# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_a _database_code_depnum_ccdc_archive 'CCDC 856748' #TrackingRef 'web_deposit_cif_file_0_DrAndreiV.Churakov_1322932073.La.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C102 H168 La2 O24 P6' _chemical_formula_sum 'C102 H168 La2 O24 P6' _chemical_formula_weight 2242.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.344(3) _cell_length_b 15.019(3) _cell_length_c 15.110(3) _cell_angle_alpha 65.955(3) _cell_angle_beta 74.968(3) _cell_angle_gamma 81.995(3) _cell_volume 2868.9(9) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4053 _cell_measurement_theta_min 2.966 _cell_measurement_theta_max 30.522 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.882 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9169 _exptl_absorpt_correction_T_max 0.9912 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _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 'Bruker SMART APEX II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 24590 _diffrn_reflns_av_R_equivalents 0.0587 _diffrn_reflns_av_sigmaI/netI 0.0890 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10682 _reflns_number_gt 7945 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10682 _refine_ls_number_parameters 628 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.0857 _refine_ls_wR_factor_gt 0.0805 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.952 _refine_ls_shift/su_max 0.003 _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 La1 La 1.045987(16) 0.135492(17) 0.898683(17) 0.02004(7) Uani 1 1 d . . . P1 P 0.86237(7) 0.13223(7) 1.07104(8) 0.0280(2) Uani 1 1 d . . . P2 P 0.86559(8) 0.00092(8) 0.87202(8) 0.0322(3) Uani 1 1 d . . . P3 P 1.13519(7) 0.32772(7) 0.74809(8) 0.0269(2) Uani 1 1 d . . . O11 O 0.85467(19) 0.1381(2) 1.1733(2) 0.0365(7) Uani 1 1 d . . . O12 O 0.75308(17) 0.13424(18) 1.06604(18) 0.0277(6) Uani 1 1 d . . . O13 O 0.91624(19) 0.21425(19) 0.9854(2) 0.0361(7) Uani 1 1 d . . . O14 O 0.90874(18) 0.03628(18) 1.06944(18) 0.0308(6) Uani 1 1 d . . . O21 O 0.75438(19) 0.0266(2) 0.8829(2) 0.0383(7) Uani 1 1 d . . . O22 O 0.89796(18) -0.03929(19) 0.78483(19) 0.0330(7) Uani 1 1 d . . . O23 O 0.92122(19) 0.08925(19) 0.84556(19) 0.0360(7) Uani 1 1 d . . . O24 O 0.8781(2) -0.0835(2) 0.96433(19) 0.0394(7) Uani 1 1 d . . . O31 O 1.0913(2) 0.43501(19) 0.7234(2) 0.0389(7) Uani 1 1 d . . . O32 O 1.23758(18) 0.34549(18) 0.67395(18) 0.0297(6) Uani 1 1 d . . . O33 O 1.14443(19) 0.27717(19) 0.85376(18) 0.0333(7) Uani 1 1 d . . . O34 O 1.07795(18) 0.26434(18) 0.72768(18) 0.0285(6) Uani 1 1 d . . . C11 C 0.6742(3) 0.1609(3) 1.1301(3) 0.0261(9) Uani 1 1 d . . . C12 C 0.6448(3) 0.2600(3) 1.1047(3) 0.0311(10) Uani 1 1 d . . . C13 C 0.5789(3) 0.2811(3) 1.1804(3) 0.0367(11) Uani 1 1 d . . . H13 H 0.5589 0.3474 1.1676 0.044 Uiso 1 1 calc R . . C14 C 0.5413(3) 0.2121(3) 1.2720(3) 0.0318(10) Uani 1 1 d . . . C15 C 0.5631(3) 0.1149(3) 1.2868(3) 0.0306(10) Uani 1 1 d . . . H15 H 0.5326 0.0661 1.3475 0.037 Uiso 1 1 calc R . . C16 C 0.6281(3) 0.0856(3) 1.2160(3) 0.0267(9) Uani 1 1 d . . . C17 C 0.6756(3) 0.3435(3) 1.0024(3) 0.0449(12) Uani 1 1 d . . . C18 C 0.6425(3) -0.0240(3) 1.2343(3) 0.0334(10) Uani 1 1 d . . . C19 C 0.4757(3) 0.2393(4) 1.3534(3) 0.0488(13) Uani 1 1 d . . . H19A H 0.4412 0.3014 1.3239 0.073 Uiso 1 1 calc R . . H19B H 0.5142 0.2460 1.3951 0.073 Uiso 1 1 calc R . . H19C H 0.4289 0.1883 1.3941 0.073 Uiso 1 1 calc R . . C21 C 0.8476(3) -0.0237(3) 0.7103(3) 0.0289(9) Uani 1 1 d . . . C22 C 0.7766(3) -0.0903(3) 0.7316(3) 0.0317(10) Uani 1 1 d . . . C23 C 0.7209(3) -0.0652(3) 0.6607(3) 0.0355(10) Uani 1 1 d . . . H23 H 0.6695 -0.1057 0.6739 0.043 Uiso 1 1 calc R . . C24 C 0.7371(3) 0.0152(3) 0.5731(3) 0.0373(11) Uani 1 1 d . . . C25 C 0.8148(3) 0.0718(3) 0.5521(3) 0.0393(11) Uani 1 1 d . . . H25 H 0.8285 0.1254 0.4899 0.047 Uiso 1 1 calc R . . C26 C 0.8739(3) 0.0534(3) 0.6187(3) 0.0299(10) Uani 1 1 d . . . C27 C 0.7549(3) -0.1881(3) 0.8227(3) 0.0404(11) Uani 1 1 d . . . C28 C 0.9605(3) 0.1215(3) 0.5833(3) 0.0389(11) Uani 1 1 d . . . C29 C 0.6744(3) 0.0390(4) 0.4989(3) 0.0584(15) Uani 1 1 d . . . H29A H 0.6232 -0.0081 0.5264 0.088 Uiso 1 1 calc R . . H29B H 0.7141 0.0355 0.4369 0.088 Uiso 1 1 calc R . . H29C H 0.6454 0.1049 0.4856 0.088 Uiso 1 1 calc R . . C31 C 1.2805(3) 0.4359(3) 0.6104(3) 0.0306(10) Uani 1 1 d . . . C32 C 1.2691(3) 0.4756(3) 0.5119(3) 0.0339(10) Uani 1 1 d . . . C33 C 1.3019(3) 0.5695(3) 0.4557(3) 0.0477(12) Uani 1 1 d . . . H33 H 1.2924 0.6010 0.3898 0.057 Uiso 1 1 calc R . . C34 C 1.3476(4) 0.6196(3) 0.4907(4) 0.0539(14) Uani 1 1 d . . . C35 C 1.3651(3) 0.5713(3) 0.5843(4) 0.0482(12) Uani 1 1 d . . . H35 H 1.3993 0.6038 0.6077 0.058 Uiso 1 1 calc R . . C36 C 1.3354(3) 0.4775(3) 0.6465(3) 0.0347(10) Uani 1 1 d . . . C37 C 1.2227(3) 0.4244(3) 0.4648(3) 0.0387(11) Uani 1 1 d . . . C38 C 1.3641(3) 0.4293(3) 0.7478(3) 0.0425(11) Uani 1 1 d . . . C39 C 1.3784(4) 0.7235(4) 0.4271(4) 0.0821(19) Uani 1 1 d . . . H39A H 1.4439 0.7302 0.4313 0.123 Uiso 1 1 calc R . . H39B H 1.3338 0.7687 0.4510 0.123 Uiso 1 1 calc R . . H39C H 1.3775 0.7387 0.3578 0.123 Uiso 1 1 calc R . . C41 C 0.5918(4) 0.4182(4) 0.9830(4) 0.0772(18) Uani 1 1 d . . . H41A H 0.5783 0.4492 1.0311 0.116 Uiso 1 1 calc R . . H41B H 0.5343 0.3855 0.9898 0.116 Uiso 1 1 calc R . . H41C H 0.6091 0.4681 0.9155 0.116 Uiso 1 1 calc R . . C42 C 0.7013(4) 0.3087(4) 0.9159(3) 0.0685(17) Uani 1 1 d . . . H42A H 0.6489 0.2702 0.9210 0.103 Uiso 1 1 calc R . . H42B H 0.7612 0.2683 0.9191 0.103 Uiso 1 1 calc R . . H42C H 0.7102 0.3654 0.8525 0.103 Uiso 1 1 calc R . . C43 C 0.7610(4) 0.3963(3) 0.9996(4) 0.0565(14) Uani 1 1 d . . . H43A H 0.7446 0.4185 1.0546 0.085 Uiso 1 1 calc R . . H43B H 0.7752 0.4527 0.9363 0.085 Uiso 1 1 calc R . . H43C H 0.8178 0.3516 1.0060 0.085 Uiso 1 1 calc R . . C44 C 0.6461(4) -0.0393(3) 1.1388(3) 0.0565(14) Uani 1 1 d . . . H44A H 0.7052 -0.0121 1.0895 0.085 Uiso 1 1 calc R . . H44B H 0.5896 -0.0064 1.1120 0.085 Uiso 1 1 calc R . . H44C H 0.6459 -0.1093 1.1541 0.085 Uiso 1 1 calc R . . C45 C 0.7336(3) -0.0693(3) 1.2732(3) 0.0468(12) Uani 1 1 d . . . H45A H 0.7296 -0.0612 1.3352 0.070 Uiso 1 1 calc R . . H45B H 0.7904 -0.0368 1.2236 0.070 Uiso 1 1 calc R . . H45C H 0.7390 -0.1390 1.2856 0.070 Uiso 1 1 calc R . . C46 C 0.5581(3) -0.0819(3) 1.3136(3) 0.0498(13) Uani 1 1 d . . . H46A H 0.5578 -0.0797 1.3777 0.075 Uiso 1 1 calc R . . H46B H 0.5655 -0.1498 1.3195 0.075 Uiso 1 1 calc R . . H46C H 0.4972 -0.0531 1.2944 0.075 Uiso 1 1 calc R . . C47 C 0.9033(3) 0.2038(3) 1.1923(4) 0.0511(13) Uani 1 1 d . . . H47A H 0.9321 0.2562 1.1288 0.061 Uiso 1 1 calc R . . H47B H 0.9559 0.1681 1.2260 0.061 Uiso 1 1 calc R . . C48 C 0.8323(4) 0.2470(4) 1.2564(4) 0.0644(15) Uani 1 1 d . . . H48A H 0.8650 0.2918 1.2699 0.097 Uiso 1 1 calc R . . H48B H 0.8044 0.1949 1.3193 0.097 Uiso 1 1 calc R . . H48C H 0.7809 0.2829 1.2224 0.097 Uiso 1 1 calc R . . C51 C 0.7208(4) -0.2628(4) 0.7923(4) 0.0724(17) Uani 1 1 d . . . H51A H 0.6568 -0.2421 0.7776 0.109 Uiso 1 1 calc R . . H51B H 0.7175 -0.3271 0.8470 0.109 Uiso 1 1 calc R . . H51C H 0.7667 -0.2665 0.7331 0.109 Uiso 1 1 calc R . . C52 C 0.6753(4) -0.1748(4) 0.9071(4) 0.0742(18) Uani 1 1 d . . . H52A H 0.6980 -0.1332 0.9326 0.111 Uiso 1 1 calc R . . H52B H 0.6595 -0.2386 0.9609 0.111 Uiso 1 1 calc R . . H52C H 0.6175 -0.1440 0.8818 0.111 Uiso 1 1 calc R . . C53 C 0.8446(4) -0.2378(3) 0.8638(4) 0.0570(14) Uani 1 1 d . . . H53A H 0.8636 -0.2001 0.8958 0.085 Uiso 1 1 calc R . . H53B H 0.8978 -0.2408 0.8092 0.085 Uiso 1 1 calc R . . H53C H 0.8295 -0.3040 0.9127 0.085 Uiso 1 1 calc R . . C54 C 0.9272(3) 0.2125(3) 0.6064(3) 0.0473(12) Uani 1 1 d . . . H54A H 0.9818 0.2549 0.5840 0.071 Uiso 1 1 calc R . . H54B H 0.9024 0.1931 0.6783 0.071 Uiso 1 1 calc R . . H54C H 0.8759 0.2477 0.5718 0.071 Uiso 1 1 calc R . . C55 C 0.9995(3) 0.1554(4) 0.4702(3) 0.0518(13) Uani 1 1 d . . . H55A H 1.0587 0.1910 0.4506 0.078 Uiso 1 1 calc R . . H55B H 0.9509 0.1983 0.4359 0.078 Uiso 1 1 calc R . . H55C H 1.0137 0.0984 0.4522 0.078 Uiso 1 1 calc R . . C56 C 1.0475(3) 0.0697(3) 0.6289(3) 0.0465(12) Uani 1 1 d . . . H56A H 1.1024 0.1127 0.5978 0.070 Uiso 1 1 calc R . . H56B H 1.0650 0.0093 0.6173 0.070 Uiso 1 1 calc R . . H56C H 1.0303 0.0543 0.7006 0.070 Uiso 1 1 calc R . . C57 C 0.7119(3) 0.1157(4) 0.8213(3) 0.0518(13) Uani 1 1 d . . . H57A H 0.7240 0.1188 0.7526 0.062 Uiso 1 1 calc R . . H57B H 0.7409 0.1728 0.8193 0.062 Uiso 1 1 calc R . . C58 C 0.6059(4) 0.1168(4) 0.8647(4) 0.0761(18) Uani 1 1 d . . . H58A H 0.5753 0.1763 0.8233 0.114 Uiso 1 1 calc R . . H58B H 0.5946 0.1151 0.9322 0.114 Uiso 1 1 calc R . . H58C H 0.5780 0.0596 0.8671 0.114 Uiso 1 1 calc R . . C61 C 1.2580(4) 0.4673(4) 0.3505(3) 0.0566(14) Uani 1 1 d . . . H61A H 1.3288 0.4645 0.3329 0.085 Uiso 1 1 calc R . . H61B H 1.2344 0.5354 0.3235 0.085 Uiso 1 1 calc R . . H61C H 1.2333 0.4294 0.3225 0.085 Uiso 1 1 calc R . . C62 C 1.1126(3) 0.4419(4) 0.4867(3) 0.0518(13) Uani 1 1 d . . . H62A H 1.0862 0.4118 0.5586 0.078 Uiso 1 1 calc R . . H62B H 1.0841 0.4128 0.4528 0.078 Uiso 1 1 calc R . . H62C H 1.0970 0.5122 0.4629 0.078 Uiso 1 1 calc R . . C63 C 1.2480(3) 0.3140(3) 0.4999(3) 0.0467(12) Uani 1 1 d . . . H63A H 1.2114 0.2806 0.5680 0.070 Uiso 1 1 calc R . . H63B H 1.3173 0.3028 0.4979 0.070 Uiso 1 1 calc R . . H63C H 1.2313 0.2884 0.4559 0.070 Uiso 1 1 calc R . . C64 C 1.4598(4) 0.4695(4) 0.7413(4) 0.0757(18) Uani 1 1 d . . . H64A H 1.5060 0.4713 0.6801 0.114 Uiso 1 1 calc R . . H64B H 1.4863 0.4271 0.7989 0.114 Uiso 1 1 calc R . . H64C H 1.4480 0.5355 0.7407 0.114 Uiso 1 1 calc R . . C65 C 1.2865(4) 0.4520(3) 0.8273(3) 0.0524(13) Uani 1 1 d . . . H65A H 1.2255 0.4244 0.8348 0.079 Uiso 1 1 calc R . . H65B H 1.2775 0.5228 0.8074 0.079 Uiso 1 1 calc R . . H65C H 1.3066 0.4233 0.8908 0.079 Uiso 1 1 calc R . . C66 C 1.3825(3) 0.3181(3) 0.7811(4) 0.0519(13) Uani 1 1 d . . . H66A H 1.3207 0.2862 0.8039 0.078 Uiso 1 1 calc R . . H66B H 1.4164 0.2942 0.8356 0.078 Uiso 1 1 calc R . . H66C H 1.4222 0.3033 0.7250 0.078 Uiso 1 1 calc R . . C67 C 0.9950(3) 0.4501(3) 0.7741(4) 0.0589(15) Uani 1 1 d . . . H67A H 0.9850 0.4076 0.8457 0.071 Uiso 1 1 calc R . . H67B H 0.9476 0.4336 0.7463 0.071 Uiso 1 1 calc R . . C68 C 0.9812(4) 0.5524(4) 0.7615(5) 0.097(2) Uani 1 1 d . . . H68A H 0.9122 0.5675 0.7819 0.145 Uiso 1 1 calc R . . H68B H 1.0052 0.5940 0.6915 0.145 Uiso 1 1 calc R . . H68C H 1.0167 0.5642 0.8027 0.145 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 La1 0.01941(12) 0.01946(12) 0.02032(12) -0.00605(9) -0.00486(9) -0.00228(8) P1 0.0248(6) 0.0253(6) 0.0322(6) -0.0135(5) 0.0003(5) -0.0007(5) P2 0.0350(7) 0.0351(6) 0.0282(6) -0.0062(5) -0.0158(5) -0.0096(5) P3 0.0277(6) 0.0217(6) 0.0267(6) -0.0054(5) -0.0036(5) -0.0043(5) O11 0.0349(17) 0.0390(17) 0.0406(17) -0.0210(15) -0.0029(14) -0.0097(13) O12 0.0231(15) 0.0315(16) 0.0283(15) -0.0154(13) -0.0001(12) 0.0013(12) O13 0.0313(16) 0.0245(15) 0.0438(17) -0.0106(14) 0.0011(13) 0.0004(13) O14 0.0266(15) 0.0311(16) 0.0320(16) -0.0132(13) -0.0015(12) 0.0003(12) O21 0.0340(17) 0.0483(19) 0.0354(17) -0.0149(15) -0.0132(14) -0.0047(14) O22 0.0306(16) 0.0372(17) 0.0321(16) -0.0086(14) -0.0140(13) -0.0067(13) O23 0.0394(17) 0.0343(17) 0.0340(16) -0.0028(14) -0.0205(14) -0.0101(13) O24 0.0495(19) 0.0376(17) 0.0331(16) -0.0024(14) -0.0227(14) -0.0181(14) O31 0.0347(17) 0.0247(16) 0.0428(18) -0.0085(14) 0.0076(14) -0.0010(13) O32 0.0279(15) 0.0263(15) 0.0306(15) -0.0072(13) -0.0018(12) -0.0085(12) O33 0.0404(17) 0.0341(16) 0.0266(15) -0.0093(13) -0.0067(13) -0.0141(13) O34 0.0295(15) 0.0297(15) 0.0245(14) -0.0058(12) -0.0073(12) -0.0080(12) C11 0.022(2) 0.031(2) 0.026(2) -0.0128(19) -0.0050(18) 0.0013(18) C12 0.030(2) 0.029(2) 0.037(2) -0.015(2) -0.012(2) 0.0072(19) C13 0.032(2) 0.034(3) 0.050(3) -0.023(2) -0.015(2) 0.013(2) C14 0.018(2) 0.046(3) 0.037(3) -0.025(2) -0.0031(19) 0.0005(19) C15 0.022(2) 0.040(3) 0.030(2) -0.014(2) -0.0036(18) -0.0065(19) C16 0.018(2) 0.034(2) 0.032(2) -0.015(2) -0.0066(18) -0.0022(18) C17 0.057(3) 0.030(3) 0.036(3) -0.004(2) -0.011(2) 0.008(2) C18 0.036(3) 0.031(2) 0.033(2) -0.014(2) -0.003(2) -0.003(2) C19 0.039(3) 0.064(3) 0.052(3) -0.039(3) 0.004(2) -0.005(2) C21 0.029(2) 0.036(2) 0.028(2) -0.015(2) -0.0120(19) -0.0014(19) C22 0.028(2) 0.036(2) 0.036(2) -0.017(2) -0.0072(19) -0.0032(19) C23 0.030(2) 0.049(3) 0.034(3) -0.020(2) -0.007(2) -0.011(2) C24 0.029(2) 0.058(3) 0.030(2) -0.022(2) -0.007(2) -0.005(2) C25 0.041(3) 0.044(3) 0.028(2) -0.006(2) -0.009(2) -0.007(2) C26 