# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1530 data_1a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H72 N9 P3' _chemical_formula_weight 723.94 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' '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 11.039(4) _cell_length_b 12.001(4) _cell_length_c 16.651(6) _cell_angle_alpha 95.81(4) _cell_angle_beta 91.38(4) _cell_angle_gamma 108.77(3) _cell_volume 2074.1(13) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.159 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 0.180 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Stoe IPDS' _diffrn_measurement_method 2theta/omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5717 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_sigmaI/netI 0.1712 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 22.50 _reflns_number_total 5408 _reflns_number_gt 2878 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0214P)^2^+2.3853P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0023(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5408 _refine_ls_number_parameters 443 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1726 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.1453 _refine_ls_wR_factor_gt 0.1160 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.015 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P -0.07239(14) 0.01077(13) 0.13048(9) 0.0229(4) Uani 1 d . . . P2 P 0.16191(14) 0.00910(14) 0.20106(9) 0.0230(4) Uani 1 d . . . P3 P -0.06511(14) -0.06944(14) 0.28297(9) 0.0231(4) Uani 1 d . . . N1 N 0.0799(4) 0.0365(4) 0.1297(3) 0.0242(11) Uani 1 d . . . N2 N 0.0856(4) -0.0419(4) 0.2765(3) 0.0238(12) Uani 1 d . . . N3 N -0.1389(4) -0.0366(4) 0.2100(3) 0.0238(11) Uani 1 d . . . N10 N -0.1575(4) -0.0828(4) 0.0538(3) 0.0262(12) Uani 1 d D . . H10 H -0.138(5) -0.067(5) 0.0096(17) 0.031 Uiso 1 d D . . C11 C -0.1961(5) -0.2117(5) 0.0553(3) 0.0242(14) Uani 1 d . . . H11 H -0.2517 -0.2317 0.1018 0.029 Uiso 1 calc R . . C12 C -0.0858(5) -0.2593(5) 0.0665(3) 0.0287(15) Uani 1 d . . . H12A H -0.0247 -0.2337 0.0242 0.034 Uiso 1 calc R . . H12B H -0.0401 -0.2250 0.1197 0.034 Uiso 1 calc R . . C13 C -0.1299(6) -0.3932(5) 0.0619(4) 0.0400(17) Uani 1 d . . . H13A H -0.1823 -0.4187 0.1083 0.048 Uiso 1 calc R . . H13B H -0.0542 -0.4201 0.0655 0.048 Uiso 1 calc R . . C14 C -0.2085(7) -0.4501(5) -0.0166(4) 0.0490(19) Uani 1 d . . . H14A H -0.1535 -0.4314 -0.0628 0.059 Uiso 1 calc R . . H14B H -0.2401 -0.5373 -0.0167 0.059 Uiso 1 calc R . . C15 C -0.3206(6) -0.4062(5) -0.0265(4) 0.0457(18) Uani 1 d . . . H15A H -0.3802 -0.4323 0.0165 0.055 Uiso 1 calc R . . H15B H -0.3674 -0.4413 -0.0793 0.055 Uiso 1 calc R . . C16 C -0.2779(5) -0.2721(5) -0.0222(4) 0.0371(17) Uani 1 d . . . H16A H -0.3544 -0.2463 -0.0248 0.044 Uiso 1 calc R . . H16B H -0.2278 -0.2468 -0.0696 0.044 Uiso 1 calc R . . N20 N 0.2382(4) -0.0759(4) 0.1568(3) 0.0262(12) Uani 1 d D . . H20 H 0.203(5) -0.106(5) 0.1144(18) 0.031 Uiso 1 d D . . C21 C 0.3052(5) -0.1384(5) 0.2017(3) 0.0226(14) Uani 1 d . . . H21 H 0.2878 -0.1268 0.2601 0.027 Uiso 1 calc R . . C22 C 0.4503(5) -0.0898(5) 0.1942(4) 0.0361(16) Uani 1 d . . . H22A H 0.4828 -0.0054 0.2170 0.043 Uiso 1 calc R . . H22B H 0.4692 -0.0946 0.1364 0.043 Uiso 1 calc R . . C23 C 0.5191(6) -0.1598(6) 0.2389(4) 0.0483(19) Uani 1 d . . . H23A H 0.6122 -0.1283 0.2314 0.058 Uiso 1 calc R . . H23B H 0.5066 -0.1489 0.2975 0.058 Uiso 1 calc R . . C24 C 0.4700(6) -0.2906(6) 0.2089(4) 0.0485(19) Uani 1 d . . . H24A H 0.5138 -0.3335 0.2406 0.058 Uiso 1 calc R . . H24B H 0.4887 -0.3029 0.1514 0.058 Uiso 1 calc R . . C25 C 0.3264(6) -0.3386(5) 0.2176(4) 0.0417(17) Uani 1 d . . . H25A H 0.3091 -0.3330 0.2756 0.050 Uiso 1 calc R . . H25B H 0.2939 -0.4233 0.1955 0.050 Uiso 1 calc R . . C26 C 0.2556(5) -0.2706(5) 0.1734(4) 0.0322(15) Uani 1 d . . . H26A H 0.2657 -0.2832 0.1146 0.039 Uiso 1 calc R . . H26B H 0.1631 -0.3020 0.1826 0.039 Uiso 1 calc R . . N30 N -0.1495(4) -0.2091(4) 0.2906(3) 0.0266(12) Uani 1 d D . . H30 H -0.184(5) -0.242(4) 0.2479(19) 0.032 Uiso 1 d D . . C31 C -0.1245(5) -0.2826(5) 0.3494(3) 0.0256(14) Uani 1 d . . . H31 H -0.1132 -0.2367 0.4043 0.031 Uiso 1 calc R . . C32 C -0.0041(6) -0.3156(5) 0.3351(4) 0.0379(17) Uani 1 d . . . H32A H 0.0711 -0.2426 0.3383 0.045 Uiso 1 calc R . . H32B H -0.0115 -0.3584 0.2802 0.045 Uiso 1 calc R . . C33 C 0.0158(6) -0.3937(5) 0.3976(4) 0.0442(18) Uani 1 d . . . H33A H 0.0946 -0.4139 0.3873 0.053 Uiso 1 calc R . . H33B H 0.0266 -0.3500 0.4524 0.053 Uiso 1 calc R . . C34 C -0.0972(6) -0.5052(5) 0.3932(4) 0.0414(17) Uani 1 d . . . H34A H -0.0841 -0.5548 0.4344 0.050 Uiso 1 calc R . . H34B H -0.1051 -0.5508 0.3393 0.050 Uiso 1 calc R . . C35 C -0.2183(6) -0.4759(5) 0.4076(4) 0.0472(19) Uani 1 d . . . H35A H -0.2136 -0.4379 0.4637 0.057 Uiso 1 calc R . . H35B H -0.2923 -0.5501 0.4015 0.057 Uiso 1 calc R . . C36 C -0.2394(6) -0.3938(5) 0.3493(4) 0.0431(18) Uani 1 d . . . H36A H -0.3153 -0.3712 0.3642 0.052 Uiso 1 calc R . . H36B H -0.2574 -0.4365 0.2940 0.052 Uiso 1 calc R . . N40 N -0.0930(4) 0.1370(4) 0.1117(3) 0.0249(12) Uani 1 d D . . H40 H -0.031(3) 0.193(3) 0.125(3) 0.030 Uiso 1 d D . . C41 C -0.2152(5) 0.1579(5) 0.1276(3) 0.0229(14) Uani 1 d . . . H41 H -0.2709 0.0891 0.1533 0.027 Uiso 1 calc R . . C42 C -0.1937(5) 0.2680(5) 0.1856(4) 0.0382(17) Uani 1 d . . . H42A H -0.1368 0.3372 0.1620 0.046 Uiso 1 calc R . . H42B H -0.1507 0.2604 0.2366 0.046 Uiso 1 calc R . . C43 C -0.3197(6) 0.2881(6) 0.2034(4) 0.0432(18) Uani 1 d . . . H43A H -0.3742 0.2216 0.2305 0.052 Uiso 1 calc R . . H43B H -0.3029 0.3619 0.2407 0.052 Uiso 1 calc R . . C44 C -0.3903(6) 0.2977(6) 0.1264(4) 0.0439(18) Uani 1 d . . . H44A H -0.4742 0.3063 0.1394 0.053 Uiso 1 calc R . . H44B H -0.3399 0.3690 0.1021 0.053 Uiso 1 calc R . . C45 C -0.4111(6) 0.1889(6) 0.0665(4) 0.0451(19) Uani 1 d . . . H45A H -0.4510 0.1996 0.0153 0.054 Uiso 1 calc R . . H45B H -0.4708 0.1193 0.0882 0.054 Uiso 1 calc R . . C46 C -0.2846(6) 0.1653(6) 0.0494(3) 0.0400(17) Uani 1 d . . . H46A H -0.3028 0.0900 0.0136 0.048 Uiso 1 calc R . . H46B H -0.2291 0.2298 0.0211 0.048 Uiso 1 calc R . . N50 N 0.2865(4) 0.1221(4) 0.2414(3) 0.0244(12) Uani 1 d D . . H50 H 0.337(4) 0.146(5) 0.208(2) 0.029 Uiso 1 d D . . C51 C 0.2734(5) 0.2137(5) 0.3031(3) 0.0248(14) Uani 1 d . . . H51 H 0.2197 0.1719 0.3454 0.030 Uiso 1 calc R . . C52 C 0.2077(6) 0.2954(6) 0.2720(4) 0.0445(18) Uani 1 d . . . H52A H 0.1200 0.2480 0.2500 0.053 Uiso 1 calc R . . H52B H 0.2556 0.3344 0.2274 0.053 Uiso 1 calc R . . C53 C 0.2000(7) 0.3895(6) 0.3381(4) 0.0484(19) Uani 1 d . . . H53A H 0.1608 0.4434 0.3148 0.058 Uiso 1 calc R . . H53B H 0.1442 0.3510 0.3799 0.058 Uiso 1 calc R . . C54 C 0.3298(6) 0.4601(6) 0.3766(4) 0.0463(19) Uani 1 d . . . H54A H 0.3210 0.5179 0.4210 0.056 Uiso 1 calc R . . H54B H 0.3833 0.5048 0.3361 0.056 Uiso 1 calc R . . C55 C 0.3948(6) 0.3789(6) 0.4099(4) 0.0463(19) Uani 1 d . . . H55A H 0.4819 0.4264 0.4327 0.056 Uiso 1 calc R . . H55B H 0.3454 0.3399 0.4539 0.056 Uiso 1 calc R . . C56 C 0.4039(3) 0.2855(3) 0.34412(17) 0.0398(17) Uani 1 d . . . H56A H 0.4422 0.2314 0.3680 0.048 Uiso 1 calc R . . H56B H 0.4612 0.3244 0.3031 0.048 Uiso 1 calc R . . N60 N -0.0765(3) -0.0044(3) 0.37247(17) 0.0288(12) Uani 1 d RD . . H60 H -0.0132 0.0441 0.3923 0.035 Uiso 1 d RD . . C61 C -0.1940(3) 0.0059(3) 0.40693(17) 0.0256(14) Uani 1 d R . . H61 H -0.2674 -0.0624 0.3809 0.031 Uiso 1 calc R . . C62 C -0.1890(6) -0.0047(6) 0.4969(3) 0.0388(17) Uani 1 d . . . H62A H -0.1834 -0.0834 0.5052 0.047 Uiso 1 calc R . . H62B H -0.1108 0.0562 0.5230 0.047 Uiso 1 calc R . . C63 C -0.3054(6) 0.0107(6) 0.5370(4) 0.0444(18) Uani 1 d . . . H63A H -0.3825 -0.0563 0.5162 0.053 Uiso 1 calc R . . H63B H -0.2945 0.0090 0.5960 0.053 Uiso 1 calc R . . C64 C -0.3253(6) 0.1256(7) 0.5217(4) 0.055(2) Uani 1 d . . . H64A H -0.2530 0.1932 0.5479 0.066 Uiso 1 calc R . . H64B H -0.4052 0.1299 0.5456 0.066 Uiso 1 calc R . . C65 C -0.3341(6) 0.1338(6) 0.4316(4) 0.0503(19) Uani 1 d . . . H65A H -0.3415 0.2117 0.4228 0.060 Uiso 1 calc R . . H65B H -0.4126 0.0717 0.4068 0.060 Uiso 1 calc R . . C66 C -0.2185(6) 0.1189(6) 0.3898(4) 0.0397(17) Uani 1 d . . . H66A H -0.2325 0.1176 0.3308 0.048 Uiso 1 calc R . . H66B H -0.1418 0.1877 0.4085 0.048 Uiso 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 0.0229(9) 0.0243(10) 0.0229(9) 0.0026(7) -0.0012(7) 0.0098(7) P2 0.0225(9) 0.0246(10) 0.0240(9) 0.0023(7) 0.0006(7) 0.0106(7) P3 0.0203(9) 0.0260(9) 0.0227(9) 0.0030(7) -0.0007(7) 0.0073(7) N1 0.020(3) 0.028(3) 0.025(3) 0.007(2) 0.002(2) 0.006(2) N2 0.024(3) 0.027(3) 0.024(3) 0.005(2) 0.002(2) 0.013(2) N3 0.022(3) 0.025(3) 0.026(3) 0.006(2) 0.002(2) 0.010(2) N10 0.026(3) 0.033(3) 0.020(3) 0.002(2) -0.002(2) 0.011(2) C11 0.026(3) 0.022(4) 0.025(3) 0.004(3) 0.004(3) 0.008(3) C12 0.032(4) 0.021(4) 0.032(4) -0.001(3) -0.002(3) 0.008(3) C13 0.055(4) 0.029(4) 0.034(4) -0.003(3) -0.004(3) 0.015(3) C14 0.068(5) 0.020(4) 0.049(5) -0.010(3) 0.001(4) 0.004(4) C15 0.037(4) 0.035(4) 0.048(4) -0.012(3) -0.006(3) -0.007(3) C16 0.026(4) 0.039(4) 0.040(4) -0.002(3) -0.007(3) 0.005(3) N20 0.028(3) 0.030(3) 0.023(3) -0.002(2) -0.009(2) 0.016(3) C21 0.021(3) 0.023(4) 0.023(3) -0.001(3) 0.003(3) 0.008(3) C22 0.020(3) 0.036(4) 0.050(4) 0.010(3) 0.005(3) 0.005(3) C23 0.024(4) 0.059(5) 0.067(5) 0.012(4) 0.000(3) 0.020(4) C24 0.048(5) 0.055(5) 0.060(5) 0.016(4) 0.005(4) 0.039(4) C25 0.045(4) 0.037(4) 0.044(4) 0.005(3) -0.003(3) 0.014(3) C26 0.031(4) 0.028(4) 0.037(4) 0.004(3) -0.001(3) 0.009(3) N30 0.027(3) 0.026(3) 0.025(3) 0.007(2) -0.004(2) 0.006(2) C31 0.034(4) 0.026(4) 0.018(3) 0.002(3) 0.002(3) 0.011(3) C32 0.038(4) 0.038(4) 0.042(4) 0.015(3) 0.000(3) 0.015(3) C33 0.048(4) 0.031(4) 0.057(5) 0.011(4) -0.014(4) 0.016(4) C34 0.065(5) 0.026(4) 0.035(4) 0.009(3) -0.011(3) 0.017(4) C35 0.049(5) 0.029(4) 0.064(5) 0.021(4) 0.014(4) 0.008(4) C36 0.032(4) 0.033(4) 0.067(5) 0.018(4) 0.010(3) 0.010(3) N40 0.022(3) 0.022(3) 0.030(3) 0.000(2) -0.001(2) 0.006(2) C41 0.025(3) 0.022(3) 0.025(3) -0.001(3) 0.000(3) 0.012(3) C42 0.037(4) 0.043(4) 0.035(4) -0.005(3) -0.002(3) 