# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Gautam Desiraju' _publ_contact_author_address ; School of Chemistry University of Hyderabad PO Central University Hyderabad Hyderabad 500046 INDIA ; _publ_contact_author_email 'GAUTAM DESIRAJU@YAHOO.COM' _publ_section_title ; Synthon evolution and unit cell evolution during crystallisation. A study of symmetry-independent molecules (Z?>1) in crystals of some hydroxy compounds ; loop_ _publ_author_name 'Gautam Desiraju' 'Rahul Banerjee' 'Roland Boese' 'Dinabandhu Das' 'Judith A. K. Howard' 'Raju Mondal' data_ddcc _database_code_depnum_ccdc_archive 'CCDC 283828' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2,3,4,5,6-pentafluorophenol ; _chemical_name_common 2,3,4,5,6-pentafluorophenol _chemical_melting_point 307(9) _chemical_formula_moiety 'C6 H F5 O' _chemical_formula_sum 'C6 H F5 O' _chemical_formula_weight 184.07 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc _symmetry_space_group_name_Hall 'C -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 21.300(4) _cell_length_b 5.7697(12) _cell_length_c 16.796(3) _cell_angle_alpha 90.00 _cell_angle_beta 114.68(3) _cell_angle_gamma 90.00 _cell_volume 1875.5(7) _cell_formula_units_Z 12 _cell_measurement_temperature 292(2) _cell_measurement_reflns_used 989 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 28.28 _exptl_crystal_description cylindrical _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.956 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 0.230 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9342 _exptl_absorpt_correction_T_max 0.9342 _exptl_absorpt_process_details SADABS _exptl_special_details ; The crystal was grown in situ on the diffractometer at 292K and the data were collected in omega scan only in order to maintain the cold gas stream of the LT device parallel to the capillary. This was necessary to avoid warming up and melting above/below the crystal. With numerous arduous attempts it was neither possible to grow better crystals or crystals which had a different orientation. ; _diffrn_ambient_temperature 292(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 'Siemens SMART CCD area detector system' _diffrn_measurement_method ; data collection in omega at 0.3deg scan width one run with 740 frames, phi = 0deg, chi = 0deg ; _diffrn_reflns_number 3432 _diffrn_reflns_av_R_equivalents 0.0169 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 28.28 _reflns_number_total 1966 _reflns_number_gt 1416 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; Bruker AXS SMART Vers. 5.054 1997/98 ; _computing_cell_refinement ; Bruker AXS SMART Vers. 5.054 1997/98 ; _computing_data_reduction ; Bruker AXS SAINT program Vers.6.45A ; _computing_structure_solution ; Bruker AXS SHELXTL Vers. 5.10 DOS/WIN95/NT ; _computing_structure_refinement ; Bruker AXS SHELXTL Vers. 5.10 DOS/WIN95/NT ; _computing_molecular_graphics ; Bruker AXS SHELXTL Vers. 5.10 DOS/WIN95/NT ; _computing_publication_material ; Bruker AXS SHELXTL Vers. 5.10 DOS/WIN95/NT ; _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. ADDSYM suggests C2/c space group. Refinement in this space group requires one and half molecules in the asymmetric unit with the half molecule showing unreasonable disorder, significatly higher R-values and problems to attain a reasonable model. This is why the space group Cc was preferred assuming pseudo symmetry for the cell. The pseudo symmetry caused correlation (up to 0.8 in the matrix) which affected the esds of the atomic positions. Theta full and data parameter ratio is low, because the data were collected with omega scan only.So the number of total refelctions is low. Moreover the the crystal was not growing properly after varius attempts also. ; _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^)+(0.0571P)^2^+1.9555P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.4(16) _refine_ls_number_reflns 1966 _refine_ls_number_parameters 328 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.1212 _refine_ls_wR_factor_gt 0.1040 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.029 _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 F15 F 0.1726(2) 0.9252(11) 0.4583(3) 0.0709(17) Uani 1 1 d . . . F14 F 0.1162(2) 1.3040(11) 0.4990(4) 0.0781(19) Uani 1 1 d . . . F12 F 0.2009(3) 1.0587(12) 0.7912(3) 0.0799(18) Uani 1 1 d . . . F11 F 0.2566(2) 0.6775(11) 0.7518(4) 0.0754(17) Uani 1 1 d . . . C11 C 0.2227(4) 0.8285(17) 0.6893(5) 0.051(2) Uani 1 1 d . . . C14 C 0.1511(4) 1.1452(18) 0.5620(5) 0.056(2) Uani 1 1 d . . . C12 C 0.1944(4) 1.019(2) 0.7084(5) 0.059(3) Uani 1 1 d . . . O11 O 0.2471(3) 0.6034(14) 0.5883(4) 0.0684(19) Uani 1 1 d . . . H11 H 0.2431 0.6075 0.5376 0.103 Uiso 1 1 calc R . . F13 F 0.1291(3) 1.3710(12) 0.6634(4) 0.0866(19) Uani 1 1 d . . . C15 C 0.1804(3) 0.9564(17) 0.5417(4) 0.050(2) Uani 1 1 d . . . C13 C 0.1581(4) 1.1758(18) 0.6447(7) 0.056(2) Uani 1 1 d . . . C16 C 0.2170(3) 0.7877(18) 0.6038(5) 0.049(2) Uani 1 1 d . . . C33 C 1.0422(4) 0.3556(19) 0.2883(5) 0.058(3) Uani 1 1 d . . . C34 C 1.0116(4) 0.166(2) 0.2416(6) 0.060(3) Uani 1 1 d . . . O31 O 0.8345(2) 0.2537(12) 0.2107(4) 0.0567(16) Uani 1 1 d . . . H31 H 0.8217 0.1343 0.1819 0.085 Uiso 1 1 calc R . . F31 F 0.8951(3) 0.6276(11) 0.3030(4) 0.0749(18) Uani 1 1 d . . . C35 C 0.9407(4) 0.1235(17) 0.2153(5) 0.045(2) Uani 1 1 d . . . F35 F 0.9119(3) -0.0698(11) 0.1679(4) 0.0783(18) Uani 1 1 d . . . C36 C 0.9030(3) 0.2816(16) 0.2356(5) 0.043(2) Uani 1 1 d . . . F34 F 1.0480(3) 0.0045(15) 0.2181(4) 0.101(2) Uani 1 1 d . . . F32 F 1.0316(3) 0.6980(14) 0.3557(4) 0.095(2) Uani 1 1 d . . . C32 C 1.0016(4) 0.5151(19) 0.3107(5) 0.051(2) Uani 1 1 d . . . C31 C 0.9339(4) 0.4739(18) 0.2828(5) 0.052(3) Uani 1 1 d . . . F33 F 1.1107(3) 0.3901(17) 0.3102(5) 0.132(3) Uani 1 1 d . . . F24 F 0.4788(3) 0.6262(11) 0.4470(4) 0.0799(18) Uani 1 1 d . . . F23 F 0.5345(2) 0.2382(12) 0.5396(3) 0.0791(18) Uani 1 1 d . . . C23 C 0.4673(3) 0.2846(18) 0.5126(5) 0.051(2) Uani 1 1 d . . . F22 F 0.4526(3) -0.0605(12) 0.5775(4) 0.0863(19) Uani 1 1 d . . . F21 F 0.3179(3) 0.0264(13) 0.5249(4) 0.092(2) Uani 1 1 d . . . F25 F 0.3434(3) 0.7254(12) 0.3942(3) 0.0796(16) Uani 1 1 d . . . C25 C 0.3686(4) 0.523(2) 0.4412(5) 0.056(3) Uani 1 1 d . . . C24 C 0.4389(3) 0.4759(17) 0.4670(5) 0.049(2) Uani 1 1 d . . . O21 O 0.2587(3) 0.4259(17) 0.4357(4) 0.098(3) Uani 1 1 d . . . H21 H 0.2346 0.3349 0.3977 0.147 Uiso 1 1 calc R . . C26 C 0.3270(4) 0.378(2) 0.4582(5) 0.060(3) Uani 1 1 d . . . C21 C 0.3569(5) 0.1772(19) 0.5058(5) 0.058(3) Uani 1 1 d . . . C22 C 0.4249(4) 0.1307(19) 0.5325(5) 0.052(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F15 0.057(2) 0.104(5) 0.044(2) 0.011(3) 0.0145(18) -0.014(3) F14 0.065(3) 0.093(6) 0.067(3) 0.033(3) 0.018(2) 0.003(3) F12 0.080(3) 0.114(6) 0.049(2) -0.012(3) 0.030(2) -0.026(3) F11 0.062(3) 0.094(6) 0.057(3) 0.023(3) 0.011(2) -0.006(3) C11 0.044(3) 0.060(8) 0.042(4) 0.004(4) 0.011(3) -0.017(3) C14 0.040(3) 0.062(8) 0.058(4) 0.020(4) 0.013(3) -0.011(3) C12 0.055(4) 0.077(9) 0.042(4) 0.002(4) 0.018(3) -0.028(4) O11 0.065(3) 0.082(6) 0.055(3) 0.000(3) 0.021(2) -0.005(3) F13 0.094(4) 0.070(6) 0.103(4) -0.006(3) 0.048(3) -0.012(3) C15 0.036(3) 0.067(8) 0.046(4) 0.000(4) 0.016(3) -0.013(3) C13 0.056(4) 0.038(8) 0.073(5) 0.002(4) 0.027(3) -0.010(3) C16 0.040(3) 0.060(8) 0.043(3) 0.001(3) 0.012(3) -0.014(3) C33 0.042(4) 0.075(9) 0.052(4) 0.028(5) 0.016(3) 0.004(4) C34 0.054(4) 0.072(9) 0.062(5) 0.020(5) 0.033(4) 0.022(4) O31 0.042(2) 0.056(5) 0.072(4) -0.005(3) 0.024(2) 0.000(3) F31 0.090(3) 0.055(6) 0.083(4) -0.009(3) 0.040(3) 0.020(3) C35 0.049(3) 0.042(7) 0.042(3) 0.009(4) 0.018(3) 0.009(3) F35 0.098(4) 0.067(5) 0.076(4) -0.013(3) 0.043(3) 0.004(3) C36 0.042(3) 0.040(7) 0.044(4) 0.002(4) 0.015(3) 0.005(3) F34 0.096(4) 0.124(6) 0.104(5) 0.035(4) 0.063(3) 0.063(4) F32 0.119(5) 0.063(5) 0.073(4) -0.002(3) 0.011(3) -0.042(4) C32 0.057(4) 0.047(8) 0.043(4) 0.000(4) 0.015(3) -0.014(4) C31 0.067(5) 0.039(9) 0.044(4) 0.001(4) 0.019(3) 0.007(4) F33 0.058(3) 0.212(9) 0.110(5) 0.052(5) 0.017(3) -0.022(4) F24 0.078(3) 0.086(5) 0.088(4) 0.016(3) 0.047(3) -0.016(3) F23 0.050(3) 0.111(6) 0.075(4) 0.004(3) 0.025(2) 0.013(3) C23 0.049(4) 0.062(8) 0.047(4) -0.004(4) 0.026(3) 0.000(4) F22 0.133(5) 0.053(6) 0.078(4) 0.002(3) 0.048(4) 0.001(4) F21 0.103(4) 0.098(5) 0.106(4) -0.022(4) 0.072(4) -0.054(4) F25 0.081(3) 0.088(5) 0.063(3) 0.013(3) 0.023(2) 0.020(3) C25 0.061(4) 0.058(9) 0.041(4) -0.006(4) 0.013(3) 0.004(4) C24 0.043(3) 0.058(8) 0.051(4) -0.007(4) 0.026(3) -0.010(4) O21 0.050(3) 0.178(8) 0.069(4) -0.046(4) 0.029(3) -0.032(4) C26 0.044(3) 0.089(10) 0.048(4) -0.023(5) 0.020(3) -0.009(4) C21 0.069(5) 0.061(9) 0.054(4) -0.024(5) 0.036(4) -0.036(5) C22 0.085(5) 0.036(8) 0.047(4) 0.003(4) 0.038(4) -0.002(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 F15 C15 1.352(8) . ? F14 C14 1.363(10) . ? F12 C12 1.358(8) . ? F11 C11 1.324(10) . ? C11 C12 1.355(14) . ? C11 C16 1.409(10) . ? C14 C13 1.345(12) . ? C14 C15 1.368(13) . ? C12 C13 1.367(14) . ? O11 C16 1.322(11) . ? O11 H11 0.8200 . ? F13 C13 1.382(12) . ? C15 C16 1.402(12) . ? C33 C34 1.345(13) . ? C33 F33 1.361(9) . ? C33 C32 1.419(13) . ? C34 F34 1.371(11) . ? C34 C35 1.406(11) . ? O31 C36 1.349(8) . ? O31 H31 0.8200 . ? F31 C31 1.347(10) . ? C35 C36 1.350(12) . ? C35 F35 1.358(11) . ? C36 C31 1.363(12) . ? F32 C32 1.300(11) . ? C32 C31 1.338(10) . ? F24 C24 1.352(9) . ? F23 C23 1.337(8) . ? C23 C24 1.335(12) . ? C23 C22 1.403(12) . ? F22 C22 1.328(11) . ? F21 C21 1.331(10) . ? F25 C25 1.386(12) . ? C25 C26 1.332(13) . ? C25 C24 1.400(10) . ? O21 C26 1.370(10) . ? O21 H21 0.8200 . ? C26 C21 1.402(14) . ? C21 C22 1.351(13) . ? 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 F11 C11 C12 119.7(7) . . ? F11 C11 C16 119.0(9) . . ? C12 C11 C16 121.3(8) . . ? C13 C14 F14 120.2(10) . . ? C13 C14 C15 119.8(8) . . ? F14 C14 C15 120.0(8) . . ? C11 C12 F12 120.9(8) . . ? C11 C12 C13 120.9(8) . . ? F12 C12 C13 118.2(10) . . ? C16 O11 H11 109.5 . . ? F15 C15 C14 119.5(8) . . ? F15 C15 C16 118.0(8) . . ? C14 C15 C16 122.5(7) . . ? C14 C13 C12 120.2(9) . . ? C14 C13 F13 118.3(10) . . ? C12 C13 F13 121.5(9) . . ? O11 C16 C15 125.2(7) . . ? O11 C16 C11 119.6(8) . . ? C15 C16 C11 115.2(8) . . ? C34 C33 F33 118.7(9) . . ? C34 C33 C32 118.7(7) . . ? F33 C33 C32 122.5(10) . . ? C33 C34 F34 121.7(8) . . ? C33 C34 C35 121.4(8) . . ? F34 C34 C35 116.9(10) . . ? C36 O31 H31 109.5 . . ? C36 C35 F35 122.1(6) . . ? C36 C35 C34 118.4(9) . . ? F35 C35 C34 119.4(8) . . ? O31 C36 C35 121.4(8) . . ? O31 C36 C31 118.3(6) . . ? C35 C36 C31 120.3(6) . . ? F32 C32 C31 123.0(9) . . ? F32 C32 C33 118.3(7) . . ? C31 C32 C33 118.7(9) . . ? C32 C31 F31 118.6(9) . . ? C32 C31 C36 122.4(8) . . ? F31 C31 C36 119.0(7) . . ? C24 C23 F23 121.7(6) . . ? C24 C23 C22 118.5(7) . . ? F23 C23 C22 119.8(8) . . ? C26 C25 F25 121.1(8) . . ? C26 C25 C24 122.2(10) . . ? F25 C25 C24 116.7(8) . . ? C23 C24 F24 119.4(6) . . ? C23 C24 C25 120.5(7) . . ? F24 C24 C25 120.0(8) . . ? C26 O21 H21 109.5 . . ? C25 C26 O21 122.6(11) . . ? C25 C26 C21 117.1(8) . . ? O21 C26 C21 120.1(9) . . ? F21 C21 C22 118.7(10) . . ? F21 C21 C26 119.8(8) . . ? C22 C21 C26 121.5(8) . . ? F22 C22 C21 120.9(8) . . ? F22 C22 C23 118.9(8) . . ? C21 C22 C23 120.1(10) . . ? _diffrn_measured_fraction_theta_max 0.691 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.691 _refine_diff_density_max 0.179 _refine_diff_density_min -0.195 _refine_diff_density_rms 0.038 data_ddpfp _database_code_depnum_ccdc_archive 'CCDC 283829' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2,3,4,5,6-pentafluorophenol ; _chemical_name_common pentafluorophenol _chemical_melting_point 307(2) _chemical_formula_moiety 'C6 H F5 O' _chemical_formula_sum 'C6 H F5 O' _chemical_formula_weight 184.07 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 13.073(3) _cell_length_b 4.9295(10) _cell_length_c 10.163(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.31(3) _cell_angle_gamma 90.00 _cell_volume 625.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 269(2) _cell_measurement_reflns_used 842 _cell_measurement_theta_min 3.25 _cell_measurement_theta_max 27.25 _exptl_crystal_description cylindrical _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.955 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 0.230 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9342 _exptl_absorpt_correction_T_max 0.9342 _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; the crystallization was performed on the diffractometer by slow cooling ; _diffrn_ambient_temperature 269(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 'Siemens SMART CCD area detector system' _diffrn_measurement_method ; data collection in omega at 0.3deg scan width one run with 740 frames, phi = 0deg, chi = 0deg ; _diffrn_reflns_number 2012 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 26.37 _reflns_number_total 1199 _reflns_number_gt 777 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; Bruker AXS SMART Vers. 5.054 1997/98 ; _computing_cell_refinement ; Bruker AXS SMART Vers. 5.054 1997/98 ; _computing_data_reduction ; Bruker AXS SAINT program Vers.6.45A ; _computing_structure_solution ; Bruker AXS SHELXTL Vers. 5.10 DOS/WIN95/NT ; _computing_structure_refinement ; Bruker AXS SHELXTL Vers. 5.10 DOS/WIN95/NT ; _computing_molecular_graphics ; Bruker AXS SHELXTL Vers. 5.10 DOS/WIN95/NT ; _computing_publication_material ; Bruker AXS SHELXTL Vers. 5.10 DOS/WIN95/NT ; _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. hydroxy hydrogen atom position taken from a Fourier-map and also refined as riding group with the 1.5 fold isotropic displacement parameters of the equivalent Uij of the corresponding oxygen atom. ; _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^)+(0.0699P)^2^+0.0641P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1199 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.1276 _refine_ls_wR_factor_gt 0.1096 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 C1 C 0.14718(15) 0.4961(4) 0.3912(2) 0.0428(5) Uani 1 1 d . . . C2 C 0.21915(16) 0.3090(4) 0.3701(2) 0.0455(5) Uani 1 1 d . . . C3 C 0.32350(16) 0.3021(4) 0.4512(2) 0.0523(6) Uani 1 1 d . . . C4 C 0.35937(16) 0.4860(5) 0.5566(2) 0.0559(6) Uani 1 1 d . . . C5 C 0.28886(18) 0.6742(4) 0.5796(2) 0.0531(6) Uani 1 1 d . . . C6 C 0.18462(17) 0.6786(4) 0.4974(2) 0.0492(5) Uani 1 1 d . . . O1 O 0.04343(11) 0.5109(3) 0.31175(18) 0.0587(5) Uani 1 1 d . . . H1 H 0.0186 0.3371 0.2700 0.088 Uiso 1 1 d R . . F1 F 0.18497(11) 0.1287(3) 0.26717(15) 0.0665(5) Uani 1 1 d . . . F2 F 0.39042(11) 0.1156(3) 0.42774(19) 0.0794(5) Uani 1 1 d . . . F3 F 0.46067(10) 0.4782(4) 0.63678(17) 0.0871(6) Uani 1 1 d . . . F4 F 0.32239(12) 0.8551(3) 0.68205(15) 0.0820(5) Uani 1 1 d . . . F5 F 0.11655(11) 0.8645(3) 0.52145(17) 0.0718(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0401(11) 0.0396(10) 0.0468(12) 0.0047(8) 0.0101(9) -0.0008(8) C2 0.0455(11) 0.0427(11) 0.0498(12) -0.0006(9) 0.0166(9) -0.0025(8) C3 0.0416(11) 0.0512(12) 0.0669(14) 0.0112(11) 0.0207(10) 0.0054(9) C4 0.0407(12) 0.0640(14) 0.0570(15) 0.0146(11) 0.0052(10) -0.0059(10) C5 0.0589(14) 0.0555(13) 0.0413(12) -0.0005(9) 0.0093(10) -0.0117(10) C6 0.0516(13) 0.0451(11) 0.0536(12) 0.0027(9) 0.0196(10) 0.0019(9) O1 0.0434(9) 0.0502(8) 0.0721(11) -0.0019(7) 0.0014(7) 0.0039(6) F1 0.0622(9) 0.0616(8) 0.0754(10) -0.0220(7) 0.0200(7) -0.0024(6) F2 0.0503(8) 0.0727(9) 0.1194(13) 0.0021(9) 0.0320(8) 0.0149(6) F3 0.0468(9) 0.1117(12) 0.0847(13) 0.0151(9) -0.0082(8) -0.0069(7) F4 0.0908(12) 0.0879(11) 0.0577(10) -0.0214(8) 0.0073(8) -0.0191(8) F5 0.0721(9) 0.0579(8) 0.0893(11) -0.0151(7) 0.0303(8) 0.0085(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.358(2) . ? C1 C6 1.378(3) . ? C1 C2 1.379(3) . ? C2 F1 1.343(2) . ? C2 C3 1.369(3) . ? C3 F2 1.339(2) . ? C3 C4 1.375(3) . ? C4 F3 1.333(2) . ? C4 C5 1.376(3) . ? C5 F4 1.342(2) . ? C5 C6 1.370(3) . ? C6 F5 1.350(2) . ? O1 H1 0.9686 . ? 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 C6 119.31(18) . . ? O1 C1 C2 123.37(18) . . ? C6 C1 C2 117.31(18) . . ? F1 C2 C3 119.58(18) . . ? F1 C2 C1 118.64(18) . . ? C3 C2 C1 121.77(19) . . ? F2 C3 C2 119.8(2) . . ? F2 C3 C4 120.16(19) . . ? C2 C3 C4 120.06(19) . . ? F3 C4 C3 120.2(2) . . ? F3 C4 C5 120.6(2) . . ? C3 C4 C5 119.12(19) . . ? F4 C5 C6 119.9(2) . . ? F4 C5 C4 120.0(2) . . ? C6 C5 C4 120.1(2) . . ? F5 C6 C5 119.34(19) . . ? F5 C6 C1 119.05(19) . . ? C5 C6 C1 121.62(19) . . ? C1 O1 H1 111.0 . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 0.206 _refine_diff_density_min -0.207 _refine_diff_density_rms 0.045 data_poly1 _database_code_depnum_ccdc_archive 'CCDC 283830' _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans -1,4-bis(phenylethynyl) cyclohexane -1,4-diol ; _chemical_name_common 'trans -1,4-bis(phenylethynyl) cyclohexane -1,4-diol' _chemical_melting_point 182 _chemical_formula_moiety 'C22 H20 O2' _chemical_formula_sum 'C22 H20 O2' _chemical_formula_weight 316.