data_tca020 # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof. Colin L. Raston' _publ_contact_author_address ; Chemistry Section, M313, School of Biomedical and Chemical Sciences, University of Western Australia, 35 Stirling Highway, Crawley, 6009, W.A., Australia ; _publ_contact_author_email 'clraston@cyllene.uwa.edu.au' _publ_contact_author_fax '+618 6488 3045' _publ_contact_author_phone '+618 6488 8683' _publ_requested_journal 'Crystal Growth and Design' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this submission for publication as a New paper in Crystal Growth and Design, 2010. The figures, chemical structure diagram (scheme), Transfer of Copyright Agreement form and structure factor listing will be sent on receipt of your acknowledgement email or letter. ; # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_address 'Thomas Clark' ; Chemistry Section, M313, School of Biomedical and Chemical Sciences, University of Western Australia, 35 Stirling Highway, Crawley, 6009, W.A., Australia ; 'Adam Martin.' ; Chemistry Section, M313, School of Biomedical and Chemical Sciences, University of Western Australia, 35 Stirling Highway, Crawley, 6009, W.A., Australia ; 'Colin L. Raston' ; Chemistry Section, M313, School of Biomedical and Chemical Sciences, University of Western Australia, 35 Stirling Highway, Crawley, 6009, W.A., Australia ; 'Alexandre N. Sobolev' ; Chemistry Section, M313, School of Biomedical and Chemical Sciences, University of Western Australia, 35 Stirling Highway, Crawley, 6009, W.A., Australia ; # 4. TEXT _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Barbour, L. J. (2001). J. Supramol. Chem., 1, 189-191. Sheldrick, G.M. (2008). Acta Cryst., A64, 112-122. ; # 5. CHEMICAL DATA _publ_section_figure_captions ; ? #<< figure captions ; #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H54 O24 P6, 4(H N O3), 6(H2 O)' _chemical_formula_sum 'C48 H70 N4 O42 P6' _chemical_formula_weight 1560.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.182(2) _cell_length_b 12.332(2) _cell_length_c 13.108(2) _cell_angle_alpha 113.447(3) _cell_angle_beta 94.212(3) _cell_angle_gamma 108.695(3) _cell_volume 1664.9(5) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 0.270 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.9355 _exptl_absorpt_correction_T_max 0.9866 _exptl_absorpt_process_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10181 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5816 _reflns_number_gt 4259 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+3.7000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5816 _refine_ls_number_parameters 444 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0947 _refine_ls_R_factor_gt 0.0697 _refine_ls_wR_factor_ref 0.2030 _refine_ls_wR_factor_gt 0.1849 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 O1 O 1.3317(3) 0.3258(3) 1.2323(3) 0.0347(7) Uani 1 1 d . . . C11 C 1.2876(4) 0.2339(4) 1.2711(4) 0.0263(9) Uani 1 1 d . . . C12 C 1.2291(4) 0.2600(4) 1.3594(3) 0.0259(9) Uani 1 1 d . . . C13 C 1.1812(4) 0.1651(4) 1.3942(4) 0.0281(9) Uani 1 1 d . . . H13 H 1.1408 0.1810 1.4545 0.034 Uiso 1 1 calc R . . C14 C 1.1918(4) 0.0471(4) 1.3414(4) 0.0295(10) Uani 1 1 d . . . C15 C 1.2509(4) 0.0240(4) 1.2517(4) 0.0303(10) Uani 1 1 d . . . H15 H 1.2574 -0.0567 1.2149 0.036 Uiso 1 1 calc R . . C16 C 1.2995(4) 0.1164(4) 1.2161(3) 0.0261(9) Uani 1 1 d . . . C17 C 1.4546(5) 0.4118(5) 1.2838(5) 0.0525(14) Uani 1 1 d . . . H171 H 1.4769 0.4723 1.2508 0.079 Uiso 1 1 calc R . . H172 H 1.5057 0.3626 1.2690 0.079 Uiso 1 1 calc R . . H173 H 1.4646 0.4590 1.3664 0.079 Uiso 1 1 calc R . . P1 P 1.13065(11) -0.07698(11) 1.38312(11) 0.0330(3) Uani 1 1 d . . . O11 O 1.0371(3) -0.1885(3) 1.2837(3) 0.0443(9) Uani 1 1 d . . . O12 O 1.0902(3) -0.0262(3) 1.4936(3) 0.0408(8) Uani 1 1 d . . . H12A H 1.0274 -0.0147 1.4803 0.061 Uiso 1 1 calc R . . O13 O 1.2345(3) -0.1155(3) 1.4147(3) 0.0378(8) Uani 1 1 d . . . H13A H 1.2439 -0.1683 1.3550 0.057 Uiso 1 1 calc R . . C1 C 1.2182(4) 0.3889(4) 1.4179(4) 0.0283(9) Uani 1 1 d . . . H11 H 1.1895 0.3958 1.4880 0.034 Uiso 1 1 calc R . . H12 H 1.2981 0.4576 1.4410 0.034 Uiso 1 1 calc R . . O2 O 0.9663(3) 0.2674(3) 1.3709(2) 0.0295(7) Uani 1 1 d . . . C21 C 1.0110(4) 0.3505(4) 1.3225(3) 0.0263(9) Uani 1 1 d . . . C22 C 0.9326(4) 0.3705(4) 1.2561(3) 0.0269(9) Uani 1 1 d . . . C23 C 0.9792(4) 0.4460(4) 1.2015(4) 0.0289(10) Uani 1 1 d . . . H23 H 0.9269 0.4566 1.1521 0.035 Uiso 1 1 calc R . . C24 C 1.1026(4) 0.5060(4) 1.2194(4) 0.0282(9) Uani 1 1 d . . . C25 C 1.1787(4) 0.4892(4) 1.2911(4) 0.0296(10) Uani 1 1 d . . . H25 H 1.2623 0.5329 1.3055 0.036 Uiso 1 1 calc R . . C26 C 1.1345(4) 0.4092(4) 1.3427(4) 0.0265(9) Uani 1 1 d . . . C27 C 0.9371(5) 0.3258(5) 1.4790(4) 0.0408(12) Uani 1 1 d . . . H271 H 0.9070 0.2619 1.5073 0.061 Uiso 1 1 calc R . . H272 H 0.8760 0.3587 1.4689 0.061 Uiso 1 1 calc R . . H273 H 1.0087 0.3964 1.5342 0.061 Uiso 1 1 calc R . . P2 P 1.16703(11) 0.60058(11) 1.14906(10) 0.0311(3) Uani 1 1 d . . . O21 O 1.2749(3) 0.7163(3) 1.2324(3) 0.0356(7) Uani 1 1 d . . . O22 O 1.2003(3) 0.5194(3) 1.0414(3) 0.0425(8) Uani 1 1 d . . . H22A H 1.2031 0.4540 1.0455 0.064 