0.017(3) C43 0.043(4) 0.046(5) 0.038(4) -0.021(3) -0.001(3) 0.019(4) C44 0.041(4) 0.042(4) 0.055(5) 0.013(4) 0.013(4) 0.021(4) C45 0.041(4) 0.071(5) 0.036(4) 0.003(4) -0.005(3) 0.037(4) C46 0.044(4) 0.062(5) 0.022(3) -0.003(3) -0.006(3) 0.030(4) N50 0.022(3) 0.030(3) 0.022(3) -0.002(2) 0.004(2) 0.009(2) C51 0.025(3) 0.021(3) 0.027(3) -0.003(3) 0.002(3) 0.007(3) C52 0.057(5) 0.039(4) 0.043(4) -0.011(3) -0.010(3) 0.028(4) C53 0.070(5) 0.039(4) 0.045(4) -0.005(4) -0.006(4) 0.033(4) C54 0.068(5) 0.034(4) 0.038(4) -0.001(3) 0.016(4) 0.017(4) C55 0.036(4) 0.055(5) 0.039(4) -0.019(4) -0.004(3) 0.010(4) C56 0.032(4) 0.043(4) 0.041(4) -0.007(3) -0.002(3) 0.012(3) N60 0.023(3) 0.037(3) 0.022(3) -0.003(2) -0.001(2) 0.005(2) C61 0.020(3) 0.035(4) 0.021(3) 0.001(3) -0.002(3) 0.008(3) C62 0.036(4) 0.057(5) 0.028(4) 0.007(3) 0.001(3) 0.020(3) C63 0.033(4) 0.066(5) 0.030(4) -0.007(4) 0.002(3) 0.013(4) C64 0.036(4) 0.075(6) 0.047(5) -0.021(4) 0.009(3) 0.015(4) C65 0.043(4) 0.050(5) 0.069(5) 0.007(4) 0.014(4) 0.030(4) C66 0.035(4) 0.047(5) 0.043(4) 0.013(3) 0.007(3) 0.020(3) _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 N3 1.596(4) . y P1 N1 1.609(4) . y P1 N10 1.657(5) . y P1 N40 1.662(5) . y P2 N2 1.593(4) . y P2 N1 1.599(4) . y P2 N20 1.650(5) . y P2 N50 1.660(5) . y P3 N3 1.597(4) . y P3 N2 1.597(4) . y P3 N60 1.638(3) . y P3 N30 1.654(5) . y N10 C11 1.470(7) . ? C11 C12 1.516(7) . ? C11 C16 1.530(7) . ? C12 C13 1.515(7) . ? C13 C14 1.520(8) . ? C14 C15 1.505(8) . ? C15 C16 1.518(8) . ? N20 C21 1.453(7) . ? C21 C26 1.521(7) . ? C21 C22 1.532(7) . ? C22 C23 1.532(8) . ? C23 C24 1.513(8) . ? C24 C25 1.519(8) . ? C25 C26 1.524(7) . ? N30 C31 1.461(7) . ? C31 C36 1.516(7) . ? C31 C32 1.522(7) . ? C32 C33 1.525(8) . ? C33 C34 1.501(8) . ? C34 C35 1.506(8) . ? C35 C36 1.515(8) . ? N40 C41 1.475(7) . ? C41 C42 1.504(7) . ? C41 C46 1.519(7) . ? C42 C43 1.518(7) . ? C43 C44 1.518(8) . ? C44 C45 1.512(8) . ? C45 C46 1.538(7) . ? N50 C51 1.471(7) . ? C51 C52 1.516(7) . ? C51 C56 1.522(6) . ? C52 C53 1.521(8) . ? C53 C54 1.499(8) . ? C54 C55 1.520(8) . ? C55 C56 1.515(6) . ? N60 C61 1.4662 . ? C61 C62 1.518(6) . ? C61 C66 1.518(6) . ? C62 C63 1.517(8) . ? C63 C64 1.510(9) . ? C64 C65 1.516(9) . ? C65 C66 1.519(8) . ? 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 N3 P1 N1 116.4(2) . . y N3 P1 N10 105.7(2) . . ? N1 P1 N10 114.8(2) . . ? N3 P1 N40 112.4(2) . . ? N1 P1 N40 104.8(2) . . ? N10 P1 N40 101.9(2) . . y N2 P2 N1 116.4(2) . . y N2 P2 N20 114.2(2) . . ? N1 P2 N20 105.4(2) . . ? N2 P2 N50 104.5(2) . . ? N1 P2 N50 115.8(2) . . ? N20 P2 N50 99.6(2) . . y N3 P3 N2 116.2(2) . . y N3 P3 N60 115.3(2) . . ? N2 P3 N60 103.6(2) . . ? N3 P3 N30 103.4(2) . . ? N2 P3 N30 115.9(2) . . ? N60 P3 N30 101.9(2) . . y P2 N1 P1 123.2(3) . . y P2 N2 P3 124.0(3) . . y P1 N3 P3 123.6(3) . . y C11 N10 P1 121.6(4) . . ? N10 C11 C12 114.6(4) . . ? N10 C11 C16 108.4(4) . . ? C12 C11 C16 110.9(5) . . ? C13 C12 C11 112.6(5) . . ? C12 C13 C14 111.1(5) . . ? C15 C14 C13 111.0(5) . . ? C14 C15 C16 111.6(5) . . ? C15 C16 C11 112.1(5) . . ? C21 N20 P2 122.9(4) . . ? N20 C21 C26 110.7(4) . . ? N20 C21 C22 111.7(5) . . ? C26 C21 C22 110.0(5) . . ? C21 C22 C23 111.1(5) . . ? C24 C23 C22 112.0(5) . . ? C23 C24 C25 109.5(5) . . ? C24 C25 C26 111.6(5) . . ? C21 C26 C25 112.2(5) . . ? C31 N30 P3 126.2(4) . . ? N30 C31 C36 109.7(4) . . ? N30 C31 C32 113.4(4) . . ? C36 C31 C32 109.9(5) . . ? C31 C32 C33 111.0(5) . . ? C34 C33 C32 110.1(5) . . ? C33 C34 C35 110.3(5) . . ? C34 C35 C36 112.0(5) . . ? C35 C36 C31 112.4(5) . . ? C41 N40 P1 120.4(4) . . ? N40 C41 C42 110.9(4) . . ? N40 C41 C46 111.0(4) . . ? C42 C41 C46 110.8(5) . . ? C41 C42 C43 110.9(5) . . ? C44 C43 C42 111.2(5) . . ? C45 C44 C43 110.5(5) . . ? C44 C45 C46 111.9(5) . . ? C41 C46 C45 110.8(5) . . ? C51 N50 P2 122.5(4) . . ? N50 C51 C52 114.5(4) . . ? N50 C51 C56 110.2(4) . . ? C52 C51 C56 110.3(4) . . ? C51 C52 C53 111.8(5) . . ? C54 C53 C52 111.6(6) . . ? C53 C54 C55 110.5(5) . . ? C56 C55 C54 110.9(5) . . ? C55 C56 C51 112.1(4) . . ? C61 N60 P3 126.52(12) . . ? N60 C61 C62 109.8(2) . . ? N60 C61 C66 112.5(3) . . ? C62 C61 C66 111.6(4) . . ? C63 C62 C61 112.4(4) . . ? C64 C63 C62 112.0(6) . . ? C63 C64 C65 110.3(6) . . ? C64 C65 C66 112.5(5) . . ? C61 C66 C65 112.1(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 P2 N1 P1 -2.2(4) . . . . y N20 P2 N1 P1 125.5(3) . . . . ? N50 P2 N1 P1 -125.6(3) . . . . ? N3 P1 N1 P2 4.0(4) . . . . y N10 P1 N1 P2 -120.2(3) . . . . ? N40 P1 N1 P2 128.9(3) . . . . ? N1 P2 N2 P3 1.7(4) . . . . y N20 P2 N2 P3 -121.5(3) . . . . ? N50 P2 N2 P3 130.8(3) . . . . ? N3 P3 N2 P2 -3.1(4) . . . . y N60 P3 N2 P2 -130.7(3) . . . . ? N30 P3 N2 P2 118.6(3) . . . . ? N1 P1 N3 P3 -5.6(4) . . . . y N10 P1 N3 P3 123.2(3) . . . . ? N40 P1 N3 P3 -126.5(3) . . . . ? N2 P3 N3 P1 5.2(4) . . . . y N60 P3 N3 P1 126.7(3) . . . . ? N30 P3 N3 P1 -122.9(3) . . . . ? N3 P1 N10 C11 -46.0(5) . . . . ? N1 P1 N10 C11 83.7(5) . . . . ? N40 P1 N10 C11 -163.6(4) . . . . ? P1 N10 C11 C12 -58.0(6) . . . . ? P1 N10 C11 C16 177.5(4) . . . . ? N10 C11 C12 C13 -176.1(5) . . . . ? C16 C11 C12 C13 -52.9(6) . . . . ? C11 C12 C13 C14 55.0(7) . . . . ? C12 C13 C14 C15 -55.9(7) . . . . ? C13 C14 C15 C16 56.0(7) . . . . ? C14 C15 C16 C11 -54.6(7) . . . . ? N10 C11 C16 C15 179.1(5) . . . . ? C12 C11 C16 C15 52.5(7) . . . . ? N2 P2 N20 C21 -39.5(5) . . . . ? N1 P2 N20 C21 -168.5(4) . . . . ? N50 P2 N20 C21 71.3(5) . . . . ? P2 N20 C21 C26 124.1(5) . . . . ? P2 N20 C21 C22 -113.0(5) . . . . ? N20 C21 C22 C23 -177.7(5) . . . . ? C26 C21 C22 C23 -54.3(7) . . . . ? C21 C22 C23 C24 56.9(7) . . . . ? C22 C23 C24 C25 -57.0(7) . . . . ? C23 C24 C25 C26 56.3(7) . . . . ? N20 C21 C26 C25 178.4(5) . . . . ? C22 C21 C26 C25 54.5(6) . . . . ? C24 C25 C26 C21 -56.3(7) . . . . ? N3 P3 N30 C31 -178.9(4) . . . . ? N2 P3 N30 C31 52.7(5) . . . . ? N60 P3 N30 C31 -59.0(5) . . . . ? P3 N30 C31 C36 166.9(4) . . . . ? P3 N30 C31 C32 -69.8(6) . . . . ? N30 C31 C32 C33 -179.2(5) . . . . ? C36 C31 C32 C33 -56.0(6) . . . . ? C31 C32 C33 C34 59.4(7) . . . . ? C32 C33 C34 C35 -58.5(7) . . . . ? C33 C34 C35 C36 55.8(7) . . . . ? C34 C35 C36 C31 -53.6(7) . . . . ? N30 C31 C36 C35 178.4(5) . . . . ? C32 C31 C36 C35 53.0(7) . . . . ? N3 P1 N40 C41 -37.2(5) . . . . ? N1 P1 N40 C41 -164.5(4) . . . . ? N10 P1 N40 C41 75.5(4) . . . . ? P1 N40 C41 C42 122.3(4) . . . . ? P1 N40 C41 C46 -114.0(5) . . . . ? N40 C41 C42 C43 -178.7(5) . . . . ? C46 C41 C42 C43 57.5(7) . . . . ? C41 C42 C43 C44 -57.9(7) . . . . ? C42 C43 C44 C45 56.0(7) . . . . ? C43 C44 C45 C46 -54.5(7) . . . . ? N40 C41 C46 C45 -179.2(5) . . . . ? C42 C41 C46 C45 -55.5(7) . . . . ? C44 C45 C46 C41 54.5(7) . . . . ? N2 P2 N50 C51 -48.2(5) . . . . ? N1 P2 N50 C51 81.2(5) . . . . ? N20 P2 N50 C51 -166.5(4) . . . . ? P2 N50 C51 C52 -70.0(6) . . . . ? P2 N50 C51 C56 165.0(3) . . . . ? N50 C51 C52 C53 -178.7(5) . . . . ? C56 C51 C52 C53 -53.8(7) . . . . ? C51 C52 C53 C54 56.0(7) . . . . ? C52 C53 C54 C55 -56.5(7) . . . . ? C53 C54 C55 C56 56.4(7) . . . . ? C54 C55 C56 C51 -55.9(6) . . . . ? N50 C51 C56 C55 -178.4(4) . . . . ? C52 C51 C56 C55 54.2(6) . . . . ? N3 P3 N60 C61 46.8(2) . . . . ? N2 P3 N60 C61 174.94(17) . . . . ? N30 P3 N60 C61 -64.4(2) . . . . ? P3 N60 C61 C62 143.5(4) . . . . ? P3 N60 C61 C66 -91.7(3) . . . . ? N60 C61 C62 C63 177.4(4) . . . . ? C66 C61 C62 C63 52.1(6) . . . . ? C61 C62 C63 C64 -54.7(7) . . . . ? C62 C63 C64 C65 55.4(7) . . . . ? C63 C64 C65 C66 -55.2(8) . . . . ? N60 C61 C66 C65 -175.3(4) . . . . ? C62 C61 C66 C65 -51.4(6) . . . . ? C64 C65 C66 C61 53.7(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N10 H10 N1 0.797(18) 2.45(2) 3.248(6) 175(6) 2 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.267 _refine_diff_density_min -0.272 _refine_diff_density_rms 0.068 data_2a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C79 H146 Li6 N18 P6' _chemical_formula_weight 1575.60 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 '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 25.993(5) _cell_length_b 17.674(4) _cell_length_c 20.639(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.81(3) _cell_angle_gamma 90.00 _cell_volume 8920(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.173 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3416 _exptl_absorpt_coefficient_mu 0.172 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 Stoe-IPDS _diffrn_measurement_method 'image plate' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12766 _diffrn_reflns_av_R_equivalents 0.1213 _diffrn_reflns_av_sigmaI/netI 0.1175 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 22.37 _reflns_number_total 5676 _reflns_number_gt 2919 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5676 _refine_ls_number_parameters 623 _refine_ls_number_restraints 1329 _refine_ls_R_factor_all 0.1117 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.2098 _refine_ls_wR_factor_gt 0.1991 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 1.019 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.25219(7) 0.16583(9) 0.11570(9) 0.0345(5) Uani 1 d . . . P2 P 0.33803(7) 0.15393(9) 0.06003(9) 0.0343(5) Uani 1 d . . . P3 P 0.23314(7) 0.09195(9) -0.01434(9) 0.0337(5) Uani 1 d . . . N1 N 0.31059(19) 0.1966(3) 0.1110(3) 0.0354(13) Uani 1 d . . . N2 N 0.29266(19) 0.1251(3) -0.0113(3) 0.0316(13) Uani 1 d . . . N3 N 0.2117(2) 0.1329(3) 0.0433(3) 0.0361(13) Uani 1 d . . . N10 N 0.2287(2) 0.2401(3) 0.1421(3) 0.0365(13) Uani 1 d . . . N20 N 0.37595(19) 0.2099(3) 0.0337(3) 0.0367(13) Uani 1 d . . . N30 N 0.1847(2) 0.1097(3) -0.0858(3) 0.0375(13) Uani 1 d . . . N40 N 0.2615(2) 0.0957(3) 0.1724(3) 0.0438(15) Uani 1 d D . . H40 H 0.245(3) 0.057(3) 0.159(4) 0.053 Uiso 1 d D . . N50 N 0.3738(2) 0.0818(3) 0.1066(3) 0.0413(14) Uani 1 d D . . H50 H 0.374(3) 0.081(4) 0.146(2) 0.050 Uiso 1 d D . . N60 N 0.2432(2) -0.0002(3) -0.0024(3) 0.0411(14) Uani 1 d D . . H60 H 0.2750(18) -0.012(4) 0.013(3) 0.049 Uiso 1 d D . . Li1 Li 0.2917(5) 0.3008(6) 0.1298(6) 0.047(3) Uani 1 d . . . Li2 Li 0.3215(5) 0.1975(6) -0.0629(6) 0.044(3) Uani 1 d . . . Li3 Li 0.1516(4) 0.1829(6) -0.0343(6) 