# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Peter Wolczanski' _publ_contact_author_email PTW2@CORNELL.EDU loop_ _publ_author_name P.Wolczanski E.B.Hulley E.Lobkovsky # Attachment 'Ta2P2(3)Aug26.cif' data_eh2 _database_code_depnum_ccdc_archive 'CCDC 715086' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H162 O6 P2 Si6 Ta2' _chemical_formula_sum 'C72 H162 O6 P2 Si6 Ta2' _chemical_formula_weight 1716.40 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' Si Si 0.0817 0.0704 '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' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.9611(7) _cell_length_b 13.1197(7) _cell_length_c 16.0871(9) _cell_angle_alpha 67.135(3) _cell_angle_beta 68.391(3) _cell_angle_gamma 61.970(2) _cell_volume 2166.2(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3542 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 902 _exptl_absorpt_coefficient_mu 2.687 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6156 _exptl_absorpt_correction_T_max 0.9359 _exptl_absorpt_process_details SADABS _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 X8 APEX II diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37459 _diffrn_reflns_av_R_equivalents 0.0924 _diffrn_reflns_av_sigmaI/netI 0.0913 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 26.52 _reflns_number_total 8957 _reflns_number_gt 7095 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT+' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All but one siloxo groups are disordered. Some carbon atoms of the methyl groups were refined isotropically. Despite the restrictions imposed on the disordered tertiary butyl groups, their geometry is sometimes is on the edge of normal values. In particular, Si(1)-C(2') and Si(1)-C(3) are on the edge of normal. In addition, C(15') has been refined isotropically and C(7') and C(22') have elongated ellipsoids; these issues result from attempts to properly model the tertiary-butyl group disorder. ; _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^)+(0.0466P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8957 _refine_ls_number_parameters 679 _refine_ls_number_restraints 1576 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1054 _refine_ls_wR_factor_gt 0.0896 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 0.949 _refine_ls_shift/su_max 0.155 _refine_ls_shift/su_mean 0.017 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 Ta1 Ta 0.457842(12) 0.082765(12) 0.321490(10) 0.01768(4) Uani 1 1 d . . . P1 P 0.42078(9) 0.07103(9) 0.47651(7) 0.0303(3) Uani 1 1 d . . . Si1 Si 0.48372(10) -0.19078(9) 0.30663(8) 0.0347(3) Uani 1 1 d . . . Si2 Si 0.72023(8) 0.14230(9) 0.19051(7) 0.0227(2) Uani 1 1 d . . . Si3 Si 0.18604(8) 0.32633(9) 0.28251(7) 0.0206(2) Uani 1 1 d . . . O1 O 0.4780(2) -0.0610(2) 0.30692(17) 0.0372(7) Uani 1 1 d . A . O2 O 0.59825(19) 0.1110(2) 0.25273(17) 0.0289(7) Uani 1 1 d . B . O3 O 0.31779(18) 0.2102(2) 0.29383(16) 0.0215(6) Uani 1 1 d . C . C1 C 0.5875(3) -0.3149(3) 0.3824(2) 0.0244(9) Uani 1 1 d D A . C4 C 0.5269(4) -0.3221(3) 0.4845(2) 0.0402(11) Uani 1 1 d D . . H4A H 0.5821 -0.3874 0.5226 0.060 Uiso 1 1 calc R A . H4B H 0.4541 -0.3373 0.4996 0.060 Uiso 1 1 calc R . . H4C H 0.5057 -0.2463 0.4968 0.060 Uiso 1 1 calc R . . C5 C 0.6272(3) -0.4378(3) 0.3661(3) 0.0390(12) Uani 1 1 d D . . H5A H 0.6807 -0.4997 0.4068 0.059 Uiso 1 1 calc R A . H5B H 0.6698 -0.4359 0.3014 0.059 Uiso 1 1 calc R . . H5C H 0.5564 -0.4558 0.3799 0.059 Uiso 1 1 calc R . . C6 C 0.7000(3) -0.2930(4) 0.3671(4) 0.0612(13) Uani 1 1 d D . . H6A H 0.7514 -0.3594 0.4076 0.092 Uiso 1 1 calc R A . H6B H 0.6765 -0.2180 0.3817 0.092 Uiso 1 1 calc R . . H6C H 0.7440 -0.2875 0.3023 0.092 Uiso 1 1 calc R . . C2 C 0.3375(5) -0.1773(5) 0.3278(4) 0.0267(18) Uani 0.523(4) 1 d PDU A 1 C7 C 0.2687(6) -0.1237(6) 0.4106(4) 0.0331(19) Uani 0.523(4) 1 d PDU A 1 H7A H 0.1844 -0.1133 0.4258 0.050 Uiso 0.523(4) 1 calc PR A 1 H7B H 0.2734 -0.0458 0.3952 0.050 Uiso 0.523(4) 1 calc PR A 1 H7C H 0.3040 -0.1775 0.4640 0.050 Uiso 0.523(4) 1 calc PR A 1 C8 C 0.2793(6) -0.0930(6) 0.2450(4) 0.035(2) Uani 0.523(4) 1 d PDU A 1 H8A H 0.1965 -0.0872 0.2604 0.052 Uiso 0.523(4) 1 calc PR A 1 H8B H 0.3251 -0.1249 0.1906 0.052 Uiso 0.523(4) 1 calc PR A 1 H8C H 0.2793 -0.0134 0.2313 0.052 Uiso 0.523(4) 1 calc PR A 1 C9 C 0.3223(6) -0.2966(5) 0.3549(5) 0.033(2) Uani 0.523(4) 1 d PDU A 1 H9A H 0.2372 -0.2811 0.3663 0.049 Uiso 0.523(4) 1 calc PR A 1 H9B H 0.3515 -0.3487 0.4113 0.049 Uiso 0.523(4) 1 calc PR A 1 H9C H 0.3685 -0.3359 0.3045 0.049 Uiso 0.523(4) 1 calc PR A 1 C2' C 0.3126(5) -0.1932(5) 0.3755(4) 0.0161(16) Uani 0.477(4) 1 d PDU A 2 C7' C 0.2631(6) -0.1579(6) 0.4682(4) 0.0226(19) Uani 0.477(4) 1 d PDU A 2 H7'A H 0.1829 -0.1604 0.4968 0.034 Uiso 0.477(4) 1 calc PR A 2 H7'B H 0.2582 -0.0768 0.4563 0.034 Uiso 0.477(4) 1 calc PR A 2 H7'C H 0.3168 -0.2142 0.5100 0.034 Uiso 0.477(4) 1 calc PR A 2 C8' C 0.2184(6) -0.1072(6) 0.3169(5) 0.028(2) Uani 0.477(4) 1 d PDU A 2 H8'A H 0.1399 -0.1111 0.3523 0.042 Uiso 0.477(4) 1 calc PR A 2 H8'B H 0.2419 -0.1307 0.2597 0.042 Uiso 0.477(4) 1 calc PR A 2 H8'C H 0.2134 -0.0253 0.3015 0.042 Uiso 0.477(4) 1 calc PR A 2 C9' C 0.3108(7) -0.3188(5) 0.3993(5) 0.030(2) Uani 0.477(4) 1 d PDU A 2 H9'A H 0.2295 -0.3164 0.4318 0.045 Uiso 0.477(4) 1 calc PR A 2 H9'B H 0.3666 -0.3770 0.4392 0.045 Uiso 0.477(4) 1 calc PR A 2 H9'C H 0.3351 -0.3424 0.3420 0.045 Uiso 0.477(4) 1 calc PR A 2 C3 C 0.5827(5) -0.2146(5) 0.1763(4) 0.0249(18) Uani 0.524(3) 1 d PDU A 1 C10 C 0.5425(6) -0.0951(6) 0.1039(5) 0.036(2) Uani 0.524(3) 1 d PDU A 1 H10A H 0.5892 -0.1053 0.0420 0.054 Uiso 0.524(3) 1 calc PR A 1 H10B H 0.5556 -0.0351 0.1163 0.054 Uiso 0.524(3) 1 calc PR A 1 H10C H 0.4570 -0.0686 0.1072 0.054 Uiso 0.524(3) 1 calc PR A 1 C11 C 0.7203(5) -0.2594(6) 0.1609(5) 0.0320(19) Uani 0.524(3) 1 d PDU A 1 H11A H 0.7586 -0.2667 0.0972 0.048 Uiso 0.524(3) 1 calc PR A 1 H11B H 0.7495 -0.3377 0.2044 0.048 Uiso 0.524(3) 1 calc PR A 1 H11C H 0.7399 -0.2023 0.1711 0.048 Uiso 0.524(3) 1 calc PR A 1 C12 C 0.5573(6) -0.3048(5) 0.1547(5) 0.0353(18) Uani 0.524(3) 1 d PDU A 1 H12A H 0.6042 -0.3150 0.0928 0.053 Uiso 0.524(3) 1 calc PR A 1 H12B H 0.4716 -0.2744 0.1568 0.053 Uiso 0.524(3) 1 calc PR A 1 H12C H 0.5800 -0.3820 0.2008 0.053 Uiso 0.524(3) 1 calc PR A 1 C3' C 0.5038(5) -0.1765(5) 0.1839(5) 0.0232(19) Uani 0.476(3) 1 d PDU A 2 C10' C 0.4278(6) -0.0535(5) 0.1316(5) 0.0234(19) Uani 0.476(3) 1 d PDU A 2 H10D H 0.4437 -0.0526 0.0669 0.035 Uiso 0.476(3) 1 calc PR A 2 H10E H 0.4483 0.0081 0.1340 0.035 Uiso 0.476(3) 1 calc PR A 2 H10F H 0.3425 -0.0374 0.1605 0.035 Uiso 0.476(3) 1 calc PR A 2 C11' C 0.6358(5) -0.1927(7) 0.1402(6) 0.030(2) Uani 0.476(3) 1 d PDU A 2 H11D H 0.6532 -0.1856 0.0740 0.045 Uiso 0.476(3) 1 calc PR A 2 H11E H 0.6876 -0.2720 0.1705 0.045 Uiso 0.476(3) 1 calc PR A 2 H11F H 0.6509 -0.1310 0.1483 0.045 Uiso 0.476(3) 1 calc PR A 2 C12' C 0.4838(6) -0.2750(5) 0.1694(5) 0.0258(19) Uani 0.476(3) 1 d PDU A 2 H12D H 0.4957 -0.2629 0.1030 0.039 Uiso 0.476(3) 1 calc PR A 2 H12E H 0.4019 -0.2708 0.2012 0.039 Uiso 0.476(3) 1 calc PR A 2 H12F H 0.5413 -0.3537 0.1947 0.039 Uiso 0.476(3) 1 calc PR A 2 C13 C 0.6990(5) 0.1946(5) 0.0727(4) 0.0245(18) Uani 0.508(4) 1 d PDU B 1 C16 C 0.6602(5) 0.1149(5) 0.0525(5) 0.0287(18) Uani 0.508(4) 1 d PDU B 1 H16A H 0.6502 0.1468 -0.0114 0.043 Uiso 0.508(4) 1 calc PR B 1 H16B H 0.5839 0.1133 0.0953 0.043 Uiso 0.508(4) 1 calc PR B 1 H16C H 0.7217 0.0335 0.0604 0.043 Uiso 0.508(4) 1 calc PR B 1 C17 C 0.5986(6) 0.3210(5) 0.0579(5) 0.035(2) Uani 0.508(4) 1 d PDU B 1 H17A H 0.5879 0.3486 -0.0055 0.052 Uiso 0.508(4) 1 calc PR B 1 H17B H 0.6209 0.3764 0.0678 0.052 Uiso 0.508(4) 1 calc PR B 1 H17C H 0.5234 0.3180 0.1020 0.052 Uiso 0.508(4) 1 calc PR B 1 C18 C 0.8142(5) 0.2034(6) -0.0006(5) 0.0236(19) Uani 0.508(4) 1 d PDU B 1 H18A H 0.7993 0.2320 -0.0628 0.035 Uiso 0.508(4) 1 calc PR B 1 H18B H 0.8795 0.1243 0.0063 0.035 Uiso 0.508(4) 1 calc PR B 1 H18C H 0.8367 0.2595 0.0083 0.035 Uiso 0.508(4) 1 calc PR B 1 C13' C 0.7427(5) 0.1459(5) 0.0603(5) 0.0216(19) Uani 0.492(4) 1 d PDU B 2 C16' C 0.7922(6) 0.0167(5) 0.0528(5) 0.030(2) Uani 0.492(4) 1 d PDU B 2 H16D H 0.8035 0.0181 -0.0112 0.045 Uiso 0.492(4) 1 calc PR B 2 H16E H 0.7351 -0.0212 0.0940 0.045 Uiso 0.492(4) 1 calc PR B 2 H16F H 0.8693 -0.0288 0.0710 0.045 Uiso 0.492(4) 1 calc PR B 2 C17' C 0.6235(5) 0.2090(7) 0.0281(5) 0.034(2) Uani 0.492(4) 1 d PDU B 2 H17D H 0.6400 0.2082 -0.0362 0.052 Uiso 0.492(4) 1 calc PR B 2 H17E H 0.5855 0.2920 0.0323 0.052 Uiso 0.492(4) 1 calc PR B 2 H17F H 0.5697 0.1670 0.0678 0.052 Uiso 0.492(4) 1 calc PR B 2 C18' C 0.8317(6) 0.2034(8) -0.0119(7) 0.044(3) Uani 0.492(4) 1 d PDU B 2 H18D H 0.8377 0.2016 -0.0739 0.065 Uiso 0.492(4) 1 calc PR B 2 H18E H 0.9109 0.1585 0.0029 0.065 Uiso 0.492(4) 1 calc PR B 2 H18F H 0.8027 0.2865 -0.0103 0.065 Uiso 0.492(4) 1 calc PR B 2 C14 C 0.7143(5) 0.2518(5) 0.2433(4) 0.0213(18) Uani 0.474(4) 1 d PDU B 1 C19 C 0.5845(6) 0.3402(6) 0.2642(6) 0.032(2) Uani 0.474(4) 1 d PDU B 1 H19A H 0.5805 0.3971 0.2917 0.048 Uiso 0.474(4) 1 calc PR B 1 H19B H 0.5335 0.2963 0.3077 0.048 Uiso 0.474(4) 1 calc PR B 1 H19C H 0.5563 0.3836 0.2066 0.048 Uiso 0.474(4) 1 calc PR B 1 C20 C 0.7568(6) 0.1960(7) 0.3349(4) 0.034(2) Uani 0.474(4) 1 d PDU B 1 H20A H 0.7506 0.2594 0.3565 0.051 Uiso 0.474(4) 1 calc PR B 1 H20B H 0.8405 0.1396 0.3245 0.051 Uiso 0.474(4) 1 calc PR B 1 H20C H 0.7062 0.1536 0.3819 0.051 Uiso 0.474(4) 1 calc PR B 1 C21 C 0.7893(6) 0.3264(6) 0.1731(6) 0.026(3) Uani 0.474(4) 1 d PDU B 1 H21A H 0.7856 0.3825 0.2013 0.039 Uiso 0.474(4) 1 calc PR B 1 H21B H 0.7566 0.3712 0.1175 0.039 Uiso 0.474(4) 1 calc PR B 1 H21C H 0.8729 0.2727 0.1560 