# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global_1 _journal_name_full Org.Biomol.Chem. _journal_coden_cambridge 0177 loop_ _publ_author_name K.Mitsudo N.Kamimoto H.Murakami H.Mandai A.Wakamiya Y.Murata ; S.Suga ; data_3g _database_code_depnum_ccdc_archive 'CCDC 868776' #TrackingRef '- bis_4-acetyl-1,1-bipheny-4-yl_butadiyne.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,4-bis(4'-acetyl-[1,1'-biphenyl]-4-yl)buta-1,3-diyne ; _chemical_name_common 1,4-bis(4'-acetyl-(1,1'-biphenyl)-4-yl)buta-1,3-diyne _chemical_melting_point ? _chemical_formula_moiety 'C32 H22 O2' _chemical_formula_sum 'C32 H22 O2' _chemical_formula_weight 438.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.271(7) _cell_length_b 9.707(7) _cell_length_c 20.928(14) _cell_angle_alpha 90.570(11) _cell_angle_beta 97.203(5) _cell_angle_gamma 114.198(13) _cell_volume 1700(2) _cell_formula_units_Z 3 _cell_measurement_temperature 93.15 _cell_measurement_reflns_used 4204 _cell_measurement_theta_min 3.3394 _cell_measurement_theta_max 27.4198 _exptl_crystal_description Platelet _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.68 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 690 _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6489 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_special_details ; The ctystals were recrystalized from chloroform. ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'Rigaku Saturn724' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20748 _diffrn_reflns_av_R_equivalents 0.0871 _diffrn_reflns_av_sigmaI/netI 0.1090 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.47 _reflns_number_total 7713 _reflns_number_gt 3941 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)' _computing_publication_material ;Yadokari-XG 2009 (Wakita,Nemoto et al., 2009) ; _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^)+(0.0557P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7713 _refine_ls_number_parameters 483 _refine_ls_number_restraints 71 _refine_ls_R_factor_all 0.1239 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1405 _refine_ls_wR_factor_gt 0.1153 _refine_ls_goodness_of_fit_ref 0.912 _refine_ls_restrained_S_all 0.914 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.6645(2) 0.08631(17) 0.93119(7) 0.0420(4) Uani 1 1 d . . . C1 C 0.3865(3) 0.0124(2) 0.90031(10) 0.0348(6) Uani 1 1 d . . . H1 H 0.3781 -0.0463 0.9386 0.052 Uiso 1 1 calc R . . H1A H 0.3288 -0.0561 0.8620 0.052 Uiso 1 1 calc R . . H1B H 0.3398 0.0852 0.9056 0.052 Uiso 1 1 calc R . . C2 C 0.5593(3) 0.0959(2) 0.89223(10) 0.0265(5) Uani 1 1 d . . . C3 C 0.6019(3) 0.1945(2) 0.83706(9) 0.0225(5) Uani 1 1 d . . . C4 C 0.7620(3) 0.2733(2) 0.82970(9) 0.0265(5) Uani 1 1 d . . . H4 H 0.8420 0.2616 0.8593 0.032 Uiso 1 1 calc R . . C5 C 0.8066(3) 0.3683(2) 0.78000(9) 0.0238(5) Uani 1 1 d . . . H5 H 0.9164 0.4200 0.7757 0.029 Uiso 1 1 calc R . . C6 C 0.6915(2) 0.3888(2) 0.73615(9) 0.0196(4) Uani 1 1 d . . . C7 C 0.5318(3) 0.3093(2) 0.74307(9) 0.0231(5) Uani 1 1 d . . . H7 H 0.4518 0.3212 0.7135 0.028 Uiso 1 1 calc R . . C8 C 0.4869(3) 0.2124(2) 0.79266(9) 0.0233(5) Uani 1 1 d . . . H8 H 0.3768 0.1581 0.7962 0.028 Uiso 1 1 calc R . . C9 C 0.7400(2) 0.4966(2) 0.68437(8) 0.0197(4) Uani 1 1 d . . . C10 C 0.8740(3) 0.5166(2) 0.65510(9) 0.0226(5) Uani 1 1 d . . . H10 H 0.9315 0.4569 0.6668 0.027 Uiso 1 1 calc R . . C11 C 0.9248(3) 0.6219(2) 0.60918(9) 0.0229(5) Uani 1 1 d . . . H11 H 1.0159 0.6334 0.5897 0.027 Uiso 1 1 calc R . . C12 C 0.8421(3) 0.7111(2) 0.59153(9) 0.0208(5) Uani 1 1 d . . . C13 C 0.7054(3) 0.6887(2) 0.61895(9) 0.0219(5) Uani 1 1 d . . . H13 H 0.6465 0.7466 0.6064 0.026 Uiso 1 1 calc R . . C14 C 0.6543(2) 0.5823(2) 0.66459(9) 0.0215(5) Uani 