# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2008 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Colin Raston' _publ_contact_author_email COLIN.RASTON@UWA.EDU.AU _publ_section_title ; Self organised nano-arrays of p-phosphonic acid functionalised higher order calixarenes ; loop_ _publ_author_name 'Colin Raston' 'Jerry L Atwood' 'Thomas E Clark' 'Michael L. Gross' 'Mohamed Makha' 'Henry Rohrs' ; A.N.Sobolev ; 'Dian Su' # Attachment '2c.cif' data_2c _database_code_depnum_ccdc_archive 'CCDC 669055' # start Validation Reply Form _vrf_PLAT761_2c ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: Positions of hydrogen atoms and their atomic displacement parameters were constrained to the bonded atoms during the refinement, using literature data. ; _vrf_PLAT762_2c ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: same, as above ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H35 Br5 O10, 3(C H2 Cl2), 2.25(H2 O)' _chemical_formula_sum 'C48 H45.5 Br5 Cl6 O12.25' _chemical_formula_weight 1430.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 37.319(8) _cell_length_b 15.438(5) _cell_length_c 21.720(6) _cell_angle_alpha 90.0 _cell_angle_beta 115.70(10) _cell_angle_gamma 90.0 _cell_volume 11276(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 992 _cell_measurement_theta_min 3.13 _cell_measurement_theta_max 26.11 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.685 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5668 _exptl_absorpt_coefficient_mu 3.906 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2455 _exptl_absorpt_correction_T_max 0.5089 _exptl_absorpt_process_details 'SADABS - Bruker area detector absorption corrections' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS CCD' _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 38911 _diffrn_reflns_av_R_equivalents 0.0723 _diffrn_reflns_av_sigmaI/netI 0.0839 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 27.18 _reflns_number_total 12406 _reflns_number_gt 7523 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL, v. 5.1' _computing_structure_refinement 'Bruker SHELXTL, v. 5.1' _computing_molecular_graphics 'X-Seed 2.0 (Barbour, 2001)' _computing_publication_material 'Bruker SHELXTL, v. 5.1' _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. To keep integrity of significantly disordered solvent molecules in crystal 6 restraints were used in the refinement. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+121.8194P] 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 12406 _refine_ls_number_parameters 651 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1294 _refine_ls_R_factor_gt 0.0710 _refine_ls_wR_factor_ref 0.1880 _refine_ls_wR_factor_gt 0.1600 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.005 _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 0.12547(14) 0.2889(3) 0.1455(2) 0.0381(11) Uani 1 1 d . . . C11 C 0.15241(19) 0.2563(4) 0.2089(4) 0.0310(15) Uani 1 1 d . . . C12 C 0.13724(19) 0.2142(4) 0.2488(4) 0.0312(15) Uani 1 1 d . . . C13 C 0.1641(2) 0.1840(4) 0.3130(4) 0.0364(16) Uani 1 1 d . . . H13 H 0.1547 0.1542 0.3414 0.044 Uiso 1 1 calc R . . C14 C 0.2047(2) 0.1978(4) 0.3352(4) 0.0352(16) Uani 1 1 d . . . C15 C 0.2190(2) 0.2420(4) 0.2954(3) 0.0322(15) Uani 1 1 d . . . H15 H 0.2468 0.2515 0.3119 0.039 Uiso 1 1 calc R . . C16 C 0.19287(19) 0.2729(4) 0.2308(3) 0.0298(14) Uani 1 1 d . . . O17 O 0.1391(2) 0.1789(5) 0.0914(3) 0.080(2) Uani 1 1 d . . . C17 C 0.1209(2) 0.2430(6) 0.0892(4) 0.052(2) Uani 1 1 d . . . C18 C 0.0890(3) 0.2866(7) 0.0253(4) 0.063(2) Uani 1 1 d . . . H181 H 0.0855 0.2534 -0.0154 0.094 Uiso 1 1 calc R . . H182 H 0.0973 0.3457 0.0215 0.094 Uiso 1 1 calc R . . H183 H 0.0637 0.2885 0.0291 0.094 Uiso 1 1 calc R . . Br1 Br 0.24115(3) 0.15506(6) 0.42157(4) 0.0555(2) Uani 1 1 d . . . C1 C 0.0931(2) 0.1981(5) 0.2236(4) 0.0395(17) Uani 1 1 d . . . H11 H 0.0884 0.1348 0.2210 0.047 Uiso 1 1 calc R . . H12 H 0.0790 0.2216 0.1767 0.047 Uiso 1 1 calc R . . O2 O 0.09403(13) 0.3816(3) 0.2518(2) 0.0359(11) Uani 1 1 d . . . C21 C 0.07320(19) 0.3262(4) 0.2769(3) 0.0329(15) Uani 1 1 d . . . C22 C 0.05438(18) 0.3637(4) 0.3134(3) 0.0326(15) Uani 1 1 d . . . C23 C 0.03715(19) 0.3070(5) 0.3439(3) 0.0363(16) Uani 1 1 d . . . H23 H 0.0239 0.3295 0.3692 0.044 Uiso 1 1 calc R . . C24 C 0.0396(2) 0.2191(5) 0.3367(4) 0.0388(17) Uani 1 1 d . . . C25 C 0.05778(18) 0.1840(5) 0.2994(4) 0.0346(15) Uani 1 1 d . . . H25 H 0.0587 0.1229 0.2949 0.041 Uiso 1 1 calc R . . C26 C 0.07496(19) 0.2382(5) 0.2681(3) 0.0336(15) Uani 1 1 d . . . O27 O 0.04059(19) 0.4119(5) 0.1545(3) 0.092(3) Uani 1 1 d . . . C27 C 0.0754(2) 0.4209(5) 0.1912(4) 0.0464(19) Uani 1 1 d . . . C28 C 0.1029(2) 0.4787(5) 0.1766(4) 0.0472(19) Uani 1 1 d . . . H281 H 0.0883 0.5064 0.1320 0.071 Uiso 1 1 calc R . . H282 H 0.1248 0.4444 0.1762 0.071 Uiso 1 1 calc R . . H283 H 0.1135 0.5233 0.2121 0.071 Uiso 1 1 calc R . . Br2 Br 0.01636(3) 0.14389(6) 0.37936(5) 0.0588(3) Uani 1 1 d . . . C2 C 0.05130(18) 0.4599(5) 0.3198(4) 0.0356(16) Uani 1 1 d . . . H21 H 0.0293 0.4719 0.3324 0.043 Uiso 1 1 calc R . . H22 H 0.0442 0.4864 0.2744 0.043 Uiso 1 1 calc R . . O3 O 0.08623(13) 0.6083(3) 0.2870(2) 0.0362(11) Uani 1 1 d . . . C31 C 0.1037(2) 0.5787(4) 0.3555(3) 0.0333(15) Uani 1 1 d . . . C32 C 0.1371(2) 0.6230(4) 0.4029(3) 0.0330(15) Uani 1 1 d . . . C33 C 0.1552(2) 0.5915(4) 0.4687(3) 0.0341(15) Uani 1 1 d . . . H33 H 0.1775 0.6205 0.5025 0.041 Uiso 1 1 calc R . . C34 C 0.1403(2) 0.5159(5) 0.4852(4) 0.0377(16) Uani 1 1 d . . . C35 C 0.1079(2) 0.4728(5) 0.4382(3) 0.0349(16) Uani 1 1 d . . . H35 H 0.0985 0.4220 0.4511 0.042 Uiso 1 1 calc R . . C36 C 0.08869(19) 0.5035(4) 0.3715(4) 0.0329(15) Uani 1 1 d . . . O37 O 0.0478(2) 0.7002(5) 0.3122(3) 0.084(2) Uani 1 1 d . . . C37 C 0.0575(2) 0.6692(6) 0.2701(4) 0.052(2) Uani 1 1 d . . . C38 C 0.0405(3) 0.6893(7) 0.1957(5) 0.077(3) Uani 1 1 d . . . H381 H 0.0198 0.7338 0.1845 0.116 Uiso 1 1 calc R . . H382 H 0.0288 0.6367 0.1693 0.116 Uiso 1 1 calc R . . H383 H 0.0616 0.7106 0.1843 0.116 Uiso 1 1 calc R . . Br3 Br 0.16609(3) 0.47464(6) 0.57665(4) 0.0518(2) Uani 1 1 d . . . C3 C 0.1527(2) 0.7047(4) 0.3847(4) 0.0379(16) Uani 1 1 d . . . H31 H 0.1727 0.7313 0.4271 0.046 Uiso 1 1 calc R . . H32 H 0.1304 0.7463 0.3636 0.046 Uiso 1 1 calc R . . O4 O 0.22595(14) 0.6157(3) 0.4249(2) 0.0338(10) Uani 1 1 d . . . C41 C 0.2081(2) 0.6473(4) 0.3574(3) 0.0316(14) Uani 1 1 d . . . C42 C 0.1716(2) 0.6898(4) 0.3353(4) 0.0340(15) Uani 1 1 d . . . C43 C 0.1536(2) 0.7159(4) 0.2688(4) 0.0368(16) Uani 1 1 d . . . H43 H 0.1287 0.7449 0.2520 0.044 Uiso 1 1 calc R . . C44 C 0.1715(2) 0.7003(5) 0.2254(4) 0.0393(17) Uani 1 1 d . . . C45 C 0.2066(2) 0.6567(4) 0.2468(4) 0.0342(15) Uani 1 1 d . . . H45 H 0.2176 0.6448 0.2156 0.041 Uiso 1 1 calc R . . C46 C 0.22615(19) 0.6296(4) 0.3141(3) 0.0286(14) Uani 1 1 d . . . O47 O 0.27304(15) 0.7189(3) 0.4562(2) 0.0438(12) Uani 1 1 d . . . C47 C 0.2603(2) 0.6551(5) 0.4698(4) 0.0365(16) Uani 1 1 d . . . C48 C 0.2778(3) 0.6047(6) 0.5347(4) 0.058(2) Uani 1 1 d . . . H481 H 0.3023 0.6327 0.5668 0.088 Uiso 1 1 calc R . . H482 H 0.2837 0.5457 0.5253 0.088 Uiso 1 1 calc R . . H483 H 0.2588 0.6025 0.5548 0.088 Uiso 1 1 calc R . . Br4 Br 0.14491(3) 0.74186(6) 0.13399(4) 0.0624(3) Uani 1 1 d . . . C4 C 0.26626(19) 0.5838(4) 0.3406(3) 0.0317(15) Uani 1 1 d . . . H41 H 0.2872 0.6278 0.3492 0.038 Uiso 1 1 calc R . . H42 H 0.2716 0.5563 0.3849 0.038 Uiso 1 1 calc R . . O5 O 0.20928(12) 0.4469(3) 0.2873(2) 0.0300(10) Uani 1 1 d . . . C51 C 0.24116(17) 0.4486(4) 0.2686(3) 0.0263(13) Uani 1 1 d . . . C52 C 0.24218(18) 0.3853(4) 0.2233(3) 0.0267(13) Uani 1 1 d . . . C53 C 0.27418(19) 0.3881(4) 0.2062(3) 0.0295(14) Uani 1 1 d . . . H53 H 0.2761 0.3460 0.1759 0.035 Uiso 1 1 calc R . . C54 C 0.30287(18) 0.4509(4) 0.2325(3) 0.0295(14) Uani 1 1 d . . . C55 C 0.30071(19) 0.5153(4) 0.2748(3) 0.0305(14) Uani 1 1 d . . . H55 H 0.3206 0.5591 0.2912 0.037 Uiso 1 1 calc R . . C56 C 0.26931(19) 0.5162(4) 0.2937(3) 0.0292(14) Uani 1 1 d . . . O57 O 0.25162(15) 0.4063(3) 0.3943(2) 0.0420(12) Uani 1 1 d . . . C57 C 0.2183(2) 0.4238(4) 0.3534(3) 0.0316(15) Uani 1 1 d . . . C58 C 0.1822(2) 0.4217(5) 0.3663(4) 0.0410(17) Uani 1 1 d . . . H581 H 0.1897 0.4052 0.4139 0.061 Uiso 1 1 calc R . . H582 H 0.1632 0.3794 0.3358 0.061 Uiso 1 1 calc R . . H583 H 0.1698 0.4792 0.3577 0.061 Uiso 1 1 calc R . . Br5 Br 0.34696(2) 0.45040(5) 0.21083(4) 0.0429(2) Uani 1 1 d . . . C5 C 0.20780(19) 0.3234(4) 0.1872(3) 0.0311(14) Uani 1 1 d . . . H51 H 0.1852 0.3571 0.1536 0.037 Uiso 1 1 calc R . . H52 H 0.2159 0.2814 0.1612 0.037 Uiso 1 1 calc R . . C01 C 0.0500(4) 0.9061(8) 0.3428(7) 0.104(4) Uani 1 1 d . . . H01A H 0.0344 0.9523 0.3516 0.124 Uiso 1 1 calc R . . H01B H 0.0358 0.8505 0.3381 0.124 Uiso 1 1 calc R . . Cl11 Cl 0.05402(11) 0.9291(3) 0.2661(2) 0.1287(14) Uani 1 1 d . . . Cl12 Cl 0.09668(14) 0.8998(4) 0.4108(3) 0.1642(19) Uani 1 1 d . . . C02 C 0.1736(4) 0.1785(5) 0.5054(7) 0.032(3) Uiso 0.50 1 d PD A 1 H02A H 0.1957 0.1722 0.4921 0.039 Uiso 0.50 1 calc PR A 1 H02B H 0.1853 0.1920 0.5549 0.039 Uiso 0.50 1 calc PR A 1 Cl21 Cl 0.14389(19) 0.2617(4) 0.4610(3) 0.0965(13) Uiso 0.50 1 d PD A 1 Cl22 Cl 0.14840(19) 0.0836(4) 0.4912(3) 0.0965(13) Uiso 0.50 1 d PD A 1 C03 C 0.0728(7) 0.0153(15) 0.0378(10) 0.101(8) Uiso 0.50 1 d PD B 1 H03A H 0.0664 -0.0342 0.0058 0.122 Uiso 0.50 1 calc PR B 1 H03B H 0.0968 0.0442 0.0392 0.122 Uiso 0.50 1 calc PR B 1 Cl31 Cl 0.0825(3) -0.0222(7) 0.1174(6) 0.168(3) Uiso 0.50 1 d PD B 1 Cl32 Cl 0.0340(3) 0.0869(7) 0.0088(6) 0.168(3) Uiso 0.50 1 d PD B 1 O1W O -0.0338(3) 0.5089(8) 0.0177(6) 0.059(3) Uiso 0.50 1 d P C 1 O2W O 0.0320(6) 0.6529(14) 0.0209(10) 0.080(6) Uiso 0.33 1 d P D 1 C04 C 0.1701(8) 0.1482(10) 0.5130(12) 0.033(6) Uiso 0.25 1 d PD E 2 H04A H 0.1848 0.1311 0.4864 0.039 Uiso 0.25 1 calc PR E 2 H04B H 0.1892 0.1773 0.5550 0.039 Uiso 0.25 1 calc PR E 2 Cl41 Cl 0.1331(4) 0.2255(8) 0.4639(6) 0.088(2) Uiso 0.25 1 d PD E 2 Cl42 Cl 0.1533(4) 0.0518(8) 0.5377(6) 0.088(2) Uiso 0.25 1 d PD E 2 C05 C 0.0499(12) -0.0692(18) 0.121(2) 0.077(12) Uiso 0.25 1 d PD F 2 H05A H 0.0757 -0.0983 0.1471 0.093 Uiso 0.25 1 calc PR F 2 H05B H 0.0379 -0.0596 0.1527 0.093 Uiso 0.25 1 calc PR F 2 Cl51 Cl 0.0599(8) 0.0249(18) 0.1005(13) 0.201(7) Uiso 0.25 1 d PD F 2 Cl52 Cl 0.0221(8) -0.1379(18) 0.0650(13) 0.201(7) Uiso 0.25 1 d PD F 2 O3W O -0.0248(3) 0.5437(7) 0.0362(5) 0.051(3) Uiso 0.50 1 d P G 2 O4W O 0.0373(3) 0.6113(6) 0.0210(5) 0.065(2) Uiso 0.67 1 d P H 2 C06 C 0.1251(8) 0.1729(5) 0.4640(13) 0.032(6) Uiso 0.25 1 d PD I 3 H06A H 0.0978 0.1739 0.4266 0.039 Uiso 0.25 1 calc PR I 3 H06B H 0.1223 0.1734 0.5073 0.039 Uiso 0.25 1 calc PR I 3 Cl61 Cl 0.1463(2) 0.2677(5) 0.4603(4) 0.0419(11) Uiso 0.25 1 d PD I 3 Cl62 Cl 0.1448(2) 0.0756(5) 0.4598(4) 0.0419(11) Uiso 0.25 1 d PD I 3 C07 C 0.0705(11) -0.0596(13) 0.0655(19) 0.063(9) Uiso 0.25 1 d PD J 3 H07A H 0.0651 -0.0762 0.0182 0.076 Uiso 0.25 1 calc PR J 3 H07B H 0.0996 -0.0651 0.0935 0.076 Uiso 0.25 1 calc PR J 3 Cl71 Cl 0.0584(7) 0.0452(14) 0.0648(11) 0.166(5) Uiso 0.25 1 d PD J 3 Cl72 Cl 0.0481(6) -0.1317(14) 0.0943(11) 0.166(5) Uiso 0.25 1 d PD J 3 O5W O 0.0000 0.5000 0.0000 0.130(9) Uiso 0.50 2 d SP K 3 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 0.033(3) 0.036(3) 0.048(3) 0.002(2) 0.020(2) 0.002(2) C11 0.031(4) 0.023(3) 0.047(4) -0.009(3) 0.025(3) -0.003(3) C12 0.030(3) 0.029(3) 0.048(4) -0.008(3) 0.029(3) -0.002(3) C13 0.048(4) 0.027(4) 0.048(4) -0.008(3) 0.034(4) -0.003(3) C14 0.033(4) 0.037(4) 0.043(4) -0.010(3) 0.024(3) -0.007(3) C15 0.033(4) 0.027(4) 0.047(4) -0.006(3) 0.027(3) -0.001(3) C16 0.037(4) 0.019(3) 0.043(4) -0.007(3) 0.026(3) -0.005(3) O17 0.069(4) 0.092(5) 0.062(4) -0.034(4) 0.013(3) 0.021(4) C17 0.026(4) 0.080(7) 0.051(5) -0.003(4) 0.016(4) -0.006(4) C18 0.051(5) 0.090(7) 0.040(4) 0.003(4) 0.014(4) -0.021(5) Br1 0.0547(5) 0.0604(6) 0.0509(5) 0.0134(4) 0.0226(4) 0.0053(4) C1 0.033(4) 0.037(4) 0.057(5) -0.013(3) 0.027(4) -0.009(3) O2 0.027(2) 0.040(3) 0.050(3) 0.002(2) 0.025(2) -0.002(2) C21 0.024(3) 0.039(4) 0.041(4) 0.004(3) 0.019(3) -0.001(3) C22 0.023(3) 0.040(4) 0.039(4) 0.001(3) 0.017(3) 0.002(3) C23 0.027(4) 0.050(5) 0.038(4) 0.002(3) 0.020(3) 0.003(3) C24 0.032(4) 0.049(5) 0.044(4) 0.013(3) 0.025(3) 0.002(3) C25 0.026(4) 0.033(4) 0.052(4) 0.002(3) 0.024(3) 0.001(3) C26 0.022(3) 0.041(4) 0.042(4) -0.001(3) 0.019(3) -0.003(3) O27 0.050(4) 0.146(7) 0.067(4) 0.049(4) 0.013(3) -0.037(4) C27 0.048(5) 0.052(5) 0.053(5) 0.002(4) 0.034(4) -0.006(4) C28 0.054(5) 0.040(4) 0.067(5) 0.003(4) 0.044(4) -0.005(4) Br2 0.0582(5) 0.0630(6) 0.0761(6) 0.0270(5) 0.0488(5) 0.0095(4) C2 0.020(3) 0.046(4) 0.048(4) 0.001(3) 0.022(3) 0.005(3) O3 0.036(3) 0.038(3) 0.043(3) 0.002(2) 0.025(2) 0.005(2) C31 0.040(4) 0.033(4) 0.040(4) -0.003(3) 0.030(3) 0.007(3) C32 0.038(4) 0.032(4) 0.043(4) -0.006(3) 0.032(3) 0.005(3) C33 0.034(4) 0.038(4) 0.041(4) -0.008(3) 0.027(3) -0.001(3) C34 0.040(4) 0.041(4) 0.045(4) 0.003(3) 0.031(3) 0.009(3) C35 0.031(4) 0.038(4) 0.045(4) -0.003(3) 0.024(3) -0.004(3) C36 0.028(4) 0.036(4) 0.045(4) -0.005(3) 0.025(3) -0.001(3) O37 0.070(4) 0.122(6) 0.066(4) 0.010(4) 0.036(4) 0.057(4) C37 0.045(5) 0.060(5) 0.056(5) 0.004(4) 0.026(4) 0.015(4) C38 0.066(6) 0.098(8) 0.068(6) 0.028(6) 0.030(5) 0.040(6) Br3 0.0614(5) 0.0561(5) 0.0406(4) 0.0033(4) 0.0247(4) 0.0045(4) C3 0.040(4) 0.036(4) 0.052(4) -0.007(3) 0.033(4) -0.002(3) O4 0.044(3) 0.030(2) 0.037(3) -0.002(2) 0.026(2) -0.001(2) C41 0.038(4) 0.026(3) 0.039(4) -0.001(3) 0.024(3) -0.003(3) C42 0.041(4) 0.029(4) 0.046(4) -0.002(3) 0.031(3) 0.001(3) C43 0.038(4) 0.032(4) 0.052(4) 0.002(3) 0.030(4) 0.002(3) C44 0.053(5) 0.033(4) 0.038(4) 0.000(3) 0.026(4) -0.004(3) C45 0.041(4) 0.029(4) 0.046(4) -0.005(3) 0.031(3) -0.006(3) C46 0.034(4) 0.019(3) 0.047(4) -0.007(3) 0.030(3) -0.007(3) O47 0.055(3) 0.040(3) 0.043(3) -0.011(2) 0.027(3) -0.009(3) C47 0.043(4) 0.033(4) 0.044(4) -0.015(3) 0.028(3) -0.006(3) C48 0.068(6) 0.064(6) 0.045(5) 0.005(4) 0.026(4) 0.005(5) Br4 0.0774(6) 0.0706(6) 0.0477(5) 0.0149(4) 0.0352(5) 0.0193(5) C4 0.029(4) 0.029(3) 0.043(4) -0.009(3) 0.022(3) -0.009(3) O5 0.030(2) 0.030(2) 0.039(2) -0.004(2) 0.024(2) 0.0011(19) C51 0.024(3) 0.026(3) 0.041(4) -0.002(3) 0.024(3) -0.002(3) C52 0.028(3) 0.026(3) 0.031(3) 0.000(3) 0.018(3) 0.000(3) C53 0.036(4) 0.021(3) 0.042(4) -0.004(3) 0.027(3) 0.003(3) C54 0.027(3) 0.032(4) 0.041(4) 0.001(3) 0.026(3) 0.003(3) C55 0.030(4) 0.026(3) 0.041(4) -0.008(3) 0.022(3) -0.005(3) C56 0.031(3) 0.027(3) 0.033(3) -0.003(3) 0.018(3) -0.001(3) O57 0.041(3) 0.046(3) 0.044(3) 0.004(2) 0.023(3) 0.003(2) C57 0.041(4) 0.025(3) 0.036(4) -0.008(3) 0.024(3) -0.003(3) C58 0.044(4) 0.044(4) 0.052(4) -0.011(3) 0.037(4) -0.009(3) Br5 0.0401(4) 0.0385(4) 0.0709(5) -0.0094(4) 0.0436(4) -0.0068(3) C5 0.036(4) 0.029(4) 0.037(4) -0.005(3) 0.025(3) -0.002(3) C01 0.100(10) 0.086(9) 0.155(12) -0.010(8) 0.083(10) -0.007(7) Cl11 0.107(3) 0.121(3) 0.207(4) 0.006(3) 0.114(3) -0.013(2) Cl12 0.121(4) 0.181(5) 0.191(5) -0.066(4) 0.068(3) -0.023(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 O1 C17 1.359(10) . ? O1 C11 1.400(8) . ? C11 C12 1.384(9) . ? C11 C16 1.396(9) . ? C12 C13 1.399(10) . ? C12 C1 1.515(9) . ? C13 C14 1.393(9) . ? C14 C15 1.379(9) . ? C14 Br1 1.896(7) . ? C15 C16 1.401(9) . ? C16 C5 1.506(8) . ? O17 C17 1.191(10) . ? C17 C18 1.537(12) . ? C1 C26 1.531(9) . ? O2 C27 1.338(9) . ? O2 C21 1.414(7) . ? C21 C26 1.377(10) . ? C21 C22 1.393(9) . ? C22 C23 1.409(9) . ? C22 C2 1.501(10) . ? C23 C24 1.373(10) . ? C24 C25 1.374(9) . ? C24 Br2 1.912(6) . ? C25 C26 1.396(9) . ? O27 C27 1.201(9) . ? C27 C28 1.495(10) . ? C2 C36 1.518(9) . ? O3 C37 1.352(9) . ? O3 C31 1.416(8) . ? C31 C36 1.397(9) . ? C31 C32 1.403(10) . ? C32 C33 1.378(9) . ? C32 C3 1.511(9) . ? C33 C34 1.405(10) . ? C34 C35 1.370(10) . ? C34 Br3 1.902(7) . ? C35 C36 1.391(10) . ? O37 C37 1.218(9) . ? C37 C38 1.492(12) . ? C3 C42 1.537(8) . ? O4 C47 1.370(8) . ? O4 C41 1.407(8) . ? C41 C42 1.397(9) . ? C41 C46 1.401(8) . ? C42 C43 1.363(10) . ? C43 C44 1.393(9) . ? C44 C45 1.362(10) . ? C44 Br4 1.905(7) . ? C45 C46 1.386(9) . ? C46 C4 1.524(9) . ? O47 C47 1.187(8) . ? C47 C48 1.491(11) . ? C4 C56 1.498(9) . ? O5 C57 1.372(8) . ? O5 C51 1.414(6) . ? C51 C52 1.400(8) . ? C51 C56 1.412(9) . ? C52 C53 1.396(8) . ? C52 C5 1.517(9) . ? C53 C54 1.371(9) . ? C54 C55 1.380(9) . ? C54 Br5 1.898(6) . ? C55 C56 1.398(8) . ? O57 C57 1.205(8) . ? C57 C58 1.491(9) . ? C01 Cl12 1.731(14) . ? C01 Cl11 1.772(13) . ? C02 Cl22 1.696(10) . ? C02 Cl21 1.698(10) . ? C03 Cl31 1.706(17) . ? C03 Cl32 1.711(17) . ? C04 Cl42 1.784(17) . ? C04 Cl41 1.785(17) . ? C05 Cl52 1.61(3) . ? C05 Cl51 1.61(3) . ? C06 Cl61 1.683(14) . ? C06 Cl62 1.691(14) . ? C07 Cl72 1.67(2) . ? C07 Cl71 1.68(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 C17 O1 C11 117.0(6) . . ? C12 C11 C16 123.3(6) . . ? C12 C11 O1 118.0(6) . . ? C16 C11 O1 118.5(6) . . ? C11 C12 C13 118.1(6) . . ? C11 C12 C1 121.8(6) . . ? C13 C12 C1 120.1(6) . . ? C14 C13 C12 119.6(6) . . ? C15 C14 C13 121.3(7) . . ? C15 C14 Br1 119.0(5) . . ? C13 C14 Br1 119.7(5) . . ? C14 C15 C16 120.3(6) . . ? C11 C16 C15 117.4(6) . . ? C11 C16 C5 121.4(6) . . ? C15 C16 C5 121.2(6) . . ? O17 C17 O1 123.3(8) . . ? O17 C17 C18 127.4(8) . . ? O1 C17 C18 109.3(8) . . ? C12 C1 C26 114.5(6) . . ? C27 O2 C21 120.9(5) . . ? C26 C21 C22 123.7(6) . . ? C26 C21 O2 118.5(5) . . ? C22 C21 O2 117.7(6) . . ? C21 C22 C23 117.1(6) . . ? C21 C22 C2 122.8(6) . . ? C23 C22 C2 120.1(6) . . ? C24 C23 C22 119.6(6) . . ? C23 C24 C25 122.0(6) . . ? C23 C24 Br2 118.6(5) . . ? C25 C24 Br2 119.3(6) . . ? C24 C25 C26 119.9(7) . . ? C21 C26 C25 117.7(6) . . ? C21 C26 C1 123.1(6) . . ? C25 C26 C1 119.2(6) . . ? O27 C27 O2 123.6(7) . . ? O27 C27 C28 124.8(8) . . ? O2 C27 C28 111.5(7) . . ? C22 C2 C36 115.2(6) . . ? C37 O3 C31 117.4(5) . . ? C36 C31 C32 123.2(6) . . ? C36 C31 O3 118.6(6) . . ? C32 C31 O3 118.1(6) . . ? C33 C32 C31 117.9(6) . . ? C33 C32 C3 119.8(6) . . ? C31 C32 C3 122.3(6) . . ? C32 C33 C34 119.3(7) . . ? C35 C34 C33 122.1(7) . . ? C35 C34 Br3 120.0(5) . . ? C33 C34 Br3 117.9(6) . . ? C34 C35 C36 120.0(6) . . ? C35 C36 C31 117.5(6) . . ? C35 C36 C2 120.8(6) . . ? C31 C36 C2 121.6(6) . . ? O37 C37 O3 122.0(7) . . ? O37 C37 C38 127.3(8) . . ? O3 C37 C38 110.7(7) . . ? C32 C3 C42 113.7(5) . . ? C47 O4 C41 117.5(5) . . ? C42 C41 C46 122.8(6) . . ? C42 C41 O4 118.1(5) . . ? C46 C41 O4 119.0(6) . . ? C43 C42 C41 117.5(6) . . ? C43 C42 C3 122.0(6) . . ? C41 C42 C3 120.4(6) . . ? C42 C43 C44 120.4(7) . . ? C45 C44 C43 121.8(7) . . ? C45 C44 Br4 120.8(5) . . ? C43 C44 Br4 117.4(6) . . ? C44 C45 C46 119.8(6) . . ? C45 C46 C41 117.6(6) . . ? C45 C46 C4 121.4(5) . . ? C41 C46 C4 121.0(6) . . ? O47 C47 O4 122.9(7) . . ? O47 C47 C48 127.6(7) . . ? O4 C47 C48 109.5(6) . . ? C56 C4 C46 114.7(5) . . ? C57 O5 C51 116.8(5) . . ? C52 C51 C56 123.0(5) . . ? C52 C51 O5 118.1(5) . . ? C56 C51 O5 118.8(5) . . ? C53 C52 C51 116.9(6) . . ? C53 C52 C5 120.8(5) . . ? C51 C52 C5 121.9(5) . . ? C54 C53 C52 121.0(6) . . ? C53 C54 C55 121.8(5) . . ? C53 C54 Br5 119.9(4) . . ? C55 C54 Br5 118.4(5) . . ? C54 C55 C56 120.0(6) . . ? C55 C56 C51 117.3(5) . . ? C55 C56 C4 121.8(6) . . ? C51 C56 C4 120.9(5) . . ? O57 C57 O5 122.4(6) . . ? O57 C57 C58 125.8(6) . . ? O5 C57 C58 111.8(6) . . ? C16 C5 C52 117.5(5) . . ? Cl12 C01 Cl11 110.3(7) . . ? Cl22 C02 Cl21 112.0(8) . . ? Cl31 C03 Cl32 111.5(16) . . ? Cl42 C04 Cl41 117.1(15) . . ? Cl52 C05 Cl51 123(3) . . ? Cl61 C06 Cl62 123.1(16) . . ? Cl72 C07 Cl71 118(2) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.18 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.927 _refine_diff_density_min -0.932 _refine_diff_density_rms 0.122 # Attachment '2d.cif' data_2d _database_code_depnum_ccdc_archive 'CCDC 669056' # start Validation Reply Form _vrf_PLAT220_2d ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.81 Ratio RESPONSE: The refinement of chemically sensible disordered groups was employed only for "well-behaved" disorder. Some minor disorder, which was not accounted, can lead to some uncertainty in values of ADP. ; _vrf_PLAT222_2d ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.79 Ratio RESPONSE: Termal parameters of H-atoms was constrained to the bonded atoms. ; _vrf_PLAT761_2d ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: Positions of hydrogen atoms and their atomic displacement parameters were constrained to the bonded atoms during the refinement, using literature data. ; _vrf_PLAT762_2d ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: same, as above ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common P(O)(OEt)2-OAc-Calix(5) _chemical_melting_point ? _chemical_formula_moiety 'C65 H85 O25 P5' _chemical_formula_sum 'C65 H85 O25 P5' _chemical_formula_weight 1421.