# ic011144x.cif _publ_contact_author_name ; Matthew W. Peters, Eric J. Werner, and Michael J. Scott ; _publ_contact_author_address ; P.O. Box 117200 University of Florida Gainesville FL, 32611 ; _publ_requested_journal ; Inorganic Chemistry ; _publ_section_title ; Selective Extraction of Actinides from Lanthanides with CMPO Ligands Secured to C3-Symmetric Triphenoxymethane Platform ; data_5_tris_nitrile _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; tris(3,5-di-tert-butyl-2-cyanomethoxyphenyl)methane ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H67 N3 O3' _chemical_formula_weight 746.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.8758(13) _cell_length_b 15.1036(13) _cell_length_c 18.5831(15) _cell_angle_alpha 90.00 _cell_angle_beta 91.221(2) _cell_angle_gamma 90.00 _cell_volume 4454.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Blocks _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.112 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 0.068 _exptl_absorpt_correction_type 'SADABS' _exptl_absorpt_correction_T_min 0.9735 _exptl_absorpt_correction_T_max 0.9834 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23606 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7824 _reflns_number_gt 6175 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0761P)^2^+2.7152P] 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 7824 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0687 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1601 _refine_ls_wR_factor_gt 0.1476 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.20863(9) 0.75185(9) 0.22830(8) 0.0324(3) Uani 1 1 d . . . O2 O 0.15338(8) 0.96382(9) 0.02016(7) 0.0298(3) Uani 1 1 d . . . O3 O 0.04832(9) 0.94852(10) 0.21748(8) 0.0362(4) Uani 1 1 d . . . N1 N 0.13838(16) 0.70293(18) 0.05915(14) 0.0678(7) Uani 1 1 d . . . N2 N 0.11488(14) 0.83277(15) -0.11984(12) 0.0542(6) Uani 1 1 d . . . N3 N 0.07174(16) 1.16471(16) 0.26866(14) 0.0651(7) Uani 1 1 d . . . C1 C 0.21604(12) 0.92653(12) 0.16321(10) 0.0263(4) Uani 1 1 d . . . H1A H 0.1639 0.9008 0.1404 0.032 Uiso 1 1 calc R . . C2 C 0.28578(12) 0.85696(12) 0.15530(10) 0.0258(4) Uani 1 1 d . . . C3 C 0.27832(12) 0.77274(12) 0.18692(10) 0.0261(4) Uani 1 1 d . . . C4 C 0.34273(12) 0.70987(12) 0.18432(10) 0.0272(4) Uani 1 1 d . . . C5 C 0.33848(13) 0.62072(13) 0.22491(11) 0.0325(5) Uani 1 1 d . . . C6 C 0.25919(15) 0.56746(14) 0.20510(15) 0.0459(6) Uani 1 1 d . . . H6A H 0.2530 0.5638 0.1526 0.069 Uiso 1 1 calc R . . H6B H 0.2097 0.5968 0.2248 0.069 Uiso 1 1 calc R . . H6C H 0.2642 0.5077 0.2252 0.069 Uiso 1 1 calc R . . C7 C 0.34037(16) 0.63927(16) 0.30624(12) 0.0444(6) Uani 1 1 d . . . H7A H 0.2924 0.6768 0.3184 0.067 Uiso 1 1 calc R . . H7B H 0.3930 0.6696 0.3196 0.067 Uiso 1 1 calc R . . H7C H 0.3370 0.5832 0.3326 0.067 Uiso 1 1 calc R . . C8 C 0.41379(15) 0.56133(14) 0.20788(13) 0.0402(5) Uani 1 1 d . . . H8A H 0.4090 0.5053 0.2341 0.060 Uiso 1 1 calc R . . H8B H 0.4662 0.5913 0.2226 0.060 Uiso 1 1 calc R . . H8C H 0.4143 0.5494 0.1560 0.060 Uiso 1 1 calc R . . C9 C 0.41438(12) 0.73292(13) 0.14591(10) 0.0281(4) Uani 1 1 d . . . H9A H 0.4585 0.6907 0.1424 0.034 Uiso 1 1 calc R . . C10 C 0.42409(12) 0.81467(13) 0.11263(10) 0.0268(4) Uani 1 1 d . . . C11 C 0.50370(13) 0.83951(14) 0.07208(11) 0.0330(5) Uani 1 1 d . . . C12 C 0.47928(15) 0.87049(17) -0.00408(12) 0.0448(6) Uani 1 1 d . . . H12A H 0.4514 0.8220 -0.0303 0.067 Uiso 1 1 calc R . . H12B H 0.5301 0.8883 -0.0294 0.067 Uiso 1 1 calc R . . H12C H 0.4407 0.9210 -0.0012 0.067 Uiso 1 1 calc R . . C13 C 0.54907(15) 0.91502(16) 0.11235(14) 0.0441(6) Uani 1 1 d . . . H13A H 0.5113 0.9661 0.1156 0.066 Uiso 1 1 calc R . . H13B H 0.5996 0.9320 0.0862 0.066 Uiso 1 1 calc R . . H13C H 0.5654 0.8952 0.1609 0.066 Uiso 1 1 calc R . . C14 C 0.56518(15) 0.76219(16) 0.06590(14) 0.0466(6) Uani 1 1 d . . . H14A H 0.5840 0.7435 0.1141 0.070 Uiso 1 1 calc R . . H14B H 0.6140 0.7808 0.0383 0.070 Uiso 1 1 calc R . . H14C H 0.5370 0.7126 0.0413 0.070 Uiso 1 1 calc R . . C15 C 0.35915(12) 0.87606(13) 0.11903(10) 0.0267(4) Uani 1 1 d . . . H15A H 0.3653 0.9329 0.0979 0.032 Uiso 1 1 calc R . . C16 C 0.23259(12) 1.01448(13) 0.12448(10) 0.0267(4) Uani 1 1 d . . . C17 C 0.19906(12) 1.03094(13) 0.05562(10) 0.0265(4) Uani 1 1 d . . . C18 C 0.20117(12) 1.11580(13) 0.02415(10) 0.0276(4) Uani 1 1 d . . . C19 C 0.15360(13) 1.13945(14) -0.04666(11) 0.0329(5) Uani 1 1 d . . . C20 C 0.16469(17) 1.23723(16) -0.06689(13) 0.0463(6) Uani 1 1 d . . . H20A H 0.2245 1.2495 -0.0743 0.069 Uiso 1 1 calc R . . H20B H 0.1441 1.2747 -0.0280 0.069 Uiso 1 1 calc R . . H20C H 0.1326 1.2499 -0.1113 0.069 Uiso 1 1 calc R . . C21 C 0.05823(14) 1.12367(18) -0.03732(13) 0.0466(6) Uani 1 1 d . . . H21A H 0.0379 1.1611 0.0017 0.070 Uiso 1 1 calc R . . H21B H 0.0485 1.0613 -0.0256 0.070 Uiso 1 1 calc R . . H21C H 0.0279 1.1386 -0.0822 0.070 Uiso 1 1 calc R . . C22 C 0.18525(16) 1.08526(16) -0.11061(11) 0.0425(5) Uani 1 1 d . . . H22A H 0.1580 1.1065 -0.1552 0.064 Uiso 1 1 calc R . . H22B H 0.1715 1.0226 -0.1036 0.064 Uiso 1 1 calc R . . H22C H 0.2464 1.0921 -0.1139 0.064 Uiso 1 1 calc R . . C23 C 0.24439(12) 1.18097(13) 0.06314(11) 0.0293(4) Uani 1 1 d . . . H23A H 0.2480 1.2385 0.0427 0.035 Uiso 1 1 calc R . . C24 C 0.28255(12) 1.16664(13) 0.13026(11) 0.0289(4) Uani 1 1 d . . . C25 C 0.32734(14) 1.24032(14) 0.17308(11) 0.0344(5) Uani 1 1 d . . . C26 C 0.3338(2) 1.32574(18) 0.12964(16) 0.0729(10) Uani 1 1 d . . . H26A H 0.3644 1.3704 0.1582 0.109 Uiso 1 1 calc R . . H26B H 0.2771 1.3476 0.1176 0.109 Uiso 1 1 calc R . . H26C H 0.3641 1.3141 0.0852 0.109 Uiso 1 1 calc R . . C27 C 0.27851(17) 1.2596(2) 0.24105(15) 0.0581(7) Uani 1 1 d . . . H27A H 0.2754 1.2058 0.2703 0.087 Uiso 1 1 calc R . . H27B H 0.2214 1.2792 0.2278 0.087 Uiso 1 1 calc R . . H27C H 0.3073 1.3063 0.2688 0.087 Uiso 1 1 calc R . . C28 C 0.41588(16) 1.2104(2) 0.19437(18) 0.0620(8) Uani 1 1 d . . . H28A H 0.4448 1.2580 0.2208 0.093 Uiso 1 1 calc R . . H28B H 0.4472 1.1961 0.1510 0.093 Uiso 1 1 calc R . . H28C H 0.4127 1.1577 0.2250 0.093 Uiso 1 1 calc R . . C29 C 0.27466(12) 1.08273(13) 0.16015(10) 0.0288(4) Uani 1 1 d . . . H29A H 0.2988 1.0717 0.2065 0.035 Uiso 1 1 calc R . . C30 C 0.19770(12) 0.93898(12) 0.24338(10) 0.0267(4) Uani 1 1 d . . . C31 C 0.11537(12) 0.94229(13) 0.26782(11) 0.0296(4) Uani 1 1 d . . . C32 C 0.09618(13) 0.93242(14) 0.34085(11) 0.0334(5) Uani 1 1 d . . . C33 C 0.00508(14) 0.91873(17) 0.36699(12) 0.0420(5) Uani 1 1 d . . . C34 C -0.03613(18) 0.8399(2) 0.32723(16) 0.0604(7) Uani 1 1 d . . . H34A H -0.0903 0.8261 0.3490 0.091 Uiso 1 1 calc R . . H34B H 0.0010 0.7882 0.3309 0.091 Uiso 1 1 calc R . . H34C H -0.0454 0.8551 0.2764 0.091 Uiso 1 1 calc R . . C35 C -0.04803(18) 1.0009(2) 0.35680(16) 0.0628(8) Uani 1 1 d . . . H35A H -0.1028 0.9920 0.3790 0.094 Uiso 1 1 calc R . . H35B H -0.0563 1.0126 0.3053 0.094 Uiso 1 1 calc R . . H35C H -0.0194 1.0515 0.3796 0.094 Uiso 1 1 calc R . . C36 C 0.00460(17) 0.8932(2) 0.44661(15) 0.0587(7) Uani 1 1 d . . . H36A H 0.0294 0.9412 0.4755 0.088 Uiso 1 1 calc R . . H36B H 0.0376 0.8390 0.4540 0.088 Uiso 1 1 calc R . . H36C H -0.0535 0.8830 0.4613 0.088 Uiso 1 1 calc R . . C37 C 0.16436(14) 0.93106(15) 0.38869(11) 0.0359(5) Uani 1 1 d . . . H37A H 0.1537 0.9252 0.4386 0.043 Uiso 1 1 calc R . . C38 C 0.24851(13) 0.93787(14) 0.36728(11) 0.0328(5) Uani 1 1 d . . . C39 C 0.32069(15) 0.93927(17) 0.42368(12) 0.0452(6) Uani 1 1 d . . . C40 C 0.3015(3) 1.0038(3) 0.4827(2) 0.1045(15) Uani 1 1 d . . . H40A H 0.3486 1.0051 0.5176 0.157 Uiso 1 1 calc R . . H40B H 0.2501 0.9854 0.5068 0.157 Uiso 1 1 calc R . . H40C H 0.2933 1.0630 0.4620 0.157 Uiso 1 1 calc R . . C41 C 0.3257(2) 0.8473(2) 0.4600(2) 0.0903(12) Uani 1 1 d . . . H41A H 0.3411 0.8027 0.4244 0.136 Uiso 1 1 calc R . . H41B H 0.2708 0.8323 0.4799 0.136 Uiso 1 1 calc R . . H41C H 0.3683 0.8485 0.4989 0.136 Uiso 1 1 calc R . . C42 C 0.4032(2) 0.9587(5) 0.3917(2) 0.149(3) Uani 1 1 d . . . H42A H 0.4018 1.0178 0.3699 0.224 Uiso 1 1 calc R . . H42B H 0.4152 0.9145 0.3547 0.224 Uiso 1 1 calc R . . H42C H 0.4473 0.9567 0.4294 0.224 Uiso 1 1 calc R . . C43 C 0.26334(13) 0.93819(13) 0.29410(11) 0.0288(4) Uani 1 1 d . . . H43A H 0.3198 0.9379 0.2782 0.035 Uiso 1 1 calc R . . C44 C 0.12802(14) 0.74307(15) 0.19480(13) 0.0392(5) Uani 1 1 d . . . H44A H 0.0973 0.7998 0.1991 0.047 Uiso 1 1 calc R . . H44B H 0.0957 0.6972 0.2204 0.047 Uiso 1 1 calc R . . C45 C 0.13221(15) 0.71913(16) 0.11906(15) 0.0444(6) Uani 1 1 d . . . C46 C 0.20339(14) 0.89624(14) -0.01176(12) 0.0360(5) Uani 1 1 d . . . H46A H 0.2175 0.8497 0.0241 0.043 Uiso 1 1 calc R . . H46B H 0.2565 0.9216 -0.0296 0.043 Uiso 1 1 calc R . . C47 C 0.15323(14) 0.85870(15) -0.07167(12) 0.0380(5) Uani 1 1 d . . . C48 C 0.03771(14) 1.03221(16) 0.18325(12) 0.0413(5) Uani 1 1 d . . . H48A H -0.0213 1.0377 0.1654 0.050 Uiso 1 1 calc R . . H48B H 0.0748 1.0351 0.1411 0.050 Uiso 1 1 calc R . . C49 C 0.05721(15) 1.10673(17) 0.23113(14) 0.0449(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0284(7) 0.0327(7) 0.0365(8) 0.0026(6) 0.0051(6) -0.0023(6) O2 0.0298(7) 0.0301(7) 0.0295(7) -0.0033(6) -0.0033(6) -0.0015(6) O3 0.0307(8) 0.0402(8) 0.0372(8) -0.0022(6) -0.0091(6) 0.0068(6) N1 0.0670(16) 0.0815(18) 0.0545(15) -0.0123(13) -0.0098(12) -0.0155(14) N2 0.0581(14) 0.0553(13) 0.0483(13) -0.0115(10) -0.0158(11) 0.0014(11) N3 0.0686(16) 0.0506(14) 0.0757(17) -0.0022(13) -0.0109(13) 0.0028(12) C1 0.0274(10) 0.0259(10) 0.0254(10) 0.0002(8) -0.0041(8) 0.0003(8) C2 0.0291(10) 0.0258(10) 0.0224(9) -0.0012(8) -0.0036(7) 0.0006(8) C3 0.0275(10) 0.0263(10) 0.0245(10) -0.0008(8) 0.0005(7) -0.0031(8) C4 0.0312(10) 0.0246(10) 0.0258(10) -0.0011(8) -0.0036(8) -0.0020(8) C5 0.0345(11) 0.0258(10) 0.0371(11) 0.0043(9) -0.0014(9) -0.0011(9) C6 0.0442(13) 0.0260(11) 0.0675(17) 0.0067(11) -0.0026(12) -0.0061(10) C7 0.0541(15) 0.0412(13) 0.0380(13) 0.0114(10) 0.0010(10) 0.0032(11) C8 0.0430(13) 0.0275(11) 0.0500(14) 0.0055(10) -0.0027(10) 0.0036(9) C9 0.0287(10) 0.0263(10) 0.0290(10) -0.0019(8) -0.0024(8) 0.0011(8) C10 0.0270(10) 0.0292(10) 0.0241(10) -0.0018(8) -0.0020(8) -0.0021(8) C11 0.0313(11) 0.0342(11) 0.0336(11) 0.0006(9) 0.0031(9) -0.0030(9) C12 0.0455(14) 0.0553(15) 0.0338(12) 0.0066(11) 0.0082(10) -0.0074(11) C13 0.0355(12) 0.0432(13) 0.0536(15) -0.0003(11) 0.0000(10) -0.0105(10) C14 0.0357(12) 0.0465(14) 0.0584(16) 0.0028(11) 0.0164(11) 0.0034(11) C15 0.0321(10) 0.0239(9) 0.0238(10) 0.0023(8) -0.0025(8) -0.0014(8) C16 0.0266(10) 0.0264(10) 0.0269(10) -0.0003(8) -0.0005(8) 0.0051(8) C17 0.0242(10) 0.0291(10) 0.0262(10) -0.0020(8) -0.0020(7) -0.0002(8) C18 0.0251(10) 0.0313(10) 0.0263(10) 0.0026(8) 0.0006(8) 0.0035(8) C19 0.0326(11) 0.0378(11) 0.0281(10) 0.0067(9) -0.0044(8) 0.0012(9) C20 0.0567(15) 0.0441(13) 0.0377(13) 0.0121(10) -0.0105(11) 0.0034(11) C21 0.0315(12) 0.0623(16) 0.0457(14) 0.0141(12) -0.0078(10) 0.0029(11) C22 0.0497(14) 0.0507(14) 0.0270(11) 0.0054(10) -0.0032(10) -0.0009(11) C23 0.0319(11) 0.0251(10) 0.0310(11) 0.0030(8) 0.0007(8) 0.0022(8) C24 0.0293(10) 0.0275(10) 0.0299(10) -0.0018(8) 0.0007(8) 0.0032(8) C25 0.0378(12) 0.0304(11) 0.0348(11) -0.0054(9) -0.0016(9) -0.0014(9) C26 0.120(3) 0.0390(15) 0.0591(18) -0.0025(13) -0.0215(18) -0.0291(16) C27 0.0543(16) 0.0657(17) 0.0545(16) -0.0290(14) 0.0024(12) -0.0085(13) C28 0.0397(14) 0.0599(17) 0.086(2) -0.0259(15) -0.0129(13) -0.0055(13) C29 0.0307(10) 0.0305(10) 0.0250(10) -0.0010(8) -0.0051(8) 0.0034(8) C30 0.0300(10) 0.0230(9) 0.0269(10) 0.0005(8) -0.0015(8) 0.0044(8) C31 0.0297(10) 0.0280(10) 0.0310(11) -0.0028(8) -0.0052(8) 0.0047(8) C32 0.0330(11) 0.0335(11) 0.0339(11) -0.0035(9) 0.0015(9) 0.0056(9) C33 0.0346(12) 0.0542(14) 0.0373(12) -0.0017(11) 0.0048(9) 0.0049(10) C34 0.0478(16) 0.0671(18) 0.0664(18) -0.0004(14) 0.0045(13) -0.0109(13) C35 0.0503(16) 0.0749(19) 0.0638(18) 0.0125(15) 0.0180(13) 0.0236(14) C36 0.0489(15) 0.0728(19) 0.0549(16) 0.0143(14) 0.0117(12) 0.0051(14) C37 0.0393(12) 0.0413(12) 0.0270(11) -0.0009(9) 0.0014(9) 0.0040(10) C38 0.0360(11) 0.0332(11) 0.0290(11) 0.0007(9) -0.0042(9) 0.0007(9) C39 0.0437(13) 0.0615(15) 0.0300(12) 0.0016(11) -0.0103(10) -0.0020(12) C40 0.100(3) 0.129(3) 0.082(3) -0.054(2) -0.050(2) 0.022(3) C41 0.091(3) 0.087(3) 0.090(3) 0.016(2) -0.045(2) 0.020(2) C42 0.053(2) 0.336(8) 0.057(2) 0.039(3) -0.0267(17) -0.071(3) C43 0.0282(10) 0.0274(10) 0.0306(11) 0.0015(8) -0.0021(8) 0.0009(8) C44 0.0321(12) 0.0355(12) 0.0500(14) -0.0029(10) 0.0027(10) -0.0035(9) C45 0.0357(13) 0.0425(13) 0.0545(16) -0.0023(11) -0.0069(11) -0.0065(10) C46 0.0394(12) 0.0346(11) 0.0335(11) -0.0047(9) -0.0069(9) 0.0036(9) C47 0.0425(13) 0.0359(12) 0.0353(12) -0.0056(10) -0.0029(10) 0.0015(10) C48 0.0358(12) 0.0495(13) 0.0382(12) 0.0031(10) -0.0048(9) 0.0143(10) C49 0.0388(13) 0.0429(14) 0.0527(15) 0.0062(12) -0.0040(11) 0.0084(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C3 1.397(2) . ? O1 C44 1.417(3) . ? O2 C17 1.403(2) . ? O2 C46 1.430(2) . ? O3 C31 1.405(2) . ? O3 C48 1.423(3) . ? N1 C45 1.146(3) . ? N2 C47 1.141(3) . ? N3 C49 1.140(3) . ? C1 C30 1.536(3) . ? C1 C2 1.536(3) . ? C1 C16 1.536(3) . ? C2 C15 1.388(3) . ? C2 C3 1.407(3) . ? C3 C4 1.397(3) . ? C4 C9 1.400(3) . ? C4 C5 1.546(3) . ? C5 C6 1.532(3) . ? C5 C8 1.533(3) . ? C5 C7 1.537(3) . ? C9 C10 1.391(3) . ? C10 C15 1.394(3) . ? C10 C11 1.532(3) . ? C11 C14 1.528(3) . ? C11 C12 1.533(3) . ? C11 C13 1.535(3) . ? C16 C29 1.389(3) . ? C16 C17 1.398(3) . ? C17 C18 1.410(3) . ? C18 C23 1.394(3) . ? C18 C19 1.545(3) . ? C19 C20 1.535(3) . ? C19 C22 1.536(3) . ? C19 C21 1.546(3) . ? C23 C24 1.392(3) . ? C24 C29 1.391(3) . ? C24 C25 1.534(3) . ? C25 C28 1.521(3) . ? C25 C27 1.524(3) . ? C25 C26 1.527(3) . ? C30 C43 1.390(3) . ? C30 C31 1.394(3) . ? C31 C32 1.405(3) . ? C32 C37 1.386(3) . ? C32 C33 1.549(3) . ? C33 C35 1.510(4) . ? C33 C36 1.529(3) . ? C33 C34 1.540(4) . ? C37 C38 1.406(3) . ? C38 C43 1.385(3) . ? C38 C39 1.537(3) . ? C39 C42 1.479(4) . ? C39 C40 1.503(4) . ? C39 C41 1.547(4) . ? C44 C45 1.456(3) . ? C46 C47 1.469(3) . ? C48 C49 1.464(4) . ? 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 C3 O1 C44 119.85(16) . . ? C17 O2 C46 115.14(15) . . ? C31 O3 C48 115.96(16) . . ? C30 C1 C2 109.19(15) . . ? C30 C1 C16 112.74(15) . . ? C2 C1 C16 114.58(16) . . ? C15 C2 C3 117.99(17) . . ? C15 C2 C1 121.22(17) . . ? C3 C2 C1 120.75(17) . . ? O1 C3 C4 117.03(17) . . ? O1 C3 C2 120.57(17) . . ? C4 C3 C2 122.13(17) . . ? C3 C4 C9 116.87(17) . . ? C3 C4 C5 122.38(17) . . ? C9 C4 C5 120.67(17) . . ? C6 C5 C8 106.47(18) . . ? C6 C5 C7 109.33(19) . . ? C8 C5 C7 108.10(18) . . ? C6 C5 C4 112.60(17) . . ? C8 C5 C4 111.50(17) . . ? C7 C5 C4 108.72(17) . . ? C10 C9 C4 123.12(18) . . ? C9 C10 C15 117.61(18) . . ? C9 C10 C11 122.45(18) . . ? C15 C10 C11 119.91(17) . . ? C14 C11 C10 112.64(17) . . ? C14 C11 C12 108.26(19) . . ? C10 C11 C12 109.51(17) . . ? C14 C11 C13 108.09(19) . . ? C10 C11 C13 109.01(17) . . ? C12 C11 C13 109.28(18) . . ? C2 C15 C10 122.21(18) . . ? C29 C16 C17 118.35(18) . . ? C29 C16 C1 120.23(17) . . ? C17 C16 C1 121.14(17) . . ? C16 C17 O2 118.99(17) . . ? C16 C17 C18 121.98(18) . . ? O2 C17 C18 118.61(16) . . ? C23 C18 C17 116.24(17) . . ? C23 C18 C19 120.37(18) . . ? C17 C18 C19 123.23(18) . . ? C20 C19 C22 106.37(18) . . ? C20 C19 C18 111.99(18) . . ? C22 C19 C18 111.94(17) . . ? C20 C19 C21 107.07(19) . . ? C22 C19 C21 109.99(19) . . ? C18 C19 C21 109.33(17) . . ? C24 C23 C18 123.78(18) . . ? C29 C24 C23 117.29(18) . . ? C29 C24 C25 119.91(18) . . ? C23 C24 C25 122.70(18) . . ? C28 C25 C27 109.0(2) . . ? C28 C25 C26 108.5(2) . . ? C27 C25 C26 108.5(2) . . ? C28 C25 C24 109.56(18) . . ? C27 C25 C24 109.29(18) . . ? C26 C25 C24 111.98(18) . . ? C16 C29 C24 122.16(18) . . ? C43 C30 C31 118.29(18) . . ? C43 C30 C1 120.12(17) . . ? C31 C30 C1 121.27(17) . . ? C30 C31 C32 122.35(18) . . ? C30 C31 O3 119.20(17) . . ? C32 C31 O3 118.25(18) . . ? C37 C32 C31 116.02(19) . . ? C37 C32 C33 121.22(19) . . ? C31 C32 C33 122.69(19) . . ? C35 C33 C36 108.3(2) . . ? C35 C33 C34 110.2(2) . . ? C36 C33 C34 104.9(2) . . ? C35 C33 C32 111.9(2) . . ? C36 C33 C32 111.2(2) . . ? C34 C33 C32 110.04(19) . . ? C32 C37 C38 123.44(19) . . ? C43 C38 C37 117.43(19) . . ? C43 C38 C39 121.99(19) . . ? C37 C38 C39 120.49(19) . . ? C42 C39 C40 111.0(3) . . ? C42 C39 C38 112.5(2) . . ? C40 C39 C38 110.3(2) . . ? C42 C39 C41 108.4(3) . . ? C40 C39 C41 105.9(3) . . ? C38 C39 C41 108.4(2) . . ? C38 C43 C30 121.67(19) . . ? O1 C44 C45 112.84(18) . . ? N1 C45 C44 177.0(3) . . ? O2 C46 C47 107.04(17) . . ? N2 C47 C46 177.1(3) . . ? O3 C48 C49 112.93(18) . . ? N3 C49 C48 179.4(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.565 _refine_diff_density_min -0.285 _refine_diff_density_rms 0.045 #===END data_8_cmpo_ligand _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; tris(3,5-di-tert-butyl-2-(2-(carbamoylmethylphosphineoxide)ethoxy)phen yl)methane ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H124 N3 O9 P3' _chemical_formula_weight 1556.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.207(2) _cell_length_b 22.309(3) _cell_length_c 22.805(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.212(5) _cell_angle_gamma 90.00 _cell_volume 8938.3(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.157 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3352 _exptl_absorpt_coefficient_mu 0.124 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.8820 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45472 _diffrn_reflns_av_R_equivalents 0.0541 _diffrn_reflns_av_sigmaI/netI 0.0629 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 24.72 _reflns_number_total 15253 _reflns_number_gt 10611 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A pentane molecule was "SQUEEZED" from the assymmetric unit ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0672P)^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 15253 _refine_ls_number_parameters 985 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0849 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1450 _refine_ls_wR_factor_gt 0.1292 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.73610(4) -0.25930(3) 0.28835(3) 0.03589(17) Uani 1 1 d . . . P2 P 0.72423(4) -0.01669(4) 0.22736(3) 0.04340(19) Uani 1 1 d . . . P3 P 0.49716(4) 0.16240(3) 0.07492(3) 0.03148(16) Uani 1 1 d . . . N1 N 0.55024(11) -0.15429(11) 0.25394(10) 0.0384(5) Uani 1 1 d . . . H1 H 0.5552(13) -0.1377(11) 0.2222(11) 0.027(7) Uiso 1 1 d . . . N2 N 0.52127(11) -0.01732(10) 0.10381(10) 0.0335(5) Uani 1 1 d . . . H2 H 0.5193(14) 0.0218(12) 0.0929(11) 0.037(7) Uiso 1 1 d . . . N3 N 0.42265(13) 0.10969(10) 0.21047(9) 0.0332(5) Uani 1 1 d . . . H3 H 0.3867(14) 0.1284(11) 0.2059(11) 0.025(7) Uiso 1 1 d . . . O1 O 0.39880(8) -0.15925(7) 0.18419(7) 0.0302(4) Uani 1 1 d . . . O2 O 0.31750(8) -0.04959(7) 0.06956(7) 0.0318(4) Uani 1 1 d . . . O3 O 0.36468(9) -0.01974(7) 0.28399(7) 0.0327(4) Uani 1 1 d . . . O4 O 0.60809(10) -0.20921(8) 0.33607(8) 0.0436(5) Uani 1 1 d . . . O5 O 0.70390(10) -0.31916(8) 0.29526(9) 0.0484(5) Uani 1 1 d . . . O6 O 0.58967(10) -0.09200(8) 0.16014(8) 0.0411(4) Uani 1 1 d . . . O7 O 0.77032(11) -0.06863(10) 0.21684(9) 0.0653(6) Uani 1 1 d . . . O8 O 0.54247(10) 0.10252(8) 0.20105(7) 0.0401(4) Uani 1 1 d . . . O9 O 0.49768(9) 0.09875(7) 0.05565(8) 0.0383(4) Uani 1 1 d . . . C1 C 0.27384(13) -0.07958(11) 0.17714(10) 0.0300(5) Uani 1 1 d . . . H1A H 0.3292 -0.0694 0.1863 0.036 Uiso 1 1 calc R . . C2 C 0.26434(13) -0.14210(11) 0.14789(10) 0.0294(5) Uani 1 1 d . . . C3 C 0.32697(12) -0.17960(11) 0.15204(10) 0.0277(5) Uani 1 1 d . . . C4 C 0.32019(13) -0.23408(11) 0.12040(10) 0.0323(6) Uani 1 1 d . . . C5 C 0.38916(14) -0.27261(12) 0.11622(12) 0.0382(6) Uani 1 1 d . . . C6 C 0.36444(19) -0.32754(16) 0.07473(17) 0.0728(10) Uani 1 1 d . . . H6A H 0.4096 -0.3496 0.0712 0.109 Uiso 1 1 calc R . . H6B H 0.3355 -0.3142 0.0343 0.109 Uiso 1 1 calc R . . H6C H 0.3325 -0.3537 0.0922 0.109 Uiso 1 1 calc R . . C7 C 0.43436(18) -0.29556(15) 0.17805(14) 0.0610(9) Uani 1 1 d . . . H7A H 0.4718 -0.3252 0.1726 0.092 Uiso 1 1 calc R . . H7B H 0.3996 -0.3143 0.1990 0.092 Uiso 1 1 calc R . . H7C H 0.4608 -0.2620 0.2024 0.092 Uiso 1 1 calc R . . C8 C 0.44144(17) -0.23570(14) 0.08802(14) 0.0557(8) Uani 1 1 d . . . H8A H 0.4841 -0.2606 0.0838 0.084 Uiso 1 1 calc R . . H8B H 0.4610 -0.2013 0.1142 0.084 Uiso 1 1 calc R . . H8C H 0.4129 -0.2214 0.0479 0.084 Uiso 1 1 calc R . . C9 C 0.24652(14) -0.25098(12) 0.08911(11) 0.0386(6) Uani 1 1 d . . . H9A H 0.2400 -0.2886 0.0689 0.046 Uiso 1 1 calc R . . C10 C 0.18196(14) -0.21640(12) 0.08563(11) 0.0373(6) Uani 1 1 d . . . C11 C 0.10362(15) -0.23827(13) 0.04858(12) 0.0462(7) Uani 1 1 d . . . C12 C 0.0923(2) -0.30403(19) 0.0618(2) 0.1086(17) Uani 1 1 d . . . H12A H 0.0412 -0.3167 0.0392 0.163 Uiso 1 1 calc R . . H12B H 0.0981 -0.3093 0.1055 0.163 Uiso 1 1 calc R . . H12C H 0.1303 -0.3284 0.0492 0.163 Uiso 1 1 calc R . . C13 C 0.09926(18) -0.23081(17) -0.01890(13) 0.0674(10) Uani 1 1 d . . . H13A H 0.0496 -0.2449 -0.0433 0.101 Uiso 1 1 calc R . . H13B H 0.1397 -0.2544 -0.0289 0.101 Uiso 1 1 calc R . . H13C H 0.1056 -0.1884 -0.0277 0.101 Uiso 1 1 calc R . . C14 C 0.03885(16) -0.20121(19) 0.06203(15) 0.0744(11) Uani 1 1 d . . . H14A H -0.0101 -0.2160 0.0371 0.112 Uiso 1 1 calc R . . H14B H 0.0450 -0.1590 0.0524 0.112 Uiso 1 1 calc R . . H14C H 0.0403 -0.2050 0.1051 0.112 Uiso 1 1 calc R . . C15 C 0.19306(13) -0.16059(12) 0.11403(10) 0.0344(6) Uani 1 1 d . . . H15A H 0.1508 -0.1346 0.1101 0.041 Uiso 1 1 calc R . . C16 C 0.23126(12) -0.03238(11) 0.13166(10) 0.0300(5) Uani 1 1 d . . . C17 C 0.25327(12) -0.02041(11) 0.07858(10) 0.0297(5) Uani 1 1 d . . . C18 C 0.21068(13) 0.01822(11) 0.03339(11) 0.0317(6) Uani 1 1 d . . . C19 C 0.22601(14) 0.02568(12) -0.02992(11) 0.0375(6) Uani 1 1 d . . . C20 C 0.16660(17) 0.06656(15) -0.07194(12) 0.0547(8) Uani 1 1 d . . . H20A H 0.1773 0.0691 -0.1118 0.082 Uiso 1 1 calc R . . H20B H 0.1691 0.1067 -0.0541 0.082 Uiso 1 1 calc R . . H20C H 0.1156 0.0498 -0.0767 0.082 Uiso 1 1 calc R . . C21 C 0.30439(15) 0.05415(14) -0.02510(12) 0.0470(7) Uani 1 1 d . . . H21A H 0.3079 0.0660 -0.0656 0.070 Uiso 1 1 calc R . . H21B H 0.3445 0.0250 -0.0078 0.070 Uiso 1 1 calc R . . H21C H 0.3107 0.0896 0.0012 0.070 Uiso 1 1 calc R . . C22 C 0.22103(15) -0.03588(13) -0.05998(12) 0.0444(7) Uani 1 1 d . . . H22A H 0.2243 -0.0313 -0.1020 0.067 Uiso 1 1 calc R . . H22B H 0.1725 -0.0548 -0.0599 0.067 Uiso 1 1 calc R . . H22C H 0.2631 -0.0610 -0.0374 0.067 Uiso 1 1 calc R . . C23 C 0.14967(13) 0.04739(12) 0.04675(11) 0.0351(6) Uani 1 1 d . . . H23A H 0.1211 0.0746 0.0175 0.042 Uiso 1 1 calc R . . C24 C 0.12791(13) 0.03928(11) 0.09998(11) 0.0317(6) Uani 1 1 d . . . C25 C 0.06052(14) 0.07512(12) 0.11010(12) 0.0401(6) Uani 1 1 d . . . C26 C 0.08036(16) 0.14223(12) 0.11239(13) 0.0484(7) Uani 1 1 d . . . H26A H 0.1276 0.1492 0.1440 0.073 Uiso 1 1 calc R . . H26B H 0.0390 0.1654 0.1216 0.073 Uiso 1 1 calc R . . H26C H 0.0871 0.1548 0.0730 0.073 Uiso 1 1 calc R . . C27 C -0.01015(14) 0.06375(14) 0.05709(15) 0.0585(9) Uani 1 1 d . . . H27A H -0.0236 0.0212 0.0559 0.088 Uiso 1 1 calc R . . H27B H 0.0009 0.0751 0.0188 0.088 Uiso 1 1 calc R . . H27C H -0.0528 0.0878 0.0628 0.088 Uiso 1 1 calc R . . C28 C 0.04186(19) 0.05799(16) 0.16948(16) 0.0682(10) Uani 1 1 d . . . H28A H 0.0299 0.0151 0.1690 0.102 Uiso 1 1 calc R . . H28B H -0.0021 0.0812 0.1738 0.102 Uiso 1 1 calc R . . H28C H 0.0858 0.0666 0.2038 0.102 Uiso 1 1 calc R . . C29 