Uiso 1 1 calc R . . O23 O 1.0736(3) 0.6406(3) 1.1029(3) 0.0383(8) Uani 1 1 d . . . H23A H 1.0595 0.6950 1.1578 0.057 Uiso 1 1 calc R . . C2 C 0.7984(4) 0.3156(4) 1.2456(4) 0.0314(10) Uani 1 1 d . . . H21 H 0.7818 0.2595 1.2843 0.038 Uiso 1 1 calc R . . H22 H 0.7732 0.3870 1.2867 0.038 Uiso 1 1 calc R . . O3 O 0.7926(3) 0.0746(3) 1.1039(3) 0.0374(8) Uani 1 1 d . . . C31 C 0.7214(4) 0.1182(4) 1.0565(4) 0.0284(9) Uani 1 1 d . . . C32 C 0.6439(4) 0.0399(4) 0.9483(4) 0.0278(9) Uani 1 1 d . . . C33 C 0.5717(4) 0.0891(4) 0.9086(4) 0.0283(9) Uani 1 1 d . . . H33 H 0.5171 0.0370 0.8362 0.034 Uiso 1 1 calc R . . C34 C 0.5779(4) 0.2136(4) 0.9726(4) 0.0277(9) Uani 1 1 d . . . C35 C 0.6536(4) 0.2881(4) 1.0819(4) 0.0287(9) Uani 1 1 d . . . H35 H 0.6569 0.3719 1.1267 0.034 Uiso 1 1 calc R . . C36 C 0.7238(4) 0.2402(4) 1.1250(4) 0.0274(9) Uani 1 1 d . . . C37 C 0.8953(5) 0.0688(5) 1.0579(5) 0.0478(13) Uani 1 1 d . . . H371 H 0.9395 0.0363 1.0961 0.072 Uiso 1 1 calc R . . H372 H 0.9467 0.1547 1.0706 0.072 Uiso 1 1 calc R . . H373 H 0.8696 0.0116 0.9757 0.072 Uiso 1 1 calc R . . P3 P 0.49031(11) 0.27689(11) 0.91612(10) 0.0313(3) Uani 1 1 d . . . O31 O 0.5165(3) 0.4108(3) 1.0054(3) 0.0474(9) Uani 1 1 d . . . O32 O 0.5190(3) 0.2653(3) 0.8002(3) 0.0392(8) Uani 1 1 d . . . H32A H 0.5904 0.2736 0.8025 0.059 Uiso 1 1 calc R . . O33 O 0.3568(3) 0.1976(3) 0.8927(3) 0.0395(8) Uani 1 1 d . . . H33A H 0.3341 0.1373 0.8262 0.059 Uiso 1 1 calc R . . C3 C 0.6328(4) -0.0958(4) 0.8796(4) 0.0321(10) Uani 1 1 d . . . H31 H 0.5474 -0.1504 0.8452 0.039 Uiso 1 1 calc R . . H32 H 0.6617 -0.1252 0.9323 0.039 Uiso 1 1 calc R . . N1A N 0.5521(5) 0.1912(9) 0.4184(6) 0.086(2) Uani 1 1 d . . . O11A O 0.5132(5) 0.2658(5) 0.4994(5) 0.0937(16) Uani 1 1 d . . . H11A H 0.4903 0.2316 0.5422 0.141 Uiso 1 1 calc R . . O12A O 0.5189(6) 0.0764(7) 0.4052(5) 0.1056(19) Uani 1 1 d . . . O13A O 0.6038(5) 0.2304(9) 0.3634(7) 0.150(3) Uani 1 1 d . . . N1B N 0.2407(7) 0.3458(9) 0.7362(8) 0.0394(14) Uiso 0.50 1 d PD A 1 O11B O 0.1775(12) 0.2377(11) 0.7462(11) 0.079(2) Uiso 0.50 1 d PD A 1 H11B H 0.1045 0.2235 0.7326 0.118 Uiso 0.50 1 calc PR A 1 O12B O 0.1877(8) 0.3841(9) 0.6860(8) 0.0564(15) Uiso 0.50 1 d PD A 1 O13B O 0.3462(8) 0.3754(10) 0.7539(9) 0.081(2) Uiso 0.50 1 d PD A 1 N1C N 0.2345(7) 0.3324(9) 0.7046(8) 0.0394(14) Uiso 0.50 1 d PD B 2 O11C O 0.1992(12) 0.2716(11) 0.7727(10) 0.079(2) Uiso 0.50 1 d PD B 2 H11C H 0.1246 0.2436 0.7616 0.118 Uiso 0.50 1 calc PR B 2 O12C O 0.1489(7) 0.3490(9) 0.6706(8) 0.0564(15) Uiso 0.50 1 d PD B 2 O13C O 0.3266(8) 0.3856(10) 0.6856(9) 0.081(2) Uiso 0.50 1 d PD B 