# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2011 data_global _journal_name_full J.Mater.Chem. _journal_coden_cambridge 1145 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Zujin Zhao' _publ_contact_author_email zjzhao@ust.hk loop_ _publ_author_name 'Zujin Zhao' 'Ben Zhong Tang' 'Chen, Shuming' 'Lam, Jacky Wing Yip' 'Wang, Zhiming' 'Lu, Ping' 'Mahtab, Faisal' 'Sung, Herman' 'Williams, Ian' 'Ma, Yuguang' 'Kwok, Hoi' 'Tang, Ben' data_zhao39cult _database_code_depnum_ccdc_archive 'CCDC 755289' #TrackingRef 'TPPyE.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H24' _chemical_formula_weight 456.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5346(6) _cell_length_b 9.5932(6) _cell_length_c 13.9476(9) _cell_angle_alpha 96.674(5) _cell_angle_beta 105.479(6) _cell_angle_gamma 94.841(5) _cell_volume 1212.24(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3040 _cell_measurement_theta_min 3.31 _cell_measurement_theta_max 71.31 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 0.537 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6354 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 67.00 _reflns_number_total 4112 _reflns_number_gt 3186 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4112 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0994 _refine_ls_wR_factor_gt 0.0960 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.63119(13) 0.52058(13) 0.23015(9) 0.0339(3) Uani 1 1 d . . . C2 C 0.63727(13) 0.40136(13) 0.17042(9) 0.0339(3) Uani 1 1 d . . . C11 C 0.51824(14) 0.53872(13) 0.28597(9) 0.0351(3) Uani 1 1 d . . . C12 C 0.47979(15) 0.43693(15) 0.34159(9) 0.0413(3) Uani 1 1 d . . . H12A H 0.5280 0.3542 0.3462 0.050 Uiso 1 1 calc R . . C13 C 0.37168(17) 0.45598(16) 0.39012(11) 0.0491(4) Uani 1 1 d . . . H13A H 0.3463 0.3861 0.4276 0.059 Uiso 1 1 calc R . . C14 C 0.30091(17) 0.57562(17) 0.38430(11) 0.0530(4) Uani 1 1 d . . . H14A H 0.2256 0.5871 0.4164 0.064 Uiso 1 1 calc R . . C15 C 0.33988(17) 0.67907(17) 0.33149(12) 0.0537(4) Uani 1 1 d . . . H15A H 0.2925 0.7623 0.3282 0.064 Uiso 1 1 calc R . . C16 C 0.44850(15) 0.66060(15) 0.28331(10) 0.0433(3) Uani 1 1 d . . . H16A H 0.4757 0.7324 0.2479 0.052 Uiso 1 1 calc R . . C21 C 0.52900(14) 0.27069(13) 0.14721(9) 0.0334(3) Uani 1 1 d . . . C22 C 0.37825(14) 0.27619(14) 0.12350(9) 0.0358(3) Uani 1 1 d . . . H22A H 0.3411 0.3648 0.1200 0.043 Uiso 1 1 calc R . . C23 C 0.28228(15) 0.15299(14) 0.10499(10) 0.0405(3) Uani 1 1 d . . . H23A H 0.1798 0.1582 0.0901 0.049 Uiso 1 1 calc R . . C24 C 0.33367(17) 0.02311(15) 0.10794(11) 0.0466(3) Uani 1 1 d . . . H24A H 0.2672 -0.0606 0.0966 0.056 Uiso 1 1 calc R . . C25 C 0.48215(17) 0.01539(15) 0.12740(11) 0.0472(4) Uani 1 1 d . . . H25A H 0.5181 -0.0740 0.1275 0.057 Uiso 1 1 calc R . . C26 C 0.57910(15) 0.13851(14) 0.14679(10) 0.0399(3) Uani 1 1 d . . . H26A H 0.6813 0.1324 0.1600 0.048 Uiso 1 1 calc R . . C31 C 0.76001(14) 0.38805(13) 0.12293(9) 0.0350(3) Uani 1 1 d . . . C32 C 0.90495(15) 0.40088(14) 0.18038(10) 0.0391(3) Uani 1 1 d . . . H32A H 0.9281 0.4235 0.2514 0.047 Uiso 1 1 calc R . . C33 C 1.01655(15) 0.38104(15) 0.13547(11) 0.0447(3) Uani 1 1 d . . . H33A H 1.1152 0.3889 0.1757 0.054 Uiso 1 1 calc R . . C34 C 0.98399(16) 0.34972(14) 0.03169(11) 0.0446(3) Uani 1 1 d . . . H34A H 1.0603 0.3365 0.0008 0.053 Uiso 1 1 calc R . . C35 C 0.84066(16) 0.33791(14) -0.02647(10) 0.0437(3) Uani 1 1 d . . . H35A H 0.8184 0.3174 -0.0976 0.052 Uiso 1 1 calc R . . C36 C 0.72868(15) 0.35592(14) 0.01846(10) 0.0402(3) Uani 1 1 d . . . H36A H 0.6300 