C 0.16858(13) -0.00188(11) 0.14148(11) 0.0319(6) Uani 1 1 d . . . H29A H 0.1534 -0.0096 0.1776 0.038 Uiso 1 1 calc R . . C30 C 0.25215(13) -0.07802(11) 0.23786(11) 0.0307(5) Uani 1 1 d . . . C31 C 0.29820(13) -0.04862(11) 0.28891(11) 0.0324(6) Uani 1 1 d . . . C32 C 0.28268(15) -0.05086(12) 0.34578(11) 0.0387(6) Uani 1 1 d . . . C33 C 0.33915(19) -0.02765(14) 0.40473(12) 0.0527(8) Uani 1 1 d . . . C34 C 0.41654(18) -0.06023(16) 0.41362(14) 0.0650(9) Uani 1 1 d . . . H34A H 0.4528 -0.0449 0.4502 0.098 Uiso 1 1 calc R . . H34B H 0.4363 -0.0530 0.3782 0.098 Uiso 1 1 calc R . . H34C H 0.4094 -0.1034 0.4180 0.098 Uiso 1 1 calc R . . C35 C 0.3505(2) 0.03969(15) 0.40237(15) 0.0745(11) Uani 1 1 d . . . H35A H 0.3010 0.0599 0.3947 0.112 Uiso 1 1 calc R . . H35B H 0.3743 0.0492 0.3697 0.112 Uiso 1 1 calc R . . H35C H 0.3834 0.0534 0.4413 0.112 Uiso 1 1 calc R . . C36 C 0.3114(2) -0.04158(18) 0.46150(14) 0.0783(11) Uani 1 1 d . . . H36A H 0.2637 -0.0201 0.4590 0.117 Uiso 1 1 calc R . . H36B H 0.3500 -0.0287 0.4979 0.117 Uiso 1 1 calc R . . H36C H 0.3027 -0.0848 0.4637 0.117 Uiso 1 1 calc R . . C37 C 0.21367(16) -0.07781(13) 0.34758(12) 0.0451(7) Uani 1 1 d . . . H37A H 0.2007 -0.0784 0.3853 0.054 Uiso 1 1 calc R . . C38 C 0.16352(15) -0.10351(12) 0.29789(12) 0.0400(6) Uani 1 1 d . . . C39 C 0.08558(16) -0.12895(15) 0.29937(14) 0.0541(8) Uani 1 1 d . . . C40 C 0.0764(2) -0.19355(17) 0.27360(17) 0.0762(11) Uani 1 1 d . . . H40A H 0.0269 -0.2096 0.2753 0.114 Uiso 1 1 calc R . . H40B H 0.1171 -0.2189 0.2979 0.114 Uiso 1 1 calc R . . H40C H 0.0795 -0.1930 0.2313 0.114 Uiso 1 1 calc R . . C41 C 0.02370(18) -0.0906(2) 0.2605(2) 0.0982(15) Uani 1 1 d . . . H41A H 0.0281 -0.0496 0.2767 0.147 Uiso 1 1 calc R . . H41B H -0.0261 -0.1071 0.2608 0.147 Uiso 1 1 calc R . . H41C H 0.0287 -0.0899 0.2188 0.147 Uiso 1 1 calc R . . C42 C 0.0768(2) -0.1334(2) 0.36433(17) 0.0895(13) Uani 1 1 d . . . H42A H 0.0754 -0.0930 0.3809 0.134 Uiso 1 1 calc R . . H42B H 0.1201 -0.1555 0.3898 0.134 Uiso 1 1 calc R . . H42C H 0.0295 -0.1545 0.3638 0.134 Uiso 1 1 calc R . . C43 C 0.18580(14) -0.10487(12) 0.24400(11) 0.0354(6) Uani 1 1 d . . . H43A H 0.1542 -0.1251 0.2099 0.043 Uiso 1 1 calc R . . C44 C 0.41435(13) -0.16508(12) 0.24908(10) 0.0323(6) Uani 1 1 d . . . H44A H 0.4193 -0.2079 0.2609 0.039 Uiso 1 1 calc R . . H44B H 0.3725 -0.1473 0.2636 0.039 Uiso 1 1 calc R . . C45 C 0.48824(13) -0.13228(12) 0.27653(11) 0.0362(6) Uani 1 1 d . . . H45A H 0.4810 -0.0890 0.2672 0.043 Uiso 1 1 calc R . . H45B H 0.5017 -0.1369 0.3213 0.043 Uiso 1 1 calc R . . C46 C 0.60578(13) -0.18987(11) 0.28535(11) 0.0327(6) Uani 1 1 d . . . C47 C 0.66624(13) -0.20470(12) 0.25235(11) 0.0370(6) Uani 1 1 d . . . H47A H 0.6931 -0.1672 0.2475 0.044 Uiso 1 1 calc R . . H47B H 0.6403 -0.2194 0.2112 0.044 Uiso 1 1 calc R . . C48 C 0.79822(14) -0.26281(13) 0.23793(11) 0.0394(6) Uani 1 1 d . . . C49 C 0.82098(16) -0.31954(15) 0.22458(13) 0.0516(8) Uani 1 1 d . . . H49A H 0.8041 -0.3539 0.2419 0.062 Uiso 1 1 calc R . . C50 C 0.86826(19) -0.32623(18) 0.18606(15) 0.0668(10) Uani 1 1 d . . . H50A H 0.8843 -0.3650 0.1776 0.080 Uiso 1 1 calc R . . C51 C 0.89172(18) -0.2763(2) 0.16022(15) 0.0695(10) Uani 1 1 d . . . H51A H 0.9237 -0.2809 0.1336 0.083 Uiso 1 1 calc R . . C52 C 0.86924(16) -0.21970(17) 0.17265(13) 0.0587(9) Uani 1 1 d . . . H52A H 0.8859 -0.1855 0.1548 0.070 Uiso 1 1 calc R . . C53 C 0.82207(14) -0.21275(14) 0.21144(12) 0.0443(7) Uani 1 1 d . . . H53A H 0.8062 -0.1738 0.2198 0.053 Uiso 1 1 calc R . . C54 C 0.79104(13) -0.23051(12) 0.36074(11) 0.0373(6) Uani 1 1 d . . . C55 C 0.85194(14) -0.19159(13) 0.36709(12) 0.0422(7) Uani 1 1 d . . . H55A H 0.8673 -0.1791 0.3323 0.051 Uiso 1 1 calc R . . C56 C 0.89065(16) -0.17069(15) 0.42430(13) 0.0555(8) Uani 1 1 d . . . H56A H 0.9321 -0.1438 0.4284 0.067 Uiso 1 1 calc R . . C57 C 0.86915(17) -0.18878(18) 0.47504(14) 0.0642(10) Uani 1 1 d . . . H57A H 0.8950 -0.1737 0.5139 0.077 Uiso 1 1 calc R . . C58 C 0.81065(17) -0.22837(17) 0.46936(13) 0.0624(9) Uani 1 1 d . . . H58A H 0.7969 -0.2417 0.5046 0.075 Uiso 1 1 calc R . . C59 C 0.77122(16) -0.24926(15) 0.41288(13) 0.0519(8) Uani 1 1 d . . . H59A H 0.7303 -0.2766 0.4095 0.062 Uiso 1 1 calc R . . C60 C 0.38829(12) -0.02179(12) 0.10080(11) 0.0319(6) Uani 1 1 d . . . H60A H 0.3975 -0.0273 0.1452 0.038 Uiso 1 1 calc R . . H60B H 0.3864 0.0217 0.0920 0.038 Uiso 1 1 calc R . . C61 C 0.45170(13) -0.05083(12) 0.07908(12) 0.0348(6) Uani 1 1 d . . . H61A H 0.4585 -0.0930 0.0930 0.042 Uiso 1 1 calc R . . H61B H 0.4389 -0.0505 0.0341 0.042 Uiso 1 1 calc R . . C62 C 0.58279(13) -0.03931(11) 0.14288(10) 0.0305(6) Uani 1 1 d . . . C63 C 0.64670(13) 0.00555(11) 0.16379(11) 0.0328(6) Uani 1 1 d . . . H63A H 0.6247 0.0432 0.1748 0.039 Uiso 1 1 calc R . . H63B H 0.6679 0.0146 0.1290 0.039 Uiso 1 1 calc R . . C64 C 0.78029(15) 0.05058(15) 0.24366(12) 0.0491(8) Uani 1 1 d . . . C65 C 0.85797(18) 0.0459(2) 0.24938(17) 0.0905(14) Uani 1 1 d . . . H65A H 0.8791 0.0081 0.2438 0.109 Uiso 1 1 calc R . . C66 C 0.9041(3) 0.0946(3) 0.2628(2) 0.121(2) Uani 1 1 d . . . H66A H 0.9573 0.0904 0.2675 0.145 Uiso 1 1 calc R . . C67 C 0.8747(3) 0.1498(3) 0.26976(19) 0.1120(19) Uani 1 1 d . . . H67A H 0.9073 0.1837 0.2785 0.134 Uiso 1 1 calc R . . C68 C 0.7964(3) 0.1567(2) 0.26395(18) 0.0963(14) Uani 1 1 d . . . H68A H 0.7756 0.1948 0.2689 0.116 Uiso 1 1 calc R . . C69 C 0.75011(19) 0.10623(16) 0.25080(15) 0.0652(9) Uani 1 1 d . . . H69A H 0.6970 0.1100 0.2467 0.078 Uiso 1 1 calc R . . C70 C 0.68740(15) -0.02824(12) 0.29256(11) 0.0393(6) Uani 1 1 d . . . C71 C 0.72313(19) -0.07134(14) 0.33456(13) 0.0573(8) Uani 1 1 d . . . H71A H 0.7651 -0.0930 0.3278 0.069 Uiso 1 1 calc R . . C72 C 0.6988(2) -0.08305(15) 0.38556(14) 0.0668(10) Uani 1 1 d . . . H72A H 0.7237 -0.1128 0.4136 0.080 Uiso 1 1 calc R . . C73 C 0.63847(19) -0.05182(14) 0.39597(13) 0.0562(8) Uani 1 1 d . . . H73A H 0.6212 -0.0603 0.4309 0.067 Uiso 1 1 calc R . . C74 C 0.60298(17) -0.00818(14) 0.35559(12) 0.0505(7) Uani 1 1 d . . . H74A H 0.5616 0.0138 0.3630 0.061 Uiso 1 1 calc R . . C75 C 0.62747(15) 0.00370(13) 0.30421(12) 0.0429(7) Uani 1 1 d . . . H75A H 0.6030 0.0340 0.2767 0.051 Uiso 1 1 calc R . . C76 C 0.35211(14) 0.03613(11) 0.25133(11) 0.0343(6) Uani 1 1 d . . . H76A H 0.3231 0.0641 0.2705 0.041 Uiso 1 1 calc R . . H76B H 0.3231 0.0294 0.2086 0.041 Uiso 1 1 calc R . . C77 C 0.42992(14) 0.06135(11) 0.25403(11) 0.0350(6) Uani 1 1 d . . . H77A H 0.4538 0.0765 0.2955 0.042 Uiso 1 1 calc R . . H77B H 0.4629 0.0294 0.2446 0.042 Uiso 1 1 calc R . . C78 C 0.47897(14) 0.12572(11) 0.18678(10) 0.0318(6) Uani 1 1 d . . . C79 C 0.45920(16) 0.17493(13) 0.13984(12) 0.0439(7) Uani 1 1 d . . . H79A H 0.4791 0.2134 0.1592 0.053 Uiso 1 1 calc R . . H79B H 0.4031 0.1784 0.1255 0.053 Uiso 1 1 calc R . . C80 C 0.59061(14) 0.19514(11) 0.09138(10) 0.0343(6) Uani 1 1 d . . . C81 C 0.60742(18) 0.25116(14) 0.11850(13) 0.0553(8) Uani 1 1 d . . . H81A H 0.5693 0.2726 0.1313 0.066 Uiso 1 1 calc R . . C82 C 0.67877(19) 0.27575(16) 0.12692(15) 0.0668(10) Uani 1 1 d . . . H82A H 0.6899 0.3137 0.1462 0.080 Uiso 1 1 calc R . . C83 C 0.73333(19) 0.24582(17) 0.10775(16) 0.0684(10) Uani 1 1 d . . . H83A H 0.7823 0.2631 0.1133 0.082 Uiso 1 1 calc R . . C84 C 0.71779(18) 0.19054(16) 0.08038(18) 0.0721(10) Uani 1 1 d . . . H84A H 0.7560 0.1698 0.0670 0.087 Uiso 1 1 calc R . . C85 C 0.64641(15) 0.16523(14) 0.07241(14) 0.0521(8) Uani 1 1 d . . . H85A H 0.6359 0.1270 0.0537 0.062 Uiso 1 1 calc R . . C86 C 0.43572(14) 0.20742(11) 0.01647(11) 0.0338(6) Uani 1 1 d . . . C87 C 0.41501(17) 0.26589(12) 0.02575(12) 0.0465(7) Uani 1 1 d . . . H87A H 0.4353 0.2848 0.0639 0.056 Uiso 1 1 calc R . . C88 C 0.36465(18) 0.29657(15) -0.02065(14) 0.0586(8) Uani 1 1 d . . . H88A H 0.3513 0.3368 -0.0145 0.070 Uiso 1 1 calc R . . C89 C 0.33380(17) 0.26881(16) -0.07588(13) 0.0544(8) Uani 1 1 d . . . H89A H 0.2993 0.2900 -0.1076 0.065 Uiso 1 1 calc R . . C90 C 0.35294(16) 0.21091(15) -0.08472(12) 0.0491(8) Uani 1 1 d . . . H90A H 0.3305 0.1915 -0.1222 0.059 Uiso 1 1 calc R . . C91 C 0.40492(14) 0.18035(13) -0.03932(11) 0.0379(6) Uani 1 1 d . . . H91A H 0.4195 0.1407 -0.0464 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0285(3) 0.0365(4) 0.0423(4) 0.0054(3) 0.0086(3) 0.0002(3) P2 0.0336(4) 0.0507(5) 0.0430(4) -0.0075(3) 0.0051(3) 0.0098(3) P3 0.0354(3) 0.0294(4) 0.0307(3) 0.0035(3) 0.0106(3) 0.0015(3) N1 0.0276(11) 0.0551(16) 0.0314(12) 0.0117(11) 0.0057(9) 0.0058(11) N2 0.0275(11) 0.0272(13) 0.0457(13) 0.0019(10) 0.0095(9) -0.0005(10) N3 0.0315(12) 0.0296(13) 0.0400(13) 0.0069(10) 0.0118(10) 0.0042(11) O1 0.0254(8) 0.0379(10) 0.0275(9) 0.0022(7) 0.0073(7) 0.0003(8) O2 0.0242(8) 0.0362(10) 0.0372(9) -0.0027(7) 0.0116(7) 0.0005(7) O3 0.0363(9) 0.0286(10) 0.0351(9) 0.0047(7) 0.0128(7) 0.0011(8) O4 0.0425(10) 0.0481(12) 0.0424(11) 0.0161(9) 0.0150(8) 0.0059(9) O5 0.0415(10) 0.0355(11) 0.0686(13) 0.0056(9) 0.0154(9) -0.0042(9) O6 0.0484(11) 0.0312(11) 0.0440(11) 0.0061(8) 0.0126(9) 0.0019(9) O7 0.0536(12) 0.0744(16) 0.0631(13) -0.0125(11) 0.0068(10) 0.0336(12) O8 0.0397(10) 0.0432(11) 0.0411(10) 0.0087(8) 0.0170(8) 0.0112(9) O9 0.0439(10) 0.0285(10) 0.0429(10) 0.0011(8) 0.0124(8) -0.0012(8) C1 0.0259(12) 0.0353(15) 0.0318(13) 0.0021(11) 0.0127(10) 0.0013(11) C2 0.0296(12) 0.0344(14) 0.0253(12) 0.0052(10) 0.0092(10) -0.0016(11) C3 0.0266(12) 0.0296(14) 0.0270(12) 0.0053(10) 0.0072(10) -0.0008(11) C4 0.0344(13) 0.0323(14) 0.0312(13) 0.0042(11) 0.0104(11) -0.0003(12) C5 0.0409(14) 0.0335(15) 0.0402(15) -0.0006(11) 0.0108(12) 0.0057(12) C6 0.065(2) 0.056(2) 0.095(3) -0.0290(19) 0.0143(19) 0.0058(18) C7 0.067(2) 0.055(2) 0.062(2) 0.0128(16) 0.0184(16) 0.0258(17) C8 0.0582(18) 0.055(2) 0.065(2) 0.0042(15) 0.0358(16) 0.0113(16) C9 0.0437(15) 0.0320(15) 0.0383(14) -0.0021(11) 0.0077(12) -0.0061(12) C10 0.0342(14) 0.0432(17) 0.0323(14) 0.0062(12) 0.0047(11) -0.0049(13) C11 0.0376(15) 0.0501(18) 0.0441(16) 0.0018(13) -0.0013(12) -0.0092(14) C12 0.064(2) 0.080(3) 0.147(4) 0.042(3) -0.035(2) -0.038(2) C13 0.0502(18) 0.092(3) 0.0484(19) -0.0116(17) -0.0076(15) 0.0035(19) C14 0.0313(15) 0.124(3) 0.064(2) -0.022(2) 0.0064(15) -0.0145(19) C15 0.0285(13) 0.0411(16) 0.0344(14) 0.0045(12) 0.0097(11) 0.0016(12) C16 0.0240(12) 0.0312(14) 0.0349(13) 0.0018(11) 0.0081(10) -0.0002(11) C17 0.0243(12) 0.0311(14) 0.0353(13) -0.0010(11) 0.0108(10) 0.0007(11) C18 0.0294(12) 0.0334(14) 0.0330(13) 0.0018(11) 0.0094(10) -0.0026(11) C19 0.0353(14) 0.0443(17) 0.0338(14) 0.0065(12) 0.0109(11) 0.0024(12) C20 0.0567(18) 0.069(2) 0.0384(16) 0.0156(15) 0.0127(14) 0.0065(17) C21 0.0486(16) 0.0564(19) 0.0387(15) -0.0011(13) 0.0164(13) -0.0167(15) C22 0.0381(14) 0.0583(19) 0.0394(15) -0.0065(13) 0.0148(12) -0.0120(14) C23 0.0299(13) 0.0364(15) 0.0383(14) 0.0062(11) 0.0075(11) 0.0016(12) C24 0.0255(12) 0.0301(14) 0.0397(14) -0.0003(11) 0.0090(11) -0.0010(11) C25 0.0327(13) 0.0340(15) 0.0575(17) 0.0009(13) 0.0187(13) 0.0024(12) C26 0.0458(16) 0.0377(17) 0.0591(18) -0.0069(14) 0.0094(14) 0.0051(14) C27 0.0278(14) 0.0486(19) 0.094(2) -0.0066(17) 0.0078(15) 0.0000(14) C28 0.070(2) 0.064(2) 0.090(3) 0.0184(19) 0.056(2) 0.0277(18) C29 0.0297(12) 0.0337(15) 0.0344(14) -0.0002(11) 0.0120(11) -0.0007(11) C30 0.0301(13) 0.0298(14) 0.0336(13) 0.0028(11) 0.0110(11) 0.0062(11) C31 0.0326(13) 0.0276(14) 0.0408(14) 0.0068(11) 0.0163(11) 0.0056(11) C32 0.0491(16) 0.0344(15) 0.0374(15) 0.0024(11) 0.0199(12) 0.0022(13) C33 0.079(2) 0.0484(19) 0.0342(15) -0.0060(13) 0.0206(15) -0.0121(17) C34 0.070(2) 0.076(2) 0.0416(18) 0.0004(16) 0.0006(15) -0.0094(19) C35 0.116(3) 0.058(2) 0.056(2) -0.0176(17) 0.033(2) -0.020(2) C36 0.110(3) 0.089(3) 0.0411(19) -0.0082(17) 0.0304(19) -0.022(2) C37 0.0585(18) 0.0451(17) 0.0408(16) 0.0071(13) 0.0292(14) 0.0044(14) C38 0.0401(14) 0.0389(16) 0.0454(16) 0.0094(12) 0.0192(13) 0.0047(13) C39 0.0447(16) 0.064(2) 0.0608(19) 0.0173(16) 0.0270(15) -0.0010(16) C40 0.062(2) 0.078(3) 0.091(3) 0.011(2) 0.0235(19) -0.018(2) C41 0.0425(19) 0.117(4) 0.142(4) 0.065(3) 0.037(2) 0.011(2) C42 0.073(2) 0.122(4) 0.091(3) 0.016(2) 0.052(2) -0.021(2) C43 0.0332(13) 0.0366(15) 0.0389(14) 0.0059(11) 0.0136(11) -0.0007(12) C44 0.0325(13) 0.0385(15) 0.0265(13) 0.0036(11) 0.0086(10) 0.0044(12) C45 0.0298(13) 0.0430(16) 0.0333(14) 0.0009(11) 0.0041(11) 0.0036(12) C46 0.0264(12) 0.0331(14) 0.0360(14) 0.0011(11) 0.0034(11) -0.0046(11) C47 0.0275(13) 0.0463(17) 0.0363(14) 0.0065(12) 0.0070(11) -0.0002(12) C48 0.0295(13) 0.0512(18) 0.0349(14) 0.0009(12) 0.0037(11) 0.0029(13) C49 0.0461(16) 0.058(2) 0.0491(17) 0.0011(14) 0.0097(14) 0.0120(15) C50 0.065(2) 0.080(3) 0.057(2) 0.0001(18) 0.0190(17) 0.026(2) C51 0.0514(19) 0.112(3) 0.0491(19) 0.006(2) 0.0201(16) 0.021(2) C52 0.0407(16) 0.087(3) 0.0486(18) 0.0124(17) 0.0121(14) 0.0037(17) C53 0.0324(14) 0.0576(19) 0.0417(16) 0.0046(14) 0.0075(12) -0.0004(14) C54 0.0276(13) 0.0425(16) 0.0409(15) 0.0104(12) 0.0074(11) 0.0117(12) C55 0.0340(14) 0.0480(18) 0.0442(16) 0.0004(13) 0.0092(12) 0.0041(13) C56 0.0377(15) 0.070(2) 0.0541(19) -0.0103(16) 0.0041(14) -0.0005(15) C57 0.0400(17) 0.103(3) 0.0445(18) -0.0073(18) 0.0027(14) 0.0141(19) C58 0.0451(18) 0.104(3) 0.0375(17) 0.0151(17) 0.0088(14) 0.0158(19) C59 0.0373(15) 0.071(2) 0.0466(17) 0.0172(15) 0.0097(13) 0.0049(15) C60 0.0252(12) 0.0383(15) 0.0341(13) -0.0029(11) 0.0112(10) -0.0032(11) C61 0.0288(13) 0.0328(15) 0.0452(15) -0.0034(11) 0.0136(11) 0.0000(11) C62 0.0332(13) 0.0339(15) 0.0283(13) -0.0022(11) 0.0150(11) 0.0023(12) C63 0.0321(13) 0.0337(15) 0.0333(13) -0.0041(11) 0.0100(11) 0.0019(11) C64 0.0367(15) 0.071(2) 0.0386(16) -0.0087(14) 0.0086(12) -0.0095(15) C65 0.0417(19) 0.149(4) 0.083(3) -0.058(3) 0.0209(18) -0.024(2) C66 0.073(3) 0.205(6) 0.098(3) -0.075(4) 0.045(3) -0.070(4) C67 0.108(4) 0.156(5) 0.070(3) -0.018(3) 0.021(3) -0.092(4) C68 0.111(3) 0.080(3) 0.081(3) 0.004(2) -0.004(2) -0.044(3) C69 0.058(2) 0.055(2) 0.073(2) 0.0040(17) 0.0016(17) -0.0178(18) C70 0.0412(15) 0.0335(15) 0.0366(14) -0.0029(11) -0.0014(12) 0.0022(13) C71 0.074(2) 0.0451(19) 0.0429(18) -0.0032(14) -0.0013(15) 0.0216(17) C72 0.103(3) 0.045(2) 0.0390(18) 0.0074(14) -0.0049(18) 0.016(2) C73 0.082(2) 0.0472(19) 0.0351(16) 0.0006(13) 0.0069(15) -0.0074(18) C74 0.0539(17) 0.057(2) 0.0407(16) 0.0052(14) 0.0121(14) 0.0038(16) C75 0.0442(15) 0.0443(17) 0.0379(15) 0.0082(12) 0.0070(12) 0.0058(13) C76 0.0383(14) 0.0285(14) 0.0381(14) 0.0049(11) 0.0137(11) 0.0036(12) C77 0.0383(14) 0.0299(14) 0.0365(14) 0.0036(11) 0.0093(11) -0.0020(12) C78 0.0391(14) 0.0292(14) 0.0281(13) -0.0014(10) 0.0109(11) 0.0042(12) C79 0.0492(16) 0.0444(17) 0.0447(16) 0.0120(13) 0.0238(13) 0.0119(14) C80 0.0400(14) 0.0327(15) 0.0290(13) 0.0035(11) 0.0069(11) 0.0009(12) C81 0.0579(19) 0.052(2) 0.0582(19) -0.0205(15) 0.0188(15) -0.0079(16) C82 0.064(2) 0.060(2) 0.073(2) -0.0213(18) 0.0132(18) -0.0232(19) C83 0.0456(18) 0.066(2) 0.089(3) -0.002(2) 0.0094(18) -0.0192(18) C84 0.0448(18) 0.060(2) 0.116(3) -0.012(2) 0.0289(19) -0.0025(17) C85 0.0397(16) 0.0394(17) 0.078(2) -0.0091(15) 0.0177(15) -0.0021(14) C86 0.0348(13) 0.0349(15) 0.0328(14) 0.0041(11) 0.0110(11) -0.0030(12) C87 0.0635(18) 0.0364(16) 0.0362(15) 0.0046(12) 0.0071(13) 0.0076(15) C88 0.070(2) 0.051(2) 0.054(2) 0.0170(15) 0.0143(16) 0.0202(17) C89 0.0498(17) 0.071(2) 0.0397(17) 0.0211(15) 0.0065(14) 0.0118(17) C90 0.0461(16) 0.065(2) 0.0327(15) 0.0060(14) 0.0049(13) -0.0054(16) C91 0.0370(14) 0.0428(16) 0.0355(14) 0.0014(12) 0.0122(12) -0.0050(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O5 1.4833(19) . ? P1 C47 1.797(3) . ? P1 C54 1.809(3) . ? P1 C48 1.814(3) . ? P2 O7 1.487(2) . ? P2 C64 1.798(3) . ? P2 C70 1.803(3) . ? P2 C63 1.807(2) . ? P3 O9 1.4872(18) . ? P3 C80 1.798(3) . ? P3 C86 1.804(2) . ? P3 C79 1.812(3) . ? N1 C46 1.336(3) . ? N1 C45 1.444(3) . ? N2 C62 1.329(3) . ? N2 C61 1.451(3) . ? N3 C78 1.327(3) . ? N3 C77 1.449(3) . ? O1 C3 1.397(3) . ? O1 C44 1.438(3) . ? O2 C17 1.400(3) . ? O2 C60 1.439(3) . ? O3 C31 1.401(3) . ? O3 C76 1.439(3) . ? O4 C46 1.225(3) . ? O6 C62 1.236(3) . ? O8 C78 1.230(3) . ? C1 C2 1.536(3) . ? C1 C30 1.537(3) . ? C1 C16 1.537(3) . ? C2 C15 1.387(3) . ? C2 C3 1.397(3) . ? C3 C4 1.402(3) . ? C4 C9 1.396(3) . ? C4 C5 1.545(3) . ? C5 C7 1.523(4) . ? C5 C8 1.523(4) . ? C5 C6 1.541(4) . ? C9 C10 1.391(4) . ? C10 C15 1.394(4) . ? C10 C11 1.534(3) . ? C11 C12 1.523(5) . ? C11 C13 1.529(4) . ? C11 C14 1.536(4) . ? C16 C29 1.396(3) . ? C16 C17 1.397(3) . ? C17 C18 1.409(3) . ? C18 C23 1.388(3) . ? C18 C19 1.550(3) . ? C19 C22 1.527(4) . ? C19 C21 1.539(3) . ? C19 C20 1.541(4) . ? C23 C24 1.384(3) . ? C24 C29 1.385(3) . ? C24 C25 1.532(3) . ? C25 C28 1.529(4) . ? C25 C26 1.538(4) . ? C25 C27 1.538(4) . ? C30 C43 1.388(3) . ? C30 C31 1.406(3) . ? C31 C32 1.399(3) . ? C32 C37 1.403(4) . ? C32 C33 1.551(4) . ? C33 C35 1.519(4) . ? C33 C36 1.540(4) . ? C33 C34 1.551(4) . ? C37 C38 1.380(4) . ? C38 C43 1.392(3) . ? C38 C39 1.537(4) . ? C39 C41 1.504(4) . ? C39 C42 1.534(4) . ? C39 C40 1.549(5) . ? C44 C45 1.515(3) . ? C46 C47 1.524(3) . ? C48 C49 1.390(4) . ? C48 C53 1.392(4) . ? C49 C50 1.390(4) . ? C50 C51 1.379(5) . ? C51 C52 1.379(5) . ? C52 C53 1.394(4) . ? C54 C55 1.386(4) . ? C54 C59 1.394(4) . ? C55 C56 1.391(4) . ? C56 C57 1.376(4) . ? C57 C58 1.364(5) . ? C58 C59 1.381(4) . ? C60 C61 1.516(3) . ? C62 C63 1.514(3) . ? C64 C69 1.384(4) . ? C64 C65 1.390(4) . ? C65 C66 1.359(6) . ? C66 C67 1.369(7) . ? C67 C68 1.404(7) . ? C68 C69 1.391(5) . ? C70 C75 1.386(4) . ? C70 C71 1.392(4) . ? C71 C72 1.374(5) . ? C72 C73 1.373(5) . ? C73 C74 1.379(4) . ? C74 C75 1.384(4) . ? C76 C77 1.511(3) . ? C78 C79 1.509(3) . ? C80 C85 1.377(4) . ? C80 C81 1.392(4) . ? C81 C82 1.376(4) . ? C82 C83 1.361(5) . ? C83 C84 1.378(5) . ? C84 C85 1.384(4) . ? C86 C91 1.387(3) . ? C86 C87 1.389(4) . ? C87 C88 1.385(4) . ? C88 C89 1.383(4) . ? C89 C90 1.366(4) . ? C90 C91 1.385(4) . ? 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 O5 P1 C47 114.01(11) . . ? O5 P1 C54 111.23(12) . . ? C47 P1 C54 109.39(12) . . ? O5 P1 C48 110.98(12) . . ? C47 P1 C48 102.94(12) . . ? C54 P1 C48 107.84(11) . . ? O7 P2 C64 111.72(14) . . ? O7 P2 C70 111.69(13) . . ? C64 P2 C70 105.22(12) . . ? O7 P2 C63 116.08(12) . . ? C64 P2 C63 102.60(13) . . ? C70 P2 C63 108.63(11) . . ? O9 P3 C80 111.74(11) . . ? O9 P3 C86 111.35(11) . . ? C80 P3 C86 107.30(11) . . ? O9 P3 C79 114.96(12) . . ? C80 P3 C79 108.04(13) . . ? C86 P3 C79 102.85(12) . . ? C46 N1 C45 124.3(2) . . ? C62 N2 C61 124.5(2) . . ? C78 N3 C77 122.6(2) . . ? C3 O1 C44 114.53(17) . . ? C17 O2 C60 113.65(17) . . ? C31 O3 C76 114.59(17) . . ? C2 C1 C30 112.67(19) . . ? C2 C1 C16 110.46(19) . . ? C30 C1 C16 112.90(19) . . ? C15 C2 C3 119.2(2) . . ? C15 C2 C1 119.6(2) . . ? C3 C2 C1 121.2(2) . . ? O1 C3 C2 118.4(2) . . ? O1 C3 C4 119.7(2) . . ? C2 C3 C4 121.6(2) . . ? C9 C4 C3 116.1(2) . . ? C9 C4 C5 120.4(2) . . ? C3 C4 C5 123.4(2) . . ? C7 C5 C8 109.1(2) . . ? C7 C5 C6 107.5(3) . . ? C8 C5 C6 106.6(2) . . ? C7 C5 C4 112.4(2) . . ? C8 C5 C4 109.5(2) . . ? C6 C5 C4 111.7(2) . . ? C10 C9 C4 124.3(2) . . ? C9 C10 C15 116.9(2) . . ? C9 C10 C11 120.3(2) . . ? C15 C10 C11 122.7(2) . . ? C12 C11 C13 109.3(3) . . ? C12 C11 C10 110.6(2) . . ? C13 C11 C10 108.4(2) . . ? C12 C11 C14 109.2(3) . . ? C13 C11 C14 107.6(2) . . ? C10 C11 C14 111.8(2) . . ? C2 C15 C10 121.6(2) . . ? C29 C16 C17 118.6(2) . . ? C29 C16 C1 121.0(2) . . ? C17 C16 C1 120.5(2) . . ? C16 C17 O2 118.6(2) . . ? C16 C17 C18 121.5(2) . . ? O2 C17 C18 119.8(2) . . ? C23 C18 C17 116.4(2) . . ? C23 C18 C19 120.3(2) . . ? C17 C18 C19 123.2(2) . . ? C22 C19 C21 110.4(2) . . ? C22 C19 C20 107.7(2) . . ? C21 C19 C20 106.6(2) . . ? C22 C19 C18 108.5(2) . . ? C21 C19 C18 111.6(2) . . ? C20 C19 C18 112.0(2) . . ? C24 C23 C18 124.1(2) . . ? C23 C24 C29 117.5(2) . . ? C23 C24 C25 119.3(2) . . ? C29 C24 C25 123.3(2) . . ? C28 C25 C24 112.1(2) . . ? C28 C25 C26 108.6(2) . . ? C24 C25 C26 108.8(2) . . ? C28 C25 C27 108.7(2) . . ? C24 C25 C27 109.5(2) . . ? C26 C25 C27 109.1(2) . . ? C24 C29 C16 121.8(2) . . ? C43 C30 C31 117.6(2) . . ? C43 C30 C1 121.1(2) . . ? C31 C30 C1 121.2(2) . . ? C32 C31 O3 118.7(2) . . ? C32 C31 C30 122.0(2) . . ? O3 C31 C30 119.2(2) . . ? C31 C32 C37 116.3(2) . . ? C31 C32 C33 122.8(2) . . ? C37 C32 C33 120.8(2) . . ? C35 C33 C36 107.9(3) . . ? C35 C33 C34 109.9(3) . . ? C36 C33 C34 106.4(3) . . ? C35 C33 C32 111.4(3) . . ? C36 C33 C32 111.8(3) . . ? C34 C33 C32 109.2(2) . . ? C38 C37 C32 124.0(2) . . ? C37 C38 C43 116.8(2) . . ? C37 C38 C39 123.5(2) . . ? C43 C38 C39 119.7(2) . . ? C41 C39 C42 110.7(3) . . ? C41 C39 C38 109.3(2) . . ? C42 C39 C38 112.0(3) . . ? C41 C39 C40 108.5(3) . . ? C42 C39 C40 106.2(3) . . ? C38 C39 C40 110.1(2) . . ? C30 C43 C38 122.9(2) . . ? O1 C44 C45 107.17(19) . . ? N1 C45 C44 112.4(2) . . ? O4 C46 N1 123.3(2) . . ? O4 C46 C47 122.7(2) . . ? N1 C46 C47 114.0(2) . . ? C46 C47 P1 115.98(17) . . ? C49 C48 C53 119.4(3) . . ? C49 C48 P1 116.7(2) . . ? C53 C48 P1 123.9(2) . . ? C50 C49 C48 120.4(3) . . ? C51 C50 C49 119.7(3) . . ? C52 C51 C50 120.6(3) . . ? C51 C52 C53 119.9(3) . . ? C48 C53 C52 120.0(3) . . ? C55 C54 C59 118.5(3) . . ? C55 C54 P1 123.6(2) . . ? C59 C54 P1 117.8(2) . . ? C54 C55 C56 120.2(3) . . ? C57 C56 C55 120.3(3) . . ? C58 C57 C56 119.8(3) . . ? C57 C58 C59 120.6(3) . . ? C58 C59 C54 120.5(3) . . ? O2 C60 C61 108.31(19) . . ? N2 C61 C60 108.3(2) . . ? O6 C62 N2 124.2(2) . . ? O6 C62 C63 121.6(2) . . ? N2 C62 C63 114.2(2) . . ? C62 C63 P2 116.44(18) . . ? C69 C64 C65 118.8(3) . . ? C69 C64 P2 123.5(2) . . ? C65 C64 P2 117.7(3) . . ? C66 C65 C64 121.0(5) . . ? C65 C66 C67 120.5(4) . . ? C66 C67 C68 120.4(4) . . ? C69 C68 C67 118.4(5) . . ? C64 C69 C68 120.9(4) . . ? C75 C70 C71 118.2(3) . . ? C75 C70 P2 124.5(2) . . ? C71 C70 P2 117.3(2) . . ? C72 C71 C70 121.2(3) . . ? C73 C72 C71 120.0(3) . . ? C72 C73 C74 119.9(3) . . ? C73 C74 C75 120.1(3) . . ? C74 C75 C70 120.6(3) . . ? O3 C76 C77 106.35(19) . . ? N3 C77 C76 109.5(2) . . ? O8 C78 N3 123.5(2) . . ? O8 C78 C79 121.7(2) . . ? N3 C78 C79 114.7(2) . . ? C78 C79 P3 113.33(18) . . ? C85 C80 C81 118.7(2) . . ? C85 C80 P3 118.3(2) . . ? C81 C80 P3 122.9(2) . . ? C82 C81 C80 120.6(3) . . ? C83 C82 C81 120.1(3) . . ? C82 C83 C84 120.3(3) . . ? C83 C84 C85 119.9(3) . . ? C80 C85 C84 120.4(3) . . ? C91 C86 C87 119.2(2) . . ? C91 C86 P3 117.3(2) . . ? C87 C86 P3 123.41(19) . . ? C88 C87 C86 119.9(3) . . ? C89 C88 C87 120.2(3) . . ? C90 C89 C88 119.9(3) . . ? C89 C90 C91 120.4(3) . . ? C90 C91 C86 120.2(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.72 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.391 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.043 #===END data_15_li_picrate_complex _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; tris(3,5-di-tert-butyl-2-(2-(carbamoylmethylphosphineoxide)ethoxy)phen yl)methane lithium picrate complex ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C101 H118 Cl12 Li N6 O16 P3' _chemical_formula_weight 2197.