2 O1W O 1.2139(4) 0.3119(4) 1.0289(3) 0.0507(9) Uani 1 1 d . . . H1WA H 1.2539 0.3222 1.0903 0.076 Uiso 1 1 d . . . H1WB H 1.2512 0.2885 0.9773 0.076 Uiso 1 1 d . . . O2W O 0.3859(4) 0.1345(5) 0.5825(4) 0.0822(15) Uani 1 1 d . . . H2WA H 0.3781 0.1793 0.6507 0.123 Uiso 1 1 d . . . H2WB H 0.3129 0.0906 0.5414 0.123 Uiso 1 1 d . . . O3W O 0.7707(4) -0.0014(3) 1.2910(3) 0.0558(10) Uani 1 1 d . . . H3WA H 0.8132 0.0627 1.2823 0.084 Uiso 1 1 d . . . H3WB H 0.8063 0.0049 1.3525 0.084 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0428(19) 0.0278(16) 0.0421(18) 0.0196(15) 0.0199(15) 0.0168(14) C11 0.028(2) 0.027(2) 0.030(2) 0.0171(19) 0.0097(18) 0.0114(18) C12 0.029(2) 0.026(2) 0.023(2) 0.0096(18) 0.0026(17) 0.0137(18) C13 0.034(2) 0.033(2) 0.024(2) 0.0139(19) 0.0150(18) 0.019(2) C14 0.035(2) 0.032(2) 0.033(2) 0.019(2) 0.0164(19) 0.019(2) C15 0.039(3) 0.025(2) 0.033(2) 0.014(2) 0.016(2) 0.018(2) C16 0.029(2) 0.026(2) 0.027(2) 0.0112(19) 0.0108(18) 0.0154(18) C17 0.043(3) 0.036(3) 0.073(4) 0.022(3) 0.026(3) 0.009(2) P1 0.0380(7) 0.0330(7) 0.0397(7) 0.0215(6) 0.0207(5) 0.0185(5) O11 0.0376(19) 0.048(2) 0.056(2) 0.0299(19) 0.0189(17) 0.0175(16) O12 0.047(2) 0.049(2) 0.047(2) 0.0307(17) 0.0285(16) 0.0281(17) O13 0.047(2) 0.0400(19) 0.0372(18) 0.0213(16) 0.0179(15) 0.0228(16) C1 0.034(2) 0.027(2) 0.024(2) 0.0092(18) 0.0077(18) 0.0139(19) O2 0.0412(18) 0.0255(15) 0.0268(15) 0.0133(13) 0.0139(13) 0.0155(14) C21 0.041(3) 0.020(2) 0.023(2) 0.0087(18) 0.0158(18) 0.0163(19) C22 0.032(2) 0.025(2) 0.024(2) 0.0089(18) 0.0112(18) 0.0127(19) C23 0.037(3) 0.030(2) 0.027(2) 0.0151(19) 0.0144(19) 0.018(2) C24 0.039(3) 0.026(2) 0.027(2) 0.0129(19) 0.0164(19) 0.018(2) C25 0.035(2) 0.028(2) 0.030(2) 0.013(2) 0.0138(19) 0.016(2) C26 0.033(2) 0.022(2) 0.025(2) 0.0058(18) 0.0104(18) 0.0163(19) C27 0.059(3) 0.035(3) 0.030(2) 0.015(2) 0.019(2) 0.016(2) P2 0.0376(7) 0.0317(6) 0.0327(6) 0.0188(5) 0.0158(5) 0.0165(5) O21 0.0383(18) 0.0345(18) 0.0393(18) 0.0199(15) 0.0165(14) 0.0145(15) O22 0.056(2) 0.046(2) 0.0386(19) 0.0236(17) 0.0251(16) 0.0256(17) O23 0.047(2) 0.0405(19) 0.0377(18) 0.0228(16) 0.0132(15) 0.0222(16) C2 0.033(2) 0.037(3) 0.033(2) 0.019(2) 0.0165(19) 0.018(2) O3 0.0453(19) 0.0448(19) 0.0435(19) 0.0283(17) 0.0195(15) 0.0302(16) C31 0.032(2) 0.032(2) 0.035(2) 0.022(2) 0.0195(19) 0.018(2) C32 0.034(2) 0.025(2) 0.036(2) 0.019(2) 0.0222(19) 0.0151(19) C33 0.031(2) 0.030(2) 0.025(2) 0.0132(19) 0.0132(18) 0.0116(19) C34 0.032(2) 0.031(2) 0.033(2) 0.020(2) 0.0193(19) 0.0181(19) C35 0.034(2) 0.028(2) 0.032(2) 0.016(2) 0.0169(19) 0.0158(19) C36 0.026(2) 0.032(2) 