# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 188/237 data_5.xylene _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '4-(triphenylmethyl)benzoic acid xylene clathrate ' _chemical_formula_moiety ' (C26 H20 O2). 0.5(C8 H10)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum '(C26 H20 O2). 0.5(C8 H10) ' _chemical_formula_weight 417.50 _chemical_melting_point ' 269 deg C ' _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3270(10) _cell_length_b 9.042(2) _cell_length_c 18.534(4) _cell_angle_alpha 88.09(3) _cell_angle_beta 85.07(3) _cell_angle_gamma 68.07(3) _cell_volume 1134.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method ? _exptl_crystal_F_000 500 _exptl_absorpt_coefficient_mu 0.084 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4264 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0622 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3986 _reflns_number_observed 2351 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.1139P)^2^+0.4342P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0227(61) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3986 _refine_ls_number_parameters 290 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1282 _refine_ls_R_factor_obs 0.0660 _refine_ls_wR_factor_all 0.2253 _refine_ls_wR_factor_obs 0.1878 _refine_ls_goodness_of_fit_all 1.038 _refine_ls_goodness_of_fit_obs 1.153 _refine_ls_restrained_S_all 1.040 _refine_ls_restrained_S_obs 1.155 _refine_ls_shift/esd_max 1.994 _refine_ls_shift/esd_mean 0.435 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group C1 C 0.1578(4) 0.1980(3) 0.8062(2) 0.0405(7) Uani 1 d . . C2 C 0.3127(4) 0.1650(4) 0.7407(2) 0.0424(7) Uani 1 d . . C3 C 0.4197(5) 0.2648(4) 0.7283(2) 0.0483(8) Uani 1 d . . H3A H 0.3891(5) 0.3557(4) 0.7590(2) 0.060 Uiso 1 d R . C4 C 0.5677(5) 0.2363(4) 0.6728(2) 0.0501(8) Uani 1 d . . H4A H 0.6396(5) 0.3059(4) 0.6659(2) 0.060 Uiso 1 d R . C5 C 0.6121(5) 0.1065(4) 0.6274(2) 0.0518(8) Uani 1 d . . C6 C 0.5038(5) 0.0101(5) 0.6373(2) 0.0627(10) Uani 1 d . . H6A H 0.5299(5) -0.0772(5) 0.6048(2) 0.080 Uiso 1 d R . C7 C 0.3575(5) 0.0385(4) 0.6930(2) 0.0560(9) Uani 1 d . . H7A H 0.2842(5) -0.0303(4) 0.6992(2) 0.060 Uiso 1 d R . C8 C 0.7784(5) 0.0653(5) 0.5708(2) 0.0618(10) Uani 1 d . . O1 O 0.9004(4) 0.1362(4) 0.57371(15) 0.0773(9) Uani 1 d . . H1O H 1.0451(4) 0.0833(4) 0.53638(15) 0.100 Uiso 1 d R . O2 O 0.7963(4) -0.0369(4) 0.5241(2) 0.0923(10) Uani 1 d . . C9 C -0.0491(5) 0.4394(4) 0.7315(2) 0.0538(8) Uani 1 d . . H9A H 0.0612(5) 0.4176(4) 0.6961(2) 0.060 Uiso 1 d R . C10 C -0.2251(6) 0.5672(5) 0.7206(2) 0.0685(11) Uani 1 d . . H10A H -0.2341(6) 0.6330(5) 0.6783(2) 0.080 Uiso 1 d R . C11 C -0.3846(6) 0.5993(4) 0.7710(2) 0.0699(11) Uani 1 d . . H11A H -0.5046(6) 0.6883(4) 0.7641(2) 0.080 Uiso 1 d R . C12 C -0.3712(5) 0.5037(4) 0.8307(2) 0.0610(10) Uani 1 d . . H12A H -0.4827(5) 0.5254(4) 0.8656(2) 0.080 Uiso 1 d R . C13 C -0.1972(5) 0.3762(4) 0.8408(2) 0.0509(8) Uani 1 d . . H13A H -0.1907(5) 0.3092(4) 0.8826(2) 0.060 Uiso 1 d R . C14 C -0.0318(4) 0.3425(4) 0.7919(2) 0.0426(7) Uani 1 d . . C15 C 0.1809(5) 0.3633(4) 0.9147(2) 0.0499(8) Uani 1 d . . H15A H 0.0549(5) 0.4428(4) 0.9054(2) 0.060 Uiso 1 d R . C16 C 0.2799(5) 0.3845(5) 0.9713(2) 0.0612(10) Uani 1 d . . H16A H 0.2225(5) 0.4785(5) 1.0008(2) 0.080 Uiso 1 d R . C17 C 0.4598(6) 0.2719(5) 0.9861(2) 0.0622(10) Uani 1 d . . H17A H 0.5269(6) 0.2859(5) 1.0261(2) 0.080 Uiso 1 d R . C18 C 0.5436(5) 0.1383(5) 0.9424(2) 0.0575(9) Uani 1 d . . H18A H 0.6702(5) 0.0596(5) 0.9515(2) 0.080 Uiso 1 d R . C19 C 0.4445(5) 0.1189(4) 0.8857(2) 0.0505(8) Uani 1 d . . H19A H 0.5046(5) 0.0264(4) 0.8555(2) 0.060 Uiso 1 d R . C20 C 0.2600(4) 0.2287(4) 0.8710(2) 0.0417(7) Uani 1 d . . C21 C -0.0203(5) 0.0212(4) 0.7734(2) 0.0513(8) Uani 1 d . . H21A H -0.0541(5) 0.0863(4) 0.7309(2) 0.060 Uiso 1 d R . C22 C -0.0852(5) -0.1034(4) 0.7842(2) 0.0612(10) Uani 1 d . . H22A H -0.1610(5) -0.1250(4) 0.7491(2) 0.080 Uiso 1 d R . C23 C -0.0408(6) -0.1971(5) 0.8454(3) 0.0734(12) Uani 1 d . . H23A H -0.0861(6) -0.2835(5) 0.8535(3) 0.080 Uiso 1 d R . C24 C 0.0677(6) -0.1648(5) 0.8950(2) 0.0729(12) Uani 1 d . . H24A H 0.0992(6) -0.2295(5) 0.9377(2) 0.080 Uiso 1 d R . C25 C 0.1343(5) -0.0395(4) 0.8838(2) 0.0560(9) Uani 1 d . . H25A H 0.2091(5) -0.0179(4) 0.9193(2) 0.060 Uiso 1 d R . C26 C 0.0926(4) 0.0549(4) 0.8220(2) 0.0437(7) Uani 1 d . . C27 C 0.3196(10) 0.5908(10) 0.5630(5) 0.101(3) Uiso 0.50 d PD . C28 C 0.2493(13) 0.4798(14) 0.5379(7) 0.118(4) Uiso 0.50 d PD . C29 C 0.3583(14) 0.3736(12) 0.4831(6) 0.142(5) Uiso 0.50 d PD . C30 C 0.5350(16) 0.3811(16) 0.4520(7) 0.182(8) Uiso 0.50 d PD . C31 C 0.6105(12) 0.4862(14) 0.4798(7) 0.174(6) Uiso 0.50 d PD . C32 C 0.4970(12) 0.5975(12) 0.5322(6) 0.106(4) Uiso 0.50 d PD . C33 C 0.2016(16) 0.7058(14) 0.6217(6) 0.144(5) Uiso 0.50 d PD . C34 C 0.8126(22) 0.4800(31) 0.4531(15) 0.175(12) Uiso 0.33 d PD . C35 C 0.6465(60) 0.2735(65) 0.3900(27) 0.234(29) Uiso 0.17 d PD . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.041(2) 0.041(2) 0.038(2) -0.0031(13) -0.0011(13) -0.0139(13) C2 0.042(2) 0.047(2) 0.039(2) -0.0013(13) -0.0041(13) -0.0180(14) C3 0.049(2) 0.051(2) 0.046(2) -0.0071(14) 0.0028(15) -0.021(2) C4 0.047(2) 0.061(2) 0.046(2) -0.001(2) 0.0013(15) -0.025(2) C5 0.044(2) 0.066(2) 0.044(2) -0.008(2) 0.0030(14) -0.020(2) C6 0.062(2) 0.071(2) 0.058(2) -0.022(2) 0.013(2) -0.030(2) C7 0.057(2) 0.058(2) 0.058(2) -0.014(2) 0.008(2) -0.029(2) C8 0.058(2) 0.080(3) 0.050(2) -0.012(2) 0.008(2) -0.030(2) O1 0.062(2) 0.108(2) 0.069(2) -0.024(2) 0.0224(13) -0.044(2) O2 0.083(2) 0.123(3) 0.080(2) -0.049(2) 0.035(2) -0.054(2) C9 0.053(2) 0.057(2) 0.051(2) 0.004(2) -0.007(2) -0.021(2) C10 0.071(3) 0.057(2) 0.073(3) 0.015(2) -0.023(2) -0.017(2) C11 0.053(2) 0.053(2) 0.095(3) -0.005(2) -0.025(2) -0.006(2) C12 0.044(2) 0.059(2) 0.076(3) -0.012(2) -0.004(2) -0.013(2) C13 0.043(2) 0.055(2) 0.054(2) -0.004(2) -0.0011(15) -0.019(2) C14 0.044(2) 0.042(2) 0.045(2) -0.0038(14) -0.0056(14) -0.0186(14) C15 0.045(2) 0.056(2) 0.047(2) -0.005(2) -0.0023(14) -0.016(2) C16 0.066(2) 0.069(2) 0.051(2) -0.015(2) -0.003(2) -0.027(2) C17 0.064(2) 0.080(3) 0.051(2) -0.006(2) -0.011(2) -0.034(2) C18 0.049(2) 0.069(2) 0.055(2) 0.001(2) -0.010(2) -0.021(2) C19 0.044(2) 0.057(2) 0.049(2) -0.006(2) -0.0027(15) -0.016(2) C20 0.040(2) 0.050(2) 0.037(2) 0.0006(13) -0.0004(13) -0.0194(14) C21 0.051(2) 0.052(2) 0.054(2) 0.000(2) -0.006(2) -0.022(2) C22 0.060(2) 0.057(2) 0.073(2) -0.004(2) -0.008(2) -0.028(2) C23 0.067(3) 0.055(2) 0.108(3) 0.011(2) -0.011(2) -0.034(2) C24 0.075(3) 0.063(2) 0.087(3) 0.028(2) -0.019(2) -0.032(2) C25 0.053(2) 0.057(2) 0.061(2) 0.008(2) -0.010(2) -0.024(2) C26 0.035(2) 0.045(2) 0.049(2) -0.0015(14) -0.0013(13) -0.0122(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.544(4) . ? C1 C14 1.546(4) . ? C1 C26 1.549(4) . ? C1 C20 1.553(4) . ? C2 C7 1.391(4) . ? C2 C3 1.402(4) . ? C3 C4 1.384(4) . ? C4 C5 1.388(5) . ? C5 C6 1.380(5) . ? C5 C8 1.480(5) . ? C6 C7 1.380(5) . ? C8 O2 1.250(4) . ? C8 O1 1.285(4) . ? C9 C14 1.383(4) . ? C9 C10 1.398(5) . ? C10 C11 1.378(6) . ? C11 C12 1.369(6) . ? C12 C13 1.385(5) . ? C13 C14 1.392(4) . ? C15 C16 1.383(5) . ? C15 C20 1.390(4) . ? C16 C17 1.375(5) . ? C17 C18 1.386(5) . ? C18 C19 1.378(5) . ? C19 C20 1.390(4) . ? C21 C22 1.380(5) . ? C21 C26 1.387(4) . ? C22 C23 1.379(6) . ? C23 C24 1.371(6) . ? C24 C25 1.394(5) . ? C25 C26 1.391(5) . ? C27 C31 1.039(14) 2_666 ? C27 C30 1.193(11) 2_666 ? C27 C32 1.3958(10) . ? C27 C28 1.3962(10) . ? C27 C34 1.401(13) 2_666 ? C27 C33 1.5012(11) . ? C27 C35 1.631(14) 2_666 ? C28 C34 0.48(2) 2_666 ? C28 C31 1.194(11) 2_666 ? C28 C29 1.3941(11) . ? C29 C32 1.193(11) 2_666 ? C29 C30 1.3957(10) . ? C29 C31 1.560(14) 2_666 ? C29 C34 1.826(13) 2_666 ? C30 C32 0.370(14) 2_666 ? C30 C27 1.193(11) 2_666 ? C30 C31 1.3968(10) . ? C30 C35 1.5016(12) . ? C30 C31 1.757(13) 2_666 ? C31 C27 1.039(14) 2_666 ? C31 C28 1.194(11) 2_666 ? C31 C32 1.316(13) 2_666 ? C31 C32 1.3951(11) . ? C31 C34 1.5016(10) . ? C31 C29 1.560(14) 2_666 ? C31 C31 1.657(11) 2_666 ? C31 C30 1.757(13) 2_666 ? C32 C30 0.370(14) 2_666 ? C32 C29 1.193(11) 2_666 ? C32 C31 1.316(13) 2_666 ? C32 C35 1.867(14) 2_666 ? C33 C35 1.196(14) 2_666 ? C34 C28 0.48(2) 2_666 ? C34 C27 1.401(13) 2_666 ? C34 C29 1.826(13) 2_666 ? C35 C33 1.196(14) 2_666 ? C35 C27 1.631(14) 2_666 ? C35 C32 1.867(14) 2_666 ? 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 C14 111.3(2) . . ? C2 C1 C26 111.5(2) . . ? C14 C1 C26 106.1(2) . . ? C2 C1 C20 105.5(2) . . ? C14 C1 C20 111.6(2) . . ? C26 C1 C20 110.8(2) . . ? C7 C2 C3 116.8(3) . . ? C7 C2 C1 123.9(3) . . ? C3 C2 C1 119.2(3) . . ? C4 C3 C2 121.8(3) . . ? C3 C4 C5 119.8(3) . . ? C6 C5 C4 119.1(3) . . ? C6 C5 C8 119.4(3) . . ? C4 C5 C8 121.4(3) . . ? C7 C6 C5 120.8(3) . . ? C6 C7 C2 121.5(3) . . ? O2 C8 O1 123.4(3) . . ? O2 C8 C5 119.6(3) . . ? O1 C8 C5 117.0(3) . . ? C14 C9 C10 121.2(3) . . ? C11 C10 C9 119.9(4) . . ? C12 C11 C10 119.8(3) . . ? C11 C12 C13 120.0(4) . . ? C12 C13 C14 121.7(3) . . ? C9 C14 C13 117.3(3) . . ? C9 C14 C1 123.5(3) . . ? C13 C14 C1 119.2(3) . . ? C16 C15 C20 121.3(3) . . ? C17 C16 C15 120.7(3) . . ? C16 C17 C18 119.1(3) . . ? C19 C18 C17 119.8(3) . . ? C18 C19 C20 122.2(3) . . ? C19 C20 C15 117.0(3) . . ? C19 C20 C1 119.0(3) . . ? C15 C20 C1 124.0(3) . . ? C22 C21 C26 122.0(3) . . ? C23 C22 C21 120.0(4) . . ? C24 C23 C22 119.4(3) . . ? C23 C24 C25 120.6(4) . . ? C26 C25 C24 120.8(3) . . ? C21 C26 C25 117.3(3) . . ? C21 C26 C1 118.7(3) . . ? C25 C26 C1 123.9(3) . . ? C31 C27 C30 77.2(7) 2_666 2_666 ? C31 C27 C32 63.4(6) 2_666 . ? C30 C27 C32 13.8(7) 2_666 . ? C31 C27 C28 56.5(6) 2_666 . ? C30 C27 C28 133.5(7) 2_666 . ? C32 C27 C28 119.87(9) . . ? C31 C27 C34 74.3(8) 2_666 2_666 ? C30 C27 C34 150.8(13) 2_666 2_666 ? C32 C27 C34 137.2(7) . 2_666 ? C28 C27 C34 19.9(8) . 2_666 ? C31 C27 C33 174.8(12) 2_666 . ? C30 C27 C33 106.5(7) 2_666 . ? C32 C27 C33 120.13(13) . . ? C28 C27 C33 119.97(13) . . ? C34 C27 C33 101.6(6) 2_666 . ? C31 C27 C35 139.1(9) 2_666 2_666 ? C30 C27 C35 62.0(6) 2_666 2_666 ? C32 C27 C35 75.7(4) . 2_666 ? C28 C27 C35 164.2(7) . 2_666 ? C34 C27 C35 146.2(10) 2_666 2_666 ? C33 C27 C35 44.7(5) . 2_666 ? C34 C28 C31 120.9(29) 2_666 2_666 ? C34 C28 C29 148.9(45) 2_666 . ? C31 C28 C29 73.7(7) 2_666 . ? C34 C28 C27 80.6(16) 2_666 . ? C31 C28 C27 46.5(7) 2_666 . ? C29 C28 C27 120.04(8) . . ? C32 C29 C28 106.3(7) 2_666 . ? C32 C29 C30 13.8(7) 2_666 . ? C28 C29 C30 119.98(9) . . ? C32 C29 C31 59.1(6) 2_666 2_666 ? C28 C29 C31 47.3(4) . 2_666 ? C30 C29 C31 72.7(4) . 2_666 ? C32 C29 C34 110.9(9) 2_666 2_666 ? C28 C29 C34 7.9(13) . 2_666 ? C30 C29 C34 124.2(5) . 2_666 ? C31 C29 C34 51.9(4) 2_666 2_666 ? C32 C30 C27 116.2(24) 2_666 2_666 ? C32 C30 C29 50.1(19) 2_666 . ? C27 C30 C29 166.3(7) 2_666 . ? C32 C30 C31 69.8(19) 2_666 . ? C27 C30 C31 46.5(7) 2_666 . ? C29 C30 C31 119.85(11) . . ? C32 C30 C35 169.7(26) 2_666 . ? C27 C30 C35 73.5(7) 2_666 . ? C29 C30 C35 120.14(14) . . ? C31 C30 C35 119.99(14) . . ? C32 C30 C31 10.6(27) 2_666 2_666 ? C27 C30 C31 108.5(9) 2_666 2_666 ? C29 C30 C31 58.0(4) . 2_666 ? C31 C30 C31 62.2(4) . 2_666 ? C35 C30 C31 175.6(30) . 2_666 ? C27 C31 C28 77.0(7) 2_666 2_666 ? C27 C31 C32 71.6(8) 2_666 2_666 ? C28 C31 C32 148.5(13) 2_666 2_666 ? C27 C31 C32 172.9(14) 2_666 . ? C28 C31 C32 106.2(7) 2_666 . ? C32 C31 C32 104.7(6) 2_666 . ? C27 C31 C30 56.4(6) 2_666 . ? C28 C31 C30 133.3(7) 2_666 . ? C32 C31 C30 15.3(6) 2_666 . ? C32 C31 C30 119.74(11) . . ? C27 C31 C34 63.9(6) 2_666 . ? C28 C31 C34 16.1(11) 2_666 . ? C32 C31 C34 135.0(6) 2_666 . ? C32 C31 C34 120.24(14) . . ? C30 C31 C34 120.01(14) . . ? C27 C31 C29 135.9(10) 2_666 2_666 ? C28 C31 C29 59.1(6) 2_666 2_666 ? C32 C31 C29 151.8(9) 2_666 2_666 ? C32 C31 C29 47.2(4) . 2_666 ? C30 C31 C29 166.2(6) . 2_666 ? C34 C31 C29 73.2(4) . 2_666 ? C27 C31 C31 125.8(10) 2_666 2_666 ? C28 C31 C31 155.8(12) 2_666 2_666 ? C32 C31 C31 54.5(4) 2_666 2_666 ? C32 C31 C31 50.2(5) . 2_666 ? C30 C31 C31 69.6(5) . 2_666 ? C34 C31 C31 170.2(7) . 2_666 ? C29 C31 C31 97.3(7) 2_666 2_666 ? C27 C31 C30 172.9(14) 2_666 2_666 ? C28 C31 C30 108.4(9) 2_666 2_666 ? C32 C31 C30 102.7(6) 2_666 2_666 ? C32 C31 C30 2.8(7) . 2_666 ? C30 C31 C30 117.8(4) . 2_666 ? C34 C31 C30 122.1(4) . 2_666 ? C29 C31 C30 49.3(4) 2_666 2_666 ? C31 C31 C30 48.2(3) 2_666 2_666 ? C30 C32 C29 116.1(24) 2_666 2_666 ? C30 C32 C31 94.9(19) 2_666 2_666 ? C29 C32 C31 148.9(12) 2_666 2_666 ? C30 C32 C31 166.6(34) 2_666 . ? C29 C32 C31 73.7(7) 2_666 . ? C31 C32 C31 75.3(6) 2_666 . ? C30 C32 C27 50.1(19) 2_666 . ? C29 C32 C27 166.2(7) 2_666 . ? C31 C32 C27 44.9(6) 2_666 . ? C31 C32 C27 119.99(10) . . ? C30 C32 C35 8.3(21) 2_666 2_666 ? C29 C32 C35 108.3(9) 2_666 2_666 ? C31 C32 C35 102.8(7) 2_666 2_666 ? C31 C32 C35 173.2(24) . 2_666 ? C27 C32 C35 57.9(4) . 2_666 ? C35 C33 C27 73.4(7) 2_666 . ? C28 C34 C27 79.4(15) 2_666 2_666 ? C28 C34 C31 43.0(19) 2_666 . ? C27 C34 C31 41.8(5) 2_666 . ? C28 C34 C29 23.2(32) 2_666 2_666 ? C27 C34 C29 96.1(6) 2_666 2_666 ? C31 C34 C29 54.9(4) . 