0.039 Uiso 0.474(4) 1 calc PR B 1 C14' C 0.6905(5) 0.3040(5) 0.1874(4) 0.0302(18) Uani 0.526(4) 1 d PDU B 2 C19' C 0.6033(6) 0.4041(6) 0.1261(5) 0.039(2) Uani 0.526(4) 1 d PDU B 2 H19D H 0.5919 0.4823 0.1285 0.059 Uiso 0.526(4) 1 calc PR B 2 H19E H 0.5258 0.3954 0.1491 0.059 Uiso 0.526(4) 1 calc PR B 2 H19F H 0.6370 0.3980 0.0620 0.059 Uiso 0.526(4) 1 calc PR B 2 C20' C 0.6281(7) 0.3195(7) 0.2860(4) 0.042(2) Uani 0.526(4) 1 d PDU B 2 H20D H 0.6113 0.4004 0.2863 0.063 Uiso 0.526(4) 1 calc PR B 2 H20E H 0.6807 0.2607 0.3282 0.063 Uiso 0.526(4) 1 calc PR B 2 H20F H 0.5527 0.3073 0.3063 0.063 Uiso 0.526(4) 1 calc PR B 2 C21' C 0.8059(6) 0.3310(8) 0.1549(7) 0.044(3) Uani 0.526(4) 1 d PDU B 2 H21D H 0.7842 0.4132 0.1552 0.067 Uiso 0.526(4) 1 calc PR B 2 H21E H 0.8469 0.3216 0.0920 0.067 Uiso 0.526(4) 1 calc PR B 2 H21F H 0.8595 0.2751 0.1970 0.067 Uiso 0.526(4) 1 calc PR B 2 C15 C 0.8612(5) -0.0086(5) 0.2140(4) 0.0306(18) Uani 0.558(4) 1 d PDU B 1 C22 C 0.8538(6) -0.0768(7) 0.3157(4) 0.044(2) Uani 0.558(4) 1 d PDU B 1 H22A H 0.9264 -0.1499 0.3219 0.066 Uiso 0.558(4) 1 calc PR B 1 H22B H 0.7832 -0.0981 0.3401 0.066 Uiso 0.558(4) 1 calc PR B 1 H22C H 0.8472 -0.0265 0.3507 0.066 Uiso 0.558(4) 1 calc PR B 1 C23 C 0.8749(6) -0.0936(5) 0.1623(5) 0.0396(19) Uani 0.558(4) 1 d PDU B 1 H23A H 0.9446 -0.1682 0.1743 0.059 Uiso 0.558(4) 1 calc PR B 1 H23B H 0.8865 -0.0551 0.0956 0.059 Uiso 0.558(4) 1 calc PR B 1 H23C H 0.8024 -0.1114 0.1843 0.059 Uiso 0.558(4) 1 calc PR B 1 C24 C 0.9741(5) 0.0220(6) 0.1724(6) 0.039(3) Uani 0.558(4) 1 d PDU B 1 H24A H 1.0452 -0.0513 0.1835 0.059 Uiso 0.558(4) 1 calc PR B 1 H24B H 0.9673 0.0786 0.2017 0.059 Uiso 0.558(4) 1 calc PR B 1 H24C H 0.9816 0.0581 0.1055 0.059 Uiso 0.558(4) 1 calc PR B 1 C15' C 0.8467(5) 0.0262(5) 0.2425(4) 0.0168(19) Uiso 0.442(4) 1 d PDU B 2 C22' C 0.8368(6) 0.0481(7) 0.3322(4) 0.0246(19) Uani 0.442(4) 1 d PDU B 2 H22D H 0.9041 -0.0141 0.3599 0.037 Uiso 0.442(4) 1 calc PR B 2 H22E H 0.7610 0.0458 0.3755 0.037 Uiso 0.442(4) 1 calc PR B 2 H22F H 0.8390 0.1267 0.3186 0.037 Uiso 0.442(4) 1 calc PR B 2 C23' C 0.8371(6) -0.0949(5) 0.2678(5) 0.020(2) Uani 0.442(4) 1 d PDU B 2 H23D H 0.9036 -0.1583 0.2959 0.030 Uiso 0.442(4) 1 calc PR B 2 H23E H 0.8409 -0.1106 0.2117 0.030 Uiso 0.442(4) 1 calc PR B 2 H23F H 0.7606 -0.0933 0.3120 0.030 Uiso 0.442(4) 1 calc PR B 2 C24' C 0.9757(6) 0.0119(9) 0.1834(6) 0.027(3) Uani 0.442(4) 1 d PDU B 2 H24D H 1.0341 -0.0525 0.2191 0.041 Uiso 0.442(4) 1 calc PR B 2 H24E H 0.9865 0.0870 0.1669 0.041 Uiso 0.442(4) 1 calc PR B 2 H24F H 0.9878 -0.0078 0.1268 0.041 Uiso 0.442(4) 1 calc PR B 2 C25 C 0.1995(5) 0.4668(5) 0.2838(4) 0.0306(19) Uani 0.553(4) 1 d PDU C 1 C28 C 0.2536(6) 0.4393(6) 0.3633(5) 0.042(2) Uani 0.553(4) 1 d PDU C 1 H28A H 0.2595 0.5116 0.3624 0.063 Uiso 0.553(4) 1 calc PR C 1 H28B H 0.3339 0.3759 0.3563 0.063 Uiso 0.553(4) 1 calc PR C 1 H28C H 0.2023 0.4129 0.4224 0.063 Uiso 0.553(4) 1 calc PR C 1 C29 C 0.2842(6) 0.5087(6) 0.1934(5) 0.038(2) Uani 0.553(4) 1 d PDU C 1 H29A H 0.2902 0.5795 0.1952 0.057 Uiso 0.553(4) 1 calc PR C 1 H29B H 0.2520 0.5287 0.1402 0.057 Uiso 0.553(4) 1 calc PR C 1 H29C H 0.3640 0.4444 0.1875 0.057 Uiso 0.553(4) 1 calc PR C 1 C30 C 0.0784(5) 0.5736(6) 0.2906(6) 0.039(3) Uani 0.553(4) 1 d PDU C 1 H30A H 0.0901 0.6420 0.2910 0.058 Uiso 0.553(4) 1 calc PR C 1 H30B H 0.0222 0.5517 0.3480 0.058 Uiso 0.553(4) 1 calc PR C 1 H30C H 0.0458 0.5952 0.2373 0.058 Uiso 0.553(4) 1 calc PR C 1 C25' C 0.1876(5) 0.4437(7) 0.3227(5) 0.024(2) Uani 0.447(4) 1 d PDU C 2 C28' C 0.1653(7) 0.4123(7) 0.4284(4) 0.033(2) Uani 0.447(4) 1 d PDU C 2 H28D H 0.1660 0.4755 0.4460 0.049 Uiso 0.447(4) 1 calc PR C 2 H28E H 0.2285 0.3361 0.4499 0.049 Uiso 0.447(4) 1 calc PR C 2 H28F H 0.0871 0.4051 0.4568 0.049 Uiso 0.447(4) 1 calc PR C 2 C29' C 0.3142(5) 0.4481(7) 0.2819(6) 0.033(2) Uani 0.447(4) 1 d PDU C 2 H29D H 0.3174 0.5085 0.3013 0.049 Uiso 0.447(4) 1 calc PR C 2 H29E H 0.3312 0.4691 0.2141 0.049 Uiso 0.447(4) 1 calc PR C 2 H29F H 0.3741 0.3696 0.3044 0.049 Uiso 0.447(4) 1 calc PR C 2 C30' C 0.0984(8) 0.5708(8) 0.2875(7) 0.047(4) Uani 0.447(4) 1 d PDU C 2 H30D H 0.1032 0.6271 0.3106 0.070 Uiso 0.447(4) 1 calc PR C 2 H30E H 0.0167 0.5719 0.3100 0.070 Uiso 0.447(4) 1 calc PR C 2 H30F H 0.1185 0.5944 0.2196 0.070 Uiso 0.447(4) 1 calc PR C 2 C26 C 0.1677(5) 0.3416(5) 0.1646(5) 0.028(2) Uani 0.502(4) 1 d PDU C 1 C31 C 0.2861(5) 0.3292(7) 0.0914(5) 0.036(2) Uani 0.502(4) 1 d PDU C 1 H31A H 0.2745 0.3369 0.0320 0.054 Uiso 0.502(4) 1 calc PR C 1 H31B H 0.3478 0.2507 0.1111 0.054 Uiso 0.502(4) 1 calc PR C 1 H31C H 0.3116 0.3922 0.0842 0.054 Uiso 0.502(4) 1 calc PR C 1 C32 C 0.1340(6) 0.2412(6) 0.1702(6) 0.041(2) Uani 0.502(4) 1 d PDU C 1 H32A H 0.1254 0.2507 0.1093 0.062 Uiso 0.502(4) 1 calc PR C 1 H32B H 0.0579 0.2453 0.2157 0.062 Uiso 0.502(4) 1 calc PR C 1 H32C H 0.1972 0.1635 0.1891 0.062 Uiso 0.502(4) 1 calc PR C 1 C33 C 0.0719(6) 0.4645(6) 0.1269(6) 0.037(2) Uiso 0.502(4) 1 d PDU C 1 H33A H 0.0660 0.4675 0.0669 0.056 Uiso 0.502(4) 1 calc PR C 1 H33B H 0.0955 0.5290 0.1193 0.056 Uiso 0.502(4) 1 calc PR C 1 H33C H -0.0062 0.4742 0.1707 0.056 Uiso 0.502(4) 1 calc PR C 1 C26' C 0.1913(5) 0.3667(5) 0.1530(5) 0.029(2) Uani 0.498(4) 1 d PDU C 2 C31' C 0.2776(6) 0.4310(6) 0.0942(5) 0.036(2) Uani 0.498(4) 1 d PDU C 2 H31D H 0.2790 0.4509 0.0285 0.054 Uiso 0.498(4) 1 calc PR C 2 H31E H 0.3584 0.3787 0.1045 0.054 Uiso 0.498(4) 1 calc PR C 2 H31F H 0.2505 0.5047 0.1119 0.054 Uiso 0.498(4) 1 calc PR C 2 C32' C 0.2376(7) 0.2546(6) 0.1194(5) 0.038(2) Uani 0.498(4) 1 d PDU C 2 H32D H 0.2393 0.2785 0.0533 0.057 Uiso 0.498(4) 1 calc PR C 2 H32E H 0.1842 0.2108 0.1544 0.057 Uiso 0.498(4) 1 calc PR C 2 H32F H 0.3188 0.2029 0.1292 0.057 Uiso 0.498(4) 1 calc PR C 2 C33' C 0.0652(6) 0.4468(8) 0.1306(7) 0.036(3) Uiso 0.498(4) 1 d PDU C 2 H33D H 0.0724 0.4651 0.0640 0.054 Uiso 0.498(4) 1 calc PR C 2 H33E H 0.0332 0.5214 0.1483 0.054 Uiso 0.498(4) 1 calc PR C 2 H33F H 0.0108 0.4042 0.1653 0.054 Uiso 0.498(4) 1 calc PR C 2 C27 C 0.0671(5) 0.2886(5) 0.3847(5) 0.0272(19) Uani 0.495(4) 1 d PDU C 1 C34 C 0.0877(7) 0.1575(5) 0.4053(6) 0.039(3) Uani 0.495(4) 1 d PDU C 1 H34A H 0.0255 0.1385 0.4586 0.059 Uiso 0.495(4) 1 calc PR C 1 H34B H 0.1669 0.1064 0.4194 0.059 Uiso 0.495(4) 1 calc PR C 1 H34C H 0.0840 0.1434 0.3511 0.059 Uiso 0.495(4) 1 calc PR C 1 C35 C 0.0628(6) 0.3077(7) 0.4748(4) 0.043(2) Uani 0.495(4) 1 d PDU C 1 H35A H -0.0012 0.2863 0.5244 0.065 Uiso 0.495(4) 1 calc PR C 1 H35B H 0.0468 0.3918 0.4649 0.065 Uiso 0.495(4) 1 calc PR C 1 H35C H 0.1400 0.2570 0.4923 0.065 Uiso 0.495(4) 1 calc PR C 1 C36 C -0.0604(5) 0.3641(7) 0.3647(6) 0.030(2) Uani 0.495(4) 1 d PDU C 1 H36A H -0.1202 0.3426 0.4192 0.045 Uiso 0.495(4) 1 calc PR C 1 H36B H -0.0640 0.3479 0.3115 0.045 Uiso 0.495(4) 1 calc PR C 1 H36C H -0.0775 0.4494 0.3509 0.045 Uiso 0.495(4) 1 calc PR C 1 C27' C 0.0608(5) 0.2663(5) 0.3622(4) 0.027(2) Uani 0.505(4) 1 d PDU C 2 C34' C 0.0500(6) 0.1864(6) 0.3196(5) 0.038(2) Uani 0.505(4) 1 d PDU C 2 H34D H -0.0132 0.1568 0.3609 0.057 Uiso 0.505(4) 1 calc PR C 2 H34E H 0.1266 0.1184 0.3115 0.057 Uiso 0.505(4) 1 calc PR C 2 H34F H 0.0298 0.2328 0.2593 0.057 Uiso 0.505(4) 1 calc PR C 2 C35' C 0.0895(6) 0.1899(7) 0.4574(4) 0.037(2) Uani 0.505(4) 1 d PDU C 2 H35D H 0.0254 0.1606 0.4963 0.056 Uiso 0.505(4) 1 calc PR C 2 H35E H 0.0957 0.2386 0.4872 0.056 Uiso 0.505(4) 1 calc PR C 2 H35F H 0.1659 0.1217 0.4493 0.056 Uiso 0.505(4) 1 calc PR C 2 C36' C -0.0620(7) 0.3710(8) 0.3760(7) 0.047(3) Uani 0.505(4) 1 d PDU C 2 H36D H -0.1238 0.3391 0.4164 0.071 Uiso 0.505(4) 1 calc PR C 2 H36E H -0.0824 0.4180 0.3158 0.071 Uiso 0.505(4) 1 calc PR C 2 H36F H -0.0574 0.4222 0.4044 0.071 Uiso 0.505(4) 1 calc PR C 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 Ta1 0.01715(6) 0.01403(6) 0.02365(7) -0.00385(5) -0.00749(5) -0.00609(5) P1 0.0389(5) 0.0305(5) 0.0250(5) -0.0033(4) -0.0141(4) -0.0140(4) Si1 0.0711(6) 0.0183(5) 0.0299(5) 0.0036(4) -0.0295(5) -0.0235(4) Si2 0.0126(4) 0.0306(5) 0.0299(5) -0.0166(4) -0.0013(4) -0.0079(4) Si3 0.0152(4) 0.0216(4) 0.0239(5) -0.0077(4) -0.0051(4) -0.0043(4) O1 0.0741(15) 0.0215(12) 0.0316(13) 0.0025(10) -0.0282(12) -0.0258(11) O2 0.0164(10) 0.0385(12) 0.0392(14) -0.0256(10) 0.0019(10) -0.0100(10) O3 0.0158(10) 0.0239(11) 0.0216(12) -0.0051(10) -0.0047(9) -0.0055(9) C1 0.0238(16) 0.0220(16) 0.0310(19) -0.0115(14) -0.0057(15) -0.0084(14) C4 0.070(2) 0.036(2) 0.027(2) -0.0021(16) -0.0195(18) -0.0281(18) C5 0.0337(19) 0.0244(18) 0.064(2) -0.0206(17) -0.0225(18) 0.0007(16) C6 0.032(2) 0.070(2) 0.112(3) -0.068(2) -0.006(2) -0.0158(19) C2 0.031(3) 0.028(3) 0.024(3) -0.007(3) -0.008(3) -0.013(3) C7 0.025(3) 0.049(3) 0.026(3) -0.014(3) 0.004(3) -0.019(3) C8 0.043(4) 0.034(4) 0.030(3) -0.003(3) -0.017(3) -0.016(3) C9 0.034(3) 0.037(3) 0.031(4) -0.001(3) 0.001(3) -0.028(3) C2' 0.026(3) 0.021(3) 0.010(3) -0.010(2) -0.004(3) -0.010(3) C7' 0.023(3) 0.026(3) 0.015(3) -0.017(3) 0.009(3) -0.007(3) C8' 0.031(4) 0.026(3) 0.026(3) -0.011(3) -0.009(3) -0.006(3) C9' 0.042(4) 0.031(3) 0.022(4) -0.009(3) 0.000(4) -0.022(3) C3 0.034(3) 0.019(3) 0.020(3) -0.004(2) -0.007(3) -0.009(3) C10 0.045(4) 0.033(3) 0.017(4) 0.003(3) 0.001(3) -0.019(3) C11 0.040(3) 0.037(3) 0.027(4) -0.012(3) -0.004(3) -0.021(3) C12 0.051(3) 0.040(3) 0.026(4) -0.016(3) -0.006(3) -0.022(3) C3' 0.032(3) 0.015(3) 0.020(4) -0.006(3) -0.002(3) -0.008(3) C10' 0.030(3) 0.021(3) 0.021(4) -0.003(3) -0.008(3) -0.011(3) C11' 0.031(3) 0.038(4) 0.022(4) -0.011(3) 0.003(3) -0.017(3) C12' 0.039(4) 0.026(3) 0.011(3) -0.007(3) 0.002(3) -0.014(3) C13 0.040(3) 0.021(3) 0.013(3) -0.003(3) -0.003(3) -0.015(2) C16 0.024(3) 0.031(3) 0.028(4) -0.013(3) -0.001(3) -0.008(3) C17 0.034(3) 0.031(3) 