# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_calix6 _database_code_depnum_ccdc_archive 'CCDC 868896' #TrackingRef 'calix6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C90 H66 N4 S24, Cl 1-, C16 H36 N 1+, 4 C H2 Cl2' _chemical_formula_sum 'C110 H110 Cl9 N7 S24' _chemical_formula_weight 2618.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.769(2) _cell_length_b 20.0818(12) _cell_length_c 24.852(2) _cell_angle_alpha 90.00 _cell_angle_beta 129.585(3) _cell_angle_gamma 90.00 _cell_volume 12219.2(14) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 11369 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 26.0 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5424 _exptl_absorpt_coefficient_mu 0.666 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.922 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 86545 _diffrn_reflns_av_R_equivalents 0.156 _diffrn_reflns_av_sigmaI/netI 0.3699 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10665 _reflns_number_gt 3192 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _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. There are two molecules of DCM in the asymmetric unit. One molecule was reasonably well behaved while the second molecule was disordered. The disordered DCM could not be adequately modeled and was removed using the utility, SQUEEZE (Sluis and Spek, 1990). ; _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^)+(0.0770P)^2^] 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 10665 _refine_ls_number_parameters 659 _refine_ls_number_restraints 438 _refine_ls_R_factor_all 0.2891 _refine_ls_R_factor_gt 0.1086 _refine_ls_wR_factor_ref 0.2479 _refine_ls_wR_factor_gt 0.2212 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.154 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 0.36281(13) 0.24316(14) 0.52554(18) 0.0830(10) Uani 1 1 d U . . S2 S 0.35312(12) 0.35717(14) 0.59545(18) 0.0794(10) Uani 1 1 d U . . S3 S 0.29890(13) 0.14871(14) 0.55282(18) 0.0817(10) Uani 1 1 d U . . S4 S 0.28805(13) 0.25731(14) 0.62442(18) 0.0829(10) Uani 1 1 d U . . S5 S 0.29510(11) 0.59813(14) 0.51630(16) 0.0708(9) Uani 1 1 d U . . S6 S 0.26964(11) 0.68002(14) 0.39810(16) 0.0686(9) Uani 1 1 d U . . S7 S 0.19467(11) 0.66646(15) 0.49653(16) 0.0726(9) Uani 1 1 d U . . S8 S 0.16859(12) 0.74555(15) 0.37845(16) 0.0773(10) Uani 1 1 d U . . S9 S 0.38258(12) 0.81925(14) 0.36985(17) 0.0772(10) Uani 1 1 d U . . S10 S 0.50267(12) 0.84913(13) 0.46811(17) 0.0796(10) Uani 1 1 d U . . S11 S 0.36124(14) 0.96959(17) 0.3101(2) 0.1041(12) Uani 1 1 d U . . S12 S 0.48072(13) 0.99464(14) 0.40725(17) 0.0833(10) Uani 1 1 d U . . N1 N 0.4225(3) 0.4095(4) 0.5153(4) 0.066(2) Uani 1 1 d U . . H1N H 0.4388 0.4356 0.5052 0.079 Uiso 1 1 calc R . . N2 N 0.3969(3) 0.5679(4) 0.4800(5) 0.072(3) Uani 1 1 d U . . H2N H 0.4249 0.5505 0.4856 0.087 Uiso 1 1 calc R . . N3 N 0.4715(4) 0.6575(4) 0.4617(4) 0.061(2) Uani 1 1 d U . . H3N H 0.4788 0.6150 0.4719 0.073 Uiso 1 1 calc R . . C1 C 0.4103(4) 0.3450(5) 0.4963(5) 0.055(3) Uani 1 1 d U . . C2 C 0.3870(4) 0.3240(5) 0.5244(6) 0.068(3) Uani 1 1 d U . . C3 C 0.3830(4) 0.3749(5) 0.5586(5) 0.059(3) Uani 1 1 d U . . C4 C 0.4059(4) 0.4298(5) 0.5532(6) 0.062(3) Uani 1 1 d U . . C5 C 0.3376(4) 0.2745(5) 0.5674(5) 0.068(3) Uani 1 1 d U . . C6 C 0.3106(4) 0.2327(5) 0.5787(5) 0.073(3) Uani 1 1 d U . . C7 C 0.2704(4) 0.1273(5) 0.5915(6) 0.064(3) Uani 1 1 d U . . C8 C 0.2518(4) 0.0644(5) 0.5892(6) 0.069(3) Uani 1 1 d U . . H8 H 0.2539 0.0299 0.5648 0.083 Uiso 1 1 calc R . . C9 C 0.2307(4) 0.0508(6) 0.6211(6) 0.072(3) Uani 1 1 d U . . H9 H 0.2178 0.0074 0.6189 0.087 Uiso 1 1 calc R . . C10 C 0.2282(4) 0.1003(6) 0.6561(6) 0.072(3) Uani 1 1 d U . . H10 H 0.2136 0.0900 0.6787 0.087 Uiso 1 1 calc R . . C11 C 0.2460(4) 0.1659(6) 0.6612(5) 0.068(3) Uani 1 1 d U . . H11 H 0.2439 0.2001 0.6858 0.082 Uiso 1 1 calc R . . C12 C 0.2671(4) 0.1762(5) 0.6269(6) 0.066(3) Uani 1 1 d U . . C13 C 0.4154(4) 0.5002(5) 0.5820(6) 0.059(3) Uani 1 1 d U . . C14 C 0.3983(4) 0.5056(5) 0.6268(6) 0.076(3) Uani 1 1 d U . . H14A H 0.4005 0.5522 0.6400 0.114 Uiso 1 1 calc R . . H14B H 0.4228 0.4785 0.6690 0.114 Uiso 1 1 calc R . . H14C H 0.3608 0.4895 0.6003 0.114 Uiso 1 1 calc R . . C15 C 0.4786(4) 0.5173(5) 0.6318(6) 0.080(4) Uani 1 1 d U . . H15A H 0.4927 0.5092 0.6069 0.120 Uiso 1 1 calc R . . H15B H 0.4981 0.4890 0.6734 0.120 Uiso 1 1 calc R . . H15C H 0.4840 0.5642 0.6457 0.120 Uiso 1 1 calc R . . C16 C 0.3832(4) 0.5511(5) 0.5216(6) 0.069(3) Uani 1 1 d U . . C17 C 0.3376(4) 0.5899(5) 0.4944(6) 0.055(3) Uani 1 1 d U . . C18 C 0.3255(4) 0.6271(5) 0.4400(6) 0.054(3) Uani 1 1 d U . . C19 C 0.3629(4) 0.6138(5) 0.4300(6) 0.059(3) Uani 1 1 d U . . C20 C 0.2539(4) 0.6569(5) 0.4516(5) 0.058(3) Uani 1 1 d U . . C21 C 0.2101(4) 0.6851(5) 0.4424(5) 0.061(3) Uani 1 1 d U . . C22 C 0.1354(4) 0.7167(5) 0.4501(6) 0.056(3) Uani 1 1 d U . . C23 C 0.1016(4) 0.7215(5) 0.4686(5) 0.064(3) Uani 1 1 d U . . H23 H 0.1103 0.6974 0.5074 0.077 Uiso 1 1 calc R . . C24 C 0.0567(4) 0.7609(5) 0.4305(6) 0.058(3) Uani 1 1 d U . . H24 H 0.0345 0.7660 0.4434 0.070 Uiso 1 1 calc R . . C25 C 0.0440(4) 0.7923(5) 0.3746(6) 0.068(3) Uani 1 1 d U . . H25 H 0.0114 0.8180 0.3471 0.081 Uiso 1 1 calc R . . C26 C 0.0762(4) 0.7896(5) 0.3544(5) 0.057(3) Uani 1 1 d U . . H26 H 0.0661 0.8126 0.3143 0.069 Uiso 1 1 calc R . . C27 C 0.1231(4) 0.7521(5) 0.3951(6) 0.049(3) Uani 1 1 d U . . C28 C 0.3693(5) 0.6395(5) 0.3795(6) 0.066(3) Uani 1 1 d U . . C29 C 0.3207(4) 0.6803(5) 0.3229(5) 0.074(3) Uani 1 1 d U . . H29A H 0.2877 0.6529 0.2980 0.112 Uiso 1 1 calc R . . H29B H 0.3259 0.6958 0.2901 0.112 Uiso 1 1 calc R . . H29C H 0.3169 0.7187 0.3438 0.112 Uiso 1 1 calc R . . C30 C 0.3742(4) 0.5809(5) 0.3419(6) 0.092(4) Uani 1 1 d U . . H30A H 0.3422 0.5519 0.3189 0.138 Uiso 1 1 calc R . . H30B H 0.4073 0.5551 0.3765 0.138 Uiso 1 1 calc R . . H30C H 0.3762 0.5991 0.3070 0.138 Uiso 1 1 calc R . . C31 C 0.4205(4) 0.6823(6) 0.4170(6) 0.062(3) Uani 1 1 d U . . C32 C 0.4267(4) 0.7509(6) 0.4140(6) 0.067(3) Uani 1 1 d U . . C33 C 0.4823(4) 0.7669(5) 0.4607(5) 0.063(3) Uani 1 1 d U . . C34 C 0.5105(4) 0.7059(6) 0.4895(6) 0.070(3) Uani 1 1 d U . . C35 C 0.4367(4) 0.8749(5) 0.4007(6) 0.075(3) Uani 1 1 d U . . C36 C 0.4262(4) 0.9376(6) 0.3743(6) 0.074(3) Uani 1 1 d U . . C37 C 0.3854(5) 1.0486(6) 0.3118(6) 0.084(4) Uani 1 1 d U . . C38 C 0.3484(5) 1.0962(7) 0.2675(6) 0.094(4) Uani 1 1 d U . . H38 H 0.3104 1.0870 0.2361 0.113 Uiso 1 1 calc R . . C39 C 0.3692(6) 1.1617(6) 0.2701(6) 0.100(4) Uani 1 1 d U . . H39 H 0.3452 1.1976 0.2430 0.120 Uiso 1 1 calc R . . C40 C 0.4245(5) 1.1699(6) 0.3129(6) 0.090(4) Uani 1 1 d U . . H40 H 0.4390 1.2117 0.3138 0.108 Uiso 1 1 calc R . . C41 C 0.4592(5) 1.1203(6) 0.3540(6) 0.086(4) Uani 1 1 d U . . H41 H 0.4975 1.1276 0.3827 0.103 Uiso 1 1 calc R . . C42 C 0.4402(5) 1.0591(6) 0.3551(6) 0.075(3) Uani 1 1 d U . . C43 C 0.5714(5) 0.6888(6) 0.5402(7) 0.083(4) Uani 1 1 d U . . C44 C 0.5844(4) 0.6460(5) 0.5992(6) 0.091(4) Uani 1 1 d U . . H44A H 0.5768 0.6710 0.6260 0.137 Uiso 1 1 calc R . . H44B H 0.6231 0.6334 0.6299 0.137 Uiso 1 1 calc R . . H44C H 0.5618 0.6057 0.5800 0.137 Uiso 1 1 calc R . . C45 C 0.6067(4) 0.7567(5) 0.5748(5) 0.081(4) Uani 1 1 d U . . H45A H 0.5982 0.7866 0.5378 0.121 Uiso 1 1 calc R . . H45B H 0.6458 0.7460 0.6060 0.121 Uiso 1 1 calc R . . H45C H 0.5977 0.7787 0.6015 0.121 Uiso 1 1 calc R . . N1A N 0.0000 0.3732(6) 0.2500 0.073(4) Uani 1 2 d SU . . C1A C 0.0496(5) 0.4165(6) 0.3082(6) 0.090(4) Uani 1 1 d U . . H1AA H 0.0381 0.4458 0.3287 0.108 Uiso 1 1 calc R . . H1AB H 0.0787 0.3867 0.3456 0.108 Uiso 1 1 calc R . . C2A C 0.0733(5) 0.4596(6) 0.2823(6) 0.090(4) Uani 1 1 d U . . H2AA H 0.0938 0.4314 0.2734 0.108 Uiso 1 1 calc R . . H2AB H 0.0433 0.4819 0.2381 0.108 Uiso 1 1 calc R . . C3A C 0.1103(5) 0.5104(6) 0.3366(7) 0.107(4) Uani 1 1 d U . . H3AA H 0.1363 0.5265 0.3302 0.129 Uiso 1 1 calc R . . H3AB H 0.1316 0.4900 0.3836 0.129 Uiso 1 1 calc R . . C4A C 0.0759(6) 0.5703(7) 0.3308(7) 0.157(6) Uani 1 1 d U . . H4AA H 0.0518 0.5870 0.2827 0.236 Uiso 1 1 calc R . . H4AB H 0.1005 0.6059 0.3625 0.236 Uiso 1 1 calc R . . H4AC H 0.0538 0.5553 0.3434 0.236 Uiso 1 1 calc R . . C5A C 0.0131(4) 0.3284(5) 0.2118(5) 0.075(3) Uani 1 1 d U . . H5AA H -0.0194 0.3008 0.1772 0.090 Uiso 1 1 calc R . . H5AB H 0.0200 0.3571 0.1859 0.090 Uiso 1 1 calc R . . C6A C 0.0615(5) 0.2829(6) 0.2591(6) 0.084(4) Uani 1 1 d U . . H6AA H 0.0956 0.3094 0.2871 0.101 Uiso 1 1 calc R . . H6AB H 0.0584 0.2596 0.2915 0.101 Uiso 1 1 calc R . . C7A C 0.0637(5) 0.2319(6) 0.2154(6) 0.089(4) Uani 1 1 d U . . H7AA H 0.0563 0.2548 0.1748 0.107 Uiso 1 1 calc R . . H7AB H 0.1010 0.2131 0.2438 0.107 Uiso 1 1 calc R . . C8A C 0.0249(5) 0.1779(6) 0.1904(6) 0.100(4) Uani 1 1 d U . . H8AA H 0.0320 0.1550 0.2303 0.150 Uiso 1 1 calc R . . H8AB H 0.0288 0.1463 0.1638 0.150 Uiso 1 1 calc R . . H8AC H -0.0123 0.1959 0.1603 0.150 Uiso 1 1 calc R . . C1B C 0.2973(7) 0.5976(9) 0.6696(9) 0.188(7) Uani 1 1 d U . . H1BA H 0.2917 0.6182 0.6292 0.226 Uiso 1 1 calc R . . H1BB H 0.2764 0.5554 0.6537 0.226 Uiso 1 1 calc R . . Cl1 Cl 0.5000 0.5000 0.5000 0.117(2) Uani 1 2 d SU . . Cl1B Cl 0.2738(2) 0.6512(3) 0.7005(3) 0.217(3) Uani 1 1 d U . . Cl2B Cl 0.3682(2) 0.5808(3) 0.7370(2) 0.208(3) Uani 1 1 d U . . 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 0.088(2) 0.056(2) 0.157(3) -0.0035(19) 0.102(2) -0.0098(17) S2 0.085(2) 0.058(2) 0.142(3) -0.0031(18) 0.094(2) -0.0079(17) S3 0.091(2) 0.057(2) 0.147(3) -0.0136(19) 0.100(2) -0.0166(17) S4 0.087(2) 0.059(2) 0.148(3) -0.0212(19) 0.096(2) -0.0189(17) S5 0.064(2) 0.0633(19) 0.120(3) 0.0049(18) 0.074(2) 0.0104(16) S6 0.0585(19) 0.070(2) 0.105(2) 0.0084(17) 0.0648(19) 0.0156(16) S7 0.060(2) 0.080(2) 0.105(2) 0.0083(18) 0.065(2) 0.0116(16) S8 0.063(2) 0.089(2) 0.108(2) 0.0125(19) 0.068(2) 0.0212(17) S9 0.071(2) 0.0580(19) 0.131(3) 0.0220(18) 0.078(2) 0.0168(17) S10 0.076(2) 0.0476(19) 0.131(3) 0.0096(18) 0.073(2) 0.0082(16) S11 0.078(2) 0.078(2) 0.157(3) 0.033(2) 0.075(2) 0.0062(19) S12 0.080(2) 0.061(2) 0.113(3) 0.0153(18) 0.064(2) 0.0038(17) N1 0.076(5) 0.049(6) 0.119(6) 0.013(5) 0.083(5) 0.008(4) N2 0.069(6) 0.073(6) 0.118(6) 0.022(5) 0.080(5) 0.019(5) N3 0.053(5) 0.046(5) 0.111(6) 0.011(4) 0.066(5) 0.004(4) C1 0.053(6) 0.051(7) 0.087(7) 0.003(5) 0.057(5) 0.007(5) C2 0.064(6) 0.067(7) 0.096(7) 0.010(6) 0.061(6) 0.000(5) C3 0.049(6) 0.045(6) 0.094(7) -0.009(5) 0.051(5) 0.006(5) C4 0.049(6) 0.044(6) 0.094(7) 0.001(5) 0.046(5) 0.008(5) C5 0.065(6) 0.075(7) 0.095(7) -0.006(5) 0.064(6) -0.020(5) C6 0.066(7) 0.065(7) 0.094(7) 0.000(5) 0.054(6) -0.007(5) C7 0.056(6) 0.051(6) 0.097(7) -0.018(5) 0.055(6) -0.017(5) C8 0.078(7) 0.051(7) 0.096(7) -0.001(5) 0.064(6) -0.003(5) C9 0.081(7) 0.072(7) 0.085(7) 0.007(6) 0.062(6) -0.006(6) C10 0.054(6) 0.091(8) 0.099(7) 0.006(6) 0.061(6) -0.001(5) C11 0.068(6) 0.065(7) 0.091(7) -0.002(5) 0.060(6) -0.013(5) C12 0.058(6) 0.064(7) 0.086(7) -0.002(6) 0.051(6) -0.001(5) C13 0.050(6) 0.048(6) 0.085(7) 0.012(5) 0.045(6) 0.006(5) C14 0.086(8) 0.057(7) 0.116(9) -0.004(6) 0.078(8) 0.003(6) C15 0.077(8) 0.044(7) 0.141(10) 0.018(6) 0.079(8) 0.020(6) C16 0.059(6) 0.061(7) 0.104(7) 0.005(6) 0.060(6) 0.010(5) C17 0.038(6) 0.044(6) 0.088(7) -0.008(5) 0.043(5) 0.005(5) C18 0.060(6) 0.047(6) 0.082(7) 0.005(5) 0.058(6) 0.005(5) C19 0.065(6) 0.044(6) 0.082(7) 0.026(5) 0.054(6) 0.022(5) C20 0.047(6) 0.061(6) 0.073(6) -0.002(5) 0.042(5) 0.004(5) C21 0.058(6) 