# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 1145/258 data_POB9819 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C42 H98 O14 Sr Ta2' _chemical_formula_weight 1276.72 _chemical_melting_point ? _chemical_compound_source ? 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' 'Sr' 'Sr' -1.5307 3.2498 '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 10.851(4) _cell_length_b 14.492(5) _cell_length_c 19.113(7) _cell_angle_alpha 97.43(3) _cell_angle_beta 96.38(4) _cell_angle_gamma 102.84(3) _cell_volume 2875.2(19) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 4.77 _cell_measurement_theta_max 12.49 _exptl_crystal_description blocks _exptl_crystal_colour Clear _exptl_crystal_size_max 0.67 _exptl_crystal_size_mid 0.67 _exptl_crystal_size_min 0.60 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.475 _exptl_crystal_density_method ? _exptl_crystal_F_000 1292 _exptl_absorpt_coefficient_mu 4.772 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 7.20 _diffrn_reflns_number 7893 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_sigmaI/netI 0.0777 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 22.50 _reflns_number_total 7417 _reflns_number_observed 5343 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 569 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0537P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6848 _refine_ls_number_parameters 592 _refine_ls_number_restraints 170 _refine_ls_R_factor_all 0.0787 _refine_ls_R_factor_obs 0.0473 _refine_ls_wR_factor_all 0.1130 _refine_ls_wR_factor_obs 0.0983 _refine_ls_goodness_of_fit_all 1.027 _refine_ls_goodness_of_fit_obs 1.091 _refine_ls_restrained_S_all 1.041 _refine_ls_restrained_S_obs 1.080 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Sr Sr 0.41415(10) 0.69638(7) 0.29064(5) 0.0390(2) Uani 1 d . . Ta1 Ta 0.20063(4) 0.45579(3) 0.22350(2) 0.03326(14) Uani 1 d . . Ta2 Ta 0.61504(4) 0.90638(3) 0.23199(2) 0.03705(15) Uani 1 d . . O1 O 0.2182(7) 0.5956(5) 0.2099(4) 0.033(2) Uani 1 d . . O2 O 0.3751(7) 0.5160(5) 0.2796(4) 0.038(2) Uani 1 d . . O3 O 0.4684(7) 0.8753(6) 0.2874(4) 0.041(2) Uani 1 d . . O4 O 0.5738(8) 0.7611(5) 0.2152(4) 0.041(2) Uani 1 d . . O5 O 0.2666(9) 0.6600(6) 0.3840(4) 0.055(2) Uani 1 d D . O6 O 0.6124(10) 0.7556(7) 0.3830(5) 0.059(2) Uani 1 d . . O7 O 0.2726(10) 0.4265(7) 0.1405(5) 0.062(3) Uani 1 d . . O8 O 0.0320(8) 0.4198(6) 0.1744(4) 0.048(2) Uani 1 d . . O9 O 0.1978(8) 0.3343(5) 0.2513(5) 0.056(2) Uani 1 d D . O10 O 0.1253(8) 0.4927(5) 0.3116(4) 0.045(2) Uani 1 d . . O11 O 0.7315(7) 0.9027(5) 0.3210(4) 0.044(2) Uani 1 d . . O12 O 0.6406(8) 1.0419(5) 0.2581(5) 0.055(2) Uani 1 d D . O13 O 0.7582(9) 0.9142(6) 0.1809(5) 0.055(2) Uani 1 d D . O14 O 0.5028(8) 0.9056(7) 0.1471(5) 0.062(3) Uani 1 d D . C1 C 0.1214(14) 0.6381(9) 0.1842(7) 0.058(3) Uani 1 d . . H1A H 0.0395(14) 0.5975(9) 0.1923(7) 0.070 Uiso 1 calc R . C2 C 0.1345(18) 0.7338(12) 0.2253(9) 0.082(5) Uani 1 d . . H2A H 0.1375(18) 0.7292(12) 0.2757(9) 0.123 Uiso 1 calc R . H2B H 0.0620(18) 0.7587(12) 0.2097(9) 0.123 Uiso 1 calc R . H2C H 0.2127(18) 0.7765(12) 0.2178(9) 0.123 Uiso 1 calc R . C3 C 0.1157(21) 0.6349(13) 0.1052(9) 0.090(6) Uani 1 d . . H3A H 0.1071(21) 0.5695(13) 0.0825(9) 0.135 Uiso 1 calc R . H3B H 0.1934(21) 0.6755(13) 0.0950(9) 0.135 Uiso 1 calc R . H3C H 0.0428(21) 0.6577(13) 0.0870(9) 0.135 Uiso 1 calc R . C4 C 0.4740(15) 0.4863(12) 0.3203(9) 0.072(4) Uani 1 d . . H4A H 0.5442(15) 0.5445(12) 0.3366(9) 0.086 Uiso 1 calc R . C5 C 0.5269(16) 0.4193(14) 0.2774(12) 0.097(6) Uani 1 d . . H5A H 0.5542(16) 0.4464(14) 0.2362(12) 0.146 Uiso 1 calc R . H5B H 0.4624(16) 0.3598(14) 0.2616(12) 0.146 Uiso 1 calc R . H5C H 0.5996(16) 0.4067(14) 0.3055(12) 0.146 Uiso 1 calc R . C6 C 0.4263(18) 0.4542(13) 0.3877(9) 0.081(5) Uani 1 d . . H6A H 0.3929(18) 0.5039(13) 0.4125(9) 0.122 Uiso 1 calc R . H6B H 0.4964(18) 0.4425(13) 0.4186(9) 0.122 Uiso 1 calc R . H6C H 0.3592(18) 0.3957(13) 0.3747(9) 0.122 Uiso 1 calc R . C7 C 0.4114(21) 0.9327(15) 0.3353(9) 0.090(6) Uani 1 d . . H7A H 0.3461(21) 0.8830(15) 0.3506(9) 0.109 Uiso 1 calc R . C8 C 0.4861(27) 0.9761(19) 0.4002(10) 0.137(11) Uani 1 d . . H8A H 0.5336(27) 0.9323(19) 0.4177(10) 0.206 Uiso 1 calc R . H8B H 0.4316(27) 0.9920(19) 0.4344(10) 0.206 Uiso 1 calc R . H8C H 0.5454(27) 1.0341(19) 0.3935(10) 0.206 Uiso 1 calc R . C9 C 0.3308(18) 0.9875(14) 0.2991(10) 0.086(5) Uani 1 d . . H9A H 0.2842(18) 0.9488(14) 0.2549(10) 0.129 Uiso 1 calc R . H9B H 0.3846(18) 1.0458(14) 0.2889(10) 0.129 Uiso 1 calc R . H9C H 0.2708(18) 1.0038(14) 0.3298(10) 0.129 Uiso 1 calc R . C10 C 0.6287(13) 0.7026(9) 0.1688(7) 0.053(3) Uani 1 d . . H10A H 0.6654(13) 0.7404(9) 