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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 12.9938(4) _cell_length_b 16.3618(5) _cell_length_c 18.4136(6) _cell_angle_alpha 100.825(3) _cell_angle_beta 94.164(3) _cell_angle_gamma 112.261(3) _cell_volume 3513.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10400 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 66.99 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1500 _exptl_absorpt_coefficient_mu 1.873 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8806 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini-R Ultra, Ruby CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4738 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41009 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 66.99 _reflns_number_total 12348 _reflns_number_gt 7153 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed 2.0 (Barbour, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. To keep integrity one of the P(O)(OEt)2 groups with relatively high values of ADP, 2 geometry restraints were used in the refinement. ; _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^)+(0.1450P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12348 _refine_ls_number_parameters 854 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1128 _refine_ls_R_factor_gt 0.0731 _refine_ls_wR_factor_ref 0.2280 _refine_ls_wR_factor_gt 0.1995 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.010 _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 O1 O 0.1819(2) 0.40387(18) 0.15812(15) 0.0350(6) Uani 1 1 d . . . C11 C 0.1174(4) 0.3279(3) 0.1008(2) 0.0348(9) Uani 1 1 d . . . C12 C 0.1284(4) 0.2455(3) 0.0997(2) 0.0395(10) Uani 1 1 d . . . C13 C 0.0595(4) 0.1697(3) 0.0440(3) 0.0441(10) Uani 1 1 d . . . H13 H 0.0639 0.1128 0.0429 0.053 Uiso 1 1 calc R . . C14 C -0.0164(4) 0.1763(3) -0.0105(2) 0.0415(10) Uani 1 1 d . . . C15 C -0.0251(4) 0.2593(3) -0.0064(2) 0.0387(9) Uani 1 1 d . . . H15 H -0.0775 0.2636 -0.0427 0.046 Uiso 1 1 calc R . . C16 C 0.0398(4) 0.3350(3) 0.0486(2) 0.0350(9) Uani 1 1 d . . . O17 O 0.3340(3) 0.4217(2) 0.10265(18) 0.0460(7) Uani 1 1 d . . . C17 C 0.2933(4) 0.4490(3) 0.1519(2) 0.0381(10) Uani 1 1 d . . . C18 C 0.3485(4) 0.5316(3) 0.2141(2) 0.0426(10) Uani 1 1 d . . . H18A H 0.4276 0.5627 0.2089 0.064 Uiso 1 1 calc R . . H18B H 0.3443 0.5140 0.2621 0.064 Uiso 1 1 calc R . . H18C H 0.3100 0.5725 0.2121 0.064 Uiso 1 1 calc R . . P1 P -0.10222(11) 0.08129(8) -0.08445(7) 0.0468(3) Uani 1 1 d . A . O11 O -0.1886(3) 0.0986(2) -0.12748(19) 0.0541(8) Uani 1 1 d . . . O12 O -0.0200(3) 0.0526(3) -0.13000(19) 0.0633(9) Uani 1 1 d . . . C121 C 0.0296(8) 0.0965(6) -0.1844(5) 0.047(2) Uiso 0.50 1 d P A 1 H12A H 0.0669 0.1628 -0.1630 0.057 Uiso 0.50 1 calc PR A 1 H12B H -0.0290 0.0854 -0.2269 0.057 Uiso 0.50 1 calc PR A 1 C122 C 0.1170(12) 0.0604(10) -0.2123(8) 0.078(3) Uiso 0.50 1 d P A 1 H12C H 0.1494 0.0895 -0.2520 0.117 Uiso 0.50 1 calc PR A 1 H12D H 0.0801 -0.0055 -0.2321 0.117 Uiso 0.50 1 calc PR A 1 H12E H 0.1769 0.0744 -0.1706 0.117 Uiso 0.50 1 calc PR A 1 C12' C -0.0459(16) 0.0137(13) -0.2047(10) 0.111(5) Uiso 0.50 1 d P A 2 H12F H -0.0844 0.0449 -0.2302 0.133 Uiso 0.50 1 calc PR A 2 H12G H -0.0983 -0.0508 -0.2128 0.133 Uiso 0.50 1 calc PR A 2 C12" C 0.0603(16) 0.0193(13) -0.2387(11) 0.110(5) Uiso 0.50 1 d P A 2 H12H H 0.0390 -0.0117 -0.2918 0.166 Uiso 0.50 1 calc PR A 2 H12I H 0.0998 -0.0098 -0.2124 0.166 Uiso 0.50 1 calc PR A 2 H12J H 0.1100 0.0832 -0.2335 0.166 Uiso 0.50 1 calc PR A 2 O13 O -0.1468(3) -0.0034(2) -0.0485(2) 0.0558(9) Uani 1 1 d . . . C131 C -0.2224(6) -0.0065(4) 0.0052(4) 0.0807(19) Uani 1 1 d . A . H13A H -0.2738 0.0216 -0.0091 0.097 Uiso 1 1 calc R . . H13B H -0.1784 0.0292 0.0551 0.097 Uiso 1 1 calc R . . C132 C -0.2879(8) -0.0983(6) 0.0098(8) 0.162(6) Uani 1 1 d . . . H13C H -0.3416 -0.0981 0.0445 0.243 Uiso 1 1 calc R A . H13D H -0.2376 -0.1247 0.0279 0.243 Uiso 1 1 calc R . . H13E H -0.3290 -0.1345 -0.0400 0.243 Uiso 1 1 calc R . . C1 C 0.2118(4) 0.2397(3) 0.1580(2) 0.0426(10) Uani 1 1 d . . . H1A H 0.2047 0.1761 0.1496 0.051 Uiso 1 1 calc R . . H1B H 0.2889 0.2777 0.1514 0.051 Uiso 1 1 calc R . . O2 O 0.3929(2) 0.37146(18) 0.27463(15) 0.0384(7) Uani 1 1 d . . . C21 C 0.2849(4) 0.3319(3) 0.2935(2) 0.0367(9) Uani 1 1 d . . . C22 C 0.2714(4) 0.3620(3) 0.3665(2) 0.0345(9) Uani 1 1 d . . . C23 C 0.1622(4) 0.3306(3) 0.3834(2) 0.0372(9) Uani 1 1 d . . . H23 H 0.1498 0.3505 0.4325 0.045 Uiso 1 1 calc R . . C24 C 0.0713(4) 0.2706(3) 0.3293(3) 0.0410(10) Uani 1 1 d . . . C25 C 0.0892(4) 0.2401(3) 0.2572(2) 0.0423(10) Uani 1 1 d . . . H25 H 0.0269 0.1979 0.2209 0.051 Uiso 1 1 calc R . . C26 C 0.1961(4) 0.2702(3) 0.2373(2) 0.0391(10) Uani 1 1 d . . . O27 O 0.4134(3) 0.2391(2) 0.2587(2) 0.0633(10) Uani 1 1 d . . . C27 C 0.4501(4) 0.3168(3) 0.2551(3) 0.0482(11) Uani 1 1 d . . . C28 C 0.5534(5) 0.3671(4) 0.2284(3) 0.0577(13) Uani 1 1 d . . . H28A H 0.5935 0.3277 0.2149 0.087 Uiso 1 1 calc R . . H28B H 0.6016 0.4201 0.2679 0.087 Uiso 1 1 calc R . . H28C H 0.5346 0.3872 0.1842 0.087 Uiso 1 1 calc R . . P2 P -0.06807(10) 0.23747(8) 0.35179(7) 0.0480(3) Uani 1 1 d . . . O21 O -0.0835(3) 0.3097(2) 0.4048(2) 0.0563(9) Uani 1 1 d . . . O22 O -0.1495(3) 0.2009(2) 0.2733(2) 0.0569(9) Uani 1 1 d . . . C221 C -0.1657(6) 0.2651(4) 0.2330(4) 0.0793(19) Uani 1 1 d . . . H22A H -0.0936 0.3185 0.2394 0.095 Uiso 1 1 calc R . . H22B H -0.2214 0.2864 0.2542 0.095 Uiso 1 1 calc R . . C222 C -0.2055(6) 0.2225(5) 0.1525(4) 0.089(2) Uani 1 1 d . . . H22C H -0.2245 0.2641 0.1278 0.134 Uiso 1 1 calc R . . H22D H -0.2724 0.1660 0.1464 0.134 Uiso 1 1 calc R . . H22E H -0.1460 0.2089 0.1300 0.134 Uiso 1 1 calc R . . O23 O -0.0877(3) 0.1475(2) 0.3780(2) 0.0623(10) Uani 1 1 d . . . C231 C -0.1828(5) 0.1069(4) 0.4145(4) 0.0793(19) Uani 1 1 d . . . H23A H -0.2540 0.0883 0.3800 0.095 Uiso 1 1 calc R . . H23B H -0.1821 0.1513 0.4594 0.095 Uiso 1 1 calc R . . C232 C -0.1751(7) 0.0268(5) 0.4364(5) 0.100(2) Uani 1 1 d . . . H23C H -0.2392 -0.0016 0.4612 0.150 Uiso 1 1 calc R . . H23D H -0.1047 0.0458 0.4708 0.150 Uiso 1 1 calc R . . H23E H -0.1762 -0.0169 0.3916 0.150 Uiso 1 1 calc R . . C2 C 0.3718(3) 0.4266(3) 0.4249(2) 0.0350(9) Uani 1 1 d . . . H2A H 0.4334 0.4052 0.4209 0.042 Uiso 1 1 calc R . . H2B H 0.3504 0.4238 0.4752 0.042 Uiso 1 1 calc R . . O3 O 0.2614(2) 0.54279(18) 0.47314(16) 0.0401(7) Uani 1 1 d . . . C31 C 0.3616(3) 0.5814(3) 0.4451(2) 0.0347(9) Uani 1 1 d . . . C32 C 0.3989(4) 0.6712(3) 0.4406(2) 0.0367(9) Uani 1 1 d . . . C33 C 0.4969(4) 0.7073(3) 0.4110(2) 0.0378(9) Uani 1 1 d . . . H33 H 0.5257 0.7693 0.4088 0.045 Uiso 1 1 calc R . . C34 C 0.5534(4) 0.6533(3) 0.3845(2) 0.0377(9) Uani 1 1 d . . . C35 C 0.5121(4) 0.5625(3) 0.3884(2) 0.0371(9) Uani 1 1 d . . . H35 H 0.5507 0.5260 0.3698 0.045 Uiso 1 1 calc R . . C36 C 0.4163(3) 0.5249(3) 0.4188(2) 0.0346(9) Uani 1 1 d . . . O37 O 0.3595(3) 0.5904(3) 0.58970(18) 0.0562(9) Uani 1 1 d . . . C37 C 0.2708(4) 0.5532(3) 0.5490(3) 0.0426(10) Uani 1 1 d . . . C38 C 0.1589(5) 0.5158(4) 0.5716(3) 0.0593(14) Uani 1 1 d . . . H38A H 0.1674 0.5245 0.6262 0.089 Uiso 1 1 calc R . . H38B H 0.1213 0.4508 0.5480 0.089 Uiso 1 1 calc R . . H38C H 0.1134 0.5473 0.5557 0.089 Uiso 1 1 calc R . . P3 P 0.67564(11) 0.69667(8) 0.34182(8) 0.0510(3) Uani 1 1 d . . . O31 O 0.6793(4) 0.6300(3) 0.2782(2) 0.0728(11) Uani 1 1 d . . . O32 O 0.6792(3) 0.7874(2) 0.32234(18) 0.0514(8) Uani 1 1 d . . . C321 C 0.5975(6) 0.7833(4) 0.2599(3) 0.0737(17) Uani 1 1 d . . . H32A H 0.6242 0.7707 0.2117 0.088 Uiso 1 1 calc R . . H32B H 0.5236 0.7336 0.2584 0.088 Uiso 1 1 calc R . . C322 C 0.5858(7) 0.8710(5) 0.2711(4) 0.094(2) Uani 1 1 d . . . H32C H 0.5358 0.8701 0.2282 0.141 Uiso 1 1 calc R . . H32D H 0.6600 0.9203 0.2755 0.141 Uiso 1 1 calc R . . H32E H 0.5539 0.8808 0.3169 0.141 Uiso 1 1 calc R . . O33 O 0.7760(3) 0.7326(3) 0.4087(3) 0.0737(12) Uani 1 1 d . . . C331 C 0.8870(5) 0.7361(5) 0.4006(5) 0.096(2) Uani 1 1 d . . . H33A H 0.9264 0.7401 0.4500 0.115 Uiso 1 1 calc R . . H33B H 0.8797 0.6789 0.3666 0.115 Uiso 1 1 calc R . . C332 C 0.9540(6) 0.8111(5) 0.3717(5) 0.097(2) Uani 1 1 d . . . H33C H 1.0279 0.8095 0.3672 0.146 Uiso 1 1 calc R . . H33D H 0.9637 0.8681 0.4058 0.146 Uiso 1 1 calc R . . H33E H 0.9163 0.8071 0.3223 0.146 Uiso 1 1 calc R . . C3 C 0.3377(4) 0.7312(3) 0.4687(2) 0.0420(10) Uani 1 1 d . . . H3A H 0.3837 0.7762 0.5149 0.050 Uiso 1 1 calc R . . H3B H 0.2653 0.6930 0.4820 0.050 Uiso 1 1 calc R . . O4 O 0.2044(2) 0.64026(17) 0.32549(15) 0.0338(6) Uani 1 1 d . . . C41 C 0.2436(4) 0.7350(3) 0.3448(2) 0.0365(9) Uani 1 1 d . . . C42 C 0.2131(4) 0.7790(3) 0.2940(2) 0.0385(9) Uani 1 1 d . . . C43 C 0.2571(4) 0.8728(3) 0.3127(3) 0.0548(13) Uani 1 1 d . . . H43 H 0.2396 0.9045 0.2787 0.066 Uiso 1 1 calc R . . C44 C 0.3269(5) 0.9215(3) 0.3806(3) 0.0645(15) Uani 1 1 d . . . C45 C 0.3546(4) 0.8756(3) 0.4299(3) 0.0567(13) Uani 1 1 d . . . H45 H 0.4018 0.9091 0.4764 0.068 Uiso 1 1 calc R . . C46 C 0.3141(4) 0.7816(3) 0.4121(3) 0.0416(10) Uani 1 1 d . . . O47 O 0.0443(3) 0.6285(2) 0.3697(2) 0.0575(9) Uani 1 1 d . . . C47 C 0.1023(4) 0.5925(3) 0.3429(2) 0.0406(10) Uani 1 1 d . . . C48 C 0.0759(4) 0.4937(3) 0.3243(3) 0.0448(10) Uani 1 1 d . . . H48A H 0.0021 0.4606 0.3373 0.067 Uiso 1 1 calc R . . H48B H 0.1336 0.4821 0.3527 0.067 Uiso 1 1 calc R . . H48C H 0.0747 0.4733 0.2706 0.067 Uiso 1 1 calc R . . P4 P 0.37446(15) 1.04299(10) 0.41099(11) 0.0801(5) Uani 1 1 d D . . O41 O 0.4067(4) 1.0806(3) 0.4915(3) 0.0908(15) Uani 1 1 d . . . O42 O 0.4793(3) 1.0777(4) 0.3725(2) 0.1075(18) Uani 1 1 d D . . C421 C 0.4612(6) 1.0661(4) 0.2927(3) 0.087(2) Uani 1 1 d D . . H42A H 0.3973 1.0813 0.2774 0.104 Uiso 1 1 calc R . . H42B H 0.4435 1.0023 0.2674 0.104 Uiso 1 1 calc R . . C422 C 0.5656(7) 1.1274(7) 0.2718(7) 0.137(4) Uani 1 1 d . . . H42C H 0.5538 1.1243 0.2180 0.205 Uiso 1 1 calc R . . H42D H 0.6270 1.1088 0.2837 0.205 Uiso 1 1 calc R . . H42E H 0.5852 1.1899 0.2999 0.205 Uiso 1 1 calc R . . O43 O 0.2772(5) 1.0609(3) 0.3712(3) 0.0981(17) Uani 1 1 d . . . C431 C 0.2609(6) 1.1428(4) 0.3970(4) 0.0760(18) Uani 1 1 d . . . H43A H 0.2600 1.1727 0.3551 0.091 Uiso 1 1 calc R . . H43B H 0.3241 1.1851 0.4367 0.091 Uiso 1 1 calc R . . C432 C 0.1548(10) 1.1227(7) 0.4265(6) 0.154(5) Uani 1 1 d . . . H43C H 0.1447 1.1792 0.4436 0.232 Uiso 1 1 calc R . . H43D H 0.1563 1.0942 0.4686 0.232 Uiso 1 1 calc R . . H43E H 0.0922 1.0813 0.3870 0.232 Uiso 1 1 calc R . . C4 C 0.1254(4) 0.7268(3) 0.2253(2) 0.0399(10) Uani 1 1 d . . . H4A H 0.1107 0.7711 0.2007 0.048 Uiso 1 1 calc R . . H4B H 0.0546 0.6909 0.2416 0.048 Uiso 1 1 calc R . . O5 O -0.0120(2) 0.53564(18) 0.17597(15) 0.0370(6) Uani 1 1 d . . . C51 C 0.0842(3) 0.5724(3) 0.1425(2) 0.0349(9) Uani 1 1 d . . . C52 C 0.1033(3) 0.5129(3) 0.0851(2) 0.0338(9) Uani 1 1 d . . . C53 C 0.1994(4) 0.5488(3) 0.0537(2) 0.0382(10) Uani 1 1 d . . . H53 H 0.2155 0.5108 0.0145 0.046 Uiso 1 1 calc R . . C54 C 0.2730(4) 0.6399(3) 0.0786(2) 0.0401(10) Uani 1 1 d . . . C55 C 0.2500(4) 0.6960(3) 0.1354(2) 0.0386(9) Uani 1 1 d . . . H55 H 0.3005 0.7580 0.1523 0.046 Uiso 1 1 calc R . . C56 C 0.1546(4) 0.6630(3) 0.1675(2) 0.0371(9) Uani 1 1 d . . . O57 O -0.1001(3) 0.5993(2) 0.10991(18) 0.0471(7) Uani 1 1 d . . . C57 C -0.1031(4) 0.5537(3) 0.1539(2) 0.0404(10) Uani 1 1 d . . . C58 C -0.1993(4) 0.5089(4) 0.1906(3) 0.0513(11) Uani 1 1 d . . . H58A H -0.2629 0.5229 0.1741 0.077 Uiso 1 1 calc R . . H58B H -0.1778 0.5311 0.2451 0.077 Uiso 1 1 calc R . . H58C H -0.2212 0.4431 0.1771 0.077 Uiso 1 1 calc R . . P5 P 0.39453(10) 0.68456(9) 0.03441(7) 0.0477(3) Uani 1 1 d . . . O51 O 0.3711(3) 0.6596(3) -0.0471(2) 0.0674(10) Uani 1 1 d . . . O52 O 0.4476(3) 0.7909(2) 0.0676(2) 0.0584(9) Uani 1 1 d . . . C521 C 0.4041(6) 0.8494(4) 0.0332(4) 0.0782(19) Uani 1 1 d . . . H52A H 0.3208 0.8248 0.0270 0.094 Uiso 1 1 calc R . . H52B H 0.4276 0.8535 -0.0164 0.094 Uiso 1 1 calc R . . C522 C 0.4579(7) 0.9458(5) 0.0900(5) 0.100(2) Uani 1 1 d . . . H52C H 0.4303 0.9875 0.0718 0.150 Uiso 1 1 calc R . . H52D H 0.5401 0.9698 0.0941 0.150 Uiso 1 1 calc R . . H52E H 0.4365 0.9398 0.1393 0.150 Uiso 1 1 calc R . . O53 O 0.4805(3) 0.6543(2) 0.07449(18) 0.0517(8) Uani 1 1 d . . . C531 C 0.5835(5) 0.6594(5) 0.0461(3) 0.0689(15) Uani 1 1 d . . . H53A H 0.6403 0.7228 0.0599 0.083 Uiso 1 1 calc R . . H53B H 0.5684 0.6387 -0.0091 0.083 Uiso 1 1 calc R . . C532 C 0.6253(6) 0.6011(5) 0.0792(4) 0.0812(19) Uani 1 1 d . . . H53C H 0.6933 0.6014 0.0592 0.122 Uiso 1 1 calc R . . H53D H 0.5674 0.5389 0.0668 0.122 Uiso 1 1 calc R . . H53E H 0.6432 0.6238 0.1337 0.122 Uiso 1 1 calc R . . C5 C 0.0132(4) 0.4180(3) 0.0536(3) 0.0395(10) Uani 1 1 d . . . H5A H -0.0483 0.4106 0.0839 0.047 Uiso 1 1 calc R . . H5B H -0.0179 0.4162 0.0024 0.047 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 O1 0.0430(16) 0.0334(14) 0.0356(15) 0.0120(12) 0.0036(12) 0.0214(13) C11 0.045(2) 0.032(2) 0.031(2) 0.0095(17) 0.0040(18) 0.0191(18) C12 0.054(3) 0.038(2) 0.035(2) 0.0120(18) 0.004(2) 0.026(2) C13 0.063(3) 0.034(2) 0.044(3) 0.0135(19) 0.005(2) 0.028(2) C14 0.052(3) 0.040(2) 0.036(2) 0.0109(19) -0.003(2) 0.023(2) C15 0.047(2) 0.040(2) 0.034(2) 0.0146(19) 0.0003(19) 0.0203(19) C16 0.044(2) 0.037(2) 0.032(2) 0.0140(18) 0.0080(18) 0.0221(19) O17 0.0507(18) 0.0507(17) 0.0458(18) 0.0128(14) 0.0120(15) 0.0287(15) C17 0.046(2) 0.043(2) 0.036(2) 0.0177(19) 0.002(2) 0.026(2) C18 0.050(3) 0.038(2) 0.043(2) 0.0145(19) 0.001(2) 0.020(2) P1 0.0607(7) 0.0375(6) 0.0437(7) 0.0098(5) -0.0039(6) 0.0234(5) O11 0.063(2) 0.0399(16) 0.056(2) 0.0102(15) -0.0126(17) 0.0213(15) O12 0.075(2) 0.075(2) 0.0417(19) 0.0021(17) -0.0024(17) 0.040(2) O13 0.073(2) 0.0378(16) 0.058(2) 0.0116(15) -0.0021(18) 0.0265(16) C131 0.102(5) 0.059(3) 0.090(5) 0.029(3) 0.017(4) 0.037(3) C132 0.117(7) 0.077(5) 0.323(17) 0.071(8) 0.122(10) 0.046(5) C1 0.056(3) 0.039(2) 0.040(2) 0.0110(19) -0.002(2) 0.028(2) O2 0.0490(17) 0.0369(15) 0.0355(16) 0.0129(12) 0.0037(13) 0.0225(13) C21 0.046(2) 0.0295(19) 0.043(2) 0.0161(18) 0.0023(19) 0.0215(18) C22 0.048(2) 0.032(2) 0.033(2) 0.0142(17) 0.0016(18) 0.0227(18) C23 0.049(2) 0.031(2) 0.039(2) 0.0148(18) 0.0039(19) 0.0213(19) C24 0.046(2) 0.031(2) 0.051(3) 0.0185(19) 0.002(2) 0.0172(19) C25 0.053(3) 0.034(2) 0.040(2) 0.0135(19) -0.007(2) 0.018(2) C26 0.056(3) 0.033(2) 0.038(2) 0.0168(18) -0.001(2) 0.027(2) O27 0.079(3) 0.060(2) 0.077(3) 0.0328(19) 0.020(2) 0.048(2) C27 0.060(3) 0.062(3) 0.042(3) 0.020(2) 0.010(2) 0.041(3) C28 0.062(3) 0.078(4) 0.048(3) 0.025(3) 0.015(2) 0.038(3) P2 0.0468(7) 0.0388(6) 0.0614(8) 0.0210(6) 0.0030(6) 0.0171(5) O21 0.0506(19) 0.0517(19) 0.072(2) 0.0224(17) 0.0139(17) 0.0224(16) O22 0.054(2) 0.0405(17) 0.072(2) 0.0207(16) -0.0068(17) 0.0138(15) C221 0.083(4) 0.047(3) 0.090(5) 0.009(3) -0.025(4) 0.017(3) C222 0.083(5) 0.110(5) 0.082(5) 0.046(4) 0.009(4) 0.036(4) O23 0.058(2) 0.0502(19) 0.087(3) 0.0355(19) 0.0094(19) 0.0219(17) C231 0.068(4) 0.078(4) 0.102(5) 0.056(4) 0.026(4) 0.021(3) C232 0.124(6) 0.067(4) 0.108(6) 0.050(4) 0.009(5) 0.024(4) C2 0.041(2) 0.038(2) 0.032(2) 0.0140(17) 0.0035(18) 0.0209(18) O3 0.0439(16) 0.0364(15) 0.0440(17) 0.0112(13) 0.0058(13) 0.0197(13) C31 0.039(2) 0.039(2) 0.027(2) 0.0095(17) -0.0017(17) 0.0168(18) C32 0.044(2) 0.032(2) 0.034(2) 0.0069(17) -0.0009(18) 0.0169(18) C33 0.047(2) 0.032(2) 0.034(2) 0.0071(17) -0.0043(19) 0.0171(18) C34 0.039(2) 0.040(2) 0.030(2) 0.0069(17) -0.0041(18) 0.0138(18) C35 0.040(2) 0.046(2) 0.028(2) 0.0093(18) -0.0015(17) 0.0214(19) C36 0.041(2) 0.034(2) 0.031(2) 0.0088(17) -0.0043(17) 0.0189(18) O37 0.067(2) 0.076(2) 0.0373(18) 0.0219(17) 0.0103(18) 0.038(2) C37 0.059(3) 0.040(2) 0.046(3) 0.022(2) 0.015(2) 0.031(2) C38 0.071(3) 0.056(3) 0.072(4) 0.030(3) 0.030(3) 0.037(3) P3 0.0496(7) 0.0486(7) 0.0599(8) 0.0196(6) 0.0158(6) 0.0207(6) O31 0.085(3) 0.061(2) 0.085(3) 0.028(2) 0.050(2) 0.032(2) O32 0.0518(19) 0.0483(18) 0.0486(19) 0.0148(15) 0.0058(15) 0.0130(15) C321 0.091(4) 0.059(3) 0.059(4) 0.025(3) -0.003(3) 0.016(3) C322 0.101(5) 0.095(5) 0.095(5) 0.040(4) -0.008(4) 0.045(4) O33 0.0403(19) 0.090(3) 0.101(3) 0.046(2) 0.008(2) 0.0261(19) C331 0.060(4) 0.076(4) 0.169(8) 0.044(5) 0.018(4) 0.038(3) C332 0.070(4) 0.081(4) 0.152(8) 0.038(5) 0.046(5) 0.032(4) C3 0.051(3) 0.037(2) 0.042(2) 0.0100(19) 0.003(2) 0.023(2) O4 0.0393(15) 0.0272(13) 0.0375(15) 0.0104(11) 0.0051(12) 0.0151(12) C41 0.043(2) 0.031(2) 0.039(2) 0.0089(18) 0.0071(19) 0.0187(18) C42 0.044(2) 0.033(2) 0.044(2) 0.0113(18) 0.0071(19) 0.0199(19) C43 0.061(3) 0.039(2) 0.069(3) 0.021(2) -0.004(3) 0.024(2) C44 0.074(4) 0.036(2) 0.077(4) 0.006(2) -0.017(3) 0.024(2) C45 0.061(3) 0.035(2) 0.066(3) 0.009(2) -0.018(3) 0.016(2) C46 0.042(2) 0.035(2) 0.049(3) 0.0106(19) 0.001(2) 0.0181(19) O47 0.056(2) 0.0506(19) 0.077(2) 0.0212(17) 0.0293(19) 0.0272(17) C47 0.045(2) 0.041(2) 0.039(2) 0.0145(19) 0.005(2) 0.018(2) C48 0.054(3) 0.034(2) 0.044(3) 0.0117(19) -0.003(2) 0.015(2) P4 0.0825(11) 0.0400(7) 0.1076(14) 0.0101(8) -0.0226(10) 0.0235(7) O41 0.102(3) 0.052(2) 0.099(3) -0.016(2) -0.037(3) 0.035(2) O42 0.136(5) 0.147(5) 0.077(3) 0.037(3) 0.006(3) 0.093(4) C421 0.096(5) 0.056(3) 0.123(6) 0.042(4) 0.023(4) 0.034(3) C422 0.105(6) 0.136(7) 0.240(12) 0.125(9) 0.085(7) 0.077(6) O43 0.133(4) 0.056(2) 0.107(4) -0.002(2) -0.024(3) 0.057(3) C431 0.083(4) 0.048(3) 0.104(5) 0.019(3) 0.000(4) 0.035(3) C432 0.230(13) 0.165(10) 0.184(11) 0.120(9) 0.117(10) 0.154(10) C4 0.049(2) 0.035(2) 0.043(2) 0.0132(19) 0.006(2) 0.0232(19) O5 0.0430(16) 0.0369(14) 0.0382(16) 0.0136(12) 0.0068(13) 0.0215(13) C51 0.040(2) 0.039(2) 0.038(2) 0.0185(18) 0.0063(18) 0.0245(18) C52 0.045(2) 0.038(2) 0.031(2) 0.0145(17) 0.0012(18) 0.0285(19) C53 0.047(2) 0.050(2) 0.032(2) 0.0150(19) 0.0067(19) 0.033(2) C54 0.043(2) 0.048(2) 0.040(2) 0.021(2) 0.0036(19) 0.025(2) C55 0.042(2) 0.040(2) 0.040(2) 0.0167(19) 0.0019(19) 0.0207(19) C56 