data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H36 N2 S5' _chemical_formula_sum 'C39 H36 N2 S5' _chemical_formula_weight 693.00 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.114(3) _cell_length_b 26.755(6) _cell_length_c 10.005(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.286(6) _cell_angle_gamma 90.00 _cell_volume 3607.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used 32617 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description needles _exptl_crystal_colour yellow _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 0.352 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.531 _exptl_absorpt_correction_T_max 0.990 _exptl_absorpt_process_details ; Abscor. T. Higashi (2001). The Rigaku Corporation. Takyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 233(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku SCX-Mini with Mercury CCD' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27560 _diffrn_reflns_av_R_equivalents 0.1108 _diffrn_reflns_av_sigmaI/netI 0.0973 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6338 _reflns_number_gt 3596 _reflns_threshold_expression >2sigma(I) _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. Both terminal thiophene rings were disordered. One n-butyl side chain was also disordered. The disorder groups were all modeled in a similar manner. For example, a disordered thiophene ring was modeled by assigning the variable x to the site occupancy factors of one orientation of the disorder and (1-x) to the site occupancy factors of the alternate orientation. A common isotropic displacement parameter was refined for all atoms in the two groups. The geometry of the thiophene rings was restrained to be equivalent while refining the variable x. In this way, the major component of the disordered thiophene ring composed of atoms, S3, C28, C29, C30 and C31, had a site occupancy factor of 81(2)%. For the thiophene ring composed of S5, C36, C37, C38 and C39, the site occupancy factor refined to 84(2)%. The atoms of the major component were refined anisotropically with their displacement parameters restrained to be approximately isotropic. The disorder in the n-butyl group was evident in the terminal three atoms, methylene carbon atoms, C21 and C22, and the methyl carbon, C23. The site occupancy for this group refined to a value very close to 50%. The site occupancy factors were thereafter fixed at 50%. These atoms were refined with anisotropic displacement parameters that were restrained to be approximately isotropic. ; _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^)+(0.0463P)^2^+2.6047P] 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 6338 _refine_ls_number_parameters 487 _refine_ls_number_restraints 492 _refine_ls_R_factor_all 0.1361 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.1622 _refine_ls_wR_factor_gt 0.1364 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.153 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.32425(9) 0.34504(4) 0.36126(13) 0.0511(4) Uani 1 1 d . . . S2 S 0.73530(8) 0.32350(4) 0.74774(12) 0.0448(3) Uani 1 1 d D . . S3 S 0.98986(19) 0.28930(10) 1.1060(3) 