0.1333(7) 0.064 Uiso 1 calc R . C11 C 0.7338(20) 0.6723(15) 0.2108(12) 0.098(6) Uani 1 d . . H11A H 0.7978(20) 0.7287(15) 0.2349(12) 0.147 Uiso 1 calc R . H11B H 0.7727(20) 0.6335(15) 0.1789(12) 0.147 Uiso 1 calc R . H11C H 0.6990(20) 0.6351(15) 0.2459(12) 0.147 Uiso 1 calc R . C12 C 0.5268(17) 0.6178(11) 0.1303(9) 0.079(5) Uani 1 d . . H12A H 0.4605(17) 0.6400(11) 0.1038(9) 0.119 Uiso 1 calc R . H12B H 0.4901(17) 0.5802(11) 0.1647(9) 0.119 Uiso 1 calc R . H12C H 0.5639(17) 0.5786(11) 0.0977(9) 0.119 Uiso 1 calc R . C13 C 0.2634(26) 0.7044(22) 0.4539(9) 0.078(11) Uani 0.55 d PD 1 H13A H 0.3328(26) 0.7636(22) 0.4636(9) 0.094 Uiso 0.55 calc PR 1 C14 C 0.2912(26) 0.6461(21) 0.5065(10) 0.068(7) Uani 0.55 d PD 1 H14A H 0.3715(26) 0.6292(21) 0.5007(10) 0.102 Uiso 0.55 calc PR 1 H14B H 0.2232(26) 0.5882(21) 0.5002(10) 0.102 Uiso 0.55 calc PR 1 H14C H 0.2975(26) 0.6818(21) 0.5538(10) 0.102 Uiso 0.55 calc PR 1 C15 C 0.1466(37) 0.7336(37) 0.4574(16) 0.104(13) Uani 0.55 d PDU 1 H15A H 0.1345(37) 0.7723(37) 0.4206(16) 0.156 Uiso 0.55 calc PR 1 H15B H 0.1502(37) 0.7710(37) 0.5039(16) 0.156 Uiso 0.55 calc PR 1 H15C H 0.0759(37) 0.6774(37) 0.4503(16) 0.156 Uiso 0.55 calc PR 1 C13' C 0.2190(27) 0.6806(19) 0.4492(11) 0.039(8) Uiso 0.45 d PD 2 H13B H 0.1588(27) 0.6245(19) 0.4609(11) 0.046 Uiso 0.45 calc PR 2 C14' C 0.3329(44) 0.7172(45) 0.5035(18) 0.143(23) Uiso 0.45 d PD 2 H14D H 0.3752(44) 0.6659(45) 0.5101(18) 0.215 Uiso 0.45 calc PR 2 H14E H 0.3075(44) 0.7405(45) 0.5483(18) 0.215 Uiso 0.45 calc PR 2 H14F H 0.3910(44) 0.7691(45) 0.4880(18) 0.215 Uiso 0.45 calc PR 2 C15' C 0.1617(62) 0.7622(41) 0.4429(28) 0.143(33) Uiso 0.45 d PD 2 H15D H 0.0855(62) 0.7424(41) 0.4076(28) 0.214 Uiso 0.45 calc PR 2 H15E H 0.2225(62) 0.8134(41) 0.4283(28) 0.214 Uiso 0.45 calc PR 2 H15F H 0.1390(62) 0.7848(41) 0.4886(28) 0.214 Uiso 0.45 calc PR 2 C16 C 0.6677(22) 0.7306(16) 0.4494(8) 0.096(7) Uani 1 d . . H16A H 0.6035(22) 0.6749(16) 0.4585(8) 0.116 Uiso 1 calc R . C17 C 0.6770(32) 0.8037(18) 0.5091(11) 0.139(11) Uani 1 d . . H17A H 0.5959(32) 0.8214(18) 0.5094(11) 0.209 Uiso 1 calc R . H17B H 0.7432(32) 0.8594(18) 0.5056(11) 0.209 Uiso 1 calc R . H17C H 0.6982(32) 0.7798(18) 0.5529(11) 0.209 Uiso 1 calc R . C18 C 0.7767(24) 0.6960(19) 0.4405(12) 0.119(8) Uani 1 d . . H18A H 0.7582(24) 0.6471(19) 0.3985(12) 0.179 Uiso 1 calc R . H18B H 0.8011(24) 0.6687(19) 0.4821(12) 0.179 Uiso 1 calc R . H18C H 0.8461(24) 0.7483(19) 0.4347(12) 0.179 Uiso 1 calc R . C19 C 0.2737(20) 0.3697(13) 0.0749(10) 0.090(6) Uani 1 d . . H19A H 0.2096(20) 0.3081(13) 0.0707(10) 0.108 Uiso 1 calc R . C20 C 0.2393(23) 0.4203(22) 0.0151(12) 0.129(9) Uani 1 d U . H20A H 0.1553(23) 0.4322(22) 0.0176(12) 0.193 Uiso 1 calc R . H20B H 0.2386(23) 0.3808(22) -0.0300(12) 0.193 Uiso 1 calc R . H20C H 0.3017(23) 0.4808(22) 0.0189(12) 0.193 Uiso 1 calc R . C21 C 0.4035(22) 0.3498(17) 0.0730(12) 0.112(7) Uani 1 d . . H21A H 0.4234(22) 0.3170(17) 0.1124(12) 0.169 Uiso 1 calc R . H21B H 0.4670(22) 0.4099(17) 0.0772(12) 0.169 Uiso 1 calc R . H21C H 0.4040(22) 0.3098(17) 0.0283(12) 0.169 Uiso 1 calc R . C22 C -0.0629(16) 0.3838(13) 0.1169(11) 0.082(5) Uani 1 d . . H22A H -0.0283(16) 0.4134(13) 0.0771(11) 0.098 Uiso 1 calc R . C23 C -0.0841(18) 0.2787(11) 0.0926(11) 0.089(5) Uani 1 d . . H23A H -0.0024(18) 0.2626(11) 0.0900(11) 0.134 Uiso 1 calc R . H23B H -0.1355(18) 0.2613(11) 0.0459(11) 0.134 Uiso 1 calc R . H23C H -0.1282(18) 0.2438(11) 0.1262(11) 0.134 Uiso 1 calc R . C24 C -0.1806(18) 0.4149(14) 0.1224(13) 0.105(7) Uani 1 d U . H24A H -0.1604(18) 0.4835(14) 0.1384(13) 0.157 Uiso 1 calc R . H24B H -0.2263(18) 0.3821(14) 0.1565(13) 0.157 Uiso 1 calc R . H24C H -0.2335(18) 0.3996(14) 0.0762(13) 0.157 Uiso 1 calc R . C25 C 0.1400(27) 0.2363(10) 0.2375(12) 0.064(7) Uani 0.55 d PDU 1 H25A H 0.0497(27) 0.2297(10) 0.2176(12) 0.077 Uiso 0.55 calc PR 1 C26 C 0.1930(41) 0.1791(18) 0.1865(19) 0.113(15) Uani 0.55 d PDU 1 H26A H 0.1925(41) 0.2052(18) 0.1423(19) 0.169 Uiso 0.55 calc PR 1 H26B H 0.1419(41) 0.1136(18) 0.1775(19) 0.169 Uiso 0.55 calc PR 1 H26C H 0.2801(41) 0.1802(18) 0.2056(19) 0.169 Uiso 0.55 calc PR 1 C27 C 0.1393(45) 0.1991(20) 0.3045(15) 0.107(12) Uani 0.55 d PDU 1 H27A H 0.1035(45) 0.2384(20) 0.3378(15) 0.161 Uiso 0.55 calc PR 1 H27B H 0.2261(45) 0.2002(20) 0.3242(15) 0.161 Uiso 0.55 calc PR 1 H27C H 0.0880(45) 0.1337(20) 0.2962(15) 0.161 Uiso 0.55 calc PR 1 C25' C 0.2065(29) 0.2433(14) 0.2637(16) 0.066(9) Uiso 0.45 d PDU 2 H25B H 0.2721(29) 0.2514(14) 0.3058(16) 0.080 Uiso 0.45 calc PR 2 C26' C 0.2468(40) 0.1907(24) 0.2048(20) 0.079(13) Uiso 0.45 d PDU 2 H26D H 0.3273(40) 0.2275(24) 0.1947(20) 0.119 Uiso 0.45 calc PR 2 H26E H 0.1827(40) 