data_dk _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H54 N10 O17 S4' _chemical_formula_weight 955.07 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.5465(8) _cell_length_b 16.3492(7) _cell_length_c 28.7869(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8728.8(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5924 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 28.13 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4032 _exptl_absorpt_coefficient_mu 0.298 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Agilent Technologies Gemini-S four-circle diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22639 _diffrn_reflns_av_R_equivalents 0.0572 _diffrn_reflns_av_sigmaI/netI 0.0616 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 24.99 _reflns_number_total 7455 _reflns_number_gt 5156 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0549P)^2^+4.3775P] 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 7455 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0884 _refine_ls_R_factor_gt 0.0551 _refine_ls_wR_factor_ref 0.1428 _refine_ls_wR_factor_gt 0.1234 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S3 S 0.89172(4) 0.60014(5) 0.18668(3) 0.0234(2) Uani 1 1 d . . . S4 S 0.60180(4) 0.63860(5) 0.18158(3) 0.0230(2) Uani 1 1 d . . . S2 S 0.87943(5) 0.60233(5) 0.45125(3) 0.0251(2) Uani 1 1 d . . . S1 S 0.59105(5) 0.62144(5) 0.44584(3) 0.0248(2) Uani 1 1 d . . . O9 O 0.93105(12) 0.67203(14) 0.20266(8) 0.0295(6) Uani 1 1 d . . . O11 O 0.57738(12) 0.71817(13) 0.19820(8) 0.0309(6) Uani 1 1 d . . . O7 O 0.87279(12) 0.60404(15) 0.13803(8) 0.0316(6) Uani 1 1 d . . . O3 O 0.56225(12) 0.70168(14) 0.43479(8) 0.0329(6) Uani 1 1 d . . . O8 O 0.92814(12) 0.52454(14) 0.19908(8) 0.0304(6) Uani 1 1 d . . . O12 O 0.62604(12) 0.64357(14) 0.13376(8) 0.0313(6) Uani 1 1 d . . . O10 O 0.54967(12) 0.57463(14) 0.18969(8) 0.0303(6) Uani 1 1 d . . . O4 O 0.85331(12) 0.58118(15) 0.49727(8) 0.0343(6) Uani 1 1 d . . . O2 O 0.61196(13) 0.61517(16) 0.49374(8) 0.0355(6) Uani 1 1 d . . . O1 O 0.54288(12) 0.55647(14) 0.43109(8) 0.0357(6) Uani 1 1 d . . . O6 O 0.92918(13) 0.54300(16) 0.43394(8) 0.0426(7) Uani 1 1 d . . . O5 O 0.90692(13) 0.68516(14) 0.44988(9) 0.0389(7) Uani 1 1 d . . . O15 O 0.45618(13) 0.79503(16) 0.23087(9) 0.0484(7) Uani 1 1 d . . . H15D H 0.4960 0.7756 0.2213 0.073 Uiso 1 1 d R . . H15F H 0.4468 0.7756 0.2576 0.073 Uiso 1 1 d R . . O14 O 0.82722(17) 0.68156(17) -0.42997(9) 0.0565(8) Uani 1 1 d . . . H14D H 0.8418 0.6535 -0.4530 0.085 Uiso 1 1 d R . . O16 O 0.53992(14) 0.82164(17) 0.50038(10) 0.0606(9) Uani 1 1 d . . . H16D H 0.5427 0.7800 0.4828 0.091 Uiso 1 1 d R . . H16F H 0.4979 0.8167 0.5118 0.091 Uiso 1 1 d R . . O13 O 0.81808(18) 0.55934(17) -0.39666(10) 0.0606(9) Uani 1 1 d . . . O17 O 0.90191(16) 0.8552(3) 0.53292(11) 0.0947(14) Uani 1 1 d . . . H17D H 0.8899 0.9051 0.5299 0.114 Uiso 1 1 d R . . H17F H 0.8901 0.8208 0.5537 0.114 Uiso 1 1 d R . . N5 N 0.88936(15) 0.37365(18) 0.15565(10) 0.0329(8) Uani 1 1 d . . . H5B H 0.8886 0.4182 0.1715 0.039 Uiso 1 1 calc R . . H5C H 0.8905 0.3272 0.1696 0.039 Uiso 1 1 calc R . . N10 N 0.64451(16) 0.57659(18) 0.04371(10) 0.0353(8) Uani 1 1 d . . . H10A H 0.6418 0.5481 0.0700 0.053 Uiso 1 1 calc R . . H10B H 0.6390 0.5431 0.0196 0.053 Uiso 1 1 calc R . . H10C H 0.6099 0.6143 0.0433 0.053 Uiso 1 1 calc R . . N4 N 0.88693(16) 0.44734(17) 0.08795(10) 0.0352(8) Uani 1 1 d . . . H4B H 0.8856 0.4488 0.0581 0.042 Uiso 1 1 calc R . . H4C H 0.8871 0.4921 0.1036 0.042 Uiso 1 1 calc R . . N6 N 0.88846(16) 0.30733(18) 0.08573(10) 0.0375(8) Uani 1 1 d . . . H6B H 0.8871 0.3085 0.0559 0.045 Uiso 1 1 calc R . . H6C H 0.8896 0.2612 0.1001 0.045 Uiso 1 1 calc R . . N1 N 0.94085(17) 0.92629(19) 0.35803(12) 0.0456(9) Uani 1 1 d . . . H1B H 0.9459 0.9753 0.3683 0.055 Uiso 1 1 calc R . . H1C H 0.9433 0.9169 0.3287 0.055 Uiso 1 1 calc R . . N2 N 0.92547(17) 0.8799(2) 0.43217(12) 0.0446(9) Uani 1 1 d . . . H2B H 0.9181 0.8404 0.4513 0.054 Uiso 1 1 calc R . . H2C H 0.9304 0.9291 0.4424 0.054 Uiso 1 1 calc R . . N3 N 0.92188(18) 0.79072(18) 0.37105(12) 0.0465(9) Uani 1 1 d . . . H3B H 0.9145 0.7506 0.3898 0.056 Uiso 1 1 calc R . . H3C H 0.9245 0.7820 0.3416 0.056 Uiso 1 1 calc R . . N9 N 1.0011(2) 0.28608(19) 0.35783(14) 0.0631(12) Uani 1 1 d . . . H9B H 1.0095 0.2587 0.3329 0.076 Uiso 1 1 calc R . . H9C H 0.9925 0.2609 0.3835 0.076 Uiso 1 1 calc R . . N8 N 1.0144(2) 0.4030(2) 0.31738(15) 0.0647(12) Uani 1 1 d . . . H8C H 1.0228 0.3752 0.2926 0.078 Uiso 1 1 calc R . . H8D H 1.0146 0.4556 0.3164 0.078 Uiso 1 1 calc R . . N7 N 0.9870(2) 0.4070(2) 0.39536(16) 0.0788(13) Uani 1 1 d . . . H7C H 0.9779 0.3814 0.4208 0.095 Uiso 1 1 calc R . . H7D H 0.9871 0.4596 0.3949 0.095 Uiso 1 1 calc R . . C9 C 0.80876(16) 0.60201(18) 0.26695(11) 0.0172(7) Uani 1 1 d . . . C10 C 0.74107(16) 