# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Krishnamurthy S. Setharampattu' _publ_contact_author_address ; Inorganic and physical Chemistry Indian Institute of Science Bangalore 560012 INDIA ; _publ_contact_author_email SSKRISH@IPC.IISC.ERNET.IN loop_ _publ_author_name 'Krishnamurthy Setharampattu' 'Pathik Maji' 'Munirathinam Nethaji' # Attachment 'NJC.CIF-27-1-10.cif' data_pat24_m _database_code_depnum_ccdc_archive 'CCDC 695456' #TrackingRef 'NJC.CIF-27-1-10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 5,11,17,23-tetra-(tert-butyl)calix[4]arene 25,26-(dihydroxy){27,28-(2,6-di-tert-butyl- 4-methyl-phenyl)}monophosphite,monohydrate ; _chemical_name_common ; 5,11,17,23-tetra-(tert-butyl)calix(4)arene 25,26- (dihydroxy)(27,28-(2,6-di-tert-butyl-4-methyl- phenyl))monophosphite,monohydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C59 H79 O6 P' _chemical_formula_sum 'C59 H79 O6 P' _chemical_formula_weight 915.19 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 MONOCLINIC _symmetry_space_group_name_H-M I2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 14.929(3) _cell_length_b 21.378(3) _cell_length_c 18.173(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.889(11) _cell_angle_gamma 90.00 _cell_volume 5487.8(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 378 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 27.0 _exptl_crystal_description RECTANGULAR _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.108 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 0.097 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.9549 _exptl_absorpt_correction_T_max 0.9714 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEX CCD' _diffrn_measurement_method OMEGA _diffrn_detector_area_resol_mean 0.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19854 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4980 _reflns_number_gt 3506 _reflns_threshold_expression >2\s(I) _computing_data_collection 'BRUKER SMART APEX CCD' _computing_cell_refinement 'BRUKER SMART APEX CCD' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP-III _computing_publication_material 'WINGX V1.80.01' _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^ > 2\s(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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4980 _refine_ls_number_parameters 326 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1373 _refine_ls_R_factor_gt 0.1067 _refine_ls_wR_factor_ref 0.3451 _refine_ls_wR_factor_gt 0.3228 _refine_ls_goodness_of_fit_ref 1.306 _refine_ls_restrained_S_all 1.312 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.005 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.76395(9) 0.5000 0.47576(7) 0.0371(3) Uani 1 2 d S . . O1 O 0.72641(18) 0.43984(13) 0.41988(14) 0.0538(8) Uani 1 1 d . . . O2 O 0.6904(2) 0.5000 0.52711(17) 0.0318(7) Uani 1 2 d S . . O3 O 0.9234(2) 0.43609(13) 0.41187(16) 0.0554(7) Uani 1 1 d D . . O4 O 0.6983(9) 0.5000 0.1599(8) 0.230(5) Uiso 0.94 2 d SP . . H3A H 0.875(2) 0.437(5) 0.440(2) 0.33(6) Uiso 1 1 d D . . C1 C 0.5377(3) 0.5000 0.3590(3) 0.0337(11) Uani 1 2 d S . . H1A H 0.5668 0.5000 0.4151 0.040 Uiso 1 2 calc SR . . H1B H 0.4695 0.5000 0.3471 0.040 Uiso 1 2 calc SR . . C2 C 0.5684(2) 0.44202(16) 0.32440(19) 0.0330(8) Uani 1 1 d . . . C3 C 0.5056(2) 0.41534(17) 0.2581(2) 0.0387(9) Uani 1 1 d . . . H3 H 0.4442 0.4310 0.2392 0.046 Uiso 1 1 calc R . . C4 C 0.5311(3) 0.36583(17) 0.2189(2) 0.0409(9) Uani 1 1 d . . . C5 C 0.6222(3) 0.34244(17) 0.2501(2) 0.0405(9) Uani 1 1 d . . . H5 H 0.6402 0.3089 0.2254 0.049 Uiso 1 1 calc R . . C6 C 0.6884(2) 0.36731(16) 0.3173(2) 0.0334(8) Uani 1 1 d . . . C7 C 0.6600(2) 0.41740(16) 0.35282(18) 0.0327(8) Uani 1 1 d . . . C8 C 0.7878(2) 0.33945(17) 0.3475(2) 0.0373(8) Uani 1 1 d . . . H8A H 0.7835 0.2944 0.3407 0.045 Uiso 1 1 calc R . . H8B H 0.8145 0.3479 0.4028 0.045 Uiso 1 1 calc R . . C9 C 0.8542(2) 0.36548(16) 0.3064(2) 0.0362(8) Uani 1 1 d . . . C10 C 0.8518(3) 0.34289(18) 0.2340(2) 0.0415(9) Uani 1 1 d . . . H10 H 0.8106 0.3103 0.2120 0.050 Uiso 1 1 calc R . . C11 C 0.9083(3) 0.36686(17) 0.1928(2) 0.0421(9) Uani 1 1 d . . . C12 C 0.9668(2) 0.41662(17) 0.2266(2) 0.0409(9) Uani 1 1 d . . . H12 H 1.0049 0.4339 0.2003 0.049 Uiso 1 1 calc R . . C13 C 0.9707(2) 0.44126(17) 0.2972(2) 0.0369(9) Uani 1 1 d . . . C14 C 0.9166(2) 0.41469(17) 0.3384(2) 0.0367(8) Uani 1 1 d D . . C15 C 1.0307(3) 0.5000 0.3283(3) 0.0434(13) Uani 1 2 d S . . H15A H 1.0862 0.5000 0.3115 0.052 Uiso 1 2 calc SR . . H15B H 1.0519 0.5000 0.3847 0.052 Uiso 1 2 calc SR . . C16 C 0.7197(3) 0.5000 0.6100(2) 0.0286(11) Uani 1 2 d S . . C17 C 0.7301(2) 0.55788(16) 0.64914(19) 0.0336(8) Uani 1 1 d . . . C18 C 0.7585(2) 0.55524(19) 0.7304(2) 0.0420(9) Uani 1 1 d . . . H18 H 0.7672 0.5926 0.7580 0.050 Uiso 1 1 calc R . . C19 C 0.7740(4) 0.5000 0.7714(3) 0.0429(13) Uani 1 2 d SD . . C20 C 0.4612(3) 0.3405(2) 0.1430(3) 0.0589(12) Uani 1 1 d . . . C21 C 0.4369(5) 0.3953(3) 0.0813(3) 0.104(2) Uani 1 1 d . . . H21A H 0.3815 0.3845 0.0386 0.156 Uiso 1 1 calc R . . H21B H 0.4892 0.4018 0.0624 0.156 Uiso 1 1 calc R . . H21C H 0.4250 0.4330 0.1053 0.156 Uiso 1 1 calc R . . C22 C 0.4993(4) 0.2856(3) 0.1090(4) 0.106(2) Uani 1 1 d . . . H22A H 0.5106 0.2508 0.1443 0.158 Uiso 1 1 calc R . . H22B H 0.5575 0.2975 0.1010 0.158 Uiso 1 1 calc R . . H22C H 0.4539 0.2738 0.0601 0.158 Uiso 1 1 calc R . . C23 C 0.3696(4) 0.3207(3) 0.1550(3) 0.105(2) Uani 1 1 d . . . H23A H 0.3806 0.2843 0.1877 0.158 Uiso 1 1 calc R . . H23B H 0.3234 0.3111 0.1056 0.158 Uiso 1 1 calc R . . H23C H 0.3465 0.3541 0.1793 0.158 Uiso 1 1 calc R . . C24 C 0.9084(3) 0.3405(2) 0.1137(2) 0.0568(11) Uani 1 1 d . . . C25 C 1.0032(4) 0.3081(4) 0.1241(4) 0.115(2) Uani 1 1 d . . . H25A H 1.0531 0.3308 0.1613 0.172 Uiso 1 1 calc R . . H25B H 1.0148 0.3070 0.0751 0.172 Uiso 1 1 calc R . . H25C H 1.0012 0.2662 0.1424 0.172 Uiso 1 1 calc R . . C26 C 0.8938(5) 0.3931(3) 0.0532(3) 0.098(2) Uani 1 1 d . . . H26A H 0.8317 0.4107 0.0426 0.147 Uiso 1 1 calc R . . H26B H 0.9000 0.3764 0.0061 0.147 Uiso 1 1 calc R . . H26C H 0.9406 0.4250 0.0731 0.147 Uiso 1 1 calc R . . C27 C 0.8284(4) 0.2936(3) 0.0792(3) 0.0958(19) Uani 1 1 d . . . H27A H 0.8358 0.2586 0.1138 0.144 Uiso 1 1 calc R . . H27B H 0.8306 0.2793 0.0297 0.144 Uiso 1 1 calc R . . H27C H 0.7686 0.3134 0.0724 0.144 Uiso 1 1 calc R . . C28 C 0.7161(3) 0.62294(16) 0.6094(2) 0.0407(9) Uani 1 1 d . . . C29 C 0.7094(4) 0.6757(2) 0.6664(3) 0.0664(13) Uani 1 1 d . . . H29A H 0.6585 0.6667 0.6862 0.100 Uiso 1 1 calc R . . H29B H 0.6977 0.7150 0.6393 0.100 Uiso 1 1 calc R . . H29C H 0.7678 0.6780 0.7087 0.100 Uiso 1 1 calc R . . C30 C 0.8009(3) 0.6385(2) 0.5825(3) 0.0522(11) Uani 1 1 d . . . H30A H 0.8548 0.6483 0.6269 0.078 Uiso 1 1 calc R . . H30B H 0.7858 0.6739 0.5482 0.078 Uiso 1 1 calc R . . H30C H 0.8152 0.6032 0.5557 0.078 Uiso 1 1 calc R . . C31 C 0.6210(3) 0.6250(2) 0.5416(3) 0.0548(12) Uani 1 1 d . . . H31A H 0.6241 0.5969 0.5012 0.082 Uiso 1 1 calc R . . H31B H 0.6097 0.6667 0.5213 0.082 Uiso 1 1 calc R . . H31C H 0.5705 0.6124 0.5602 0.082 Uiso 1 1 calc R . . C32 C 0.8072(5) 0.5000 0.8601(4) 0.075(2) Uani 1 2 d SD . . H32A H 0.8829(12) 0.5000 0.879(3) 0.23(5) Uiso 1 2 d SD . . H32B H 0.7504(18) 0.5000 0.883(2) 0.18(5) Uiso 1 2 d SD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0311(6) 0.0576(8) 0.0210(6) 0.000 0.0062(5) 0.000 O1 0.0484(15) 0.0697(18) 0.0329(13) -0.0169(12) -0.0013(11) 0.0185(13) O2 0.0341(16) 0.0355(17) 0.0253(15) 0.000 0.0087(13) 0.000 O3 0.0623(16) 0.0613(18) 0.0461(15) -0.0088(13) 0.0224(13) -0.0054(14) C1 0.032(2) 0.040(3) 0.029(2) 0.000 0.0104(19) 0.000 C2 0.0341(16) 0.0352(18) 0.0309(16) 0.0047(14) 0.0125(13) -0.0024(14) C3 0.0355(17) 0.041(2) 0.0387(19) -0.0017(16) 0.0104(15) -0.0051(16) C4 0.0412(19) 0.041(2) 0.0396(19) -0.0061(16) 0.0117(16) -0.0101(16) C5 0.048(2) 0.0346(19) 0.0427(19) -0.0099(16) 0.0201(16) -0.0035(16) C6 0.0330(17) 0.0328(18) 0.0346(17) 0.0037(14) 0.0113(14) -0.0025(14) C7 0.0352(17) 0.0395(19) 0.0239(15) -0.0006(14) 0.0105(13) -0.0025(15) C8 0.0444(19) 0.0323(18) 0.0387(18) 0.0029(15) 0.0182(15) 0.0032(15) C9 0.0340(17) 0.0307(18) 0.0442(19) 0.0047(15) 0.0131(15) 0.0052(15) C10 0.0423(19) 0.0362(19) 0.047(2) 0.0018(16) 0.0153(16) 0.0024(16) C11 0.046(2) 0.039(2) 0.044(2) 0.0036(16) 0.0181(16) 0.0057(17) C12 0.0357(17) 0.041(2) 0.049(2) 0.0058(17) 0.0185(15) 0.0028(16) C13 0.0241(16) 0.042(2) 0.0426(19) 0.0044(16) 0.0075(14) 0.0079(15) C14 0.0334(17) 0.0389(19) 0.0380(18) 0.0033(15) 0.0120(14) 0.0097(15) C15 0.028(2) 0.052(3) 0.054(3) 0.000 0.017(2) 0.000 C16 0.021(2) 0.040(3) 0.023(2) 0.000 0.0053(17) 0.000 C17 0.0238(15) 0.044(2) 0.0334(17) 0.0000(15) 0.0100(13) 0.0036(14) C18 0.0376(19) 0.054(2) 0.0336(18) -0.0126(17) 0.0104(15) 0.0016(17) C19 0.041(3) 0.060(3) 0.027(2) 0.000 0.010(2) 0.000 C20 0.057(2) 0.068(3) 0.047(2) -0.022(2) 0.011(2) -0.009(2) C21 0.121(5) 0.119(5) 0.047(3) -0.007(3) -0.007(3) -0.019(4) C22 0.086(4) 0.123(5) 0.082(4) -0.061(4) -0.009(3) 0.011(4) C23 0.077(3) 0.153(6) 0.085(4) -0.062(4) 0.025(3) -0.052(4) C24 0.073(3) 0.058(3) 0.046(2) -0.0039(19) 0.030(2) -0.004(2) C25 0.108(4) 0.160(6) 0.076(4) -0.034(4) 0.029(3) 0.050(4) C26 0.167(6) 0.080(4) 0.055(3) 0.002(3) 0.047(3) -0.018(4) C27 0.123(4) 0.114(4) 0.060(3) -0.031(3) 0.043(3) -0.058(4) C28 0.0401(19) 0.0329(19) 