0.055(6) 0.081(7) -0.009(5) 0.049(5) 0.000(5) C22 0.040(6) 0.055(6) 0.081(7) -0.008(5) 0.041(5) -0.001(5) C23 0.053(6) 0.070(7) 0.083(7) 0.007(5) 0.050(6) -0.005(5) C24 0.042(6) 0.064(6) 0.077(7) 0.006(5) 0.042(5) 0.010(5) C25 0.051(6) 0.062(7) 0.087(7) 0.002(6) 0.043(6) 0.006(5) C26 0.040(6) 0.062(6) 0.079(7) 0.000(5) 0.043(5) 0.001(5) C27 0.038(6) 0.045(6) 0.072(7) -0.004(5) 0.038(5) 0.004(5) C28 0.071(7) 0.054(6) 0.093(7) -0.004(6) 0.061(6) 0.008(6) C29 0.074(8) 0.057(7) 0.115(9) -0.005(7) 0.071(7) -0.016(6) C30 0.091(9) 0.076(8) 0.152(10) 0.003(7) 0.098(8) 0.004(7) C31 0.047(6) 0.067(7) 0.099(7) 0.006(6) 0.059(6) -0.003(5) C32 0.052(6) 0.076(7) 0.097(7) -0.003(6) 0.058(6) 0.000(5) C33 0.057(6) 0.062(7) 0.088(7) 0.006(5) 0.055(6) 0.010(5) C34 0.052(6) 0.089(7) 0.092(7) -0.002(6) 0.056(6) 0.016(6) C35 0.083(7) 0.058(7) 0.104(7) 0.022(6) 0.069(6) 0.009(5) C36 0.074(7) 0.075(7) 0.094(7) 0.010(6) 0.064(6) 0.008(6) C37 0.075(7) 0.067(7) 0.102(8) 0.035(6) 0.053(6) 0.020(6) C38 0.080(7) 0.108(8) 0.103(8) 0.013(6) 0.062(6) -0.018(6) C39 0.108(8) 0.091(8) 0.109(8) 0.026(6) 0.073(7) 0.017(7) C40 0.078(7) 0.092(8) 0.099(8) 0.007(6) 0.055(6) -0.026(6) C41 0.077(7) 0.079(7) 0.101(8) 0.016(6) 0.056(6) 0.007(6) C42 0.065(7) 0.068(7) 0.100(8) 0.010(6) 0.055(6) -0.006(6) C43 0.074(7) 0.078(7) 0.113(8) 0.010(6) 0.066(6) -0.001(6) C44 0.083(8) 0.081(8) 0.145(10) 0.037(8) 0.090(8) 0.033(7) C45 0.072(8) 0.078(8) 0.116(9) 0.001(7) 0.071(7) 0.025(6) N1A 0.073(7) 0.076(7) 0.081(8) 0.000 0.054(6) 0.000 C1A 0.097(8) 0.076(7) 0.092(7) -0.008(6) 0.058(6) -0.006(6) C2A 0.096(8) 0.088(7) 0.083(7) -0.005(6) 0.057(6) -0.024(6) C3A 0.100(8) 0.094(8) 0.119(8) -0.023(7) 0.066(6) -0.014(7) C4A 0.146(12) 0.090(10) 0.179(13) -0.024(9) 0.077(10) -0.004(9) C5A 0.089(7) 0.063(7) 0.087(7) -0.010(5) 0.063(6) -0.013(6) C6A 0.083(7) 0.085(7) 0.094(7) -0.008(6) 0.061(6) -0.008(6) C7A 0.086(7) 0.102(8) 0.102(7) -0.019(6) 0.070(6) 0.000(6) C8A 0.086(9) 0.082(8) 0.142(10) -0.039(8) 0.077(8) -0.024(7) C1B 0.184(11) 0.203(12) 0.188(11) 0.013(8) 0.124(9) 0.014(8) Cl1 0.122(4) 0.055(3) 0.269(6) 0.051(3) 0.169(4) 0.036(3) Cl1B 0.216(5) 0.299(7) 0.225(5) 0.132(5) 0.183(5) 0.132(5) Cl2B 0.184(5) 0.308(7) 0.146(4) 0.031(4) 0.112(4) 0.100(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C5 1.785(10) . ? S1 C2 1.804(10) . ? S2 C3 1.724(10) . ? S2 C5 1.746(11) . ? S3 C7 1.743(11) . ? S3 C6 1.759(11) . ? S4 C6 1.756(11) . ? S4 C12 1.776(11) . ? S5 C20 1.734(10) . ? S5 C17 1.756(10) . ? S6 C18 1.735(10) . ? S6 C20 1.756(10) . ? S7 C21 1.742(10) . ? S7 C22 1.769(10) . ? S8 C27 1.742(9) . ? S8 C21 1.751(10) . ? S9 C35 1.765(11) . ? S9 C32 1.758(11) . ? S10 C35 1.729(11) . ? S10 C33 1.740(10) . ? S11 C36 1.738(11) . ? S11 C37 1.751(12) . ? S12 C42 1.699(12) . ? S12 C36 1.782(11) . ? N1 C1 1.347(11) . ? N1 C4 1.402(11) . ? N2 C19 1.360(11) . ? N2 C16 1.396(12) . ? N3 C31 1.346(11) . ? N3 C34 1.367(12) . ? C1 C2 1.368(12) . ? C1 C43 1.516(14) 5_666 ? C2 C3 1.386(12) . ? C3 C4 1.373(12) . ? C4 C13 1.525(13) . ? C5 C6 1.350(12) . ? C7 C12 1.367(13) . ? C7 C8 1.381(12) . ? C8 C9 1.352(13) . ? C9 C10 1.356(13) . ? C10 C11 1.408(13) . ? C11 C12 1.394(13) . ? C13 C14 1.521(12) . ? C13 C16 1.544(13) . ? C13 C15 1.586(13) . ? C16 C17 1.384(12) . ? C17 C18 1.370(12) . ? C18 C19 1.385(12) . ? C19 C28 1.487(13) . ? C20 C21 1.379(12) . ? C22 C27 1.359(12) . ? C22 C23 1.414(12) . ? C23 C24 1.354(12) . ? C24 C25 1.333(12) . ? C25 C26 1.398(12) . ? C26 C27 1.375(11) . ? C28 C31 1.522(13) . ? C28 C29 1.505(12) . ? C28 C30 1.571(13) . ? C31 C32 1.401(13) . ? C32 C33 1.399(12) . ? C33 C34 1.414(13) . ? C34 C43 1.530(14) . ? C35 C36 1.360(12) . ? C37 C38 1.363(14) . ? C37 C42 1.358(13) . ? C38 C39 1.455(15) . ? C39 C40 1.365(14) . ? C40 C41 1.347(14) . ? C41 C42 1.376(13) . ? C43 C44 1.512(14) . ? C43 C1 1.516(14) 5_666 ? C43 C45 1.622(14) . ? N1A C5A 1.544(11) 2 ? N1A C5A 1.544(11) . ? N1A C1A 1.557(12) . ? N1A C1A 1.557(11) 2 ? C1A C2A 1.530(14) . ? C2A C3A 1.491(14) . ? C3A C4A 1.569(15) . ? C5A C6A 1.509(13) . ? C6A C7A 1.526(13) . ? C7A C8A 1.452(13) . ? C1B Cl1B 1.745(18) . ? C1B Cl2B 1.785(18) . ? 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 C5 S1 C2 92.6(5) . . ? C3 S2 C5 95.5(5) . . ? C7 S3 C6 95.6(5) . . ? C6 S4 C12 94.7(5) . . ? C20 S5 C17 93.0(5) . . ? C18 S6 C20 93.5(5) . . ? C21 S7 C22 94.6(5) . . ? C27 S8 C21 95.5(5) . . ? C35 S9 C32 93.1(5) . . ? C35 S10 C33 92.4(5) . . ? C36 S11 C37 93.8(6) . . ? C42 S12 C36 95.6(6) . . ? C1 N1 C4 111.5(8) . . ? C19 N2 C16 113.6(9) . . ? C31 N3 C34 112.4(9) . . ? N1 C1 C2 104.3(9) . . ? N1 C1 C43 120.4(10) . 5_666 ? C2 C1 C43 134.9(11) . 5_666 ? C1 C2 C3 112.1(10) . . ? C1 C2 S1 131.3(10) . . ? C3 C2 S1 116.6(9) . . ? C4 C3 C2 105.7(9) . . ? C4 C3 S2 136.3(9) . . ? C2 C3 S2 118.0(9) . . ? C3 C4 N1 106.4(9) . . ? C3 C4 C13 131.1(10) . . ? N1 C4 C13 122.5(10) . . ? C6 C5 S2 124.3(8) . . ? C6 C5 S1 118.9(8) . . ? S2 C5 S1 116.7(6) . . ? C5 C6 S3 122.3(9) . . ? C5 C6 S4 122.3(8) . . ? S3 C6 S4 115.3(6) . . ? C12 C7 C8 118.5(10) . . ? C12 C7 S3 117.3(8) . . ? C8 C7 S3 124.2(9) . . ? C9 C8 C7 121.3(11) . . ? C8 C9 C10 118.8(11) . . ? C9 C10 C11 124.0(10) . . ? C12 C11 C10 113.9(10) . . ? C7 C12 C11 123.5(10) . . ? C7 C12 S4 116.8(9) . . ? C11 C12 S4 119.6(9) . . ? C14 C13 C4 110.7(8) . . ? C14 C13 C16 109.9(8) . . ? C4 C13 C16 110.3(9) . . ? C14 C13 C15 106.1(9) . . ? C4 C13 C15 109.9(8) . . ? C16 C13 C15 109.9(8) . . ? C17 C16 N2 103.0(9) . . ? C17 C16 C13 133.3(11) . . ? N2 C16 C13 123.7(9) . . ? C18 C17 C16 109.7(9) . . ? C18 C17 S5 117.9(8) . . ? C16 C17 S5 132.4(10) . . ? C19 C18 C17 109.8(9) . . ? C19 C18 S6 132.7(9) . . ? C17 C18 S6 117.5(8) . . ? N2 C19 C18 103.9(9) . . ? N2 C19 C28 123.4(10) . . ? C18 C19 C28 132.7(10) . . ? C21 C20 S5 121.3(8) . . ? C21 C20 S6 120.6(8) . . ? S5 C20 S6 118.1(6) . . ? C20 C21 S7 122.3(8) . . ? C20 C21 S8 122.2(8) . . ? S7 C21 S8 115.4(6) . . ? C27 C22 C23 120.1(9) . . ? C27 C22 S7 117.2(8) . . ? C23 C22 S7 122.7(9) . . ? C24 C23 C22 119.4(10) . . ? C23 C24 C25 119.4(10) . . ? C24 C25 C26 123.4(10) . . ? C27 C26 C25 117.1(10) . . ? C22 C27 C26 120.5(9) . . ? C22 C27 S8 116.8(8) . . ? C26 C27 S8 122.7(9) . . ? C19 C28 C31 110.3(9) . . ? C19 C28 C29 111.5(9) . . ? C31 C28 C29 108.9(9) . . ? C19 C28 C30 111.1(9) . . ? C31 C28 C30 108.4(9) . . ? C29 C28 C30 106.5(9) . . ? N3 C31 C32 105.8(9) . . ? N3 C31 C28 123.4(10) . . ? C32 C31 C28 130.9(10) . . ? C31 C32 C33 109.1(9) . . ? C31 C32 S9 135.9(9) . . ? C33 C32 S9 114.9(9) . . ? C34 C33 C32 106.2(9) . . ? C34 C33 S10 134.0(9) . . ? C32 C33 S10 119.6(8) . . ? N3 C34 C33 106.3(9) . . ? N3 C34 C43 121.3(10) . . ? C33 C34 C43 132.3(11) . . ? C36 C35 S10 121.2(9) . . ? C36 C35 S9 120.3(9) . . ? S10 C35 S9 118.4(6) . . ? C35 C36 S11 124.7(9) . . ? C35 C36 S12 120.3(9) . . ? S11 C36 S12 115.0(6) . . ? C38 C37 C42 122.7(11) . . ? C38 C37 S11 118.5(10) . . ? C42 C37 S11 118.8(9) . . ? C37 C38 C39 117.7(12) . . ? C40 C39 C38 117.8(12) . . ? C41 C40 C39 121.8(12) . . ? C40 C41 C42 121.2(12) . . ? C37 C42 C41 118.7(11) . . ? C37 C42 S12 116.8(9) . . ? C41 C42 S12 124.5(10) . . ? C44 C43 C1 110.7(10) . 5_666 ? C44 C43 C34 110.4(9) . . ? C1 C43 C34 111.9(10) 5_666 . ? C44 C43 C45 107.2(10) . . ? C1 C43 C45 107.1(9) 5_666 . ? C34 C43 C45 109.4(10) . . ? C5A N1A C5A 108.7(11) 2 . ? C5A N1A C1A 105.3(6) 2 . ? C5A N1A C1A 112.7(6) . . ? C5A N1A C1A 112.7(6) 2 2 ? C5A N1A C1A 105.3(6) . 2 ? C1A N1A C1A 112.1(12) . 2 ? C2A C1A N1A 113.8(9) . . ? C3A C2A C1A 108.8(10) . . ? C2A C3A C4A 109.8(11) . . ? C6A C5A N1A 114.5(8) . . ? C7A C6A C5A 109.8(9) . . ? C8A C7A C6A 113.2(10) . . ? Cl1B C1B Cl2B 110.0(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 C4 N1 C1 C2 -1.6(11) . . . . ? C4 N1 C1 C43 -175.2(9) . . . 5_666 ? N1 C1 C2 C3 1.8(12) . . . . ? C43 C1 C2 C3 174.0(11) 5_666 . . . ? N1 C1 C2 S1 -176.6(8) . . . . ? C43 C1 C2 S1 -4(2) 5_666 . . . ? C5 S1 C2 C1 -175.9(11) . . . . ? C5 S1 C2 C3 5.7(9) . . . . ? C1 C2 C3 C4 -1.4(12) . . . . ? S1 C2 C3 C4 177.3(7) . . . . ? C1 C2 C3 S2 178.7(7) . . . . ? S1 C2 C3 S2 -2.6(12) . . . . ? C5 S2 C3 C4 178.1(12) . . . . ? C5 S2 C3 C2 -2.1(9) . . . . ? C2 C3 C4 N1 0.4(11) . . . . ? S2 C3 C4 N1 -179.8(8) . . . . ? C2 C3 C4 C13 -177.8(10) . . . . ? S2 C3 C4 C13 2.0(19) . . . . ? C1 N1 C4 C3 0.8(12) . . . . ? C1 N1 C4 C13 179.2(9) . . . . ? C3 S2 C5 C6 -177.5(10) . . . . ? C3 S2 C5 S1 6.2(7) . . . . ? C2 S1 C5 C6 176.3(9) . . . . ? C2 S1 C5 S2 -7.1(7) . . . . ? S2 C5 C6 S3 -176.9(6) . . . . ? S1 C5 C6 S3 -0.6(14) . . . . ? S2 C5 C6 S4 -0.5(15) . . . . ? S1 C5 C6 S4 175.8(6) . . . . ? C7 S3 C6 C5 174.2(10) . . . . ? C7 S3 C6 S4 -2.4(7) . . . . ? C12 S4 C6 C5 -172.6(10) . . . . ? C12 S4 C6 S3 4.0(7) . . . . ? C6 S3 C7 C12 -1.0(9) . . . . ? C6 S3 C7 C8 179.9(10) . . . . ? C12 C7 C8 C9 0.1(16) . . . . ? S3 C7 C8 C9 179.1(9) . . . . ? C7 C8 C9 C10 -0.4(17) . . . . ? C8 C9 C10 C11 0.5(17) . . . . ? C9 C10 C11 C12 -0.3(16) . . . . ? C8 C7 C12 C11 0.2(16) . . . . ? S3 C7 C12 C11 -178.9(8) . . . . ? C8 C7 C12 S4 -176.8(8) . . . . ? S3 C7 C12 S4 4.1(12) . . . . ? C10 C11 C12 C7 -0.1(15) . . . . ? C10 C11 C12 S4 176.8(7) . . . . ? C6 S4 C12 C7 -4.8(9) . . . . ? C6 S4 C12 C11 178.1(9) . . . . ? C3 C4 C13 C14 3.7(15) . . . . ? N1 C4 C13 C14 -174.3(9) . . . . ? C3 C4 C13 C16 -118.1(12) . . . . ? N1 C4 C13 C16 63.9(12) . . . . ? C3 C4 C13 C15 120.6(12) . . . . ? N1 C4 C13 C15 -57.4(12) . . . . ? C19 N2 C16 C17 0.0(12) . . . . ? C19 N2 C16 C13 180.0(9) . . . . ? C14 C13 C16 C17 -13.3(16) . . . . ? C4 C13 C16 C17 109.0(13) . . . . ? C15 C13 C16 C17 -129.7(12) . . . . ? C14 C13 C16 N2 166.7(9) . . . . ? C4 C13 C16 N2 -71.0(12) . . . . ? C15 C13 C16 N2 50.3(13) . . . . ? N2 C16 C17 C18 0.0(11) . . . . ? C13 C16 C17 C18 180.0(11) . . . . ? N2 C16 C17 S5 179.4(8) . . . . ? C13 C16 C17 S5 -0.6(18) . . . . ? C20 S5 C17 C18 -0.7(9) . . . . ? C20 S5 C17 C16 180.0(10) . . . . ? C16 C17 C18 C19 0.0(12) . . . . ? S5 C17 C18 C19 -179.5(7) . . . . ? C16 C17 C18 S6 -179.8(7) . . . . ? S5 C17 C18 S6 0.7(11) . . . . ? C20 S6 C18 C19 179.9(11) . . . . ? C20 S6 C18 C17 -0.4(9) . . . . ? C16 N2 C19 C18 0.0(12) . . . . ? C16 N2 C19 C28 179.9(9) . . . . ? C17 C18 C19 N2 0.0(12) . . . . ? S6 C18 C19 N2 179.7(8) . . . . ? C17 C18 C19 C28 -179.8(11) . . . . ? S6 C18 C19 C28 -0.1(19) . . . . ? C17 S5 C20 C21 -179.3(9) . . . . ? C17 S5 C20 S6 0.4(6) . . . . ? C18 S6 C20 C21 179.6(8) . . . . ? C18 S6 C20 S5 -0.1(7) . . . . ? S5 C20 C21 S7 2.5(13) . . . . ? S6 C20 C21 S7 -177.2(5) . . . . ? S5 C20 C21 S8 178.9(5) . . . . ? S6 C20 C21 S8 -0.8(12) . . . . ? C22 S7 C21 C20 -177.6(9) . . . . ? C22 S7 C21 S8 5.8(6) . . . . ? C27 S8 C21 C20 176.8(9) . . . . ? C27 S8 C21 S7 -6.6(6) . . . . ? C21 S7 C22 C27 -2.5(9) . . . . ? C21 S7 C22 C23 178.4(9) . . . . ? C27 C22 C23 C24 1.0(15) . . . . ? S7 C22 C23 C24 -179.9(8) . . . . ? C22 C23 C24 C25 2.5(15) . . . . ? C23 C24 C25 C26 -3.1(16) . . . . ? C24 C25 C26 C27 0.0(15) . . . . ? C23 C22 C27 C26 -4.1(15) . . . . ? S7 C22 C27 C26 176.7(7) . . . . ? C23 C22 C27 S8 177.5(7) . . . . ? S7 C22 C27 S8 -1.7(11) . . . . ? C25 C26 C27 C22 3.6(14) . . . . ? C25 C26 C27 S8 -178.1(7) . . . . ? C21 S8 C27 C22 4.9(9) . . . . ? C21 S8 C27 C26 -173.5(8) . . . . ? N2 C19 C28 C31 -68.7(13) . . . . ? C18 C19 C28 C31 111.1(13) . . . . ? N2 C19 C28 C29 170.1(9) . . . . ? C18 C19 C28 C29 -10.1(17) . . . . ? N2 C19 C28 C30 51.5(14) . . . . ? C18 C19 C28 C30 -128.7(12) . . . . ? C34 N3 C31 C32 1.6(12) . . . . ? C34 N3 C31 C28 -179.0(9) . . . . ? C19 C28 C31 N3 69.3(12) . . . . ? C29 C28 C31 N3 -168.0(9) . . . . ? C30 C28 C31 N3 -52.5(13) . . . . ? C19 C28 C31 C32 -111.4(13) . . . . ? C29 C28 C31 C32 11.3(16) . . . . ? C30 C28 C31 C32 126.8(12) . . . . ? N3 C31 C32 C33 -3.1(12) . . . . ? C28 C31 C32 C33 177.5(10) . . . . ? N3 C31 C32 S9 -180.0(8) . . . . ? C28 C31 C32 S9 0.7(19) . . . . ? C35 S9 C32 C31 -174.4(12) . . . . ? C35 S9 C32 C33 8.9(9) . . . . ? C31 C32 C33 C34 3.5(12) . . . . ? S9 C32 C33 C34 -179.0(7) . . . . ? C31 C32 C33 S10 179.7(7) . . . . ? S9 C32 C33 S10 -2.8(11) . . . . ? C35 S10 C33 C34 169.8(11) . . . . ? C35 S10 C33 C32 -5.2(9) . . . . ? C31 N3 C34 C33 0.5(12) . . . . ? C31 N3 C34 C43 -178.4(9) . . . . ? C32 C33 C34 N3 -2.4(11) . . . . ? S10 C33 C34 N3 -177.9(8) . . . . ? C32 C33 C34 C43 176.4(11) . . . . ? S10 C33 C34 C43 0.9(19) . . . . ? C33 S10 C35 C36 -171.7(10) . . . . ? C33 S10 C35 S9 11.7(7) . . . . ? C32 S9 C35 C36 170.4(9) . . . . ? C32 S9 C35 S10 -13.1(7) . . . . ? S10 C35 C36 S11 -176.3(6) . . . . ? S9 C35 C36 S11 0.1(14) . . . . ? S10 C35 C36 S12 1.7(14) . . . . ? S9 C35 C36 S12 178.2(6) . . . . ? C37 S11 C36 C35 177.6(10) . . . . ? C37 S11 C36 S12 -0.5(7) . . . . ? C42 S12 C36 C35 -178.9(9) . . . . ? C42 S12 C36 S11 -0.7(7) . . . . ? C36 S11 C37 C38 179.4(10) . . . . ? C36 S11 C37 C42 1.9(11) . . . . ? C42 C37 C38 C39 -3.2(19) . . . . ? S11 C37 C38 C39 179.5(9) . . . . ? C37 C38 C39 C40 4.8(18) . . . . ? C38 C39 C40 C41 -2.9(19) . . . . ? C39 C40 C41 C42 -1(2) . . . . ? C38 C37 C42 C41 -0.4(19) . . . . ? S11 C37 C42 C41 176.9(9) . . . . ? C38 C37 C42 S12 179.8(10) . . . . ? S11 C37 C42 S12 -2.8(14) . . . . ? C40 C41 C42 C37 2.5(19) . . . . ? C40 C41 C42 S12 -177.7(10) . . . . ? C36 S12 C42 C37 2.1(11) . . . . ? C36 S12 C42 C41 -177.7(11) . . . . ? N3 C34 C43 C44 -51.7(14) . . . . ? C33 C34 C43 C44 129.7(12) . . . . ? N3 C34 C43 C1 72.1(13) . . . 5_666 ? C33 C34 C43 C1 -106.6(14) . . . 5_666 ? N3 C34 C43 C45 -169.4(9) . . . . ? C33 C34 C43 C45 11.9(16) . . . . ? C5A N1A C1A C2A 173.7(9) 2 . . . ? C5A N1A C1A C2A 55.3(13) . . . . ? C1A N1A C1A C2A -63.3(8) 2 . . . ? N1A C1A C2A C3A 165.9(10) . . . . ? C1A C2A C3A C4A -81.2(13) . . . . ? C5A N1A C5A C6A -60.5(7) 2 . . . ? C1A N1A C5A C6A 55.8(12) . . . . ? C1A N1A C5A C6A 178.4(9) 2 . . . ? N1A C5A C6A C7A 168.8(9) . . . . ? C5A C6A C7A C8A -77.9(13) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N Cl1 0.88 2.40 3.272(8) 168 . N2 H2N Cl1 0.88 2.40 3.279(8) 178 . N3 H3N Cl1 0.88 2.38 3.261(8) 179 . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.499 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.092 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.304 0.041 0.410 192 57 ' ' 2 0.304 -0.041 0.910 192 57 ' ' 3 0.696 -0.041 0.590 192 56 ' ' 4 0.696 0.041 1.090 192 54 ' ' 5 0.000 0.094 0.750 7 1 ' ' 6 0.500 0.187 0.250 7 1 ' ' 7 0.000 0.312 0.750 7 1 ' ' 8 0.196 0.459 0.590 192 56 ' ' 9 0.804 0.459 0.910 192 57 ' ' 10 0.196 0.541 0.090 192 54 ' ' 11 0.500 0.406 0.250 7 2 ' ' 12 0.804 0.541 0.410 192 57 ' ' 13 0.500 0.594 0.750 7 1 ' ' 14 0.000 0.687 0.250 7 1 ' ' 15 0.500 0.812 0.750 7 1 ' ' 16 0.000 0.906 0.250 7 2 ' ' _platon_squeeze_details ; ; data_js417 _database_code_depnum_ccdc_archive 'CCDC 868897' #TrackingRef 'js417.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C75 H55 N5 S20, C24 H52 N 1+, Cl 1-, 2 C5 H12, C H2 Cl2' _chemical_formula_sum 'C110 H127 Cl3 N6 S20' _chemical_formula_weight 2280.73 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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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 Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 28.3045(9) _cell_length_b 24.6469(8) _cell_length_c 17.5652(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12253.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4800 _exptl_absorpt_coefficient_mu 4.215 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-Axis Spider with Image Plate' _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 10554 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0710 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 6.72 _diffrn_reflns_theta_max 70.00 _reflns_number_total 10554 _reflns_number_gt 5599 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _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. A large region of disordered solvent was found near 1/2, 1/4, 3/4. The solvent molecules in this location could not be modeled well. As a result, the utility SQUEEZE (Sluis and Spek, 1990) in PLATON98 (Spek, 1998). PLATON98 was used as incorporated in WinGX (Farrugia, 1999). For the purposes of calculating F(000), the linear absorption coeffient and the crystal density, it was assumed that this solvent region contained 0ne molecule of n-pentane and one molecule of dichloromethane. The cation was disordered around the crystallographic mirror plane of symmetry at y = 1/4. The disorder was modeled using a PART -1 instruction in shelxl and including all the atoms of the cation. The atoms were assigned a site occupancy factor of 1/2 and refined with the C-N, C-C bond lengths and angles to be essentially equal. One benzene ring on the ttf-calixpyrrole was disorded. The disorder was modeled by assigning the variable x to the site occupancy factors for one component of the disorder given by atoms, C35, C36 and C378. The factor (1-x) was assigned to the alternate conformation composed of atoms C35a, C36a and C37a. A common isotropic displacement parameter was refined for these atoms while refining x. In this way, the site occupancy factor for the major component composed of atoms C35, C36 and C37 refined to 63(2)%. ; _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^)+(0.0789P)^2^+1.9557P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10554 _refine_ls_number_parameters 774 _refine_ls_number_restraints 1021 _refine_ls_R_factor_all 0.1520 _refine_ls_R_factor_gt 0.0874 _refine_ls_wR_factor_ref 0.2662 _refine_ls_wR_factor_gt 0.2161 _refine_ls_goodness_of_fit_ref 1.651 _refine_ls_restrained_S_all 1.630 _refine_ls_shift/su_max 0.032 _refine_ls_shift/su_mean 0.004 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 0.21600(5) 0.35282(8) 0.43959(9) 0.0573(5) Uani 1 1 d U . . S2 S 0.22096(6) 0.44289(8) 0.32593(10) 0.0596(5) Uani 1 1 d U . . S3 S 0.31032(6) 0.49299(8) 0.41119(11) 0.0687(6) Uani 1 1 d U . . S4 S 0.30752(6) 0.40473(8) 0.52554(10) 0.0658(6) Uani 1 1 d U . . S5 S 0.07441(6) 0.50349(8) 0.26003(10) 0.0633(6) Uani 1 1 d U . . S6 S -0.02546(6) 0.47738(8) 0.21952(10) 0.0623(6) Uani 1 1 d U . . S7 S -0.06230(6) 0.54646(9) 0.35933(11) 0.0743(6) Uani 1 1 d U . . S8 S 0.03502(6) 0.56404(9) 0.41529(10) 0.0677(6) Uani 1 1 d U . . S9 S -0.03458(5) 0.31086(8) 0.30164(9) 0.0552(5) Uani 1 1 d U . . S10 S -0.08646(6) 0.31036(8) 0.46566(10) 0.0670(6) Uani 1 1 d U . . Cl1 Cl 0.09702(7) 0.2500 0.11249(13) 0.0598(7) Uani 1 2 d SU . . N1 N 0.14459(17) 0.3204(2) 0.2518(3) 0.0515(15) Uani 1 1 d U . . H1 H 0.1260 0.3022 0.2208 0.062 Uiso 1 1 calc R . . N2 N 0.06487(17) 0.3725(2) 0.1318(3) 0.0543(15) Uani 1 1 d U . . H2 H 0.0748 0.3446 0.1049 0.065 Uiso 1 1 calc R . . N3 N -0.0198(2) 0.2500 0.0960(4) 0.052(2) Uani 1 2 d SU . . H3A H -0.0169 0.2500 0.0462 0.063 Uiso 1 2 calc SR . . C1 C 0.1591(2) 0.3012(3) 0.3229(4) 0.0507(18) Uani 1 1 d U . . C2 C 0.1883(2) 0.3406(3) 0.3519(3) 0.0477(17) Uani 1 1 d U . . C3 C 0.1908(2) 0.3843(3) 0.2982(4) 0.0514(18) Uani 1 1 d U . . C4 C 0.1628(2) 0.3714(3) 0.2355(4) 0.0526(18) Uani 1 1 d U . . C5 C 0.2449(2) 0.4115(3) 0.4063(3) 0.0523(18) Uani 1 1 d U . . C6 C 0.2831(2) 0.4331(3) 0.4420(4) 0.0555(18) Uani 1 1 d U . . C7 C 0.3604(2) 0.4840(3) 0.4690(4) 0.062(2) Uani 1 1 d U . . C8 C 0.3994(3) 0.5200(3) 0.4639(4) 0.070(2) Uani 1 1 d U . . H8 H 0.3995 0.5492 0.4287 0.084 Uiso 1 1 calc R . . C9 C 0.4369(3) 0.5110(4) 0.5116(5) 0.074(2) Uani 1 1 d U . . H9 H 0.4637 0.5342 0.5087 0.088 Uiso 1 1 calc R . . C10 C 0.4367(3) 0.4690(4) 0.5638(4) 0.070(2) Uani 1 1 d U . . H10 H 0.4631 0.4638 0.5962 0.084 Uiso 1 1 calc R . . C11 C 0.3979(2) 0.4343(3) 0.5691(4) 0.062(2) Uani 1 1 d U . . H11 H 0.3977 0.4054 0.6050 0.075 Uiso 1 1 calc R . . C12 C 0.3597(2) 0.4425(3) 0.5215(4) 0.0567(19) Uani 1 1 d U . . C13 C 0.1480(2) 0.4028(3) 0.1666(4) 0.0528(18) Uani 1 1 d U . . C14 C 0.1635(2) 0.3751(3) 0.0912(3) 0.062(2) Uani 1 1 d U . . H14A H 0.1980 0.3771 0.0863 0.094 Uiso 1 1 calc R . . H14B H 0.1488 0.3937 0.0480 0.094 Uiso 1 1 calc R . . H14C H 0.1536 0.3370 0.0917 0.094 Uiso 1 1 calc R . . C15 C 0.1705(2) 0.4598(3) 0.1691(4) 0.061(2) Uani 1 1 d U . . H15A H 0.1603 0.4786 0.2154 0.091 Uiso 1 1 calc R . . H15B H 0.1605 0.4805 0.1243 0.091 Uiso 1 1 calc R . . H15C H 0.2050 0.4563 0.1692 0.091 Uiso 1 1 calc R . . C16 C 0.0943(2) 0.4093(3) 0.1694(4) 0.0542(18) Uani 1 1 d U . . C17 C 0.0650(2) 0.4454(3) 0.2049(4) 0.0512(18) Uani 1 1 d U . . C18 C 0.0176(2) 0.4323(3) 0.1869(3) 0.0490(17) Uani 1 1 d U . . C19 C 0.0177(2) 0.3863(3) 0.1428(3) 0.0491(17) Uani 1 1 d U . . C20 C 0.0139(2) 0.5084(3) 0.2840(4) 0.0583(19) Uani 1 1 d U . . C21 C -0.0012(2) 0.5360(3) 0.3442(4) 0.0584(19) Uani 1 1 d U . . C22 C -0.0560(2) 0.5664(3) 0.4551(4) 0.0598(19) Uani 1 1 d U . . C23 C -0.0945(2) 0.5749(3) 0.5037(4) 0.062(2) Uani 1 1 d U . . H23 H -0.1258 0.5705 0.4853 0.074 Uiso 1 1 calc R . . C24 C -0.0870(2) 0.5893(3) 0.5773(4) 0.061(2) Uani 1 1 d U . . H24 H -0.1130 0.5951 0.6106 0.073 Uiso 1 1 calc R . . C25 C -0.0412(2) 0.5955(3) 0.6036(4) 0.062(2) Uani 1 1 d U . . H25 H -0.0361 0.6060 0.6550 0.075 Uiso 1 1 calc R . . C26 C -0.0023(2) 0.5868(3) 0.5561(4) 0.0595(19) Uani 1 1 d U . . H26 H 0.0290 0.5905 0.5751 0.071 Uiso 1 1 calc R . . C27 C -0.0102(2) 0.5727(3) 0.4815(4) 0.0525(18) Uani 1 1 d U . . C28 C -0.0208(2) 0.3527(3) 0.1052(3) 0.0489(17) Uani 1 1 d U . . C29 C -0.0109(2) 0.3500(3) 0.0193(3) 0.061(2) Uani 1 1 d U . . H29A H 0.0194 0.3318 0.0105 0.091 Uiso 1 1 calc R . . H29B H -0.0096 0.3869 -0.0015 0.091 Uiso 1 1 calc R . . H29C H -0.0362 0.3297 -0.0060 0.091 Uiso 1 1 calc R . . C30 C -0.0686(2) 0.3805(3) 0.1177(4) 0.0598(19) Uani 1 1 d U . . H30A H -0.0931 0.3613 0.0890 0.090 Uiso 1 1 calc R . . H30B H -0.0668 0.4182 0.1001 0.090 Uiso 1 1 calc R . . H30C H -0.0765 0.3799 0.1720 0.090 Uiso 1 1 calc R . . C31 C -0.0223(2) 0.2961(3) 0.1394(4) 0.0491(17) Uani 1 1 d U . . C32 C -0.02898(19) 0.2784(2) 0.2119(3) 0.0468(17) Uani 1 1 d U . . C33 C -0.0506(3) 0.2500 0.3490(5) 0.046(2) Uani 1 2 d SU . . C34 C -0.0717(3) 0.2500 0.4169(5) 0.048(2) Uani 1 2 d SU . . C35 C -0.1180(5) 0.2775(9) 0.5387(11) 0.068(3) Uani 0.63 1 d PU . 1 C36 C -0.1393(4) 0.3074(6) 0.5946(7) 0.076(3) Uani 0.63 1 d PU . 1 H36A H -0.1385 0.3459 0.5950 0.091 Uiso 0.63 1 calc PR . 1 C37 C -0.1627(4) 0.2771(4) 0.6518(7) 0.080(3) Uani 0.63 1 d PU . 1 H37A H -0.1788 0.2958 0.6913 0.096 Uiso 0.63 1 calc PR . 1 C35A C -0.1037(9) 0.2787(16) 0.549(2) 0.069(4) Uani 0.37 1 d PU . 2 C36A C -0.1124(7) 0.3055(10) 0.6177(12) 0.072(3) Uani 0.37 1 d PU . 2 H36B H -0.1098 0.3439 0.6196 0.087 Uiso 0.37 1 calc PR . 2 C37A C -0.1245(7) 0.2781(7) 0.6815(11) 0.075(4) Uani 0.37 1 d PU . 2 H37B H -0.1330 0.2974 0.7263 0.090 Uiso 0.37 1 calc PR . 