Supplementary Material (ESI) for Chemical Communications This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name 'Francois Diederich' 'Corinne Boudon' 'Jean-Paul Gisselbrecht' 'Maurice Gross' 'Frieder Mitzel' ; P.Seiler ; _publ_contact_author_name 'Prof Francois Diederich' _publ_contact_author_address ; Department of Chemistry ETH Zurich ETH Hoenggerberg HCI G313 Zurich CH-8093 SWITZERLAND ; _publ_contact_author_email DIEDERICH@ORG.CHEM.ETHZ.CH _publ_section_title ; Donor-substituted peralkynylated ; data_mitz1 _database_code_CSD 208124 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C70 H40 N2' _chemical_formula_sum 'C70 H40 N2' _chemical_formula_weight 909.04 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' _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 13.6643(5) _cell_length_b 14.0449(6) _cell_length_c 15.9105(8) _cell_angle_alpha 66.12(1) _cell_angle_beta 68.03(1) _cell_angle_gamma 83.06(1) _cell_volume 2587.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 10833 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 27.49 _exptl_crystal_description 'Cut fragment' _exptl_crystal_colour BLACK _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.167 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 948 _exptl_absorpt_coefficient_mu 0.067 _exptl_absorpt_correction_type 'no correction' _exptl_absorpt_correction_T_min 0.9801 _exptl_absorpt_correction_T_max 0.9933 _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kappa CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_reflns_number 19969 _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_sigmaI/netI 0.0822 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 27.49 _reflns_number_total 11698 _reflns_number_gt 7437 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa CCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo + Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al.,1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson,1976)' _computing_publication_material SHELXL97 _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 'w=1/[\s^2^(Fo^2^)+(0.0591P)^2^+0.3731P] 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 'H-atoms riding' _refine_ls_extinction_method SHELXL97 _refine_ls_extinction_coef 0.019(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11698 _refine_ls_number_parameters 690 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1080 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1509 _refine_ls_wR_factor_gt 0.1295 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.34890(14) 0.42497(13) 0.52040(13) 0.0371(4) Uani 1 d . . . C2 C 0.34116(14) 0.31502(14) 0.57506(13) 0.0389(4) Uani 1 d . . . C3 C 0.33670(14) 0.22210(14) 0.61991(13) 0.0377(4) Uani 1 d . . . C4 C 0.34195(13) 0.11710(13) 0.66660(13) 0.0354(4) Uani 1 d . . . C5 C 0.35307(13) 0.02459(13) 0.70437(13) 0.0346(4) Uani 1 d . . . C6 C 0.39584(13) -0.07635(12) 0.72670(12) 0.0319(4) Uani 