Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Alexander Steiner' 'Jamie F. Bickley' 'Richard Bonar-Law' 'Gavin T. Lawson' 'Philip I. Richards' ; F.Rivals ; 'Stefano Zacchini' _publ_contact_author_name 'Dr Alexander Steiner' _publ_contact_author_address ; Department of Chemistry University of Liverpool Crown Street Liverpool L69 7ZD UNITED KINGDOM ; _publ_contact_author_email A.STEINER@LIV.AC.UK _publ_section_title ; Supramolecular variations on a molecular theme: The structural diversity of phosphazenes (RNH)6P3N3 in the solid state ; data_P1(B212308H) _database_code_CSD 199621 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H60 N9 P3' _chemical_formula_weight 567.72 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 P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 10.4238(18) _cell_length_b 11.4040(19) _cell_length_c 14.704(2) _cell_angle_alpha 101.117(3) _cell_angle_beta 108.382(3) _cell_angle_gamma 90.023(3) _cell_volume 1624.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(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 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.161 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 0.212 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart Apex CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9422 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.0861 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7736 _reflns_number_gt 6083 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.47(8) _refine_ls_number_reflns 7736 _refine_ls_number_parameters 721 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1038 _refine_ls_wR_factor_gt 0.1001 _refine_ls_goodness_of_fit_ref 0.925 _refine_ls_restrained_S_all 0.923 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P11 P 0.62622(11) 0.30209(9) 0.86246(8) 0.0168(3) Uani 1 1 d . . . N11 N 0.6870(4) 0.2148(3) 0.9326(2) 0.0171(8) Uani 1 1 d . . . P12 P 0.68373(11) 0.07505(10) 0.89681(8) 0.0172(3) Uani 1 1 d . . . N12 N 0.5932(4) 0.0254(3) 0.7873(3) 0.0177(8) Uani 1 1 d . . . P13 P 0.57148(11) 0.10643(10) 0.70851(8) 0.0176(3) Uani 1 1 d . . . N13 N 0.5766(4) 0.2454(3) 0.7481(3) 0.0176(8) Uani 1 1 d . . . N110 N 0.4931(4) 0.3664(3) 0.8784(3) 0.0205(9) Uani 1 1 d D . . H110 H 0.428(4) 0.351(4) 0.833(3) 0.025 Uiso 1 1 d D . . C111 C 0.4706(5) 0.4449(4) 0.9623(3) 0.0221(11) Uani 1 1 d . . . C112 C 0.4912(6) 0.5749(4) 0.9569(4) 0.0357(14) Uani 1 1 d . . . H11A H 0.5865 0.5930 0.9647 0.054 Uiso 1 1 calc R . . H11B H 0.4665 0.6271 1.0092 0.054 Uiso 1 1 calc R . . H11C H 0.4339 0.5886 0.8932 0.054 Uiso 1 1 calc R . . C113 C 0.5669(5) 0.4211(4) 1.0570(3) 0.0275(12) Uani 1 1 d . . . H11D H 0.6603 0.4403 1.0606 0.041 Uiso 1 1 calc R . . H11E H 0.5559 0.3365 1.0593 0.041 Uiso 1 1 calc R . . H11F H 0.5470 0.4712 1.1124 0.041 Uiso 1 1 calc R . . C114 C 0.3263(5) 0.4200(4) 0.9573(4) 0.0338(13) Uani 1 1 d . . . H11G H 0.2647 0.4347 0.8953 0.051 Uiso 1 1 calc R . . H11H H 0.3077 0.4729 1.0120 0.051 Uiso 1 1 calc R . . H11I H 0.3127 0.3364 0.9612 0.051 Uiso 1 1 calc R . . N120 N 0.6368(4) -0.0048(3) 0.9636(3) 0.0204(9) Uani 1 1 d D . . H120 H 0.693(4) 0.015(4) 1.014(2) 0.025 Uiso 1 1 d D . . C121 C 0.4985(5) -0.0319(4) 0.9616(3) 0.0244(11) Uani 1 1 d . . . C122 C 0.4185(5) 0.0783(4) 0.9643(4) 0.0344(13) Uani 1 1 d . . . H12A H 0.4639 0.1374 1.0241 0.052 Uiso 1 1 calc R . . H12B H 0.3271 0.0564 0.9635 0.052 Uiso 1 1 calc R . . H12C H 0.4124 0.1127 0.9070 0.052 Uiso 1 1 calc R . . C123 C 0.5126(6) -0.0811(5) 1.0540(4) 0.0371(13) Uani 1 1 d . . . H12D H 0.5536 -0.0181 1.1120 0.056 Uiso 1 1 calc R . . H12E H 0.5704 -0.1490 1.0555 0.056 Uiso 1 1 calc R . . H12F H 0.4229 -0.1078 1.0534 0.056 Uiso 1 1 calc R . . C124 C 0.4285(5) -0.1255(4) 0.8736(4) 0.0329(13) Uani 1 1 d . . . H12G H 0.4794 -0.1978 0.8750 0.049 Uiso 1 1 calc R . . H12H H 0.4234 -0.0957 0.8144 0.049 Uiso 1 1 calc R . . H12I H 0.3368 -0.1447 0.8734 0.049 Uiso 1 1 calc R . . N130 N 0.4316(4) 0.0705(3) 0.6170(3) 0.0226(9) Uani 1 1 d D . . H130 H 0.425(5) 0.003(2) 0.591(3) 0.027 Uiso 1 1 d D . . C131 C 0.2935(5) 0.1069(4) 0.6084(3) 0.0256(11) Uani 1 1 d . . . C132 C 0.2825(5) 0.2338(4) 0.5938(4) 0.0348(14) Uani 1 1 d . . . H13A H 0.2967 0.2386 0.5318 0.052 Uiso 1 1 calc R . . H13B H 0.3514 0.2862 0.6479 0.052 Uiso 1 1 calc R . . H13C H 0.1923 0.2595 0.5923 0.052 Uiso 1 1 calc R . . C133 C 0.2542(5) 0.0950(5) 0.6965(4) 0.0348(13) Uani 1 1 d . . . H13D H 0.2638 0.0125 0.7064 0.052 Uiso 1 1 calc R . . H13E H 0.1599 0.1150 0.6860 0.052 Uiso 1 1 calc R . . H13F H 0.3134 0.1498 0.7545 0.052 Uiso 1 1 calc R . . C134 C 0.2002(5) 0.0241(4) 0.5191(4) 0.0338(13) Uani 1 1 d . . . H13G H 0.2061 -0.0585 0.5292 0.051 Uiso 1 1 calc R . . H13H H 0.2271 0.0297 0.4619 0.051 Uiso 1 1 calc R . . H13I H 0.1069 0.0472 0.5082 0.051 Uiso 1 1 calc R . . N140 N 0.7376(4) 0.4171(3) 0.8940(3) 0.0202(9) Uani 1 1 d D . . H140 H 0.702(5) 0.468(3) 0.869(3) 0.024 Uiso 1 1 d D . . C141 C 0.8840(4) 0.4156(4) 0.9110(3) 0.0215(11) Uani 1 1 d . . . C142 C 0.9309(5) 0.5397(4) 0.9094(4) 0.0332(13) Uani 1 1 d . . . H14A H 0.9048 0.5982 0.9576 0.050 Uiso 1 1 calc R . . H14B H 0.8888 0.5567 0.8440 0.050 Uiso 1 1 calc R . . H14C H 1.0297 0.5451 0.9255 0.050 Uiso 1 1 calc R . . C143 C 0.9536(5) 0.3905(4) 1.0126(4) 0.0293(12) Uani 1 1 d . . . H14D H 0.9402 0.4559 1.0621 0.044 Uiso 1 1 calc R . . H14E H 1.0508 0.3845 1.0229 0.044 Uiso 1 1 calc R . . H14F H 0.9146 0.3150 1.0181 0.044 Uiso 1 1 calc R . . C144 C 0.9177(5) 0.3250(4) 0.8345(4) 0.0312(12) Uani 1 1 d . . . H14G H 0.8836 0.2450 0.8347 0.047 Uiso 1 1 calc R . . H14H H 1.0162 0.3265 0.8490 0.047 Uiso 1 1 calc R . . H14I H 0.8754 0.3444 0.7700 0.047 Uiso 1 1 calc R . . N150 N 0.8440(4) 0.0490(3) 0.9211(3) 0.0224(9) Uani 1 1 d D . . H150 H 0.884(4) 0.111(3) 0.941(4) 0.027 Uiso 1 1 d D . . C151 C 0.9121(5) -0.0640(4) 0.9149(4) 0.0284(12) Uani 1 1 d . . . C152 C 1.0405(5) -0.0388(5) 0.8955(5) 0.0528(17) Uani 1 1 d . . . H15A H 1.0194 -0.0124 0.8331 0.079 Uiso 1 1 calc R . . H15B H 1.0899 -0.1118 0.8924 0.079 Uiso 1 1 calc R . . H15C H 1.0966 0.0242 0.9484 0.079 Uiso 1 1 calc R . . C153 C 0.9446(6) -0.1051(5) 1.0124(4) 0.0450(16) Uani 1 1 d . . . H15D H 0.8600 -0.1222 1.0246 0.067 Uiso 1 1 calc R . . H15E H 0.9999 -0.0418 1.0654 0.067 Uiso 1 1 calc R . . H15F H 0.9946 -0.1777 1.0096 0.067 Uiso 1 1 calc R . . C154 C 0.8238(6) -0.1601(4) 0.8352(4) 0.0400(15) Uani 1 1 d . . . H15G H 0.7396 -0.1744 0.8488 0.060 Uiso 1 1 calc R . . H15H H 0.8715 -0.2341 0.8322 0.060 Uiso 1 1 calc R . . H15I H 0.8026 -0.1347 0.7724 0.060 Uiso 1 1 calc R . . N160 N 0.6864(4) 0.0668(4) 0.6562(3) 0.0270(10) Uani 1 1 d D . . H160 H 0.738(4) 0.026(4) 0.683(4) 0.032 Uiso 1 1 d D . . C161 C 0.7091(5) 0.0940(5) 0.5689(4) 0.0308(12) Uani 1 1 d . . . C162 C 0.6654(6) 0.2171(5) 0.5556(4) 0.0397(14) Uani 1 1 d . . . H16A H 0.5685 0.2204 0.5473 0.060 Uiso 1 1 calc R . . H16B H 0.6821 0.2345 0.4974 0.060 Uiso 1 1 calc R . . H16C H 0.7170 0.2766 0.6133 0.060 Uiso 1 1 calc R . . C163 C 0.6343(6) 0.0017(5) 0.4781(4) 0.0477(16) Uani 1 1 d . . . H16D H 0.5364 0.0064 0.4649 0.072 Uiso 1 1 calc R . . H16E H 0.6597 -0.0785 0.4886 0.072 Uiso 1 1 calc R . . H16F H 0.6583 0.0176 0.4221 0.072 Uiso 1 1 calc R . . C164 C 0.8594(6) 0.0921(5) 0.5863(4) 0.0498(16) Uani 1 1 d . . . H16G H 0.9074 0.1516 0.6452 0.075 Uiso 1 1 calc R . . H16H H 0.8797 0.1110 0.5299 0.075 Uiso 1 1 calc R . . H16I H 0.8890 0.0123 0.5953 0.075 Uiso 1 1 calc R . . P21 P 0.20226(11) 0.55702(10) 0.49627(8) 0.0177(3) Uani 1 1 d . . . N21 N 0.1786(4) 0.4349(3) 0.4186(3) 0.0181(9) Uani 1 1 d . . . P22 P 0.09069(12) 0.42914(10) 0.30887(8) 0.0197(3) Uani 1 1 d . . . N22 N 0.0869(4) 0.5503(3) 0.2707(3) 0.0193(9) Uani 1 1 d . . . P23 P 0.15195(11) 0.67251(10) 0.34060(8) 0.0170(3) Uani 1 1 d . . . N23 N 0.2009(4) 0.6737(3) 0.4537(3) 0.0186(9) Uani 1 1 d . . . N210 N 0.0874(4) 0.5471(3) 0.5489(3) 0.0230(9) Uani 1 1 d D . . H210 H 0.029(4) 0.489(3) 0.519(3) 0.028 Uiso 1 1 d D . . C211 C 0.0647(5) 0.6225(4) 0.6340(3) 0.0292(12) Uani 1 1 d . . . C212 C 0.1108(6) 0.7506(4) 0.6458(4) 0.0396(14) Uani 1 1 d . . . H21A H 0.2090 0.7571 0.6593 0.059 Uiso 1 1 calc R . . H21B H 0.0879 0.7997 0.7003 0.059 Uiso 1 1 calc R . . H21C H 0.0655 0.7788 0.5854 0.059 Uiso 1 1 calc R . . C213 C 0.1376(6) 0.5769(5) 0.7259(4) 0.0486(16) Uani 1 1 d . . . H21D H 0.2357 0.5865 0.7392 0.073 Uiso 1 1 calc R . . H21E H 0.1105 0.4920 0.7166 0.073 Uiso 1 1 calc R . . H21F H 0.1139 0.6228 0.7812 0.073 Uiso 1 1 calc R . . C214 C -0.0854(5) 0.6133(5) 0.6160(4) 0.0442(15) Uani 1 1 d . . . H21G H -0.1325 0.6427 0.5565 0.066 Uiso 1 1 calc R . . H21H H -0.1059 0.6617 0.6719 0.066 Uiso 1 1 calc R . . H21I H -0.1159 0.5294 0.6079 0.066 Uiso 1 1 calc R . . N220 N -0.0729(4) 0.3945(3) 0.2863(3) 0.0272(10) Uani 1 1 d D . . H220 H -0.134(4) 0.437(4) 0.260(3) 0.033 Uiso 1 1 d D . . C221 C -0.1401(5) 0.2867(4) 0.2918(4) 0.0301(12) Uani 1 1 d . . . C222 C -0.0560(5) 0.2316(5) 0.3753(4) 0.0343(13) Uani 1 1 d . . . H22A H 0.0234 0.1985 0.3603 0.051 Uiso 1 1 calc R . . H22B H -0.1107 0.1675 0.3842 0.051 Uiso 1 1 calc R . . H22C H -0.0263 0.2932 0.4356 0.051 Uiso 1 1 calc R . . C223 C -0.2705(6) 0.3249(5) 0.3118(5) 0.0519(16) Uani 1 1 d . . . H22D H -0.2484 0.3852 0.3727 0.078 Uiso 1 1 calc R . . H22E H -0.3195 0.2551 0.3181 0.078 Uiso 1 1 calc R . . H22F H -0.3274 0.3588 0.2575 0.078 Uiso 1 1 calc R . . C224 C -0.1776(6) 0.1958(4) 0.1978(4) 0.0400(15) Uani 1 1 d . . . H22G H -0.0957 0.1602 0.1888 0.060 Uiso 1 1 calc R . . H22H H -0.2216 0.2348 0.1430 0.060 Uiso 1 1 calc R . . H22I H -0.2401 0.1329 0.1999 0.060 Uiso 1 1 calc R . . N230 N 0.0437(4) 0.7740(3) 0.3083(3) 0.0205(9) Uani 1 1 d D . . H230 H 0.082(4) 0.841(3) 0.342(3) 0.025 Uiso 1 1 d D . . C231 C -0.1031(4) 0.7655(4) 0.2880(3) 0.0237(11) Uani 1 1 d . . . C232 C -0.1718(5) 0.6916(4) 0.1876(4) 0.0320(13) Uani 1 1 d . . . H23A H -0.1536 0.7303 0.1385 0.048 Uiso 1 1 calc R . . H23B H -0.2698 0.6846 0.1756 0.048 Uiso 1 1 calc R . . H23C H -0.1370 0.6116 0.1830 0.048 Uiso 1 1 calc R . . C233 C -0.1476(5) 0.8927(4) 0.2901(4) 0.0356(13) Uani 1 1 d . . . H23D H -0.1051 0.9417 0.3557 0.053 Uiso 1 1 calc R . . H23E H -0.2464 0.8918 0.2736 0.053 Uiso 1 1 calc R . . H23F H -0.1200 0.9268 0.2423 0.053 Uiso 1 1 calc R . . C234 C -0.1414(5) 0.7160(5) 0.3649(4) 0.0356(13) Uani 1 1 d . . . H23G H -0.1003 0.7686 0.4291 0.053 Uiso 1 1 calc R . . H23H H -0.1087 0.6356 0.3667 0.053 Uiso 1 1 calc R . . H23I H -0.2402 0.7116 0.3488 0.053 Uiso 1 1 calc R . . N240 N 0.3432(4) 0.5661(3) 0.5887(3) 0.0208(9) Uani 1 1 d D . . H240 H 0.336(5) 0.509(3) 0.615(3) 0.025 Uiso 1 1 d D . . C241 C 0.4810(5) 0.6015(4) 0.5949(3) 0.0232(11) Uani 1 1 d . . . C242 C 0.5172(5) 0.5434(5) 0.5069(4) 0.0332(13) Uani 1 1 d . . . H24A H 0.4535 0.5644 0.4482 0.050 Uiso 1 1 calc R . . H24B H 0.5125 0.4563 0.5007 0.050 Uiso 1 1 calc R . . H24C H 0.6094 0.5715 0.5140 0.050 Uiso 1 1 calc R . . C243 C 0.4954(5) 0.7358(4) 0.6088(4) 0.0340(13) Uani 1 1 d . . . H24D H 0.4791 0.7728 0.6698 0.051 Uiso 1 1 calc R . . H24E H 0.4293 0.7616 0.5536 0.051 Uiso 1 1 calc R . . H24F H 0.5871 0.7604 0.6122 0.051 Uiso 1 1 calc R . . C244 C 0.5738(5) 0.5631(4) 0.6847(4) 0.0344(13) Uani 1 1 d . . . H24G H 0.5507 0.6020 0.7425 0.052 Uiso 1 1 calc R . . H24H H 0.6680 0.5864 0.6932 0.052 Uiso 1 1 calc R . . H24I H 0.5628 0.4759 0.6766 0.052 Uiso 1 1 calc R . . N250 N 0.1331(4) 0.3139(3) 0.2430(3) 0.0251(10) Uani 1 1 d D . . H250 H 0.061(4) 0.293(4) 0.195(3) 0.030 Uiso 1 1 d D . . C251 C 0.2723(5) 0.2836(4) 0.2430(3) 0.0271(11) Uani 1 1 d . . . C252 C 0.2513(6) 0.1861(4) 0.1525(4) 0.0366(13) Uani 1 1 d . . . H25A H 0.1904 0.1211 0.1532 0.055 Uiso 1 1 calc R . . H25B H 0.3388 0.1550 0.1520 0.055 Uiso 1 1 calc R . . H25C H 0.2113 0.2193 0.0939 0.055 Uiso 1 1 calc R . . C253 C 0.3484(5) 0.3889(5) 0.2363(4) 0.0392(14) Uani 1 1 d . . . H25D H 0.3015 0.4150 0.1752 0.059 Uiso 1 1 calc R . . H25E H 0.4398 0.3676 0.2371 0.059 Uiso 1 1 calc R . . H25F H 0.3545 0.4540 0.2920 0.059 Uiso 1 1 calc R . . C254 C 0.3385(5) 0.2346(4) 0.3325(4) 0.0335(13) Uani 1 1 d . . . H25G H 0.2829 0.1655 0.3328 0.050 Uiso 1 1 calc R . . H25H H 0.3474 0.2965 0.3909 0.050 Uiso 1 1 calc R . . H25I H 0.4284 0.2097 0.3325 0.050 Uiso 1 1 calc R . . N260 N 0.2865(4) 0.7249(3) 0.3236(3) 0.0212(9) Uani 1 1 d D . . H260 H 0.357(3) 0.737(4) 0.372(3) 0.025 Uiso 1 1 d D . . C261 C 0.3079(4) 0.7583(4) 0.2378(3) 0.0198(10) Uani 1 1 d . . . C262 C 0.2117(5) 0.6862(4) 0.1444(3) 0.0270(11) Uani 1 1 d . . . H26A H 0.1182 0.7008 0.1421 0.040 Uiso 1 1 calc R . . H26B H 0.2258 0.6009 0.1418 0.040 Uiso 1 1 calc R . . H26C H 0.2283 0.7101 0.0883 0.040 Uiso 1 1 calc R . . C263 C 0.4509(5) 0.7324(4) 0.2422(4) 0.0329(12) Uani 1 1 d . . . H26D H 0.4635 0.6474 0.2427 0.049 Uiso 1 1 calc R . . H26E H 0.5140 0.7811 0.3020 0.049 Uiso 1 1 calc R . . H26F H 0.4682 0.7519 0.1849 0.049 Uiso 1 1 calc R . . C264 C 0.2906(5) 0.8912(4) 0.2406(4) 0.0320(13) Uani 1 1 d . . . H26G H 0.1968 0.9083 0.2359 0.048 Uiso 1 1 calc R . . H26H H 0.3117 0.9134 0.1855 0.048 Uiso 1 1 calc R . . H26I H 0.3521 0.9376 0.3023 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P11 0.0187(6) 0.0187(6) 0.0108(6) 0.0020(5) 0.0021(5) 0.0009(5) N11 0.021(2) 0.0210(19) 0.0080(19) 0.0011(15) 0.0040(16) 0.0015(15) P12 0.0177(6) 0.0196(6) 0.0126(6) 0.0027(5) 0.0027(5) 0.0017(5) N12 0.024(2) 0.0129(18) 0.015(2) 0.0004(15) 0.0056(16) 0.0017(15) P13 0.0175(6) 0.0222(6) 0.0109(6) 0.0011(5) 0.0028(5) 0.0003(5) N13 0.019(2) 0.023(2) 0.012(2) 0.0041(16) 0.0068(16) 0.0050(16) N110 0.018(2) 0.027(2) 0.013(2) 0.0006(17) 0.0015(16) 0.0053(17) C111 0.030(3) 0.020(2) 0.013(2) -0.0001(19) 0.005(2) 0.006(2) C112 0.050(4) 0.028(3) 0.025(3) 0.001(2) 0.009(3) 0.011(2) C113 0.037(3) 0.027(3) 0.015(2) -0.004(2) 0.008(2) 0.007(2) C114 0.032(3) 0.040(3) 0.030(3) 0.002(2) 0.014(2) 0.009(2) N120 0.021(2) 0.024(2) 0.011(2) 0.0051(17) -0.0016(16) 0.0011(17) C121 0.025(3) 0.028(3) 0.019(3) 0.004(2) 0.006(2) -0.004(2) C122 0.026(3) 0.041(3) 0.040(3) 0.005(3) 0.018(3) 0.003(2) C123 0.042(3) 0.046(3) 0.025(3) 0.009(3) 0.013(3) -0.011(3) C124 0.033(3) 0.031(3) 0.030(3) -0.001(2) 0.008(2) -0.008(2) N130 0.022(2) 0.023(2) 0.018(2) -0.0010(17) 0.0018(17) 0.0016(18) C131 0.019(2) 0.036(3) 0.016(2) 0.002(2) 0.001(2) 0.004(2) C132 0.034(3) 0.036(3) 0.027(3) 0.008(2) -0.002(2) 0.009(2) C133 0.022(3) 0.056(3) 0.024(3) 0.009(3) 0.005(2) 0.005(2) C134 0.021(3) 0.043(3) 0.030(3) 0.006(3) 0.000(2) 0.001(2) N140 0.019(2) 0.023(2) 0.017(2) 0.0071(17) 0.0014(17) 0.0047(16) C141 0.017(2) 0.023(2) 0.022(3) 0.004(2) 0.003(2) -0.0022(19) C142 0.025(3) 0.039(3) 0.031(3) 0.010(2) 0.000(2) -0.009(2) C143 0.024(3) 0.034(3) 0.024(3) 0.005(2) -0.001(2) -0.003(2) C144 0.028(3) 0.038(3) 0.025(3) 0.004(2) 0.007(2) -0.005(2) N150 0.021(2) 0.017(2) 0.025(2) -0.0019(18) 0.0048(17) -0.0022(16) C151 0.027(3) 0.022(2) 0.028(3) -0.001(2) 0.000(2) 0.005(2) C152 0.032(3) 0.050(4) 0.072(5) -0.006(3) 0.022(3) 0.012(3) C153 0.054(4) 0.036(3) 0.034(3) 0.004(3) 0.000(3) 0.017(3) C154 0.046(4) 0.026(3) 0.035(3) -0.003(2) 0.002(3) 0.012(2) N160 0.022(2) 0.036(2) 0.022(2) 0.0082(19) 0.0039(18) 0.0080(18) C161 0.028(3) 0.048(3) 0.016(3) 0.003(2) 0.009(2) 0.004(2) C162 0.041(3) 0.058(4) 0.029(3) 0.021(3) 0.016(3) 0.011(3) C163 0.049(4) 0.072(4) 0.018(3) -0.004(3) 0.013(3) -0.003(3) C164 0.043(4) 0.076(4) 0.041(4) 0.015(3) 0.027(3) 0.012(3) P21 0.0172(6) 0.0233(6) 0.0112(6) 0.0029(5) 0.0029(5) 0.0015(5) N21 0.023(2) 0.0129(18) 0.014(2) 0.0026(15) 0.0001(16) 0.0035(15) P22 0.0254(7) 0.0192(6) 0.0124(6) 0.0023(5) 0.0038(5) 0.0023(5) N22 0.021(2) 0.024(2) 0.0104(19) 0.0018(16) 0.0032(16) -0.0003(16) P23 0.0174(6) 0.0194(6) 0.0123(6) 0.0028(5) 0.0022(5) 0.0018(5) N23 0.023(2) 0.021(2) 0.0096(19) -0.0020(16) 0.0056(16) -0.0008(16) N210 0.017(2) 0.031(2) 0.019(2) -0.0002(18) 0.0074(17) -0.0035(17) C211 0.031(3) 0.044(3) 0.013(2) -0.001(2) 0.013(2) 0.001(2) C212 0.047(4) 0.044(3) 0.023(3) -0.010(2) 0.014(3) -0.001(3) C213 0.058(4) 0.070(4) 0.019(3) 0.007(3) 0.017(3) 0.007(3) C214 0.035(3) 0.065(4) 0.035(3) -0.002(3) 0.022(3) 0.007(3) N220 0.024(2) 0.030(2) 0.026(2) 0.0104(19) 0.0019(18) -0.0004(17) C221 0.027(3) 0.034(3) 0.026(3) 0.011(2) 0.002(2) -0.002(2) C222 0.035(3) 0.040(3) 0.026(3) 0.016(2) 0.001(2) -0.006(2) C223 0.038(4) 0.068(4) 0.057(4) 0.030(3) 0.015(3) 0.002(3) C224 0.044(4) 0.038(3) 0.027(3) 0.007(3) -0.003(3) -0.016(3) N230 0.020(2) 0.0180(19) 0.022(2) 0.0023(17) 0.0044(17) 0.0004(16) C231 0.016(2) 0.028(3) 0.025(3) 0.006(2) 0.003(2) 0.007(2) C232 0.024(3) 0.039(3) 0.027(3) 0.004(2) 0.000(2) 0.006(2) C233 0.028(3) 0.035(3) 0.038(3) 0.003(2) 0.005(2) 0.014(2) C234 0.023(3) 0.050(3) 0.037(3) 0.014(3) 0.011(2) 0.008(2) N240 0.023(2) 0.025(2) 0.015(2) 0.0058(17) 0.0056(17) 0.0007(18) C241 0.018(2) 0.032(3) 0.014(2) 0.003(2) -0.0018(19) -0.002(2) C242 0.023(3) 0.049(3) 0.021(3) -0.002(2) 0.003(2) -0.004(2) C243 0.030(3) 0.036(3) 0.028(3) 0.004(2) 0.001(2) -0.006(2) C244 0.023(3) 0.047(3) 0.025(3) 0.011(3) -0.006(2) 0.000(2) N250 0.030(2) 0.025(2) 0.013(2) -0.0024(17) 0.0010(17) 0.0015(18) C251 0.038(3) 0.027(3) 0.017(3) 0.001(2) 0.011(2) 0.005(2) C252 0.049(4) 0.037(3) 0.024(3) -0.001(2) 0.016(3) 0.015(3) C253 0.033(3) 0.049(3) 0.040(3) 0.008(3) 0.018(3) 0.006(3) C254 0.033(3) 0.038(3) 0.033(3) 0.013(2) 0.012(2) 0.020(2) N260 0.016(2) 0.029(2) 0.012(2) 0.0026(17) -0.0043(16) -0.0006(17) C261 0.019(2) 0.026(2) 0.017(2) 0.007(2) 0.0072(19) 0.0042(19) C262 0.030(3) 0.036(3) 0.019(3) 0.011(2) 0.011(2) 0.006(2) C263 0.031(3) 0.043(3) 0.029(3) 0.011(2) 0.014(2) 0.000(2) C264 0.039(3) 0.032(3) 0.031(3) 0.012(2) 0.016(3) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P11 N11 1.563(4) . ? P11 N13 1.595(4) . ? P11 N110 1.630(4) . ? P11 N140 1.645(4) . ? N11 P12 1.576(4) . ? P12 N12 1.579(4) . ? P12 N150 1.634(4) . ? P12 N120 1.637(4) . ? N12 P13 1.580(4) . ? P13 N13 1.575(4) . ? P13 N130 1.629(4) . ? P13 N160 1.636(5) . ? N110 C111 1.461(6) . ? C111 C114 1.506(7) . ? C111 C113 1.511(6) . ? C111 C112 1.519(6) . ? N120 C121 1.464(6) . ? C121 C124 1.490(6) . ? C121 C122 1.510(7) . ? C121 C123 1.532(7) . ? N130 C131 1.471(6) . ? C131 C132 1.503(6) . ? C131 C133 1.506(7) . ? C131 C134 1.509(6) . ? N140 C141 1.467(6) . ? C141 C144 1.503(7) . ? C141 C142 1.505(6) . ? C141 C143 1.523(6) . ? N150 C151 1.473(6) . ? C151 C152 1.493(7) . ? C151 C154 1.498(6) . ? C151 C153 1.530(8) . ? N160 C161 1.465(6) . ? C161 C162 1.506(7) . ? C161 C164 1.507(7) . ? C161 C163 1.516(7) . ? P21 N23 1.574(4) . ? P21 N21 1.585(3) . ? P21 N210 1.632(4) . ? P21 N240 1.644(4) . ? N21 P22 1.573(4) . ? P22 N22 1.584(4) . ? P22 N250 1.625(4) . ? P22 N220 1.664(4) . ? N22 P23 1.570(4) . ? P23 N23 1.576(4) . ? P23 N260 1.632(4) . ? P23 N230 1.648(4) . ? N210 C211 1.461(6) . ? C211 C212 1.498(7) . ? C211 C214 1.503(7) . ? C211 C213 1.515(7) . ? N220 C221 1.443(6) . ? C221 C224 1.498(7) . ? C221 C222 1.513(6) . ? C221 C223 1.526(8) . ? N230 C231 1.463(6) . ? C231 C232 1.502(6) . ? C231 C234 1.512(7) . ? C231 C233 1.521(6) . ? N240 C241 1.462(6) . ? C241 C242 1.494(7) . ? C241 C243 1.507(6) . ? C241 C244 1.514(6) . ? N250 C251 1.492(6) . ? C251 C253 1.475(7) . ? C251 C254 1.493(7) . ? C251 C252 1.516(6) . ? N260 C261 1.466(6) . ? C261 C263 1.503(6) . ? C261 C262 1.505(6) . ? C261 C264 1.520(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 P11 N13 116.43(18) . . ? N11 P11 N110 114.7(2) . . ? N13 P11 N110 102.92(19) . . ? N11 P11 N140 106.59(19) . . ? N13 P11 N140 113.6(2) . . ? N110 P11 N140 101.8(2) . . ? P11 N11 P12 123.4(2) . . ? N11 P12 N12 115.12(18) . . ? N11 P12 N150 103.25(19) . . ? N12 P12 N150 114.8(2) . . ? N11 P12 N120 115.0(2) . . ? N12 P12 N120 106.54(19) . . ? N150 P12 N120 101.6(2) . . ? P12 N12 P13 120.2(2) . . ? N13 P13 N12 116.01(19) . . ? N13 P13 N130 107.29(19) . . ? N12 P13 N130 113.6(2) . . ? N13 P13 N160 113.4(2) . . ? N12 P13 N160 103.9(2) . . ? N130 P13 N160 101.9(2) . . ? P13 N13 P11 121.7(2) . . ? C111 N110 P11 132.7(3) . . ? N110 C111 C114 107.7(4) . . ? N110 C111 C113 110.5(4) . . ? C114 C111 C113 110.1(4) . . ? N110 C111 C112 109.7(4) . . ? C114 C111 C112 109.2(4) . . ? C113 C111 C112 109.6(4) . . ? C121 N120 P12 127.3(3) . . ? N120 C121 C124 109.8(4) . . ? N120 C121 C122 112.1(4) . . ? C124 C121 C122 110.7(4) . . ? N120 C121 C123 106.0(4) . . ? C124 C121 C123 109.3(4) . . ? C122 C121 C123 108.8(4) . . ? C131 N130 P13 129.6(3) . . ? N130 C131 C132 109.7(4) . . ? N130 C131 C133 112.1(4) . . ? C132 C131 C133 110.0(4) . . ? N130 C131 C134 106.3(4) . . ? C132 C131 C134 109.6(4) . . ? C133 C131 C134 109.2(4) . . ? C141 N140 P11 128.1(3) . . ? N140 C141 C144 112.2(4) . . ? N140 C141 C142 106.3(4) . . ? C144 C141 C142 110.3(4) . . ? N140 C141 C143 109.1(4) . . ? C144 C141 C143 110.5(4) . . ? C142 C141 C143 108.3(4) . . ? C151 N150 P12 131.3(3) . . ? N150 C151 C152 107.0(4) . . ? N150 C151 C154 111.0(4) . . ? C152 C151 C154 110.8(5) . . ? N150 C151 C153 109.5(4) . . ? C152 C151 C153 109.7(4) . . ? C154 C151 C153 108.8(4) . . ? C161 N160 P13 132.1(3) . . ? N160 C161 C162 110.4(4) . . ? N160 C161 C164 106.6(4) . . ? C162 C161 C164 108.8(5) . . ? N160 C161 C163 111.3(4) . . ? C162 C161 C163 109.9(4) . . ? C164 C161 C163 109.8(5) . . ? N23 P21 N21 115.22(19) . . ? N23 P21 N210 114.4(2) . . ? N21 P21 N210 103.9(2) . . ? N23 P21 N240 107.44(19) . . ? N21 P21 N240 113.41(19) . . ? N210 P21 N240 101.8(2) . . ? P22 N21 P21 120.3(2) . . ? N21 P22 N22 115.96(18) . . ? N21 P22 N250 107.49(19) . . ? N22 P22 N250 115.5(2) . . ? N21 P22 N220 113.3(2) . . ? N22 P22 N220 102.05(19) . . ? N250 P22 N220 101.7(2) . . ? P23 N22 P22 122.4(2) . . ? N22 P23 N23 116.47(19) . . ? N22 P23 N260 114.8(2) . . ? N23 P23 N260 103.00(19) . . ? N22 P23 N230 106.28(19) . . ? N23 P23 N230 113.9(2) . . ? N260 P23 N230 101.6(2) . . ? P21 N23 P23 122.9(2) . . ? C211 N210 P21 131.7(3) . . ? N210 C211 C212 111.4(4) . . ? N210 C211 C214 106.3(4) . . ? C212 C211 C214 109.4(5) . . ? N210 C211 C213 110.3(4) . . ? C212 C211 C213 109.8(4) . . ? C214 C211 C213 109.6(5) . . ? C221 N220 P22 130.2(3) . . ? N220 C221 C224 112.5(4) . . ? N220 C221 C222 111.7(4) . . ? C224 C221 C222 110.1(4) . . ? N220 C221 C223 105.9(4) . . ? C224 C221 C223 108.1(4) . . ? C222 C221 C223 108.4(5) . . ? C231 N230 P23 127.8(3) . . ? N230 C231 C232 110.3(4) . . ? N230 C231 C234 111.9(4) . . ? C232 C231 C234 111.0(4) . . ? N230 C231 C233 106.0(4) . . ? C232 C231 C233 108.5(4) . . ? C234 C231 C233 108.9(4) . . ? C241 N240 P21 128.9(3) . . ? N240 C241 C242 112.8(4) . . ? N240 C241 C243 108.8(4) . . ? C242 C241 C243 110.2(4) . . ? N240 C241 C244 106.0(4) . . ? C242 C241 C244 109.6(4) . . ? C243 C241 C244 109.3(4) . . ? C251 N250 P22 127.5(3) . . ? C253 C251 N250 110.6(4) . . ? C253 C251 C254 113.5(4) . . ? N250 C251 C254 107.8(4) . . ? C253 C251 C252 109.9(4) . . ? N250 C251 C252 105.0(4) . . ? C254 C251 C252 109.7(4) . . ? C261 N260 P23 131.8(3) . . ? N260 C261 C263 107.1(4) . . ? N260 C261 C262 111.2(4) . . ? C263 C261 C262 109.2(4) . . ? N260 C261 C264 110.4(4) . . ? C263 C261 C264 109.1(4) . . ? C262 C261 C264 109.9(4) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.417 _refine_diff_density_min -0.347 _refine_diff_density_rms 0.057 #===END data_P3 _database_code_CSD 199622 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H48 N9 P3' _chemical_formula_weight 483.56 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 Rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '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' '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' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-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' '-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' _cell_length_a 36.840(10) _cell_length_b 36.840(10) _cell_length_c 10.799(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 12693(7) _cell_formula_units_Z 18 _cell_measurement_temperature 150(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 0.55 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.139 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4752 _exptl_absorpt_coefficient_mu 0.233 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19266 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0179 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 23.27 _reflns_number_total 4045 _reflns_number_gt 3539 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+57.2946P] 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 4045 _refine_ls_number_parameters 293 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.0563 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1320 _refine_ls_wR_factor_gt 0.1264 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 1.02833(2) 0.22826(2) 0.46644(7) 0.0257(2) Uani 1 1 d . . . P2 P 1.01934(2) 0.14821(2) 0.43347(6) 0.0228(2) Uani 1 1 d . . . P3 P 0.94926(2) 0.15717(2) 0.48218(7) 0.0279(2) Uani 1 1 d . . . N1 N 1.04711(7) 0.19822(7) 0.4415(2) 0.0286(6) Uani 1 1 d . . . N2 N 0.96977(7) 0.12948(7) 0.4439(2) 0.0246(5) Uani 1 1 d . . . N3 N 0.97857(7) 0.20658(7) 0.4688(2) 0.0302(6) Uani 1 1 d . . . N10 N 1.05236(8) 0.25427(8) 0.5939(3) 0.0341(6) Uani 1 1 d D . . H10 H 1.0542(10) 0.2395(9) 0.642(3) 0.030(9) Uiso 1 1 d D . . C11 C 1.04134(11) 0.28358(10) 0.6524(3) 0.0450(9) Uani 1 1 d . . . H11 H 1.0159 0.2805 0.6098 0.054 Uiso 1 1 calc R . . C12 C 1.03076(14) 0.27304(13) 0.7871(4) 0.0630(11) Uani 1 1 d . . . H12A H 1.0077 0.2441 0.7946 0.094 Uiso 1 1 calc R . . H12B H 1.0223 0.2921 0.8231 0.094 Uiso 1 1 calc R . . H12C H 1.0554 0.2761 0.8311 0.094 Uiso 1 1 calc R . . C13 C 1.07629(16) 0.32827(12) 0.6357(4) 0.0723(13) Uani 1 1 d . . . H13A H 1.0824 0.3341 0.5473 0.108 Uiso 1 1 calc R . . H13B H 1.1014 0.3323 0.6788 0.108 Uiso 1 1 calc R . . H13C H 1.0677 0.3474 0.6702 0.108 Uiso 1 1 calc R . . N20 N 1.03179(8) 0.12201(8) 0.5312(2) 0.0276(6) Uani 1 1 d D . . H20 H 1.0556(6) 0.1295(9) 0.531(3) 0.022(8) Uiso 1 1 d D . . C21 C 1.01187(9) 0.10794(9) 0.6527(3) 0.0306(7) Uani 1 1 d . . . H21 H 0.9816 0.0994 0.6439 0.037 Uiso 1 1 calc R . . C22 C 1.03126(12) 0.14280(13) 0.7483(3) 0.0558(10) Uani 1 1 d . . . H22A H 1.0291 0.1669 0.7194 0.084 Uiso 1 1 calc R . . H22B H 1.0608 0.1512 0.7599 0.084 Uiso 1 1 calc R . . H22C H 1.0163 0.1328 0.8271 0.084 Uiso 1 1 calc R . . C23 C 1.01426(12) 0.06988(13) 0.6907(4) 0.0587(11) Uani 1 1 d . . . H23A H 1.0014 0.0483 0.6266 0.088 Uiso 1 1 calc R . . H23B H 0.9993 0.0590 0.7691 0.088 Uiso 1 1 calc R . . H23C H 1.0437 0.0776 0.7012 0.088 Uiso 1 1 calc R . . N30 N 0.93440(9) 0.14498(9) 0.6296(3) 0.0417(7) Uani 1 1 d D . . H30 H 0.9232(11) 0.1206(7) 0.641(3) 0.047(11) Uiso 1 1 d D . . C31 C 0.92074(12) 0.16801(12) 0.7066(4) 0.0520(10) Uani 1 1 d . . . H31 H 0.9368 0.1982 0.6815 0.062 Uiso 1 1 calc R . . C32 C 0.87567(15) 0.15392(19) 0.6962(6) 0.0991(19) Uani 1 1 d . . . H32A H 0.8687 0.1556 0.6095 0.149 Uiso 1 1 calc R . . H32B H 0.8691 0.1719 0.7471 0.149 Uiso 1 1 calc R . . H32C H 0.8592 0.1249 0.7250 0.149 Uiso 1 1 calc R . . C33 C 0.93108(18) 0.16500(15) 0.8430(4) 0.0761(14) Uani 1 1 d . . . H33A H 0.9608 0.1734 0.8504 0.114 Uiso 1 1 calc R . . H33B H 0.9138 0.1361 0.8719 0.114 Uiso 1 1 calc R . . H33C H 0.9253 0.1836 0.8935 0.114 Uiso 1 1 calc R . . N40 N 1.04415(9) 0.26788(8) 0.3697(2) 0.0352(6) Uani 1 1 d D B . H40 H 1.0683(7) 0.2838(9) 0.368(3) 0.042(11) Uiso 1 1 d D . . C41 C 1.02197(11) 0.27051(11) 0.2619(3) 0.0460(9) Uani 1 1 d DU . . H41 H 0.9991 0.2410 0.2481 0.055 Uiso 1 1 calc R A 1 C42 C 1.0005(5) 0.2933(5) 0.2760(14) 0.087(5) Uiso 0.359(12) 1 d PDU B 1 H42A H 0.9839 0.2845 0.3523 0.130 Uiso 0.359(12) 1 calc PR B 1 H42B H 0.9818 0.2878 0.2050 0.130 Uiso 0.359(12) 1 calc PR B 1 H42C H 1.0208 0.3234 0.2803 0.130 Uiso 0.359(12) 1 calc PR B 1 C43 C 1.0520(5) 0.2797(6) 0.1506(11) 0.077(4) Uiso 0.359(12) 1 d PDU B 1 H43A H 1.0628 0.2602 0.1522 0.116 Uiso 0.359(12) 1 calc PR B 1 H43B H 1.0754 0.3086 0.1562 0.116 Uiso 0.359(12) 1 calc PR B 1 H43C H 1.0368 0.2761 0.0731 0.116 Uiso 0.359(12) 1 calc PR B 1 C42' C 1.0284(2) 0.3153(2) 0.2573(6) 0.058(2) Uiso 0.641(12) 1 d PDU B 2 H42D H 1.0219 0.3226 0.3383 0.087 Uiso 0.641(12) 1 calc PR B 2 H42E H 1.0099 0.3166 0.1945 0.087 Uiso 0.641(12) 1 calc PR B 2 H42F H 1.0576 0.3353 0.2360 0.087 Uiso 0.641(12) 1 calc PR B 2 C43' C 1.0328(3) 0.2595(3) 0.1418(6) 0.072(2) Uiso 0.641(12) 1 d PDU B 2 H43D H 1.0283 0.2310 0.1457 0.107 Uiso 0.641(12) 1 calc PR B 2 H43E H 1.0623 0.2792 0.1228 0.107 Uiso 0.641(12) 1 calc PR B 2 H43F H 1.0150 0.2611 0.0769 0.107 Uiso 0.641(12) 1 calc PR B 2 N50 N 1.03515(8) 0.13605(8) 0.3045(2) 0.0286(6) Uani 1 1 d D . . H50 H 1.0281(9) 0.1124(6) 0.299(3) 0.023(9) Uiso 1 1 d D . . C51 C 1.03812(10) 0.15543(10) 0.1840(3) 0.0343(7) Uani 1 1 d . . . H51 H 1.0551 0.1865 0.1948 0.041 Uiso 1 1 calc R . . C52 C 1.06146(12) 0.14247(13) 0.0959(3) 0.0496(9) Uani 1 1 d . . . H52A H 1.0888 0.1499 0.1314 0.074 Uiso 1 1 calc R . . H52B H 1.0656 0.1570 0.0167 0.074 Uiso 1 1 calc R . . H52C H 1.0452 0.1121 0.0824 0.074 Uiso 1 1 calc R . . C53 C 0.99592(12) 0.14505(16) 0.1307(3) 0.0644(12) Uani 1 1 d . . . H53A H 0.9814 0.1538 0.1891 0.097 Uiso 1 1 calc R . . H53B H 0.9790 0.1148 0.1166 0.097 Uiso 1 1 calc R . . H53C H 1.0001 0.1599 0.0521 0.097 Uiso 1 1 calc R . . N60 N 0.90655(9) 0.14450(9) 0.4050(3) 0.0457(8) Uani 1 1 d D D . H60 H 0.8868(9) 0.1236(9) 0.427(4) 0.055(12) Uiso 1 1 d D . . C61 C 0.90355(12) 0.16367(11) 0.2908(4) 0.0514(10) Uani 1 1 d D . . H61 H 0.9314 0.1873 0.2646 0.062 Uiso 1 1 calc R C 1 C62 C 0.88211(14) 0.13345(14) 0.1876(4) 0.0675(12) Uani 1 1 d D D . H62A H 0.8950 0.1159 0.1765 0.101 Uiso 1 1 calc R . . H62B H 0.8849 0.1489 0.1111 0.101 Uiso 1 1 calc R . . H62C H 0.8523 0.1156 0.2076 0.101 Uiso 1 1 calc R . . C63 C 0.8715(4) 0.1795(4) 0.3242(10) 0.0661(17) Uiso 0.415(11) 1 d PD D 1 H63A H 0.8830 0.1999 0.3920 0.099 Uiso 0.415(11) 1 calc PR D 1 H63B H 0.8447 0.1556 0.3497 0.099 Uiso 0.415(11) 1 calc PR D 1 H63C H 0.8673 0.1928 0.2513 0.099 Uiso 0.415(11) 1 calc PR D 1 C63' C 0.8935(3) 0.1972(3) 0.3046(8) 0.0661(17) Uiso 0.585(11) 1 d PD D 2 H63D H 0.9093 0.2151 0.3746 0.099 Uiso 0.585(11) 1 calc PR D 2 H63E H 0.8634 0.1849 0.3199 0.099 Uiso 0.585(11) 1 calc PR D 2 H63F H 0.9011 0.2140 0.2287 0.099 Uiso 0.585(11) 1 calc PR D 2 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 0.0251(4) 0.0219(4) 0.0285(4) 0.0024(3) 0.0011(3) 0.0106(3) P2 0.0219(4) 0.0240(4) 0.0226(4) -0.0001(3) 0.0006(3) 0.0116(3) P3 0.0225(4) 0.0238(4) 0.0379(5) 0.0019(3) 0.0025(3) 0.0118(3) N1 0.0211(12) 0.0266(13) 0.0352(14) 0.0006(11) 0.0017(10) 0.0098(11) N2 0.0240(13) 0.0226(12) 0.0258(13) -0.0022(10) -0.0010(10) 0.0106(10) N3 0.0288(14) 0.0267(13) 0.0386(15) 0.0028(11) 0.0025(11) 0.0165(11) N10 0.0407(16) 0.0286(14) 0.0343(16) -0.0013(12) -0.0043(12) 0.0183(13) C11 0.051(2) 0.040(2) 0.047(2) -0.0124(16) -0.0053(17) 0.0261(17) C12 0.068(3) 0.059(3) 0.055(3) -0.012(2) 0.014(2) 0.027(2) C13 0.103(4) 0.035(2) 0.068(3) -0.009(2) 0.012(3) 0.027(2) N20 0.0209(14) 0.0334(14) 0.0303(14) 0.0048(11) 0.0026(11) 0.0149(12) C21 0.0264(16) 0.0376(17) 0.0271(16) 0.0078(13) 0.0026(12) 0.0153(14) C22 0.047(2) 0.069(3) 0.0286(19) -0.0057(17) -0.0025(16) 0.012(2) C23 0.054(2) 0.065(3) 0.069(3) 0.038(2) 0.023(2) 0.039(2) N30 0.0506(18) 0.0276(16) 0.0453(17) 0.0024(13) 0.0165(14) 0.0183(14) C31 0.059(2) 0.045(2) 0.060(2) -0.0004(18) 0.0174(19) 0.0314(19) C32 0.062(3) 0.119(5) 0.117(4) -0.053(4) 0.000(3) 0.045(3) C33 0.119(4) 0.068(3) 0.052(3) 0.004(2) 0.020(3) 0.055(3) N40 0.0289(16) 0.0297(15) 0.0401(16) 0.0085(12) 0.0006(12) 0.0096(13) C41 0.048(2) 0.040(2) 0.044(2) 0.0120(16) -0.0046(16) 0.0179(17) N50 0.0337(14) 0.0278(15) 0.0268(14) 0.0004(11) 0.0020(11) 0.0174(12) C51 0.0353(17) 0.0443(19) 0.0248(16) 0.0018(13) 0.0002(13) 0.0210(15) C52 0.052(2) 0.077(3) 0.0283(18) -0.0014(17) 0.0054(16) 0.039(2) C53 0.052(2) 0.118(4) 0.035(2) 0.008(2) -0.0018(17) 0.052(3) N60 0.0280(16) 0.0361(17) 0.067(2) 0.0123(15) -0.0046(14) 0.0115(14) C61 0.051(2) 0.042(2) 0.064(2) 0.0109(18) -0.0139(19) 0.0257(18) C62 0.075(3) 0.065(3) 0.058(3) 0.010(2) -0.003(2) 0.032(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 N3 1.592(2) . ? P1 N1 1.594(2) . ? P1 N40 1.647(3) . ? P1 N10 1.657(3) . ? P2 N1 1.601(2) . ? P2 N2 1.601(2) . ? P2 N20 1.643(3) . ? P2 N50 1.656(3) . ? P3 N3 1.592(2) . ? P3 N2 1.598(2) . ? P3 N60 1.629(3) . ? P3 N30 1.670(3) . ? N10 C11 1.473(4) . ? C11 C12 1.505(5) . ? C11 C13 1.510(5) . ? N20 C21 1.466(4) . ? C21 C23 1.505(5) . ? C21 C22 1.519(5) . ? N30 C31 1.447(4) . ? C31 C32 1.476(6) . ? C31 C33 1.539(6) . ? N40 C41 1.453(4) . ? C41 C42 1.422(11) . ? C41 C43' 1.472(7) . ? C41 C42' 1.547(7) . ? C41 C43 1.553(11) . ? N50 C51 1.461(4) . ? C51 C52 1.511(4) . ? C51 C53 1.517(5) . ? N60 C61 1.453(5) . ? C61 C63' 1.462(7) . ? C61 C62 1.492(5) . ? C61 C63 1.597(10) . ? 