# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 440/108 data_ig129 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C77 H91 N6 O12 P S' _chemical_formula_weight 1355.59 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' 'P' 'P' 0.1023 0.0942 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.2730(10) _cell_length_b 15.6930(10) _cell_length_c 16.7140(10) _cell_angle_alpha 82.1390(10) _cell_angle_beta 81.1230(10) _cell_angle_gamma 73.6740(10) _cell_volume 3532.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(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 1.274 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1444 _exptl_absorpt_coefficient_mu 0.135 _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 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14654 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1361 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 28.27 _reflns_number_total 14654 _reflns_number_gt 7426 _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^)+(0.1000P)^2^+0.0000P] 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 14654 _refine_ls_number_parameters 874 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1615 _refine_ls_R_factor_gt 0.0718 _refine_ls_wR_factor_ref 0.2055 _refine_ls_wR_factor_gt 0.1654 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.981 _refine_ls_shift/su_max 2.104 _refine_ls_shift/su_mean 0.080 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 S2 S 0.11477(7) 0.37758(7) 0.82705(6) 0.0327(3) Uani 1 1 d . . . P1 P 0.18964(7) 0.35237(7) 0.91822(5) 0.0232(2) Uani 1 1 d . . . O3 O 0.59852(18) 0.46037(17) 1.20586(15) 0.0289(6) Uani 1 1 d . . . O4 O 0.77488(18) 0.47279(16) 1.44433(14) 0.0270(6) Uani 1 1 d . . . O5 O 0.44828(19) 0.03897(17) 1.60446(15) 0.0310(6) Uani 1 1 d . . . O6 O 0.68794(19) -0.02105(18) 1.12209(15) 0.0330(6) Uani 1 1 d . . . O7 O 0.07104(19) 0.47461(19) 1.41625(15) 0.0339(7) Uani 1 1 d . . . O8 O 0.88104(18) -0.05466(17) 1.33250(14) 0.0286(6) Uani 1 1 d . . . O9 O 0.61810(18) 0.49628(16) 1.54854(15) 0.0306(6) Uani 1 1 d . . . O11 O 0.66417(19) 0.07909(19) 0.98725(15) 0.0362(7) Uani 1 1 d . . . O12 O 0.38932(18) 0.20075(16) 1.65719(15) 0.0290(6) Uani 1 1 d . . . O13 O 0.9752(2) 0.06689(18) 1.29022(15) 0.0366(7) Uani 1 1 d . . . O14 O 0.1413(2) 0.29586(19) 1.45543(15) 0.0364(7) Uani 1 1 d . . . O16 O 0.41309(19) 0.5256(2) 1.19638(17) 0.0433(8) Uani 1 1 d . . . N10 N 0.1375(2) 0.4211(2) 0.99063(17) 0.0249(7) Uani 1 1 d . . . N15 N 0.2014(2) 0.2500(2) 0.96495(17) 0.0253(7) Uani 1 1 d . . . N17 N 0.2934(2) 0.2111(2) 0.99076(18) 0.0261(7) Uani 1 1 d . . . N18 N 0.3028(2) 0.3646(2) 0.89333(16) 0.0239(7) Uani 1 1 d . . . N19 N 0.3409(2) 0.3853(2) 0.95793(17) 0.0231(7) Uani 1 1 d . . . N20 N 0.1497(2) 0.3830(2) 1.06959(17) 0.0251(7) Uani 1 1 d . . . C21 C 0.3039(3) 0.1462(3) 1.0469(2) 0.0268(8) Uani 1 1 d . . . H21A H 0.2780 0.1011 1.0308 0.032 Uiso 1 1 calc R . . H21B H 0.2626 0.1680 1.0956 0.032 Uiso 1 1 calc R . . C22 C 0.7484(3) 0.2673(2) 1.6254(2) 0.0246(8) Uani 1 1 d . . . C23 C 0.1296(3) 0.4351(3) 1.1264(2) 0.0264(8) Uani 1 1 d . . . H23A H 0.0628 0.4721 1.1238 0.032 Uiso 1 1 calc R . . H23B H 0.1726 0.4745 1.1137 0.032 Uiso 1 1 