0.047(3) Uani 1 d . . . C11 C 0.1946(2) 0.2314(4) 0.1862(3) 0.0418(17) Uani 1 d DU . . H11 H 0.2025 0.1808 0.2091 0.050 Uiso 1 calc R . . C12 C 0.1338(3) 0.2361(5) 0.1460(4) 0.070(2) Uani 1 d DU . . H12A H 0.1239 0.1968 0.1097 0.084 Uiso 1 calc R . . H12B H 0.1254 0.2861 0.1233 0.084 Uiso 1 calc R . . C13 C 0.0996(3) 0.2249(6) 0.1932(4) 0.085(3) Uani 1 d DU . . H13A H 0.0603 0.2296 0.1657 0.101 Uiso 1 calc R . . H13B H 0.1059 0.1733 0.2131 0.101 Uiso 1 calc R . . C14 C 0.1140(4) 0.2812(6) 0.2494(5) 0.093(3) Uani 1 d DU . . H14A H 0.0937 0.2698 0.2810 0.112 Uiso 1 calc R . . H14B H 0.1029 0.3322 0.2297 0.112 Uiso 1 calc R . . C15 C 0.1740(4) 0.2810(7) 0.2890(5) 0.105(4) Uani 1 d DU . . H15A H 0.1842 0.2326 0.3142 0.126 Uiso 1 calc R . . H15B H 0.1826 0.3225 0.3233 0.126 Uiso 1 calc R . . C16 C 0.2078(3) 0.2914(5) 0.2412(4) 0.083(3) Uani 1 d DU . . H16A H 0.2001 0.3419 0.2192 0.099 Uiso 1 calc R . . H16B H 0.2472 0.2892 0.2688 0.099 Uiso 1 calc R . . C21 C 0.4354(2) 0.2165(4) 0.0723(3) 0.0431(17) Uani 1 d DU . . H21 H 0.4478 0.1678 0.0974 0.052 Uiso 1 calc R . . C22 C 0.4668(3) 0.2276(6) 0.0236(4) 0.086(3) Uani 1 d DU . . H22A H 0.4541 0.2744 -0.0034 0.103 Uiso 1 calc R . . H22B H 0.4595 0.1846 -0.0090 0.103 Uiso 1 calc R . . C23 C 0.5281(3) 0.2331(7) 0.0625(5) 0.104(4) Uani 1 d DU . . H23A H 0.5415 0.1835 0.0838 0.125 Uiso 1 calc R . . H23B H 0.5470 0.2445 0.0292 0.125 Uiso 1 calc R . . C24 C 0.5428(3) 0.2920(5) 0.1170(4) 0.077(3) Uani 1 d DU . . H24A H 0.5343 0.3426 0.0955 0.093 Uiso 1 calc R . . H24B H 0.5825 0.2897 0.1428 0.093 Uiso 1 calc R . . C25 C 0.5119(3) 0.2808(6) 0.1656(4) 0.076(3) Uani 1 d DU . . H25A H 0.5203 0.3224 0.1996 0.091 Uiso 1 calc R . . H25B H 0.5231 0.2325 0.1908 0.091 Uiso 1 calc R . . C26 C 0.4500(3) 0.2793(5) 0.1246(4) 0.072(3) Uani 1 d DU . . H26A H 0.4296 0.2725 0.1569 0.087 Uiso 1 calc R . . H26B H 0.4389 0.3283 0.1008 0.087 Uiso 1 calc R . . C31 C 0.1655(2) 0.0554(4) -0.1430(3) 0.0420(17) Uani 1 d DU . . H31 H 0.1913 0.0115 -0.1325 0.050 Uiso 1 calc R A 1 C32 C 0.1615(10) 0.0866(11) -0.2125(6) 0.067(6) Uani 0.63(3) d PDU . 1 H32A H 0.1986 0.1016 -0.2112 0.081 Uiso 0.63(3) calc PR . 1 H32B H 0.1386 0.1327 -0.2213 0.081 Uiso 0.63(3) calc PR . 1 C33 C 0.1376(12) 0.0315(12) -0.2722(8) 0.081(7) Uani 0.63(3) d PDU . 1 H33A H 0.1342 0.0571 -0.3161 0.097 Uiso 0.63(3) calc PR . 1 H33B H 0.1626 -0.0121 -0.2668 0.097 Uiso 0.63(3) calc PR . 1 C34 C 0.0826(12) 0.0039(11) -0.2746(9) 0.082(7) Uani 0.63(3) d PDU . 1 H34A H 0.0690 -0.0343 -0.3117 0.099 Uiso 0.63(3) calc PR . 1 H34B H 0.0564 0.0466 -0.2853 0.099 Uiso 0.63(3) calc PR . 1 C35 C 0.0858(7) -0.0310(9) -0.2065(9) 0.065(5) Uani 0.63(3) d PDU . 1 H35A H 0.1097 -0.0761 -0.1974 0.078 Uiso 0.63(3) calc PR . 1 H35B H 0.0489 -0.0473 -0.2083 0.078 Uiso 0.63(3) calc PR . 1 C36 C 0.1083(5) 0.0261(10) -0.1490(10) 0.053(5) Uani 0.63(3) d PDU . 1 H36A H 0.1101 0.0024 -0.1048 0.063 Uiso 0.63(3) calc PR . 1 H36B H 0.0828 0.0695 -0.1571 0.063 Uiso 0.63(3) calc PR . 1 C32' C 0.1857(14) 0.0791(18) -0.2008(12) 0.058(8) Uani 0.37(3) d PDU . 2 H32C H 0.2261 0.0820 -0.1828 0.069 Uiso 0.37(3) calc PR . 2 H32D H 0.1715 0.1303 -0.2167 0.069 Uiso 0.37(3) calc PR . 2 C33' C 0.1679(13) 0.0247(19) -0.2617(13) 0.063(7) Uani 0.37(3) d PDU . 2 H33C H 0.1786 0.0459 -0.2997 0.076 Uiso 0.37(3) calc PR . 2 H33D H 0.1872 -0.0240 -0.2478 0.076 Uiso 0.37(3) calc PR . 2 C34' C 0.1077(12) 0.011(2) -0.2870(12) 0.064(8) Uani 0.37(3) d PDU . 2 H34C H 0.0889 0.0564 -0.3119 0.076 Uiso 0.37(3) calc PR . 2 H34D H 0.0995 -0.0316 -0.3203 0.076 Uiso 0.37(3) calc PR . 2 C35' C 0.0853(11) -0.007(3) -0.2312(17) 0.083(10) Uani 0.37(3) d PDU . 2 H35C H 0.0970 -0.0591 -0.2139 0.099 Uiso 0.37(3) calc PR . 2 H35D H 0.0449 -0.0070 -0.2505 0.099 Uiso 0.37(3) calc PR . 2 C36' C 0.1040(6) 0.048(2) -0.1714(15) 0.065(9) Uani 0.37(3) d PDU . 2 H36C H 0.0877 0.0982 -0.1870 0.078 Uiso 0.37(3) calc PR . 2 H36D H 0.0907 0.0306 -0.1343 0.078 Uiso 0.37(3) calc PR . 2 C41 C 0.3007(3) 0.0898(4) 0.2397(4) 0.061(2) Uani 1 d DU . . H41 H 0.3320 0.1223 0.2389 0.074 Uiso 1 calc R B 1 C42 C 0.2904(5) 0.1109(8) 0.3016(5) 0.073(4) Uani 0.673(8) d PDU C 1 H42A H 0.2581 0.0823 0.3033 0.088 Uiso 0.673(8) calc PR C 1 H42B H 0.2808 0.1653 0.2986 0.088 Uiso 0.673(8) calc PR C 1 C43 C 0.3365(5) 0.0978(7) 0.3677(6) 0.081(4) Uani 0.673(8) d PDU C 1 H43A H 0.3244 0.1099 0.4070 0.098 Uiso 0.673(8) calc PR C 1 H43B H 0.3674 0.1318 0.3699 0.098 Uiso 0.673(8) calc PR C 1 C44 C 0.3555(7) 0.0170(9) 0.3730(7) 0.081(5) Uani 0.673(8) d PDU C 1 H44A H 0.3873 0.0105 0.4158 0.098 Uiso 0.673(8) calc PR C 1 H44B H 0.3258 -0.0165 0.3760 0.098 Uiso 0.673(8) calc PR C 1 C45 C 0.3713(5) -0.0057(7) 0.3123(5) 0.076(4) Uani 0.673(8) d PDU C 1 H45A H 0.3820 -0.0597 0.3163 0.091 Uiso 0.673(8) calc PR C 1 H45B H 0.4029 0.0248 0.3111 0.091 Uiso 0.673(8) calc PR C 1 C46 C 0.3231(5) 0.0069(5) 0.2468(5) 0.058(3) Uani 0.673(8) d PDU C 1 H46A H 0.2933 -0.0284 0.2461 0.069 Uiso 0.673(8) calc PR C 1 H46B H 0.3343 -0.0051 0.2067 0.069 Uiso 0.673(8) calc PR C 1 C42' C 0.2737(7) 0.0419(16) 0.2801(10) 0.075(7) Uani 0.327(8) d PDU C 2 H42C H 0.2377 0.0648 0.2746 0.090 Uiso 0.327(8) calc PR C 2 H42D H 0.2665 -0.0087 0.2583 0.090 Uiso 0.327(8) calc PR C 2 C43' C 0.3029(9) 0.0306(18) 0.3554(10) 0.085(8) Uani 0.327(8) d PDU C 2 H43C H 0.2952 0.0743 0.3808 0.102 Uiso 0.327(8) calc PR C 2 H43D H 0.2884 -0.0153 0.3706 0.102 Uiso 0.327(8) calc PR C 2 C44 C 0.3634(10) 0.023(2) 0.3739(16) 0.082(10) Uani 0.327(8) d PDU C 2 H44C H 0.3717 -0.0272 0.3578 0.098 Uiso 0.327(8) calc PR C 2 H44D H 0.3807 0.0241 0.4246 0.098 Uiso 0.327(8) calc PR C 2 C45' C 0.3873(8) 0.0839(17) 0.3427(9) 0.085(8) Uani 0.327(8) d PDU C 2 H45C H 0.4271 0.0751 0.3543 0.102 Uiso 0.327(8) calc PR C 2 H45D H 0.3823 0.1334 0.3622 0.102 Uiso 0.327(8) calc PR C 2 C46' C 0.3602(5) 0.0852(15) 0.2657(9) 0.064(7) Uani 0.327(8) d PDU C 2 H46C H 0.3748 0.1290 0.2475 0.077 Uiso 0.327(8) calc PR C 2 H46D H 0.3711 0.0389 0.2467 0.077 Uiso 0.327(8) calc PR C 2 C51 C 0.4014(3) 0.0201(4) 0.0866(4) 0.054(2) Uani 1 d DU . . H51 H 0.3798 0.0154 0.0365 0.065 Uiso 1 calc R D 1 C52 C 0.4571(4) 0.0202(6) 0.0858(8) 0.062(4) Uani 0.578(10) d PDU E 1 H52A H 0.4820 0.0326 0.1328 0.074 Uiso 0.578(10) calc PR E 1 H52B H 0.4604 0.0613 0.0549 0.074 Uiso 0.578(10) calc PR E 1 C53 C 0.4769(5) -0.0531(6) 0.0631(8) 0.066(4) Uani 0.578(10) d PDU E 1 H53A H 0.4576 -0.0607 0.0132 0.079 Uiso 0.578(10) calc PR E 1 H53B H 0.5165 -0.0492 0.0708 0.079 Uiso 0.578(10) calc PR E 1 C54 C 0.4668(6) -0.1198(8) 0.1018(11) 0.066(6) Uani 0.578(10) d PDU E 1 H54A H 0.4874 -0.1139 0.1516 0.079 Uiso 0.578(10) calc PR E 1 H54B H 0.4795 -0.1666 0.0857 0.079 Uiso 0.578(10) calc PR E 1 C55 C 0.4066(5) -0.1257(6) 0.0904(8) 0.059(4) Uani 0.578(10) d PDU E 1 H55A H 0.3997 -0.1695 0.1162 0.071 Uiso 0.578(10) calc PR E 1 H55B H 0.3862 -0.1338 0.0409 0.071 Uiso 0.578(10) calc PR E 1 C56 C 0.3863(5) -0.0525(5) 0.1148(8) 0.043(3) Uani 0.578(10) d PDU E 1 H56A H 0.3460 -0.0550 0.1014 0.052 Uiso 0.578(10) calc PR E 1 H56B H 0.4015 -0.0506 0.1657 0.052 Uiso 0.578(10) calc PR E 1 C52' C 0.4544(6) 0.0123(10) 0.1526(9) 0.074(6) Uani 0.422(10) d PDU E 2 H52C H 0.4731 0.0620 0.1620 0.088 Uiso 0.422(10) calc PR E 2 H52D H 0.4432 -0.0005 0.1925 0.088 Uiso 0.422(10) calc PR E 2 C53' C 0.4950(6) -0.0469(9) 0.1466(11) 0.075(6) Uani 0.422(10) d PDU E 2 H53C H 0.5135 -0.0286 0.1147 0.091 Uiso 0.422(10) calc PR E 2 H53D H 0.5233 -0.0551 0.1923 0.091 Uiso 0.422(10) calc PR E 2 C54' C 0.4665(10) -0.1200(11) 0.1204(15) 0.084(9) Uani 0.422(10) d PDU E 2 H54C H 0.4528 -0.1419 0.1555 0.101 Uiso 0.422(10) calc PR E 2 H54D H 0.4929 -0.1562 0.1125 0.101 Uiso 0.422(10) calc PR E 2 C55' C 0.4196(8) -0.1085(11) 0.0544(12) 0.077(6) Uani 0.422(10) d PDU E 2 H55C H 0.4015 -0.1577 0.0386 0.093 Uiso 0.422(10) calc PR E 2 H55D H 0.4337 -0.0893 0.0186 0.093 Uiso 0.422(10) calc PR E 2 C56' C 0.3777(6) -0.0526(8) 0.0637(12) 0.061(5) Uani 0.422(10) d PDU E 2 H56C H 0.3474 -0.0466 0.0193 0.073 Uiso 0.422(10) calc PR E 2 H56D H 0.3622 -0.0732 0.0977 0.073 Uiso 0.422(10) calc PR E 2 C61 C 0.2044(3) -0.0590(3) 0.0012(3) 0.0402(17) Uani 1 d DU . . H61 H 0.1667 -0.0406 -0.0249 0.048 Uiso 1 calc R . . C62 C 0.2070(3) -0.0765(4) 0.0737(4) 0.058(2) Uani 1 d DU . . H62A H 0.1970 -0.0306 0.0942 0.069 Uiso 1 calc R . . H62B H 0.2451 -0.0899 0.1016 0.069 Uiso 1 calc R . . C63 C 0.1693(3) -0.1411(4) 0.0772(4) 0.065(2) Uani 1 d DU . . H63A H 0.1750 -0.1528 0.1261 0.078 Uiso 1 calc R . . H63B H 0.1308 -0.1250 0.0552 0.078 Uiso 1 calc R . . C64 C 0.1795(3) -0.2110(4) 0.0420(4) 0.062(2) Uani 1 d DU . . H64A H 0.2161 -0.2314 0.0682 0.075 Uiso 1 calc R . . H64B H 0.1520 -0.2500 0.0417 0.075 Uiso 1 calc R . . C65 C 0.1763(4) -0.1947(4) -0.0304(4) 0.071(2) Uani 1 d DU . . H65A H 0.1383 -0.1810 -0.0581 0.086 Uiso 1 calc R . . H65B H 0.1862 -0.2409 -0.0507 0.086 Uiso 1 calc R . . C66 C 0.2144(3) -0.1305(4) -0.0335(4) 0.062(2) Uani 1 d DU . . H66A H 0.2527 -0.1469 -0.0110 0.075 Uiso 1 calc R . . H66B H 0.2092 -0.1193 -0.0823 0.075 Uiso 1 calc R . . C1T C 0.0177(5) -0.0450(8) -0.0403(7) 0.121(4) Uiso 1 d U . . C2T C 0.0518(5) 0.0095(8) -0.0006(7) 0.132(4) Uiso 1 d U . . C3T C -0.0379(6) -0.0579(9) -0.0419(8) 0.153(5) Uiso 1 d U . . C4T C 0.0269(14) -0.1035(19) -0.0908(17) 0.172(12) Uiso 0.50 d PU . . 