# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 188/262 #============================================================================== data_global #============================================================================== _audit_creation_date 04-20-00 _audit_creation_method ? _audit_update_record ; ? ; # 1. SUBMISSION DETAILS _publ_contact_author ; H. Irngartinger Organisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg ; _publ_contact_author_email 'e56@ix.urz.uni-heidelberg.de' _publ_contact_author_fax '(+49) 6221 544205' _publ_contact_author_phone '(+49) 6221 548422' _publ_requested_journal '' _publ_requested_coeditor_name ? _publ_contact_letter ; ; # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? # 3. TITLE AND AUTHOR LIST _publ_section_title ; Ozonolysis of (10R)-10-Acetoxy-3,14-didehydroginkgolide ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Weinges, Klaus' #<--'Last name, first name' ; Organisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg ; 'Schick, Hartmut' #<--'Last name, first name' ; Organisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg ; 'Irngartinger, Hermann' #<--'Last name, first name' ; Organisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg ; 'Oeser, Thomas' #<--'Last name, first name' ; Organisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg ; # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_experimental ; ? ; _publ_section_references ; Enraf-Nonius, CAD4 Operations Manual, Delft, 1988. International Tables for X-Ray Crystallography, Vol. IV, The Kynoch Press, Birmingham, England, 1974 ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; We thank the Deutsche Forschungsgemeinschaft for financial support of the X-ray diffraction facility. ; data_todarac _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetra-(4-chlorophenyl)ethene (3) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H16 Cl4' _chemical_formula_weight 470.19 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 15.9253(4) _cell_length_b 15.9655(4) _cell_length_c 17.8820(3) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 4546.6(2) _cell_formula_units_Z 8 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 77955 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 0.532 _exptl_absorpt_correction_type DENZU_scalepack _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type NONIUS_KAPPA_CCD _diffrn_measurement_method '\p- and \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 77955 _diffrn_reflns_av_R_equivalents 0.130 _diffrn_reflns_av_sigmaI/netI 0.112 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.1 _diffrn_reflns_theta_max 32.6 _reflns_number_total 7077 _reflns_number_gt 3607 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0502P)^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 'refined isotropic' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7077 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.141 _refine_ls_R_factor_gt 0.046 _refine_ls_wR_factor_ref 0.110 _refine_ls_wR_factor_gt 0.089 _refine_ls_goodness_of_fit_ref 0.95 _refine_ls_restrained_S_all 0.95 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.55065(3) 0.39733(3) 0.49104(2) 0.03166(14) Uani 1 1 d . . . Cl1A Cl 0.57668(4) 0.57078(3) 0.17704(3) 0.04124(16) Uani 1 1 d . . . Cl2 Cl 0.59840(4) 0.45954(4) -0.06588(3) 0.04357(17) Uani 1 1 d . . . Cl2A Cl 0.56606(3) 0.57021(4) 0.73519(3) 0.03774(15) Uani 1 1 d . . . C1 C 0.71977(12) 0.27952(11) 0.20937(9) 0.0220(4) Uani 1 1 d . . . C1A C 0.72054(12) 0.72011(11) 0.45845(9) 0.0239(4) Uani 1 1 d . . . C2 C 0.67851(12) 0.30834(11) 0.27992(9) 0.0224(4) Uani 1 1 d . . . C2A C 0.68603(12) 0.68197(11) 0.38795(9) 0.0229(4) Uani 1 1 d . . . C3 C 0.67195(13) 0.39326(12) 0.29619(10) 0.0252(4) Uani 1 1 d . . . C3A C 0.73792(14) 0.64836(12) 0.33278(10) 0.0281(5) Uani 1 1 d . . . C4 C 0.63338(13) 0.42120(13) 0.36101(10) 0.0263(5) Uani 1 1 d . . . C4A C 0.70390(15) 0.61443(12) 0.26817(10) 0.0314(5) Uani 1 1 d . . . C5 C 0.59967(12) 0.36257(12) 0.40970(9) 0.0243(4) Uani 1 1 d . . . C5A C 0.61850(14) 0.61362(12) 0.25863(9) 0.0283(5) Uani 1 1 d . . . C6 C 0.60394(13) 0.27812(12) 0.39467(10) 0.0269(4) Uani 1 1 d . . . C6A C 0.56519(14) 0.64550(13) 0.31258(10) 0.0288(5) Uani 1 1 d . . . C7 C 0.64336(12) 0.25126(13) 0.32999(10) 0.0257(4) Uani 1 1 d . . . C7A C 0.59977(13) 0.67938(12) 0.37717(10) 0.0253(4) Uani 1 1 d . . . C8 C 0.68887(12) 0.32202(11) 0.13997(9) 0.0217(4) Uani 1 1 d . . . C8A C 0.68327(12) 0.68504(11) 0.52881(9) 0.0230(4) Uani 1 1 d . . . C9 C 0.74497(13) 0.34974(11) 0.08583(10) 0.0242(4) Uani 1 1 d . . . C9A C 0.64410(13) 0.73470(13) 0.58207(10) 0.0277(5) Uani 1 1 d . . . C10 C 0.71705(14) 0.39148(12) 0.02243(10) 0.0279(5) Uani 1 1 d . . . C10A C 0.60802(13) 0.70010(13) 0.64544(10) 0.0290(5) Uani 1 1 d . . . C11 C 0.63261(13) 0.40611(12) 0.01357(10) 0.0281(5) Uani 1 1 d . . . C11A C 0.61175(12) 0.61486(12) 0.65575(9) 0.0264(4) Uani 1 1 d . . . C12 C 0.57487(14) 0.37943(13) 0.06598(11) 0.0290(5) Uani 1 1 d . . . C12A C 0.65023(13) 0.56348(13) 0.60391(10) 0.0278(5) Uani 1 1 d . . . C13 C 0.60370(13) 0.33796(12) 0.12940(10) 0.0264(4) Uani 1 1 d . . . C13A C 0.68491(13) 0.59882(12) 0.54052(10) 0.0259(4) Uani 1 1 d . . . H3 H 0.6965(11) 0.4324(10) 0.2627(8) 0.015(4) Uiso 1 1 d . . . H3A H 0.7971(14) 0.6470(12) 0.3409(10) 0.034(6) Uiso 1 1 d . . . H4 H 0.6288(12) 0.4776(12) 0.3723(9) 0.024(5) Uiso 1 1 d . . . H4A H 0.7418(14) 0.5907(11) 0.2328(10) 0.036(5) Uiso 1 1 d . . . H6 H 0.5785(12) 0.2402(13) 0.4260(10) 0.034(6) Uiso 1 1 d . . . H6A H 0.5078(13) 0.6419(11) 0.3070(9) 0.028(5) Uiso 1 1 d . . . H7 H 0.6480(12) 0.1917(13) 0.3204(9) 0.032(5) Uiso 1 1 d . . . H7A H 0.5637(12) 0.7022(12) 0.4145(9) 0.031(5) Uiso 1 1 d . . . H9 H 0.8033(13) 0.3410(11) 0.0912(9) 0.023(5) Uiso 1 1 d . . . H9A H 0.6412(11) 0.7922(12) 0.5750(9) 0.020(5) Uiso 1 1 d . . . H10 H 0.7575(13) 0.4103(11) -0.0128(9) 0.024(5) Uiso 1 1 d . . . H10A H 0.5790(12) 0.7355(12) 0.6810(10) 0.034(5) Uiso 1 1 d . . . H12 H 0.5212(13) 0.3895(11) 0.0588(9) 0.024(5) Uiso 1 1 d . . . H12A H 0.6522(12) 0.5063(12) 0.6120(9) 0.025(5) Uiso 1 1 d . . . H13 H 0.5669(12) 0.3218(11) 0.1653(9) 0.019(5) Uiso 1 1 d . . . H13A H 0.7121(11) 0.5633(11) 0.5049(9) 0.021(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0291(3) 0.0391(3) 0.0267(2) -0.0053(2) 0.0025(2) 0.0048(2) Cl1A 0.0628(4) 0.0370(3) 0.0239(2) -0.0001(2) -0.0044(2) -0.0212(3) Cl2 0.0555(4) 0.0451(4) 0.0302(3) 0.0046(2) -0.0087(2) 0.0188(3) Cl2A 0.0339(3) 0.0527(4) 0.0267(2) 0.0061(2) 0.0033(2) -0.0100(3) C1 0.0215(11) 0.0190(10) 0.0257(9) -0.0005(7) -0.0003(7) -0.0021(8) C1A 0.0250(12) 0.0190(10) 0.0276(9) 0.0000(7) 0.0008(8) 0.0026(8) C2 0.0192(10) 0.0230(11) 0.0250(9) 0.0001(7) -0.0026(7) 0.0026(8) C2A 0.0260(11) 0.0190(10) 0.0236(9) 0.0014(7) 0.0011(8) -0.0030(9) C3 0.0301(12) 0.0219(11) 0.0235(9) 0.0015(8) -0.0008(8) 0.0013(9) C3A 0.0258(13) 0.0246(11) 0.0340(10) -0.0037(8) 0.0053(9) -0.0042(9) C4 0.0303(12) 0.0197(11) 0.0290(10) -0.0023(8) -0.0045(8) 0.0052(9) C4A 0.0388(14) 0.0261(12) 0.0292(10) -0.0037(8) 0.0110(9) -0.0099(10) C5 0.0224(11) 0.0300(11) 0.0207(9) -0.0017(8) -0.0014(7) 0.0039(9) C5A 0.0431(14) 0.0218(11) 0.0201(9) 0.0028(7) -0.0015(9) -0.0114(10) C6 0.0256(12) 0.0250(11) 0.0301(10) 0.0049(8) 0.0035(8) -0.0005(9) C6A 0.0273(13) 0.0293(12) 0.0297(10) 0.0044(8) -0.0044(9) -0.0056(10) C7 0.0247(12) 0.0181(10) 0.0342(10) 0.0015(8) 0.0010(8) 0.0037(9) C7A 0.0260(12) 0.0234(11) 0.0265(10) 0.0014(8) 0.0030(8) -0.0006(9) C8 0.0229(11) 0.0159(9) 0.0261(9) -0.0032(7) -0.0008(8) 0.0018(8) C8A 0.0203(11) 0.0247(11) 0.0240(9) -0.0016(7) -0.0001(7) -0.0012(9) C9 0.0193(12) 0.0202(10) 0.0332(10) -0.0007(8) -0.0019(8) 0.0027(9) C9A 0.0281(12) 0.0219(12) 0.0333(11) -0.0054(8) 0.0010(8) -0.0020(9) C10 0.0338(13) 0.0216(11) 0.0282(10) 0.0011(8) 0.0027(9) 0.0022(9) C10A 0.0261(12) 0.0324(12) 0.0285(10) -0.0082(8) 0.0037(9) -0.0020(10) C11 0.0359(13) 0.0249(11) 0.0236(9) -0.0028(8) -0.0073(9) 0.0051(9) C11A 0.0214(11) 0.0371(12) 0.0207(9) 0.0025(8) -0.0017(8) -0.0075(9) C12 0.0229(12) 0.0323(12) 0.0318(11) -0.0071(8) -0.0048(9) 0.0088(10) C12A 0.0325(13) 0.0238(11) 0.0273(10) 0.0018(8) -0.0037(8) -0.0057(10) C13 0.0256(12) 0.0260(11) 0.0276(10) -0.0035(8) 0.0011(9) 0.0024(9) C13A 0.0312(12) 0.0216(11) 0.0249(9) -0.0043(8) 0.0013(8) 0.0007(9) _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 Cl1 C5 1.7416(17) . ? Cl1A C5A 1.7434(18) . ? Cl2 C11 1.7445(18) . ? Cl2A C11A 1.7479(18) . ? C1 C1 1.347(4) 2_655 ? C1 C2 1.495(2) . ? C1 C8 1.498(2) . ? C1A C1A 1.338(4) 2_665 ? C1A C8A 1.500(2) . ? C1A C2A 1.504(2) . ? C2 C3 1.391(2) . ? C2 C7 1.395(2) . ? C2A C7A 1.388(3) . ? C2A C3A 1.394(3) . ? C3 C4 1.386(3) . ? C3 H3 0.950(16) . ? C3A C4A 1.386(3) . ? C3A H3A 0.95(2) . ? C4 C5 1.387(3) . ? C4 H4 0.926(18) . ? C4A C5A 1.371(3) . ? C4A H4A 0.95(2) . ? C5 C6 1.376(3) . ? C5A C6A 1.382(3) . ? C6 C7 1.384(3) . ? C6 H6 0.918(19) . ? C6A C7A 1.389(3) . ? C6A H6A 0.92(2) . ? C7 H7 0.969(19) . ? C7A H7A 0.953(18) . ? C8 C9 1.390(2) . ? C8 C13 1.393(3) . ? C8A C9A 1.387(3) . ? C8A C13A 1.393(3) . ? C9 C10 1.388(3) . ? C9 H9 0.94(2) . ? C9A C10A 1.385(3) . ? C9A H9A 0.927(18) . ? C10 C11 1.374(3) . ? C10 H10 0.950(18) . ? C10A C11A 1.375(3) . ? C10A H10A 0.968(19) . ? C11 C12 1.380(3) . ? C11A C12A 1.381(3) . ? C12 C13 1.391(3) . ? C12 H12 0.88(2) . ? C12A C13A 1.381(3) . ? C12A H12A 0.924(19) . ? C13 H13 0.907(17) . ? C13A H13A 0.956(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 C1 C2 121.96(9) 2_655 . ? C1 C1 C8 123.49(10) 2_655 . ? C2 C1 C8 114.54(15) . . ? C1A C1A C8A 122.94(10) 2_665 . ? C1A C1A C2A 123.02(9) 2_665 . ? C8A C1A C2A 114.05(15) . . ? C3 C2 C7 118.20(17) . . ? C3 C2 C1 120.63(16) . . ? C7 C2 C1 121.14(16) . . ? C7A C2A C3A 118.48(17) . . ? C7A C2A C1A 119.35(16) . . ? C3A C2A C1A 122.17(18) . . ? C4 C3 C2 121.48(18) . . ? C4 C3 H3 119.9(10) . . ? C2 C3 H3 118.6(10) . . ? C4A C3A C2A 120.6(2) . . ? C4A C3A H3A 120.2(11) . . ? C2A C3A H3A 119.2(11) . . ? C3 C4 C5 118.66(18) . . ? C3 C4 H4 122.0(11) . . ? C5 C4 H4 119.3(11) . . ? C5A C4A C3A 119.68(19) . . ? C5A C4A H4A 122.8(12) . . ? C3A C4A H4A 117.5(12) . . ? C6 C5 C4 121.31(17) . . ? C6 C5 Cl1 119.82(14) . . ? C4 C5 Cl1 118.87(15) . . ? C4A C5A C6A 121.27(18) . . ? C4A C5A Cl1A 119.13(15) . . ? C6A C5A Cl1A 119.59(17) . . ? C5 C6 C7 119.27(18) . . ? C5 C6 H6 120.3(12) . . ? C7 C6 H6 120.3(12) . . ? C5A C6A C7A 118.7(2) . . ? C5A C6A H6A 120.7(11) . . ? C7A C6A H6A 120.5(11) . . ? C6 C7 C2 121.07(19) . . ? C6 C7 H7 119.1(11) . . ? C2 C7 H7 119.8(11) . . ? C2A C7A C6A 121.29(18) . . ? C2A C7A H7A 119.2(11) . . ? C6A C7A H7A 119.5(11) . . ? C9 C8 C13 118.25(16) . . ? C9 C8 C1 120.68(17) . . ? C13 C8 C1 121.01(16) . . ? C9A C8A C13A 118.03(17) . . ? C9A C8A C1A 122.72(17) . . ? C13A C8A C1A 119.20(16) . . ? C10 C9 C8 121.05(19) . . ? C10 C9 H9 118.0(10) . . ? C8 C9 H9 120.9(10) . . ? C10A C9A C8A 121.35(19) . . ? C10A C9A H9A 119.0(11) . . ? C8A C9A H9A 119.6(11) . . ? C11 C10 C9 119.29(19) . . ? C11 C10 H10 122.3(11) . . ? C9 C10 H10 118.4(11) . . ? C11A C10A