0.046(2) -0.0058(16) 0.0095(16) 0.0032(16) C29 0.087(3) 0.049(2) 0.065(3) -0.010(2) 0.027(2) 0.014(2) C30 0.060(2) 0.046(2) 0.055(2) 0.0003(19) 0.0236(19) -0.0108(19) C31 0.045(2) 0.049(2) 0.061(3) 0.008(2) 0.004(2) 0.0134(19) C32 0.081(5) 0.108(6) 0.031(3) 0.000 0.011(3) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O1 1.622(3) . ? P1 O1 1.622(3) 6_565 ? P1 O2 1.655(3) . ? O1 C7 1.384(3) . ? O2 C16 1.426(4) . ? O3 C14 1.383(4) . ? O3 H3A 1.014(19) . ? C1 C2 1.526(4) . ? C1 C2 1.526(4) 6_565 ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.387(5) . ? C2 C7 1.399(5) . ? C3 C4 1.396(5) . ? C3 H3 0.9300 . ? C4 C5 1.386(5) . ? C4 C20 1.535(5) . ? C5 C6 1.404(5) . ? C5 H5 0.9300 . ? C6 C7 1.385(5) . ? C6 C8 1.526(5) . ? C8 C9 1.528(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.391(5) . ? C9 C14 1.401(5) . ? C10 C11 1.394(5) . ? C10 H10 0.9300 . ? C11 C12 1.387(5) . ? C11 C24 1.545(6) . ? C12 C13 1.371(5) . ? C12 H12 0.9300 . ? C13 C14 1.388(5) . ? C13 C15 1.540(4) . ? C15 C13 1.540(4) 6_565 ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.411(4) 6_565 ? C16 C17 1.411(4) . ? C17 C18 1.399(5) . ? C17 C28 1.550(5) . ? C18 C19 1.375(5) . ? C18 H18 0.9300 . ? C19 C18 1.375(5) 6_565 ? C19 C32 1.526(8) . ? C20 C23 1.514(7) . ? C20 C22 1.520(7) . ? C20 C21 1.582(8) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C27 1.529(7) . ? C24 C25 1.532(7) . ? C24 C26 1.538(7) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C30 1.534(6) . ? C28 C31 1.550(5) . ? C28 C29 1.557(6) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 1.070(16) . ? C32 H32B 1.064(18) . ? 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 O1 P1 O1 104.9(2) . 6_565 ? O1 P1 O2 101.25(13) . . ? O1 P1 O2 101.25(13) 6_565 . ? C7 O1 P1 146.09(19) . . ? C16 O2 P1 124.28(19) . . ? C14 O3 H3A 131(3) . . ? C2 C1 C2 108.6(4) . 6_565 ? C2 C1 H1A 110.0 . . ? C2 C1 H1A 110.0 6_565 . ? C2 C1 H1B 110.0 . . ? C2 C1 H1B 110.0 6_565 . ? H1A C1 H1B 108.3 . . ? C3 C2 C7 118.1(3) . . ? C3 C2 C1 118.9(3) . . ? C7 C2 C1 122.8(3) . . ? C2 C3 C4 122.3(3) . . ? C2 C3 H3 118.8 . . ? C4 C3 H3 118.8 . . ? C5 C4 C3 117.3(3) . . ? C5 C4 C20 122.1(4) . . ? C3 C4 C20 120.5(3) . . ? C4 C5 C6 122.7(3) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C7 C6 C5 117.6(3) . . ? C7 C6 C8 122.8(3) . . ? C5 C6 C8 119.6(3) . . ? O1 C7 C6 116.0(3) . . ? O1 C7 C2 122.0(3) . . ? C6 C7 C2 121.9(3) . . ? C6 C8 C9 113.0(3) . . ? C6 C8 H8A 109.0 . . ? C9 C8 H8A 109.0 . . ? C6 C8 H8B 109.0 . . ? C9 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C10 C9 C14 117.7(3) . . ? C10 C9 C8 121.0(3) . . ? C14 C9 C8 121.3(3) . . ? C9 C10 C11 123.0(3) . . ? C9 C10 H10 118.5 . . ? C11 C10 H10 118.5 . . ? C12 C11 C10 116.7(4) . . ? C12 C11 C24 120.1(4) . . ? C10 C11 C24 123.2(3) . . ? C13 C12 C11 122.5(4) . . ? C13 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? C12 C13 C14 119.5(3) . . ? C12 C13 C15 120.0(4) . . ? C14 C13 C15 120.5(4) . . ? O3 C14 C13 120.7(3) . . ? O3 C14 C9 118.8(3) . . ? C13 C14 C9 120.5(3) . . ? C13 C15 C13 109.2(4) . 6_565 ? C13 C15 H15A 109.8 . . ? C13 C15 H15A 109.8 6_565 . ? C13 C15 H15B 109.8 . . ? C13 C15 H15B 109.8 6_565 . ? H15A C15 H15B 108.3 . . ? C17 C16 C17 122.6(4) 6_565 . ? C17 C16 O2 118.6(2) 6_565 . ? C17 C16 O2 118.6(2) . . ? C18 C17 C16 116.3(3) . . ? C18 C17 C28 118.5(3) . . ? C16 C17 C28 125.1(3) . . ? C19 C18 C17 123.1(4) . . ? C19 C18 H18 118.4 . . ? C17 C18 H18 118.4 . . ? C18 C19 C18 118.4(5) 6_565 . ? C18 C19 C32 120.8(2) 6_565 . ? C18 C19 C32 120.8(2) . . ? C23 C20 C22 108.5(5) . . ? C23 C20 C4 110.6(4) . . ? C22 C20 C4 113.8(4) . . ? C23 C20 C21 107.3(5) . . ? C22 C20 C21 108.3(5) . . ? C4 C20 C21 108.0(4) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C27 C24 C25 108.8(5) . . ? C27 C24 C26 106.0(4) . . ? C25 C24 C26 109.3(5) . . ? C27 C24 C11 112.7(4) . . ? C25 C24 C11 109.2(4) . . ? C26 C24 C11 110.8(4) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C30 C28 C31 112.3(3) . . ? C30 C28 C17 110.0(3) . . ? C31 C28 C17 110.3(3) . . ? C30 C28 C29 107.0(3) . . ? C31 C28 C29 105.6(3) . . ? C17 C28 C29 111.6(3) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C19 C32 H32A 106(3) . . ? C19 C32 H32B 113(2) . . ? H32A C32 H32B 140(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 O1 P1 O1 C7 -23.6(5) 6_565 . . . ? O2 P1 O1 C7 81.4(4) . . . . ? O1 P1 O2 C16 126.06(10) . . . . ? O1 P1 O2 C16 -126.06(10) 6_565 . . . ? C2 C1 C2 C3 -92.1(4) 6_565 . . . ? C2 C1 C2 C7 82.6(4) 6_565 . . . ? C7 C2 C3 C4 -0.9(5) . . . . ? C1 C2 C3 C4 174.1(3) . . . . ? C2 C3 C4 C5 1.9(6) . . . . ? C2 C3 C4 C20 -176.2(4) . . . . ? C3 C4 C5 C6 -1.3(6) . . . . ? C20 C4 C5 C6 176.7(4) . . . . ? C4 C5 C6 C7 -0.2(5) . . . . ? C4 C5 C6 C8 -179.3(3) . . . . ? P1 O1 C7 C6 152.5(3) . . . . ? P1 O1 C7 C2 -30.1(5) . . . . ? C5 C6 C7 O1 178.7(3) . . . . ? C8 C6 C7 O1 -2.3(5) . . . . ? C5 C6 C7 C2 1.3(5) . . . . ? C8 C6 C7 C2 -179.7(3) . . . . ? C3 C2 C7 O1 -178.0(3) . . . . ? C1 C2 C7 O1 7.3(5) . . . . ? C3 C2 C7 C6 -0.8(5) . . . . ? C1 C2 C7 C6 -175.5(3) . . . . ? C7 C6 C8 C9 -95.9(4) . . . . ? C5 C6 C8 C9 83.1(4) . . . . ? C6 C8 C9 C10 -80.5(4) . . . . ? C6 C8 C9 C14 96.7(4) . . . . ? C14 C9 C10 C11 0.2(5) . . . . ? C8 C9 C10 C11 177.4(3) . . . . ? C9 C10 C11 C12 -1.8(5) . . . . ? C9 C10 C11 C24 177.9(3) . . . . ? C10 C11 C12 C13 0.6(5) . . . . ? C24 C11 C12 C13 -179.0(3) . . . . ? C11 C12 C13 C14 2.1(5) . . . . ? C11 C12 C13 C15 -174.8(3) . . . . ? C12 C13 C14 O3 176.0(3) . . . . ? C15 C13 C14 O3 -7.1(5) . . . . ? C12 C13 C14 C9 -3.8(5) . . . . ? C15 C13 C14 C9 173.1(3) . . . . ? C10 C9 C14 O3 -177.1(3) . . . . ? C8 C9 C14 O3 5.7(5) . . . . ? C10 C9 C14 C13 2.7(5) . . . . ? C8 C9 C14 C13 -174.5(3) . . . . ? C12 C13 C15 C13 87.4(5) . . . 6_565 ? C14 C13 C15 C13 -89.5(5) . . . 6_565 ? P1 O2 C16 C17 -92.3(3) . . . 6_565 ? P1 O2 C16 C17 92.3(3) . . . . ? C17 C16 C17 C18 4.5(6) 6_565 . . . ? O2 C16 C17 C18 179.7(3) . . . . ? C17 C16 C17 C28 -177.7(3) 6_565 . . . ? O2 C16 C17 C28 -2.5(5) . . . . ? C16 C17 C18 C19 -1.3(6) . . . . ? C28 C17 C18 C19 -179.2(4) . . . . ? C17 C18 C19 C18 -1.7(8) . . . 6_565 ? C17 C18 C19 C32 178.5(5) . . . . ? C5 C4 C20 C23 126.0(5) . . . . ? C3 C4 C20 C23 -56.0(6) . . . . ? C5 C4 C20 C22 3.5(7) . . . . ? C3 C4 C20 C22 -178.5(4) . . . . ? C5 C4 C20 C21 -116.8(5) . . . . ? C3 C4 C20 C21 61.1(5) . . . . ? C12 C11 C24 C27 -170.4(4) . . . . ? C10 C11 C24 C27 10.0(6) . . . . ? C12 C11 C24 C25 68.6(5) . . . . ? C10 C11 C24 C25 -111.0(5) . . . . ? C12 C11 C24 C26 -51.8(5) . . . . ? C10 C11 C24 C26 128.6(5) . . . . ? C18 C17 C28 C30 102.8(4) . . . . ? C16 C17 C28 C30 -75.0(4) . . . . ? C18 C17 C28 C31 -132.9(4) . . . . ? C16 C17 C28 C31 49.4(5) . . . . ? C18 C17 C28 C29 -15.8(5) . . . . ? C16 C17 C28 C29 166.4(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.253 _refine_diff_density_min -0.478 _refine_diff_density_rms 0.114 data_pat22n_m _database_code_depnum_ccdc_archive 'CCDC 695457' #TrackingRef 'NJC.CIF-27-1-10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 5,11,17,23-tetra-(tert-butyl)calix[4]arene 25,26-(dihydroxy){27,28-(2,6-di-isopropyl-phenyl)} monophosphite ; _chemical_name_common ; 5,11,17,23-tetra-(tert-butyl)calix(4)arene 25,26- (dihydroxy)(27,28-(2,6-di-isopropyl-phenyl)) monophosphite ; _chemical_melting_point ? _chemical_formula_moiety 'C56 H71 O5 P' _chemical_formula_sum 'C56 H71 O5 P' _chemical_formula_weight 855.10 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 MONOCLINIC _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.280(5) _cell_length_b 27.784(5) _cell_length_c 17.984(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 91.060(5) _cell_angle_gamma 90.000(5) _cell_volume 5136(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 356 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 27.00 _exptl_crystal_description RECTANGULAR _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.106 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 0.098 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.9636 _exptl_absorpt_correction_T_max 0.9730 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEX CCD' _diffrn_measurement_method OMEGA _diffrn_detector_area_resol_mean 0.