2_666 ? C33 C35 C30 106.3(8) 2_666 . ? C33 C35 C27 61.9(6) 2_666 2_666 ? C30 C35 C27 44.5(4) . 2_666 ? C33 C35 C32 108.1(10) 2_666 2_666 ? C30 C35 C32 2.0(5) . 2_666 ? C27 C35 C32 46.4(4) 2_666 2_666 ? _refine_diff_density_max 0.709 _refine_diff_density_min -0.252 _refine_diff_density_rms 0.054 data_5.Ph-Cl _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '4-(triphenylmethyl)benzoic acid chlorobenzene clathrate ' _chemical_formula_moiety ' (C26 H20 O2). 0.5(C6 H5 Cl)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum '(C26 H20 O2). 0.5(C6 H5 Cl) ' _chemical_formula_weight 420.69 _chemical_melting_point ' 245 deg C ' _chemical_compound_source ? 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3100(10) _cell_length_b 8.9940(10) _cell_length_c 18.454(2) _cell_angle_alpha 89.190(10) _cell_angle_beta 85.750(10) _cell_angle_gamma 68.230(10) _cell_volume 1123.5(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.244 _exptl_crystal_density_method ? _exptl_crystal_F_000 442 _exptl_absorpt_coefficient_mu 0.134 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4765 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0924 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.99 _reflns_number_total 4398 _reflns_number_observed 2212 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.1523P)^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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0152(71) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4396 _refine_ls_number_parameters 270 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1694 _refine_ls_R_factor_obs 0.0755 _refine_ls_wR_factor_all 0.2716 _refine_ls_wR_factor_obs 0.2204 _refine_ls_goodness_of_fit_all 1.039 _refine_ls_goodness_of_fit_obs 1.224 _refine_ls_restrained_S_all 1.047 _refine_ls_restrained_S_obs 1.224 _refine_ls_shift/esd_max 0.005 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group C1 C 0.1579(4) 0.1919(4) 0.8050(2) 0.0408(7) Uani 1 d . . C2 C 0.3134(5) 0.1570(4) 0.7394(2) 0.0420(8) Uani 1 d . . C3 C 0.4178(5) 0.2595(4) 0.7270(2) 0.0484(8) Uani 1 d . . H3A H 0.3872(5) 0.3504(4) 0.7577(2) 0.060 Uiso 1 d R . C4 C 0.5659(5) 0.2309(4) 0.6723(2) 0.0510(9) Uani 1 d . . H4A H 0.6379(5) 0.3005(4) 0.6654(2) 0.060 Uiso 1 d R . C5 C 0.6141(5) 0.0986(4) 0.6268(2) 0.0529(9) Uani 1 d . . C6 C 0.5078(6) 0.0000(5) 0.6369(2) 0.0613(10) Uani 1 d . . H6A H 0.5340(6) -0.0874(5) 0.6045(2) 0.080 Uiso 1 d R . C7 C 0.3601(5) 0.0280(4) 0.6924(2) 0.0533(9) Uani 1 d . . H7A H 0.2868(5) -0.0407(4) 0.6986(2) 0.060 Uiso 1 d R . C8 C 0.7795(6) 0.0579(5) 0.5710(2) 0.0643(11) Uani 1 d . . O1 O 0.8956(5) 0.1347(4) 0.5725(2) 0.0855(10) Uani 1 d . . H1O H 1.0403(5) 0.0818(4) 0.5352(2) 0.100 Uiso 1 d R . O2 O 0.8018(5) -0.0495(4) 0.5242(2) 0.0944(11) Uani 1 d . . C9 C -0.0491(6) 0.4325(4) 0.7295(2) 0.0540(9) Uani 1 d . . H9A H 0.0612(6) 0.4107(4) 0.6941(2) 0.060 Uiso 1 d R . C10 C -0.2271(6) 0.5593(5) 0.7188(2) 0.0673(11) Uani 1 d . . H10A H -0.2362(6) 0.6252(5) 0.6766(2) 0.080 Uiso 1 d R . C11 C -0.3872(6) 0.5927(5) 0.7678(3) 0.0699(12) Uani 1 d . . H11A H -0.5072(6) 0.6817(5) 0.7609(3) 0.080 Uiso 1 d R . C12 C -0.3723(5) 0.4981(4) 0.8288(2) 0.0623(11) Uani 1 d . . H12A H -0.4838(5) 0.5197(4) 0.8636(2) 0.080 Uiso 1 d R . C13 C -0.1980(5) 0.3719(4) 0.8390(2) 0.0522(9) Uani 1 d . . H13A H -0.1915(5) 0.3049(4) 0.8808(2) 0.060 Uiso 1 d R . C14 C -0.0323(5) 0.3375(4) 0.7901(2) 0.0440(8) Uani 1 d . . C15 C 0.1804(5) 0.3617(4) 0.9141(2) 0.0491(8) Uani 1 d . . H15A H 0.0544(5) 0.4412(4) 0.9049(2) 0.060 Uiso 1 d R . C16 C 0.2801(6) 0.3844(5) 0.9710(2) 0.0619(10) Uani 1 d . . H16A H 0.2227(6) 0.4784(5) 1.0004(2) 0.080 Uiso 1 d R . C17 C 0.4609(6) 0.2725(5) 0.9867(2) 0.0642(11) Uani 1 d . . H17A H 0.5279(6) 0.2865(5) 1.0267(2) 0.080 Uiso 1 d R . C18 C 0.5449(6) 0.1375(5) 0.9423(2) 0.0576(10) Uani 1 d . . H18A H 0.6716(6) 0.0589(5) 0.9514(2) 0.080 Uiso 1 d R . C19 C 0.4444(5) 0.1151(4) 0.8849(2) 0.0507(9) Uani 1 d . . H19A H 0.5046(5) 0.0226(4) 0.8547(2) 0.060 Uiso 1 d R . C20 C 0.2593(5) 0.2255(4) 0.8703(2) 0.0422(8) Uani 1 d . . C21 C -0.0192(5) 0.0116(4) 0.7711(2) 0.0515(9) Uani 1 d . . H21A H -0.0530(5) 0.0767(4) 0.7286(2) 0.060 Uiso 1 d R . C22 C -0.0826(6) -0.1130(5) 0.7816(2) 0.0617(10) Uani 1 d . . H22A H -0.1584(6) -0.1346(5) 0.7465(2) 0.080 Uiso 1 d R . C23 C -0.0400(6) -0.2042(5) 0.8420(3) 0.0733(13) Uani 1 d . . H23A H -0.0853(6) -0.2907(5) 0.8500(3) 0.080 Uiso 1 d R . C24 C 0.0679(6) -0.1688(5) 0.8932(3) 0.0724(12) Uani 1 d . . H24A H 0.0994(6) -0.2335(5) 0.9359(3) 0.080 Uiso 1 d R . C25 C 0.1322(5) -0.0438(4) 0.8821(2) 0.0559(10) Uani 1 d . . H25A H 0.2070(5) -0.0222(4) 0.9176(2) 0.060 Uiso 1 d R . C26 C 0.0924(5) 0.0482(4) 0.8203(2) 0.0429(8) Uani 1 d . . Cl1 Cl 0.3032(20) 0.6407(15) 0.5914(7) 0.180(4) Uiso 0.25 d P . C27 C 0.6341(16) 0.6026(11) 0.5117(6) 0.119(4) Uiso 0.50 d PG . C28 C 0.7942(11) 0.5263(11) 0.4625(5) 0.134(5) Uiso 0.50 d PG . C29 C 0.7970(12) 0.3981(11) 0.4206(5) 0.098(3) Uiso 0.50 d PG . C30 C 0.6396(15) 0.3463(11) 0.4279(5) 0.122(6) Uiso 0.50 d PG . C31 C 0.4794(13) 0.4227(15) 0.4772(7) 0.104(4) Uiso 0.50 d PG . C32 C 0.4766(14) 0.5508(16) 0.5191(7) 0.243(12) Uiso 0.50 d PG . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.039(2) 0.043(2) 0.043(2) -0.0005(14) -0.0012(14) -0.0176(14) C2 0.041(2) 0.048(2) 0.036(2) 0.0001(14) -0.0053(13) -0.0159(14) C3 0.054(2) 0.057(2) 0.041(2) -0.007(2) 0.000(2) -0.029(2) C4 0.049(2) 0.060(2) 0.049(2) -0.002(2) 0.003(2) -0.028(2) C5 0.048(2) 0.068(2) 0.044(2) -0.002(2) 0.000(2) -0.023(2) C6 0.064(2) 0.064(2) 0.058(2) -0.022(2) 0.012(2) -0.029(2) C7 0.057(2) 0.051(2) 0.056(2) -0.006(2) 0.004(2) -0.027(2) C8 0.062(2) 0.081(3) 0.053(2) -0.007(2) 0.006(2) -0.031(2) O1 0.076(2) 0.121(3) 0.073(2) -0.025(2) 0.025(2) -0.056(2) O2 0.090(2) 0.121(3) 0.081(2) -0.046(2) 0.035(2) -0.055(2) C9 0.059(2) 0.051(2) 0.053(2) 0.005(2) -0.010(2) -0.021(2) C10 0.071(3) 0.061(2) 0.071(3) 0.020(2) -0.027(2) -0.022(2) C11 0.054(2) 0.049(2) 0.100(3) -0.003(2) -0.024(2) -0.007(2) C12 0.048(2) 0.057(2) 0.080(3) -0.016(2) -0.007(2) -0.017(2) C13 0.047(2) 0.052(2) 0.057(2) -0.004(2) -0.004(2) -0.019(2) C14 0.043(2) 0.045(2) 0.048(2) -0.0012(15) -0.0077(15) -0.0199(15) C15 0.047(2) 0.051(2) 0.049(2) -0.001(2) -0.006(2) -0.017(2) C16 0.068(2) 0.068(2) 0.052(2) -0.016(2) -0.007(2) -0.027(2) C17 0.063(2) 0.088(3) 0.048(2) -0.007(2) -0.010(2) -0.034(2) C18 0.051(2) 0.069(2) 0.055(2) 0.006(2) -0.016(2) -0.024(2) C19 0.045(2) 0.057(2) 0.051(2) -0.003(2) -0.006(2) -0.018(2) C20 0.043(2) 0.050(2) 0.039(2) 0.0021(14) -0.0009(14) -0.024(2) C21 0.050(2) 0.049(2) 0.059(2) 0.004(2) -0.012(2) -0.021(2) C22 0.058(2) 0.056(2) 0.079(3) 0.002(2) -0.014(2) -0.030(2) C23 0.066(3) 0.056(2) 0.110(4) 0.008(2) -0.012(3) -0.037(2) C24 0.079(3) 0.063(2) 0.084(3) 0.030(2) -0.019(2) -0.035(2) C25 0.056(2) 0.055(2) 0.061(2) 0.011(2) -0.011(2) -0.024(2) C26 0.039(2) 0.042(2) 0.047(2) 0.0012(14) -0.0036(14) -0.0134(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C20 1.549(4) . ? C1 C2 1.549(4) . ? C1 C26 1.552(4) . ? C1 C14 1.555(4) . ? C2 C7 1.380(5) . ? C2 C3 1.406(5) . ? C3 C4 1.376(5) . ? C4 C5 1.385(5) . ? C5 C6 1.381(5) . ? C5 C8 1.469(5) . ? C6 C7 1.385(5) . ? C8 O2 1.262(5) . ? C8 O1 1.280(5) . ? C9 C14 1.382(5) . ? C9 C10 1.401(5) . ? C10 C11 1.366(6) . ? C11 C12 1.387(6) . ? C12 C13 1.380(5) . ? C13 C14 1.395(5) . ? C15 C16 1.379(5) . ? C15 C20 1.387(4) . ? C16 C17 1.381(5) . ? C17 C18 1.387(5) . ? C18 C19 1.390(5) . ? C19 C20 1.393(5) . ? C21 C22 1.369(5) . ? C21 C26 1.385(5) . ? C22 C23 1.359(6) . ? C23 C24 1.386(6) . ? C24 C25 1.378(5) . ? C25 C26 1.383(5) . ? Cl1 C30 0.57(2) 2_666 ? Cl1 C29 0.96(3) 2_666 ? Cl1 C32 1.749(13) . ? Cl1 C31 1.87(2) 2_666 ? Cl1 C28 2.17(3) 2_666 ? C27 C31 0.95(2) 2_666 ? C27 C28 1.39 . ? C27 C32 1.39 . ? C27 C32 1.95(2) 2_666 ? C28 C29 1.39 . ? C28 Cl1 2.165(15) 2_666 ? C29 Cl1 0.960(14) 2_666 ? C29 C30 1.39 . ? C30 Cl1 0.57(2) 2_666 ? C30 C32 1.36(2) 2_666 ? C30 C31 1.39 . ? C31 C32 0.475(14) 2_666 ? C31 C27 0.946(14) 2_666 ? C31 C32 1.39 . ? C31 C31 1.77(2) 2_666 ? C31 Cl1 1.87(2) 2_666 ? C32 C31 0.47(2) 2_666 ? C32 C32 1.09(2) 2_666 ? C32 C30 1.36(2) 2_666 ? C32 C27 1.95(2) 2_666 ? 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 C20 C1 C2 105.6(2) . . ? C20 C1 C26 111.0(2) . . ? C2 C1 C26 111.5(3) . . ? C20 C1 C14 111.5(3) . . ? C2 C1 C14 111.0(3) . . ? C26 C1 C14 106.3(2) . . ? C7 C2 C3 117.1(3) . . ? C7 C2 C1 123.9(3) . . ? C3 C2 C1 118.9(3) . . ? C4 C3 C2 122.2(3) . . ? C3 C4 C5 119.8(3) . . ? C6 C5 C4 118.5(3) . . ? C6 C5 C8 119.9(3) . . ? C4 C5 C8 121.5(3) . . ? C5 C6 C7 121.6(3) . . ? C2 C7 C6 120.7(3) . . ? O2 C8 O1 123.0(4) . . ? O2 C8 C5 119.5(4) . . ? O1 C8 C5 117.5(4) . . ? C14 C9 C10 120.4(4) . . ? C11 C10 C9 121.2(4) . . ? C10 C11 C12 119.0(3) . . ? C13 C12 C11 120.0(4) . . ? C12 C13 C14 121.8(4) . . ? C9 C14 C13 117.7(3) . . ? C9 C14 C1 123.6(3) . . ? C13 C14 C1 118.7(3) . . ? C16 C15 C20 121.0(3) . . ? C15 C16 C17 121.5(4) . . ? C16 C17 C18 118.4(3) . . ? C17 C18 C19 120.0(4) . . ? C18 C19 C20 121.7(3) . . ? C15 C20 C19 117.3(3) . . ? C15 C20 C1 124.2(3) . . ? C19 C20 C1 118.5(3) . . ? C22 C21 C26 121.8(3) . . ? C23 C22 C21 120.7(4) . . ? C22 C23 C24 119.1(4) . . ? C25 C24 C23 120.0(4) . . ? C24 C25 C26 121.4(4) . . ? C25 C26 C21 117.0(3) . . ? C25 C26 C1 124.0(3) . . ? C21 C26 C1 118.9(3) . . ? C30 Cl1 C29 128.2(39) 2_666 2_666 ? C30 Cl1 C32 40.0(23) 2_666 . ? C29 Cl1 C32 98.1(12) 2_666 . ? C30 Cl1 C31 27.8(17) 2_666 2_666 ? C29 Cl1 C31 112.5(17) 2_666 2_666 ? C32 Cl1 C31 14.6(7) . 2_666 ? C30 Cl1 C28 108.3(27) 2_666 2_666 ? C29 Cl1 C28 27.8(8) 2_666 2_666 ? C32 Cl1 C28 72.2(5) . 2_666 ? C31 Cl1 C28 86.7(9) 2_666 2_666 ? C31 C27 C28 128.2(11) 2_666 . ? C31 C27 C32 8.4(11) 2_666 . ? C28 C27 C32 120.0 . . ? C31 C27 C32 41.5(7) 2_666 2_666 ? C28 C27 C32 86.8(5) . 2_666 ? C32 C27 C32 33.2(5) . 2_666 ? C29 C28 C27 120.0 . . ? C29 C28 Cl1 18.8(5) . 2_666 ? C27 C28 Cl1 101.9(5) . 2_666 ? Cl1 C29 C30 18.9(11) 2_666 . ? Cl1 C29 C28 133.4(11) 2_666 . ? C30 C29 C28 120.0 . . ? Cl1 C30 C32 124.3(20) 2_666 2_666 ? Cl1 C30 C29 32.9(16) 2_666 . ? C32 C30 C29 100.2(6) 2_666 . ? Cl1 C30 C31 141.1(18) 2_666 . ? C32 C30 C31 19.8(6) 2_666 . ? C29 C30 C31 120.0 . . ? C32 C31 C27 154.7(36) 2_666 2_666 ? C32 C31 C30 76.7(24) 2_666 . ? C27 C31 C30 128.2(13) 2_666 . ? C32 C31 C32 43.4(23) 2_666 . ? C27 C31 C32 111.7(13) 2_666 . ? C30 C31 C32 120.0 . . ? C32 C31 C31 32.8(23) 2_666 2_666 ? C27 C31 C31 122.3(14) 2_666 2_666 ? C30 C31 C31 109.4(5) . 2_666 ? C32 C31 C31 10.7(5) . 2_666 ? C32 C31 Cl1 68.0(22) 2_666 2_666 ? C27 C31 Cl1 137.3(15) 2_666 2_666 ? C30 C31 Cl1 11.1(5) . 2_666 ? C32 C31 Cl1 110.7(5) . 2_666 ? C31 C31 Cl1 100.2(6) 2_666 2_666 ? C31 C32 C32 119.2(22) 2_666 2_666 ? C31 C32 C30 83.5(24) 2_666 2_666 ? C32 C32 C30 157.0(18) 2_666 2_666 ? C31 C32 C31 136.6(18) 2_666 . ? C32 C32 C31 17.3(6) 2_666 . ? C30 C32 C31 139.8(15) 2_666 . ? C31 C32 C27 16.9(19) 2_666 . ? C32 C32 C27 102.7(6) 2_666 . ? C30 C32 C27 100.2(15) 2_666 . ? C31 C32 C27 120.0 . . ? C31 C32 Cl1 97.5(20) 2_666 . ? C32 C32 Cl1 141.8(11) 2_666 . ? C30 C32 Cl1 15.7(11) 2_666 . ? C31 C32 Cl1 125.1(7) . . ? C27 C32 Cl1 114.4(7) . . ? C31 C32 C27 163.0(24) 2_666 2_666 ? C32 C32 C27 44.1(5) 2_666 2_666 ? C30 C32 C27 113.0(14) 2_666 2_666 ? C31 C32 C27 26.8(4) . 2_666 ? C27 C32 C27 146.8(4) . 2_666 ? Cl1 C32 C27 98.4(7) . 2_666 ? _refine_diff_density_max 0.636 _refine_diff_density_min -0.263 _refine_diff_density_rms 0.064 data_5.m-xylene _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '4-(triphenylmethyl)benzoic acid m-xylene clathrate ' _chemical_formula_moiety '(C26 H20 O2). 0.5(C8 H10)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum '(C26 H20 O2). 0.5(C8 H10) ' _chemical_formula_weight 417.50 _chemical_melting_point '246 deg C ' _chemical_compound_source ? 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 7.329(1) _cell_length_b 9.044(1) _cell_length_c 18.547(1) _cell_angle_alpha 88.54(1) _cell_angle_beta 85.33(1) _cell_angle_gamma 67.63(1) _cell_volume 1133.