C9A 119.11(18) . . ? C11A C10A H10A 120.7(11) . . ? C9A C10A H10A 120.2(11) . . ? C10 C11 C12 121.42(18) . . ? C10 C11 Cl2 118.86(16) . . ? C12 C11 Cl2 119.72(16) . . ? C10A C11A C12A 121.14(17) . . ? C10A C11A Cl2A 119.65(15) . . ? C12A C11A Cl2A 119.21(15) . . ? C11 C12 C13 118.7(2) . . ? C11 C12 H12 119.5(12) . . ? C13 C12 H12 121.8(12) . . ? C11A C12A C13A 119.05(19) . . ? C11A C12A H12A 119.8(11) . . ? C13A C12A H12A 121.2(11) . . ? C12 C13 C8 121.26(19) . . ? C12 C13 H13 120.0(11) . . ? C8 C13 H13 118.8(11) . . ? C12A C13A C8A 121.31(18) . . ? C12A C13A H13A 119.0(10) . . ? C8A C13A H13A 119.6(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C1 C2 C3 129.7(2) 2_655 . . . ? C8 C1 C2 C3 -49.8(2) . . . . ? C1 C1 C2 C7 -52.3(3) 2_655 . . . ? C8 C1 C2 C7 128.18(18) . . . . ? C1A C1A C2A C7A -127.8(3) 2_665 . . . ? C8A C1A C2A C7A 52.4(2) . . . . ? C1A C1A C2A C3A 52.6(3) 2_665 . . . ? C8A C1A C2A C3A -127.22(18) . . . . ? C7 C2 C3 C4 1.4(3) . . . . ? C1 C2 C3 C4 179.52(17) . . . . ? C7A C2A C3A C4A 1.0(3) . . . . ? C1A C2A C3A C4A -179.38(17) . . . . ? C2 C3 C4 C5 -1.0(3) . . . . ? C2A C3A C4A C5A -0.3(3) . . . . ? C3 C4 C5 C6 0.0(3) . . . . ? C3 C4 C5 Cl1 -179.69(15) . . . . ? C3A C4A C5A C6A -0.5(3) . . . . ? C3A C4A C5A Cl1A 179.96(15) . . . . ? C4 C5 C6 C7 0.6(3) . . . . ? Cl1 C5 C6 C7 -179.74(15) . . . . ? C4A C5A C6A C7A 0.5(3) . . . . ? Cl1A C5A C6A C7A -179.98(14) . . . . ? C5 C6 C7 C2 -0.2(3) . . . . ? C3 C2 C7 C6 -0.8(3) . . . . ? C1 C2 C7 C6 -178.91(18) . . . . ? C3A C2A C7A C6A -1.1(3) . . . . ? C1A C2A C7A C6A 179.35(17) . . . . ? C5A C6A C7A C2A 0.3(3) . . . . ? C1 C1 C8 C9 -43.8(3) 2_655 . . . ? C2 C1 C8 C9 135.76(17) . . . . ? C1 C1 C8 C13 139.0(2) 2_655 . . . ? C2 C1 C8 C13 -41.5(2) . . . . ? C1A C1A C8A C9A 56.8(3) 2_665 . . . ? C2A C1A C8A C9A -123.34(19) . . . . ? C1A C1A C8A C13A -125.6(3) 2_665 . . . ? C2A C1A C8A C13A 54.2(2) . . . . ? C13 C8 C9 C10 -0.7(3) . . . . ? C1 C8 C9 C10 -178.00(16) . . . . ? C13A C8A C9A C10A 0.4(3) . . . . ? C1A C8A C9A C10A 178.01(18) . . . . ? C8 C9 C10 C11 0.5(3) . . . . ? C8A C9A C10A C11A 0.4(3) . . . . ? C9 C10 C11 C12 -0.7(3) . . . . ? C9 C10 C11 Cl2 179.36(14) . . . . ? C9A C10A C11A C12A -0.4(3) . . . . ? C9A C10A C11A Cl2A -179.68(15) . . . . ? C10 C11 C12 C13 0.9(3) . . . . ? Cl2 C11 C12 C13 -179.12(15) . . . . ? C10A C11A C12A C13A -0.4(3) . . . . ? Cl2A C11A C12A C13A 178.82(15) . . . . ? C11 C12 C13 C8 -1.0(3) . . . . ? C9 C8 C13 C12 0.9(3) . . . . ? C1 C8 C13 C12 178.25(17) . . . . ? C11A C12A C13A C8A 1.3(3) . . . . ? C9A C8A C13A C12A -1.3(3) . . . . ? C1A C8A C13A C12A -178.99(18) . . . . ? _diffrn_measured_fraction_theta_max 0.855 _diffrn_reflns_theta_full 32.56 _diffrn_measured_fraction_theta_full 0.855 _refine_diff_density_max 0.472 _refine_diff_density_min -0.347 _refine_diff_density_rms 0.071 #=== data_753tj4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetra-(4-jodophenyl)ethene (5) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H16 I4' _chemical_formula_weight 835.99 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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.648(1) _cell_length_b 16.605(7) _cell_length_c 15.810(6) _cell_angle_alpha 90.0 _cell_angle_beta 97.61(2) _cell_angle_gamma 90.0 _cell_volume 2511(1) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.1 _cell_measurement_theta_max 22.1 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.212 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 4.976 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.198 _exptl_absorpt_correction_T_max 0.495 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type NONIUS_CAD4 _diffrn_measurement_method \w2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% -3 _diffrn_reflns_number 6370 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0230 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 27.97 _reflns_number_total 6027 _reflns_number_gt 4936 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0658P)^2^+3.9785P] 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 6027 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.053 _refine_ls_R_factor_gt 0.038 _refine_ls_wR_factor_ref 0.103 _refine_ls_wR_factor_gt 0.097 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 1.28177(3) 0.36940(2) 0.352837(19) 0.03656(10) Uani 1 1 d . . . I2 I 0.57239(5) 0.47368(2) -0.19918(2) 0.05038(13) Uani 1 1 d . . . I3 I 0.63863(3) 0.10671(2) 0.560912(17) 0.03284(9) Uani 1 1 d . . . I4 I 0.16062(4) 0.02107(2) -0.08063(2) 0.04160(10) Uani 1 1 d . . . C1 C 0.6056(4) 0.2180(3) 0.1731(3) 0.0240(8) Uani 1 1 d . . . C2 C 0.6903(4) 0.2751(3) 0.1466(3) 0.0245(8) Uani 1 1 d . . . C3 C 0.8247(4) 0.2979(2) 0.1982(2) 0.0216(7) Uani 1 1 d . . . C4 C 0.9244(5) 0.2392(3) 0.2251(3) 0.0293(9) Uani 1 1 d . . . H4 H 0.9030 0.1842 0.2134 0.035 Uiso 1 1 calc R . . C5 C 1.0538(5) 0.2593(3) 0.2684(3) 0.0311(9) Uani 1 1 d . . . H5 H 1.1204 0.2185 0.2861 0.037 Uiso 1 1 calc R . . C6 C 1.0852(4) 0.3394(3) 0.2858(2) 0.0242(8) Uani 1 1 d . . . C7 C 0.9895(5) 0.3991(3) 0.2608(3) 0.0274(8) Uani 1 1 d . . . H7 H 1.0113 0.4539 0.2738 0.033 Uiso 1 1 calc R . . C8 C 0.8601(5) 0.3781(3) 0.2163(3) 0.0253(8) Uani 1 1 d . . . H8 H 0.7946 0.4193 0.1978 0.030 Uiso 1 1 calc R . . C9 C 0.6601(4) 0.3171(3) 0.0636(3) 0.0237(8) Uani 1 1 d . . . C10 C 0.5295(5) 0.3525(3) 0.0391(3) 0.0335(10) Uani 1 1 d . . . H10 H 0.4573 0.3462 0.0740 0.040 Uiso 1 1 calc R . . C11 C 0.5044(5) 0.3967(3) -0.0358(3) 0.0371(11) Uani 1 1 d . . . H11 H 0.4158 0.4213 -0.0516 0.045 Uiso 1 1 calc R . . C12 C 0.6081(5) 0.4048(3) -0.0872(3) 0.0312(10) Uani 1 1 d . . . C13 C 0.7381(5) 0.3700(3) -0.0649(3) 0.0323(10) Uani 1 1 d . . . H13 H 0.8092 0.3759 -0.1006 0.039 Uiso 1 1 calc R . . C14 C 0.7628(4) 0.3264(3) 0.0101(3) 0.0285(9) Uani 1 1 d . . . H14 H 0.8519 0.3023 0.0255 0.034 Uiso 1 1 calc R . . C15 C 0.6188(4) 0.1916(3) 0.2643(3) 0.0239(8) Uani 1 1 d . . . C16 C 0.6160(5) 0.1097(3) 0.2854(3) 0.0295(9) Uani 1 1 d . . . H16 H 0.6100 0.0704 0.2414 0.035 Uiso 1 1 calc R . . C17 C 0.6220(5) 0.0853(3) 0.3699(3) 0.0308(9) Uani 1 1 d . . . H17 H 0.6205 0.0296 0.3837 0.037 Uiso 1 1 calc R . . C18 C 0.6302(4) 0.1426(3) 0.4337(3) 0.0252(8) Uani 1 1 d . . . C19 C 0.6330(5) 0.2236(3) 0.4141(3) 0.0319(9) Uani 1 1 d . . . H19 H 0.6380 0.2628 0.4582 0.038 Uiso 1 1 calc R . . C20 C 0.6283(5) 0.2470(3) 0.3298(3) 0.0296(9) Uani 1 1 d . . . H20 H 0.6317 0.3028 0.3167 0.035 Uiso 1 1 calc R . . C21 C 0.4969(4) 0.1756(3) 0.1141(3) 0.0248(8) Uani 1 1 d . . . C22 C 0.3632(5) 0.1592(3) 0.1347(3) 0.0349(10) Uani 1 1 d . . . H22 H 0.3386 0.1783 0.1874 0.042 Uiso 1 1 calc R . . C23 C 0.2658(5) 0.1162(4) 0.0808(3) 0.0371(11) Uani 1 1 d . . . H23 H 0.1751 0.1066 0.0957 0.044 Uiso 1 1 calc R . . C24 C 0.3026(5) 0.0873(3) 0.0042(3) 0.0299(9) Uani 1 1 d . . . C25 C 0.4343(5) 0.1013(3) -0.0172(3) 0.0332(10) Uani 1 1 d . . . H25 H 0.4593 0.0808 -0.0691 0.040 Uiso 1 1 calc R . . C26 C 0.5314(5) 0.1458(3) 0.0376(3) 0.0308(9) Uani 1 1 d . . . H26 H 0.6217 0.1557 0.0222 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.02766(15) 0.0464(2) 0.03269(16) 0.01073(13) -0.00667(12) -0.00876(13) I2 0.0863(3) 0.03256(18) 0.02511(16) 0.00938(12) -0.01933(17) -0.01911(17) I3 0.02887(15) 0.04727(19) 0.02198(14) 0.00954(11) 0.00189(11) 0.00286(12) I4 0.03794(18) 0.0454(2) 0.03635(18) 0.00555(13) -0.01394(14) -0.01172(14) C1 0.0250(19) 0.025(2) 0.0220(18) 0.0036(15) 0.0030(15) 0.0002(16) C2 0.0230(18) 0.025(2) 0.0251(19) 0.0016(15) 0.0021(15) 0.0008(16) C3 0.0225(18) 0.0237(19) 0.0182(16) 0.0048(14) 0.0016(14) 0.0026(15) C4 0.028(2) 0.021(2) 0.037(2) 0.0040(17) -0.0012(17) 0.0017(17) C5 0.029(2) 0.027(2) 0.035(2) 0.0091(18) -0.0039(18) 0.0060(18) C6 0.0216(18) 0.030(2) 0.0195(17) 0.0054(15) -0.0025(14) -0.0025(16) C7 0.032(2) 0.025(2) 0.0231(19) 0.0007(16) -0.0020(16) -0.0002(17) C8 0.028(2) 0.0218(19) 0.0250(19) 0.0027(15) -0.0005(16) 0.0041(16) C9 0.0213(18) 0.025(2) 0.0237(18) 0.0052(15) -0.0009(15) -0.0034(15) C10 0.024(2) 0.036(3) 0.041(2) 0.015(2) 0.0045(18) 0.0004(18) C11 0.029(2) 0.035(3) 0.044(3) 0.012(2) -0.009(2) 0.0005(19) C12 0.040(2) 0.028(2) 0.0221(19) 0.0080(16) -0.0106(17) -0.0130(19) C13 0.029(2) 0.044(3) 0.023(2) 0.0053(18) 0.0010(17) -0.0104(19) C14 0.0201(18) 0.040(3) 0.0237(19) 0.0043(18) -0.0023(15) -0.0040(17) C15 0.0253(19) 0.027(2) 0.0191(17) 0.0023(15) 0.0033(14) -0.0022(16) C16 0.040(2) 0.024(2) 0.0234(19) -0.0017(16) 0.0025(18) -0.0075(18) C17 0.042(2) 0.022(2) 0.029(2) 0.0037(17) 0.0065(18) -0.0051(18) C18 0.0221(18) 0.032(2) 0.0215(18) 0.0048(16) 0.0025(15) -0.0008(16) C19 0.046(3) 0.028(2) 0.023(2) -0.0036(17) 0.0082(18) -0.0005(19) C20 0.042(2) 0.021(2) 0.026(2) 0.0012(16) 0.0083(18) 0.0020(18) C21 0.0220(18) 0.029(2) 0.0228(18) 0.0052(16) -0.0002(15) 0.0007(16) C22 0.031(2) 0.050(3) 0.024(2) 0.000(2) 0.0087(17) -0.005(2) C23 0.025(2) 0.055(3) 0.030(2) 0.004(2) 0.0022(18) -0.009(2) C24 0.027(2) 0.035(2) 0.025(2) 0.0076(17) -0.0068(16) -0.0047(18) C25 0.033(2) 0.041(3) 0.026(2) -0.0040(18) 0.0026(18) -0.008(2) C26 0.027(2) 0.036(2) 0.030(2) 0.0012(18) 0.0071(17) -0.0092(18) _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 I1 C6 2.107(4) . ? I2 C12 2.097(4) . ? I3 C18 2.089(4) . ? I4 C24 2.097(5) . ? C1 C2 1.354(6) . ? C1 C21 1.486(6) . ? C1 C15 1.497(5) . ? C2 C9 1.481(6) . ? C2 C3 1.486(6) . ? C3 C4 1.395(6) . ? C3 C8 1.396(6) . ? C4 C5 1.382(6) . ? C4 H4 0.9500 . ? C5 C6 1.383(7) . ? C5 H5 0.9500 . ? C6 C7 1.377(6) . ? C7 C8 1.394(6) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C14 1.395(6) . ? C9 C10 1.398(6) . ? C10 C11 1.386(7) . ? C10 H10 0.9500 . ? C11 C12 1.377(7) . ? C11 H11 0.9500 . ? C12 C13 1.384(7) . ? C13 C14 1.382(6) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C20 1.380(6) . ? C15 C16 1.400(6) . ? C16 C17 1.391(6) . ? C16 H16 0.9500 . ? C17 C18 1.381(6) . ? C17 H17 0.9500 . ? C18 C19 1.381(6) . ? C19 C20 1.383(6) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C26 1.387(6) . ? C21 C22 1.398(6) . ? C22 C23 1.381(7) . ? C22 H22 0.9500 . ? C23 C24 1.391(7) . ? C23 H23 0.9500 . ? C24 C25 1.378(6) . ? C25 C26 1.399(6) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C21 122.9(4) . . ? C2 C1 C15 121.7(4) . . ? C21 C1 C15 115.4(3) . . ? C1 C2 C9 123.2(4) . . ? C1 C2 C3 121.8(4) . . ? C9 C2 C3 114.9(3) . . ? C4 C3 C8 117.6(4) . . ? C4 C3 C2 120.4(4) . . ? C8 C3 C2 121.8(4) . . ? C5 C4 C3 121.6(4) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C4 C5 C6 119.4(4) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C7 C6 C5 121.0(4) . . ? C7 C6 I1 119.9(3) . . ? C5 C6 I1 119.1(3) . . ? C6 C7 C8 119.1(4) . . ? C6 C7 H7 120.5 . . ? C8 C7 H7 120.5 . . ? C7 C8 C3 121.4(4) . . ? C7 C8 H8 119.3 . . ? C3 C8 H8 119.3 . . ? C14 C9 C10 118.2(4) . . ? C14 C9 C2 121.2(4) . . ? C10 C9 C2 120.6(4) . . ? C11 C10 C9 120.6(4) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C12 C11 C10 119.8(4) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 120.9(4) . . ? C11 C12 I2 120.1(4) . . ? C13 C12 I2 119.0(3) . . ? C14 C13 C12 119.0(4) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? C13 C14 C9 