data_sio28 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34.38 H41.75 Cl2.75 N O6' _chemical_formula_weight 662.43 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' 'O' 'O' 0.0492 0.0322 '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 Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.7897(12) _cell_length_b 14.5693(14) _cell_length_c 19.106(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.564(6) _cell_angle_gamma 90.00 _cell_volume 3266.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9909 _cell_measurement_theta_min 3.82 _cell_measurement_theta_max 65.56 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1399 _exptl_absorpt_coefficient_mu 2.728 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5981 _exptl_absorpt_correction_T_max 0.8757 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_number 34969 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 65.89 _reflns_number_total 10167 _reflns_number_gt 9769 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0915P)^2^+2.0814P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.030(14) _refine_ls_number_reflns 10167 _refine_ls_number_parameters 830 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1394 _refine_ls_wR_factor_gt 0.1375 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.054 _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 O1 O 0.45507(18) 0.79321(17) 0.32141(12) 0.0232(5) Uani 1 1 d . . . O2 O 0.16703(18) 0.62627(18) 0.12792(12) 0.0248(5) Uani 1 1 d . . . O3 O -0.07190(18) 0.73236(17) 0.32400(12) 0.0228(5) Uani 1 1 d . . . H3 H -0.1145 0.7226 0.2869 0.034 Uiso 1 1 calc R . . O4 O -0.05602(18) 0.73097(18) 0.14714(12) 0.0266(5) Uani 1 1 d . . . O5 O 0.43875(19) 0.60745(18) 0.39823(12) 0.0252(5) Uani 1 1 d . . . O6 O 0.73811(17) 0.71952(17) 0.23411(13) 0.0245(5) Uani 1 1 d . . . N1 N 0.5466(2) 0.72817(19) 0.20569(14) 0.0172(5) Uani 1 1 d . . . H1 H 0.5492 0.7712 0.1735 0.021 Uiso 1 1 calc R . . C1 C 0.3919(2) 0.7455(2) 0.28222(15) 0.0165(6) Uani 1 1 d . . . C2 C 0.4404(2) 0.6887(2) 0.22432(15) 0.0152(6) Uani 1 1 d . . . C3 C 0.3537(2) 0.6810(2) 0.15939(15) 0.0156(6) Uani 1 1 d . . . H3B H 0.3581 0.7380 0.1316 0.019 Uiso 1 1 calc R . . H3A H 0.3777 0.6298 0.1301 0.019 Uiso 1 1 calc R . . C4 C 0.2310(2) 0.6658(2) 0.17144(15) 0.0154(6) Uani 1 1 d . . . C5 C 0.1900(2) 0.7038(2) 0.23694(15) 0.0140(6) Uani 1 1 d . . . C6 C 0.2691(2) 0.7397(2) 0.29031(16) 0.0149(6) Uani 1 1 d . . . C7 C 0.2296(3) 0.7713(2) 0.35252(16) 0.0189(6) Uani 1 1 d . . . H7 H 0.2826 0.7959 0.3883 0.023 Uiso 1 1 calc R . . C8 C 0.1163(3) 0.7677(2) 0.36348(16) 0.0194(6) Uani 1 1 d . . . C9 C 0.0374(2) 0.7348(2) 0.30915(16) 0.0163(6) Uani 1 1 d . . . C10 C 0.0737(2) 0.7032(2) 0.24642(15) 0.0164(6) Uani 1 1 d . . . C11 C -0.0148(2) 0.6729(2) 0.18844(16) 0.0207(7) Uani 1 1 d . . . C12 C -0.0557(3) 0.5773(3) 0.1863(2) 0.0279(8) Uani 1 1 d . . . C13 C -0.0149(3) 0.5223(2) 0.2394(2) 0.0252(7) Uani 1 1 d . . . H13 H 0.0387 0.5510 0.2728 0.030 Uiso 1 1 calc R . . C14 C -0.0382(3) 0.4268(3) 0.2550(2) 0.0346(9) Uani 1 1 d . . . C15 C 0.0076(3) 0.3896(3) 0.3147(3) 0.0382(10) Uani 1 1 d . . . H15 H -0.0107 0.3269 0.3211 0.046 Uiso 1 1 calc R . . C16 C 0.0853(3) 0.4324(3) 0.3748(2) 0.0363(9) Uani 1 1 d . . . H16 H 0.0419 0.4824 0.3962 0.044 Uiso 1 1 calc R . . C17 C 0.1927(3) 0.4739(2) 0.35043(18) 0.0236(7) Uani 1 1 d . . . H17 H 0.2115 0.4570 0.3050 0.028 Uiso 1 1 calc R . . C18 C 0.2627(3) 0.5316(2) 0.38669(17) 0.0221(7) Uani 1 1 d . . . C19 C 0.3723(3) 0.5611(2) 0.36034(16) 0.0190(7) Uani 1 1 d . . . C20 C 0.4016(2) 0.5310(2) 0.28776(15) 0.0156(6) Uani 1 1 d . . . H20 H 0.3287 0.5321 0.2563 0.019 Uiso 1 1 calc R . . C21 C 0.4861(2) 0.5931(2) 0.25304(16) 0.0164(6) Uani 1 1 d . . . H21 H 0.5037 0.5586 0.2102 0.020 Uiso 1 1 calc R . . C22 C 0.6040(2) 0.6189(2) 0.29037(16) 0.0188(6) Uani 1 1 d . . . H22 H 0.5907 0.6489 0.3359 0.023 