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 116.40(12) . . ? N3 P1 N40 105.27(13) . . ? N1 P1 N40 115.08(14) . . ? N3 P1 N10 115.15(14) . . ? N1 P1 N10 104.47(13) . . ? N40 P1 N10 99.47(14) . . ? N1 P2 N2 115.28(12) . . ? N1 P2 N20 115.83(13) . . ? N2 P2 N20 107.16(12) . . ? N1 P2 N50 104.36(13) . . ? N2 P2 N50 114.99(13) . . ? N20 P2 N50 98.17(13) . . ? N3 P3 N2 116.07(12) . . ? N3 P3 N60 106.68(14) . . ? N2 P3 N60 112.47(15) . . ? N3 P3 N30 109.73(14) . . ? N2 P3 N30 105.72(13) . . ? N60 P3 N30 105.72(16) . . ? P1 N1 P2 123.95(15) . . ? P3 N2 P2 123.01(14) . . ? P3 N3 P1 121.85(15) . . ? C11 N10 P1 121.1(2) . . ? N10 C11 C12 110.9(3) . . ? N10 C11 C13 110.5(3) . . ? C12 C11 C13 111.5(3) . . ? C21 N20 P2 123.0(2) . . ? N20 C21 C23 108.7(3) . . ? N20 C21 C22 111.6(3) . . ? C23 C21 C22 112.4(3) . . ? C31 N30 P3 123.6(2) . . ? N30 C31 C32 114.2(3) . . ? N30 C31 C33 109.7(3) . . ? C32 C31 C33 108.9(4) . . ? C41 N40 P1 127.3(2) . . ? C42 C41 N40 116.9(7) . . ? C42 C41 C43' 124.3(7) . . ? N40 C41 C43' 116.7(4) . . ? C42 C41 C42' 37.5(7) . . ? N40 C41 C42' 107.8(4) . . ? C43' C41 C42' 110.3(5) . . ? C42 C41 C43 120.1(9) . . ? N40 C41 C43 105.7(6) . . ? C43' C41 C43 27.9(6) . . ? C42' C41 C43 91.7(7) . . ? C51 N50 P2 124.5(2) . . ? N50 C51 C52 108.8(3) . . ? N50 C51 C53 113.4(3) . . ? C52 C51 C53 110.8(3) . . ? C61 N60 P3 126.3(3) . . ? N60 C61 C63' 115.9(4) . . ? N60 C61 C62 114.3(3) . . ? C63' C61 C62 116.3(4) . . ? N60 C61 C63 103.6(5) . . ? C63' C61 C63 28.8(4) . . ? C62 C61 C63 103.2(5) . . ? 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 N20 H20 N2 0.775(19) 2.39(2) 3.155(3) 171(3) 11_666 N30 H30 N1 0.79(2) 2.87(3) 3.486(4) 137(3) 12_546 N60 H60 N1 0.79(2) 2.82(3) 3.537(4) 152(4) 12_546 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.781 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.056 #===END data_P4 _database_code_CSD 199623 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H48 N9 P3' _chemical_formula_weight 771.80 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 monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.627(3) _cell_length_b 24.689(3) _cell_length_c 15.391(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.950(10) _cell_angle_gamma 90.00 _cell_volume 4097.9(13) _cell_formula_units_Z 4 _cell_measurement_temperature 123(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 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 0.187 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart Apex CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16189 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0644 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 22.41 _reflns_number_total 8648 _reflns_number_gt 6019 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0444P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.65(9) _refine_ls_number_reflns 8648 _refine_ls_number_parameters 976 _refine_ls_number_restraints 3628 _refine_ls_R_factor_all 0.0594 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.0824 _refine_ls_wR_factor_gt 0.0769 _refine_ls_goodness_of_fit_ref 0.852 _refine_ls_restrained_S_all 0.952 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N11 N 0.4148(3) -0.01311(16) 0.6971(2) 0.0505(10) Uani 1 1 d . . . P11 P 0.55692(12) -0.01660(6) 0.70898(9) 0.0513(4) Uani 1 1 d . B . N12 N 0.3452(3) 0.02892(18) 0.5244(2) 0.0563(12) Uani 1 1 d . . . P12 P 0.30385(11) 0.01051(6) 0.60689(8) 0.0516(4) Uani 1 1 d . . . N13 N 0.5849(3) -0.00070(19) 0.6183(2) 0.0580(12) Uani 1 1 d . . . P13 P 0.47996(11) 0.02117(7) 0.52391(8) 0.0573(4) Uani 1 1 d . . . N21 N 0.0854(3) 0.04110(16) 0.7552(2) 0.0487(11) Uani 1 1 d . . . P21 P 0.19137(11) 0.01768(6) 0.84742(8) 0.0505(4) Uani 1 1 d . A . N22 N -0.0902(4) 0.03363(18) 0.8278(3) 0.0543(12) Uani 1 1 d . . . P22 P -0.05800(12) 0.04801(6) 0.73925(8) 0.0486(4) Uani 1 1 d . A . N23 N 0.1443(3) 0.00195(19) 0.9279(2) 0.0615(13) Uani 1 1 d . . . P23 P 0.0154(3) 0.01239(16) 0.9259(2) 0.0458(11) Uiso 0.543(8) 1 d PD A 1 P43 P -0.0071(4) -0.0005(2) 0.9135(3) 0.0549(15) Uiso 0.457(8) 1 d PD A 2 N110 N 0.6388(3) 0.0159(2) 0.8052(2) 0.0580(11) Uani 1 1 d D . . H110 H 0.707(2) 0.018(2) 0.808(3) 0.070 Uiso 1 1 d D . . C111 C 0.5962(5) 0.0648(2) 0.8368(3) 0.0563(14) Uani 1 1 d D . . H11A H 0.5074 0.0703 0.7980 0.068 Uiso 1 1 calc R . . H11B H 0.6426 0.0961 0.8263 0.068 Uiso 1 1 calc R . . C112 C 0.6116(4) 0.0638(2) 0.9377(3) 0.0465(14) Uani 1 1 d D . . C113 C 0.6258(5) 0.1119(2) 0.9868(4) 0.0716(17) Uani 1 1 d D . . H113 H 0.6301 0.1451 0.9568 0.086 Uiso 1 1 calc R . . C114 C 0.6338(7) 0.1126(3) 1.0786(5) 0.099(2) Uani 1 1 d D . . H114 H 0.6415 0.1461 1.1107 0.119 Uiso 1 1 calc R . . C115 C 0.6306(6) 0.0647(3) 1.1236(4) 0.089(2) Uani 1 1 d D . . H115 H 0.6383 0.0648 1.1873 0.106 Uiso 1 1 calc R . . C116 C 0.6162(5) 0.0172(3) 1.0755(4) 0.0693(16) Uani 1 1 d D . . H116 H 0.6123 -0.0160 1.1056 0.083 Uiso 1 1 calc R . . C117 C 0.6072(4) 0.0167(2) 0.9834(3) 0.0527(13) Uani 1 1 d D . . H117 H 0.5978 -0.0169 0.9513 0.063 Uiso 1 1 calc R . . N120 N 0.2286(4) 0.06200(18) 0.6253(3) 0.0541(11) Uani 1 1 d D . . H120 H 0.184(4) 0.055(2) 0.651(3) 0.065 Uiso 1 1 d D . . C121 C 0.2794(5) 0.1166(2) 0.6359(4) 0.0607(14) Uani 1 1 d D . . H12A H 0.3244 0.1210 0.5930 0.073 Uiso 1 1 calc R . . H12B H 0.3403 0.1210 0.7007 0.073 Uiso 1 1 calc R . . C122 C 0.1841(5) 0.1608(2) 0.6163(3) 0.0550(13) Uani 1 1 d D . . C123 C 0.2203(6) 0.2107(3) 0.6563(4) 0.094(2) Uani 1 1 d D . . H123 H 0.3040 0.2157 0.6975 0.113 Uiso 1 1 calc R . . C124 C 0.1406(9) 0.2533(3) 0.6391(6) 0.128(3) Uani 1 1 d D . . H124 H 0.1695 0.2876 0.6663 0.154 Uiso 1 1 calc R . . C125 C 0.0198(8) 0.2466(3) 0.5832(5) 0.107(3) Uani 1 1 d D . . H125 H -0.0357 0.2764 0.5705 0.129 Uiso 1 1 calc R . . C126 C -0.0225(6) 0.1968(3) 0.5449(4) 0.096(2) Uani 1 1 d D . . H126 H -0.1075 0.1916 0.5071 0.116 Uiso 1 1 calc R . . C127 C 0.0612(5) 0.1541(2) 0.5621(4) 0.0740(16) Uani 1 1 d D . . H127 H 0.0325 0.1196 0.5356 0.089 Uiso 1 1 calc R . . N130 N 0.5406(4) 0.0763(2) 0.5001(3) 0.0742(14) Uani 1 1 d D . . H130 H 0.584(5) 0.092(2) 0.544(3) 0.089 Uiso 1 1 d D . . C131 C 0.4656(6) 0.1143(3) 0.4288(5) 0.099(2) Uani 1 1 d D . . H13A H 0.4222 0.1391 0.4570 0.119 Uiso 1 1 calc R . . H13B H 0.4020 0.0940 0.3780 0.119 Uiso 1 1 calc R . . C132 C 0.5415(6) 0.1473(2) 0.3877(4) 0.0727(16) Uani 1 1 d D . . C133 C 0.6445(6) 0.1279(3) 0.3766(4) 0.094(2) Uani 1 1 d D . . H133 H 0.6735 0.0927 0.3992 0.113 Uiso 1 1 calc R . . C134 C 0.7081(7) 0.1579(3) 0.3333(5) 0.106(2) Uani 1 1 d D . . H134 H 0.7777 0.1427 0.3240 0.127 Uiso 1 1 calc R . . C135 C 0.6710(9) 0.2088(4) 0.3042(5) 0.114(3) Uani 1 1 d D . . H135 H 0.7167 0.2305 0.2776 0.137 Uiso 1 1 calc R . . C136 C 0.5684(10) 0.2281(3) 0.3135(6) 0.130(3) Uani 1 1 d D . . H136 H 0.5395 0.2631 0.2899 0.156 Uiso 1 1 calc R . . C137 C 0.5027(7) 0.1984(3) 0.3569(5) 0.100(2) Uani 1 1 d D . . H137 H 0.4321 0.2135 0.3648 0.120 Uiso 1 1 calc R . . N140 N 0.6180(5) -0.0775(2) 0.7379(3) 0.0777(14) Uani 1 1 d D . . H140 H 0.628(6) -0.084(3) 0.790(2) 0.093 Uiso 1 1 d D . . C141 C 0.5742(9) -0.1175(4) 0.6538(9) 0.077(4) Uiso 0.590(17) 1 d PD B 1 H14A H 0.5087 -0.1407 0.6607 0.092 Uiso 0.590(17) 1 calc PR B 1 H14B H 0.5350 -0.0959 0.5960 0.092 Uiso 0.590(17) 1 calc PR B 1 C142 C 0.6656(9) -0.1530(4) 0.6393(9) 0.071(3) Uiso 0.590(17) 1 d PD B 1 C143 C 0.6414(12) -0.1767(5) 0.5544(9) 0.088(4) Uiso 0.590(17) 1 d PD B 1 H143 H 0.5638 -0.1696 0.5055 0.106 Uiso 0.590(17) 1 calc PR B 1 C144 C 0.7220(11) -0.2094(5) 0.5366(9) 0.099(4) Uiso 0.590(17) 1 d PD B 1 H144 H 0.7016 -0.2258 0.4769 0.118 Uiso 0.590(17) 1 calc PR B 1 C145 C 0.8355(12) -0.2186(6) 0.6076(9) 0.101(5) Uiso 0.590(17) 1 d PD B 1 H145 H 0.8964 -0.2388 0.5941 0.122 Uiso 0.590(17) 1 calc PR B 1 C146 C 0.8628(17) -0.2000(9) 0.6953(13) 0.158(9) Uiso 0.590(17) 1 d PD B 1 H146 H 0.9374 -0.2101 0.7449 0.189 Uiso 0.590(17) 1 calc PR B 1 C147 C 0.7752(11) -0.1646(5) 0.7109(10) 0.092(4) Uiso 0.590(17) 1 d PD B 1 H147 H 0.7931 -0.1490 0.7710 0.110 Uiso 0.590(17) 1 calc PR B 1 C341 C 0.5832(12) -0.1261(5) 0.6940(13) 0.068(5) Uiso 0.410(17) 1 d PD B 2 H34A H 0.5193 -0.1201 0.6308 0.081 Uiso 0.410(17) 1 calc PR B 2 H34B H 0.5462 -0.1487 0.7299 0.081 Uiso 0.410(17) 1 calc PR B 2 C342 C 0.6927(14) -0.1557(6) 0.6853(14) 0.074(5) Uiso 0.410(17) 1 d PD B 2 C343 C 0.684(2) -0.1760(11) 0.5999(16) 0.148(10) Uiso 0.410(17) 1 d PD B 2 H343 H 0.6112 -0.1687 0.5465 0.178 Uiso 0.410(17) 1 calc PR B 2 C344 C 0.780(3) -0.2072(15) 0.589(2) 0.205(15) Uiso 0.410(17) 1 d PD B 2 H344 H 0.7744 -0.2244 0.5321 0.245 Uiso 0.410(17) 1 calc PR B 2 C345 C 0.879(2) -0.2092(12) 0.669(2) 0.136(11) Uiso 0.410(17) 1 d PD B 2 H345 H 0.9530 -0.2204 0.6625 0.163 Uiso 0.410(17) 1 calc PR B 2 C346 C 0.892(3) -0.1982(16) 0.759(2) 0.247(19) Uiso 0.410(17) 1 d PD B 2 H346 H 0.9609 -0.2100 0.8120 0.296 Uiso 0.410(17) 1 calc PR B 2 C347 C 0.7916(16) -0.1669(8) 0.7663(16) 0.121(8) Uiso 0.410(17) 1 d PD B 2 H347 H 0.7937 -0.1544 0.8253 0.145 Uiso 0.410(17) 1 calc PR B 2 N150 N 0.1927(4) -0.0354(2) 0.5813(3) 0.0622(12) Uani 1 1 d D . . H150 H 0.130(3) -0.025(2) 0.546(3) 0.075 Uiso 1 1 d D . . C151 C 0.2136(5) -0.0936(2) 0.5814(4) 0.0682(17) Uani 1 1 d D . . H15A H 0.1424 -0.1121 0.5889 0.082 Uiso 1 1 calc R . . H15B H 0.2883 -0.1024 0.6371 0.082 Uiso 1 1 calc R . . C152 C 0.2303(5) -0.1167(3) 0.4970(4) 0.0692(18) Uani 1 1 d D . . C153 C 0.2796(7) -0.1687(3) 0.5044(6) 0.113(3) Uani 1 1 d D . . H153 H 0.3033 -0.1881 0.5617 0.136 Uiso 1 1 calc R . . C154 C 0.2935(8) -0.1917(4) 0.4264(8) 0.154(5) Uani 1 1 d D . . H154 H 0.3256 -0.2274 0.4311 0.185 Uiso 1 1 calc R . . C155 C 0.2632(8) -0.1651(5) 0.3445(7) 0.135(4) Uani 1 1 d D . . H155 H 0.2761 -0.1815 0.2931 0.162 Uiso 1 1 calc R . . C156 C 0.2137(8) -0.1141(4) 0.3360(5) 0.119(3) Uani 1 1 d D . . H156 H 0.1907 -0.0950 0.2784 0.143 Uiso 1 1 calc R . . C157 C 0.1974(6) -0.0907(3) 0.4131(5) 0.082(2) Uani 1 1 d D . . H157 H 0.1622 -0.0555 0.4070 0.098 Uiso 1 1 calc R . . N160 N 0.4570(4) -0.0158(2) 0.4299(3) 0.0712(14) Uani 1 1 d D . . H160 H 0.419(5) -0.0429(15) 0.421(4) 0.085 Uiso 1 1 d D . . C161 C 0.5536(5) -0.0355(3) 0.4005(3) 0.080(2) Uani 1 1 d D . . H16A H 0.5980 -0.0657 0.4418 0.096 Uiso 1 1 calc R . . H16B H 0.6140 -0.0061 0.4064 0.096 Uiso 1 1 calc R . . C162 C 0.5004(5) -0.0551(2) 0.2998(3) 0.0603(15) Uani 1 1 d D . . C163 C 0.5392(6) -0.1028(3) 0.2752(4) 0.0786(19) Uani 1 1 d D . . H163 H 0.5992 -0.1245 0.3209 0.094 Uiso 1 1 calc R . . C164 C 0.4894(9) -0.1191(3) 0.1814(6) 0.114(3) Uani 1 1 d D . . H164 H 0.5169 -0.1519 0.1631 0.137 Uiso 1 1 calc R . . C165 C 0.4022(8) -0.0886(4) 0.1165(5) 0.121(4) Uani 1 1 d D . . H165 H 0.3684 -0.1004 0.0532 0.145 Uiso 1 1 calc R . . C166 C 0.3630(7) -0.0418(4) 0.1406(4) 0.108(3) Uani 1 1 d D . . H166 H 0.3022 -0.0205 0.0947 0.130 Uiso 1 1 calc R . . C167 C 0.4114(5) -0.0251(3) 0.2319(4) 0.0825(19) Uani 1 1 d D . . H167 H 0.3832 0.0078 0.2489 0.099 Uiso 1 1 calc R . . N210 N 0.3043(4) 0.06229(19) 0.8757(3) 0.0618(12) Uani 1 1 d D . . H210 H 0.360(4) 0.047(2) 0.912(3) 0.074 Uiso 1 1 d D . . C211 C 0.2860(5) 0.1205(2) 0.8776(3) 0.0601(14) Uani 1 1 d D A . H21A H 0.2106 0.1300 0.8229 0.072 Uiso 1 1 calc R . . H21B H 0.3570 0.1386 0.8691 0.072 Uiso 1 1 calc R . . C212 C 0.2726(5) 0.1439(2) 0.9644(4) 0.0593(16) Uani 1 1 d D . . C213 C 0.2226(6) 0.1945(3) 0.9589(4) 0.088(2) Uani 1 1 d D A . H213 H 0.1955 0.2133 0.9008 0.106 Uiso 1 1 calc R . . C214 C 0.2104(7) 0.2191(3) 1.0358(6) 0.110(3) Uani 1 1 d D . . H214 H 0.1748 0.2542 1.0306 0.132 Uiso 1 1 calc R A . C215 C 0.2505(8) 0.1920(4) 1.1197(6) 0.120(3) Uani 1 1 d D A . H215 H 0.2433 0.2083 1.1734 0.144 Uiso 1 1 calc R . . C216 C 0.3003(8) 0.1421(4) 1.1255(5) 0.110(3) Uani 1 1 d D . . H216 H 0.3273 0.1233 1.1836 0.132 Uiso 1 1 calc R A . C217 C 0.3130(6) 0.1175(3) 1.0481(4) 0.086(2) Uani 1 1 d D A . H217 H 0.3495 0.0826 1.0537 0.104 Uiso 1 1 calc R . . N220 N -0.1132(4) 0.1101(2) 0.7083(3) 0.0672(13) Uani 1 1 d D . . H220 H -0.107(5) 0.119(2) 0.662(2) 0.081 Uiso 1 1 d D . . C221 C -0.0893(13) 0.1515(6) 0.7874(11) 0.106(7) Uiso 0.585(17) 1 d PD A 1 H22A H -0.0225 0.1767 0.7887 0.127 Uiso 0.585(17) 1 calc PR A 1 H22B H -0.0632 0.1327 0.8486 0.127 Uiso 0.585(17) 1 calc PR A 1 C222 C -0.2111(12) 0.1831(4) 0.7690(8) 0.063(4) Uiso 0.585(17) 1 d PD A 1 C223 C -0.2047(12) 0.2150(4) 0.8448(8) 0.078(4) Uiso 0.585(17) 1 d PD A 1 H223 H -0.1278 0.2173 0.8964 0.094 Uiso 0.585(17) 1 calc PR A 1 C224 C -0.3057(14) 0.2440(5) 0.8488(9) 0.082(4) Uiso 0.585(17) 1 d PD A 1 H224 H -0.3027 0.2653 0.9010 0.099 Uiso 0.585(17) 1 calc PR A 1 C225 C -0.4110(13) 0.2382(5) 0.7679(10) 0.102(5) Uiso 0.585(17) 1 d PD A 1 H225 H -0.4842 0.2556 0.7672 0.122 Uiso 0.585(17) 1 calc PR A 1 C226 C -0.4200(10) 0.2100(5) 0.6889(11) 0.095(4) Uiso 0.585(17) 1 d PD A 1 H226 H -0.4942 0.2103 0.6347 0.113 Uiso 0.585(17) 1 calc PR A 1 C227 C -0.3152(8) 0.1806(4) 0.6911(9) 0.061(3) Uiso 0.585(17) 1 d PD A 1 H227 H -0.3177 0.1595 0.6388 0.073 Uiso 0.585(17) 1 calc PR A 1 C421 C -0.0764(10) 0.1542(6) 0.7695(11) 0.043(5) Uiso 0.415(17) 1 d PD A 2 H42A H -0.0103 0.1419 0.8281 0.051 Uiso 0.415(17) 1 calc PR A 2 H42B H -0.0395 0.1818 0.7410 0.051 Uiso 0.415(17) 1 calc PR A 2 C422 C -0.1755(12) 0.1813(5) 0.7947(10) 0.046(4) Uiso 0.415(17) 1 d PD A 2 C423 C -0.1497(17) 0.2070(7) 0.8783(11) 0.089(6) Uiso 0.415(17) 1 d PD A 2 H423 H -0.0694 0.2057 0.9264 0.107 Uiso 0.415(17) 1 calc PR A 2 C424 C -0.2471(16) 0.2352(7) 0.8898(13) 0.097(6) Uiso 0.415(17) 1 d PD A 2 H424 H -0.2321 0.2541 0.9467 0.116 Uiso 0.415(17) 1 calc PR A 2 C425 C -0.3636(16) 0.2364(6) 0.8214(13) 0.072(6) Uiso 0.415(17) 1 d PD A 2 H425 H -0.4246 0.2579 0.8324 0.086 Uiso 0.415(17) 1 calc PR A 2 C426 C -0.3978(12) 0.2092(6) 0.7395(12) 0.074(5) Uiso 0.415(17) 1 d PD A 2 H426 H -0.4789 0.2096 0.6924 0.089 Uiso 0.415(17) 1 calc PR A 2 C427 C -0.2965(10) 0.1802(5) 0.7334(11) 0.048(4) Uiso 0.415(17) 1 d PD A 2 H427 H -0.3143 0.1572 0.6805 0.058 Uiso 0.415(17) 1 calc PR A 2 N230 N 0.0422(7) 0.0466(4) 1.0208(4) 0.053(2) Uiso 0.543(8) 1 d PD A 1 H230 H 0.1191 0.0548 1.0564 0.064 Uiso 0.543(8) 1 calc PR A 1 C231 C -0.0615(8) 0.0644(4) 1.0493(5) 0.054(3) Uiso 0.543(8) 1 d PD A 1 H23A H -0.1223 0.0347 1.0399 0.064 Uiso 0.543(8) 1 calc PR A 1 H23B H -0.1048 0.0960 1.0116 0.064 Uiso 0.543(8) 1 calc PR A 1 C232 C -0.0041(13) 0.0794(6) 1.1514(7) 0.072(6) Uiso 0.543(8) 1 d PD A 1 C233 C -0.0192(18) 0.1291(6) 1.1828(10) 0.106(7) Uiso 0.543(8) 1 d PD A 1 H233 H -0.0616 0.1565 1.1392 0.128 Uiso 0.543(8) 1 calc PR A 1 C234 C 0.0277(15) 0.1407(6) 1.2802(10) 0.095(4) Uiso 0.543(8) 1 d PD A 1 H234 H 0.0054 0.1726 1.3048 0.114 Uiso 0.543(8) 1 calc PR A 1 C235 C 0.1070(12) 0.1030(5) 1.3363(8) 0.074(3) Uiso 0.543(8) 1 d PD A 1 H235 H 0.1423 0.1100 1.4017 0.088 Uiso 0.543(8) 1 calc PR A 1 C236 C 0.1382(12) 0.0566(6) 1.3045(7) 0.082(4) Uiso 0.543(8) 1 d PD A 1 H236 H 0.1905 0.0310 1.3472 0.098 Uiso 0.543(8) 1 calc PR A 1 C237 C 0.0933(14) 0.0466(6) 1.2087(8) 0.080(5) Uiso 0.543(8) 1 d PD A 1 H237 H 0.1272 0.0186 1.1830 0.096 Uiso 0.543(8) 1 calc PR A 1 N430 N -0.0235(11) 0.0220(5) 1.0099(6) 0.081(4) Uiso 0.457(8) 1 d PD A 2 H430 H -0.0436 -0.0011 1.0454 0.098 Uiso 0.457(8) 1 calc PR A 2 C431 C -0.0056(15) 0.0788(5) 1.0377(7) 0.074(4) Uiso 0.457(8) 1 d PD A 2 H43A H -0.0783 0.0996 0.9965 0.089 Uiso 0.457(8) 1 calc PR A 2 H43B H 0.0680 0.0925 1.0271 0.089 Uiso 0.457(8) 1 calc PR A 2 C432 C 0.0117(16) 0.0900(6) 1.1396(8) 0.070(6) Uiso 0.457(8) 1 d PD A 2 C433 C -0.043(2) 0.1357(7) 1.1594(12) 0.094(7) Uiso 0.457(8) 1 d PD A 2 H433 H -0.1094 0.1517 1.1095 0.113 Uiso 0.457(8) 1 calc PR A 2 C434 C -0.0068(16) 0.1602(7) 1.2468(10) 0.105(6) Uiso 0.457(8) 1 d PD A 2 H434 H -0.0355 0.1951 1.2548 0.127 Uiso 0.457(8) 1 calc PR A 2 C435 C 0.0716(16) 0.1313(7) 1.3200(10) 0.085(5) Uiso 0.457(8) 1 d PD A 2 H435 H 0.0968 0.1462 1.3813 0.102 Uiso 0.457(8) 1 calc PR A 2 C436 C 0.1152(15) 0.0817(7) 1.3088(10) 0.082(5) Uiso 0.457(8) 1 d PD A 2 H436 H 0.1735 0.0632 1.3607 0.098 Uiso 0.457(8) 1 calc PR A 2 C437 C 0.0718(17) 0.0583(7) 1.2178(9) 0.080(6) Uiso 0.457(8) 1 d PD A 2 H437 H 0.0840 0.0207 1.2107 0.096 Uiso 0.457(8) 1 calc PR A 2 N240 N 0.2669(4) -0.03555(18) 0.8316(3) 0.0565(12) Uani 1 1 d D . . H240 H 0.306(4) -0.029(2) 0.801(3) 0.068 Uiso 1 1 d D . . C241 C 0.2100(5) -0.0887(2) 0.8201(4) 0.0618(14) Uani 1 1 d D A . H24A H 0.1628 -0.0951 0.7525 0.074 Uiso 1 1 calc R . . H24B H 0.1501 -0.0891 0.8519 0.074 Uiso 1 1 calc R . . C242 C 0.3004(5) -0.1343(2) 0.8579(3) 0.0582(14) Uani 1 1 d D . . C243 C 0.2607(6) -0.1818(3) 0.8845(4) 0.0840(18) Uani 1 1 d D A . H243 H 0.1773 -0.1846 0.8803 0.101 Uiso 1 1 calc R . . C244 C 0.3392(9) -0.2252(3) 0.9170(5) 0.110(2) Uani 1 1 d D . . H244 H 0.3095 -0.2576 0.9342 0.132 Uiso 1 1 calc R A . C245 C 0.4591(8) -0.2218(3) 0.9246(4) 0.104(2) Uani 1 1 d D A . H245 H 0.5136 -0.2516 0.9476 0.124 Uiso 1 1 calc R . . C246 C 0.5006(6) -0.1751(3) 0.8988(5) 0.100(2) Uani 1 1 d D . . H246 H 0.5844 -0.1723 0.9039 0.120 Uiso 1 1 calc R A . C247 C 0.4202(6) -0.1317(2) 0.8649(4) 0.0819(18) Uani 1 1 d D A . H247 H 0.4496 -0.0995 0.8463 0.098 Uiso 1 1 calc R . . N250 N -0.1401(3) 0.0159(2) 0.6428(3) 0.0607(12) Uani 1 1 d D . . H250 H -0.211(2) 0.017(2) 0.630(3) 0.073 Uiso 1 1 d D . . C251 C -0.1028(5) -0.0350(2) 0.6136(3) 0.0616(17) Uani 1 1 d D A . H25A H -0.1541 -0.0646 0.6234 0.074 Uiso 1 1 calc R . . H25B H -0.0154 -0.0425 0.6537 0.074 Uiso 1 1 calc R . . C252 C -0.1153(4) -0.0352(2) 0.5123(3) 0.0482(13) Uani 1 1 d D . . C253 C -0.1183(5) -0.0841(3) 0.4672(4) 0.0648(17) Uani 1 1 d D A . H253 H -0.1173 -0.1174 0.4986 0.078 Uiso 1 1 calc R . . C254 C -0.1229(6) -0.0842(3) 0.3761(4) 0.083(2) Uani 1 1 d D . . H254 H -0.1240 -0.1178 0.3457 0.100 Uiso 1 1 calc R A . C255 C -0.1259(6) -0.0370(3) 0.3288(4) 0.0862(19) Uani 1 1 d D A . H255 H -0.1291 -0.0380 0.2663 0.103 Uiso 1 1 calc R . . C256 C -0.1243(5) 0.0115(3) 0.3720(4) 0.0737(16) Uani 1 1 d D . . H256 H -0.1276 0.0446 0.3396 0.088 Uiso 1 1 calc R A . C257 C -0.1176(5) 0.0115(3) 0.4634(4) 0.0580(15) Uani 1 1 d D A . H257 H -0.1145 0.0453 0.4937 0.070 Uiso 1 1 calc R . . N260 N -0.0477(7) -0.0445(3) 0.9472(6) 0.056(2) Uiso 0.543(8) 1 d PD A 1 H260 H -0.1256 -0.0519 0.9129 0.067 Uiso 0.543(8) 1 calc PR A 1 C261 C 0.0220(8) -0.0819(4) 1.0201(7) 0.060(3) Uiso 0.543(8) 1 d PD A 1 H26A H 0.0876 -0.0616 1.0696 0.072 Uiso 0.543(8) 1 calc PR A 1 H26B H 0.0633 -0.1086 0.9934 0.072 Uiso 0.543(8) 1 calc PR A 1 C262 C -0.0546(10) -0.1122(5) 1.0645(9) 0.067(4) Uiso 0.543(8) 1 d PD A 1 C263 C -0.1711(10) -0.0946(5) 1.0525(9) 0.073(4) Uiso 0.543(8) 1 d PD A 1 H263 H -0.1960 -0.0602 1.0237 0.087 Uiso 0.543(8) 1 calc PR A 1 C264 C -0.2558(12) -0.1229(5) 1.0790(9) 0.064(4) Uiso 0.543(8) 1 d PD A 1 H264 H -0.3427 -0.1170 1.0520 0.077 Uiso 0.543(8) 1 calc PR A 1 C265 C -0.2032(11) -0.1591(6) 1.1459(9) 0.073(4) Uiso 0.543(8) 1 d PD A 1 H265 H -0.2473 -0.1716 1.1830 0.088 Uiso 0.543(8) 1 calc PR A 1 C266 C -0.0859(13) -0.1790(6) 1.1629(10) 0.078(5) Uiso 0.543(8) 1 d PD A 1 H266 H -0.0566 -0.2089 1.2041 0.094 Uiso 0.543(8) 1 calc PR A 1 C267 C -0.0095(13) -0.1563(6) 1.1213(11) 0.078(6) Uiso 0.543(8) 1 d PD A 1 H267 H 0.0702 -0.1708 1.1317 0.094 Uiso 0.543(8) 1 calc PR A 1 N460 N -0.0630(9) -0.0615(4) 0.9040(8) 0.066(3) Uiso 0.457(8) 1 d PD A 2 H460 H -0.1321 -0.0690 0.8566 0.079 Uiso 0.457(8) 1 calc PR A 2 C461 C -0.0046(11) -0.1033(5) 0.9695(9) 0.071(4) Uiso 0.457(8) 1 d PD A 2 H46A H 0.0804 -0.0912 1.0081 0.086 Uiso 0.457(8) 1 calc PR A 2 H46B H 0.0032 -0.1356 0.9340 0.086 Uiso 0.457(8) 1 calc PR A 2 C462 C -0.0675(10) -0.1200(5) 1.0340(9) 0.050(4) Uiso 0.457(8) 1 d PD A 2 C463 C -0.1889(11) -0.1073(6) 1.0207(9) 0.067(4) Uiso 0.457(8) 1 d PD A 2 H463 H -0.2437 -0.0888 0.9671 0.080 Uiso 0.457(8) 1 calc PR A 2 C464 C -0.2244(18) -0.1255(8) 1.0983(12) 0.099(8) Uiso 0.457(8) 1 d PD A 2 H464 H -0.2849 -0.1059 1.1133 0.118 Uiso 0.457(8) 1 calc PR A 2 C465 C -0.1703(17) -0.1706(7) 1.1493(12) 0.092(6) Uiso 0.457(8) 1 d PD A 2 H465 H -0.2136 -0.1919 1.1785 0.110 Uiso 0.457(8) 1 calc PR A 2 C466 C -0.0535(17) -0.1844(8) 1.1571(13) 0.100(8) Uiso 0.457(8) 1 d PD A 2 H466 H -0.0077 -0.2116 1.1998 0.120 Uiso 0.457(8) 1 calc PR A 2 C467 C -0.0048(14) -0.1576(6) 1.1009(12) 0.069(6) Uiso 0.457(8) 1 d PD A 2 H467 H 0.0785 -0.1655 1.1087 0.083 Uiso 0.457(8) 1 calc PR A 2 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 N11 0.032(2) 0.058(3) 0.064(3) 0.007(2) 0.0209(17) 0.001(2) P11 0.0350(8) 0.0587(10) 0.0604(9) -0.0010(7) 0.0182(6) 0.0029(7) N12 0.036(2) 0.076(3) 0.057(2) -0.003(2) 0.0182(17) 0.005(2) P12 0.0336(7) 0.0614(10) 0.0605(8) -0.0037(7) 0.0187(6) 0.0028(8) N13 0.034(2) 0.086(4) 0.057(2) -0.008(2) 0.0196(18) 0.004(2) P13 0.0378(7) 0.0858(12) 0.0513(7) -0.0089(7) 0.0201(5) 0.0018(8) N21 0.040(2) 0.062(3) 0.046(2) 0.0000(19) 0.0184(16) 0.003(2) P21 0.0357(7) 0.0575(9) 0.0553(8) 0.0032(7) 0.0136(5) -0.0002(7) N22 0.043(2) 0.071(4) 0.053(2) 0.003(2) 0.0237(19) 0.010(2) P22 0.0368(8) 0.0598(10) 0.0528(8) 0.0031(6) 0.0210(6) 0.0061(7) N23 0.047(3) 0.082(4) 0.047(2) 0.010(2) 0.0076(18) 0.002(2) N110 0.033(2) 0.091(4) 0.051(2) 0.001(2) 0.0164(19) 0.001(3) C111 0.047(3) 0.066(4) 0.055(3) 0.007(3) 0.019(3) -0.001(3) C112 0.034(3) 0.051(4) 0.051(3) 0.004(3) 0.012(2) -0.004(3) C113 0.074(4) 0.058(4) 0.066(4) 0.001(3) 0.007(3) -0.013(3) C114 0.128(6) 0.077(6) 0.075(5) -0.015(4) 0.018(4) -0.012(5) C115 0.109(5) 0.099(6) 0.051(4) -0.008(4) 0.024(3) -0.010(5) C116 0.072(4) 0.071(5) 0.062(4) 0.010(4) 0.022(3) 0.007(4) C117 0.049(3) 0.060(4) 0.043(3) -0.010(3) 0.009(2) -0.004(3) N120 0.037(3) 0.057(3) 0.075(3) 0.000(2) 0.029(2) 0.002(2) C121 0.050(3) 0.063(4) 0.074(4) 0.000(3) 0.029(3) 0.001(3) C122 0.062(4) 0.050(4) 0.054(3) 0.000(2) 0.023(3) 0.008(3) C123 0.103(5) 0.075(5) 0.084(5) -0.002(4) 0.013(4) 0.011(4) C124 0.165(9) 0.071(6) 0.125(7) -0.008(4) 0.028(6) 0.040(6) C125 0.123(7) 0.085(6) 0.115(6) 0.021(5) 0.046(5) 0.056(5) C126 0.075(5) 0.114(7) 0.099(5) 0.025(4) 0.030(4) 0.035(5) C127 0.064(4) 0.076(5) 0.079(4) 0.002(3) 0.024(3) 0.014(4) N130 0.058(3) 0.093(4) 0.072(3) 0.002(3) 0.023(2) -0.012(3) C131 0.077(5) 0.104(6) 0.123(5) 0.023(4) 0.046(4) 0.018(4) C132 0.073(4) 0.064(4) 0.076(4) -0.003(3) 0.023(3) 0.006(3) C133 0.103(5) 0.068(5) 0.135(6) 0.016(4) 0.069(5) -0.002(4) C134 0.127(6) 0.096(6) 0.112(5) -0.012(4) 0.066(5) -0.022(5) C135 0.154(9) 0.093(7) 0.089(5) 0.005(5) 0.038(5) -0.049(6) C136 0.181(10) 0.070(6) 0.106(6) 0.012(4) 0.016(6) -0.004(7) C137 0.126(6) 0.070(5) 0.094(5) 0.000(4) 0.030(4) 0.011(5) N140 0.061(3) 0.068(4) 0.103(4) 0.001(3) 0.029(3) 0.009(3) N150 0.034(3) 0.066(4) 0.083(4) -0.010(2) 0.018(2) -0.001(2) C151 0.050(4) 0.064(5) 0.088(5) -0.008(3) 0.023(3) -0.007(3) C152 0.040(3) 0.072(5) 0.090(5) -0.026(4) 0.017(3) -0.010(3) C153 0.072(5) 0.100(7) 0.137(7) -0.043(5) 0.005(4) 0.018(5) C154 0.094(6) 0.162(10) 0.170(9) -0.091(9) 0.008(6) 0.022(6) C155 0.081(6) 0.191(12) 0.132(8) -0.100(8) 0.040(6) -0.024(7) C156 0.097(6) 0.150(9) 0.107(6) -0.060(6) 0.035(5) -0.040(6) C157 0.066(4) 0.092(5) 0.087(5) -0.028(4) 0.027(4) -0.017(4) N160 0.044(3) 0.114(5) 0.058(3) -0.024(3) 0.022(2) -0.001(3) C161 0.041(3) 0.133(6) 0.058(3) -0.012(3) 0.010(2) 0.019(3) C162 0.055(3) 0.079(4) 0.053(3) -0.017(3) 0.027(3) -0.009(3) C163 0.073(4) 0.087(5) 0.088(4) -0.016(4) 0.043(3) -0.011(4) C164 0.143(8) 0.113(7) 0.126(7) -0.064(6) 0.096(6) -0.051(6) C165 0.108(7) 0.195(11) 0.070(5) -0.044(6) 0.046(5) -0.069(7) C166 0.086(5) 0.171(9) 0.058(5) 0.019(4) 0.015(4) -0.025(6) C167 0.073(4) 0.107(5) 0.052(4) 0.004(3) 0.005(3) 0.005(4) N210 0.044(3) 0.059(4) 0.070(3) 0.004(2) 0.008(2) 0.004(2) C211 0.044(3) 0.059(4) 0.071(4) 0.005(3) 0.015(3) -0.010(3) C212 0.043(3) 0.062(5) 0.062(4) -0.005(3) 0.007(3) -0.012(3) C213 0.083(5) 0.087(6) 0.081(5) -0.012(4) 0.016(3) 0.005(4) C214 0.103(6) 0.108(7) 0.106(6) -0.038(5) 0.024(5) 0.011(5) C215 0.096(6) 0.158(10) 0.108(7) -0.055(7) 0.040(5) -0.028(6) C216 0.125(7) 0.126(8) 0.069(5) -0.012(5) 0.025(4) -0.025(6) C217 0.075(5) 0.092(6) 0.077(5) -0.006(4) 0.011(3) -0.006(4) N220 0.060(3) 0.075(4) 0.074(3) 0.014(3) 0.033(3) 0.022(3) N240 0.044(3) 0.050(3) 0.080(3) 0.010(2) 0.028(2) 0.000(2) C241 0.048(3) 0.063(4) 0.073(4) 0.007(3) 0.020(3) 0.001(3) C242 0.064(4) 0.058(4) 0.053(3) -0.005(3) 0.023(3) -0.005(3) C243 0.099(5) 0.061(5) 0.105(5) 0.003(3) 0.052(4) 0.009(4) C244 0.153(8) 0.070(6) 0.133(6) 0.014(4) 0.083(6) 0.009(6) C245 0.132(7) 0.075(6) 0.087(5) 0.003(4) 0.022(4) 0.039(5) C246 0.069(5) 0.076(6) 0.137(6) 0.001(4) 0.016(4) 0.018(4) C247 0.067(4) 0.057(4) 0.114(5) 0.012(3) 0.024(3) 0.009(3) N250 0.031(2) 0.088(4) 0.060(3) -0.016(3) 0.0143(19) 0.011(3) C251 0.046(4) 0.068(5) 0.061(4) 0.005(3) 0.009(3) -0.008(3) C252 0.022(3) 0.054(4) 0.060(3) -0.007(3) 0.007(2) -0.006(3) C253 0.057(4) 0.057(5) 0.081(4) -0.009(3) 0.027(3) -0.008(3) C254 0.090(5) 0.080(5) 0.085(5) -0.043(4) 0.039(4) -0.015(4) C255 0.090(5) 0.099(6) 0.076(4) -0.012(4) 0.039(3) -0.004(4) C256 0.070(4) 0.076(5) 0.075(4) 0.006(4) 0.027(3) -0.004(4) C257 0.051(3) 0.050(4) 0.071(4) -0.002(3) 0.020(3) -0.004(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 N11 P11 1.596(4) . ? N11 P12 1.610(4) . ? P11 N13 1.596(4) . ? P11 N110 1.640(4) . ? P11 N140 1.651(5) . ? N12 P13 1.581(4) . ? N12 P12 1.584(4) . ? P12 N120 1.627(4) . ? P12 N150 1.653(5) . ? N13 P13 1.602(4) . ? P13 N130 1.637(5) . ? P13 N160 1.645(4) . ? N21 P22 1.601(4) . ? N21 P21 1.599(4) . ? P21 N23 1.579(4) . ? P21 N210 1.643(5) . ? P21 N240 1.649(5) . ? N22 P43 1.559(6) . ? N22 P22 1.582(4) . ? N22 P23 1.636(5) . ? P22 N250 1.639(4) . ? P22 N220 1.662(5) . ? N23 P23 1.510(5) . ? N23 P43 1.691(6) . ? P23 N230 1.613(7) . ? P23 N260 1.672(8) . ? P43 N460 1.625(9) . ? P43 N430 1.661(9) . ? N110 C111 1.455(6) . ? C111 C112 1.495(5) . ? C112 C117 1.370(7) . ? C112 C113 1.385(7) . ? C113 C114 1.381(7) . ? C114 C115 1.379(8) . ? C115 C116 1.364(8) . ? C116 C117 1.381(6) . ? N120 C121 1.457(6) . ? C121 C122 1.504(6) . ? C122 C123 1.371(7) . ? C122 C127 1.369(6) . ? C123 C124 1.359(8) . ? C124 C125 1.356(9) . ? C125 C126 1.371(8) . ? C126 C127 1.392(7) . ? N130 C131 1.459(7) . ? C131 C132 1.503(7) . ? C132 C133 1.359(7) . ? C132 C137 1.363(7) . ? C133 C134 1.381(8) . ? C134 C135 1.350(9) . ? C135 C136 1.341(9) . ? C136 C137 1.395(9) . ? N140 C341 1.362(11) . ? N140 C141 1.555(10) . ? C141 C142 1.457(10) . ? C142 C143 1.362(11) . ? C142 C147 1.366(11) . ? C143 C144 1.341(10) . ? C144 C145 1.382(13) . ? C145 C146 1.347(13) . ? C146 C147 1.430(13) . ? C341 C342 1.518(12) . ? C342 C343 1.374(13) . ? C342 C347 1.371(13) . ? C343 C344 1.417(15) . ? C344 C345 1.342(15) . ? C345 C346 1.359(15) . ? C346 C347 1.438(15) . ? N150 C151 1.455(7) . ? C151 C152 1.496(7) . ? C152 C157 1.363(7) . ? C152 C153 1.393(8) . ? C153 C154 1.390(9) . ? C154 C155 1.346(10) . ? C155 C156 1.369(9) . ? C156 C157 1.396(8) . ? N160 C161 1.444(6) . ? C161 C162 1.517(6) . ? C162 C163 1.364(7) . ? C162 C167 1.379(7) . ? C163 C164 1.398(8) . ? C164 C165 1.355(9) . ? C165 C166 1.344(9) . ? C166 C167 1.367(7) . ? N210 C211 1.453(6) . ? C211 C212 1.516(6) . ? C212 C217 1.361(7) . ? C212 C213 1.369(7) . ? C213 C214 1.384(8) . ? C214 C215 1.372(9) . ? C215 C216 1.350(9) . ? C216 C217 1.393(8) . ? N220 C221 1.533(12) . ? N220 C421 1.398(11) . ? C221 C222 1.548(12) . ? C222 C223 1.386(10) . ? C222 C227 1.350(11) . ? C223 C224 1.397(12) . ? C224 C225 1.390(12) . ? C225 C226 1.370(12) . ? C226 C227 1.408(10) . ? C421 C422 1.502(12) . ? C422 C423 1.364(12) . ? C422 C427 1.370(12) . ? C423 C424 1.396(13) . ? C424 C425 1.371(14) . ? C425 C426 1.351(13) . ? C426 C427 1.412(12) . ? N230 C231 1.496(10) . ? C231 C232 1.505(11) . ? C232 C233 1.355(12) . ? C232 C237 1.404(12) . ? C233 C234 1.421(12) . ? C234 C235 1.366(13) . ? C235 C236 1.349(13) . ? C236 C237 1.390(11) . ? N430 C431 1.458(12) . ? C431 C432 1.529(12) . ? C432 C433 1.382(13) . ? C432 C437 1.387(12) . ? C433 C434 1.388(13) . ? C434 C435 1.357(14) . ? C435 C436 1.360(14) . ? C436 C437 1.422(13) . ? N240 C241 1.452(6) . ? C241 C242 1.500(7) . ? C242 C247 1.358(7) . ? C242 C243 1.376(7) . ? C243 C244 1.375(8) . ? C244 C245 1.357(8) . ? C245 C246 1.364(8) . ? C246 C247 1.389(7) . ? N250 C251 1.453(7) . ? C251 C252 1.510(6) . ? C252 C257 1.373(7) . ? C252 C253 1.387(7) . ? C253 C254 1.383(6) . ? C254 C255 1.368(8) . ? C255 C256 1.367(8) . ? C256 C257 1.380(6) . ? N260 C261 1.446(9) . ? C261 C262 1.508(11) . ? C262 C263 1.368(11) . ? C262 C267 1.372(11) . ? C263 C264 1.388(11) . ? C264 C265 1.327(12) . ? C265 C266 1.379(13) . ? C266 C267 1.392(13) . ? N460 C461 1.424(11) . ? C461 C462 1.495(11) . ? C462 C467 1.376(12) . ? C462 C463 1.385(11) . ? C463 C464 1.472(13) . ? C464 C465 1.373(14) . ? C465 C466 1.361(14) . ? C466 C467 1.369(13) . ? 