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.6377(8) _cell_length_b 18.8315(9) _cell_length_c 23.3591(11) _cell_angle_alpha 78.402(2) _cell_angle_beta 88.367(2) _cell_angle_gamma 67.611(2) _cell_volume 7017.4(6) _cell_formula_units_Z 16 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7769 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 25.83 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.198 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2688 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 95843 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0616 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 27.49 _reflns_number_total 32149 _reflns_number_gt 16870 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Disorder. Molecule A has both Ph ring disordered, one of them between 2 orientations: atoms C(11A) to C(16A) [and attached hydrogens] with the occupancy 0.9, C(31A) to C(36) with occupancy 0.1, the second Ph ring between 3 orientations, C(17A) to C(22A) with occupancy 0.8, C(37A) to C(42A) and C(47A) to C(52A) with occupancies 0.1. Molecule B has one Ph ring disordered between 2 orientations: atoms C(17B) to C(22B) with occupancy 0.9, C(27B) to C(32B) with occupancy 0.1. Molecule D has both Ph ring disordered between 2 orientations: atoms C(11D) to C(22D) with occupancy 0.9, C(31D) to C(42D) with occupancy 0.1. Molecule E has one Ph ring disordered between 2 orientations: atoms C(17E) to C(22E) with occupancy 0.9, C(27E) to C(32E) with occupancy 0.1. Molecule F has one Ph ring disordered between 2 orientations: atoms C(17F) to C(22F) with occupancy 0.9, C(27F) to C(32F) with occupancy 0.1. Molecule H has its only independent Ph ring disordered between 2 orientations: atoms C(11H) to C(16H) with occupancy 0.9, C(31H) to C(36H) with occupancy 0.1. In each case, non-hydrogen atoms of the major orientation were refined in anisotropic approximation with the hydrogen atoms riding on them. The minor orientations were refined as rigid bodies (ideal hexagon rings) and finally were treated as riding on the terminal acetylenic atoms C(8) and/or C(10). Whereas all major phenyl ring orientations are compatible with each other, and all minor orientations with each other, major orientations are not compatible with minor orientations of other molecules. Hence the disorder in all molecules must be concerted. ; _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^)+(0.0758P)^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 32149 _refine_ls_number_parameters 1784 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1046 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1565 _refine_ls_wR_factor_gt 0.1360 _refine_ls_goodness_of_fit_ref 0.896 _refine_ls_restrained_S_all 0.896 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1A O 0.77614(7) 0.24962(8) 0.40888(5) 0.0332(3) Uani 1 1 d . . . H01A H 0.7791 0.2785 0.3771 0.050 Uiso 1 1 d R . . O2A O 0.47690(7) 0.23965(6) 0.34332(5) 0.0214(3) Uani 1 1 d . . . H02A H 0.4347 0.2813 0.3363 0.032 Uiso 1 1 d R . . C1A C 0.70160(10) 0.23566(10) 0.40768(7) 0.0234(4) Uani 1 1 d . . . C2A C 0.62746(10) 0.31406(10) 0.39678(7) 0.0225(4) Uani 1 1 d . . . H2A1 H 0.6251 0.3408 0.4296 0.029 Uiso 1 1 d R . . H2A2 H 0.6341 0.3482 0.3604 0.029 Uiso 1 1 d R . . C3A C 0.54715(9) 0.30230(10) 0.39125(7) 0.0193(4) Uani 1 1 d . . . H3A1 H 0.5380 0.2722 0.4289 0.025 Uiso 1 1 d R . . H3A2 H 0.5009 0.3541 0.3829 0.025 Uiso 1 1 d R . . C4A C 0.54825(9) 0.25850(9) 0.34262(7) 0.0173(3) Uani 1 1 d . . . C5A C 0.62230(10) 0.18012(9) 0.35322(7) 0.0213(4) Uani 1 1 d . . . H5A1 H 0.6151 0.1456 0.3892 0.028 Uiso 1 1 d R . . H5A2 H 0.6246 0.1540 0.3201 0.028 Uiso 1 1 d R . . C6A C 0.70263(10) 0.19066(10) 0.35966(7) 0.0251(4) Uani 1 1 d . . . H6A1 H 0.7133 0.2194 0.3219 0.033 Uiso 1 1 d R . . H6A2 H 0.7480 0.1384 0.3690 0.033 Uiso 1 1 d R . . C7A C 0.69779(10) 0.19051(10) 0.46668(8) 0.0243(4) Uani 1 1 d . A . C8A C 0.69003(10) 0.15930(10) 0.51504(7) 0.0246(4) Uani 1 1 d . . . C31A C 0.68159(10) 0.11504(10) 0.56932(7) 0.0212(4) Uani 0.10 1 d PR A 2 C32A C 0.73830(10) 0.04205(10) 0.59657(7) 0.045(11) Uiso 0.10 1 d PR A 2 H32A H 0.7844 0.0150 0.5764 0.054 Uiso 0.10 1 d PR A 2 C33A C 0.72755(10) 0.00867(10) 0.65336(7) 0.038(10) Uiso 0.10 1 d PR A 2 H33A H 0.7663 -0.0412 0.6720 0.045 Uiso 0.10 1 d PR A 2 C34A C 0.66008(10) 0.04827(10) 0.68289(7) 0.050(12) Uiso 0.10 1 d PR A 2 H34A H 0.6527 0.0255 0.7217 0.060 Uiso 0.10 1 d PR A 2 C35A C 0.60337(10) 0.12126(10) 0.65564(7) 0.058(7) Uiso 0.10 1 d PR A 2 H35A H 0.5573 0.1483 0.6758 0.069 Uiso 0.10 1 d PR A 2 C36A C 0.61413(10) 0.15464(10) 0.59885(7) 0.043(6) Uiso 0.10 1 d PR A 2 H36A H 0.5754 0.2045 0.5802 0.052 Uiso 0.10 1 d PR A 2 C9A C 0.55106(10) 0.30625(9) 0.28454(7) 0.0194(4) Uani 1 1 d . B . C10A C 0.55363(10) 0.34288(10) 0.23702(7) 0.0211(4) Uani 1 1 d . . . C37A C 0.56720(10) 0.35564(10) 0.17323(7) 0.037(7) Uiso 0.10 1 d PR B 2 C38A C 0.59485(10) 0.30359(10) 0.13553(7) 0.055(6) Uiso 0.10 1 d PR B 2 H38A H 0.6092 0.2490 0.1501 0.066 Uiso 0.10 1 d PR B 2 C39A C 0.60149(10) 0.33142(10) 0.07658(7) 0.046(6) Uiso 0.10 1 d PR B 2 H39A H 0.6204 0.2958 0.0508 0.056 Uiso 0.10 1 d PR B 2 C40A C 0.58049(10) 0.41129(10) 0.05532(7) 0.042(6) Uiso 0.10 1 d PR B 2 H40A H 0.5850 0.4303 0.0150 0.050 Uiso 0.10 1 d PR B 2 C41A C 0.55284(10) 0.46334(10) 0.09301(7) 0.045(7) Uiso 0.10 1 d PR B 2 H41A H 0.5385 0.5179 0.0785 0.055 Uiso 0.10 1 d PR B 2 C42A C 0.54620(10) 0.43552(10) 0.15197(7) 0.051(6) Uiso 0.10 1 d PR B 2 H42A H 0.5273 0.4711 0.1777 0.061 Uiso 0.10 1 d PR B 2 C47A C 0.55119(10) 0.37916(10) 0.16988(7) 0.0169(4) Uani 0.10 1 d PR B 3 C48A C 0.62107(10) 0.39120(10) 0.14954(7) 0.0213(4) Uani 0.10 1 d PR B 3 H48A H 0.6660 0.3798 0.1761 0.026 Uiso 0.10 1 d PR B 3 C49A C 0.62522(10) 0.41997(10) 0.09038(7) 0.0278(5) Uani 0.10 1 d PR B 3 H49A H 0.6730 0.4282 0.0765 0.033 Uiso 0.10 1 d PR B 3 C50A C 0.55950(10) 0.43671(10) 0.05156(7) 0.089(12) Uiso 0.10 1 d PR B 3 H50A H 0.5623 0.4564 0.0111 0.106 Uiso 0.10 1 d PR B 3 C51A C 0.48962(10) 0.42467(10) 0.07189(7) 0.055(6) Uiso 0.10 1 d PR B 3 H51A H 0.4447 0.4361 0.0454 0.066 Uiso 0.10 1 d PR B 3 C52A C 0.48547(10) 0.39590(10) 0.13106(7) 0.052(6) Uiso 0.10 1 d PR B 3 H52A H 0.4377 0.3877 0.1450 0.063 Uiso 0.10 1 d PR B 3 C11A C 0.67831(11) 0.12892(11) 0.57494(8) 0.0212(4) Uani 0.90 1 d P A 1 C12A C 0.71091(19) 0.04805(12) 0.59849(8) 0.0231(5) Uani 0.90 1 d P A 1 H12A H 0.7422 0.0123 0.5752 0.028 Uiso 0.90 1 d PR A 1 C13A C 0.69842(19) 0.02074(13) 0.65631(8) 0.0268(5) Uani 0.90 1 d P A 1 H13A H 0.7207 -0.0341 0.6721 0.032 Uiso 0.90 1 d PR A 1 C14A C 0.65514(12) 0.07204(17) 0.69127(9) 0.0260(5) Uani 0.90 1 d P A 1 H14A H 0.6467 0.0526 0.7307 0.031 Uiso 0.90 1 d PR A 1 C15A C 0.62299(12) 0.15210(12) 0.66784(9) 0.0294(5) Uani 0.90 1 d P A 1 H15A H 0.5931 0.1876 0.6917 0.035 Uiso 0.90 1 d PR A 1 C16A C 0.63447(11) 0.18033(12) 0.61030(8) 0.0267(5) Uani 0.90 1 d P A 1 H16A H 0.6121 0.2352 0.5948 0.032 Uiso 0.90 1 d PR A 1 C17A C 0.55765(13) 0.38664(13) 0.18007(8) 0.0169(4) Uani 0.80 1 d P B 1 C18A C 0.63368(13) 0.37336(12) 0.15551(9) 0.0213(4) Uani 0.80 1 d P B 1 H18A H 0.6827 0.3382 0.1775 0.026 Uiso 0.80 1 d PR B 1 C19A C 0.63823(14) 0.41497(14) 0.10045(9) 0.0278(5) Uani 0.80 1 d P B 1 H19A H 0.6900 0.4066 0.0840 0.033 Uiso 0.80 1 d PR B 1 C20A C 0.56733(15) 0.46814(13) 0.06857(10) 0.0284(5) Uani 0.80 1 d P B 1 H20A H 0.5703 0.4963 0.0305 0.034 Uiso 0.80 1 d PR B 1 C21A C 0.49153(14) 0.47954(13) 0.09210(9) 0.0299(5) Uani 0.80 1 d P B 1 H21A H 0.4427 0.5152 0.0701 0.036 Uiso 0.80 1 d PR B 1 C22A C 0.48679(13) 0.43951(12) 0.14783(9) 0.0246(5) Uani 0.80 1 d P B 1 H22A H 0.4350 0.4491 0.1645 0.029 Uiso 0.80 1 d PR B 1 O1B O 0.16961(7) 0.64753(6) 0.18056(5) 0.0219(3) Uani 1 1 d . . . H01B H 0.1950 0.6656 0.1544 0.033 Uiso 1 1 d R . . O2B O 0.32075(7) 0.35186(6) 0.32746(5) 0.0206(3) Uani 1 1 d . . . H02B H 0.2971 0.3332 0.3546 0.031 Uiso 1 1 d R . . C1B C 0.21619(9) 0.56517(9) 0.20179(7) 0.0167(3) Uani 1 1 d . . . C2B C 0.15733(9) 0.53176(9) 0.23560(7) 0.0200(4) Uani 1 1 d . . . H2B1 H 0.1317 0.5629 0.2655 0.026 Uiso 1 1 d R . . H2B2 H 0.1130 0.5363 0.2083 0.026 Uiso 1 1 d R . . C3B C 0.20191(10) 0.44575(9) 0.26544(7) 0.0195(4) Uani 1 1 d . . . H3B1 H 0.2236 0.4140 0.2352 0.025 Uiso 1 1 d R . . H3B2 H 0.1623 0.4266 0.2876 0.025 Uiso 1 1 d R . . C4B C 0.27303(9) 0.43424(9) 0.30742(7) 0.0170(3) Uani 1 1 d . . . C5B C 0.33154(10) 0.46852(9) 0.27422(7) 0.0197(4) Uani 1 1 d . . . H5B1 H 0.3749 0.4647 0.3020 0.026 Uiso 1 1 d R . . H5B2 H 0.3584 0.4372 0.2447 0.026 Uiso 1 1 d R . . C6B C 0.28703(10) 0.55422(9) 0.24380(7) 0.0190(4) Uani 1 1 d . . . H6B1 H 0.3266 0.5732 0.2216 0.025 Uiso 1 1 d R . . H6B2 H 0.2650 0.5864 0.2737 0.025 Uiso 1 1 d R . . C7B C 0.24622(10) 0.52723(10) 0.15153(7) 0.0209(4) Uani 1 1 d . . . C8B C 0.26720(11) 0.49662(10) 0.11052(7) 0.0247(4) Uani 1 1 d . . . C9B C 0.24235(10) 0.47080(9) 0.35830(7) 0.0208(4) Uani 1 1 d . C . C10B C 0.21947(10) 0.50071(10) 0.39933(7) 0.0250(4) Uani 1 1 d . . . C27B C 0.21892(10) 0.54492(10) 0.44354(7) 0.023(7) Uiso 0.10 1 d PR C 2 C28B C 0.23732(10) 0.50000(10) 0.50010(7) 0.0267(4) Uani 0.10 1 d PR C 2 H28B H 0.2612 0.4444 0.5062 0.032 Uiso 0.10 1 d PR C 2 C29B C 0.22085(10) 0.53647(10) 0.54775(7) 0.0318(5) Uani 0.10 1 d PR C 2 H29B H 0.2334 0.5058 0.5864 0.038 Uiso 0.10 1 d PR C 2 C30B C 0.18597(10) 0.61787(10) 0.53884(7) 0.023(6) Uiso 0.10 1 d PR C 2 H30B H 0.1747 0.6428 0.5714 0.028 Uiso 0.10 1 d PR C 2 C31B C 0.16756(10) 0.66279(10) 0.48229(7) 0.075(8) Uiso 0.10 1 d PR C 2 H31B H 0.1437 0.7184 0.4762 0.089 Uiso 0.10 1 d PR C 2 C32B C 0.18404(10) 0.62632(10) 0.43464(7) 0.080(9) Uiso 0.10 1 d PR C 2 H32B H 0.1715 0.6570 0.3960 0.096 Uiso 0.10 1 d PR C 2 C11B C 0.28931(12) 0.45956(10) 0.06078(7) 0.0275(4) Uani 1 1 d . . . C12B C 0.34785(18) 0.38423(12) 0.06703(9) 0.0722(9) Uani 1 1 d . . . H12B H 0.3760 0.3575 0.1039 0.087 Uiso 1 1 d R . . C13B C 0.3657(2) 0.34718(13) 0.01979(10) 0.0833(11) Uani 1 1 d . . . H13B H 0.4056 0.2951 0.0247 0.100 Uiso 1 1 d R . . C14B C 0.32555(16) 0.38506(13) -0.03400(9) 0.0488(6) Uani 1 1 d . . . H14B H 0.3379 0.3598 -0.0664 0.059 Uiso 1 1 d R . . C15B C 0.26847(13) 0.45931(13) -0.04018(8) 0.0395(5) Uani 1 1 d . . . H15B H 0.2404 0.4857 -0.0772 0.047 Uiso 1 1 d R . . C16B C 0.25029(11) 0.49720(12) 0.00658(8) 0.0311(4) Uani 1 1 d . . . H16B H 0.2109 0.5495 0.0012 0.037 Uiso 1 1 d R . . C17B C 0.19437(15) 0.53891(11) 0.44845(8) 0.0212(4) Uani 0.90 1 d P C 1 C18B C 0.24369(12) 0.51092(12) 0.50009(8) 0.0267(4) Uani 0.90 1 d P C 1 H18B H 0.2901 0.4629 0.5048 0.032 Uiso 0.90 1 d PR C 1 C19B C 0.22304(13) 0.55192(13) 0.54504(9) 0.0318(5) Uani 0.90 1 d P C 1 H19B H 0.2558 0.5314 0.5806 0.038 Uiso 0.90 1 d PR C 1 C20B C 0.15422(16) 0.62045(13) 0.53895(9) 0.0335(5) Uani 0.90 1 d P C 1 H20B H 0.1425 0.6495 0.5692 0.040 Uiso 0.90 1 d PR C 1 C21B C 0.10532(14) 0.64789(13) 0.48830(10) 0.0429(6) Uani 0.90 1 d P C 1 H21B H 0.0576 0.6948 0.4845 0.051 Uiso 0.90 1 d PR C 1 C22B C 0.12448(13) 0.60726(12) 0.44328(9) 0.0359(5) Uani 0.90 1 d P C 1 H22B H 0.0894 0.6259 0.4089 0.043 Uiso 0.90 1 d PR C 1 O1C O 0.69023(7) 0.64276(7) 0.18183(5) 0.0231(3) Uani 1 1 d . . . H01C H 0.6394 0.6688 0.1811 0.035 Uiso 1 1 d R . . O2C O 0.82265(7) 0.33701(7) 0.31645(5) 0.0227(3) Uani 1 1 d . . . H02C H 0.8731 0.3101 0.3164 0.034 Uiso 1 1 d R . . C1C C 0.71313(9) 0.57700(9) 0.23035(7) 0.0170(3) Uani 1 1 d . . . C2C C 0.80696(9) 0.53662(9) 0.23167(7) 0.0185(4) Uani 1 1 d . . . H2C1 H 0.8237 0.5254 0.1926 0.024 Uiso 1 1 d R . . H2C2 H 0.8319 0.5726 0.2404 0.024 Uiso 1 1 d R . . C3C C 0.83959(9) 0.46009(9) 0.27736(7) 0.0178(3) Uani 1 1 d . . . H3C1 H 0.8283 0.4720 0.3169 0.023 Uiso 1 1 d R . . H3C2 H 0.8998 0.4348 0.2752 0.023 Uiso 1 1 d R . . C4C C 0.79987(9) 0.40285(9) 0.26825(7) 0.0173(3) Uani 1 1 d . . . C5C C 0.70619(9) 0.44377(9) 0.26744(7) 0.0181(3) Uani 1 1 d . . . H5C1 H 0.6808 0.4078 0.2595 0.023 Uiso 1 1 d R . . H5C2 H 0.6900 0.4557 0.3064 0.023 Uiso 1 1 d R . . C6C C 0.67391(9) 0.51965(9) 0.22127(7) 0.0180(3) Uani 1 1 d . . . H6C1 H 0.6136 0.5449 0.2231 0.023 Uiso 1 1 d R . . H6C2 H 0.6858 0.5073 0.1819 0.023 Uiso 1 1 d R . . C7C C 0.68740(10) 0.60443(9) 0.28522(7) 0.0188(4) Uani 1 1 d . . . C8C C 0.66659(10) 0.62718(9) 0.32968(7) 0.0206(4) Uani 1 1 d . . . C9C C 0.82620(10) 0.37556(9) 0.21294(7) 0.0198(4) Uani 1 1 d . . . C10C C 0.84892(10) 0.35326(10) 0.16853(7) 0.0216(4) Uani 1 1 d . . . C11C C 0.64521(10) 0.65593(9) 0.38307(7) 0.0208(4) Uani 1 1 d . . . C12C C 0.57644(11) 0.65370(11) 0.41201(8) 0.0315(5) Uani 1 1 d . . . H12C H 0.5409 0.6346 0.3960 0.038 Uiso 1 1 d R . . C13C C 0.55866(11) 0.67961(13) 0.46407(9) 0.0410(5) Uani 1 1 d . . . H13C H 0.5117 0.6771 0.4840 0.049 Uiso 1 1 d R . . C14C C 0.60850(12) 0.70938(12) 0.48705(8) 0.0357(5) Uani 1 1 d . . . H14C H 0.5956 0.7281 0.5224 0.043 Uiso 1 1 d R . . C15C C 0.67714(13) 0.71203(12) 0.45840(8) 0.0398(5) Uani 1 1 d . . . H15C H 0.7120 0.7319 0.4744 0.048 Uiso 1 1 d R . . C16C C 0.69563(12) 0.68548(12) 0.40666(8) 0.0330(5) Uani 1 1 d . . . H16C H 0.7432 0.6871 0.3873 0.040 Uiso 1 1 d R . . C17C C 0.87248(10) 0.32806(10) 0.11415(7) 0.0225(4) Uani 1 1 d . . . C18C C 0.83956(13) 0.27959(13) 0.09520(9) 0.0427(6) Uani 1 1 d . . . H18C H 0.8042 0.2607 0.1194 0.051 Uiso 1 1 d R . . C19C C 0.85864(14) 0.25830(14) 0.04148(9) 0.0487(6) Uani 1 1 d . . . H19C H 0.8355 0.2257 0.0288 0.058 Uiso 1 1 d R . . C20C C 0.91097(12) 0.28412(12) 0.00660(8) 0.0341(5) Uani 1 1 d . . . H20C H 0.9239 0.2695 -0.0302 0.041 Uiso 1 1 d R . . C21C C 0.94477(10) 0.33114(10) 0.02549(7) 0.0259(4) Uani 1 1 d . . . H21C H 0.9811 0.3488 0.0015 0.031 Uiso 1 1 d R . . C22C C 0.92598(10) 0.35312(10) 0.07877(7) 0.0214(4) Uani 1 1 d . . . H22C H 0.9495 0.3856 0.0912 0.026 Uiso 1 1 d R . . O1D O 0.77512(7) 0.26218(6) 0.90430(5) 0.0238(3) Uani 1 1 d . . . H01D H 0.8166 0.2201 0.9131 0.036 Uiso 1 1 d R . . O2D O 0.46945(7) 0.25998(7) 0.84625(5) 0.0280(3) Uani 1 1 d . . . H02D H 0.4705 0.2242 0.8747 0.042 Uiso 1 1 d R . . C1D C 0.70251(9) 0.24497(9) 0.90796(7) 0.0185(4) Uani 1 1 d . . . C2D C 0.69959(9) 0.20043(9) 0.86094(7) 0.0198(4) Uani 1 1 d . . . H2D1 H 0.7088 0.2287 0.8225 0.026 Uiso 1 1 d R . . H2D2 H 0.7444 0.1478 0.8696 0.026 Uiso 1 1 d R . . C3D C 0.61769(9) 0.19107(9) 0.85737(7) 0.0208(4) Uani 1 1 d . . . H3D1 H 0.6109 0.1584 0.8945 0.027 Uiso 1 1 d R . . H3D2 H 0.6175 0.1638 0.8253 0.027 Uiso 1 1 d R . . C4D C 0.54557(9) 0.27109(9) 0.84637(7) 0.0200(4) Uani 1 1 d . . . C5D C 0.54784(10) 0.31581(10) 0.89380(7) 0.0217(4) Uani 1 1 d . . . H5D1 H 0.5032 0.3685 0.8850 0.028 Uiso 1 1 d R . . H5D2 H 0.5382 0.2875 0.9320 0.028 Uiso 1 1 d R . . C6D C 0.63001(10) 0.32457(9) 0.89795(7) 0.0215(4) Uani 1 1 d . . . H6D1 H 0.6302 0.3509 0.9306 0.028 Uiso 1 1 d R . . H6D2 H 0.6367 0.3581 0.8613 0.028 Uiso 1 1 d R . . C7D C 0.69986(10) 0.20024(10) 0.96740(7) 0.0206(4) Uani 1 1 d . D . C8D C 0.69419(10) 0.16917(10) 1.01638(7) 0.0212(4) Uani 1 1 d . . . C31D C 0.69407(10) 0.12228(10) 1.06711(7) 0.065(15) Uiso 0.10 1 d PR D 2 C32D C 0.76495(10) 0.07072(10) 1.10022(7) 0.115(13) Uiso 0.10 1 d PR D 2 H32D H 0.8172 0.0628 1.0847 0.138 Uiso 0.10 1 d PR D 2 C33D C 0.75931(10) 0.03072(10) 1.15604(7) 0.144(16) Uiso 0.10 1 d PR D 2 H33D H 0.8078 -0.0045 1.1787 0.173 Uiso 0.10 1 d PR D 2 C34D C 0.68280(10) 0.04226(10) 1.17875(7) 0.076(15) Uiso 0.10 1 d PR D 2 H34D H 0.6789 0.0149 1.2169 0.091 Uiso 0.10 1 d PR D 2 C35D C 0.61192(10) 0.09381(10) 1.14564(7) 0.097(10) Uiso 0.10 1 d PR D 2 H35D H 0.5596 0.1017 1.1612 0.116 Uiso 0.10 1 d PR D 2 C36D C 0.61755(10) 0.13382(10) 1.08982(7) 0.076(8) Uiso 0.10 1 d PR D 2 H36D H 0.5700 0.1730 1.0683 0.091 Uiso 0.10 1 d PR D 2 C9D C 0.55007(10) 0.31611(10) 0.78745(7) 0.0218(4) Uani 1 1 d . E . C10D C 0.55893(10) 0.34973(10) 0.74004(7) 0.0222(4) Uani 1 1 d . . . C37D C 0.57460(10) 0.37181(10) 0.67667(7) 0.0193(4) Uani 0.10 1 d PR E 2 C38D C 0.53675(10) 0.45157(10) 0.65288(7) 0.029(9) Uiso 0.10 1 d PR E 2 H38D H 0.5027 0.4862 0.6760 0.035 Uiso 0.10 1 d PR E 2 C39D C 0.54872(10) 0.48067(10) 0.59525(7) 0.0292(5) Uani 0.10 1 d PR E 2 H39D H 0.5229 0.5352 0.5790 0.035 Uiso 0.10 1 d PR E 2 C40D C 0.59855(10) 0.43001(10) 0.56142(7) 0.0309(5) Uani 0.10 1 d PR E 2 H40D H 0.6067 0.4499 0.5220 0.037 Uiso 0.10 1 d PR E 2 C41D C 0.63640(10) 0.35025(10) 0.58520(7) 0.058(7) Uiso 0.10 1 d PR E 2 H41D H 0.6704 0.3156 0.5621 0.070 Uiso 0.10 1 d PR E 2 C42D C 0.62442(10) 0.32115(10) 0.64283(7) 0.049(7) Uiso 0.10 1 d PR E 2 H42D H 0.6503 0.2666 0.6591 0.059 Uiso 0.10 1 d PR E 2 C11D C 0.68403(12) 0.14019(15) 1.07711(10) 0.0180(4) Uani 0.90 1 d P D 1 C12D C 0.65465(11) 0.19337(11) 1.11416(8) 0.0223(4) Uani 0.90 1 d P D 1 H12D H 0.6422 0.2476 1.0993 0.027 Uiso 0.90 1 d PR D 1 C13D C 0.64361(11) 0.16733(11) 1.17233(8) 0.0252(4) Uani 0.90 1 d P D 1 H13D H 0.6245 0.2036 1.1976 0.030 Uiso 0.90 1 d PR D 1 C14D C 0.66037(12) 0.08860(12) 1.19409(8) 0.0277(5) Uani 0.90 1 d P D 1 H14D H 0.6519 0.0710 1.2339 0.033 Uiso 0.90 1 d PR D 1 C15D C 0.68880(13) 0.03523(12) 1.15713(12) 0.0308(5) Uani 0.90 1 d P D 1 H15D H 0.7003 -0.0188 1.1720 0.037 Uiso 0.90 1 d PR D 1 C16D C 0.70094(12) 0.06107(11) 1.09897(8) 0.0245(4) Uani 0.90 1 d P D 1 H16D H 0.7214 0.0242 1.0743 0.029 Uiso 0.90 1 d PR D 1 C17D C 0.56963(11) 0.38783(10) 0.68233(8) 0.0193(4) Uani 0.90 1 d P E 1 C18D C 0.5110(2) 0.45826(12) 0.65340(8) 0.0239(5) Uani 0.90 1 d P E 1 H18D H 0.4644 0.4855 0.6730 0.029 Uiso 0.90 1 d PR E 1 C19D C 0.52107(13) 0.49000(11) 0.59640(9) 0.0292(5) Uani 0.90 1 d P E 1 H19D H 0.4806 0.5383 0.5769 0.035 Uiso 0.90 1 d PR E 1 C20D C 0.58960(13) 0.45337(12) 0.56763(9) 0.0309(5) Uani 0.90 1 d P E 1 H20D H 0.5954 0.4748 0.5281 0.037 Uiso 0.90 1 d PR E 1 C21D C 0.64938(13) 0.38380(13) 0.59632(9) 0.0347(5) Uani 0.90 1 d P E 1 H21D H 0.6975 0.3585 0.5772 0.042 Uiso 0.90 1 d PR E 1 C22D C 0.63986(12) 0.35074(12) 0.65332(9) 0.0263(5) Uani 0.90 1 d P E 1 H22D H 0.6812 0.3030 0.6729 0.032 Uiso 0.90 1 d PR E 1 O1E O -0.01714(7) 0.23438(8) 0.33784(5) 0.0288(3) Uani 1 1 d . . . H01E H -0.0250 0.2111 0.3707 0.043 Uiso 1 1 d R . . O2E O 0.26893(6) 0.26069(6) 0.41272(5) 0.0194(3) Uani 1 1 d . . . H02E H 0.3126 0.2204 0.4191 0.029 Uiso 1 1 d R . . C1E C 0.05457(10) 0.25177(10) 0.34222(7) 0.0208(4) Uani 1 1 d . . . C2E C 0.13058(10) 0.17535(9) 0.35625(7) 0.0207(4) Uani 1 1 d . . . H2E1 H 0.1226 0.1415 0.3923 0.027 Uiso 1 1 d R . . H2E2 H 0.1377 0.1470 0.3238 0.027 Uiso 1 1 d R . . C3E C 0.20787(9) 0.19090(9) 0.36485(7) 0.0186(4) Uani 1 1 d . . . H3E1 H 0.2189 0.2201 0.3275 0.024 Uiso 1 1 d R . . H3E2 H 0.2552 0.1402 0.3756 0.024 Uiso 1 1 d R . . C4E C 0.20013(9) 0.23796(9) 0.41253(7) 0.0162(3) Uani 1 1 d . . . C5E C 0.12366(9) 0.31453(9) 0.39888(7) 0.0198(4) Uani 1 1 d . . . H5E1 H 0.1167 0.3425 0.4315 0.026 Uiso 1 1 d R . . H5E2 H 0.1313 0.3488 0.3630 0.026 Uiso 1 1 d R . . C6E C 0.04647(10) 0.29875(10) 0.39014(7) 0.0224(4) Uani 1 1 d . . . H6E1 H -0.0010 0.3494 0.3796 0.029 Uiso 1 1 d R . . H6E2 H 0.0356 0.2692 0.4274 0.029 Uiso 1 1 d R . . C7E C 0.06054(10) 0.29766(10) 0.28415(7) 0.0218(4) Uani 1 1 d . . . C8E C 0.06742(10) 0.33310(10) 0.23685(7) 0.0224(4) Uani 1 1 d . . . C9E C 0.19686(9) 0.19223(9) 0.47140(7) 0.0185(4) Uani 1 1 d . F . C10E C 0.19630(10) 0.15941(9) 0.52069(7) 0.0196(4) Uani 1 1 d . . . C27E C 0.18658(10) 0.12765(9) 0.58269(7) 0.0209(4) Uani 0.10 1 d PR F 2 C28E C 0.16424(10) 0.17977(9) 0.62049(7) 0.101(11) Uiso 0.10 1 d PR F 2 H28E H 0.1531 0.2338 0.6059 0.121 Uiso 0.10 1 d PR F 2 C29E C 0.15819(10) 0.15284(9) 0.67969(7) 0.075(8) Uiso 0.10 1 d PR F 2 H29E H 0.1429 0.1885 0.7055 0.090 Uiso 0.10 1 d PR F 2 C30E C 0.17448(10) 0.07379(9) 0.70111(7) 0.0406(5) Uani 0.10 1 d PR F 2 H30E H 0.1703 0.0554 0.7416 0.049 Uiso 0.10 1 d PR F 2 C31E C 0.19682(10) 0.02166(9) 0.66332(7) 0.052(6) Uiso 0.10 1 d PR F 2 H31E H 0.2079 -0.0324 0.6780 0.062 Uiso 0.10 1 d PR F 2 C32E C 0.20287(10) 0.04859(9) 0.60411(7) 0.068(8) Uiso 0.10 1 d PR F 2 H32E H 0.2181 0.0130 0.5783 0.082 Uiso 0.10 1 d PR F 2 C11E C 0.07490(10) 0.37250(10) 0.17876(7) 0.0218(4) Uani 1 1 d . . . C12E C 0.02518(11) 0.45074(10) 0.15720(7) 0.0265(4) Uani 1 1 d . . . H12E H -0.0129 0.4799 0.1817 0.032 Uiso 1 1 d R . . C13E C 0.03111(12) 0.48618(11) 0.10023(8) 0.0313(4) Uani 1 1 d . . . H13E H -0.0038 0.5394 0.0857 0.038 Uiso 1 1 d R . . C14E C 0.08682(11) 0.44532(12) 0.06449(8) 0.0331(5) Uani 1 1 d . . . H14E H 0.0906 0.4701 0.0254 0.040 Uiso 1 1 d R . . C15E C 0.13718(13) 0.36858(14) 0.08571(9) 0.0510(6) Uani 1 1 d . . . H15E H 0.1763 0.3403 0.0614 0.061 Uiso 1 1 d R . . C16E C 0.13097(12) 0.33196(12) 0.14240(9) 0.0449(6) Uani 1 1 d . . . H16E H 0.1656 0.2786 0.1565 0.054 Uiso 1 1 d R . . C17E C 0.19673(11) 0.12425(11) 0.58159(8) 0.0209(4) Uani 0.90 1 d P F 1 C18E C 0.26082(12) 0.11050(14) 0.62027(9) 0.0389(6) Uani 0.90 1 d P F 1 H18E H 0.3074 0.1207 0.6060 0.047 Uiso 0.90 1 d PR F 1 C19E C 0.25830(13) 0.08170(15) 0.67936(10) 0.0495(7) Uani 0.90 1 d P F 1 H19E H 0.3019 0.0741 0.7058 0.059 Uiso 0.90 1 d PR F 1 C20E C 0.19224(13) 0.06338(14) 0.69961(9) 0.0406(5) Uani 0.90 1 d P F 1 H20E H 0.1909 0.0419 0.7399 0.049 Uiso 0.90 1 d PR F 1 C21E C 0.12764(13) 0.07709(13) 0.66185(9) 0.0322(5) Uani 0.90 1 d P F 1 H21E H 0.0818 0.0654 0.6759 0.039 Uiso 0.90 1 d PR F 1 C22E C 0.12937(12) 0.10755(12) 0.60325(8) 0.0278(5) Uani 0.90 1 d P F 1 H22E H 0.0845 0.1169 0.5773 0.033 Uiso 0.90 1 d PR F 1 O1F O 0.27800(7) 0.25067(7) 0.90475(5) 0.0300(3) Uani 1 1 d . . . H01F H 0.2789 0.2839 0.8750 0.045 Uiso 1 1 d R . . O2F O -0.01767(7) 0.23462(6) 0.83917(5) 0.0220(3) Uani 1 1 d . . . H02F H -0.0601 0.2760 0.8315 0.033 Uiso 1 1 d R . . C1F C 0.20394(9) 0.23623(10) 0.90275(7) 0.0201(4) Uani 1 1 d . . . C2F C 0.20751(10) 0.18898(10) 0.85591(7) 0.0226(4) Uani 1 1 d . . . H2F1 H 0.2180 0.2170 0.8178 0.029 Uiso 1 1 d R . . H2F2 H 0.2537 0.1374 0.8663 0.029 