Uiso 1 1 calc R . . C23 C 0.6401(3) 0.6936(2) 0.24164(16) 0.0191(6) Uani 1 1 d . . . C24 C 0.0733(3) 0.7989(3) 0.43079(18) 0.0283(8) Uani 1 1 d . . . H24A H 0.0355 0.7476 0.4522 0.042 Uiso 1 1 calc R . . H24B H 0.0189 0.8492 0.4210 0.042 Uiso 1 1 calc R . . H24C H 0.1375 0.8202 0.4631 0.042 Uiso 1 1 calc R . . C25 C -0.1410(4) 0.5554(4) 0.1258(3) 0.0520(12) Uani 1 1 d . . . H25A H -0.1110 0.5068 0.0973 0.078 Uiso 1 1 calc R . . H25C H -0.1561 0.6104 0.0970 0.078 Uiso 1 1 calc R . . H25B H -0.2119 0.5345 0.1435 0.078 Uiso 1 1 calc R . . C26 C -0.1133(4) 0.3685(3) 0.2057(3) 0.0549(14) Uani 1 1 d . . . H26B H -0.1204 0.3073 0.2262 0.082 Uiso 1 1 calc R . . H26A H -0.0800 0.3631 0.1609 0.082 Uiso 1 1 calc R . . H26C H -0.1889 0.3968 0.1977 0.082 Uiso 1 1 calc R . . C27 C 0.1184(4) 0.3599(4) 0.4323(3) 0.0553(13) Uani 1 1 d . . . H27A H 0.1581 0.3088 0.4119 0.083 Uiso 1 1 calc R . . H27B H 0.0495 0.3370 0.4512 0.083 Uiso 1 1 calc R . . H27C H 0.1687 0.3879 0.4702 0.083 Uiso 1 1 calc R . . C28 C 0.2432(3) 0.5686(3) 0.45828(19) 0.0337(9) Uani 1 1 d . . . H28A H 0.1627 0.5614 0.4660 0.051 Uiso 1 1 calc R . . H28C H 0.2638 0.6337 0.4609 0.051 Uiso 1 1 calc R . . H28B H 0.2905 0.5345 0.4945 0.051 Uiso 1 1 calc R . . C29 C 0.4428(3) 0.4303(2) 0.29070(18) 0.0234(7) Uani 1 1 d . . . H29C H 0.5086 0.4244 0.3259 0.035 Uiso 1 1 calc R . . H29B H 0.4649 0.4121 0.2445 0.035 Uiso 1 1 calc R . . H29A H 0.3812 0.3904 0.3035 0.035 Uiso 1 1 calc R . . C30 C 0.6911(3) 0.5425(3) 0.3070(2) 0.0295(8) Uani 1 1 d . . . H30A H 0.6708 0.4894 0.2759 0.035 Uiso 1 1 calc R . . H30B H 0.7672 0.5645 0.2968 0.035 Uiso 1 1 calc R . . C31 C 0.6973(3) 0.5110(4) 0.3830(2) 0.0422(11) Uani 1 1 d . . . H31 H 0.6174 0.5079 0.3962 0.051 Uiso 1 1 calc R . . C32 C 0.7486(4) 0.4144(5) 0.3932(3) 0.074(2) Uani 1 1 d . . . H32C H 0.8286 0.4156 0.3834 0.112 Uiso 1 1 calc R . . H32A H 0.7061 0.3715 0.3610 0.112 Uiso 1 1 calc R . . H32B H 0.7437 0.3944 0.4418 0.112 Uiso 1 1 calc R . . C33 C 0.7619(4) 0.5835(5) 0.4324(3) 0.073(2) Uani 1 1 d . . . H33B H 0.7574 0.5659 0.4815 0.110 Uiso 1 1 calc R . . H33A H 0.7268 0.6439 0.4239 0.110 Uiso 1 1 calc R . . H33C H 0.8419 0.5861 0.4227 0.110 Uiso 1 1 calc R . . O1' O 1.08708(18) 0.42200(16) 0.76074(11) 0.0200(5) Uani 1 1 d . . . O2' O 0.86525(18) 0.41623(17) 0.99259(11) 0.0216(5) Uani 1 1 d . . . O3' O 0.56445(17) 0.47937(17) 0.78458(12) 0.0211(5) Uani 1 1 d . . . H3' H 0.5335 0.4682 0.8215 0.032 Uiso 1 1 calc R . . O4' O 0.62698(19) 0.35957(16) 0.93516(12) 0.0237(5) Uani 1 1 d . . . O5' O 1.06328(17) 0.63149(16) 0.77971(11) 0.0188(4) Uani 1 1 d . . . O6' O 1.39640(17) 0.41340(15) 0.85424(12) 0.0204(5) Uani 1 1 d . . . N1' N 1.2156(2) 0.38647(19) 0.88241(14) 0.0180(5) Uani 1 1 d . . . H1' H 1.2238 0.3272 0.8903 0.022 Uiso 1 1 calc R . . C1' C 1.0391(2) 0.4314(2) 0.81363(15) 0.0151(6) Uani 1 1 d . . . C2' C 1.1076(2) 0.4357(2) 0.88617(16) 0.0165(6) Uani 1 1 d . . . C3' C 1.0406(2) 0.3957(2) 0.94392(16) 0.0201(6) Uani 1 1 d . . . H3'A H 1.0493 0.3282 0.9435 0.024 Uiso 1 1 calc R . . H3'B H 1.0762 0.4180 0.9899 0.024 Uiso 1 1 calc R . . C4' C 0.9147(2) 0.4176(2) 0.93938(16) 0.0154(6) Uani 1 1 d . . . C5' C 0.8531(2) 0.4368(2) 0.86956(15) 0.0143(6) Uani 1 1 d . . . C6' C 0.9132(2) 0.4433(2) 0.80980(16) 0.0156(6) Uani 1 1 d . . . C7' C 0.8551(3) 0.4624(2) 0.74487(16) 0.0160(6) Uani 1 1 d . . . H7' H 0.8966 0.4664 0.7048 0.019 Uiso 1 1 calc R . . C8' C 0.7382(3) 0.4759(2) 0.73663(16) 0.0174(6) Uani 1 1 d . . . C9' C 0.6777(3) 0.4666(2) 0.79668(16) 0.0164(6) Uani 1 1 d . . . C10' C 0.7340(3) 0.4485(2) 0.86282(16) 0.0146(6) Uani 1 1 d . . . C11' C 0.6631(2) 0.4355(2) 0.92407(15) 0.0163(6) Uani 1 1 d . . . C12' C 0.6309(2) 0.5163(2) 0.96524(16) 0.0166(6) Uani 1 1 d . . . C13' C 0.6667(2) 0.5999(2) 0.94692(16) 0.0161(6) Uani 1 1 d . . . H13A H 0.7102 0.5997 0.9076 0.019 Uiso 1 1 calc R . . C14' C 0.6505(2) 0.6910(2) 