121.5(4) . . ? C13 C14 H14 119.2 . . ? C9 C14 H14 119.2 . . ? C20 C15 C16 118.1(4) . . ? C20 C15 C1 121.1(4) . . ? C16 C15 C1 120.7(4) . . ? C17 C16 C15 120.8(4) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C18 C17 C16 119.4(4) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C17 C18 C19 120.6(4) . . ? C17 C18 I3 119.8(3) . . ? C19 C18 I3 119.6(3) . . ? C18 C19 C20 119.3(4) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? C15 C20 C19 121.7(4) . . ? C15 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? C26 C21 C22 118.0(4) . . ? C26 C21 C1 119.1(4) . . ? C22 C21 C1 122.8(4) . . ? C23 C22 C21 121.9(4) . . ? C23 C22 H22 119.0 . . ? C21 C22 H22 119.0 . . ? C22 C23 C24 119.0(4) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C25 C24 C23 120.3(4) . . ? C25 C24 I4 118.5(3) . . ? C23 C24 I4 121.2(3) . . ? C24 C25 C26 120.1(4) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C21 C26 C25 120.6(4) . . ? C21 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 C1 C2 C9 17.5(7) . . . . ? C15 C1 C2 C9 -164.5(4) . . . . ? C21 C1 C2 C3 -160.1(4) . . . . ? C15 C1 C2 C3 18.0(6) . . . . ? C1 C2 C3 C4 54.2(6) . . . . ? C9 C2 C3 C4 -123.6(4) . . . . ? C1 C2 C3 C8 -130.5(5) . . . . ? C9 C2 C3 C8 51.7(5) . . . . ? C8 C3 C4 C5 0.2(6) . . . . ? C2 C3 C4 C5 175.8(4) . . . . ? C3 C4 C5 C6 0.2(7) . . . . ? C4 C5 C6 C7 0.2(7) . . . . ? C4 C5 C6 I1 179.4(3) . . . . ? C5 C6 C7 C8 -1.0(6) . . . . ? I1 C6 C7 C8 179.8(3) . . . . ? C6 C7 C8 C3 1.4(6) . . . . ? C4 C3 C8 C7 -1.0(6) . . . . ? C2 C3 C8 C7 -176.5(4) . . . . ? C1 C2 C9 C14 -133.0(5) . . . . ? C3 C2 C9 C14 44.7(6) . . . . ? C1 C2 C9 C10 50.5(6) . . . . ? C3 C2 C9 C10 -131.7(4) . . . . ? C14 C9 C10 C11 -1.1(7) . . . . ? C2 C9 C10 C11 175.4(5) . . . . ? C9 C10 C11 C12 1.0(8) . . . . ? C10 C11 C12 C13 -0.5(8) . . . . ? C10 C11 C12 I2 -178.7(4) . . . . ? C11 C12 C13 C14 0.1(7) . . . . ? I2 C12 C13 C14 178.2(4) . . . . ? C12 C13 C14 C9 -0.1(7) . . . . ? C10 C9 C14 C13 0.6(7) . . . . ? C2 C9 C14 C13 -175.9(4) . . . . ? C2 C1 C15 C20 47.8(6) . . . . ? C21 C1 C15 C20 -134.0(4) . . . . ? C2 C1 C15 C16 -134.8(5) . . . . ? C21 C1 C15 C16 43.4(6) . . . . ? C20 C15 C16 C17 0.3(7) . . . . ? C1 C15 C16 C17 -177.1(4) . . . . ? C15 C16 C17 C18 0.3(7) . . . . ? C16 C17 C18 C19 -0.2(7) . . . . ? C16 C17 C18 I3 179.8(3) . . . . ? C17 C18 C19 C20 -0.4(7) . . . . ? I3 C18 C19 C20 179.6(4) . . . . ? C16 C15 C20 C19 -1.0(7) . . . . ? C1 C15 C20 C19 176.5(4) . . . . ? C18 C19 C20 C15 1.0(8) . . . . ? C2 C1 C21 C26 46.2(6) . . . . ? C15 C1 C21 C26 -132.0(4) . . . . ? C2 C1 C21 C22 -138.3(5) . . . . ? C15 C1 C21 C22 43.5(6) . . . . ? C26 C21 C22 C23 -1.3(8) . . . . ? C1 C21 C22 C23 -176.7(5) . . . . ? C21 C22 C23 C24 1.0(8) . . . . ? C22 C23 C24 C25 0.1(8) . . . . ? C22 C23 C24 I4 179.7(4) . . . . ? C23 C24 C25 C26 -0.9(8) . . . . ? I4 C24 C25 C26 179.5(4) . . . . ? C22 C21 C26 C25 0.4(7) . . . . ? C1 C21 C26 C25 176.1(4) . . . . ? C24 C25 C26 C21 0.6(8) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.97 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.68 _refine_diff_density_min -0.19 _refine_diff_density_rms 0.188 #=== data_732todac _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetra-(4-chlorophenyl)ethene p-xylene inclusion compound (3.pXy) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H26 Cl4' _chemical_formula_weight 576.35 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 8.635(2) _cell_length_b 14.707(4) _cell_length_c 22.891(12) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 2907.0(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.2 _cell_measurement_theta_max 15.9 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 0.429 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.847 _exptl_absorpt_correction_T_max 0.958 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type NONIUS_CAD4 _diffrn_measurement_method \w2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 2 _diffrn_reflns_number 3951 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI 0.057 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 28.00 _reflns_number_total 3951 _reflns_number_gt 2636 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+0.3827P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(7) _refine_ls_number_reflns 3951 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.094 _refine_ls_R_factor_gt 0.034 _refine_ls_wR_factor_ref 0.084 _refine_ls_wR_factor_gt 0.071 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl -0.75573(15) 0.11577(7) -0.56805(4) 0.0700(4) Uani 1 1 d . . . Cl2 Cl -0.69315(11) 0.15303(6) -0.12672(3) 0.0465(2) Uani 1 1 d . . . Cl3 Cl -0.79145(11) -0.41743(6) -0.54577(3) 0.0437(2) Uani 1 1 d . . . Cl4 Cl -0.79225(14) -0.38078(6) -0.11147(3) 0.0514(3) Uani 1 1 d . . . C1 C -0.7657(3) -0.17331(18) -0.33653(11) 0.0230(6) Uani 1 1 d . . . C2 C -0.7550(3) -0.08210(19) -0.33937(11) 0.0236(6) Uani 1 1 d . . . C3 C -0.7585(4) -0.03216(18) -0.39634(11) 0.0267(7) Uani 1 1 d . . . C4 C -0.8767(4) -0.0449(2) -0.43609(13) 0.0315(7) Uani 1 1 d . . . C5 C -0.8769(4) -0.0002(2) -0.48917(13) 0.0385(8) Uani 1 1 d . . . C6 C -0.7581(5) 0.0590(2) -0.50147(12) 0.0401(9) Uani 1 1 d . . . C7 C -0.6410(4) 0.0748(2) -0.46240(14) 0.0385(8) Uani 1 1 d . . . C8 C -0.6417(4) 0.0297(2) -0.40943(13) 0.0315(7) Uani 1 1 d . . . C9 C -0.7371(3) -0.02330(18) -0.28705(11) 0.0239(6) Uani 1 1 d . . . C10 C -0.6285(4) -0.0426(2) -0.24371(12) 0.0266(6) Uani 1 1 d . . . C11 C -0.6142(4) 0.0114(2) -0.19498(13) 0.0302(7) Uani 1 1 d . . . C12 C -0.7116(4) 0.0849(2) -0.18874(11) 0.0283(6) Uani 1 1 d . . . C13 C -0.8177(4) 0.10756(19) -0.23106(12) 0.0302(7) Uani 1 1 d . . . C14 C -0.8284(4) 0.05368(19) -0.28056(13) 0.0281(7) Uani 1 1 d . . . C15 C -0.7701(4) -0.23252(17) -0.38921(11) 0.0231(6) Uani 1 1 d . . . C16 C -0.8901(4) -0.2951(2) -0.39552(13) 0.0286(7) Uani 1 1 d . . . C17 C -0.8986(4) -0.3517(2) -0.44351(13) 0.0296(7) Uani 1 1 d . . . C18 C -0.7838(4) -0.34673(18) -0.48508(12) 0.0295(7) Uani 1 1 d . . . C19 C -0.6616(4) -0.2867(2) -0.47977(13) 0.0338(8) Uani 1 1 d . . . C20 C -0.6570(4) -0.2294(2) -0.43176(14) 0.0310(7) Uani 1 1 d . . . C21 C -0.7744(4) -0.22474(17) -0.28036(12) 0.0233(6) Uani 1 1 d . . . C22 C -0.6829(4) -0.30090(19) -0.27204(12) 0.0282(7) Uani 1 1 d . . . C23 C -0.6856(4) -0.3485(2) -0.22000(13) 0.0314(7) Uani 1 1 d . . . C24 C -0.7851(4) -0.32082(19) -0.17668(11) 0.0303(7) Uani 1 1 d . . . C25 C -0.8821(4) -0.2469(2) -0.18422(12) 0.0300(7) Uani 1 1 d . . . C26 C -0.8752(4) -0.1994(2) -0.23602(13) 0.0273(7) Uani 1 1 d . . . C27 C -0.7731(4) -0.3532(2) 0.10863(14) 0.0425(9) Uani 1 1 d . . . C28 C -0.7005(5) -0.4289(2) 0.13050(16) 0.0485(9) Uani 1 1 d . . . C29 C -0.6904(5) -0.4440(2) 0.18982(17) 0.0461(9) Uani 1 1 d . . . C30 C -0.7499(4) -0.3825(2) 0.22955(14) 0.0367(8) Uani 1 1 d . . . C31 C -0.8234(4) -0.3070(2) 0.20735(15) 0.0386(8) Uani 1 1 d . . . C32 C -0.8356(5) -0.2921(2) 0.14801(16) 0.0435(9) Uani 1 1 d . . . C33 C -0.7861(7) -0.3363(3) 0.04364(16) 0.0763(14) Uani 1 1 d . . . H33A H -0.7545 -0.3910 0.0223 0.114 Uiso 1 1 calc R . . H33B H -0.7186 -0.2855 0.0327 0.114 Uiso 1 1 calc R . . H33C H -0.8936 -0.3213 0.0338 0.114 Uiso 1 1 calc R . . C34 C -0.7358(5) -0.3967(3) 0.29442(15) 0.0575(11) Uani 1 1 d . . . H34A H -0.8367 -0.4145 0.3104 0.086 Uiso 1 1 calc R . . H34B H -0.7014 -0.3402 0.3130 0.086 Uiso 1 1 calc R . . H34C H -0.6601 -0.4449 0.3022 0.086 Uiso 1 1 calc R . . H4 H -0.957(4) -0.089(2) -0.4286(13) 0.036(9) Uiso 1 1 d . . . H5 H -0.961(4) -0.008(2) -0.5162(15) 0.049(10) Uiso 1 1 d . . . H7 H -0.563(4) 0.117(2) -0.4740(14) 0.045(10) Uiso 1 1 d . . . H8 H -0.557(4) 0.0389(19) -0.3833(13) 0.033(9) Uiso 1 1 d . . . H10 H -0.566(3) -0.0963(19) -0.2485(11) 0.019(7) Uiso 1 1 d . . . H11 H -0.533(4) -0.002(2) -0.1663(14) 0.047(10) Uiso 1 1 d . . . H13 H -0.886(3) 0.160(2) -0.2246(13) 0.033(9) Uiso 1 1 d . . . H14 H -0.901(3) 0.067(2) -0.3099(12) 0.032(9) Uiso 1 1 d . . . H16 H -0.967(3) -0.2960(17) -0.3675(11) 0.016(7) Uiso 1 1 d . . . H17 H -0.976(4) -0.392(2) -0.4469(14) 0.039(9) Uiso 1 1 d . . . H19 H -0.577(4) -0.283(2) -0.5093(15) 0.049(10) Uiso 1 1 d . . . H20 H -0.576(4) -0.190(2) -0.4301(14) 0.042(10) Uiso 1 1 d . . . H22 H -0.611(3) -0.319(2) -0.3033(13) 0.032(8) Uiso 1 1 d . . . H23 H -0.624(4) -0.399(2) -0.2153(13) 0.036(9) Uiso 1 1 d . . . H25 H -0.955(4) -0.228(2) -0.1561(14) 0.040(10) Uiso 1 1 d . . . H26 H -0.942(3) -0.1492(19) -0.2371(12) 0.026(8) Uiso 1 1 d . . . H28 H -0.655(4) -0.476(2) 0.1047(15) 0.056(11) Uiso 1 1 d . . . H29 H -0.646(4) -0.495(2) 0.2039(15) 0.046(11) Uiso 1 1 d . . . H31 H -0.870(4) -0.268(2) 0.2316(16) 0.054(11) Uiso 1 1 d . . . H32 H -0.883(4) -0.239(2) 0.1349(14) 0.037(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.1064(10) 0.0709(6) 0.0326(4) 0.0239(4) -0.0054(5) -0.0198(7) Cl2 0.0463(5) 0.0558(5) 0.0373(4) -0.0199(4) -0.0015(4) 0.0001(5) Cl3 0.0411(5) 0.0472(4) 0.0428(4) -0.0227(4) -0.0020(4) 0.0038(4) Cl4 0.0830(7) 0.0448(4) 0.0264(3) 0.0129(3) 0.0017(5) 0.0043(5) C1 0.0204(15) 0.0269(14) 0.0217(13) 0.0019(11) 0.0027(12) 0.0025(12) C2 0.0193(15) 0.0244(13) 0.0270(13) -0.0001(11) 0.0016(12) 0.0037(12) C3 0.0332(19) 0.0236(13) 0.0233(13) -0.0014(11) 0.0023(13) 0.0032(13) C4 0.0329(18) 0.0276(15) 0.0340(16) 0.0044(13) -0.0007(15) -0.0026(15) C5 0.048(2) 0.0392(18) 0.0287(16) 0.0043(14) -0.0089(17) -0.0032(17) C6 0.061(3) 0.0349(17) 0.0241(13) 0.0081(12) 0.0028(17) -0.0008(18) C7 0.049(2) 0.0318(17) 0.0346(16) 0.0069(14) 0.0079(17) -0.0084(17) C8 0.0340(19) 0.0313(16) 0.0291(15) 0.0007(13) 0.0009(15) -0.0064(15) C9 0.0251(16) 0.0203(13) 0.0261(13) 0.0028(10) 0.0014(13) -0.0006(12) C10 0.0231(16) 0.0248(14) 0.0320(15) -0.0002(12) 0.0003(13) 0.0034(13) C11 0.0252(16) 0.0380(17) 0.0276(15) 0.0009(13) -0.0033(14) -0.0021(15) C12 0.0300(16) 0.0323(14) 0.0225(12) -0.0041(12) 0.0035(14) -0.0018(15) C13 0.0308(18) 0.0245(14) 0.0354(15) -0.0026(12) 0.0042(15) 0.0018(14) C14 0.0308(18) 0.0268(15) 0.0267(13) 0.0027(11) -0.0005(14) 0.0042(13) C15 0.0260(17) 0.0208(13) 0.0225(12) 0.0023(10) 0.0013(13) 0.0027(12) C16 0.0289(17) 0.0293(15) 0.0276(14) 0.0033(12) 0.0064(14) 0.0007(14) C17 0.0276(17) 0.0248(15) 0.0364(16) -0.0009(13) -0.0024(15) -0.0029(14) C18 0.0350(18) 0.0241(13) 0.0296(14) -0.0073(11) -0.0025(15) 0.0055(15) C19 0.034(2) 0.0351(17) 0.0320(15) -0.0053(13) 0.0121(15) -0.0021(15) C20 0.0296(19) 0.0272(15) 0.0363(16) -0.0048(13) 0.0056(15) -0.0037(14) C21 0.0264(16) 0.0203(13) 0.0232(12) -0.0003(10) 0.0009(13) -0.0020(13) C22 0.0331(18) 0.0252(14) 0.0263(13) -0.0023(11) 0.0018(15) 0.0040(14) C23 0.0376(19) 0.0247(14) 0.0317(15) 0.0025(12) -0.0015(16) 0.0038(16) C24 0.0419(19) 0.0274(14) 0.0215(12) 0.0047(11) -0.0050(15) -0.0086(16) C25 0.0330(18) 0.0314(16) 0.0255(14) -0.0017(13) 0.0032(14) -0.0047(15) C26 0.0260(16) 0.0246(14) 0.0314(15) -0.0018(12) -0.0001(13) 0.0006(14) C27 0.052(2) 0.0399(18) 0.0359(16) -0.0043(14) 0.0061(17) -0.0117(19) C28 0.049(2) 0.0414(19) 0.055(2) -0.0151(17) 0.009(2) -0.003(2) C29 0.039(2) 0.0357(18) 0.063(2) 0.0014(17) -0.007(2) 0.0020(18) C30 0.0269(18) 0.0411(18) 0.0421(17) 