0.028(2) 0.036(2) 0.025(2) -0.011(2) -0.0066(18) 0.0000(19) C27 0.041(3) 0.031(3) 0.051(3) -0.012(2) -0.016(2) -0.011(2) C28 0.034(3) 0.042(3) 0.032(2) -0.003(2) -0.008(2) -0.011(2) C29 0.047(3) 0.093(4) 0.037(3) -0.016(3) -0.016(2) -0.021(3) C31 0.023(2) 0.027(2) 0.035(2) -0.009(2) 0.0041(19) -0.0064(18) C32 0.028(2) 0.033(2) 0.029(2) -0.008(2) 0.0074(19) -0.0081(19) C33 0.052(3) 0.044(3) 0.033(3) -0.001(2) -0.004(2) -0.011(2) C34 0.056(3) 0.040(3) 0.055(3) -0.013(3) 0.006(3) -0.020(2) C35 0.053(3) 0.041(3) 0.053(3) -0.019(3) -0.005(3) -0.019(2) C36 0.031(2) 0.033(2) 0.040(3) -0.015(2) -0.001(2) -0.008(2) C37 0.033(3) 0.048(3) 0.028(2) -0.010(2) 0.0006(19) -0.009(2) C38 0.042(3) 0.036(3) 0.055(3) -0.020(2) -0.014(2) -0.007(2) C39 0.108(5) 0.048(4) 0.072(4) -0.001(3) -0.006(4) -0.043(3) C41 0.085(4) 0.060(4) 0.061(4) -0.002(3) -0.026(3) 0.032(3) C42 0.114(5) 0.052(3) 0.030(3) -0.008(3) -0.021(3) 0.012(3) C43 0.070(4) 0.031(3) 0.048(3) -0.009(2) 0.009(3) -0.002(3) C44 0.084(4) 0.042(3) 0.053(3) -0.024(3) -0.009(3) -0.021(3) C45 0.047(3) 0.027(2) 0.052(3) -0.005(2) -0.004(2) 0.001(2) C46 0.045(3) 0.039(3) 0.059(3) -0.018(3) 0.004(2) -0.015(2) C47 0.051(3) 0.051(3) 0.063(3) -0.028(3) -0.016(3) -0.014(2) C48 0.096(4) 0.055(3) 0.056(3) -0.035(3) -0.019(3) 0.000(3) C51 0.087(4) 0.044(3) 0.096(5) -0.016(3) -0.045(4) -0.020(3) C52 0.073(4) 0.053(4) 0.059(4) 0.002(3) 0.013(3) -0.016(3) C53 0.065(4) 0.035(3) 0.070(4) -0.005(3) -0.037(3) -0.006(2) C54 0.049(3) 0.044(3) 0.049(3) -0.009(2) -0.020(2) -0.013(2) C55 0.042(3) 0.066(3) 0.038(3) -0.009(3) -0.002(2) -0.023(3) C56 0.030(3) 0.056(3) 0.048(3) -0.010(2) -0.007(2) -0.019(2) C57 0.058(3) 0.061(3) 0.041(3) -0.022(3) -0.021(3) 0.012(3) C58 0.043(3) 0.098(5) 0.086(4) -0.034(4) -0.024(3) 0.013(3) C61 0.061(3) 0.070(4) 0.033(3) -0.012(3) -0.002(2) -0.022(3) C62 0.042(3) 0.066(3) 0.041(3) -0.010(3) -0.011(2) -0.008(3) C63 0.058(3) 0.050(3) 0.042(3) -0.026(2) -0.014(2) -0.003(2) C64 0.063(4) 0.080(4) 0.098(5) -0.028(4) -0.035(3) -0.032(3) C65 0.076(4) 0.044(3) 0.043(3) -0.019(2) -0.016(3) -0.009(3) C66 0.046(3) 0.051(3) 0.066(3) -0.024(3) -0.027(3) 0.003(2) C67 0.046(3) 0.036(3) 0.074(4) -0.016(3) 0.009(3) 0.004(2) C68 0.072(4) 0.066(4) 0.138(6) -0.048(4) 0.010(4) 0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O24 2.386(3) 2_757 ? La1 O23 2.424(2) . ? La1 O13 2.442(3) . ? La1 O14 2.448(3) 2_757 ? La1 O33 2.479(3) . ? La1 O34 2.488(2) . ? La1 O14 2.793(2) . ? La1 La1 4.1139(8) 2_757 ? P1 O13 1.496(3) . ? P1 O14 1.508(3) . ? P1 O11 1.557(3) . ? P1 O12 1.584(3) . ? P2 O24 1.487(3) . ? P2 O23 1.501(3) . ? P2 O21 1.570(3) . ? P2 O22 1.603(3) . ? P3 O33 1.496(3) . ? P3 O34 1.504(3) . ? P3 O31 1.576(3) . ? P3 O32 1.580(3) . ? O11 C47 1.439(5) . ? O12 C11 1.414(4) . ? O14 La1 2.448(3) 2_757 ? O21 C57 1.442(5) . ? O22 C21 1.417(4) . ? O24 La1 2.386(3) 2_757 ? O31 C67 1.432(5) . ? O32 C31 1.418(4) . ? C11 C16 1.404(5) . ? C11 C12 1.408(5) . ? C12 C13 1.398(5) . ? C12 C17 1.542(6) . ? C13 C14 1.371(6) . ? C13 H13 0.9500 . ? C14 C15 1.387(5) . ? C14 C19 1.506(5) . ? C15 C16 1.399(5) . ? C15 H15 0.9500 . ? C16 C18 1.547(5) . ? C17 C41 1.526(6) . ? C17 C43 1.532(7) . ? C17 C42 1.540(6) . ? C18 C45 1.530(6) . ? C18 C46 1.532(5) . ? C18 C44 1.538(6) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C21 C26 1.394(5) . ? C21 C22 1.411(5) . ? C22 C23 1.399(5) . ? C22 C27 1.551(6) . ? C23 C24 1.371(6) . ? C23 H23 0.9500 . ? C24 C25 1.389(6) . ? C24 C29 1.517(6) . ? C25 C26 1.398(5) . ? C25 H25 0.9500 . ? C26 C28 1.562(5) . ? C27 C52 1.536(6) . ? C27 C53 1.539(6) . ? C27 C51 1.548(6) . ? C28 C54 1.529(6) . ? C28 C55 1.538(6) . ? C28 C56 1.541(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C31 C36 1.395(5) . ? C31 C32 1.405(5) . ? C32 C33 1.390(6) . ? C32 C37 1.541(6) . ? C33 C34 1.384(6) . ? C33 H33 0.9500 . ? C34 C35 1.374(7) . ? C34 C39 1.518(6) . ? C35 C36 1.388(6) . ? C35 H35 0.9500 . ? C36 C38 1.542(6) . ? C37 C62 1.535(6) . ? C37 C63 1.543(6) . ? C37 C61 1.544(6) . ? C38 C65 1.528(6) . ? C38 C64 1.539(6) . ? C38 C66 1.540(6) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.488(6) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.493(6) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 C68 1.459(7) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? 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 O24 La1 O23 141.02(9) 2_757 . ? O24 La1 O13 89.07(10) 2_757 . ? O23 La1 O13 86.46(9) . . ? O24 La1 O14 76.01(9) 2_757 2_757 ? O23 La1 O14 78.61(9) . 2_757 ? O13 La1 O14 132.14(8) . 2_757 ? O24 La1 O33 78.13(9) 2_757 . ? O23 La1 O33 140.10(9) . . ? O13 La1 O33 87.19(9) . . ? O14 La1 O33 131.51(9) 2_757 . ? O24 La1 O34 134.29(8) 2_757 . ? O23 La1 O34 84.43(8) . . ? O13 La1 O34 101.24(9) . . ? O14 La1 O34 121.82(8) 2_757 . ? O33 La1 O34 58.38(8) . . ? O24 La1 O14 73.05(8) 2_757 . ? O23 La1 O14 72.66(8) . . ? O13 La1 O14 55.36(8) . . ? O14 La1 O14 76.77(9) 2_757 . ? O33 La1 O14 132.05(8) . . ? O34 La1 O14 147.32(8) . . ? O24 La1 La1 70.02(6) 2_757 2_757 ? O23 La1 La1 71.34(6) . 2_757 ? O13 La1 La1 90.76(6) . 2_757 ? O14 La1 La1 41.37(6) 2_757 2_757 ? O33 La1 La1 148.11(6) . 2_757 ? O34 La1 La1 152.28(6) . 2_757 ? O14 La1 La1 35.40(5) . 2_757 ? O13 P1 O14 109.45(15) . . ? O13 P1 O11 113.01(16) . . ? O14 P1 O11 111.18(15) . . ? O13 P1 O12 111.92(15) . . ? O14 P1 O12 107.70(14) . . ? O11 P1 O12 103.36(14) . . ? O24 P2 O23 115.86(15) . . ? O24 P2 O21 107.21(16) . . ? O23 P2 O21 111.20(16) . . ? O24 P2 O22 105.61(16) . . ? O23 P2 O22 109.92(15) . . ? O21 P2 O22 106.49(14) . . ? O33 P3 O34 107.69(15) . . ? O33 P3 O31 112.86(16) . . ? O34 P3 O31 113.11(16) . . ? O33 P3 O32 111.28(15) . . ? O34 P3 O32 110.13(14) . . ? O31 P3 O32 101.75(14) . . ? C47 O11 P1 127.1(3) . . ? C11 O12 P1 123.9(2) . . ? P1 O13 La1 105.04(13) . . ? P1 O14 La1 166.63(16) . 2_757 ? P1 O14 La1 90.14(12) . . ? La1 O14 La1 103.23(8) 2_757 . ? C57 O21 P2 125.3(3) . . ? C21 O22 P2 126.4(2) . . ? P2 O23 La1 138.79(15) . . ? P2 O24 La1 143.11(16) . 2_757 ? C67 O31 P3 119.1(3) . . ? C31 O32 P3 127.9(2) . . ? P3 O33 La1 97.22(12) . . ? P3 O34 La1 96.62(12) . . ? C16 C11 C12 123.3(4) . . ? C16 C11 O12 117.3(3) . . ? C12 C11 O12 119.3(3) . . ? C13 C12 C11 115.0(4) . . ? C13 C12 C17 118.8(4) . . ? C11 C12 C17 126.2(4) . . ? C14 C13 C12 124.1(4) . . ? C14 C13 H13 118.0 . . ? C12 C13 H13 118.0 . . ? C13 C14 C15 117.6(4) . . ? C13 C14 C19 122.0(4) . . ? C15 C14 C19 120.4(4) . . ? C14 C15 C16 122.7(4) . . ? C14 C15 H15 118.6 . . ? C16 C15 H15 118.6 . . ? C15 C16 C11 115.9(4) . . ? C15 C16 C18 119.7(3) . . ? C11 C16 C18 124.4(3) . . ? C41 C17 C43 107.5(4) . . ? C41 C17 C42 106.3(4) . . ? C43 C17 C42 109.5(4) . . ? C41 C17 C12 109.4(4) . . ? C43 C17 C12 111.0(4) . . ? C42 C17 C12 112.9(4) . . ? C45 C18 C46 106.0(4) . . ? C45 C18 C44 110.0(4) . . ? C46 C18 C44 107.1(4) . . ? C45 C18 C16 112.1(3) . . ? C46 C18 C16 110.8(3) . . ? C44 C18 C16 110.7(3) . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C26 C21 C22 123.7(4) . . ? C26 C21 O22 118.4(3) . . ? C22 C21 O22 117.8(3) . . ? C23 C22 C21 115.6(4) . . ? C23 C22 C27 116.8(4) . . ? C21 C22 C27 127.7(4) . . ? C24 C23 C22 123.0(4) . . ? C24 C23 H23 118.5 . . ? C22 C23 H23 118.5 . . ? C23 C24 C25 118.3(4) . . ? C23 C24 C29 120.8(4) . . ? C25 C24 C29 120.8(4) . . ? C24 C25 C26 122.8(4) . . ? C24 C25 H25 118.6 . . ? C26 C25 H25 118.6 . . ? C21 C26 C25 115.7(4) . . ? C21 C26 C28 127.3(3) . . ? C25 C26 C28 117.0(3) . . ? C52 C27 C53 108.9(4) . . ? C52 C27 C51 108.0(4) . . ? C53 C27 C51 104.6(4) . . ? C52 C27 C22 111.7(4) . . ? C53 C27 C22 113.1(3) . . ? C51 C27 C22 110.1(4) . . ? C54 C28 C55 107.7(4) . . ? C54 C28 C56 110.6(4) . . ? C55 C28 C56 105.1(4) . . ? C54 C28 C26 109.9(3) . . ? C55 C28 C26 110.5(3) . . ? C56 C28 C26 112.8(3) . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C36 C31 C32 123.8(4) . . ? C36 C31 O32 119.1(4) . . ? C32 C31 O32 117.0(3) . . ? C33 C32 C31 115.0(4) . . ? C33 C32 C37 119.6(4) . . ? C31 C32 C37 125.4(4) . . ? C34 C33 C32 123.5(4) . . ? C34 C33 H33 118.2 . . ? C32 C33 H33 118.2 . . ? C35 C34 C33 117.5(4) . . ? C35 C34 C39 121.4(5) . . ? C33 C34 C39 121.0(5) . . ? C34 C35 C36 123.5(4) . . ? C34 C35 H35 118.3 . . ? C36 C35 H35 118.3 . . ? C35 C36 C31 115.6(4) . . ? C35 C36 C38 118.5(4) . . ? C31 C36 C38 125.9(4) . . ? C62 C37 C32 110.1(4) . . ? C62 C37 C63 110.0(4) . . ? C32 C37 C63 113.0(3) . . ? C62 C37 C61 106.6(4) . . ? C32 C37 C61 110.7(3) . . ? C63 C37 C61 106.4(4) . . ? C65 C38 C64 108.1(4) . . ? C65 C38 C66 109.8(4) . . ? C64 C38 C66 105.4(4) . . ? C65 C38 C36 110.1(4) . . ? C64 C38 C36 110.0(4) . . ? C66 C38 C36 113.2(4) . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C17 C41 H41A 109.5 . . ? C17 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C17 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C17 C42 H42A 109.5 . . ? C17 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C17 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C17 C43 H43A 109.5 . . ? C17 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C17 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C18 C44 H44A 109.5 . . ? C18 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C18 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C18 C45 H45A 109.5 . . ? C18 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C18 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C18 C46 H46A 109.5 . . ? C18 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C18 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O11 C47 C48 109.0(4) . . ? O11 C47 H47A 109.9 . . ? C48 C47 H47A 109.9 . . ? O11 C47 H47B 109.9 . . ? C48 C47 H47B 109.9 . . ? H47A C47 H47B 108.3 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C27 C51 H51A 109.5 . . ? C27 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C27 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C27 C52 H52A 109.5 . . ? C27 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C27 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C27 C53 H53A 109.5 . . ? C27 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C27 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C28 C54 H54A 109.5 . . ? C28 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C28 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C28 C55 H55A 109.5 . . ? C28 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C28 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C28 C56 H56A 109.5 . . ? C28 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C28 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O21 C57 C58 108.1(4) . . ? O21 C57 H57A 110.1 . . ? C58 C57 H57A 110.1 . . ? O21 C57 H57B 110.1 . . ? C58 C57 H57B 110.1 . . ? H57A C57 H57B 108.4 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C37 C61 H61A 109.5 . . ? C37 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C37 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C37 C62 H62A 109.5 . . ? C37 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C37 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C37 C63 H63A 109.5 . . ? C37 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C37 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C38 C64 H64A 109.5 . . ? C38 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C38 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C38 C65 H65A 109.5 . . ? C38 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C38 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C38 C66 H66A 109.5 . . ? C38 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C38 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? O31 C67 C68 108.6(4) . . ? O31 C67 H67A 110.0 . . ? C68 C67 H67A 110.0 . . ? O31 C67 H67B 110.0 . . ? C68 C67 H67B 110.0 . . ? H67A C67 H67B 108.4 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.968 _refine_diff_density_min -0.801 _refine_diff_density_rms 0.090 data_c _database_code_depnum_ccdc_archive 'CCDC 856749' #TrackingRef 'web_deposit_cif_file_1_DrAndreiV.Churakov_1322932073.Nd.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C102 H168 Nd2 O24 P6' _chemical_formula_sum 'C102 H168 Nd2 O24 P6' _chemical_formula_weight 2252.