0.3464 -0.0221 0.048 Uiso 1 1 calc R . . C41 C 0.73740(13) 0.64968(13) 0.23891(9) 0.0329(3) Uani 1 1 d . . . C42 C 0.84670(13) 0.70154(13) 0.32966(9) 0.0327(3) Uani 1 1 d . . . C43 C 0.86325(15) 0.63590(14) 0.41877(9) 0.0374(3) Uani 1 1 d . . . H43A H 0.7958 0.5569 0.4182 0.045 Uiso 1 1 calc R . . C44 C 0.97279(16) 0.68384(14) 0.50364(10) 0.0405(3) Uani 1 1 d . . . H44A H 0.9793 0.6386 0.5615 0.049 Uiso 1 1 calc R . . C45 C 1.07935(15) 0.80139(14) 0.50828(10) 0.0395(3) Uani 1 1 d . . . C46 C 1.06566(14) 0.87006(13) 0.42195(10) 0.0366(3) Uani 1 1 d . . . C47 C 0.94888(14) 0.82138(13) 0.33293(9) 0.0338(3) Uani 1 1 d . . . C48 C 0.93705(15) 0.89000(14) 0.24647(10) 0.0389(3) Uani 1 1 d . . . C49 C 0.82540(15) 0.83802(14) 0.15952(10) 0.0408(3) Uani 1 1 d . . . H49A H 0.8146 0.8847 0.1020 0.049 Uiso 1 1 calc R . . C50 C 0.72944(15) 0.71873(14) 0.15554(10) 0.0380(3) Uani 1 1 d . . . H50A H 0.6566 0.6834 0.0943 0.046 Uiso 1 1 calc R . . C51 C 1.19731(17) 0.84817(16) 0.59352(12) 0.0508(4) Uani 1 1 d . . . H51A H 1.2076 0.8023 0.6514 0.061 Uiso 1 1 calc R . . C52 C 1.29923(18) 0.96048(18) 0.59452(13) 0.0582(4) Uani 1 1 d . . . H52A H 1.3789 0.9906 0.6530 0.070 Uiso 1 1 calc R . . C53 C 1.28618(17) 1.02909(16) 0.51131(12) 0.0548(4) Uani 1 1 d . . . H53A H 1.3569 1.1061 0.5134 0.066 Uiso 1 1 calc R . . C54 C 1.17044(16) 0.98685(15) 0.42409(11) 0.0449(3) Uani 1 1 d . . . C55 C 1.15343(17) 1.05457(15) 0.33597(12) 0.0522(4) Uani 1 1 d . . . H55A H 1.2220 1.1327 0.3365 0.063 Uiso 1 1 calc R . . C56 C 1.04198(17) 1.00960(15) 0.25216(11) 0.0488(4) Uani 1 1 d . . . H56A H 1.0327 1.0582 0.1956 0.059 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 0.0353(6) 0.0316(7) 0.0337(6) 0.0022(5) 0.0090(5) 0.0036(5) C2 0.0338(6) 0.0326(7) 0.0345(6) 0.0018(5) 0.0095(5) 0.0035(5) C11 0.0356(6) 0.0317(7) 0.0348(6) -0.0043(5) 0.0096(5) 0.0001(5) C12 0.0479(8) 0.0378(7) 0.0375(7) -0.0013(6) 0.0154(6) -0.0001(6) C13 0.0560(9) 0.0494(9) 0.0413(7) -0.0052(6) 0.0217(7) -0.0080(7) C14 0.0484(8) 0.0576(10) 0.0546(9) -0.0104(7) 0.0269(7) -0.0007(7) C15 0.0503(9) 0.0477(9) 0.0654(10) -0.0061(8) 0.0242(7) 0.0116(7) C16 0.0459(8) 0.0363(7) 0.0491(8) 0.0004(6) 0.0178(6) 0.0051(6) C21 0.0386(7) 0.0315(6) 0.0301(6) 0.0010(5) 0.0115(5) 0.0026(5) C22 0.0393(7) 0.0307(7) 0.0383(7) 0.0023(5) 0.0135(5) 0.0040(5) C23 0.0388(7) 0.0388(7) 0.0435(7) 0.0023(6) 0.0140(6) -0.0007(6) C24 0.0532(8) 0.0326(7) 0.0533(8) 0.0024(6) 0.0182(7) -0.0042(6) C25 0.0560(9) 0.0299(7) 0.0572(8) 0.0033(6) 0.0191(7) 0.0067(6) C26 0.0408(7) 0.0356(7) 0.0433(7) 0.0021(6) 0.0127(6) 0.0068(6) C31 0.0391(7) 0.0264(6) 0.0403(7) 0.0006(5) 0.0147(5) 0.0037(5) C32 0.0408(7) 0.0369(7) 0.0394(7) 0.0017(6) 0.0120(5) 0.0064(6) C33 0.0378(7) 0.0429(8) 0.0553(8) 0.0065(7) 0.0156(6) 0.0080(6) C34 0.0490(8) 0.0358(7) 0.0579(9) 0.0049(6) 0.0303(7) 0.0075(6) C35 0.0552(8) 0.0346(7) 0.0431(7) -0.0012(6) 0.0220(6) -0.0016(6) C36 0.0402(7) 0.0376(7) 0.0396(7) -0.0027(6) 0.0116(6) -0.0028(6) C41 0.0344(6) 0.0277(6) 0.0388(6) 0.0016(5) 0.0147(5) 0.0064(5) C42 0.0366(6) 0.0259(6) 0.0373(6) 0.0008(5) 0.0145(5) 0.0052(5) C43 0.0439(7) 0.0283(6) 0.0404(7) 0.0042(5) 0.0135(6) 0.0034(5) C44 0.0509(8) 0.0326(7) 0.0385(7) 0.0054(6) 0.0125(6) 0.0068(6) C45 0.0427(7) 0.0325(7) 0.0416(7) -0.0020(6) 0.0115(6) 0.0068(6) C46 0.0385(7) 0.0268(6) 0.0446(7) -0.0038(5) 0.0155(5) 0.0034(5) C47 0.0371(6) 0.0266(6) 0.0401(7) 0.0003(5) 0.0162(5) 0.0053(5) C48 0.0462(7) 0.0304(7) 0.0450(7) 0.0040(6) 0.0217(6) 0.0037(6) C49 0.0505(8) 0.0373(7) 0.0400(7) 0.0110(6) 0.0189(6) 0.0076(6) C50 