0.97669(15) 0.0177(6) Uani 1 1 d . . . C15' C 0.6866(3) 0.7665(2) 0.94581(17) 0.0198(6) Uani 1 1 d . . . H15A H 0.6762 0.8228 0.9694 0.024 Uiso 1 1 calc R . . C16' C 0.7420(3) 0.7729(2) 0.87773(17) 0.0190(6) Uani 1 1 d . . . H16A H 0.6871 0.7488 0.8389 0.023 Uiso 1 1 calc R . . C17' C 0.8503(2) 0.7169(2) 0.87988(16) 0.0177(6) Uani 1 1 d . . . H17A H 0.8877 0.7023 0.9248 0.021 Uiso 1 1 calc R . . C18' C 0.8974(2) 0.6864(2) 0.82358(15) 0.0164(6) Uani 1 1 d . . . C19' C 1.0115(2) 0.6415(2) 0.83118(15) 0.0144(6) Uani 1 1 d . . . C20' C 1.0656(2) 0.6117(2) 0.90405(16) 0.0166(6) Uani 1 1 d . . . H20A H 1.0024 0.5884 0.9306 0.020 Uiso 1 1 calc R . . C21' C 1.1541(2) 0.5342(2) 0.90395(16) 0.0158(6) Uani 1 1 d . . . H21A H 1.1868 0.5299 0.9541 0.019 Uiso 1 1 calc R . . C22' C 1.2592(2) 0.5401(2) 0.86226(16) 0.0169(6) Uani 1 1 d . . . H22A H 1.2308 0.5528 0.8122 0.020 Uiso 1 1 calc R . . C23' C 1.3003(2) 0.4413(2) 0.86569(15) 0.0166(6) Uani 1 1 d . . . C24' C 0.6756(3) 0.4992(3) 0.66687(17) 0.0248(7) Uani 1 1 d . . . H24E H 0.7299 0.5033 0.6313 0.037 Uiso 1 1 calc R . . H24F H 0.6367 0.5582 0.6702 0.037 Uiso 1 1 calc R . . H24D H 0.6194 0.4513 0.6535 0.037 Uiso 1 1 calc R . . C25' C 0.5579(3) 0.4923(3) 1.02346(18) 0.0266(7) Uani 1 1 d . . . H25D H 0.5191 0.4338 1.0126 0.040 Uiso 1 1 calc R . . H25E H 0.5011 0.5407 1.0275 0.040 Uiso 1 1 calc R . . H25F H 0.6062 0.4869 1.0680 0.040 Uiso 1 1 calc R . . C26' C 0.5911(3) 0.7030(3) 1.04263(17) 0.0252(7) Uani 1 1 d . . . H26D H 0.5126 0.6807 1.0343 0.038 Uiso 1 1 calc R . . H26F H 0.5906 0.7682 1.0553 0.038 Uiso 1 1 calc R . . H26E H 0.6316 0.6680 1.0811 0.038 Uiso 1 1 calc R . . C27' C 0.7674(3) 0.8738(2) 0.86195(18) 0.0246(7) Uani 1 1 d . . . H27F H 0.8265 0.8969 0.8971 0.037 Uiso 1 1 calc R . . H27E H 0.6978 0.9103 0.8636 0.037 Uiso 1 1 calc R . . H27D H 0.7939 0.8786 0.8151 0.037 Uiso 1 1 calc R . . C28' C 0.8438(2) 0.6996(2) 0.74933(16) 0.0194(6) Uani 1 1 d . . . H28F H 0.8600 0.7618 0.7334 0.029 Uiso 1 1 calc R . . H28E H 0.7612 0.6910 0.7479 0.029 Uiso 1 1 calc R . . H28D H 0.8755 0.6547 0.7184 0.029 Uiso 1 1 calc R . . C29' C 1.1176(3) 0.6958(2) 0.94493(16) 0.0211(6) Uani 1 1 d . . . H29E H 1.1776 0.7227 0.9193 0.032 Uiso 1 1 calc R . . H29F H 1.1501 0.6765 0.9917 0.032 Uiso 1 1 calc R . . H29D H 1.0579 0.7417 0.9496 0.032 Uiso 1 1 calc R . . C30' C 1.3495(3) 0.6126(2) 0.88416(17) 0.0197(6) Uani 1 1 d . . . H30D H 1.3400 0.6328 0.9327 0.024 Uiso 1 1 calc R . . H30C H 1.4259 0.5843 0.8845 0.024 Uiso 1 1 calc R . . C31' C 1.3442(3) 0.6968(2) 0.83611(19) 0.0249(7) Uani 1 1 d . . . H31A H 1.2621 0.7092 0.8209 0.030 Uiso 1 1 calc R . . C32' C 1.3929(3) 0.7818(3) 0.8745(2) 0.0364(9) Uani 1 1 d . . . H32F H 1.4736 0.7716 0.8901 0.055 Uiso 1 1 calc R . . H32E H 1.3509 0.7939 0.9153 0.055 Uiso 1 1 calc R . . H32D H 1.3856 0.8346 0.8426 0.055 Uiso 1 1 calc R . . C33' C 1.4036(4) 0.6789(3) 0.7704(2) 0.0409(9) Uani 1 1 d . . . H33F H 1.4857 0.6727 0.7832 0.061 Uiso 1 1 calc R . . H33E H 1.3894 0.7304 0.7376 0.061 Uiso 1 1 calc R . . H33D H 1.3739 0.6223 0.7479 0.061 Uiso 1 1 calc R . . C1S C 0.1055(4) 0.5758(3) 0.6237(2) 0.0461(11) Uani 1 1 d . . . H1SA H 0.1575 0.5287 0.6075 0.055 Uiso 1 1 calc R . . H1SB H 0.0942 0.5625 0.6734 0.055 Uiso 1 1 calc R . . C2S C 0.4602(9) 0.2743(5) 0.5013(4) 0.109(3) Uani 1 1 d . . . H2SB H 0.5255 0.2376 0.5223 0.131 Uiso 0.677(13) 1 calc PR A 1 H2SA H 0.4008 0.2722 0.5345 0.131 Uiso 0.677(13) 1 calc PR A 1 H2SC H 0.3788 0.2722 0.5050 0.131 Uiso 0.323(13) 1 d PR A 2 H2SD H 0.4990 0.2436 0.5418 0.131 Uiso 0.323(13) 1 d PR A 2 C3S C 0.3163(5) 0.4029(4) 0.6649(3) 0.064(2) Uani 0.75 1 d PD . . H3SA H 0.3777 0.3694 0.6933 0.077 Uiso 0.75 1 calc PR . . H3SB H 0.2551 0.4155 0.6956 0.077 Uiso 0.75 1 calc PR . . Cl1S Cl 0.16791(9) 0.68538(8) 0.61796(5) 0.0449(2) Uani 1 1 d . . . Cl2S Cl -0.02563(14) 0.56990(13) 0.57256(6) 0.0788(5) Uani 1 1 d . . . Cl3S Cl 0.4093(6) 0.22259(19) 0.42909(18) 0.094(2) Uani 0.677(13) 1 d P A 1 Cl3B Cl 0.4943(13) 0.2170(4) 0.4160(3) 0.091(3) Uani 0.323(13) 1 d P A 2 Cl4S Cl 0.50527(12) 0.38690(10) 0.49678(7) 0.0588(3) Uani 1 1 d . A . Cl5S Cl 0.3715(2) 0.5093(2) 0.63730(13) 0.0952(8) Uani 0.75 1 d PD . . Cl6S Cl 0.2660(2) 0.3378(3) 0.60116(16) 0.1144(11) Uani 0.75 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0156(10) 0.0244(13) 0.0298(12) -0.0077(10) 0.0032(9) -0.0011(9) O2 0.0186(11) 0.0344(14) 0.0218(11) -0.0076(10) 0.0039(9) -0.0002(10) O3 0.0141(10) 0.0298(13) 0.0257(11) -0.0025(10) 0.0090(8) 0.0005(9) O4 0.0192(10) 0.0339(14) 0.0263(12) -0.0027(11) -0.0003(9) 0.0060(10) O5 0.0220(11) 0.0336(14) 0.0199(11) -0.0002(10) 0.0018(9) 0.0022(10) O6 0.0127(10) 0.0271(13) 0.0347(12) 0.0028(10) 0.0070(9) -0.0009(9) N1 0.0124(11) 0.0162(14) 0.0241(13) 0.0031(11) 0.0078(10) -0.0005(10) C1 0.0153(14) 0.0141(16) 0.0203(15) 0.0006(12) 0.0025(12) 0.0008(12) C2 0.0126(13) 0.0161(16) 0.0179(14) 0.0027(12) 0.0064(11) 0.0015(11) C3 0.0152(13) 0.0169(15) 0.0155(13) -0.0001(12) 0.0049(11) 0.0013(12) C4 0.0182(14) 0.0154(16) 0.0130(13) 0.0008(11) 0.0028(11) 0.0010(12) C5 0.0140(13) 0.0104(14) 0.0177(14) 0.0007(11) 0.0023(11) 0.0014(11) C6 0.0146(14) 0.0118(15) 0.0189(14) 0.0006(12) 0.0044(11) 0.0010(11) C7 0.0210(15) 0.0167(16) 0.0189(15) 0.0023(12) 0.0014(12) 0.0025(12) C8 0.0183(15) 0.0222(17) 0.0189(15) -0.0008(12) 0.0074(12) 0.0023(12) C9 0.0124(13) 0.0143(15) 0.0229(15) 0.0014(12) 0.0048(11) 0.0029(11) C10 0.0173(14) 0.0133(15) 0.0184(14) 0.0006(11) 0.0014(11) -0.0007(11) C11 0.0104(13) 0.0284(19) 0.0240(15) -0.0043(14) 0.0054(12) 0.0053(12) C12 0.0150(15) 0.030(2) 0.0391(19) -0.0151(16) 0.0027(13) -0.0003(14) C13 0.0126(14) 0.0215(17) 0.043(2) -0.0103(15) 0.0087(13) -0.0033(13) C14 0.0148(15) 0.0195(19) 0.071(3) -0.0088(19) 0.0134(16) -0.0003(13) C15 0.0218(17) 0.0151(18) 0.081(3) 0.0006(19) 0.0236(18) -0.0035(14) C16 0.0260(18) 0.029(2) 0.058(2) 0.0089(18) 0.0272(17) -0.0027(16) C17 0.0185(15) 0.0226(18) 0.0321(17) 0.0072(14) 0.0139(13) 0.0032(13) C18 0.0222(16) 0.0231(18) 0.0225(16) 0.0079(13) 0.0101(13) 0.0045(13) C19 0.0163(14) 0.0204(17) 0.0208(15) 0.0070(13) 0.0046(12) 0.0035(12) C20 0.0115(13) 0.0198(17) 0.0162(14) 0.0039(12) 0.0053(11) 0.0002(12) C21 0.0124(13) 0.0177(16) 0.0197(14) 0.0027(12) 0.0051(11) 0.0019(12) C22 0.0110(13) 0.0226(18) 0.0233(15) 0.0049(13) 0.0038(11) 0.0016(12) C23 0.0166(14) 0.0190(17) 0.0226(15) 0.0001(13) 0.0068(11) 0.0021(12) C24 0.0203(16) 0.039(2) 0.0262(18) -0.0083(15) 0.0077(13) 0.0004(15) C25 0.051(3) 0.043(3) 0.057(3) -0.020(2) -0.020(2) -0.001(2) C26 0.028(2) 0.027(2) 0.109(4) -0.024(2) 0.004(2) -0.0053(17) C27 0.057(3) 0.050(3) 0.064(3) 0.019(2) 0.031(2) -0.016(2) C28 0.0357(19) 0.041(2) 0.0274(18) 0.0045(16) 0.0173(15) 0.0029(17) C29 0.0224(15) 0.0182(17) 0.0310(17) 0.0056(14) 0.0103(13) 0.0052(13) C30 0.0108(14) 0.033(2) 0.045(2) 0.0123(17) 0.0094(14) 0.0054(13) C31 0.0156(16) 0.062(3) 0.050(2) 0.029(2) 0.0042(15) 0.0105(17) C32 0.036(2) 0.092(5) 0.101(4) 0.069(4) 0.034(3) 0.041(3) C33 0.045(3) 0.131(6) 0.041(3) 0.035(3) -0.009(2) -0.005(3) O1' 0.0175(10) 0.0229(12) 0.0207(10) -0.0011(9) 0.0079(8) 0.0016(9) O2' 0.0198(10) 0.0275(13) 0.0185(10) 0.0044(9) 0.0070(8) 0.0048(9) O3' 0.0116(10) 0.0285(13) 0.0233(11) 0.0020(9) 0.0028(8) 0.0015(9) O4' 0.0247(11) 0.0196(13) 0.0288(12) -0.0018(9) 0.0131(9) -0.0044(9) O5' 0.0167(10) 0.0219(12) 0.0186(10) -0.0006(9) 0.0054(8) 0.0024(9) O6' 0.0124(10) 0.0178(12) 0.0317(12) 0.0000(9) 0.0061(8) 0.0020(8) N1' 0.0105(11) 0.0162(14) 0.0276(13) 0.0036(11) 0.0033(10) 0.0029(10) C1' 0.0121(13) 0.0128(15) 0.0210(15) -0.0004(12) 0.0054(11) -0.0025(11) C2' 0.0121(13) 0.0166(16) 0.0212(15) 0.0022(12) 0.0042(11) 0.0044(12) C3' 0.0149(14) 0.0217(17) 0.0242(15) 0.0066(13) 0.0048(12) 0.0013(13) C4' 0.0155(14) 0.0112(15) 0.0201(14) 0.0006(11) 