0.60728(18) 0.29066(11) 0.0174(7) Uani 1 1 d . . . C12 C 0.67590(17) 0.61477(18) 0.26485(11) 0.0184(7) Uani 1 1 d . . . C4 C 0.80518(16) 0.60270(18) 0.36635(11) 0.0183(7) Uani 1 1 d . . . C5 C 0.73930(16) 0.60723(17) 0.34027(11) 0.0176(7) Uani 1 1 d . . . C6 C 0.67172(17) 0.61279(18) 0.36386(11) 0.0197(7) Uani 1 1 d . . . C16 C 0.60736(16) 0.61912(19) 0.33631(11) 0.0204(8) Uani 1 1 d . . . H16A H 0.5630 0.6224 0.3513 0.025 Uiso 1 1 calc R . . C8 C 0.87326(17) 0.59690(18) 0.29453(11) 0.0204(7) Uani 1 1 d . . . H8B H 0.9175 0.5926 0.2796 0.024 Uiso 1 1 calc R . . C2 C 0.73555(18) 0.60653(18) 0.43759(12) 0.0235(8) Uani 1 1 d . . . H2D H 0.7342 0.6057 0.4699 0.028 Uiso 1 1 calc R . . C11 C 0.67987(16) 0.61711(18) 0.21597(11) 0.0191(7) Uani 1 1 d . . . C14 C 0.74538(17) 0.60972(18) 0.19324(11) 0.0212(8) Uani 1 1 d . . . H14A H 0.7468 0.6097 0.1609 0.025 Uiso 1 1 calc R . . C13 C 0.80882(16) 0.60237(18) 0.21829(11) 0.0183(7) Uani 1 1 d . . . C15 C 0.60908(17) 0.62039(19) 0.28986(12) 0.0240(8) Uani 1 1 d . . . H15A H 0.5661 0.6250 0.2734 0.029 Uiso 1 1 calc R . . C7 C 0.87167(17) 0.59819(19) 0.34072(11) 0.0216(8) Uani 1 1 d . . . H7B H 0.9150 0.5961 0.3570 0.026 Uiso 1 1 calc R . . C3 C 0.80137(17) 0.60269(19) 0.41503(11) 0.0199(7) Uani 1 1 d . . . C19 C 0.88872(17) 0.3767(2) 0.10962(13) 0.0278(8) Uani 1 1 d . . . C1 C 0.67158(17) 0.61162(18) 0.41289(11) 0.0201(7) Uani 1 1 d . . . C17 C 0.92923(18) 0.8653(2) 0.38735(14) 0.0320(9) Uani 1 1 d . . . C25 C 0.7376(2) 0.6681(2) -0.17916(12) 0.0325(9) Uani 1 1 d . . . H25A H 0.7760 0.7077 -0.1747 0.039 Uiso 1 1 calc R . . H25B H 0.6931 0.6984 -0.1836 0.039 Uiso 1 1 calc R . . C27 C 0.7641(2) 0.6725(2) -0.26562(12) 0.0307(9) Uani 1 1 d . . . H27A H 0.7195 0.7012 -0.2723 0.037 Uiso 1 1 calc R . . H27B H 0.8007 0.7131 -0.2590 0.037 Uiso 1 1 calc R . . C28 C 0.7863(2) 0.6245(2) -0.30838(11) 0.0312(9) Uani 1 1 d . . . H28A H 0.7496 0.5840 -0.3152 0.037 Uiso 1 1 calc R . . H28B H 0.8309 0.5958 -0.3019 0.037 Uiso 1 1 calc R . . C23 C 0.7255(2) 0.6671(2) -0.09123(12) 0.0320(9) Uani 1 1 d . . . H23A H 0.7673 0.7026 -0.0892 0.038 Uiso 1 1 calc R . . H23B H 0.6831 0.7018 -0.0930 0.038 Uiso 1 1 calc R . . C22 C 0.7211(2) 0.6166(2) -0.04762(12) 0.0332(9) Uani 1 1 d . . . H22A H 0.7608 0.5779 -0.0474 0.040 Uiso 1 1 calc R . . H22B H 0.6766 0.5856 -0.0480 0.040 Uiso 1 1 calc R . . C24 C 0.7307(2) 0.6175(2) -0.13581(12) 0.0328(9) Uani 1 1 d . . . H24A H 0.7721 0.5814 -0.1337 0.039 Uiso 1 1 calc R . . H24B H 0.6881 0.5834 -0.1385 0.039 Uiso 1 1 calc R . . C21 C 0.72390(19) 0.6669(2) -0.00350(12) 0.0329(9) Uani 1 1 d . . . H21A H 0.7693 0.6964 -0.0027 0.040 Uiso 1 1 calc R . . H21B H 0.6854 0.7071 -0.0044 0.040 Uiso 1 1 calc R . . C26 C 0.7533(2) 0.6198(2) -0.22275(12) 0.0334(9) Uani 1 1 d . . . H26A H 0.7136 0.5824 -0.2284 0.040 Uiso 1 1 calc R . . H26B H 0.7963 0.5873 -0.2178 0.040 Uiso 1 1 calc R . . C30 C 0.8148(2) 0.6325(2) -0.39362(13) 0.0360(9) Uani 1 1 d . . . C29 C 0.7967(2) 0.6788(2) -0.35069(12) 0.0342(9) Uani 1 1 d . . . H29A H 0.7529 0.7097 -0.3560 0.041 Uiso 1 1 calc R . . H29B H 0.8351 0.7176 -0.3443 0.041 Uiso 1 1 calc R . . C20 C 0.7168(2) 0.6176(2) 0.04071(13) 0.0390(10) Uani 1 1 d . . . H20A H 0.7545 0.5764 0.0417 0.047 Uiso 1 1 calc R . . H20B H 0.7231 0.6534 0.0673 0.047 Uiso 1 1 calc R . . C18 C 1.0012(2) 0.3652(3) 0.35677(18) 0.0469(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S3 0.0217(4) 0.0293(5) 0.0191(5) -0.0013(4) 0.0060(4) 0.0000(4) S4 0.0217(4) 0.0296(5) 0.0178(5) -0.0001(4) -0.0031(4) 0.0025(4) S2 0.0259(5) 0.0324(5) 0.0169(5) -0.0012(4) -0.0040(4) 0.0038(4) S1 0.0242(4) 0.0326(5) 0.0176(5) -0.0016(4) 0.0052(4) -0.0001(4) O9 0.0269(13) 0.0329(13) 0.0286(14) 0.0008(12) 0.0067(11) -0.0082(11) O11 0.0354(13) 0.0308(13) 0.0267(14) 0.0022(12) -0.0008(12) 0.0086(12) O7 0.0281(13) 0.0480(15) 0.0188(13) -0.0005(13) 0.0098(11) 0.0034(12) O3 0.0319(14) 0.0370(13) 0.0296(14) -0.0040(13) 0.0070(11) 0.0072(12) O8 0.0281(13) 0.0326(13) 0.0305(14) -0.0066(12) 0.0047(11) 0.0059(11) O12 0.0320(13) 0.0477(15) 0.0142(12) 0.0027(12) -0.0041(11) 0.0073(12) O10 0.0260(13) 0.0335(13) 0.0315(14) -0.0008(12) -0.0035(11) -0.0044(11) O4 0.0361(14) 0.0504(15) 0.0164(13) 0.0034(12) -0.0060(11) 0.0013(13) O2 0.0343(14) 0.0549(16) 0.0174(13) 0.0036(13) 0.0072(11) 0.0012(13) O1 0.0326(14) 0.0400(14) 0.0345(15) -0.0101(13) 0.0105(12) -0.0124(12) O6 0.0416(15) 0.0588(17) 0.0274(15) -0.0098(14) -0.0083(12) 0.0267(14) O5 0.0408(15) 0.0348(14) 0.0412(16) 0.0045(13) -0.0134(13) -0.0087(12) O15 0.0401(15) 0.0574(17) 0.0477(17) 0.0131(16) 0.0143(14) 0.0128(14) O14 0.090(2) 0.0549(18) 0.0245(15) 0.0005(15) 0.0136(15) 0.0013(17) O16 0.0354(16) 0.0637(18) 0.083(2) -0.0428(19) 0.0229(16) -0.0106(15) O13 0.104(3) 0.0409(17) 0.0364(17) -0.0081(15) 0.0194(17) 0.0037(17) O17 0.0442(19) 0.197(4) 0.0425(19) 