0.033(2) 0.018(2) 0.0164(18) 0.0139(19) C37 0.041(3) 0.056(3) 0.056(3) 0.021(3) 0.019(2) 0.033(3) P3 0.0374(7) 0.0356(7) 0.0311(6) 0.0175(5) 0.0118(5) 0.0220(5) O31 0.069(2) 0.040(2) 0.041(2) 0.0165(17) 0.0058(18) 0.0346(19) O32 0.0336(18) 0.057(2) 0.0357(18) 0.0260(17) 0.0114(14) 0.0202(16) O33 0.0372(19) 0.051(2) 0.0384(18) 0.0210(17) 0.0134(15) 0.0246(16) C3 0.037(3) 0.028(2) 0.039(3) 0.018(2) 0.021(2) 0.015(2) N1A 0.052(3) 0.149(7) 0.088(5) 0.081(5) 0.028(3) 0.038(4) O11A 0.102(4) 0.089(4) 0.087(4) 0.040(3) 0.037(3) 0.030(3) O12A 0.099(5) 0.133(6) 0.099(4) 0.051(4) 0.026(4) 0.062(4) O13A 0.076(4) 0.263(10) 0.163(7) 0.154(7) 0.061(4) 0.044(5) O1W 0.073(3) 0.054(2) 0.043(2) 0.0228(18) 0.0286(19) 0.041(2) O2W 0.079(3) 0.098(4) 0.053(3) 0.035(3) 0.009(2) 0.013(3) O3W 0.079(3) 0.041(2) 0.043(2) 0.0220(18) 0.0117(19) 0.0129(19) _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 O1 C11 1.393(5) . ? O1 C17 1.445(6) . ? C11 C12 1.386(6) . ? C11 C16 1.401(6) . ? C12 C13 1.393(6) . ? C12 C1 1.521(6) . ? C13 C14 1.395(6) . ? C14 C15 1.404(6) . ? C14 P1 1.787(4) . ? C15 C16 1.378(6) . ? C16 C3 1.533(6) 2_757 ? P1 O11 1.496(4) . ? P1 O12 1.521(3) . ? P1 O13 1.569(3) . ? C1 C26 1.512(6) . ? O2 C21 1.399(5) . ? O2 C27 1.441(5) . ? C21 C22 1.390(6) . ? C21 C26 1.396(6) . ? C22 C23 1.396(6) . ? C22 C2 1.528(6) . ? C23 C24 1.400(6) . ? C24 C25 1.392(6) . ? C24 P2 1.789(4) . ? C25 C26 1.402(6) . ? P2 O21 1.518(3) . ? P2 O22 1.542(3) . ? P2 O23 1.551(3) . ? C2 C36 1.506(6) . ? O3 C31 1.383(5) . ? O3 C37 1.438(6) . ? C31 C36 1.401(6) . ? C31 C32 1.401(6) . ? C32 C33 1.392(6) . ? C32 C3 1.506(6) . ? C33 C34 1.400(6) . ? C34 C35 1.401(6) . ? C34 P3 1.781(4) . ? C35 C36 1.385(6) . ? P3 O31 1.506(4) . ? P3 O33 1.537(3) . ? P3 O32 1.545(3) . ? C3 C16 1.533(6) 2_757 ? N1A O13A 1.139(8) . ? N1A O12A 1.275(9) . ? N1A O11A 1.331(9) . ? N1B O13B 1.194(7) . ? N1B O12B 1.206(7) . ? N1B O11B 1.372(9) . ? N1C O13C 1.205(7) . ? N1C O12C 1.212(7) . ? N1C O11C 1.388(9) . ? 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 C11 O1 C17 115.8(4) . . ? C12 C11 O1 118.9(4) . . ? C12 C11 C16 122.4(4) . . ? O1 C11 C16 118.6(4) . . ? C11 C12 C13 118.3(4) . . ? C11 C12 C1 121.1(4) . . ? C13 C12 C1 120.6(4) . . ? C12 C13 C14 120.8(4) . . ? C13 C14 C15 119.3(4) . . ? C13 C14 P1 122.0(3) . . ? C15 C14 P1 118.7(3) . . ? C16 C15 C14 121.0(4) . . ? C15 C16 C11 118.2(4) . . ? C15 C16 C3 122.5(4) . 2_757 ? C11 C16 C3 119.3(4) . 