1 d . . . C7 C 0.49650(14) -0.07635(13) 0.65465(13) 0.0356(4) Uani 1 d . . . C8 C 0.57766(14) -0.05223(13) 0.58415(13) 0.0368(4) Uani 1 d . . . C9 C 0.66388(13) -0.00637(14) 0.50295(13) 0.0370(4) Uani 1 d . . . C10 C 0.73337(13) 0.04835(13) 0.43070(13) 0.0355(4) Uani 1 d . . . C11 C 0.79630(13) 0.13540(13) 0.35064(12) 0.0336(4) Uani 1 d . . . C12 C 0.74348(14) 0.23025(14) 0.34568(13) 0.0361(4) Uani 1 d . . . C13 C 0.67844(14) 0.29281(14) 0.36242(13) 0.0387(4) Uani 1 d . . . C14 C 0.60057(15) 0.35879(14) 0.38551(13) 0.0396(4) Uani 1 d . . . C15 C 0.52679(15) 0.40970(13) 0.41166(13) 0.0390(4) Uani 1 d . . . C16 C 0.43985(14) 0.47074(13) 0.44045(13) 0.0372(4) Uani 1 d . . . C17 C 0.26186(15) 0.48541(14) 0.54935(14) 0.0403(4) Uani 1 d . . . C18 C 0.18938(15) 0.53881(14) 0.57199(14) 0.0403(4) Uani 1 d . . . C19 C 0.10549(14) 0.60586(14) 0.59297(14) 0.0379(4) Uani 1 d . . . C20 C 0.00545(15) 0.56809(15) 0.66299(14) 0.0436(5) Uani 1 d . . . H20A H -0.0067 0.4952 0.7000 0.049(6) Uiso 1 calc R . . C21 C -0.07585(15) 0.63369(15) 0.67973(15) 0.0466(5) Uani 1 d . . . H21A H -0.1429 0.6054 0.7280 0.057(6) Uiso 1 calc R . . C22 C -0.06142(15) 0.74210(15) 0.62652(14) 0.0413(4) Uani 1 d . . . C23 C 0.03938(15) 0.78022(14) 0.55736(14) 0.0403(4) Uani 1 d . . . H23A H 0.0521 0.8532 0.5211 0.051(6) Uiso 1 calc R . . C24 C 0.12003(14) 0.71378(14) 0.54120(14) 0.0388(4) Uani 1 d . . . H24A H 0.1875 0.7419 0.4936 0.050(6) Uiso 1 calc R . . N25 N -0.14268(14) 0.80833(14) 0.64154(14) 0.0568(5) Uani 1 d . . . C26 C -0.2443(2) 0.7682(3) 0.7143(3) 0.1073(13) Uani 1 d . . . H26A H -0.2925 0.8257 0.7150 0.111(10) Uiso 1 calc R . . H26B H -0.2380 0.7325 0.7791 0.161(18) Uiso 1 calc R . . H26C H -0.2719 0.7189 0.6985 0.19(2) Uiso 1 calc R . . C27 C -0.12363(19) 0.91928(17) 0.5960(2) 0.0609(6) Uani 1 d . . . H27A H -0.1902 0.9539 0.6148 0.072(7) Uiso 1 calc R . . H27B H -0.0943 0.9414 0.5243 0.094(10) Uiso 1 calc R . . H27C H -0.0734 0.9383 0.6178 0.095(9) Uiso 1 calc R . . C28 C 0.45017(15) 0.57964(14) 0.38288(14) 0.0402(4) Uani 1 d . . . C29 C 0.46336(15) 0.67072(14) 0.33060(15) 0.0427(4) Uani 1 d . . . C30 C 0.47961(15) 0.77794(13) 0.26432(14) 0.0389(4) Uani 1 d . . . C31 C 0.41132(15) 0.85436(14) 0.28397(15) 0.0433(5) Uani 1 d . . . H31A H 0.3530 0.8359 0.3445 0.050(6) Uiso 1 calc R . . C32 C 0.42663(16) 0.95665(14) 0.21722(15) 0.0442(5) Uani 1 d . . . H32A H 0.3784 1.0071 0.2325 0.051(6) Uiso 1 calc R . . C33 C 0.51206(15) 0.98737(14) 0.12728(14) 0.0397(4) Uani 1 d . . . C34 C 0.58200(15) 0.91026(15) 0.10925(14) 0.0428(4) Uani 1 d . . . H34A H 0.6417 0.9287 0.0498 0.048(6) Uiso 1 calc R . . C35 C 0.56593(15) 0.80872(14) 0.17566(15) 0.0430(5) Uani 1 d . . . H35A H 0.6145 0.7582 0.1611 0.055(6) Uiso 1 calc R . . N36 N 0.52628(14) 1.08829(12) 0.05935(12) 0.0518(4) Uani 1 d . . . C37 C 0.4481(2) 1.16411(16) 0.07449(18) 0.0612(6) Uani 1 d . . . H37A H 0.4712 1.2315 0.0191 0.102(10) Uiso 1 calc