0.1794(24) 0.1630(20) 0.119 Uiso 0.45 calc PR 2 H26F H 0.2576(40) 0.1298(24) 0.2169(20) 0.119 Uiso 0.45 calc PR 2 C27' C 0.0860(34) 0.1913(23) 0.2810(25) 0.086(13) Uiso 0.45 d PDU 2 H27D H 0.0619(34) 0.2287(23) 0.3208(25) 0.129 Uiso 0.45 calc PR 2 H27E H 0.0953(34) 0.1304(23) 0.2939(25) 0.129 Uiso 0.45 calc PR 2 H27F H 0.0204(34) 0.1800(23) 0.2400(25) 0.129 Uiso 0.45 calc PR 2 C28 C 0.0153(13) 0.4416(10) 0.3345(7) 0.054(3) Uani 1 d . . H28A H -0.0185(13) 0.3820(10) 0.2997(7) 0.064 Uiso 1 calc R . C29 C 0.0447(21) 0.4128(16) 0.4054(9) 0.099(6) Uani 1 d . . H29A H 0.1103(21) 0.3771(16) 0.4035(9) 0.149 Uiso 1 calc R . H29B H -0.0319(21) 0.3729(16) 0.4174(9) 0.149 Uiso 1 calc R . H29C H 0.0748(21) 0.4696(16) 0.4413(9) 0.149 Uiso 1 calc R . C30 C -0.0847(17) 0.4967(16) 0.3333(12) 0.093(6) Uani 1 d . . H30A H -0.1005(17) 0.5138(16) 0.2862(12) 0.140 Uiso 1 calc R . H30B H -0.0561(17) 0.5545(16) 0.3683(12) 0.140 Uiso 1 calc R . H30C H -0.1628(17) 0.4578(16) 0.3444(12) 0.140 Uiso 1 calc R . C31 C 0.8535(14) 0.9682(10) 0.3438(8) 0.059(4) Uani 1 d . . H31A H 0.8662(14) 1.0154(10) 0.3105(8) 0.071 Uiso 1 calc R . C32 C 0.8600(23) 1.0212(15) 0.4173(10) 0.110(7) Uani 1 d . . H32A H 0.7928(23) 1.0555(15) 0.4179(10) 0.165 Uiso 1 calc R . H32B H 0.9424(23) 1.0664(15) 0.4310(10) 0.165 Uiso 1 calc R . H32C H 0.8491(23) 0.9759(15) 0.4506(10) 0.165 Uiso 1 calc R . C33 C 0.9566(17) 0.9141(17) 0.3409(15) 0.119(9) Uani 1 d . . H33A H 0.9506(17) 0.8804(17) 0.2929(15) 0.178 Uiso 1 calc R . H33B H 0.9462(17) 0.8682(17) 0.3739(15) 0.178 Uiso 1 calc R . H33C H 1.0396(17) 0.9587(17) 0.3542(15) 0.178 Uiso 1 calc R . C34 C 0.6853(20) 1.1352(10) 0.2428(10) 0.053(5) Uani 0.65 d PD 1 H34A H 0.7648(20) 1.1391(10) 0.2212(10) 0.064 Uiso 0.65 calc PR 1 C35 C 0.7105(40) 1.2029(17) 0.3092(15) 0.105(12) Uani 0.65 d PDU 1 H35A H 0.7757(40) 1.1882(17) 0.3419(15) 0.158 Uiso 0.65 calc PR 1 H35B H 0.6326(40) 1.1980(17) 0.3305(15) 0.158 Uiso 0.65 calc PR 1 H35C H 0.7398(40) 1.2676(17) 0.2993(15) 0.158 Uiso 0.65 calc PR 1 C36 C 0.5866(40) 1.1570(18) 0.1929(19) 0.082(15) Uani 0.65 d PDU 1 H36A H 0.5704(40) 1.1118(18) 0.1489(19) 0.123 Uiso 0.65 calc PR 1 H36B H 0.6157(40) 1.2216(18) 0.1828(19) 0.123 Uiso 0.65 calc PR 1 H36C H 0.5086(40) 1.1520(18) 0.2140(19) 0.123 Uiso 0.65 calc PR 1 C34' C 0.6265(36) 1.1359(15) 0.2620(21) 0.061(12) Uiso 0.35 d PD 2 H34B H 0.5610(36) 1.1453(15) 0.2926(21) 0.074 Uiso 0.35 calc PR 2 C35' C 0.7483(46) 1.2012(25) 0.2922(32) 0.079(19) Uiso 0.35 d PD 2 H35D H 0.7738(46) 1.1891(25) 0.3398(32) 0.119 Uiso 0.35 calc PR 2 H35E H 0.7401(46) 1.2668(25) 0.2946(32) 0.119 Uiso 0.35 calc PR 2 H35F H 0.8124(46) 1.1912(25) 0.2624(32) 0.119 Uiso 0.35 calc PR 2 C36' C 0.5877(87) 1.1537(41) 0.1906(33) 0.109(36) Uiso 0.35 d PDU 2 H36D H 0.5063(87) 1.1099(41) 0.1706(33) 0.163 Uiso 0.35 calc PR 2 H36E H 0.6516(87) 1.1436(41) 0.1607(33) 0.163 Uiso 0.35 calc PR 2 H36F H 0.5793(87) 1.2192(41) 0.1929(33) 0.163 Uiso 0.35 calc PR 2 C37 C 0.8049(17) 0.9203(13) 0.1155(8) 0.061(5) Uani 0.75 d PD 1 H37A H 0.7339(17) 0.8859(13) 0.0776(8) 0.073 Uiso 0.75 calc PR 1 C38 C 0.8373(30) 1.0199(17) 0.1042(18) 0.100(10) Uani 0.75 d PD 1 H38A H 0.7647(30) 1.0476(17) 0.1095(18) 0.150 Uiso 0.75 calc PR 1 H38B H 0.8593(30) 1.0226(17) 0.0566(18) 0.150 Uiso 0.75 calc PR 1 H38C H 0.9096(30) 1.0556(17) 0.1391(18) 0.150 Uiso 0.75 calc PR 1 C39 C 0.9089(24) 0.8733(18) 0.1085(16) 0.095(8) Uani 0.75 d PD 1 H39A H 0.8821(24) 0.8076(18) 0.1166(16) 0.143 Uiso 0.75 calc PR 1 H39B H 0.9822(24) 0.9070(18) 0.1435(16) 0.143 Uiso 0.75 calc PR 1 H39C H 0.9320(24) 0.8740(18) 0.0610(16) 0.143 Uiso 0.75 calc PR 1 C37' C 0.8548(36) 0.9662(33) 0.1502(25) 0.064(16) Uiso 0.25 d PD 2 H37B H 0.8869(36) 1.0304(33) 0.1796(25) 0.077 Uiso 0.25 calc PR 2 C38' C 0.8080(77) 0.9778(73) 0.0788(31) 0.116(43) Uiso 0.25 d PD 2 H38D H 0.7380(77) 1.0092(73) 0.0804(31) 0.175 Uiso 0.25 calc PR 2 H38E H 0.7782(77) 0.9154(73) 0.0492(31) 0.175 Uiso 0.25 calc PR 2 H38F H 0.8764(77) 1.0165(73) 0.0590(31) 0.175 Uiso 0.25 calc PR 2 C39' C 0.9594(57) 0.9192(79) 0.1481(58) 0.156(52) Uiso 0.25 d PD 2 H39D H 0.9906(57) 0.9116(79) 0.1961(58) 0.235 Uiso 0.25 calc PR 2 H39E H 1.0279(57) 0.9579(79) 0.1284(58) 0.235 Uiso 0.25 calc PR 2 H39F H 0.9298(57) 0.8568(79) 0.1185(58) 0.235 Uiso 0.25 calc PR 2 C40 C 0.4013(16) 0.8615(16) 0.0959(9) 0.056(6) Uani 0.60 d PD 1 H40A H 0.3598(16) 0.8001(16) 0.1102(9) 0.067 Uiso 0.60 calc PR 1 C41 C 0.3064(28) 0.9183(31) 0.0896(16) 0.071(9) Uani 0.60 d PDU 1 H41A H 0.2795(28) 0.9325(31) 0.1357(16) 0.107 Uiso 0.60 calc PR 1 H41B H 0.2332(28) 0.8825(31) 0.0555(16) 0.107 Uiso 0.60 calc PR 1 H41C H 0.3435(28) 0.9778(31) 0.0735(16) 0.107 Uiso 0.60 calc PR 1 C42 C 