2 C38 C 0.1385(3) 0.2500 0.3560(5) 0.051(2) Uani 1 2 d SU . . C39 C 0.0847(3) 0.2500 0.3448(5) 0.055(3) Uani 1 2 d SU . . H39A H 0.0708 0.2197 0.3730 0.083 Uiso 0.50 1 calc PR . . H39B H 0.0774 0.2461 0.2905 0.083 Uiso 0.50 1 calc PR . . H39C H 0.0715 0.2842 0.3636 0.083 Uiso 0.50 1 calc PR . . C40 C 0.1491(3) 0.2500 0.4428(5) 0.057(3) Uani 1 2 d SU . . H40A H 0.1290 0.2231 0.4681 0.085 Uiso 0.50 1 calc PR . . H40B H 0.1425 0.2861 0.4638 0.085 Uiso 0.50 1 calc PR . . H40C H 0.1823 0.2408 0.4513 0.085 Uiso 0.50 1 calc PR . . N1A N 0.3088(2) 0.2522(11) 0.2478(4) 0.056(2) Uani 0.50 1 d PDU A -1 C1A C 0.2974(3) 0.2583(12) 0.3304(4) 0.050(4) Uani 0.50 1 d PDU A -1 H1A1 H 0.2763 0.2281 0.3457 0.060 Uiso 0.50 1 calc PR A -1 H1A2 H 0.2796 0.2925 0.3375 0.060 Uiso 0.50 1 calc PR A -1 C2A C 0.3402(3) 0.2589(10) 0.3839(4) 0.058(4) Uani 0.50 1 d PDU A -1 H2A1 H 0.3586 0.2925 0.3754 0.070 Uiso 0.50 1 calc PR A -1 H2A2 H 0.3609 0.2276 0.3719 0.070 Uiso 0.50 1 calc PR A -1 C3A C 0.3253(3) 0.2559(15) 0.4680(4) 0.063(4) Uani 0.50 1 d PDU A -1 H3A1 H 0.3038 0.2866 0.4791 0.076 Uiso 0.50 1 calc PR A -1 H3A2 H 0.3074 0.2219 0.4762 0.076 Uiso 0.50 1 calc PR A -1 C4A C 0.3661(3) 0.2576(10) 0.5235(4) 0.075(4) Uani 0.50 1 d PDU A -1 H4A1 H 0.3778 0.2954 0.5270 0.090 Uiso 0.50 1 calc PR A -1 H4A2 H 0.3922 0.2351 0.5032 0.090 Uiso 0.50 1 calc PR A -1 C5A C 0.3536(4) 0.2377(7) 0.6034(6) 0.092(4) Uani 0.50 1 d PDU A -1 H5A1 H 0.3814 0.2421 0.6370 0.110 Uiso 0.50 1 calc PR A -1 H5A2 H 0.3459 0.1985 0.6011 0.110 Uiso 0.50 1 calc PR A -1 C6A C 0.3116(6) 0.2683(8) 0.6382(8) 0.145(8) Uani 0.50 1 d PDU A -1 H6A1 H 0.2820 0.2527 0.6193 0.217 Uiso 0.50 1 calc PR A -1 H6A2 H 0.3133 0.3067 0.6236 0.217 Uiso 0.50 1 calc PR A -1 H6A3 H 0.3127 0.2652 0.6937 0.217 Uiso 0.50 1 calc PR A -1 C7A C 0.3341(8) 0.3034(8) 0.2254(16) 0.053(5) Uani 0.50 1 d PDU A -1 H7A1 H 0.3373 0.3027 0.1693 0.063 Uiso 0.50 1 calc PR A -1 H7A2 H 0.3664 0.3008 0.2465 0.063 Uiso 0.50 1 calc PR A -1 C8A C 0.3152(8) 0.3594(8) 0.2465(10) 0.054(4) Uani 0.50 1 d PDU A -1 H8A1 H 0.3211 0.3658 0.3014 0.065 Uiso 0.50 1 calc PR A -1 H8A2 H 0.2806 0.3599 0.2384 0.065 Uiso 0.50 1 calc PR A -1 C9A C 0.3376(9) 0.4055(8) 0.2007(9) 0.059(4) Uani 0.50 1 d PDU A -1 H9A1 H 0.3296 0.4404 0.2253 0.070 Uiso 0.50 1 calc PR A -1 H9A2 H 0.3724 0.4014 0.2021 0.070 Uiso 0.50 1 calc PR A -1 C10A C 0.3214(7) 0.4071(9) 0.1179(8) 0.062(4) Uani 0.50 1 d PDU A -1 H10A H 0.3286 0.3716 0.0941 0.074 Uiso 0.50 1 calc PR A -1 H10B H 0.2867 0.4119 0.1168 0.074 Uiso 0.50 1 calc PR A -1 C11A C 0.3439(7) 0.4516(9) 0.0702(9) 0.075(5) Uani 0.50 1 d PDU A -1 H11A H 0.3785 0.4456 0.0684 0.089 Uiso 0.50 1 calc PR A -1 H11B H 0.3384 0.4870 0.0954 0.089 Uiso 0.50 1 calc PR A -1 C12A C 0.3251(7) 0.4545(10) -0.0114(9) 0.086(6) Uani 0.50 1 d PDU A -1 H12A H 0.3254 0.4182 -0.0341 0.129 Uiso 0.50 1 calc PR A -1 H12B H 0.3451 0.4788 -0.0416 0.129 Uiso 0.50 1 calc PR A -1 H12C H 0.2926 0.4685 -0.0109 0.129 Uiso 0.50 1 calc PR A -1 C13A C 0.2627(3) 0.2465(17) 0.2057(5) 0.073(3) Uani 0.50 1 d PDU A -1 H13A H 0.2446 0.2807 0.2114 0.088 Uiso 0.50 1 calc PR A -1 H13B H 0.2441 0.2172 0.2297 0.088 Uiso 0.50 1 calc PR A -1 C14A C 0.2679(5) 0.2340(7) 0.1207(6) 0.100(4) Uani 0.50 1 d PDU A -1 H14D H 0.3001 0.2441 0.1042 0.120 Uiso 0.50 1 calc PR A -1 H14E H 0.2642 0.1944 0.1130 0.120 Uiso 0.50 1 calc PR A -1 C15A C 0.2324(5) 0.2634(7) 0.0707(5) 0.111(4) Uani 0.50 1 d PDU A -1 H15D H 0.2002 0.2522 0.0861 0.133 Uiso 0.50 1 calc PR A -1 H15E H 0.2352 0.3028 0.0801 0.133 Uiso 0.50 1 calc PR A -1 C16A C 0.2380(4) 0.2532(13) -0.0140(5) 0.110(4) Uani 0.50 1 d PDU A -1 H16A H 0.2645 0.2275 -0.0216 0.132 Uiso 0.50 1 calc PR A -1 H16B H 0.2467 0.2878 -0.0390 0.132 Uiso 0.50 1 calc PR A -1 C17A C 0.1943(5) 0.2304(7) -0.0534(7) 0.125(5) Uani 0.50 1 d PDU A -1 H17A H 0.1898 0.1924 -0.0367 0.150 Uiso 0.50 1 calc PR A -1 H17B H 0.1664 0.2514 -0.0365 0.150 Uiso 1 2 calc SR A -1 C18A C 0.1963(6) 0.2316(10) -0.1394(7) 0.172(9) Uani 0.50 1 d PDU A -1 H18A H 0.2289 0.2385 -0.1558 0.258 Uiso 0.50 1 calc PR A -1 H18B H 0.1757 0.2606 -0.1584 0.258 Uiso 0.50 1 calc PR A -1 H18C H 0.1857 0.1966 -0.1596 0.258 Uiso 0.50 1 calc PR A -1 C19A C 0.3417(9) 0.2058(8) 0.2313(19) 0.067(6) Uani 0.50 1 d PDU A -1 H19A H 0.3720 0.2117 0.2583 0.081 Uiso 0.50 1 calc PR A -1 H19B H 0.3484 0.2045 0.1760 0.081 Uiso 0.50 1 calc PR A -1 C20A C 0.3204(9) 0.1518(8) 0.2564(11) 0.065(5) Uani 0.50 1 d PDU A -1 H20A H 0.2856 0.1537 0.2510 0.078 Uiso 0.50 1 calc PR A -1 H20B H 0.3276 0.1460 0.3110 0.078 Uiso 0.50 1 calc PR A -1 C21A C 0.3387(10) 0.1031(9) 0.2109(11) 0.066(5) Uani 0.50 1 d PDU A -1 H21A H 0.3730 0.1080 0.2015 0.079 Uiso 0.50 1 calc PR A -1 H21B H 0.3347 0.0698 0.2417 0.079 Uiso 0.50 1 calc PR A -1 C22A C 0.3138(7) 0.0955(9) 0.1349(10) 0.070(5) Uani 0.50 1 d PDU A -1 H22A H 0.2800 0.0883 0.1449 0.084 Uiso 0.50 1 calc PR A -1 H22B H 0.3158 0.1300 0.1062 0.084 Uiso 0.50 1 calc PR A -1 C23A C 0.3329(7) 0.0503(9) 0.0849(10) 0.075(5) Uani 0.50 1 d PDU A -1 H23A H 0.3318 0.0158 0.1138 0.090 Uiso 0.50 1 calc PR A -1 H23B H 0.3664 0.0580 0.0728 0.090 Uiso 0.50 1 calc PR A -1 C24A C 0.3053(7) 0.0432(10) 0.0103(9) 0.088(6) Uani 0.50 1 d PDU A -1 H24A H 0.2739 0.0285 0.0214 0.132 Uiso 0.50 1 calc PR A -1 H24B H 0.3224 0.0182 -0.0233 0.132 Uiso 0.50 1 calc PR A -1 H24C H 0.3020 0.0785 -0.0149 0.132 Uiso 0.50 1 calc PR A -1 C1D C 0.1990(4) 0.5929(5) 0.2724(7) 0.176(5) Uani 1 1 d DU . . H1D1 H 0.2044 0.6197 0.3127 0.264 Uiso 1 1 calc R . . H1D2 H 0.1852 0.5600 0.2945 0.264 Uiso 1 1 calc R . . H1D3 H 0.1774 0.6080 0.2344 0.264 Uiso 1 1 calc R . . C2D C 0.2461(3) 0.5788(4) 0.2344(6) 0.130(4) Uani 1 1 d DU . . H2D1 H 0.2668 0.5602 0.2715 0.156 Uiso 1 1 calc R . . H2D2 H 0.2404 0.5537 0.1913 0.156 Uiso 1 1 calc R . . C3D C 0.2704(3) 0.6299(5) 0.2055(6) 0.160(4) Uani 1 1 d DU . . H3D1 H 0.2496 0.6482 0.1681 0.192 Uiso 1 1 calc R . . H3D2 H 0.2755 0.6551 0.2486 0.192 Uiso 1 1 calc R . . C4D C 0.3168(3) 0.6173(4) 0.1688(6) 0.127(4) Uani 1 1 d DU . . H4D1 H 0.3115 0.5940 0.1237 0.152 Uiso 1 1 calc R . . H4D2 H 0.3368 0.5970 0.2051 0.152 Uiso 1 1 calc R . . C5D C 0.3424(4) 0.6691(5) 0.1444(6) 0.160(5) Uani 1 1 d DU . . H5D1 H 0.3192 0.6960 0.1273 0.240 Uiso 1 1 calc R . . H5D2 H 0.3642 0.6607 0.1027 0.240 Uiso 1 1 calc R . . H5D3 H 0.3602 0.6837 0.1876 0.240 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 S1 0.0497(10) 0.0685(15) 0.0539(10) -0.0055(10) -0.0064(8) 0.0005(9) S2 0.0542(10) 0.0615(15) 0.0631(11) -0.0023(10) -0.0042(8) -0.0019(9) S3 0.0620(11) 0.0765(16) 0.0677(12) -0.0042(11) -0.0021(9) -0.0105(10) S4 0.0525(10) 0.0840(16) 0.0609(11) -0.0052(11) -0.0079(8) -0.0068(10) S5 0.0513(10) 0.0757(16) 0.0630(11) -0.0057(11) 0.0046(8) -0.0054(10) S6 0.0497(10) 0.0764(16) 0.0609(11) -0.0031(10) 0.0008(8) 0.0006(9) S7 0.0533(11) 0.1068(18) 0.0627(12) -0.0142(12) -0.0019(9) 0.0096(11) S8 0.0540(10) 0.0847(17) 0.0644(12) -0.0073(11) 0.0042(9) -0.0035(10) S9 0.0508(10) 0.0650(15) 0.0497(10) -0.0034(9) -0.0014(7) -0.0010(9) S10 0.0675(12) 0.0765(16) 0.0570(11) -0.0043(11) 0.0065(9) 0.0011(10) Cl1 0.0493(13) 0.070(2) 0.0598(15) 0.000 -0.0046(11) 0.000 N1 0.044(3) 0.058(4) 0.053(3) 0.006(3) -0.003(2) 0.003(3) N2 0.049(3) 0.059(4) 0.055(3) 0.004(3) -0.002(3) 0.000(3) N3 0.047(4) 0.072(6) 0.037(4) 0.000 -0.012(3) 0.000 C1 0.042(3) 0.059(5) 0.051(4) 0.010(4) 0.005(3) 0.004(3) C2 0.040(3) 0.054(5) 0.049(4) -0.005(3) -0.007(3) -0.001(3) C3 0.042(3) 0.060(5) 0.052(4) -0.008(4) -0.001(3) -0.002(3) C4 0.045(3) 0.058(5) 0.055(4) 0.009(4) -0.001(3) 0.001(3) C5 0.050(4) 0.051(5) 0.056(4) -0.006(3) -0.001(3) -0.005(3) C6 0.052(4) 0.054(5) 0.061(4) -0.001(4) -0.003(3) -0.002(3) C7 0.043(4) 0.074(5) 0.070(4) -0.026(4) 0.003(3) -0.006(4) C8 0.066(4) 0.066(5) 0.078(5) -0.018(4) 0.005(4) -0.002(4) C9 0.055(4) 0.082(6) 0.084(5) -0.024(5) 0.003(4) -0.006(4) C10 0.056(4) 0.079(6) 0.076(5) -0.031(4) -0.006(4) 0.002(4) C11 0.058(4) 0.067(5) 0.063(4) -0.025(4) 0.004(3) -0.001(4) C12 0.053(4) 0.065(5) 0.052(4) -0.008(4) -0.008(3) -0.007(4) C13 0.039(3) 0.059(5) 0.060(4) 0.004(4) 0.000(3) -0.001(3) C14 0.045(4) 0.082(6) 0.061(4) -0.008(4) 0.006(3) -0.007(4) C15 0.047(4) 0.077(6) 0.058(4) 0.010(4) 0.000(3) -0.004(4) C16 0.051(4) 0.057(5) 0.054(4) 0.010(4) -0.001(3) -0.005(3) C17 0.051(4) 0.051(5) 0.052(4) -0.004(3) 0.004(3) -0.004(3) C18 0.043(3) 0.055(5) 0.049(4) -0.001(3) 0.000(3) -0.001(3) C19 0.043(3) 0.055(5) 0.049(4) 0.008(4) -0.001(3) -0.002(3) C20 0.060(4) 0.065(5) 0.050(4) -0.007(4) 0.000(3) -0.001(4) C21 0.051(4) 0.080(5) 0.044(4) -0.013(4) 0.002(3) -0.009(4) C22 0.053(4) 0.067(5) 0.060(4) -0.006(4) 0.000(3) 0.009(4) C23 0.058(4) 0.063(5) 0.065(4) 0.002(4) 0.002(3) 0.011(4) C24 0.056(4) 0.070(5) 0.057(4) -0.008(4) 0.002(3) 0.004(4) C25 0.068(4) 0.059(5) 0.060(4) 0.001(4) -0.002(3) -0.008(4) C26 0.055(4) 0.067(5) 0.056(4) -0.005(4) 0.010(3) 0.001(4) C27 0.050(4) 0.054(5) 0.053(4) -0.003(3) 0.007(3) 0.004(3) C28 0.043(3) 0.061(5) 0.043(3) -0.005(3) -0.001(3) 0.001(3) C29 0.054(4) 0.079(6) 0.049(4) 0.003(4) -0.005(3) -0.005(4) C30 0.050(4) 0.068(5) 0.061(4) 0.005(4) 0.002(3) 0.005(4) C31 0.049(3) 0.054(5) 0.044(4) 0.003(3) 0.006(3) -0.003(3) C32 0.040(3) 0.051(5) 0.049(4) -0.001(3) 0.006(3) 0.003(3) C33 0.046(4) 0.047(6) 0.046(5) 0.000 -0.001(4) 0.000 C34 0.051(5) 0.055(6) 0.039(5) 0.000 0.005(4) 0.000 C35 0.067(6) 0.081(5) 0.056(5) -0.007(4) 0.014(5) 0.001(5) C36 0.071(5) 0.086(5) 0.070(5) -0.002(4) 0.012(4) 0.001(5) C37 0.078(5) 0.088(6) 0.074(5) -0.002(5) 0.007(5) 0.002(5) C35A 0.068(6) 0.079(6) 0.060(6) -0.006(5) 0.017(6) 0.000(6) C36A 0.072(6) 0.082(5) 0.063(5) -0.003(5) 0.011(5) -0.004(5) C37A 0.074(6) 0.082(7) 0.069(6) -0.002(5) 0.004(6) 0.000(6) C38 0.038(4) 0.063(6) 0.052(5) 0.000 0.003(4) 0.000 C39 0.038(5) 0.071(7) 0.057(6) 0.000 -0.002(4) 0.000 C40 0.053(5) 0.067(7) 0.050(5) 0.000 -0.007(4) 0.000 N1A 0.049(4) 0.065(6) 0.055(4) 0.000(10) 0.006(3) 0.006(10) C1A 0.046(5) 0.049(9) 0.054(5) -0.006(6) -0.005(4) -0.003(6) C2A 0.049(4) 0.057(8) 0.069(5) 0.001(6) 0.002(4) -0.005(6) C3A 0.064(5) 0.064(8) 0.061(5) 0.000(6) -0.003(4) 0.002(6) C4A 0.073(5) 0.081(7) 0.072(5) -0.001(6) -0.012(4) 0.007(6) C5A 0.089(6) 0.098(8) 0.088(6) -0.003(6) -0.008(5) -0.001(6) C6A 0.161(12) 0.143(15) 0.129(11) 0.002(10) -0.026(10) -0.001(11) C7A 0.045(7) 0.059(8) 0.054(7) 0.008(6) 0.009(6) 0.006(6) C8A 0.051(6) 0.059(7) 0.053(6) 0.001(6) 0.004(5) 0.012(6) C9A 0.055(6) 0.064(7) 0.057(6) 0.002(6) 0.004(5) 0.002(6) C10A 0.058(7) 0.064(7) 0.063(7) 0.006(6) 0.005(5) -0.001(5) C11A 0.071(7) 0.081(8) 0.072(7) 0.010(6) 0.003(6) -0.002(6) C12A 0.076(11) 0.109(12) 0.074(10) -0.001(10) -0.007(9) -0.003(10) C13A 0.071(5) 0.079(7) 0.069(5) -0.001(8) -0.014(5) -0.004(8) C14A 0.100(6) 0.097(8) 0.103(6) -0.004(6) -0.021(5) -0.002(6) C15A 0.114(6) 0.106(7) 0.113(6) -0.003(6) -0.015(6) -0.012(6) C16A 0.110(6) 0.115(7) 0.106(6) -0.003(7) -0.018(5) -0.006(7) C17A 0.128(7) 0.130(9) 0.117(7) -0.005(7) -0.004(6) -0.005(6) C18A 0.190(12) 0.171(16) 0.156(12) -0.002(12) 0.000(11) -0.003(12) C19A 0.066(9) 0.067(9) 0.069(8) -0.006(7) 0.006(6) 0.003(7) C20A 0.064(7) 0.065(8) 0.066(7) -0.004(6) 0.001(6) 0.001(6) C21A 0.063(7) 0.066(7) 0.067(7) -0.007(6) 0.000(6) -0.003(6) C22A 0.065(7) 0.070(7) 0.075(7) -0.007(6) 0.000(6) -0.003(6) C23A 0.069(8) 0.079(8) 0.078(8) -0.009(6) -0.001(6) -0.004(6) C24A 0.091(12) 0.097(12) 0.075(10) -0.009(10) -0.019(9) -0.010(10) C1D 0.147(9) 0.166(11) 0.215(12) -0.018(9) 0.062(9) -0.003(8) C2D 0.145(7) 0.119(7) 0.127(7) 0.016(6) -0.002(6) -0.028(6) C3D 0.154(8) 0.179(9) 0.148(8) -0.024(7) 0.001(7) -0.006(7) C4D 0.123(7) 0.120(7) 0.138(7) 0.006(6) 0.035(6) -0.001(6) C5D 0.151(9) 0.168(11) 0.160(10) -0.006(9) 0.027(8) -0.015(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C2 