R . . H37B H 0.4392 1.1711 0.1357 0.094(9) Uiso 1 calc R . . H37C H 0.3807 1.1413 0.0789 0.086(9) Uiso 1 calc R . . C38 C 0.62049(19) 1.12155(17) -0.02816(16) 0.0579(6) Uani 1 d . . . H38A H 0.6168 1.1956 -0.0676 0.091(9) Uiso 1 calc R . . H38B H 0.6258 1.0807 -0.0670 0.086(9) Uiso 1 calc R . . H38C H 0.6827 1.1109 -0.0092 0.098(10) Uiso 1 calc R . . C39 C 0.89568(13) 0.12653(13) 0.28874(12) 0.0332(4) Uani 1 d . . . C40 C 0.95993(13) 0.21480(14) 0.21253(13) 0.0361(4) Uani 1 d . . . C41 C 1.01968(14) 0.28458(14) 0.14789(13) 0.0393(4) Uani 1 d . . . C42 C 1.08774(15) 0.36834(15) 0.06674(14) 0.0423(4) Uani 1 d . . . C43 C 1.07742(17) 0.46881(15) 0.06357(16) 0.0485(5) Uani 1 d . . . H43A H 1.0280 0.4826 0.1176 0.051(6) Uiso 1 calc R . . C44 C 1.14001(19) 0.54960(17) -0.01939(19) 0.0617(7) Uani 1 d . . . H44A H 1.1326 0.6188 -0.0220 0.074(8) Uiso 1 calc R . . C45 C 1.2120(2) 0.5304(2) -0.0971(2) 0.0786(9) Uani 1 d . . . H45A H 1.2551 0.5858 -0.1530 0.089(8) Uiso 1 calc R . . C46 C 1.2218(2) 0.4316(3) -0.0942(2) 0.0906(10) Uani 1 d . . . H46A H 1.2709 0.4187 -0.1490 0.115(11) Uiso 1 calc R . . C47 C 1.1613(2) 0.3500(2) -0.01273(18) 0.0708(7) Uani 1 d . . . H47A H 1.1699 0.2812 -0.0110 0.092(9) Uiso 1 calc R . . C48 C 0.93805(13) 0.02606(14) 0.30059(13) 0.0357(4) Uani 1 d . . . C49 C 0.97549(14) -0.05785(14) 0.31020(13) 0.0387(4) Uani 1 d . . . C50 C 1.02095(15) -0.15796(14) 0.32326(14) 0.0389(4) Uani 1 d . . . C51 C 0.95851(16) -0.24898(15) 0.38441(15) 0.0460(5) Uani 1 d . . . H51A H 0.8849 -0.2451 0.4168 0.056(6) Uiso 1 calc R . . C52 C 1.00409(19) -0.34505(16) 0.39788(17) 0.0527(5) Uani 1 d . . . H52A H 0.9614 -0.4070 0.4391 0.080(8) Uiso 1 calc R . . C53 C 1.11057(19) -0.35133(17) 0.35202(17) 0.0568(6) Uani 1 d . . . H53A H 1.1413 -0.4175 0.3619 0.070(7) Uiso 1 calc R . . C54 C 1.17299(18) -0.26175(17) 0.29167(18) 0.0571(6) Uani 1 d . . . H54A H 1.2467 -0.2664 0.2603 0.062(7) Uiso 1 calc R . . C55 C 1.12890(16) -0.16563(16) 0.27674(16) 0.0486(5) Uani 1 d . . . H55A H 1.1722 -0.1042 0.2345 0.054(6) Uiso 1 calc R . . C56 C 0.34991(13) -0.16442(12) 0.80889(12) 0.0322(4) Uani 1 d . . . C57 C 0.40726(13) -0.25787(13) 0.82491(13) 0.0353(4) Uani 1 d . . . C58 C 0.46181(14) -0.33229(14) 0.83532(13) 0.0390(4) Uani 1 d . . . C59 C 0.53183(14) -0.41780(13) 0.84693(13) 0.0377(4) Uani 1 d . . . C60 C 0.59413(16) -0.43249(16) 0.90272(16) 0.0486(5) Uani 1 d . . . H60A H 0.5886 -0.3873 0.9353 0.075(8) Uiso 1 calc R . . C61 C 0.66397(16) -0.51226(16) 0.91108(16) 0.0511(5) Uani 1 d . . . H61A H 0.7064 -0.5213 0.9492 0.097(9) Uiso 1 calc R . . C62 C 0.67287(18) -0.57802(17) 0.86565(18) 0.0579(6) Uani 1 d . . . H62A H 0.7234 -0.6309 0.8694 0.068(7) Uiso 1 calc R . . C63 C 0.6081(2) -0.5677(2) 0.8141(2) 0.0823(8) Uani 1 d . . . H63A H 0.6117 -0.6156 0.7848 0.115(11) Uiso 1 calc R . . C64 C 0.5381(2) -0.48791(19) 0.80457(19) 0.0643(6) Uani 1 d . . . H64A H 0.4938 -0.4812 0.7686 0.090(9) Uiso 