0.0918(8) Uani 0.81 1 d PDU A 1 C28 C 0.9064(5) 0.3214(2) 0.9720(9) 0.0521(15) Uani 0.81 1 d PDU A 1 C29 C 0.9447(7) 0.3675(3) 0.9529(9) 0.089(2) Uani 0.81 1 d PDU A 1 H29A H 0.9103 0.3906 0.8849 0.107 Uiso 0.81 1 calc PR A 1 C30 C 1.0391(5) 0.3764(2) 1.0441(9) 0.084(2) Uani 0.81 1 d PDU A 1 H30A H 1.0750 0.4060 1.0437 0.101 Uiso 0.81 1 calc PR A 1 C31 C 1.0731(5) 0.3385(3) 1.1322(8) 0.085(2) Uani 0.81 1 d PDU A 1 H31A H 1.1353 0.3385 1.2008 0.102 Uiso 0.81 1 calc PR A 1 S3A S 0.9433(12) 0.3693(5) 0.9435(15) 0.090(3) Uiso 0.19 1 d PDU A 2 C28A C 0.902(2) 0.3116(10) 0.979(4) 0.066(3) Uiso 0.19 1 d PDU A 2 C29A C 0.975(3) 0.2883(9) 1.085(4) 0.069(4) Uiso 0.19 1 d PDU A 2 H29B H 0.9662 0.2564 1.1196 0.083 Uiso 0.19 1 calc PR A 2 C30A C 1.060(2) 0.3158(11) 1.135(3) 0.073(4) Uiso 0.19 1 d PDU A 2 H30B H 1.1151 0.3047 1.2075 0.088 Uiso 0.19 1 calc PR A 2 C31A C 1.0560(16) 0.3608(10) 1.071(3) 0.075(4) Uiso 0.19 1 d PDU A 2 H31B H 1.1079 0.3843 1.0926 0.090 Uiso 0.19 1 calc PR A 2 S5 S 0.6274(2) -0.00334(8) 0.6409(4) 0.0765(6) Uani 0.84 1 d PDU B 1 C36 C 0.6608(5) 0.0567(2) 0.6102(8) 0.0496(15) Uani 0.84 1 d PDU B 1 C37 C 0.7570(5) 0.0562(3) 0.6017(7) 0.068(2) Uani 0.84 1 d PDU B 1 H37A H 0.7899 0.0851 0.5858 0.082 Uiso 0.84 1 calc PR B 1 C38 C 0.8005(4) 0.0087(3) 0.6189(7) 0.088(2) Uani 0.84 1 d PDU B 1 H38A H 0.8652 0.0024 0.6154 0.105 Uiso 0.84 1 calc PR B 1 C39 C 0.7390(5) -0.0269(2) 0.6413(6) 0.081(2) Uani 0.84 1 d PDU B 1 H39A H 0.7562 -0.0609 0.6554 0.097 Uiso 0.84 1 calc PR B 1 S5A S 0.7549(12) 0.0593(6) 0.5618(16) 0.083(3) Uiso 0.16 1 d PDU B 2 C36A C 0.645(2) 0.0510(13) 0.602(5) 0.061(3) Uiso 0.16 1 d PDU B 2 C37A C 0.632(3) 0.0005(14) 0.623(5) 0.068(3) Uiso 0.16 1 d PDU B 2 H37B H 0.5763 -0.0121 0.6454 0.082 Uiso 0.16 1 calc PR B 2 C38A C 0.707(3) -0.0298(8) 0.606(4) 0.077(3) Uiso 0.16 1 d PDU B 2 H38B H 0.7083 -0.0647 0.6167 0.092 Uiso 0.16 1 calc PR B 2 C39A C 0.779(2) -0.0032(7) 0.573(3) 0.074(4) Uiso 0.16 1 d PDU B 2 H39B H 0.8361 -0.0176 0.5573 0.089 Uiso 0.16 1 calc PR B 2 S4 S 0.62623(9) 0.15826(4) 0.57331(14) 0.0492(4) Uani 1 1 d . B . N1 N 0.4072(2) 0.25521(12) 0.4666(4) 0.0388(9) Uani 1 1 d . . . N2 N 0.4983(2) 0.31976(11) 0.5552(4) 0.0370(9) Uani 1 1 d . . . C1 C 0.4091(3) 0.30649(15) 0.4602(4) 0.0386(11) Uani 1 1 d . . . C2 C 0.5513(3) 0.27721(14) 0.6203(4) 0.0356(10) Uani 1 1 d . . . C3 C 0.4941(3) 0.23656(15) 0.5623(4) 0.0359(10) Uani 1 1 d . . . C4 C 0.3258(3) 0.22531(15) 0.3835(5) 0.0405(11) Uani 1 1 d . . . C5 C 0.3385(3) 0.19655(16) 0.2765(5) 0.0467(12) Uani 1 1 d . . . H5 H 0.3993 0.1970 0.2559 0.056 Uiso 1 1 calc R . . C6 C 0.2613(4) 0.16688(18) 0.1990(5) 0.0574(14) Uani 1 1 d . . . H6 H 0.2706 0.1467 0.1271 0.069 Uiso 1 1 calc R . . C7 C 0.1703(4) 0.16658(18) 0.2259(5) 0.0568(14) Uani 1 1 d . . . C8 C 0.1594(4) 0.19666(19) 0.3326(6) 0.0599(14) Uani 1 1 d . . . H8 H 0.0981 0.1972 0.3517 0.072 Uiso 1 1 calc R . . C9 C 0.2359(3) 0.22593(17) 0.4120(5) 0.0527(13) Uani 1 1 d . . . H9 H 0.2269 0.2460 0.4844 0.063 Uiso 1 1 calc R . . C10 C 0.0844(4) 0.1341(2) 0.1394(7) 0.0832(19) Uani 1 1 d . . . H10A H 0.1084 0.0998 0.1399 0.100 Uiso 1 1 calc R . . H10B H 0.0324 0.1339 0.1861 