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.273(3) _cell_length_b 14.921(3) _cell_length_c 15.089(3) _cell_angle_alpha 65.781(2) _cell_angle_beta 75.178(3) _cell_angle_gamma 82.048(3) _cell_volume 2831.1(9) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9905 _cell_measurement_theta_min 2.339 _cell_measurement_theta_max 29.566 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1182 _exptl_absorpt_coefficient_mu 1.057 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8165 _exptl_absorpt_correction_T_max 0.9017 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _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 'Bruker SMART APEX II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 29369 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 28.00 _reflns_number_total 13617 _reflns_number_gt 11903 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13617 _refine_ls_number_parameters 628 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0827 _refine_ls_wR_factor_gt 0.0794 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 1.045182(8) 0.133775(8) 0.901922(8) 0.01873(4) Uani 1 1 d . . . P1 P 0.86403(4) 0.13134(4) 1.07062(5) 0.02451(13) Uani 1 1 d . . . P2 P 0.86731(5) 0.00291(5) 0.87178(5) 0.02777(13) Uani 1 1 d . . . P3 P 1.13435(4) 0.32251(4) 0.75172(4) 0.02420(12) Uani 1 1 d . . . O11 O 0.85684(13) 0.13546(13) 1.17381(13) 0.0338(4) Uani 1 1 d . . . O12 O 0.75412(11) 0.13559(12) 1.06447(12) 0.0262(3) Uani 1 1 d . . . O13 O 0.91960(12) 0.21326(12) 0.98473(13) 0.0325(4) Uani 1 1 d . . . O14 O 0.90934(12) 0.03435(12) 1.06851(12) 0.0280(4) Uani 1 1 d . . . O21 O 0.75637(13) 0.03045(14) 0.88230(13) 0.0359(4) Uani 1 1 d . . . O22 O 0.89877(12) -0.03704(12) 0.78476(12) 0.0287(4) Uani 1 1 d . . . O23 O 0.92456(12) 0.09060(12) 0.84539(13) 0.0315(4) Uani 1 1 d . . . O24 O 0.87908(14) -0.08262(13) 0.96496(13) 0.0354(4) Uani 1 1 d . . . O31 O 1.09118(13) 0.43045(12) 0.72568(14) 0.0381(4) Uani 1 1 d . . . O32 O 1.23710(11) 0.33973(11) 0.67819(12) 0.0262(3) Uani 1 1 d . . . O33 O 1.14290(12) 0.27226(12) 0.85853(12) 0.0299(4) Uani 1 1 d . . . O34 O 1.07703(11) 0.25743(12) 0.73263(12) 0.0279(4) Uani 1 1 d . . . C11 C 0.67560(16) 0.16460(17) 1.12751(17) 0.0235(5) Uani 1 1 d . . . C12 C 0.64866(17) 0.26456(18) 1.10142(18) 0.0275(5) Uani 1 1 d . . . C13 C 0.58262(18) 0.28800(19) 1.1760(2) 0.0325(5) Uani 1 1 d . . . H13 H 0.5645 0.3552 1.1627 0.039 Uiso 1 1 calc R . . C14 C 0.54271(17) 0.2182(2) 1.2676(2) 0.0319(6) Uani 1 1 d . . . C15 C 0.56259(17) 0.11981(18) 1.28287(18) 0.0286(5) Uani 1 1 d . . . H15 H 0.5307 0.0712 1.3434 0.034 Uiso 1 1 calc R . . C16 C 0.62724(16) 0.08923(17) 1.21337(18) 0.0252(5) Uani 1 1 d . . . C17 C 0.6826(2) 0.34873(19) 0.9990(2) 0.0396(6) Uani 1 1 d . . . C18 C 0.63850(18) -0.02057(18) 1.23107(19) 0.0305(5) Uani 1 1 d . . . C19 C 0.4765(2) 0.2465(2) 1.3481(2) 0.0448(7) Uani 1 1 d . . . H19A H 0.4457 0.3113 1.3178 0.067 Uiso 1 1 calc R . . H19B H 0.5143 0.2488 1.3929 0.067 Uiso 1 1 calc R . . H19C H 0.4265 0.1977 1.3861 0.067 Uiso 1 1 calc R . . C21 C 0.84849(17) -0.02364(18) 0.71115(17) 0.0257(5) Uani 1 1 d . . . C22 C 0.77671(17) -0.09032(18) 0.73281(18) 0.0287(5) Uani 1 1 d . . . C23 C 0.72172(18) -0.0660(2) 0.66147(19) 0.0337(6) Uani 1 1 d . . . H23 H 0.6706 -0.1073 0.6748 0.040 Uiso 1 1 calc R . . C24 C 0.73744(19) 0.0146(2) 0.57288(19) 0.0365(6) Uani 1 1 d . . . C25 C 0.81534(19) 0.0713(2) 0.55162(19) 0.0352(6) Uani 1 1 d . . . H25 H 0.8292 0.1247 0.4887 0.042 Uiso 1 1 calc R . . C26 C 0.87430(17) 0.05422(18) 0.61751(17) 0.0276(5) Uani 1 1 d . . . C27 C 0.75545(19) -0.18827(19) 0.8252(2) 0.0353(6) Uani 1 1 d . . . C28 C 0.96176(18) 0.1215(2) 0.58288(19) 0.0331(6) Uani 1 1 d . . . C29 C 0.6750(2) 0.0373(3) 0.4982(2) 0.0538(9) Uani 1 1 d . . . H29A H 0.6276 -0.0140 0.5233 0.081 Uiso 1 1 calc R . . H29B H 0.7161 0.0394 0.4346 0.081 Uiso 1 1 calc R . . H29C H 0.6408 0.1011 0.4886 0.081 Uiso 1 1 calc R . . C31 C 1.28051(17) 0.43048(17) 0.61441(18) 0.0274(5) Uani 1 1 d . . . C32 C 1.26900(17) 0.47169(19) 0.51578(18) 0.0307(5) Uani 1 1 d . . . C33 C 1.3029(2) 0.5665(2) 0.4592(2) 0.0435(7) Uani 1 1 d . . . H33 H 1.2939 0.5987 0.3929 0.052 Uiso 1 1 calc R . . C34 C 1.3488(2) 0.6153(2) 0.4953(2) 0.0486(8) Uani 1 1 d . . . C35 C 1.3666(2) 0.5670(2) 0.5887(2) 0.0443(7) Uani 1 1 d . . . H35 H 1.4014 0.5996 0.6120 0.053 Uiso 1 1 calc R . . C36 C 1.33612(18) 0.47152(19) 0.6518(2) 0.0326(5) Uani 1 1 d . . . C37 C 1.22234(19) 0.4212(2) 0.46798(19) 0.0344(6) Uani 1 1 d . . . C38 C 1.3641(2) 0.4226(2) 0.7536(2) 0.0386(6) Uani 1 1 d . . . C39 C 1.3814(3) 0.7199(3) 0.4318(3) 0.0778(13) Uani 1 1 d . . . H39A H 1.4297 0.7350 0.4592 0.117 Uiso 1 1 calc R . . H39B H 1.3254 0.7660 0.4321 0.117 Uiso 1 1 calc R . . H39C H 1.4101 0.7261 0.3633 0.117 Uiso 1 1 calc R . . C41 C 0.5998(3) 0.4269(3) 0.9782(3) 0.0637(10) Uani 1 1 d . . . H41A H 0.5405 0.3954 0.9867 0.096 Uiso 1 1 calc R . . H41B H 0.6174 0.4757 0.9097 0.096 Uiso 1 1 calc R . . H41C H 0.5887 0.4596 1.0248 0.096 Uiso 1 1 calc R . . C42 C 0.7076(3) 0.3147(2) 0.9126(2) 0.0608(10) Uani 1 1 d . . . H42A H 0.6543 0.2770 0.9171 0.091 Uiso 1 1 calc R . . H42B H 0.7672 0.2732 0.9162 0.091 Uiso 1 1 calc R . . H42C H 0.7172 0.3722 0.8493 0.091 Uiso 1 1 calc R . . C43 C 0.7697(2) 0.3991(2) 0.9983(2) 0.0492(8) Uani 1 1 d . . . H43A H 0.7541 0.4193 1.0548 0.074 Uiso 1 1 calc R . . H43B H 0.7846 0.4571 0.9359 0.074 Uiso 1 1 calc R . . H43C H 0.8260 0.3530 1.0038 0.074 Uiso 1 1 calc R . . C44 C 0.6388(3) -0.0344(2) 1.1358(2) 0.0516(8) Uani 1 1 d . . . H44A H 0.6374 -0.1047 1.1507 0.077 Uiso 1 1 calc R . . H44B H 0.6976 -0.0072 1.0855 0.077 Uiso 1 1 calc R . . H44C H 0.5815 -0.0003 1.1103 0.077 Uiso 1 1 calc R . . C45 C 0.7305(2) -0.0691(2) 1.2691(2) 0.0472(7) Uani 1 1 d . . . H45A H 0.7292 -0.0607 1.3305 0.071 Uiso 1 1 calc R . . H45B H 0.7878 -0.0383 1.2184 0.071 Uiso 1 1 calc R . . H45C H 0.7333 -0.1394 1.2826 0.071 Uiso 1 1 calc R . . C46 C 0.5538(2) -0.0777(2) 1.3112(2) 0.0487(8) Uani 1 1 d . . . H46A H 0.5529 -0.0730 1.3743 0.073 Uiso 1 1 calc R . . H46B H 0.5614 -0.1468 1.3198 0.073 Uiso 1 1 calc R . . H46C H 0.4927 -0.0497 1.2908 0.073 Uiso 1 1 calc R . . C47 C 0.9044(2) 0.2019(2) 1.1936(2) 0.0418(7) Uani 1 1 d . . . H47A H 0.9341 0.2545 1.1301 0.050 Uiso 1 1 calc R . . H47B H 0.9564 0.1661 1.2289 0.050 Uiso 1 1 calc R . . C48 C 0.8312(3) 0.2458(2) 1.2562(2) 0.0554(9) Uani 1 1 d . . . H48A H 0.8632 0.2898 1.2718 0.083 Uiso 1 1 calc R . . H48B H 0.8011 0.1932 1.3181 0.083 Uiso 1 1 calc R . . H48C H 0.7813 0.2832 1.2197 0.083 Uiso 1 1 calc R . . C51 C 0.7193(3) -0.2635(2) 0.7973(3) 0.0624(10) Uani 1 1 d . . . H51A H 0.7641 -0.2680 0.7379 0.094 Uiso 1 1 calc R . . H51B H 0.6546 -0.2425 0.7834 0.094 Uiso 1 1 calc R . . H51C H 0.7163 -0.3280 0.8527 0.094 Uiso 1 1 calc R . . C52 C 0.6775(3) -0.1729(3) 0.9089(3) 0.0661(10) Uani 1 1 d . . . H52A H 0.7028 -0.1331 0.9349 0.099 Uiso 1 1 calc R . . H52B H 0.6593 -0.2369 0.9626 0.099 Uiso 1 1 calc R . . H52C H 0.6204 -0.1389 0.8830 0.099 Uiso 1 1 calc R . . C53 C 0.8452(2) -0.2385(2) 0.8660(3) 0.0501(8) Uani 1 1 d . . . H53A H 0.8678 -0.1982 0.8933 0.075 Uiso 1 1 calc R . . H53B H 0.8966 -0.2462 0.8121 0.075 Uiso 1 1 calc R . . H53C H 0.8286 -0.3034 0.9187 0.075 Uiso 1 1 calc R . . C54 C 0.9282(2) 0.2134(2) 0.6063(2) 0.0413(6) Uani 1 1 d . . . H54A H 0.9068 0.1939 0.6786 0.062 Uiso 1 1 calc R . . H54B H 0.8742 0.2471 0.5745 0.062 Uiso 1 1 calc R . . H54C H 0.9821 0.2579 0.5808 0.062 Uiso 1 1 calc R . . C55 C 0.9996(2) 0.1568(2) 0.4679(2) 0.0481(8) Uani 1 1 d . . . H55A H 1.0131 0.0997 0.4495 0.072 Uiso 1 1 calc R . . H55B H 1.0591 0.1926 0.4475 0.072 Uiso 1 1 calc R . . H55C H 0.9502 0.2002 0.4343 0.072 Uiso 1 1 calc R . . C56 C 1.04961(19) 0.0706(2) 0.6267(2) 0.0420(7) Uani 1 1 d . . . H56A H 1.0335 0.0544 0.6985 0.063 Uiso 1 1 calc R . . H56B H 1.1042 0.1146 0.5949 0.063 Uiso 1 1 calc R . . H56C H 1.0675 0.0101 0.6146 0.063 Uiso 1 1 calc R . . C57 C 0.7157(2) 0.1214(2) 0.8183(2) 0.0466(7) Uani 1 1 d . . . H57A H 0.7280 0.1237 0.7498 0.056 Uiso 1 1 calc R . . H57B H 0.7458 0.1785 0.8158 0.056 Uiso 1 1 calc R . . C58 C 0.6094(2) 0.1245(3) 0.8603(3) 0.0739(12) Uani 1 1 d . . . H58A H 0.5799 0.1849 0.8178 0.111 Uiso 1 1 calc R . . H58B H 0.5980 0.1233 0.9276 0.111 Uiso 1 1 calc R . . H58C H 0.5804 0.0673 0.8630 0.111 Uiso 1 1 calc R . . C61 C 1.2586(2) 0.4647(3) 0.3539(2) 0.0529(8) Uani 1 1 d . . . H61A H 1.2359 0.5336 0.3267 0.079 Uiso 1 1 calc R . . H61B H 1.2333 0.4273 0.3252 0.079 Uiso 1 1 calc R . . H61C H 1.3297 0.4607 0.3371 0.079 Uiso 1 1 calc R . . C62 C 1.1119(2) 0.4394(2) 0.4896(2) 0.0456(7) Uani 1 1 d . . . H62A H 1.0855 0.4098 0.5616 0.068 Uiso 1 1 calc R . . H62B H 1.0829 0.4098 0.4563 0.068 Uiso 1 1 calc R . . H62C H 1.0967 0.5104 0.4647 0.068 Uiso 1 1 calc R . . C63 C 1.2471(2) 0.3105(2) 0.5029(2) 0.0439(7) Uani 1 1 d . . . H63A H 1.2102 0.2767 0.5711 0.066 Uiso 1 1 calc R . . H63B H 1.3167 0.2988 0.5014 0.066 Uiso 1 1 calc R . . H63C H 1.2303 0.2852 0.4587 0.066 Uiso 1 1 calc R . . C64 C 1.4617(3) 0.4603(3) 0.7478(3) 0.0655(10) Uani 1 1 d . . . H64A H 1.5098 0.4549 0.6906 0.098 Uiso 1 1 calc R . . H64B H 1.4843 0.4208 0.8091 0.098 Uiso 1 1 calc R . . H64C H 1.4531 0.5293 0.7399 0.098 Uiso 1 1 calc R . . C65 C 1.2867(2) 0.4470(2) 0.8328(2) 0.0485(7) Uani 1 1 d . . . H65A H 1.2255 0.4180 0.8422 0.073 Uiso 1 1 calc R . . H65B H 1.2772 0.5185 0.8110 0.073 Uiso 1 1 calc R . . H65C H 1.3080 0.4199 0.8959 0.073 Uiso 1 1 calc R . . C66 C 1.3803(2) 0.3100(2) 0.7885(2) 0.0440(7) Uani 1 1 d . . . H66A H 1.4217 0.2941 0.7337 0.066 Uiso 1 1 calc R . . H66B H 1.3176 0.2794 0.8086 0.066 Uiso 1 1 calc R . . H66C H 1.4117 0.2851 0.8452 0.066 Uiso 1 1 calc R . . C67 C 0.9940(2) 0.4473(2) 0.7767(3) 0.0603(10) Uani 1 1 d . . . H67A H 0.9842 0.4059 0.8488 0.072 Uiso 1 1 calc R . . H67B H 0.9456 0.4302 0.7500 0.072 Uiso 1 1 calc R . . C68 C 0.9821(3) 0.5516(3) 0.7608(4) 0.0918(16) Uani 1 1 d . . . H68A H 0.9135 0.5676 0.7831 0.138 Uiso 1 1 calc R . . H68B H 1.0040 0.5920 0.6898 0.138 Uiso 1 1 calc R . . H68C H 1.0207 0.5648 0.7990 0.138 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 Nd1 0.01747(6) 0.01846(7) 0.01961(6) -0.00656(5) -0.00424(4) -0.00116(4) P1 0.0215(3) 0.0215(3) 0.0285(3) -0.0118(2) 0.0009(2) 0.0000(2) P2 0.0307(3) 0.0295(3) 0.0245(3) -0.0057(3) -0.0135(2) -0.0075(3) P3 0.0238(3) 0.0198(3) 0.0250(3) -0.0056(2) -0.0024(2) -0.0039(2) O11 0.0333(9) 0.0374(10) 0.0364(10) -0.0211(8) -0.0037(8) -0.0065(8) O12 0.0229(8) 0.0293(9) 0.0262(8) -0.0140(7) -0.0006(6) 0.0005(6) O13 0.0267(9) 0.0244(9) 0.0375(10) -0.0100(8) 0.0037(7) -0.0004(7) O14 0.0269(8) 0.0237(8) 0.0314(9) -0.0125(7) -0.0020(7) 0.0029(6) O21 0.0312(9) 0.0463(11) 0.0317(9) -0.0136(9) -0.0105(8) -0.0045(8) O22 0.0270(8) 0.0330(9) 0.0276(9) -0.0082(7) -0.0126(7) -0.0048(7) O23 0.0358(9) 0.0280(9) 0.0300(9) -0.0033(7) -0.0166(8) -0.0078(7) O24 0.0463(11) 0.0313(10) 0.0292(9) -0.0023(8) -0.0188(8) -0.0141(8) O31 0.0324(9) 0.0214(9) 0.0430(11) -0.0033(8) 0.0053(8) -0.0014(7) O32 0.0245(8) 0.0218(8) 0.0271(8) -0.0061(7) 0.0003(7) -0.0072(6) O33 0.0356(9) 0.0282(9) 0.0254(8) -0.0075(7) -0.0051(7) -0.0124(7) O34 0.0254(8) 0.0312(9) 0.0228(8) -0.0045(7) -0.0047(7) -0.0085(7) C11 0.0207(10) 0.0261(12) 0.0249(11) -0.0128(10) -0.0044(9) 0.0031(9) C12 0.0243(11) 0.0277(12) 0.0310(12) -0.0128(10) -0.0074(10) 0.0040(9) C13 0.0279(12) 0.0292(13) 0.0436(15) -0.0199(12) -0.0080(11) 0.0067(10) C14 0.0194(11) 0.0445(15) 0.0411(14) -0.0282(13) -0.0028(10) -0.0007(10) C15 0.0228(11) 0.0343(13) 0.0295(12) -0.0150(11) -0.0003(9) -0.0061(10) C16 0.0192(10) 0.0286(12) 0.0286(12) -0.0126(10) -0.0044(9) -0.0009(9) C17 0.0537(17) 0.0260(13) 0.0302(13) -0.0057(11) -0.0093(12) 0.0100(12) C18 0.0305(12) 0.0254(12) 0.0335(13) -0.0128(11) 0.0011(10) -0.0058(10) C19 0.0361(15) 0.0547(19) 0.0545(18) -0.0407(16) 0.0060(13) -0.0050(13) C21 0.0249(11) 0.0305(12) 0.0258(11) -0.0126(10) -0.0096(9) -0.0011(9) C22 0.0267(12) 0.0305(13) 0.0317(13) -0.0141(11) -0.0057(10) -0.0056(10) C23 0.0289(12) 0.0462(16) 0.0342(13) -0.0202(12) -0.0088(10) -0.0098(11) C24 0.0310(13) 0.0544(17) 0.0293(13) -0.0186(13) -0.0100(11) -0.0056(12) C25 0.0345(13) 0.0462(16) 0.0229(12) -0.0082(11) -0.0084(10) -0.0085(12) C26 0.0270(12) 0.0331(13) 0.0246(11) -0.0120(10) -0.0052(9) -0.0056(10) C27 0.0341(14) 0.0307(14) 0.0400(15) -0.0098(12) -0.0094(11) -0.0078(11) C28 0.0298(13) 0.0385(14) 0.0280(12) -0.0061(11) -0.0075(10) -0.0121(11) C29 0.0449(17) 0.084(3) 0.0358(16) -0.0166(16) -0.0162(13) -0.0209(16) C31 0.0237(11) 0.0215(11) 0.0302(12) -0.0062(10) 0.0013(9) -0.0053(9) C32 0.0258(12) 0.0305(13) 0.0272(12) -0.0058(10) 0.0020(10) -0.0063(10) C33 0.0479(17) 0.0363(16) 0.0317(14) -0.0021(12) 0.0015(12) -0.0109(13) C34 0.0541(18) 0.0314(15) 0.0476(18) -0.0070(13) 0.0044(14) -0.0184(13) C35 0.0472(17) 0.0357(15) 0.0489(17) -0.0154(14) -0.0012(14) -0.0197(13) C36 0.0293(12) 