? C32 C26 C28 C30 28.3(13) . . . . ? C31 C26 C28 C29 -176(2) . . . . ? C30 C26 C28 C29 50.7(13) . . . . ? C25 C26 C28 C29 -166.2(15) . . . . ? C27 C26 C28 C29 -1.7(7) . . . . ? C32 C26 C28 C29 78.9(11) . . . . ? C26 C27 C29 C30 37.4(9) . . . . ? C30 C27 C29 C26 -37.4(9) . . . . ? C30 C27 C29 C28 -39.3(11) . . . . ? C26 C27 C29 C28 -1.9(8) . . . . ? C31 C26 C29 C27 -175.3(15) . . . . ? C30 C26 C29 C27 81.8(16) . . . . ? C25 C26 C29 C27 -42(4) . . . . ? C28 C26 C29 C27 -177.7(10) . . . . ? C32 C26 C29 C27 84.3(11) . . . . ? C31 C26 C29 C30 103(2) . . . . ? C25 C26 C29 C30 -124(5) . . . . ? C28 C26 C29 C30 100.5(17) . . . . ? C27 C26 C29 C30 -81.8(16) . . . . ? C32 C26 C29 C30 2.4(17) . . . . ? C31 C26 C29 C28 2.3(12) . . . . ? C30 C26 C29 C28 -100.5(17) . . . . ? C25 C26 C29 C28 136(5) . . . . ? C27 C26 C29 C28 177.7(10) . . . . ? C32 C26 C29 C28 -98.0(11) . . . . ? C31 C28 C29 C27 0.3(13) . . . . ? C26 C28 C29 C27 2.1(9) . . . . ? C30 C28 C29 C27 37.8(11) . . . . ? C31 C28 C29 C30 -37.5(12) . . . . ? C26 C28 C29 C30 -35.7(9) . . . . ? C31 C28 C29 C26 -1.8(9) . . . . ? C30 C28 C29 C26 35.7(9) . . . . ? C31 C26 C30 C32 86(3) . . . . ? C25 C26 C30 C32 -24(4) . . . . ? C28 C26 C30 C32 112(3) . . . . ? C27 C26 C30 C32 -131(3) . . . . ? C29 C26 C30 C32 175(3) . . . . ? C31 C26 C30 C27 -143.4(15) . . . . ? C25 C26 C30 C27 107(2) . . . . ? C28 C26 C30 C27 -117.6(10) . . . . ? C29 C26 C30 C27 -54.0(10) . . . . ? C32 C26 C30 C27 131(3) . . . . ? C25 C26 C30 C31 -110(3) . . . . ? C28 C26 C30 C31 25.8(13) . . . . ? C27 C26 C30 C31 143.4(15) . . . . ? C29 C26 C30 C31 89.4(17) . . . . ? C32 C26 C30 C31 -86(3) . . . . ? C31 C26 C30 C29 -89.4(17) . . . . ? C25 C26 C30 C29 160.7(19) . . . . ? C28 C26 C30 C29 -63.6(11) . . . . ? C27 C26 C30 C29 54.0(10) . . . . ? C32 C26 C30 C29 -175(3) . . . . ? C31 C26 C30 C28 -25.8(13) . . . . ? C25 C26 C30 C28 -136(2) . . . . ? C27 C26 C30 C28 117.6(10) . . . . ? C29 C26 C30 C28 63.6(11) . . . . ? C32 C26 C30 C28 -112(3) . . . . ? C31 C26 C30 C25 110(3) . . . . ? C28 C26 C30 C25 136(2) . . . . ? C27 C26 C30 C25 -107(2) . . . . ? C29 C26 C30 C25 -160.7(19) . . . . ? C32 C26 C30 C25 24(4) . . . . ? C29 C27 C30 C26 102.4(15) . . . . ? C29 C27 C30 C32 -127(2) . . . . ? C26 C27 C30 C32 131(3) . . . . ? C29 C27 C30 C31 82.2(14) . . . . ? C26 C27 C30 C31 -20.3(9) . . . . ? C26 C27 C30 C29 -102.4(15) . . . . ? C29 C27 C30 C28 42.7(11) . . . . ? C26 C27 C30 C28 -59.8(13) . . . . ? C29 C27 C30 C25 125.2(12) . . . . ? C26 C27 C30 C25 22.7(9) . . . . ? C27 C29 C30 C26 -78.4(15) . . . . ? C28 C29 C30 C26 59.6(13) . . . . ? C27 C29 C30 C32 107(3) . . . . ? C26 C29 C30 C32 -174(4) . . . . ? C28 C29 C30 C32 -115(3) . . . . ? C26 C29 C30 C27 78.4(15) . . . . ? C28 C29 C30 C27 138.0(11) . . . . ? C27 C29 C30 C31 -111.4(13) . . . . ? C26 C29 C30 C31 -33.1(10) . . . . ? C28 C29 C30 C31 26.6(8) . . . . ? C27 C29 C30 C28 -138.0(11) . . . . ? C26 C29 C30 C28 -59.6(13) . . . . ? C27 C29 C30 C25 -69.6(13) . . . . ? C26 C29 C30 C25 8.8(9) . . . . ? C28 C29 C30 C25 68.4(13) . . . . ? C31 C28 C30 C26 23.3(12) . . . . ? C29 C28 C30 C26 -108.6(16) . . . . ? C31 C28 C30 C32 -95(2) . . . . ? C26 C28 C30 C32 -118(2) . . . . ? C29 C28 