1 1 d . . . H14 H 0.5602 0.5676 0.6825 0.026 Uiso 1 1 calc R . . C15 C 0.9047(3) 0.8306(2) 0.54890(9) 0.0233(5) Uani 1 1 d . . . C16 C 0.9647(3) 0.9382(2) 0.51763(9) 0.0234(5) Uani 1 1 d . . . O2 O 0.22061(19) -0.38324(15) 0.80196(7) 0.0333(4) Uani 1 1 d . . . C17 C 0.4837(3) -0.3629(2) 0.83669(10) 0.0376(6) Uani 1 1 d . . . H17 H 0.4288 -0.4457 0.8633 0.056 Uiso 1 1 calc R . . H17A H 0.5579 -0.2742 0.8647 0.056 Uiso 1 1 calc R . . H17B H 0.5433 -0.3947 0.8087 0.056 Uiso 1 1 calc R . . C18 C 0.3629(3) -0.3231(2) 0.79585(9) 0.0250(5) Uani 1 1 d . . . C19 C 0.4183(3) -0.2106(2) 0.74639(9) 0.0217(5) Uani 1 1 d . . . C20 C 0.5796(3) -0.1212(2) 0.74434(9) 0.0242(5) Uani 1 1 d . . . H20 H 0.6584 -0.1302 0.7756 0.029 Uiso 1 1 calc R . . C21 C 0.6261(3) -0.0192(2) 0.69687(9) 0.0238(5) Uani 1 1 d . . . H21 H 0.7364 0.0417 0.6963 0.029 Uiso 1 1 calc R . . C22 C 0.5122(3) -0.0048(2) 0.64981(9) 0.0212(5) Uani 1 1 d . . . C23 C 0.3518(3) -0.0942(2) 0.65234(9) 0.0262(5) Uani 1 1 d . . . H23 H 0.2730 -0.0864 0.6207 0.031 Uiso 1 1 calc R . . C24 C 0.3048(3) -0.1948(2) 0.70039(9) 0.0260(5) Uani 1 1 d . . . H24 H 0.1943 -0.2532 0.7018 0.031 Uiso 1 1 calc R . . C25 C 0.5627(3) 0.1039(2) 0.59917(9) 0.0215(5) Uani 1 1 d . . . C26 C 0.7039(3) 0.1323(2) 0.57352(9) 0.0268(5) Uani 1 1 d . . . H26 H 0.7666 0.0790 0.5879 0.032 Uiso 1 1 calc R . . C27 C 0.7535(3) 0.2369(2) 0.52746(9) 0.0272(5) Uani 1 1 d . . . H27 H 0.8494 0.2542 0.5105 0.033 Uiso 1 1 calc R . . C28 C 0.6634(3) 0.3171(2) 0.50586(9) 0.0237(5) Uani 1 1 d . . . C29 C 0.5221(3) 0.2891(2) 0.53088(9) 0.0237(5) Uani 1 1 d . . . H29 H 0.4598 0.3428 0.5166 0.028 Uiso 1 1 calc R . . C30 C 0.4722(3) 0.1832(2) 0.57659(9) 0.0234(5) Uani 1 1 d . . . H30 H 0.3751 0.1642 0.5928 0.028 Uiso 1 1 calc R . . C31 C 0.7166(3) 0.4277(2) 0.45932(9) 0.0229(5) Uani 1 1 d . . . C32 C 0.7604(3) 0.5203(2) 0.41989(9) 0.0250(5) Uani 1 1 d . . . C33 C 0.8090(3) 0.6231(2) 0.37384(9) 0.0246(5) Uani 1 1 d . . . C34 C 0.8492(2) 0.7119(2) 0.33244(9) 0.0239(5) Uani 1 1 d . . . C35 C 0.8953(2) 0.8148(2) 0.28242(9) 0.0226(5) Uani 1 1 d . . . C36 C 0.9508(3) 0.9710(2) 0.29582(9) 0.0252(5) Uani 1 1 d . . . H36 H 0.9563 1.0095 0.3384 0.030 Uiso 1 1 calc R . . C37 C 0.9976(3) 1.0697(2) 0.24763(9) 0.0242(5) Uani 1 1 d . . . H37 H 1.0352 1.1754 0.2577 0.029 Uiso 1 1 calc R . . C38 C 0.9905(2) 1.0167(2) 0.18425(9) 0.0217(5) Uani 1 1 d . . . C39 C 0.9291(2) 0.8597(2) 0.17109(9) 0.0240(5) Uani 1 1 d . . . H39 H 0.9187 0.8207 0.1281 0.029 Uiso 1 1 calc R . . C40 C 0.8834(2) 0.7602(2) 0.21900(9) 0.0238(5) Uani 1 1 d . . . H40 H 0.8438 0.6543 0.2088 0.029 Uiso 1 1 calc R . . C41 C 1.0502(3) 1.1214(2) 0.13301(9) 0.0238(5) Uani 1 1 d . . . C42 C 1.0502(3) 1.2643(2) 0.13351(10) 0.0332(6) Uani 1 1 d . . . H42 H 1.0050 1.2954 0.1661 0.040 Uiso 1 1 calc R . . C43 C 1.1160(3) 1.3625(2) 0.08652(10) 0.0415(7) Uani 1 1 d . . . H43 H 1.1157 1.4603 0.0877 0.050 Uiso 1 1 calc R . . C44 C 1.1820(3) 1.3200(2) 0.03801(10) 0.0344(6) Uani 1 1 d D A . C45 C 1.1800(3) 1.1759(2) 0.03667(9) 0.0307(5) Uani 1 1 d . . . H45 H 1.2234 1.1443 0.0036 0.037 Uiso 1 1 calc R . . C46 C 1.1146(3) 1.0780(2) 0.08373(9) 0.0277(5) Uani 1 1 d . . . H46 H 1.1137 0.9798 0.0823 0.033 Uiso 1 1 calc R . . C47 C 1.2612(4) 1.4236(3) -0.01159(11) 0.0455(7) Uani 1 1 d DU . . O3B O 1.334(3) 1.3887(19) -0.0501(9) 0.032(3) Uani 0.34(3) 1 d PDU A 2 C48A C 1.303(2) 1.5902(8) -0.0033(5) 0.054(2) Uani 0.66(3) 1 d PDU A 1 H48A H 1.3459 1.6394 -0.0416 0.081 Uiso 0.66(3) 1 calc PR A 1 H48B H 1.3834 1.6345 0.0349 0.081 Uiso 0.66(3) 1 calc PR A 1 H48C H 1.2070 1.6053 0.0022 0.081 Uiso 0.66(3) 1 calc PR A 1 C48B C 1.234(3) 1.572(2) -0.0172(11) 0.055(4) Uani 0.34(3) 1 d PDU A 2 H48D H 1.2685 1.6182 -0.0572 