0.045(2) 0.039(2) 0.035(2) 0.0147(18) 0.0008(18) 0.0239(19) O57 0.0466(18) 0.0576(19) 0.0498(18) 0.0219(16) 0.0072(14) 0.0302(15) C57 0.044(2) 0.040(2) 0.040(2) 0.007(2) 0.0006(19) 0.0227(19) C58 0.049(3) 0.065(3) 0.050(3) 0.019(2) 0.015(2) 0.029(2) P5 0.0459(7) 0.0643(8) 0.0440(7) 0.0245(6) 0.0104(5) 0.0278(6) O51 0.061(2) 0.098(3) 0.049(2) 0.031(2) 0.0133(17) 0.030(2) O52 0.055(2) 0.061(2) 0.074(2) 0.0389(19) 0.0179(18) 0.0274(17) C521 0.085(4) 0.080(4) 0.100(5) 0.056(4) 0.028(4) 0.046(4) C522 0.105(6) 0.073(4) 0.132(7) 0.036(5) 0.017(5) 0.041(4) O53 0.0502(19) 0.069(2) 0.0487(19) 0.0211(16) 0.0121(15) 0.0329(17) C531 0.059(3) 0.101(4) 0.063(4) 0.021(3) 0.017(3) 0.047(3) C532 0.082(4) 0.124(6) 0.063(4) 0.016(4) 0.009(3) 0.072(4) C5 0.045(2) 0.038(2) 0.044(2) 0.0129(19) 0.0026(19) 0.0250(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 C17 1.377(5) . ? O1 C11 1.398(5) . ? C11 C16 1.393(6) . ? C11 C12 1.406(5) . ? C12 C13 1.393(6) . ? C12 C1 1.510(6) . ? C13 C14 1.403(6) . ? C14 C15 1.394(6) . ? C14 P1 1.785(5) . ? C15 C16 1.373(6) . ? C16 C5 1.512(5) . ? O17 C17 1.183(5) . ? C17 C18 1.489(6) . ? P1 O11 1.471(3) . ? P1 O12 1.558(4) . ? P1 O13 1.577(3) . ? O12 C12' 1.360(18) . ? O12 C121 1.396(10) . ? C121 C122 1.542(17) . ? C12' C12" 1.54(2) . ? O13 C131 1.438(8) . ? C131 C132 1.441(10) . ? C1 C26 1.507(6) . ? O2 C27 1.380(5) . ? O2 C21 1.406(5) . ? C21 C22 1.390(6) . ? C21 C26 1.405(6) . ? C22 C23 1.394(6) . ? C22 C2 1.517(6) . ? C23 C24 1.391(6) . ? C24 C25 1.396(7) . ? C24 P2 1.787(5) . ? C25 C26 1.389(7) . ? O27 C27 1.195(6) . ? C27 C28 1.461(7) . ? P2 O21 1.471(4) . ? P2 O23 1.569(3) . ? P2 O22 1.594(4) . ? O22 C221 1.462(7) . ? C221 C222 1.475(9) . ? O23 C231 1.445(7) . ? C231 C232 1.476(8) . ? C2 C36 1.519(5) . ? O3 C37 1.365(5) . ? O3 C31 1.399(5) . ? C31 C32 1.382(6) . ? C31 C36 1.405(6) . ? C32 C33 1.385(6) . ? C32 C3 1.524(6) . ? C33 C34 1.393(6) . ? C34 C35 1.393(6) . ? C34 P3 1.784(4) . ? C35 C36 1.376(6) . ? O37 C37 1.197(6) . ? C37 C38 1.474(7) . ? P3 O31 1.460(4) . ? P3 O33 1.574(4) . ? P3 O32 1.576(3) . ? O32 C321 1.480(7) . ? C321 C322 1.478(9) . ? O33 C331 1.442(7) . ? C331 C332 1.432(10) . ? C3 C46 1.526(6) . ? O4 C47 1.358(5) . ? O4 C41 1.399(5) . ? C41 C46 1.380(6) . ? C41 C42 1.402(6) . ? C42 C43 1.382(6) . ? C42 C4 1.509(6) . ? C43 C44 1.390(8) . ? C44 C45 1.389(7) . ? C44 P4 1.803(5) . ? C45 C46 1.387(6) . ? O47 C47 1.199(5) . ? C47 C48 1.484(6) . ? P4 O41 1.457(5) . ? P4 O42 1.545(5) . ? P4 O43 1.563(5) . ? O42 C421 1.435(7) . ? C421 C422 1.478(10) . ? O43 C431 1.435(7) . ? C431 C432 1.461(11) . ? C4 C56 1.519(6) . ? O5 C57 1.376(5) . ? O5 C51 1.409(5) . ? C51 C56 1.378(6) . ? C51 C52 1.400(6) . ? C52 C53 1.384(6) . ? C52 C5 1.518(6) . ? C53 C54 1.395(6) . ? C54 C55 1.385(6) . ? C54 P5 1.797(4) . ? C55 C56 1.377(6) . ? O57 C57 1.194(5) . ? C57 C58 1.473(7) . ? P5 O51 1.457(4) . ? P5 O53 1.573(3) . ? P5 O52 1.584(4) . ? O52 C521 1.490(6) . ? C521 C522 1.585(10) . ? O53 C531 1.451(6) . ? C531 C532 1.463(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 C17 O1 C11 116.9(3) . . ? C16 C11 O1 118.9(3) . . ? C16 C11 C12 122.0(4) . . ? O1 C11 C12 119.0(3) . . ? C13 C12 C11 117.9(4) . . ? C13 C12 C1 121.4(4) . . ? C11 C12 C1 120.6(4) . . ? C12 C13 C14 120.8(4) . . ? C15 C14 C13 118.9(4) . . ? C15 C14 P1 119.3(3) . . ? C13 C14 P1 121.8(3) . . ? C16 C15 C14 121.8(4) . . ? C15 C16 C11 118.4(4) . . ? C15 C16 C5 117.3(4) . . ? C11 C16 C5 124.0(4) . . ? O17 C17 O1 121.5(4) . . ? O17 C17 C18 127.9(4) . . ? O1 C17 C18 110.6(4) . . ? O11 P1 O12 116.3(2) . . ? O11 P1 O13 115.9(2) . . ? O12 P1 O13 97.3(2) . . ? O11 P1 C14 112.76(19) . . ? O12 P1 C14 106.4(2) . . ? O13 P1 C14 106.67(19) . . ? C12' O12 C121 56.2(9) . . ? C12' O12 P1 123.0(8) . . ? C121 O12 P1 122.2(5) . . ? O12 C121 C122 109.6(8) . . ? O12 C12' C12" 111.2(14) . . ? C131 O13 P1 119.6(3) . . ? O13 C131 C132 111.7(6) . . ? C26 C1 C12 113.7(4) . . ? C27 O2 C21 118.5(3) . . ? C22 C21 C26 123.9(4) . . ? C22 C21 O2 117.0(4) . . ? C26 C21 O2 119.0(4) . . ? C21 C22 C23 117.2(4) . . ? C21 C22 C2 120.9(4) . . ? C23 C22 C2 121.8(4) . . ? C24 C23 C22 121.1(4) . . ? C23 C24 C25 119.7(4) . . ? C23 C24 P2 119.5(4) . . ? C25 C24 P2 120.7(3) . . ? C26 C25 C24 121.5(4) . . ? C25 C26 C21 116.6(4) . . ? C25 C26 C1 120.1(4) . . ? C21 C26 C1 123.2(4) . . ? O27 C27 O2 121.7(4) . . ? O27 C27 C28 128.1(4) . . ? O2 C27 C28 110.2(4) . . ? O21 P2 O23 116.4(2) . . ? O21 P2 O22 115.0(2) . . ? O23 P2 O22 102.2(2) . . ? O21 P2 C24 113.3(2) . . ? O23 P2 C24 103.03(19) . . ? O22 P2 C24 105.4(2) . . ? C221 O22 P2 119.9(3) . . ? O22 C221 C222 110.9(5) . . ? C231 O23 P2 121.0(3) . . ? O23 C231 C232 108.5(6) . . ? C22 C2 C36 114.8(3) . . ? C37 O3 C31 116.3(3) . . ? C32 C31 O3 119.1(4) . . ? C32 C31 C36 123.1(4) . . ? O3 C31 C36 117.7(3) . . ? C31 C32 C33 118.0(4) . . ? C31 C32 C3 122.3(4) . . ? C33 C32 C3 119.7(3) . . ? C32 C33 C34 120.5(4) . . ? C33 C34 C35 120.0(4) . . ? C33 C34 P3 121.3(3) . . ? C35 C34 P3 118.7(3) . . ? C36 C35 C34 121.1(4) . . ? C35 C36 C31 117.3(4) . . ? C35 C36 C2 121.6(4) . . ? C31 C36 C2 121.1(4) . . ? O37 C37 O3 122.6(4) . . ? O37 C37 C38 126.6(4) . . ? O3 C37 C38 110.7(4) . . ? O31 P3 O33 115.9(3) . . ? O31 P3 O32 114.3(2) . . ? O33 P3 O32 102.3(2) . . ? O31 P3 C34 112.5(2) . . ? O33 P3 C34 103.8(2) . . ? O32 P3 C34 106.83(19) . . ? C321 O32 P3 119.6(3) . . ? C322 C321 O32 109.1(5) . . ? C331 O33 P3 124.0(5) . . ? C332 C331 O33 113.4(5) . . ? C32 C3 C46 113.8(4) . . ? C47 O4 C41 116.9(3) . . ? C46 C41 O4 118.6(3) . . ? C46 C41 C42 122.6(4) . . ? O4 C41 C42 118.8(4) . . ? C43 C42 C41 117.8(4) . . ? C43 C42 C4 120.2(4) . . ? C41 C42 C4 121.7(4) . . ? C42 C43 C44 120.8(4) . . ? C45 C44 C43 119.9(4) . . ? C45 C44 P4 117.9(4) . . ? C43 C44 P4 122.0(4) . . ? C46 C45 C44 120.8(5) . . ? C41 C46 C45 118.1(4) . . ? C41 C46 C3 121.1(4) . . ? C45 C46 C3 120.6(4) . . ? O47 C47 O4 122.5(4) . . ? O47 C47 C48 126.8(4) . . ? O4 C47 C48 110.8(4) . . ? O41 P4 O42 109.2(3) . . ? O41 P4 O43 116.7(3) . . ? O42 P4 O43 109.1(3) . . ? O41 P4 C44 116.0(3) . . ? O42 P4 C44 102.4(3) . . ? O43 P4 C44 102.3(3) . . ? C421 O42 P4 117.6(4) . . ? O42 C421 C422 107.7(6) . . ? C431 O43 P4 121.4(4) . . ? O43 C431 C432 110.4(6) . . ? C42 C4 C56 116.1(4) . . ? C57 O5 C51 116.3(3) . . ? C56 C51 C52 123.4(4) . . ? C56 C51 O5 119.6(4) . . ? C52 C51 O5 117.0(4) . . ? C53 C52 C51 116.8(4) . . ? C53 C52 C5 123.0(4) . . ? C51 C52 C5 119.7(4) . . ? C52 C53 C54 121.0(4) . . ? C55 C54 C53 120.0(4) . . ? C55 C54 P5 120.4(3) . . ? C53 C54 P5 119.6(3) . . ? C56 C55 C54 120.6(4) . . ? C55 C56 C51 118.2(4) . . ? C55 C56 C4 120.1(4) . . ? C51 C56 C4 121.6(4) . . ? O57 C57 O5 121.8(4) . . ? O57 C57 C58 127.1(4) . . ? O5 C57 C58 111.1(4) . . ? O51 P5 O53 117.9(2) . . ? O51 P5 O52 113.1(2) . . ? O53 P5 O52 102.0(2) . . ? O51 P5 C54 114.1(2) . . ? O53 P5 C54 102.10(18) . . ? O52 P5 C54 106.0(2) . . ? C521 O52 P5 119.6(4) . . ? O52 C521 C522 105.0(5) . . ? C531 O53 P5 121.6(3) . . ? O53 C531 C532 108.0(5) . . ? C16 C5 C52 121.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C17 O1 C11 C16 -105.4(4) . . . . ? C17 O1 C11 C12 77.9(4) . . . . ? C16 C11 C12 C13 0.5(6) . . . . ? O1 C11 C12 C13 177.1(4) . . . . ? C16 C11 C12 C1 -178.8(4) . . . . ? O1 C11 C12 C1 -2.2(6) . . . . ? C11 C12 C13 C14 1.7(7) . . . . ? C1 C12 C13 C14 -179.0(4) . . . . ? C12 C13 C14 C15 -2.5(7) . . . . ? C12 C13 C14 P1 177.8(4) . . . . ? C13 C14 C15 C16 1.2(7) . . . . ? P1 C14 C15 C16 -179.1(3) . . . . ? C14 C15 C16 C11 1.0(6) . . . . ? C14 C15 C16 C5 -172.5(4) . . . . ? O1 C11 C16 C15 -178.4(4) . . . . ? C12 C11 C16 C15 -1.9(6) . . . . ? O1 C11 C16 C5 -5.4(6) . . . . ? C12 C11 C16 C5 171.2(4) . . . . ? C11 O1 C17 O17 -4.3(5) . . . . ? C11 O1 C17 C18 176.1(3) . . . . ? C15 C14 P1 O11 -9.4(5) . . . . ? C13 C14 P1 O11 170.3(4) . . . . ? C15 C14 P1 O12 119.1(4) . . . . ? C13 C14 P1 O12 -61.2(4) . . . . ? C15 C14 P1 O13 -137.8(4) . . . . ? C13 C14 P1 O13 41.9(4) . . . . ? O11 P1 O12 C12' -23.4(10) . . . . ? O13 P1 O12 C12' 100.3(10) . . . . ? C14 P1 O12 C12' -149.9(10) . . . . ? O11 P1 O12 C121 44.6(6) . . . . ? O13 P1 O12 C121 168.3(6) . . . . ? C14 P1 O12 C121 -81.8(6) . . . . ? C12' O12 C121 C122 -76.1(12) . . . . ? P1 O12 C121 C122 173.1(7) . . . . ? C121 O12 C12' C12" 53.5(12) . . . . ? P1 O12 C12' C12" 162.8(10) . . . . ? O11 P1 O13 C131 -60.7(5) . . . . ? O12 P1 O13 C131 175.3(4) . . . . ? C14 P1 O13 C131 65.8(5) . . . . ? P1 O13 C131 C132 157.1(7) . . . . ? C13 C12 C1 C26 -123.5(4) . . . . ? C11 C12 C1 C26 55.8(6) . . . . ? C27 O2 C21 C22 115.9(4) . . . . ? C27 O2 C21 C26 -68.7(4) . . . . ? C26 C21 C22 C23 -2.1(5) . . . . ? O2 C21 C22 C23 173.1(3) . . . . ? C26 C21 C22 C2 178.1(3) . . . . ? O2 C21 C22 C2 -6.7(5) . . . . ? C21 C22 C23 C24 0.9(5) . . . . ? C2 C22 C23 C24 -179.2(3) . . . . ? C22 C23 C24 C25 0.8(5) . . . . ? C22 C23 C24 P2 -176.2(3) . . . . ? C23 C24 C25 C26 -1.6(5) . . . . ? P2 C24 C25 C26 175.4(3) . . . . ? C24 C25 C26 C21 0.6(5) . . . . ? C24 C25 C26 C1 -176.9(3) . . . . ? C22 C21 C26 C25 1.3(5) . . . . ? O2 C21 C26 C25 -173.8(3) . . . . ? C22 C21 C26 C1 178.7(3) . . . . ? O2 C21 C26 C1 3.6(5) . . . . ? C12 C1 C26 C25 46.2(5) . . . . ? C12 C1 C26 C21 -131.1(4) . . . . ? C21 O2 C27 O27 -5.0(6) . . . . ? C21 O2 C27 C28 172.8(4) . . . . ? C23 C24 P2 O21 33.3(4) . . . . ? C25 C24 P2 O21 -143.8(3) . . . . ? C23 C24 P2 O23 -93.4(3) . . . . ? C25 C24 P2 O23 89.6(3) . . . . ? C23 C24 P2 O22 159.9(3) . . . . ? C25 C24 P2 O22 -17.2(3) . . . . ? O21 P2 O22 C221 46.4(5) . . . . ? O23 P2 O22 C221 173.5(4) . . . . ? C24 P2 O22 C221 -79.1(5) . . . . ? P2 O22 C221 C222 158.1(4) . . . . ? O21 P2 O23 C231 43.8(5) . . . . ? O22 P2 O23 C231 -82.4(5) . . . . ? C24 P2 O23 C231 168.4(5) . . . . ? P2 O23 C231 C232 -176.7(5) . . . . ? C21 C22 C2 C36 77.0(5) . . . . ? C23 C22 C2 C36 -102.9(4) . . . . ? C37 O3 C31 C32 -87.3(4) . . . . ? C37 O3 C31 C36 96.2(4) . . . . ? O3 C31 C32 C33 -178.5(3) . . . . ? C36 C31 C32 C33 -2.2(6) . . . . ? O3 C31 C32 C3 3.0(6) . . . . ? C36 C31 C32 C3 179.4(4) . . . . ? C31 C32 C33 C34 2.0(6) . . . . ? C3 C32 C33 C34 -179.5(4) . . . . ? C32 C33 C34 C35 -0.7(6) . . . . ? C32 C33 C34 P3 176.8(3) . . . . ? C33 C34 C35 C36 -0.6(6) . . . . ? P3 C34 C35 C36 -178.1(3) . . . . ? C34 C35 C36 C31 0.5(6) . . . . ? C34 C35 C36 C2 -178.7(4) . . . . ? C32 C31 C36 C35 0.9(6) . . . . ? O3 C31 C36 C35 177.3(3) . . . . ? C32 C31 C36 C2 -179.9(4) . . . . ? O3 C31 C36 C2 -3.5(5) . . . . ? C22 C2 C36 C35 -102.7(4) . . . . ? C22 C2 C36 C31 78.2(5) . . . . ? C31 O3 C37 O37 -2.6(5) . . . . ? C31 O3 C37 C38 175.6(3) . . . . ? C33 C34 P3 O31 -141.4(4) . . . . ? C35 C34 P3 O31 36.1(4) . . . . ? C33 C34 P3 O33 92.4(4) . . . . ? C35 C34 P3 O33 -90.1(4) . . . . ? C33 C34 P3 O32 -15.2(4) . . . . ? C35 C34 P3 O32 162.3(3) . . . . ? O31 P3 O32 C321 52.8(5) . . . . ? O33 P3 O32 C321 178.9(4) . . . . ? C34 P3 O32 C321 -72.3(4) . . . . ? P3 O32 C321 C322 157.5(5) . . . . ? O31 P3 O33 C331 27.1(5) . . . . ? O32 P3 O33 C331 -97.9(5) . . . . ? C34 P3 O33 C331 151.1(4) . . . . ? P3 O33 C331 C332 78.1(8) . . . . ? C31 C32 C3 C46 -130.0(4) . . . . ? C33 C32 C3 C46 51.6(5) . . . . ? C47 O4 C41 C46 94.7(5) . . . . ? C47 O4 C41 C42 -87.6(5) . . . . ? C46 C41 C42 C43 0.6(7) . . . . ? O4 C41 C42 C43 -176.9(4) . . . . ? C46 C41 C42 C4 -172.7(4) . . . . ? O4 C41 C42 C4 9.7(6) . . . . ? C41 C42 C43 C44 -1.7(8) . . . . ? C4 C42 C43 C44 171.7(5) . . . . ? C42 C43 C44 C45 1.2(9) . . . . ? C42 C43 C44 P4 -173.7(4) . . . . ? C43 C44 C45 C46 0.5(9) . . . . ? P4 C44 C45 C46 175.6(4) . . . . ? O4 C41 C46 C45 178.5(4) . . . . ? C42 C41 C46 C45 1.0(7) . . . . ? O4 C41 C46 C3 -7.5(6) . . . . ? C42 C41 C46 C3 174.9(4) . . . . ? C44 C45 C46 C41 -1.5(8) . . . . ? C44 C45 C46 C3 -175.5(5) . . . . ? C32 C3 C46 C41 64.0(6) . . . . ? C32 C3 C46 C45 -122.1(5) . . . . ? C41 O4 C47 O47 4.2(6) . . . . ? C41 O4 C47 C48 -175.7(3) . . . . ? C45 C44 P4 O41 -18.8(6) . . . . ? C43 C44 P4 O41 156.2(5) . . . . ? C45 C44 P4 O42 100.0(5) . . . . ? C43 C44 P4 O42 -85.0(6) . . . . ? C45 C44 P4 O43 -147.0(5) . . . . ? C43 C44 P4 O43 28.0(6) . . . . ? O41 P4 O42 C421 -165.7(4) . . . . ? O43 P4 O42 C421 -37.0(5) . . . . ? C44 P4 O42 C421 70.9(5) . . . . ? P4 O42 C421 C422 162.8(5) . . . . ? O41 P4 O43 C431 32.4(7) . . . . ? O42 P4 O43 C431 -92.0(6) . . . . ? C44 P4 O43 C431 160.1(5) . . . . ? P4 O43 C431 C432 -113.6(7) . . . . ? C43 C42 C4 C56 122.4(5) . . . . ? C41 C42 C4 C56 -64.4(5) . . . . ? C57 O5 C51 C56 78.2(5) . . . . ? C57 O5 C51 C52 -102.3(4) . . . . ? C56 C51 C52 C53 1.0(5) . . . . ? O5 C51 C52 C53 -178.4(3) . . . . ? C56 C51 C52 C5 -171.2(3) . . . . ? O5 C51 C52 C5 9.4(5) . . . . ? C51 C52 C53 C54 0.1(5) . . . . ? C5 C52 C53 C54 172.0(3) . . . . ? C52 C53 C54 C55 -0.4(6) . . . . ? C52 C53 C54 P5 -178.1(3) . . . . ? C53 C54 C55 C56 -0.2(6) . . . . ? P5 C54 C55 C56 177.4(3) . . . . ? C54 C55 C56 C51 1.2(6) . . . . ? C54 C55 C56 C4 -175.2(4) . . . . ? C52 C51 C56 C55 -1.7(6) . . . . ? O5 C51 C56 C55 177.8(3) . . . . ? C52 C51 C56 C4 174.7(3) . . . . ? O5 C51 C56 C4 -5.9(5) . . . . ? C42 C4 C56 C55 -58.2(5) . . . . ? C42 C4 C56 C51 125.5(4) . . . . ? C51 O5 C57 O57 -1.3(6) . . . . ? C51 O5 C57 C58 177.9(4) . . . . ? C55 C54 P5 O51 -131.2(4) . . . . ? C53 C54 P5 O51 46.5(4) . . . . ? C55 C54 P5 O53 100.4(3) . . . . ? C53 C54 P5 O53 -81.9(3) . . . . ? C55 C54 P5 O52 -6.1(4) . . . . ? C53 C54 P5 O52 171.6(3) . . . . ? O51 P5 O52 C521 40.5(4) . . . . ? O53 P5 O52 C521 168.2(4) . . . . ? C54 P5 O52 C521 -85.3(4) . . . . ? P5 O52 C521 C522 168.7(4) . . . . ? O51 P5 O53 C531 41.2(5) . . . . ? O52 P5 O53 C531 -83.3(4) . . . . ? C54 P5 O53 C531 167.2(4) . . . . ? P5 O53 C531 C532 -162.0(4) . . . . ? C15 C16 C5 C52 -152.5(4) . . . . ? C11 C16 C5 C52 34.4(6) . . . . ? C53 C52 C5 C16 60.9(5) . . . . ? C51 C52 C5 C16 -127.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 66.99 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.634 _refine_diff_density_min -1.124 _refine_diff_density_rms 0.085 # Attachment 'TC027-3c.CIF' data_tc027 _database_code_depnum_ccdc_archive 'CCDC 669057' # start Validation Reply Form _vrf_PLAT761_tc027 ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: Positions of hydrogen atoms and their atomic displacement parameters were constrained to the bonded atoms during the refinement, using literature data. ; _vrf_PLAT762_tc027 ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: same, as above ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H42 Br6 O12, 2(C8 H10)' _chemical_formula_sum 'C70 H62 Br6 O12' _chemical_formula_weight 1574.66 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 11.347(2) _cell_length_b 12.878(2) _cell_length_c 13.849(2) _cell_angle_alpha 112.802(2) _cell_angle_beta 98.427(2) _cell_angle_gamma 110.792(2) _cell_volume 1646.6(5) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 5919 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 28.0 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_absorpt_coefficient_mu 3.719 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3178 _exptl_absorpt_correction_T_max 0.7552 _exptl_absorpt_process_details 'SADABS - Bruker area detector absorption corrections' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS CCD' _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 14667 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0613 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.00 _reflns_number_total 7632 _reflns_number_gt 5452 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL, v. 5.1' _computing_structure_refinement 'Bruker SHELXTL, v. 5.1' _computing_molecular_graphics 'Bruker SHELXTL, v. 5.1' _computing_publication_material 'Bruker SHELXTL, v. 5.1' _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^)+(0.0767P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_reflns 7632 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0720 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1356 _refine_ls_wR_factor_gt 0.1251 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 Br1 Br 0.43419(4) -0.38025(5) -0.00891(4) 0.04973(14) Uani 1 1 d . . . O1 O -0.1014(2) -0.3939(2) -0.1533(2) 0.0303(5) Uani 1 1 d . . . C11 C 0.0178(3) -0.4031(3) -0.1243(3) 0.0257(7) Uani 1 1 d . . . C12 C 0.0781(3) -0.3580(3) -0.0120(3) 0.0283(7) Uani 1 1 d . . . C13 C 0.2009(4) -0.3547(3) 0.0212(3) 0.0305(8) Uani 1 1 d . . . H13 H 0.2446 -0.3249 0.0973 0.037 Uiso 1 1 calc R . . C14 C 0.2601(4) -0.3953(4) -0.0573(3) 0.0343(8) Uani 1 1 d . . . C15 C 0.1979(4) -0.4406(3) -0.1690(3) 0.0329(8) Uani 1 1 d . . . H15 H 0.2399 -0.4685 -0.2214 0.040 Uiso 1 1 calc R . . C16 C 0.0741(4) -0.4453(3) -0.2047(3) 0.0292(8) Uani 1 1 d . . . C17 C -0.2179(4) -0.5026(4) -0.2096(3) 0.0337(8) Uani 1 1 d . . . O17 O -0.2217(3) -0.6051(3) -0.2399(2) 0.0416(7) Uani 1 1 d . . . C18 C -0.3333(4) -0.4734(5) -0.2246(4) 0.0547(12) Uani 1 1 d . . . H181 H -0.4165 -0.5524 -0.2649 0.082 Uiso 1 1 calc R . . H182 H -0.3234 -0.4269 -0.2670 0.082 Uiso 1 1 calc R . . H183 H -0.3357 -0.4219 -0.1518 0.082 Uiso 1 1 calc R . . C1 C 0.0169(4) -0.3064(3) 0.0731(3) 0.0305(8) Uani 1 1 d . . . H11 H 0.0524 -0.3106 0.1404 0.037 Uiso 1 1 calc R . . H12 H -0.0808 -0.3603 0.0432 0.037 Uiso 1 1 calc R . . Br2 Br 0.25838(4) 0.11575(4) 0.03759(4) 0.03953(13) Uani 1 1 d . . . O2 O -0.0719(2) -0.1701(2) 0.2365(2) 0.0294(5) Uani 1 1 d . . . C21 C -0.0046(3) -0.1090(3) 0.1817(3) 0.0263(7) Uani 1 1 d . . . C22 C 0.0167(3) 0.0145(3) 0.2144(3) 0.0293(8) Uani 1 1 d . . . C23 C 0.0957(4) 0.0804(3) 0.1694(3) 0.0313(8) Uani 1 1 d . . . H23 H 0.1127 0.1651 0.1900 0.038 Uiso 1 1 calc R . . C24 C 0.1489(3) 0.0219(3) 0.0951(3) 0.0290(7) Uani 1 1 d . . . C25 C 0.1235(4) -0.1025(3) 0.0609(3) 0.0302(8) Uani 1 1 d . . . H25 H 0.1592 -0.1413 0.0077 0.036 Uiso 1 1 calc R . . C26 C 0.0448(3) -0.1711(3) 0.1049(3) 0.0260(7) Uani 1 1 d . . . C27 C -0.2070(4) -0.2411(4) 0.1917(4) 0.0418(10) Uani 1 1 d . . . O27 O -0.2659(3) -0.2701(4) 0.0985(4) 0.0781(13) Uani 1 1 d . . . C28 C -0.2629(5) -0.2779(4) 0.2711(4) 0.0488(11) Uani 1 1 d . . . H281 H -0.3599 -0.3293 0.2371 0.073 Uiso 1 1 calc R . . H282 H -0.2425 -0.2018 0.3390 0.073 Uiso 1 1 calc R . . H283 H -0.2228 -0.3269 0.2893 0.073 Uiso 1 1 calc R . . C2 C -0.0433(4) 0.0746(3) 0.2974(4) 0.0374(9) Uani 1 1 d . . . H21 H -0.1390 0.0440 0.2591 0.045 Uiso 1 1 calc R . . H22 H -0.0375 0.0479 0.3553 0.045 Uiso 1 1 calc R . . Br3 Br 0.37917(4) 0.50263(4) 0.60318(4) 0.04280(13) Uani 1 1 d . . . O3 O -0.1397(3) 0.2158(2) 0.2218(2) 0.0357(6) Uani 1 1 d . . . C31 C -0.0221(3) 0.2853(3) 0.3152(3) 0.0300(8) Uani 1 1 d . . . C32 C 0.0446(4) 0.4168(3) 0.3613(3) 0.0304(8) Uani 1 1 d . . . C33 C 0.1654(4) 0.4791(3) 0.4466(3) 0.0297(8) Uani 1 1 d . . . H33 H 0.2144 0.5683 0.4795 0.036 Uiso 1 1 calc R . . C34 C 0.2153(4) 0.4132(4) 0.4842(3) 0.0353(8) Uani 1 1 d . . . C35 C 0.1473(4) 0.2839(4) 0.4391(3) 0.0358(9) Uani 1 1 d . . . H35 H 0.1824 0.2406 0.4672 0.043 Uiso 1 1 calc R . . C36 C 0.0263(4) 0.2168(3) 0.3517(3) 0.0351(8) Uani 1 1 d . . . C37 C -0.2553(4) 0.2106(3) 0.2417(4) 0.0372(9) Uani 1 1 d . . . O37 O -0.2599(3) 0.2586(3) 0.3325(3) 0.0521(8) Uani 1 1 d . . . C38 C -0.3697(4) 0.1371(4) 0.1356(4) 0.0506(11) Uani 1 1 d . . . H381 H -0.4517 0.1344 0.1517 0.076 Uiso 1 1 calc R . . H382 H -0.3802 0.0509 0.0966 0.076 Uiso 1 1 calc R . . H383 H -0.3524 0.1777 0.0888 0.076 Uiso 1 1 calc R . . C3 C -0.0103(4) 0.4932(3) 0.3268(3) 0.0312(8) Uani 1 1 d . . . H31 H -0.0775 0.5020 0.3634 0.037 Uiso 1 1 calc R . . H32 H 0.0637 0.5789 0.3571 0.037 Uiso 1 1 calc R . . C1A C 0.4004(5) 0.1207(5) 0.4771(5) 0.0540(12) Uani 1 1 d . . . C2A C 0.4652(5) 0.1327(4) 0.5796(5) 0.0594(14) Uani 1 1 d . . . H2A H 0.5505 0.2020 0.6253 0.071 Uiso 1 1 calc R . . C3A C 0.4060(5) 0.0450(4) 0.6138(4) 0.0524(12) Uani 1 1 d . . . C4A C 0.2841(5) -0.0552(5) 0.5474(5) 0.0633(14) Uani 1 1 d . . . H4A H 0.2436 -0.1158 0.5704 0.076 Uiso 1 1 calc R . . C5A C 0.2214(5) -0.0690(6) 0.4507(6) 0.0735(17) Uani 1 1 d . . . H5A H 0.1362 -0.1388 0.4061 0.088 Uiso 1 1 calc R . . C6A C 0.2785(5) 0.0163(5) 0.4147(5) 0.0625(14) Uani 1 1 d . . . H6A H 0.2324 0.0029 0.3446 0.075 Uiso 1 1 calc R . . C11A C 0.4617(7) 0.2120(6) 0.4386(7) 0.088(2) Uani 1 1 d . . . H11A H 0.4017 0.1869 0.3664 0.131 Uiso 1 1 calc R . . H11B H 0.5469 0.2139 0.4313 0.131 Uiso 1 1 calc R . . H11C H 0.4772 0.2962 0.4924 0.131 Uiso 1 1 calc R . . C13A C 0.4788(7) 0.0637(6) 0.7253(5) 0.0839(19) Uani 1 1 d . . . H13A H 0.4250 -0.0055 0.7379 0.126 Uiso 1 1 calc R . . H13B H 0.4928 0.1442 0.7846 0.126 Uiso 1 1 calc R . . H13C H 0.5653 0.0642 0.7251 0.126 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 Br1 0.0307(2) 0.0664(3) 0.0552(3) 0.0265(2) 0.01054(19) 0.0292(2) O1 0.0211(12) 0.0298(13) 0.0380(14) 0.0119(11) 0.0104(11) 0.0140(10) C11 0.0236(16) 0.0227(16) 0.0305(18) 0.0107(14) 0.0081(14) 0.0126(13) C12 0.0282(17) 0.0214(16) 0.0330(19) 0.0120(15) 0.0126(15) 0.0090(14) C13 0.0267(18) 0.0290(18) 0.033(2) 0.0142(16) 0.0063(15) 0.0122(15) C14 0.0246(18) 0.037(2) 0.041(2) 0.0167(18) 0.0083(16) 0.0165(16) C15 0.0289(19) 0.0341(19) 0.040(2) 0.0163(17) 0.0140(16) 0.0186(16) C16 0.0306(18) 0.0267(17) 0.0316(19) 0.0122(15) 0.0095(15) 0.0163(15) C17 0.0260(18) 0.040(2) 0.035(2) 0.0184(18) 0.0078(16) 0.0152(16) O17 0.0301(14) 0.0342(15) 0.0496(17) 0.0176(13) 0.0053(13) 0.0092(12) C18 0.027(2) 0.056(3) 0.070(3) 0.021(2) 0.006(2) 0.021(2) C1 0.0307(18) 0.0260(17) 0.033(2) 0.0123(16) 0.0127(16) 0.0119(15) Br2 0.0411(2) 0.0318(2) 0.0466(2) 0.02007(18) 0.02384(19) 0.01209(17) O2 0.0260(12) 0.0297(13) 0.0333(14) 0.0159(11) 0.0120(11) 0.0116(10) C21 0.0209(16) 0.0276(17) 0.0284(18) 0.0125(15) 0.0072(14) 0.0102(14) C22 0.0213(16) 0.0277(17) 0.034(2) 0.0101(16) 0.0097(15) 0.0103(14) C23 0.0278(18) 0.0247(17) 0.040(2) 0.0141(16) 0.0117(16) 0.0117(15) C24 0.0240(17) 0.0270(17) 0.0323(19) 0.0141(15) 0.0099(15) 0.0076(14) C25 0.0285(18) 0.0307(18) 0.033(2) 0.0139(16) 0.0142(15) 0.0149(15) C26 0.0192(16) 0.0234(16) 0.0304(18) 0.0111(14) 0.0057(14) 0.0073(13) C27 0.0272(19) 0.049(2) 0.064(3) 0.038(2) 0.019(2) 0.0186(18) O27 0.0241(16) 0.118(3) 0.099(3) 0.083(3) 0.0085(18) 0.0091(18) C28 0.047(3) 0.048(2) 0.073(3) 0.040(2) 0.039(2) 0.024(2) C2 0.036(2) 0.0317(19) 0.052(2) 0.0198(18) 0.0273(19) 0.0189(17) Br3 0.0307(2) 0.0553(3) 0.0458(3) 0.0271(2) 0.00943(17) 0.02054(19) O3 0.0306(14) 0.0325(14) 0.0334(14) 0.0063(12) 0.0109(11) 0.0137(11) C31 0.0245(17) 0.0279(18) 0.032(2) 0.0085(16) 0.0109(15) 0.0122(14) C32 0.0323(19) 0.0318(18) 0.0283(19) 0.0108(16) 0.0133(15) 0.0182(16) C33 0.0287(18) 0.0284(18) 0.0263(18) 0.0085(15) 0.0083(15) 0.0122(15) C34 0.0304(19) 0.047(2) 0.039(2) 0.0232(19) 0.0162(17) 0.0236(18) C35 0.034(2) 0.038(2) 0.051(2) 0.0242(19) 0.0237(18) 0.0254(17) C36 0.033(2) 0.0317(19) 0.044(2) 0.0158(18) 0.0196(18) 0.0180(16) C37 0.0285(19) 0.0278(19) 0.044(2) 0.0090(18) 0.0106(17) 0.0105(16) O37 0.0347(16) 0.0535(19) 0.0473(19) 0.0060(15) 0.0184(14) 0.0168(14) C38 0.034(2) 0.048(3) 0.054(3) 0.015(2) 0.007(2) 0.014(2) C3 0.035(2) 0.0324(19) 0.0269(19) 0.0118(16) 0.0101(16) 0.0193(16) C1A 0.039(2) 0.050(3) 0.076(4) 0.025(3) 0.022(2) 0.026(2) C2A 0.034(2) 0.039(2) 0.076(4) 0.002(2) 0.016(2) 0.016(2) C3A 0.052(3) 0.046(3) 0.058(3) 0.017(2) 0.023(2) 0.028(2) C4A 0.046(3) 0.058(3) 0.087(4) 0.032(3) 0.031(3) 0.024(2) C5A 0.039(3) 0.075(4) 0.097(5) 0.044(4) 0.010(3) 0.016(3) C6A 0.043(3) 0.069(3) 0.073(4) 0.035(3) 0.009(3) 0.025(3) C11A 0.086(4) 0.077(4) 0.141(6) 0.064(4) 0.070(5) 0.052(4) C13A 0.089(5) 0.066(4) 0.067(4) 0.016(3) 0.012(3) 0.026(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 Br1 C14 1.905(4) . ? O1 C17 1.362(4) . ? O1 C11 1.414(4) . ? C11 C12 1.389(5) . ? C11 C16 1.389(5) . ? C12 C13 1.382(5) . ? C12 C1 1.507(5) . ? C13 C14 1.389(5) . ? C14 C15 1.386(6) . ? C15 C16 1.391(5) . ? C16 C3 1.510(5) 2 ? C17 O17 1.202(5) . ? C17 C18 1.492(5) . ? C1 C26 1.517(5) . ? Br2 C24 1.899(3) . ? O2 C27 1.363(5) . ? O2 C21 1.408(4) . ? C21 C26 1.385(5) . ? C21 C22 1.390(5) . ? C22 C23 1.395(5) . ? C22 C2 1.516(5) . ? C23 C24 1.377(5) . ? C24 C25 1.385(5) . ? C25 C26 1.403(5) . ? C27 O27 1.203(6) . ? C27 C28 1.494(6) . ? C2 C36 1.508(5) . ? Br3 C34 1.900(4) . ? O3 C37 1.363(5) . ? O3 C31 1.416(4) . ? C31 C36 1.395(5) . ? C31 C32 1.399(5) . ? C32 C33 1.388(5) . ? C32 C3 1.516(5) . ? C33 C34 1.382(5) . ? C34 C35 1.377(5) . ? C35 C36 1.398(5) . ? C37 O37 1.185(5) . ? C37 C38 1.494(6) . ? C3 C16 1.510(5) 2 ? C1A C6A 1.376(7) . ? C1A C2A 1.423(7) . ? C1A C11A 1.472(8) . ? C2A C3A 1.386(7) . ? C3A C4A 1.365(7) . ? C3A C13A 1.523(8) . ? C4A C5A 1.333(8) . ? C5A C6A 1.375(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 C17 O1 C11 118.0(3) . . ? C12 C11 C16 123.6(3) . . ? C12 C11 O1 116.1(3) . . ? C16 C11 O1 120.1(3) . . ? C13 C12 C11 118.0(3) . . ? C13 C12 C1 120.2(3) . . ? C11 C12 C1 121.7(3) . . ? C12 C13 C14 119.7(4) . . ? C15 C14 C13 121.4(3) . . ? C15 C14 Br1 119.5(3) . . ? C13 C14 Br1 119.0(3) . . ? C14 C15 C16 120.1(4) . . ? C11 C16 C15 117.3(3) . . ? C11 C16 C3 124.1(3) . 2 ? C15 C16 C3 118.7(3) . 2 ? O17 C17 O1 122.5(3) . . ? O17 C17 C18 127.3(4) . . ? O1 C17 C18 110.3(3) . . ? C12 C1 C26 113.0(3) . . ? C27 O2 C21 118.8(3) . . ? C26 C21 C22 123.8(3) . . ? C26 C21 O2 118.7(3) . . ? C22 C21 O2 117.3(3) . . ? C21 C22 C23 117.7(3) . . ? C21 C22 C2 120.4(3) . . ? C23 C22 C2 121.9(3) . . ? C24 C23 C22 119.6(3) . . ? C23 C24 C25 121.9(3) . . ? C23 C24 Br2 118.3(3) . . ? C25 C24 Br2 119.8(3) . . ? C24 C25 C26 119.8(3) . . ? C21 C26 C25 117.1(3) . . ? C21 C26 C1 120.8(3) . . ? C25 C26 C1 122.2(3) . . ? O27 C27 O2 121.2(4) . . ? O27 C27 C28 127.9(4) . . ? O2 C27 C28 110.8(4) . . ? C36 C2 C22 112.4(3) . . ? C37 O3 C31 116.9(3) . . ? C36 C31 C32 123.2(3) . . ? C36 C31 O3 117.3(3) . . ? C32 C31 O3 119.3(3) . . ? C33 C32 C31 116.9(3) . . ? C33 C32 C3 119.2(3) . . ? C31 C32 C3 123.8(3) . . ? C34 C33 C32 120.9(3) . . ? C35 C34 C33 121.5(4) . . ? C35 C34 Br3 119.0(3) . . ? C33 C34 Br3 119.5(3) . . ? C34 C35 C36 119.7(3) . . ? C31 C36 C35 117.8(3) . . ? C31 C36 C2 122.6(4) . . ? C35 C36 C2 119.6(3) . . ? O37 C37 O3 122.6(4) . . ? O37 C37 C38 126.6(4) . . ? O3 C37 C38 110.8(4) . . ? C16 C3 C32 118.6(3) 2 . ? C6A C1A C2A 115.8(5) . . ? C6A C1A C11A 122.1(6) . . ? C2A C1A C11A 122.0(5) . . ? C3A C2A C1A 121.0(4) . . ? C4A C3A C2A 119.4(5) . . ? C4A C3A C13A 121.7(5) . . ? C2A C3A C13A 118.9(5) . . ? C5A C4A C3A 120.8(5) . . ? C4A C5A C6A 120.9(5) . . ? C5A C6A C1A 122.1(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C17 O1 C11 C12 -110.6(4) . . . . ? C17 O1 C11 C16 74.6(4) . . . . ? C16 C11 C12 C13 0.3(5) . . . . ? O1 C11 C12 C13 -174.3(3) . . . . ? C16 C11 C12 C1 176.6(3) . . . . ? O1 C11 C12 C1 1.9(5) . . . . ? C11 C12 C13 C14 0.3(5) . . . . ? C1 C12 C13 C14 -176.0(3) . . . . ? C12 C13 C14 C15 -0.8(6) . . . . ? C12 C13 C14 Br1 176.2(3) . . . . ? C13 C14 C15 C16 0.5(6) . . . . ? Br1 C14 C15 C16 -176.4(3) . . . . ? C12 C11 C16 C15 -0.5(5) . . . . ? O1 C11 C16 C15 173.9(3) . . . . ? C12 C11 C16 C3 -179.3(3) . . . 2 ? O1 C11 C16 C3 -4.9(5) . . . 2 ? C14 C15 C16 C11 0.1(5) . . . . ? C14 C15 C16 C3 178.9(3) . . . 2 ? C11 O1 C17 O17 -3.8(5) . . . . ? C11 O1 C17 C18 175.4(3) . . . . ? C13 C12 C1 C26 95.7(4) . . . . ? C11 C12 C1 C26 -80.5(4) . . . . ? C27 O2 C21 C26 -91.7(4) . . . . ? C27 O2 C21 C22 93.0(4) . . . . ? C26 C21 C22 C23 -2.0(5) . . . . ? O2 C21 C22 C23 173.2(3) . . . . ? C26 C21 C22 C2 178.8(3) . . . . ? O2 C21 C22 C2 -6.1(5) . . . . ? C21 C22 C23 C24 0.2(5) . . . . ? C2 C22 C23 C24 179.4(4) . . . . ? C22 C23 C24 C25 1.8(6) . . . . ? C22 C23 C24 Br2 -179.0(3) . . . . ? C23 C24 C25 C26 -2.0(6) . . . . ? Br2 C24 C25 C26 178.7(3) . . . . ? C22 C21 C26 C25 1.7(5) . . . . ? O2 C21 C26 C25 -173.4(3) . . . . ? C22 C21 C26 C1 -179.8(3) . . . . ? O2 C21 C26 C1 5.2(5) . . . . ? C24 C25 C26 C21 0.3(5) . . . . ? C24 C25 C26 C1 -178.2(3) . . . . ? C12 C1 C26 C21 179.6(3) . . . . ? C12 C1 C26 C25 -1.9(5) . . . . ? C21 O2 C27 O27 13.0(6) . . . . ? C21 O2 C27 C28 -169.4(3) . . . . ? C21 C22 C2 C36 160.3(3) . . . . ? C23 C22 C2 C36 -18.9(5) . . . . ? C37 O3 C31 C36 103.1(4) . . . . ? C37 O3 C31 C32 -81.2(4) . . . . ? C36 C31 C32 C33 0.8(5) . . . . ? O3 C31 C32 C33 -174.6(3) . . . . ? C36 C31 C32 C3 -176.5(4) . . . . ? O3 C31 C32 C3 8.1(5) . . . . ? C31 C32 C33 C34 -0.8(5) . . . . ? C3 C32 C33 C34 176.6(3) . . . . ? C32 C33 C34 C35 -0.2(6) . . . . ? C32 C33 C34 Br3 -178.7(3) . . . . ? C33 C34 C35 C36 1.3(6) . . . . ? Br3 C34 C35 C36 179.8(3) . . . . ? C32 C31 C36 C35 0.2(6) . . . . ? O3 C31 C36 C35 175.7(3) . . . . ? C32 C31 C36 C2 -176.9(3) . . . . ? O3 C31 C36 C2 -1.4(5) . . . . ? C34 C35 C36 C31 -1.3(5) . . . . ? C34 C35 C36 C2 175.9(3) . . . . ? C22 C2 C36 C31 97.2(4) . . . . ? C22 C2 C36 C35 -79.9(5) . . . . ? C31 O3 C37 O37 -1.9(6) . . . . ? C31 O3 C37 C38 178.6(3) . . . . ? C33 C32 C3 C16 139.1(4) . . . 2 ? C31 C32 C3 C16 -43.6(5) . . . 2 ? C6A C1A C2A C3A -1.3(7) . . . . ? C11A C1A C2A C3A -179.6(5) . . . . ? C1A C2A C3A C4A 0.7(7) . . . . ? C1A C2A C3A C13A -179.0(5) . . . . ? C2A C3A C4A C5A -0.5(8) . . . . ? C13A C3A C4A C5A 179.3(6) . . . . ? C3A C4A C5A C6A 0.8(9) . . . . ? C4A C5A C6A C1A -1.5(9) . . . . ? C2A C1A C6A C5A 1.7(8) . . . . ? C11A C1A C6A C5A 179.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.440 _refine_diff_density_min -1.060 _refine_diff_density_rms 0.106 # Attachment '3d.cif' data_3d _database_code_depnum_ccdc_archive 'CCDC 669058' # start Validation Reply Form _vrf_PLAT029_3d ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.88 RESPONSE: A few reflections were inaccessible with the data-acquisition regime employed. ; _vrf_PLAT220_3d ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 9.73 Ratio RESPONSE: The refinement of chemically sensible disordered groups was employed only for "well-behaved" disorder. Some minor disorder, which was not accounted, can lead to some uncertainty in values of ADP. ; _vrf_PLAT222_3d ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 6.82 Ratio RESPONSE: same as above ; _vrf_PLAT780_3d ; PROBLEM: Coordinates do not Form a Properly Connected Set ? RESPONSE: Because the uncertainty in positioning of disordered groups. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C78 H102 O30 P6, 0.5(C7 H8), H2 O' _chemical_formula_sum 'C81.50 H108 O31 P6' _chemical_formula_weight 1769.50 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.701(2) _cell_length_b 15.946(2) _cell_length_c 20.010(2) _cell_angle_alpha 72.218(2) _cell_angle_beta 85.667(2) _cell_angle_gamma 80.292(2) _cell_volume 4700.7(10) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 6520 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 28.23 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1870 _exptl_absorpt_coefficient_mu 0.190 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9026 _exptl_absorpt_correction_T_max 0.9193 _exptl_absorpt_process_details 'SADABS - Bruker area detector absorption corrections' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS CCD' _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 34889 _diffrn_reflns_av_R_equivalents 0.0201 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 28.54 _reflns_number_total 21036 _reflns_number_gt 13529 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL, v. 5.1' _computing_structure_refinement 'Bruker SHELXTL, v. 5.1' _computing_molecular_graphics 'Bruker SHELXTL, v. 5.1' _computing_publication_material 'Bruker SHELXTL, v. 5.1' _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. Some of the P(O)(OEt)2 groups is extremely disordered with high values of ADP's, which introduce large distortion in geometrical characteristics of the disordered group. Large number of geometrical constrains was used to keep chemically reasonable interatomic distances. Disorder also did not allowed to calculate proper positions of H-atoms in these groups. ; _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^+23.0000P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0019(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 21036 _refine_ls_number_parameters 983 _refine_ls_number_restraints 111 _refine_ls_R_factor_all 0.1752 _refine_ls_R_factor_gt 0.1346 _refine_ls_wR_factor_ref 0.3120 _refine_ls_wR_factor_gt 0.2911 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.164 _refine_ls_shift/su_max 0.004 _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 -0.3537(2) 1.3197(3) 0.11400(18) 0.0397(8) Uani 1 1 d . . . C11 C -0.3281(3) 1.3712(4) 0.1529(3) 0.0415(12) Uani 1 1 d . . . C12 C -0.3152(3) 1.4589(4) 0.1178(3) 0.0426(12) Uani 1 1 d . . . C13 C -0.2843(4) 1.5058(4) 0.1573(3) 0.0517(14) Uani 1 1 d . . . H13A H -0.2740 1.5652 0.1353 0.062 Uiso 1 1 calc R . . C14 C -0.2681(4) 1.4657(5) 0.2292(4) 0.0608(18) Uani 1 1 d . A . C15 C -0.2824(4) 1.3791(4) 0.2613(3) 0.0585(17) Uani 1 1 d . . . H15A H -0.2717 1.3526 0.3099 0.070 Uiso 1 1 calc R . . C16 C -0.3126(4) 1.3295(4) 0.2235(3) 0.0471(13) Uani 1 1 d . . . C17 C -0.4401(3) 1.3243(4) 0.1057(3) 0.0468(13) Uani 1 1 d . . . O17 O -0.4931(3) 1.3691(4) 0.1319(3) 0.0791(16) Uani 1 1 d . . . C18 C -0.4554(4) 1.2693(4) 0.0611(3) 0.0542(15) Uani 1 1 d . . . H18A H -0.5133 1.2523 0.0718 0.081 Uiso 1 1 calc R . . H18B H -0.4120 1.2155 0.0707 0.081 Uiso 1 1 calc R . . H18C H -0.4512 1.3038 0.0115 0.081 Uiso 1 1 calc R . . P1 P -0.22713(17) 1.52907(15) 0.27668(13) 0.0908(8) Uani 1 1 d D . . O11 O -0.1552(5) 1.5756(7) 0.2464(7) 0.112(4) Uiso 0.50 1 d PD A 1 O12 O -0.3130(4) 1.5863(5) 0.2966(5) 0.079(2) Uiso 0.50 1 d PD A 1 C121 C -0.3418(12) 1.6711(10) 0.2444(9) 0.112(4) Uiso 0.50 1 d PD A 1 H12A H -0.3609 1.6605 0.2020 0.134 Uiso 0.50 1 calc PR A 1 H12B H -0.2938 1.7064 0.2306 0.134 Uiso 0.50 1 calc PR A 1 C122 C -0.4148(14) 1.7202(11) 0.2757(13) 0.145(7) Uiso 0.50 1 d PD A 1 H12E H -0.4387 1.7748 0.2400 0.217 Uiso 0.50 1 calc PR A 1 H12F H -0.3940 1.7357 0.3147 0.217 Uiso 0.50 1 calc PR A 1 H12G H -0.4598 1.6825 0.2932 0.217 Uiso 0.50 1 calc PR A 1 O13 O -0.2183(9) 1.4633(8) 0.3542(4) 0.101(3) Uiso 0.50 1 d PD A 1 C131 C -0.1375(10) 1.4036(15) 0.3753(11) 0.155(7) Uiso 0.50 1 d PD A 1 C132 C -0.1512(15) 1.3375(12) 0.4443(10) 0.130(6) Uiso 0.50 1 d PD A 1 O11' O -0.2311(8) 1.4983(8) 0.3527(3) 0.112(4) Uiso 0.50 1 d PD A 2 O12' O -0.2581(6) 1.6312(4) 0.2385(5) 0.079(2) Uiso 0.50 1 d PD A 2 C12' C -0.3510(7) 1.6616(9) 0.2437(12) 0.112(4) Uiso 0.50 1 d PD A 2 H12C H -0.3787 1.6157 0.2797 0.134 Uiso 0.50 1 calc PR A 2 H12D H -0.3781 1.6724 0.1982 0.134 Uiso 0.50 1 calc PR A 2 C12" C -0.3624(14) 1.7454(13) 0.2636(16) 0.145(7) Uiso 0.50 1 d PD A 2 H12H H -0.4139 1.7482 0.2942 0.217 Uiso 0.50 1 calc PR A 2 H12I H -0.3692 1.7967 0.2212 0.217 Uiso 0.50 1 calc PR A 2 H12J H -0.3115 1.7467 0.2886 0.217 Uiso 0.50 1 calc PR A 2 O13' O -0.1335(5) 1.5396(10) 0.2405(6) 0.101(3) Uiso 0.50 1 d PD A 2 C13' C -0.0520(9) 1.4968(17) 0.2744(10) 0.155(7) Uiso 0.50 1 d PD A 2 H13D H -0.0481 1.4312 0.2871 0.186 Uiso 0.50 1 calc PR A 2 H13E H -0.0487 1.5132 0.3179 0.186 Uiso 0.50 1 calc PR A 2 C13" C 0.0201(6) 1.5264(19) 0.2253(14) 0.130(6) Uiso 0.50 1 d PD A 2 C1 C -0.3348(3) 1.5045(4) 0.0414(3) 0.0432(12) Uani 1 1 d . . . H1A H -0.3073 1.5590 0.0258 0.052 Uiso 1 1 calc R . . H1B H -0.3981 1.5236 0.0375 0.052 Uiso 1 1 calc R . . O2 O -0.1642(2) 1.3948(3) 0.0428(2) 0.0500(10) Uani 1 1 d . . . C21 C -0.2226(3) 1.4011(4) -0.0092(3) 0.0411(12) Uani 1 1 d . . . C22 C -0.1967(3) 1.3508(4) -0.0551(3) 0.0406(12) Uani 1 1 d . . . C23 C -0.2561(4) 1.3482(4) -0.1021(3) 0.0434(12) Uani 1 1 d . . . H23A H -0.2398 1.3142 -0.1339 0.052 Uiso 1 1 calc R . . C24 C -0.3399(3) 1.3953(4) -0.1031(3) 0.0412(12) Uani 1 1 d . . . C25 C -0.3633(3) 1.4459(4) -0.0569(3) 0.0401(12) Uani 1 1 d . . . H25A H -0.4200 1.4786 -0.0584 0.048 Uiso 1 1 calc R . . C26 C -0.3058(3) 1.4498(3) -0.0087(3) 0.0395(12) Uani 1 1 d . . . C27 C -0.1243(4) 1.4671(6) 0.0350(5) 0.070(2) Uani 1 1 d . . . O27 O -0.1370(4) 1.5328(4) -0.0123(4) 0.096(2) Uani 1 1 d . . . C28 C -0.0640(5) 1.4494(6) 0.0947(5) 0.092(3) Uani 1 1 d . . . H28A H -0.0444 1.5051 0.0937 0.138 Uiso 1 1 calc R . . H28B H -0.0139 1.4056 0.0899 0.138 Uiso 1 1 calc R . . H28C H -0.0945 1.4261 0.1395 0.138 Uiso 1 1 calc R . . P2 P -0.42150(10) 1.38780(12) -0.15790(8) 0.0532(4) Uani 1 1 d D . . O21 O -0.5071(2) 1.3881(3) -0.1227(2) 0.0598(11) Uani 1 1 d D . . O22 O -0.4135(3) 1.4662(3) -0.2262(2) 0.0826(17) Uani 1 1 d D . . C221 C -0.4857(5) 1.5145(5) -0.2698(5) 0.101(3) Uani 1 1 d D . . H22A H -0.5385 1.5203 -0.2402 0.121 Uiso 1 1 calc R . . H22B H -0.4963 1.4819 -0.3025 0.121 Uiso 1 1 calc R . . C222 C -0.4652(7) 1.6043(5) -0.3100(5) 0.139(5) Uani 1 1 d D . . H22C H -0.5145 1.6387 -0.3386 0.208 Uiso 1 1 calc R . . H22D H -0.4143 1.5980 -0.3406 0.208 Uiso 1 1 calc R . . H22E H -0.4533 1.6355 -0.2772 0.208 Uiso 1 1 calc R . . O23 O -0.3877(3) 1.3028(3) -0.1823(3) 0.0801(16) Uani 1 1 d D . . C231 C -0.3945(8) 1.2163(4) -0.1312(5) 0.122(4) Uani 1 1 d D . . H23B H -0.4549 1.2144 -0.1131 0.146 Uiso 1 1 calc R . . H23C H -0.3569 1.2063 -0.0910 0.146 Uiso 1 1 calc R . . C232 C -0.3674(9) 1.1463(5) -0.1662(8) 0.177(7) Uani 1 1 d D . . H23D H -0.3747 1.0881 -0.1333 0.265 Uiso 1 1 calc R . . H23E H -0.3065 1.1462 -0.1812 0.265 Uiso 1 1 calc R . . H23F H -0.4030 1.1584 -0.2072 0.265 Uiso 1 1 calc R . . C2 C -0.1066(3) 1.2976(4) -0.0519(3) 0.0456(13) Uani 1 1 d . . . H2A H -0.0898 1.2916 -0.0991 0.055 Uiso 1 1 calc R . . H2B H -0.0658 1.3319 -0.0403 0.055 Uiso 1 1 calc R . . O3 O 0.0556(2) 1.1896(3) -0.0309(2) 0.0521(10) Uani 1 1 d . . . C31 C -0.0142(3) 1.1537(4) 0.0112(3) 0.0390(11) Uani 1 1 d . . . C32 C 0.0012(3) 1.0669(4) 0.0553(3) 0.0365(11) Uani 1 1 d . . . C33 C -0.0702(3) 1.0300(4) 0.0904(3) 0.0387(11) Uani 1 1 d . . . H33A H -0.0623 0.9705 0.1205 0.046 Uiso 1 1 calc R . . C34 C -0.1534(3) 1.0795(4) 0.0820(3) 0.0386(11) Uani 1 1 d . . . C35 C -0.1656(3) 1.1666(4) 0.0381(3) 0.0375(11) Uani 1 1 d . . . H35A H -0.2220 1.2004 0.0334 0.045 Uiso 1 1 calc R . . C36 C -0.0961(3) 1.2054(4) 0.0007(3) 0.0372(11) Uani 1 1 d . . . C37 C 0.0928(4) 1.2463(5) -0.0083(4) 0.0595(17) Uani 1 1 d . . . O37 O 0.0712(3) 1.2635(4) 0.0453(3) 0.0732(14) Uani 1 1 d . . . C38 C 0.1626(4) 1.2833(6) -0.0618(5) 0.084(3) Uani 1 1 d . . . H38A H 0.2029 1.3060 -0.0390 0.126 Uiso 1 1 calc R . . H38B H 0.1354 1.3318 -0.1008 0.126 Uiso 1 1 calc R . . H38C H 0.1941 1.2358 -0.0797 0.126 Uiso 1 1 calc R . . P3 P -0.24401(9) 1.02828(10) 0.12591(8) 0.0458(4) Uani 1 1 d D B . O31 O -0.3154(2) 1.0913(3) 0.1429(2) 0.0577(11) Uani 1 1 d D . . O32 O -0.2647(3) 0.9765(3) 0.0763(2) 0.0678(13) Uani 1 1 d D . . C321 C -0.3392(5) 0.9296(6) 0.0929(5) 0.127(5) Uani 1 1 d D . . H32A H -0.3601 0.9250 0.1416 0.152 Uiso 1 1 calc R . . H32B H -0.3231 0.8687 0.0886 0.152 Uiso 1 1 calc R . . C322 