0.0040(11) -0.0007(11) C5' 0.0138(13) 0.0128(15) 0.0168(14) -0.0016(11) 0.0041(11) -0.0008(11) C6' 0.0145(14) 0.0114(15) 0.0215(15) -0.0010(12) 0.0047(11) -0.0029(11) C7' 0.0189(15) 0.0132(15) 0.0165(14) -0.0002(11) 0.0052(11) -0.0035(11) C8' 0.0183(15) 0.0145(16) 0.0197(15) -0.0001(12) 0.0037(12) -0.0031(12) C9' 0.0137(14) 0.0142(16) 0.0217(15) -0.0018(11) 0.0040(11) -0.0010(11) C10' 0.0165(14) 0.0102(15) 0.0179(14) -0.0020(11) 0.0054(11) -0.0012(11) C11' 0.0108(13) 0.0212(17) 0.0173(14) -0.0001(12) 0.0035(11) 0.0000(12) C12' 0.0146(13) 0.0175(16) 0.0179(14) -0.0007(12) 0.0027(11) 0.0033(12) C13' 0.0132(13) 0.0190(16) 0.0162(13) -0.0001(11) 0.0023(11) 0.0038(12) C14' 0.0140(13) 0.0201(16) 0.0192(14) -0.0044(12) 0.0021(11) 0.0038(12) C15' 0.0153(14) 0.0202(17) 0.0243(15) -0.0043(13) 0.0045(12) 0.0014(12) C16' 0.0177(14) 0.0142(16) 0.0248(16) -0.0001(12) 0.0011(12) 0.0038(12) C17' 0.0158(14) 0.0179(16) 0.0194(14) 0.0014(12) 0.0018(11) -0.0008(12) C18' 0.0151(13) 0.0154(15) 0.0190(14) 0.0034(12) 0.0028(11) -0.0024(12) C19' 0.0131(13) 0.0118(15) 0.0182(14) 0.0007(11) 0.0010(11) 0.0008(11) C20' 0.0148(14) 0.0182(17) 0.0173(14) 0.0011(12) 0.0047(11) 0.0015(12) C21' 0.0139(13) 0.0142(16) 0.0193(14) -0.0005(11) 0.0021(11) 0.0003(11) C22' 0.0121(13) 0.0177(17) 0.0210(15) 0.0016(12) 0.0029(11) 0.0029(12) C23' 0.0144(14) 0.0176(16) 0.0177(14) 0.0008(11) 0.0013(11) -0.0005(12) C24' 0.0208(15) 0.030(2) 0.0236(16) 0.0023(14) 0.0009(12) -0.0048(13) C25' 0.0354(18) 0.0199(18) 0.0269(17) 0.0026(14) 0.0154(14) 0.0041(14) C26' 0.0272(16) 0.0251(19) 0.0248(16) -0.0046(13) 0.0103(13) 0.0037(14) C27' 0.0297(17) 0.0179(18) 0.0265(16) 0.0030(13) 0.0043(13) 0.0013(13) C28' 0.0165(14) 0.0233(18) 0.0183(14) 0.0013(12) 0.0021(11) 0.0014(12) C29' 0.0200(14) 0.0203(18) 0.0232(15) -0.0035(13) 0.0025(12) 0.0017(13) C30' 0.0143(14) 0.0170(17) 0.0272(16) 0.0003(12) -0.0014(12) 0.0005(12) C31' 0.0153(14) 0.0203(18) 0.0384(18) 0.0048(15) -0.0006(13) -0.0013(13) C32' 0.0255(18) 0.021(2) 0.061(3) 0.0071(18) -0.0036(17) -0.0041(15) C33' 0.040(2) 0.039(2) 0.045(2) 0.0111(19) 0.0122(17) -0.0062(18) C1S 0.066(3) 0.048(3) 0.0276(19) -0.0120(18) 0.0174(19) -0.022(2) C2S 0.160(8) 0.076(5) 0.078(4) 0.041(4) -0.055(5) -0.054(5) C3S 0.046(3) 0.080(5) 0.072(4) 0.047(4) 0.039(3) 0.037(4) Cl1S 0.0499(5) 0.0428(6) 0.0435(5) -0.0104(4) 0.0119(4) -0.0112(5) Cl2S 0.0832(9) 0.1170(14) 0.0365(6) -0.0029(7) 0.0066(6) -0.0607(9) Cl3S 0.166(5) 0.0552(15) 0.0563(16) -0.0156(10) -0.006(2) 0.0039(18) Cl3B 0.162(9) 0.047(3) 0.070(3) -0.005(2) 0.037(4) -0.007(4) Cl4S 0.0681(7) 0.0603(8) 0.0482(6) 0.0128(5) 0.0069(5) -0.0149(6) Cl5S 0.0853(14) 0.113(2) 0.0822(14) -0.0140(14) -0.0193(12) 0.0278(14) Cl6S 0.0822(15) 0.156(3) 0.1042(19) 0.054(2) 0.0046(14) -0.0372(17) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 C1 1.221(4) . ? O2 C4 1.212(4) . ? O3 C9 1.346(4) . ? O3 H3 0.8400 . ? O4 C11 1.225(4) . ? O5 C19 1.218(4) . ? O6 C23 1.237(4) . ? N1 C23 1.340(4) . ? N1 C2 1.453(4) . ? N1 H1 0.8800 . ? C1 C6 1.474(4) . ? C1 C2 1.536(4) . ? C2 C3 1.533(4) . ? C2 C21 1.572(4) . ? C3 C4 1.503(4) . ? C3 H3B 0.9900 . ? C3 H3A 0.9900 . ? C4 C5 1.491(4) . ? C5 C10 1.400(4) . ? C5 C6 1.414(4) . ? C6 C7 1.396(4) . ? C7 C8 1.373(5) . ? C7 H7 0.9500 . ? C8 C9 1.409(5) . ? C8 C24 1.498(4) . ? C9 C10 1.390(4) . ? C10 C11 1.513(4) . ? C11 C12 1.473(5) . ? C12 C13 1.345(6) . ? C12 C25 1.491(5) . ? C13 C14 1.454(5) . ? C13 H13 0.9500 . ? C14 C15 1.329(7) . ? C14 C26 1.494(6) . ? C15 C16 1.530(6) . ? C15 H15 0.9500 . ? C16 C17 1.516(4) . ? C16 C27 1.548(6) . ? C16 H16 1.0000 . ? C17 C18 1.326(5) . ? C17 H17 0.9500 . ? C18 C19 1.494(4) . ? C18 C28 1.508(5) . ? C19 C20 1.526(4) . ? C20 C21 1.543(4) . ? C20 C29 1.546(5) . ? C20 H20 1.0000 . ? C21 C22 1.546(4) . ? C21 H21 1.0000 . ? C22 C23 1.519(4) . ? C22 C30 1.527(4) . ? C22 H22 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25C 