0.039(4) -0.004(3) -0.012(3) -0.013(3) C18 0.038(3) 0.030(3) 0.014(3) -0.009(3) -0.008(3) -0.017(3) C13' 0.022(3) 0.021(3) 0.018(3) -0.004(3) -0.006(3) -0.006(3) C16' 0.034(4) 0.026(3) 0.028(4) -0.012(3) -0.010(3) -0.004(3) C17' 0.036(3) 0.033(4) 0.044(4) -0.017(3) -0.021(3) -0.007(3) C18' 0.029(4) 0.033(4) 0.027(6) 0.008(4) 0.013(4) -0.006(3) C14 0.027(3) 0.022(3) 0.019(3) -0.010(3) 0.002(3) -0.014(2) C19 0.032(3) 0.031(3) 0.045(4) -0.028(3) -0.002(3) -0.011(3) C20 0.034(3) 0.053(4) 0.032(3) -0.019(3) -0.008(3) -0.023(3) C21 0.026(3) 0.019(3) 0.037(4) -0.015(3) -0.002(3) -0.009(3) C14' 0.034(3) 0.035(3) 0.032(3) -0.012(3) 0.006(3) -0.029(2) C19' 0.049(4) 0.032(4) 0.035(3) -0.018(3) -0.005(3) -0.009(3) C20' 0.053(4) 0.046(4) 0.039(3) -0.020(3) -0.007(3) -0.024(4) C21' 0.057(3) 0.054(5) 0.049(5) -0.016(4) -0.005(4) -0.045(3) C15 0.020(3) 0.033(3) 0.035(3) -0.011(3) -0.009(3) -0.003(3) C22 0.031(4) 0.053(4) 0.039(3) -0.013(3) -0.006(3) -0.012(3) C23 0.032(3) 0.033(3) 0.049(4) -0.019(3) -0.004(3) -0.006(3) C24 0.014(3) 0.037(4) 0.061(5) -0.012(3) -0.019(3) 0.002(3) C22' 0.025(3) 0.043(4) 0.014(3) -0.003(3) -0.014(3) -0.016(3) C23' 0.025(3) 0.011(3) 0.017(4) 0.006(3) -0.009(3) -0.006(3) C24' 0.023(4) 0.039(5) 0.013(4) 0.000(4) -0.003(4) -0.013(4) C25 0.040(3) 0.024(3) 0.027(3) -0.017(3) -0.005(3) -0.006(3) C28 0.047(3) 0.024(3) 0.064(4) -0.018(3) -0.031(3) -0.001(3) C29 0.036(3) 0.025(3) 0.047(4) -0.001(3) -0.009(3) -0.015(3) C30 0.026(3) 0.019(3) 0.069(5) -0.003(4) -0.015(3) -0.010(3) C25' 0.013(3) 0.030(4) 0.028(4) -0.011(3) -0.006(3) -0.004(3) C28' 0.022(4) 0.039(4) 0.039(3) -0.029(3) -0.006(3) 0.002(3) C29' 0.026(3) 0.038(4) 0.049(5) -0.026(3) -0.007(3) -0.014(3) C30' 0.036(5) 0.047(6) 0.050(5) -0.031(4) -0.022(4) 0.012(5) C26 0.029(3) 0.027(3) 0.032(4) -0.009(3) -0.011(3) -0.009(3) C31 0.029(3) 0.047(4) 0.025(4) -0.015(3) -0.009(3) -0.004(3) C32 0.057(4) 0.035(4) 0.049(4) -0.006(3) -0.035(3) -0.018(3) C26' 0.039(4) 0.022(3) 0.031(4) 0.005(3) -0.025(3) -0.013(3) C31' 0.036(4) 0.028(4) 0.026(4) 0.000(3) -0.002(3) -0.008(3) C32' 0.044(4) 0.042(3) 0.023(4) -0.006(3) -0.001(4) -0.022(3) C27 0.025(3) 0.026(3) 0.040(3) -0.014(3) -0.015(3) -0.008(3) C34 0.033(4) 0.023(3) 0.034(5) 0.000(3) 0.012(4) -0.010(3) C35 0.024(4) 0.066(4) 0.026(3) -0.029(3) 0.012(3) -0.007(4) C36 0.007(3) 0.030(4) 0.044(5) -0.013(3) 0.008(3) -0.007(3) C27' 0.017(3) 0.032(4) 0.027(4) 0.000(3) -0.007(3) -0.009(3) C34' 0.036(3) 0.042(4) 0.040(4) -0.001(3) -0.021(3) -0.017(3) C35' 0.030(4) 0.043(5) 0.023(3) -0.002(3) -0.002(3) -0.011(3) C36' 0.028(5) 0.058(5) 0.034(5) -0.011(4) -0.005(4) -0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1 O3 1.858(2) . ? Ta1 O2 1.872(2) . ? Ta1 O1 1.874(3) . ? Ta1 P1 2.3158(11) . ? P1 P1 2.1709(19) 2_656 ? Si1 O1 1.672(3) . ? Si1 C2 1.731(7) . ? Si1 C3' 1.838(7) . ? Si1 C1 1.885(3) . ? Si1 C3 2.071(6) . ? Si1 C2' 2.092(6) . ? Si2 O2 1.672(3) . ? Si2 C13 1.825(7) . ? Si2 C15' 1.838(6) . ? Si2 C14 1.895(8) . ? Si2 C14' 1.953(7) . ? Si2 C15 1.982(5) . ? Si2 C13' 1.991(7) . ? Si3 O3 1.685(2) . ? Si3 C27 1.882(6) . ? Si3 C25' 1.897(9) . ? Si3 C26' 1.922(8) . ? Si3 C26 1.920(8) . ? Si3 C25 1.939(8) . ? Si3 C27' 1.946(7) . ? C1 C4 1.524(5) . ? C1 C6 1.531(5) . ? C1 C5 1.543(5) . ? C2 C7 1.526(8) . ? C2 C8 1.541(7) . ? C2 C9 1.542(8) . ? C2' C8' 1.543(8) . ? C2' C7' 1.549(7) . ? C2' C9' 1.549(8) . ? C3 C10 1.531(7) . ? C3 C11 1.546(7) . ? C3 C12 1.549(9) . ? C3' C10' 1.531(7) . ? C3' C11' 1.534(8) . ? C3' C12' 1.545(9) . ? C13 C16 1.527(9) . ? C13 C17 1.547(7) . ? C13 C18 1.547(7) . ? C13' C16' 1.542(8) . ? C13' C17' 1.546(8) . ? C13' C18' 1.549(8) . ? C14 C19 1.530(7) . ? C14 C20 1.547(8) . ? C14 C21 1.550(8) . ? C14' C20' 1.537(8) . ? C14' C19' 1.546(7) . ? C14' C21' 1.554(8) . ? C15 C22 1.521(7) . ? C15 C23 1.547(8) . ? C15 C24 1.540(8) . ? C15' C22' 1.526(8) . ? C15' C23' 1.534(8) . ? C15' C24' 1.552(8) . ? C25 C28 1.525(8) . ? C25 C30 1.538(7) . ? C25 C29 1.547(7) . ? C25' C28' 1.533(8) . ? C25' C30' 1.541(9) . ? C25' C29' 1.547(8) . ? C26 C32 1.533(9) . ? C26 C31 1.534(8) . ? C26 C33 1.556(7) . ? C26' C31' 1.531(8) . ? C26' C32' 1.538(9) . ? C26' C33' 1.559(8) . ? C27 C34 1.527(8) . ? C27 C35 1.540(9) . ? C27 C36 1.556(8) . ? C27' C34' 1.534(9) . ? C27' C35' 1.538(8) . ? C27' C36' 1.546(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ta1 O2 114.10(10) . . ? O3 Ta1 O1 114.08(12) . . ? O2 Ta1 O1 106.83(11) . . ? O3 Ta1 P1 99.14(8) . . ? O2 Ta1 P1 111.85(9) . . ? O1 Ta1 P1 110.85(8) . . ? P1 P1 Ta1 105.67(6) 2_656 . ? O1 Si1 C2 107.4(2) . . ? O1 Si1 C3' 104.3(2) . . ? C2 Si1 C3' 89.6(3) . . ? O1 Si1 C1 107.77(16) . . ? C2 Si1 C1 120.9(2) . . ? C3' Si1 C1 124.5(2) . . ? O1 Si1 C3 105.5(2) . . ? C2 Si1 C3 112.6(3) . . ? C3' Si1 C3 25.3(2) . . ? C1 Si1 C3 101.58(18) . . ? O1 Si1 C2' 105.95(19) . . ? C2 Si1 C2' 18.2(2) . . ? C3' Si1 C2' 107.3(3) . . ? C1 Si1 C2' 105.70(18) . . ? C3 Si1 C2' 129.0(3) . . ? O2 Si2 C13 101.9(2) . . ? O2 Si2 C15' 107.4(2) . . ? C13 Si2 C15' 131.9(3) . . ? O2 Si2 C14 104.1(2) . . ? C13 Si2 C14 119.0(3) . . ? C15' Si2 C14 89.8(3) . . ? O2 Si2 C14' 109.60(18) . . ? C13 Si2 C14' 90.7(3) . . ? C15' Si2 C14' 113.4(3) . . ? C14 Si2 C14' 28.5(2) . . ? O2 Si2 C15 106.75(19) . . ? C13 Si2 C15 114.3(2) . . ? C15' Si2 C15 20.3(3) . . ? C14 Si2 C15 109.3(3) . . ? C14' Si2 C15 129.8(3) . . ? O2 Si2 C13' 107.3(2) . . ? C13 Si2 C13' 19.5(2) . . ? C15' Si2 C13' 113.2(2) . . ? C14 Si2 C13' 132.4(3) . . ? C14' Si2 C13' 105.8(3) . . ? C15 Si2 C13' 94.9(2) . . ? O3 Si3 C27 107.44(18) . . ? O3 Si3 C25' 105.2(2) . . ? C27 Si3 C25' 95.5(3) . . ? O3 Si3 C26' 103.00(19) . . ? C27 Si3 C26' 128.0(3) . . ? C25' Si3 C26' 115.8(3) . . ? O3 Si3 C26 104.27(18) . . ? C27 Si3 C26 114.8(3) . . ? C25' Si3 C26 128.1(3) . . ? C26' Si3 C26 14.7(3) . . ? O3 Si3 C25 108.0(2) . . ? C27 Si3 C25 110.1(3) . . ? C25' Si3 C25 17.2(2) . . ? C26' Si3 C25 98.8(3) . . ? C26 Si3 C25 111.8(3) . . ? O3 Si3 C27' 106.40(19) . . ? C27 Si3 C27' 17.7(3) . . ? C25' Si3 C27' 112.4(3) . . ? C26' Si3 C27' 112.8(3) . . ? C26 Si3 C27' 98.7(3) . . ? C25 Si3 C27' 125.6(3) . . ? Si1 O1 Ta1 172.84(17) . . ? Si2 O2 Ta1 177.60(15) . . ? Si3 O3 Ta1 172.88(16) . . ? C4 C1 C6 104.9(3) . . ? C4 C1 C5 108.4(3) . . ? C6 C1 C5 108.4(3) . . ? C4 C1 Si1 110.7(2) . . ? C6 C1 Si1 112.1(3) . . ? C5 C1 Si1 112.0(3) . . ? C7 C2 C8 108.9(5) . . ? C7 C2 C9 106.9(5) . . ? C8 C2 C9 108.1(6) . . ? C7 C2 Si1 105.6(5) . . ? C8 C2 Si1 112.3(4) . . ? C9 C2 Si1 114.7(4) . . ? C8' C2' C7' 106.3(5) . . ? C8' C2' C9' 105.8(6) . . ? C7' C2' C9' 106.3(5) . . ? C8' C2' Si1 112.6(4) . . ? C7' C2' Si1 113.4(5) . . ? C9' C2' Si1 111.9(4) . . ? C10 C3 C11 107.4(5) . . ? C10 C3 C12 107.2(6) . . ? C11 C3 C12 107.2(5) . . ? C10 C3 Si1 108.8(4) . . ? C11 C3 Si1 115.8(5) . . ? C12 C3 Si1 110.2(4) . . ? C10' C3' C11' 107.1(5) . . ? C10' C3' C12' 109.5(6) . . ? C11' C3' C12' 107.8(5) . . ? C10' C3' Si1 114.2(5) . . ? C11' C3' Si1 104.8(5) . . ? C12' C3' Si1 113.0(4) . . ? C16 C13 C17 106.4(5) . . ? C16 C13 C18 108.3(5) . . ? C17 C13 C18 107.3(5) . . ? C16 C13 Si2 112.8(4) . . ? C17 C13 Si2 109.9(5) . . ? C18 C13 Si2 111.8(5) . . ? C16' C13' C17' 104.7(6) . . ? C16' C13' C18' 106.7(6) . . ? C17' C13' C18' 108.0(6) . . ? C16' C13' Si2 109.2(4) . . ? C17' C13' Si2 113.0(4) . . ? C18' C13' Si2 114.6(6) . . ? C19 C14 C20 106.6(5) . . ? C19 C14 C21 106.8(5) . . ? C20 C14 C21 108.2(6) . . ? C19 C14 Si2 108.8(5) . . ? C20 C14 Si2 115.6(5) . . ? C21 C14 Si2 110.3(5) . . ? C20' C14' C19' 105.2(5) . . ? C20' C14' C21' 108.3(7) . . ? C19' C14' C21' 107.0(6) . . ? C20' C14' Si2 107.7(5) . . ? C19' C14' Si2 114.0(5) . . ? C21' C14' Si2 114.1(5) . . ? C22 C15 C23 107.0(6) . . ? C22 C15 C24 110.9(6) . . ? C23 C15 C24 107.0(5) . . ? C22 C15 Si2 114.2(4) . . ? C23 C15 Si2 109.8(4) . . ? C24 C15 Si2 107.9(4) . . ? C22' C15' C23' 107.5(6) . . ? C22' C15' C24' 106.7(7) . . ? C23' C15' C24' 106.7(6) . . ? C22' C15' Si2 109.6(4) . . ? C23' C15' Si2 108.0(5) . . ? C24' C15' Si2 117.8(5) . . ? C28 C25 C30 109.1(6) . . ? C28 C25 C29 106.6(6) . . ? C30 C25 C29 106.6(5) . . ? C28 C25 Si3 111.1(4) . . ? C30 C25 Si3 112.7(5) . . ? C29 C25 Si3 110.5(5) . . ? C28' C25' C30' 109.5(6) . . ? C28' C25' C29' 107.2(7) . . ? C30' C25' C29' 106.4(7) . . ? C28' C25' Si3 112.3(6) . . ? C30' C25' Si3 113.4(7) . . ? C29' C25' Si3 107.7(5) . . ? C32 C26 C31 105.8(6) . . ? C32 C26 C33 108.9(6) . . ? C31 C26 C33 107.0(5) . . ? C32 C26 Si3 110.9(5) . . ? C31 C26 Si3 111.0(5) . . ? C33 C26 Si3 112.8(5) . . ? C31' C26' C32' 106.3(6) . . ? C31' C26' C33' 109.1(6) . . ? C32' C26' C33' 106.3(7) . . ? C31' C26' Si3 110.7(6) . . ? C32' C26' Si3 111.7(4) . . ? C33' C26' Si3 112.4(5) . . ? C34 C27 C35 107.0(6) . . ? C34 C27 C36 106.7(6) . . ? C35 C27 C36 106.9(6) . . ? C34 C27 Si3 109.9(4) . . ? C35 C27 Si3 114.5(5) . . ? C36 C27 Si3 111.5(4) . . ? C34' C27' C35' 107.2(6) . . ? C34' C27' C36' 108.2(7) . . ? C35' C27' C36' 109.1(6) . . ? C34' C27' Si3 110.7(4) . . ? C35' C27' Si3 110.9(5) . . ? C36' C27' Si3 110.6(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.52 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.821 _refine_diff_density_min -1.058 _refine_diff_density_rms 0.170 data_eh4 _database_code_depnum_ccdc_archive 'CCDC 715087' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H162 Nb2 O6 P2 Si6' _chemical_formula_sum 'C72 H162 Nb2 O6 P2 Si6' _chemical_formula_weight 1540.32 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' Si Si 0.0817 0.0704 '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' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.9765(6) _cell_length_b 13.1430(6) _cell_length_c 16.0885(8) _cell_angle_alpha 67.128(2) _cell_angle_beta 68.430(2) _cell_angle_gamma 