0.0020(15) -0.0003(15) -0.0122(15) C31 0.035(2) 0.0347(18) 0.0459(19) -0.0073(15) 0.0083(18) -0.0042(17) C32 0.047(2) 0.0350(18) 0.049(2) 0.0054(16) 0.0053(18) 0.0005(18) C33 0.110(4) 0.078(3) 0.041(2) 0.0002(19) 0.007(3) -0.003(3) C34 0.054(3) 0.071(3) 0.047(2) 0.0093(18) -0.0075(19) -0.021(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 Cl1 C6 1.738(3) . ? Cl2 C12 1.745(3) . ? Cl3 C18 1.737(3) . ? Cl4 C24 1.735(3) . ? C1 C2 1.346(4) . ? C1 C15 1.488(4) . ? C1 C21 1.494(4) . ? C2 C9 1.485(4) . ? C2 C3 1.497(4) . ? C3 C4 1.380(4) . ? C3 C8 1.391(4) . ? C4 C5 1.381(4) . ? C4 H4 0.96(3) . ? C5 C6 1.375(5) . ? C5 H5 0.96(4) . ? C6 C7 1.370(5) . ? C7 C8 1.382(4) . ? C7 H7 0.95(3) . ? C8 H8 0.95(3) . ? C9 C14 1.388(4) . ? C9 C10 1.395(4) . ? C10 C11 1.375(4) . ? C10 H10 0.96(3) . ? C11 C12 1.377(4) . ? C11 H11 0.98(4) . ? C12 C13 1.375(4) . ? C13 C14 1.386(4) . ? C13 H13 0.98(3) . ? C14 H14 0.93(3) . ? C15 C20 1.380(4) . ? C15 C16 1.393(4) . ? C16 C17 1.381(4) . ? C16 H16 0.92(3) . ? C17 C18 1.376(4) . ? C17 H17 0.90(3) . ? C18 C19 1.381(4) . ? C19 C20 1.386(4) . ? C19 H19 1.00(4) . ? C20 H20 0.91(3) . ? C21 C22 1.384(4) . ? C21 C26 1.388(4) . ? C22 C23 1.382(4) . ? C22 H22 0.98(3) . ? C23 C24 1.373(4) . ? C23 H23 0.92(3) . ? C24 C25 1.384(4) . ? C25 C26 1.378(4) . ? C25 H25 0.94(3) . ? C26 H26 0.94(3) . ? C27 C28 1.372(5) . ? C27 C32 1.382(5) . ? C27 C33 1.513(5) . ? C28 C29 1.379(5) . ? C28 H28 1.00(4) . ? C29 C30 1.382(5) . ? C29 H29 0.90(3) . ? C30 C31 1.376(5) . ? C30 C34 1.505(5) . ? C31 C32 1.380(5) . ? C31 H31 0.89(4) . ? C32 H32 0.93(3) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C15 123.1(2) . . ? C2 C1 C21 123.3(2) . . ? C15 C1 C21 113.6(2) . . ? C1 C2 C9 123.3(2) . . ? C1 C2 C3 122.0(2) . . ? C9 C2 C3 114.8(2) . . ? C4 C3 C8 118.9(3) . . ? C4 C3 C2 121.5(3) . . ? C8 C3 C2 119.6(3) . . ? C3 C4 C5 121.1(3) . . ? C3 C4 H4 120.5(18) . . ? C5 C4 H4 118.3(18) . . ? C6 C5 C4 118.7(3) . . ? C6 C5 H5 121(2) . . ? C4 C5 H5 121(2) . . ? C7 C6 C5 121.6(3) . . ? C7 C6 Cl1 118.8(3) . . ? C5 C6 Cl1 119.5(3) . . ? C6 C7 C8 119.2(3) . . ? C6 C7 H7 117(2) . . ? C8 C7 H7 124(2) . . ? C7 C8 C3 120.4(3) . . ? C7 C8 H8 118.6(18) . . ? C3 C8 H8 120.9(18) . . ? C14 C9 C10 118.2(3) . . ? C14 C9 C2 120.2(2) . . ? C10 C9 C2 121.7(3) . . ? C11 C10 C9 121.3(3) . . ? C11 C10 H10 121.0(16) . . ? C9 C10 H10 117.7(16) . . ? C10 C11 C12 118.9(3) . . ? C10 C11 H11 119.2(19) . . ? C12 C11 H11 121.9(19) . . ? C13 C12 C11 121.6(3) . . ? C13 C12 Cl2 119.7(2) . . ? C11 C12 Cl2 118.7(2) . . ? C12 C13 C14 118.8(3) . . ? C12 C13 H13 119.0(18) . . ? C14 C13 H13 122.1(18) . . ? C13 C14 C9 121.1(3) . . ? C13 C14 H14 121.0(18) . . ? C9 C14 H14 117.9(18) . . ? C20 C15 C16 118.4(3) . . ? C20 C15 C1 122.3(3) . . ? C16 C15 C1 119.3(3) . . ? C17 C16 C15 121.4(3) . . ? C17 C16 H16 120.4(16) . . ? C15 C16 H16 118.2(16) . . ? C18 C17 C16 118.7(3) . . ? C18 C17 H17 121(2) . . ? C16 C17 H17 120(2) . . ? C17 C18 C19 121.6(3) . . ? C17 C18 Cl3 119.6(2) . . ? C19 C18 Cl3 118.8(2) . . ? C18 C19 C20 118.7(3) . . ? C18 C19 H19 122.2(19) . . ? C20 C19 H19 119.1(19) . . ? C15 C20 C19 121.3(3) . . ? C15 C20 H20 122(2) . . ? C19 C20 H20 116(2) . . ? C22 C21 C26 118.4(3) . . ? C22 C21 C1 120.0(3) . . ? C26 C21 C1 121.7(3) . . ? C23 C22 C21 121.3(3) . . ? C23 C22 H22 120.3(17) . . ? C21 C22 H22 118.4(17) . . ? C24 C23 C22 118.8(3) . . ? C24 C23 H23 121(2) . . ? C22 C23 H23 120(2) . . ? C23 C24 C25 121.5(3) . . ? C23 C24 Cl4 119.5(2) . . ? C25 C24 Cl4 119.0(2) . . ? C26 C25 C24 118.7(3) . . ? C26 C25 H25 118(2) . . ? C24 C25 H25 123(2) . . ? C25 C26 C21 121.3(3) . . ? C25 C26 H26 113.3(18) . . ? C21 C26 H26 125.4(18) . . ? C28 C27 C32 117.9(3) . . ? C28 C27 C33 121.8(3) . . ? C32 C27 C33 120.3(4) . . ? C27 C28 C29 121.3(3) . . ? C27 C28 H28 122(2) . . ? C29 C28 H28 116(2) . . ? C28 C29 C30 121.2(4) . . ? C28 C29 H29 121(2) . . ? C30 C29 H29 118(2) . . ? C31 C30 C29 117.2(3) . . ? C31 C30 C34 121.0(3) . . ? C29 C30 C34 121.9(3) . . ? C30 C31 C32 121.8(3) . . ? C30 C31 H31 120(2) . . ? C32 C31 H31 119(2) . . ? C31 C32 C27 120.6(4) . . ? C31 C32 H32 119(2) . . ? C27 C32 H32 120(2) . . ? C27 C33 H33A 109.5 . . ? C27 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C27 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C30 C34 H34A 109.5 . . ? C30 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C30 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 C1 C2 C9 -174.6(3) . . . . ? C21 C1 C2 C9 5.4(5) . . . . ? C15 C1 C2 C3 4.7(5) . . . . ? C21 C1 C2 C3 -175.3(3) . . . . ? C1 C2 C3 C4 53.4(4) . . . . ? C9 C2 C3 C4 -127.2(3) . . . . ? C1 C2 C3 C8 -127.7(3) . . . . ? C9 C2 C3 C8 51.7(4) . . . . ? C8 C3 C4 C5 2.8(5) . . . . ? C2 C3 C4 C5 -178.3(3) . . . . ? C3 C4 C5 C6 -1.3(5) . . . . ? C4 C5 C6 C7 -0.3(5) . . . . ? C4 C5 C6 Cl1 179.9(3) . . . . ? C5 C6 C7 C8 0.4(5) . . . . ? Cl1 C6 C7 C8 -179.8(3) . . . . ? C6 C7 C8 C3 1.1(5) . . . . ? C4 C3 C8 C7 -2.6(5) . . . . ? C2 C3 C8 C7 178.4(3) . . . . ? C1 C2 C9 C14 -133.0(3) . . . . ? C3 C2 C9 C14 47.7(4) . . . . ? C1 C2 C9 C10 47.7(4) . . . . ? C3 C2 C9 C10 -131.6(3) . . . . ? C14 C9 C10 C11 1.7(4) . . . . ? C2 C9 C10 C11 -179.0(3) . . . . ? C9 C10 C11 C12 1.2(5) . . . . ? C10 C11 C12 C13 -2.7(5) . . . . ? C10 C11 C12 Cl2 179.9(2) . . . . ? C11 C12 C13 C14 1.3(5) . . . . ? Cl2 C12 C13 C14 178.7(2) . . . . ? C12 C13 C14 C9 1.7(4) . . . . ? C10 C9 C14 C13 -3.1(4) . . . . ? C2 C9 C14 C13 177.6(3) . . . . ? C2 C1 C15 C20 54.9(4) . . . . ? C21 C1 C15 C20 -125.2(3) . . . . ? C2 C1 C15 C16 -126.7(3) . . . . ? C21 C1 C15 C16 53.2(4) . . . . ? C20 C15 C16 C17 -1.2(4) . . . . ? C1 C15 C16 C17 -179.7(3) . . . . ? C15 C16 C17 C18 1.2(4) . . . . ? C16 C17 C18 C19 -0.1(4) . . . . ? C16 C17 C18 Cl3 179.8(2) . . . . ? C17 C18 C19 C20 -1.1(5) . . . . ? Cl3 C18 C19 C20 179.0(2) . . . . ? C16 C15 C20 C19 0.0(4) . . . . ? C1 C15 C20 C19 178.5(3) . . . . ? C18 C19 C20 C15 1.1(5) . . . . ? C2 C1 C21 C22 -133.6(3) . . . . ? C15 C1 C21 C22 46.4(4) . . . . ? C2 C1 C21 C26 47.8(4) . . . . ? C15 C1 C21 C26 -132.2(3) . . . . ? C26 C21 C22 C23 -3.0(5) . . . . ? C1 C21 C22 C23 178.4(3) . . . . ? C21 C22 C23 C24 2.0(5) . . . . ? C22 C23 C24 C25 0.2(5) . . . . ? C22 C23 C24 Cl4 179.1(2) . . . . ? C23 C24 C25 C26 -1.4(5) . . . . ? Cl4 C24 C25 C26 179.7(2) . . . . ? C24 C25 C26 C21 0.4(5) . . . . ? C22 C21 C26 C25 1.7(4) . . . . ? C1 C21 C26 C25 -179.7(3) . . . . ? C32 C27 C28 C29 0.3(6) . . . . ? C33 C27 C28 C29 -179.5(4) . . . . ? C27 C28 C29 C30 -1.5(6) . . . . ? C28 C29 C30 C31 1.9(5) . . . . ? C28 C29 C30 C34 -178.3(4) . . . . ? C29 C30 C31 C32 -1.0(5) . . . . ? C34 C30 C31 C32 179.1(4) . . . . ? C30 C31 C32 C27 -0.2(6) . . . . ? C28 C27 C32 C31 0.6(6) . . . . ? C33 C27 C32 C31 -179.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.220 _refine_diff_density_min -0.293 _refine_diff_density_rms 0.056 #=== data_tan1b _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetra-(4-bromophenyl)ethene THF inclusion compound (2.THF) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H32 Br4 O2' _chemical_formula_weight 792.24 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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 9.3337(2) _cell_length_b 15.1835(3) _cell_length_c 21.9443(5) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 3109.9(1) _cell_formula_units_Z 4 _cell_measurement_temperature 208(2) _cell_measurement_reflns_used 7274 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 27.9 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.692 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 5.206 _exptl_absorpt_correction_type 'Scalepack/DENZO' _exptl_absorpt_correction_T_min 0.230 _exptl_absorpt_correction_T_max 0.422 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 208(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type NONIUS_KAPPA_CCD _diffrn_measurement_method '\p- and \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7236 _diffrn_reflns_av_R_equivalents 0.054 _diffrn_reflns_av_sigmaI/netI 0.085 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 27.89 _reflns_number_total 7236 _reflns_number_gt 5278 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0180P)^2^+7.5607P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.001(13) _refine_ls_number_reflns 7236 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.093 _refine_ls_R_factor_gt 0.052 _refine_ls_wR_factor_ref 0.093 _refine_ls_wR_factor_gt 0.082 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.76656(7) 0.22899(4) -0.19922(3) 0.04194(18) Uani 1 1 d . . . Br2 Br 0.45557(7) 0.47480(5) 0.21613(3) 0.03761(17) Uani 1 1 d . . . Br3 Br 0.79549(7) 0.78667(4) -0.31889(3) 0.03395(16) Uani 1 1 d . . . Br4 Br 0.71785(7) 0.94380(4) 0.13133(3) 0.03314(15) Uani 1 1 d . . . C1 C 0.6918(6) 0.6449(4) -0.0595(2) 0.0200(12) Uani 1 1 d . . . C2 C 0.6579(6) 0.5610(4) -0.0446(3) 0.0227(13) Uani 1 1 d . . . C3 C 0.6772(5) 0.4855(4) -0.0876(2) 0.0207(13) Uani 1 1 d . . . C4 C 0.8087(6) 0.4732(4) -0.1174(3) 0.0267(13) Uani 1 1 d . . . H4 H 0.8809 0.5160 -0.1139 0.032 Uiso 1 1 calc R . . C5 C 0.8328(6) 0.3984(4) -0.1519(3) 0.0303(15) Uani 1 1 d . . . H5 H 0.9204 0.3910 -0.1724 0.036 Uiso 1 1 calc R . . C6 C 0.7284(7) 0.3353(4) -0.1561(3) 0.0287(14) Uani 1 1 d . . . C7 C 0.5948(6) 0.3460(4) -0.1281(3) 0.0301(15) Uani 1 1 d . . . H7 H 0.5225 0.3033 -0.1323 0.036 Uiso 1 1 calc R . . C8 C 0.5726(6) 0.4210(4) -0.0942(3) 0.0241(13) Uani 1 1 d . . . H8 H 0.4837 0.4289 -0.0749 0.029 Uiso 1 1 calc R . . C9 C 0.6000(6) 0.5363(4) 0.0165(3) 0.0198(12) Uani 1 1 d . . . C10 C 0.4945(6) 0.5856(4) 0.0445(3) 0.0206(13) Uani 1 1 d . . . H10 H 0.4533 0.6332 0.0235 0.025 Uiso 1 1 calc R . . C11 C 0.4483(6) 0.5661(4) 0.1027(3) 0.0267(13) Uani 1 1 d . . . H11 H 0.3770 0.6006 0.1213 0.032 Uiso 1 1 calc R . . C12 C 0.5078(6) 0.4954(4) 0.1337(3) 0.0283(14) Uani 1 1 d . . . C13 C 0.6075(6) 0.4419(4) 0.1059(3) 0.0316(15) Uani 1 1 d . . . H13 H 0.6447 0.3925 0.1262 0.038 Uiso 1 1 calc R . . C14 C 0.6517(6) 0.4622(4) 0.0473(3) 0.0259(14) Uani 1 1 d . . . H14 H 0.7183 0.4253 0.0277 0.031 Uiso 1 1 calc R . . C15 C 0.7236(6) 0.6724(3) -0.1237(2) 0.0183(11) Uani 1 1 d . . . C16 C 0.8521(5) 0.7127(4) -0.1388(3) 0.0207(12) Uani 1 1 d . . . H16 H 0.9230 0.7193 -0.1087 0.025 Uiso 1 1 calc R . . C17 C 0.8785(6) 0.7437(4) -0.1973(3) 0.0267(14) Uani 1 1 d . . . H17 H 0.9678 0.7680 -0.2077 0.032 Uiso 1 1 calc R . . C18 C 0.7703(6) 0.7378(3) -0.2393(2) 0.0235(12) Uani 1 1 d . . . C19 C 0.6383(6) 0.6988(4) -0.2263(2) 0.0216(13) Uani 1 1 d . . . H19 H 0.5656 0.6957 -0.2559 0.026 Uiso 1 1 calc R . . C20 C 0.6182(6) 0.6649(4) -0.1681(3) 0.0237(13) Uani 1 1 d . . . H20 H 0.5317 0.6364 -0.1587 0.028 Uiso 1 1 calc R . . C21 C 0.7006(6) 0.7165(4) -0.0137(2) 0.0208(12) Uani 1 1 d . . . C22 C 0.6373(5) 0.7998(4) -0.0255(3) 0.0200(12) Uani 1 1 d . . . H22 H 0.5911 0.8101 -0.0629 0.024 Uiso 1 1 calc R . . C23 C 0.6431(6) 0.8658(4) 0.0176(3) 0.0226(13) Uani 1 1 d . . . H23 H 0.6006 0.9206 0.0094 0.027 Uiso 1 1 calc R . . C24 C 0.7100(6) 0.8523(3) 0.0722(3) 0.0222(12) Uani 1 1 d . . . C25 C 0.7791(6) 0.7727(4) 0.0842(2) 0.0249(12) Uani 