C30 C32 134(2) . . . . ? C31 C28 C30 C27 95.4(16) . . . . ? C26 C28 C30 C27 72.2(15) . . . . ? C29 C28 C30 C27 -36.4(10) . . . . ? C26 C28 C30 C31 -23.3(12) . . . . ? C29 C28 C30 C31 -131.9(15) . . . . ? C31 C28 C30 C29 131.9(15) . . . . ? C26 C28 C30 C29 108.6(16) . . . . ? C31 C28 C30 C25 6.8(11) . . . . ? C26 C28 C30 C25 -16.5(9) . . . . ? C29 C28 C30 C25 -125.1(12) . . . . ? C31 C25 C30 C26 -45(2) . . . . ? C26 C25 C30 C32 160(3) . . . . ? C31 C25 C30 C32 115(2) . . . . ? C26 C25 C30 C27 -73(2) . . . . ? C31 C25 C30 C27 -117.7(14) . . . . ? C26 C25 C30 C31 45(2) . . . . ? C26 C25 C30 C29 -22(2) . . . . ? C31 C25 C30 C29 -67.3(15) . . . . ? C26 C25 C30 C28 40(2) . . . . ? C31 C25 C30 C28 -5.6(9) . . . . ? C30 C26 C31 C28 48(2) . . . . ? C25 C26 C31 C28 -172.2(16) . . . . ? C27 C26 C31 C28 -9(3) . . . . ? C29 C26 C31 C28 -3.7(19) . . . . ? C32 C26 C31 C28 79.6(18) . . . . ? C30 C26 C31 C25 -139.4(19) . . . . ? C28 C26 C31 C25 172.2(16) . . . . ? C27 C26 C31 C25 163(3) . . . . ? C29 C26 C31 C25 168.5(13) . . . . ? C32 C26 C31 C25 -108.3(14) . . . . ? C25 C26 C31 C30 139.4(19) . . . . ? C28 C26 C31 C30 -48(2) . . . . ? C27 C26 C31 C30 -57(2) . . . . ? C29 C26 C31 C30 -52.1(14) . . . . ? C32 C26 C31 C30 31.2(14) . . . . ? C30 C28 C31 C26 -29.6(15) . . . . ? C29 C28 C31 C26 3.6(18) . . . . ? C26 C28 C31 C25 -39(8) . . . . ? C30 C28 C31 C25 -69(8) . . . . ? C29 C28 C31 C25 -36(9) . . . . ? C26 C28 C31 C30 29.6(15) . . . . ? C29 C28 C31 C30 33.2(10) . . . . ? C30 C25 C31 C26 25.4(13) . . . . ? C26 C25 C31 C28 43(8) . . . . ? C30 C25 C31 C28 69(8) . . . . ? C26 C25 C31 C30 -25.4(13) . . . . ? C32 C30 C31 C26 -114(3) . . . . ? C27 C30 C31 C26 39.4(17) . . . . ? C29 C30 C31 C26 94(2) . . . . ? C28 C30 C31 C26 139(2) . . . . ? C25 C30 C31 C26 -31.8(16) . . . . ? C26 C30 C31 C28 -139(2) . . . . ? C32 C30 C31 C28 107(2) . . . . ? C27 C30 C31 C28 -99.5(15) . . . . ? C29 C30 C31 C28 -44.6(14) . . . . ? C25 C30 C31 C28 -170.7(14) . . . . ? C26 C30 C31 C25 31.8(16) . . . . ? C32 C30 C31 C25 -83(2) . . . . ? C27 C30 C31 C25 71.2(14) . . . . ? C29 C30 C31 C25 126.1(12) . . . . ? C28 C30 C31 C25 170.7(14) . . . . ? C26 C30 C32 C32 -144(4) . . . 2_366 ? C27 C30 C32 C32 105(4) . . . 2_366 ? C31 C30 C32 C32 -106(4) . . . 2_366 ? C29 C30 C32 C32 29(6) . . . 2_366 ? C28 C30 C32 C32 -64(5) . . . 2_366 ? C25 C30 C32 C32 -153(4) . . . 2_366 ? C27 C30 C32 C26 -112(3) . . . . ? C31 C30 C32 C26 37.5(16) . . . . ? C29 C30 C32 C26 173(5) . . . . ? C28 C30 C32 C26 80(3) . . . . ? C25 C30 C32 C26 -9.8(17) . . . . ? C31 C26 C32 C30 -102(3) . . . . ? C25 C26 C32 C30 163(3) . . . . ? C28 C26 C32 C30 -67(3) . . . . ? C27 C26 C32 C30 41(3) . . . . ? C29 C26 C32 C30 -4(3) . . . . ? C31 C26 C32 C32 -50(5) . . . 2_366 ? C30 C26 C32 C32 52(5) . . . 2_366 ? C25 C26 C32 C32 -146(5) . . . 2_366 ? C28 C26 C32 C32 -16(5) . . . 2_366 ? C27 C26 C32 C32 92(5) . . . 2_366 ? C29 C26 C32 C32 48(5) . . . 2_366 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O21 0.84 1.94 2.766(3) 169.5 . _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.926 _refine_diff_density_min -0.450 _refine_diff_density_rms 0.094 #========================================================END