data_06019 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55.50 H88 N2 P2' _chemical_formula_weight 845.22 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' 'P' 'P' 0.1023 0.0942 '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' _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 34.147(3) _cell_length_b 9.3537(7) _cell_length_c 33.687(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.516(2) _cell_angle_gamma 90.00 _cell_volume 10739.4(16) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description iregblok _exptl_crystal_colour colourless _exptl_crystal_size_min 0.280 _exptl_crystal_size_mid 0.330 _exptl_crystal_size_max 0.480 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.046 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3720 _exptl_absorpt_coefficient_mu 0.116 _exptl_absorpt_correction_type none _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 'Bruker P4' _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 51634 _diffrn_reflns_av_R_equivalents 0.1204 _diffrn_reflns_av_sigmaI/netI 0.1159 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 28.29 _reflns_number_total 13317 _reflns_number_gt 6679 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 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^)+(0.1218P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13317 _refine_ls_number_parameters 562 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1334 _refine_ls_R_factor_gt 0.0707 _refine_ls_wR_factor_ref 0.2176 _refine_ls_wR_factor_gt 0.1846 _refine_ls_goodness_of_fit_ref 0.884 _refine_ls_restrained_S_all 0.886 _refine_ls_shift/su_max 0.300 _refine_ls_shift/su_mean 0.009 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 P1 P 0.32684(2) 0.06208(8) -0.01065(2) 0.0408(2) Uani 1 1 d . . . P2 P 0.323706(18) 0.04662(7) 0.147298(18) 0.03046(17) Uani 1 1 d . . . C1 C 0.33595(7) 0.1576(3) 0.03002(7) 0.0376(6) Uani 1 1 d . . . H1A H 0.3547 0.2295 0.0292 0.045 Uiso 1 1 calc R . . C2 C 0.31643(7) 0.1377(3) 0.06802(7) 0.0402(6) Uani 1 1 d . . . H2A H 0.2965 0.0642 0.0647 0.048 Uiso 1 1 calc R . . H2B H 0.3038 0.2260 0.0752 0.048 Uiso 1 1 calc R . . C3 C 0.34703(7) 0.0940(3) 0.10119(7) 0.0370(6) Uani 1 1 d . . . H3A H 0.3652 0.1724 0.1065 0.044 Uiso 1 1 calc R . . H3B H 0.3619 0.0128 0.0924 0.044 Uiso 1 1 calc R . . C4 C 0.32646(8) -0.1520(3) 0.15110(8) 0.0406(6) Uani 1 1 d . . . H4A H 0.3536 -0.1849 0.1554 0.049 Uiso 1 1 calc R . . C5 C 0.30139(9) -0.2007(3) 0.18459(9) 0.0547(8) Uani 1 1 d . . . H5A H 0.2999 -0.1265 0.2045 0.066 Uiso 1 1 calc R . . H5B H 0.3122 -0.2864 0.1972 0.066 Uiso 1 1 calc R . . C6 C 0.26099(9) -0.2304(3) 0.16428(9) 0.0525(8) Uani 1 1 d . . . H6A H 0.2484 -0.3106 0.1765 0.063 Uiso 1 1 calc R . . H6B H 0.2441 -0.1472 0.1651 0.063 Uiso 1 1 calc R . . N7 N 0.27019(7) -0.2634(2) 0.12398(7) 0.0492(6) Uani 1 1 d . A . C8 C 0.30648(8) -0.2194(3) 0.11468(9) 0.0447(7) Uani 1 1 d . A . C9 C 0.24252(10) -0.3229(4) 0.09385(11) 0.0628(9) Uani 1 1 d D . . C10 C 0.25587(18) -0.2850(8) 0.05507(18) 0.0526(11) Uiso 0.468(4) 1 d PD A 1 H10A H 0.2525 -0.1834 0.0503 0.063 Uiso 0.468(4) 1 calc PR A 1 H10B H 0.2410 -0.3368 0.0343 0.063 Uiso 0.468(4) 1 calc PR A 1 C11 C 0.29901(18) -0.3253(8) 0.0554(2) 0.0463(11) Uiso 0.468(4) 1 d PD A 1 H11A H 0.3025 -0.4232 0.0645 0.056 Uiso 0.468(4) 1 calc PR A 1 H11B H 0.3079 -0.3192 0.0287 0.056 Uiso 0.468(4) 1 calc PR A 1 C10' C 0.26875(17) -0.3871(6) 0.05979(16) 0.0526(11) Uiso 0.532(4) 1 d PD A 2 H10C H 0.2846 -0.4655 0.0706 0.063 Uiso 0.532(4) 1 calc PR A 2 H10D H 0.2517 -0.4240 0.0381 0.063 Uiso 0.532(4) 1 calc PR A 2 C11' C 0.29483(17) -0.2735(7) 0.04451(17) 0.0463(11) Uiso 0.532(4) 1 d PD A 2 H11C H 0.2796 -0.1923 0.0345 0.056 Uiso 0.532(4) 1 calc PR A 2 H11D H 0.3100 -0.3104 0.0234 0.056 Uiso 0.532(4) 1 calc PR A 2 N12 N 0.32212(7) -0.2306(3) 0.08139(9) 0.0685(8) Uani 1 1 d . . . C13 C 0.36440(7) 0.1345(3) -0.04244(7) 0.0318(5) Uani 1 1 d . . . C14 C 0.40209(7) 0.0674(3) -0.04215(7) 0.0323(5) Uani 1 1 d . . . C15 C 0.43234(7) 0.1401(3) -0.05856(7) 0.0346(6) Uani 1 1 d . . . H15A H 0.4569 0.0971 -0.0580 0.042 Uiso 1 1 calc R . . C16 C 0.42786(7) 0.2749(3) -0.07603(7) 0.0345(6) Uani 1 1 d . . . C17 C 0.39036(7) 0.3305(3) -0.07915(7) 0.0350(6) Uani 1 1 d . . . H17A H 0.3865 0.4176 -0.0921 0.042 Uiso 1 1 calc R . . C18 C 0.35807(7) 0.2640(3) -0.06406(7) 0.0325(6) Uani 1 1 d . . . C19 C 0.41147(8) -0.0845(3) -0.02446(8) 0.0418(6) Uani 1 1 d . . . C20 C 0.38127(10) -0.1953(3) -0.04014(10) 0.0616(9) Uani 1 1 d . . . H20A H 0.3885 -0.2880 -0.0298 0.092 Uiso 1 1 calc R . . H20B H 0.3806 -0.1974 -0.0687 0.092 Uiso 1 1 calc R . . H20C H 0.3558 -0.1700 -0.0317 0.092 Uiso 1 1 calc R . . C21 C 0.41409(10) -0.0839(3) 0.02105(9) 0.0612(9) Uani 1 1 d . . . H21A H 0.4253 -0.1725 0.0307 0.092 Uiso 1 1 calc R . . H21B H 0.3883 -0.0731 0.0305 0.092 Uiso 1 1 calc R . . H21C H 0.4304 -0.0059 0.0305 0.092 Uiso 1 1 calc R . . C22 C 0.45116(9) -0.1402(3) -0.03704(9) 0.0541(8) Uani 1 1 d . . . H22A H 0.4550 -0.2365 -0.0278 0.081 Uiso 1 1 calc R . . H22B H 0.4718 -0.0806 -0.0257 0.081 Uiso 1 1 calc R . . H22C H 0.4515 -0.1382 -0.0655 0.081 Uiso 1 1 calc R . . C23 C 0.46334(8) 0.3522(3) -0.09125(9) 0.0463(7) Uani 1 1 d . . . C24 C 0.49453(11) 0.3681(5) -0.05720(14) 0.1157(19) Uani 1 1 d . . . H24A H 0.5172 0.4143 -0.0667 0.173 Uiso 1 1 calc R . . H24B H 0.5017 0.2753 -0.0470 0.173 Uiso 1 1 calc R . . H24C H 0.4843 0.4247 -0.0364 0.173 Uiso 1 1 calc R . . C25 C 0.47914(13) 0.2696(4) -0.12479(15) 0.1121(18) Uani 1 1 d . . . H25A H 0.4600 0.2676 -0.1468 0.168 Uiso 1 1 calc R . . H25B H 0.4849 0.1736 -0.1162 0.168 Uiso 1 1 calc R . . H25C H 0.5027 0.3145 -0.1328 0.168 Uiso 1 1 calc R . . C26 C 0.45315(10) 0.5021(4) -0.10628(12) 0.0722(10) Uani 1 1 d . . . H26A H 0.4336 0.4962 -0.1279 0.108 Uiso 1 1 calc R . . H26B H 0.4763 0.5472 -0.1152 0.108 Uiso 1 1 calc R . . H26C H 0.4432 0.5574 -0.0851 0.108 Uiso 1 1 calc R . . C27 C 0.31723(7) 0.3338(3) -0.07275(8) 0.0401(6) Uani 1 1 d . . . C28 C 0.31799(9) 0.4426(3) -0.10719(9) 0.0572(8) Uani 1 1 d . . . H28A H 0.3276 0.3968 -0.1302 0.086 Uiso 1 1 calc R . . H28B H 0.3349 0.5210 -0.0993 0.086 Uiso 1 1 calc R . . H28C H 0.2919 0.4777 -0.1135 0.086 Uiso 1 1 calc R . . C29 C 0.28666(8) 0.2214(3) -0.08646(9) 0.0507(7) Uani 1 1 d . . . H29A H 0.2960 0.1687 -0.1085 0.076 Uiso 1 1 calc R . . H29B H 0.2624 0.2680 -0.0946 0.076 Uiso 1 1 calc R . . H29C H 0.2824 0.1571 -0.0649 0.076 Uiso 1 1 calc R . . C30 C 0.30371(9) 0.4189(3) -0.03703(9) 0.0542(8) Uani 1 1 d . . . H30A H 0.3241 0.4839 -0.0279 0.081 Uiso 1 1 calc R . . H30B H 0.2982 0.3541 -0.0160 0.081 Uiso 1 1 calc R . . H30C H 0.2804 0.4718 -0.0449 0.081 Uiso 1 1 calc R . . C31 C 0.35401(7) 0.0932(2) 0.19354(7) 0.0289(5) Uani 1 1 d . . . C32 C 0.38747(7) 0.0156(3) 0.20996(7) 0.0347(6) Uani 1 1 d . . . C33 C 0.39265(8) 0.0083(3) 0.25102(8) 0.0449(7) Uani 1 1 d . . . H33A H 0.4136 -0.0457 0.2617 0.054 Uiso 1 1 calc R . . C34 C 0.36918(8) 0.0746(3) 0.27707(8) 0.0507(8) Uani 1 1 d . . . C35 C 0.34115(8) 0.1673(3) 0.26023(7) 0.0439(7) Uani 1 1 d . . . H35A H 0.3269 0.2227 0.2771 0.053 Uiso 1 1 calc R . . C36 C 0.33329(7) 0.1818(2) 0.21981(7) 0.0313(5) Uani 1 1 d . . . C37 C 0.42163(8) -0.0562(3) 0.18819(8) 0.0465(7) Uani 1 1 d . . . C38 C 0.42093(8) -0.0428(3) 0.14351(8) 0.0548(8) Uani 1 1 d . . . H38A H 0.4163 0.0551 0.1360 0.082 Uiso 1 1 calc R . . H38B H 0.4003 -0.1016 0.1317 0.082 Uiso 1 1 calc R . . H38C H 0.4457 -0.0734 0.1344 0.082 Uiso 1 1 calc R . . C39 C 0.42511(11) -0.2151(3) 0.19891(11) 0.0722(10) Uani 1 1 d . . . H39A H 0.4463 -0.2568 0.1855 0.108 Uiso 1 1 calc R . . H39B H 0.4011 -0.2630 0.1908 0.108 Uiso 1 1 calc R . . H39C H 0.4301 -0.2250 0.2271 0.108 Uiso 1 1 calc R . . C40 C 0.46003(8) 0.0177(4) 0.20398(10) 0.0665(9) Uani 1 1 d . . . H40A H 0.4587 0.1178 0.1979 0.100 Uiso 1 1 calc R . . H40B H 0.4819 -0.0243 0.1916 0.100 Uiso 1 1 calc R . . H40C H 0.4634 0.0052 0.2323 0.100 Uiso 1 1 calc R . . C41 C 0.37473(10) 0.0427(5) 0.32178(9) 0.0834(14) Uani 1 1 d . . . C42 C 0.36951(14) -0.1241(6) 0.32774(14) 0.133(2) Uani 1 1 d . . . H42A H 0.3435 -0.1518 0.3184 0.200 Uiso 1 1 calc R . . H42B H 0.3736 -0.1471 0.3555 0.200 Uiso 1 1 calc R . . H42C H 0.3883 -0.1745 0.3129 0.200 Uiso 1 1 calc R . . C43 C 0.41634(11) 0.0809(5) 0.33694(10) 0.0923(14) Uani 1 1 d . . . H43A H 0.4204 0.1817 0.3339 0.138 Uiso 1 1 calc R . . H43B H 0.4347 0.0292 0.3220 0.138 Uiso 1 1 calc R . . H43C H 0.4201 0.0558 0.3645 0.138 Uiso 1 1 calc R . . C44 C 0.34419(16) 0.1073(9) 0.34454(11) 0.174(3) Uani 1 1 d . . . H44A H 0.3478 0.2091 0.3455 0.261 Uiso 1 1 calc R . . H44B H 0.3458 0.0695 0.3711 0.261 Uiso 1 1 calc R . . H44C H 0.3189 0.0858 0.3320 0.261 Uiso 1 1 calc R . . C45 C 0.30219(8) 0.2954(3) 0.20617(7) 0.0383(6) Uani 1 1 d . . . C46 C 0.30147(11) 0.4167(3) 0.23739(9) 0.0649(10) Uani 1 1 d . . . H46A H 0.3276 0.4517 0.2431 0.097 Uiso 1 1 calc R . . H46B H 0.2912 0.3804 0.2613 0.097 Uiso 1 1 calc R . . H46C H 0.2851 0.4931 0.2271 0.097 Uiso 1 1 calc R . . C47 C 0.26062(8) 0.2307(3) 0.20251(9) 0.0549(8) Uani 1 1 d . . . H47A H 0.2592 0.1606 0.1817 0.082 Uiso 1 1 calc R . . H47B H 0.2418 0.3050 0.1964 0.082 Uiso 1 1 calc R . . H47C H 0.2550 0.1862 0.2272 0.082 Uiso 1 1 calc R . . C48 C 0.31197(9) 0.3689(3) 0.16738(8) 0.0481(7) Uani 1 1 d . . . H48A H 0.3380 0.4079 0.1703 0.072 Uiso 1 1 calc R . . H48B H 0.2935 0.4445 0.1614 0.072 Uiso 1 1 calc R . . H48C H 0.3105 0.3005 0.1461 0.072 Uiso 1 1 calc R . . C50 C 0.4318(2) 0.3901(8) 0.1499(3) 0.198(3) Uani 1 1 d . . . H50A H 0.4266 0.4804 0.1620 0.297 Uiso 1 1 calc R . . H50B H 0.4584 0.3623 0.1568 0.297 Uiso 1 1 calc R . . H50C H 0.4143 0.3190 0.1592 0.297 Uiso 1 1 calc R . . C51 C 0.42634(13) 0.4022(5) 0.10970(12) 0.0806(13) Uani 1 1 d . . . C52 C 0.44574(10) 0.3108(4) 0.08333(15) 0.0731(11) Uani 1 1 d . . . H52A H 0.4630 0.2402 0.0929 0.088 Uiso 1 1 calc R . . C53 C 0.43797(13) 0.3311(5) 0.04379(14) 0.0797(11) Uani 1 1 d . . . H53A H 0.4497 0.2712 0.0260 0.096 Uiso 1 1 calc R . . C54 C 0.41387(14) 0.4346(5) 0.02953(15) 0.0894(13) Uani 1 1 d . . . H54A H 0.4102 0.4489 0.0022 0.107 Uiso 1 1 calc R . . C55 C 0.39528(12) 0.5167(5) 0.05456(16) 0.0845(12) Uani 1 1 d . . . H55A H 0.3779 0.5855 0.0441 0.101 Uiso 1 1 calc R . . C56 C 0.40055(11) 0.5048(4) 0.09383(15) 0.0745(11) Uani 1 1 d . . . H56A H 0.3871 0.5643 0.1104 0.089 Uiso 1 1 calc R . . C57 C 0.0635(4) 0.9517(10) 0.2286(3) 0.239(6) Uani 1 1 d . . . H57A H 0.0710 0.8853 0.2087 0.358 Uiso 1 1 calc R . . H57B H 0.0839 0.9570 0.2495 0.358 Uiso 1 1 calc R . . H57C H 0.0595 1.0445 0.2169 0.358 Uiso 1 1 calc R . . C58 C 0.0284(9) 0.905(2) 0.2446(7) 0.52(3) Uani 1 1 d . . . H58A H 0.0197 0.8249 0.2280 0.627 Uiso 1 1 calc R . . H58B H 0.0366 0.8643 0.2702 0.627 Uiso 1 1 calc R . . C59 C 0.0000 0.968(3) 0.2500 0.33(2) Uani 1 2 d S . . H9 H 0.2269(14) -0.408(5) 0.1004(14) 0.130(16) Uiso 1 1 d . . . H9' H 0.2161(10) -0.267(4) 0.0891(9) 0.072(10) Uiso 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 P1 0.0349(4) 0.0561(5) 0.0313(4) -0.0031(3) 0.0011(3) -0.0123(3) P2 0.0302(3) 0.0316(3) 0.0293(3) -0.0024(3) -0.0004(3) -0.0014(3) C1 0.0300(13) 0.0504(16) 0.0322(13) -0.0005(11) 0.0009(11) -0.0029(11) C2 0.0318(14) 0.0562(18) 0.0325(14) -0.0034(12) 0.0023(11) -0.0035(12) C3 0.0306(13) 0.0492(16) 0.0312(13) -0.0052(11) 0.0028(10) -0.0036(11) C4 0.0413(15) 0.0300(13) 0.0497(16) -0.0062(12) -0.0037(12) -0.0015(11) C5 0.075(2) 0.0333(15) 0.0536(18) 0.0092(13) -0.0118(16) -0.0119(14) C6 0.0596(19) 0.0440(17) 0.0545(18) 0.0078(14) 0.0075(15) -0.0126(14) N7 0.0463(14) 0.0449(14) 0.0559(15) -0.0098(11) -0.0012(11) -0.0140(11) C8 0.0366(15) 0.0348(15) 0.0624(19) -0.0145(13) 0.0006(14) -0.0019(12) C9 0.053(2) 0.063(2) 0.070(2) -0.0046(17) -0.0116(17) -0.0262(18) N12 0.0476(15) 0.082(2) 0.0772(19) -0.0522(16) 0.0104(14) -0.0133(14) C13 0.0311(13) 0.0379(14) 0.0260(12) -0.0058(10) -0.0010(10) -0.0071(10) C14 0.0344(13) 0.0342(14) 0.0276(12) -0.0055(10) -0.0042(10) -0.0006(11) C15 0.0277(13) 0.0364(14) 0.0394(14) -0.0051(11) -0.0007(11) 0.0014(11) C16 0.0289(13) 0.0378(14) 0.0366(14) -0.0050(11) 0.0015(10) -0.0039(11) C17 0.0341(14) 0.0335(14) 0.0370(14) -0.0020(11) -0.0014(11) 0.0003(11) C18 0.0283(13) 0.0386(14) 0.0303(13) -0.0106(11) -0.0014(10) -0.0020(10) C19 0.0470(16) 0.0393(15) 0.0385(15) 0.0013(12) -0.0036(12) 0.0016(12) C20 0.070(2) 0.0390(17) 0.074(2) 0.0003(15) -0.0080(17) -0.0061(15) C21 0.076(2) 0.064(2) 0.0428(17) 0.0090(15) -0.0036(16) 0.0170(17) C22 0.0600(19) 0.0432(17) 0.0592(19) 0.0011(14) 0.0033(15) 0.0124(14) C23 0.0311(14) 0.0460(16) 0.0625(19) 0.0051(14) 0.0095(13) -0.0055(12) C24 0.063(2) 0.147(4) 0.132(4) 0.070(3) -0.036(2) -0.061(3) C25 0.106(3) 0.082(3) 0.160(4) -0.024(3) 0.101(3) -0.022(2) C26 0.061(2) 0.0544(19) 0.103(3) 0.018(2) 0.022(2) -0.0063(17) C27 0.0294(13) 0.0463(16) 0.0440(15) -0.0053(12) -0.0034(11) 0.0023(11) C28 0.0427(17) 0.064(2) 0.064(2) 0.0096(16) -0.0059(15) 0.0122(15) C29 0.0312(14) 0.0604(19) 0.0589(18) -0.0090(14) -0.0105(13) 0.0005(13) C30 0.0460(17) 0.0597(19) 0.0565(19) -0.0116(15) -0.0005(14) 0.0167(14) C31 0.0312(13) 0.0278(12) 0.0275(12) 0.0006(10) 0.0013(10) -0.0033(10) C32 0.0309(13) 0.0358(14) 0.0370(14) -0.0009(11) -0.0001(11) 0.0026(10) C33 0.0369(15) 0.0546(17) 0.0422(16) 0.0109(13) -0.0040(12) 0.0099(13) C34 0.0423(16) 0.080(2) 0.0296(14) 0.0075(14) 0.0016(12) 0.0143(15) C35 0.0454(16) 0.0592(18) 0.0277(13) -0.0032(12) 0.0069(12) 0.0095(13) C36 0.0336(13) 0.0314(13) 0.0289(12) 0.0013(10) 0.0024(10) -0.0001(10) C37 0.0365(15) 0.0551(18) 0.0475(16) -0.0043(13) -0.0018(12) 0.0117(13) C38 0.0349(15) 0.079(2) 0.0502(18) -0.0087(15) 0.0040(13) 0.0210(15) C39 0.077(2) 0.058(2) 0.081(2) 0.0015(18) -0.0033(19) 0.0324(18) C40 0.0331(16) 0.112(3) 0.0540(19) -0.0078(19) -0.0026(14) 0.0069(17) C41 0.061(2) 0.156(4) 0.0329(17) 0.017(2) 0.0002(16) 0.043(2) C42 0.116(4) 0.194(6) 0.088(3) 0.093(4) -0.006(3) -0.013(4) C43 0.089(3) 0.144(4) 0.0410(19) -0.004(2) -0.0177(19) 0.023(3) C44 0.117(4) 0.376(10) 0.030(2) 0.028(4) 0.014(2) 0.106(5) C45 0.0498(16) 0.0316(14) 0.0342(14) 0.0018(11) 0.0081(12) 0.0125(12) C46 0.102(3) 0.0463(18) 0.0473(18) -0.0049(14) 0.0135(18) 0.0229(18) C47 0.0432(17) 0.063(2) 0.0594(19) 0.0126(15) 0.0099(14) 0.0201(15) C48 0.073(2) 0.0318(14) 0.0400(15) 0.0049(12) 0.0067(14) 0.0097(14) C50 0.202(8) 0.151(6) 0.238(10) 0.004(6) -0.012(7) -0.072(6) C51 0.090(3) 0.100(3) 0.051(2) 0.003(2) 0.002(2) -0.051(3) C52 0.048(2) 0.054(2) 0.117(4) 0.003(2) 0.013(2) -0.0156(16) C53 0.081(3) 0.070(3) 0.089(3) -0.020(2) 0.016(2) -0.032(2) C54 0.074(3) 0.099(4) 0.094(3) -0.009(3) -0.007(3) -0.039(3) C55 0.061(2) 0.085(3) 0.107(4) 0.017(3) -0.002(3) -0.029(2) C56 0.066(2) 0.053(2) 0.107(3) -0.006(2) 0.017(2) -0.0088(18) C57 0.40(2) 0.170(9) 0.143(7) -0.034(6) -0.005(9) 0.088(10) C58 0.78(7) 0.31(2) 0.50(3) 0.20(2) 0.18(4) -0.10(3) C59 0.44(5) 0.30(3) 0.22(2) 0.000 -0.21(3) 0.000 _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 P1 C1 1.650(3) . ? P1 C13 1.849(2) . ? P2 C3 1.843(2) . ? P2 C4 1.864(3) . ? P2 C31 1.868(2) . ? C1 C2 1.491(3) . ? C2 C3 1.538(3) . ? C4 C8 1.505(4) . ? C4 C5 1.527(4) . ? C5 C6 1.528(4) . ? C6 N7 1.446(4) . ? N7 C8 1.361(3) . ? N7 C9 1.454(4) . ? C8 N12 1.276(4) . ? C9 C10 1.454(7) . ? C9 C10' 1.614(6) . ? C10 C11 1.520(8) . ? C11 N12 1.445(7) . ? C10' C11' 1.497(7) . ? C11' N12 1.559(6) . ? C13 C18 1.423(3) . ? C13 C14 1.432(3) . ? C14 C15 1.380(3) . ? C14 C19 1.566(3) . ? C15 C16 1.396(3) . ? C16 C17 1.380(3) . ? C16 C23 1.526(4) . ? C17 C18 1.389(3) . ? C18 C27 1.551(3) . ? C19 C21 1.530(4) . ? C19 C20 1.533(4) . ? C19 C22 1.535(4) . ? C23 C25 1.497(5) . ? C23 C26 1.524(4) . ? C23 C24 1.524(5) . ? C27 C29 1.533(4) . ? C27 C30 1.537(4) . ? C27 C28 1.545(4) . ? C31 C36 1.431(3) . ? C31 C32 1.435(3) . ? C32 C33 1.385(3) . ? C32 C37 1.567(4) . ? C33 C34 1.372(4) . ? C34 C35 1.387(4) . ? C34 C41 1.536(4) . ? C35 C36 1.378(3) . ? C36 C45 1.552(3) . ? C37 C38 1.509(4) . ? C37 C39 1.533(4) . ? C37 C40 1.547(4) . ? C41 C44 1.463(6) . ? C41 C43 1.523(5) . ? C41 C42 1.584(7) . ? C45 C48 1.532(4) . ? C45 C47 1.541(4) . ? C45 C46 1.548(4) . ? C50 C51 1.360(8) . ? C51 C56 1.387(6) . ? C51 C52 1.425(6) . ? C52 C53 1.355(6) . ? C53 C54 1.340(6) . ? C54 C55 1.331(6) . ? C55 C56 1.329(6) . ? C57 C58 1.41(3) . ? C58 C59 1.16(4) . ? C59 C58 1.16(4) 2 ? 