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 0.0418(10) 0.0273(9) 0.0372(10) 0.0011(8) 0.0168(8) 0.0021(8) P2 0.0371(10) 0.0275(10) 0.0393(11) 0.0008(8) 0.0143(8) 0.0062(8) P3 0.0396(10) 0.0234(9) 0.0400(11) 0.0005(8) 0.0158(8) 0.0017(8) N1 0.030(3) 0.038(3) 0.043(3) -0.005(3) 0.019(3) -0.004(2) N2 0.029(3) 0.025(3) 0.044(3) -0.002(2) 0.017(3) -0.002(2) N3 0.040(3) 0.038(3) 0.034(3) -0.001(2) 0.018(3) 0.004(3) N10 0.046(3) 0.030(3) 0.039(3) 0.001(3) 0.021(3) 0.008(3) N20 0.028(3) 0.036(3) 0.049(3) 0.003(3) 0.016(3) 0.005(2) N30 0.043(3) 0.033(3) 0.032(3) -0.005(2) 0.008(3) -0.007(3) N40 0.058(4) 0.032(3) 0.041(4) 0.009(3) 0.015(3) -0.004(3) N50 0.053(3) 0.032(3) 0.040(4) 0.005(3) 0.017(3) 0.016(3) N60 0.039(3) 0.031(3) 0.054(4) 0.001(3) 0.016(3) 0.005(3) Li1 0.061(7) 0.033(6) 0.055(8) -0.001(6) 0.030(6) 0.005(6) Li2 0.051(7) 0.040(7) 0.044(7) -0.001(5) 0.021(6) 0.006(5) Li3 0.041(6) 0.042(7) 0.057(8) 0.001(6) 0.015(6) 0.019(5) C11 0.056(5) 0.039(4) 0.036(4) 0.002(3) 0.023(4) 0.008(3) C12 0.049(5) 0.108(7) 0.062(5) 0.008(5) 0.031(4) -0.003(5) C13 0.055(5) 0.128(8) 0.086(7) 0.005(6) 0.044(5) -0.009(6) C14 0.088(7) 0.098(7) 0.128(9) -0.017(7) 0.082(7) -0.007(6) C15 0.113(8) 0.136(9) 0.097(8) -0.061(7) 0.075(7) -0.044(7) C16 0.081(6) 0.115(8) 0.071(6) -0.045(6) 0.050(5) -0.029(6) C21 0.039(4) 0.041(4) 0.050(4) -0.002(3) 0.016(3) -0.008(3) C22 0.043(5) 0.150(9) 0.069(6) -0.026(6) 0.025(4) -0.006(5) C23 0.037(5) 0.196(11) 0.086(7) -0.043(8) 0.029(5) -0.023(6) C24 0.046(5) 0.103(7) 0.080(7) -0.002(6) 0.017(5) -0.020(5) C25 0.044(5) 0.113(7) 0.069(6) -0.031(5) 0.016(4) -0.015(5) C26 0.038(5) 0.109(7) 0.072(6) -0.034(5) 0.021(4) -0.011(5) C31 0.047(4) 0.034(4) 0.042(4) -0.001(3) 0.012(3) 0.008(3) C32 0.090(14) 0.064(10) 0.036(8) 0.002(7) 0.006(8) -0.012(10) C33 0.104(19) 0.078(11) 0.053(10) -0.004(8) 0.017(12) -0.013(14) C34 0.108(15) 0.063(9) 0.054(11) 0.003(9) -0.001(12) -0.020(11) C35 0.069(9) 0.044(9) 0.058(11) -0.004(8) -0.010(8) -0.002(7) C36 0.040(8) 0.039(9) 0.065(10) -0.002(8) -0.001(6) -0.005(6) C32' 0.077(18) 0.053(14) 0.041(14) 0.000(11) 0.016(12) -0.004(14) C33' 0.073(17) 0.074(14) 0.054(14) -0.012(11) 0.037(13) -0.017(14) C34' 0.054(18) 0.073(16) 0.065(15) -0.012(13) 0.022(14) -0.006(15) C35' 0.077(15) 0.088(19) 0.07(2) -0.017(18) 0.015(16) -0.007(15) C36' 0.056(13) 0.079(18) 0.051(15) -0.031(14) 0.007(11) 0.011(12) C41 0.070(5) 0.057(5) 0.047(5) 0.017(4) 0.008(4) -0.007(4) C42 0.071(8) 0.081(9) 0.052(8) -0.028(7) 0.001(7) 0.020(7) C43 0.092(9) 0.081(9) 0.062(8) -0.022(7) 0.013(7) 0.019(8) C44 0.068(10) 0.104(11) 0.067(10) 0.025(9) 0.016(8) 0.020(9) C45 0.083(9) 0.066(8) 0.065(9) -0.005(7) 0.008(7) 0.021(7) C46 0.079(8) 0.031(6) 0.056(7) 0.007(5) 0.015(6) 0.012(6) C42' 0.057(14) 0.097(17) 0.069(15) 0.017(14) 0.020(12) -0.022(13) C43' 0.061(14) 0.112(17) 0.076(15) 0.041(14) 0.015(12) -0.018(13) C44 0.070(16) 0.101(17) 0.067(16) 0.019(16) 0.014(15) 0.016(15) C45' 0.069(14) 0.111(17) 0.067(14) 0.004(14) 0.014(12) 0.004(14) C46' 0.037(12) 0.103(16) 0.058(13) 0.003(13) 0.026(10) -0.020(12) C51 0.056(5) 0.050(5) 0.065(5) 0.019(4) 0.033(4) 0.025(4) C52 0.047(8) 0.055(8) 0.102(11) 0.002(8) 0.049(8) 0.004(6) C53 0.048(8) 0.056(9) 0.107(11) -0.006(8) 0.044(8) 0.019(7) C54 0.055(10) 0.049(10) 0.095(12) 0.005(9) 0.028(9) 0.018(9) C55 0.079(9) 0.038(8) 0.066(10) 0.001(7) 0.032(8) 0.009(7) C56 0.053(8) 0.025(6) 0.057(9) -0.001(7) 0.026(7) 0.001(6) C52' 0.071(12) 0.052(11) 0.099(15) 0.000(11) 0.030(11) 0.026(10) C53' 0.059(11) 0.069(12) 0.090(13) -0.001(11) 0.014(10) 0.025(10) C54' 0.077(15) 0.047(14) 0.131(18) 0.014(13) 0.038(13) 0.024(13) C55' 0.072(13) 0.040(11) 0.124(16) -0.022(12) 0.040(12) 0.021(10) C56' 0.063(11) 0.036(10) 0.087(14) -0.019(11) 0.029(11) 0.007(9) C61 0.042(4) 0.022(4) 0.058(5) -0.003(3) 0.020(4) -0.002(3) C62 0.076(5) 0.048(5) 0.061(5) -0.007(4) 0.039(4) -0.016(4) C63 0.089(6) 0.043(5) 0.079(6) 0.000(4) 0.050(5) -0.016(4) C64 0.078(6) 0.021(4) 0.100(7) 0.003(4) 0.046(5) -0.007(4) C65 0.100(7) 0.045(5) 0.080(6) -0.014(4) 0.045(5) -0.023(5) C66 0.096(6) 0.035(4) 0.070(6) -0.006(4) 0.045(5) -0.006(4) _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 N3 1.617(5) . y P1 N10 1.618(5) . y P1 N1 1.646(5) . y P1 N40 1.666(6) . y P1 Li1 2.574(11) . ? P1 Li2 3.045(11) 7 ? P2 N20 1.615(5) . y P2 N2 1.625(5) . y P2 N1 1.641(5) . y P2 N50 1.675(5) . y P2 Li2 2.545(11) . ? P2 Li3 2.962(12) 7 ? P3 N30 1.612(5) . y P3 N2 1.636(5) . y P3 N3 1.644(5) . y P3 N60 1.654(6) . y P3 Li3 2.579(10) . ? P3 Li1 2.940(12) 7 ? N1 Li1 1.979(12) . y N2 Li2 1.969(12) . y N3 Li3 2.022(12) . y N10 C11 1.478(8) . ? N10 Li2 2.035(12) 7 y N10 Li1 2.043(12) . y N20 C21 1.483(8) . ? N20 Li2 2.029(12) . y N20 Li3 2.028(11) 7 y N30 C31 1.471(8) . ? N30 Li1 2.020(12) 7 y N30 Li3 2.040(12) . y N40 C41 1.420(9) . ? N50 C51 1.441(8) . ? N60 C61 1.466(8) . ? Li1 N30 2.020(12) 7 ? Li1 C32' 2.53(3) 7 ? Li1 C32 2.64(2) 7 ? Li1 C31 2.750(13) 7 ? Li1 Li2 2.794(16) 7 ? Li1 Li3 2.847(16) 7 ? Li1 P3 2.940(12) 7 ? Li2 N10 2.035(12) 7 ? Li2 C12 2.648(13) 7 ? Li2 C11 2.739(13) 7 ? Li2 Li1 2.794(16) 7 ? Li2 Li3 2.834(16) 7 ? Li2 P1 3.045(11) 7 ? Li3 N20 2.028(11) 7 ? Li3 C26 2.750(13) 7 ? Li3 C21 2.773(12) 7 ? Li3 Li2 2.834(16) 7 ? Li3 Li1 2.847(16) 7 ? Li3 P2 2.962(12) 7 ? C11 C16 1.505(8) . ? C11 C12 1.518(8) . ? C11 Li2 2.739(13) 7 ? C12 C13 1.539(8) . ? C12 Li2 2.648(13) 7 ? C13 C14 1.477(10) . ? C14 C15 1.496(10) . ? C15 C16 1.538(9) . ? C21 C26 1.503(8) . ? C21 C22 1.508(8) . ? C21 Li3 2.773(12) 7 ? C22 C23 1.526(9) . ? C23 C24 1.484(10) . ? C24 C25 1.494(9) . ? C25 C26 1.544(8) . ? C26 Li3 2.750(13) 7 ? C31 C32 1.507(12) . ? C31 C36' 1.510(14) . ? C31 C32' 1.515(14) . ? C31 C36 1.540(11) . ? C31 Li1 2.750(13) 7 ? C32 C33 1.528(13) . ? C32 Li1 2.64(2) 7 ? C33 C34 1.496(13) . ? C34 C35 1.512(13) . ? C35 C36 1.515(12) . ? C32' C33' 1.526(14) . ? C32' Li1 2.53(3) 7 ? C33' C34' 1.492(14) . ? C34' C35' 1.491(15) . ? C35' C36' 1.520(14) . ? C41 C42 1.442(10) . ? C41 C46' 1.456(12) . ? C41 C42' 1.520(13) . ? C41 C46 1.566(9) . ? C42 C43 1.498(11) . ? C43 C44 1.501(13) . ? C44 C45 1.499(13) . ? C45 C46 1.517(11) . ? C42' C43' 1.494(14) . ? C43' C44 1.494(15) . ? C44 C45' 1.498(15) . ? C45' C46' 1.505(14) . ? C51 C56' 1.433(12) . ? C51 C52 1.455(10) . ? C51 C56 1.514(10) . ? C51 C52' 1.581(12) . ? C52 C53 1.525(11) . ? C53 C54 1.497(13) . ? C54 C55 1.505(13) . ? C55 C56 1.544(12) . ? C52' C53' 1.522(13) . ? C53' C54' 1.496(14) . ? C54' C55' 1.503(15) . ? C55' C56' 1.530(13) . ? C61 C62 1.507(8) . ? C61 C66 1.519(8) . ? C62 C63 1.523(8) . ? C63 C64 1.502(8) . ? C64 C65 1.497(9) . ? C65 C66 1.521(8) . ? C1T C2T 1.375(16) . ? C1T C3T 1.453(16) . ? C1T C4T 1.54(3) . ? C2T C3T 1.358(17) 5 ? C3T C2T 1.358(17) 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 N3 P1 N10 113.7(3) . . y N3 P1 N1 112.9(3) . . y N10 P1 N1 102.3(3) . . y N3 P1 N40 106.0(3) . . y N10 P1 N40 110.4(3) . . y N1 P1 N40 111.7(3) . . y N3 P1 Li1 123.2(3) . . ? N10 P1 Li1 52.5(3) . . ? N1 P1 Li1 50.2(3) . . ? N40 P1 Li1 130.8(3) . . ? N3 P1 Li2 79.7(3) . 7 ? N10 P1 Li2 38.2(3) . 7 ? N1 P1 Li2 101.4(3) . 7 ? N40 P1 Li2 140.0(3) . 7 ? Li1 P1 Li2 58.9(3) . 7 ? N20 P2 N2 103.0(3) . . y N20 P2 N1 112.5(3) . . y N2 P2 N1 112.6(3) . . y N20 P2 N50 112.1(3) . . y N2 P2 N50 111.9(3) . . y N1 P2 N50 105.0(3) . . y N20 P2 Li2 52.8(3) . . ? N2 P2 Li2 50.7(3) . . ? N1 P2 Li2 122.5(3) . . ? N50 P2 Li2 132.6(3) . . ? N20 P2 Li3 40.6(3) . 7 ? N2 P2 Li3 103.0(3) . 7 ? N1 P2 Li3 75.7(3) . 7 ? N50 P2 Li3 141.0(3) . 7 ? Li2 P2 Li3 61.4(3) . 7 ? N30 P3 N2 113.6(3) . . y N30 P3 N3 103.0(3) . . y N2 P3 N3 111.3(3) . . y N30 P3 N60 111.3(3) . . y N2 P3 N60 104.3(3) . . y N3 P3 N60 113.6(3) . . y N30 P3 Li3 52.3(3) . . ? N2 P3 Li3 119.9(3) . . ? N3 P3 Li3 51.6(3) . . ? N60 P3 Li3 135.8(3) . . ? N30 P3 Li1 40.9(3) . 7 ? N2 P3 Li1 75.2(3) . 7 ? N3 P3 Li1 105.5(3) . 7 ? N60 P3 Li1 137.4(3) . 7 ? Li3 P3 Li1 61.7(3) . 7 ? P2 N1 P1 119.8(3) . . y P2 N1 Li1 138.1(4) . . ? P1 N1 Li1 90.0(4) . . ? P2 N2 P3 122.3(3) . . y P2 N2 Li2 89.7(4) . . ? P3 N2 Li2 137.8(5) . . ? P1 N3 P3 123.5(3) . . y P1 N3 Li3 131.4(4) . . ? P3 N3 Li3 88.8(4) . . ? C11 N10 P1 119.7(4) . . ? C11 N10 Li2 101.3(5) . 7 ? P1 N10 Li2 112.4(4) . 7 ? C11 N10 Li1 143.5(5) . . ? P1 N10 Li1 88.6(4) . . ? Li2 N10 Li1 86.5(5) 7 . ? C21 N20 P2 120.7(4) . . ? C21 N20 Li2 142.2(5) . . ? P2 N20 Li2 87.9(4) . . ? C21 N20 Li3 103.2(5) . 7 ? P2 N20 Li3 108.2(4) . 7 ? Li2 N20 Li3 88.6(5) . 7 ? C31 N30 P3 123.7(4) . . ? C31 N30 Li1 102.9(5) . 7 ? P3 N30 Li1 107.6(4) . 7 ? C31 N30 Li3 137.9(5) . . ? P3 N30 Li3 89.0(4) . . ? Li1 N30 Li3 89.1(5) 7 . ? C41 N40 P1 128.7(5) . . ? C51 N50 P2 130.1(5) . . ? C61 N60 P3 129.0(4) . . ? N1 Li1 N30 120.5(6) . 7 ? N1 Li1 N10 78.4(4) . . ? N30 Li1 N10 147.7(7) 7 . ? N1 Li1 C32' 150.4(11) . 7 ? N30 Li1 C32' 63.7(5) 7 7 ? N10 Li1 C32' 114.0(7) . 7 ? N1 Li1 P1 39.7(3) . . ? N30 Li1 P1 147.7(6) 7 . ? N10 Li1 P1 38.9(2) . . ? C32' Li1 P1 148.0(6) 7 . ? N1 Li1 C32 137.7(8) . 7 ? N30 Li1 C32 63.6(4) 7 7 ? N10 Li1 C32 121.9(6) . 7 ? C32' Li1 C32 13.3(9) 7 7 ? P1 Li1 C32 148.4(6) . 7 ? N1 Li1 C31 139.5(5) . 7 ? N30 Li1 C31 31.4(3) 7 7 ? N10 Li1 C31 141.9(5) . 7 ? C32' Li1 C31 33.0(4) 7 7 ? P1 Li1 C31 179.0(5) . 7 ? C32 Li1 C31 32.4(3) 7 7 ? N1 Li1 Li2 101.7(5) . 7 ? N30 Li1 Li2 101.5(5) 7 7 ? N10 Li1 Li2 46.6(4) . 7 ? C32' Li1 Li2 106.0(9) 7 7 ? P1 Li1 Li2 69.0(4) . 7 ? C32 Li1 Li2 119.3(7) 7 7 ? C31 Li1 Li2 111.2(5) 7 7 ? N1 Li1 Li3 74.8(4) . 7 ? N30 Li1 Li3 45.8(3) 7 7 ? N10 Li1 Li3 139.8(6) . 7 ? C32' Li1 Li3 104.0(6) 7 7 ? P1 Li1 Li3 107.2(4) . 7 ? C32 Li1 Li3 97.9(6) 7 7 ? C31 Li1 Li3 71.8(4) 7 7 ? Li2 Li1 Li3 111.3(5) 7 7 ? N1 Li1 P3 116.3(5) . 7 ? N30 Li1 P3 31.5(2) 7 7 ? N10 Li1 P3 118.3(5) . 7 ? C32' Li1 P3 82.7(7) 7 7 ? P1 Li1 P3 122.4(5) . 7 ? C32 Li1 P3 87.9(4) 7 7 ? C31 Li1 P3 57.0(3) 7 7 ? Li2 Li1 P3 71.8(4) 7 7 ? Li3 Li1 P3 52.9(3) 7 7 ? N2 Li2 N20 78.7(5) . . ? N2 Li2 N10 121.9(6) . 7 ? N20 Li2 N10 140.8(6) . 7 ? N2 Li2 P2 39.7(3) . . ? N20 Li2 P2 39.3(2) . . ? N10 Li2 P2 144.1(5) 7 . ? N2 Li2 C12 165.7(6) . 7 ? N20 Li2 C12 106.0(5) . 7 ? N10 Li2 C12 62.8(4) 7 7 ? P2 Li2 C12 144.7(5) . 7 ? N2 Li2 C11 146.6(6) . 7 ? N20 Li2 C11 134.4(5) . 7 ? N10 Li2 C11 31.9(2) 7 7 ? P2 Li2 C11 170.4(5) . 7 ? C12 Li2 C11 32.7(2) 7 7 ? N2 Li2 Li1 75.2(4) . 7 ? N20 Li2 Li1 138.7(5) . 7 ? N10 Li2 Li1 46.9(4) 7 7 ? P2 Li2 Li1 106.8(4) . 7 ? C12 Li2 Li1 107.2(5) 7 7 ? C11 Li2 Li1 74.5(4) 7 7 ? N2 Li2 Li3 98.6(5) . 7 ? N20 Li2 Li3 45.7(3) . 7 ? N10 Li2 Li3 95.9(5) 7 7 ? P2 Li2 Li3 66.6(4) . 7 ? C12 Li2 Li3 94.1(5) 7 7 ? C11 Li2 Li3 103.8(4) 7 7 ? Li1 Li2 Li3 107.9(5) 7 7 ? N2 Li2 P1 113.6(5) . 7 ? N20 Li2 P1 114.3(5) . 7 ? N10 Li2 P1 29.4(2) 7 7 ? P2 Li2 P1 118.0(4) . 7 ? C12 Li2 P1 77.2(3) 7 7 ? C11 Li2 P1 54.9(2) 7 7 ? Li1 Li2 P1 52.1(3) 7 7 ? Li3 Li2 P1 68.7(3) 7 7 ? N3 Li3 N20 125.6(6) . 7 ? N3 Li3 N30 77.7(4) . . ? N20 Li3 N30 143.9(7) 7 . ? N3 Li3 P3 39.6(2) . . ? N20 Li3 P3 148.7(6) 7 . ? N30 Li3 P3 38.7(2) . . ? N3 Li3 C26 161.7(6) . 