Uiso 1 1 d R . . C3F C 0.12789(9) 0.17620(9) 0.84972(7) 0.0205(4) Uani 1 1 d . . . H3F1 H 0.1204 0.1431 0.8864 0.027 Uiso 1 1 d R . . H3F2 H 0.1317 0.1480 0.8176 0.027 Uiso 1 1 d R . . C4F C 0.05345(9) 0.25423(9) 0.83687(7) 0.0170(3) Uani 1 1 d . . . C5F C 0.05049(9) 0.30146(9) 0.88363(7) 0.0194(4) Uani 1 1 d . . . H5F1 H 0.0041 0.3530 0.8735 0.025 Uiso 1 1 d R . . H5F2 H 0.0404 0.2733 0.9218 0.025 Uiso 1 1 d R . . C6F C 0.12993(9) 0.31449(9) 0.88925(7) 0.0201(4) Uani 1 1 d . . . H6F1 H 0.1261 0.3434 0.9209 0.026 Uiso 1 1 d R . . H6F2 H 0.1376 0.3469 0.8523 0.026 Uiso 1 1 d R . . C7F C 0.19862(10) 0.19176(10) 0.96152(7) 0.0217(4) Uani 1 1 d . . . C8F C 0.19056(10) 0.15789(10) 1.00904(7) 0.0225(4) Uani 1 1 d . . . C9F C 0.05699(10) 0.29863(9) 0.77750(7) 0.0194(4) Uani 1 1 d . G . C10F C 0.05958(10) 0.33112(10) 0.72838(7) 0.0206(4) Uani 1 1 d . . . C27F C 0.04806(10) 0.37860(10) 0.66965(7) 0.0185(4) Uani 0.10 1 d PR G 2 C28F C 0.11346(10) 0.40072(10) 0.65285(7) 0.096(10) Uiso 0.10 1 d PR G 2 H28F H 0.1529 0.3966 0.6815 0.115 Uiso 0.10 1 d PR G 2 C29F C 0.12110(10) 0.42892(10) 0.59414(7) 0.079(9) Uiso 0.10 1 d PR G 2 H29F H 0.1658 0.4440 0.5827 0.094 Uiso 0.10 1 d PR G 2 C30F C 0.06335(10) 0.43501(10) 0.55223(7) 0.08(2) Uiso 0.10 1 d PR G 2 H30F H 0.0686 0.4543 0.5121 0.093 Uiso 0.10 1 d PR G 2 C31F C -0.00204(10) 0.41289(10) 0.56902(7) 0.104(11) Uiso 0.10 1 d PR G 2 H31F H -0.0415 0.4170 0.5404 0.124 Uiso 0.10 1 d PR G 2 C32F C -0.00968(10) 0.38468(10) 0.62773(7) 0.119(13) Uiso 0.10 1 d PR G 2 H32F H -0.0544 0.3696 0.6392 0.143 Uiso 0.10 1 d PR G 2 C11F C 0.18240(10) 0.12017(10) 1.06779(7) 0.0219(4) Uani 1 1 d . . . C12F C 0.12104(12) 0.16039(12) 1.10172(9) 0.0444(6) Uani 1 1 d . . . H12F H 0.0829 0.2117 1.0854 0.053 Uiso 1 1 d R . . C13F C 0.11488(13) 0.12641(13) 1.15888(9) 0.0526(7) Uani 1 1 d . . . H13F H 0.0722 0.1542 1.1813 0.063 Uiso 1 1 d R . . C14F C 0.16955(12) 0.05235(12) 1.18332(8) 0.0353(5) Uani 1 1 d . . . H14F H 0.1661 0.0298 1.2230 0.042 Uiso 1 1 d R . . C15F C 0.22990(12) 0.01145(10) 1.14994(8) 0.0290(4) Uani 1 1 d . . . H15F H 0.2676 -0.0399 1.1666 0.035 Uiso 1 1 d R . . C16F C 0.23604(11) 0.04449(10) 1.09241(7) 0.0244(4) Uani 1 1 d . . . H16F H 0.2771 0.0154 1.0696 0.029 Uiso 1 1 d R . . C17F C 0.06575(11) 0.36310(11) 0.66785(8) 0.0185(4) Uani 0.90 1 d P G 1 C18F C 0.04698(12) 0.44400(11) 0.64813(8) 0.0277(5) Uani 0.90 1 d P G 1 H18F H 0.0302 0.4785 0.6748 0.033 Uiso 0.90 1 d PR G 1 C19F C 0.05441(13) 0.47305(12) 0.58983(9) 0.0330(5) Uani 0.90 1 d P G 1 H19F H 0.0437 0.5273 0.5769 0.040 Uiso 0.90 1 d PR G 1 C20F C 0.0784(2) 0.42365(17) 0.55059(9) 0.0306(9) Uani 0.90 1 d P G 1 H20F H 0.0819 0.4444 0.5105 0.037 Uiso 0.90 1 d PR G 1 C21F C 0.09582(12) 0.34440(12) 0.56973(8) 0.0296(5) Uani 0.90 1 d P G 1 H21F H 0.1124 0.3105 0.5426 0.035 Uiso 0.90 1 d PR G 1 C22F C 0.08975(11) 0.31404(11) 0.62808(8) 0.0227(4) Uani 0.90 1 d P G 1 H22F H 0.1026 0.2594 0.6410 0.027 Uiso 0.90 1 d PR G 1 O1G O 0.92716(7) 0.14738(6) 0.92546(5) 0.0208(3) Uani 1 1 d . . . H01G H 0.9511 0.1655 0.8983 0.031 Uiso 1 1 d R . . C1G C 0.97370(10) 0.06492(9) 0.94692(7) 0.0177(3) Uani 1 1 d . . . C2G C 1.04252(10) 0.05429(9) 0.99058(7) 0.0189(4) Uani 1 1 d . . . H2G1 H 1.0829 0.0733 0.9696 0.025 Uiso 1 1 d R . . H2G2 H 1.0189 0.0864 1.0203 0.025 Uiso 1 1 d R . . C3G C 1.08636(10) -0.03134(9) 1.02134(7) 0.0199(4) Uani 1 1 d . . . H3G1 H 1.1288 -0.0353 1.0500 0.026 Uiso 1 1 d R . . H3G2 H 1.1142 -0.0627 0.9921 0.026 Uiso 1 1 d R . . C7G C 1.00679(10) 0.02740(9) 0.89697(7) 0.0207(4) Uani 1 1 d . . . C8G C 1.03112(10) -0.00263(10) 0.85602(7) 0.0236(4) Uani 1 1 d . . . C11G C 1.05638(10) -0.04028(10) 0.80676(7) 0.0229(4) Uani 1 1 d . . . C12G C 1.13422(12) -0.09894(12) 0.80748(9) 0.0429(5) Uani 1 1 d . . . H12G H 1.1728 -0.1119 0.8393 0.052 Uiso 1 1 d R . . C13G C 1.15544(14) -0.13818(13) 0.76154(9) 0.0514(6) Uani 1 1 d . . . H13G H 1.2085 -0.1782 0.7621 0.062 Uiso 1 1 d R . . C14G C 1.09988(12) -0.11915(12) 0.71481(8) 0.0362(5) Uani 1 1 d . . . H14G H 1.1142 -0.1474 0.6841 0.043 Uiso 1 1 d R . . C15G C 1.02527(12) -0.05967(12) 0.71290(8) 0.0362(5) Uani 1 1 d . . . H15G H 0.9878 -0.0459 0.6803 0.043 Uiso 1 1 d R . . C16G C 1.00341(11) -0.01954(11) 0.75834(8) 0.0317(4) Uani 1 1 d . . . H16G H 0.9512 0.0221 0.7564 0.038 Uiso 1 1 d R . . O1H O 0.42408(7) 0.14810(6) 0.42740(5) 0.0216(3) Uani 1 1 d . . . H01H H 0.4480 0.1652 0.3997 0.032 Uiso 1 1 d R . . C1H C 0.46896(10) 0.06526(9) 0.44754(7) 0.0180(3) Uani 1 1 d . . . C2H C 0.41103(9) 0.03526(9) 0.48578(7) 0.0197(4) Uani 1 1 d . . . H2H1 H 0.3909 0.0669 0.5162 0.026 Uiso 1 1 d R . . H2H2 H 0.3630 0.0418 0.4613 0.026 Uiso 1 1 d R . . C3H C 0.45406(10) -0.05113(9) 0.51507(7) 0.0208(4) Uani 1 1 d . . . H3H1 H 0.4700 -0.0832 0.4847 0.027 Uiso 1 1 d R . . H3H2 H 0.4155 -0.0681 0.5403 0.027 Uiso 1 1 d R . . C7H C 0.49123(10) 0.02611(9) 0.39744(7) 0.0211(4) Uani 1 1 d . H . C8H C 0.50850(10) -0.00696(10) 0.35763(7) 0.0228(4) Uani 1 1 d . . . C31H C 0.55232(10) -0.04187(10) 0.30246(7) 0.0174(4) Uani 0.10 1 d PR H 2 C32H C 0.50695(10) -0.01365(10) 0.24930(7) 0.0253(4) Uani 0.10 1 d PR H 2 H32H H 0.4609 0.0348 0.2431 0.030 Uiso 0.10 1 d PR H 2 C33H C 0.52893(10) -0.05636(10) 0.20519(7) 0.0312(5) Uani 0.10 1 d PR H 2 H33H H 0.4979 -0.0371 0.1689 0.037 Uiso 0.10 1 d PR H 2 C34H C 0.59627(10) -0.12730(10) 0.21424(7) 0.100(19) Uiso 0.10 1 d PR H 2 H34H H 0.6113 -0.1565 0.1841 0.120 Uiso 0.10 1 d PR H 2 C35H C 0.64164(10) -0.15552(10) 0.26740(7) 0.081(9) Uiso 0.10 1 d PR H 2 H35H H 0.6877 -0.2040 0.2736 0.097 Uiso 0.10 1 d PR H 2 C36H C 0.61966(10) -0.11280(10) 0.31151(7) 0.060(7) Uiso 0.10 1 d PR H 2 H36H H 0.6507 -0.1321 0.3478 0.072 Uiso 0.10 1 d PR H 2 C11H C 0.52652(10) -0.04490(10) 0.30863(8) 0.0174(4) Uani 0.90 1 d P H 1 C12H C 0.51146(12) 0.00104(11) 0.25181(8) 0.0253(4) Uani 0.90 1 d P H 1 H12H H 0.4880 0.0567 0.2456 0.030 Uiso 0.90 1 d PR H 1 C13H C 0.52878(13) -0.03464(12) 0.20425(8) 0.0312(5) Uani 0.90 1 d P H 1 H13H H 0.5167 -0.0035 0.1657 0.037 Uiso 0.90 1 d PR H 1 C14H C 0.56295(19) -0.11611(13) 0.21215(9) 0.0310(5) Uani 0.90 1 d P H 1 H14H H 0.5772 -0.1403 0.1793 0.037 Uiso 0.90 1 d PR H 1 C15H C 0.57751(13) -0.16145(12) 0.26816(9) 0.0320(5) Uani 0.90 1 d P H 1 H15H H 0.5996 -0.2171 0.2738 0.038 Uiso 0.90 1 d PR H 1 C16H C 0.55972(12) -0.12633(11) 0.31624(8) 0.0249(4) Uani 0.90 1 d P H 1 H16H H 0.5695 -0.1578 0.3546 0.030 Uiso 0.90 1 d PR H 1 O1I O 0.43704(7) 0.15428(7) -0.06582(5) 0.0228(3) Uani 1 1 d . . . H01I H 0.3860 0.1797 -0.0677 0.034 Uiso 1 1 d R . . C1I C 0.45876(9) 0.08760(9) -0.01805(7) 0.0174(3) Uani 1 1 d . . . C2I C 0.55228(9) 0.04498(9) -0.01723(7) 0.0190(4) Uani 1 1 d . . . H2I1 H 0.5683 0.0341 -0.0565 0.025 Uiso 1 1 d R . . H2I2 H 0.5789 0.0795 -0.0081 0.025 Uiso 1 1 d R . . C3I C 0.58298(9) -0.03234(9) 0.02803(7) 0.0186(4) Uani 1 1 d . . . H3I1 H 0.5719 -0.0210 0.0677 0.024 Uiso 1 1 d R . . H3I2 H 0.6431 -0.0589 0.0260 0.024 Uiso 1 1 d R . . C7I C 0.43407(9) 0.11387(9) 0.03745(7) 0.0187(4) Uani 1 1 d . . . C8I C 0.41328(10) 0.13533(9) 0.08241(7) 0.0201(4) Uani 1 1 d . . . C11I C 0.39175(10) 0.16157(9) 0.13661(7) 0.0193(4) Uani 1 1 d . . . C12I C 0.43518(11) 0.19985(10) 0.15811(7) 0.0266(4) Uani 1 1 d . . . H12I H 0.4782 0.2092 0.1366 0.032 Uiso 1 1 d R . . C13I C 0.41604(12) 0.22418(11) 0.21065(8) 0.0312(4) Uani 1 1 d . . . H13I H 0.4457 0.2505 0.2249 0.037 Uiso 1 1 d R . . C14I C 0.35401(11) 0.21028(11) 0.24230(8) 0.0301(4) Uani 1 1 d . . . H14I H 0.3411 0.2268 0.2784 0.036 Uiso 1 1 d R . . C15I C 0.31101(11) 0.17217(11) 0.22136(8) 0.0309(4) Uani 1 1 d . . . H15I H 0.2685 0.1625 0.2433 0.037 Uiso 1 1 d R . . C16I C 0.32921(10) 0.14813(10) 0.16863(8) 0.0249(4) Uani 1 1 d . . . H16I H 0.2989 0.1225 0.1543 0.030 Uiso 1 1 d R . . O1J O 0.93619(7) 0.15284(7) 0.43285(5) 0.0257(3) Uani 1 1 d . . . H01J H 0.8852 0.1782 0.4312 0.039 Uiso 1 1 d R . . C1J C 0.95837(10) 0.08684(10) 0.48122(7) 0.0197(4) Uani 1 1 d . . . C2J C 0.91682(10) 0.03130(10) 0.47226(7) 0.0206(4) Uani 1 1 d . . . H2J1 H 0.8567 0.0578 0.4744 0.027 Uiso 1 1 d R . . H2J2 H 0.9278 0.0188 0.4329 0.027 Uiso 1 1 d R . . C3J C 0.94818(9) -0.04467(10) 0.51847(7) 0.0204(4) Uani 1 1 d . . . H3J1 H 0.9217 -0.0799 0.5107 0.027 Uiso 1 1 d R . . H3J2 H 0.9327 -0.0326 0.5575 0.027 Uiso 1 1 d R . . C7J C 0.93344(10) 0.11421(10) 0.53638(7) 0.0206(4) Uani 1 1 d . . . C8J C 0.91187(10) 0.13557(10) 0.58112(7) 0.0222(4) Uani 1 1 d . . . C11J C 0.88892(10) 0.16073(10) 0.63581(7) 0.0216(4) Uani 1 1 d . . . C12J C 0.83289(10) 0.13873(10) 0.67019(7) 0.0221(4) Uani 1 1 d . . . H12J H 0.8075 0.1081 0.6571 0.026 Uiso 1 1 d R . . C13J C 0.81401(10) 0.16091(10) 0.72351(8) 0.0257(4) Uani 1 1 d . . . H13J H 0.7760 0.1451 0.7469 0.031 Uiso 1 1 d R . . C15J C 0.90532(13) 0.22887(13) 0.70890(9) 0.0430(5) Uani 1 1 d . . . H15J H 0.9299 0.2601 0.7220 0.052 Uiso 1 1 d R . . C14J C 0.85032(11) 0.20569(11) 0.74305(8) 0.0314(4) Uani 1 1 d . . . H14J H 0.8374 0.2205 0.7798 0.038 Uiso 1 1 d R . . C16J C 0.92472(12) 0.20652(12) 0.65568(8) 0.0381(5) Uani 1 1 d . . . H16J H 0.9626 0.2227 0.6323 0.046 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1A 0.0188(6) 0.0481(9) 0.0281(7) 0.0137(6) -0.0040(5) -0.0183(6) O2A 0.0185(6) 0.0188(6) 0.0252(7) 0.0010(5) -0.0019(5) -0.0079(5) C1A 0.0151(8) 0.0303(10) 0.0209(9) 0.0052(8) -0.0013(7) -0.0095(7) C2A 0.0217(9) 0.0271(10) 0.0196(9) -0.0026(7) -0.0008(7) -0.0113(8) C3A 0.0163(8) 0.0231(9) 0.0173(9) -0.0045(7) 0.0032(7) -0.0063(7) C4A 0.0167(8) 0.0182(8) 0.0159(8) -0.0017(7) 0.0023(7) -0.0066(7) C5A 0.0218(9) 0.0185(9) 0.0172(9) -0.0005(7) 0.0009(7) -0.0021(7) C6A 0.0174(9) 0.0298(10) 0.0175(9) 0.0017(8) 0.0049(7) -0.0010(8) C7A 0.0172(9) 0.0318(10) 0.0220(10) -0.0002(8) -0.0004(7) -0.0098(8) C8A 0.0194(9) 0.0325(10) 0.0206(10) -0.0003(8) -0.0015(7) -0.0109(8) C31A 0.0195(9) 0.0290(10) 0.0161(9) -0.0004(8) -0.0012(7) -0.0124(8) C9A 0.0176(8) 0.0190(9) 0.0201(9) -0.0040(7) 0.0011(7) -0.0053(7) C10A 0.0191(9) 0.0223(9) 0.0210(9) -0.0039(7) 0.0012(7) -0.0071(7) C47A 0.0254(11) 0.0141(11) 0.0128(10) -0.0033(8) 0.0024(8) -0.0089(8) C48A 0.0238(11) 0.0241(11) 0.0173(10) -0.0012(9) -0.0005(8) -0.0118(9) C49A 0.0345(12) 0.0388(13) 0.0195(11) -0.0060(10) 0.0062(9) -0.0247(11) C11A 0.0195(9) 0.0290(10) 0.0161(9) -0.0004(8) -0.0012(7) -0.0124(8) C12A 0.0291(13) 0.0243(12) 0.0214(12) -0.0075(9) 0.0013(9) -0.0149(9) C13A 0.0376(15) 0.0237(11) 0.0214(12) 0.0024(9) -0.0059(9) -0.0175(10) C14A 0.0310(13) 0.0389(13) 0.0139(10) -0.0010(11) 0.0013(8) -0.0221(10) C15A 0.0250(11) 0.0358(12) 0.0238(11) -0.0077(9) 0.0084(9) -0.0072(9) C16A 0.0241(10) 0.0211(10) 0.0265(11) 0.0014(9) 0.0010(8) -0.0027(9) C17A 0.0254(11) 0.0141(11) 0.0128(10) -0.0033(8) 0.0024(8) -0.0089(8) C18A 0.0238(11) 0.0241(11) 0.0173(10) -0.0012(9) -0.0005(8) -0.0118(9) C19A 0.0345(12) 0.0388(13) 0.0195(11) -0.0060(10) 0.0062(9) -0.0247(11) C20A 0.0493(16) 0.0218(12) 0.0148(12) 0.0010(10) 0.0081(11) -0.0173(11) C21A 0.0360(13) 0.0226(12) 0.0170(11) 0.0012(9) -0.0004(10) 0.0016(10) C22A 0.0242(12) 0.0241(12) 0.0156(11) -0.0001(9) 0.0053(9) -0.0009(9) O1B 0.0220(6) 0.0155(6) 0.0233(7) 0.0023(5) 0.0014(5) -0.0050(5) O2B 0.0224(6) 0.0147(6) 0.0196(6) 0.0017(5) 0.0039(5) -0.0041(5) C1B 0.0197(8) 0.0129(8) 0.0160(8) 0.0004(6) -0.0004(7) -0.0061(7) C2B 0.0172(8) 0.0209(9) 0.0205(9) 0.0012(7) -0.0012(7) -0.0083(7) C3B 0.0225(9) 0.0177(9) 0.0205(9) 0.0000(7) -0.0005(7) -0.0118(7) C4B 0.0184(8) 0.0128(8) 0.0167(8) -0.0011(6) -0.0005(7) -0.0033(7) C5B 0.0188(8) 0.0209(9) 0.0189(9) -0.0012(7) 0.0006(7) -0.0086(7) C6B 0.0213(9) 0.0193(9) 0.0187(9) -0.0022(7) -0.0004(7) -0.0110(7) C7B 0.0247(9) 0.0190(9) 0.0174(9) 0.0013(7) -0.0032(7) -0.0090(7) C8B 0.0332(10) 0.0193(9) 0.0187(9) 0.0015(7) -0.0036(8) -0.0091(8) C9B 0.0226(9) 0.0176(9) 0.0175(9) 0.0011(7) 0.0000(7) -0.0049(7) C10B 0.0290(10) 0.0206(9) 0.0203(9) -0.0021(7) 0.0008(8) -0.0050(8) C28B 0.0264(10) 0.0283(10) 0.0223(10) -0.0014(8) 0.0035(8) -0.0092(8) C29B 0.0358(11) 0.0439(13) 0.0177(10) -0.0071(9) 0.0041(8) -0.0173(10) C11B 0.0440(11) 0.0230(10) 0.0169(9) -0.0040(7) 0.0008(8) -0.0143(9) C12B 0.138(3) 0.0234(12) 0.0244(12) -0.0039(9) -0.0092(14) 0.0037(14) C13B 0.164(3) 0.0233(12) 0.0361(14) -0.0116(11) 0.0065(17) -0.0046(15) C14B 0.0944(19) 0.0437(14) 0.0235(11) -0.0163(10) 0.0138(12) -0.0390(14) C15B 0.0485(13) 0.0580(15) 0.0182(10) -0.0057(10) 0.0021(9) -0.0282(12) C16B 0.0326(11) 0.0369(11) 0.0220(10) -0.0046(8) 0.0021(8) -0.0122(9) C17B 0.0245(11) 0.0243(11) 0.0162(11) -0.0046(8) 0.0081(8) -0.0113(10) C18B 0.0264(10) 0.0283(10) 0.0223(10) -0.0014(8) 0.0035(8) -0.0092(8) C19B 0.0358(11) 0.0439(13) 0.0177(10) -0.0071(9) 0.0041(8) -0.0173(10) C20B 0.0387(16) 0.0438(15) 0.0267(13) -0.0205(10) 0.0139(10) -0.0198(11) C21B 0.0452(14) 0.0357(13) 0.0331(13) -0.0155(11) 0.0041(11) 0.0046(11) C22B 0.0381(13) 0.0367(13) 0.0215(11) -0.0093(10) -0.0010(9) -0.0001(10) O1C 0.0193(6) 0.0247(7) 0.0186(6) 0.0057(5) 0.0008(5) -0.0061(5) O2C 0.0217(6) 0.0224(6) 0.0193(6) 0.0028(5) 0.0038(5) -0.0069(5) C1C 0.0182(8) 0.0196(8) 0.0113(8) 0.0004(7) 0.0004(6) -0.0068(7) C2C 0.0173(8) 0.0224(9) 0.0155(8) -0.0012(7) 0.0018(7) -0.0089(7) C3C 0.0170(8) 0.0205(9) 0.0143(8) -0.0017(7) 0.0003(6) -0.0066(7) C4C 0.0194(8) 0.0183(8) 0.0129(8) -0.0014(7) 0.0026(7) -0.0070(7) C5C 0.0192(8) 0.0227(9) 0.0146(8) -0.0033(7) 0.0037(7) -0.0110(7) C6C 0.0153(8) 0.0253(9) 0.0149(8) -0.0052(7) 0.0020(6) -0.0089(7) C7C 0.0184(8) 0.0177(8) 0.0187(9) -0.0005(7) -0.0006(7) -0.0067(7) C8C 0.0211(9) 0.0193(9) 0.0206(9) -0.0026(7) 0.0006(7) -0.0077(7) C9C 0.0195(8) 0.0205(9) 0.0203(9) -0.0034(7) 0.0029(7) -0.0090(7) C10C 0.0238(9) 0.0225(9) 0.0203(9) -0.0054(7) 0.0035(7) -0.0104(7) C11C 0.0237(9) 0.0200(9) 0.0172(9) -0.0053(7) -0.0016(7) -0.0058(7) C12C 0.0241(10) 0.0484(12) 0.0308(11) -0.0244(9) 0.0031(8) -0.0155(9) C13C 0.0244(10) 0.0702(15) 0.0382(12) -0.0356(11) 0.0100(9) -0.0173(10) C14C 0.0382(11) 0.0440(12) 0.0281(11) -0.0221(9) 0.0000(9) -0.0117(10) C15C 0.0544(14) 0.0537(14) 0.0290(11) -0.0145(10) -0.0023(10) -0.0367(11) C16C 0.0397(11) 0.0492(13) 0.0225(10) -0.0109(9) 0.0042(8) -0.0291(10) C17C 0.0259(9) 0.0244(9) 0.0202(9) -0.0104(7) 0.0050(7) -0.0105(8) C18C 0.0594(14) 0.0585(14) 0.0387(12) -0.0282(11) 0.0288(11) -0.0466(12) C19C 0.0671(15) 0.0678(16) 0.0463(14) -0.0413(12) 0.0279(12) -0.0512(13) C20C 0.0398(11) 0.0484(13) 0.0290(11) -0.0260(10) 0.0157(9) -0.0251(10) C21C 0.0245(9) 0.0346(11) 0.0234(10) -0.0119(8) 0.0095(8) -0.0143(8) C22C 0.0218(9) 0.0235(9) 0.0220(9) -0.0087(7) 0.0027(7) -0.0101(7) O1D 0.0171(6) 0.0199(6) 0.0311(7) 0.0042(5) -0.0025(5) -0.0081(5) O2D 0.0185(6) 0.0312(7) 0.0299(7) 0.0106(6) -0.0035(5) -0.0128(5) C1D 0.0156(8) 0.0176(8) 0.0203(9) 0.0010(7) 0.0007(7) -0.0066(7) C2D 0.0171(8) 0.0186(9) 0.0196(9) -0.0029(7) 0.0022(7) -0.0031(7) C3D 0.0205(9) 0.0192(9) 0.0211(9) -0.0013(7) -0.0003(7) -0.0072(7) C4D 0.0151(8) 0.0205(9) 0.0207(9) 0.0027(7) -0.0003(7) -0.0061(7) C5D 0.0175(8) 0.0200(9) 0.0204(9) -0.0004(7) 0.0032(7) -0.0013(7) C6D 0.0229(9) 0.0172(9) 0.0221(9) -0.0028(7) 0.0011(7) -0.0059(7) C7D 0.0194(9) 0.0195(9) 0.0225(10) -0.0023(7) -0.0005(7) -0.0079(7) C8D 0.0202(9) 0.0225(9) 0.0214(9) -0.0012(7) -0.0026(7) -0.0101(7) C9D 0.0182(9) 0.0218(9) 0.0233(10) -0.0008(7) -0.0008(7) -0.0070(7) C10D 0.0201(9) 0.0221(9) 0.0236(10) -0.0011(7) -0.0016(7) -0.0088(7) C37D 0.0250(9) 0.0184(9) 0.0180(9) -0.0028(7) -0.0024(7) -0.0124(8) C39D 0.0374(13) 0.0199(10) 0.0260(11) 0.0030(8) -0.0065(9) -0.0096(9) C40D 0.0448(12) 0.0292(12) 0.0210(10) 0.0016(9) 0.0021(9) -0.0201(10) C11D 0.0165(10) 0.0223(10) 0.0155(10) 0.0006(10) -0.0024(8) -0.0098(8) C12D 0.0211(10) 0.0184(10) 0.0253(11) -0.0021(8) 0.0011(8) -0.0062(8) C13D 0.0265(10) 0.0245(11) 0.0235(11) -0.0092(8) 0.0052(8) -0.0068(9) C14D 0.0346(12) 0.0314(12) 0.0148(10) -0.0026(9) 0.0035(8) -0.0113(10) C15D 0.0472(15) 0.0201(11) 0.0228(13) 0.0000(9) -0.0003(10) -0.0124(10) C16D 0.0358(12) 0.0192(10) 0.0181(10) -0.0041(8) -0.0025(8) -0.0096(9) C17D 0.0250(9) 0.0184(9) 0.0180(9) -0.0028(7) -0.0024(7) -0.0124(8) C18D 0.0252(14) 0.0211(12) 0.0235(14) -0.0046(8) -0.0006(8) -0.0065(9) C19D 0.0374(13) 0.0199(10) 0.0260(11) 0.0030(8) -0.0065(9) -0.0096(9) C20D 0.0448(12) 0.0292(12) 0.0210(10) 0.0016(9) 0.0021(9) -0.0201(10) C21D 0.0355(13) 0.0366(13) 0.0308(12) -0.0046(10) 0.0123(10) -0.0143(11) C22D 0.0255(11) 0.0221(10) 0.0257(11) 0.0017(9) -0.0001(8) -0.0060(9) O1E 0.0219(6) 0.0398(8) 0.0245(7) 0.0080(6) -0.0042(5) -0.0185(6) O2E 0.0172(6) 0.0180(6) 0.0225(6) -0.0006(5) -0.0017(5) -0.0078(5) C1E 0.0172(8) 0.0287(10) 0.0167(9) 0.0005(7) -0.0006(7) -0.0116(7) C2E 0.0218(9) 0.0224(9) 0.0183(9) -0.0020(7) -0.0014(7) -0.0100(7) C3E 0.0171(8) 0.0206(9) 0.0174(9) -0.0049(7) 0.0020(7) -0.0059(7) C4E 0.0152(8) 0.0188(8) 0.0142(8) -0.0014(7) 0.0000(6) -0.0070(7) C5E 0.0213(9) 0.0186(9) 0.0156(9) -0.0020(7) 0.0016(7) -0.0042(7) C6E 0.0160(8) 0.0252(9) 0.0183(9) 0.0004(7) 0.0028(7) -0.0020(7) C7E 0.0179(9) 0.0277(10) 0.0192(9) -0.0013(8) -0.0020(7) -0.0096(7) C8E 0.0197(9) 0.0261(10) 0.0200(9) -0.0007(7) -0.0031(7) -0.0089(7) C9E 0.0171(8) 0.0187(9) 0.0188(9) -0.0035(7) -0.0009(7) -0.0059(7) C10E 0.0175(8) 0.0191(9) 0.0220(9) -0.0037(7) -0.0011(7) -0.0071(7) C27E 0.0209(9) 0.0194(9) 0.0205(9) -0.0004(7) 0.0026(7) -0.0075(7) C30E 0.0373(13) 0.0508(14) 0.0232(11) 0.0115(10) 0.0049(9) -0.0152(11) C11E 0.0200(9) 0.0281(10) 0.0167(9) 0.0021(7) -0.0029(7) -0.0116(8) C12E 0.0376(11) 0.0241(10) 0.0215(10) -0.0080(8) 0.0001(8) -0.0143(8) C13E 0.0476(12) 0.0216(10) 0.0263(10) 0.0020(8) -0.0047(9) -0.0179(9) C14E 0.0339(11) 0.0450(12) 0.0215(10) 0.0080(9) -0.0012(8) -0.0235(10) C15E 0.0348(12) 0.0641(16) 0.0290(12) 0.0017(11) 0.0146(9) 0.0022(11) C16E 0.0347(12) 0.0400(13) 0.0311(12) 0.0074(10) 0.0073(9) 0.0096(10) C17E 0.0209(9) 0.0194(9) 0.0205(9) -0.0004(7) 0.0026(7) -0.0075(7) C18E 0.0227(11) 0.0661(16) 0.0211(11) 0.0142(11) -0.0027(9) -0.0207(11) C19E 0.0289(12) 0.0816(19) 0.0279(13) 0.0181(12) -0.0065(10) -0.0241(13) C20E 0.0373(13) 0.0508(14) 0.0232(11) 0.0115(10) 0.0049(9) -0.0152(11) C21E 0.0353(12) 0.0450(13) 0.0271(12) -0.0071(10) 0.0115(10) -0.0281(11) C22E 0.0292(11) 0.0431(13) 0.0214(11) -0.0087(9) 0.0037(9) -0.0242(10) O1F 0.0195(6) 0.0364(8) 0.0305(8) 0.0133(6) -0.0069(5) -0.0162(6) O2F 0.0181(6) 0.0204(6) 0.0269(7) 0.0020(5) -0.0027(5) -0.0097(5) C1F 0.0145(8) 0.0233(9) 0.0201(9) 0.0034(7) -0.0019(7) -0.0082(7) C2F 0.0160(8) 0.0234(9) 0.0203(9) 0.0004(7) 0.0036(7) -0.0013(7) C3F 0.0215(9) 0.0179(9) 0.0185(9) -0.0026(7) 0.0019(7) -0.0043(7) C4F 0.0148(8) 0.0176(8) 0.0170(9) -0.0010(7) -0.0001(7) -0.0058(7) C5F 0.0174(8) 0.0207(9) 0.0175(9) -0.0030(7) 0.0021(7) -0.0050(7) C6F 0.0214(9) 0.0192(9) 0.0190(9) -0.0007(7) -0.0016(7) -0.0083(7) C7F 0.0192(9) 0.0236(9) 0.0210(9) 0.0000(7) -0.0029(7) -0.0088(7) C8F 0.0191(9) 0.0252(9) 0.0215(10) -0.0007(8) -0.0032(7) -0.0084(7) C9F 0.0175(8) 0.0201(9) 0.0204(9) -0.0040(7) 0.0001(7) -0.0071(7) C10F 0.0210(9) 0.0225(9) 0.0192(9) -0.0029(7) -0.0002(7) -0.0100(7) C27F 0.0165(9) 0.0212(10) 0.0175(9) -0.0019(7) -0.0006(7) -0.0077(8) C11F 0.0199(9) 0.0269(10) 0.0185(9) 0.0018(7) -0.0021(7) -0.0115(8) C12F 0.0339(11) 0.0380(12) 0.0330(12) 0.0102(9) 0.0059(9) 0.0081(9) C13F 0.0427(13) 0.0546(15) 0.0332(12) 0.0053(11) 0.0174(10) 0.0030(11) C14F 0.0424(12) 0.0401(12) 0.0209(10) 0.0054(9) 0.0023(9) -0.0190(10) C15F 0.0407(11) 0.0189(9) 0.0256(10) 0.0023(8) -0.0034(8) -0.0127(8) C16F 0.0313(10) 0.0204(9) 0.0226(10) -0.0058(7) 