0.009(3) -0.0020(16) 0.003(2) N5 0.0446(19) 0.0311(16) 0.0229(18) 0.0005(15) 0.0020(14) -0.0055(15) N10 0.049(2) 0.0407(18) 0.0161(16) -0.0003(15) 0.0032(15) 0.0062(16) N4 0.052(2) 0.0318(17) 0.0217(17) 0.0017(15) -0.0012(15) 0.0047(16) N6 0.057(2) 0.0318(17) 0.0237(17) 0.0005(16) -0.0026(16) -0.0081(16) N1 0.049(2) 0.0401(19) 0.048(2) 0.0073(19) 0.0039(18) 0.0019(17) N2 0.052(2) 0.0438(19) 0.038(2) -0.0014(18) 0.0039(18) 0.0004(17) N3 0.061(2) 0.0342(18) 0.045(2) -0.0026(18) -0.0008(18) -0.0067(17) N9 0.094(3) 0.035(2) 0.060(3) -0.012(2) 0.039(2) -0.007(2) N8 0.066(3) 0.035(2) 0.093(3) 0.001(2) -0.001(2) -0.0084(19) N7 0.077(3) 0.058(2) 0.102(3) -0.042(3) 0.017(3) 0.007(2) C9 0.0159(16) 0.0142(15) 0.0217(18) -0.0020(15) 0.0019(14) -0.0002(14) C10 0.0178(16) 0.0163(15) 0.0180(18) 0.0014(15) -0.0006(14) -0.0013(14) C12 0.0221(17) 0.0145(15) 0.0185(18) -0.0007(15) 0.0020(14) -0.0006(14) C4 0.0178(16) 0.0159(16) 0.0212(18) 0.0003(15) -0.0006(14) 0.0003(14) C5 0.0214(17) 0.0142(15) 0.0172(18) -0.0008(15) 0.0005(14) 0.0020(14) C6 0.0199(17) 0.0182(16) 0.0211(18) 0.0017(16) 0.0006(15) 0.0014(14) C16 0.0172(17) 0.0216(17) 0.0225(19) -0.0007(16) 0.0053(14) -0.0005(15) C8 0.0169(16) 0.0210(17) 0.0233(19) 0.0011(16) 0.0029(15) 0.0008(14) C2 0.032(2) 0.0227(17) 0.0158(18) 0.0026(16) -0.0029(16) 0.0005(16) C11 0.0197(16) 0.0186(16) 0.0190(18) -0.0005(15) -0.0034(14) -0.0001(14) C14 0.0291(19) 0.0211(16) 0.0133(17) -0.0028(15) 0.0007(15) -0.0022(16) C13 0.0196(17) 0.0163(15) 0.0189(18) -0.0037(16) 0.0028(15) -0.0011(14) C15 0.0187(17) 0.0274(18) 0.026(2) -0.0011(17) 0.0000(15) 0.0018(15) C7 0.0211(17) 0.0247(17) 0.0190(19) 0.0006(16) -0.0031(15) 0.0009(15) C3 0.0212(17) 0.0201(16) 0.0185(18) -0.0026(16) 0.0002(15) 0.0014(14) C19 0.0212(18) 0.035(2) 0.027(2) -0.0021(19) -0.0003(16) -0.0034(17) C1 0.0218(17) 0.0201(16) 0.0185(18) -0.0008(16) 0.0020(15) 0.0003(14) C17 0.0213(18) 0.036(2) 0.039(2) 0.005(2) 0.0007(17) 0.0037(17) C25 0.044(2) 0.0269(18) 0.027(2) 0.0007(18) 0.0015(18) -0.0001(18) C27 0.037(2) 0.0272(18) 0.028(2) -0.0024(18) 0.0015(17) -0.0004(17) C28 0.037(2) 0.031(2) 0.025(2) -0.0031(18) 0.0014(17) 0.0020(17) C23 0.036(2) 0.0333(19) 0.027(2) -0.0016(19) 0.0065(17) -0.0004(18) C22 0.037(2) 0.035(2) 0.028(2) 0.0017(19) 0.0056(18) -0.0006(18) C24 0.043(2) 0.0287(19) 0.027(2) -0.0035(18) 0.0067(18) -0.0023(18) C21 0.031(2) 0.041(2) 0.027(2) -0.0013(19) 0.0024(17) -0.0003(18) C26 