2_757 ? O11 P1 O12 115.6(2) . . ? O11 P1 O13 110.10(19) . . ? O12 P1 O13 104.52(18) . . ? O11 P1 C14 108.2(2) . . ? O12 P1 C14 110.6(2) . . ? O13 P1 C14 107.55(19) . . ? C26 C1 C12 113.1(3) . . ? C21 O2 C27 114.4(3) . . ? C22 C21 C26 122.6(4) . . ? C22 C21 O2 119.7(4) . . ? C26 C21 O2 117.6(4) . . ? C21 C22 C23 118.6(4) . . ? C21 C22 C2 121.2(4) . . ? C23 C22 C2 120.1(4) . . ? C22 C23 C24 120.2(4) . . ? C25 C24 C23 119.6(4) . . ? C25 C24 P2 118.3(3) . . ? C23 C24 P2 122.1(3) . . ? C24 C25 C26 121.3(4) . . ? C21 C26 C25 117.4(4) . . ? C21 C26 C1 121.8(4) . . ? C25 C26 C1 120.8(4) . . ? O21 P2 O22 111.59(19) . . ? O21 P2 O23 111.45(18) . . ? O22 P2 O23 104.41(19) . . ? O21 P2 C24 108.96(19) . . ? O22 P2 C24 110.10(19) . . ? O23 P2 C24 110.3(2) . . ? C36 C2 C22 115.0(3) . . ? C31 O3 C37 115.4(3) . . ? O3 C31 C36 116.9(4) . . ? O3 C31 C32 121.3(4) . . ? C36 C31 C32 121.6(4) . . ? C33 C32 C31 117.8(4) . . ? C33 C32 C3 120.5(4) . . ? C31 C32 C3 121.6(4) . . ? C32 C33 C34 121.5(4) . . ? C33 C34 C35 119.3(4) . . ? C33 C34 P3 120.5(3) . . ? C35 C34 P3 120.2(3) . . ? C36 C35 C34 120.3(4) . . ? C35 C36 C31 119.3(4) . . ? C35 C36 C2 120.6(4) . . ? C31 C36 C2 120.0(4) . . ? O31 P3 O33 108.3(2) . . ? O31 P3 O32 115.5(2) . . ? O33 P3 O32 107.36(18) . . ? O31 P3 C34 107.3(2) . . ? O33 P3 C34 110.63(19) . . ? O32 P3 C34 107.66(19) . . ? C32 C3 C16 115.4(3) . 2_757 ? O13A N1A O12A 125.8(10) . . ? O13A N1A O11A 119.5(10) . . ? O12A N1A O11A 114.5(6) . . ? O13B N1B O12B 123.9(10) . . ? O13B N1B O11B 115.4(10) . . ? O12B N1B O11B 118.2(10) . . ? O13C N1C O12C 115.4(10) . . ? O13C N1C O11C 137.1(10) . . ? O12C N1C O11C 106.5(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 C17 O1 C11 C12 93.7(5) . . . . ? C17 O1 C11 C16 -89.0(5) . . . . ? O1 C11 C12 C13 177.4(4) . . . . ? C16 C11 C12 C13 0.2(6) . . . . ? O1 C11 C12 C1 -3.2(6) . . . . ? C16 C11 C12 C1 179.7(4) . . . . ? C11 C12 C13 C14 0.0(6) . . . . ? C1 C12 C13 C14 -179.5(4) . . . . ? C12 C13 C14 C15 -0.5(7) . . . . ? C12 C13 C14 P1 -179.6(3) . . . . ? C13 C14 C15 C16 0.8(7) . . . . ? P1 C14 C15 C16 179.9(3) . . . . ? C14 C15 C16 C11 -0.6(7) . . . . ? C14 C15 C16 C3 178.5(4) . . . 2_757 ? C12 C11 C16 C15 0.1(6) . . . . ? O1 C11 C16 C15 -177.1(4) . . . . ? C12 C11 C16 C3 -179.0(4) . . . 2_757 ? O1 C11 C16 C3 3.8(6) . . . 2_757 ? C13 C14 P1 O11 116.7(4) . . . . ? C15 C14 P1 O11 -62.3(4) . . . . ? C13 C14 P1 O12 -10.8(4) . . . . ? C15 C14 P1 O12 170.1(3) . . . . ? C13 C14 P1 O13 -124.3(4) . . . . ? C15 C14 P1 O13 56.6(4) . . . . ? C11 C12 C1 C26 70.5(5) . . . . ? C13 C12 C1 C26 -110.1(4) . . . . ? C27 O2 C21 C22 -85.4(5) . . . . ? C27 O2 C21 C26 95.3(5) . . . . ? C26 C21 C22 C23 4.2(6) . . . . ? O2 C21 C22 C23 -175.1(4) . . . . ? C26 C21 C22 C2 -173.7(4) . . . . ? O2 