0.0007(8) -0.0105(8) C17F 0.0165(9) 0.0212(10) 0.0175(9) -0.0019(7) -0.0006(7) -0.0077(8) C18F 0.0435(13) 0.0207(10) 0.0196(10) -0.0025(8) -0.0025(9) -0.0135(9) C19F 0.0490(14) 0.0245(11) 0.0242(11) 0.0073(9) -0.0073(10) -0.0180(10) C20F 0.0374(13) 0.0399(15) 0.0137(12) 0.0022(9) 0.0020(9) -0.0178(10) C21F 0.0331(12) 0.0342(12) 0.0190(10) -0.0071(9) 0.0065(9) -0.0099(10) C22F 0.0247(10) 0.0221(10) 0.0211(10) -0.0041(8) 0.0045(8) -0.0093(8) O1G 0.0214(6) 0.0135(6) 0.0223(7) 0.0014(5) 0.0025(5) -0.0035(5) C1G 0.0190(8) 0.0121(8) 0.0192(9) -0.0012(7) -0.0007(7) -0.0039(7) C2G 0.0209(9) 0.0192(9) 0.0189(9) -0.0024(7) -0.0001(7) -0.0109(7) C3G 0.0188(8) 0.0192(9) 0.0202(9) -0.0010(7) -0.0011(7) -0.0070(7) C7G 0.0216(9) 0.0171(9) 0.0204(9) -0.0004(7) -0.0004(7) -0.0059(7) C8G 0.0258(9) 0.0204(9) 0.0224(9) -0.0015(7) 0.0007(7) -0.0079(7) C11G 0.0285(10) 0.0236(9) 0.0175(9) -0.0047(7) 0.0039(7) -0.0110(8) C12G 0.0385(12) 0.0476(13) 0.0310(11) -0.0175(10) -0.0047(9) 0.0014(10) C13G 0.0437(13) 0.0547(15) 0.0414(13) -0.0266(11) 0.0012(11) 0.0053(11) C14G 0.0442(12) 0.0434(12) 0.0305(11) -0.0206(9) 0.0106(9) -0.0214(10) C15G 0.0312(11) 0.0602(14) 0.0236(10) -0.0147(10) 0.0027(8) -0.0216(10) C16G 0.0221(9) 0.0412(12) 0.0296(11) -0.0104(9) 0.0040(8) -0.0083(9) O1H 0.0220(6) 0.0143(6) 0.0230(7) 0.0012(5) 0.0020(5) -0.0033(5) C1H 0.0197(8) 0.0139(8) 0.0171(9) -0.0006(7) -0.0024(7) -0.0039(7) C2H 0.0182(8) 0.0184(9) 0.0192(9) 0.0005(7) -0.0025(7) -0.0053(7) C3H 0.0228(9) 0.0186(9) 0.0218(9) -0.0007(7) -0.0018(7) -0.0104(7) C7H 0.0222(9) 0.0187(9) 0.0188(9) 0.0000(7) -0.0028(7) -0.0055(7) C8H 0.0234(9) 0.0204(9) 0.0202(9) -0.0001(7) -0.0023(7) -0.0055(7) C31H 0.0142(9) 0.0208(9) 0.0180(9) -0.0044(7) 0.0050(7) -0.0075(7) C32H 0.0331(10) 0.0175(10) 0.0201(9) -0.0016(8) 0.0026(8) -0.0053(8) C33H 0.0449(12) 0.0267(12) 0.0149(9) -0.0009(8) 0.0030(8) -0.0078(10) C11H 0.0142(9) 0.0208(9) 0.0180(9) -0.0044(7) 0.0050(7) -0.0075(7) C12H 0.0331(10) 0.0175(10) 0.0201(9) -0.0016(8) 0.0026(8) -0.0053(8) C13H 0.0449(12) 0.0267(12) 0.0149(9) -0.0009(8) 0.0030(8) -0.0078(10) C14H 0.0448(15) 0.0289(13) 0.0192(12) -0.0112(9) 0.0049(9) -0.0111(10) C15H 0.0454(13) 0.0187(10) 0.0305(12) -0.0072(9) 0.0043(10) -0.0097(10) C16H 0.0329(11) 0.0202(10) 0.0179(10) 0.0018(8) 0.0013(8) -0.0088(9) O1I 0.0200(6) 0.0249(7) 0.0174(6) 0.0050(5) 0.0014(5) -0.0067(5) C1I 0.0186(8) 0.0201(9) 0.0119(8) 0.0000(7) 0.0009(6) -0.0073(7) C2I 0.0163(8) 0.0243(9) 0.0165(9) -0.0021(7) 0.0022(7) -0.0090(7) C3I 0.0163(8) 0.0239(9) 0.0144(8) -0.0019(7) 0.0000(6) -0.0075(7) C7I 0.0178(8) 0.0203(9) 0.0174(9) -0.0011(7) 0.0012(7) -0.0083(7) C8I 0.0203(9) 0.0180(9) 0.0200(9) -0.0013(7) -0.0015(7) -0.0064(7) C11I 0.0219(9) 0.0152(8) 0.0181(9) -0.0040(7) -0.0013(7) -0.0036(7) C12I 0.0325(10) 0.0311(10) 0.0219(10) -0.0031(8) 0.0004(8) -0.0195(8) C13I 0.0451(12) 0.0321(11) 0.0261(10) -0.0094(8) -0.0035(9) -0.0231(9) C14I 0.0332(10) 0.0344(11) 0.0254(10) -0.0170(8) 0.0021(8) -0.0106(9) C15I 0.0244(10) 0.0435(12) 0.0293(11) -0.0181(9) 0.0085(8) -0.0132(9) C16I 0.0210(9) 0.0322(10) 0.0261(10) -0.0142(8) 0.0031(7) -0.0114(8) O1J 0.0211(6) 0.0327(7) 0.0189(6) 0.0044(5) 0.0017(5) -0.0102(6) C1J 0.0191(8) 0.0271(9) 0.0131(8) -0.0005(7) 0.0016(7) -0.0108(7) C2J 0.0177(8) 0.0303(10) 0.0143(8) -0.0030(7) 0.0010(7) -0.0106(7) C3J 0.0187(8) 0.0295(10) 0.0160(9) -0.0029(7) 0.0036(7) -0.0134(7) C7J 0.0189(9) 0.0256(9) 0.0182(9) -0.0020(7) 0.0010(7) -0.0106(7) C8J 0.0195(9) 0.0272(10) 0.0208(9) -0.0038(8) 0.0012(7) -0.0105(7) C11J 0.0228(9) 0.0256(9) 0.0179(9) -0.0059(7) 0.0004(7) -0.0101(8) C12J 0.0193(9) 0.0267(9) 0.0237(9) -0.0095(8) 0.0008(7) -0.0104(7) C13J 0.0228(9) 0.0318(10) 0.0248(10) -0.0102(8) 0.0066(7) -0.0113(8) C15J 0.0570(14) 0.0629(15) 0.0348(12) -0.0251(11) 0.0121(10) -0.0445(12) C14J 0.0334(11) 0.0428(12) 0.0246(10) -0.0175(9) 0.0064(8) -0.0168(9) C16J 0.0475(13) 0.0584(14) 0.0308(11) -0.0180(10) 0.0141(9) -0.0412(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1A C1A 1.4376(19) . ? O2A C4A 1.4307(18) . ? C1A C7A 1.481(2) . ? C1A C6A 1.532(2) . ? C1A C2A 1.534(2) . ? C2A C3A 1.527(2) . ? C3A C4A 1.528(2) . ? C4A C9A 1.480(2) . ? C4A C5A 1.532(2) . ? C5A C6A 1.519(2) . ? C7A C8A 1.194(2) . ? C8A C31A 1.4082 . ? C8A C11A 1.442(2) . ? C31A C36A 1.3900 . ? C31A C32A 1.3900 . ? C32A C33A 1.3900 . ? C33A C34A 1.3900 . ? C34A C35A 1.3900 . ? C35A C36A 1.3900 . ? C9A C10A 1.193(2) . ? C10A C17A 1.433(3) . ? C10A C37A 1.4884 . ? C10A C47A 1.5746 . ? C37A C42A 1.3900 . ? C37A C38A 1.3901 . ? C38A C39A 1.3900 . ? C39A C40A 1.3900 . ? C40A C41A 1.3900 . ? C41A C42A 1.3900 . ? C47A C52A 1.3900 . ? C47A C48A 1.3900 . ? C48A C49A 1.3900 . ? C49A C50A 1.3900 . ? C50A C51A 1.3900 . ? C51A C52A 1.3900 . ? C11A C16A 1.390(3) . ? C11A C12A 1.402(3) . ? C12A C13A 1.388(3) . ? C13A C14A 1.379(4) . ? C14A C15A 1.389(3) . ? C15A C16A 1.382(3) . ? C17A C22A 1.387(3) . ? C17A C18A 1.396(3) . ? C18A C19A 1.383(3) . ? C19A C20A 1.386(3) . ? C20A C21A 1.387(3) . ? C21A C22A 1.385(3) . ? O1B C1B 1.4386(18) . ? O2B C4B 1.4388(18) . ? C1B C7B 1.477(2) . ? C1B C2B 1.533(2) . ? C1B C6B 1.536(2) . ? C2B C3B 1.528(2) . ? C3B C4B 1.536(2) . ? C4B C9B 1.479(2) . ? C4B C5B 1.531(2) . ? C5B C6B 1.527(2) . ? C7B C8B 1.194(2) . ? C8B C11B 1.443(2) . ? C9B C10B 1.192(2) . ? C10B C17B 1.446(2) . ? C10B C27B 1.4487 . ? C27B C32B 1.3900 . ? C27B C28B 1.3900 . ? C28B C29B 1.3900 . ? C29B C30B 1.3900 . ? C30B C31B 1.3900 . ? C31B C32B 1.3900 . ? C11B C16B 1.377(2) . ? C11B C12B 1.382(3) . ? C12B C13B 1.388(3) . ? C13B C14B 1.377(3) . ? C14B C15B 1.358(3) . ? C15B C16B 1.387(3) . ? C17B C22B 1.389(3) . ? C17B C18B 1.395(3) . ? C18B C19B 1.386(3) . ? C19B C20B 1.379(3) . ? C20B C21B 1.372(3) . ? C21B C22B 1.383(3) . ? O1C C1C 1.4359(18) . ? O2C C4C 1.4321(18) . ? C1C C7C 1.473(2) . ? C1C C2C 1.534(2) . ? C1C C6C 1.536(2) . ? C2C C3C 1.527(2) . ? C3C C4C 1.541(2) . ? C4C C9C 1.483(2) . ? C4C C5C 1.533(2) . ? C5C C6C 1.525(2) . ? C7C C8C 1.198(2) . ? C8C C11C 1.442(2) . ? C9C C10C 1.198(2) . ? C10C C17C 1.440(2) . ? C11C C12C 1.382(2) . ? C11C C16C 1.390(2) . ? C12C C13C 1.384(2) . ? C13C C14C 1.378(3) . ? C14C C15C 1.379(3) . ? C15C C16C 1.383(2) . ? C17C C22C 1.391(2) . ? C17C C18C 1.395(2) . ? C18C C19C 1.387(3) . ? C19C C20C 1.376(3) . ? C20C C21C 1.381(2) . ? C21C C22C 1.382(2) . ? O1D C1D 1.4324(18) . ? O2D C4D 1.4356(18) . ? C1D C7D 1.482(2) . ? C1D C2D 1.523(2) . ? C1D C6D 1.534(2) . ? C2D C3D 1.527(2) . ? C3D C4D 1.535(2) . ? C4D C9D 1.482(2) . ? C4D C5D 1.530(2) . ? C5D C6D 1.528(2) . ? C7D C8D 1.196(2) . ? C8D C31D 1.3285 . ? C8D C11D 1.446(3) . ? C31D C36D 1.3899 . ? C31D C32D 1.3900 . ? C32D C33D 1.3900 . ? C33D C34D 1.3900 . ? C34D C35D 1.3900 . ? C35D C36D 1.3900 . ? C9D C10D 1.198(2) . ? C10D C17D 1.438(2) . ? C10D C37D 1.5025 . ? C37D C38D 1.3900 . ? C37D C42D 1.3900 . ? C38D C39D 1.3900 . ? C39D C40D 1.3900 . ? C40D C41D 1.3900 . ? C41D C42D 1.3900 . ? C11D C16D 1.391(3) . ? C11D C12D 1.396(4) . ? C12D C13D 1.384(2) . ? C13D C14D 1.384(3) . ? C14D C15D 1.395(3) . ? C15D C16D 1.388(3) . ? C17D C18D 1.385(3) . ? C17D C22D 1.402(3) . ? C18D C19D 1.382(3) . ? C19D C20D 1.376(3) . ? C20D C21D 1.383(3) . ? C21D C22D 1.386(3) . ? O1E C1E 1.4331(19) . ? O2E C4E 1.4325(18) . ? C1E C7E 1.479(2) . ? C1E C2E 1.530(2) . ? C1E C6E 1.532(2) . ? C2E C3E 1.526(2) . ? C3E C4E 1.530(2) . ? C4E C9E 1.481(2) . ? C4E C5E 1.536(2) . ? C5E C6E 1.527(2) . ? C7E C8E 1.199(2) . ? C8E C11E 1.438(2) . ? C9E C10E 1.194(2) . ? C10E C17E 1.442(2) . ? C10E C27E 1.4835 . ? C27E C32E 1.3900 . ? C27E C28E 1.3901 . ? C28E C29E 1.3900 . ? C29E C30E 1.3900 . ? C30E C31E 1.3900 . ? C31E C32E 1.3900 . ? C11E C16E 1.386(2) . ? C11E C12E 1.391(2) . ? C12E C13E 1.384(2) . ? C13E C14E 1.375(3) . ? C14E C15E 1.372(3) . ? C15E C16E 1.387(3) . ? C17E C18E 1.379(3) . ? C17E C22E 1.398(2) . ? C18E C19E 1.384(3) . ? C19E C20E 1.382(3) . ? C20E C21E 1.373(3) . ? C21E C22E 1.378(3) . ? O1F C1F 1.4358(18) . ? O2F C4F 1.4332(18) . ? C1F C7F 1.478(2) . ? C1F C2F 1.529(2) . ? C1F C6F 1.532(2) . ? C2F C3F 1.528(2) . ? C3F C4F 1.533(2) . ? C4F C9F 1.482(2) . ? C4F C5F 1.529(2) . ? C5F C6F 1.525(2) . ? C7F C8F 1.198(2) . ? C8F C11F 1.443(2) . ? C9F C10F 1.195(2) . ? C10F C17F 1.440(2) . ? C10F C27F 1.4518 . ? C27F C28F 1.3900 . ? C27F C32F 1.3900 . ? C28F C29F 1.3900 . ? C29F C30F 1.3900 . ? C30F C31F 1.3900 . ? C31F C32F 1.3900 . ? C11F C16F 1.390(2) . ? C11F C12F 1.393(2) . ? C12F C13F 1.380(3) . ? C13F C14F 1.374(3) . ? C14F C15F 1.380(3) . ? C15F C16F 1.383(2) . ? C17F C22F 1.386(2) . ? C17F C18F 1.409(2) . ? C18F C19F 1.384(3) . ? C19F C20F 1.380(3) . ? C20F C21F 1.383(3) . ? C21F C22F 1.386(3) . ? O1G C1G 1.4409(18) . ? C1G C7G 1.477(2) . ? C1G C3G 1.532(2) 2_757 ? C1G C2G 1.535(2) . ? C2G C3G 1.527(2) . ? C3G C1G 1.532(2) 2_757 ? C7G C8G 1.195(2) . ? C8G C11G 1.443(2) . ? C11G C16G 1.382(2) . ? C11G C12G 1.394(2) . ? C12G C13G 1.387(3) . ? C13G C14G 1.384(3) . ? C14G C15G 1.360(3) . ? C15G C16G 1.387(2) . ? O1H C1H 1.4376(18) . ? C1H C7H 1.472(2) . ? C1H C2H 1.532(2) . ? C1H C3H 1.541(2) 2_656 ? C2H C3H 1.527(2) . ? C3H C1H 1.541(2) 2_656 ? C7H C8H 1.191(2) . ? C8H C11H 1.434(2) . ? C8H C31H 1.6083 . ? C31H C36H 1.3900 . ? C31H C32H 1.3900 . ? C32H C33H 1.3900 . ? C33H C34H 1.3900 . ? C34H C35H 1.3900 . ? C35H C36H 1.3900 . ? C11H C16H 1.392(2) . ? C11H C12H 1.401(2) . ? C12H C13H 1.380(3) . ? C13H C14H 1.393(3) . ? C14H C15H 1.382(3) . ? C15H C16H 1.385(3) . ? O1I C1I 1.4364(18) . ? C1I C7I 1.475(2) . ? C1I C2I 1.534(2) . ? C1I C3I 1.540(2) 2_655 ? C2I C3I 1.531(2) . ? C3I C1I 1.540(2) 2_655 ? C7I C8I 1.198(2) . ? C8I C11I 1.440(2) . ? C11I C16I 1.389(2) . ? C11I C12I 1.395(2) . ? C12I C13I 1.384(2) . ? C13I C14I 1.381(2) . ? C14I C15I 1.381(2) . ? C15I C16I 1.384(2) . ? O1J C1J 1.4368(19) . ? C1J C7J 1.477(2) . ? C1J C3J 1.532(2) 2_756 ? C1J C2J 1.535(2) . ? C2J C3J 1.526(2) . ? C3J C1J 1.532(2) 2_756 ? C7J C8J 1.195(2) . ? C8J C11J 1.445(2) . ? C11J C12J 1.388(2) . ? C11J C16J 1.396(2) . ? C12J C13J 1.384(2) . ? C13J C14J 1.383(2) . ? C15J C14J 1.381(3) . ? C15J C16J 1.384(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A C1A C7A 105.98(13) . . ? O1A C1A C6A 110.17(14) . . ? C7A C1A C6A 112.03(15) . . ? O1A C1A C2A 109.76(14) . . ? C7A C1A C2A 108.77(14) . . ? C6A C1A C2A 110.03(13) . . ? C3A C2A C1A 111.54(14) . . ? C2A C3A C4A 111.70(13) . . ? O2A C4A C9A 109.09(13) . . ? O2A C4A C3A 110.40(12) . . ? C9A C4A C3A 110.95(14) . . ? O2A C4A C5A 106.30(13) . . ? C9A C4A C5A 110.16(13) . . ? C3A C4A C5A 109.84(13) . . ? C6A C5A C4A 112.14(14) . . ? C5A C6A C1A 112.30(13) . . ? C8A C7A C1A 174.92(19) . . ? C7A C8A C31A 173.41(12) . . ? C7A C8A C11A 174.5(2) . . ? C31A C8A C11A 12.06(11) . . ? C36A C31A C32A 120.0 . . ? C36A C31A C8A 113.9 . . ? C32A C31A C8A 125.6 . . ? C31A C32A C33A 120.0 . . ? C34A C33A C32A 120.0 . . ? C35A C34A C33A 120.0 . . ? C34A C35A C36A 120.0 . . ? C31A C36A C35A 120.0 . . ? C10A C9A C4A 178.08(18) . . ? C9A C10A C17A 179.39(19) . . ? C9A C10A C37A 156.48(11) . . ? C17A C10A C37A 23.47(11) . . ? C9A C10A C47A 168.43(11) . . ? C17A C10A C47A 11.88(11) . . ? C37A C10A C47A 15.3 . . ? C42A C37A C38A 120.0 . . ? C42A C37A C10A 108.4 . . ? C38A C37A C10A 131.6 . . ? C39A C38A C37A 120.0 . . ? C40A C39A C38A 120.0 . . ? C41A C40A C39A 120.0 . . ? C40A C41A C42A 120.0 . . ? C37A C42A C41A 120.0 . . ? C52A C47A C48A 120.0 . . ? C52A C47A C10A 123.6 . . ? C48A C47A C10A 116.4 . . ? C49A C48A C47A 120.0 . . ? C48A C49A C50A 120.0 . . ? C51A C50A C49A 120.0 . . ? C50A C51A C52A 120.0 . . ? C47A C52A C51A 120.0 . . ? C16A C11A C12A 119.11(18) . . ? C16A C11A C8A 119.78(18) . . ? C12A C11A C8A 121.10(18) . . ? C13A C12A C11A 119.6(2) . . ? C14A C13A C12A 121.0(2) . . ? C13A C14A C15A 119.23(18) . . ? C16A C15A C14A 120.59(19) . . ? C15A C16A C11A 120.43(18) . . ? C22A C17A C18A 119.40(18) . . ? C22A C17A C10A 120.99(18) . . ? C18A C17A C10A 119.55(19) . . ? C19A C18A C17A 120.0(2) . . ? C18A C19A C20A 120.3(2) . . ? C19A C20A C21A 119.7(2) . . ? C22A C21A C20A 120.2(2) . . ? C21A C22A C17A 120.3(2) . . ? O1B C1B C7B 109.21(13) . . ? O1B C1B C2B 106.49(12) . . ? C7B C1B C2B 110.42(13) . . ? O1B C1B C6B 109.70(12) . . ? C7B C1B C6B 111.83(13) . . ? C2B C1B C6B 109.05(13) . . ? C3B C2B C1B 111.47(13) . . ? C2B C3B C4B 112.00(13) . . ? O2B C4B C9B 109.53(13) . . ? O2B C4B C5B 105.83(12) . . ? C9B C4B C5B 110.81(13) . . ? O2B C4B C3B 109.95(12) . . ? C9B C4B C3B 111.22(13) . . ? C5B C4B C3B 109.36(13) . . ? C6B C5B C4B 112.03(13) . . ? C5B C6B C1B 112.06(13) . . ? C8B C7B C1B 177.19(18) . . ? C7B C8B C11B 177.70(19) . . ? C10B C9B C4B 178.23(19) . . ? C9B C10B C17B 177.3(2) . . ? C9B C10B C27B 157.73(12) . . ? C17B C10B C27B 19.60(12) . . ? C32B C27B C28B 120.0 . . ? C32B C27B C10B 124.2 . . ? C28B C27B C10B 114.0 . . ? C29B C28B C27B 120.0 . . ? C30B C29B C28B 120.0 . . ? C29B C30B C31B 120.0 . . ? C30B C31B C32B 120.0 . . ? C27B C32B C31B 120.0 . . ? C16B C11B C12B 118.51(18) . . ? C16B C11B C8B 120.79(17) . . ? C12B C11B C8B 120.65(17) . . ? C11B C12B C13B 120.5(2) . . ? C14B C13B C12B 120.4(2) . . ? C15B C14B C13B 119.0(2) . . ? C14B C15B C16B 121.16(19) . . ? C11B C16B C15B 120.38(19) . . ? C22B C17B C18B 119.14(18) . . ? C22B C17B C10B 120.50(18) . . ? C18B C17B C10B 120.17(18) . . ? C19B C18B C17B 119.82(19) . . ? C20B C19B C18B 120.44(19) . . ? C21B C20B C19B 119.85(19) . . ? C20B C21B C22B 120.5(2) . . ? C21B C22B C17B 120.3(2) . . ? O1C C1C C7C 109.96(13) . . ? O1C C1C C2C 106.36(12) . . ? C7C C1C C2C 110.19(13) . . ? O1C C1C C6C 110.15(12) . . ? C7C C1C C6C 110.37(13) . . ? C2C C1C C6C 109.72(13) . . ? C3C C2C C1C 112.20(13) . . ? C2C C3C C4C 111.89(13) . . ? O2C C4C C9C 109.89(13) . . ? O2C C4C C5C 106.31(12) . . ? C9C C4C C5C 111.05(13) . . ? O2C C4C C3C 110.30(12) . . ? C9C C4C C3C 109.82(13) . . ? C5C C4C C3C 109.42(13) . . ? C6C C5C C4C 111.97(12) . . ? C5C C6C C1C 111.68(13) . . ? C8C C7C C1C 179.54(18) . . ? C7C C8C C11C 176.91(18) . . ? C10C C9C C4C 178.81(17) . . ? C9C C10C C17C 177.46(19) . . ? C12C C11C C16C 119.00(16) . . ? C12C C11C C8C 121.67(15) . . ? C16C C11C C8C 119.32(16) . . ? C11C C12C C13C 120.45(17) . . ? C14C C13C C12C 120.31(18) . . ? C13C C14C C15C 119.65(17) . . ? C14C C15C C16C 120.26(18) . . ? C15C C16C C11C 120.31(18) . . ? C22C C17C C18C 118.76(15) . . ? C22C C17C C10C 121.17(15) . . ? C18C C17C C10C 120.04(16) . . ? C19C C18C C17C 120.43(17) . . ? C20C C19C C18C 120.26(18) . . ? C19C C20C C21C 119.62(17) . . ? C20C C21C C22C 120.73(16) . . ? C21C C22C C17C 120.20(16) . . ? O1D C1D C7D 109.62(13) . . ? O1D C1D C2D 110.30(13) . . ? C7D C1D C2D 111.68(14) . . ? O1D C1D C6D 105.98(12) . . ? C7D C1D C6D 108.90(13) . . ? C2D C1D C6D 110.20(13) . . ? C1D C2D C3D 112.17(13) . . ? C2D C3D C4D 111.18(13) . . ? O2D C4D C9D 106.67(13) . . ? O2D C4D C5D 110.13(13) . . ? C9D C4D C5D 111.01(14) . . ? O2D C4D C3D 109.72(13) . . ? C9D C4D C3D 109.35(13) . . ? C5D C4D C3D 109.91(13) . . ? C6D C5D C4D 111.87(13) . . ? C5D C6D C1D 111.87(13) . . ? C8D C7D C1D 175.28(18) . . ? C7D C8D C31D 169.27(12) . . ? C7D C8D C11D 173.6(2) . . ? C31D C8D C11D 17.09(14) . . ? C8D C31D C36D 115.9 . . ? C8D C31D C32D 123.7 . . ? C36D C31D C32D 120.0 . . ? C33D C32D C31D 120.0 . . ? C32D C33D C34D 120.0 . . ? C35D C34D C33D 120.0 . . ? C34D C35D C36D 120.0 . . ? C31D C36D C35D 120.0 . . ? C10D C9D C4D 175.86(18) . . ? C9D C10D C17D 178.02(19) . . ? C9D C10D C37D 165.27(12) . . ? C17D C10D C37D 12.79(10) . . ? C38D C37D C42D 120.0 . . ? C38D C37D C10D 113.9 . . ? C42D C37D C10D 126.1 . . ? C37D C38D C39D 120.0 . . ? C40D C39D C38D 120.0 . . ? C39D C40D C41D 120.0 . . ? C40D C41D C42D 120.0 . . ? C37D C42D C41D 120.0 . . ? C16D C11D C12D 119.41(18) . . ? C16D C11D C8D 121.6(3) . . ? C12D C11D C8D 119.0(2) . . ? C13D C12D C11D 120.21(17) . . ? C12D C13D C14D 120.37(18) . . ? C13D C14D C15D 119.74(18) . . ? C16D C15D C14D 119.97(18) . . ? C15D C16D C11D 120.3(2) . . ? C18D C17D C22D 118.88(19) . . ? C18D C17D C10D 122.13(19) . . ? C22D C17D C10D 118.92(17) . . ? C19D C18D C17D 120.2(3) . . ? C20D C19D C18D 121.0(2) . . ? C19D C20D C21D 119.41(19) . . ? C20D C21D C22D 120.29(19) . . ? C21D C22D C17D 120.16(18) . . ? O1E C1E C7E 106.07(13) . . ? O1E C1E C2E 109.71(13) . . ? C7E C1E C2E 109.75(13) . . ? O1E C1E C6E 110.35(13) . . ? C7E C1E C6E 111.17(14) . . ? C2E C1E C6E 109.74(13) . . ? C3E C2E C1E 111.50(13) . . ? C2E C3E C4E 112.31(13) . . ? O2E C4E C9E 108.55(12) . . ? O2E C4E C3E 109.76(12) . . ? C9E C4E C3E 111.94(13) . . ? O2E C4E C5E 106.15(12) . . ? C9E C4E C5E 110.33(13) . . ? C3E C4E C5E 109.93(13) . . ? C6E C5E C4E 111.47(13) . . ? C5E C6E C1E 112.23(13) . . ? C8E C7E C1E 178.1(2) . . ? C7E C8E C11E 176.92(19) . . ? C10E C9E C4E 174.63(18) . . ? C9E C10E C17E 175.85(19) . . ? C9E C10E C27E 172.78(11) . . ? C17E C10E C27E 6.42(10) . . ? C32E C27E C28E 120.0 . . ? C32E C27E C10E 122.7 . . ? C28E C27E C10E 117.2 . . ? C29E C28E C27E 120.0 . . ? C28E C29E C30E 120.0 . . ? C31E C30E C29E 120.0 . . ? C30E C31E C32E 120.0 . . ? C27E C32E C31E 120.0 . . ? C16E C11E C12E 118.55(16) . . ? C16E C11E C8E 120.04(16) . . ? C12E C11E C8E 121.38(16) . . ? C13E C12E C11E 120.16(17) . . ? C14E C13E C12E 120.78(18) . . ? C15E C14E C13E 119.48(17) . . ? C14E C15E C16E 120.34(19) . . ? C11E C16E C15E 120.66(18) . . ? C18E C17E C22E 118.54(18) . . ? C18E C17E C10E 121.22(17) . . ? C22E C17E C10E 120.14(17) . . ? C17E C18E C19E 120.93(19) . . ? C20E C19E C18E 119.6(2) . . ? C21E C20E C19E 120.3(2) . . ? C20E C21E C22E 120.00(19) . . ? C21E C22E C17E 120.61(19) . . ? O1F C1F C7F 106.26(13) . . ? O1F C1F C2F 110.14(13) . . ? C7F C1F C2F 110.92(14) . . ? O1F C1F C6F 109.61(13) . . ? C7F C1F C6F 109.92(14) . . ? C2F C1F C6F 109.93(13) . . ? C3F C2F C1F 112.04(13) . . ? C2F C3F C4F 111.47(13) . . ? O2F C4F C9F 109.47(13) . . ? O2F C4F C5F 109.53(12) . . ? C9F C4F C5F 111.50(13) . . ? O2F C4F C3F 106.33(12) . . ? C9F C4F C3F 109.85(13) . . ? C5F C4F C3F 110.03(13) . . ? C6F C5F C4F 112.14(13) . . ? C5F C6F C1F 111.04(13) . . ? C8F C7F C1F 176.99(18) . . ? C7F C8F C11F 176.58(19) . . ? C10F C9F C4F 176.38(18) . . ? C9F C10F C17F 174.63(19) . . ? C9F C10F C27F 170.21(11) . . ? C17F C10F C27F 13.70(10) . . ? C28F C27F C32F 120.0 . . ? C28F C27F C10F 113.6 . . ? C32F C27F C10F 124.2 . . ? C27F C28F C29F 120.0 . . ? C28F C29F C30F 120.0 . . ? C31F C30F C29F 120.0 . . ? C30F C31F C32F 120.0 . . ? C27F C32F C31F 120.0 . . ? C16F C11F C12F 118.46(16) . . ? C16F C11F C8F 121.46(16) . . ? C12F C11F C8F 120.05(16) . . ? C13F C12F C11F 120.68(18) . . ? C14F C13F C12F 120.41(19) . . ? C13F C14F C15F 119.49(18) . . ? C14F C15F C16F 120.62(17) . . ? C15F C16F C11F 120.29(16) . . ? C22F C17F C18F 119.22(17) . . ? C22F C17F C10F 119.83(17) . . ? C18F C17F C10F 120.95(17) . . ? C19F C18F C17F 119.75(18) . . ? C20F C19F C18F 120.53(19) . . ? C19F C20F C21F 119.78(19) . . ? C20F C21F C22F 120.5(2) . . ? C17F C22F C21F 120.16(18) . . ? O1G C1G C7G 109.19(13) . . ? O1G C1G C3G 106.31(12) . 2_757 ? C7G C1G C3G 110.75(13) . 2_757 ? O1G C1G C2G 109.56(12) . . ? C7G C1G C2G 111.55(13) . . ? C3G C1G C2G 109.35(13) 2_757 . ? C3G C2G C1G 111.98(13) . . ? C2G C3G C1G 111.59(13) . 2_757 ? C8G C7G C1G 177.94(18) . . ? C7G C8G C11G 176.59(19) . . ? C16G C11G C12G 118.79(16) . . ? C16G C11G C8G 120.56(16) . . ? C12G C11G C8G 120.64(16) . . ? C13G C12G C11G 119.85(18) . . ? C14G C13G C12G 120.35(19) . . ? C15G C14G C13G 119.79(18) . . ? C14G C15G C16G 120.46(18) . . ? C11G C16G C15G 120.61(17) . . ? O1H C1H C7H 110.20(13) . . ? O1H C1H C2H 105.88(12) . . ? C7H C1H C2H 110.32(14) . . ? O1H C1H C3H 109.86(12) . 