7 ? N20 Li3 C26 61.1(3) 7 7 ? N30 Li3 C26 106.2(5) . 7 ? P3 Li3 C26 144.0(5) . 7 ? N3 Li3 C21 147.2(6) . 7 ? N20 Li3 C21 31.4(2) 7 7 ? N30 Li3 C21 135.0(6) . 7 ? P3 Li3 C21 172.7(5) . 7 ? C26 Li3 C21 31.6(2) 7 7 ? N3 Li3 Li2 80.0(5) . 7 ? N20 Li3 Li2 45.7(4) 7 7 ? N30 Li3 Li2 142.6(6) . 7 ? P3 Li3 Li2 111.1(5) . 7 ? C26 Li3 Li2 104.4(4) 7 7 ? C21 Li3 Li2 72.8(4) 7 7 ? N3 Li3 Li1 98.7(5) . 7 ? N20 Li3 Li1 100.2(5) 7 7 ? N30 Li3 Li1 45.2(3) . 7 ? P3 Li3 Li1 65.4(3) . 7 ? C26 Li3 Li1 96.3(5) 7 7 ? C21 Li3 Li1 107.6(5) 7 7 ? Li2 Li3 Li1 110.7(5) 7 7 ? N3 Li3 P2 118.3(5) . 7 ? N20 Li3 P2 31.2(2) 7 7 ? N30 Li3 P2 116.3(5) . 7 ? P3 Li3 P2 121.0(4) . 7 ? C26 Li3 P2 76.5(3) 7 7 ? C21 Li3 P2 55.9(2) 7 7 ? Li2 Li3 P2 52.0(3) 7 7 ? Li1 Li3 P2 71.2(4) 7 7 ? N10 C11 C16 111.2(5) . . ? N10 C11 C12 112.8(5) . . ? C16 C11 C12 107.6(6) . . ? N10 C11 Li2 46.8(3) . 7 ? C16 C11 Li2 107.6(6) . 7 ? C12 C11 Li2 70.4(4) . 7 ? C11 C12 C13 111.4(6) . . ? C11 C12 Li2 77.0(4) . 7 ? C13 C12 Li2 160.3(7) . 7 ? C14 C13 C12 111.2(7) . . ? C13 C14 C15 111.6(7) . . ? C14 C15 C16 111.4(8) . . ? C11 C16 C15 111.5(6) . . ? N20 C21 C26 114.1(5) . . ? N20 C21 C22 110.6(5) . . ? C26 C21 C22 108.7(6) . . ? N20 C21 Li3 45.4(4) . 7 ? C26 C21 Li3 73.4(5) . 7 ? C22 C21 Li3 107.6(6) . 7 ? C21 C22 C23 111.3(6) . . ? C24 C23 C22 113.4(7) . . ? C23 C24 C25 111.0(7) . . ? C24 C25 C26 109.4(7) . . ? C21 C26 C25 111.6(6) . . ? C21 C26 Li3 75.1(4) . 7 ? C25 C26 Li3 161.9(7) . 7 ? N30 C31 C32 114.8(8) . . ? N30 C31 C36' 113.3(10) . . ? C32 C31 C36' 86.6(13) . . ? N30 C31 C32' 109.7(11) . . ? C32 C31 C32' 23.1(14) . . ? C36' C31 C32' 108.7(14) . . ? N30 C31 C36 109.9(7) . . ? C32 C31 C36 107.0(9) . . ? C36' C31 C36 22.0(15) . . ? C32' C31 C36 127.7(12) . . ? N30 C31 Li1 45.7(4) . 7 ? C32 C31 Li1 69.6(7) . 7 ? C36' C31 Li1 117.3(16) . 7 ? C32' C31 Li1 65.6(11) . 7 ? C36 C31 Li1 131.8(8) . 7 ? C31 C32 C33 114.4(12) . . ? C31 C32 Li1 78.0(7) . 7 ? C33 C32 Li1 167.4(10) . 7 ? C34 C33 C32 111.1(13) . . ? C33 C34 C35 110.5(14) . . ? C34 C35 C36 110.0(11) . . ? C35 C36 C31 113.2(11) . . ? C31 C32' C33' 112.7(15) . . ? C31 C32' Li1 81.4(10) . 7 ? C33' C32' Li1 162.1(18) . 7 ? C34' C33' C32' 112.4(16) . . ? C35' C34' C33' 113.7(18) . . ? C34' C35' C36' 112.8(18) . . ? C31 C36' C35' 112.1(16) . . ? N40 C41 C42 124.0(7) . . ? N40 C41 C46' 133.3(9) . . ? C42 C41 C46' 100.4(10) . . ? N40 C41 C42' 105.3(9) . . ? C42 C41 C42' 52.9(12) . . ? C46' C41 C42' 113.4(11) . . ? N40 C41 C46 106.3(6) . . ? C42 C41 C46 109.5(8) . . ? C46' C41 C46 66.4(11) . . ? C42' C41 C46 69.6(13) . . ? C41 C42 C43 115.8(9) . . ? C42 C43 C44 110.8(10) . . ? C45 C44 C43 111.7(11) . . ? C44 C45 C46 109.1(10) . . ? C45 C46 C41 112.9(8) . . ? C43' C42' C41 118.6(13) . . ? C44 C43' C42' 113.6(16) . . ? C43' C44 C45' 112.0(17) . . ? C44 C45' C46' 110.6(17) . . ? C41 C46' C45' 116.8(13) . . ? C56' C51 N50 125.0(8) . . ? C56' C51 C52 108.4(9) . . ? N50 C51 C52 126.6(7) . . ? C56' C51 C56 39.6(9) . . ? N50 C51 C56 108.3(6) . . ? C52 C51 C56 113.2(8) . . ? C56' C51 C52' 111.0(11) . . ? N50 C51 C52' 101.1(7) . . ? C52 C51 C52' 55.1(9) . . ? C56 C51 C52' 81.9(10) . . ? C51 C52 C53 116.2(9) . . ? C54 C53 C52 111.5(11) . . ? C53 C54 C55 109.3(12) . . ? C54 C55 C56 110.1(11) . . ? C51 C56 C55 115.0(9) . . ? C53' C52' C51 114.6(11) . . ? C54' C53' C52' 110.5(14) . . ? C53' C54' C55' 111.2(16) . . ? C54' C55' C56' 111.6(16) . . ? C51 C56' C55' 112.1(12) . . ? N60 C61 C62 113.3(5) . . ? N60 C61 C66 109.6(5) . . ? C62 C61 C66 109.9(5) . . ? C61 C62 C63 112.8(6) . . ? C64 C63 C62 111.8(6) . . ? C65 C64 C63 111.4(6) . . ? C64 C65 C66 111.7(6) . . ? C61 C66 C65 112.5(6) . . ? C2T C1T C3T 123.9(13) . . ? C2T C1T C4T 131.0(17) . . ? C3T C1T C4T 105.1(17) . . ? C3T C2T C1T 124.7(13) 5 . ? C2T C3T C1T 111.4(14) 5 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N20 P2 N1 P1 152.7(3) . . . . ? N2 P2 N1 P1 36.7(4) . . . . y N50 P2 N1 P1 -85.2(4) . . . . ? Li2 P2 N1 P1 93.5(5) . . . . ? Li3 P2 N1 P1 135.1(4) 7 . . . ? N20 P2 N1 Li1 23.1(8) . . . . ? N2 P2 N1 Li1 -92.9(7) . . . . ? N50 P2 N1 Li1 145.2(7) . . . . ? Li2 P2 N1 Li1 -36.1(8) . . . . ? Li3 P2 N1 Li1 5.5(7) 7 . . . ? N3 P1 N1 P2 -34.0(4) . . . . y N10 P1 N1 P2 -156.6(3) . . . . ? N40 P1 N1 P2 85.3(4) . . . . ? Li1 P1 N1 P2 -149.0(6) . . . . ? Li2 P1 N1 P2 -117.6(4) 7 . . . ? N3 P1 N1 Li1 115.0(4) . . . . ? N10 P1 N1 Li1 -7.6(4) . . . . ? N40 P1 N1 Li1 -125.7(4) . . . . ? Li2 P1 N1 Li1 31.4(4) 7 . . . ? N20 P2 N2 P3 -157.9(3) . . . . ? N1 P2 N2 P3 -36.5(4) . . . . y N50 P2 N2 P3 81.5(4) . . . . ? Li2 P2 N2 P3 -150.7(5) . . . . ? Li3 P2 N2 P3 -116.2(4) 7 . . . ? N20 P2 N2 Li2 -7.2(4) . . . . ? N1 P2 N2 Li2 114.2(4) . . . . ? N50 P2 N2 Li2 -127.8(4) . . . . ? Li3 P2 N2 Li2 34.5(4) 7 . . . ? N30 P3 N2 P2 147.8(3) . . . . ? N3 P3 N2 P2 32.1(4) . . . . y N60 P3 N2 P2 -90.8(4) . . . . ? Li3 P3 N2 P2 89.1(5) . . . . ? Li1 P3 N2 P2 133.3(4) 7 . . . ? N30 P3 N2 Li2 14.5(7) . . . . ? N3 P3 N2 Li2 -101.2(6) . . . . ? N60 P3 N2 Li2 135.9(6) . . . . ? Li3 P3 N2 Li2 -44.2(7) . . . . ? Li1 P3 N2 Li2 0.0(6) 7 . . . ? N10 P1 N3 P3 146.8(3) . . . . ? N1 P1 N3 P3 30.8(5) . . . . y N40 P1 N3 P3 -91.8(4) . . . . ? Li1 P1 N3 P3 87.2(5) . . . . ? Li2 P1 N3 P3 129.0(4) 7 . . . ? N10 P1 N3 Li3 23.3(6) . . . . ? N1 P1 N3 Li3 -92.6(6) . . . . ? N40 P1 N3 Li3 144.8(6) . . . . ? Li1 P1 N3 Li3 -36.2(7) . . . . ? Li2 P1 N3 Li3 5.6(6) 7 . . . ? N30 P3 N3 P1 -151.4(4) . . . . ? N2 P3 N3 P1 -29.3(5) . . . . y N60 P3 N3 P1 88.1(4) . . . . ? Li3 P3 N3 P1 -141.2(6) . . . . ? Li1 P3 N3 P1 -109.2(4) 7 . . . ? N30 P3 N3 Li3 -10.2(4) . . . . ? N2 P3 N3 Li3 111.9(4) . . . . ? N60 P3 N3 Li3 -130.7(4) . . . . ? Li1 P3 N3 Li3 32.0(5) 7 . . . ? N3 P1 N10 C11 89.5(5) . . . . ? N1 P1 N10 C11 -148.4(5) . . . . ? N40 P1 N10 C11 -29.4(6) . . . . ? Li1 P1 N10 C11 -155.8(7) . . . . ? Li2 P1 N10 C11 118.6(7) 7 . . . ? N3 P1 N10 Li2 -29.1(5) . . . 7 ? N1 P1 N10 Li2 92.9(5) . . . 7 ? N40 P1 N10 Li2 -148.0(4) . . . 7 ? Li1 P1 N10 Li2 85.6(5) . . . 7 ? N3 P1 N10 Li1 -114.7(4) . . . . ? N1 P1 N10 Li1 7.3(4) . . . . ? N40 P1 N10 Li1 126.4(4) . . . . ? Li2 P1 N10 Li1 -85.6(5) 7 . . . ? N2 P2 N20 C21 -146.8(4) . . . . ? N1 P2 N20 C21 91.7(5) . . . . ? N50 P2 N20 C21 -26.3(5) . . . . ? Li2 P2 N20 C21 -153.8(6) . . . . ? Li3 P2 N20 C21 118.4(7) 7 . . . ? N2 P2 N20 Li2 7.0(4) . . . . ? N1 P2 N20 Li2 -114.5(4) . . . . ? N50 P2 N20 Li2 127.5(4) . . . . ? Li3 P2 N20 Li2 -87.9(5) 7 . . . ? N2 P2 N20 Li3 94.9(5) . . . 7 ? N1 P2 N20 Li3 -26.7(5) . . . 7 ? N50 P2 N20 Li3 -144.7(4) . . . 7 ? Li2 P2 N20 Li3 87.9(5) . . . 7 ? N2 P3 N30 C31 97.7(5) . . . . ? N3 P3 N30 C31 -141.7(5) . . . . ? N60 P3 N30 C31 -19.7(6) . . . . ? Li3 P3 N30 C31 -151.8(7) . . . . ? Li1 P3 N30 C31 119.5(7) 7 . . . ? N2 P3 N30 Li1 -21.7(5) . . . 7 ? N3 P3 N30 Li1 98.8(4) . . . 7 ? N60 P3 N30 Li1 -139.2(4) . . . 7 ? Li3 P3 N30 Li1 88.7(5) . . . 7 ? N2 P3 N30 Li3 -110.5(4) . . . . ? N3 P3 N30 Li3 10.1(4) . . . . ? N60 P3 N30 Li3 132.1(4) . . . . ? Li1 P3 N30 Li3 -88.7(5) 7 . . . ? N3 P1 N40 C41 167.4(6) . . . . ? N10 P1 N40 C41 -69.1(7) . . . . ? N1 P1 N40 C41 44.0(7) . . . . ? Li1 P1 N40 C41 -11.5(8) . . . . ? Li2 P1 N40 C41 -99.7(7) 7 . . . ? N20 P2 N50 C51 -65.4(7) . . . . ? N2 P2 N50 C51 49.8(7) . . . . ? N1 P2 N50 C51 172.2(6) . . . . ? Li2 P2 N50 C51 -6.3(8) . . . . ? Li3 P2 N50 C51 -102.1(7) 7 . . . ? N30 P3 N60 C61 -58.3(6) . . . . ? N2 P3 N60 C61 178.8(6) . . . . ? N3 P3 N60 C61 57.4(6) . . . . ? Li3 P3 N60 C61 -1.1(8) . . . . ? Li1 P3 N60 C61 -97.6(7) 7 . . . ? P2 N1 Li1 N30 -7.6(12) . . . 7 ? P1 N1 Li1 N30 -145.6(7) . . . 7 ? P2 N1 Li1 N10 144.0(5) . . . . ? P1 N1 Li1 N10 6.0(4) . . . . ? P2 N1 Li1 C32' -97.4(14) . . . 7 ? P1 N1 Li1 C32' 124.5(13) . . . 7 ? P2 N1 Li1 P1 138.0(7) . . . . ? P2 N1 Li1 C32 -90.8(10) . . . 7 ? P1 N1 Li1 C32 131.1(8) . . . 7 ? P2 N1 Li1 C31 -41.0(13) . . . 7 ? P1 N1 Li1 C31 -179.0(8) . . . 7 ? P2 N1 Li1 Li2 103.3(6) . . . 7 ? P1 N1 Li1 Li2 -34.7(4) . . . 7 ? P2 N1 Li1 Li3 -5.8(7) . . . 7 ? P1 N1 Li1 Li3 -143.8(4) . . . 7 ? P2 N1 Li1 P3 28.0(10) . . . 7 ? P1 N1 Li1 P3 -110.0(5) . . . 7 ? C11 N10 Li1 N1 137.1(8) . . . . ? P1 N10 Li1 N1 -6.1(4) . . . . ? Li2 N10 Li1 N1 -118.6(5) 7 . . . ? C11 N10 Li1 N30 -92.8(14) . . . 7 ? P1 N10 Li1 N30 124.0(11) . . . 7 ? Li2 N10 Li1 N30 11.5(12) 7 . . 7 ? C11 N10 Li1 C32' -14.5(14) . . . 7 ? P1 N10 Li1 C32' -157.7(10) . . . 7 ? Li2 N10 Li1 C32' 89.8(10) 7 . . 7 ? C11 N10 Li1 P1 143.2(9) . . . . ? Li2 N10 Li1 P1 -112.5(4) 7 . . . ? C11 N10 Li1 C32 -2.5(13) . . . 7 ? P1 N10 Li1 C32 -145.7(8) . . . 7 ? Li2 N10 Li1 C32 101.8(8) 7 . . 7 ? C11 N10 Li1 C31 -37.7(15) . . . 7 ? P1 N10 Li1 C31 179.2(9) . . . 7 ? Li2 N10 Li1 C31 66.6(10) 7 . . 7 ? C11 N10 Li1 Li2 -104.3(9) . . . 7 ? P1 N10 Li1 Li2 112.5(4) . . . 7 ? C11 N10 Li1 Li3 -174.1(7) . . . 7 ? P1 N10 Li1 Li3 42.7(9) . . . 7 ? Li2 N10 Li1 Li3 -69.8(9) 7 . . 7 ? C11 N10 Li1 P3 -109.2(8) . . . 7 ? P1 N10 Li1 P3 107.6(4) . . . 7 ? Li2 N10 Li1 P3 -4.9(5) 7 . . 7 ? N3 P1 Li1 N1 -93.5(4) . . . . ? N10 P1 Li1 N1 170.6(6) . . . . ? N40 P1 Li1 N1 85.3(5) . . . . ? Li2 P1 Li1 N1 -143.4(5) 7 . . . ? N3 P1 Li1 N30 -28.0(12) . . . 7 ? N10 P1 Li1 N30 -123.9(12) . . . 7 ? N1 P1 Li1 N30 65.4(10) . . . 7 ? N40 P1 Li1 N30 150.7(9) . . . 7 ? Li2 P1 Li1 N30 -77.9(11) 7 . . 7 ? N3 P1 Li1 N10 95.9(4) . . . . ? N1 P1 Li1 N10 -170.6(5) . . . . ? N40 P1 Li1 N10 -85.4(5) . . . . ? Li2 P1 Li1 N10 46.0(4) 7 . . . ? N3 P1 Li1 C32' 136.7(18) . . . 7 ? N10 P1 Li1 C32' 40.8(18) . . . 7 ? N1 P1 Li1 C32' -130(2) . . . 7 ? N40 P1 Li1 C32' -45(2) . . . 7 ? Li2 P1 Li1 C32' 86.8(19) 7 . . 7 ? N3 P1 Li1 C32 161.9(13) . . . 7 ? N10 P1 Li1 C32 66.0(14) . . . 7 ? N1 P1 Li1 C32 -104.6(15) . . . 7 ? N40 P1 Li1 C32 -19.3(16) . . . 7 ? Li2 P1 Li1 C32 112.1(15) 7 . . 7 ? N3 P1 Li1 C31 -52(34) . . . 7 ? N10 P1 Li1 C31 -148(34) . . . 7 ? N1 P1 Li1 C31 42(34) . . . 7 ? N40 P1 Li1 C31 127(34) . . . 7 ? Li2 P1 Li1 C31 -102(34) 7 . . 7 ? N3 P1 Li1 Li2 49.9(4) . . . 7 ? N10 P1 Li1 Li2 -46.0(4) . . . 7 ? N1 P1 Li1 Li2 143.4(5) . . . 7 ? N40 P1 Li1 Li2 -131.4(4) . . . 7 ? N3 P1 Li1 Li3 -56.8(5) . . . 7 ? N10 P1 Li1 Li3 -152.7(6) . . . 