C -0.4080(5) 0.9809(10) 0.0426(8) 0.204(9) Uani 1 1 d D . . H32C H -0.4551 0.9460 0.0476 0.307 Uiso 1 1 calc R . . H32D H -0.3839 0.9934 -0.0054 0.307 Uiso 1 1 calc R . . H32E H -0.4304 1.0372 0.0526 0.307 Uiso 1 1 calc R . . O33 O -0.2077(3) 0.9498(3) 0.1928(2) 0.0649(12) Uani 1 1 d D . . C331 C -0.1906(5) 0.9690(5) 0.2569(3) 0.074(2) Uiso 0.50 1 d PD B 1 H33B H -0.1747 1.0294 0.2450 0.089 Uiso 0.50 1 calc PR B 1 H33C H -0.1415 0.9256 0.2812 0.089 Uiso 0.50 1 calc PR B 1 C332 C -0.2678(8) 0.9635(11) 0.3036(5) 0.075(4) Uiso 0.50 1 d PD B 1 H33F H -0.2557 0.9759 0.3467 0.113 Uiso 0.50 1 calc PR B 1 H33G H -0.2833 0.9035 0.3154 0.113 Uiso 0.50 1 calc PR B 1 H33H H -0.3160 1.0073 0.2797 0.113 Uiso 0.50 1 calc PR B 1 C33' C -0.1906(5) 0.9690(5) 0.2569(3) 0.074(2) Uiso 0.50 1 d P B 2 H33D H -0.2193 1.0293 0.2568 0.089 Uiso 0.50 1 calc PR B 2 H33E H -0.1277 0.9643 0.2629 0.089 Uiso 0.50 1 calc PR B 2 C33" C -0.2303(12) 0.8950(13) 0.3160(10) 0.092(5) Uiso 0.50 1 d P B 2 H33I H -0.2168 0.8981 0.3621 0.138 Uiso 0.50 1 calc PR B 2 H33J H -0.2057 0.8362 0.3114 0.138 Uiso 0.50 1 calc PR B 2 H33K H -0.2931 0.9044 0.3114 0.138 Uiso 0.50 1 calc PR B 2 C3 C 0.0915(3) 1.0115(4) 0.0635(3) 0.0388(11) Uani 1 1 d . . . H3A H 0.0858 0.9484 0.0705 0.047 Uiso 1 1 calc R . . H3B H 0.1252 1.0319 0.0192 0.047 Uiso 1 1 calc R . . O4 O 0.0599(2) 0.9144(3) 0.2084(2) 0.0449(9) Uani 1 1 d . . . C41 C 0.1274(3) 0.9658(4) 0.1933(3) 0.0415(12) Uani 1 1 d . . . C42 C 0.1759(3) 0.9649(4) 0.2493(3) 0.0458(13) Uani 1 1 d . . . C43 C 0.2405(3) 1.0189(5) 0.2343(3) 0.0541(16) Uani 1 1 d . . . H43A H 0.2742 1.0204 0.2713 0.065 Uiso 1 1 calc R . . C44 C 0.2566(3) 1.0707(5) 0.1660(3) 0.0539(16) Uani 1 1 d . C . C45 C 0.2073(3) 1.0686(4) 0.1109(3) 0.0462(13) Uani 1 1 d . . . H45A H 0.2188 1.1034 0.0643 0.055 Uiso 1 1 calc R . . C46 C 0.1419(3) 1.0162(4) 0.1236(3) 0.0395(12) Uani 1 1 d . . . C47 C 0.0780(5) 0.8289(5) 0.2040(4) 0.0607(17) Uani 1 1 d . . . O47 O 0.1479(4) 0.7977(4) 0.1879(3) 0.0840(17) Uani 1 1 d . . . C48 C -0.0007(5) 0.7846(5) 0.2215(5) 0.076(2) Uani 1 1 d . . . H48A H 0.0160 0.7202 0.2298 0.114 Uiso 1 1 calc R . . H48B H -0.0405 0.8086 0.1824 0.114 Uiso 1 1 calc R . . H48C H -0.0293 0.7958 0.2639 0.114 Uiso 1 1 calc R . . P4 P 0.33933(13) 1.1381(2) 0.14680(10) 0.0931(9) Uani 1 1 d D . . O41 O 0.3645(6) 1.1737(6) 0.0722(2) 0.0694(18) Uiso 0.50 1 d PD C 1 O42 O 0.3142(9) 1.2080(6) 0.1887(4) 0.095(2) Uiso 0.50 1 d PD C 1 C421 C 0.2591(10) 1.2875(7) 0.1478(9) 0.098(4) Uiso 0.50 1 d PD C 1 H42A H 0.1974 1.2816 0.1587 0.117 Uiso 0.50 1 calc PR C 1 H42B H 0.2702 1.2961 0.0970 0.117 Uiso 0.50 1 calc PR C 1 C422 C 0.2799(14) 1.3645(6) 0.1671(12) 0.102(5) Uiso 0.50 1 d PD C 1 H42E H 0.2298 1.4120 0.1586 0.153 Uiso 0.50 1 calc PR C 1 H42F H 0.3294 1.3868 0.1384 0.153 Uiso 0.50 1 calc PR C 1 H42G H 0.2941 1.3457 0.2168 0.153 Uiso 0.50 1 calc PR C 1 O43 O 0.4119(5) 1.0698(5) 0.1968(4) 0.0626(17) Uiso 0.50 1 d PD C 1 C431 C 0.4859(9) 1.0977(9) 0.2198(9) 0.088(4) Uiso 0.50 1 d PD C 1 H43B H 0.4661 1.1475 0.2398 0.106 Uiso 0.50 1 calc PR C 1 H43C H 0.5256 1.1183 0.1794 0.106 Uiso 0.50 1 calc PR C 1 C432 C 0.5313(10) 1.0200(13) 0.2737(9) 0.110(5) Uiso 0.50 1 d PD C 1 H43F H 0.5817 1.0370 0.2894 0.165 Uiso 0.50 1 calc PR C 1 H43G H 0.5502 0.9709 0.2536 0.165 Uiso 0.50 1 calc PR C 1 H43H H 0.4918 1.0009 0.3139 0.165 Uiso 0.50 1 calc PR C 1 O41' O 0.3725(6) 1.1453(7) 0.0752(3) 0.0694(18) Uiso 0.50 1 d PD C 2 O42' O 0.3007(10) 1.2241(6) 0.1669(6) 0.095(2) Uiso 0.50 1 d PD C 2 C42' C 0.2817(14) 1.3175(7) 0.1280(7) 0.098(4) Uiso 0.50 1 d PD C 2 H42C H 0.2399 1.3259 0.0910 0.117 Uiso 0.50 1 calc PR C 2 H42D H 0.3352 1.3393 0.1051 0.117 Uiso 0.50 1 calc PR C 2 C42" C 0.2447(14) 1.3685(8) 0.1770(11) 0.102(5) Uiso 0.50 1 d PD C 2 H42H H 0.1980 1.4152 0.1542 0.153 Uiso 0.50 1 calc PR C 2 H42I H 0.2900 1.3958 0.1898 0.153 Uiso 0.50 1 calc PR C 2 H42J H 0.2218 1.3282 0.2194 0.153 Uiso 0.50 1 calc PR C 2 O43' O 0.4050(4) 1.1217(6) 0.2055(3) 0.0626(17) Uiso 0.50 1 d PD C 2 C43' C 0.4860(6) 1.0647(9) 0.1977(7) 0.088(4) Uiso 0.50 1 d PD C 2 H43D H 0.5357 1.0956 0.1978 0.106 Uiso 0.50 1 calc PR C 2 H43E H 0.4875 1.0506 0.1527 0.106 Uiso 0.50 1 calc PR C 2 C43" C 0.4915(12) 0.9815(8) 0.2574(10) 0.110(5) Uiso 0.50 1 d PD C 2 H43I H 0.5280 0.9331 0.2435 0.165 Uiso 0.50 1 calc PR C 2 H43J H 0.4334 0.9661 0.2704 0.165 Uiso 0.50 1 calc PR C 2 H43K H 0.5166 0.9905 0.2975 0.165 Uiso 0.50 1 calc PR C 2 C4 C 0.1634(4) 0.9038(5) 0.3226(3) 0.0528(15) Uani 1 1 d . . . H4A H 0.2069 0.9113 0.3529 0.063 Uiso 1 1 calc R . . H4B H 0.1762 0.8416 0.3208 0.063 Uiso 1 1 calc R . . O5 O 0.0680(3) 1.0768(3) 0.3268(2) 0.0575(11) Uani 1 1 d . . . C51 C 0.0344(4) 0.9989(4) 0.3647(3) 0.0463(13) Uani 1 1 d . . . C52 C -0.0421(4) 1.0086(4) 0.4045(3) 0.0461(13) Uani 1 1 d . . . C53 C -0.0809(4) 0.9336(5) 0.4342(3) 0.0547(15) Uani 1 1 d . . . H53A H -0.1330 0.9383 0.4612 0.066 Uiso 1 1 calc R . . C54 C -0.0458(5) 0.8522(5) 0.4257(4) 0.0639(18) Uani 1 1 d . . . C55 C 0.0340(4) 0.8442(5) 0.3890(4) 0.0601(16) Uani 1 1 d . . . H55A H 0.0601 0.7873 0.3857 0.072 Uiso 1 1 calc R . . C56 C 0.0748(4) 0.9164(4) 0.3580(3) 0.0489(14) Uani 1 1 d . . . C57 C 0.1289(4) 1.1031(5) 0.3583(4) 0.0596(17) Uani 1 1 d . . . O57 O 0.1579(3) 1.0599(4) 0.4131(3) 0.0740(14) Uani 1 1 d . . . C58 C 0.1501(6) 1.1922(6) 0.3144(5) 0.099(3) Uani 1 1 d . . . H58A H 0.1912 1.2113 0.3390 0.148 Uiso 1 1 calc R . . H58B H 0.0972 1.2359 0.3062 0.148 Uiso 1 1 calc R . . H58C H 0.1758 1.1874 0.2693 0.148 Uiso 1 1 calc R . . P5 P -0.1003(2) 0.7584(2) 0.4612(2) 0.1244(13) Uani 1 1 d D . . O51 O -0.1842(4) 0.7819(6) 0.4918(4) 0.138(3) Uiso 1 1 d D . . O52 O -0.1010(7) 0.7159(6) 0.3995(4) 0.173(4) Uiso 1 1 d D . . C521 C -0.1726(9) 0.6725(10) 0.3903(9) 0.208 Uiso 1 1 d D . . H52A H -0.1702 0.6665 0.3424 0.208 Uiso 1 1 calc R . . H52B H -0.2286 0.7083 0.3973 0.208 Uiso 1 1 calc R . . C522 C -0.1635(13) 0.5828(10) 0.4437(11) 0.260 Uiso 1 1 d D . . H52C H -0.2003 0.5460 0.4315 0.260 Uiso 1 1 calc R . . H52D H -0.1811 0.5893 0.4901 0.260 Uiso 1 1 calc R . . H52E H -0.1031 0.5541 0.4445 0.260 Uiso 1 1 calc R . . O53 O -0.0357(7) 0.6805(7) 0.5048(6) 0.237(6) Uiso 1 1 d D . . C531 C -0.0141(12) 0.6898(15) 0.5720(8) 0.284 Uiso 1 1 d D . . H53B H 0.0292 0.7305 0.5647 0.284 Uiso 1 1 calc R . . H53C H 0.0099 0.6311 0.6041 0.284 Uiso 1 1 calc R . . C532 C -0.0969(18) 0.727(2) 0.6018(12) 0.355 Uiso 1 1 d D . . C5 C -0.0771(4) 1.0964(4) 0.4189(3) 0.0472(13) Uani 1 1 d . . . H5A H -0.0649 1.0908 0.4680 0.057 Uiso 1 1 calc R . . H5B H -0.0458 1.1433 0.3879 0.057 Uiso 1 1 calc R . . O6 O -0.1546(3) 1.1567(3) 0.2815(2) 0.0524(10) Uani 1 1 d . . . C61 C -0.2078(4) 1.1605(4) 0.3408(3) 0.0479(14) Uani 1 1 d . . . C62 C -0.2954(4) 1.1904(4) 0.3298(3) 0.0520(15) Uani 1 1 d . . . C63 C -0.3503(4) 1.1825(5) 0.3877(3) 0.0560(16) Uani 1 1 d . . . H63A H -0.4105 1.2026 0.3814 0.067 Uiso 1 1 calc R . . C64 C -0.3190(4) 1.1453(5) 0.4557(3) 0.0573(16) Uani 1 1 d . D . C65 C -0.2306(4) 1.1192(4) 0.4648(3) 0.0509(14) Uani 1 1 d . . . H65A H -0.2090 1.0964 0.5110 0.061 Uiso 1 1 calc R . . C66 C -0.1732(4) 1.1258(4) 0.4077(3) 0.0461(13) Uani 1 1 d . . . C67 C -0.0972(4) 1.2161(5) 0.2558(3) 0.0554(16) Uani 1 1 d . . . O67 O -0.0862(3) 1.2705(3) 0.2829(2) 0.0638(12) Uani 1 1 d . . . C68 C -0.0524(5) 1.2007(6) 0.1907(3) 0.071(2) Uani 1 1 d . . . H68A H -0.0007 1.2297 0.1803 0.106 Uiso 1 1 calc R . . H68B H -0.0917 1.2258 0.1513 0.106 Uiso 1 1 calc R . . H68C H -0.0358 1.1365 0.1981 0.106 Uiso 1 1 calc R . . P6 P -0.39140(12) 1.12744(18) 0.53096(10) 0.0836(7) Uani 1 1 d D . . O61 O -0.4820(4) 1.1536(6) 0.5105(6) 0.084(2) Uiso 0.50 1 d PD D 1 O62 O -0.3679(6) 1.0313(4) 0.5823(5) 0.081(2) Uiso 0.50 1 d PD D 1 C621 C -0.3988(17) 0.9620(7) 0.5609(10) 0.126(6) Uiso 0.50 1 d PD D 1 H62A H -0.3745 0.9616 0.5138 0.151 Uiso 0.50 1 calc PR D 1 H62B H -0.4626 0.9737 0.5585 0.151 Uiso 0.50 1 calc PR D 1 C622 C -0.3707(17) 0.8749(5) 0.6133(13) 0.129(6) Uiso 0.50 1 d PD D 1 H62E H -0.3732 0.8267 0.5930 0.193 Uiso 0.50 1 calc PR D 1 H62F H -0.4089 0.8682 0.6550 0.193 Uiso 0.50 1 calc PR D 1 H62G H -0.3112 0.8723 0.6266 0.193 Uiso 0.50 1 calc PR D 1 O63 O -0.3599(5) 1.1873(5) 0.5721(4) 0.0608(16) Uiso 0.50 1 d PD D 1 C631 C -0.4050(14) 1.2105(15) 0.6318(10) 0.143(7) Uiso 0.50 1 d PD D 1 H63B H -0.3977 1.1585 0.6745 0.172 Uiso 0.50 1 calc PR D 1 H63C H -0.4676 1.2288 0.6226 0.172 Uiso 0.50 1 calc PR D 1 C632 C -0.3676(16) 1.2855(14) 0.6421(11) 0.135(6) Uiso 0.50 1 d PD D 1 H63F H -0.3991 1.3047 0.6803 0.203 Uiso 0.50 1 calc PR D 1 H63G H -0.3724 1.3355 0.5987 0.203 Uiso 0.50 1 calc PR D 1 H63H H -0.3065 1.2657 0.6538 0.203 Uiso 0.50 1 calc PR D 1 O61' O -0.3515(6) 1.1155(6) 0.5968(4) 0.084(2) Uiso 0.50 1 d PD D 2 O62' O -0.4253(7) 1.0384(5) 0.5275(5) 0.081(2) Uiso 0.50 1 d PD D 2 C62' C -0.3701(13) 0.9521(9) 0.5407(11) 0.126(6) Uiso 0.50 1 d PD D 2 H62C H -0.3101 0.9578 0.5487 0.151 Uiso 0.50 1 calc PR D 2 H62D H -0.3695 0.9294 0.4998 0.151 Uiso 0.50 1 calc PR D 2 C62" C -0.4054(18) 0.8895(9) 0.6041(12) 0.129(6) Uiso 0.50 1 d PD D 2 O63' O -0.4766(4) 1.1911(6) 0.5117(4) 0.0608(16) Uiso 0.50 1 d PD D 2 C63' C -0.5444(9) 1.1960(15) 0.5647(7) 0.143(7) Uiso 0.50 1 d PD D 2 H63D H -0.5228 1.2145 0.6025 0.172 Uiso 0.50 1 calc PR D 2 H63E H -0.5629 1.1370 0.5858 0.172 Uiso 0.50 1 calc PR D 2 C63" C -0.6185(8) 1.2627(15) 0.5298(12) 0.135(6) Uiso 0.50 1 d PD D 2 C6 C -0.3292(4) 1.2338(4) 0.2562(3) 0.0529(15) Uani 1 1 d . . . H6A H -0.3922 1.2330 0.2576 0.063 Uiso 1 1 calc R . . H6B H -0.3018 1.1977 0.2257 0.063 Uiso 1 1 calc R . . C1A C 0.0988(8) 0.5284(9) 0.2789(6) 0.091(2) Uiso 0.50 1 d PG E 1 C2A C 0.0474(7) 0.5528(9) 0.3317(7) 0.091(2) Uiso 0.50 1 d PG E 1 H2AA H -0.0125 0.5484 0.3352 0.109 Uiso 0.50 1 calc PR E 1 C3A C 0.0836(8) 0.5836(8) 0.3793(6) 0.091(2) Uiso 0.50 1 d PG E 1 H3AA H 0.0485 0.6002 0.4153 0.109 Uiso 0.50 1 calc PR E 1 C4A C 0.1712(8) 0.5900(8) 0.3740(6) 0.091(2) Uiso 0.50 1 d PG E 1 H4AA H 0.1960 0.6111 0.4066 0.109 Uiso 0.50 1 calc PR E 1 C5A C 0.2226(7) 0.5657(8) 0.3212(7) 0.091(2) Uiso 0.50 1 d PG E 1 H5AA H 0.2825 0.5701 0.3177 0.109 Uiso 0.50 1 calc PR E 1 C6A C 0.1864(8) 0.5349(8) 0.2737(6) 0.091(2) Uiso 0.50 1 d PG E 1 H6AA H 0.2215 0.5182 0.2376 0.109 Uiso 0.50 1 calc PR E 1 C7A C 0.0593(14) 0.4942(14) 0.2312(11) 0.093(6) Uiso 0.50 1 d P E 1 H7AA H 0.0912 0.4356 0.2318 0.139 Uiso 0.50 1 calc PR E 1 H7AB H 0.0610 0.5353 0.1836 0.139 Uiso 0.50 1 calc PR E 1 H7AC H -0.0009 0.4885 0.2462 0.139 Uiso 0.50 1 calc PR E 1 O1W O -0.6276(3) 1.2691(4) -0.0679(3) 0.0755(14) Uani 1 1 d . . . H1W H -0.5911 1.3048 -0.0841 0.113 Uiso 1 1 d . . . H2W H -0.6297 1.2399 -0.0248 0.113 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 0.0282(17) 0.052(2) 0.0378(19) -0.0135(16) -0.0029(14) -0.0018(15) C11 0.030(2) 0.053(3) 0.040(3) -0.019(2) -0.006(2) 0.006(2) C12 0.032(3) 0.048(3) 0.049(3) -0.019(3) -0.005(2) 0.006(2) C13 0.044(3) 0.051(4) 0.063(4) -0.025(3) -0.010(3) 0.005(3) C14 0.059(4) 0.062(4) 0.066(4) -0.033(3) -0.026(3) 0.015(3) C15 0.066(4) 0.060(4) 0.048(3) -0.023(3) -0.025(3) 0.020(3) C16 0.042(3) 0.052(3) 0.042(3) -0.014(3) -0.008(2) 0.011(2) C17 0.030(3) 0.054(4) 0.048(3) -0.004(3) -0.006(2) -0.002(2) O17 0.033(2) 0.094(4) 0.120(5) -0.053(4) -0.005(2) 0.005(2) C18 0.045(3) 0.065(4) 0.051(3) -0.008(3) -0.010(3) -0.017(3) P1 0.1166(19) 0.0720(14) 0.0930(16) -0.0457(12) -0.0621(15) 0.0262(13) C1 0.039(3) 0.041(3) 0.047(3) -0.014(2) -0.002(2) 0.003(2) O2 0.0327(19) 0.056(3) 0.063(3) -0.024(2) -0.0044(17) -0.0001(17) C21 0.033(3) 0.040(3) 0.046(3) -0.009(2) 0.000(2) -0.001(2) C22 0.034(3) 0.037(3) 0.044(3) -0.007(2) 0.008(2) -0.001(2) C23 0.045(3) 0.039(3) 0.040(3) -0.007(2) 0.006(2) 0.000(2) C24 0.038(3) 0.043(3) 0.037(3) -0.008(2) 0.001(2) 0.000(2) C25 0.035(3) 0.040(3) 0.038(3) -0.006(2) 0.003(2) 0.003(2) C26 0.037(3) 0.038(3) 0.038(3) -0.008(2) 0.003(2) 0.002(2) C27 0.041(3) 0.069(5) 0.109(6) -0.042(5) -0.007(4) -0.002(3) O27 0.070(4) 0.065(4) 0.150(6) -0.015(4) -0.024(4) -0.022(3) C28 0.054(4) 0.102(7) 0.142(8) -0.071(6) -0.032(5) 0.003(4) P2 0.0477(8) 0.0662(11) 0.0428(8) -0.0185(7) -0.0058(6) 0.0057(7) O21 0.048(2) 0.075(3) 0.057(3) -0.021(2) -0.0039(19) -0.009(2) O22 0.053(3) 0.117(4) 0.046(3) 0.006(3) 0.000(2) 0.018(3) C221 0.083(6) 0.100(7) 0.089(6) 0.003(5) -0.019(5) 0.018(5) C222 0.153(11) 0.109(9) 0.102(8) 0.014(7) 0.012(7) 0.032(8) O23 0.074(3) 0.097(4) 0.082(4) -0.055(3) -0.023(3) 0.012(3) C231 0.113(8) 0.098(8) 0.178(12) -0.076(9) 0.007(8) -0.018(7) C232 0.140(12) 0.135(11) 0.29(2) -0.137(14) -0.021(12) 0.017(9) C2 0.034(3) 0.045(3) 0.053(3) -0.012(3) 0.009(2) -0.003(2) O3 0.0306(19) 0.052(2) 0.070(3) -0.017(2) 0.0056(18) -0.0031(17) C31 0.026(2) 0.049(3) 0.045(3) -0.021(2) 0.001(2) -0.004(2) C32 0.027(2) 0.046(3) 0.041(3) -0.022(2) -0.0041(19) 0.000(2) C33 0.031(2) 0.046(3) 0.039(3) -0.014(2) -0.002(2) -0.001(2) C34 0.028(2) 0.050(3) 0.040(3) -0.017(2) -0.0009(19) -0.004(2) C35 0.025(2) 0.047(3) 0.042(3) -0.018(2) -0.0024(19) 0.000(2) C36 0.029(2) 0.043(3) 0.040(3) -0.017(2) 0.0011(19) -0.002(2) C37 0.035(3) 0.071(5) 0.073(5) -0.026(4) -0.002(3) -0.003(3) O37 0.059(3) 0.083(4) 0.091(4) -0.040(3) 0.005(3) -0.024(3) C38 0.043(4) 0.090(6) 0.109(7) -0.014(5) 0.014(4) -0.023(4) P3 0.0304(7) 0.0505(9) 0.0542(9) -0.0138(7) 0.0043(6) -0.0054(6) O31 0.037(2) 0.066(3) 0.069(3) -0.023(2) 0.0097(19) -0.0069(19) O32 0.046(2) 0.088(4) 0.085(3) -0.045(3) 0.017(2) -0.026(2) C321 0.078(6) 0.167(11) 0.195(12) -0.124(10) 0.033(7) -0.066(7) C322 0.079(8) 0.30(2) 0.32(2) -0.20(2) -0.025(11) -0.037(11) O33 0.061(3) 0.058(3) 0.068(3) -0.009(2) 0.005(2) -0.007(2) C3 0.027(2) 0.049(3) 0.043(3) -0.021(2) -0.003(2) 0.002(2) O4 0.041(2) 0.043(2) 0.051(2) -0.0163(18) -0.0032(16) -0.0003(16) C41 0.029(2) 0.049(3) 0.047(3) -0.019(2) -0.003(2) 0.004(2) C42 0.031(3) 0.061(4) 0.041(3) -0.016(3) -0.005(2) 0.007(2) C43 0.031(3) 0.090(5) 0.043(3) -0.023(3) -0.006(2) -0.003(3) C44 0.027(2) 0.094(5) 0.046(3) -0.027(3) -0.001(2) -0.012(3) C45 0.027(2) 0.071(4) 0.041(3) -0.020(3) 0.000(2) -0.004(2) C46 0.026(2) 0.051(3) 0.042(3) -0.020(2) -0.0044(19) 0.005(2) C47 0.071(4) 0.052(4) 0.060(4) -0.021(3) -0.009(3) 0.002(3) O47 0.071(3) 0.068(3) 0.116(5) -0.047(3) -0.004(3) 0.018(3) C48 0.089(6) 0.046(4) 0.091(6) -0.016(4) -0.003(4) -0.013(4) P4 0.0607(12) 0.187(3) 0.0489(10) -0.0350(13) 0.0056(8) -0.0710(15) C4 0.040(3) 0.068(4) 0.044(3) -0.014(3) -0.008(2) 0.009(3) O5 0.059(3) 0.057(3) 0.042(2) 0.0001(19) 0.0012(19) 0.002(2) C51 0.040(3) 0.055(4) 0.037(3) -0.008(2) -0.007(2) 0.002(2) C52 0.039(3) 0.055(4) 0.039(3) -0.011(3) -0.010(2) 0.004(2) C53 0.042(3) 0.066(4) 0.057(4) -0.021(3) 0.001(3) -0.006(3) C54 0.058(4) 0.065(4) 0.073(5) -0.027(4) 0.009(3) -0.015(3) C55 0.058(4) 0.057(4) 0.067(4) -0.025(3) -0.001(3) -0.002(3) C56 0.042(3) 0.060(4) 0.039(3) -0.012(3) -0.007(2) 0.006(3) C57 0.050(4) 0.054(4) 0.068(4) -0.014(3) 0.014(3) -0.003(3) O57 0.075(3) 0.068(3) 0.078(3) -0.016(3) -0.018(3) -0.011(3) C58 0.083(6) 0.072(6) 0.117(8) 0.002(5) 0.033(5) -0.020(4) P5 0.118(2) 0.094(2) 0.184(3) -0.077(2) 0.076(2) -0.0500(18) C5 0.044(3) 0.054(3) 0.039(3) -0.012(3) -0.006(2) 0.004(3) O6 0.051(2) 0.065(3) 0.036(2) -0.0149(19) -0.0012(17) 0.005(2) C61 0.049(3) 0.053(3) 0.036(3) -0.012(2) -0.004(2) 0.007(3) C62 0.049(3) 0.061(4) 0.039(3) -0.011(3) -0.009(2) 0.010(3) C63 0.044(3) 0.071(4) 0.044(3) -0.014(3) -0.006(2) 0.010(3) C64 0.049(3) 0.075(4) 0.040(3) -0.014(3) -0.002(3) 0.007(3) C65 0.047(3) 0.064(4) 0.035(3) -0.010(3) -0.007(2) 0.004(3) C66 0.043(3) 0.050(3) 0.040(3) -0.011(2) -0.005(2) 0.004(2) C67 0.058(4) 0.057(4) 0.040(3) -0.009(3) -0.004(3) 0.011(3) O67 0.071(3) 0.060(3) 0.053(3) -0.012(2) 0.005(2) -0.002(2) C68 0.067(4) 0.096(6) 0.042(3) -0.020(4) 0.009(3) -0.003(4) P6 0.0494(10) 0.151(2) 0.0450(10) -0.0250(12) 0.0006(8) -0.0100(12) C6 0.050(3) 0.066(4) 0.037(3) -0.014(3) -0.010(2) 0.010(3) O1W 0.064(3) 0.084(4) 0.078(3) -0.012(3) -0.015(3) -0.026(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 O1 C17 1.366(6) . ? O1 C11 1.410(6) . ? C11 C16 1.387(7) . ? C11 C12 1.402(8) . ? C12 C13 1.400(8) . ? C12 C1 1.508(8) . ? C13 C14 1.408(9) . ? C13 H13A 0.9500 . ? C14 C15 1.382(10) . ? C14 P1 1.799(7) . ? C15 C16 1.402(9) . ? C15 H15A 0.9500 . ? C16 C6 1.525(9) . ? C17 O17 1.201(7) . ? C17 C18 1.485(9) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? P1 O11 1.448(5) . ? P1 O11' 1.448(5) . ? P1 O12' 1.581(4) . ? P1 O13 1.586(5) . ? P1 O12 1.592(4) . ? P1 O13' 1.601(5) . ? O12 C121 1.458(5) . ? C121 C122 1.486(5) . ? C121 H12A 0.9900 . ? C121 H12B 0.9900 . ? C122 H12E 0.9800 . ? C122 H12F 0.9800 . ? C122 H12G 0.9800 . ? O13 C131 1.456(5) . ? C131 C132 1.486(5) . ? O12' C12' 1.464(5) . ? C12' C12" 1.488(5) . ? C12' H12C 0.9900 . ? C12' H12D 0.9900 . ? C12" H12H 0.9800 . ? C12" H12I 0.9800 . ? C12" H12J 0.9800 . ? O13' C13' 1.454(5) . ? C13' C13" 1.484(5) . ? C13' H13D 0.9900 . ? C13' H13E 0.9900 . ? C1 C26 1.519(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? O2 C27 1.367(9) . ? O2 C21 1.409(7) . ? C21 C22 1.390(7) . ? C21 C26 1.403(7) . ? C22 C23 1.389(8) . ? C22 C2 1.517(7) . ? C23 C24 1.398(7) . ? C23 H23A 0.9500 . ? C24 C25 1.395(7) . ? C24 P2 1.790(6) . ? C25 C26 1.392(8) . ? C25 H25A 0.9500 . ? C27 O27 1.178(10) . ? C27 C28 1.510(11) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? P2 O21 1.469(3) . ? P2 O22 1.559(3) . ? P2 O23 1.574(3) . ? O22 C221 1.443(5) . ? C221 C222 1.489(5) . ? C221 H22A 0.9900 . ? C221 H22B 0.9900 . ? C222 H22C 0.9800 . ? C222 H22D 0.9800 . ? C222 H22E 0.9800 . ? O23 C231 1.461(5) . ? C231 C232 1.479(5) . ? C231 H23B 0.9900 . ? C231 H23C 0.9900 . ? C232 H23D 0.9800 . ? C232 H23E 0.9800 . ? C232 H23F 0.9800 . ? C2 C36 1.515(8) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? O3 C37 1.352(8) . ? O3 C31 1.420(6) . ? C31 C32 1.388(8) . ? C31 C36 1.399(7) . ? C32 C33 1.395(7) . ? C32 C3 1.531(6) . ? C33 C34 1.401(7) . ? C33 H33A 0.9500 . ? C34 C35 1.389(8) . ? C34 P3 1.797(5) . ? C35 C36 1.398(7) . ? C35 H35A 0.9500 . ? C37 O37 1.198(8) . ? C37 C38 1.533(10) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? P3 O31 1.467(3) . ? P3 O32 1.554(3) . ? P3 O33 1.592(3) . ? O32 C321 1.457(4) . ? C321 C322 1.487(5) . ? C321 H32A 0.9900 . ? C321 H32B 0.9900 . ? C322 H32C 0.9800 . ? C322 H32D 0.9800 . ? C322 H32E 0.9800 . ? O33 C331 1.461(4) . ? C331 C332 1.471(5) . ? C331 H33B 0.9900 . ? C331 H33C 0.9900 . ? C332 H33F 0.9800 . ? C332 H33G 0.9800 . ? C332 H33H 0.9800 . ? C33" H33I 0.9800 . ? C33" H33J 0.9800 . ? C33" H33K 0.9800 . ? C3 C46 1.516(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? O4 C47 1.374(7) . ? O4 C41 1.407(7) . ? C41 C42 1.396(7) . ? C41 C46 1.403(8) . ? C42 C43 1.398(9) . ? C42 C4 1.513(8) . ? C43 C44 1.393(9) . ? C43 H43A 0.9500 . ? C44 C45 1.407(8) . ? C44 P4 1.770(6) . ? C45 C46 1.392(8) . ? C45 H45A 0.9500 . ? C47 O47 1.190(8) . ? C47 C48 1.493(10) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? P4 O41' 1.465(4) . ? P4 O41 1.474(4) . ? P4 O43' 1.555(4) . ? P4 O42' 1.559(5) . ? P4 O42 1.573(5) . ? P4 O43 1.604(4) . ? O42 C421 1.459(5) . ? C421 C422 1.485(5) . ? C421 H42A 0.9900 . ? C421 H42B 0.9900 . ? C422 H42E 0.9800 . ? C422 H42F 0.9800 . ? C422 H42G 0.9800 . ? O43 C431 1.463(5) . ? C431 C432 1.487(5) . ? C431 H43B 0.9900 . ? C431 H43C 0.9900 . ? C432 H43F 0.9800 . ? C432 H43G 0.9800 . ? C432 H43H 0.9800 . ? O42' C42' 1.447(5) . ? C42' C42" 1.484(5) . ? C42' H42C 0.9900 . ? C42' H42D 0.9900 . ? C42" H42H 0.9800 . ? C42" H42I 0.9800 . ? C42" H42J 0.9800 . ? O43' C43' 1.461(5) . ? C43' C43" 1.483(5) . ? C43' H43D 0.9900 . ? C43' H43E 0.9900 . ? C43" H43I 0.9800 . ? C43" H43J 0.9800 . ? C43" H43K 0.9800 . ? C4 C56 1.523(8) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? O5 C57 1.368(9) . ? O5 C51 1.408(7) . ? C51 C56 1.402(8) . ? C51 C52 1.402(8) . ? C52 C53 1.383(9) . ? C52 C5 1.519(8) . ? C53 C54 1.379(9) . ? C53 H53A 0.9500 . ? C54 C55 1.411(9) . ? C54 P5 1.778(8) . ? C55 C56 1.368(9) . ? C55 H55A 0.9500 . ? C57 O57 1.181(8) . ? C57 C58 1.502(10) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? P5 O51 1.450(5) . ? P5 O53 1.542(5) . ? P5 O52 1.582(5) . ? O52 C521 1.466(5) . ? C521 C522 1.493(5) . ? C521 H52A 0.9900 . ? C521 H52B 0.9900 . ? C522 H52C 0.9800 . ? C522 H52D 0.9800 . ? C522 H52E 0.9800 . ? O53 C531 1.466(5) . ? C531 C532 1.497(5) . ? C531 H53B 0.9900 . ? C531 H53C 0.9900 . ? C5 C66 1.515(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? O6 C67 1.376(8) . ? O6 C61 1.410(7) . ? C61 C62 1.389(8) . ? C61 C66 1.396(7) . ? C62 C63 1.377(8) . ? C62 C6 1.517(7) . ? C63 C64 1.397(8) . ? C63 H63A 0.9500 . ? C64 C65 1.390(8) . ? C64 P6 1.797(6) . ? C65 C66 1.391(8) . ? C65 H65A 0.9500 . ? C67 O67 1.195(8) . ? C67 C68 1.500(9) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? P6 O61' 1.448(4) . ? P6 O61 1.466(4) . ? P6 O63' 1.533(4) . ? P6 O62 1.564(4) . ? P6 O63 1.592(4) . ? P6 O62' 1.620(4) . ? O62 C621 1.463(5) . ? C621 C622 1.483(5) . ? C621 H62A 0.9900 . ? C621 H62B 0.9900 . ? C622 H62E 0.9800 . ? C622 H62F 0.9800 . ? C622 H62G 0.9800 . ? O63 C631 1.455(5) . ? C631 C632 1.492(5) . ? C631 H63B 0.9900 . ? C631 H63C 0.9900 . ? C632 H63F 0.9800 . ? C632 H63G 0.9800 . ? C632 H63H 0.9800 . ? O62' C62' 1.459(5) . ? C62' C62" 1.489(5) . ? C62' H62C 0.9900 . ? C62' H62D 0.9900 . ? O63' C63' 1.456(5) . ? C63' C63" 1.491(5) . ? C63' H63D 0.9900 . ? C63' H63E 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C1A C6A 1.391(8) . ? C1A C2A 1.391(8) . ? C1A C7A 1.45(2) . ? C2A C3A 1.390(8) . ? C2A H2AA 0.9500 . ? C3A C4A 1.391(8) . ? C3A H3AA 0.9500 . ? C4A C5A 1.391(8) . ? C4A H4AA 0.9500 . ? C5A C6A 1.390(8) . ? C5A H5AA 0.9500 . ? C6A H6AA 0.9500 . ? C7A H7AA 0.9800 . ? C7A H7AB 0.9800 . ? C7A H7AC 0.9800 . ? O1W H1W 0.8528 . ? O1W H2W 0.8466 . ? 