2_656 ? C7H C1H C3H 111.07(13) . 2_656 ? C2H C1H C3H 109.38(13) . 2_656 ? C3H C2H C1H 111.42(13) . . ? C2H C3H C1H 111.59(13) . 2_656 ? C8H C7H C1H 178.32(19) . . ? C7H C8H C11H 177.95(19) . . ? C7H C8H C31H 163.49(12) . . ? C11H C8H C31H 17.49(9) . . ? C36H C31H C32H 120.0 . . ? C36H C31H C8H 119.8 . . ? C32H C31H C8H 117.1 . . ? C33H C32H C31H 120.0 . . ? C32H C33H C34H 120.0 . . ? C33H C34H C35H 120.0 . . ? C34H C35H C36H 120.0 . . ? C31H C36H C35H 120.0 . . ? C16H C11H C12H 119.25(17) . . ? C16H C11H C8H 121.49(16) . . ? C12H C11H C8H 119.26(16) . . ? C13H C12H C11H 119.90(18) . . ? C12H C13H C14H 120.58(18) . . ? C15H C14H C13H 119.54(18) . . ? C14H C15H C16H 120.40(19) . . ? C15H C16H C11H 120.31(17) . . ? O1I C1I C7I 109.95(13) . . ? O1I C1I C2I 106.42(12) . . ? C7I C1I C2I 110.52(13) . . ? O1I C1I C3I 110.22(12) . 2_655 ? C7I C1I C3I 110.12(13) . 2_655 ? C2I C1I C3I 109.55(13) . 2_655 ? C3I C2I C1I 111.89(13) . . ? C2I C3I C1I 112.06(13) . 2_655 ? C8I C7I C1I 179.41(17) . . ? C7I C8I C11I 177.43(18) . . ? C16I C11I C12I 119.18(15) . . ? C16I C11I C8I 121.07(15) . . ? C12I C11I C8I 119.74(15) . . ? C13I C12I C11I 120.34(16) . . ? C14I C13I C12I 120.08(17) . . ? C15I C14I C13I 119.85(17) . . ? C14I C15I C16I 120.55(17) . . ? C15I C16I C11I 120.00(16) . . ? O1J C1J C7J 109.92(14) . . ? O1J C1J C3J 106.15(12) . 2_756 ? C7J C1J C3J 111.04(13) . 2_756 ? O1J C1J C2J 110.08(13) . . ? C7J C1J C2J 109.91(13) . . ? C3J C1J C2J 109.67(14) 2_756 . ? C3J C2J C1J 111.32(13) . . ? C2J C3J C1J 111.76(13) . 2_756 ? C8J C7J C1J 178.40(18) . . ? C7J C8J C11J 177.88(18) . . ? C12J C11J C16J 118.70(16) . . ? C12J C11J C8J 121.23(15) . . ? C16J C11J C8J 120.05(16) . . ? C13J C12J C11J 120.41(16) . . ? C14J C13J C12J 120.46(17) . . ? C14J C15J C16J 120.07(18) . . ? C15J C14J C13J 119.71(17) . . ? C15J C16J C11J 120.65(17) . . ? 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 O1A H01A O2C 0.84 1.94 2.7462(16) 160.1 . O2A H02A O2B 0.84 1.93 2.7382(15) 160.8 . O1B H01B O1D 0.84 1.94 2.7508(15) 161.9 2_666 O2B H02B O2E 0.84 1.92 2.7326(15) 162.1 . O1C H01C O2D 0.84 1.91 2.7221(15) 161.3 2_666 O2C H02C O1E 0.84 1.92 2.7389(16) 163.7 1_655 O1D H01D O1G 0.84 1.90 2.7089(15) 161.9 . O2D H02D O1I 0.84 1.96 2.7683(15) 162.4 1_556 O1E H01E O1J 0.84 1.91 2.7293(16) 164.2 1_455 O2E H02E O1H 0.84 1.91 2.7281(15) 165.4 . O1F H01F O1C 0.84 1.94 2.7553(15) 163.4 2_666 O2F H02F O1B 0.84 1.91 2.7291(15) 165.9 2_566 O1G H01G O2F 0.84 1.92 2.7355(15) 163.7 1_655 O1H H01H O2A 0.84 1.93 2.7305(15) 159.2 . O1I H01I O1F 0.84 1.90 2.7140(16) 162.2 1_554 O1J H01J O1A 0.84 1.89 2.7138(16) 165.0 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.424 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.061 # Attachment '2-L.cif' data_poly2 _database_code_depnum_ccdc_archive 'CCDC 283831' _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans -1,4-bis(phenylethynyl) cyclohexane -1,4-diol ; _chemical_name_common 'trans -1,4-bis(phenylethynyl) cyclohexane -1,4-diol' _chemical_melting_point 182 _chemical_formula_moiety 'C22 H20 O2' _chemical_formula_sum 'C22 H20 O2' _chemical_formula_weight 316.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4940(3) _cell_length_b 14.0677(5) _cell_length_c 14.4606(5) _cell_angle_alpha 95.625(2) _cell_angle_beta 106.478(1) _cell_angle_gamma 104.627(2) _cell_volume 1761.8(1) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5997 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 26.02 _exptl_crystal_description Plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.193 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.0 _exptl_absorpt_correction_T_max 0.0 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20278 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _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 8067 _reflns_number_gt 5523 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. Phenyl substituent at C(8), i.e. atoms C(11) to C(16) with attached hydrogens, is disordered between 3 orientations with occupancies 0.5 (unprimed), 0.25 (primed) and 0.25 (double-primed). Ring C(17) to C(22) is disordered between 2 orientations with occupancies 0.55 (unprimed) and 0.45 (primed). The phenyl attached to C(10A) is disordered between 2 orientations: atomic positions C(11A) to C(16A) (occupancy 0.75) and C(11C) to C(16C) (occupancy 0.25). The phenyl attached to C(10B) is disordered between 2 orientations: atomic positions C(11B) to C(16B) (occupancy 0.4) and C(11D) to C(16D) (occupancy 0.6). Each phenyl ring was refined as a rigid body (ideal hexagon). The ADP of near-overlapping atoms belonging to different orientations, were constrained to equivalence. Hydroxy H atoms were refined in isotropic approximation (refall), other H atoms were treated as riding on teh corresponding C atoms (constr). ; _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^)+(0.0368P)^2^+1.1285P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8067 _refine_ls_number_parameters 444 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1012 _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.1401 _refine_ls_wR_factor_gt 0.1242 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.41816(15) 0.44201(10) 0.36272(10) 0.0283(3) Uani 1 1 d . . . H01 H 0.519(3) 0.4537(19) 0.4036(19) 0.060(8) Uiso 1 1 d . . . O2 O 0.06788(18) 0.06580(12) 0.13141(12) 0.0482(5) Uani 1 1 d . . . H02 H 0.131(3) 0.064(2) 0.101(2) 0.070(9) Uiso 1 1 d . . . C1 C 0.3680(2) 0.35307(13) 0.29012(13) 0.0227(4) Uani 1 1 d . . . C2 C 0.2039(2) 0.34479(15) 0.22768(14) 0.0273(4) Uani 1 1 d . . . H2A H 0.1412 0.3495 0.2712 0.035 Uiso 1 1 d R . . H2B H 0.2060 0.4014 0.1920 0.035 Uiso 1 1 d R . . C3 C 0.1293(2) 0.24718(16) 0.15425(14) 0.0329(5) Uani 1 1 d . . . H3A H 0.1851 0.2459 0.1060 0.043 Uiso 1 1 d R . . H3B H 0.0219 0.2435 0.1183 0.043 Uiso 1 1 d R . . C4 C 0.1300(2) 0.15624(15) 0.20385(14) 0.0318(5) Uani 1 1 d . . . C5 C 0.2947(2) 0.16411(14) 0.26564(15) 0.0306(4) Uani 1 1 d . . . H5A H 0.2931 0.1072 0.3009 0.040 Uiso 1 1 d R . . H5B H 0.3571 0.1601 0.2218 0.040 Uiso 1 1 d R . . C6 C 0.3684(2) 0.26190(14) 0.33969(13) 0.0254(4) Uani 1 1 d . . . H6A H 0.4757 0.2657 0.3762 0.033 Uiso 1 1 d R . . H6B H 0.3118 0.2627 0.3875 0.033 Uiso 1 1 d R . . C7 C 0.4698(2) 0.36333(14) 0.22821(14) 0.0269(4) Uani 1 1 d . A . C8 C 0.5485(2) 0.37585(15) 0.17647(14) 0.0304(4) Uani 1 1 d . . . C9 C 0.0314(2) 0.14716(15) 0.26771(15) 0.0325(5) Uani 1 1 d . B . C10 C -0.0420(2) 0.14106(15) 0.32302(15) 0.0322(5) Uani 1 1 d . . . C11 C 0.6260(3) 0.4029(2) 0.10472(19) 0.0239(12) Uiso 0.50 1 d PG A 1 C12 C 0.7429(3) 0.3612(2) 0.1017(2) 0.0333(9) Uani 0.50 1 d PG A 1 H12 H 0.7705 0.3183 0.1460 0.040 Uiso 0.50 1 d PR A 1 C13 C 0.8196(3) 0.3822(2) 0.0338(2) 0.0439(12) Uani 0.50 1 d PG A 1 H13 H 0.8995 0.3536 0.0317 0.053 Uiso 0.50 1 d PR A 1 C14 C 0.7792(4) 0.4449(2) -0.0310(2) 0.0387(12) Uani 0.50 1 d PG A 1 H14 H 0.8316 0.4592 -0.0773 0.046 Uiso 0.50 1 d PR A 1 C15 C 0.6622(4) 0.4866(2) -0.02793(19) 0.0406(10) Uani 0.50 1 d PG A 1 H15 H 0.6346 0.5295 -0.0722 0.049 Uiso 0.50 1 d PR A 1 C16 C 0.5856(3) 0.4656(2) 0.0399(2) 0.0337(9) Uani 0.50 1 d PG A 1 H16 H 0.5056 0.4941 0.0420 0.040 Uiso 0.50 1 d PR A 1 C11' C 0.6482(5) 0.3782(5) 0.1216(4) 0.0223(19) Uiso 0.25 1 d PG A 2 C12' C 0.5837(5) 0.3389(4) 0.0219(4) 0.0233(18) Uiso 0.25 1 d PG A 2 H12' H 0.4768 0.3053 -0.0051 0.028 Uiso 0.25 1 d PR A 2 C13' C 0.6755(6) 0.3488(5) -0.0384(3) 0.034(2) Uiso 0.25 1 d PG A 2 H13' H 0.6313 0.3219 -0.1066 0.041 Uiso 0.25 1 d PR A 2 C14' C 0.8319(6) 0.3980(5) 0.0011(4) 0.029(2) Uiso 0.25 1 d PG A 2 H14' H 0.8946 0.4047 -0.0401 0.035 Uiso 0.25 1 d PR A 2 C15' C 0.8965(4) 0.4373(5) 0.1008(4) 0.040(2) Uiso 0.25 1 d PG A 2 H15' H 1.0034 0.4709 0.1278 0.048 Uiso 0.25 1 d PR A 2 C16' C 0.8046(6) 0.4274(5) 0.1610(3) 0.0339(18) Uiso 0.25 1 d PG A 2 H16' H 0.8488 0.4543 0.2292 0.041 Uiso 0.25 1 d PR A 2 C11" C 0.6559(7) 0.4021(4) 0.1155(4) 0.026(3) Uiso 0.25 1 d PG A 3 C12" C 0.6283(7) 0.3382(3) 0.0285(4) 0.0262(18) Uiso 0.25 1 d PG A 3 H12" H 0.5504 0.2759 0.0111 0.031 Uiso 0.25 1 d PR A 3 C13" C 0.7148(8) 0.3655(4) -0.0329(4) 0.031(2) Uiso 0.25 1 d PG A 3 H13" H 0.6959 0.3218 -0.0924 0.037 Uiso 0.25 1 d PR A 3 C14" C 0.8288(7) 0.4566(5) -0.0074(4) 0.037(3) Uiso 0.25 1 d PG A 3 H14" H 0.8879 0.4752 -0.0494 0.044 Uiso 0.25 1 d PR A 3 C15" C 0.8564(6) 0.5205(4) 0.0796(4) 0.046(3) Uani 0.25 1 d PG A 3 H15" H 0.9343 0.5828 0.0971 0.055 Uiso 0.25 1 d PR A 3 C16" C 0.7699(7) 0.4933(4) 0.1411(4) 0.038(2) Uani 0.25 1 d PG A 3 H16" H 0.7887 0.5370 0.2005 0.046 Uiso 0.25 1 d PR A 3 C17 C -0.1300(8) 0.1354(4) 0.3893(3) 0.0264(7) Uani 0.55 1 d PG B 1 C18 C -0.0588(5) 0.1318(3) 0.4866(3) 0.0422(13) Uani 0.55 1 d PG B 1 H18 H 0.0486 0.1403 0.5098 0.051 Uiso 0.55 1 d PR B 1 C19 C -0.1447(5) 0.1160(3) 0.5502(3) 0.0468(13) Uani 0.55 1 d PG B 1 H19 H -0.0960 0.1135 0.6167 0.056 Uiso 0.55 1 d PR B 1 C20 C -0.3017(5) 0.1037(4) 0.5163(4) 0.0374(12) Uani 0.55 1 d PG B 1 H20 H -0.3604 0.0929 0.5598 0.045 Uiso 0.55 1 d PR B 1 C21 C -0.3729(5) 0.1073(5) 0.4190(4) 0.0304(13) Uani 0.55 1 d PG B 1 H21 H -0.4802 0.0989 0.3959 0.036 Uiso 0.55 1 d PR B 1 C22 C -0.2870(8) 0.1231(5) 0.3555(3) 0.0278(11) Uani 0.55 1 d PG B 1 H22 H -0.3357 0.1256 0.2889 0.033 Uiso 0.55 1 d PR B 1 C17' C -0.1243(10) 0.1201(5) 0.3952(4) 0.0264(7) Uani 0.45 1 d PG B 2 C18' C -0.0621(6) 0.0828(4) 0.4779(4) 0.0422(13) Uani 0.45 1 d PG B 2 H18' H 0.0334 0.0688 0.4878 0.051 Uiso 0.45 1 d PR B 2 C19' C -0.1396(7) 0.0659(4) 0.5459(4) 0.0468(13) Uani 0.45 1 d PG B 2 H19' H -0.0970 0.0404 0.6024 0.056 Uiso 0.45 1 d PR B 2 C20' C -0.2793(7) 0.0863(5) 0.5312(5) 0.0374(12) Uani 0.45 1 d PG B 2 H20' H -0.3323 0.0747 0.5776 0.045 Uiso 0.45 1 d PR B 2 C21' C -0.3416(7) 0.1236(6) 0.4485(6) 0.0304(13) Uani 0.45 1 d PG B 2 H21' H -0.4371 0.1375 0.4385 0.036 Uiso 0.45 1 d PR B 2 C22' C -0.2641(10) 0.1405(6) 0.3805(4) 0.0278(11) Uani 0.45 1 d PG B 2 H22' H -0.3066 0.1660 0.3240 0.033 Uiso 0.45 1 d PR B 2 O1A O 0.21548(17) 0.02187(11) 0.00215(11) 0.0339(3) Uani 1 1 d . . . H01A H 0.131(3) -0.0097(18) -0.0512(18) 0.046(7) Uiso 1 1 d . . . C1A C 0.3521(2) 0.02618(14) -0.02370(14) 0.0272(4) Uani 1 1 d . . . C2A C 0.4881(2) 0.07889(14) 0.06934(13) 0.0282(4) Uani 1 1 d . . . H2A1 H 0.4871 0.1484 0.0871 0.037 Uiso 1 1 d R . . H2A2 H 0.4766 0.0441 0.1243 0.037 Uiso 1 1 d R . . C6A C 0.3581(2) -0.07990(14) -0.05486(14) 0.0283(4) Uani 1 1 d . . . H6A1 H 0.3422 -0.1199 -0.0041 0.037 Uiso 1 1 d R . . H6A2 H 0.2739 -0.1122 -0.1169 0.037 Uiso 1 1 d R . . C9A C 0.3546(2) 0.08317(14) -0.10431(14) 0.0293(4) Uani 1 1 d . C . C10A C 0.3567(2) 0.12819(15) -0.17003(15) 0.0313(4) Uani 1 1 d . . . C11A C 0.3619(6) 0.1884(3) -0.2495(3) 0.0286(5) Uani 0.75 1 d PG C 2 C12A C 0.3766(7) 0.2899(3) -0.23168(18) 0.0513(12) Uani 0.75 1 d PG C 2 H12A H 0.3793 0.3210 -0.1696 0.062 Uiso 0.75 1 d PR C 2 C13A C 0.3872(6) 0.3459(3) -0.3048(2) 0.0547(12) Uani 0.75 1 d PG C 2 H13A H 0.3972 0.4153 -0.2926 0.066 Uiso 0.75 1 d PR C 2 C14A C 0.3832(5) 0.3004(3) -0.39564(19) 0.0364(8) Uani 0.75 1 d PG C 2 H14A H 0.3904 0.3387 -0.4456 0.044 Uiso 0.75 1 d PR C 2 C15A C 0.3685(3) 0.1989(3) -0.4134(2) 0.0285(7) Uani 0.75 1 d PG C 2 H15A H 0.3658 0.1678 -0.4755 0.034 Uiso 0.75 1 d PR C 2 C16A C 0.3579(4) 0.1429(2) -0.3404(3) 0.0253(7) Uani 0.75 1 d PG C 2 H16A H 0.3479 0.0735 -0.3525 0.030 Uiso 0.75 1 d PR C 2 C11C C 0.3612(19) 0.1814(11) -0.2393(10) 0.0286(5) Uani 0.25 1 d PG C 1 C12C C 0.411(2) 0.2843(12) -0.2073(7) 0.0513(12) Uani 0.25 1 d PG C 1 H12C H 0.4393 0.3112 -0.1396 0.062 Uiso 0.25 1 d PR C 1 C13C C 0.421(2) 0.3480(9) -0.2745(9) 0.0547(12) Uani 0.25 1 d PG C 1 H13C H 0.4552 0.4183 -0.2526 0.066 Uiso 0.25 1 d PR C 1 C14C C 0.3801(17) 0.3087(9) -0.3736(8) 0.0364(8) Uani 0.25 1 d PG C 1 H14C H 0.3866 0.3522 -0.4195 0.044 Uiso 0.25 1 d PR C 1 C15C C 0.3299(12) 0.2058(9) -0.4056(7) 0.0285(7) Uani 0.25 1 d PG C 1 H15C H 0.3020 0.1789 -0.4733 0.034 Uiso 0.25 1 d PR C 1 C16C C 0.3204(13) 0.1421(8) -0.3384(11) 0.0253(7) Uani 0.25 1 d PG C 1 H16C H 0.2861 0.0718 -0.3602 0.030 Uiso 0.25 1 d PR C 1 O1B O 0.29626(14) 0.50080(10) 0.50116(10) 0.0280(3) Uani 1 1 d . . . H01B H 0.320(3) 0.4827(18) 0.4464(18) 0.052(7) Uiso 1 1 d . . . C1B C 0.1466(2) 0.51600(14) 0.47573(14) 0.0245(4) Uani 1 1 d . . . C2B C 0.1383(2) 0.57336(14) 0.56854(15) 0.0295(4) Uani 1 1 d . . . H2B1 H 0.1649 0.5373 0.6234 0.038 Uiso 1 1 d R . . H2B2 H 0.2147 0.6403 0.5861 0.038 Uiso 1 1 d R . . C6B C 0.0217(2) 0.41466(14) 0.44526(15) 0.0276(4) Uani 1 1 d . . . H6B1 H 0.0230 0.3791 0.3831 0.036 Uiso 1 1 d R . . H6B2 H 0.0445 0.3735 0.4961 0.036 Uiso 1 1 d R . . C9B C 0.1297(2) 0.57504(16) 0.39633(16) 0.0329(5) Uani 1 1 d . D . C10B C 0.1185(2) 0.62502(18) 0.33401(19) 0.0427(6) Uani 1 1 d . . . C11B C 0.1197(4) 0.7047(3) 0.2802(3) 0.0263(11) Uiso 0.40 1 d PG D 1 C12B C 0.2424(3) 0.7359(3) 0.2449(3) 0.0312(14) Uiso 0.40 1 d PG D 1 H12B H 0.3290 0.7116 0.2651 0.037 Uiso 0.40 1 d PR D 1 C13B C 0.2385(4) 0.8027(3) 0.1802(3) 0.0382(15) Uiso 0.40 1 d PG D 1 H13B H 0.3224 0.8240 0.1561 0.046 Uiso 0.40 1 d PR D 1 C14B C 0.1119(4) 0.8383(3) 0.1506(3) 0.0361(13) Uiso 0.40 1 d PG D 1 H14B H 0.1092 0.8839 0.1064 0.043 Uiso 0.40 1 d PR D 1 C15B C -0.0108(4) 0.8071(4) 0.1859(3) 0.066(2) Uani 0.40 1 d PG D 1 H15B H -0.0973 0.8314 0.1657 0.080 Uiso 0.40 1 d PR D 1 C16B C -0.0069(4) 0.7403(4) 0.2507(3) 0.061(2) Uani 0.40 1 d PG D 1 H16B H -0.0907 0.7190 0.2748 0.073 Uiso 0.40 1 d PR D 1 C11D C 0.0996(3) 0.68029(18) 0.25003(18) 0.0288(8) Uiso 0.60 1 d PG D 2 C12D C 0.2270(2) 0.7562(2) 0.25156(17) 0.0340(10) Uiso 0.60 1 d PG D 2 H12D H 0.3245 0.7638 0.2980 0.041 Uiso 0.60 1 d PR D 2 C13D C 0.2117(2) 0.82099(17) 0.18519(19) 0.0362(9) Uiso 0.60 1 d PG D 2 H13D H 0.2988 0.8729 0.1862 0.043 Uiso 0.60 1 d PR D 2 C14D C 0.0690(3) 0.80984(19) 0.11729(18) 0.0376(9) Uiso 0.60 1 d PG D 2 H14D H 0.0586 0.8541 0.0719 0.045 Uiso 0.60 1 d PR D 2 C15D C -0.0584(2) 0.7339(2) 0.1158(2) 0.0704(16) Uani 0.60 1 d PG D 2 H15D H -0.1559 0.7263 0.0693 0.084 Uiso 0.60 1 d PR D 2 C16D C -0.0431(2) 0.6691(2) 0.1821(2) 0.0600(14) Uani 0.60 1 d PG D 2 H16D H -0.1302 0.6172 0.1811 0.072 Uiso 0.60 1 d PR D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0216(7) 0.0237(7) 0.0357(8) -0.0044(6) 0.0085(6) 0.0043(5) O2 0.0350(9) 0.0460(10) 0.0496(10) -0.0253(8) 0.0270(8) -0.0143(7) C1 0.0203(9) 0.0221(9) 0.0227(9) 0.0008(7) 0.0070(7) 0.0024(7) C2 0.0221(9) 0.0334(11) 0.0269(10) 0.0095(8) 0.0098(8) 0.0055(8) C3 0.0202(9) 0.0508(13) 0.0208(9) 0.0005(9) 0.0070(8) 0.0004(9) C4 0.0273(10) 0.0315(11) 0.0292(10) -0.0091(8) 0.0151(8) -0.0057(8) C5 0.0333(11) 0.0240(10) 0.0351(11) 0.0011(8) 0.0170(9) 0.0043(8) C6 0.0250(9) 0.0260(10) 0.0233(9) 0.0027(8) 0.0074(7) 0.0056(8) C7 0.0238(9) 0.0252(10) 0.0288(10) 0.0034(8) 0.0072(8) 0.0041(8) C8 0.0252(10) 0.0280(11) 0.0319(11) -0.0033(8) 0.0095(8) 0.0003(8) C9 0.0295(10) 0.0285(11) 0.0326(11) -0.0050(9) 0.0132(9) -0.0031(8) C10 0.0292(10) 0.0282(11) 0.0333(11) -0.0045(9) 0.0129(9) -0.0013(8) C12 0.036(2) 0.031(2) 0.045(2) 0.0217(19) 0.022(2) 0.0146(18) C13 0.049(3) 0.049(3) 0.058(3) 0.027(3) 0.038(3) 0.027(2) C14 0.051(3) 0.047(3) 0.028(2) 0.011(2) 0.026(3) 0.014(3) C15 0.055(3) 0.040(3) 0.031(2) 0.014(2) 0.014(2) 0.018(2) C16 0.039(2) 0.035(2) 0.031(2) 0.0052(18) 0.0110(18) 0.0179(19) C15" 0.040(5) 0.048(6) 0.038(5) -0.010(4) 0.028(4) -0.020(4) C16" 0.035(4) 0.036(5) 0.036(5) -0.009(4) 0.023(4) -0.009(4) C17 0.0245(11) 0.0212(17) 0.0314(11) -0.0009(10) 0.0138(9) -0.0003(11) C18 0.0233(12) 0.070(4) 0.0318(16) 0.002(3) 0.0088(11) 0.013(2) C19 0.0413(16) 0.074(4) 0.0303(14) 0.011(3) 0.0148(12) 0.021(3) C20 0.0367(18) 0.042(2) 0.040(2) 0.0058(16) 0.0245(17) 0.0094(15) C21 0.028(2) 0.027(2) 0.042(4) 0.004(3) 0.017(2) 0.010(2) C22 0.034(2) 0.023(3) 0.029(2) 0.004(2) 0.012(2) 0.009(2) C17' 0.0245(11) 0.0212(17) 0.0314(11) -0.0009(10) 0.0138(9) -0.0003(11) C18' 0.0233(12) 0.070(4) 0.0318(16) 0.002(3) 0.0088(11) 0.013(2) C19' 0.0413(16) 0.074(4) 0.0303(14) 0.011(3) 0.0148(12) 0.021(3) C20' 0.0367(18) 0.042(2) 0.040(2) 0.0058(16) 0.0245(17) 0.0094(15) C21' 0.028(2) 0.027(2) 0.042(4) 0.004(3) 0.017(2) 0.010(2) C22' 0.034(2) 0.023(3) 0.029(2) 0.004(2) 0.012(2) 0.009(2) O1A 0.0327(8) 0.0372(8) 0.0295(8) -0.0027(6) 0.0190(7) -0.0006(6) C1A 0.0316(10) 0.0266(10) 0.0253(9) 0.0021(8) 0.0192(8) 0.0013(8) C2A 0.0369(11) 0.0231(10) 0.0238(9) -0.0001(8) 0.0174(8) 0.0004(8) C6A 0.0345(10) 0.0234(10) 0.0240(9) 0.0011(8) 0.0153(8) -0.0019(8) C9A 0.0315(10) 0.0252(10) 0.0298(10) -0.0014(8) 0.0167(9) 0.0007(8) C10A 0.0344(11) 0.0258(10) 0.0335(11) 0.0014(9) 0.0178(9) 0.0024(8) C11A 0.0356(11) 0.0226(12) 0.0347(14) 0.0120(9) 0.0208(11) 0.0072(9) C12A 0.103(4) 0.0264(14) 0.043(2) 0.0131(18) 0.047(3) 0.0209(18) C13A 0.107(4) 0.0263(13) 0.053(3) 0.0178(17) 0.052(3) 0.0249(17) C14A 0.0548(15) 0.0306(14) 0.032(2) 0.0157(15) 0.0228(15) 0.0133(11) C15A 0.034(2) 0.0289(13) 0.0243(12) 0.0047(10) 0.0118(12) 0.0092(14) C16A 0.021(2) 0.0212(10) 0.0310(11) 0.0052(8) 0.0088(14) 0.0021(12) C11C 0.0356(11) 0.0226(12) 0.0347(14) 0.0120(9) 0.0208(11) 0.0072(9) C12C 0.103(4) 0.0264(14) 0.043(2) 0.0131(18) 0.047(3) 0.0209(18) C13C 0.107(4) 0.0263(13) 0.053(3) 0.0178(17) 0.052(3) 0.0249(17) C14C 0.0548(15) 0.0306(14) 0.032(2) 0.0157(15) 0.0228(15) 0.0133(11) C15C 0.034(2) 0.0289(13) 0.0243(12) 0.0047(10) 0.0118(12) 0.0092(14) C16C 0.021(2) 0.0212(10) 0.0310(11) 0.0052(8) 0.0088(14) 0.0021(12) O1B 0.0202(7) 0.0332(8) 0.0333(8) 0.0070(6) 0.0095(6) 0.0114(6) C1B 0.0165(8) 0.0227(9) 0.0360(10) 0.0061(8) 0.0094(8) 0.0071(7) C2B 0.0200(9) 0.0249(10) 0.0395(11) -0.0003(9) 0.0084(8) 0.0033(8) C6B 0.0233(9) 0.0205(9) 0.0389(11) 0.0017(8) 0.0110(8) 0.0066(8) C9B 0.0207(9) 0.0337(11) 0.0485(13) 0.0127(10) 0.0146(9) 0.0093(8) C10B 0.0246(10) 0.0491(14) 0.0653(16) 0.0314(13) 0.0201(10) 0.0155(10) C15B 0.038(4) 0.111(7) 0.078(5) 0.068(5) 0.026(4) 0.042(4) C16B 0.033(3) 0.105(6) 0.070(5) 0.062(5) 0.032(3) 0.029(4) C15D 0.036(2) 0.094(4) 0.077(3) 0.062(3) 0.004(2) 0.010(2) C16D 0.028(2) 0.076(3) 0.068(3) 0.049(3) 0.003(2) 0.002(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 1.433(2) . ? O2 C4 1.440(2) . ? C1 C7 1.484(2) . ? C1 C6 1.530(3) . ? C1 C2 1.531(2) . ? C2 C3 1.520(3) . ? C3 C4 1.527(3) . ? C4 C9 1.483(3) . ? C4 C5 1.534(3) . ? C5 C6 1.526(3) . ? C7 C8 1.194(3) . ? C8 C11' 1.394(4) . ? C8 C11 1.460(3) . ? C8 C11" 1.528(4) . ? C9 C10 1.196(3) . ? C10 C17 1.434(5) . ? C10 C17' 1.482(6) . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3902 . ? C13 C14 1.3899 . ? C14 C15 1.3899 . ? C15 C16 1.3900 . ? C11' C16' 1.3899 . ? C11' C12' 1.3901 . ? C12' C13' 1.3899 . ? C13' C14' 1.3900 . ? C14' C15' 1.3900 . ? C15' C16' 1.3900 . ? C11" C16" 1.3899 . ? C11" C12" 1.3900 . ? C12" C13" 1.3899 . ? C13" C14" 1.3899 . ? C14" C15" 1.3901 . ? C15" C16" 1.3900 . ? C17 C18 1.3900 . ? C17 C22 1.3901 . ? C18 C19 1.3900 . ? C19 C20 1.3900 . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C17' C22' 1.3900 . ? C17' C18' 1.3900 . ? C18' C19' 1.3899 . ? C19' C20' 1.3901 . ? C20' C21' 1.3899 . ? C21' C22' 1.3901 . ? O1A C1A 1.438(2) . ? C1A C9A 1.480(3) . ? C1A C6A 1.536(3) . ? C1A C2A 1.537(3) . ? C2A C6A 1.529(3) 2_655 ? C6A C2A 1.530(3) 2_655 ? C9A C10A 1.194(3) . ? C10A C11C 1.312(10) . ? C10A C11A 1.497(3) . ? C11A C12A 1.3900 . ? C11A C16A 1.3900 . ? C12A C13A 1.3900 . ? C13A C14A 1.3900 . ? C14A C15A 1.3900 . ? C15A C16A 1.3900 . ? C11C C12C 1.3900 . ? C11C C16C 1.3900 . ? C12C C13C 1.3900 . ? C13C C14C 1.3900 . ? C14C C15C 1.3900 . ? C15C C16C 1.3900 . ? O1B C1B 1.439(2) . ? C1B C9B 1.478(3) . ? C1B C2B 1.529(3) . ? C1B C6B 1.536(2) . ? C2B C6B 1.529(2) 2_566 ? C6B C2B 1.529(2) 2_566 ? C9B C10B 1.194(3) . ? C10B C11B 1.426(3) . ? C10B C11D 1.498(3) . ? C11B C12B 1.3901 . ? C11B C16B 1.3902 . ? C12B C13B 1.3898 . ? C13B C14B 1.3901 . ? C14B C15B 1.3898 . ? C15B C16B 1.3900 . ? C11D C16D 1.3899 . ? C11D C12D 1.3900 . ? C12D C13D 1.3899 . ? C13D C14D 1.3899 . ? C14D C15D 1.3901 . ? C15D C16D 1.3899 . ? 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 109.05(14) . . ? O1 C1 C6 110.05(14) . . ? C7 C1 C6 111.41(15) . . ? O1 C1 C2 106.43(14) . . ? C7 C1 C2 109.92(15) . . ? C6 C1 C2 109.85(15) . . ? C3 C2 C1 112.13(16) . . ? C2 C3 C4 112.09(15) . . ? O2 C4 C9 106.14(15) . . ? O2 C4 C3 110.33(17) . . ? C9 C4 C3 111.51(17) . . ? O2 C4 C5 109.67(17) . . ? C9 C4 C5 109.17(17) . . ? C3 C4 C5 109.93(15) . . ? C6 C5 C4 111.46(16) . . ? C5 C6 C1 112.00(15) . . ? C8 C7 C1 176.3(2) . . ? C7 C8 C11' 171.0(3) . . ? C7 C8 C11 168.8(2) . . ? C11' C8 C11 20.0(3) . . ? C7 C8 C11" 174.5(3) . . ? C11' C8 C11" 12.8(4) . . ? C11 C8 C11" 10.7(3) . . ? C10 C9 C4 176.9(2) . . ? C9 C10 C17 179.1(3) . . ? C9 C10 C17' 171.2(3) . . ? C17 C10 C17' 9.7(5) . . ? C12 C11 C16 120.0 . . ? C12 C11 C8 116.93(19) . . ? C16 C11 C8 123.06(19) . . ? C11 C12 C13 120.0 . . ? C14 C13 C12 120.0 . . ? C13 C14 C15 120.0 . . ? C14 C15 C16 120.0 . . ? C15 C16 C11 120.0 . . ? C16' C11' C12' 120.0 . . ? C16' C11' C8 122.2(3) . . ? C12' C11' C8 117.5(3) . . ? C13' C12' C11' 120.0 . . ? C12' C13' C14' 120.0 . . ? C15' C14' C13' 120.0 . . ? C14' C15' C16' 120.0 . . ? C11' C16' C15' 120.0 . . ? C16" C11" C12" 120.0 . . ? C16" C11" C8 120.6(3) . . ? C12" C11" C8 119.0(3) . . ? C13" C12" C11" 120.0 . . ? C12" C13" C14" 120.0 . . ? C13" C14" C15" 120.0 . . ? C16" C15" C14" 120.0 . . ? C11" C16" C15" 120.0 . . ? C18 C17 C22 120.0 . . ? C18 C17 C10 118.7(4) . . ? C22 C17 C10 121.0(4) . . ? C19 C18 C17 120.0 . . ? C20 C19 C18 120.0 . . ? C19 C20 C21 120.0 . . ? C20 C21 C22 120.0 . . ? C21 C22 C17 120.0 . . ? C22' C17' C18' 120.0 . . ? C22' C17' C10 119.0(5) . . ? C18' C17' C10 121.0(5) . . ? C19' C18' C17' 120.0 . . ? C18' C19' C20' 120.0 . . ? C21' C20' C19' 120.0 . . ? C20' C21' C22' 120.0 . . ? C17' C22' C21' 120.0 . . ? O1A C1A C9A 109.77(16) . . ? O1A C1A C6A 110.11(14) . . ? C9A C1A C6A 110.21(15) . . ? O1A C1A C2A 106.17(14) . . ? C9A C1A C2A 110.92(15) . . ? C6A C1A C2A 109.58(17) . . ? C6A C2A C1A 111.69(14) 2_655 . ? C2A C6A C1A 111.63(15) 2_655 . ? C10A C9A C1A 179.2(2) . . ? C9A C10A C11C 177.4(7) . . ? C9A C10A C11A 177.7(3) . . ? C11C C10A C11A 0.4(8) . . ? C12A C11A C16A 120.0 . . ? C12A C11A C10A 120.4(3) . . ? C16A C11A C10A 119.5(3) . . ? C11A C12A C13A 120.0 . . ? C12A C13A C14A 120.0 . . ? C15A C14A C13A 120.0 . . ? C14A C15A C16A 120.0 . . ? C15A C16A C11A 120.0 . . ? C10A C11C C12C 115.1(11) . . ? C10A C11C C16C 124.9(11) . . ? C12C C11C C16C 120.0 . . ? C13C C12C C11C 120.0 . . ? C12C C13C C14C 120.0 . . ? C15C C14C C13C 120.0 . . ? C16C C15C C14C 120.0 . . ? C15C C16C C11C 120.0 . . ? O1B C1B C9B 109.46(15) . . ? O1B C1B C2B 106.32(15) . . ? C9B C1B C2B 110.52(16) . . ? O1B C1B C6B 109.87(14) . . ? C9B C1B C6B 111.39(16) . . ? C2B C1B C6B 109.15(15) . . ? C6B C2B C1B 111.79(15) 2_566 . ? C2B C6B C1B 111.88(15) 2_566 . ? C10B C9B C1B 178.2(2) . . ? C9B C10B C11B 165.6(3) . . ? C9B C10B C11D 175.5(3) . . ? C11B C10B C11D 18.89(19) . . ? C12B C11B C16B 120.0 . . ? C12B C11B C10B 117.7(2) . . ? C16B C11B C10B 121.6(2) . . ? C13B C12B C11B 120.0 . . ? C12B C13B C14B 120.0 . . ? C15B C14B C13B 120.0 . . ? C14B C15B C16B 120.0 . . ? C15B C16B C11B 120.0 . . ? C16D C11D C12D 120.0 . . ? C16D C11D C10B 122.28(17) . . ? C12D C11D C10B 116.87(17) . . ? C13D C12D C11D 120.0 . . ? C12D C13D C14D 120.0 . . ? C13D C14D C15D 120.0 . . ? C16D C15D C14D 120.0 . . ? C15D C16D C11D 120.0 . . ? 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 H01 O1B 0.94(3) 1.81(3) 2.7264(19) 166(2) 2_666 O2 H02 O1A 0.85(3) 1.93(3) 2.745(2) 160(3) . O1A H01A O2 0.92(2) 1.83(3) 2.720(2) 163(2) 2 O1B H01B O1 0.91(3) 1.85(3) 2.7394(19) 163(2) . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.289 _refine_diff_density_min -0.277 _refine_diff_density_rms 0.043 # Attachment '2-H_neutron.cif' data_chph20 _database_code_depnum_ccdc_archive 'CCDC 283832' _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans -1,4-bis(phenylethynyl) cyclohexane -1,4-diol ; _chemical_name_common 'trans -1,4-bis(phenylethynyl) cyclohexane -1,4-diol' _chemical_melting_point 182 _chemical_formula_moiety 'C22 H20 O2' _chemical_formula_sum 'C22 H20 O2' _chemical_formula_weight 316.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0000 0.0000 '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 0.0000 0.0000 '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 17.6377(8) _cell_length_b 18.8315(9) _cell_length_c 23.3591(11) _cell_angle_alpha 78.402(2) _cell_angle_beta 88.367(2) _cell_angle_gamma 67.611(2) _cell_volume 7017.4(6) _cell_formula_units_Z 16 _cell_measurement_temperature 20(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 1.20 _exptl_crystal_size_mid 0.85 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.196 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2688 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.715 _exptl_absorpt_correction_T_max 0.966 _exptl_absorpt_process_details 'calculated wavelength-dependent absorption coefficient' _exptl_special_details ; A rectangular crystal of dimensions 1.2 mm x 0.85 mm x 0.2 mm was wrapped in thin Al foil and glued to a standard sample pin with all face edges at large angles to the rotation axis. The crystal was cooled to 20 K, and data were collected on the Very-Intense Vertical-Axis Laue Diffractometer (VIVALDI) at the Institut Laue-Langevin [1]. 14 Laue diffraction patterns, each accumulated over 6 h, were at mostly 20\% intervals in a rotation of the crystal about the vertical axis perpendicular to the incident neutron beam. For a triclinic crystal, rotation about a single axis leads to a lack of small d data close to that axis. The crystal was therefore remounted to put this axis in the equatorial plane and a further six Laue patterns were collected at 30\% intervals about the vertical axis. A total of 51904 single, resolved reflections were recorded i n the wavelength range 0.9 -- 3.5 \%A, of which 13238 were independent, corresponding to 66 % of the complete unique set to d = 0.90 \%A, the average minimum v alue of the d spacing observed over all patterns. The intensities were indexed and processed using the program LAUEGEN [2] and the reflections were integrated and the background was removed using the program ARGONNE_BOXES, which is based on the multidimensional minimum s(I)/I method described in [3]. Each observation was corrected for absorption in the crystal, using the calculated wavelength-dependent absorption coefficient, 0.0886l + 0.0940 mm-1, and for absorption of the diffracted beam through the cylindrical cryostat heat shields; the maximum and minimum values of the transmission were 0.966 and 0.715 respectively. The reflections were normalised to a common incident wavelength using the program LAUENORM [4]. Since only the ratios between unit cell dimensions can be determined in the white-beam Laue technique, the dimensions found by X-ray diffraction at ?K were used in the neutron refinement; the observed ratios and angles were, however, in accord with the X-ray values. Unit cell parameters for the neutron analysis (and their estimated standard deviations) were assumed to be the same as those for the X-ray analysis since both data sets were collected at the same temperature. ; _diffrn_ambient_temperature 20(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 'Very-Intense Vertical-Axis Laue diffractometer ' _diffrn_measurement_method test _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51904 _diffrn_reflns_av_R_equivalents 0.2672 _diffrn_reflns_av_sigmaI/netI 0.2908 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 23.39 _reflns_number_total 13238 _reflns_number_gt 6142 _reflns_threshold_expression >2sigma(I) _computing_data_collection VIVALDI _computing_cell_refinement VIVALDI _computing_data_reduction LAUEGEN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Isotropic refinement of F^2^against ALL reflections.The weighted R-factor wRand 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^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13238 _refine_ls_number_parameters 1409 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2649 _refine_ls_R_factor_gt 0.1392 _refine_ls_wR_factor_ref 0.2560 _refine_ls_wR_factor_gt 0.2260 _refine_ls_goodness_of_fit_ref 1.485 _refine_ls_restrained_S_all 1.485 _refine_ls_shift/su_max 0.475 _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 O2 O -0.1774(8) 0.3358(7) 0.3160(5) 0.020(3) Uiso 1 1 d . . . O1 O -0.3097(7) 0.6426(7) 0.1826(4) 0.009(2) Uiso 1 1 d . . . O2A O 0.4766(7) 0.2382(7) 1.3421(4) 0.009(2) Uiso 1 1 d . . . C8 C -0.3357(5) 0.6284(5) 0.3294(4) 0.005(2) Uiso 1 1 d . . . C9 C -0.1734(6) 0.3746(6) 0.2140(4) 0.013(2) Uiso 1 1 d . . . C3 C -0.1603(5) 0.4612(6) 0.2785(4) 0.003(2) Uiso 1 1 d . . . C4 C -0.1996(5) 0.4035(5) 0.2689(3) 0.0017(18) Uiso 1 1 d . . . C1 C -0.2871(5) 0.5772(5) 0.2304(3) 0.0013(18) Uiso 1 1 d . . . C7 C -0.3138(5) 0.6052(5) 0.2853(3) 0.005(2) Uiso 1 1 d . . . C10 C -0.1496(5) 0.3522(5) 0.1687(4) 0.006(2) Uiso 1 1 d . . . C11 C -0.3558(6) 0.6576(6) 0.3828(4) 0.006(2) Uiso 1 1 d . . . C21 C -0.0533(6) 0.3294(6) 0.0251(4) 0.009(2) Uiso 1 1 d . . . C5 C -0.2943(6) 0.4441(6) 0.2678(4) 0.012(2) Uiso 1 1 d . . . C6 C -0.3273(6) 0.5203(6) 0.2210(4) 0.008(2) Uiso 1 1 d . . . C22 C -0.0719(5) 0.3530(5) 0.0795(3) 0.0015(19) Uiso 1 1 d . . . O1A O 0.7746(6) 0.2532(7) 1.4097(4) 0.008(2) Uiso 1 1 d . . . C17 C -0.1265(6) 0.3287(6) 0.1144(4) 0.012(2) Uiso 1 1 d . . . C2 C -0.1932(5) 0.5373(5) 0.2316(4) 0.002(2) Uiso 1 1 d . . . C4A C 0.5472(6) 0.2573(6) 1.3420(4) 0.008(2) Uiso 1 1 d . . . C15 C -0.3221(6) 0.7134(6) 0.4579(4) 0.015(2) Uiso 1 1 d . . . C16 C -0.3030(6) 0.6848(6) 0.4056(4) 0.013(2) Uiso 1 1 d . . . C12 C -0.4257(6) 0.6534(5) 0.4123(4) 0.007(2) Uiso 1 1 d . . . C9A C 0.5517(6) 0.3061(6) 1.2847(4) 0.016(2) Uiso 1 1 d . . . C10A C 0.5562(6) 0.3413(6) 1.2349(4) 0.012(2) Uiso 1 1 d . . . C3A C 0.5459(6) 0.3040(6) 1.3902(4) 0.010(2) Uiso 1 1 d . . . C5A C 0.6216(5) 0.1828(6) 1.3528(4) 0.005(2) Uiso 1 1 d . . . C18 C -0.1582(6) 0.2747(6) 0.0968(4) 0.020(2) Uiso 1 1 d . . . C15A C 0.6207(6) 0.1523(6) 1.6690(4) 0.014(2) Uiso 1 1 d . . . C13A C 0.7012(6) 0.0178(6) 1.6577(4) 0.016(2) Uiso 1 1 d . . . C11A C 0.6770(5) 0.1283(5) 1.5755(4) 0.006(2) Uiso 1 1 d . . . C2A C 0.6258(5) 0.3162(5) 1.3963(4) 0.003(2) Uiso 1 1 d . . . C6A C 0.7043(5) 0.1924(6) 1.3600(4) 0.004(2) Uiso 1 1 d . . . C14 C -0.3921(5) 0.7111(5) 0.4871(4) 0.009(2) Uiso 1 1 d . . . C12A C 0.7114(6) 0.0455(6) 1.6004(4) 0.019(2) Uiso 1 1 d . . . C7A C 0.6970(6) 0.1918(7) 1.4677(4) 0.018(3) Uiso 1 1 d . . . C20 C -0.0883(6) 0.2826(6) 0.0074(4) 0.013(2) Uiso 1 1 d . . . C8A C 0.6880(6) 0.1599(6) 1.5157(4) 0.010(2) Uiso 1 1 d . . . C16A C 0.6309(6) 0.1846(7) 1.6103(4) 0.019(2) Uiso 1 1 d . . . C17A C 0.5583(6) 0.3844(6) 1.1774(4) 0.010(2) Uiso 1 1 d . . . C14A C 0.6552(6) 0.0685(6) 1.6936(4) 0.013(2) Uiso 1 1 d . . . C19 C -0.1396(6) 0.2544(6) 0.0435(4) 0.016(2) Uiso 1 1 d . . . C1A C 0.7016(5) 0.2372(6) 1.4093(4) 0.006(2) Uiso 1 1 d . . . C13 C -0.4441(6) 0.6817(6) 0.4642(4) 0.009(2) Uiso 1 1 d . . . C18A C 0.6343(6) 0.3745(7) 1.1552(4) 0.023(2) Uiso 1 1 d . . . C22A C 0.4876(7) 0.4433(6) 1.1481(4) 0.021(2) Uiso 1 1 d . . . H22A H 0.4345(15) 0.4500(13) 1.1634(9) 0.040(5) Uiso 1 1 d . . . C19A C 0.6417(7) 0.4133(7) 1.0974(4) 0.024(3) Uiso 1 1 d . . . C21A C 0.4943(7) 0.4815(7) 1.0909(5) 0.027(3) Uiso 1 1 d . . . C20A C 0.5693(6) 0.4678(7) 1.0681(5) 0.022(3) Uiso 1 1 d . . . O2B O 0.3193(7) 0.3519(7) 0.3277(5) 0.013(3) Uiso 1 1 d . . . O1B O 0.1699(6) 0.6478(7) 0.1798(4) 0.007(2) Uiso 1 1 d . . . C7B C 0.2461(6) 0.5277(6) 0.1506(4) 0.013(2) Uiso 1 1 d . . . C9B C 0.2425(6) 0.4697(6) 0.3586(4) 0.012(2) Uiso 1 1 d . . . C8B C 0.2674(5) 0.4993(5) 0.1083(4) 0.007(2) Uiso 1 1 d . . . C1B C 0.2169(6) 0.5667(6) 0.2012(4) 0.009(2) Uiso 1 1 d . . . C4B C 0.2727(5) 0.4319(5) 0.3062(4) 0.0049(19) Uiso 1 1 d . . . C2B C 0.1579(6) 0.5306(6) 0.2340(4) 0.008(2) Uiso 1 1 d . . . C10B C 0.2190(6) 0.4988(6) 0.4007(4) 0.011(2) Uiso 1 1 d . . . C6B C 0.2875(5) 0.5552(6) 0.2430(4) 0.005(2) Uiso 1 1 d . . . C3B C 0.2034(5) 0.4447(6) 0.2651(4) 0.006(2) Uiso 1 1 d . . . C11B C 0.2920(6) 0.4599(6) 0.0607(4) 0.018(2) Uiso 1 1 d . . . C17B C 0.1928(6) 0.5392(6) 0.4492(4) 0.011(2) Uiso 1 1 d . . . C5B C 0.3324(6) 0.4684(6) 0.2743(4) 0.008(2) Uiso 1 1 d . . . C18B C 0.2433(5) 0.5081(6) 0.4999(3) 0.010(2) Uiso 1 1 d . . . C19B C 0.2241(6) 0.5479(6) 0.5449(4) 0.011(2) Uiso 1 1 d . . . C22B C 0.1252(6) 0.6071(6) 0.4423(4) 0.013(2) Uiso 1 1 d . . . C20B C 0.1530(6) 0.6196(6) 0.5397(4) 0.011(2) Uiso 1 1 d . . . C14B C 0.3294(6) 0.3842(6) -0.0346(4) 0.017(2) Uiso 1 1 d . . . C16B C 0.2502(5) 0.4976(5) 0.0061(3) 0.004(2) Uiso 1 1 d . . . C15B C 0.2672(6) 0.4582(6) -0.0413(4) 0.013(2) Uiso 1 1 d . . . C21B C 0.1068(7) 0.6468(7) 0.4886(4) 0.026(3) Uiso 1 1 d . . . H21C H 0.0560(13) 0.6963(13) 0.4847(9) 0.034(5) Uiso 1 1 d . . . C13B C 0.3723(7) 0.3463(7) 0.0192(4) 0.023(2) Uiso 1 1 d . . . H13B H 0.4144(16) 0.2922(17) 0.0243(11) 0.055(7) Uiso 1 1 d . . . C12B C 0.3552(6) 0.3858(6) 0.0682(4) 0.024(2) Uiso 1 1 d . . . H12B H 0.3833(19) 0.3562(19) 0.1088(13) 0.063(8) Uiso 1 1 d . . . O1D O 0.7752(6) 0.2628(6) 0.9066(4) 0.002(2) Uiso 1 1 d . . . O2D O 0.4699(6) 0.2589(7) 0.8446(4) 0.009(2) Uiso 1 1 d . . . O1C O -0.4374(6) 0.8441(6) 0.0667(4) 0.004(2) Uiso 1 1 d . . . C10D C 0.5611(6) 0.3484(6) 0.7389(4) 0.016(2) Uiso 1 1 d . . . C5D C 0.5468(6) 0.3167(6) 0.8936(4) 0.012(2) Uiso 1 1 d . . . C3D C 0.6194(5) 0.1903(6) 0.8561(4) 0.003(2) Uiso 1 1 d . . . C1C C -0.4590(5) 0.9136(5) 0.0169(4) 0.0047(19) Uiso 1 1 d . . . C4D C 0.5461(6) 0.2696(6) 0.8473(4) 0.008(2) Uiso 1 1 d . . . C8C C -0.4128(6) 0.8651(6) -0.0822(4) 0.011(2) Uiso 1 1 d . . . C9D C 0.5499(5) 0.3146(5) 0.7873(4) 0.004(2) Uiso 1 1 d . . . C7C C -0.4347(5) 0.8859(5) -0.0366(4) 0.006(2) Uiso 1 1 d . . . C6C C -0.4162(6) 0.9685(6) 0.0277(4) 0.007(2) Uiso 1 1 d . . . C7D C 0.7003(5) 0.1990(5) 0.9673(4) 0.003(2) Uiso 1 1 d . . . C16C C -0.3295(6) 0.8529(6) -0.1697(4) 0.012(2) Uiso 1 1 d . . . C2D C 0.7025(6) 0.2005(6) 0.8610(4) 0.008(2) Uiso 1 1 d . . . C12D C 0.6552(6) 0.1947(7) 1.1146(4) 0.018(2) Uiso 1 1 d . . . C17D C 0.5717(6) 0.3863(6) 0.6815(4) 0.009(2) Uiso 1 1 d . . . C1D C 0.7027(6) 0.2440(6) 0.9102(4) 0.009(2) Uiso 1 1 d . . . C8D C 0.6944(6) 0.1656(6) 1.0168(4) 0.010(2) Uiso 1 1 d . . . C11D C 0.6836(5) 0.1390(5) 1.0780(3) 0.004(2) Uiso 1 1 d . . . C11C C -0.3917(6) 0.8390(6) -0.1358(4) 0.009(2) Uiso 1 1 d . . . C16D C 0.7002(6) 0.0611(6) 1.1006(4) 0.017(2) Uiso 1 1 d . . . C6D C 0.6300(5) 0.3245(6) 0.8986(4) 0.003(2) Uiso 1 1 d . . . C13D C 0.6430(6) 0.1669(6) 1.1730(4) 0.017(2) Uiso 1 1 d . . . C2C C -0.5535(5) 0.9565(5) 0.0166(4) 0.004(2) Uiso 1 1 d . . . C14C C -0.3525(5) 0.7887(5) -0.2433(4) 0.008(2) Uiso 1 1 d . . . C12C C -0.4332(6) 0.7979(6) -0.1570(4) 0.012(2) Uiso 1 1 d . . . C14D C 0.6613(6) 0.0855(6) 1.1957(4) 0.016(2) Uiso 1 1 d . . . C18D C 0.5132(6) 0.4589(6) 0.6540(4) 0.009(2) Uiso 1 1 d . . . C13C C -0.4159(6) 0.7745(6) -0.2111(4) 0.017(2) Uiso 1 1 d . . . C19D C 0.5220(6) 0.4903(6) 0.5947(4) 0.019(2) Uiso 1 1 d . . . C15C C -0.3086(6) 0.8291(6) -0.2224(4) 0.009(2) Uiso 1 1 d . . . C22D C 0.6408(6) 0.3487(6) 0.6529(4) 0.021(2) Uiso 1 1 d . . . C15D C 0.6879(6) 0.0323(7) 1.1584(4) 0.017(2) Uiso 1 1 d . . . C21D C 0.6537(7) 0.3824(6) 0.5944(4) 0.019(2) Uiso 1 1 d . . . C20D C 0.5912(6) 0.4533(6) 0.5649(4) 0.012(2) Uiso 1 1 d . . . O2I O -0.0182(7) 0.2336(7) 0.8370(4) 0.011(3) Uiso 1 1 d . . . C17I C 0.0637(5) 0.3650(5) 0.6681(4) 0.005(2) Uiso 1 1 d . . . C10I C 0.0625(5) 0.3307(6) 0.7266(4) 0.009(2) Uiso 1 1 d . . . C16I C 0.2373(6) 0.0421(6) 1.0921(4) 0.010(2) Uiso 1 1 d . . . O1I O 0.2781(6) 0.2518(6) 0.9059(4) 0.007(2) Uiso 1 1 d . . . C11I C 0.1828(5) 0.1219(5) 1.0693(4) 0.005(2) Uiso 1 1 d . . . C9I C 0.0587(6) 0.2993(6) 0.7765(4) 0.008(2) Uiso 1 1 d . . . C4I C 0.0538(5) 0.2533(6) 0.8378(4) 0.006(2) Uiso 1 1 d . . . C15I C 0.2288(5) 0.0104(6) 1.1508(4) 0.007(2) Uiso 1 1 d . . . C5I C 0.0495(6) 0.3031(6) 0.8836(4) 0.009(2) Uiso 1 1 d . . . C20I C 0.0772(6) 0.4241(6) 0.5498(4) 0.020(2) Uiso 1 1 d . . . C8I C 0.1900(5) 0.1582(5) 1.0106(4) 0.003(2) Uiso 1 1 d . . . C3I C 0.1277(6) 0.1778(6) 0.8503(4) 0.012(2) Uiso 1 1 d . . . C14I C 0.1725(6) 0.0547(6) 1.1859(4) 0.012(2) Uiso 1 1 d . . . C7I C 0.1987(6) 0.1924(6) 0.9622(4) 0.018(3) Uiso 1 1 d . . . C1I C 0.2051(5) 0.2374(5) 0.9046(4) 0.004(2) Uiso 1 1 d . . . C6I C 0.1282(5) 0.3183(5) 0.8895(4) 0.002(2) Uiso 1 1 d . . . C12I C 0.1222(6) 0.1642(6) 1.1054(4) 0.013(2) Uiso 1 1 d . . . C22I C 0.0889(5) 0.3124(6) 0.6274(4) 0.011(2) Uiso 1 1 d . . . C2I C 0.2071(6) 0.1900(6) 0.8561(4) 0.008(2) Uiso 1 1 d . . . C21I C 0.0971(6) 0.3434(7) 0.5681(4) 0.020(2) Uiso 1 1 d . . . H21B H 0.1118(16) 0.3103(16) 0.5391(11) 0.051(6) Uiso 1 1 d . . . C13I C 0.1170(6) 0.1295(6) 1.1625(4) 0.014(2) Uiso 1 1 d . . . C18I C 0.0471(6) 0.4451(6) 0.6479(4) 0.016(2) Uiso 1 1 d . . . C19I C 0.0547(6) 0.4741(6) 0.5878(4) 0.015(2) Uiso 1 1 d . . . O2E O 0.2688(6) 0.2611(6) 0.4135(4) 0.001(2) Uiso 1 1 d . . . O1E O -0.0172(7) 0.2332(7) 0.3373(5) 0.013(3) Uiso 1 1 d . . . C4E C 0.2005(5) 0.2368(5) 0.4132(4) 0.004(2) Uiso 1 1 d . . . C11E C 0.0767(6) 0.3719(6) 0.1775(4) 0.007(2) Uiso 1 1 d . . . C7E C 0.0612(6) 0.2997(6) 0.2841(4) 0.010(2) Uiso 1 1 d . . . C9E C 0.1975(5) 0.1923(5) 0.4720(4) 0.002(2) Uiso 1 1 d . . . C17E C 0.1935(6) 0.1269(6) 0.5824(4) 0.009(2) Uiso 1 1 d . . . C10E C 0.1951(5) 0.1586(6) 0.5203(4) 0.007(2) Uiso 1 1 d . . . C8E C 0.0701(5) 0.3328(6) 0.2357(4) 0.007(2) Uiso 1 1 d . . . C5E C 0.1227(5) 0.3172(5) 0.3984(4) 0.0000(19) Uiso 1 1 d . . . C1E C 0.0567(6) 0.2525(6) 0.3429(4) 0.013(2) Uiso 1 1 d . . . C6E C 0.0455(7) 0.3011(7) 0.3887(4) 0.019(3) Uiso 1 1 d . . . C3E C 0.2088(6) 0.1907(6) 0.3648(4) 0.010(2) Uiso 1 1 d . . . C2E C 0.1308(6) 0.1764(6) 0.3555(4) 0.012(2) Uiso 1 1 d . . . C12E C 0.0236(5) 0.4522(5) 0.1566(4) 0.006(2) Uiso 1 1 d . . . C16E C 0.1347(6) 0.3334(6) 0.1433(4) 0.018(2) Uiso 1 1 d . . . C21E C 0.1230(6) 0.0772(6) 0.6630(4) 0.017(2) Uiso 1 1 d . . . C22E C 0.1259(6) 0.1087(6) 0.6039(4) 0.015(2) Uiso 1 1 d . . . C15E C 0.1405(7) 0.3720(7) 0.0842(5) 0.023(3) Uiso 1 1 d . . . C13E C 0.0282(6) 0.4891(6) 0.0987(4) 0.018(2) Uiso 1 1 d . . . C14E C 0.0854(6) 0.4519(6) 0.0634(4) 0.013(2) Uiso 1 1 d . . . C18E C 0.2618(6) 0.1123(6) 0.6205(4) 0.019(2) Uiso 1 1 d . . . H18C H 0.3077(12) 0.1303(11) 0.6057(8) 0.026(4) Uiso 1 1 d . . . C20E C 0.1884(6) 0.0658(6) 0.7029(4) 0.014(2) Uiso 1 1 d . . . C19E C 0.2598(7) 0.0829(6) 0.6822(4) 0.023(2) Uiso 1 1 d . . . H19C H 0.3002(17) 0.0773(17) 0.7071(12) 0.060(7) Uiso 1 1 d . . . O1F O 0.4254(6) 0.1496(6) 0.4263(4) 