0.100 Uiso 1 1 calc R . . C11 C 0.0406(6) 0.1491(3) -0.0029(8) 0.137(3) Uani 1 1 d . . . H11A H 0.0922 0.1484 -0.0503 0.164 Uiso 1 1 calc R . . H11B H 0.0183 0.1838 -0.0035 0.164 Uiso 1 1 calc R . . C12 C -0.0480(6) 0.1171(3) -0.0891(8) 0.138(3) Uani 1 1 d . . . H12A H -0.0581 0.1238 -0.1887 0.166 Uiso 1 1 calc R . . H12B H -0.0304 0.0818 -0.0725 0.166 Uiso 1 1 calc R . . C13 C -0.1383(6) 0.1253(4) -0.0599(10) 0.152(4) Uani 1 1 d . . . H13A H -0.1291 0.1197 0.0389 0.228 Uiso 1 1 calc R . . H13B H -0.1881 0.1024 -0.1147 0.228 Uiso 1 1 calc R . . H13C H -0.1599 0.1595 -0.0838 0.228 Uiso 1 1 calc R . . C14 C 0.5351(3) 0.37077(15) 0.5734(5) 0.0372(11) Uani 1 1 d . . . C15 C 0.5307(3) 0.39872(16) 0.6866(5) 0.0463(12) Uani 1 1 d . . . H15 H 0.5013 0.3856 0.7519 0.056 Uiso 1 1 calc R . . C16 C 0.5707(3) 0.44711(17) 0.7031(6) 0.0546(14) Uani 1 1 d . . . H16 H 0.5692 0.4661 0.7814 0.066 Uiso 1 1 calc R . . C17 C 0.6126(3) 0.46745(16) 0.6059(6) 0.0529(14) Uani 1 1 d . D . C18 C 0.6142(3) 0.43828(17) 0.4923(5) 0.0532(13) Uani 1 1 d . . . H18 H 0.6415 0.4515 0.4249 0.064 Uiso 1 1 calc R . . C19 C 0.5762(3) 0.38994(16) 0.4755(5) 0.0443(12) Uani 1 1 d . . . H19 H 0.5786 0.3706 0.3982 0.053 Uiso 1 1 calc R . . C20 C 0.6568(4) 0.51943(17) 0.6243(7) 0.0758(18) Uani 1 1 d D . . H20C H 0.6521 0.5330 0.7110 0.091 Uiso 0.50 1 d PR C 2 H20D H 0.6168 0.5398 0.5499 0.091 Uiso 0.50 1 d PR C 2 H20A H 0.6138 0.5410 0.6565 0.091 Uiso 0.50 1 d PR C 1 H20B H 0.6594 0.5316 0.5352 0.091 Uiso 0.50 1 d PR C 1 C21 C 0.7611(7) 0.5221(6) 0.7261(14) 0.110(5) Uani 0.50 1 d PDU D 1 H21A H 0.7628 0.5056 0.8141 0.132 Uiso 0.50 1 calc PR D 1 H21B H 0.7805 0.5571 0.7466 0.132 Uiso 0.50 1 calc PR D 1 C22 C 0.8355(8) 0.4956(7) 0.659(2) 0.124(5) Uani 0.50 1 d PDU D 1 H22A H 0.8264 0.4597 0.6702 0.149 Uiso 0.50 1 calc PR D 1 H22B H 0.8092 0.5021 0.5579 0.149 Uiso 0.50 1 calc PR D 1 C23 C 0.9331(9) 0.5020(8) 0.689(2) 0.153(7) Uani 0.50 1 d PDU D 1 H23A H 0.9560 0.5237 0.7697 0.229 Uiso 0.50 1 calc PR D 1 H23B H 0.9484 0.5170 0.6096 0.229 Uiso 0.50 1 calc PR D 1 H23C H 0.9661 0.4699 0.7097 0.229 Uiso 0.50 1 calc PR D 1 C21A C 0.7639(7) 0.5230(6) 0.6249(17) 0.112(5) Uani 0.50 1 d PDU D 2 H21C H 0.7847 0.5581 0.6348 0.135 Uiso 0.50 1 calc PR D 2 H21D H 0.7698 0.5108 0.5354 0.135 Uiso 0.50 1 calc PR D 2 C22A C 0.8342(7) 0.4918(6) 0.748(2) 0.110(5) Uani 0.50 1 d PDU D 2 H22C H 0.8154 0.5003 0.8316 0.132 Uiso 0.50 1 calc PR D 2 H22D H 0.8155 0.4567 0.7269 0.132 Uiso 0.50 1 calc PR D 2 C23A C 0.9351(8) 0.4929(7) 0.787(2) 0.135(6) Uani 0.50 1 d PDU D 2 H23D H 0.9588 0.4716 0.7251 0.203 Uiso 0.50 1 calc PR D 2 H23E H 0.9611 0.4810 0.8823 0.203 Uiso 0.50 1 calc PR D 2 H23F H 0.9573 0.5269 0.7810 0.203 Uiso 0.50 1 calc PR D 2 C24 C 0.6428(3) 0.27920(14) 0.7352(4) 0.0377(11) Uani 1 1 d D . . C25 C 0.6712(3) 0.24690(14) 0.8460(4) 0.0465(12) Uani 1 1 d D . . H25 H 0.6314 0.2202 0.8584 0.056 Uiso 1 1 calc R . . C26 C 0.7649(3) 0.25714(16) 0.9394(4) 0.0542(13) Uani 1 1 d D A . H26 H 0.7940 0.2384 1.0207 0.065 Uiso 1 1 calc R . . C27 C 0.8091(3) 0.29733(15) 0.8992(4) 0.0430(12) Uani 1 1 d D . . C32 C 0.5139(3) 0.18302(15) 0.5817(4) 0.0378(11) Uani 1 1 d . . . C33 