0.083 Uiso 0.34(3) 1 calc PR A 2 H48E H 1.2967 1.6433 0.0198 0.083 Uiso 0.34(3) 1 calc PR A 2 H48F H 1.1206 1.5481 -0.0176 0.083 Uiso 0.34(3) 1 calc PR A 2 O3A O 1.3042(17) 1.3722(12) -0.0559(5) 0.058(3) Uani 0.66(3) 1 d PDU A 1 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 0.0387(11) 0.0563(10) 0.0400(9) 0.0264(8) 0.0122(8) 0.0263(9) C1 0.0349(16) 0.0394(13) 0.0316(12) 0.0164(10) 0.0120(11) 0.0146(12) C2 0.0320(15) 0.0289(11) 0.0242(10) 0.0075(9) 0.0090(9) 0.0168(11) C3 0.0254(14) 0.0233(10) 0.0231(10) 0.0070(9) 0.0081(9) 0.0129(10) C4 0.0272(14) 0.0300(11) 0.0259(10) 0.0068(9) 0.0024(9) 0.0157(11) C5 0.0214(13) 0.0260(11) 0.0255(10) 0.0061(9) 0.0077(9) 0.0100(10) C6 0.0191(13) 0.0190(10) 0.0208(9) 0.0027(8) 0.0053(8) 0.0072(9) C7 0.0222(13) 0.0266(11) 0.0211(10) 0.0047(9) 0.0028(9) 0.0108(10) C8 0.0187(13) 0.0248(10) 0.0258(10) 0.0039(9) 0.0089(9) 0.0066(10) C9 0.0188(12) 0.0191(10) 0.0183(9) 0.0004(8) 0.0039(8) 0.0047(9) C10 0.0235(13) 0.0221(10) 0.0234(10) 0.0049(8) 0.0052(9) 0.0102(10) C11 0.0203(13) 0.0240(10) 0.0222(10) 0.0032(8) 0.0065(9) 0.0060(10) C12 0.0210(13) 0.0214(10) 0.0172(9) 0.0031(8) 0.0043(8) 0.0055(10) C13 0.0229(13) 0.0234(10) 0.0215(10) 0.0025(8) 0.0031(9) 0.0115(10) C14 0.0198(13) 0.0236(10) 0.0213(10) 0.0032(8) 0.0057(8) 0.0083(10) C15 0.0245(13) 0.0265(11) 0.0200(10) 0.0020(9) 0.0030(9) 0.0115(10) C16 0.0242(13) 0.0271(11) 0.0214(10) 0.0041(9) 0.0057(9) 0.0124(10) O2 0.0298(11) 0.0302(8) 0.0384(9) 0.0123(7) 0.0131(7) 0.0084(8) C17 0.0375(16) 0.0376(13) 0.0330(12) 0.0194(10) 0.0069(11) 0.0099(12) C18 0.0314(15) 0.0207(11) 0.0223(10) 0.0021(9) 0.0074(10) 0.0093(11) C19 0.0226(13) 0.0193(10) 0.0220(10) 0.0036(8) 0.0083(9) 0.0061(10) C20 0.0258(14) 0.0235(11) 0.0241(10) 0.0047(9) 0.0046(9) 0.0106(10) C21 0.0207(13) 0.0232(10) 0.0281(11) 0.0062(9) 0.0082(9) 0.0083(10) C22 0.0244(13) 0.0202(10) 0.0204(10) 0.0027(8) 0.0069(9) 0.0094(10) C23 0.0272(14) 0.0244(11) 0.0248(10) 0.0047(9) 0.0017(9) 0.0092(10) C24 0.0190(13) 0.0267(11) 0.0284(11) 0.0046(9) 0.0049(9) 0.0051(10) C25 0.0256(13) 0.0189(10) 0.0211(10) 0.0036(8) 0.0078(9) 0.0091(10) C26 0.0334(15) 0.0277(11) 0.0273(11) 0.0091(9) 0.0093(10) 0.0192(11) C27 0.0285(14) 0.0285(11) 0.0303(11) 0.0097(9) 0.0146(10) 0.0142(11) C28 0.0296(14) 0.0229(10) 0.0208(10) 0.0049(8) 0.0083(9) 0.0115(10) C29 0.0259(14) 0.0256(11) 0.0216(10) 0.0051(9) 0.0030(9) 0.0128(10) C30 0.0217(13) 0.0264(11) 0.0218(10) 0.0043(9) 0.0046(9) 0.0093(10) C31 0.0214(13) 0.0269(11) 0.0237(10) 0.0032(9) 0.0052(9) 0.0126(10) C32 0.0248(14) 0.0291(11) 0.0241(10) 0.0053(9) 0.0058(9) 0.0135(10) C33 0.0230(13) 0.0290(11) 0.0252(10) 0.0063(9) 0.0059(9) 0.0133(10) C34 0.0183(13) 0.0290(11) 0.0275(10) 0.0047(9) 0.0045(9) 0.0126(10) C35 0.0197(13) 0.0230(11) 0.0244(10) 0.0086(9) 0.0060(9) 0.0070(10) C36 0.0251(14) 0.0291(11) 0.0203(10) 0.0023(9) 0.0041(9) 0.0097(10) C37 0.0241(13) 0.0207(10) 0.0255(10) 0.0040(9) 0.0051(9) 0.0065(10) C38 0.0187(12) 0.0221(10) 0.0233(10) 0.0054(9) 0.0047(9) 0.0070(10) C39 0.0225(13) 0.0265(11) 0.0237(10) 0.0044(9) 0.0070(9) 0.0100(10) C40 0.0224(13) 0.0200(10) 0.0289(11) 0.0054(9) 0.0060(9) 0.0079(10) C41 0.0246(13) 0.0234(11) 0.0193(10) 0.0033(8) 0.0010(9) 0.0065(10) C42 0.0456(17) 0.0309(12) 0.0261(11) 0.0061(10) 0.0147(11) 0.0161(12) C43 0.064(2) 0.0272(12) 0.0322(12) 0.0080(10) 0.0116(12) 0.0160(13) C44 0.0457(17) 0.0252(12) 0.0216(11) 0.0027(9) 0.0034(11) 0.0042(12) C45 0.0339(15) 0.0307(12) 0.0221(10) 0.0014(9) 0.0069(10) 0.0073(11) C46 0.0322(14) 0.0245(11) 0.0234(10) 0.0054(9) 0.0065(9) 0.0079(10) C47 0.066(2) 0.0326(13) 0.0268(12) 0.0041(11) 0.0123(13) 0.0077(13) O3B 0.043(6) 0.014(4) 0.030(5) 0.006(3) 0.007(4) 0.003(4) C48A 0.076(6) 0.034(3) 0.047(3) 0.014(2) 0.027(3) 