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 P11 N11 P12 125.4(2) . . ? N11 P11 N13 115.31(19) . . ? N11 P11 N110 107.7(2) . . ? N13 P11 N110 115.5(2) . . ? N11 P11 N140 113.7(2) . . ? N13 P11 N140 104.6(2) . . ? N110 P11 N140 99.0(3) . . ? P13 N12 P12 124.6(2) . . ? N12 P12 N11 114.2(2) . . ? N12 P12 N120 105.1(2) . . ? N11 P12 N120 116.2(2) . . ? N12 P12 N150 116.8(2) . . ? N11 P12 N150 105.1(2) . . ? N120 P12 N150 98.9(2) . . ? P11 N13 P13 122.8(2) . . ? N12 P13 N13 117.2(2) . . ? N12 P13 N130 114.3(3) . . ? N13 P13 N130 103.8(2) . . ? N12 P13 N160 103.6(2) . . ? N13 P13 N160 115.4(3) . . ? N130 P13 N160 101.9(3) . . ? P22 N21 P21 126.0(2) . . ? N23 P21 N21 114.0(2) . . ? N23 P21 N210 115.7(2) . . ? N21 P21 N210 105.5(2) . . ? N23 P21 N240 106.3(2) . . ? N21 P21 N240 115.7(2) . . ? N210 P21 N240 99.0(2) . . ? P43 N22 P22 125.4(3) . . ? P43 N22 P23 14.5(2) . . ? P22 N22 P23 122.0(3) . . ? N22 P22 N21 114.3(2) . . ? N22 P22 N250 115.2(2) . . ? N21 P22 N250 107.96(19) . . ? N22 P22 N220 105.3(2) . . ? N21 P22 N220 114.3(2) . . ? N250 P22 N220 98.9(2) . . ? P23 N23 P21 125.1(3) . . ? P23 N23 P43 13.2(2) . . ? P21 N23 P43 123.7(3) . . ? N23 P23 N230 102.5(4) . . ? N23 P23 N22 118.0(3) . . ? N230 P23 N22 119.5(4) . . ? N23 P23 N260 110.9(4) . . ? N230 P23 N260 102.3(4) . . ? N22 P23 N260 102.6(4) . . ? N22 P43 N460 108.9(4) . . ? N22 P43 N430 109.5(5) . . ? N460 P43 N430 102.4(6) . . ? N22 P43 N23 112.2(3) . . ? N460 P43 N23 114.0(4) . . ? N430 P43 N23 109.4(5) . . ? C111 N110 P11 123.5(3) . . ? N110 C111 C112 114.2(4) . . ? C117 C112 C113 117.9(4) . . ? C117 C112 C111 122.3(4) . . ? C113 C112 C111 119.7(5) . . ? C114 C113 C112 121.2(5) . . ? C115 C114 C113 120.0(6) . . ? C116 C115 C114 119.1(6) . . ? C115 C116 C117 120.8(6) . . ? C112 C117 C116 121.1(5) . . ? C121 N120 P12 121.4(3) . . ? N120 C121 C122 114.3(4) . . ? C123 C122 C127 117.3(5) . . ? C123 C122 C121 118.8(5) . . ? C127 C122 C121 123.8(5) . . ? C124 C123 C122 122.3(6) . . ? C125 C124 C123 119.9(7) . . ? C124 C125 C126 120.1(7) . . ? C125 C126 C127 119.0(6) . . ? C122 C127 C126 121.3(6) . . ? C131 N130 P13 121.2(4) . . ? N130 C131 C132 112.7(5) . . ? C133 C132 C137 118.3(6) . . ? C133 C132 C131 123.0(6) . . ? C137 C132 C131 118.6(6) . . ? C132 C133 C134 121.8(6) . . ? C135 C134 C133 119.8(7) . . ? C136 C135 C134 118.9(8) . . ? C135 C136 C137 122.1(8) . . ? C132 C137 C136 118.9(7) . . ? C341 N140 C141 23.6(8) . . ? C341 N140 P11 130.6(8) . . ? C141 N140 P11 112.4(5) . . ? C142 C141 N140 118.6(8) . . ? C143 C142 C147 118.7(9) . . ? C143 C142 C141 120.2(9) . . ? C147 C142 C141 121.1(10) . . ? C142 C143 C144 123.0(10) . . ? C145 C144 C143 118.2(11) . . ? C146 C145 C144 122.3(12) . . ? C145 C146 C147 117.5(14) . . ? C142 C147 C146 120.1(11) . . ? N140 C341 C342 111.4(11) . . ? C343 C342 C347 122.3(14) . . ? C343 C342 C341 119.7(14) . . ? C347 C342 C341 117.5(13) . . ? C342 C343 C344 122.2(16) . . ? C345 C344 C343 110.4(18) . . ? C344 C345 C346 131.6(19) . . ? C345 C346 C347 113.6(17) . . ? C342 C347 C346 117.8(15) . . ? C151 N150 P12 124.2(4) . . ? N150 C151 C152 116.8(5) . . ? C157 C152 C153 118.2(6) . . ? C157 C152 C151 124.1(6) . . ? C153 C152 C151 117.7(7) . . ? C154 C153 C152 118.9(8) . . ? C155 C154 C153 122.3(9) . . ? C154 C155 C156 119.4(9) . . ? C155 C156 C157 119.1(8) . . ? C152 C157 C156 122.0(8) . . ? C161 N160 P13 125.0(3) . . ? N160 C161 C162 111.1(4) . . ? C163 C162 C167 119.0(5) . . ? C163 C162 C161 120.6(5) . . ? C167 C162 C161 120.4(5) . . ? C162 C163 C164 118.9(6) . . ? C165 C164 C163 120.5(7) . . ? C166 C165 C164 120.8(7) . . ? C165 C166 C167 119.4(7) . . ? C166 C167 C162 121.4(6) . . ? C211 N210 P21 124.0(4) . . ? N210 C211 C212 117.2(5) . . ? C217 C212 C213 118.9(6) . . ? C217 C212 C211 122.7(6) . . ? C213 C212 C211 118.4(5) . . ? C212 C213 C214 121.7(6) . . ? C215 C214 C213 118.9(8) . . ? C216 C215 C214 119.6(8) . . ? C215 C216 C217 121.4(7) . . ? C212 C217 C216 119.5(7) . . ? C221 N220 C421 13.3(12) . . ? C221 N220 P22 116.8(7) . . ? C421 N220 P22 122.5(7) . . ? N220 C221 C222 108.0(9) . . ? C223 C222 C227 121.5(10) . . ? C223 C222 C221 112.0(10) . . ? C227 C222 C221 126.5(9) . . ? C222 C223 C224 123.2(10) . . ? C225 C224 C223 112.4(10) . . ? C226 C225 C224 126.7(11) . . ? C225 C226 C227 117.6(10) . . ? C222 C227 C226 118.6(9) . . ? C422 C421 N220 116.7(9) . . ? C423 C422 C427 117.8(10) . . ? C423 C422 C421 122.0(11) . . ? C427 C422 C421 120.2(10) . . ? C422 C423 C424 116.7(12) . . ? C425 C424 C423 122.0(13) . . ? C426 C425 C424 124.6(13) . . ? C425 C426 C427 110.7(12) . . ? C422 C427 C426 127.7(12) . . ? C231 N230 P23 121.0(6) . . ? N230 C231 C232 106.6(8) . . ? C233 C232 C237 118.7(12) . . ? C233 C232 C231 121.9(11) . . ? C237 C232 C231 116.9(9) . . ? C232 C233 C234 120.6(13) . . ? C235 C234 C233 115.6(12) . . ? C236 C235 C234 124.0(11) . . ? C235 C236 C237 119.4(11) . . ? C236 C237 C232 117.3(12) . . ? C431 N430 P43 122.2(9) . . ? N430 C431 C432 115.1(10) . . ? C433 C432 C437 113.1(12) . . ? C433 C432 C431 118.6(12) . . ? C437 C432 C431 128.2(12) . . ? C432 C433 C434 124.9(14) . . ? C435 C434 C433 116.2(13) . . ? C434 C435 C436 122.2(13) . . ? C435 C436 C437 118.7(13) . . ? C432 C437 C436 120.2(13) . . ? C241 N240 P21 119.7(3) . . ? N240 C241 C242 114.1(4) . . ? C247 C242 C243 117.7(5) . . ? C247 C242 C241 123.0(5) . . ? C243 C242 C241 119.3(5) . . ? C244 C243 C242 121.4(6) . . ? C245 C244 C243 120.3(7) . . ? C244 C245 C246 119.4(7) . . ? C245 C246 C247 120.0(7) . . ? C242 C247 C246 121.3(6) . . ? C251 N250 P22 123.9(3) . . ? N250 C251 C252 113.4(4) . . ? C257 C252 C253 117.7(5) . . ? C257 C252 C251 122.5(4) . . ? C253 C252 C251 119.7(5) . . ? C254 C253 C252 119.6(5) . . ? C255 C254 C253 121.4(6) . . ? C254 C255 C256 119.7(6) . . ? C255 C256 C257 118.7(6) . . ? C252 C257 C256 122.8(5) . . ? C261 N260 P23 122.0(6) . . ? N260 C261 C262 114.5(8) . . ? C263 C262 C267 117.5(10) . . ? C263 C262 C261 120.2(9) . . ? C267 C262 C261 122.2(10) . . ? C262 C263 C264 125.1(10) . . ? C265 C264 C263 113.3(11) . . ? C264 C265 C266 121.6(11) . . ? C265 C266 C267 121.7(11) . . ? C262 C267 C266 117.0(11) . . ? C461 N460 P43 122.6(9) . . ? N460 C461 C462 116.6(9) . . ? C467 C462 C463 119.3(10) . . ? C467 C462 C461 115.5(10) . . ? C463 C462 C461 124.4(10) . . ? C462 C463 C464 113.0(11) . . ? C465 C464 C463 120.2(14) . . ? C466 C465 C464 118.9(14) . . ? C465 C466 C467 117.2(13) . . ? C466 C467 C462 124.8(13) . . ? 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 N110 H110 N22 0.78(2) 2.29(2) 3.071(5) 173(5) 1_655 N120 H120 N21 0.78(2) 2.32(2) 3.087(5) 168(5) . N240 H240 N11 0.79(2) 2.41(2) 3.194(5) 174(5) . N250 H250 N13 0.77(2) 2.35(3) 3.104(5) 164(5) 1_455 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 22.41 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.195 _refine_diff_density_min -0.214 _refine_diff_density_rms 0.032 #===END data_P5 _database_code_CSD 199624 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H68 N9 O P3' _chemical_formula_weight 928.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 33.828(3) _cell_length_b 12.5140(10) _cell_length_c 25.588(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.0730(10) _cell_angle_gamma 90.00 _cell_volume 10107.5(14) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.220 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3968 _exptl_absorpt_coefficient_mu 0.165 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart Apex CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20873 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.0580 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 25.03 _reflns_number_total 8915 _reflns_number_gt 6905 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+0.8445P] 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 8915 _refine_ls_number_parameters 644 _refine_ls_number_restraints 191 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1147 _refine_ls_wR_factor_gt 0.1061 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.22076(5) 0.96708(11) 0.24064(6) 0.0207(3) Uani 1 1 d . . . P1 P 0.212397(15) 0.85325(4) 0.210131(19) 0.01837(13) Uani 1 1 d . . . N2 N 0.25950(5) 0.86704(11) 0.33926(6) 0.0208(3) Uani 1 1 d . . . P2 P 0.251240(15) 0.97640(4) 0.305182(19) 0.01873(13) Uani 1 1 d . . . N3 N 0.21338(5) 0.75085(11) 0.24853(6) 0.0192(3) Uani 1 1 d . . . P3 P 0.245440(15) 0.75159(4) 0.312177(19) 0.01857(13) Uani 1 1 d . . . N10 N 0.24606(5) 0.82407(12) 0.17917(6) 0.0230(4) Uani 1 1 d D . . H10 H 0.2558(6) 0.7654(12) 0.1834(8) 0.028 Uiso 1 1 d D . . C11 C 0.25427(6) 0.89159(15) 0.13786(7) 0.0253(4) Uani 1 1 d . . . H11A H 0.2851 0.8908 0.1452 0.030 Uiso 1 1 calc R . . H11B H 0.2463 0.9660 0.1429 0.030 Uiso 1 1 calc R . . C12 C 0.23059(7) 0.85844(16) 0.07700(8) 0.0307(5) Uani 1 1 d . . . H12A H 0.2379 0.7837 0.0715 0.037 Uiso 1 1 calc R . . H12B H 0.1997 0.8619 0.0687 0.037 Uiso 1 1 calc R . . C13 C 0.24188(6) 0.93043(16) 0.03748(7) 0.0273(5) Uani 1 1 d . . . C14 C 0.27505(7) 0.90662(18) 0.01973(8) 0.0342(5) Uani 1 1 d . . . H14 H 0.2903 0.8418 0.0314 0.041 Uiso 1 1 calc R . . C15 C 0.28638(8) 0.9762(2) -0.01485(9) 0.0444(6) Uani 1 1 d . . . H15 H 0.3091 0.9584 -0.0269 0.053 Uiso 1 1 calc R . . C16 C 0.26479(9) 1.0706(2) -0.03168(9) 0.0493(7) Uani 1 1 d . . . H16 H 0.2725 1.1181 -0.0554 0.059 Uiso 1 1 calc R . . C17 C 0.23228(9) 1.0959(2) -0.01423(9) 0.0501(7) Uani 1 1 d . . . H17 H 0.2176 1.1616 -0.0255 0.060 Uiso 1 1 calc R . . C18 C 0.22050(7) 1.02613(18) 0.01988(8) 0.0385(5) Uani 1 1 d . . . H18 H 0.1975 1.0442 0.0313 0.046 Uiso 1 1 calc R . . N20 N 0.29702(5) 1.03497(12) 0.31699(7) 0.0241(4) Uani 1 1 d D . . H20 H 0.2956(6) 1.0923(13) 0.3034(8) 0.029 Uiso 1 1 d D . . C21 C 0.33565(6) 0.97782(15) 0.32093(8) 0.0263(4) Uani 1 1 d . . . H21A H 0.3316 0.9006 0.3257 0.032 Uiso 1 1 calc R . . H21B H 0.3592 1.0028 0.3545 0.032 Uiso 1 1 calc R . . C22 C 0.34779(7) 0.9934(2) 0.26983(9) 0.0394(6) Uani 1 1 d . . . H22A H 0.3249 0.9647 0.2365 0.047 Uiso 1 1 calc R . . H22B H 0.3503 1.0709 0.2638 0.047 Uiso 1 1 calc R . . C23 C 0.38859(7) 0.93976(17) 0.27533(8) 0.0321(5) Uani 1 1 d . . . C24 C 0.42742(8) 0.9855(2) 0.30622(10) 0.0531(7) Uani 1 1 d . . . H24 H 0.4283 1.0539 0.3227 0.064 Uiso 1 1 calc R . . C25 C 0.46505(9) 0.9319(4) 0.31319(14) 0.0829(12) Uani 1 1 d . . . H25 H 0.4915 0.9631 0.3347 0.100 Uiso 1 1 calc R . . C26 C 0.46372(13) 0.8334(4) 0.28870(16) 0.0976(15) Uani 1 1 d . . . H26 H 0.4893 0.7966 0.2935 0.117 Uiso 1 1 calc R . . C27 C 0.42672(12) 0.7894(3) 0.25834(12) 0.0774(11) Uani 1 1 d . . . H27 H 0.4261 0.7217 0.2413 0.093 Uiso 1 1 calc R . . C28 C 0.38934(8) 0.8414(2) 0.25149(9) 0.0449(6) Uani 1 1 d . . . H28 H 0.3633 0.8085 0.2297 0.054 Uiso 1 1 calc R . . N30 N 0.28833(5) 0.68371(12) 0.31845(6) 0.0229(4) Uani 1 1 d D . . H30 H 0.2837(6) 0.6290(13) 0.3011(8) 0.027 Uiso 1 1 d D . . C31 C 0.32658(6) 0.68382(15) 0.36890(8) 0.0245(4) Uani 1 1 d . . . H31A H 0.3246 0.6266 0.3946 0.029 Uiso 1 1 calc R . . H31B H 0.3291 0.7531 0.3885 0.029 Uiso 1 1 calc R . . C32 C 0.36527(6) 0.66602(16) 0.35362(8) 0.0281(5) Uani 1 1 d . . . H32A H 0.3620 0.5973 0.3333 0.034 Uiso 1 1 calc R . . H32B H 0.3667 0.7235 0.3278 0.034 Uiso 1 1 calc R . . C33 C 0.40637(6) 0.66395(15) 0.40304(8) 0.0258(4) Uani 1 1 d . . . C34 C 0.43718(7) 0.74100(17) 0.40961(9) 0.0340(5) Uani 1 1 d . . . H34 H 0.4319 0.7977 0.3833 0.041 Uiso 1 1 calc R . . C35 C 0.47549(7) 0.73685(18) 0.45383(10) 0.0405(6) Uani 1 1 d . . . H35 H 0.4963 0.7902 0.4576 0.049 Uiso 1 1 calc R . . C36 C 0.48356(7) 0.65594(19) 0.49230(10) 0.0428(6) Uani 1 1 d . . . H36 H 0.5100 0.6528 0.5225 0.051 Uiso 1 1 calc R . . C37 C 0.45314(7) 0.57887(19) 0.48710(9) 0.0409(6) Uani 1 1 d . . . H37 H 0.4586 0.5231 0.5140 0.049 Uiso 1 1 calc R . . C38 C 0.41474(7) 0.58271(16) 0.44277(9) 0.0323(5) Uani 1 1 d . . . H38 H 0.3939 0.5295 0.4394 0.039 Uiso 1 1 calc R . . N40 N 0.16620(5) 0.86643(12) 0.15846(7) 0.0237(4) Uani 1 1 d D . . H40 H 0.1495(6) 0.8982(15) 0.1678(8) 0.028 Uiso 1 1 d D . . C41 C 0.14713(6) 0.76922(15) 0.12745(8) 0.0268(4) Uani 1 1 d . . . H41A H 0.1357 0.7252 0.1508 0.032 Uiso 1 1 calc R . . H41B H 0.1694 0.7270 0.1203 0.032 Uiso 1 1 calc R . . C42 C 0.11181(6) 0.79288(16) 0.07196(8) 0.0312(5) Uani 1 1 d . . . H42A H 0.0899 0.8378 0.0783 0.037 Uiso 1 1 calc R . . H42B H 0.1233 0.8322 0.0470 0.037 Uiso 1 1 calc R . . C43 C 0.09271(6) 0.68862(16) 0.04523(8) 0.0318(5) Uani 1 1 d . . . C44 C 0.10526(8) 0.64058(19) 0.00511(10) 0.0454(6) Uani 1 1 d . . . H44 H 0.1244 0.6765 -0.0084 0.054 Uiso 1 1 calc R . . C45 C 0.09005(9) 0.5401(2) -0.01568(11) 0.0576(7) Uani 1 1 d . . . H45 H 0.0986 0.5081 -0.0436 0.069 Uiso 1 1 calc R . . C46 C 0.06279(9) 0.4871(2) 0.00386(11) 0.0536(7) Uani 1 1 d . . . H46 H 0.0526 0.4182 -0.0102 0.064 Uiso 1 1 calc R . . C47 C 0.05018(7) 0.53354(19) 0.04365(10) 0.0450(6) Uani 1 1 d . . . H47 H 0.0314 0.4967 0.0574 0.054 Uiso 1 1 calc R . . C48 C 0.06479(7) 0.63398(17) 0.06382(9) 0.0380(5) Uani 1 1 d . . . H48 H 0.0555 0.6661 0.0910 0.046 Uiso 1 1 calc R . . N50 N 0.22940(5) 1.07044(12) 0.33237(6) 0.0220(4) Uani 1 1 d D . . H50 H 0.2463(6) 1.0812(16) 0.3639(6) 0.026 Uiso 1 1 d D . . C51 C 0.18624(6) 1.05626(16) 0.33223(8) 0.0279(5) Uani 1 1 d . . . H51A H 0.1818 0.9808 0.3404 0.033 Uiso 1 1 calc R . . H51B H 0.1653 1.0744 0.2949 0.033 Uiso 1 1 calc R . . C52 C 0.18002(6) 1.12847(16) 0.37631(8) 0.0307(5) Uani 1 1 d . . . H52A H 0.2014 1.1092 0.4132 0.037 Uiso 1 1 calc R . . H52B H 0.1858 1.2030 0.3682 0.037 Uiso 1 1 calc R . . C53 C 0.13682(7) 1.12459(17) 0.38074(8) 0.0309(5) Uani 1 1 d . . . C54 C 0.11408(7) 1.21759(19) 0.37876(9) 0.0395(5) Uani 1 1 d . . . H54 H 0.1258 1.2842 0.3739 0.047 Uiso 1 1 calc R . . C55 C 0.07461(8) 1.2153(2) 0.38372(10) 0.0504(7) Uani 1 1 d . . . H55 H 0.0596 1.2799 0.3824 0.060 Uiso 1 1 calc R . . C56 C 0.05734(8) 1.1198(2) 0.39055(11) 0.0565(7) Uani 1 1 d . . . H56 H 0.0301 1.1179 0.3935 0.068 Uiso 1 1 calc R . . C57 C 0.07939(9) 1.0269(2) 0.39313(13) 0.0642(8) Uani 1 1 d . . . H57 H 0.0676 0.9606 0.3982 0.077 Uiso 1 1 calc R . . C58 C 0.11889(8) 1.02965(19) 0.38837(11) 0.0490(6) Uani 1 1 d . . . H58 H 0.1340 0.9648 0.3904 0.059 Uiso 1 1 calc R . . N60 N 0.22192(5) 0.68150(12) 0.34765(6) 0.0235(4) Uani 1 1 d D . . H60 H 0.2387(6) 0.6564(16) 0.3748(7) 0.028 Uiso 1 1 d D . . C61 C 0.18123(6) 0.71234(15) 0.35022(8) 0.0268(4) Uani 1 1 d . . . H61A H 0.1616 0.7317 0.3123 0.032 Uiso 1 1 calc R . . H61B H 0.1850 0.7759 0.3746 0.032 Uiso 1 1 calc R . . C62 C 0.16231(7) 0.62144(17) 0.37313(9) 0.0352(5) Uani 1 1 d . . . H62A H 0.1583 0.5584 0.3484 0.042 Uiso 1 1 calc R . . H62B H 0.1824 0.6013 0.4107 0.042 Uiso 1 1 calc R . . C63 C 0.12055(7) 0.65133(16) 0.37723(9) 0.0345(5) Uani 1 1 d . . . C64 C 0.11883(8) 0.70679(19) 0.42324(11) 0.0486(6) Uani 1 1 d . . . H64 H 0.1445 0.7248 0.4527 0.058 Uiso 1 1 calc R . . C65 C 0.08125(11) 0.7361(2) 0.42730(14) 0.0660(8) Uani 1 1 d . . . H65 H 0.0810 0.7728 0.4597 0.079 Uiso 1 1 calc R . . C66 C 0.04419(11) 0.7133(3) 0.38545(16) 0.0717(9) Uani 1 1 d . . . H66 H 0.0181 0.7353 0.3882 0.086 Uiso 1 1 calc R . . C67 C 0.04428(9) 0.6580(3) 0.33881(14) 0.0718(9) Uani 1 1 d . . . H67 H 0.0183 0.6415 0.3095 0.086 Uiso 1 1 calc R . . C68 C 0.08278(8) 0.6263(2) 0.33490(11) 0.0523(7) Uani 1 1 d . . . H68 H 0.0829 0.5875 0.3031 0.063 Uiso 1 1 calc R . . O1 O 0.0870(2) 0.9202(7) 0.1823(3) 0.091(3) Uani 0.465(9) 1 d PDU A 1 C71 C 0.0516(4) 0.9838(12) 0.1708(5) 0.090(3) Uani 0.465(9) 1 d PDU A 1 H71A H 0.0311 0.9681 0.1328 0.108 Uiso 0.465(9) 1 calc PR A 1 H71B H 0.0596 1.0601 0.1724 0.108 Uiso 0.465(9) 1 calc PR A 1 C72 C 0.0324(3) 0.9614(9) 0.2127(5) 0.078(3) Uani 0.465(9) 1 d PDU A 1 H72A H 0.0361 1.0231 0.2382 0.093 Uiso 0.465(9) 1 calc PR A 1 H72B H 0.0017 0.9470 0.1941 0.093 Uiso 0.465(9) 1 calc PR A 1 C73 C 0.0539(3) 0.8684(9) 0.2434(5) 0.083(3) Uani 0.465(9) 1 d PDU A 1 H73A H 0.0358 0.8042 0.2315 0.100 Uiso 0.465(9) 1 calc PR A 1 H73B H 0.0611 0.8789 0.2841 0.100 Uiso 0.465(9) 1 calc PR A 1 C74 C 0.0931(2) 0.8565(6) 0.2301(2) 0.076(3) Uani 0.465(9) 1 d PDU A 1 H74A H 0.1181 0.8812 0.2619 0.091 Uiso 0.465(9) 1 calc PR A 1 H74B H 0.0974 0.7808 0.2222 0.091 Uiso 0.465(9) 1 calc PR A 1 O1' O 0.0693(2) 0.8619(6) 0.1637(2) 0.100(3) Uani 0.535(9) 1 d PRDU A 2 C71' C 0.0425(2) 0.9499(6) 0.1597(2) 0.079(4) Uani 0.535(9) 1 d PRDU A 2 H71C H 0.0124 0.9283 0.1444 0.095 Uiso 0.535(9) 1 d PR A 2 H71D H 0.0473 1.0066 0.1356 0.095 Uiso 0.535(9) 1 d PR A 2 C72' C 0.0551(4) 0.9872(7) 0.2199(4) 0.112(3) Uani 0.535(9) 1 d PDU A 2 H72C H 0.0757 1.0467 0.2274 0.135 Uiso 0.535(9) 1 calc PR A 2 H72D H 0.0299 1.0119 0.2275 0.135 Uiso 0.535(9) 1 calc PR A 2 C73' C 0.0740(4) 0.8960(8) 0.2542(4) 0.090(3) Uani 0.535(9) 1 d PDU A 2 H73C H 0.0557 0.8701 0.2743 0.108 Uiso 0.535(9) 1 calc PR A 2 H73D H 0.1021 0.9146 0.2821 0.108 Uiso 0.535(9) 1 calc PR A 2 C74' C 0.0780(3) 0.8132(6) 0.2144(3) 0.070(2) Uani 0.535(9) 1 d PDU A 2 H74C H 0.1071 0.7835 0.2279 0.083 Uiso 0.535(9) 1 calc PR A 2 H74D H 0.0578 0.7541 0.2111 0.083 Uiso 0.535(9) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0300(9) 0.0143(8) 0.0158(8) 0.0017(6) 0.0057(7) 0.0012(6) P1 0.0252(3) 0.0141(2) 0.0137(2) 0.00032(18) 0.0044(2) -0.00024(19) N2 0.0311(9) 0.0173(8) 0.0125(7) -0.0005(6) 0.0060(7) -0.0001(6) P2 0.0265(3) 0.0137(2) 0.0150(2) -0.00172(18) 0.0062(2) -0.00032(19) N3 0.0250(9) 0.0141(8) 0.0172(8) -0.0008(6) 0.0061(7) -0.0020(6) P3 0.0259(3) 0.0142(2) 0.0148(2) 0.00102(18) 0.0063(2) -0.00016(19) N10 0.0366(10) 0.0143(8) 0.0194(8) 0.0031(7) 0.0118(8) 0.0027(7) C11 0.0367(12) 0.0219(10) 0.0186(10) 0.0006(8) 0.0117(9) -0.0036(8) C12 0.0384(13) 0.0327(12) 0.0195(10) 0.0003(9) 0.0085(9) -0.0061(9) C13 0.0361(12) 0.0314(11) 0.0118(9) -0.0008(8) 0.0055(9) -0.0034(9) C14 0.0375(13) 0.0403(13) 0.0210(11) -0.0037(9) 0.0060(10) -0.0017(10) C15 0.0480(15) 0.0649(17) 0.0241(12) -0.0101(11) 0.0176(11) -0.0164(13) C16 0.0730(19) 0.0534(16) 0.0198(11) 0.0034(11) 0.0145(12) -0.0214(14) C17 0.0749(19) 0.0406(14) 0.0268(12) 0.0122(11) 0.0085(13) 0.0045(13) C18 0.0486(14) 0.0428(13) 0.0236(11) 0.0033(10) 0.0125(11) 0.0060(11) N20 0.0301(9) 0.0136(8) 0.0263(9) 0.0009(7) 0.0073(8) 0.0008(7) C21 0.0276(11) 0.0230(10) 0.0260(11) 0.0041(8) 0.0069(9) 0.0006(8) C22 0.0438(14) 0.0482(14) 0.0274(12) 0.0055(10) 0.0144(11) 0.0163(11) C23 0.0374(13) 0.0370(12) 0.0239(11) 0.0072(9) 0.0134(10) 0.0036(10) C24 0.0542(18) 0.0543(16) 0.0451(15) 0.0125(13) 0.0108(13) -0.0135(13) C25 0.0303(17) 0.144(4) 0.067(2) 0.047(2) 0.0091(15) -0.0109(19) C26 0.072(3) 0.176(5) 0.062(2) 0.046(3) 0.045(2) 0.068(3) C27 0.100(3) 0.097(3) 0.0399(16) 0.0128(16) 0.0306(18) 0.064(2) C28 0.0571(16) 0.0499(15) 0.0282(12) 0.0007(11) 0.0161(12) 0.0127(12) N30 0.0280(9) 0.0177(8) 0.0185(8) -0.0042(7) 0.0029(7) -0.0005(7) C31 0.0275(11) 0.0236(10) 0.0194(10) 0.0015(8) 0.0047(9) 0.0017(8) C32 0.0305(12) 0.0259(11) 0.0266(11) -0.0023(8) 0.0088(9) -0.0022(8) C33 0.0255(11) 0.0250(10) 0.0254(11) -0.0050(8) 0.0072(9) 0.0016(8) C34 0.0316(12) 0.0319(12) 0.0358(12) -0.0011(10) 0.0088(10) -0.0007(9) C35 0.0309(13) 0.0410(14) 0.0457(14) -0.0104(11) 0.0091(11) -0.0044(10) C36 0.0297(13) 0.0505(15) 0.0395(13) -0.0103(12) 0.0019(11) 0.0112(11) C37 0.0434(15) 0.0424(14) 0.0334(12) 0.0070(11) 0.0097(11) 0.0193(11) C38 0.0330(12) 0.0245(11) 0.0395(12) -0.0013(10) 0.0132(11) 0.0041(9) N40 0.0280(10) 0.0168(8) 0.0212(9) -0.0016(7) 0.0025(7) 0.0028(7) C41 0.0290(11) 0.0194(10) 0.0248(10) 0.0000(8) 0.0011(9) -0.0016(8) C42 0.0320(12) 0.0241(11) 0.0267(11) 0.0010(9) -0.0025(9) 0.0008(9) C43 0.0283(12) 0.0281(11) 0.0253(11) 0.0026(9) -0.0069(9) 0.0011(9) C44 0.0539(16) 0.0421(14) 0.0376(13) -0.0055(11) 0.0134(12) -0.0094(11) C45 0.078(2) 0.0481(16) 0.0489(16) -0.0196(13) 0.0252(15) -0.0119(14) C46 0.0657(18) 0.0364(14) 0.0497(15) -0.0123(12) 0.0099(14) -0.0186(12) C47 0.0410(14) 0.0413(14) 0.0431(14) -0.0032(11) 0.0037(12) -0.0142(11) C48 0.0336(13) 0.0371(13) 0.0328(12) -0.0007(10) -0.0010(10) -0.0022(10) N50 0.0277(10) 0.0189(8) 0.0171(8) -0.0046(7) 0.0053(7) -0.0003(7) C51 0.0314(12) 0.0254(11) 0.0269(11) -0.0048(8) 0.0105(9) -0.0005(9) C52 0.0357(13) 0.0303(11) 0.0267(11) -0.0032(9) 0.0119(10) 0.0028(9) C53 0.0351(12) 0.0353(12) 0.0228(11) -0.0014(9) 0.0111(10) 0.0042(9) C54 0.0428(14) 0.0384(13) 0.0382(13) -0.0011(10) 0.0157(11) 0.0057(10) C55 0.0422(15) 0.0609(17) 0.0467(15) -0.0036(13) 0.0142(12) 0.0184(13) C56 0.0379(15) 0.077(2) 0.0620(17) -0.0144(15) 0.0264(14) -0.0041(14) C57 0.0629(19) 0.0553(18) 0.094(2) -0.0070(16) 0.0518(18) -0.0089(14) C58 0.0556(16) 0.0376(14) 0.0668(17) 0.0016(12) 0.0376(14) 0.0042(11) N60 0.0288(10) 0.0215(8) 0.0182(8) 0.0071(7) 0.0059(7) 0.0023(7) C61 0.0347(12) 0.0235(10) 0.0242(10) 0.0032(8) 0.0130(9) 0.0012(9) C62 0.0459(14) 0.0290(11) 0.0378(12) 0.0077(9) 0.0237(11) 0.0007(10) C63 0.0457(14) 0.0261(11) 0.0396(13) 0.0071(10) 0.0250(12) -0.0018(10) C64 0.0612(17) 0.0382(14) 0.0597(16) -0.0075(12) 0.0378(14) -0.0080(12) C65 0.084(2) 0.0478(17) 0.095(2) -0.0035(16) 0.068(2) 0.0034(15) C66 0.067(2) 0.067(2) 0.105(3) 0.0308(19) 0.060(2) 0.0220(17) C67 0.0448(18) 0.093(2) 0.076(2) 0.0305(19) 0.0195(16) -0.0041(16) C68 0.0540(17) 0.0613(17) 0.0473(15) 0.0061(13) 0.0250(14) -0.0068(13) O1 0.066(4) 0.112(6) 0.119(5) 0.070(4) 0.060(4) 0.053(4) C71 0.078(6) 0.109(7) 0.104(7) 0.062(6) 0.060(6) 0.041(6) C72 0.061(5) 0.092(7) 0.104(6) 0.034(5) 0.059(5) 0.015(4) C73 0.107(8) 0.074(6) 0.071(6) 0.015(5) 0.034(6) -0.012(5) C74 0.062(6) 0.096(7) 0.071(6) 0.037(6) 0.026(5) 0.019(5) O1' 0.111(5) 0.142(6) 0.055(3) 0.029(3) 0.040(3) 0.078(4) C71' 0.066(5) 0.097(7) 0.083(6) 0.030(5) 0.036(4) 0.036(4) C72' 0.134(9) 0.060(5) 0.145(8) 0.004(5) 0.052(8) 0.013(6) C73' 0.101(8) 0.101(7) 0.060(5) -0.011(4) 0.021(5) -0.019(5) C74' 0.070(5) 0.079(5) 0.058(4) 0.012(4) 0.021(4) 0.030(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 N1 P1 1.5999(15) . ? N1 P2 1.6062(15) . ? P1 N3 1.6077(14) . ? P1 N10 1.6452(16) . ? P1 N40 1.6527(16) . ? N2 P2 1.5926(15) . ? N2 P3 1.5990(15) . ? P2 N20 1.6402(17) . ? P2 N50 1.6687(15) . ? N3 P3 1.5997(15) . ? P3 N30 1.6386(16) . ? P3 N60 1.6569(16) . ? N10 C11 1.456(2) . ? C11 C12 1.530(3) . ? C12 C13 1.503(3) . ? C13 C14 1.386(3) . ? C13 C18 1.388(3) . ? C14 C15 1.390(3) . ? C15 C16 1.374(4) . ? C16 C17 1.365(4) . ? C17 C18 1.390(3) . ? N20 C21 1.461(2) . ? C21 C22 1.517(3) . ? C22 C23 1.495(3) . ? C23 C28 1.378(3) . ? C23 C24 1.390(3) . ? C24 C25 1.393(4) . ? C25 C26 1.376(5) . ? C26 C27 1.332(5) . ? C27 C28 1.376(4) . ? N30 C31 1.463(2) . ? C31 C32 1.511(3) . ? C32 C33 1.506(3) . ? C33 C34 1.385(3) . ? C33 C38 1.393(3) . ? C34 C35 1.381(3) . ? C35 C36 1.370(3) . ? C36 C37 1.381(3) . ? C37 C38 1.384(3) . ? N40 C41 1.469(2) . ? C41 C42 1.520(3) . ? C42 C43 1.507(3) . ? C43 C44 1.382(3) . ? C43 C48 1.382(3) . ? C44 C45 1.390(3) . ? C45 C46 1.368(4) . ? C46 C47 1.367(3) . ? C47 C48 1.381(3) . ? N50 C51 1.469(2) . ? C51 C52 1.518(3) . ? C52 C53 1.506(3) . ? C53 C58 1.379(3) . ? C53 C54 1.386(3) . ? C54 C55 1.386(3) . ? C55 C56 1.369(4) . ? C56 C57 1.369(4) . ? C57 C58 1.385(3) . ? N60 C61 1.454(2) . ? C61 C62 1.522(3) . ? C62 C63 1.501(3) . ? C63 C68 1.382(3) . ? C63 C64 1.386(3) . ? C64 C65 1.362(3) . ? C65 C66 1.355(4) . ? C66 C67 1.381(4) . ? C67 C68 1.399(4) . ? O1 C71 1.380(8) . ? O1 C74 1.411(8) . ? C71 C72 1.464(9) . ? C72 C73 1.445(10) . ? C73 C74 1.490(10) . ? O1' C74' 1.367(8) . ? O1' C71' 1.4070 . ? C71' C72' 1.516(10) . ? C72' C73' 1.442(10) . ? C73' C74' 1.494(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 N1 P2 120.12(9) . . ? N1 P1 N3 116.76(8) . . ? N1 P1 N10 113.64(8) . . ? N3 P1 N10 104.57(8) . . ? N1 P1 N40 104.59(8) . . ? N3 P1 N40 111.97(8) . . ? N10 P1 N40 104.84(8) . . ? P2 N2 P3 124.95(9) . . ? N2 P2 N1 114.96(8) . . ? N2 P2 N20 108.36(8) . . ? N1 P2 N20 115.87(8) . . ? N2 P2 N50 113.24(8) . . ? N1 P2 N50 105.25(8) . . ? N20 P2 N50 97.95(8) . . ? P3 N3 P1 118.36(9) . . ? N2 P3 N3 115.70(8) . . ? N2 P3 N30 108.12(8) . . ? N3 P3 N30 110.43(8) . . ? N2 P3 N60 111.56(8) . . ? N3 P3 N60 105.74(8) . . ? N30 P3 N60 104.75(8) . . ? C11 N10 P1 124.51(13) . . ? N10 C11 C12 114.51(15) . . ? C13 C12 C11 110.82(16) . . ? C14 C13 C18 117.90(19) . . ? C14 C13 C12 121.55(19) . . ? C18 C13 C12 120.47(19) . . ? C13 C14 C15 121.0(2) . . ? C16 C15 C14 120.1(2) . . ? C17 C16 C15 119.8(2) . . ? C16 C17 C18 120.4(2) . . ? C13 C18 C17 120.8(2) . . ? C21 N20 P2 123.76(13) . . ? N20 C21 C22 112.95(16) . . ? C23 C22 C21 112.80(17) . . ? C28 C23 C24 117.1(2) . . ? C28 C23 C22 121.5(2) . . ? C24 C23 C22 121.3(2) . . ? C23 C24 C25 120.5(3) . . ? C26 C25 C24 119.6(3) . . ? C27 C26 C25 120.4(3) . . ? C26 C27 C28 120.4(3) . . ? C27 C28 C23 121.9(3) . . ? C31 N30 P3 123.85(12) . . ? N30 C31 C32 110.18(15) . . ? C33 C32 C31 114.15(16) . . ? C34 C33 C38 118.22(19) . . ? C34 C33 C32 121.14(18) . . ? C38 C33 C32 120.63(18) . . ? C35 C34 C33 121.1(2) . . ? C36 C35 C34 120.2(2) . . ? C35 C36 C37 119.9(2) . . ? C36 C37 C38 120.1(2) . . ? C37 C38 C33 120.5(2) . . ? C41 N40 P1 117.05(12) . . ? N40 C41 C42 112.85(15) . . ? C43 C42 C41 108.67(16) . . ? C44 C43 C48 118.1(2) . . ? C44 C43 C42 121.2(2) . . ? C48 C43 C42 120.46(19) . . ? C43 C44 C45 120.5(2) . . ? C46 C45 C44 120.3(2) . . ? C47 C46 C45 119.9(2) . . ? C46 C47 C48 120.0(2) . . ? C47 C48 C43 121.2(2) . . ? C51 N50 P2 120.15(12) . . ? N50 C51 C52 109.23(15) . . ? C53 C52 C51 115.72(17) . . ? C58 C53 C54 117.5(2) . . ? C58 C53 C52 121.75(19) . . ? C54 C53 C52 120.72(19) . . ? C53 C54 C55 121.3(2) . . ? C56 C55 C54 119.9(2) . . ? C55 C56 C57 119.8(2) . . ? C56 C57 C58 120.1(3) . . ? C53 C58 C57 121.4(2) . . ? C61 N60 P3 122.23(12) . . ? N60 C61 C62 110.81(16) . . ? C63 C62 C61 112.17(17) . . ? C68 C63 C64 118.0(2) . . ? C68 C63 C62 121.1(2) . . ? C64 C63 C62 120.8(2) . . ? C65 C64 C63 121.7(3) . . ? C66 C65 C64 120.4(3) . . ? C65 C66 C67 120.0(3) . . ? C66 C67 C68 119.7(3) . . ? C63 C68 C67 120.1(3) . . ? C71 O1 C74 110.7(6) . . ? O1 C71 C72 108.3(6) . . ? C73 C72 C71 106.5(7) . . ? C72 C73 C74 105.7(6) . . ? O1 C74 C73 106.2(6) . . ? C74' O1' C71' 109.3(4) . . ? O1' C71' C72' 103.2(4) . . ? C73' C72' C71' 106.1(6) . . ? C72' C73' C74' 105.2(7) . . ? O1' C74' C73' 107.3(6) . . ? 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 N50 0.796(14) 2.552(15) 3.321(2) 162.9(19) 4_545 N20 H20 N3 0.791(14) 2.346(15) 3.132(2) 172(2) 4 N30 H30 N1 0.799(14) 2.271(15) 3.065(2) 173(2) 4_545 N40 H40 O1 0.794(14) 2.291(17) 3.029(6) 155(2) . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.379 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.049 #===END data_P6 _database_code_CSD 199625 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H60 N9 P3' _chemical_formula_weight 567.72 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 P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 13.424(7) _cell_length_b 14.344(8) _cell_length_c 24.639(13) _cell_angle_alpha 89.324(10) _cell_angle_beta 87.424(11) _cell_angle_gamma 65.306(9) _cell_volume 4306(4) _cell_formula_units_Z 5 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.095 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 0.200 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart Apex CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13197 _diffrn_reflns_av_R_equivalents 0.0962 _diffrn_reflns_av_sigmaI/netI 0.2220 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 19.98 _reflns_number_total 10124 _reflns_number_gt 5097 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0858P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.2(2) _refine_ls_number_reflns 10124 _refine_ls_number_parameters 813 _refine_ls_number_restraints 496 _refine_ls_R_factor_all 0.1793 _refine_ls_R_factor_gt 0.0927 _refine_ls_wR_factor_ref 0.2310 _refine_ls_wR_factor_gt 0.1966 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N11 N 0.8164(13) 1.4172(11) -0.1516(6) 0.030(4) Uiso 1 1 d U . . P11 P 0.9121(5) 1.3248(4) -0.1279(2) 0.0343(16) Uani 1 1 d U . . N12 N 0.6667(13) 1.3528(11) -0.1096(6) 0.025(4) Uiso 1 1 d U . . P12 P 0.6884(4) 1.4375(4) -0.1456(2) 0.0340(16) Uani 1 1 d U . . N13 N 0.8806(13) 1.2442(11) -0.0918(6) 0.027(4) Uiso 1 1 d U . . P13 P 0.7570(5) 1.2551(4) -0.0836(2) 0.0328(16) Uani 1 1 d U . . N110 N 0.9889(13) 1.3620(11) -0.0895(6) 0.035(4) Uiso 1 1 d U . . H110 H 1.0497 1.3630 -0.1037 0.042 Uiso 1 1 calc R . . C111 C 0.9559(16) 1.3936(13) -0.0313(7) 0.032(5) Uiso 1 1 d U . . H11A H 1.0169 1.4028 -0.0145 0.038 Uiso 1 1 calc R . . H11B H 0.9459 1.3371 -0.0119 0.038 Uiso 1 1 calc R . . C112 C 0.8474(17) 1.4956(14) -0.0219(7) 0.035(6) Uiso 1 1 d U . . H112 H 0.7833 1.4846 -0.0345 0.042 Uiso 1 1 calc R . . C113 C 0.8610(19) 1.5812(16) -0.0561(9) 0.057(7) Uiso 1 1 d U . . H11C H 0.7939 1.6447 -0.0520 0.086 Uiso 1 1 calc R . . H11D H 0.8744 1.5603 -0.0944 0.086 Uiso 1 1 calc R . . H11E H 0.9232 1.5926 -0.0435 0.086 Uiso 1 1 calc R . . C114 C 0.8309(18) 1.5214(16) 0.0368(8) 0.054(7) Uiso 1 1 d U . . H11F H 0.7637 1.5843 0.0429 0.081 Uiso 1 1 calc R . . H11G H 0.8937 1.5321 0.0492 0.081 Uiso 1 1 calc R . . H11H H 0.8243 1.4650 0.0571 0.081 Uiso 1 1 calc R . . N120 N 0.6210(14) 1.5564(12) -0.1205(6) 0.040(5) Uiso 1 1 d U . . H120 H 0.6551 1.5970 -0.1192 0.049 Uiso 1 1 calc R . . C121 C 0.5079(18) 1.5940(16) -0.1008(9) 0.052(7) Uiso 1 1 d U . . H12A H 0.4991 1.5407 -0.0777 0.062 Uiso 1 1 calc R . . H12B H 0.4610 1.6050 -0.1322 0.062 Uiso 1 1 calc R . . C122 C 0.468(2) 1.6915(18) -0.0688(10) 0.070(8) Uiso 1 1 d U . . H122 H 0.5159 1.6781 -0.0369 0.083 Uiso 1 1 calc R . . C123 C 0.344(2) 1.7233(19) -0.0452(11) 0.094(9) Uiso 1 1 d U . . H12C H 0.3212 1.7851 -0.0225 0.140 Uiso 1 1 calc R . . H12D H 0.3409 1.6670 -0.0233 0.140 Uiso 1 1 calc R . . H12E H 0.2951 1.7371 -0.0754 0.140 Uiso 1 1 calc R . . C124 C 0.470(3) 1.774(2) -0.0942(12) 0.122(12) Uiso 1 1 d U . . H12F H 0.4438 1.8321 -0.0689 0.184 Uiso 1 1 calc R . . H12G H 0.4224 1.7904 -0.1251 0.184 Uiso 1 1 calc R . . H12H H 0.5453 1.7590 -0.1072 0.184 Uiso 1 1 calc R . . N130 N 0.7200(12) 1.2503(11) -0.0198(6) 0.031(4) Uiso 1 1 d U . . H130 H 0.7262 1.1914 -0.0060 0.038 Uiso 1 1 calc R . . C131 C 0.6756(17) 1.3446(14) 0.0153(8) 0.040(6) Uiso 1 1 d U . . H13A H 0.6502 1.4061 -0.0081 0.049 Uiso 1 1 calc R . . H13B H 0.7351 1.3457 0.0373 0.049 Uiso 1 1 calc R . . C132 C 0.5794(17) 1.3490(15) 0.0537(8) 0.043(6) Uiso 1 1 d U . . H132 H 0.6052 1.2871 0.0774 0.052 Uiso 1 1 calc R . . C133 C 0.5471(19) 1.4466(16) 0.0897(9) 0.061(7) Uiso 1 1 d U . . H13C H 0.4878 1.4517 0.1158 0.092 Uiso 1 1 calc R . . H13D H 0.5222 1.5075 0.0666 0.092 Uiso 1 1 calc R . . H13E H 0.6109 1.4420 0.1093 0.092 Uiso 1 1 calc R . . C134 C 0.4832(19) 1.3525(17) 0.0220(9) 0.065(7) Uiso 1 1 d U . . H13F H 0.4240 1.3544 0.0474 0.097 Uiso 1 1 calc R . . H13G H 0.5072 1.2913 -0.0013 0.097 Uiso 1 1 calc R . . H13H H 0.4564 1.4140 -0.0007 0.097 Uiso 1 1 calc R . . N140 N 0.9977(13) 1.2636(12) -0.1793(6) 0.038(5) Uiso 1 1 d U . . H140 H 0.9815 1.2866 -0.2125 0.046 Uiso 1 1 calc R . . C141 C 1.0985(18) 1.1733(15) -0.1713(8) 0.045(6) Uiso 1 1 d U . . H14A H 1.0816 1.1275 -0.1458 0.054 Uiso 1 1 calc R . . H14B H 1.1498 1.1952 -0.1533 0.054 Uiso 1 1 calc R . . C142 C 1.1567(19) 1.1121(17) -0.2206(9) 0.052(7) Uiso 1 1 d U . . H142 H 1.1768 1.1579 -0.2453 0.063 Uiso 1 1 calc R . . C143 C 1.077(2) 1.0799(19) -0.2509(10) 0.081(8) Uiso 1 1 d U . . H14C H 1.1136 1.0437 -0.2846 0.121 Uiso 1 1 calc R . . H14D H 1.0114 1.1411 -0.2595 0.121 Uiso 1 1 calc R . . H14E H 1.0561 1.0344 -0.2277 0.121 Uiso 1 1 calc R . . C144 C 1.2615(18) 1.0198(16) -0.2087(9) 0.058(7) Uiso 1 1 d U . . H14F H 1.2958 0.9836 -0.2427 0.087 Uiso 1 1 calc R . . H14G H 1.2445 0.9736 -0.1842 0.087 Uiso 1 1 calc R . . H14H H 1.3120 1.0425 -0.1915 0.087 Uiso 1 1 calc R . . N150 N 0.6291(13) 1.4458(11) -0.2038(6) 0.034(4) Uiso 1 1 d U . . H150 H 0.5778 1.5045 -0.2141 0.041 Uiso 1 1 calc R . . C151 C 0.6634(17) 1.3538(14) -0.2378(8) 0.040(6) Uiso 1 1 d U . . H15A H 0.6668 1.2961 -0.2144 0.048 Uiso 1 1 calc R . . H15B H 0.7388 1.3369 -0.2528 0.048 Uiso 1 1 calc R . . C152 C 0.5922(17) 1.3605(15) -0.2842(8) 0.041(6) Uiso 1 1 d U . . H152 H 0.5791 1.4250 -0.3047 0.049 Uiso 1 1 calc R . . C153 C 0.645(2) 1.2703(16) -0.3233(9) 0.065(8) Uiso 1 1 d U . . H15C H 0.5951 1.2780 -0.3528 0.097 Uiso 1 1 calc R . . H15D H 0.6583 1.2064 -0.3039 0.097 Uiso 1 1 calc R . . H15E H 0.7142 1.2683 -0.3386 0.097 Uiso 1 1 calc R . . C154 C 0.4796(19) 1.3678(17) -0.2601(9) 0.064(7) Uiso 1 1 d U . . H15F H 0.4301 1.3762 -0.2896 0.095 Uiso 1 1 calc R . . H15G H 0.4472 1.4269 -0.2353 0.095 Uiso 1 1 calc R . . H15H H 0.4909 1.3049 -0.2401 0.095 Uiso 1 1 calc R . . N160 N 0.7622(12) 1.1462(10) -0.1088(5) 0.021(4) Uiso 1 1 d U . . H160 H 0.8247 1.0931 -0.1163 0.026 Uiso 1 1 calc R . . C161 C 0.6550(17) 1.1444(15) -0.1176(8) 0.043(6) Uiso 1 1 d U . . H16A H 0.6167 1.1471 -0.0820 0.052 Uiso 1 1 calc R . . H16B H 0.6095 1.2061 -0.1382 0.052 Uiso 1 1 calc R . . C162 C 0.6661(17) 1.0520(15) -0.1475(8) 0.037(6) Uiso 1 1 d U . . H162 H 0.7114 0.9907 -0.1258 0.044 Uiso 1 1 calc R . . C163 C 0.7194(18) 1.0393(15) -0.2037(8) 0.052(7) Uiso 1 1 d U . . H16C H 0.7226 0.9763 -0.2204 0.079 Uiso 1 1 calc R . . H16D H 0.7939 1.0349 -0.2014 0.079 Uiso 1 1 calc R . . H16E H 0.6762 1.0983 -0.2260 0.079 Uiso 1 1 calc R . . C164 C 0.5466(19) 1.0528(17) -0.1522(9) 0.065(7) Uiso 1 1 d U . . H16F H 0.5535 0.9910 -0.1716 0.097 Uiso 1 1 calc R . . H16G H 0.4996 1.1137 -0.1721 0.097 Uiso 1 1 calc R . . H16H H 0.5138 1.0541 -0.1157 0.097 Uiso 1 1 calc R . . N21 N 1.0971(15) 0.9106(12) 0.0317(6) 0.042(5) Uiso 1 1 d U . . P21 P 1.0793(5) 0.8509(4) 0.0834(2) 0.0353(16) Uani 1 1 d U . . N22 N 0.8922(13) 1.0672(11) 0.0474(6) 0.030(4) Uiso 1 1 d U . . P22 P 1.0001(5) 1.0082(4) 0.0063(2) 0.0317(16) Uani 1 1 d U . . P23 P 0.8702(5) 1.0142(4) 0.1016(2) 0.0360(16) Uani 1 1 d U . . N23 N 0.9577(14) 0.9015(12) 0.1129(6) 0.034(5) Uiso 1 1 d U . . N210 N 1.1604(14) 0.8323(12) 0.1326(7) 0.045(5) Uiso 1 1 d U . . H210 H 1.1318 0.8548 0.1653 0.054 Uiso 1 1 calc R . . C211 C 1.2826(19) 0.7780(16) 0.1248(9) 0.054(7) Uiso 1 1 d U . . H21A H 1.3004 0.7208 0.0988 0.064 Uiso 1 1 calc R . . H21B H 1.3134 0.7480 0.1600 0.064 Uiso 1 1 calc R . . C212 C 1.3389(18) 0.8453(15) 0.1043(9) 0.047(6) Uiso 1 1 d U . . H212 H 1.3110 0.8703 0.0675 0.056 Uiso 1 1 calc R . . C213 C 1.322(2) 0.9409(16) 0.1387(9) 0.067(7) Uiso 1 1 d U . . H21C H 1.3583 0.9797 0.1198 0.100 Uiso 1 1 calc R . . H21D H 1.3545 0.9188 0.1741 0.100 Uiso 1 1 calc R . . H21E H 1.2437 0.9844 0.1440 0.100 Uiso 1 1 calc R . . C214 C 1.468(2) 0.7743(18) 0.0962(10) 0.081(8) Uiso 1 1 d U . . H21F H 1.5052 0.8147 0.0798 0.122 Uiso 1 1 calc R . . H21G H 1.4800 0.7162 0.0723 0.122 Uiso 1 1 calc R . . H21H H 1.4989 0.7487 0.1315 0.122 Uiso 1 1 calc R . . N220 N 1.0538(13) 1.0863(11) -0.0166(6) 0.037(5) Uiso 1 1 d U . . H220 H 1.0461 1.1066 -0.0506 0.045 Uiso 1 1 calc R . . C221 C 1.1142(16) 1.1217(14) 0.0197(7) 0.030(5) Uiso 1 1 d U . . H22A H 1.1526 1.0674 0.0461 0.037 Uiso 1 1 calc R . . H22B H 1.0624 1.1831 0.0402 0.037 Uiso 1 1 calc R . . C222 C 1.200(2) 1.1492(17) -0.0146(9) 0.055(7) Uiso 1 1 d U . . H222 H 1.1616 1.1982 -0.0439 0.066 Uiso 1 1 calc R . . C223 C 1.2892(19) 1.0541(16) -0.0406(9) 0.057(7) Uiso 1 1 d U . . H22C H 1.3418 1.0729 -0.0616 0.086 Uiso 1 1 calc R . . H22D H 1.2560 1.0224 -0.0649 0.086 Uiso 1 1 calc R . . H22E H 1.3273 1.0053 -0.0123 0.086 Uiso 1 1 calc R . . C224 C 1.2472(19) 1.2024(16) 0.0236(9) 0.060(7) Uiso 1 1 d U . . H22F H 1.3004 1.2213 0.0033 0.090 Uiso 1 1 calc R . . H22G H 1.2837 1.1557 0.0530 0.090 Uiso 1 1 calc R . . H22H H 1.1876 1.2643 0.0390 0.090 Uiso 1 1 calc R . . N230 N 0.8504(14) 1.0954(11) 0.1501(6) 0.035(5) Uiso 1 1 d U . . H230 H 0.7882 1.1200 0.1696 0.042 Uiso 1 1 calc R . . C231 C 0.9392(18) 1.1279(17) 0.1613(9) 0.051(7) Uiso 1 1 d U . . H23A H 0.9745 1.0921 0.1946 0.061 Uiso 1 1 calc R . . H23B H 0.9951 1.1020 0.1311 0.061 Uiso 1 1 calc R . . C232 C 0.916(3) 1.227(3) 0.1680(15) 0.137(12) Uiso 1 1 d U . . H232 H 0.9081 1.2236 0.2085 0.164 Uiso 1 1 calc R . . C233 C 1.013(3) 1.258(2) 0.1702(12) 0.119(12) Uiso 1 1 d U . . H23C H 0.9894 1.3299 0.1591 0.179 Uiso 1 1 calc R . . H23D H 1.0735 1.2139 0.1456 0.179 Uiso 1 1 calc R . . H23E H 1.0387 1.2505 0.2074 0.179 Uiso 1 1 calc R . . C234 C 0.815(3) 1.316(2) 0.1649(12) 0.106(10) Uiso 1 1 d U . . H23F H 0.8300 1.3738 0.1517 0.159 Uiso 1 1 calc R . . H23G H 0.7782 1.3324 0.2010 0.159 Uiso 1 1 calc R . . H23H H 0.7677 1.3028 0.1398 0.159 Uiso 1 1 calc R . . N240 N 1.1171(13) 0.7281(11) 0.0605(6) 0.037(5) Uiso 1 1 d U . . H240 H 1.1494 0.7101 0.0280 0.045 Uiso 1 1 calc R . . C241 C 1.0974(18) 0.6557(15) 0.0927(8) 0.046(6) Uiso 1 1 d U . . H24A H 1.0225 0.6617 0.0870 0.055 Uiso 1 1 calc R . . H24B H 1.1019 0.6700 0.1315 0.055 Uiso 1 1 calc R . . C242 C 1.1829(19) 0.5442(15) 0.0781(8) 0.047(6) Uiso 1 1 d U . . H242 H 1.2589 0.5375 0.0837 0.056 Uiso 1 1 calc R . . C243 C 1.155(2) 0.4688(18) 0.1174(9) 0.079(8) Uiso 1 1 d U . . H24C H 1.2078 0.3979 0.1096 0.118 Uiso 1 1 calc R . . H24D H 1.0808 0.4759 0.1117 0.118 Uiso 1 1 calc R . . H24E H 1.1608 0.4859 0.1553 0.118 Uiso 1 1 calc R . . C244 C 1.1706(19) 0.5261(16) 0.0196(8) 0.060(7) Uiso 1 1 d U . . H24F H 1.2238 0.4571 0.0087 0.090 Uiso 1 1 calc R . . H24G H 1.1837 0.5770 -0.0028 0.090 Uiso 1 1 calc R . . H24H H 1.0961 0.5322 0.0145 0.090 Uiso 1 1 calc R . . N250 N 0.9560(14) 0.9738(11) -0.0468(6) 0.037(5) Uiso 1 1 d U . . H250 H 0.8864 0.9849 -0.0465 0.044 Uiso 1 1 calc R . . C251 C 1.0252(17) 0.9253(15) -0.0951(8) 0.040(6) Uiso 1 1 d U . . H25A H 1.1021 0.8887 -0.0843 0.048 Uiso 1 1 calc R . . H25B H 1.0226 0.9798 -0.1209 0.048 Uiso 1 1 calc R . . C252 C 0.9934(18) 0.8507(15) -0.1242(8) 0.039(6) Uiso 1 1 d U . . H252 H 0.9152 0.8877 -0.1342 0.046 Uiso 1 1 calc R . . C253 C 1.0648(19) 0.8106(16) -0.1769(9) 0.060(7) Uiso 1 1 d U . . H25C H 1.0416 0.7635 -0.1956 0.091 Uiso 1 1 calc R . . H25D H 1.1419 0.7744 -0.1680 0.091 Uiso 1 1 calc R . . H25E H 1.0560 0.8686 -0.2007 0.091 Uiso 1 1 calc R . . C254 C 1.0024(18) 0.7588(15) -0.0857(8) 0.050(7) Uiso 1 1 d U . . H25F H 0.9798 0.7120 -0.1049 0.076 Uiso 1 1 calc R . . H25G H 0.9546 0.7858 -0.0531 0.076 Uiso 1 1 calc R . . H25H H 1.0785 0.7218 -0.0751 0.076 Uiso 1 1 calc R . . N260 N 0.7487(14) 1.0084(12) 0.1034(6) 0.036(5) Uiso 1 1 d U . . H260 H 0.6941 1.0521 0.1239 0.044 Uiso 1 1 calc R . . C261 C 0.7325(18) 0.9333(15) 0.0719(8) 0.041(6) Uiso 1 1 d U . . H26A H 0.6899 0.9040 0.0945 0.049 Uiso 1 1 calc R . . H26B H 0.8049 0.8770 0.0624 0.049 Uiso 1 1 calc R . . C262 C 0.674(2) 0.9736(18) 0.0214(10) 0.068(7) Uiso 1 1 d U . . H262 H 0.7176 1.0043 -0.0005 0.081 Uiso 1 1 calc R . . C263 C 0.556(2) 1.0550(19) 0.0277(10) 0.087(9) Uiso 1 1 d U . . H26C H 0.5274 1.0778 -0.0083 0.130 Uiso 1 1 calc R . . H26D H 0.5543 1.1137 0.0484 0.130 Uiso 1 1 calc R . . H26E H 0.5107 1.0256 0.0471 0.130 Uiso 1 1 calc R . . C264 C 0.674(2) 0.882(2) -0.0121(11) 0.109(10) Uiso 1 1 d U . . H26F H 0.6394 0.9068 -0.0467 0.163 Uiso 1 1 calc R . . H26G H 0.6326 0.8496 0.0086 0.163 Uiso 1 1 calc R . . H26H H 0.7496 0.8309 -0.0192 0.163 Uiso 1 1 calc R . . N31 N 0.8184(15) 0.9948(13) 0.2579(7) 0.041(5) Uiso 1 1 d U . . P31 P 0.6965(5) 1.0417(5) 0.2889(3) 0.0456(18) Uani 1 1 d U . . N32 N 0.8892(15) 0.8288(12) 0.3245(7) 0.041(5) Uiso 1 1 d U . . P32 P 0.9074(5) 0.8832(4) 0.2685(2) 0.0385(17) Uani 1 1 d U B . N33 N 0.6785(15) 0.9707(13) 0.3364(7) 0.049(5) Uiso 1 1 d U . . P33 P 0.7783(5) 0.8791(4) 0.3611(2) 0.0410(18) Uani 1 1 d U . . N310 N 0.6613(14) 1.1601(12) 0.3177(7) 0.046(5) Uiso 1 1 d U . . H310 H 0.6370 1.1700 0.3518 0.056 Uiso 1 1 calc R . . C311 C 0.670(2) 1.2415(17) 0.2891(10) 0.065(7) Uiso 1 1 d U . . H31A H 0.6713 1.2284 0.2496 0.078 Uiso 1 1 calc R . . H31B H 0.7394 1.2450 0.2973 0.078 Uiso 1 1 calc R . . C312 C 0.572(2) 1.3472(17) 0.3036(9) 0.063(7) Uiso 1 1 d U . . H312 H 0.5018 1.3449 0.2931 0.076 Uiso 1 1 calc R . . C313 C 0.591(2) 1.429(2) 0.2688(11) 0.101(10) Uiso 1 1 d U . . H31C H 0.5964 1.4107 0.2303 0.151 Uiso 1 1 calc R . . H31D H 0.6599 1.4319 0.2788 0.151 Uiso 1 1 calc R . . H31E H 0.5301 1.4961 0.2754 0.151 Uiso 1 1 calc R . . C314 C 0.564(2) 1.372(2) 0.3615(10) 0.091(9) Uiso 1 1 d U . . H31F H 0.4999 1.4369 0.3689 0.136 Uiso 1 1 calc R . . H31G H 0.6304 1.3778 0.3717 0.136 Uiso 1 1 calc R . . H31H H 0.5550 1.3171 0.3826 0.136 Uiso 1 1 calc R . . N320 N 1.0286(14) 0.8913(12) 0.2650(6) 0.037(5) Uiso 1 1 d U . . H320 H 1.0834 0.8509 0.2434 0.044 Uiso 1 1 calc R . . C321 C 1.0393(16) 0.9713(14) 0.3006(8) 0.030(6) Uiso 1 1 d U . . H32A H 1.0409 0.9501 0.3391 0.036 Uiso 1 1 calc R . . H32B H 0.9746 1.0374 0.2968 0.036 Uiso 1 1 calc R . . C322 C 1.147(2) 0.986(2) 0.2848(11) 0.082(9) Uiso 1 1 d U . . H322 H 1.1466 1.0032 0.2454 0.098 Uiso 1 1 calc R . . C323 C 1.139(2) 1.078(2) 0.3179(11) 0.096(9) Uiso 1 1 d U . . H32C H 1.2020 1.0944 0.3079 0.143 Uiso 1 1 calc R . . H32D H 1.1400 1.0626 0.3567 0.143 Uiso 1 1 calc R . . H32E H 1.0710 1.1378 0.3103 0.143 Uiso 1 1 calc R . . C324 C 1.241(2) 0.897(2) 0.2936(11) 0.095(9) Uiso 1 1 d U . . H32F H 1.3061 0.9086 0.2832 0.142 Uiso 1 1 calc R . . H32G H 1.2400 0.8409 0.2716 0.142 Uiso 1 1 calc R . . H32H H 1.2424 0.8789 0.3321 0.142 Uiso 1 1 calc R . . N330 N 0.8068(17) 0.9195(14) 0.4202(8) 0.067(6) Uiso 1 1 d U . . H330 H 0.8762 0.8994 0.4276 0.081 Uiso 1 1 calc R . . C331 C 0.724(2) 0.985(2) 0.4601(11) 0.086(9) Uiso 1 1 d U . . H33A H 0.6582 1.0305 0.4407 0.103 Uiso 1 1 calc R . . H33B H 0.7024 0.9418 0.4849 0.103 Uiso 1 1 calc R . . C332 C 0.759(2) 1.048(2) 0.4917(11) 0.080(8) Uiso 1 1 d U . . H332 H 0.8328 1.0029 0.5056 0.096 Uiso 1 1 calc R . . C333 C 0.772(2) 1.133(2) 0.4623(11) 0.097(10) Uiso 1 1 d U . . H33C H 0.7969 1.1708 0.4870 0.146 Uiso 1 1 calc R . . H33D H 0.7010 1.1793 0.4483 0.146 Uiso 1 1 calc R . . H33E H 0.8257 1.1050 0.4319 0.146 Uiso 1 1 calc R . . C334 C 0.680(3) 1.091(2) 0.5414(12) 0.118(12) Uiso 1 1 d U . . H33F H 0.7058 1.1323 0.5637 0.177 Uiso 1 1 calc R . . H33G H 0.6774 1.0345 0.5629 0.177 Uiso 1 1 calc R . . H33H H 0.6066 1.1347 0.5292 0.177 Uiso 1 1 calc R . . N340 N 0.6105(15) 1.0689(13) 0.2378(7) 0.052(5) Uiso 1 1 d U . . H340 H 0.6400 1.0617 0.2046 0.062 Uiso 1 1 calc R . . C341 C 0.492(2) 1.1031(18) 0.2427(10) 0.062(7) Uiso 1 1 d U . . H34A H 0.4617 1.1549 0.2722 0.074 Uiso 1 1 calc R . . H34B H 0.4752 1.0440 0.2531 0.074 Uiso 1 1 calc R . . C342 C 0.436(2) 1.1479(18) 0.1923(10) 0.067(7) Uiso 1 1 d U . . H342 H 0.4635 1.0943 0.1630 0.080 Uiso 1 1 calc R . . C343 C 0.313(2) 1.1753(18) 0.2050(10) 0.074(8) Uiso 1 1 d U . . H34C H 0.2721 1.2022 0.1722 0.111 Uiso 1 1 calc R . . H34D H 0.2854 1.2275 0.2338 0.111 Uiso 1 1 calc R . . H34E H 0.3044 1.1137 0.2169 0.111 Uiso 1 1 calc R . . C344 C 0.456(2) 1.2425(18) 0.1728(10) 0.083(9) Uiso 1 1 d U . . H34F H 0.4208 1.2667 0.1383 0.124 Uiso 1 1 calc R . . H34G H 0.5350 1.2230 0.1679 0.124 Uiso 1 1 calc R . . H34H H 0.4246 1.2975 0.2001 0.124 Uiso 1 1 calc R . . N350 N 0.9259(13) 0.8005(11) 0.2195(6) 0.032(4) Uiso 1 1 d DU . . H350 H 0.9527 0.8141 0.1887 0.039 Uiso 1 1 calc R A 1 C351 C 0.905(2) 0.7072(19) 0.2180(12) 0.053(9) Uiso 0.71(2) 1 d PDU B 1 H35A H 0.9739 0.6491 0.2051 0.064 Uiso 0.71(2) 1 calc PR B 1 H35B H 0.8880 0.6915 0.2556 0.064 Uiso 0.71(2) 1 calc PR B 1 C352 C 0.818(2) 0.7133(17) 0.1840(12) 0.047(10) Uiso 0.71(2) 1 d PDU B 1 H352 H 0.8399 0.7226 0.1458 0.056 Uiso 0.71(2) 1 calc PR B 1 C353 C 0.791(3) 0.616(2) 0.1844(14) 0.078(12) Uiso 0.71(2) 1 d PDU B 1 H35C H 0.7314 0.6274 0.1598 0.117 Uiso 0.71(2) 1 calc PR B 1 H35D H 0.7676 0.6052 0.2213 0.117 Uiso 0.71(2) 1 calc PR B 1 H35E H 0.8563 0.5557 0.1723 0.117 Uiso 0.71(2) 1 calc PR B 1 C354 C 0.701(2) 0.802(2) 0.1967(14) 0.075(12) Uiso 0.71(2) 1 d PDU B 1 H35F H 0.6490 0.7989 0.1709 0.112 Uiso 0.71(2) 1 calc PR B 1 H35G H 0.7054 0.8687 0.1933 0.112 Uiso 0.71(2) 1 calc PR B 1 H35H H 0.6758 0.7950 0.2338 0.112 Uiso 0.71(2) 1 calc PR B 1 C355 C 0.819(3) 0.794(3) 0.213(2) 0.034(15) Uiso 0.29(2) 1 d PDU B 2 H35I H 0.7814 0.8028 0.2497 0.040 Uiso 0.29(2) 1 calc PR B 2 H35J H 0.7728 0.8518 0.1905 0.040 Uiso 0.29(2) 1 calc PR B 2 C356 C 0.831(4) 0.698(4) 0.189(2) 0.052(18) Uiso 0.29(2) 1 d PDU B 2 H356 H 0.8743 0.6902 0.1543 0.063 Uiso 0.29(2) 1 calc PR B 2 C357 C 0.724(5) 0.687(5) 0.176(3) 0.08(3) Uiso 0.29(2) 1 d PDU B 2 H35K H 0.7429 0.6235 0.1554 0.121 Uiso 0.29(2) 1 calc PR B 2 H35L H 0.6765 0.7457 0.1554 0.121 Uiso 0.29(2) 1 calc PR B 2 H35M H 0.6849 0.6831 0.2105 0.121 Uiso 0.29(2) 1 calc PR B 2 C358 C 0.895(6) 0.600(4) 0.224(3) 0.09(3) Uiso 0.29(2) 1 d PDU B 2 H35N H 0.9082 0.5388 0.2023 0.137 Uiso 0.29(2) 1 calc PR B 2 H35O H 0.8506 0.6013 0.2568 0.137 Uiso 0.29(2) 1 calc PR B 2 H35P H 0.9649 0.5993 0.2339 0.137 Uiso 0.29(2) 1 calc PR B 2 N360 N 0.7339(19) 0.7938(16) 0.3848(9) 0.089(7) Uiso 1 1 d U . . H360 H 0.7503 0.7697 0.4178 0.106 Uiso 1 1 calc R . . C361 C 0.674(3) 0.761(2) 0.3554(12) 0.106(10) Uiso 1 1 d U . . H36A H 0.7245 0.7017 0.3330 0.127 Uiso 1 1 calc R . . H36B H 0.6314 0.8161 0.3303 0.127 Uiso 1 1 calc R . . C362 C 0.587(2) 0.725(2) 0.3914(12) 0.090(9) Uiso 1 1 d U . . H362 H 0.6291 0.6734 0.4189 0.108 Uiso 1 1 calc R . . C363 C 0.504(4) 0.810(3) 0.4191(17) 0.196(19) Uiso 1 1 d U . . H36C H 0.4583 0.7868 0.4426 0.294 Uiso 1 1 calc R . . H36D H 0.4579 0.8590 0.3925 0.294 Uiso 1 1 calc R . . H36E H 0.5378 0.8445 0.4413 0.294 Uiso 1 1 calc R . . C364 C 0.546(3) 0.674(3) 0.3511(15) 0.165(16) Uiso 1 1 d U . . H36F H 0.4980 0.6464 0.3698 0.248 Uiso 1 1 calc R . . H36G H 0.6086 0.6170 0.3332 0.248 Uiso 1 1 calc R . . H36H H 0.5050 0.7233 0.3237 0.248 Uiso 1 1 calc R . . N41 N 0.9937(15) 0.6967(13) 0.4642(7) 0.051(5) Uiso 1 1 d U . . P41 P 1.1081(5) 0.6776(5) 0.4315(3) 0.0514(19) Uani 1 1 d U . . N42 N 1.0880(14) 0.5164(12) 0.5199(7) 0.041(5) Uiso 1 1 d U . . P42 P 0.9778(5) 0.6058(4) 0.4949(2) 0.0420(17) Uani 1 1 d U . . N43 N 1.2128(15) 0.5807(13) 0.4506(7) 0.051(5) Uiso 1 1 d U . . P43 P 1.2044(5) 0.4937(5) 0.4888(2) 0.0437(17) Uani 1 1 d U . . N410 N 1.1266(18) 0.7858(15) 0.4349(9) 0.083(7) Uiso 1 1 d U . . H410 H 1.1270 0.8195 0.4048 0.099 Uiso 1 1 calc R . . C411 C 1.141(3) 0.823(2) 0.4833(12) 0.110(10) Uiso 1 1 d U . . H41A H 1.1949 0.7651 0.5036 0.133 Uiso 1 1 calc R . . H41B H 1.0706 0.8487 0.5048 0.133 Uiso 1 1 calc R . . C412 C 1.181(2) 0.9092(18) 0.4796(10) 0.065(7) Uiso 1 1 d U . . H412 H 1.2348 0.8957 0.4480 0.078 Uiso 1 1 calc R . . C413 C 1.234(2) 0.917(2) 0.5304(11) 0.100(10) Uiso 1 1 d U . . H41C H 1.2625 0.9696 0.5258 0.150 Uiso 1 1 calc R . . H41D H 1.2941 0.8509 0.5379 0.150 Uiso 1 1 calc R . . H41E H 1.1793 0.9366 0.5608 0.150 Uiso 1 1 calc R . . C414 C 1.080(3) 1.010(2) 0.4706(13) 0.142(13) Uiso 1 1 d U . . H41F H 1.1028 1.0656 0.4638 0.213 Uiso 1 1 calc R . . H41G H 1.0301 1.0263 0.5030 0.213 Uiso 1 1 calc R . . H41H H 1.0414 1.0021 0.4392 0.213 Uiso 1 1 calc R . . N420 N 0.8928(14) 0.6495(12) 0.5477(7) 0.044(5) Uiso 1 1 d U . . H420 H 0.9135 0.6204 0.5793 0.053 Uiso 1 1 calc R . . C421 C 0.7840(19) 0.7345(16) 0.5448(9) 0.055(7) Uiso 1 1 d U . . H42A H 0.7581 0.7373 0.5076 0.066 Uiso 1 1 calc R . . H42B H 0.7903 0.7996 0.5517 0.066 Uiso 1 1 calc R . . C422 C 0.6981(18) 0.7262(15) 0.5855(9) 0.045(6) Uiso 1 1 d U . . H422 H 0.7268 0.7176 0.6228 0.054 Uiso 1 1 calc R . . C423 C 0.675(2) 0.6359(17) 0.5724(9) 0.069(8) Uiso 1 1 d U . . H42C H 0.6224 0.6303 0.5997 0.104 Uiso 1 1 calc R . . H42D H 0.7432 0.5732 0.5724 0.104 Uiso 1 1 calc R . . H42E H 0.6438 0.6449 0.5364 0.104 Uiso 1 1 calc R . . C424 C 0.593(2) 0.8262(17) 0.5838(10) 0.070(8) Uiso 1 1 d U . . H42F H 0.5393 0.8241 0.6114 0.106 Uiso 1 1 calc R . . H42G H 0.5626 0.8337 0.5478 0.106 Uiso 1 1 calc R . . H42H H 0.6106 0.8846 0.5911 0.106 Uiso 1 1 calc R . . N430 N 1.2880(15) 0.4579(12) 0.5375(7) 0.048(5) Uiso 1 1 d U . . H430 H 1.2597 0.4658 0.5710 0.058 Uiso 1 1 calc R . . C431 C 1.406(2) 0.4139(18) 0.5303(10) 0.064(7) Uiso 1 1 d U . . H43A H 1.4249 0.3844 0.4931 0.077 Uiso 1 1 calc R . . H43B H 1.4356 0.3560 0.5559 0.077 Uiso 1 1 calc R . . C432 C 1.463(3) 0.479(2) 0.5374(13) 0.117(11) Uiso 1 1 d U . . H432 H 1.4572 0.4779 0.5780 0.140 Uiso 1 1 calc R . . C433 C 1.417(2) 0.5866(18) 0.5338(10) 0.083(9) Uiso 1 1 d U . . H43C H 1.4662 0.6126 0.5499 0.124 Uiso 1 1 calc R . . H43D H 1.3456 0.6155 0.5535 0.124 Uiso 1 1 calc R . . H43E H 1.4079 0.6067 0.4956 0.124 Uiso 1 1 calc R . . C434 C 1.593(2) 0.415(2) 0.5338(11) 0.098(10) Uiso 1 1 d U . . H43F H 1.6284 0.4568 0.5471 0.148 Uiso 1 1 calc R . . H43G H 1.6175 0.3945 0.4959 0.148 Uiso 1 1 calc R . . H43H H 1.6129 0.3528 0.5561 0.148 Uiso 1 1 calc R . . N440 N 1.0974(17) 0.6678(13) 0.3667(7) 0.064(6) Uiso 1 1 d U . . H440 H 1.0328 0.6847 0.3529 0.077 Uiso 1 1 calc R . . C441 C 1.197(3) 0.631(2) 0.3320(13) 0.127(11) Uiso 1 1 d U . . H44A H 1.2572 0.5832 0.3538 0.153 Uiso 1 1 calc R . . H44B H 1.2134 0.6900 0.3229 0.153 Uiso 1 1 calc R . . C442 C 1.200(3) 0.577(2) 0.2800(13) 0.113(11) Uiso 1 1 d U . . H442 H 1.1262 0.6161 0.2649 0.136 Uiso 1 1 calc R . . C443 C 1.204(3) 0.468(2) 0.2934(12) 0.119(12) Uiso 1 1 d U . . H44C H 1.1969 0.4351 0.2600 0.179 Uiso 1 1 calc R . . H44D H 1.1435 0.4749 0.3193 0.179 Uiso 1 1 calc R . . H44E H 1.2740 0.4250 0.3094 0.179 Uiso 1 1 calc R . . C444 C 1.273(3) 0.578(2) 0.2396(13) 0.127(12) Uiso 1 1 d U . . H44F H 1.2652 0.5431 0.2072 0.191 Uiso 1 1 calc R . . H44G H 1.3484 0.5420 0.2520 0.191 Uiso 1 1 calc R . . H44H H 1.2593 0.6489 0.2307 0.191 Uiso 1 1 calc R . . N450 N 0.912(2) 0.5726(19) 0.4533(9) 0.099(8) Uiso 1 1 d U . . H450 H 0.8755 0.6208 0.4302 0.119 Uiso 1 1 calc R . . C451 C 0.903(4) 0.495(3) 0.4474(16) 0.169(15) Uiso 1 1 d U . . H45A H 0.8330 0.5056 0.4671 0.203 Uiso 1 1 calc R . . H45B H 0.9616 0.4438 0.4687 0.203 Uiso 1 1 calc R . . C452 C 0.903(4) 0.439(3) 0.3959(18) 0.155(14) Uiso 1 1 d U . . H452 H 0.8217 0.4770 0.3940 0.186 Uiso 1 1 calc R . . C453 C 0.893(3) 0.338(2) 0.4195(12) 0.115(11) Uiso 1 1 d U . . H45C H 0.8866 0.2972 0.3894 0.172 Uiso 1 1 calc R . . H45D H 0.8273 0.3586 0.4439 0.172 Uiso 1 1 calc R . . H45E H 0.9580 0.2972 0.4397 0.172 Uiso 1 1 calc R . . C454 C 0.917(3) 0.435(3) 0.3403(16) 0.168(15) Uiso 1 1 d U . . H45F H 0.8916 0.3856 0.3260 0.251 Uiso 1 1 calc R . . H45G H 0.9947 0.4135 0.3299 0.251 Uiso 1 1 calc R . . H45H H 0.8740 0.5030 0.3252 0.251 Uiso 1 1 calc R . . N460 N 1.2525(14) 0.3901(12) 0.4484(7) 0.049(5) Uiso 1 1 d U . . H460 H 1.2771 0.3950 0.4153 0.058 Uiso 1 1 calc R . . C461 C 1.255(2) 0.2958(18) 0.4656(10) 0.076(8) Uiso 1 1 d U . . H46A H 1.1885 0.2899 0.4531 0.091 Uiso 1 1 calc R . . H46B H 1.2509 0.2952 0.5059 0.091 Uiso 1 1 calc R . . C462 C 1.356(2) 0.2018(19) 0.4453(10) 0.071(8) Uiso 1 1 d U . . H462 H 1.4198 0.2130 0.4586 0.086 Uiso 1 1 calc R . . C463 C 1.371(3) 0.099(2) 0.4675(12) 0.123(12) Uiso 1 1 d U . . H46C H 1.4400 0.0463 0.4524 0.184 Uiso 1 1 calc R . . H46D H 1.3097 0.0841 0.4573 0.184 Uiso 1 1 calc R . . H46E H 1.3734 0.1005 0.5071 0.184 Uiso 1 1 calc R . . C464 C 1.373(3) 0.195(2) 0.3883(12) 0.125(12) Uiso 1 1 d U . . H46F H 1.4423 0.1370 0.3785 0.187 Uiso 1 1 calc R . . H46G H 1.3750 0.2587 0.3745 0.187 Uiso 1 1 calc R . . H46H H 1.3123 0.1854 0.3722 0.187 Uiso 1 1 calc R . . N51 N 1.1870(12) 0.4828(11) 0.6551(6) 0.027(4) Uiso 1 1 d U . . P51 P 1.1519(5) 0.3927(4) 0.6701(2) 0.0353(16) Uani 1 1 d U . . N52 N 1.0458(15) 0.6083(13) 0.7339(7) 0.054(5) Uiso 1 1 d U . . P52 P 1.1319(5) 0.5949(4) 0.6838(2) 0.0360(16) Uani 1 1 d U . . N53 N 1.0751(12) 0.4070(10) 0.7257(6) 0.025(4) Uiso 1 1 d U . . P53 P 1.0268(5) 0.5132(4) 0.7594(2) 0.0342(16) Uani 1 1 d U . . N510 N 1.2586(12) 0.2806(10) 0.6775(6) 0.028(4) Uiso 1 1 d U . . H510 H 1.2627 0.2452 0.7074 0.034 Uiso 1 1 calc R . . C511 C 1.3433(18) 0.2411(15) 0.6362(9) 0.051(7) Uiso 1 1 d U . . H51A H 1.3959 0.2722 0.6403 0.061 Uiso 1 1 calc R . . H51B H 1.3109 0.2609 0.6003 0.061 Uiso 1 1 calc R . . C512 C 1.406(2) 0.1220(17) 0.6385(9) 0.058(7) Uiso 1 1 d U . . H512 H 1.4617 0.0999 0.6075 0.070 Uiso 1 1 calc R . . C513 C 1.3290(19) 0.0676(16) 0.6316(9) 0.060(7) Uiso 1 1 d U . . H51C H 1.3714 -0.0068 0.6338 0.090 Uiso 1 1 calc R . . H51D H 1.2957 0.0850 0.5962 0.090 Uiso 1 1 calc R . . H51E H 1.2712 0.0903 0.6605 0.090 Uiso 1 1 calc R . . C514 C 1.468(2) 0.0853(18) 0.6915(9) 0.076(8) Uiso 1 1 d U . . H51F H 1.5047 0.0101 0.6914 0.113 Uiso 1 1 calc R . . H51G H 1.4157 0.1089 0.7228 0.113 Uiso 1 1 calc R . . H51H H 1.5227 0.1135 0.6938 0.113 Uiso 1 1 calc R . . N520 N 1.2250(13) 0.6326(11) 0.7116(6) 0.032(4) Uiso 1 1 d U . . H520 H 1.2165 0.6516 0.7459 0.038 Uiso 1 1 calc R . . C521 C 1.318(2) 0.6332(17) 0.6788(9) 0.063(7) Uiso 1 1 d U . . H52A H 1.3784 0.5638 0.6778 0.076 Uiso 1 1 calc R . . H52B H 1.2956 0.6535 0.6411 0.076 Uiso 1 1 calc R . . C522 C 1.353(3) 0.706(3) 0.7026(13) 0.115(11) Uiso 1 1 d U . . H522 H 1.4295 0.6736 0.6862 0.138 Uiso 1 1 calc R . . C523 C 1.329(3) 0.797(3) 0.6817(14) 0.148(14) Uiso 1 1 d U . . H52C H 1.3724 0.8280 0.6984 0.221 Uiso 1 1 calc R . . H52D H 1.2506 0.8399 0.6886 0.221 Uiso 1 1 calc R . . H52E H 1.3456 0.7897 0.6425 0.221 Uiso 1 1 calc R . . C524 C 1.386(2) 0.6930(17) 0.7589(9) 0.064(7) Uiso 1 1 d U . . H52F H 1.4224 0.7374 0.7663 0.095 Uiso 1 1 calc R . . H52G H 1.4357 0.6213 0.7649 0.095 Uiso 1 1 calc R . . H52H H 1.3202 0.7117 0.7832 0.095 Uiso 1 1 calc R . . N530 N 1.0785(13) 0.4829(11) 0.8202(6) 0.037(4) Uiso 1 1 d U . . H530 H 1.0378 0.5088 0.8500 0.044 Uiso 1 1 calc R . . C531 C 1.2029(18) 0.4063(16) 0.8232(9) 0.053(6) Uiso 1 1 d U . . H53A H 1.2114 0.3351 0.8178 0.064 Uiso 1 1 calc R . . H53B H 1.2468 0.4219 0.7941 0.064 Uiso 1 1 calc R . . C532 C 1.2422(19) 0.4165(15) 0.8765(8) 0.047(6) Uiso 1 1 d U . . H532 H 1.1849 0.4267 0.9060 0.057 Uiso 1 1 calc R . . C533 C 1.277(2) 0.5030(19) 0.8753(11) 0.091(9) Uiso 1 1 d U . . H53C H 1.3066 0.5075 0.9104 0.137 Uiso 1 1 calc R . . H53D H 1.2138 0.5675 0.8684 0.137 Uiso 1 1 calc R . . H53E H 1.3339 0.4905 0.8464 0.137 Uiso 1 1 calc R . . C534 C 1.344(2) 0.319(2) 0.8849(11) 0.101(10) Uiso 1 1 d U . . H53F H 1.3755 0.3240 0.9193 0.151 Uiso 1 1 calc R . . H53G H 1.3978 0.3102 0.8549 0.151 Uiso 1 1 calc R . . H53H H 1.3246 0.2605 0.8859 0.151 Uiso 1 1 calc R . . N540 N 1.0945(12) 0.3787(10) 0.6155(6) 0.025(4) Uiso 1 1 d U . . H540 H 1.0848 0.4225 0.5888 0.029 Uiso 1 1 calc R . . C541 C 1.0585(15) 0.2962(13) 0.6092(8) 0.029(5) Uiso 1 1 d U . . H54A H 1.0741 0.2542 0.6425 0.035 Uiso 1 1 calc R . . H54B H 1.1012 0.2513 0.5785 0.035 Uiso 1 1 calc R . . C542 C 0.9330(17) 0.3374(15) 0.5985(8) 0.040(6) Uiso 1 1 d U . . H542 H 0.9150 0.3873 0.5679 0.048 Uiso 1 1 calc R . . C543 C 0.9098(19) 0.2444(15) 0.5822(8) 0.055(7) Uiso 1 1 d U . . H54C H 0.8318 0.2680 0.5752 0.082 Uiso 1 1 calc R . . H54D H 0.9289 0.1946 0.6118 0.082 Uiso 1 1 calc R . . H54E H 0.9541 0.2120 0.5494 0.082 Uiso 1 1 calc R . . C544 C 0.8662(19) 0.3902(16) 0.6484(8) 0.059(7) Uiso 1 1 d U . . H54F H 0.7880 0.4166 0.6412 0.089 Uiso 1 1 calc R . . H54G H 0.8841 0.4473 0.6582 0.089 Uiso 1 1 calc R . . H54H H 0.8829 0.3413 0.6784 0.089 Uiso 1 1 calc R . . N550 N 1.0821(13) 0.6767(12) 0.6331(6) 0.041(5) Uiso 1 1 d U . . H550 H 1.0710 0.6539 0.6020 0.049 Uiso 1 1 calc R . . C551 C 1.0553(19) 0.7906(16) 0.6396(9) 0.060(7) Uiso 1 1 d U . . H55A H 1.0657 0.8036 0.6778 0.072 Uiso 1 1 calc R . . H55B H 1.1091 0.8060 0.6167 0.072 Uiso 1 1 calc R . . C552 C 0.943(2) 0.8638(17) 0.6251(10) 0.063(7) Uiso 1 1 d U . . H552 H 0.9317 0.8515 0.5864 0.076 Uiso 1 1 calc R . . C553 C 0.933(2) 0.9770(16) 0.6311(9) 0.062(7) Uiso 1 1 d U . . H55C H 0.8616 1.0258 0.6192 0.093 Uiso 1 1 calc R . . H55D H 0.9915 0.9846 0.6085 0.093 Uiso 1 1 calc R . . H55E H 0.9410 0.9907 0.6691 0.093 Uiso 1 1 calc R . . C554 C 0.8524(19) 0.8576(16) 0.6600(9) 0.060(7) Uiso 1 1 d U . . H55F H 0.7816 0.9057 0.6467 0.090 Uiso 1 1 calc R . . H55G H 0.8590 0.8755 0.6975 0.090 Uiso 1 1 calc R . . H55H H 0.8571 0.7877 0.6586 0.090 Uiso 1 1 calc R . . N560 N 0.8910(15) 0.5584(12) 0.7770(7) 0.048(5) Uiso 1 1 d U . . H560 H 0.8734 0.5356 0.8076 0.057 Uiso 1 1 calc R . . C561 C 0.8048(17) 0.6277(15) 0.7481(8) 0.041(6) Uiso 1 1 d U . . H56A H 0.7742 0.5887 0.7266 0.049 Uiso 1 1 calc R . . H56B H 