# 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 ? loop_ _publ_author_name C.J.Clark B.K.Nicholson C.E.Wright _publ_contact_author_name 'B Nicholson' _publ_contact_author_email B.NICHOLSON@WAIKATO.AC.NZ _database_code_depnum_ccdc_archive 'CCDC 702086' data_ccbm_squeeze _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H65 N12 Na2 O58 Sb12, C10 H16 N' _chemical_formula_sum 'C82 H81 N13 Na2 O58 Sb12' _chemical_formula_weight 3683.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 '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/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 30.6262(6) _cell_length_b 22.5295(4) _cell_length_c 25.1789(8) _cell_angle_alpha 90.00 _cell_angle_beta 122.5690(10) _cell_angle_gamma 90.00 _cell_volume 14641.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9041 _cell_measurement_theta_min 2 _cell_measurement_theta_max 54 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.671 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7048 _exptl_absorpt_coefficient_mu 2.262 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5406 _exptl_absorpt_correction_T_max 0.7424 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 APEX II CCD' _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 165946 _diffrn_reflns_av_R_equivalents 0.0830 _diffrn_reflns_av_sigmaI/netI 0.0528 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 27.00 _reflns_number_total 16399 _reflns_number_gt 11131 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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. The structure was solved by direct methods (SHELXS97) to give the positions of the Sb atoms, showing the anion was on the mirror plane of C2/m. A subsequent difference map showed all the anion O atoms and the two Na+ cations. With further cycles the aryl rings were located, but some were partially disordered. The two aryl rings that are bisected by the mirror plane were disordered so were refined as rigid hexag onswith isotropic U parameters. The other aryl rings were linked via the SAME constraints and with temperature factors constrained by the SIMU and DELU options of SHELXL97. The PhCH2NMe3 cation was found to be disordered over two symmetry equivalent sites, with 50% occupancy, and the phenyl ring was constrained to a rigid hexagon with the AFIX 66 instruction. The NMe3 group was partially disordered so was also treated isotropically without Hato ms added. Four H2O molecules coordinated to Na+ cations were well defined, so were included. In addition there were at least 15 lattice water molecules revealed in difference maps, some clearly having partial