0.0294(13) 0.0378(14) -0.0145(11) -0.0004(11) -0.0061(10) C37 0.0329(13) 0.0396(15) 0.0254(12) -0.0073(11) -0.0021(10) -0.0098(11) C38 0.0403(15) 0.0345(15) 0.0472(16) -0.0183(13) -0.0126(13) -0.0083(12) C39 0.114(4) 0.044(2) 0.061(2) -0.0017(18) -0.007(2) -0.041(2) C41 0.068(2) 0.048(2) 0.055(2) -0.0032(16) -0.0215(18) 0.0227(17) C42 0.100(3) 0.0442(19) 0.0284(15) -0.0063(14) -0.0165(17) 0.0079(18) C43 0.0549(18) 0.0270(14) 0.0482(18) -0.0073(13) 0.0069(15) -0.0039(13) C44 0.080(2) 0.0374(16) 0.0444(17) -0.0207(14) -0.0077(16) -0.0196(16) C45 0.0438(16) 0.0273(14) 0.0558(19) -0.0052(13) -0.0072(14) 0.0026(12) C46 0.0482(17) 0.0352(16) 0.0540(19) -0.0154(14) 0.0091(14) -0.0188(13) C47 0.0399(15) 0.0394(16) 0.0550(18) -0.0238(14) -0.0144(13) -0.0046(12) C48 0.077(2) 0.054(2) 0.0491(19) -0.0324(16) -0.0170(17) -0.0004(17) C51 0.076(2) 0.0354(17) 0.083(3) -0.0105(17) -0.044(2) -0.0172(16) C52 0.065(2) 0.046(2) 0.055(2) -0.0005(16) 0.0127(17) -0.0103(17) C53 0.0559(19) 0.0281(14) 0.064(2) -0.0048(14) -0.0309(16) -0.0050(13) C54 0.0472(16) 0.0352(15) 0.0429(16) -0.0096(13) -0.0169(13) -0.0108(12) C55 0.0453(17) 0.060(2) 0.0307(14) -0.0054(14) -0.0038(13) -0.0244(15) C56 0.0279(13) 0.0494(17) 0.0419(16) -0.0068(13) -0.0095(12) -0.0120(12) C57 0.0471(17) 0.0550(19) 0.0408(16) -0.0221(15) -0.0172(13) 0.0129(14) C58 0.0401(19) 0.102(3) 0.084(3) -0.039(3) -0.0271(19) 0.0203(19) C61 0.060(2) 0.063(2) 0.0292(14) -0.0090(15) -0.0046(14) -0.0216(17) C62 0.0350(15) 0.0533(19) 0.0415(16) -0.0092(14) -0.0091(12) -0.0076(13) C63 0.0518(17) 0.0462(17) 0.0397(16) -0.0233(14) -0.0079(13) -0.0039(14) C64 0.057(2) 0.068(2) 0.082(3) -0.024(2) -0.032(2) -0.0212(18) C65 0.069(2) 0.0383(16) 0.0425(16) -0.0198(14) -0.0122(15) -0.0037(15) C66 0.0440(16) 0.0386(16) 0.0557(18) -0.0190(14) -0.0244(14) 0.0057(13) C67 0.0381(16) 0.0355(17) 0.084(3) -0.0161(17) 0.0103(16) 0.0049(13) C68 0.069(3) 0.049(2) 0.141(4) -0.045(3) 0.013(3) 0.0070(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O24 2.3259(17) 2_757 ? Nd1 O23 2.3698(16) . ? Nd1 O13 2.3796(16) . ? Nd1 O14 2.3860(16) 2_757 ? Nd1 O33 2.4215(16) . ? Nd1 O34 2.4305(16) . ? Nd1 O14 2.7425(17) . ? Nd1 Nd1 4.0172(6) 2_757 ? P1 O13 1.4985(18) . ? P1 O14 1.5106(16) . ? P1 O11 1.5601(18) . ? P1 O12 1.5862(17) . ? P2 O24 1.4910(18) . ? P2 O23 1.4966(18) . ? P2 O21 1.5641(19) . ? P2 O22 1.5961(18) . ? P3 O33 1.5028(17) . ? P3 O34 1.5050(17) . ? P3 O31 1.5679(18) . ? P3 O32 1.5765(16) . ? O11 C47 1.437(3) . ? O12 C11 1.416(3) . ? O14 Nd1 2.3860(16) 2_757 ? O21 C57 1.451(3) . ? O22 C21 1.405(3) . ? O24 Nd1 2.3259(17) 2_757 ? O31 C67 1.448(3) . ? O32 C31 1.415(3) . ? C11 C12 1.402(3) . ? C11 C16 1.408(3) . ? C12 C13 1.402(3) . ? C12 C17 1.547(4) . ? C13 C14 1.379(4) . ? C13 H13 0.9500 . ? C14 C15 1.388(4) . ? C14 C19 1.507(3) . ? C15 C16 1.393(3) . ? C15 H15 0.9500 . ? C16 C18 1.540(3) . ? C17 C42 1.529(4) . ? C17 C43 1.535(4) . ? C17 C41 1.537(4) . ? C18 C46 1.530(4) . ? C18 C44 1.533(4) . ? C18 C45 1.536(4) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C21 C26 1.410(3) . ? C21 C22 1.411(3) . ? C22 C23 1.393(3) . ? C22 C27 1.551(4) . ? C23 C24 1.373(4) . ? C23 H23 0.9500 . ? C24 C25 1.382(4) . ? C24 C29 1.515(4) . ? C25 C26 1.387(3) . ? C25 H25 0.9500 . ? C26 C28 1.556(3) . ? C27 C52 1.527(4) . ? C27 C53 1.530(4) . ? C27 C51 1.537(4) . ? C28 C56 1.528(4) . ? C28 C54 1.538(4) . ? C28 C55 1.559(4) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C31 C32 1.402(3) . ? C31 C36 1.403(4) . ? C32 C33 1.397(4) . ? C32 C37 1.537(4) . ? C33 C34 1.377(4) . ? C33 H33 0.9500 . ? C34 C35 1.368(4) . ? C34 C39 1.521(4) . ? C35 C36 1.405(4) . ? C35 H35 0.9500 . ? C36 C38 1.538(4) . ? C37 C63 1.533(4) . ? C37 C62 1.536(4) . ? C37 C61 1.541(4) . ? C38 C65 1.533(4) . ? C38 C64 1.543(4) . ? C38 C66 1.543(4) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.492(4) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.489(4) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 C68 1.465(5) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? 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 O24 Nd1 O23 142.64(6) 2_757 . ? O24 Nd1 O13 89.54(7) 2_757 . ? O23 Nd1 O13 87.68(6) . . ? O24 Nd1 O14 76.25(6) 2_757 2_757 ? O23 Nd1 O14 78.99(6) . 2_757 ? O13 Nd1 O14 133.64(6) . 2_757 ? O24 Nd1 O33 77.49(6) 2_757 . ? O23 Nd1 O33 139.39(6) . . ? O13 Nd1 O33 86.66(6) . . ? O14 Nd1 O33 130.69(6) 2_757 . ? O24 Nd1 O34 134.64(6) 2_757 . ? O23 Nd1 O34 82.19(6) . . ? O13 Nd1 O34 101.79(6) . . ? O14 Nd1 O34 119.67(6) 2_757 . ? O33 Nd1 O34 59.84(5) . . ? O24 Nd1 O14 74.01(6) 2_757 . ? O23 Nd1 O14 73.49(6) . . ? O13 Nd1 O14 56.56(5) . . ? O14 Nd1 O14 77.09(5) 2_757 . ? O33 Nd1 O14 132.72(5) . . ? O34 Nd1 O14 147.34(5) . . ? O24 Nd1 Nd1 70.78(4) 2_757 2_757 ? O23 Nd1 Nd1 72.10(4) . 2_757 ? O13 Nd1 Nd1 91.93(4) . 2_757 ? O14 Nd1 Nd1 41.72(4) 2_757 2_757 ? O33 Nd1 Nd1 148.25(4) . 2_757 ? O34 Nd1 Nd1 150.32(4) . 2_757 ? O14 Nd1 Nd1 35.38(3) . 2_757 ? O13 P1 O14 108.86(10) . . ? O13 P1 O11 113.62(10) . . ? O14 P1 O11 111.02(10) . . ? O13 P1 O12 111.83(10) . . ? O14 P1 O12 107.79(9) . . ? O11 P1 O12 103.52(9) . . ? O24 P2 O23 115.66(10) . . ? O24 P2 O21 107.13(11) . . ? O23 P2 O21 111.21(11) . . ? O24 P2 O22 105.96(10) . . ? O23 P2 O22 109.66(10) . . ? O21 P2 O22 106.72(9) . . ? O33 P3 O34 107.15(9) . . ? O33 P3 O31 112.60(10) . . ? O34 P3 O31 113.80(10) . . ? O33 P3 O32 111.51(10) . . ? O34 P3 O32 110.22(9) . . ? O31 P3 O32 101.58(9) . . ? C47 O11 P1 127.03(18) . . ? C11 O12 P1 123.70(14) . . ? P1 O13 Nd1 104.96(9) . . ? P1 O14 Nd1 167.44(10) . 2_757 ? P1 O14 Nd1 89.62(8) . . ? Nd1 O14 Nd1 102.91(5) 2_757 . ? C57 O21 P2 124.57(18) . . ? C21 O22 P2 127.53(15) . . ? P2 O23 Nd1 138.34(10) . . ? P2 O24 Nd1 142.59(10) . 2_757 ? C67 O31 P3 119.38(17) . . ? C31 O32 P3 127.78(15) . . ? P3 O33 Nd1 96.66(8) . . ? P3 O34 Nd1 96.23(8) . . ? C12 C11 C16 123.5(2) . . ? C12 C11 O12 119.6(2) . . ? C16 C11 O12 116.96(19) . . ? C11 C12 C13 115.5(2) . . ? C11 C12 C17 126.3(2) . . ? C13 C12 C17 118.2(2) . . ? C14 C13 C12 123.1(2) . . ? C14 C13 H13 118.4 . . ? C12 C13 H13 118.4 . . ? C13 C14 C15 117.9(2) . . ? C13 C14 C19 121.6(2) . . ? C15 C14 C19 120.4(2) . . ? C14 C15 C16 122.9(2) . . ? C14 C15 H15 118.5 . . ? C16 C15 H15 118.5 . . ? C15 C16 C11 115.7(2) . . ? C15 C16 C18 120.0(2) . . ? C11 C16 C18 124.3(2) . . ? C42 C17 C43 109.6(3) . . ? C42 C17 C41 106.2(3) . . ? C43 C17 C41 107.5(3) . . ? C42 C17 C12 113.0(2) . . ? C43 C17 C12 111.1(2) . . ? C41 C17 C12 109.1(2) . . ? C46 C18 C44 107.0(2) . . ? C46 C18 C45 105.9(2) . . ? C44 C18 C45 110.1(2) . . ? C46 C18 C16 110.9(2) . . ? C44 C18 C16 110.7(2) . . ? C45 C18 C16 112.0(2) . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O22 C21 C26 118.4(2) . . ? O22 C21 C22 118.8(2) . . ? C26 C21 C22 122.8(2) . . ? C23 C22 C21 115.7(2) . . ? C23 C22 C27 117.4(2) . . ? C21 C22 C27 126.9(2) . . ? C24 C23 C22 123.6(2) . . ? C24 C23 H23 118.2 . . ? C22 C23 H23 118.2 . . ? C23 C24 C25 117.8(2) . . ? C23 C24 C29 121.1(2) . . ? C25 C24 C29 121.0(3) . . ? C24 C25 C26 123.3(2) . . ? C24 C25 H25 118.3 . . ? C26 C25 H25 118.3 . . ? C25 C26 C21 116.0(2) . . ? C25 C26 C28 118.1(2) . . ? C21 C26 C28 125.9(2) . . ? C52 C27 C53 108.9(3) . . ? C52 C27 C51 108.1(3) . . ? C53 C27 C51 104.7(2) . . ? C52 C27 C22 111.2(2) . . ? C53 C27 C22 113.6(2) . . ? C51 C27 C22 110.1(2) . . ? C56 C28 C54 110.6(2) . . ? C56 C28 C26 114.3(2) . . ? C54 C28 C26 109.3(2) . . ? C56 C28 C55 105.0(2) . . ? C54 C28 C55 107.5(2) . . ? C26 C28 C55 109.8(2) . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C32 C31 C36 123.9(2) . . ? C32 C31 O32 117.6(2) . . ? C36 C31 O32 118.4(2) . . ? C33 C32 C31 115.5(2) . . ? C33 C32 C37 119.3(2) . . ? C31 C32 C37 125.2(2) . . ? C34 C33 C32 122.9(3) . . ? C34 C33 H33 118.6 . . ? C32 C33 H33 118.6 . . ? C35 C34 C33 118.6(3) . . ? C35 C34 C39 120.5(3) . . ? C33 C34 C39 120.9(3) . . ? C34 C35 C36 123.2(3) . . ? C34 C35 H35 118.4 . . ? C36 C35 H35 118.4 . . ? C31 C36 C35 115.1(2) . . ? C31 C36 C38 126.3(2) . . ? C35 C36 C38 118.7(2) . . ? C63 C37 C62 110.1(2) . . ? C63 C37 C32 112.8(2) . . ? C62 C37 C32 109.9(2) . . ? C63 C37 C61 106.3(2) . . ? C62 C37 C61 107.0(2) . . ? C32 C37 C61 110.6(2) . . ? C65 C38 C36 110.4(2) . . ? C65 C38 C64 108.3(3) . . ? C36 C38 C64 110.2(2) . . ? C65 C38 C66 109.5(2) . . ? C36 C38 C66 113.3(2) . . ? C64 C38 C66 104.9(3) . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C17 C41 H41A 109.5 . . ? C17 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C17 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C17 C42 H42A 109.5 . . ? C17 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C17 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C17 C43 H43A 109.5 . . ? C17 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C17 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C18 C44 H44A 109.5 . . ? C18 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C18 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C18 C45 H45A 109.5 . . ? C18 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C18 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C18 C46 H46A 109.5 . . ? C18 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C18 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O11 C47 C48 108.7(2) . . ? O11 C47 H47A 109.9 . . ? C48 C47 H47A 109.9 . . ? O11 C47 H47B 109.9 . . ? C48 C47 H47B 109.9 . . ? H47A C47 H47B 108.3 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C27 C51 H51A 109.5 . . ? C27 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C27 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C27 C52 H52A 109.5 . . ? C27 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C27 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C27 C53 H53A 109.5 . . ? C27 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C27 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C28 C54 H54A 109.5 . . ? C28 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C28 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C28 C55 H55A 109.5 . . ? C28 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C28 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C28 C56 H56A 109.5 . . ? C28 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C28 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O21 C57 C58 107.8(3) . . ? O21 C57 H57A 110.2 . . ? C58 C57 H57A 110.2 . . ? O21 C57 H57B 110.2 . . ? C58 C57 H57B 110.2 . . ? H57A C57 H57B 108.5 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C37 C61 H61A 109.5 . . ? C37 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C37 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C37 C62 H62A 109.5 . . ? C37 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C37 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C37 C63 H63A 109.5 . . ? C37 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C37 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C38 C64 H64A 109.5 . . ? C38 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C38 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C38 C65 H65A 109.5 . . ? C38 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C38 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C38 C66 H66A 109.5 . . ? C38 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C38 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? O31 C67 C68 108.1(3) . . ? O31 C67 H67A 110.1 . . ? C68 C67 H67A 110.1 . . ? O31 C67 H67B 110.1 . . ? C68 C67 H67B 110.1 . . ? H67A C67 H67B 108.4 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.972 _refine_diff_density_min -0.456 _refine_diff_density_rms 0.082 data_y _database_code_depnum_ccdc_archive 'CCDC 866340' #TrackingRef 'web_deposit_cif_file_0_DrAndreiV.Churakov_1328800800.y.