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 C1 P1 C13 100.39(12) . . ? C3 P2 C4 105.96(12) . . ? C3 P2 C31 113.65(11) . . ? C4 P2 C31 98.74(11) . . ? C2 C1 P1 125.0(2) . . ? C1 C2 C3 109.7(2) . . ? C2 C3 P2 111.53(17) . . ? C8 C4 C5 103.3(2) . . ? C8 C4 P2 110.05(18) . . ? C5 C4 P2 108.66(19) . . ? C4 C5 C6 104.8(2) . . ? N7 C6 C5 102.5(2) . . ? C8 N7 C6 113.9(2) . . ? C8 N7 C9 121.1(3) . . ? C6 N7 C9 124.6(2) . . ? N12 C8 N7 127.9(3) . . ? N12 C8 C4 123.9(2) . . ? N7 C8 C4 108.2(3) . . ? C10 C9 N7 107.9(3) . . ? C10 C9 C10' 40.0(3) . . ? N7 C9 C10' 105.9(3) . . ? C9 C10 C11 106.8(5) . . ? N12 C11 C10 110.2(5) . . ? C11' C10' C9 110.4(4) . . ? C10' C11' N12 104.3(4) . . ? C8 N12 C11 109.9(3) . . ? C8 N12 C11' 117.4(3) . . ? C11 N12 C11' 23.4(3) . . ? C18 C13 C14 119.0(2) . . ? C18 C13 P1 121.29(18) . . ? C14 C13 P1 119.37(18) . . ? C15 C14 C13 118.4(2) . . ? C15 C14 C19 117.3(2) . . ? C13 C14 C19 124.3(2) . . ? C14 C15 C16 123.3(2) . . ? C17 C16 C15 116.7(2) . . ? C17 C16 C23 123.2(2) . . ? C15 C16 C23 120.1(2) . . ? C16 C17 C18 123.8(2) . . ? C17 C18 C13 118.0(2) . . ? C17 C18 C27 117.8(2) . . ? C13 C18 C27 124.1(2) . . ? C21 C19 C20 110.2(3) . . ? C21 C19 C22 106.2(2) . . ? C20 C19 C22 105.2(2) . . ? C21 C19 C14 112.1(2) . . ? C20 C19 C14 111.4(2) . . ? C22 C19 C14 111.5(2) . . ? C25 C23 C26 108.1(3) . . ? C25 C23 C24 110.5(4) . . ? C26 C23 C24 107.2(3) . . ? C25 C23 C16 109.8(2) . . ? C26 C23 C16 112.2(2) . . ? C24 C23 C16 109.0(2) . . ? C29 C27 C30 111.0(2) . . ? C29 C27 C28 105.6(2) . . ? C30 C27 C28 105.5(2) . . ? C29 C27 C18 110.9(2) . . ? C30 C27 C18 112.3(2) . . ? C28 C27 C18 111.3(2) . . ? C36 C31 C32 117.8(2) . . ? C36 C31 P2 112.41(16) . . ? C32 C31 P2 126.22(17) . . ? C33 C32 C31 117.4(2) . . ? C33 C32 C37 113.1(2) . . ? C31 C32 C37 129.3(2) . . ? C34 C33 C32 124.9(2) . . ? C33 C34 C35 115.9(2) . . ? C33 C34 C41 119.8(3) . . ? C35 C34 C41 124.3(3) . . ? C36 C35 C34 123.6(2) . . ? C35 C36 C31 118.7(2) . . ? C35 C36 C45 116.6(2) . . ? C31 C36 C45 124.7(2) . . ? C38 C37 C39 108.2(2) . . ? C38 C37 C40 105.5(2) . . ? C39 C37 C40 107.5(3) . . ? C38 C37 C32 117.7(2) . . ? C39 C37 C32 110.8(3) . . ? C40 C37 C32 106.7(2) . . ? C44 C41 C43 114.1(4) . . ? C44 C41 C34 112.6(3) . . ? C43 C41 C34 109.9(3) . . ? C44 C41 C42 104.6(4) . . ? C43 C41 C42 107.4(3) . . ? C34 C41 C42 107.9(3) . . ? C48 C45 C47 110.9(2) . . ? C48 C45 C46 105.3(2) . . ? C47 C45 C46 106.8(2) . . ? C48 C45 C36 112.3(2) . . ? C47 C45 C36 111.4(2) . . ? C46 C45 C36 109.9(2) . . ? C50 C51 C56 119.1(6) . . ? C50 C51 C52 122.0(6) . . ? C56 C51 C52 118.9(4) . . ? C53 C52 C51 117.3(4) . . ? C54 C53 C52 122.1(4) . . ? C55 C54 C53 119.8(5) . . ? C54 C55 C56 122.8(5) . . ? C55 C56 C51 119.1(4) . . ? C59 C58 C57 130(2) . . ? C58 C59 C58 119(4) 2 . ? 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 C13 P1 C1 C2 -174.8(2) . . . . ? P1 C1 C2 C3 117.1(2) . . . . ? C1 C2 C3 P2 -173.08(18) . . . . ? C4 P2 C3 C2 105.8(2) . . . . ? C31 P2 C3 C2 -146.90(18) . . . . ? C3 P2 C4 C8 -57.7(2) . . . . ? C31 P2 C4 C8 -175.44(19) . . . . ? C3 P2 C4 C5 -170.15(17) . . . . ? C31 P2 C4 C5 72.07(19) . . . . ? C8 C4 C5 C6 -25.1(3) . . . . ? P2 C4 C5 C6 91.8(2) . . . . ? C4 C5 C6 N7 25.8(3) . . . . ? C5 C6 N7 C8 -17.6(3) . . . . ? C5 C6 N7 C9 169.2(3) . . . . ? C6 N7 C8 N12 -178.2(3) . . . . ? C9 N7 C8 N12 -4.8(5) . . . . ? C6 N7 C8 C4 1.7(3) . . . . ? C9 N7 C8 C4 175.1(3) . . . . ? C5 C4 C8 N12 -165.0(3) . . . . ? P2 C4 C8 N12 79.1(3) . . . . ? C5 C4 C8 N7 15.1(3) . . . . ? P2 C4 C8 N7 -100.8(2) . . . . ? C8 N7 C9 C10 -16.7(5) . . . . ? C6 N7 C9 C10 156.0(4) . . . . ? C8 N7 C9 C10' 25.1(4) . . . . ? C6 N7 C9 C10' -162.2(3) . . . . ? N7 C9 C10 C11 49.8(6) . . . . ? C10' C9 C10 C11 -43.7(5) . . . . ? C9 C10 C11 N12 -70.2(7) . . . . ? C10 C9 C10' C11' 42.9(5) . . . . ? N7 C9 C10' C11' -56.2(5) . . . . ? C9 C10' C11' N12 62.6(5) . . . . ? N7 C8 N12 C11 -12.0(5) . . . . ? C4 C8 N12 C11 168.2(4) . . . . ? N7 C8 N12 C11' 12.3(5) . . . . ? C4 C8 N12 C11' -167.6(3) . . . . ? C10 C11 N12 C8 48.1(6) . . . . ? C10 C11 N12 C11' -65.1(9) . . . . ? C10' C11' N12 C8 -41.2(6) . . . . ? C10' C11' N12 C11 35.4(8) . . . . ? C1 P1 C13 C18 -82.1(2) . . . . ? C1 P1 C13 C14 91.3(2) . . . . ? C18 C13 C14 C15 8.2(3) . . . . ? P1 C13 C14 C15 -165.44(18) . . . . ? C18 C13 C14 C19 -171.6(2) . . . . ? P1 C13 C14 C19 14.8(3) . . . . ? C13 C14 C15 C16 -1.1(3) . . . . ? C19 C14 C15 C16 178.7(2) . . . . ? C14 C15 C16 C17 -4.9(4) . . . . ? C14 C15 C16 C23 176.2(2) . . . . ? C15 C16 C17 C18 3.8(4) . . . . ? C23 C16 C17 C18 -177.4(2) . . . . ? C16 C17 C18 C13 3.2(4) . . . . ? C16 C17 C18 C27 -175.3(2) . . . . ? C14 C13 C18 C17 -9.2(3) . . . . ? P1 C13 C18 C17 164.32(18) . . . . ? C14 C13 C18 C27 169.2(2) . . . . ? P1 C13 C18 C27 -17.3(3) . . . . ? C15 C14 C19 C21 106.1(3) . . . . ? C13 C14 C19 C21 -74.2(3) . . . . ? C15 C14 C19 C20 -130.0(3) . . . . ? C13 C14 C19 C20 49.8(3) . . . . ? C15 C14 C19 C22 -12.8(3) . . . . ? C13 C14 C19 C22 166.9(2) . . . . ? C17 C16 C23 C25 -114.6(3) . . . . ? C15 C16 C23 C25 64.2(4) . . . . ? C17 C16 C23 C26 5.7(4) . . . . ? C15 C16 C23 C26 -175.5(3) . . . . ? C17 C16 C23 C24 124.2(3) . . . . ? C15 C16 C23 C24 -57.0(4) . . . . ? C17 C18 C27 C29 133.8(2) . . . . ? C13 C18 C27 C29 -44.6(3) . . . . ? C17 C18 C27 C30 -101.3(3) . . . . ? C13 C18 C27 C30 80.2(3) . . . . ? C17 C18 C27 C28 16.6(3) . . . . ? C13 C18 C27 C28 -161.8(2) . . . . ? C3 P2 C31 C36 124.91(18) . . . . ? C4 P2 C31 C36 -123.31(18) . . . . ? C3 P2 C31 C32 -77.1(2) . . . . ? C4 P2 C31 C32 34.7(2) . . . . ? C36 C31 C32 C33 13.0(3) . . . . ? P2 C31 C32 C33 -144.0(2) . . . . ? C36 C31 C32 C37 -162.6(2) . . . . ? P2 C31 C32 C37 40.4(4) . . . . ? C31 C32 C33 C34 -3.0(4) . . . . ? C37 C32 C33 C34 173.3(3) . . . . ? C32 C33 C34 C35 -7.3(5) . . . . ? C32 C33 C34 C41 172.1(3) . . . . ? C33 C34 C35 C36 7.6(4) . . . . ? C41 C34 C35 C36 -171.8(3) . . . . ? C34 C35 C36 C31 2.4(4) . . . . ? C34 C35 C36 C45 -177.5(3) . . . . ? C32 C31 C36 C35 -12.8(3) . . . . ? P2 C31 C36 C35 147.3(2) . . . . ? C32 C31 C36 C45 167.0(2) . . . . ? P2 C31 C36 C45 -32.9(3) . . . . ? C33 C32 C37 C38 -174.6(3) . . . . ? C31 C32 C37 C38 1.1(4) . . . . ? C33 C32 C37 C39 60.3(3) . . . . ? C31 C32 C37 C39 -124.0(3) . . . . ? C33 C32 C37 C40 -56.4(3) . . . . ? C31 C32 C37 C40 119.3(3) . . . . ? C33 C34 C41 C44 -172.5(5) . . . . ? C35 C34 C41 C44 6.9(6) . . . . ? C33 C34 C41 C43 59.2(5) . . . . ? C35 C34 C41 C43 -121.4(4) . . . . ? C33 C34 C41 C42 -57.6(4) . . . . ? C35 C34 C41 C42 121.8(4) . . . . ? C35 C36 C45 C48 145.0(2) . . . . ? C31 C36 C45 C48 -34.8(3) . . . . ? C35 C36 C45 C47 -90.0(3) . . . . ? C31 C36 C45 C47 90.2(3) . . . . ? C35 C36 C45 C46 28.2(3) . . . . ? C31 C36 C45 C46 -151.6(2) . . . . ? C50 C51 C52 C53 179.4(4) . . . . ? C56 C51 C52 C53 0.6(5) . . . . ? C51 C52 C53 C54 1.7(5) . . . . ? C52 C53 C54 C55 -3.3(6) . . . . ? C53 C54 C55 C56 2.6(6) . . . . ? C54 C55 C56 C51 -0.3(6) . . . . ? C50 C51 C56 C55 179.9(4) . . . . ? C52 C51 C56 C55 -1.3(5) . . . . ? C57 C58 C59 C58 164(4) . . . 2 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.731 _refine_diff_density_min -0.405 _refine_diff_density_rms 0.067 #===END data_06006 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H32 P2' _chemical_formula_weight 346.41 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' 'P' 'P' 0.1023 0.0942 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.087(5) _cell_length_b 6.235(2) _cell_length_c 22.974(8) _cell_angle_alpha 90.00 _cell_angle_beta 91.509(6) _cell_angle_gamma 90.00 _cell_volume 2017.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description wedge _exptl_crystal_colour colourless _exptl_crystal_size_min 0.120 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_max 0.360 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.141 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 0.214 _exptl_absorpt_correction_type none _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 'Bruker P4' _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 6429 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 27.54 _reflns_number_total 6439 _reflns_number_gt 4940 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 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^)+(0.1989P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6439 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1082 _refine_ls_R_factor_gt 0.0882 _refine_ls_wR_factor_ref 0.2773 _refine_ls_wR_factor_gt 0.2555 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 P1 P 0.28043(7) 0.67016(15) 0.20867(4) 0.0268(3) Uani 1 1 d . . . C1 C 0.2360(3) 0.9060(8) 0.3014(2) 0.0461(12) Uani 1 1 d . . . H1 H 0.231(3) 0.974(7) 0.3375(18) 0.030(10) Uiso 1 1 d . . . P2 P 0.23446(8) 0.63002(19) 0.29305(5) 0.0409(3) Uani 1 1 d . . . C2 C 0.2555(3) 1.0381(7) 0.2532(2) 0.0460(12) Uani 1 1 d . . . H2 H 0.257(3) 1.194(10) 0.255(2) 0.073(18) Uiso 1 1 d . . . C3 C 0.2724(3) 0.9449(6) 0.2015(2) 0.0398(10) Uani 1 1 d . . . H3 H 0.289(3) 1.018(7) 0.165(2) 0.041(12) Uiso 1 1 d . . . C4 C 0.2653(2) 0.4972(5) 0.14510(15) 0.0221(7) Uani 1 1 d . . . C5 C 0.3494(2) 0.4170(6) 0.11894(15) 0.0225(7) Uani 1 1 d . . . C6 C 0.3381(2) 0.2846(5) 0.07118(16) 0.0244(8) Uani 1 1 d . . . H6A H 0.3925 0.2327 0.0539 0.029 Uiso 1 1 calc R . . C7 C 0.2499(2) 0.2235(5) 0.04712(14) 0.0215(7) Uani 1 1 d . . . C8 C 0.1709(2) 0.3031(6) 0.07392(17) 0.0265(8) Uani 1 1 d . . . H8A H 0.1115 0.2614 0.0593 0.032 Uiso 1 1 calc R . . C9 C 0.1741(2) 0.4407(6) 0.12106(16) 0.0232(8) Uani 1 1 d . . . C10 C 0.4527(2) 0.4610(6) 0.14143(17) 0.0254(8) Uani 1 1 d . . . C11 C 0.5265(3) 0.3513(7) 0.1032(2) 0.0366(10) Uani 1 1 d . . . H11A H 0.5892 0.3865 0.1175 0.055 Uiso 1 1 calc R . . H11B H 0.5185 0.4003 0.0638 0.055 Uiso 1 1 calc R . . H11C H 0.5177 0.1987 0.1046 0.055 Uiso 1 1 calc R . . C12 C 0.4708(3) 0.3683(6) 0.20320(18) 0.0332(9) Uani 1 1 d . . . H12A H 0.5361 0.3892 0.2146 0.050 Uiso 1 1 calc R . . H12B H 0.4565 0.2177 0.2031 0.050 Uiso 1 1 calc R . . H12C H 0.4308 0.4403 0.2302 0.050 Uiso 1 1 calc R . . C13 C 0.4779(3) 0.7023(6) 0.13952(19) 0.0323(9) Uani 1 1 d . . . H13A H 0.5427 0.7221 0.1524 0.048 Uiso 1 1 calc R . . H13B H 0.4368 0.7803 0.1646 0.048 Uiso 1 1 calc R . . H13C H 0.4699 0.7543 0.1004 0.048 Uiso 1 1 calc R . . C14 C 0.2450(3) 0.0819(6) -0.00657(16) 0.0289(8) Uani 1 1 d . . . C15 C 0.3014(4) -0.1260(8) 0.0049(3) 0.0659(16) Uani 1 1 d . . . H15A H 0.3672 -0.0918 0.0118 0.099 Uiso 1 1 calc R . . H15B H 0.2951 -0.2185 -0.0284 0.099 Uiso 1 1 calc R . . H15C H 0.2771 -0.1972 0.0384 0.099 Uiso 1 1 calc R . . C16 C 0.2863(5) 0.2002(10) -0.0565(2) 0.079(2) Uani 1 1 d . . . H16A H 0.2487 0.3254 -0.0650 0.118 Uiso 1 1 calc R . . H16B H 0.2864 0.1086 -0.0901 0.118 Uiso 1 1 calc R . . H16C H 0.3502 0.2424 -0.0466 0.118 Uiso 1 1 calc R . . C17 C 0.1434(3) 0.0114(9) -0.0234(2) 0.0624(16) Uani 1 1 d . . . H17A H 0.1062 0.1350 -0.0340 0.094 Uiso 1 1 calc R . . H17B H 0.1155 -0.0593 0.0091 0.094 Uiso 1 1 calc R . . H17C H 0.1451 -0.0856 -0.0558 0.094 Uiso 1 1 calc R . . C18 C 0.0754(3) 0.5115(6) 0.14466(18) 0.0308(9) Uani 1 1 d . . . C19 C 0.0526(3) 0.3811(7) 0.1986(2) 0.0412(10) Uani 1 1 d . . . H19A H -0.0105 0.4145 0.2106 0.062 Uiso 1 1 calc R . . H19B H 0.0973 0.4157 0.2295 0.062 Uiso 1 1 calc R . . H19C H 0.0567 0.2309 0.1898 0.062 Uiso 1 1 calc R . . C20 C 0.0676(3) 0.7536(7) 0.1575(2) 0.0444(11) Uani 1 1 d . . . H20A H 0.0021 0.7916 0.1615 0.067 Uiso 1 1 calc R . . H20B H 0.0938 0.8335 0.1260 0.067 Uiso 1 1 calc R . . H20C H 0.1022 0.7863 0.1930 0.067 Uiso 1 1 calc R . . C21 C -0.0052(3) 0.4658(10) 0.0991(2) 0.0571(15) Uani 1 1 d . . . H21A H -0.0626 0.5336 0.1111 0.086 Uiso 1 1 calc R . . H21B H -0.0151 0.3139 0.0961 0.086 Uiso 1 1 calc R . . H21C H 0.0123 0.5216 0.0620 0.086 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 P1 0.0362(5) 0.0230(4) 0.0213(5) -0.0022(4) 0.0031(4) -0.0008(4) C1 0.045(3) 0.048(2) 0.046(3) -0.027(2) 0.005(2) 0.007(2) P2 0.0529(7) 0.0448(6) 0.0254(6) -0.0006(5) 0.0066(5) -0.0017(5) C2 0.039(2) 0.029(2) 0.070(4) -0.014(2) 0.002(2) 0.0007(18) C3 0.051(3) 0.0211(18) 0.047(3) 0.0030(18) -0.004(2) -0.0065(18) C4 0.0296(18) 0.0193(15) 0.0176(16) 0.0032(13) 0.0038(14) 0.0011(14) C5 0.0242(17) 0.0227(17) 0.0207(19) 0.0041(14) 0.0012(13) -0.0005(14) C6 0.0239(17) 0.0231(17) 0.026(2) -0.0012(15) 0.0065(14) -0.0010(14) C7 0.0262(17) 0.0209(16) 0.0174(17) 0.0034(13) 0.0021(13) -0.0008(13) C8 0.0224(17) 0.0284(19) 0.029(2) 0.0005(16) 0.0003(14) -0.0028(14) C9 0.0245(18) 0.0239(17) 0.0215(19) 0.0021(15) 0.0047(13) 0.0015(14) C10 0.0221(18) 0.0272(18) 0.027(2) -0.0036(16) 0.0036(14) -0.0012(14) C11 0.0221(18) 0.045(2) 0.042(3) -0.014(2) 0.0033(16) 0.0029(17) C12 0.0273(18) 0.038(2) 0.034(2) -0.0011(19) -0.0038(15) 0.0008(17) C13 0.0273(18) 0.033(2) 0.036(2) -0.0007(18) -0.0005(16) -0.0095(16) C14 0.0306(19) 0.0315(19) 0.0244(19) -0.0063(15) 0.0002(15) -0.0049(16) C15 0.081(4) 0.054(3) 0.061(4) -0.030(3) -0.013(3) 0.023(3) C16 0.128(5) 0.082(4) 0.027(3) -0.013(3) 0.016(3) -0.053(4) C17 0.056(3) 0.075(4) 0.056(3) -0.039(3) -0.005(3) -0.010(3) C18 0.0261(19) 0.036(2) 0.031(2) -0.0017(17) 0.0073(15) 0.0061(16) C19 0.033(2) 0.045(2) 0.046(3) 0.004(2) 0.0138(17) -0.0018(19) C20 0.040(2) 0.037(2) 0.057(3) -0.001(2) 0.009(2) 0.0104(19) C21 0.030(2) 0.084(4) 0.057(3) -0.031(3) -0.001(2) 0.007(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 P1 C3 1.725(4) . ? P1 C4 1.824(4) . ? P1 P2 2.0750(18) . ? C1 C2 1.412(7) . ? C1 P2 1.732(5) . ? C2 C3 1.349(6) . ? C4 C9 1.429(5) . ? C4 C5 1.432(5) . ? C5 C6 1.379(5) . ? C5 C10 1.556(5) . ? C6 C7 1.399(5) . ? C7 C8 1.379(5) . ? C7 C14 1.517(5) . ? C8 C9 1.381(5) . ? C9 C18 1.569(5) . ? C10 C11 1.538(5) . ? C10 C13 1.547(5) . ? C10 C12 1.547(5) . ? C14 C16 1.496(6) . ? C14 C17 1.536(6) . ? C14 C15 1.539(6) . ? C18 C19 1.524(6) . ? C18 C20 1.543(6) . ? C18 C21 1.550(6) . ? 