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5 _cell_measurement_theta_max 15 _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method ? _exptl_crystal_F_000 500 _exptl_absorpt_coefficient_mu 0.084 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.970 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; Rigaku RU-200 rotating-anode generator powered at 50kV and 90mA ; _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC7R' _diffrn_measurement_method '\w scan' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4258 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0593 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3982 _reflns_number_observed 2061 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'MSC/AFC Diffractometer Control' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL-PC' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 6 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0941P)^2^+0.1520P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0310(47) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3976 _refine_ls_number_parameters 299 _refine_ls_number_restraints 218 _refine_ls_R_factor_all 0.1199 _refine_ls_R_factor_obs 0.0519 _refine_ls_wR_factor_all 0.1925 _refine_ls_wR_factor_obs 0.1473 _refine_ls_goodness_of_fit_all 1.023 _refine_ls_goodness_of_fit_obs 1.133 _refine_ls_restrained_S_all 1.014 _refine_ls_restrained_S_obs 1.086 _refine_ls_shift/esd_max -0.003 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group C1 C 0.1579(3) 0.6955(3) 0.30607(12) 0.0435(6) Uani 1 d D . C2 C 0.3130(3) 0.6627(3) 0.23994(12) 0.0449(6) Uani 1 d D . C3 C 0.4171(4) 0.7629(3) 0.22817(13) 0.0516(6) Uani 1 d D . H3 H 0.3862(4) 0.8511(3) 0.25832(13) 0.062 Uiso 1 calc R . C4 C 0.5648(4) 0.7351(3) 0.17307(13) 0.0538(7) Uani 1 d D . H4 H 0.6333(4) 0.8031(3) 0.16691(13) 0.065 Uiso 1 calc R . C5 C 0.6108(4) 0.6056(3) 0.12696(14) 0.0563(7) Uani 1 d D . C6 C 0.5027(4) 0.5097(4) 0.13594(15) 0.0656(8) Uani 1 d D . H6 H 0.5277(4) 0.4258(4) 0.10377(15) 0.079 Uiso 1 calc R . C7 C 0.3576(4) 0.5367(3) 0.19214(14) 0.0584(7) Uani 1 d D . H7 H 0.2888(4) 0.4689(3) 0.19791(14) 0.070 Uiso 1 calc R . C8 C 0.7770(4) 0.5646(4) 0.0704(2) 0.0651(8) Uani 1 d . . O1 O 0.7982(3) 0.4610(3) 0.02351(13) 0.0952(8) Uani 1 d . . O2 O 0.8961(3) 0.6366(3) 0.07428(11) 0.0835(7) Uani 1 d . . H2 H 0.9829(3) 0.6065(3) 0.04100(11) 0.104 Uiso 1 calc R . C9 C 0.0943(3) 0.5522(3) 0.32092(13) 0.0461(6) Uani 1 d D . C10 C 0.1357(4) 0.4584(3) 0.3824(2) 0.0593(7) Uani 1 d D . H10 H 0.2081(4) 0.4795(3) 0.4168(2) 0.071 Uiso 1 calc R . C11 C 0.0707(5) 0.3335(4) 0.3933(2) 0.0752(9) Uani 1 d D . H11 H 0.1005(5) 0.2718(4) 0.4348(2) 0.090 Uiso 1 calc R . C12 C -0.0366(5) 0.3002(4) 0.3437(2) 0.0754(9) Uani 1 d D . H12 H -0.0788(5) 0.2157(4) 0.3510(2) 0.090 Uiso 1 calc R . C13 C -0.0815(4) 0.3937(3) 0.2826(2) 0.0664(8) Uani 1 d D . H13 H -0.1544(4) 0.3722(3) 0.2484(2) 0.080 Uiso 1 calc R . C14 C -0.0189(4) 0.5179(3) 0.27225(15) 0.0543(7) Uani 1 d D . H14 H -0.0533(4) 0.5812(3) 0.23140(15) 0.065 Uiso 1 calc R . C15 C 0.2594(3) 0.7271(3) 0.37076(12) 0.0445(6) Uani 1 d D . C16 C 0.1809(4) 0.8611(3) 0.41448(13) 0.0531(7) Uani 1 d D . H16 H 0.0585(4) 0.9388(3) 0.40555(13) 0.064 Uiso 1 calc R . C17 C 0.2794(4) 0.8829(3) 0.47122(15) 0.0647(8) Uani 1 d D . H17 H 0.2226(4) 0.9742(3) 0.49999(15) 0.078 Uiso 1 calc R . C18 C 0.4608(4) 0.7701(4) 0.48523(15) 0.0654(8) Uani 1 d D . H18 H 0.5264(4) 0.7838(4) 0.52381(15) 0.079 Uiso 1 calc R . C19 C 0.5446(4) 0.6364(4) 0.44162(15) 0.0609(7) Uani 1 d D . H19 H 0.6682(4) 0.5601(4) 0.45031(15) 0.073 Uiso 1 calc R . C20 C 0.4455(4) 0.6158(3) 0.38518(14) 0.0538(7) Uani 1 d D . H20 H 0.5042(4) 0.5253(3) 0.35593(14) 0.065 Uiso 1 calc R . C21 C -0.0343(3) 0.8412(3) 0.29214(13) 0.0461(6) Uani 1 d D . C22 C -0.1986(4) 0.8750(3) 0.34102(14) 0.0528(6) Uani 1 d D . H22 H -0.1905(4) 0.8103(3) 0.38140(14) 0.063 Uiso 1 calc R . C23 C -0.3738(4) 1.0021(3) 0.3313(2) 0.0633(8) Uani 1 d D . H23 H -0.4817(4) 1.0228(3) 0.3651(2) 0.076 Uiso 1 calc R . C24 C -0.3880(4) 1.0976(4) 0.2717(2) 0.0730(9) Uani 1 d D . H24 H -0.5053(4) 1.1839(4) 0.2652(2) 0.088 Uiso 1 calc R . C25 C -0.2295(5) 1.0658(4) 0.2219(2) 0.0707(8) Uani 1 d D . H25 H -0.2398(5) 1.1299(4) 0.1813(2) 0.085 Uiso 1 calc R . C26 C -0.0531(4) 0.9380(3) 0.23185(14) 0.0561(7) Uani 1 d D . H26 H 0.0537(4) 0.9173(3) 0.19758(14) 0.067 Uiso 1 calc R . C27 C 0.6618(13) 0.9314(8) -0.0514(5) 0.225(3) Uani 1 d U . C28 C 0.5087(11) 0.8954(9) -0.0383(3) 0.165(2) Uani 1 d U . C29 C 0.3502(18) 0.8644(15) -0.0162(5) 0.139(4) Uani 0.50 d PU . C30 C 0.2198(9) 0.9986(10) 0.0460(4) 0.176(3) Uani 1 d U . C31 C 0.7897(21) 0.7964(12) -0.1219(7) 0.168(5) Uani 0.50 d PU . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0440(13) 0.0425(13) 0.0432(13) -0.0008(10) -0.0009(10) -0.0160(11) C2 0.0439(13) 0.0484(14) 0.0412(13) -0.0014(11) -0.0014(10) -0.0164(11) C3 0.0530(14) 0.0538(15) 0.0512(15) -0.0071(12) 0.0037(12) -0.0251(12) C4 0.0519(15) 0.060(2) 0.0531(15) -0.0013(13) 0.0007(12) -0.0261(13) C5 0.0515(15) 0.067(2) 0.0482(15) -0.0058(13) 0.0047(12) -0.0214(13) C6 0.065(2) 0.072(2) 0.062(2) -0.0225(14) 0.0129(14) -0.031(2) C7 0.060(2) 0.060(2) 0.060(2) -0.0148(13) 0.0098(13) -0.0300(13) C8 0.059(2) 0.082(2) 0.055(2) -0.0107(15) 0.0101(14) -0.030(2) O1 0.088(2) 0.125(2) 0.0800(15) -0.0445(14) 0.0343(13) -0.0531(14) O2 0.0701(13) 0.112(2) 0.0742(14) -0.0200(12) 0.0262(11) -0.0466(13) C9 0.0404(13) 0.0437(13) 0.0522(14) -0.0006(11) -0.0005(11) -0.0142(11) C10 0.058(2) 0.055(2) 0.067(2) 0.0097(14) -0.0106(14) -0.0241(13) C11 0.077(2) 0.063(2) 0.093(2) 0.029(2) -0.020(2) -0.034(2) C12 0.071(2) 0.054(2) 0.109(3) 0.010(2) -0.007(2) -0.033(2) C13 0.063(2) 0.058(2) 0.084(2) -0.001(2) -0.009(2) -0.0295(14) C14 0.054(2) 0.0525(15) 0.059(2) -0.0019(12) -0.0025(13) -0.0235(13) C15 0.0439(13) 0.0480(14) 0.0429(13) 0.0008(11) 0.0001(11) -0.0197(11) C16 0.0515(15) 0.054(2) 0.0518(15) -0.0043(13) -0.0008(12) -0.0175(13) C17 0.073(2) 0.067(2) 0.056(2) -0.0136(14) -0.0035(14) -0.027(2) C18 0.071(2) 0.080(2) 0.052(2) -0.0038(15) -0.0135(14) -0.035(2) C19 0.054(2) 0.071(2) 0.057(2) 0.0041(14) -0.0104(13) -0.0223(14) C20 0.0479(15) 0.058(2) 0.0536(15) -0.0039(13) -0.0034(12) -0.0178(13) C21 0.0492(14) 0.0458(14) 0.0470(14) -0.0051(11) -0.0057(11) -0.0215(11) C22 0.0482(14) 0.0529(15) 0.055(2) -0.0018(12) 0.0009(12) -0.0179(12) C23 0.048(2) 0.061(2) 0.077(2) -0.010(2) -0.0018(14) -0.0158(14) C24 0.058(2) 0.055(2) 0.101(2) -0.004(2) -0.021(2) -0.0122(15) C25 0.073(2) 0.059(2) 0.077(2) 0.016(2) -0.019(2) -0.021(2) C26 0.057(2) 0.057(2) 0.055(2) 0.0048(13) -0.0041(13) -0.0216(13) C27 0.291(8) 0.166(5) 0.299(8) 0.155(5) -0.212(7) -0.148(5) C28 0.163(5) 0.217(6) 0.146(5) 0.080(4) -0.053(4) -0.102(5) C29 0.149(9) 0.167(9) 0.100(7) -0.023(6) 0.015(6) -0.060(8) C30 0.162(5) 0.238(7) 0.171(5) 0.076(5) -0.054(4) -0.121(5) C31 0.226(13) 0.110(7) 0.154(9) -0.060(7) -0.024(9) -0.044(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C9 1.547(3) . ? C1 C15 1.549(3) . ? C1 C21 1.555(3) . ? C1 C2 1.556(3) . ? C2 C7 1.383(3) . ? C2 C3 1.392(3) . ? C3 C4 1.380(3) . ? C4 C5 1.386(4) . ? C5 C6 1.378(4) . ? C5 C8 1.480(4) . ? C6 C7 1.383(4) . ? C8 O1 1.251(4) . ? C8 O2 1.280(4) . ? C9 C10 1.387(3) . ? C9 C14 1.390(4) . ? C10 C11 1.388(4) . ? C11 C12 1.367(4) . ? C12 C13 1.381(4) . ? C13 C14 1.370(4) . ? C15 C16 1.379(3) . ? C15 C20 1.395(3) . ? C16 C17 1.382(4) . ? C17 C18 1.373(4) . ? C18 C19 1.377(4) . ? C19 C20 1.377(4) . ? C21 C26 1.385(3) . ? C21 C22 1.386(3) . ? C22 C23 1.381(4) . ? C23 C24 1.371(4) . ? C24 C25 1.367(4) . ? C25 C26 1.389(4) . ? C27 C30 1.264(8) 2_675 ? C27 C28 1.286(8) . ? C27 C31 1.758(13) . ? C28 C29 1.327(12) . ? C29 C30 1.650(12) . ? C30 C27 1.264(8) 2_675 ? 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 C9 C1 C15 111.3(2) . . ? C9 C1 C21 106.1(2) . . ? C15 C1 C21 111.4(2) . . ? C9 C1 C2 111.5(2) . . ? C15 C1 C2 105.7(2) . . ? C21 C1 C2 111.1(2) . . ? C7 C2 C3 117.3(2) . . ? C7 C2 C1 123.7(2) . . ? C3 C2 C1 119.0(2) . . ? C4 C3 C2 121.9(2) . . ? C3 C4 C5 119.8(2) . . ? C6 C5 C4 118.9(2) . . ? C6 C5 C8 119.4(3) . . ? C4 C5 C8 121.7(3) . . ? C5 C6 C7 120.9(3) . . ? C2 C7 C6 121.1(2) . . ? O1 C8 O2 123.6(3) . . ? O1 C8 C5 120.0(3) . . ? O2 C8 C5 116.3(3) . . ? C10 C9 C14 117.0(2) . . ? C10 C9 C1 123.8(2) . . ? C14 C9 C1 119.2(2) . . ? C11 C10 C9 121.0(3) . . ? C12 C11 C10 120.7(3) . . ? C11 C12 C13 119.1(3) . . ? C14 C13 C12 120.2(3) . . ? C13 C14 C9 122.0(3) . . ? C16 C15 C20 117.0(2) . . ? C16 C15 C1 124.4(2) . . ? C20 C15 C1 118.5(2) . . ? C15 C16 C17 121.7(2) . . ? C18 C17 C16 120.2(3) . . ? C17 C18 C19 119.4(3) . . ? C18 C19 C20 120.0(3) . . ? C19 C20 C15 121.6(2) . . ? C26 C21 C22 117.5(2) . . ? C26 C21 C1 123.4(2) . . ? C22 C21 C1 119.1(2) . . ? C23 C22 C21 121.7(3) . . ? C24 C23 C22 119.7(3) . . ? C23 C24 C25 120.0(3) . . ? C24 C25 C26 120.3(3) . . ? C21 C26 C25 120.8(3) . . ? C30 C27 C28 159.5(11) 2_675 . ? C30 C27 C31 99.8(9) 2_675 . ? C28 C27 C31 100.8(8) . . ? C27 C28 C29 172.6(10) . . ? C28 C29 C30 107.9(9) . . ? C27 C30 C29 98.8(8) 2_675 . ? _refine_diff_density_max 0.312 _refine_diff_density_min -0.228 _refine_diff_density_rms 0.043 data_5.o-xylene _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '4-(triphenylmethyl)benzoic acid o-xylene clathrate ' _chemical_formula_moiety '(C26 H20 O2). 0.5(C8 H10)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum '(C26 H20 O2). 0.5(C8 H10) ' _chemical_formula_weight 417.50 _chemical_melting_point '246 deg C ' _chemical_compound_source ? 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 7.368(1) _cell_length_b 9.010(1) _cell_length_c 18.522(1) _cell_angle_alpha 88.00(1) _cell_angle_beta 84.97(1) _cell_angle_gamma 67.94(1) _cell_volume 1135.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5 _cell_measurement_theta_max 15 _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method ? _exptl_crystal_F_000 500 _exptl_absorpt_coefficient_mu 0.084 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.910 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; Rigaku RU-200 rotating-anode generator powered at 50kV and 90mA ; _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC7R four-circle diffractometer' _diffrn_measurement_method '2\q/\w scan' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4262 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.1858 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3983 _reflns_number_observed 1541 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'MSC/AFC' _computing_cell_refinement 'MSC/AFC' _computing_data_reduction 'MSC/AFC' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL-PC' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0669P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3980 _refine_ls_number_parameters 299 _refine_ls_number_restraints 254 _refine_ls_R_factor_all 0.2179 _refine_ls_R_factor_obs 0.0576 _refine_ls_wR_factor_all 0.1733 _refine_ls_wR_factor_obs 0.1330 _refine_ls_goodness_of_fit_all 0.938 _refine_ls_goodness_of_fit_obs 1.232 _refine_ls_restrained_S_all 0.993 _refine_ls_restrained_S_obs 1.297 _refine_ls_shift/esd_max -0.010 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group C1 C 0.1605(4) 0.6992(4) 0.8063(2) 0.0400(8) Uani 1 d D . C2 C 0.3167(4) 0.6652(4) 0.7407(2) 0.0425(9) Uani 1 d D . C3 C 0.4230(4) 0.7648(4) 0.7287(2) 0.0462(9) Uani 1 d D . H3 H 0.3929(4) 0.8528(4) 0.7587(2) 0.055 Uiso 1 calc R . C4 C 0.5713(4) 0.7367(4) 0.6738(2) 0.0475(9) Uani 1 d D . H4 H 0.6403(4) 0.8045(4) 0.6675(2) 0.057 Uiso 1 calc R . C5 C 0.6165(4) 0.6067(4) 0.6282(2) 0.0492(9) Uani 1 d D . C6 C 0.5073(5) 0.5119(4) 0.6373(2) 0.0623(11) Uani 1 d D . H6 H 0.5329(5) 0.4274(4) 0.6056(2) 0.075 Uiso 1 calc R . C7 C 0.3599(5) 0.5397(4) 0.6929(2) 0.0550(10) Uani 1 d D . H7 H 0.2891(5) 0.4731(4) 0.6982(2) 0.066 Uiso 1 calc R . C8 C 0.7818(5) 0.5641(5) 0.5714(2) 0.0616(11) Uani 1 d . . O1 O 0.8041(4) 0.4598(4) 0.5253(2) 0.0904(9) Uani 1 d . . O2 O 0.9006(4) 0.6384(3) 0.57396(14) 0.0771(8) Uani 1 d . . H2 H 0.9872(4) 0.6076(3) 0.54074(14) 0.123(18) Uiso 1 calc R . C9 C 0.0958(4) 0.5546(4) 0.8219(2) 0.0436(9) Uani 1 d D . C10 C 0.1359(5) 0.4605(4) 0.8836(2) 0.0575(10) Uani 1 d D . H10 H 0.2075(5) 0.4811(4) 0.9182(2) 0.069 Uiso 1 calc R . C11 C 0.0694(6) 0.3350(4) 0.8941(2) 0.0728(12) Uani 1 d D . H11 H 0.0978(6) 0.2722(4) 0.9356(2) 0.087 Uiso 1 calc R . C12 C -0.0370(6) 0.3029(4) 0.8440(2) 0.0734(13) Uani 1 d D . H12 H -0.0794(6) 0.2181(4) 0.8512(2) 0.088 Uiso 1 calc R . C13 C -0.0803(5) 0.3965(4) 0.7836(2) 0.0603(11) Uani 1 d D . H13 H -0.1543(5) 0.3763(4) 0.7498(2) 0.072 Uiso 1 calc R . C14 C -0.0152(5) 0.5208(4) 0.7724(2) 0.0505(9) Uani 1 d D . H14 H -0.0459(5) 0.5834(4) 0.7308(2) 0.061 Uiso 1 calc R . C15 C 0.2619(4) 0.7297(4) 0.8710(2) 0.0406(8) Uani 1 d D . C16 C 0.1819(5) 0.8643(4) 0.9151(2) 0.0490(9) Uani 1 d D . H16 H 0.0604(5) 0.9417(4) 0.9061(2) 0.059 Uiso 1 calc R . C17 C 0.2798(5) 0.8854(4) 0.9721(2) 0.0579(10) Uani 1 d D . H17 H 0.2225(5) 0.9757(4) 1.0013(2) 0.069 Uiso 1 calc R . C18 C 0.4595(5) 0.7746(5) 0.9857(2) 0.0636(11) Uani 1 d D . H18 H 0.5252(5) 0.7890(5) 1.0239(2) 0.076 Uiso 1 calc R . C19 C 0.5425(5) 0.6412(4) 0.9422(2) 0.0583(10) Uani 1 d D . H19 H 0.6652(5) 0.5653(4) 0.9510(2) 0.070 Uiso 1 calc R . C20 C 0.4458(4) 0.6189(4) 0.8858(2) 0.0516(10) Uani 1 d D . H20 H 0.5044(4) 0.5281(4) 0.8569(2) 0.062 Uiso 1 calc R . C21 C -0.0276(4) 0.8437(4) 0.7917(2) 0.0407(8) Uani 1 d D . C22 C -0.1937(5) 0.8779(4) 0.8397(2) 0.0502(10) Uani 1 d D . H22 H -0.1883(5) 0.8138(4) 0.8806(2) 0.060 Uiso 1 calc R . C23 C -0.3665(5) 1.0043(4) 0.8284(2) 0.0595(11) Uani 1 d D . H23 H -0.4753(5) 1.0241(4) 0.8616(2) 0.071 Uiso 1 calc R . C24 C -0.3791(5) 1.1006(4) 