1.754(6) . ? S1 C5 1.761(7) . ? S2 C5 1.748(7) . ? S2 C3 1.746(7) . ? S3 C6 1.751(7) . ? S3 C7 1.758(7) . ? S4 C12 1.747(7) . ? S4 C6 1.766(7) . ? S5 C17 1.748(7) . ? S5 C20 1.769(7) . ? S6 C18 1.747(7) . ? S6 C20 1.762(7) . ? S7 C22 1.762(7) . ? S7 C21 1.769(6) . ? S8 C27 1.742(6) . ? S8 C21 1.757(6) . ? S9 C33 1.774(5) . ? S9 C32 1.775(6) . ? S10 C35A 1.72(4) . ? S10 C35 1.760(19) . ? S10 C34 1.767(5) . ? N1 C4 1.390(8) . ? N1 C1 1.396(7) . ? N1 H1 0.8800 . ? N2 C19 1.391(7) . ? N2 C16 1.399(7) . ? N2 H2 0.8800 . ? N3 C31 1.370(7) . ? N3 C31 1.370(7) 8_565 ? N3 H3A 0.8800 . ? C1 C2 1.373(8) . ? C1 C38 1.507(8) . ? C2 C3 1.434(8) . ? C3 C4 1.393(8) . ? C4 C13 1.496(8) . ? C5 C6 1.357(8) . ? C7 C12 1.377(9) . ? C7 C8 1.417(9) . ? C8 C9 1.372(9) . ? C8 H8 0.9500 . ? C9 C10 1.382(10) . ? C9 H9 0.9500 . ? C10 C11 1.396(9) . ? C10 H10 0.9500 . ? C11 C12 1.383(8) . ? C11 H11 0.9500 . ? C13 C16 1.529(8) . ? C13 C15 1.542(8) . ? C13 C14 1.555(8) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.368(8) . ? C17 C18 1.415(8) . ? C18 C19 1.372(8) . ? C19 C28 1.520(8) . ? C20 C21 1.328(8) . ? C22 C27 1.385(8) . ? C22 C23 1.401(8) . ? C23 C24 1.358(8) . ? C23 H23 0.9500 . ? C24 C25 1.385(8) . ? C24 H24 0.9500 . ? C25 C26 1.399(8) . ? C25 H25 0.9500 . ? C26 C27 1.375(8) . ? C26 H26 0.9500 . ? C28 C31 1.519(9) . ? C28 C30 1.534(8) . ? C28 C29 1.536(8) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.359(8) . ? C32 C32 1.400(12) 8_565 ? C33 C34 1.334(10) . ? C33 S9 1.774(5) 8_565 ? C34 S10 1.767(5) 8_565 ? C35 C35 1.35(4) 8_565 ? C35 C36 1.37(2) . ? C36 C37 1.417(15) . ? C36 H36A 0.9500 . ? C37 C37 1.34(2) 8_565 ? C37 H37A 0.9500 . ? C35A C36A 1.40(4) . ? C35A C35A 1.41(8) 8_565 ? C36A C37A 1.35(2) . ? C36A H36B 0.9500 . ? C37A C37A 1.39(4) 8_565 ? C37A H37B 0.9500 . ? C38 C1 1.507(8) 8_565 ? C38 C39 1.536(10) . ? C38 C40 1.553(11) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? N1A C1A 1.496(7) . ? N1A C19A 1.503(8) . ? N1A C7A 1.503(8) . ? N1A C13A 1.506(7) . ? C1A C2A 1.534(6) . ? C1A H1A1 0.9900 . ? C1A H1A2 0.9900 . ? C2A C3A 1.537(6) . ? C2A H2A1 0.9900 . ? C2A H2A2 0.9900 . ? C3A C4A 1.513(7) . ? C3A H3A1 0.9900 . ? C3A H3A2 0.9900 . ? C4A C5A 1.530(7) . ? C4A H4A1 0.9900 . ? C4A H4A2 0.9900 . ? C5A C6A 1.535(7) . ? C5A H5A1 0.9900 . ? C5A H5A2 0.9900 . ? C6A H6A1 0.9800 . ? C6A H6A2 0.9800 . ? C6A H6A3 0.9800 . ? C7A C8A 1.525(7) . ? C7A H7A1 0.9900 . ? C7A H7A2 0.9900 . ? C8A C9A 1.529(7) . ? C8A H8A1 0.9900 . ? C8A H8A2 0.9900 . ? C9A C10A 1.526(7) . ? C9A H9A1 0.9900 . ? C9A H9A2 0.9900 . ? C10A C11A 1.521(7) . ? C10A H10A 0.9900 . ? C10A H10B 0.9900 . ? C11A C12A 1.532(7) . ? C11A H11A 0.9900 . ? C11A H11B 0.9900 . ? C12A H12A 0.9800 . ? C12A H12B 0.9800 . ? C12A H12C 0.9800 . ? C13A C14A 1.532(7) . ? C13A H13A 0.9900 . ? C13A H13B 0.9900 . ? C14A C15A 1.517(7) . ? C14A H14D 0.9900 . ? C14A H14E 0.9900 . ? C15A C16A 1.516(7) . ? C15A H15D 0.9900 . ? C15A H15E 0.9900 . ? C16A C17A 1.524(8) . ? C16A H16A 0.9900 . ? C16A H16B 0.9900 . ? C17A C18A 1.511(7) . ? C17A H17A 0.9900 . ? C17A H17B 0.9900 . ? C18A H18A 0.9800 . ? C18A H18B 0.9800 . ? C18A H18C 0.9800 . ? C19A C20A 1.526(7) . ? C19A H19A 0.9900 . ? C19A H19B 0.9900 . ? C20A C21A 1.532(7) . ? C20A H20A 0.9900 . ? C20A H20B 0.9900 . ? C21A C22A 1.521(7) . ? C21A H21A 0.9900 . ? C21A H21B 0.9900 . ? C22A C23A 1.519(7) . ? C22A H22A 0.9900 . ? C22A H22B 0.9900 . ? C23A C24A 1.537(7) . ? C23A H23A 0.9900 . ? C23A H23B 0.9900 . ? C24A H24A 0.9800 . ? C24A H24B 0.9800 . ? C24A H24C 0.9800 . ? C1D C2D 1.530(8) . ? C1D H1D1 0.9800 . ? C1D H1D2 0.9800 . ? C1D H1D3 0.9800 . ? C2D C3D 1.522(8) . ? C2D H2D1 0.9900 . ? C2D H2D2 0.9900 . ? C3D C4D 1.496(8) . ? C3D H3D1 0.9900 . ? C3D H3D2 0.9900 . ? C4D C5D 1.529(8) . ? C4D H4D1 0.9900 . ? C4D H4D2 0.9900 . ? C5D H5D1 0.9800 . ? C5D H5D2 0.9800 . ? C5D H5D3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 S1 C5 93.3(3) . . ? C5 S2 C3 92.8(3) . . ? C6 S3 C7 94.0(4) . . ? C12 S4 C6 94.9(3) . . ? C17 S5 C20 92.3(3) . . ? C18 S6 C20 92.6(3) . . ? C22 S7 C21 94.9(3) . . ? C27 S8 C21 95.4(3) . . ? C33 S9 C32 93.3(3) . . ? C35A S10 C35 14.5(12) . . ? C35A S10 C34 95.5(13) . . ? C35 S10 C34 94.9(7) . . ? C4 N1 C1 112.4(6) . . ? C4 N1 H1 123.8 . . ? C1 N1 H1 123.8 . . ? C19 N2 C16 110.3(6) . . ? C19 N2 H2 124.8 . . ? C16 N2 H2 124.8 . . ? C31 N3 C31 112.1(8) . 8_565 ? C31 N3 H3A 124.0 . . ? C31 N3 H3A 124.0 8_565 . ? C2 C1 N1 105.7(6) . . ? C2 C1 C38 132.9(6) . . ? N1 C1 C38 121.0(6) . . ? C1 C2 C3 108.5(6) . . ? C1 C2 S1 135.8(6) . . ? C3 C2 S1 115.2(5) . . ? C4 C3 C2 108.7(6) . . ? C4 C3 S2 133.4(6) . . ? C2 C3 S2 117.5(5) . . ? N1 C4 C3 104.8(6) . . ? N1 C4 C13 122.1(6) . . ? C3 C4 C13 132.8(7) . . ? C6 C5 S2 120.5(5) . . ? C6 C5 S1 122.6(5) . . ? S2 C5 S1 116.8(4) . . ? C5 C6 S3 122.6(5) . . ? C5 C6 S4 122.7(5) . . ? S3 C6 S4 114.7(4) . . ? C12 C7 C8 121.2(7) . . ? C12 C7 S3 117.9(5) . . ? C8 C7 S3 120.8(7) . . ? C9 C8 C7 117.6(8) . . ? C9 C8 H8 121.2 . . ? C7 C8 H8 121.2 . . ? C8 C9 C10 121.4(8) . . ? C8 C9 H9 119.3 . . ? C10 C9 H9 119.3 . . ? C9 C10 C11 120.5(7) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C12 C11 C10 119.0(8) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C7 C12 C11 120.2(7) . . ? C7 C12 S4 115.9(5) . . ? C11 C12 S4 123.9(6) . . ? C4 C13 C16 107.9(5) . . ? C4 C13 C15 109.4(6) . . ? C16 C13 C15 108.3(6) . . ? C4 C13 C14 112.5(6) . . ? C16 C13 C14 110.7(5) . . ? C15 C13 C14 107.9(5) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 N2 106.0(6) . . ? C17 C16 C13 133.3(7) . . ? N2 C16 C13 120.6(6) . . ? C16 C17 C18 108.9(6) . . ? C16 C17 S5 133.8(5) . . ? C18 C17 S5 117.1(5) . . ? C19 C18 C17 108.3(6) . . ? C19 C18 S6 135.4(5) . . ? C17 C18 S6 116.2(5) . . ? C18 C19 N2 106.4(6) . . ? C18 C19 C28 134.0(6) . . ? N2 C19 C28 119.6(6) . . ? C21 C20 S6 122.1(5) . . ? C21 C20 S5 122.4(5) . . ? S6 C20 S5 115.5(4) . . ? C20 C21 S8 125.5(5) . . ? C20 C21 S7 120.6(5) . . ? S8 C21 S7 114.0(4) . . ? C27 C22 C23 120.6(6) . . ? C27 C22 S7 116.5(5) . . ? C23 C22 S7 123.0(5) . . ? C24 C23 C22 119.8(7) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C25 119.5(7) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C24 C25 C26 121.5(7) . . ? C24 C25 H25 119.3 . . ? C26 C25 H25 119.3 . . ? C27 C26 C25 118.6(6) . . ? C27 C26 H26 120.7 . . ? C25 C26 H26 120.7 . . ? C26 C27 C22 120.0(6) . . ? C26 C27 S8 123.2(5) . . ? C22 C27 S8 116.8(5) . . ? C19 C28 C31 110.4(5) . . ? C19 C28 C30 109.0(6) . . ? C31 C28 C30 109.2(5) . . ? C19 C28 C29 108.7(5) . . ? C31 C28 C29 110.8(5) . . ? C30 C28 C29 108.7(5) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 N3 105.2(7) . . ? C32 C31 C28 132.1(6) . . ? N3 C31 C28 122.6(5) . . ? C31 C32 C32 108.7(4) . 8_565 ? C31 C32 S9 134.4(5) . . ? C32 C32 S9 116.8(2) 8_565 . ? C34 C33 S9 122.2(2) . . ? C34 C33 S9 122.2(2) . 8_565 ? S9 C33 S9 115.5(5) . 8_565 ? C33 C34 S10 122.7(2) . . ? C33 C34 S10 122.7(2) . 8_565 ? S10 C34 S10 114.7(5) . 8_565 ? C35 C35 C36 122.6(10) 8_565 . ? C35 C35 S10 117.4(7) 8_565 . ? C36 C35 S10 119.9(15) . . ? C35 C36 C37 115.6(14) . . ? C35 C36 H36A 122.2 . . ? C37 C36 H36A 122.2 . . ? C37 C37 C36 121.8(7) 8_565 . ? C37 C37 H37A 119.1 8_565 . ? C36 C37 H37A 119.1 . . ? C36A C35A C35A 118.1(18) . 8_565 ? C36A C35A S10 125(3) . . ? C35A C35A S10 116.9(13) 8_565 . ? C37A C36A C35A 122(2) . . ? C37A C36A H36B 119.2 . . ? C35A C36A H36B 119.2 . . ? C36A C37A C37A 120.0(13) . 8_565 ? C36A C37A H37B 120.0 . . ? C37A C37A H37B 120.0 8_565 . ? C1 C38 C1 113.7(7) . 8_565 ? C1 C38 C39 109.5(5) . . ? C1 C38 C39 109.5(5) 8_565 . ? C1 C38 C40 107.8(5) . . ? C1 C38 C40 107.8(5) 8_565 . ? C39 C38 C40 108.5(7) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C1A N1A C19A 113(2) . . ? C1A N1A C7A 106(2) . . ? C19A N1A C7A 107.1(7) . . ? C1A N1A C13A 107.4(6) . . ? C19A N1A C13A 112(2) . . ? C7A N1A C13A 111(2) . . ? N1A C1A C2A 115.1(7) . . ? N1A C1A H1A1 108.5 . . ? C2A C1A H1A1 108.5 . . ? N1A C1A H1A2 108.5 . . ? C2A C1A H1A2 108.5 . . ? H1A1 C1A H1A2 107.5 . . ? C1A C2A C3A 111.8(6) . . ? C1A C2A H2A1 109.3 . . ? C3A C2A H2A1 109.3 . . ? C1A C2A H2A2 109.3 . . ? C3A C2A H2A2 109.3 . . ? H2A1 C2A H2A2 107.9 . . ? C4A C3A C2A 114.1(6) . . ? C4A C3A H3A1 108.7 . . ? C2A C3A H3A1 108.7 . . ? C4A C3A H3A2 108.7 . . ? C2A C3A H3A2 108.7 . . ? H3A1 C3A H3A2 107.6 . . ? C3A C4A C5A 113.9(7) . . ? C3A C4A H4A1 108.8 . . ? C5A C4A H4A1 108.8 . . ? C3A C4A H4A2 108.8 . . ? C5A C4A H4A2 108.8 . . ? H4A1 C4A H4A2 107.7 . . ? C4A C5A C6A 112.7(7) . . ? C4A C5A H5A1 109.0 . . ? C6A C5A H5A1 109.1 . . ? C4A C5A H5A2 109.0 . . ? C6A C5A H5A2 109.0 . . ? H5A1 C5A H5A2 107.8 . . ? N1A C7A C8A 122.0(19) . . ? N1A C7A H7A1 106.8 . . ? C8A C7A H7A1 106.8 . . ? N1A C7A H7A2 106.8 . . ? C8A C7A H7A2 106.8 . . ? H7A1 C7A H7A2 106.7 . . ? C7A C8A C9A 113.6(6) . . ? C7A C8A H8A1 108.9 . . ? C9A C8A H8A1 108.8 . . ? C7A C8A H8A2 108.9 . . ? C9A C8A H8A2 108.8 . . ? H8A1 C8A H8A2 107.7 . . ? C10A C9A C8A 113.4(7) . . ? C10A C9A H9A1 108.9 . . ? C8A C9A H9A1 108.9 . . ? C10A C9A H9A2 108.9 . . ? C8A C9A H9A2 108.9 . . ? H9A1 C9A H9A2 107.7 . . ? C11A C10A C9A 114.8(7) . . ? C11A C10A H10A 108.6 . . ? C9A C10A H10A 108.6 . . ? C11A C10A H10B 108.6 . . ? C9A C10A H10B 108.6 . . ? H10A C10A H10B 107.5 . . ? C10A C11A C12A 113.8(7) . . ? C10A C11A H11A 108.8 . . ? C12A C11A H11A 108.8 . . ? C10A C11A H11B 108.8 . . ? C12A C11A H11B 108.8 . . ? H11A C11A H11B 107.7 . . ? N1A C13A C14A 114.5(8) . . ? N1A C13A H13A 108.6 . . ? C14A C13A H13A 108.6 . . ? N1A C13A H13B 108.7 . . ? C14A C13A H13B 108.6 . . ? H13A C13A H13B 107.6 . . ? C15A C14A C13A 113.9(8) . . ? C15A C14A H14D 108.8 . . ? C13A C14A H14D 108.8 . . ? C15A C14A H14E 108.8 . . ? C13A C14A H14E 108.8 . . ? H14D C14A H14E 107.7 . . ? C16A C15A C14A 114.8(8) . . ? C16A C15A H15D 108.6 . . ? C14A C15A H15D 108.6 . . ? C16A C15A H15E 108.6 . . ? C14A C15A H15E 108.6 . . ? H15D C15A H15E 107.5 . . ? C15A C16A C17A 114.9(7) . . ? C15A C16A H16A 108.5 . . ? C17A C16A H16A 108.5 . . ? C15A C16A H16B 108.5 . . ? C17A C16A H16B 108.5 . . ? H16A C16A H16B 107.5 . . ? C18A C17A C16A 114.6(8) . . ? C18A C17A H17A 108.6 . . ? C16A C17A H17A 108.6 . . ? C18A C17A H17B 108.6 . . ? C16A C17A H17B 108.6 . . ? H17A C17A H17B 107.6 . . ? C17A C18A H18A 109.5 . . ? C17A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? C17A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? N1A C19A C20A 111(2) . . ? N1A C19A H19A 109.4 . . ? C20A C19A H19A 109.4 . . ? N1A C19A H19B 109.4 . . ? C20A C19A H19B 109.4 . . ? H19A C19A H19B 108.0 . . ? C19A C20A C21A 113.4(7) . . ? C19A C20A H20A 108.9 . . ? C21A C20A H20A 108.9 . . ? C19A C20A H20B 108.9 . . ? C21A C20A H20B 108.9 . . ? H20A C20A H20B 107.7 . . ? C22A C21A C20A 113.4(7) . . ? C22A C21A H21A 108.9 . . ? C20A C21A H21A 108.9 . . ? C22A C21A H21B 108.9 . . ? C20A C21A H21B 108.9 . . ? H21A C21A H21B 107.7 . . ? C23A C22A C21A 115.6(7) . . ? C23A C22A H22A 108.4 . . ? C21A C22A H22A 108.4 . . ? C23A C22A H22B 108.4 . . ? C21A C22A H22B 108.4 . . ? H22A C22A H22B 107.4 . . ? C22A C23A C24A 113.3(7) . . ? C22A C23A H23A 108.9 . . ? C24A C23A H23A 108.9 . . ? C22A C23A H23B 108.9 . . ? C24A C23A H23B 108.9 . . ? H23A C23A H23B 107.7 . . ? C2D C1D H1D1 109.5 . . ? C2D C1D H1D2 109.5 . . ? H1D1 C1D H1D2 109.5 . . ? C2D C1D H1D3 109.5 . . ? H1D1 C1D H1D3 109.5 . . ? H1D2 C1D H1D3 109.5 . . ? C3D C2D C1D 110.5(8) . . ? C3D C2D H2D1 109.5 . . ? C1D C2D H2D1 109.5 . . ? C3D C2D H2D2 