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36813 _diffrn_reflns_av_R_equivalents 0.1786 _diffrn_reflns_av_sigmaI/netI 0.1840 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9034 _reflns_number_gt 3663 _reflns_threshold_expression >2\s(I) _computing_data_collection 'BRUKER SMART APEX CCD' _computing_cell_refinement 'BRUKER SMART APEX CCD' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP-III _computing_publication_material 'WINGX V1.80.01' _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^ > 2\s(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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1909P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9034 _refine_ls_number_parameters 583 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2505 _refine_ls_R_factor_gt 0.1108 _refine_ls_wR_factor_ref 0.3289 _refine_ls_wR_factor_gt 0.2604 _refine_ls_goodness_of_fit_ref 0.877 _refine_ls_restrained_S_all 0.877 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.009 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.05294(13) 0.16905(5) 0.70639(8) 0.0371(4) Uani 1 1 d . . . O1 O -0.0647(3) 0.14078(12) 0.7500(2) 0.0435(10) Uani 1 1 d . . . O2 O 0.1752(3) 0.13422(12) 0.72199(19) 0.0397(9) Uani 1 1 d . . . O3 O 0.0819(3) 0.21153(12) 0.76780(19) 0.0414(10) Uani 1 1 d . . . O4 O 0.2634(4) 0.15470(14) 0.5538(2) 0.0538(12) Uani 1 1 d . . . O5 O -0.0166(4) 0.03331(14) 0.5843(2) 0.0553(12) Uani 1 1 d . . . H5A H 0.062(6) 0.028(3) 0.578(4) 0.10(3) Uiso 1 1 d . . . H4A H 0.185(6) 0.157(2) 0.544(4) 0.10(3) Uiso 1 1 d . . . C1 C -0.0600(5) 0.0926(2) 0.7704(3) 0.0402(15) Uani 1 1 d . . . C2 C -0.1314(5) 0.0591(2) 0.7292(3) 0.0417(16) Uani 1 1 d . . . C3 C -0.1264(5) 0.0115(2) 0.7528(4) 0.0479(17) Uani 1 1 d . . . H3 H -0.1744 -0.0112 0.7260 0.057 Uiso 1 1 calc R . . C4 C -0.0530(5) -0.0041(2) 0.8147(4) 0.0461(17) Uani 1 1 d . . . C5 C 0.0160(5) 0.0307(2) 0.8532(3) 0.0475(17) Uani 1 1 d . . . H5 H 0.0651 0.0215 0.8947 0.057 Uiso 1 1 calc R . . C6 C 0.0157(5) 0.0788(2) 0.8331(3) 0.0401(15) Uani 1 1 d . . . C7 C 0.0952(5) 0.1157(2) 0.8767(3) 0.0470(17) Uani 1 1 d . . . H7A H 0.0555 0.1471 0.8706 0.056 Uiso 1 1 calc R . . H7B H 0.0935 0.1075 0.9292 0.056 Uiso 1 1 calc R . . C8 C 0.2355(5) 0.11810(19) 0.8523(3) 0.0355(14) Uani 1 1 d . . . C9 C 0.3373(6) 0.1088(2) 0.9031(3) 0.0453(16) Uani 1 1 d . . . H9 H 0.3165 0.1026 0.9523 0.054 Uiso 1 1 calc R . . C10 C 0.4684(6) 0.1085(2) 0.8839(3) 0.0443(16) Uani 1 1 d . . . C11 C 0.4954(5) 0.1193(2) 0.8105(3) 0.0430(16) Uani 1 1 d . . . H11 H 0.5818 0.1203 0.7962 0.052 Uiso 1 1 calc R . . C12 C 0.3991(5) 0.12877(19) 0.7575(3) 0.0356(14) Uani 1 1 d . . . C13 C 0.2692(5) 0.12802(19) 0.7794(3) 0.0365(14) Uani 1 1 d . . . C14 C 0.4314(5) 0.1375(2) 0.6766(3) 0.0415(16) Uani 1 1 d . . . H14A H 0.3927 0.1677 0.6604 0.050 Uiso 1 1 calc R . . H14B H 0.5250 0.1403 0.6720 0.050 Uiso 1 1 calc R . . C15 C 0.3821(5) 0.0973(2) 0.6267(3) 0.0369(15) Uani 1 1 d . . . C16 C 0.2943(5) 0.1073(2) 0.5678(3) 0.0410(15) Uani 1 1 d . . . C17 C 0.2397(5) 0.0703(2) 0.5254(3) 0.0448(16) Uani 1 1 d . . . C18 C 0.2765(5) 0.0234(2) 0.5412(3) 0.0469(17) Uani 1 1 d . . . H18 H 0.2403 -0.0013 0.5127 0.056 Uiso 1 1 calc R . . C19 C 0.3665(5) 0.0113(2) 0.5985(4) 0.0481(17) Uani 1 1 d . . . C20 C 0.4156(5) 0.0495(2) 0.6398(3) 0.0403(15) Uani 1 1 d . . . H20 H 0.4742 0.0428 0.6784 0.048 Uiso 1 1 calc R . . C21 C 0.1308(6) 0.0810(2) 0.4679(3) 0.0532(18) Uani 1 1 d . . . H21A H 0.1628 0.1030 0.4306 0.064 Uiso 1 1 calc R . . H21B H 0.1049 0.0514 0.4432 0.064 Uiso 1 1 calc R . . C22 C 0.0133(6) 0.1032(2) 0.5057(3) 0.0467(17) Uani 1 1 d . . . C23 C -0.0326(6) 0.1484(2) 0.4852(4) 0.0536(18) Uani 1 1 d . . . H23 H 0.0075 0.1645 0.4464 0.064 Uiso 1 1 calc R . . C24 C -0.1365(6) 0.1708(2) 0.5205(3) 0.0500(17) Uani 1 1 d . . . C25 C -0.1924(6) 0.1457(2) 0.5783(4) 0.0516(18) Uani 1 1 d . . . H25 H -0.2608 0.1600 0.6031 0.062 Uiso 1 1 calc R . . C26 C -0.1525(5) 0.1009(2) 0.6007(3) 0.0445(17) Uani 1 1 d . . . C27 C -0.0500(6) 0.0793(2) 0.5630(3) 0.0457(17) Uani 1 1 d . . . C28 C -0.2165(5) 0.0739(2) 0.6632(3) 0.0492(17) Uani 1 1 d . . . H28A H -0.2558 0.0451 0.6424 0.059 Uiso 1 1 calc R . . H28B H -0.2865 0.0938 0.6817 0.059 Uiso 1 1 calc R . . C29 C 0.0498(6) 0.2593(2) 0.7465(3) 0.0434(16) Uani 1 1 d . . . C30 C 0.1354(6) 0.2846(2) 0.7010(3) 0.0478(17) Uani 1 1 d . . . C31 C 0.1026(7) 0.3315(2) 0.6817(4) 0.067(2) Uani 1 1 d . . . H31 H 0.1580 0.3494 0.6522 0.081 Uiso 1 1 calc R . . C32 C -0.0116(8) 0.3518(2) 0.7059(4) 0.073(2) Uani 1 1 d . . . H32 H -0.0331 0.3830 0.6919 0.088 Uiso 1 1 calc R . . C33 C -0.0930(7) 0.3266(3) 0.7501(4) 0.070(2) Uani 1 1 d . . . H33 H -0.1694 0.3411 0.7657 0.084 Uiso 1 1 calc R . . C34 C -0.0651(6) 0.2790(2) 0.7730(3) 0.0491(17) Uani 1 1 d . . . C35 C -0.0549(7) -0.0571(2) 0.8388(4) 0.064(2) Uani 1 1 d . . . C36 C -0.1759(10) -0.0670(3) 0.8798(6) 0.183(5) Uani 1 1 d . . . H36A H -0.1840 -0.1011 0.8878 0.275 Uiso 1 1 calc R . . H36B H -0.2496 -0.0557 0.8513 0.275 Uiso 1 1 calc R . . H36C H -0.1724 -0.0508 0.9269 0.275 Uiso 1 1 calc R . . C37 C 0.0575(11) -0.0705(3) 0.8874(8) 0.183(6) Uani 1 1 d . . . H37A H 0.0627 -0.0488 0.9290 0.275 Uiso 1 1 calc R . . H37B H 0.1362 -0.0684 0.8597 0.275 Uiso 1 1 calc R . . H37C H 0.0464 -0.1028 0.9051 0.275 Uiso 1 1 calc R . . C38 C -0.0556(13) -0.0906(3) 0.7714(6) 0.154(5) Uani 1 1 d . . . H38A H 0.0252 -0.0875 0.7459 0.230 Uiso 1 1 calc R . . H38B H -0.1262 -0.0820 0.7383 0.230 Uiso 1 1 calc R . . H38C H -0.0661 -0.1232 0.7877 0.230 Uiso 1 1 calc R . . C39 C 0.5793(6) 0.0947(3) 0.9391(4) 0.059(2) Uani 1 1 d . . . C40 C 0.5306(8) 0.0898(4) 1.0168(4) 0.102(3) Uani 1 1 d . . . H40A H 0.4905 0.1193 1.0317 0.153 Uiso 1 1 calc R . . H40B H 0.6022 0.0826 1.0500 0.153 Uiso 1 1 calc R . . H40C H 0.4680 0.0642 1.0185 0.153 Uiso 1 1 calc R . . C41 C 0.6393(9) 0.0478(3) 0.9135(5) 0.103(3) Uani 1 1 d . . . H41A H 0.7110 0.0395 0.9460 0.154 Uiso 1 1 calc R . . H41B H 0.6698 0.0514 0.8637 0.154 Uiso 1 1 calc R . . H41C H 0.5751 0.0227 0.9147 0.154 Uiso 1 1 calc R . . C42 C 0.6859(8) 0.1336(3) 0.9378(5) 0.100(3) Uani 1 1 d . . . H42A H 0.6520 0.1632 0.9571 0.151 Uiso 1 1 calc R . . H42B H 0.7132 0.1385 0.8876 0.151 Uiso 1 1 calc R . . H42C H 0.7588 0.1235 0.9680 0.151 Uiso 1 1 calc R . . C43 C 0.3987(6) -0.0412(2) 0.6175(4) 0.0547(19) Uani 1 1 d . . . C44 C 0.3003(9) -0.0595(3) 0.6704(6) 0.141(4) Uani 1 1 d . . . H44A H 0.3104 -0.0431 0.7171 0.212 Uiso 1 1 calc R . . H44B H 0.3128 -0.0934 0.6778 0.212 Uiso 1 1 calc R . . H44C H 0.2145 -0.0538 0.6503 0.212 Uiso 1 1 calc R . . C45 C 0.5370(7) -0.0451(2) 0.6521(5) 0.081(3) Uani 1 1 d . . . H45A H 0.5375 -0.0318 0.7013 0.121 Uiso 1 1 calc R . . H45B H 0.5970 -0.0277 0.6220 0.121 Uiso 1 1 calc R . . H45C H 0.5623 -0.0784 0.6545 0.121 Uiso 1 1 calc R . . C46 C 0.3990(9) -0.0733(3) 0.5479(5) 0.101(3) Uani 1 1 d . . . H46A H 0.4292 -0.1049 0.5612 0.152 Uiso 1 1 calc R . . H46B H 0.4556 -0.0596 0.5116 0.152 Uiso 1 1 calc R . . H46C H 0.3123 -0.0754 0.5273 0.152 Uiso 1 1 calc R . . C47 C -0.1851(7) 0.2212(3) 0.4959(4) 0.068(2) Uani 1 1 d . . . C48 C -0.0791(9) 0.2522(3) 0.4687(6) 0.171(4) Uani 1 1 d . . . H48A H -0.1155 0.2780 0.4394 0.256 Uiso 1 1 calc R . . H48B H -0.0216 0.2335 0.4388 0.256 Uiso 1 1 calc R . . H48C H -0.0314 0.2654 0.5104 0.256 Uiso 1 1 calc R . . C49 C -0.2847(13) 0.2160(4) 0.4354(8) 0.219(7) Uani 1 1 d . . . H49A H -0.2889 0.1830 0.4197 0.328 Uiso 1 1 calc R . . H49B H -0.2615 0.2359 0.3940 0.328 Uiso 1 1 calc R . . H49C H -0.3680 0.2258 0.4533 0.328 Uiso 1 1 calc R . . C50 C -0.2449(9) 0.2476(3) 0.5573(6) 0.193(4) Uani 1 1 d . . . H50A H -0.1917 0.2443 0.6014 0.290 Uiso 1 1 calc R . . H50B H -0.3299 0.2347 0.5661 0.290 Uiso 1 1 calc R . . H50C H -0.2523 0.2810 0.5444 0.290 Uiso 1 1 calc R . . C51 C 0.2617(6) 0.2621(3) 0.6743(4) 0.0589(19) Uani 1 1 d . . . H51 H 0.2453 0.2274 0.6711 0.071 Uiso 1 1 calc R . . C52 C 0.3700(8) 0.2683(4) 0.7308(5) 0.128(4) Uani 1 1 d . . . H52A H 0.4491 0.2553 0.7114 0.193 Uiso 1 1 calc R . . H52B H 0.3485 0.2516 0.7756 0.193 Uiso 1 1 calc R . . H52C H 0.3817 0.3019 0.7414 0.193 Uiso 1 1 calc R . . C53 C 0.3028(9) 0.2772(3) 0.5986(5) 0.104(3) Uani 1 1 d . . . H53A H 0.3361 0.3094 0.6007 0.156 Uiso 1 1 calc R . . H53B H 0.2293 0.2760 0.5649 0.156 Uiso 1 1 calc R . . H53C H 0.3693 0.2558 0.5815 0.156 Uiso 1 1 calc R . . C54 C -0.1563(6) 0.2518(3) 0.8218(4) 0.061(2) Uani 1 1 d . . . H54 H -0.1143 0.2212 0.8352 0.073 Uiso 1 1 calc R . . C55 C -0.2828(8) 0.2402(4) 0.7820(5) 0.113(3) Uani 1 1 d . . . H55A H -0.3244 0.2695 0.7664 0.169 Uiso 1 1 calc R . . H55B H -0.3386 0.2230 0.8150 0.169 Uiso 1 1 calc R . . H55C H -0.2658 0.2206 0.7393 0.169 Uiso 1 1 calc R . . C56 C -0.1829(11) 0.2789(4) 0.8940(5) 0.134(4) Uani 1 1 d . . . H56A H -0.1018 0.2874 0.9179 0.201 Uiso 1 1 calc R . . H56B H -0.2322 0.2588 0.9265 0.201 Uiso 1 1 calc R . . H56C H -0.2313 0.3077 0.8829 0.201 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0353(7) 0.0367(8) 0.0393(8) 0.0032(7) 0.0008(6) -0.0004(6) O1 0.0338(19) 0.033(2) 0.063(3) 0.0034(19) 0.0069(18) 0.0038(16) O2 0.0346(19) 0.041(2) 0.043(2) -0.0035(18) -0.0021(17) 0.0018(16) O3 0.048(2) 0.036(2) 0.040(2) -0.0001(18) -0.0037(18) -0.0017(17) O4 0.059(3) 0.048(3) 0.054(3) 0.000(2) -0.003(2) 0.008(2) O5 0.042(2) 0.047(3) 0.076(3) 0.006(2) 0.006(2) 0.003(2) C1 0.030(3) 0.036(3) 0.055(4) 0.001(3) 0.010(3) -0.005(3) C2 0.030(3) 0.044(4) 0.051(4) 0.006(3) 0.006(3) -0.004(3) C3 0.033(3) 0.043(4) 0.068(5) 0.003(3) 0.007(3) -0.011(3) C4 0.036(3) 0.039(4) 0.064(4) 0.012(3) 0.012(3) -0.006(3) C5 0.037(3) 0.052(4) 0.054(4) 0.015(3) 0.007(3) -0.002(3) C6 0.032(3) 0.047(4) 0.042(4) 0.009(3) 0.006(3) -0.007(3) C7 0.043(3) 0.057(4) 0.040(4) 0.009(3) 0.002(3) -0.003(3) C8 0.039(3) 0.034(3) 0.034(3) -0.009(3) 0.002(3) 0.001(3) C9 0.058(4) 0.042(4) 0.036(4) -0.006(3) -0.002(3) -0.007(3) C10 0.047(4) 0.036(4) 0.050(4) -0.015(3) -0.003(3) -0.003(3) C11 0.032(3) 0.052(4) 0.044(4) -0.003(3) -0.007(3) -0.002(3) C12 0.030(3) 0.036(3) 0.041(4) -0.003(3) 0.006(3) -0.003(2) C13 0.041(3) 0.028(3) 0.041(4) -0.004(3) 0.004(3) 0.000(3) C14 0.020(3) 0.050(4) 0.054(4) 0.006(3) -0.003(3) 0.001(3) C15 0.021(3) 0.055(4) 0.035(3) -0.003(3) 0.003(2) 0.001(3) C16 0.045(3) 0.038(4) 0.040(4) 0.001(3) 0.004(3) 0.011(3) C17 0.044(3) 0.054(4) 0.036(4) -0.001(3) 0.000(3) 0.008(3) C18 0.038(3) 0.053(4) 0.050(4) -0.011(3) 0.004(3) 0.002(3) C19 0.033(3) 0.051(4) 0.061(4) -0.005(3) 0.007(3) -0.002(3) C20 0.041(3) 0.036(4) 0.044(4) 0.000(3) -0.001(3) 