0.0417(7) 0.0356(7) 0.0378(7) 0.0036(5) 0.0130(5) 0.0066(6) C51 0.0550(9) 0.0442(8) 0.0460(8) -0.0040(7) 0.0060(7) 0.0065(7) C52 0.0523(9) 0.0535(10) 0.0555(9) -0.0113(8) 0.0032(7) -0.0016(8) C53 0.0487(8) 0.0427(8) 0.0652(10) -0.0134(7) 0.0161(7) -0.0085(7) C54 0.0452(8) 0.0335(7) 0.0548(8) -0.0070(6) 0.0194(6) -0.0014(6) C55 0.0583(9) 0.0359(8) 0.0650(10) -0.0021(7) 0.0302(8) -0.0091(7) C56 0.0614(9) 0.0374(8) 0.0536(8) 0.0069(7) 0.0283(7) -0.0019(7) _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 1.3494(17) . ? C1 C11 1.4979(17) . ? C1 C41 1.5037(17) . ? C2 C31 1.4980(17) . ? C2 C21 1.5003(17) . ? C11 C16 1.3924(19) . ? C11 C12 1.3990(19) . ? C12 C13 1.3891(19) . ? C13 C14 1.379(2) . ? C14 C15 1.385(2) . ? C15 C16 1.389(2) . ? C21 C26 1.3922(19) . ? C21 C22 1.3933(18) . ? C22 C23 1.3861(18) . ? C23 C24 1.378(2) . ? C24 C25 1.379(2) . ? C25 C26 1.3895(19) . ? C31 C32 1.3872(18) . ? C31 C36 1.3982(18) . ? C32 C33 1.3868(19) . ? C33 C34 1.387(2) . ? C34 C35 1.378(2) . ? C35 C36 1.3877(19) . ? C41 C50 1.3919(18) . ? C41 C42 1.4134(17) . ? C42 C47 1.4311(18) . ? C42 C43 1.4354(18) . ? C43 C44 1.3550(18) . ? C44 C45 1.4362(19) . ? C45 C51 1.3988(19) . ? C45 C46 1.4198(19) . ? C46 C47 1.4279(18) . ? C46 C54 1.4289(19) . ? C47 C48 1.4230(19) . ? C48 C49 1.3904(19) . ? C48 C56 1.4375(19) . ? C49 C50 1.3897(19) . ? C51 C52 1.385(2) . ? C52 C53 1.382(2) . ? C53 C54 1.398(2) . ? C54 C55 1.434(2) . ? C55 C56 1.351(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C11 124.54(11) . . ? C2 C1 C41 119.80(11) . . ? C11 C1 C41 115.56(10) . . ? C1 C2 C31 121.27(11) . . ? C1 C2 C21 125.00(11) . . ? C31 C2 C21 113.71(10) . . ? C16 C11 C12 118.21(12) . . ? C16 C11 C1 119.57(12) . . ? C12 C11 C1 122.22(12) . . ? C13 C12 C11 120.46(14) . . ? C14 C13 C12 120.47(14) . . ? C13 C14 C15 119.87(13) . . ? C14 C15 C16 119.76(15) . . ? C15 C16 C11 121.18(14) . . ? C26 C21 C22 118.19(12) . . ? C26 C21 C2 119.53(12) . . ? C22 C21 C2 122.26(12) . . ? C23 C22 C21 120.33(13) . . ? C24 C23 C22 120.81(13) . . ? C23 C24 C25 119.58(13) . . ? C24 C25 C26 119.91(14) . . ? C25 C26 C21 121.09(13) . . ? C32 C31 C36 118.60(12) . . ? C32 C31 C2 121.60(11) . . ? C36 C31 C2 119.74(12) . . ? C33 C32 C31 120.85(13) . . ? C32 C33 C34 119.95(13) . . ? C35 C34 C33 119.88(13) . . ? C34 C35 C36 120.23(13) . . ? C35 C36 C31 120.48(13) . . ? C50 C41 C42 119.13(12) . . ? C50 C41 C1 119.40(11) . . ? C42 C41 C1 121.47(11) . . ? C41 C42 C47 119.29(12) . . ? C41 C42 C43 122.66(11) . . ? C47 C42 C43 118.01(11) . . ? C44 C43 C42 121.62(12) . . ? C43 C44 C45 121.61(13) . . ? C51 C45 C46 119.09(13) . . ? C51 C45 C44 122.49(14) . . ? C46 C45 C44 118.40(12) . . ? C45 C46 C47 120.15(12) . . ? C45 C46 C54 119.70(13) . . ? C47 C46 C54 120.15(13) . . ? C48 C47 C46 119.70(12) . . ? C48 C47 C42 120.10(12) . . ? C46 C47 C42 120.17(12) . . ? C49 C48 C47 118.78(12) . . ? C49 C48 C56 122.56(13) . . ? C47 C48 C56 118.66(13) . . ? C50 C49 C48 120.97(13) . . ? C49 C50 C41 121.67(12) . . ? C52 C51 C45 120.80(16) . . ? C53 C52 C51 120.62(15) . . ? C52 C53 C54 121.02(14) . . ? C53 C54 C46 118.76(15) . . ? C53 C54 C55 122.77(14) . . ? C46 C54 C55 118.47(13) . . ? C56 C55 C54 121.39(13) . . ? C55 C56 C48 121.59(14) . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 66.50 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.148 _refine_diff_density_min -0.183 _refine_diff_density_rms 0.036 # Attachment 'cis-DPDPyE.cif' data_zhao41 _database_code_depnum_ccdc_archive 'CCDC 755290' #TrackingRef 'cis-DPDPyE.