7 ? N1 P1 Li1 Li3 36.6(4) . . . 7 ? N40 P1 Li1 Li3 121.9(5) . . . 7 ? Li2 P1 Li1 Li3 -106.7(5) 7 . . 7 ? N3 P1 Li1 P3 -0.3(6) . . . 7 ? N10 P1 Li1 P3 -96.2(5) . . . 7 ? N1 P1 Li1 P3 93.2(5) . . . 7 ? N40 P1 Li1 P3 178.5(3) . . . 7 ? Li2 P1 Li1 P3 -50.2(4) 7 . . 7 ? P2 N2 Li2 N20 5.7(3) . . . . ? P3 N2 Li2 N20 147.7(5) . . . . ? P2 N2 Li2 N10 -138.1(6) . . . 7 ? P3 N2 Li2 N10 3.9(10) . . . 7 ? P3 N2 Li2 P2 142.0(6) . . . . ? P2 N2 Li2 C12 117(2) . . . 7 ? P3 N2 Li2 C12 -101(2) . . . 7 ? P2 N2 Li2 C11 -167.5(9) . . . 7 ? P3 N2 Li2 C11 -25.5(13) . . . 7 ? P2 N2 Li2 Li1 -142.0(3) . . . 7 ? P3 N2 Li2 Li1 0.0(6) . . . 7 ? P2 N2 Li2 Li3 -35.6(4) . . . 7 ? P3 N2 Li2 Li3 106.4(6) . . . 7 ? P2 N2 Li2 P1 -106.0(4) . . . 7 ? P3 N2 Li2 P1 36.0(8) . . . 7 ? C21 N20 Li2 N2 136.0(7) . . . . ? P2 N20 Li2 N2 -5.7(3) . . . . ? Li3 N20 Li2 N2 -114.1(5) 7 . . . ? C21 N20 Li2 N10 -96.5(11) . . . 7 ? P2 N20 Li2 N10 121.7(9) . . . 7 ? Li3 N20 Li2 N10 13.4(10) 7 . . 7 ? C21 N20 Li2 P2 141.7(9) . . . . ? Li3 N20 Li2 P2 -108.3(4) 7 . . . ? C21 N20 Li2 C12 -30.2(10) . . . 7 ? P2 N20 Li2 C12 -171.9(4) . . . 7 ? Li3 N20 Li2 C12 79.8(5) 7 . . 7 ? C21 N20 Li2 C11 -49.2(12) . . . 7 ? P2 N20 Li2 C11 169.1(6) . . . 7 ? Li3 N20 Li2 C11 60.7(7) 7 . . 7 ? C21 N20 Li2 Li1 -172.5(7) . . . 7 ? P2 N20 Li2 Li1 45.7(8) . . . 7 ? Li3 N20 Li2 Li1 -62.6(9) 7 . . 7 ? C21 N20 Li2 Li3 -110.0(9) . . . 7 ? P2 N20 Li2 Li3 108.3(4) . . . 7 ? C21 N20 Li2 P1 -113.0(7) . . . 7 ? P2 N20 Li2 P1 105.3(4) . . . 7 ? Li3 N20 Li2 P1 -3.1(5) 7 . . 7 ? N20 P2 Li2 N2 171.1(5) . . . . ? N1 P2 Li2 N2 -93.9(4) . . . . ? N50 P2 Li2 N2 84.4(5) . . . . ? Li3 P2 Li2 N2 -141.1(4) 7 . . . ? N2 P2 Li2 N20 -171.1(5) . . . . ? N1 P2 Li2 N20 94.9(4) . . . . ? N50 P2 Li2 N20 -86.8(5) . . . . ? Li3 P2 Li2 N20 47.8(3) 7 . . . ? N20 P2 Li2 N10 -113.6(10) . . . 7 ? N2 P2 Li2 N10 75.3(9) . . . 7 ? N1 P2 Li2 N10 -18.7(11) . . . 7 ? N50 P2 Li2 N10 159.6(8) . . . 7 ? Li3 P2 Li2 N10 -65.8(9) 7 . . 7 ? N20 P2 Li2 C12 13.6(7) . . . 7 ? N2 P2 Li2 C12 -157.5(10) . . . 7 ? N1 P2 Li2 C12 108.5(8) . . . 7 ? N50 P2 Li2 C12 -73.2(10) . . . 7 ? Li3 P2 Li2 C12 61.4(8) 7 . . 7 ? N20 P2 Li2 C11 -54(3) . . . 7 ? N2 P2 Li2 C11 135(3) . . . 7 ? N1 P2 Li2 C11 41(3) . . . 7 ? N50 P2 Li2 C11 -141(3) . . . 7 ? Li3 P2 Li2 C11 -6(3) 7 . . 7 ? N20 P2 Li2 Li1 -150.4(6) . . . 7 ? N2 P2 Li2 Li1 38.4(4) . . . 7 ? N1 P2 Li2 Li1 -55.5(5) . . . 7 ? N50 P2 Li2 Li1 122.8(5) . . . 7 ? Li3 P2 Li2 Li1 -102.7(5) 7 . . 7 ? N20 P2 Li2 Li3 -47.8(3) . . . 7 ? N2 P2 Li2 Li3 141.1(4) . . . 7 ? N1 P2 Li2 Li3 47.2(4) . . . 7 ? N50 P2 Li2 Li3 -134.5(4) . . . 7 ? N20 P2 Li2 P1 -94.9(5) . . . 7 ? N2 P2 Li2 P1 94.0(5) . . . 7 ? N1 P2 Li2 P1 0.0(6) . . . 7 ? N50 P2 Li2 P1 178.3(3) . . . 7 ? Li3 P2 Li2 P1 -47.1(4) 7 . . 7 ? P1 N3 Li3 N20 -5.6(10) . . . 7 ? P3 N3 Li3 N20 -141.5(7) . . . 7 ? P1 N3 Li3 N30 143.9(4) . . . . ? P3 N3 Li3 N30 8.0(3) . . . . ? P1 N3 Li3 P3 135.9(6) . . . . ? P1 N3 Li3 C26 -111.5(18) . . . 7 ? P3 N3 Li3 C26 112.6(18) . . . 7 ? P1 N3 Li3 C21 -39.8(13) . . . 7 ? P3 N3 Li3 C21 -175.7(10) . . . 7 ? P1 N3 Li3 Li2 -6.0(6) . . . 7 ? P3 N3 Li3 Li2 -141.9(4) . . . 7 ? P1 N3 Li3 Li1 103.6(5) . . . 7 ? P3 N3 Li3 Li1 -32.3(4) . . . 7 ? P1 N3 Li3 P2 30.4(8) . . . 7 ? P3 N3 Li3 P2 -105.5(5) . . . 7 ? C31 N30 Li3 N3 135.9(7) . . . . ? P3 N30 Li3 N3 -8.1(3) . . . . ? Li1 N30 Li3 N3 -115.8(5) 7 . . . ? C31 N30 Li3 N20 -88.6(13) . . . 7 ? P3 N30 Li3 N20 127.4(10) . . . 7 ? Li1 N30 Li3 N20 19.7(11) 7 . . 7 ? C31 N30 Li3 P3 144.1(8) . . . . ? Li1 N30 Li3 P3 -107.6(4) 7 . . . ? C31 N30 Li3 C26 -25.7(10) . . . 7 ? P3 N30 Li3 C26 -169.7(4) . . . 7 ? Li1 N30 Li3 C26 82.7(6) 7 . . 7 ? C31 N30 Li3 C21 -41.3(12) . . . 7 ? P3 N30 Li3 C21 174.7(7) . . . 7 ? Li1 N30 Li3 C21 67.1(8) 7 . . 7 ? C31 N30 Li3 Li2 -169.5(7) . . . 7 ? P3 N30 Li3 Li2 46.4(10) . . . 7 ? Li1 N30 Li3 Li2 -61.2(10) 7 . . 7 ? C31 N30 Li3 Li1 -108.3(8) . . . 7 ? P3 N30 Li3 Li1 107.6(4) . . . 7 ? C31 N30 Li3 P2 -108.3(7) . . . 7 ? P3 N30 Li3 P2 107.6(4) . . . 7 ? Li1 N30 Li3 P2 0.0(6) 7 . . 7 ? N30 P3 Li3 N3 167.5(5) . . . . ? N2 P3 Li3 N3 -94.5(4) . . . . ? N60 P3 Li3 N3 85.3(5) . . . . ? Li1 P3 Li3 N3 -144.5(5) 7 . . . ? N30 P3 Li3 N20 -115.7(12) . . . 7 ? N2 P3 Li3 N20 -17.7(13) . . . 7 ? N3 P3 Li3 N20 76.8(11) . . . 7 ? N60 P3 Li3 N20 162.1(9) . . . 7 ? Li1 P3 Li3 N20 -67.7(11) 7 . . 7 ? N2 P3 Li3 N30 98.0(4) . . . . ? N3 P3 Li3 N30 -167.5(5) . . . . ? N60 P3 Li3 N30 -82.1(5) . . . . ? Li1 P3 Li3 N30 48.0(4) 7 . . . ? N30 P3 Li3 C26 16.9(7) . . . 7 ? N2 P3 Li3 C26 114.9(8) . . . 7 ? N3 P3 Li3 C26 -150.5(10) . . . 7 ? N60 P3 Li3 C26 -65.2(10) . . . 7 ? Li1 P3 Li3 C26 64.9(8) 7 . . 7 ? N30 P3 Li3 C21 -31(4) . . . 7 ? N2 P3 Li3 C21 67(4) . . . 7 ? N3 P3 Li3 C21 161(4) . . . 7 ? N60 P3 Li3 C21 -113(4) . . . 7 ? Li1 P3 Li3 C21 17(4) 7 . . 7 ? N30 P3 Li3 Li2 -151.9(6) . . . 7 ? N2 P3 Li3 Li2 -53.9(6) . . . 7 ? N3 P3 Li3 Li2 40.7(4) . . . 7 ? N60 P3 Li3 Li2 126.0(5) . . . 7 ? Li1 P3 Li3 Li2 -103.9(6) 7 . . 7 ? N30 P3 Li3 Li1 -48.0(4) . . . 7 ? N2 P3 Li3 Li1 50.0(4) . . . 7 ? N3 P3 Li3 Li1 144.5(5) . . . 7 ? N60 P3 Li3 Li1 -130.2(5) . . . 7 ? N30 P3 Li3 P2 -94.4(5) . . . 7 ? N2 P3 Li3 P2 3.6(6) . . . 7 ? N3 P3 Li3 P2 98.1(5) . . . 7 ? N60 P3 Li3 P2 -176.6(3) . . . 7 ? Li1 P3 Li3 P2 -46.4(4) 7 . . 7 ? P1 N10 C11 C16 141.2(6) . . . . ? Li2 N10 C11 C16 -94.6(7) 7 . . . ? Li1 N10 C11 C16 4.9(11) . . . . ? P1 N10 C11 C12 -97.8(6) . . . . ? Li2 N10 C11 C12 26.3(7) 7 . . . ? Li1 N10 C11 C12 125.8(9) . . . . ? P1 N10 C11 Li2 -124.2(6) . . . 7 ? Li1 N10 C11 Li2 99.5(9) . . . 7 ? N10 C11 C12 C13 178.6(6) . . . . ? C16 C11 C12 C13 -58.4(9) . . . . ? Li2 C11 C12 C13 -161.3(8) 7 . . . ? N10 C11 C12 Li2 -20.1(5) . . . 7 ? C16 C11 C12 Li2 102.9(6) . . . 7 ? C11 C12 C13 C14 57.6(11) . . . . ? Li2 C12 C13 C14 -55(2) 7 . . . ? C12 C13 C14 C15 -54.2(11) . . . . ? C13 C14 C15 C16 53.9(12) . . . . ? N10 C11 C16 C15 -177.9(7) . . . . ? C12 C11 C16 C15 58.1(10) . . . . ? Li2 C11 C16 C15 132.5(8) 7 . . . ? C14 C15 C16 C11 -56.9(12) . . . . ? P2 N20 C21 C26 -92.7(7) . . . . ? Li2 N20 C21 C26 133.4(8) . . . . ? Li3 N20 C21 C26 28.2(7) 7 . . . ? P2 N20 C21 C22 144.4(6) . . . . ? Li2 N20 C21 C22 10.5(11) . . . . ? Li3 N20 C21 C22 -94.7(7) 7 . . . ? P2 N20 C21 Li3 -120.9(6) . . . 7 ? Li2 N20 C21 Li3 105.2(9) . . . 7 ? N20 C21 C22 C23 -179.0(7) . . . . ? C26 C21 C22 C23 55.0(10) . . . . ? Li3 C21 C22 C23 132.9(8) 7 . . . ? C21 C22 C23 C24 -54.1(12) . . . . ? C22 C23 C24 C25 54.3(12) . . . . ? C23 C24 C25 C26 -55.6(11) . . . . ? N20 C21 C26 C25 177.2(6) . . . . ? C22 C21 C26 C25 -58.9(9) . . . . ? Li3 C21 C26 C25 -162.3(8) 7 . . . ? N20 C21 C26 Li3 -20.5(5) . . . 7 ? C22 C21 C26 Li3 103.4(6) . . . 7 ? C24 C25 C26 C21 59.7(10) . . . . ? C24 C25 C26 Li3 -49(2) . . . 7 ? P3 N30 C31 C32 -130.4(12) . . . . ? Li1 N30 C31 C32 -8.7(13) 7 . . . ? Li3 N30 C31 C32 94.4(14) . . . . ? P3 N30 C31 C36' 132.3(18) . . . . ? Li1 N30 C31 C36' -106.1(19) 7 . . . ? Li3 N30 C31 C36' -3(2) . . . . ? P3 N30 C31 C32' -106.0(16) . . . . ? Li1 N30 C31 C32' 15.6(17) 7 . . . ? Li3 N30 C31 C32' 118.8(17) . . . . ? P3 N30 C31 C36 108.8(9) . . . . ? Li1 N30 C31 C36 -129.5(10) 7 . . . ? Li3 N30 C31 C36 -26.3(12) . . . . ? P3 N30 C31 Li1 -121.7(6) . . . 7 ? Li3 N30 C31 Li1 103.2(8) . . . 7 ? N30 C31 C32 C33 -175.7(12) . . . . ? C36' C31 C32 C33 -61.6(18) . . . . ? C32' C31 C32 C33 102(4) . . . . ? C36 C31 C32 C33 -53.4(17) . . . . ? Li1 C31 C32 C33 177.6(16) 7 . . . ? N30 C31 C32 Li1 6.7(10) . . . 7 ? C36' C31 C32 Li1 120.8(15) . . . 7 ? C32' C31 C32 Li1 -75(4) . . . 7 ? C36 C31 C32 Li1 129.0(9) . . . 7 ? C31 C32 C33 C34 56(2) . . . . ? Li1 C32 C33 C34 -135(6) 7 . . . ? C32 C33 C34 C35 -55(2) . . . . ? C33 C34 C35 C36 57(2) . . . . ? C34 C35 C36 C31 -58.6(18) . . . . ? N30 C31 C36 C35 -179.4(9) . . . . ? C32 C31 C36 C35 55.2(14) . . . . ? C36' C31 C36 C35 78(4) . . . . ? C32' C31 C36 C35 43(2) . . . . ? Li1 C31 C36 C35 132.8(10) 7 . . . ? N30 C31 C32' C33' 179.2(16) . . . . ? C32 C31 C32' C33' -73(4) . . . . ? C36' C31 C32' C33' -56(2) . . . . ? C36 C31 C32' C33' -44(3) . . . . ? Li1 C31 C32' C33' -169(2) 7 . . . ? N30 C31 C32' Li1 -12.2(13) . . . 7 ? C32 C31 C32' Li1 95(4) . . . 7 ? C36' C31 C32' Li1 112.2(17) . . . 7 ? C36 C31 C32' Li1 125.0(12) . . . 7 ? C31 C32' C33' C34' 53(3) . . . . ? Li1 C32' C33' C34' -88(6) 7 . . . ? C32' C33' C34' C35' -48(4) . . . . ? C33' C34' C35' C36' 49(4) . . . . ? N30 C31 C36' C35' 179.0(18) . . . . ? C32 C31 C36' C35' 63(2) . . . . ? C32' C31 C36' C35' 57(3) . . . . ? C36 C31 C36' C35' -95(5) . . . . ? Li1 C31 C36' C35' 128(2) 7 . . . ? C34' C35' C36' C31 -54(3) . . . . ? P1 N40 C41 C42 94.8(10) . . . . ? P1 N40 C41 C46' -64.5(18) . . . . ? P1 N40 C41 C42' 150.1(13) . . . . ? P1 N40 C41 C46 -137.2(7) . . . . ? N40 C41 C42 C43 177.8(9) . . . . ? C46' C41 C42 C43 -17.3(17) . . . . ? C42' C41 C42 C43 94.2(15) . . . . ? C46 C41 C42 C43 51.2(14) . . . . ? C41 C42 C43 C44 -54.4(17) . . . . ? C42 C43 C44 C45 55.7(18) . . . . ? C43 C44 C45 C46 -57.1(17) . . . . ? C44 C45 C46 C41 55.1(14) . . . . ? N40 C41 C46 C45 172.0(9) . . . . ? C42 C41 C46 C45 -51.9(12) . . . . ? C46' C41 C46 C45 41.2(11) . . . . ? C42' C41 C46 C45 -87.4(12) . . . . ? N40 C41 C42' C43' -175(2) . . . . ? C42 C41 C42' C43' -53(2) . . . . ? C46' C41 C42' C43' 32(3) . . . . ? C46 C41 C42' C43' 83(2) . . . . ? C41 C42' C43' C44 -37(4) . . . . ? C42' C43' C44 C45' 49(4) . . . . ? C43' C44 C45' C46' -56(3) . . . . ? N40 C41 C46' C45' 176.7(15) . . . . ? C42 C41 C46' C45' 14(2) . . . . ? C42' C41 C46' C45' -40(3) . . . . ? C46 C41 C46' C45' -93(2) . . . . ? C44 C45' C46' C41 53(3) . . . . ? P2 N50 C51 C56' -92.7(14) . . . . ? P2 N50 C51 C52 87.1(11) . . . . ? P2 N50 C51 C56 -133.3(8) . . . . ? P2 N50 C51 C52' 141.6(9) . . . . ? C56' C51 C52 C53 -0.8(18) . . . . ? N50 C51 C52 C53 179.4(9) . . . . ? C56 C51 C52 C53 41.4(16) . . . . ? C52' C51 C52 C53 102.4(14) . . . . ? C51 C52 C53 C54 -51.0(17) . . . . ? C52 C53 C54 C55 58.8(19) . . . . ? C53 C54 C55 C56 -58.8(19) . . . . ? C56' C51 C56 C55 49.4(13) . . . . ? N50 C51 C56 C55 172.6(10) . . . . ? C52 C51 C56 C55 -41.8(15) . . . . ? C52' C51 C56 C55 -88.3(12) . . . . ? C54 C55 C56 C51 51.2(17) . . . . ? C56' C51 C52' C53' 49(2) . . . . ? N50 C51 C52' C53' -176.8(14) . . . . ? C52 C51 C52' C53' -49.6(14) . . . . ? C56 C51 C52' C53' 76.1(16) . . . . ? C51 C52' C53' C54' -49(2) . . . . ? C52' C53' C54' C55' 54(3) . . . . ? C53' C54' C55' C56' -59(3) . . . . ? N50 C51 C56' C55' -173.3(12) . . . . ? C52 C51 C56' C55' 7(2) . . . . ? C56 C51 C56' C55' -97.6(19) . . . . ? C52' C51 C56' C55' -52(2) . . . . ? C54' C55' C56' C51 59(3) . . . . ? P3 N60 C61 C62 -94.3(7) . . . . ? P3 N60 C61 C66 142.5(6) . . . . ? N60 C61 C62 C63 -176.3(6) . . . . ? C66 C61 C62 C63 -53.3(8) . . . . ? C61 C62 C63 C64 54.3(9) . . . . ? C62 C63 C64 C65 -53.9(10) . . . . ? C63 C64 C65 C66 54.3(9) . . . . ? N60 C61 C66 C65 178.8(6) . . . . ? C62 C61 C66 C65 53.6(9) . . . . ? C64 C65 C66 C61 -54.9(9) . . . . ? C3T C1T C2T C3T 0(3) . . . 