0.8345 0.6639 0.7221 0.049 Uiso 1 1 calc R . . C562 C 0.7130(18) 0.7066(16) 0.7819(8) 0.047(6) Uiso 1 1 d U . . H562 H 0.6784 0.6722 0.8071 0.057 Uiso 1 1 calc R . . C563 C 0.7680(18) 0.7622(15) 0.8148(8) 0.055(7) Uiso 1 1 d U . . H56C H 0.7132 0.8120 0.8398 0.082 Uiso 1 1 calc R . . H56D H 0.7989 0.7979 0.7899 0.082 Uiso 1 1 calc R . . H56E H 0.8268 0.7117 0.8357 0.082 Uiso 1 1 calc R . . C564 C 0.6252(19) 0.7858(16) 0.7466(9) 0.061(7) Uiso 1 1 d U . . H56F H 0.5651 0.8335 0.7702 0.092 Uiso 1 1 calc R . . H56G H 0.5964 0.7501 0.7224 0.092 Uiso 1 1 calc R . . H56H H 0.6582 0.8241 0.7249 0.092 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P11 0.036(4) 0.035(4) 0.036(4) 0.003(3) -0.004(3) -0.019(3) P12 0.021(4) 0.039(4) 0.046(4) -0.006(3) 0.008(3) -0.018(3) P13 0.024(4) 0.036(4) 0.049(4) 0.003(3) -0.005(3) -0.022(3) P21 0.024(4) 0.035(4) 0.041(4) -0.001(3) 0.001(3) -0.008(3) P22 0.019(4) 0.025(4) 0.044(4) 0.000(3) -0.002(3) -0.002(3) P23 0.021(4) 0.035(4) 0.040(4) 0.000(3) -0.002(3) 0.000(3) P31 0.027(4) 0.039(4) 0.055(4) 0.009(3) 0.003(4) 0.001(3) P32 0.022(4) 0.042(4) 0.044(4) -0.003(3) 0.000(3) -0.005(3) P33 0.038(4) 0.037(4) 0.045(4) 0.009(3) 0.001(4) -0.013(4) P41 0.047(5) 0.035(4) 0.057(5) 0.002(3) 0.007(4) -0.003(4) P42 0.037(4) 0.045(4) 0.034(4) 0.001(3) -0.006(3) -0.006(3) P43 0.035(4) 0.048(4) 0.040(4) 0.012(3) -0.004(3) -0.009(3) P51 0.024(4) 0.023(3) 0.050(4) 0.005(3) -0.001(3) 0.000(3) P52 0.024(4) 0.031(4) 0.048(4) 0.000(3) 0.004(3) -0.007(3) P53 0.029(4) 0.035(4) 0.041(4) 0.006(3) 0.004(3) -0.017(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 N11 P11 1.541(16) . ? N11 P12 1.618(16) . ? P11 N13 1.631(15) . ? P11 N140 1.657(16) . ? P11 N110 1.673(16) . ? N12 P13 1.573(16) . ? N12 P12 1.610(15) . ? P12 N150 1.648(16) . ? P12 N120 1.673(16) . ? N13 P13 1.603(16) . ? P13 N130 1.636(15) . ? P13 N160 1.662(14) . ? N110 C111 1.50(2) . ? C111 C112 1.58(2) . ? C112 C114 1.48(2) . ? C112 C113 1.55(2) . ? N120 C121 1.44(2) . ? C121 C122 1.49(3) . ? C122 C124 1.34(3) . ? C122 C123 1.62(3) . ? N130 C131 1.50(2) . ? C131 C132 1.55(3) . ? C132 C134 1.52(3) . ? C132 C133 1.56(3) . ? N140 C141 1.45(2) . ? C141 C142 1.49(3) . ? C142 C144 1.51(3) . ? C142 C143 1.55(3) . ? N150 C151 1.46(2) . ? C151 C152 1.50(2) . ? C152 C153 1.52(3) . ? C152 C154 1.56(3) . ? N160 C161 1.47(2) . ? C161 C162 1.47(2) . ? C162 C163 1.51(2) . ? C162 C164 1.61(3) . ? N21 P21 1.593(16) . ? N21 P22 1.605(18) . ? P21 N210 1.611(18) . ? P21 N23 1.623(17) . ? P21 N240 1.712(15) . ? N22 P23 1.604(16) . ? N22 P22 1.645(16) . ? P22 N250 1.624(16) . ? P22 N220 1.647(15) . ? P23 N23 1.581(16) . ? P23 N230 1.613(15) . ? P23 N260 1.665(17) . ? N210 C211 1.50(3) . ? C211 C212 1.52(2) . ? C212 C213 1.55(3) . ? C212 C214 1.61(3) . ? N220 C221 1.46(2) . ? C221 C222 1.58(3) . ? C222 C223 1.51(3) . ? C222 C224 1.53(3) . ? N230 C231 1.49(2) . ? C231 C232 1.33(3) . ? C232 C234 1.42(4) . ? C232 C233 1.56(4) . ? N240 C241 1.40(2) . ? C241 C242 1.56(3) . ? C242 C244 1.50(3) . ? C242 C243 1.59(3) . ? N250 C251 1.46(2) . ? C251 C252 1.51(2) . ? C252 C253 1.54(3) . ? C252 C254 1.58(2) . ? N260 C261 1.43(2) . ? C261 C262 1.48(3) . ? C262 C263 1.53(3) . ? C262 C264 1.57(3) . ? N31 P32 1.574(17) . ? N31 P31 1.640(18) . ? P31 N33 1.619(17) . ? P31 N340 1.678(19) . ? P31 N310 1.714(17) . ? N32 P33 1.596(18) . ? N32 P32 1.636(17) . ? P32 N350 1.638(15) . ? P32 N320 1.678(17) . ? N33 P33 1.574(19) . ? P33 N360 1.66(2) . ? P33 N330 1.690(19) . ? N310 C311 1.40(2) . ? C311 C312 1.57(3) . ? C312 C314 1.46(3) . ? C312 C313 1.55(3) . ? N320 C321 1.51(2) . ? C321 C322 1.58(3) . ? C322 C324 1.39(3) . ? C322 C323 1.53(3) . ? N330 C331 1.46(3) . ? C331 C332 1.43(3) . ? C332 C333 1.47(3) . ? C332 C334 1.54(3) . ? N340 C341 1.46(3) . ? C341 C342 1.48(3) . ? C342 C343 1.54(3) . ? C342 C344 1.56(3) . ? N350 C351 1.48(2) . ? N350 C355 1.48(3) . ? C351 C352 1.45(3) . ? C352 C354 1.57(3) . ? C352 C353 1.58(2) . ? C355 C356 1.45(4) . ? C356 C358 1.57(3) . ? C356 C357 1.57(3) . ? N360 C361 1.33(3) . ? C361 C362 1.68(3) . ? C362 C363 1.42(4) . ? C362 C364 1.50(4) . ? N41 P42 1.584(18) . ? N41 P41 1.620(19) . ? P41 N43 1.595(19) . ? P41 N440 1.621(19) . ? P41 N410 1.68(2) . ? N42 P43 1.615(18) . ? N42 P42 1.640(18) . ? P42 N450 1.58(2) . ? P42 N420 1.635(17) . ? N43 P43 1.592(17) . ? P43 N430 1.608(18) . ? P43 N460 1.672(17) . ? N410 C411 1.37(3) . ? C411 C412 1.54(3) . ? C412 C413 1.49(3) . ? C412 C414 1.54(4) . ? N420 C421 1.46(3) . ? C421 C422 1.53(3) . ? C422 C423 1.50(2) . ? C422 C424 1.54(3) . ? N430 C431 1.44(3) . ? C431 C432 1.45(3) . ? C432 C433 1.41(3) . ? C432 C434 1.59(4) . ? N440 C441 1.45(3) . ? C441 C442 1.49(4) . ? C442 C444 1.37(4) . ? C442 C443 1.58(3) . ? N450 C451 1.18(3) . ? C451 C452 1.50(4) . ? C452 C454 1.37(4) . ? C452 C453 1.62(4) . ? N460 C461 1.40(2) . ? C461 C462 1.53(3) . ? C462 C464 1.41(3) . ? C462 C463 1.50(3) . ? N51 P51 1.584(14) . ? N51 P52 1.617(15) . ? P51 N540 1.636(15) . ? P51 N53 1.639(15) . ? P51 N510 1.662(15) . ? N52 P53 1.605(17) . ? N52 P52 1.610(18) . ? P52 N550 1.663(16) . ? P52 N520 1.725(15) . ? N53 P53 1.608(15) . ? P53 N530 1.656(16) . ? P53 N560 1.696(18) . ? N510 C511 1.42(2) . ? C511 C512 1.56(3) . ? C512 C514 1.55(3) . ? C512 C513 1.55(3) . ? N520 C521 1.45(2) . ? C521 C522 1.45(3) . ? C522 C523 1.31(3) . ? C522 C524 1.46(3) . ? N530 C531 1.57(3) . ? C531 C532 1.47(3) . ? C532 C533 1.50(3) . ? C532 C534 1.51(3) . ? N540 C541 1.465(19) . ? C541 C542 1.57(3) . ? C542 C544 1.50(3) . ? C542 C543 1.55(2) . ? N550 C551 1.53(2) . ? C551 C552 1.49(3) . ? C552 C554 1.49(3) . ? C552 C553 1.58(3) . ? N560 C561 1.39(2) . ? C561 C562 1.50(3) . ? C562 C564 1.55(3) . ? C562 C563 1.55(3) . ? 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 P11 N11 P12 125.2(10) . . ? N11 P11 N13 117.0(9) . . ? N11 P11 N140 107.4(8) . . ? N13 P11 N140 109.9(8) . . ? N11 P11 N110 111.8(8) . . ? N13 P11 N110 106.7(8) . . ? N140 P11 N110 103.2(9) . . ? P13 N12 P12 126.0(10) . . ? N12 P12 N11 113.7(9) . . ? N12 P12 N150 107.2(8) . . ? N11 P12 N150 114.5(8) . . ? N12 P12 N120 112.8(8) . . ? N11 P12 N120 106.3(8) . . ? N150 P12 N120 101.9(8) . . ? P13 N13 P11 122.5(10) . . ? N12 P13 N13 115.6(8) . . ? N12 P13 N130 108.2(8) . . ? N13 P13 N130 113.1(8) . . ? N12 P13 N160 112.7(8) . . ? N13 P13 N160 104.0(8) . . ? N130 P13 N160 102.5(7) . . ? C111 N110 P11 121.3(13) . . ? N110 C111 C112 115.4(14) . . ? C114 C112 C113 111.8(16) . . ? C114 C112 C111 109.1(16) . . ? C113 C112 C111 107.7(17) . . ? C121 N120 P12 121.4(13) . . ? N120 C121 C122 114.2(18) . . ? C124 C122 C121 117(2) . . ? C124 C122 C123 107(3) . . ? C121 C122 C123 110.5(19) . . ? C131 N130 P13 121.0(12) . . ? N130 C131 C132 112.0(15) . . ? C134 C132 C131 111.5(17) . . ? C134 C132 C133 111.7(19) . . ? C131 C132 C133 106.1(15) . . ? C141 N140 P11 122.1(13) . . ? N140 C141 C142 117.1(17) . . ? C141 C142 C144 113.7(19) . . ? C141 C142 C143 109.3(19) . . ? C144 C142 C143 111.1(19) . . ? C151 N150 P12 118.8(13) . . ? N150 C151 C152 116.2(17) . . ? C151 C152 C153 112.5(19) . . ? C151 C152 C154 108.0(17) . . ? C153 C152 C154 111.0(17) . . ? C161 N160 P13 115.6(12) . . ? C162 C161 N160 112.3(17) . . ? C161 C162 C163 115.4(16) . . ? C161 C162 C164 109.1(17) . . ? C163 C162 C164 108.5(16) . . ? P21 N21 P22 123.2(11) . . ? N21 P21 N210 117.5(9) . . ? N21 P21 N23 115.4(10) . . ? N210 P21 N23 103.8(9) . . ? N21 P21 N240 104.4(8) . . ? N210 P21 N240 101.3(8) . . ? N23 P21 N240 113.9(8) . . ? P23 N22 P22 122.0(10) . . ? N21 P22 N250 110.1(8) . . ? N21 P22 N22 115.1(8) . . ? N250 P22 N22 106.5(9) . . ? N21 P22 N220 107.4(9) . . ? N250 P22 N220 105.4(8) . . ? N22 P22 N220 112.0(8) . . ? N23 P23 N22 116.1(9) . . ? N23 P23 N230 114.8(9) . . ? N22 P23 N230 105.8(8) . . ? N23 P23 N260 106.1(8) . . ? N22 P23 N260 112.7(9) . . ? N230 P23 N260 100.4(9) . . ? P23 N23 P21 123.7(10) . . ? C211 N210 P21 122.4(15) . . ? N210 C211 C212 114.9(17) . . ? C211 C212 C213 117.8(18) . . ? C211 C212 C214 108.2(17) . . ? C213 C212 C214 108.9(18) . . ? C221 N220 P22 119.9(13) . . ? N220 C221 C222 109.7(16) . . ? C223 C222 C224 112(2) . . ? C223 C222 C221 110.9(17) . . ? C224 C222 C221 107.5(17) . . ? C231 N230 P23 118.9(14) . . ? C232 C231 N230 120(3) . . ? C231 C232 C234 131(3) . . ? C231 C232 C233 118(3) . . ? C234 C232 C233 110(3) . . ? C241 N240 P21 121.0(14) . . ? N240 C241 C242 111.0(18) . . ? C244 C242 C241 107.1(18) . . ? C244 C242 C243 112.5(18) . . ? C241 C242 C243 107.1(18) . . ? C251 N250 P22 123.9(14) . . ? N250 C251 C252 114.7(16) . . ? C251 C252 C253 110.8(16) . . ? C251 C252 C254 110.6(16) . . ? C253 C252 C254 110.8(17) . . ? C261 N260 P23 120.5(14) . . ? N260 C261 C262 114.0(17) . . ? C261 C262 C263 117(2) . . ? C261 C262 C264 109(2) . . ? C263 C262 C264 108(2) . . ? P32 N31 P31 122.7(10) . . ? N33 P31 N31 115.4(10) . . ? N33 P31 N340 115.5(9) . . ? N31 P31 N340 103.6(9) . . ? N33 P31 N310 106.1(9) . . ? N31 P31 N310 113.4(9) . . ? N340 P31 N310 102.3(9) . . ? P33 N32 P32 121.3(11) . . ? N31 P32 N32 116.1(9) . . ? N31 P32 N350 114.8(9) . . ? N32 P32 N350 106.0(8) . . ? N31 P32 N320 105.9(8) . . ? N32 P32 N320 112.4(9) . . ? N350 P32 N320 100.8(8) . . ? P33 N33 P31 121.4(12) . . ? N33 P33 N32 117.7(9) . . ? N33 P33 N360 108.0(11) . . ? N32 P33 N360 113.1(10) . . ? N33 P33 N330 108.2(10) . . ? N32 P33 N330 108.5(10) . . ? N360 P33 N330 99.7(10) . . ? C311 N310 P31 122.6(15) . . ? N310 C311 C312 113(2) . . ? C314 C312 C313 111(2) . . ? C314 C312 C311 112(2) . . ? C313 C312 C311 107(2) . . ? C321 N320 P32 116.8(13) . . ? N320 C321 C322 111.3(16) . . ? C324 C322 C323 114(3) . . ? C324 C322 C321 112(2) . . ? C323 C322 C321 106(2) . . ? C331 N330 P33 124.6(18) . . ? C332 C331 N330 114(2) . . ? C331 C332 C333 115(2) . . ? C331 C332 C334 110(2) . . ? C333 C332 C334 110(2) . . ? C341 N340 P31 126.6(16) . . ? N340 C341 C342 113(2) . . ? C341 C342 C343 106(2) . . ? C341 C342 C344 113(2) . . ? C343 C342 C344 112(2) . . ? C351 N350 C355 53(2) . . ? C351 N350 P32 131.3(15) . . ? C355 N350 P32 107(2) . . ? C352 C351 N350 115.2(19) . . ? C351 C352 C354 117(2) . . ? C351 C352 C353 116(2) . . ? C354 C352 C353 102(2) . . ? C356 C355 N350 113(3) . . ? C355 C356 C358 115(3) . . ? C355 C356 C357 118(3) . . ? C358 C356 C357 103(3) . . ? C361 N360 P33 122(2) . . ? N360 C361 C362 115(2) . . ? C363 C362 C364 115(3) . . ? C363 C362 C361 111(3) . . ? C364 C362 C361 105(3) . . ? P42 N41 P41 121.0(12) . . ? N43 P41 N41 115.2(10) . . ? N43 P41 N440 108.9(10) . . ? N41 P41 N440 110.9(11) . . ? N43 P41 N410 111.6(11) . . ? N41 P41 N410 108.0(10) . . ? N440 P41 N410 101.5(10) . . ? P43 N42 P42 117.4(10) . . ? N450 P42 N41 102.7(11) . . ? N450 P42 N420 104.4(11) . . ? N41 P42 N420 110.5(9) . . ? N450 P42 N42 118.2(11) . . ? N41 P42 N42 116.4(10) . . ? N420 P42 N42 104.0(9) . . ? P43 N43 P41 123.1(12) . . ? N43 P43 N430 115.4(9) . . ? N43 P43 N42 118.2(10) . . ? N430 P43 N42 102.5(9) . . ? N43 P43 N460 103.2(9) . . ? N430 P43 N460 102.3(9) . . ? N42 P43 N460 114.6(9) . . ? C411 N410 P41 121.3(19) . . ? N410 C411 C412 116(2) . . ? C413 C412 C414 110(2) . . ? C413 C412 C411 112(2) . . ? C414 C412 C411 107(2) . . ? C421 N420 P42 123.2(14) . . ? N420 C421 C422 113.8(16) . . ? C423 C422 C421 110.9(18) . . ? C423 C422 C424 111(2) . . ? C421 C422 C424 108.4(17) . . ? C431 N430 P43 124.7(16) . . ? N430 C431 C432 119(2) . . ? C433 C432 C431 126(3) . . ? C433 C432 C434 120(3) . . ? C431 C432 C434 112(2) . . ? C441 N440 P41 119(2) . . ? N440 C441 C442 120(3) . . ? C444 C442 C441 117(3) . . ? C444 C442 C443 115(3) . . ? C441 C442 C443 109(3) . . ? C451 N450 P42 132(3) . . ? N450 C451 C452 130(4) . . ? C454 C452 C451 147(4) . . ? C454 C452 C453 111(3) . . ? C451 C452 C453 102(3) . . ? C461 N460 P43 122.0(16) . . ? N460 C461 C462 115(2) . . ? C464 C462 C463 110(2) . . ? C464 C462 C461 114(2) . . ? C463 C462 C461 118(2) . . ? P51 N51 P52 123.6(10) . . ? N51 P51 N540 103.8(8) . . ? N51 P51 N53 116.9(8) . . ? N540 P51 N53 113.3(8) . . ? N51 P51 N510 112.9(8) . . ? N540 P51 N510 104.8(8) . . ? N53 P51 N510 104.6(7) . . ? P53 N52 P52 122.3(11) . . ? N52 P52 N51 116.2(8) . . ? N52 P52 N550 114.8(9) . . ? N51 P52 N550 105.0(8) . . ? N52 P52 N520 102.7(9) . . ? N51 P52 N520 114.0(8) . . ? N550 P52 N520 103.7(8) . . ? P53 N53 P51 120.9(8) . . ? N52 P53 N53 118.0(9) . . ? N52 P53 N530 111.7(8) . . ? N53 P53 N530 105.1(8) . . ? N52 P53 N560 106.3(10) . . ? N53 P53 N560 114.4(8) . . ? N530 P53 N560 99.9(9) . . ? C511 N510 P51 120.9(13) . . ? N510 C511 C512 112.3(16) . . ? C514 C512 C513 109.4(18) . . ? C514 C512 C511 112.4(18) . . ? C513 C512 C511 112.2(19) . . ? C521 N520 P52 120.7(13) . . ? C522 C521 N520 109(2) . . ? C523 C522 C521 122(3) . . ? C523 C522 C524 116(3) . . ? C521 C522 C524 119(3) . . ? C531 N530 P53 117.9(13) . . ? C532 C531 N530 109.2(17) . . ? C531 C532 C533 109.6(18) . . ? C531 C532 C534 106.5(19) . . ? C533 C532 C534 107(2) . . ? C541 N540 P51 122.7(12) . . ? N540 C541 C542 112.8(15) . . ? C544 C542 C543 111.4(17) . . ? C544 C542 C541 110.0(17) . . ? C543 C542 C541 107.7(16) . . ? C551 N550 P52 121.4(14) . . ? C552 C551 N550 116.1(18) . . ? C554 C552 C551 115(2) . . ? C554 C552 C553 106.7(18) . . ? C551 C552 C553 108.5(19) . . ? C561 N560 P53 126.8(15) . . ? N560 C561 C562 115.4(17) . . ? C561 C562 C564 112.1(17) . . ? C561 C562 C563 105.1(18) . . ? C564 C562 C563 109.0(17) . . ? 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 N110 H110 N530 0.88 2.65 3.29(2) 130.2 1_564 N130 H130 N22 0.88 2.60 3.19(2) 124.9 . N140 H140 N53 0.88 2.91 3.50(2) 126.0 1_564 N160 H160 N250 0.88 2.58 3.18(2) 126.2 . N210 H210 N320 0.88 2.71 3.57(2) 167.6 . N220 H220 N13 0.88 2.52 3.14(2) 128.0 . N230 H230 N31 0.88 2.74 3.11(2) 106.5 . N250 H250 N160 0.88 2.72 3.18(2) 113.7 . N340 H340 N260 0.88 2.78 3.65(2) 171.5 . N350 H350 N23 0.88 2.25 3.08(2) 157.6 . N430 H430 N51 0.88 2.22 3.10(2) 178.7 . N440 H440 N32 0.88 2.29 3.01(3) 138.8 . N450 H450 N360 0.88 2.69 3.54(3) 164.4 . N540 H540 N42 0.88 2.16 3.04(2) 171.0 . N550 H550 N420 0.88 2.82 3.52(2) 137.7 . N560 H560 N11 0.88 2.34 3.11(2) 146.4 1_546 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 19.98 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.563 _refine_diff_density_min -0.321 _refine_diff_density_rms 0.082 #===END data_P7 _database_code_CSD 199626 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H36 N9 P3' _chemical_formula_weight 687.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 18.160(4) _cell_length_b 7.1790(10) _cell_length_c 13.001(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.22(3) _cell_angle_gamma 90.00 _cell_volume 1687.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 0.218 _exptl_absorpt_correction_type 'not applied' _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 ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3788 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.1423 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 24.22 _reflns_number_total 2563 _reflns_number_gt 1422 _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^)+(0.0249P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(13) _refine_ls_number_reflns 2563 _refine_ls_number_parameters 227 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0848 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0700 _refine_ls_wR_factor_gt 0.0566 _refine_ls_goodness_of_fit_ref 0.634 _refine_ls_restrained_S_all 0.633 _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 1.0000 0.5321(2) 0.5000 0.0330(4) Uani 1 d S . . P2 P 1.06519(6) 0.19173(15) 0.56691(9) 0.0327(3) Uani 1 d . . . N1 N 1.06150(19) 0.4119(4) 0.5660(3) 0.0272(8) Uani 1 d . . . N2 N 1.0000 0.0843(6) 0.5000 0.0389(14) Uani 1 d S . . N10 N 0.9677(2) 0.6876(6) 0.5784(2) 0.0465(10) Uani 1 d D . . H10 H 0.944(2) 0.756(5) 0.547(3) 0.056 Uiso 1 d D . . N20 N 1.06428(18) 0.1018(5) 0.6839(3) 0.0384(10) Uani 1 d D . . H20 H 1.033(2) 0.039(6) 0.693(4) 0.046 Uiso 1 d D . . N30 N 1.14802(19) 0.1273(5) 0.5359(3) 0.0381(10) Uani 1 d D . . H30 H 1.169(2) 0.057(5) 0.568(3) 0.046 Uiso 1 d D . . C11 C 0.95175(19) 0.6852(6) 0.6823(3) 0.0300(9) Uani 1 d . . . C12 C 0.9917(2) 0.5783(5) 0.7565(3) 0.0330(11) Uani 1 d . . . H12 H 1.0305 0.5000 0.7377 0.040 Uiso 1 calc R . . C13 C 0.9750(2) 0.5858(6) 0.8580(3) 0.0426(12) Uani 1 d . . . H13 H 1.0024 0.5111 0.9083 0.051 Uiso 1 calc R . . C14 C 0.9195(2) 0.6991(7) 0.8880(3) 0.0459(11) Uani 1 d . . . H14 H 0.9078 0.7018 0.9578 0.055 Uiso 1 calc R . . C15 C 0.8814(2) 0.8084(8) 0.8140(3) 0.0503(11) Uani 1 d . . . H15 H 0.8444 0.8913 0.8335 0.060 Uiso 1 calc R . . C16 C 0.8961(2) 0.7993(7) 0.7126(3) 0.0442(10) Uani 1 d . . . H16 H 0.8679 0.8722 0.6624 0.053 Uiso 1 calc R . . C21 C 1.0999(2) 0.1615(6) 0.7790(3) 0.0327(10) Uani 1 d . . . C22 C 1.0770(2) 0.0920(6) 0.8699(4) 0.0489(13) Uani 1 d . . . H22 H 1.0390 0.0007 0.8674 0.059 Uiso 1 calc R . . C23 C 1.1090(3) 0.1542(8) 0.9652(4) 0.0631(15) Uani 1 d . . . H23 H 1.0926 0.1058 1.0272 0.076 Uiso 1 calc R . . C24 C 1.1637(3) 0.2847(9) 0.9694(4) 0.0598(13) Uani 1 d . . . H24 H 1.1858 0.3257 1.0345 0.072 Uiso 1 calc R . . C25 C 1.1871(2) 0.3571(6) 0.8806(4) 0.0471(13) Uani 1 d . . . H25 H 1.2243 0.4505 0.8843 0.057 Uiso 1 calc R . . C26 C 1.15624(19) 0.2938(7) 0.7842(3) 0.0412(10) Uani 1 d . . . H26 H 1.1737 0.3410 0.7226 0.049 Uiso 1 calc R . . C31 C 1.1855(2) 0.1856(7) 0.4513(3) 0.0323(9) Uani 1 d . . . C32 C 1.1481(2) 0.2743(6) 0.3667(3) 0.0367(11) Uani 1 d . . . H32 H 1.0965 0.2960 0.3657 0.044 Uiso 1 calc R . . C33 C 1.1856(2) 0.3314(6) 0.2840(3) 0.0395(11) Uani 1 d . . . H33 H 1.1597 0.3945 0.2276 0.047 Uiso 1 calc R . . C34 C 1.2603(2) 0.2970(7) 0.2831(3) 0.0446(11) Uani 1 d . . . H34 H 1.2861 0.3365 0.2266 0.054 Uiso 1 calc R . . C35 C 1.2970(2) 0.2041(7) 0.3658(4) 0.0474(12) Uani 1 d . . . H35 H 1.3482 0.1776 0.3650 0.057 Uiso 1 calc R . . C36 C 1.2606(2) 0.1494(5) 0.4495(4) 0.0382(12) Uani 1 d . . . H36 H 1.2869 0.0869 0.5059 0.046 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 0.0555(12) 0.0173(9) 0.0262(10) 0.000 0.0036(9) 0.000 P2 0.0445(7) 0.0216(6) 0.0299(6) 0.0008(7) -0.0078(5) 0.0005(7) N1 0.044(2) 0.0112(17) 0.025(2) 0.0037(16) -0.0026(16) 0.0041(16) N2 0.048(3) 0.019(3) 0.043(3) 0.000 -0.034(3) 0.000 N10 0.094(3) 0.021(2) 0.024(2) -0.005(2) 0.0022(18) 0.027(2) N20 0.043(2) 0.034(2) 0.036(2) 0.0124(18) -0.0057(19) -0.0139(17) N30 0.041(2) 0.036(3) 0.036(2) 0.0092(17) -0.0056(17) 0.0146(17) C11 0.048(2) 0.020(2) 0.022(2) -0.004(3) 0.0028(18) -0.001(2) C12 0.042(2) 0.029(3) 0.028(3) 0.000(2) 0.001(2) 0.010(2) C13 0.061(3) 0.040(3) 0.026(3) 0.001(2) 0.000(2) 0.007(2) C14 0.058(3) 0.047(3) 0.034(2) -0.006(3) 0.013(2) -0.006(3) C15 0.050(3) 0.055(3) 0.046(3) -0.008(3) 0.005(2) 0.018(3) C16 0.055(3) 0.035(2) 0.040(3) 0.000(3) -0.009(2) 0.014(3) C21 0.039(2) 0.027(3) 0.032(3) 0.007(2) 0.0005(19) 0.003(2) C22 0.054(3) 0.048(3) 0.045(3) 0.014(3) 0.009(2) -0.006(2) C23 0.089(4) 0.068(4) 0.034(3) 0.017(3) 0.012(3) -0.005(3) C24 0.069(3) 0.071(4) 0.037(3) 0.001(3) -0.009(2) 0.012(3) C25 0.045(3) 0.058(4) 0.036(3) -0.011(3) -0.008(2) -0.005(2) C26 0.040(2) 0.050(3) 0.034(3) 0.004(3) 0.0013(18) -0.005(3) C31 0.047(2) 0.0176(19) 0.031(2) -0.006(3) -0.0033(19) 0.004(3) C32 0.045(2) 0.032(3) 0.031(3) -0.002(2) -0.006(2) 0.009(2) C33 0.053(3) 0.033(3) 0.031(3) -0.004(2) -0.003(2) 0.010(2) C34 0.049(3) 0.035(2) 0.051(3) -0.001(3) 0.007(2) 0.006(3) C35 0.041(2) 0.034(3) 0.067(4) -0.001(3) 0.004(2) 0.003(3) C36 0.039(3) 0.022(3) 0.050(3) -0.001(2) -0.013(2) 0.008(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 N1 1.598(3) 2_756 ? P1 N1 1.598(3) . ? P1 N10 1.655(4) . ? P1 N10 1.655(4) 2_756 ? P2 N1 1.582(3) . ? P2 N2 1.602(2) . ? P2 N20 1.654(4) . ? P2 N30 1.658(4) . ? N2 P2 1.602(2) 2_756 ? N10 C11 1.407(5) . ? N10 H10 0.74(3) . ? N20 C21 1.409(5) . ? N20 H20 0.74(3) . ? N30 C31 1.410(5) . ? N30 H30 0.73(3) . ? C11 C16 1.385(5) . ? C11 C12 1.385(5) . ? C12 C13 1.381(6) . ? C12 H12 0.9500 . ? C13 C14 1.379(6) . ? C13 H13 0.9500 . ? C14 C15 1.378(6) . ? C14 H14 0.9500 . ? C15 C16 1.370(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C21 C22 1.381(6) . ? C21 C26 1.393(5) . ? C22 C23 1.394(6) . ? C22 H22 0.9500 . ? C23 C24 1.363(6) . ? C23 H23 0.9500 . ? C24 C25 1.368(6) . ? C24 H24 0.9500 . ? C25 C26 1.401(6) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C31 C36 1.391(5) . ? C31 C32 1.393(5) . ? C32 C33 1.385(5) . ? C32 H32 0.9500 . ? C33 C34 1.380(5) . ? C33 H33 0.9500 . ? C34 C35 1.384(6) . ? C34 H34 0.9500 . ? C35 C36 1.380(6) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? 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 N1 P1 N1 114.7(2) 2_756 . ? N1 P1 N10 115.15(19) 2_756 . ? N1 P1 N10 107.66(17) . . ? N1 P1 N10 107.66(17) 2_756 2_756 ? N1 P1 N10 115.15(19) . 2_756 ? N10 P1 N10 95.1(3) . 2_756 ? N1 P2 N2 116.6(2) . . ? N1 P2 N20 113.1(2) . . ? N2 P2 N20 104.04(16) . . ? N1 P2 N30 108.4(2) . . ? N2 P2 N30 112.08(17) . . ? N20 P2 N30 101.51(19) . . ? P2 N1 P1 124.8(2) . . ? P2 N2 P2 122.4(3) . 2_756 ? C11 N10 P1 134.3(3) . . ? C11 N10 H10 112(3) . . ? P1 N10 H10 109(4) . . ? C21 N20 P2 130.2(3) . . ? C21 N20 H20 110(4) . . ? P2 N20 H20 117(4) . . ? C31 N30 P2 128.3(3) . . ? C31 N30 H30 112(3) . . ? P2 N30 H30 119(3) . . ? C16 C11 C12 118.6(4) . . ? C16 C11 N10 119.0(4) . . ? C12 C11 N10 122.4(4) . . ? C13 C12 C11 119.8(4) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C14 C13 C12 121.5(4) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C15 C14 C13 118.1(4) . . ? C15 C14 H14 120.9 . . ? C13 C14 H14 120.9 . . ? C16 C15 C14 121.0(4) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C11 120.8(4) . . ? C15 C16 H16 119.6 . . ? C11 C16 H16 119.6 . . ? C22 C21 C26 118.8(4) . . ? C22 C21 N20 119.4(4) . . ? C26 C21 N20 121.8(3) . . ? C21 C22 C23 120.8(4) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C24 C23 C22 119.9(4) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 120.6(4) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C24 C25 C26 120.1(4) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C21 C26 C25 119.8(4) . . ? C21 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C36 C31 C32 118.7(4) . . ? C36 C31 N30 120.1(4) . . ? C32 C31 N30 121.1(3) . . ? C33 C32 C31 120.6(4) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C34 C33 C32 120.4(4) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 118.9(4) . . ? C33 C34 H34 120.5 . . ? C35 C34 H34 120.5 . . ? C36 C35 C34 121.3(4) . . ? C36 C35 H35 119.4 . . ? C34 C35 H35 119.4 . . ? C35 C36 C31 120.0(4) . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? 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 -2.7(3) . . . . ? N20 P2 N1 P1 -123.4(2) . . . . ? N30 P2 N1 P1 124.8(3) . . . . ? N1 P1 N1 P2 1.45(18) 2_756 . . . ? N10 P1 N1 P2 131.0(3) . . . . ? N10 P1 N1 P2 -124.3(3) 2_756 . . . ? N1 P2 N2 P2 1.28(16) . . . 2_756 ? N20 P2 N2 P2 126.64(16) . . . 2_756 ? N30 P2 N2 P2 -124.50(17) . . . 2_756 ? N1 P1 N10 C11 91.6(4) 2_756 . . . ? N1 P1 N10 C11 -37.7(5) . . . . ? N10 P1 N10 C11 -156.2(5) 2_756 . . . ? N1 P2 N20 C21 -40.3(4) . . . . ? N2 P2 N20 C21 -167.8(4) . . . . ? N30 P2 N20 C21 75.7(4) . . . . ? N1 P2 N30 C31 -50.3(4) . . . . ? N2 P2 N30 C31 79.8(4) . . . . ? N20 P2 N30 C31 -169.7(4) . . . . ? P1 N10 C11 C16 -150.4(4) . . . . ? P1 N10 C11 C12 32.2(7) . . . . ? C16 C11 C12 C13 0.7(6) . . . . ? N10 C11 C12 C13 178.1(4) . . . . ? C11 C12 C13 C14 -0.6(6) . . . . ? C12 C13 C14 C15 -1.1(7) . . . . ? C13 C14 C15 C16 2.6(8) . . . . ? C14 C15 C16 C11 -2.5(8) . . . . ? C12 C11 C16 C15 0.8(7) . . . . ? N10 C11 C16 C15 -176.6(4) . . . . ? P2 N20 C21 C22 164.1(4) . . . . ? P2 N20 C21 C26 -13.7(6) . . . . ? C26 C21 C22 C23 0.7(6) . . . . ? N20 C21 C22 C23 -177.2(4) . . . . ? C21 C22 C23 C24 -0.2(7) . . . . ? C22 C23 C24 C25 0.8(8) . . . . ? C23 C24 C25 C26 -1.7(7) . . . . ? C22 C21 C26 C25 -1.6(6) . . . . ? N20 C21 C26 C25 176.2(4) . . . . ? C24 C25 C26 C21 2.2(7) . . . . ? P2 N30 C31 C36 165.8(3) . . . . ? P2 N30 C31 C32 -16.4(6) . . . . ? C36 C31 C32 C33 -2.3(7) . . . . ? N30 C31 C32 C33 179.9(4) . . . . ? C31 C32 C33 C34 1.6(7) . . . . ? C32 C33 C34 C35 0.3(7) . . . . ? C33 C34 C35 C36 -1.4(7) . . . . ? C34 C35 C36 C31 0.7(7) . . . . ? C32 C31 C36 C35 1.2(6) . . . . ? N30 C31 C36 C35 179.0(4) . . . . ? 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 N2 0.74(3) 2.66(4) 3.099(6) 120(4) 1_565 _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 24.22 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.173 _refine_diff_density_min -0.228 _refine_diff_density_rms 0.042 #===END data_P8 _database_code_CSD 199627 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H48 N9 P3' _chemical_formula_weight 771.80 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 7.224(4) _cell_length_b 10.017(6) _cell_length_c 28.331(15) _cell_angle_alpha 90.054(11) _cell_angle_beta 91.593(11) _cell_angle_gamma 107.718(7) _cell_volume 1952.1(19) _cell_formula_units_Z 2 _cell_measurement_temperature 150(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 0.29 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 0.197 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart Apex CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7889 _diffrn_reflns_av_R_equivalents 0.1017 _diffrn_reflns_av_sigmaI/netI 0.1717 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 22.49 _reflns_number_total 5004 _reflns_number_gt 2525 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1101P)^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 5004 _refine_ls_number_parameters 493 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1497 _refine_ls_R_factor_gt 0.0793 _refine_ls_wR_factor_ref 0.2158 _refine_ls_wR_factor_gt 0.1910 _refine_ls_goodness_of_fit_ref 0.915 _refine_ls_restrained_S_all 0.915 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.6789(8) 0.3936(6) 0.2202(2) 0.0252(15) Uani 1 1 d . . . P1 P 0.8536(3) 0.4937(2) 0.25184(7) 0.0232(5) Uani 1 1 d . . . N2 N 0.4297(8) 0.5392(6) 0.24261(19) 0.0241(15) Uani 1 1 d . . . P2 P 0.4695(3) 0.4145(2) 0.21313(7) 0.0233(5) Uani 1 1 d . . . N3 N 0.7931(8) 0.6065(6) 0.28253(19) 0.0232(15) Uani 1 1 d . . . P3 P 0.5869(3) 0.6328(2) 0.28015(7) 0.0240(5) Uani 1 1 d . . . N10 N 0.9666(8) 0.4083(6) 0.28768(19) 0.0263(15) Uani 1 1 d . . . H10 H 1.0776 0.4020 0.2775 0.032 Uiso 1 1 calc R . . C11 C 0.9104(11) 0.3440(8) 0.3323(2) 0.0258(19) Uani 1 1 d . . . C12 C 0.8598(12) 0.4205(8) 0.3691(3) 0.035(2) Uani 1 1 d . . . H12 H 0.8578 0.5139 0.3641 0.042 Uiso 1 1 calc R . . C13 C 0.8129(12) 0.3570(9) 0.4127(3) 0.037(2) Uani 1 1 d . . . H13 H 0.7770 0.4085 0.4371 0.044 Uiso 1 1 calc R . . C14 C 0.8162(12) 0.2226(9) 0.4220(3) 0.039(2) Uani 1 1 d . . . C15 C 0.8726(12) 0.1494(9) 0.3847(3) 0.037(2) Uani 1 1 d . . . H15 H 0.8791 0.0572 0.3897 0.044 Uiso 1 1 calc R . . C16 C 0.9176(11) 0.2111(8) 0.3415(3) 0.033(2) Uani 1 1 d . . . H16 H 0.9550 0.1601 0.3172 0.040 Uiso 1 1 calc R . . C17 C 0.7576(14) 0.1488(9) 0.4681(3) 0.052(3) Uani 1 1 d . . . H17A H 0.8055 0.2153 0.4943 0.078 Uiso 1 1 calc R . . H17B H 0.8135 0.0715 0.4711 0.078 Uiso 1 1 calc R . . H17C H 0.6155 0.1118 0.4687 0.078 Uiso 1 1 calc R . . N20 N 0.3086(10) 0.2636(6) 0.2223(2) 0.0330(17) Uani 1 1 d . . . H20 H 0.2109 0.2387 0.2015 0.040 Uiso 1 1 calc R . . C21 C 0.3044(10) 0.1678(8) 0.2587(2) 0.0206(18) Uani 1 1 d . . . C22 C 0.3981(11) 0.2179(8) 0.3030(3) 0.029(2) Uani 1 1 d . . . H22 H 0.4680 0.3142 0.3075 0.034 Uiso 1 1 calc R . . C23 C 0.3857(11) 0.1246(8) 0.3391(3) 0.030(2) Uani 1 1 d . . . H23 H 0.4514 0.1591 0.3682 0.036 Uiso 1 1 calc R . . C24 C 0.2844(11) -0.0154(8) 0.3357(3) 0.031(2) Uani 1 1 d . . . C25 C 0.1903(11) -0.0623(8) 0.2925(3) 0.033(2) Uani 1 1 d . . . H25 H 0.1186 -0.1585 0.2884 0.039 Uiso 1 1 calc R . . C26 C 0.1998(11) 0.0281(8) 0.2559(3) 0.031(2) Uani 1 1 d . . . H26 H 0.1309 -0.0073 0.2272 0.038 Uiso 1 1 calc R . . C27 C 0.2753(13) -0.1126(9) 0.3761(3) 0.048(2) Uani 1 1 d . . . H27A H 0.4062 -0.0970 0.3899 0.072 Uiso 1 1 calc R . . H27B H 0.2236 -0.2097 0.3648 0.072 Uiso 1 1 calc R . . H27C H 0.1903 -0.0948 0.4001 0.072 Uiso 1 1 calc R . . N30 N 0.4730(9) 0.6015(6) 0.3308(2) 0.0313(16) Uani 1 1 d . . . H30 H 0.3505 0.5498 0.3279 0.038 Uiso 1 1 calc R . . C31 C 0.5369(11) 0.6429(8) 0.3785(3) 0.0274(19) Uani 1 1 d . . . C32 C 0.4112(12) 0.5836(8) 0.4139(3) 0.034(2) Uani 1 1 d . . . H32 H 0.2888 0.5168 0.4065 0.040 Uiso 1 1 calc R . . C33 C 0.4664(12) 0.6231(9) 0.4609(3) 0.038(2) Uani 1 1 d . . . H33 H 0.3781 0.5857 0.4852 0.045 Uiso 1 1 calc R . . C34 C 0.6456(12) 0.7150(9) 0.4724(3) 0.039(2) Uani 1 1 d . . . C35 C 0.7706(11) 0.7713(8) 0.4359(3) 0.032(2) Uani 1 1 d . . . H35 H 0.8947 0.8358 0.4434 0.038 Uiso 1 1 calc R . . C36 C 0.7180(11) 0.7355(8) 0.3890(3) 0.030(2) Uani 1 1 d . . . H36 H 0.8053 0.7740 0.3645 0.036 Uiso 1 1 calc R . . C37 C 0.7051(13) 0.7587(10) 0.5241(3) 0.048(2) Uani 1 1 d . . . H37A H 0.5944 0.7181 0.5443 0.073 Uiso 1 1 calc R . . H37B H 0.7449 0.8611 0.5269 0.073 Uiso 1 1 calc R . . H37C H 0.8137 0.7248 0.5340 0.073 Uiso 1 1 calc R . . N40 N 1.0411(9) 0.5594(6) 0.2177(2) 0.0294(16) Uani 1 1 d . . . H40 H 1.1537 0.5648 0.2316 0.035 Uiso 1 1 calc R . . C41 C 1.0581(11) 0.6091(8) 0.1704(2) 0.0255(19) Uani 1 1 d . . . C42 C 1.2063(11) 0.7229(8) 0.1585(3) 0.030(2) Uani 1 1 d . . . H42 H 1.2923 0.7733 0.1829 0.037 Uiso 1 1 calc R . . C43 C 1.2380(12) 0.7688(9) 0.1130(3) 0.038(2) Uani 1 1 d . . . H43 H 1.3463 0.8474 0.1063 0.045 Uiso 1 1 calc R . . C44 C 1.1075(12) 0.6979(9) 0.0755(3) 0.037(2) Uani 1 1 d . . . C45 C 0.9543(11) 0.5857(8) 0.0879(3) 0.034(2) Uani 1 1 d . . . H45 H 0.8640 0.5384 0.0638 0.040 Uiso 1 1 calc R . . C46 C 0.9239(11) 0.5370(8) 0.1341(3) 0.032(2) Uani 1 1 d . . . H46 H 0.8167 0.4580 0.1412 0.039 Uiso 1 1 calc R . . C47 C 1.1410(13) 0.7455(10) 0.0250(3) 0.058(3) Uani 1 1 d . . . H47A H 1.0270 0.6963 0.0052 0.087 Uiso 1 1 calc R . . H47B H 1.2557 0.7242 0.0135 0.087 Uiso 1 1 calc R . . H47C H 1.1618 0.8467 0.0234 0.087 Uiso 1 1 calc R . . N50 N 0.4193(9) 0.4505(6) 0.15787(19) 0.0276(16) Uani 1 1 d . . . H50 H 0.3935 0.5304 0.1545 0.033 Uiso 1 1 calc R . . C51 C 0.4109(11) 0.3740(8) 0.1151(3) 0.0261(19) Uani 1 1 d . . . C52 C 0.3673(11) 0.4329(8) 0.0739(3) 0.032(2) Uani 1 1 d . . . H52 H 0.3513 0.5235 0.0746 0.039 Uiso 1 1 calc R . . C53 C 0.3467(11) 0.3602(8) 0.0313(3) 0.035(2) Uani 1 1 d . . . H53 H 0.3140 0.4012 0.0033 0.042 Uiso 1 1 calc R . . C54 C 0.3732(11) 0.2281(8) 0.0288(3) 0.031(2) Uani 1 1 d . . . C55 C 0.4255(12) 0.1714(9) 0.0699(3) 0.037(2) Uani 1 1 d . . . H55 H 0.4477 0.0827 0.0689 0.045 Uiso 1 1 calc R . . C56 C 0.4459(11) 0.2457(8) 0.1134(3) 0.034(2) Uani 1 1 d . . . H56 H 0.4836 0.2074 0.1413 0.041 Uiso 1 1 calc R . . C57 C 0.3334(13) 0.1448(9) -0.0177(3) 0.047(2) Uani 1 1 d . . . H57A H 0.1928 0.1069 -0.0237 0.070 Uiso 1 1 calc R . . H57B H 0.3900 0.0675 -0.0156 0.070 Uiso 1 1 calc R . . H57C H 0.3920 0.2066 -0.0436 0.070 Uiso 1 1 calc R . . N60 N 0.6169(8) 0.7983(6) 0.2710(2) 0.0279(16) Uani 1 1 d . . . H60 H 0.5812 0.8422 0.2943 0.033 Uiso 1 1 calc R . . C61 C 0.6901(10) 0.8820(7) 0.2324(2) 0.0196(17) Uani 1 1 d U . . C62 C 0.7033(10) 1.0206(8) 0.2284(3) 0.0241(18) Uani 1 1 d . . . H62 H 0.6596 1.0635 0.2540 0.029 Uiso 1 1 calc R . . C63 C 0.7740(10) 1.1010(8) 0.1908(3) 0.0266(19) Uani 1 1 d . . . H63 H 0.7808 1.1972 0.1908 0.032 Uiso 1 1 calc R . . C64 C 0.8384(10) 1.0417(8) 0.1510(3) 0.0264(19) Uani 1 1 d . . . C65 C 0.8261(10) 0.9029(8) 0.1542(3) 0.0264(19) Uani 1 1 d . . . H65 H 0.8701 0.8606 0.1286 0.032 Uiso 1 1 calc R . . C66 C 0.7540(11) 0.8217(8) 0.1923(3) 0.0270(19) Uani 1 1 d . . . H66 H 0.7461 0.7253 0.1922 0.032 Uiso 1 1 calc R . . C67 C 0.9156(12) 1.1315(8) 0.1095(3) 0.040(2) Uani 1 1 d . . . H67A H 1.0183 1.1008 0.0954 0.059 Uiso 1 1 calc R . . H67B H 0.9689 1.2294 0.1199 0.059 Uiso 1 1 calc R . . H67C H 0.8102 1.1230 0.0861 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.026(4) 0.034(4) 0.017(3) -0.012(3) -0.005(3) 0.011(3) P1 0.0211(11) 0.0332(12) 0.0152(11) -0.0051(9) -0.0047(9) 0.0087(9) N2 0.021(4) 0.034(4) 0.019(4) -0.010(3) -0.009(3) 0.012(3) P2 0.0213(11) 0.0361(13) 0.0129(11) -0.0107(9) -0.0077(9) 0.0101(9) N3 0.026(4) 0.030(4) 0.016(3) -0.008(3) 0.001(3) 0.011(3) P3 0.0231(12) 0.0338(13) 0.0137(11) -0.0084(9) -0.0066(9) 0.0071(9) N10 0.019(3) 0.048(4) 0.016(4) -0.004(3) -0.005(3) 0.017(3) C11 0.023(5) 0.035(5) 0.020(5) 0.002(4) 0.003(4) 0.010(4) C12 0.042(5) 0.036(5) 0.027(5) 0.000(4) 0.002(4) 0.013(4) C13 0.039(5) 0.052(6) 0.020(5) -0.010(4) -0.001(4) 0.015(4) C14 0.037(5) 0.043(6) 0.033(5) 0.011(4) -0.005(4) 0.009(4) C15 0.038(5) 0.041(5) 0.035(6) 0.002(4) 0.004(4) 0.016(4) C16 0.029(5) 0.038(5) 0.031(5) 0.001(4) 0.000(4) 0.007(4) C17 0.068(7) 0.064(6) 0.030(6) 0.006(5) 0.005(5) 0.027(5) N20 0.045(4) 0.038(4) 0.020(4) 0.001(3) 0.010(3) 0.017(3) C21 0.013(4) 0.034(5) 0.014(4) -0.010(4) -0.012(3) 0.007(3) C22 0.026(5) 0.030(5) 0.026(5) -0.009(4) -0.002(4) 0.004(4) C23 0.023(5) 0.045(6) 0.024(5) -0.001(4) 0.000(4) 0.013(4) C24 0.032(5) 0.038(5) 0.023(5) 0.001(4) 0.000(4) 0.012(4) C25 0.027(5) 0.026(5) 0.043(6) 0.000(4) 0.005(4) 0.004(4) C26 0.028(5) 0.029(5) 0.036(5) -0.009(4) 0.007(4) 0.007(4) C27 0.046(6) 0.049(6) 0.053(6) 0.007(5) 0.010(5) 0.018(5) N30 0.025(4) 0.048(4) 0.017(4) -0.012(3) -0.003(3) 0.007(3) C31 0.027(5) 0.030(5) 0.026(5) -0.001(4) -0.004(4) 0.010(4) C32 0.033(5) 0.042(5) 0.018(5) -0.008(4) -0.008(4) 0.000(4) C33 0.031(5) 0.060(6) 0.024(5) -0.001(4) 0.001(4) 0.017(5) C34 0.039(6) 0.057(6) 0.019(5) -0.004(4) -0.005(4) 0.013(5) C35 0.026(5) 0.040(5) 0.023(5) -0.011(4) -0.012(4) 0.002(4) C36 0.031(5) 0.043(5) 0.014(4) -0.010(4) -0.007(4) 0.008(4) C37 0.039(6) 0.086(7) 0.020(5) -0.011(5) -0.007(4) 0.018(5) N40 0.023(4) 0.046(4) 0.019(4) -0.009(3) -0.015(3) 0.010(3) C41 0.028(5) 0.035(5) 0.016(5) 0.007(4) -0.001(4) 0.013(4) C42 0.032(5) 0.034(5) 0.026(5) 0.001(4) 0.002(4) 0.010(4) C43 0.032(5) 0.045(5) 0.032(5) 0.009(4) -0.003(4) 0.004(4) C44 0.036(5) 0.055(6) 0.023(5) 0.005(4) 0.007(4) 0.016(5) C45 0.030(5) 0.056(6) 0.015(5) -0.004(4) -0.007(4) 0.013(4) C46 0.028(5) 0.040(5) 0.025(5) 0.000(4) -0.006(4) 0.007(4) C47 0.040(6) 0.094(8) 0.033(6) 0.015(5) 0.000(5) 0.011(5) N50 0.034(4) 0.039(4) 0.012(3) -0.009(3) -0.013(3) 0.016(3) C51 0.029(5) 0.036(5) 0.016(4) -0.005(4) -0.005(4) 0.014(4) C52 0.044(5) 0.033(5) 0.021(5) -0.008(4) -0.004(4) 0.014(4) C53 0.038(5) 0.049(6) 0.016(5) -0.002(4) -0.009(4) 0.010(4) C54 0.030(5) 0.043(5) 0.016(5) -0.016(4) -0.008(4) 0.009(4) C55 0.040(5) 0.046(5) 0.025(5) -0.007(4) -0.002(4) 0.013(4) C56 0.040(5) 0.041(5) 0.022(5) 0.001(4) -0.005(4) 0.014(4) C57 0.050(6) 0.073(7) 0.021(5) -0.028(4) -0.012(4) 0.026(5) N60 0.016(3) 0.045(4) 0.024(4) -0.006(3) -0.005(3) 0.012(3) C61 0.012(4) 0.025(4) 0.019(4) -0.014(3) -0.011(3) 0.003(3) C62 0.011(4) 0.039(5) 0.021(5) -0.006(4) -0.011(3) 0.008(4) C63 0.024(5) 0.028(5) 0.030(5) -0.005(4) -0.006(4) 0.011(4) C64 0.017(4) 0.037(5) 0.024(5) -0.005(4) -0.009(4) 0.008(4) C65 0.027(5) 0.029(5) 0.020(5) -0.006(4) -0.008(4) 0.005(4) C66 0.027(5) 0.024(4) 0.033(5) -0.005(4) 0.000(4) 0.011(4) C67 0.038(5) 0.038(5) 0.037(5) -0.002(4) -0.009(4) 0.004(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 N1 P2 1.596(6) . ? N1 P1 1.602(6) . ? P1 N3 1.595(6) . ? P1 N40 1.655(6) . ? P1 N10 1.676(6) . ? N2 P2 1.604(6) . ? N2 P3 1.607(6) . ? P2 N20 1.628(6) . ? P2 N50 1.662(6) . ? N3 P3 1.590(6) . ? P3 N60 1.627(6) . ? P3 N30 1.657(6) . ? N10 C11 1.432(9) . ? C11 C16 1.372(10) . ? C11 C12 1.413(10) . ? C12 C13 1.393(10) . ? C13 C14 1.380(11) . ? C14 C15 1.422(11) . ? C14 C17 1.507(11) . ? C15 C16 1.375(10) . ? N20 C21 1.405(9) . ? C21 C26 1.375(10) . ? C21 C22 1.425(10) . ? C22 C23 1.372(10) . ? C23 C24 1.372(10) . ? C24 C25 1.393(11) . ? C24 C27 1.492(10) . ? C25 C26 1.367(10) . ? N30 C31 1.435(9) . ? C31 C36 1.378(10) . ? C31 C32 1.382(10) . ? C32 C33 1.399(10) . ? C33 C34 1.371(11) . ? C34 C35 1.395(10) . ? C34 C37 1.540(11) . ? C35 C36 1.389(10) . ? N40 C41 1.425(9) . ? C41 C42 1.355(10) . ? C41 C46 1.426(10) . ? C42 C43 1.372(10) . ? C43 C44 1.433(11) . ? C44 C45 1.370(10) . ? C44 C47 1.512(11) . ? C45 C46 1.397(10) . ? N50 C51 1.424(9) . ? C51 C52 1.381(10) . ? C51 C56 1.384(10) . ? C52 C53 1.389(10) . ? C53 C54 1.396(11) . ? C54 C55 1.389(10) . ? C54 C57 1.532(10) . ? C55 C56 1.418(10) . ? N60 C61 1.395(9) . ? C61 C62 1.367(9) . ? C61 C66 1.437(10) . ? C62 C63 1.352(9) . ? C63 C64 1.427(10) . ? C64 C65 1.370(10) . ? C64 C67 1.495(10) . ? C65 C66 1.368(10) . ? 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 P2 N1 P1 124.7(4) . . ? N3 P1 N1 114.0(3) . . ? N3 P1 N40 114.9(3) . . ? N1 P1 N40 108.4(3) . . ? N3 P1 N10 108.4(3) . . ? N1 P1 N10 114.3(3) . . ? N40 P1 N10 95.6(3) . . ? P2 N2 P3 121.9(4) . . ? N1 P2 N2 116.8(3) . . ? N1 P2 N20 107.3(3) . . ? N2 P2 N20 112.5(3) . . ? N1 P2 N50 113.6(3) . . ? N2 P2 N50 102.7(3) . . ? N20 P2 N50 103.2(3) . . ? P3 N3 P1 125.5(4) . . ? N3 P3 N2 116.4(3) . . ? N3 P3 N60 109.3(3) . . ? N2 P3 N60 109.9(3) . . ? N3 P3 N30 113.0(3) . . ? N2 P3 N30 103.5(3) . . ? N60 P3 N30 103.9(3) . . ? C11 N10 P1 130.0(5) . . ? C16 C11 C12 118.6(7) . . ? C16 C11 N10 121.1(7) . . ? C12 C11 N10 120.2(7) . . ? C13 C12 C11 119.0(7) . . ? C14 C13 C12 122.9(8) . . ? C13 C14 C15 116.8(7) . . ? C13 C14 C17 124.1(8) . . ? C15 C14 C17 119.0(7) . . ? C16 C15 C14 120.5(8) . . ? C11 C16 C15 122.2(8) . . ? C21 N20 P2 128.8(6) . . ? C26 C21 N20 123.8(7) . . ? C26 C21 C22 116.7(7) . . ? N20 C21 C22 119.3(6) . . ? C23 C22 C21 118.9(7) . . ? C22 C23 C24 124.0(8) . . ? C23 C24 C25 116.4(7) . . ? C23 C24 C27 122.0(8) . . ? C25 C24 C27 121.6(7) . . ? C26 C25 C24 120.9(7) . . ? C25 C26 C21 123.0(8) . . ? C31 N30 P3 132.0(5) . . ? C36 C31 C32 120.9(7) . . ? C36 C31 N30 121.7(7) . . ? C32 C31 N30 117.3(6) . . ? C31 C32 C33 119.1(7) . . ? C34 C33 C32 121.3(7) . . ? C33 C34 C35 118.2(7) . . ? C33 C34 C37 121.0(7) . . ? C35 C34 C37 120.8(7) . . ? C36 C35 C34 121.6(7) . . ? C31 C36 C35 118.8(7) . . ? C41 N40 P1 133.3(5) . . ? C42 C41 N40 120.7(7) . . ? C42 C41 C46 118.5(6) . . ? N40 C41 C46 120.7(7) . . ? C41 C42 C43 123.1(8) . . ? C42 C43 C44 119.9(8) . . ? C45 C44 C43 116.7(7) . . ? C45 C44 C47 122.4(8) . . ? C43 C44 C47 120.8(7) . . ? C44 C45 C46 123.4(8) . . ? C45 C46 C41 118.3(7) . . ? C51 N50 P2 130.9(5) . . ? C52 C51 C56 119.5(7) . . ? C52 C51 N50 117.5(7) . . ? C56 C51 N50 123.0(7) . . ? C51 C52 C53 120.3(7) . . ? C52 C53 C54 121.3(7) . . ? C55 C54 C53 118.5(7) . . ? C55 C54 C57 121.1(7) . . ? C53 C54 C57 120.3(7) . . ? C54 C55 C56 120.1(8) . . ? C51 C56 C55 120.2(7) . . ? C61 N60 P3 130.6(5) . . ? C62 C61 N60 125.1(7) . . ? C62 C61 C66 115.2(7) . . ? N60 C61 C66 119.6(6) . . ? C63 C62 C61 124.8(7) . . ? C62 C63 C64 120.2(7) . . ? C65 C64 C63 116.0(7) . . ? C65 C64 C67 124.2(7) . . ? C63 C64 C67 119.7(7) . . ? C66 C65 C64 123.6(7) . . ? C65 C66 C61 120.1(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 N40 H40 N2 0.88 2.10 2.942(8) 159.5 1_655 N10 H10 N2 0.88 2.71 3.481(8) 146.8 1_655 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.940 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.115 #===END data_P9 _database_code_CSD 199628 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H48 N9 P3' _chemical_formula_weight 483.56 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 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 42.210(5) _cell_length_b 11.3419(12) _cell_length_c 23.092(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.105(2) _cell_angle_gamma 90.00 _cell_volume 11053(2) _cell_formula_units_Z 16 _cell_measurement_temperature 150(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 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.162 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4224 _exptl_absorpt_coefficient_mu 0.238 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart Apex CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28263 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -50 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.03 _reflns_number_total 9739 _reflns_number_gt 5828 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1223P)^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 9739 _refine_ls_number_parameters 773 _refine_ls_number_restraints 1694 _refine_ls_R_factor_all 0.1002 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.2038 _refine_ls_wR_factor_gt 0.1804 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.194 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P11 P 0.04657(2) 0.55408(10) 0.29227(5) 0.0563(3) Uani 1 1 d . . . N11 N 0.07981(7) 0.5466(3) 0.32559(14) 0.0578(9) Uani 1 1 d . . . P12 P 0.11249(2) 0.51908(11) 0.29323(5) 0.0605(4) Uani 1 1 d . . . N12 N 0.10984(7) 0.5115(3) 0.22434(15) 0.0619(10) Uani 1 1 d . . . P13 P 0.07719(2) 0.47674(10) 0.19233(5) 0.0551(3) Uani 1 1 d . B . N13 N 0.04600(7) 0.5082(3) 0.22685(15) 0.0625(10) Uani 1 1 d . . . N110 N 0.02071(8) 0.4900(3) 0.33411(17) 0.0632(10) Uani 1 1 d D . . H110 H 0.0023(7) 0.496(4) 0.3181(19) 0.076 Uiso 1 1 d D . . C111 C 0.02671(10) 0.3832(4) 0.36734(18) 0.0631(11) Uani 1 1 d DU . . H11A H 0.0498 0.3690 0.3699 0.076 Uiso 1 1 calc R . . H11B H 0.0168 0.3154 0.3469 0.076 Uiso 1 1 calc R . . C112 C 0.01373(12) 0.3908(4) 0.4279(2) 0.0767(13) Uani 1 1 d DU . . H11C H 0.0248 0.4547 0.4494 0.092 Uiso 1 1 calc R . . H11D H -0.0091 0.4109 0.4255 0.092 Uiso 1 1 calc R . . C113 C 0.01785(14) 0.2767(5) 0.4607(2) 0.1010(18) Uani 1 1 d DU . . H11E H 0.0090 0.2851 0.4994 0.152 Uiso 1 1 calc R . . H11F H 0.0404 0.2577 0.4642 0.152 Uiso 1 1 calc R . . H11G H 0.0068 0.2133 0.4398 0.152 Uiso 1 1 calc R . . N120 N 0.12518(8) 0.3921(3) 0.32090(17) 0.0670(10) Uani 1 1 d D . . H120 H 0.1206(11) 0.393(4) 0.3559(10) 0.080 Uiso 1 1 d D . . C121 C 0.15721(11) 0.3515(5) 0.3092(2) 0.0876(15) Uani 1 1 d DU . . H12A H 0.1719 0.3833 0.3392 0.105 Uiso 1 1 calc R . . H12B H 0.1638 0.3834 0.2713 0.105 Uiso 1 1 calc R . . C122 C 0.16011(12) 0.2204(5) 0.3080(3) 0.0988(17) Uani 1 1 d DU . . H12C H 0.1473 0.1889 0.2752 0.119 Uiso 1 1 calc R . . H12D H 0.1516 0.1875 0.3443 0.119 Uiso 1 1 calc R . . C123 C 0.19414(14) 0.1814(7) 0.3019(3) 0.132(3) Uani 1 1 d DU . . H12E H 0.1951 0.0951 0.3007 0.198 Uiso 1 1 calc R . . H12F H 0.2068 0.2102 0.3350 0.198 Uiso 1 1 calc R . . H12G H 0.2026 0.2135 0.2660 0.198 Uiso 1 1 calc R . . N130 N 0.08078(8) 0.3354(3) 0.17724(17) 0.0692(11) Uani 1 1 d D . . H130 H 0.1003 0.3094 0.1733 0.083 Uiso 1 1 calc RD A 1 C131 C 0.05678(17) 0.2519(7) 0.1700(3) 0.072(2) Uani 0.590(6) 1 d PDU B 1 H13A H 0.0663 0.1820 0.1514 0.086 Uiso 0.590(6) 1 calc PR B 1 H13B H 0.0411 0.2849 0.1419 0.086 Uiso 0.590(6) 1 calc PR B 1 C132 C 0.0388(2) 0.2088(8) 0.2209(4) 0.074(2) Uani 0.590(6) 1 d PDU B 1 H13C H 0.0214 0.1574 0.2067 0.088 Uiso 0.590(6) 1 calc PR B 1 H13D H 0.0291 0.2775 0.2402 0.088 Uiso 0.590(6) 1 calc PR B 1 C133 C 0.0586(3) 0.1402(11) 0.2661(5) 0.101(3) Uani 0.590(6) 1 d PDU B 1 H13E H 0.0451 0.1171 0.2983 0.151 Uiso 0.590(6) 1 calc PR B 1 H13F H 0.0759 0.1902 0.2807 0.151 Uiso 0.590(6) 1 calc PR B 1 H13G H 0.0674 0.0694 0.2481 0.151 Uiso 0.590(6) 1 calc PR B 1 C331 C 0.0855(2) 0.2405(9) 0.2118(5) 0.067(3) Uani 0.410(6) 1 d PDU B 2 H33A H 0.1015 0.2626 0.2418 0.080 Uiso 0.410(6) 1 calc PR B 2 H33B H 0.0951 0.1777 0.1880 0.080 Uiso 0.410(6) 1 calc PR B 2 C332 C 0.0575(4) 0.1875(13) 0.2423(6) 0.078(3) Uani 0.410(6) 1 d PDU B 2 H33C H 0.0449 0.2503 0.2607 0.094 Uiso 0.410(6) 1 calc PR B 2 H33D H 0.0650 0.1321 0.2728 0.094 Uiso 0.410(6) 1 calc PR B 2 C333 C 0.0376(3) 0.1228(14) 0.1975(7) 0.106(5) Uani 0.410(6) 1 d PDU B 2 H33E H 0.0191 0.0883 0.2160 0.159 Uiso 0.410(6) 1 calc PR B 2 H33F H 0.0502 0.0601 0.1800 0.159 Uiso 0.410(6) 1 calc PR B 2 H33G H 0.0305 0.1782 0.1673 0.159 Uiso 0.410(6) 1 calc PR B 2 N140 N 0.03257(9) 0.6903(3) 0.28808(16) 0.0637(10) Uani 1 1 d D F . H140 H 0.034(2) 0.736(8) 0.260(3) 0.076 Uiso 0.50 1 d PD C 1 H340 H 0.0464(15) 0.723(8) 0.268(4) 0.076 Uiso 0.50 1 d PD D 2 C141 C 0.03092(11) 0.7631(4) 0.34082(19) 0.0700(12) Uani 1 1 d DU . . H14A H 0.0503 0.7515 0.3649 0.084 Uiso 1 1 calc R E 1 H14B H 0.0125 0.7389 0.3638 0.084 Uiso 1 1 calc R E 1 C142 C 0.0279(4) 0.8893(8) 0.3243(5) 0.077(3) Uani 0.541(19) 1 d PDU F 1 H14C H 0.0082 0.8994 0.3008 0.092 Uiso 0.541(19) 1 calc PR F 1 H14D H 0.0459 0.9105 0.2995 0.092 Uiso 0.541(19) 1 calc PR F 1 C143 C 0.0271(4) 0.9750(12) 0.3753(7) 0.102(4) Uani 0.541(19) 1 d PDU F 1 H14E H 0.0255 1.0559 0.3608 0.153 Uiso 0.541(19) 1 calc PR F 1 H14F H 0.0466 0.9666 0.3987 0.153 Uiso 0.541(19) 1 calc PR F 1 H14G H 0.0088 0.9574 0.3992 0.153 Uiso 0.541(19) 1 calc PR F 1 C342 C 0.0121(4) 0.8732(11) 0.3353(6) 0.082(3) Uani 0.459(19) 1 d PDU F 2 H34A H -0.0102 0.8528 0.3251 0.098 Uiso 0.459(19) 1 calc PR F 2 H34B H 0.0205 0.9214 0.3034 0.098 Uiso 0.459(19) 1 calc PR F 2 C343 C 0.0127(5) 0.9469(14) 0.3918(7) 0.101(5) Uani 0.459(19) 1 d PDU F 2 H34C H 0.0003 1.0190 0.3859 0.152 Uiso 0.459(19) 1 calc PR F 2 H34D H 0.0347 0.9677 0.4019 0.152 Uiso 0.459(19) 1 calc PR F 2 H34E H 0.0037 0.9006 0.4232 0.152 Uiso 0.459(19) 1 calc PR F 2 N150 N 0.14080(8) 0.6132(4) 0.30846(17) 0.0714(11) Uani 1 1 d D H . H150 H 0.1442(11) 0.617(4) 0.3447(10) 0.086 Uiso 1 1 d D . . C151 C 0.14284(11) 0.7274(4) 0.2838(2) 0.0821(14) Uani 1 1 d DU . . H15A H 0.1365 0.7240 0.2423 0.099 Uiso 1 1 calc R G 1 H15B H 0.1650 0.7557 0.2864 0.099 Uiso 1 1 calc R G 1 C152 C 0.1215(2) 0.8124(7) 0.3152(4) 0.084(2) Uani 0.709(9) 1 d PDU H 1 H15C H 0.0992 0.7867 0.3114 0.100 Uiso 0.709(9) 1 calc PR H 1 H15D H 0.1274 0.8151 0.3568 0.100 Uiso 0.709(9) 1 calc PR H 1 C153 C 0.1256(2) 0.9319(6) 0.2883(4) 0.103(3) Uani 0.709(9) 1 d PDU H 1 H15E H 0.1121 0.9891 0.3080 0.154 Uiso 0.709(9) 1 calc PR H 1 H15F H 0.1194 0.9284 0.2472 0.154 Uiso 0.709(9) 1 calc PR H 1 H15G H 0.1478 0.9562 0.2921 0.154 Uiso 0.709(9) 1 calc PR H 1 C352 C 0.1188(5) 0.8266(18) 0.2869(9) 0.084(4) Uani 0.291(9) 1 d PDU H 2 H35A H 0.1219 0.8833 0.2549 0.100 Uiso 0.291(9) 1 calc PR H 2 H35B H 0.0970 0.7946 0.2836 0.100 Uiso 0.291(9) 1 calc PR H 2 C353 C 0.1236(4) 0.8874(17) 0.3446(8) 0.086(5) Uani 0.291(9) 1 d PDU H 2 H35C H 0.1082 0.9517 0.3481 0.129 Uiso 0.291(9) 1 calc PR H 2 H35D H 0.1451 0.9194 0.3473 0.129 Uiso 0.291(9) 1 calc PR H 2 H35E H 0.1205 0.8305 0.3760 0.129 Uiso 0.291(9) 1 calc PR H 2 N160 N 0.07238(8) 0.5297(3) 0.12750(16) 0.0665(10) Uani 1 1 d D . . H160 H 0.0854(9) 0.506(4) 0.1037(16) 0.080 Uiso 1 1 d D . . C161 C 0.0609(2) 0.6497(6) 0.1210(4) 0.079(2) Uani 0.750(9) 1 d PDU B 1 H16A H 0.0437 0.6630 0.1487 0.095 Uiso 0.750(9) 1 calc PR B 1 H16B H 0.0518 0.6594 0.0814 0.095 Uiso 0.750(9) 1 calc PR B 1 C162 C 0.0862(2) 0.7419(7) 0.1309(5) 0.111(3) Uani 0.750(9) 1 d PDU B 1 H16C H 0.1032 0.7326 0.1023 0.133 Uiso 0.750(9) 1 calc PR B 1 H16D H 0.0957 0.7337 0.1702 0.133 Uiso 0.750(9) 1 calc PR B 1 C163 C 0.0706(3) 0.8626(8) 0.1241(5) 0.145(4) Uani 0.750(9) 1 d PDU B 1 H16E H 0.0866 0.9244 0.1300 0.217 Uiso 0.750(9) 1 calc PR B 1 H16F H 0.0540 0.8712 0.1529 0.217 Uiso 0.750(9) 1 calc PR B 1 H16G H 0.0613 0.8696 0.0851 0.217 Uiso 0.750(9) 1 calc PR B 1 C361 C 0.0541(6) 0.6251(16) 0.1002(13) 0.082(5) Uani 0.250(9) 1 d PDU B 2 H36A H 0.0357 0.6417 0.1247 0.099 Uiso 0.250(9) 1 calc PR B 2 H36B H 0.0457 0.5957 0.0625 0.099 Uiso 0.250(9) 1 calc PR B 2 C362 C 0.0707(6) 0.7388(16) 0.0895(9) 0.098(4) Uani 0.250(9) 1 d PDU B 2 H36C H 0.0564 0.7942 0.0685 0.117 Uiso 0.250(9) 1 calc PR B 2 H36D H 0.0896 0.7255 0.0657 0.117 Uiso 0.250(9) 1 calc PR B 2 C363 C 0.0802(8) 0.789(3) 0.1479(12) 0.113(7) Uani 0.250(9) 1 d PDU B 2 H36E H 0.0908 0.8652 0.1425 0.170 Uiso 0.250(9) 1 calc PR B 2 H36F H 0.0948 0.7345 0.1678 0.170 Uiso 0.250(9) 1 calc PR B 2 H36G H 0.0613 0.8003 0.1712 0.170 Uiso 0.250(9) 1 calc PR B 2 P21 P 0.31633(3) -0.09824(12) 0.52918(5) 0.0654(4) Uani 1 1 d . I . N21 N 0.31393(8) -0.0984(4) 0.46044(15) 0.0712(11) Uani 1 1 d . . . P22 P 0.34451(3) -0.08170(12) 0.42185(5) 0.0642(4) Uani 1 1 d . J . N22 N 0.37454(8) -0.0240(3) 0.45368(15) 0.0622(9) Uani 1 1 d . . . P23 P 0.37825(3) -0.00954(11) 0.52197(5) 0.0638(4) Uani 1 1 d . K . N23 N 0.34752(8) -0.0443(3) 0.55796(15) 0.0668(10) Uani 1 1 d . . . N210 N 0.28388(10) -0.0343(4) 0.5495(2) 0.0885(14) Uani 1 1 d D . . H210 H 0.2741(13) 0.008(5) 0.522(2) 0.106 Uiso 1 1 d D . . C211 C 0.2752(2) -0.0206(12) 0.6050(4) 0.099(3) Uani 0.50 1 d PDU I 1 H21A H 0.2901 0.0366 0.6231 0.118 Uiso 0.50 1 calc PR I 1 H21B H 0.2789 -0.0971 0.6248 0.118 Uiso 0.50 1 calc PR I 1 C212 C 0.2441(3) 0.0166(15) 0.6182(5) 0.138(4) Uani 0.50 1 d PDU I 1 H21C H 0.2290 -0.0448 0.6047 0.165 Uiso 0.50 1 calc PR I 1 H21D H 0.2394 0.0894 0.5960 0.165 Uiso 0.50 1 calc PR I 1 C213 C 0.2383(4) 0.0407(16) 0.6821(6) 0.159(6) Uani 0.50 1 d PDU I 1 H21E H 0.2162 0.0646 0.6870 0.239 Uiso 0.50 1 calc PR I 1 H21F H 0.2524 0.1040 0.6956 0.239 Uiso 0.50 1 calc PR I 1 H21G H 0.2426 -0.0310 0.7046 0.239 Uiso 0.50 1 calc PR I 1 C411 C 0.2771(3) 0.0920(10) 0.5318(6) 0.110(4) Uani 0.50 1 d PDU I -2 H41A H 0.2898 0.1458 0.5568 0.132 Uiso 0.50 1 calc PR I -2 H41B H 0.2837 0.1039 0.4913 0.132 Uiso 0.50 1 calc PR I -2 C412 C 0.2439(3) 0.1216(11) 0.5365(6) 0.121(4) Uani 0.50 1 d PDU I -2 H41C H 0.2381 0.1223 0.5778 0.146 Uiso 0.50 1 calc PR I -2 H41D H 0.2309 0.0603 0.5167 0.146 Uiso 0.50 1 calc PR I -2 C413 C 0.2361(3) 0.2407(12) 0.5100(7) 0.142(5) Uani 0.50 1 d PDU I -2 H41E H 0.2136 0.2581 0.5150 0.213 Uiso 0.50 1 calc PR I -2 H41F H 0.2408 0.2393 0.4686 0.213 Uiso 0.50 1 calc PR I -2 H41G H 0.2490 0.3017 0.5292 0.213 Uiso 0.50 1 calc PR I -2 N220 N 0.33332(9) -0.0086(4) 0.36312(18) 0.0830(13) Uani 1 1 d D . . H220 H 0.3480(10) -0.006(4) 0.3371(18) 0.100 Uiso 1 1 d D . . C221 C 0.3143(4) 0.0976(13) 0.3626(8) 0.094(3) Uani 0.593(9) 1 d PDU J 1 H22A H 0.3285 0.1669 0.3664 0.112 Uiso 0.593(9) 1 calc PR J 1 H22B H 0.3003 0.0970 0.3965 0.112 Uiso 0.593(9) 1 calc PR J 1 C222 C 0.2941(2) 0.1105(11) 0.3077(5) 0.089(3) Uani 0.593(9) 1 d PDU J 1 H22C H 0.3072 0.0984 0.2732 0.106 Uiso 0.593(9) 1 calc PR J 1 H22D H 0.2769 0.0510 0.3072 0.106 Uiso 0.593(9) 1 calc PR J 1 C223 C 0.2803(3) 0.2320(12) 0.3072(6) 0.156(5) Uani 0.593(9) 1 d PDU J 1 H22E H 0.2676 0.2433 0.2716 0.234 Uiso 0.593(9) 1 calc PR J 1 H22F H 0.2975 0.2902 0.3086 0.234 Uiso 0.593(9) 1 calc PR J 1 H22G H 0.2669 0.2423 0.3409 0.234 Uiso 0.593(9) 1 calc PR J 1 C421 C 0.3204(5) 0.1112(16) 0.3720(13) 0.098(4) Uani 0.407(9) 1 d PDU J 2 H42A H 0.3328 0.1685 0.3494 0.117 Uiso 0.407(9) 1 calc PR J 2 H42B H 0.3226 0.1325 0.4134 0.117 Uiso 0.407(9) 1 calc PR J 2 C422 C 0.2859(3) 0.1190(14) 0.3534(7) 0.106(3) Uani 0.407(9) 1 d PDU J 2 H42C H 0.2729 0.0714 0.3801 0.128 Uiso 0.407(9) 1 calc PR J 2 H42D H 0.2787 0.2019 0.3560 0.128 Uiso 0.407(9) 1 calc PR J 2 C423 C 0.2808(5) 0.075(2) 0.2922(8) 0.133(6) Uani 0.407(9) 1 d PDU J 2 H42E H 0.2582 0.0815 0.2814 0.199 Uiso 0.407(9) 1 calc PR J 2 H42F H 0.2874 -0.0074 0.2897 0.199 Uiso 0.407(9) 1 calc PR J 2 H42G H 0.2933 0.1230 0.2657 0.199 Uiso 0.407(9) 1 calc PR J 2 N230 N 0.38699(10) 0.1275(4) 0.54177(19) 0.0835(13) Uani 1 1 d D . . H230 H 0.4055(8) 0.147(5) 0.529(2) 0.100 Uiso 1 1 d D . . C231 C 0.3621(3) 0.2167(9) 0.5257(8) 0.087(3) Uani 0.66(2) 1 d PDU K 1 H23A H 0.3431 0.2037 0.5495 0.105 Uiso 0.66(2) 1 calc PR K 1 H23B H 0.3557 0.2060 0.4845 0.105 Uiso 0.66(2) 1 calc PR K 1 C232 C 0.3741(3) 0.3427(8) 0.5349(6) 0.095(3) Uani 0.66(2) 1 d PDU K 1 H23C H 0.3910 0.3595 0.5069 0.114 Uiso 0.66(2) 1 calc PR K 1 H23D H 0.3834 0.3500 0.5744 0.114 Uiso 0.66(2) 1 calc PR K 1 C233 C 0.3475(4) 0.4335(10) 0.5269(7) 0.130(5) Uani 0.66(2) 1 d PDU K 1 H23E H 0.3561 0.5130 0.5324 0.195 Uiso 0.66(2) 1 calc PR K 1 H23F H 0.3311 0.4190 0.5555 0.195 Uiso 0.66(2) 1 calc PR K 1 H23G H 0.3382 0.4265 0.4878 0.195 Uiso 0.66(2) 1 calc PR K 1 C431 C 0.3675(7) 0.2318(17) 0.5374(18) 0.096(4) Uani 0.34(2) 1 d PDU K 2 H43A H 0.3477 0.2199 0.5590 0.115 Uiso 0.34(2) 1 calc PR K 2 H43B H 0.3617 0.2470 0.4963 0.115 Uiso 0.34(2) 1 calc PR K 2 C432 C 0.3859(6) 0.3385(16) 0.5628(12) 0.097(4) Uani 0.34(2) 1 d PDU K 2 H43C H 0.3919 0.3247 0.6039 0.116 Uiso 0.34(2) 1 calc PR K 2 H43D H 0.4053 0.3541 0.5406 0.116 Uiso 0.34(2) 1 calc PR K 2 C433 C 0.3627(7) 0.4395(17) 0.5570(13) 0.120(6) Uani 0.34(2) 1 d PDU K 2 H43E H 0.3720 0.5105 0.5745 0.181 Uiso 0.34(2) 1 calc PR K 2 H43F H 0.3431 0.4194 0.5769 0.181 Uiso 0.34(2) 1 calc PR K 2 H43G H 0.3580 0.4540 0.5159 0.181 Uiso 0.34(2) 1 calc PR K 2 N240 N 0.31246(9) -0.2275(4) 0.56046(17) 0.0752(11) Uani 1 1 d D . . H240 H 0.3305(8) -0.261(4) 0.568(2) 0.090 Uiso 1 1 d D . . C241 C 0.28748(16) -0.3100(6) 0.5449(3) 0.121(2) Uani 1 1 d DU I . H24A H 0.2948 -0.3623 0.5137 0.145 Uiso 1 1 calc R . . H24B H 0.2688 -0.2658 0.5300 0.145 Uiso 1 1 calc R . . C242 C 0.2779(2) -0.3845(8) 0.5965(3) 0.157(3) Uani 1 1 d DU . . H24C H 0.2615 -0.4414 0.5830 0.189 Uiso 1 1 calc R I . H24D H 0.2965 -0.4305 0.6098 0.189 Uiso 1 1 calc R . . C243 C 0.26512(19) -0.3189(9) 0.6477(4) 0.188(4) Uani 1 1 d DU I . H24E H 0.2596 -0.3752 0.6780 0.281 Uiso 1 1 calc R . . H24F H 0.2462 -0.2744 0.6356 0.281 Uiso 1 1 calc R . . H24G H 0.2813 -0.2642 0.6627 0.281 Uiso 1 1 calc R . . N250 N 0.35680(8) -0.2088(4) 0.39726(16) 0.0672(10) Uani 1 1 d D . . H250 H 0.3748(7) -0.195(4) 0.3844(19) 0.081 Uiso 1 1 d D . . C251 C 0.33511(14) -0.2846(5) 0.3635(3) 0.1051(18) Uani 1 1 d DU J . H25A H 0.3299 -0.2458 0.3261 0.126 Uiso 1 1 calc R L 1 H25B H 0.3152 -0.2947 0.3848 0.126 Uiso 1 1 calc R L 1 C252 C 0.3498(5) -0.4074(11) 0.3516(7) 0.117(4) Uani 0.410(11) 1 d PDU J 1 H25C H 0.3375 -0.4458 0.3199 0.140 Uiso 0.410(11) 1 calc PR J 1 H25D H 0.3717 -0.3965 0.3383 0.140 Uiso 0.410(11) 1 calc PR J 1 C253 C 0.3504(5) -0.4859(14) 0.4021(7) 0.128(6) Uani 0.410(11) 1 d PDU J 1 H25E H 0.3597 -0.5618 0.3913 0.192 Uiso 0.410(11) 1 calc PR J 1 H25F H 0.3287 -0.4983 0.4153 0.192 Uiso 0.410(11) 1 calc PR J 1 H25G H 0.3631 -0.4501 0.4333 0.192 Uiso 0.410(11) 1 calc PR J 1 C452 C 0.3410(4) -0.4088(10) 0.3775(6) 0.132(4) Uani 0.590(11) 1 d PDU J 2 H45A H 0.3636 -0.4260 0.3704 0.159 Uiso 0.590(11) 1 calc PR J 2 H45B H 0.3375 -0.4203 0.4194 0.159 Uiso 0.590(11) 1 calc PR J 2 C453 C 0.3219(4) -0.4942(11) 0.3458(6) 0.168(6) Uani 0.590(11) 1 d PDU J 2 H45C H 0.3286 -0.5741 0.3567 0.253 Uiso 0.590(11) 1 calc PR J 2 H45D H 0.3247 -0.4831 0.3041 0.253 Uiso 0.590(11) 1 calc PR J 2 H45E H 0.2996 -0.4832 0.3550 0.253 Uiso 0.590(11) 1 calc PR J 2 N260 N 0.41084(9) -0.0754(4) 0.54302(16) 0.0695(11) Uani 1 1 d D . . H260 H 0.4133(11) -0.085(4) 0.5800(12) 0.083 Uiso 1 1 d D . . C261 C 0.42649(12) -0.1693(4) 0.5100(2) 0.0829(14) Uani 1 1 d DU K . H26A H 0.4263 -0.1481 0.4684 0.100 Uiso 1 1 calc R . . H26B H 0.4489 -0.1760 0.5232 0.100 Uiso 1 1 calc R . . C262 C 0.41066(12) -0.2829(5) 0.5174(2) 0.0936(16) Uani 1 1 d DU . . H26C H 0.3883 -0.2774 0.5038 0.112 Uiso 1 1 calc R K . H26D H 0.4109 -0.3052 0.5589 0.112 Uiso 1 1 calc R . . C263 C 0.42903(16) -0.3798(5) 0.4806(3) 0.113(2) Uani 1 1 d DU K . H26E H 0.4188 -0.4567 0.4852 0.169 Uiso 1 1 calc R . . H26F H 0.4511 -0.3848 0.4944 0.169 Uiso 1 1 calc R . . H26G H 0.4285 -0.3574 0.4396 0.169 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P11 0.0422(6) 0.0601(7) 0.0674(7) -0.0211(5) 0.0248(5) -0.0087(5) N11 0.0452(18) 0.066(2) 0.063(2) -0.0231(17) 0.0234(16) -0.0101(16) P12 0.0406(6) 0.0763(8) 0.0655(7) -0.0290(6) 0.0230(5) -0.0133(5) N12 0.0398(18) 0.082(3) 0.065(2) -0.0265(18) 0.0207(16) -0.0135(16) P13 0.0411(6) 0.0628(7) 0.0620(7) -0.0202(5) 0.0192(5) -0.0075(5) N13 0.0395(18) 0.078(2) 0.070(2) -0.0286(19) 0.0189(16) -0.0087(16) N110 0.0433(19) 0.066(2) 0.081(3) -0.013(2) 0.0270(18) -0.0070(18) C111 0.052(2) 0.065(3) 0.073(3) -0.020(2) 0.022(2) -0.012(2) C112 0.073(3) 0.081(3) 0.078(3) -0.017(3) 0.028(2) -0.024(2) C113 0.112(4) 0.100(4) 0.092(4) -0.006(3) 0.036(3) -0.039(3) N120 0.050(2) 0.074(3) 0.078(3) -0.023(2) 0.0236(19) 0.0029(18) C121 0.063(3) 0.113(4) 0.088(3) -0.031(3) 0.027(2) 0.002(3) C122 0.087(4) 0.108(4) 0.103(4) -0.027(3) 0.033(3) 0.018(3) C123 0.098(4) 0.175(7) 0.122(5) -0.022(5) 0.014(4) 0.055(4) N130 0.047(2) 0.064(2) 0.098(3) -0.022(2) 0.0304(19) -0.0046(17) C131 0.063(4) 0.076(5) 0.076(5) -0.030(4) 0.005(4) -0.007(4) C132 0.070(5) 0.071(5) 0.080(5) -0.026(4) 0.008(4) -0.015(4) C133 0.096(6) 0.106(8) 0.101(7) 0.017(6) 0.023(6) 0.000(6) C331 0.073(6) 0.057(6) 0.070(6) -0.004(5) 0.013(5) -0.006(5) C332 0.082(6) 0.067(6) 0.086(7) -0.009(6) 0.018(6) 0.004(6) C333 0.106(9) 0.087(9) 0.126(10) 0.002(8) 0.016(8) -0.012(8) N140 0.062(2) 0.060(2) 0.070(3) -0.0160(19) 0.0284(19) -0.0138(19) C141 0.062(3) 0.068(3) 0.081(3) -0.029(2) 0.018(2) -0.001(2) C142 0.073(6) 0.062(5) 0.096(6) -0.029(4) 0.014(5) 0.002(5) C143 0.113(9) 0.080(7) 0.114(9) -0.018(6) 0.013(7) 0.005(6) C342 0.096(7) 0.065(5) 0.085(6) -0.016(5) 0.032(6) -0.008(5) C343 0.136(11) 0.063(7) 0.106(9) -0.035(7) 0.041(8) -0.009(7) N150 0.054(2) 0.085(3) 0.075(3) -0.034(2) 0.025(2) -0.0279(19) C151 0.062(3) 0.079(3) 0.106(4) -0.030(3) 0.017(3) -0.012(2) C152 0.073(4) 0.082(5) 0.097(6) -0.028(5) 0.012(5) -0.005(4) C153 0.109(6) 0.070(5) 0.130(7) -0.011(5) 0.009(5) 0.003(4) C352 0.072(6) 0.087(7) 0.093(8) -0.026(7) 0.021(7) -0.007(6) C353 0.083(9) 0.082(10) 0.092(10) -0.019(8) 0.003(8) -0.010(8) N160 0.049(2) 0.082(3) 0.070(3) -0.005(2) 0.0219(17) 0.0048(19) C161 0.081(4) 0.064(4) 0.094(6) 0.013(4) 0.029(4) 0.002(3) C162 0.131(6) 0.088(5) 0.114(6) 0.020(5) 0.008(5) 0.000(5) C163 0.168(8) 0.093(6) 0.174(8) 0.036(6) 0.014(7) -0.015(6) C361 0.084(8) 0.064(8) 0.099(10) 0.008(8) 0.025(8) -0.001(7) C362 0.104(7) 0.079(7) 0.111(8) 0.011(6) 0.016(6) -0.001(6) C363 0.130(11) 0.086(12) 0.124(12) 0.001(10) 0.014(10) 0.010(11) P21 0.0459(6) 0.0882(9) 0.0627(7) 0.0082(6) 0.0199(5) -0.0010(6) N21 0.0443(19) 0.109(3) 0.061(2) 0.013(2) 0.0177(16) -0.0029(19) P22 0.0467(6) 0.0851(9) 0.0615(7) 0.0085(6) 0.0203(5) 0.0004(6) N22 0.050(2) 0.075(2) 0.062(2) -0.0055(18) 0.0268(16) -0.0040(17) P23 0.0540(7) 0.0687(8) 0.0696(8) -0.0157(6) 0.0272(6) -0.0094(5) N23 0.057(2) 0.085(3) 0.060(2) -0.0148(19) 0.0257(17) -0.0075(19) N210 0.061(3) 0.118(4) 0.088(3) 0.032(3) 0.032(2) 0.026(2) C211 0.066(6) 0.170(9) 0.060(6) -0.017(6) 0.002(5) 0.027(6) C212 0.113(7) 0.207(10) 0.094(7) -0.009(7) 0.030(6) 0.043(7) C213 0.145(11) 0.216(13) 0.117(10) -0.012(10) 0.034(9) 0.029(10) C411 0.111(8) 0.095(7) 0.127(8) 0.025(6) 0.060(7) 0.019(6) C412 0.116(8) 0.110(7) 0.139(8) 0.017(7) 0.014(7) 0.020(7) C413 0.139(11) 0.121(9) 0.168(11) 0.012(9) 0.028(10) 0.043(10) N220 0.061(2) 0.115(3) 0.075(3) 0.026(2) 0.028(2) 0.016(2) C221 0.068(6) 0.119(6) 0.094(6) 0.024(5) 0.026(5) 0.023(5) C222 0.076(6) 0.114(6) 0.078(6) 0.027(5) 0.023(4) 0.008(5) C223 0.128(9) 0.199(11) 0.142(9) 0.021(9) 0.015(7) 0.012(8) C421 0.077(8) 0.112(7) 0.104(8) 0.035(6) 0.030(6) 0.028(7) C422 0.085(6) 0.122(6) 0.113(6) 0.023(6) 0.028(6) 0.023(6) C423 0.102(11) 0.169(12) 0.128(11) 0.030(10) 0.022(9) 0.044(10) N230 0.082(3) 0.073(3) 0.097(3) -0.025(2) 0.046(2) -0.017(2) C231 0.107(6) 0.061(4) 0.096(7) -0.023(4) 0.035(5) -0.006(5) C232 0.114(6) 0.068(4) 0.105(7) -0.014(5) 0.036(5) 0.000(5) C233 0.157(10) 0.091(6) 0.143(10) -0.012(7) 0.032(8) -0.002(7) C431 0.111(8) 0.074(6) 0.105(9) -0.018(7) 0.035(7) -0.012(7) C432 0.110(9) 0.070(6) 0.112(9) -0.004(7) 0.036(7) -0.008(7) C433 0.136(12) 0.096(10) 0.130(12) -0.022(9) 0.015(10) -0.010(10) N240 0.073(3) 0.079(3) 0.074(3) 0.012(2) -0.004(2) -0.010(2) C241 0.146(5) 0.123(5) 0.092(4) 0.026(4) -0.026(4) -0.059(4) C242 0.170(6) 0.178(7) 0.124(5) 0.014(5) -0.004(5) -0.087(5) C243 0.134(6) 0.272(11) 0.157(7) 0.008(7) 0.030(6) -0.056(7) N250 0.054(2) 0.082(3) 0.066(2) -0.001(2) 0.0137(18) -0.014(2) C251 0.102(4) 0.104(4) 0.110(4) -0.005(4) 0.010(3) -0.028(4) C252 0.144(7) 0.100(7) 0.107(8) -0.001(6) 0.021(7) -0.042(6) C253 0.154(11) 0.103(10) 0.127(11) 0.013(9) -0.010(9) 0.009(9) C452 0.164(7) 0.112(6) 0.120(7) 0.019(6) 0.003(6) -0.050(6) C453 0.218(11) 0.145(9) 0.143(10) -0.024(8) 0.023(9) -0.090(8) N260 0.060(2) 0.086(3) 0.063(2) -0.025(2) 0.020(2) -0.0032(19) C261 0.075(3) 0.098(4) 0.076(3) -0.001(3) 0.010(3) -0.014(3) C262 0.079(3) 0.114(4) 0.088(4) 0.020(3) 0.018(3) -0.017(3) C263 0.152(6) 0.067(3) 0.120(5) -0.015(3) 0.035(4) 0.000(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 P11 N11 1.589(3) . ? P11 N13 1.598(3) . ? P11 N110 1.641(3) . ? P11 N140 1.656(4) . ? N11 P12 1.612(3) . ? P12 N12 1.595(4) . ? P12 N150 1.636(4) . ? P12 N120 1.660(4) . ? N12 P13 1.600(3) . ? P13 N13 1.593(3) . ? P13 N160 1.622(4) . ? P13 N130 1.648(4) . ? N110 C111 1.453(5) . ? C111 C112 1.514(5) . ? C112 C113 1.507(7) . ? N120 C121 1.459(5) . ? C121 C122 1.492(7) . ? C122 C123 1.512(6) . ? N130 C331 1.353(9) . ? N130 C131 1.394(7) . ? C131 C132 1.494(9) . ? C132 C133 1.536(11) . ? C331 C332 1.511(12) . ? C332 C333 1.512(14) . ? N140 C141 1.474(5) . ? C141 C142 1.487(10) . ? C141 C342 1.485(11) . ? C142 C143 1.528(11) . ? C342 C343 1.549(12) . ? N150 C151 1.419(6) . ? C151 C152 1.513(8) . ? C151 C352 1.518(14) . ? C152 C153 1.502(10) . ? C352 C353 1.510(15) . ? N160 C161 1.452(7) . ? N160 C361 1.465(15) . ? C161 C162 1.511(10) . ? C162 C163 1.525(11) . ? C361 C362 1.490(16) . ? C362 C363 1.513(16) . ? P21 N23 1.586(4) . ? P21 N21 1.589(4) . ? P21 N210 1.627(4) . ? P21 N240 1.644(4) . ? N21 P22 1.594(3) . ? P22 N22 1.593(4) . ? P22 N250 1.637(4) . ? P22 N220 1.651(4) . ? N22 P23 1.590(4) . ? P23 N23 1.603(3) . ? P23 N260 1.631(4) . ? P23 N230 1.660(4) . ? N210 C211 1.348(9) . ? N210 C411 1.515(10) . ? C211 C212 1.419(11) . ? C212 C213 1.523(12) . ? C411 C412 1.449(12) . ? C412 C413 1.515(13) . ? N220 C221 1.448(11) . ? N220 C421 1.480(14) . ? C221 C222 1.522(13) . ? C222 C223 1.496(13) . ? C421 C422 1.513(14) . ? C422 C423 1.511(15) . ? N230 C431 1.443(15) . ? N230 C231 1.502(10) . ? C231 C232 1.531(11) . ? C232 C233 1.532(11) . ? C431 C432 1.547(15) . ? C432 C433 1.510(15) . ? N240 C241 1.449(6) . ? C241 C242 1.521(8) . ? C242 C243 1.505(9) . ? N250 C251 1.470(6) . ? C251 C452 1.466(11) . ? C251 C252 1.550(13) . ? C252 C253 1.466(15) . ? C452 C453 1.450(12) . ? N260 C261 1.473(6) . ? C261 C262 1.463(6) . ? C262 C263 1.600(7) . ? 