0.4436(39) 0.8392(39) 0.0270(12) 0.108(20) Uani 0.60 d PDU 1 H42A H 0.5066(39) 0.8014(39) 0.0321(12) 0.162 Uiso 0.60 calc PR 1 H42B H 0.4813(39) 0.8983(39) 0.0107(12) 0.162 Uiso 0.60 calc PR 1 H42C H 0.3710(39) 0.8030(39) -0.0074(12) 0.162 Uiso 0.60 calc PR 1 C40' C 0.4499(32) 0.9233(26) 0.0832(12) 0.061(9) Uiso 0.40 d PD 2 H40B H 0.5092(32) 0.9798(26) 0.0715(12) 0.073 Uiso 0.40 calc PR 2 C41' C 0.3291(48) 0.9482(57) 0.0868(34) 0.123(38) Uiso 0.40 d PD 2 H41D H 0.3389(48) 1.0008(57) 0.1255(34) 0.184 Uiso 0.40 calc PR 2 H41E H 0.2664(48) 0.8932(57) 0.0952(34) 0.184 Uiso 0.40 calc PR 2 H41F H 0.3007(48) 0.9674(57) 0.0422(34) 0.184 Uiso 0.40 calc PR 2 C42' C 0.4409(85) 0.8450(57) 0.0263(21) 0.132(35) Uiso 0.40 d PDU 2 H42D H 0.5238(85) 0.8304(57) 0.0256(21) 0.199 Uiso 0.40 calc PR 2 H42E H 0.4137(85) 0.8631(57) -0.0189(21) 0.199 Uiso 0.40 calc PR 2 H42F H 0.3793(85) 0.7890(57) 0.0341(21) 0.199 Uiso 0.40 calc PR 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 Sr 0.0414(6) 0.0386(5) 0.0369(5) 0.0036(4) 0.0088(4) 0.0090(4) Ta1 0.0352(3) 0.0329(2) 0.0342(3) 0.0050(2) 0.0082(2) 0.0120(2) Ta2 0.0410(3) 0.0314(3) 0.0390(3) 0.0045(2) 0.0019(2) 0.0118(2) O1 0.046(4) 0.030(3) 0.031(4) 0.016(3) 0.013(3) 0.017(3) O2 0.030(4) 0.042(4) 0.050(4) 0.012(3) 0.005(3) 0.021(3) O3 0.040(4) 0.047(4) 0.043(4) 0.002(3) 0.012(3) 0.022(3) O4 0.053(5) 0.031(4) 0.040(4) -0.001(3) 0.018(4) 0.012(3) O5 0.060(5) 0.062(5) 0.043(5) -0.003(4) 0.021(4) 0.016(4) O6 0.071(6) 0.064(5) 0.044(5) 0.020(4) -0.007(4) 0.019(5) O7 0.080(7) 0.053(5) 0.054(5) -0.013(4) 0.034(5) 0.017(5) O8 0.045(5) 0.044(4) 0.050(5) 0.006(4) 0.000(4) 0.004(4) O9 0.052(5) 0.046(5) 0.072(6) 0.010(4) 0.005(4) 0.014(4) O10 0.047(5) 0.042(4) 0.045(4) 0.007(3) 0.015(4) 0.006(4) O11 0.041(4) 0.043(4) 0.044(4) 0.002(3) -0.005(3) 0.011(3) O12 0.056(5) 0.028(4) 0.079(6) 0.005(4) 0.007(5) 0.011(4) O13 0.063(6) 0.035(4) 0.068(6) 0.013(4) 0.023(5) 0.004(4) O14 0.051(5) 0.076(6) 0.055(5) 0.025(5) -0.021(4) 0.011(5) C1 0.069(9) 0.046(7) 0.060(8) 0.019(6) -0.006(7) 0.016(6) C2 0.090(12) 0.075(10) 0.083(11) 0.008(8) -0.014(9) 0.040(9) C3 0.118(15) 0.079(11) 0.066(10) 0.018(8) -0.021(10) 0.020(10) C4 0.049(8) 0.074(10) 0.092(11) 0.006(8) -0.012(8) 0.029(7) C5 0.052(9) 0.100(13) 0.155(19) 0.021(12) 0.010(10) 0.054(10) C6 0.095(12) 0.079(11) 0.072(10) 0.031(8) -0.011(9) 0.027(9) C7 0.126(16) 0.114(14) 0.061(10) 0.002(9) 0.024(10) 0.091(13) C8 0.198(28) 0.168(23) 0.064(12) -0.038(13) 0.013(14) 0.118(22) C9 0.085(12) 0.092(12) 0.099(13) 0.013(10) 0.021(10) 0.056(10) C10 0.067(8) 0.044(7) 0.051(7) -0.005(5) 0.023(6) 0.016(6) C11 0.095(14) 0.093(13) 0.122(16) 0.007(11) 0.027(12) 0.058(11) C12 0.087(11) 0.061(9) 0.077(10) -0.014(8) 0.044(9) -0.010(8) C13 0.039(16) 0.127(30) 0.051(17) -0.017(17) -0.011(13) 0.012(18) C14 0.059(15) 0.098(21) 0.045(13) 0.000(13) 0.006(11) 0.022(15) C15 0.119(27) 0.146(29) 0.067(18) 0.002(20) 0.053(19) 0.062(23) C16 0.132(17) 0.130(16) 0.048(9) 0.016(9) -0.011(9) 0.085(14) C17 0.228(34) 0.111(17) 0.073(13) 0.006(12) -0.025(17) 0.055(20) C18 0.132(20) 0.138(20) 0.101(15) 0.028(14) -0.015(14) 0.074(17) C19 0.108(14) 0.074(11) 0.084(12) -0.021(9) 0.042(11) 0.022(10) C20 0.099(15) 0.198(24) 0.080(13) -0.010(14) 0.036(11) 0.024(15) C21 0.119(17) 0.119(17) 0.112(16) -0.017(13) 0.035(13) 0.066(14) C22 0.057(9) 0.077(11) 0.095(12) -0.017(9) -0.027(9) 0.019(8) C23 0.087(12) 0.054(9) 0.103(13) -0.010(8) -0.017(10) -0.005(8) C24 0.069(11) 0.088(12) 0.137(17) -0.033(11) -0.025(11) 0.026(9) C25 0.096(19) 0.020(10) 0.078(16) 0.016(10) 0.005(15) 0.015(11) C26 0.119(29) 0.032(15) 0.164(35) -0.006(18) -0.021(29) 0.002(17) C27 0.169(27) 0.070(17) 0.074(18) 0.043(15) -0.024(20) 0.011(18) C28 0.051(8) 0.055(8) 0.053(8) 0.013(6) 0.025(6) 0.000(6) C29 0.114(15) 0.118(15) 0.057(10) 0.028(10) 0.028(10) -0.008(12) C30 0.058(10) 0.116(15) 0.124(16) 0.031(12) 0.036(10) 0.042(10) C31 0.054(8) 0.050(7) 0.061(8) -0.002(6) -0.017(7) 0.006(6) C32 0.121(17) 0.098(14) 0.076(12) -0.016(10) -0.025(12) -0.008(12) C33 0.045(10) 0.109(16) 0.184(25) 0.000(15) -0.022(12) 0.011(10) C34 0.065(14) 0.029(9) 0.066(13) 0.001(8) 0.024(11) 0.006(9) C35 0.114(24) 0.069(18) 0.116(25) -0.016(16) 0.015(22) 0.006(16) C36 0.107(24) 0.036(12) 0.099(22) 0.026(11) -0.029(15) 0.023(11) C37 0.066(12) 0.076(13) 0.045(10) 0.016(9) 0.012(9) 0.021(10) C38 0.118(22) 0.080(19) 0.141(25) 0.068(20) 0.081(20) 0.045(17) C39 0.104(20) 0.080(16) 0.118(22) 0.035(16) 0.050(17) 0.030(15) C40 0.038(11) 0.071(15) 0.048(12) -0.007(10) 0.005(9) -0.001(11) C41 0.053(14) 0.088(21) 0.069(17) 0.001(14) -0.013(12) 0.026(15) C42 0.102(26) 0.148(37) 0.049(17) -0.053(19) 0.005(15) 