0.046(2) 0.0292(19) 0.025(2) -0.0013(18) 0.0030(18) 0.0017(18) C30 0.041(2) 0.039(2) 0.028(2) -0.002(2) 0.0033(18) -0.003(2) C29 0.041(2) 0.036(2) 0.026(2) -0.0043(19) 0.0033(18) -0.0047(18) C20 0.038(2) 0.054(2) 0.024(2) -0.002(2) -0.0006(18) 0.003(2) C18 0.039(2) 0.037(2) 0.066(3) -0.008(3) 0.010(2) -0.002(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 S3 O7 1.445(2) . ? S3 O8 1.453(2) . ? S3 O9 1.458(2) . ? S3 C13 1.787(3) . ? S4 O10 1.443(2) . ? S4 O12 1.450(2) . ? S4 O11 1.458(2) . ? S4 C11 1.789(3) . ? S2 O6 1.428(2) . ? S2 O5 1.448(2) . ? S2 O4 1.452(2) . ? S2 C3 1.784(3) . ? S1 O2 1.436(2) . ? S1 O3 1.452(2) . ? S1 O1 1.451(2) . ? S1 C1 1.777(3) . ? O15 H15D 0.8501 . ? O15 H15F 0.8500 . ? O14 C30 1.339(4) . ? O14 H14D 0.8500 . ? O16 H16D 0.8499 . ? O16 H16F 0.8498 . ? O13 C30 1.200(4) . ? O17 H17D 0.8500 . ? O17 H17F 0.8501 . ? N5 C19 1.326(4) . ? N5 H5B 0.8600 . ? N5 H5C 0.8600 . ? N10 C20 1.502(5) . ? N10 H10A 0.8900 . ? N10 H10B 0.8900 . ? N10 H10C 0.8900 . ? N4 C19 1.314(4) . ? N4 H4B 0.8600 . ? N4 H4C 0.8600 . ? N6 C19 1.326(4) . ? N6 H6B 0.8600 . ? N6 H6C 0.8600 . ? N1 C17 1.324(4) . ? N1 H1B 0.8600 . ? N1 H1C 0.8600 . ? N2 C17 1.314(5) . ? N2 H2B 0.8600 . ? N2 H2C 0.8600 . ? N3 C17 1.314(4) . ? N3 H3B 0.8600 . ? N3 H3C 0.8600 . ? N9 C18 1.294(5) . ? N9 H9B 0.8600 . ? N9 H9C 0.8600 . ? N8 C18 1.315(5) . ? N8 H8C 0.8600 . ? N8 H8D 0.8600 . ? N7 C18 1.330(5) . ? N7 H7C 0.8600 . ? N7 H7D 0.8600 . ? C9 C13 1.401(4) . ? C9 C10 1.432(4) . ? C9 C8 1.438(4) . ? C10 C12 1.424(4) . ? C10 C5 1.429(4) . ? C12 C11 1.410(4) . ? C12 C15 1.436(4) . ? C4 C3 1.403(4) . ? C4 C7 1.439(4) . ? C4 C5 1.436(4) . ? C5 C6 1.428(4) . ? C6 C1 1.412(4) . ? C6 C16 1.437(4) . ? C16 C15 1.338(5) . ? C16 H16A 0.9300 . ? C8 C7 1.330(4) . ? C8 H8B 0.9300 . ? C2 C3 1.384(4) . ? C2 C1 1.386(4) . ? C2 H2D 0.9300 . ? C11 C14 1.385(4) . ? C14 C13 1.385(4) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C7 H7B 0.9300 . ? C25 C24 1.503(5) . ? C25 C26 1.511(5) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C27 C28 1.516(5) . ? C27 C26 1.518(5) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.519(5) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C23 C22 1.505(5) . ? C23 C24 1.522(5) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C22 C21 1.514(5) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C21 C20 1.513(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C30 C29 1.488(5) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? 