61.974(2) _cell_volume 2173.19(18) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 838 _exptl_absorpt_coefficient_mu 0.426 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8480 _exptl_absorpt_correction_T_max 0.9790 _exptl_absorpt_process_details SADABS _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52030 _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_av_sigmaI/netI 0.0513 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 28.28 _reflns_number_total 10782 _reflns_number_gt 8780 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT+' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All but one siloxo groups are disorderd into two positions each. Despite the restrictions imposed on the of disordered tertiary butyl groups, their geometry is sometime is on the edge of normal values. In particular, the Si(1)-C(2') and Si(1)-C(3) bond lengths are on the edge of normal; these abnormally long lengths result from attempts to properly model the tertiary-butyl group disorder. ; _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^)+(0.0380P)^2^+0.8935P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10782 _refine_ls_number_parameters 689 _refine_ls_number_restraints 2614 _refine_ls_R_factor_all 0.0527 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.0939 _refine_ls_wR_factor_gt 0.0876 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.169 _refine_ls_shift/su_max 0.081 _refine_ls_shift/su_mean 0.002 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 Nb1 Nb 0.457655(15) 0.583556(15) 0.321000(13) 0.01606(5) Uani 1 1 d . . . P1 P 0.42180(6) 0.56985(5) 0.47684(4) 0.02964(14) Uani 1 1 d . . . Si1 Si 0.48380(7) 0.30937(5) 0.30661(5) 0.03511(16) Uani 1 1 d D . . Si2 Si 0.18587(5) 0.82700(5) 0.28259(4) 0.01938(12) Uani 1 1 d D . . Si3 Si 0.72073(5) 0.64220(5) 0.19052(4) 0.02242(13) Uani 1 1 d D . . O1 O 0.47771(17) 0.43837(14) 0.30779(12) 0.0412(4) Uani 1 1 d . A . O2 O 0.31648(11) 0.71140(12) 0.29509(10) 0.0208(3) Uani 1 1 d . B . O3 O 0.59972(12) 0.61038(14) 0.25347(12) 0.0316(4) Uani 1 1 d . C . C1 C 0.58744(18) 0.18508(18) 0.38313(16) 0.0235(5) Uani 1 1 d DU A . C4 C 0.6266(2) 0.0627(2) 0.3674(2) 0.0399(6) Uani 1 1 d DU . . H4A H 0.6802 0.0010 0.4080 0.060 Uiso 1 1 calc R A . H4B H 0.6688 0.0644 0.3026 0.060 Uiso 1 1 calc R . . H4C H 0.5558 0.0448 0.3815 0.060 Uiso 1 1 calc R . . C5 C 0.7004(2) 0.2063(3) 0.3685(3) 0.0620(9) Uani 1 1 d DU . . H5A H 0.7513 0.1399 0.4093 0.093 Uiso 1 1 calc R A . H5B H 0.6771 0.2812 0.3830 0.093 Uiso 1 1 calc R . . H5C H 0.7448 0.2116 0.3038 0.093 Uiso 1 1 calc R . . C6 C 0.5269(3) 0.1773(2) 0.48517(16) 0.0395(6) Uani 1 1 d DU . . H6A H 0.5822 0.1125 0.5233 0.059 Uiso 1 1 calc R A . H6B H 0.4546 0.1613 0.5001 0.059 Uiso 1 1 calc R . . H6C H 0.5048 0.2530 0.4978 0.059 Uiso 1 1 calc R . . C2 C 0.3363(4) 0.3247(4) 0.3283(3) 0.0253(11) Uani 0.502(3) 1 d PDU A 1 C7 C 0.2666(4) 0.3813(5) 0.4101(4) 0.0338(12) Uani 0.502(3) 1 d PDU A 1 H7A H 0.1824 0.3921 0.4250 0.051 Uiso 0.502(3) 1 calc PR A 1 H7B H 0.2719 0.4590 0.3934 0.051 Uiso 0.502(3) 1 calc PR A 1 H7C H 0.3011 0.3288 0.4641 0.051 Uiso 0.502(3) 1 calc PR A 1 C8 C 0.2799(4) 0.4081(4) 0.2468(3) 0.0340(12) Uani 0.502(3) 1 d PDU A 1 H8A H 0.1972 0.4144 0.2617 0.051 Uiso 0.502(3) 1 calc PR A 1 H8B H 0.3259 0.3766 0.1923 0.051 Uiso 0.502(3) 1 calc PR A 1 H8C H 0.2802 0.4873 0.2336 0.051 Uiso 0.502(3) 1 calc PR A 1 C9 C 0.3211(5) 0.2054(5) 0.3562(4) 0.0355(14) Uani 0.502(3) 1 d PDU A 1 H9A H 0.2362 0.2209 0.3671 0.053 Uiso 0.502(3) 1 calc PR A 1 H9B H 0.3496 0.1541 0.4130 0.053 Uiso 0.502(3) 1 calc PR A 1 H9C H 0.3677 0.1653 0.3063 0.053 Uiso 0.502(3) 1 calc PR A 1 C2' C 0.3138(4) 0.3061(4) 0.3743(3) 0.0192(10) Uani 0.498(3) 1 d PDU A 2 C7' C 0.2656(4) 0.3419(4) 0.4667(3) 0.0241(10) Uani 0.498(3) 1 d PDU A 2 H7'A H 0.1852 0.3404 0.4956 0.036 Uiso 0.498(3) 1 calc PR A 2 H7'B H 0.2617 0.4226 0.4543 0.036 Uiso 0.498(3) 1 calc PR A 2 H7'C H 0.3193 0.2854 0.5085 0.036 Uiso 0.498(3) 1 calc PR A 2 C8' C 0.2185(4) 0.3912(4) 0.3168(3) 0.0306(11) Uani 0.498(3) 1 d PDU A 2 H8'A H 0.1407 0.3862 0.3527 0.046 Uiso 0.498(3) 1 calc PR A 2 H8'B H 0.2416 0.3682 0.2594 0.046 Uiso 0.498(3) 1 calc PR A 2 H8'C H 0.2125 0.4733 0.3016 0.046 Uiso 0.498(3) 1 calc PR A 2 C9' C 0.3124(5) 0.1804(4) 0.3988(4) 0.0268(12) Uani 0.498(3) 1 d PDU A 2 H9'A H 0.2309 0.1830 0.4303 0.040 Uiso 0.498(3) 1 calc PR A 2 H9'B H 0.3671 0.1231 0.4398 0.040 Uiso 0.498(3) 1 calc PR A 2 H9'C H 0.3382 0.1556 0.3419 0.040 Uiso 0.498(3) 1 calc PR A 2 C3 C 0.5813(4) 0.2854(4) 0.1777(3) 0.0248(10) Uani 0.508(3) 1 d PDU A 1 C10 C 0.5440(4) 0.4039(4) 0.1037(3) 0.0330(11) Uani 0.508(3) 1 d PDU A 1 H10A H 0.5901 0.3916 0.0423 0.049 Uiso 0.508(3) 1 calc PR A 1 H10B H 0.5597 0.4631 0.1147 0.049 Uiso 0.508(3) 1 calc PR A 1 H10C H 0.4583 0.4327 0.1069 0.049 Uiso 0.508(3) 1 calc PR A 1 C11 C 0.7200(4) 0.2402(4) 0.1608(3) 0.0299(11) Uani 0.508(3) 1 d PDU A 1 H11A H 0.7572 0.2314 0.0975 0.045 Uiso 0.508(3) 1 calc PR A 1 H11B H 0.7495 0.1629 0.2051 0.045 Uiso 0.508(3) 1 calc PR A 1 H11C H 0.7404 0.2981 0.1691 0.045 Uiso 0.508(3) 1 calc PR A 1 C12 C 0.5574(5) 0.1948(4) 0.1565(3) 0.0321(11) Uani 0.508(3) 1 d PDU A 1 H12A H 0.5811 0.1177 0.2024 0.048 Uiso 0.508(3) 1 calc PR A 1 H12B H 0.6040 0.1850 0.0945 0.048 Uiso 0.508(3) 1 calc PR A 1 H12C H 0.4718 0.2241 0.1590 0.048 Uiso 0.508(3) 1 calc PR A 1 C3' C 0.5042(4) 0.3223(4) 0.1843(3) 0.0219(10) Uani 0.492(3) 1 d PDU A 2 C10' C 0.4291(4) 0.4449(4) 0.1311(3) 0.0295(11) Uani 0.492(3) 1 d PDU A 2 H10D H 0.4449 0.4448 0.0667 0.044 Uiso 0.492(3) 1 calc PR A 2 H10E H 0.4505 0.5063 0.1326 0.044 Uiso 0.492(3) 1 calc PR A 2 H10F H 0.3438 0.4619 0.1600 0.044 Uiso 0.492(3) 1 calc PR A 2 C11' C 0.6343(4) 0.3070(4) 0.1411(4) 0.0294(11) Uani 0.492(3) 1 d PDU A 2 H11D H 0.6521 0.3127 0.0751 0.044 Uiso 0.492(3) 1 calc PR A 2 H11E H 0.6863 0.2287 0.1721 0.044 Uiso 0.492(3) 1 calc PR A 2 H11F H 0.6485 0.3699 0.1482 0.044 Uiso 0.492(3) 1 calc PR A 2 C12' C 0.4838(4) 0.2265(4) 0.1676(4) 0.0295(11) Uiso 0.492(3) 1 d PDU A 2 H12D H 0.5309 0.1472 0.2013 0.044 Uiso 0.492(3) 1 calc PR A 2 H12E H 0.5089 0.2317 0.1012 0.044 Uiso 0.492(3) 1 calc PR A 2 H12F H 0.3985 0.2395 0.1895 0.044 Uiso 0.492(3) 1 calc PR A 2 C13 C 0.1660(4) 0.8432(5) 0.1650(4) 0.0242(13) Uani 0.505(4) 1 d PDU B 1 C16 C 0.2843(4) 0.8283(4) 0.0931(3) 0.0340(12) Uani 0.505(4) 1 d PDU B 1 H16A H 0.2729 0.8363 0.0335 0.051 Uiso 0.505(4) 1 calc PR B 1 H16B H 0.3446 0.7491 0.1134 0.051 Uiso 0.505(4) 1 calc PR B 1 H16C H 0.3116 0.8898 0.0860 0.051 Uiso 0.505(4) 1 calc PR B 1 C17 C 0.1329(4) 0.7414(4) 0.1724(4) 0.0376(12) Uani 0.505(4) 1 d PDU B 1 H17A H 0.1233 0.7499 0.1121 0.056 Uiso 0.505(4) 1 calc PR B 1 H17B H 0.0575 0.7451 0.2186 0.056 Uiso 0.505(4) 1 calc PR B 1 H17C H 0.1967 0.6643 0.1911 0.056 Uiso 0.505(4) 1 calc PR B 1 C18 C 0.0697(7) 0.9634(8) 0.1286(7) 0.037(2) Uani 0.505(4) 1 d PDU B 1 H18A H 0.0635 0.9663 0.0688 0.056 Uiso 0.505(4) 1 calc PR B 1 H18B H 0.0919 1.0287 0.1209 0.056 Uiso 0.505(4) 1 calc PR B 1 H18C H -0.0077 0.9717 0.1729 0.056 Uiso 0.505(4) 1 calc PR B 1 C13' C 0.1928(5) 0.8647(5) 0.1537(4) 0.0241(14) Uani 0.495(4) 1 d PDU B 2 C16' C 0.2796(4) 0.9284(4) 0.0942(3) 0.0357(13) Uani 0.495(4) 1 d PDU B 2 H16D H 0.2815 0.9470 0.0286 0.054 Uiso 0.495(4) 1 calc PR B 2 H16E H 0.3601 0.8763 0.1051 0.054 Uiso 0.495(4) 1 calc PR B 2 H16F H 0.2525 1.0026 0.1110 0.054 Uiso 0.495(4) 1 calc PR B 2 C17' C 0.2390(5) 0.7534(4) 0.1204(3) 0.0353(12) Uani 0.495(4) 1 d PDU B 2 H17D H 0.2409 0.7772 0.0543 0.053 Uiso 0.495(4) 1 calc PR B 2 H17E H 0.1857 0.7097 0.1553 0.053 Uiso 0.495(4) 1 calc PR B 2 H17F H 0.3200 0.7019 0.1304 0.053 Uiso 0.495(4) 1 calc PR B 2 C18' C 0.0695(7) 0.9471(8) 0.1292(8) 0.041(3) Uani 0.495(4) 1 d PDU B 2 H18D H 0.0779 0.9639 0.0627 0.061 Uiso 0.495(4) 1 calc PR B 2 H18E H 0.0398 1.0221 0.1455 0.061 Uiso 0.495(4) 1 calc PR B 2 H18F H 0.0126 0.9074 0.1640 0.061 Uiso 0.495(4) 1 calc PR B 2 C14 C 0.0628(5) 0.7908(5) 0.3856(4) 0.0294(14) Uani 0.503(4) 1 d PDU B 1 C19 C 0.0861(4) 0.6587(4) 0.4074(4) 0.0400(14) Uani 0.503(4) 1 d PDU B 1 H19A H 0.0239 0.6393 0.4603 0.060 Uiso 0.503(4) 1 calc PR B 1 H19B H 0.1648 0.6094 0.4225 0.060 Uiso 0.503(4) 1 calc PR B 1 H19C H 0.0846 0.6427 0.3533 0.060 Uiso 0.503(4) 1 calc PR B 1 C20 C 0.0626(5) 0.8078(5) 0.4753(3) 0.0393(13) Uani 0.503(4) 1 d PDU B 1 H20A H -0.0016 0.7881 0.5255 0.059 Uiso 0.503(4) 1 calc PR B 1 H20B H 0.0494 0.8911 0.4654 0.059 Uiso 0.503(4) 1 calc PR B 1 H20C H 0.1400 0.7551 0.4920 0.059 Uiso 0.503(4) 1 calc PR B 1 C21 C -0.0634(6) 0.8653(7) 0.3656(6) 0.034(2) Uani 0.503(4) 1 d PDU B 1 H21A H -0.1232 0.8444 0.4202 0.051 Uiso 0.503(4) 1 calc PR B 1 H21B H -0.0670 0.8483 0.3127 0.051 Uiso 0.503(4) 1 calc PR B 1 H21C H -0.0802 0.9505 0.3511 0.051 Uiso 0.503(4) 1 calc PR B 1 C14' C 0.0635(4) 0.7663(5) 0.3623(4) 0.0235(13) Uani 0.497(4) 1 d PDU B 2 C19' C 0.0509(4) 0.6865(4) 0.3207(4) 0.0358(12) Uani 0.497(4) 1 d PDU B 2 H19D H -0.0122 0.6573 0.3627 0.054 Uiso 0.497(4) 1 calc PR B 2 H19E H 0.1270 0.6184 0.3122 0.054 Uiso 0.497(4) 1 calc PR B 2 H19F H 0.0297 0.7329 0.2606 0.054 Uiso 0.497(4) 1 calc PR B 2 C20' C 0.0885(4) 0.6918(4) 0.4578(3) 0.0303(12) Uani 0.497(4) 1 d PDU B 2 H20D H 0.0235 0.6636 0.4956 0.045 Uiso 0.497(4) 1 calc PR B 2 H20E H 0.0936 0.7409 0.4879 0.045 Uiso 0.497(4) 1 calc PR B 2 H20F H 0.1645 0.6230 0.4514 0.045 Uiso 0.497(4) 1 calc PR B 2 C21' C -0.0596(7) 0.8711(8) 0.3764(7) 0.038(2) Uani 0.497(4) 1 d PDU B 2 H21D H -0.1212 0.8392 0.4172 0.057 Uiso 0.497(4) 1 calc PR B 2 H21E H -0.0805 0.9180 0.3164 0.057 Uiso 0.497(4) 1 calc PR B 2 H21F H -0.0548 0.9223 0.4046 0.057 Uiso 0.497(4) 1 calc PR B 2 C15 C 0.1975(4) 0.9689(4) 0.2834(3) 0.0261(12) Uani 0.513(4) 1 