0.002(3) C21 0.053(4) 0.055(4) 0.052(4) -0.006(3) 0.001(3) 0.002(3) C22 0.046(4) 0.046(4) 0.047(4) 0.001(3) -0.012(3) -0.003(3) C23 0.053(4) 0.065(5) 0.043(4) 0.011(3) -0.007(3) -0.001(3) C24 0.045(3) 0.063(4) 0.042(4) 0.004(3) -0.016(3) 0.003(3) C25 0.040(3) 0.055(4) 0.059(4) -0.003(4) -0.002(3) 0.004(3) C26 0.036(3) 0.053(4) 0.044(4) 0.010(3) -0.005(3) -0.010(3) C27 0.046(3) 0.039(4) 0.052(4) 0.002(3) -0.011(3) 0.001(3) C28 0.033(3) 0.048(4) 0.066(4) 0.001(3) -0.005(3) 0.000(3) C29 0.051(4) 0.036(4) 0.043(4) -0.007(3) -0.005(3) 0.007(3) C30 0.051(4) 0.042(4) 0.050(4) -0.002(3) -0.004(3) -0.011(3) C31 0.089(5) 0.037(4) 0.075(5) 0.009(4) 0.007(4) 0.000(4) C32 0.105(6) 0.033(4) 0.083(6) 0.005(4) 0.018(5) 0.016(4) C33 0.076(5) 0.054(5) 0.081(5) -0.006(4) 0.013(4) 0.023(4) C34 0.047(4) 0.053(4) 0.047(4) -0.005(3) 0.003(3) 0.006(3) C35 0.069(5) 0.038(4) 0.084(5) 0.009(4) 0.009(4) -0.001(3) C36 0.185(8) 0.086(6) 0.284(10) 0.121(7) 0.153(8) 0.027(6) C37 0.188(10) 0.053(6) 0.304(15) 0.052(8) -0.143(11) -0.013(6) C38 0.266(14) 0.040(6) 0.154(10) 0.008(6) 0.003(10) 0.007(7) C39 0.055(4) 0.082(5) 0.040(4) -0.003(4) -0.007(3) 0.005(4) C40 0.088(6) 0.164(9) 0.053(5) 0.010(5) -0.029(4) 0.024(6) C41 0.113(7) 0.097(7) 0.099(7) -0.008(5) -0.021(6) 0.049(5) C42 0.078(5) 0.109(7) 0.113(7) 0.010(6) -0.047(5) -0.021(5) C43 0.054(4) 0.036(4) 0.073(5) 0.002(3) -0.007(4) -0.005(3) C44 0.111(7) 0.101(7) 0.214(11) 0.085(8) 0.075(7) 0.021(6) C45 0.083(5) 0.045(5) 0.113(7) 0.008(4) -0.024(5) 0.019(4) C46 0.141(8) 0.057(5) 0.104(7) -0.025(5) -0.033(6) 0.027(5) C47 0.065(4) 0.063(5) 0.076(5) 0.017(4) -0.004(4) 0.020(4) C48 0.119(7) 0.083(6) 0.310(11) 0.098(7) -0.006(8) -0.011(6) C49 0.282(14) 0.098(8) 0.269(14) 0.059(9) -0.204(12) 0.008(9) C50 0.254(6) 0.139(6) 0.191(9) 0.069(6) 0.112(7) 0.178(5) C51 0.051(4) 0.057(5) 0.068(5) 0.003(4) 0.001(4) -0.006(3) C52 0.062(5) 0.200(12) 0.123(8) -0.045(8) -0.010(6) 0.010(6) C53 0.120(7) 0.113(8) 0.081(6) 0.010(6) 0.024(6) 0.037(6) C54 0.055(4) 0.062(5) 0.065(5) -0.006(4) 0.005(4) 0.014(3) C55 0.072(6) 0.148(9) 0.119(8) 0.041(7) -0.010(5) -0.033(6) C56 0.163(10) 0.155(10) 0.086(7) -0.024(7) 0.053(7) -0.038(8) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O2 1.607(3) . ? P1 O3 1.640(4) . ? P1 O1 1.652(4) . ? O1 C1 1.390(6) . ? O2 C13 1.412(6) . ? O3 C29 1.420(6) . ? O4 C16 1.378(6) . ? O4 H4A 0.82(6) . ? O5 C27 1.375(6) . ? O5 H5A 0.83(7) . ? C1 C2 1.389(8) . ? C1 C6 1.411(8) . ? C2 C3 1.390(8) . ? C2 C28 1.517(8) . ? C3 C4 1.403(8) . ? C3 H3 0.9300 . ? C4 C5 1.379(8) . ? C4 C35 1.535(9) . ? C5 C6 1.385(8) . ? C5 H5 0.9300 . ? C6 C7 1.518(8) . ? C7 C8 1.517(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C13 1.389(8) . ? C8 C9 1.400(8) . ? C9 C10 1.397(8) . ? C9 H9 0.9300 . ? C10 C11 1.388(8) . ? C10 C39 1.546(8) . ? C11 C12 1.386(7) . ? C11 H11 0.9300 . ? C12 C13 1.400(7) . ? C12 C14 1.518(8) . ? C14 C15 1.515(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C20 1.390(8) . ? C15 C16 1.406(7) . ? C16 C17 1.390(8) . ? C17 C18 1.387(8) . ? C17 C21 1.538(8) . ? C18 C19 1.413(8) . ? C18 H18 0.9300 . ? C19 C20 1.384(8) . ? C19 C43 1.533(8) . ? C20 H20 0.9300 . ? C21 C22 1.528(8) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.389(8) . ? C22 C27 1.397(8) . ? C23 C24 1.398(9) . ? C23 H23 0.9300 . ? C24 C25 1.385(9) . ? C24 C47 1.549(9) . ? C25 C26 1.368(8) . ? C25 H25 0.9300 . ? C26 C27 1.399(8) . ? C26 C28 1.512(8) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C34 1.393(8) . ? C29 C30 1.402(8) . ? C30 C31 1.387(9) . ? C30 C51 1.526(8) . ? C31 C32 1.380(10) . ? C31 H31 0.9300 . ? C32 C33 1.359(10) . ? C32 H32 0.9300 . ? C33 C34 1.412(9) . ? C33 H33 0.9300 . ? C34 C54 1.501(9) . ? C35 C37 1.484(11) . ? C35 C36 1.484(10) . ? C35 C38 1.527(11) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C40 1.499(10) . ? C39 C41 1.518(10) . ? C39 C42 1.540(10) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 C44 1.490(10) . ? C43 C46 1.538(10) . ? C43 C45 1.545(9) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 C50 1.470(10) . ? C47 C48 1.480(10) . ? C47 C49 1.487(12) . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 C53 1.493(10) . ? C51 C52 1.504(10) . ? C51 H51 0.9800 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 C55 1.507(10) . ? C54 C56 1.531(11) . ? C54 H54 0.9800 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? 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 O2 P1 O3 100.61(18) . . ? O2 P1 O1 102.00(19) . . ? O3 P1 O1 98.52(19) . . ? C1 O1 P1 124.2(2) . . ? C13 O2 P1 136.4(2) . . ? C29 O3 P1 117.0(2) . . ? C16 O4 H4A 111(5) . . ? C27 O5 H5A 112(5) . . ? C2 C1 O1 119.2(5) . . ? C2 C1 C6 121.6(5) . . ? O1 C1 C6 119.2(5) . . ? C1 C2 C3 117.2(5) . . ? C1 C2 C28 121.8(5) . . ? C3 C2 C28 120.9(5) . . ? C2 C3 C4 123.6(6) . . ? C2 C3 H3 118.2 . . ? C4 C3 H3 118.2 . . ? C5 C4 C3 116.5(5) . . ? C5 C4 C35 122.7(6) . . ? C3 C4 C35 120.7(6) . . ? C4 C5 C6 123.2(6) . . ? C4 C5 H5 118.4 . . ? C6 C5 H5 118.4 . . ? C5 C6 C1 117.9(5) . . ? C5 C6 C7 121.1(5) . . ? C1 C6 C7 121.0(5) . . ? C8 C7 C6 112.7(5) . . ? C8 C7 H7A 109.1 . . ? C6 C7 H7A 109.1 . . ? C8 C7 H7B 109.1 . . ? C6 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? C13 C8 C9 117.1(5) . . ? C13 C8 C7 122.5(5) . . ? C9 C8 C7 120.4(5) . . ? C10 C9 C8 123.6(6) . . ? C10 C9 H9 118.2 . . ? C8 C9 H9 118.2 . . ? C11 C10 C9 116.4(5) . . ? C11 C10 C39 120.4(5) . . ? C9 C10 C39 123.1(6) . . ? C12 C11 C10 122.8(5) . . ? C12 C11 H11 118.6 . . ? C10 C11 H11 118.6 . . ? C11 C12 C13 118.4(5) . . ? C11 C12 C14 121.5(5) . . ? C13 C12 C14 120.0(5) . . ? C8 C13 C12 121.7(5) . . ? C8 C13 O2 122.4(5) . . ? C12 C13 O2 115.8(5) . . ? C15 C14 C12 111.9(5) . . ? C15 C14 H14A 109.2 . . ? C12 C14 H14A 109.2 . . ? C15 C14 H14B 109.2 . . ? C12 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C20 C15 C16 118.0(5) . . ? C20 C15 C14 121.7(5) . . ? C16 C15 C14 120.3(5) . . ? O4 C16 C17 121.1(5) . . ? O4 C16 C15 117.9(5) . . ? C17 C16 C15 121.0(5) . . ? C18 C17 C16 118.4(5) . . ? C18 C17 C21 120.8(5) . . ? C16 C17 C21 120.6(5) . . ? C17 C18 C19 123.0(6) . . ? C17 C18 H18 118.5 . . ? C19 C18 H18 118.5 . . ? C20 C19 C18 115.9(6) . . ? C20 C19 C43 122.4(5) . . ? C18 C19 C43 121.5(5) . . ? C19 C20 C15 123.7(5) . . ? C19 C20 H20 118.2 . . ? C15 C20 H20 118.2 . . ? C22 C21 C17 110.5(5) . . ? C22 C21 H21A 109.5 . . ? C17 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? C17 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? C23 C22 C27 117.8(6) . . ? C23 C22 C21 121.0(6) . . ? C27 C22 C21 121.2(6) . . ? C22 C23 C24 122.6(6) . . ? C22 C23 H23 118.7 . . ? C24 C23 H23 118.7 . . ? C25 C24 C23 116.7(6) . . ? C25 C24 C47 122.2(6) . . ? C23 C24 C47 121.1(6) . . ? C26 C25 C24 123.5(6) . . ? C26 C25 H25 118.2 . . ? C24 C25 H25 118.2 . . ? C25 C26 C27 118.2(6) . . ? C25 C26 C28 122.6(6) . . ? C27 C26 C28 119.3(6) . . ? O5 C27 C22 122.0(5) . . ? O5 C27 C26 116.8(5) . . ? C22 C27 C26 121.2(6) . . ? C26 C28 C2 117.5(5) . . ? C26 C28 H28A 107.9 . . ? C2 C28 H28A 107.9 . . ? C26 C28 H28B 107.9 . . ? C2 C28 H28B 107.9 . . ? H28A C28 H28B 107.2 . . ? C34 C29 C30 123.3(6) . . ? C34 C29 O3 118.0(5) . . ? C30 C29 O3 118.8(5) . . ? C31 C30 C29 117.6(6) . . ? C31 C30 C51 120.7(6) . . ? C29 C30 C51 121.7(6) . . ? C32 C31 C30 120.6(7) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C33 C32 C31 120.7(7) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C32 C33 C34 121.9(7) . . ? C32 C33 H33 119.0 . . ? C34 C33 H33 119.0 . . ? C29 C34 C33 115.9(6) . . ? C29 C34 C54 123.0(6) . . ? C33 C34 C54 121.1(6) . . ? C37 C35 C36 108.1(8) . . ? C37 C35 C38 107.9(8) . . ? C36 C35 C38 106.9(8) . . ? C37 C35 C4 113.1(6) . . ? C36 C35 C4 109.5(6) . . ? C38 C35 C4 111.1(6) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C41 110.4(7) . . ? C40 C39 C42 109.2(6) . . ? C41 C39 C42 107.8(7) . . ? C40 C39 C10 111.5(6) . . ? C41 C39 C10 108.4(6) . . ? C42 C39 C10 109.5(6) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 C19 108.7(6) . . ? C44 C43 C46 109.4(7) . . ? C19 C43 C46 112.1(6) . . ? C44 C43 C45 110.4(7) . . ? C19 C43 C45 110.5(5) . . ? C46 C43 C45 105.7(6) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C50 C47 C48 106.1(8) . . ? C50 C47 C49 107.8(8) . . ? C48 C47 C49 108.4(8) . . ? C50 C47 C24 112.0(6) . . ? C48 C47 C24 112.7(6) . . ? C49 C47 C24 109.6(7) . . ? 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 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C47 C50 H50A 109.5 . . ? C47 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C47 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C53 C51 C52 111.4(7) . . ? C53 C51 C30 115.4(6) . . ? C52 C51 C30 111.3(6) . . ? C53 C51 H51 106.0 . . ? C52 C51 H51 106.0 . . ? C30 C51 H51 106.0 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C34 C54 C55 111.9(6) . . ? C34 C54 C56 111.7(6) . . ? C55 C54 C56 110.0(7) . . ? C34 C54 H54 107.7 . . ? C55 C54 H54 107.7 . . ? C56 C54 H54 107.7 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? 