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 O7 S3 O8 112.86(14) . . ? O7 S3 O9 113.06(14) . . ? O8 S3 O9 112.06(14) . . ? O7 S3 C13 106.48(14) . . ? O8 S3 C13 107.00(14) . . ? O9 S3 C13 104.68(14) . . ? O10 S4 O12 113.70(14) . . ? O10 S4 O11 112.66(14) . . ? O12 S4 O11 110.97(14) . . ? O10 S4 C11 108.07(14) . . ? O12 S4 C11 106.58(14) . . ? O11 S4 C11 104.18(14) . . ? O6 S2 O5 113.46(16) . . ? O6 S2 O4 111.84(15) . . ? O5 S2 O4 111.41(15) . . ? O6 S2 C3 108.81(15) . . ? O5 S2 C3 105.47(15) . . ? O4 S2 C3 105.26(14) . . ? O2 S1 O3 111.98(15) . . ? O2 S1 O1 113.26(15) . . ? O3 S1 O1 111.76(15) . . ? O2 S1 C1 106.21(15) . . ? O3 S1 C1 105.90(14) . . ? O1 S1 C1 107.17(14) . . ? H15D O15 H15F 109.3 . . ? C30 O14 H14D 109.9 . . ? H16D O16 H16F 102.1 . . ? H17D O17 H17F 129.8 . . ? C19 N5 H5B 120.0 . . ? C19 N5 H5C 120.0 . . ? H5B N5 H5C 120.0 . . ? C20 N10 H10A 109.5 . . ? C20 N10 H10B 109.5 . . ? H10A N10 H10B 109.5 . . ? C20 N10 H10C 109.5 . . ? H10A N10 H10C 109.5 . . ? H10B N10 H10C 109.5 . . ? C19 N4 H4B 120.0 . . ? C19 N4 H4C 120.0 . . ? H4B N4 H4C 120.0 . . ? C19 N6 H6B 120.0 . . ? C19 N6 H6C 120.0 . . ? H6B N6 H6C 120.0 . . ? C17 N1 H1B 120.0 . . ? C17 N1 H1C 120.0 . . ? H1B N1 H1C 120.0 . . ? C17 N2 H2B 120.0 . . ? C17 N2 H2C 120.0 . . ? H2B N2 H2C 120.0 . . ? C17 N3 H3B 120.0 . . ? C17 N3 H3C 120.0 . . ? H3B N3 H3C 120.0 . . ? C18 N9 H9B 120.0 . . ? C18 N9 H9C 120.0 . . ? H9B N9 H9C 120.0 . . ? C18 N8 H8C 120.0 . . ? C18 N8 H8D 120.0 . . ? H8C N8 H8D 120.0 . . ? C18 N7 H7C 120.0 . . ? C18 N7 H7D 120.0 . . ? H7C N7 H7D 120.0 . . ? C13 C9 C10 118.5(3) . . ? C13 C9 C8 123.5(3) . . ? C10 C9 C8 118.0(3) . . ? C12 C10 C9 120.0(3) . . ? C12 C10 C5 120.1(3) . . ? C9 C10 C5 119.8(3) . . ? C11 C12 C10 118.6(3) . . ? C11 C12 C15 122.9(3) . . ? C10 C12 C15 118.4(3) . . ? C3 C4 C7 123.7(3) . . ? C3 C4 C5 118.6(3) . . ? C7 C4 C5 117.6(3) . . ? C10 C5 C6 119.7(3) . . ? C10 C5 C4 120.2(3) . . ? C6 C5 C4 120.1(3) . . ? C1 C6 C5 118.4(3) . . ? C1 C6 C16 123.5(3) . . ? C5 C6 C16 118.1(3) . . ? C15 C16 C6 122.2(3) . . ? C15 C16 H16A 118.9 . . ? C6 C16 H16A 118.9 . . ? C7 C8 C9 122.2(3) . . ? C7 C8 H8B 118.9 . . ? C9 C8 H8B 118.9 . . ? C3 C2 C1 121.1(3) . . ? C3 C2 H2D 119.4 . . ? C1 C2 H2D 119.4 . . ? C14 C11 C12 121.0(3) . . ? C14 C11 S4 117.7(2) . . ? C12 C11 S4 121.0(2) . . ? C11 C14 C13 