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 C3 P1 C4 120.31(19) . . ? C3 P1 P2 100.85(17) . . ? C4 P1 P2 130.10(12) . . ? C2 C1 P2 119.7(3) . . ? C1 P2 P1 88.84(18) . . ? C3 C2 C1 118.8(4) . . ? C2 C3 P1 110.8(4) . . ? C9 C4 C5 119.8(3) . . ? C9 C4 P1 122.7(3) . . ? C5 C4 P1 117.5(3) . . ? C6 C5 C4 117.7(3) . . ? C6 C5 C10 117.2(3) . . ? C4 C5 C10 125.1(3) . . ? C5 C6 C7 124.0(3) . . ? C8 C7 C6 116.4(3) . . ? C8 C7 C14 123.5(3) . . ? C6 C7 C14 120.1(3) . . ? C7 C8 C9 124.3(3) . . ? C8 C9 C4 117.8(3) . . ? C8 C9 C18 115.7(3) . . ? C4 C9 C18 126.4(3) . . ? C11 C10 C13 104.9(3) . . ? C11 C10 C12 105.1(3) . . ? C13 C10 C12 110.9(3) . . ? C11 C10 C5 111.8(3) . . ? C13 C10 C5 112.1(3) . . ? C12 C10 C5 111.6(3) . . ? C16 C14 C7 109.1(3) . . ? C16 C14 C17 109.1(4) . . ? C7 C14 C17 113.2(3) . . ? C16 C14 C15 109.7(4) . . ? C7 C14 C15 109.8(3) . . ? C17 C14 C15 106.0(4) . . ? C19 C18 C20 110.4(4) . . ? C19 C18 C21 106.6(4) . . ? C20 C18 C21 104.7(4) . . ? C19 C18 C9 109.8(3) . . ? C20 C18 C9 114.2(3) . . ? C21 C18 C9 110.8(3) . . ? 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 C2 C1 P2 P1 5.7(4) . . . . ? C3 P1 P2 C1 -8.1(2) . . . . ? C4 P1 P2 C1 -154.5(2) . . . . ? P2 C1 C2 C3 0.1(6) . . . . ? C1 C2 C3 P1 -7.5(5) . . . . ? C4 P1 C3 C2 160.6(3) . . . . ? P2 P1 C3 C2 9.9(3) . . . . ? C3 P1 C4 C9 -80.4(3) . . . . ? P2 P1 C4 C9 60.6(3) . . . . ? C3 P1 C4 C5 99.5(3) . . . . ? P2 P1 C4 C5 -119.5(2) . . . . ? C9 C4 C5 C6 -0.7(5) . . . . ? P1 C4 C5 C6 179.4(3) . . . . ? C9 C4 C5 C10 -178.5(3) . . . . ? P1 C4 C5 C10 1.6(5) . . . . ? C4 C5 C6 C7 -0.3(5) . . . . ? C10 C5 C6 C7 177.6(3) . . . . ? C5 C6 C7 C8 -0.1(5) . . . . ? C5 C6 C7 C14 178.3(3) . . . . ? C6 C7 C8 C9 1.7(5) . . . . ? C14 C7 C8 C9 -176.7(3) . . . . ? C7 C8 C9 C4 -2.7(6) . . . . ? C7 C8 C9 C18 180.0(3) . . . . ? C5 C4 C9 C8 2.1(5) . . . . ? P1 C4 C9 C8 -178.0(3) . . . . ? C5 C4 C9 C18 179.1(3) . . . . ? P1 C4 C9 C18 -1.0(5) . . . . ? C6 C5 C10 C11 2.3(5) . . . . ? C4 C5 C10 C11 -179.9(3) . . . . ? C6 C5 C10 C13 119.8(4) . . . . ? C4 C5 C10 C13 -62.4(5) . . . . ? C6 C5 C10 C12 -115.1(4) . . . . ? C4 C5 C10 C12 62.7(4) . . . . ? C8 C7 C14 C16 114.0(5) . . . . ? C6 C7 C14 C16 -64.4(5) . . . . ? C8 C7 C14 C17 -7.6(5) . . . . ? C6 C7 C14 C17 174.0(4) . . . . ? C8 C7 C14 C15 -125.8(4) . . . . ? C6 C7 C14 C15 55.8(5) . . . . ? C8 C9 C18 C19 100.6(4) . . . . ? C4 C9 C18 C19 -76.5(5) . . . . ? C8 C9 C18 C20 -134.8(4) . . . . ? C4 C9 C18 C20 48.1(5) . . . . ? C8 C9 C18 C21 -16.8(5) . . . . ? C4 C9 C18 C21 166.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.653 _refine_diff_density_min -0.565 _refine_diff_density_rms 0.089 #===END data_06069 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H75 F3 N2 O3 P2 S' _chemical_formula_weight 867.09 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' 'F' 'F' 0.0171 0.0103 '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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.124(3) _cell_length_b 20.119(5) _cell_length_c 24.693(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5030(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description wedge _exptl_crystal_colour colourless _exptl_crystal_size_min 0.010 _exptl_crystal_size_mid 0.070 _exptl_crystal_size_max 0.130 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.145 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 0.177 _exptl_absorpt_correction_type none _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 'Bruker P4' _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 39210 _diffrn_reflns_av_R_equivalents 0.1983 _diffrn_reflns_av_sigmaI/netI 0.1592 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 23.86 _reflns_number_total 7744 _reflns_number_gt 3294 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 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^)+(0.0778P)^2^+0.2436P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.10(17) _refine_ls_number_reflns 7744 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2069 _refine_ls_R_factor_gt 0.0777 _refine_ls_wR_factor_ref 0.2066 _refine_ls_wR_factor_gt 0.1552 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _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 P1 P 0.4918(2) 0.30512(12) 0.31903(9) 0.0698(7) Uani 1 1 d . . . P2 P 0.4492(2) 0.44109(12) 0.12215(8) 0.0624(7) Uani 1 1 d . . . N7 N 0.2672(8) 0.3331(5) 0.0486(3) 0.079(2) Uani 1 1 d . . . N12 N 0.4408(8) 0.2742(4) 0.0847(3) 0.074(2) Uani 1 1 d . . . H12A H 0.5216 0.2737 0.0954 0.088 Uiso 1 1 calc R . . C1 C 0.5235(8) 0.3221(4) 0.2561(3) 0.074(2) Uani 1 1 d . . . H1A H 0.6042 0.3053 0.2443 0.089 Uiso 1 1 calc R . . C2 C 0.4506(8) 0.3587(4) 0.2135(3) 0.069(2) Uani 1 1 d . . . H2A H 0.3892 0.3891 0.2306 0.082 Uiso 1 1 calc R . . H2B H 0.3996 0.3273 0.1923 0.082 Uiso 1 1 calc R . . C3 C 0.5417(8) 0.3983(4) 0.1752(3) 0.070(2) Uani 1 1 d . . . H3A H 0.6046 0.3681 0.1587 0.084 Uiso 1 1 calc R . . H3B H 0.5910 0.4307 0.1962 0.084 Uiso 1 1 calc R . . C4 C 0.4631(9) 0.3915(4) 0.0581(3) 0.064(2) Uani 1 1 d . . . H4A H 0.5548 0.3857 0.0462 0.077 Uiso 1 1 calc R . . C5 C 0.3759(9) 0.4257(4) 0.0148(3) 0.082(3) Uani 1 1 d . . . H5A H 0.3769 0.4736 0.0193 0.099 Uiso 1 1 calc R . . H5B H 0.4059 0.4149 -0.0214 0.099 Uiso 1 1 calc R . . C6 C 0.2392(10) 0.3978(6) 0.0252(4) 0.097(3) Uani 1 1 d . . . H6A H 0.1903 0.4256 0.0503 0.117 Uiso 1 1 calc R . . H6B H 0.1895 0.3937 -0.0082 0.117 Uiso 1 1 calc R . . C8 C 0.3924(9) 0.3278(5) 0.0640(3) 0.063(2) Uani 1 1 d . . . C9 C 0.1745(10) 0.2798(6) 0.0528(4) 0.098(3) Uani 1 1 d . . . H9A H 0.1073 0.2913 0.0792 0.118 Uiso 1 1 calc R . . H9B H 0.1313 0.2734 0.0182 0.118 Uiso 1 1 calc R . . C10 C 0.2360(15) 0.2204(7) 0.0685(8) 0.214(10) Uani 1 1 d . . . H10A H 0.1763 0.1997 0.0941 0.257 Uiso 1 1 calc R . . H10B H 0.2352 0.1923 0.0365 0.257 Uiso 1 1 calc R . . C11 C 0.3591(13) 0.2136(5) 0.0902(4) 0.101(3) Uani 1 1 d . . . H11A H 0.4038 0.1769 0.0725 0.121 Uiso 1 1 calc R . . H11B H 0.3507 0.2026 0.1283 0.121 Uiso 1 1 calc R . . C12 C 0.3268(7) 0.3430(5) 0.3284(3) 0.053(2) Uani 1 1 d . . . C13 C 0.2111(9) 0.3061(5) 0.3123(3) 0.063(2) Uani 1 1 d . . . C14 C 0.0959(8) 0.3422(6) 0.3039(3) 0.072(3) Uani 1 1 d . . . H14A H 0.0216 0.3196 0.2916 0.087 Uiso 1 1 calc R . . C15 C 0.0852(8) 0.4105(5) 0.3128(3) 0.064(2) Uani 1 1 d . . . C16 C 0.1951(8) 0.4416(5) 0.3343(3) 0.066(2) Uani 1 1 d . . . H16A H 0.1899 0.4867 0.3422 0.079 Uiso 1 1 calc R . . C17 C 0.3131(8) 0.4085(5) 0.3445(3) 0.063(2) Uani 1 1 d . . . C18 C 0.2082(8) 0.2300(5) 0.3042(3) 0.066(2) Uani 1 1 d . . . C19 C 0.2549(9) 0.2117(5) 0.2472(3) 0.100(3) Uani 1 1 d . . . H19A H 0.2305 0.1666 0.2393 0.150 Uiso 1 1 calc R . . H19B H 0.3492 0.2161 0.2451 0.150 Uiso 1 1 calc R . . H19C H 0.2144 0.2409 0.2213 0.150 Uiso 1 1 calc R . . C20 C 0.2903(9) 0.1921(4) 0.3463(4) 0.089(3) Uani 1 1 d . . . H20A H 0.2819 0.1452 0.3401 0.134 Uiso 1 1 calc R . . H20B H 0.2591 0.2027 0.3819 0.134 Uiso 1 1 calc R . . H20C H 0.3814 0.2048 0.3431 0.134 Uiso 1 1 calc R . . C21 C 0.0660(8) 0.2024(5) 0.3098(3) 0.091(3) Uani 1 1 d . . . H21A H 0.0680 0.1547 0.3082 0.137 Uiso 1 1 calc R . . H21B H 0.0122 0.2193 0.2809 0.137 Uiso 1 1 calc R . . H21C H 0.0296 0.2161 0.3439 0.137 Uiso 1 1 calc R . . C22 C -0.0371(8) 0.4509(5) 0.2993(4) 0.081(3) Uani 1 1 d . . . C23 C -0.1522(8) 0.4048(5) 0.2819(4) 0.109(4) Uani 1 1 d . . . H23A H -0.1261 0.3795 0.2506 0.164 Uiso 1 1 calc R . . H23B H -0.2282 0.4312 0.2732 0.164 Uiso 1 1 calc R . . H23C H -0.1734 0.3750 0.3110 0.164 Uiso 1 1 calc R . . C24 C -0.0840(9) 0.4894(6) 0.3500(4) 0.114(4) Uani 1 1 d . . . H24A H -0.0134 0.5170 0.3631 0.171 Uiso 1 1 calc R . . H24B H -0.1094 0.4585 0.3777 0.171 Uiso 1 1 calc R . . H24C H -0.1582 0.5168 0.3406 0.171 Uiso 1 1 calc R . . C25 C -0.0066(9) 0.4989(5) 0.2542(4) 0.124(4) Uani 1 1 d . . . H25A H 0.0619 0.5288 0.2655 0.186 Uiso 1 1 calc R . . H25B H -0.0846 0.5238 0.2453 0.186 Uiso 1 1 calc R . . H25C H 0.0224 0.4746 0.2228 0.186 Uiso 1 1 calc R . . C26 C 0.4215(7) 0.4500(4) 0.3746(3) 0.059(2) Uani 1 1 d . . . C27 C 0.3631(11) 0.4971(6) 0.4152(5) 0.148(5) Uani 1 1 d . . . H27A H 0.3215 0.5334 0.3967 0.222 Uiso 1 1 calc R . . H27B H 0.4317 0.5139 0.4383 0.222 Uiso 1 1 calc R . . H27C H 0.2986 0.4741 0.4367 0.222 Uiso 1 1 calc R . . C28 C 0.4999(10) 0.4913(6) 0.3355(4) 0.125(4) Uani 1 1 d . . . H28A H 0.4410 0.5178 0.3140 0.187 Uiso 1 1 calc R . . H28B H 0.5502 0.4626 0.3122 0.187 Uiso 1 1 calc R . . H28C H 0.5588 0.5198 0.3552 0.187 Uiso 1 1 calc R . . C29 C 0.5193(11) 0.4074(5) 0.4063(5) 0.136(5) Uani 1 1 d . . . H29A H 0.5760 0.4357 0.4273 0.204 Uiso 1 1 calc R . . H29B H 0.5715 0.3817 0.3815 0.204 Uiso 1 1 calc R . . H29C H 0.4718 0.3781 0.4300 0.204 Uiso 1 1 calc R . . C30 C 0.5195(7) 0.5204(4) 0.0993(3) 0.054(2) Uani 1 1 d . . . C31 C 0.4294(7) 0.5743(4) 0.1045(3) 0.051(2) Uani 1 1 d . . . C32 C 0.4347(7) 0.6263(4) 0.0686(3) 0.056(2) Uani 1 1 d . . . H32A H 0.3736 0.6605 0.0724 0.067 Uiso 1 1 calc R . . C33 C 0.5272(8) 0.6307(4) 0.0266(3) 0.054(2) Uani 1 1 d . . . C34 C 0.6256(8) 0.5836(4) 0.0270(3) 0.057(2) Uani 1 1 d . . . H34A H 0.6934 0.5881 0.0018 0.068 Uiso 1 1 calc R . . C35 C 0.6314(7) 0.5301(4) 0.0619(3) 0.050(2) Uani 1 1 d . . . C36 C 0.3242(7) 0.5809(5) 0.1509(3) 0.066(2) Uani 1 1 d . . . C37 C 0.3715(8) 0.5509(4) 0.2044(3) 0.075(3) Uani 1 1 d . . . H37A H 0.3099 0.5618 0.2326 0.112 Uiso 1 1 calc R . . H37B H 0.4568 0.5686 0.2133 0.112 Uiso 1 1 calc R . . H37C H 0.3774 0.5035 0.2008 0.112 Uiso 1 1 calc R . . C38 C 0.1930(7) 0.5498(5) 0.1338(3) 0.093(3) Uani 1 1 d . . . H38A H 0.1276 0.5581 0.1611 0.139 Uiso 1 1 calc R . . H38B H 0.2042 0.5027 0.1293 0.139 Uiso 1 1 calc R . . H38C H 0.1648 0.5690 0.1001 0.139 Uiso 1 1 calc R . . C39 C 0.2918(9) 0.6537(5) 0.1631(4) 0.090(3) Uani 1 1 d . . . H39A H 0.2365 0.6562 0.1946 0.134 Uiso 1 1 calc R . . H39B H 0.2465 0.6729 0.1327 0.134 Uiso 1 1 calc R . . H39C H 0.3722 0.6778 0.1696 0.134 Uiso 1 1 calc R . . C40 C 0.5197(8) 0.6866(4) -0.0139(3) 0.065(2) Uani 1 1 d . . . C41 C 0.3872(8) 0.6777(5) -0.0455(3) 0.092(3) Uani 1 1 d . . . H41A H 0.3850 0.6344 -0.0618 0.138 Uiso 1 1 calc R . . H41B H 0.3809 0.7111 -0.0732 0.138 Uiso 1 1 calc R . . H41C H 0.3144 0.6822 -0.0209 0.138 Uiso 1 1 calc R . . C42 C 0.5182(8) 0.7539(4) 0.0130(3) 0.078(3) Uani 1 1 d . . . H42A H 0.5931 0.7578 0.0366 0.117 Uiso 1 1 calc R . . H42B H 0.4384 0.7587 0.0337 0.117 Uiso 1 1 calc R . . H42C H 0.5220 0.7880 -0.0141 0.117 Uiso 1 1 calc R . . C43 C 0.6310(8) 0.6861(4) -0.0554(3) 0.081(3) Uani 1 1 d . . . H43A H 0.7145 0.6856 -0.0370 0.122 Uiso 1 1 calc R . . H43B H 0.6251 0.7251 -0.0777 0.122 Uiso 1 1 calc R . . H43C H 0.6234 0.6472 -0.0778 0.122 Uiso 1 1 calc R . . C44 C 0.7625(7) 0.4906(4) 0.0593(3) 0.060(2) Uani 1 1 d . . . C45 C 0.8769(7) 0.5402(4) 0.0634(3) 0.076(3) Uani 1 1 d . . . H45A H 0.9592 0.5171 0.0589 0.114 Uiso 1 1 calc R . . H45B H 0.8751 0.5612 0.0983 0.114 Uiso 1 1 calc R . . H45C H 0.8681 0.5732 0.0356 0.114 Uiso 1 1 calc R . . C46 C 0.7741(8) 0.4576(5) 0.0024(3) 0.088(3) Uani 1 1 d . . . H46A H 0.7006 0.4282 -0.0032 0.131 Uiso 1 1 calc R . . H46B H 0.8550 0.4328 0.0004 0.131 Uiso 1 1 calc R . . H46C H 0.7739 0.4914 -0.0250 0.131 Uiso 1 1 calc R . . C47 C 0.7834(8) 0.4403(5) 0.1024(4) 0.100(3) Uani 1 1 d . . . H47A H 0.7229 0.4041 0.0973 0.150 Uiso 1 1 calc R . . H47B H 0.7685 0.4603 0.1371 0.150 Uiso 1 1 calc R . . H47C H 0.8724 0.4240 0.1006 0.150 Uiso 1 1 calc R . . S1 S 0.7886(4) 0.21579(19) 0.09788(13) 0.1103(10) Uani 1 1 d . . . F1 F 0.9242(16) 0.1553(5) 0.1688(4) 0.289(7) Uani 1 1 d . . . F2 F 0.7716(11) 0.2101(5) 0.2005(3) 0.229(5) Uani 1 1 d . . . F3 F 0.9357(9) 0.2610(6) 0.1695(3) 0.215(4) Uani 1 1 d . . . O1 O 0.7155(7) 0.2764(4) 0.0998(3) 0.135(3) Uani 1 1 d . . . O2 O 0.8960(6) 0.2113(4) 0.0630(3) 0.122(3) Uani 1 1 d . . . O3 O 0.6980(11) 0.1575(5) 0.0965(5) 0.223(6) Uani 1 1 d . . . C1' C 0.8455(17) 0.2131(16) 0.1552(10) 0.319(19) 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 P1 0.0610(14) 0.0883(18) 0.0602(14) 0.0044(13) -0.0033(12) -0.0068(14) P2 0.0577(13) 0.0825(17) 0.0468(12) 0.0044(12) 0.0009(11) -0.0154(13) N7 0.078(6) 0.100(7) 0.059(5) 0.006(5) -0.005(4) -0.036(6) N12 0.083(5) 0.068(6) 0.070(5) -0.002(4) -0.007(4) -0.024(5) C1 0.059(5) 0.088(7) 0.076(6) 0.011(5) -0.006(5) -0.001(5) C2 0.064(6) 0.081(6) 0.060(5) 0.004(5) -0.002(5) -0.009(5) C3 0.062(5) 0.083(6) 0.064(5) 0.013(5) -0.005(5) -0.008(5) C4 0.070(6) 0.081(6) 0.041(5) 0.005(4) 0.004(4) -0.006(5) C5 0.102(7) 0.084(7) 0.061(6) 0.003(5) -0.015(5) -0.033(6) C6 0.105(9) 0.115(10) 0.072(7) 0.021(6) -0.030(6) -0.020(7) C8 0.068(7) 0.074(8) 0.047(5) -0.003(5) 0.001(5) -0.013(6) C9 0.100(8) 0.110(9) 0.085(7) -0.006(7) -0.010(6) -0.044(8) C10 0.140(13) 0.070(10) 0.43(3) 0.042(14) -0.090(16) -0.055(10) C11 0.140(10) 0.090(9) 0.074(6) 0.020(6) -0.008(7) -0.037(8) C12 0.041(5) 0.072(6) 0.046(5) 0.009(5) 0.002(4) -0.008(5) C13 0.066(6) 0.081(7) 0.042(5) 0.008(5) 0.004(4) 0.003(6) C14 0.052(6) 0.110(9) 0.055(5) 0.020(6) -0.004(4) -0.022(6) C15 0.049(6) 0.084(8) 0.059(5) 0.012(5) 0.001(4) -0.008(6) C16 0.055(6) 0.080(7) 0.062(6) 0.004(5) 0.014(4) -0.006(6) C17 0.048(6) 0.095(8) 0.046(5) 0.003(5) 0.006(4) -0.009(6) C18 0.069(6) 0.084(7) 0.045(5) -0.006(5) 0.007(4) -0.013(5) C19 0.124(8) 0.105(8) 0.071(6) -0.014(6) 0.020(6) -0.038(7) C20 0.100(7) 0.088(7) 0.079(6) 0.021(6) -0.007(6) -0.009(6) C21 0.083(6) 0.106(8) 0.084(6) 0.008(6) 0.000(6) -0.038(6) C22 0.043(5) 0.110(8) 0.089(7) 0.031(6) -0.002(5) -0.011(6) C23 0.058(6) 0.142(10) 0.127(9) 0.011(8) -0.018(6) 0.006(7) C24 0.078(7) 0.140(10) 0.125(9) 0.020(8) 0.014(7) 0.014(7) C25 0.075(6) 0.158(10) 0.140(9) 0.087(9) 0.005(6) 0.019(8) C26 0.047(5) 0.065(6) 0.066(5) 0.001(5) 0.005(4) -0.018(5) C27 0.104(8) 0.180(12) 0.160(11) -0.113(10) 0.006(8) -0.009(9) C28 0.097(7) 0.174(11) 0.103(8) 0.022(8) -0.030(6) -0.068(8) C29 0.163(11) 0.091(8) 0.153(10) 0.005(7) -0.109(10) 0.000(8) C30 0.051(5) 0.072(6) 0.040(4) 0.001(4) -0.001(4) -0.017(5) C31 0.047(5) 0.064(6) 0.042(5) -0.007(4) 0.008(4) -0.015(5) C32 0.041(5) 0.068(6) 0.059(5) 0.003(5) 0.001(4) 0.002(4) C33 0.051(5) 0.061(6) 0.051(5) 0.008(4) -0.001(4) -0.017(5) C34 0.052(5) 0.073(7) 0.046(5) -0.001(5) 0.002(4) -0.007(5) C35 0.043(5) 0.055(6) 0.053(5) -0.008(4) 0.003(4) -0.015(4) C36 0.054(5) 0.088(7) 0.056(5) 0.005(5) 0.011(4) -0.005(5) C37 0.059(5) 0.104(7) 0.061(5) -0.006(5) 0.013(4) 0.007(5) C38 0.038(5) 0.148(9) 0.093(7) 0.018(7) 0.005(5) -0.015(6) C39 0.085(6) 0.095(8) 0.089(7) 0.005(6) 0.019(5) 0.017(6) C40 0.067(6) 0.065(6) 0.065(5) -0.004(5) -0.006(5) 0.000(5) C41 0.089(7) 0.131(9) 0.056(5) 0.012(6) -0.019(5) -0.009(6) C42 0.076(6) 0.069(7) 0.090(7) 0.016(5) -0.001(5) 0.002(5) C43 0.071(6) 0.105(8) 0.068(6) 0.021(5) 0.017(5) -0.005(6) C44 0.043(5) 0.078(6) 0.059(6) 0.003(5) 0.008(4) -0.004(5) C45 0.047(5) 0.105(8) 0.075(6) 0.004(5) 0.010(4) -0.008(5) C46 0.073(6) 0.104(8) 0.085(7) -0.024(6) 0.033(5) -0.011(6) C47 0.039(5) 0.128(9) 0.132(9) 0.032(8) 0.008(5) 0.011(6) S1 0.121(3) 0.130(3) 0.080(2) 0.010(2) 0.004(2) 0.011(3) F1 0.47(2) 0.240(11) 0.159(8) 0.013(7) -0.004(11) 0.214(13) F2 0.325(13) 0.263(11) 0.097(5) 0.032(6) 0.056(7) 0.119(10) F3 0.189(8) 0.349(13) 0.106(5) -0.077(7) -0.043(6) 0.030(9) O1 0.113(6) 0.107(6) 0.186(8) 0.009(6) -0.033(5) 0.042(5) O2 0.082(5) 0.191(8) 0.094(5) -0.022(5) 0.009(4) -0.030(5) O3 0.239(12) 0.182(9) 0.247(12) -0.086(9) 0.104(10) -0.127(9) C1' 0.104(12) 0.52(4) 0.33(3) -0.37(3) -0.043(15) 0.083(17) _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 P1 C1 1.624(8) . ? P1 C12 1.851(8) . ? P2 C3 1.827(8) . ? P2 C30 1.836(7) . ? P2 C4 1.875(8) . ? N7 C8 1.327(10) . ? N7 C9 1.430(11) . ? N7 C6 1.452(11) . ? N12 C8 1.290(10) . ? N12 C11 1.480(11) . ? C1 C2 1.480(10) . ? C2 C3 1.542(10) . ? C4 C8 1.475(11) . ? C4 C5 1.548(10) . ? C5 C6 1.516(11) . ? C9 C10 1.401(15) . ? C10 C11 1.364(15) . ? C12 C17 1.384(11) . ? C12 C13 1.443(11) . ? C13 C14 1.390(11) . ? C13 C18 1.545(12) . ? C14 C15 1.396(11) . ? C15 C16 1.382(10) . ? C15 C22 1.517(11) . ? C16 C17 1.391(11) . ? C17 C26 1.566(11) . ? C18 C19 1.530(10) . ? C18 C20 1.533(11) . ? C18 C21 1.549(11) . ? C22 C25 1.507(11) . ? C22 C24 1.546(13) . ? C22 C23 1.551(12) . ? C26 C28 1.500(11) . ? C26 C27 1.501(11) . ? C26 C29 1.525(11) . ? C30 C31 1.423(9) . ? C30 C35 1.474(9) . ? C31 C32 1.372(9) . ? C31 C36 1.570(10) . ? C32 C33 1.401(10) . ? C33 C34 1.376(10) . ? C33 C40 1.507(10) . ? C34 C35 1.379(10) . ? C35 C44 1.549(10) . ? C36 C37 1.527(10) . ? C36 C38 1.529(10) . ? C36 C39 1.531(11) . ? C40 C42 1.509(10) . ? C40 C43 1.523(10) . ? C40 C41 1.562(11) . ? C44 C47 1.484(11) . ? C44 C45 1.532(10) . ? C44 C46 1.557(10) . ? S1 O2 1.390(7) . ? S1 O1 1.427(7) . ? S1 O3 1.490(9) . ? S1 C1' 1.53(2) . ? F1 C1' 1.45(3) . ? F2 C1' 1.35(2) . ? F3 C1' 1.38(2) . ? 