0.022(21) _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 Sr O4 2.478(8) . ? Sr O1 2.519(8) . ? Sr O2 2.531(7) . ? Sr O6 2.535(9) . ? Sr O3 2.539(8) . ? Sr O5 2.554(8) . ? Ta1 O7 1.886(8) . ? Ta1 O8 1.889(8) . ? Ta1 O9 1.898(8) . ? Ta1 O10 2.014(8) . ? Ta1 O2 2.017(7) . ? Ta1 O1 2.046(6) . ? Ta2 O12 1.913(7) . ? Ta2 O14 1.915(7) . ? Ta2 O13 1.915(8) . ? Ta2 O3 2.009(8) . ? Ta2 O11 2.017(7) . ? Ta2 O4 2.027(7) . ? O1 C1 1.40(2) . ? O2 C4 1.43(2) . ? O3 C7 1.44(2) . ? O4 C10 1.417(14) . ? O5 C13 1.41(2) . ? O5 C13' 1.42(2) . ? O6 C16 1.47(2) . ? O7 C19 1.41(2) . ? O8 C22 1.38(2) . ? O9 C25' 1.39(2) . ? O9 C25 1.40(2) . ? O10 C28 1.40(2) . ? O11 C31 1.43(2) . ? O12 C34' 1.40(2) . ? O12 C34 1.411(15) . ? O13 C37' 1.38(2) . ? O13 C37 1.405(14) . ? O14 C40 1.365(15) . ? O14 C40' 1.37(2) . ? C1 C2 1.47(2) . ? C1 C3 1.50(2) . ? C4 C5 1.45(2) . ? C4 C6 1.53(3) . ? C7 C8 1.39(3) . ? C7 C9 1.48(2) . ? C10 C11 1.50(2) . ? C10 C12 1.50(2) . ? C13 C15 1.43(2) . ? C13 C14 1.44(2) . ? C13' C15' 1.47(2) . ? C13' C14' 1.47(2) . ? C16 C18 1.40(3) . ? C16 C17 1.43(3) . ? C19 C20 1.49(3) . ? C19 C21 1.50(3) . ? C22 C24 1.46(2) . ? C22 C23 1.49(2) . ? C25 C26 1.45(2) . ? C25 C27 1.45(2) . ? C25' C26' 1.44(2) . ? C25' C27' 1.45(2) . ? C28 C30 1.48(2) . ? C28 C29 1.49(2) . ? C31 C32 1.50(2) . ? C31 C33 1.51(2) . ? C34 C35 1.46(2) . ? C34 C36 1.47(2) . ? C34' C35' 1.45(2) . ? C34' C36' 1.45(2) . ? C37 C39 1.45(2) . ? C37 C38 1.46(2) . ? C37' C38' 1.45(2) . ? C37' C39' 1.45(2) . ? C40 C41 1.46(2) . ? C40 C42 1.46(2) . ? C40' C41' 1.44(2) . ? C40' C42' 1.44(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Sr O1 108.2(2) . . ? O4 Sr O2 111.3(2) . . ? O1 Sr O2 62.1(2) . . ? O4 Sr O6 79.4(3) . . ? O1 Sr O6 164.7(2) . . ? O2 Sr O6 103.0(3) . . ? O4 Sr O3 61.3(2) . . ? O1 Sr O3 117.3(2) . . ? O2 Sr O3 172.4(2) . . ? O6 Sr O3 78.0(3) . . ? O4 Sr O5 169.1(3) . . ? O1 Sr O5 80.8(3) . . ? O2 Sr O5 78.1(3) . . ? O6 Sr O5 93.4(3) . . ? O3 Sr O5 109.4(3) . . ? O7 Ta1 O8 93.2(4) . . ? O7 Ta1 O9 93.2(4) . . ? O8 Ta1 O9 95.1(4) . . ? O7 Ta1 O10 177.7(4) . . ? O8 Ta1 O10 87.1(4) . . ? O9 Ta1 O10 89.0(4) . . ? O7 Ta1 O2 91.3(4) . . ? O8 Ta1 O2 170.5(3) . . ? O9 Ta1 O2 93.0(3) . . ? O10 Ta1 O2 88.1(3) . . ? O7 Ta1 O1 92.6(3) . . ? O8 Ta1 O1 91.8(3) . . ? O9 Ta1 O1 170.8(3) . . ? O10 Ta1 O1 85.1(3) . . ? O2 Ta1 O1 79.7(3) . . ? O12 Ta2 O14 91.6(4) . . ? O12 Ta2 O13 95.2(4) . . ? O14 Ta2 O13 91.6(4) . . ? O12 Ta2 O3 93.9(4) . . ? O14 Ta2 O3 92.0(4) . . ? O13 Ta2 O3 170.1(3) . . ? O12 Ta2 O11 90.1(3) . . ? O14 Ta2 O11 178.2(4) . . ? O13 Ta2 O11 88.6(4) . . ? O3 Ta2 O11 87.5(3) . . ? O12 Ta2 O4 172.3(4) . . ? O14 Ta2 O4 90.7(4) . . ? O13 Ta2 O4 92.0(3) . . ? O3 Ta2 O4 78.7(3) . . ? O11 Ta2 O4 87.5(3) . . ? C1 O1 Ta1 127.5(7) . . ? C1 O1 Sr 120.1(7) . . ? Ta1 O1 Sr 108.3(3) . . ? C4 O2 Ta1 138.0(8) . . ? C4 O2 Sr 112.8(8) . . ? Ta1 O2 Sr 108.8(3) . . ? C7 O3 Ta2 133.4(11) . . ? C7 O3 Sr 116.3(10) . . ? Ta2 O3 Sr 108.7(3) . . ? C10 O4 Ta2 126.2(7) . . ? C10 O4 Sr 123.4(7) . . ? Ta2 O4 Sr 110.4(3) . . ? C13 O5 Sr 134.1(14) . . ? C13' O5 Sr 154.4(13) . . ? C16 O6 Sr 138.9(12) . . ? C19 O7 Ta1 152.8(11) . . ? C22 O8 Ta1 156.4(11) . . ? C25' O9 Ta1 171.5(12) . . ? C25 O9 Ta1 146.0(12) . . ? C28 O10 Ta1 127.4(8) . . ? C31 O11 Ta2 123.5(8) . . ? C34' O12 Ta2 162.8(16) . . ? C34 O12 Ta2 149.2(10) . . ? C37' O13 Ta2 151.1(22) . . ? C37 O13 Ta2 147.7(10) . . ? C40 O14 Ta2 151.3(12) . . ? C40' O14 Ta2 164.6(17) . . ? O1 C1 C2 111.2(11) . . ? O1 C1 C3 109.8(13) . . ? C2 C1 C3 115.0(13) . . ? O2 C4 C5 112.2(14) . . ? O2 C4 C6 109.1(13) . . ? C5 C4 C6 116.0(16) . . ? C8 C7 O3 116.3(16) . . ? C8 C7 C9 118.4(17) . . ? O3 C7 C9 113.8(14) . . ? O4 C10 C11 109.5(12) . . ? O4 C10 C12 109.4(11) . . ? C11 C10 C12 111.7(14) . . ? O5 C13 C15 110.3(18) . . ? O5 C13 C14 112.0(18) . . ? C15 C13 C14 114.2(22) . . ? O5 C13' C15' 106.5(21) . . ? O5 C13' C14' 105.4(21) . . ? C15' C13' C14' 105.6(22) . . ? C18 C16 C17 117.4(22) . . ? C18 C16 O6 111.5(16) . . ? C17 C16 O6 111.9(16) . . ? O7 C19 C20 109.5(16) . . ? O7 C19 C21 109.4(17) . . ? C20 C19 C21 111.2(18) . . ? O8 C22 C24 114.9(15) . . ? O8 C22 C23 114.0(14) . . ? C24 C22 C23 113.5(16) . . ? O9 C25 C26 115.9(19) . . ? O9 C25 C27 109.0(18) . . ? C26 C25 C27 110.9(20) . . ? O9 C25' C26' 112.2(21) . . ? O9 C25' C27' 110.0(21) . . ? C26' C25' C27' 111.8(22) . . ? O10 C28 C30 110.5(12) . . ? O10 C28 C29 111.9(13) . . ? C30 C28 C29 112.5(15) . . ? O11 C31 C32 111.0(14) . . ? O11 C31 C33 109.3(12) . . ? C32 C31 C33 110.9(16) . . ? O12 C34 C35 108.6(17) . . ? O12 C34 C36 108.8(16) . . ? C35 C34 C36 109.9(20) . . ? O12 C34' C35' 108.6(23) . . ? O12 C34' C36' 109.1(25) . . ? C35' C34' C36' 109.7(25) . . ? O13 C37 C39 112.7(15) . . ? O13 C37 C38 110.1(14) . . ? C39 C37 C38 113.0(16) . . ? O13 C37' C38' 110.8(26) . . ? O13 C37' C39' 110.4(26) . . ? C38' C37' C39' 109.7(25) . . ? O14 C40 C41 112.0(17) . . ? O14 C40 C42 111.0(18) . . ? C41 C40 C42 110.5(20) . . ? O14 C40' C41' 112.7(25) . . ? O14 C40' C42' 111.6(25) . . ? C41' C40' C42' 111.9(25) . . ? _refine_diff_density_max 1.135 _refine_diff_density_min -1.254 _refine_diff_density_rms 0.141 data_t3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H72 Mg Nb2 O14' _chemical_formula_weight 843.