d PDU B 1 C22 C 0.2520(4) 0.9408(4) 0.3641(3) 0.0345(12) Uani 0.513(4) 1 d PDU B 1 H22A H 0.2580 1.0127 0.3633 0.052 Uiso 0.513(4) 1 calc PR B 1 H22B H 0.3321 0.8773 0.3572 0.052 Uiso 0.513(4) 1 calc PR B 1 H22C H 0.2006 0.9144 0.4230 0.052 Uiso 0.513(4) 1 calc PR B 1 C23 C 0.2831(4) 1.0113(4) 0.1941(3) 0.0361(12) Uani 0.513(4) 1 d PDU B 1 H23A H 0.2883 1.0820 0.1968 0.054 Uiso 0.513(4) 1 calc PR B 1 H23B H 0.2523 1.0316 0.1401 0.054 Uiso 0.513(4) 1 calc PR B 1 H23C H 0.3630 0.9473 0.1888 0.054 Uiso 0.513(4) 1 calc PR B 1 C24 C 0.0787(7) 1.0788(7) 0.2932(7) 0.044(3) Uani 0.513(4) 1 d PDU B 1 H24A H 0.0950 1.1445 0.2932 0.066 Uiso 0.513(4) 1 calc PR B 1 H24B H 0.0234 1.0579 0.3515 0.066 Uiso 0.513(4) 1 calc PR B 1 H24C H 0.0425 1.1037 0.2412 0.066 Uiso 0.513(4) 1 calc PR B 1 C15' C 0.1909(5) 0.9428(5) 0.3211(4) 0.0274(13) Uani 0.487(4) 1 d PDU B 2 C22' C 0.1659(5) 0.9126(5) 0.4269(3) 0.0408(14) Uani 0.487(4) 1 d PDU B 2 H22D H 0.1679 0.9750 0.4446 0.061 Uiso 0.487(4) 1 calc PR B 2 H22E H 0.2272 0.8356 0.4497 0.061 Uiso 0.487(4) 1 calc PR B 2 H22F H 0.0867 0.9079 0.4542 0.061 Uiso 0.487(4) 1 calc PR B 2 C23' C 0.3135(4) 0.9502(5) 0.2826(4) 0.0424(14) Uani 0.487(4) 1 d PDU B 2 H23D H 0.3141 1.0109 0.3032 0.064 Uiso 0.487(4) 1 calc PR B 2 H23E H 0.3314 0.9719 0.2148 0.064 Uiso 0.487(4) 1 calc PR B 2 H23F H 0.3743 0.8725 0.3051 0.064 Uiso 0.487(4) 1 calc PR B 2 C24' C 0.0953(8) 1.0653(8) 0.2875(8) 0.038(2) Uani 0.487(4) 1 d PDU B 2 H24D H 0.0970 1.1252 0.3084 0.057 Uiso 0.487(4) 1 calc PR B 2 H24E H 0.0159 1.0607 0.3130 0.057 Uiso 0.487(4) 1 calc PR B 2 H24F H 0.1119 1.0881 0.2197 0.057 Uiso 0.487(4) 1 calc PR B 2 C25 C 0.7142(4) 0.7523(4) 0.2427(3) 0.0227(10) Uani 0.496(3) 1 d PDU C 1 C28 C 0.7569(4) 0.6972(4) 0.3330(3) 0.0316(11) Uani 0.496(3) 1 d PDU C 1 H28A H 0.7501 0.7606 0.3548 0.047 Uiso 0.496(3) 1 calc PR C 1 H28B H 0.8407 0.6416 0.3222 0.047 Uiso 0.496(3) 1 calc PR C 1 H28C H 0.7071 0.6541 0.3800 0.047 Uiso 0.496(3) 1 calc PR C 1 C29 C 0.5837(4) 0.8404(5) 0.2657(4) 0.0336(14) Uani 0.496(3) 1 d PDU C 1 H29A H 0.5807 0.8970 0.2930 0.050 Uiso 0.496(3) 1 calc PR C 1 H29B H 0.5338 0.7960 0.3100 0.050 Uiso 0.496(3) 1 calc PR C 1 H29C H 0.5537 0.8841 0.2089 0.050 Uiso 0.496(3) 1 calc PR C 1 C30 C 0.7886(6) 0.8279(7) 0.1740(5) 0.0292(17) Uani 0.496(3) 1 d PDU C 1 H30A H 0.7836 0.8835 0.2033 0.044 Uiso 0.496(3) 1 calc PR C 1 H30B H 0.7567 0.8731 0.1181 0.044 Uiso 0.496(3) 1 calc PR C 1 H30C H 0.8725 0.7749 0.1573 0.044 Uiso 0.496(3) 1 calc PR C 1 C25' C 0.6910(4) 0.8059(4) 0.1879(3) 0.0249(10) Uani 0.504(3) 1 d PDU C 2 C28' C 0.6042(4) 0.9038(4) 0.1254(3) 0.0329(12) Uani 0.504(3) 1 d PDU C 2 H28D H 0.5923 0.9828 0.1262 0.049 Uiso 0.504(3) 1 calc PR C 2 H28E H 0.5269 0.8948 0.1486 0.049 Uiso 0.504(3) 1 calc PR C 2 H28F H 0.6384 0.8957 0.0618 0.049 Uiso 0.504(3) 1 calc PR C 2 C29' C 0.6299(5) 0.8187(5) 0.2862(4) 0.0334(13) Uani 0.504(3) 1 d PDU C 2 H29D H 0.6137 0.8987 0.2879 0.050 Uiso 0.504(3) 1 calc PR C 2 H29E H 0.6824 0.7585 0.3280 0.050 Uiso 0.504(3) 1 calc PR C 2 H29F H 0.5542 0.8073 0.3059 0.050 Uiso 0.504(3) 1 calc PR C 2 C30' C 0.8059(6) 0.8300(7) 0.1543(6) 0.0352(18) Uani 0.504(3) 1 d PDU C 2 H30D H 0.7862 0.9116 0.1543 0.053 Uiso 0.504(3) 1 calc PR C 2 H30E H 0.8450 0.8205 0.0913 0.053 Uiso 0.504(3) 1 calc PR C 2 H30F H 0.8601 0.7732 0.1957 0.053 Uiso 0.504(3) 1 calc PR C 2 C26 C 0.8612(4) 0.4920(4) 0.2137(3) 0.0229(11) Uani 0.506(3) 1 d PDU C 1 C31 C 0.8552(4) 0.4217(4) 0.3160(3) 0.0303(11) Uani 0.506(3) 1 d PDU C 1 H31A H 0.9281 0.3490 0.3213 0.045 Uiso 0.506(3) 1 calc PR C 1 H31B H 0.7850 0.3999 0.3405 0.045 Uiso 0.506(3) 1 calc PR C 1 H31C H 0.8488 0.4712 0.3515 0.045 Uiso 0.506(3) 1 calc PR C 1 C32 C 0.8773(4) 0.4051(4) 0.1630(3) 0.0299(11) Uani 0.506(3) 1 d PDU C 1 H32A H 0.9476 0.3316 0.1754 0.045 Uiso 0.506(3) 1 calc PR C 1 H32B H 0.8887 0.4427 0.0962 0.045 Uiso 0.506(3) 1 calc PR C 1 H32C H 0.8057 0.3858 0.1852 0.045 Uiso 0.506(3) 1 calc PR C 1 C33 C 0.9750(5) 0.5201(7) 0.1754(6) 0.028(2) Uani 0.506(3) 1 d PDU C 1 H33A H 1.0450 0.4459 0.1868 0.042 Uiso 0.506(3) 1 calc PR C 1 H33B H 0.9682 0.5748 0.2064 0.042 Uiso 0.506(3) 1 calc PR C 1 H33C H 0.9843 0.5576 0.1086 0.042 Uiso 0.506(3) 1 calc PR C 1 C26' C 0.8475(4) 0.5263(4) 0.2420(3) 0.0246(11) Uani 0.494(3) 1 d PDU C 2 C31' C 0.8376(5) 0.5470(5) 0.3331(3) 0.0352(12) Uani 0.494(3) 1 d PDU C 2 H31D H 0.9056 0.4853 0.3601 0.053 Uiso 0.494(3) 1 calc PR C 2 H31E H 0.7626 0.5430 0.3767 0.053 Uiso 0.494(3) 1 calc PR C 2 H31F H 0.8384 0.6259 0.3203 0.053 Uiso 0.494(3) 1 calc PR C 2 C32' C 0.8376(4) 0.4056(4) 0.2686(4) 0.0321(12) Uani 0.494(3) 1 d PDU C 2 H32D H 0.9048 0.3425 0.2958 0.048 Uiso 0.494(3) 1 calc PR C 2 H32E H 0.8395 0.3898 0.2132 0.048 Uiso 0.494(3) 1 calc PR C 2 H32F H 0.7619 0.4073 0.3138 0.048 Uiso 0.494(3) 1 calc PR C 2 C33' C 0.9747(7) 0.5131(9) 0.1816(7) 0.041(3) Uani 0.494(3) 1 d PDU C 2 H33D H 1.0342 0.4495 0.2167 0.061 Uiso 0.494(3) 1 calc PR C 2 H33E H 0.9850 0.5886 0.1643 0.061 Uiso 0.494(3) 1 calc PR C 2 H33F H 0.9858 0.4928 0.1256 0.061 Uiso 0.494(3) 1 calc PR C 2 C27 C 0.6993(4) 0.6946(4) 0.0726(3) 0.0241(11) Uani 0.497(3) 1 d PDU C 1 C34 C 0.6604(4) 0.6146(4) 0.0526(3) 0.0297(11) Uani 0.497(3) 1 d PDU C 1 H34A H 0.6502 0.6462 -0.0112 0.045 Uiso 0.497(3) 1 calc PR C 1 H34B H 0.5843 0.6130 0.0956 0.045 Uiso 0.497(3) 1 calc PR C 1 H34C H 0.7218 0.5334 0.0607 0.045 Uiso 0.497(3) 1 calc PR C 1 C35 C 0.5984(4) 0.8200(4) 0.0583(3) 0.0306(11) Uani 0.497(3) 1 d PDU C 1 H35A H 0.5877 0.8479 -0.0051 0.046 Uiso 0.497(3) 1 calc PR C 1 H35B H 0.6200 0.8755 0.0687 0.046 Uiso 0.497(3) 1 calc PR C 1 H35C H 0.5236 0.8161 0.1023 0.046 Uiso 0.497(3) 1 calc PR C 1 C36 C 0.8126(6) 0.7036(7) -0.0014(6) 0.0317(19) Uani 0.497(3) 1 d PDU C 1 H36A H 0.7963 0.7327 -0.0631 0.048 Uiso 0.497(3) 1 calc PR C 1 H36B H 0.8779 0.6247 0.0048 0.048 Uiso 0.497(3) 1 calc PR C 1 H36C H 0.8359 0.7594 0.0070 0.048 Uiso 0.497(3) 1 calc PR C 1 C27' C 0.7429(4) 0.6464(4) 0.0604(3) 0.0227(10) Uani 0.503(3) 1 d PDU C 2 C34' C 0.7915(4) 0.5167(4) 0.0542(3) 0.0316(11) Uani 0.503(3) 1 d PDU C 2 H34D H 0.8033 0.5171 -0.0097 0.047 Uiso 0.503(3) 1 calc PR C 2 H34E H 0.7339 0.4798 0.0953 0.047 Uiso 0.503(3) 1 calc PR C 2 H34F H 0.8682 0.4708 0.0730 0.047 Uiso 0.503(3) 1 calc PR C 2 C35' C 0.6240(4) 0.7101(5) 0.0294(4) 0.0346(12) Uani 0.503(3) 1 d PDU C 2 H35D H 0.6394 0.7099 -0.0349 0.052 Uiso 0.503(3) 1 calc PR C 2 H35E H 0.5867 0.7927 0.0339 0.052 Uiso 0.503(3) 1 calc PR C 2 H35F H 0.5701 0.6684 0.0693 0.052 Uiso 0.503(3) 1 calc PR C 2 C36' C 0.8330(7) 0.7010(8) -0.0096(6) 0.033(2) Uani 0.503(3) 1 d PDU C 2 H36D H 0.8397 0.6997 -0.0719 0.050 Uiso 0.503(3) 1 calc PR C 2 H36E H 0.9114 0.6547 0.0062 0.050 Uiso 0.503(3) 1 calc PR C 2 H36F H 0.8054 0.7838 -0.0080 0.050 Uiso 0.503(3) 1 calc PR C 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 Nb1 0.01678(8) 0.01169(8) 0.02106(9) -0.00228(6) -0.00767(7) -0.00558(6) P1 0.0404(3) 0.0282(3) 0.0229(3) -0.0026(2) -0.0148(3) -0.0127(3) Si1 0.0761(4) 0.0167(3) 0.0286(3) 0.0048(2) -0.0317(3) -0.0241(3) Si2 0.0148(2) 0.0195(3) 0.0208(3) -0.0050(2) -0.0058(2) -0.0031(2) Si3 0.0144(2) 0.0286(3) 0.0294(3) -0.0156(2) -0.0019(2) -0.0082(2) O1 0.0846(12) 0.0199(7) 0.0376(9) 0.0026(7) -0.0349(9) -0.0268(8) O2 0.0151(6) 0.0234(7) 0.0194(7) -0.0038(6) -0.0055(6) -0.0041(6) O3 0.0167(7) 0.0444(9) 0.0438(10) -0.0293(8) 0.0026(7) -0.0126(7) C1 0.0212(9) 0.0191(9) 0.0334(12) -0.0103(9) -0.0080(9) -0.0061(8) C4 0.0385(13) 0.0235(11) 0.0618(17) -0.0191(11) -0.0221(12) -0.0010(10) C5 0.0297(12) 0.0723(17) 0.112(3) -0.0681(18) 0.0020(15) -0.0198(13) C6 0.0697(16) 0.0329(12) 0.0261(12) -0.0001(10) -0.0211(12) -0.0261(12) C2 0.034(2) 0.022(2) 0.024(3) -0.0019(19) -0.012(2) -0.0138(18) C7 0.027(2) 0.035(3) 0.034(3) -0.006(2) -0.007(2) -0.011(2) C8 0.035(2) 0.033(2) 0.037(3) -0.005(2) -0.019(2) -0.011(2) C9 0.031(2) 0.038(3) 0.041(4) -0.006(2) 0.001(3) -0.026(2) C2' 0.025(2) 0.0148(19) 0.020(2) -0.0008(18) -0.0102(19) -0.0081(17) C7' 0.024(2) 0.024(2) 0.024(2) -0.0057(19) -0.0011(19) -0.0119(17) C8' 0.025(2) 0.038(2) 0.028(3) -0.010(2) -0.0034(19) -0.0128(19) C9' 0.035(2) 0.029(2) 0.026(3) -0.009(2) 0.003(2) -0.025(2) C3 0.034(2) 0.021(2) 0.021(2) -0.0005(17) -0.008(2) -0.0145(19) C10 0.041(2) 0.033(2) 0.024(2) -0.0024(19) -0.012(2) -0.013(2) C11 0.032(2) 0.031(2) 0.020(2) -0.0089(18) 0.0027(18) -0.0115(19) C12 0.052(3) 0.032(2) 0.020(2) -0.0074(18) -0.012(2) -0.019(2) C3' 0.025(2) 0.022(2) 0.020(2) -0.0055(17) -0.0051(18) -0.0105(18) C10' 0.042(2) 0.025(2) 0.021(2) -0.0003(18) -0.010(2) -0.015(2) C11' 0.032(2) 0.031(2) 0.022(3) -0.011(2) -0.001(2) -0.011(2) C13 0.022(2) 0.029(2) 0.024(3) -0.008(2) -0.0098(19) -0.009(2) C16 0.037(2) 0.037(3) 0.028(2) -0.011(2) -0.012(2) -0.009(2) C17 0.036(2) 0.043(3) 0.045(3) -0.014(2) -0.018(2) -0.016(2) C18 0.034(3) 0.042(3) 0.036(4) -0.008(3) -0.025(3) -0.004(3) C13' 0.023(3) 0.023(2) 0.024(3) 0.001(2) -0.009(2) -0.010(2) C16' 0.039(3) 0.032(2) 0.028(3) -0.002(2) -0.001(2) -0.016(2) C17' 0.046(3) 0.040(3) 0.025(2) -0.012(2) -0.005(2) -0.019(2) C18' 0.041(4) 0.033(4) 0.036(5) 0.003(3) -0.021(4) -0.004(3) C14 0.020(2) 0.028(2) 0.035(3) -0.013(2) -0.001(2) -0.0049(19) C19 0.030(2) 0.032(2) 0.045(3) -0.005(2) 0.002(2) -0.015(2) C20 0.035(3) 0.043(3) 0.030(3) -0.013(2) 0.000(2) -0.010(2) C21 0.020(3) 0.033(3) 0.039(4) -0.014(3) 0.003(3) -0.006(2) C14' 0.0116(19) 0.024(3) 0.023(3) -0.004(2) -0.0011(19) -0.0022(18) C19' 0.028(2) 0.043(3) 0.038(3) -0.003(2) -0.008(2) -0.021(2) C20' 0.022(2) 0.033(3) 0.026(2) -0.003(2) -0.0019(18) -0.0085(19) C21' 0.014(3) 0.050(4) 0.032(4) -0.002(3) -0.005(3) -0.005(3) C15 0.030(2) 0.020(2) 0.028(3) -0.007(2) -0.016(2) -0.0017(18) C22 0.038(2) 0.028(2) 