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C102 H168 O24 P6 Y2, C6 H14' _chemical_formula_sum 'C108 H182 O24 P6 Y2' _chemical_formula_weight 2228.18 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' 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.049(2) _cell_length_b 20.351(3) _cell_length_c 22.399(3) _cell_angle_alpha 81.292(2) _cell_angle_beta 87.985(2) _cell_angle_gamma 76.987(2) _cell_volume 6606.5(16) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9208 _cell_measurement_theta_min 2.242 _cell_measurement_theta_max 21.544 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.120 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2380 _exptl_absorpt_coefficient_mu 1.005 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7872 _exptl_absorpt_correction_T_max 0.8243 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 56736 _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_av_sigmaI/netI 0.0781 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.50 _reflns_number_total 24561 _reflns_number_gt 14593 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1361P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 24561 _refine_ls_number_parameters 1052 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.1266 _refine_ls_R_factor_gt 0.0709 _refine_ls_wR_factor_ref 0.2282 _refine_ls_wR_factor_gt 0.1989 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.041 _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 Y1 Y 0.84069(3) 0.20341(2) 0.15875(2) 0.03763(14) Uani 1 1 d . . . Y2 Y 0.66013(3) 0.20715(2) 0.29889(2) 0.03805(14) Uani 1 1 d . . . P1 P 0.83080(9) 0.06249(7) 0.25284(6) 0.0458(3) Uani 1 1 d . . . P2 P 0.60508(9) 0.17821(7) 0.16426(6) 0.0447(3) Uani 1 1 d . . . P3 P 0.69738(10) 0.34820(7) 0.18621(6) 0.0490(3) Uani 1 1 d . . . P4 P 0.87184(10) 0.22995(8) 0.31434(6) 0.0538(4) Uani 1 1 d . . . P5 P 0.96075(10) 0.20810(7) 0.05573(6) 0.0478(3) Uani 1 1 d . . . P6 P 0.53505(10) 0.21566(7) 0.39886(6) 0.0488(3) Uani 1 1 d . . . O11 O 0.7862(2) 0.00761(17) 0.23142(16) 0.0543(9) Uani 1 1 d . . . O12 O 0.8980(2) 0.02332(17) 0.30671(15) 0.0506(9) Uani 1 1 d . . . O13 O 0.8832(2) 0.09320(17) 0.20277(16) 0.0530(9) Uani 1 1 d . . . O14 O 0.7587(2) 0.11273(17) 0.27945(16) 0.0538(9) Uani 1 1 d . . . O21 O 0.5418(2) 0.23650(18) 0.12256(16) 0.0557(9) Uani 1 1 d . . . O22 O 0.5924(2) 0.11036(18) 0.14268(15) 0.0513(9) Uani 1 1 d . . . O23 O 0.5774(2) 0.17835(18) 0.22920(15) 0.0503(9) Uani 1 1 d . . . O24 O 0.7015(2) 0.18309(19) 0.15269(15) 0.0528(9) Uani 1 1 d . . . O31 O 0.7327(3) 0.40141(19) 0.21655(17) 0.0632(10) Uani 1 1 d . . . O32 O 0.6111(2) 0.38967(17) 0.14794(15) 0.0513(9) Uani 1 1 d . . . O33 O 0.7683(3) 0.31331(17) 0.14586(16) 0.0567(10) Uani 1 1 d . . . O34 O 0.6632(3) 0.30059(18) 0.23374(15) 0.0565(10) Uani 1 1 d . . . O41 O 0.9472(3) 0.1724(2) 0.34963(17) 0.0675(11) Uani 1 1 d . . . O42 O 0.9012(3) 0.29865(19) 0.31931(16) 0.0590(10) Uani 1 1 d . . . O43 O 0.7798(2) 0.2301(2) 0.34137(16) 0.0580(10) Uani 1 1 d . . . O44 O 0.8773(3) 0.22258(19) 0.24898(16) 0.0581(10) Uani 1 1 d . . . O51 O 1.0430(3) 0.15469(19) 0.03619(17) 0.0684(12) Uani 1 1 d . . . O52 O 0.9565(2) 0.26893(17) 0.00319(15) 0.0498(9) Uani 1 1 d . . . O53 O 0.8733(2) 0.18467(18) 0.06005(15) 0.0543(9) Uani 1 1 d . . . O54 O 0.9745(2) 0.22722(18) 0.11639(15) 0.0521(9) Uani 1 1 d . . . O61 O 0.4394(3) 0.1981(2) 0.40899(17) 0.0655(11) Uani 1 1 d . . . O62 O 0.5491(2) 0.24028(19) 0.45967(15) 0.0558(9) Uani 1 1 d . . . O63 O 0.6090(2) 0.15544(17) 0.38815(14) 0.0505(9) Uani 1 1 d . . . O64 O 0.5393(3) 0.27063(18) 0.34634(15) 0.0579(10) Uani 1 1 d . . . C11 C 0.9240(4) -0.0481(3) 0.3239(2) 0.0491(13) Uani 1 1 d . . . C12 C 1.0114(4) -0.0808(3) 0.3083(2) 0.0536(14) Uani 1 1 d . . . C13 C 1.0316(4) -0.1514(3) 0.3190(3) 0.0674(17) Uani 1 1 d . . . H13A H 1.0893 -0.1748 0.3089 0.081 Uiso 1 1 calc R . . C14 C 0.9696(5) -0.1884(3) 0.3439(3) 0.0769(19) Uani 1 1 d . . . C15 C 0.8888(5) -0.1517(3) 0.3654(3) 0.0740(19) Uani 1 1 d . . . H15A H 0.8486 -0.1761 0.3856 0.089 Uiso 1 1 calc R . . C16 C 0.8645(4) -0.0829(3) 0.3589(2) 0.0586(15) Uani 1 1 d . . . C17 C 1.0875(4) -0.0448(3) 0.2836(3) 0.0641(16) Uani 1 1 d . . . C18 C 0.7782(4) -0.0482(3) 0.3930(3) 0.0669(17) Uani 1 1 d . . . C19 C 0.9945(6) -0.2658(3) 0.3500(4) 0.113(3) Uani 1 1 d U . . H19A H 1.0491 -0.2830 0.3736 0.170 Uiso 1 1 calc R . . H19B H 1.0045 -0.2794 0.3107 0.170 Uiso 1 1 calc R . . H19C H 0.9457 -0.2840 0.3697 0.170 Uiso 1 1 calc R . . C21 C 0.5271(4) 0.1057(3) 0.1003(2) 0.0468(12) Uani 1 1 d . . . C22 C 0.5483(4) 0.1158(3) 0.0385(2) 0.0528(14) Uani 1 1 d . . . C23 C 0.4753(5) 0.1245(3) -0.0005(3) 0.0732(18) Uani 1 1 d . . . H23A H 0.4859 0.1344 -0.0417 0.088 Uiso 1 1 calc R . . C24 C 0.3882(5) 0.1195(4) 0.0179(3) 0.077(2) Uani 1 1 d . . . C25 C 0.3776(5) 0.0989(4) 0.0788(3) 0.079(2) Uani 1 1 d . . . H25A H 0.3212 0.0908 0.0919 0.095 Uiso 1 1 calc R . . C26 C 0.4454(4) 0.0892(3) 0.1220(3) 0.0602(15) Uani 1 1 d . . . C27 C 0.6447(4) 0.1173(3) 0.0114(2) 0.0609(15) Uani 1 1 d . . . C28 C 0.4278(5) 0.0591(4) 0.1869(3) 0.080(2) Uani 1 1 d . . . C29 C 0.3104(6) 0.1334(5) -0.0263(4) 0.113(3) Uani 1 1 d U . . H29A H 0.3261 0.1042 -0.0568 0.170 Uiso 1 1 calc R . . H29B H 0.2991 0.1802 -0.0450 0.170 Uiso 1 1 calc R . . H29C H 0.2566 0.1246 -0.0053 0.170 Uiso 1 1 calc R . . C31 C 0.5917(3) 0.4603(3) 0.1275(2) 0.0478(13) Uani 1 1 d . . . C32 C 0.5404(4) 0.5041(3) 0.1655(3) 0.0653(16) Uani 1 1 d . . . C33 C 0.5371(4) 0.5739(3) 0.1476(3) 0.0711(18) Uani 1 1 d . . . H33A H 0.5073 0.6045 0.1726 0.085 Uiso 1 1 calc R . . C34 C 0.5751(4) 0.5991(3) 0.0955(3) 0.0671(17) Uani 1 1 d . . . C35 C 0.6146(4) 0.5537(3) 0.0573(3) 0.0589(15) Uani 1 1 d . . . H35A H 0.6371 0.5709 0.0205 0.071 Uiso 1 1 calc R . . C36 C 0.6226(3) 0.4850(3) 0.0703(2) 0.0491(13) Uani 1 1 d . . . C37 C 0.4872(5) 0.4826(4) 0.2224(3) 0.080(2) Uani 1 1 d . . . C38 C 0.6638(4) 0.4398(3) 0.0217(2) 0.0504(13) Uani 1 1 d . . . C39 C 0.5707(6) 0.6748(3) 0.0803(3) 0.094(2) Uani 1 1 d U . . H39A H 0.5786 0.6863 0.0376 0.141 Uiso 1 1 calc R . . H39B H 0.6183 0.6863 0.1014 0.141 Uiso 1 1 calc R . . H39C H 0.5125 0.6998 0.0922 0.141 Uiso 1 1 calc R . . C41 C 0.9669(4) 0.3082(3) 0.3597(3) 0.0580(15) Uani 1 1 d . . . C42 C 0.9350(4) 0.3319(3) 0.4135(3) 0.0682(17) Uani 1 1 d . . . C43 C 1.0021(5) 0.3292(4) 0.4556(3) 0.079(2) Uani 1 1 d . . . H43A H 0.9842 0.3413 0.4934 0.095 Uiso 1 1 calc R . . C44 C 1.0942(5) 0.3095(4) 0.4435(3) 0.078(2) Uani 1 1 d . . . C45 C 1.1203(4) 0.2974(3) 0.3863(3) 0.0672(17) Uani 1 1 d . . . H45A H 1.1821 0.2896 0.3767 0.081 Uiso 1 1 calc R . . C46 C 1.0593(4) 0.2963(3) 0.3427(3) 0.0639(16) Uani 1 1 d . . . C47 C 0.8327(5) 0.3577(4) 0.4303(3) 0.085(2) Uani 1 1 d . . . C48 C 1.0960(4) 0.2842(3) 0.2782(3) 0.0674(17) Uani 1 1 d . . . C49 C 1.1641(6) 0.3079(5) 0.4909(4) 0.108(3) Uani 1 1 d U . . H49A H 1.1512 0.2805 0.5275 0.162 Uiso 1 1 calc R . . H49B H 1.1615 0.3535 0.4985 0.162 Uiso 1 1 calc R . . H49C H 1.2239 0.2888 0.4767 0.162 Uiso 1 1 calc R . . C51 C 1.0153(4) 0.2788(3) -0.0462(2) 0.0499(13) Uani 1 1 d . . . C52 C 0.9945(4) 0.2606(3) -0.1009(2) 0.0580(15) Uani 1 1 d . . . C53 C 1.0585(5) 0.2659(3) -0.1463(3) 0.0713(18) Uani 1 1 d . . . H53A H 1.0496 0.2512 -0.1825 0.086 Uiso 1 1 calc R . . C54 C 1.1340(5) 0.2914(4) -0.1408(3) 0.079(2) Uani 1 1 d . . . C55 C 1.1455(4) 0.3152(3) -0.0881(3) 0.0717(18) Uani 1 1 d . . . H55A H 1.1947 0.3351 -0.0849 0.086 Uiso 1 1 calc R . . C56 C 1.0862(4) 0.3108(3) -0.0390(3) 0.0568(14) Uani 1 1 d . . . C57 C 0.9080(5) 0.2364(3) -0.1131(3) 0.0679(17) Uani 1 1 d . . . C58 C 1.1031(4) 0.3416(3) 0.0176(3) 0.0665(17) Uani 1 1 d . . . C59 C 1.2039(6) 0.2962(5) -0.1911(4) 0.117(3) Uani 1 1 d U . . H59A H 1.2201 0.2536 -0.2066 0.175 Uiso 1 1 calc R . . H59B H 1.2572 0.3060 -0.1754 0.175 Uiso 1 1 calc R . . H59C H 1.1783 0.3319 -0.2229 0.175 Uiso 1 1 calc R . . C61 C 0.4910(4) 0.2467(3) 0.5106(2) 0.0518(14) Uani 1 1 d . . . C62 C 0.5003(4) 0.1906(3) 0.5564(2) 0.0583(15) Uani 1 1 d . . . C63 C 0.4349(5) 0.1982(4) 0.6031(3) 0.0736(19) Uani 1 1 d . . . H63A H 0.4362 0.1614 0.6335 0.088 Uiso 1 1 calc R . . C64 C 0.3707(5) 0.2556(4) 0.6058(3) 0.0718(18) Uani 1 1 d . . . C65 C 0.3726(4) 0.3111(4) 0.5636(3) 0.0712(18) Uani 1 1 d . . . H65A H 0.3317 0.3520 0.5675 0.085 Uiso 1 1 calc R . . C66 C 0.4332(4) 0.3096(3) 0.5148(3) 0.0592(15) Uani 1 1 d . . . C67 C 0.5736(4) 0.1242(3) 0.5592(2) 0.0661(16) Uani 1 1 d . . . C68 C 0.4327(5) 0.3768(3) 0.4690(3) 0.0758(19) Uani 1 1 d . . . C69 C 0.3030(5) 0.2580(5) 0.6578(3) 0.109(3) Uani 1 1 d U . . H69A H 0.2725 0.2211 0.6593 0.163 Uiso 1 1 calc R . . H69B H 0.2589 0.3006 0.6517 0.163 Uiso 1 1 calc R . . H69C H 0.3348 0.2539 0.6950 0.163 Uiso 1 1 calc R . . C71 C 1.0786(6) -0.0259(4) 0.2167(4) 0.112(3) Uiso 1 1 d . . . H71A H 1.0155 -0.0168 0.2056 0.168 Uiso 1 1 calc R . . H71B H 1.1125 -0.0629 0.1974 0.168 Uiso 1 1 calc R . . H71C H 1.1022 0.0141 0.2040 0.168 Uiso 1 1 calc R . . C72 C 1.1817(6) -0.0911(5) 0.2962(4) 0.127(3) Uiso 1 1 d . . . H72A H 1.1900 -0.1043 0.3389 0.190 Uiso 1 1 calc R . . H72B H 1.2275 -0.0671 0.2803 0.190 Uiso 1 1 calc R . . H72C H 1.1869 -0.1310 0.2771 0.190 Uiso 1 1 calc R . . C73 C 1.0895(7) 0.0153(5) 0.3126(5) 0.142(4) Uiso 1 1 d . . . H73A H 1.0406 0.0524 0.2970 0.213 Uiso 1 1 calc R . . H73B H 1.1467 0.0282 0.3041 0.213 Uiso 1 1 calc R . . H73C H 1.0824 0.0044 0.3554 0.213 Uiso 1 1 calc R . . C74 C 0.7933(5) 0.0135(3) 0.4194(3) 0.0798(19) Uiso 1 1 d . . . H74A H 0.8399 -0.0013 0.4498 0.120 Uiso 1 1 calc R . . H74B H 0.7376 0.0353 0.4372 0.120 Uiso 1 1 calc R . . H74C H 0.8119 0.0451 0.3879 0.120 Uiso 1 1 calc R . . C75 C 0.7585(5) -0.0996(4) 0.4473(3) 0.090(2) Uiso 1 1 d . . . H75A H 0.8126 -0.1170 0.4713 0.135 Uiso 1 1 calc R . . H75B H 0.7401 -0.1365 0.4328 0.135 Uiso 1 1 calc R . . H75C H 0.7106 -0.0771 0.4715 0.135 Uiso 1 1 calc R . . C76 C 0.6913(5) -0.0293(3) 0.3534(3) 0.0800(19) Uiso 1 1 d . . . H76A H 0.6974 0.0058 0.3207 0.120 Uiso 1 1 calc R . . H76B H 0.6392 -0.0131 0.3774 0.120 Uiso 1 1 calc R . . H76C H 0.6835 -0.0688 0.3374 0.120 Uiso 1 1 calc R . . C77 C 0.8320(5) -0.0361(3) 0.1894(3) 0.0783(19) Uiso 1 1 d . . . H77A H 0.8934 -0.0574 0.2035 0.094 Uiso 1 1 calc R . . H77B H 0.8361 -0.0091 0.1502 0.094 Uiso 1 1 calc R . . C78 C 0.7815(7) -0.0889(5) 0.1837(4) 0.129(3) Uiso 1 1 d . . . H78A H 0.8063 -0.1127 0.1509 0.194 Uiso 1 1 calc R . . H78B H 0.7184 -0.0680 0.1760 0.194 Uiso 1 1 calc R . . H78C H 0.7870 -0.1205 0.2205 0.194 Uiso 1 1 calc R . . C81 C 0.6583(5) 0.1909(3) -0.0003(3) 0.0740(18) Uiso 1 1 d . . . H81A H 0.6503 0.2098 0.0368 0.111 Uiso 1 1 calc R . . H81B H 0.6143 0.2179 -0.0293 0.111 Uiso 1 1 calc R . . H81C H 0.7187 0.1909 -0.0156 0.111 Uiso 1 1 calc R . . C82 C 0.7224(4) 0.0723(3) 0.0507(3) 0.0741(18) Uiso 1 1 d . . . H82A H 0.7223 0.0889 0.0886 0.111 Uiso 1 1 calc R . . H82B H 0.7794 0.0733 0.0305 0.111 Uiso 1 1 calc R . . H82C H 0.7142 0.0263 0.0577 0.111 Uiso 1 1 calc R . . C83 C 0.6539(6) 0.0912(4) -0.0495(3) 0.097(2) Uiso 1 1 d . . . H83A H 0.6368 0.0481 -0.0452 0.146 Uiso 1 1 calc R . . H83B H 0.7160 0.0859 -0.0631 0.146 Uiso 1 1 calc R . . H83C H 0.6147 0.1234 -0.0785 0.146 Uiso 1 1 calc R . . C84 C 0.3634(6) 0.0097(4) 0.1882(4) 0.117(3) Uiso 1 1 d . . . H84A H 0.3036 0.0349 0.1753 0.175 Uiso 1 1 calc R . . H84B H 0.3600 -0.0134 0.2286 0.175 Uiso 1 1 calc R . . H84C H 0.3864 -0.0231 0.1617 0.175 Uiso 1 1 calc R . . C85 C 0.3823(7) 0.1165(5) 0.2221(5) 0.141(4) Uiso 1 1 d . . . H85A H 0.3453 0.1528 0.1952 0.211 Uiso 1 1 calc R . . H85B H 0.4283 0.1335 0.2397 0.211 Uiso 1 1 calc R . . H85C H 0.3447 0.0994 0.2534 0.211 Uiso 1 1 calc R . . C86 C 0.5139(8) 0.0169(6) 0.2203(5) 0.151(4) Uiso 1 1 d . . . H86A H 0.5443 -0.0176 0.1970 0.226 Uiso 1 1 calc R . . H86B H 0.4973 -0.0043 0.2590 0.226 Uiso 1 1 calc R . . H86C H 0.5540 0.0462 0.2256 0.226 Uiso 1 1 calc R . . C87 C 0.4596(7) 0.2748(5) 0.1410(4) 0.125(3) Uiso 1 1 d . . . H87A H 0.4297 0.2443 0.1678 0.150 Uiso 1 1 calc R . . H87B H 0.4734 0.3074 0.1647 0.150 Uiso 1 1 calc R . . C88 C 0.3991(7) 0.3095(6) 0.0973(5) 0.148(4) Uiso 1 1 d . . . H88A H 0.3381 0.3094 0.1114 0.223 Uiso 1 1 calc R . . H88B H 0.4102 0.2880 0.0617 0.223 Uiso 1 1 calc R . . H88C H 0.4062 0.3556 0.0881 0.223 Uiso 1 1 calc R . . C91 C 0.3988(6) 0.5379(4) 0.2268(4) 0.111(3) Uiso 1 1 d . . . H91A H 0.3657 0.5462 0.1895 0.166 Uiso 1 1 calc R . . H91B H 0.4142 0.5792 0.2342 0.166 Uiso 1 1 calc R . . H91C H 0.3618 0.5224 0.2593 0.166 Uiso 1 1 calc R . . C92 C 0.5454(7) 0.4735(5) 0.2793(4) 0.137(3) Uiso 1 1 d . . . H92A H 0.5922 0.4325 0.2808 0.206 Uiso 1 1 calc R . . H92B H 0.5074 0.4704 0.3145 0.206 Uiso 1 1 calc R . . H92C H 0.5729 0.5119 0.2781 0.206 Uiso 1 1 calc R . . C93 C 0.4515(6) 0.4169(4) 0.2191(4) 0.111(3) Uiso 1 1 d . . . H93A H 0.4186 0.4224 0.1821 0.166 Uiso 1 1 calc R . . H93B H 0.4118 0.4096 0.2528 0.166 Uiso 1 1 calc R . . H93C H 0.5022 0.3785 0.2204 0.166 Uiso 1 1 calc R . . C94 C 0.6277(4) 0.3752(3) 0.0228(3) 0.0629(15) Uiso 1 1 d . . . H94A H 0.6542 0.3420 0.0562 0.094 Uiso 1 1 calc R . . H94B H 0.6437 0.3570 -0.0142 0.094 Uiso 1 1 calc R . . H94C H 0.5625 0.3859 0.0272 0.094 Uiso 1 1 calc R . . C95 C 0.7676(4) 0.4227(3) 0.0252(3) 0.0602(15) Uiso 1 1 d . . . H95A H 0.7868 0.3934 0.0624 0.090 Uiso 1 1 calc R . . H95B H 