0.011(3) C48B 0.066(9) 0.046(6) 0.056(7) 0.025(5) 0.025(6) 0.020(6) O3A 0.076(6) 0.048(4) 0.025(3) 0.000(2) 0.021(3) -0.004(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 C2 1.225(2) . ? C1 C2 1.503(3) . ? C1 H1 0.9800 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C2 C3 1.494(3) . ? C3 C8 1.392(3) . ? C3 C4 1.393(3) . ? C4 C5 1.385(3) . ? C4 H4 0.9500 . ? C5 C6 1.397(3) . ? C5 H5 0.9500 . ? C6 C7 1.388(3) . ? C6 C9 1.494(3) . ? C7 C8 1.394(3) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.397(3) . ? C9 C14 1.401(3) . ? C10 C11 1.389(3) . ? C10 H10 0.9500 . ? C11 C12 1.398(3) . ? C11 H11 0.9500 . ? C12 C13 1.393(3) . ? C12 C15 1.441(3) . ? C13 C14 1.391(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.208(3) . ? C16 C16 1.380(4) 2_776 ? O2 C18 1.228(3) . ? C17 C18 1.502(3) . ? C17 H17 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 C19 1.491(3) . ? C19 C24 1.392(3) . ? C19 C20 1.395(3) . ? C20 C21 1.390(3) . ? C20 H20 0.9500 . ? C21 C22 1.402(3) . ? C21 H21 0.9500 . ? C22 C23 1.389(3) . ? C22 C25 1.483(3) . ? C23 C24 1.392(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.398(3) . ? C25 C26 1.401(3) . ? C26 C27 1.386(3) . ? C26 H26 0.9500 . ? C27 C28 1.397(3) . ? C27 H27 0.9500 . ? C28 C29 1.395(3) . ? C28 C31 1.433(3) . ? C29 C30 1.388(3) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.205(3) . ? C32 C33 1.374(3) . ? C33 C34 1.210(3) . ? C34 C35 1.435(3) . ? C35 C40 1.399(3) . ? C35 C36 1.400(3) . ? C36 C37 1.382(3) . ? C36 H36 0.9500 . ? C37 C38 1.402(3) . ? C37 H37 0.9500 . ? C38 C39 1.402(3) . ? C38 C41 1.483(3) . ? C39 C40 1.381(3) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.388(3) . ? C41 C46 1.396(3) . ? C42 C43 1.393(3) . ? C42 H42 0.9500 . ? C43 C44 1.390(3) . ? C43 H43 0.9500 . ? C44 C45 1.391(3) . ? C44 C47 1.495(3) . ? C45 C46 1.392(3) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 O3A 1.230(10) . ? C47 O3B 1.239(18) . ? C47 C48A 1.503(7) . ? C47 C48B 1.565(15) . ? C48A H48A 0.9800 . ? C48A H48B 0.9800 . ? C48A H48C 0.9800 . ? C48B H48D 0.9800 . ? C48B H48E 0.9800 . ? C48B H48F 0.9800 . ? 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 C2 C1 H1 109.5 . . ? C2 C1 H1A 109.5 . . ? H1 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C2 C3 120.2(2) . . ? O1 C2 C1 120.57(19) . . ? C3 C2 C1 119.16(18) . . ? C8 C3 C4 118.29(18) . . ? C8 C3 C2 122.3(2) . . ? C4 C3 C2 119.40(18) . . ? C5 C4 C3 121.18(19) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C4 C5 C6 120.6(2) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C7 C6 C5 118.24(18) . . ? C7 C6 C9 121.16(18) . . ? C5 C6 C9 120.58(19) . . ? C6 C7 C8 121.14(19) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C3 C8 C7 120.5(2) . . ? C3 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C10 C9 C14 118.18(18) . . ? C10 C9 C6 120.82(18) . . ? C14 C9 C6 121.00(19) . . ? C11 C10 C9 121.28(19) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C10 C11 C12 120.2(2) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C13 C12 C11 118.95(18) . . ? C13 C12 C15 121.15(18) . . ? C11 C12 C15 119.8(2) . . ? C14 C13 C12 120.68(19) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C9 120.7(2) . . ? C13 C14 H14 119.7 . . ? C9 C14 H14 119.7 . . ? C16 C15 C12 174.6(2) . . ? C15 C16 C16 179.2(3) . 