5 ? C4T C1T C2T C3T 180(2) . . . 5 ? C2T C1T C3T C2T 0(2) . . . 5 ? C4T C1T C3T C2T -179.8(17) . . . 5 ? _diffrn_measured_fraction_theta_max 0.476 _diffrn_reflns_theta_full 22.37 _diffrn_measured_fraction_theta_full 0.476 _refine_diff_density_max 0.350 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.069 data_2b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H113 Li3 N9 O10 P3' _chemical_formula_weight 1426.48 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' 'Li' 'Li' -0.0003 0.0001 '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 rhombohedral _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 21.620(3) _cell_length_b 21.620(3) _cell_length_c 61.490(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 24891(7) _cell_formula_units_Z 12 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour golden-brown _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.142 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9192 _exptl_absorpt_coefficient_mu 0.129 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 Stoe-IPDS _diffrn_measurement_method 'image plate' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13763 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0583 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -66 _diffrn_reflns_limit_l_max 66 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 22.49 _reflns_number_total 3619 _reflns_number_gt 2188 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1144P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3619 _refine_ls_number_parameters 305 _refine_ls_number_restraints 584 _refine_ls_R_factor_all 0.0856 _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_ref 0.1661 _refine_ls_wR_factor_gt 0.1555 _refine_ls_goodness_of_fit_ref 0.873 _refine_ls_restrained_S_all 1.039 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.25362(5) 0.59816(5) 0.018257(17) 0.0385(4) Uani 1 d . . . N1 N 0.26680(17) 0.67782(17) 0.02265(5) 0.0396(8) Uani 1 d . . . N2 N 0.18365(17) 0.55033(17) 0.03227(5) 0.0426(9) Uani 1 d . . . N3 N 0.2405(2) 0.57808(19) -0.00881(6) 0.0459(9) Uani 1 d . . . H3 H 0.272(2) 0.570(2) -0.0140(7) 0.053(14) Uiso 1 d . . . Li1 Li 0.1772(4) 0.6372(4) 0.04187(12) 0.0548(19) Uani 1 d . . . C11 C 0.1472(2) 0.4764(2) 0.03384(7) 0.0447(11) Uani 1 d . . . C12 C 0.1637(3) 0.4308(2) 0.02235(8) 0.0561(12) Uani 1 d . . . H12 H 0.2032 0.4506 0.0126 0.067 Uiso 1 calc R . . C13 C 0.1241(3) 0.3575(3) 0.02479(10) 0.0726(16) Uani 1 d . . . H13 H 0.1364 0.3277 0.0167 0.087 Uiso 1 calc R . . C14 C 0.0663(3) 0.3272(3) 0.03901(12) 0.0839(19) Uani 1 d . . . H14 H 0.0386 0.2768 0.0406 0.101 Uiso 1 calc R . . C15 C 0.0498(3) 0.3708(3) 0.05069(10) 0.0773(17) Uani 1 d . . . H15 H 0.0111 0.3506 0.0607 0.093 Uiso 1 calc R . . C16 C 0.0887(2) 0.4437(3) 0.04816(8) 0.0583(13) Uani 1 d . . . H16 H 0.0757 0.4728 0.0563 0.070 Uiso 1 calc R . . C21 C 0.2003(2) 0.5892(2) -0.02424(7) 0.0434(11) Uani 1 d . . . C22 C 0.2121(3) 0.5846(3) -0.04615(7) 0.0652(14) Uani 1 d . . . H22 H 0.2481 0.5741 -0.0505 0.078 Uiso 1 calc R . . C23 C 0.1725(3) 0.5947(4) -0.06178(8) 0.0860(18) Uani 1 d . . . H23 H 0.1809 0.5905 -0.0767 0.103 Uiso 1 calc R . . C24 C 0.1211(3) 0.6109(3) -0.05602(9) 0.0801(17) Uani 1 d . . . H24 H 0.0939 0.6180 -0.0669 0.096 Uiso 1 calc R . . C25 C 0.1092(3) 0.6168(3) -0.03447(8) 0.0631(14) Uani 1 d . . . H25 H 0.0737 0.6282 -0.0304 0.076 Uiso 1 calc R . . C26 C 0.1481(2) 0.6063(2) -0.01862(7) 0.0500(11) Uani 1 d . . . H26 H 0.1393 0.6107 -0.0037 0.060 Uiso 1 calc R . . O1 O 0.19194(19) 0.6805(2) 0.07068(6) 0.0776(11) Uani 1 d DU . . C31 C 0.2589(4) 0.7072(4) 0.08100(10) 0.102(2) Uani 1 d DU . . H31A H 0.2957 0.7139 0.0702 0.122 Uiso 0.45(2) calc PR A 1 H31B H 0.2563 0.6730 0.0922 0.122 Uiso 0.45(2) calc PR A 1 H31A H 0.2981 0.7293 0.0702 0.122 Uiso 0.55(2) calc PR A 2 H31B H 0.2618 0.6683 0.0886 0.122 Uiso 0.55(2) calc PR A 2 C32 C 0.2773(9) 0.7754(9) 0.0911(4) 0.109(7) Uiso 0.45(2) d PDU A 1 H32A H 0.2908 0.7764 0.1065 0.131 Uiso 0.45(2) calc PR A 1 H32B H 0.3173 0.8156 0.0833 0.131 Uiso 0.45(2) calc PR A 1 C33 C 0.2126(8) 0.7789(8) 0.0892(4) 0.102(6) Uiso 0.45(2) d PDU A 1 H33A H 0.2186 0.8145 0.0780 0.123 Uiso 0.45(2) calc PR A 1 H33B H 0.2015 0.7936 0.1033 0.123 Uiso 0.45(2) calc PR A 1 C34 C 0.1521(7) 0.7050(9) 0.0828(4) 0.102(6) Uiso 0.45(2) d PDU A 1 H34A H 0.1287 0.6746 0.0956 0.122 Uiso 0.45(2) calc PR A 1 H34B H 0.1158 0.7078 0.0737 0.122 Uiso 0.45(2) calc PR A 1 C32' C 0.2637(9) 0.7617(10) 0.0970(3) 0.130(8) Uiso 0.55(2) d PDU A 2 H32C H 0.2816 0.7556 0.1112 0.156 Uiso 0.55(2) calc PR A 2 H32D H 0.2965 0.8106 0.0916 0.156 Uiso 0.55(2) calc PR A 2 C33' C 0.1906(7) 0.7496(9) 0.0991(2) 0.097(5) Uiso 0.55(2) d PDU A 2 H33C H 0.1902 0.7928 0.1043 0.116 Uiso 0.55(2) calc PR A 2 H33D H 0.1608 0.7089 0.1089 0.116 Uiso 0.55(2) calc PR A 2 C34' C 0.1676(6) 0.7327(7) 0.07535(17) 0.070(4) Uiso 0.55(2) d PDU A 2 H34C H 0.1153 0.7109 0.0737 0.084 Uiso 0.55(2) calc PR A 2 H34D H 0.1921 0.7757 0.0660 0.084 Uiso 0.55(2) calc PR A 2 O2 O 0.08851(16) 0.63412(17) 0.03267(6) 0.0677(10) Uani 1 d DU . . C41 C 0.0216(3) 0.5689(3) 0.03072(10) 0.0780(16) Uani 1 d DU . . H41A H -0.0030 0.5546 0.0450 0.094 Uiso 0.709(16) calc PR B 1 H41B H 0.0289 0.5300 0.0253 0.094 Uiso 0.709(16) calc PR B 1 H41A H 0.0108 0.5408 0.0443 0.094 Uiso 0.291(16) calc PR B 2 H41B H 0.0234 0.5399 0.0186 0.094 Uiso 0.291(16) calc PR B 2 C42 C -0.0213(4) 0.5853(4) 0.01466(18) 0.075(3) Uiso 0.709(16) d PDU B 1 H42A H -0.0179 0.5689 -0.0001 0.090 Uiso 0.709(16) calc PR B 1 H42B H -0.0722 0.5613 0.0190 0.090 Uiso 0.709(16) calc PR B 1 C43 C 0.0094(5) 0.6618(5) 0.0150(2) 0.093(3) Uiso 0.709(16) d PDU B 1 H43A H 0.0075 0.6797 0.0004 0.111 Uiso 0.709(16) calc PR B 1 H43B H -0.0171 0.6754 0.0252 0.111 Uiso 0.709(16) calc PR B 1 C44 C 0.0806(4) 0.6908(4) 0.02182(18) 0.068(3) Uiso 0.709(16) d PDU B 1 H44A H 0.0932 0.7307 0.0320 0.082 Uiso 0.709(16) calc PR B 1 H44B H 0.1129 0.7094 0.0091 0.082 Uiso 0.709(16) calc PR B 1 C42' C -0.0327(8) 0.5885(8) 0.0266(5) 0.084(7) Uiso 0.291(16) d PDU B 2 H42C H -0.0683 0.5711 0.0385 0.101 Uiso 0.291(16) calc PR B 2 H42D H -0.0578 0.5672 0.0128 0.101 Uiso 0.291(16) calc PR B 2 C43' C 0.0043(9) 0.6673(9) 0.0254(5) 0.081(7) Uiso 0.291(16) d PDU B 2 H43C H 0.0109 0.6838 0.0101 0.098 Uiso 0.291(16) calc PR B 2 H43D H -0.0223 0.6864 0.0333 0.098 Uiso 0.291(16) calc PR B 2 C44' C 0.0711(8) 0.6882(8) 0.0355(4) 0.067(6) Uiso 0.291(16) d PDU B 2 H44C H 0.1087 0.7333 0.0289 0.080 Uiso 0.291(16) calc PR B 2 H44D H 0.0683 0.6965 0.0512 0.080 Uiso 0.291(16) calc PR B 2 O3 O 0.1860(9) 0.4009(8) -0.0472(3) 0.215(7) Uiso 0.604(15) d PDU C 1 C51 C 0.1305(11) 0.3813(11) -0.0631(3) 0.190(8) Uiso 0.604(15) d PDU C 1 H51A H 0.0860 0.3750 -0.0564 0.228 Uiso 0.604(15) calc PR C 1 H51B H 0.1456 0.4168 -0.0750 0.228 Uiso 0.604(15) calc PR C 1 C52 C 0.1223(11) 0.3157(12) -0.0704(3) 0.190(8) Uiso 0.604(15) d PDU C 1 H52A H 0.1266 0.3170 -0.0865 0.228 Uiso 0.604(15) calc PR C 1 H52B H 0.0740 0.2766 -0.0665 0.228 Uiso 0.604(15) calc PR C 1 C53 C 0.1761(11) 0.3009(11) -0.0609(3) 0.176(8) Uiso 0.604(15) d PDU C 1 H53A H 0.2200 0.3215 -0.0699 0.211 Uiso 0.604(15) calc PR C 1 H53B H 0.1571 0.2489 -0.0592 0.211 Uiso 0.604(15) calc PR C 1 C54 C 0.1898(11) 0.3367(11) -0.0396(3) 0.169(7) Uiso 0.604(15) d PDU C 1 H54A H 0.2373 0.3497 -0.0337 0.203 Uiso 0.604(15) calc PR C 1 H54B H 0.1522 0.3081 -0.0288 0.203 Uiso 0.604(15) calc PR C 1 O3' O 0.1377(14) 0.2470(12) -0.0463(5) 0.231(12) Uiso 0.396(15) d PDU C 2 C51' C 0.1628(19) 0.2935(17) -0.0287(4) 0.195(12) Uiso 0.396(15) d PDU C 2 H51C H 0.2084 0.2985 -0.0235 0.234 Uiso 0.396(15) calc PR C 2 H51D H 0.1278 0.2741 -0.0167 0.234 Uiso 0.396(15) calc PR C 2 C52' C 0.1738(18) 0.3627(14) -0.0351(5) 0.170(10) Uiso 0.396(15) d PDU C 2 H52C H 0.2235 0.4008 -0.0322 0.204 Uiso 0.396(15) calc PR C 2 H52D H 0.1406 0.3740 -0.0273 0.204 Uiso 0.396(15) calc PR C 2 C53' C 0.158(3) 0.3544(16) -0.0591(5) 0.248(13) Uiso 0.396(15) d PDU C 2 H53C H 0.1256 0.3725 -0.0629 0.298 Uiso 0.396(15) calc PR C 2 H53D H 0.2031 0.3821 -0.0675 0.298 Uiso 0.396(15) calc PR C 2 C54' C 0.125(2) 0.2787(17) -0.0645(5) 0.198(12) Uiso 0.396(15) d PDU C 2 H54C H 0.0733 0.2579 -0.0670 0.238 Uiso 0.396(15) calc PR C 2 H54D H 0.1471 0.2717 -0.0777 0.238 Uiso 0.396(15) calc PR C 2 O4 O 0.128(2) 0.155(2) -0.0109(7) 0.308(17) Uiso 0.33 d PDU D -1 C61 C 0.061(2) 0.129(2) -0.0222(5) 0.227(16) Uiso 0.33 d PDU D -1 H61A H 0.0349 0.0763 -0.0230 0.272 Uiso 0.33 calc PR D -1 H61B H 0.0690 0.1490 -0.0371 0.272 Uiso 0.33 calc PR D -1 C62 C 0.025(2) 0.156(3) -0.0085(7) 0.237(18) Uiso 0.33 d PDU D -1 H62A H 0.0453 0.2081 -0.0099 0.284 Uiso 0.33 calc PR D -1 H62B H -0.0273 0.1314 -0.0115 0.284 Uiso 0.33 calc PR D -1 C63 C 0.040(3) 0.136(2) 0.0127(5) 0.235(17) Uiso 0.33 d PDU D -1 H63A H 0.0119 0.0838 0.0149 0.281 Uiso 0.33 calc PR D -1 H63B H 0.0285 0.1600 0.0246 0.281 Uiso 0.33 calc PR D -1 C64 C 0.116(3) 0.161(3) 0.0117(7) 0.239(17) Uiso 0.33 d PDU D -1 H64A H 0.1442 0.2117 0.0165 0.287 Uiso 0.33 calc PR D -1 H64B H 0.1286 0.1316 0.0207 0.287 Uiso 0.33 calc PR D -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 P1 0.0375(6) 0.0387(6) 0.0387(6) -0.0010(5) -0.0001(5) 0.0185(5) N1 0.0381(19) 0.0388(19) 0.0423(19) 0.0002(15) 0.0009(15) 