calc R . . C24 C 0.4209(3) 0.4452(3) 1.0795(2) 0.0293(9) Uani 1 1 d . . . H24 H 0.3537 0.4680 1.0768 0.035 Uiso 1 1 calc R . . C25 C 0.7700(3) 0.4009(2) 1.5000(2) 0.0233(8) Uani 1 1 d . . . C26 C 0.8486(3) 0.4592(3) 1.3748(2) 0.0299(9) Uani 1 1 d . . . H26A H 0.9110 0.4250 1.3928 0.036 Uiso 1 1 calc R . . H26B H 0.8563 0.5166 1.3495 0.036 Uiso 1 1 calc R . . C27 C 0.6864(3) 0.4149(2) 1.5581(2) 0.0255(8) Uani 1 1 d . . . C28 C 0.4165(3) 0.0483(3) 1.1406(2) 0.0306(9) Uani 1 1 d . . . H28 H 0.3620 0.0403 1.1761 0.037 Uiso 1 1 calc R . . C29 C 0.8230(3) 0.4107(3) 1.3125(2) 0.0267(8) Uani 1 1 d . . . H29A H 0.8256 0.3498 1.3347 0.032 Uiso 1 1 calc R . . H29B H 0.8711 0.4088 1.2645 0.032 Uiso 1 1 calc R . . C30 C 0.1786(3) 0.2739(3) 1.3146(2) 0.0338(10) Uani 1 1 d . . . H30 H 0.2051 0.2134 1.3288 0.041 Uiso 1 1 calc R . . C31 C 0.8400(3) 0.3199(2) 1.5061(2) 0.0257(8) Uani 1 1 d . . . H31 H 0.8955 0.3103 1.4677 0.031 Uiso 1 1 calc R . . C32 C 0.1061(3) 0.4217(3) 1.3537(2) 0.0270(9) Uani 1 1 d . . . C33 C 0.5638(3) 0.4335(2) 1.1447(2) 0.0243(8) Uani 1 1 d . . . C34 C 0.7978(3) 0.0195(2) 1.6164(2) 0.0277(9) Uani 1 1 d . . . H34A H 0.8043 -0.0441 1.6262 0.033 Uiso 1 1 calc R . . H34B H 0.8339 0.0346 1.6545 0.033 Uiso 1 1 calc R . . C35 C 0.6989(3) 0.4174(3) 1.2186(2) 0.0279(9) Uani 1 1 d . . . H35A H 0.7427 0.4277 1.1699 0.033 Uiso 1 1 calc R . . H35B H 0.7081 0.3536 1.2311 0.033 Uiso 1 1 calc R . . C36 C 0.5573(3) 0.1925(2) 1.6749(2) 0.0254(8) Uani 1 1 d . . . H36 H 0.5353 0.2470 1.6969 0.031 Uiso 1 1 calc R . . C37 C 0.9103(3) 0.1648(2) 1.5667(2) 0.0284(9) Uani 1 1 d . . . H37A H 0.9099 0.1343 1.6213 0.034 Uiso 1 1 calc R . . H37B H 0.9738 0.1773 1.5513 0.034 Uiso 1 1 calc R . . C38 C 0.6776(3) 0.3491(2) 1.6199(2) 0.0253(8) Uani 1 1 d . . . H38 H 0.6230 0.3595 1.6591 0.030 Uiso 1 1 calc R . . C39 C 0.6897(3) 0.0684(2) 1.6343(2) 0.0252(8) Uani 1 1 d . . . C40 C 0.1371(3) 0.3963(3) 1.2110(2) 0.0267(8) Uani 1 1 d . . . C41 C 0.8456(3) 0.0392(2) 1.5305(2) 0.0247(8) Uani 1 1 d . . . C42 C 0.4862(3) 0.1149(2) 1.0164(2) 0.0270(8) Uani 1 1 d . . . H42 H 0.4780 0.1524 0.9684 0.032 Uiso 1 1 calc R . . C43 C 0.3660(3) 0.2901(2) 1.6183(2) 0.0275(8) Uani 1 1 d . . . H43A H 0.4062 0.3229 1.6358 0.033 Uiso 1 1 calc R . . H43B H 0.2976 0.3195 1.6352 0.033 Uiso 1 1 calc R . . C44 C 0.7033(3) -0.0770(3) 1.1970(2) 0.0301(9) Uani 1 1 d . . . H44A H 0.6742 -0.1263 1.1997 0.036 Uiso 1 1 calc R . . H44B H 0.6733 -0.0431 1.2430 0.036 Uiso 1 1 calc R . . C45 C 0.8389(3) -0.1682(3) 1.2777(2) 0.0291(9) Uani 1 1 d . . . H45A H 0.7999 -0.2111 1.2888 0.035 Uiso 1 1 calc R . . H45B H 0.9075 -0.2015 1.2702 0.035 Uiso 1 1 calc R . . C46 C 0.5926(3) 0.0172(3) 1.1085(2) 0.0290(9) Uani 1 1 d . . . C47 C 0.5770(3) 0.3546(3) 1.0281(2) 0.0313(9) Uani 1 1 d . . . H47 H 0.6159 0.3169 0.9904 0.038 Uiso 1 1 calc R . . C48 C 0.4339(3) 0.3660(2) 0.9574(2) 0.0248(8) Uani 1 1 d . . . H48A H 0.4600 0.3942 0.9068 0.030 Uiso 1 1 calc R . . H48B H 0.4587 0.3021 0.9548 0.030 Uiso 1 1 calc R . . C49 C 0.8977(2) 0.1033(2) 1.5085(2) 0.0238(8) Uani 1 1 d . . . C50 C 0.4028(3) 0.1020(2) 1.0694(2) 0.0283(9) Uani 1 1 d . . . C51 C 0.9340(3) 0.0610(3) 1.3703(2) 0.0284(9) Uani 1 1 d . . . C52 C 0.8308(3) 