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0906(11) _cell_length_b 16.7425(15) _cell_length_c 28.071(3) _cell_angle_alpha 102.015(2) _cell_angle_beta 91.830(2) _cell_angle_gamma 100.091(2) _cell_volume 5458.0(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2292 _exptl_absorpt_coefficient_mu 0.412 _exptl_absorpt_correction_type 'SADABS' _exptl_absorpt_correction_T_min 0.7210 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28811 _diffrn_reflns_av_R_equivalents 0.0621 _diffrn_reflns_av_sigmaI/netI 0.1426 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 24.50 _reflns_number_total 18059 _reflns_number_gt 8877 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One chloroform molecule was "SQUEEZED" from the asymmetric unit' ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0934P)^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 18059 _refine_ls_number_parameters 1373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1605 _refine_ls_R_factor_gt 0.0798 _refine_ls_wR_factor_ref 0.2073 _refine_ls_wR_factor_gt 0.1736 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.962 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 1.1113(7) 0.4920(5) 0.2301(3) 0.029(2) Uani 1 1 d . . . P1 P 1.31213(11) 0.44281(8) 0.27748(5) 0.0276(3) Uani 1 1 d . . . P2 P 1.17383(12) 0.48076(8) 0.12897(5) 0.0290(3) Uani 1 1 d . . . P3 P 0.85357(11) 0.42927(8) 0.25875(5) 0.0272(3) Uani 1 1 d . . . O1 O 1.3050(3) 0.75197(19) 0.34045(12) 0.0278(8) Uani 1 1 d . . . O2 O 1.2378(3) 0.83990(18) 0.22440(11) 0.0254(8) Uani 1 1 d . . . O3 O 0.9831(3) 0.78979(18) 0.31477(11) 0.0251(8) Uani 1 1 d . . . O4 O 1.5535(3) 0.6128(2) 0.25465(13) 0.0382(9) Uani 1 1 d . . . O5 O 1.2124(3) 0.48547(19) 0.28380(12) 0.0297(8) Uani 1 1 d . . . O6 O 1.1228(3) 0.60811(19) 0.21989(12) 0.0296(8) Uani 1 1 d . . . O7 O 1.1775(3) 0.4419(2) 0.17217(12) 0.0326(9) Uani 1 1 d . . . O8 O 0.8141(3) 0.5954(2) 0.35133(14) 0.0374(9) Uani 1 1 d . . . O9 O 0.9636(3) 0.4433(2) 0.23712(12) 0.0320(8) Uani 1 1 d . . . N1 N 1.3739(4) 0.6292(2) 0.26324(16) 0.0295(11) Uani 1 1 d . . . H1 H 1.304(5) 0.608(4) 0.266(2) 0.06(2) Uiso 1 1 d . . . N2 N 1.1107(3) 0.6973(2) 0.16986(17) 0.0276(10) Uani 1 1 d . . . H2 H 1.119(4) 0.698(3) 0.1395(19) 0.027(15) Uiso 1 1 d . . . N3 N 0.9559(4) 0.6204(2) 0.30355(19) 0.0302(11) Uani 1 1 d . . . H3 H 0.970(4) 0.615(3) 0.2776(16) 0.009(15) Uiso 1 1 d . . . C1 C 1.2046(4) 0.8882(3) 0.32647(17) 0.0225(11) Uani 1 1 d . . . H1A H 1.1838 0.8308 0.3057 0.027 Uiso 1 1 calc R . . C2 C 1.2474(4) 0.8793(3) 0.37646(17) 0.0250(11) Uani 1 1 d . A . C3 C 1.2937(4) 0.8099(3) 0.38258(18) 0.0259(12) Uani 1 1 d . . . C4 C 1.3193(4) 0.7966(3) 0.42862(19) 0.0302(12) Uani 1 1 d . A . C5 C 1.3552(5) 0.7168(3) 0.4385(2) 0.0375(14) Uani 1 1 d . . . C6 C 1.2676(10) 0.6402(9) 0.4134(7) 0.059(4) Uani 0.70 1 d P A 11 H6A H 1.2618 0.6373 0.3782 0.089 Uiso 0.70 1 calc PR A 11 H6B H 1.1942 0.6446 0.4265 0.089 Uiso 0.70 1 calc PR A 11 H6C H 1.2910 0.5899 0.4196 0.089 Uiso 0.70 1 calc PR A 11 C7 C 1.3731(13) 0.7193(8) 0.4902(5) 0.078(4) Uani 0.70 1 d P A 11 H7A H 1.4334 0.7661 0.5048 0.118 Uiso 0.70 1 calc PR A 11 H7B H 1.3945 0.6673 0.4945 0.118 Uiso 0.70 1 calc PR A 11 H7C H 1.3035 0.7263 0.5063 0.118 Uiso 0.70 1 calc PR A 11 C8 C 1.4707(8) 0.7067(6) 0.4158(4) 0.063(3) Uani 0.70 1 d P A 11 H8A H 1.5276 0.7564 0.4293 0.095 Uiso 0.70 1 calc PR A 11 H8B H 1.4613 0.6995 0.3802 0.095 Uiso 0.70 1 calc PR A 11 H8C H 1.4952 0.6579 0.4236 0.095 Uiso 0.70 1 calc PR A 11 C6' C 1.297(2) 0.6961(17) 0.4867(10) 0.052(8) Uani 0.30 1 d P A 12 H6'A H 1.3335 0.7365 0.5157 0.078 Uiso 0.30 1 calc PR A 12 H6'B H 1.3041 0.6400 0.4896 0.078 Uiso 0.30 1 calc PR A 12 H6'C H 1.2165 0.6995 0.4840 0.078 Uiso 0.30 1 calc PR A 12 C7' C 1.4785(19) 0.7294(14) 0.4531(9) 0.052(6) Uiso 0.30 1 d P A 12 H7'A H 1.4945 0.7651 0.4859 0.078 Uiso 0.30 1 calc PR A 12 H7'B H 1.5221 0.7557 0.4298 0.078 Uiso 0.30 1 calc PR A 12 H7'C H 1.4995 0.6755 0.4532 0.078 Uiso 0.30 1 calc PR A 12 C8' C 1.322(2) 0.6397(17) 0.4001(13) 0.045(8) Uani 0.30 1 d P A 12 H8'A H 1.3482 0.6498 0.3689 0.067 Uiso 0.30 1 calc PR A 12 H8'B H 1.2398 0.6230 0.3972 0.067 Uiso 0.30 1 calc PR A 12 H8'C H 1.3560 0.5953 0.4090 0.067 Uiso 0.30 1 calc PR A 12 C9 C 1.3106(4) 0.8603(3) 0.46866(19) 0.0351(13) Uani 1 1 d . . . H9A H 1.3324 0.8544 0.5004 0.042 Uiso 1 1 calc R A . C10 C 1.2708(5) 0.9329(3) 0.46410(19) 0.0350(13) Uani 1 1 d . A . C11 C 1.2633(5) 1.0002(3) 0.5090(2) 0.0437(15) Uani 1 1 d . . . C12 C 1.2103(15) 1.0710(8) 0.4969(4) 0.060(4) Uani 0.50 1 d P A 1 H12A H 1.1351 1.0483 0.4806 0.090 Uiso 0.50 1 calc PR A 1 H12B H 1.2577 1.0988 0.4752 0.090 Uiso 0.50 1 calc PR A 1 H12C H 1.2042 1.1112 0.5271 0.090 Uiso 0.50 1 calc PR A 1 C13 C 1.3766(13) 1.0360(9) 0.5341(5) 0.061(4) Uani 0.50 1 d P A 1 H13A H 1.4079 0.9924 0.5453 0.092 Uiso 0.50 1 calc PR A 1 H13B H 1.3702 1.0805 0.5621 0.092 Uiso 0.50 1 calc PR A 1 H13C H 1.4263 1.0587 0.5113 0.092 Uiso 0.50 1 calc PR A 1 C14 C 1.1846(12) 0.9600(7) 0.5458(4) 0.052(3) Uani 0.50 1 d P A 1 H14A H 1.2098 0.9098 0.5511 0.078 Uiso 0.50 1 calc PR A 1 H14B H 1.1065 0.9455 0.5319 0.078 Uiso 0.50 1 calc PR A 1 H14C H 1.1893 1.0001 0.5770 0.078 Uiso 0.50 1 calc PR A 1 C12' C 1.3302(14) 1.0860(8) 0.4995(5) 0.072(4) Uani 0.50 1 d P A 2 H12D H 1.2989 1.0963 0.4692 0.107 Uiso 0.50 1 calc PR A 2 H12E H 1.4100 1.0829 0.4967 0.107 Uiso 0.50 1 calc PR A 2 H12F H 1.3227 1.1314 0.5268 0.107 Uiso 0.50 1 calc PR A 2 C13' C 1.323(2) 0.9894(13) 0.5547(6) 0.104(7) Uani 0.50 1 d P A 2 H13D H 1.2859 0.9377 0.5633 0.155 Uiso 0.50 1 calc PR A 2 H13E H 1.3190 1.0365 0.5816 0.155 Uiso 0.50 1 calc PR A 2 H13F H 1.4016 0.9867 0.5490 0.155 Uiso 0.50 1 calc PR A 2 C14' C 1.1469(14) 1.0092(11) 0.5148(6) 0.090(5) Uiso 0.50 1 d P A 2 H14D H 1.1042 0.9586 0.5225 0.135 Uiso 0.50 1 calc PR A 2 H14E H 1.1141 1.0182 0.4845 0.135 Uiso 0.50 1 calc PR A 2 H14F H 1.1440 1.0569 0.5415 0.135 Uiso 0.50 1 calc PR A 2 C15 C 1.2371(4) 0.9382(3) 0.41782(17) 0.0248(11) Uani 1 1 d . . . H15A H 1.2051 0.9847 0.4141 0.030 Uiso 1 1 calc R A . C16 C 1.2940(4) 0.9361(3) 0.30077(18) 0.0238(11) Uani 1 1 d . B . C17 C 1.3045(4) 0.9128(3) 0.25068(18) 0.0259(12) Uani 1 1 d . . . C18 C 1.3905(4) 0.9556(3) 0.22763(18) 0.0282(12) Uani 1 1 d . . . C19 C 1.4151(4) 0.9260(3) 0.17410(19) 0.0331(13) Uani 1 1 d . . . C20 C 1.4459(5) 0.8388(3) 0.1665(2) 0.0515(17) Uani 1 1 d . . . H20A H 1.5062 0.8394 0.1908 0.077 Uiso 1 1 calc R . . H20B H 1.4715 0.8235 0.1337 0.077 Uiso 1 1 calc R . . H20C H 1.3795 0.7983 0.1703 0.077 Uiso 1 1 calc R . . C21 C 1.3159(5) 0.9238(4) 0.1386(2) 0.0491(16) Uani 1 1 d . . . H21A H 1.2844 0.9744 0.1485 0.074 Uiso 1 1 calc R . . H21B H 1.2578 0.8751 0.1387 0.074 Uiso 1 1 calc R . . H21C H 1.3417 0.9206 0.1056 0.074 Uiso 1 1 calc R . . C22 C 1.5162(6) 0.9827(4) 0.1594(2) 0.063(2) Uani 1 1 d . . . H22A H 1.5837 0.9826 0.1797 0.095 Uiso 1 1 calc R . . H22B H 1.5013 1.0394 0.1641 0.095 Uiso 1 1 calc R . . H22C H 1.5281 0.9623 0.1250 0.095 Uiso 1 1 calc R . . C23 C 1.4557(4) 1.0269(3) 0.2567(2) 0.0303(13) Uani 1 1 d . . . H23A H 1.5109 1.0592 0.2417 0.036 Uiso 1 1 calc R . . C24 C 1.4453(4) 1.0538(3) 0.3065(2) 0.0293(13) Uani 1 1 d . B . C25 C 1.5192(4) 1.1341(3) 0.33622(19) 0.0304(13) Uani 1 1 d . . . C26 C 1.5866(9) 1.1076(6) 0.3773(4) 0.038(3) Uani 0.50 1 d P B 3 H26A H 1.5337 1.0805 0.3974 0.058 Uiso 0.50 1 calc PR B 3 H26B H 1.6342 1.1570 0.3979 0.058 Uiso 0.50 1 calc PR B 3 H26C H 1.6341 1.0689 0.3623 0.058 Uiso 0.50 1 calc PR B 3 C27 C 1.4511(9) 1.1947(6) 0.3573(4) 0.030(2) Uani 0.50 1 d P B 3 H27A H 1.3968 1.1700 0.3778 0.044 Uiso 0.50 1 calc PR B 3 H27B H 1.4105 1.2107 0.3311 0.044 Uiso 0.50 1 calc PR B 3 H27C H 1.5001 1.2440 0.3772 0.044 Uiso 0.50 1 calc PR B 3 C28 C 1.6104(10) 1.1709(7) 0.3037(4) 0.046(3) Uani 0.50 1 d P B 3 H28A H 1.6496 1.1271 0.2879 0.068 Uiso 0.50 1 calc PR B 3 H28B H 1.6648 1.2161 0.3244 0.068 Uiso 0.50 1 calc PR B 3 H28C H 1.5734 1.1923 0.2788 0.068 Uiso 0.50 1 calc PR B 3 C26' C 1.4850(11) 1.1580(8) 0.3900(4) 0.055(4) Uani 0.50 1 d P B 4 H26D H 1.4057 1.1637 0.3897 0.082 Uiso 0.50 1 calc PR B 4 H26E H 1.5322 1.2108 0.4067 0.082 Uiso 0.50 1 calc PR B 4 H26F H 1.4959 1.1144 0.4073 0.082 Uiso 0.50 1 calc PR B 4 C27' C 1.4906(10) 1.2081(7) 0.3143(5) 0.057(4) Uani 0.50 1 d P B 4 H27D H 1.4088 1.2051 0.3122 0.085 Uiso 0.50 1 calc PR B 4 H27E H 1.5181 1.2041 0.2816 0.085 Uiso 0.50 1 calc PR B 4 H27F H 1.5270 1.2611 0.3354 0.085 Uiso 0.50 1 calc PR B 4 C28' C 1.6387(10) 1.1341(8) 0.3352(6) 0.062(4) Uani 0.50 1 d P B 4 H28D H 1.6558 1.0862 0.3471 0.093 Uiso 0.50 1 calc PR B 4 H28E H 1.6805 1.1855 0.3561 0.093 Uiso 0.50 1 calc PR B 4 H28F H 1.6608 1.1304 0.3016 0.093 Uiso 0.50 1 calc PR B 4 C29 C 1.3661(4) 1.0076(3) 0.32821(18) 0.0224(11) Uani 1 1 d . . . H29A H 1.3594 1.0237 0.3623 0.027 Uiso 1 1 calc R B . C30 C 1.0968(4) 0.9258(3) 0.32901(17) 0.0221(11) Uani 1 1 d . C . C31 C 0.9893(4) 0.8757(3) 0.32214(17) 0.0241(11) Uani 1 1 d . . . C32 C 0.8912(4) 0.9075(3) 0.31740(16) 0.0225(11) Uani 1 1 d . . . C33 C 0.7749(4) 0.8525(3) 0.30134(19) 0.0291(12) Uani 1 1 d . . . C34 C 0.7807(5) 0.7943(3) 0.2512(2) 0.0424(15) Uani 1 1 d . . . H34A H 0.7986 0.8277 0.2267 0.064 Uiso 1 1 calc R . . H34B H 0.7078 0.7570 0.2416 0.064 Uiso 1 1 calc R . . H34C H 0.8393 0.7613 0.2535 0.064 Uiso 1 1 calc R . . C35 C 0.7352(4) 0.7998(3) 0.3381(2) 0.0381(14) Uani 1 1 d . . . H35A H 0.7829 0.7581 0.3381 0.057 Uiso 1 1 calc R . . H35B H 0.6569 0.7718 0.3291 0.057 Uiso 1 1 calc R . . H35C H 0.7404 0.8357 0.3708 0.057 Uiso 1 1 calc R . . C36 C 0.6842(5) 0.9026(3) 0.2946(2) 0.0434(15) Uani 1 1 d . . . H36A H 0.7085 0.9391 0.2722 0.065 Uiso 1 1 calc R . . H36B H 0.6719 0.9364 0.3262 0.065 Uiso 1 1 calc R . . H36C H 0.6140 0.8647 0.2809 0.065 Uiso 1 1 calc R . . C37 C 0.9047(4) 0.9935(3) 0.32605(17) 0.0279(12) Uani 1 1 d . . . H37A H 0.8390 1.0173 0.3254 0.034 Uiso 1 1 calc R . . C38 C 1.0093(4) 1.0471(3) 0.33575(18) 0.0269(12) Uani 1 1 d . C . C39 C 1.0163(5) 1.1418(3) 0.3464(2) 0.0406(15) Uani 1 1 d . . . C40 C 0.9491(9) 1.1673(5) 0.3060(4) 0.057(3) Uani 0.70 1 d P C 5 H40A H 0.9819 1.1518 0.2747 0.085 Uiso 0.70 1 calc PR C 5 H40B H 0.9523 1.2275 0.3142 0.085 Uiso 0.70 1 calc PR C 5 H40C H 0.8705 1.1386 0.3036 0.085 Uiso 0.70 1 calc PR C 5 C41 C 0.9564(11) 1.1668(5) 0.3953(4) 0.074(3) Uani 0.70 1 d P C 5 H41A H 0.8837 1.1294 0.3938 0.111 Uiso 0.70 1 calc PR C 5 H41B H 0.9445 1.2242 0.3994 0.111 Uiso 0.70 1 calc PR C 5 H41C H 1.0042 1.1623 0.4232 0.111 Uiso 0.70 1 calc PR C 5 C42 C 1.1343(8) 1.1896(5) 0.3551(6) 0.095(5) Uani 0.70 1 d P C 5 H42A H 1.1751 1.1757 0.3257 0.142 Uiso 0.70 1 calc PR C 5 H42B H 1.1721 1.1751 0.3826 0.142 Uiso 0.70 1 calc PR C 5 H42C H 1.1332 1.2493 0.3625 0.142 Uiso 0.70 1 calc PR C 5 C40' C 0.9149(19) 1.1679(14) 0.3402(9) 0.055(6) Uiso 0.30 1 d P C 6 H40D H 0.8788 1.1404 0.3078 0.082 Uiso 0.30 1 calc PR C 6 H40E H 0.9291 1.2283 0.3432 0.082 Uiso 0.30 1 calc PR C 6 H40F H 0.8653 1.1535 0.3653 0.082 Uiso 0.30 1 calc PR C 6 C41' C 1.076(2) 1.1807(10) 0.3965(7) 0.043(5) Uani 0.30 1 d P C 6 H41D H 1.1521 1.1676 0.3974 0.065 Uiso 0.30 1 calc PR C 6 H41E H 1.0337 1.1584 0.4215 0.065 Uiso 0.30 1 calc PR C 6 H41F H 1.0818 1.2411 0.4030 0.065 Uiso 0.30 1 calc PR C 6 C42' C 1.093(2) 1.1703(11) 0.3062(8) 0.051(6) Uani 0.30 1 d P C 6 H42D H 1.0552 1.1459 0.2738 0.076 Uiso 0.30 1 calc PR C 6 H42E H 1.1651 1.1516 0.3085 0.076 Uiso 0.30 1 calc PR C 6 H42F H 1.1067 1.2310 0.3115 0.076 Uiso 0.30 1 calc PR C 6 C43 C 1.1029(4) 1.0112(3) 0.33591(17) 0.0257(12) Uani 1 1 d . . . H43A H 1.1750 1.0462 0.3409 0.031 Uiso 1 1 calc R C . C44 C 1.4057(4) 0.7710(3) 0.31712(19) 0.0320(13) Uani 1 1 d . . . H44A H 1.4700 0.7595 0.3357 0.038 Uiso 1 1 calc R . . H44B H 1.4208 0.8306 0.3161 0.038 Uiso 1 1 calc R . . C45 C 1.3935(4) 0.7186(3) 0.26589(19) 0.0306(13) Uani 1 1 d . . . H45A H 1.3300 0.7318 0.2477 0.037 Uiso 1 1 calc R . . H45B H 1.4628 0.7341 0.2494 0.037 Uiso 1 1 calc R . . C46 C 1.4533(4) 0.5826(3) 0.25444(17) 0.0279(12) Uani 1 1 d . . . C47 C 1.4125(4) 0.4895(3) 0.24073(18) 0.0299(12) Uani 1 1 d . . . H47A H 1.4793 0.4627 0.2408 0.036 Uiso 1 1 calc R . . H47B H 1.3789 0.4754 0.2067 0.036 Uiso 1 1 calc R . . C48 C 1.2734(5) 0.3354(3) 0.2470(2) 0.0367(14) Uani 1 1 d . . . C49 C 1.1633(5) 0.3020(3) 0.2287(2) 0.0482(16) Uani 1 1 d . . . H49A H 1.1074 0.3357 0.2338 0.058 Uiso 1 1 calc R . . C50 C 1.1340(6) 0.2216(4) 0.2034(3) 0.0616(19) Uani 1 1 d . . . H50A H 1.0585 0.2000 0.1906 0.074 Uiso 1 1 calc R . . C51 C 1.2137(8) 0.1720(5) 0.1964(3) 0.092(3) Uani 1 1 d . . . H51A H 1.1928 0.1158 0.1793 0.110 Uiso 1 1 calc R . . C52 C 1.3228(8) 0.2029(4) 0.2140(4) 0.103(3) Uani 1 1 d . . . H52A H 1.3778 0.1684 0.2088 0.123 Uiso 1 1 calc R . . C53 C 1.3530(6) 0.2847(4) 0.2396(3) 0.068(2) Uani 1 1 d . . . H53A H 1.4288 0.3061 0.2521 0.081 Uiso 1 1 calc R . . C54 C 1.3867(5) 0.4454(3) 0.33457(19) 0.0335(13) Uani 1 1 d . . . C55 C 1.3331(5) 0.4020(4) 0.3668(2) 0.0512(16) Uani 1 1 d . . . H55A H 1.2583 0.3719 0.3588 0.061 Uiso 1 1 calc R . . C56 C 1.3884(7) 0.4024(5) 0.4103(3) 0.066(2) Uani 1 1 d . . . H56A H 1.3520 0.3714 0.4320 0.080 Uiso 1 1 calc R . . C57 C 1.4962(7) 0.4475(5) 0.4230(3) 0.066(2) Uani 1 1 d . . . H57A H 1.5326 0.4494 0.4539 0.080 Uiso 1 1 calc R . . C58 C 1.5494(6) 0.4886(4) 0.3914(2) 0.0542(17) Uani 1 1 d . . . H58A H 1.6245 0.5180 0.3996 0.065 Uiso 1 1 calc R . . C59 C 1.4959(5) 0.4885(3) 0.3476(2) 0.0421(14) Uani 1 1 d . . . H59A H 1.5342 0.5183 0.3258 0.051 Uiso 1 1 calc R . . C60 C 1.1227(4) 0.8422(3) 0.21081(18) 0.0260(12) Uani 1 1 d . . . H60A H 1.1186 0.8634 0.1805 0.031 Uiso 1 1 calc R . . H60B H 1.0918 0.8795 0.2370 0.031 Uiso 1 1 calc R . . C61 C 1.0564(4) 0.7555(3) 0.20286(18) 0.0276(12) Uani 1 1 d . . . H61A H 1.0496 0.7387 0.2346 0.033 Uiso 1 1 calc R . . H61B H 0.9796 0.7540 0.1889 0.033 Uiso 1 1 calc R . . C62 C 1.1451(4) 0.6325(3) 0.18145(18) 0.0245(12) Uani 1 1 d . . . C63 C 1.2207(4) 0.5923(3) 0.14614(18) 0.0284(12) Uani 1 1 d . . . H63A H 1.2986 0.6049 0.1613 0.034 Uiso 1 1 calc R . . H63B H 1.2213 0.6158 0.1165 0.034 Uiso 1 1 calc R . . C64 C 1.2638(4) 0.4430(3) 0.08443(19) 0.0347(13) Uani 1 1 d . . . C65 C 1.3019(5) 0.3700(3) 0.0864(2) 0.0469(16) Uani 1 1 d . . . H65A H 1.2820 0.3417 0.1118 0.056 Uiso 1 1 calc R . . C66 C 1.3696(6) 0.3391(4) 0.0506(3) 0.0617(19) Uani 1 1 d . . . H66A H 1.3960 0.2892 0.0516 0.074 Uiso 1 1 calc R . . C67 C 1.3988(5) 0.3799(5) 0.0138(3) 0.0622(19) Uani 1 1 d . . . H67A H 1.4447 0.3577 -0.0106 0.075 Uiso 1 1 calc R . . C68 C 1.3629(5) 0.4514(4) 0.0118(2) 0.0535(17) Uani 1 1 d . . . H68A H 1.3825 0.4786 -0.0141 0.064 Uiso 1 1 calc R . . C69 C 1.2983(5) 0.4842(4) 0.0473(2) 0.0433(15) Uani 1 1 d . . . H69A H 1.2765 0.5359 0.0467 0.052 Uiso 1 1 calc R . . C70 C 1.0338(4) 0.4632(3) 0.10185(18) 0.0296(12) Uani 1 1 d . . . C71 C 0.9541(5) 0.4013(3) 0.1127(2) 0.0395(14) Uani 1 1 d . . . H71A H 0.9738 0.3696 0.1350 0.047 Uiso 1 1 calc R . . C72 C 0.8452(5) 0.3852(4) 0.0913(2) 0.0478(16) Uani 1 1 d . . . H72A H 0.7906 0.3420 0.0986 0.057 Uiso 1 1 calc R . . C73 C 0.8166(5) 0.4313(4) 0.0599(2) 0.0512(17) Uani 1 1 d . . . H73A H 0.7421 0.4197 0.0452 0.061 Uiso 1 1 calc R . . C74 C 0.8947(5) 0.4952(4) 0.0490(2) 0.0489(16) Uani 1 1 d . . . H74A H 0.8736 0.5280 0.0276 0.059 Uiso 1 1 calc R . . C75 C 1.0032(5) 0.5102(3) 0.06970(19) 0.0383(14) Uani 1 1 d . . . H75A H 1.0577 0.5530 0.0620 0.046 Uiso 1 1 calc R . . C76 C 0.9989(4) 0.7596(3) 0.35790(17) 0.0282(12) Uani 1 1 d . . . H76A H 0.9282 0.7541 0.3748 0.034 Uiso 1 1 calc R . . H76B H 1.0586 0.7984 0.3805 0.034 Uiso 1 1 calc R . . C77 C 1.0325(4) 0.6760(3) 0.34208(19) 0.0307(12) Uani 1 1 d . . . H77A H 1.1093 0.6840 0.3305 0.037 Uiso 1 1 calc R . . H77B H 1.0347 0.6499 0.3706 0.037 Uiso 1 1 calc R . . C78 C 0.8534(4) 0.5834(3) 0.3108(2) 0.0289(12) Uani 1 1 d . . . C79 C 0.7906(5) 0.5211(3) 0.26775(19) 0.0330(13) Uani 1 1 d . . . H79A H 0.7955 0.5447 0.2382 0.040 Uiso 1 1 calc R . . H79B H 0.7102 0.5068 0.2740 0.040 Uiso 1 1 calc R . . C80 C 0.7539(4) 0.3459(3) 0.22144(19) 0.0320(13) Uani 1 1 d . . . C81 C 0.7724(5) 0.2646(3) 0.2171(2) 0.0469(16) Uani 1 1 d . . . H81A H 0.8329 0.2540 0.2358 0.056 Uiso 1 1 calc R . . C82 C 0.7023(7) 0.1999(4) 0.1856(2) 0.065(2) Uani 1 1 d . . . H82A H 0.7141 0.1445 0.1829 0.077 Uiso 1 1 calc R . . C83 C 0.6170(7) 0.2151(4) 0.1587(2) 0.068(2) Uani 1 1 d . . . H83A H 0.5700 0.1700 0.1370 0.082 Uiso 1 1 calc R . . C84 C 0.5965(6) 0.2935(4) 0.1619(2) 0.0602(19) Uani 1 1 d . . . H84A H 0.5359 0.3029 0.1427 0.072 Uiso 1 1 calc R . . C85 C 0.6659(5) 0.3601(4) 0.1939(2) 0.0536(17) Uani 1 1 d . . . H85A H 0.6524 0.4150 0.1967 0.064 Uiso 1 1 calc R . . C86 C 0.8682(4) 0.4070(3) 0.31731(19) 0.0289(12) Uani 1 1 d . . . C87 C 0.7761(5) 0.3810(3) 0.3428(2) 0.0386(14) Uani 1 1 d . . . H87A H 0.7025 0.3697 0.3272 0.046 Uiso 1 1 calc R . . C88 C 0.7897(5) 0.3711(3) 0.3904(2) 0.0438(15) Uani 1 1 d . . . H88A H 0.7263 0.3524 0.4071 0.053 Uiso 1 1 calc R . . C89 C 0.8956(6) 0.3887(4) 0.4128(2) 0.0472(16) Uani 1 1 d . . . H89A H 0.9055 0.3827 0.4455 0.057 Uiso 1 1 calc R . . C90 C 0.9877(5) 0.4146(4) 0.3894(2) 0.0476(16) Uani 1 1 d . . . H90A H 1.0604 0.4262 0.4059 0.057 Uiso 1 1 calc R . . C91 C 0.9763(5) 0.4243(3) 0.3412(2) 0.0376(14) Uani 1 1 d . . . H91A H 1.0407 0.4423 0.3250 0.045 Uiso 1 1 calc R . . C100 C 0.8271(5) 1.2604(3) -0.0400(2) 0.0406(15) Uani 1 1 d . . . C101 C 0.9316(6) 1.2457(3) -0.0217(2) 0.0488(16) Uani 1 1 d . . . C102 C 0.9414(8) 1.2078(4) 0.0179(3) 0.070(2) Uani 1 1 d . . . H10A H 1.0134 1.2042 0.0309 0.085 Uiso 1 1 calc R . . C103 C 0.8469(9) 1.1766(4) 0.0373(3) 0.073(2) Uani 1 1 d . . . C104 C 0.7414(8) 1.1848(4) 0.0211(2) 0.068(2) Uani 1 1 d . . . H10B H 0.6759 1.1605 0.0345 0.082 Uiso 1 1 calc R . . C105 C 0.7325(6) 1.2278(4) -0.0142(2) 0.0489(16) Uani 1 1 d . . . O10 O 0.8171(4) 1.2965(2) -0.07427(14) 0.0510(11) Uani 1 1 d . . . N4 N 1.0342(6) 1.2750(4) -0.0438(3) 0.0756(19) Uani 1 1 d . . . O11 O 1.0281(4) 1.2745(3) -0.0881(2) 0.0777(15) Uani 1 1 d . . . O12 O 1.1200(6) 1.2960(5) -0.0192(3) 0.139(3) Uani 1 1 d . . . N5 N 0.8635(12) 1.1357(5) 0.0773(3) 0.112(4) Uani 1 1 d . . . O13 O 0.9497(9) 1.1363(4) 0.0952(2) 0.153(4) Uani 1 1 d . . . O14 O 0.7667(8) 1.0972(5) 0.0895(2) 0.123(3) Uani 1 1 d . . . N6 N 0.6219(6) 1.2414(4) -0.0276(2) 0.0708(18) Uani 1 1 d . . . O15 O 0.6115(4) 1.3020(4) -0.04262(18) 0.0784(15) Uani 1 1 d . . . O16 O 0.5381(5) 1.1873(4) -0.0254(3) 0.122(2) Uani 1 1 d . . . C200 C -0.3638(6) 0.6057(4) 0.1508(3) 0.0522(17) Uani 1 1 d . . . Cl1 Cl -0.4583(5) 0.6657(5) 0.1318(4) 0.0789(19) Uani 0.50 1 d P D 7 Cl2 Cl -0.2370(5) 0.6333(4) 0.1298(2) 0.0657(15) Uani 0.50 1 d P D 7 Cl1' Cl -0.3961(9) 0.6811(6) 0.1258(4) 0.143(4) Uani 0.50 1 d P D 8 Cl2' Cl -0.2105(5) 0.6083(4) 0.1504(2) 0.0809(18) Uani 0.50 1 d P D 8 H20F H -0.372(4) 0.612(3) 0.187(2) 0.046(16) Uiso 1 1 d . . . Cl3 Cl -0.42863(15) 0.50418(10) 0.12600(6) 0.0645(5) Uani 1 1 d . D . C201 C -0.1448(6) 0.6481(5) 0.4620(2) 0.078(2) Uani 1 1 d . . . H20D H -0.1515 0.6239 0.4261 0.094 Uiso 1 1 calc R . . Cl4 Cl -0.1680(3) 0.56640(16) 0.49348(9) 0.1329(11) Uani 1 1 d . . . Cl5 Cl -0.2450(2) 0.70677(17) 0.47527(11) 0.1254(10) Uani 1 1 d . . . Cl6 Cl -0.0099(2) 0.7088(2) 0.47816(8) 0.1434(12) Uani 1 1 d . . . C202 C 1.1151(7) 1.0397(4) -0.1339(3) 0.077(2) Uani 1 1 d . . . H20E H 1.1470 0.9982 -0.1194 0.093 Uiso 1 1 calc R . . Cl7 Cl 1.0917(3) 1.00253(15) -0.19661(8) 0.1199(9) Uani 1 1 d . . . Cl8 Cl 1.2090(2) 1.13319(16) -0.12004(10) 0.1232(9) Uani 1 1 d . . . Cl9 Cl 0.9850(2) 1.05194(15) -0.10869(9) 0.1054(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.035(5) 0.023(4) 0.028(5) 0.004(4) 0.004(4) 0.003(4) P1 0.0281(8) 0.0189(7) 0.0374(9) 0.0086(6) 0.0048(6) 0.0051(6) P2 0.0336(8) 0.0249(7) 0.0275(8) 0.0026(6) 0.0025(6) 0.0065(6) P3 0.0281(8) 0.0198(7) 0.0332(8) 0.0068(6) 0.0007(6) 0.0018(6) O1 0.0196(19) 0.0223(18) 0.040(2) 0.0041(16) 0.0045(16) 0.0022(15) O2 0.0205(19) 0.0167(17) 0.037(2) 0.0020(15) -0.0018(15) 0.0029(14) O3 0.028(2) 0.0139(17) 0.033(2) 0.0059(14) 0.0039(15) 0.0028(14) O4 0.025(2) 0.032(2) 0.057(3) 0.0116(18) 0.0075(18) 0.0022(17) O5 0.028(2) 0.031(2) 0.032(2) 0.0066(15) 0.0093(15) 0.0099(16) O6 0.042(2) 0.0239(19) 0.023(2) 0.0077(15) 0.0060(16) 0.0030(16) O7 0.039(2) 0.030(2) 0.029(2) 0.0072(16) 0.0021(16) 0.0064(17) O8 0.039(2) 0.026(2) 0.045(3) 0.0061(17) 0.0038(19) 0.0015(17) O9 0.022(2) 0.035(2) 0.037(2) 0.0081(16) 0.0055(16) -0.0018(16) N1 0.024(3) 0.019(2) 0.045(3) 0.007(2) 0.009(2) 0.004(2) N2 0.033(3) 0.023(2) 0.023(3) 0.002(2) 0.004(2) 0.001(2) N3 0.039(3) 0.020(2) 0.028(3) 0.003(2) 0.003(2) 0.000(2) C1 0.026(3) 0.016(2) 0.027(3) 0.005(2) 0.005(2) 0.004(2) C2 0.023(3) 0.021(3) 0.029(3) 0.002(2) 0.004(2) 0.001(2) C3 0.020(3) 0.019(3) 0.035(3) -0.003(2) 0.001(2) 0.003(2) C4 0.027(3) 0.029(3) 0.037(3) 0.010(2) 0.001(2) 0.009(2) C5 0.042(4) 0.029(3) 0.045(4) 0.016(3) -0.007(3) 0.007(3) C6 0.047(9) 0.038(6) 0.102(12) 0.035(6) -0.003(8) 0.011(7) C7 0.126(13) 0.063(9) 0.064(9) 0.025(7) 0.007(10) 0.052(10) C8 0.057(7) 0.051(6) 0.097(9) 0.030(6) -0.003(6) 0.032(5) C6' 0.09(2) 0.041(15) 0.043(16) 0.026(12) 0.049(18) 0.028(16) C8' 0.034(17) 0.015(11) 0.08(2) 0.018(13) -0.029(16) -0.001(13) C9 0.040(3) 0.036(3) 0.031(3) 0.008(3) 0.000(3) 0.009(3) C10 0.039(3) 0.027(3) 0.039(4) 0.008(2) 0.002(3) 0.005(3) C11 0.061(4) 0.037(3) 0.031(3) -0.004(3) 0.002(3) 0.018(3) C12 0.127(14) 0.046(8) 0.017(7) 0.001(6) 0.013(7) 0.048(9) C13 0.079(12) 0.052(9) 0.036(9) -0.019(7) 0.005(8) 0.000(8) C14 0.067(10) 0.048(8) 0.037(8) -0.002(6) 0.019(6) 0.013(7) C12' 0.084(12) 0.049(9) 0.060(10) -0.027(7) -0.003(9) 0.005(8) C13' 0.16(2) 0.126(18) 0.045(11) -0.005(10) 0.012(11) 0.105(17) C15 0.027(3) 0.020(3) 0.029(3) 0.008(2) 0.003(2) 0.007(2) C16 0.027(3) 0.021(3) 0.028(3) 0.009(2) 0.003(2) 0.011(2) C17 0.024(3) 0.020(3) 0.033(3) 0.005(2) -0.003(2) 0.005(2) C18 0.030(3) 0.021(3) 0.036(3) 0.009(2) 0.009(2) 0.007(2) C19 0.038(3) 0.026(3) 0.035(3) 0.008(2) 0.011(3) 0.001(2) C20 0.066(5) 0.040(4) 0.051(4) 0.005(3) 0.016(3) 0.022(3) C21 0.057(4) 0.052(4) 0.039(4) 0.008(3) 0.009(3) 0.012(3) C22 0.065(5) 0.056(4) 0.058(5) 0.005(3) 0.019(4) -0.014(4) C23 0.026(3) 0.020(3) 0.045(4) 0.014(2) 0.002(2) -0.002(2) C24 0.025(3) 0.018(3) 0.048(4) 0.011(2) -0.002(2) 0.007(2) C25 0.029(3) 0.021(3) 0.036(3) 0.003(2) -0.002(2) -0.004(2) C26 0.030(7) 0.032(6) 0.049(8) 0.004(5) -0.002(6) 0.002(5) C27 0.036(7) 0.020(6) 0.031(7) 0.002(5) -0.003(5) 0.006(5) C28 0.038(7) 0.040(7) 0.052(8) 0.013(6) -0.004(6) -0.014(6) C26' 0.049(8) 0.054(8) 0.045(8) 0.000(6) 0.002(6) -0.021(7) C27' 0.039(8) 0.027(7) 0.095(12) 0.002(7) -0.013(7) -0.004(6) C28' 0.035(8) 0.032(7) 0.099(13) -0.023(8) -0.011(8) -0.001(6) C29 0.026(3) 0.018(3) 0.024(3) 0.007(2) 0.001(2) 0.005(2) C30 0.023(3) 0.020(3) 0.023(3) 0.002(2) 0.005(2) 0.006(2) C31 0.028(3) 0.020(3) 0.025(3) 0.004(2) 0.007(2) 0.004(2) C32 0.021(3) 0.025(3) 0.022(3) 0.004(2) 0.004(2) 0.004(2) C33 0.019(3) 0.029(3) 0.038(3) 0.006(2) 0.005(2) 0.003(2) C34 0.031(3) 0.042(3) 0.043(4) -0.007(3) 0.000(3) -0.003(3) C35 0.022(3) 0.033(3) 0.058(4) 0.012(3) 0.010(3) 0.000(2) C36 0.030(3) 0.045(4) 0.056(4) 0.012(3) 0.002(3) 0.007(3) C37 0.031(3) 0.022(3) 0.034(3) 0.009(2) 0.001(2) 0.009(2) C38 0.028(3) 0.022(3) 0.033(3) 0.008(2) -0.002(2) 0.009(2) C39 0.039(4) 0.015(3) 0.067(4) 0.008(3) -0.005(3) 0.005(3) C40 0.062(7) 0.028(5) 0.081(8) 0.019(5) -0.012(6) 0.008(5) C41 0.116(10) 0.022(5) 0.080(8) -0.004(5) 0.021(7) 0.019(6) C42 0.043(7) 0.013(5) 0.220(17) 0.021(7) -0.008(9) -0.008(4) C41' 0.067(16) 0.008(9) 0.050(14) -0.003(8) 0.019(11) -0.001(9) C42' 0.100(19) 0.015(10) 0.044(13) 0.016(9) 0.033(13) 0.014(11) C43 0.028(3) 0.017(3) 0.031(3) 0.007(2) 0.000(2) -0.001(2) C44 0.026(3) 0.021(3) 0.046(4) 0.002(2) 0.010(3) 0.001(2) C45 0.028(3) 0.016(3) 0.051(4) 0.015(2) 0.011(3) 0.004(2) C46 0.029(3) 0.032(3) 0.025(3) 0.011(2) 0.004(2) 0.005(3) C47 0.032(3) 0.026(3) 0.032(3) 0.007(2) 0.006(2) 0.007(2) C48 0.045(4) 0.020(3) 0.044(4) 0.009(2) 0.011(3) 0.004(3) C49 0.047(4) 0.030(3) 0.060(4) 0.008(3) -0.004(3) -0.008(3) C50 0.062(5) 0.040(4) 