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0020 0.0020 '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' 0.0080 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mg' 'Mg' 0.0420 0.0360 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nb' 'Nb' -2.1970 0.6210 '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 8.956(3) _cell_length_b 11.370(3) _cell_length_c 11.630(5) _cell_angle_alpha 95.79(4) _cell_angle_beta 110.06(4) _cell_angle_gamma 94.27(4) _cell_volume 1099.2(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.274 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 446 _exptl_absorpt_coefficient_mu 0.511 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _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 6878 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 24.01 _reflns_number_total 3199 _reflns_number_gt 2675 _reflns_threshold_expression >2sigma(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 w=1/[\s^2^(Fo^2^)+(0.0877P)^2^+0.3501P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3199 _refine_ls_number_parameters 323 _refine_ls_number_restraints 576 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1366 _refine_ls_wR_factor_gt 0.1313 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.080 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.58215(6) 0.72345(3) 0.72103(4) 0.0580(2) Uani 1 d . . . Mg1 Mg 0.5000 0.5000 0.5000 0.0428(4) Uani 1 d S . . O1 O 0.6719(5) 0.6048(3) 0.4585(4) 0.0785(11) Uani 1 d . . . H1 H 0.714(9) 0.694(7) 0.530(7) 0.13(2) Uiso 1 d . . . C11 C 0.7748(8) 0.5860(5) 0.3929(6) 0.0799(16) Uani 1 d U . . H11A H 0.7580 0.5026 0.3588 0.096 Uiso 1 calc R . . H11B H 0.8844 0.6031 0.4500 0.096 Uiso 1 calc R . . C12 C 0.7540(12) 0.6566(9) 0.2944(7) 0.132(3) Uani 1 d U . . H12A H 0.8284 0.6391 0.2539 0.197 Uiso 1 calc R . . H12B H 0.7730 0.7395 0.3274 0.197 Uiso 1 calc R . . H12C H 0.6467 0.6387 0.2360 0.197 Uiso 1 calc R . . O2 O 0.4255(4) 0.6595(2) 0.5458(3) 0.0573(7) Uani 1 d D . . C21 C 0.3874(12) 0.7392(8) 0.4527(9) 0.065(3) Uani 0.519(10) d PDU A 1 H21A H 0.3834 0.6990 0.3739 0.078 Uiso 0.519(10) calc PR A 1 H21B H 0.4673 0.8083 0.4769 0.078 Uiso 0.519(10) calc PR A 1 C22 C 0.2238(19) 0.776(2) 0.444(2) 0.078(4) Uani 0.519(10) d PDU A 1 H22A H 0.1922 0.8293 0.3824 0.117 Uiso 0.519(10) calc PR A 1 H22B H 0.2300 0.8162 0.5222 0.117 Uiso 0.519(10) calc PR A 1 H22C H 0.1465 0.7071 0.4205 0.117 Uiso 0.519(10) calc PR A 1 O3 O 0.6360(4) 0.5557(3) 0.6832(3) 0.0561(7) Uani 1 d D . . C31 C 0.6921(14) 0.4821(10) 0.7808(10) 0.078(3) Uani 0.507(10) d PDU B 1 H31A H 0.6443 0.4004 0.7511 0.094 Uiso 0.507(10) calc PR B 1 H31B H 0.6618 0.5103 0.8503 0.094 Uiso 0.507(10) calc PR B 1 C32 C 0.8723(17) 0.489(2) 0.821(2) 0.094(5) Uani 0.507(10) d PDU B 1 H32A H 0.9113 0.4399 0.8848 0.141 Uiso 0.507(10) calc PR B 1 H32B H 0.9187 0.5697 0.8511 0.141 Uiso 0.507(10) calc PR B 1 H32C H 0.9013 0.4609 0.7514 0.141 Uiso 0.507(10) calc PR B 1 O4 O 0.7352(4) 0.7833(3) 0.6437(3) 0.0683(9) Uani 1 d D . . C41 C 0.877(2) 0.8651(15) 0.6997(12) 0.092(4) Uani 0.57(2) d PDU C 1 H41A H 0.9599 0.8270 0.7564 0.110 Uiso 0.57(2) calc PR C 1 H41B H 0.8555 0.9334 0.7460 0.110 Uiso 0.57(2) calc PR C 1 C42 C 0.933(2) 0.9047(15) 0.6006(15) 0.081(4) Uani 0.57(2) d PDU C 1 H42A H 1.0264 0.9620 0.6374 0.121 Uiso 0.57(2) calc PR C 1 H42B H 0.8498 0.9402 0.5434 0.121 Uiso 0.57(2) calc PR C 1 H42C H 0.9593 0.8373 0.5577 0.121 Uiso 0.57(2) calc PR C 1 O5 O 0.4385(6) 0.6707(4) 0.7986(4) 0.0887(12) Uani 1 d D . . C51 C 0.320(2) 0.7131(15) 0.8431(16) 0.126(4) Uani 0.570(13) d PDU D 1 H51A H 0.2162 0.6988 0.7779 0.152 Uiso 0.570(13) calc PR D 1 H51B H 0.3454 0.7980 0.8705 0.152 Uiso 0.570(13) calc PR D 1 C52 C 0.319(3) 0.6490(19) 0.9476(17) 0.142(5) Uani 0.570(13) d PDU D 1 H52A H 0.2355 0.6728 0.9758 0.213 Uiso 0.570(13) calc PR D 1 H52B H 0.4204 0.6679 1.0139 0.213 Uiso 0.570(13) calc PR D 1 H52C H 0.3005 0.5648 0.9209 0.213 Uiso 0.570(13) calc PR D 1 O6 O 0.7544(5) 0.7540(3) 0.8744(3) 0.0837(11) Uani 1 d D . . C61 C 0.780(2) 0.7589(16) 1.0013(10) 0.102(4) Uani 0.494(17) d PDU E 1 H61A H 0.7921 0.6801 1.0258 0.122 Uiso 