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 C17 O1 C11 118.1(4) . . ? C16 C11 C12 123.8(5) . . ? C16 C11 O1 117.2(5) . . ? C12 C11 O1 118.9(5) . . ? C13 C12 C11 117.1(5) . . ? C13 C12 C1 119.5(5) . . ? C11 C12 C1 123.4(5) . . ? C12 C13 C14 120.6(6) . . ? C12 C13 H13A 119.7 . . ? C14 C13 H13A 119.7 . . ? C15 C14 C13 119.9(6) . . ? C15 C14 P1 121.7(5) . . ? C13 C14 P1 118.4(6) . . ? C14 C15 C16 121.3(6) . . ? C14 C15 H15A 119.4 . . ? C16 C15 H15A 119.4 . . ? C11 C16 C15 117.3(6) . . ? C11 C16 C6 119.3(5) . . ? C15 C16 C6 123.4(5) . . ? O17 C17 O1 121.3(6) . . ? O17 C17 C18 127.7(5) . . ? O1 C17 C18 111.0(5) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O11 P1 O11' 115.1(10) . . ? O11 P1 O12' 68.1(5) . . ? O11' P1 O12' 118.4(5) . . ? O11 P1 O13 117.8(5) . . ? O11' P1 O13 20.3(7) . . ? O12' P1 O13 138.7(7) . . ? O11 P1 O12 117.5(5) . . ? O11' P1 O12 76.2(6) . . ? O12' P1 O12 55.1(5) . . ? O13 P1 O12 92.6(6) . . ? O11 P1 O13' 24.2(7) . . ? O11' P1 O13' 116.6(5) . . ? O12' P1 O13' 89.0(6) . . ? O13 P1 O13' 110.2(8) . . ? O12 P1 O13' 141.5(6) . . ? O11 P1 C14 118.8(7) . . ? O11' P1 C14 118.4(7) . . ? O12' P1 C14 107.7(4) . . ? O13 P1 C14 103.6(6) . . ? O12 P1 C14 102.3(5) . . ? O13' P1 C14 101.9(6) . . ? C121 O12 P1 116.0(6) . . ? O12 C121 C122 108.3(5) . . ? O12 C121 H12A 110.0 . . ? C122 C121 H12A 110.0 . . ? O12 C121 H12B 110.0 . . ? C122 C121 H12B 110.0 . . ? H12A C121 H12B 108.4 . . ? C131 O13 P1 119.8(11) . . ? O13 C131 C132 109.2(5) . . ? C12' O12' P1 115.5(7) . . ? O12' C12' C12" 107.7(5) . . ? O12' C12' H12C 110.2 . . ? C12" C12' H12C 110.2 . . ? O12' C12' H12D 110.2 . . ? C12" C12' H12D 110.2 . . ? H12C C12' H12D 108.5 . . ? C12' C12" H12H 109.5 . . ? C12' C12" H12I 109.5 . . ? H12H C12" H12I 109.5 . . ? C12' C12" H12J 109.5 . . ? H12H C12" H12J 109.5 . . ? H12I C12" H12J 109.5 . . ? C13' O13' P1 124.9(11) . . ? O13' C13' C13" 108.8(5) . . ? O13' C13' H13D 109.9 . . ? C13" C13' H13D 109.9 . . ? O13' C13' H13E 109.9 . . ? C13" C13' H13E 109.9 . . ? H13D C13' H13E 108.3 . . ? C12 C1 C26 116.2(4) . . ? C12 C1 H1A 108.2 . . ? C26 C1 H1A 108.2 . . ? C12 C1 H1B 108.2 . . ? C26 C1 H1B 108.2 . . ? H1A C1 H1B 107.4 . . ? C27 O2 C21 117.0(5) . . ? C22 C21 C26 123.0(5) . . ? C22 C21 O2 117.1(4) . . ? C26 C21 O2 119.6(5) . . ? C23 C22 C21 118.4(5) . . ? C23 C22 C2 121.0(5) . . ? C21 C22 C2 120.6(5) . . ? C22 C23 C24 120.5(5) . . ? C22 C23 H23A 119.7 . . ? C24 C23 H23A 119.7 . . ? C25 C24 C23 119.5(5) . . ? C25 C24 P2 117.9(4) . . ? C23 C24 P2 122.4(4) . . ? C26 C25 C24 121.7(5) . . ? C26 C25 H25A 119.2 . . ? C24 C25 H25A 119.2 . . ? C25 C26 C21 116.8(5) . . ? C25 C26 C1 119.7(4) . . ? C21 C26 C1 123.5(5) . . ? O27 C27 O2 123.0(7) . . ? O27 C27 C28 126.7(8) . . ? O2 C27 C28 110.3(8) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O21 P2 O22 115.8(2) . . ? O21 P2 O23 114.8(3) . . ? O22 P2 O23 103.1(3) . . ? O21 P2 C24 112.2(3) . . ? O22 P2 C24 103.9(3) . . ? O23 P2 C24 106.0(3) . . ? C221 O22 P2 123.5(4) . . ? O22 C221 C222 108.5(5) . . ? O22 C221 H22A 110.0 . . ? C222 C221 H22A 110.0 . . ? O22 C221 H22B 110.0 . . ? C222 C221 H22B 110.0 . . ? H22A C221 H22B 108.4 . . ? C221 C222 H22C 109.5 . . ? C221 C222 H22D 109.5 . . ? H22C C222 H22D 109.5 . . ? C221 C222 H22E 109.5 . . ? H22C C222 H22E 109.5 . . ? H22D C222 H22E 109.5 . . ? C231 O23 P2 116.9(4) . . ? O23 C231 C232 108.4(5) . . ? O23 C231 H23B 110.0 . . ? C232 C231 H23B 110.0 . . ? O23 C231 H23C 110.0 . . ? C232 C231 H23C 110.0 . . ? H23B C231 H23C 108.4 . . ? C231 C232 H23D 109.5 . . ? C231 C232 H23E 109.5 . . ? H23D C232 H23E 109.5 . . ? C231 C232 H23F 109.5 . . ? H23D C232 H23F 109.5 . . ? H23E C232 H23F 109.5 . . ? C36 C2 C22 115.4(4) . . ? C36 C2 H2A 108.4 . . ? C22 C2 H2A 108.4 . . ? C36 C2 H2B 108.4 . . ? C22 C2 H2B 108.4 . . ? H2A C2 H2B 107.5 . . ? C37 O3 C31 116.2(5) . . ? C32 C31 C36 123.9(5) . . ? C32 C31 O3 118.3(4) . . ? C36 C31 O3 117.5(5) . . ? C31 C32 C33 117.1(4) . . ? C31 C32 C3 122.2(5) . . ? C33 C32 C3 120.6(5) . . ? C32 C33 C34 121.0(5) . . ? C32 C33 H33A 119.5 . . ? C34 C33 H33A 119.5 . . ? C35 C34 C33 119.9(5) . . ? C35 C34 P3 120.5(4) . . ? C33 C34 P3 119.6(4) . . ? C34 C35 C36 121.0(4) . . ? C34 C35 H35A 119.5 . . ? C36 C35 H35A 119.5 . . ? C35 C36 C31 117.1(5) . . ? C35 C36 C2 123.2(4) . . ? C31 C36 C2 119.6(5) . . ? O37 C37 O3 122.9(6) . . ? O37 C37 C38 127.6(7) . . ? O3 C37 C38 109.5(6) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O31 P3 O32 116.6(2) . . ? O31 P3 O33 113.4(2) . . ? O32 P3 O33 102.2(3) . . ? O31 P3 C34 113.7(3) . . ? O32 P3 C34 102.8(2) . . ? O33 P3 C34 106.9(2) . . ? C321 O32 P3 118.9(4) . . ? O32 C321 C322 108.0(5) . . ? O32 C321 H32A 110.1 . . ? C322 C321 H32A 110.1 . . ? O32 C321 H32B 110.1 . . ? C322 C321 H32B 110.1 . . ? H32A C321 H32B 108.4 . . ? C321 C322 H32C 109.5 . . ? C321 C322 H32D 109.5 . . ? H32C C322 H32D 109.5 . . ? C321 C322 H32E 109.5 . . ? H32C C322 H32E 109.5 . . ? H32D C322 H32E 109.5 . . ? C331 O33 P3 120.4(4) . . ? O33 C331 C332 109.9(5) . . ? O33 C331 H33B 109.7 . . ? C332 C331 H33B 109.7 . . ? O33 C331 H33C 109.7 . . ? C332 C331 H33C 109.7 . . ? H33B C331 H33C 108.2 . . ? H33I C33" H33J 109.5 . . ? H33I C33" H33K 109.5 . . ? H33J C33" H33K 109.5 . . ? C46 C3 C32 114.7(4) . . ? C46 C3 H3A 108.6 . . ? C32 C3 H3A 108.6 . . ? C46 C3 H3B 108.6 . . ? C32 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? C47 O4 C41 117.8(5) . . ? C42 C41 C46 123.4(5) . . ? C42 C41 O4 117.7(5) . . ? C46 C41 O4 118.9(5) . . ? C41 C42 C43 117.4(5) . . ? C41 C42 C4 121.8(6) . . ? C43 C42 C4 120.7(5) . . ? C44 C43 C42 121.2(5) . . ? C44 C43 H43A 119.4 . . ? C42 C43 H43A 119.4 . . ? C43 C44 C45 119.7(6) . . ? C43 C44 P4 121.3(4) . . ? C45 C44 P4 119.1(5) . . ? C46 C45 C44 121.0(5) . . ? C46 C45 H45A 119.5 . . ? C44 C45 H45A 119.5 . . ? C45 C46 C41 117.4(5) . . ? C45 C46 C3 120.5(5) . . ? C41 C46 C3 122.0(5) . . ? O47 C47 O4 122.4(7) . . ? O47 C47 C48 127.0(7) . . ? O4 C47 C48 110.6(6) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O41' P4 O41 17.1(6) . . ? O41' P4 O43' 118.6(4) . . ? O41 P4 O43' 120.7(6) . . ? O41' P4 O42' 119.7(4) . . ? O41 P4 O42' 102.7(6) . . ? O43' P4 O42' 85.5(6) . . ? O41' P4 O42 133.1(7) . . ? O41 P4 O42 116.4(4) . . ? O43' P4 O42 69.4(5) . . ? O42' P4 O42 17.5(6) . . ? O41' P4 O43 105.1(5) . . ? O41 P4 O43 116.4(4) . . ? O43' P4 O43 32.5(4) . . ? O42' P4 O43 117.0(6) . . ? O42 P4 O43 99.9(5) . . ? O41' P4 C44 108.7(5) . . ? O41 P4 C44 116.8(5) . . ? O43' P4 C44 116.8(4) . . ? O42' P4 C44 105.7(6) . . ? O42 P4 C44 106.1(6) . . ? O43 P4 C44 98.4(4) . . ? C421 O42 P4 111.4(6) . . ? O42 C421 C422 107.4(5) . . ? O42 C421 H42A 110.2 . . ? C422 C421 H42A 110.2 . . ? O42 C421 H42B 110.2 . . ? C422 C421 H42B 110.2 . . ? H42A C421 H42B 108.5 . . ? C431 O43 P4 123.1(8) . . ? O43 C431 C432 108.1(5) . . ? O43 C431 H43B 110.1 . . ? C432 C431 H43B 110.1 . . ? O43 C431 H43C 110.1 . . ? C432 C431 H43C 110.1 . . ? H43B C431 H43C 108.4 . . ? C42' O42' P4 134.2(9) . . ? O42' C42' C42" 109.0(5) . . ? O42' C42' H42C 109.9 . . ? C42" C42' H42C 109.9 . . ? O42' C42' H42D 109.9 . . ? C42" C42' H42D 109.9 . . ? H42C C42' H42D 108.3 . . ? C42' C42" H42H 109.5 . . ? C42' C42" H42I 109.5 . . ? H42H C42" H42I 109.5 . . ? C42' C42" H42J 109.5 . . ? H42H C42" H42J 109.5 . . ? H42I C42" H42J 109.5 . . ? C43' O43' P4 114.4(6) . . ? O43' C43' C43" 108.2(5) . . ? O43' C43' H43D 110.1 . . ? C43" C43' H43D 110.1 . . ? O43' C43' H43E 110.1 . . ? C43" C43' H43E 110.1 . . ? H43D C43' H43E 108.4 . . ? C43' C43" H43I 109.5 . . ? C43' C43" H43J 109.5 . . ? H43I C43" H43J 109.5 . . ? C43' C43" H43K 109.5 . . ? H43I C43" H43K 109.5 . . ? H43J C43" H43K 109.5 . . ? C42 C4 C56 117.2(5) . . ? C42 C4 H4A 108.0 . . ? C56 C4 H4A 108.0 . . ? C42 C4 H4B 108.0 . . ? C56 C4 H4B 108.0 . . ? H4A C4 H4B 107.2 . . ? C57 O5 C51 117.8(5) . . ? C56 C51 C52 122.8(6) . . ? C56 C51 O5 119.4(5) . . ? C52 C51 O5 117.6(5) . . ? C53 C52 C51 117.4(6) . . ? C53 C52 C5 121.2(5) . . ? C51 C52 C5 121.2(6) . . ? C54 C53 C52 121.5(6) . . ? C54 C53 H53A 119.2 . . ? C52 C53 H53A 119.2 . . ? C53 C54 C55 119.1(6) . . ? C53 C54 P5 120.2(5) . . ? C55 C54 P5 120.7(6) . . ? C56 C55 C54 121.7(6) . . ? C56 C55 H55A 119.1 . . ? C54 C55 H55A 119.1 . . ? C55 C56 C51 117.2(6) . . ? C55 C56 C4 119.9(6) . . ? C51 C56 C4 122.8(6) . . ? O57 C57 O5 122.5(6) . . ? O57 C57 C58 126.7(8) . . ? O5 C57 C58 110.7(7) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? O51 P5 O53 119.4(5) . . ? O51 P5 O52 115.7(5) . . ? O53 P5 O52 93.9(6) . . ? O51 P5 C54 112.2(5) . . ? O53 P5 C54 108.4(6) . . ? O52 P5 C54 105.2(5) . . ? C521 O52 P5 122.4(10) . . ? O52 C521 C522 107.3(5) . . ? O52 C521 H52A 110.3 . . ? C522 C521 H52A 110.3 . . ? O52 C521 H52B 110.3 . . ? C522 C521 H52B 110.3 . . ? H52A C521 H52B 108.5 . . ? C521 C522 H52C 109.5 . . ? C521 C522 H52D 109.5 . . ? H52C C522 H52D 109.5 . . ? C521 C522 H52E 109.5 . . ? H52C C522 H52E 109.5 . . ? H52D C522 H52E 109.5 . . ? C531 O53 P5 114.6(7) . . ? O53 C531 C532 106.0(5) . . ? O53 C531 H53B 110.5 . . ? C532 C531 H53B 110.5 . . ? O53 C531 H53C 110.5 . . ? C532 C531 H53C 110.5 . . ? H53B C531 H53C 108.7 . . ? C66 C5 C52 114.2(5) . . ? C66 C5 H5A 108.7 . . ? C52 C5 H5A 108.7 . . ? C66 C5 H5B 108.7 . . ? C52 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? C67 O6 C61 120.4(5) . . ? C62 C61 C66 122.8(5) . . ? C62 C61 O6 117.2(5) . . ? C66 C61 O6 119.6(5) . . ? C63 C62 C61 118.1(5) . . ? C63 C62 C6 121.0(5) . . ? C61 C62 C6 120.9(5) . . ? C62 C63 C64 121.2(6) . . ? C62 C63 H63A 119.4 . . ? C64 C63 H63A 119.4 . . ? C65 C64 C63 119.2(6) . . ? C65 C64 P6 119.7(5) . . ? C63 C64 P6 121.1(5) . . ? C64 C65 C66 121.3(5) . . ? C64 C65 H65A 119.3 . . ? C66 C65 H65A 119.3 . . ? C65 C66 C61 117.3(5) . . ? C65 C66 C5 120.4(5) . . ? C61 C66 C5 122.3(5) . . ? O67 C67 O6 123.5(6) . . ? O67 C67 C68 126.9(7) . . ? O6 C67 C68 109.5(6) . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? O61' P6 O61 130.9(7) . . ? O61' P6 O63' 120.0(4) . . ? O61 P6 O63' 24.0(4) . . ? O61' P6 O62 60.6(5) . . ? O61 P6 O62 115.6(4) . . ? O63' P6 O62 133.6(5) . . ? O61' P6 O63 41.6(4) . . ? O61 P6 O63 114.2(4) . . ? O63' P6 O63 92.2(5) . . ? O62 P6 O63 102.2(5) . . ? O61' P6 O62' 112.8(4) . . ? O61 P6 O62' 73.1(5) . . ? O63' P6 O62' 97.1(5) . . ? O62 P6 O62' 53.7(5) . . ? O63 P6 O62' 152.7(5) . . ? O61' P6 C64 114.7(5) . . ? O61 P6 C64 111.6(5) . . ? O63' P6 C64 109.1(4) . . ? O62 P6 C64 110.8(5) . . ? O63 P6 C64 101.1(4) . . ? O62' P6 C64 99.9(5) . . ? C621 O62 P6 114.1(6) . . ? O62 C621 C622 108.2(5) . . ? O62 C621 H62A 110.1 . . ? C622 C621 H62A 110.1 . . ? O62 C621 H62B 110.1 . . ? C622 C621 H62B 110.1 . . ? H62A C621 H62B 108.4 . . ? C631 O63 P6 125.5(9) . . ? O63 C631 C632 107.9(5) . . ? O63 C631 H63B 110.1 . . ? C632 C631 H63B 110.1 . . ? O63 C631 H63C 110.1 . . ? C632 C631 H63C 110.1 . . ? H63B C631 H63C 108.4 . . ? C62' O62' P6 123.1(12) . . ? O62' C62' C62" 107.9(5) . . ? O62' C62' H62C 110.1 . . ? C62" C62' H62C 110.1 . . ? O62' C62' H62D 110.1 . . ? C62" C62' H62D 110.1 . . ? H62C C62' H62D 108.4 . . ? C63' O63' P6 120.6(6) . . ? O63' C63' C63" 107.8(5) . . ? O63' C63' H63D 110.1 . . ? C63" C63' H63D 110.1 . . ? O63' C63' H63E 110.1 . . ? C63" C63' H63E 110.1 . . ? H63D C63' H63E 108.5 . . ? C62 C6 C16 114.2(5) . . ? C62 C6 H6A 108.7 . . ? C16 C6 H6A 108.7 . . ? C62 C6 H6B 108.7 . . ? C16 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? C6A C1A C2A 120.0 . . ? C6A C1A C7A 121.4(11) . . ? C2A C1A C7A 118.6(12) . . ? C3A C2A C1A 120.0 . . ? C3A C2A H2AA 120.0 . . ? C1A C2A H2AA 120.0 . . ? C2A C3A C4A 120.0 . . ? C2A C3A H3AA 120.0 . . ? C4A C3A H3AA 120.0 . . ? C5A C4A C3A 120.0 . . ? C5A C4A H4AA 120.0 . . ? C3A C4A H4AA 120.0 . . ? C6A C5A C4A 120.0 . . ? C6A C5A H5AA 120.0 . . ? C4A C5A H5AA 120.0 . . ? C5A C6A C1A 120.0 . . ? C5A C6A H6AA 120.0 . . ? C1A C6A H6AA 120.0 . . ? H1W O1W H2W 121.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C17 O1 C11 C16 95.1(6) . . . . ? C17 O1 C11 C12 -88.3(6) . . . . ? C16 C11 C12 C13 0.5(8) . . . . ? O1 C11 C12 C13 -175.9(4) . . . . ? C16 C11 C12 C1 -178.1(5) . . . . ? O1 C11 C12 C1 5.6(7) . . . . ? C11 C12 C13 C14 -0.7(8) . . . . ? C1 C12 C13 C14 177.9(5) . . . . ? C12 C13 C14 C15 0.4(9) . . . . ? C12 C13 C14 P1 179.2(4) . . . . ? C13 C14 C15 C16 0.3(10) . . . . ? P1 C14 C15 C16 -178.5(5) . . . . ? C12 C11 C16 C15 0.1(8) . . . . ? O1 C11 C16 C15 176.5(5) . . . . ? C12 C11 C16 C6 179.8(5) . . . . ? O1 C11 C16 C6 -3.8(7) . . . . ? C14 C15 C16 C11 -0.5(9) . . . . ? C14 C15 C16 C6 179.8(6) . . . . ? C11 O1 C17 O17 -1.6(8) . . . . ? C11 O1 C17 C18 177.5(5) . . . . ? C15 C14 P1 O11 131.3(7) . . . . ? C13 C14 P1 O11 -47.5(7) . . . . ? C15 C14 P1 O11' -16.6(8) . . . . ? C13 C14 P1 O11' 164.5(7) . . . . ? C15 C14 P1 O12' -154.4(6) . . . . ? C13 C14 P1 O12' 26.8(7) . . . . ? C15 C14 P1 O13 -1.6(8) . . . . ? C13 C14 P1 O13 179.5(7) . . . . ? C15 C14 P1 O12 -97.4(6) . . . . ? C13 C14 P1 O12 83.7(6) . . . . ? C15 C14 P1 O13' 112.8(8) . . . . ? C13 C14 P1 O13' -66.0(7) . . . . ? O11 P1 O12 C121 44.7(17) . . . . ? O11' P1 O12 C121 156.0(16) . . . . ? O12' P1 O12 C121 15.7(15) . . . . ? O13 P1 O12 C121 168.1(15) . . . . ? O13' P1 O12 C121 40.4(19) . . . . ? C14 P1 O12 C121 -87.4(15) . . . . ? P1 O12 C121 C122 -172.3(17) . . . . ? O11 P1 O13 C131 -43(2) . . . . ? O11' P1 O13 C131 -130(3) . . . . ? O12' P1 O13 C131 -130.6(17) . . . . ? O12 P1 O13 C131 -165.9(18) . . . . ? O13' P1 O13 C131 -18(2) . . . . ? C14 P1 O13 C131 90.7(18) . . . . ? P1 O13 C131 C132 -168.9(17) . . . . ? O11 P1 O12' C12' -176.5(13) . . . . ? O11' P1 O12' C12' -69.0(14) . . . . ? O13 P1 O12' C12' -68.8(15) . . . . ? O12 P1 O12' C12' -24.1(12) . . . . ? O13' P1 O12' C12' 171.0(12) . . . . ? C14 P1 O12' C12' 68.8(12) . . . . ? P1 O12' C12' C12" 132.8(15) . . . . ? O11 P1 O13' C13' 112(3) . . . . ? O11' P1 O13' C13' 20(2) . . . . ? O12' P1 O13' C13' 141(2) . . . . ? O13 P1 O13' C13' -1(2) . . . . ? O12 P1 O13' C13' 121.2(19) . . . . ? C14 P1 O13' C13' -110.9(19) . . . . ? P1 O13' C13' C13" -177.2(17) . . . . ? C13 C12 C1 C26 137.4(5) . . . . ? C11 C12 C1 C26 -44.1(7) . . . . ? C27 O2 C21 C22 108.3(6) . . . . ? C27 O2 C21 C26 -77.7(7) . . . . ? C26 C21 C22 C23 -0.5(8) . . . . ? O2 C21 C22 C23 173.3(5) . . . . ? C26 C21 C22 C2 -178.4(5) . . . . ? O2 C21 C22 C2 -4.6(7) . . . . ? C21 C22 C23 C24 0.1(8) . . . . ? C2 C22 C23 C24 178.0(5) . . . . ? C22 C23 C24 C25 0.7(8) . . . . ? C22 C23 C24 P2 -175.2(4) . . . . ? C23 C24 C25 C26 -1.2(8) . . . . ? P2 C24 C25 C26 175.0(4) . . . . ? C24 C25 C26 C21 0.7(8) . . . . ? C24 C25 C26 C1 -178.9(5) . . . . ? C22 C21 C26 C25 0.1(8) . . . . ? O2 C21 C26 C25 -173.6(5) . . . . ? C22 C21 C26 C1 179.7(5) . . . . ? O2 C21 C26 C1 6.0(8) . . . . ? C12 C1 C26 C25 131.4(5) . . . . ? C12 C1 C26 C21 -48.2(7) . . . . ? C21 O2 C27 O27 0.4(10) . . . . ? C21 O2 C27 C28 -179.8(5) . . . . ? C25 C24 P2 O21 -34.1(5) . . . . ? C23 C24 P2 O21 141.9(4) . . . . ? C25 C24 P2 O22 91.7(5) . . . . ? C23 C24 P2 O22 -92.3(5) . . . . ? C25 C24 P2 O23 -160.1(4) . . . . ? C23 C24 P2 O23 16.0(5) . . . . ? O21 P2 O22 C221 -25.2(8) . . . . ? O23 P2 O22 C221 101.0(7) . . . . ? C24 P2 O22 C221 -148.6(7) . . . . ? P2 O22 C221 C222 156.0(7) . . . . ? O21 P2 O23 C231 -47.5(7) . . . . ? O22 P2 O23 C231 -174.4(6) . . . . ? C24 P2 O23 C231 76.8(7) . . . . ? P2 O23 C231 C232 174.7(8) . . . . ? C23 C22 C2 C36 -92.2(6) . . . . ? C21 C22 C2 C36 85.6(7) . . . . ? C37 O3 C31 C32 -102.4(6) . . . . ? C37 O3 C31 C36 83.4(6) . . . . ? C36 C31 C32 C33 0.5(8) . . . . ? O3 C31 C32 C33 -173.4(5) . . . . ? C36 C31 C32 C3 178.0(5) . . . . ? O3 C31 C32 C3 4.1(7) . . . . ? C31 C32 C33 C34 -1.0(7) . . . . ? C3 C32 C33 C34 -178.5(5) . . . . ? C32 C33 C34 C35 0.1(8) . . . . ? C32 C33 C34 P3 177.9(4) . . . . ? C33 C34 C35 C36 1.5(8) . . . . ? P3 C34 C35 C36 -176.4(4) . . . . ? C34 C35 C36 C31 -1.9(7) . . . . ? C34 C35 C36 C2 175.4(5) . . . . ? C32 C31 C36 C35 1.0(8) . . . . ? O3 C31 C36 C35 174.9(5) . . . . ? C32 C31 C36 C2 -176.5(5) . . . . ? O3 C31 C36 C2 -2.6(7) . . . . ? C22 C2 C36 C35 7.3(8) . . . . ? C22 C2 C36 C31 -175.4(5) . . . . ? C31 O3 C37 O37 2.8(9) . . . . ? C31 O3 C37 C38 -176.4(5) . . . . ? C35 C34 P3 O31 -31.1(5) . . . . ? C33 C34 P3 O31 151.1(4) . . . . ? C35 C34 P3 O32 95.8(5) . . . . ? C33 C34 P3 O32 -82.1(5) . . . . ? C35 C34 P3 O33 -157.0(4) . . . . ? C33 C34 P3 O33 25.2(5) . . . . ? O31 P3 O32 C321 -51.4(6) . . . . ? O33 P3 O32 C321 72.8(6) . . . . ? C34 P3 O32 C321 -176.5(6) . . . . ? P3 O32 C321 C322 106.5(9) . . . . ? O31 P3 O33 C331 -45.7(5) . . . . ? O32 P3 O33 C331 -172.0(4) . . . . ? C34 P3 O33 C331 80.4(5) . . . . ? P3 O33 C331 C332 91.1(9) . . . . ? C31 C32 C3 C46 93.0(6) . . . . ? C33 C32 C3 C46 -89.6(6) . . . . ? C47 O4 C41 C42 -92.6(6) . . . . ? C47 O4 C41 C46 88.4(6) . . . . ? C46 C41 C42 C43 1.6(8) . . . . ? O4 C41 C42 C43 -177.4(5) . . . . ? C46 C41 C42 C4 -174.7(5) . . . . ? O4 C41 C42 C4 6.4(8) . . . . ? C41 C42 C43 C44 -0.8(9) . . . . ? C4 C42 C43 C44 175.5(6) . . . . ? C42 C43 C44 C45 -0.3(10) . . . . ? C42 C43 C44 P4 -179.2(5) . . . . ? C43 C44 C45 C46 0.8(9) . . . . ? P4 C44 C45 C46 179.7(4) . . . . ? C44 C45 C46 C41 -0.1(8) . . . . ? C44 C45 C46 C3 -177.6(5) . . . . ? C42 C41 C46 C45 -1.1(8) . . . . ? O4 C41 C46 C45 177.9(5) . . . . ? C42 C41 C46 C3 176.3(5) . . . . ? O4 C41 C46 C3 -4.7(7) . . . . ? C32 C3 C46 C45 -102.7(6) . . . . ? C32 C3 C46 C41 79.9(6) . . . . ? C41 O4 C47 O47 -0.3(9) . . . . ? C41 O4 C47 C48 -179.9(5) . . . . ? C43 C44 P4 O41' 150.0(6) . . . . ? C45 C44 P4 O41' -28.8(7) . . . . ? C43 C44 P4 O41 166.3(6) . . . . ? C45 C44 P4 O41 -12.6(7) . . . . ? C43 C44 P4 O43' 12.6(7) . . . . ? C45 C44 P4 O43' -166.3(5) . . . . ? C43 C44 P4 O42' -80.3(7) . . . . ? C45 C44 P4 O42' 100.9(7) . . . . ? C43 C44 P4 O42 -62.0(7) . . . . ? C45 C44 P4 O42 119.1(6) . . . . ? C43 C44 P4 O43 40.9(7) . . . . ? C45 C44 P4 O43 -137.9(6) . . . . ? O41' P4 O42 C421 48.0(16) . . . . ? O41 P4 O42 C421 43.4(14) . . . . ? O43' P4 O42 C421 158.4(13) . . . . ? O42' P4 O42 C421 3(3) . . . . ? O43 P4 O42 C421 169.7(11) . . . . ? C44 P4 O42 C421 -88.5(11) . . . . ? P4 O42 C421 C422 -147.1(14) . . . . ? O41' P4 O43 C431 87.5(12) . . . . ? O41 P4 O43 C431 73.8(13) . . . . ? O43' P4 O43 C431 -32.5(11) . . . . ? O42' P4 O43 C431 -48.0(14) . . . . ? O42 P4 O43 C431 -52.4(13) . . . . ? C44 P4 O43 C431 -160.5(12) . . . . ? P4 O43 C431 C432 171.3(12) . . . . ? O41' P4 O42' C42' 6(2) . . . . ? O41 P4 O42' C42' 6(2) . . . . ? O43' P4 O42' C42' 126(2) . . . . ? O42 P4 O42' C42' 149(5) . . . . ? O43 P4 O42' C42' 134.7(18) . . . . ? C44 P4 O42' C42' -117.0(19) . . . . ? P4 O42' C42' C42" -180.0(16) . . . . ? O41' P4 O43' C43' -35.2(10) . . . . ? O41 P4 O43' C43' -54.7(10) . . . . ? O42' P4 O43' C43' -156.8(9) . . . . ? O42 P4 O43' C43' -164.0(10) . . . . ? O43 P4 O43' C43' 37.1(8) . . . . ? C44 P4 O43' C43' 97.9(8) . . . . ? P4 O43' C43' C43" -114.7(13) . . . . ? C41 C42 C4 C56 -61.7(8) . . . . ? C43 C42 C4 C56 122.2(6) . . . . ? C57 O5 C51 C56 -90.2(7) . . . . ? C57 O5 C51 C52 93.5(6) . . . . ? C56 C51 C52 C53 -4.2(8) . . . . ? O5 C51 C52 C53 171.9(5) . . . . ? C56 C51 C52 C5 171.3(5) . . . . ? O5 C51 C52 C5 -12.6(8) . . . . ? C51 C52 C53 C54 0.4(9) . . . . ? C5 C52 C53 C54 -175.1(6) . . . . ? C52 C53 C54 C55 3.6(10) . . . . ? C52 C53 C54 P5 -177.0(5) . . . . ? C53 C54 C55 C56 -4.1(11) . . . . ? P5 C54 C55 C56 176.5(5) . . . . ? C54 C55 C56 C51 0.6(10) . . . . ? C54 C55 C56 C4 176.4(6) . . . . ? C52 C51 C56 C55 3.7(9) . . . . ? O5 C51 C56 C55 -172.4(5) . . . . ? C52 C51 C56 C4 -172.0(5) . . . . ? O5 C51 C56 C4 11.9(8) . . . . ? C42 C4 C56 C55 131.1(6) . . . . ? C42 C4 C56 C51 -53.4(8) . . . . ? C51 O5 C57 O57 5.3(9) . . . . ? C51 O5 C57 C58 -173.6(6) . . . . ? C53 C54 P5 O51 5.2(8) . . . . ? C55 C54 P5 O51 -175.4(6) . . . . ? C53 C54 P5 O53 -128.7(8) . . . . ? C55 C54 P5 O53 50.7(8) . . . . ? C53 C54 P5 O52 131.8(7) . . . . ? C55 C54 P5 O52 -48.8(8) . . . . ? O51 P5 O52 C521 -22.0(11) . . . . ? O53 P5 O52 C521 103.4(11) . . . . ? C54 P5 O52 C521 -146.3(9) . . . . ? P5 O52 C521 C522 -76.8(18) . . . . ? O51 P5 O53 C531 -56.9(16) . . . . ? O52 P5 O53 C531 -179.4(13) . . . . ? C54 P5 O53 C531 73.1(14) . . . . ? P5 O53 C531 C532 40(3) . . . . ? C53 C52 C5 C66 -50.6(7) . . . . ? C51 C52 C5 C66 134.0(5) . . . . ? C67 O6 C61 C62 109.1(7) . . . . ? C67 O6 C61 C66 -77.7(7) . . . . ? C66 C61 C62 C63 -2.2(10) . . . . ? O6 C61 C62 C63 170.7(6) . . . . ? C66 C61 C62 C6 175.5(6) . . . . ? O6 C61 C62 C6 -11.6(9) . . . . ? C61 C62 C63 C64 -0.1(11) . . . . ? C6 C62 C63 C64 -177.8(7) . . . . ? C62 C63 C64 C65 2.5(11) . . . . ? C62 C63 C64 P6 -175.3(6) . . . . ? C63 C64 C65 C66 -2.7(11) . . . . ? P6 C64 C65 C66 175.1(5) . . . . ? C64 C65 C66 C61 0.6(10) . . . . ? C64 C65 C66 C5 -179.6(6) . . . . ? C62 C61 C66 C65 2.0(10) . . . . ? O6 C61 C66 C65 -170.8(6) . . . . ? C62 C61 C66 C5 -177.9(6) . . . . ? O6 C61 C66 C5 9.4(9) . . . . ? C52 C5 C66 C65 105.6(7) . . . . ? C52 C5 C66 C61 -74.5(8) . . . . ? C61 O6 C67 O67 3.3(9) . . . . ? C61 O6 C67 C68 -177.0(5) . . . . ? C65 C64 P6 O61' 20.6(8) . . . . ? C63 C64 P6 O61' -161.6(6) . . . . ? C65 C64 P6 O61 -176.0(6) . . . . ? C63 C64 P6 O61 1.8(8) . . . . ? C65 C64 P6 O63' 158.5(6) . . . . ? C63 C64 P6 O63' -23.7(8) . . . . ? C65 C64 P6 O62 -45.7(7) . . . . ? C63 C64 P6 O62 132.2(7) . . . . ? C65 C64 P6 O63 62.2(7) . . . . ? C63 C64 P6 O63 -120.0(7) . . . . ? C65 C64 P6 O62' -100.4(7) . . . . ? C63 C64 P6 O62' 77.4(7) . . . . ? O61' P6 O62 C621 173.2(16) . . . . ? O61 P6 O62 C621 48.9(16) . . . . ? O63' P6 O62 C621 68.4(16) . . . . ? O63 P6 O62 C621 173.6(14) . . . . ? O62' P6 O62 C621 7.8(14) . . . . ? C64 P6 O62 C621 -79.3(15) . . . . ? P6 O62 C621 C622 179.0(16) . . . . ? O61' P6 O63 C631 -76.2(17) . . . . ? O61 P6 O63 C631 49.0(17) . . . . ? O63' P6 O63 C631 59.0(16) . . . . ? O62 P6 O63 C631 -76.6(16) . . . . ? O62' P6 O63 C631 -51(2) . . . . ? C64 P6 O63 C631 168.9(15) . . . . ? P6 O63 C631 C632 -165.0(15) . . . . ? O61' P6 O62' C62' -54.0(13) . . . . ? O61 P6 O62' C62' 178.0(12) . . . . ? O63' P6 O62' C62' 179.1(11) . . . . ? O62 P6 O62' C62' -40.3(11) . . . . ? O63 P6 O62' C62' -71.8(17) . . . . ? C64 P6 O62' C62' 68.3(11) . . . . ? P6 O62' C62' C62" 116.7(18) . . . . ? O61' P6 O63' C63' -39.5(17) . . . . ? O61 P6 O63' C63' 85(2) . . . . ? O62 P6 O63' C63' 37.0(18) . . . . ? O63 P6 O63' C63' -72.3(16) . . . . ? O62' P6 O63' C63' 82.0(16) . . . . ? C64 P6 O63' C63' -174.9(15) . . . . ? P6 O63' C63' C63" -179.5(15) . . . . ? C63 C62 C6 C16 101.6(7) . . . . ? C61 C62 C6 C16 -76.0(8) . . . . ? C11 C16 C6 C62 169.9(5) . . . . ? C15 C16 C6 C62 -10.4(8) . . . . ? C6A C1A C2A C3A 0.0 . . . . ? C7A C1A C2A C3A 178.3(14) . . . . ? C1A C2A C3A C4A 0.0 . . . . ? C2A C3A C4A C5A 0.0 . . . . ? C3A C4A C5A C6A 0.0 . . . . ? C4A C5A C6A C1A 0.0 . . . . ? C2A C1A C6A C5A 0.0 . . . . ? C7A C1A C6A C5A -178.3(15) . . . . ? 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 O1W H1W O21 0.85 1.98 2.830(6) 179.4 . O1W H2W O41 0.85 1.91 2.756(7) 179.4 1_455 _diffrn_measured_fraction_theta_max 0.880 _diffrn_reflns_theta_full 28.54 _diffrn_measured_fraction_theta_full 0.880 _refine_diff_density_max 1.830 _refine_diff_density_min -1.330 _refine_diff_density_rms 0.115 # Attachment '4d.cif' data_tca013 _database_code_depnum_ccdc_archive 'CCDC 669059' # start Validation Reply Form _vrf_PLAT220_tca013 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 7.88 Ratio RESPONSE: The refinement of chemically sensible disordered groups was employed only for "well-behaved" disorder. Some minor disorder, which was not accounted, can lead to some uncertainty in values of ADP. ; _vrf_PLAT222_tca013 ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 9.35 Ratio RESPONSE: Termal parameters of H-atoms was constrained to the bonded atoms. ; _vrf_PLAT241_tca013 ; PROBLEM: Check High Ueq as Compared to Neighbors for O41 RESPONSE: Some minor disorder, which was not accounted, can lead to some uncertainty in values of ADP. ; _vrf_PLAT242_tca013 ; PROBLEM: Check Low Ueq as Compared to Neighbors for C322 RESPONSE: Some minor disorder, which was not accounted, can lead to some uncertainty in values of ADP. ; _vrf_PLAT761_tca013 ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: Positions of hydrogen atoms and their atomic displacement parameters were constrained to the bonded atoms during the refinement, using literature data. ; _vrf_PLAT762_tca013 ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: same, as above. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C104 H136 O40 P8' _chemical_formula_sum 'C104 H136 O40 P8' _chemical_formula_weight 2273.89 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' 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 14.055(2) _cell_length_b 14.498(2) _cell_length_c 15.077(2) _cell_angle_alpha 75.011(3) _cell_angle_beta 88.677(3) _cell_angle_gamma 74.754(3) _cell_volume 2859.9(7) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 936 _cell_measurement_theta_min 2.98 _cell_measurement_theta_max 26.90 _exptl_crystal_description colourless _exptl_crystal_colour plate _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 0.205 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9045 _exptl_absorpt_correction_T_max 0.9602 _exptl_absorpt_process_details 'SADABS - Bruker area detector absorption corrections' _exptl_special_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). ; _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 20387 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.15 _reflns_number_total 12270 _reflns_number_gt 8474 _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. Some of the P(O)(OEt)2 groups is extremely disordered with high values of ADP's, which introduce large distortion in geometrical characteristics of the disordered group. Large number of geometrical constrains was used to keep chemically reasonable interatomic distances. ; _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^)+(0.1704P)^2^+4.6579P] 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 12270 _refine_ls_number_parameters 669 _refine_ls_number_restraints 370 _refine_ls_R_factor_all 0.1308 _refine_ls_R_factor_gt 0.0985 _refine_ls_wR_factor_ref 0.3068 _refine_ls_wR_factor_gt 0.2717 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.221 _refine_ls_shift/su_max 0.004 _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 0.5966(2) -0.0254(2) -0.1915(2) 0.0373(7) Uani 1 1 d . . . C11 C 0.6274(3) 0.0550(3) -0.2470(3) 0.0332(9) Uani 1 1 d . . . C12 C 0.6904(3) 0.0939(3) -0.2070(3) 0.0339(9) Uani 1 1 d . . . C13 C 0.7303(3) 0.1645(4) -0.2647(3) 0.0385(10) Uani 1 1 d . . . H13 H 0.7755 0.1907 -0.2397 0.046 Uiso 1 1 calc R . . C14 C 0.7050(4) 0.1973(4) -0.3585(3) 0.0388(10) Uani 1 1 d . A . C15 C 0.6386(4) 0.1597(4) -0.3954(3) 0.0403(10) Uani 1 1 d . . . H15 H 0.6199 0.1837 -0.4590 0.048 Uiso 1 1 calc R . . C16 C 0.5991(3) 0.0875(3) -0.3405(3) 0.0348(9) Uani 1 1 d . . . O17 O 0.4524(3) 0.0742(3) -0.1696(3) 0.0664(12) Uani 1 1 d . . . C17 C 0.5073(4) -0.0059(4) -0.1528(3) 0.0438(11) Uani 1 1 d . . . C18 C 0.4928(5) -0.0967(4) -0.0867(4) 0.0560(14) Uani 1 1 d . . . H18A H 0.4285 -0.0808 -0.0595 0.084 Uiso 1 1 calc R . . H18B H 0.5452 -0.1213 -0.0380 0.084 Uiso 1 1 calc R . . H18C H 0.4952 -0.1477 -0.1191 0.084 Uiso 1 1 calc R . . P1 P 0.76190(12) 0.28175(13) -0.43595(11) 0.0567(4) Uani 1 1 d D . . O11 O 0.6951(7) 0.3391(8) -0.5183(6) 0.072(3) Uiso 0.50 1 d PD A 1 O12 O 0.8076(7) 0.3366(7) -0.3820(7) 0.048(3) Uiso 0.50 1 d PD A 1 C121 C 0.7566(13) 0.4345(10) -0.3804(10) 0.098(5) Uiso 0.50 1 d PD A 1 H12A H 0.6852 0.4401 -0.3868 0.118 Uiso 0.50 1 calc PR A 1 H12B H 0.7732 0.4794 -0.4365 0.118 Uiso 0.50 1 calc PR A 1 C122 C 0.7697(11) 0.4737(9) -0.3052(10) 0.075(4) Uiso 0.50 1 d PD A 1 H12E H 0.7246 0.5401 -0.3146 0.113 Uiso 0.50 1 calc PR A 1 H12F H 0.8380 0.4776 -0.3016 0.113 Uiso 0.50 1 calc PR A 1 H12G H 0.7554 0.4303 -0.2479 0.113 Uiso 0.50 1 calc PR A 1 O13 O 0.8573(5) 0.2070(5) -0.4607(6) 0.059(2) Uiso 0.50 1 d PD A 1 C131 C 0.8570(8) 0.1266(7) -0.5003(7) 0.044(2) Uiso 0.50 1 d PD A 1 H13A H 0.7884 0.1344 -0.5213 0.053 Uiso 0.50 1 calc PR A 1 H13B H 0.8772 0.0638 -0.4514 0.053 Uiso 0.50 1 calc PR A 1 C132 C 0.9201(10) 0.1184(9) -0.5765(8) 0.045(3) Uiso 0.50 1 d PD A 1 H13E H 0.9744 0.0579 -0.5581 0.068 Uiso 0.50 1 calc PR A 1 H13F H 0.9470 0.1761 -0.5943 0.068 Uiso 0.50 1 calc PR A 1 H13G H 0.8817 0.1156 -0.6287 0.068 Uiso 0.50 1 calc PR A 1 O11' O 0.8285(8) 0.3192(9) -0.3836(8) 0.061(4) Uiso 0.50 1 d PD A -2 O12' O 0.8079(6) 0.2409(6) -0.5152(5) 0.0540(18) Uiso 0.50 1 d PD A -2 C12' C 0.8875(12) 0.1527(12) -0.4940(12) 0.094(5) Uiso 0.50 1 d PD A -2 H12C H 0.8627 0.0981 -0.4558 0.113 Uiso 0.50 1 calc PR A -2 H12D H 0.9388 0.1628 -0.4565 0.113 Uiso 0.50 1 calc PR A -2 C12" C 0.933(2) 0.122(2) -0.5726(19) 0.146(15) Uiso 0.50 1 d PD A -2 H12H H 0.9108 0.0660 -0.5808 0.219 Uiso 0.50 1 calc PR A -2 H12I H 1.0053 0.1014 -0.5620 0.219 Uiso 0.50 1 calc PR A -2 H12J H 0.9151 0.1772 -0.6279 0.219 Uiso 0.50 1 calc PR A -2 O13' O 0.6766(6) 0.3676(6) -0.4966(7) 0.067(3) Uiso 0.50 1 d PD A -2 C13' C 0.6034(11) 0.4414(13) -0.4686(13) 0.101(5) Uiso 0.50 1 d PD A -2 H13C H 0.6257 0.5027 -0.4818 0.121 Uiso 0.50 1 calc PR A -2 H13D H 0.5987 0.4191 -0.4011 0.121 Uiso 0.50 1 calc PR A -2 C13" C 0.5051(10) 0.465(2) -0.512(2) 0.164(11) Uiso 0.50 1 d PD A -2 H13H H 0.4608 0.5186 -0.4898 0.246 Uiso 0.50 1 calc PR A -2 H13I H 0.4799 0.4064 -0.4953 0.246 Uiso 0.50 1 calc PR A -2 H13J H 0.5085 0.4869 -0.5785 0.246 Uiso 0.50 1 calc PR A -2 C1 C 0.7157(4) 0.0564(3) -0.1039(3) 0.0376(10) Uani 1 1 d . . . H1A H 0.6589 0.0353 -0.0734 0.045 Uiso 1 1 calc R . . H1B H 0.7725 -0.0032 -0.0932 0.045 Uiso 1 1 calc R . . O2 O 0.5830(2) 0.2406(2) -0.1053(2) 0.0361(7) Uani 1 1 d . . . C21 C 0.6746(3) 0.2189(3) -0.0580(3) 0.0328(9) Uani 1 1 d . . . C22 C 0.6919(3) 0.2827(3) -0.0097(3) 0.0315(9) Uani 1 1 d . . . C23 C 0.7817(3) 0.2529(3) 0.0417(3) 0.0346(9) Uani 1 1 d . . . H23 H 0.7960 0.2948 0.0758 0.042 Uiso 1 1 calc R . . C24 C 0.8504(3) 0.1633(3) 0.0438(3) 0.0353(9) Uani 1 1 d . . . C25 C 0.8290(3) 0.1016(3) -0.0061(3) 0.0361(10) Uani 1 1 d . . . H25 H 0.8756 0.0404 -0.0047 0.043 Uiso 1 1 calc R . . C26 C 0.7408(3) 0.1284(3) -0.0576(3) 0.0337(9) Uani 1 1 d . . . O27 O 0.6226(3) 0.3603(3) -0.2175(2) 0.0504(9) Uani 1 1 d . . . C27 C 0.5672(4) 0.3109(4) -0.1899(3) 0.0427(11) Uani 1 1 d . . . C28 C 0.4755(4) 0.3125(4) -0.2367(4) 0.0577(15) Uani 1 1 d . . . H28A H 0.4651 0.3623 -0.2961 0.087 Uiso 1 1 calc R . . H28B H 0.4195 0.3290 -0.1984 0.087 Uiso 1 1 calc R . . H28C H 0.4810 0.2471 -0.2467 0.087 Uiso 1 1 calc R . . P2 P 0.96207(10) 0.11925(11) 0.11292(10) 0.0493(4) Uani 1 1 d D . . O21 O 1.0518(3) 0.0980(4) 0.0627(3) 0.0776(15) Uani 1 1 d D . . O22 O 0.9588(3) 0.1931(3) 0.1717(3) 0.0667(12) Uani 1 1 d D . . C221 C 1.0359(5) 0.2417(5) 0.1728(6) 0.083(2) Uani 1 1 d D . . H22A H 1.0082 0.3035 0.1919 0.100 Uiso 1 1 calc R . . H22B H 1.0585 0.2604 0.1096 0.100 Uiso 1 1 calc R . . C222 C 1.1211(5) 0.1812(8) 0.2341(6) 0.101(3) Uani 1 1 d D . . H22C H 1.1700 0.2189 0.2319 0.152 Uiso 1 1 calc R . . H22D H 1.1505 0.1209 0.2146 0.152 Uiso 1 1 calc R . . H22E H 1.0997 0.1632 0.2972 0.152 Uiso 1 1 calc R . . O23 O 0.9372(4) 0.0290(4) 0.1847(4) 0.0882(16) Uani 1 1 d D . . C231 C 1.0057(6) -0.0554(5) 0.2410(6) 0.090(2) Uani 1 1 d D . . H23A H 0.9993 -0.0527 0.3058 0.108 Uiso 1 1 calc R . . H23B H 1.0735 -0.0524 0.2239 0.108 Uiso 1 1 calc R . . C232 C 0.9925(7) -0.1497(5) 0.2337(8) 0.108(3) Uani 1 1 d D . . H23C H 1.0415 -0.2042 0.2746 0.162 Uiso 1 1 calc R . . H23D H 1.0012 -0.1542 0.1701 0.162 Uiso 1 1 calc R . . H23E H 0.9260 -0.1539 0.2514 0.162 Uiso 1 1 calc R . . C2 C 0.6180(3) 0.3791(3) -0.0089(3) 0.0335(9) Uani 1 1 d . . . H2A H 0.5943 0.4154 -0.0729 0.040 Uiso 1 1 calc R . . H2B H 0.6518 0.4201 0.0154 0.040 Uiso 1 1 calc R . . O3 O 0.6310(2) 0.3269(2) 0.1844(2) 0.0356(7) Uani 1 1 d . . . C31 C 0.5370(3) 0.3457(3) 0.1438(3) 0.0322(9) Uani 1 1 d . . . C32 C 0.4567(3) 0.3391(3) 0.1987(3) 0.0354(10) Uani 1 1 d . . . C33 C 0.3659(4) 0.3535(3) 0.1552(3) 0.0391(10) Uani 1 1 d . . . H33 H 0.3103 0.3481 0.1912 0.047 Uiso 1 1 calc R . . C34 C 0.3550(3) 0.3756(3) 0.0598(3) 0.0391(10) Uani 1 1 d . . . C35 C 0.4371(3) 0.3822(3) 0.0071(3) 0.0355(9) Uani 1 1 d . . . H35 H 0.4297 0.3973 -0.0579 0.043 Uiso 1 1 calc R . . C36 C 0.5294(3) 0.3672(3) 0.0480(3) 0.0316(9) Uani 1 1 d . . . O37 O 0.5882(3) 0.4748(3) 0.2155(3) 0.0529(9) Uani 1 1 d . . . C37 C 0.6493(4) 0.3988(4) 0.2202(3) 0.0399(10) Uani 1 1 d . . . C38 C 0.7501(4) 0.3671(5) 0.2641(4) 0.0535(13) Uani 1 1 d . . . H38A H 0.7613 0.4199 0.2887 0.080 Uiso 1 1 calc R . . H38B H 0.7988 0.3536 0.2183 0.080 Uiso 1 1 calc R . . H38C H 0.7568 0.3069 0.3142 0.080 Uiso 1 1 calc R . . P3 P 0.23738(12) 0.40026(16) 0.00333(12) 0.0692(5) Uani 1 1 d D B . O31 O 0.2263(4) 0.4753(7) -0.0826(4) 0.150(4) Uani 1 1 d . . . O32 O 0.2216(6) 0.2979(5) 0.0045(6) 0.146(3) Uani 1 1 d D . . C321 C 0.2699(11) 0.2171(12) -0.0310(13) 0.103(6) Uiso 0.50 1 d PD B 1 H32A H 0.2969 0.1589 0.0214 0.123 Uiso 0.50 1 calc PR B 1 H32B H 0.3266 0.2337 -0.0655 0.123 Uiso 0.50 1 calc PR B 1 C322 C 0.2096(16) 0.1889(14) -0.0909(13) 0.086(5) Uiso 0.50 1 d PD B 1 H32E H 0.2498 0.1328 -0.1117 0.128 Uiso 0.50 1 calc PR B 1 H32F H 0.1839 0.2450 -0.1443 0.128 Uiso 0.50 1 calc PR B 1 H32G H 0.1544 0.1697 -0.0572 0.128 Uiso 0.50 1 calc PR B 1 C32' C 0.1795(15) 0.256(2) -0.055(2) 0.173(12) Uiso 0.50 1 d PD B 2 H32C H 0.1456 0.3097 -0.1080 0.208 Uiso 0.50 1 calc PR B 2 H32D H 0.1284 0.2265 -0.0215 0.208 Uiso 0.50 1 calc PR B 2 C32" C 0.246(2) 0.180(2) -0.090(2) 0.142(12) Uiso 0.50 1 d PD B 2 H32H H 0.2092 0.1577 -0.1308 0.213 Uiso 0.50 1 calc PR B 2 H32I H 0.2780 0.1240 -0.0388 0.213 Uiso 0.50 1 calc PR B 2 H32J H 0.2968 0.2078 -0.1247 0.213 Uiso 0.50 1 calc PR B 2 O33 O 0.1571(3) 0.4243(4) 0.0711(3) 0.0835(16) Uani 1 1 d D . . C331 C 0.1280(9) 0.5243(7) 0.0804(11) 0.151(5) Uani 1 1 d D B . H33A H 0.1163 0.5708 0.0183 0.181 Uiso 1 1 calc R . . H33B H 0.1832 0.5363 0.1114 0.181 Uiso 1 1 calc R . . C332 C 0.0400(9) 0.5460(14) 0.1319(15) 0.250(12) Uani 1 1 d D . . H33C H 0.0223 0.6161 0.1318 0.374 Uiso 1 1 calc R B . H33D H 0.0528 0.5048 0.1954 0.374 Uiso 1 1 calc R . . H33E H -0.0146 0.5318 0.1033 0.374 Uiso 1 1 calc R . . C3 C 0.4668(4) 0.3179(3) 0.3027(3) 0.0397(10) Uani 1 1 d . . . H3A H 0.5376 0.2995 0.3220 0.048 Uiso 1 1 calc R . . H3B H 0.4339 0.3788 0.3214 0.048 Uiso 1 1 calc R . . O4 O 0.5431(2) 0.1191(2) 0.2896(2) 0.0354(7) Uani 1 1 d . . . C41 C 0.4626(3) 0.1386(3) 0.3451(3) 0.0320(9) Uani 1 1 d . . . C42 C 0.4235(3) 0.0597(3) 0.3880(3) 0.0341(9) Uani 1 1 d . . . C43 C 0.3403(3) 0.0803(4) 0.4381(3) 0.0382(10) Uani 1 1 d . . . H43 H 0.3114 0.0285 0.4671 0.046 Uiso 1 1 calc R . . C44 C 0.2985(4) 0.1755(4) 0.4465(3) 0.0397(10) Uani 1 1 d . C . C45 C 0.3396(4) 0.2523(4) 0.4031(3) 0.0422(11) Uani 1 1 d . . . H45 H 0.3107 0.3173 0.4092 0.051 Uiso 1 1 calc R . . C46 C 0.4219(3) 0.2352(3) 0.3514(3) 0.0349(9) Uani 1 1 d . . . O47 O 0.6466(3) 0.1227(3) 0.3983(3) 0.0533(9) Uani 1 1 d . . . C47 C 0.6350(4) 0.1090(3) 0.3255(3) 0.0393(10) Uani 1 1 d . . . C48 C 0.7131(4) 0.0776(4) 0.2622(4) 0.0521(13) Uani 1 1 d . . . H48A H 0.7782 0.0706 0.2893 0.078 Uiso 1 1 calc R . . H48B H 0.7023 0.1278 0.2030 0.078 Uiso 1 1 calc R . . H48C H 0.7102 0.0140 0.2527 0.078 Uiso 1 1 calc R . . P4 P 0.19390(12) 0.19496(14) 0.51645(11) 0.0616(5) Uani 1 1 d D . . O41 O 0.1656(10) 0.1124(8) 0.5811(9) 0.110(4) Uiso 0.50 1 d PD C 1 O42 O 0.2064(10) 0.2824(8) 0.5558(9) 0.107(4) Uiso 0.50 1 d PD C 1 C421 C 0.2551(18) 0.2704(16) 0.6420(14) 0.136(10) Uiso 0.50 1 d PD C 1 H42A H 0.3260 0.2648 0.6322 0.163 Uiso 0.50 1 calc PR C 1 H42B H 0.2498 0.2074 0.6845 0.163 Uiso 0.50 1 calc PR C 1 C422 C 0.217(2) 0.3499(18) 0.6860(14) 0.137(9) Uiso 0.50 1 d PD C 1 H42E H 0.2541 0.3355 0.7444 0.206 Uiso 0.50 1 calc PR C 1 H42F H 0.1470 0.3552 0.6977 0.206 Uiso 0.50 1 calc PR C 1 H42G H 0.2237 0.4124 0.6457 0.206 Uiso 0.50 1 calc PR C 1 O43 O 0.1155(6) 0.2754(7) 0.4462(6) 0.076(3) Uiso 0.50 1 d PD C 1 C431 C 0.0313(8) 0.3285(8) 0.4870(8) 0.059(3) Uiso 0.50 1 d PD C 1 H43A H 0.0544 0.3405 0.5435 0.071 Uiso 0.50 1 calc PR C 1 H43B H -0.0149 0.2865 0.5051 0.071 Uiso 0.50 1 