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 O2 P1 O1 C1 -18.7(3) . . . . ? O3 P1 O1 C1 -121.5(3) . . . . ? O3 P1 O2 C13 16.2(4) . . . . ? O1 P1 O2 C13 -85.0(4) . . . . ? O2 P1 O3 C29 143.5(3) . . . . ? O1 P1 O3 C29 -112.5(3) . . . . ? P1 O1 C1 C2 -104.0(4) . . . . ? P1 O1 C1 C6 76.9(5) . . . . ? O1 C1 C2 C3 -178.4(4) . . . . ? C6 C1 C2 C3 0.8(8) . . . . ? O1 C1 C2 C28 -1.2(8) . . . . ? C6 C1 C2 C28 177.9(5) . . . . ? C1 C2 C3 C4 -0.7(9) . . . . ? C28 C2 C3 C4 -177.9(5) . . . . ? C2 C3 C4 C5 0.5(9) . . . . ? C2 C3 C4 C35 178.4(6) . . . . ? C3 C4 C5 C6 -0.4(8) . . . . ? C35 C4 C5 C6 -178.3(6) . . . . ? C4 C5 C6 C1 0.5(8) . . . . ? C4 C5 C6 C7 -179.0(5) . . . . ? C2 C1 C6 C5 -0.7(8) . . . . ? O1 C1 C6 C5 178.4(4) . . . . ? C2 C1 C6 C7 178.8(5) . . . . ? O1 C1 C6 C7 -2.0(7) . . . . ? C5 C6 C7 C8 84.4(7) . . . . ? C1 C6 C7 C8 -95.1(6) . . . . ? C6 C7 C8 C13 57.3(7) . . . . ? C6 C7 C8 C9 -120.8(6) . . . . ? C13 C8 C9 C10 -0.9(8) . . . . ? C7 C8 C9 C10 177.3(5) . . . . ? C8 C9 C10 C11 1.8(8) . . . . ? C8 C9 C10 C39 -175.6(6) . . . . ? C9 C10 C11 C12 -1.8(9) . . . . ? C39 C10 C11 C12 175.6(6) . . . . ? C10 C11 C12 C13 1.0(9) . . . . ? C10 C11 C12 C14 -176.2(5) . . . . ? C9 C8 C13 C12 0.0(8) . . . . ? C7 C8 C13 C12 -178.1(5) . . . . ? C9 C8 C13 O2 175.0(4) . . . . ? C7 C8 C13 O2 -3.2(8) . . . . ? C11 C12 C13 C8 -0.1(8) . . . . ? C14 C12 C13 C8 177.2(5) . . . . ? C11 C12 C13 O2 -175.3(4) . . . . ? C14 C12 C13 O2 2.0(7) . . . . ? P1 O2 C13 C8 57.8(6) . . . . ? P1 O2 C13 C12 -127.0(4) . . . . ? C11 C12 C14 C15 112.3(6) . . . . ? C13 C12 C14 C15 -64.9(7) . . . . ? C12 C14 C15 C20 -55.0(7) . . . . ? C12 C14 C15 C16 121.3(5) . . . . ? C20 C15 C16 O4 -178.6(4) . . . . ? C14 C15 C16 O4 4.9(7) . . . . ? C20 C15 C16 C17 1.9(8) . . . . ? C14 C15 C16 C17 -174.6(5) . . . . ? O4 C16 C17 C18 178.8(5) . . . . ? C15 C16 C17 C18 -1.7(8) . . . . ? O4 C16 C17 C21 -7.5(8) . . . . ? C15 C16 C17 C21 172.0(5) . . . . ? C16 C17 C18 C19 0.3(9) . . . . ? C21 C17 C18 C19 -173.5(5) . . . . ? C17 C18 C19 C20 1.0(8) . . . . ? C17 C18 C19 C43 176.3(6) . . . . ? C18 C19 C20 C15 -0.8(8) . . . . ? C43 C19 C20 C15 -176.0(5) . . . . ? C16 C15 C20 C19 -0.6(8) . . . . ? C14 C15 C20 C19 175.8(5) . . . . ? C18 C17 C21 C22 113.8(6) . . . . ? C16 C17 C21 C22 -59.8(7) . . . . ? C17 C21 C22 C23 120.8(6) . . . . ? C17 C21 C22 C27 -57.9(7) . . . . ? C27 C22 C23 C24 1.3(9) . . . . ? C21 C22 C23 C24 -177.4(5) . . . . ? C22 C23 C24 C25 0.5(9) . . . . ? C22 C23 C24 C47 -179.9(6) . . . . ? C23 C24 C25 C26 -1.1(9) . . . . ? C47 C24 C25 C26 179.3(6) . . . . ? C24 C25 C26 C27 -0.3(9) . . . . ? C24 C25 C26 C28 -179.0(6) . . . . ? C23 C22 C27 O5 176.1(5) . . . . ? C21 C22 C27 O5 -5.1(8) . . . . ? C23 C22 C27 C26 -2.8(9) . . . . ? C21 C22 C27 C26 176.0(5) . . . . ? C25 C26 C27 O5 -176.7(5) . . . . ? C28 C26 C27 O5 2.0(8) . . . . ? C25 C26 C27 C22 2.3(9) . . . . ? C28 C26 C27 C22 -179.0(5) . . . . ? C25 C26 C28 C2 -121.8(6) . . . . ? C27 C26 C28 C2 59.6(8) . . . . ? C1 C2 C28 C26 56.9(8) . . . . ? C3 C2 C28 C26 -126.1(6) . . . . ? P1 O3 C29 C34 101.4(5) . . . . ? P1 O3 C29 C30 -79.5(5) . . . . ? C34 C29 C30 C31 -0.1(9) . . . . ? O3 C29 C30 C31 -179.3(5) . . . . ? C34 C29 C30 C51 178.9(6) . . . . ? O3 C29 C30 C51 -0.2(8) . . . . ? C29 C30 C31 C32 -1.0(10) . . . . ? C51 C30 C31 C32 -180.0(6) . . . . ? C30 C31 C32 C33 1.1(11) . . . . ? C31 C32 C33 C34 0.0(12) . . . . ? C30 C29 C34 C33 1.1(9) . . . . ? O3 C29 C34 C33 -179.8(5) . . . . ? C30 C29 C34 C54 -179.9(6) . . . . ? O3 C29 C34 C54 -0.8(8) . . . . ? C32 C33 C34 C29 -1.0(10) . . . . ? C32 C33 C34 C54 180.0(7) . . . . ? C5 C4 C35 C37 -21.3(10) . . . . ? C3 C4 C35 C37 160.9(8) . . . . ? C5 C4 C35 C36 99.3(8) . . . . ? C3 C4 C35 C36 -78.5(9) . . . . ? C5 C4 C35 C38 -142.9(8) . . . . ? C3 C4 C35 C38 39.3(9) . . . . ? C11 C10 C39 C40 173.8(6) . . . . ? C9 C10 C39 C40 -9.0(9) . . . . ? C11 C10 C39 C41 -64.5(8) . . . . ? C9 C10 C39 C41 112.7(7) . . . . ? C11 C10 C39 C42 52.9(8) . . . . ? C9 C10 C39 C42 -129.9(7) . . . . ? C20 C19 C43 C44 89.5(8) . . . . ? C18 C19 C43 C44 -85.5(8) . . . . ? C20 C19 C43 C46 -149.4(6) . . . . ? C18 C19 C43 C46 35.6(8) . . . . ? C20 C19 C43 C45 -31.8(8) . . . . ? C18 C19 C43 C45 153.2(6) . . . . ? C25 C24 C47 C50 27.3(10) . . . . ? C23 C24 C47 C50 -152.3(7) . . . . ? C25 C24 C47 C48 146.8(7) . . . . ? C23 C24 C47 C48 -32.8(10) . . . . ? C25 C24 C47 C49 -92.3(10) . . . . ? C23 C24 C47 C49 88.1(10) . . . . ? C31 C30 C51 C53 -34.7(9) . . . . ? C29 C30 C51 C53 146.3(7) . . . . ? C31 C30 C51 C52 93.6(8) . . . . ? C29 C30 C51 C52 -85.4(8) . . . . ? C29 C34 C54 C55 -111.1(8) . . . . ? C33 C34 C54 C55 67.8(9) . . . . ? C29 C34 C54 C56 125.0(8) . . . . ? C33 C34 C54 C56 -56.0(9) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.622 _refine_diff_density_min -0.550 _refine_diff_density_rms 0.059 data_pat2_m _database_code_depnum_ccdc_archive 'CCDC 695459' #TrackingRef 'NJC.CIF-27-1-10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 5,11,17,23-tetra-(tert-butyl)calix[4]arene {25,26-(2,6-di-tert-butyl-4-methyl-phenyl) 27,28-(2,4-di-tert-butyl-phenyl)}diphosphite ; _chemical_name_common ; 5,11,17,23-tetra-(tert-butyl)calix(4)arene (25,26-(2,6-di- tert-butyl-4-methyl-phenyl) 27,28-(2,4-di-tert-butyl-phenyl))diphosphite ; _chemical_melting_point ? _chemical_formula_moiety 'C73 H96 O6 P2' _chemical_formula_sum 'C73 H96 O6 P2' _chemical_formula_weight 1131.44 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 13.6778(15) _cell_length_b 16.7394(18) _cell_length_c 19.432(2) _cell_angle_alpha 71.800(2) _cell_angle_beta 78.874(2) _cell_angle_gamma 77.135(2) _cell_volume 4083.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 368 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 27.00 _exptl_crystal_description RECTANGULAR _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.920 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.094 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.9564 _exptl_absorpt_correction_T_max 0.9688 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEX CCD' _diffrn_measurement_method OMEGA _diffrn_detector_area_resol_mean 0.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29696 _diffrn_reflns_av_R_equivalents 0.0602 _diffrn_reflns_av_sigmaI/netI 0.1163 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14290 _reflns_number_gt 5895 _reflns_threshold_expression >2\s(I) _computing_data_collection 'BRUKER SMART APEX CCD' _computing_cell_refinement 'BRUKER SMART APEX CCD' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP-III _computing_publication_material 'WINHX V1.80.01' _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^ > 2\s(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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 14290 _refine_ls_number_parameters 740 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.2291 _refine_ls_R_factor_gt 0.1151 _refine_ls_wR_factor_ref 0.3908 _refine_ls_wR_factor_gt 0.3161 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.006 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.25815(12) 0.82537(11) 0.27016(9) 0.0586(5) Uani 1 1 d . . . P2 P 0.00418(13) 0.82256(11) 0.35346(9) 0.0614(5) Uani 1 1 d . . . O1 O 0.2411(3) 0.8750(3) 0.1851(2) 0.0605(11) Uani 1 1 d . . . O2 O 0.2168(3) 0.9051(2) 0.30454(19) 0.0557(10) Uani 1 1 d . . . O3 O 0.3822(3) 0.8138(3) 0.2640(2) 0.0605(11) Uani 1 1 d . . . O4 O -0.0252(3) 0.8775(3) 0.4131(2) 0.0655(11) Uani 1 1 d . . . O5 O 0.0005(3) 0.8995(2) 0.27808(18) 0.0560(10) Uani 1 1 d . . . O6 O -0.1023(3) 0.7927(3) 0.3537(2) 0.0698(12) Uani 1 1 d . . . C1 C 0.2551(5) 1.0239(5) 0.1489(3) 0.0578(17) Uani 1 1 d . . . C2 C 0.3486(5) 1.0059(5) 0.1857(3) 0.0634(18) Uani 1 1 d . . . H2A H 0.3933 1.0455 0.1572 0.076 Uiso 1 1 calc R . . H2B H 0.3843 0.9485 0.1871 0.076 Uiso 1 1 calc R . . C3 C 0.3225(5) 1.0143(4) 0.2638(3) 0.0575(16) Uani 1 1 d . . . C4 C 0.3635(5) 1.0723(5) 0.2826(4) 0.0692(19) Uani 1 1 d . . . H4 H 0.4070 1.1042 0.2473 0.083 Uiso 1 1 calc R . . C5 C 0.3420(6) 1.0847(5) 0.3525(4) 0.076(2) Uani 1 1 d . . . C6 C 0.2698(6) 1.0411(5) 0.4004(4) 0.074(2) Uani 1 1 d . . . H6 H 0.2508 1.0501 0.4464 0.088 Uiso 1 1 calc R . . C7 C 0.2246(5) 0.9849(4) 0.3836(3) 0.0553(16) Uani 1 1 d . . . C8 C 0.1354(4) 0.9484(4) 0.4333(3) 0.0607(18) Uani 1 1 d . . . H8A H 0.1391 0.8901 0.4325 0.073 Uiso 1 1 calc R . . H8B H 0.1373 0.9477 0.4832 0.073 Uiso 1 1 calc R . . C9 C 0.0379(5) 1.0024(5) 0.4076(3) 0.0598(17) Uani 1 1 d . . . C10 C 0.0215(5) 1.0913(5) 0.3923(3) 0.0666(19) Uani 1 1 d . . . H10 H 0.0698 1.1163 0.4018 0.080 Uiso 1 1 calc R . . C11 C -0.0637(6) 1.1441(5) 0.3637(4) 0.0690(19) Uani 1 1 d . . . C12 C -0.1332(6) 1.1039(5) 0.3500(3) 0.073(2) Uani 1 1 d . . . H12 H -0.1901 1.1379 0.3297 0.087 Uiso 1 1 calc R . . C13 C -0.1231(5) 1.0180(5) 0.3644(3) 0.0608(18) Uani 1 1 d . . . C14 C -0.1984(5) 0.9784(5) 0.3440(3) 0.0673(19) Uani 1 1 d . . . H14A H -0.2654 1.0119 0.3506 0.081 Uiso 1 1 calc R . . H14B H -0.1994 0.9213 0.3767 0.081 Uiso 1 1 calc R . . C15 C -0.1744(5) 0.9733(4) 0.2659(3) 0.0585(17) Uani 1 1 d . . . C16 C -0.2481(5) 1.0100(4) 0.2190(3) 0.0624(18) Uani 1 1 d . . . H16 H -0.3116 1.0344 0.2377 0.075 Uiso 1 1 calc R . . C17 C -0.2309(5) 1.0117(5) 0.1454(3) 0.0640(18) Uani 1 1 d . . . C18 C -0.1334(5) 0.9760(4) 0.1191(3) 0.0609(18) Uani 1 1 d . . . H18 H -0.1191 0.9771 0.0700 0.073 Uiso 1 1 calc R . . C19 C -0.0579(4) 0.9393(4) 0.1630(3) 0.0494(15) Uani 1 1 d . . . C20 C 0.0500(4) 0.9113(4) 0.1316(3) 0.0545(16) Uani 1 1 d . . . H20A H 0.0509 0.9031 0.0842 0.065 Uiso 1 1 calc R . . H20B H 0.0784 0.8572 0.1636 0.065 Uiso 1 1 calc R . . C21 C 0.1137(4) 0.9782(4) 0.1237(3) 0.0535(16) Uani 1 1 d . . . C22 C 0.0794(5) 1.0633(5) 0.0844(3) 0.0629(18) Uani 1 1 