109.5 . . ? C1D C2D H2D2 109.5 . . ? H2D1 C2D H2D2 108.1 . . ? C4D C3D C2D 111.7(9) . . ? C4D C3D H3D1 109.3 . . ? C2D C3D H3D1 109.3 . . ? C4D C3D H3D2 109.3 . . ? C2D C3D H3D2 109.3 . . ? H3D1 C3D H3D2 107.9 . . ? C3D C4D C5D 111.4(8) . . ? C3D C4D H4D1 109.3 . . ? C5D C4D H4D1 109.4 . . ? C3D C4D H4D2 109.3 . . ? C5D C4D H4D2 109.3 . . ? H4D1 C4D H4D2 108.0 . . ? C4D C5D H5D1 109.5 . . ? C4D C5D H5D2 109.5 . . ? H5D1 C5D H5D2 109.5 . . ? C4D C5D H5D3 109.5 . . ? H5D1 C5D H5D3 109.5 . . ? H5D2 C5D H5D3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 N1 C1 C2 -1.5(7) . . . . ? C4 N1 C1 C38 172.1(6) . . . . ? N1 C1 C2 C3 0.9(7) . . . . ? C38 C1 C2 C3 -171.5(7) . . . . ? N1 C1 C2 S1 171.7(5) . . . . ? C38 C1 C2 S1 -0.7(12) . . . . ? C5 S1 C2 C1 177.4(7) . . . . ? C5 S1 C2 C3 -12.2(5) . . . . ? C1 C2 C3 C4 -0.1(7) . . . . ? S1 C2 C3 C4 -173.1(4) . . . . ? C1 C2 C3 S2 173.5(4) . . . . ? S1 C2 C3 S2 0.6(6) . . . . ? C5 S2 C3 C4 -176.8(6) . . . . ? C5 S2 C3 C2 11.5(5) . . . . ? C1 N1 C4 C3 1.4(7) . . . . ? C1 N1 C4 C13 -173.2(5) . . . . ? C2 C3 C4 N1 -0.7(7) . . . . ? S2 C3 C4 N1 -173.0(5) . . . . ? C2 C3 C4 C13 173.0(6) . . . . ? S2 C3 C4 C13 0.7(11) . . . . ? C3 S2 C5 C6 161.7(6) . . . . ? C3 S2 C5 S1 -20.4(4) . . . . ? C2 S1 C5 C6 -161.3(6) . . . . ? C2 S1 C5 S2 20.8(4) . . . . ? S2 C5 C6 S3 0.5(8) . . . . ? S1 C5 C6 S3 -177.2(3) . . . . ? S2 C5 C6 S4 177.5(4) . . . . ? S1 C5 C6 S4 -0.3(8) . . . . ? C7 S3 C6 C5 -167.7(6) . . . . ? C7 S3 C6 S4 15.2(4) . . . . ? C12 S4 C6 C5 166.8(6) . . . . ? C12 S4 C6 S3 -16.1(4) . . . . ? C6 S3 C7 C12 -8.2(6) . . . . ? C6 S3 C7 C8 174.5(6) . . . . ? C12 C7 C8 C9 1.8(10) . . . . ? S3 C7 C8 C9 179.0(5) . . . . ? C7 C8 C9 C10 -1.0(11) . . . . ? C8 C9 C10 C11 0.2(11) . . . . ? C9 C10 C11 C12 -0.1(10) . . . . ? C8 C7 C12 C11 -1.8(10) . . . . ? S3 C7 C12 C11 -179.0(5) . . . . ? C8 C7 C12 S4 175.6(5) . . . . ? S3 C7 C12 S4 -1.7(8) . . . . ? C10 C11 C12 C7 0.9(10) . . . . ? C10 C11 C12 S4 -176.3(5) . . . . ? C6 S4 C12 C7 10.5(6) . . . . ? C6 S4 C12 C11 -172.2(6) . . . . ? N1 C4 C13 C16 56.7(8) . . . . ? C3 C4 C13 C16 -116.2(8) . . . . ? N1 C4 C13 C15 174.3(5) . . . . ? C3 C4 C13 C15 1.5(9) . . . . ? N1 C4 C13 C14 -65.7(7) . . . . ? C3 C4 C13 C14 121.5(8) . . . . ? C19 N2 C16 C17 1.1(7) . . . . ? C19 N2 C16 C13 179.5(5) . . . . ? C4 C13 C16 C17 83.9(9) . . . . ? C15 C13 C16 C17 -34.4(10) . . . . ? C14 C13 C16 C17 -152.6(7) . . . . ? C4 C13 C16 N2 -94.0(7) . . . . ? C15 C13 C16 N2 147.7(6) . . . . ? C14 C13 C16 N2 29.5(8) . . . . ? N2 C16 C17 C18 -2.3(7) . . . . ? C13 C16 C17 C18 179.6(7) . . . . ? N2 C16 C17 S5 -177.8(5) . . . . ? C13 C16 C17 S5 4.1(12) . . . . ? C20 S5 C17 C16 -172.0(7) . . . . ? C20 S5 C17 C18 12.8(5) . . . . ? C16 C17 C18 C19 2.7(8) . . . . ? S5 C17 C18 C19 179.1(4) . . . . ? C16 C17 C18 S6 -174.2(5) . . . . ? S5 C17 C18 S6 2.2(7) . . . . ? C20 S6 C18 C19 168.3(7) . . . . ? C20 S6 C18 C17 -15.9(5) . . . . ? C17 C18 C19 N2 -1.9(7) . . . . ? S6 C18 C19 N2 174.1(5) . . . . ? C17 C18 C19 C28 -179.3(7) . . . . ? S6 C18 C19 C28 -3.2(12) . . . . ? C16 N2 C19 C18 0.5(7) . . . . ? C16 N2 C19 C28 178.4(5) . . . . ? C18 S6 C20 C21 -158.4(7) . . . . ? C18 S6 C20 S5 25.0(4) . . . . ? C17 S5 C20 C21 159.4(7) . . . . ? C17 S5 C20 S6 -24.0(4) . . . . ? S6 C20 C21 S8 175.1(4) . . . . ? S5 C20 C21 S8 -8.6(10) . . . . ? S6 C20 C21 S7 -3.9(9) . . . . ? S5 C20 C21 S7 172.4(4) . . . . ? C27 S8 C21 C20 -163.0(7) . . . . ? C27 S8 C21 S7 16.0(5) . . . . ? C22 S7 C21 C20 164.7(7) . . . . ? C22 S7 C21 S8 -14.4(5) . . . . ? C21 S7 C22 C27 6.5(6) . . . . ? C21 S7 C22 C23 -172.5(6) . . . . ? C27 C22 C23 C24 0.0(11) . . . . ? S7 C22 C23 C24 178.9(6) . . . . ? C22 C23 C24 C25 0.0(11) . . . . ? C23 C24 C25 C26 -0.6(11) . . . . ? C24 C25 C26 C27 1.2(11) . . . . ? C25 C26 C27 C22 -1.2(10) . . . . ? C25 C26 C27 S8 176.6(5) . . . . ? C23 C22 C27 C26 0.6(11) . . . . ? S7 C22 C27 C26 -178.4(6) . . . . ? C23 C22 C27 S8 -177.3(6) . . . . ? S7 C22 C27 S8 3.7(8) . . . . ? C21 S8 C27 C26 170.3(6) . . . . ? C21 S8 C27 C22 -11.9(6) . . . . ? C18 C19 C28 C31 -115.6(8) . . . . ? N2 C19 C28 C31 67.4(7) . . . . ? C18 C19 C28 C30 4.4(10) . . . . ? N2 C19 C28 C30 -172.7(5) . . . . ? C18 C19 C28 C29 122.7(7) . . . . ? N2 C19 C28 C29 -54.4(8) . . . . ? C31 N3 C31 C32 -3.0(9) 8_565 . . . ? C31 N3 C31 C28 -179.5(3) 8_565 . . . ? C19 C28 C31 C32 58.2(8) . . . . ? C30 C28 C31 C32 -61.7(8) . . . . ? C29 C28 C31 C32 178.7(6) . . . . ? C19 C28 C31 N3 -126.4(6) . . . . ? C30 C28 C31 N3 113.7(6) . . . . ? C29 C28 C31 N3 -5.9(8) . . . . ? N3 C31 C32 C32 1.8(5) . . . 8_565 ? C28 C31 C32 C32 177.8(5) . . . 8_565 ? N3 C31 C32 S9 178.4(5) . . . . ? C28 C31 C32 S9 -5.6(11) . . . . ? C33 S9 C32 C31 171.6(6) . . . . ? C33 S9 C32 C32 -12.0(3) . . . 8_565 ? C32 S9 C33 C34 -162.0(7) . . . . ? C32 S9 C33 S9 20.3(5) . . . 8_565 ? S9 C33 C34 S10 0.9(11) . . . . ? S9 C33 C34 S10 178.4(4) 8_565 . . . ? S9 C33 C34 S10 -178.4(4) . . . 8_565 ? S9 C33 C34 S10 -0.9(11) 8_565 . . 8_565 ? C35A S10 C34 C33 -172.6(11) . . . . ? C35 S10 C34 C33 172.9(9) . . . . ? C35A S10 C34 S10 6.8(10) . . . 8_565 ? C35 S10 C34 S10 -7.8(7) . . . 8_565 ? C35A S10 C35 C35 -88(7) . . . 8_565 ? C34 S10 C35 C35 4.7(4) . . . 8_565 ? C35A S10 C35 C36 89(7) . . . . ? C34 S10 C35 C36 -178.4(11) . . . . ? C35 C35 C36 C37 -1.7(14) 8_565 . . . ? S10 C35 C36 C37 -178.4(10) . . . . ? C35 C36 C37 C37 1.6(14) . . . 8_565 ? C35 S10 C35A C36A -103(8) . . . . ? C34 S10 C35A C36A 168(2) . . . . ? C35 S10 C35A C35A 84(7) . . . 8_565 ? C34 S10 C35A C35A -4.1(6) . . . 8_565 ? C35A C35A C36A C37A -5(3) 8_565 . . . ? S10 C35A C36A C37A -178.0(18) . . . . ? C35A C36A C37A C37A 6(3) . . . 8_565 ? C2 C1 C38 C1 -110.0(8) . . . 8_565 ? N1 C1 C38 C1 78.5(8) . . . 8_565 ? C2 C1 C38 C39 127.2(8) . . . . ? N1 C1 C38 C39 -44.3(8) . . . . ? C2 C1 C38 C40 9.4(10) . . . . ? N1 C1 C38 C40 -162.1(6) . . . . ? C19A N1A C1A C2A 50(3) . . . . ? C7A N1A C1A C2A -67(3) . . . . ? C13A N1A C1A C2A 174(2) . . . . ? N1A C1A C2A C3A -171(2) . . . . ? C1A C2A C3A C4A -179(2) . . . . ? C2A C3A C4A C5A -162(2) . . . . ? C3A C4A C5A C6A -55(2) . . . . ? C1A N1A C7A C8A -48(2) . . . . ? C19A N1A C7A C8A -169(3) . . . . ? C13A N1A C7A C8A 68(2) . . . . ? N1A C7A C8A C9A -163.8(17) . . . . ? C7A C8A C9A C10A 72(2) . . . . ? C8A C9A C10A C11A -178.5(17) . . . . ? C9A C10A C11A C12A -177(2) . . . . ? C1A N1A C13A C14A -174(2) . . . . ? C19A N1A C13A C14A -49(3) . . . . ? C7A N1A C13A C14A 71(3) . . . . ? N1A C13A C14A C15A -141(2) . . . . ? C13A C14A C15A C16A 177.8(16) . . . . ? C14A C15A C16A C17A 123(2) . . . . ? C15A C16A C17A C18A 167.5(18) . . . . ? C1A N1A C19A C20A 60(2) . . . . ? C7A N1A C19A C20A 177(2) . . . . ? C13A N1A C19A C20A -61(3) . . . . ? N1A C19A C20A C21A 153.0(16) . . . . ? C19A C20A C21A C22A -82(3) . . . . ? C20A C21A C22A C23A 175.9(18) . . . . ? C21A C22A C23A C24A 178(2) . . . . ? C1D C2D C3D C4D 179.3(10) . . . . ? C2D C3D C4D C5D -176.4(9) . . . . ? _diffrn_measured_fraction_theta_max 0.886 _diffrn_reflns_theta_full 70.00 _diffrn_measured_fraction_theta_full 0.886 _refine_diff_density_max 0.755 _refine_diff_density_min -0.555 _refine_diff_density_rms 0.111 data_pnnm _database_code_depnum_ccdc_archive 'CCDC 868898' #TrackingRef 'pnnm.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H44 N4 S16, Cl 1-, C16 H36 N 1+, 2 C H2 Cl2, C H Cl3' _chemical_formula_sum 'C79 H85 Cl8 N5 S16' _chemical_formula_weight 1901.08 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnnm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' _cell_length_a 29.858(6) _cell_length_b 14.168(3) _cell_length_c 21.609(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9141(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16107 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3944 _exptl_absorpt_coefficient_mu 0.656 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.679 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ; Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC-12 with Saturn 724+ 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 33353 _diffrn_reflns_av_R_equivalents 0.1536 _diffrn_reflns_av_sigmaI/netI 0.1833 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8260 _reflns_number_gt 3271 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _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. The complex lies on a crystallographic mirror plane of symmetry at x, y, 0. The cation also lies on this plane and is disordered about it. The geometry of the cation was restrained during refinement so that the N-C, C-C bonds and related angles were equivalent. In addition to this disorder, there were several regions where there was disordered solvent. The solvent appeared to be a mixture of methylene chloride and chloroform. The solvent molecules were also disordered. ; _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^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8260 _refine_ls_number_parameters 578 _refine_ls_number_restraints 137 _refine_ls_R_factor_all 0.2526 _refine_ls_R_factor_gt 0.1431 _refine_ls_wR_factor_ref 0.3361 _refine_ls_wR_factor_gt 0.3074 _refine_ls_goodness_of_fit_ref 1.673 _refine_ls_restrained_S_all 1.675 _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 0.1888(3) 0.3613(8) 0.1326(5) 0.049(3) Uani 1 1 d U . . C2 C 0.2213(4) 0.4202(7) 0.1596(5) 0.049(3) Uani 1 1 d . . . C3 C 0.2622(3) 0.3757(8) 0.1577(4) 0.050(3) Uani 1 1 d . . . C4 C 0.2570(3) 0.2866(8) 0.1297(4) 0.047(3) Uani 1 1 d . . . C5 C 0.2796(3) 0.5443(9) 0.1943(4) 0.055(3) Uani 1 1 d . . . C6 C 0.3015(3) 0.6241(8) 0.2027(5) 0.050(3) Uani 1 1 d . . . C7 C 0.3634(4) 0.7489(8) 0.1910(5) 0.058(3) Uani 1 1 d . . . C8 C 0.3243(3) 0.7995(8) 0.1929(5) 0.049(3) Uani 1 1 d . . . C9 C 0.3229(4) 0.8967(9) 0.1835(5) 0.064(3) Uani 1 1 d . . . H9 H 0.2958 0.9313 0.1865 0.077 Uiso 1 1 calc R . . C10 C 0.3646(5) 0.9418(10) 0.1690(5) 0.073(4) Uani 1 1 d . . . H10 H 0.3650 1.0080 0.1618 0.087 Uiso 1 1 calc R . . C11 C 0.4049(5) 0.8911(10) 0.1653(5) 0.068(3) Uani 1 1 d . . . H11 H 0.4322 0.9219 0.1551 0.082 Uiso 1 1 calc R . . C12 C 0.4039(4) 0.7945(10) 0.1770(5) 0.068(3) Uani 1 1 d . . . H12 H 0.4309 0.7590 0.1755 0.082 Uiso 1 1 calc R . . C13 C 0.2909(3) 0.2080(8) 0.1164(5) 0.053(3) Uani 1 1 d . . . C14 C 0.2679(3) 0.1100(7) 0.1213(5) 0.062(3) Uani 1 1 d . . . H14A H 0.2412 0.1091 0.0950 0.093 Uiso 1 1 calc R . . H14B H 0.2592 0.0982 0.1643 0.093 Uiso 1 1 calc R . . H14C H 0.2888 0.0609 0.1076 0.093 Uiso 1 1 calc R . . C15 C 0.3295(3) 0.2114(7) 0.1649(5) 0.058(3) Uani 1 1 d . . . H15A H 0.3509 0.1605 0.1564 0.087 Uiso 1 1 calc R . . H15B H 0.3171 0.2033 0.2066 0.087 Uiso 1 1 calc R . . H15C H 0.3449 0.2724 0.1623 0.087 Uiso 1 1 calc R . . C16 C 0.1404(3) 0.3756(8) 0.1169(5) 0.052(3) Uani 1 1 d . . . C17 C 0.1188(3) 0.4434(8) 0.1654(5) 0.066(3) Uani 1 1 d . . . H17A H 0.1196 0.4139 0.2064 0.099 Uiso 1 1 calc R . . H17B H 0.0877 0.4562 0.1537 0.099 Uiso 1 1 calc R . . H17C H 0.1356 0.5028 0.1664 0.099 Uiso 1 1 calc R . . C18 C 0.1149(3) 0.2816(8) 0.1200(5) 0.062(3) Uani 1 1 d . . . H18A H 0.1271 0.2379 0.0892 0.093 Uiso 1 1 calc R . . H18B H 0.0831 0.2927 0.1114 0.093 Uiso 1 1 calc R . . H18C H 0.1182 0.2542 0.1614 0.093 Uiso 1 1 calc R . . C19 C 0.1363(3) 0.4197(9) 0.0522(5) 0.054(3) Uani 1 1 d . . . C20 C 0.1286(3) 0.5089(8) 0.0329(5) 0.049(3) Uani 1 1 d . . . C21 C 0.0985(6) 0.6718(13) 0.0000 0.067(5) Uani 1 2 d S . . C22 C 0.0691(5) 0.7485(13) 0.0000 0.071(5) Uani 1 2 d S . . C23 C 