0.2521(2) 1.5676(2) 0.0243(8) Uani 1 1 d . . . C53 C 0.5789(3) 0.0723(3) 1.0357(2) 0.0286(9) Uani 1 1 d . . . C54 C 0.5252(3) 0.5053(3) 1.5975(2) 0.0336(9) Uani 1 1 d . . . H54A H 0.4837 0.5642 1.5863 0.050 Uiso 1 1 calc R . . H54B H 0.5349 0.4954 1.6540 0.050 Uiso 1 1 calc R . . H54C H 0.4947 0.4621 1.5852 0.050 Uiso 1 1 calc R . . C55 C 0.4775(3) 0.3885(2) 1.0230(2) 0.0250(8) Uani 1 1 d . . . C56 C 0.5105(3) 0.0054(3) 1.1611(2) 0.0301(9) Uani 1 1 d . . . H56 H 0.5184 -0.0309 1.2098 0.036 Uiso 1 1 calc R . . C57 C 0.6197(3) 0.3768(3) 1.0895(2) 0.0316(9) Uani 1 1 d . . . H57 H 0.6866 0.3528 1.0929 0.038 Uiso 1 1 calc R . . C58 C 0.1439(3) 0.3303(3) 1.3742(2) 0.0289(9) Uani 1 1 d . . . C59 C 0.8822(3) -0.0038(2) 1.3925(2) 0.0240(8) Uani 1 1 d . . . C60 C 0.5358(3) 0.2745(3) 1.3314(3) 0.0345(10) Uani 1 1 d . . . H60 H 0.4771 0.3150 1.3487 0.041 Uiso 1 1 calc R . . C61 C 0.0408(3) 0.5685(3) 1.3959(2) 0.0353(10) Uani 1 1 d . . . H61A H 0.0178 0.5978 1.4448 0.053 Uiso 1 1 calc R . . H61B H -0.0113 0.5826 1.3623 0.053 Uiso 1 1 calc R . . H61C H 0.0955 0.5886 1.3670 0.053 Uiso 1 1 calc R . . C62 C 0.7207(3) 0.4566(3) 1.2885(2) 0.0307(9) Uani 1 1 d . . . H62A H 0.6721 0.4513 1.3350 0.037 Uiso 1 1 calc R . . H62B H 0.7153 0.5196 1.2736 0.037 Uiso 1 1 calc R . . C63 C 0.8221(3) -0.1171(2) 1.3508(2) 0.0263(8) Uani 1 1 d . . . H63A H 0.7531 -0.0857 1.3617 0.032 Uiso 1 1 calc R . . H63B H 0.8413 -0.1574 1.3984 0.032 Uiso 1 1 calc R . . C64 C 0.7258(3) 0.1971(2) 1.6928(2) 0.0257(8) Uani 1 1 d . . . H64A H 0.7867 0.1538 1.7048 0.031 Uiso 1 1 calc R . . H64B H 0.6954 0.2255 1.7418 0.031 Uiso 1 1 calc R . . C65 C 0.8380(3) -0.0128(2) 1.4717(2) 0.0248(8) Uani 1 1 d . . . H65 H 0.8021 -0.0548 1.4862 0.030 Uiso 1 1 calc R . . C66 C 0.4625(3) 0.4681(3) 1.1394(2) 0.0278(9) Uani 1 1 d . . . C67 C 0.1181(3) 0.5178(2) 0.9705(2) 0.0298(9) Uani 1 1 d . . . H67A H 0.1116 0.5322 0.9135 0.045 Uiso 1 1 calc R . . H67B H 0.1716 0.5375 0.9829 0.045 Uiso 1 1 calc R . . H67C H 0.0582 0.5472 1.0018 0.045 Uiso 1 1 calc R . . C68 C 0.3683(3) 0.3173(3) 0.8273(2) 0.0291(9) Uani 1 1 d . . . H68A H 0.3297 0.3090 0.7882 0.044 Uiso 1 1 calc R . . H68B H 0.4054 0.2603 0.8493 0.044 Uiso 1 1 calc R . . H68C H 0.4124 0.3518 0.8013 0.044 Uiso 1 1 calc R . . C69 C 0.2074(3) 0.3195(3) 1.5001(2) 0.0329(9) Uani 1 1 d . . . H69A H 0.1820 0.3172 1.5574 0.040 Uiso 1 1 calc R . . H69B H 0.2098 0.3803 1.4818 0.040 Uiso 1 1 calc R . . C70 C 0.1033(3) 0.4538(3) 1.2723(2) 0.0263(8) Uani 1 1 d . . . H70 H 0.0785 0.5146 1.2583 0.032 Uiso 1 1 calc R . . C71 C 0.5194(3) 0.0736(3) 1.6221(2) 0.0274(9) Uani 1 1 d . . . C72 C 0.3826(3) 0.2930(3) 1.5270(2) 0.0306(9) Uani 1 1 d . . . H72A H 0.4487 0.2574 1.5109 0.037 Uiso 1 1 calc R . . H72B H 0.3784 0.3541 1.5044 0.037 Uiso 1 1 calc R . . C73 C 0.1750(3) 0.3058(3) 1.2328(2) 0.0328(9) Uani 1 1 d . . . H73 H 0.1979 0.2665 1.1928 0.039 Uiso 1 1 calc R . . C74 C 0.8136(3) -0.1115(3) 1.1987(2) 0.0280(9) Uani 1 1 d . . . H74A H 0.8421 -0.0613 1.1923 0.034 Uiso 1 1 calc R . . H74B H 0.8422 -0.1468 1.1533 0.034 Uiso 1 1 calc R . . C75 C 0.6206(3) 0.0300(2) 1.6140(2) 0.0272(9) Uani 1 1 d . . . H75 H 0.6419 -0.0259 1.5946 0.033 Uiso 1 1 calc R . . C76 C 0.3096(3) 0.2589(3) 