d . . . H22 H 0.0205 1.0760 0.0630 0.075 Uiso 1 1 calc R . . C23 C 0.1319(6) 1.1290(5) 0.0769(3) 0.0688(19) Uani 1 1 d . . . C24 C 0.2185(5) 1.1072(5) 0.1105(3) 0.0693(19) Uani 1 1 d . . . H24 H 0.2537 1.1501 0.1072 0.083 Uiso 1 1 calc R . . C25 C 0.2031(4) 0.9597(4) 0.1535(3) 0.0535(16) Uani 1 1 d . . . C26 C 0.2569(5) 0.9675(4) 0.3166(3) 0.0552(16) Uani 1 1 d . . . C28 C -0.0799(4) 0.9364(4) 0.2369(3) 0.0516(15) Uani 1 1 d . . . C27 C -0.0367(5) 0.9668(4) 0.3943(3) 0.0610(18) Uani 1 1 d . . . C29 C 0.4428(5) 0.7322(4) 0.2849(4) 0.0642(18) Uani 1 1 d . . . C30 C 0.4772(5) 0.7037(5) 0.3534(4) 0.0656(18) Uani 1 1 d . . . C31 C 0.5271(5) 0.6207(5) 0.3755(4) 0.078(2) Uani 1 1 d . . . H31 H 0.5500 0.6012 0.4210 0.094 Uiso 1 1 calc R . . C32 C 0.5443(6) 0.5654(5) 0.3331(5) 0.084(2) Uani 1 1 d . . . C33 C 0.5179(5) 0.5971(5) 0.2645(5) 0.080(2) Uani 1 1 d . . . H33 H 0.5326 0.5609 0.2348 0.096 Uiso 1 1 calc R . . C34 C 0.4705(5) 0.6800(5) 0.2364(4) 0.079(2) Uani 1 1 d . . . C35 C -0.1252(5) 0.7159(4) 0.4014(3) 0.0605(17) Uani 1 1 d . . . C36 C -0.1474(5) 0.6543(5) 0.3750(4) 0.0663(19) Uani 1 1 d . . . C37 C -0.1722(5) 0.5818(5) 0.4282(4) 0.0690(19) Uani 1 1 d . . . H37 H -0.1887 0.5400 0.4125 0.083 Uiso 1 1 calc R . . C38 C -0.1745(5) 0.5667(5) 0.5016(4) 0.0657(18) Uani 1 1 d . . . C39 C -0.1513(6) 0.6284(5) 0.5247(4) 0.080(2) Uani 1 1 d . . . H39 H -0.1516 0.6198 0.5744 0.096 Uiso 1 1 calc R . . C40 C -0.1270(6) 0.7041(5) 0.4752(4) 0.076(2) Uani 1 1 d . . . H40 H -0.1123 0.7461 0.4916 0.092 Uiso 1 1 calc R . . C41 C 0.0959(8) 1.2185(6) 0.0325(5) 0.095(3) Uani 1 1 d . . . C42 C 0.0968(18) 1.2791(8) 0.0668(8) 0.294(12) Uani 1 1 d . . . H42A H 0.0993 1.3334 0.0310 0.441 Uiso 1 1 calc R . . H42B H 0.1551 1.2628 0.0920 0.441 Uiso 1 1 calc R . . H42C H 0.0366 1.2832 0.1012 0.441 Uiso 1 1 calc R . . C43 C 0.0173(17) 1.2276(9) -0.0081(12) 0.303(14) Uani 1 1 d . . . H43A H -0.0466 1.2335 0.0222 0.454 Uiso 1 1 calc R . . H43B H 0.0258 1.1781 -0.0251 0.454 Uiso 1 1 calc R . . H43C H 0.0192 1.2774 -0.0493 0.454 Uiso 1 1 calc R . . C44 C 0.1687(18) 1.2425(11) -0.0353(9) 0.322(15) Uani 1 1 d . . . H44A H 0.1328 1.2819 -0.0736 0.483 Uiso 1 1 calc R . . H44B H 0.2016 1.1923 -0.0498 0.483 Uiso 1 1 calc R . . H44C H 0.2185 1.2689 -0.0259 0.483 Uiso 1 1 calc R . . C45 C 0.3914(7) 1.1418(7) 0.3746(6) 0.117(3) Uani 1 1 d D . . C46 C 0.4958(13) 1.1311(11) 0.3549(9) 0.245(7) Uiso 1 1 d D . . H46A H 0.5216 1.0730 0.3547 0.367 Uiso 1 1 calc R . . H46B H 0.5264 1.1445 0.3895 0.367 Uiso 1 1 calc R . . H46C H 0.5115 1.1685 0.3071 0.367 Uiso 1 1 calc R . . C47 C 0.3602(14) 1.1385(12) 0.4575(10) 0.280(9) Uiso 1 1 d D . . H47A H 0.4091 1.0976 0.4858 0.419 Uiso 1 1 calc R . . H47B H 0.2949 1.1219 0.4740 0.419 Uiso 1 1 calc R . . H47C H 0.3574 1.1938 0.4634 0.419 Uiso 1 1 calc R . . C48 C 0.3355(18) 1.2327(14) 0.3507(13) 0.344(12) Uiso 1 1 d D . . H48A H 0.3670 1.2696 0.3653 0.517 Uiso 1 1 calc R . . H48B H 0.2663 1.2355 0.3733 0.517 Uiso 1 1 calc R . . H48C H 0.3377 1.2506 0.2986 0.517 Uiso 1 1 calc R . . C49 C -0.0747(7) 1.2399(6) 0.3463(5) 0.094(3) Uani 1 1 d . . . C50 C -0.1595(19) 1.2853(9) 0.3111(19) 0.40(2) Uani 1 1 d . . . H50A H -0.2011 1.3215 0.3391 0.596 Uiso 1 1 calc R . . H50B H -0.1978 1.2457 0.3070 0.596 Uiso 1 1 calc R . . H50C H -0.1374 1.3195 0.2632 0.596 Uiso 1 1 calc R . . C51 C 0.0007(18) 1.2716(9) 0.2834(12) 0.339(16) Uani 1 1 d . . . H51A H 0.0010 1.3306 0.2776 0.508 Uiso 1 1 calc R . . H51B H -0.0167 1.2659 0.2398 0.508 Uiso 1 1 calc R . . H51C H 0.0666 1.2388 0.2919 0.508 Uiso 1 1 calc R . . C52 C -0.054(2) 1.2645(8) 0.4020(11) 0.354(18) Uani 1 1 d . . . H52A H -0.0384 1.3210 0.3833 0.530 Uiso 1 1 calc R . . H52B H 0.0019 1.2255 0.4232 0.530 Uiso 1 1 calc R . . H52C H -0.1128 1.2644 0.4385 0.530 Uiso 1 1 calc R . . C53 C -0.3100(5) 1.0498(6) 0.0951(4) 0.090(3) Uani 1 1 d . . . C54 C -0.3394(12) 0.9869(11) 0.0714(12) 0.271(12) Uani 1 1 d . . . H54A H -0.2825 0.9617 0.0430 0.407 Uiso 1 1 calc R . . H54B H -0.3932 1.0134 0.0421 0.407 Uiso 1 1 calc R . . H54C H -0.3622 0.9434 0.1132 0.407 Uiso 1 1 calc R . . C55 C -0.4025(7) 1.1020(9) 0.1266(5) 0.155(5) Uani 1 1 d . . . H55A H -0.4543 1.1169 0.0956 0.232 Uiso 1 1 calc R . . H55B H -0.3851 1.1532 0.1298 0.232 Uiso 1 1 calc R . . H55C H -0.4268 1.0692 0.1746 0.232 Uiso 1 1 calc R . . C56 C -0.2695(8) 1.1110(11) 0.0246(6) 0.207(8) Uani 1 1 d . . . H56A H -0.2007 1.0881 0.0095 0.310 Uiso 1 1 calc R . . H56B H -0.2722 1.1653 0.0326 0.310 Uiso 1 1 calc R . . H56C H -0.3101 1.1183 -0.0128 0.310 Uiso 1 1 calc R . . C57 C 0.4660(7) 0.7607(5) 0.4036(4) 0.084(2) Uani 1 1 d . . . C58 C 0.3562(7) 0.7715(6) 0.4421(4) 0.104(3) Uani 1 1 d . . . H58A H 0.3104 0.7921 0.4061 0.156 Uiso 1 1 calc R . . H58B H 0.3471 0.8116 0.4698 0.156 Uiso 1 1 calc R . . H58C H 0.3427 0.7174 0.4742 0.156 Uiso 1 1 calc R . . C59 C 0.4989(7) 0.8466(6) 0.3622(5) 0.101(3) Uani 1 1 d . . . H59A H 0.5692 0.8372 0.3429 0.152 Uiso 1 1 calc R . . H59B H 0.4886 0.8812 0.3950 0.152 Uiso 1 1 calc R . . H59C H 0.4594 0.8752 0.3229 0.152 Uiso 1 1 calc R . . C60 C 0.5337(8) 0.7182(6) 0.4663(5) 0.131(4) Uani 1 1 d . . . H60A H 0.5158 0.6638 0.4939 0.196 Uiso 1 1 calc R . . H60B H 0.5232 0.7543 0.4978 0.196 Uiso 1 1 calc R . . H60C H 0.6035 0.7104 0.4455 0.196 Uiso 1 1 calc R . . C61 C 0.4562(7) 0.7104(7) 0.1542(5) 0.101(3) Uani 1 1 d . . . C62 C 0.5382(9) 0.6546(8) 0.1106(6) 0.169(6) Uani 1 1 d . . . H62A H 0.5263 0.5968 0.1268 0.253 Uiso 1 1 calc R . . H62B H 0.6045 0.6557 0.1194 0.253 Uiso 1 1 calc R . . H62C H 0.5334 0.6776 0.0593 0.253 Uiso 1 1 calc R . . C63 C 0.3530(8) 0.6962(6) 0.1472(5) 0.129(4) Uani 1 1 d . . . H63A H 0.3432 0.6399 0.1764 0.193 Uiso 1 1 calc R . . H63B H 0.3494 0.7020 0.0970 0.193 Uiso 1 1 calc R . . H63C H 0.3012 0.7377 0.1639 0.193 Uiso 1 1 calc R . . C64 C 0.4718(6) 0.8040(6) 0.1186(4) 0.102(3) Uani 1 1 d . . . H64A H 0.4779 0.8166 0.0664 0.153 Uiso 1 1 calc R . . H64B H 0.5323 0.8118 0.1319 0.153 Uiso 1 1 calc R . . H64C H 0.4148 0.8417 0.1353 0.153 Uiso 1 1 calc R . . C65 C 0.5934(7) 0.4719(5) 0.3600(6) 0.119(3) Uani 1 1 d . . . H65A H 0.5477 0.4360 0.3599 0.179 Uiso 1 1 calc R . . H65B H 0.6085 0.4603 0.4088 0.179 Uiso 1 1 calc R . . H65C H 0.6548 0.4607 0.3284 0.179 Uiso 1 1 calc R . . C66 C -0.1479(6) 0.6682(6) 0.2928(4) 0.084(2) Uani 1 1 d . . . C67 C -0.1745(9) 0.5911(7) 0.2799(5) 0.137(4) Uani 1 1 d . . . H67A H -0.2384 0.5800 0.3080 0.205 Uiso 1 1 calc R . . H67B H -0.1230 0.5422 0.2946 0.205 Uiso 1 1 calc R . . H67C H -0.1789 0.6024 0.2289 0.205 Uiso 1 1 calc R . . C68 C -0.2277(7) 0.7455(7) 0.2624(5) 0.119(3) Uani 1 1 d . . . H68A H -0.2235 0.7553 0.2106 0.179 Uiso 1 1 calc R . . H68B H -0.2155 0.7951 0.2720 0.179 Uiso 1 1 calc R . . H68C H -0.2939 0.7345 0.2855 0.179 Uiso 1 1 calc R . . C69 C -0.0415(7) 0.6849(6) 0.2507(4) 0.105(3) Uani 1 1 d . . . H69A H 0.0097 0.6390 0.2716 0.157 Uiso 1 1 calc R . . H69B H -0.0294 0.7377 0.2544 0.157 Uiso 1 1 calc R . . H69C H -0.0395 0.6884 0.2002 0.157 Uiso 1 1 calc R . . C70 C -0.2019(6) 0.4856(5) 0.5569(4) 0.087(2) Uani 1 1 d . . . C71 C -0.1389(14) 0.4535(10) 0.6178(8) 0.251(10) Uani 1 1 d . . . H71A H -0.1715 0.4775 0.6570 0.377 Uiso 1 1 calc R . . H71B H -0.0736 0.4700 0.6005 0.377 Uiso 1 1 calc R . . H71C H -0.1309 0.3924 0.6350 0.377 Uiso 1 1 calc R . . C72 C -0.166(2) 0.4082(8) 0.5255(9) 0.333(15) Uani 1 1 d . . . H72A H -0.1513 0.3572 0.5645 0.499 Uiso 1 1 calc R . . H72B H -0.1061 0.4166 0.4909 0.499 Uiso 1 1 calc R . . H72C H -0.2183 0.4027 0.5016 0.499 Uiso 1 1 calc R . . C73 C -0.3036(10) 0.4956(11) 0.5845(14) 0.44(2) Uani 1 1 d . . . H73A H -0.3311 0.4482 0.5832 0.660 Uiso 1 1 calc R . . H73B H -0.3387 0.5477 0.5554 0.660 Uiso 1 1 calc R . . H73C H -0.3114 0.4978 0.6341 0.660 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0523(10) 0.0703(11) 0.0553(10) -0.0254(9) -0.0061(8) -0.0046(8) P2 0.0588(11) 0.0682(11) 0.0483(9) -0.0071(8) -0.0067(8) -0.0066(9) O1 0.046(2) 0.077(3) 0.062(3) -0.031(2) -0.014(2) 0.003(2) O2 0.052(2) 0.070(3) 0.050(2) -0.026(2) -0.0058(19) -0.009(2) O3 0.049(2) 0.070(3) 0.062(3) -0.021(2) -0.013(2) 0.000(2) O4 0.072(3) 0.073(3) 0.048(2) -0.014(2) -0.005(2) -0.012(2) O5 0.048(2) 0.070(3) 0.042(2) -0.011(2) -0.0048(18) -0.004(2) O6 0.065(3) 0.074(3) 0.062(3) -0.003(2) -0.010(2) -0.019(2) C1 0.047(4) 0.088(5) 0.042(3) -0.022(4) 0.003(3) -0.020(4) C2 0.051(4) 0.086(5) 0.061(4) -0.031(4) -0.001(3) -0.019(4) C3 0.046(4) 0.074(4) 0.059(4) -0.032(4) -0.009(3) -0.004(3) C4 0.054(4) 0.084(5) 0.076(5) -0.034(4) -0.009(4) -0.008(4) C5 0.070(5) 0.087(5) 0.090(6) -0.049(5) -0.021(4) -0.007(4) C6 0.069(5) 0.100(6) 0.063(5) -0.044(4) -0.013(4) -0.002(4) C7 0.052(4) 0.062(4) 0.051(4) -0.022(3) -0.010(3) 0.003(3) C8 0.056(4) 0.076(5) 0.048(4) -0.026(3) -0.011(3) 0.010(3) C9 0.058(4) 0.084(5) 0.037(3) -0.027(3) -0.001(3) -0.005(4) C10 0.071(5) 0.077(5) 0.049(4) -0.027(4) -0.002(3) 0.002(4) C11 0.076(5) 0.075(5) 0.049(4) -0.025(4) -0.001(4) 0.004(4) C12 0.068(5) 0.091(6) 0.045(4) -0.021(4) -0.009(3) 0.019(4) C13 0.056(4) 0.082(5) 0.034(3) -0.015(3) 0.000(3) 0.003(4) C14 0.048(4) 0.097(5) 0.048(4) -0.020(4) 0.003(3) -0.003(4) C15 0.050(4) 0.076(4) 0.042(3) -0.011(3) 0.002(3) -0.013(3) C16 0.040(4) 0.088(5) 0.052(4) -0.021(4) 0.005(3) -0.003(3) C17 0.035(4) 0.095(5) 0.059(4) -0.018(4) -0.009(3) -0.008(3) C18 0.049(4) 0.095(5) 0.035(3) -0.014(3) 