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 N11 P11 N13 115.95(17) . . ? N11 P11 N110 106.4(2) . . ? N13 P11 N110 114.47(18) . . ? N11 P11 N140 112.86(19) . . ? N13 P11 N140 104.5(2) . . ? N110 P11 N140 101.96(18) . . ? P11 N11 P12 122.8(2) . . ? N12 P12 N11 115.38(18) . . ? N12 P12 N150 106.66(19) . . ? N11 P12 N150 113.70(18) . . ? N12 P12 N120 110.67(19) . . ? N11 P12 N120 105.21(19) . . ? N150 P12 N120 104.7(2) . . ? P12 N12 P13 121.1(2) . . ? N13 P13 N12 115.24(17) . . ? N13 P13 N160 106.79(19) . . ? N12 P13 N160 115.23(19) . . ? N13 P13 N130 113.82(18) . . ? N12 P13 N130 104.79(19) . . ? N160 P13 N130 100.1(2) . . ? P13 N13 P11 123.3(2) . . ? C111 N110 P11 124.7(3) . . ? N110 C111 C112 112.2(4) . . ? C113 C112 C111 112.0(4) . . ? C121 N120 P12 119.7(3) . . ? N120 C121 C122 113.2(4) . . ? C121 C122 C123 111.8(5) . . ? C331 N130 C131 68.2(6) . . ? C331 N130 P13 131.5(5) . . ? C131 N130 P13 128.0(4) . . ? N130 C131 C132 120.4(6) . . ? C131 C132 C133 115.0(8) . . ? N130 C331 C332 118.9(10) . . ? C331 C332 C333 107.7(11) . . ? C141 N140 P11 119.8(3) . . ? N140 C141 C142 109.4(6) . . ? N140 C141 C342 115.7(6) . . ? C142 C141 C342 28.9(5) . . ? C141 C142 C143 114.7(9) . . ? C141 C342 C343 112.4(11) . . ? C151 N150 P12 124.0(4) . . ? N150 C151 C152 110.3(5) . . ? N150 C151 C352 127.7(11) . . ? C152 C151 C352 25.9(7) . . ? C153 C152 C151 107.6(7) . . ? C353 C352 C151 107.6(13) . . ? C161 N160 C361 24.6(10) . . ? C161 N160 P13 118.6(4) . . ? C361 N160 P13 136.6(13) . . ? N160 C161 C162 113.5(6) . . ? C161 C162 C163 107.6(8) . . ? N160 C361 C362 117.7(17) . . ? C361 C362 C363 107.3(18) . . ? N23 P21 N21 117.09(18) . . ? N23 P21 N210 113.8(2) . . ? N21 P21 N210 104.5(2) . . ? N23 P21 N240 104.4(2) . . ? N21 P21 N240 115.6(2) . . ? N210 P21 N240 100.4(2) . . ? P21 N21 P22 121.5(2) . . ? N21 P22 N22 115.88(19) . . ? N21 P22 N250 110.8(2) . . ? N22 P22 N250 105.46(18) . . ? N21 P22 N220 107.30(19) . . ? N22 P22 N220 112.7(2) . . ? N250 P22 N220 104.2(2) . . ? P23 N22 P22 124.2(2) . . ? N22 P23 N23 115.04(19) . . ? N22 P23 N260 108.35(18) . . ? N23 P23 N260 114.8(2) . . ? N22 P23 N230 112.8(2) . . ? N23 P23 N230 105.38(19) . . ? N260 P23 N230 99.5(2) . . ? P21 N23 P23 123.4(2) . . ? C211 N210 C411 95.4(8) . . ? C211 N210 P21 124.7(5) . . ? C411 N210 P21 120.0(5) . . ? N210 C211 C212 120.5(8) . . ? C211 C212 C213 115.4(11) . . ? C412 C411 N210 112.1(9) . . ? C411 C412 C413 112.2(10) . . ? C221 N220 C421 14.3(10) . . ? C221 N220 P22 125.0(8) . . ? C421 N220 P22 116.6(12) . . ? N220 C221 C222 112.8(10) . . ? C223 C222 C221 107.8(10) . . ? N220 C421 C422 111.8(13) . . ? C423 C422 C421 111.4(15) . . ? C431 N230 C231 15.1(13) . . ? C431 N230 P23 128.7(11) . . ? C231 N230 P23 114.3(6) . . ? N230 C231 C232 111.4(9) . . ? C231 C232 C233 111.7(8) . . ? N230 C431 C432 109.5(15) . . ? C433 C432 C431 103.9(14) . . ? C241 N240 P21 123.0(3) . . ? N240 C241 C242 111.7(5) . . ? C243 C242 C241 116.4(8) . . ? C251 N250 P22 120.1(3) . . ? C452 C251 N250 110.1(7) . . ? C452 C251 C252 26.9(8) . . ? N250 C251 C252 111.9(9) . . ? C253 C252 C251 114.0(13) . . ? C453 C452 C251 116.1(11) . . ? C261 N260 P23 124.1(3) . . ? C262 C261 N260 111.4(4) . . ? C261 C262 C263 108.4(4) . . ? 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 N110 H110 N13 0.86(2) 2.27(2) 3.130(5) 178(5) 2 N120 H120 N230 0.83(2) 2.40(2) 3.230(6) 171(5) 7_556 N130 H130 N250 0.88 2.47 3.213(5) 142.8 4 N140 H140 N140 0.84(2) 3.04(9) 3.235(8) 96(7) 2 N150 H150 N23 0.85(2) 2.41(3) 3.211(6) 157(5) 7_556 N160 H160 N22 0.83(2) 2.20(2) 3.011(5) 168(5) 4 N220 H220 N12 0.87(3) 2.31(3) 3.174(5) 174(5) 4_545 N250 H250 N130 0.83(2) 2.40(3) 3.213(5) 164(4) 4_545 N260 H260 N11 0.87(2) 2.24(3) 3.069(5) 161(4) 7_556 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.699 _refine_diff_density_min -0.336 _refine_diff_density_rms 0.057 #===END data_P10 _database_code_CSD 199629 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H36 N9 P3' _chemical_formula_weight 471.47 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.552(6) _cell_length_b 20.301(13) _cell_length_c 21.372(11) _cell_angle_alpha 90.00 _cell_angle_beta 94.17(3) _cell_angle_gamma 90.00 _cell_volume 4999(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 0.262 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart Apex CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24959 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0800 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 25.02 _reflns_number_total 25137 _reflns_number_gt 18253 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1615P)^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 25137 _refine_ls_number_parameters 589 _refine_ls_number_restraints 95 _refine_ls_R_factor_all 0.1188 _refine_ls_R_factor_gt 0.0904 _refine_ls_wR_factor_ref 0.2399 _refine_ls_wR_factor_gt 0.2199 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N11 N 0.6163(2) 0.82929(15) 0.98139(18) 0.0197(8) Uani 1 1 d . . . P11 P 0.55239(9) 0.76767(5) 1.01060(5) 0.0189(3) Uani 1 1 d . . . N12 N 0.4240(3) 0.90203(14) 0.98808(17) 0.0230(8) Uani 1 1 d . . . P12 P 0.55811(9) 0.90026(5) 0.97191(5) 0.0187(3) Uani 1 1 d . . . N13 N 0.4140(3) 0.76997(14) 1.00568(17) 0.0217(8) Uani 1 1 d . . . P13 P 0.34550(8) 0.83768(5) 0.99122(6) 0.0208(3) Uani 1 1 d . . . N21 N 0.0552(3) 0.73392(14) 0.99093(17) 0.0206(8) Uani 1 1 d . . . P21 P -0.07917(8) 0.73766(5) 1.00622(5) 0.0177(3) Uani 1 1 d . . . N22 N 0.0456(3) 0.60080(14) 0.97682(17) 0.0196(8) Uani 1 1 d . . . P22 P 0.11906(8) 0.66726(5) 0.97360(5) 0.0171(3) Uani 1 1 d . . . N23 N -0.1433(2) 0.66783(15) 1.00805(16) 0.0178(7) Uani 1 1 d . . . P23 P -0.08930(8) 0.59846(5) 0.99004(5) 0.0169(3) Uani 1 1 d . . . N110 N 0.5896(3) 0.69693(15) 0.97940(19) 0.0246(9) Uani 1 1 d D . . H110 H 0.649(3) 0.684(2) 0.992(2) 0.030 Uiso 1 1 d D . . C111 C 0.5557(4) 0.6828(2) 0.9141(2) 0.0368(12) Uani 1 1 d . . . H11A H 0.6170 0.6989 0.8879 0.044 Uiso 1 1 calc R . . H11B H 0.4835 0.7071 0.9015 0.044 Uiso 1 1 calc R . . C112 C 0.5361(4) 0.6106(2) 0.9016(3) 0.0460(14) Uani 1 1 d . . . H112 H 0.5186 0.5978 0.8592 0.055 Uiso 1 1 calc R . . C113 C 0.5410(4) 0.5646(2) 0.9430(3) 0.0567(18) Uani 1 1 d . . . H11C H 0.5583 0.5750 0.9859 0.068 Uiso 1 1 calc R . . H11D H 0.5273 0.5202 0.9306 0.068 Uiso 1 1 calc R . . N120 N 0.5639(3) 0.92997(17) 0.89979(18) 0.0252(8) Uani 1 1 d D . . H120 H 0.626(2) 0.933(2) 0.890(2) 0.030 Uiso 1 1 d D . . C121 C 0.4964(4) 0.8971(2) 0.8489(2) 0.0386(12) Uani 1 1 d . . . H12A H 0.4188 0.8862 0.8629 0.046 Uiso 1 1 calc R . . H12B H 0.5351 0.8552 0.8392 0.046 Uiso 1 1 calc R . . C122 C 0.4816(4) 0.9376(3) 0.7904(2) 0.0427(13) Uani 1 1 d . . . H122 H 0.4401 0.9178 0.7553 0.051 Uiso 1 1 calc R . . C123 C 0.5192(5) 0.9968(3) 0.7826(3) 0.0531(15) Uani 1 1 d . . . H12C H 0.5612 1.0190 0.8162 0.064 Uiso 1 1 calc R . . H12D H 0.5049 1.0182 0.7432 0.064 Uiso 1 1 calc R . . N130 N 0.2662(3) 0.82572(16) 0.9254(2) 0.0280(9) Uani 1 1 d D B . H130 H 0.257(4) 0.7901(13) 0.916(2) 0.034 Uiso 1 1 d D . . C131 C 0.1761(4) 0.8735(2) 0.9042(3) 0.0499(16) Uani 1 1 d DU . . H13A H 0.1006 0.8589 0.9185 0.060 Uiso 1 1 calc R A 1 H13B H 0.1948 0.9168 0.9238 0.060 Uiso 1 1 calc R A 1 C132 C 0.1658(11) 0.8810(6) 0.8362(5) 0.089(4) Uiso 0.796(15) 1 d PDU B 1 H132 H 0.2433 0.8879 0.8255 0.107 Uiso 0.796(15) 1 calc PR B 1 C133 C 0.1128(14) 0.8828(7) 0.7899(7) 0.152(7) Uiso 0.796(15) 1 d PDU B 1 H13C H 0.0310 0.8772 0.7885 0.182 Uiso 0.796(15) 1 calc PR B 1 H13D H 0.1499 0.8901 0.7522 0.182 Uiso 0.796(15) 1 calc PR B 1 C332 C 0.130(2) 0.8604(14) 0.8411(8) 0.043(7) Uiso 0.204(15) 1 d PDU B 2 H332 H 0.0487 0.8569 0.8327 0.052 Uiso 0.204(15) 1 calc PR B 2 C333 C 0.1868(16) 0.8542(9) 0.8020(8) 0.015(6) Uiso 0.204(15) 1 d PDU B 2 H33A H 0.2687 0.8576 0.8095 0.018 Uiso 0.204(15) 1 calc PR B 2 H33B H 0.1536 0.8456 0.7609 0.018 Uiso 0.204(15) 1 calc PR B 2 N140 N 0.6059(3) 0.76311(17) 1.08408(18) 0.0244(8) Uani 1 1 d D D . H140 H 0.671(2) 0.770(2) 1.088(2) 0.029 Uiso 1 1 d D . . C141 C 0.5684(5) 0.7107(2) 1.1256(3) 0.0449(14) Uani 1 1 d DU . . H14A H 0.6279 0.6755 1.1299 0.054 Uiso 1 1 calc R C 1 H14B H 0.4947 0.6910 1.1080 0.054 Uiso 1 1 calc R C 1 C142 C 0.5512(9) 0.7426(7) 1.1915(4) 0.047(3) Uiso 0.63(3) 1 d PDU D 1 H142 H 0.5293 0.7130 1.2230 0.056 Uiso 0.63(3) 1 calc PR D 1 C143 C 0.5628(10) 0.8037(8) 1.2087(6) 0.066(4) Uiso 0.63(3) 1 d PDU D 1 H14C H 0.5846 0.8359 1.1795 0.079 Uiso 0.63(3) 1 calc PR D 1 H14D H 0.5495 0.8162 1.2504 0.079 Uiso 0.63(3) 1 calc PR D 1 C342 C 0.5707(15) 0.7171(11) 1.1916(5) 0.041(5) Uiso 0.37(3) 1 d PDU D 2 H342 H 0.5644 0.6792 1.2172 0.050 Uiso 0.37(3) 1 calc PR D 2 C343 C 0.5814(14) 0.7745(11) 1.2167(8) 0.047(5) Uiso 0.37(3) 1 d PDU D 2 H34A H 0.5877 0.8122 1.1909 0.057 Uiso 0.37(3) 1 calc PR D 2 H34B H 0.5830 0.7791 1.2609 0.057 Uiso 0.37(3) 1 calc PR D 2 N150 N 0.6405(3) 0.95397(15) 1.01083(18) 0.0232(8) Uani 1 1 d D . . H150 H 0.628(4) 0.9902(12) 1.004(2) 0.028 Uiso 1 1 d D . . C151 C 0.6839(4) 0.9426(2) 1.0752(2) 0.0283(11) Uani 1 1 d . . . H15A H 0.6540 0.8997 1.0891 0.034 Uiso 1 1 calc R . . H15B H 0.6530 0.9772 1.1020 0.034 Uiso 1 1 calc R . . C152 C 0.8135(4) 0.9422(2) 1.0852(2) 0.0359(12) Uani 1 1 d . . . H152 H 0.8461 0.9383 1.1271 0.043 Uiso 1 1 calc R . . C153 C 0.8866(4) 0.9469(2) 1.0403(3) 0.0408(13) Uani 1 1 d . . . H15C H 0.8575 0.9509 0.9977 0.049 Uiso 1 1 calc R . . H15D H 0.9679 0.9463 1.0507 0.049 Uiso 1 1 calc R . . N160 N 0.2475(3) 0.85476(18) 1.0418(2) 0.0321(10) Uani 1 1 d D . . H160 H 0.193(3) 0.834(2) 1.036(2) 0.039 Uiso 1 1 d D . . C161 C 0.2772(4) 0.8819(2) 1.1038(2) 0.0384(12) Uani 1 1 d . . . H16A H 0.3595 0.8960 1.1068 0.046 Uiso 1 1 calc R . . H16B H 0.2683 0.8473 1.1358 0.046 Uiso 1 1 calc R . . C162 C 0.2030(4) 0.9387(2) 1.1171(3) 0.0422(13) Uani 1 1 d . . . H162 H 0.2032 0.9744 1.0884 0.051 Uiso 1 1 calc R . . C163 C 0.1372(5) 0.9453(3) 1.1637(3) 0.0590(16) Uani 1 1 d . . . H16C H 0.1336 0.9110 1.1938 0.071 Uiso 1 1 calc R . . H16D H 0.0928 0.9843 1.1676 0.071 Uiso 1 1 calc R . . N210 N -0.1414(3) 0.79212(16) 0.95820(18) 0.0227(8) Uani 1 1 d D . . H210 H -0.199(2) 0.805(2) 0.962(2) 0.027 Uiso 1 1 d D . . C211 C -0.1284(4) 0.7909(2) 0.8908(2) 0.0303(11) Uani 1 1 d . . . H21A H -0.1794 0.7564 0.8710 0.036 Uiso 1 1 calc R . . H21B H -0.0472 0.7797 0.8832 0.036 Uiso 1 1 calc R . . C212 C -0.1589(4) 0.8561(2) 0.8619(2) 0.0374(12) Uani 1 1 d . . . H212 H -0.1301 0.8946 0.8829 0.045 Uiso 1 1 calc R . . C213 C -0.2231(5) 0.8635(3) 0.8092(3) 0.0576(16) Uani 1 1 d . . . H21C H -0.2532 0.8259 0.7870 0.069 Uiso 1 1 calc R . . H21D H -0.2394 0.9064 0.7932 0.069 Uiso 1 1 calc R . . N220 N 0.1647(3) 0.68097(16) 0.90189(18) 0.0211(8) Uani 1 1 d D . . H220 H 0.122(3) 0.697(2) 0.8810(19) 0.025 Uiso 1 1 d D . . C221 C 0.2148(4) 0.6257(2) 0.8699(2) 0.0341(11) Uani 1 1 d . . . H22A H 0.1520 0.5943 0.8572 0.041 Uiso 1 1 calc R . . H22B H 0.2702 0.6028 0.9000 0.041 Uiso 1 1 calc R . . C222 C 0.2767(4) 0.6435(3) 0.8129(3) 0.0469(14) Uani 1 1 d . . . H222 H 0.3038 0.6077 0.7893 0.056 Uiso 1 1 calc R . . C223 C 0.2965(6) 0.6992(4) 0.7931(3) 0.0716(19) Uani 1 1 d . . . H22C H 0.2714 0.7369 0.8148 0.086 Uiso 1 1 calc R . . H22D H 0.3367 0.7045 0.7562 0.086 Uiso 1 1 calc R . . N230 N -0.1577(3) 0.56397(17) 0.92692(19) 0.0232(8) Uani 1 1 d D F . H230 H -0.218(2) 0.558(2) 0.932(2) 0.028 Uiso 1 1 d D . . C231 C -0.1448(4) 0.5940(2) 0.8655(2) 0.0316(11) Uani 1 1 d DU . . H23A H -0.0634 0.6086 0.8633 0.038 Uiso 1 1 calc R E 1 H23B H -0.1951 0.6335 0.8610 0.038 Uiso 1 1 calc R E 1 C232 C -0.1754(9) 0.5484(5) 0.8132(4) 0.038(3) Uiso 0.634(13) 1 d PDU F 1 H232 H -0.1424 0.5055 0.8133 0.046 Uiso 0.634(13) 1 calc PR F 1 C233 C -0.2490(8) 0.5671(5) 0.7657(5) 0.058(3) Uiso 0.634(13) 1 d PDU F 1 H23C H -0.2820 0.6100 0.7655 0.069 Uiso 0.634(13) 1 calc PR F 1 H23D H -0.2685 0.5376 0.7321 0.069 Uiso 0.634(13) 1 calc PR F 1 C432 C -0.2115(14) 0.5560(7) 0.8163(6) 0.032(4) Uiso 0.366(13) 1 d PDU F 2 H432 H -0.2916 0.5490 0.8214 0.038 Uiso 0.366(13) 1 calc PR F 2 C433 C -0.1683(17) 0.5309(8) 0.7656(8) 0.073(7) Uiso 0.366(13) 1 d PDU F 2 H43A H -0.0886 0.5368 0.7589 0.087 Uiso 0.366(13) 1 calc PR F 2 H43B H -0.2171 0.5069 0.7360 0.087 Uiso 0.366(13) 1 calc PR F 2 N240 N -0.1032(3) 0.77364(16) 1.07403(18) 0.0256(8) Uani 1 1 d D . . H240 H -0.096(4) 0.8085(11) 1.078(2) 0.031 Uiso 1 1 d D . . C241 C -0.0737(4) 0.7406(2) 1.1332(2) 0.0357(12) Uani 1 1 d . . . H24A H 0.0097 0.7290 1.1358 0.043 Uiso 1 1 calc R . . H24B H -0.1187 0.6992 1.1345 0.043 Uiso 1 1 calc R . . C242 C -0.0977(5) 0.7816(3) 1.1880(3) 0.0461(13) Uani 1 1 d . . . H242 H -0.1738 0.7992 1.1886 0.055 Uiso 1 1 calc R . . C243 C -0.0278(6) 0.7955(3) 1.2338(3) 0.0592(16) Uani 1 1 d . . . H24C H 0.0494 0.7791 1.2355 0.071 Uiso 1 1 calc R . . H24D H -0.0521 0.8224 1.2668 0.071 Uiso 1 1 calc R . . N250 N 0.2435(3) 0.65365(15) 1.01300(19) 0.0228(8) Uani 1 1 d D . . H250 H 0.288(3) 0.6786(18) 1.015(2) 0.027 Uiso 1 1 d D . . C251 C 0.2660(4) 0.6052(2) 1.0614(2) 0.0303(11) Uani 1 1 d . . . H25A H 0.3430 0.5854 1.0562 0.036 Uiso 1 1 calc R . . H25B H 0.2075 0.5697 1.0551 0.036 Uiso 1 1 calc R . . C252 C 0.2641(4) 0.6301(2) 1.1276(2) 0.0396(13) Uani 1 1 d . . . H252 H 0.2761 0.5989 1.1605 0.048 Uiso 1 1 calc R . . C253 C 0.2471(5) 0.6914(3) 1.1431(3) 0.0556(16) Uani 1 1 d . . . H25C H 0.2348 0.7240 1.1115 0.067 Uiso 1 1 calc R . . H25D H 0.2471 0.7033 1.1861 0.067 Uiso 1 1 calc R . . N260 N -0.1201(3) 0.54410(15) 1.04359(17) 0.0210(8) Uani 1 1 d D . . H260 H -0.111(4) 0.5119(14) 1.031(2) 0.025 Uiso 1 1 d D . . C261 C -0.0741(4) 0.5541(2) 1.1079(2) 0.0343(11) Uani 1 1 d . . . H26A H -0.0307 0.5962 1.1103 0.041 Uiso 1 1 calc R . . H26B H -0.0184 0.5184 1.1195 0.041 Uiso 1 1 calc R . . C262 C -0.1634(5) 0.5557(2) 1.1541(3) 0.0431(13) Uani 1 1 d . . . H262 H -0.1368 0.5621 1.1967 0.052 Uiso 1 1 calc R . . C263 C -0.2751(6) 0.5491(3) 1.1420(3) 0.0585(17) Uani 1 1 d . . . H26C H -0.3060 0.5426 1.1000 0.070 Uiso 1 1 calc R . . H26D H -0.3255 0.5509 1.1751 0.070 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N11 0.0119(15) 0.0123(16) 0.036(2) 0.0033(15) 0.0051(16) 0.0042(13) P11 0.0186(6) 0.0082(5) 0.0303(6) 0.0012(4) 0.0042(5) 0.0022(4) N12 0.0230(17) 0.0095(16) 0.037(2) -0.0020(15) 0.0058(17) 0.0016(12) P12 0.0206(6) 0.0078(5) 0.0278(6) 0.0019(4) 0.0034(5) -0.0002(4) N13 0.0189(18) 0.0072(15) 0.039(2) 0.0018(15) 0.0018(16) -0.0014(12) P13 0.0188(5) 0.0098(5) 0.0344(7) 0.0006(5) 0.0046(5) 0.0008(4) N21 0.0209(17) 0.0078(15) 0.034(2) -0.0001(15) 0.0094(17) -0.0015(12) P21 0.0219(6) 0.0079(5) 0.0238(6) -0.0001(4) 0.0061(5) 0.0015(4) N22 0.0224(17) 0.0095(16) 0.027(2) -0.0038(14) 0.0059(16) 0.0017(12) P22 0.0184(5) 0.0086(5) 0.0249(6) -0.0002(4) 0.0054(5) 0.0003(4) N23 0.0172(15) 0.0143(16) 0.023(2) -0.0010(14) 0.0092(15) -0.0008(13) P23 0.0194(6) 0.0092(5) 0.0225(6) 0.0005(4) 0.0043(5) -0.0004(4) N110 0.025(2) 0.0048(16) 0.043(3) -0.0015(16) 0.0012(19) 0.0027(13) C111 0.043(3) 0.027(2) 0.039(3) -0.011(2) -0.002(2) 0.007(2) C112 0.042(3) 0.027(3) 0.067(4) -0.021(3) -0.013(3) 0.007(2) C113 0.039(3) 0.024(3) 0.108(6) -0.014(3) 0.005(3) -0.005(2) N120 0.029(2) 0.0185(18) 0.029(2) 0.0043(16) 0.0066(19) -0.0003(15) C121 0.045(3) 0.031(3) 0.039(3) 0.000(2) -0.001(2) -0.006(2) C122 0.037(3) 0.057(3) 0.034(3) 0.003(3) 0.001(2) 0.004(2) C123 0.063(4) 0.055(4) 0.042(4) 0.022(3) 0.004(3) 0.009(3) N130 0.0246(19) 0.0097(17) 0.049(3) 0.0052(18) -0.0034(18) -0.0011(15) C131 0.039(3) 0.028(3) 0.079(5) 0.005(3) -0.025(3) 0.004(2) N140 0.0182(17) 0.0205(18) 0.035(2) 0.0026(17) 0.0045(17) 0.0009(14) C141 0.038(3) 0.040(3) 0.055(4) 0.024(3) -0.002(3) -0.008(2) N150 0.0270(18) 0.0094(16) 0.033(2) 0.0035(16) -0.0006(17) -0.0008(13) C151 0.035(3) 0.013(2) 0.038(3) 0.001(2) 0.005(2) -0.0030(17) C152 0.048(3) 0.019(2) 0.038(3) -0.001(2) -0.016(3) 0.003(2) C153 0.032(3) 0.032(3) 0.058(4) 0.006(3) -0.005(3) -0.003(2) N160 0.026(2) 0.026(2) 0.045(3) -0.0072(19) 0.012(2) -0.0009(15) C161 0.038(3) 0.037(3) 0.040(3) -0.001(2) 0.008(2) 0.008(2) C162 0.045(3) 0.035(3) 0.048(4) 0.000(2) 0.012(3) 0.000(2) C163 0.054(3) 0.067(4) 0.057(4) -0.002(3) 0.017(3) 0.013(3) N210 0.0232(19) 0.0168(18) 0.029(2) 0.0031(16) 0.0083(17) 0.0048(14) C211 0.041(3) 0.025(2) 0.025(3) 0.004(2) 0.005(2) 0.0070(19) C212 0.039(3) 0.037(3) 0.037(3) 0.011(2) 0.010(2) 0.014(2) C213 0.061(4) 0.066(4) 0.048(4) 0.021(3) 0.018(3) 0.018(3) N220 0.0191(18) 0.0159(18) 0.029(2) 0.0034(15) 0.0077(16) 0.0037(13) C221 0.038(3) 0.032(3) 0.035(3) -0.001(2) 0.015(2) 0.007(2) C222 0.040(3) 0.062(4) 0.041(3) 0.015(3) 0.010(3) 0.017(3) C223 0.067(4) 0.093(5) 0.058(5) -0.002(4) 0.022(4) 0.003(4) N230 0.0231(19) 0.0177(18) 0.029(2) 0.0009(15) 0.0026(18) -0.0006(15) C231 0.040(3) 0.024(2) 0.030(3) -0.002(2) -0.003(2) -0.0066(19) N240 0.037(2) 0.0105(16) 0.030(2) -0.0021(17) 0.0069(18) 0.0069(16) C241 0.052(3) 0.021(2) 0.033(3) -0.004(2) 0.001(2) 0.011(2) C242 0.049(3) 0.049(3) 0.041(3) -0.002(3) 0.008(3) 0.005(2) C243 0.079(4) 0.058(4) 0.038(4) -0.010(3) -0.010(3) 0.011(3) N250 0.0246(19) 0.0138(19) 0.031(2) 0.0044(16) 0.0065(17) -0.0032(13) C251 0.033(2) 0.017(2) 0.040(3) 0.006(2) -0.004(2) -0.0013(18) C252 0.040(3) 0.043(3) 0.035(3) 0.009(2) -0.004(2) -0.012(2) C253 0.065(4) 0.066(4) 0.037(3) -0.014(3) 0.009(3) -0.016(3) N260 0.0289(19) 0.0101(16) 0.025(2) 0.0011(15) 0.0089(16) 0.0012(14) C261 0.050(3) 0.021(2) 0.031(3) 0.002(2) 0.001(2) 0.002(2) C262 0.071(4) 0.026(3) 0.034(3) 0.000(2) 0.022(3) 0.009(2) C263 0.085(5) 0.041(3) 0.055(4) -0.001(3) 0.042(4) 0.002(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 N11 P12 1.597(3) . ? N11 P11 1.602(3) . ? P11 N13 1.595(3) . ? P11 N140 1.648(4) . ? P11 N110 1.653(3) . ? N12 P13 1.595(3) . ? N12 P12 1.612(4) . ? P12 N150 1.634(4) . ? P12 N120 1.661(4) . ? N13 P13 1.605(3) . ? P13 N130 1.640(4) . ? P13 N160 1.658(4) . ? N21 P22 1.597(3) . ? N21 P21 1.612(3) . ? P21 N23 1.601(3) . ? P21 N210 1.639(4) . ? P21 N240 1.664(4) . ? N22 P22 1.598(3) . ? N22 P23 1.605(3) . ? P22 N250 1.636(4) . ? P22 N220 1.680(4) . ? N23 P23 1.598(3) . ? P23 N260 1.647(4) . ? P23 N230 1.667(4) . ? N110 C111 1.451(6) . ? C111 C112 1.505(6) . ? C112 C113 1.284(8) . ? N120 C121 1.455(6) . ? C121 C122 1.496(7) . ? C122 C123 1.293(7) . ? N130 C131 1.470(5) . ? C131 C332 1.438(16) . ? C131 C132 1.458(11) . ? C132 C133 1.126(14) . ? C332 C333 1.104(19) . ? N140 C141 1.471(6) . ? C141 C342 1.415(13) . ? C141 C142 1.576(11) . ? C142 C143 1.298(12) . ? C342 C343 1.284(16) . ? N150 C151 1.449(6) . ? C151 C152 1.497(6) . ? C152 C153 1.327(7) . ? N160 C161 1.453(6) . ? C161 C162 1.477(6) . ? C162 C163 1.303(7) . ? N210 C211 1.459(6) . ? C211 C212 1.492(6) . ? C212 C213 1.311(7) . ? N220 C221 1.456(5) . ? C221 C222 1.499(7) . ? C222 C223 1.236(8) . ? N230 C231 1.464(6) . ? C231 C432 1.475(11) . ? C231 C232 1.477(9) . ? C232 C233 1.331(11) . ? C432 C433 1.328(15) . ? N240 C241 1.449(6) . ? C241 C242 1.480(7) . ? C242 C243 1.255(7) . ? N250 C251 1.436(5) . ? C251 C252 1.504(7) . ? C252 C253 1.306(7) . ? N260 C261 1.451(6) . ? C261 C262 1.479(7) . ? C262 C263 1.304(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 P12 N11 P11 123.53(19) . . ? N13 P11 N11 116.07(16) . . ? N13 P11 N140 111.7(2) . . ? N11 P11 N140 105.28(19) . . ? N13 P11 N110 106.72(17) . . ? N11 P11 N110 112.36(19) . . ? N140 P11 N110 104.18(19) . . ? P13 N12 P12 123.3(2) . . ? N11 P12 N12 113.29(17) . . ? N11 P12 N150 108.25(18) . . ? N12 P12 N150 114.14(19) . . ? N11 P12 N120 113.60(19) . . ? N12 P12 N120 107.17(19) . . ? N150 P12 N120 99.71(19) . . ? P11 N13 P13 121.04(19) . . ? N12 P13 N13 115.84(17) . . ? N12 P13 N130 111.65(19) . . ? N13 P13 N130 105.97(18) . . ? N12 P13 N160 105.87(18) . . ? N13 P13 N160 113.8(2) . . ? N130 P13 N160 103.0(2) . . ? P22 N21 P21 123.69(19) . . ? N23 P21 N21 114.66(16) . . ? N23 P21 N210 115.47(19) . . ? N21 P21 N210 106.86(18) . . ? N23 P21 N240 105.10(19) . . ? N21 P21 N240 114.95(19) . . ? N210 P21 N240 98.97(19) . . ? P22 N22 P23 123.92(19) . . ? N21 P22 N22 116.74(17) . . ? N21 P22 N250 115.27(18) . . ? N22 P22 N250 106.54(17) . . ? N21 P22 N220 104.60(17) . . ? N22 P22 N220 112.46(18) . . ? N250 P22 N220 100.08(19) . . ? P23 N23 P21 125.82(19) . . ? N23 P23 N22 114.64(16) . . ? N23 P23 N260 108.37(19) . . ? N22 P23 N260 113.83(18) . . ? N23 P23 N230 113.25(18) . . ? N22 P23 N230 106.21(19) . . ? N260 P23 N230 99.62(19) . . ? C111 N110 P11 120.0(3) . . ? N110 C111 C112 113.0(4) . . ? C113 C112 C111 125.9(5) . . ? C121 N120 P12 118.1(3) . . ? N120 C121 C122 113.2(4) . . ? C123 C122 C121 127.0(5) . . ? C131 N130 P13 120.3(3) . . ? C332 C131 C132 23.9(11) . . ? C332 C131 N130 111.7(11) . . ? C132 C131 N130 112.3(7) . . ? C133 C132 C131 151.6(15) . . ? C333 C332 C131 122(2) . . ? C141 N140 P11 120.6(3) . . ? C342 C141 N140 123.3(9) . . ? C342 C141 C142 20.9(7) . . ? N140 C141 C142 107.6(6) . . ? C143 C142 C141 129.0(9) . . ? C343 C342 C141 119.6(14) . . ? C151 N150 P12 121.7(3) . . ? N150 C151 C152 114.2(4) . . ? C153 C152 C151 125.4(5) . . ? C161 N160 P13 123.1(3) . . ? N160 C161 C162 111.7(4) . . ? C163 C162 C161 127.3(5) . . ? C211 N210 P21 122.3(3) . . ? N210 C211 C212 110.9(4) . . ? C213 C212 C211 124.1(5) . . ? C221 N220 P22 117.6(3) . . ? N220 C221 C222 115.2(4) . . ? C223 C222 C221 127.5(6) . . ? C231 N230 P23 118.5(3) . . ? N230 C231 C432 109.8(6) . . ? N230 C231 C232 112.5(5) . . ? C432 C231 C232 17.7(7) . . ? C233 C232 C231 120.2(9) . . ? C433 C432 C231 125.1(15) . . ? C241 N240 P21 120.9(3) . . ? N240 C241 C242 112.6(4) . . ? C243 C242 C241 126.7(5) . . ? C251 N250 P22 126.3(3) . . ? N250 C251 C252 115.7(4) . . ? C253 C252 C251 124.9(5) . . ? C261 N260 P23 118.7(3) . . ? N260 C261 C262 114.2(4) . . ? C263 C262 C261 126.4(5) . . ? 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 N110 H110 N23 0.77(2) 2.42(3) 3.158(5) 162(5) 1_655 N130 H130 N220 0.76(2) 2.47(3) 3.190(5) 161(5) . N140 H140 N240 0.77(2) 2.64(3) 3.389(5) 165(5) 1_655 N150 H150 N12 0.76(2) 2.28(3) 3.017(5) 164(5) 3_677 N160 H160 N21 0.76(2) 2.71(3) 3.433(5) 158(5) . N210 H210 N11 0.72(2) 2.26(2) 2.975(5) 171(5) 1_455 N250 H250 N13 0.72(2) 2.37(2) 3.086(5) 169(5) . N260 H260 N22 0.72(2) 2.42(3) 3.105(5) 160(5) 3_567 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.944 _refine_diff_density_min -0.600 _refine_diff_density_rms 0.119 #===END data_P11 _database_code_CSD 199630 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 N9 P3' _chemical_formula_weight 459.37 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.3518(16) _cell_length_b 7.3886(9) _cell_length_c 22.943(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.712(3) _cell_angle_gamma 90.00 _cell_volume 2216.