0.7689(2) 0.0658(12) Uani 1 d D . H24 H -0.4952(5) 1.1865(4) 0.7616(2) 0.079 Uiso 1 calc R . C25 C -0.2176(5) 1.0685(4) 0.7201(2) 0.0656(11) Uani 1 d D . H25 H -0.2249(5) 1.1332(4) 0.6793(2) 0.079 Uiso 1 calc R . C26 C -0.0436(5) 0.9407(4) 0.7309(2) 0.0539(10) Uani 1 d D . H26 H 0.0636(5) 0.9199(4) 0.6969(2) 0.065 Uiso 1 calc R . C27 C 0.5074(9) 0.0625(6) 0.5192(3) 0.120(2) Uani 1 d DU . C28 C 0.3620(10) 0.1470(7) 0.5762(4) 0.145(2) Uani 1 d DU . H28 H 0.3682(10) 0.2286(7) 0.6041(4) 0.174 Uiso 1 calc R . C29 C 0.2354(15) 0.0978(14) 0.5822(6) 0.119(3) Uani 0.50 d PDU . H29 H 0.1339(15) 0.1501(14) 0.6169(6) 0.143 Uiso 0.50 calc PR . C30 C 0.2119(13) -0.0207(14) 0.5479(5) 0.105(3) Uani 0.50 d PDU . H30 H 0.1015(13) -0.0442(14) 0.5623(5) 0.127 Uiso 0.50 calc PR . C31 C 0.6757(11) 0.1009(8) 0.5013(3) 0.147(2) Uani 1 d DU . H31 H 0.6989(11) 0.1806(8) 0.5249(3) 0.177 Uiso 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 C1 0.038(2) 0.043(2) 0.039(2) -0.0044(15) -0.0032(15) -0.015(2) C2 0.040(2) 0.044(2) 0.042(2) -0.002(2) -0.006(2) -0.013(2) C3 0.048(2) 0.050(2) 0.043(2) -0.009(2) 0.002(2) -0.022(2) C4 0.042(2) 0.053(2) 0.049(2) -0.003(2) -0.001(2) -0.019(2) C5 0.037(2) 0.060(2) 0.048(2) -0.006(2) 0.005(2) -0.016(2) C6 0.065(2) 0.064(2) 0.060(2) -0.021(2) 0.015(2) -0.029(2) C7 0.053(2) 0.059(2) 0.056(2) -0.014(2) 0.012(2) -0.027(2) C8 0.054(2) 0.075(3) 0.056(2) -0.007(2) 0.004(2) -0.026(2) O1 0.084(2) 0.114(2) 0.081(2) -0.047(2) 0.033(2) -0.051(2) O2 0.060(2) 0.107(2) 0.071(2) -0.026(2) 0.0213(15) -0.043(2) C9 0.036(2) 0.041(2) 0.050(2) -0.005(2) 0.001(2) -0.011(2) C10 0.056(2) 0.058(2) 0.064(2) 0.013(2) -0.015(2) -0.026(2) C11 0.079(3) 0.058(3) 0.089(3) 0.033(2) -0.024(2) -0.034(2) C12 0.068(2) 0.052(2) 0.110(3) 0.011(2) -0.019(3) -0.031(2) C13 0.050(2) 0.058(2) 0.078(3) -0.003(2) -0.012(2) -0.024(2) C14 0.048(2) 0.054(2) 0.055(2) 0.003(2) -0.006(2) -0.024(2) C15 0.040(2) 0.047(2) 0.038(2) -0.001(2) 0.001(2) -0.020(2) C16 0.047(2) 0.051(2) 0.047(2) -0.006(2) -0.001(2) -0.016(2) C17 0.058(2) 0.064(2) 0.050(2) -0.013(2) -0.006(2) -0.020(2) C18 0.065(2) 0.084(3) 0.049(2) -0.011(2) -0.007(2) -0.034(2) C19 0.045(2) 0.073(3) 0.059(2) 0.011(2) -0.015(2) -0.022(2) C20 0.041(2) 0.057(2) 0.050(2) -0.003(2) -0.004(2) -0.009(2) C21 0.042(2) 0.043(2) 0.039(2) -0.004(2) -0.009(2) -0.016(2) C22 0.043(2) 0.054(2) 0.050(2) -0.004(2) 0.002(2) -0.015(2) C23 0.040(2) 0.057(2) 0.079(3) -0.010(2) -0.007(2) -0.014(2) C24 0.051(2) 0.048(2) 0.091(3) -0.007(2) -0.018(2) -0.008(2) C25 0.066(2) 0.048(2) 0.076(3) 0.013(2) -0.022(2) -0.011(2) C26 0.057(2) 0.055(2) 0.050(2) 0.000(2) -0.007(2) -0.020(2) C27 0.172(4) 0.098(4) 0.111(4) 0.020(3) -0.089(4) -0.060(4) C28 0.198(5) 0.106(4) 0.134(5) -0.010(4) -0.053(5) -0.051(4) C29 0.116(5) 0.170(8) 0.112(8) 0.050(7) -0.035(6) -0.098(5) C30 0.088(6) 0.186(8) 0.071(6) 0.002(7) -0.011(5) -0.083(5) C31 0.204(6) 0.125(5) 0.117(5) 0.004(4) -0.062(5) -0.056(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C21 1.541(4) . ? C1 C15 1.552(4) . ? C1 C2 1.553(4) . ? C1 C9 1.557(4) . ? C2 C7 1.382(4) . ? C2 C3 1.397(4) . ? C3 C4 1.381(4) . ? C4 C5 1.386(4) . ? C5 C6 1.374(5) . ? C5 C8 1.480(5) . ? C6 C7 1.386(4) . ? C8 O1 1.246(4) . ? C8 O2 1.291(4) . ? C9 C10 1.384(4) . ? C9 C14 1.393(4) . ? C10 C11 1.392(5) . ? C11 C12 1.369(5) . ? C12 C13 1.364(5) . ? C13 C14 1.377(5) . ? C15 C16 1.390(4) . ? C15 C20 1.391(4) . ? C16 C17 1.386(4) . ? C17 C18 1.365(5) . ? C18 C19 1.378(5) . ? C19 C20 1.375(4) . ? C21 C26 1.387(4) . ? C21 C22 1.389(4) . ? C22 C23 1.379(4) . ? C23 C24 1.367(5) . ? C24 C25 1.374(5) . ? C25 C26 1.389(4) . ? C27 C27 1.396(9) 2_656 ? C27 C31 1.417(8) . ? C27 C28 1.445(7) . ? C28 C29 1.170(10) . ? C29 C30 1.335(12) . ? C30 C31 1.225(9) 2_656 ? C31 C30 1.225(9) 2_656 ? 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 C21 C1 C15 111.9(2) . . ? C21 C1 C2 111.5(2) . . ? C15 C1 C2 105.2(2) . . ? C21 C1 C9 106.1(2) . . ? C15 C1 C9 111.0(3) . . ? C2 C1 C9 111.3(2) . . ? C7 C2 C3 117.1(3) . . ? C7 C2 C1 123.9(3) . . ? C3 C2 C1 119.0(3) . . ? C4 C3 C2 122.1(3) . . ? C3 C4 C5 119.6(3) . . ? C6 C5 C4 118.8(3) . . ? C6 C5 C8 118.9(3) . . ? C4 C5 C8 122.3(3) . . ? C5 C6 C7 121.2(3) . . ? C2 C7 C6 120.9(3) . . ? O1 C8 O2 123.2(3) . . ? O1 C8 C5 120.8(4) . . ? O2 C8 C5 116.0(3) . . ? C10 C9 C14 117.7(3) . . ? C10 C9 C1 123.9(3) . . ? C14 C9 C1 118.4(3) . . ? C9 C10 C11 120.3(3) . . ? C12 C11 C10 120.9(4) . . ? C13 C12 C11 119.4(4) . . ? C12 C13 C14 120.4(4) . . ? C13 C14 C9 121.4(3) . . ? C16 C15 C20 117.2(3) . . ? C16 C15 C1 123.8(3) . . ? C20 C15 C1 119.0(3) . . ? C17 C16 C15 121.3(3) . . ? C18 C17 C16 120.5(3) . . ? C17 C18 C19 119.1(3) . . ? C20 C19 C18 120.7(3) . . ? C19 C20 C15 121.2(3) . . ? C26 C21 C22 117.1(3) . . ? C26 C21 C1 123.3(3) . . ? C22 C21 C1 119.6(3) . . ? C23 C22 C21 121.8(3) . . ? C24 C23 C22 120.5(3) . . ? C23 C24 C25 119.0(3) . . ? C24 C25 C26 120.8(4) . . ? C21 C26 C25 120.9(3) . . ? C27 C27 C31 117.0(8) 2_656 . ? C27 C27 C28 122.2(8) 2_656 . ? C31 C27 C28 120.8(5) . . ? C29 C28 C27 110.1(8) . . ? C28 C29 C30 131.0(11) . . ? C31 C30 C29 125.1(10) 2_656 . ? C30 C31 C27 114.7(8) 2_656 . ? _refine_diff_density_max 0.171 _refine_diff_density_min -0.232 _refine_diff_density_rms 0.043 data_5.p-xylene _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '4-(triphenylmethyl)benzoic acid p-xylene clathrate ' _chemical_melting_point ' 248 deg C ' _chemical_formula_moiety '(C26 H20 O2). 0.5(C8 H10)' _chemical_formula_sum 'C30 H25 O2' _chemical_formula_weight 417.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.241(2) _cell_length_b 9.011(2) _cell_length_c 18.916(3) _cell_angle_alpha 84.25(2) _cell_angle_beta 87.25(2) _cell_angle_gamma 66.66(2) _cell_volume 1127.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5 _cell_measurement_theta_max 15 _exptl_crystal_description plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.230 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 442 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.951 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; Rigaku RU-200 rotating-anode generator powered at 50kV and 90mA ; _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 197 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.10 _diffrn_reflns_number 4714 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_sigmaI/netI 0.0762 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4414 _reflns_number_gt 2463 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'MSC/AFC Diffractometer Control' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PC (Siemens, 1990)' _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^)+(0.0834P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.026(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4414 _refine_ls_number_parameters 290 _refine_ls_number_restraints 172 _refine_ls_R_factor_all 0.1269 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.1716 _refine_ls_wR_factor_gt 0.1480 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.033 _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 C1 C 0.6711(3) 0.1630(2) 0.19484(10) 0.0356(5) Uani 1 1 d D . . C2 C 0.5491(3) 0.1265(2) 0.25928(10) 0.0358(5) Uani 1 1 d D . . C3 C 0.3512(3) 0.2365(3) 0.26872(11) 0.0436(5) Uani 1 1 d D . . H3 H 0.2997 0.3298 0.2377 0.052 Uiso 1 1 calc R . . C4 C 0.2303(3) 0.2105(3) 0.32268(11) 0.0460(6) Uani 1 1 d D . . H4 H 0.0991 0.2858 0.3275 0.055 Uiso 1 1 calc R . . C5 C 0.3028(3) 0.0731(3) 0.36977(11) 0.0438(5) Uani 1 1 d D . . C6 C 0.5002(3) -0.0357(3) 0.36190(12) 0.0509(6) Uani 1 1 d D . . H6 H 0.5527 -0.1267 0.3942 0.061 Uiso 1 1 calc R . . C7 C 0.6206(3) -0.0106(3) 0.30665(11) 0.0465(6) Uani 1 1 d D . . H7 H 0.7511 -0.0869 0.3014 0.056 Uiso 1 1 calc R . . C8 C 0.1734(3) 0.0403(3) 0.42696(12) 0.0502(6) Uani 1 1 d D . . O1 O -0.0164(2) 0.1183(2) 0.41974(9) 0.0738(6) Uani 1 1 d D . . H1 H -0.0750 0.0940 0.4543 0.111 Uiso 1 1 calc R . . O2 O 0.2506(3) -0.0625(2) 0.47825(9) 0.0713(6) Uani 1 1 d D . . C9 C 0.8731(3) 0.0184(2) 0.18327(11) 0.0372(5) Uani 1 1 d D . . C10 C 1.0224(3) -0.0271(3) 0.23426(12) 0.0448(5) Uani 1 1 d D . . H10 H 0.9967 0.0282 0.2749 0.054 Uiso 1 1 calc R . . C11 C 1.2071(3) -0.1517(3) 0.22628(13) 0.0534(6) Uani 1 1 d D . . H11 H 1.3028 -0.1809 0.2618 0.064 Uiso 1 1 calc R . . C12 C 1.2503(3) -0.2334(3) 0.16560(15) 0.0587(7) Uani 1 1 d D . . H12 H 1.3748 -0.3176 0.1599 0.070 Uiso 1 1 calc R . . C13 C 1.1072(3) -0.1886(3) 0.11394(14) 0.0563(7) Uani 1 1 d D . . H13 H 1.1355 -0.2425 0.0728 0.068 Uiso 1 1 calc R . . C14 C 0.9202(3) -0.0637(3) 0.12232(12) 0.0480(6) Uani 1 1 d D . . H14 H 0.8254 -0.0347 0.0866 0.058 Uiso 1 1 calc R . . C15 C 0.5309(3) 0.2019(3) 0.13003(10) 0.0370(5) Uani 1 1 d D . . C16 C 0.4529(3) 0.0902(3) 0.11579(12) 0.0451(5) Uani 1 1 d D . . H16 H 0.4872 -0.0060 0.1450 0.054 Uiso 1 1 calc R . . C17 C 0.3258(3) 0.1181(3) 0.05936(12) 0.0538(6) Uani 1 1 d D . . H17 H 0.2760 0.0409 0.0509 0.065 Uiso 1 1 calc R . . C18 C 0.2726(4) 0.2595(3) 0.01560(13) 0.0586(7) Uani 1 1 d D . . H18 H 0.1889 0.2777 -0.0229 0.070 Uiso 1 1 calc R . . C19 C 0.3441(4) 0.3738(3) 0.02933(13) 0.0557(6) Uani 1 1 d D . . H19 H 0.3070 0.4704 0.0003 0.067 Uiso 1 1 calc R . . C20 C 0.4718(3) 0.3462(3) 0.08636(11) 0.0451(5) Uani 1 1 d D . . H20 H 0.5181 0.4251 0.0953 0.054 Uiso 1 1 calc R . . C21 C 0.7278(3) 0.3076(2) 0.20653(11) 0.0368(5) Uani 1 1 d D . . C22 C 0.8506(3) 0.3499(3) 0.15676(12) 0.0429(5) Uani 1 1 d D . . H22 H 0.8966 0.2909 0.1173 0.051 Uiso 1 1 calc R . . C23 C 0.9057(3) 0.4776(3) 0.16471(13) 0.0518(6) Uani 1 1 d D . . H23 H 0.9865 0.5043 0.1304 0.062 Uiso 1 1 calc R . . C24 C 0.8421(4) 0.5652(3) 0.22265(14) 0.0570(7) Uani 1 1 d D . . H24 H 0.8773 0.6523 0.2275 0.068 Uiso 1 1 calc R . . C25 C 0.7259(4) 0.5230(3) 0.27362(14) 0.0573(7) Uani 1 1 d D . . H25 H 0.6844 0.5806 0.3136 0.069 Uiso 1 1 calc R . . C26 C 0.6698(3) 0.3946(3) 0.26586(12) 0.0446(5) Uani 1 1 d D . . H26 H 0.5921 0.3667 0.3010 0.054 Uiso 1 1 calc R . . C27 C 0.1493(5) 0.5276(4) 0.45716(15) 0.0727(8) Uani 1 1 d D . . C28 C -0.0437(5) 0.6423(4) 0.45981(17) 0.0889(10) Uani 1 1 d D . . H28 H -0.0765 0.7411 0.4326 0.107 Uiso 1 1 calc R . . C29 C 0.1898(5) 0.3847(4) 0.49853(18) 0.0876(10) Uani 1 1 d D . . H29 H 0.3191 0.3042 0.4984 0.105 Uiso 1 1 calc R . . C30 C 0.3107(6) 0.5569(5) 0.4115(2) 0.1189(14) Uani 1 1 d D . . H30A H 0.2545 0.6625 0.3861 0.178 Uiso 1 1 calc R . . H30B H 0.3622 0.4759 0.3782 0.178 Uiso 1 1 calc R . . H30C H 0.4178 0.5510 0.4411 0.178 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 C1 0.0364(11) 0.0398(11) 0.0331(11) 0.0002(9) 0.0011(8) -0.0185(9) C2 0.0326(10) 0.0438(11) 0.0353(11) -0.0022(9) 0.0009(8) -0.0200(9) C3 0.0374(11) 0.0498(13) 0.0409(12) 0.0072(10) 0.0004(9) -0.0170(10) C4 0.0328(11) 0.0572(14) 0.0456(13) 0.0009(11) 0.0038(9) -0.0168(10) C5 0.0412(12) 0.0580(13) 0.0365(12) -0.0023(10) 0.0046(9) -0.0252(11) C6 0.0487(13) 0.0544(14) 0.0437(13) 0.0102(11) 0.0037(11) -0.0181(12) C7 0.0405(12) 0.0512(13) 0.0428(12) 0.0042(10) 0.0038(10) -0.0153(10) C8 0.0445(13) 0.0679(15) 0.0421(13) 0.0012(12) 0.0070(10) -0.0284(12) O1 0.0476(10) 0.1150(16) 0.0568(11) 0.0140(10) 0.0104(8) -0.0363(10) O2 0.0606(11) 0.0869(13) 0.0548(11) 0.0204(10) 0.0121(9) -0.0246(10) C9 0.0343(10) 0.0394(11) 0.0428(12) 0.0001(9) 0.0042(9) -0.0211(9) C10 0.0406(12) 0.0470(12) 0.0477(13) -0.0031(10) -0.0003(10) -0.0186(10) C11 0.0389(12) 0.0533(14) 0.0658(16) 0.0002(12) -0.0042(11) -0.0166(11) C12 0.0388(13) 0.0478(14) 0.0846(19) -0.0114(13) 0.0026(13) -0.0109(11) C13 0.0493(14) 0.0498(14) 0.0698(16) -0.0237(12) 0.0115(12) -0.0166(12) C14 0.0456(13) 0.0516(13) 0.0497(14) -0.0086(11) 0.0024(11) -0.0217(11) C15 0.0333(10) 0.0467(12) 0.0344(11) -0.0036(9) 0.0036(9) -0.0198(9) C16 0.0442(12) 0.0534(13) 0.0433(12) 0.0013(10) -0.0028(10) -0.0261(11) C17 0.0525(13) 0.0655(15) 0.0538(14) -0.0062(12) -0.0045(12) -0.0336(12) C18 0.0544(14) 0.0817(18) 0.0446(14) -0.0003(13) -0.0129(11) -0.0317(14) C19 0.0596(15) 0.0607(15) 0.0452(13) 0.0100(11) -0.0112(11) -0.0244(13) C20 0.0487(13) 0.0479(13) 0.0441(13) 0.0011(10) -0.0038(10) -0.0257(11) C21 0.0315(10) 0.0391(11) 0.0405(12) -0.0002(9) -0.0038(9) -0.0149(9) C22 0.0423(12) 0.0447(12) 0.0433(12) 0.0002(10) 0.0011(10) -0.0200(10) C23 0.0432(12) 0.0514(14) 0.0649(16) 0.0058(12) -0.0028(11) -0.0254(11) C24 0.0524(14) 0.0417(13) 0.0830(19) -0.0034(13) -0.0076(13) -0.0247(11) C25 0.0556(15) 0.0514(14) 0.0683(17) -0.0196(13) 0.0014(13) -0.0216(12) C26 0.0417(12) 0.0469(13) 0.0473(13) -0.0085(10) 0.0065(10) -0.0194(10) C27 0.083(2) 0.078(2) 0.0547(17) -0.0134(15) 0.0097(15) -0.0287(17) C28 0.098(2) 0.084(2) 0.073(2) 0.0118(17) -0.0005(19) -0.028(2) C29 0.072(2) 0.091(2) 0.086(2) -0.0092(19) 0.0034(18) -0.0172(18) C30 0.126(3) 0.137(3) 0.105(3) -0.028(3) 0.045(2) -0.065(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C9 1.549(3) . ? C1 C21 1.551(3) . ? C1 C15 1.552(3) . ? C1 C2 1.556(3) . ? C2 C7 1.383(3) . ? C2 C3 1.398(3) . ? C3 C4 1.375(3) . ? C4 C5 1.382(3) . ? C5 C6 1.387(3) . ? C5 C8 1.481(3) . ? C6 C7 1.387(3) . ? C8 O2 1.254(3) . ? C8 O1 1.278(3) . ? C9 C14 1.388(3) . ? C9 C10 1.392(3) . ? C10 C11 1.377(3) . ? C11 C12 1.382(3) . ? C12 C13 1.371(3) . ? C13 C14 1.390(3) . ? C15 C16 1.387(3) . ? C15 C20 1.391(3) . ? C16 C17 1.381(3) . ? C17 C18 1.374(3) . ? C18 C19 1.373(3) . ? C19 C20 1.393(3) . ? C21 C26 1.386(3) . ? C21 C22 1.392(3) . ? C22 C23 1.382(3) . ? C23 C24 1.368(3) . ? C24 C25 1.373(3) . ? C25 C26 1.392(3) . ? C27 C29 1.370(4) . ? C27 C28 1.373(4) . ? C27 C30 1.511(4) . ? C28 C29 1.373(4) 2_566 ? C29 C28 1.373(4) 2_566 ? 