calc PR C 1 C432 C -0.0214(17) 0.4228(13) 0.4259(17) 0.151(11) Uiso 0.50 1 d PD C 1 H43E H -0.0753 0.4563 0.4583 0.226 Uiso 0.50 1 calc PR C 1 H43F H -0.0485 0.4112 0.3717 0.226 Uiso 0.50 1 calc PR C 1 H43G H 0.0242 0.4643 0.4066 0.226 Uiso 0.50 1 calc PR C 1 O41' O 0.1438(5) 0.1097(5) 0.5312(6) 0.0462(16) Uiso 0.50 1 d PD C 2 O42' O 0.2338(5) 0.1853(5) 0.6151(4) 0.0476(16) Uiso 0.50 1 d PD C 2 C42' C 0.2914(9) 0.2470(9) 0.6342(11) 0.067(4) Uiso 0.50 1 d PD C 2 H42C H 0.3390 0.2554 0.5853 0.081 Uiso 0.50 1 calc PR C 2 H42D H 0.3300 0.2121 0.6929 0.081 Uiso 0.50 1 calc PR C 2 C42" C 0.2353(15) 0.3445(10) 0.6406(17) 0.113(7) Uiso 0.50 1 d PD C 2 H42H H 0.2808 0.3823 0.6501 0.169 Uiso 0.50 1 calc PR C 2 H42I H 0.1920 0.3376 0.6924 0.169 Uiso 0.50 1 calc PR C 2 H42J H 0.1953 0.3794 0.5835 0.169 Uiso 0.50 1 calc PR C 2 O43' O 0.1335(5) 0.2988(5) 0.4758(5) 0.0489(18) Uiso 0.50 1 d PD C 2 C43' C 0.0742(13) 0.334(2) 0.3923(11) 0.173(12) Uiso 0.50 1 d PD C 2 H43C H 0.0747 0.2764 0.3681 0.208 Uiso 0.50 1 calc PR C 2 H43D H 0.1051 0.3783 0.3468 0.208 Uiso 0.50 1 calc PR C 2 C43" C -0.0281(10) 0.3866(16) 0.3992(14) 0.105(6) Uiso 0.50 1 d PD C 2 H43H H -0.0636 0.4033 0.3395 0.158 Uiso 0.50 1 calc PR C 2 H43I H -0.0302 0.4475 0.4169 0.158 Uiso 0.50 1 calc PR C 2 H43J H -0.0592 0.3445 0.4456 0.158 Uiso 0.50 1 calc PR C 2 C4 C 0.4714(4) -0.0448(3) 0.3817(3) 0.0384(10) Uani 1 1 d . . . H4A H 0.4947 -0.0876 0.4440 0.046 Uiso 1 1 calc R . . H4B H 0.5296 -0.0447 0.3435 0.046 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 O1 0.0467(18) 0.0340(16) 0.0341(17) -0.0121(13) 0.0026(14) -0.0126(13) C11 0.035(2) 0.033(2) 0.034(2) -0.0148(17) 0.0050(17) -0.0072(17) C12 0.031(2) 0.038(2) 0.034(2) -0.0192(18) 0.0045(17) -0.0028(17) C13 0.034(2) 0.048(3) 0.042(3) -0.025(2) 0.0075(19) -0.0135(19) C14 0.041(2) 0.045(3) 0.037(2) -0.019(2) 0.0115(19) -0.016(2) C15 0.047(3) 0.044(3) 0.035(2) -0.018(2) 0.003(2) -0.014(2) C16 0.039(2) 0.036(2) 0.033(2) -0.0152(18) 0.0014(18) -0.0094(18) O17 0.057(2) 0.051(2) 0.089(3) -0.018(2) 0.028(2) -0.0118(19) C17 0.053(3) 0.047(3) 0.038(3) -0.018(2) 0.009(2) -0.019(2) C18 0.080(4) 0.058(3) 0.039(3) -0.015(2) 0.013(3) -0.033(3) P1 0.0648(10) 0.0698(10) 0.0496(8) -0.0228(7) 0.0223(7) -0.0366(8) C1 0.039(2) 0.038(2) 0.039(2) -0.0175(19) 0.0011(19) -0.0075(19) O2 0.0338(16) 0.0411(17) 0.0344(16) -0.0156(13) -0.0029(13) -0.0057(13) C21 0.031(2) 0.040(2) 0.028(2) -0.0112(17) 0.0026(16) -0.0081(17) C22 0.033(2) 0.033(2) 0.030(2) -0.0111(17) 0.0061(16) -0.0085(17) C23 0.038(2) 0.039(2) 0.031(2) -0.0150(18) 0.0036(17) -0.0106(18) C24 0.032(2) 0.043(2) 0.032(2) -0.0150(19) 0.0025(17) -0.0069(18) C25 0.034(2) 0.041(2) 0.034(2) -0.0181(19) 0.0038(18) -0.0040(18) C26 0.035(2) 0.040(2) 0.029(2) -0.0143(18) 0.0063(17) -0.0092(18) O27 0.057(2) 0.053(2) 0.0370(19) -0.0097(16) 0.0035(16) -0.0091(18) C27 0.049(3) 0.042(3) 0.035(2) -0.018(2) -0.002(2) 0.000(2) C28 0.059(3) 0.050(3) 0.059(3) -0.021(3) -0.024(3) 0.003(3) P2 0.0385(7) 0.0547(8) 0.0542(8) -0.0274(7) -0.0114(6) 0.0023(6) O21 0.038(2) 0.113(4) 0.097(4) -0.072(3) -0.004(2) -0.003(2) O22 0.043(2) 0.092(3) 0.076(3) -0.058(3) -0.0098(19) -0.002(2) C221 0.086(5) 0.078(5) 0.104(6) -0.051(5) 0.004(4) -0.025(4) C222 0.064(5) 0.168(9) 0.094(6) -0.065(6) -0.009(4) -0.038(5) O23 0.065(3) 0.090(4) 0.082(4) 0.006(3) -0.015(3) -0.001(3) C231 0.079(5) 0.075(5) 0.103(6) -0.017(4) -0.027(5) -0.001(4) C232 0.082(6) 0.083(6) 0.149(9) -0.012(6) -0.003(6) -0.024(5) C2 0.041(2) 0.031(2) 0.029(2) -0.0086(17) 0.0039(17) -0.0103(18) O3 0.0381(17) 0.0339(16) 0.0309(16) -0.0108(12) -0.0010(12) -0.0005(13) C31 0.035(2) 0.027(2) 0.033(2) -0.0104(16) 0.0019(17) -0.0017(16) C32 0.044(3) 0.028(2) 0.033(2) -0.0082(17) 0.0070(18) -0.0089(18) C33 0.040(2) 0.037(2) 0.039(3) -0.0071(19) 0.0099(19) -0.0103(19) C34 0.037(2) 0.037(2) 0.040(3) -0.0054(19) -0.0003(19) -0.0083(19) C35 0.039(2) 0.032(2) 0.032(2) -0.0070(17) 0.0007(18) -0.0055(18) C36 0.038(2) 0.0248(19) 0.030(2) -0.0085(16) 0.0038(17) -0.0038(16) O37 0.056(2) 0.0403(19) 0.065(3) -0.0208(17) 0.0045(18) -0.0116(17) C37 0.047(3) 0.041(3) 0.032(2) -0.0087(19) 0.0054(19) -0.013(2) C38 0.054(3) 0.067(4) 0.041(3) -0.012(2) -0.007(2) -0.018(3) P3 0.0429(8) 0.1059(14) 0.0528(9) -0.0001(9) -0.0054(7) -0.0291(9) O31 0.054(3) 0.264(10) 0.082(4) 0.061(5) -0.024(3) -0.058(4) O32 0.131(6) 0.184(8) 0.158(7) -0.057(6) -0.038(5) -0.085(6) O33 0.045(2) 0.104(4) 0.080(3) 0.005(3) 0.005(2) -0.014(2) C331 0.122(10) 0.110(9) 0.207(15) -0.037(9) 0.033(10) -0.016(7) C332 0.063(7) 0.34(3) 0.38(3) -0.21(3) 0.023(12) -0.001(11) C3 0.053(3) 0.036(2) 0.034(2) -0.0140(19) 0.011(2) -0.013(2) O4 0.0366(16) 0.0402(17) 0.0312(16) -0.0151(13) 0.0065(12) -0.0081(13) C41 0.040(2) 0.038(2) 0.0208(19) -0.0117(16) 0.0030(16) -0.0113(18) C42 0.040(2) 0.039(2) 0.026(2) -0.0116(17) -0.0049(17) -0.0102(18) C43 0.039(2) 0.048(3) 0.031(2) -0.0094(19) 0.0017(18) -0.018(2) C44 0.038(2) 0.047(3) 0.032(2) -0.012(2) 0.0077(18) -0.009(2) C45 0.050(3) 0.043(3) 0.032(2) -0.014(2) 0.007(2) -0.006(2) C46 0.042(2) 0.038(2) 0.026(2) -0.0106(17) 0.0063(17) -0.0107(19) O47 0.049(2) 0.072(3) 0.042(2) -0.0183(18) -0.0029(16) -0.0166(18) C47 0.042(3) 0.036(2) 0.037(3) -0.0077(19) 0.0020(19) -0.0085(19) C48 0.042(3) 0.053(3) 0.057(3) -0.013(3) 0.010(2) -0.007(2) P4 0.0460(8) 0.0881(12) 0.0524(9) -0.0249(8) 0.0197(7) -0.0158(8) C4 0.046(3) 0.037(2) 0.034(2) -0.0097(18) -0.0049(19) -0.0123(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 C17 1.365(6) . ? O1 C11 1.410(5) . ? C11 C12 1.388(6) . ? C11 C16 1.396(6) . ? C12 C13 1.392(7) . ? C12 C1 1.524(6) . ? C13 C14 1.392(7) . ? C14 C15 1.388(7) . ? C14 P1 1.798(5) . ? C15 C16 1.387(7) . ? C16 C4 1.517(6) 2_655 ? O17 C17 1.181(7) . ? C17 C18 1.490(7) . ? P1 O11 1.492(7) . ? P1 O11' 1.522(7) . ? P1 O12' 1.526(6) . ? P1 O12 1.529(6) . ? P1 O13' 1.581(6) . ? P1 O13 1.592(6) . ? O12 C121 1.418(9) . ? C121 C122 1.428(9) . ? O13 C131 1.441(8) . ? C131 C132 1.445(8) . ? O12' C12' 1.429(9) . ? C12' C12" 1.451(10) . ? O13' C13' 1.420(9) . ? C13' C13" 1.457(10) . ? C1 C26 1.512(6) . ? O2 C27 1.392(6) . ? O2 C21 1.406(5) . ? C21 C22 1.386(6) . ? C21 C26 1.394(6) . ? C22 C23 1.402(6) . ? C22 C2 1.510(6) . ? C23 C24 1.393(6) . ? C24 C25 1.399(6) . ? C24 P2 1.778(5) . ? C25 C26 1.387(6) . ? O27 C27 1.191(6) . ? C27 C28 1.476(7) . ? P2 O21 1.460(4) . ? P2 O22 1.549(4) . ? P2 O23 1.580(5) . ? O22 C221 1.442(7) . ? C221 C222 1.462(8) . ? O23 C231 1.423(6) . ? C231 C232 1.458(8) . ? C2 C36 1.517(6) . ? O3 C37 1.372(6) . ? O3 C31 1.399(5) . ? C31 C32 1.393(6) . ? C31 C36 1.396(6) . ? C32 C33 1.390(7) . ? C32 C3 1.521(6) . ? C33 C34 1.392(7) . ? C34 C35 1.396(7) . ? C34 P3 1.785(5) . ? C35 C36 1.390(6) . ? O37 C37 1.192(6) . ? C37 C38 1.484(7) . ? P3 O31 1.441(6) . ? P3 O33 1.536(5) . ? P3 O32 1.553(6) . ? O32 C321 1.418(9) . ? O32 C32' 1.426(9) . ? C321 C322 1.453(10) . ? C32' C32" 1.447(10) . ? O33 C331 1.442(8) . ? C331 C332 1.453(9) . ? C3 C46 1.514(6) . ? O4 C47 1.369(6) . ? O4 C41 1.404(5) . ? C41 C46 1.393(6) . ? C41 C42 1.401(6) . ? C42 C43 1.384(7) . ? C42 C4 1.514(6) . ? C43 C44 1.387(7) . ? C44 C45 1.396(7) . ? C44 P4 1.794(5) . ? C45 C46 1.384(6) . ? O47 C47 1.187(6) . ? C47 C48 1.496(7) . ? P4 O41 1.473(8) . ? P4 O43' 1.495(6) . ? P4 O41' 1.543(6) . ? P4 O42' 1.560(6) . ? P4 O43 1.560(7) . ? P4 O42 1.581(7) . ? O42 C421 1.432(9) . ? C421 C422 1.452(10) . ? O43 C431 1.450(8) . ? C431 C432 1.454(10) . ? O42' C42' 1.437(8) . ? C42' C42" 1.453(10) . ? O43' C43' 1.426(9) . ? C43' C43" 1.455(10) . ? C4 C16 1.517(6) 2_655 ? 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 C17 O1 C11 118.2(4) . . ? C12 C11 C16 122.9(4) . . ? C12 C11 O1 118.0(4) . . ? C16 C11 O1 119.0(4) . . ? C11 C12 C13 117.5(4) . . ? C11 C12 C1 119.7(4) . . ? C13 C12 C1 122.7(4) . . ? C12 C13 C14 121.1(4) . . ? C15 C14 C13 119.8(4) . . ? C15 C14 P1 118.2(4) . . ? C13 C14 P1 122.0(4) . . ? C16 C15 C14 120.9(4) . . ? C15 C16 C11 117.9(4) . . ? C15 C16 C4 120.6(4) . 2_655 ? C11 C16 C4 121.6(4) . 2_655 ? O17 C17 O1 122.4(5) . . ? O17 C17 C18 126.6(5) . . ? O1 C17 C18 111.0(5) . . ? O11 P1 O11' 127.6(7) . . ? O11 P1 O12' 74.4(6) . . ? O11' P1 O12' 116.0(6) . . ? O11 P1 O12 119.6(6) . . ? O11' P1 O12 12.7(6) . . ? O12' P1 O12 126.0(5) . . ? O11 P1 O13' 22.1(5) . . ? O11' P1 O13' 113.2(6) . . ? O12' P1 O13' 95.9(5) . . ? O12 P1 O13' 102.6(6) . . ? O11 P1 O13 112.3(6) . . ? O11' P1 O13 89.1(6) . . ? O12' P1 O13 38.1(4) . . ? O12 P1 O13 101.7(5) . . ? O13' P1 O13 133.0(5) . . ? O11 P1 C14 110.7(5) . . ? O11' P1 C14 111.0(5) . . ? O12' P1 C14 112.1(3) . . ? O12 P1 C14 109.7(4) . . ? O13' P1 C14 107.6(4) . . ? O13 P1 C14 101.1(3) . . ? C121 O12 P1 119.5(9) . . ? O12 C121 C122 121.7(10) . . ? C131 O13 P1 125.4(7) . . ? O13 C131 C132 115.6(8) . . ? C12' O12' P1 118.1(8) . . ? O12' C12' C12" 115.6(10) . . ? C13' O13' P1 128.5(10) . . ? O13' C13' C13" 115.6(9) . . ? C26 C1 C12 116.5(4) . . ? C27 O2 C21 117.5(4) . . ? C22 C21 C26 123.6(4) . . ? C22 C21 O2 119.9(4) . . ? C26 C21 O2 116.3(4) . . ? C21 C22 C23 117.0(4) . . ? C21 C22 C2 122.8(4) . . ? C23 C22 C2 120.1(4) . . ? C24 C23 C22 121.3(4) . . ? C23 C24 C25 119.3(4) . . ? C23 C24 P2 123.0(3) . . ? C25 C24 P2 117.7(3) . . ? C26 C25 C24 121.1(4) . . ? C25 C26 C21 117.7(4) . . ? C25 C26 C1 119.9(4) . . ? C21 C26 C1 122.2(4) . . ? O27 C27 O2 122.4(5) . . ? O27 C27 C28 127.4(5) . . ? O2 C27 C28 110.2(5) . . ? O21 P2 O22 114.9(3) . . ? O21 P2 O23 117.2(3) . . ? O22 P2 O23 102.2(3) . . ? O21 P2 C24 114.9(2) . . ? O22 P2 C24 106.7(2) . . ? O23 P2 C24 98.9(2) . . ? C221 O22 P2 122.7(4) . . ? O22 C221 C222 113.9(6) . . ? C231 O23 P2 126.9(5) . . ? O23 C231 C232 113.9(6) . . ? C22 C2 C36 114.2(3) . . ? C37 O3 C31 117.2(3) . . ? C32 C31 C36 122.9(4) . . ? C32 C31 O3 120.0(4) . . ? C36 C31 O3 117.0(4) . . ? C33 C32 C31 117.8(4) . . ? C33 C32 C3 120.5(4) . . ? C31 C32 C3 121.7(4) . . ? C32 C33 C34 121.2(4) . . ? C33 C34 C35 119.4(4) . . ? C33 C34 P3 121.4(4) . . ? C35 C34 P3 119.2(4) . . ? C36 C35 C34 121.2(4) . . ? C35 C36 C31 117.6(4) . . ? C35 C36 C2 121.6(4) . . ? C31 C36 C2 120.8(4) . . ? O37 C37 O3 121.4(5) . . ? O37 C37 C38 127.4(5) . . ? O3 C37 C38 111.2(4) . . ? O31 P3 O33 114.1(4) . . ? O31 P3 O32 119.4(5) . . ? O33 P3 O32 95.4(4) . . ? O31 P3 C34 111.8(3) . . ? O33 P3 C34 108.3(3) . . ? O32 P3 C34 106.3(3) . . ? C321 O32 C32' 52.8(10) . . ? C321 O32 P3 136.0(11) . . ? C32' O32 P3 137.8(15) . . ? O32 C321 C322 116.0(9) . . ? O32 C32' C32" 117.0(10) . . ? C331 O33 P3 117.6(6) . . ? O33 C331 C332 114.2(8) . . ? C46 C3 C32 112.3(4) . . ? C47 O4 C41 117.6(3) . . ? C46 C41 C42 122.9(4) . . ? C46 C41 O4 119.4(4) . . ? C42 C41 O4 117.6(4) . . ? C43 C42 C41 117.5(4) . . ? C43 C42 C4 121.1(4) . . ? C41 C42 C4 121.4(4) . . ? C42 C43 C44 121.1(4) . . ? C43 C44 C45 119.9(4) . . ? C43 C44 P4 118.3(4) . . ? C45 C44 P4 121.8(4) . . ? C46 C45 C44 120.9(4) . . ? C45 C46 C41 117.7(4) . . ? C45 C46 C3 121.7(4) . . ? C41 C46 C3 120.6(4) . . ? O47 C47 O4 121.9(4) . . ? O47 C47 C48 127.2(5) . . ? O4 C47 C48 110.9(4) . . ? O41 P4 O43' 129.3(6) . . ? O41 P4 O41' 31.9(6) . . ? O43' P4 O41' 118.9(4) . . ? O41 P4 O42' 71.4(7) . . ? O43' P4 O42' 109.6(4) . . ? O41' P4 O42' 103.2(4) . . ? O41 P4 O43 120.2(7) . . ? O43' P4 O43 26.8(4) . . ? O41' P4 O43 98.1(5) . . ? O42' P4 O43 134.6(5) . . ? O41 P4 O42 117.1(8) . . ? O43' P4 O42 59.6(6) . . ? O41' P4 O42 144.0(6) . . ? O42' P4 O42 53.6(5) . . ? O43 P4 O42 86.4(7) . . ? O41 P4 C44 122.2(6) . . ? O43' P4 C44 106.2(3) . . ? O41' P4 C44 111.2(3) . . ? O42' P4 C44 107.3(3) . . ? O43 P4 C44 101.4(4) . . ? O42 P4 C44 102.7(5) . . ? C421 O42 P4 125.2(12) . . ? O42 C421 C422 115.0(10) . . ? C431 O43 P4 114.9(7) . . ? O43 C431 C432 113.4(9) . . ? C42' O42' P4 123.1(8) . . ? O42' C42' C42" 115.4(9) . . ? C43' O43' P4 126.4(14) . . ? O43' C43' C43" 115.8(10) . . ? C42 C4 C16 112.2(4) . 2_655 ? 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 96.8(5) . . . . ? C17 O1 C11 C16 -87.5(5) . . . . ? C16 C11 C12 C13 -3.5(6) . . . . ? O1 C11 C12 C13 172.0(4) . . . . ? C16 C11 C12 C1 178.4(4) . . . . ? O1 C11 C12 C1 -6.1(6) . . . . ? C11 C12 C13 C14 2.3(6) . . . . ? C1 C12 C13 C14 -179.7(4) . . . . ? C12 C13 C14 C15 0.3(7) . . . . ? C12 C13 C14 P1 -175.6(3) . . . . ? C13 C14 C15 C16 -1.9(7) . . . . ? P1 C14 C15 C16 174.1(4) . . . . ? C14 C15 C16 C11 0.8(7) . . . . ? C14 C15 C16 C4 -178.4(4) . . . 2_655 ? C12 C11 C16 C15 2.0(7) . . . . ? O1 C11 C16 C15 -173.5(4) . . . . ? C12 C11 C16 C4 -178.8(4) . . . 2_655 ? O1 C11 C16 C4 5.8(6) . . . 2_655 ? C11 O1 C17 O17 5.8(7) . . . . ? C11 O1 C17 C18 -172.2(4) . . . . ? C15 C14 P1 O11 29.7(7) . . . . ? C13 C14 P1 O11 -154.4(6) . . . . ? C15 C14 P1 O11' 177.3(6) . . . . ? C13 C14 P1 O11' -6.8(7) . . . . ? C15 C14 P1 O12' -51.2(5) . . . . ? C13 C14 P1 O12' 124.7(5) . . . . ? C15 C14 P1 O12 163.8(5) . . . . ? C13 C14 P1 O12 -20.3(6) . . . . ? C15 C14 P1 O13' 52.9(6) . . . . ? C13 C14 P1 O13' -131.2(6) . . . . ? C15 C14 P1 O13 -89.4(5) . . . . ? C13 C14 P1 O13 86.5(5) . . . . ? O11 P1 O12 C121 29.0(14) . . . . ? O11' P1 O12 C121 161(4) . . . . ? O12' P1 O12 C121 120.6(12) . . . . ? O13' P1 O12 C121 13.7(13) . . . . ? O13 P1 O12 C121 153.1(11) . . . . ? C14 P1 O12 C121 -100.5(12) . . . . ? P1 O12 C121 C122 152.6(14) . . . . ? O11 P1 O13 C131 -60.7(10) . . . . ? O11' P1 O13 C131 168.6(9) . . . . ? O12' P1 O13 C131 -54.4(8) . . . . ? O12 P1 O13 C131 170.4(8) . . . . ? O13' P1 O13 C131 -69.8(10) . . . . ? C14 P1 O13 C131 57.3(8) . . . . ? P1 O13 C131 C132 133.6(9) . . . . ? O11 P1 O12' C12' -169.7(13) . . . . ? O11' P1 O12' C12' 65.7(13) . . . . ? O12 P1 O12' C12' 74.8(13) . . . . ? O13' P1 O12' C12' -174.9(12) . . . . ? O13 P1 O12' C12' 16.3(11) . . . . ? C14 P1 O12' C12' -63.3(12) . . . . ? P1 O12' C12' C12" -175(2) . . . . ? O11 P1 O13' C13' 169(3) . . . . ? O11' P1 O13' C13' -56.1(14) . . . . ? O12' P1 O13' C13' -177.6(13) . . . . ? O12 P1 O13' C13' -48.7(14) . . . . ? O13 P1 O13' C13' -168.2(11) . . . . ? C14 P1 O13' C13' 67.0(13) . . . . ? P1 O13' C13' C13" -140.6(19) . . . . ? C11 C12 C1 C26 -151.8(4) . . . . ? C13 C12 C1 C26 30.3(6) . . . . ? C27 O2 C21 C22 78.7(5) . . . . ? C27 O2 C21 C26 -105.9(4) . . . . ? C26 C21 C22 C23 0.2(6) . . . . ? O2 C21 C22 C23 175.2(4) . . . . ? C26 C21 C22 C2 -178.2(4) . . . . ? O2 C21 C22 C2 -3.2(6) . . . . ? C21 C22 C23 C24 0.2(6) . . . . ? C2 C22 C23 C24 178.6(4) . . . . ? C22 C23 C24 C25 -0.3(7) . . . . ? C22 C23 C24 P2 -176.4(3) . . . . ? C23 C24 C25 C26 0.2(7) . . . . ? P2 C24 C25 C26 176.4(4) . . . . ? C24 C25 C26 C21 0.2(7) . . . . ? C24 C25 C26 C1 -174.5(4) . . . . ? C22 C21 C26 C25 -0.3(7) . . . . ? O2 C21 C26 C25 -175.5(4) . . . . ? C22 C21 C26 C1 174.2(4) . . . . ? O2 C21 C26 C1 -1.0(6) . . . . ? C12 C1 C26 C25 -125.8(5) . . . . ? C12 C1 C26 C21 59.7(6) . . . . ? C21 O2 C27 O27 -9.0(6) . . . . ? C21 O2 C27 C28 170.6(4) . . . . ? C23 C24 P2 O21 -123.5(4) . . . . ? C25 C24 P2 O21 60.4(5) . . . . ? C23 C24 P2 O22 5.1(5) . . . . ? C25 C24 P2 O22 -171.0(4) . . . . ? C23 C24 P2 O23 110.8(4) . . . . ? C25 C24 P2 O23 -65.3(4) . . . . ? O21 P2 O22 C221 3.4(6) . . . . ? O23 P2 O22 C221 131.5(5) . . . . ? C24 P2 O22 C221 -125.3(5) . . . . ? P2 O22 C221 C222 -82.0(8) . . . . ? O21 P2 O23 C231 34.5(7) . . . . ? O22 P2 O23 C231 -92.1(7) . . . . ? C24 P2 O23 C231 158.6(6) . . . . ? P2 O23 C231 C232 -127.0(8) . . . . ? C21 C22 C2 C36 73.3(5) . . . . ? C23 C22 C2 C36 -105.1(5) . . . . ? C37 O3 C31 C32 -75.0(5) . . . . ? C37 O3 C31 C36 107.2(4) . . . . ? C36 C31 C32 C33 0.9(6) . . . . ? O3 C31 C32 C33 -176.7(4) . . . . ? C36 C31 C32 C3 -178.6(4) . . . . ? O3 C31 C32 C3 3.8(6) . . . . ? C31 C32 C33 C34 -1.2(7) . . . . ? C3 C32 C33 C34 178.3(4) . . . . ? C32 C33 C34 C35 0.8(7) . . . . ? C32 C33 C34 P3 -176.8(4) . . . . ? C33 C34 C35 C36 -0.1(7) . . . . ? P3 C34 C35 C36 177.6(3) . . . . ? C34 C35 C36 C31 -0.3(6) . . . . ? C34 C35 C36 C2 -177.0(4) . . . . ? C32 C31 C36 C35 -0.2(6) . . . . ? O3 C31 C36 C35 177.6(4) . . . . ? C32 C31 C36 C2 176.6(4) . . . . ? O3 C31 C36 C2 -5.7(6) . . . . ? C22 C2 C36 C35 -106.0(5) . . . . ? C22 C2 C36 C31 77.4(5) . . . . ? C31 O3 C37 O37 -1.3(6) . . . . ? C31 O3 C37 C38 177.8(4) . . . . ? C33 C34 P3 O31 144.0(6) . . . . ? C35 C34 P3 O31 -33.6(6) . . . . ? C33 C34 P3 O33 17.5(5) . . . . ? C35 C34 P3 O33 -160.2(4) . . . . ? C33 C34 P3 O32 -84.1(5) . . . . ? C35 C34 P3 O32 98.3(5) . . . . ? O31 P3 O32 C321 66.1(13) . . . . ? O33 P3 O32 C321 -172.3(12) . . . . ? C34 P3 O32 C321 -61.4(13) . . . . ? O31 P3 O32 C32' -15.1(17) . . . . ? O33 P3 O32 C32' 106.5(16) . . . . ? C34 P3 O32 C32' -142.6(16) . . . . ? C32' O32 C321 C322 0(2) . . . . ? P3 O32 C321 C322 -123.3(15) . . . . ? C321 O32 C32' C32" -7(2) . . . . ? P3 O32 C32' C32" 114(3) . . . . ? O31 P3 O33 C331 -42.5(9) . . . . ? O32 P3 O33 C331 -168.1(9) . . . . ? C34 P3 O33 C331 82.7(8) . . . . ? P3 O33 C331 C332 169.1(11) . . . . ? C33 C32 C3 C46 50.0(6) . . . . ? C31 C32 C3 C46 -130.5(4) . . . . ? C47 O4 C41 C46 81.1(5) . . . . ? C47 O4 C41 C42 -102.3(5) . . . . ? C46 C41 C42 C43 0.4(6) . . . . ? O4 C41 C42 C43 -176.0(4) . . . . ? C46 C41 C42 C4 -178.4(4) . . . . ? O4 C41 C42 C4 5.2(6) . . . . ? C41 C42 C43 C44 -1.1(7) . . . . ? C4 C42 C43 C44 177.7(4) . . . . ? C42 C43 C44 C45 0.9(7) . . . . ? C42 C43 C44 P4 -177.5(3) . . . . ? C43 C44 C45 C46 0.0(7) . . . . ? P4 C44 C45 C46 178.3(4) . . . . ? C44 C45 C46 C41 -0.7(7) . . . . ? C44 C45 C46 C3 179.2(4) . . . . ? C42 C41 C46 C45 0.4(7) . . . . ? O4 C41 C46 C45 176.8(4) . . . . ? C42 C41 C46 C3 -179.4(4) . . . . ? O4 C41 C46 C3 -3.0(6) . . . . ? C32 C3 C46 C45 -113.7(5) . . . . ? C32 C3 C46 C41 66.1(6) . . . . ? C41 O4 C47 O47 -5.1(7) . . . . ? C41 O4 C47 C48 173.8(4) . . . . ? C43 C44 P4 O41 14.5(9) . . . . ? C45 C44 P4 O41 -163.9(8) . . . . ? C43 C44 P4 O43' -149.9(5) . . . . ? C45 C44 P4 O43' 31.8(6) . . . . ? C43 C44 P4 O41' -19.2(5) . . . . ? C45 C44 P4 O41' 162.4(5) . . . . ? C43 C44 P4 O42' 93.0(5) . . . . ? C45 C44 P4 O42' -85.4(5) . . . . ? C43 C44 P4 O43 -122.7(6) . . . . ? C45 C44 P4 O43 59.0(6) . . . . ? C43 C44 P4 O42 148.5(6) . . . . ? C45 C44 P4 O42 -29.9(7) . . . . ? O41 P4 O42 C421 43(2) . . . . ? O43' P4 O42 C421 164.9(19) . . . . ? O41' P4 O42 C421 67(2) . . . . ? O42' P4 O42 C421 8.7(16) . . . . ? O43 P4 O42 C421 165.5(18) . . . . ? C44 P4 O42 C421 -93.6(17) . . . . ? P4 O42 C421 C422 -149.4(19) . . . . ? O41 P4 O43 C431 59.0(12) . . . . ? O43' P4 O43 C431 -59.3(11) . . . . ? O41' P4 O43 C431 83.6(10) . . . . ? O42' P4 O43 C431 -34.2(12) . . . . ? O42 P4 O43 C431 -60.5(10) . . . . ? C44 P4 O43 C431 -162.7(8) . . . . ? P4 O43 C431 C432 159.8(16) . . . . ? O41 P4 O42' C42' 177.9(10) . . . . ? O43' P4 O42' C42' -55.9(9) . . . . ? O41' P4 O42' C42' 176.5(8) . . . . ? O43 P4 O42' C42' -67.7(11) . . . . ? O42 P4 O42' C42' -34.2(9) . . . . ? C44 P4 O42' C42' 59.0(8) . . . . ? P4 O42' C42' C42" 80.7(16) . . . . ? O41 P4 O43' C43' -89.6(16) . . . . ? O41' P4 O43' C43' -52.9(15) . . . . ? O42' P4 O43' C43' -171.1(14) . . . . ? O43 P4 O43' C43' -9.9(16) . . . . ? O42 P4 O43' C43' 168.7(16) . . . . ? C44 P4 O43' C43' 73.3(14) . . . . ? P4 O43' C43' C43" 127(2) . . . . ? C43 C42 C4 C16 59.1(5) . . . 2_655 ? C41 C42 C4 C16 -122.2(5) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 27.15 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.388 _refine_diff_density_min -0.920 _refine_diff_density_rms 0.107