0.072(5) 0.001(3) 0.005(4) -0.007(4) C51 0.099(7) 0.041(5) 0.110(7) -0.018(4) 0.019(5) -0.014(5) C52 0.091(7) 0.032(4) 0.173(9) -0.013(5) 0.031(6) 0.016(4) C53 0.053(5) 0.028(4) 0.120(6) 0.003(4) 0.022(4) 0.014(3) C54 0.036(3) 0.036(3) 0.032(3) 0.011(2) 0.008(3) 0.011(3) C55 0.047(4) 0.055(4) 0.059(5) 0.028(3) 0.010(3) 0.010(3) C56 0.085(6) 0.081(5) 0.052(5) 0.042(4) 0.021(4) 0.032(5) C57 0.075(6) 0.082(5) 0.055(5) 0.021(4) -0.002(4) 0.043(5) C58 0.056(4) 0.055(4) 0.055(5) 0.016(3) -0.003(3) 0.018(3) C59 0.037(4) 0.046(4) 0.044(4) 0.010(3) 0.001(3) 0.010(3) C60 0.028(3) 0.019(3) 0.033(3) 0.007(2) 0.004(2) 0.010(2) C61 0.025(3) 0.022(3) 0.034(3) -0.001(2) 0.006(2) 0.007(2) C62 0.022(3) 0.020(3) 0.024(3) -0.004(2) -0.006(2) -0.003(2) C63 0.025(3) 0.025(3) 0.032(3) 0.002(2) 0.006(2) 0.000(2) C64 0.037(3) 0.038(3) 0.027(3) -0.001(2) 0.002(2) 0.012(3) C65 0.047(4) 0.031(3) 0.059(4) -0.003(3) 0.003(3) 0.011(3) C66 0.057(5) 0.051(4) 0.072(5) -0.009(4) -0.003(4) 0.026(4) C67 0.044(4) 0.086(6) 0.050(5) -0.006(4) 0.006(3) 0.019(4) C68 0.040(4) 0.083(5) 0.040(4) 0.009(3) 0.011(3) 0.021(4) C69 0.033(3) 0.058(4) 0.036(4) 0.002(3) 0.004(3) 0.010(3) C70 0.029(3) 0.031(3) 0.028(3) 0.001(2) 0.005(2) 0.006(2) C71 0.036(4) 0.036(3) 0.041(4) 0.001(3) 0.001(3) 0.000(3) C72 0.040(4) 0.035(3) 0.054(4) -0.009(3) 0.006(3) -0.007(3) C73 0.031(4) 0.063(4) 0.049(4) -0.013(3) 0.003(3) 0.008(3) C74 0.041(4) 0.053(4) 0.048(4) -0.002(3) -0.005(3) 0.014(3) C75 0.038(4) 0.036(3) 0.037(3) -0.001(3) -0.003(3) 0.007(3) C76 0.027(3) 0.026(3) 0.029(3) 0.006(2) 0.000(2) -0.001(2) C77 0.020(3) 0.023(3) 0.047(4) 0.005(2) -0.001(2) 0.003(2) C78 0.033(3) 0.024(3) 0.034(3) 0.010(2) 0.005(3) 0.009(2) C79 0.038(3) 0.021(3) 0.038(3) 0.004(2) -0.010(3) 0.006(2) C80 0.032(3) 0.024(3) 0.037(3) 0.003(2) 0.006(3) 0.002(2) C81 0.063(4) 0.026(3) 0.046(4) 0.007(3) -0.005(3) -0.005(3) C82 0.096(6) 0.030(4) 0.057(5) 0.004(3) 0.002(4) -0.011(4) C83 0.094(6) 0.041(4) 0.047(4) 0.000(3) 0.002(4) -0.035(4) C84 0.057(5) 0.059(5) 0.050(4) 0.000(3) -0.014(3) -0.009(4) C85 0.044(4) 0.063(4) 0.048(4) 0.009(3) -0.002(3) -0.003(3) C86 0.029(3) 0.019(3) 0.038(3) 0.004(2) 0.005(2) 0.006(2) C87 0.037(3) 0.029(3) 0.050(4) 0.011(3) 0.007(3) 0.005(3) C88 0.055(4) 0.043(4) 0.040(4) 0.016(3) 0.016(3) 0.015(3) C89 0.067(5) 0.043(4) 0.038(4) 0.014(3) 0.005(3) 0.020(3) C90 0.046(4) 0.058(4) 0.043(4) 0.014(3) -0.002(3) 0.020(3) C91 0.035(3) 0.035(3) 0.042(4) 0.006(3) 0.003(3) 0.007(3) C100 0.071(5) 0.022(3) 0.029(3) 0.002(2) 0.002(3) 0.012(3) C101 0.065(5) 0.028(3) 0.048(4) -0.002(3) -0.007(3) 0.007(3) C102 0.104(7) 0.052(5) 0.055(5) -0.003(4) -0.025(5) 0.036(5) C103 0.125(8) 0.049(5) 0.055(5) 0.016(4) 0.013(5) 0.036(5) C104 0.132(8) 0.037(4) 0.044(4) 0.013(3) 0.038(4) 0.031(4) C105 0.068(5) 0.036(3) 0.049(4) 0.012(3) 0.018(3) 0.021(3) O10 0.071(3) 0.052(3) 0.038(3) 0.024(2) 0.005(2) 0.016(2) N4 0.071(5) 0.060(4) 0.092(6) 0.012(4) -0.023(4) 0.013(4) O11 0.056(3) 0.093(4) 0.098(4) 0.047(3) 0.015(3) 0.020(3) O12 0.071(5) 0.187(7) 0.132(6) 0.000(5) -0.040(4) -0.005(5) N5 0.242(13) 0.063(5) 0.060(6) 0.034(4) 0.030(7) 0.075(7) O13 0.287(12) 0.108(5) 0.079(5) 0.032(4) -0.068(6) 0.074(7) O14 0.222(9) 0.115(6) 0.071(4) 0.052(4) 0.052(5) 0.091(6) N6 0.075(5) 0.046(4) 0.102(5) 0.031(4) 0.046(4) 0.017(4) O15 0.072(4) 0.097(4) 0.080(4) 0.037(3) 0.020(3) 0.028(3) O16 0.075(5) 0.122(5) 0.186(7) 0.073(5) 0.029(4) 0.012(4) C200 0.068(5) 0.044(4) 0.045(4) 0.009(3) 0.010(3) 0.012(3) Cl1 0.078(4) 0.066(4) 0.111(4) 0.036(3) 0.017(3) 0.043(3) Cl2 0.045(3) 0.068(3) 0.068(4) -0.010(2) 0.026(2) -0.005(2) Cl1' 0.262(12) 0.068(4) 0.104(6) 0.009(4) -0.045(8) 0.066(8) Cl2' 0.056(3) 0.078(4) 0.084(5) -0.021(3) 0.026(3) -0.012(3) Cl3 0.0627(12) 0.0545(10) 0.0680(12) 0.0070(8) 0.0014(9) -0.0033(9) C201 0.075(5) 0.134(7) 0.035(4) 0.016(4) -0.007(4) 0.050(5) Cl4 0.218(3) 0.1060(19) 0.0823(17) -0.0011(14) -0.0292(18) 0.083(2) Cl5 0.119(2) 0.128(2) 0.151(2) 0.0351(18) 0.0065(17) 0.0750(18) Cl6 0.0886(19) 0.269(4) 0.0602(15) 0.0243(18) -0.0094(13) 0.016(2) C202 0.110(7) 0.058(5) 0.081(6) 0.032(4) 0.021(5) 0.034(5) Cl7 0.180(3) 0.1004(18) 0.0726(16) 0.0190(13) 0.0116(16) 0.0077(18) Cl8 0.128(2) 0.0992(19) 0.131(2) 0.0201(16) 0.0132(17) -0.0025(16) Cl9 0.1054(19) 0.1116(19) 0.113(2) 0.0433(15) 0.0155(15) 0.0342(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 O9 1.863(9) . ? Li1 O7 1.935(9) . ? Li1 O5 1.942(9) . ? Li1 O6 2.005(8) . ? Li1 P2 2.939(8) . ? Li1 P1 3.048(8) . ? P1 O5 1.503(3) . ? P1 C48 1.795(5) . ? P1 C47 1.798(5) . ? P1 C54 1.802(5) . ? P2 O7 1.494(3) . ? P2 C64 1.773(5) . ? P2 C70 1.784(5) . ? P2 C63 1.811(5) . ? P3 O9 1.481(3) . ? P3 C86 1.770(5) . ? P3 C80 1.794(5) . ? P3 C79 1.808(5) . ? O1 C3 1.392(5) . ? O1 C44 1.419(6) . ? O2 C17 1.388(5) . ? O2 C60 1.440(5) . ? O3 C31 1.399(5) . ? O3 C76 1.425(5) . ? O4 C46 1.228(6) . ? O6 C62 1.252(6) . ? O8 C78 1.238(6) . ? N1 C46 1.338(6) . ? N1 C45 1.461(6) . ? N2 C62 1.325(6) . ? N2 C61 1.458(6) . ? N3 C78 1.327(7) . ? N3 C77 1.452(6) . ? C1 C16 1.523(6) . ? C1 C2 1.525(6) . ? C1 C30 1.541(6) . ? C2 C15 1.383(6) . ? C2 C3 1.414(6) . ? C3 C4 1.390(7) . ? C4 C9 1.400(7) . ? C4 C5 1.549(7) . ? C5 C7 1.452(14) . ? C5 C8' 1.48(3) . ? C5 C7' 1.50(2) . ? C5 C6 1.537(16) . ? C5 C8 1.576(11) . ? C5 C6' 1.62(2) . ? C9 C10 1.411(7) . ? C10 C15 1.374(7) . ? C10 C11 1.522(7) . ? C11 C14' 1.452(17) . ? C11 C13 1.485(16) . ? C11 C13' 1.510(17) . ? C11 C12 1.534(12) . ? C11 C12' 1.597(16) . ? C11 C14 1.598(13) . ? C16 C17 1.395(7) . ? C16 C29 1.412(6) . ? C17 C18 1.410(7) . ? C18 C23 1.391(7) . ? C18 C19 1.537(7) . ? C19 C21 1.526(8) . ? C19 C22 1.535(7) . ? C19 C20 1.542(7) . ? C23 C24 1.393(7) . ? C24 C29 1.365(7) . ? C24 C25 1.539(7) . ? C25 C28' 1.446(13) . ? C25 C27 1.460(11) . ? C25 C26' 1.568(13) . ? C25 C26 1.572(12) . ? C25 C28 1.576(12) . ? C25 C27' 1.578(13) . ? C30 C43 1.391(6) . ? C30 C31 1.402(6) . ? C31 C32 1.395(6) . ? C32 C37 1.388(6) . ? C32 C33 1.537(6) . ? C33 C36 1.523(7) . ? C33 C35 1.529(7) . ? C33 C34 1.548(7) . ? C37 C38 1.400(7) . ? C38 C43 1.370(7) . ? C38 C39 1.538(6) . ? C39 C40' 1.39(2) . ? C39 C42 1.494(11) . ? C39 C41' 1.52(2) . ? C39 C40 1.544(10) . ? C39 C42' 1.579(19) . ? C39 C41 1.588(11) . ? C44 C45 1.508(7) . ? C46 C47 1.513(7) . ? C48 C53 1.384(8) . ? C48 C49 1.387(8) . ? C49 C50 1.364(8) . ? C50 C51 1.371(10) . ? C51 C52 1.365(11) . ? C52 C53 1.387(9) . ? C54 C55 1.383(8) . ? C54 C59 1.386(7) . ? C55 C56 1.372(9) . ? C56 C57 1.382(10) . ? C57 C58 1.346(9) . ? C58 C59 1.372(8) . ? C60 C61 1.499(6) . ? C62 C63 1.505(7) . ? C64 C65 1.390(7) . ? C64 C69 1.401(8) . ? C65 C66 1.388(9) . ? C66 C67 1.377(9) . ? C67 C68 1.353(9) . ? C68 C69 1.370(8) . ? C70 C71 1.376(7) . ? C70 C75 1.396(7) . ? C71 C72 1.388(8) . ? C72 C73 1.360(8) . ? C73 C74 1.390(8) . ? C74 C75 1.377(8) . ? C76 C77 1.509(6) . ? C78 C79 1.505(7) . ? C80 C85 1.376(8) . ? C80 C81 1.400(7) . ? C81 C82 1.381(8) . ? C82 C83 1.350(10) . ? C83 C84 1.364(9) . ? C84 C85 1.400(8) . ? C86 C87 1.398(7) . ? C86 C91 1.404(7) . ? C87 C88 1.387(7) . ? C88 C89 1.365(8) . ? C89 C90 1.363(8) . ? C90 C91 1.400(8) . ? C100 O10 1.252(6) . ? C100 C101 1.428(8) . ? C100 C105 1.459(8) . ? C101 C102 1.402(9) . ? C101 N4 1.459(9) . ? C102 C103 1.350(11) . ? C103 C104 1.380(11) . ? C103 N5 1.458(10) . ? C104 C105 1.352(8) . ? C105 N6 1.446(9) . ? N4 O12 1.184(7) . ? N4 O11 1.242(7) . ? N5 O13 1.140(13) . ? N5 O14 1.325(12) . ? N6 O15 1.201(6) . ? N6 O16 1.248(7) . ? C200 Cl1' 1.662(11) . ? C200 Cl2 1.683(9) . ? C200 Cl3 1.730(6) . ? C200 Cl1 1.785(10) . ? C200 Cl2' 1.847(9) . ? C201 Cl5 1.693(7) . ? C201 Cl6 1.754(8) . ? C201 Cl4 1.766(8) . ? C202 Cl8 1.728(8) . ? C202 Cl7 1.737(8) . ? C202 Cl9 1.771(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Li1 O7 115.5(4) . . ? O9 Li1 O5 111.4(4) . . ? O7 Li1 O5 104.4(4) . . ? O9 Li1 O6 112.1(4) . . ? O7 Li1 O6 100.1(4) . . ? O5 Li1 O6 112.7(4) . . ? O9 Li1 P2 115.4(4) . . ? O7 Li1 P2 26.82(16) . . ? O5 Li1 P2 124.2(4) . . ? O6 Li1 P2 75.7(3) . . ? O9 Li1 P1 121.8(4) . . ? O7 Li1 P1 80.3(3) . . ? O5 Li1 P1 24.15(16) . . ? O6 Li1 P1 119.7(3) . . ? P2 Li1 P1 101.9(3) . . ? O5 P1 C48 112.4(2) . . ? O5 P1 C47 111.7(2) . . ? C48 P1 C47 105.7(2) . . ? O5 P1 C54 113.0(2) . . ? C48 P1 C54 106.6(2) . . ? C47 P1 C54 106.9(2) . . ? O5 P1 Li1 31.9(2) . . ? C48 P1 Li1 93.6(2) . . ? C47 P1 Li1 94.3(2) . . ? C54 P1 Li1 144.9(2) . . ? O7 P2 C64 111.7(2) . . ? O7 P2 C70 111.1(2) . . ? C64 P2 C70 109.4(2) . . ? O7 P2 C63 111.3(2) . . ? C64 P2 C63 106.3(2) . . ? C70 P2 C63 106.7(2) . . ? O7 P2 Li1 35.8(2) . . ? C64 P2 Li1 146.0(2) . . ? C70 P2 Li1 96.4(2) . . ? C63 P2 Li1 86.1(2) . . ? O9 P3 C86 111.6(2) . . ? O9 P3 C80 112.7(2) . . ? C86 P3 C80 108.1(2) . . ? O9 P3 C79 111.3(2) . . ? C86 P3 C79 105.5(2) . . ? C80 P3 C79 107.2(2) . . ? C3 O1 C44 114.8(4) . . ? C17 O2 C60 117.7(3) . . ? C31 O3 C76 115.2(3) . . ? P1 O5 Li1 123.9(3) . . ? C62 O6 Li1 126.9(4) . . ? P2 O7 Li1 117.4(3) . . ? P3 O9 Li1 159.1(3) . . ? C46 N1 C45 123.9(5) . . ? C62 N2 C61 124.3(5) . . ? C78 N3 C77 123.5(5) . . ? C16 C1 C2 113.1(4) . . ? C16 C1 C30 111.0(4) . . ? C2 C1 C30 112.1(4) . . ? C15 C2 C3 117.8(4) . . ? C15 C2 C1 120.2(4) . . ? C3 C2 C1 121.9(4) . . ? C4 C3 O1 121.1(4) . . ? C4 C3 C2 121.8(4) . . ? O1 C3 C2 117.0(4) . . ? C3 C4 C9 116.8(4) . . ? C3 C4 C5 124.9(5) . . ? C9 C4 C5 118.3(5) . . ? C7 C5 C8' 124.8(14) . . ? C7 C5 C7' 69.3(11) . . ? C8' C5 C7' 109.5(14) . . ? C7 C5 C6 111.1(9) . . ? C8' C5 C6 29.3(11) . . ? C7' C5 C6 133.1(11) . . ? C7 C5 C4 112.7(7) . . ? C8' C5 C4 117.2(12) . . ? C7' C5 C4 112.7(9) . . ? C6 C5 C4 109.8(6) . . ? C7 C5 C8 106.2(8) . . ? C8' C5 C8 78.1(11) . . ? C7' C5 C8 39.1(9) . . ? C6 C5 C8 107.2(7) . . ? C4 C5 C8 109.7(5) . . ? C7 C5 C6' 34.8(10) . . ? C8' C5 C6' 105.2(16) . . ? C7' C5 C6' 102.9(15) . . ? C6 C5 C6' 81.7(13) . . ? C4 C5 C6' 108.0(10) . . ? C8 C5 C6' 135.0(12) . . ? C4 C9 C10 123.0(5) . . ? C15 C10 C9 116.8(5) . . ? C15 C10 C11 122.5(5) . . ? C9 C10 C11 120.7(5) . . ? C14' C11 C13 139.0(10) . . ? C14' C11 C13' 113.4(12) . . ? C13 C11 C13' 46.6(9) . . ? C14' C11 C10 110.2(8) . . ? C13 C11 C10 110.8(7) . . ? C13' C11 C10 113.7(7) . . ? C14' C11 C12 54.5(9) . . ? C13 C11 C12 108.6(10) . . ? C13' C11 C12 132.9(9) . . ? C10 C11 C12 112.8(6) . . ? C14' C11 C12' 107.3(10) . . ? C13 C11 C12' 60.6(9) . . ? C13' C11 C12' 104.4(12) . . ? C10 C11 C12' 107.3(6) . . ? C12 C11 C12' 54.1(8) . . ? C14' C11 C14 55.7(9) . . ? C13 C11 C14 108.9(9) . . ? C13' C11 C14 64.1(11) . . ? C10 C11 C14 108.8(6) . . ? C12 C11 C14 106.8(8) . . ? C12' C11 C14 143.7(7) . . ? C10 C15 C2 123.3(5) . . ? C17 C16 C29 119.1(4) . . ? C17 C16 C1 121.9(4) . . ? C29 C16 C1 119.0(4) . . ? O2 C17 C16 118.8(4) . . ? O2 C17 C18 119.3(4) . . ? C16 C17 C18 121.4(4) . . ? C23 C18 C17 115.9(5) . . ? C23 C18 C19 120.7(4) . . ? C17 C18 C19 123.3(4) . . ? C21 C19 C22 106.5(5) . . ? C21 C19 C18 112.4(4) . . ? C22 C19 C18 112.1(4) . . ? C21 C19 C20 109.6(5) . . ? C22 C19 C20 106.3(5) . . ? C18 C19 C20 109.8(4) . . ? C18 C23 C24 124.2(5) . . ? C29 C24 C23 118.1(5) . . ? C29 C24 C25 120.6(5) . . ? C23 C24 C25 121.3(4) . . ? C28' C25 C27 134.8(7) . . ? C28' C25 C24 113.8(6) . . ? C27 C25 C24 111.4(5) . . ? C28' C25 C26' 110.9(9) . . ? C27 C25 C26' 50.7(7) . . ? C24 C25 C26' 112.9(6) . . ? C28' C25 C26 58.1(8) . . ? C27 C25 C26 111.0(7) . . ? C24 C25 C26 106.1(5) . . ? C26' C25 C26 62.0(7) . . ? C28' C25 C28 48.5(7) . . ? C27 C25 C28 111.9(7) . . ? C24 C25 C28 110.3(6) . . ? C26' C25 C28 136.8(7) . . ? C26 C25 C28 105.9(7) . . ? C28' C25 C27' 109.5(9) . . ? C27 C25 C27' 53.0(7) . . ? C24 C25 C27' 107.1(5) . . ? C26' C25 C27' 101.8(8) . . ? C26 C25 C27' 146.7(7) . . ? C28 C25 C27' 64.6(7) . . ? C24 C29 C16 121.0(5) . . ? C43 C30 C31 117.4(4) . . ? C43 C30 C1 120.8(4) . . ? C31 C30 C1 121.8(4) . . ? C32 C31 O3 119.7(4) . . ? C32 C31 C30 122.6(4) . . ? O3 C31 C30 117.4(4) . . ? C37 C32 C31 115.9(4) . . ? C37 C32 C33 120.7(4) . . ? C31 C32 C33 123.3(4) . . ? C36 C33 C35 107.3(4) . . ? C36 C33 C32 112.6(4) . . ? C35 C33 C32 112.1(4) . . ? C36 C33 C34 106.4(4) . . ? C35 C33 C34 109.1(4) . . ? C32 C33 C34 109.2(4) . . ? C32 C37 C38 123.8(4) . . ? C43 C38 C37 117.1(4) . . ? C43 C38 C39 122.6(4) . . ? C37 C38 C39 120.4(4) . . ? C40' C39 C42 130.8(11) . . ? C40' C39 C41' 112.5(14) . . ? C42 C39 C41' 55.2(10) . . ? C40' C39 C38 115.3(10) . . ? C42 C39 C38 113.3(5) . . ? C41' C39 C38 109.6(8) . . ? C40' C39 C40 41.8(10) . . ? C42 C39 C40 111.9(8) . . ? C41' C39 C40 139.0(8) . . ? C38 C39 C40 110.9(5) . . ? C40' C39 C42' 106.5(14) . . ? C42 C39 C42' 53.9(10) . . ? C41' C39 C42' 108.7(13) . . ? C38 C39 C42' 103.6(8) . . ? C40 C39 C42' 67.4(10) . . ? C40' C39 C41 65.4(11) . . ? C42 C39 C41 106.5(8) . . ? C41' C39 C41 54.5(9) . . ? C38 C39 C41 107.4(5) . . ? C40 C39 C41 106.3(7) . . ? C42' C39 C41 148.3(8) . . ? C38 C43 C30 122.8(5) . . ? O1 C44 C45 109.3(4) . . ? N1 C45 C44 114.3(4) . . ? O4 C46 N1 122.6(5) . . ? O4 C46 C47 121.0(5) . . ? N1 C46 C47 116.3(5) . . ? C46 C47 P1 118.4(4) . . ? C53 C48 C49 118.3(5) . . ? C53 C48 P1 121.0(5) . . ? C49 C48 P1 120.6(4) . . ? C50 C49 C48 121.2(6) . . ? C49 C50 C51 119.9(7) . . ? C52 C51 C50 120.5(7) . . ? C51 C52 C53 119.8(8) . . ? C48 C53 C52 120.4(7) . . ? C55 C54 C59 118.4(5) . . ? C55 C54 P1 118.6(5) . . ? C59 C54 P1 123.0(4) . . ? C56 C55 C54 119.8(6) . . ? C55 C56 C57 120.9(6) . . ? C58 C57 C56 119.5(6) . . ? C57 C58 C59 120.5(7) . . ? C58 C59 C54 121.0(6) . . ? O2 C60 C61 107.9(4) . . ? N2 C61 C60 110.9(4) . . ? O6 C62 N2 123.7(5) . . ? O6 C62 C63 121.4(4) . . ? N2 C62 C63 114.8(5) . . ? C62 C63 P2 111.3(3) . . ? C65 C64 C69 118.6(5) . . ? C65 C64 P2 119.0(4) . . ? C69 C64 P2 122.4(4) . . ? C66 C65 C64 119.0(6) . . ? C67 C66 C65 120.8(6) . . ? C68 C67 C66 120.7(6) . . ? C67 C68 C69 119.7(6) . . ? C68 C69 C64 121.2(6) . . ? C71 C70 C75 119.2(5) . . ? C71 C70 P2 119.1(4) . . ? C75 C70 P2 121.7(4) . . ? C70 C71 C72 120.3(6) . . ? C73 C72 C71 119.9(6) . . ? C72 C73 C74 121.2(6) . . ? C75 C74 C73 118.8(6) . . ? C74 C75 C70 120.7(6) . . ? O3 C76 C77 106.9(4) . . ? N3 C77 C76 112.6(4) . . ? O8 C78 N3 122.2(5) . . ? O8 C78 C79 121.6(5) . . ? N3 C78 C79 116.0(5) . . ? C78 C79 P3 108.1(3) . . ? C85 C80 C81 119.3(5) . . ? C85 C80 P3 122.1(4) . . ? C81 C80 P3 118.4(4) . . ? C82 C81 C80 119.7(6) . . ? C83 C82 C81 120.1(6) . . ? C82 C83 C84 121.8(6) . . ? C83 C84 C85 119.1(6) . . ? C80 C85 C84 120.0(6) . . ? C87 C86 C91 118.3(5) . . ? C87 C86 P3 122.9(4) . . ? C91 C86 P3 118.5(4) . . ? C88 C87 C86 121.6(5) . . ? C89 C88 C87 118.8(6) . . ? C90 C89 C88 121.5(6) . . ? C89 C90 C91 120.8(6) . . ? C90 C91 C86 119.0(5) . . ? O10 C100 C101 124.3(6) . . ? O10 C100 C105 123.7(6) . . ? C101 C100 C105 112.1(5) . . ? C102 C101 C100 123.3(7) . . ? C102 C101 N4 118.1(7) . . ? C100 C101 N4 118.5(6) . . ? C103 C102 C101 119.0(7) . . ? C102 C103 C104 122.1(7) . . ? C102 C103 N5 115.9(10) . . ? C104 C103 N5 122.0(10) . . ? C105 C104 C103 119.0(7) . . ? C104 C105 N6 117.9(7) . . ? C104 C105 C100 124.2(7) . . ? N6 C105 C100 117.9(5) . . ? O12 N4 O11 122.9(8) . . ? O12 N4 C101 118.9(8) . . ? O11 N4 C101 118.2(6) . . ? O13 N5 O14 124.7(9) . . ? O13 N5 C103 123.5(12) . . ? O14 N5 C103 111.7(11) . . ? O15 N6 O16 120.6(7) . . ? O15 N6 C105 120.5(6) . . ? O16 N6 C105 118.8(6) . . ? Cl1' C200 Cl2 83.0(5) . . ? Cl1' C200 Cl3 118.9(5) . . ? Cl2 C200 Cl3 113.9(4) . . ? Cl1' C200 Cl1 26.1(4) . . ? Cl2 C200 Cl1 108.9(5) . . ? Cl3 C200 Cl1 103.6(5) . . ? Cl1' C200 Cl2' 109.4(5) . . ? Cl2 C200 Cl2' 27.9(2) . . ? Cl3 C200 Cl2' 106.7(4) . . ? Cl1 C200 Cl2' 135.4(5) . . ? Cl5 C201 Cl6 110.7(5) . . ? Cl5 C201 Cl4 108.6(4) . . ? Cl6 C201 Cl4 110.8(4) . . ? Cl8 C202 Cl7 111.2(4) . . ? Cl8 C202 Cl9 110.1(4) . . ? Cl7 C202 Cl9 109.1(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.632 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.069 #===END data_12_neodymium_complex _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; tris(3,5-di-tert-butyl-2-(2-(carbamoylmethylphosphineoxide)ethoxy)phen yl)methane neodymium nitrate complex ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C194.50 H244.75 N24.25 Nd4 O55 P6' _chemical_formula_weight 4565.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nd' 'Nd' -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.4930(7) _cell_length_b 23.0241(11) _cell_length_c 34.5340(18) _cell_angle_alpha 80.9640(10) _cell_angle_beta 81.6050(10) _cell_angle_gamma 86.2560(10) _cell_volume 11248.0(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plates _exptl_crystal_colour Colorless _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4703 _exptl_absorpt_coefficient_mu 1.030 _exptl_absorpt_correction_type 'SADABS' _exptl_absorpt_correction_T_min 0.5515 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45369 _diffrn_reflns_av_R_equivalents 0.1029 _diffrn_reflns_av_sigmaI/netI 0.2176 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 0.90 _diffrn_reflns_theta_max 22.50 _reflns_number_total 27965 _reflns_number_gt 14290 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. 2.75 acetonitrile molecules and one ether was "SQUEEZED" from the asymmetric unit. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1029P)^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 27965 _refine_ls_number_parameters 1603 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1725 _refine_ls_R_factor_gt 0.0961 _refine_ls_wR_factor_ref 0.2531 _refine_ls_wR_factor_gt 0.2197 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _refine_ls_shift/su_max 0.057 _refine_ls_shift/su_mean 0.001 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 Nd1 Nd 1.11869(5) 0.22962(4) 0.11647(3) 0.0269(2) Uani 1 1 d . . . P1 P 1.2707(3) 0.31957(18) 0.15646(13) 0.0314(10) Uani 1 1 d . . . P2 P 1.3108(2) 0.15783(17) 0.05911(12) 0.0256(9) Uani 1 1 d . . . P3 P 0.9612(2) 0.15463(18) 0.06927(11) 0.0262(10) Uani 1 1 d . . . O1 O 1.1640(7) 0.1426(4) 0.2890(3) 0.044(3) Uani 1 1 d . . . O2 O 1.1734(6) 0.0226(4) 0.2185(3) 0.025(2) Uani 1 1 d . . . O3 O 0.9082(6) 0.0879(4) 0.2616(3) 0.030(2) Uani 1 1 d . . . O4 O 1.0818(6) 0.2545(4) 0.1808(3) 0.030(2) Uani 1 1 d . . . O5 O 1.2504(6) 0.2748(4) 0.1326(3) 0.037(3) Uani 1 1 d . . . O6 O 1.1966(6) 0.1435(5) 0.1466(3) 0.035(3) Uani 1 1 d . . . O7 O 1.2476(6) 0.2109(4) 0.0675(3) 0.025(2) Uani 1 1 d . . . O8 O 1.0039(6) 0.1620(4) 0.1538(3) 0.033(3) Uani 1 1 d . . . O9 O 1.0506(6) 0.1857(4) 0.0675(3) 0.028(2) Uani 1 1 d . . . N1 N 1.1050(8) 0.2545(5) 0.2432(4) 0.032(3) Uani 1 1 d . . . H1A H 1.1333 0.2700 0.2597 0.039 Uiso 1 1 calc R . . N2 N 1.3188(7) 0.0829(5) 0.1633(4) 0.032(3) Uani 1 1 d . . . H2A H 1.3680 0.0615 0.1549 0.038 Uiso 1 1 calc R . . N3 N 0.9041(7) 0.0916(5) 0.1712(3) 0.027(3) Uani 1 1 d . . . H3A H 0.8477 0.0814 0.1692 0.033 Uiso 1 1 calc R . . C1 C 1.0713(8) 0.0336(6) 0.2933(4) 0.027(4) Uani 1 1 d . . . H1B H 1.0755 0.0663 0.2705 0.032 Uiso 1 1 calc R . . C2 C 1.1486(10) 0.0423(6) 0.3190(4) 0.030(4) Uiso 1 1 d . A . C3 C 1.1880(10) 0.0954(7) 0.3166(5) 0.038(4) Uiso 1 1 d . . . C4 C 1.2622(11) 0.1016(7) 0.3384(5) 0.048(5) Uiso 1 1 d . . . C5 C 1.3155(12) 0.1590(8) 0.3325(6) 0.056(5) Uiso 1 1 d . . . C6 C 1.3959(14) 0.1500(9) 0.3579(6) 0.083(7) Uiso 1 1 d . . . H6A H 1.4233 0.1879 0.3576 0.124 Uiso 1 1 calc R . . H6B H 1.4437 0.1226 0.3470 0.124 Uiso 1 1 calc R . . H6C H 1.3717 0.1337 0.3851 0.124 Uiso 1 1 calc R . . C7 C 1.3645(15) 0.1692(10) 0.2892(7) 0.091(7) Uiso 1 1 d . . . H7A H 1.4127 0.1980 0.2866 0.137 Uiso 1 1 calc R . . H7B H 1.3184 0.1841 0.2715 0.137 Uiso 1 1 calc R . . H7C H 1.3933 0.1320 0.2821 0.137 Uiso 1 1 calc R . . C8 C 1.2528(14) 0.2100(9) 0.3431(6) 0.078(6) Uiso 1 1 d . . . H8A H 1.2821 0.2312 0.3603 0.116 Uiso 1 1 calc R . . H8B H 1.1929 0.1957 0.3571 0.116 Uiso 1 1 calc R . . H8C H 1.2423 0.2367 0.3189 0.116 Uiso 1 1 calc R . . C9 C 1.2856(11) 0.0530(7) 0.3641(5) 0.049(5) Uiso 1 1 d . . . H9A H 1.3310 0.0568 0.3807 0.059 Uiso 1 1 calc R . . C10 C 1.2475(11) -0.0005(7) 0.3672(5) 0.044(4) Uiso 1 1 d . A . C11 C 1.2762(12) -0.0545(8) 0.3988(6) 0.055(5) Uiso 1 1 d . . . C12 C 1.229(2) -0.1107(15) 0.3964(11) 0.096(11) Uiso 0.67 1 d P A 1 H12A H 1.2601 -0.1285 0.3737 0.144 Uiso 0.67 1 calc PR A 1 H12B H 1.1630 -0.1013 0.3931 0.144 Uiso 0.67 1 calc PR A 1 H12C H 1.2323 -0.1385 0.4207 0.144 Uiso 0.67 1 calc PR A 1 C13 C 1.386(2) -0.0590(15) 0.3911(11) 0.095(11) Uiso 0.67 1 d P A 1 H13A H 1.4106 -0.0200 0.3897 0.142 Uiso 0.67 1 calc PR A 1 H13B H 1.4064 -0.0741 0.3661 0.142 Uiso 0.67 1 calc PR A 1 H13C H 1.4095 -0.0859 0.4128 0.142 Uiso 0.67 1 calc PR A 1 C14 C 1.251(2) -0.0356(15) 0.4385(11) 0.095(11) Uiso 0.67 1 d P A 1 H14A H 1.2832 0.0001 0.4393 0.142 Uiso 0.67 1 calc PR A 1 H14B H 1.2692 -0.0670 0.4589 0.142 Uiso 0.67 1 calc PR A 1 H14C H 1.1832 -0.0276 0.4434 0.142 Uiso 0.67 1 calc PR A 1 C12A C 1.322(5) -0.099(3) 0.375(2) 0.09(2) Uiso 0.33 1 d P A 2 H12D H 1.3755 -0.0821 0.3575 0.137 Uiso 0.33 1 calc PR A 2 H12E H 1.2775 -0.1118 0.3601 0.137 Uiso 0.33 1 calc PR A 2 H12F H 1.3436 -0.1329 0.3934 0.137 Uiso 0.33 1 calc PR A 2 C13A C 1.340(4) -0.038(3) 0.4273(19) 0.069(17) Uiso 0.33 1 d P A 2 H13D H 1.3794 -0.0728 0.4357 0.104 Uiso 0.33 1 calc PR A 2 H13E H 1.3012 -0.0258 0.4505 0.104 Uiso 0.33 1 calc PR A 2 H13F H 1.3791 -0.0062 0.4137 0.104 Uiso 0.33 1 calc PR A 2 C14A C 1.180(3) -0.081(2) 0.4257(16) 0.050(14) Uiso 0.33 1 d P A 2 H14D H 1.1892 -0.0899 0.4536 0.076 Uiso 0.33 1 calc PR A 2 H14E H 1.1651 -0.1172 0.4166 0.076 Uiso 0.33 1 calc PR A 2 H14F H 1.1279 -0.0520 0.4229 0.076 Uiso 0.33 1 calc PR A 2 C15 C 1.1793(9) -0.0060(6) 0.3439(4) 0.030(4) Uiso 1 1 d . . . H15A H 1.1533 -0.0431 0.3449 0.036 Uiso 1 1 calc R A . C16 C 1.0805(9) -0.0231(6) 0.2766(4) 0.023(3) Uiso 1 1 d . . . C17 C 1.1289(9) -0.0266(6) 0.2396(4) 0.024(3) Uiso 1 1 d . . . C18 C 1.1257(9) -0.0759(6) 0.2214(4) 0.024(3) Uiso 1 1 d . . . C19 C 1.1699(9) -0.0821(6) 0.1782(4) 0.028(4) Uiso 1 1 d . . . C20 C 1.2791(10) -0.0791(7) 0.1727(5) 0.048(5) Uiso 1 1 d . . . H20A H 1.3032 -0.1012 0.1960 0.072 Uiso 1 1 calc R . . H20B H 1.2960 -0.0379 0.1695 0.072 Uiso 1 1 calc R . . H20C H 1.3062 -0.0962 0.1491 0.072 Uiso 1 1 calc R . . C21 C 1.1477(12) -0.1376(7) 0.1641(5) 0.055(5) Uiso 1 1 d . . . H21A H 1.1720 -0.1719 0.1809 0.082 Uiso 1 1 calc R . . H21B H 1.1767 -0.1375 0.1366 0.082 Uiso 1 1 calc R . . H21C H 1.0799 -0.1396 0.1657 0.082 Uiso 1 1 calc R . . C22 C 1.1364(12) -0.0282(7) 0.1479(5) 0.058(5) Uiso 1 1 d . . . H22A H 1.0706 -0.0319 0.1456 0.087 Uiso 1 1 calc R . . H22B H 1.1741 -0.0284 0.1220 0.087 Uiso 1 1 calc R . . H22C H 1.1440 0.0087 0.1576 0.087 Uiso 1 1 calc R . . C23 C 1.0758(9) -0.1239(6) 0.2425(4) 0.028(4) Uiso 1 1 d . . . H23A H 1.0709 -0.1571 0.2298 0.034 Uiso 1 1 calc R . . C24 C 1.0333(10) -0.1244(6) 0.2812(4) 0.031(4) Uiso 1 1 d . . . C25 C 0.9793(11) -0.1766(7) 0.3042(5) 0.047(5) Uiso 1 1 d . . . C26 C 0.9607(14) -0.2181(9) 0.2755(6) 0.075(6) Uiso 1 1 d . . . H26A H 1.0152 -0.2202 0.2553 0.112 Uiso 1 1 calc R . . H26B H 0.9061 -0.2029 0.2628 0.112 Uiso 1 1 calc R . . H26C H 0.9489 -0.2574 0.2903 0.112 Uiso 1 1 calc R . . C27 C 0.8815(14) -0.1565(9) 0.3238(7) 0.086(7) Uiso 1 1 d . . . H27A H 0.8824 -0.1572 0.3522 0.129 Uiso 1 1 calc R . . H27B H 0.8348 -0.1833 0.3200 0.129 Uiso 1 1 calc R . . H27C H 0.8655 -0.1165 0.3116 0.129 Uiso 1 1 calc R . . C28 C 1.0300(15) -0.2058(10) 0.3375(7) 0.090(7) Uiso 1 1 d . . . H28A H 1.0954 -0.2141 0.3273 0.135 Uiso 1 1 calc R . . H28B H 1.0006 -0.2427 0.3495 0.135 Uiso 1 1 calc R . . H28C H 1.0270 -0.1796 0.3575 0.135 Uiso 1 1 calc R . . C29 C 1.0334(9) -0.0729(6) 