1 1 d . . . H25 H 0.8295 0.7644 0.1208 0.030 Uiso 1 1 calc R . . C26 C 0.7720(6) 0.7070(4) 0.0417(2) 0.0227(12) Uani 1 1 d . . . H26 H 0.8172 0.6531 0.0503 0.027 Uiso 1 1 calc R . . O50 O 0.9666(5) 0.5978(3) 0.1404(2) 0.0451(12) Uani 1 1 d . . . C51 C 0.8510(7) 0.5924(4) 0.1832(3) 0.0391(17) Uani 1 1 d . . . H51A H 0.7586 0.5893 0.1621 0.047 Uiso 1 1 calc R . . H51B H 0.8507 0.6437 0.2104 0.047 Uiso 1 1 calc R . . C53 C 1.0407(7) 0.5139(5) 0.2274(3) 0.0473(19) Uani 1 1 d . . . H53A H 1.0832 0.4550 0.2294 0.057 Uiso 1 1 calc R . . H53B H 1.0651 0.5465 0.2645 0.057 Uiso 1 1 calc R . . C54 C 1.0908(7) 0.5637(5) 0.1700(3) 0.0415(18) Uani 1 1 d . . . H54A H 1.1554 0.6119 0.1813 0.050 Uiso 1 1 calc R . . H54B H 1.1423 0.5237 0.1426 0.050 Uiso 1 1 calc R . . C52 C 0.8789(7) 0.5089(5) 0.2186(3) 0.0450(18) Uani 1 1 d . . . H52A H 0.8514 0.4565 0.1953 0.054 Uiso 1 1 calc R . . H52B H 0.8283 0.5089 0.2577 0.054 Uiso 1 1 calc R . . O60 O -0.0584(6) 0.3214(3) 0.0322(3) 0.0615(15) Uani 1 1 d . . . C61 C 0.0304(9) 0.3853(5) 0.0622(4) 0.057(2) Uani 1 1 d . . . H61A H 0.0290 0.3762 0.1064 0.069 Uiso 1 1 calc R . . H61B H -0.0034 0.4451 0.0534 0.069 Uiso 1 1 calc R . . C62 C 0.1806(8) 0.3718(6) 0.0371(4) 0.054(2) Uani 1 1 d . . . H62A H 0.2330 0.4276 0.0351 0.065 Uiso 1 1 calc R . . H62B H 0.2347 0.3301 0.0623 0.065 Uiso 1 1 calc R . . C63 C 0.1545(9) 0.3354(6) -0.0252(4) 0.063(2) Uani 1 1 d . . . H63A H 0.2348 0.2985 -0.0385 0.075 Uiso 1 1 calc R . . H63B H 0.1401 0.3828 -0.0549 0.075 Uiso 1 1 calc R . . C64 C 0.0198(9) 0.2814(5) -0.0173(3) 0.056(2) Uani 1 1 d . . . H64A H -0.0374 0.2823 -0.0547 0.067 Uiso 1 1 calc R . . H64B H 0.0437 0.2202 -0.0075 0.067 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0539(4) 0.0286(3) 0.0433(4) -0.0119(3) 0.0113(3) 0.0018(3) Br2 0.0501(4) 0.0406(4) 0.0222(3) 0.0020(3) 0.0047(3) -0.0120(3) Br3 0.0429(4) 0.0379(4) 0.0211(3) 0.0053(3) 0.0051(3) 0.0003(3) Br4 0.0349(3) 0.0332(3) 0.0313(3) -0.0117(3) -0.0023(3) 0.0005(3) C1 0.015(3) 0.025(3) 0.020(3) 0.004(3) 0.001(2) 0.002(2) C2 0.019(3) 0.026(3) 0.024(3) 0.003(3) 0.000(2) -0.001(2) C3 0.024(3) 0.019(3) 0.019(3) -0.001(3) 0.003(2) -0.001(2) C4 0.025(3) 0.026(3) 0.028(3) 0.004(3) 0.003(3) 0.002(3) C5 0.028(3) 0.028(4) 0.035(4) -0.005(3) 0.010(3) 0.006(3) C6 0.036(4) 0.024(3) 0.026(3) -0.002(3) 0.008(3) 0.005(3) C7 0.035(3) 0.025(3) 0.030(4) -0.003(3) -0.001(3) -0.004(3) C8 0.017(3) 0.024(3) 0.031(3) -0.003(3) 0.003(3) -0.001(2) C9 0.023(3) 0.017(3) 0.020(3) 0.007(3) -0.002(2) -0.004(2) C10 0.022(3) 0.017(3) 0.022(3) -0.001(3) -0.002(2) 0.001(2) C11 0.027(3) 0.024(3) 0.029(3) 0.001(3) 0.002(3) -0.003(3) C12 0.035(3) 0.029(3) 0.021(3) 0.005(3) 0.007(3) -0.010(3) C13 0.041(4) 0.026(3) 0.028(3) 0.005(3) 0.000(3) 0.004(3) C14 0.027(3) 0.026(3) 0.024(3) 0.004(3) 0.005(2) 0.001(3) C15 0.020(3) 0.015(3) 0.020(3) -0.001(2) 0.000(3) 0.000(2) C16 0.022(3) 0.020(3) 0.020(3) -0.002(3) -0.003(2) 0.002(2) C17 0.025(3) 0.028(3) 0.027(3) -0.005(3) 0.003(3) 0.002(2) C18 0.037(3) 0.018(3) 0.015(3) 0.002(2) 0.001(3) 0.001(3) C19 0.027(3) 0.025(3) 0.012(3) -0.001(3) -0.002(2) 0.000(2) C20 0.025(3) 0.020(3) 0.026(3) 0.002(3) -0.002(3) -0.002(2) C21 0.019(3) 0.019(3) 0.024(3) 0.001(3) 0.004(2) -0.003(3) C22 0.018(3) 0.023(3) 0.019(3) 0.002(3) 0.004(2) 0.001(2) C23 0.025(3) 0.020(3) 0.023(3) 0.005(3) 0.001(3) 0.002(2) C24 0.019(3) 0.021(3) 0.027(3) -0.005(3) 0.007(3) 0.000(2) C25 0.022(3) 0.031(3) 0.021(3) 0.002(3) -0.001(3) -0.005(3) C26 0.024(3) 0.024(3) 0.021(3) 0.000(3) 0.003(2) -0.001(3) O50 0.036(3) 0.059(3) 0.040(3) 0.023(3) 0.003(2) -0.005(2) C51 0.044(4) 0.042(4) 0.031(4) 0.009(4) 0.006(3) 0.004(3) C53 0.045(4) 0.061(5) 0.036(4) 0.010(4) -0.006(3) -0.009(4) C54 0.032(4) 0.045(4) 0.048(5) -0.002(4) 0.001(3) -0.004(3) C52 0.043(4) 0.046(4) 0.046(4) 0.011(4) 0.012(4) 0.014(3) O60 0.054(3) 0.050(3) 0.080(4) -0.021(3) 0.002(3) 0.002(3) C61 0.065(5) 0.047(5) 0.060(5) -0.019(4) 0.001(4) 0.009(4) C62 0.046(5) 0.060(5) 0.057(5) -0.002(4) -0.006(4) 0.001(4) C63 0.064(6) 0.074(6) 0.050(5) -0.014(5) 0.004(4) -0.001(5) C64 0.085(6) 0.038(4) 0.043(5) -0.015(4) -0.008(4) 0.006(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 Br1 C6 1.905(6) . ? Br2 C12 1.899(6) . ? Br3 C18 1.912(5) . ? Br4 C24 1.903(5) . ? C1 C2 1.354(8) . ? C1 C21 1.482(8) . ? C1 C15 1.499(7) . ? C2 C9 1.493(8) . ? C2 C3 1.494(8) . ? C3 C8 1.391(8) . ? C3 C4 1.404(7) . ? C4 C5 1.382(8) . ? C4 H4 0.9400 . ? C5 C6 1.370(8) . ? C5 H5 0.9400 . ? C6 C7 1.400(8) . ? C7 C8 1.375(8) . ? C7 H7 0.9400 . ? C8 H8 0.9400 . ? C9 C10 1.381(8) . ? C9 C14 1.398(8) . ? C10 C11 1.380(8) . ? C10 H10 0.9400 . ? C11 C12 1.388(8) . ? C11 H11 0.9400 . ? C12 C13 1.378(8) . ? C13 C14 1.386(8) . ? C13 H13 0.9400 . ? C14 H14 0.9400 . ? C15 C16 1.386(7) . ? C15 C20 1.390(7) . ? C16 C17 1.388(8) . ? C16 H16 0.9400 . ? C17 C18 1.371(8) . ? C17 H17 0.9400 . ? C18 C19 1.395(8) . ? C19 C20 1.389(8) . ? C19 H19 0.9400 . ? C20 H20 0.9400 . ? C21 C26 1.394(7) . ? C21 C22 1.420(7) . ? C22 C23 1.379(8) . ? C22 H22 0.9400 . ? C23 C24 1.365(8) . ? C23 H23 0.9400 . ? C24 C25 1.395(8) . ? C25 C26 1.367(7) . ? C25 H25 0.9400 . ? C26 H26 0.9400 . ? O50 C54 1.425(8) . ? O50 C51 1.433(7) . ? C51 C52 1.510(9) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C53 C52 1.524(9) . ? C53 C54 1.542(9) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? O60 C61 1.435(9) . ? O60 C64 1.442(9) . ? C61 C62 1.520(10) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C62 C63 1.494(11) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C63 C64 1.511(11) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C21 122.7(5) . . ? C2 C1 C15 122.3(5) . . ? C21 C1 C15 115.0(5) . . ? C1 C2 C9 122.5(5) . . ? C1 C2 C3 122.8(5) . . ? C9 C2 C3 114.7(5) . . ? C8 C3 C4 118.1(5) . . ? C8 C3 C2 121.4(5) . . ? C4 C3 C2 120.2(5) . . ? C5 C4 C3 120.5(5) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C6 C5 C4 119.7(5) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C7 121.5(5) . . ? C5 C6 Br1 119.5(4) . . ? C7 C6 Br1 118.9(5) . . ? C8 C7 C6 117.9(5) . . ? C8 C7 H7 121.1 . . ? C6 C7 H7 121.1 . . ? C7 C8 C3 122.3(5) . . ? C7 C8 H8 118.9 . . ? C3 C8 H8 118.9 . . ? C10 C9 C14 117.8(5) . . ? C10 C9 C2 121.5(5) . . ? C14 C9 C2 120.7(5) . . ? C11 C10 C9 121.3(5) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C10 C11 C12 119.7(6) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C13 C12 C11 120.6(6) . . ? C13 C12 Br2 119.9(5) . . ? C11 C12 Br2 119.5(5) . . ? C12 C13 C14 118.8(6) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? C13 C14 C9 121.7(6) . . ? C13 C14 H14 119.2 . . ? C9 C14 H14 119.2 . . ? C16 C15 C20 118.7(5) . . ? C16 C15 C1 121.3(5) . . ? C20 C15 C1 119.8(5) . . ? C15 C16 C17 121.6(5) . . ? C15 C16 H16 119.2 . . ? C17 C16 H16 119.2 . . ? C18 C17 C16 118.0(5) . . ? C18 C17 H17 121.0 . . ? C16 C17 H17 121.0 . . ? C17 C18 C19 122.7(5) . . ? C17 C18 Br3 119.9(4) . . ? C19 C18 Br3 117.4(4) . . ? C20 C19 C18 117.6(5) . . ? C20 C19 H19 121.2 . . ? C18 C19 H19 121.2 . . ? C19 C20 C15 121.3(5) . . ? C19 C20 H20 119.4 . . ? C15 C20 H20 119.4 . . ? C26 C21 C22 116.7(5) . . ? C26 C21 C1 122.8(5) . . ? C22 C21 C1 120.4(5) . . ? C23 C22 C21 120.3(5) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C24 C23 C22 120.7(5) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C25 120.5(5) . . ? C23 C24 Br4 120.4(4) . . ? C25 C24 Br4 119.0(4) . . ? C26 C25 C24 118.7(5) . . ? C26 C25 H25 120.6 . . ? C24 C25 H25 120.6 . . ? C25 C26 C21 122.9(5) . . ? C25 C26 H26 118.6 . . ? C21 C26 H26 118.6 . . ? C54 O50 C51 107.1(5) . . ? O50 C51 C52 104.7(5) . . ? O50 C51 H51A 110.8 . . ? C52 C51 H51A 110.8 . . ? O50 C51 H51B 110.8 . . ? C52 C51 H51B 110.8 . . ? H51A C51 H51B 108.9 . . ? C52 C53 C54 102.8(6) . . ? C52 C53 H53A 111.2 . . ? C54 C53 H53A 111.2 . . ? C52 C53 H53B 111.2 . . ? C54 C53 H53B 111.2 . . ? H53A C53 H53B 109.1 . . ? O50 C54 C53 107.6(5) . . ? O50 C54 H54A 110.2 . . ? C53 C54 H54A 110.2 . . ? O50 C54 H54B 110.2 . . ? C53 C54 H54B 110.2 . . ? H54A C54 H54B 108.5 . . ? C51 C52 C53 101.2(6) . . ? C51 C52 H52A 111.5 . . ? C53 C52 H52A 111.5 . . ? C51 C52 H52B 111.5 . . ? C53 C52 H52B 111.5 . . ? H52A C52 H52B 109.3 . . ? C61 O60 C64 109.7(6) . . ? O60 C61 C62 106.0(6) . . ? O60 C61 H61A 110.5 . . ? C62 C61 H61A 110.5 . . ? O60 C61 H61B 110.5 . . ? C62 C61 H61B 110.5 . . ? H61A C61 H61B 108.7 . . ? C63 C62 C61 103.3(6) . . ? C63 C62 H62A 111.1 . . ? C61 C62 H62A 111.1 . . ? C63 C62 H62B 111.1 . . ? C61 C62 H62B 111.1 . . ? H62A C62 H62B 109.1 . . ? C62 C63 C64 103.4(7) . . ? C62 C63 H63A 111.1 . . ? C64 C63 H63A 111.1 . . ? C62 C63 H63B 111.1 . . ? C64 C63 H63B 111.1 . . ? H63A C63 H63B 109.1 . . ? O60 C64 C63 106.2(6) . . ? O60 C64 H64A 110.5 . . ? C63 C64 H64A 110.5 . . ? O60 C64 H64B 110.5 . . ? C63 C64 H64B 110.5 . . ? H64A C64 H64B 108.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 C1 C2 C9 11.8(8) . . . . ? C15 C1 C2 C9 -168.4(5) . . . . ? C21 C1 C2 C3 -167.3(5) . . . . ? C15 C1 C2 C3 12.5(8) . . . . ? C1 C2 C3 C8 -136.5(6) . . . . ? C9 C2 C3 C8 44.4(7) . . . . ? C1 C2 C3 C4 50.4(8) . . . . ? C9 C2 C3 C4 -128.8(5) . . . . ? C8 C3 C4 C5 -0.5(9) . . . . ? C2 C3 C4 C5 172.8(5) . . . . ? C3 C4 C5 C6 -1.1(9) . . . . ? C4 C5 C6 C7 2.5(10) . . . . ? C4 C5 C6 Br1 -175.9(4) . . . . ? C5 C6 C7 C8 -2.1(9) . . . . ? Br1 C6 C7 C8 176.3(5) . . . . ? C6 C7 C8 C3 0.4(9) . . . . ? C4 C3 C8 C7 0.8(9) . . . . ? C2 C3 C8 C7 -172.4(6) . . . . ? C1 C2 C9 C10 44.1(8) . . . . ? C3 C2 C9 C10 -136.7(5) . . . . ? C1 C2 C9 C14 -135.7(6) . . . . ? C3 C2 C9 C14 43.5(7) . . . . ? C14 C9 C10 C11 4.4(8) . . . . ? C2 C9 C10 C11 -175.5(5) . . . . ? C9 C10 C11 C12 -0.5(8) . . . . ? C10 C11 C12 C13 -3.2(9) . . . . ? C10 C11 C12 Br2 174.8(4) . . . . ? C11 C12 C13 C14 2.8(9) . . . . ? Br2 C12 C13 C14 -175.2(4) . . . . ? C12 C13 C14 C9 1.3(9) . . . . ? C10 C9 C14 C13 -4.8(8) . . . . ? C2 C9 C14 C13 175.1(5) . . . . ? C2 C1 C15 C16 -123.5(6) . . . . ? C21 C1 C15 C16 56.4(7) . . . . ? C2 C1 C15 C20 62.5(7) . . . . ? C21 C1 C15 C20 -117.6(5) . . . . ? C20 C15 C16 C17 -1.5(8) . . . . ? C1 C15 C16 C17 -175.6(5) . . . . ? C15 C16 C17 C18 3.6(8) . . . . ? C16 C17 C18 C19 -2.7(9) . . . . ? C16 C17 C18 Br3 175.7(4) . . . . ? C17 C18 C19 C20 -0.2(9) . . . . ? Br3 C18 C19 C20 -178.6(4) . . . . ? C18 C19 C20 C15 2.4(8) . . . . ? C16 C15 C20 C19 -1.6(8) . . . . ? C1 C15 C20 C19 172.6(5) . . . . ? C2 C1 C21 C26 46.3(8) . . . . ? C15 C1 C21 C26 -133.6(5) . . . . ? C2 C1 C21 C22 -134.9(6) . . . . ? C15 C1 C21 C22 45.2(7) . . . . ? C26 C21 C22 C23 -2.4(8) . . . . ? C1 C21 C22 C23 178.7(5) . . . . ? C21 C22 C23 C24 0.2(8) . . . . ? C22 C23 C24 C25 2.8(9) . . . . ? C22 C23 C24 Br4 179.9(4) . . . . ? C23 C24 C25 C26 -3.4(8) . . . . ? Br4 C24 C25 C26 179.5(4) . . . . ? C24 C25 C26 C21 1.1(8) . . . . ? C22 C21 C26 C25 1.8(8) . . . . ? C1 C21 C26 C25 -179.4(5) . . . . ? C54 O50 C51 C52 -35.3(7) . . . . ? C51 O50 C54 C53 14.8(7) . . . . ? C52 C53 C54 O50 11.0(8) . . . . ? O50 C51 C52 C53 41.0(7) . . . . ? C54 C53 C52 C51 -30.7(7) . . . . ? C64 O60 C61 C62 -10.9(8) . . . . ? O60 C61 C62 C63 27.9(9) . . . . ? C61 C62 C63 C64 -33.5(9) . . . . ? C61 O60 C64 C63 -10.5(8) . . . . ? C62 C63 C64 O60 27.8(8) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.248 _refine_diff_density_min -0.724 _refine_diff_density_rms 0.116 #=== data_731todaf _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetra-(4-fluorophenyl)ethene xylene inclusion compound (4.pXy) ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H31 F4' _chemical_formula_weight 563.