C 0.4534(3) 0.14575(16) 0.6002(5) 0.0462(12) Uani 1 1 d . . . H33 H 0.3890 0.1515 0.6060 0.055 Uiso 1 1 calc R . . C34 C 0.4959(4) 0.09803(16) 0.6100(5) 0.0504(13) Uani 1 1 d . B . H34 H 0.4626 0.0688 0.6228 0.060 Uiso 1 1 calc R . . C35 C 0.5906(4) 0.09786(15) 0.5991(5) 0.0432(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0337(7) 0.0474(7) 0.0622(9) 0.0097(6) -0.0010(6) -0.0001(5) S2 0.0320(7) 0.0443(7) 0.0503(7) 0.0035(5) 0.0003(6) -0.0057(5) S3 0.0512(14) 0.1190(17) 0.0762(15) 0.0054(12) -0.0256(11) 0.0091(12) C28 0.040(3) 0.053(3) 0.057(3) -0.011(3) 0.004(3) 0.003(3) C29 0.061(4) 0.098(4) 0.096(4) -0.020(3) 0.002(3) -0.005(3) C30 0.056(4) 0.092(4) 0.092(4) -0.023(3) 0.003(3) -0.017(3) C31 0.057(4) 0.098(4) 0.084(4) -0.018(4) -0.004(3) -0.016(3) S5 0.0930(14) 0.0383(9) 0.0994(17) 0.0056(9) 0.0306(11) 0.0060(9) C36 0.055(3) 0.042(3) 0.051(3) -0.006(2) 0.014(3) 0.004(2) C37 0.068(3) 0.059(3) 0.079(4) 0.005(3) 0.024(3) 0.011(3) C38 0.076(4) 0.080(4) 0.101(4) -0.007(3) 0.017(3) 0.026(3) C39 0.082(4) 0.058(3) 0.088(4) -0.002(3) 0.003(3) 0.023(3) S4 0.0387(7) 0.0361(7) 0.0722(9) 0.0020(6) 0.0153(7) -0.0003(5) N1 0.029(2) 0.035(2) 0.046(2) 0.0017(16) 0.0020(18) -0.0021(15) N2 0.030(2) 0.031(2) 0.044(2) 0.0011(16) 0.0017(18) -0.0050(15) C1 0.027(3) 0.040(3) 0.045(3) -0.002(2) 0.004(2) -0.0024(18) C2 0.034(3) 0.030(2) 0.042(3) 0.0010(19) 0.009(2) -0.0015(19) C3 0.031(3) 0.037(3) 0.038(3) 0.0013(19) 0.006(2) -0.0035(19) C4 0.033(3) 0.038(3) 0.043(3) 0.001(2) 0.000(2) -0.007(2) C5 0.038(3) 0.049(3) 0.052(3) -0.006(2) 0.013(2) -0.009(2) C6 0.069(4) 0.051(3) 0.050(3) -0.012(2) 0.015(3) -0.014(3) C7 0.051(4) 0.054(3) 0.056(4) 0.004(3) 0.001(3) -0.020(2) C8 0.040(3) 0.069(4) 0.070(4) -0.004(3) 0.014(3) -0.015(3) C9 0.036(3) 0.057(3) 0.064(3) -0.014(2) 0.013(3) -0.013(2) C10 0.071(4) 0.072(4) 0.092(5) -0.009(3) 0.001(4) -0.037(3) C11 0.121(7) 0.158(8) 0.092(6) -0.005(5) -0.026(5) -0.072(6) C12 0.084(6) 0.200(9) 0.107(6) -0.055(6) -0.008(5) -0.057(6) C13 0.074(6) 0.196(9) 0.188(9) -0.078(7) 0.039(6) -0.016(6) C14 0.026(2) 0.034(2) 0.044(3) 0.001(2) -0.001(2) 0.0018(18) C15 0.041(3) 0.044(3) 0.054(3) -0.005(2) 0.014(2) 0.000(2) C16 0.048(3) 0.047(3) 0.064(4) -0.017(3) 0.008(3) 0.004(2) C17 0.040(3) 0.031(3) 0.075(4) 0.000(3) -0.003(3) 0.002(2) C18 0.047(3) 0.050(3) 0.059(3) 0.011(3) 0.009(3) -0.012(2) C19 0.042(3) 0.041(3) 0.048(3) 0.003(2) 0.011(2) -0.004(2) C20 0.047(3) 0.037(3) 0.129(5) -0.001(3) 0.005(3) -0.005(2) C21 0.064(6) 0.047(5) 0.171(14) 0.015(8) -0.038(7) -0.009(4) C22 0.065(6) 0.074(6) 0.187(14) 0.002(9) -0.035(7) -0.001(5) C23 0.105(9) 0.118(10) 0.217(17) 0.013(12) 0.019(11) -0.024(8) C21A 0.063(6) 0.052(5) 0.180(14) 0.009(9) -0.029(7) -0.010(4) C22A 0.054(5) 0.065(5) 0.172(13) 0.018(8) -0.026(7) -0.013(4) C23A 0.094(9) 0.099(9) 0.182(16) 0.030(11) -0.006(10) -0.022(7) C24 0.030(3) 0.030(2) 0.049(3) -0.003(2) 0.005(2) -0.0002(18) C25 0.053(3) 0.031(3) 0.050(3) 0.003(2) 0.008(3) -0.003(2) C26 0.056(3) 0.049(3) 0.044(3) 0.005(2) -0.006(3) 0.010(2) C27 0.032(3) 0.041(3) 0.048(3) -0.006(2) 0.000(2) 0.007(2) C32 0.032(3) 0.036(3) 0.041(3) -0.0003(19) 0.005(2) -0.0023(19) C33 0.036(3) 0.039(3) 