2_776 ? C18 C17 H17 109.5 . . ? C18 C17 H17A 109.5 . . ? H17 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O2 C18 C19 120.18(19) . . ? O2 C18 C17 121.16(19) . . ? C19 C18 C17 118.6(2) . . ? C24 C19 C20 118.84(18) . . ? C24 C19 C18 118.8(2) . . ? C20 C19 C18 122.39(19) . . ? C21 C20 C19 120.48(19) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 120.8(2) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C23 C22 C21 118.22(18) . . ? C23 C22 C25 121.23(18) . . ? C21 C22 C25 120.5(2) . . ? C22 C23 C24 121.11(19) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C23 C24 C19 120.5(2) . . ? C23 C24 H24 119.8 . . ? C19 C24 H24 119.8 . . ? C30 C25 C26 118.15(18) . . ? C30 C25 C22 121.0(2) . . ? C26 C25 C22 120.89(18) . . ? C27 C26 C25 121.00(19) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 C28 120.4(2) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C29 C28 C27 119.03(18) . . ? C29 C28 C31 120.58(19) . . ? C27 C28 C31 120.4(2) . . ? C30 C29 C28 120.33(19) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C30 C25 121.1(2) . . ? C29 C30 H30 119.5 . . ? C25 C30 H30 119.5 . . ? C32 C31 C28 179.5(3) . . ? C31 C32 C33 178.7(2) . . ? C34 C33 C32 178.7(2) . . ? C33 C34 C35 178.9(2) . . ? C40 C35 C36 118.75(17) . . ? C40 C35 C34 120.40(17) . . ? C36 C35 C34 120.84(18) . . ? C37 C36 C35 120.55(18) . . ? C37 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C36 C37 C38 121.24(18) . . ? C36 C37 H37 119.4 . . ? C38 C37 H37 119.4 . . ? C39 C38 C37 117.50(17) . . ? C39 C38 C41 120.56(18) . . ? C37 C38 C41 121.91(17) . . ? C40 C39 C38 121.68(18) . . ? C40 C39 H39 119.2 . . ? C38 C39 H39 119.2 . . ? C39 C40 C35 120.20(18) . . ? C39 C40 H40 119.9 . . ? C35 C40 H40 119.9 . . ? C42 C41 C46 118.38(19) . . ? C42 C41 C38 122.2(2) . . ? C46 C41 C38 119.33(18) . . ? C41 C42 C43 120.4(2) . . ? C41 C42 H42 119.8 . . ? C43 C42 H42 119.8 . . ? C44 C43 C42 121.1(2) . . ? C44 C43 H43 119.4 . . ? C42 C43 H43 119.4 . . ? C43 C44 C45 118.7(2) . . ? C43 C44 C47 123.2(2) . . ? C45 C44 C47 118.0(2) . . ? C44 C45 C46 120.1(2) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C45 C46 C41 121.27(19) . . ? C45 C46 H46 119.4 . . ? C41 C46 H46 119.4 . . ? O3A C47 O3B 12.4(15) . . ? O3A C47 C44 118.6(5) . . ? O3B C47 C44 122.0(7) . . ? O3A C47 C48A 120.7(6) . . ? O3B C47 C48A 114.8(8) . . ? C44 C47 C48A 120.3(4) . . ? O3A C47 C48B 121.6(8) . . ? O3B C47 C48B 121.1(9) . . ? C44 C47 C48B 116.7(7) . . ? C48A C47 C48B 23.1(7) . . ? C47 C48A H48A 109.5 . . ? C47 C48A H48B 109.5 . . ? C47 C48A H48C 109.5 . . ? C47 C48B H48D 109.5 . . ? C47 C48B H48E 109.5 . . ? H48D C48B H48E 109.5 . . ? C47 C48B H48F 109.5 . . ? H48D C48B H48F 109.5 . . ? H48E C48B H48F 109.5 . . ? 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 C2 C3 C8 -178.11(19) . . . . ? C1 C2 C3 C8 0.1(3) . . . . ? O1 C2 C3 C4 1.2(3) . . . . ? C1 C2 C3 C4 179.39(19) . . . . ? C8 C3 C4 C5 0.7(3) . . . . ? C2 C3 C4 C5 -178.65(17) . . . . ? C3 C4 C5 C6 0.7(3) . . . . ? C4 C5 C6 C7 -1.2(3) . . . . ? C4 C5 C6 C9 177.23(17) . . . . ? C5 C6 C7 C8 0.5(3) . . . . ? C9 C6 C7 C8 -177.94(17) . . . . ? C4 C3 C8 C7 -1.4(3) . . . . ? C2 C3 C8 C7 177.91(17) . . . . ? C6 C7 C8 C3 0.8(3) . . . . ? C7 C6 C9 C10 -146.9(2) . . . . ? C5 C6 C9 C10 34.7(3) . . . . ? C7 C6 C9 C14 34.2(3) . . . . ? C5 C6 C9 C14 -144.19(19) . . . . ? C14 C9 C10 C11 2.2(3) . . . . ? C6 C9 C10 C11 -176.78(16) . . . . ? C9 C10 C11 C12 0.3(3) . . . . ? C10 C11 C12 C13 -2.3(3) . . . . ? C10 C11 C12 C15 173.67(17) . . . . ? C11 C12 C13 C14 1.8(3) . . . . ? C15 C12 C13 C14 -174.06(16) . . . . ? C12 C13 C14 C9 0.6(3) . . . . ? C10 C9 C14 C13 -2.6(3) . . . . ? C6 C9 C14 C13 176.33(16) . . . . ? C13 C12 C15 C16 90(2) . . . . ? C11 C12 C15 C16 -86(2) . . . . ? C12 C15 C16 C16 43(24) . . . 