1.4898(2) 0.0313(9) Uani 1 1 d . . . H76A H 0.3314 0.2541 1.4323 0.038 Uiso 1 1 calc R . . H76B H 0.3089 0.1998 1.5157 0.038 Uiso 1 1 calc R . . C77 C 0.6579(3) 0.1499(2) 1.6678(2) 0.0251(8) Uani 1 1 d . . . C78 C 0.6539(3) 0.1337(3) 0.9120(2) 0.0359(10) Uani 1 1 d . . . H78A H 0.7179 0.1334 0.8837 0.054 Uiso 1 1 calc R . . H78B H 0.6184 0.1937 0.9224 0.054 Uiso 1 1 calc R . . H78C H 0.6186 0.1110 0.8793 0.054 Uiso 1 1 calc R . . C79 C 1.0091(3) 0.1442(3) 1.2613(3) 0.0446(11) Uani 1 1 d . . . H79A H 1.0363 0.1411 1.2052 0.067 Uiso 1 1 calc R . . H79B H 1.0587 0.1468 1.2930 0.067 Uiso 1 1 calc R . . H79C H 0.9550 0.1966 1.2663 0.067 Uiso 1 1 calc R . . C80 C 0.9233(8) 0.1554(17) 0.8249(9) 0.221(14) Uani 1 1 d . . . H80 H 0.9394 0.1583 0.7687 0.265 Uiso 1 1 calc R . . C81 C 0.1155(3) 0.2190(3) 1.0004(2) 0.0359(10) Uani 1 1 d . . . H81A H 0.0592 0.2541 0.9751 0.054 Uiso 1 1 calc R . . H81B H 0.1038 0.2248 1.0578 0.054 Uiso 1 1 calc R . . H81C H 0.1270 0.1575 0.9917 0.054 Uiso 1 1 calc R . . C82 C 0.9414(3) 0.1129(3) 1.4275(2) 0.0284(9) Uani 1 1 d . . . H82 H 0.9764 0.1556 1.4124 0.034 Uiso 1 1 calc R . . C83 C 0.7116(4) 0.1585(3) 1.2828(3) 0.0496(12) Uani 1 1 d . . . H83 H 0.7713 0.1192 1.2659 0.059 Uiso 1 1 calc R . . C84 C 0.4894(3) 0.1572(2) 1.6507(2) 0.0264(8) Uani 1 1 d . . . C85 C 0.5437(4) 0.2339(3) 1.2627(3) 0.0481(12) Uani 1 1 d . . . C86 C 0.6182(3) 0.2547(3) 1.3771(3) 0.0548(14) Uani 1 1 d . . . H86 H 0.6108 0.2824 1.4243 0.066 Uiso 1 1 calc R . . C87 C 0.4747(3) -0.0544(3) 1.5957(3) 0.0394(10) Uani 1 1 d . . . H87A H 0.4189 -0.0707 1.5833 0.059 Uiso 1 1 calc R . . H87B H 0.4954 -0.0875 1.6455 0.059 Uiso 1 1 calc R . . H87C H 0.5275 -0.0679 1.5523 0.059 Uiso 1 1 calc R . . C88 C 0.6364(3) 0.1737(3) 1.2361(3) 0.0461(12) Uani 1 1 d . . . H88 H 0.6451 0.1460 1.1888 0.055 Uiso 1 1 calc R . . C89 C 0.8481(6) 0.1486(7) 1.0705(5) 0.155(4) Uani 1 1 d . . . H89A H 0.8281 0.2088 1.0848 0.232 Uiso 1 1 calc R . . H89B H 0.9037 0.1153 1.0977 0.232 Uiso 1 1 calc R . . H89C H 0.7948 0.1214 1.0868 0.232 Uiso 1 1 calc R . . C90 C 0.3097(3) 0.5573(5) 1.1955(3) 0.091(2) Uani 1 1 d . . . H90A H 0.2821 0.5966 1.2374 0.136 Uiso 1 1 calc R . . H90B H 0.2812 0.5076 1.2051 0.136 Uiso 1 1 calc R . . H90C H 0.2959 0.5890 1.1435 0.136 Uiso 1 1 calc R . . C91 C 0.4610(4) 0.2473(4) 1.2195(4) 0.0706(17) Uani 1 1 d . . . H91A H 0.4803 0.2137 1.1730 0.106 Uiso 1 1 calc R . . H91B H 0.4375 0.3096 1.2018 0.106 Uiso 1 1 calc R . . H91C H 0.4097 0.2277 1.2546 0.106 Uiso 1 1 calc R . . C92 C 0.7040(4) 0.1988(3) 1.3549(3) 0.0538(13) Uani 1 1 d . . . H92 H 0.7565 0.1867 1.3853 0.065 Uiso 1 1 calc R . . C93 C 0.8735(4) 0.1487(5) 0.9876(3) 0.0721(18) Uani 1 1 d . . . C94 C 0.8681(4) 0.2379(5) 0.9426(5) 0.086(2) Uani 1 1 d . . . H94 H 0.8482 0.2903 0.9681 0.104 Uiso 1 1 calc R . . C95 C 0.9058(5) 0.0819(5) 0.9387(7) 0.105(3) Uani 1 1 d . . . H95 H 0.9118 0.0275 0.9702 0.126 Uiso 1 1 calc R . . C96 C 0.8943(6) 0.2366(9) 0.8621(6) 0.130(4) Uani 1 1 d . . . H96 H 0.8936 0.2899 0.8299 0.157 Uiso 1 1 calc R . . C97 C 0.9293(9) 0.0691(18) 0.8688(12) 0.319(18) Uani 1 1 d . . . H97 H 0.9477 0.0144 0.8472 0.383 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 S2 0.0325(6) 0.0427(6) 