0.002(2) Uiso 1 1 d . . . C11F C 0.5295(5) -0.0438(5) 0.3073(4) 0.009(2) Uiso 1 1 d . . . C7F C 0.4921(6) 0.0278(6) 0.3987(4) 0.011(2) Uiso 1 1 d . . . C8F C 0.5098(6) -0.0061(6) 0.3579(4) 0.012(2) Uiso 1 1 d . . . C12F C 0.5100(6) 0.0003(6) 0.2507(4) 0.010(2) Uiso 1 1 d . . . C1F C 0.4683(5) 0.0653(6) 0.4475(4) 0.007(2) Uiso 1 1 d . . . C2F C 0.4108(5) 0.0334(6) 0.4864(4) 0.002(2) Uiso 1 1 d . . . C13F C 0.5291(5) -0.0354(6) 0.2031(4) 0.008(2) Uiso 1 1 d . . . C16F C 0.5603(6) -0.1278(6) 0.3184(4) 0.022(2) Uiso 1 1 d . . . C14F C 0.5654(6) -0.1170(6) 0.2122(4) 0.011(2) Uiso 1 1 d . . . C6F C 0.5472(5) 0.0512(6) 0.4852(4) 0.005(2) Uiso 1 1 d . . . C15F C 0.5785(6) -0.1659(7) 0.2685(4) 0.016(2) Uiso 1 1 d . . . H15F H 0.5954(19) -0.212(2) 0.2773(12) 0.059(8) Uiso 1 1 d . . . O1G O 0.9281(6) 0.1499(6) 0.9247(4) 0.003(2) Uiso 1 1 d . . . C11G C 1.0553(5) -0.0387(6) 0.8058(4) 0.008(2) Uiso 1 1 d . . . C8G C 1.0326(5) -0.0019(5) 0.8564(4) 0.006(2) Uiso 1 1 d . . . C2G C 1.0434(5) 0.0530(5) 0.9902(4) 0.003(2) Uiso 1 1 d . . . C7G C 1.0079(5) 0.0272(5) 0.8972(3) 0.0010(19) Uiso 1 1 d . . . C1G C 0.9731(6) 0.0661(6) 0.9472(4) 0.009(2) Uiso 1 1 d . . . C16G C 1.0006(6) -0.0198(6) 0.7580(4) 0.015(2) Uiso 1 1 d . . . C15G C 1.0234(6) -0.0588(6) 0.7124(4) 0.017(2) Uiso 1 1 d . . . C14G C 1.0998(6) -0.1198(6) 0.7126(4) 0.018(2) Uiso 1 1 d . . . C3G C 1.0869(6) -0.0318(6) 1.0208(4) 0.005(2) Uiso 1 1 d . . . C12G C 1.1365(6) -0.0946(6) 0.8053(4) 0.020(2) Uiso 1 1 d . . . C13G C 1.1601(7) -0.1386(6) 0.7595(4) 0.018(2) Uiso 1 1 d . . . H13G H 1.2164(15) -0.1756(14) 0.7576(9) 0.039(5) Uiso 1 1 d . . . O1H O 0.9355(7) 0.1553(6) 0.4331(4) 0.006(2) Uiso 1 1 d . . . C8H C 0.9098(6) 0.1351(6) 0.5820(4) 0.011(2) Uiso 1 1 d . . . C1H C 0.9574(5) 0.0886(6) 0.4822(4) 0.010(2) Uiso 1 1 d . . . C12H C 0.8335(6) 0.1379(6) 0.6714(4) 0.007(2) Uiso 1 1 d . . . C7H C 0.9333(5) 0.1149(5) 0.5352(4) 0.006(2) Uiso 1 1 d . . . C13H C 0.8116(6) 0.1605(6) 0.7238(4) 0.011(2) Uiso 1 1 d . . . C11H C 0.8877(5) 0.1607(5) 0.6358(4) 0.006(2) Uiso 1 1 d . . . C6H C 1.0531(6) 0.0452(6) 0.4832(4) 0.009(2) Uiso 1 1 d . . . C2H C 0.9162(6) 0.0298(6) 0.4721(4) 0.010(2) Uiso 1 1 d . . . C14H C 0.8510(5) 0.2076(5) 0.7443(4) 0.005(2) Uiso 1 1 d . . . C15H C 0.9063(6) 0.2284(6) 0.7098(4) 0.016(2) Uiso 1 1 d . . . C16H C 0.9228(5) 0.2091(5) 0.6544(3) 0.0065(19) Uiso 1 1 d . . . H3L H 0.2178(12) 0.2273(12) 0.3216(8) 0.024(5) Uiso 1 1 d . . . H5U H 0.0393(11) 0.2685(11) 0.9236(7) 0.014(4) Uiso 1 1 d . . . H61 H -0.3536(11) 0.9397(11) 0.0269(7) 0.018(4) Uiso 1 1 d . . . H52 H 0.5358(10) 0.2808(11) 0.9338(7) 0.012(4) Uiso 1 1 d . . . H62 H 0.4931(13) 0.3556(13) 1.3821(8) 0.026(5) Uiso 1 1 d . . . H51 H -0.0046(11) 0.3545(12) 0.3785(7) 0.017(4) Uiso 1 1 d . . . H3T H 0.1168(14) 0.1420(14) 0.8895(9) 0.030(6) Uiso 1 1 d . . . H6E H 0.3320(12) 0.5785(12) 0.2209(9) 0.028(5) Uiso 1 1 d . . . H3B H -0.1740(9) 0.4703(9) 0.3232(6) 0.005(4) Uiso 1 1 d . . . H2P H 1.0895(11) 0.0769(11) 0.9686(7) 0.017(4) Uiso 1 1 d . . . H2K H 0.1193(14) 0.1387(14) 0.3968(9) 0.030(5) Uiso 1 1 d . . . H4E H 0.3626(10) 0.4313(11) 0.2440(7) 0.015(4) Uiso 1 1 d . . . H27A H 0.7522(12) 0.1434(12) 0.8704(8) 0.021(5) Uiso 1 1 d . . . H2U H 0.2600(13) 0.1332(14) 0.8686(9) 0.033(5) Uiso 1 1 d . . . H3C H 0.5350(11) 0.2676(12) 1.4298(8) 0.018(4) Uiso 1 1 d . . . H6A H -0.3923(13) 0.5444(13) 0.2193(9) 0.030(5) Uiso 1 1 d . . . H2R H 1.0817(13) 0.0814(13) 0.4891(9) 0.031(5) Uiso 1 1 d . . . H5L H 0.1314(12) 0.3534(13) 0.3584(9) 0.025(5) Uiso 1 1 d . . . H6T H 0.1406(12) 0.3511(12) 0.8462(8) 0.025(5) Uiso 1 1 d . . . H2T H 0.2207(12) 0.2240(13) 0.8144(9) 0.029(5) Uiso 1 1 d . . . H6R H 0.8493(11) 0.0606(11) 0.4730(7) 0.020(4) Uiso 1 1 d . . . H2C H 0.6349(16) 0.3554(15) 1.3565(11) 0.046(7) Uiso 1 1 d . . . H6D H 0.7131(12) 0.2234(12) 1.3189(8) 0.024(5) Uiso 1 1 d . . . H6C H 0.7526(13) 0.1354(13) 1.3692(9) 0.029(5) Uiso 1 1 d . . . H3K H 0.2611(10) 0.1364(11) 0.3739(7) 0.012(4) Uiso 1 1 d . . . H6L H 0.0330(10) 0.2646(11) 0.4279(7) 0.012(4) Uiso 1 1 d . . . H212 H -0.1789(12) 0.5265(12) 0.1889(8) 0.024(5) Uiso 1 1 d . . . H5A H -0.3110(13) 0.4581(13) 0.3111(9) 0.031(5) Uiso 1 1 d . . . H5C H 0.6242(11) 0.1472(11) 1.3165(8) 0.019(4) Uiso 1 1 d . . . H6M H 0.5904(12) 0.0734(12) 0.4587(8) 0.024(5) Uiso 1 1 d . . . H3A H -0.0906(12) 0.4331(12) 0.2788(8) 0.029(5) Uiso 1 1 d . . . H2A H -0.1667(12) 0.5798(12) 0.2446(9) 0.028(5) Uiso 1 1 d . . . H1 H -0.3679(13) 0.6687(12) 0.1777(8) 0.024(5) Uiso 1 1 d . . . H6I H 0.6409(11) 0.3613(11) 0.8583(8) 0.016(4) Uiso 1 1 d . . . H5T H -0.0038(13) 0.3563(14) 0.8739(9) 0.032(5) Uiso 1 1 d . . . H3I H 0.6098(11) 0.1547(11) 0.8984(8) 0.015(4) Uiso 1 1 d . . . H3E H 0.2293(10) 0.4080(10) 0.2316(7) 0.010(4) Uiso 1 1 d . . . H5K H 0.1142(11) 0.3495(11) 0.4350(7) 0.014(4) Uiso 1 1 d . . . H5I H 0.4973(11) 0.3750(11) 0.8848(7) 0.016(4) Uiso 1 1 d . . . H3Q H 1.1357(12) -0.0368(12) 1.0511(8) 0.026(5) Uiso 1 1 d . . . H2F H -0.5835(12) 0.9179(12) 0.0061(8) 0.024(5) Uiso 1 1 d . . . H28 H 0.1069(12) 0.5395(12) 0.2030(8) 0.023(5) Uiso 1 1 d . . . H27 H -0.0650(13) 0.2839(13) 0.8283(8) 0.028(5) Uiso 1 1 d . . . H65 H 0.1243(12) 0.3508(12) 0.9288(8) 0.023(5) Uiso 1 1 d . . . H2Q H 1.0124(10) 0.0918(10) 1.0230(7) 0.012(4) Uiso 1 1 d . . . H3P H 1.1163(12) -0.0664(12) 0.9856(8) 0.026(5) Uiso 1 1 d . . . H6F H 0.2622(12) 0.5904(13) 0.2751(9) 0.030(5) Uiso 1 1 d . . . H3J H 0.6170(12) 0.1577(12) 0.8225(8) 0.021(5) Uiso 1 1 d . . . H24 H -0.5700(10) 0.9666(10) 0.0600(7) 0.013(4) Uiso 1 1 d . . . H22 H -0.0436(13) 0.3912(14) 0.0925(9) 0.036(5) Uiso 1 1 d . . . H2H H 0.1335(13) 0.1446(13) 0.3250(9) 0.028(5) Uiso 1 1 d . . . H29 H 0.4292(12) 0.2905(12) 1.3337(8) 0.023(5) Uiso 1 1 d . . . H2E H 0.1276(11) 0.5695(11) 0.2647(7) 0.018(4) Uiso 1 1 d . . . H6N H 0.5243(12) 0.0904(13) 0.5199(8) 0.029(5) Uiso 1 1 d . . . H16C H -0.2962(10) 0.8850(10) -0.1519(7) 0.013(4) Uiso 1 1 d . . . H2J H 0.7095(10) 0.2354(11) 0.8185(7) 0.012(4) Uiso 1 1 d . . . H1C H -0.3765(12) 0.8173(12) 0.0672(8) 0.024(5) Uiso 1 1 d . . . H12A H 0.7470(12) 0.0045(12) 1.5721(8) 0.028(5) Uiso 1 1 d . . . H13H H 0.7667(12) 0.1405(12) 0.7502(8) 0.024(4) Uiso 1 1 d . . . H1B H 0.2001(11) 0.6687(11) 0.1533(8) 0.017(4) Uiso 1 1 d . . . H12H H 0.8029(12) 0.1067(12) 0.6559(8) 0.024(5) Uiso 1 1 d . . . H14 H -0.4062(13) 0.7341(13) 0.5264(9) 0.037(6) Uiso 1 1 d . . . H2N H 0.3882(11) 0.0672(11) 0.5202(7) 0.017(4) Uiso 1 1 d . . . H5F H 0.3794(12) 0.4628(12) 0.3051(8) 0.023(5) Uiso 1 1 d . . . H5B H -0.3210(11) 0.4036(11) 0.2606(8) 0.020(4) Uiso 1 1 d . . . H23 H 0.4671(12) 0.2226(13) 0.8811(9) 0.029(5) Uiso 1 1 d . . . H3F H 0.1611(11) 0.4193(11) 0.2883(8) 0.020(4) Uiso 1 1 d . . . H14C H -0.3380(13) 0.7699(13) -0.2862(9) 0.031(5) Uiso 1 1 d . . . H2M H 0.3584(11) 0.0382(11) 0.4576(7) 0.018(4) Uiso 1 1 d . . . H6S H 1.0653(11) 0.0330(11) 0.4390(8) 0.018(4) Uiso 1 1 d . . . H2D H 0.6231(11) 0.3466(11) 1.4339(8) 0.017(4) Uiso 1 1 d . . . H14I H 0.1680(14) 0.0271(14) 1.2317(9) 0.033(6) Uiso 1 1 d . . . H31 H 0.1300(11) 0.1428(12) 0.8144(8) 0.020(4) Uiso 1 1 d . . . H6J H 0.6273(13) 0.3492(13) 0.9348(9) 0.028(5) Uiso 1 1 d . . . H1A H 0.7782(11) 0.2874(11) 1.3756(8) 0.018(4) Uiso 1 1 d . . . H15C H -0.2612(14) 0.8438(14) -0.2471(10) 0.039(6) Uiso 1 1 d . . . H5D H 0.6118(12) 0.1437(12) 1.3921(8) 0.019(5) Uiso 1 1 d . . . H6B H -0.3158(11) 0.5146(11) 0.1748(7) 0.015(4) Uiso 1 1 d . . . H2S H 0.9338(13) 0.0108(13) 0.4299(9) 0.030(5) Uiso 1 1 d . . . H12C H -0.4828(12) 0.7871(12) -0.1331(8) 0.029(5) Uiso 1 1 d . . . H1H H 0.8768(13) 0.1802(12) 0.4318(8) 0.023(5) Uiso 1 1 d . . . H14F H 0.5791(13) -0.1438(13) 0.1765(9) 0.032(5) Uiso 1 1 d . . . H14B H 0.3412(18) 0.3581(18) -0.0718(13) 0.064(8) Uiso 1 1 d . . . H69 H -0.4336(14) 0.9827(14) 0.0690(10) 0.037(6) Uiso 1 1 d . . . H16I H 0.2777(13) 0.0152(13) 1.0671(9) 0.030(5) Uiso 1 1 d . . . H1I H 0.2792(10) 0.2900(11) 0.8729(8) 0.015(4) Uiso 1 1 d . . . H1F H 0.4548(11) 0.1688(11) 0.3951(8) 0.017(4) Uiso 1 1 d . . . H18 H -0.1923(14) 0.2551(14) 0.1234(10) 0.041(6) Uiso 1 1 d . . . H20B H 0.1379(15) 0.6466(15) 0.5734(11) 0.046(6) Uiso 1 1 d . . . H20D H 0.6040(15) 0.4776(15) 0.5239(11) 0.042(6) Uiso 1 1 d . . . H12E H -0.0231(12) 0.4829(12) 0.1845(8) 0.027(5) Uiso 1 1 d . . . H1E H -0.0185(11) 0.1957(12) 0.3702(8) 0.021(4) Uiso 1 1 d . . . H14H H 0.8357(12) 0.2216(12) 0.7878(8) 0.027(5) Uiso 1 1 d . . . H16G H 0.9440(13) 0.0224(12) 0.7603(8) 0.028(5) Uiso 1 1 d . . . H20I H 0.0800(13) 0.4499(13) 0.5031(9) 0.035(6) Uiso 1 1 d . . . H14G H 1.1148(14) -0.1477(14) 0.6784(10) 0.038(6) Uiso 1 1 d . . . H15I H 0.2710(14) -0.0462(14) 1.1705(9) 0.037(5) Uiso 1 1 d . . . H14D H 0.6525(12) 0.0654(13) 1.2403(8) 0.027(5) Uiso 1 1 d . . . H21 H -0.0126(11) 0.3481(11) -0.0017(7) 0.019(4) Uiso 1 1 d . . . H13A H 0.7213(15) -0.0419(16) 1.6756(10) 0.047(6) Uiso 1 1 d . . . H18D H 0.4623(17) 0.4889(17) 0.6758(12) 0.057(7) Uiso 1 1 d . . . H1G H 0.9587(10) 0.1684(10) 0.8921(7) 0.009(4) Uiso 1 1 d . . . H19D H 0.4719(14) 0.5506(14) 0.5751(9) 0.039(5) Uiso 1 1 d . . . H1D H 0.8249(10) 0.2147(11) 0.9163(7) 0.010(4) Uiso 1 1 d . . . H26 H 0.3215(11) 0.2159(11) 0.4209(7) 0.013(4) Uiso 1 1 d . . . H12 H -0.4681(13) 0.6363(13) 0.3925(9) 0.032(5) Uiso 1 1 d . . . H15G H 0.9820(17) -0.0468(16) 0.6785(12) 0.060(7) Uiso 1 1 d . . . H21D H 0.7033(16) 0.3549(15) 0.5774(10) 0.048(6) Uiso 1 1 d . . . H14E H 0.0935(13) 0.4779(14) 0.0206(9) 0.030(6) Uiso 1 1 d . . . H16D H 0.7229(14) 0.0188(14) 1.0706(10) 0.042(6) Uiso 1 1 d . . . H22I H 0.1056(12) 0.2542(13) 0.6440(8) 0.030(5) Uiso 1 1 d . . . H12I H 0.0794(14) 0.2234(15) 1.0876(10) 0.044(6) Uiso 1 1 d . . . H18I H 0.0258(14) 0.4847(14) 0.6785(10) 0.042(6) Uiso 1 1 d . . . H15D H 0.6997(13) -0.0257(15) 1.1733(9) 0.038(5) Uiso 1 1 d . . . H15H H 0.9368(14) 0.2631(14) 0.7239(10) 0.043(6) Uiso 1 1 d . . . H12D H 0.6422(11) 0.2510(12) 1.0965(8) 0.022(4) Uiso 1 1 d . . . H15B H 0.2328(14) 0.4846(14) -0.0850(10) 0.043(6) Uiso 1 1 d . . . H13I H 0.0701(13) 0.1607(13) 1.1886(9) 0.035(5) Uiso 1 1 d . . . H15E H 0.1862(15) 0.3434(14) 0.0605(10) 0.042(6) Uiso 1 1 d . . . H13F H 0.5129(13) 0.0036(13) 0.1600(9) 0.033(5) Uiso 1 1 d . . . H19B H 0.2622(14) 0.5269(14) 0.5859(10) 0.044(6) Uiso 1 1 d . . . H22D H 0.6858(13) 0.3001(13) 0.6751(9) 0.034(5) Uiso 1 1 d . . . H13C H -0.4471(12) 0.7437(12) -0.2254(8) 0.027(5) Uiso 1 1 d . . . H14A H 0.6484(12) 0.0435(12) 1.7381(9) 0.027(5) Uiso 1 1 d . . . H13E H -0.0124(15) 0.5497(16) 0.0839(10) 0.048(6) Uiso 1 1 d . . . H12F H 0.4852(12) 0.0672(13) 0.2420(9) 0.033(5) Uiso 1 1 d . . . H16 H -0.2527(14) 0.6865(14) 0.3863(9) 0.039(5) Uiso 1 1 d . . . H18B H 0.2958(12) 0.4560(12) 0.5055(8) 0.024(4) Uiso 1 1 d . . . H12G H 1.1815(15) -0.1094(15) 0.8411(11) 0.051(7) Uiso 1 1 d . . . H13D H 0.6201(14) 0.2086(14) 1.2015(9) 0.040(5) Uiso 1 1 d . . . H16H H 0.9670(13) 0.2266(13) 0.6265(9) 0.033(5) Uiso 1 1 d . . . H16B H 0.2025(14) 0.5559(14) -0.0028(9) 0.038(5) Uiso 1 1 d . . . H13 H -0.4963(13) 0.6755(13) 0.4859(9) 0.034(5) Uiso 1 1 d . . . H2 H -0.1180(11) 0.3055(11) 0.3166(7) 0.013(4) Uiso 1 1 d . . . H20 H -0.0699(12) 0.2624(12) -0.0342(8) 0.027(5) Uiso 1 1 d . . . H20E H 0.1848(12) 0.0461(12) 0.7446(9) 0.028(5) Uiso 1 1 d . . . H211 H 0.2904(11) 0.3295(11) 0.3556(7) 0.015(4) Uiso 1 1 d . . . H22E H 0.0820(15) 0.1129(15) 0.5765(10) 0.048(6) Uiso 1 1 d . . . H16E H 0.1782(15) 0.2810(15) 0.1592(10) 0.044(6) Uiso 1 1 d . . . H15A H 0.5887(13) 0.1970(13) 1.6953(9) 0.034(5) Uiso 1 1 d . . . H21E H 0.0798(12) 0.0616(12) 0.6798(8) 0.026(4) Uiso 1 1 d . . . H15 H -0.2849(15) 0.7321(15) 0.4761(10) 0.047(6) Uiso 1 1 d . . . H19 H -0.1612(14) 0.2124(14) 0.0291(10) 0.044(6) Uiso 1 1 d . . . H19I H 0.0406(13) 0.5353(14) 0.5737(9) 0.034(5) Uiso 1 1 d . . . H18A H 0.6911(13) 0.3320(13) 1.1804(8) 0.034(5) Uiso 1 1 d . . . H16A H 0.6127(14) 0.2357(16) 1.5963(10) 0.040(5) Uiso 1 1 d . . . H22B H 0.0841(12) 0.6288(12) 0.4039(8) 0.029(5) Uiso 1 1 d . . . H16F H 0.5641(14) -0.1572(14) 0.3594(10) 0.042(6) Uiso 1 1 d . . . H21A H 0.5762(15) 0.5009(15) 1.0280(10) 0.045(6) Uiso 1 1 d . . . H19A H 0.6927(15) 0.4049(14) 1.0823(9) 0.041(6) Uiso 1 1 d . . . H20A H 0.4402(14) 0.5207(14) 1.0697(9) 0.040(5) Uiso 1 1 d . . . _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 O2 C4 1.439(15) . ? O2 H2 0.98(3) . ? O1 C1 1.420(14) . ? O1 H1 0.95(3) . ? O2A C4A 1.421(15) . ? O2A H29 1.01(3) . ? C8 C7 1.197(12) . ? C8 C11 1.443(14) . ? C9 C10 1.222(13) . ? C9 C4 1.485(13) . ? C3 C2 1.537(13) . ? C3 C4 1.546(13) . ? C3 H3B 1.097(19) . ? C3 H3A 1.14(2) . ? C4 C5 1.549(13) . ? C1 C7 1.481(13) . ? C1 C2 1.534(12) . ? C1 C6 1.544(14) . ? C10 C17 1.425(14) . ? C11 C16 1.383(14) . ? C11 C12 1.417(13) . ? C21 C20 1.380(14) . ? C21 C22 1.417(13) . ? C21 H21 1.05(2) . ? C5 C6 1.537(14) . ? C5 H5A 1.10(3) . ? C5 H5B 1.08(3) . ? C6 H6A 1.06(3) . ? C6 H6B 1.11(2) . ? C22 C17 1.395(14) . ? C22 H22 1.11(3) . ? O1A C1A 1.429(15) . ? O1A H1A 0.94(3) . ? C17 C18 1.458(15) . ? C2 H212 1.06(2) . ? C2 H2A 1.16(3) . ? C4A C9A 1.484(14) . ? C4A C5A 1.493(14) . ? C4A C3A 1.556(14) . ? C15 C14 1.403(14) . ? C15 C16 1.415(14) . ? C15 H15 0.99(3) . ? C16 H16 0.99(3) . ? C12 C13 1.400(14) . ? C12 H12 1.07(3) . ? C9A C10A 1.235(14) . ? C10A C17A 1.429(14) . ? C3A C2A 1.526(13) . ? C3A H62 1.05(3) . ? C3A H3C 1.09(2) . ? C5A C6A 1.553(13) . ? C5A H5C 1.17(2) . ? C5A H5D 1.11(2) . ? C18 C19 1.371(15) . ? C18 H18 0.97(3) . ? C15A C16A 1.420(14) . ? C15A C14A 1.453(15) . ? C15A H15A 1.11(3) . ? C13A C12A 1.368(15) . ? C13A C14A 1.403(15) . ? C13A H13A 1.04(3) . ? C11A C12A 1.439(15) . ? C11A C8A 1.444(14) . ? C11A C16A 1.449(15) . ? C2A C1A 1.556(13) . ? C2A H2C 1.11(3) . ? C2A H2D 1.13(2) . ? C6A C1A 1.551(13) . ? C6A H6D 1.06(2) . ? C6A H6C 1.07(3) . ? C14 C13 1.403(14) . ? C14 H14 1.08(3) . ? C12A H12A 1.11(3) . ? C7A C8A 1.198(14) . ? C7A C1A 1.475(14) . ? C20 C19 1.398(14) . ? C20 H20 1.11(2) . ? C16A H16A 0.88(4) . ? C17A C18A 1.382(14) . ? C17A C22A 1.394(14) . ? C14A H14A 1.08(2) . ? C19 H19 1.11(3) . ? C13 H13 1.07(3) . ? C18A C19A 1.428(15) . ? C18A H18A 1.11(2) . ? C22A C21A 1.411(15) . ? C22A H22A 0.96(3) . ? C19A C20A 1.386(15) . ? C19A H19A 0.93(3) . ? C21A C20A 1.362(16) . ? C21A H20A 1.02(3) . ? C20A H21A 1.05(3) . ? O2B C4B 1.405(15) . ? O2B H211 0.95(3) . ? O1B C1B 1.423(15) . ? O1B H1B 0.93(3) . ? C7B C8B 1.199(13) . ? C7B C1B 1.494(14) . ? C9B C10B 1.208(13) . ? C9B C4B 1.521(14) . ? C8B C11B 1.426(15) . ? C1B C6B 1.526(13) . ? C1B C2B 1.553(14) . ? C4B C3B 1.491(12) . ? C4B C5B 1.562(14) . ? C2B C3B 1.537(15) . ? C2B H28 1.11(2) . ? C2B H2E 1.11(2) . ? C10B C17B 1.456(14) . ? C6B C5B 1.550(14) . ? C6B H6E 1.11(3) . ? C6B H6F 1.08(3) . ? C3B H3E 1.12(2) . ? C3B H3F 1.11(2) . ? C11B C12B 1.396(15) . ? C11B C16B 1.402(13) . ? C17B C22B 1.360(13) . ? C17B C18B 1.388(13) . ? C5B H4E 1.08(2) . ? C5B H5F 1.07(2) . ? C18B C19B 1.372(14) . ? C18B H18B 1.05(3) . ? C19B C20B 1.436(14) . ? C19B H19B 1.10(2) . ? C22B C21B 1.399(15) . ? C22B H22B 1.08(2) . ? C20B C21B 1.357(14) . ? C20B H20B 1.00(3) . ? C14B C15B 1.388(14) . ? C14B C13B 1.394(14) . ? C14B H14B 1.06(4) . ? C16B C15B 1.417(13) . ? C16B H16B 1.08(3) . ? C15B H15B 1.12(2) . ? C21B H21C 1.01(3) . ? C13B C12B 1.454(16) . ? C13B H13B 0.99(3) . ? C12B H12B 1.03(3) . ? O1D C1D 1.447(14) . ? O1D H1D 0.98(2) . ? O2D C4D 1.437(15) . ? O2D H23 0.99(3) . ? O1C C1C 1.498(13) . ? O1C H1C 1.00(3) . ? C10D C9D 1.232(13) . ? C10D C17D 1.430(14) . ? C5D C4D 1.533(14) . ? C5D C6D 1.541(14) . ? C5D H52 1.10(2) . ? C5D H5I 1.10(2) . ? C3D C4D 1.537(13) . ? C3D C2D 1.558(13) . ? C3D H3I 1.12(2) . ? C3D H3J 1.10(2) . ? C1C C7C 1.442(13) . ? C1C C2C 1.549(12) . ? C1C C6C 1.555(14) . ? C4D C9D 1.499(13) . ? C8C C7C 1.210(13) . ? C8C C11C 1.426(14) . ? C6C C2C 1.489(14) 2_475 ? C6C H61 1.03(2) . ? C6C H69 1.06(3) . ? C7D C8D 1.221(13) . ? C7D C1D 1.439(13) . ? C16C C15C 1.386(14) . ? C16C C11C 1.408(14) . ? C16C H16C 1.13(2) . ? C2D C1D 1.540(14) . ? C2D H27A 1.08(2) . ? C2D H2J 1.11(2) . ? C12D C13D 1.403(15) . ? C12D C11D 1.420(14) . ? C12D H12D 1.00(3) . ? C17D C22D 1.385(14) . ? C17D C18D 1.398(14) . ? C1D C6D 1.545(14) . ? C8D C11D 1.449(13) . ? C11D C16D 1.374(14) . ? C11C C12C 1.410(14) . ? C16D C15D 1.393(15) . ? C16D H16D 1.12(3) . ? C6D H6I 1.11(2) . ? C6D H6J 1.04(3) . ? C13D C14D 1.429(15) . ? C13D H13D 1.08(3) . ? C2C C6C 1.489(14) 2_475 ? C2C H2F 1.12(3) . ? C2C H24 1.08(2) . ? C14C C13C 1.410(14) . ? C14C C15C 1.427(14) . ? C14C H14C 1.12(2) . ? C12C C13C 1.410(14) . ? C12C H12C 1.09(2) . ? C14D C15D 1.399(15) . ? C14D H14D 1.06(2) . ? C18D C19D 1.421(14) . ? C18D H18D 1.04(3) . ? C13C H13C 1.04(3) . ? C19D C20D 1.399(15) . ? C19D H19D 1.15(3) . ? C15C H15C 1.09(3) . ? C22D C21D 1.437(15) . ? C22D H22D 1.01(3) . ? C15D H15D 1.02(3) . ? C21D C20D 1.423(15) . ? C21D H21D 0.95(3) . ? C20D H20D 1.03(3) . ? O2I C4I 1.453(15) . ? O2I H27 0.98(3) . ? C17I C10I 1.392(13) . ? C17I C18I 1.404(14) . ? C17I C22I 1.449(14) . ? C10I C9I 1.209(13) . ? C16I C15I 1.409(14) . ? C16I C11I 1.440(14) . ? C16I H16I 0.96(3) . ? O1I C1I 1.416(14) . ? O1I H1I 0.95(3) . ? C11I C8I 1.431(13) . ? C11I C12I 1.434(14) . ? C9I C4I 1.535(13) . ? C4I C3I 1.498(14) . ? C4I C5I 1.543(14) . ? C15I C14I 1.398(14) . ? C15I H15I 1.06(3) . ? C5I C6I 1.536(13) . ? C5I H5U 1.08(2) . ? C5I H5T 1.07(3) . ? C20I C19I 1.365(15) . ? C20I C21I 1.399(15) . ? C20I H20I 1.11(2) . ? C8I C7I 1.221(14) . ? C3I C2I 1.516(14) . ? C3I H3T 1.08(3) . ? C3I H31 1.16(2) . ? C14I C13I 1.382(14) . ? C14I H14I 1.11(2) . ? C7I C1I 1.465(14) . ? C1I C2I 1.569(13) . ? C1I C6I 1.588(13) . ? C6I H6T 1.14(2) . ? C6I H65 1.19(2) . ? C12I C13I 1.381(14) . ? C12I H12I 1.08(3) . ? C22I C21I 1.417(15) . ? C22I H22I 1.02(3) . ? C2I H2U 1.11(3) . ? C2I H2T 1.12(2) . ? C21I H21B 0.97(3) . ? C13I H13I 1.07(3) . ? C18I C19I 1.424(14) . ? C18I H18I 1.09(3) . ? C19I H19I 1.06(3) . ? O2E C4E 1.444(14) . ? O2E H26 0.98(2) . ? O1E C1E 1.495(15) . ? O1E H1E 0.94(3) . ? C4E C9E 1.469(13) . ? C4E C3E 1.531(14) . ? C4E C5E 1.589(13) . ? C11E C16E 1.354(14) . ? C11E C12E 1.432(14) . ? C11E C8E 1.435(13) . ? C7E C8E 1.214(13) . ? C7E C1E 1.496(14) . ? C9E C10E 1.188(13) . ? C17E C22E 1.415(14) . ? C17E C18E 1.424(14) . ? C17E C10E 1.455(13) . ? C5E C6E 1.535(14) . ? C5E H5L 1.09(2) . ? C5E H5K 1.12(2) . ? C1E C6E 1.505(15) . ? C1E C2E 1.508(14) . ? C6E H51 1.04(3) . ? C6E H6L 1.10(2) . ? C3E C2E 1.527(14) . ? C3E H3L 1.14(2) . ? C3E H3K 1.07(2) . ? C2E H2K 1.14(3) . ? C2E H2H 1.01(3) . ? C12E C13E 1.407(14) . ? C12E H12E 1.09(2) . ? C16E C15E 1.445(15) . ? C16E H16E 1.00(3) . ? C21E C22E 1.397(14) . ? C21E C20E 1.426(14) . ? C21E H21E 0.96(3) . ? C22E H22E 0.99(3) . ? C15E C14E 1.436(15) . ? C15E H15E 1.01(3) . ? C13E C14E 1.354(15) . ? C13E H13E 1.08(3) . ? C14E H14E 1.05(3) . ? C18E C19E 1.441(15) . ? C18E H18C 1.02(3) . ? C20E C19E 1.462(15) . ? C20E H20E 0.98(3) . ? C19E H19C 0.89(4) . ? O1F C1F 1.459(14) . ? O1F H1F 0.97(2) . ? C11F C12F 1.387(13) . ? C11F C16F 1.434(14) . ? C11F C8F 1.466(14) . ? C7F C8F 1.220(14) . ? C7F C1F 1.430(14) . ? C12F C13F 1.381(14) . ? C12F H12F 1.14(3) . ? C1F C2F 1.551(13) . ? C1F C6F 1.572(12) . ? C2F C6F 1.494(14) 2_656 ? C2F H2N 1.09(2) . ? C2F H2M 1.12(2) . ? C13F C14F 1.394(13) . ? C13F H13F 1.09(2) . ? C16F C15F 1.455(15) . ? C16F H16F 0.99(3) . ? C14F C15F 1.415(15) . ? C14F H14F 1.03(3) . ? C6F C2F 1.494(14) 2_656 ? C6F H6M 1.12(2) . ? C6F H6N 1.17(2) . ? C15F H15F 0.79(4) . ? O1G