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 C9 C1 C21 105.66(15) . . ? C9 C1 C15 111.19(16) . . ? C21 C1 C15 111.59(16) . . ? C9 C1 C2 112.50(16) . . ? C21 C1 C2 110.99(16) . . ? C15 C1 C2 105.06(15) . . ? C7 C2 C3 117.47(18) . . ? C7 C2 C1 124.45(17) . . ? C3 C2 C1 118.03(17) . . ? C4 C3 C2 121.8(2) . . ? C3 C4 C5 120.37(19) . . ? C4 C5 C6 118.48(19) . . ? C4 C5 C8 121.25(19) . . ? C6 C5 C8 120.3(2) . . ? C5 C6 C7 121.0(2) . . ? C2 C7 C6 120.8(2) . . ? O2 C8 O1 123.2(2) . . ? O2 C8 C5 120.2(2) . . ? O1 C8 C5 116.6(2) . . ? C14 C9 C10 117.09(19) . . ? C14 C9 C1 123.70(18) . . ? C10 C9 C1 119.08(18) . . ? C11 C10 C9 122.0(2) . . ? C10 C11 C12 120.1(2) . . ? C13 C12 C11 119.1(2) . . ? C12 C13 C14 120.8(2) . . ? C9 C14 C13 121.0(2) . . ? C16 C15 C20 117.46(19) . . ? C16 C15 C1 118.82(18) . . ? C20 C15 C1 123.67(19) . . ? C17 C16 C15 121.7(2) . . ? C18 C17 C16 120.2(2) . . ? C19 C18 C17 119.4(2) . . ? C18 C19 C20 120.6(2) . . ? C15 C20 C19 120.7(2) . . ? C26 C21 C22 117.25(19) . . ? C26 C21 C1 123.57(18) . . ? C22 C21 C1 119.12(18) . . ? C23 C22 C21 121.4(2) . . ? C24 C23 C22 120.5(2) . . ? C23 C24 C25 119.3(2) . . ? C24 C25 C26 120.4(2) . . ? C21 C26 C25 121.0(2) . . ? C29 C27 C28 116.7(3) . . ? C29 C27 C30 121.3(3) . . ? C28 C27 C30 122.0(3) . . ? C29 C28 C27 121.8(3) 2_566 . ? C27 C29 C28 121.5(3) . 2_566 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.256 _refine_diff_density_min -0.221 _refine_diff_density_rms 0.044 data_5.anisole _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '4-(triphenylmethyl)benzoic acid anisole clathrate ' _chemical_formula_moiety '(C26 H20 O2). 0.5(C7 H8 O)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum ' (C26 H20 O2). 0.5(C7 H8 O) ' _chemical_formula_weight 418.77 _chemical_melting_point ' 270 deg C' _chemical_compound_source ? 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 7.310(1) _cell_length_b 8.998(1) _cell_length_c 18.464(1) _cell_angle_alpha 89.98(1) _cell_angle_beta 86.26(1) _cell_angle_gamma 67.50(1) _cell_volume 1119.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5 _cell_measurement_theta_max 15 _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method ? _exptl_crystal_F_000 500 _exptl_absorpt_coefficient_mu 0.088 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.958 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; Rigaku RU-200 rotating-anode generator powered at 50kV and 90mA ; _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC7R four-circle diffractometer' _diffrn_measurement_method '2\q/\w scan' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4671 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0981 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4375 _reflns_number_observed 1957 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'MSC/AFC' _computing_cell_refinement 'MSC/AFC' _computing_data_reduction 'MSC/AFC' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL-PC' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0686P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4373 _refine_ls_number_parameters 299 _refine_ls_number_restraints 243 _refine_ls_R_factor_all 0.1485 _refine_ls_R_factor_obs 0.0525 _refine_ls_wR_factor_all 0.1664 _refine_ls_wR_factor_obs 0.1311 _refine_ls_goodness_of_fit_all 0.972 _refine_ls_goodness_of_fit_obs 1.199 _refine_ls_restrained_S_all 0.972 _refine_ls_restrained_S_obs 1.162 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group C1 C 0.1571(3) 0.6884(3) 0.80415(12) 0.0365(5) Uani 1 d D . C2 C 0.3117(3) 0.6544(3) 0.73776(12) 0.0386(6) Uani 1 d D . C3 C 0.4118(3) 0.7580(3) 0.72679(13) 0.0442(6) Uani 1 d D . H3 H 0.3777(3) 0.8484(3) 0.75718(13) 0.053 Uiso 1 calc R . C4 C 0.5590(3) 0.7303(3) 0.67238(13) 0.0486(6) Uani 1 d D . H4 H 0.6252(3) 0.8001(3) 0.66694(13) 0.058 Uiso 1 calc R . C5 C 0.6091(3) 0.5979(3) 0.62548(13) 0.0457(6) Uani 1 d D . C6 C 0.5073(4) 0.4972(3) 0.63390(14) 0.0538(7) Uani 1 d D . H6 H 0.5374(4) 0.4099(3) 0.60190(14) 0.065 Uiso 1 calc R . C7 C 0.3606(4) 0.5245(3) 0.68954(14) 0.0489(6) Uani 1 d D . H7 H 0.2940(4) 0.4549(3) 0.69462(14) 0.059 Uiso 1 calc R . C8 C 0.7766(4) 0.5589(3) 0.56956(14) 0.0547(7) Uani 1 d . . O1 O 0.8009(3) 0.4510(3) 0.52182(11) 0.0814(7) Uani 1 d . . O2 O 0.8917(3) 0.6337(3) 0.57362(11) 0.0777(6) Uani 1 d . . H2 H 0.9786(3) 0.6031(3) 0.54031(11) 0.116 Uiso 1 calc R . C9 C 0.0941(3) 0.5442(3) 0.81841(13) 0.0399(6) Uani 1 d D . C10 C 0.1349(4) 0.4523(3) 0.87967(14) 0.0512(7) Uani 1 d D . H10 H 0.2066(4) 0.4751(3) 0.91482(14) 0.061 Uiso 1 calc R . C11 C 0.0711(4) 0.3267(3) 0.8898(2) 0.0649(8) Uani 1 d D . H11 H 0.1009(4) 0.2663(3) 0.9315(2) 0.078 Uiso 1 calc R . C12 C -0.0356(4) 0.2909(3) 0.8389(2) 0.0658(8) Uani 1 d D . H12 H -0.0766(4) 0.2056(3) 0.8455(2) 0.079 Uiso 1 calc R . C13 C -0.0811(4) 0.3823(3) 0.7783(2) 0.0568(7) Uani 1 d D . H13 H -0.1550(4) 0.3598(3) 0.7438(2) 0.068 Uiso 1 calc R . C14 C -0.0182(3) 0.5067(3) 0.76811(14) 0.0478(6) Uani 1 d D . H14 H -0.0510(3) 0.5677(3) 0.72675(14) 0.057 Uiso 1 calc R . C15 C 0.2592(3) 0.7211(3) 0.86948(12) 0.0396(6) Uani 1 d D . C16 C 0.1805(4) 0.8573(3) 0.91358(13) 0.0461(6) Uani 1 d D . H16 H 0.0575(4) 0.9353(3) 0.90466(13) 0.055 Uiso 1 calc R . C17 C 0.2813(4) 0.8806(3) 0.97137(14) 0.0581(7) Uani 1 d D . H17 H 0.2245(4) 0.9729(3) 1.00084(14) 0.070 Uiso 1 calc R . C18 C 0.4639(4) 0.7677(3) 0.98480(14) 0.0579(7) Uani 1 d D . H18 H 0.5311(4) 0.7829(3) 1.02340(14) 0.069 Uiso 1 calc R . C19 C 0.5467(4) 0.6324(3) 0.94093(14) 0.0542(7) Uani 1 d D . H19 H 0.6707(4) 0.5556(3) 0.94974(14) 0.065 Uiso 1 calc R . C20 C 0.4469(3) 0.6095(3) 0.88366(13) 0.0465(6) Uani 1 d D . H20 H 0.5059(3) 0.5179(3) 0.85391(13) 0.056 Uiso 1 calc R . C21 C -0.0364(3) 0.8335(3) 0.79029(13) 0.0391(6) Uani 1 d D . C22 C -0.2006(3) 0.8696(3) 0.84014(14) 0.0465(6) Uani 1 d D . H22 H -0.1905(3) 0.8069(3) 0.88088(14) 0.056 Uiso 1 calc R . C23 C -0.3770(4) 0.9958(3) 0.8304(2) 0.0560(7) Uani 1 d D . H23 H -0.4838(4) 1.0177(3) 0.8646(2) 0.067 Uiso 1 calc R . C24 C -0.3964(4) 1.0899(3) 0.7703(2) 0.0629(8) Uani 1 d D . H24 H -0.5152(4) 1.1757(3) 0.7639(2) 0.075 Uiso 1 calc R . C25 C -0.2386(4) 1.0555(3) 0.7203(2) 0.0624(8) Uani 1 d D . H25 H -0.2510(4) 1.1182(3) 0.6794(2) 0.075 Uiso 1 calc R . C26 C -0.0596(4) 0.9280(3) 0.72960(14) 0.0502(7) Uani 1 d D . H26 H 0.0457(4) 0.9060(3) 0.69471(14) 0.060 Uiso 1 calc R . C27 C 0.5106(9) 0.0653(7) 0.5195(3) 0.133(2) Uani 1 d DU . C28 C 0.3815(11) 0.1538(7) 0.5727(3) 0.131(2) Uani 0.847(5) d PDU . H28 H 0.4057(11) 0.2347(7) 0.5966(3) 0.157 Uiso 0.847(5) calc PR . C29 C 0.2159(12) 0.1258(9) 0.5918(4) 0.159(3) Uani 0.847(5) d PDU . H29 H 0.1258(12) 0.1824(9) 0.6296(4) 0.191 Uiso 0.847(5) calc PR . C30 C 0.1919(16) 0.0164(13) 0.5543(4) 0.263(7) Uani 0.847(5) d PDU . H30 H 0.0734(16) 0.0027(13) 0.5651(4) 0.315 Uiso 0.847(5) calc PR . C31 C 0.3195(17) -0.0870(10) 0.4987(5) 0.214(4) Uani 0.847(5) d PDU . H31 H 0.2881(17) -0.1655(10) 0.4760(5) 0.257 Uiso 0.847(5) calc PR . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0350(12) 0.0389(13) 0.0348(13) 0.0000(10) 0.0014(10) -0.0139(10) C2 0.0347(12) 0.0429(13) 0.0382(13) 0.0025(11) -0.0032(10) -0.0146(11) C3 0.0466(13) 0.0458(14) 0.0424(14) -0.0062(11) 0.0025(12) -0.0211(12) C4 0.0454(14) 0.060(2) 0.0470(15) 0.0009(13) 0.0042(12) -0.0289(12) C5 0.0403(13) 0.056(2) 0.0384(14) -0.0015(12) 0.0016(11) -0.0169(12) C6 0.0526(15) 0.060(2) 0.050(2) -0.0129(13) 0.0084(13) -0.0243(14) C7 0.0488(14) 0.0497(15) 0.0506(15) -0.0094(12) 0.0084(12) -0.0235(12) C8 0.0486(15) 0.071(2) 0.044(2) -0.0053(14) 0.0075(13) -0.0243(14) O1 0.0774(13) 0.108(2) 0.0666(13) -0.0357(12) 0.0299(11) -0.0493(13) O2 0.0649(12) 0.112(2) 0.0676(13) -0.0188(12) 0.0229(11) -0.0505(12) C9 0.0330(12) 0.0393(13) 0.0454(14) -0.0028(11) 0.0035(10) -0.0128(10) C10 0.0494(15) 0.053(2) 0.055(2) 0.0112(13) -0.0075(13) -0.0240(13) C11 0.066(2) 0.059(2) 0.077(2) 0.026(2) -0.016(2) -0.0311(15) C12 0.059(2) 0.048(2) 0.097(2) 0.010(2) -0.006(2) -0.0283(14) C13 0.053(2) 0.054(2) 0.070(2) 0.0005(14) -0.0100(14) -0.0254(13) C14 0.0477(14) 0.0470(15) 0.050(2) 0.0042(12) -0.0043(12) -0.0195(12) C15 0.0375(12) 0.0473(14) 0.0360(13) 0.0015(11) -0.0011(10) -0.0188(11) C16 0.0432(13) 0.049(2) 0.0434(15) -0.0016(12) -0.0030(12) -0.0147(12) C17 0.060(2) 0.060(2) 0.051(2) -0.0115(14) -0.0029(14) -0.0204(14) C18 0.055(2) 0.075(2) 0.047(2) -0.0031(14) -0.0104(13) -0.0285(15) C19 0.0435(14) 0.063(2) 0.055(2) 0.0063(14) -0.0114(13) -0.0182(13) C20 0.0424(14) 0.050(2) 0.0451(15) -0.0025(12) -0.0023(12) -0.0157(12) C21 0.0387(12) 0.0369(13) 0.0439(14) -0.0011(11) -0.0068(11) -0.0164(10) C22 0.0383(13) 0.0502(15) 0.0497(15) -0.0023(12) 0.0008(12) -0.0161(12) C23 0.0401(14) 0.054(2) 0.071(2) -0.0106(15) 0.0000(13) -0.0148(13) C24 0.047(2) 0.045(2) 0.089(2) 0.001(2) -0.016(2) -0.0065(13) C25 0.068(2) 0.053(2) 0.067(2) 0.0155(14) -0.021(2) -0.0210(15) C26 0.0487(14) 0.051(2) 0.052(2) 0.0063(13) -0.0089(12) -0.0193(13) C27 0.144(4) 0.156(6) 0.107(4) 0.040(4) -0.039(4) -0.061(4) C28 0.190(6) 0.107(4) 0.097(4) -0.020(3) 0.006(4) -0.060(4) C29 0.174(7) 0.153(7) 0.114(6) 0.017(5) 0.009(5) -0.025(5) C30 0.326(13) 0.244(12) 0.101(6) 0.023(6) 0.008(7) 0.018(10) C31 0.337(13) 0.168(7) 0.163(8) 0.030(6) -0.090(9) -0.114(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 C1 C15 1.544(3) . ? C1 C21 1.551(3) . ? C1 C9 1.551(3) . ? C1 C2 1.558(3) . ? C2 C7 1.388(3) . ? C2 C3 1.396(3) . ? C3 C4 1.373(3) . ? C4 C5 1.389(3) . ? C5 C6 1.379(3) . ? C5 C8 1.481(3) . ? C6 C7 1.386(3) . ? C8 O1 1.265(3) . ? C8 O2 1.269(3) . ? C9 C10 1.381(3) . ? C9 C14 1.401(3) . ? C10 C11 1.386(4) . ? C11 C12 1.373(4) . ? C12 C13 1.371(4) . ? C13 C14 1.372(3) . ? C15 C16 1.377(3) . ? C15 C20 1.397(3) . ? C16 C17 1.395(3) . ? C17 C18 1.372(4) . ? C18 C19 1.371(4) . ? C19 C20 1.382(3) . ? C21 C26 1.386(3) . ? C21 C22 1.397(3) . ? C22 C23 1.376(3) . ? C23 C24 1.377(4) . ? C24 C25 1.367(4) . ? C25 C26 1.392(4) . ? C27 C28 1.339(7) . ? C27 C31 1.351(11) 2_656 ? C27 C27 1.442(11) 2_656 ? C28 C29 1.353(9) . ? C29 C30 1.275(11) . ? C30 C31 1.415(10) . ? C31 C27 1.351(11) 2_656 ? 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 C15 C1 C21 111.8(2) . . ? C15 C1 C9 110.9(2) . . ? C21 C1 C9 105.8(2) . . ? C15 C1 C2 105.8(2) . . ? C21 C1 C2 110.9(2) . . ? C9 C1 C2 111.8(2) . . ? C7 C2 C3 117.5(2) . . ? C7 C2 C1 124.1(2) . . ? C3 C2 C1 118.4(2) . . ? C4 C3 C2 121.8(2) . . ? C3 C4 C5 119.9(2) . . ? C6 C5 C4 119.1(2) . . ? C6 C5 C8 119.8(2) . . ? C4 C5 C8 121.0(2) . . ? C5 C6 C7 120.7(2) . . ? C6 C7 C2 120.8(2) . . ? O1 C8 O2 123.5(2) . . ? O1 C8 C5 119.0(2) . . ? O2 C8 C5 117.5(2) . . ? C10 C9 C14 116.8(2) . . ? C10 C9 C1 124.1(2) . . ? C14 C9 C1 119.0(2) . . ? C9 C10 C11 121.3(3) . . ? C12 C11 C10 120.5(3) . . ? C13 C12 C11 119.2(3) . . ? C12 C13 C14 120.3(3) . . ? C13 C14 C9 121.7(2) . . ? C16 C15 C20 117.2(2) . . ? C16 C15 C1 124.2(2) . . ? C20 C15 C1 118.6(2) . . ? C15 C16 C17 121.4(2) . . ? C18 C17 C16 120.1(2) . . ? C19 C18 C17 119.5(2) . . ? C18 C19 C20 120.3(2) . . ? C19 C20 C15 121.4(2) . . ? C26 C21 C22 117.2(2) . . ? C26 C21 C1 123.9(2) . . ? C22 C21 C1 118.9(2) . . ? C23 C22 C21 121.6(2) . . ? C22 C23 C24 120.4(3) . . ? C25 C24 C23 119.1(2) . . ? C24 C25 C26 121.0(3) . . ? C21 C26 C25 120.8(3) . . ? C28 C27 C31 121.3(7) . 2_656 ? C28 C27 C27 124.2(7) . 2_656 ? C31 C27 C27 114.3(8) 2_656 2_656 ? C27 C28 C29 120.2(6) . . ? C30 C29 C28 115.4(8) . . ? C29 C30 C31 129.3(11) . . ? C27 C31 C30 116.3(9) 2_656 . ? _refine_diff_density_max 0.175 _refine_diff_density_min -0.190 _refine_diff_density_rms 0.043 data_5.mesitylene _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ' 4-(triphenylmethyl)benzoic acid mesitylene clathrate ' _chemical_formula_moiety '(C26 H20 O2). (C9 H12)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C35 H32 O2' _chemical_formula_weight 484.61 _chemical_melting_point ' 258 deg C ' _chemical_compound_source ? 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 7.390(1) _cell_length_b 13.637(1) _cell_length_c 14.349(1) _cell_angle_alpha 75.92(1) _cell_angle_beta 81.64(1) _cell_angle_gamma 85.16(1) _cell_volume 1385.