0.062(3) 0.001(2) 0.012(2) -0.003(2) C34 0.052(3) 0.036(3) 0.062(3) 0.004(2) 0.015(3) -0.013(2) C35 0.048(3) 0.035(3) 0.041(3) -0.0048(19) 0.003(2) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C1 1.665(4) . ? S2 C27 1.712(4) . ? S2 C24 1.740(4) . ? S3 C28 1.728(5) . ? S3 C31 1.731(6) . ? C28 C29 1.382(7) . ? C28 C27 1.496(7) . ? C29 C30 1.394(8) . ? C29 H29A 0.9400 . ? C30 C31 1.336(9) . ? C30 H30A 0.9400 . ? C31 H31A 0.9400 . ? S3A C28A 1.725(8) . ? S3A C31A 1.733(8) . ? C28A C27 1.37(2) . ? C28A C29A 1.388(8) . ? C29A C30A 1.371(9) . ? C29A H29B 0.9400 . ? C30A C31A 1.360(14) . ? C30A H30B 0.9400 . ? C31A H31B 0.9400 . ? S5 C39 1.696(6) . ? S5 C36 1.727(5) . ? C36 C37 1.384(6) . ? C36 C35 1.465(7) . ? C37 C38 1.399(6) . ? C37 H37A 0.9400 . ? C38 C39 1.352(7) . ? C38 H38A 0.9400 . ? C39 H39A 0.9400 . ? S5A C39A 1.705(9) . ? S5A C36A 1.727(8) . ? C36A C37A 1.387(8) . ? C36A C35 1.47(3) . ? C37A C38A 1.385(8) . ? C37A H37B 0.9400 . ? C38A C39A 1.366(9) . ? C38A H38B 0.9400 . ? C39A H39B 0.9400 . ? S4 C35 1.735(4) . ? S4 C32 1.743(4) . ? N1 C1 1.374(5) . ? N1 C3 1.405(5) . ? N1 C4 1.443(5) . ? N2 C1 1.379(5) . ? N2 C2 1.411(5) . ? N2 C14 1.452(5) . ? C2 C3 1.376(5) . ? C2 C24 1.453(5) . ? C3 C32 1.461(6) . ? C4 C5 1.373(6) . ? C4 C9 1.381(6) . ? C5 C6 1.384(6) . ? C5 H5 0.9400 . ? C6 C7 1.389(7) . ? C6 H6 0.9400 . ? C7 C8 1.382(7) . ? C7 C10 1.533(6) . ? C8 C9 1.378(6) . ? C8 H8 0.9400 . ? C9 H9 0.9400 . ? C10 C11 1.430(8) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 C12 1.548(8) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 C13 1.406(9) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 C15 1.373(6) . ? C14 C19 1.378(6) . ? C15 C16 1.402(6) . ? C15 H15 0.9400 . ? C16 C17 1.391(7) . ? C16 H16 0.9400 . ? C17 C18 1.384(7) . ? C17 C20 1.513(6) . ? C18 C19 1.391(6) . ? C18 H18 0.9400 . ? C19 H19 0.9400 . ? C20 C21A 1.513(10) . ? C20 C21 1.523(9) . ? C20 H20C 0.9601 . ? C20 H20D 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9599 . ? C21 C22 1.577(14) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 C23 1.330(11) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C21A C22A 1.571(13) . ? C21A H21C 0.9800 . ? C21A H21D 0.9800 . ? C22A C23A 1.360(11) . ? C22A H22C 0.9800 . ? C22A H22D 0.9800 . ? C23A H23D 0.9700 . ? C23A H23E 0.9700 . ? C23A H23F 0.9700 . ? C24 C25 1.368(5) . ? C25 C26 1.401(5) . ? C25 H25 0.9400 . ? C26 C27 1.363(5) . ? C26 H26 0.9400 . ? C32 C33 1.361(6) . ? C33 C34 1.402(6) . ? C33 H33 0.9400 . ? C34 C35 1.372(6) . ? C34 H34 0.9400 . ? 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 C27 S2 C24 91.79(19) . . ? C28 S3 C31 90.9(3) . . ? C29 C28 C27 131.0(6) . . ? C29 C28 S3 110.3(4) . . ? C27 C28 S3 118.7(4) . . ? C28 C29 C30 113.5(5) . . ? C28 C29 H29A 123.2 . . ? C30 C29 H29A 123.2 . . ? C31 C30 C29 112.8(5) . . ? C31 C30 H30A 123.6 . . ? C29 C30 H30A 123.6 . . ? C30 C31 S3 112.5(4) . . ? C30 C31 H31A 123.7 . . ? S3 C31 H31A 123.7 . . ? C28A S3A C31A 91.5(4) . . ? C27 C28A C29A 133.1(17) . . ? C27 C28A S3A 117.1(16) . . ? C29A C28A S3A 109.8(5) . . ? C30A C29A C28A 114.2(6) . . ? C30A C29A H29B 122.9 . . ? C28A C29A H29B 122.9 . . ? C31A C30A