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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 9.175(5) _cell_length_b 9.522(2) _cell_length_c 17.790(4) _cell_angle_alpha 91.15(2) _cell_angle_beta 97.65(3) _cell_angle_gamma 104.15(2) _cell_volume 1491.5(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.2 _cell_measurement_theta_max 18.6 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.255 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 590 _exptl_absorpt_coefficient_mu 0.089 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.961 _exptl_absorpt_correction_T_max 0.987 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type NONIUS_CAD4 _diffrn_measurement_method \w2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 2 _diffrn_reflns_number 7597 _diffrn_reflns_av_R_equivalents 0.0135 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 27.97 _reflns_number_total 7170 _reflns_number_gt 4562 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0642P)^2^+0.2255P] 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 7170 _refine_ls_number_parameters 470 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.091 _refine_ls_R_factor_gt 0.041 _refine_ls_wR_factor_ref 0.122 _refine_ls_wR_factor_gt 0.104 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.010 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group F1 F 0.91724(13) 0.83079(11) -0.10147(5) 0.0519(3) Uani 1 d . . . F2 F 0.91367(15) 1.27586(11) 0.37547(6) 0.0635(3) Uani 1 d . . . F3 F 0.60466(12) 0.12874(10) 0.03252(5) 0.0481(3) Uani 1 d . . . F4 F 0.74523(16) 0.51915(14) 0.53496(6) 0.0716(4) Uani 1 d . . . C1 C 0.78030(15) 0.62585(14) 0.22851(7) 0.0271(3) Uani 1 d . . . C2 C 0.82515(15) 0.75833(14) 0.20164(7) 0.0269(3) Uani 1 d . . . C3 C 0.85073(16) 0.77759(14) 0.12112(7) 0.0276(3) Uani 1 d . . . C4 C 0.94963(18) 0.71158(18) 0.08956(9) 0.0366(3) Uani 1 d . . . C5 C 0.97232(19) 0.72861(19) 0.01459(9) 0.0414(4) Uani 1 d . . . C6 C 0.89559(18) 0.81337(16) -0.02785(8) 0.0360(3) Uani 1 d . . . C7 C 0.79932(18) 0.88284(16) 0.00095(8) 0.0356(3) Uani 1 d . . . C8 C 0.77774(17) 0.86472(15) 0.07599(8) 0.0307(3) Uani 1 d . . . C9 C 0.84895(17) 0.89494(14) 0.24889(7) 0.0285(3) Uani 1 d . . . C10 C 0.73775(18) 0.91759(16) 0.29012(8) 0.0336(3) Uani 1 d . . . C11 C 0.7584(2) 1.04646(18) 0.33259(9) 0.0410(4) Uani 1 d . . . C12 C 0.8922(2) 1.14994(16) 0.33329(8) 0.0420(4) Uani 1 d . . . C13 C 1.0040(2) 1.13320(17) 0.29269(9) 0.0412(4) Uani 1 d . . . C14 C 0.98107(18) 1.00466(16) 0.24966(8) 0.0335(3) Uani 1 d . . . C15 C 0.73304(16) 0.49304(14) 0.17689(7) 0.0268(3) Uani 1 d . . . C16 C 0.80006(17) 0.37782(15) 0.18956(8) 0.0314(3) Uani 1 d . . . C17 C 0.75893(19) 0.25549(16) 0.14070(9) 0.0357(3) Uani 1 d . . . C18 C 0.64736(18) 0.24885(15) 0.08045(8) 0.0337(3) Uani 1 d . . . C19 C 0.57444(18) 0.35774(16) 0.06681(8) 0.0346(3) Uani 1 d . . . C20 C 0.61900(17) 0.48024(15) 0.11538(8) 0.0307(3) Uani 1 d . . . C21 C 0.77259(17) 0.60029(14) 0.31045(8) 0.0287(3) Uani 1 d . . . C22 C 0.6396(2) 0.51849(19) 0.33272(9) 0.0422(4) Uani 1 d . . . C23 C 0.6294(2) 0.4922(2) 0.40819(10) 0.0518(5) Uani 1 d . . . C24 C 0.7550(2) 0.54581(19) 0.46051(9) 0.0459(4) Uani 1 d . . . C25 C 0.8891(2) 0.62398(18) 0.44168(9) 0.0420(4) Uani 1 d . . . C26 C 0.89707(19) 0.65232(16) 0.36589(8) 0.0344(3) Uani 1 d . . . C27 C 0.2994(2) 0.6537(2) 0.20360(12) 0.0508(4) Uani 1 d . . . C28 C 0.2883(2) 0.7186(2) 0.27205(13) 0.0605(5) Uani 1 d . . . C29 C 0.3228(2) 0.8676(2) 0.28328(11) 0.0551(5) Uani 1 d . . . C30 C 0.37130(19) 0.95769(19) 0.22673(10) 0.0433(4) Uani 1 d . . . C31 C 0.3856(2) 0.8929(2) 0.15887(10) 0.0434(4) Uani 1 d . . . C32 C 0.3500(2) 0.7442(2) 0.14757(11) 0.0475(4) Uani 1 d . . . C33 C 0.2547(3) 0.4920(2) 0.18979(17) 0.0790(7) Uani 1 d . . . H33A H 0.2548 0.4459 0.2386 0.119 Uiso 1 calc R . . H33B H 0.3273 0.4620 0.1612 0.119 Uiso 1 calc R . . H33C H 0.1528 0.4623 0.1606 0.119 Uiso 1 calc R . . C34 C 0.4075(2) 1.1200(2) 0.23855(13) 0.0599(5) Uani 1 d . . . H34A H 0.5147 1.1613 0.2342 0.090 Uiso 1 calc R . . H34B H 0.3876 1.1456 0.2892 0.090 Uiso 1 calc R . . H34C H 0.3437 1.1589 0.1999 0.090 Uiso 1 calc R . . C35 C 0.3483(2) 0.0098(2) 0.48735(9) 0.0438(4) Uani 1 d . . . C36 C 0.3837(2) -0.1227(2) 0.48633(11) 0.0508(4) Uani 1 d . . . C37 C 0.4670(2) 0.1319(2) 0.50143(10) 0.0489(4) Uani 1 d . . . C38 C 0.1861(2) 0.0199(3) 0.47376(12) 0.0646(6) Uani 1 d . . . H38A H 0.1807 0.1173 0.4898 0.097 Uiso 1 calc R . . H38B H 0.1247 -0.0520 0.5030 0.097 Uiso 1 calc R . . H38C H 0.1470 0.0009 0.4196 0.097 Uiso 1 calc R . . H4 H 1.003(2) 0.652(2) 0.1200(11) 0.049(5) Uiso 1 d . . . H5 H 1.038(2) 0.683(2) -0.0088(11) 0.058(6) Uiso 1 d . . . H7 H 0.747(2) 0.946(2) -0.0313(11) 0.051(5) Uiso 1 d . . . H8 H 0.7094(19) 0.9159(17) 0.0982(9) 0.036(4) Uiso 1 d . . . H10 H 0.646(2) 0.8443(18) 0.2900(9) 0.036(4) Uiso 1 d . . . H11 H 0.680(2) 1.063(2) 0.3614(11) 0.052(5) Uiso 1 d . . . H13 H 1.100(2) 1.207(2) 0.2942(11) 0.055(5) Uiso 1 d . . . H14 H 1.061(2) 0.9902(18) 0.2192(10) 0.043(5) Uiso 1 d . . . H16 H 0.8775(19) 0.3883(17) 0.2326(10) 0.034(4) Uiso 1 d . . . H17 H 0.802(2) 0.178(2) 0.1487(10) 0.050(5) Uiso 1 d . . . H19 H 0.496(2) 0.3446(18) 0.0240(10) 0.039(4) Uiso 1 d . . . H20 H 0.5717(19) 0.5599(18) 0.1076(9) 0.036(4) Uiso 1 d . . . H22 H 0.556(2) 0.483(2) 0.2947(11) 0.053(5) Uiso 1 d . . . H23 H 0.540(3) 0.437(2) 0.4229(12) 0.070(7) Uiso 1 d . . . H25 H 0.971(2) 0.655(2) 0.4809(11) 0.048(5) Uiso 1 d . . . H26 H 0.990(2) 0.7066(19) 0.3503(10) 0.043(5) Uiso 1 d . . . H28 H 0.259(3) 0.658(3) 0.3129(14) 0.083(7) Uiso 1 d . . . H29 H 0.317(2) 0.915(2) 0.3320(12) 0.062(6) Uiso 1 d . . . H31 H 0.418(2) 0.951(2) 0.1157(12) 0.061(6) Uiso 1 d . . . H32 H 0.359(2) 0.698(2) 0.0993(12) 0.060(6) Uiso 1 d . . . H36 H 0.298(3) -0.213(2) 0.4739(12) 0.066(6) Uiso 1 d . . . H37 H 0.448(2) 0.232(2) 0.5052(12) 0.065(6) Uiso 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 F1 0.0646(7) 0.0611(6) 0.0296(5) 0.0118(4) 0.0147(4) 0.0101(5) F2 0.1051(10) 0.0398(5) 0.0420(5) -0.0137(4) -0.0082(6) 0.0228(6) F3 0.0688(7) 0.0331(5) 0.0396(5) -0.0089(4) 0.0018(5) 0.0112(4) F4 0.0989(10) 0.0834(8) 0.0305(5) 0.0163(5) 0.0203(6) 0.0118(7) C1 0.0270(7) 0.0280(7) 0.0264(6) 0.0025(5) 0.0022(5) 0.0079(5) C2 0.0265(7) 0.0273(7) 0.0275(6) 0.0034(5) 0.0029(5) 0.0079(5) C3 0.0282(7) 0.0257(6) 0.0272(6) 0.0043(5) 0.0032(5) 0.0039(5) C4 0.0344(8) 0.0438(8) 0.0363(8) 0.0127(7) 0.0095(6) 0.0158(7) C5 0.0407(9) 0.0506(10) 0.0381(8) 0.0082(7) 0.0156(7) 0.0155(8) C6 0.0405(9) 0.0373(8) 0.0257(7) 0.0054(6) 0.0067(6) -0.0001(6) C7 0.0418(9) 0.0299(7) 0.0321(7) 0.0063(6) -0.0016(6) 0.0066(6) C8 0.0358(8) 0.0250(7) 0.0307(7) 0.0014(5) 0.0018(6) 0.0080(6) C9 0.0353(8) 0.0257(6) 0.0245(6) 0.0054(5) 0.0010(5) 0.0092(6) C10 0.0388(9) 0.0330(8) 0.0313(7) 0.0056(6) 0.0060(6) 0.0121(7) C11 0.0581(11) 0.0423(9) 0.0291(7) 0.0048(6) 0.0078(7) 0.0241(8) C12 0.0686(12) 0.0310(8) 0.0245(7) -0.0014(6) -0.0083(7) 0.0171(8) C13 0.0488(10) 0.0304(8) 0.0363(8) 0.0037(6) -0.0082(7) 0.0022(7) C14 0.0369(8) 0.0307(7) 0.0309(7) 0.0060(6) 0.0003(6) 0.0066(6) C15 0.0296(7) 0.0243(6) 0.0269(6) 0.0042(5) 0.0059(5) 0.0060(5) C16 0.0343(8) 0.0300(7) 0.0303(7) 0.0045(6) 0.0013(6) 0.0100(6) C17 0.0439(9) 0.0290(7) 0.0379(8) 0.0041(6) 0.0077(7) 0.0150(7) C18 0.0434(9) 0.0267(7) 0.0300(7) -0.0007(5) 0.0088(6) 0.0052(6) C19 0.0372(8) 0.0333(7) 0.0297(7) 0.0026(6) -0.0019(6) 0.0051(6) C20 0.0314(7) 0.0277(7) 0.0331(7) 0.0050(5) 0.0017(6) 0.0088(6) C21 0.0360(8) 0.0235(6) 0.0276(7) 0.0045(5) 0.0061(6) 0.0085(5) C22 0.0397(9) 0.0462(9) 0.0352(8) 0.0060(7) 0.0060(7) -0.0004(7) C23 0.0541(11) 0.0560(11) 0.0420(9) 0.0126(8) 0.0183(8) 0.0006(9) C24 0.0674(12) 0.0458(9) 0.0273(7) 0.0093(7) 0.0140(8) 0.0150(8) C25 0.0529(10) 0.0430(9) 0.0285(7) 0.0022(6) -0.0006(7) 0.0123(8) C26 0.0373(8) 0.0345(8) 0.0304(7) 0.0038(6) 0.0034(6) 0.0079(6) C27 0.0311(9) 0.0530(10) 0.0721(12) 0.0096(9) 0.0088(8) 0.0161(8) C28 0.0552(12) 0.0701(13) 0.0691(13) 0.0325(11) 0.0298(10) 0.0270(10) C29 0.0614(12) 0.0725(13) 0.0433(10) 0.0123(9) 0.0205(9) 0.0314(10) C30 0.0353(9) 0.0543(10) 0.0456(9) 0.0080(7) 0.0072(7) 0.0203(8) C31 0.0390(9) 0.0596(11) 0.0377(8) 0.0130(8) 0.0076(7) 0.0220(8) C32 0.0407(10) 0.0627(11) 0.0431(9) 0.0001(8) 0.0025(7) 0.0226(8) C33 0.0488(13) 0.0551(13) 0.134(2) 0.0100(13) 0.0139(13) 0.0129(10) C34 0.0553(12) 0.0576(12) 0.0710(13) 0.0022(10) 0.0106(10) 0.0212(10) C35 0.0519(10) 0.0567(10) 0.0289(7) 0.0079(7) 0.0112(7) 0.0218(8) C36 0.0569(12) 0.0462(10) 0.0504(10) 0.0016(8) 0.0139(9) 0.0117(9) C37 0.0656(12) 0.0454(10) 0.0454(9) 0.0082(8) 0.0176(9) 0.0266(9) C38 0.0568(13) 0.0963(17) 0.0500(11) 0.0083(11) 0.0105(9) 0.0346(12) _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 F1 C6 1.3579(16) . ? F2 C12 1.3596(17) . ? F3 C18 1.3570(17) . ? F4 C24 1.3641(18) . ? C1 C2 1.3463(19) . ? C1 C15 1.4867(19) . ? C1 C21 1.4907(19) . ? C2 C9 1.4882(19) . ? C2 C3 1.4897(18) . ? C3 C4 1.391(2) . ? C3 C8 1.392(2) . ? C4 C5 1.384(2) . ? C4 H4 0.965(19) . ? C5 C6 1.370(2) . ? C5 H5 0.95(2) . ? C6 C7 1.369(2) . ? C7 C8 1.384(2) . ? C7 H7 1.000(19) . ? C8 H8 0.997(17) . ? C9 C10 1.388(2) . ? C9 C14 1.392(2) . ? C10 C11 1.387(2) . ? C10 H10 0.955(17) . ? C11 C12 1.372(3) . ? C11 H11 0.98(2) . ? C12 C13 1.368(3) . ? C13 C14 1.386(2) . ? C13 H13 0.98(2) . ? C14 H14 1.003(18) . ? C15 C20 1.391(2) . ? C15 C16 1.391(2) . ? C16 C17 1.383(2) . ? C16 H16 0.959(17) . ? C17 C18 1.369(2) . ? C17 H17 0.920(19) . ? C18 C19 1.374(2) . ? C19 C20 1.381(2) . ? C19 H19 0.960(18) . ? C20 H20 0.966(17) . ? C21 C26 1.388(2) . ? C21 C22 1.389(2) . ? C22 C23 1.382(2) . ? C22 H22 0.94(2) . ? C23 C24 1.365(3) . ? C23 H23 0.93(2) . ? C24 C25 1.361(3) . ? C25 C26 1.388(2) . ? C25 H25 0.94(2) . ? C26 H26 0.958(19) . ? C27 C28 1.382(3) . ? C27 C32 1.384(3) . ? C27 C33 1.500(3) . ? C28 C29 1.380(3) . ? C28 H28 0.96(3) . ? C29 C30 1.383(3) . ? C29 H29 0.98(2) . ? C30 C31 1.381(2) . ? C30 C34 1.503(3) . ? C31 C32 1.377(3) . ? C31 H31 0.99(2) . ? C32 H32 0.98(2) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C37 1.378(3) . ? C35 C36 1.378(3) . ? C35 C38 1.503(3) . ? C36 C37 1.382(3) 2_656 ? C36 H36 1.01(2) . ? C37 C36 1.383(3) 2_656 ? C37 H37 1.02(2) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C15 121.31(12) . . ? C2 C1 C21 123.59(12) . . ? C15 C1 C21 115.10(11) . . ? C1 C2 C9 122.96(12) . . ? C1 C2 C3 121.68(12) . . ? C9 C2 C3 115.35(11) . . ? C4 C3 C8 118.35(13) . . ? C4 C3 C2 121.16(12) . . ? C8 C3 C2 120.48(13) . . ? C5 C4 C3 121.09(14) . . ? C5 C4 H4 118.9(11) . . ? C3 C4 H4 120.0(11) . . ? C6 C5 C4 118.28(15) . . ? C6 C5 H5 118.8(12) . . ? C4 C5 H5 122.9(12) . . ? F1 C6 C7 118.43(14) . . ? F1 