0.494(17) calc PR E 1 H61B H 0.6882 0.7865 1.0177 0.122 Uiso 0.494(17) calc PR E 1 C62 C 0.927(2) 0.842(2) 1.0739(16) 0.119(5) Uani 0.494(17) d PDU E 1 H62A H 0.9459 0.8440 1.1605 0.179 Uiso 0.494(17) calc PR E 1 H62B H 0.9130 0.9203 1.0512 0.179 Uiso 0.494(17) calc PR E 1 H62C H 1.0171 0.8147 1.0566 0.179 Uiso 0.494(17) calc PR E 1 O7 O 0.5047(5) 0.8734(3) 0.7185(4) 0.0808(11) Uani 1 d D . . C71 C 0.510(2) 0.9898(9) 0.6916(13) 0.104(4) Uani 0.58(2) d PDU F 1 H71A H 0.4182 0.9981 0.6200 0.124 Uiso 0.58(2) calc PR F 1 H71B H 0.6065 1.0103 0.6735 0.124 Uiso 0.58(2) calc PR F 1 C72 C 0.511(3) 1.0708(17) 0.802(2) 0.142(6) Uani 0.58(2) d PDU F 1 H72A H 0.5164 1.1519 0.7862 0.214 Uiso 0.58(2) calc PR F 1 H72B H 0.6023 1.0615 0.8728 0.214 Uiso 0.58(2) calc PR F 1 H72C H 0.4148 1.0508 0.8186 0.214 Uiso 0.58(2) calc PR F 1 C21' C 0.2594(12) 0.6906(9) 0.5032(11) 0.067(3) Uani 0.481(10) d PDU A 2 H21C H 0.2311 0.7207 0.5731 0.080 Uiso 0.481(10) calc PR A 2 H21D H 0.1850 0.6210 0.4584 0.080 Uiso 0.481(10) calc PR A 2 C22' C 0.253(3) 0.786(2) 0.419(2) 0.083(5) Uani 0.481(10) d PDU A 2 H22D H 0.1469 0.8087 0.3892 0.125 Uiso 0.481(10) calc PR A 2 H22E H 0.2813 0.7550 0.3502 0.125 Uiso 0.481(10) calc PR A 2 H22F H 0.3273 0.8541 0.4644 0.125 Uiso 0.481(10) calc PR A 2 C31' C 0.8010(13) 0.5322(11) 0.7229(11) 0.086(3) Uani 0.493(10) d PDU B 2 H31C H 0.8721 0.6059 0.7433 0.103 Uiso 0.493(10) calc PR B 2 H31D H 0.8207 0.4819 0.6583 0.103 Uiso 0.493(10) calc PR B 2 C32' C 0.827(2) 0.469(2) 0.836(2) 0.103(6) Uani 0.493(10) d PDU B 2 H32D H 0.9355 0.4501 0.8664 0.154 Uiso 0.493(10) calc PR B 2 H32E H 0.7547 0.3974 0.8150 0.154 Uiso 0.493(10) calc PR B 2 H32F H 0.8085 0.5205 0.8996 0.154 Uiso 0.493(10) calc PR B 2 C41' C 0.817(2) 0.8965(11) 0.656(2) 0.083(4) Uani 0.43(2) d PDU C 2 H41C H 0.8349 0.9390 0.7367 0.099 Uiso 0.43(2) calc PR C 2 H41D H 0.7526 0.9414 0.5942 0.099 Uiso 0.43(2) calc PR C 2 C42' C 0.974(2) 0.886(2) 0.639(3) 0.094(6) Uani 0.43(2) d PDU C 2 H42D H 1.0295 0.9646 0.6491 0.141 Uiso 0.43(2) calc PR C 2 H42E H 0.9566 0.8465 0.5581 0.141 Uiso 0.43(2) calc PR C 2 H42F H 1.0381 0.8419 0.7001 0.141 Uiso 0.43(2) calc PR C 2 C51' C 0.417(2) 0.674(2) 0.9135(15) 0.130(5) Uani 0.430(13) d PDU D 2 H51C H 0.4918 0.7362 0.9732 0.156 Uiso 0.430(13) calc PR D 2 H51D H 0.4344 0.5987 0.9448 0.156 Uiso 0.430(13) calc PR D 2 C52' C 0.250(3) 0.699(3) 0.894(3) 0.146(6) Uani 0.430(13) d PDU D 2 H52D H 0.2316 0.7011 0.9706 0.218 Uiso 0.430(13) calc PR D 2 H52E H 0.1768 0.6380 0.8341 0.218 Uiso 0.430(13) calc PR D 2 H52F H 0.2345 0.7749 0.8644 0.218 Uiso 0.430(13) calc PR D 2 C61' C 0.867(3) 0.7650(19) 0.9958(13) 0.129(5) Uani 0.506(17) d PDU E 2 H61C H 0.9748 0.7732 0.9951 0.155 Uiso 0.506(17) calc PR E 2 H61D H 0.8520 0.6954 1.0344 0.155 Uiso 0.506(17) calc PR E 2 C62' C 0.837(3) 0.8766(14) 1.0664(16) 0.116(5) Uani 0.506(17) d PDU E 2 H62D H 0.9061 0.8850 1.1513 0.174 Uiso 0.506(17) calc PR E 2 H62E H 0.7272 0.8693 1.0618 0.174 Uiso 0.506(17) calc PR E 2 H62F H 0.8580 0.9453 1.0303 0.174 Uiso 0.506(17) calc PR E 2 C71' C 0.446(2) 0.9834(14) 0.725(3) 0.126(5) Uani 0.42(2) d PDU F 2 H71C H 0.3614 0.9785 0.7595 0.151 Uiso 0.42(2) calc PR F 2 H71D H 0.4037 1.0077 0.6438 0.151 Uiso 0.42(2) calc PR F 2 C72' C 0.587(3) 1.0723(18) 0.809(3) 0.113(5) Uani 0.42(2) d PDU F 2 H72D H 0.5565 1.1514 0.8073 0.170 Uiso 0.42(2) calc PR F 2 H72E H 0.6759 1.0676 0.7813 0.170 Uiso 0.42(2) calc PR F 2 H72F H 0.6180 1.0537 0.8925 0.170 Uiso 0.42(2) calc PR F 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 0.0732(3) 0.0470(3) 0.0500(3) -0.00712(17) 0.0224(2) -0.00104(19) Mg1 0.0504(11) 0.0383(9) 0.0409(10) 0.0020(7) 0.0199(9) -0.0024(8) O1 0.096(3) 0.067(2) 0.083(2) -0.0130(18) 0.059(2) -0.0263(19) C11 0.084(4) 0.077(3) 0.085(4) -0.001(3) 0.047(3) -0.011(3) C12 0.165(7) 0.150(7) 0.091(5) 0.020(4) 0.067(5) -0.021(6) O2 0.064(2) 0.0427(15) 0.0554(18) 0.0002(13) 0.0102(16) 0.0107(13) C21 0.069(5) 0.051(4) 0.073(5) 0.011(4) 0.020(4) 0.009(4) C22 0.067(7) 0.073(7) 0.090(8) 0.009(6) 0.022(6) 0.021(6) O3 0.0590(19) 0.0494(16) 0.0480(17) 0.0001(13) 0.0056(16) 0.0068(13) C31 0.089(6) 0.074(5) 0.059(5) 0.010(4) 0.008(5) 0.016(5) C32 0.094(9) 0.089(8) 0.082(7) 0.003(6) 0.011(7) 0.017(7) O4 0.078(2) 0.0564(18) 0.068(2) -0.0030(15) 0.0291(19) -0.0118(16) C41 0.090(7) 0.090(6) 0.088(6) 0.011(5) 0.027(5) -0.013(5) C42 0.077(7) 0.074(6) 0.095(8) 0.013(6) 0.035(7) -0.002(5) O5 0.115(3) 0.085(3) 0.078(3) -0.006(2) 0.057(3) -0.003(2) C51 0.134(7) 0.156(8) 0.125(7) 0.020(6) 0.089(6) 0.025(6) C52 0.145(10) 0.176(10) 0.133(9) 0.022(8) 0.085(8) 0.007(8) O6 0.105(3) 0.078(2) 0.0459(19) -0.0103(16) 0.008(2) -0.010(2) C61 0.109(7) 0.114(6) 