0.041(3) -0.015(2) -0.015(2) -0.006(2) C23 0.043(3) 0.025(2) 0.041(3) -0.003(2) -0.014(2) -0.014(2) C24 0.041(3) 0.021(3) 0.058(5) -0.016(3) -0.022(3) 0.009(3) C15' 0.022(2) 0.027(3) 0.034(3) -0.019(2) -0.012(2) 0.002(2) C22' 0.041(3) 0.044(3) 0.040(3) -0.024(2) -0.014(2) -0.004(2) C23' 0.036(2) 0.035(3) 0.066(4) -0.026(3) -0.010(3) -0.012(2) C24' 0.042(4) 0.021(3) 0.053(4) -0.023(3) -0.011(3) -0.003(3) C25 0.0221(19) 0.027(2) 0.020(2) -0.0070(18) -0.0018(17) -0.0121(17) C28 0.039(2) 0.041(3) 0.027(2) -0.013(2) -0.009(2) -0.019(2) C29 0.030(2) 0.031(3) 0.039(3) -0.019(2) -0.001(2) -0.009(2) C30 0.028(2) 0.035(3) 0.024(3) -0.010(2) 0.000(2) -0.014(2) C25' 0.032(2) 0.022(2) 0.026(2) -0.0083(18) -0.0044(19) -0.0144(17) C28' 0.040(2) 0.019(2) 0.035(3) -0.0083(19) -0.009(2) -0.0061(19) C29' 0.042(3) 0.030(3) 0.029(3) -0.011(2) -0.005(2) -0.014(2) C30' 0.045(3) 0.039(3) 0.039(4) -0.011(3) -0.005(3) -0.033(3) C26 0.0188(19) 0.026(2) 0.022(2) -0.0004(18) -0.0083(18) -0.0093(18) C31 0.030(2) 0.032(2) 0.024(2) -0.0026(19) -0.0067(19) -0.0119(19) C32 0.025(2) 0.027(2) 0.035(3) -0.0098(19) -0.0065(19) -0.0067(18) C33 0.005(2) 0.038(4) 0.041(4) -0.015(3) -0.008(2) -0.001(2) C26' 0.023(2) 0.029(2) 0.024(3) -0.004(2) -0.0079(19) -0.0116(19) C31' 0.044(3) 0.039(3) 0.029(3) 0.000(2) -0.016(2) -0.021(2) C32' 0.030(2) 0.026(2) 0.037(3) -0.002(2) -0.010(2) -0.0103(19) C33' 0.040(4) 0.040(5) 0.033(5) 0.005(4) -0.007(4) -0.020(4) C27 0.025(2) 0.021(2) 0.027(2) -0.0049(19) -0.0055(19) -0.0100(18) C34 0.036(2) 0.028(2) 0.030(2) -0.0070(19) -0.013(2) -0.0126(19) C35 0.033(2) 0.028(2) 0.028(2) -0.0032(19) -0.011(2) -0.0107(19) C36 0.029(3) 0.039(3) 0.028(4) -0.014(3) -0.002(2) -0.013(2) C27' 0.026(2) 0.022(2) 0.019(2) -0.0031(19) -0.0077(18) -0.0082(19) C34' 0.032(2) 0.031(2) 0.030(3) -0.014(2) -0.003(2) -0.0099(19) C35' 0.034(2) 0.039(3) 0.036(3) -0.017(2) -0.013(2) -0.008(2) C36' 0.033(3) 0.034(3) 0.018(3) 0.000(3) 0.002(3) -0.013(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 Nb1 O2 1.8648(13) . ? Nb1 O3 1.8824(15) . ? Nb1 O1 1.8873(15) . ? Nb1 P1 2.3249(7) . ? P1 P1 2.1430(12) 2_666 ? Si1 O1 1.6672(16) . ? Si1 C2 1.740(5) . ? Si1 C3' 1.835(4) . ? Si1 C1 1.893(2) . ? Si1 C3 2.050(5) . ? Si1 C2' 2.084(4) . ? Si2 O2 1.6777(14) . ? Si2 C15' 1.887(6) . ? Si2 C13' 1.914(6) . ? Si2 C14 1.918(5) . ? Si2 C13 1.920(6) . ? Si2 C14' 1.924(5) . ? Si2 C15 1.945(6) . ? Si3 O3 1.6688(16) . ? Si3 C26' 1.838(5) . ? Si3 C27 1.828(5) . ? Si3 C25 1.893(4) . ? Si3 C25' 1.985(4) . ? Si3 C27' 1.987(5) . ? Si3 C26 1.976(4) . ? C1 C6 1.523(3) . ? C1 C4 1.537(3) . ? C1 C5 1.537(3) . ? C2 C8 1.513(6) . ? C2 C7 1.535(6) . ? C2 C9 1.543(6) . ? C2' C8' 1.540(6) . ? C2' C9' 1.550(6) . ? C2' C7' 1.551(6) . ? C3 C10 1.534(6) . ? C3 C12 1.540(6) . ? C3 C11 1.557(6) . ? C3' C11' 1.517(6) . ? C3' C10' 1.531(6) . ? C3' C12' 1.536(6) . ? C13 C16 1.525(6) . ? C13 C17 1.539(7) . ? C13 C18 1.537(8) . ? C13' C17' 1.527(7) . ? C13' C16' 1.535(6) . ? C13' C18' 1.546(9) . ? C14 C19 1.530(7) . ? C14 C21 1.543(8) . ? C14 C20 1.543(7) . ? C14' C20' 1.525(6) . ? C14' C19' 1.537(7) . ? C14' C21' 1.553(8) . ? C15 C22 1.543(7) . ? C15 C24 1.547(7) . ? C15 C23 1.549(6) . ? C15' C23' 1.516(7) . ? C15' C22' 1.533(7) . ? C15' C24' 1.537(8) . ? C25 C28 1.530(6) . ? C25 C29 1.541(6) . ? C25 C30 1.550(8) . ? C25' C29' 1.523(6) . ? C25' C30' 1.528(8) . ? C25' C28' 1.549(6) . ? C26 C31 1.536(6) . ? C26 C33 1.538(7) . ? C26 C32 1.545(6) . ? C26' C32' 1.530(6) . ? C26' C31' 1.542(7) . ? C26' C33' 1.543(8) . ? C27 C34 1.531(6) . ? C27 C36 1.536(7) . ? C27 C35 1.543(6) . ? C27' C36' 1.530(8) . ? C27' C35' 1.536(6) . ? C27' C34' 1.547(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Nb1 O3 115.25(7) . . ? O2 Nb1 O1 114.74(7) . . ? O3 Nb1 O1 107.08(8) . . ? O2 Nb1 P1 98.74(5) . . ? O3 Nb1 P1 111.07(5) . . ? O1 Nb1 P1 109.76(5) . . ? P1 P1 Nb1 106.15(4) 2_666 . ? O1 Si1 C2 106.51(17) . . ? O1 Si1 C3' 105.18(15) . . ? C2 Si1 C3' 90.0(2) . . ? O1 Si1 C1 107.48(9) . . ? C2 Si1 C1 121.02(17) . . ? C3' Si1 C1 124.39(15) . . ? O1 Si1 C3 106.21(14) . . ? C2 Si1 C3 112.9(2) . . ? C3' Si1 C3 25.04(16) . . ? C1 Si1 C3 101.80(14) . . ? O1 Si1 C2' 106.11(14) . . ? C2 Si1 C2' 17.67(18) . . ? C3' Si1 C2' 106.84(19) . . ? C1 Si1 C2' 105.64(14) . . ? C3 Si1 C2' 128.23(19) . . ? O2 Si2 C15' 104.04(17) . . ? O2 Si2 C13' 102.77(16) . . ? C15' Si2 C13' 116.0(2) . . ? O2 Si2 C14 107.95(16) . . ? C15' Si2 C14 96.6(2) . . ? C13' Si2 C14 127.5(2) . . ? O2 Si2 C13 105.33(15) . . ? C15' Si2 C13 127.7(2) . . ? C13' Si2 C13 14.7(2) . . ? C14 Si2 C13 113.8(2) . . ? O2 Si2 C14' 105.47(15) . . ? C15' Si2 C14' 113.5(2) . . ? C13' Si2 C14' 113.3(2) . . ? C14 Si2 C14' 17.3(2) . . ? C13 Si2 C14' 98.9(2) . . ? O2 Si2 C15 108.58(16) . . ? C15' Si2 C15 16.89(19) . . ? C13' Si2 C15 99.2(2) . . ? C14 Si2 C15 109.7(2) . . ? C13 Si2 C15 111.3(2) . . ? C14' Si2 C15 125.4(2) . . ? O3 Si3 C26' 107.19(16) . . ? O3 Si3 C27 102.41(16) . . ? C26' Si3 C27 131.6(2) . . ? O3 Si3 C25 103.87(14) . . ? C26' Si3 C25 90.3(2) . . ? C27 Si3 C25 118.6(2) . . ? O3 Si3 C25' 109.64(13) . . ? C26' Si3 C25' 113.1(2) . . ? C27 Si3 C25' 91.0(2) . . ? C25 Si3 C25' 27.82(17) . . ? O3 Si3 C27' 107.82(15) . . ? C26' Si3 C27' 113.0(2) . . ? C27 Si3 C27' 19.39(15) . . ? C25 Si3 C27' 131.90(19) . . ? C25' Si3 C27' 105.90(19) . . ? O3 Si3 C26 106.45(14) . . ? C26' Si3 C26 20.25(17) . . ? C27 Si3 C26 114.2(2) . . ? C25 Si3 C26 109.8(2) . . ? C25' Si3 C26 129.68(19) . . ? C27' Si3 C26 94.88(19) . . ? Si1 O1 Nb1 173.79(13) . . ? Si2 O2 Nb1 174.36(9) . . ? Si3 O3 Nb1 176.63(11) . . ? C6 C1 C4 107.83(19) . . ? C6 C1 C5 104.9(2) . . ? C4 C1 C5 108.42(19) . . ? C6 C1 Si1 111.03(15) . . ? C4 C1 Si1 111.97(16) . . ? C5 C1 Si1 112.35(18) . . ? C8 C2 C7 107.7(4) . . ? C8 C2 C9 109.0(4) . . ? C7 C2 C9 107.6(4) . . ? C8 C2 Si1 112.0(3) . . ? C7 C2 Si1 106.2(3) . . ? C9 C2 Si1 114.0(3) . . ? C8' C2' C9' 105.7(4) . . ? C8' C2' C7' 106.1(4) . . ? C9' C2' C7' 106.5(4) . . ? C8' C2' Si1 113.6(3) . . ? C9' C2' Si1 112.2(3) . . ? C7' C2' Si1 112.2(3) . . ? C10 C3 C12 107.6(4) . . ? C10 C3 C11 105.8(4) . . ? C12 C3 C11 106.2(4) . . ? C10 C3 Si1 109.9(3) . . ? C12 C3 Si1 110.6(3) . . ? C11 C3 Si1 116.5(3) . . ? C11' C3' C10' 106.4(4) . . ? C11' C3' C12' 108.0(4) . . ? C10' C3' C12' 108.2(4) . . ? C11' C3' Si1 104.8(3) . . ? C10' C3' Si1 114.3(3) . . ? C12' C3' Si1 114.7(3) . . ? C16 C13 C17 105.3(4) . . ? C16 C13 C18 108.9(5) . . ? C17 C13 C18 108.8(6) . . ? C16 C13 Si2 110.4(4) . . ? C17 C13 Si2 109.9(4) . . ? C18 C13 Si2 113.2(5) . . ? C17' C13' C16' 105.8(4) . . ? C17' C13' C18' 107.3(6) . . ? C16' C13' C18' 107.3(5) . . ? C17' C13' Si2 112.5(3) . . ? C16' C13' Si2 110.9(4) . . ? C18' C13' Si2 112.7(5) . . ? C19 C14 C21 108.0(6) . . ? C19 C14 C20 105.5(5) . . ? C21 C14 C20 108.7(5) . . ? C19 C14 Si2 108.9(3) . . ? C21 C14 Si2 112.4(4) . . ? C20 C14 Si2 112.9(4) . . ? C20' C14' C19' 107.0(4) . . ? C20' C14' C21' 107.5(5) . . ? C19' C14' C21' 107.7(6) . . ? C20' C14' Si2 112.8(4) . . ? C19' C14' Si2 111.5(3) . . ? C21' C14' Si2 110.2(5) . . ? C22 C15 C24 106.0(6) . . ? C22 C15 C23 105.8(4) . . ? C24 C15 C23 106.4(5) . . ? C22 C15 Si2 110.3(3) . . ? C24 C15 Si2 116.4(6) . . ? C23 C15 Si2 111.2(3) . . ? C23' C15' C22' 107.3(5) . . ? C23' C15' C24' 109.5(6) . . ? C22' C15' C24' 108.2(6) . . ? C23' C15' Si2 110.8(4) . . ? C22' C15' Si2 111.6(4) . . ? C24' C15' Si2 109.5(6) . . ? C28 C25 C29 105.7(4) . . ? C28 C25 C30 107.1(5) . . ? C29 C25 C30 106.9(4) . . ? C28 C25 Si3 115.3(3) . . ? C29 C25 Si3 109.7(3) . . ? C30 C25 Si3 111.6(4) . . ? C29' C25' C30' 110.1(5) . . ? C29' C25' C28' 106.9(4) . . ? C30' C25' C28' 107.6(4) . . ? C29' C25' Si3 106.9(3) . . ? C30' C25' Si3 112.8(4) . . ? C28' C25' Si3 112.4(3) . . ? C31 C26 C33 108.6(5) . . ? C31 C26 C32 105.7(4) . . ? C33 C26 C32 107.2(5) . . ? C31 C26 Si3 114.8(3) . . ? C33 C26 Si3 109.1(4) . . ? C32 C26 Si3 111.2(3) . . ? C32' C26' C31' 106.2(4) . . ? C32' C26' C33' 107.2(5) . . ? C31' C26' C33' 107.8(6) . . ? C32' C26' Si3 108.2(3) . . ? C31' C26' Si3 109.8(3) . . ? C33' C26' Si3 117.1(5) . . ? C34 C27 C36 107.8(5) . . ? C34 C27 C35 106.1(4) . . ? C36 C27 C35 107.5(4) . . ? C34 C27 Si3 112.6(3) . . ? C36 C27 Si3 112.7(5) . . ? C35 C27 Si3 109.8(3) . . ? C36' C27' C35' 109.4(5) . . ? C36' C27' C34' 106.8(5) . . ? C35' C27' C34' 105.3(4) . . ? C36' C27' Si3 114.0(5) . . ? C35' C27' Si3 112.4(3) . . ? C34' C27' Si3 108.4(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.539 _refine_diff_density_min -0.660 _refine_diff_density_rms 0.075 data_eh6 _database_code_depnum_ccdc_archive 'CCDC 715088' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H162 Nb2 O6 P6 Si6' _chemical_formula_sum 'C72 H162 Nb2 O6 P6 Si6' _chemical_formula_weight 1664.20 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' Si Si 0.0817 0.0704 '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' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 33.163(2) _cell_length_b 13.0037(9) _cell_length_c 22.9736(15) _cell_angle_alpha 90.00 _cell_angle_beta 103.448(3) _cell_angle_gamma 90.00 _cell_volume 9635.