0.0195(16) N2 0.0393(19) 0.040(2) 0.044(2) 0.0011(16) 0.0029(16) 0.0167(17) N3 0.046(2) 0.055(2) 0.043(2) -0.0070(17) -0.0023(18) 0.0292(19) Li1 0.052(4) 0.056(5) 0.057(5) -0.010(4) 0.000(4) 0.027(4) C11 0.039(2) 0.044(3) 0.048(3) 0.006(2) -0.007(2) 0.018(2) C12 0.051(3) 0.043(3) 0.072(3) 0.000(2) -0.002(2) 0.022(2) C13 0.064(3) 0.048(3) 0.105(4) -0.002(3) -0.014(3) 0.028(3) C14 0.057(4) 0.050(3) 0.132(6) 0.030(4) -0.008(4) 0.017(3) C15 0.056(3) 0.068(4) 0.102(4) 0.040(3) 0.013(3) 0.026(3) C16 0.049(3) 0.056(3) 0.068(3) 0.019(2) 0.005(2) 0.025(2) C21 0.039(2) 0.039(2) 0.043(3) -0.0037(19) -0.003(2) 0.013(2) C22 0.066(3) 0.094(4) 0.042(3) -0.008(3) 0.000(2) 0.045(3) C23 0.099(5) 0.135(6) 0.039(3) -0.010(3) -0.008(3) 0.070(4) C24 0.083(4) 0.112(5) 0.056(4) 0.001(3) -0.017(3) 0.056(4) C25 0.057(3) 0.077(4) 0.060(3) -0.002(3) -0.010(2) 0.037(3) C26 0.047(3) 0.057(3) 0.043(3) -0.001(2) -0.001(2) 0.025(2) O1 0.075(2) 0.089(3) 0.071(2) -0.028(2) 0.0037(19) 0.043(2) C31 0.104(5) 0.158(7) 0.068(4) -0.022(4) -0.012(4) 0.084(5) O2 0.0470(19) 0.057(2) 0.100(3) -0.0095(19) -0.0070(18) 0.0267(17) C41 0.050(3) 0.064(3) 0.108(5) 0.014(3) 0.004(3) 0.019(3) _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 N2 1.592(3) . ? P1 N1 1.614(3) 2_665 ? P1 N1 1.621(3) . ? P1 N3 1.708(4) . ? P1 Li1 2.634(7) . ? N1 P1 1.614(3) 3_565 ? N1 Li1 2.054(8) . ? N2 C11 1.387(5) . ? N2 Li1 2.038(8) . ? N3 C21 1.387(5) . ? Li1 O1 1.954(8) . ? Li1 O2 1.969(8) . ? C11 C12 1.398(6) . ? C11 C16 1.407(6) . ? C12 C13 1.382(7) . ? C13 C14 1.392(8) . ? C14 C15 1.367(9) . ? C15 C16 1.374(7) . ? C21 C22 1.385(6) . ? C21 C26 1.393(6) . ? C22 C23 1.376(7) . ? C23 C24 1.369(8) . ? C24 C25 1.368(7) . ? C25 C26 1.379(6) . ? O1 C31 1.412(7) . ? O1 C34 1.425(12) . ? O1 C34' 1.493(9) . ? C31 C32 1.460(13) . ? C31 C32' 1.498(13) . ? C32 C33 1.443(14) . ? C33 C34 1.528(15) . ? C32' C33' 1.475(13) . ? C33' C34' 1.529(12) . ? O2 C44' 1.407(13) . ? O2 C41 1.433(6) . ? O2 C44 1.478(7) . ? C41 C42' 1.456(13) . ? C41 C42 1.513(8) . ? C42 C43 1.442(10) . ? C43 C44 1.403(10) . ? C42' C43' 1.479(15) . ? C43' C44' 1.423(15) . ? O3 C51 1.434(14) . ? O3 C54 1.506(14) . ? C51 C52 1.412(15) . ? C52 C53 1.474(15) . ? C53 C54 1.475(14) . ? O3' C51' 1.391(16) . ? O3' C54' 1.406(17) . ? C51' C52' 1.447(16) . ? C52' C53' 1.504(16) . ? C53' C54' 1.459(16) . ? O4 C64 1.429(17) . ? O4 C61 1.431(17) . ? C61 C62 1.466(17) . ? C62 C63 1.457(17) . ? C63 C64 1.458(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 P1 N1 117.55(18) . 2_665 ? N2 P1 N1 101.83(17) . . ? N1 P1 N1 114.7(2) 2_665 . ? N2 P1 N3 112.28(18) . . ? N1 P1 N3 100.24(18) 2_665 . ? N1 P1 N3 110.54(18) . . ? N2 P1 Li1 50.6(2) . . ? N1 P1 Li1 135.1(2) 2_665 . ? N1 P1 Li1 51.2(2) . . ? N3 P1 Li1 124.6(2) . . ? P1 N1 P1 119.8(2) 3_565 . ? P1 N1 Li1 144.6(3) 3_565 . ? P1 N1 Li1 90.8(3) . . ? C11 N2 P1 126.5(3) . . ? C11 N2 Li1 141.2(4) . . ? P1 N2 Li1 92.2(3) . . ? C21 N3 P1 131.4(3) . . ? O1 Li1 O2 101.5(4) . . ? O1 Li1 N2 129.4(4) . . ? O2 Li1 N2 113.6(4) . . ? O1 Li1 N1 115.1(4) . . ? O2 Li1 N1 122.9(4) . . ? N2 Li1 N1 75.1(3) . . ? O1 Li1 P1 132.5(4) . . ? O2 Li1 P1 125.9(4) . . ? N2 Li1 P1 37.16(16) . . ? N1 Li1 P1 37.98(16) . . ? N2 C11 C12 125.4(4) . . ? N2 C11 C16 118.3(4) . . ? C12 C11 C16 116.3(4) . . ? C13 C12 C11 121.6(5) . . ? C12 C13 C14 120.3(5) . . ? C15 C14 C13 119.1(5) . . ? C14 C15 C16 120.7(5) . . ? C15 C16 C11 121.9(5) . . ? C22 C21 N3 119.9(4) . . ? C22 C21 C26 117.6(4) . . ? N3 C21 C26 122.5(4) . . ? C23 C22 C21 121.1(5) . . ? C24 C23 C22 120.7(5) . . ? C25 C24 C23 119.2(5) . . ? C24 C25 C26 120.7(5) . . ? C25 C26 C21 120.7(4) . . ? C31 O1 C34 107.5(7) . . ? C31 O1 C34' 106.4(5) . . ? C34 O1 C34' 27.3(8) . . ? C31 O1 Li1 119.4(4) . . ? C34 O1 Li1 131.8(8) . . ? C34' O1 Li1 120.2(5) . . ? O1 C31 C32 108.0(7) . . ? O1 C31 C32' 105.7(7) . . ? C32 C31 C32' 18.0(14) . . ? C33 C32 C31 103.7(10) . . ? C32 C33 C34 108.1(11) . . ? O1 C34 C33 99.4(10) . . ? C33' C32' C31 105.8(10) . . ? C32' C33' C34' 98.5(10) . . ? O1 C34' C33' 99.8(8) . . ? C44' O2 C41 105.7(7) . . ? C44' O2 C44 34.6(9) . . ? C41 O2 C44 107.4(4) . . ? C44' O2 Li1 126.7(7) . . ? C41 O2 Li1 123.0(4) . . ? C44 O2 Li1 128.1(4) . . ? O2 C41 C42' 107.0(7) . . ? O2 C41 C42 105.1(5) . . ? C42' C41 C42 30.8(11) . . ? C43 C42 C41 105.9(6) . . ? C44 C43 C42 106.8(7) . . ? C43 C44 O2 108.7(6) . . ? C41 C42' C43' 107.0(11) . . ? C44' C43' C42' 102.8(12) . . ? O2 C44' C43' 109.5(12) . . ? C51 O3 C54 111.3(13) . . ? C52 C51 O3 100.4(12) . . ? C51 C52 C53 112.1(13) . . ? C52 C53 C54 102.2(12) . . ? C53 C54 O3 96.7(12) . . ? C51' O3' C54' 111.4(16) . . ? O3' C51' C52' 109.8(15) . . ? C51' C52' C53' 103.5(14) . . ? C54' C53' C52' 108.0(15) . . ? O3' C54' C53' 105.2(16) . . ? C64 O4 C61 108.6(18) . . ? O4 C61 C62 101.5(18) . . ? C63 C62 C61 99.0(18) . . ? C62 C63 C64 103.0(18) . . ? O4 C64 C63 103.4(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 P1 N1 P1 160.4(2) . . . 3_565 ? N1 P1 N1 P1 32.3(4) 2_665 . . 3_565 ? N3 P1 N1 P1 -80.1(3) . . . 3_565 ? Li1 P1 N1 P1 161.4(4) . . . 3_565 ? N2 P1 N1 Li1 -1.0(3) . . . . ? N1 P1 N1 Li1 -129.1(3) 2_665 . . . ? N3 P1 N1 Li1 118.4(3) . . . . ? N1 P1 N2 C11 -55.9(4) 2_665 . . . ? N1 P1 N2 C11 177.8(3) . . . . ? N3 P1 N2 C11 59.6(4) . . . . ? Li1 P1 N2 C11 176.8(5) . . . . ? N1 P1 N2 Li1 127.3(3) 2_665 . . . ? N1 P1 N2 Li1 1.0(3) . . . . ? N3 P1 N2 Li1 -117.2(3) . . . . ? N2 P1 N3 C21 69.6(4) . . . . ? N1 P1 N3 C21 -164.8(4) 2_665 . . . ? N1 P1 N3 C21 -43.4(4) . . . . ? Li1 P1 N3 C21 13.0(5) . . . . ? C11 N2 Li1 O1 72.8(8) . . . . ? P1 N2 Li1 O1 -111.3(5) . . . . ? C11 N2 Li1 O2 -56.9(7) . . . . ? P1 N2 Li1 O2 119.0(4) . . . . ? C11 N2 Li1 N1 -176.7(5) . . . . ? P1 N2 Li1 N1 -0.8(2) . . . . ? C11 N2 Li1 P1 -175.9(6) . . . . ? P1 N1 Li1 O1 -23.8(8) 3_565 . . . ? P1 N1 Li1 O1 127.7(4) . . . . ? P1 N1 Li1 O2 100.6(6) 3_565 . . . ? P1 N1 Li1 O2 -107.9(4) . . . . ? P1 N1 Li1 N2 -150.7(4) 3_565 . . . ? P1 N1 Li1 N2 0.8(2) . . . . ? P1 N1 Li1 P1 -151.5(5) 3_565 . . . ? N2 P1 Li1 O1 102.5(6) . . . . ? N1 P1 Li1 O1 11.1(7) 2_665 . . . ? N1 P1 Li1 O1 -76.2(5) . . . . ? N3 P1 Li1 O1 -165.8(4) . . . . ? N2 P1 Li1 O2 -82.0(4) . . . . ? N1 P1 Li1 O2 -173.4(3) 2_665 . . . ? N1 P1 Li1 O2 99.3(5) . . . . ? N3 P1 Li1 O2 9.7(6) . . . . ? N1 P1 Li1 N2 -91.3(3) 2_665 . . . ? N1 P1 Li1 N2 -178.7(3) . . . . ? N3 P1 Li1 N2 91.7(3) . . . . ? N2 P1 Li1 N1 178.7(3) . . . . ? N1 P1 Li1 N1 87.3(3) 2_665 . . . ? N3 P1 Li1 N1 -89.6(3) . . . . ? P1 N2 C11 C12 -3.6(6) . . . . ? Li1 N2 C11 C12 171.3(5) . . . . ? P1 N2 C11 C16 176.1(3) . . . . ? Li1 N2 C11 C16 -9.0(7) . . . . ? N2 C11 C12 C13 -179.5(4) . . . . ? C16 C11 C12 C13 0.8(7) . . . . ? C11 C12 C13 C14 -0.3(8) . . . . ? C12 C13 C14 C15 -0.8(8) . . . . ? C13 C14 C15 C16 1.4(9) . . . . ? C14 C15 C16 C11 -0.9(8) . . . . ? N2 C11 C16 C15 -179.9(4) . . . . ? C12 C11 C16 C15 -0.2(7) . . . . ? P1 N3 C21 C22 163.7(4) . . . . ? P1 N3 C21 C26 -15.4(6) . . . . ? N3 C21 C22 C23 179.4(5) . . . . ? C26 C21 C22 C23 -1.5(7) . . . . ? C21 C22 C23 C24 1.1(9) . . . . ? C22 C23 C24 C25 -0.2(10) . . . . ? C23 C24 C25 C26 -0.3(9) . . . . ? C24 C25 C26 C21 -0.2(8) . . . . ? C22 C21 C26 C25 1.0(7) . . . . ? N3 C21 C26 C25 -179.8(4) . . . . ? O2 Li1 O1 C31 -165.7(5) . . . . ? N2 Li1 O1 C31 60.3(7) . . . . ? N1 Li1 O1 C31 -30.7(7) . . . . ? P1 Li1 O1 C31 10.6(8) . . . . ? O2 Li1 O1 C34 -0.3(13) . . . . ? N2 Li1 O1 C34 -134.3(12) . . . . ? N1 Li1 O1 C34 134.7(12) . . . . ? P1 Li1 O1 C34 175.9(12) . . . . ? O2 Li1 O1 C34' -31.1(8) . . . . ? N2 Li1 O1 C34' -165.1(7) . . . . ? N1 Li1 O1 C34' 103.9(8) . . . . ? P1 Li1 O1 C34' 145.2(7) . . . . ? C34 O1 C31 C32 -30.7(17) . . . . ? C34' O1 C31 C32 -2.2(14) . . . . ? Li1 O1 C31 C32 137.9(12) . . . . ? C34 O1 C31 C32' -12.0(17) . . . . ? C34' O1 C31 C32' 16.5(14) . . . . ? Li1 O1 C31 C32' 156.6(11) . . . . ? O1 C31 C32 C33 9.8(19) . . . . ? C32' C31 C32 C33 -76(3) . . . . ? C31 C32 C33 C34 13(2) . . . . ? C31 O1 C34 C33 36.2(19) . . . . ? C34' O1 C34 C33 -55.7(14) . . . . ? Li1 O1 C34 C33 -130.4(12) . . . . ? C32 C33 C34 O1 -30(2) . . . . ? O1 C31 C32' C33' 15.0(16) . . . . ? C32 C31 C32' C33' 115(4) . . . . ? C31 C32' C33' C34' -38.8(16) . . . . ? C31 O1 C34' C33' -40.5(12) . . . . ? C34 O1 C34' C33' 56.1(15) . . . . ? Li1 O1 C34' C33' 179.8(9) . . . . ? C32' C33' C34' O1 47.3(13) . . . . ? O1 Li1 O2 C44' 42.2(14) . . . . ? N2 Li1 O2 C44' -175.2(14) . . . . ? N1 Li1 O2 C44' -88.1(14) . . . . ? P1 Li1 O2 C44' -134.4(14) . . . . ? O1 Li1 O2 C41 -110.0(5) . . . . ? N2 Li1 O2 C41 32.7(6) . . . . ? N1 Li1 O2 C41 119.7(5) . . . . ? P1 Li1 O2 C41 73.4(6) . . . . ? O1 Li1 O2 C44 86.1(7) . . . . ? N2 Li1 O2 C44 -131.2(6) . . . . ? N1 Li1 O2 C44 -44.2(8) . . . . ? P1 Li1 O2 C44 -90.5(7) . . . . ? C44' O2 C41 C42' 15.0(15) . . . . ? C44 O2 C41 C42' -21.1(14) . . . . ? Li1 O2 C41 C42' 172.1(14) . . . . ? C44' O2 C41 C42 47.0(11) . . . . ? C44 O2 C41 C42 10.9(7) . . . . ? Li1 O2 C41 C42 -155.8(6) . . . . ? O2 C41 C42 C43 -22.2(9) . . . . ? C42' C41 C42 C43 75.9(15) . . . . ? C41 C42 C43 C44 25.3(11) . . . . ? C42 C43 C44 O2 -18.8(11) . . . . ? C44' O2 C44 C43 -88.1(13) . . . . ? C41 O2 C44 C43 4.4(9) . . . . ? Li1 O2 C44 C43 170.3(6) . . . . ? O2 C41 C42' C43' 2(2) . . . . ? C42 C41 C42' C43' -89(2) . . . . ? C41 C42' C43' C44' -18(3) . . . . ? C41 O2 C44' C43' -27.8(19) . . . . ? C44 O2 C44' C43' 70.3(17) . . . . ? Li1 O2 C44' C43' 176.2(13) . . . . ? C42' C43' C44' O2 28(3) . . . . ? C54 O3 C51 C52 -21(2) . . . . ? O3 C51 C52 C53 -6(3) . . . . ? C51 C52 C53 C54 30(3) . . . . ? C52 C53 C54 O3 -38.2(19) . . . . ? C51 O3 C54 C53 39(2) . . . . ? C54' O3' C51' C52' -5(4) . . . . ? O3' C51' C52' C53' -5(4) . . . . ? C51' C52' C53' C54' 12(5) . . . . ? C51' O3' C54' C53' 12(5) . . . . ? C52' C53' C54' O3' -14(5) . . . . ? C64 O4 C61 C62 28(5) . . . . ? O4 C61 C62 C63 -45(4) . . . . ? C61 C62 C63 C64 47(4) . . . . ? C61 O4 C64 C63 2(5) . . . . ? C62 C63 C64 O4 -31(5) . . . . ? _diffrn_measured_fraction_theta_max 0.304 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.304 _refine_diff_density_max 0.484 _refine_diff_density_min -0.269 _refine_diff_density_rms 0.051