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H29 Cl3' _chemical_formula_weight 700.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7695(6) _cell_length_b 13.3414(11) _cell_length_c 15.9829(11) _cell_angle_alpha 77.119(8) _cell_angle_beta 89.166(6) _cell_angle_gamma 71.187(6) _cell_volume 1722.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5624 _cell_measurement_theta_min 3.58 _cell_measurement_theta_max 71.26 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 2.667 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.56 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8722 _diffrn_reflns_av_R_equivalents 0.0649 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.60 _diffrn_reflns_theta_max 66.99 _reflns_number_total 5520 _reflns_number_gt 4415 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1480P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5520 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0875 _refine_ls_R_factor_gt 0.0747 _refine_ls_wR_factor_ref 0.2066 _refine_ls_wR_factor_gt 0.1970 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4529(4) 0.7494(3) 0.1662(2) 0.0551(8) Uani 1 1 d . . . H1A H 0.5584 0.6973 0.1558 0.066 Uiso 1 1 calc R . . Cl1 Cl 0.33936(12) 0.80640(8) 0.06852(6) 0.0654(3) Uani 1 1 d . . . Cl2 Cl 0.35302(13) 0.67626(10) 0.23945(7) 0.0813(4) Uani 1 1 d . . . Cl3 Cl 0.49232(14) 0.84791(10) 0.21002(8) 0.0793(4) Uani 1 1 d . . . C10 C 0.5574(3) 0.2134(2) 0.25638(18) 0.0356(6) Uani 1 1 d . . . C11 C 0.7173(3) 0.1405(2) 0.23812(18) 0.0362(6) Uani 1 1 d . . . C12 C 0.8040(4) 0.1796(3) 0.1729(2) 0.0455(7) Uani 1 1 d . . . H12A H 0.7634 0.2535 0.1421 0.055 Uiso 1 1 calc R . . C13 C 0.9509(4) 0.1113(4) 0.1520(2) 0.0590(9) Uani 1 1 d . . . H13A H 1.0090 0.1394 0.1074 0.071 Uiso 1 1 calc R . . C14 C 1.0111(4) 0.0045(4) 0.1953(2) 0.0608(10) Uani 1 1 d . . . H14A H 1.1107 -0.0415 0.1811 0.073 Uiso 1 1 calc R . . C15 C 0.9246(4) -0.0357(3) 0.2605(2) 0.0526(8) Uani 1 1 d . . . H15A H 0.9656 -0.1097 0.2908 0.063 Uiso 1 1 calc R . . C16 C 0.7788(4) 0.0313(3) 0.2816(2) 0.0435(7) Uani 1 1 d . . . H16A H 0.7207 0.0026 0.3259 0.052 Uiso 1 1 calc R . . C20 C 0.4966(3) 0.2153(2) 0.33364(18) 0.0347(6) Uani 1 1 d . . . C21 C 0.5875(3) 0.1613(2) 0.41982(17) 0.0342(6) Uani 1 1 d . . . C22 C 0.7484(3) 0.1508(2) 0.4326(2) 0.0410(6) Uani 1 1 d . . . H22A H 0.8050 0.1762 0.3860 0.049 Uiso 1 1 calc R . . C23 C 0.8274(4) 0.1030(3) 0.5138(2) 0.0481(7) Uani 1 1 d . . . H23A H 0.9379 0.0956 0.5219 0.058 Uiso 1 1 calc R . . C24 C 0.7471(4) 0.0661(3) 0.5827(2) 0.0517(8) Uani 1 1 d . . . H24A H 0.8013 0.0339 0.6380 0.062 Uiso 1 1 calc R . . C25 C 0.5872(4) 0.0768(3) 0.5697(2) 0.0524(8) Uani 1 1 d . . . H25A H 0.5312 0.0505 0.6163 0.063 Uiso 1 1 calc R . . C26 C 0.5068(3) 0.1255(3) 0.4897(2) 0.0417(6) Uani 1 1 d . . . H26A H 0.3955 0.1344 0.4824 0.050 Uiso 1 1 calc R . . C31 C 0.4599(3) 0.2925(2) 0.17786(18) 0.0366(6) Uani 1 1 d . . . C32 C 0.3928(3) 0.2601(2) 0.11363(18) 0.0362(6) Uani 1 1 d . . . C33 C 0.4090(3) 0.1478(2) 0.1177(2) 0.0405(6) Uani 1 1 d . . . H33A H 0.4706 0.0928 0.1646 0.049 Uiso 1 1 calc R . . C34 C 0.3383(4) 0.1191(3) 0.0563(2) 0.0445(7) Uani 1 1 d . . . H34A H 0.3528 0.0444 0.0605 0.053 Uiso 1 1 calc R . . C35 C 0.2418(4) 0.1994(3) -0.0152(2) 0.0461(7) Uani 1 1 d . . . C36 C 0.2254(3) 0.3094(3) -0.02227(19) 0.0430(7) Uani 1 1 d . . . C37 C 0.3009(3) 0.3399(2) 0.04167(18) 0.0378(6) Uani 1 1 d . . . C38 C 0.2809(4) 0.4525(3) 0.0353(2) 0.0442(7) Uani 1 1 d . . . C39 C 0.3521(4) 0.4807(3) 0.0987(2) 0.0505(8) Uani 1 1 d . . . H39A H 0.3419 