occupancy or loosely held positions. These could not be sensibly modelled so the data was treated using the SQUEEZE option of PLATON. Final refinement therefore excluded this diffuse lattice water, and calculations of density etc also ignore this contribution. The H atoms were included in calculated positions for the ordered rings of the cation and anion, but those of the disordered rings, the methyl groups and the water molecules were omitted. ; _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^)+(0.1077P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16399 _refine_ls_number_parameters 704 _refine_ls_number_restraints 627 _refine_ls_R_factor_all 0.0921 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.1917 _refine_ls_wR_factor_gt 0.1780 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.137 _refine_ls_shift/su_max 0.123 _refine_ls_shift/su_mean 0.013 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 Sb1 Sb 0.23317(3) 0.0000 0.39331(4) 0.0369(2) Uani 1 2 d S . . Sb2 Sb 0.23486(2) 0.13036(2) 0.30936(2) 0.03343(15) Uani 1 1 d . . . Sb3 Sb 0.30191(2) 0.14382(2) 0.22686(3) 0.03591(15) Uani 1 1 d . . . Sb4 Sb 0.29766(3) 0.0000 0.15760(3) 0.03256(19) Uani 1 2 d S . . Sb5 Sb 0.124979(19) 0.06964(2) 0.24266(2) 0.03096(15) Uani 1 1 d . . . Sb6 Sb 0.158221(19) 0.13862(2) 0.16186(2) 0.03141(15) Uani 1 1 d . . . Sb7 Sb 0.19188(2) 0.06939(2) 0.08137(2) 0.03061(14) Uani 1 1 d . . . Na1 Na 0.2617(2) 0.0000 0.2624(2) 0.0428(12) Uani 1 2 d S . . Na2 Na 0.07939(17) 0.0000 0.08329(19) 0.0352(10) Uani 1 2 d SD . . O1 O 0.2024(2) 0.0618(3) 0.4193(3) 0.0475(16) Uani 1 1 d . A . O2 O 0.26090(19) 0.0588(2) 0.3605(2) 0.0350(13) Uani 1 1 d . . . O3 O 0.2891(2) 0.1184(3) 0.2920(3) 0.0356(13) Uani 1 1 d . . . O4 O 0.2795(2) 0.2271(3) 0.2289(3) 0.0506(16) Uani 1 1 d . A . O5 O 0.3082(2) 0.1667(3) 0.1554(3) 0.0428(14) Uani 1 1 d . A . O6 O 0.3167(2) 0.0591(2) 0.2221(2) 0.0340(13) Uani 1 1 d . . . O7 O 0.18724(19) 0.0740(2) 0.2313(2) 0.0297(12) Uani 1 1 d . . . O8 O 0.22283(19) 0.1274(2) 0.1571(2) 0.0308(12) Uani 1 1 d . . . O9 O 0.1987(2) 0.1888(2) 0.2372(2) 0.0353(13) Uani 1 1 d . . . O10 O 0.1694(2) 0.1264(2) 0.3098(2) 0.0355(13) Uani 1 1 d . . . O11 O 0.09818(19) 0.1256(2) 0.1707(2) 0.0303(12) Uani 1 1 d . . . O12 O 0.0959(3) 0.0000 0.1858(3) 0.0300(17) Uani 1 2 d S . . O13 O 0.13406(19) 0.0789(2) 0.0947(2) 0.0309(12) Uani 1 1 d . . . O14 O 0.1588(3) 0.0000 0.0241(3) 0.0310(17) Uani 1 2 d S . . O15 O 0.2596(2) 0.0626(2) 0.0910(2) 0.0346(13) Uani 1 1 d . . . O16 O 0.1617(3) 0.0000 0.3048(3) 0.0319(17) Uani 1 2 d S . . O17 O 0.2224(3) 0.0000 0.1444(3) 0.0266(16) Uani 1 2 d S . . C11 C 