0.0241(5) -0.0031(5) -0.0104(4) -0.0083(5) P1 0.0232(5) 0.0289(5) 0.0176(5) -0.0040(4) -0.0026(4) -0.0064(4) O3 0.0257(14) 0.0366(16) 0.0270(14) -0.0059(12) -0.0086(10) -0.0084(12) O4 0.0287(14) 0.0267(14) 0.0239(14) 0.0003(11) -0.0014(10) -0.0070(11) O5 0.0347(16) 0.0250(15) 0.0340(15) -0.0070(12) 0.0007(12) -0.0099(12) O6 0.0320(16) 0.0400(17) 0.0251(14) 0.0085(13) -0.0077(11) -0.0098(13) O7 0.0352(16) 0.0445(18) 0.0197(13) -0.0117(13) -0.0003(11) -0.0045(13) O8 0.0318(15) 0.0318(15) 0.0242(14) -0.0073(12) 0.0008(11) -0.0119(12) O9 0.0237(14) 0.0236(14) 0.0367(16) 0.0012(12) 0.0020(11) 0.0011(11) O11 0.0307(15) 0.0489(18) 0.0245(15) 0.0129(13) -0.0031(11) -0.0110(13) O12 0.0298(15) 0.0237(14) 0.0288(14) 0.0025(12) 0.0017(11) -0.0049(11) O13 0.0435(17) 0.0405(17) 0.0300(15) -0.0075(13) 0.0077(12) -0.0224(14) O14 0.0471(18) 0.0473(18) 0.0214(14) -0.0006(13) -0.0067(12) -0.0231(14) O16 0.0239(15) 0.065(2) 0.0446(17) -0.0291(16) -0.0044(12) -0.0063(14) N10 0.0273(17) 0.0285(18) 0.0161(15) -0.0027(14) -0.0035(12) -0.0024(14) N15 0.0221(16) 0.0344(18) 0.0203(16) -0.0017(14) -0.0025(12) -0.0094(14) N17 0.0277(18) 0.0251(17) 0.0249(17) -0.0032(14) -0.0057(13) -0.0047(14) N18 0.0282(17) 0.0304(17) 0.0146(15) -0.0037(13) -0.0026(12) -0.0096(14) N19 0.0250(17) 0.0291(17) 0.0178(15) -0.0033(13) -0.0018(12) -0.0116(14) N20 0.0237(17) 0.0312(18) 0.0194(16) -0.0024(14) -0.0019(12) -0.0062(14) C21 0.035(2) 0.029(2) 0.0198(19) -0.0097(17) -0.0010(15) -0.0104(17) C22 0.030(2) 0.0215(19) 0.0233(19) -0.0027(16) -0.0092(15) -0.0050(16) C23 0.0161(18) 0.041(2) 0.0245(19) -0.0071(18) -0.0001(14) -0.0105(17) C24 0.021(2) 0.033(2) 0.035(2) -0.0069(19) -0.0044(15) -0.0063(17) C25 0.026(2) 0.024(2) 0.0232(19) -0.0017(16) -0.0069(14) -0.0098(16) C26 0.025(2) 0.035(2) 0.029(2) 0.0033(18) -0.0033(15) -0.0097(18) C27 0.026(2) 0.023(2) 0.027(2) -0.0078(16) -0.0045(15) -0.0021(16) C28 0.037(2) 0.035(2) 0.020(2) 0.0008(18) -0.0001(16) -0.0133(19) C29 0.025(2) 0.032(2) 0.0229(19) -0.0018(17) -0.0032(14) -0.0068(17) C30 0.044(3) 0.032(2) 0.028(2) -0.0005(19) -0.0118(17) -0.0115(19) C31 0.022(2) 0.032(2) 0.0255(19) -0.0122(17) -0.0039(14) -0.0072(17) C32 0.0210(19) 0.046(2) 0.0167(18) -0.0107(18) 0.0013(14) -0.0110(18) C33 0.027(2) 0.026(2) 0.0219(19) -0.0010(16) -0.0040(14) -0.0101(16) C34 0.030(2) 0.023(2) 0.029(2) -0.0016(17) -0.0075(16) -0.0025(16) C35 0.024(2) 0.036(2) 0.026(2) 0.0008(18) -0.0070(15) -0.0104(17) C36 0.034(2) 0.022(2) 0.0179(18) -0.0023(16) -0.0004(15) -0.0053(17) C37 0.024(2) 0.028(2) 0.030(2) -0.0042(17) -0.0086(15) 0.0010(16) C38 0.026(2) 0.029(2) 0.0204(19) -0.0058(16) 0.0004(14) -0.0055(16) C39 0.033(2) 0.022(2) 0.0158(18) 0.0008(15) -0.0021(14) -0.0015(16) C40 0.026(2) 0.037(2) 0.0190(19) -0.0033(17) -0.0032(14) -0.0109(17) C41 0.024(2) 0.0193(19) 0.0249(19) -0.0030(16) -0.0047(14) 0.0043(15) C42 0.033(2) 0.028(2) 0.0200(19) 0.0009(17) -0.0056(15) -0.0092(17) C43 0.029(2) 0.0197(19) 0.033(2) -0.0035(17) -0.0087(16) -0.0028(16) C44 0.039(2) 0.030(2) 0.022(2) 0.0072(17) -0.0099(16) -0.0114(18) C45 0.028(2) 0.027(2) 0.031(2) -0.0048(18) -0.0046(16) -0.0044(17) C46 0.032(2) 0.036(2) 0.021(2) 0.0034(17) -0.0076(15) -0.0124(18) C47 0.030(2) 0.038(2) 