C21 C22 C2 7.0(6) . . . . ? C21 C22 C23 C24 -3.8(6) . . . . ? C2 C22 C23 C24 174.1(4) . . . . ? C22 C23 C24 C25 0.5(6) . . . . ? C22 C23 C24 P2 178.5(3) . . . . ? C23 C24 C25 C26 2.5(6) . . . . ? P2 C24 C25 C26 -175.5(3) . . . . ? C22 C21 C26 C25 -1.2(6) . . . . ? O2 C21 C26 C25 178.1(3) . . . . ? C22 C21 C26 C1 178.3(4) . . . . ? O2 C21 C26 C1 -2.4(6) . . . . ? C24 C25 C26 C21 -2.2(6) . . . . ? C24 C25 C26 C1 178.3(4) . . . . ? C12 C1 C26 C21 76.5(5) . . . . ? C12 C1 C26 C25 -104.1(5) . . . . ? C25 C24 P2 O21 -41.0(4) . . . . ? C23 C24 P2 O21 141.1(3) . . . . ? C25 C24 P2 O22 81.7(4) . . . . ? C23 C24 P2 O22 -96.3(4) . . . . ? C25 C24 P2 O23 -163.6(3) . . . . ? C23 C24 P2 O23 18.4(4) . . . . ? C21 C22 C2 C36 -128.4(4) . . . . ? C23 C22 C2 C36 53.7(5) . . . . ? C37 O3 C31 C36 -108.6(5) . . . . ? C37 O3 C31 C32 76.1(5) . . . . ? O3 C31 C32 C33 177.5(4) . . . . ? C36 C31 C32 C33 2.4(6) . . . . ? O3 C31 C32 C3 1.1(6) . . . . ? C36 C31 C32 C3 -174.0(4) . . . . ? C31 C32 C33 C34 1.5(6) . . . . ? C3 C32 C33 C34 178.0(4) . . . . ? C32 C33 C34 C35 -3.5(6) . . . . ? C32 C33 C34 P3 176.6(3) . . . . ? C33 C34 C35 C36 1.5(6) . . . . ? P3 C34 C35 C36 -178.5(3) . . . . ? C34 C35 C36 C31 2.3(6) . . . . ? C34 C35 C36 C2 -175.3(4) . . . . ? O3 C31 C36 C35 -179.6(4) . . . . ? C32 C31 C36 C35 -4.3(6) . . . . ? O3 C31 C36 C2 -2.0(6) . . . . ? C32 C31 C36 C2 173.3(4) . . . . ? C22 C2 C36 C35 -109.4(4) . . . . ? C22 C2 C36 C31 73.1(5) . . . . ? C33 C34 P3 O31 179.6(3) . . . . ? C35 C34 P3 O31 -0.4(4) . . . . ? C33 C34 P3 O33 61.6(4) . . . . ? C35 C34 P3 O33 -118.4(3) . . . . ? C33 C34 P3 O32 -55.4(4) . . . . ? C35 C34 P3 O32 124.6(3) . . . . ? C33 C32 C3 C16 82.7(5) . . . 2_757 ? C31 C32 C3 C16 -100.9(5) . . . 2_757 ? 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 O12 H12A O12 0.84 1.68 2.481(6) 158.6 2_758 O13 H13A O21 0.84 1.83 2.672(5) 175.0 1_545 O22 H22A O1W 0.84 1.73 2.558(5) 169.4 . O23 H23A O11 0.84 1.81 2.653(5) 175.7 1_565 O32 H32A O21 0.84 1.71 2.532(4) 163.5 2_767 O33 H33A O3W 0.84 1.76 2.543(5) 154.8 2_657 O11A H11A O2W 0.84 1.72 2.501(7) 153.8 . O11B H11B O11 0.84 1.61 2.450(14) 173.4 2_657 O11C H11C O11 0.84 1.83 2.661(14) 170.1 2_657 O1W H1WA O1 0.85 2.00 2.848(5) 172.6 . O1W H1WB O33 0.85 2.07 2.870(5) 156.4 1_655 O2W H2WA O32 0.88 2.14 2.713(5) 122.0 . O2W H2WB O13 0.87 2.23 2.847(6) 127.3 1_454 O3W H3WA O2 0.85 2.35 3.094(5) 146.0 . O3W H3WA O3 0.85 2.40 2.954(5) 123.2 . O3W H3WB O12 0.85 2.17 3.020(5) 175.7 2_758 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.072 _refine_diff_density_min -0.801 _refine_diff_density_rms 0.094