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 C1 P1 C12 102.2(4) . . ? C3 P2 C30 115.6(4) . . ? C3 P2 C4 108.4(4) . . ? C30 P2 C4 100.0(3) . . ? C8 N7 C9 123.1(9) . . ? C8 N7 C6 111.9(8) . . ? C9 N7 C6 125.0(9) . . ? C8 N12 C11 120.9(8) . . ? C2 C1 P1 133.3(7) . . ? C1 C2 C3 113.2(6) . . ? C2 C3 P2 112.2(5) . . ? C8 C4 C5 100.3(7) . . ? C8 C4 P2 110.0(5) . . ? C5 C4 P2 107.6(6) . . ? C6 C5 C4 103.8(7) . . ? N7 C6 C5 102.8(8) . . ? N12 C8 N7 122.9(9) . . ? N12 C8 C4 125.5(8) . . ? N7 C8 C4 111.4(9) . . ? C10 C9 N7 111.6(9) . . ? C11 C10 C9 126.8(11) . . ? C10 C11 N12 113.1(10) . . ? C17 C12 C13 119.2(7) . . ? C17 C12 P1 121.2(6) . . ? C13 C12 P1 119.1(7) . . ? C14 C13 C12 117.0(8) . . ? C14 C13 C18 118.9(8) . . ? C12 C13 C18 124.1(8) . . ? C13 C14 C15 123.8(8) . . ? C16 C15 C14 116.3(8) . . ? C16 C15 C22 119.9(9) . . ? C14 C15 C22 123.8(8) . . ? C15 C16 C17 123.0(9) . . ? C12 C17 C16 119.3(8) . . ? C12 C17 C26 125.0(8) . . ? C16 C17 C26 115.6(8) . . ? C19 C18 C20 109.7(8) . . ? C19 C18 C13 110.6(7) . . ? C20 C18 C13 113.2(7) . . ? C19 C18 C21 106.5(7) . . ? C20 C18 C21 105.4(7) . . ? C13 C18 C21 111.1(7) . . ? C25 C22 C15 109.7(7) . . ? C25 C22 C24 109.9(9) . . ? C15 C22 C24 110.0(8) . . ? C25 C22 C23 109.4(8) . . ? C15 C22 C23 110.7(8) . . ? C24 C22 C23 107.2(7) . . ? C28 C26 C27 106.9(9) . . ? C28 C26 C29 107.3(8) . . ? C27 C26 C29 105.5(8) . . ? C28 C26 C17 111.2(7) . . ? C27 C26 C17 112.1(7) . . ? C29 C26 C17 113.5(7) . . ? C31 C30 C35 116.6(6) . . ? C31 C30 P2 112.7(5) . . ? C35 C30 P2 127.3(6) . . ? C32 C31 C30 119.8(6) . . ? C32 C31 C36 115.7(7) . . ? C30 C31 C36 124.5(7) . . ? C31 C32 C33 123.6(7) . . ? C34 C33 C32 115.7(7) . . ? C34 C33 C40 123.8(7) . . ? C32 C33 C40 120.4(8) . . ? C33 C34 C35 125.0(7) . . ? C34 C35 C30 117.5(7) . . ? C34 C35 C44 114.2(7) . . ? C30 C35 C44 128.1(7) . . ? C37 C36 C38 110.5(7) . . ? C37 C36 C39 106.0(7) . . ? C38 C36 C39 105.1(7) . . ? C37 C36 C31 112.6(6) . . ? C38 C36 C31 110.6(6) . . ? C39 C36 C31 111.7(7) . . ? C33 C40 C42 112.2(6) . . ? C33 C40 C43 113.9(7) . . ? C42 C40 C43 108.1(7) . . ? C33 C40 C41 106.8(7) . . ? C42 C40 C41 108.3(7) . . ? C43 C40 C41 107.4(6) . . ? C47 C44 C45 106.8(7) . . ? C47 C44 C35 116.2(6) . . ? C45 C44 C35 108.1(7) . . ? C47 C44 C46 110.2(8) . . ? C45 C44 C46 106.3(6) . . ? C35 C44 C46 108.7(6) . . ? O2 S1 O1 118.8(5) . . ? O2 S1 O3 114.6(5) . . ? O1 S1 O3 110.7(6) . . ? O2 S1 C1' 106.1(8) . . ? O1 S1 C1' 101.3(10) . . ? O3 S1 C1' 103.0(13) . . ? F2 C1' F3 100.8(11) . . ? F2 C1' F1 94(2) . . ? F3 C1' F1 97.9(13) . . ? F2 C1' S1 124.1(13) . . ? F3 C1' S1 118(3) . . ? F1 C1' S1 116.8(11) . . ? 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 C12 P1 C1 C2 1.3(9) . . . . ? P1 C1 C2 C3 144.3(7) . . . . ? C1 C2 C3 P2 178.5(6) . . . . ? C30 P2 C3 C2 147.7(6) . . . . ? C4 P2 C3 C2 -101.0(6) . . . . ? C3 P2 C4 C8 67.6(7) . . . . ? C30 P2 C4 C8 -171.0(6) . . . . ? C3 P2 C4 C5 175.9(5) . . . . ? C30 P2 C4 C5 -62.7(6) . . . . ? C8 C4 C5 C6 30.3(8) . . . . ? P2 C4 C5 C6 -84.6(8) . . . . ? C8 N7 C6 C5 14.6(10) . . . . ? C9 N7 C6 C5 -162.9(8) . . . . ? C4 C5 C6 N7 -27.8(9) . . . . ? C11 N12 C8 N7 2.7(13) . . . . ? C11 N12 C8 C4 178.1(8) . . . . ? C9 N7 C8 N12 -0.7(13) . . . . ? C6 N7 C8 N12 -178.3(8) . . . . ? C9 N7 C8 C4 -176.6(7) . . . . ? C6 N7 C8 C4 5.8(10) . . . . ? C5 C4 C8 N12 161.3(8) . . . . ? P2 C4 C8 N12 -85.6(9) . . . . ? C5 C4 C8 N7 -22.9(9) . . . . ? P2 C4 C8 N7 90.2(7) . . . . ? C8 N7 C9 C10 -7.5(15) . . . . ? C6 N7 C9 C10 169.7(12) . . . . ? N7 C9 C10 C11 15(2) . . . . ? C9 C10 C11 N12 -14(2) . . . . ? C8 N12 C11 C10 3.9(15) . . . . ? C1 P1 C12 C17 -89.1(7) . . . . ? C1 P1 C12 C13 83.4(6) . . . . ? C17 C12 C13 C14 12.2(10) . . . . ? P1 C12 C13 C14 -160.4(6) . . . . ? C17 C12 C13 C18 -167.6(7) . . . . ? P1 C12 C13 C18 19.8(9) . . . . ? C12 C13 C14 C15 -3.4(11) . . . . ? C18 C13 C14 C15 176.4(7) . . . . ? C13 C14 C15 C16 -4.0(12) . . . . ? C13 C14 C15 C22 174.9(7) . . . . ? C14 C15 C16 C17 2.9(12) . . . . ? C22 C15 C16 C17 -176.1(7) . . . . ? C13 C12 C17 C16 -13.5(11) . . . . ? P1 C12 C17 C16 158.9(6) . . . . ? C13 C12 C17 C26 166.1(7) . . . . ? P1 C12 C17 C26 -21.4(10) . . . . ? C15 C16 C17 C12 5.9(12) . . . . ? C15 C16 C17 C26 -173.7(7) . . . . ? C14 C13 C18 C19 95.4(9) . . . . ? C12 C13 C18 C19 -84.7(9) . . . . ? C14 C13 C18 C20 -141.0(7) . . . . ? C12 C13 C18 C20 38.8(10) . . . . ? C14 C13 C18 C21 -22.6(10) . . . . ? C12 C13 C18 C21 157.2(7) . . . . ? C16 C15 C22 C25 65.5(11) . . . . ? C14 C15 C22 C25 -113.4(10) . . . . ? C16 C15 C22 C24 -55.5(10) . . . . ? C14 C15 C22 C24 125.6(9) . . . . ? C16 C15 C22 C23 -173.8(7) . . . . ? C14 C15 C22 C23 7.4(12) . . . . ? C12 C17 C26 C28 96.1(10) . . . . ? C16 C17 C26 C28 -84.3(9) . . . . ? C12 C17 C26 C27 -144.4(9) . . . . ? C16 C17 C26 C27 35.3(11) . . . . ? C12 C17 C26 C29 -25.0(11) . . . . ? C16 C17 C26 C29 154.7(8) . . . . ? C3 P2 C30 C31 -123.2(5) . . . . ? C4 P2 C30 C31 120.7(5) . . . . ? C3 P2 C30 C35 78.5(7) . . . . ? C4 P2 C30 C35 -37.7(7) . . . . ? C35 C30 C31 C32 12.0(10) . . . . ? P2 C30 C31 C32 -148.8(6) . . . . ? C35 C30 C31 C36 -165.4(6) . . . . ? P2 C30 C31 C36 33.7(8) . . . . ? C30 C31 C32 C33 -1.4(11) . . . . ? C36 C31 C32 C33 176.3(6) . . . . ? C31 C32 C33 C34 -8.1(11) . . . . ? C31 C32 C33 C40 175.0(7) . . . . ? C32 C33 C34 C35 6.5(11) . . . . ? C40 C33 C34 C35 -176.7(7) . . . . ? C33 C34 C35 C30 4.0(11) . . . . ? C33 C34 C35 C44 -171.6(7) . . . . ? C31 C30 C35 C34 -13.2(9) . . . . ? P2 C30 C35 C34 144.4(6) . . . . ? C31 C30 C35 C44 161.7(7) . . . . ? P2 C30 C35 C44 -40.7(10) . . . . ? C32 C31 C36 C37 -144.8(7) . . . . ? C30 C31 C36 C37 32.7(10) . . . . ? C32 C31 C36 C38 91.0(9) . . . . ? C30 C31 C36 C38 -91.5(9) . . . . ? C32 C31 C36 C39 -25.7(10) . . . . ? C30 C31 C36 C39 151.9(7) . . . . ? C34 C33 C40 C42 -122.5(8) . . . . ? C32 C33 C40 C42 54.2(10) . . . . ? C34 C33 C40 C43 0.7(11) . . . . ? C32 C33 C40 C43 177.3(7) . . . . ? C34 C33 C40 C41 119.0(8) . . . . ? C32 C33 C40 C41 -64.3(9) . . . . ? C34 C35 C44 C47 169.6(7) . . . . ? C30 C35 C44 C47 -5.5(12) . . . . ? C34 C35 C44 C45 49.6(8) . . . . ? C30 C35 C44 C45 -125.4(8) . . . . ? C34 C35 C44 C46 -65.4(8) . . . . ? C30 C35 C44 C46 119.6(8) . . . . ? O2 S1 C1' F2 -174(2) . . . . ? O1 S1 C1' F2 61(3) . . . . ? O3 S1 C1' F2 -53(3) . . . . ? O2 S1 C1' F3 58.7(15) . . . . ? O1 S1 C1' F3 -66.0(12) . . . . ? O3 S1 C1' F3 179.4(11) . . . . ? O2 S1 C1' F1 -57(2) . . . . ? O1 S1 C1' F1 178.1(19) . . . . ? O3 S1 C1' F1 63(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.86 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.307 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.046 #===END data_07049 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H76 N2 O P2' _chemical_formula_weight 735.03 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8533(17) _cell_length_b 14.226(2) _cell_length_c 17.618(3) _cell_angle_alpha 79.224(2) _cell_angle_beta 77.112(2) _cell_angle_gamma 71.911(2) _cell_volume 2269.8(6) _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 ireg.blok _exptl_crystal_colour gold _exptl_crystal_size_min 0.160 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_max 0.480 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.075 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.129 _exptl_absorpt_correction_type none _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 'Bruker P4' _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 34307 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0582 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 28.10 _reflns_number_total 10951 _reflns_number_gt 7880 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 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^)+(0.0641P)^2^+0.2745P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10951 _refine_ls_number_parameters 506 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0748 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1417 _refine_ls_wR_factor_gt 0.1271 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _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 N1' N 0.249(5) 0.104(3) 0.270(2) 0.035(11) Uani 0.083(3) 1 d P A 2 P1' P 0.2014(8) 0.0079(5) 0.3140(6) 0.038(3) Uani 0.083(3) 1 d P A 2 P2' P 0.1140(9) 0.2133(6) 0.2998(9) 0.051(3) Uani 0.083(3) 1 d P A 2 P1 P 0.20175(5) 0.01487(4) 0.26336(5) 0.0214(2) Uani 0.917(3) 1 d P A 1 P2 P 0.11484(6) 0.22074(4) 0.25485(5) 0.02126(16) Uani 0.917(3) 1 d P A 1 O1 O 0.87075(19) -0.00918(12) 0.12077(11) 0.0691(5) Uani 1 1 d . A 1 N1 N 0.2396(4) 0.1146(3) 0.29458(18) 0.0215(6) Uani 0.917(3) 1 d P A 1 N2 N 0.72561(16) 0.14725(12) 0.14056(9) 0.0340(4) Uani 1 1 d . A 1 C1 C 0.03476(19) 0.01293(14) 0.33532(11) 0.0318(4) Uani 1 1 d . A 1 H1A H 0.0050 -0.0455 0.3338 0.038 Uiso 1 1 calc R A 1 H1B H 0.0500 0.0120 0.3880 0.038 Uiso 1 1 calc R A 1 C2 C -0.08108(18) 0.10900(13) 0.31127(11) 0.0299(4) Uani 1 1 d . A 1 H2A H -0.0855 0.1121 0.2564 0.036 Uiso 1 1 calc R A 1 H2B H -0.1750 0.1060 0.3417 0.036 Uiso 1 1 calc R A 1 C3 C -0.05125(18) 0.20423(13) 0.32339(11) 0.0309(4) Uani 1 1 d . A 1 H3A H -0.0385 0.1996 0.3771 0.037 Uiso 1 1 calc R A 1 H3B H -0.1331 0.2613 0.3139 0.037 Uiso 1 1 calc R A 1 C4 C 0.39097(17) 0.11482(12) 0.28734(10) 0.0244(4) Uani 1 1 d . A 1 H4A H 0.4423 0.0512 0.3128 0.029 Uiso 1 1 calc R A 1 H4B H 0.3912 0.1658 0.3169 0.029 Uiso 1 1 calc R A 1 C5 C 0.47869(18) 0.13205(13) 0.20553(10) 0.0284(4) Uani 1 1 d . A 1 H5A H 0.4768 0.0842 0.1734 0.034 Uiso 1 1 calc R A 1 H5B H 0.4368 0.1985 0.1806 0.034 Uiso 1 1 calc R A 1 C6 C 0.6337(2) 0.12030(17) 0.21276(12) 0.0411(5) Uani 1 1 d . A 1 H6A H 0.6320 0.1611 0.2515 0.049 Uiso 1 1 calc R A 1 H6B H 0.6769 0.0514 0.2323 0.049 Uiso 1 1 calc R A 1 C7 C 0.7277(2) 0.24905(15) 0.11354(13) 0.0463(5) Uani 1 1 d . A 1 H7A H 0.7587 0.2760 0.1513 0.056 Uiso 1 1 calc R A 1 H7B H 0.6326 0.2908 0.1046 0.056 Uiso 1 1 calc R A 1 C8 C 0.8365(2) 0.24235(16) 0.03720(13) 0.0468(5) Uani 1 1 d . A 1 H8A H 0.7881 0.2544 -0.0074 0.056 Uiso 1 1 calc R A 1 H8B H 0.8916 0.2902 0.0304 0.056 Uiso 1 1 calc R A 1 C9 C 0.9332(2) 0.13708(17) 0.04629(13) 0.0450(5) Uani 1 1 d . A 1 H9A H 0.9628 0.1102 -0.0034 0.054 Uiso 1 1 calc R A 1 H9B H 1.0192 0.1344 0.0657 0.054 Uiso 1 1 calc R A 1 C10 C 0.8413(2) 0.08013(15) 0.10485(12) 0.0368(4) Uani 1 1 d . A 1 C11 C 0.36246(17) -0.09495(12) 0.27601(10) 0.0224(3) Uani 1 1 d . A 1 C12 C 0.43973(17) -0.12273(12) 0.20095(9) 0.0225(3) Uani 1 1 d . A 1 C13 C 0.58807(18) -0.17360(12) 0.19364(10) 0.0246(4) Uani 1 1 d . A 1 H13A H 0.6398 -0.1879 0.1441 0.030 Uiso 1 1 calc R A 1 C14 C 0.66107(17) -0.20353(12) 0.25649(10) 0.0242(4) Uani 1 1 d . A 1 C15 C 0.57788(18) -0.19031(12) 0.33051(10) 0.0257(4) Uani 1 1 d . A 1 H15A H 0.6227 -0.2170 0.3740 0.031 Uiso 1 1 calc R A 1 C16 C 0.43106(18) -0.13920(12) 0.34303(10) 0.0247(4) Uani 1 1 d . A 1 C17 C 0.36937(18) -0.10817(13) 0.12694(10) 0.0263(4) Uani 1 1 d . A 1 C18 C 0.2284(2) -0.13961(15) 0.14943(11) 0.0351(4) Uani 1 1 d . A 1 H18A H 0.2486 -0.2076 0.1738 0.053 Uiso 1 1 calc R A 1 H18B H 0.1887 -0.1336 0.1031 0.053 Uiso 1 1 calc R A 1 H18C H 0.1597 -0.0973 0.1855 0.053 Uiso 1 1 calc R A 1 C19 C 0.3452(2) -0.00221(14) 0.08179(11) 0.0346(4) Uani 1 1 d . A 1 H19A H 0.2757 0.0445 0.1142 0.052 Uiso 1 1 calc R A 1 H19B H 0.3095 0.0001 0.0348 0.052 Uiso 1 1 calc R A 1 H19C H 0.4354 0.0148 0.0682 0.052 Uiso 1 1 calc R A 1 C20 C 0.4682(2) -0.17750(14) 0.06667(11) 0.0345(4) Uani 1 1 d . A 1 H20A H 0.4954 -0.2446 0.0923 0.052 Uiso 1 1 calc R A 1 H20B H 0.5537 -0.1561 0.0446 0.052 Uiso 1 1 calc R A 1 H20C H 0.4169 -0.1748 0.0256 0.052 Uiso 1 1 calc R A 1 C21 C 0.82410(17) -0.25556(13) 0.24783(10) 0.0264(4) Uani 1 1 d . A 1 C22 C 0.8956(2) -0.19976(15) 0.28669(12) 0.0380(5) Uani 1 1 d . A 1 H22A H 0.8832 -0.1329 0.2604 0.057 Uiso 1 1 calc R A 1 H22B H 0.9972 -0.2336 0.2830 0.057 Uiso 1 1 calc R A 1 H22C H 0.8510 -0.1979 0.3409 0.057 Uiso 1 1 calc R A 1 C23 C 0.8988(2) -0.25750(15) 0.16195(11) 0.0379(5) Uani 1 1 d . A 1 H23A H 0.8597 -0.2952 0.1370 0.057 Uiso 1 1 calc R A 1 H23B H 1.0011 -0.2880 0.1594 0.057 Uiso 1 1 calc R A 1 H23C H 0.8826 -0.1906 0.1355 0.057 Uiso 1 1 calc R A 1 C24 C 0.8473(2) -0.36307(14) 0.28806(12) 0.0364(4) Uani 1 1 d . A 1 H24A H 0.8063 -0.3986 0.2622 0.055 Uiso 1 1 calc R A 1 H24B H 0.8009 -0.3630 0.3421 0.055 Uiso 1 1 calc R A 1 H24C H 0.9494 -0.3950 0.2851 0.055 Uiso 1 1 calc R A 1 C25 C 0.34805(19) -0.14164(13) 0.42867(10) 0.0297(4) Uani 1 1 d . A 1 C26 C 0.4416(2) -0.20941(17) 0.48743(11) 0.0462(6) Uani 1 1 d . A 1 H26A H 0.3844 -0.2101 0.5392 0.069 Uiso 1 1 calc R A 1 H26B H 0.5223 -0.1847 0.4865 0.069 Uiso 1 1 calc R A 1 H26C H 0.4768 -0.2759 0.4734 0.069 Uiso 1 1 calc R A 1 C27 C 0.2234(2) -0.18717(15) 0.43433(12) 0.0385(5) Uani 1 1 d . A 1 H27A H 0.1649 -0.1509 0.3957 0.058 Uiso 1 1 calc R A 1 H27B H 0.1649 -0.1835 0.4857 0.058 Uiso 1 1 calc R A 1 H27C H 0.2625 -0.2556 0.4251 0.058 Uiso 1 1 calc R A 1 C28 C 0.2934(2) -0.03784(14) 0.45609(11) 0.0365(4) Uani 1 1 d . A 1 H28A H 0.2418 0.0090 0.4182 0.055 Uiso 1 1 calc R A 1 H28B H 0.3745 -0.0172 0.4613 0.055 Uiso 1 1 calc R A 1 H28C H 0.2297 -0.0404 0.5059 0.055 Uiso 1 1 calc R A 1 C29 C 0.17183(17) 0.32866(12) 0.27093(10) 0.0232(3) Uani 1 1 d . A 1 C30 C 0.21847(18) 0.38294(12) 0.19813(10) 0.0261(4) Uani 1 1 d . A 1 C31 C 0.31678(19) 0.43668(13) 0.19569(11) 0.0300(4) Uani 1 1 d . A 1 H31A H 0.3506 0.4689 0.1475 0.036 Uiso 1 1 calc R A 1 C32 C 0.36622(19) 0.44437(12) 0.26081(11) 0.0298(4) Uani 1 1 d . A 1 C33 C 0.30104(19) 0.40464(13) 0.33270(11) 0.0293(4) Uani 1 1 d . A 1 H33A H 0.3251 0.4149 0.3780 0.035 Uiso 1 1 calc R A 1 C34 C 0.20200(18) 0.35047(12) 0.34082(10) 0.0245(4) Uani 1 1 d . A 1 C35 C 0.1572(2) 0.39465(14) 0.12155(10) 0.0331(4) Uani 1 1 d . A 1 C36 C 0.2316(2) 0.30850(17) 0.07272(12) 0.0459(5) Uani 1 1 d . A 1 H36A H 0.1942 0.3228 0.0247 0.069 Uiso 1 1 calc