1 calc R . . C65 C 0.24760(14) -0.16386(13) 0.87819(13) 0.0358(4) Uani 1 d . . . C66 C 0.16064(14) -0.16668(14) 0.93620(14) 0.0394(4) Uani 1 d . . . C67 C 0.05477(14) -0.16817(16) 1.00321(14) 0.0433(5) Uani 1 d . . . C68 C -0.01612(16) -0.09666(17) 0.97014(18) 0.0523(5) Uani 1 d . . . H68A H 0.0052 -0.0480 0.9037 0.067(7) Uiso 1 calc R . . C69 C -0.11785(18) -0.0971(2) 1.0347(2) 0.0715(7) Uani 1 d . . . H69A H -0.1663 -0.0481 1.0126 0.099(10) Uiso 1 calc R . . C70 C -0.14922(19) -0.1683(3) 1.1311(2) 0.0827(9) Uani 1 d . . . H70A H -0.2191 -0.1681 1.1751 0.095(9) Uiso 1 calc R . . C71 C -0.0801(2) -0.2395(3) 1.16359(19) 0.0879(10) Uani 1 d . . . H71A H -0.1025 -0.2890 1.2298 0.091(9) Uiso 1 calc R . . C72 C 0.02243(18) -0.2397(2) 1.10031(16) 0.0675(7) Uani 1 d . . . H72A H 0.0704 -0.2886 1.1232 0.082(9) 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 0.0407(10) 0.0294(9) 0.0416(10) -0.0144(8) -0.0167(8) 0.0083(7) C2 0.0376(9) 0.0354(10) 0.0411(10) -0.0163(8) -0.0117(8) 0.0076(8) C3 0.0359(9) 0.0341(9) 0.0397(10) -0.0150(8) -0.0113(8) 0.0071(7) C4 0.0327(9) 0.0356(9) 0.0350(9) -0.0152(8) -0.0080(7) 0.0032(7) C5 0.0323(9) 0.0339(9) 0.0336(9) -0.0128(7) -0.0074(7) -0.0007(7) C6 0.0292(8) 0.0285(8) 0.0347(9) -0.0119(7) -0.0088(7) 0.0016(7) C7 0.0352(9) 0.0286(8) 0.0364(9) -0.0099(7) -0.0090(8) 0.0013(7) C8 0.0341(9) 0.0328(9) 0.0366(9) -0.0107(8) -0.0088(8) 0.0026(7) C9 0.0313(9) 0.0397(9) 0.0356(9) -0.0145(8) -0.0086(8) 0.0044(8) C10 0.0317(9) 0.0374(9) 0.0342(9) -0.0144(8) -0.0087(7) 0.0040(7) C11 0.0310(8) 0.0357(9) 0.0312(9) -0.0125(7) -0.0090(7) 0.0016(7) C12 0.0326(9) 0.0384(9) 0.0323(9) -0.0119(8) -0.0081(7) 0.0004(8) C13 0.0379(10) 0.0385(10) 0.0353(9) -0.0127(8) -0.0108(8) 0.0029(8) C14 0.0409(10) 0.0354(9) 0.0371(10) -0.0121(8) -0.0117(8) 0.0045(8) C15 0.0445(10) 0.0328(9) 0.0379(10) -0.0118(8) -0.0159(8) 0.0051(8) C16 0.0427(10) 0.0302(9) 0.0401(10) -0.0146(8) -0.0174(8) 0.0081(8) C17 0.0419(10) 0.0320(9) 0.0441(10) -0.0145(8) -0.0137(8) 0.0041(8) C18 0.0421(10) 0.0363(9) 0.0423(10) -0.0163(8) -0.0147(8) 0.0046(8) C19 0.0363(9) 0.0359(9) 0.0442(10) -0.0198(8) -0.0147(8) 0.0079(8) C20 0.0458(11) 0.0352(10) 0.0438(11) -0.0145(8) -0.0110(9) 0.0031(8) C21 0.0381(10) 0.0460(11) 0.0444(11) -0.0149(9) -0.0058(9) 0.0017(9) C22 0.0380(10) 0.0443(10) 0.0417(10) -0.0207(9) -0.0128(8) 0.0108(8) C23 0.0427(10) 0.0343(9) 0.0445(10) -0.0157(8) -0.0174(8) 0.0055(8) C24 0.0340(9) 0.0370(9) 0.0440(10) -0.0169(8) -0.0113(8) 0.0012(8) N25 0.0443(9) 0.0513(10) 0.0606(11) -0.0208(9) -0.0094(8) 0.0162(8) C26 0.0529(15) 0.080(2) 0.117(3) -0.012(2) 0.0109(16) 0.0247(15) C27 0.0585(14) 0.0525(13) 0.0825(18) -0.0342(12) -0.0346(13) 0.0229(11) C28 0.0410(10) 0.0359(10) 0.0444(10) -0.0176(8) -0.0159(8) 0.0074(8) C29 0.0479(11) 0.0360(10) 0.0466(11) -0.0159(9) -0.0202(9) 0.0034(8) C30 0.0414(10) 0.0328(9) 0.0444(10) -0.0143(8) -0.0184(8) 0.0021(8) C31 0.0460(11) 0.0349(9) 