C29A 113.2(6) . . ? C31A C30A H30B 123.4 . . ? C29A C30A H30B 123.4 . . ? C30A C31A S3A 111.3(5) . . ? C30A C31A H31B 124.4 . . ? S3A C31A H31B 124.4 . . ? C39 S5 C36 92.5(3) . . ? C37 C36 C35 131.0(5) . . ? C37 C36 S5 109.1(4) . . ? C35 C36 S5 119.9(4) . . ? C36 C37 C38 113.7(4) . . ? C36 C37 H37A 123.1 . . ? C38 C37 H37A 123.1 . . ? C39 C38 C37 112.4(4) . . ? C39 C38 H38A 123.8 . . ? C37 C38 H38A 123.8 . . ? C38 C39 S5 112.3(4) . . ? C38 C39 H39A 123.9 . . ? S5 C39 H39A 123.9 . . ? C39A S5A C36A 92.2(4) . . ? C37A C36A C35 137.8(19) . . ? C37A C36A S5A 109.4(5) . . ? C35 C36A S5A 112.7(18) . . ? C38A C37A C36A 114.1(5) . . ? C38A C37A H37B 123.0 . . ? C36A C37A H37B 123.0 . . ? C39A C38A C37A 112.4(5) . . ? C39A C38A H38B 123.8 . . ? C37A C38A H38B 123.8 . . ? C38A C39A S5A 111.9(5) . . ? C38A C39A H39B 124.0 . . ? S5A C39A H39B 124.0 . . ? C35 S4 C32 92.2(2) . . ? C1 N1 C3 111.2(3) . . ? C1 N1 C4 123.4(3) . . ? C3 N1 C4 125.5(3) . . ? C1 N2 C2 111.1(3) . . ? C1 N2 C14 123.2(3) . . ? C2 N2 C14 125.4(3) . . ? N1 C1 N2 104.6(3) . . ? N1 C1 S1 128.7(3) . . ? N2 C1 S1 126.7(3) . . ? C3 C2 N2 106.2(3) . . ? C3 C2 C24 129.4(4) . . ? N2 C2 C24 124.1(3) . . ? C2 C3 N1 106.9(3) . . ? C2 C3 C32 130.9(4) . . ? N1 C3 C32 122.2(3) . . ? C5 C4 C9 120.6(4) . . ? C5 C4 N1 119.6(4) . . ? C9 C4 N1 119.9(4) . . ? C4 C5 C6 119.6(4) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C5 C6 C7 121.0(5) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C8 C7 C6 117.9(4) . . ? C8 C7 C10 121.0(5) . . ? C6 C7 C10 121.1(5) . . ? C9 C8 C7 121.9(5) . . ? C9 C8 H8 119.0 . . ? C7 C8 H8 119.0 . . ? C8 C9 C4 119.0(5) . . ? C8 C9 H9 120.5 . . ? C4 C9 H9 120.5 . . ? C11 C10 C7 116.0(5) . . ? C11 C10 H10A 108.3 . . ? C7 C10 H10A 108.3 . . ? C11 C10 H10B 108.3 . . ? C7 C10 H10B 108.3 . . ? H10A C10 H10B 107.4 . . ? C10 C11 C12 116.0(6) . . ? C10 C11 H11A 108.3 . . ? C12 C11 H11A 108.3 . . ? C10 C11 H11B 108.3 . . ? C12 C11 H11B 108.3 . . ? H11A C11 H11B 107.4 . . ? C13 C12 C11 115.5(8) . . ? C13 C12 H12A 108.4 . . ? C11 C12 H12A 108.4 . . ? C13 C12 H12B 108.4 . . ? C11 C12 H12B 108.4 . . ? H12A C12 H12B 107.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C19 121.0(4) . . ? C15 C14 N2 120.9(4) . . ? C19 C14 N2 118.1(4) . . ? C14 C15 C16 119.0(5) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? C17 C16 C15 121.3(5) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C18 C17 C16 117.9(4) . . ? C18 C17 C20 120.8(5) . . ? C16 C17 C20 121.3(5) . . ? C17 C18 C19 121.6(5) . . ? C17 C18 H18 119.2 . . ? C19 C18 H18 119.2 . . ? C14 C19 C18 119.3(4) . . ? C14 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? C17 C20 C21A 115.7(7) . . ? C17 C20 C21 114.0(7) . . ? C17 C20 H20C 108.7 . . ? C21A C20 H20C 108.0 . . ? C17 C20 H20D 107.5 . . ? C21A C20 H20D 108.9 . . ? H20C C20 H20D 107.6 . . ? C17 C20 H20A 108.4 . . ? C21 C20 H20A 109.2 . . ? C17 C20 H20B 109.0 . . ? C21 C20 H20B 108.0 . . ? H20A C20 H20B 108.0 . . ? C20 C21 C22 109.1(9) . . ? C20 C21 H21A 109.9 . . ? C22 C21 H21A 109.9 . . ? C20 C21 H21B 109.9 . . ? C22 C21 H21B 109.9 . . ? H21A C21 H21B 108.3 . . ? C23 C22 C21 128.3(12) . . ? C23 C22 H22A 105.2 . . ? C21 C22 H22A 