C1G 1.461(15) . ? O1G H1G 1.00(2) . ? C11G C16G 1.395(13) . ? C11G C12G 1.420(14) . ? C11G C8G 1.458(14) . ? C8G C7G 1.186(12) . ? C2G C3G 1.513(14) . ? C2G C1G 1.532(12) . ? C2G H2P 1.13(2) . ? C2G H2Q 1.15(2) . ? C7G C1G 1.496(13) . ? C1G C3G 1.543(14) 2_757 ? C16G C15G 1.379(15) . ? C16G H16G 1.02(3) . ? C15G C14G 1.397(15) . ? C15G H15G 1.02(3) . ? C14G C13G 1.443(14) . ? C14G H14G 1.02(3) . ? C3G C1G 1.543(14) 2_757 ? C3G H3Q 1.09(2) . ? C3G H3P 1.14(2) . ? C12G C13G 1.440(15) . ? C12G H12G 1.09(3) . ? C13G H13G 0.98(3) . ? O1H C1H 1.456(14) . ? O1H H1H 0.96(3) . ? C8H C7H 1.240(13) . ? C8H C11H 1.425(14) . ? C1H C7H 1.418(14) . ? C1H C6H 1.568(13) . ? C1H C2H 1.593(15) . ? C12H C13H 1.373(14) . ? C12H C11H 1.384(14) . ? C12H H12H 1.05(3) . ? C13H C14H 1.469(14) . ? C13H H13H 1.12(2) . ? C11H C16H 1.416(13) . ? C6H C2H 1.495(14) 2_756 ? C6H H2R 1.02(3) . ? C6H H6S 1.10(2) . ? C2H C6H 1.495(14) 2_756 ? C2H H6R 1.10(2) . ? C2H H2S 1.11(3) . ? C14H C15H 1.369(14) . ? C14H H14H 1.10(2) . ? C15H C16H 1.407(13) . ? C15H H15H 1.09(3) . ? C16H H16H 1.10(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 C4 O2 H2 109.1(14) . . ? C1 O1 H1 110.9(15) . . ? C4A O2A H29 104.3(15) . . ? C7 C8 C11 175.2(10) . . ? C10 C9 C4 177.5(11) . . ? C2 C3 C4 110.8(7) . . ? C2 C3 H3B 113.6(12) . . ? C4 C3 H3B 105.6(11) . . ? C2 C3 H3A 110.4(12) . . ? C4 C3 H3A 111.1(13) . . ? H3B C3 H3A 105.1(14) . . ? O2 C4 C9 107.2(8) . . ? O2 C4 C3 112.0(8) . . ? C9 C4 C3 111.4(8) . . ? O2 C4 C5 105.8(8) . . ? C9 C4 C5 110.6(7) . . ? C3 C4 C5 109.7(7) . . ? O1 C1 C7 109.3(8) . . ? O1 C1 C2 106.1(8) . . ? C7 C1 C2 110.7(7) . . ? O1 C1 C6 110.1(7) . . ? C7 C1 C6 110.0(7) . . ? C2 C1 C6 110.6(7) . . ? C8 C7 C1 179.6(11) . . ? C9 C10 C17 176.7(10) . . ? C16 C11 C12 121.5(8) . . ? C16 C11 C8 118.7(9) . . ? C12 C11 C8 119.7(9) . . ? C20 C21 C22 120.5(9) . . ? C20 C21 H21 120.2(13) . . ? C22 C21 H21 119.3(13) . . ? C6 C5 C4 111.9(8) . . ? C6 C5 H5A 108.9(14) . . ? C4 C5 H5A 107.8(13) . . ? C6 C5 H5B 110.8(12) . . ? C4 C5 H5B 109.0(13) . . ? H5A C5 H5B 108.3(18) . . ? C5 C6 C1 110.7(7) . . ? C5 C6 H6A 110.1(14) . . ? C1 C6 H6A 114.5(14) . . ? C5 C6 H6B 116.7(13) . . ? C1 C6 H6B 103.8(12) . . ? H6A C6 H6B 100.7(16) . . ? C17 C22 C21 118.9(9) . . ? C17 C22 H22 121.9(14) . . ? C21 C22 H22 119.2(14) . . ? C1A O1A H1A 112.7(14) . . ? C22 C17 C10 121.8(9) . . ? C22 C17 C18 119.7(9) . . ? C10 C17 C18 118.5(9) . . ? C1 C2 C3 111.9(7) . . ? C1 C2 H212 105.8(12) . . ? C3 C2 H212 111.7(14) . . ? C1 C2 H2A 107.2(12) . . ? C3 C2 H2A 106.7(12) . . ? H212 C2 H2A 113.6(17) . . ? O2A C4A C9A 110.4(8) . . ? O2A C4A C5A 108.4(9) . . ? C9A C4A C5A 109.2(8) . . ? O2A C4A C3A 111.8(8) . . ? C9A C4A C3A 107.8(9) . . ? C5A C4A C3A 109.1(7) . . ? C14 C15 C16 119.9(10) . . ? C14 C15 H15 118.8(16) . . ? C16 C15 H15 121.2(17) . . ? C11 C16 C15 119.1(9) . . ? C11 C16 H16 122.8(15) . . ? C15 C16 H16 118.0(15) . . ? C13 C12 C11 119.0(9) . . ? C13 C12 H12 120.1(14) . . ? C11 C12 H12 120.4(14) . . ? C10A C9A C4A 174.5(11) . . ? C9A C10A C17A 177.8(11) . . ? C2A C3A C4A 112.9(8) . . ? C2A C3A H62 114.7(15) . . ? C4A C3A H62 107.9(13) . . ? C2A C3A H3C 111.9(12) . . ? C4A C3A H3C 103.1(13) . . ? H62 C3A H3C 105.4(17) . . ? C4A C5A C6A 115.4(8) . . ? C4A C5A H5C 110.1(11) . . ? C6A C5A H5C 111.1(12) . . ? C4A C5A H5D 107.4(13) . . ? C6A C5A H5D 110.6(12) . . ? H5C C5A H5D 101.3(15) . . ? C19 C18 C17 119.2(10) . . ? C19 C18 H18 122.6(16) . . ? C17 C18 H18 118.2(16) . . ? C16A C15A C14A 122.9(10) . . ? C16A C15A H15A 113.8(13) . . ? C14A C15A H15A 123.1(13) . . ? C12A C13A C14A 121.3(10) . . ? C12A C13A H13A 122.0(16) . . ? C14A C13A H13A 116.3(16) . . ? C12A C11A C8A 122.4(9) . . ? C12A C11A C16A 121.1(9) . . ? C8A C11A C16A 116.4(9) . . ? C3A C2A C1A 112.1(8) . . ? C3A C2A H2C 111.2(15) . . ? C1A C2A H2C 110.0(15) . . ? C3A C2A H2D 109.8(12) . . ? C1A C2A H2D 107.2(11) . . ? H2C C2A H2D 106.2(18) . . ? C1A C6A C5A 111.0(7) . . ? C1A C6A H6D 111.4(14) . . ? C5A C6A H6D 106.0(12) . . ? C1A C6A H6C 110.8(13) . . ? C5A C6A H6C 108.7(14) . . ? H6D C6A H6C 108.8(17) . . ? C15 C14 C13 120.5(9) . . ? C15 C14 H14 118.8(14) . . ? C13 C14 H14 120.6(14) . . ? C13A C12A C11A 120.8(10) . . ? C13A C12A H12A 120.7(14) . . ? C11A C12A H12A 118.5(13) . . ? C8A C7A C1A 175.0(12) . . ? C21 C20 C19 121.0(9) . . ? C21 C20 H20 118.8(14) . . ? C19 C20 H20 119.9(14) . . ? C7A C8A C11A 174.2(12) . . ? C15A C16A C11A 115.5(10) . . ? C15A C16A H16A 122.5(17) . . ? C11A C16A H16A 121.9(17) . . ? C18A C17A C22A 120.1(9) . . ? C18A C17A C10A 117.7(8) . . ? C22A C17A C10A 121.4(9) . . ? C13A C14A C15A 118.3(9) . . ? C13A C14A H14A 118.2(14) . . ? C15A C14A H14A 123.5(14) . . ? C18 C19 C20 120.4(10) . . ? C18 C19 H19 121.2(15) . . ? C20 C19 H19 118.2(15) . . ? O1A C1A C7A 108.0(8) . . ? O1A C1A C6A 109.1(8) . . ? C7A C1A C6A 112.4(9) . . ? O1A C1A C2A 109.1(8) . . ? C7A C1A C2A 109.9(8) . . ? C6A C1A C2A 108.3(7) . . ? C12 C13 C14 119.9(9) . . ? C12 C13 H13 116.4(14) . . ? C14 C13 H13 123.5(14) . . ? C17A C18A C19A 121.2(9) . . ? C17A C18A H18A 120.6(14) . . ? C19A C18A H18A 118.0(14) . . ? C17A C22A C21A 118.0(10) . . ? C17A C22A H22A 120.2(15) . . ? C21A C22A H22A 120.6(15) . . ? C20A C19A C18A 116.1(10) . . ? C20A C19A H19A 122.9(16) . . ? C18A C19A H19A 120.8(16) . . ? C20A C21A C22A 120.4(10) . . ? C20A C21A H20A 124.2(16) . . ? C22A C21A H20A 115.4(16) . . ? C21A C20A C19A 123.0(10) . . ? C21A C20A H21A 121.5(16) . . ? C19A C20A H21A 115.3(16) . . ? C4B O2B H211 110.8(14) . . ? C1B O1B H1B 109.1(14) . . ? C8B C7B C1B 177.2(10) . . ? C10B C9B C4B 179.2(11) . . ? C7B C8B C11B 175.3(11) . . ? O1B C1B C7B 109.0(8) . . ? O1B C1B C6B 110.9(9) . . ? C7B C1B C6B 112.3(8) . . ? O1B C1B C2B 107.1(8) . . ? C7B C1B C2B 107.3(8) . . ? C6B C1B C2B 110.0(7) . . ? O2B C4B C3B 112.4(9) . . ? O2B C4B C9B 107.5(8) . . ? C3B C4B C9B 111.7(8) . . ? O2B C4B C5B 106.9(8) . . ? C3B C4B C5B 110.1(7) . . ? C9B C4B C5B 107.9(8) . . ? C3B C2B C1B 112.2(8) . . ? C3B C2B H28 113.8(13) . . ? C1B C2B H28 108.9(13) . . ? C3B C2B H2E 112.8(11) . . ? C1B C2B H2E 104.8(12) . . ? H28 C2B H2E 103.7(15) . . ? C9B C10B C17B 175.3(11) . . ? C1B C6B C5B 112.5(8) . . ? C1B C6B H6E 112.2(12) . . ? C5B C6B H6E 110.2(13) . . ? C1B C6B H6F 107.6(13) . . ? C5B C6B H6F 109.3(13) . . ? H6E C6B H6F 104.7(17) . . ? C4B C3B C2B 114.2(8) . . ? C4B C3B H3E 107.4(11) . . ? C2B C3B H3E 109.2(11) . . ? C4B C3B H3F 109.5(11) . . ? C2B C3B H3F 111.9(12) . . ? H3E C3B H3F 103.9(15) . . ? C12B C11B C16B 120.8(9) . . ? C12B C11B C8B 121.2(8) . . ? C16B C11B C8B 118.0(9) . . ? C22B C17B C18B 122.7(9) . . ? C22B C17B C10B 120.4(8) . . ? C18B C17B C10B 116.7(9) . . ? C6B C5B C4B 112.7(8) . . ? C6B C5B H4E 112.1(12) . . ? C4B C5B H4E 105.2(12) . . ? C6B C5B H5F 110.7(13) . . ? C4B C5B H5F 109.4(13) . . ? H4E C5B H5F 106.4(16) . . ? C19B C18B C17B 118.4(9) . . ? C19B C18B H18B 118.2(12) . . ? C17B C18B H18B 123.4(13) . . ? C18B C19B C20B 120.7(8) . . ? C18B C19B H19B 121.9(15) . . ? C20B C19B H19B 117.3(15) . . ? C17B C22B C21B 118.0(8) . . ? C17B C22B H22B 122.2(14) . . ? C21B C22B H22B 119.7(14) . . ? C21B C20B C19B 117.6(9) . . ? C21B C20B H20B 122.1(17) . . ? C19B C20B H20B 120.2(16) . . ? C15B C14B C13B 120.7(10) . . ? C15B C14B H14B 116.8(17) . . ? C13B C14B H14B 122.4(18) . . ? C11B C16B C15B 120.2(9) . . ? C11B C16B H16B 124.2(14) . . ? C15B C16B H16B 115.5(13) . . ? C14B C15B C16B 119.7(8) . . ? C14B C15B H15B 117.5(15) . . ? C16B C15B H15B 122.8(15) . . ? C20B C21B C22B 122.5(10) . . ? C20B C21B H21C 118.5(15) . . ? C22B C21B H21C 119.0(15) . . ? C14B C13B C12B 120.1(10) . . ? C14B C13B H13B 120.4(17) . . ? C12B C13B H13B 119.5(17) . . ? C11B C12B C13B 118.2(9) . . ? C11B C12B H12B 121(2) . . ? C13B C12B H12B 120.0(19) . . ? C1D O1D H1D 110.4(14) . . ? C4D O2D H23 108.2(14) . . ? C1C O1C H1C 105.1(14) . . ? C9D C10D C17D 177.4(11) . . ? C4D C5D C6D 111.7(8) . . ? C4D C5D H52 102.3(12) . . ? C6D C5D H52 111.2(12) . . ? C4D C5D H5I 111.9(12) . . ? C6D C5D H5I 109.7(12) . . ? H52 C5D H5I 109.9(15) . . ? C4D C3D C2D 111.6(8) . . ? C4D C3D H3I 105.6(12) . . ? C2D C3D H3I 109.7(11) . . ? C4D C3D H3J 110.8(12) . . ? C2D C3D H3J 113.8(12) . . ? H3I C3D H3J 104.9(15) . . ? C7C C1C O1C 108.7(8) . . ? C7C C1C C2C 111.2(7) . . ? O1C C1C C2C 105.4(8) . . ? C7C C1C C6C 111.5(8) . . ? O1C C1C C6C 110.0(7) . . ? C2C C1C C6C 109.9(8) . . ? O2D C4D C9D 103.8(7) . . ? O2D C4D C5D 111.7(8) . . ? C9D C4D C5D 110.3(8) . . ? O2D C4D C3D 110.8(8) . . ? C9D C4D C3D 107.3(8) . . ? C5D C4D C3D 112.5(7) . . ? C7C C8C C11C 176.0(11) . . ? C10D C9D C4D 173.9(9) . . ? C8C C7C C1C 177.1(10) . . ? C2C C6C C1C 110.8(7) 2_475 . ? C2C C6C H61 111.4(13) 2_475 . ? C1C C6C H61 109.0(14) . . ? C2C C6C H69 107.2(15) 2_475 . ? C1C C6C H69 106.8(15) . . ? H61 C6C H69 111.6(17) . . ? C8D C7D C1D 175.4(10) . . ? C15C C16C C11C 123.2(10) . . ? C15C C16C H16C 120.2(13) . . ? C11C C16C H16C 116.6(12) . . ? C1D C2D C3D 111.0(8) . . ? C1D C2D H27A 108.8(12) . . ? C3D C2D H27A 109.6(13) . . ? C1D C2D H2J 109.5(12) . . ? C3D C2D H2J 107.1(11) . . ? H27A C2D H2J 110.8(16) . . ? C13D C12D C11D 117.3(10) . . ? C13D C12D H12D 124.5(14) . . ? C11D C12D H12D 118.1(13) . . ? C22D C17D C18D 120.4(9) . . ? C22D C17D C10D 118.4(9) . . ? C18D C17D C10D 121.2(9) . . ? C7D C1D O1D 110.4(7) . . ? C7D C1D C2D 112.4(9) . . ? O1D C1D C2D 108.5(8) . . ? C7D C1D C6D 111.1(8) . . ? O1D C1D C6D 104.7(8) . . ? C2D C1D C6D 109.4(7) . . ? C7D C8D C11D 170.3(11) . . ? C16D C11D C12D 120.1(9) . . ? C16D C11D C8D 120.8(9) . . ? C12D C11D C8D 119.1(9) . . ? C16C C11C C12C 117.4(9) . . ? C16C C11C C8C 122.1(9) . . ? C12C C11C C8C 120.4(9) . . ? C11D C16D C15D 123.6(10) . . ? C11D C16D H16D 118.2(14) . . ? C15D C16D H16D 118.2(15) . . ? C5D C6D C1D 112.2(8) . . ? C5D C6D H6I 111.3(12) . . ? C1D C6D H6I 108.3(12) . . ? C5D C6D H6J 105.5(14) . . ? C1D C6D H6J 107.6(13) . . ? H6I C6D H6J 111.8(17) . . ? C12D C13D C14D 121.6(10) . . ? C12D C13D H13D 118.5(15) . . ? C14D C13D H13D 119.8(14) . . ? C6C C2C C1C 111.8(8) 2_475 . ? C6C C2C H2F 108.4(12) 2_475 . ? C1C C2C H2F 109.2(12) . . ? C6C C2C H24 111.1(13) 2_475 . ? C1C C2C H24 108.8(11) . . ? H2F C2C H24 107.5(16) . . ? C13C C14C C15C 120.2(9) . . ? C13C C14C H14C 119.8(14) . . ? C15C C14C H14C 119.9(14) . . ? C13C C12C C11C 121.5(9) . . ? C13C C12C H12C 118.0(14) . . ? C11C C12C H12C 120.3(13) . . ? C15D C14D C13D 119.7(9) . . ? C15D C14D H14D 119.7(15) . . ? C13D C14D H14D 120.6(15) . . ? C17D C18D C19D 119.1(9) . . ? C17D C18D H18D 121.0(16) . . ? C19D C18D H18D 119.8(17) . . ? C12C C13C C14C 119.2(10) . . ? C12C C13C H13C 119.9(14) . . ? C14C C13C H13C 120.8(14) . . ? C20D C19D C18D 121.4(9) . . ? C20D C19D H19D 123.1(14) . . ? C18D C19D H19D 115.2(14) . . ? C16C C15C C14C 118.4(9) . . ? C16C C15C H15C 119.1(14) . . ? C14C C15C H15C 122.5(14) . . ? C17D C22D C21D 121.1(9) . . ? C17D C22D H22D 119.3(14) . . ? C21D C22D H22D 119.1(15) . . ? C16D C15D C14D 117.6(11) . . ? C16D C15D H15D 121.4(15) . . ? C14D C15D H15D 121.0(15) . . ? C20D C21D C22D 118.4(10) . . ? C20D C21D H21D 124.0(16) . . ? C22D C21D H21D 117.6(17) . . ? C19D C20D C21D 119.3(9) . . ? C19D C20D H20D 124.0(16) . . ? C21D C20D H20D 116.2(16) . . ? C4I O2I H27 105.4(16) . . ? C10I C17I C18I 123.9(9) . . ? C10I C17I C22I 116.5(9) . . ? C18I C17I C22I 119.5(8) . . ? C9I C10I C17I 176.7(11) . . ? C15I C16I C11I 116.5(9) . . ? C15I C16I H16I 125.0(15) . . ? C11I C16I H16I 118.5(14) . . ? C1I O1I H1I 111.3(13) . . ? C8I C11I C12I 120.6(8) . . ? C8I C11I C16I 119.2(8) . . ? C12I C11I C16I 120.2(8) . . ? C10I C9I C4I 174.9(11) . . ? O2I C4I C3I 107.6(9) . . ? O2I C4I C9I 107.8(7) . . ? C3I C4I C9I 109.0(8) . . ? O2I C4I C5I 111.8(8) . . ? C3I C4I C5I 110.9(7) . . ? C9I C4I C5I 109.7(8) . . ? C14I C15I C16I 122.1(9) . . ? C14I C15I H15I 118.5(14) . . ? C16I C15I H15I 119.0(15) . . ? C6I C5I C4I 113.0(8) . . ? C6I C5I H5U 111.3(12) . . ? C4I C5I H5U 103.4(12) . . ? C6I C5I H5T 112.2(15) . . ? C4I C5I H5T 109.4(14) . . ? H5U C5I H5T 107.0(17) . . ? C19I C20I C21I 122.3(10) . . ? C19I C20I H20I 117.2(15) . . ? C21I C20I H20I 120.5(15) . . ? C7I C8I C11I 175.1(10) . . ? C4I C3I C2I 113.0(9) . . ? C4I C3I H3T 107.1(14) . . ? C2I C3I H3T 112.1(14) . . ? C4I C3I H31 109.0(11) . . ? C2I C3I H31 111.6(12) . . ? H3T C3I H31 103.6(17) . . ? C13I C14I C15I 120.7(9) . . ? C13I C14I H14I 119.7(15) . . ? C15I C14I H14I 119.3(14) . . ? C8I C7I C1I 176.7(11) . . ? O1I C1I C7I 108.1(8) . . ? O1I C1I C2I 110.4(8) . . ? C7I C1I C2I 110.1(8) . . ? O1I C1I C6I 109.7(8) . . ? C7I C1I C6I 110.6(8) . . ? C2I C1I C6I 107.9(7) . . ? C5I C6I C1I 110.0(8) . . ? C5I C6I H6T 110.5(12) . . ? C1I C6I H6T 105.9(12) . . ? C5I C6I H65 110.1(12) . . ? C1I C6I H65 106.9(11) . . ? H6T C6I H65 113.2(16) . . ? C13I C12I C11I 120.3(9) . . ? C13I C12I H12I 119.6(15) . . ? C11I C12I H12I 120.1(15) . . ? C21I C22I C17I 118.9(10) . . ? C21I C22I H22I 123.3(14) . . ? C17I C22I H22I 117.5(13) . . ? C3I C2I C1I 112.3(8) . . ? C3I C2I H2U 111.3(15) . . ? C1I C2I H2U 106.2(13) . . ? C3I C2I H2T 112.3(13) . . ? C1I C2I H2T 106.1(13) . . ? H2U C2I H2T 108.4(17) . . ? C20I C21I C22I 119.4(10) . . ? C20I C21I H21B 119.1(17) . . ? C22I C21I H21B 121.3(17) . . ? C12I C13I C14I 119.9(9) . . ? C12I C13I H13I 119.8(14) . . ? C14I C13I H13I 120.2(14) . . ? C17I C18I C19I 119.8(10) . . ? C17I C18I H18I 119.0(14) . . ? C19I C18I H18I 121.1(15) . . ? C20I C19I C18I 120.0(10) . . ? C20I C19I H19I 122.0(14) . . ? C18I C19I H19I 117.9(14) . . ? C4E O2E H26 111.6(14) . . ? C1E O1E H1E 109.8(14) . . ? O2E C4E C9E 108.1(7) . . ? O2E C4E C3E 109.7(8) . . ? C9E C4E C3E 113.7(8) . . ? O2E C4E C5E 103.9(8) . . ? C9E C4E C5E 111.1(7) . . ? C3E C4E C5E 109.9(7) . . ? C16E C11E C12E 120.4(8) . . ? C16E C11E C8E 119.8(9) . . ? C12E C11E C8E 119.8(8) . . ? C8E C7E C1E 174.8(11) . . ? C10E C9E C4E 177.6(10) . . ? C22E C17E C18E 120.7(8) . . ? C22E C17E C10E 120.0(8) . . ? C18E C17E C10E 119.3(9) . . ? C9E C10E C17E 171.5(11) . . ? C7E C8E C11E 177.1(10) . . ? C6E C5E C4E 110.1(8) . . ? C6E C5E H5L 107.9(13) . . ? C4E C5E H5L 109.6(13) . . ? C6E C5E H5K 109.9(12) . . ? C4E C5E H5K 110.2(11) . . ? H5L C5E H5K 109.1(16) . . ? O1E C1E C7E 104.8(8) . . ? O1E C1E C6E 110.4(9) . . ? C7E C1E C6E 109.7(9) . . ? O1E C1E C2E 107.8(9) . . ? C7E C1E C2E 110.1(8) . . ? C6E C1E C2E 113.6(8) . . ? C1E C6E C5E 111.6(9) . . ? C1E C6E H51 112.6(13) . . ? C5E C6E H51 108.9(14) . . ? C1E C6E H6L 103.2(13) . . ? C5E C6E H6L 111.6(12) . . ? H51 C6E H6L 108.9(16) . . ? C2E C3E C4E 111.6(8) . . ? C2E C3E H3L 106.5(12) . . ? C4E C3E H3L 108.6(13) . . ? C2E C3E H3K 110.8(13) . . ? C4E C3E H3K 110.9(12) . . ? H3L C3E H3K 108.1(16) . . ? C1E C2E C3E 111.2(9) . . ? C1E C2E H2K 107.2(14) . . ? C3E C2E H2K 110.0(13) . . ? C1E C2E H2H 110.4(14) . . ? C3E C2E H2H 115.1(14) . . ? H2K C2E H2H 102.4(18) . . ? C13E C12E C11E 119.4(9) . . ? C13E C12E H12E 120.4(13) . . ? C11E C12E H12E 120.0(13) . . ? C11E C16E C15E 119.9(10) . . ? C11E C16E H16E 121.4(16) . . ? C15E C16E H16E 118.3(16) . . ? C22E C21E C20E 119.1(10) . . ? C22E C21E H21E 125.1(13) . . ? C20E C21E H21E 115.8(13) . . ? C21E C22E C17E 121.5(9) . . ? C21E C22E H22E 118.1(17) . . ? C17E C22E H22E 120.1(16) . . ? C14E C15E C16E 118.9(10) . . ? C14E C15E H15E 122.4(16) . . ? C16E C15E H15E 118.4(16) . . ? C14E C13E C12E 121.2(10) . . ? C14E C13E H13E 120.5(16) . . ? C12E C13E H13E 118.2(16) . . ? C13E C14E C15E 119.9(9) . . ? C13E C14E H14E 124.2(15) . . ? C15E C14E H14E 115.9(15) . . ? C17E C18E C19E 119.6(9) . . ? C17E C18E H18C 120.4(13) . . ? C19E C18E H18C 119.4(13) . . ? C21E C20E C19E 120.9(9) . . ? C21E C20E H20E 118.9(15) . . ? C19E C20E H20E 120.2(15) . . ? C18E C19E C20E 118.0(9) . . ? C18E C19E H19C 121(2) . . ? C20E C19E H19C 121.2(19) . . ? C1F O1F H1F 110.3(14) . . ? C12F C11F C16F 120.9(9) . . ? C12F C11F C8F 121.0(9) . . ? C16F C11F C8F 117.6(8) . . ? C8F C7F C1F 176.8(11) . . ? C7F C8F C11F 177.8(10) . . ? C13F C12F C11F 120.9(9) . . ? C13F C12F H12F 117.9(13) . . ? C11F C12F H12F 120.8(13) . . ? C7F C1F O1F 109.3(8) . . ? C7F C1F C2F 111.3(8) . . ? O1F C1F C2F 108.8(8) . . ? C7F C1F C6F 109.4(8) . . ? O1F C1F C6F 108.4(8) . . ? C2F C1F C6F 109.5(7) . . ? C6F C2F C1F 112.4(8) 2_656 . ? C6F C2F H2N 108.8(11) 2_656 . ? C1F C2F H2N 109.9(12) . . ? C6F C2F H2M 107.1(12) 2_656 . ? C1F C2F H2M 108.2(12) . . ? H2N C2F H2M 110.5(15) . . ? C12F C13F C14F 119.6(8) . . ? C12F C13F H13F 116.3(14) . . ? C14F C13F H13F 124.1(14) . . ? C11F C16F C15F 118.1(9) . . ? C11F C16F H16F 118.8(16) . . ? C15F C16F H16F 122.9(16) . . ? C13F C14F C15F 122.5(9) . . ? C13F C14F H14F 119.6(14) . . ? C15F C14F H14F 117.6(15) . . ? C2F C6F C1F 111.1(8) 2_656 . ? C2F C6F H6M 111.1(12) 2_656 . ? C1F C6F H6M 111.7(11) . . ? C2F C6F H6N 111.4(12) 2_656 . ? C1F C6F H6N 105.7(12) . . ? H6M C6F H6N 105.6(16) . . ? C14F C15F C16F 117.3(10) . . ? C14F C15F H15F 129(2) . . ? C16F C15F H15F 114(2) . . ? C1G O1G H1G 108.7(13) . . ? C16G C11G C12G 119.4(9) . . ? C16G C11G C8G 122.3(8) . . ? C12G C11G C8G 118.3(8) . . ? C7G C8G C11G 174.4(10) . . ? C3G C2G C1G 113.5(8) . . ? C3G C2G H2P 110.0(11) . . ? C1G C2G H2P 111.9(11) . . ? C3G C2G H2Q 111.3(11) . . ? C1G C2G H2Q 104.1(11) . . ? H2P C2G H2Q 105.7(15) . . ? C8G C7G C1G 177.4(9) . . ? O1G C1G C7G 109.1(7) . . ? O1G C1G C2G 110.3(8) . . ? C7G C1G C2G 109.1(7) . . ? O1G C1G C3G 108.3(8) . 2_757 ? C7G C1G C3G 110.7(8) . 2_757 ? C2G C1G C3G 109.3(7) . 2_757 ? C15G C16G C11G 120.3(9) . . ? C15G C16G H16G 124.2(14) . . ? C11G C16G H16G 115.5(14) . . ? C16G C15G C14G 122.3(9) . . ? C16G C15G H15G 119.9(18) . . ? C14G C15G H15G 117.6(18) . . ? C15G C14G C13G 119.4(9) . . ? C15G C14G H14G 120.5(15) . . ? C13G C14G H14G 119.8(15) . . ? C2G C3G C1G 111.9(8) . 2_757 ? C2G C3G H3Q 109.7(14) . . ? C1G C3G H3Q 111.0(13) 2_757 . ? C2G C3G H3P 107.2(12) . . ? C1G C3G H3P 108.6(13) 2_757 . ? H3Q C3G H3P 108.3(16) . . ? C11G C12G C13G 120.7(9) . . ? C11G C12G H12G 121.6(16) . . ? C13G C12G H12G 117.5(16) . . ? C12G C13G C14G 117.3(10) . . ? C12G C13G H13G 121.8(16) . . ? C14G C13G H13G 120.5(15) . . ? C1H O1H H1H 105.7(14) . . ? C7H C8H C11H 175.5(10) . . ? C7H C1H O1H 110.1(8) . . ? C7H C1H C6H 110.7(7) . . ? O1H C1H C6H 106.2(8) . . ? C7H C1H C2H 111.0(8) . . ? O1H C1H C2H 110.2(8) . . ? C6H C1H C2H 108.4(8) . . ? C13H C12H C11H 123.0(9) . . ? C13H C12H H12H 118.0(13) . . ? C11H C12H H12H 118.8(13) . . ? C8H C7H C1H 176.4(10) . . ? C12H C13H C14H 118.3(9) . . ? C12H C13H H13H 119.4(13) . . ? C14H C13H H13H 122.3(12) . . ? C12H C11H C16H 118.6(8) . . ? C12H C11H C8H 121.3(9) . . ? C16H C11H C8H 120.1(8) . . ? C2H C6H C1H 112.2(8) 2_756 . ? C2H C6H H2R 111.4(13) 2_756 . ? C1H C6H H2R 110.8(14) . . ? C2H C6H H6S 110.0(13) 2_756 . ? C1H C6H H6S 104.6(11) . . ? H2R C6H H6S 107.6(18) . . ? C6H C2H C1H 112.1(8) 2_756 . ? C6H C2H H6R 111.4(13) 2_756 . ? C1H C2H H6R 107.4(13) . . ? C6H C2H H2S 103.8(14) 2_756 . ? C1H C2H H2S 110.8(14) . . ? H6R C2H H2S 111.4(16) . . ? C15H C14H C13H 118.7(8) . . ? C15H C14H H14H 124.2(14) . . ? C13H C14H H14H 117.1(13) . . ? C14H C15H C16H 121.5(10) . . ? C14H C15H H15H 120.4(15) . . ? C16H C15H H15H 118.1(15) . . ? C15H C16H C11H 119.7(8) . . ? C15H C16H H16H 121.2(14) . . ? C11H C16H H16H 118.9(13) . . ? _diffrn_measured_fraction_theta_max 0.646 _diffrn_reflns_theta_full 23.39 _diffrn_measured_fraction_theta_full 0.646 _refine_diff_density_max 1.703 _refine_diff_density_min -1.281 _refine_diff_density_rms 0.272