R A 1 H36B H 0.2131 0.2483 0.1018 0.069 Uiso 1 1 calc R A 1 H36C H 0.3342 0.3003 0.0610 0.069 Uiso 1 1 calc R A 1 C37 C 0.1785(3) 0.49039(18) 0.06745(13) 0.0559(6) Uani 1 1 d . A 1 H37A H 0.1251 0.5036 0.0254 0.084 Uiso 1 1 calc R A 1 H37B H 0.2797 0.4810 0.0462 0.084 Uiso 1 1 calc R A 1 H37C H 0.1439 0.5457 0.0973 0.084 Uiso 1 1 calc R A 1 C38 C -0.0078(2) 0.41227(15) 0.14053(12) 0.0394(5) Uani 1 1 d . A 1 H38A H -0.0455 0.4274 0.0926 0.059 Uiso 1 1 calc R A 1 H38B H -0.0512 0.4671 0.1708 0.059 Uiso 1 1 calc R A 1 H38C H -0.0299 0.3533 0.1702 0.059 Uiso 1 1 calc R A 1 C39 C 0.4776(2) 0.50067(14) 0.25830(13) 0.0382(5) Uani 1 1 d . A 1 C40 C 0.6013(2) 0.43133(18) 0.29841(15) 0.0536(6) Uani 1 1 d . A 1 H40A H 0.5637 0.4117 0.3522 0.080 Uiso 1 1 calc R A 1 H40B H 0.6724 0.4655 0.2963 0.080 Uiso 1 1 calc R A 1 H40C H 0.6455 0.3732 0.2719 0.080 Uiso 1 1 calc R A 1 C41 C 0.5420(3) 0.53538(18) 0.17440(15) 0.0569(6) Uani 1 1 d . A 1 H41A H 0.5898 0.4786 0.1467 0.085 Uiso 1 1 calc R A 1 H41B H 0.6108 0.5701 0.1756 0.085 Uiso 1 1 calc R A 1 H41C H 0.4658 0.5793 0.1482 0.085 Uiso 1 1 calc R A 1 C42 C 0.4032(3) 0.59246(17) 0.30151(17) 0.0621(7) Uani 1 1 d . A 1 H42A H 0.3685 0.5715 0.3555 0.093 Uiso 1 1 calc R A 1 H42B H 0.3231 0.6342 0.2773 0.093 Uiso 1 1 calc R A 1 H42C H 0.4715 0.6291 0.2988 0.093 Uiso 1 1 calc R A 1 C43 C 0.11887(19) 0.32806(13) 0.42446(10) 0.0275(4) Uani 1 1 d . A 1 C44 C 0.1536(2) 0.37761(15) 0.48529(11) 0.0369(4) Uani 1 1 d . A 1 H44A H 0.0919 0.3679 0.5349 0.055 Uiso 1 1 calc R A 1 H44B H 0.1375 0.4477 0.4680 0.055 Uiso 1 1 calc R A 1 H44C H 0.2532 0.3482 0.4911 0.055 Uiso 1 1 calc R A 1 C45 C -0.04398(19) 0.37708(13) 0.42305(11) 0.0313(4) Uani 1 1 d . A 1 H45A H -0.0993 0.3617 0.4736 0.047 Uiso 1 1 calc R A 1 H45B H -0.0723 0.3520 0.3839 0.047 Uiso 1 1 calc R A 1 H45C H -0.0617 0.4480 0.4109 0.047 Uiso 1 1 calc R A 1 C46 C 0.1534(2) 0.21656(13) 0.45509(10) 0.0314(4) Uani 1 1 d . A 1 H46A H 0.0875 0.2063 0.5029 0.047 Uiso 1 1 calc R A 1 H46B H 0.2511 0.1929 0.4650 0.047 Uiso 1 1 calc R A 1 H46C H 0.1434 0.1807 0.4166 0.047 Uiso 1 1 calc R A 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 N1' 0.025(14) 0.019(11) 0.07(3) -0.034(17) -0.032(19) 0.016(9) P1' 0.047(4) 0.029(3) 0.031(6) -0.002(3) 0.003(3) -0.009(3) P2' 0.053(5) 0.043(4) 0.056(8) -0.014(5) -0.005(5) -0.010(3) P1 0.0194(2) 0.0215(2) 0.0231(4) -0.0060(2) -0.0020(2) -0.00510(18) P2 0.0217(2) 0.0205(2) 0.0217(4) -0.0033(2) -0.0060(2) -0.00419(18) O1 0.0661(11) 0.0428(10) 0.0742(12) 0.0027(9) 0.0074(9) -0.0007(8) N1 0.0168(9) 0.0195(14) 0.0293(15) -0.0070(10) -0.0035(10) -0.0046(9) N2 0.0273(8) 0.0338(8) 0.0371(9) -0.0018(7) 0.0017(7) -0.0100(7) C1 0.0281(9) 0.0302(9) 0.0393(11) -0.0047(8) -0.0052(8) -0.0117(8) C2 0.0194(8) 0.0350(10) 0.0374(10) -0.0093(8) -0.0032(7) -0.0091(7) C3 0.0217(8) 0.0325(10) 0.0367(10) -0.0085(8) -0.0070(7) -0.0014(7) C4 0.0198(8) 0.0229(8) 0.0315(9) -0.0036(7) -0.0064(7) -0.0060(6) C5 0.0256(8) 0.0295(9) 0.0305(10) -0.0034(7) -0.0051(7) -0.0083(7) C6 0.0263(9) 0.0585(13) 0.0340(11) 0.0030(9) -0.0011(8) -0.0138(9) C7 0.0518(13) 0.0357(11) 0.0508(13) -0.0054(10) -0.0014(10) -0.0169(10) C8 0.0594(14) 0.0458(13) 0.0420(12) -0.0032(10) -0.0028(10) -0.0304(11) C9 0.0344(10) 0.0600(14) 0.0384(12) -0.0077(10) 0.0032(9) -0.0161(10) C10 0.0325(10) 0.0346(11) 0.0369(11) -0.0035(8) -0.0044(8) -0.0023(8) C11 0.0217(8) 0.0201(8) 0.0258(9) -0.0046(6) -0.0006(7) -0.0079(6) C12 0.0252(8) 0.0178(8) 0.0246(9) -0.0023(6) -0.0019(7) -0.0083(6) C13 0.0262(8) 0.0236(8) 0.0219(8) -0.0039(7) 0.0005(7) -0.0066(7) C14 0.0228(8) 0.0199(8) 0.0289(9) -0.0032(7) -0.0012(7) -0.0068(6) C15 0.0281(8) 0.0247(8) 0.0227(9) -0.0002(7) -0.0052(7) -0.0061(7) C16 0.0261(8) 0.0220(8) 0.0256(9) -0.0043(7) 0.0000(7) -0.0084(7) C17 0.0277(8) 0.0252(9) 0.0253(9) -0.0066(7) -0.0026(7) -0.0059(7) C18 0.0342(10) 0.0407(11) 0.0361(11) -0.0126(9) -0.0047(8) -0.0155(8) C19 0.0422(11) 0.0306(10) 0.0296(10) -0.0009(8) -0.0103(8) -0.0075(8) C20 0.0401(10) 0.0363(10) 0.0259(9) -0.0105(8) -0.0038(8) -0.0069(8) C21 0.0209(8) 0.0264(9) 0.0295(9) -0.0031(7) -0.0018(7) -0.0054(7) C22 0.0284(9) 0.0402(11) 0.0475(12) -0.0102(9) -0.0047(9) -0.0116(8) C23 0.0264(9) 0.0410(11) 0.0386(11) -0.0071(9) 0.0029(8) -0.0035(8) C24 0.0313(9) 0.0282(10) 0.0438(11) -0.0023(8) -0.0041(8) -0.0033(8) C25 0.0294(9) 0.0298(9) 0.0239(9) -0.0022(7) -0.0005(7) -0.0036(7) C26 0.0421(11) 0.0550(13) 0.0250(10) 0.0024(9) 0.0016(9) 0.0003(10) C27 0.0396(11) 0.0347(10) 0.0351(11) 0.0040(8) 0.0040(9) -0.0142(9) C28 0.0404(11) 0.0385(11) 0.0266(10) -0.0070(8) 0.0022(8) -0.0095(9) C29 0.0225(8) 0.0196(8) 0.0259(9) -0.0047(6) -0.0066(7) -0.0010(6) C30 0.0276(8) 0.0215(8) 0.0258(9) -0.0038(7) -0.0042(7) -0.0018(7) C31 0.0333(9) 0.0233(9) 0.0310(10) 0.0010(7) -0.0037(8) -0.0085(7) C32 0.0303(9) 0.0192(8) 0.0404(11) -0.0049(7) -0.0084(8) -0.0057(7) C33 0.0338(9) 0.0255(9) 0.0318(10) -0.0074(7) -0.0110(8) -0.0072(7) C34 0.0259(8) 0.0204(8) 0.0257(9) -0.0037(7) -0.0074(7) -0.0022(7) C35 0.0429(11) 0.0310(10) 0.0250(9) 0.0006(7) -0.0098(8) -0.0097(8) C36 0.0548(13) 0.0523(13) 0.0281(11) -0.0138(9) -0.0064(9) -0.0071(11) C37 0.0792(17) 0.0558(14) 0.0368(12) 0.0156(11) -0.0255(12) -0.0267(13) C38 0.0422(11) 0.0361(11) 0.0370(11) -0.0032(9) -0.0199(9) 0.0012(9) C39 0.0372(10) 0.0285(10) 0.0532(13) -0.0051(9) -0.0097(9) -0.0144(8) C40 0.0430(12) 0.0490(13) 0.0766(17) -0.0007(12) -0.0211(12) -0.0209(11) C41 0.0587(15) 0.0517(14) 0.0674(16) 0.0048(12) -0.0070(12) -0.0358(12) C42 0.0637(16) 0.0352(12) 0.095(2) -0.0209(13) -0.0073(14) -0.0216(11) C43 0.0321(9) 0.0267(9) 0.0231(9) -0.0045(7) -0.0061(7) -0.0058(7) C44 0.0448(11) 0.0399(11) 0.0292(10) -0.0115(8) -0.0079(8) -0.0114(9) C45 0.0322(9) 0.0283(9) 0.0299(10) -0.0081(7) -0.0016(8) -0.0037(7) C46 0.0373(10) 0.0300(9) 0.0242(9) -0.0026(7) -0.0056(8) -0.0058(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 N1' P1' 1.59(5) . ? N1' P2' 1.78(4) . ? P1 N1 1.779(3) . ? P1 C1 1.8438(19) . ? P1 C11 1.8679(17) . ? P2 N1 1.766(4) . ? P2 C3 1.8554(19) . ? P2 C29 1.8767(18) . ? O1 C10 1.205(2) . ? N1 C4 1.469(4) . ? N2 C10 1.355(2) . ? N2 C7 1.443(3) . ? N2 C6 1.451(2) . ? C1 C2 1.543(2) . ? C2 C3 1.533(3) . ? C4 C5 1.526(2) . ? C5 C6 1.515(2) . ? C7 C8 1.519(3) . ? C8 C9 1.506(3) . ? C9 C10 1.506(3) . ? C11 C12 1.430(2) . ? C11 C16 1.436(2) . ? C12 C13 1.404(2) . ? C12 C17 1.561(2) . ? C13 C14 1.383(2) . ? C14 C15 1.388(2) . ? C14 C21 1.532(2) . ? C15 C16 1.391(2) . ? C16 C25 1.547(2) . ? C17 C18 1.537(2) . ? C17 C19 1.541(2) . ? C17 C20 1.543(2) . ? C21 C23 1.529(2) . ? C21 C24 1.531(2) . ? C21 C22 1.536(3) . ? C25 C26 1.534(3) . ? C25 C27 1.534(3) . ? C25 C28 1.536(3) . ? C29 C30 1.428(2) . ? C29 C34 1.437(2) . ? C30 C31 1.398(2) . ? C30 C35 1.559(2) . ? C31 C32 1.377(3) . ? C32 C33 1.390(3) . ? C32 C39 1.535(3) . ? C33 C34 1.389(2) . ? C34 C43 1.547(2) . ? C35 C36 1.528(3) . ? C35 C38 1.534(3) . ? C35 C37 1.553(3) . ? C39 C41 1.528(3) . ? C39 C40 1.528(3) . ? C39 C42 1.533(3) . ? C43 C46 1.533(2) . ? C43 C44 1.536(2) . ? C43 C45 1.542(2) . ? 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 P1' N1' P2' 110(3) . . ? N1 P1 C1 97.83(13) . . ? N1 P1 C11 105.26(14) . . ? C1 P1 C11 115.83(8) . . ? N1 P2 C3 97.55(13) . . ? N1 P2 C29 104.34(12) . . ? C3 P2 C29 113.28(8) . . ? C4 N1 P2 119.4(2) . . ? C4 N1 P1 119.5(2) . . ? P2 N1 P1 102.73(19) . . ? C10 N2 C7 112.95(16) . . ? C10 N2 C6 122.83(17) . . ? C7 N2 C6 122.00(17) . . ? C2 C1 P1 105.78(12) . . ? C3 C2 C1 113.29(14) . . ? C2 C3 P2 109.58(12) . . ? N1 C4 C5 118.72(18) . . ? C6 C5 C4 108.96(14) . . ? N2 C6 C5 115.13(16) . . ? N2 C7 C8 104.00(16) . . ? C9 C8 C7 103.87(17) . . ? C10 C9 C8 104.56(16) . . ? O1 C10 N2 126.09(19) . . ? O1 C10 C9 125.87(19) . . ? N2 C10 C9 107.86(17) . . ? C12 C11 C16 117.90(14) . . ? C12 C11 P1 109.81(12) . . ? C16 C11 P1 130.99(12) . . ? C13 C12 C11 118.38(15) . . ? C13 C12 C17 116.54(14) . . ? C11 C12 C17 124.90(14) . . ? C14 C13 C12 123.19(15) . . ? C13 C14 C15 116.82(15) . . ? C13 C14 C21 123.05(15) . . ? C15 C14 C21 120.00(15) . . ? C14 C15 C16 123.46(16) . . ? C15 C16 C11 118.51(15) . . ? C15 C16 C25 117.63(15) . . ? C11 C16 C25 123.62(14) . . ? C18 C17 C19 111.61(15) . . ? C18 C17 C20 104.94(15) . . ? C19 C17 C20 104.96(14) . . ? C18 C17 C12 110.19(14) . . ? C19 C17 C12 113.75(14) . . ? C20 C17 C12 110.93(14) . . ? C23 C21 C24 108.56(15) . . ? C23 C21 C14 112.44(14) . . ? C24 C21 C14 109.12(14) . . ? C23 C21 C22 107.77(15) . . ? C24 C21 C22 109.63(15) . . ? C14 C21 C22 109.29(14) . . ? C26 C25 C27 105.50(16) . . ? C26 C25 C28 106.32(16) . . ? C27 C25 C28 111.85(15) . . ? C26 C25 C16 112.78(14) . . ? C27 C25 C16 108.18(15) . . ? C28 C25 C16 112.06(14) . . ? C30 C29 C34 117.36(15) . . ? C30 C29 P2 111.34(12) . . ? C34 C29 P2 129.94(13) . . ? C31 C30 C29 118.78(16) . . ? C31 C30 C35 116.52(15) . . ? C29 C30 C35 124.47(16) . . ? C32 C31 C30 123.47(17) . . ? C31 C32 C33 116.35(17) . . ? C31 C32 C39 123.82(17) . . ? C33 C32 C39 119.64(17) . . ? C34 C33 C32 123.82(17) . . ? C33 C34 C29 118.29(15) . . ? C33 C34 C43 117.15(15) . . ? C29 C34 C43 124.18(15) . . ? C36 C35 C38 111.58(17) . . ? C36 C35 C37 106.19(17) . . ? C38 C35 C37 104.30(17) . . ? C36 C35 C30 113.74(15) . . ? C38 C35 C30 110.38(15) . . ? C37 C35 C30 110.14(16) . . ? C41 C39 C40 108.20(18) . . ? C41 C39 C42 108.46(19) . . ? C40 C39 C42 109.99(19) . . ? C41 C39 C32 112.29(17) . . ? C40 C39 C32 108.85(16) . . ? C42 C39 C32 109.04(17) . . ? C46 C43 C44 105.81(14) . . ? C46 C43 C45 112.89(15) . . ? C44 C43 C45 104.93(14) . . ? C46 C43 C34 113.25(14) . . ? C44 C43 C34 112.47(15) . . ? C45 C43 C34 107.26(13) . . ? 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 C3 P2 N1 C4 -151.86(19) . . . . ? C29 P2 N1 C4 -35.4(2) . . . . ? C3 P2 N1 P1 73.11(15) . . . . ? C29 P2 N1 P1 -170.44(12) . . . . ? C1 P1 N1 C4 147.9(2) . . . . ? C11 P1 N1 C4 28.3(3) . . . . ? C1 P1 N1 P2 -77.11(16) . . . . ? C11 P1 N1 P2 163.32(12) . . . . ? N1 P1 C1 C2 70.12(18) . . . . ? C11 P1 C1 C2 -178.67(11) . . . . ? P1 C1 C2 C3 -68.30(17) . . . . ? C1 C2 C3 P2 66.76(18) . . . . ? N1 P2 C3 C2 -65.38(16) . . . . ? C29 P2 C3 C2 -174.59(12) . . . . ? P2 N1 C4 C5 -58.1(3) . . . . ? P1 N1 C4 C5 69.5(3) . . . . ? N1 C4 C5 C6 -175.2(2) . . . . ? C10 N2 C6 C5 -114.6(2) . . . . ? C7 N2 C6 C5 83.5(2) . . . . ? C4 C5 C6 N2 -172.35(16) . . . . ? C10 N2 C7 C8 16.8(2) . . . . ? C6 N2 C7 C8 -179.71(17) . . . . ? N2 C7 C8 C9 -25.0(2) . . . . ? C7 C8 C9 C10 24.4(2) . . . . ? C7 N2 C10 O1 174.2(2) . . . . ? C6 N2 C10 O1 10.9(3) . . . . ? C7 N2 C10 C9 -1.2(2) . . . . ? C6 N2 C10 C9 -164.50(17) . . . . ? C8 C9 C10 O1 169.5(2) . . . . ? C8 C9 C10 N2 -15.1(2) . . . . ? N1 P1 C11 C12 -112.81(16) . . . . ? C1 P1 C11 C12 140.39(12) . . . . ? N1 P1 C11 C16 53.6(2) . . . . ? C1 P1 C11 C16 -53.21(18) . . . . ? C16 C11 C12 C13 -13.6(2) . . . . ? P1 C11 C12 C13 154.80(13) . . . . ? C16 C11 C12 C17 161.40(15) . . . . ? P1 C11 C12 C17 -30.18(19) . . . . ? C11 C12 C13 C14 4.1(2) . . . . ? C17 C12 C13 C14 -171.34(15) . . . . ? C12 C13 C14 C15 6.5(3) . . . . ? C12 C13 C14 C21 -177.64(15) . . . . ? C13 C14 C15 C16 -7.6(3) . . . . ? C21 C14 C15 C16 176.44(16) . . . . ? C14 C15 C16 C11 -2.0(3) . . . . ? C14 C15 C16 C25 172.54(16) . . . . ? C12 C11 C16 C15 12.7(2) . . . . ? P1 C11 C16 C15 -152.84(14) . . . . ? C12 C11 C16 C25 -161.56(15) . . . . ? P1 C11 C16 C25 32.9(2) . . . . ? C13 C12 C17 C18 131.07(16) . . . . ? C11 C12 C17 C18 -44.0(2) . . . . ? C13 C12 C17 C19 -102.75(17) . . . . ? C11 C12 C17 C19 82.2(2) . . . . ? C13 C12 C17 C20 15.3(2) . . . . ? C11 C12 C17 C20 -159.79(16) . . . . ? C13 C14 C21 C23 7.8(2) . . . . ? C15 C14 C21 C23 -176.47(16) . . . . ? C13 C14 C21 C24 -112.72(18) . . . . ? C15 C14 C21 C24 63.0(2) . . . . ? C13 C14 C21 C22 127.41(18) . . . . ? C15 C14 C21 C22 -56.8(2) . . . . ? C15 C16 C25 C26 -4.8(2) . . . . ? C11 C16 C25 C26 169.50(17) . . . . ? C15 C16 C25 C27 -121.08(17) . . . . ? C11 C16 C25 C27 53.2(2) . . . . ? C15 C16 C25 C28 115.16(18) . . . . ? C11 C16 C25 C28 -70.6(2) . . . . ? N1 P2 C29 C30 116.32(15) . . . . ? C3 P2 C29 C30 -138.75(12) . . . . ? N1 P2 C29 C34 -49.73(19) . . . . ? C3 P2 C29 C34 55.21(17) . . . . ? C34 C29 C30 C31 14.0(2) . . . . ? P2 C29 C30 C31 -154.02(13) . . . . ? C34 C29 C30 C35 -160.39(15) . . . . ? P2 C29 C30 C35 31.6(2) . . . . ? C29 C30 C31 C32 -3.3(3) . . . . ? C35 C30 C31 C32 171.46(16) . . . . ? C30 C31 C32 C33 -7.0(3) . . . . ? C30 C31 C32 C39 178.14(16) . . . . ? C31 C32 C33 C34 6.6(3) . . . . ? C39 C32 C33 C34 -178.32(16) . . . . ? C32 C33 C34 C29 4.1(2) . . . . ? C32 C33 C34 C43 -169.16(16) . . . . ? C30 C29 C34 C33 -14.3(2) . . . . ? P2 C29 C34 C33 151.06(14) . . . . ? C30 C29 C34 C43 158.47(15) . . . . ? P2 C29 C34 C43 -36.2(2) . . . . ? C31 C30 C35 C36 100.07(19) . . . . ? C29 C30 C35 C36 -85.5(2) . . . . ? C31 C30 C35 C38 -133.63(17) . . . . ? C29 C30 C35 C38 40.8(2) . . . . ? C31 C30 C35 C37 -19.0(2) . . . . ? C29 C30 C35 C37 155.48(18) . . . . ? C31 C32 C39 C41 -7.5(3) . . . . ? C33 C32 C39 C41 177.75(18) . . . . ? C31 C32 C39 C40 -127.3(2) . . . . ? C33 C32 C39 C40 58.0(2) . . . . ? C31 C32 C39 C42 112.7(2) . . . . ? C33 C32 C39 C42 -62.0(2) . . . . ? C33 C34 C43 C46 -115.73(17) . . . . ? C29 C34 C43 C46 71.4(2) . . . . ? C33 C34 C43 C44 4.2(2) . . . . ? C29 C34 C43 C44 -168.66(15) . . . . ? C33 C34 C43 C45 119.05(16) . . . . ? C29 C34 C43 C45 -53.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.10 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.573 _refine_diff_density_min -0.262 _refine_diff_density_rms 0.051 #===END data_06033 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H77 Br Cl2 N2 P2' _chemical_formula_weight 882.86 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' 'Br' 'Br' -0.2901 2.4595 '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' 'N' 'N' 0.0061 0.0033 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.6830(16) _cell_length_b 9.1194(7) _cell_length_c 27.150(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.0550(10) _cell_angle_gamma 90.00 _cell_volume 4967.