0.9800 . ? C25 H25B 0.9800 . ? C26 H26B 0.9800 . ? C26 H26A 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28C 0.9800 . ? C28 H28B 0.9800 . ? C29 H29C 0.9800 . ? C29 H29B 0.9800 . ? C29 H29A 0.9800 . ? C30 C31 1.518(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.537(7) . ? C31 C33 1.563(9) . ? C31 H31 1.0000 . ? C32 H32C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C33 H33B 0.9800 . ? C33 H33A 0.9800 . ? C33 H33C 0.9800 . ? O1' C1' 1.213(4) . ? O2' C4' 1.220(4) . ? O3' C9' 1.346(4) . ? O3' H3' 0.8400 . ? O4' C11' 1.212(4) . ? O5' C19' 1.215(4) . ? O6' C23' 1.243(4) . ? N1' C23' 1.341(4) . ? N1' C2' 1.469(4) . ? N1' H1' 0.8800 . ? C1' C6' 1.489(4) . ? C1' C2' 1.536(4) . ? C2' C3' 1.533(4) . ? C2' C21' 1.562(4) . ? C3' C4' 1.513(4) . ? C3' H3'A 0.9900 . ? C3' H3'B 0.9900 . ? C4' C5' 1.482(4) . ? C5' C6' 1.404(4) . ? C5' C10' 1.408(4) . ? C6' C7' 1.386(4) . ? C7' C8' 1.386(4) . ? C7' H7' 0.9500 . ? C8' C9' 1.415(4) . ? C8' C24' 1.498(4) . ? C9' C10' 1.394(4) . ? C10' C11' 1.515(4) . ? C11' C12' 1.485(4) . ? C12' C13' 1.346(5) . ? C12' C25' 1.512(4) . ? C13' C14' 1.464(4) . ? C13' H13A 0.9500 . ? C14' C15' 1.337(5) . ? C14' C26' 1.510(4) . ? C15' C16' 1.514(4) . ? C15' H15A 0.9500 . ? C16' C17' 1.513(4) . ? C16' C27' 1.537(5) . ? C16' H16A 1.0000 . ? C17' C18' 1.333(4) . ? C17' H17A 0.9500 . ? C18' C19' 1.491(4) . ? C18' C28' 1.508(4) . ? C19' C20' 1.537(4) . ? C20' C21' 1.537(4) . ? C20' C29' 1.548(4) . ? C20' H20A 1.0000 . ? C21' C22' 1.539(4) . ? C21' H21A 1.0000 . ? C22' C23' 1.518(5) . ? C22' C30' 1.530(4) . ? C22' H22A 1.0000 . ? C24' H24E 0.9800 . ? C24' H24F 0.9800 . ? C24' H24D 0.9800 . ? C25' H25D 0.9800 . ? C25' H25E 0.9800 . ? C25' H25F 0.9800 . ? C26' H26D 0.9800 . ? C26' H26F 0.9800 . ? C26' H26E 0.9800 . ? C27' H27F 0.9800 . ? C27' H27E 0.9800 . ? C27' H27D 0.9800 . ? C28' H28F 0.9800 . ? C28' H28E 0.9800 . ? C28' H28D 0.9800 . ? C29' H29E 0.9800 . ? C29' H29F 0.9800 . ? C29' H29D 0.9800 . ? C30' C31' 1.529(5) . ? C30' H30D 0.9900 . ? C30' H30C 0.9900 . ? C31' C33' 1.519(5) . ? C31' C32' 1.523(5) . ? C31' H31A 1.0000 . ? C32' H32F 0.9800 . ? C32' H32E 0.9800 . ? C32' H32D 0.9800 . ? C33' H33F 0.9800 . ? C33' H33E 0.9800 . ? C33' H33D 0.9800 . ? C1S Cl2S 1.749(5) . ? C1S Cl1S 1.766(5) . ? C1S H1SA 0.9900 . ? C1S H1SB 0.9900 . ? C2S Cl3S 1.634(8) . ? C2S Cl4S 1.729(7) . ? C2S Cl3B 1.909(13) . ? C2S H2SB 0.9900 . ? C2S H2SA 0.9900 . ? C2S H2SC 0.9700 . ? C2S H2SD 0.9700 . ? C3S Cl6S 1.610(7) . ? C3S Cl5S 1.781(6) . ? C3S H3SA 0.9900 . ? C3S H3SB 0.9900 . ? Cl3S H2SC 1.6895 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 O3 H3 109.5 . . ? C23 N1 C2 114.3(3) . . ? C23 N1 H1 122.9 . . ? C2 N1 H1 122.9 . . ? O1 C1 C6 121.0(3) . . ? O1 C1 C2 120.1(3) . . ? C6 C1 C2 118.9(3) . . ? N1 C2 C3 110.7(2) . . ? N1 C2 C1 110.6(3) . . ? C3 C2 C1 110.9(2) . . ? N1 C2 C21 99.3(2) . . ? C3 C2 C21 113.4(3) . . ? C1 C2 C21 111.4(2) . . ? C4 C3 C2 117.6(2) . . ? C4 C3 H3B 107.9 . . ? C2 C3 H3B 107.9 . . ? C4 C3 H3A 107.9 . . ? C2 C3 H3A 107.9 . . ? H3B C3 H3A 107.2 . . ? O2 C4 C5 121.4(3) . . ? O2 C4 C3 120.6(3) . . ? C5 C4 C3 118.0(3) . . ? C10 C5 C6 119.6(3) . . ? C10 C5 C4 120.5(3) . . ? C6 C5 C4 119.9(3) . . ? C7 C6 C5 119.0(3) . . ? C7 C6 C1 118.9(3) . . ? C5 C6 C1 122.1(3) . . ? C8 C7 C6 121.8(3) . . ? C8 C7 H7 119.1 . . ? C6 C7 H7 119.1 . . ? C7 C8 C9 118.9(3) . . ? C7 C8 C24 122.3(3) . . ? C9 C8 C24 118.7(3) . . ? O3 C9 C10 123.7(3) . . ? O3 C9 C8 115.5(3) . . ? C10 C9 C8 120.7(3) . . ? C9 C10 C5 119.8(3) . . ? C9 C10 C11 118.7(3) . . ? C5 C10 C11 121.4(3) . . ? O4 C11 C12 121.8(3) . . ? O4 C11 C10 118.2(3) . . ? C12 C11 C10 119.8(3) . . ? C13 C12 C11 116.8(3) . . ? C13 C12 C25 128.4(4) . . ? C11 C12 C25 114.7(4) . . ? C12 C13 C14 131.6(3) . . ? C12 C13 H13 114.2 . . ? C14 C13 H13 114.2 . . ? C15 C14 C13 119.8(4) . . ? C15 C14 C26 118.4(4) . . ? C13 C14 C26 121.8(4) . . ? C14 