0.0428(11) -0.0140(8) -0.0101(9) 0.0000(8) C32 0.0486(11) 0.0341(9) 0.0497(11) -0.0196(8) -0.0164(9) 0.0097(8) C33 0.0459(10) 0.0339(9) 0.0411(10) -0.0129(8) -0.0185(9) -0.0018(8) C34 0.0387(10) 0.0436(10) 0.0426(11) -0.0154(9) -0.0121(9) 0.0001(8) C35 0.0432(10) 0.0344(9) 0.0507(11) -0.0165(9) -0.0172(9) 0.0049(8) N36 0.0647(11) 0.0354(8) 0.0459(10) -0.0098(7) -0.0170(9) 0.0035(8) C37 0.0888(18) 0.0325(10) 0.0612(15) -0.0163(10) -0.0298(13) 0.0087(11) C38 0.0651(14) 0.0480(12) 0.0506(13) -0.0053(11) -0.0201(11) -0.0156(11) C39 0.0309(9) 0.0344(9) 0.0317(9) -0.0122(7) -0.0086(7) -0.0003(7) C40 0.0318(9) 0.0375(9) 0.0371(9) -0.0169(8) -0.0085(8) 0.0036(8) C41 0.0353(9) 0.0399(10) 0.0387(10) -0.0144(8) -0.0095(8) -0.0007(8) C42 0.0394(10) 0.0411(10) 0.0394(10) -0.0075(8) -0.0126(8) -0.0092(8) C43 0.0483(11) 0.0426(11) 0.0561(12) -0.0122(10) -0.0263(10) -0.0043(9) C44 0.0686(15) 0.0410(12) 0.0731(16) 0.0031(11) -0.0451(13) -0.0170(11) C45 0.0811(18) 0.0798(19) 0.0522(15) 0.0094(14) -0.0241(14) -0.0441(15) C46 0.0856(19) 0.094(2) 0.0572(16) -0.0222(15) 0.0155(15) -0.0394(17) C47 0.0682(15) 0.0636(15) 0.0562(14) -0.0229(12) 0.0096(12) -0.0201(12) C48 0.0294(8) 0.0372(10) 0.0340(9) -0.0132(8) -0.0048(7) 0.0003(7) C49 0.0361(9) 0.0396(10) 0.0372(10) -0.0160(8) -0.0091(8) 0.0028(8) C50 0.0416(10) 0.0379(10) 0.0404(10) -0.0183(8) -0.0164(8) 0.0071(8) C51 0.0449(11) 0.0445(11) 0.0504(11) -0.0198(9) -0.0175(9) 0.0009(9) C52 0.0661(14) 0.0372(11) 0.0593(13) -0.0173(10) -0.0281(11) -0.0004(10) C53 0.0708(15) 0.0431(12) 0.0691(15) -0.0294(11) -0.0350(13) 0.0184(11) C54 0.0503(12) 0.0546(13) 0.0693(15) -0.0333(11) -0.0187(11) 0.0157(10) C55 0.0439(11) 0.0425(11) 0.0519(12) -0.0195(9) -0.0088(9) 0.0036(9) C56 0.0300(8) 0.0284(8) 0.0337(9) -0.0107(7) -0.0077(7) -0.0003(7) C57 0.0324(9) 0.0296(9) 0.0353(9) -0.0092(7) -0.0054(7) -0.0034(7) C58 0.0380(10) 0.0334(9) 0.0376(10) -0.0097(8) -0.0091(8) -0.0007(8) C59 0.0364(9) 0.0313(9) 0.0383(10) -0.0091(8) -0.0111(8) 0.0024(7) C60 0.0458(11) 0.0458(11) 0.0594(13) -0.0230(10) -0.0228(10) 0.0053(9) C61 0.0437(11) 0.0533(12) 0.0544(12) -0.0147(10) -0.0240(10) 0.0064(9) C62 0.0563(13) 0.0481(12) 0.0756(16) -0.0256(11) -0.0348(12) 0.0218(10) C63 0.101(2) 0.0791(17) 0.118(2) -0.0685(17) -0.0746(19) 0.0536(16) C64 0.0801(16) 0.0680(15) 0.0744(16) -0.0438(13) -0.0511(14) 0.0353(13) C65 0.0358(9) 0.0280(8) 0.0368(9) -0.0089(7) -0.0091(8) -0.0014(7) C66 0.0351(9) 0.0385(10) 0.0404(10) -0.0153(8) -0.0085(8) -0.0011(8) C67 0.0337(9) 0.0551(11) 0.0422(10) -0.0270(9) -0.0047(8) -0.0032(9) C68 0.0406(11) 0.0555(12) 0.0635(14) -0.0330(11) -0.0113(10) 0.0034(9) C69 0.0391(12) 0.0922(18) 0.104(2) -0.0690(17) -0.0161(13) 0.0087(13) C70 0.0360(12) 0.151(3) 0.0791(19) -0.082(2) 0.0041(13) -0.0094(15) C71 0.0473(14) 0.167(3) 0.0422(13) -0.0429(17) 0.0015(11) -0.0208(17) C72 0.0434(12) 0.107(2) 0.0409(12) -0.0212(13) -0.0083(10) -0.0070(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 