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 9995 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 26.36 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.147 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3592 _exptl_absorpt_coefficient_mu 0.453 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8952 _exptl_absorpt_correction_T_max 0.9777 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 X8 APEX II diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52990 _diffrn_reflns_av_R_equivalents 0.0916 _diffrn_reflns_av_sigmaI/netI 0.0643 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 23.26 _reflns_number_total 6930 _reflns_number_gt 5781 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT+' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The specimen was a multiple twin. Due to main residue disorder, some carbon atoms were refined isotropically. Despite the restrictions imposed on the of disordered tertiary butyl groups, their geometry is sometimes on the edge of normal values. In particular, Si(3)-C(29') and Si(3)-C(33) are abnormally long. The data was affected by disordered crystallization solvent (diethyl ether) in the lattice, which was taken care of by the SQUEEZE procedure (from PLATON). The volumes occupied by the solvent were 180, 180, 180 and 180 \%A3, respectively; the number of electrons per unit cell deduced by SQUEEZE were 70, 71, 70, and 71. There were eight additional voids identified by SQUEEZE of 11 \%A3 each; four containing two electrons and four containing three electrons. Disorder in the peripheral tBu groups and twinning problems have led to a low accuracy structure; these problems, however, are likely to affect the accuracy of the metric parameters of the tertiary-butyl groups more than those of the core of the molecule. ; # SQUEEZE RESULTS # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material _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^)+(0.0000P)^2^+550.0000P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6930 _refine_ls_number_parameters 406 _refine_ls_number_restraints 392 _refine_ls_R_factor_all 0.1236 _refine_ls_R_factor_gt 0.1095 _refine_ls_wR_factor_ref 0.2584 _refine_ls_wR_factor_gt 0.2526 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.002 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 Nb1 Nb 0.10385(2) 0.14318(6) 0.04758(4) 0.02152(19) Uani 1 1 d U . . P1 P 0.02782(7) 0.18375(19) 0.04194(13) 0.0342(6) Uani 1 1 d U . . P2 P 0.05278(7) 0.0579(2) 0.10129(11) 0.0307(6) Uani 1 1 d U . . P3 P 0.03180(7) 0.03095(19) 0.00599(11) 0.0282(6) Uani 1 1 d U . . Si1 Si 0.14522(8) 0.32820(19) 0.15841(12) 0.0268(6) Uani 1 1 d U . . Si2 Si 0.16254(7) -0.0896(2) 0.06439(13) 0.0307(6) Uani 1 1 d U . . Si3 Si 0.09305(8) 0.2411(2) -0.10072(12) 0.0394(7) Uani 1 1 d U . . O1 O 0.12865(17) 0.2345(4) 0.1061(3) 0.0251(13) Uani 1 1 d U . . O2 O 0.13659(16) 0.0209(5) 0.0506(3) 0.0272(14) Uani 1 1 d U . . O3 O 0.10170(18) 0.1980(5) -0.0296(3) 0.0319(15) Uani 1 1 d U A . C1 C 0.1955(3) 0.3807(6) 0.1422(4) 0.040(2) Uani 1 1 d DU . . C2 C 0.2223(3) 0.2900(7) 0.1288(5) 0.056(3) Uani 1 1 d DU . . H2A H 0.2480 0.3165 0.1214 0.084 Uiso 1 1 calc R . . H2B H 0.2073 0.2531 0.0937 0.084 Uiso 1 1 calc R . . H2C H 0.2284 0.2437 0.1628 0.084 Uiso 1 1 calc R . . C3 C 0.1868(3) 0.4516(8) 0.0863(4) 0.061(3) Uani 1 1 d DU . . H3A H 0.2128 0.4776 0.0799 0.092 Uiso 1 1 calc R . . H3B H 0.1695 0.5088 0.0926 0.092 Uiso 1 1 calc R . . H3C H 0.1727 0.4127 0.0515 0.092 Uiso 1 1 calc R . . C4 C 0.2220(3) 0.4416(8) 0.1954(5) 0.057(3) Uani 1 1 d DU . . H4A H 0.2470 0.4661 0.1848 0.085 Uiso 1 1 calc R . . H4B H 0.2295 0.3971 0.2301 0.085 Uiso 1 1 calc R . . H4C H 0.2062 0.4997 0.2045 0.085 Uiso 1 1 calc R . . C5 C 0.1022(3) 0.4288(7) 0.1464(4) 0.030(2) Uani 1 1 d U . . C6 C 0.0861(3) 0.4519(8) 0.0795(5) 0.043(3) Uani 1 1 d U . . H6A H 0.0645 0.5037 0.0744 0.064 Uiso 1 1 calc R . . H6B H 0.0749 0.3895 0.0587 0.064 Uiso 1 1 calc R . . H6C H 0.1087 0.4771 0.0632 0.064 Uiso 1 1 calc R . . C7 C 0.1167(4) 0.5290(8) 0.1784(5) 0.052(3) Uani 1 1 d U . . H7A H 0.0940 0.5780 0.1709 0.078 Uiso 1 1 calc R . . H7B H 0.1396 0.5567 0.1636 0.078 Uiso 1 1 calc R . . H7C H 0.1257 0.5165 0.2211 0.078 Uiso 1 1 calc R . . C8 C 0.0651(3) 0.3928(9) 0.1692(5) 0.048(3) Uani 1 1 d U . . H8A H 0.0441 0.4462 0.1624 0.072 Uiso 1 1 calc R . . H8B H 0.0738 0.3783 0.2117 0.072 Uiso 1 1 calc R . . H8C H 0.0538 0.3309 0.1480 0.072 Uiso 1 1 calc R . . C9 C 0.1538(3) 0.2625(8) 0.2352(4) 0.036(2) Uani 1 1 d U . . C10 C 0.1576(4) 0.3401(8) 0.2866(5) 0.049(3) Uani 1 1 d U . . H10A H 0.1620 0.3035 0.3243 0.074 Uiso 1 1 calc R . . H10B H 0.1323 0.3801 0.2807 0.074 Uiso 1 1 calc R . . H10C H 0.1808 0.3856 0.2871 0.074 Uiso 1 1 calc R . . C11 C 0.1177(3) 0.1879(8) 0.2372(4) 0.040(2) Uani 1 1 d U . . H11A H 0.1228 0.1549 0.2761 0.060 Uiso 1 1 calc R . . H11B H 0.1158 0.1360 0.2064 0.060 Uiso 1 1 calc R . . H11C H 0.0919 0.2261 0.2304 0.060 Uiso 1 1 calc R . . C12 C 0.1930(3) 0.1983(9) 0.2485(6) 0.056(3) Uani 1 1 d U . . H12A H 0.1964 0.1658 0.2873 0.084 Uiso 1 1 calc R . . H12B H 0.2167 0.2423 0.2487 0.084 Uiso 1 1 calc R . . H12C H 0.1912 0.1459 0.2179 0.084 Uiso 1 1 calc R . . C13 C 0.1558(3) -0.1424(8) 0.1395(5) 0.039(2) Uani 1 1 d U . . C14 C 0.1585(3) -0.0564(8) 0.1865(5) 0.044(2) Uani 1 1 d U . . H14A H 0.1548 -0.0857 0.2237 0.066 Uiso 1 1 calc R . . H14B H 0.1369 -0.0059 0.1720 0.066 Uiso 1 1 calc R . . H14C H 0.1854 -0.0234 0.1932 0.066 Uiso 1 1 calc R . . C15 C 0.1125(3) -0.1916(8) 0.1345(6) 0.053(3) Uani 1 1 d U . . H15A H 0.1106 -0.2172 0.1734 0.079 Uiso 1 1 calc R . . H15B H 0.1088 -0.2479 0.1062 0.079 Uiso 1 1 calc R . . H15C H 0.0912 -0.1402 0.1209 0.079 Uiso 1 1 calc R . . C16 C 0.1891(3) -0.2229(8) 0.1675(5) 0.046(3) Uani 1 1 d U . . H16A H 0.1840 -0.2470 0.2051 0.070 Uiso 1 1 calc R . . H16B H 0.2164 -0.1917 0.1747 0.070 Uiso 1 1 calc R . . H16C H 0.1878 -0.2806 0.1403 0.070 Uiso 1 1 calc R . . C17 C 0.1414(3) -0.1862(8) 0.0012(5) 0.049(2) Uani 1 1 d U . . C18 C 0.1538(4) -0.1588(11) -0.0576(5) 0.071(3) Uani 1 1 d U . . H18A H 0.1425 -0.2097 -0.0879 0.107 Uiso 1 1 calc R . . H18B H 0.1838 -0.1581 -0.0507 0.107 Uiso 1 1 calc R . . H18C H 0.1430 -0.0915 -0.0711 0.107 Uiso 1 1 calc R . . C19 C 0.0932(3) -0.1827(9) -0.0154(6) 0.056(3) Uani 1 1 d U . . H19A H 0.0828 -0.2316 -0.0472 0.083 Uiso 1 1 calc R . . H19B H 0.0841 -0.1140 -0.0289 0.083 Uiso 1 1 calc R . . H19C H 0.0828 -0.2002 0.0194 0.083 Uiso 1 1 calc R . . C20 C 0.1560(4) -0.2937(9) 0.0171(6) 0.071(4) Uani 1 1 d U . . H20A H 0.1445 -0.3393 -0.0160 0.107 Uiso 1 1 calc R . . H20B H 0.1468 -0.3156 0.0524 0.107 Uiso 1 1 calc R . . H20C H 0.1860 -0.2959 0.0254 0.107 Uiso 1 1 calc R . . C21 C 0.2188(3) -0.0510(8) 0.0666(5) 0.037(2) Uani 1 1 d U . . C22 C 0.2201(3) 0.0229(9) 0.0153(5) 0.048(3) Uani 1 1 d U . . H22A H 0.2486 0.0429 0.0173 0.072 Uiso 1 1 calc R . . H22B H 0.2038 0.0835 0.0186 0.072 Uiso 1 1 calc R . . H22C H 0.2088 -0.0110 -0.0226 0.072 Uiso 1 1 calc R . . C23 C 0.2377(3) 0.0073(8) 0.1260(5) 0.040(2) Uani 1 1 d U . . H23A H 0.2660 0.0271 0.1266 0.061 Uiso 1 1 calc R . . H23B H 0.2375 -0.0372 0.1598 0.061 Uiso 1 1 calc R . . H23C H 0.2214 0.0684 0.1285 0.061 Uiso 1 1 calc R . . C24 C 0.2470(3) -0.1436(10) 0.0627(5) 0.054(3) Uani 1 1 d U . . H24A H 0.2750 -0.1196 0.0645 0.080 Uiso 1 1 calc R . . H24B H 0.2366 -0.1797 0.0253 0.080 Uiso 1 1 calc R . . H24C H 0.2473 -0.1899 0.0959 0.080 Uiso 1 1 calc R . . C25 C 0.1394(4) 0.3224(10) -0.1002(5) 0.032(4) Uiso 0.538(10) 1 d PDU A 1 C26 C 0.1338(6) 0.4274(11) -0.0710(7) 0.048(5) Uiso 0.538(10) 1 d PDU A 1 H26A H 0.1581 0.4698 -0.0694 0.072 Uiso 0.538(10) 1 calc PR A 1 H26B H 0.1303 0.4162 -0.0308 0.072 Uiso 0.538(10) 1 calc PR A 1 H26C H 0.1095 0.4619 -0.0946 0.072 Uiso 0.538(10) 1 calc PR A 1 C27 C 0.1808(4) 0.2769(12) -0.0618(6) 0.024(4) Uiso 0.538(10) 1 d PDU A 1 H27A H 0.2035 0.3232 -0.0631 0.035 Uiso 0.538(10) 1 calc PR A 1 H27B H 0.1860 0.2105 -0.0778 0.035 Uiso 0.538(10) 1 calc PR A 1 H27C H 0.1785 0.2688 -0.0207 0.035 Uiso 0.538(10) 1 calc PR A 1 C28 C 0.1438(5) 0.3451(14) -0.1642(5) 0.032(4) Uiso 0.538(10) 1 d PDU A 1 H28A H 0.1683 0.3868 -0.1626 0.048 Uiso 0.538(10) 1 calc PR A 1 H28B H 0.1194 0.3819 -0.1859 0.048 Uiso 0.538(10) 1 calc PR A 1 H28C H 0.1463 0.2809 -0.1845 0.048 Uiso 0.538(10) 1 calc PR A 1 C25' C 0.1451(4) 0.2571(9) -0.1196(5) 0.024(4) Uiso 0.462(10) 1 d PDU A 2 C26' C 0.1758(6) 0.3004(15) -0.0633(7) 0.029(6) Uiso 0.462(10) 1 d PDU A 2 H26D H 0.2027 0.3109 -0.0721 0.044 Uiso 0.462(10) 1 calc PR A 2 H26E H 0.1783 0.2520 -0.0305 0.044 Uiso 0.462(10) 1 calc PR A 2 H26F H 0.1654 0.3655 -0.0521 0.044 Uiso 0.462(10) 1 calc PR A 2 C27' C 0.1591(6) 0.1444(10) -0.1279(9) 0.043(6) Uiso 0.462(10) 1 d PDU A 2 H27D H 0.1857 0.1453 -0.1388 0.064 Uiso 0.462(10) 1 calc PR A 2 H27E H 0.1387 0.1111 -0.1594 0.064 Uiso 0.462(10) 1 calc PR A 2 H27F H 0.1617 0.1068 -0.0908 0.064 Uiso 0.462(10) 1 calc PR A 2 C28' C 0.1508(7) 0.3188(14) -0.1741(7) 0.035(6) Uiso 0.462(10) 1 d PDU A 2 H28D H 0.1797 0.3171 -0.1760 0.052 Uiso 0.462(10) 1 calc PR A 2 H28E H 0.1424 0.3896 -0.1705 0.052 Uiso 0.462(10) 1 calc PR A 2 H28F H 0.1339 0.2889 -0.2103 0.052 Uiso 0.462(10) 1 calc PR A 2 C29 C 0.0418(4) 0.2929(9) -0.1186(5) 0.028(4) Uiso 0.520(10) 1 d PDU A 1 C30 C 0.0058(5) 0.2138(12) -0.1249(8) 0.039(5) Uiso 0.520(10) 1 d PDU A 1 H30A H -0.0205 0.2496 -0.1351 0.058 Uiso 0.520(10) 1 calc PR A 1 H30B H 0.0083 0.1775 -0.0874 0.058 Uiso 0.520(10) 1 calc PR A 1 H30C H 0.0073 0.1650 -0.1563 0.058 Uiso 0.520(10) 1 calc PR A 1 C31 C 0.0344(6) 0.3726(13) -0.0707(7) 0.040(6) Uiso 0.520(10) 1 d PDU A 1 H31A H 0.0061 0.3975 -0.0820 0.060 Uiso 0.520(10) 1 calc PR A 1 H31B H 0.0534 0.4299 -0.0689 0.060 Uiso 0.520(10) 1 calc PR A 1 H31C H 0.0392 0.3395 -0.0319 0.060 Uiso 0.520(10) 1 calc PR A 1 C32 C 0.0361(6) 0.3516(14) -0.1783(6) 0.052(6) Uiso 0.520(10) 1 d PDU A 1 H32A H 0.0082 0.3792 -0.1897 0.078 Uiso 0.520(10) 1 calc PR A 1 H32B H 0.0406 0.3050 -0.2092 0.078 Uiso 0.520(10) 1 calc PR A 1 H32C H 0.0560 0.4075 -0.1736 0.078 Uiso 0.520(10) 1 calc PR A 1 C29' C 0.0672(4) 0.3934(11) -0.1097(5) 0.027(4) Uiso 0.480(10) 1 d PDU A 2 C30' C 0.0329(5) 0.391(2) -0.0738(8) 0.053(8) Uiso 0.480(10) 1 d PDU A 2 H30D H 0.0200 0.4586 -0.0755 0.079 Uiso 0.480(10) 1 calc PR A 2 H30E H 0.0452 0.3738 -0.0324 