0.7890 0.4640 0.0237 0.090 Uiso 1 1 calc R . . H95C H 0.7925 0.4000 -0.0082 0.090 Uiso 1 1 calc R . . C96 C 0.6361(4) 0.4808(3) -0.0421(3) 0.0727(17) Uiso 1 1 d . . . H96A H 0.6662 0.5181 -0.0498 0.109 Uiso 1 1 calc R . . H96B H 0.5712 0.4981 -0.0435 0.109 Uiso 1 1 calc R . . H96C H 0.6538 0.4513 -0.0721 0.109 Uiso 1 1 calc R . . C97 C 0.8062(5) 0.4334(4) 0.1921(4) 0.094(2) Uiso 1 1 d . . . H97A H 0.8630 0.4089 0.2116 0.112 Uiso 1 1 calc R . . H97B H 0.8125 0.4306 0.1492 0.112 Uiso 1 1 calc R . . C98 C 0.7890(9) 0.5038(6) 0.2009(6) 0.176(5) Uiso 1 1 d . . . H98A H 0.8389 0.5232 0.1847 0.265 Uiso 1 1 calc R . . H98B H 0.7831 0.5067 0.2433 0.265 Uiso 1 1 calc R . . H98C H 0.7337 0.5285 0.1806 0.265 Uiso 1 1 calc R . . C101 C 0.7965(6) 0.2975(4) 0.4654(4) 0.104(3) Uiso 1 1 d . . . H10D H 0.7979 0.2636 0.4396 0.156 Uiso 1 1 calc R . . H10E H 0.7349 0.3137 0.4782 0.156 Uiso 1 1 calc R . . H10F H 0.8342 0.2778 0.5001 0.156 Uiso 1 1 calc R . . C102 C 0.7742(6) 0.3927(4) 0.3764(4) 0.110(3) Uiso 1 1 d . . . H10G H 0.7751 0.3611 0.3485 0.165 Uiso 1 1 calc R . . H10H H 0.7976 0.4307 0.3569 0.165 Uiso 1 1 calc R . . H10I H 0.7127 0.4086 0.3894 0.165 Uiso 1 1 calc R . . C103 C 0.8287(7) 0.4121(5) 0.4731(4) 0.136(3) Uiso 1 1 d . . . H10J H 0.8500 0.3897 0.5125 0.204 Uiso 1 1 calc R . . H10K H 0.7670 0.4373 0.4759 0.204 Uiso 1 1 calc R . . H10L H 0.8667 0.4427 0.4572 0.204 Uiso 1 1 calc R . . C104 C 1.0314(5) 0.3276(4) 0.2295(3) 0.083(2) Uiso 1 1 d . . . H10M H 1.0156 0.3739 0.2375 0.124 Uiso 1 1 calc R . . H10N H 0.9771 0.3102 0.2296 0.124 Uiso 1 1 calc R . . H10O H 1.0606 0.3261 0.1908 0.124 Uiso 1 1 calc R . . C105 C 1.1114(5) 0.2095(4) 0.2686(3) 0.090(2) Uiso 1 1 d . . . H10P H 1.0541 0.1960 0.2711 0.135 Uiso 1 1 calc R . . H10Q H 1.1517 0.1813 0.2993 0.135 Uiso 1 1 calc R . . H10R H 1.1380 0.2044 0.2296 0.135 Uiso 1 1 calc R . . C106 C 1.1883(5) 0.3069(4) 0.2676(4) 0.097(2) Uiso 1 1 d . . . H10S H 1.1814 0.3521 0.2775 0.145 Uiso 1 1 calc R . . H10T H 1.2058 0.3068 0.2260 0.145 Uiso 1 1 calc R . . H10U H 1.2344 0.2759 0.2928 0.145 Uiso 1 1 calc R . . C107 C 0.9354(6) 0.1386(4) 0.4113(4) 0.106(3) Uiso 1 1 d . . . H10V H 0.8842 0.1660 0.4304 0.127 Uiso 1 1 calc R . . H10W H 0.9217 0.0946 0.4096 0.127 Uiso 1 1 calc R . . C108 C 1.0136(8) 0.1295(6) 0.4462(5) 0.173(5) Uiso 1 1 d . . . H10X H 1.0043 0.1063 0.4857 0.259 Uiso 1 1 calc R . . H10Y H 1.0258 0.1732 0.4495 0.259 Uiso 1 1 calc R . . H10Z H 1.0645 0.1028 0.4273 0.259 Uiso 1 1 calc R . . C111 C 0.8223(5) 0.2833(4) -0.0902(3) 0.083(2) Uiso 1 1 d . . . H11A H 0.8230 0.2774 -0.0468 0.124 Uiso 1 1 calc R . . H11B H 0.7686 0.2718 -0.1036 0.124 Uiso 1 1 calc R . . H11C H 0.8220 0.3300 -0.1058 0.124 Uiso 1 1 calc R . . C112 C 0.8935(6) 0.2420(4) -0.1818(4) 0.106(3) Uiso 1 1 d . . . H11D H 0.9342 0.2045 -0.1969 0.158 Uiso 1 1 calc R . . H11E H 0.9057 0.2842 -0.2018 0.158 Uiso 1 1 calc R . . H11F H 0.8316 0.2406 -0.1894 0.158 Uiso 1 1 calc R . . C113 C 0.9115(5) 0.1637(3) -0.0867(3) 0.0794(19) Uiso 1 1 d . . . H11G H 0.9674 0.1354 -0.0985 0.119 Uiso 1 1 calc R . . H11H H 0.8607 0.1494 -0.1013 0.119 Uiso 1 1 calc R . . H11I H 0.9086 0.1597 -0.0435 0.119 Uiso 1 1 calc R . . C114 C 1.1558(5) 0.2863(4) 0.0646(3) 0.082(2) Uiso 1 1 d . . . H11J H 1.2145 0.2675 0.0486 0.123 Uiso 1 1 calc R . . H11K H 1.1226 0.2510 0.0748 0.123 Uiso 1 1 calc R . . H11L H 1.1637 0.3055 0.1001 0.123 Uiso 1 1 calc R . . C115 C 1.1608(6) 0.3954(4) 0.0004(4) 0.102(2) Uiso 1 1 d . . . H11M H 1.2220 0.3732 -0.0088 0.153 Uiso 1 1 calc R . . H11N H 1.1617 0.4201 0.0336 0.153 Uiso 1 1 calc R . . H11O H 1.1347 0.4265 -0.0344 0.153 Uiso 1 1 calc R . . C116 C 1.0128(5) 0.3801(3) 0.0439(3) 0.0783(19) Uiso 1 1 d . . . H11P H 0.9798 0.3477 0.0638 0.117 Uiso 1 1 calc R . . H11Q H 0.9763 0.4092 0.0118 0.117 Uiso 1 1 calc R . . H11R H 1.0264 0.4072 0.0725 0.117 Uiso 1 1 calc R . . C117 C 1.0737(7) 0.0903(5) 0.0761(5) 0.132(3) Uiso 1 1 d . . . H11S H 1.1314 0.0896 0.0945 0.158 Uiso 1 1 calc R . . H11T H 1.0294 0.0856 0.1081 0.158 Uiso 1 1 calc R . . C118 C 1.0835(10) 0.0388(7) 0.0441(6) 0.203(6) Uiso 1 1 d . . . H11U H 1.1345 0.0033 0.0594 0.304 Uiso 1 1 calc R . . H11V H 1.0939 0.0548 0.0025 0.304 Uiso 1 1 calc R . . H11W H 1.0291 0.0212 0.0476 0.304 Uiso 1 1 calc R . . C121 C 0.6685(5) 0.1383(4) 0.5413(3) 0.083(2) Uiso 1 1 d . . . H12A H 0.6810 0.1716 0.5640 0.125 Uiso 1 1 calc R . . H12B H 0.6691 0.1553 0.4989 0.125 Uiso 1 1 calc R . . H12C H 0.7142 0.0968 0.5499 0.125 Uiso 1 1 calc R . . C122 C 0.5843(5) 0.0863(4) 0.6244(3) 0.098(2) Uiso 1 1 d . . . H12D H 0.6026 0.1145 0.6501 0.147 Uiso 1 1 calc R . . H12E H 0.6298 0.0446 0.6254 0.147 Uiso 1 1 calc R . . H12F H 0.5272 0.0760 0.6382 0.147 Uiso 1 1 calc R . . C123 C 0.5476(4) 0.0745(3) 0.5196(3) 0.0730(18) Uiso 1 1 d . . . H12G H 0.5896 0.0311 0.5273 0.109 Uiso 1 1 calc R . . H12H H 0.5502 0.0930 0.4777 0.109 Uiso 1 1 calc R . . H12I H 0.4868 0.0690 0.5295 0.109 Uiso 1 1 calc R . . C124 C 0.3809(5) 0.3784(4) 0.4123(3) 0.089(2) Uiso 1 1 d . . . H12J H 0.4133 0.3435 0.3901 0.134 Uiso 1 1 calc R . . H12K H 0.3750 0.4221 0.3878 0.134 Uiso 1 1 calc R . . H12L H 0.3214 0.3704 0.4228 0.134 Uiso 1 1 calc R . . C125 C 0.3859(6) 0.4405(5) 0.4968(4) 0.125(3) Uiso 1 1 d . . . H12M H 0.3886 0.4807 0.4687 0.188 Uiso 1 1 calc R . . H12N H 0.4166 0.4414 0.5334 0.188 Uiso 1 1 calc R . . H12O H 0.3234 0.4393 0.5056 0.188 Uiso 1 1 calc R . . C126 C 0.5283(5) 0.3861(4) 0.4533(3) 0.093(2) Uiso 1 1 d . . . H12P H 0.5585 0.3515 0.4301 0.140 Uiso 1 1 calc R . . H12Q H 0.5620 0.3824 0.4897 0.140 Uiso 1 1 calc R . . H12R H 0.5252 0.4303 0.4300 0.140 Uiso 1 1 calc R . . C127 C 0.4055(5) 0.1638(4) 0.3656(3) 0.086(2) Uiso 1 1 d . . . H12S H 0.4546 0.1291 0.3527 0.103 Uiso 1 1 calc R . . H12T H 0.3821 0.1963 0.3304 0.103 Uiso 1 1 calc R . . C128 C 0.3320(5) 0.1322(4) 0.3939(4) 0.098(2) Uiso 1 1 d . . . H12U H 0.3074 0.1110 0.3648 0.148 Uiso 1 1 calc R . . H12V H 0.2846 0.1666 0.4078 0.148 Uiso 1 1 calc R . . H12W H 0.3563 0.0984 0.4275 0.148 Uiso 1 1 calc R . . C1 C 0.7130(15) 0.3540(12) 0.6298(10) 0.176(3) Uiso 0.50 1 d PD A 1 H1A H 0.7057 0.3847 0.5923 0.264 Uiso 0.50 1 calc PR A 1 H1B H 0.7647 0.3171 0.6270 0.264 Uiso 0.50 1 calc PR A 1 H1C H 0.7225 0.3780 0.6619 0.264 Uiso 0.50 1 calc PR A 1 C2 C 0.6282(14) 0.3262(12) 0.6426(9) 0.176(3) Uiso 0.50 1 d PD A 1 H2A H 0.6179 0.3021 0.6101 0.211 Uiso 0.50 1 calc PR A 1 H2B H 0.5756 0.3633 0.6452 0.211 Uiso 0.50 1 calc PR A 1 C3 C 0.6408(13) 0.2778(12) 0.7019(9) 0.176(3) Uiso 0.50 1 d PD A 1 H3A H 0.6828 0.2356 0.6958 0.211 Uiso 0.50 1 calc PR A 1 H3B H 0.6675 0.2980 0.7314 0.211 Uiso 0.50 1 calc PR A 1 C4 C 0.5531(13) 0.2625(11) 0.7260(9) 0.176(3) Uiso 0.50 1 d PD A 1 H4A H 0.5249 0.2448 0.6955 0.211 Uiso 0.50 1 calc PR A 1 H4B H 0.5124 0.3045 0.7339 0.211 Uiso 0.50 1 calc PR A 1 C5 C 0.5644(13) 0.2114(12) 0.7834(9) 0.176(3) Uiso 0.50 1 d PD A 1 H5A H 0.6129 0.1722 0.7784 0.211 Uiso 0.50 1 calc PR A 1 H5B H 0.5804 0.2320 0.8167 0.211 Uiso 0.50 1 calc PR A 1 C6 C 0.4750(14) 0.1894(12) 0.7967(10) 0.176(3) Uiso 0.50 1 d PD A 1 H6A H 0.4738 0.1693 0.8383 0.264 Uiso 0.50 1 calc PR A 1 H6B H 0.4695 0.1566 0.7712 0.264 Uiso 0.50 1 calc PR A 1 H6C H 0.4252 0.2284 0.7890 0.264 Uiso 0.50 1 calc PR A 1 C10 C 0.0722(15) 0.5083(13) 0.4110(8) 0.176(3) Uiso 0.50 1 d PD B 2 H10A H 0.0503 0.5409 0.4379 0.264 Uiso 0.50 1 calc PR B 2 H10B H 0.1351 0.5077 0.4014 0.264 Uiso 0.50 1 calc PR B 2 H10C H 0.0668 0.4638 0.4300 0.264 Uiso 0.50 1 calc PR B 2 C20 C 0.0158(12) 0.5281(13) 0.3529(8) 0.176(3) Uiso 0.50 1 d PD B 2 H20A H -0.0203 0.4951 0.3492 0.211 Uiso 0.50 1 calc PR B 2 H20B H -0.0243 0.5729 0.3517 0.211 Uiso 0.50 1 calc PR B 2 C30 C 0.0879(13) 0.5281(13) 0.3037(7) 0.176(3) Uiso 0.50 1 d PD B 2 H30A H 0.1172 0.5655 0.3061 0.211 Uiso 0.50 1 calc PR B 2 H30B H 0.1340 0.4861 0.3119 0.211 Uiso 0.50 1 calc PR B 2 C40 C 0.0541(13) 0.5346(13) 0.2405(7) 0.176(3) Uiso 0.50 1 d PD B 2 H40A H 0.0142 0.5792 0.2297 0.211 Uiso 0.50 1 calc PR B 2 H40B H 0.0189 0.5005 0.2385 0.211 Uiso 0.50 1 calc PR B 2 C50 C 0.1322(13) 0.5254(14) 0.1956(8) 0.176(3) Uiso 0.50 1 d PD B 2 H50A H 0.1772 0.4842 0.2097 0.211 Uiso 0.50 1 calc PR B 2 H50B H 0.1613 0.5637 0.1924 0.211 Uiso 0.50 1 calc PR B 2 C60 C 0.0971(16) 0.5207(13) 0.1342(8) 0.176(3) Uiso 0.50 1 d PD B 2 H60A H 0.1251 0.5476 0.1035 0.264 Uiso 0.50 1 calc PR B 2 H60B H 0.0322 0.5373 0.1328 0.264 Uiso 0.50 1 calc PR B 2 H60C H 0.1119 0.4740 0.1274 0.264 Uiso 0.50 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0392(3) 0.0403(3) 0.0338(3) -0.0049(2) 0.00460(19) -0.0107(2) Y2 0.0403(3) 0.0413(3) 0.0319(3) -0.0060(2) 0.00463(19) -0.0083(2) P1 0.0501(8) 0.0368(7) 0.0467(8) -0.0025(6) 0.0030(6) -0.0047(6) P2 0.0428(8) 0.0553(8) 0.0404(7) -0.0102(6) -0.0002(6) -0.0176(6) P3 0.0570(9) 0.0384(7) 0.0471(8) 0.0008(6) 0.0024(7) -0.0066(7) P4 0.0544(9) 0.0676(10) 0.0452(8) -0.0141(7) -0.0057(7) -0.0209(8) P5 0.0517(8) 0.0508(8) 0.0420(8) -0.0078(6) 0.0139(6) -0.0149(7) P6 0.0497(8) 0.0570(9) 0.0379(7) -0.0092(6) 0.0125(6) -0.0087(7) O11 0.063(2) 0.048(2) 0.055(2) -0.0145(17) 0.0021(18) -0.0120(18) O12 0.052(2) 0.042(2) 0.055(2) -0.0036(16) -0.0025(17) -0.0047(17) O13 0.054(2) 0.046(2) 0.051(2) 0.0016(16) 0.0098(17) -0.0036(17) O14 0.055(2) 0.046(2) 0.055(2) -0.0059(17) 0.0067(17) -0.0017(17) O21 0.054(2) 0.057(2) 0.052(2) -0.0070(18) 0.0040(18) -0.0054(19) O22 0.057(2) 0.058(2) 0.043(2) -0.0110(17) -0.0031(17) -0.0201(18) O23 0.050(2) 0.067(2) 0.039(2) -0.0126(17) 0.0028(16) -0.0196(18) O24 0.045(2) 0.071(2) 0.047(2) -0.0083(18) 0.0019(16) -0.0232(19) O31 0.071(3) 0.055(2) 0.066(3) -0.0078(19) 0.001(2) -0.020(2) O32 0.055(2) 0.043(2) 0.051(2) -0.0002(16) -0.0011(17) -0.0055(17) O33 0.063(2) 0.043(2) 0.055(2) 0.0031(17) 0.0090(18) -0.0027(18) O34 0.067(2) 0.051(2) 0.046(2) -0.0003(17) 0.0095(18) -0.0074(19) O41 0.064(3) 0.081(3) 0.056(2) -0.005(2) -0.012(2) -0.013(2) O42 0.066(3) 0.066(2) 0.054(2) -0.0145(19) -0.0085(19) -0.026(2) O43 0.056(2) 0.074(3) 0.050(2) -0.0139(19) -0.0056(18) -0.022(2) O44 0.065(2) 0.072(3) 0.046(2) -0.0185(18) -0.0009(18) -0.024(2) O51 0.075(3) 0.055(2) 0.061(3) 0.0032(19) 0.028(2) 0.002(2) O52 0.052(2) 0.051(2) 0.047(2) -0.0058(16) 0.0168(16) -0.0159(17) O53 0.066(2) 0.063(2) 0.041(2) -0.0117(17) 0.0118(17) -0.030(2) O54 0.048(2) 0.068(2) 0.043(2) -0.0079(17) 0.0071(16) -0.0198(18) O61 0.060(2) 0.092(3) 0.051(2) -0.023(2) 0.0170(19) -0.026(2) O62 0.055(2) 0.073(3) 0.042(2) -0.0141(18) 0.0155(17) -0.017(2) O63 0.060(2) 0.047(2) 0.0386(19) -0.0003(15) 0.0113(16) -0.0066(18) O64 0.065(2) 0.054(2) 0.044(2) -0.0032(17) 0.0165(18) 0.0022(19) C11 0.056(3) 0.044(3) 0.044(3) -0.002(2) 0.002(2) -0.007(3) C12 0.053(3) 0.051(3) 0.051(3) -0.002(3) 0.002(3) -0.003(3) C13 0.069(4) 0.062(4) 0.064(4) -0.007(3) 0.007(3) 0.000(3) C14 0.098(5) 0.051(4) 0.070(4) 0.009(3) 0.014(4) -0.007(4) C15 0.084(5) 0.056(4) 0.073(4) 0.006(3) 0.020(4) -0.010(4) C16 0.065(4) 0.054(4) 0.050(3) -0.001(3) 0.007(3) -0.005(3) C17 0.051(4) 0.056(4) 0.079(4) -0.007(3) 0.003(3) -0.003(3) C18 0.068(4) 0.071(4) 0.055(4) 0.007(3) 0.014(3) -0.016(3) C19 0.135(6) 0.059(4) 0.135(6) 0.000(4) 0.035(5) -0.013(4) C21 0.053(3) 0.049(3) 0.043(3) -0.010(2) -0.004(2) -0.018(3) C22 0.068(4) 0.048(3) 0.048(3) -0.008(2) -0.001(3) -0.022(3) C23 0.093(5) 0.089(5) 0.048(4) -0.005(3) -0.014(3) -0.041(4) C24 0.087(5) 0.096(5) 0.064(4) -0.007(4) -0.016(4) -0.053(4) C25 0.072(4) 0.104(5) 0.080(5) -0.017(4) 0.004(4) -0.057(4) C26 0.069(4) 0.073(4) 0.052(3) -0.018(3) 0.004(3) -0.036(3) C27 0.080(4) 0.067(4) 0.042(3) -0.019(3) 0.008(3) -0.022(3) C28 0.079(5) 0.105(5) 0.072(4) -0.020(4) 0.018(4) -0.053(4) C29 0.111(6) 0.139(6) 0.103(5) -0.007(5) -0.035(4) -0.058(5) C31 0.039(3) 0.046(3) 0.052(3) -0.001(2) 0.001(2) -0.001(2) C32 0.063(4) 0.065(4) 0.061(4) -0.010(3) -0.001(3) 0.000(3) C33 0.079(5) 0.048(4) 0.076(5) -0.017(3) -0.001(4) 0.013(3) C34 0.070(4) 0.045(3) 0.077(5) -0.002(3) -0.012(3) 0.004(3) C35 0.061(4) 0.051(4) 0.057(4) 0.008(3) 0.001(3) -0.006(3) C36 0.038(3) 0.048(3) 0.057(3) -0.001(3) -0.002(2) -0.004(2) C37 0.075(5) 0.096(5) 0.060(4) -0.021(4) 0.018(3) 0.006(4) C38 0.051(3) 0.047(3) 0.049(3) -0.003(2) 0.006(2) -0.007(3) C39 0.118(5) 0.060(4) 0.098(5) -0.009(4) -0.003(4) -0.009(4) C41 0.063(4) 0.060(4) 0.054(4) -0.011(3) -0.010(3) -0.018(3) C42 0.065(4) 0.078(4) 0.070(4) -0.029(3) 0.002(3) -0.021(3) C43 0.092(5) 0.100(5) 0.060(4) -0.021(4) -0.004(4) -0.043(4) C44 0.072(5) 0.103(5) 0.069(5) -0.004(4) -0.019(4) -0.041(4) C45 0.058(4) 0.083(4) 0.067(4) -0.009(3) -0.008(3) -0.030(3) C46 