0.2968(4) 0.024(3) Uiso 1 1 d . . . H29A H 1.0001 -0.0709 0.3224 0.029 Uiso 1 1 calc R . . C30 C 0.9733(10) 0.0414(6) 0.3190(4) 0.030(4) Uiso 1 1 d . . . C31 C 0.8966(9) 0.0703(6) 0.3011(4) 0.023(3) Uiso 1 1 d . . . C32 C 0.8134(10) 0.0883(6) 0.3254(5) 0.033(4) Uiso 1 1 d . . . C33 C 0.7373(11) 0.1259(7) 0.3080(5) 0.042(4) Uiso 1 1 d . . . C34 C 0.6584(11) 0.1390(8) 0.3402(5) 0.055(5) Uiso 1 1 d . . . H34A H 0.6840 0.1551 0.3608 0.082 Uiso 1 1 calc R . . H34B H 0.6272 0.1025 0.3518 0.082 Uiso 1 1 calc R . . H34C H 0.6132 0.1677 0.3287 0.082 Uiso 1 1 calc R . . C35 C 0.7782(11) 0.1853(7) 0.2884(5) 0.051(5) Uiso 1 1 d . . . H35A H 0.8056 0.2028 0.3080 0.077 Uiso 1 1 calc R . . H35B H 0.7284 0.2119 0.2786 0.077 Uiso 1 1 calc R . . H35C H 0.8265 0.1789 0.2663 0.077 Uiso 1 1 calc R . . C36 C 0.6911(12) 0.0982(8) 0.2773(6) 0.061(5) Uiso 1 1 d . . . H36A H 0.6767 0.0573 0.2881 0.091 Uiso 1 1 calc R . . H36B H 0.7342 0.0991 0.2526 0.091 Uiso 1 1 calc R . . H36C H 0.6333 0.1207 0.2721 0.091 Uiso 1 1 calc R . . C37 C 0.8092(11) 0.0678(6) 0.3650(5) 0.038(4) Uiso 1 1 d . . . H37A H 0.7530 0.0768 0.3813 0.046 Uiso 1 1 calc R . . C38 C 0.8799(10) 0.0347(6) 0.3842(5) 0.035(4) Uiso 1 1 d . . . C39 C 0.8740(13) 0.0111(8) 0.4282(6) 0.062(5) Uiso 1 1 d . . . C40 C 0.7792(15) 0.0318(10) 0.4485(7) 0.091(7) Uiso 1 1 d . . . H40A H 0.7292 0.0184 0.4361 0.137 Uiso 1 1 calc R . . H40B H 0.7756 0.0749 0.4456 0.137 Uiso 1 1 calc R . . H40C H 0.7720 0.0153 0.4766 0.137 Uiso 1 1 calc R . . C41 C 0.8801(16) -0.0559(9) 0.4343(7) 0.096(8) Uiso 1 1 d . . . H41A H 0.8182 -0.0707 0.4343 0.143 Uiso 1 1 calc R . . H41B H 0.9022 -0.0706 0.4596 0.143 Uiso 1 1 calc R . . H41C H 0.9238 -0.0695 0.4128 0.143 Uiso 1 1 calc R . . C42 C 0.9552(17) 0.0371(11) 0.4443(8) 0.113(9) Uiso 1 1 d . . . H42A H 0.9341 0.0750 0.4528 0.169 Uiso 1 1 calc R . . H42B H 1.0086 0.0428 0.4233 0.169 Uiso 1 1 calc R . . H42C H 0.9738 0.0097 0.4668 0.169 Uiso 1 1 calc R . . C43 C 0.9627(10) 0.0253(6) 0.3591(5) 0.036(4) Uiso 1 1 d . . . H43A H 1.0146 0.0067 0.3706 0.044 Uiso 1 1 calc R . . C44 C 1.0739(10) 0.1700(7) 0.2975(5) 0.039(4) Uiso 1 1 d . . . H44A H 1.0758 0.1980 0.3164 0.047 Uiso 1 1 calc R . . H44B H 1.0284 0.1399 0.3097 0.047 Uiso 1 1 calc R . . C45 C 1.0445(10) 0.2026(6) 0.2589(4) 0.032(4) Uiso 1 1 d . . . H45A H 1.0503 0.1754 0.2390 0.039 Uiso 1 1 calc R . . H45B H 0.9784 0.2166 0.2636 0.039 Uiso 1 1 calc R . . C46 C 1.1163(10) 0.2769(7) 0.2054(5) 0.033(4) Uiso 1 1 d . . . C47 C 1.1722(9) 0.3320(6) 0.1940(4) 0.025(3) Uiso 1 1 d . . . H47A H 1.1952 0.3420 0.2176 0.031 Uiso 1 1 calc R . . H47B H 1.1318 0.3653 0.1835 0.031 Uiso 1 1 calc R . . C48 C 1.2923(9) 0.3891(6) 0.1261(4) 0.028(4) Uiso 1 1 d . . . C49 C 1.3105(12) 0.3905(8) 0.0849(5) 0.055(5) Uiso 1 1 d . . . H49A H 1.3129 0.3554 0.0734 0.066 Uiso 1 1 calc R . . C50 C 1.3244(12) 0.4437(8) 0.0621(6) 0.060(5) Uiso 1 1 d . . . H50A H 1.3329 0.4461 0.0341 0.072 Uiso 1 1 calc R . . C51 C 1.3266(13) 0.4936(9) 0.0785(6) 0.071(6) Uiso 1 1 d . . . H51A H 1.3394 0.5299 0.0619 0.085 Uiso 1 1 calc R . . C52 C 1.3104(13) 0.4920(9) 0.1190(6) 0.067(6) Uiso 1 1 d . . . H52A H 1.3124 0.5271 0.1301 0.080 Uiso 1 1 calc R . . C53 C 1.2916(11) 0.4407(7) 0.1428(5) 0.049(5) Uiso 1 1 d . . . H53A H 1.2782 0.4396 0.1707 0.059 Uiso 1 1 calc R . . C54 C 1.3701(9) 0.2963(6) 0.1807(4) 0.029(4) Uiso 1 1 d . . . C55 C 1.4007(11) 0.2391(7) 0.1827(5) 0.045(4) Uiso 1 1 d . . . H55A H 1.3648 0.2120 0.1738 0.054 Uiso 1 1 calc R . . C56 C 1.4827(12) 0.2191(8) 0.1975(6) 0.060(5) Uiso 1 1 d . . . H56A H 1.5039 0.1791 0.1981 0.072 Uiso 1 1 calc R . . C57 C 1.5317(13) 0.2574(8) 0.2108(6) 0.059(5) Uiso 1 1 d . . . H57A H 1.5847 0.2431 0.2233 0.071 Uiso 1 1 calc R . . C58 C 1.5088(15) 0.3140(10) 0.2072(6) 0.081(7) Uiso 1 1 d . . . H58A H 1.5481 0.3406 0.2147 0.098 Uiso 1 1 calc R . . C59 C 1.4239(15) 0.3355(10) 0.1919(7) 0.086(7) Uiso 1 1 d . . . H59A H 1.4056 0.3761 0.1897 0.104 Uiso 1 1 calc R . . C60 C 1.2624(9) 0.0322(6) 0.2294(4) 0.030(4) Uiso 1 1 d . . . H60A H 1.3063 -0.0015 0.2243 0.036 Uiso 1 1 calc R . . H60B H 1.2556 0.0352 0.2579 0.036 Uiso 1 1 calc R . . C61 C 1.3000(9) 0.0881(6) 0.2054(4) 0.026(3) Uiso 1 1 d . . . H61A H 1.2542 0.1212 0.2093 0.031 Uiso 1 1 calc R . . H61B H 1.3584 0.0969 0.2146 0.031 Uiso 1 1 calc R . . C62 C 1.2641(10) 0.1093(6) 0.1372(4) 0.026(4) Uiso 1 1 d . . . C63 C 1.2856(10) 0.0920(6) 0.0967(4) 0.029(4) Uiso 1 1 d . . . H63A H 1.2317 0.0723 0.0907 0.035 Uiso 1 1 calc R . . H63B H 1.3402 0.0639 0.0957 0.035 Uiso 1 1 calc R . . C64 C 1.4305(10) 0.1721(6) 0.0583(5) 0.032(4) Uiso 1 1 d . . . C65 C 1.4477(13) 0.2104(8) 0.0830(6) 0.063(5) Uiso 1 1 d . . . H65A H 1.3979 0.2322 0.0961 0.075 Uiso 1 1 calc R . . C66 C 1.5385(15) 0.2166(9) 0.0885(7) 0.080(7) Uiso 1 1 d . . . H66A H 1.5518 0.2387 0.1079 0.096 Uiso 1 1 calc R . . C67 C 1.6118(13) 0.1895(8) 0.0648(6) 0.060(5) Uiso 1 1 d . . . H67A H 1.6746 0.1989 0.0650 0.072 Uiso 1 1 calc R . . C68 C 1.5934(11) 0.1507(7) 0.0421(5) 0.046(4) Uiso 1 1 d . . . H68A H 1.6424 0.1290 0.0285 0.055 Uiso 1 1 calc R . . C69 C 1.5019(10) 0.1432(7) 0.0389(5) 0.040(4) Uiso 1 1 d . . . H69A H 1.4884 0.1166 0.0223 0.048 Uiso 1 1 calc R . . C70 C 1.2993(10) 0.1365(6) 0.0126(4) 0.032(4) Uiso 1 1 d . . . C71 C 1.2643(11) 0.1803(8) -0.0149(5) 0.053(5) Uiso 1 1 d . . . H71A H 1.2493 0.2188 -0.0085 0.063 Uiso 1 1 calc R . . C72 C 1.2516(14) 0.1672(9) -0.0519(7) 0.077(6) Uiso 1 1 d . . . H72A H 1.2284 0.1965 -0.0711 0.092 Uiso 1 1 calc R . . C73 C 1.2735(13) 0.1109(8) -0.0598(6) 0.064(6) Uiso 1 1 d . . . H73A H 1.2658 0.1016 -0.0850 0.077 Uiso 1 1 calc R . . C74 C 1.3050(13) 0.0691(9) -0.0333(6) 0.065(6) Uiso 1 1 d . . . H74A H 1.3192 0.0307 -0.0399 0.078 Uiso 1 1 calc R . . C75 C 1.3175(12) 0.0801(8) 0.0028(6) 0.054(5) Uiso 1 1 d . . . H75A H 1.3386 0.0493 0.0216 0.065 Uiso 1 1 calc R . . C76 C 0.9001(10) 0.0396(6) 0.2400(4) 0.029(4) Uiso 1 1 d . . . H76A H 0.8336 0.0345 0.2384 0.035 Uiso 1 1 calc R . . H76B H 0.9258 0.0026 0.2541 0.035 Uiso 1 1 calc R . . C77 C 0.9530(11) 0.0528(7) 0.1992(5) 0.040(4) Uiso 1 1 d . . . H77A H 1.0121 0.0708 0.2011 0.048 Uiso 1 1 calc R . . H77B H 0.9694 0.0153 0.1888 0.048 Uiso 1 1 calc R . . C78 C 0.9324(9) 0.1397(6) 0.1484(4) 0.022(3) Uiso 1 1 d . . . C79 C 0.8831(9) 0.1625(6) 0.1150(4) 0.027(4) Uiso 1 1 d . . . H79A H 0.8641 0.2044 0.1156 0.032 Uiso 1 1 calc R . . H79B H 0.8263 0.1402 0.1164 0.032 Uiso 1 1 calc R . . C80 C 0.9838(10) 0.0793(6) 0.0670(4) 0.029(4) Uiso 1 1 d . . . C81 C 0.9168(10) 0.0367(6) 0.0832(5) 0.037(4) Uiso 1 1 d . . . H81A H 0.8585 0.0481 0.0970 0.044 Uiso 1 1 calc R . . C82 C 0.9378(12) -0.0221(8) 0.0786(5) 0.054(5) Uiso 1 1 d . . . H82A H 0.8926 -0.0506 0.0891 0.065 Uiso 1 1 calc R . . C83 C 1.0232(11) -0.0400(7) 0.0591(5) 0.046(4) Uiso 1 1 d . . . H83A H 1.0370 -0.0802 0.0566 0.055 Uiso 1 1 calc R . . C84 C 1.0860(12) 0.0010(7) 0.0439(5) 0.052(5) Uiso 1 1 d . . . H84A H 1.1449 -0.0109 0.0309 0.062 Uiso 1 1 calc R . . C85 C 1.0671(10) 0.0601(6) 0.0467(4) 0.029(4) Uiso 1 1 d . . . H85A H 1.1119 0.0880 0.0344 0.035 Uiso 1 1 calc R . . C86 C 0.8984(9) 0.1835(6) 0.0285(4) 0.024(3) Uiso 1 1 d . . . C87 C 0.8694(10) 0.1483(7) 0.0052(5) 0.036(4) Uiso 1 1 d . . . H87A H 0.8819 0.1070 0.0102 0.043 Uiso 1 1 calc R . . C88 C 0.8216(11) 0.1722(7) -0.0260(5) 0.044(4) Uiso 1 1 d . . . H88A H 0.8001 0.1477 -0.0423 0.053 Uiso 1 1 calc R . . C89 C 0.8062(11) 0.2325(7) -0.0329(5) 0.047(5) Uiso 1 1 d . . . H89A H 0.7744 0.2492 -0.0544 0.057 Uiso 1 1 calc R . . C90 C 0.8336(10) 0.2676(7) -0.0109(4) 0.034(4) Uiso 1 1 d . . . H90A H 0.8213 0.3089 -0.0163 0.041 Uiso 1 1 calc R . . C91 C 0.8816(10) 0.2430(7) 0.0208(5) 0.037(4) Uiso 1 1 d . . . H91A H 0.9024 0.2679 0.0369 0.045 Uiso 1 1 calc R . . N4 N 1.0055(9) 0.3421(7) 0.0997(3) 0.033(3) Uani 1 1 d . . . O10 O 0.9722(7) 0.2915(5) 0.1033(3) 0.041(3) Uani 1 1 d . . . O11 O 1.0936(7) 0.3412(4) 0.1024(3) 0.037(3) Uani 1 1 d . . . O12 O 0.9623(8) 0.3898(5) 0.0934(4) 0.054(3) Uani 1 1 d . . . Nd2 Nd 0.61525(6) -0.01921(4) 0.18144(3) 0.0419(3) Uani 1 1 d . . . N5 N 0.8049(9) -0.0664(6) 0.1788(5) 0.048(4) Uani 1 1 d . . . O13 O 0.7631(7) -0.0633(5) 0.1497(4) 0.050(3) Uani 1 1 d . . . O14 O 0.7618(8) -0.0519(6) 0.2097(4) 0.070(4) Uani 1 1 d . . . O15 O 0.8895(8) -0.0840(5) 0.1775(5) 0.081(5) Uani 1 1 d . . . N6 N 0.5087(12) -0.0036(7) 0.2576(6) 0.068(5) Uani 1 1 d . . . O16 O 0.5958(8) -0.0202(5) 0.2531(3) 0.055(3) Uani 1 1 d . . . O17 O 0.4712(8) -0.0042(6) 0.2259(5) 0.072(4) Uani 1 1 d . . . O18 O 0.4677(10) 0.0079(7) 0.2893(5) 0.095(5) Uani 1 1 d . . . N7 N 0.5332(9) 0.0144(6) 0.1093(5) 0.048(4) Uani 1 1 d . . . O19 O 0.6167(9) -0.0044(6) 0.1076(3) 0.069(4) Uani 1 1 d . . . O20 O 0.4979(8) 0.0321(5) 0.1395(4) 0.062(4) Uani 1 1 d . . . O21 O 0.4920(8) 0.0169(5) 0.0791(4) 0.059(4) Uani 1 1 d . . . N8 N 0.5357(10) -0.1351(7) 0.1816(5) 0.063(5) Uani 1 1 d . . . O22 O 0.5975(8) -0.1291(5) 0.2033(4) 0.059(3) Uani 1 1 d . . . O23 O 0.5103(11) -0.0887(7) 0.1634(6) 0.123(8) Uani 1 1 d . . . O24 O 0.5050(11) -0.1820(6) 0.1816(6) 0.113(7) Uani 1 1 d . . . N9 N 0.6669(9) 0.1053(7) 0.1738(5) 0.048(4) Uani 1 1 d . . . O25 O 0.7166(7) 0.0663(5) 0.1560(4) 0.049(3) Uani 1 1 d . . . O26 O 0.5929(9) 0.0878(5) 0.1948(4) 0.071(4) Uani 1 1 d . . . O27 O 0.6885(8) 0.1550(5) 0.1695(4) 0.070(4) Uani 1 1 d . . . Nd1' Nd 0.64308(5) -0.37542(4) 0.35335(3) 0.0271(2) Uani 1 1 d . . . P1' P 0.3976(3) -0.41476(19) 0.38492(13) 0.0348(11) Uani 1 1 d . . . P2' P 0.5797(3) -0.21707(17) 0.33350(12) 0.0299(10) Uani 1 1 d . . . P3' P 0.7171(3) -0.52980(18) 0.37800(12) 0.0306(10) Uani 1 1 d . . . O1' O 0.5224(6) -0.4301(4) 0.2115(3) 0.031(2) Uani 1 1 d . . . O2' O 0.7493(6) -0.3301(4) 0.1770(3) 0.026(2) Uani 1 1 d . . . O3' O 0.7773(6) -0.5111(4) 0.2090(3) 0.025(2) Uani 1 1 d . . . O4' O 0.5454(6) -0.4129(5) 0.3101(3) 0.040(3) Uani 1 1 d . . . O5' O 0.4830(6) -0.3841(4) 0.3861(3) 0.033(3) Uani 1 1 d . . . O6' O 0.6669(7) -0.3172(4) 0.2879(3) 0.039(3) Uani 1 1 d . . . O7' O 0.5768(7) -0.2764(4) 0.3581(3) 0.041(3) Uani 1 1 d . . . O8' O 0.7486(7) -0.4303(4) 0.3067(3) 0.040(3) Uani 1 1 d . . . O9' O 0.6500(6) -0.4788(4) 0.3817(3) 0.032(3) Uani 1 1 d . . . N1' N 0.4781(7) -0.4872(5) 0.2934(3) 0.029(3) Uani 1 1 d . . . H1'A H 0.4288 -0.5089 0.2988 0.035 Uiso 1 1 calc R . . N2' N 0.6388(8) -0.2529(5) 0.2344(3) 0.031(3) Uani 1 1 d . . . H2'A H 0.6422 -0.2165 0.2220 0.037 Uiso 1 1 calc R . . N3' N 0.8552(8) -0.4802(5) 0.2728(3) 0.027(3) Uani 1 1 d . . . H3'A H 0.8934 -0.5115 0.2725 0.033 Uiso 1 1 calc R . . C1' C 0.6866(8) -0.4323(6) 0.1541(4) 0.022(3) Uani 1 1 d . . . H1'B H 0.6877 -0.4281 0.1825 0.026 Uiso 1 1 calc R . . C2' C 0.5889(9) -0.4102(6) 0.1428(4) 0.022(3) Uiso 1 1 d . B . C3' C 0.5103(9) -0.4104(6) 0.1733(4) 0.023(3) Uiso 1 1 d . . . C4' C 0.4233(10) -0.3843(6) 0.1632(4) 0.030(4) Uiso 1 1 d . . . C5' C 0.3404(11) -0.3761(7) 0.1956(5) 0.040(4) Uiso 1 1 d . . . C6' C 0.3089(12) -0.4381(7) 0.2169(5) 0.056(5) Uiso 1 1 d . . . H6'A H 0.3523 -0.4544 0.2355 0.084 Uiso 1 1 calc R . . H6'B H 0.3089 -0.4644 0.1971 0.084 Uiso 1 1 calc R . . H6'C H 0.2459 -0.4344 0.2313 0.084 Uiso 1 1 calc R . . C7' C 0.2538(11) -0.3437(7) 0.1764(5) 0.054(5) Uiso 1 1 d . . . H7'A H 0.2707 -0.3041 0.1633 0.081 Uiso 1 1 calc R . . H7'B H 0.2005 -0.3408 0.1971 0.081 Uiso 1 1 calc R . . H7'C H 0.2370 -0.3663 0.1568 0.081 Uiso 1 1 calc R . . C8' C 0.3634(12) -0.3383(8) 0.2248(5) 0.056(5) Uiso 1 1 d . . . H8'A H 0.4174 -0.3561 0.2371 0.085 Uiso 1 1 calc R . . H8'B H 0.3096 -0.3354 0.2453 0.085 Uiso 1 1 calc R . . H8'C H 0.3781 -0.2989 0.2108 0.085 Uiso 1 1 calc R . . C9' C 0.4185(10) -0.3623(6) 0.1247(4) 0.034(4) Uiso 1 1 d . . . H9'A H 0.3605 -0.3452 0.1180 0.040 Uiso 1 1 calc R . . C10' C 0.4937(9) -0.3631(6) 0.0942(4) 0.026(3) Uiso 1 1 d . B . C11' C 0.4858(11) -0.3349(7) 0.0522(5) 0.039(4) Uiso 1 1 d . . . C12' C 0.5597(19) -0.2907(13) 0.0405(9) 0.067(8) Uiso 0.67 1 d P B 3 H12G H 0.5422 -0.2566 0.0541 0.100 Uiso 0.67 1 calc PR B 3 H12H H 0.5663 -0.2781 0.0118 0.100 Uiso 0.67 1 calc PR B 3 H12I H 0.6192 -0.3085 0.0478 0.100 Uiso 0.67 1 calc PR B 3 C13' C 0.5232(19) -0.3873(12) 0.0251(8) 0.062(8) Uiso 0.67 1 d P B 3 H13G H 0.5908 -0.3939 0.0245 0.093 Uiso 0.67 1 calc PR B 3 H13H H 0.5087 -0.3753 -0.0019 0.093 Uiso 0.67 1 calc PR B 3 H13I H 0.4921 -0.4238 0.0367 0.093 Uiso 0.67 1 calc PR B 3 C14' C 0.3964(19) -0.3118(13) 0.0430(9) 0.066(9) Uiso 0.67 1 d P B 3 H14G H 0.3703 -0.2851 0.0617 0.100 Uiso 0.67 1 calc PR B 3 H14H H 0.3546 -0.3443 0.0451 0.100 Uiso 0.67 1 calc PR B 3 H14I H 0.4031 -0.2903 0.0160 0.100 Uiso 0.67 1 calc PR B 3 C12B C 0.466(5) -0.268(3) 0.055(2) 0.08(2) Uiso 0.33 1 d P B 4 H12J H 0.4000 -0.2610 0.0643 0.127 Uiso 0.33 1 calc PR B 4 H12K H 0.4827 -0.2451 0.0288 0.127 Uiso 0.33 1 calc PR B 4 H12L H 0.5041 -0.2565 0.0736 0.127 Uiso 0.33 1 calc PR B 4 C13B C 0.557(4) -0.339(3) 0.0226(16) 0.057(15) Uiso 0.33 1 d P B 4 H13J H 0.6123 -0.3211 0.0287 0.085 Uiso 0.33 1 calc PR B 4 H13K H 0.5394 -0.3179 -0.0023 0.085 Uiso 0.33 1 calc PR B 4 H13L H 0.5724 -0.3803 0.0201 0.085 Uiso 0.33 1 calc PR B 4 C14B C 0.391(3) -0.354(2) 0.0378(15) 0.041(13) Uiso 0.33 1 d P B 4 H14J H 0.3454 -0.3204 0.0372 0.061 Uiso 0.33 1 calc PR B 4 H14K H 0.3649 -0.3872 0.0563 0.061 Uiso 0.33 1 calc PR B 4 H14L H 0.4062 -0.3647 0.0112 0.061 Uiso 0.33 1 calc PR B 4 C15' C 0.5782(9) -0.3879(6) 0.1045(4) 0.024(3) Uiso 1 1 d . . . H15B H 0.6301 -0.3895 0.0844 0.029 Uiso 1 1 calc R B . C16' C 0.7629(9) -0.3922(6) 0.1274(4) 0.023(3) Uiso 1 1 d . C . C17' C 0.7946(10) -0.3436(6) 0.1396(5) 0.032(4) Uiso 1 1 d . . . C18' C 0.8709(9) -0.3141(6) 0.1194(4) 0.029(4) Uiso 1 1 d . . . C19' C 0.9172(10) -0.2681(7) 0.1385(5) 0.038(4) Uiso 1 1 d . . . C20' C 0.9584(12) -0.3032(7) 0.1734(5) 0.055(5) Uiso 1 1 d . . . H20D H 1.0146 -0.3256 0.1638 0.082 Uiso 1 1 calc R . . H20E H 0.9125 -0.3304 0.1886 0.082 Uiso 1 1 calc R . . H20F H 0.9747 -0.2762 0.1905 0.082 Uiso 1 1 calc R . . C21' C 0.8556(12) -0.2153(7) 0.1498(5) 0.053(5) Uiso 1 1 d . . . H21D H 0.8087 -0.2285 0.1725 0.080 Uiso 1 1 calc R . . H21E H 0.8241 -0.1973 0.1273 0.080 Uiso 1 1 calc R . . H21F H 0.8943 -0.1864 0.1570 0.080 Uiso 1 1 calc R . . C22' C 0.9970(12) -0.2396(8) 0.1095(6) 0.065(6) Uiso 1 1 d . . . H22D H 1.0435 -0.2701 0.1019 0.098 Uiso 1 1 calc R . . H22E H 1.0261 -0.2116 0.1221 0.098 Uiso 1 1 calc R . . H22F H 0.9726 -0.2188 0.0858 0.098 Uiso 1 1 calc R . . C23' C 0.9027(9) -0.3272(6) 0.0828(4) 0.027(4) Uiso 1 1 d . . . H23B H 0.9503 -0.3042 0.0669 0.033 Uiso 1 1 calc R . . C24' C 0.8685(9) -0.3737(6) 0.0669(4) 0.027(4) Uiso 1 1 d . C . C25' C 0.9009(10) -0.3828(7) 0.0245(5) 0.036(4) Uiso 1 1 d . . . C26' C 0.876(2) -0.3259(13) -0.0053(9) 0.073(9) Uiso 0.66 1 d P C 5 H26D H 0.8232 -0.3038 0.0071 0.109 Uiso 0.66 1 calc PR C 5 H26E H 0.8606 -0.3377 -0.0295 0.109 Uiso 0.66 1 calc PR C 5 H26F H 0.9305 -0.3009 -0.0120 0.109 Uiso 0.66 1 calc PR C 5 C27' C 1.0057(15) -0.3934(11) 0.0155(7) 0.039(6) Uiso 0.66 1 d P C 5 H27D H 1.0374 -0.3683 0.0294 0.058 Uiso 0.66 1 calc PR C 5 H27E H 1.0251 -0.3839 -0.0131 0.058 Uiso 0.66 1 calc PR C 5 H27F H 1.0222 -0.4348 0.0243 0.058 Uiso 0.66 1 calc PR C 5 C28' C 0.8545(18) -0.4312(11) 0.0115(8) 0.048(7) Uiso 0.66 1 d P C 5 H28D H 0.7867 -0.4235 0.0151 0.072 Uiso 0.66 1 calc PR C 5 H28E H 0.8695 -0.4688 0.0275 0.072 Uiso 0.66 1 calc PR C 5 H28F H 0.8767 -0.4331 -0.0165 0.072 Uiso 0.66 1 calc PR C 5 C26B C 0.979(3) -0.349(2) 0.0071(15) 0.043(13) Uiso 0.33 1 d P C 6 H26G H 0.9605 -0.3066 0.0054 0.064 Uiso 0.33 1 calc PR C 6 H26H H 1.0008 -0.3581 -0.0195 0.064 Uiso 0.33 1 calc PR C 6 H26I H 1.0294 -0.3575 0.0235 0.064 Uiso 0.33 1 calc PR C 6 C27B C 0.923(7) -0.448(4) 0.025(3) 0.15(4) Uiso 0.33 1 d P C 6 H27G H 0.8721 -0.4699 0.0420 0.226 Uiso 0.33 1 calc PR C 6 H27H H 0.9813 -0.4585 0.0364 0.226 Uiso 0.33 1 calc PR C 6 H27I H 0.9294 -0.4574 -0.0015 0.226 Uiso 0.33 1 calc PR C 6 C28B C 0.822(3) -0.379(2) 0.0043(15) 0.046(14) Uiso 0.33 1 d P C 6 H28G H 0.8006 -0.3371 -0.0014 0.069 Uiso 0.33 1 calc PR C 6 H28H H 0.7713 -0.4009 0.0210 0.069 Uiso 0.33 1 calc PR C 6 H28I H 0.8381 -0.3947 -0.0205 0.069 Uiso 0.33 1 calc PR C 6 C29' C 0.8001(9) -0.4060(6) 0.0913(4) 0.022(3) Uiso 1 1 d . . . H29B H 0.7781 -0.4391 0.0826 0.026 Uiso 1 1 calc R C . C30' C 0.7087(9) -0.4974(6) 0.1492(4) 0.021(3) Uiso 1 1 d . . . C31' C 0.7563(9) -0.5338(6) 0.1770(4) 0.025(3) Uiso 1 1 d . . . C32' C 0.7693(9) -0.5943(6) 0.1744(4) 0.026(3) Uiso 1 1 d . . . C33' C 0.8167(10) -0.6365(6) 0.2064(5) 0.034(4) Uiso 1 1 d . . . C34' C 0.9146(11) -0.6213(7) 0.2100(5) 0.053(5) Uiso 1 1 d . . . H34D H 0.9119 -0.5891 0.2257 0.079 Uiso 1 1 calc R . . H34E H 0.9483 -0.6089 0.1835 0.079 Uiso 1 1 calc R . . H34F H 0.9472 -0.6559 0.2230 0.079 Uiso 1 1 calc R . . C35' C 0.8253(12) -0.7007(7) 0.1951(6) 0.060(5) Uiso 1 1 d . . . H35D H 0.8338 -0.7294 0.2186 0.090 Uiso 1 1 calc R . . H35E H 0.8792 -0.7038 0.1747 0.090 Uiso 1 1 calc R . . H35F H 0.7684 -0.7087 0.1850 0.090 Uiso 1 1 calc R . . C36' C 0.7582(11) -0.6374(7) 0.2463(5) 0.052(5) Uiso 1 1 d . . . H36D H 0.7510 -0.5975 0.2531 0.078 Uiso 1 1 calc R . . H36E H 0.7889 -0.6634 0.2663 0.078 Uiso 1 1 calc R . . H36F H 0.6966 -0.6519 0.2453 0.078 Uiso 1 1 calc R . . C37' C 0.7440(11) -0.6138(7) 0.1419(5) 0.043(4) Uiso 1 1 d . . . H37B H 0.7586 -0.6537 0.1386 0.052 Uiso 1 1 calc R . . C38' C 0.6986(9) -0.5783(6) 0.1141(4) 0.021(3) Uiso 1 1 d . . . C39' C 0.6659(11) -0.6021(7) 0.0798(5) 0.045(4) Uiso 1 1 d . . . C40' C 0.7023(16) -0.5690(10) 0.0447(7) 0.105(8) Uiso 1 1 d . . . H40D H 0.6960 -0.5897 0.0225 0.157 Uiso 1 1 calc R . . H40E H 0.7685 -0.5631 0.0451 0.157 Uiso 1 1 calc R . . H40F H 0.6684 -0.5307 0.0414 0.157 Uiso 1 1 calc R . . C41' C 0.7132(15) -0.6613(9) 0.0738(7) 0.093(7) Uiso 1 1 d . . . H41D H 0.6912 -0.6751 0.0515 0.140 Uiso 1 1 calc R . . H41E H 0.6981 -0.6897 0.0979 0.140 Uiso 1 1 calc R . . H41F H 0.7810 -0.6573 0.0683 0.140 Uiso 1 1 calc R . . C42' C 0.5679(14) -0.6100(10) 0.0866(7) 0.089(7) Uiso 1 1 d . . . H42D H 0.5482 -0.6217 0.0631 0.134 Uiso 1 1 calc R . . H42E H 0.5350 -0.5729 0.0920 0.134 Uiso 1 1 calc R . . H42F H 0.5532 -0.6407 0.1094 0.134 Uiso 1 1 calc R . . C43' C 0.6785(9) -0.5222(6) 0.1202(4) 0.022(3) Uiso 1 1 d . . . H43B H 0.6408 -0.4983 0.1031 0.026 Uiso 1 1 calc R . . C44' C 0.5334(10) -0.4924(6) 0.2228(4) 0.028(4) Uiso 1 1 d . . . H44C H 0.5840 -0.5086 0.2046 0.034 Uiso 1 1 calc R . . H44D H 0.4749 -0.5113 0.2213 0.034 Uiso 1 1 calc R . . C45' C 0.5567(10) -0.5051(7) 0.2645(4) 0.035(4) Uiso 1 1 d . . . H45C H 0.5716 -0.5478 0.2713 0.042 Uiso 1 1 calc R . . H45D H 0.6127 -0.4837 0.2663 0.042 Uiso 1 1 calc R . . C46' C 0.4774(10) -0.4418(6) 0.3111(4) 0.027(4) Uiso 1 1 d . . . C47' C 0.3863(9) -0.4251(6) 0.3358(4) 0.027(4) Uiso 1 1 d . . . H47C H 0.3416 -0.4563 0.3372 0.032 Uiso 1 1 calc R . . H47D H 0.3594 -0.3882 0.3221 0.032 Uiso 1 1 calc R . . C48' C 0.2943(10) -0.3692(7) 0.3991(5) 0.037(4) Uiso 1 1 d . . . C49' C 0.3079(16) -0.3205(10) 0.4078(7) 0.083(7) Uiso 1 1 d . . . H49B H 0.3700 -0.3087 0.4062 0.099 Uiso 1 1 calc R . . C50' C 0.2269(19) -0.2794(12) 0.4210(8) 0.121(9) Uiso 1 1 d . . . H50B H 0.2345 -0.2455 0.4325 0.145 Uiso 1 1 calc R . . C51' C 0.1406(16) -0.2963(10) 0.4146(7) 0.083(7) Uiso 1 1 d . . . H51B H 0.0874 -0.2707 0.4194 0.100 Uiso 1 1 calc R . . C52' C 0.129(2) -0.3450(13) 0.4025(9) 0.131(10) Uiso 1 1 d . . . H52B H 0.0691 -0.3538 0.3980 0.157 Uiso 1 1 calc R . . C53' C 0.2089(15) -0.3879(10) 0.3952(7) 0.087(7) Uiso 1 1 d . . . H53B H 0.2009 -0.4255 0.3885 0.104 Uiso 1 1 calc R . . C54' C 0.3953(10) -0.4844(7) 0.4157(5) 0.039(4) Uiso 1 1 d . . . C55' C 0.4567(11) -0.4946(7) 0.4446(5) 0.045(4) Uiso 1 1 d . . . H55B H 0.4964 -0.4647 0.4474 0.053 Uiso 1 1 calc R . . C56' C 0.4583(12) -0.5476(8) 0.4682(5) 0.054(5) Uiso 1 1 d . . . H56B H 0.5035 -0.5563 0.4859 0.065 Uiso 1 1 calc R . . C57' C 0.3967(14) -0.5877(9) 0.4668(6) 0.073(6) Uiso 1 1 d . . . H57B H 0.3944 -0.6229 0.4854 0.087 Uiso 1 1 calc R . . C58' C 0.3335(15) -0.5787(9) 0.4375(6) 0.079(6) Uiso 1 1 d . . . H58B H 0.2910 -0.6078 0.4361 0.095 Uiso 1 1 calc R . . C59' C 0.3367(13) -0.5283(8) 0.4124(6) 0.060(5) Uiso 1 1 d . . . H59B H 0.2982 -0.5222 0.3920 0.073 Uiso 1 1 calc R . . C60' C 0.6614(10) -0.2963(6) 0.1741(4) 0.033(4) Uiso 1 1 d . . . H60C H 0.6239 -0.3138 0.1574 0.039 Uiso 1 1 calc R . . H60D H 0.6736 -0.2553 0.1617 0.039 Uiso 1 1 calc R . . C61' C 0.6099(10) -0.2972(7) 0.2145(5) 0.037(4) Uiso 1 1 d . . . H61C H 0.5422 -0.2911 0.2129 0.045 Uiso 1 1 calc R . . H61D H 0.6200 -0.3364 0.2302 0.045 Uiso 1 1 calc R . . C62' C 0.6605(10) -0.2648(7) 0.2709(5) 0.031(4) Uiso 1 1 d . . . C63' C 0.6731(9) -0.2154(6) 0.2916(4) 0.023(3) Uiso 1 1 d . . . H63C H 0.6694 -0.1777 0.2735 0.027 Uiso 1 1 calc R . . H63D H 0.7348 -0.2195 0.3010 0.027 Uiso 1 1 calc R . . C64' C 0.4746(10) -0.2006(6) 0.3132(4) 0.028(4) Uiso 1 1 d . . . C65' C 0.4108(15) -0.2409(10) 0.3165(7) 0.081(7) Uiso 1 1 d . . . H65B H 0.4243 -0.2799 0.3287 0.097 Uiso 1 1 calc R . . C66' C 0.3246(16) -0.2279(10) 0.3027(7) 0.085(7) Uiso 1 1 d . . . H66B H 0.2799 -0.2574 0.3066 0.102 Uiso 1 1 calc R . . C67' C 0.3055(14) -0.1757(8) 0.2846(6) 0.064(6) Uiso 1 1 d . . . H67B H 0.2460 -0.1673 0.2760 0.077 Uiso 1 1 calc R . . C68' C 0.3658(14) -0.1345(9) 0.2779(6) 0.072(6) Uiso 1 1 d . . . H68B H 0.3522 -0.0973 0.2632 0.087 Uiso 1 1 calc R . . C69' C 0.4521(13) -0.1464(8) 0.2930(6) 0.066(6) Uiso 1 1 d . . . H69B H 0.4955 -0.1161 0.2891 0.079 Uiso 1 1 calc R . . C70' C 0.6005(11) -0.1595(7) 0.3614(5) 0.040(4) Uiso 1 1 d . . . C71' C 0.5782(13) -0.1751(9) 0.4015(6) 0.064(5) Uiso 1 1 d . . . H71B H 0.5536 -0.2121 0.4127 0.077 Uiso 1 1 calc R . . C72' C 0.5942(17) -0.1320(12) 0.4254(9) 0.111(9) Uiso 1 1 d . . . H72B H 0.5843 -0.1407 0.4535 0.133 Uiso 1 1 calc R . . C73' C 0.6229(16) -0.0804(11) 0.4075(8) 0.102(8) Uiso 1 1 d . . . H73B H 0.6281 -0.0520 0.4242 0.122 Uiso 1 1 calc R . . C74' C 0.6452(15) -0.0634(10) 0.3695(7) 0.088(7) Uiso 1 1 d . . . H74B H 0.6678 -0.0254 0.3592 0.106 Uiso 1 1 calc R . . C75' C 0.6332(11) -0.1061(7) 0.3436(6) 0.052(5) Uiso 1 1 d . . . H75B H 0.6476 -0.0971 0.3157 0.062 Uiso 1 1 calc R . . C76' C 0.8584(9) -0.4748(6) 0.2007(4) 0.029(4) Uiso 1 1 d . . . H76C H 0.8573 -0.4478 0.1754 0.035 Uiso 1 1 calc R . . H76D H 0.9167 -0.4997 0.1988 0.035 Uiso 1 1 calc R . . C77' C 0.8521(10) -0.4391(6) 0.2360(4) 0.032(4) Uiso 1 1 d . . . H77C H 0.9049 -0.4125 0.2317 0.038 Uiso 1 1 calc R . . H77D H 0.7933 -0.4147 0.2377 0.038 Uiso 1 1 calc R . . C78' C 0.8035(9) -0.4724(6) 0.3059(4) 0.020(3) Uiso 1 1 d . . . C79' C 0.8208(10) -0.5137(7) 0.3443(5) 0.037(4) Uiso 1 1 d . . . H79C H 0.8645 -0.4953 0.3577 0.044 Uiso 1 1 calc R . . H79D H 0.8511 -0.5511 0.3371 0.044 Uiso 1 1 calc R . . C80' C 0.7614(11) -0.5566(7) 0.4231(5) 0.038(4) Uiso 1 1 d . . . C81' C 0.7242(12) -0.5317(8) 0.4554(5) 0.056(5) Uiso 1 1 d . . . H81B H 0.6766 -0.5015 0.4530 0.067 Uiso 1 1 calc R . . C82' C 0.7557(14) -0.5503(9) 0.4928(7) 0.079(6) Uiso 1 1 d . . . H82B H 0.7273 -0.5345 0.5157 0.095 Uiso 1 1 calc R . . C83' C 0.8305(15) -0.5931(9) 0.4950(7) 0.083(7) Uiso 1 1 d . . . H83B H 0.8519 -0.6073 0.5197 0.099 Uiso 1 1 calc R . . C84' C 0.8724(16) -0.6141(10) 0.4605(7) 0.088(7) Uiso 1 1 d . . . H84B H 0.9260 -0.6400 0.4608 0.106 Uiso 1 1 calc R . . C85' C 0.8348(12) -0.5965(8) 0.4262(6) 0.056(5) Uiso 1 1 d . . . H85B H 0.8613 -0.6130 0.4033 0.068 Uiso 1 1 calc R . . C86' C 0.6634(10) -0.5888(7) 0.3648(5) 0.037(4) Uiso 1 1 d . . . C87' C 0.7143(12) -0.6382(7) 0.3529(5) 0.049(5) Uiso 1 1 d . . . H87B H 0.7805 -0.6400 0.3506 0.059 Uiso 1 1 calc R . . C88' C 0.6677(13) -0.6846(9) 0.3445(6) 0.064(5) Uiso 1 1 d . . . H88B H 0.7015 -0.7185 0.3367 0.077 Uiso 1 1 calc R . . C89' C 0.5723(14) -0.6807(9) 0.3478(6) 0.072(6) Uiso 1 1 d . . . H89B H 0.5411 -0.7122 0.3415 0.086 Uiso 1 1 calc R . . C90' C 0.5184(14) -0.6324(8) 0.3600(6) 0.070(6) Uiso 1 1 d . . . H90B H 0.4523 -0.6313 0.3622 0.084 Uiso 1 1 calc R . . C91' C 0.5652(11) -0.5861(8) 0.3689(5) 0.049(5) Uiso 1 1 d . . . H91B H 0.5309 -0.5528 0.3776 0.058 Uiso 1 1 calc R . . N4' N 0.8337(9) -0.3454(7) 0.3657(4) 0.044(4) Uani 1 1 d . . . O10' O 0.8065(7) -0.3975(5) 0.3778(4) 0.057(4) Uani 1 1 d . . . O11' O 0.7808(8) -0.3071(5) 0.3526(4) 0.068(4) Uani 1 1 d . . . O12' O 0.9136(8) -0.3352(6) 0.3698(5) 0.088(5) Uani 1 1 d . . . O100 O 0.6368(6) -0.3659(5) 0.4253(3) 0.041(3) Uani 1 1 d . . . Nd2' Nd 0.13721(6) -0.58603(5) 0.32740(3) 0.0526(3) Uani 1 1 d . . . N5' N -0.0069(10) -0.6680(8) 0.3159(5) 0.059(4) Uani 1 1 d . . . O13' O 0.0830(7) -0.6725(5) 0.3045(4) 0.054(3) Uani 1 1 d . . . O14' O -0.0295(8) -0.6246(6) 0.3354(4) 0.067(4) Uani 1 1 d . . . O15' O -0.0601(7) -0.7020(5) 0.3102(4) 0.052(3) Uani 1 1 d . . . N6' N 0.3329(11) -0.6053(8) 0.2920(5) 0.067(5) Uani 1 1 d . . . O16' O 0.3050(7) -0.5601(5) 0.3090(4) 0.049(3) Uani 1 1 d . . . O17' O 0.2748(8) -0.6434(5) 0.2938(4) 0.061(4) Uani 1 1 d . . . O18' O 0.4109(9) -0.6087(7) 0.2765(5) 0.095(5) Uani 1 1 d . . . N7' N 0.0575(13) -0.5241(18) 0.3919(9) 0.25(2) Uani 1 1 d . . . O19' O 0.1447(13) -0.5314(11) 0.3836(10) 0.237(17) Uani 1 1 d . . . O20' O 0.0125(10) -0.5311(6) 0.3699(4) 0.083(4) Uani 1 1 d . . . O21' O 0.0281(13) -0.4876(8) 0.4191(6) 0.129(7) Uani 1 1 d . . . N8' N 0.1691(15) -0.6682(9) 0.3968(7) 0.083(6) Uani 1 1 d . . . O22' O 0.2333(13) -0.6410(9) 0.3768(5) 0.107(6) Uani 1 1 d . . . O23' O 0.0918(11) -0.6602(8) 0.3879(5) 0.112(7) Uani 1 1 d . . . O24' O 0.1822(15) -0.7010(9) 0.4325(5) 0.141(8) Uani 1 1 d . . . N9' N 0.1004(12) -0.5355(8) 0.2453(6) 0.067(5) Uani 1 1 d . . . O25' O 0.1747(8) -0.5595(6) 0.2516(4) 0.061(4) Uani 1 1 d . . . O26' O 0.0344(11) -0.5405(8) 0.2766(5) 0.108(6) Uani 1 1 d . . . O27' O 0.0831(9) -0.5101(8) 0.2144(6) 0.103(6) Uani 1 1 d . . . N101 N 0.1524(18) -0.4685(12) 0.3133(8) 0.092(8) Uiso 0.75 1 d P . . C101 C 0.099(2) -0.3607(16) 0.3004(11) 0.112(12) Uiso 0.75 1 d P . . C102 C 0.113(3) -0.423(2) 0.3042(15) 0.164(18) Uiso 0.75 1 d P . . N201 N 1.1524(14) 0.6138(9) 0.0915(6) 0.103(7) Uiso 1 1 d . . . C201 C 1.1114(17) 0.5738(11) 0.1034(7) 0.091(7) Uiso 1 1 d . . . C202 C 1.0612(18) 0.5170(12) 0.1168(8) 0.109(9) Uiso 1 1 d . . . N301 N 0.3234(14) -0.0664(9) 0.0471(6) 0.102(6) Uiso 1 1 d . . . C301 C 0.3846(15) -0.0907(9) 0.0598(6) 0.073(6) Uiso 1 1 d . . . C302 C 0.4594(16) -0.1252(10) 0.0781(7) 0.090(7) Uiso 1 1 d . . . N401 N -0.5166(16) -0.3047(10) 0.4706(7) 0.073(7) Uiso 0.75 1 d P . . C401 C -0.573(3) -0.3029(16) 0.4963(13) 0.114(12) Uiso 0.75 1 d P . . C402 C -0.651(3) -0.304(2) 0.5317(15) 0.167(18) Uiso 0.75 1 d P . . 