0.027(2) -0.0069(18) -0.0042(16) -0.0095(18) C48 0.036(2) 0.0158(18) 0.0235(19) 0.0031(16) -0.0047(15) -0.0097(16) C49 0.0191(19) 0.023(2) 0.027(2) -0.0069(16) -0.0064(14) 0.0023(15) C50 0.031(2) 0.026(2) 0.027(2) -0.0044(17) -0.0026(16) -0.0053(17) C51 0.023(2) 0.031(2) 0.028(2) -0.0029(18) 0.0002(15) -0.0044(17) C52 0.024(2) 0.027(2) 0.0241(19) -0.0067(17) -0.0088(15) -0.0053(16) C53 0.033(2) 0.035(2) 0.0187(19) 0.0033(17) -0.0023(15) -0.0134(18) C54 0.027(2) 0.027(2) 0.040(2) -0.0041(19) 0.0028(17) 0.0005(17) C55 0.030(2) 0.024(2) 0.0222(19) -0.0006(16) -0.0038(15) -0.0082(16) C56 0.039(2) 0.032(2) 0.0176(19) 0.0073(17) -0.0045(16) -0.0104(18) C57 0.028(2) 0.034(2) 0.032(2) -0.0069(19) -0.0061(16) -0.0039(18) C58 0.031(2) 0.037(2) 0.023(2) -0.0007(18) -0.0053(15) -0.0157(18) C59 0.0212(19) 0.023(2) 0.027(2) -0.0063(17) -0.0034(14) -0.0026(15) C60 0.032(2) 0.026(2) 0.043(3) 0.0016(19) -0.0015(18) -0.0078(18) C61 0.037(2) 0.042(3) 0.030(2) -0.0153(19) -0.0008(17) -0.011(2) C62 0.025(2) 0.036(2) 0.031(2) -0.0023(19) -0.0093(16) -0.0071(18) C63 0.027(2) 0.023(2) 0.028(2) 0.0003(17) -0.0067(15) -0.0057(16) C64 0.035(2) 0.025(2) 0.0180(18) -0.0013(16) -0.0058(15) -0.0066(17) C65 0.024(2) 0.0209(19) 0.027(2) -0.0030(16) -0.0011(15) -0.0022(16) C66 0.027(2) 0.030(2) 0.028(2) -0.0053(18) -0.0048(15) -0.0083(17) C67 0.029(2) 0.029(2) 0.027(2) -0.0002(17) -0.0014(16) -0.0041(17) C68 0.029(2) 0.036(2) 0.0219(19) -0.0056(17) -0.0038(15) -0.0059(18) C69 0.039(2) 0.039(2) 0.022(2) 0.0001(18) -0.0130(16) -0.0092(19) C70 0.022(2) 0.033(2) 0.0250(19) -0.0068(17) -0.0007(14) -0.0073(16) C71 0.033(2) 0.031(2) 0.0188(19) -0.0010(17) 0.0012(15) -0.0126(18) C72 0.036(2) 0.030(2) 0.025(2) 0.0016(17) 0.0004(16) -0.0106(18) C73 0.042(2) 0.035(2) 0.025(2) -0.0103(18) -0.0053(17) -0.0115(19) C74 0.032(2) 0.027(2) 0.024(2) -0.0045(17) -0.0010(15) -0.0071(17) C75 0.039(2) 0.0194(19) 0.0195(19) 0.0006(16) -0.0014(15) -0.0031(17) C76 0.037(2) 0.033(2) 0.0230(19) -0.0073(17) 0.0025(16) -0.0077(18) C77 0.035(2) 0.023(2) 0.0143(18) 0.0031(16) -0.0029(14) -0.0054(17) C78 0.042(3) 0.037(2) 0.025(2) 0.0102(19) -0.0027(17) -0.013(2) C79 0.057(3) 0.047(3) 0.035(2) -0.001(2) 0.000(2) -0.026(2) C80 0.039(6) 0.56(4) 0.103(8) -0.110(14) 0.014(5) -0.126(15) C81 0.037(2) 0.042(3) 0.031(2) 0.001(2) -0.0043(17) -0.017(2) C82 0.023(2) 0.027(2) 0.034(2) -0.0021(18) -0.0023(16) -0.0064(17) C83 0.067(3) 0.038(3) 0.046(3) -0.010(2) 0.001(2) -0.019(2) C84 0.029(2) 0.023(2) 0.0223(19) -0.0013(16) 0.0026(15) -0.0027(16) C85 0.068(3) 0.035(3) 0.046(3) 0.012(2) -0.011(2) -0.027(2) C86 0.045(3) 0.038(3) 0.070(4) 0.012(2) 0.007(2) -0.010(2) C87 0.052(3) 0.030(2) 0.039(2) -0.0031(19) -0.0036(19) -0.018(2) C88 0.045(3) 0.032(2) 0.055(3) 0.006(2) 0.000(2) -0.007(2) C89 0.081(6) 0.289(13) 0.101(6) -0.037(8) -0.014(5) -0.051(7) C90 0.027(3) 0.162(6) 0.092(4) -0.099(4) -0.002(3) -0.001(3) C91 0.078(4) 0.061(4) 0.078(4) 0.020(3) -0.019(3) -0.035(3) C92 0.047(3) 0.048(3) 0.062(3) 0.011(3) -0.011(2) -0.010(2) C93 0.034(3) 0.127(6) 0.051(3) -0.017(4) -0.013(2) -0.007(3) C94 0.044(4) 0.103(6) 0.113(6) 0.002(5) -0.021(4) -0.021(3) C95 0.049(4) 0.081(5) 0.198(9) -0.070(6) -0.030(5) -0.003(3) C96 0.056(5) 0.243(14) 