105.2 . . ? C23 C22 H22B 105.2 . . ? C21 C22 H22B 105.2 . . ? H22A C22 H22B 105.9 . . ? C20 C21A C22A 111.6(9) . . ? C20 C21A H21C 109.3 . . ? C22A C21A H21C 109.3 . . ? H20B C21A H21C 97.3 . . ? C20 C21A H21D 109.3 . . ? C22A C21A H21D 109.3 . . ? H21C C21A H21D 108.0 . . ? C23A C22A C21A 125.2(11) . . ? C23A C22A H22C 106.0 . . ? C21A C22A H22C 106.0 . . ? C23A C22A H22D 106.0 . . ? C21A C22A H22D 106.0 . . ? H22C C22A H22D 106.3 . . ? C22A C23A H23D 109.5 . . ? C22A C23A H23E 109.5 . . ? H23D C23A H23E 109.5 . . ? C22A C23A H23F 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? C25 C24 C2 126.6(4) . . ? C25 C24 S2 109.8(3) . . ? C2 C24 S2 123.6(3) . . ? C24 C25 C26 114.1(3) . . ? C24 C25 H25 123.0 . . ? C26 C25 H25 123.0 . . ? C27 C26 C25 112.4(3) . . ? C27 C26 H26 123.8 . . ? C25 C26 H26 123.8 . . ? C26 C27 C28A 119.3(10) . . ? C26 C27 C28 129.1(4) . . ? C26 C27 S2 111.9(3) . . ? C28A C27 S2 128.8(10) . . ? C28 C27 S2 118.9(4) . . ? C33 C32 C3 129.3(4) . . ? C33 C32 S4 110.2(3) . . ? C3 C32 S4 120.5(3) . . ? C32 C33 C34 113.8(4) . . ? C32 C33 H33 123.1 . . ? C34 C33 H33 123.1 . . ? C35 C34 C33 113.8(4) . . ? C35 C34 H34 123.1 . . ? C33 C34 H34 123.1 . . ? C34 C35 C36 130.5(4) . . ? C34 C35 C36A 121.2(10) . . ? C34 C35 S4 110.0(3) . . ? C36 C35 S4 119.5(4) . . ? C36A C35 S4 128.7(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C31 S3 C28 C29 0.08(15) . . . . ? C31 S3 C28 C27 -179.3(8) . . . . ? C27 C28 C29 C30 179.4(10) . . . . ? S3 C28 C29 C30 0.1(2) . . . . ? C28 C29 C30 C31 -0.3(4) . . . . ? C29 C30 C31 S3 0.4(5) . . . . ? C28 S3 C31 C30 -0.3(3) . . . . ? C31A S3A C28A C27 -179(4) . . . . ? C31A S3A C28A C29A -0.02(16) . . . . ? C27 C28A C29A C30A 178(5) . . . . ? S3A C28A C29A C30A 0.0(2) . . . . ? C28A C29A C30A C31A 0.0(5) . . . . ? C29A C30A C31A S3A 0.0(5) . . . . ? C28A S3A C31A C30A 0.0(4) . . . . ? C39 S5 C36 C37 -0.14(15) . . . . ? C39 S5 C36 C35 -179.4(6) . . . . ? C35 C36 C37 C38 179.5(7) . . . . ? S5 C36 C37 C38 0.3(2) . . . . ? C36 C37 C38 C39 -0.4(4) . . . . ? C37 C38 C39 S5 0.3(4) . . . . ? C36 S5 C39 C38 -0.1(3) . . . . ? C39A S5A C36A C37A 0.05(16) . . . . ? C39A S5A C36A C35 -177(3) . . . . ? C35 C36A C37A C38A 176(5) . . . . ? S5A C36A C37A C38A 0.0(2) . . . . ? C36A C37A C38A C39A -0.1(4) . . . . ? C37A C38A C39A S5A 0.2(5) . . . . ? C36A S5A C39A C38A -0.1(4) . . . . ? C3 N1 C1 N2 -0.8(5) . . . . ? C4 N1 C1 N2 179.7(4) . . . . ? C3 N1 C1 S1 179.1(3) . . . . ? C4 N1 C1 S1 -0.4(6) . . . . ? C2 N2 C1 N1 -0.2(5) . . . . ? C14 N2 C1 N1 174.3(4) . . . . ? C2 N2 C1 S1 179.9(3) . . . . ? C14 N2 C1 S1 -5.6(6) . . . . ? C1 N2 C2 C3 1.1(5) . . . . ? C14 N2 C2 C3 -173.3(4) . . . . ? C1 N2 C2 C24 -173.4(4) . . . . ? C14 N2 C2 C24 12.3(6) . . . . ? N2 C2 C3 N1 -1.5(5) . . . . ? C24 C2 C3 N1 172.5(4) . . . . ? N2 C2 C3 C32 175.3(4) . . . . ? C24 C2 C3 C32 -10.7(8) . . . . ? C1 N1 C3 C2 1.5(5) . . . . ? C4 N1 C3 C2 -179.0(4) . . . . ? C1 N1 C3 C32 -175.6(4) . . . . ? C4 N1 C3 C32 3.8(6) . . . . ? C1 N1 C4 C5 109.5(5) . . . . ? C3 N1 C4 C5 -69.9(6) . . . . ? C1 N1 C4 C9 -70.3(6) . . . . ? C3 N1 C4 C9 110.3(5) . . . . ? C9 C4 C5 C6 -1.8(7) . . . . ? N1 C4 C5 C6 178.4(4) . . . . ? C4 