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelpiped _exptl_crystal_colour colourless _exptl_crystal_size_min 0.130 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_max 0.220 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.180 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 1.031 _exptl_absorpt_correction_type none _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 'Bruker P4' _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 62932 _diffrn_reflns_av_R_equivalents 0.1154 _diffrn_reflns_av_sigmaI/netI 0.1143 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 28.31 _reflns_number_total 12315 _reflns_number_gt 6482 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 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^)+(0.0585P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12315 _refine_ls_number_parameters 513 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1106 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1317 _refine_ls_wR_factor_gt 0.1160 _refine_ls_goodness_of_fit_ref 0.880 _refine_ls_restrained_S_all 0.880 _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 P1 P 0.19506(4) -0.04019(9) 0.25550(3) 0.0317(2) Uani 1 1 d . . . P2 P 0.30628(4) 0.28901(8) 0.12383(3) 0.02314(17) Uani 1 1 d . . . N7 N 0.37057(13) 0.6065(3) 0.18502(9) 0.0349(6) Uani 1 1 d . . . N12 N 0.39196(13) 0.4131(3) 0.24166(9) 0.0332(6) Uani 1 1 d . . . C1 C 0.25535(16) 0.0542(3) 0.23945(12) 0.0306(7) Uani 1 1 d . . . C2 C 0.25439(14) 0.1691(3) 0.20042(11) 0.0298(7) Uani 1 1 d . . . H2A H 0.2660 0.2629 0.2171 0.036 Uiso 1 1 calc R . . H2B H 0.2097 0.1771 0.1788 0.036 Uiso 1 1 calc R . . C3 C 0.30328(13) 0.1344(3) 0.16758(10) 0.0257(6) Uani 1 1 d . . . H3A H 0.2892 0.0459 0.1481 0.031 Uiso 1 1 calc R . . H3B H 0.3474 0.1176 0.1892 0.031 Uiso 1 1 calc R . . C4 C 0.38869(14) 0.3835(3) 0.14996(10) 0.0247(6) Uani 1 1 d . . . H4A H 0.4261 0.3143 0.1568 0.030 Uiso 1 1 calc R . . C5 C 0.39822(16) 0.5078(3) 0.11371(12) 0.0374(8) Uani 1 1 d . . . H5A H 0.4451 0.5218 0.1150 0.045 Uiso 1 1 calc R . . H5B H 0.3747 0.4857 0.0790 0.045 Uiso 1 1 calc R . . C6 C 0.36948(19) 0.6418(4) 0.13276(13) 0.0508(10) Uani 1 1 d . . . H6A H 0.3965 0.7276 0.1309 0.061 Uiso 1 1 calc R . . H6B H 0.3243 0.6598 0.1132 0.061 Uiso 1 1 calc R . . C8 C 0.38480(13) 0.4679(3) 0.19588(11) 0.0259(6) Uani 1 1 d . . . C9 C 0.3673(2) 0.7181(4) 0.22304(14) 0.0550(11) Uani 1 1 d . . . H9A H 0.4078 0.7761 0.2304 0.066 Uiso 1 1 calc R . . H9B H 0.3299 0.7832 0.2101 0.066 Uiso 1 1 calc R . . C10 C 0.3594(3) 0.6480(5) 0.26872(18) 0.1000(19) Uani 1 1 d . . . H10A H 0.3740 0.7171 0.2964 0.120 Uiso 1 1 calc R . . H10B H 0.3121 0.6321 0.2650 0.120 Uiso 1 1 calc R . . C11 C 0.3926(2) 0.5116(4) 0.28422(13) 0.0572(11) Uani 1 1 d . . . H11A H 0.3712 0.4632 0.3078 0.069 Uiso 1 1 calc R . . H11B H 0.4385 0.5313 0.3019 0.069 Uiso 1 1 calc R . . C13 C 0.11860(13) 0.0274(3) 0.21031(11) 0.0251(6) Uani 1 1 d . . . C14 C 0.08669(14) 0.1587(3) 0.22031(11) 0.0255(6) Uani 1 1 d . . . C15 C 0.03628(14) 0.2165(3) 0.18170(11) 0.0288(7) Uani 1 1 d . . . H15A H 0.0166 0.3043 0.1877 0.035 Uiso 1 1 calc R . . C16 C 0.01376(14) 0.1499(3) 0.13467(11) 0.0291(7) Uani 1 1 d . . . C17 C 0.04168(14) 0.0172(3) 0.12764(11) 0.0288(7) Uani 1 1 d . . . H17A H 0.0256 -0.0310 0.0969 0.035 Uiso 1 1 calc R . . C18 C 0.09254(14) -0.0492(3) 0.16377(11) 0.0257(6) Uani 1 1 d . . . C19 C 0.10188(15) 0.2396(3) 0.27269(11) 0.0325(7) Uani 1 1 d . . . C20 C 0.09993(17) 0.1291(4) 0.31522(12) 0.0431(8) Uani 1 1 d . . . H20A H 0.0578 0.0792 0.3075 0.065 Uiso 1 1 calc R . . H20B H 0.1056 0.1803 0.3469 0.065 Uiso 1 1 calc R . . H20C H 0.1352 0.0590 0.3178 0.065 Uiso 1 1 calc R . . C21 C 0.16900(15) 0.3211(3) 0.28422(12) 0.0393(8) Uani 1 1 d . . . H21A H 0.1704 0.3853 0.2565 0.059 Uiso 1 1 calc R . . H21B H 0.2047 0.2513 0.2886 0.059 Uiso 1 1 calc R . . H21C H 0.1738 0.3776 0.3147 0.059 Uiso 1 1 calc R . . C22 C 0.04937(16) 0.3560(4) 0.27489(13) 0.0448(9) Uani 1 1 d . . . H22A H 0.0515 0.4331 0.2513 0.067 Uiso 1 1 calc R . . H22B H 0.0578 0.3958 0.3086 0.067 Uiso 1 1 calc R . . H22C H 0.0059 0.3122 0.2662 0.067 Uiso 1 1 calc R . . C23 C -0.04215(15) 0.2219(3) 0.09434(12) 0.0367(8) Uani 1 1 d . . . C24 C -0.02003(18) 0.3752(4) 0.08260(15) 0.0556(10) Uani 1 1 d . . . H24A H 0.0190 0.3678 0.0695 0.083 Uiso 1 1 calc R . . H24B H -0.0100 0.4328 0.1131 0.083 Uiso 1 1 calc R . . H24C H -0.0552 0.4214 0.0578 0.083 Uiso 1 1 calc R . . C25 C -0.10426(17) 0.2360(4) 0.11563(15) 0.0599(11) Uani 1 1 d . . . H25A H -0.1187 0.1402 0.1230 0.090 Uiso 1 1 calc R . . H25B H -0.1393 0.2832 0.0910 0.090 Uiso 1 1 calc R . . H25C H -0.0936 0.2933 0.1462 0.090 Uiso 1 1 calc R . . C26 C -0.05989(19) 0.1352(4) 0.04474(13) 0.0572(11) Uani 1 1 d . . . H26A H -0.0782 0.0419 0.0506 0.086 Uiso 1 1 calc R . . H26B H -0.0205 0.1203 0.0326 0.086 Uiso 1 1 calc R . . H26C H -0.0921 0.1888 0.0199 0.086 Uiso 1 1 calc R . . C27 C 0.11644(14) -0.2023(3) 0.15048(12) 0.0306(7) Uani 1 1 d . . . C28 C 0.12038(18) -0.3135(3) 0.19335(14) 0.0501(10) Uani 1 1 d . . . H28A H 0.1543 -0.2838 0.2225 0.075 Uiso 1 1 calc R . . H28B H 0.1312 -0.4084 0.1823 0.075 Uiso 1 1 calc R . . H28C H 0.0782 -0.3180 0.2021 0.075 Uiso 1 1 calc R . . C29 C 0.06754(18) -0.2697(4) 0.10369(14) 0.0516(10) Uani 1 1 d . . . H29A H 0.0233 -0.2692 0.1089 0.077 Uiso 1 1 calc R . . H29B H 0.0806 -0.3687 0.0990 0.077 Uiso 1 1 calc R . . H29C H 0.0684 -0.2130 0.0741 0.077 Uiso 1 1 calc R . . C30 C 0.18434(16) -0.1924(3) 0.13707(14) 0.0437(9) Uani 1 1 d . . . H30A H 0.2170 -0.1549 0.1657 0.066 Uiso 1 1 calc R . . H30B H 0.1809 -0.1280 0.1086 0.066 Uiso 1 1 calc R . . H30C H 0.1976 -0.2882 0.1286 0.066 Uiso 1 1 calc R . . C31 C 0.31725(13) 0.2317(3) 0.06051(10) 0.0221(6) Uani 1 1 d . . . C32 C 0.37847(13) 0.1924(3) 0.04820(10) 0.0228(6) Uani 1 1 d . . . C33 C 0.38859(14) 0.2396(3) 0.00179(11) 0.0277(7) Uani 1 1 d . . . H33A H 0.4290 0.2164 -0.0057 0.033 Uiso 1 1 calc R . . C34 C 0.34253(14) 0.3185(3) -0.03385(11) 0.0268(7) Uani 1 1 d . . . C35 C 0.27993(14) 0.3329(3) -0.02462(11) 0.0264(6) Uani 1 1 d . . . H35A H 0.2461 0.3743 -0.0498 0.032 Uiso 1 1 calc R . . C36 C 0.26503(13) 0.2887(3) 0.02031(10) 0.0231(6) Uani 1 1 d . . . C37 C 0.43500(13) 0.0914(3) 0.07827(11) 0.0273(6) Uani 1 1 d . . . C38 C 0.42414(14) 0.0244(3) 0.12713(11) 0.0302(7) Uani 1 1 d . . . H38A H 0.4290 0.0991 0.1527 0.045 Uiso 1 1 calc R . . H38B H 0.4565 -0.0514 0.1386 0.045 Uiso 1 1 calc R . . H38C H 0.3801 -0.0166 0.1208 0.045 Uiso 1 1 calc R . . C39 C 0.50249(14) 0.1716(3) 0.09054(12) 0.0365(8) Uani 1 1 d . . . H39A H 0.5004 0.2543 0.1120 0.055 Uiso 1 1 calc R . . H39B H 0.5123 0.2048 0.0596 0.055 Uiso 1 1 calc R . . H39C H 0.5368 0.1058 0.1077 0.055 Uiso 1 1 calc R . . C40 C 0.43909(16) -0.0413(3) 0.04345(12) 0.0372(8) Uani 1 1 d . . . H40A H 0.4766 -0.1013 0.0591 0.056 Uiso 1 1 calc R . . H40B H 0.4443 -0.0067 0.0112 0.056 Uiso 1 1 calc R . . H40C H 0.3989 -0.0981 0.0385 0.056 Uiso 1 1 calc R . . C41 C 0.36034(15) 0.3767(3) -0.08154(11) 0.0335(7) Uani 1 1 d . . . C42 C 0.4257(2) 0.4584(6) -0.06751(15) 0.0879(17) Uani 1 1 d . . . H42A H 0.4217 0.5400 -0.0461 0.132 Uiso 1 1 calc R . . H42B H 0.4368 0.4933 -0.0978 0.132 Uiso 1 1 calc R . . H42C H 0.4601 0.3937 -0.0497 0.132 Uiso 1 1 calc R . . C43 C 0.3672(2) 0.2489(4) -0.11602(14) 0.0654(12) Uani 1 1 d . . . H43A H 0.3988 0.1795 -0.0974 0.098 Uiso 1 1 calc R . . H43B H 0.3825 0.2846 -0.1445 0.098 Uiso 1 1 calc R . . H43C H 0.3247 0.2019 -0.1279 0.098 Uiso 1 1 calc R . . C44 C 0.3074(2) 0.4776(5) -0.11194(14) 0.0714(13) Uani 1 1 d . . . H44A H 0.3003 0.5576 -0.0909 0.107 Uiso 1 1 calc R . . H44B H 0.2666 0.4241 -0.1237 0.107 Uiso 1 1 calc R . . H44C H 0.3218 0.5152 -0.1405 0.107 Uiso 1 1 calc R . . C45 C 0.19015(14) 0.3013(3) 0.02229(11) 0.0291(7) Uani 1 1 d . . . C46 C 0.17439(16) 0.4520(3) 0.04148(13) 0.0416(8) Uani 1 1 d . . . H46A H 0.1272 0.4602 0.0381 0.062 Uiso 1 1 calc R . . H46B H 0.1886 0.5274 0.0218 0.062 Uiso 1 1 calc R . . H46C H 0.1974 0.4628 0.0765 0.062 Uiso 1 1 calc R . . C47 C 0.17046(15) 0.1783(4) 0.05463(12) 0.0379(8) Uani 1 1 d . . . H47A H 0.1230 0.1788 0.0504 0.057 Uiso 1 1 calc R . . H47B H 0.1921 0.1940 0.0897 0.057 Uiso 1 1 calc R . . H47C H 0.1840 0.0853 0.0439 0.057 Uiso 1 1 calc R . . C48 C 0.14415(15) 0.2835(4) -0.03121(12) 0.0418(8) Uani 1 1 d . . . H48A H 0.0988 0.2740 -0.0287 0.063 Uiso 1 1 calc R . . H48B H 0.1568 0.1974 -0.0469 0.063 Uiso 1 1 calc R . . H48C H 0.1482 0.3681 -0.0513 0.063 Uiso 1 1 calc R . . Cl49 Cl 0.29339(10) 0.61542(16) 0.40606(8) 0.1461(7) Uani 1 1 d . . . Cl51 Cl 0.26348(6) 0.70487(15) 0.49924(5) 0.0995(5) Uani 1 1 d . . . C50 C 0.2669(2) 0.5635(4) 0.45844(18) 0.0783(14) Uani 1 1 d . . . H50A H 0.2968 0.4887 0.4766 0.094 Uiso 1 1 calc R . . H50B H 0.2229 0.5201 0.4474 0.094 Uiso 1 1 calc R . . Br1 Br 0.451899(16) 0.08566(4) 0.279823(13) 0.04053(11) Uani 1 1 d . . . H1 H 0.2980(16) 0.039(3) 0.2556(11) 0.040(9) Uiso 1 1 d . . . H12 H 0.4119(14) 0.325(3) 0.2499(10) 0.027(8) Uiso 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 P1 0.0292(4) 0.0336(4) 0.0338(5) 0.0076(4) 0.0108(4) 0.0011(3) P2 0.0244(4) 0.0231(4) 0.0225(4) -0.0013(3) 0.0069(3) -0.0038(3) N7 0.0466(16) 0.0237(14) 0.0281(14) -0.0046(11) -0.0032(12) 0.0003(12) N12 0.0410(16) 0.0304(14) 0.0267(14) -0.0068(12) 0.0056(12) 0.0040(13) C1 0.0282(18) 0.0363(18) 0.0287(17) 0.0015(14) 0.0098(14) 0.0051(14) C2 0.0297(16) 0.0297(16) 0.0327(18) 0.0015(13) 0.0127(14) 0.0006(13) C3 0.0250(15) 0.0289(15) 0.0248(16) -0.0007(12) 0.0093(13) -0.0040(12) C4 0.0266(15) 0.0243(15) 0.0240(15) -0.0014(12) 0.0077(12) -0.0057(12) C5 0.0440(19) 0.0375(18) 0.0309(18) 0.0027(15) 0.0092(15) -0.0182(15) C6 0.074(3) 0.0285(18) 0.043(2) 0.0069(16) -0.0006(19) -0.0066(18) C8 0.0223(15) 0.0259(15) 0.0277(17) -0.0040(13) 0.0026(13) -0.0028(12) C9 0.066(3) 0.037(2) 0.052(2) -0.0174(19) -0.004(2) 0.0146(18) C10 0.195(6) 0.054(3) 0.070(3) -0.017(3) 0.068(4) 0.026(3) C11 0.078(3) 0.059(2) 0.029(2) -0.0107(18) 0.0031(19) 0.013(2) C13 0.0235(15) 0.0236(14) 0.0310(17) 0.0061(13) 0.0121(13) -0.0021(12) C14 0.0263(16) 0.0270(15) 0.0253(16) -0.0002(13) 0.0103(13) -0.0056(12) C15 0.0306(17) 0.0236(15) 0.0333(17) -0.0017(13) 0.0096(14) -0.0009(13) C16 0.0268(16) 0.0262(15) 0.0336(18) 0.0022(14) 0.0060(14) -0.0033(13) C17 0.0311(17) 0.0274(16) 0.0278(17) -0.0037(13) 0.0070(14) -0.0078(13) C18 0.0284(16) 0.0204(14) 0.0323(17) 0.0013(12) 0.0149(14) -0.0045(12) C19 0.0322(17) 0.0364(17) 0.0316(17) -0.0036(14) 0.0129(14) -0.0011(14) C20 0.049(2) 0.054(2) 0.0287(18) -0.0010(16) 0.0148(16) -0.0042(17) C21 0.0427(19) 0.0384(18) 0.0377(19) -0.0115(15) 0.0116(16) -0.0056(15) C22 0.044(2) 0.049(2) 0.045(2) -0.0131(17) 0.0191(17) 0.0043(17) C23 0.0337(18) 0.0333(17) 0.0374(19) 0.0009(15) -0.0022(15) 0.0012(14) C24 0.056(2) 0.043(2) 0.060(3) 0.0178(19) -0.003(2) 0.0038(18) C25 0.033(2) 0.074(3) 0.066(3) -0.002(2) -0.0025(19) 0.0077(19) C26 0.060(2) 0.056(2) 0.042(2) -0.0057(19) -0.0125(19) 0.011(2) C27 0.0319(17) 0.0195(15) 0.0436(19) -0.0018(14) 0.0156(15) -0.0016(12) C28 0.065(2) 0.0232(17) 0.070(3) 0.0068(17) 0.032(2) 0.0045(16) C29 0.057(2) 0.0327(19) 0.064(3) -0.0192(18) 0.014(2) -0.0047(17) C30 0.046(2) 0.0341(18) 0.059(2) -0.0113(17) 0.0274(18) -0.0004(15) C31 0.0252(15) 0.0177(13) 0.0238(15) -0.0018(12) 0.0065(12) -0.0040(11) C32 0.0237(15) 0.0223(14) 0.0221(15) -0.0035(12) 0.0049(12) -0.0029(12) C33 0.0264(16) 0.0314(16) 0.0272(16) -0.0023(13) 0.0101(13) -0.0015(13) C34 0.0344(17) 0.0234(15) 0.0218(15) -0.0015(12) 0.0053(13) -0.0044(13) C35 0.0292(16) 0.0261(15) 0.0222(15) 0.0006(12) 0.0026(13) 0.0007(12) C36 0.0256(15) 0.0207(14) 0.0235(15) -0.0037(12) 0.0069(12) -0.0028(12) C37 0.0232(15) 0.0295(15) 0.0304(16) 0.0026(14) 0.0089(13) 0.0021(13) C38 0.0322(17) 0.0256(15) 0.0342(17) 0.0075(14) 0.0109(14) 0.0044(13) C39 0.0301(17) 0.0434(19) 0.0378(19) 0.0102(16) 0.0115(15) 0.0018(15) C40 0.0363(18) 0.0344(17) 0.042(2) -0.0014(15) 0.0127(16) 0.0088(14) C41 0.0421(19) 0.0356(18) 0.0252(16) 0.0048(14) 0.0128(14) -0.0043(14) C42 0.084(3) 0.124(4) 0.052(3) 0.024(3) 0.008(2) -0.064(3) C43 0.101(3) 0.063(3) 0.043(2) 0.002(2) 0.040(2) -0.001(2) C44 0.098(3) 0.078(3) 0.043(2) 0.029(2) 0.029(2) 0.024(3) C45 0.0255(16) 0.0309(16) 0.0300(17) -0.0006(14) 0.0048(13) -0.0006(13) C46 0.0373(19) 0.0387(19) 0.049(2) -0.0046(16) 0.0118(17) 0.0111(15) C47 0.0267(17) 0.046(2) 0.040(2) 0.0052(16) 0.0056(15) -0.0062(15) C48 0.0333(18) 0.050(2) 0.0373(19) 0.0015(17) -0.0004(15) 0.0017(16) Cl49 0.217(2) 0.0699(9) 0.1943(18) 0.0106(11) 0.1328(17) 0.0235(11) Cl51 0.0747(8) 0.1020(10) 0.1074(10) -0.0137(8) -0.0057(7) 0.0355(7) C50 0.066(3) 0.058(3) 0.097(4) 0.021(3) -0.006(3) -0.002(2) Br1 0.03796(19) 0.0457(2) 0.03641(19) 0.00423(16) 0.00614(15) 0.00894(16) _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 P1 C1 1.658(3) . ? P1 C13 1.856(3) . ? P2 C3 1.854(3) . ? P2 C31 1.863(3) . ? P2 C4 1.888(3) . ? N7 C8 1.315(3) . ? N7 C6 1.450(4) . ? N7 C9 1.463(4) . ? N12 C8 1.314(4) . ? N12 C11 1.461(4) . ? C1 C2 1.487(4) . ? C2 C3 1.535(4) . ? C4 C8 1.484(4) . ? C4 C5 1.545(4) . ? C5 C6 1.505(5) . ? C9 C10 1.439(6) . ? C10 C11 1.434(6) . ? C13 C14 1.425(4) . ? C13 C18 1.430(4) . ? C14 C15 1.390(4) . ? C14 C19 1.565(4) . ? C15 C16 1.388(4) . ? C16 C17 1.373(4) . ? C16 C23 1.534(4) . ? C17 C18 1.391(4) . ? C18 C27 1.553(4) . ? C19 C22 1.530(4) . ? C19 C20 1.540(4) . ? C19 C21 1.538(4) . ? C23 C24 1.529(4) . ? C23 C26 1.528(4) . ? C23 C25 1.537(5) . ? C27 C28 1.530(4) . ? C27 C30 1.537(4) . ? C27 C29 1.546(4) . ? C31 C32 1.431(4) . ? C31 C36 1.434(4) . ? C32 C33 1.394(4) . ? C32 C37 1.555(4) . ? C33 C34 1.384(4) . ? C34 C35 1.383(4) . ? C34 C41 1.525(4) . ? C35 C36 1.389(4) . ? C36 C45 1.567(4) . ? C37 C38 1.526(4) . ? C37 C39 1.539(4) . ? C37 C40 1.551(4) . ? C41 C42 1.509(5) . ? C41 C44 1.512(5) . ? C41 C43 1.523(4) . ? C45 C46 1.532(4) . ? C45 C47 1.539(4) . ? C45 C48 1.540(4) . ? Cl49 C50 1.710(5) . ? Cl51 C50 1.713(5) . ? 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 C1 P1 C13 103.20(14) . . ? C3 P2 C31 114.11(12) . . ? C3 P2 C4 105.90(12) . . ? C31 P2 C4 99.99(12) . . ? C8 N7 C6 112.5(3) . . ? C8 N7 C9 123.8(3) . . ? C6 N7 C9 123.0(3) . . ? C8 N12 C11 119.4(3) . . ? C2 C1 P1 132.2(2) . . ? C1 C2 C3 111.8(2) . . ? C2 C3 P2 110.16(19) . . ? C8 C4 C5 101.3(2) . . ? C8 C4 P2 108.91(19) . . ? C5 C4 P2 109.80(19) . . ? C6 C5 C4 104.8(3) . . ? N7 C6 C5 104.0(2) . . ? N12 C8 N7 123.0(3) . . ? N12 C8 C4 125.5(3) . . ? N7 C8 C4 111.4(3) . . ? C10 C9 N7 109.5(3) . . ? C11 C10 C9 119.5(4) . . ? C10 C11 N12 112.9(3) . . ? C14 C13 C18 119.1(2) . . ? C14 C13 P1 120.9(2) . . ? C18 C13 P1 120.0(2) . . ? C15 C14 C13 118.2(3) . . ? C15 C14 C19 117.1(2) . . ? C13 C14 C19 124.7(2) . . ? C16 C15 C14 123.4(3) . . ? C17 C16 C15 117.0(3) . . ? C17 C16 C23 123.2(3) . . ? C15 C16 C23 119.7(3) . . ? C16 C17 C18 123.8(3) . . ? C17 C18 C13 117.9(3) . . ? C17 C18 C27 117.2(3) . . ? C13 C18 C27 124.9(3) . . ? C22 C19 C20 106.1(3) . . ? C22 C19 C21 105.7(2) . . ? C20 C19 C21 110.5(3) . . ? C22 C19 C14 112.0(2) . . ? C20 C19 C14 109.7(2) . . ? C21 C19 C14 112.6(2) . . ? C24 C23 C26 108.0(3) . . ? C24 C23 C16 109.2(2) . . ? C26 C23 C16 112.7(3) . . ? C24 C23 C25 108.8(3) . . ? C26 C23 C25 109.3(3) . . ? C16 C23 C25 108.7(3) . . ? C28 C27 C30 109.6(3) . . ? C28 C27 C29 105.4(3) . . ? C30 C27 C29 106.4(3) . . ? C28 C27 C18 112.3(3) . . ? C30 C27 C18 111.3(2) . . ? C29 C27 C18 111.5(2) . . ? C32 C31 C36 117.3(2) . . ? C32 C31 P2 126.8(2) . . ? C36 C31 P2 111.26(19) . . ? C33 C32 C31 118.0(2) . . ? C33 C32 C37 113.5(2) . . ? C31 C32 C37 128.4(2) . . ? C34 C33 C32 124.3(3) . . ? C33 C34 C35 116.0(3) . . ? C33 C34 C41 120.5(3) . . ? C35 C34 C41 123.4(3) . . ? C34 C35 C36 123.3(3) . . ? C35 C36 C31 119.1(2) . . ? C35 C36 C45 116.2(2) . . ? C31 C36 C45 124.7(2) . . ? C38 C37 C39 108.6(2) . . ? C38 C37 C40 105.0(2) . . ? C39 C37 C40 108.8(2) . . ? C38 C37 C32 116.3(2) . . ? C39 C37 C32 111.0(2) . . ? C40 C37 C32 106.7(2) . . ? C42 C41 C44 108.8(3) . . ? C42 C41 C34 110.1(3) . . ? C44 C41 C34 112.5(3) . . ? C42 C41 C43 108.7(3) . . ? C44 C41 C43 107.1(3) . . ? C34 C41 C43 109.5(2) . . ? C46 C45 C47 110.6(3) . . ? C46 C45 C48 106.3(2) . . ? C47 C45 C48 105.8(2) . . ? C46 C45 C36 111.8(2) . . ? C47 C45 C36 111.5(2) . . ? C48 C45 C36 110.5(2) . . ? Cl49 C50 Cl51 113.6(2) . . ? 