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 0.294 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart Apex CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13224 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 28.29 _reflns_number_total 5119 _reflns_number_gt 3799 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0458P)^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 5119 _refine_ls_number_parameters 289 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0527 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0867 _refine_ls_wR_factor_gt 0.0818 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.34037(10) 1.05451(19) 0.45911(6) 0.0191(3) Uani 1 1 d . . . P1 P 0.34764(3) 0.84699(6) 0.478996(18) 0.01694(11) Uani 1 1 d . . . N2 N 0.14591(10) 1.08346(18) 0.47349(6) 0.0197(3) Uani 1 1 d . . . P2 P 0.24181(3) 1.18109(6) 0.454989(19) 0.01856(11) Uani 1 1 d . . . N3 N 0.24510(10) 0.76274(19) 0.49325(6) 0.0188(3) Uani 1 1 d . . . P3 P 0.15173(3) 0.88605(6) 0.503146(19) 0.01757(11) Uani 1 1 d . . . N10 N 0.44036(11) 0.8014(2) 0.53682(6) 0.0207(3) Uani 1 1 d D . . H10 H 0.4971(11) 0.824(3) 0.5361(8) 0.025 Uiso 1 1 d D . . C11 C 0.42554(14) 0.8347(3) 0.59728(8) 0.0273(4) Uani 1 1 d . . . H11A H 0.3560 0.7955 0.6005 0.033 Uiso 1 1 calc R . . H11B H 0.4313 0.9661 0.6058 0.033 Uiso 1 1 calc R . . C12 C 0.50125(15) 0.7371(3) 0.64122(8) 0.0291(4) Uani 1 1 d . . . C13 C 0.56130(18) 0.6585(3) 0.67686(9) 0.0429(5) Uani 1 1 d . . . H13 H 0.6098 0.5950 0.7057 0.051 Uiso 1 1 calc R . . N20 N 0.28523(12) 1.3660(2) 0.49110(7) 0.0245(3) Uani 1 1 d D . . H20 H 0.2519(14) 1.451(2) 0.4881(9) 0.029 Uiso 1 1 d D . . C21 C 0.35749(13) 1.3600(2) 0.54778(8) 0.0250(4) Uani 1 1 d . . . H21A H 0.3966 1.4748 0.5528 0.030 Uiso 1 1 calc R . . H21B H 0.4067 1.2608 0.5463 0.030 Uiso 1 1 calc R . . C22 C 0.31251(15) 1.3333(3) 0.60007(9) 0.0329(5) Uani 1 1 d . . . C23 C 0.2799(2) 1.3111(4) 0.64299(11) 0.0582(7) Uani 1 1 d . . . H23 H 0.2533 1.2931 0.6780 0.070 Uiso 1 1 calc R . . N30 N 0.14962(13) 0.9237(2) 0.57313(7) 0.0257(4) Uani 1 1 d D . . H30 H 0.1480(16) 1.020(2) 0.5839(9) 0.031 Uiso 1 1 d D . . C31 C 0.14568(16) 0.7855(3) 0.61772(8) 0.0341(5) Uani 1 1 d . . . H31A H 0.1606 0.6659 0.6020 0.041 Uiso 1 1 calc R . . H31B H 0.0759 0.7810 0.6262 0.041 Uiso 1 1 calc R . . C32 C 0.21918(17) 0.8222(3) 0.67276(9) 0.0403(5) Uani 1 1 d . . . C33 C 0.2802(2) 0.8590(4) 0.71548(11) 0.0647(8) Uani 1 1 d . . . H33 H 0.3297 0.8889 0.7501 0.078 Uiso 1 1 calc R . . N40 N 0.39396(12) 0.7384(2) 0.42754(7) 0.0226(3) Uani 1 1 d D . . H40 H 0.4032(15) 0.6348(19) 0.4325(9) 0.027 Uiso 1 1 d D . . C41 C 0.37396(14) 0.7885(3) 0.36496(8) 0.0274(4) Uani 1 1 d . . . H41A H 0.4325 0.7489 0.3476 0.033 Uiso 1 1 calc R . . H41B H 0.3699 0.9220 0.3619 0.033 Uiso 1 1 calc R . . C42 C 0.27966(15) 0.7110(3) 0.32952(8) 0.0295(4) Uani 1 1 d . . . C43 C 0.20469(17) 0.6455(3) 0.30168(9) 0.0409(5) Uani 1 1 d . . . H43 H 0.1442 0.5926 0.2792 0.049 Uiso 1 1 calc R . . N50 N 0.19779(12) 1.2719(2) 0.38885(7) 0.0253(3) Uani 1 1 d D . . H50 H 0.2341(14) 1.343(2) 0.3799(9) 0.030 Uiso 1 1 d D . . C51 C 0.15260(16) 1.1537(3) 0.33935(8) 0.0328(5) Uani 1 1 d . . . H51A H 0.2068 1.1157 0.3182 0.039 Uiso 1 1 calc R . . H51B H 0.1259 1.0435 0.3555 0.039 Uiso 1 1 calc R . . C52 C 0.06980(16) 1.2388(3) 0.29678(8) 0.0333(5) Uani 1 1 d . . . C53 C 0.00267(17) 1.2989(4) 0.26116(9) 0.0492(6) Uani 1 1 d . . . H53 H -0.0518 1.3477 0.2323 0.059 Uiso 1 1 calc R . . N60 N 0.04995(11) 0.7586(2) 0.48255(7) 0.0248(3) Uani 1 1 d D . . H60 H 0.0045(13) 0.795(3) 0.4927(9) 0.030 Uiso 1 1 d D . . C61 C 0.02976(15) 0.6493(3) 0.42871(9) 0.0337(5) Uani 1 1 d . . . H61A H -0.0211 0.5554 0.4331 0.040 Uiso 1 1 calc R . . H61B H 0.0937 0.5864 0.4252 0.040 Uiso 1 1 calc R . . C62 C -0.00835(14) 0.7494(3) 0.37290(9) 0.0319(5) Uani 1 1 d . . . C63 C -0.03725(17) 0.8287(3) 0.32849(10) 0.0430(5) Uani 1 1 d . . . H63 H -0.0607 0.8931 0.2925 0.052 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0188(7) 0.0151(7) 0.0235(7) 0.0013(6) 0.0046(6) -0.0001(6) P1 0.0156(2) 0.0152(2) 0.0196(2) -0.00016(17) 0.00251(16) 0.00128(17) N2 0.0176(7) 0.0159(7) 0.0253(7) 0.0025(6) 0.0036(6) 0.0040(6) P2 0.0196(2) 0.0151(2) 0.0200(2) 0.00177(17) 0.00161(17) 0.00119(17) N3 0.0176(7) 0.0143(7) 0.0246(7) 0.0000(6) 0.0045(6) 0.0010(6) P3 0.0153(2) 0.0157(2) 0.0215(2) 0.00015(17) 0.00312(17) 0.00088(17) N10 0.0158(7) 0.0226(8) 0.0230(7) 0.0016(6) 0.0022(6) -0.0002(6) C11 0.0273(10) 0.0298(10) 0.0234(9) 0.0003(8) 0.0021(8) 0.0058(8) C12 0.0331(11) 0.0303(11) 0.0227(9) -0.0021(8) 0.0024(8) -0.0014(8) C13 0.0529(14) 0.0428(13) 0.0285(11) 0.0020(10) -0.0021(10) 0.0104(11) N20 0.0271(8) 0.0136(8) 0.0296(8) -0.0002(6) -0.0013(7) 0.0032(6) C21 0.0227(9) 0.0206(10) 0.0302(9) -0.0022(8) 0.0016(7) -0.0021(7) C22 0.0332(11) 0.0301(11) 0.0327(11) -0.0022(9) 0.0004(9) -0.0003(9) C23 0.0537(16) 0.084(2) 0.0390(13) 0.0007(13) 0.0143(12) -0.0035(14) N30 0.0355(9) 0.0181(8) 0.0252(8) 0.0000(7) 0.0102(7) 0.0020(7) C31 0.0433(12) 0.0325(12) 0.0292(10) 0.0047(9) 0.0139(9) -0.0009(9) C32 0.0449(13) 0.0470(14) 0.0309(11) 0.0119(10) 0.0122(10) 0.0060(11) C33 0.0658(18) 0.087(2) 0.0366(13) 0.0192(14) -0.0009(12) -0.0086(16) N40 0.0252(8) 0.0191(8) 0.0237(8) -0.0014(7) 0.0054(6) 0.0042(7) C41 0.0290(10) 0.0313(11) 0.0232(9) -0.0032(8) 0.0084(8) -0.0023(8) C42 0.0354(11) 0.0283(11) 0.0240(9) 0.0015(8) 0.0042(8) 0.0039(9) C43 0.0416(13) 0.0377(13) 0.0375(11) 0.0035(10) -0.0060(10) -0.0037(10) N50 0.0279(9) 0.0218(9) 0.0241(8) 0.0047(7) 0.0005(7) -0.0034(6) C51 0.0399(12) 0.0313(11) 0.0248(9) 0.0001(8) 0.0006(8) 0.0011(9) C52 0.0325(11) 0.0427(12) 0.0247(10) 0.0008(9) 0.0057(9) -0.0049(9) C53 0.0376(13) 0.0760(18) 0.0305(11) 0.0074(12) -0.0011(10) 0.0047(12) N60 0.0159(8) 0.0232(9) 0.0351(9) -0.0021(7) 0.0047(7) 0.0008(6) C61 0.0269(10) 0.0242(10) 0.0451(12) -0.0082(9) -0.0045(9) -0.0032(8) C62 0.0227(10) 0.0338(11) 0.0375(11) -0.0128(9) 0.0018(8) -0.0017(8) C63 0.0407(13) 0.0471(14) 0.0394(12) -0.0069(11) 0.0036(10) -0.0028(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 P1 1.5970(14) . ? N1 P2 1.6014(14) . ? P1 N3 1.5970(14) . ? P1 N40 1.6483(16) . ? P1 N10 1.6552(15) . ? N2 P2 1.6003(15) . ? N2 P3 1.6046(14) . ? P2 N20 1.6416(16) . ? P2 N50 1.6541(15) . ? N3 P3 1.5971(14) . ? P3 N30 1.6354(16) . ? P3 N60 1.6420(16) . ? N10 C11 1.461(2) . ? C11 C12 1.464(2) . ? C12 C13 1.176(3) . ? N20 C21 1.454(2) . ? C21 C22 1.460(3) . ? C22 C23 1.166(3) . ? N30 C31 1.454(2) . ? C31 C32 1.459(3) . ? C32 C33 1.173(3) . ? N40 C41 1.454(2) . ? C41 C42 1.469(3) . ? C42 C43 1.177(3) . ? N50 C51 1.462(2) . ? C51 C52 1.461(3) . ? C52 C53 1.171(3) . ? N60 C61 1.454(2) . ? C61 C62 1.477(3) . ? C62 C63 1.171(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 N1 P2 125.39(9) . . ? N1 P1 N3 115.33(7) . . ? N1 P1 N40 105.83(8) . . ? N3 P1 N40 114.75(8) . . ? N1 P1 N10 114.62(8) . . ? N3 P1 N10 106.82(7) . . ? N40 P1 N10 98.43(8) . . ? P2 N2 P3 123.34(9) . . ? N2 P2 N1 114.41(7) . . ? N2 P2 N20 117.44(8) . . ? N1 P2 N20 104.75(8) . . ? N2 P2 N50 105.76(8) . . ? N1 P2 N50 115.21(8) . . ? N20 P2 N50 98.55(8) . . ? P1 N3 P3 122.21(9) . . ? N3 P3 N2 115.49(7) . . ? N3 P3 N30 113.97(8) . . ? N2 P3 N30 104.63(8) . . ? N3 P3 N60 104.84(8) . . ? N2 P3 N60 115.67(8) . . ? N30 P3 N60 101.65(8) . . ? C11 N10 P1 120.22(12) . . ? N10 C11 C12 111.29(15) . . ? C13 C12 C11 179.3(2) . . ? C21 N20 P2 121.88(12) . . ? N20 C21 C22 115.47(16) . . ? C23 C22 C21 177.7(2) . . ? C31 N30 P3 125.57(13) . . ? N30 C31 C32 111.38(17) . . ? C33 C32 C31 176.5(3) . . ? C41 N40 P1 124.25(13) . . ? N40 C41 C42 114.36(16) . . ? C43 C42 C41 178.6(2) . . ? C51 N50 P2 118.94(12) . . ? C52 C51 N50 113.53(17) . . ? C53 C52 C51 176.6(2) . . ? C61 N60 P3 124.25(13) . . ? N60 C61 C62 115.49(16) . . ? C63 C62 C61 179.1(2) . . ? 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 0.779(14) 2.331(14) 3.099(2) 168.8(19) 3_676 N20 H20 N3 0.766(14) 2.307(17) 2.982(2) 148(2) 1_565 N60 H60 N2 0.743(14) 2.465(14) 3.208(2) 180(3) 3_576 _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.929 _refine_diff_density_max 0.470 _refine_diff_density_min -0.201 _refine_diff_density_rms 0.066 data_P12 _database_code_CSD 199631 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H24 N9 P3' _chemical_formula_weight 315.25 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 Rhombohedral _symmetry_space_group_name_H-M R3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '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' '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' _cell_length_a 7.0898(10) _cell_length_b 7.0898(10) _cell_length_c 51.178(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2227.8(6) _cell_formula_units_Z 6 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 0.401 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4515 _diffrn_reflns_av_R_equivalents 0.1403 _diffrn_reflns_av_sigmaI/netI 0.0845 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -57 _diffrn_reflns_limit_l_max 57 _diffrn_reflns_theta_min 3.34 _diffrn_reflns_theta_max 24.02 _reflns_number_total 1527 _reflns_number_gt 1298 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1885P)^2^+9.5142P] 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 0.058(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.7(5) _refine_ls_number_reflns 1527 _refine_ls_number_parameters 128 _refine_ls_number_restraints 145 _refine_ls_R_factor_all 0.1086 _refine_ls_R_factor_gt 0.0989 _refine_ls_wR_factor_ref 0.2657 _refine_ls_wR_factor_gt 0.2467 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.4354(3) 0.1020(3) 0.03720(7) 0.0404(7) Uani 1 1 d DU . . N1 N 0.4544(9) 0.3335(12) 0.0370(2) 0.071(3) Uani 1 1 d DU . . N10 N 0.2824(17) -0.0477(15) 0.06112(15) 0.090(4) Uani 1 1 d DU . . H10 H 0.1591 -0.1661 0.0572 0.108 Uiso 1 1 calc R . . C11 C 0.3364(16) 0.0015(17) 0.0878(2) 0.078(3) Uani 1 1 d DU . . H11A H 0.2148 -0.1028 0.0987 0.117 Uiso 1 1 calc R . . H11B H 0.3650 0.1493 0.0914 0.117 Uiso 1 1 calc R . . H11C H 0.4667 -0.0077 0.0918 0.117 Uiso 1 1 calc R . . N20 N 0.2792(17) -0.0464(16) 0.01333(16) 0.091(4) Uani 1 1 d DU . . H20 H 0.1531 -0.1609 0.0173 0.110 Uiso 1 1 calc R . . C21 C 0.3380(18) 0.0010(19) -0.0146(2) 0.084(4) Uani 1 1 d DU . . H21A H 0.2149 -0.1010 -0.0254 0.126 Uiso 1 1 calc R . . H21B H 0.4648 -0.0150 -0.0184 0.126 Uiso 1 1 calc R . . H21C H 0.3731 0.1504 -0.0185 0.126 Uiso 1 1 calc R . . P11 P 0.1001(16) 0.0004(16) -0.13177(15) 0.0689(19) Uiso 0.33 1 d PDU A -1 N11 N 0.115(4) -0.219(3) -0.1349(5) 0.072(6) Uiso 0.33 1 d PDU A -1 N110 N -0.073(3) -0.054(4) -0.1078(3) 0.061(7) Uiso 0.33 1 d PDU A -1 H110 H -0.2120 -0.1283 -0.1119 0.073 Uiso 0.33 1 calc PR A -1 C111 C -0.022(12) 0.007(16) -0.0813(4) 0.073(9) Uiso 0.33 1 d PDU A -1 H11D H -0.1559 -0.0589 -0.0710 0.110 Uiso 0.33 1 calc PR A -1 H11E H 0.0516 0.1657 -0.0798 0.110 Uiso 0.33 1 calc PR A -1 H11F H 0.0749 -0.0446 -0.0748 0.110 Uiso 0.33 1 calc PR A -1 N120 N -0.068(4) -0.029(6) -0.1557(3) 0.074(8) Uiso 0.33 1 d PDU A -1 H120 H -0.1948 -0.0432 -0.1514 0.089 Uiso 0.33 1 calc PR A -1 C121 C -0.022(11) -0.034(10) -0.1838(3) 0.068(9) Uiso 0.33 1 d PDU A -1 H12A H -0.1438 -0.0453 -0.1942 0.102 Uiso 0.33 1 calc PR A -1 H12B H -0.0036 -0.1592 -0.1874 0.102 Uiso 0.33 1 calc PR A -1 H12C H 0.1116 0.1007 -0.1885 0.102 Uiso 0.33 1 calc PR A -1 P12 P 0.3369(17) -0.2240(14) -0.12926(16) 0.0662(19) Uiso 0.33 1 d PDU A -1 N12 N 0.561(4) 0.005(4) -0.1275(5) 0.089(8) Uiso 0.33 1 d PDU A -1 N130 N 0.369(6) -0.364(5) -0.1058(3) 0.075(8) Uiso 0.33 1 d PDU A -1 H130 H 0.3863 -0.4745 -0.1101 0.090 Uiso 0.33 1 calc PR A -1 C131 C 0.371(9) -0.316(12) -0.0789(3) 0.070(10) Uiso 0.33 1 d PDU A -1 H13A H 0.4184 -0.4016 -0.0686 0.105 Uiso 0.33 1 calc PR A -1 H13B H 0.2236 -0.3529 -0.0734 0.105 Uiso 0.33 1 calc PR A -1 H13C H 0.4710 -0.1605 -0.0759 0.105 Uiso 0.33 1 calc PR A -1 N140 N 0.376(6) -0.355(5) -0.1531(3) 0.077(9) Uiso 0.33 1 d PDU A -1 H140 H 0.4463 -0.4234 -0.1489 0.092 Uiso 0.33 1 calc PR A -1 C141 C 0.307(10) -0.374(7) -0.1807(3) 0.067(9) Uiso 0.33 1 d PDU A -1 H14A H 0.3664 -0.4504 -0.1907 0.100 Uiso 0.33 1 calc PR A -1 H14B H 0.3613 -0.2280 -0.1881 0.100 Uiso 0.33 1 calc PR A -1 H14C H 0.1475 -0.4557 -0.1818 0.100 Uiso 0.33 1 calc PR A -1 P13 P 0.5615(16) 0.2387(15) -0.12739(15) 0.0675(19) Uiso 0.33 1 d PDU A -1 N13 N 0.328(3) 0.226(5) -0.1273(6) 0.092(7) Uiso 0.33 1 d PDU A -1 N150 N 0.691(5) 0.401(3) -0.1030(3) 0.067(7) Uiso 0.33 1 d PDU A -1 H150 H 0.7971 0.5337 -0.1067 0.080 Uiso 0.33 1 calc PR A -1 C151 C 0.645(12) 0.344(13) -0.0763(3) 0.073(11) Uiso 0.33 1 d PDU A -1 H15A H 0.7424 0.4685 -0.0654 0.110 Uiso 0.33 1 calc PR A -1 H15B H 0.6668 0.2208 -0.0725 0.110 Uiso 0.33 1 calc PR A -1 H15C H 0.4934 0.3026 -0.0726 0.110 Uiso 0.33 1 calc PR A -1 N160 N 0.690(4) 0.407(3) -0.1511(3) 0.059(6) Uiso 0.33 1 d PDU A -1 H160 H 0.7611 0.5459 -0.1469 0.070 Uiso 0.33 1 calc PR A -1 C161 C 0.703(10) 0.358(12) -0.1789(4) 0.082(11) Uiso 0.33 1 d PDU A -1 H16A H 0.7848 0.4943 -0.1887 0.123 Uiso 0.33 1 calc PR A -1 H16B H 0.5556 0.2738 -0.1861 0.123 Uiso 0.33 1 calc PR A -1 H16C H 0.7769 0.2728 -0.1804 0.123 Uiso 0.33 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0173(9) 0.0169(9) 0.0692(12) -0.0007(7) 0.0004(7) -0.0049(6) N1 0.021(4) 0.028(4) 0.170(9) 0.002(3) 0.002(3) 0.018(3) N10 0.061(5) 0.042(4) 0.073(5) 0.010(6) 0.010(6) -0.045(4) C11 0.056(6) 0.063(6) 0.083(7) 0.009(5) 0.012(5) 0.006(4) N20 0.054(5) 0.048(4) 0.077(6) -0.002(6) -0.012(6) -0.045(4) C21 0.072(7) 0.080(8) 0.075(8) -0.015(5) -0.004(5) 0.020(5) _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 N1 1.576(8) 2_655 ? P1 N1 1.578(8) . ? P1 N10 1.628(7) . ? P1 N20 1.631(7) . ? N1 P1 1.576(8) 3_665 ? N10 C11 1.414(15) . ? N20 C21 1.481(15) . ? P11 N11 1.615(17) . ? P11 N13 1.62(3) . ? P11 N110 1.637(14) . ? P11 N120 1.648(15) . ? N11 P12 1.62(2) . ? N110 C111 1.41(2) . ? N120 C121 1.48(2) . ? P12 N12 1.610(17) . ? P12 N140 1.638(16) . ? P12 N130 1.646(15) . ? N12 P13 1.65(3) . ? N130 C131 1.42(2) . ? N140 C141 1.48(2) . ? P13 N13 1.613(17) . ? P13 N160 1.626(15) . ? P13 N150 1.636(15) . ? N150 C151 1.42(2) . ? N160 C161 1.48(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 P1 N1 111.6(3) 2_655 . ? N1 P1 N10 112.7(7) 2_655 . ? N1 P1 N10 111.5(7) . . ? N1 P1 N20 113.0(7) 2_655 . ? N1 P1 N20 110.1(7) . . ? N10 P1 N20 97.3(3) . . ? P1 N1 P1 128.4(3) 3_665 . ? C11 N10 P1 123.7(6) . . ? C21 N20 P1 123.6(6) . . ? N11 P11 N13 116.8(13) . . ? N11 P11 N110 104.4(13) . . ? N13 P11 N110 112.7(13) . . ? N11 P11 N120 101.3(14) . . ? N13 P11 N120 121.9(16) . . ? N110 P11 N120 96.7(10) . . ? P11 N11 P12 122.5(15) . . ? C111 N110 P11 127(3) . . ? C121 N120 P11 125(3) . . ? N12 P12 N11 117.8(14) . . ? N12 P12 N140 104.8(15) . . ? N11 P12 N140 108.8(13) . . ? N12 P12 N130 101.7(15) . . ? N11 P12 N130 125.0(15) . . ? N140 P12 N130 95.1(10) . . ? P12 N12 P13 121.2(19) . . ? C131 N130 P12 123(3) . . ? C141 N140 P12 128(3) . . ? N13 P13 N160 102.9(14) . . ? N13 P13 N150 103.7(14) . . ? N160 P13 N150 98.1(10) . . ? N13 P13 N12 117.2(13) . . ? N160 P13 N12 117.0(13) . . ? N150 P13 N12 115.3(13) . . ? P13 N13 P11 122.8(18) . . ? C151 N150 P13 124(3) . . ? C161 N160 P13 129(3) . . ? 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 0.88 2.27 3.125(10) 165.5 3 N20 H20 N1 0.88 2.25 3.111(10) 164.6 3 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 24.02 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.784 _refine_diff_density_min -0.753 _refine_diff_density_rms 0.116 #===END #===END data_P2 _database_code_CSD 199632 _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 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 0.38 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.25 _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 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Rigaku AFC6S' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 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^)+(0.0207P)^2^+2.4380P] 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 0.0022(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 449 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1726 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.1451 _refine_ls_wR_factor_gt 0.1158 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.014 _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) 0.20105(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(12) Uani 1 d . . . N2 N 0.0856(4) -0.0419(4) 0.2765(3) 0.0239(12) Uani 1 d . . . N3 N -0.1389(4) -0.0366(4) 0.2100(3) 0.0238(11) Uani 1 d . . . N10 N -0.1574(4) -0.0828(4) 0.0538(3) 0.0260(12) Uani 1 d D . . H10 H -0.137(5) -0.067(5) 0.0086(19) 0.031 Uiso 1 d D . . N20 N 0.2382(4) -0.0759(4) 0.1568(3) 0.0261(12) Uani 1 d D . . H20 H 0.202(5) -0.107(5) 0.114(2) 0.031 Uiso 1 d D . . N30 N -0.1496(4) -0.2091(4) 0.2905(3) 0.0265(12) Uani 1 d D . . H30 H -0.184(5) -0.243(4) 0.247(2) 0.032 Uiso 1 d D . . N40 N -0.0930(4) 0.1371(4) 0.1117(3) 0.0248(12) Uani 1 d D . . H40 H -0.029(4) 0.194(3) 0.125(3) 0.030 Uiso 1 d D . . N50 N 0.2865(4) 0.1221(4) 0.2414(3) 0.0243(12) Uani 1 d D . . H50 H 0.338(4) 0.147(5) 0.207(3) 0.029 Uiso 1 d D . . N60 N -0.0763(4) -0.0042(4) 0.3726(3) 0.0286(12) Uani 1 d D . . H60 H -0.011(4) 0.046(4) 0.392(3) 0.034 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 -0.2316 0.1018 0.029 Uiso 1 calc R . . C12 C -0.0858(5) -0.2593(5) 0.0665(3) 0.0288(15) Uani 1 d . . . H12A H -0.0247 -0.2337 0.0241 0.035 Uiso 1 calc R . . H12B H -0.0401 -0.2250 0.1197 0.035 Uiso 1 calc R . . C13 C -0.1299(6) -0.3932(5) 0.0619(4) 0.0401(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 -0.3207(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 0.045 Uiso 1 calc R . . H16B H -0.2279 -0.2468 -0.0696 0.045 Uiso 1 calc R . . 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 0.4504(5) -0.0898(5) 0.1942(4) 0.0361(16) Uani 1 d . . . H22A H 0.4692 -0.0946 0.1364 0.043 Uiso 1 calc R . . H22B H 0.4828 -0.0054 0.2170 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 0.4701(6) -0.2906(6) 0.2089(4) 0.0486(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) -0.2705(5) 0.1734(4) 0.0323(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 . . C31 C -0.1245(5) -0.2826(5) 0.3495(3) 0.0257(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 -0.3501 0.4524 0.053 Uiso 1 calc R . . C34 C -0.0972(6) -0.5052(5) 0.3932(4) 0.0414(18) Uani 1 d . . . H34A H -0.0841 -0.5548 0.4344 0.050 Uiso 1 calc R . . H34B H -0.1051 -0.5509 0.3393 0.050 Uiso 1 calc R . . C35 C -0.2183(6) -0.4759(5) 0.4076(4) 0.0473(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) 0.0432(18) Uani 1 d . . . H36A H -0.3153 -0.3712 0.3642 0.052 Uiso 1 calc R . . H36B H -0.2575 -0.4365 0.2940 0.052 Uiso 1 calc R . . 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) 0.0383(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 -0.3198(6) 0.2881(6) 0.2034(4) 0.0433(18) Uani 1 d . . . H43A H -0.3742 0.2215 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 0.3062 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 . . C51 C 0.2734(5) 0.2137(5) 0.3031(3) 0.0248(14) Uani 1 d . . . H51 H 0.2197 0.1718 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 0.1999(7) 0.3895(6) 0.3381(4) 0.0484(19) Uani 1 d . . . H53A H 0.1607 0.4434 0.3148 0.058 Uiso 1 calc R . . H53B H 0.1442 0.3510 0.3800 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 0.4540 0.056 Uiso 1 calc R . . C56 C 0.4038(4) 0.2854(4) 0.3441(2) 0.0398(17) Uani 1 d . . . H56A H 0.4421 0.2312 0.3679 0.048 Uiso 1 calc R . . H56B H 0.4610 0.3243 0.3030 0.048 Uiso 1 calc R . . C61 C -0.1941(4) 0.0058(4) 0.4069(2) 0.0257(14) Uani 1 d R . . H61 H -0.2675 -0.0625 0.3808 0.031 Uiso 1 calc R . . C62 C -0.1890(6) -0.0046(6) 0.4969(3) 0.0389(17) Uani 1 d . . . H62A H -0.1833 -0.0834 0.5053 0.047 Uiso 1 calc R . . H62B H -0.1108 0.0563 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 -0.3824 -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 0.1300 0.5456 0.066 Uiso 1 calc R . . C65 C -0.3341(6) 0.1338(6) 0.4316(4) 0.0504(19) Uani 1 d . . . H65A H -0.3415 0.2117 0.4227 0.060 Uiso 1 calc R . . H65B H -0.4125 0.0717 0.4068 0.060 Uiso 1 calc R . . C66 C -0.2184(6) 0.1189(6) 0.3898(4) 0.0398(17) Uani 1 d . . . H66A H -0.2324 0.1177 0.3308 0.048 Uiso 1 calc R . . H66B H -0.1418 0.1876 0.4086 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(10) 0.0228(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) N20 0.028(3) 0.030(3) 0.023(3) -0.002(2) -0.009(2) 0.016(3) N30 0.027(3) 0.026(3) 0.025(3) 0.007(2) -0.004(2) 0.006(2) N40 0.022(3) 0.022(3) 0.030(3) 0.000(2) -0.001(2) 0.006(2) N50 0.021(3) 0.029(3) 0.022(3) -0.002(2) 0.004(2) 0.009(2) N60 0.023(3) 0.037(3) 0.022(3) -0.003(2) 0.000(2) 0.005(3) 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) 0.035(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) C21 0.021(3) 0.023(4) 0.023(3) -0.001(3) 0.003(3) 0.007(3) C22 0.020(3) 0.036(4) 0.050(4) 0.009(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) 0.061(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) 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) 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) 0.021(3) -0.003(3) -0.006(3) 0.030(4) 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) -0.018(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) C61 0.020(3) 0.034(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) -0.008(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) 0.048(5) 0.043(4) 0.014(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) . ? P1 N1 1.609(4) . ? P1 N10 1.657(5) . ? P1 N40 1.662(5) . ? P2 N2 1.593(4) . ? P2 N1 1.599(4) . ? P2 N20 1.651(5) . ? P2 N50 1.660(5) . ? P3 N3 1.597(4) . ? P3 N2 1.597(4) . ? P3 N60 1.640(5) . ? P3 N30 1.654(5) . ? N10 C11 1.470(7) . ? N10 H10 0.81(2) . ? N20 C21 1.453(7) . ? N20 H20 0.81(2) . ? N30 C31 1.461(7) . ? N30 H30 0.81(2) . ? N40 C41 1.475(7) . ? N40 H40 0.81(2) . ? N50 C51 1.471(7) . ? N50 H50 0.82(2) . ? N60 C61 1.467(6) . ? N60 H60 0.82(2) . ? C11 C12 1.516(7) . ? C11 C16 1.530(7) . ? C11 H11 1.0000 . ? C12 C13 1.515(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.521(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.505(8) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.518(8) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C21 C26 1.521(7) . ? C21 C22 1.532(7) . ? C21 H21 1.0000 . ? C22 C23 1.532(8) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.513(8) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.519(8) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.524(7) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C31 C36 1.517(7) . ? C31 C32 1.522(7) . ? C31 H31 1.0000 . ? C32 C33 1.525(8) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.501(8) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.506(8) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.515(8) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C41 C42 1.504(7) . ? C41 C46 1.519(7) . ? C41 H41 1.0000 . ? C42 C43 1.518(8) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.518(8) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.512(8) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.538(8) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C51 C52 1.516(7) . ? C51 C56 1.521(6) . ? C51 H51 1.0000 . ? C52 C53 1.521(8) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.499(8) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.520(8) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.516(7) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C61 C66 1.518(7) . ? C61 C62 1.518(7) . ? C61 H61 1.0000 . ? C62 C63 1.517(8) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.510(9) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.517(9) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.519(8) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? 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) . . ? 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) . . ? N2 P2 N1 116.4(2) . . ? N2 P2 N20 114.2(2) . . ? N1 P2 N20 105.4(2) . . ? N2 P2 N50 104.6(2) . . ? N1 P2 N50 115.7(2) . . ? N20 P2 N50 99.6(2) . . ? N3 P3 N2 116.2(2) . . ? 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 102.0(3) . . ? P2 N1 P1 123.2(3) . . ? P2 N2 P3 124.0(3) . . ? P1 N3 P3 123.6(3) . . ? C11 N10 P1 121.5(4) . . ? C11 N10 H10 110(4) . . ? P1 N10 H10 117(4) . . ? C21 N20 P2 122.8(4) . . ? C21 N20 H20 119(4) . . ? P2 N20 H20 110(4) . . ? C31 N30 P3 126.2(4) . . ? C31 N30 H30 117(4) . . ? P3 N30 H30 111(4) . . ? C41 N40 P1 120.3(4) . . ? C41 N40 H40 114(4) . . ? P1 N40 H40 112(4) . . ? C51 N50 P2 122.5(4) . . ? C51 N50 H50 115(4) . . ? P2 N50 H50 111(4) . . ? C61 N60 P3 126.3(3) . . ? C61 N60 H60 115(4) . . ? P3 N60 H60 115(4) . . ? N10 C11 C12 114.6(4) . . ? N10 C11 C16 108.4(4) . . ? C12 C11 C16 110.9(5) . . ? N10 C11 H11 107.6 . . ? C12 C11 H11 107.6 . . ? C16 C11 H11 107.6 . . ? C13 C12 C11 112.6(5) . . ? C13 C12 H12A 109.1 . . ? C11 C12 H12A 109.1 . . ? C13 C12 H12B 109.1 . . ? C11 C12 H12B 109.1 . . ? H12A C12 H12B 107.8 . . ? C12 C13 C14 111.1(5) . . ? C12 C13 H13A 109.4 . . ? C14 C13 H13A 109.4 . . ? C12 C13 H13B 109.4 . . ? C14 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? C15 C14 C13 111.0(5) . . ? C15 C14 H14A 109.4 . . ? C13 C14 H14A 109.4 . . ? C15 C14 H14B 109.4 . . ? C13 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C14 C15 C16 111.6(5) . . ? C14 C15 H15A 109.3 . . ? C16 C15 H15A 109.3 . . ? C14 C15 H15B 109.3 . . ? C16 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? C15 C16 C11 112.1(5) . . ? C15 C16 H16A 109.2 . . ? C11 C16 H16A 109.2 . . ? C15 C16 H16B 109.2 . . ? C11 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? N20 C21 C26 110.7(4) . . ? N20 C21 C22 111.7(4) . . ? C26 C21 C22 110.0(5) . . ? N20 C21 H21 108.1 . . ? C26 C21 H21 108.1 . . ? C22 C21 H21 108.1 . . ? C23 C22 C21 111.1(5) . . ? C23 C22 H22A 109.4 . . ? C21 C22 H22A 109.4 . . ? C23 C22 H22B 109.4 . . ? C21 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C24 C23 C22 112.0(5) . . ? C24 C23 H23A 109.2 . . ? C22 C23 H23A 109.2 . . ? C24 C23 H23B 109.2 . . ? C22 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C23 C24 C25 109.5(5) . . ? C23 C24 H24A 109.8 . . ? C25 C24 H24A 109.8 . . ? C23 C24 H24B 109.8 . . ? C25 C24 H24B 109.8 . . ? H24A C24 H24B 108.2 . . ? C24 C25 C26 111.6(5) . . ? C24 C25 H25A 109.3 . . ? C26 C25 H25A 109.3 . . ? C24 C25 H25B 109.3 . . ? C26 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? C21 C26 C25 112.2(5) . . ? C21 C26 H26A 109.2 . . ? C25 C26 H26A 109.2 . . ? C21 C26 H26B 109.2 . . ? C25 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? N30 C31 C36 109.7(4) . . ? N30 C31 C32 113.4(4) . . ? C36 C31 C32 109.9(5) . . ? N30 C31 H31 107.9 . . ? C36 C31 H31 107.9 . . ? C32 C31 H31 107.9 . . ? C31 C32 C33 111.0(5) . . ? C31 C32 H32A 109.4 . . ? C33 C32 H32A 109.4 . . ? C31 C32 H32B 109.4 . . ? C33 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? C34 C33 C32 110.1(5) . . ? C34 C33 H33A 109.6 . . ? C32 C33 H33A 109.6 . . ? C34 C33 H33B 109.6 . . ? C32 C33 H33B 109.6 . . ? H33A C33 H33B 108.2 . . ? C33 C34 C35 110.3(5) . . ? C33 C34 H34A 109.6 . . ? C35 C34 H34A 109.6 . . ? C33 C34 H34B 109.6 . . ? C35 C34 H34B 109.6 . . ? H34A C34 H34B 108.1 . . ? C34 C35 C36 112.0(5) . . ? C34 C35 H35A 109.2 . . ? C36 C35 H35A 109.2 . . ? C34 C35 H35B 109.2 . . ? C36 C35 H35B 109.2 . . ? H35A C35 H35B 107.9 . . ? C35 C36 C31 112.4(5) . . ? C35 C36 H36A 109.1 . . ? C31 C36 H36A 109.1 . . ? C35 C36 H36B 109.1 . . ? C31 C36 H36B 109.1 . . ? H36A C36 H36B 107.9 . . ? N40 C41 C42 110.9(4) . . ? N40 C41 C46 111.0(4) . . ? C42 C41 C46 110.8(5) . . ? N40 C41 H41 108.0 . . ? C42 C41 H41 108.0 . . ? C46 C41 H41 108.0 . . ? C41 C42 C43 110.9(5) . . ? C41 C42 H42A 109.5 . . ? C43 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? C43 C42 H42B 109.5 . . ? H42A C42 H42B 108.0 . . ? C44 C43 C42 111.2(5) . . ? C44 C43 H43A 109.4 . . ? C42 C43 H43A 109.4 . . ? C44 C43 H43B 109.4 . . ? C42 C43 H43B 109.4 . . ? H43A C43 H43B 108.0 . . ? C45 C44 C43 110.5(5) . . ? C45 C44 H44A 109.5 . . ? C43 C44 H44A 109.5 . . ? C45 C44 H44B 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 108.1 . . ? C44 C45 C46 111.9(5) . . ? C44 C45 H45A 109.2 . . ? C46 C45 H45A 109.2 . . ? C44 C45 H45B 109.2 . . ? C46 C45 H45B 109.2 . . ? H45A C45 H45B 107.9 . . ? C41 C46 C45 110.8(5) . . ? C41 C46 H46A 109.5 . . ? C45 C46 H46A 109.5 . . ? C41 C46 H46B 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 108.1 . . ? N50 C51 C52 114.5(4) . . ? N50 C51 C56 110.1(4) . . ? C52 C51 C56 110.3(4) . . ? N50 C51 H51 107.2 . . ? C52 C51 H51 107.2 . . ? C56 C51 H51 107.2 . . ? C51 C52 C53 111.9(5) . . ? C51 C52 H52A 109.2 . . ? C53 C52 H52A 109.2 . . ? C51 C52 H52B 109.2 . . ? C53 C52 H52B 109.2 . . ? H52A C52 H52B 107.9 . . ? C54 C53 C52 111.6(6) . . ? C54 C53 H53A 109.3 . . ? C52 C53 H53A 109.3 . . ? C54 C53 H53B 109.3 . . ? C52 C53 H53B 109.3 . . ? H53A C53 H53B 108.0 . . ? C53 C54 C55 110.5(5) . . ? C53 C54 H54A 109.6 . . ? C55 C54 H54A 109.6 . . ? C53 C54 H54B 109.6 . . ? C55 C54 H54B 109.6 . . ? H54A C54 H54B 108.1 . . ? C56 C55 C54 110.9(5) . . ? C56 C55 H55A 109.5 . . ? C54 C55 H55A 109.5 . . ? C56 C55 H55B 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 108.0 . . ? C55 C56 C51 112.1(4) . . ? C55 C56 H56A 109.2 . . ? C51 C56 H56A 109.2 . . ? C55 C56 H56B 109.2 . . ? C51 C56 H56B 109.2 . . ? H56A C56 H56B 107.9 . . ? N60 C61 C66 112.4(4) . . ? N60 C61 C62 109.7(4) . . ? C66 C61 C62 111.5(4) . . ? N60 C61 H61 107.7 . . ? C66 C61 H61 107.7 . . ? C62 C61 H61 107.7 . . ? C63 C62 C61 112.4(5) . . ? C63 C62 H62A 109.1 . . ? C61 C62 H62A 109.1 . . ? C63 C62 H62B 109.1 . . ? C61 C62 H62B 109.1 . . ? H62A C62 H62B 107.9 . . ? C64 C63 C62 112.0(6) . . ? C64 C63 H63A 109.2 . . ? C62 C63 H63A 109.2 . . ? C64 C63 H63B 109.2 . . ? C62 C63 H63B 109.2 . . ? H63A C63 H63B 107.9 . . ? C63 C64 C65 110.2(6) . . ? C63 C64 H64A 109.6 . . ? C65 C64 H64A 109.6 . . ? C63 C64 H64B 109.6 . . ? C65 C64 H64B 109.6 . . ? H64A C64 H64B 108.1 . . ? C64 C65 C66 112.5(5) . . ? C64 C65 H65A 109.1 . . ? C66 C65 H65A 109.1 . . ? C64 C65 H65B 109.1 . . ? C66 C65 H65B 109.1 . . ? H65A C65 H65B 107.8 . . ? C61 C66 C65 112.1(5) . . ? C61 C66 H66A 109.2 . . ? C65 C66 H66A 109.2 . . ? C61 C66 H66B 109.2 . . ? C65 C66 H66B 109.2 . . ? H66A C66 H66B 107.9 . . ? 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) . . . . ? N20 P2 N1 P1 125.5(3) . . . . ? N50 P2 N1 P1 -125.6(3) . . . . ? N3 P1 N1 P2 4.0(4) . . . . ? N10 P1 N1 P2 -120.2(3) . . . . ? N40 P1 N1 P2 128.9(3) . . . . ? N1 P2 N2 P3 1.7(4) . . . . ? N20 P2 N2 P3 -121.5(3) . . . . ? N50 P2 N2 P3 130.8(3) . . . . ? N3 P3 N2 P2 -3.1(4) . . . . ? N60 P3 N2 P2 -130.7(3) . . . . ? N30 P3 N2 P2 118.6(3) . . . . ? N1 P1 N3 P3 -5.6(4) . . . . ? N10 P1 N3 P3 123.2(3) . . . . ? N40 P1 N3 P3 -126.5(3) . . . . ? N2 P3 N3 P1 5.2(4) . . . . ? 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 83.8(5) . . . . ? N40 P1 N10 C11 -163.6(4) . . . . ? N2 P2 N20 C21 -39.5(5) . . . . ? N1 P2 N20 C21 -168.5(4) . . . . ? N50 P2 N20 C21 71.3(5) . . . . ? N3 P3 N30 C31 -178.9(4) . . . . ? N2 P3 N30 C31 52.7(5) . . . . ? N60 P3 N30 C31 -58.9(5) . . . . ? N3 P1 N40 C41 -37.2(5) . . . . ? N1 P1 N40 C41 -164.5(4) . . . . ? N10 P1 N40 C41 75.5(4) . . . . ? N2 P2 N50 C51 -48.2(5) . . . . ? N1 P2 N50 C51 81.2(5) . . . . ? N20 P2 N50 C51 -166.5(4) . . . . ? N3 P3 N60 C61 46.9(5) . . . . ? N2 P3 N60 C61 175.0(4) . . . . ? N30 P3 N60 C61 -64.3(5) . . . . ? P1 N10 C11 C12 -58.1(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 -56.0(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) . . . . ? P2 N20 C21 C26 124.1(5) . . . . ? P2 N20 C21 C22 -113.0(5) . . . . ? N20 C21 C22 C23 -177.6(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 178.3(5) . . . . ? C22 C21 C26 C25 54.5(6) . . . . ? C24 C25 C26 C21 -56.3(7) . . . . ? P3 N30 C31 C36 166.9(4) . . . . ? P3 N30 C31 C32 -69.8(6) . . . . ? N30 C31 C32 C33 -179.1(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) . . . . ? P1 N40 C41 C42 122.3(4) . . . . ? P1 N40 C41 C46 -114.0(5) . . . . ? N40 C41 C42 C43 -178.8(5) . . . . ? C46 C41 C42 C43 57.5(7) . . . . ? C41 C42 C43 C44 -57.9(7) . . . . ? C42 C43 C44 C45 56.1(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) . . . . ? 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 -178.5(4) . . . . ? C52 C51 C56 C55 54.2(6) . . . . ? P3 N60 C61 C66 -91.9(5) . . . . ? P3 N60 C61 C62 143.5(4) . . . . ? N60 C61 C62 C63 177.3(5) . . . . ? C66 C61 C62 C63 52.2(6) . . . . ? C61 C62 C63 C64 -54.8(7) . . . . ? C62 C63 C64 C65 55.4(7) . . . . ? C63 C64 C65 C66 -55.2(8) . . . . ? N60 C61 C66 C65 -175.1(5) . . . . ? C62 C61 C66 C65 -51.5(6) . . . . ? C64 C65 C66 C61 53.8(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 0.81(2) 2.43(3) 3.247(6) 175(5) 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