0.3029(4) 0.0053(7) 0.4847(5) 0.041(3) Uiso 0.50 1 d PGU A -1 C12 C 0.3337(4) 0.0558(5) 0.5079(4) 0.029(3) Uiso 0.50 1 d PGU A -1 C13 C 0.3791(4) 0.0548(5) 0.5673(5) 0.020(3) Uiso 0.50 1 d PGU A -1 C14 C 0.3938(5) 0.0034(7) 0.6034(5) 0.093(6) Uiso 0.50 1 d PGU A -1 C13A C 0.3630(7) -0.0471(6) 0.5801(8) 0.187(18) Uiso 0.50 1 d PGU A -1 C12A C 0.3176(7) -0.0462(6) 0.5208(8) 0.205(19) Uiso 0.50 1 d PGU A -1 N1 N 0.4393(10) 0.0000 0.6761(12) 0.151(8) Uiso 1 2 d SU A -1 O1A O 0.4650(5) 0.0502(6) 0.6862(6) 0.139(4) Uiso 1 1 d U A -1 C21 C 0.2731(3) 0.1939(3) 0.3824(4) 0.0356(18) Uani 1 1 d DU A . C22 C 0.2702(3) 0.1913(4) 0.4345(4) 0.045(2) Uani 1 1 d DU . . H22 H 0.2498 0.1612 0.4373 0.054 Uiso 1 1 calc R A . C23 C 0.2966(3) 0.2319(4) 0.4841(4) 0.052(2) Uani 1 1 d DU A . H23 H 0.2935 0.2305 0.5197 0.062 Uiso 1 1 calc R . . C24 C 0.3261(3) 0.2726(4) 0.4797(4) 0.048(2) Uani 1 1 d DU . . C25 C 0.3303(4) 0.2767(5) 0.4302(5) 0.063(3) Uani 1 1 d DU A . H25 H 0.3522 0.3059 0.4291 0.075 Uiso 1 1 calc R . . C26 C 0.3026(4) 0.2377(5) 0.3795(5) 0.060(3) Uani 1 1 d DU . . H26 H 0.3042 0.2418 0.3430 0.072 Uiso 1 1 calc R A . N2 N 0.3541(3) 0.3165(4) 0.5317(4) 0.067(2) Uani 1 1 d DU A . O2A O 0.3506(3) 0.3110(4) 0.5773(4) 0.080(2) Uani 1 1 d DU . . O2B O 0.3793(4) 0.3559(4) 0.5269(4) 0.114(4) Uani 1 1 d DU . . C31 C 0.3814(3) 0.1644(5) 0.2943(4) 0.049(2) Uani 1 1 d DU A . C32 C 0.4005(4) 0.1717(7) 0.3563(4) 0.084(4) Uani 1 1 d DU . . H32 H 0.3784 0.1654 0.3714 0.100 Uiso 1 1 calc R A . C33 C 0.4524(4) 0.1883(8) 0.3992(5) 0.109(5) Uani 1 1 d DU A . H33 H 0.4656 0.1929 0.4429 0.131 Uiso 1 1 calc R . . C34 C 0.4824(4) 0.1974(9) 0.3765(5) 0.112(5) Uani 1 1 d DU . . C35 C 0.4661(5) 0.1898(11) 0.3172(5) 0.156(7) Uani 1 1 d DU A . H35 H 0.4883 0.1968 0.3023 0.187 Uiso 1 1 calc R . . C36 C 0.4146(5) 0.1709(10) 0.2760(6) 0.138(6) Uani 1 1 d DU . . H36 H 0.4032 0.1624 0.2334 0.166 Uiso 1 1 calc R A . N3 N 0.5390(5) 0.2071(9) 0.4219(7) 0.164(7) Uiso 1 1 d DU A . O3A O 0.5528(6) 0.2200(8) 0.4764(7) 0.201(7) Uiso 1 1 d DU . . O3B O 0.5686(4) 0.2059(5) 0.4033(5) 0.124(4) Uiso 1 1 d DU . . C41 C 0.36580(15) -0.0009(3) 0.15656(19) 0.039(3) Uiso 1 2 d SGU A -1 C42 C 0.3874(3) 0.0493(3) 0.1474(4) 0.039(4) Uiso 0.50 1 d PGU A -1 C43 C 0.4335(3) 0.0448(3) 0.1493(4) 0.048(5) Uiso 0.50 1 d PGU A -1 C44 C 0.45793(16) -0.0098(3) 0.1603(2) 0.025(3) Uiso 0.50 1 d PGU A -1 C43A C 0.4363(3) -0.0600(3) 0.1694(4) 0.045(4) Uiso 0.50 1 d PGU A -1 C42A C 0.3903(3) -0.0556(3) 0.1675(4) 0.054(5) Uiso 0.50 1 d PGU A -1 N4 N 0.50685(19) 0.0000(3) 0.1645(3) 0.064(3) Uiso 1 2 d SGU . . O4A O 0.52643(19) -0.0477(3) 0.1662(3) 0.099(3) Uiso 