C6 C5 118.69(15) . . ? C7 C6 C5 122.88(14) . . ? C6 C7 C8 118.17(14) . . ? C6 C7 H7 120.8(11) . . ? C8 C7 H7 121.0(11) . . ? C7 C8 C3 121.21(14) . . ? C7 C8 H8 119.3(9) . . ? C3 C8 H8 119.5(9) . . ? C10 C9 C14 119.01(14) . . ? C10 C9 C2 120.79(13) . . ? C14 C9 C2 120.15(13) . . ? C11 C10 C9 120.76(15) . . ? C11 C10 H10 118.7(10) . . ? C9 C10 H10 120.5(10) . . ? C12 C11 C10 118.18(16) . . ? C12 C11 H11 120.8(11) . . ? C10 C11 H11 121.1(12) . . ? F2 C12 C13 118.50(16) . . ? F2 C12 C11 118.41(16) . . ? C13 C12 C11 123.08(15) . . ? C12 C13 C14 118.17(16) . . ? C12 C13 H13 122.6(11) . . ? C14 C13 H13 119.2(11) . . ? C13 C14 C9 120.78(16) . . ? C13 C14 H14 119.6(10) . . ? C9 C14 H14 119.7(10) . . ? C20 C15 C16 118.43(13) . . ? C20 C15 C1 120.69(12) . . ? C16 C15 C1 120.87(13) . . ? C17 C16 C15 121.06(14) . . ? C17 C16 H16 121.8(10) . . ? C15 C16 H16 117.1(10) . . ? C18 C17 C16 118.24(14) . . ? C18 C17 H17 119.9(12) . . ? C16 C17 H17 121.9(12) . . ? F3 C18 C17 118.88(13) . . ? F3 C18 C19 118.20(14) . . ? C17 C18 C19 122.91(14) . . ? C18 C19 C20 118.02(14) . . ? C18 C19 H19 118.2(10) . . ? C20 C19 H19 123.7(10) . . ? C19 C20 C15 121.28(13) . . ? C19 C20 H20 120.9(10) . . ? C15 C20 H20 117.9(10) . . ? C26 C21 C22 118.25(14) . . ? C26 C21 C1 121.81(13) . . ? C22 C21 C1 119.91(14) . . ? C23 C22 C21 121.20(17) . . ? C23 C22 H22 121.0(12) . . ? C21 C22 H22 117.8(12) . . ? C24 C23 C22 118.26(17) . . ? C24 C23 H23 120.8(14) . . ? C22 C23 H23 120.9(14) . . ? C25 C24 F4 118.75(16) . . ? C25 C24 C23 122.99(15) . . ? F4 C24 C23 118.26(16) . . ? C24 C25 C26 118.24(16) . . ? C24 C25 H25 117.8(11) . . ? C26 C25 H25 124.0(12) . . ? C21 C26 C25 121.03(15) . . ? C21 C26 H26 118.1(11) . . ? C25 C26 H26 120.8(11) . . ? C28 C27 C32 117.20(19) . . ? C28 C27 C33 121.5(2) . . ? C32 C27 C33 121.3(2) . . ? C29 C28 C27 121.28(18) . . ? C29 C28 H28 119.9(14) . . ? C27 C28 H28 118.8(14) . . ? C28 C29 C30 121.29(19) . . ? C28 C29 H29 122.0(12) . . ? C30 C29 H29 116.7(12) . . ? C31 C30 C29 117.44(18) . . ? C31 C30 C34 121.15(16) . . ? C29 C30 C34 121.40(17) . . ? C32 C31 C30 121.18(17) . . ? C32 C31 H31 117.3(11) . . ? C30 C31 H31 121.5(11) . . ? C31 C32 C27 121.57(18) . . ? C31 C32 H32 121.1(12) . . ? C27 C32 H32 117.4(12) . . ? C27 C33 H33A 109.5 . . ? C27 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C27 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C30 C34 H34A 109.5 . . ? C30 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C30 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C37 C35 C36 117.45(17) . . ? C37 C35 C38 121.56(18) . . ? C36 C35 C38 120.99(19) . . ? C35 C36 C37 120.95(19) . 2_656 ? C35 C36 H36 118.4(12) . . ? C37 C36 H36 120.6(12) 2_656 . ? C35 C37 C36 121.60(17) . 2_656 ? C35 C37 H37 120.9(12) . . ? C36 C37 H37 117.5(12) 2_656 . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 C1 C2 C9 169.68(13) . . . . ? C21 C1 C2 C9 -9.8(2) . . . . ? C15 C1 C2 C3 -8.8(2) . . . . ? C21 C1 C2 C3 171.77(13) . . . . ? C1 C2 C3 C4 -55.1(2) . . . . ? C9 C2 C3 C4 126.31(15) . . . . ? C1 C2 C3 C8 126.06(15) . . . . ? C9 C2 C3 C8 -52.52(18) . . . . ? C8 C3 C4 C5 -1.7(2) . . . . ? C2 C3 C4 C5 179.47(15) . . . . ? C3 C4 C5 C6 0.5(2) . . . . ? C4 C5 C6 F1 179.95(14) . . . . ? C4 C5 C6 C7 0.8(3) . . . . ? F1 C6 C7 C8 -179.98(13) . . . . ? C5 C6 C7 C8 -0.8(2) . . . . ? C6 C7 C8 C3 -0.4(2) . . . . ? C4 C3 C8 C7 1.7(2) . . . . ? C2 C3 C8 C7 -179.49(13) . . . . ? C1 C2 C9 C10 -51.01(19) . . . . ? C3 C2 C9 C10 127.54(14) . . . . ? C1 C2 C9 C14 131.77(15) . . . . ? C3 C2 C9 C14 -49.68(17) . . . . ? C14 C9 C10 C11 -1.1(2) . . . . ? C2 C9 C10 C11 -178.33(13) . . . . ? C9 C10 C11 C12 -0.7(2) . . . . ? C10 C11 C12 F2 -179.32(13) . . . . ? C10 C11 C12 C13 1.7(2) . . . . ? F2 C12 C13 C14 -179.83(13) . . . . ? C11 C12 C13 C14 -0.8(2) . . . . ? C12 C13 C14 C9 -1.0(2) . . . . ? C10 C9 C14 C13 1.9(2) . . . . ? C2 C9 C14 C13 179.21(13) . . . . ? C2 C1 C15 C20 -54.9(2) . . . . ? C21 C1 C15 C20 124.55(14) . . . . ? C2 C1 C15 C16 126.05(15) . . . . ? C21 C1 C15 C16 -54.45(18) . . . . ? C20 C15 C16 C17 2.5(2) . . . . ? C1 C15 C16 C17 -178.50(14) . . . . ? C15 C16 C17 C18 -1.7(2) . . . . ? C16 C17 C18 F3 -179.27(14) . . . . ? C16 C17 C18 C19 -0.3(2) . . . . ? F3 C18 C19 C20 -179.53(13) . . . . ? C17 C18 C19 C20 1.5(2) . . . . ? C18 C19 C20 C15 -0.7(2) . . . . ? C16 C15 C20 C19 -1.2(2) . . . . ? C1 C15 C20 C19 179.73(13) . . . . ? C2 C1 C21 C26 -54.7(2) . . . . ? C15 C1 C21 C26 125.84(15) . . . . ? C2 C1 C21 C22 127.42(16) . . . . ? C15 C1 C21 C22 -52.06(19) . . . . ? C26 C21 C22 C23 1.6(2) . . . . ? C1 C21 C22 C23 179.58(16) . . . . ? C21 C22 C23 C24 -1.6(3) . . . . ? C22 C23 C24 C25 0.2(3) . . . . ? C22 C23 C24 F4 -179.63(17) . . . . ? F4 C24 C25 C26 -179.04(15) . . . . ? C23 C24 C25 C26 1.2(3) . . . . ? C22 C21 C26 C25 -0.2(2) . . . . ? C1 C21 C26 C25 -178.15(14) . . . . ? C24 C25 C26 C21 -1.1(2) . . . . ? C32 C27 C28 C29 1.5(3) . . . . ? C33 C27 C28 C29 -176.92(19) . . . . ? C27 C28 C29 C30 -0.6(3) . . . . ? C28 C29 C30 C31 -0.7(3) . . . . ? C28 C29 C30 C34 179.39(19) . . . . ? C29 C30 C31 C32 1.2(2) . . . . ? C34 C30 C31 C32 -178.92(17) . . . . ? C30 C31 C32 C27 -0.3(3) . . . . ? C28 C27 C32 C31 -1.0(3) . . . . ? C33 C27 C32 C31 177.39(18) . . . . ? C37 C35 C36 C37 -0.4(3) . . . 2_656 ? C38 C35 C36 C37 179.76(17) . . . 2_656 ? C36 C35 C37 C36 0.4(3) . . . 2_656 ? C38 C35 C37 C36 -179.76(17) . . . 2_656 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.97 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.234 _refine_diff_density_min -0.218 _refine_diff_density_rms 0.047 #=== data_770tooh _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetra(4-hydroxyphenyl)ethene acetylacetate water inclusion compound (7.E-W) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H30 O7' _chemical_formula_weight 502.54 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 10.343(4) _cell_length_b 10.887(5) _cell_length_c 13.918(6) _cell_angle_alpha 103.65(4) _cell_angle_beta 91.19(3) _cell_angle_gamma 117.64(3) _cell_volume 1333.6(10) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.1 _cell_measurement_theta_max 18.8 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 532 _exptl_absorpt_coefficient_mu 0.089 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.961 _exptl_absorpt_correction_T_max 0.993 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type NONIUS_CAD4 _diffrn_measurement_method \w2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 7 _diffrn_reflns_number 6848 _diffrn_reflns_av_R_equivalents 0.041 _diffrn_reflns_av_sigmaI/netI 0.045 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 27.98 _reflns_number_total 6419 _reflns_number_gt 4232 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0711P)^2^+1.5635P] 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 6419 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.105 _refine_ls_R_factor_gt 0.059 _refine_ls_wR_factor_ref 0.184 _refine_ls_wR_factor_gt 0.164 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.6560(2) 0.2922(2) 1.31274(14) 0.0371(5) Uani 1 1 d . . . O2 O 0.5709(2) 0.1631(2) 0.62735(13) 0.0366(5) Uani 1 1 d . . . O3 O 1.4772(2) 0.4128(2) 1.31497(14) 0.0343(4) Uani 1 1 d . . . O4 O 1.2753(2) 0.0549(2) 0.62435(13) 0.0363(5) Uani 1 1 d . . . C1 C 1.0674(3) 0.2461(3) 0.97080(17) 0.0238(5) Uani 1 1 d . . . C2 C 0.9361(3) 0.2454(3) 0.97103(16) 0.0234(5) Uani 1 1 d . . . C3 C 0.8694(3) 0.2641(3) 1.06363(16) 0.0236(5) Uani 1 1 d . . . C4 C 0.8630(3) 0.1888(3) 1.13344(18) 0.0275(5) Uani 1 1 d . . . C5 C 0.7932(3) 0.2002(3) 1.21636(19) 0.0295(5) Uani 1 1 d . . . C6 C 0.7275(3) 0.2875(3) 1.23039(17) 0.0272(5) Uani 1 1 d . . . C7 C 0.7325(3) 0.3644(3) 1.16294(19) 0.0286(5) Uani 1 1 d . . . C8 C 0.8029(3) 0.3517(3) 1.08032(18) 0.0269(5) Uani 1 1 d . . . C9 C 0.8433(3) 0.2222(3) 0.87834(16) 0.0231(5) Uani 1 1 d . . . C10 C 0.9029(3) 0.2895(3) 0.80401(17) 0.0240(5) Uani 1 1 d . . . C11 C 0.8148(3) 0.2711(3) 0.71995(17) 0.0252(5) Uani 1 1 d . . . C12 C 0.6632(3) 0.1833(3) 0.70878(17) 0.0251(5) Uani 1 1 d . . . C13 C 0.6005(3) 0.1149(3) 0.78111(19) 0.0292(5) Uani 1 1 d . . . C14 C 0.6897(3) 0.1352(3) 0.86494(18) 0.0279(5) Uani 1 1 d . . . C15 C 1.1713(3) 0.2905(3) 1.06399(17) 0.0238(5) Uani 1 1 d . . . C16 C 1.2374(3) 0.2074(3) 1.07625(18) 0.0274(5) Uani 1 1 d . . . C17 C 1.3370(3) 0.2483(3) 1.15999(18) 0.0292(5) Uani 1 1 d . . . C18 C 1.3737(3) 0.3746(3) 1.23403(17) 0.0252(5) Uani 1 1 d . . . C19 C 1.3095(3) 0.4585(3) 1.22429(18) 0.0277(5) Uani 1 1 d . . . C20 C 1.2098(3) 0.4164(3) 1.13947(18) 0.0273(5) Uani 1 1 d . . . C21 C 1.1211(3) 0.2001(3) 0.87712(17) 0.0245(5) Uani 1 1 d . . . C22 C 1.2669(3) 0.2788(3) 0.86366(18) 0.0290(5) Uani 1 1 d . . . C23 C 1.3202(3) 0.2344(3) 0.77923(19) 0.0306(5) Uani 1 1 d . . . C24 C 1.2270(3) 0.1071(3) 0.70735(17) 0.0262(5) Uani 1 1 d . . . C25 C 1.0806(3) 0.0269(3) 0.71797(18) 0.0279(5) Uani 1 1 d . . . C26 C 1.0290(3) 0.0724(3) 0.80270(18) 0.0260(5) Uani 1 1 d . . . H1 H 0.606(4) 0.346(4) 1.314(3) 0.061(11) Uiso 1 1 d . . . H2 H 0.627(4) 0.185(4) 0.573(3) 0.050(10) Uiso 1 1 d . . . H3 H 1.498(4) 0.498(4) 1.358(3) 0.064(11) Uiso 1 1 d . . . H4A H 1.374(5) 0.106(4) 0.627(3) 0.066(12) Uiso 1 1 d . . . H4 H 0.907(3) 0.127(3) 1.1259(19) 0.019(6) Uiso 1 1 d . . . H5 H 0.783(3) 0.140(3) 1.261(2) 0.033(8) Uiso 1 1 d . . . H7 H 0.686(3) 0.423(3) 1.172(2) 0.039(8) Uiso 1 1 d . . . H8 H 0.797(3) 0.402(3) 1.035(2) 0.035(8) Uiso 1 1 d . . . H10 H 1.007(3) 0.357(3) 0.8144(19) 0.021(6) Uiso 1 1 d . . . H11 H 0.858(3) 0.314(3) 0.666(2) 0.033(8) Uiso 1 1 d . . . H13 H 0.501(4) 0.055(3) 0.772(2) 0.041(9) Uiso 1 1 d . . . H14 H 0.641(3) 0.080(3) 0.916(2) 0.039(8) Uiso 1 1 d . . . H16 H 1.213(3) 0.122(3) 1.024(2) 0.030(7) Uiso 1 1 d . . . H17 H 1.387(3) 0.191(3) 1.166(2) 0.025(7) Uiso 1 1 d . . . H19 H 1.337(3) 0.548(3) 1.276(2) 0.042(8) Uiso 1 1 d . . . H20 H 1.173(3) 0.480(3) 1.131(2) 0.026(7) Uiso 1 1 d . . . H22 H 1.333(3) 0.369(3) 0.920(2) 0.029(7) Uiso 1 1 d . . . H23 H 1.418(4) 0.283(3) 0.773(2) 0.038(8) Uiso 1 1 d . . . H25 H 1.013(4) -0.066(4) 0.665(3) 0.052(10) Uiso 1 1 d . . . H26 H 0.923(3) 0.011(3) 0.814(2) 0.035(8) Uiso 1 1 d . . . O50 O 1.4346(3) 0.3363(2) 0.53937(16) 0.0474(5) Uani 1 1 d . B . C50 C 1.3329(3) 0.2485(3) 0.4745(2) 0.0406(7) Uani 1 1 d . . . C51 C 1.3243(4) 0.1157(4) 0.4083(2) 0.0430(7) Uani 1 1 d . B . C52 C 1.2151(5) 0.3951(5) 0.5050(4) 0.0863(16) Uani 1 1 d . . . H52A H 1.1970 0.3872 0.5727 0.104 Uiso 1 1 calc R A 1 H52B H 1.3096 0.4819 0.5104 0.104 Uiso 1 1 calc R A 1 O51 O 1.2217(3) 0.2683(3) 0.4473(2) 0.0433(7) Uani 0.75 1 d P B 1 C53 C 1.1035(14) 0.4062(12) 0.4587(12) 0.076(4) Uani 0.40 1 d P B 1 H53A H 1.0993 0.4907 0.4974 0.114 Uiso 0.40 1 calc PR B 1 H53B H 1.0100 0.3206 0.4541 0.114 Uiso 0.40 1 calc PR B 1 H53C H 1.1224 0.4152 0.3921 0.114 Uiso 0.40 1 calc PR B 1 C53A C 1.1264(13) 0.3438(16) 0.5772(11) 0.086(4) Uani 0.35 1 d P B 2 H53G H 1.0571 0.3810 0.5846 0.129 Uiso 0.35 1 calc PR B 2 H53H H 1.1886 0.3760 0.6408 0.129 Uiso 0.35 1 calc PR B 2 H53I H 1.0726 0.2392 0.5558 0.129 Uiso 0.35 1 calc PR B 2 O51A O 1.1845(16) 0.2210(15) 