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 Nd1 0.0150(4) 0.0358(5) 0.0317(5) -0.0088(4) -0.0043(4) -0.0039(4) P1 0.018(2) 0.035(3) 0.042(3) -0.008(2) -0.003(2) -0.0087(18) P2 0.0147(19) 0.035(2) 0.026(2) -0.0053(19) 0.0040(18) -0.0063(17) P3 0.0153(19) 0.042(3) 0.022(2) -0.006(2) -0.0002(17) -0.0087(18) O1 0.028(6) 0.038(7) 0.064(9) 0.001(6) -0.008(6) -0.004(5) O2 0.018(5) 0.030(6) 0.025(6) 0.002(5) -0.006(4) -0.001(4) O3 0.033(6) 0.034(6) 0.024(6) -0.007(5) -0.009(5) -0.002(5) O4 0.026(5) 0.046(7) 0.022(6) -0.011(5) -0.003(5) -0.024(5) O5 0.019(5) 0.037(6) 0.063(8) -0.026(6) -0.008(5) -0.003(5) O6 0.022(5) 0.066(7) 0.009(6) 0.004(5) 0.008(5) 0.016(5) O7 0.018(5) 0.031(6) 0.028(6) -0.012(5) -0.006(5) -0.008(4) O8 0.026(5) 0.041(6) 0.035(7) -0.004(5) -0.004(5) -0.026(5) O9 0.017(5) 0.036(6) 0.030(6) 0.000(5) 0.000(5) -0.009(4) N1 0.033(7) 0.032(7) 0.039(9) -0.013(7) -0.018(7) -0.008(6) N2 0.019(6) 0.030(7) 0.042(9) -0.005(6) 0.006(6) 0.008(6) N3 0.018(6) 0.041(8) 0.024(7) -0.006(6) -0.008(6) -0.002(6) C1 0.012(7) 0.040(9) 0.026(9) 0.000(7) -0.010(7) 0.016(7) N4 0.030(8) 0.052(10) 0.013(7) -0.006(7) 0.010(6) 0.001(8) O10 0.033(6) 0.044(7) 0.048(8) -0.013(6) -0.008(6) -0.010(6) O11 0.035(7) 0.036(6) 0.036(7) 0.002(5) -0.002(5) -0.005(5) O12 0.042(7) 0.053(8) 0.063(9) -0.010(7) -0.006(6) 0.017(6) Nd2 0.0179(5) 0.0468(6) 0.0584(7) -0.0015(5) -0.0047(5) 0.0001(4) N5 0.025(8) 0.065(11) 0.061(12) -0.033(9) -0.005(8) -0.002(7) O13 0.040(7) 0.057(8) 0.052(8) -0.007(7) -0.006(6) -0.004(6) O14 0.050(8) 0.119(12) 0.051(9) -0.040(9) -0.021(7) 0.019(8) O15 0.031(7) 0.056(9) 0.164(16) -0.027(9) -0.029(8) 0.014(6) N6 0.047(12) 0.078(13) 0.070(14) 0.003(11) 0.007(11) -0.007(10) O16 0.042(7) 0.081(9) 0.050(8) -0.028(7) -0.006(6) -0.017(7) O17 0.026(7) 0.082(10) 0.099(13) 0.002(9) 0.002(8) 0.009(7) O18 0.080(10) 0.111(13) 0.074(12) -0.016(10) 0.051(10) 0.004(9) N7 0.019(8) 0.045(10) 0.082(14) -0.018(9) -0.005(9) 0.011(7) O19 0.053(8) 0.124(12) 0.034(8) -0.033(8) 0.000(7) 0.014(8) O20 0.042(7) 0.064(9) 0.064(10) 0.003(8) 0.018(7) 0.034(7) O21 0.038(7) 0.078(9) 0.066(9) -0.025(8) -0.015(7) 0.010(6) N8 0.052(10) 0.048(11) 0.091(14) 0.013(10) -0.043(10) 0.002(9) O22 0.055(8) 0.052(8) 0.073(10) -0.008(7) -0.020(7) -0.003(6) O23 0.110(13) 0.084(12) 0.187(19) 0.047(12) -0.115(14) -0.037(10) O24 0.129(14) 0.049(10) 0.184(19) -0.023(10) -0.075(13) -0.040(10) N9 0.017(7) 0.032(10) 0.091(13) -0.002(9) 0.001(8) -0.002(7) O25 0.022(6) 0.043(7) 0.083(10) -0.019(7) 0.001(6) -0.012(6) O26 0.059(8) 0.045(8) 0.098(12) -0.008(7) 0.032(8) -0.016(7) O27 0.063(9) 0.032(8) 0.107(12) -0.004(7) 0.014(8) -0.009(7) Nd1' 0.0188(4) 0.0298(5) 0.0316(5) -0.0016(4) -0.0030(4) -0.0010(4) P1' 0.017(2) 0.053(3) 0.033(3) -0.003(2) 0.0001(19) -0.007(2) P2' 0.031(2) 0.028(2) 0.027(3) -0.004(2) 0.0012(19) 0.0074(19) P3' 0.027(2) 0.036(3) 0.025(2) 0.000(2) 0.0039(19) 0.0012(19) O1' 0.017(5) 0.049(7) 0.024(6) -0.005(5) 0.004(5) 0.005(5) O2' 0.022(5) 0.042(6) 0.015(6) -0.007(5) -0.004(4) 0.001(5) O3' 0.016(5) 0.046(6) 0.012(5) -0.004(5) 0.002(4) -0.005(4) O4' 0.027(6) 0.058(7) 0.038(7) -0.016(6) 0.007(5) -0.024(5) O5' 0.017(5) 0.058(7) 0.022(6) -0.004(5) -0.002(5) -0.003(5) O6' 0.055(7) 0.044(7) 0.018(6) -0.005(5) -0.009(5) 0.000(6) O7' 0.039(6) 0.038(7) 0.032(7) 0.012(5) 0.015(5) 0.000(5) O8' 0.042(6) 0.047(7) 0.024(6) -0.006(5) 0.012(5) 0.013(6) O9' 0.025(5) 0.030(6) 0.033(7) -0.003(5) 0.016(5) -0.001(5) N1' 0.018(6) 0.046(8) 0.021(7) 0.000(6) 0.010(6) -0.018(6) N2' 0.037(7) 0.036(8) 0.017(7) -0.002(6) 0.002(6) 0.003(6) N3' 0.032(7) 0.026(7) 0.027(8) -0.003(6) -0.017(6) 0.001(6) C1' 0.016(7) 0.031(9) 0.018(8) 0.004(7) 0.001(6) -0.012(6) N4' 0.030(9) 0.046(10) 0.049(10) 0.006(8) 0.012(7) -0.022(8) O10' 0.026(6) 0.047(8) 0.095(11) 0.003(7) -0.016(7) -0.009(6) O11' 0.039(7) 0.052(8) 0.109(12) 0.033(8) -0.036(8) -0.024(7) O12' 0.035(8) 0.081(10) 0.145(15) 0.015(9) -0.034(9) -0.022(7) O100 0.025(6) 0.055(7) 0.042(7) -0.002(6) -0.008(5) 0.003(5) Nd2' 0.0306(5) 0.0544(7) 0.0782(9) -0.0240(6) -0.0088(5) -0.0052(5) N5' 0.037(10) 0.087(14) 0.052(11) -0.014(10) 0.002(8) 0.000(10) O13' 0.037(7) 0.048(8) 0.079(10) -0.024(7) -0.001(7) -0.001(6) O14' 0.034(7) 0.077(10) 0.094(11) -0.041(9) 0.005(7) -0.003(7) O15' 0.029(6) 0.067(8) 0.068(9) -0.026(7) 0.001(6) -0.026(6) N6' 0.036(10) 0.065(13) 0.097(15) -0.025(11) 0.013(10) -0.001(9) O16' 0.027(6) 0.059(8) 0.061(9) -0.009(7) -0.007(6) -0.007(6) O17' 0.041(7) 0.055(8) 0.081(10) -0.004(7) 0.018(7) -0.016(7) O18' 0.034(8) 0.121(13) 0.135(15) -0.055(11) 0.016(9) -0.008(8) N7' 0.037(12) 0.56(6) 0.24(3) -0.33(4) -0.083(17) 0.12(2) O19' 0.077(14) 0.23(3) 0.48(5) -0.24(3) -0.09(2) 0.050(15) O20' 0.070(10) 0.105(12) 0.082(12) -0.042(9) -0.011(9) -0.005(9) O21' 0.125(15) 0.136(16) 0.129(18) -0.029(14) -0.021(13) -0.004(12) N8' 0.078(15) 0.068(14) 0.11(2) -0.038(13) -0.001(15) -0.002(12) O22' 0.119(15) 0.154(17) 0.054(11) -0.010(11) -0.023(11) -0.032(13) O23' 0.061(10) 0.157(16) 0.122(15) 0.024(12) -0.038(10) -0.076(11) O24' 0.21(2) 0.153(18) 0.067(13) 0.010(13) -0.063(14) -0.019(16) N9' 0.040(11) 0.090(13) 0.078(15) 0.001(11) -0.047(11) 0.000(10) O25' 0.026(7) 0.098(10) 0.059(9) -0.022(8) 0.002(6) 0.008(7) O26' 0.069(10) 0.149(16) 0.085(13) 0.011(11) 0.014(10) 0.023(10) O27' 0.036(8) 0.141(15) 0.128(16) 0.015(12) -0.035(10) -0.008(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O4 2.358(9) . ? Nd1 O6 2.386(9) . ? Nd1 O7 2.394(9) . ? Nd1 O5 2.405(8) . ? Nd1 O8 2.437(9) . ? Nd1 O9 2.452(9) . ? Nd1 O10 2.535(10) . ? Nd1 O11 2.552(10) . ? Nd1 N4 2.997(15) . ? P1 O5 1.486(10) . ? P1 C54 1.780(14) . ? P1 C48 1.790(15) . ? P1 C47 1.822(14) . ? P2 O7 1.519(9) . ? P2 C64 1.783(14) . ? P2 C70 1.785(15) . ? P2 C63 1.852(14) . ? P3 O9 1.510(9) . ? P3 C80 1.756(14) . ? P3 C86 1.803(14) . ? P3 C79 1.829(14) . ? O1 C3 1.390(18) . ? O1 C44 1.424(17) . ? O2 C17 1.389(16) . ? O2 C60 1.433(15) . ? O3 C31 1.352(16) . ? O3 C76 1.450(16) . ? O4 C46 1.240(16) . ? O6 C62 1.252(16) . ? O8 C78 1.236(14) . ? N1 C46 1.316(18) . ? N1 C45 1.510(17) . ? N2 C62 1.338(16) . ? N2 C61 1.459(17) . ? N3 C78 1.307(17) . ? N3 C77 1.442(17) . ? C1 C16 1.500(18) . ? C1 C2 1.567(18) . ? C1 C30 1.575(19) . ? C2 C3 1.368(19) . ? C2 C15 1.384(19) . ? C3 C4 1.43(2) . ? C4 C9 1.37(2) . ? C4 C5 1.55(2) . ? C5 C8 1.50(2) . ? C5 C6 1.54(2) . ? C5 C7 1.55(3) . ? C9 C10 1.37(2) . ? C10 C15 1.387(19) . ? C10 C11 1.60(2) . ? C11 C12A 1.47(7) . ? C11 C14 1.49(4) . ? C11 C12 1.53(3) . ? C11 C13A 1.54(5) . ? C11 C13 1.57(3) . ? C11 C14A 1.66(5) . ? C16 C17 1.377(19) . ? C16 C29 1.407(18) . ? C17 C18 1.386(18) . ? C18 C23 1.405(19) . ? C18 C19 1.560(19) . ? C19 C21 1.51(2) . ? C19 C20 1.570(19) . ? C19 C22 1.59(2) . ? C23 C24 1.386(19) . ? C24 C29 1.377(18) . ? C24 C25 1.53(2) . ? C25 C28 1.50(2) . ? C25 C26 1.54(2) . ? C25 C27 1.55(3) . ? C30 C43 1.36(2) . ? C30 C31 1.427(18) . ? C31 C32 1.44(2) . ? C32 C37 1.37(2) . ? C32 C33 1.49(2) . ? C33 C34 1.53(2) . ? C33 C35 1.54(2) . ? C33 C36 1.57(2) . ? C37 C38 1.418(19) . ? C38 C43 1.40(2) . ? C38 C39 1.52(2) . ? C39 C41 1.52(3) . ? C39 C40 1.53(3) . ? C39 C42 1.56(3) . ? C44 C45 1.53(2) . ? C46 C47 1.517(19) . ? C48 C53 1.40(2) . ? C48 C49 1.41(2) . ? C49 C50 1.36(2) . ? C50 C51 1.36(2) . ? C51 C52 1.38(3) . ? C52 C53 1.35(2) . ? C54 C55 1.36(2) . ? C54 C59 1.36(2) . ? C55 C56 1.38(2) . ? C56 C57 1.34(2) . ? C57 C58 1.32(2) . ? C58 C59 1.44(3) . ? C60 C61 1.506(18) . ? C62 C63 1.498(19) . ? C64 C69 1.35(2) . ? C64 C65 1.38(2) . ? C65 C66 1.37(2) . ? C66 C67 1.42(3) . ? C67 C68 1.34(2) . ? C68 C69 1.37(2) . ? C70 C75 1.39(2) . ? C70 C71 1.40(2) . ? C71 C72 1.40(2) . ? C72 C73 1.37(2) . ? C73 C74 1.33(2) . ? C74 C75 1.35(2) . ? C76 C77 1.50(2) . ? C78 C79 1.455(18) . ? C80 C85 1.387(19) . ? C80 C81 1.418(19) . ? C81 C82 1.40(2) . ? C82 C83 1.39(2) . ? C83 C84 1.35(2) . ? C84 C85 1.39(2) . ? C86 C87 1.352(18) . ? C86 C91 1.366(19) . ? C87 C88 1.39(2) . ? C88 C89 1.38(2) . ? C89 C90 1.31(2) . ? C90 C91 1.407(19) . ? N4 O12 1.233(15) . ? N4 O10 1.271(15) . ? N4 O11 1.291(14) . ? Nd2 O17 2.445(13) . ? Nd2 O16 2.446(11) . ? Nd2 O23 2.483(13) . ? Nd2 O14 2.489(11) . ? Nd2 O13 2.491(11) . ? Nd2 O25 2.502(10) . ? Nd2 O20 2.511(11) . ? Nd2 O19 2.517(12) . ? Nd2 O22 2.543(11) . ? Nd2 O26 2.569(12) . ? Nd2 N5 2.883(14) . ? Nd2 N7 2.891(17) . ? N5 O13 1.235(16) . ? N5 O14 1.240(17) . ? N5 O15 1.262(16) . ? N6 O18 1.22(2) . ? N6 O16 1.289(18) . ? N6 O17 1.29(2) . ? N7 O20 1.212(18) . ? N7 O19 1.254(16) . ? N7 O21 1.269(17) . ? N8 O24 1.194(17) . ? N8 O23 1.216(17) . ? N8 O22 1.278(16) . ? N9 O27 1.189(15) . ? N9 O26 1.256(16) . ? N9 O25 1.289(16) . ? Nd1' O9' 2.429(9) . ? Nd1' O6' 2.430(10) . ? Nd1' O5' 2.434(9) . ? Nd1' O7' 2.436(10) . ? Nd1' O4' 2.482(9) . ? Nd1' O8' 2.490(10) . ? Nd1' O100 2.518(10) . ? Nd1' O11' 2.615(10) . ? Nd1' O10' 2.621(10) . ? Nd1' N4' 2.996(13) . ? P1' O5' 1.472(9) . ? P1' C54' 1.779(16) . ? P1' C47' 1.780(14) . ? P1' C48' 1.823(16) . ? P2' O7' 1.490(10) . ? P2' C64' 1.762(14) . ? P2' C70' 1.822(16) . ? P2' C63' 1.830(14) . ? P3' O9' 1.484(10) . ? P3' C86' 1.759(15) . ? P3' C80' 1.778(16) . ? P3' C79' 1.783(15) . ? O1' C3' 1.360(16) . ? O1' C44' 1.431(16) . ? O2' C17' 1.433(17) . ? O2' C60' 1.457(16) . ? O3' C31' 1.376(16) . ? O3' C76' 1.456(15) . ? O4' C46' 1.219(16) . ? O6' C62' 1.261(17) . ? O8' C78' 1.214(15) . ? N1' C46' 1.289(17) . ? N1' C45' 1.482(18) . ? N2' C62' 1.324(18) . ? N2' C61' 1.431(17) . ? N3' C78' 1.303(17) . ? N3' C77' 1.465(17) . ? C1' C30' 1.544(18) . ? C1' C2' 1.555(17) . ? C1' C16' 1.579(18) . ? C2' C15' 1.368(18) . ? C2' C3' 1.433(19) . ? C3' C4' 1.427(18) . ? C4' C9' 1.354(19) . ? C4' C5' 1.54(2) . ? C5' C8' 1.51(2) . ? C5' C6' 1.56(2) . ? C5' C7' 1.59(2) . ? C9' C10' 1.40(2) . ? C10' C15' 1.387(18) . ? C10' C11' 1.51(2) . ? C11' C13B 1.36(5) . ? C11' C14' 1.43(3) . ? C11' C12' 1.49(3) . ? C11' C12B 1.56(6) . ? C11' C14B 1.63(4) . ? C11' C13' 1.66(3) . ? C16' C29' 1.361(18) . ? C16' C17' 1.381(18) . ? C17' C18' 1.376(19) . ? C18' C23' 1.353(19) . ? C18' C19' 1.57(2) . ? C19' C20' 1.52(2) . ? C19' C22' 1.53(2) . ? C19' C21' 1.53(2) . ? C23' C24' 1.423(18) . ? C24' C29' 1.379(18) . ? C24' C25' 1.51(2) . ? C25' C28B 1.42(5) . ? C25' C26B 1.42(5) . ? C25' C28' 1.50(3) . ? C25' C27B 1.51(9) . ? C25' C27' 1.52(3) . ? C25' C26' 1.59(3) . ? C30' C43' 1.365(18) . ? C30' C31' 1.401(17) . ? C31' C32' 1.408(18) . ? C32' C37' 1.37(2) . ? C32' C33' 1.562(19) . ? C33' C36' 1.50(2) . ? C33' C34' 1.51(2) . ? C33' C35' 1.58(2) . ? C37' C38' 1.376(19) . ? C38' C43' 1.349(17) . ? C38' C39' 1.53(2) . ? C39' C40' 1.38(3) . ? C39' C42' 1.42(2) . ? C39' C41' 1.51(2) . ? C44' C45' 1.507(19) . ? C46' C47' 1.526(19) . ? C48' C49' 1.24(2) . ? C48' C53' 1.37(2) . ? C49' C50' 1.52(3) . ? C50' C51' 1.39(3) . ? C51' C52' 1.28(3) . ? C52' C53' 1.48(3) . ? C54' C59' 1.39(2) . ? C54' C55' 1.41(2) . ? C55' C56' 1.36(2) . ? C56' C57' 1.34(2) . ? C57' C58' 1.44(3) . ? C58' C59' 1.33(2) . ? C60' C61' 1.48(2) . ? C62' C63' 1.468(19) . ? C64' C65' 1.33(2) . ? C64' C69' 1.38(2) . ? C65' C66' 1.40(3) . ? C66' C67' 1.30(3) . ? C67' C68' 1.30(2) . ? C68' C69' 1.42(2) . ? C70' C75' 1.37(2) . ? C70' C71' 1.37(2) . ? C71' C72' 1.44(3) . ? C72' C73' 1.31(3) . ? C73' C74' 1.31(3) . ? C74' C75' 1.46(3) . ? C76' C77' 1.564(19) . ? C78' C79' 1.548(19) . ? C80' C81' 1.36(2) . ? C80' C85' 1.37(2) . ? C81' C82' 1.43(3) . ? C82' C83' 1.42(3) . ? C83' C84' 1.40(3) . ? C84' C85' 1.37(3) . ? C86' C87' 1.40(2) . ? C86' C91' 1.41(2) . ? C87' C88' 1.39(2) . ? C88' C89' 1.37(2) . ? C89' C90' 1.40(3) . ? C90' C91' 1.40(2) . ? N4' O11' 1.208(15) . ? N4' O12' 1.228(15) . ? N4' O10' 1.275(15) . ? Nd2' O13' 2.467(11) . ? Nd2' O19' 2.49(2) . ? Nd2' O22' 2.499(16) . ? Nd2' O16' 2.508(10) . ? Nd2' O23' 2.519(16) . ? Nd2' O26' 2.524(15) . ? Nd2' O17' 2.555(12) . ? Nd2' O20' 2.556(14) . ? Nd2' O25' 2.577(13) . ? Nd2' O14' 2.590(11) . ? Nd2' N101 2.69(3) . ? Nd2' N8' 2.89(2) . ? N5' O15' 1.193(17) . ? N5' O14' 1.288(18) . ? N5' O13' 1.306(17) . ? N6' O18' 1.181(18) . ? N6' O17' 1.243(17) . ? N6' O16' 1.288(17) . ? N7' O20' 1.106(19) . ? N7' O19' 1.26(2) . ? N7' O21' 1.36(2) . ? N8' O23' 1.20(2) . ? N8' O22' 1.22(2) . ? N8' O24' 1.37(2) . ? N9' O27' 1.18(2) . ? N9' O25' 1.211(17) . ? N9' O26' 1.33(2) . ? N101 C102 1.18(5) . ? C101 C102 1.43(5) . ? N201 C201 1.12(3) . ? C201 C202 1.51(3) . ? N301 C301 1.12(2) . ? C301 C302 1.46(3) . ? N401 C401 1.12(4) . ? C401 C402 1.54(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Nd1 O6 86.2(3) . . ? O4 Nd1 O7 142.5(3) . . ? O6 Nd1 O7 75.9(3) . . ? O4 Nd1 O5 71.1(3) . . ? O6 Nd1 O5 81.2(3) . . ? O7 Nd1 O5 73.7(3) . . ? O4 Nd1 O8 71.8(3) . . ? O6 Nd1 O8 70.3(3) . . ? O7 Nd1 O8 129.0(3) . . ? O5 Nd1 O8 134.2(3) . . ? O4 Nd1 O9 141.1(3) . . ? O6 Nd1 O9 98.7(3) . . ? O7 Nd1 O9 75.0(3) . . ? O5 Nd1 O9 147.7(3) . . ? O8 Nd1 O9 73.7(3) . . ? O4 Nd1 O10 84.1(3) . . ? O6 Nd1 O10 152.0(3) . . ? O7 Nd1 O10 125.5(3) . . ? O5 Nd1 O10 119.9(3) . . ? O8 Nd1 O10 81.7(3) . . ? O9 Nd1 O10 73.6(3) . . ? O4 Nd1 O11 78.0(3) . . ? O6 Nd1 O11 151.3(3) . . ? O7 Nd1 O11 102.6(3) . . ? O5 Nd1 O11 71.2(3) . . ? O8 Nd1 O11 125.1(3) . . ? O9 Nd1 O11 108.6(3) . . ? O10 Nd1 O11 50.1(3) . . ? O4 Nd1 N4 79.5(3) . . ? O6 Nd1 N4 165.6(3) . . ? O7 Nd1 N4 116.8(3) . . ? O5 Nd1 N4 95.7(3) . . ? O8 Nd1 N4 103.2(3) . . ? O9 Nd1 N4 91.5(3) . . ? O10 Nd1 N4 24.8(3) . . ? O11 Nd1 N4 25.3(3) . . ? O5 P1 C54 110.4(6) . . ? O5 P1 C48 111.2(7) . . ? C54 P1 C48 108.8(6) . . ? O5 P1 C47 111.3(6) . . ? C54 P1 C47 108.4(7) . . ? C48 P1 C47 106.7(7) . . ? O7 P2 C64 111.4(6) . . ? O7 P2 C70 112.2(6) . . ? C64 P2 C70 107.4(7) . . ? O7 P2 C63 112.8(6) . . ? C64 P2 C63 106.6(7) . . ? C70 P2 C63 106.1(7) . . ? O9 P3 C80 111.1(6) . . ? O9 P3 C86 112.1(6) . . ? C80 P3 C86 106.7(6) . . ? O9 P3 C79 110.9(6) . . ? C80 P3 C79 108.5(7) . . ? C86 P3 C79 107.4(6) . . ? C3 O1 C44 116.2(12) . . ? C17 O2 C60 115.4(10) . . ? C31 O3 C76 111.8(10) . . ? C46 O4 Nd1 140.9(10) . . ? P1 O5 Nd1 139.6(6) . . ? C62 O6 Nd1 137.8(9) . . ? P2 O7 Nd1 135.5(5) . . ? C78 O8 Nd1 137.8(9) . . ? P3 O9 Nd1 132.9(5) . . ? C46 N1 C45 121.6(11) . . ? C62 N2 C61 122.5(11) . . ? C78 N3 C77 128.6(12) . . ? C16 C1 C2 115.1(11) . . ? C16 C1 C30 111.8(11) . . ? C2 C1 C30 108.0(11) . . ? C3 C2 C15 119.6(13) . . ? C3 C2 C1 122.0(13) . . ? C15 C2 C1 118.4(13) . . ? C2 C3 O1 119.9(13) . . ? C2 C3 C4 121.1(15) . . ? O1 C3 C4 118.5(14) . . ? C9 C4 C3 116.2(16) . . ? C9 C4 C5 121.7(15) . . ? C3 C4 C5 122.1(15) . . ? C8 C5 C6 109.9(16) . . ? C8 C5 C4 111.9(15) . . ? C6 C5 C4 109.4(15) . . ? C8 C5 C7 112.9(17) . . ? C6 C5 C7 104.7(16) . . ? C4 C5 C7 107.7(15) . . ? C10 C9 C4 123.9(16) . . ? C9 C10 C15 118.4(15) . . ? C9 C10 C11 120.8(14) . . ? C15 C10 C11 120.7(14) . . ? C12A C11 C14 148(3) . . ? C12A C11 C12 58(3) . . ? C14 C11 C12 111(2) . . ? C12A C11 C13A 111(4) . . ? C14 C11 C13A 50(3) . . ? C12 C11 C13A 133(3) . . ? C12A C11 C13 61(3) . . ? C14 C11 C13 106(2) . . ? C12 C11 C13 115(2) . . ? C13A C11 C13 56(3) . . ? C12A C11 C10 106(3) . . ? C14 C11 C10 106.6(19) . . ? C12 C11 C10 112.5(18) . . ? C13A C11 C10 114(3) . . ? C13 C11 C10 104.8(18) . . ? C12A C11 C14A 109(3) . . ? C14 C11 C14A 64(2) . . ? C12 C11 C14A 52(2) . . ? C13A C11 C14A 108(3) . . ? C13 C11 C14A 147(3) . . ? C10 C11 C14A 109(2) . . ? C2 C15 C10 120.6(14) . . ? C17 C16 C29 118.0(12) . . ? C17 C16 C1 121.0(13) . . ? C29 C16 C1 120.8(13) . . ? C16 C17 C18 121.2(13) . . ? C16 C17 O2 118.9(12) . . ? C18 C17 O2 119.5(13) . . ? C17 C18 C23 118.4(13) . . ? C17 C18 C19 125.4(12) . . ? C23 C18 C19 116.1(12) . . ? C21 C19 C18 114.9(13) . . ? C21 C19 C20 107.5(12) . . ? C18 C19 C20 111.6(11) . . ? C21 C19 C22 107.1(12) . . ? C18 C19 C22 110.5(12) . . ? C20 C19 C22 104.7(12) . . ? C24 C23 C18 122.2(13) . . ? C29 C24 C23 116.7(14) . . ? C29 C24 C25 120.7(14) . . ? C23 C24 C25 122.2(13) . . ? C28 C25 C24 109.8(14) . . ? C28 C25 C26 114.2(15) . . ? C24 C25 C26 109.7(15) . . ? C28 C25 C27 106.0(17) . . ? C24 C25 C27 111.5(14) . . ? C26 C25 C27 105.6(15) . . ? C24 C29 C16 123.0(14) . . ? C43 C30 C31 118.9(14) . . ? C43 C30 C1 120.6(13) . . ? C31 C30 C1 120.3(12) . . ? O3 C31 C30 118.8(12) . . ? O3 C31 C32 120.3(12) . . ? C30 C31 C32 120.3(13) . . ? C37 C32 C31 115.2(14) . . ? C37 C32 C33 123.1(14) . . ? C31 C32 C33 121.7(13) . . ? C32 C33 C34 110.8(14) . . ? C32 C33 C35 107.9(13) . . ? C34 C33 C35 107.2(13) . . ? C32 C33 C36 114.6(13) . . ? C34 C33 C36 106.1(13) . . ? C35 C33 C36 110.0(14) . . ? C32 C37 C38 126.7(15) . . ? C43 C38 C37 114.1(14) . . ? C43 C38 C39 119.4(14) . . ? C37 C38 C39 126.4(15) . . ? C38 C39 C41 109.8(16) . . ? C38 C39 C40 107.8(16) . . ? C41 C39 C40 108.9(17) . . ? C38 C39 C42 107.7(16) . . ? C41 C39 C42 111.9(17) . . ? C40 C39 C42 110.7(18) . . ? C30 C43 C38 124.1(15) . . ? O1 C44 C45 108.6(13) . . ? N1 C45 C44 110.5(11) . . ? O4 C46 N1 121.3(14) . . ? O4 C46 C47 122.2(14) . . ? N1 C46 C47 116.5(13) . . ? C46 C47 P1 109.8(10) . . ? C53 C48 C49 120.8(15) . . ? C53 C48 P1 121.2(12) . . ? C49 C48 P1 118.1(12) . . ? C50 C49 C48 117.5(17) . . ? C49 C50 C51 122(2) . . ? C50 C51 C52 121(2) . . ? C53 C52 C51 120(2) . . ? C52 C53 C48 119.4(18) . . ? C55 C54 C59 118.8(15) . . ? C55 C54 P1 118.5(11) . . ? C59 C54 P1 122.0(13) . . ? C54 C55 C56 121.8(15) . . ? C57 C56 C55 118.6(18) . . ? C58 C57 C56 122(2) . . ? C57 C58 C59 120(2) . . ? C54 C59 C58 119(2) . . ? O2 C60 C61 109.3(11) . . ? N2 C61 C60 111.0(11) . . ? O6 C62 N2 122.2(13) . . ? O6 C62 C63 122.5(13) . . ? N2 C62 C63 115.1(12) . . ? C62 C63 P2 110.3(10) . . ? C69 C64 C65 120.1(15) . . ? C69 C64 P2 123.9(12) . . ? C65 C64 P2 115.6(13) . . ? C66 C65 C64 118.7(19) . . ? C65 C66 C67 119(2) . . ? C68 C67 C66 120.6(19) . . ? C67 C68 C69 118.1(17) . . ? C64 C69 C68 122.7(15) . . ? C75 C70 C71 118.8(15) . . ? C75 C70 P2 125.5(12) . . ? C71 C70 P2 115.6(12) . . ? C70 C71 C72 119.5(17) . . ? C73 C72 C71 118(2) . . ? C74 C73 C72 122(2) . . ? C73 C74 C75 121(2) . . ? C74 C75 C70 120.1(18) . . ? O3 C76 C77 109.1(11) . . ? N3 C77 C76 115.1(12) . . ? O8 C78 N3 119.5(12) . . ? O8 C78 C79 121.8(13) . . ? N3 C78 C79 118.4(12) . . ? C78 C79 P3 108.5(9) . . ? C85 C80 C81 117.7(13) . . ? C85 C80 P3 120.1(11) . . ? C81 C80 P3 122.1(11) . . ? C82 C81 C80 119.1(15) . . ? C83 C82 C81 121.6(17) . . ? C84 C83 C82 118.5(17) . . ? C83 C84 C85 121.8(17) . . ? C84 C85 C80 121.3(15) . . ? C87 C86 C91 119.6(14) . . ? C87 C86 P3 122.1(11) . . ? C91 C86 P3 118.4(11) . . ? C86 C87 C88 120.4(14) . . ? C89 C88 C87 118.3(15) . . ? C90 C89 C88 122.7(17) . . ? C89 C90 C91 118.7(15) . . ? C86 C91 C90 120.4(14) . . ? O12 N4 O10 126.1(13) . . ? O12 N4 O11 119.4(13) . . ? O10 N4 O11 114.4(13) . . ? O12 N4 Nd1 176.9(10) . . ? O10 N4 Nd1 56.8(7) . . ? O11 N4 Nd1 57.7(7) . . ? N4 O10 Nd1 98.4(8) . . ? N4 O11 Nd1 97.0(8) . . ? O17 Nd2 O16 51.9(4) . . ? O17 Nd2 O23 77.8(6) . . ? O16 Nd2 O23 111.1(5) . . ? O17 Nd2 O14 119.5(5) . . ? O16 Nd2 O14 68.0(4) . . ? O23 Nd2 O14 123.0(5) . . ? O17 Nd2 O13 162.7(4) . . ? O16 Nd2 O13 117.9(4) . . ? O23 Nd2 O13 96.1(5) . . ? O14 Nd2 O13 50.6(4) . . ? O17 Nd2 O25 118.8(4) . . ? O16 Nd2 O25 102.7(4) . . ? O23 Nd2 O25 145.0(5) . . ? O14 Nd2 O25 77.7(4) . . ? O13 Nd2 O25 75.3(4) . . ? O17 Nd2 O20 72.9(5) . . ? O16 Nd2 O20 121.8(4) . . ? O23 Nd2 O20 67.5(5) . . ? O14 Nd2 O20 164.0(4) . . ? O13 Nd2 O20 120.1(4) . . ? O25 Nd2 O20 87.3(4) . . ? O17 Nd2 O19 121.0(5) . . ? O16 Nd2 O19 170.8(4) . . ? O23 Nd2 O19 69.9(5) . . ? O14 Nd2 O19 119.6(4) . . ? O13 Nd2 O19 70.6(4) . . ? O25 Nd2 O19 75.3(4) . . ? O20 Nd2 O19 49.5(4) . . ? O17 Nd2 O22 87.2(4) . . ? O16 Nd2 O22 81.3(4) . . ? O23 Nd2 O22 48.8(4) . . ? O14 Nd2 O22 76.5(4) . . ? O13 Nd2 O22 76.8(4) . . ? O25 Nd2 O22 150.2(4) . . ? O20 Nd2 O22 116.1(4) . . ? O19 Nd2 O22 105.0(4) . . ? O17 Nd2 O26 68.5(4) . . ? O16 Nd2 O26 71.9(4) . . ? O23 Nd2 O26 133.3(5) . . ? O14 Nd2 O26 101.8(4) . . ? O13 Nd2 O26 124.6(4) . . ? O25 Nd2 O26 50.3(4) . . ? O20 Nd2 O26 72.2(4) . . ? O19 Nd2 O26 100.6(5) . . ? O22 Nd2 O26 151.4(4) . . ? O17 Nd2 N5 143.6(5) . . ? O16 Nd2 N5 93.2(4) . . ? O23 Nd2 N5 111.8(5) . . ? O14 Nd2 N5 25.4(4) . . ? O13 Nd2 N5 25.2(4) . . ? O25 Nd2 N5 74.1(4) . . ? O20 Nd2 N5 143.5(5) . . ? O19 Nd2 N5 94.8(4) . . ? O22 Nd2 N5 76.2(4) . . ? O26 Nd2 N5 114.5(4) . . ? O17 Nd2 N7 95.4(5) . . ? O16 Nd2 N7 146.2(4) . . ? O23 Nd2 N7 61.9(5) . . ? O14 Nd2 N7 145.1(4) . . ? O13 Nd2 N7 95.9(4) . . ? O25 Nd2 N7 85.0(4) . . ? O20 Nd2 N7 24.7(3) . . ? O19 Nd2 N7 25.6(4) . . ? O22 Nd2 N7 108.3(4) . . ? O26 Nd2 N7 89.5(4) . . ? N5 Nd2 N7 120.4(5) . . ? O13 N5 O14 118.4(13) . . ? O13 N5 