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 C13 P1 C1 C2 1.4(3) . . . . ? P1 C1 C2 C3 -129.7(3) . . . . ? C1 C2 C3 P2 -174.5(2) . . . . ? C31 P2 C3 C2 -144.60(19) . . . . ? C4 P2 C3 C2 106.4(2) . . . . ? C3 P2 C4 C8 -74.1(2) . . . . ? C31 P2 C4 C8 167.15(19) . . . . ? C3 P2 C4 C5 175.8(2) . . . . ? C31 P2 C4 C5 57.1(2) . . . . ? C8 C4 C5 C6 -23.9(3) . . . . ? P2 C4 C5 C6 91.1(3) . . . . ? C8 N7 C6 C5 -10.3(4) . . . . ? C9 N7 C6 C5 160.1(3) . . . . ? C4 C5 C6 N7 21.3(3) . . . . ? C11 N12 C8 N7 -7.9(5) . . . . ? C11 N12 C8 C4 174.7(3) . . . . ? C6 N7 C8 N12 176.3(3) . . . . ? C9 N7 C8 N12 6.0(5) . . . . ? C6 N7 C8 C4 -6.0(4) . . . . ? C9 N7 C8 C4 -176.3(3) . . . . ? C5 C4 C8 N12 -163.4(3) . . . . ? P2 C4 C8 N12 80.9(3) . . . . ? C5 C4 C8 N7 18.9(3) . . . . ? P2 C4 C8 N7 -96.8(2) . . . . ? C8 N7 C9 C10 -19.2(5) . . . . ? C6 N7 C9 C10 171.5(4) . . . . ? N7 C9 C10 C11 36.3(6) . . . . ? C9 C10 C11 N12 -39.5(7) . . . . ? C8 N12 C11 C10 23.6(5) . . . . ? C1 P1 C13 C14 -83.8(2) . . . . ? C1 P1 C13 C18 93.6(2) . . . . ? C18 C13 C14 C15 -7.6(4) . . . . ? P1 C13 C14 C15 169.9(2) . . . . ? C18 C13 C14 C19 169.4(3) . . . . ? P1 C13 C14 C19 -13.2(4) . . . . ? C13 C14 C15 C16 2.6(4) . . . . ? C19 C14 C15 C16 -174.6(3) . . . . ? C14 C15 C16 C17 2.7(4) . . . . ? C14 C15 C16 C23 -179.9(3) . . . . ? C15 C16 C17 C18 -3.0(4) . . . . ? C23 C16 C17 C18 179.8(3) . . . . ? C16 C17 C18 C13 -2.0(4) . . . . ? C16 C17 C18 C27 177.6(3) . . . . ? C14 C13 C18 C17 7.3(4) . . . . ? P1 C13 C18 C17 -170.1(2) . . . . ? C14 C13 C18 C27 -172.2(2) . . . . ? P1 C13 C18 C27 10.3(4) . . . . ? C15 C14 C19 C22 9.9(4) . . . . ? C13 C14 C19 C22 -167.1(3) . . . . ? C15 C14 C19 C20 127.3(3) . . . . ? C13 C14 C19 C20 -49.7(4) . . . . ? C15 C14 C19 C21 -109.2(3) . . . . ? C13 C14 C19 C21 73.8(4) . . . . ? C17 C16 C23 C24 -123.8(3) . . . . ? C15 C16 C23 C24 59.0(4) . . . . ? C17 C16 C23 C26 -3.7(4) . . . . ? C15 C16 C23 C26 179.1(3) . . . . ? C17 C16 C23 C25 117.7(3) . . . . ? C15 C16 C23 C25 -59.5(4) . . . . ? C17 C18 C27 C28 -131.3(3) . . . . ? C13 C18 C27 C28 48.3(4) . . . . ? C17 C18 C27 C30 105.4(3) . . . . ? C13 C18 C27 C30 -75.1(4) . . . . ? C17 C18 C27 C29 -13.2(4) . . . . ? C13 C18 C27 C29 166.3(3) . . . . ? C3 P2 C31 C32 -80.9(3) . . . . ? C4 P2 C31 C32 31.7(3) . . . . ? C3 P2 C31 C36 124.28(19) . . . . ? C4 P2 C31 C36 -123.17(19) . . . . ? C36 C31 C32 C33 13.1(4) . . . . ? P2 C31 C32 C33 -140.4(2) . . . . ? C36 C31 C32 C37 -161.6(3) . . . . ? P2 C31 C32 C37 44.8(4) . . . . ? C31 C32 C33 C34 -1.9(4) . . . . ? C37 C32 C33 C34 173.6(3) . . . . ? C32 C33 C34 C35 -8.7(4) . . . . ? C32 C33 C34 C41 174.7(3) . . . . ? C33 C34 C35 C36 8.0(4) . . . . ? C41 C34 C35 C36 -175.5(3) . . . . ? C34 C35 C36 C31 3.2(4) . . . . ? C34 C35 C36 C45 -175.0(3) . . . . ? C32 C31 C36 C35 -13.8(4) . . . . ? P2 C31 C36 C35 143.6(2) . . . . ? C32 C31 C36 C45 164.2(2) . . . . ? P2 C31 C36 C45 -38.3(3) . . . . ? C33 C32 C37 C38 -174.6(2) . . . . ? C31 C32 C37 C38 0.3(4) . . . . ? C33 C32 C37 C39 60.5(3) . . . . ? C31 C32 C37 C39 -124.5(3) . . . . ? C33 C32 C37 C40 -57.9(3) . . . . ? C31 C32 C37 C40 117.1(3) . . . . ? C33 C34 C41 C42 -50.3(4) . . . . ? C35 C34 C41 C42 133.4(3) . . . . ? C33 C34 C41 C44 -171.9(3) . . . . ? C35 C34 C41 C44 11.8(4) . . . . ? C33 C34 C41 C43 69.2(4) . . . . ? C35 C34 C41 C43 -107.1(3) . . . . ? C35 C36 C45 C46 -89.0(3) . . . . ? C31 C36 C45 C46 92.9(3) . . . . ? C35 C36 C45 C47 146.6(3) . . . . ? C31 C36 C45 C47 -31.5(4) . . . . ? C35 C36 C45 C48 29.2(3) . . . . ? C31 C36 C45 C48 -148.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.651 _refine_diff_density_min -0.643 _refine_diff_density_rms 0.082 #===END data_06276 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51.50 H78 N2 O2 P2 Ru' _chemical_formula_weight 920.17 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' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.419(4) _cell_length_b 15.628(5) _cell_length_c 17.189(6) _cell_angle_alpha 106.128(5) _cell_angle_beta 107.568(5) _cell_angle_gamma 95.599(5) _cell_volume 2512.5(15) _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 flatneedle _exptl_crystal_colour gold _exptl_crystal_size_min 0.030 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_max 0.500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.216 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 982 _exptl_absorpt_coefficient_mu 0.414 _exptl_absorpt_correction_type none _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 'Bruker P4' _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 35485 _diffrn_reflns_av_R_equivalents 0.0657 _diffrn_reflns_av_sigmaI/netI 0.0811 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 27.55 _reflns_number_total 11533 _reflns_number_gt 8352 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 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^)+(0.0431P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11533 _refine_ls_number_parameters 566 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1099 _refine_ls_wR_factor_gt 0.0976 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.002 _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 Ru1 Ru 0.92290(2) 0.214518(15) 0.079654(14) 0.01902(7) Uani 1 1 d . . . P1 P 0.82594(7) 0.22378(5) -0.06212(5) 0.01945(16) Uani 1 1 d . . . O1 O 0.6789(2) 0.22056(17) 0.13775(15) 0.0431(6) Uani 1 1 d . . . N1 N 1.1615(3) 0.16267(17) -0.09058(15) 0.0274(6) Uani 1 1 d . . . C1 C 0.7741(3) 0.2208(2) 0.11681(18) 0.0250(7) Uani 1 1 d . . . P2 P 1.08083(8) 0.34195(5) 0.19912(5) 0.02100(17) Uani 1 1 d . . . O2 O 0.9343(3) 0.02199(15) 0.08535(16) 0.0473(6) Uani 1 1 d . . . N2 N 1.0944(2) 0.19815(15) 0.03262(14) 0.0205(5) Uani 1 1 d . . . C2 C 0.9275(3) 0.0946(2) 0.08339(18) 0.0264(7) Uani 1 1 d . . . C3 C 0.9282(3) 0.15286(19) -0.11453(17) 0.0215(6) Uani 1 1 d . . . H3A H 0.8894 0.0895 -0.1242 0.026 Uiso 1 1 calc R . . C4 C 0.9541(3) 0.1551(2) -0.19735(18) 0.0294(7) Uani 1 1 d . . . H4A H 0.8837 0.1123 -0.2482 0.035 Uiso 1 1 calc R . . H4B H 0.9580 0.2155 -0.2025 0.035 Uiso 1 1 calc R . . C5 C 1.0942(3) 0.1271(2) -0.18410(19) 0.0325(7) Uani 1 1 d . . . H5A H 1.0838 0.0616 -0.2053 0.039 Uiso 1 1 calc R . . H5B H 1.1454 0.1542 -0.2129 0.039 Uiso 1 1 calc R . . C6 C 1.0698(3) 0.17390(18) -0.04962(18) 0.0213(6) Uani 1 1 d . . . C7 C 1.3006(3) 0.1573(2) -0.0452(2) 0.0369(8) Uani 1 1 d . . . H7A H 1.3621 0.1752 -0.0730 0.044 Uiso 1 1 calc R . . H7B H 1.3053 0.0956 -0.0453 0.044 Uiso 1 1 calc R . . C8 C 1.3413(3) 0.2210(3) 0.0463(2) 0.0429(9) Uani 1 1 d . . . H8A H 1.3494 0.2833 0.0461 0.051 Uiso 1 1 calc R . . H8B H 1.4302 0.2139 0.0803 0.051 Uiso 1 1 calc R . . C9 C 1.2361(3) 0.2017(2) 0.0870(2) 0.0339(8) Uani 1 1 d . . . H9A H 1.2416 0.1441 0.0975 0.041 Uiso 1 1 calc R . . H9B H 1.2581 0.2487 0.1422 0.041 Uiso 1 1 calc R . . C10 C 0.9119(3) 0.33830(18) -0.05224(18) 0.0227(6) Uani 1 1 d . . . H10A H 0.9565 0.3327 -0.0950 0.027 Uiso 1 1 calc R . . H10B H 0.8438 0.3757 -0.0631 0.027 Uiso 1 1 calc R . . C11 C 1.0194(3) 0.38407(19) 0.03879(18) 0.0246(6) Uani 1 1 d . . . H11A H 1.1052 0.3641 0.0406 0.029 Uiso 1 1 calc R . . H11B H 1.0360 0.4494 0.0512 0.029 Uiso 1 1 calc R . . C12 C 0.9716(3) 0.36112(19) 0.10668(18) 0.0228(6) Uani 1 1 d . . . H12 H 0.904(3) 0.3845(19) 0.1130(18) 0.024(8) Uiso 1 1 d . . . C13 C 0.6642(3) 0.20210(19) -0.15536(18) 0.0229(6) Uani 1 1 d . . . C14 C 0.6186(3) 0.11633(19) -0.22247(19) 0.0264(7) Uani 1 1 d . . . C15 C 0.5672(3) 0.1171(2) -0.30696(19) 0.0307(7) Uani 1 1 d . . . H15A H 0.5446 0.0620 -0.3513 0.037 Uiso 1 1 calc R . . C16 C 0.5474(3) 0.1949(2) -0.32921(19) 0.0281(7) Uani 1 1 d . . . C17 C 0.5568(3) 0.2717(2) -0.26133(19) 0.0285(7) Uani 1 1 d . . . H17A H 0.5276 0.3221 -0.2742 0.034 Uiso 1 1 calc R . . C18 C 0.6077(3) 0.27659(19) -0.17525(18) 0.0241(6) Uani 1 1 d . . . C19 C 0.5988(3) 0.02195(19) -0.20859(19) 0.0289(7) Uani 1 1 d . . . C20 C 0.6328(3) 0.0275(2) -0.11392(19) 0.0310(7) Uani 1 1 d . . . H20A H 0.7307 0.0407 -0.0859 0.046 Uiso 1 1 calc R . . H20B H 0.5950 -0.0296 -0.1110 0.046 Uiso 1 1 calc R . . H20C H 0.5941 0.0747 -0.0856 0.046 Uiso 1 1 calc R . . C21 C 0.6754(4) -0.0444(2) -0.2515(2) 0.0389(8) Uani 1 1 d . . . H21A H 0.7725 -0.0239 -0.2218 0.058 Uiso 1 1 calc R . . H21B H 0.6538 -0.0472 -0.3107 0.058 Uiso 1 1 calc R . . H21C H 0.6478 -0.1037 -0.2490 0.058 Uiso 1 1 calc R . . C22 C 0.4432(3) -0.0180(2) -0.2518(2) 0.0433(9) Uani 1 1 d . . . H22A H 0.4161 -0.0264 -0.3124 0.065 Uiso 1 1 calc R . . H22B H 0.3932 0.0231 -0.2263 0.065 Uiso 1 1 calc R . . H22C H 0.4236 -0.0755 -0.2435 0.065 Uiso 1 1 calc R . . C23 C 0.5067(3) 0.1929(2) -0.42303(19) 0.0346(8) Uani 1 1 d . . . C24 C 0.6274(4) 0.1702(3) -0.4541(2) 0.0556(11) Uani 1 1 d . . . H24A H 0.6043 0.1675 -0.5133 0.083 Uiso 1 1 calc R . . H24B H 0.6451 0.1125 -0.4489 0.083 Uiso 1 1 calc R . . H24C H 0.7078 0.2165 -0.4193 0.083 Uiso 1 1 calc R . . C25 C 0.3791(4) 0.1198(2) -0.4797(2) 0.0489(10) Uani 1 1 d . . . H25A H 0.3037 0.1328 -0.4602 0.073 Uiso 1 1 calc R . . H25B H 0.3969 0.0616 -0.4761 0.073 Uiso 1 1 calc R . . H25C H 0.3563 0.1188 -0.5384 0.073 Uiso 1 1 calc R . . C26 C 0.4783(4) 0.2838(2) -0.4334(2) 0.0492(10) Uani 1 1 d . . . H26A H 0.4040 0.2991 -0.4137 0.074 Uiso 1 1 calc R . . H26B H 0.4540 0.2793 -0.4931 0.074 Uiso 1 1 calc R . . H26C H 0.5591 0.3302 -0.4000 0.074 Uiso 1 1 calc R . . C27 C 0.5728(3) 0.3545(2) -0.11059(19) 0.0277(7) Uani 1 1 d . . . C28 C 0.4142(3) 0.3397(2) -0.1452(2) 0.0417(9) Uani 1 1 d . . . H28A H 0.3839 0.3793 -0.1037 0.062 Uiso 1 1 calc R . . H28B H 0.3758 0.2777 -0.1549 0.062 Uiso 1 1 calc R . . H28C H 0.3847 0.3528 -0.1985 0.062 Uiso 1 1 calc R . . C29 C 0.6286(4) 0.4507(2) -0.1081(2) 0.0389(8) Uani 1 1 d . . . H29A H 0.5877 0.4940 -0.0767 0.058 Uiso 1 1 calc R . . H29B H 0.6062 0.4527 -0.1659 0.058 Uiso 1 1 calc R . . H29C H 0.7265 0.4654 -0.0802 0.058 Uiso 1 1 calc R . . C30 C 0.6111(3) 0.3484(2) -0.01953(19) 0.0321(7) Uani 1 1 d . . . H30A H 0.5693 0.3896 0.0132 0.048 Uiso 1 1 calc R . . H30B H 0.7091 0.3643 0.0080 0.048 Uiso 1 1 calc R . . H30C H 0.5789 0.2875 -0.0225 0.048 Uiso 1 1 calc R . . C31 C 0.9904(3) 0.38008(19) 0.27750(17) 0.0209(6) Uani 1 1 d . . . C32 C 0.9556(3) 0.32325(19) 0.32237(18) 0.0237(6) Uani 1 1 d . . . C33 C 0.8399(3) 0.3330(2) 0.34690(19) 0.0273(7) Uani 1 1 d . . . H33A H 0.8138 0.2938 0.3738 0.033 Uiso 1 1 calc R . . C34 C 0.7620(3) 0.3982(2) 0.33332(19) 0.0282(7) Uani 1 1 d . . . C35 C 0.8162(3) 0.4640(2) 0.30527(19) 0.0283(7) Uani 1 1 d . . . H35A H 0.7727 0.5127 0.3020 0.034 Uiso 1 1 calc R . . C36 C 0.9333(3) 0.45998(19) 0.28185(18) 0.0242(6) Uani 1 1 d . . . C37 C 1.0345(3) 0.2519(2) 0.35037(19) 0.0279(7) Uani 1 1 d . . . C38 C 1.1718(3) 0.2501(3) 0.3349(2) 0.0419(9) Uani 1 1 d . . . H38A H 1.1550 0.2267 0.2741 0.063 Uiso 1 1 calc R . . H38B H 1.2205 0.2118 0.3631 0.063 Uiso 1 1 calc R . . H38C H 1.2258 0.3106 0.3579 0.063 Uiso 1 1 calc R . . C39 C 0.9465(4) 0.1561(2) 0.3076(2) 0.0400(9) Uani 1 1 d . . . H39A H 0.8669 0.1536 0.3247 0.060 Uiso 1 1 calc R . . H39B H 0.9992 0.1134 0.3253 0.060 Uiso 1 1 calc R . . H39C H 0.9181 0.1410 0.2461 0.060 Uiso 1 1 calc R . . C40 C 1.0704(4) 0.2761(2) 0.44862(19) 0.0383(8) Uani 1 1 d . . . H40A H 0.9874 0.2689 0.4616 0.058 Uiso 1 1 calc R . . H40B H 1.1189 0.3380 0.4764 0.058 Uiso 1 1 calc R . . H40C H 1.1272 0.2366 0.4691 0.058 Uiso 1 1 calc R . . C41 C 0.6284(3) 0.3995(2) 0.3525(2) 0.0357(8) Uani 1 1 d . . . C42 C 0.5441(4) 0.3040(3) 0.3214(3) 0.0738(14) Uani 1 1 d . . . H42A H 0.4579 0.3066 0.3305 0.111 Uiso 1 1 calc R . . H42B H 0.5932 0.2684 0.3529 0.111 Uiso 1 1 calc R . . H42C H 0.5278 0.2766 0.2610 0.111 Uiso 1 1 calc R . . C43 C 0.6593(5) 0.4388(4) 0.4486(3) 0.117(3) Uani 1 1 d . . . H43A H 0.7036 0.5015 0.4684 0.176 Uiso 1 1 calc R . . H43B H 0.7186 0.4057 0.4778 0.176 Uiso 1 1 calc R . . H43C H 0.5751 0.4342 0.4606 0.176 Uiso 1 1 calc R . . C44 C 0.5384(5) 0.4516(5) 0.3049(5) 0.136(3) Uani 1 1 d . . . H44A H 0.5785 0.5153 0.3296 0.204 Uiso 1 1 calc R . . H44B H 0.4489 0.4418 0.3095 0.204 Uiso 1 1 calc R . . H44C H 0.5303 0.4311 0.2453 0.204 Uiso 1 1 calc R . . C45 C 0.9966(3) 0.5493(2) 0.2722(2) 0.0306(7) Uani 1 1 d . . . C46 C 1.0130(4) 0.6266(2) 0.3556(2) 0.0517(10) Uani 1 1 d . . . H46A H 1.0617 0.6820 0.3557 0.078 Uiso 1 1 calc R . . H46B H 1.0635 0.6111 0.4049 0.078 Uiso 1 1 calc R . . H46C H 0.9239 0.6345 0.3581 0.078 Uiso 1 1 calc R . . C47 C 0.9033(4) 0.5720(2) 0.1963(2) 0.0407(9) Uani 1 1 d . . . H47A H 0.9062 0.5324 0.1433 0.061 Uiso 1 1 calc R . . H47B H 0.9341 0.6339 0.2015 0.061 Uiso 1 1 calc R . . H47C H 0.8108 0.5640 0.1964 0.061 Uiso 1 1 calc R . . C48 C 1.1416(3) 0.5538(2) 0.2668(2) 0.0387(8) Uani 1 1 d . . . H48A H 1.1371 0.5127 0.2124 0.058 Uiso 1 1 calc R . . H48B H 1.1998 0.5370 0.3129 0.058 Uiso 1 1 calc R . . H48C H 1.1784 0.6146 0.2716 0.058 Uiso 1 1 calc R . . C50 C 0.0512(7) 0.1310(4) 0.6007(4) 0.0894(17) Uani 1 1 d . . . C51 C 0.0093(12) 0.0488(7) 0.5327(7) 0.070(3) Uani 0.50 1 d P . . C52 C 0.0947(6) -0.0233(4) 0.5444(4) 0.0716(14) Uani 1 1 d . . . C53 C -0.0547(11) 0.1043(7) 0.5220(9) 0.076(3) Uani 0.50 1 d P . . C54 C 0.1306(12) 0.0555(8) 0.6091(7) 0.081(3) Uani 0.50 1 d P . . 