2_776 ? O2 C18 C19 C24 -11.1(3) . . . . ? C17 C18 C19 C24 167.78(19) . . . . ? O2 C18 C19 C20 169.30(19) . . . . ? C17 C18 C19 C20 -11.8(3) . . . . ? C24 C19 C20 C21 -0.5(3) . . . . ? C18 C19 C20 C21 179.13(18) . . . . ? C19 C20 C21 C22 -0.6(3) . . . . ? C20 C21 C22 C23 0.7(3) . . . . ? C20 C21 C22 C25 -179.81(17) . . . . ? C21 C22 C23 C24 0.3(3) . . . . ? C25 C22 C23 C24 -179.20(18) . . . . ? C22 C23 C24 C19 -1.4(3) . . . . ? C20 C19 C24 C23 1.5(3) . . . . ? C18 C19 C24 C23 -178.16(17) . . . . ? C23 C22 C25 C30 35.7(3) . . . . ? C21 C22 C25 C30 -143.8(2) . . . . ? C23 C22 C25 C26 -145.5(2) . . . . ? C21 C22 C25 C26 35.0(3) . . . . ? C30 C25 C26 C27 0.6(3) . . . . ? C22 C25 C26 C27 -178.24(17) . . . . ? C25 C26 C27 C28 0.3(3) . . . . ? C26 C27 C28 C29 -0.6(3) . . . . ? C26 C27 C28 C31 178.58(18) . . . . ? C27 C28 C29 C30 0.1(3) . . . . ? C31 C28 C29 C30 -179.15(17) . . . . ? C28 C29 C30 C25 0.8(3) . . . . ? C26 C25 C30 C29 -1.1(3) . . . . ? C22 C25 C30 C29 177.66(17) . . . . ? C29 C28 C31 C32 -56(34) . . . . ? C27 C28 C31 C32 124(34) . . . . ? C28 C31 C32 C33 -45(41) . . . . ? C31 C32 C33 C34 35(19) . . . . ? C32 C33 C34 C35 -28(21) . . . . ? C33 C34 C35 C40 -15(12) . . . . ? C33 C34 C35 C36 164(12) . . . . ? C40 C35 C36 C37 -2.0(3) . . . . ? C34 C35 C36 C37 178.9(2) . . . . ? C35 C36 C37 C38 0.2(3) . . . . ? C36 C37 C38 C39 2.1(3) . . . . ? C36 C37 C38 C41 -175.9(2) . . . . ? C37 C38 C39 C40 -2.8(3) . . . . ? C41 C38 C39 C40 175.3(2) . . . . ? C38 C39 C40 C35 1.0(3) . . . . ? C36 C35 C40 C39 1.4(3) . . . . ? C34 C35 C40 C39 -179.5(2) . . . . ? C39 C38 C41 C42 153.0(2) . . . . ? C37 C38 C41 C42 -29.1(3) . . . . ? C39 C38 C41 C46 -29.5(3) . . . . ? C37 C38 C41 C46 148.4(2) . . . . ? C46 C41 C42 C43 -1.3(3) . . . . ? C38 C41 C42 C43 176.2(2) . . . . ? C41 C42 C43 C44 0.4(4) . . . . ? C42 C43 C44 C45 0.6(4) . . . . ? C42 C43 C44 C47 -176.9(2) . . . . ? C43 C44 C45 C46 -0.8(3) . . . . ? C47 C44 C45 C46 176.9(2) . . . . ? C44 C45 C46 C41 -0.1(3) . . . . ? C42 C41 C46 C45 1.2(3) . . . . ? C38 C41 C46 C45 -176.42(19) . . . . ? C43 C44 C47 O3A -174.0(8) . . . . ? C45 C44 C47 O3A 8.5(8) . . . . ? C43 C44 C47 O3B 172.2(13) . . . . ? C45 C44 C47 O3B -5.3(13) . . . . ? C43 C44 C47 C48A 12.5(9) . . . . ? C45 C44 C47 C48A -165.0(8) . . . . ? C43 C44 C47 C48B -13.5(13) . . . . ? C45 C44 C47 C48B 168.9(13) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.301 _refine_diff_density_min -0.273 _refine_diff_density_rms 0.057 _chemical_absolute_configuration ? _iucr_refine_instructions_details ; TITL REM Yadorkari-X generated CELL 0.71075 9.2709 9.7075 20.9279 90.5703 97.2029 114.1980 ZERR 3.0 0.0069 0.0068 0.0137 0.0106 0.0050 0.0130 LATT 1 REM SPGR P-1 triclinic SFAC C H O UNIT 96 66 6 SIZE 0.68 0.20 0.05 TEMP -179.8 L.S. 5 FMAP 2 PLAN -20 ACTA CONF BOND $H MERG 2 DELU 0.01 0.01 O3A C47 C48A SIMU 0.02 0.04 1.7 O3A C47 C48A ISOR 0.01 0.01 O3A C47 C48A DELU 0.01 0.01 O3B C47 C48B SIMU 0.02 0.04 1.7 O3B C47 C48B ISOR 0.01 0.01 O3B C47 C48B SADI 0.05 C47 C48A C47 C48B SADI 0.05 C47 O3A C47 O3B SADI 0.05 O3A C48A O3B C48B FLAT 0.1 C44 C47 C48A O3A FLAT 0.1 C44 C47 C48B O3B WGHT 0.055700 FVAR 4.90667 0.66225 O1 3 0.664452 0.086306 0.931188 11.00000 0.03870 0.05630 = 0.03998 0.02636 0.01225 0.02634 C1 1 0.386470 0.012407 0.900306 11.00000 0.03486 0.03942 = 0.03164 0.01638 0.01205 0.01456 AFIX 137 H1 2 0.378120 -0.046305 0.938565 11.00000 -1.50000 H1A 2 0.328792 -0.056123 0.862033 11.00000 -1.50000 H1B 2 0.339800 0.085234 0.905584 11.00000 -1.50000 AFIX 0 C2 1 0.559342 0.095876 0.892229 11.00000 0.03200 0.02892 = 0.02417 0.00745 0.00900 0.01681 C3 1 0.601887 0.194537 0.837056 11.00000 0.02535 0.02330 = 0.02313 0.00696 0.00810 0.01291 C4 1 0.761964 0.273263 0.829701 11.00000 0.02718 0.02996 = 0.02585 0.00682 0.00236 0.01572 AFIX 43 H4 2 0.841994 0.261563 0.859308 11.00000 -1.20000 AFIX 0 C5 1 0.806558 0.368302 0.779997 11.00000 0.02140 0.02602 = 0.02549 0.00608 0.00767 0.01005 AFIX 43 H5 2 0.916423 0.420029 0.775674 11.00000 -1.20000 AFIX 0 C6 1 0.691450 0.388808 0.736148 11.00000 0.01912 0.01901 = 0.02075 0.00267 0.00533 0.00724 C7 1 0.531827 0.309335 0.743075 