0.4830(10) 0.074(4) Uiso 0.25 1 d P B 3 C53B C 1.086(3) 0.380(3) 0.505(2) 0.094(9) Uiso 0.25 1 d P B 3 H53D H 1.0913 0.4736 0.5171 0.140 Uiso 0.25 1 calc PR B 3 H53E H 1.0421 0.3364 0.5574 0.140 Uiso 0.25 1 calc PR B 3 H53F H 1.0268 0.3183 0.4408 0.140 Uiso 0.25 1 calc PR B 3 H51A H 1.229(5) 0.029(5) 0.408(3) 0.075(13) Uiso 1 1 d . . . H51C H 1.319(5) 0.123(5) 0.348(4) 0.078(14) Uiso 1 1 d . . . H51B H 1.399(6) 0.093(5) 0.433(4) 0.103(17) Uiso 1 1 d . . . O60 O 0.7207(3) 0.2089(3) 0.47554(16) 0.0460(5) Uani 1 1 d . . . H60A H 0.694(4) 0.240(4) 0.428(3) 0.061(11) Uiso 1 1 d . . . H60B H 0.732(5) 0.130(5) 0.443(3) 0.076(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0459(12) 0.0577(13) 0.0282(9) 0.0206(9) 0.0183(8) 0.0369(11) O2 0.0286(10) 0.0625(13) 0.0230(9) 0.0143(9) 0.0020(7) 0.0244(9) O3 0.0360(10) 0.0394(11) 0.0263(9) -0.0025(8) -0.0089(8) 0.0231(9) O4 0.0319(10) 0.0502(12) 0.0248(9) 0.0029(8) 0.0080(8) 0.0216(10) C1 0.0245(11) 0.0278(12) 0.0198(10) 0.0061(9) 0.0021(9) 0.0134(10) C2 0.0248(11) 0.0284(12) 0.0186(10) 0.0069(9) 0.0040(9) 0.0139(10) C3 0.0232(11) 0.0295(12) 0.0181(10) 0.0055(9) 0.0022(9) 0.0132(10) C4 0.0289(13) 0.0330(13) 0.0263(12) 0.0080(10) 0.0042(10) 0.0195(11) C5 0.0353(14) 0.0377(14) 0.0251(12) 0.0140(10) 0.0084(10) 0.0226(12) C6 0.0278(12) 0.0368(13) 0.0203(11) 0.0076(10) 0.0054(9) 0.0182(11) C7 0.0304(13) 0.0341(13) 0.0284(12) 0.0081(10) 0.0055(10) 0.0215(11) C8 0.0289(12) 0.0339(13) 0.0231(11) 0.0109(10) 0.0056(9) 0.0180(11) C9 0.0238(11) 0.0298(12) 0.0191(10) 0.0064(9) 0.0038(9) 0.0159(10) C10 0.0200(11) 0.0277(12) 0.0228(11) 0.0060(9) 0.0015(9) 0.0108(10) C11 0.0274(12) 0.0317(12) 0.0199(11) 0.0084(9) 0.0053(9) 0.0162(10) C12 0.0263(12) 0.0328(13) 0.0183(10) 0.0041(9) 0.0013(9) 0.0174(10) C13 0.0201(12) 0.0386(14) 0.0264(12) 0.0084(10) 0.0026(9) 0.0125(11) C14 0.0252(12) 0.0370(14) 0.0221(11) 0.0093(10) 0.0056(9) 0.0149(11) C15 0.0219(11) 0.0286(12) 0.0212(11) 0.0056(9) 0.0029(9) 0.0130(10) C16 0.0298(13) 0.0280(12) 0.0232(11) 0.0001(9) 0.0003(9) 0.0163(10) C17 0.0307(13) 0.0325(13) 0.0265(12) 0.0038(10) -0.0003(10) 0.0193(11) C18 0.0225(11) 0.0293(12) 0.0207(11) 0.0027(9) -0.0002(9) 0.0121(10) C19 0.0262(12) 0.0272(12) 0.0251(12) -0.0009(9) 0.0004(9) 0.0131(10) C20 0.0258(12) 0.0297(12) 0.0284(12) 0.0051(10) 0.0000(10) 0.0164(10) C21 0.0234(11) 0.0303(12) 0.0226(11) 0.0069(9) 0.0029(9) 0.0155(10) C22 0.0255(12) 0.0311(13) 0.0243(12) 0.0029(10) 0.0020(10) 0.0111(11) C23 0.0228(12) 0.0365(14) 0.0291(13) 0.0081(11) 0.0067(10) 0.0120(11) C24 0.0270(12) 0.0355(13) 0.0193(11) 0.0068(9) 0.0056(9) 0.0181(11) C25 0.0241(12) 0.0304(13) 0.0247(12) 0.0015(10) -0.0004(9) 0.0126(10) C26 0.0223(11) 0.0304(12) 0.0259(12) 0.0083(10) 0.0041(9) 0.0129(10) O50 0.0526(13) 0.0383(11) 0.0392(11) -0.0011(9) -0.0097(10) 0.0183(10) C50 0.0422(16) 0.0396(16) 0.0345(14) 0.0011(12) 0.0003(12) 0.0198(13) C51 0.0499(19) 0.0380(16) 0.0341(16) -0.0002(12) -0.0002(14) 0.0207(15) C52 0.059(3) 0.060(3) 0.120(4) -0.011(3) 0.014(3) 0.029(2) O51 0.0295(14) 0.0375(16) 0.0523(18) -0.0041(14) -0.0004(13) 0.0156(12) C53 0.069(7) 0.054(6) 0.118(11) 0.021(7) 0.014(7) 0.042(6) C53A 0.037(6) 0.083(9) 0.100(10) 0.021(8) 0.007(6) 0.000(6) O60 0.0635(15) 0.0588(14) 0.0271(10) 0.0158(10) 0.0120(10) 0.0368(12) _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 C6 1.380(3) . ? O1 H1 0.94(4) . ? O2 C12 1.374(3) . ? O2 H2 0.97(4) . ? O3 C18 1.380(3) . ? O3 H3 0.90(4) . ? O4 C24 1.373(3) . ? O4 H4A 0.90(4) . ? C1 C2 1.354(3) . ? C1 C15 1.495(3) . ? C1 C21 1.496(3) . ? C2 C9 1.489(3) . ? C2 C3 1.491(3) . ? C3 C8 1.395(3) . ? C3 C4 1.395(3) . ? C4 C5 1.385(4) . ? C4 H4 0.95(3) . ? C5 C6 1.386(4) . ? C5 H5 0.99(3) . ? C6 C7 1.385(4) . ? C7 C8 1.388(3) . ? C7 H7 0.95(3) . ? C8 H8 0.94(3) . ? C9 C10 1.397(3) . ? C9 C14 1.402(3) . ? C10 C11 1.384(3) . ? C10 H10 0.96(3) . ? C11 C12 1.388(4) . ? C11 H11 0.98(3) . ? C12 C13 1.386(4) . ? C13 C14 1.380(3) . ? C13 H13 0.91(3) . ? C14 H14 1.02(3) . ? C15 C20 1.392(3) . ? C15 C16 1.399(3) . ? C16 C17 1.377(4) . ? C16 H16 0.95(3) . ? C17 C18 1.389(3) . ? C17 H17 0.99(3) . ? C18 C19 1.382(3) . ? C19 C20 1.387(3) . ? C19 H19 0.98(3) . ? C20 H20 0.97(3) . ? C21 C22 1.390(4) . ? C21 C26 1.401(3) . ? C22 C23 1.388(4) . ? C22 H22 1.02(3) . ? C23 C24 1.384(4) . ? C23 H23 0.91(3) . ? C24 C25 1.386(4) . ? C25 C26 1.385(3) . ? C25 H25 1.01(4) . ? C26 H26 1.03(3) . ? O50 C50 1.206(4) . ? C50 O51 1.328(4) . ? C50 O51A 1.434(15) . ? C50 C51 1.482(4) . ? C51 H51A 1.00(5) . ? C51 H51C 0.87(5) . ? C51 H51B 0.99(5) . ? C52 C53B 1.26(3) . ? C52 C53 1.378(13) . ? C52 C53A 1.411(14) . ? C52 O51 1.457(5) . ? C52 O51A 1.719(15) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C53 H53C 0.9700 . ? C53A H53G 0.9700 . ? C53A H53H 0.9700 . ? C53A H53I 0.9700 . ? C53B H53D 0.9700 . ? C53B H53E 0.9700 . ? C53B H53F 0.9700 . ? O60 H60A 0.90(4) . ? O60 H60B 0.93(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 O1 H1 112(2) . . ? C12 O2 H2 110(2) . . ? C18 O3 H3 112(3) . . ? C24 O4 H4A 112(3) . . ? C2 C1 C15 123.3(2) . . ? C2 C1 C21 123.1(2) . . ? C15 C1 C21 113.6(2) . . ? C1 C2 C9 123.0(2) . . ? C1 C2 C3 123.1(2) . . ? C9 C2 C3 113.8(2) . . ? C8 C3 C4 117.6(2) . . ? C8 C3 C2 120.6(2) . . ? C4 C3 C2 121.7(2) . . ? C5 C4 C3 121.4(2) . . ? C5 C4 H4 117.4(15) . . ? C3 C4 H4 121.2(15) . . ? C4 C5 C6 119.5(2) . . ? C4 C5 H5 119.7(17) . . ? C6 C5 H5 120.5(17) . . ? O1 C6 C7 122.1(2) . . ? O1 C6 C5 117.3(2) . . ? C7 C6 C5 120.6(2) . . ? C6 C7 C8 119.1(2) . . ? C6 C7 H7 120.8(19) . . ? C8 C7 H7 120.1(19) . . ? C7 C8 C3 121.8(2) . . ? C7 C8 H8 114.7(18) . . ? C3 C8 H8 123.4(18) . . ? C10 C9 C14 117.3(2) . . ? C10 C9 C2 122.4(2) . . ? C14 C9 C2 120.2(2) . . ? C11 C10 C9 121.8(2) . . ? C11 C10 H10 119.1(15) . . ? C9 C10 H10 118.9(15) . . ? C10 C11 C12 119.3(2) . . ? C10 C11 H11 121.3(17) . . ? C12 C11 H11 119.3(17) . . ? O2 C12 C13 118.1(2) . . ? O2 C12 C11 121.5(2) . . ? C13 C12 C11 120.4(2) . . ? C14 C13 C12 119.6(2) . . ? C14 C13 H13 120(2) . . ? C12 C13 H13 120(2) . . ? C13 C14 C9 121.5(2) . . ? C13 C14 H14 117.8(18) . . ? C9 C14 H14 120.5(18) . . ? C20 C15 C16 117.6(2) . . ? C20 C15 C1 122.1(2) . . ? C16 C15 C1 120.2(2) . . ? C17 C16 C15 121.3(2) . . ? C17 C16 H16 120.4(17) . . ? C15 C16 H16 118.2(18) . . ? C16 C17 C18 119.8(2) . . ? C16 C17 H17 120.2(16) . . ? C18 C17 H17 119.9(16) . . ? O3 C18 C19 122.4(2) . . ? O3 C18 C17 117.4(2) . . ? C19 C18 C17 120.2(2) . . ? C18 C19 C20 119.4(2) . . ? C18 C19 H19 120.0(19) . . ? C20 C19 H19 120.6(19) . . ? C19 C20 C15 121.6(2) . . ? C19 C20 H20 118.3(17) . . ? C15 C20 H20 119.9(17) . . ? C22 C21 C26 117.7(2) . . ? C22 C21 C1 120.9(2) . . ? C26 C21 C1 121.3(2) . . ? C23 C22 C21 121.7(2) . . ? C23 C22 H22 121.7(16) . . ? C21 C22 H22 116.6(16) . . ? C24 C23 C22 119.3(2) . . ? C24 C23 H23 119.4(19) . . ? C22 C23 H23 121(2) . . ? O4 C24 C23 121.9(2) . . ? O4 C24 C25 117.7(2) . . ? C23 C24 C25 120.5(2) . . ? C26 C25 C24 119.5(2) . . ? C26 C25 H25 120(2) . . ? C24 C25 H25 120(2) . . ? C25 C26 C21 121.3(2) . . ? C25 C26 H26 120.4(17) . . ? C21 C26 H26 118.3(17) . . ? O50 C50 O51 122.9(3) . . ? O50 C50 O51A 121.5(6) . . ? O51 C50 O51A 32.4(5) . . ? O50 C50 C51 125.0(3) . . ? O51 C50 C51 111.7(3) . . ? O51A C50 C51 107.4(6) . . ? C50 C51 H51A 111(2) . . ? C50 C51 H51C 106(3) . . ? H51A C51 H51C 105(4) . . ? C50 C51 H51B 112(3) . . ? H51A C51 H51B 103(4) . . ? H51C C51 H51B 120(4) . . ? C53B C52 C53 33.0(12) . . ? C53B C52 C53A 57.2(13) . . ? C53 C52 C53A 90.1(9) . . ? C53B C52 O51 114.5(14) . . ? C53 C52 O51 109.7(6) . . ? C53A C52 O51 103.0(8) . . ? C53B C52 O51A 102.8(14) . . ? C53 C52 O51A 113.8(7) . . ? C53A C52 O51A 76.6(9) . . ? O51 C52 O51A 26.8(5) . . ? C53B C52 H52A 77.9 . . ? C53 C52 H52A 109.7 . . ? C53A C52 H52A 25.5 . . ? O51 C52 H52A 109.7 . . ? O51A C52 H52A 84.0 . . ? C53B C52 H52B 129.9 . . ? C53 C52 H52B 109.7 . . ? C53A C52 H52B 132.1 . . ? O51 C52 H52B 109.7 . . ? O51A C52 H52B 127.1 . . ? H52A C52 H52B 108.2 . . ? C50 O51 C52 118.3(3) . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C53A H53G 109.5 . . ? C52 C53A H53H 109.5 . . ? H53G C53A H53H 109.5 . . ? C52 C53A H53I 109.5 . . ? H53G C53A H53I 109.5 . . ? H53H C53A H53I 109.5 . . ? C50 O51A C52 98.3(8) . . ? C52 C53B H53D 109.5 . . ? C52 C53B H53E 109.5 . . ? H53D C53B H53E 109.5 . . ? C52 C53B H53F 109.5 . . ? H53D C53B H53F 109.5 . . ? H53E C53B H53F 109.5 . . ? H60A O60 H60B 107(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 C1 C2 C9 170.7(2) . . . . ? C21 C1 C2 C9 -10.3(4) . . . . ? C15 C1 C2 C3 -11.0(4) . . . . ? C21 C1 C2 C3 168.1(2) . . . . ? C1 C2 C3 C8 137.6(3) . . . . ? C9 C2 C3 C8 -43.9(3) . . . . ? C1 C2 C3 C4 -46.2(4) . . . . ? C9 C2 C3 C4 132.3(2) . . . . ? C8 C3 C4 C5 0.0(4) . . . . ? C2 C3 C4 C5 -176.2(2) . . . . ? C3 C4 C5 C6 0.4(4) . . . . ? C4 C5 C6 O1 178.3(2) . . . . ? C4 C5 C6 C7 -0.7(4) . . . . ? O1 C6 C7 C8 -178.3(2) . . . . ? C5 C6 C7 C8 0.7(4) . . . . ? C6 C7 C8 C3 -0.3(4) . . . . ? C4 C3 C8 C7 -0.1(4) . . . . ? C2 C3 C8 C7 176.2(2) . . . . ? C1 C2 C9 C10 -43.9(4) . . . . ? C3 C2 C9 C10 137.6(2) . . . . ? C1 C2 C9 C14 138.9(3) . . . . ? C3 C2 C9 C14 -39.6(3) . . . . ? C14 C9 C10 C11 -0.3(4) . . . . ? C2 C9 C10 C11 -177.6(2) . . . . ? C9 C10 C11 C12 -0.2(4) . . . . ? C10 C11 C12 O2 179.2(2) . . . . ? C10 C11 C12 C13 0.2(4) . . . . ? O2 C12 C13 C14 -178.6(2) . . . . ? C11 C12 C13 C14 0.4(4) . . . . ? C12 C13 C14 C9 -0.9(4) . . . . ? C10 C9 C14 C13 0.9(4) . . . . ? C2 C9 C14 C13 178.2(2) . . . . ? C2 C1 C15 C20 -47.6(4) . . . . ? C21 C1 C15 C20 133.3(2) . . . . ? C2 C1 C15 C16 134.5(3) . . . . ? C21 C1 C15 C16 -44.6(3) . . . . ? C20 C15 C16 C17 0.1(4) . . . . ? C1 C15 C16 C17 178.0(2) . . . . ? C15 C16 C17 C18 -0.3(4) . . . . ? C16 C17 C18 O3 -178.2(2) . . . . ? C16 C17 C18 C19 0.6(4) . . . . ? O3 C18 C19 C20 177.9(2) . . . . ? C17 C18 C19 C20 -0.8(4) . . . . ? C18 C19 C20 C15 0.7(4) . . . . ? C16 C15 C20 C19 -0.3(4) . . . . ? C1 C15 C20 C19 -178.2(2) . . . . ? C2 C1 C21 C22 136.9(3) . . . . ? C15 C1 C21 C22 -44.0(3) . . . . ? C2 C1 C21 C26 -46.8(4) . . . . ? C15 C1 C21 C26 132.3(2) . . . . ? C26 C21 C22 C23 0.7(4) . . . . ? C1 C21 C22 C23 177.2(2) . . . . ? C21 C22 C23 C24 -1.3(4) . . . . ? C22 C23 C24 O4 -177.3(2) . . . . ? C22 C23 C24 C25 1.9(4) . . . . ? O4 C24 C25 C26 177.2(2) . . . . ? C23 C24 C25 C26 -2.0(4) . . . . ? C24 C25 C26 C21 1.5(4) . . . . ? C22 C21 C26 C25 -0.8(4) . . . . ? C1 C21 C26 C25 -177.3(2) . . . . ? O50 C50 O51 C52 -6.2(6) . . . . ? O51A C50 O51 C52 91.8(12) . . . . ? C51 C50 O51 C52 -179.7(4) . . . . ? C53B C52 O51 C50 -151.9(15) . . . . ? C53 C52 O51 C50 172.8(8) . . . . ? C53A C52 O51 C50 -92.3(7) . . . . ? O51A C52 O51 C50 -83.2(12) . . . . ? O50 C50 O51A C52 54.1(9) . . . . ? O51 C50 O51A C52 -49.0(8) . . . . ? C51 C50 O51A C52 -152.2(5) . . . . ? C53B C52 O51A C50 174.5(15) . . . . ? C53 C52 O51A C50 141.7(10) . . . . ? C53A C52 O51A C50 -134.2(9) . . . . ? O51 C52 O51A C50 54.9(9) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.98 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.307 _refine_diff_density_min -0.301 _refine_diff_density_rms 0.064 #===END