C16 1.387(3) . ? C1 C17 1.418(3) . ? C1 C2 1.427(2) . ? C2 C3 1.204(2) . ? C3 C4 1.364(2) . ? C4 C5 1.209(2) . ? C5 C6 1.423(2) . ? C6 C56 1.378(2) . ? C6 C7 1.423(2) . ? C7 C8 1.206(2) . ? C8 C9 1.358(2) . ? C9 C10 1.207(2) . ? C10 C11 1.425(2) . ? C11 C39 1.374(2) . ? C11 C12 1.424(2) . ? C12 C13 1.207(2) . ? C13 C14 1.368(3) . ? C14 C15 1.206(3) . ? C15 C16 1.421(3) . ? C16 C28 1.421(2) . ? C17 C18 1.202(3) . ? C18 C19 1.421(3) . ? C19 C20 1.396(3) . ? C19 C24 1.398(2) . ? C20 C21 1.373(3) . ? C21 C22 1.406(3) . ? C22 N25 1.374(2) . ? C22 C23 1.401(3) . ? C23 C24 1.373(3) . ? N25 C26 1.429(3) . ? N25 C27 1.437(3) . ? C28 C29 1.201(2) . ? C29 C30 1.431(3) . ? C30 C31 1.390(3) . ? C30 C35 1.397(3) . ? C31 C32 1.381(3) . ? C32 C33 1.403(3) . ? C33 N36 1.373(2) . ? C33 C34 1.402(3) . ? C34 C35 1.371(3) . ? N36 C37 1.440(3) . ? N36 C38 1.446(3) . ? C39 C48 1.425(2) . ? C39 C40 1.424(2) . ? C40 C41 1.197(2) . ? C41 C42 1.433(2) . ? C42 C43 1.383(3) . ? C42 C47 1.387(3) . ? C43 C44 1.392(3) . ? C44 C45 1.365(4) . ? C45 C46 1.361(4) . ? C46 C47 1.379(3) . ? C48 C49 1.200(2) . ? C49 C50 1.433(3) . ? C50 C55 1.394(3) . ? C50 C51 1.394(3) . ? C51 C52 1.385(3) . ? C52 C53 1.373(3) . ? C53 C54 1.379(3) . ? C54 C55 1.376(3) . ? C56 C65 1.422(2) . ? C56 C57 1.426(2) . ? C57 C58 1.200(2) . ? C58 C59 1.438(3) . ? C59 C64 1.380(3) . ? C59 C60 1.389(3) . ? C60 C61 1.378(3) . ? C61 C62 1.356(3) . ? C62 C63 1.376(3) . ? C63 C64 1.381(3) . ? C65 C66 1.194(2) . ? C66 C67 1.437(3) . ? C67 C72 1.390(3) . ? C67 C68 1.394(3) . ? C68 C69 1.385(3) . ? C69 C70 1.381(4) . ? C70 C71 1.371(4) . ? C71 C72 1.386(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 C1 C17 121.25(15) . . ? C16 C1 C2 120.17(16) . . ? C17 C1 C2 118.58(16) . . ? C3 C2 C1 178.64(19) . . ? C2 C3 C4 174.50(19) . . ? C5 C4 C3 175.98(19) . . ? C4 C5 C6 163.18(18) . . ? C56 C6 C5 125.76(15) . . ? C56 C6 C7 122.44(15) . . ? C5 C6 C7 111.76(14) . . ? C8 C7 C6 164.86(18) . . ? C7 C8 C9 169.17(19) . . ? C10 C9 C8 170.12(19) . . ? C9 C10 C11 163.88(19) . . ? C39 C11 C12 125.66(15) . . ? C39 C11 C10 123.14(16) . . ? C12 C11 C10 111.18(15) . . ? C13 C12 C11 162.78(17) . . ? C12 C13 C14 176.55(18) . . ? C15 C14 C13 174.56(19) . . ? C14 C15 C16 178.8(2) . . ? C1 C16 C28 122.02(16) . . ? C1 C16 C15 120.99(15) . . ? C28 C16 C15 116.98(16) . . ? C18 C17 C1 178.39(19) . . ? C17 C18 C19 176.7(2) . . ? C20 C19 C24 117.19(16) . . ? C20 C19 C18 122.36(16) . . ? C24 C19 C18 120.43(16) . . ? C21 C20 C19 121.63(17) . . ? C20 C21 C22 121.05(17) . . ? N25 C22 C23 121.09(17) . . ? N25 C22 C21 121.55(17) . . ? C23 C22 C21 117.36(17) . . ? C24 C23 C22 121.02(17) . . ? C23 C24 C19 121.73(17) . . ? C22 N25 C26 120.25(19) . . ? C22 N25 C27 120.77(17) . . ? C26 N25 C27 118.3(2) . . ? C29 C28 C16 176.6(2) . . ? C28 C29 C30 177.2(2) . . ? C31 C30 C35 117.65(16) . . ? C31 C30 C29 122.36(17) . . ? C35 C30 C29 119.98(17) . . ? C32 C31 C30 