0.5549 0.0939 0.061 Uiso 1 1 calc R . . C40 C 0.4382(4) 0.4030(3) 0.1693(2) 0.0444(7) Uani 1 1 d . . . H40A H 0.4835 0.4251 0.2128 0.053 Uiso 1 1 calc R . . C41 C 0.1641(4) 0.1719(4) -0.0779(2) 0.0610(9) Uani 1 1 d . . . H41A H 0.1746 0.0978 -0.0739 0.073 Uiso 1 1 calc R . . C42 C 0.0720(5) 0.2511(4) -0.1458(3) 0.0680(10) Uani 1 1 d . . . H42A H 0.0208 0.2309 -0.1882 0.082 Uiso 1 1 calc R . . C43 C 0.0539(4) 0.3592(4) -0.1525(2) 0.0633(10) Uani 1 1 d . . . H43A H -0.0113 0.4126 -0.1991 0.076 Uiso 1 1 calc R . . C44 C 0.1297(4) 0.3917(3) -0.0921(2) 0.0517(8) Uani 1 1 d . . . C45 C 0.1137(4) 0.5022(3) -0.0971(2) 0.0582(9) Uani 1 1 d . . . H45A H 0.0511 0.5567 -0.1440 0.070 Uiso 1 1 calc R . . C46 C 0.1850(4) 0.5314(3) -0.0373(2) 0.0569(9) Uani 1 1 d . . . H46A H 0.1718 0.6062 -0.0429 0.068 Uiso 1 1 calc R . . C51 C 0.3206(3) 0.2757(2) 0.33613(18) 0.0357(6) Uani 1 1 d . . . C52 C 0.2632(3) 0.3720(2) 0.36554(17) 0.0340(6) Uani 1 1 d . . . C53 C 0.3696(3) 0.4211(2) 0.39653(18) 0.0378(6) Uani 1 1 d . . . H53A H 0.4829 0.3854 0.3997 0.045 Uiso 1 1 calc R . . C54 C 0.3126(3) 0.5160(2) 0.42098(19) 0.0388(6) Uani 1 1 d . . . H54A H 0.3866 0.5451 0.4413 0.047 Uiso 1 1 calc R . . C55 C 0.1426(3) 0.5742(2) 0.41718(19) 0.0405(6) Uani 1 1 d . . . C56 C 0.0340(3) 0.5281(2) 0.38755(17) 0.0374(6) Uani 1 1 d . . . C57 C 0.0938(3) 0.4278(2) 0.36233(17) 0.0352(6) Uani 1 1 d . . . C58 C -0.0166(3) 0.3836(2) 0.33293(18) 0.0385(6) Uani 1 1 d . . . C59 C 0.0439(3) 0.2862(2) 0.30559(19) 0.0407(6) Uani 1 1 d . . . H59A H -0.0287 0.2558 0.2855 0.049 Uiso 1 1 calc R . . C60 C 0.2091(3) 0.2335(2) 0.30750(19) 0.0393(6) Uani 1 1 d . . . H60A H 0.2474 0.1674 0.2890 0.047 Uiso 1 1 calc R . . C61 C 0.0811(4) 0.6730(3) 0.4407(2) 0.0466(7) Uani 1 1 d . . . H61A H 0.1537 0.7044 0.4594 0.056 Uiso 1 1 calc R . . C62 C -0.0829(4) 0.7269(3) 0.4377(2) 0.0527(8) Uani 1 1 d . . . H62A H -0.1223 0.7938 0.4550 0.063 Uiso 1 1 calc R . . C63 C -0.1907(4) 0.6823(3) 0.4090(2) 0.0532(8) Uani 1 1 d . . . H63A H -0.3034 0.7196 0.4068 0.064 Uiso 1 1 calc R . . C64 C -0.1357(3) 0.5845(3) 0.38385(19) 0.0426(7) Uani 1 1 d . . . C65 C -0.2426(3) 0.5360(3) 0.3544(2) 0.0542(9) Uani 1 1 d . . . H65A H -0.3558 0.5718 0.3522 0.065 Uiso 1 1 calc R . . C66 C -0.1881(4) 0.4432(3) 0.3302(2) 0.0489(8) Uani 1 1 d . . . H66A H -0.2631 0.4145 0.3104 0.059 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 0.0440(16) 0.0512(19) 0.060(2) -0.0022(16) 0.0102(15) -0.0088(14) Cl1 0.0739(6) 0.0665(6) 0.0497(5) -0.0067(4) 0.0083(4) -0.0194(5) Cl2 0.0684(6) 0.0938(8) 0.0699(6) 0.0249(6) -0.0096(5) -0.0395(6) Cl3 0.0802(7) 0.0744(7) 0.0802(7) -0.0079(5) -0.0120(5) -0.0269(5) C10 0.0316(13) 0.0334(13) 0.0396(14) -0.0065(11) 0.0013(11) -0.0089(11) C11 0.0326(13) 0.0385(14) 0.0357(13) -0.0103(11) -0.0006(10) -0.0078(11) C12 0.0375(14) 0.0524(17) 0.0449(16) -0.0098(14) 0.0046(12) -0.0133(13) C13 0.0365(16) 0.081(3) 0.057(2) -0.0187(18) 0.0160(14) -0.0151(16) C14 0.0357(15) 0.078(3) 0.057(2) -0.0257(19) 0.0050(14) 0.0038(15) C15 0.0437(16) 0.0496(18) 0.0539(18) -0.0168(15) -0.0026(14) 0.0026(14) C16 0.0380(14) 0.0431(16) 0.0461(16) -0.0111(13) 0.0039(12) -0.0081(12) C20 0.0304(12) 0.0320(13) 0.0393(14) -0.0061(11) 0.0015(10) -0.0085(10) C21 0.0347(13) 0.0283(12) 0.0349(13) -0.0085(10) 0.0008(10) -0.0033(10) C22 0.0358(14) 0.0400(14) 0.0463(15) -0.0135(12) 0.0032(11) -0.0089(12) C23 0.0383(15) 0.0409(15) 0.0596(19) -0.0133(14) -0.0110(13) -0.0037(12) C24 0.0565(18) 0.0452(17) 0.0448(17) -0.0059(14) -0.0124(14) -0.0074(14) C25 0.0587(19) 0.0523(19) 