0.001(3) -0.018(4) C19 0.041(4) 0.068(4) 0.038(3) -0.014(3) 0.003(3) -0.016(3) C20 0.042(4) 0.075(4) 0.045(3) -0.020(3) -0.002(3) -0.008(3) C21 0.039(4) 0.081(5) 0.037(3) -0.016(3) 0.000(3) -0.010(3) C22 0.048(4) 0.093(5) 0.046(4) -0.013(4) -0.005(3) -0.017(4) C23 0.064(5) 0.088(5) 0.051(4) -0.012(4) -0.006(4) -0.018(4) C24 0.075(5) 0.086(5) 0.051(4) -0.017(4) 0.000(4) -0.032(4) C25 0.040(4) 0.080(5) 0.040(3) -0.024(3) 0.002(3) -0.006(3) C26 0.047(4) 0.065(4) 0.053(4) -0.022(3) -0.011(3) 0.004(3) C28 0.040(4) 0.061(4) 0.050(4) -0.010(3) -0.005(3) -0.010(3) C27 0.060(4) 0.078(5) 0.036(3) -0.015(3) 0.003(3) -0.002(4) C29 0.055(4) 0.069(5) 0.073(5) -0.031(4) -0.009(4) -0.005(3) C30 0.054(4) 0.073(5) 0.073(5) -0.029(4) -0.017(4) 0.001(4) C31 0.066(5) 0.080(6) 0.087(5) -0.019(5) -0.027(4) -0.003(4) C32 0.063(5) 0.073(5) 0.110(7) -0.021(5) -0.014(5) -0.002(4) C33 0.063(5) 0.081(6) 0.099(6) -0.040(5) -0.010(4) 0.004(4) C34 0.058(5) 0.090(6) 0.084(5) -0.029(5) -0.015(4) 0.005(4) C35 0.059(4) 0.058(4) 0.055(4) -0.006(3) -0.006(3) -0.007(3) C36 0.056(4) 0.083(5) 0.057(4) -0.015(4) -0.004(3) -0.018(4) C37 0.070(5) 0.069(5) 0.070(5) -0.017(4) -0.014(4) -0.017(4) C38 0.056(4) 0.065(5) 0.066(5) -0.007(4) -0.004(3) -0.010(3) C39 0.096(6) 0.086(6) 0.051(4) -0.010(4) -0.004(4) -0.017(5) C40 0.098(6) 0.072(5) 0.059(4) -0.014(4) -0.007(4) -0.023(4) C41 0.128(8) 0.078(6) 0.077(6) -0.004(5) -0.035(5) -0.023(5) C42 0.61(4) 0.088(9) 0.185(14) -0.032(9) -0.22(2) 0.075(14) C43 0.38(3) 0.119(11) 0.42(3) 0.088(13) -0.31(3) -0.066(14) C44 0.41(3) 0.196(17) 0.164(15) 0.076(13) 0.078(17) 0.075(18) C45 0.088(7) 0.155(9) 0.139(8) -0.095(7) 0.002(6) -0.024(6) C49 0.111(7) 0.080(6) 0.074(5) -0.021(5) -0.012(5) 0.017(5) C50 0.36(3) 0.084(10) 0.82(6) -0.098(19) -0.40(4) 0.059(14) C51 0.42(3) 0.092(11) 0.37(3) -0.023(14) 0.20(2) -0.041(14) C52 0.80(6) 0.076(9) 0.24(2) -0.059(11) -0.25(3) -0.022(17) C53 0.047(5) 0.155(8) 0.065(5) -0.038(5) -0.011(4) 0.004(5) C54 0.212(16) 0.241(18) 0.48(3) -0.22(2) -0.26(2) 0.076(14) C55 0.077(7) 0.266(14) 0.107(8) -0.055(8) -0.046(6) 0.031(8) C56 0.089(8) 0.34(2) 0.098(8) 0.030(10) -0.018(6) 0.031(10) C57 0.094(6) 0.085(6) 0.075(5) -0.025(4) -0.041(5) 0.011(5) C58 0.125(8) 0.111(7) 0.066(5) -0.025(5) -0.016(5) 0.002(6) C59 0.103(7) 0.094(6) 0.119(7) -0.031(6) -0.052(6) -0.009(5) C60 0.172(10) 0.114(8) 0.122(8) -0.033(6) -0.095(7) 0.010(7) C61 0.103(7) 0.116(8) 0.091(6) -0.059(6) -0.021(5) 0.017(6) C62 0.199(12) 0.161(11) 0.112(8) -0.076(8) -0.016(8) 0.087(9) C63 0.162(10) 0.125(8) 0.128(8) -0.049(7) -0.076(7) -0.015(7) C64 0.089(6) 0.130(8) 0.072(5) -0.026(5) -0.006(4) 0.007(5) C65 0.120(8) 0.073(6) 0.152(9) -0.020(6) -0.038(7) 0.007(5) C66 0.094(6) 0.107(6) 0.057(4) -0.018(4) -0.010(4) -0.035(5) C67 0.196(12) 0.171(10) 0.079(6) -0.040(7) -0.022(7) -0.092(9) C68 0.092(7) 0.167(10) 0.091(6) -0.012(6) -0.039(5) -0.021(6) C69 0.115(7) 0.136(8) 0.059(5) -0.030(5) 0.006(5) -0.027(6) C70 0.081(6) 0.072(5) 0.088(6) 0.008(4) -0.017(5) -0.012(4) C71 0.32(2) 0.202(15) 0.209(15) 0.124(13) -0.175(16) -0.148(15) C72 0.66(5) 0.085(10) 0.190(16) 0.006(10) 0.04(2) -0.079(17) C73 0.097(10) 0.232(17) 0.62(4) 0.30(2) 0.093(15) 0.008(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O2 1.619(4) . ? P1 O1 1.637(4) . ? P1 O3 1.649(4) . ? P2 O5 1.621(4) . ? P2 O4 1.634(4) . ? P2 O6 1.641(4) . ? O1 C25 1.382(6) . ? O2 C26 1.381(6) . ? O3 C29 1.413(7) . ? O4 C27 1.403(7) . ? O5 C28 1.400(6) . ? O6 C35 1.390(6) . ? C1 C25 1.386(9) . ? C1 C24 1.391(9) . ? C1 C2 1.512(8) . ? C2 C3 1.534(8) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C26 1.389(9) . ? C3 C4 1.390(9) . ? C4 C5 1.404(9) . ? C4 H4 0.9300 . ? C5 C6 1.385(10) . ? C5 C45 1.488(11) . ? C6 C7 1.379(9) . ? C6 H6 0.9300 . ? C7 C26 1.390(8) . ? C7 C8 1.519(9) . ? C8 C9 1.511(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C27 1.392(9) . ? C9 C10 1.397(9) . ? C10 C11 1.390(9) . ? C10 H10 0.9300 . ? C11 C12 1.387(10) . ? C11 C49 1.510(11) . ? C12 C13 1.358(10) . ? C12 H12 0.9300 . ? C13 C27 1.404(9) . ? C13 C14 1.510(9) . ? C14 C15 1.513(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.399(8) . ? C15 C28 1.397(8) . ? C16 C17 1.397(8) . ? C16 H16 0.9300 . ? C17 C18 1.404(8) . ? C17 C53 1.496(9) . ? C18 C19 1.379(8) . ? C18 H18 0.9300 . ? C19 C28 1.396(8) . ? C19 C20 1.515(8) . ? C20 C21 1.522(8) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C25 1.385(8) . ? C21 C22 1.412(9) . ? C22 C23 1.400(9) . ? C22 H22 0.9300 . ? C23 C24 1.384(9) . ? C23 C41 1.503(11) . ? C24 H24 0.9300 . ? C29 C30 1.402(9) . ? C29 C34 1.423(9) . ? C30 C31 1.379(9) . ? C30 C57 1.532(10) . ? C31 C32 1.377(10) . ? C31 H31 0.9300 . ? C32 C33 1.358(10) . ? C32 C65 1.527(11) . ? C33 C34 1.380(10) . ? C33 H33 0.9300 . ? C34 C61 1.555(11) . ? C35 C40 1.379(9) . ? C35 C36 1.396(9) . ? C36 C37 1.385(9) . ? C36 C66 1.542(9) . ? C37 C38 1.365(9) . ? C37 H37 0.9300 . ? C38 C39 1.363(10) . ? C38 C70 1.516(10) . ? C39 C40 1.395(9) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 C42 1.379(14) . ? C41 C43 1.408(14) . ? C41 C44 1.494(17) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.391(16) . ? C45 C48 1.51(2) . ? C45 C47 1.572(17) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 C52 1.365(15) . ? C49 C50 1.407(16) . ? C49 C51 1.480(16) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 C54 1.431(14) . ? C53 C55 1.511(12) . ? C53 C56 1.522(13) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 C59 1.529(11) . ? C57 C58 1.542(11) . ? C57 C60 1.564(10) . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 C63 1.520(12) . ? C61 C64 1.547(12) . ? C61 C62 1.583(11) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C66 C67 1.520(12) . ? C66 C68 1.535(12) . ? C66 C69 1.564(11) . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? C70 C73 1.383(14) . ? C70 C71 1.490(13) . ? C70 C72 1.546(16) . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? C73 H73A 0.9600 . ? C73 H73B 0.9600 . ? C73 H73C 0.9600 . ? 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 O2 P1 O1 98.74(19) . . ? O2 P1 O3 103.61(19) . . ? O1 P1 O3 100.72(18) . . ? O5 P2 O4 100.22(19) . . ? O5 P2 O6 97.48(19) . . ? O4 P2 O6 103.5(2) . . ? C25 O1 P1 129.7(3) . . ? C26 O2 P1 136.9(3) . . ? C29 O3 P1 121.3(3) . . ? C27 O4 P2 123.9(2) . . ? C28 O5 P2 128.6(3) . . ? C35 O6 P2 120.2(3) . . ? C25 C1 C24 118.8(6) . . ? C25 C1 C2 121.8(6) . . ? C24 C1 C2 119.5(6) . . ? C1 C2 C3 111.9(5) . . ? C1 C2 H2A 109.2 . . ? C3 C2 H2A 109.2 . . ? C1 C2 H2B 109.2 . . ? C3 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? C26 C3 C4 118.2(6) . . ? C26 C3 C2 122.4(6) . . ? C4 C3 C2 119.4(6) . . ? C3 C4 C5 122.8(7) . . ? C3 C4 H4 118.6 . . ? C5 C4 H4 118.6 . . ? C6 C5 C4 115.8(7) . . ? C6 C5 C45 121.1(7) . . ? C4 C5 C45 123.0(8) . . ? C7 C6 C5 123.4(6) . . ? C7 C6 H6 118.3 . . ? C5 C6 H6 118.3 . . ? C6 C7 C26 118.5(6) . . ? C6 C7 C8 121.4(6) . . ? C26 C7 C8 119.8(6) . . ? C9 C8 C7 109.4(5) . . ? C9 C8 H8A 109.8 . . ? C7 C8 H8A 109.8 . . ? C9 C8 H8B 109.8 . . ? C7 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? C27 C9 C10 117.0(6) . . ? C27 C9 C8 121.8(6) . . ? C10 C9 C8 121.1(6) . . ? C11 C10 C9 123.2(7) . . ? C11 C10 H10 118.4 . . ? C9 C10 H10 118.4 . . ? C12 C11 C10 116.3(7) . . ? C12 C11 C49 123.5(7) . . ? C10 C11 C49 120.2(8) . . ? C13 C12 C11 123.8(7) . . ? C13 C12 H12 118.1 . . ? C11 C12 H12 118.1 . . ? C12 C13 C27 118.1(7) . . ? C12 C13 C14 121.2(7) . . ? C27 C13 C14 120.5(7) . . ? C13 C14 C15 113.0(5) . . ? C13 C14 H14A 109.0 . . ? C15 C14 H14A 109.0 . . ? C13 C14 H14B 109.0 . . ? C15 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? C16 C15 C28 117.5(5) . . ? C16 C15 C14 119.3(6) . . ? C28 C15 C14 123.2(6) . . ? C15 C16 C17 123.1(6) . . ? C15 C16 H16 118.5 . . ? C17 C16 H16 118.5 . . ? C16 C17 C18 116.5(6) . . ? C16 C17 C53 123.3(6) . . ? C18 C17 C53 120.2(6) . . ? C19 C18 C17 122.6(5) . . ? C19 C18 H18 118.7 . . ? C17 C18 H18 118.7 . . ? C18 C19 C28 118.6(5) . . ? C18 C19 C20 121.6(5) . . ? C28 C19 C20 119.4(5) . . ? C19 C20 C21 110.2(5) . . ? C19 C20 H20A 109.6 . . ? C21 C20 H20A 109.6 . . ? C19 C20 H20B 109.6 . . ? C21 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? C25 C21 C22 118.7(6) . . ? C25 C21 C20 123.1(6) . . ? C22 C21 C20 118.2(5) . . ? C23 C22 C21 121.5(6) . . ? C23 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C24 C23 C22 117.1(7) . . ? C24 C23 C41 122.4(7) . . ? C22 C23 C41 120.5(7) . . ? C1 C24 C23 122.8(7) . . ? C1 C24 H24 118.6 . . ? C23 C24 H24 118.6 . . ? O1 C25 C21 117.9(5) . . ? O1 C25 C1 121.1(5) . . ? C21 C25 C1 121.0(6) . . ? O2 C26 C3 122.5(5) . . ? O2 C26 C7 116.8(5) . . ? C3 C26 C7 120.6(6) . . ? C19 C28 C15 121.5(5) . . ? C19 C28 O5 115.7(5) . . ? C15 C28 O5 122.6(5) . . ? C9 C27 O4 118.4(6) . . ? C9 C27 C13 121.5(7) . . ? O4 C27 C13 120.1(6) . . ? C30 C29 O3 119.4(6) . . ? C30 C29 C34 120.1(6) . . ? O3 C29 C34 120.5(6) . . ? C31 C30 C29 118.2(7) . . ? C31 C30 C57 118.2(7) . . ? C29 C30 C57 123.6(6) . . ? C30 C31 C32 122.5(7) . . ? C30 C31 H31 118.7 . . ? C32 C31 H31 118.7 . . ? C33 C32 C31 117.7(7) . . ? C33 C32 C65 120.1(9) . . ? C31 C32 C65 122.2(9) . . ? C32 C33 C34 124.0(8) . . ? C32 C33 H33 118.0 . . ? C34 C33 H33 118.0 . . ? C33 C34 C29 116.7(7) . . ? C33 C34 C61 118.2(8) . . ? C29 C34 C61 125.1(7) . . ? C40 C35 C36 121.8(6) . . ? C40 C35 O6 117.6(6) . . ? C36 C35 O6 120.5(5) . . ? C37 C36 