0.058(4) 0.081(4) 0.056(4) -0.004(3) -0.004(3) -0.026(3) C47 0.090(5) 0.098(5) 0.076(5) -0.049(4) -0.001(4) -0.014(4) C48 0.043(3) 0.085(5) 0.069(4) -0.005(3) 0.012(3) -0.011(3) C49 0.102(5) 0.140(6) 0.095(5) -0.012(5) -0.029(4) -0.054(5) C51 0.053(3) 0.051(3) 0.043(3) -0.004(2) 0.021(2) -0.012(3) C52 0.071(4) 0.056(3) 0.045(3) -0.004(3) 0.014(3) -0.015(3) C53 0.082(5) 0.077(4) 0.053(4) -0.009(3) 0.022(3) -0.019(4) C54 0.075(5) 0.089(5) 0.065(4) -0.004(4) 0.038(4) -0.010(4) C55 0.064(4) 0.084(5) 0.069(4) -0.008(4) 0.027(3) -0.027(3) C56 0.054(3) 0.057(3) 0.059(4) -0.009(3) 0.019(3) -0.016(3) C57 0.096(5) 0.071(4) 0.041(3) -0.010(3) 0.010(3) -0.028(4) C58 0.058(4) 0.075(4) 0.078(4) -0.021(3) 0.026(3) -0.034(3) C59 0.111(6) 0.148(6) 0.091(5) -0.017(5) 0.058(4) -0.039(5) C61 0.051(3) 0.071(4) 0.039(3) -0.020(3) 0.015(2) -0.019(3) C62 0.063(4) 0.078(4) 0.040(3) -0.013(3) 0.006(3) -0.026(3) C63 0.081(5) 0.102(5) 0.044(4) -0.010(3) 0.016(3) -0.037(4) C64 0.064(4) 0.098(5) 0.056(4) -0.020(4) 0.022(3) -0.021(4) C65 0.057(4) 0.092(5) 0.071(4) -0.041(4) 0.012(3) -0.010(3) C66 0.058(4) 0.067(4) 0.057(4) -0.022(3) 0.015(3) -0.017(3) C67 0.081(4) 0.071(4) 0.041(3) 0.001(3) -0.001(3) -0.014(4) C68 0.082(5) 0.058(4) 0.087(5) -0.028(3) 0.029(4) -0.007(3) C69 0.099(5) 0.141(6) 0.084(5) -0.024(4) 0.049(4) -0.024(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 O44 2.226(3) . ? Y1 O24 2.236(3) . ? Y1 O33 2.236(3) . ? Y1 O13 2.267(3) . ? Y1 O54 2.315(3) . ? Y1 O53 2.317(3) . ? Y2 O34 2.223(3) . ? Y2 O43 2.237(3) . ? Y2 O14 2.237(3) . ? Y2 O23 2.252(3) . ? Y2 O63 2.306(3) . ? Y2 O64 2.308(3) . ? P1 O14 1.489(4) . ? P1 O13 1.489(4) . ? P1 O11 1.566(4) . ? P1 O12 1.595(4) . ? P2 O24 1.488(4) . ? P2 O23 1.499(3) . ? P2 O21 1.551(4) . ? P2 O22 1.582(4) . ? P3 O34 1.486(4) . ? P3 O33 1.498(4) . ? P3 O31 1.557(4) . ? P3 O32 1.581(4) . ? P4 O43 1.491(4) . ? P4 O44 1.492(4) . ? P4 O41 1.570(4) . ? P4 O42 1.578(4) . ? P5 O53 1.493(4) . ? P5 O54 1.502(4) . ? P5 O51 1.551(4) . ? P5 O52 1.565(4) . ? P6 O63 1.501(4) . ? P6 O64 1.506(4) . ? P6 O62 1.557(4) . ? P6 O61 1.561(4) . ? O11 C77 1.443(7) . ? O12 C11 1.413(6) . ? O21 C87 1.391(10) . ? O22 C21 1.419(6) . ? O31 C97 1.455(8) . ? O32 C31 1.408(6) . ? O41 C107 1.471(9) . ? O42 C41 1.426(6) . ? O51 C117 1.460(10) . ? O52 C51 1.412(5) . ? O61 C127 1.446(8) . ? O62 C61 1.416(6) . ? C11 C12 1.392(7) . ? C11 C16 1.410(7) . ? C12 C13 1.385(8) . ? C12 C17 1.539(8) . ? C13 C14 1.379(9) . ? C13 H13A 0.9300 . ? C14 C15 1.388(9) . ? C14 C19 1.521(9) . ? C15 C16 1.351(8) . ? C15 H15A 0.9300 . ? C16 C18 1.565(8) . ? C17 C73 1.475(11) . ? C17 C71 1.494(10) . ? C17 C72 1.523(10) . ? C18 C74 1.529(9) . ? C18 C75 1.545(9) . ? C18 C76 1.549(9) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C21 C26 1.397(7) . ? C21 C22 1.405(7) . ? C22 C23 1.391(8) . ? C22 C27 1.558(8) . ? C23 C24 1.383(9) . ? C23 H23A 0.9300 . ? C24 C25 1.379(9) . ? C24 C29 1.509(9) . ? C25 C26 1.392(8) . ? C25 H25A 0.9300 . ? C26 C28 1.527(8) . ? C27 C82 1.524(8) . ? C27 C83 1.528(9) . ? C27 C81 1.540(8) . ? C28 C85 1.528(11) . ? C28 C86 1.532(12) . ? C28 C84 1.542(10) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C31 C36 1.407(7) . ? C31 C32 1.410(7) . ? C32 C33 1.408(8) . ? C32 C37 1.541(9) . ? C33 C34 1.361(9) . ? C33 H33A 0.9300 . ? C34 C35 1.377(8) . ? C34 C39 1.514(8) . ? C35 C36 1.363(7) . ? C35 H35A 0.9300 . ? C36 C38 1.554(7) . ? C37 C92 1.534(11) . ? C37 C91 1.548(10) . ? C37 C93 1.561(10) . ? C38 C95 1.524(7) . ? C38 C94 1.529(7) . ? C38 C96 1.559(8) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C41 C42 1.396(8) . ? C41 C46 1.406(8) . ? C42 C43 1.392(9) . ? C42 C47 1.562(9) . ? C43 C44 1.383(9) . ? C43 H43A 0.9300 . ? C44 C45 1.368(9) . ? C44 C49 1.512(9) . ? C45 C46 1.371(8) . ? C45 H45A 0.9300 . ? C46 C48 1.563(8) . ? C47 C102 1.508(10) . ? C47 C101 1.547(10) . ? C47 C103 1.561(11) . ? C48 C104 1.519(9) . ? C48 C105 1.532(9) . ? C48 C106 1.559(9) . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C51 C56 1.395(7) . ? C51 C52 1.397(8) . ? C52 C53 1.384(8) . ? C52 C57 1.537(9) . ? C53 C54 1.369(9) . ? C53 H53A 0.9300 . ? C54 C55 1.373(9) . ? C54 C59 1.521(8) . ? C55 C56 1.395(7) . ? C55 H55A 0.9300 . ? C56 C58 1.549(8) . ? C57 C113 1.498(8) . ? C57 C111 1.544(9) . ? C57 C112 1.547(9) . ? C58 C114 1.517(9) . ? C58 C115 1.543(9) . ? C58 C116 1.554(8) . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C61 C66 1.389(8) . ? C61 C62 1.400(8) . ? C62 C63 1.411(8) . ? C62 C67 1.534(8) . ? C63 C64 1.346(9) . ? C63 H63A 0.9300 . ? C64 C65 1.365(9) . ? C64 C69 1.518(8) . ? C65 C66 1.398(8) . ? C65 H65A 0.9300 . ? C66 C68 1.579(9) . ? C67 C122 1.541(9) . ? C67 C121 1.546(9) . ? C67 C123 1.561(8) . ? C68 C124 1.507(10) . ? C68 C126 1.516(9) . ? C68 C125 1.538(10) . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? C73 H73A 0.9600 . ? C73 H73B 0.9600 . ? C73 H73C 0.9600 . ? C74 H74A 0.9600 . ? C74 H74B 0.9600 . ? C74 H74C 0.9600 . ? C75 H75A 0.9600 . ? C75 H75B 0.9600 . ? C75 H75C 0.9600 . ? C76 H76A 0.9600 . ? C76 H76B 0.9600 . ? C76 H76C 0.9600 . ? C77 C78 1.472(10) . ? C77 H77A 0.9700 . ? C77 H77B 0.9700 . ? C78 H78A 0.9600 . ? C78 H78B 0.9600 . ? C78 H78C 0.9600 . ? C81 H81A 0.9600 . ? C81 H81B 0.9600 . ? C81 H81C 0.9600 . ? C82 H82A 0.9600 . ? C82 H82B 0.9600 . ? C82 H82C 0.9600 . ? C83 H83A 0.9600 . ? C83 H83B 0.9600 . ? C83 H83C 0.9600 . ? C84 H84A 0.9600 . ? C84 H84B 0.9600 . ? C84 H84C 0.9600 . ? C85 H85A 0.9600 . ? C85 H85B 0.9600 . ? C85 H85C 0.9600 . ? C86 H86A 0.9600 . ? C86 H86B 0.9600 . ? C86 H86C 0.9600 . ? C87 C88 1.361(12) . ? C87 H87A 0.9700 . ? C87 H87B 0.9700 . ? C88 H88A 0.9600 . ? C88 H88B 0.9600 . ? C88 H88C 0.9600 . ? C91 H91A 0.9600 . ? C91 H91B 0.9600 . ? C91 H91C 0.9600 . ? C92 H92A 0.9600 . ? C92 H92B 0.9600 . ? C92 H92C 0.9600 . ? C93 H93A 0.9600 . ? C93 H93B 0.9600 . ? C93 H93C 0.9600 . ? C94 H94A 0.9600 . ? C94 H94B 0.9600 . ? C94 H94C 0.9600 . ? C95 H95A 0.9600 . ? C95 H95B 0.9600 . ? C95 H95C 0.9600 . ? C96 H96A 0.9600 . ? C96 H96B 0.9600 . ? C96 H96C 0.9600 . ? C97 C98 1.441(12) . ? C97 H97A 0.9700 . ? C97 H97B 0.9700 . ? C98 H98A 0.9600 . ? C98 H98B 0.9600 . ? C98 H98C 0.9600 . ? C101 H10D 0.9600 . ? C101 H10E 0.9600 . ? C101 H10F 0.9600 . ? C102 H10G 0.9600 . ? C102 H10H 0.9600 . ? C102 H10I 0.9600 . ? C103 H10J 0.9600 . ? C103 H10K 0.9600 . ? C103 H10L 0.9600 . ? C104 H10M 0.9600 . ? C104 H10N 0.9600 . ? C104 H10O 0.9600 . ? C105 H10P 0.9600 . ? C105 H10Q 0.9600 . ? C105 H10R 0.9600 . ? C106 H10S 0.9600 . ? C106 H10T 0.9600 . ? C106 H10U 0.9600 . ? C107 C108 1.397(12) . ? C107 H10V 0.9700 . ? C107 H10W 0.9700 . ? C108 H10X 0.9600 . ? C108 H10Y 0.9600 . ? C108 H10Z 0.9600 . ? C111 H11A 0.9600 . ? C111 H11B 0.9600 . ? C111 H11C 0.9600 . ? C112 H11D 0.9600 . ? C112 H11E 0.9600 . ? C112 H11F 0.9600 . ? C113 H11G 0.9600 . ? C113 H11H 0.9600 . ? C113 H11I 0.9600 . ? C114 H11J 0.9600 . ? C114 H11K 0.9600 . ? C114 H11L 0.9600 . ? C115 H11M 0.9600 . ? C115 H11N 0.9600 . ? C115 H11O 0.9600 . ? C116 H11P 0.9600 . ? C116 H11Q 0.9600 . ? C116 H11R 0.9600 . ? C117 C118 1.336(14) . ? C117 H11S 0.9700 . ? C117 H11T 0.9700 . ? C118 H11U 0.9600 . ? C118 H11V 0.9600 . ? C118 H11W 0.9600 . ? C121 H12A 0.9600 . ? C121 H12B 0.9600 . ? C121 H12C 0.9600 . ? C122 H12D 0.9600 . ? C122 H12E 0.9600 . ? C122 H12F 0.9600 . ? C123 H12G 0.9600 . ? C123 H12H 0.9600 . ? C123 H12I 0.9600 . ? C124 H12J 0.9600 . ? C124 H12K 0.9600 . ? C124 H12L 0.9600 . ? C125 H12M 0.9600 . ? C125 H12N 0.9600 . ? C125 H12O 0.9600 . ? C126 H12P 0.9600 . ? C126 H12Q 0.9600 . ? C126 H12R 0.9600 . ? C127 C128 1.479(9) . ? C127 H12S 0.9700 . ? C127 H12T 0.9700 . ? C128 H12U 0.9600 . ? C128 H12V 0.9600 . ? C128 H12W 0.9600 . ? C1 C2 1.511(10) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.520(9) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.487(9) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.514(9) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.517(10) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C10 C20 1.528(10) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C20 C30 1.519(10) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C30 C40 1.498(9) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C40 C50 1.517(10) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C50 C60 1.515(10) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O44 Y1 O24 115.08(13) . . ? O44 Y1 O33 84.76(14) . . ? O24 Y1 O33 84.93(14) . . ? O44 Y1 O13 82.20(14) . . ? O24 Y1 O13 85.92(13) . . ? O33 Y1 O13 159.12(13) . . ? O44 Y1 O54 91.85(13) . . ? O24 Y1 O54 152.59(12) . . ? O33 Y1 O54 92.98(13) . . ? O13 Y1 O54 103.64(13) . . ? O44 Y1 O53 153.28(13) . . ? O24 Y1 O53 91.42(12) . . ? O33 Y1 O53 101.82(13) . . ? O13 Y1 O53 97.13(13) . . ? O54 Y1 O53 62.20(12) . . ? O34 Y2 O43 84.93(14) . . ? O34 Y2 O14 115.13(13) . . ? O43 Y2 O14 84.83(14) . . ? O34 Y2 O23 86.47(13) . . ? O43 Y2 O23 159.08(13) . . ? O14 Y2 O23 81.63(13) . . ? O34 Y2 O63 150.11(12) . . ? O43 Y2 O63 94.37(13) . . ? O14 Y2 O63 94.50(12) . . ? O23 Y2 O63 102.50(12) . . ? O34 Y2 O64 88.08(13) . . ? O43 Y2 O64 101.86(14) . . ? O14 Y2 O64 156.48(13) . . ? O23 Y2 O64 96.86(13) . . ? O63 Y2 O64 62.75(12) . . ? O14 P1 O13 114.3(2) . . ? O14 P1 O11 108.8(2) . . ? O13 P1 O11 110.7(2) . . ? O14 P1 O12 106.5(2) . . ? O13 P1 O12 109.9(2) . . ? O11 P1 O12 106.10(19) . . ? O24 P2 O23 113.5(2) . . ? O24 P2 O21 109.1(2) . . ? O23 P2 O21 111.3(2) . . ? O24 P2 O22 107.8(2) . . ? O23 P2 O22 109.9(2) . . ? O21 P2 O22 104.9(2) . . ? O34 P3 O33 113.8(2) . . ? O34 P3 O31 109.1(2) . . ? O33 P3 O31 111.4(2) . . ? O34 P3 O32 106.0(2) . . ? O33 P3 O32 110.1(2) . . ? O31 P3 O32 105.9(2) . . ? O43 P4 O44 113.7(2) . . ? O43 P4 O41 111.3(2) . . ? O44 P4 O41 109.0(2) . . ? O43 P4 O42 111.0(2) . . ? O44 P4 O42 106.3(2) . . ? O41 P4 O42 105.1(2) . . ? O53 P5 O54 106.03(19) . . ? O53 P5 O51 113.5(2) . . ? O54 P5 O51 112.6(2) . . ? O53 P5 O52 110.6(2) . . ? O54 P5 O52 112.6(2) . . ? O51 P5 O52 101.59(19) . . ? O63 P6 O64 106.03(19) . . ? O63 P6 O62 111.5(2) . . ? O64 P6 O62 110.8(2) . . ? O63 P6 O61 113.1(2) . . ? O64 P6 O61 114.2(2) . . ? O62 P6 O61 101.3(2) . . ? C77 O11 P1 121.4(4) . . ? C11 O12 P1 126.3(3) . . ? P1 O13 Y1 122.9(2) . . ? P1 O14 Y2 164.8(2) . . ? C87 O21 P2 124.0(5) . . ? C21 O22 P2 125.9(3) . . ? P2 O23 Y2 123.66(19) . . ? P2 O24 Y1 164.1(2) . . ? C97 O31 P3 123.8(4) . . ? C31 O32 P3 125.5(3) . . ? P3 O33 Y1 127.3(2) . . ? P3 O34 Y2 159.8(2) . . ? C107 O41 P4 123.9(4) . . ? C41 O42 P4 126.9(4) . . ? P4 O43 Y2 127.4(2) . . ? P4 O44 Y1 161.0(2) . . ? C117 O51 P5 119.0(5) . . ? C51 O52 P5 131.4(3) . . ? P5 O53 Y1 95.96(17) . . ? P5 O54 Y1 95.79(17) . . ? C127 O61 P6 119.3(4) . . ? C61 O62 P6 130.2(3) . . ? P6 O63 Y2 95.74(16) . . ? P6 O64 Y2 95.49(17) . . ? C12 C11 C16 122.3(5) . . ? C12 C11 O12 117.5(5) . . ? C16 C11 O12 120.0(5) . . ? C13 C12 C11 116.6(5) . . ? C13 C12 C17 118.1(5) . . ? C11 C12 C17 125.2(5) . . ? C14 C13 C12 122.6(6) . . ? C14 C13 H13A 118.7 . . ? C12 C13 H13A 118.7 . . ? C13 C14 C15 116.7(6) . . ? C13 C14 C19 119.6(6) . . ? C15 C14 C19 123.7(6) . . ? C16 C15 C14 124.5(6) . . ? C16 C15 H15A 117.8 . . ? C14 C15 H15A 117.8 . . ? C15 C16 C11 115.7(5) . . ? C15 C16 C18 119.1(5) . . ? C11 C16 C18 125.1(5) . . ? C73 C17 C71 110.9(7) . . ? C73 C17 C72 104.3(7) . . ? C71 C17 C72 107.0(6) . . ? C73 C17 C12 113.0(6) . . ? C71 C17 C12 109.8(6) . . ? C72 C17 C12 111.6(6) . . ? C74 C18 C75 106.2(5) . . ? C74 C18 C76 111.2(5) . . ? C75 C18 C76 105.7(5) . . ? C74 C18 C16 112.1(5) . . ? C75 C18 C16 108.8(5) . . ? C76 C18 C16 112.4(5) . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C26 C21 C22 122.9(5) . . ? C26 C21 O22 118.4(5) . . ? C22 C21 O22 118.6(5) . . ? C23 C22 C21 115.4(5) . . ? C23 C22 C27 119.0(5) . . ? C21 C22 C27 125.7(5) . . ? C24 C23 C22 124.3(6) . . ? C24 C23 H23A 117.9 . . ? C22 C23 H23A 117.9 . . ? C23 C24 C25 115.8(6) . . ? C23 C24 C29 121.9(6) . . ? C25 C24 C29 122.3(7) . . ? C24 C25 C26 124.7(6) . . ? C24 C25 H25A 117.6 . . ? C26 C25 H25A 117.6 . . ? C25 C26 C21 115.1(5) . . ? C25 C26 C28 119.2(5) . . ? C21 C26 C28 125.6(5) . . ? C82 C27 C83 106.3(5) . . ? C82 C27 C81 109.4(5) . . ? C83 C27 C81 107.0(5) . . ? C82 C27 C22 113.6(5) . . ? C83 C27 C22 109.9(5) . . ? C81 C27 C22 110.4(5) . . ? C26 C28 C85 109.4(7) . . ? C26 C28 C86 113.7(6) . . ? C85 C28 C86 109.5(7) . . ? C26 C28 C84 110.8(6) . . ? C85 C28 C84 108.1(7) . . ? C86 C28 C84 105.1(7) . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O32 C31 C36 119.7(4) . . ? O32 C31 C32 118.2(5) . . ? C36 C31 C32 122.1(5) . . ? C33 C32 C31 115.2(6) . . ? C33 C32 C37 118.5(6) . . ? C31 C32 C37 126.3(6) . . ? C34 C33 C32 123.4(6) . . ? C34 C33 H33A 118.3 . . ? C32 C33 H33A 118.3 . . ? C33 C34 C35 117.7(6) . . ? C33 C34 C39 120.2(6) . . ? C35 C34 C39 122.1(6) . . ? C36 C35 C34 123.8(6) . . ? C36 C35 H35A 118.1 . . ? C34 C35 H35A 118.1 . . ? C35 C36 C31 116.6(5) . . ? C35 C36 C38 118.6(5) . . ? C31 C36 C38 124.8(5) . . ? C92 C37 C32 110.7(6) . . ? C92 C37 C91 110.1(6) . . ? C32 C37 C91 108.9(6) . . ? C92 C37 C93 110.6(7) . . ? C32 C37 C93 112.9(6) . . ? C91 C37 C93 103.4(6) . . ? C95 C38 C94 110.8(4) . . ? C95 C38 C36 110.2(4) . . ? C94 C38 C36 115.1(4) . . ? C95 C38 C96 107.8(4) . . ? C94 C38 C96 103.8(5) . . ? C36 C38 C96 108.8(4) . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C42 C41 C46 123.1(5) . . ? C42 C41 O42 117.7(5) . . ? C46 C41 O42 119.2(5) . . ? C43 C42 C41 115.2(6) . . ? C43 C42 C47 119.0(6) . . ? C41 C42 C47 125.7(6) . . ? C44 C43 C42 122.7(6) . . ? C44 C43 H43A 118.7 . . ? C42 C43 H43A 118.7 . . ? C45 C44 C43 118.4(6) . . ? C45 C44 C49 121.0(7) . . ? C43 C44 C49 120.4(7) . . ? C44 C45 C46 122.8(6) . . ? C44 C45 H45A 118.6 . . ? C46 C45 H45A 118.6 . . ? C45 C46 C41 116.3(6) . . ? C45 C46 C48 118.7(6) . . ? C41 C46 C48 125.0(5) . . ? C102 C47 C101 112.2(7) . . ? C102 C47 C42 113.0(6) . . ? C101 C47 C42 109.2(6) . . ? C102 C47 C103 106.5(7) . . ? C101 C47 C103 108.3(7) . . ? C42 C47 C103 107.4(6) . . ? C104 C48 C105 108.4(6) . . ? C104 C48 C106 106.3(5) . . ? C105 C48 C106 108.4(5) . . ? C104 C48 C46 111.2(5) . . ? C105 C48 C46 112.9(5) . . ? C106 C48 C46 109.4(5) . . ? C44 C49 H49A 109.5 . . ? C44 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C44 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C56 C51 C52 123.9(5) . . ? C56 C51 O52 118.3(5) . . ? C52 C51 O52 117.6(5) . . ? C53 C52 C51 115.1(6) . . ? C53 C52 C57 119.9(5) . . ? C51 C52 C57 125.0(5) . . ? C54 C53 C52 123.7(6) . . ? C54 C53 H53A 118.1 . . ? C52 C53 H53A 118.1 . . ? C53 C54 C55 118.2(6) . . ? C53 C54 C59 122.8(7) . . ? C55 C54 C59 119.0(7) . . ? C54 C55 C56 122.6(6) . . ? C54 C55 H55A 118.7 . . ? C56 C55 H55A 118.7 . . ? C55 C56 C51 115.7(5) . . ? C55 C56 C58 118.6(5) . . ? C51 C56 C58 125.7(5) . . ? C113 C57 C52 113.4(6) . . ? C113 C57 C111 110.1(5) . . ? C52 C57 C111 110.8(5) . . ? C113 C57 C112 106.7(5) . . ? C52 C57 C112 110.2(5) . . ? C111 C57 C112 105.3(6) . . ? C114 C58 C115 107.7(6) . . ? C114 C58 C56 110.1(5) . . ? C115 C58 C56 109.9(5) . . ? C114 C58 C116 111.5(5) . . ? C115 C58 C116 105.5(5) . . ? C56 C58 C116 111.9(5) . . ? C54 C59 H59A 109.5 . . ? C54 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C54 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C66 C61 C62 123.4(5) . . ? C66 C61 O62 118.6(5) . . ? C62 C61 O62 117.8(5) . . ? C61 C62 C63 114.8(6) . . ? C61 C62 C67 125.7(5) . . ? C63 C62 C67 119.5(6) . . ? C64 C63 C62 123.6(6) . . ? C64 C63 H63A 118.2 . . ? C62 C63 H63A 118.2 . . ? C63 C64 C65 118.3(6) . . ? C63 C64 C69 119.3(7) . . ? C65 C64 C69 122.2(7) . . ? C64 C65 C66 123.1(6) . . ? C64 C65 H65A 118.5 . . ? C66 C65 H65A 118.5 . . ? C61 C66 C65 115.7(6) . . ? C61 C66 C68 124.5(5) . . ? C65 C66 C68 119.8(5) . . ? C62 C67 C122 110.3(5) . . ? C62 C67 C121 111.5(5) . . ? C122 C67 C121 105.4(5) . . ? C62 C67 C123 111.7(5) . . ? C122 C67 C123 106.7(5) . . ? C121 C67 C123 110.9(5) . . ? C124 C68 C126 110.0(6) . . ? C124 C68 C125 106.7(6) . . ? C126 C68 C125 105.1(6) . . ? C124 C68 C66 111.5(6) . . ? C126 C68 C66 112.0(6) . . ? C125 C68 C66 111.1(6) . . ? C64 C69 H69A 109.5 . . ? C64 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C64 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C17 C71 H71A 109.5 . . ? C17 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C17 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C17 C72 H72A 109.5 . . ? C17 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C17 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C17 C73 H73A 109.5 . . ? C17 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C17 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C18 C74 H74A 109.5 . . ? C18 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C18 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C18 C75 H75A 109.5 . . ? C18 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C18 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C18 C76 H76A 109.5 . . ? C18 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C18 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? O11 C77 C78 110.1(6) . . ? O11 C77 H77A 109.6 . . ? C78 C77 H77A 109.6 . . ? O11 C77 H77B 109.6 . . ? C78 C77 H77B 109.6 . . ? H77A C77 H77B 108.2 . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C27 C81 H81A 109.5 . . ? C27 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C27 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C27 C82 H82A 109.5 . . ? C27 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C27 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C27 C83 H83A 109.5 . . ? C27 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C27 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C28 C84 H84A 109.5 . . ? C28 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C28 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C28 C85 H85A 109.5 . . ? C28 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C28 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? C28 C86 H86A 109.5 . . ? C28 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C28 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C88 C87 O21 117.5(9) . . ? C88 C87 H87A 107.9 . . ? O21 C87 H87A 107.9 . . ? C88 C87 H87B 107.9 . . ? O21 C87 H87B 107.9 . . ? H87A C87 H87B 107.2 . . ? C87 C88 H88A 109.5 . . ? C87 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C87 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C37 C91 H91A 109.5 . . ? C37 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C37 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C37 C92 H92A 109.5 . . ? C37 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C37 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C37 C93 H93A 109.5 . . ? C37 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C37 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C38 C94 H94A 109.5 . . ? C38 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? C38 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? C38 C95 H95A 109.5 . . ? C38 C95 H95B 109.5 . . ? H95A C95 H95B 109.5 . . ? C38 C95 H95C 109.5 . . ? H95A C95 H95C 109.5 . . ? H95B C95 H95C 109.5 . . ? C38 C96 H96A 109.5 . . ? C38 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? C38 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? C98 C97 O31 111.6(8) . . ? C98 C97 H97A 109.3 . . ? O31 C97 H97A 109.3 . . ? C98 C97 H97B 109.3 . . ? O31 C97 H97B 109.3 . . ? H97A C97 H97B 108.0 . . ? C97 C98 H98A 109.5 . . ? C97 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? C97 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? C47 C101 H10D 109.5 . . ? C47 C101 H10E 109.5 . . ? H10D C101 H10E 109.5 . . ? C47 C101 H10F 109.5 . . ? H10D C101 H10F 109.5 . . ? H10E C101 H10F 109.5 . . ? C47 C102 H10G 109.5 . . ? C47 C102 H10H 109.5 . . ? H10G C102 H10H 109.5 . . ? C47 C102 H10I 109.5 . . ? H10G C102 H10I 109.5 . . ? H10H C102 H10I 109.5 . . ? C47 C103 H10J 109.5 . . ? C47 C103 H10K 109.5 . . ? H10J C103 H10K 109.5 . . ? C47 C103 H10L 109.5 . . ? H10J C103 H10L 109.5 . . ? H10K C103 H10L 109.5 . . ? C48 C104 H10M 109.5 . . ? C48 C104 H10N 109.5 . . ? H10M C104 H10N 109.5 . . ? C48 C104 H10O 109.5 . . ? H10M C104 H10O 109.5 . . ? H10N C104 H10O 109.5 . . ? C48 C105 H10P 109.5 . . ? C48 C105 H10Q 109.5 . . ? H10P C105 H10Q 109.5 . . ? C48 C105 H10R 109.5 . . ? H10P C105 H10R 109.5 . . ? H10Q C105 H10R 109.5 . . ? C48 C106 H10S 109.5 . . ? C48 C106 H10T 109.5 . . ? H10S C106 H10T 109.5 . . ? C48 C106 H10U 109.5 . . ? H10S C106 H10U 109.5 . . ? H10T C106 H10U 109.5 . . ? C108 C107 O41 111.5(8) . . ? C108 C107 H10V 109.3 . . ? O41 C107 H10V 109.3 . . ? C108 C107 H10W 109.3 . . ? O41 C107 H10W 109.3 . . ? H10V C107 H10W 108.0 . . ? C107 C108 H10X 109.5 . . ? C107 C108 H10Y 109.5 . . ? H10X C108 H10Y 109.5 . . ? C107 C108 H10Z 109.5 . . ? H10X C108 H10Z 109.5 . . ? H10Y C108 H10Z 109.5 . . ? C57 C111 H11A 109.5 . . ? C57 C111 H11B 109.5 . . ? H11A C111 H11B 109.5 . . ? C57 C111 H11C 109.5 . . ? H11A C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? C57 C112 H11D 109.5 . . ? C57 C112 H11E 109.5 . . ? H11D C112 H11E 109.5 . . ? C57 C112 H11F 109.5 . . ? H11D C112 H11F 109.5 . . ? H11E C112 H11F 109.5 . . ? C57 C113 H11G 109.5 . . ? C57 C113 H11H 109.5 . . ? H11G C113 H11H 109.5 . . ? C57 C113 H11I 109.5 . . ? H11G C113 H11I 109.5 . . ? H11H C113 H11I 109.5 . . ? C58 C114 H11J 109.5 . . ? C58 C114 H11K 109.5 . . ? H11J C114 H11K 109.5 . . ? C58 C114 H11L 109.5 . . ? H11J C114 H11L 109.5 . . ? H11K C114 H11L 109.5 . . ? C58 C115 H11M 109.5 . . ? C58 C115 H11N 109.5 . . ? H11M C115 H11N 109.5 . . ? C58 C115 H11O 109.5 . . ? H11M C115 H11O 109.5 . . ? H11N C115 H11O 109.5 . . ? C58 C116 H11P 109.5 . . ? C58 C116 H11Q 109.5 . . ? H11P C116 H11Q 109.5 . . ? C58 C116 H11R 109.5 . . ? H11P C116 H11R 109.5 . . ? H11Q C116 H11R 109.5 . . ? C118 C117 O51 109.2(10) . . ? C118 C117 H11S 109.8 . . ? O51 C117 H11S 109.8 . . ? C118 C117 H11T 109.8 . . ? O51 C117 H11T 109.8 . . ? H11S C117 H11T 108.3 . . ? C117 C118 H11U 109.5 . . ? C117 C118 H11V 109.5 . . ? H11U C118 H11V 109.5 . . ? C117 C118 H11W 109.5 . . ? H11U C118 H11W 109.5 . . ? H11V C118 H11W 109.5 . . ? C67 C121 H12A 109.5 . . ? C67 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? C67 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? C67 C122 H12D 109.5 . . ? C67 C122 H12E 109.5 . . ? H12D C122 H12E 109.5 . . ? C67 C122 H12F 109.5 . . ? H12D C122 H12F 109.5 . . ? H12E C122 H12F 109.5 . . ? C67 C123 H12G 109.5 . . ? C67 C123 H12H 109.5 . . ? H12G C123 H12H 109.5 . . ? C67 C123 H12I 109.5 . . ? H12G C123 H12I 109.5 . . ? H12H C123 H12I 109.5 . . ? C68 C124 H12J 109.5 . . ? C68 C124 H12K 109.5 . . ? H12J C124 H12K 109.5 . . ? C68 C124 H12L 109.5 . . ? H12J C124 H12L 109.5 . . ? H12K C124 H12L 109.5 . . ? C68 C125 H12M 109.5 . . ? C68 C125 H12N 109.5 . . ? H12M C125 H12N 109.5 . . ? C68 C125 H12O 109.5 . . ? H12M C125 H12O 109.5 . . ? H12N C125 H12O 109.5 . . ? C68 C126 H12P 109.5 . . ? C68 C126 H12Q 109.5 . . ? H12P C126 H12Q 109.5 . . ? C68 C126 H12R 109.5 . . ? H12P C126 H12R 109.5 . . ? H12Q C126 H12R 109.5 . . ? O61 C127 C128 109.1(6) . . ? O61 C127 H12S 109.9 . . ? C128 C127 H12S 109.9 . . ? O61 C127 H12T 109.9 . . ? C128 C127 H12T 109.9 . . ? H12S C127 H12T 108.3 . . ? C127 C128 H12U 109.5 . . ? C127 C128 H12V 109.5 . . ? H12U C128 H12V 109.5 . . ? C127 C128 H12W 109.5 . . ? H12U C128 H12W 109.5 . . ? H12V C128 H12W 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 C3 108.9(12) . . ? C1 C2 H2A 109.9 . . ? C3 C2 H2A 109.9 . . ? C1 C2 H2B 109.9 . . ? C3 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C4 C3 C2 112.2(12) . . ? C4 C3 H3A 109.2 . . ? C2 C3 H3A 109.2 . . ? C4 C3 H3B 109.2 . . ? C2 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C3 C4 C5 113.2(12) . . ? C3 C4 H4A 108.9 . . ? C5 C4 H4A 108.9 . . ? C3 C4 H4B 108.9 . . ? C5 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C6 C5 C4 108.4(12) . . ? C6 C5 H5A 110.0 . . ? C4 C5 H5A 110.0 . . ? C6 C5 H5B 110.0 . . ? C4 C5 H5B 110.0 . . ? H5A C5 H5B 108.4 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C20 C10 H10A 109.5 . . ? C20 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C20 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C30 C20 C10 103.1(11) . . ? C30 C20 H20A 111.1 . . ? C10 C20 H20A 111.1 . . ? C30 C20 H20B 111.1 . . ? C10 C20 H20B 111.1 . . ? H20A C20 H20B 109.1 . . ? C40 C30 C20 115.7(12) . . ? C40 C30 H30A 108.4 . . ? C20 C30 H30A 108.4 . . ? C40 C30 H30B 108.4 . . ? C20 C30 H30B 108.4 . . ? H30A C30 H30B 107.4 . . ? C30 C40 C50 111.7(12) . . ? C30 C40 H40A 109.3 . . ? C50 C40 H40A 109.3 . . ? C30 C40 H40B 109.3 . . ? C50 C40 H40B 109.3 . . ? H40A C40 H40B 107.9 . . ? C40 C50 C60 110.3(12) . . ? C40 C50 H50A 109.6 . . ? C60 C50 H50A 109.6 . . ? C40 C50 H50B 109.6 . . ? C60 C50 H50B 109.6 . . ? H50A C50 H50B 108.1 . . ? C50 C60 H60A 109.5 . . ? C50 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C50 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.928 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.089