0.0372(16) -0.0007(14) 0.0017(14) -0.0124(15) C26 0.0344(13) 0.0456(16) 0.0412(15) -0.0066(13) -0.0004(11) -0.0098(12) C31 0.0318(12) 0.0372(14) 0.0353(14) -0.0025(11) 0.0038(10) -0.0077(11) C32 0.0301(13) 0.0358(14) 0.0376(14) -0.0029(11) 0.0059(10) -0.0079(11) C33 0.0363(14) 0.0383(15) 0.0439(15) -0.0063(12) 0.0040(11) -0.0104(11) C34 0.0424(15) 0.0448(16) 0.0448(16) -0.0100(13) 0.0051(12) -0.0127(13) C35 0.0377(14) 0.0562(18) 0.0438(16) -0.0114(14) 0.0070(12) -0.0148(13) C36 0.0324(13) 0.0547(18) 0.0352(14) -0.0058(13) 0.0064(11) -0.0083(12) C37 0.0341(13) 0.0400(15) 0.0323(13) -0.0015(11) 0.0074(10) -0.0074(11) C38 0.0413(15) 0.0403(15) 0.0413(15) 0.0029(12) 0.0042(12) -0.0088(12) C39 0.0520(17) 0.0336(15) 0.060(2) 0.0008(14) 0.0012(15) -0.0144(13) C40 0.0442(15) 0.0382(15) 0.0458(16) -0.0018(13) -0.0006(12) -0.0122(12) C41 0.055(2) 0.072(2) 0.055(2) -0.0134(18) -0.0026(16) -0.0198(17) C42 0.058(2) 0.088(3) 0.057(2) -0.027(2) -0.0059(17) -0.015(2) C43 0.0522(19) 0.086(3) 0.0389(17) -0.0077(17) -0.0038(14) -0.0101(18) C44 0.0389(15) 0.064(2) 0.0383(15) -0.0003(15) 0.0051(12) -0.0064(14) C45 0.0558(19) 0.060(2) 0.0376(16) 0.0092(15) 0.0055(14) -0.0032(16) C46 0.0518(18) 0.0486(18) 0.0528(19) 0.0118(16) 0.0054(15) -0.0087(15) C51 0.0309(13) 0.0348(13) 0.0367(14) -0.0023(11) -0.0003(10) -0.0081(11) C52 0.0265(12) 0.0371(14) 0.0324(13) 0.0008(10) 0.0005(10) -0.0079(10) C53 0.0261(12) 0.0407(15) 0.0409(14) -0.0026(12) 0.0005(10) -0.0079(11) C54 0.0346(13) 0.0377(14) 0.0416(14) -0.0053(11) 0.0014(11) -0.0112(11) C55 0.0371(14) 0.0412(15) 0.0359(14) 0.0012(12) 0.0040(11) -0.0100(12) C56 0.0308(13) 0.0386(14) 0.0324(13) 0.0014(11) 0.0019(10) -0.0037(11) C57 0.0280(12) 0.0378(14) 0.0299(12) 0.0030(11) 0.0015(10) -0.0045(11) C58 0.0291(13) 0.0456(15) 0.0354(13) 0.0007(12) -0.0002(10) -0.0117(11) C59 0.0342(14) 0.0467(16) 0.0418(15) -0.0059(12) -0.0022(11) -0.0170(12) C60 0.0342(13) 0.0400(14) 0.0398(15) -0.0057(12) 0.0008(11) -0.0094(11) C61 0.0479(17) 0.0390(15) 0.0476(17) -0.0069(13) 0.0059(13) -0.0094(13) C62 0.0576(19) 0.0420(16) 0.0470(17) -0.0057(14) 0.0125(14) -0.0040(14) C63 0.0368(15) 0.0528(19) 0.0477(17) 0.0013(14) 0.0067(13) 0.0065(13) C64 0.0314(13) 0.0463(16) 0.0349(14) 0.0025(12) 0.0048(11) -0.0002(12) C65 0.0235(13) 0.077(2) 0.0482(17) 0.0010(17) -0.0017(12) -0.0072(14) C66 0.0299(14) 0.069(2) 0.0425(16) -0.0023(15) -0.0028(12) -0.0166(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 Cl1 1.742(4) . ? C1 Cl3 1.746(4) . ? C1 Cl2 1.761(3) . ? C10 C20 1.340(4) . ? C10 C11 1.494(4) . ? C10 C31 1.509(4) . ? C11 C12 1.388(4) . ? C11 C16 1.396(4) . ? C12 C13 1.403(5) . ? C13 C14 1.369(6) . ? C14 C15 1.392(6) . ? C15 C16 1.390(5) . ? C20 C51 1.498(4) . ? C20 C21 1.507(4) . ? C21 C22 1.386(4) . ? C21 C26 1.391(4) . ? C22 C23 1.394(5) . ? C23 C24 1.382(5) . ? C24 C25 1.377(5) . ? C25 C26 1.384(4) . ? C31 C40 1.399(4) . ? C31 C32 1.403(4) . ? C32 C37 1.426(4) . ? C32 C33 1.445(4) . ? C33 C34 1.354(4) . ? C34 C35 1.437(5) . ? C35 C41 1.396(5) . ? C35 C36 1.406(5) . ? C36 C37 1.424(5) . ? C36 C44 1.429(4) . ? C37 C38 1.435(4) . ? C38 C39 1.378(5) . ? C38 C46 1.440(4) . ? C39 C40 1.385(4) . ? C41 C42 1.382(6) . ? C42 C43 1.379(7) . ? C43 C44 1.398(6) . ? C44 C45 1.419(6) . ? C45 C46 1.341(6) . ? C51 C60 1.402(4) . ? C51 C52 1.405(4) . ? C52 C57 1.427(4) . ? C52 C53 1.449(4) . ? C53 C54 1.345(4) . ? C54 C55 1.436(4) . ? C55 C61 1.388(5) . ? C55 C56 1.426(4) . ? C56 C57 1.417(4) . ? C56 C64 1.430(4) . ? C57 C58 1.419(4) . ? C58 C59 1.401(5) . ? C58 C66 1.453(4) . ? C59 