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5 _cell_measurement_theta_max 15 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.161 _exptl_crystal_density_method ? _exptl_crystal_F_000 516 _exptl_absorpt_coefficient_mu 0.070 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.925 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; Rigaku RU-200 rotating-anode generator powered at 50kV and 90mA ; _diffrn_radiation_monochromator graphite _diffrn_measurement_device ; Rigaku AFC7R four-circle diffractometer ; _diffrn_measurement_method '\w scan' _diffrn_standards_number 3 _diffrn_standards_interval_count 197 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4748 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0708 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4537 _reflns_number_observed 2311 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'MSC/AFC' _computing_cell_refinement 'MSC/AFC' _computing_data_reduction 'MSC/AFC' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL-PC' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0768P)^2^+0.0038P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4537 _refine_ls_number_parameters 334 _refine_ls_number_restraints 267 _refine_ls_R_factor_all 0.1321 _refine_ls_R_factor_obs 0.0493 _refine_ls_wR_factor_all 0.1585 _refine_ls_wR_factor_obs 0.1309 _refine_ls_goodness_of_fit_all 1.013 _refine_ls_goodness_of_fit_obs 1.215 _refine_ls_restrained_S_all 0.989 _refine_ls_restrained_S_obs 1.152 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group C1 C 0.1780(3) 0.27387(15) 0.85896(15) 0.0419(5) Uani 1 d . . C2 C 0.3239(3) 0.32523(15) 0.7764(2) 0.0420(5) Uani 1 d D . C3 C 0.4432(3) 0.3871(2) 0.7986(2) 0.0503(6) Uani 1 d D . H3 H 0.4261(3) 0.3999(2) 0.8602(2) 0.060 Uiso 1 calc R . C4 C 0.5849(3) 0.4299(2) 0.7332(2) 0.0538(6) Uani 1 d D . H4 H 0.6625(3) 0.4707(2) 0.7507(2) 0.065 Uiso 1 calc R . C5 C 0.6126(3) 0.4126(2) 0.6414(2) 0.0503(6) Uani 1 d D . C6 C 0.4948(3) 0.3527(2) 0.6160(2) 0.0552(6) Uani 1 d D . H6 H 0.5119(3) 0.3410(2) 0.5540(2) 0.066 Uiso 1 calc R . C7 C 0.3505(3) 0.3097(2) 0.6833(2) 0.0488(6) Uani 1 d D . H7 H 0.2710(3) 0.2702(2) 0.6655(2) 0.059 Uiso 1 calc R . C8 C 0.7748(3) 0.4541(2) 0.5756(2) 0.0610(7) Uani 1 d D . O1 O 0.8047(2) 0.42915(15) 0.49333(14) 0.0871(6) Uani 1 d . . H1 H 0.8970(2) 0.45554(15) 0.46176(14) 0.105 Uiso 1 calc R . O2 O 0.8786(3) 0.5064(2) 0.60045(14) 0.0908(6) Uani 1 d . . C9 C 0.2877(3) 0.2243(2) 0.9441(2) 0.0440(5) Uani 1 d D . C10 C 0.2437(3) 0.2384(2) 1.0369(2) 0.0542(6) Uani 1 d D . H10 H 0.1400(3) 0.2783(2) 1.0515(2) 0.065 Uiso 1 calc R . C11 C 0.3517(4) 0.1941(2) 1.1087(2) 0.0672(7) Uani 1 d D . H11 H 0.3199(4) 0.2047(2) 1.1707(2) 0.081 Uiso 1 calc R . C12 C 0.5045(4) 0.1348(2) 1.0894(2) 0.0684(7) Uani 1 d D . H12 H 0.5757(4) 0.1047(2) 1.1381(2) 0.082 Uiso 1 calc R . C13 C 0.5519(3) 0.1202(2) 0.9973(2) 0.0611(7) Uani 1 d D . H13 H 0.6562(3) 0.0806(2) 0.9832(2) 0.073 Uiso 1 calc R . C14 C 0.4444(3) 0.1644(2) 0.9263(2) 0.0522(6) Uani 1 d D . H14 H 0.4777(3) 0.1538(2) 0.8643(2) 0.063 Uiso 1 calc R . C15 C 0.0303(3) 0.3531(2) 0.8856(2) 0.0451(5) Uani 1 d D . C16 C 0.0346(3) 0.4553(2) 0.8456(2) 0.0529(6) Uani 1 d D . H16 H 0.1307(3) 0.4797(2) 0.7983(2) 0.063 Uiso 1 calc R . C17 C -0.1002(3) 0.5230(2) 0.8737(2) 0.0656(7) Uani 1 d D . H17 H -0.0934(3) 0.5918(2) 0.8453(2) 0.079 Uiso 1 calc R . C18 C -0.2437(3) 0.4892(2) 0.9432(2) 0.0695(8) Uani 1 d D . H18 H -0.3322(3) 0.5348(2) 0.9637(2) 0.083 Uiso 1 calc R . C19 C -0.2547(3) 0.3871(2) 0.9819(2) 0.0669(7) Uani 1 d D . H19 H -0.3532(3) 0.3630(2) 1.0276(2) 0.080 Uiso 1 calc R . C20 C -0.1207(3) 0.3200(2) 0.9533(2) 0.0567(6) Uani 1 d D . H20 H -0.1310(3) 0.2510(2) 0.9797(2) 0.068 Uiso 1 calc R . C21 C 0.0773(3) 0.1934(2) 0.8292(2) 0.0425(5) Uani 1 d D . C22 C -0.0403(3) 0.2245(2) 0.7595(2) 0.0521(6) Uani 1 d D . H22 H -0.0547(3) 0.2931(2) 0.7308(2) 0.063 Uiso 1 calc R . C23 C -0.1368(3) 0.1566(2) 0.7315(2) 0.0627(7) Uani 1 d D . H23 H -0.2128(3) 0.1795(2) 0.6835(2) 0.075 Uiso 1 calc R . C24 C -0.1205(3) 0.0550(2) 0.7744(2) 0.0658(7) Uani 1 d D . H24 H -0.1854(3) 0.0090(2) 0.7559(2) 0.079 Uiso 1 calc R . C25 C -0.0076(3) 0.0224(2) 0.8448(2) 0.0637(7) Uani 1 d D . H25 H 0.0034(3) -0.0461(2) 0.8745(2) 0.076 Uiso 1 calc R . C26 C 0.0906(3) 0.0911(2) 0.8723(2) 0.0515(6) Uani 1 d D . H26 H 0.1663(3) 0.0679(2) 0.9203(2) 0.062 Uiso 1 calc R . C27 C 0.4996(5) 0.9499(2) 0.6361(2) 0.0762(8) Uani 1 d D . C28 C 0.3846(5) 0.8712(3) 0.6712(2) 0.0880(9) Uani 1 d D . H28 H 0.2648(5) 0.8847(3) 0.6970(2) 0.106 Uiso 1 calc R . C29 C 0.4432(6) 0.7721(3) 0.6691(2) 0.1034(11) Uani 1 d D . C30 C 0.6200(7) 0.7543(3) 0.6297(3) 0.1203(14) Uani 1 d D . H30 H 0.6608(7) 0.6881(3) 0.6286(3) 0.144 Uiso 1 calc R . C31 C 0.7375(6) 0.8294(4) 0.5923(3) 0.1122(13) Uani 1 d D . C32 C 0.6754(5) 0.9269(3) 0.5967(2) 0.0928(10) Uani 1 d D . H32 H 0.7551(5) 0.9791(3) 0.5721(2) 0.111 Uiso 1 calc R . C33 C 0.4387(5) 1.0564(2) 0.6403(2) 0.1046(11) Uani 1 d D . H33A H 0.5376(5) 1.1000(2) 0.6124(2) 0.157 Uiso 1 calc R . H33B H 0.4029(5) 1.0596(2) 0.7066(2) 0.157 Uiso 1 calc R . H33C H 0.3364(5) 1.0777(2) 0.6046(2) 0.157 Uiso 1 calc R . C34 C 0.3118(7) 0.6877(3) 0.7128(3) 0.172(2) Uani 1 d D . H34A H 0.1958(7) 0.7161(3) 0.7362(3) 0.258 Uiso 1 calc R . H34B H 0.3615(7) 0.6408(3) 0.7655(3) 0.258 Uiso 1 calc R . H34C H 0.2954(7) 0.6529(3) 0.6641(3) 0.258 Uiso 1 calc R . C35 C 0.9302(6) 0.8076(4) 0.5460(4) 0.183(2) Uani 1 d D . H35A H 0.9929(6) 0.8695(4) 0.5238(4) 0.274 Uiso 1 calc R . H35B H 0.9242(6) 0.7784(4) 0.4921(4) 0.274 Uiso 1 calc R . H35C H 0.9954(6) 0.7610(4) 0.5929(4) 0.274 Uiso 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 C1 0.0352(11) 0.0389(12) 0.0495(13) -0.0096(10) 0.0018(10) -0.0040(9) C2 0.0333(11) 0.0393(12) 0.0504(14) -0.0076(10) -0.0005(10) -0.0025(9) C3 0.0433(12) 0.0562(14) 0.0508(14) -0.0130(11) 0.0006(11) -0.0095(11) C4 0.0428(13) 0.0577(15) 0.061(2) -0.0167(12) 0.0015(12) -0.0118(11) C5 0.0404(12) 0.0444(13) 0.059(2) -0.0034(11) 0.0033(11) -0.0030(10) C6 0.0538(14) 0.059(2) 0.0501(14) -0.0123(12) 0.0041(12) -0.0064(12) C7 0.0433(12) 0.0482(13) 0.0535(15) -0.0095(11) -0.0014(11) -0.0094(10) C8 0.058(2) 0.062(2) 0.057(2) -0.0107(13) 0.0113(13) -0.0108(13) O1 0.0757(12) 0.110(2) 0.0731(13) -0.0266(11) 0.0263(10) -0.0405(11) O2 0.0768(13) 0.114(2) 0.0854(14) -0.0382(12) 0.0266(11) -0.0494(12) C9 0.0423(12) 0.0433(12) 0.0466(13) -0.0103(10) -0.0017(10) -0.0104(10) C10 0.0539(14) 0.0539(15) 0.056(2) -0.0157(12) -0.0037(12) -0.0092(11) C11 0.075(2) 0.075(2) 0.053(2) -0.0147(13) -0.0105(14) -0.014(2) C12 0.071(2) 0.065(2) 0.068(2) -0.0007(14) -0.0276(14) -0.0106(15) C13 0.0510(14) 0.052(2) 0.078(2) -0.0084(13) -0.0125(14) -0.0023(12) C14 0.0455(13) 0.0530(14) 0.0554(14) -0.0086(11) -0.0053(11) -0.0024(11) C15 0.0359(11) 0.0480(13) 0.0538(13) -0.0180(11) -0.0013(10) -0.0054(10) C16 0.0462(13) 0.0455(14) 0.067(2) -0.0163(12) 0.0008(11) -0.0067(11) C17 0.059(2) 0.0491(15) 0.091(2) -0.0267(13) -0.0070(15) 0.0051(13) C18 0.0491(15) 0.072(2) 0.098(2) -0.046(2) -0.0045(14) 0.0097(13) C19 0.0433(14) 0.082(2) 0.079(2) -0.034(2) 0.0060(13) -0.0011(13) C20 0.0443(13) 0.0566(15) 0.068(2) -0.0171(12) 0.0023(12) -0.0068(11) C21 0.0353(11) 0.0440(13) 0.0482(13) -0.0139(10) 0.0020(10) -0.0052(10) C22 0.0460(13) 0.0494(14) 0.0609(15) -0.0109(11) -0.0100(12) -0.0021(11) C23 0.0537(14) 0.071(2) 0.068(2) -0.0202(14) -0.0124(12) -0.0096(13) C24 0.061(2) 0.064(2) 0.080(2) -0.0280(15) -0.0093(14) -0.0192(13) C25 0.069(2) 0.0445(14) 0.077(2) -0.0118(13) -0.0075(15) -0.0116(12) C26 0.0516(13) 0.0462(14) 0.0554(15) -0.0078(11) -0.0068(11) -0.0082(11) C27 0.109(2) 0.067(2) 0.062(2) -0.0231(14) -0.031(2) 0.003(2) C28 0.111(2) 0.084(2) 0.075(2) -0.022(2) -0.023(2) -0.011(2) C29 0.160(3) 0.071(2) 0.086(2) -0.009(2) -0.044(2) -0.018(2) C30 0.177(4) 0.092(3) 0.101(3) -0.030(2) -0.055(3) 0.028(3) C31 0.129(3) 0.124(3) 0.090(3) -0.040(2) -0.031(2) 0.034(3) C32 0.116(3) 0.092(2) 0.073(2) -0.021(2) -0.020(2) -0.006(2) C33 0.145(3) 0.079(2) 0.102(2) -0.036(2) -0.037(2) 0.000(2) C34 0.246(5) 0.096(3) 0.173(4) 0.002(3) -0.061(4) -0.054(3) C35 0.151(4) 0.226(5) 0.176(5) -0.083(4) -0.020(4) 0.072(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 C1 C15 1.545(3) . ? C1 C9 1.549(3) . ? C1 C21 1.549(3) . ? C1 C2 1.551(3) . ? C2 C7 1.387(3) . ? C2 C3 1.389(3) . ? C3 C4 1.367(3) . ? C4 C5 1.378(3) . ? C5 C6 1.384(3) . ? C5 C8 1.474(3) . ? C6 C7 1.394(3) . ? C8 O2 1.232(3) . ? C8 O1 1.291(3) . ? C9 C10 1.381(3) . ? C9 C14 1.389(3) . ? C10 C11 1.384(3) . ? C11 C12 1.367(3) . ? C12 C13 1.375(3) . ? C13 C14 1.375(3) . ? C15 C16 1.373(3) . ? C15 C20 1.397(3) . ? C16 C17 1.385(3) . ? C17 C18 1.372(3) . ? C18 C19 1.373(3) . ? C19 C20 1.377(3) . ? C21 C26 1.382(3) . ? C21 C22 1.385(3) . ? C22 C23 1.380(3) . ? C23 C24 1.374(3) . ? C24 C25 1.370(3) . ? C25 C26 1.392(3) . ? C27 C28 1.376(4) . ? C27 C32 1.382(4) . ? C27 C33 1.496(4) . ? C28 C29 1.391(4) . ? C29 C30 1.373(5) . ? C29 C34 1.523(5) . ? C30 C31 1.355(5) . ? C31 C32 1.383(4) . ? C31 C35 1.519(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 C15 C1 C9 112.2(2) . . ? C15 C1 C21 106.8(2) . . ? C9 C1 C21 110.8(2) . . ? C15 C1 C2 110.4(2) . . ? C9 C1 C2 104.6(2) . . ? C21 C1 C2 112.1(2) . . ? C7 C2 C3 117.4(2) . . ? C7 C2 C1 124.8(2) . . ? C3 C2 C1 117.7(2) . . ? C4 C3 C2 122.3(2) . . ? C3 C4 C5 120.0(2) . . ? C4 C5 C6 119.4(2) . . ? C4 C5 C8 118.1(2) . . ? C6 C5 C8 122.4(2) . . ? C5 C6 C7 120.0(2) . . ? C2 C7 C6 120.9(2) . . ? O2 C8 O1 122.6(2) . . ? O2 C8 C5 121.1(2) . . ? O1 C8 C5 116.3(2) . . ? C10 C9 C14 117.1(2) . . ? C10 C9 C1 124.2(2) . . ? C14 C9 C1 118.6(2) . . ? C9 C10 C11 120.9(2) . . ? C12 C11 C10 120.8(2) . . ? C11 C12 C13 119.3(2) . . ? C12 C13 C14 119.7(2) . . ? C13 C14 C9 122.1(2) . . ? C16 C15 C20 116.8(2) . . ? C16 C15 C1 124.4(2) . . ? C20 C15 C1 118.7(2) . . ? C15 C16 C17 121.8(2) . . ? C18 C17 C16 120.4(2) . . ? C17 C18 C19 119.0(2) . . ? C18 C19 C20 120.4(2) . . ? C19 C20 C15 121.5(2) . . ? C26 C21 C22 117.3(2) . . ? C26 C21 C1 123.4(2) . . ? C22 C21 C1 119.2(2) . . ? C23 C22 C21 121.9(2) . . ? C24 C23 C22 120.0(2) . . ? C25 C24 C23 119.3(2) . . ? C24 C25 C26 120.5(2) . . ? C21 C26 C25 121.0(2) . . ? C28 C27 C32 117.4(3) . . ? C28 C27 C33 121.8(3) . . ? C32 C27 C33 120.8(3) . . ? C27 C28 C29 121.6(3) . . ? C30 C29 C28 118.1(3) . . ? C30 C29 C34 122.7(4) . . ? C28 C29 C34 119.2(4) . . ? C31 C30 C29 122.6(4) . . ? C30 C31 C32 117.8(4) . . ? C30 C31 C35 121.3(4) . . ? C32 C31 C35 121.0(4) . . ? C27 C32 C31 122.6(3) . . ? _refine_diff_density_max 0.153 _refine_diff_density_min -0.167 _refine_diff_density_rms 0.034 data_5.Ph-Br _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '4-(triphenylmethyl)benzoic acid bromobenzene clathrate ' _chemical_melting_point '270 deg C ' _chemical_formula_moiety '(C26 H20 O2). 0.5(C6 H5 Br)' _chemical_formula_sum ' (C26 H20 O2). 0.5(C6 H5 Br) ' _chemical_formula_weight 442.92 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3066(2) _cell_length_b 8.9943(2) _cell_length_c 18.4963(5) _cell_angle_alpha 89.764(1) _cell_angle_beta 85.946(1) _cell_angle_gamma 67.868(1) _cell_volume 1122.82(5) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.310 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 460 _exptl_absorpt_coefficient_mu 0.964 _exptl_absorpt_correction_type 'SADABS (Bruker, 1998)' _exptl_absorpt_correction_T_min 0.386 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'Bruker SMART CCD Area Detector' _diffrn_measurement_method '\w and \f scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5937 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0492 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3797 _reflns_number_gt 2621 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL NT 5.1 (Bruker, 1998)' _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^)+(0.1922P)^2^+0.2056P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.024(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3797 _refine_ls_number_parameters 308 _refine_ls_number_restraints 367 _refine_ls_R_factor_all 0.1185 _refine_ls_R_factor_gt 0.0886 _refine_ls_wR_factor_ref 0.2802 _refine_ls_wR_factor_gt 0.2516 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.004 _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 C1 C 0.6584(4) 0.6896(3) 0.30487(13) 0.0358(6) Uani 1 1 d DU . . C2 C 0.7606(4) 0.7232(3) 0.37032(13) 0.0365(6) Uani 1 1 d DU . . C3 C 0.6807(4) 0.8588(3) 0.41443(15) 0.0453(7) Uani 1 1 d DU . . H3 H 0.5580 0.9363 0.4056 0.054 Uiso 1 1 calc R . . C4 C 0.7806(5) 0.8815(4) 0.47175(17) 0.0552(8) Uani 1 1 d DU . . H4 H 0.7237 0.9733 0.5012 0.066 Uiso 1 1 calc R . . C5 C 0.9644(5) 0.7686(4) 0.48561(17) 0.0575(8) Uani 1 1 d DU . . H5 H 1.0312 0.7841 0.5241 0.069 Uiso 1 1 calc R . . C6 C 1.0461(5) 0.6340(4) 0.44191(17) 0.0539(8) Uani 1 1 d DU . . H6 H 1.1692 0.5572 0.4509 0.065 Uiso 1 1 calc R . . C7 C 0.9481(4) 0.6110(4) 0.38479(15) 0.0447(7) Uani 1 1 d DU . . H7 H 1.0070 0.5196 0.3552 0.054 Uiso 1 1 calc R . . C8 C 0.5943(4) 0.5449(3) 0.31986(14) 0.0378(6) Uani 1 1 d DU . . C9 C 0.6339(5) 0.4541(4) 0.38105(17) 0.0518(8) Uani 1 1 d DU . . H9 H 0.7045 0.4777 0.4162 0.062 Uiso 1 1 calc R . . C10 C 0.5706(5) 0.3286(4) 0.3912(2) 0.0648(9) Uani 1 1 d DU . . H10 H 0.6001 0.2683 0.4328 0.078 Uiso 1 1 calc R . . C11 C 0.4638(5) 0.2913(4) 0.3404(2) 0.0661(10) Uani 1 1 d DU . . H11 H 0.4220 0.2063 0.3473 0.079 Uiso 1 1 calc R . . C12 C 0.4205(5) 0.3823(4) 0.2791(2) 0.0561(8) Uani 1 1 d DU . . H12 H 0.3490 0.3586 0.2443 0.067 Uiso 1 1 calc R . . C13 C 0.4826(4) 0.5083(4) 0.26922(16) 0.0466(7) Uani 1 1 d DU . . H13 H 0.4498 0.5702 0.2282 0.056 Uiso 1 1 calc R . . C14 C 0.4675(4) 0.8341(3) 0.29051(15) 0.0389(6) Uani 1 1 d DU . . C15 C 0.3023(4) 0.8695(3) 0.33989(17) 0.0459(7) Uani 1 1 d DU . . H15 H 0.3102 0.8064 0.3804 0.055 Uiso 1 1 calc R . . C16 C 0.1260(4) 0.9975(4) 0.32954(19) 0.0542(8) Uani 1 1 d DU . . H16 H 0.0184 1.0197 0.3635 0.065 Uiso 1 1 calc R . . C17 C 0.1096(5) 1.0906(4) 0.2701(2) 0.0608(9) Uani 1 1 d DU . . H17 H -0.0077 1.1770 0.2635 0.073 Uiso 1 1 calc R . . C18 C 0.2700(5) 1.0546(4) 0.2199(2) 0.0627(9) Uani 1 1 d DU . . H18 H 0.2591 1.1158 0.1786 0.075 Uiso 1 1 calc R . . C19 C 0.4477(4) 0.9283(3) 0.23010(16) 0.0475(7) Uani 1 1 d DU . . H19 H 0.5545 0.9070 0.1959 0.057 Uiso 1 1 calc R . . C20 C 0.8161(4) 0.6538(3) 0.23933(13) 0.0371(6) Uani 1 1 d DU . . C21 C 0.9164(4) 0.7566(3) 0.22840(15) 0.0435(7) Uani 1 1 d DU . . H21 H 0.8839 0.8459 0.2591 0.052 Uiso 1 1 calc R . . C22 C 1.0637(4) 0.7301(4) 0.17312(16) 0.0473(7) Uani 1 1 d DU . . H22 H 1.1287 0.8009 0.1669 0.057 Uiso 1 1 calc R . . C23 C 1.1138(4) 0.5969(4) 0.12695(16) 0.0466(7) Uani 1 1 d DU . . C24 C 1.0076(5) 0.4972(4) 0.13595(18) 0.0558(8) Uani 1 1 d DU . . H24 H 1.0347 0.4109 0.1039 0.067 Uiso 1 1 calc R . . C25 C 0.8631(5) 0.5252(4) 0.19170(16) 0.0492(7) Uani 1 1 d DU . . H25 H 0.7957 0.4559 0.1974 0.059 Uiso 1 1 calc R . . C26 C 1.2795(5) 0.5590(4) 0.07051(17) 0.0556(8) Uani 1 1 d DU . . O1 O 1.3968(4) 0.6324(4) 0.07386(14) 0.0759(7) Uani 1 1 d DU . . O2 O 1.3004(4) 0.4509(4) 0.02353(15) 0.0846(8) Uani 1 1 d DU . . Br1 Br 0.7792(5) 0.1375(4) 0.09081(14) 0.2151(13) Uani 0.50 1 d PDU . . C27 C 1.0009(8) 0.0621(5) 0.0219(3) 0.090(2) Uani 0.50 1 d PDU . . C28 C 1.1636(12) 0.1006(10) 0.0052(5) 0.122(3) Uani 0.50 1 d PDU . . C29 C 1.3019(13) 0.0119(11) -0.0448(5) 0.113(3) Uani 0.50 1 d PDU . . C30 C 1.3193(15) -0.1185(14) -0.0858(8) 0.167(5) Uani 0.50 1 d PDU . . C31 C 1.1431(11) -0.1460(10) -0.0768(5) 0.187(4) Uani 0.50 1 d PDU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0346(13) 0.0384(12) 0.0359(13) 0.0010(10) -0.0011(10) -0.0155(11) C2 0.0349(12) 0.0431(13) 0.0333(13) 0.0022(11) -0.0003(10) -0.0171(11) C3 0.0434(15) 0.0474(15) 0.0439(15) -0.0020(12) -0.0035(12) -0.0156(13) C4 0.0586(18) 0.0605(17) 0.0471(17) -0.0113(14) -0.0029(14) -0.0233(15) C5 0.0602(18) 0.074(2) 0.0450(17) -0.0017(15) -0.0159(14) -0.0306(17) C6 0.0419(15) 0.0671(18) 0.0539(18) 0.0095(15) -0.0126(13) -0.0204(14) C7 0.0405(14) 0.0491(15) 0.0415(15) -0.0021(12) -0.0023(12) -0.0135(13) C8 0.0327(13) 0.0361(12) 0.0430(15) -0.0006(11) -0.0004(11) -0.0114(11) C9 0.0493(16) 0.0541(16) 0.0559(18) 0.0120(14) -0.0131(14) -0.0227(14) C10 0.065(2) 0.0556(17) 0.080(2) 0.0287(16) -0.0157(17) -0.0279(16) C11 0.0595(19) 0.0467(17) 0.099(3) 0.0126(17) -0.0099(19) -0.0277(15) C12 0.0489(17) 0.0498(16) 0.073(2) -0.0037(15) -0.0104(15) -0.0214(14) C13 0.0448(15) 0.0499(15) 0.0491(17) 0.0029(13) -0.0067(13) -0.0218(13) C14 0.0396(13) 0.0401(13) 0.0415(14) -0.0018(11) -0.0049(11) -0.0197(11) C15 0.0398(14) 0.0441(14) 0.0523(17) -0.0010(12) -0.0013(12) -0.0146(12) C16 0.0377(15) 0.0524(17) 0.069(2) -0.0106(15) -0.0037(14) -0.0127(14) C17 0.0493(17) 0.0461(17) 0.081(2) -0.0015(16) -0.0207(16) -0.0083(15) C18 0.068(2) 0.0516(17) 0.069(2) 0.0184(15) -0.0259(17) -0.0198(16) C19 0.0466(15) 0.0478(15) 0.0496(17) 0.0056(13) -0.0108(13) -0.0182(13) C20 0.0370(13) 0.0404(13) 0.0337(13) 0.0005(11) -0.0029(11) -0.0142(11) C21 0.0445(14) 0.0470(14) 0.0402(15) -0.0062(12) 0.0026(12) -0.0197(13) C22 0.0455(15) 0.0561(16) 0.0439(16) 0.0001(13) 0.0006(12) -0.0241(14) C23 0.0406(15) 0.0614(17) 0.0382(15) -0.0012(13) 0.0002(12) -0.0201(14) C24 0.0576(18) 0.0573(17) 0.0518(18) -0.0165(14) 0.0104(14) -0.0231(15) C25 0.0503(16) 0.0508(15) 0.0484(17) -0.0098(13) 0.0074(13) -0.0231(14) C26 0.0542(17) 0.074(2) 0.0434(17) -0.0056(15) 0.0028(13) -0.0302(16) O1 0.0666(14) 0.1050(18) 0.0653(15) -0.0194(14) 0.0232(12) -0.0477(15) O2 0.0770(16) 0.113(2) 0.0708(17) -0.0385(15) 0.0293(13) -0.0491(16) Br1 0.216(2) 0.191(2) 0.1445(17) 0.0350(16) 0.0208(17) 0.0222(19) C27 0.135(6) 0.066(5) 0.047(4) 0.003(3) -0.022(4) -0.012(5) C28 0.231(7) 0.099(5) 0.078(5) 0.035(4) -0.070(5) -0.102(6) C29 0.114(5) 0.149(6) 0.125(7) 0.079(5) -0.068(4) -0.094(5) C30 0.229(10) 0.101(7) 0.123(9) 0.069(5) 0.002(10) -0.012(8) C31 0.285(7) 0.054(4) 0.269(10) 0.011(6) -0.240(7) -0.077(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C14 1.546(3) . ? C1 C2 1.554(4) . ? C1 C8 1.559(4) . ? C1 C20 1.558(3) . ? C2 C3 1.378(4) . ? C2 C7 1.405(4) . ? C3 C4 1.386(4) . ? C4 C5 1.385(4) . ? C5 C6 1.368(4) . ? C6 C7 1.376(4) . ? C8 C9 1.376(4) . ? C8 C13 1.402(4) . ? C9 C10 1.379(4) . ? C10 C11 1.382(5) . ? C11 C12 1.380(5) . ? C12 C13 1.377(4) . ? C14 C19 1.382(4) . ? C14 C15 1.396(4) . ? C15 C16 1.392(4) . ? C16 C17 1.364(5) . ? C17 C18 1.379(5) . ? C18 C19 1.391(4) . ? C20 C25 1.378(4) . ? C20 C21 1.386(4) . ? C21 C22 1.383(4) . ? C22 C23 1.390(4) . ? C23 C24 1.392(4) . ? C23 C26 1.478(4) . ? C24 C25 1.375(4) . ? C26 O2 1.265(4) . ? C26 O1 1.268(4) . ? Br1 C27 1.896(6) . ? C27 C28 1.373(8) . ? C27 C27 1.389(8) 2_755 ? C27 C31 1.401(6) 2_755 ? C28 C29 1.335(8) . ? C29 C30 1.359(9) . ? C30 C31 1.398(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C14 C1 C2 111.8(2) . . ? C14 C1 C8 106.22(19) . . ? C2 C1 C8 110.7(2) . . ? C14 C1 C20 111.4(2) . . ? C2 C1 C20 105.16(19) . . ? C8 C1 C20 111.7(2) . . ? C3 C2 C7 117.5(2) . . ? C3 C2 C1 124.0(2) . . ? C7 C2 C1 118.5(2) . . ? C2 C3 C4 121.0(3) . . ? C5 C4 C3 120.6(3) . . ? C6 C5 C4 119.0(3) . . ? C5 C6 C7 120.6(3) . . ? C6 C7 C2 121.2(3) . . ? C9 C8 C13 117.7(3) . . ? C9 C8 C1 124.2(2) . . ? C13 C8 C1 118.1(2) . . ? C8 C9 C10 121.1(3) . . ? C9 C10 C11 120.9(3) . . ? C12 C11 C10 118.8(3) . . ? C13 C12 C11 120.3(3) . . ? C12 C13 C8 121.2(3) . . ? C19 C14 C15 117.5(3) . . ? C19 C14 C1 123.8(2) . . ? C15 C14 C1 118.6(2) . . ? C16 C15 C14 121.2(3) . . ? C17 C16 C15 120.6(3) . . ? C16 C17 C18 118.9(3) . . ? C17 C18 C19 121.1(3) . . ? C14 C19 C18 120.8(3) . . ? C25 C20 C21 117.9(2) . . ? C25 C20 C1 123.9(2) . . ? C21 C20 C1 118.2(2) . . ? C22 C21 C20 121.9(3) . . ? C21 C22 C23 119.6(3) . . ? C22 C23 C24 118.6(3) . . ? C22 C23 C26 121.0(3) . . ? C24 C23 C26 120.4(3) . . ? C25 C24 C23 120.7(3) . . ? C24 C25 C20 121.3(3) . . ? O2 C26 O1 123.9(3) . . ? O2 C26 C23 118.1(3) . . ? O1 C26 C23 117.9(3) . . ? C28 C27 C27 112.2(7) . 2_755 ? C28 C27 Br1 135.3(5) . . ? C27 C27 Br1 112.5(6) 2_755 . ? C29 C28 C27 118.9(7) . . ? C28 C29 C30 132.5(9) . . ? C29 C30 C31 109.3(8) . . ? C30 C31 C27 119.5(7) . 2_755 ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.814 _refine_diff_density_min -0.791 _refine_diff_density_rms 0.090 data_5.Ph-NO2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '4-(triphenylmethyl)benzoic acid nitrobenzene clathrate' _chemical_melting_point '268 deg C ' _chemical_formula_moiety '(C26 H20 O2). 0.5(C6 H5 N O2)' _chemical_formula_sum '(C26 H20 O2). 0.5(C6 H5 N O2) ' _chemical_formula_weight 425.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.340(2) _cell_length_b 8.982(2) _cell_length_c 18.366(4) _cell_angle_alpha 89.33(3) _cell_angle_beta 86.14(3) _cell_angle_gamma 67.55(3) _cell_volume 1116.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 4.56 _cell_measurement_theta_max 8.36 _exptl_crystal_description prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 448 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type 'PSI scan' _exptl_absorpt_correction_T_min 0.946 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; Rigaku RU-200 rotating-anode generator powered at 50kV / 90mA ; _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.32 _diffrn_reflns_number 4165 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0554 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3895 _reflns_number_gt 2393 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'MSC/AFC Diffractometer Control' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL-PC (Siemens, 1990)' _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^)+(0.1980P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.021(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3895 _refine_ls_number_parameters 308 _refine_ls_number_restraints 296 _refine_ls_R_factor_all 0.1446 _refine_ls_R_factor_gt 0.0905 _refine_ls_wR_factor_ref 0.2924 _refine_ls_wR_factor_gt 0.2718 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.087 _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 C1 C 0.6558(4) 0.6930(3) 0.30324(14) 0.0419(6) Uani 1 1 d D . . C2 C 0.7603(4) 0.7251(3) 0.36937(15) 0.0434(7) Uani 1 1 d D . . C3 C 0.6785(4) 0.8606(4) 0.41383(16) 0.0508(7) Uani 1 1 d D . . H3 H 0.5544 0.9372 0.4054 0.061 Uiso 1 1 calc R . . C4 C 0.7800(5) 0.8833(4) 0.47102(18) 0.0610(9) Uani 1 1 d D . . H4 H 0.7241 0.9763 0.4998 0.073 Uiso 1 1 calc R . . C5 C 0.9623(5) 0.7705(4) 0.48580(18) 0.0647(9) Uani 1 1 d D . . H5 H 1.0278 0.7852 0.5250 0.078 Uiso 1 1 calc R . . C6 C 1.0461(5) 0.6349(4) 0.44125(18) 0.0604(9) Uani 1 1 d D . . H6 H 1.1697 0.5580 0.4500 0.072 Uiso 1 1 calc R . . C7 C 0.9453(4) 0.6142(4) 0.38360(16) 0.0513(8) Uani 1 1 d D . . H7 H 1.0036 0.5233 0.3536 0.062 Uiso 1 1 calc R . . C8 C 0.4626(4) 0.8388(3) 0.28947(15) 0.0442(7) Uani 1 1 d D . . C9 C 0.3010(4) 0.8723(4) 0.33789(17) 0.0509(8) Uani 1 1 d D . . H9 H 0.3105 0.8076 0.3785 0.061 Uiso 1 1 calc R . . C10 C 0.1226(5) 1.0010(4) 0.3281(2) 0.0620(9) Uani 1 1 d D . . H10 H 0.0158 1.0213 0.3621 0.074 Uiso 1 1 calc R . . C11 C 0.1052(5) 1.0966(4) 0.2686(2) 0.0688(10) Uani 1 1 d D . . H11 H -0.0128 1.1827 0.2617 0.083 Uiso 1 1 calc R . . C12 C 0.2662(5) 1.0633(4) 0.2186(2) 0.0684(10) Uani 1 1 d D . . H12 H 0.2550 1.1268 0.1775 0.082 Uiso 1 1 calc R . . C13 C 0.4436(5) 0.9370(4) 0.22879(18) 0.0546(8) Uani 1 1 d D . . H13 H 0.5505 0.9176 0.1950 0.066 Uiso 1 1 calc R . . C14 C 0.5938(4) 0.5476(3) 0.31785(15) 0.0449(7) Uani 1 1 d D . . C15 C 0.6341(5) 0.4566(4) 0.38056(18) 0.0573(8) Uani 1 1 d D . . H15 H 0.7048 0.4798 0.4159 0.069 Uiso 1 1 calc R . . C16 C 0.5694(5) 0.3309(4) 0.3908(2) 0.0734(11) Uani 1 1 d D . . H16 H 0.5982 0.2702 0.4329 0.088 Uiso 1 1 calc R . . C17 C 0.4632(5) 0.2946(4) 0.3396(2) 0.0739(11) Uani 1 1 d D . . H17 H 0.4218 0.2093 0.3465 0.089 Uiso 1 1 calc R . . C18 C 0.4200(5) 0.3861(4) 0.2785(2) 0.0632(9) Uani 1 1 d D . . H18 H 0.3473 0.3636 0.2437 0.076 Uiso 1 1 calc R . . C19 C 0.4826(4) 0.5111(4) 0.26796(18) 0.0529(8) Uani 1 1 d D . . H19 H 0.4497 0.5729 0.2263 0.063 Uiso 1 1 calc R . . C20 C 0.8107(4) 0.6595(3) 0.23756(15) 0.0442(7) Uani 1 1 d D . . C21 C 0.9139(4) 0.7616(4) 0.22638(16) 0.0497(7) Uani 1 1 d D . . H21 H 0.8822 0.8512 0.2568 0.060 Uiso 1 1 calc R . . C22 C 1.0602(4) 0.7330(4) 0.17180(17) 0.0516(8) Uani 1 1 d D . . H22 H 1.1279 0.8017 0.1662 0.062 Uiso 1 1 calc R . . C23 C 1.1080(4) 0.6010(4) 0.12469(17) 0.0530(8) Uani 1 1 d D . . C24 C 1.0048(5) 0.5012(4) 0.13337(18) 0.0594(9) Uani 1 1 d D . . H24 H 1.0339 0.4142 0.1015 0.071 Uiso 1 1 calc R . . C25 C 0.8573(5) 0.5293(4) 0.18946(18) 0.0539(8) Uani 1 1 d D . . H25 H 0.7895 0.4607 0.1948 0.065 Uiso 1 1 calc R . . C26 C 1.2769(5) 0.5604(4) 0.06963(18) 0.0601(9) Uani 1 1 d D . . O1 O 1.3011(4) 0.4493(4) 0.02413(16) 0.0939(9) Uani 1 1 d D . . H1 H 1.3999 0.4354 -0.0030 0.141 Uiso 1 1 calc R . . O2 O 1.3891(4) 0.6376(4) 0.07013(16) 0.0860(8) Uani 1 1 d D . . C27 C 1.0033(11) 0.9365(8) -0.0218(4) 0.165(6) Uani 0.50 1 d PDU . . C28 C 1.1664(12) 0.8711(11) -0.0704(4) 0.159(4) Uani 0.50 1 d PDU . . C29 C 1.3141(13) 0.9220(12) -0.0741(4) 0.149(4) Uani 0.50 1 d PDU . . C30 C 1.3320(18) 1.0208(16) -0.0237(8) 0.227(6) Uani 0.50 1 d PDU . . C31 C 1.1583(16) 1.1005(16) 0.0173(9) 0.187(7) Uani 0.50 1 d PDU . . O3 O 1.181(2) 0.754(2) -0.1024(12) 0.371(10) Uani 0.50 1 d PDU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0418(14) 0.0451(14) 0.0403(15) 0.0000(11) -0.0033(12) -0.0182(12) C2 0.0424(14) 0.0501(15) 0.0398(15) 0.0020(12) -0.0008(12) -0.0203(12) C3 0.0500(15) 0.0525(16) 0.0486(17) -0.0046(13) -0.0035(13) -0.0182(13) C4 0.072(2) 0.0666(19) 0.0482(18) -0.0104(15) -0.0053(16) -0.0304(17) C5 0.0657(19) 0.086(2) 0.0520(19) -0.0019(17) -0.0154(16) -0.0375(18) C6 0.0499(17) 0.075(2) 0.0580(19) 0.0012(16) -0.0078(15) -0.0247(16) C7 0.0442(15) 0.0618(18) 0.0488(17) -0.0026(14) -0.0035(13) -0.0209(14) C8 0.0440(14) 0.0472(15) 0.0466(16) -0.0022(12) -0.0062(12) -0.0225(12) C9 0.0484(16) 0.0505(16) 0.0539(18) -0.0009(14) -0.0052(14) -0.0188(13) C10 0.0484(17) 0.063(2) 