0.0029(4) 0.8479(8) 0.0336(6) 0.077(4) Uani 1 1 d . . . C24 C -0.0314(4) 0.8919(9) 0.0660(8) 0.092(5) Uani 1 1 d . . . H24A H -0.0317 0.8952 0.1099 0.110 Uiso 1 1 calc R . . C25 C -0.0655(5) 0.9310(9) 0.0300(7) 0.107(7) Uani 1 1 d . . . H25A H -0.0901 0.9593 0.0507 0.128 Uiso 1 1 calc R . . C26 C 0.3108(4) 0.2171(7) 0.0519(5) 0.053(3) Uani 1 1 d . . . C27 C 0.3532(3) 0.2381(9) 0.0321(5) 0.067(3) Uani 1 1 d . . . C28 C 0.4351(6) 0.2776(16) 0.0000 0.094(7) Uani 1 2 d S . . C29 C 0.4763(7) 0.3165(17) 0.0000 0.108(7) Uani 1 2 d S . . C30 C 0.5472(4) 0.4040(13) -0.0325(6) 0.116(6) Uani 1 1 d . . . C31 C 0.5812(5) 0.4561(14) -0.0670(8) 0.132(7) Uani 1 1 d . . . H31A H 0.5803 0.4614 -0.1108 0.158 Uiso 1 1 calc R . . C32 C 0.6157(5) 0.4987(12) -0.0310(7) 0.124(6) Uani 1 1 d . . . H32A H 0.6398 0.5285 -0.0520 0.149 Uiso 1 1 calc R . . Cl1 Cl 0.18110(12) 0.1436(3) 0.0000 0.0582(11) Uani 1 2 d S . . N1 N 0.2860(4) 0.2069(9) 0.0000 0.057(3) Uani 1 2 d S . . H1N H 0.2571 0.1950 0.0000 0.068 Uiso 1 2 calc SR . . N2 N 0.2127(3) 0.2826(6) 0.1157(4) 0.050(2) Uani 1 1 d . . . H2N H 0.2004 0.2337 0.0973 0.060 Uiso 1 1 calc R . . N3 N 0.1405(3) 0.3663(8) 0.0000 0.046(3) Uani 1 2 d S . . H3N H 0.1453 0.3050 0.0000 0.055 Uiso 1 2 calc SR . . S1 S 0.30827(9) 0.4341(2) 0.19116(13) 0.0600(9) Uani 1 1 d . . . S2 S 0.22005(9) 0.5350(2) 0.19139(13) 0.0598(9) Uani 1 1 d . . . S3 S 0.27525(10) 0.7355(2) 0.21104(14) 0.0667(9) Uani 1 1 d . . . S4 S 0.36045(10) 0.6284(2) 0.20800(15) 0.0682(10) Uani 1 1 d . . . S5 S 0.40605(11) 0.2502(3) 0.06942(16) 0.1044(15) Uani 1 1 d . . . S6 S 0.50531(12) 0.3398(4) -0.06855(18) 0.141(2) Uani 1 1 d . . . S7 S 0.11849(10) 0.6194(2) 0.06908(14) 0.0638(9) Uani 1 1 d . . . S8 S 0.04925(11) 0.7964(2) 0.06807(18) 0.0822(11) Uani 1 1 d . . . N4 N 0.2414(3) 0.8040(7) 0.0000 0.064(4) Uani 1 2 d SD . . C1A C 0.2874(5) 0.8279(12) -0.0243(6) 0.072(8) Uani 0.50 1 d PD A -1 H1A1 H 0.2869 0.8941 -0.0390 0.086 Uiso 0.50 1 calc PR A -1 H1A2 H 0.2934 0.7874 -0.0607 0.086 Uiso 0.50 1 calc PR A -1 C2A C 0.3269(6) 0.8173(15) 0.0209(7) 0.067(7) Uani 0.50 1 d PD A -1 H2A1 H 0.3205 0.8522 0.0596 0.080 Uiso 0.50 1 calc PR A -1 H2A2 H 0.3312 0.7499 0.0313 0.080 Uiso 0.50 1 calc PR A -1 C3A C 0.3694(5) 0.8566(13) -0.0095(18) 0.071(9) Uani 0.50 1 d PD A -1 H3A1 H 0.3709 0.8361 -0.0533 0.085 Uiso 0.50 1 calc PR A -1 H3A2 H 0.3962 0.8323 0.0122 0.085 Uiso 0.50 1 calc PR A -1 C4A C 0.3684(7) 0.9648(13) -0.006(4) 0.096(14) Uani 0.50 1 d PD A -1 H4A1 H 0.3630 0.9845 0.0367 0.144 Uiso 0.50 1 calc PR A -1 H4A2 H 0.3444 0.9888 -0.0327 0.144 Uiso 0.50 1 calc PR A -1 H4A3 H 0.3972 0.9900 -0.0202 0.144 Uiso 0.50 1 calc PR A -1 C5A C 0.2426(5) 0.7071(10) 0.0305(6) 0.063(7) Uani 0.50 1 d PD A -1 H5A1 H 0.2129 0.6954 0.0494 0.076 Uiso 0.50 1 calc PR A -1 H5A2 H 0.2647 0.7093 0.0646 0.076 Uiso 0.50 1 calc PR A -1 C6A C 0.2540(7) 0.6225(10) -0.0107(9) 0.076(8) Uani 0.50 1 d PD A -1 H6A1 H 0.2823 0.6346 -0.0333 0.091 Uiso 0.50 1 calc PR A -1 H6A2 H 0.2299 0.6126 -0.0415 0.091 Uiso 0.50 1 calc PR A -1 C7A C 0.2590(8) 0.5341(10) 0.0299(7) 0.064(7) Uani 0.50 1 d PD A -1 H7A1 H 0.2855 0.5407 0.0571 0.077 Uiso 0.50 1 calc PR A -1 H7A2 H 0.2321 0.5263 0.0563 0.077 Uiso 0.50 1 calc PR A -1 C8A C 0.2646(7) 0.4477(10) -0.0123(10) 0.053(8) Uani 0.50 1 d PD A -1 H8A1 H 0.2359 0.4331 -0.0321 0.080 Uiso 0.50 1 calc PR A -1 H8A2 H 0.2744 0.3935 0.0124 0.080 Uiso 0.50 1 calc PR A -1 H8A3 H 0.2870 0.4614 -0.0441 0.080 Uiso 0.50 1 calc PR A -1 C9A C 0.2292(6) 0.8758(11) 0.0505(6) 0.074(9) Uani 0.50 1 d PD A -1 H9A1 H 0.2521 0.8716 0.0834 0.089 Uiso 0.50 1 calc PR A -1 H9A2 H 0.2315 0.9397 0.0322 0.089 Uiso 0.50 1 calc PR A -1 C10A C 0.1831(7) 0.8675(18) 0.0812(12) 0.061(9) Uani 0.50 1 d PD A -1 H10A H 0.1594 0.8753 0.0496 0.074 Uiso 0.50 1 calc PR A -1 H10B H 0.1798 0.8042 0.1000 0.074 Uiso 0.50 1 calc PR A -1 C11A C 0.1781(8) 0.9434(19) 0.1311(13) 0.074(12) Uani 0.50 1 d PD A -1 H11A H 0.1781 1.0067 0.1117 0.089 Uiso 0.50 1 calc PR A -1 H11B H 0.2037 0.9401 0.1602 0.089 Uiso 0.50 1 calc PR A -1 C12A C 0.1340(6) 0.9277(18) 0.1662(11) 0.072(8) Uani 0.50 1 d PD A -1 H12A H 0.1096 0.9188 0.1365 0.108 Uiso 0.50 1 calc PR A -1 H12B H 0.1277 0.9829 0.1922 0.108 Uiso 0.50 1 calc PR A -1 H12C H 0.1367 0.8715 0.1924 0.108 Uiso 0.50 1 calc PR A -1 C13A C 0.2069(5) 0.8056(12) -0.0501(7) 0.066(8) Uani 0.50 1 d PD A -1 H13A H 0.1778 0.7851 -0.0327 0.079 Uiso 0.50 1 calc PR A -1 H13B H 0.2155 0.7599 -0.0826 0.079 Uiso 0.50 1 calc PR A -1 C14A C 0.2012(8) 0.9031(14) -0.0794(13) 0.058(8) Uani 0.50 1 d PD A -1 H14D H 0.2292 0.9219 -0.1006 0.069 Uiso 0.50 1 calc PR A -1 H14E H 0.1946 0.9504 -0.0470 0.069 Uiso 0.50 1 calc PR A -1 C15A C 0.1626(8) 0.8998(17) -0.1263(12) 0.055(8) Uani 0.50 1 d PD A -1 H15D H 0.1709 0.8567 -0.1604 0.066 Uiso 0.50 1 calc PR A -1 H15E H 0.1358 0.8734 -0.1057 0.066 Uiso 0.50 1 calc PR A -1 C16A C 0.1514(10) 0.992(2) -0.1521(14) 0.087(11) Uani 0.50 1 d PD A -1 H16A H 0.1215 0.9888 -0.1708 0.130 Uiso 0.50 1 calc PR A -1 H16B H 0.1734 1.0086 -0.1838 0.130 Uiso 0.50 1 calc PR A -1 H16C H 0.1516 1.0391 -0.1192 0.130 Uiso 0.50 1 calc PR A -1 Cl1B Cl -0.0229(4) 0.6009(7) 0.0132(10) 0.222(6) Uiso 0.50 1 d PD B -1 Cl3B Cl 0.0020(4) 0.4530(7) -0.0708(6) 0.180(5) Uiso 0.50 1 d PD B -1 C1B C -0.0176(9) 0.4650(13) 0.0142(11) 0.158(14) Uiso 0.50 1 d PD B -1 Cl1C Cl 0.0088(3) 0.2942(7) 0.2064(5) 0.153(4) Uiso 0.50 1 d PD C -1 Cl2C Cl -0.0855(3) 0.3033(8) 0.2268(6) 0.182(5) Uiso 0.50 1 d PD C -1 Cl3C Cl -0.0269(5) 0.3829(13) 0.3150(7) 0.291(9) Uiso 0.50 1 d PD C -1 C1C C -0.0353(4) 0.390(2) 0.2260(10) 0.24(2) Uiso 0.50 1 d PD C -1 Cl1D Cl 0.0304(5) 0.0662(10) 0.2611(8) 0.229(6) Uiso 0.50 1 d PD D -1 C1D C 0.0540(13) -0.0616(18) 0.271(2) 0.061(12) Uiso 0.25 1 d PD D -1 Cl1E Cl 0.4950(6) 1.0461(9) 0.0648(8) 0.225(7) Uiso 0.50 1 d PD E -1 C1E C 0.4949(9) 0.9262(18) 0.0203(15) 0.130(13) Uiso 0.50 1 d PD E -1 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 0.054(6) 0.050(6) 0.042(6) 0.005(5) -0.006(5) -0.001(5) C2 0.065(7) 0.045(7) 0.038(7) -0.004(5) 0.005(6) 0.006(6) C3 0.064(7) 0.059(8) 0.029(6) 0.006(6) 0.005(5) -0.002(7) C4 0.050(6) 0.061(8) 0.030(6) 0.002(6) -0.002(5) 0.002(6) C5 0.060(7) 0.082(9) 0.024(6) 0.000(6) 0.007(5) 0.007(7) C6 0.065(7) 0.050(7) 0.034(7) 0.001(6) -0.007(5) -0.007(6) C7 0.078(8) 0.062(8) 0.035(7) -0.012(6) 0.002(6) -0.008(7) C8 0.053(7) 0.053(8) 0.042(7) -0.013(6) 0.002(5) 0.000(6) C9 0.078(9) 0.066(9) 0.048(8) 0.006(7) -0.009(6) 0.015(7) C10 0.104(10) 0.077(10) 0.037(7) 0.008(7) -0.017(7) -0.007(9) C11 0.093(10) 0.067(10) 0.045(8) 0.009(7) 0.003(7) -0.018(8) C12 0.064(8) 0.079(10) 0.061(9) -0.001(7) 0.002(6) 0.006(8) C13 0.065(7) 0.057(8) 0.037(7) 0.000(6) -0.007(5) 0.003(7) C14 0.075(8) 0.059(8) 0.052(8) 0.007(6) 0.003(6) -0.006(7) C15 0.070(7) 0.056(8) 0.047(7) 0.007(6) -0.018(6) 0.006(6) C16 0.056(7) 0.071(8) 0.030(6) 0.000(6) -0.002(5) -0.018(6) C17 0.064(7) 0.100(10) 0.033(7) -0.001(7) 0.017(5) 0.000(7) C18 0.057(7) 0.087(10) 0.041(7) 0.003(6) -0.002(5) 0.000(7) C19 0.061(7) 0.057(8) 0.044(8) -0.008(6) 0.003(5) 0.003(6) C20 0.043(6) 0.053(7) 0.052(7) -0.014(6) -0.001(5) 0.003(6) C21 0.075(11) 0.083(14) 0.042(11) 0.000 0.000 -0.021(11) C22 0.060(10) 0.079(14) 0.075(14) 0.000 0.000 -0.020(10) C23 0.050(7) 0.055(8) 0.127(13) -0.012(7) 0.020(7) -0.003(6) C24 0.062(8) 0.061(10) 0.152(15) -0.005(10) 0.000(9) -0.019(8) C25 0.072(8) 0.079(10) 0.17(2) -0.021(9) 0.006(9) -0.011(8) C26 0.055(7) 0.063(8) 0.039(7) -0.005(6) -0.006(5) 0.013(6) C27 0.052(7) 0.103(10) 0.046(7) 0.002(6) 0.000(5) -0.008(7) C28 0.059(11) 0.17(2) 0.052(13) 0.000 0.000 -0.035(13) C29 0.122(17) 0.17(2) 0.035(12) 0.000 0.000 -0.032(16) C30 0.058(8) 0.228(18) 0.062(9) -0.022(10) 0.000(6) -0.031(10) C31 0.072(10) 0.24(2) 0.080(12) 0.011(13) 0.008(9) -0.045(12) C32 0.071(9) 0.201(17) 0.099(13) 0.007(10) 0.022(8) -0.019(11) Cl1 0.063(2) 0.061(3) 0.051(3) 0.000 0.000 -0.004(2) N1 0.055(7) 0.082(10) 0.033(8) 0.000 0.000 0.004(7) N2 0.064(6) 0.053(6) 0.033(5) 0.003(4) -0.003(4) -0.007(5) N3 0.056(7) 0.039(8) 0.043(8) 0.000 0.000 0.008(6) S1 0.0664(18) 0.060(2) 0.0536(19) -0.0015(16) -0.0078(15) -0.0045(17) S2 0.0652(18) 0.064(2) 0.0499(19) -0.0065(16) 0.0034(15) -0.0021(16) S3 0.082(2) 0.068(2) 0.050(2) -0.0031(16) 0.0034(16) -0.0016(18) S4 0.0668(19) 0.066(2) 0.072(2) 0.0022(18) -0.0083(16) -0.0037(17) S5 0.062(2) 0.202(5) 0.049(2) 0.004(3) -0.0090(16) -0.028(2) S6 0.076(2) 0.295(7) 0.052(2) -0.005(3) 0.0081(19) -0.052(3) S7 0.0635(18) 0.064(2) 0.064(2) -0.0049(18) -0.0025(16) 0.0000(16) S8 0.073(2) 0.071(2) 0.102(3) -0.021(2) -0.003(2) 0.0054(19) N4 0.084(10) 0.044(9) 0.064(10) 0.000 0.000 -0.014(8) C1A 0.060(14) 0.086(18) 0.07(2) 0.010(12) 0.005(12) -0.014(14) C2A 0.081(15) 0.090(18) 0.029(16) 0.002(11) 0.009(11) 0.006(15) C3A 0.088(14) 0.102(18) 0.02(3) 0.013(16) -0.009(14) -0.004(13) C4A 0.098(16) 0.104(18) 0.09(4) -0.03(4) 0.05(4) -0.039(14) C5A 0.067(14) 0.074(18) 0.050(15) 0.001(13) 0.024(11) 0.004(14) C6A 0.082(14) 0.093(18) 0.05(2) 0.03(2) 0.013(17) -0.013(14) C7A 0.091(17) 0.052(15) 0.048(14) 0.032(13) -0.018(11) 0.004(14) C8A 0.116(15) 0.034(11) 0.01(2) 0.010(10) -0.030(12) -0.016(11) C9A 0.08(2) 0.13(3) 0.007(12) 0.008(15) 0.005(11) -0.007(19) C10A 0.08(2) 0.031(18) 0.07(2) -0.028(17) -0.019(17) -0.015(15) C11A 0.06(2) 0.10(3) 0.07(2) 0.03(2) -0.013(18) -0.044(19) C12A 0.08(2) 0.08(2) 0.061(19) -0.026(18) -0.024(14) 0.022(17) C13A 0.059(15) 0.10(2) 0.036(15) -0.027(15) -0.009(11) -0.028(16) C14A 0.10(2) 0.033(18) 0.038(17) 0.007(14) 0.012(16) -0.036(16) C15A 0.028(14) 0.08(2) 0.060(19) -0.017(17) -0.025(14) -0.005(15) C16A 0.11(3) 0.07(3) 0.08(3) 0.00(2) 0.03(2) 0.00(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 C1 N2 1.374(12) . ? C1 C2 1.404(13) . ? C1 C16 1.499(13) . ? C2 C3 1.375(13) . ? C2 S2 1.766(10) . ? C3 C4 1.409(13) . ? C3 S1 1.760(11) . ? C4 N2 1.358(11) . ? C4 C13 1.530(14) . ? C5 C6 1.319(13) . ? C5 S1 1.782(11) . ? C5 S2 1.784(11) . ? C6 S4 1.766(11) . ? C6 S3 1.771(11) . ? C7 C8 1.370(14) . ? C7 C12 1.404(15) . ? C7 S4 1.748(12) . ? C8 C9 1.393(14) . ? C8 S3 1.766(11) . ? C9 C10 1.434(15) . ? C9 H9 0.9500 . ? C10 C11 1.403(15) . ? C10 H10 0.9500 . ? C11 C12 1.392(15) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C26 1.520(14) . ? C13 C14 1.552(13) . ? C13 C15 1.560(13) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C18 1.536(13) . ? C16 C19 1.536(14) . ? C16 C17 1.560(13) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.350(13) . ? C19 N3 1.365(11) . ? C20 C20 1.42(2) 6 ? C20 S7 1.776(11) . ? C21 C22 1.40(2) . ? C21 S7 1.770(11) . ? C21 S7 1.770(11) 6 ? C22 S8 1.725(11) . ? C22 S8 1.725(11) 6 ? C23 C24 1.390(16) . ? C23 C23 1.45(3) 6 ? C23 S8 1.732(12) . ? C24 C25 1.394(17) . ? C24 H24A 0.9500 . ? C25 C25 1.30(3) 6 ? C25 H25A 0.9500 . ? C26 N1 1.350(11) . ? C26 C27 1.370(13) . ? C27 C27 1.39(2) 6 ? C27 S5 1.780(11) . ? C28 C29 1.35(2) . ? C28 S5 1.776(10) 6 ? C28 S5 1.776(10) . ? C29 S6 1.748(12) 6 ? C29 S6 1.748(12) . ? C30 C30 1.41(3) 6 ? C30 C31 1.459(18) . ? C30 S6 1.731(14) . ? C31 C32 1.425(18) . ? C31 H31A 0.9500 . ? C32 C32 1.34(3) 6 ? C32 H32A 0.9500 . ? N1 C26 1.350(11) 6 ? N1 H1N 0.8800 . ? N2 H2N 0.8800 . ? N3 C19 1.365(11) 6 ? N3 H3N 0.8800 . ? N4 C13A 1.494(12) 6 ? N4 C13A 1.494(12) . ? N4 C1A 1.509(12) . ? N4 C1A 1.509(12) 6 ? N4 C5A 1.524(12) 6 ? N4 C5A 1.524(12) . ? N4 C9A 1.536(12) 6 ? N4 C9A 1.536(12) . ? C1A C2A 1.538(11) . ? C1A H1A1 0.9900 . ? C1A H1A2 0.9900 . ? C2A C3A 1.534(11) . ? C2A H2A1 0.9900 . ? C2A H2A2 0.9900 . ? C3A C4A 1.534(11) . ? C3A H3A1 0.9900 . ? C3A H3A2 0.9900 . ? C4A H4A1 0.9800 . ? C4A H4A2 0.9800 . ? C4A H4A3 0.9800 . ? C5A C6A 1.532(11) . ? C5A H5A1 0.9900 . ? C5A H5A2 0.9900 . ? C6A C7A 1.536(11) . ? C6A H6A1 0.9900 . ? C6A H6A2 0.9900 . ? C7A C8A 1.535(10) . ? C7A H7A1 0.9900 . ? C7A H7A2 0.9900 . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? C9A C10A 1.531(10) . ? C9A H9A1 0.9900 . ? C9A H9A2 0.9900 . ? C10A C11A 1.530(11) . ? C10A H10A 0.9900 . ? C10A H10B 0.9900 . ? C11A C12A 1.536(11) . ? C11A H11A 0.9900 . ? C11A H11B 0.9900 . ? C12A H12A 0.9800 . ? C12A H12B 0.9800 . ? C12A H12C 0.9800 . ? C13A C14A 1.529(10) . ? C13A H13A 0.9900 . ? C13A H13B 0.9900 . ? C14A C15A 1.533(11) . ? C14A H14D 0.9900 . ? C14A H14E 0.9900 . ? C15A C16A 1.45(3) . ? C15A H15D 0.9900 . ? C15A H15E 0.9900 . ? C16A H16A 0.9800 . ? C16A H16B 0.9800 . ? C16A H16C 0.9800 . ? Cl1B C1B 1.932(17) . ? Cl3B C1B 1.936(18) . ? Cl1C C1C 1.941(18) . ? Cl2C C1C 1.940(18) . ? Cl3C C1C 1.940(18) . ? Cl1D C1D 1.955(18) . ? Cl1E C1E 1.952(18) . ? 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 N2 C1 C2 103.6(8) . . ? N2 C1 C16 123.4(10) . . ? C2 C1 C16 132.8(10) . . ? C3 C2 C1 109.2(9) . . ? C3 C2 S2 116.8(9) . . ? C1 C2 S2 133.9(9) . . ? C2 C3 C4 109.0(9) . . ? C2 C3 S1 117.9(9) . . ? C4 C3 S1 133.1(9) . . ? N2 C4 C3 103.8(9) . . ? N2 C4 C13 124.8(10) . . ? C3 C4 C13 131.3(9) . . ? C6 C5 S1 121.2(8) . . ? C6 C5 S2 124.2(9) . . ? S1 C5 S2 114.4(7) . . ? C5 C6 S4 122.2(8) . . ? C5 C6 S3 124.0(8) . . ? S4 C6 S3 113.8(6) . . ? C8 C7 C12 120.0(11) . . ? C8 C7 S4 117.5(9) . . ? C12 C7 S4 122.5(10) . . ? C7 C8 C9 122.5(10) . . ? C7 C8 S3 116.4(9) . . ? C9 C8 S3 121.0(9) . . ? C8 C9 C10 116.6(11) . . ? C8 C9 H9 121.7 . . ? C10 C9 H9 121.7 . . ? C11 C10 C9 121.9(12) . . ? C11 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? C12 C11 C10 118.4(12) . . ? C12 C11 H11 120.8 . . ? C10 C11 H11 120.8 . . ? C11 C12 C7 120.6(12) . . ? C11 C12 H12 119.7 . . ? C7 C12 H12 119.7 . . ? C26 C13 C4 111.6(8) . . ? C26 C13 C14 108.1(8) . . ? C4 C13 C14 110.2(8) . . ? C26 C13 C15 109.0(9) . . ? C4 C13 C15 109.9(9) . . ? C14 C13 C15 108.0(8) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C1 C16 C18 110.6(9) . . ? C1 C16 C19 109.7(8) . . ? C18 C16 C19 110.7(8) . . ? C1 C16 C17 109.2(9) . . ? C18 C16 C17 107.4(8) . . ? C19 C16 C17 109.1(9) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 N3 106.2(10) . . ? C20 C19 C16 132.5(10) . . ? N3 C19 C16 121.3(10) . . ? C19 C20 C20 108.0(6) . 6 ? C19 C20 S7 135.9(9) . . ? C20 C20 S7 116.1(4) 6 . ? C22 C21 S7 122.5(5) . . ? C22 C21 S7 122.5(5) . 6 ? S7 C21 S7 115.0(11) . 6 ? C21 C22 S8 121.5(6) . . ? C21 C22 S8 121.5(6) . 6 ? S8 C22 S8 117.0(12) . 6 ? C24 C23 C23 120.3(9) . 6 ? C24 C23 S8 124.1(11) . . ? C23 C23 S8 115.5(4) 6 . ? C23 C24 C25 115.8(15) . . ? C23 C24 H24A 122.1 . . ? C25 C24 H24A 122.1 . . ? C25 C25 C24 123.9(9) 6 . ? C25 C25 H25A 118.1 6 . ? C24 C25 H25A 118.1 . . ? N1 C26 C27 105.6(10) . . ? N1 C26 C13 122.6(9) . . ? C27 C26 C13 131.8(9) . . ? C26 C27 C27 108.2(6) . 6 ? C26 C27 S5 134.3(8) . . ? C27 C27 S5 116.9(3) 6 . ? C29 C28 S5 122.4(5) . 6 ? C29 C28 S5 122.4(5) . . ? S5 C28 S5 115.2(10) 6 . ? C28 C29 S6 122.0(6) . 6 ? C28 C29 S6 122.0(6) . . ? S6 C29 S6 115.9(13) 6 . ? C30 C30 C31 120.7(8) 6 . ? C30 C30 S6 116.7(5) 6 . ? C31 C30 S6 122.6(11) . . ? C32 C31 C30 116.1(14) . . ? C32 C31 H31A 122.0 . . ? C30 C31 H31A 122.0 . . ? C32 C32 C31 123.0(9) 6 . ? C32 C32 H32A 118.5 6 . ? C31 C32 H32A 118.5 . . ? C26 N1 C26 112.3(13) . 6 ? C26 N1 H1N 123.8 . . ? C26 N1 H1N 123.8 6 . ? C4 N2 C1 114.4(9) . . ? C4 N2 H2N 122.8 . . ? C1 N2 H2N 122.8 . . ? C19 N3 C19 111.6(13) . 6 ? C19 N3 H3N 124.2 . . ? C19 N3 H3N 124.2 6 . ? C3 S1 C5 93.0(5) . . ? C2 S2 C5 93.5(5) . . ? C8 S3 C6 93.9(5) . . ? C7 S4 C6 94.0(6) . . ? C28 S5 C27 94.1(6) . . ? C30 S6 C29 94.4(8) . . ? C21 S7 C20 93.2(7) . . ? C22 S8 C23 94.2(7) . . ? C13A N4 C1A 111.8(5) . . ? C13A N4 C5A 110.1(5) . . ? C1A N4 C5A 109.4(5) . . ? C13A N4 C9A 109.9(5) . . ? C1A N4 C9A 108.3(5) . . ? C5A N4 C9A 107.2(5) . . ? N4 C1A C2A 117.0(11) . . ? N4 C1A H1A1 108.0 . . ? C2A C1A H1A1 108.0 . . ? N4 C1A H1A2 108.0 . . ? C2A C1A H1A2 108.0 . . ? H1A1 C1A H1A2 107.3 . . ? C3A C2A C1A 109.1(11) . . ? C3A C2A H2A1 109.9 . . ? C1A C2A H2A1 109.9 . . ? C3A C2A H2A2 109.9 . . ? C1A C2A H2A2 109.9 . . ? H2A1 C2A H2A2 108.3 . . ? C2A C3A C4A 109.0(11) . . ? C2A C3A H3A1 109.9 . . ? C4A C3A H3A1 109.9 . . ? C2A C3A H3A2 109.9 . . ? C4A C3A H3A2 109.9 . . ? H3A1 C3A H3A2 108.3 . . ? N4 C5A C6A 117.3(10) . . ? N4 C5A H5A1 108.0 . . ? C6A C5A H5A1 108.0 . . ? N4 C5A H5A2 108.0 . . ? C6A C5A H5A2 108.0 . . ? H5A1 C5A H5A2 107.2 . . ? C5A C6A C7A 109.1(12) . . ? C5A C6A H6A1 109.9 . . ? C7A C6A H6A1 109.9 . . ? C5A C6A H6A2 109.9 . . ? C7A C6A H6A2 109.9 . . ? H6A1 C6A H6A2 108.3 . . ? C8A C7A C6A 108.7(11) . . ? C8A C7A H7A1 109.9 . . ? C6A C7A H7A1 109.9 . . ? C8A C7A H7A2 109.9 . . ? C6A C7A H7A2 109.9 . . ? H7A1 C7A H7A2 108.3 . . ? C10A C9A N4 118.0(10) . . ? C10A C9A H9A1 107.8 . . ? N4 C9A H9A1 107.8 . . ? C10A C9A H9A2 107.8 . . ? N4 C9A H9A2 107.8 . . ? H9A1 C9A H9A2 107.1 . . ? C11A C10A C9A 109.8(10) . . ? C11A C10A H10A 109.7 . . ? C9A C10A H10A 109.7 . . ? C11A C10A H10B 109.7 . . ? C9A C10A H10B 109.7 . . ? H10A C10A H10B 108.2 . . ? C10A C11A C12A 109.3(11) . . ? C10A C11A H11A 109.8 . . ? C12A C11A H11A 109.8 . . ? C10A C11A H11B 109.8 . . ? C12A C11A H11B 109.8 . . ? H11A C11A H11B 108.3 . . ? N4 C13A C14A 113.0(11) . . ? N4 C13A H13A 109.0 . . ? C14A C13A H13A 109.0 . . ? N4 C13A H13B 109.0 . . ? C14A C13A H13B 109.0 . . ? H13A C13A H13B 107.8 . . ? C13A C14A C15A 109.3(10) . . ? C13A C14A H14D 109.8 . . ? C15A C14A H14D 109.8 . . ? C13A C14A H14E 109.8 . . ? C15A C14A H14E 109.8 . . ? H14D C14A H14E 108.3 . . ? C16A C15A C14A 113.6(17) . . ? C16A C15A H15D 108.9 . . ? C14A C15A H15D 108.9 . . ? C16A C15A H15E 108.9 . . ? C14A C15A H15E 108.9 . . ? H15D C15A H15E 107.7 . . ? Cl1B C1B Cl3B 95.8(12) . . ? Cl2C C1C Cl3C 93.3(12) . . ? Cl2C C1C Cl1C 94.7(12) . . ? Cl3C C1C Cl1C 95.3(12) . . ? 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 N2 C1 C2 C3 0.1(11) . . . . ? C16 C1 C2 C3 -173.7(10) . . . . ? N2 C1 C2 S2 177.9(8) . . . . ? C16 C1 C2 S2 4.1(19) . . . . ? C1 C2 C3 C4 -0.3(12) . . . . ? S2 C2 C3 C4 -178.5(7) . . . . ? C1 C2 C3 S1 -178.1(7) . . . . ? S2 C2 C3 S1 3.7(11) . . . . ? C2 C3 C4 N2 0.4(11) . . . . ? S1 C3 C4 N2 177.7(8) . . . . ? C2 C3 C4 C13 -179.4(10) . . . . ? S1 C3 C4 C13 -2.1(17) . . . . ? S1 C5 C6 S4 2.9(12) . . . . ? S2 C5 C6 S4 177.7(5) . . . . ? S1 C5 C6 S3 -176.1(5) . . . . ? S2 C5 C6 S3 -1.3(13) . . . . ? C12 C7 C8 C9 -2.3(16) . . . . ? S4 C7 C8 C9 176.5(8) . . . . ? C12 C7 C8 S3 -180.0(8) . . . . ? S4 C7 C8 S3 -1.2(11) . . . . ? C7 C8 C9 C10 2.4(15) . . . . ? S3 C8 C9 C10 180.0(8) . . . . ? C8 C9 C10 C11 -0.8(16) . . . . ? C9 C10 C11 C12 -1.0(17) . . . . ? C10 C11 C12 C7 1.2(16) . . . . ? C8 C7 C12 C11 0.4(16) . . . . ? S4 C7 C12 C11 -178.3(9) . . . . ? N2 C4 C13 C26 87.7(12) . . . . ? C3 C4 C13 C26 -92.6(13) . . . . ? N2 C4 C13 C14 -32.5(13) . . . . ? C3 C4 C13 C14 147.2(10) . . . . ? N2 C4 C13 C15 -151.4(9) . . . . ? C3 C4 C13 C15 28.4(15) . . . . ? N2 C1 C16 C18 36.5(13) . . . . ? C2 C1 C16 C18 -150.8(11) . . . . ? N2 C1 C16 C19 -85.9(12) . . . . ? C2 C1 C16 C19 86.9(14) . . . . ? N2 C1 C16 C17 154.5(9) . . . . ? C2 C1 C16 C17 -32.7(16) . . . . ? C1 C16 C19 C20 -101.0(14) . . . . ? C18 C16 C19 C20 136.7(12) . . . . ? C17 C16 C19 C20 18.7(16) . . . . ? C1 C16 C19 N3 79.1(13) . . . . ? C18 C16 C19 N3 -43.2(13) . . . . ? C17 C16 C19 N3 -161.2(10) . . . . ? N3 C19 C20 C20 -0.5(9) . . . 6 ? C16 C19 C20 C20 179.6(10) . . . 6 ? N3 C19 C20 S7 178.6(9) . . . . ? C16 C19 C20 S7 -1(2) . . . . ? S7 C21 C22 S8 -1(2) . . . . ? S7 C21 C22 S8 178.6(8) 6 . . . ? S7 C21 C22 S8 -178.6(8) . . . 6 ? S7 C21 C22 S8 1(2) 6 . . 6 ? C23 C23 C24 C25 2.5(13) 6 . . . ? S8 C23 C24 C25 178.7(9) . . . . ? C23 C24 C25 C25 -2.6(14) . . . 6 ? C4 C13 C26 N1 -65.5(14) . . . . ? C14 C13 C26 N1 55.9(13) . . . . ? C15 C13 C26 N1 173.0(10) . . . . ? C4 C13 C26 C27 112.6(13) . . . . ? C14 C13 C26 C27 -126.0(13) . . . . ? C15 C13 C26 C27 -8.9(17) . . . . ? N1 C26 C27 C27 -1.2(10) . . . 6 ? C13 C26 C27 C27 -179.5(10) . . . 6 ? N1 C26 C27 S5 -172.5(11) . . . . ? C13 C26 C27 S5 9(2) . . . . ? S5 C28 C29 S6 -178.0(13) 6 . . 6 ? S5 C28 C29 S6 2(3) . . . 6 ? S5 C28 C29 S6 -2(3) 6 . . . ? S5 C28 C29 S6 178.0(13) . . . . ? C30 C30 C31 C32 5(2) 6 . . . ? S6 C30 C31 C32 -174.7(13) . . . . ? C30 C31 C32 C32 -5(2) . . . 6 ? C27 C26 N1 C26 2.1(17) . . . 6 ? C13 C26 N1 C26 -179.4(6) . . . 6 ? C3 C4 N2 C1 -0.4(11) . . . . ? C13 C4 N2 C1 179.4(9) . . . . ? C2 C1 N2 C4 0.2(11) . . . . ? C16 C1 N2 C4 174.7(9) . . . . ? C20 C19 N3 C19 0.9(16) . . . 6 ? C16 C19 N3 C19 -179.2(6) . . . 6 ? C2 C3 S1 C5 -14.8(9) . . . . ? C4 C3 S1 C5 168.1(10) . . . . ? C6 C5 S1 C3 -163.8(9) . . . . ? S2 C5 S1 C3 20.9(6) . . . . ? C3 C2 S2 C5 9.5(9) . . . . ? C1 C2 S2 C5 -168.1(11) . . . . ? C6 C5 S2 C2 165.4(9) . . . . ? S1 C5 S2 C2 -19.5(6) . . . . ? C7 C8 S3 C6 -11.4(9) . . . . ? C9 C8 S3 C6 170.9(9) . . . . ? C5 C6 S3 C8 -161.0(9) . . . . ? S4 C6 S3 C8 20.0(6) . . . . ? C8 C7 S4 C6 13.1(9) . . . . ? C12 C7 S4 C6 -168.2(9) . . . . ? C5 C6 S4 C7 160.5(9) . . . . ? S3 C6 S4 C7 -20.4(6) . . . . ? C29 C28 S5 C27 164(2) . . . . ? S5 C28 S5 C27 -15.9(13) 6 . . . ? C26 C27 S5 C28 -179.8(15) . . . . ? C27 C27 S5 C28 9.5(8) 6 . . . ? C30 C30 S6 C29 8.0(9) 6 . . . ? C31 C30 S6 C29 -172.0(16) . . . . ? C28 C29 S6 C30 170(2) . . . . ? S6 C29 S6 C30 -13.5(15) 6 . . . ? C22 C21 S7 C20 155.0(13) . . . . ? S7 C21 S7 C20 -24.8(9) 6 . . . ? C19 C20 S7 C21 -164.6(12) . . . . ? C20 C20 S7 C21 14.6(5) 6 . . . ? C21 C22 S8 C23 -158.4(13) . . . . ? S8 C22 S8 C23 19.0(10) 6 . . . ? C24 C23 S8 C22 172.8(11) . . . . ? C23 C23 S8 C22 -10.9(6) 6 . . . ? C13A N4 C1A C2A 40(2) 6 . . . ? C13A N4 C1A C2A -172.9(15) . . . . ? C1A N4 C1A C2A 18.3(16) 6 . . . ? C5A N4 C1A C2A -100.0(16) 6 . . . ? C5A N4 C1A C2A -50.7(16) . . . . ? C9A N4 C1A C2A 152.9(17) 6 . . . ? C9A N4 C1A C2A 65.8(16) . . . . ? N4 C1A C2A C3A -172.8(13) . . . . ? C1A C2A C3A C4A 78(3) . . . . ? C13A N4 C5A C6A 147.2(18) 6 . . . ? C13A N4 C5A C6A 60.3(16) . . . . ? C1A N4 C5A C6A -63.0(16) . . . . ? C1A N4 C5A C6A -100.5(17) 6 . . . ? C5A N4 C5A C6A 13.1(16) 6 . . . ? C9A N4 C5A C6A 45(3) 6 . . . ? C9A N4 C5A C6A 179.8(15) . . . . ? N4 C5A C6A C7A 173.3(15) . . . . ? C5A C6A C7A C8A 173.0(17) . . . . ? C13A N4 C9A C10A -18.2(17) 6 . . . ? C13A N4 C9A C10A 56(2) . . . . ? C1A N4 C9A C10A 178.4(19) . . . . ? C1A N4 C9A C10A -152(2) 6 . . . ? C5A N4 C9A C10A -38(3) 6 . . . ? C5A N4 C9A C10A -64(2) . . . . ? C9A N4 C9A C10A 99.2(19) 6 . . . ? N4 C9A C10A C11A 178(2) . . . . ? C9A C10A C11A C12A -174(3) . . . . ? C13A N4 C13A C14A 102.0(17) 6 . . . ? C1A N4 C13A C14A -62.7(18) . . . . ? C1A N4 C13A C14A -47(3) 6 . . . ? C5A N4 C13A C14A -147.9(19) 6 . . . ? C5A N4 C13A C14A 175.4(17) . . . . ? C9A N4 C13A C14A -13.1(16) 6 . . . ? C9A N4 C13A C14A 57.6(18) . . . . ? N4 C13A C14A C15A -175(2) . . . . ? C13A C14A C15A C16A 174(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N Cl1 0.88 2.38 3.259(13) 173 . N2 H2N Cl1 0.88 2.53 3.319(9) 150 . N3 H3N Cl1 0.88 2.52 3.380(12) 164 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.476 _refine_diff_density_min -0.940 _refine_diff_density_rms 0.155