C35 115.1(6) . . ? C37 C36 C66 122.9(7) . . ? C35 C36 C66 122.0(6) . . ? C38 C37 C36 125.4(7) . . ? C38 C37 H37 117.3 . . ? C36 C37 H37 117.3 . . ? C39 C38 C37 117.3(6) . . ? C39 C38 C70 119.9(7) . . ? C37 C38 C70 122.8(7) . . ? C38 C39 C40 121.2(7) . . ? C38 C39 H39 119.4 . . ? C40 C39 H39 119.4 . . ? C35 C40 C39 119.1(7) . . ? C35 C40 H40 120.4 . . ? C39 C40 H40 120.4 . . ? C42 C41 C43 120.5(14) . . ? C42 C41 C23 112.9(8) . . ? C43 C41 C23 115.4(9) . . ? C42 C41 C44 102.3(14) . . ? C43 C41 C44 91.9(13) . . ? C23 C41 C44 110.1(10) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C5 113.9(10) . . ? C46 C45 C48 115.3(14) . . ? C5 C45 C48 109.3(12) . . ? C46 C45 C47 112.2(12) . . ? C5 C45 C47 112.6(10) . . ? C48 C45 C47 91.6(12) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C52 C49 C50 118.5(16) . . ? C52 C49 C11 112.4(9) . . ? C50 C49 C11 113.8(10) . . ? C52 C49 C51 104.9(16) . . ? C50 C49 C51 95.1(16) . . ? C11 C49 C51 109.9(8) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 C17 112.3(9) . . ? C54 C53 C55 109.9(10) . . ? C17 C53 C55 113.6(7) . . ? C54 C53 C56 104.1(11) . . ? C17 C53 C56 111.1(7) . . ? C55 C53 C56 105.2(9) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C30 C57 C59 111.9(7) . . ? C30 C57 C58 109.2(7) . . ? C59 C57 C58 112.2(7) . . ? C30 C57 C60 111.4(7) . . ? C59 C57 C60 106.4(7) . . ? C58 C57 C60 105.6(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 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C63 C61 C64 112.9(8) . . ? C63 C61 C34 108.7(8) . . ? C64 C61 C34 111.6(7) . . ? C63 C61 C62 107.1(9) . . ? C64 C61 C62 106.3(8) . . ? C34 C61 C62 110.1(7) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C32 C65 H65A 109.5 . . ? C32 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C32 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C67 C66 C68 107.1(8) . . ? C67 C66 C36 110.6(7) . . ? C68 C66 C36 110.9(7) . . ? C67 C66 C69 110.4(8) . . ? C68 C66 C69 108.6(7) . . ? C36 C66 C69 109.2(6) . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C66 C68 H68A 109.5 . . ? C66 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C66 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C66 C69 H69A 109.5 . . ? C66 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C66 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C73 C70 C71 110.2(14) . . ? C73 C70 C38 111.8(7) . . ? C71 C70 C38 112.7(8) . . ? C73 C70 C72 113.2(15) . . ? C71 C70 C72 96.9(11) . . ? C38 C70 C72 111.2(8) . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C70 C72 H72A 109.5 . . ? C70 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C70 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C70 C73 H73A 109.5 . . ? C70 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C70 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? 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 O2 P1 O1 C25 0.3(4) . . . . ? O3 P1 O1 C25 -105.4(3) . . . . ? O1 P1 O2 C26 -90.5(4) . . . . ? O3 P1 O2 C26 12.9(4) . . . . ? O2 P1 O3 C29 136.4(3) . . . . ? O1 P1 O3 C29 -121.8(3) . . . . ? O5 P2 O4 C27 -6.1(4) . . . . ? O6 P2 O4 C27 -106.4(3) . . . . ? O4 P2 O5 C28 -94.4(3) . . . . ? O6 P2 O5 C28 10.9(4) . . . . ? O5 P2 O6 C35 167.4(3) . . . . ? O4 P2 O6 C35 -90.1(3) . . . . ? C25 C1 C2 C3 -90.0(7) . . . . ? C24 C1 C2 C3 88.7(7) . . . . ? C1 C2 C3 C26 56.7(9) . . . . ? C1 C2 C3 C4 -121.6(7) . . . . ? C26 C3 C4 C5 0.6(10) . . . . ? C2 C3 C4 C5 178.9(6) . . . . ? C3 C4 C5 C6 -5.6(11) . . . . ? C3 C4 C5 C45 175.3(8) . . . . ? C4 C5 C6 C7 3.4(11) . . . . ? C45 C5 C6 C7 -177.4(8) . . . . ? C5 C6 C7 C26 3.6(10) . . . . ? C5 C6 C7 C8 -171.0(6) . . . . ? C6 C7 C8 C9 94.3(7) . . . . ? C26 C7 C8 C9 -80.2(7) . . . . ? C7 C8 C9 C27 127.5(6) . . . . ? C7 C8 C9 C10 -48.9(7) . . . . ? C27 C9 C10 C11 -1.2(9) . . . . ? C8 C9 C10 C11 175.4(6) . . . . ? C9 C10 C11 C12 -0.6(9) . . . . ? C9 C10 C11 C49 -178.0(6) . . . . ? C10 C11 C12 C13 1.6(10) . . . . ? C49 C11 C12 C13 178.9(6) . . . . ? C11 C12 C13 C27 -0.7(10) . . . . ? C11 C12 C13 C14 -176.3(6) . . . . ? C12 C13 C14 C15 85.4(8) . . . . ? C27 C13 C14 C15 -90.0(7) . . . . ? C13 C14 C15 C16 -124.8(7) . . . . ? C13 C14 C15 C28 52.5(9) . . . . ? C28 C15 C16 C17 -0.5(10) . . . . ? C14 C15 C16 C17 177.0(6) . . . . ? C15 C16 C17 C18 -1.5(10) . . . . ? C15 C16 C17 C53 179.1(7) . . . . ? C16 C17 C18 C19 1.2(10) . . . . ? C53 C17 C18 C19 -179.4(7) . . . . ? C17 C18 C19 C28 1.1(10) . . . . ? C17 C18 C19 C20 -172.2(6) . . . . ? C18 C19 C20 C21 99.6(7) . . . . ? C28 C19 C20 C21 -73.6(7) . . . . ? C19 C20 C21 C25 125.9(6) . . . . ? C19 C20 C21 C22 -53.6(7) . . . . ? C25 C21 C22 C23 -1.8(9) . . . . ? C20 C21 C22 C23 177.7(5) . . . . ? C21 C22 C23 C24 -0.7(9) . . . . ? C21 C22 C23 C41 177.8(7) . . . . ? C25 C1 C24 C23 0.4(9) . . . . ? C2 C1 C24 C23 -178.3(6) . . . . ? C22 C23 C24 C1 1.5(10) . . . . ? C41 C23 C24 C1 -177.0(7) . . . . ? P1 O1 C25 C21 -116.5(4) . . . . ? P1 O1 C25 C1 66.5(6) . . . . ? C22 C21 C25 O1 -173.3(5) . . . . ? C20 C21 C25 O1 7.1(8) . . . . ? C22 C21 C25 C1 3.7(8) . . . . ? C20 C21 C25 C1 -175.8(5) . . . . ? C24 C1 C25 O1 173.9(5) . . . . ? C2 C1 C25 O1 -7.4(8) . . . . ? C24 C1 C25 C21 -3.1(9) . . . . ? C2 C1 C25 C21 175.6(5) . . . . ? P1 O2 C26 C3 46.0(7) . . . . ? P1 O2 C26 C7 -137.0(4) . . . . ? C4 C3 C26 O2 -176.3(5) . . . . ? C2 C3 C26 O2 5.4(9) . . . . ? C4 C3 C26 C7 6.9(9) . . . . ? C2 C3 C26 C7 -171.4(6) . . . . ? C6 C7 C26 O2 174.1(5) . . . . ? C8 C7 C26 O2 -11.2(8) . . . . ? C6 C7 C26 C3 -8.9(9) . . . . ? C8 C7 C26 C3 165.8(6) . . . . ? C18 C19 C28 C15 -3.2(9) . . . . ? C20 C19 C28 C15 170.2(6) . . . . ? C18 C19 C28 O5 -179.1(5) . . . . ? C20 C19 C28 O5 -5.7(8) . . . . ? C16 C15 C28 C19 2.9(9) . . . . ? C14 C15 C28 C19 -174.5(6) . . . . ? C16 C15 C28 O5 178.5(5) . . . . ? C14 C15 C28 O5 1.1(9) . . . . ? P2 O5 C28 C19 -126.7(4) . . . . ? P2 O5 C28 C15 57.4(7) . . . . ? C10 C9 C27 O4 -176.3(5) . . . . ? C8 C9 C27 O4 7.1(8) . . . . ? C10 C9 C27 C13 2.1(9) . . . . ? C8 C9 C27 C13 -174.4(5) . . . . ? P2 O4 C27 C9 -107.1(5) . . . . ? P2 O4 C27 C13 74.4(6) . . . . ? C12 C13 C27 C9 -1.2(9) . . . . ? C14 C13 C27 C9 174.3(5) . . . . ? C12 C13 C27 O4 177.2(5) . . . . ? C14 C13 C27 O4 -7.2(8) . . . . ? P1 O3 C29 C30 -100.2(6) . . . . ? P1 O3 C29 C34 81.1(6) . . . . ? O3 C29 C30 C31 173.3(6) . . . . ? C34 C29 C30 C31 -8.0(10) . . . . ? O3 C29 C30 C57 -9.1(10) . . . . ? C34 C29 C30 C57 169.6(7) . . . . ? C29 C30 C31 C32 0.2(11) . . . . ? C57 C30 C31 C32 -177.5(7) . . . . ? C30 C31 C32 C33 5.4(12) . . . . ? C30 C31 C32 C65 -175.9(7) . . . . ? C31 C32 C33 C34 -3.3(12) . . . . ? C65 C32 C33 C34 178.0(8) . . . . ? C32 C33 C34 C29 -4.1(11) . . . . ? C32 C33 C34 C61 172.9(8) . . . . ? C30 C29 C34 C33 9.8(10) . . . . ? O3 C29 C34 C33 -171.5(6) . . . . ? C30 C29 C34 C61 -167.0(7) . . . . ? O3 C29 C34 C61 11.7(11) . . . . ? P2 O6 C35 C40 57.0(7) . . . . ? P2 O6 C35 C36 -124.3(5) . . . . ? C40 C35 C36 C37 0.7(10) . . . . ? O6 C35 C36 C37 -177.9(5) . . . . ? C40 C35 C36 C66 178.5(7) . . . . ? O6 C35 C36 C66 -0.2(10) . . . . ? C35 C36 C37 C38 -1.3(11) . . . . ? C66 C36 C37 C38 -179.0(7) . . . . ? C36 C37 C38 C39 0.7(11) . . . . ? C36 C37 C38 C70 -179.7(7) . . . . ? C37 C38 C39 C40 0.5(11) . . . . ? C70 C38 C39 C40 -179.2(7) . . . . ? C36 C35 C40 C39 0.3(11) . . . . ? O6 C35 C40 C39 179.0(6) . . . . ? C38 C39 C40 C35 -0.9(11) . . . . ? C24 C23 C41 C42 -46.4(15) . . . . ? C22 C23 C41 C42 135.2(13) . . . . ? C24 C23 C41 C43 169.5(14) . . . . ? C22 C23 C41 C43 -8.9(17) . . . . ? C24 C23 C41 C44 67.2(15) . . . . ? C22 C23 C41 C44 -111.2(14) . . . . ? C6 C5 C45 C46 134.7(11) . . . . ? C4 C5 C45 C46 -46.3(14) . . . . ? C6 C5 C45 C48 -94.7(14) . . . . ? C4 C5 C45 C48 84.3(13) . . . . ? C6 C5 C45 C47 5.6(14) . . . . ? C4 C5 C45 C47 -175.4(10) . . . . ? C12 C11 C49 C52 135.1(16) . . . . ? C10 C11 C49 C52 -47.7(17) . . . . ? C12 C11 C49 C50 -3(2) . . . . ? C10 C11 C49 C50 174.1(18) . . . . ? C12 C11 C49 C51 -108.4(15) . . . . ? C10 C11 C49 C51 68.8(15) . . . . ? C16 C17 C53 C54 -113.6(12) . . . . ? C18 C17 C53 C54 67.0(13) . . . . ? C16 C17 C53 C55 11.9(13) . . . . ? C18 C17 C53 C55 -167.5(8) . . . . ? C16 C17 C53 C56 130.3(10) . . . . ? C18 C17 C53 C56 -49.1(12) . . . . ? C31 C30 C57 C59 130.2(7) . . . . ? C29 C30 C57 C59 -47.3(10) . . . . ? C31 C30 C57 C58 -105.0(7) . . . . ? C29 C30 C57 C58 77.5(9) . . . . ? C31 C30 C57 C60 11.3(11) . . . . ? C29 C30 C57 C60 -166.2(8) . . . . ? C33 C34 C61 C63 92.9(9) . . . . ? C29 C34 C61 C63 -90.3(10) . . . . ? C33 C34 C61 C64 -142.0(7) . . . . ? C29 C34 C61 C64 34.8(11) . . . . ? C33 C34 C61 C62 -24.2(12) . . . . ? C29 C34 C61 C62 152.6(9) . . . . ? C37 C36 C66 C67 -2.4(11) . . . . ? C35 C36 C66 C67 -180.0(8) . . . . ? C37 C36 C66 C68 116.2(8) . . . . ? C35 C36 C66 C68 -61.3(9) . . . . ? C37 C36 C66 C69 -124.1(8) . . . . ? C35 C36 C66 C69 58.3(10) . . . . ? C39 C38 C70 C73 85.4(17) . . . . ? C37 C38 C70 C73 -94.3(17) . . . . ? C39 C38 C70 C71 -39.4(14) . . . . ? C37 C38 C70 C71 140.9(12) . . . . ? C39 C38 C70 C72 -147.0(12) . . . . ? C37 C38 C70 C72 33.4(14) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.977 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.089 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.000 1052 93 ' ' 2 0.353 0.923 0.535 14 1 ' ' 3 0.425 0.085 0.020 7 0 ' ' 4 0.575 0.915 0.980 8 1 ' ' 5 0.647 0.077 0.465 14 1 ' ' _platon_squeeze_details ; ;