11.00000 0.02218 0.02662 = 0.02114 0.00465 0.00281 0.01080 AFIX 43 H7 2 0.451842 0.321217 0.713509 11.00000 -1.20000 AFIX 0 C8 1 0.486861 0.212402 0.792656 11.00000 0.01868 0.02477 = 0.02581 0.00388 0.00894 0.00656 AFIX 43 H8 2 0.376840 0.158098 0.796174 11.00000 -1.20000 AFIX 0 C9 1 0.740010 0.496610 0.684369 11.00000 0.01876 0.01913 = 0.01835 0.00037 0.00390 0.00469 C10 1 0.873995 0.516564 0.655097 11.00000 0.02351 0.02215 = 0.02344 0.00493 0.00524 0.01021 AFIX 43 H10 2 0.931482 0.456919 0.666821 11.00000 -1.20000 AFIX 0 C11 1 0.924787 0.621929 0.609178 11.00000 0.02030 0.02400 = 0.02219 0.00318 0.00649 0.00597 AFIX 43 H11 2 1.015944 0.633381 0.589724 11.00000 -1.20000 AFIX 0 C12 1 0.842097 0.711146 0.591528 11.00000 0.02096 0.02142 = 0.01725 0.00310 0.00428 0.00549 C13 1 0.705407 0.688694 0.618952 11.00000 0.02291 0.02340 = 0.02150 0.00247 0.00312 0.01155 AFIX 43 H13 2 0.646524 0.746641 0.606359 11.00000 -1.20000 AFIX 0 C14 1 0.654258 0.582286 0.664587 11.00000 0.01977 0.02361 = 0.02130 0.00319 0.00574 0.00833 AFIX 43 H14 2 0.560206 0.567593 0.682513 11.00000 -1.20000 AFIX 0 C15 1 0.904733 0.830594 0.548900 11.00000 0.02448 0.02648 = 0.02000 0.00196 0.00305 0.01151 C16 1 0.964722 0.938250 0.517627 11.00000 0.02421 0.02710 = 0.02144 0.00406 0.00567 0.01237 O2 3 0.220609 -0.383238 0.801965 11.00000 0.02979 0.03019 = 0.03844 0.01234 0.01314 0.00845 C17 1 0.483699 -0.362887 0.836685 11.00000 0.03746 0.03761 = 0.03305 0.01939 0.00691 0.00994 AFIX 137 H17 2 0.428834 -0.445666 0.863331 11.00000 -1.50000 H17A 2 0.557863 -0.274188 0.864651 11.00000 -1.50000 H17B 2 0.543254 -0.394749 0.808723 11.00000 -1.50000 AFIX 0 C18 1 0.362856 -0.323131 0.795846 11.00000 0.03145 0.02066 = 0.02227 0.00213 0.00742 0.00925 C19 1 0.418280 -0.210584 0.746391 11.00000 0.02262 0.01931 = 0.02197 0.00362 0.00827 0.00614 C20 1 0.579643 -0.121228 0.744341 11.00000 0.02578 0.02345 = 0.02411 0.00474 0.00462 0.01063 AFIX 43 H20 2 0.658379 -0.130198 0.775627 11.00000 -1.20000 AFIX 0 C21 1 0.626083 -0.019177 0.696870 11.00000 0.02072 0.02316 = 0.02811 0.00617 0.00816 0.00832 AFIX 43 H21 2 0.736369 0.041652 0.696296 11.00000 -1.20000 AFIX 0 C22 1 0.512228 -0.004846 0.649805 11.00000 0.02438 0.02020 = 0.02041 0.00270 0.00691 0.00943 C23 1 0.351844 -0.094163 0.652341 11.00000 0.02723 0.02440 = 0.02484 0.00470 0.00165 0.00921 AFIX 43 H23 2 0.272973 -0.086402 0.620744 11.00000 -1.20000 AFIX 0 C24 1 0.304751 -0.194830 0.700392 11.00000 0.01895 0.02674 = 0.02843 0.00463 0.00490 0.00514 AFIX 43 H24 2 0.194330 -0.253232 0.701819 11.00000 -1.20000 AFIX 0 C25 1 0.562666 0.103932 0.599172 11.00000 0.02560 0.01889 = 0.02112 0.00357 0.00784 0.00911 C26 1 0.703891 0.132281 0.573523 11.00000 0.03345 0.02770 = 0.02728 0.00907 0.00928 0.01924 AFIX 43 H26 2 0.766604 0.078971 0.587925 11.00000 -1.20000 AFIX 0 C27 1 0.753521 0.236912 0.527457 11.00000 0.02845 0.02851 = 0.03026 0.00971 0.01455 0.01422 AFIX 43 H27 2 0.849376 0.254248 0.510457 11.00000 -1.20000 AFIX 0 C28 1 0.663426 0.317071 0.505861 11.00000 0.02962 0.02286 = 0.02075 0.00488 0.00830 0.01146 C29 1 0.522141 0.289078 0.530876 11.00000 0.02588 0.02559 = 0.02163 0.00512 0.00302 0.01284 AFIX 43 H29 2 0.459775 0.342767 0.516551 11.00000 -1.20000 AFIX 0 C30 1 0.472244 0.183179 0.576586 11.00000 0.02173 0.02639 = 0.02182 0.00429 0.00464 0.00927 AFIX 43 H30 2 0.375066 0.164241 0.592787 11.00000 -1.20000 AFIX 0 C31 1 0.716638 0.427707 0.459316 11.00000 0.02137 0.02692 = 0.02372 0.00320 0.00515 0.01263 C32 1 0.760414 0.520267 0.419886 11.00000 0.02477 0.02908 = 0.02409 0.00526 0.00580 0.01349 C33 1 0.808973 0.623098 0.373837 11.00000 0.02302 0.02900 = 0.02517 0.00633 0.00595 0.01330 C34 1 0.849206 0.711911 0.332440 11.00000 0.01833 0.02904 = 0.02754 0.00466 0.00447 0.01255 C35 1 0.895301 0.814752 0.282416 11.00000 0.01970 0.02295 = 0.02438 0.00859 0.00600 0.00698 C36 1 0.950758 0.970980 0.295823 11.00000 0.02508 0.02907 = 0.02029 0.00232 0.00414 0.00971 AFIX 43 H36 2 0.956286 1.009523 0.338393 11.00000 -1.20000 AFIX 0 C37 1 0.997554 1.069663 0.247633 11.00000 0.02411 0.02065 = 0.02552 0.00399 0.00509 0.00648 AFIX 43 H37 2 1.035180 1.175365 0.257656 11.00000 -1.20000 AFIX 0 C38 1 0.990530 1.016682 0.184250 11.00000 0.01869 0.02209 = 0.02334 0.00544 0.00469 0.00699 C39 1 0.929125 0.859656 0.171091 11.00000 0.02251 0.02652 = 0.02372 0.00435 0.00696 0.00997 AFIX 43 H39 2 0.918676 0.820660 0.128126 11.00000 -1.20000 AFIX 0 C40 1 0.883415 0.760156 0.218998 11.00000 0.02236 0.02001 = 0.02887 0.00539 0.00599 0.00787 AFIX 43 H40 2 0.843782 0.654313 0.208837 11.00000 -1.20000 AFIX 0 C41 1 1.050244 1.121354 0.133011 11.00000 0.02462 0.02337 = 0.01934 0.00326 0.00096 0.00647 C42 1 1.050194 1.264338 0.133510 11.00000 0.04556 0.03087 = 0.02613 0.00612 0.01469 0.01611 AFIX 43 H42 2 1.005015 1.295404 0.166095 11.00000 -1.20000 AFIX 0 C43 1 1.115981 1.362530 0.086525 11.00000 0.06373 0.02721 = 0.03222 0.00797 0.01161 0.01596 AFIX 43 H43 2 1.115705 1.460277 0.087660 11.00000 -1.20000 AFIX 0 C44 1 1.182025 1.319956 0.038008 11.00000 0.04575 0.02523 = 0.02157 0.00275 0.00344 0.00423 C45 1 1.180034 1.175915 0.036667 11.00000 0.03395 0.03067 = 0.02208 0.00140 0.00692 0.00727 AFIX 43 H45 2 1.223418 1.144290 0.003574 11.00000 -1.20000 AFIX 0 C46 1 1.114582 1.078028 0.083729 11.00000 0.03217 0.02449 = 0.02340 0.00541 0.00654 0.00791 AFIX 43 H46 2 1.113685 0.979833 0.082278 11.00000 -1.20000 AFIX 0 C47 1 1.261240 1.423585 -0.011586 11.00000 0.06597 0.03265 = 0.02684 0.00410 0.01234 0.00769 PART 2 O3B 3 1.333859 1.388703 -0.050075 -21.00000 0.04348 0.01354 = 0.03041 0.00630 0.00654 0.00261 PART 1 C48A 1 1.303032 1.590207 -0.003328 21.00000 0.07572 0.03354 = 0.04654 0.01359 0.02717 0.01112 AFIX 137 H48A 2 1.345927 1.639416 -0.041622 21.00000 -1.50000 H48B 2 1.383440 1.634484 0.034865 21.00000 -1.50000 H48C 2 1.206970 1.605338 0.002156 21.00000 -1.50000 PART 2 AFIX 0 C48B 1 1.234245 1.572192 -0.017171 -21.00000 0.06565 0.04611 = 0.05611 0.02481 0.02471 0.01964 AFIX 137 H48D 2 1.268550 1.618196 -0.057206 -21.00000 -1.50000 H48E 2 1.296680 1.643287 0.019828 -21.00000 -1.50000 H48F 2 1.120601 1.548147 -0.017633 -21.00000 -1.50000 PART 1 AFIX 0 O3A 3 1.304247 1.372197 -0.055868 21.00000 0.07562 0.04823 = 0.02545 0.00017 0.02145 -0.00388 PART 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM REM R1 = 0.0581 for 3941 Fo > 4sig(Fo) and 0.1239 for all 7713 data REM 483 parameters refined using 71 restraints END WGHT 0.0557 0.0000 REM Highest difference peak 0.301, deepest hole -0.273, 1-sigma level 0.057 Q1 1 0.5662 -0.0260 0.6609 11.00000 0.05 0.30 Q2 1 0.7164 0.4473 0.7158 11.00000 0.05 0.27 Q3 1 0.3842 -0.2190 0.7190 11.00000 0.05 0.26 Q4 1 0.7163 0.2912 0.5201 11.00000 0.05 0.24 Q5 1 0.5015 0.1255 0.5792 11.00000 0.05 0.24 Q6 1 0.5560 0.1685 0.8094 11.00000 0.05 0.23 Q7 1 0.9752 1.3338 0.1286 11.00000 0.05 0.23 Q8 1 0.5268 0.0397 0.6212 11.00000 0.05 0.23 Q9 1 0.8920 0.6806 0.6030 11.00000 0.05 0.21 Q10 1 0.6765 0.5151 0.6600 11.00000 0.05 0.21 Q11 1 0.5775 0.1579 0.8617 11.00000 0.05 0.21 Q12 1 0.7829 0.4912 0.8397 11.00000 0.05 0.20 Q13 1 0.5473 -0.4790 0.8803 11.00000 0.05 0.20 Q14 1 0.4302 -0.3328 0.8171 11.00000 0.05 0.20 Q15 1 0.8344 0.4213 0.6975 11.00000 0.05 0.20 Q16 1 0.6311 0.4922 0.4427 11.00000 0.05 0.20 Q17 1 0.4003 -0.2621 0.7671 11.00000 0.05 0.20 Q18 1 0.6169 -0.0069 0.9801 11.00000 0.05 0.20 Q19 1 0.5608 0.2333 0.8291 11.00000 0.05 0.19 Q20 1 0.7783 0.5908 0.1802 11.00000 0.05 0.19 ;