C60 1.388(4) . ? C61 C62 1.381(5) . ? C62 C63 1.398(6) . ? C63 C64 1.386(5) . ? C64 C65 1.435(5) . ? C65 C66 1.317(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 Cl1 C1 Cl3 111.8(2) . . ? Cl1 C1 Cl2 110.18(19) . . ? Cl3 C1 Cl2 110.2(2) . . ? C20 C10 C11 126.6(2) . . ? C20 C10 C31 118.9(2) . . ? C11 C10 C31 114.4(2) . . ? C12 C11 C16 118.4(3) . . ? C12 C11 C10 119.7(3) . . ? C16 C11 C10 121.8(3) . . ? C11 C12 C13 120.7(3) . . ? C14 C13 C12 120.6(3) . . ? C13 C14 C15 119.1(3) . . ? C16 C15 C14 120.7(3) . . ? C15 C16 C11 120.4(3) . . ? C10 C20 C51 117.7(2) . . ? C10 C20 C21 126.5(2) . . ? C51 C20 C21 115.7(2) . . ? C22 C21 C26 118.7(3) . . ? C22 C21 C20 121.7(2) . . ? C26 C21 C20 119.5(2) . . ? C21 C22 C23 120.1(3) . . ? C24 C23 C22 121.0(3) . . ? C25 C24 C23 118.7(3) . . ? C24 C25 C26 120.9(3) . . ? C25 C26 C21 120.6(3) . . ? C40 C31 C32 119.3(3) . . ? C40 C31 C10 117.6(3) . . ? C32 C31 C10 123.1(3) . . ? C31 C32 C37 119.8(3) . . ? C31 C32 C33 122.7(3) . . ? C37 C32 C33 117.5(3) . . ? C34 C33 C32 121.5(3) . . ? C33 C34 C35 121.4(3) . . ? C41 C35 C36 118.8(3) . . ? C41 C35 C34 122.3(3) . . ? C36 C35 C34 118.9(3) . . ? C35 C36 C37 120.0(3) . . ? C35 C36 C44 120.6(3) . . ? C37 C36 C44 119.4(3) . . ? C36 C37 C32 120.7(3) . . ? C36 C37 C38 119.9(3) . . ? C32 C37 C38 119.3(3) . . ? C39 C38 C37 119.1(3) . . ? C39 C38 C46 122.9(3) . . ? C37 C38 C46 118.0(3) . . ? C38 C39 C40 121.2(3) . . ? C39 C40 C31 121.3(3) . . ? C42 C41 C35 120.9(4) . . ? C43 C42 C41 120.5(4) . . ? C42 C43 C44 121.3(3) . . ? C43 C44 C45 122.7(3) . . ? C43 C44 C36 117.9(4) . . ? C45 C44 C36 119.4(3) . . ? C46 C45 C44 121.5(3) . . ? C45 C46 C38 121.8(4) . . ? C60 C51 C52 119.0(2) . . ? C60 C51 C20 118.0(3) . . ? C52 C51 C20 123.0(2) . . ? C51 C52 C57 119.9(2) . . ? C51 C52 C53 122.7(2) . . ? C57 C52 C53 117.4(3) . . ? C54 C53 C52 121.9(2) . . ? C53 C54 C55 121.7(3) . . ? C61 C55 C56 119.2(3) . . ? C61 C55 C54 122.7(3) . . ? C56 C55 C54 118.1(3) . . ? C57 C56 C55 120.3(2) . . ? C57 C56 C64 120.7(3) . . ? C55 C56 C64 118.9(3) . . ? C56 C57 C58 119.3(2) . . ? C56 C57 C52 120.6(3) . . ? C58 C57 C52 120.0(3) . . ? C59 C58 C57 118.8(2) . . ? C59 C58 C66 122.8(3) . . ? C57 C58 C66 118.3(3) . . ? C60 C59 C58 120.7(3) . . ? C59 C60 C51 121.6(3) . . ? C62 C61 C55 121.7(3) . . ? C61 C62 C63 119.6(3) . . ? C64 C63 C62 121.1(3) . . ? C63 C64 C56 119.5(3) . . ? C63 C64 C65 122.7(3) . . ? C56 C64 C65 117.9(3) . . ? C66 C65 C64 121.8(3) . . ? C65 C66 C58 121.9(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C20 C10 C11 C12 -144.3(3) . . . . ? C31 C10 C11 C12 34.8(4) . . . . ? C20 C10 C11 C16 39.5(4) . . . . ? C31 C10 C11 C16 -141.4(3) . . . . ? C16 C11 C12 C13 -0.8(4) . . . . ? C10 C11 C12 C13 -177.1(3) . . . . ? C11 C12 C13 C14 0.3(5) . . . . ? C12 C13 C14 C15 0.1(6) . . . . ? C13 C14 C15 C16 0.0(6) . . . . ? C14 C15 C16 C11 -0.5(5) . . . . ? C12 C11 C16 C15 0.8(4) . . . . ? C10 C11 C16 C15 177.1(3) . . . . ? C11 C10 C20 C51 -166.1(3) . . . . ? C31 C10 C20 C51 14.8(4) . . . . ? C11 C10 C20 C21 13.2(5) . . . . ? C31 C10 C20 C21 -165.9(3) . . . . ? C10 C20 C21 C22 33.2(4) . . . . ? C51 C20 C21 C22 -147.5(3) . . . . ? C10 C20 C21 C26 -149.9(3) . . . . ? C51 C20 C21 C26 29.4(4) . . . . ? C26 C21 C22 C23 1.4(4) . . . . ? C20 C21 C22 C23 178.3(3) . . . . ? C21 C22 C23 C24 -0.4(5) . . . . ? C22 C23 C24 C25 0.3(5) . . . . ? C23 C24 C25 C26 -1.2(5) . . . . ? C24 C25 C26 C21 2.2(5) . . . . ? C22 C21 C26 C25 -2.2(5) . . . . ? C20 C21 C26 C25 -179.2(3) . . . . ? C20 C10 C31 C40 68.3(3) . . . . ? C11 C10 C31 C40 -110.9(3) . . . . ? C20 C10 C31 C32 -112.4(3) . . . . ? C11 C10 C31 C32 68.4(3) . . . . ? C40 C31 C32 C37 -1.3(4) . . . . ? C10 C31 C32 C37 179.4(2) . . . . ? C40 C31 C32 C33 -179.7(3) . . . . ? C10 C31 C32 C33 1.0(4) . . . . ? C31 C32 C33 C34 177.7(3) . . . . ? C37 C32 C33 C34 -0.7(4) . . . . ? C32 C33 C34 C35 -1.0(5) . . . . ? C33 C34 C35 C41 -178.1(3) . . . . ? C33 C34 C35 C36 2.0(4) . . . . ? C41 C35 C36 C37 178.8(3) . . . . ? C34 C35 C36 C37 -1.3(4) . . . . ? C41 C35 C36 C44 0.5(5) . . . . ? C34 C35 C36 C44 -179.6(3) . . . . ? C35 C36 C37 C32 -0.4(4) . . . . ? C44 C36 C37 C32 177.9(3) . . . . ? C35 C36 C37 C38 -178.6(3) . . . . ? C44 C36 C37 C38 -0.3(4) . . . . ? C31 C32 C37 C36 -177.1(2) . . . . ? C33 C32 C37 C36 1.4(4) . . . . ? C31 C32 C37 C38 1.1(4) . . . . ? C33 C32 C37 C38 179.6(2) . . . . ? C36 C37 C38 C39 178.7(3) . . . . ? C32 C37 C38 C39 0.5(4) . . . . ? C36 C37 C38 C46 -0.7(4) . . . . ? C32 C37 C38 C46 -178.9(3) . . . . ? C37 C38 C39 C40 -1.9(5) . . . . ? C46 C38 C39 C40 177.4(3) . . . . ? C38 C39 C40 C31 1.7(5) . . . . ? C32 C31 C40 C39 -0.1(4) . . . . ? C10 C31 C40 C39 179.2(3) . . . . ? C36 C35 C41 C42 -0.2(5) . . . . ? C34 C35 C41 C42 179.9(4) . . . . ? C35 C41 C42 C43 -0.6(6) . . . . ? C41 C42 C43 C44 1.1(6) . . . . ? C42 C43 C44 C45 179.9(3) . . . . ? C42 C43 C44 C36 -0.7(5) . . . . ? C35 C36 C44 C43 -0.1(5) . . . . ? C37 C36 C44 C43 -178.4(3) . . . . ? C35 C36 C44 C45 179.3(3) . . . . ? C37 C36 C44 C45 1.0(4) . . . . ? C43 C44 C45 C46 178.6(3) . . . . ? C36 C44 C45 C46 -0.8(5) . . . . ? C44 C45 C46 C38 -0.2(5) . . . . ? C39 C38 C46 C45 -178.4(3) . . . . ? C37 C38 C46 C45 0.9(5) . . . . ? C10 C20 C51 C60 67.9(3) . . . . ? C21 C20 C51 C60 -111.5(3) . . . . ? C10 C20 C51 C52 -112.0(3) . . . . ? C21 C20 C51 C52 68.6(3) . . . . ? C60 C51 C52 C57 -2.8(4) . . . . ? C20 C51 C52 C57 177.1(2) . . . . ? C60 C51 C52 C53 179.8(3) . . . . ? C20 C51 C52 C53 -0.4(4) . . . . ? C51 C52 C53 C54 177.1(3) . . . . ? C57 C52 C53 C54 -0.4(4) . . . . ? C52 C53 C54 C55 -0.4(4) . . . . ? C53 C54 C55 C61 -178.9(3) . . . . ? C53 C54 C55 C56 0.8(4) . . . . ? C61 C55 C56 C57 179.4(3) . . . . ? C54 C55 C56 C57 -0.3(4) . . . . ? C61 C55 C56 C64 -0.7(4) . . . . ? C54 C55 C56 C64 179.6(2) . . . . ? C55 C56 C57 C58 -179.9(2) . . . . ? C64 C56 C57 C58 0.2(4) . . . . ? C55 C56 C57 C52 -0.5(4) . . . . ? C64 C56 C57 C52 179.6(2) . . . . ? C51 C52 C57 C56 -176.7(2) . . . . ? C53 C52 C57 C56 0.9(4) . . . . ? C51 C52 C57 C58 2.7(4) . . . . ? C53 C52 C57 C58 -179.7(2) . . . . ? C56 C57 C58 C59 178.0(2) . . . . ? C52 C57 C58 C59 -1.4(4) . . . . ? C56 C57 C58 C66 -0.2(4) . . . . ? C52 C57 C58 C66 -179.7(2) . . . . ? C57 C58 C59 C60 0.2(4) . . . . ? C66 C58 C59 C60 178.4(3) . . . . ? C58 C59 C60 C51 -0.4(4) . . . . ? C52 C51 C60 C59 1.6(4) . . . . ? C20 C51 C60 C59 -178.3(2) . . . . ? C56 C55 C61 C62 1.2(4) . . . . ? C54 C55 C61 C62 -179.1(3) . . . . ? C55 C61 C62 C63 -1.0(5) . . . . ? C61 C62 C63 C64 0.3(5) . . . . ? C62 C63 C64 C56 0.2(5) . . . . ? C62 C63 C64 C65 179.8(3) . . . . ? C57 C56 C64 C63 179.9(3) . . . . ? C55 C56 C64 C63 0.0(4) . . . . ? C57 C56 C64 C65 0.3(4) . . . . ? C55 C56 C64 C65 -179.6(3) . . . . ? C63 C64 C65 C66 179.6(3) . . . . ? C56 C64 C65 C66 -0.9(5) . . . . ? C64 C65 C66 C58 0.8(5) . . . . ? C59 C58 C66 C65 -178.4(3) . . . . ? C57 C58 C66 C65 -0.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.899 _diffrn_reflns_theta_full 66.50 _diffrn_measured_fraction_theta_full 0.900 _refine_diff_density_max 0.515 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.077