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 Ru1 0.01788(13) 0.02112(12) 0.01944(13) 0.00880(9) 0.00599(10) 0.00494(9) P1 0.0187(4) 0.0202(4) 0.0190(4) 0.0081(3) 0.0042(3) 0.0040(3) O1 0.0226(12) 0.0680(17) 0.0424(14) 0.0177(13) 0.0162(11) 0.0091(12) N1 0.0249(14) 0.0343(15) 0.0262(14) 0.0097(11) 0.0132(12) 0.0062(12) C1 0.0225(16) 0.0279(16) 0.0223(15) 0.0099(13) 0.0034(13) 0.0037(13) P2 0.0177(4) 0.0253(4) 0.0197(4) 0.0077(3) 0.0056(3) 0.0038(3) O2 0.0694(18) 0.0257(12) 0.0582(16) 0.0221(12) 0.0282(14) 0.0160(12) N2 0.0172(12) 0.0236(12) 0.0201(12) 0.0084(10) 0.0040(10) 0.0053(10) C2 0.0297(18) 0.0318(17) 0.0215(15) 0.0105(13) 0.0120(14) 0.0080(14) C3 0.0239(16) 0.0206(14) 0.0203(15) 0.0066(12) 0.0081(13) 0.0044(12) C4 0.0370(19) 0.0319(17) 0.0212(15) 0.0090(13) 0.0113(14) 0.0099(15) C5 0.0332(19) 0.0419(19) 0.0274(17) 0.0117(15) 0.0175(15) 0.0066(15) C6 0.0228(16) 0.0174(14) 0.0265(16) 0.0088(12) 0.0105(13) 0.0046(12) C7 0.0232(18) 0.052(2) 0.040(2) 0.0140(17) 0.0170(16) 0.0102(16) C8 0.0198(18) 0.063(2) 0.039(2) 0.0063(18) 0.0096(16) 0.0071(17) C9 0.0253(18) 0.048(2) 0.0267(17) 0.0091(15) 0.0080(14) 0.0137(16) C10 0.0253(16) 0.0240(15) 0.0230(15) 0.0124(12) 0.0092(13) 0.0067(13) C11 0.0243(16) 0.0206(15) 0.0273(16) 0.0093(13) 0.0062(13) 0.0020(13) C12 0.0235(17) 0.0223(15) 0.0233(16) 0.0074(12) 0.0088(13) 0.0053(13) C13 0.0197(15) 0.0224(15) 0.0258(16) 0.0106(12) 0.0043(13) 0.0042(12) C14 0.0231(16) 0.0244(15) 0.0287(16) 0.0108(13) 0.0027(14) 0.0049(13) C15 0.0329(18) 0.0228(16) 0.0241(16) 0.0019(13) -0.0013(14) 0.0032(14) C16 0.0236(17) 0.0315(17) 0.0231(16) 0.0116(13) -0.0015(13) 0.0015(14) C17 0.0296(18) 0.0228(15) 0.0284(17) 0.0107(13) 0.0012(14) 0.0052(13) C18 0.0178(15) 0.0257(15) 0.0268(16) 0.0115(13) 0.0028(13) 0.0021(12) C19 0.0315(18) 0.0206(15) 0.0265(16) 0.0077(13) 0.0000(14) 0.0013(13) C20 0.0318(18) 0.0243(16) 0.0356(18) 0.0142(14) 0.0067(15) 0.0020(14) C21 0.051(2) 0.0238(16) 0.0321(18) 0.0068(14) 0.0026(17) 0.0067(16) C22 0.034(2) 0.0345(19) 0.047(2) 0.0158(17) -0.0045(17) -0.0049(16) C23 0.036(2) 0.0380(19) 0.0234(16) 0.0149(15) -0.0012(15) 0.0020(16) C24 0.061(3) 0.068(3) 0.044(2) 0.025(2) 0.022(2) 0.012(2) C25 0.054(2) 0.047(2) 0.0295(19) 0.0144(17) -0.0066(18) 0.0014(19) C26 0.066(3) 0.041(2) 0.0292(19) 0.0189(17) -0.0032(18) 0.0021(19) C27 0.0223(16) 0.0289(16) 0.0305(17) 0.0106(14) 0.0050(14) 0.0092(13) C28 0.0296(19) 0.055(2) 0.041(2) 0.0184(18) 0.0066(16) 0.0210(17) C29 0.049(2) 0.0277(17) 0.043(2) 0.0121(15) 0.0160(18) 0.0152(16) C30 0.0250(17) 0.0391(19) 0.0329(18) 0.0109(15) 0.0099(15) 0.0125(15) C31 0.0151(14) 0.0261(15) 0.0189(14) 0.0060(12) 0.0037(12) 0.0040(12) C32 0.0255(16) 0.0266(15) 0.0197(15) 0.0084(12) 0.0079(13) 0.0056(13) C33 0.0297(18) 0.0297(16) 0.0282(17) 0.0146(14) 0.0127(14) 0.0070(14) C34 0.0277(17) 0.0323(17) 0.0302(17) 0.0115(14) 0.0152(14) 0.0096(14) C35 0.0292(18) 0.0264(16) 0.0350(18) 0.0112(14) 0.0162(15) 0.0104(14) C36 0.0246(16) 0.0253(15) 0.0202(15) 0.0054(12) 0.0064(13) 0.0031(13) C37 0.0295(17) 0.0378(18) 0.0240(16) 0.0163(14) 0.0115(14) 0.0143(15) C38 0.034(2) 0.066(2) 0.045(2) 0.0356(19) 0.0181(17) 0.0307(19) C39 0.055(2) 0.0361(19) 0.0359(19) 0.0186(16) 0.0161(18) 0.0185(18) C40 0.041(2) 0.055(2) 0.0274(17) 0.0227(16) 0.0117(16) 0.0209(18) C41 0.0302(19) 0.0352(18) 0.051(2) 0.0170(17) 0.0228(17) 0.0125(15) C42 0.043(3) 0.073(3) 0.111(4) 0.020(3) 0.042(3) 0.009(2) C43 0.068(4) 0.169(6) 0.081(4) -0.032(4) 0.057(3) -0.012(4) C44 0.063(3) 0.201(7) 0.270(9) 0.194(7) 0.108(5) 0.088(4) C45 0.0354(19) 0.0218(15) 0.0371(18) 0.0067(14) 0.0194(16) 0.0024(14) C46 0.060(3) 0.032(2) 0.057(2) -0.0047(18) 0.034(2) -0.0025(18) C47 0.049(2) 0.0305(18) 0.053(2) 0.0211(17) 0.0231(19) 0.0119(17) C48 0.035(2) 0.0282(17) 0.049(2) 0.0051(16) 0.0184(17) -0.0049(15) C50 0.129(5) 0.096(4) 0.076(4) 0.049(4) 0.059(4) 0.031(4) C51 0.104(8) 0.078(7) 0.074(7) 0.052(6) 0.065(7) 0.029(7) C52 0.090(4) 0.090(4) 0.082(4) 0.061(3) 0.056(3) 0.045(3) C53 0.086(8) 0.073(7) 0.143(11) 0.081(8) 0.087(8) 0.053(6) C54 0.114(9) 0.100(8) 0.081(7) 0.054(7) 0.072(7) 0.058(7) _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 Ru1 C1 1.847(3) . ? Ru1 C2 1.897(3) . ? Ru1 N2 2.181(2) . ? Ru1 C12 2.182(3) . ? Ru1 P1 2.3913(11) . ? Ru1 P2 2.4370(9) . ? P1 C3 1.852(3) . ? P1 C10 1.860(3) . ? P1 C13 1.866(3) . ? O1 C1 1.153(3) . ? N1 C6 1.345(3) . ? N1 C7 1.447(4) . ? N1 C5 1.460(4) . ? P2 C12 1.775(3) . ? P2 C31 1.868(3) . ? O2 C2 1.154(3) . ? N2 C6 1.293(3) . ? N2 C9 1.476(4) . ? C3 C6 1.496(4) . ? C3 C4 1.536(4) . ? C4 C5 1.534(4) . ? C7 C8 1.514(4) . ? C8 C9 1.515(4) . ? C10 C11 1.542(4) . ? C11 C12 1.512(4) . ? C13 C14 1.428(4) . ? C13 C18 1.432(4) . ? C14 C15 1.392(4) . ? C14 C19 1.562(4) . ? C15 C16 1.389(4) . ? C16 C17 1.393(4) . ? C16 C23 1.529(4) . ? C17 C18 1.390(4) . ? C18 C27 1.559(4) . ? C19 C20 1.533(4) . ? C19 C21 1.533(4) . ? C19 C22 1.545(4) . ? C23 C25 1.525(5) . ? C23 C26 1.526(4) . ? C23 C24 1.542(5) . ? C27 C30 1.527(4) . ? C27 C29 1.542(4) . ? C27 C28 1.547(4) . ? C31 C32 1.415(4) . ? C31 C36 1.428(4) . ? C32 C33 1.400(4) . ? C32 C37 1.546(4) . ? C33 C34 1.388(4) . ? C34 C35 1.391(4) . ? C34 C41 1.525(4) . ? C35 C36 1.396(4) . ? C36 C45 1.558(4) . ? C37 C39 1.529(4) . ? C37 C38 1.533(4) . ? C37 C40 1.540(4) . ? C41 C44 1.506(5) . ? C41 C43 1.512(6) . ? C41 C42 1.517(5) . ? C45 C47 1.526(4) . ? C45 C48 1.537(4) . ? C45 C46 1.547(4) . ? C50 C53 1.385(13) . ? C50 C51 1.398(12) . ? C50 C54 1.520(11) . ? C51 C53 1.165(12) . ? C51 C52 1.358(12) 2_556 ? C51 C54 1.493(16) . ? C51 C52 1.521(11) . ? C51 C51 1.58(2) 2_556 ? C52 C54 1.338(11) . ? C52 C51 1.358(12) 2_556 ? C52 C53 1.373(13) 2_556 ? C53 C52 1.373(13) 2_556 ? 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 C1 Ru1 C2 92.44(13) . . ? C1 Ru1 N2 176.51(11) . . ? C2 Ru1 N2 84.42(11) . . ? C1 Ru1 C12 93.17(12) . . ? C2 Ru1 C12 163.62(12) . . ? N2 Ru1 C12 90.26(10) . . ? C1 Ru1 P1 101.09(9) . . ? C2 Ru1 P1 114.44(9) . . ? N2 Ru1 P1 78.89(6) . . ? C12 Ru1 P1 79.48(8) . . ? C1 Ru1 P2 96.69(9) . . ? C2 Ru1 P2 119.22(9) . . ? N2 Ru1 P2 86.21(7) . . ? C12 Ru1 P2 44.76(8) . . ? P1 Ru1 P2 122.17(3) . . ? C3 P1 C10 99.74(13) . . ? C3 P1 C13 100.75(13) . . ? C10 P1 C13 102.16(13) . . ? C3 P1 Ru1 98.18(9) . . ? C10 P1 Ru1 103.25(9) . . ? C13 P1 Ru1 145.04(10) . . ? C6 N1 C7 120.5(2) . . ? C6 N1 C5 111.7(2) . . ? C7 N1 C5 124.6(2) . . ? O1 C1 Ru1 176.9(3) . . ? C12 P2 C31 101.02(14) . . ? C12 P2 Ru1 59.99(10) . . ? C31 P2 Ru1 106.86(9) . . ? C6 N2 C9 116.2(2) . . ? C6 N2 Ru1 118.73(19) . . ? C9 N2 Ru1 124.66(18) . . ? O2 C2 Ru1 177.8(3) . . ? C6 C3 C4 103.3(2) . . ? C6 C3 P1 106.69(18) . . ? C4 C3 P1 125.7(2) . . ? C5 C4 C3 102.1(2) . . ? N1 C5 C4 102.9(2) . . ? N2 C6 N1 127.5(3) . . ? N2 C6 C3 123.0(3) . . ? N1 C6 C3 109.5(2) . . ? N1 C7 C8 107.4(3) . . ? C7 C8 C9 111.1(3) . . ? N2 C9 C8 112.8(3) . . ? C11 C10 P1 110.37(18) . . ? C12 C11 C10 111.4(2) . . ? C11 C12 P2 124.3(2) . . ? C11 C12 Ru1 111.47(19) . . ? P2 C12 Ru1 75.25(11) . . ? C14 C13 C18 116.7(3) . . ? C14 C13 P1 120.3(2) . . ? C18 C13 P1 120.2(2) . . ? C15 C14 C13 117.3(3) . . ? C15 C14 C19 116.7(3) . . ? C13 C14 C19 125.1(3) . . ? C16 C15 C14 124.1(3) . . ? C15 C16 C17 115.2(3) . . ? C15 C16 C23 121.4(3) . . ? C17 C16 C23 123.2(3) . . ? C18 C17 C16 123.2(3) . . ? C17 C18 C13 118.1(3) . . ? C17 C18 C27 115.9(2) . . ? C13 C18 C27 125.0(3) . . ? C20 C19 C21 110.0(3) . . ? C20 C19 C22 105.3(3) . . ? C21 C19 C22 108.2(3) . . ? C20 C19 C14 114.1(2) . . ? C21 C19 C14 113.2(3) . . ? C22 C19 C14 105.4(2) . . ? C25 C23 C26 108.4(3) . . ? C25 C23 C16 110.8(3) . . ? C26 C23 C16 112.6(3) . . ? C25 C23 C24 108.9(3) . . ? C26 C23 C24 108.6(3) . . ? C16 C23 C24 107.5(3) . . ? C30 C27 C29 110.7(3) . . ? C30 C27 C28 105.6(3) . . ? C29 C27 C28 107.1(3) . . ? C30 C27 C18 113.9(2) . . ? C29 C27 C18 114.1(3) . . ? C28 C27 C18 104.6(2) . . ? C32 C31 C36 117.9(2) . . ? C32 C31 P2 121.0(2) . . ? C36 C31 P2 120.1(2) . . ? C33 C32 C31 117.8(3) . . ? C33 C32 C37 115.2(3) . . ? C31 C32 C37 126.9(3) . . ? C34 C33 C32 123.6(3) . . ? C33 C34 C35 116.1(3) . . ? C33 C34 C41 121.5(3) . . ? C35 C34 C41 122.4(3) . . ? C34 C35 C36 122.8(3) . . ? C35 C36 C31 118.3(3) . . ? C35 C36 C45 114.9(3) . . ? C31 C36 C45 126.5(3) . . ? C39 C37 C38 108.4(3) . . ? C39 C37 C40 108.1(3) . . ? C38 C37 C40 105.6(3) . . ? C39 C37 C32 111.6(3) . . ? C38 C37 C32 115.4(3) . . ? C40 C37 C32 107.3(2) . . ? C44 C41 C43 110.8(4) . . ? C44 C41 C42 105.4(4) . . ? C43 C41 C42 108.3(4) . . ? C44 C41 C34 111.6(3) . . ? C43 C41 C34 110.0(3) . . ? C42 C41 C34 110.7(3) . . ? C47 C45 C48 109.0(3) . . ? C47 C45 C46 107.7(3) . . ? C48 C45 C46 105.0(3) . . ? C47 C45 C36 112.6(3) . . ? C48 C45 C36 115.6(3) . . ? C46 C45 C36 106.4(3) . . ? C53 C50 C51 49.5(6) . . ? C53 C50 C54 110.9(7) . . ? C51 C50 C54 61.4(7) . . ? C53 C51 C52 65.4(10) . 2_556 ? C53 C51 C50 64.7(9) . . ? C52 C51 C50 130.1(9) 2_556 . ? C53 C51 C54 128.0(14) . . ? C52 C51 C54 166.5(10) 2_556 . ? C50 C51 C54 63.3(8) . . ? C53 C51 C52 178.1(9) . . ? C52 C51 C52 113.9(8) 2_556 . ? C50 C51 C52 116.0(10) . . ? C54 C51 C52 52.7(6) . . ? C53 C51 C51 127.3(17) . 2_556 ? C52 C51 C51 61.9(8) 2_556 2_556 ? C50 C51 C51 167.9(15) . 2_556 ? C54 C51 C51 104.7(11) . 2_556 ? C52 C51 C51 52.0(6) . 2_556 ? C54 C52 C51 128.7(8) . 2_556 ? C54 C52 C53 178.7(7) . 2_556 ? C51 C52 C53 50.5(6) 2_556 2_556 ? C54 C52 C51 62.6(7) . . ? C51 C52 C51 66.1(8) 2_556 . ? C53 C52 C51 116.6(9) 2_556 . ? C51 C53 C52 64.1(9) . 2_556 ? C51 C53 C50 65.8(9) . . ? C52 C53 C50 129.9(8) 2_556 . ? C52 C54 C51 64.7(7) . . ? C52 C54 C50 120.0(9) . . ? C51 C54 C50 55.3(6) . . ? 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 C1 Ru1 P1 C3 -148.22(13) . . . . ? C2 Ru1 P1 C3 -50.36(14) . . . . ? N2 Ru1 P1 C3 28.22(11) . . . . ? C12 Ru1 P1 C3 120.58(13) . . . . ? P2 Ru1 P1 C3 106.50(10) . . . . ? C1 Ru1 P1 C10 109.69(13) . . . . ? C2 Ru1 P1 C10 -152.45(14) . . . . ? N2 Ru1 P1 C10 -73.87(11) . . . . ? C12 Ru1 P1 C10 18.49(13) . . . . ? P2 Ru1 P1 C10 4.41(10) . . . . ? C1 Ru1 P1 C13 -25.92(19) . . . . ? C2 Ru1 P1 C13 71.94(19) . . . . ? N2 Ru1 P1 C13 150.52(17) . . . . ? C12 Ru1 P1 C13 -117.12(18) . . . . ? P2 Ru1 P1 C13 -131.21(16) . . . . ? C2 Ru1 C1 O1 -38(5) . . . . ? N2 Ru1 C1 O1 -11(6) . . . . ? C12 Ru1 C1 O1 158(5) . . . . ? P1 Ru1 C1 O1 78(5) . . . . ? P2 Ru1 C1 O1 -157(5) . . . . ? C1 Ru1 P2 C12 -87.76(15) . . . . ? C2 Ru1 P2 C12 175.65(15) . . . . ? N2 Ru1 P2 C12 94.20(13) . . . . ? P1 Ru1 P2 C12 19.86(12) . . . . ? C1 Ru1 P2 C31 5.44(13) . . . . ? C2 Ru1 P2 C31 -91.15(14) . . . . ? N2 Ru1 P2 C31 -172.60(11) . . . . ? C12 Ru1 P2 C31 93.19(15) . . . . ? P1 Ru1 P2 C31 113.05(10) . . . . ? C1 Ru1 N2 C6 70.6(18) . . . . ? C2 Ru1 N2 C6 96.9(2) . . . . ? C12 Ru1 N2 C6 -98.6(2) . . . . ? P1 Ru1 N2 C6 -19.42(19) . . . . ? P2 Ru1 N2 C6 -143.3(2) . . . . ? C1 Ru1 N2 C9 -101.5(17) . . . . ? C2 Ru1 N2 C9 -75.2(2) . . . . ? C12 Ru1 N2 C9 89.3(2) . . . . ? P1 Ru1 N2 C9 168.5(2) . . . . ? P2 Ru1 N2 C9 44.6(2) . . . . ? C1 Ru1 C2 O2 -168(7) . . . . ? N2 Ru1 C2 O2 14(7) . . . . ? C12 Ru1 C2 O2 -58(8) . . . . ? P1 Ru1 C2 O2 89(7) . . . . ? P2 Ru1 C2 O2 -69(8) . . . . ? C10 P1 C3 C6 67.6(2) . . . . ? C13 P1 C3 C6 172.11(18) . . . . ? Ru1 P1 C3 C6 -37.43(19) . . . . ? C10 P1 C3 C4 -53.2(3) . . . . ? C13 P1 C3 C4 51.3(3) . . . . ? Ru1 P1 C3 C4 -158.2(2) . . . . ? C6 C3 C4 C5 28.8(3) . . . . ? P1 C3 C4 C5 151.0(2) . . . . ? C6 N1 C5 C4 23.2(3) . . . . ? C7 N1 C5 C4 -177.1(3) . . . . ? C3 C4 C5 N1 -31.2(3) . . . . ? C9 N2 C6 N1 -9.1(4) . . . . ? Ru1 N2 C6 N1 178.1(2) . . . . ? C9 N2 C6 C3 170.3(3) . . . . ? Ru1 N2 C6 C3 -2.5(3) . . . . ? C7 N1 C6 N2 14.3(4) . . . . ? C5 N1 C6 N2 175.0(3) . . . . ? C7 N1 C6 C3 -165.1(3) . . . . ? C5 N1 C6 C3 -4.5(3) . . . . ? C4 C3 C6 N2 164.4(3) . . . . ? P1 C3 C6 N2 30.2(3) . . . . ? C4 C3 C6 N1 -16.2(3) . . . . ? P1 C3 C6 N1 -150.3(2) . . . . ? C6 N1 C7 C8 -35.5(4) . . . . ? C5 N1 C7 C8 166.4(3) . . . . ? N1 C7 C8 C9 52.6(4) . . . . ? C6 N2 C9 C8 27.7(4) . . . . ? Ru1 N2 C9 C8 -160.0(2) . . . . ? C7 C8 C9 N2 -50.8(4) . . . . ? C3 P1 C10 C11 -97.2(2) . . . . ? C13 P1 C10 C11 159.4(2) . . . . ? Ru1 P1 C10 C11 3.6(2) . . . . ? P1 C10 C11 C12 -36.2(3) . . . . ? C10 C11 C12 P2 142.8(2) . . . . ? C10 C11 C12 Ru1 56.4(3) . . . . ? C31 P2 C12 C11 150.6(2) . . . . ? Ru1 P2 C12 C11 -106.2(3) . . . . ? C31 P2 C12 Ru1 -103.22(11) . . . . ? C1 Ru1 C12 C11 -142.2(2) . . . . ? C2 Ru1 C12 C11 108.0(4) . . . . ? N2 Ru1 C12 C11 37.2(2) . . . . ? P1 Ru1 C12 C11 -41.46(19) . . . . ? P2 Ru1 C12 C11 121.5(2) . . . . ? C1 Ru1 C12 P2 96.30(12) . . . . ? C2 Ru1 C12 P2 -13.6(5) . . . . ? N2 Ru1 C12 P2 -84.35(11) . . . . ? P1 Ru1 C12 P2 -163.00(10) . . . . ? C3 P1 C13 C14 31.7(3) . . . . ? C10 P1 C13 C14 134.3(2) . . . . ? Ru1 P1 C13 C14 -89.9(3) . . . . ? C3 P1 C13 C18 -128.7(2) . . . . ? C10 P1 C13 C18 -26.2(3) . . . . ? Ru1 P1 C13 C18 109.7(2) . . . . ? C18 C13 C14 C15 23.1(4) . . . . ? P1 C13 C14 C15 -138.0(3) . . . . ? C18 C13 C14 C19 -146.0(3) . . . . ? P1 C13 C14 C19 52.9(4) . . . . ? C13 C14 C15 C16 -5.4(5) . . . . ? C19 C14 C15 C16 164.6(3) . . . . ? C14 C15 C16 C17 -12.1(5) . . . . ? C14 C15 C16 C23 172.7(3) . . . . ? C15 C16 C17 C18 11.9(5) . . . . ? C23 C16 C17 C18 -172.9(3) . . . . ? C16 C17 C18 C13 5.7(5) . . . . ? C16 C17 C18 C27 -163.1(3) . . . . ? C14 C13 C18 C17 -23.3(4) . . . . ? P1 C13 C18 C17 137.8(2) . . . . ? C14 C13 C18 C27 144.3(3) . . . . ? P1 C13 C18 C27 -54.5(4) . . . . ? C15 C14 C19 C20 -169.2(3) . . . . ? C13 C14 C19 C20 0.0(4) . . . . ? C15 C14 C19 C21 63.9(4) . . . . ? C13 C14 C19 C21 -126.9(3) . . . . ? C15 C14 C19 C22 -54.1(4) . . . . ? C13 C14 C19 C22 115.1(3) . . . . ? C15 C16 C23 C25 53.4(4) . . . . ? C17 C16 C23 C25 -121.4(3) . . . . ? C15 C16 C23 C26 175.0(3) . . . . ? C17 C16 C23 C26 0.2(5) . . . . ? C15 C16 C23 C24 -65.5(4) . . . . ? C17 C16 C23 C24 119.7(3) . . . . ? C17 C18 C27 C30 170.9(3) . . . . ? C13 C18 C27 C30 3.0(4) . . . . ? C17 C18 C27 C29 -60.6(4) . . . . ? C13 C18 C27 C29 131.4(3) . . . . ? C17 C18 C27 C28 56.1(3) . . . . ? C13 C18 C27 C28 -111.9(3) . . . . ? C12 P2 C31 C32 127.5(2) . . . . ? Ru1 P2 C31 C32 65.7(2) . . . . ? C12 P2 C31 C36 -41.2(3) . . . . ? Ru1 P2 C31 C36 -103.0(2) . . . . ? C36 C31 C32 C33 18.0(4) . . . . ? P2 C31 C32 C33 -151.0(2) . . . . ? C36 C31 C32 C37 -160.1(3) . . . . ? P2 C31 C32 C37 31.0(4) . . . . ? C31 C32 C33 C34 -3.2(4) . . . . ? C37 C32 C33 C34 175.1(3) . . . . ? C32 C33 C34 C35 -9.5(4) . . . . ? C32 C33 C34 C41 173.4(3) . . . . ? C33 C34 C35 C36 7.5(4) . . . . ? C41 C34 C35 C36 -175.5(3) . . . . ? C34 C35 C36 C31 7.1(4) . . . . ? C34 C35 C36 C45 -166.9(3) . . . . ? C32 C31 C36 C35 -19.9(4) . . . . ? P2 C31 C36 C35 149.1(2) . . . . ? C32 C31 C36 C45 153.3(3) . . . . ? P2 C31 C36 C45 -37.6(4) . . . . ? C33 C32 C37 C39 63.8(3) . . . . ? C31 C32 C37 C39 -118.1(3) . . . . ? C33 C32 C37 C38 -171.9(3) . . . . ? C31 C32 C37 C38 6.3(4) . . . . ? C33 C32 C37 C40 -54.5(3) . . . . ? C31 C32 C37 C40 123.6(3) . . . . ? C33 C34 C41 C44 -159.6(4) . . . . ? C35 C34 C41 C44 23.4(5) . . . . ? C33 C34 C41 C43 77.0(5) . . . . ? C35 C34 C41 C43 -99.9(4) . . . . ? C33 C34 C41 C42 -42.6(4) . . . . ? C35 C34 C41 C42 140.5(4) . . . . ? C35 C36 C45 C47 -67.0(3) . . . . ? C31 C36 C45 C47 119.5(3) . . . . ? C35 C36 C45 C48 166.8(3) . . . . ? C31 C36 C45 C48 -6.7(4) . . . . ? C35 C36 C45 C46 50.7(4) . . . . ? C31 C36 C45 C46 -122.8(3) . . . . ? C54 C50 C51 C53 -179.2(8) . . . . ? C53 C50 C51 C52 0.1(8) . . . 2_556 ? C54 C50 C51 C52 -179.1(11) . . . 2_556 ? C53 C50 C51 C54 179.2(8) . . . . ? C53 C50 C51 C52 178.1(9) . . . . ? C54 C50 C51 C52 -1.1(6) . . . . ? C53 C50 C51 C51 172(5) . . . 2_556 ? C54 C50 C51 C51 -7(4) . . . 2_556 ? C53 C51 C52 C54 113(48) . . . . ? C52 C51 C52 C54 179.6(9) 2_556 . . . ? C50 C51 C52 C54 1.2(7) . . . . ? C51 C51 C52 C54 179.6(9) 2_556 . . . ? C53 C51 C52 C51 -67(48) . . . 2_556 ? C52 C51 C52 C51 0.002(3) 2_556 . . 2_556 ? C50 C51 C52 C51 -178.3(11) . . . 2_556 ? C54 C51 C52 C51 -179.6(9) . . . 2_556 ? C53 C51 C52 C53 -68(48) . . . 2_556 ? C52 C51 C52 C53 -1.6(8) 2_556 . . 2_556 ? C50 C51 C52 C53 -179.9(6) . . . 2_556 ? C54 C51 C52 C53 178.8(8) . . . 2_556 ? C51 C51 C52 C53 -1.6(8) 2_556 . . 2_556 ? C50 C51 C53 C52 179.9(6) . . . 2_556 ? C54 C51 C53 C52 179.0(11) . . . 2_556 ? C52 C51 C53 C52 67(48) . . . 2_556 ? C51 C51 C53 C52 2.1(10) 2_556 . . 2_556 ? C52 C51 C53 C50 -179.9(6) 2_556 . . . ? C54 C51 C53 C50 -0.9(9) . . . . ? C52 C51 C53 C50 -113(48) . . . . ? C51 C51 C53 C50 -177.8(13) 2_556 . . . ? C54 C50 C53 C51 0.7(8) . . . . ? C51 C50 C53 C52 -0.1(8) . . . 2_556 ? C54 C50 C53 C52 0.6(11) . . . 2_556 ? C51 C52 C54 C51 0.5(10) 2_556 . . . ? C53 C52 C54 C51 -52(31) 2_556 . . . ? C51 C52 C54 C50 -0.7(12) 2_556 . . . ? C53 C52 C54 C50 -54(32) 2_556 . . . ? C51 C52 C54 C50 -1.2(6) . . . . ? C53 C51 C54 C52 -177.8(11) . . . . ? C52 C51 C54 C52 -2(3) 2_556 . . . ? C50 C51 C54 C52 -178.7(7) . . . . ? C51 C51 C54 C52 -0.4(7) 2_556 . . . ? C53 C51 C54 C50 0.9(9) . . . . ? C52 C51 C54 C50 177(4) 2_556 . . . ? C52 C51 C54 C50 178.7(7) . . . . ? C51 C51 C54 C50 178.4(10) 2_556 . . . ? C53 C50 C54 C52 0.7(10) . . . . ? C51 C50 C54 C52 1.3(7) . . . . ? C53 C50 C54 C51 -0.6(7) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.861 _refine_diff_density_min -0.775 _refine_diff_density_rms 0.090 #===END