0.094(7) 0.039(8) -0.013(5) -0.067(7) C97 0.054(7) 0.64(5) 0.25(2) -0.32(3) -0.045(11) 0.069(14) _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 S2 P1 1.9288(13) . ? P1 N15 1.663(3) . ? P1 N18 1.663(3) . ? P1 N10 1.677(3) . ? O3 C33 1.363(4) . ? O3 C35 1.436(4) . ? O4 C25 1.371(4) . ? O4 C26 1.437(4) . ? O5 C71 1.364(4) . ? O5 C87 1.430(5) . ? O6 C46 1.366(4) . ? O6 C44 1.436(4) . ? O7 C32 1.369(4) . ? O7 C61 1.423(5) . ? O8 C59 1.369(4) . ? O8 C63 1.436(4) . ? O9 C27 1.378(4) . ? O9 C54 1.428(4) . ? O11 C53 1.376(4) . ? O11 C78 1.424(4) . ? O12 C84 1.394(4) . ? O12 C43 1.434(4) . ? O13 C51 1.378(4) . ? O13 C79 1.426(5) . ? O14 C58 1.389(4) . ? O14 C69 1.441(4) . ? O16 C66 1.374(4) . ? O16 C90 1.420(5) . ? N10 N20 1.388(4) . ? N10 C67 1.464(5) . ? N15 N17 1.391(4) . ? N15 C81 1.458(5) . ? N17 C21 1.279(4) . ? N18 N19 1.394(4) . ? N18 C68 1.468(4) . ? N19 C48 1.276(4) . ? N20 C23 1.283(4) . ? C21 C50 1.469(5) . ? C22 C38 1.395(5) . ? C22 C52 1.389(5) . ? C22 C64 1.528(5) . ? C23 C40 1.468(5) . ? C24 C66 1.374(5) . ? C24 C55 1.389(5) . ? C25 C31 1.381(5) . ? C25 C27 1.403(5) . ? C26 C29 1.513(5) . ? C27 C38 1.374(5) . ? C28 C50 1.368(5) . ? C28 C56 1.393(5) . ? C29 C62 1.524(5) . ? C30 C58 1.365(5) . ? C30 C73 1.395(5) . ? C31 C52 1.394(5) . ? C32 C58 1.399(5) . ? C32 C70 1.388(5) . ? C33 C57 1.372(5) . ? C33 C66 1.406(5) . ? C34 C39 1.521(5) . ? C34 C41 1.522(5) . ? C35 C62 1.503(5) . ? C36 C84 1.375(5) . ? C36 C77 1.397(5) . ? C37 C52 1.514(5) . ? C37 C49 1.522(5) . ? C39 C75 1.394(5) . ? C39 C77 1.395(5) . ? C40 C73 1.389(5) . ? C40 C70 1.398(5) . ? C41 C65 1.395(5) . ? C41 C49 1.390(5) . ? C42 C53 1.371(5) . ? C42 C50 1.415(5) . ? C43 C72 1.504(5) . ? C44 C74 1.518(5) . ? C45 C63 1.505(5) . ? C45 C74 1.520(5) . ? C46 C53 1.398(5) . ? C46 C56 1.393(5) . ? C47 C55 1.382(5) . ? C47 C57 1.399(5) . ? C48 C55 1.467(5) . ? C49 C82 1.408(5) . ? C51 C82 1.373(5) . ? C51 C59 1.396(5) . ? C59 C65 1.383(5) . ? C60 C85 1.363(6) . ? C60 C86 1.438(6) . ? C64 C77 1.509(5) . ? C69 C76 1.500(5) . ? C71 C84 1.388(5) . ? C71 C75 1.407(5) . ? C72 C76 1.536(5) . ? C80 C97 1.44(3) . ? C80 C96 1.42(2) . ? C83 C88 1.371(7) . ? C83 C92 1.413(7) . ? C85 C91 1.429(7) . ? C85 C88 1.439(6) . ? C86 C92 1.324(6) . ? C89 C93 1.377(8) . ? C93 C95 1.352(9) . ? C93 C94 1.482(9) . ? C94 C96 1.341(11) . ? C95 C97 1.192(17) . ? 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 N15 P1 N18 106.53(15) . . ? N15 P1 N10 105.29(15) . . ? N18 P1 N10 105.18(15) . . ? N15 P1 S2 113.82(12) . . ? N18 P1 S2 113.30(11) . . ? N10 P1 S2 112.01(11) . . ? C33 O3 C35 116.7(3) . . ? C25 O4 C26 118.1(3) . . ? C71 O5 C87 117.3(3) . . ? C46 O6 C44 116.6(3) . . ? C32 O7 C61 117.7(3) . . ? C59 O8 C63 117.7(3) . . ? C27 O9 C54 116.5(3) . . ? C53 O11 C78 117.0(3) . . ? C84 O12 C43 114.7(3) . . ? C51 O13 C79 116.8(3) . . ? C58 O14 C69 114.8(3) . . ? C66 O16 C90 115.8(3) . . ? N20 N10 C67 120.9(3) . . ? N20 N10 P1 114.8(2) . . ? C67 N10 P1 119.9(2) . . ? N17 N15 C81 121.7(3) . . ? N17 N15 P1 113.6(2) . . ? C81 N15 P1 121.2(3) . . ? C21 N17 N15 119.8(3) . . ? N19 N18 C68 120.8(3) . . ? N19 N18 P1 113.2(2) . . ? C68 N18 P1 119.9(2) . . ? C48 N19 N18 119.1(3) . . ? C23 N20 N10 118.1(3) . . ? N17 