0.076(5) -0.007(5) 0.037(5) -0.013(6) C62 0.114(10) 0.132(9) 0.077(7) -0.022(7) 0.009(8) -0.023(8) O7 0.108(3) 0.0479(18) 0.086(3) -0.0119(17) 0.039(2) 0.0114(18) C71 0.129(7) 0.071(5) 0.115(6) 0.002(5) 0.052(5) 0.009(5) C72 0.156(11) 0.094(7) 0.167(9) -0.037(7) 0.057(9) 0.025(8) C21' 0.065(5) 0.058(5) 0.076(5) 0.007(4) 0.021(4) 0.018(4) C22' 0.091(9) 0.066(7) 0.087(9) 0.026(6) 0.017(7) 0.022(7) C31' 0.090(6) 0.071(5) 0.076(5) 0.000(4) 0.006(5) 0.011(5) C32' 0.108(10) 0.093(8) 0.083(8) 0.016(6) 0.001(8) 0.011(8) C41' 0.087(7) 0.070(6) 0.092(7) 0.004(5) 0.034(6) 0.006(5) C42' 0.081(9) 0.093(9) 0.103(10) 0.011(8) 0.030(8) -0.006(8) C51' 0.132(8) 0.168(8) 0.119(8) 0.010(6) 0.084(6) 0.019(6) C52' 0.133(10) 0.184(11) 0.148(11) 0.023(9) 0.083(9) 0.031(9) C61' 0.126(8) 0.130(7) 0.108(6) -0.019(6) 0.024(6) 0.001(7) C62' 0.134(10) 0.113(8) 0.079(7) -0.028(6) 0.028(8) -0.018(8) C71' 0.134(8) 0.101(7) 0.135(8) -0.013(6) 0.047(6) 0.013(6) C72' 0.130(11) 0.075(7) 0.135(9) -0.022(7) 0.058(9) 0.002(8) _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 O7 1.887(4) . ? Nb1 O6 1.895(4) . ? Nb1 O5 1.903(4) . ? Nb1 O4 1.995(3) . ? Nb1 O3 2.044(3) . ? Nb1 O2 2.058(3) . ? Nb1 Mg1 3.2727(17) . ? Mg1 O2 2.061(3) . ? Mg1 O2 2.061(3) 2_666 ? Mg1 O3 2.063(3) 2_666 ? Mg1 O3 2.063(3) . ? Mg1 O1 2.092(3) . ? Mg1 O1 2.092(3) 2_666 ? Mg1 Nb1 3.2727(17) 2_666 ? O1 C11 1.398(6) . ? C11 C12 1.433(9) . ? O2 C21 1.450(9) . ? O2 C21' 1.480(9) . ? C21 C22 1.527(13) . ? O3 C31' 1.444(11) . ? O3 C31 1.451(10) . ? C31 C32 1.512(14) . ? O4 C41' 1.403(11) . ? O4 C41 1.429(10) . ? C41 C42 1.499(13) . ? O5 C51' 1.413(12) . ? O5 C51 1.420(11) . ? C51 C52 1.482(14) . ? O6 C61 1.409(11) . ? O6 C61' 1.411(13) . ? C61 C62 1.495(14) . ? O7 C71 1.393(10) . ? O7 C71' 1.397(13) . ? C71 C72 1.504(14) . ? C21' C22' 1.525(14) . ? C31' C32' 1.521(14) . ? C41' C42' 1.496(14) . ? C51' C52' 1.481(15) . ? C61' C62' 1.531(14) . ? C71' C72' 1.530(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Nb1 O6 99.25(19) . . ? O7 Nb1 O5 89.67(19) . . ? O6 Nb1 O5 91.51(19) . . ? O7 Nb1 O4 89.19(16) . . ? O6 Nb1 O4 87.29(17) . . ? O5 Nb1 O4 178.19(15) . . ? O7 Nb1 O3 167.33(15) . . ? O6 Nb1 O3 92.96(16) . . ? O5 Nb1 O3 93.42(16) . . ? O4 Nb1 O3 87.99(14) . . ? O7 Nb1 O2 93.20(16) . . ? O6 Nb1 O2 166.54(16) . . ? O5 Nb1 O2 93.67(17) . . ? O4 Nb1 O2 87.80(14) . . ? O3 Nb1 O2 74.35(13) . . ? O7 Nb1 Mg1 129.97(13) . . ? O6 Nb1 Mg1 129.38(14) . . ? O5 Nb1 Mg1 98.83(13) . . ? O4 Nb1 Mg1 82.98(10) . . ? O3 Nb1 Mg1 37.38(9) . . ? O2 Nb1 Mg1 37.42(8) . . ? O2 Mg1 O2 180.0 . 2_666 ? O2 Mg1 O3 106.11(13) . 2_666 ? O2 Mg1 O3 73.89(13) 2_666 2_666 ? O2 Mg1 O3 73.89(13) . . ? O2 Mg1 O3 106.11(13) 2_666 . ? O3 Mg1 O3 180.0 2_666 . ? O2 Mg1 O1 85.22(14) . . ? O2 Mg1 O1 94.78(14) 2_666 . ? O3 Mg1 O1 93.62(15) 2_666 . ? O3 Mg1 O1 86.38(15) . . ? O2 Mg1 O1 94.78(14) . 2_666 ? O2 Mg1 O1 85.22(14) 2_666 2_666 ? O3 Mg1 O1 86.38(15) 2_666 2_666 ? O3 Mg1 O1 93.62(15) . 2_666 ? O1 Mg1 O1 180.0 . 2_666 ? O2 Mg1 Nb1 142.64(9) . 2_666 ? O2 Mg1 Nb1 37.36(9) 2_666 2_666 ? O3 Mg1 Nb1 36.96(9) 2_666 2_666 ? O3 Mg1 Nb1 143.04(9) . 2_666 ? O1 Mg1 Nb1 99.60(10) . 2_666 ? O1 Mg1 Nb1 80.40(10) 2_666 2_666 ? O2 Mg1 Nb1 37.36(9) . . ? O2 Mg1 Nb1 142.64(9) 2_666 . ? O3 Mg1 Nb1 143.04(9) 2_666 . ? O3 Mg1 Nb1 36.96(9) . . ? O1 Mg1 Nb1 80.40(10) . . ? O1 Mg1 Nb1 99.60(10) 2_666 . ? Nb1 Mg1 Nb1 180.0 2_666 . ? C11 O1 Mg1 136.2(3) . . ? O1 C11 C12 114.2(6) . . ? C21 O2 C21' 63.8(6) . . ? C21 O2 Nb1 119.0(4) . . ? C21' O2 Nb1 120.7(5) . . ? C21 O2 Mg1 116.9(4) . . ? C21' O2 Mg1 126.6(5) . . ? Nb1 O2 Mg1 105.22(14) . . ? O2 C21 C22 105.9(9) . . ? C31' O3 C31 61.2(7) . . ? C31' O3 Nb1 119.7(5) . . ? C31 O3 Nb1 120.6(5) . . ? C31' O3 Mg1 116.4(5) . . ? C31 O3 Mg1 127.4(5) . . ? Nb1 O3 Mg1 105.66(14) . . ? O3 C31 C32 108.4(11) . . ? C41' O4 C41 30.5(8) . . ? C41' O4 Nb1 131.6(7) . . ? C41 O4 Nb1 128.1(5) . . ? O4 C41 C42 109.0(11) . . ? C51' O5 C51 46.5(9) . . ? C51' O5 Nb1 143.3(10) . . ? C51 O5 Nb1 140.3(7) . . ? O5 C51 C52 108.1(12) . . ? C61 O6 C61' 33.0(9) . . ? C61 O6 Nb1 138.8(8) . . ? C61' O6 Nb1 170.7(12) . . ? O6 C61 C62 109.3(12) . . ? C71 O7 C71' 33.5(11) . . ? C71 O7 Nb1 150.0(9) . . ? C71' O7 Nb1 175.6(15) . . ? O7 C71 C72 108.0(13) . . ? O2 C21' C22' 106.9(10) . . ? O3 C31' C32' 105.7(11) . . ? O4 C41' C42' 110.6(14) . . ? O5 C51' C52' 107.8(15) . . ? O6 C61' C62' 106.5(13) . . ? O7 C71' C72' 106.6(15) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O4 1.19(8) 1.53(8) 2.681(5) 159(6) . _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 24.01 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 0.855 _refine_diff_density_min -0.744 _refine_diff_density_rms 0.070