O15 121.7(16) . . ? O14 N5 O15 119.8(15) . . ? O13 N5 Nd2 59.3(8) . . ? O14 N5 Nd2 59.3(7) . . ? O15 N5 Nd2 176.5(10) . . ? N5 O13 Nd2 95.5(10) . . ? N5 O14 Nd2 95.4(9) . . ? O18 N6 O16 122.3(19) . . ? O18 N6 O17 125.8(18) . . ? O16 N6 O17 111.8(17) . . ? O18 N6 Nd2 174.1(14) . . ? O16 N6 Nd2 56.4(9) . . ? O17 N6 Nd2 56.4(10) . . ? N6 O16 Nd2 97.6(11) . . ? N6 O17 Nd2 97.5(10) . . ? O20 N7 O19 117.3(15) . . ? O20 N7 O21 123.5(14) . . ? O19 N7 O21 119.1(16) . . ? O20 N7 Nd2 59.9(9) . . ? O19 N7 Nd2 60.3(9) . . ? O21 N7 Nd2 166.8(11) . . ? N7 O19 Nd2 94.1(11) . . ? N7 O20 Nd2 95.5(9) . . ? O24 N8 O23 125.7(16) . . ? O24 N8 O22 121.3(16) . . ? O23 N8 O22 112.8(16) . . ? O24 N8 Nd2 179.1(15) . . ? O23 N8 Nd2 54.9(9) . . ? O22 N8 Nd2 58.1(8) . . ? N8 O22 Nd2 96.6(10) . . ? N8 O23 Nd2 101.5(11) . . ? O27 N9 O26 122.3(15) . . ? O27 N9 O25 121.9(14) . . ? O26 N9 O25 115.8(13) . . ? O27 N9 Nd2 177.9(14) . . ? O26 N9 Nd2 59.3(8) . . ? O25 N9 Nd2 56.5(7) . . ? N9 O25 Nd2 98.1(9) . . ? N9 O26 Nd2 95.8(10) . . ? O9' Nd1' O6' 137.4(3) . . ? O9' Nd1' O5' 80.8(3) . . ? O6' Nd1' O5' 117.2(3) . . ? O9' Nd1' O7' 148.5(3) . . ? O6' Nd1' O7' 71.5(3) . . ? O5' Nd1' O7' 72.2(3) . . ? O9' Nd1' O4' 81.7(3) . . ? O6' Nd1' O4' 70.9(3) . . ? O5' Nd1' O4' 69.8(3) . . ? O7' Nd1' O4' 103.3(3) . . ? O9' Nd1' O8' 71.3(3) . . ? O6' Nd1' O8' 69.7(3) . . ? O5' Nd1' O8' 135.5(3) . . ? O7' Nd1' O8' 140.1(3) . . ? O4' Nd1' O8' 72.3(3) . . ? O9' Nd1' O100 80.2(3) . . ? O6' Nd1' O100 141.0(3) . . ? O5' Nd1' O100 70.5(3) . . ? O7' Nd1' O100 75.7(3) . . ? O4' Nd1' O100 138.4(3) . . ? O8' Nd1' O100 134.1(3) . . ? O9' Nd1' O11' 121.7(3) . . ? O6' Nd1' O11' 73.1(4) . . ? O5' Nd1' O11' 136.5(4) . . ? O7' Nd1' O11' 72.2(4) . . ? O4' Nd1' O11' 143.2(4) . . ? O8' Nd1' O11' 88.0(4) . . ? O100 Nd1' O11' 77.2(4) . . ? O9' Nd1' O10' 73.0(3) . . ? O6' Nd1' O10' 107.9(4) . . ? O5' Nd1' O10' 133.6(4) . . ? O7' Nd1' O10' 114.9(4) . . ? O4' Nd1' O10' 139.5(4) . . ? O8' Nd1' O10' 69.8(4) . . ? O100 Nd1' O10' 67.9(4) . . ? O11' Nd1' O10' 48.7(4) . . ? O9' Nd1' N4' 98.1(4) . . ? O6' Nd1' N4' 89.0(4) . . ? O5' Nd1' N4' 142.5(3) . . ? O7' Nd1' N4' 93.7(4) . . ? O4' Nd1' N4' 147.5(4) . . ? O8' Nd1' N4' 76.8(4) . . ? O100 Nd1' N4' 72.5(3) . . ? O11' Nd1' N4' 23.6(3) . . ? O10' Nd1' N4' 25.1(3) . . ? O5' P1' C54' 111.5(6) . . ? O5' P1' C47' 111.5(6) . . ? C54' P1' C47' 109.0(7) . . ? O5' P1' C48' 110.4(7) . . ? C54' P1' C48' 110.6(7) . . ? C47' P1' C48' 103.5(7) . . ? O7' P2' C64' 110.0(6) . . ? O7' P2' C70' 112.4(7) . . ? C64' P2' C70' 109.9(7) . . ? O7' P2' C63' 110.8(6) . . ? C64' P2' C63' 106.4(7) . . ? C70' P2' C63' 107.3(7) . . ? O9' P3' C86' 110.9(6) . . ? O9' P3' C80' 112.2(7) . . ? C86' P3' C80' 106.9(7) . . ? O9' P3' C79' 114.5(6) . . ? C86' P3' C79' 109.3(8) . . ? C80' P3' C79' 102.5(7) . . ? C3' O1' C44' 117.1(10) . . ? C17' O2' C60' 112.8(10) . . ? C31' O3' C76' 114.5(10) . . ? C46' O4' Nd1' 142.3(10) . . ? P1' O5' Nd1' 140.7(6) . . ? C62' O6' Nd1' 141.1(10) . . ? P2' O7' Nd1' 138.2(6) . . ? C78' O8' Nd1' 142.0(10) . . ? P3' O9' Nd1' 136.5(5) . . ? C46' N1' C45' 124.2(12) . . ? C62' N2' C61' 122.3(13) . . ? C78' N3' C77' 122.6(12) . . ? C30' C1' C2' 112.1(10) . . ? C30' C1' C16' 110.1(11) . . ? C2' C1' C16' 108.8(11) . . ? C15' C2' C3' 119.7(12) . . ? C15' C2' C1' 120.8(12) . . ? C3' C2' C1' 119.4(12) . . ? O1' C3' C4' 121.5(13) . . ? O1' C3' C2' 119.4(11) . . ? C4' C3' C2' 118.9(13) . . ? C9' C4' C3' 117.9(14) . . ? C9' C4' C5' 121.1(13) . . ? C3' C4' C5' 120.7(13) . . ? C8' C5' C4' 112.4(13) . . ? C8' C5' C6' 111.6(14) . . ? C4' C5' C6' 108.7(13) . . ? C8' C5' C7' 106.5(13) . . ? C4' C5' C7' 110.2(13) . . ? C6' C5' C7' 107.3(12) . . ? C4' C9' C10' 124.3(14) . . ? C15' C10' C9' 117.1(13) . . ? C15' C10' C11' 120.7(13) . . ? C9' C10' C11' 122.0(13) . . ? C13B C11' C14' 120(3) . . ? C13B C11' C12' 56(2) . . ? C14' C11' C12' 112.7(19) . . ? C13B C11' C10' 121(3) . . ? C14' C11' C10' 118.3(18) . . ? C12' C11' C10' 107.3(15) . . ? C13B C11' C12B 107(4) . . ? C14' C11' C12B 65(3) . . ? C12' C11' C12B 57(3) . . ? C10' C11' C12B 104(3) . . ? C13B C11' C14B 108(3) . . ? C14' C11' C14B 38.1(18) . . ? C12' C11' C14B 140(2) . . ? C10' C11' C14B 111(2) . . ? C12B C11' C14B 103(3) . . ? C13B C11' C13' 47(2) . . ? C14' C11' C13' 109.5(18) . . ? C12' C11' C13' 103.2(18) . . ? C10' C11' C13' 104.5(14) . . ? C12B C11' C13' 149(3) . . ? C14B C11' C13' 76(2) . . ? C2' C15' C10' 122.0(14) . . ? C29' C16' C17' 118.3(13) . . ? C29' C16' C1' 119.4(12) . . ? C17' C16' C1' 122.3(13) . . ? C18' C17' C16' 122.4(14) . . ? C18' C17' O2' 122.0(12) . . ? C16' C17' O2' 115.2(12) . . ? C23' C18' C17' 116.5(13) . . ? C23' C18' C19' 122.8(13) . . ? C17' C18' C19' 120.7(13) . . ? C20' C19' C22' 108.0(13) . . ? C20' C19' C21' 112.6(14) . . ? C22' C19' C21' 103.1(13) . . ? C20' C19' C18' 105.6(12) . . ? C22' C19' C18' 110.4(14) . . ? C21' C19' C18' 116.9(12) . . ? C18' C23' C24' 123.3(14) . . ? C29' C24' C23' 116.0(13) . . ? C29' C24' C25' 123.1(13) . . ? C23' C24' C25' 120.7(13) . . ? C28B C25' C26B 119(3) . . ? C28B C25' C28' 52(2) . . ? C26B C25' C28' 133(3) . . ? C28B C25' C27B 98(4) . . ? C26B C25' C27B 112(4) . . ? C28' C25' C27B 46(3) . . ? C28B C25' C24' 108(2) . . ? C26B C25' C24' 112(2) . . ? C28' C25' C24' 114.3(15) . . ? C27B C25' C24' 106(4) . . ? C28B C25' C27' 138(3) . . ? C26B C25' C27' 43(2) . . ? C28' C25' C27' 108.1(17) . . ? C27B C25' C27' 71(4) . . ? C24' C25' C27' 113.4(14) . . ? C28B C25' C26' 58(2) . . ? C26B C25' C26' 66(2) . . ? C28' C25' C26' 104.1(17) . . ? C27B C25' C26' 140(4) . . ? C24' C25' C26' 110.7(16) . . ? C27' C25' C26' 105.3(18) . . ? C16' C29' C24' 122.3(13) . . ? C43' C30' C31' 118.2(12) . . ? C43' C30' C1' 122.5(12) . . ? C31' C30' C1' 119.2(11) . . ? O3' C31' C30' 118.7(11) . . ? O3' C31' C32' 121.6(12) . . ? C30' C31' C32' 119.0(12) . . ? C37' C32' C31' 118.1(13) . . ? C37' C32' C33' 121.8(13) . . ? C31' C32' C33' 120.0(12) . . ? C36' C33' C34' 108.4(13) . . ? C36' C33' C32' 110.0(12) . . ? C34' C33' C32' 114.5(13) . . ? C36' C33' C35' 109.1(13) . . ? C34' C33' C35' 105.8(13) . . ? C32' C33' C35' 108.8(12) . . ? C32' C37' C38' 123.1(15) . . ? C43' C38' C37' 116.5(13) . . ? C43' C38' C39' 121.4(12) . . ? C37' C38' C39' 122.0(13) . . ? C40' C39' C42' 117.8(18) . . ? C40' C39' C41' 99.5(18) . . ? C42' C39' C41' 107.1(16) . . ? C40' C39' C38' 108.9(16) . . ? C42' C39' C38' 111.4(16) . . ? C41' C39' C38' 111.5(14) . . ? C38' C43' C30' 124.4(13) . . ? O1' C44' C45' 109.3(11) . . ? N1' C45' C44' 111.5(12) . . ? O4' C46' N1' 123.9(14) . . ? O4' C46' C47' 118.6(13) . . ? N1' C46' C47' 117.5(13) . . ? C46' C47' P1' 114.7(10) . . ? C49' C48' C53' 124.6(19) . . ? C49' C48' P1' 116.7(15) . . ? C53' C48' P1' 118.3(14) . . ? C48' C49' C50' 121(2) . . ? C51' C50' C49' 114(2) . . ? C52' C51' C50' 123(3) . . ? C51' C52' C53' 121(3) . . ? C48' C53' C52' 115(2) . . ? C59' C54' C55' 119.6(15) . . ? C59' C54' P1' 123.0(13) . . ? C55' C54' P1' 117.4(12) . . ? C56' C55' C54' 119.2(15) . . ? C57' C56' C55' 120.4(18) . . ? C56' C57' C58' 121(2) . . ? C59' C58' C57' 118(2) . . ? C58' C59' C54' 121.1(18) . . ? O2' C60' C61' 108.3(12) . . ? N2' C61' C60' 112.4(13) . . ? O6' C62' N2' 120.8(13) . . ? O6' C62' C63' 120.7(14) . . ? N2' C62' C63' 118.5(13) . . ? C62' C63' P2' 107.2(10) . . ? C65' C64' C69' 115.1(16) . . ? C65' C64' P2' 121.4(14) . . ? C69' C64' P2' 123.4(12) . . ? C64' C65' C66' 122(2) . . ? C67' C66' C65' 120(2) . . ? C66' C67' C68' 122(2) . . ? C67' C68' C69' 119(2) . . ? C64' C69' C68' 121.7(18) . . ? C75' C70' C71' 124.4(17) . . ? C75' C70' P2' 122.6(14) . . ? C71' C70' P2' 113.0(13) . . ? C70' C71' C72' 116(2) . . ? C73' C72' C71' 118(3) . . ? C74' C73' C72' 128(3) . . ? C73' C74' C75' 116(2) . . ? C70' C75' C74' 117.1(19) . . ? O3' C76' C77' 105.9(11) . . ? N3' C77' C76' 109.1(11) . . ? O8' C78' N3' 119.7(13) . . ? O8' C78' C79' 121.3(14) . . ? N3' C78' C79' 118.7(13) . . ? C78' C79' P3' 113.7(10) . . ? C81' C80' C85' 118.9(16) . . ? C81' C80' P3' 117.0(13) . . ? C85' C80' P3' 123.9(14) . . ? C80' C81' C82' 120.9(18) . . ? C83' C82' C81' 118(2) . . ? C84' C83' C82' 119(2) . . ? C85' C84' C83' 119(2) . . ? C80' C85' C84' 124(2) . . ? C87' C86' C91' 120.5(15) . . ? C87' C86' P3' 122.3(12) . . ? C91' C86' P3' 117.1(12) . . ? C88' C87' C86' 119.7(16) . . ? C89' C88' C87' 119.0(19) . . ? C88' C89' C90' 123(2) . . ? C91' C90' C89' 117.8(19) . . ? C90' C91' C86' 119.7(16) . . ? O11' N4' O12' 121.7(14) . . ? O11' N4' O10' 120.6(13) . . ? O12' N4' O10' 117.6(15) . . ? O11' N4' Nd1' 60.2(7) . . ? O12' N4' Nd1' 177.0(12) . . ? O10' N4' Nd1' 60.8(7) . . ? N4' O10' Nd1' 94.1(9) . . ? N4' O11' Nd1' 96.2(9) . . ? O13' Nd2' O19' 147.8(8) . . ? O13' Nd2' O22' 97.2(5) . . ? O19' Nd2' O22' 67.8(7) . . ? O13' Nd2' O16' 119.3(4) . . ? O19' Nd2' O16' 83.4(6) . . ? O22' Nd2' O16' 69.8(5) . . ? O13' Nd2' O23' 72.8(5) . . ? O19' Nd2' O23' 76.1(9) . . ? O22' Nd2' O23' 49.3(5) . . ? O16' Nd2' O23' 119.2(4) . . ? O13' Nd2' O26' 77.0(5) . . ? O19' Nd2' O26' 116.8(7) . . ? O22' Nd2' O26' 174.2(6) . . ? O16' Nd2' O26' 113.5(5) . . ? O23' Nd2' O26' 127.0(5) . . ? O13' Nd2' O17' 69.4(4) . . ? O19' Nd2' O17' 124.7(5) . . ? O22' Nd2' O17' 68.7(5) . . ? O16' Nd2' O17' 50.3(4) . . ? O23' Nd2' O17' 99.4(5) . . ? O26' Nd2' O17' 109.4(5) . . ? O13' Nd2' O20' 115.0(4) . . ? O19' Nd2' O20' 47.6(5) . . ? O22' Nd2' O20' 103.2(5) . . ? O16' Nd2' O20' 125.7(4) . . ? O23' Nd2' O20' 75.9(6) . . ? O26' Nd2' O20' 78.9(5) . . ? O17' Nd2' O20' 171.5(4) . . ? O13' Nd2' O25' 78.2(4) . . ? O19' Nd2' O25' 133.5(8) . . ? O22' Nd2' O25' 130.5(5) . . ? O16' Nd2' O25' 70.3(4) . . ? O23' Nd2' O25' 150.3(5) . . ? O26' Nd2' O25' 49.5(4) . . ? O17' Nd2' O25' 63.6(4) . . ? O20' Nd2' O25' 123.6(4) . . ? O13' Nd2' O14' 50.3(4) . . ? O19' Nd2' O14' 107.6(6) . . ? O22' Nd2' O14' 112.6(6) . . ? O16' Nd2' O14' 169.0(4) . . ? O23' Nd2' O14' 64.0(4) . . ? O26' Nd2' O14' 63.1(5) . . ? O17' Nd2' O14' 119.7(4) . . ? O20' Nd2' O14' 64.9(4) . . ? O25' Nd2' O14' 101.8(4) . . ? O13' Nd2' N101 145.9(6) . . ? O19' Nd2' N101 60.5(9) . . ? O22' Nd2' N101 116.0(7) . . ? O16' Nd2' N101 69.2(6) . . ? O23' Nd2' N101 135.0(7) . . ? O26' Nd2' N101 69.9(7) . . ? O17' Nd2' N101 114.1(6) . . ? O20' Nd2' N101 66.8(7) . . ? O25' Nd2' N101 74.4(6) . . ? O14' Nd2' N101 116.8(6) . . ? O13' Nd2' N8' 84.3(5) . . ? O19' Nd2' N8' 70.4(8) . . ? O22' Nd2' N8' 24.9(5) . . ? O16' Nd2' N8' 94.7(5) . . ? O23' Nd2' N8' 24.5(4) . . ? O26' Nd2' N8' 151.2(6) . . ? O17' Nd2' N8' 83.6(5) . . ? O20' Nd2' N8' 89.6(5) . . ? O25' Nd2' N8' 146.5(5) . . ? O14' Nd2' N8' 88.1(5) . . ? N101 Nd2' N8' 129.4(7) . . ? O15' N5' O14' 124.8(15) . . ? O15' N5' O13' 123.0(16) . . ? O14' N5' O13' 112.1(15) . . ? N5' O13' Nd2' 101.4(10) . . ? N5' O14' Nd2' 96.0(9) . . ? O18' N6' O17' 124.3(18) . . ? O18' N6' O16' 119.1(17) . . ? O17' N6' O16' 116.6(15) . . ? O18' N6' Nd2' 175.0(15) . . ? O17' N6' Nd2' 59.4(8) . . ? O16' N6' Nd2' 57.5(8) . . ? N6' O16' Nd2' 96.9(9) . . ? N6' O17' Nd2' 95.9(10) . . ? O20' N7' O19' 119(2) . . ? O20' N7' O21' 121(2) . . ? O19' N7' O21' 116(2) . . ? O20' N7' Nd2' 61.5(12) . . ? O19' N7' Nd2' 59.1(14) . . ? O21' N7' Nd2' 171(3) . . ? N7' O19' Nd2' 95.1(15) . . ? N7' O20' Nd2' 96.1(14) . . ? O23' N8' O22' 120(2) . . ? O23' N8' O24' 119(2) . . ? O22' N8' O24' 120(2) . . ? O23' N8' Nd2' 60.4(13) . . ? O22' N8' Nd2' 59.5(13) . . ? O24' N8' Nd2' 172.3(14) . . ? N8' O22' Nd2' 95.6(15) . . ? N8' O23' Nd2' 95.1(14) . . ? O27' N9' O25' 126(2) . . ? O27' N9' O26' 120.0(17) . . ? O25' N9' O26' 114.2(17) . . ? O27' N9' Nd2' 173.0(16) . . ? O25' N9' Nd2' 58.2(10) . . ? O26' N9' Nd2' 56.6(10) . . ? N9' O25' Nd2' 98.2(12) . . ? N9' O26' Nd2' 97.3(11) . . ? C102 N101 Nd2' 145(3) . . ? N101 C102 C101 155(5) . . ? N201 C201 C202 175(3) . . ? N301 C301 C302 176(3) . . ? N401 C401 C402 177(4) . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 1.513 _refine_diff_density_min -1.560 _refine_diff_density_rms 0.146 #===END data_9_thorium_nitrate_complex _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; tris(3,5-di-tert-butyl-2-(2-(carbamoylmethylphosphineoxide)ethoxy)phen yl)methane thorium nitrate complex ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C95.50 H122 N7 O24 P3 Th' _chemical_formula_weight 2076.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Th' 'Th' -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3375(8) _cell_length_b 17.7417(11) _cell_length_c 24.8533(16) _cell_angle_alpha 102.4780(10) _cell_angle_beta 102.1550(10) _cell_angle_gamma 95.5900(10) _cell_volume 5134.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2142 _exptl_absorpt_coefficient_mu 1.571 _exptl_absorpt_correction_type 'SADABS' _exptl_absorpt_correction_T_min 0.5515 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25051 _diffrn_reflns_av_R_equivalents 0.0733 _diffrn_reflns_av_sigmaI/netI 0.1864 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 24.00 _reflns_number_total 16050 _reflns_number_gt 9115 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Two and a half methanol molecules and one half ether molecule were "SQUEEZED" out of the asymmetric unit. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0632P)^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 16050 _refine_ls_number_parameters 1030 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1362 _refine_ls_R_factor_gt 0.0706 _refine_ls_wR_factor_ref 0.1624 _refine_ls_wR_factor_gt 0.1375 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.954 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Th1 Th -0.68282(4) -0.60441(2) 0.182202(17) 0.02814(13) Uani 1 1 d . . . P1 P -0.9752(2) -0.59771(15) 0.19598(12) 0.0347(7) Uani 1 1 d . . . P2 P -0.5960(2) -0.70396(16) 0.05517(11) 0.0355(7) Uani 1 1 d . C . P3 P -0.5873(3) -0.47160(17) 0.32390(13) 0.0504(9) Uani 1 1 d . . . N1 N -0.9599(7) -0.8156(4) 0.1499(3) 0.035(2) Uani 1 1 d . . . H1B H -1.0313 -0.8300 0.1476 0.043 Uiso 1 1 calc R . . N2 N -0.4880(7) -0.8196(5) 0.1682(3) 0.032(2) Uani 1 1 d . . . H2A H -0.4452 -0.8456 0.1491 0.038 Uiso 1 1 calc R . . N3 N -0.6778(7) -0.6633(4) 0.3552(3) 0.037(2) Uani 1 1 d . . . H3A H -0.6554 -0.6435 0.3920 0.044 Uiso 1 1 calc R . . O1 O -0.9233(5) -0.9009(3) 0.2379(2) 0.0296(16) Uani 1 1 d . . . O2 O -0.6447(6) -0.9538(4) 0.1788(3) 0.0315(16) Uani 1 1 d . . . O3 O -0.6208(6) -0.8188(4) 0.3379(3) 0.0341(17) Uani 1 1 d . . . O4 O -0.8236(6) -0.7192(3) 0.1563(3) 0.0333(17) Uani 1 1 d . . . O5 O -0.8497(6) -0.5706(3) 0.2134(3) 0.0361(17) Uani 1 1 d . . . O6 O -0.6035(6) -0.7287(4) 0.1703(3) 0.0362(18) Uani 1 1 d . . . O7 O -0.6472(6) -0.6426(4) 0.0898(3) 0.0362(18) Uani 1 1 d . . . O8 O -0.6672(6) -0.6499(4) 0.2681(3) 0.0343(17) Uani 1 1 d . . . O9 O -0.6242(6) -0.4911(4) 0.2610(3) 0.045(2) Uani 1 1 d . . . C1 C -0.7307(7) -0.9729(5) 0.2739(4) 0.025(2) Uani 1 1 d . . . H1A H -0.7312 -0.9252 0.2585 0.030 Uiso 1 1 calc R . . C2 C -0.8385(8) -0.9849(5) 0.2938(4) 0.023(2) Uani 1 1 d . A . C3 C -0.9303(9) -0.9514(5) 0.2740(4) 0.027(2) Uani 1 1 d . . . C4 C -1.0312(8) -0.9586(5) 0.2941(4) 0.027(2) Uani 1 1 d . . . C5 C -1.1320(9) -0.9172(7) 0.2780(4) 0.043(3) Uani 1 1 d . . . C6 C -1.0975(11) -0.8285(7) 0.2899(7) 0.093(5) Uani 1 1 d . . . H6A H -1.0782 -0.8059 0.3309 0.140 Uiso 1 1 calc R . . H6B H -1.1600 -0.8054 0.2718 0.140 Uiso 1 1 calc R . . H6C H -1.0323 -0.8178 0.2745 0.140 Uiso 1 1 calc R . . C7 C -1.1887(11) -0.9477(8) 0.2147(5) 0.074(4) Uani 1 1 d . . . H7A H -1.1406 -0.9288 0.1922 0.111 Uiso 1 1 calc R . . H7B H -1.2611 -0.9288 0.2066 0.111 Uiso 1 1 calc R . . H7C H -1.2007 -1.0049 0.2049 0.111 Uiso 1 1 calc R . . C8 C -1.2215(10) -0.9295(8) 0.3107(5) 0.069(4) Uani 1 1 d . . . H8A H -1.1870 -0.9147 0.3516 0.104 Uiso 1 1 calc R . . H8B H -1.2551 -0.9846 0.2996 0.104 Uiso 1 1 calc R . . H8C H -1.2797 -0.8972 0.3020 0.104 Uiso 1 1 calc R . . C9 C -1.0324(9) -1.0071(6) 0.3321(4) 0.038(3) Uani 1 1 d . . . H9A H -1.0989 -1.0156 0.3449 0.046 Uiso 1 1 calc R . . C10 C -0.9438(9) -1.0429(6) 0.3519(4) 0.037(3) Uani 1 1 d . A . C11 C -0.9498(10) -1.0951(6) 0.3931(4) 0.044(3) Uani 1 1 d . . . C12 C -1.0578(18) -1.0927(12) 0.4152(9) 0.038(5) Uiso 0.50 1 d P A 1 H12A H -1.0655 -1.0383 0.4306 0.057 Uiso 0.50 1 calc PR A 1 H12B H -1.0535 -1.1212 0.4451 0.057 Uiso 0.50 1 calc PR A 1 H12C H -1.1229 -1.1170 0.3839 0.057 Uiso 0.50 1 calc PR A 1 C13 C -0.917(2) -1.1681(13) 0.3755(10) 0.055(7) Uiso 0.50 1 d P A 1 H13A H -0.9064 -1.1940 0.4068 0.083 Uiso 0.50 1 calc PR A 1 H13B H -0.8456 -1.1608 0.3641 0.083 Uiso 0.50 1 calc PR A 1 H13C H -0.9743 -1.2004 0.3432 0.083 Uiso 0.50 1 calc PR A 1 C14 C -0.855(2) -1.0508(14) 0.4522(10) 0.067(8) Uiso 0.50 1 d P A 1 H14A H -0.8566 -1.0807 0.4809 0.101 Uiso 0.50 1 calc PR A 1 H14B H -0.8708 -0.9981 0.4664 0.101 Uiso 0.50 1 calc PR A 1 H14C H -0.7799 -1.0472 0.4444 0.101 Uiso 0.50 1 calc PR A 1 C12' C -1.044(2) -1.1702(15) 0.3595(11) 0.072(8) Uiso 0.50 1 d P A 2 H12D H -1.0236 -1.1963 0.3248 0.108 Uiso 0.50 1 calc PR A 2 H12E H -1.1169 -1.1531 0.3497 0.108 Uiso 0.50 1 calc PR A 2 H12F H -1.0473 -1.2067 0.3839 0.108 Uiso 0.50 1 calc PR A 2 C13' C -0.8438(19) -1.1325(12) 0.4074(9) 0.040(6) Uiso 0.50 1 d P A 2 H13D H -0.7780 -1.0917 0.4208 0.061 Uiso 0.50 1 calc PR A 2 H13E H -0.8363 -1.1696 0.3734 0.061 Uiso 0.50 1 calc PR A 2 H13F H -0.8492 -1.1599 0.4372 0.061 Uiso 0.50 1 calc PR A 2 C14' C -0.975(3) -1.0548(16) 0.4423(11) 0.075(8) Uiso 0.50 1 d P A 2 H14D H -0.9146 -1.0110 0.4617 0.113 Uiso 0.50 1 calc PR A 2 H14E H -0.9809 -1.0900 0.4673 0.113 Uiso 0.50 1 calc PR A 2 H14F H -1.0457 -1.0349 0.4326 0.113 Uiso 0.50 1 calc PR A 2 C15 C -0.8465(8) -1.0287(5) 0.3331(4) 0.030(2) Uani 1 1 d . . . H15A H -0.7824 -1.0502 0.3480 0.036 Uiso 1 1 calc R A . C16 C -0.7245(8) -1.0419(5) 0.2262(4) 0.030(2) Uani 1 1 d . . . C17 C -0.6814(8) -1.0313(5) 0.1801(4) 0.032(3) Uani 1 1 d . . . C18 C -0.6873(8) -1.0919(6) 0.1334(4) 0.031(3) Uani 1 1 d . . . C19 C -0.6656(11) -1.0824(7) 0.0762(4) 0.050(3) Uani 1 1 d . . . C20 C -0.7623(12) -1.0399(8) 0.0506(5) 0.077(4) Uani 1 1 d . . . H20A H -0.7514 -0.9858 0.0729 0.116 Uiso 1 1 calc R . . H20B H -0.8346 -1.0669 0.0518 0.116 Uiso 1 1 calc R . . H20C H -0.7613 -1.0405 0.0112 0.116 Uiso 1 1 calc R . . C21 C -0.5527(11) -1.0342(8) 0.0815(5) 0.073(4) Uani 1 1 d . . . H21A H -0.5532 -0.9796 0.1003 0.110 Uiso 1 1 calc R . . H21B H -0.5395 -1.0371 0.0437 0.110 Uiso 1 1 calc R . . H21C H -0.4928 -1.0548 0.1041 0.110 Uiso 1 1 calc R . . C22 C -0.6698(12) -1.1614(7) 0.0339(5) 0.069(4) Uani 1 1 d . . . H22A H -0.6199 -1.1929 0.0523 0.104 Uiso 1 1 calc R . . H22B H -0.6456 -1.1519 0.0006 0.104 Uiso 1 1 calc R . . H22C H -0.7467 -1.1894 0.0222 0.104 Uiso 1 1 calc R . . C23 C -0.7206(9) -1.1670(7) 0.1379(5) 0.047(3) Uani 1 1 d . . . H23A H -0.7183 -1.2099 0.1080 0.056 Uiso 1 1 calc R . . C24 C -0.7577(8) -1.1823(6) 0.1851(4) 0.038(3) Uani 1 1 d . . . C25 C -0.7924(10) -1.2674(6) 0.1868(5) 0.049(3) Uani 1 1 d . . . C26 C -0.8665(12) -1.3156(7) 0.1301(6) 0.081(5) Uani 1 1 d . . . H26A H -0.9337 -1.2914 0.1201 0.121 Uiso 1 1 calc R . . H26B H -0.8886 -1.3687 0.1333 0.121 Uiso 1 1 calc R . . H26C H -0.8247 -1.3176 0.1005 0.121 Uiso 1 1 calc R . . C27 C -0.6786(11) -1.3013(7) 0.2023(6) 0.071(4) Uani 1 1 d . . . H27A H -0.6381 -1.3008 0.1725 0.107 Uiso 1 1 calc R . . H27B H -0.6953 -1.3551 0.2056 0.107 Uiso 1 1 calc R . . H27C H -0.6322 -1.2691 0.2385 0.107 Uiso 1 1 calc R . . C28 C -0.8540(11) -1.2705(6) 0.2336(6) 0.067(4) Uani 1 1 d . . . H28A H -0.9207 -1.2448 0.2270 0.100 Uiso 1 1 calc R . . H28B H -0.8043 -1.2437 0.2704 0.100 Uiso 1 1 calc R . . H28C H -0.8767 -1.3251 0.2333 0.100 Uiso 1 1 calc R . . C29 C -0.7616(9) -1.1188(6) 0.2269(4) 0.034(3) Uani 1 1 d . . . H29A H -0.7909 -1.1274 0.2578 0.041 Uiso 1 1 calc R . . C30 C -0.6282(8) -0.9581(5) 0.3242(4) 0.025(2) Uani 1 1 d . B . C31 C -0.5761(8) -0.8817(5) 0.3544(4) 0.024(2) Uani 1 1 d . . . C32 C -0.4732(8) -0.8699(6) 0.3957(4) 0.032(3) Uani 1 1 d . . . C33 C -0.4047(10) -0.7880(7) 0.4250(5) 0.047(3) Uani 1 1 d . . . C34 C -0.3826(10) -0.7442(7) 0.3802(5) 0.057(3) Uani 1 1 d . . . H34A H -0.3348 -0.7717 0.3582 0.086 Uiso 1 1 calc R . . H34B H -0.3450 -0.6910 0.3992 0.086 Uiso 1 1 calc R . . H34C H -0.4541 -0.7422 0.3547 0.086 Uiso 1 1 calc R . . C35 C -0.4713(11) -0.7383(7) 0.4635(5) 0.064(4) Uani 1 1 d . . . H35A H -0.4910 -0.7670 0.4905 0.096 Uiso 1 1 calc R . . H35B H -0.5400 -0.7285 0.4397 0.096 Uiso 1 1 calc R . . H35C H -0.4246 -0.6884 0.4843 0.096 Uiso 1 1 calc R . . C36 C -0.2926(10) -0.7906(7) 0.4623(5) 0.070(4) Uani 1 1 d . . . H36A H -0.2560 -0.8307 0.4423 0.105 Uiso 1 1 calc R . . H36B H -0.3033 -0.8031 0.4975 0.105 Uiso 1 1 calc R . . H36C H -0.2455 -0.7396 0.4712 0.105 Uiso 1 1 calc R . . C37 C -0.4339(9) -0.9347(7) 0.4096(4) 0.041(3) Uani 1 1 d . . . H37A H -0.3672 -0.9277 0.4386 0.049 Uiso 1 1 calc R . . C38 C -0.4880(10) -1.0102(6) 0.3830(5) 0.043(3) Uani 1 1 d . B . C39 C -0.4404(10) -1.0813(7) 0.4013(5) 0.055(3) Uani 1 1 d . . . C40 C -0.325(2) -1.0833(15) 0.4003(11) 0.067(8) Uiso 0.50 1 d P B 3 H40A H -0.2943 -1.1181 0.4233 0.100 Uiso 0.50 1 calc PR B 3 H40B H -0.2828 -1.0306 0.4158 0.100 Uiso 0.50 1 calc PR B 3 H40C H -0.3195 -1.1026 0.3611 0.100 Uiso 0.50 1 calc PR B 3 C41 C -0.445(2) -1.0744(15) 0.4676(10) 0.067(7) Uiso 0.50 1 d P B 3 H41A H -0.4134 -1.0212 0.4900 0.100 Uiso 0.50 1 calc PR B 3 H41B H -0.4004 -1.1115 0.4826 0.100 Uiso 0.50 1 calc PR B 3 H41C H -0.5225 -1.0863 0.4699 0.100 Uiso 0.50 1 calc PR B 3 C42 C -0.516(2) -1.1632(12) 0.3680(10) 0.047(6) Uiso 0.50 1 d P B 3 H42A H -0.5121 -1.1748 0.3282 0.071 Uiso 0.50 1 calc PR B 3 H42B H -0.5944 -1.1604 0.3701 0.071 Uiso 0.50 1 calc PR B 3 H42C H -0.4893 -1.2046 0.3854 0.071 Uiso 0.50 1 calc PR B 3 C40' C -0.341(2) -1.0538(16) 0.4515(12) 0.080(9) Uiso 0.50 1 d P B 4 H40D H -0.2800 -1.0255 0.4404 0.120 Uiso 0.50 1 calc PR B 4 H40E H -0.3146 -1.0990 0.4641 0.120 Uiso 0.50 1 calc PR B 4 H40F H -0.3624 -1.0192 0.4826 0.120 Uiso 0.50 1 calc PR B 4 C41' C -0.529(2) -1.1282(16) 0.4111(12) 0.072(8) Uiso 0.50 1 d P B 4 H41D H -0.5535 -1.1747 0.3795 0.108 Uiso 0.50 1 calc PR B 4 H41E H -0.5910 -1.0987 0.4141 0.108 Uiso 0.50 1 calc PR B 4 H41F H -0.5028 -1.1441 0.4464 0.108 Uiso 0.50 1 calc PR B 4 C42' C -0.399(2) -1.1218(16) 0.3484(11) 0.077(8) Uiso 0.50 1 d P B 4 H42D H -0.4506 -1.1177 0.3137 0.116 Uiso 0.50 1 calc PR B 4 H42E H -0.3965 -1.1769 0.3480 0.116 Uiso 0.50 1 calc PR B 4 H42F H -0.3237 -1.0960 0.3504 0.116 Uiso 0.50 1 calc PR B 4 C43 C -0.5808(8) -1.0210(6) 0.3394(4) 0.028(2) Uani 1 1 d . . . H43A H -0.6139 -1.0726 0.3190 0.033 Uiso 1 1 calc R B . C44 C -0.9262(9) -0.9362(5) 0.1798(4) 0.034(3) Uani 1 1 d . . . H44A H -1.0038 -0.9600 0.1591 0.041 Uiso 1 1 calc R . . H44B H -0.8780 -0.9777 0.1779 0.041 Uiso 1 1 calc R . . C45 C -0.8847(9) -0.8739(5) 0.1537(4) 0.035(3) Uani 1 1 d . . . H45A H -0.8095 -0.8478 0.1767 0.042 Uiso 1 1 calc R . . H45B H -0.8770 -0.8984 0.1151 0.042 Uiso 1 1 calc R . . C46 C -0.9277(9) -0.7430(5) 0.1496(4) 0.027(2) Uani 1 1 d . . . C47 C -1.0125(8) -0.6881(5) 0.1422(4) 0.034(3) Uani 1 1 d . . . H47A H -1.0864 -0.7141 0.1434 0.040 Uiso 1 1 calc R . . H47B H -1.0198 -0.6767 0.1045 0.040 Uiso 1 1 calc R . . C48 C -1.0506(9) -0.5286(5) 0.1688(5) 0.037(3) Uani 1 1 d . . . C49 C -1.0802(10) -0.4689(7) 0.2063(6) 0.056(4) Uani 1 1 d . . . H49A H -1.0643 -0.4682 0.2455 0.068 Uiso 1 1 calc R . . C50 C -1.1330(12) -0.4096(8) 0.1879(7) 0.074(4) Uani 1 1 d . . . H50A H -1.1534 -0.3694 0.2143 0.089 Uiso 1 1 calc R . . C51 C -1.1548(11) -0.4104(7) 0.1319(7) 0.070(4) Uani 1 1 d . . . H51A H -1.1895 -0.3698 0.1192 0.084 Uiso 1 1 calc R . . C52 C -1.1273(10) -0.4688(7) 0.0935(5) 0.057(3) Uani 1 1 d . . . H52A H -1.1448 -0.4692 0.0544 0.068 Uiso 1 1 calc R . . C53 C -1.0738(9) -0.5274(6) 0.1115(5) 0.044(3) Uani 1 1 d . . . H53A H -1.0530 -0.5668 0.0848 0.053 Uiso 1 1 calc R . . C54 C -1.0269(9) -0.6112(6) 0.2556(4) 0.033(3) Uani 1 1 d . . . C55 C -1.1403(9) -0.6315(6) 0.2501(5) 0.045(3) Uani 1 1 d . . . H55A H -1.1904 -0.6423 0.2137 0.054 Uiso 1 1 calc R . . C56 C -1.1824(12) -0.6365(7) 0.2978(6) 0.067(4) Uani 1 1 d . . . H56A H -1.2607 -0.6466 0.2948 0.080 Uiso 1 1 calc R . . C57 C -1.1055(14) -0.6260(8) 0.3494(6) 0.076(4) Uani 1 1 d . . . H57A H -1.1318 -0.6319 0.3817 0.091 Uiso 1 1 calc R . . C58 C -0.9946(12) -0.6077(7) 0.3547(5) 0.062(4) Uani 1 1 d . . . H58A H -0.9433 -0.6002 0.3904 0.074 Uiso 1 1 calc R . . C59 C -0.9560(11) -0.6000(6) 0.3071(5) 0.049(3) Uani 1 1 d . . . H59A H -0.8778 -0.5866 0.3109 0.058 Uiso 1 1 calc R . . C60 C -0.5326(8) -0.9257(5) 0.2140(4) 0.030(2) Uani 1 1 d . . . H60A H -0.4776 -0.9530 0.1965 0.036 Uiso 1 1 calc R . . H60B H -0.5274 -0.9362 0.2519 0.036 Uiso 1 1 calc R . . C61 C -0.5076(9) -0.8400(5) 0.2195(4) 0.031(3) Uani 1 1 d . . . H61A H -0.5712 -0.8151 0.2298 0.038 Uiso 1 1 calc R . . H61B H -0.4404 -0.8181 0.2508 0.038 Uiso 1 1 calc R . . C62 C -0.5337(8) -0.7631(6) 0.1501(4) 0.029(2) Uani 1 1 d . . . C63 C -0.4896(9) -0.7373(6) 0.1024(4) 0.038(3) Uani 1 1 d . . . H63A H -0.4621 -0.7816 0.0803 0.045 Uiso 1 1 calc R . . H63B H -0.4256 -0.6946 0.1194 0.045 Uiso 1 1 calc R . . C64 C -0.5296(10) -0.6647(7) 0.0078(4) 0.043(3) Uani 1 1 d . . . C65 C -0.586(2) -0.6895(14) -0.0510(10) 0.054(7) Uiso 0.50 1 d P C 5 H65A H -0.6499 -0.7284 -0.0654 0.065 Uiso 0.50 1 calc PR C 5 C66 C -0.534(2) -0.6489(14) -0.0869(11) 0.054(7) Uiso 0.50 1 d P C 5 H66A H -0.5652 -0.6612 -0.1266 0.065 Uiso 0.50 1 calc PR C 5 C65' C -0.590(2) -0.6279(12) -0.0274(9) 0.043(6) Uiso 0.50 1 d P C 6 H65B H -0.6667 -0.6266 -0.0282 0.052 Uiso 0.50 1 calc PR C 6 C66' C -0.541(2) -0.5918(16) -0.0628(11) 0.073(8) Uiso 0.50 1 d P C 6 H66B H -0.5860 -0.5668 -0.0874 0.088 Uiso 0.50 1 calc PR C 6 C67 C -0.4366(12) -0.5912(7) -0.0631(6) 0.069(4) Uiso 1 1 d . . . H67A H -0.4035 -0.5660 -0.0870 0.083 Uiso 1 1 calc R C 5 C68 C -0.394(3) -0.573(2) -0.0097(15) 0.108(12) Uiso 0.50 1 d P C 5 H68A H -0.3294 -0.5352 0.0064 0.129 Uiso 0.50 1 calc PR C 5 C69 C -0.446(3) -0.613(2) 0.0258(15) 0.094(11) Uiso 0.50 1 d P C 5 H69A H -0.4151 -0.5975 0.0655 0.113 Uiso 0.50 1 calc PR C 5 C68' C -0.3654(19) -0.6196(12) -0.0221(8) 0.034(5) Uiso 0.50 1 d P C 6 H68B H -0.2876 -0.6168 -0.0210 0.040 Uiso 0.50 1 calc PR C 6 C69' C -0.4083(16) -0.6512(11) 0.0161(8) 0.024(5) Uiso 0.50 1 d P C 6 H69B H -0.3604 -0.6640 0.0470 0.029 Uiso 0.50 1 calc PR C 6 C70 C -0.6984(9) -0.7845(6) 0.0165(4) 0.037(3) Uani 1 1 d . . . C71 C -0.8091(12) -0.7828(8) 0.0153(5) 0.072(4) Uiso 1 1 d . C . H71A H -0.8317 -0.7367 0.0342 0.086 Uiso 1 1 calc R . . C72 C -0.8906(15) -0.8485(9) -0.0135(6) 0.098(5) Uiso 1 1 d . . . H72A H -0.9676 -0.8486 -0.0134 0.118 Uiso 1 1 calc R C . C73 C -0.8516(13) -0.9152(9) -0.0431(6) 0.084(4) Uiso 1 1 d . C . H73A H -0.9042 -0.9603 -0.0633 0.100 Uiso 1 1 calc R . . C74 C -0.7439(13) -0.9158(8) -0.0430(6) 0.076(4) Uiso 1 1 d . . . H74A H -0.7205 -0.9604 -0.0635 0.091 Uiso 1 1 calc R C . C75 C -0.6670(11) -0.8515(7) -0.0133(5) 0.060(3) Uiso 1 1 d . C . H75A H -0.5900 -0.8526 -0.0129 0.072 Uiso 1 1 calc R . . C76 C -0.7185(8) -0.8003(5) 0.3589(4) 0.027(2) Uani 1 1 d . . . H76A H -0.6983 -0.7841 0.4009 0.032 Uiso 1 1 calc R . . H76B H -0.7776 -0.8466 0.3468 0.032 Uiso 1 1 calc R . . C77 C -0.7596(9) -0.7350(5) 0.3348(4) 0.039(3) Uani 1 1 d . . . H77A H -0.7754 -0.7511 0.2929 0.046 Uiso 1 1 calc R . . H77B H -0.8306 -0.7244 0.3454 0.046 Uiso 1 1 calc R . . C78 C -0.6358(9) -0.6267(6) 0.3214(4) 0.038(3) Uani 1 1 d . . . C79 C -0.5484(10) -0.5558(6) 0.3480(5) 0.051(3) Uani 1 1 d . . . H79A H -0.4765 -0.5669 0.3387 0.061 Uiso 1 1 calc R . . H79B H -0.5370 -0.5444 0.3898 0.061 Uiso 1 1 calc R . . C80 C -0.6967(12) -0.4384(6) 0.3563(5) 0.052(4) Uani 1 1 d . . . C81 C -0.7773(12) -0.4051(8) 0.3256(6) 0.070(4) Uani 1 1 d . . . H81A H -0.7734 -0.4013 0.2885 0.083 Uiso 1 1 calc R . . C82 C -0.8633(14) -0.3774(8) 0.3477(6) 0.087(5) Uani 1 1 d . . . H82A H -0.9202 -0.3571 0.3253 0.105 Uiso 1 1 calc R . . C83 C -0.8658(17) -0.3795(9) 0.4035(8) 0.095(6) Uani 1 1 d . . . H83A H -0.9222 -0.3582 0.4200 0.114 Uiso 1 1 calc R . . C84 C -0.7869(17) -0.4125(8) 0.4336(6) 0.088(6) Uani 1 1 d . . . H84A H -0.7907 -0.4157 0.4709 0.106 Uiso 1 1 calc R . . C85 C -0.7003(13) -0.4416(6) 0.4115(5) 0.069(4) Uani 1 1 d . . . H85A H -0.6448 -0.4633 0.4335 0.083 Uiso 1 1 calc R . . C86 C -0.4714(7) -0.3963(5) 0.3472(4) 0.062(4) Uiso 1 1 d G . . C87 C -0.4292(8) -0.3619(5) 0.4047(4) 0.078(4) Uiso 1 1 d G . . H87A H -0.4684 -0.3741 0.4315 0.093 Uiso 1 1 calc R . . C88 C -0.3298(8) -0.3096(5) 0.4229(3) 0.076(4) Uiso 1 1 d G . . H88A H -0.3010 -0.2861 0.4622 0.091 Uiso 1 1 calc R . . C89 C -0.2725(7) -0.2918(6) 0.3837(5) 0.127(7) Uiso 1 1 d G . . H89A H -0.2045 -0.2561 0.3961 0.153 Uiso 1 1 calc R . . C90 C -0.3146(10) -0.3262(7) 0.3262(5) 0.182(10) Uiso 1 1 d G . . H90A H -0.2755 -0.3140 0.2993 0.219 Uiso 1 1 calc R . . C91 C -0.4141(10) -0.3784(6) 0.3080(3) 0.143(7) Uiso 1 1 d G . . H91A H -0.4429 -0.4019 0.2687 0.172 Uiso 1 1 calc R . . N4 N -0.8104(9) -0.5321(6) 0.0929(4) 0.042(2) Uani 1 1 d . . . O10 O -0.8495(6) -0.6002(4) 0.0957(3) 0.0381(18) Uani 1 1 d . . . O11 O -0.7296(7) -0.4959(4) 0.1341(3) 0.0401(19) Uani 1 1 d . . . O12 O -0.8464(8) -0.5041(5) 0.0538(3) 0.063(2) Uani 1 1 d . . . N5 N -0.4368(12) -0.5405(7) 0.1973(6) 0.077(4) Uani 1 1 d . . . O13 O -0.4667(7) -0.5928(5) 0.2222(4) 0.081(3) Uani 1 1 d . . . O14 O -0.5133(8) -0.5129(5) 0.1694(4) 0.062(2) Uani 1 1 d . . . O15 O -0.3395(9) -0.5192(8) 0.2015(8) 0.177(7) Uani 1 1 d . . . N6 N 0.7405(7) 0.1414(5) 0.1123(3) 0.033(2) Uani 1 1 d . . . O16 O 0.6461(6) 0.1014(4) 0.0967(3) 0.0453(19) Uani 1 1 d . . . O17 O 0.7543(6) 0.2082(4) 0.1413(3) 0.058(2) Uani 1 1 d . . . O18 O 0.8221(6) 0.1119(4) 0.0968(3) 0.047(2) Uani 1 1 d . . . N7 N 0.6783(17) 0.5788(11) 0.5136(8) 0.144(6) Uiso 1 1 d D . . O19 O 0.5893(11) 0.5778(6) 0.5258(5) 0.108(4) Uiso 1 1 d D . . O20 O 0.6808(13) 0.5168(9) 0.4676(6) 0.164(5) Uiso 1 1 d D . . O21 O 0.7751(16) 0.6189(10) 0.5336(7) 0.186(6) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Th1 0.0270(2) 0.0273(2) 0.0330(2) 0.00651(15) 0.01606(17) -0.00017(16) P1 0.0353(18) 0.0320(16) 0.0423(17) 0.0086(13) 0.0223(15) 0.0039(14) P2 0.0384(19) 0.0400(17) 0.0351(16) 0.0123(13) 0.0191(15) 0.0100(15) P3 0.066(2) 0.0380(18) 0.0395(19) -0.0005(14) 0.0189(18) -0.0189(17) N1 0.027(5) 0.032(5) 0.049(6) 0.012(4) 0.011(5) 0.000(4) N2 0.032(5) 0.041(5) 0.032(5) 0.018(4) 0.017(4) 0.013(4) N3 0.054(6) 0.028(5) 0.028(5) 0.006(4) 0.017(5) -0.005(5) O1 0.035(4) 0.027(4) 0.029(4) 0.012(3) 0.007(3) 0.003(3) O2 0.029(4) 0.037(4) 0.031(4) 0.012(3) 0.009(3) 0.004(3) O3 0.030(4) 0.040(4) 0.032(4) 0.004(3) 0.013(4) 0.004(4) O4 0.032(5) 0.024(4) 0.044(4) 0.006(3) 0.011(4) -0.002(3) O5 0.032(4) 0.028(4) 0.042(4) -0.006(3) 0.014(4) -0.003(3) O6 0.036(5) 0.036(4) 0.045(4) 0.013(3) 0.023(4) 0.009(4) O7 0.046(5) 0.032(4) 0.034(4) 0.008(3) 0.016(4) 0.009(4) O8 0.039(5) 0.034(4) 0.034(4) 0.011(3) 0.017(4) 0.000(4) O9 0.052(5) 0.044(4) 0.039(4) 0.005(3) 0.022(4) -0.010(4) C1 0.012(5) 0.029(5) 0.031(6) 0.007(5) 0.002(5) -0.004(4) C2 0.013(5) 0.035(6) 0.019(5) 0.007(4) -0.002(4) 0.007(5) C3 0.039(7) 0.016(5) 0.030(6) 0.007(4) 0.018(5) -0.003(5) C4 0.024(6) 0.030(6) 0.030(6) 0.016(5) 0.002(5) 0.007(5) C5 0.036(7) 0.060(8) 0.036(7) 0.017(6) 0.014(6) 0.000(6) C6 0.053(10) 0.061(9) 0.194(17) 0.060(10) 0.052(11) 0.031(8) C7 0.039(9) 0.121(12) 0.065(10) 0.033(9) 0.006(7) 0.017(9) C8 0.054(9) 0.105(11) 0.077(10) 0.046(8) 0.032(8) 0.051(8) C9 0.022(6) 0.054(7) 0.048(7) 0.025(6) 0.020(6) -0.001(6) C10 0.033(7) 0.046(7) 0.042(7) 0.021(5) 0.018(6) 0.016(6) C11 0.058(8) 0.057(8) 0.034(7) 0.029(6) 0.027(6) 0.019(7) C15 0.027(6) 0.039(6) 0.023(6) 0.011(5) -0.001(5) 0.005(5) C16 0.033(7) 0.029(6) 0.030(6) 0.004(5) 0.015(5) 0.002(5) C17 0.025(6) 0.026(6) 0.042(7) 0.001(5) 0.013(5) 0.002(5) C18 0.025(6) 0.042(7) 0.027(6) 0.001(5) 0.016(5) 0.000(5) C19 0.062(9) 0.052(7) 0.034(7) 0.007(6) 0.014(6) 0.004(7) C20 0.091(12) 0.089(11) 0.056(9) 0.024(8) 0.019(9) 0.019(9) C21 0.079(11) 0.095(10) 0.046(8) 0.002(7) 0.045(8) -0.016(9) C22 0.103(12) 0.061(9) 0.053(8) 0.009(7) 0.044(8) 0.012(8) C23 0.035(7) 0.052(8) 0.045(7) -0.005(6) 0.017(6) -0.006(6) C24 0.022(6) 0.041(7) 0.053(7) 0.004(6) 0.024(6) -0.002(5) C25 0.046(8) 0.029(6) 0.066(8) -0.004(6) 0.027(7) -0.010(6) C26 0.079(11) 0.050(8) 0.094(11) -0.010(8) 0.021(9) -0.022(8) C27 0.080(11) 0.048(8) 0.108(11) 0.037(8) 0.041(9) 0.031(8) C28 0.079(10) 0.033(7) 0.106(11) 0.024(7) 0.054(9) 0.012(7) C29 0.044(7) 0.034(6) 0.039(6) 0.017(5) 0.028(6) 0.014(5) C30 0.022(6) 0.033(6) 0.025(6) 0.011(5) 0.009(5) 0.004(5) C31 0.022(6) 0.030(6) 0.025(6) 0.011(5) 0.015(5) 0.006(5) C32 0.019(6) 0.050(7) 0.019(6) -0.002(5) 0.005(5) -0.001(5) C33 0.036(7) 0.060(8) 0.041(7) 0.005(6) 0.007(6) 0.005(6) C34 0.048(8) 0.055(8) 0.053(8) -0.015(6) 0.014(7) -0.005(7) C35 0.055(9) 0.063(9) 0.064(9) -0.011(7) 0.016(8) 0.014(7) C36 0.026(7) 0.064(9) 0.086(10) -0.021(7) -0.019(7) 0.006(7) C37 0.031(7) 0.061(8) 0.035(7) 0.019(6) 0.004(6) 0.016(6) C38 0.045(8) 0.045(7) 0.046(7) 0.012(6) 0.019(7) 0.013(6) C39 0.041(8) 0.065(8) 0.059(8) 0.023(7) 0.001(7) 0.019(7) C43 0.014(6) 0.036(6) 0.033(6) 0.011(5) 0.003(5) 0.006(5) C44 0.043(7) 0.038(6) 0.023(6) 0.007(5) 0.013(5) 0.003(5) C45 0.034(7) 0.035(6) 0.047(7) 0.020(5) 0.019(6) 0.017(5) C46 0.028(7) 0.023(6) 0.026(6) 0.004(4) 0.004(5) -0.003(5) C47 0.019(6) 0.034(6) 0.045(7) 0.004(5) 0.010(5) -0.001(5) C48 0.037(7) 0.026(6) 0.049(7) 0.006(5) 0.017(6) 0.002(5) C49 0.054(9) 0.054(8) 0.085(10) 0.031(7) 0.043(8) 0.031(7) C50 0.086(12) 0.073(10) 0.091(12) 0.032(9) 0.051(10) 0.053(9) C51 0.056(10) 0.053(9) 0.118(13) 0.033(9) 0.033(10) 0.029(7) C52 0.057(9) 0.059(8) 0.058(8) 0.026(7) 0.009(7) 0.017(7) C53 0.026(7) 0.044(7) 0.068(9) 0.020(6) 0.016(6) 0.007(6) C54 0.035(7) 0.036(6) 0.032(6) 0.011(5) 0.015(6) 0.002(5) C55 0.030(7) 0.056(7) 0.052(7) 0.019(6) 0.017(6) -0.002(6) C56 0.067(10) 0.074(9) 0.063(9) 0.009(8) 0.041(9) -0.004(8) C57 0.091(13) 0.079(10) 0.057(10) 0.013(8) 0.037(10) -0.014(9) C58 0.074(11) 0.064(9) 0.044(8) 0.008(6) 0.021(8) -0.013(8) C59 0.061(9) 0.042(7) 0.056(8) 0.017(6) 0.037(8) 0.015(6) C60 0.025(6) 0.037(6) 0.033(6) 0.011(5) 0.015(5) 0.005(5) C61 0.033(7) 0.035(6) 0.030(6) 0.005(5) 0.020(5) 0.001(5) C62 0.025(6) 0.028(6) 0.031(6) -0.003(5) 0.011(5) -0.005(5) C63 0.035(7) 0.053(7) 0.040(6) 0.025(5) 0.025(6) 0.012(6) C64 0.046(8) 0.053(7) 0.038(7) 0.012(6) 0.022(6) 0.011(6) C70 0.047(8) 0.043(7) 0.028(6) 0.011(5) 0.018(6) 0.012(6) C76 0.029(6) 0.015(5) 0.031(6) -0.002(4) 0.006(5) -0.006(5) C77 0.044(7) 0.032(6) 0.040(7) 0.010(5) 0.013(6) -0.002(6) C78 0.045(7) 0.033(6) 0.033(7) 0.003(5) 0.015(6) -0.011(5) C79 0.047(8) 0.051(7) 0.042(7) -0.005(6) 0.013(6) -0.020(6) C80 0.079(10) 0.026(6) 0.051(8) 0.000(6) 0.036(8) -0.013(7) C81 0.079(12) 0.074(10) 0.062(9) 0.005(8) 0.039(9) 0.017(9) C82 0.113(14) 0.075(10) 0.080(11) -0.002(8) 0.055(11) 0.025(10) C83 0.128(17) 0.064(11) 0.101(14) 0.011(10) 0.059(13) -0.002(10) C84 0.162(19) 0.054(10) 0.061(10) -0.007(8) 0.076(12) 0.010(10) C85 0.117(13) 0.037(7) 0.054(9) 0.009(6) 0.029(9) 0.003(8) N4 0.046(7) 0.047(6) 0.045(6) 0.019(6) 0.020(6) 0.019(6) O10 0.031(5) 0.038(4) 0.050(5) 0.014(4) 0.014(4) 0.007(4) O11 0.051(5) 0.028(4) 0.041(5) 0.008(4) 0.012(4) 0.001(4) O12 0.080(7) 0.064(6) 0.056(5) 0.033(5) 0.016(5) 0.017(5) N5 0.066(10) 0.050(8) 0.123(12) 0.021(7) 0.041(9) -0.003(7) O13 0.035(6) 0.060(6) 0.141(9) 0.033(6) 0.001(6) 0.008(5) O14 0.057(7) 0.076(6) 0.061(6) 0.014(5) 0.038(5) -0.007(5) O15 0.044(8) 0.155(12) 0.36(2) 0.095(13) 0.080(11) -0.016(8) N6 0.026(6) 0.034(6) 0.036(5) 0.006(4) 0.007(5) -0.001(5) O16 0.019(4) 0.043(4) 0.064(5) 0.000(4) 0.008(4) -0.011(4) O17 0.047(6) 0.035(5) 0.086(6) -0.008(4) 0.030(5) -0.003(4) O18 0.025(4) 0.056(5) 0.053(5) -0.004(4) 0.012(4) 0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Th1 O7 2.395(6) . ? Th1 O9 2.412(7) . ? Th1 O8 2.419(6) . ? Th1 O4 2.419(6) . ? Th1 O5 2.431(6) . ? Th1 O6 2.483(6) . ? Th1 O11 2.528(6) . ? Th1 O13 2.613(8) . ? Th1 O14 2.637(8) . ? Th1 O10 2.664(7) . ? Th1 N4 3.032(10) . ? P1 O5 1.516(7) . ? P1 C48 1.772(11) . ? P1 C54 1.783(9) . ? P1 C47 1.800(9) . ? P2 O7 1.511(6) . ? P2 C70 1.762(11) . ? P2 C64 1.787(10) . ? P2 C63 1.802(10) . ? P3 O9 1.485(7) . ? P3 C86 1.764(8) . ? P3 C80 1.796(12) . ? P3 C79 1.796(12) . ? N1 C46 1.312(11) . ? N1 C45 1.460(11) . ? N2 C62 1.313(12) . ? N2 C61 1.458(10) . ? N3 C78 1.321(11) . ? N3 C77 1.465(12) . ? O1 C3 1.407(10) . ? O1 C44 1.435(10) . ? O2 C17 1.414(10) . ? O2 C60 1.447(11) . ? O3 C31 1.394(10) . ? O3 C76 1.449(11) . ? O4 C46 1.276(11) . ? O6 C62 1.233(10) . ? O8 C78 1.262(11) . ? C1 C2 1.525(12) . ? C1 C16 1.530(12) . ? C1 C30 1.535(12) . ? C2 C3 1.380(12) . ? C2 C15 1.386(12) . ? C3 C4 1.440(13) . ? C4 C9 1.411(12) . ? C4 C5 1.530(14) . ? C5 C8 1.528(14) . ? C5 C7 1.534(15) . ? C5 C6 1.535(15) . ? C9 C10 1.373(13) . ? C10 C15 1.397(13) . ? C10 C11 1.529(13) . ? C11 C14' 1.39(3) . ? C11 C13 1.40(2) . ? C11 C13' 1.53(2) . ? C11 C12 1.55(2) . ? C11 C12' 1.62(3) . ? C11 C14 1.66(3) . ? C16 C29 1.401(12) . ? C16 C17 1.401(12) . ? C17 C18 1.385(12) . ? C18 C23 1.390(13) . ? C18 C19 1.542(13) . ? C19 C21 1.527(16) . ? C19 C22 1.549(14) . ? C19 C20 1.568(16) . ? C23 C24 1.412(13) . ? C24 C29 1.369(13) . ? C24 C25 1.541(13) . ? C25 C28 1.524(14) . ? C25 C26 1.530(16) . ? C25 C27 1.587(16) . ? C30 C43 1.396(12) . ? C30 C31 1.414(12) . ? C31 C32 1.419(13) . ? C32 C37 1.375(13) . ? C32 C33 1.549(14) . ? C33 C36 1.504(15) . ? C33 C34 1.543(14) . ? C33 C35 1.573(14) . ? C37 C38 1.390(14) . ? C38 C43 1.366(14) . ? C38 C39 1.557(15) . ? C39 C41' 1.40(3) . ? C39 C40 1.43(3) . ? C39 C40' 1.51(3) . ? C39 C42' 1.57(3) . ? C39 C42 1.60(2) . ? C39 C41 1.64(2) . ? C44 C45 1.499(12) . ? C46 C47 1.507(13) . ? C48 C49 1.384(14) . ? C48 C53 1.396(14) . ? C49 C50 1.398(15) . ? C50 C51 1.358(17) . ? C51 C52 1.370(16) . ? C52 C53 1.388(14) . ? C54 C59 1.353(14) . ? C54 C55 1.381(14) . ? C55 C56 1.406(14) . ? C56 C57 1.389(18) . ? C57 C58 1.347(18) . ? C58 C59 1.392(14) . ? C60 C61 1.494(12) . ? C62 C63 1.539(12) . ? C64 C69 1.25(3) . ? C64 C65' 1.34(2) . ? C64 C65 1.43(2) . ? C64 C69' 1.46(2) . ? C65 C66 1.47(3) . ? C66 C67 1.42(3) . ? C65' C66' 1.39(3) . ? C66' C67 1.29(3) . ? C67 C68 1.28(3) . ? C67 C68' 1.41(2) . ? C68 C69 1.45(4) . ? C68' C69' 1.37(2) . ? C70 C71 1.364(16) . ? C70 C75 1.393(14) . ? C71 C72 1.411(19) . ? C72 C73 1.434(18) . ? C73 C74 1.329(18) . ? C74 C75 1.371(17) . ? C76 C77 1.499(12) . ? C78 C79 1.502(13) . ? C80 C81 1.381(17) . ? C80 C85 1.395(15) . ? C81 C82 1.378(17) . ? C82 C83 1.403(18) . ? C83 C84 1.36(2) . ? C84 C85 1.394(19) . ? C86 C87 1.3900 . ? C86 C91 1.3900 . ? C87 C88 1.3900 . ? C88 C89 1.3900 . ? C89 C90 1.3900 . ? C90 C91 1.3900 . ? N4 O12 1.209(10) . ? N4 O11 1.270(11) . ? N4 O10 1.277(10) . ? N5 O15 1.198(14) . ? N5 O14 1.253(14) . ? N5 O13 1.288(13) . ? N6 O17 1.222(10) . ? N6 O16 1.241(10) . ? N6 O18 1.271(10) . ? N7 O19 1.198(18) . ? N7 O21 1.27(2) . ? N7 O20 1.413(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Th1 O9 135.6(2) . . ? O7 Th1 O8 139.7(2) . . ? O9 Th1 O8 72.8(2) . . ? O7 Th1 O4 88.2(2) . . ? O9 Th1 O4 135.6(2) . . ? O8 Th1 O4 75.4(2) . . ? O7 Th1 O5 132.2(2) . . ? O9 Th1 O5 72.8(2) . . ? O8 Th1 O5 76.7(2) . . ? O4 Th1 O5 70.3(2) . . ? O7 Th1 O6 69.1(2) . . ? O9 Th1 O6 127.3(2) . . ? O8 Th1 O6 70.6(2) . . ? O4 Th1 O6 66.6(2) . . ? O5 Th1 O6 130.8(2) . . ? O7 Th1 O11 73.9(2) . . ? O9 Th1 O11 78.6(2) . . ? O8 Th1 O11 146.4(2) . . ? O4 Th1 O11 116.3(2) . . ? O5 Th1 O11 78.3(2) . . ? O6 Th1 O11 142.8(2) . . ? O7 Th1 O13 86.7(3) . . ? O9 Th1 O13 71.6(3) . . ? O8 Th1 O13 76.1(3) . . ? O4 Th1 O13 128.5(2) . . ? O5 Th1 O13 140.1(3) . . ? O6 Th1 O13 63.8(2) . . ? O11 Th1 O13 111.2(3) . . ? O7 Th1 O14 67.5(2) . . ? O9 Th1 O14 69.1(2) . . ? O8 Th1 O14 119.9(3) . . ? O4 Th1 O14 155.2(2) . . ? O5 Th1 O14 129.6(2) . . ? O6 Th1 O14 98.8(3) . . ? O11 Th1 O14 62.9(3) . . ? O13 Th1 O14 48.8(3) . . ? O7 Th1 O10 64.2(2) . . ? O9 Th1 O10 118.6(2) . . ? O8 Th1 O10 135.7(2) . . ? O4 Th1 O10 68.1(2) . . ? O5 Th1 O10 68.1(2) . . ? O6 Th1 O10 114.1(2) . . ? O11 Th1 O10 48.9(2) . . ? O13 Th1 O10 147.4(3) . . ? O14 Th1 O10 103.3(3) . . ? O7 Th1 N4 64.5(2) . . ? O9 Th1 N4 100.1(3) . . ? O8 Th1 N4 150.8(2) . . ? O4 Th1 N4 92.9(3) . . ? O5 Th1 N4 74.2(2) . . ? O6 Th1 N4 129.5(2) . . ? O11 Th1 N4 24.3(2) . . ? O13 Th1 N4 129.5(3) . . ? O14 Th1 N4 81.2(3) . . ? O10 Th1 N4 24.8(2) . . ? O5 P1 C48 112.4(4) . . ? O5 P1 C54 110.6(5) . . ? C48 P1 C54 106.0(5) . . ? O5 P1 C47 112.2(4) . . ? C48 P1 C47 107.0(5) . . ? C54 P1 C47 108.2(5) . . ? O7 P2 C70 110.8(5) . . ? O7 P2 C64 111.2(4) . . ? C70 P2 C64 109.8(5) . . ? O7 P2 C63 109.0(4) . . ? C70 P2 C63 108.6(5) . . ? C64 P2 C63 107.5(5) . . ? O9 P3 C86 109.9(4) . . ? O9 P3 C80 111.5(6) . . ? C86 P3 C80 107.8(5) . . ? O9 P3 C79 110.4(5) . . ? C86 P3 C79 109.2(5) . . ? C80 P3 C79 108.0(5) . . ? C46 N1 C45 124.2(8) . . ? C62 N2 C61 120.7(8) . . ? C78 N3 C77 123.8(8) . . ? C3 O1 C44 117.1(7) . . ? C17 O2 C60 111.3(7) . . ? C31 O3 C76 114.1(7) . . ? C46 O4 Th1 144.2(6) . . ? P1 O5 Th1 138.5(4) . . ? C62 O6 Th1 143.5(6) . . ? P2 O7 Th1 140.7(4) . . ? C78 O8 Th1 142.1(6) . . ? P3 O9 Th1 139.5(4) . . ? C2 C1 C16 111.3(7) . . ? C2 C1 C30 110.3(7) . . ? C16 C1 C30 111.5(8) . . ? C3 C2 C15 118.0(8) . . ? C3 C2 C1 120.9(8) . . ? C15 C2 C1 121.0(9) . . ? C2 C3 O1 120.2(8) . . ? C2 C3 C4 122.2(8) . . ? O1 C3 C4 117.2(8) . . ? C9 C4 C3 115.1(9) . . ? C9 C4 C5 119.9(9) . . ? C3 C4 C5 125.0(8) . . ? C8 C5 C4 112.9(8) . . ? C8 C5 C7 107.0(10) . . ? C4 C5 C7 110.4(9) . . ? C8 C5 C6 106.4(10) . . ? C4 C5 C6 111.7(9) . . ? C7 C5 C6 108.0(10) . . ? C10 C9 C4 124.3(9) . . ? C9 C10 C15 116.8(9) . . ? C9 C10 C11 122.1(9) . . ? C15 C10 C11 121.2(9) . . ? C14' C11 C13 135.1(16) . . ? C14' C11 C10 111.0(14) . . ? C13 C11 C10 113.4(12) . . ? C14' C11 C13' 110.4(16) . . ? C13 C11 C13' 43.7(12) . . ? C10 C11 C13' 113.5(11) . . ? C14' C11 C12 46.1(13) . . ? C13 C11 C12 118.2(15) . . ? C10 C11 C12 112.3(11) . . ? C13' C11 C12 133.9(13) . . ? C14' C11 C12' 112.3(17) . . ? C13 C11 C12' 60.3(14) . . ? C10 C11 C12' 106.8(12) . . ? C13' C11 C12' 102.4(14) . . ? C12 C11 C12' 68.3(13) . . ? C14' C11 C14 55.6(15) . . ? C13 C11 C14 104.8(16) . . ? C10 C11 C14 105.8(12) . . ? C13' C11 C14 62.6(13) . . ? C12 C11 C14 100.3(13) . . ? C12' C11 C14 147.4(14) . . ? C2 C15 C10 123.3(9) . . ? C29 C16 C17 117.0(8) . . ? C29 C16 C1 121.3(8) . . ? C17 C16 C1 121.7(8) . . ? C18 C17 C16 122.4(9) . . ? C18 C17 O2 119.7(8) . . ? C16 C17 O2 117.4(8) . . ? C17 C18 C23 117.0(9) . . ? C17 C18 C19 125.3(9) . . ? C23 C18 C19 117.7(9) . . ? C21 C19 C18 113.9(9) . . ? C21 C19 C22 106.5(10) . . ? C18 C19 C22 112.9(9) . . ? C21 C19 C20 109.2(10) . . ? C18 C19 C20 105.5(9) . . ? C22 C19 C20 108.6(10) . . ? C18 C23 C24 122.9(10) . . ? C29 C24 C23 116.8(9) . . ? C29 C24 C25 123.7(9) . . ? C23 C24 C25 119.5(9) . . ? C28 C25 C26 109.2(10) . . ? C28 C25 C24 110.9(9) . . ? C26 C25 C24 112.0(10) . . ? C28 C25 C27 108.0(10) . . ? C26 C25 C27 111.0(10) . . ? C24 C25 C27 105.7(9) . . ? C24 C29 C16 123.2(9) . . ? C43 C30 C31 118.2(9) . . ? C43 C30 C1 119.9(8) . . ? C31 C30 C1 121.9(8) . . ? O3 C31 C30 118.2(8) . . ? O3 C31 C32 120.8(9) . . ? C30 C31 C32 120.5(9) . . ? C37 C32 C31 117.6(9) . . ? C37 C32 C33 119.5(10) . . ? C31 C32 C33 123.0(9) . . ? C36 C33 C34 107.2(10) . . ? C36 C33 C32 113.4(9) . . ? C34 C33 C32 110.2(9) . . ? C36 C33 C35 107.2(9) . . ? C34 C33 C35 108.3(9) . . ? C32 C33 C35 110.3(9) . . ? C32 C37 C38 122.6(10) . . ? C43 C38 C37 119.1(10) . . ? C43 C38 C39 120.7(10) . . ? C37 C38 C39 120.1(11) . . ? C41' C39 C40 138.2(18) . . ? C41' C39 C40' 114.3(18) . . ? C40 C39 C40' 53.6(14) . . ? C41' C39 C38 107.6(15) . . ? C40 C39 C38 114.1(14) . . ? C40' C39 C38 110.4(14) . . ? C41' C39 C42' 112.5(17) . . ? C40 C39 C42' 55.5(14) . . ? C40' C39 C42' 108.7(17) . . ? C38 C39 C42' 102.7(13) . . ? C41' C39 C42 45.0(12) . . ? C40 C39 C42 111.3(16) . . ? C40' C39 C42 135.9(16) . . ? C38 C39 C42 113.2(12) . . ? C42' C39 C42 67.8(13) . . ? C41' C39 C41 63.2(15) . . ? C40 C39 C41 105.3(16) . . ? C40' C39 C41 55.0(14) . . ? C38 C39 C41 108.0(12) . . ? C42' C39 C41 148.7(16) . . ? C42 C39 C41 104.0(14) . . ? C38 C43 C30 121.6(10) . . ? O1 C44 C45 108.2(8) . . ? N1 C45 C44 112.2(8) . . ? O4 C46 N1 119.2(9) . . ? O4 C46 C47 120.5(8) . . ? N1 C46 C47 120.3(9) . . ? C46 C47 P1 112.8(7) . . ? C49 C48 C53 117.8(10) . . ? C49 C48 P1 118.9(9) . . ? C53 C48 P1 123.1(8) . . ? C48 C49 C50 121.7(12) . . ? C51 C50 C49 119.0(12) . . ? C50 C51 C52 120.9(12) . . ? C51 C52 C53 120.4(12) . . ? C52 C53 C48 120.2(11) . . ? C59 C54 C55 119.0(10) . . ? C59 C54 P1 120.5(8) . . ? C55 C54 P1 120.5(9) . . ? C54 C55 C56 120.7(11) . . ? C57 C56 C55 117.8(12) . . ? C58 C57 C56 121.6(12) . . ? C57 C58 C59 119.1(13) . . ? C54 C59 C58 121.7(12) . . ? O2 C60 C61 108.5(8) . . ? N2 C61 C60 114.0(8) . . ? O6 C62 N2 124.5(9) . . ? O6 C62 C63 119.9(9) . . ? N2 C62 C63 115.5(8) . . ? C62 C63 P2 112.3(7) . . ? C69 C64 C65' 96(2) . . ? C69 C64 C65 122(2) . . ? C65' C64 C65 48.1(11) . . ? C69 C64 C69' 37.4(15) . . ? C65' C64 C69' 116.9(15) . . ? C65 C64 C69' 111.8(14) . . ? C69 C64 P2 121.4(18) . . ? C65' C64 P2 118.4(12) . . ? C65 C64 P2 116.0(12) . . ? C69' C64 P2 122.4(10) . . ? C64 C65 C66 113(2) . . ? C67 C66 C65 121(2) . . ? C64 C65' C66' 121(2) . . ? C67 C66' C65' 122(3) . . ? C68 C67 C66' 99(2) . . ? C68 C67 C68' 40.5(16) . . ? C66' C67 C68' 119.7(19) . . ? C68 C67 C66 120(2) . . ? C66' C67 C66 46.7(14) . . ? C68' C67 C66 106.8(16) . . ? C67 C68 C69 119(3) . . ? C64 C69 C68 125(3) . . ? C69' C68' C67 120.1(19) . . ? C68' C69' C64 118.0(17) . . ? C71 C70 C75 118.8(12) . . ? C71 C70 P2 121.0(9) . . ? C75 C70 P2 120.2(9) . . ? C70 C71 C72 121.1(14) . . ? C71 C72 C73 116.7(16) . . ? C74 C73 C72 122.0(16) . . ? C73 C74 C75 119.5(14) . . ? C74 C75 C70 121.9(13) . . ? O3 C76 C77 107.3(8) . . ? N3 C77 C76 112.1(9) . . ? O8 C78 N3 121.7(9) . . ? O8 C78 C79 119.9(9) . . ? N3 C78 C79 118.4(9) . . ? C78 C79 P3 112.2(8) . . ? C81 C80 C85 119.3(12) . . ? C81 C80 P3 117.8(9) . . ? C85 C80 P3 122.8(12) . . ? C82 C81 C80 121.4(13) . . ? C81 C82 C83 119.2(16) . . ? C84 C83 C82 119.4(16) . . ? C83 C84 C85 121.8(14) . . ? C84 C85 C80 118.8(14) . . ? C87 C86 C91 120.0 . . ? C87 C86 P3 120.7(7) . . ? C91 C86 P3 118.8(7) . . ? C86 C87 C88 120.0 . . ? C87 C88 C89 120.0 . . ? C90 C89 C88 120.0 . . ? C91 C90 C89 120.0 . . ? C90 C91 C86 120.0 . . ? O12 N4 O11 121.9(10) . . ? O12 N4 O10 122.8(10) . . ? O11 N4 O10 115.3(9) . . ? O12 N4 Th1 169.6(7) . . ? O11 N4 Th1 55.0(5) . . ? O10 N4 Th1 61.2(5) . . ? N4 O10 Th1 94.0(6) . . ? N4 O11 Th1 100.7(6) . . ? O15 N5 O14 122.3(14) . . ? O15 N5 O13 120.5(16) . . ? O14 N5 O13 117.2(11) . . ? N5 O13 Th1 97.0(8) . . ? N5 O14 Th1 96.8(7) . . ? O17 N6 O16 120.5(9) . . ? O17 N6 O18 120.8(9) . . ? O16 N6 O18 118.7(8) . . ? O19 N7 O21 136(2) . . ? O19 N7 O20 113.6(19) . . ? O21 N7 O20 109.9(18) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.996 _refine_diff_density_min -1.294 _refine_diff_density_rms 0.138 #===END