C21 C50 119.0(3) . . ? C38 C22 C52 119.2(3) . . ? C38 C22 C64 116.7(3) . . ? C52 C22 C64 124.0(3) . . ? N20 C23 C40 119.2(4) . . ? C66 C24 C55 121.0(4) . . ? O4 C25 C31 126.7(3) . . ? O4 C25 C27 114.9(3) . . ? C31 C25 C27 118.3(3) . . ? O4 C26 C29 112.5(3) . . ? C38 C27 O9 124.5(3) . . ? C38 C27 C25 119.5(3) . . ? O9 C27 C25 116.0(3) . . ? C50 C28 C56 121.3(4) . . ? C26 C29 C62 111.3(3) . . ? C58 C30 C73 120.9(4) . . ? C52 C31 C25 122.6(3) . . ? O7 C32 C58 117.4(3) . . ? O7 C32 C70 123.5(4) . . ? C58 C32 C70 119.1(3) . . ? O3 C33 C57 125.1(3) . . ? O3 C33 C66 116.0(3) . . ? C57 C33 C66 119.0(3) . . ? C39 C34 C41 115.5(3) . . ? O3 C35 C62 107.4(3) . . ? C84 C36 C77 122.7(3) . . ? C52 C37 C49 113.2(3) . . ? C27 C38 C22 121.9(3) . . ? C75 C39 C77 119.5(3) . . ? C75 C39 C34 117.6(3) . . ? C77 C39 C34 122.9(3) . . ? C73 C40 C70 118.8(3) . . ? C73 C40 C23 123.4(3) . . ? C70 C40 C23 117.8(4) . . ? C65 C41 C49 119.1(3) . . ? C65 C41 C34 116.8(3) . . ? C49 C41 C34 124.1(3) . . ? C53 C42 C50 120.2(4) . . ? O12 C43 C72 112.4(3) . . ? O6 C44 C74 107.2(3) . . ? C63 C45 C74 115.1(3) . . ? O6 C46 C53 115.9(3) . . ? O6 C46 C56 125.0(3) . . ? C53 C46 C56 119.1(3) . . ? C55 C47 C57 120.5(4) . . ? N19 C48 C55 121.1(3) . . ? C41 C49 C82 118.6(3) . . ? C41 C49 C37 124.1(3) . . ? C82 C49 C37 117.3(3) . . ? C28 C50 C42 118.9(4) . . ? C28 C50 C21 121.5(3) . . ? C42 C50 C21 119.6(3) . . ? C82 C51 O13 124.7(3) . . ? C82 C51 C59 119.6(3) . . ? O13 C51 C59 115.7(3) . . ? C22 C52 C31 118.5(3) . . ? C22 C52 C37 123.3(3) . . ? C31 C52 C37 118.2(3) . . ? C42 C53 O11 124.3(3) . . ? C42 C53 C46 120.7(3) . . ? O11 C53 C46 115.0(3) . . ? C24 C55 C47 118.9(3) . . ? C24 C55 C48 121.2(3) . . ? C47 C55 C48 119.9(3) . . ? C28 C56 C46 119.8(4) . . ? C33 C57 C47 120.5(4) . . ? C30 C58 C32 120.1(3) . . ? C30 C58 O14 119.7(4) . . ? C32 C58 O14 120.1(3) . . ? O8 C59 C65 125.2(3) . . ? O8 C59 C51 115.9(3) . . ? C65 C59 C51 118.8(3) . . ? C85 C60 C86 119.9(4) . . ? C35 C62 C29 112.3(3) . . ? O8 C63 C45 107.1(3) . . ? C77 C64 C22 111.0(3) . . ? C59 C65 C41 122.1(4) . . ? O16 C66 C24 125.1(3) . . ? O16 C66 C33 114.7(3) . . ? C24 C66 C33 120.1(3) . . ? O14 C69 C76 112.6(3) . . ? C32 C70 C40 121.1(4) . . ? O5 C71 C84 117.4(3) . . ? O5 C71 C75 124.5(3) . . ? C84 C71 C75 118.1(4) . . ? C43 C72 C76 114.5(3) . . ? C40 C73 C30 119.9(4) . . ? C44 C74 C45 111.9(3) . . ? C39 C75 C71 121.8(4) . . ? C69 C76 C72 112.0(3) . . ? C39 C77 C36 117.9(3) . . ? C39 C77 C64 124.1(3) . . ? C36 C77 C64 118.0(3) . . ? C97 C80 C96 124.0(17) . . ? C51 C82 C49 121.8(4) . . ? C88 C83 C92 124.1(5) . . ? C36 C84 O12 122.3(3) . . ? C36 C84 C71 119.8(3) . . ? O12 C84 C71 117.8(3) . . ? C60 C85 C91 121.1(5) . . ? C60 C85 C88 118.6(4) . . ? C91 C85 C88 120.2(5) . . ? C92 C86 C60 122.9(5) . . ? C83 C88 C85 118.0(5) . . ? C86 C92 C83 116.4(5) . . ? C95 C93 C89 132.0(9) . . ? C95 C93 C94 112.8(7) . . ? C89 C93 C94 115.2(8) . . ? C96 C94 C93 114.3(8) . . ? C97 C95 C93 141.4(17) . . ? C80 C96 C94 121.5(12) . . ? C95 C97 C80 106(2) . . ? _diffrn_measured_fraction_theta_max 0.838 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.838 _refine_diff_density_max 0.685 _refine_diff_density_min -0.606 _refine_diff_density_rms 0.069