120.4(3) . . ? C11 C14 H14A 119.8 . . ? C13 C14 H14A 119.8 . . ? C14 C13 C9 121.3(3) . . ? C14 C13 S3 117.9(2) . . ? C9 C13 S3 120.7(2) . . ? C16 C15 C12 121.4(3) . . ? C16 C15 H15A 119.3 . . ? C12 C15 H15A 119.3 . . ? C8 C7 C4 122.2(3) . . ? C8 C7 H7B 118.9 . . ? C4 C7 H7B 118.9 . . ? C2 C3 C4 120.9(3) . . ? C2 C3 S2 116.2(2) . . ? C4 C3 S2 122.9(2) . . ? N4 C19 N6 120.4(3) . . ? N4 C19 N5 120.5(3) . . ? N6 C19 N5 119.1(3) . . ? C2 C1 C6 120.8(3) . . ? C2 C1 S1 116.8(2) . . ? C6 C1 S1 122.3(2) . . ? N2 C17 N3 120.9(4) . . ? N2 C17 N1 119.8(4) . . ? N3 C17 N1 119.2(4) . . ? C24 C25 C26 114.7(3) . . ? C24 C25 H25A 108.6 . . ? C26 C25 H25A 108.6 . . ? C24 C25 H25B 108.6 . . ? C26 C25 H25B 108.6 . . ? H25A C25 H25B 107.6 . . ? C28 C27 C26 113.8(3) . . ? C28 C27 H27A 108.8 . . ? C26 C27 H27A 108.8 . . ? C28 C27 H27B 108.8 . . ? C26 C27 H27B 108.8 . . ? H27A C27 H27B 107.7 . . ? C27 C28 C29 112.6(3) . . ? C27 C28 H28A 109.1 . . ? C29 C28 H28A 109.1 . . ? C27 C28 H28B 109.1 . . ? C29 C28 H28B 109.1 . . ? H28A C28 H28B 107.8 . . ? C22 C23 C24 114.5(3) . . ? C22 C23 H23A 108.6 . . ? C24 C23 H23A 108.6 . . ? C22 C23 H23B 108.6 . . ? C24 C23 H23B 108.6 . . ? H23A C23 H23B 107.6 . . ? C23 C22 C21 113.6(3) . . ? C23 C22 H22A 108.9 . . ? C21 C22 H22A 108.9 . . ? C23 C22 H22B 108.9 . . ? C21 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? C25 C24 C23 114.3(3) . . ? C25 C24 H24A 108.7 . . ? C23 C24 H24A 108.7 . . ? C25 C24 H24B 108.7 . . ? C23 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? C20 C21 C22 114.4(3) . . ? C20 C21 H21A 108.7 . . ? C22 C21 H21A 108.7 . . ? C20 C21 H21B 108.7 . . ? C22 C21 H21B 108.7 . . ? H21A C21 H21B 107.6 . . ? C25 C26 C27 113.8(3) . . ? C25 C26 H26A 108.8 . . ? C27 C26 H26A 108.8 . . ? C25 C26 H26B 108.8 . . ? C27 C26 H26B 108.8 . . ? H26A C26 H26B 107.7 . . ? O13 C30 O14 122.1(4) . . ? O13 C30 C29 125.4(4) . . ? O14 C30 C29 112.5(3) . . ? C30 C29 C28 113.4(3) . . ? C30 C29 H29A 108.9 . . ? C28 C29 H29A 108.9 . . ? C30 C29 H29B 108.9 . . ? C28 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? N10 C20 C21 111.3(3) . . ? N10 C20 H20A 109.4 . . ? C21 C20 H20A 109.4 . . ? N10 C20 H20B 109.4 . . ? C21 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? N9 C18 N8 119.4(4) . . ? N9 C18 N7 119.5(5) . . ? N8 C18 N7 121.0(4) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.419 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.067