C15 C16 129.9(4) . . ? C14 C15 H15 115.0 . . ? C16 C15 H15 115.0 . . ? C17 C16 C15 112.9(3) . . ? C17 C16 C27 109.2(3) . . ? C15 C16 C27 110.2(4) . . ? C17 C16 H16 108.1 . . ? C15 C16 H16 108.1 . . ? C27 C16 H16 108.1 . . ? C18 C17 C16 126.1(3) . . ? C18 C17 H17 117.0 . . ? C16 C17 H17 117.0 . . ? C17 C18 C19 121.4(3) . . ? C17 C18 C28 123.9(3) . . ? C19 C18 C28 114.6(3) . . ? O5 C19 C18 119.1(3) . . ? O5 C19 C20 120.7(3) . . ? C18 C19 C20 120.2(3) . . ? C19 C20 C21 115.8(3) . . ? C19 C20 C29 109.7(3) . . ? C21 C20 C29 111.0(2) . . ? C19 C20 H20 106.6 . . ? C21 C20 H20 106.6 . . ? C29 C20 H20 106.6 . . ? C20 C21 C22 122.3(3) . . ? C20 C21 C2 117.1(2) . . ? C22 C21 C2 102.0(2) . . ? C20 C21 H21 104.5 . . ? C22 C21 H21 104.5 . . ? C2 C21 H21 104.5 . . ? C23 C22 C30 115.3(3) . . ? C23 C22 C21 100.6(2) . . ? C30 C22 C21 118.4(3) . . ? C23 C22 H22 107.3 . . ? C30 C22 H22 107.3 . . ? C21 C22 H22 107.3 . . ? O6 C23 N1 123.8(3) . . ? O6 C23 C22 127.6(3) . . ? N1 C23 C22 108.6(2) . . ? C8 C24 H24A 109.5 . . ? C8 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C8 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C12 C25 H25A 109.5 . . ? C12 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? C12 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? H25C C25 H25B 109.5 . . ? C14 C26 H26B 109.5 . . ? C14 C26 H26A 109.5 . . ? H26B C26 H26A 109.5 . . ? C14 C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? C16 C27 H27A 109.5 . . ? C16 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C16 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C18 C28 H28A 109.5 . . ? C18 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? C18 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? H28C C28 H28B 109.5 . . ? C20 C29 H29C 109.5 . . ? C20 C29 H29B 109.5 . . ? H29C C29 H29B 109.5 . . ? C20 C29 H29A 109.5 . . ? H29C C29 H29A 109.5 . . ? H29B C29 H29A 109.5 . . ? C31 C30 C22 112.9(3) . . ? C31 C30 H30A 109.0 . . ? C22 C30 H30A 109.0 . . ? C31 C30 H30B 109.0 . . ? C22 C30 H30B 109.0 . . ? H30A C30 H30B 107.8 . . ? C30 C31 C32 112.3(4) . . ? C30 C31 C33 110.4(4) . . ? C32 C31 C33 112.3(4) . . ? C30 C31 H31 107.2 . . ? C32 C31 H31 107.2 . . ? C33 C31 H31 107.2 . . ? C31 C32 H32C 109.5 . . ? C31 C32 H32A 109.5 . . ? H32C C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32C C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C33 H33B 109.5 . . ? C31 C33 H33A 109.5 . . ? H33B C33 H33A 109.5 . . ? C31 C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? C9' O3' H3' 109.5 . . ? C23' N1' C2' 113.0(3) . . ? C23' N1' H1' 123.5 . . ? C2' N1' H1' 123.5 . . ? O1' C1' C6' 121.0(3) . . ? O1' C1' C2' 120.6(3) . . ? C6' C1' C2' 118.3(2) . . ? N1' C2' C3' 111.1(2) . . ? N1' C2' C1' 108.6(2) . . ? C3' C2' C1' 111.8(2) . . ? N1' C2' C21' 99.9(2) . . ? C3' C2' C21' 112.8(3) . . ? C1' C2' C21' 112.1(3) . . ? C4' C3' C2' 116.7(3) . . ? C4' C3' H3'A 108.1 . . ? C2' C3' H3'A 108.1 . . ? C4' C3' H3'B 108.1 . . ? C2' C3' H3'B 108.1 . . ? H3'A C3' H3'B 107.3 . . ? O2' C4' C5' 121.4(3) . . ? O2' C4' C3' 119.6(3) . . ? C5' C4' C3' 118.9(3) . . ? C6' C5' C10' 119.6(3) . . ? C6' C5' C4' 120.2(3) . . ? C10' C5' C4' 120.1(3) . . ? C7' C6' C5' 119.8(3) . . ? C7' C6' C1' 118.1(3) . . ? C5' C6' C1' 122.1(3) . . ? C8' C7' C6' 122.0(3) . . ? C8' C7' H7' 119.0 . . ? C6' C7' H7' 119.0 . . ? C7' C8' C9' 117.9(3) . . ? C7' C8' C24' 122.1(3) . . ? C9' C8' C24' 120.0(3) . . ? O3' C9' C10' 124.0(3) . . ? O3' C9' C8' 114.7(3) . . ? C10' C9' C8' 121.3(3) . . ? C9' C10' C5' 119.2(3) . . ? C9' C10' C11' 118.3(3) . . ? C5' C10' C11' 122.3(3) . . ? O4' C11' C12' 121.3(3) . . ? O4' C11' C10' 118.6(3) . . ? C12' C11' C10' 119.9(3) . . ? C13' C12' C11' 118.5(3) . . ? C13' C12' C25' 128.0(3) . . ? C11' C12' C25' 113.5(3) . . ? C12' C13' C14' 131.6(3) . . ? C12' C13' H13A 114.2 . . ? C14' C13' H13A 114.2 . . ? C15' C14' C13' 