121.24(18) . . ? C31 C32 C33 121.21(18) . . ? N36 C33 C32 121.60(17) . . ? N36 C33 C34 121.29(17) . . ? C32 C33 C34 117.11(16) . . ? C35 C34 C33 121.32(18) . . ? C34 C35 C30 121.43(18) . . ? C33 N36 C37 120.57(18) . . ? C33 N36 C38 121.03(17) . . ? C37 N36 C38 118.39(17) . . ? C11 C39 C48 119.76(15) . . ? C11 C39 C40 122.45(16) . . ? C48 C39 C40 117.79(15) . . ? C41 C40 C39 175.50(19) . . ? C40 C41 C42 176.5(2) . . ? C43 C42 C47 119.14(19) . . ? C43 C42 C41 121.03(19) . . ? C47 C42 C41 119.72(19) . . ? C42 C43 C44 119.5(2) . . ? C45 C44 C43 120.6(2) . . ? C46 C45 C44 119.9(2) . . ? C45 C46 C47 120.7(3) . . ? C46 C47 C42 120.1(3) . . ? C49 C48 C39 178.83(19) . . ? C48 C49 C50 178.8(2) . . ? C55 C50 C51 119.04(17) . . ? C55 C50 C49 120.35(17) . . ? C51 C50 C49 120.59(17) . . ? C52 C51 C50 119.85(19) . . ? C53 C52 C51 120.4(2) . . ? C52 C53 C54 120.1(2) . . ? C55 C54 C53 120.2(2) . . ? C54 C55 C50 120.32(19) . . ? C6 C56 C65 121.63(15) . . ? C6 C56 C57 118.88(15) . . ? C65 C56 C57 119.49(14) . . ? C58 C57 C56 175.46(18) . . ? C57 C58 C59 176.80(19) . . ? C64 C59 C60 118.33(18) . . ? C64 C59 C58 121.34(18) . . ? C60 C59 C58 120.32(18) . . ? C61 C60 C59 120.4(2) . . ? C62 C61 C60 120.8(2) . . ? C61 C62 C63 119.5(2) . . ? C62 C63 C64 120.4(2) . . ? C63 C64 C59 120.5(2) . . ? C66 C65 C56 177.53(19) . . ? C65 C66 C67 178.0(2) . . ? C72 C67 C68 119.74(19) . . ? C72 C67 C66 120.9(2) . . ? C68 C67 C66 119.37(18) . . ? C69 C68 C67 119.6(2) . . ? C70 C69 C68 120.3(3) . . ? C71 C70 C69 120.3(2) . . ? C70 C71 C72 120.3(3) . . ? C71 C72 C67 119.8(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 C16 C1 C2 C3 0(9) . . . . ? C17 C1 C2 C3 -180(100) . . . . ? C1 C2 C3 C4 17(10) . . . . ? C2 C3 C4 C5 -9(5) . . . . ? C3 C4 C5 C6 -6(3) . . . . ? C4 C5 C6 C56 171.4(6) . . . . ? C4 C5 C6 C7 -6.4(7) . . . . ? C56 C6 C7 C8 -177.2(7) . . . . ? C5 C6 C7 C8 0.7(8) . . . . ? C6 C7 C8 C9 13.0(17) . . . . ? C7 C8 C9 C10 -5(2) . . . . ? C8 C9 C10 C11 -0.5(18) . . . . ? C9 C10 C11 C39 174.8(6) . . . . ? C9 C10 C11 C12 -4.1(8) . . . . ? C39 C11 C12 C13 -179.8(6) . . . . ? C10 C11 C12 C13 -1.1(7) . . . . ? C11 C12 C13 C14 -7(4) . . . . ? C12 C13 C14 C15 2(5) . . . . ? C13 C14 C15 C16 -124(9) . . . . ? C17 C1 C16 C28 -0.8(3) . . . . ? C2 C1 C16 C28 178.81(18) . . . . ? C17 C1 C16 C15 -179.87(18) . . . . ? C2 C1 C16 C15 -0.2(3) . . . . ? C14 C15 C16 C1 130(9) . . . . ? C14 C15 C16 C28 -49(9) . . . . ? C16 C1 C17 C18 1(8) . . . . ? C2 C1 C17 C18 -178(100) . . . . ? C1 C17 C18 C19 29(10) . . . . ? C17 C18 C19 C20 142(4) . . . . ? C17 C18 C19 C24 -36(4) . . . . ? C24 C19 C20 C21 0.8(3) . . . . ? C18 C19 C20 C21 -177.5(2) . . . . ? C19 C20 C21 C22 0.1(3) . . . . ? C20 C21 C22 N25 178.9(2) . . . . ? C20 C21 C22 C23 -1.1(3) . . . . ? N25 C22 C23 C24 -178.84(19) . . . . ? C21 C22 C23 C24 1.2(3) . . . . ? C22 C23 C24 C19 -0.3(3) . . . . ? C20 C19 C24 C23 -0.7(3) . . . . ? C18 C19 C24 C23 177.61(18) . . . . ? C23 C22 