0.071(2) -0.0093(17) -0.0041(16) -0.0164(15) C11 0.0584(19) 0.0463(18) 0.097(3) -0.0029(18) -0.0222(19) -0.0120(15) C12 0.074(2) 0.0567(19) 0.073(2) 0.0152(17) -0.0179(19) -0.0218(17) C13 0.0543(17) 0.0574(18) 0.0530(18) 0.0069(14) -0.0116(14) -0.0212(14) C14 0.0393(13) 0.0437(15) 0.0484(16) -0.0025(13) 0.0017(12) -0.0128(12) C15 0.0553(17) 0.0582(18) 0.061(2) 0.0112(15) -0.0152(15) -0.0232(15) C16 0.075(2) 0.062(2) 0.091(3) 0.0272(19) -0.020(2) -0.0327(17) C17 0.076(2) 0.0553(19) 0.101(3) 0.009(2) -0.013(2) -0.0361(17) C18 0.0613(18) 0.0586(19) 0.076(2) -0.0037(17) -0.0097(17) -0.0289(15) C19 0.0512(16) 0.0549(17) 0.0552(18) -0.0016(14) -0.0037(14) -0.0233(14) C20 0.0443(14) 0.0483(15) 0.0411(15) 0.0002(12) -0.0042(12) -0.0188(12) C21 0.0535(16) 0.0512(16) 0.0481(17) -0.0054(13) 0.0020(14) -0.0247(13) C22 0.0506(15) 0.0593(17) 0.0510(17) -0.0022(14) 0.0018(14) -0.0283(14) C23 0.0482(16) 0.0629(19) 0.0460(17) -0.0008(14) 0.0019(13) -0.0201(14) C24 0.0650(19) 0.0623(19) 0.0502(18) -0.0187(15) 0.0090(15) -0.0251(16) C25 0.0562(16) 0.0564(17) 0.0558(18) -0.0076(14) 0.0035(14) -0.0300(14) C26 0.0608(18) 0.074(2) 0.0453(18) -0.0113(16) 0.0064(15) -0.0269(17) O1 0.0811(17) 0.128(2) 0.0769(19) -0.0441(17) 0.0350(14) -0.0505(16) O2 0.0773(16) 0.112(2) 0.0784(18) -0.0236(15) 0.0271(14) -0.0522(16) C27 0.110(6) 0.195(12) 0.088(8) 0.093(6) 0.021(6) 0.049(8) C28 0.150(7) 0.157(8) 0.076(6) 0.060(5) 0.029(6) 0.039(6) C29 0.118(6) 0.165(8) 0.074(5) 0.080(4) 0.044(5) 0.038(5) C30 0.257(13) 0.137(11) 0.239(15) 0.057(8) 0.046(11) -0.031(9) C31 0.237(15) 0.122(10) 0.155(12) -0.015(8) -0.021(11) -0.014(11) O3 0.333(18) 0.393(19) 0.36(2) -0.184(16) 0.153(17) -0.135(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C20 1.549(4) . ? C1 C8 1.553(4) . ? C1 C14 1.554(4) . ? C1 C2 1.564(4) . ? C2 C3 1.381(4) . ? C2 C7 1.383(4) . ? C3 C4 1.388(4) . ? C4 C5 1.378(4) . ? C5 C6 1.384(5) . ? C6 C7 1.385(4) . ? C8 C9 1.371(4) . ? C8 C13 1.394(4) . ? C9 C10 1.398(4) . ? C10 C11 1.365(5) . ? C11 C12 1.385(5) . ? C12 C13 1.384(4) . ? C14 C15 1.386(4) . ? C14 C19 1.387(4) . ? C15 C16 1.389(5) . ? C16 C17 1.378(5) . ? C17 C18 1.364(5) . ? C18 C19 1.374(4) . ? C20 C25 1.394(4) . ? C20 C21 1.400(4) . ? C21 C22 1.369(4) . ? C22 C23 1.393(4) . ? C23 C24 1.379(5) . ? C23 C26 1.479(4) . ? C24 C25 1.394(4) . ? C26 O1 1.261(4) . ? C26 O2 1.264(5) . ? C27 C31 1.346(9) 2_775 ? C27 C28 1.382(8) . ? C27 C27 1.384(9) 2_775 ? C28 O3 1.174(9) . ? C28 C29 1.325(9) . ? C29 C30 1.337(9) . ? C30 C31 1.376(9) . ? C31 C27 1.346(9) 2_775 ? 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 C20 C1 C8 111.7(2) . . ? C20 C1 C14 111.7(2) . . ? C8 C1 C14 105.9(2) . . ? C20 C1 C2 104.9(2) . . ? C8 C1 C2 111.8(2) . . ? C14 C1 C2 111.0(2) . . ? C3 C2 C7 118.0(3) . . ? C3 C2 C1 123.3(2) . . ? C7 C2 C1 118.7(2) . . ? C2 C3 C4 120.5(3) . . ? C5 C4 C3 121.1(3) . . ? C4 C5 C6 118.8(3) . . ? C5 C6 C7 119.8(3) . . ? C2 C7 C6 121.8(3) . . ? C9 C8 C13 117.7(3) . . ? C9 C8 C1 119.3(2) . . ? C13 C8 C1 122.9(2) . . ? C8 C9 C10 122.0(3) . . ? C11 C10 C9 119.9(3) . . ? C10 C11 C12 118.9(3) . . ? C13 C12 C11 121.2(3) . . ? C12 C13 C8 120.3(3) . . ? C15 C14 C19 117.5(3) . . ? C15 C14 C1 123.4(3) . . ? C19 C14 C1 119.0(2) . . ? C14 C15 C16 120.3(3) . . ? C17 C16 C15 121.1(3) . . ? C18 C17 C16 118.7(3) . . ? C17 C18 C19 120.6(3) . . ? C18 C19 C14 121.7(3) . . ? C25 C20 C21 117.7(3) . . ? C25 C20 C1 123.2(3) . . ? C21 C20 C1 119.1(2) . . ? C22 C21 C20 121.7(3) . . ? C21 C22 C23 120.2(3) . . ? C24 C23 C22 119.2(3) . . ? C24 C23 C26 119.9(3) . . ? C22 C23 C26 120.8(3) . . ? C23 C24 C25 120.6(3) . . ? C20 C25 C24 120.6(3) . . ? O1 C26 O2 123.3(3) . . ? O1 C26 C23 117.7(3) . . ? O2 C26 C23 119.1(3) . . ? C31 C27 C28 126.4(8) 2_775 . ? C31 C27 C27 116.6(9) 2_775 2_775 ? C28 C27 C27 116.8(9) . 2_775 ? O3 C28 C29 120.3(9) . . ? O3 C28 C27 116.6(10) . . ? C29 C28 C27 122.4(9) . . ? C28 C29 C30 122.3(9) . . ? C29 C30 C31 112.8(11) . . ? C27 C31 C30 126.6(11) 2_775 . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.916 _refine_diff_density_min -0.408 _refine_diff_density_rms 0.099 data_5.apohost _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ' 4-(triphenylmethyl)benzoic acid, unsolvated form ' _chemical_formula_moiety 'C26 H20 O2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H20 O2' _chemical_formula_weight 364.42 _chemical_melting_point '268 deg C ' _chemical_compound_source ? 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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 7.390(2) _cell_length_b 15.477(2) _cell_length_c 33.858(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3872.5(14) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'Take 4 still photos' _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.250 _exptl_crystal_density_method ? _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_type ABSCOR _exptl_absorpt_correction_T_min 0.743 _exptl_absorpt_correction_T_max 1.156 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; Rigaku RU-200 rotating-anode generator powered at 50kV and 90mA ; _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku RAXIS IIc' _diffrn_measurement_method ; Data was collected to 0.82\%A with 85% completeness by taking 40 oscillation photos in the range of 0 - 180\%, \D\f = 4.5\%, exposure time 10 min. per frame. Crystal to detector distance is 78.021mm, background level -40. ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7212 _diffrn_reflns_av_R_equivalents 0.0605 _diffrn_reflns_av_sigmaI/netI 0.0869 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 25.55 _reflns_number_total 2936 _reflns_number_observed 1503 _reflns_observed_criterion 'F>6sigma(F)' _computing_data_collection 'BioteX ver. 1.0 (MSC, 1995)' _computing_cell_refinement 'BioteX ver. 1.0 (MSC, 1995)' _computing_data_reduction 'BioteX ver. 1.0 (MSC, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXTL-PC (Siemens, 1990)' _computing_molecular_graphics 'SHELXTL-PC (Siemens, 1990)' _computing_publication_material ? _refine_special_details 'Refinement against F' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo) + 0.0002(Fo^2^)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment calc _refine_ls_extinction_method 'F^*^ = F [ 1 + 0.002\cF^2^/sin(2\q) ]^-1/4^' _refine_ls_extinction_coef 0.00067(11) _refine_ls_number_reflns 1503 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.0494 _refine_ls_wR_factor_obs 0.0529 _refine_ls_R_factor_all 0.1600 _refine_ls_wR_factor_all 0.0890 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.37 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/esd_max 0.066 _refine_ls_shift/esd_mean 0.003 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group C1 C 0.1124(4) 0.7171(2) 0.1340(1) 0.045(1) Uani 1 d D . C2 C -0.0122(4) 0.7703(2) 0.1064(1) 0.045(1) Uani 1 d D . C3 C -0.1551(4) 0.8177(2) 0.1229(1) 0.051(1) Uani 1 d D . H3 H -0.1738 0.8157 0.1509 0.080 Uiso 1 calc R . C4 C -0.2701(4) 0.8672(2) 0.1000(1) 0.051(1) Uani 1 d D . H4 H -0.3641 0.9008 0.1121 0.080 Uiso 1 calc R . C5 C -0.2484(4) 0.8679(2) 0.0590(1) 0.047(1) Uani 1 d D . C6 C -0.1132(4) 0.8187(2) 0.0423(1) 0.054(1) Uani 1 d D . H6 H -0.1000 0.8176 0.0141 0.080 Uiso 1 calc R . C7 C 0.0047(4) 0.7706(2) 0.0657(1) 0.050(1) Uani 1 d D . H7 H 0.0987 0.7373 0.0534 0.080 Uiso 1 calc R . C8 C -0.3654(5) 0.9216(3) 0.0337(1) 0.053(1) Uani 1 d D . O1 O -0.4615(4) 0.9791(2) 0.0494(1) 0.088(1) Uani 1 d D . H1 H -0.5240 1.0266 0.0266 0.120 Uiso 1 calc R . O2 O -0.3651(4) 0.9096(2) -0.0032(1) 0.087(1) Uani 1 d D . C9 C -0.0158(4) 0.6599(2) 0.1591(1) 0.046(1) Uani 1 d D . C10 C -0.0106(5) 0.6574(3) 0.2003(1) 0.056(1) Uani 1 d D . H10 H 0.0773 0.6911 0.2143 0.080 Uiso 1 calc R . C11 C -0.1324(5) 0.6060(3) 0.2210(1) 0.065(1) Uani 1 d D . H11 H -0.1258 0.6042 0.2493 0.080 Uiso 1 calc R . C12 C -0.2622(5) 0.5577(3) 0.2019(1) 0.064(1) Uani 1 d D . H12 H -0.3456 0.5228 0.2167 0.080 Uiso 1 calc R . C13 C -0.2702(5) 0.5606(3) 0.1612(1) 0.062(1) Uani 1 d D . H13 H -0.3597 0.5274 0.1474 0.080 Uiso 1 calc R . C14 C -0.1499(4) 0.6111(2) 0.1403(1) 0.056(1) Uani 1 d D . H14 H -0.1583 0.6128 0.1120 0.080 Uiso 1 calc R . C15 C 0.2462(4) 0.6620(2) 0.1094(1) 0.047(1) Uani 1 d D . C16 C 0.3852(4) 0.7044(3) 0.0887(1) 0.055(1) Uani 1 d D . H16 H 0.3947 0.7662 0.0905 0.080 Uiso 1 calc R . C17 C 0.5087(5) 0.6594(3) 0.0660(1) 0.061(1) Uani 1 d D . H17 H 0.6030 0.6898 0.0523 0.080 Uiso 1 calc R . C18 C 0.4964(5) 0.5710(3) 0.0630(1) 0.067(1) Uani 1 d D . H18 H 0.5805 0.5398 0.0468 0.080 Uiso 1 calc R . C19 C 0.3641(5) 0.5276(3) 0.0831(1) 0.064(1) Uani 1 d D . H19 H 0.3566 0.4658 0.0812 0.080 Uiso 1 calc R . C20 C 0.2392(5) 0.5728(2) 0.1066(1) 0.053(1) Uani 1 d D . H20 H 0.1481 0.5415 0.1209 0.080 Uiso 1 calc R . C21 C 0.2306(4) 0.7756(3) 0.1610(1) 0.049(1) Uani 1 d D . C22 C 0.3770(5) 0.7378(3) 0.1806(1) 0.059(1) Uani 1 d D . H22 H 0.4017 0.6774 0.1768 0.080 Uiso 1 calc R . C23 C 0.4875(5) 0.7856(3) 0.2057(1) 0.067(1) Uani 1 d D . H23 H 0.5861 0.7581 0.2192 0.080 Uiso 1 calc R . C24 C 0.4555(5) 0.8723(3) 0.2110(1) 0.077(1) Uani 1 d D . H24 H 0.5305 0.9056 0.2284 0.080 Uiso 1 calc R . C25 C 0.3145(5) 0.9110(3) 0.1910(1) 0.080(1) Uani 1 d D . H25 H 0.2930 0.9718 0.1943 0.080 Uiso 1 calc R . C26 C 0.2034(5) 0.8632(3) 0.1662(1) 0.066(1) Uani 1 d D . H26 H 0.1062 0.8913 0.1525 0.080 Uiso 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C1 0.052(1) 0.038(1) 0.044(1) 0.007(1) -0.008(1) -0.001(1) C2 0.047(1) 0.041(1) 0.047(1) 0.000(1) -0.006(1) 0.001(1) C3 0.054(1) 0.050(1) 0.048(1) 0.005(1) -0.002(1) 0.003(1) C4 0.050(1) 0.049(1) 0.055(1) 0.000(1) -0.001(1) 0.003(1) C5 0.046(1) 0.044(1) 0.050(1) 0.003(1) -0.006(1) 0.005(1) C6 0.057(1) 0.061(1) 0.045(1) 0.009(1) 0.002(1) 0.000(1) C7 0.056(1) 0.047(1) 0.049(1) 0.009(1) -0.003(1) 0.003(1) C8 0.052(1) 0.054(1) 0.054(1) 0.010(1) -0.003(1) 0.000(1) O1 0.101(1) 0.097(1) 0.067(1) 0.054(1) -0.015(1) -0.002(1) O2 0.103(1) 0.104(1) 0.053(1) 0.045(1) -0.012(1) 0.004(1) C9 0.048(1) 0.043(1) 0.046(1) 0.007(1) -0.003(1) 0.003(1) C10 0.060(1) 0.059(1) 0.050(1) 0.000(1) -0.002(1) 0.003(1) C11 0.074(1) 0.068(1) 0.053(1) 0.007(1) 0.003(1) 0.008(1) C12 0.064(1) 0.055(1) 0.073(1) 0.009(1) 0.015(1) 0.008(1) C13 0.054(1) 0.058(1) 0.075(1) -0.009(1) -0.001(1) 0.001(1) C14 0.058(1) 0.053(1) 0.058(1) -0.003(1) -0.004(1) 0.004(1) C15 0.048(1) 0.043(1) 0.050(1) 0.004(1) -0.007(1) 0.003(1) C16 0.050(1) 0.052(1) 0.062(1) 0.001(1) -0.004(1) 0.006(1) C17 0.052(1) 0.066(1) 0.065(1) 0.005(1) 0.002(1) 0.005(1) C18 0.058(1) 0.071(1) 0.071(1) 0.017(1) 0.000(1) 0.001(1) C19 0.068(1) 0.053(1) 0.070(1) 0.012(1) -0.007(1) -0.003(1) C20 0.057(1) 0.047(1) 0.054(1) 0.003(1) -0.002(1) 0.003(1) C21 0.058(1) 0.045(1) 0.044(1) -0.003(1) -0.005(1) 0.006(1) C22 0.061(1) 0.059(1) 0.055(1) -0.002(1) -0.009(1) 0.001(1) C23 0.060(1) 0.080(1) 0.060(1) -0.008(1) -0.013(1) 0.005(1) C24 0.097(1) 0.071(1) 0.065(1) -0.027(1) -0.017(1) -0.006(1) C25 0.105(1) 0.053(1) 0.081(1) -0.004(1) -0.022(1) 0.000(1) C26 0.081(1) 0.052(1) 0.063(1) -0.001(1) -0.020(1) -0.004(1) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.547(5) . ? C1 C9 1.551(5) . ? C1 C15 1.548(5) . ? C1 C21 1.556(5) . ? C2 C3 1.402(5) . ? C2 C7 1.385(4) . ? C3 C4 1.383(5) . ? C4 C5 1.395(4) . ? C5 C6 1.377(5) . ? C5 C8 1.475(5) . ? C6 C7 1.392(5) . ? C8 O1 1.257(5) . ? C8 O2 1.262(4) . ? C9 C10 1.394(4) . ? C9 C14 1.399(5) . ? C10 C11 1.390(5) . ? C11 C12 1.376(5) . ? C12 C13 1.380(5) . ? C13 C14 1.379(5) . ? C15 C16 1.406(5) . ? C15 C20 1.384(5) . ? C16 C17 1.382(5) . ? C17 C18 1.375(6) . ? C18 C19 1.368(5) . ? C19 C20 1.405(5) . ? C21 C22 1.399(5) . ? C21 C26 1.381(6) . ? C22 C23 1.390(5) . ? C23 C24 1.375(6) . ? C24 C25 1.379(6) . ? C25 C26 1.388(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C9 105.7(2) . . ? C2 C1 C15 110.5(3) . . ? C9 C1 C15 111.8(3) . . ? C2 C1 C21 112.2(3) . . ? C9 C1 C21 110.6(3) . . ? C15 C1 C21 106.2(2) . . ? C1 C2 C3 119.2(3) . . ? C1 C2 C7 123.3(3) . . ? C3 C2 C7 117.5(3) . . ? C2 C3 C4 122.0(3) . . ? C3 C4 C5 119.4(3) . . ? C4 C5 C6 119.1(3) . . ? C4 C5 C8 121.0(3) . . ? C6 C5 C8 119.9(3) . . ? C5 C6 C7 121.1(3) . . ? C2 C7 C6 120.8(3) . . ? C5 C8 O1 119.0(3) . . ? C5 C8 O2 119.4(3) . . ? O1 C8 O2 121.6(3) . . ? C1 C9 C10 123.3(3) . . ? C1 C9 C14 119.3(3) . . ? C10 C9 C14 117.3(3) . . ? C9 C10 C11 120.1(3) . . ? C10 C11 C12 121.7(3) . . ? C11 C12 C13 118.7(3) . . ? C12 C13 C14 120.3(3) . . ? C9 C14 C13 121.9(3) . . ? C1 C15 C16 118.4(3) . . ? C1 C15 C20 124.2(3) . . ? C16 C15 C20 117.4(3) . . ? C15 C16 C17 121.6(4) . . ? C16 C17 C18 120.0(3) . . ? C17 C18 C19 119.9(4) . . ? C18 C19 C20 120.5(4) . . ? C15 C20 C19 120.6(3) . . ? C1 C21 C22 118.0(3) . . ? C1 C21 C26 124.4(3) . . ? C22 C21 C26 117.6(3) . . ? C21 C22 C23 121.4(4) . . ? C22 C23 C24 119.9(3) . . ? C23 C24 C25 119.3(4) . . ? C24 C25 C26 120.8(4) . . ? C21 C26 C25 121.0(3) . . ? _refine_diff_density_max 0.190 _refine_diff_density_min -0.150 _refine_diff_density_rms 0.040