121.1(3) . . ? C15' C14' C26' 117.8(3) . . ? C13' C14' C26' 121.2(3) . . ? C14' C15' C16' 127.7(3) . . ? C14' C15' H15A 116.1 . . ? C16' C15' H15A 116.1 . . ? C17' C16' C15' 112.1(3) . . ? C17' C16' C27' 110.0(3) . . ? C15' C16' C27' 109.6(3) . . ? C17' C16' H16A 108.3 . . ? C15' C16' H16A 108.3 . . ? C27' C16' H16A 108.3 . . ? C18' C17' C16' 125.0(3) . . ? C18' C17' H17A 117.5 . . ? C16' C17' H17A 117.5 . . ? C17' C18' C19' 120.6(3) . . ? C17' C18' C28' 123.2(3) . . ? C19' C18' C28' 116.1(3) . . ? O5' C19' C18' 119.6(3) . . ? O5' C19' C20' 120.2(3) . . ? C18' C19' C20' 120.2(2) . . ? C19' C20' C21' 115.4(2) . . ? C19' C20' C29' 110.0(3) . . ? C21' C20' C29' 110.3(2) . . ? C19' C20' H20A 106.9 . . ? C21' C20' H20A 106.9 . . ? C29' C20' H20A 106.9 . . ? C20' C21' C22' 122.7(3) . . ? C20' C21' C2' 116.8(2) . . ? C22' C21' C2' 102.8(2) . . ? C20' C21' H21A 104.2 . . ? C22' C21' H21A 104.2 . . ? C2' C21' H21A 104.2 . . ? C23' C22' C30' 115.6(2) . . ? C23' C22' C21' 101.2(2) . . ? C30' C22' C21' 118.1(3) . . ? C23' C22' H22A 107.1 . . ? C30' C22' H22A 107.1 . . ? C21' C22' H22A 107.1 . . ? O6' C23' N1' 124.1(3) . . ? O6' C23' C22' 126.5(3) . . ? N1' C23' C22' 109.4(3) . . ? C8' C24' H24E 109.5 . . ? C8' C24' H24F 109.5 . . ? H24E C24' H24F 109.5 . . ? C8' C24' H24D 109.5 . . ? H24E C24' H24D 109.5 . . ? H24F C24' H24D 109.5 . . ? C12' C25' H25D 109.5 . . ? C12' C25' H25E 109.5 . . ? H25D C25' H25E 109.5 . . ? C12' C25' H25F 109.5 . . ? H25D C25' H25F 109.5 . . ? H25E C25' H25F 109.5 . . ? C14' C26' H26D 109.5 . . ? C14' C26' H26F 109.5 . . ? H26D C26' H26F 109.5 . . ? C14' C26' H26E 109.5 . . ? H26D C26' H26E 109.5 . . ? H26F C26' H26E 109.5 . . ? C16' C27' H27F 109.5 . . ? C16' C27' H27E 109.5 . . ? H27F C27' H27E 109.5 . . ? C16' C27' H27D 109.5 . . ? H27F C27' H27D 109.5 . . ? H27E C27' H27D 109.5 . . ? C18' C28' H28F 109.5 . . ? C18' C28' H28E 109.5 . . ? H28F C28' H28E 109.5 . . ? C18' C28' H28D 109.5 . . ? H28F C28' H28D 109.5 . . ? H28E C28' H28D 109.5 . . ? C20' C29' H29E 109.5 . . ? C20' C29' H29F 109.5 . . ? H29E C29' H29F 109.5 . . ? C20' C29' H29D 109.5 . . ? H29E C29' H29D 109.5 . . ? H29F C29' H29D 109.5 . . ? C31' C30' C22' 113.7(3) . . ? C31' C30' H30D 108.8 . . ? C22' C30' H30D 108.8 . . ? C31' C30' H30C 108.8 . . ? C22' C30' H30C 108.8 . . ? H30D C30' H30C 107.7 . . ? C33' C31' C32' 110.8(3) . . ? C33' C31' C30' 111.3(3) . . ? C32' C31' C30' 111.8(3) . . ? C33' C31' H31A 107.6 . . ? C32' C31' H31A 107.6 . . ? C30' C31' H31A 107.6 . . ? C31' C32' H32F 109.5 . . ? C31' C32' H32E 109.5 . . ? H32F C32' H32E 109.5 . . ? C31' C32' H32D 109.5 . . ? H32F C32' H32D 109.5 . . ? H32E C32' H32D 109.5 . . ? C31' C33' H33F 109.5 . . ? C31' C33' H33E 109.5 . . ? H33F C33' H33E 109.5 . . ? C31' C33' H33D 109.5 . . ? H33F C33' H33D 109.5 . . ? H33E C33' H33D 109.5 . . ? Cl2S C1S Cl1S 111.1(3) . . ? Cl2S C1S H1SA 109.4 . . ? Cl1S C1S H1SA 109.4 . . ? Cl2S C1S H1SB 109.4 . . ? Cl1S C1S H1SB 109.4 . . ? H1SA C1S H1SB 108.0 . . ? Cl3S C2S Cl4S 119.0(4) . . ? Cl3S C2S Cl3B 33.7(3) . . ? Cl4S C2S Cl3B 106.3(5) . . ? Cl3S C2S H2SB 107.6 . . ? Cl4S C2S H2SB 107.6 . . ? Cl3B C2S H2SB 83.8 . . ? Cl3S C2S H2SA 107.6 . . ? Cl4S C2S H2SA 107.6 . . ? Cl3B C2S H2SA 138.9 . . ? H2SB C2S H2SA 107.0 . . ? Cl3S C2S H2SC 76.2 . . ? Cl4S C2S H2SC 110.2 . . ? Cl3B C2S H2SC 109.9 . . ? H2SB C2S H2SC 133.6 . . ? H2SA C2S H2SC 35.5 . . ? Cl3S C2S H2SD 124.5 . . ? Cl4S C2S H2SD 110.8 . . ? Cl3B C2S H2SD 110.9 . . ? H2SB C2S H2SD 30.4 . . ? H2SA C2S H2SD 77.4 . . ? H2SC C2S H2SD 108.7 . . ? Cl6S C3S Cl5S 114.0(4) . . ? Cl6S C3S H3SA 108.7 . . ? Cl5S C3S H3SA 108.7 . . ? Cl6S C3S H3SB 108.7 . . ? Cl5S C3S H3SB 108.7 . . ? H3SA C3S H3SB 107.6 . . ? C2S Cl3S H2SC 33.9 . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 65.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.608 _refine_diff_density_min -0.944 _refine_diff_density_rms 0.070