C5 C6 C7 1.4(7) . . . . ? C5 C6 C7 C8 -0.2(7) . . . . ? C5 C6 C7 C10 179.4(5) . . . . ? C6 C7 C8 C9 -0.6(8) . . . . ? C10 C7 C8 C9 179.7(5) . . . . ? C7 C8 C9 C4 0.3(8) . . . . ? C5 C4 C9 C8 1.0(7) . . . . ? N1 C4 C9 C8 -179.2(4) . . . . ? C8 C7 C10 C11 110.2(7) . . . . ? C6 C7 C10 C11 -69.4(8) . . . . ? C7 C10 C11 C12 -178.4(7) . . . . ? C10 C11 C12 C13 75.5(11) . . . . ? C1 N2 C14 C15 103.8(5) . . . . ? C2 N2 C14 C15 -82.5(5) . . . . ? C1 N2 C14 C19 -77.5(5) . . . . ? C2 N2 C14 C19 96.3(5) . . . . ? C19 C14 C15 C16 -1.3(6) . . . . ? N2 C14 C15 C16 177.4(4) . . . . ? C14 C15 C16 C17 1.3(7) . . . . ? C15 C16 C17 C18 -0.4(7) . . . . ? C15 C16 C17 C20 -179.3(4) . . . . ? C16 C17 C18 C19 -0.7(7) . . . . ? C20 C17 C18 C19 178.3(4) . . . . ? C15 C14 C19 C18 0.3(6) . . . . ? N2 C14 C19 C18 -178.5(4) . . . . ? C17 C18 C19 C14 0.7(7) . . . . ? C18 C17 C20 C21A -55.1(9) . . . . ? C16 C17 C20 C21A 123.8(8) . . . . ? C18 C17 C20 C21 -98.7(8) . . . . ? C16 C17 C20 C21 80.2(8) . . . . ? C17 C20 C21 C22 69.9(15) . . . . ? C21A C20 C21 C22 -32.0(10) . . . . ? C20 C21 C22 C23 157.7(18) . . . . ? C17 C20 C21A C22A -60.6(18) . . . . ? C21 C20 C21A C22A 36.6(11) . . . . ? C20 C21A C22A C23A -170.7(17) . . . . ? C3 C2 C24 C25 -29.2(7) . . . . ? N2 C2 C24 C25 143.9(4) . . . . ? C3 C2 C24 S2 148.9(4) . . . . ? N2 C2 C24 S2 -38.0(6) . . . . ? C27 S2 C24 C25 0.4(4) . . . . ? C27 S2 C24 C2 -177.9(4) . . . . ? C2 C24 C25 C26 178.3(4) . . . . ? S2 C24 C25 C26 0.0(5) . . . . ? C24 C25 C26 C27 -0.6(6) . . . . ? C25 C26 C27 C28A -179(2) . . . . ? C25 C26 C27 C28 177.4(6) . . . . ? C25 C26 C27 S2 0.9(5) . . . . ? C29A C28A C27 C26 14(4) . . . . ? S3A C28A C27 C26 -167.3(16) . . . . ? C29A C28A C27 C28 178(16) . . . . ? S3A C28A C27 C28 -3(11) . . . . ? C29A C28A C27 S2 -165.4(15) . . . . ? S3A C28A C27 S2 13(4) . . . . ? C29 C28 C27 C26 -164.1(5) . . . . ? S3 C28 C27 C26 15.1(10) . . . . ? C29 C28 C27 C28A 178(14) . . . . ? S3 C28 C27 C28A -3(13) . . . . ? C29 C28 C27 S2 12.1(8) . . . . ? S3 C28 C27 S2 -168.7(4) . . . . ? C24 S2 C27 C26 -0.8(4) . . . . ? C24 S2 C27 C28A 179(3) . . . . ? C24 S2 C27 C28 -177.6(5) . . . . ? C2 C3 C32 C33 135.9(5) . . . . ? N1 C3 C32 C33 -47.7(7) . . . . ? C2 C3 C32 S4 -47.8(6) . . . . ? N1 C3 C32 S4 128.6(4) . . . . ? C35 S4 C32 C33 -1.3(4) . . . . ? C35 S4 C32 C3 -178.2(4) . . . . ? C3 C32 C33 C34 177.6(4) . . . . ? S4 C32 C33 C34 0.9(5) . . . . ? C32 C33 C34 C35 0.1(6) . . . . ? C33 C34 C35 C36 176.9(5) . . . . ? C33 C34 C35 C36A -178(2) . . . . ? C33 C34 C35 S4 -1.0(5) . . . . ? C37 C36 C35 C34 -178.8(4) . . . . ? S5 C36 C35 C34 0.4(8) . . . . ? C37 C36 C35 C36A 155(11) . . . . ? S5 C36 C35 C36A -26(11) . . . . ? C37 C36 C35 S4 -1.0(7) . . . . ? S5 C36 C35 S4 178.1(3) . . . . ? C37A C36A C35 C34 -5(4) . . . . ? S5A C36A C35 C34 171.3(14) . . . . ? C37A C36A C35 C36 152(13) . . . . ? S5A C36A C35 C36 -32(9) . . . . ? C37A C36A C35 S4 178.8(16) . . . . ? S5A C36A C35 S4 -5(4) . . . . ? C32 S4 C35 C34 1.3(4) . . . . ? C32 S4 C35 C36 -176.9(4) . . . . ? C32 S4 C35 C36A 178(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.340 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.060