0.079 Uiso 0.480(10) 1 calc PR A 2 H30F H 0.0122 0.3405 -0.0909 0.079 Uiso 0.480(10) 1 calc PR A 2 C31' C 0.0984(5) 0.4762(14) -0.0770(8) 0.040(5) Uiso 0.480(10) 1 d PDU A 2 H31D H 0.0852 0.5432 -0.0820 0.060 Uiso 0.480(10) 1 calc PR A 2 H31E H 0.1226 0.4771 -0.0940 0.060 Uiso 0.480(10) 1 calc PR A 2 H31F H 0.1068 0.4597 -0.0347 0.060 Uiso 0.480(10) 1 calc PR A 2 C32' C 0.0480(6) 0.4310(17) -0.1737(6) 0.052(6) Uiso 0.480(10) 1 d PDU A 2 H32D H 0.0374 0.5002 -0.1722 0.078 Uiso 0.480(10) 1 calc PR A 2 H32E H 0.0256 0.3855 -0.1924 0.078 Uiso 0.480(10) 1 calc PR A 2 H32F H 0.0691 0.4310 -0.1968 0.078 Uiso 0.480(10) 1 calc PR A 2 C33 C 0.0970(4) 0.1071(11) -0.1469(6) 0.037(5) Uiso 0.539(9) 1 d PDU A 1 C34 C 0.1423(4) 0.0685(15) -0.1395(8) 0.049(5) Uiso 0.539(9) 1 d PDU A 1 H34A H 0.1422 0.0046 -0.1613 0.074 Uiso 0.539(9) 1 calc PR A 1 H34B H 0.1546 0.0571 -0.0974 0.074 Uiso 0.539(9) 1 calc PR A 1 H34C H 0.1582 0.1198 -0.1551 0.074 Uiso 0.539(9) 1 calc PR A 1 C35 C 0.0733(5) 0.0167(13) -0.1258(8) 0.046(5) Uiso 0.539(9) 1 d PDU A 1 H35A H 0.0757 -0.0442 -0.1491 0.069 Uiso 0.539(9) 1 calc PR A 1 H35B H 0.0443 0.0349 -0.1313 0.069 Uiso 0.539(9) 1 calc PR A 1 H35C H 0.0851 0.0030 -0.0838 0.069 Uiso 0.539(9) 1 calc PR A 1 C36 C 0.0785(5) 0.1245(15) -0.2145(6) 0.048(5) Uiso 0.539(9) 1 d PDU A 1 H36A H 0.0800 0.0610 -0.2361 0.071 Uiso 0.539(9) 1 calc PR A 1 H36B H 0.0940 0.1777 -0.2292 0.071 Uiso 0.539(9) 1 calc PR A 1 H36C H 0.0497 0.1455 -0.2205 0.071 Uiso 0.539(9) 1 calc PR A 1 C33' C 0.0544(4) 0.1607(10) -0.1539(6) 0.030(5) Uiso 0.461(9) 1 d PDU A 2 C34' C 0.0675(6) 0.0483(11) -0.1361(8) 0.028(5) Uiso 0.461(9) 1 d PDU A 2 H34D H 0.0486 0.0012 -0.1616 0.042 Uiso 0.461(9) 1 calc PR A 2 H34E H 0.0665 0.0368 -0.0947 0.042 Uiso 0.461(9) 1 calc PR A 2 H34F H 0.0955 0.0367 -0.1407 0.042 Uiso 0.461(9) 1 calc PR A 2 C35' C 0.0090(4) 0.1731(16) -0.1473(9) 0.036(5) Uiso 0.461(9) 1 d PDU A 2 H35D H -0.0091 0.1282 -0.1756 0.054 Uiso 0.461(9) 1 calc PR A 2 H35E H 0.0003 0.2439 -0.1553 0.054 Uiso 0.461(9) 1 calc PR A 2 H35F H 0.0075 0.1549 -0.1069 0.054 Uiso 0.461(9) 1 calc PR A 2 C36' C 0.0551(6) 0.1740(16) -0.2204(6) 0.042(6) Uiso 0.461(9) 1 d PDU A 2 H36D H 0.0339 0.1307 -0.2449 0.062 Uiso 0.461(9) 1 calc PR A 2 H36E H 0.0821 0.1543 -0.2262 0.062 Uiso 0.461(9) 1 calc PR A 2 H36F H 0.0497 0.2453 -0.2319 0.062 Uiso 0.461(9) 1 calc PR A 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 Nb1 0.0159(3) 0.0214(4) 0.0305(4) -0.0088(4) 0.0118(3) -0.0073(3) P1 0.0219(11) 0.0267(13) 0.0583(16) -0.0055(12) 0.0178(11) -0.0046(10) P2 0.0203(11) 0.0379(14) 0.0360(13) 0.0002(11) 0.0109(10) -0.0100(10) P3 0.0164(10) 0.0314(13) 0.0402(13) -0.0076(11) 0.0133(10) -0.0071(9) Si1 0.0290(12) 0.0186(12) 0.0353(14) -0.0078(10) 0.0128(11) -0.0083(10) Si2 0.0202(11) 0.0270(13) 0.0470(15) -0.0120(12) 0.0123(11) -0.0001(10) Si3 0.0314(13) 0.0593(19) 0.0297(14) -0.0104(13) 0.0118(12) -0.0185(14) O1 0.027(3) 0.020(3) 0.033(3) -0.014(2) 0.015(2) -0.012(2) O2 0.018(2) 0.029(3) 0.039(3) -0.010(2) 0.015(2) -0.005(2) O3 0.025(3) 0.037(4) 0.037(3) -0.004(3) 0.015(2) -0.009(3) C1 0.028(4) 0.043(5) 0.052(5) -0.017(4) 0.017(4) -0.020(3) C2 0.033(5) 0.055(6) 0.087(8) -0.032(5) 0.031(5) -0.022(4) C3 0.063(6) 0.066(7) 0.064(6) -0.003(5) 0.034(5) -0.032(5) C4 0.046(6) 0.050(6) 0.075(6) -0.024(5) 0.012(5) -0.027(5) C5 0.036(4) 0.017(4) 0.040(5) -0.005(3) 0.014(4) -0.003(3) C6 0.050(6) 0.029(5) 0.046(5) -0.002(4) 0.006(4) -0.002(5) C7 0.066(7) 0.030(5) 0.061(6) -0.019(5) 0.018(6) -0.006(4) C8 0.042(5) 0.044(6) 0.065(6) -0.010(5) 0.027(5) -0.003(4) C9 0.039(5) 0.039(5) 0.029(4) -0.002(3) 0.006(4) -0.001(4) C10 0.069(7) 0.040(6) 0.035(5) 0.001(4) 0.004(5) -0.015(5) C11 0.050(5) 0.038(5) 0.037(5) -0.002(4) 0.020(4) -0.001(4) C12 0.045(5) 0.047(6) 0.067(8) 0.009(5) -0.004(5) -0.004(4) C13 0.033(4) 0.031(5) 0.056(4) 0.003(4) 0.016(4) 0.000(4) C14 0.056(6) 0.030(5) 0.053(5) 0.002(4) 0.025(5) 0.009(4) C15 0.044(4) 0.030(6) 0.090(8) 0.009(5) 0.029(5) -0.004(4) C16 0.047(5) 0.026(5) 0.070(7) 0.006(4) 0.021(5) 0.004(4) C17 0.035(4) 0.041(5) 0.067(5) -0.032(4) 0.007(5) -0.002(4) C18 0.050(6) 0.102(9) 0.058(5) -0.037(5) 0.008(5) 0.020(7) C19 0.036(4) 0.043(6) 0.080(8) -0.039(6) -0.001(5) -0.001(4) C20 0.052(7) 0.045(5) 0.105(9) -0.037(5) -0.007(7) 0.012(5) C21 0.018(3) 0.045(5) 0.050(5) -0.007(4) 0.010(4) -0.002(3) C22 0.026(5) 0.068(6) 0.055(5) -0.003(5) 0.020(4) -0.013(5) C23 0.030(5) 0.034(5) 0.056(5) -0.010(4) 0.010(4) -0.009(4) C24 0.030(4) 0.079(6) 0.051(6) -0.017(5) 0.010(5) 0.017(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 Nb1 O1 1.838(5) . ? Nb1 O3 1.898(6) . ? Nb1 O2 1.917(6) . ? Nb1 P1 2.550(2) . ? Nb1 P2 2.567(3) . ? Nb1 P3 2.773(2) . ? P1 P2 2.167(4) . ? P1 P3 2.167(4) . ? P2 P3 2.166(4) . ? P3 P3 2.214(4) 5 ? Si1 O1 1.711(6) . ? Si1 C5 1.907(9) . ? Si1 C1 1.915(9) . ? Si1 C9 1.922(10) . ? Si2 O2 1.668(6) . ? Si2 C13 1.918(11) . ? Si2 C21 1.921(9) . ? Si2 C17 1.925(10) . ? Si3 O3 1.687(7) . ? Si3 C29 1.785(13) . ? Si3 C25 1.864(13) . ? Si3 C25' 1.888(15) . ? Si3 C33' 1.871(14) . ? Si3 C33 2.061(14) . ? Si3 C29' 2.147(15) . ? C1 C3 1.553(11) . ? C1 C4 1.548(10) . ? C1 C2 1.551(11) . ? C5 C7 1.517(13) . ? C5 C8 1.519(14) . ? C5 C6 1.535(13) . ? C9 C10 1.535(14) . ? C9 C12 1.516(15) . ? C9 C11 1.548(14) . ? C13 C15 1.551(14) . ? C13 C14 1.542(14) . ? C13 C16 1.550(14) . ? C17 C20 1.496(16) . ? C17 C18 1.541(17) . ? C17 C19 1.555(14) . ? C21 C22 1.529(15) . ? C21 C23 1.558(14) . ? C21 C24 1.541(15) . ? C25 C28 1.539(13) . ? C25 C27 1.564(13) . ? C25 C26 1.551(13) . ? C25' C28' 1.535(13) . ? C25' C27' 1.563(14) . ? C25' C26' 1.554(14) . ? C29 C32 1.543(13) . ? C29 C31 1.569(14) . ? C29 C30 1.556(13) . ? C29' C32' 1.540(13) . ? C29' C31' 1.560(14) . ? C29' C30' 1.553(14) . ? C33 C35 1.554(14) . ? C33 C36 1.548(13) . ? C33 C34 1.553(13) . ? C33' C36' 1.543(13) . ? C33' C35' 1.556(14) . ? C33' C34' 1.552(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Nb1 O3 110.7(3) . . ? O1 Nb1 O2 110.8(2) . . ? O3 Nb1 O2 104.1(3) . . ? O1 Nb1 P1 99.94(19) . . ? O3 Nb1 P1 93.05(19) . . ? O2 Nb1 P1 135.93(18) . . ? O1 Nb1 P2 99.24(19) . . ? O3 Nb1 P2 136.55(18) . . ? O2 Nb1 P2 93.22(19) . . ? P1 Nb1 P2 50.11(8) . . ? O1 Nb1 P3 142.66(19) . . ? O3 Nb1 P3 91.94(18) . . ? O2 Nb1 P3 90.66(17) . . ? P1 Nb1 P3 47.83(8) . . ? P2 Nb1 P3 47.66(8) . . ? P2 P1 P3 59.96(12) . . ? P2 P1 Nb1 65.37(9) . . ? P3 P1 Nb1 71.49(9) . . ? P3 P2 P1 60.03(12) . . ? P3 P2 Nb1 71.15(10) . . ? P1 P2 Nb1 64.52(9) . . ? P2 P3 P1 60.01(12) . . ? P2 P3 P3 104.91(17) . 5 ? P1 P3 P3 103.89(16) . 5 ? P2 P3 Nb1 61.19(8) . . ? P1 P3 Nb1 60.68(8) . . ? P3 P3 Nb1 162.50(18) 5 . ? O1 Si1 C5 106.3(4) . . ? O1 Si1 C1 105.6(3) . . ? C5 Si1 C1 112.5(4) . . ? O1 Si1 C9 106.5(4) . . ? C5 Si1 C9 112.6(4) . . ? C1 Si1 C9 112.8(4) . . ? O2 Si2 C13 108.5(4) . . ? O2 Si2 C21 103.6(4) . . ? C13 Si2 C21 112.7(4) . . ? O2 Si2 C17 109.7(4) . . ? C13 Si2 C17 110.3(5) . . ? C21 Si2 C17 111.8(5) . . ? O3 Si3 C29 106.6(4) . . ? O3 Si3 C25 103.2(4) . . ? C29 Si3 C25 121.8(5) . . ? O3 Si3 C25' 107.5(4) . . ? C29 Si3 C25' 141.1(6) . . ? C25 Si3 C25' 30.8(5) . . ? O3 Si3 C33' 112.5(5) . . ? C29 Si3 C33' 65.8(5) . . ? C25 Si3 C33' 139.5(6) . . ? C25' Si3 C33' 115.8(5) . . ? O3 Si3 C33 101.6(4) . . ? C29 Si3 C33 111.9(5) . . ? C25 Si3 C33 109.3(5) . . ? C25' Si3 C33 78.6(5) . . ? C33' Si3 C33 46.2(5) . . ? O3 Si3 C29' 111.9(4) . . ? C29 Si3 C29' 45.0(5) . . ? C25 Si3 C29' 77.7(5) . . ? C25' Si3 C29' 104.0(5) . . ? C33' Si3 C29' 104.8(5) . . ? C33 Si3 C29' 143.3(5) . . ? Si1 O1 Nb1 172.0(4) . . ? Si2 O2 Nb1 169.9(4) . . ? Si3 O3 Nb1 172.2(4) . . ? C3 C1 C4 108.1(8) . . ? C3 C1 C2 106.9(8) . . ? C4 C1 C2 107.4(7) . . ? C3 C1 Si1 111.8(6) . . ? C4 C1 Si1 113.0(6) . . ? C2 C1 Si1 109.5(6) . . ? C7 C5 C8 106.7(9) . . ? C7 C5 C6 108.3(8) . . ? C8 C5 C6 106.5(8) . . ? C7 C5 Si1 112.2(7) . . ? C8 C5 Si1 112.1(7) . . ? C6 C5 Si1 110.7(7) . . ? C10 C9 C12 107.1(8) . . ? C10 C9 C11 108.4(8) . . ? C12 C9 C11 106.4(9) . . ? C10 C9 Si1 112.4(7) . . ? C12 C9 Si1 111.5(8) . . ? C11 C9 Si1 110.8(6) . . ? C15 C13 C14 104.6(9) . . ? C15 C13 C16 108.0(8) . . ? C14 C13 C16 106.3(8) . . ? C15 C13 Si2 112.4(7) . . ? C14 C13 Si2 111.7(7) . . ? C16 C13 Si2 113.3(7) . . ? C20 C17 C18 107.1(10) . . ? C20 C17 C19 110.0(9) . . ? C18 C17 C19 104.3(9) . . ? C20 C17 Si2 112.6(8) . . ? C18 C17 Si2 112.7(8) . . ? C19 C17 Si2 109.8(7) . . ? C22 C21 C23 106.9(8) . . ? C22 C21 C24 108.6(9) . . ? C23 C21 C24 107.8(8) . . ? C22 C21 Si2 110.2(6) . . ? C23 C21 Si2 110.0(7) . . ? C24 C21 Si2 113.2(7) . . ? C28 C25 C27 110.3(11) . . ? C28 C25 C26 107.0(11) . . ? C27 C25 C26 105.5(10) . . ? C28 C25 Si3 111.3(9) . . ? C27 C25 Si3 113.7(9) . . ? C26 C25 Si3 108.6(10) . . ? C28' C25' C27' 107.2(12) . . ? C28' C25' C26' 108.0(12) . . ? C27' C25' C26' 106.6(12) . . ? C28' C25' Si3 122.5(11) . . ? C27' C25' Si3 103.8(10) . . ? C26' C25' Si3 107.7(11) . . ? C32 C29 C31 106.8(11) . . ? C32 C29 C30 108.1(11) . . ? C31 C29 C30 105.1(11) . . ? C32 C29 Si3 107.6(10) . . ? C31 C29 Si3 112.5(10) . . ? C30 C29 Si3 116.1(9) . . ? C32' C29' C31' 108.7(12) . . ? C32' C29' C30' 108.8(12) . . ? C31' C29' C30' 104.0(12) . . ? C32' C29' Si3 116.8(11) . . ? C31' C29' Si3 112.7(9) . . ? C30' C29' Si3 105.0(12) . . ? C35 C33 C36 108.1(11) . . ? C35 C33 C34 105.5(11) . . ? C36 C33 C34 107.9(12) . . ? C35 C33 Si3 112.4(10) . . ? C36 C33 Si3 109.6(10) . . ? C34 C33 Si3 113.1(10) . . ? C36' C33' C35' 108.8(12) . . ? C36' C33' C34' 107.4(12) . . ? C35' C33' C34' 106.9(12) . . ? C36' C33' Si3 114.7(11) . . ? C35' C33' Si3 114.2(10) . . ? C34' C33' Si3 104.3(9) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.741 _refine_diff_density_min -1.227 _refine_diff_density_rms 0.143