N25 C26 -178.4(3) . . . . ? C21 C22 N25 C26 1.6(4) . . . . ? C23 C22 N25 C27 -7.9(3) . . . . ? C21 C22 N25 C27 172.0(2) . . . . ? C1 C16 C28 C29 -166(3) . . . . ? C15 C16 C28 C29 13(4) . . . . ? C16 C28 C29 C30 48(7) . . . . ? C28 C29 C30 C31 129(4) . . . . ? C28 C29 C30 C35 -51(4) . . . . ? C35 C30 C31 C32 1.6(3) . . . . ? C29 C30 C31 C32 -177.64(19) . . . . ? C30 C31 C32 C33 -0.4(3) . . . . ? C31 C32 C33 N36 178.21(19) . . . . ? C31 C32 C33 C34 -1.2(3) . . . . ? N36 C33 C34 C35 -177.83(18) . . . . ? C32 C33 C34 C35 1.6(3) . . . . ? C33 C34 C35 C30 -0.4(3) . . . . ? C31 C30 C35 C34 -1.2(3) . . . . ? C29 C30 C35 C34 178.04(18) . . . . ? C32 C33 N36 C37 -5.8(3) . . . . ? C34 C33 N36 C37 173.6(2) . . . . ? C32 C33 N36 C38 173.2(2) . . . . ? C34 C33 N36 C38 -7.4(3) . . . . ? C12 C11 C39 C48 -178.40(17) . . . . ? C10 C11 C39 C48 3.0(3) . . . . ? C12 C11 C39 C40 2.3(3) . . . . ? C10 C11 C39 C40 -176.35(17) . . . . ? C11 C39 C40 C41 167(3) . . . . ? C48 C39 C40 C41 -13(3) . . . . ? C39 C40 C41 C42 112(4) . . . . ? C40 C41 C42 C43 104(3) . . . . ? C40 C41 C42 C47 -72(3) . . . . ? C47 C42 C43 C44 0.6(3) . . . . ? C41 C42 C43 C44 -175.65(18) . . . . ? C42 C43 C44 C45 -0.6(3) . . . . ? C43 C44 C45 C46 1.0(4) . . . . ? C44 C45 C46 C47 -1.4(5) . . . . ? C45 C46 C47 C42 1.4(5) . . . . ? C43 C42 C47 C46 -1.0(4) . . . . ? C41 C42 C47 C46 175.3(2) . . . . ? C11 C39 C48 C49 -141(10) . . . . ? C40 C39 C48 C49 38(10) . . . . ? C39 C48 C49 C50 56(15) . . . . ? C48 C49 C50 C55 -81(9) . . . . ? C48 C49 C50 C51 97(9) . . . . ? C55 C50 C51 C52 -0.1(3) . . . . ? C49 C50 C51 C52 -178.61(19) . . . . ? C50 C51 C52 C53 0.5(3) . . . . ? C51 C52 C53 C54 -0.3(4) . . . . ? C52 C53 C54 C55 -0.3(4) . . . . ? C53 C54 C55 C50 0.7(3) . . . . ? C51 C50 C55 C54 -0.4(3) . . . . ? C49 C50 C55 C54 178.0(2) . . . . ? C5 C6 C56 C65 4.8(3) . . . . ? C7 C6 C56 C65 -177.62(17) . . . . ? C5 C6 C56 C57 -174.53(17) . . . . ? C7 C6 C56 C57 3.0(3) . . . . ? C6 C56 C57 C58 32(3) . . . . ? C65 C56 C57 C58 -147(2) . . . . ? C56 C57 C58 C59 18(6) . . . . ? C57 C58 C59 C64 -137(4) . . . . ? C57 C58 C59 C60 44(4) . . . . ? C64 C59 C60 C61 3.2(3) . . . . ? C58 C59 C60 C61 -177.73(17) . . . . ? C59 C60 C61 C62 -0.3(3) . . . . ? C60 C61 C62 C63 -2.8(4) . . . . ? C61 C62 C63 C64 3.1(4) . . . . ? C62 C63 C64 C59 -0.2(4) . . . . ? C60 C59 C64 C63 -2.9(4) . . . . ? C58 C59 C64 C63 178.0(2) . . . . ? C6 C56 C65 C66 130(4) . . . . ? C57 C56 C65 C66 -50(5) . . . . ? C56 C65 C66 C67 -84(7) . . . . ? C65 C66 C67 C72 160(6) . . . . ? C65 C66 C67 C68 -20(6) . . . . ? C72 C67 C68 C69 0.6(3) . . . . ? C66 C67 C68 C69 -179.3(2) . . . . ? C67 C68 C69 C70 -0.5(3) . . . . ? C68 C69 C70 C71 -0.2(4) . . . . ? C69 C70 C71 C72 0.8(4) . . . . ? C70 C71 C72 C67 -0.7(4) . . . . ? C68 C67 C72 C71 0.0(4) . . . . ? C66 C67 C72 C71 179.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.277 _refine_diff_density_min -0.202 _refine_diff_density_rms 0.035