1 1 d GU A . C51 C 0.0617(2) 0.0792(4) 0.2541(3) 0.049(2) Uani 1 1 d GDU . . C52 C 0.01182(19) 0.0728(5) 0.2056(3) 0.099(5) Uani 1 1 d GDU A . H52 H 0.0054 0.0652 0.1649 0.119 Uiso 1 1 calc R . . C53 C -0.0299(4) 0.0767(8) 0.2117(5) 0.105(5) Uani 1 1 d DU . . H53 H -0.0644 0.0732 0.1763 0.126 Uiso 1 1 calc R A . C54 C -0.0202(4) 0.0855(14) 0.2689(6) 0.209(8) Uani 1 1 d DU A . C55 C 0.0276(5) 0.0946(16) 0.3194(7) 0.233(10) Uani 1 1 d DU . . H55 H 0.0333 0.1039 0.3595 0.279 Uiso 1 1 calc R A . C56 C 0.0692(5) 0.0897(12) 0.3102(5) 0.159(7) Uani 1 1 d DU A . H56 H 0.1036 0.0941 0.3454 0.191 Uiso 1 1 calc R . . N5 N -0.0650(5) 0.0986(14) 0.2750(9) 0.313(11) Uani 1 1 d DU . . O5A O -0.0582(7) 0.1353(13) 0.3162(9) 0.334(15) Uani 1 1 d DU A . O5B O -0.1084(5) 0.0855(14) 0.2278(7) 0.347(15) Uani 1 1 d DU A . C61 C 0.1246(3) 0.2120(3) 0.1000(4) 0.043(2) Uani 1 1 d DU . . C62 C 0.0800(4) 0.2052(4) 0.0418(5) 0.079(4) Uani 1 1 d DU A . H62 H 0.0652 0.1668 0.0286 0.095 Uiso 1 1 calc R . . C63 C 0.0559(5) 0.2535(5) 0.0014(6) 0.108(5) Uani 1 1 d DU . . H63 H 0.0231 0.2494 -0.0367 0.130 Uiso 1 1 calc R A . C64 C 0.0810(4) 0.3066(4) 0.0185(5) 0.066(3) Uani 1 1 d DU A . C65 C 0.1251(5) 0.3146(5) 0.0726(5) 0.097(5) Uani 1 1 d DU . . H65 H 0.1407 0.3528 0.0841 0.117 Uiso 1 1 calc R A . C66 C 0.1491(5) 0.2658(4) 0.1132(5) 0.086(4) Uani 1 1 d DU A . H66 H 0.1826 0.2703 0.1502 0.103 Uiso 1 1 calc R . . N6 N 0.0577(5) 0.3571(5) -0.0255(6) 0.103(4) Uani 1 1 d DU . . O6A O 0.0809(5) 0.4035(4) -0.0138(5) 0.130(4) Uani 1 1 d DU A . O6B O 0.0151(5) 0.3459(6) -0.0745(7) 0.213(9) Uani 1 1 d DU A . C71 C 0.1638(3) 0.1359(3) 0.0110(4) 0.0369(19) Uani 1 1 d DU . . C72 C 0.1205(4) 0.1288(5) -0.0469(5) 0.074(4) Uani 1 1 d DU A . H72 H 0.1040 0.0911 -0.0584 0.089 Uiso 1 1 calc R . . C73 C 0.0996(4) 0.1750(5) -0.0898(5) 0.083(4) Uani 1 1 d DU . . H73 H 0.0691 0.1690 -0.1302 0.099 Uiso 1 1 calc R A . C74 C 0.1224(4) 0.2276(4) -0.0742(4) 0.054(2) Uani 1 1 d DU A . C75 C 0.1681(4) 0.2347(5) -0.0207(5) 0.079(4) Uani 1 1 d DU . . H75 H 0.1860 0.2713 -0.0121 0.094 Uiso 1 1 calc R A . C76 C 0.1896(4) 0.1883(4) 0.0229(5) 0.072(3) Uani 1 1 d DU A . H76 H 0.2224 0.1934 0.0610 0.087 Uiso 1 1 calc R . . N7 N 0.0981(4) 0.2793(4) -0.1168(5) 0.075(3) Uani 1 1 d DU . . O7A O 0.1180(4) 0.3270(4) -0.0991(5) 0.129(4) Uani 1 1 d DU A . O7B O 0.0608(3) 0.2668(5) -0.1702(4) 0.125(4) Uani 1 1 d DU A . N8 N 0.0960(4) 0.2920(5) 0.2565(5) 0.021(2) Uiso 0.50 1 d PDU . . C81 C 0.0722(7) 0.3388(9) 0.2730(9) 0.050(5) Uiso 0.50 1 d PU . . C82 C 0.0997(11) 0.3142(13) 0.2077(14) 0.092(8) Uiso 0.50 1 d PU . . C83 C 0.0625(9) 0.2389(10) 0.2311(12) 0.083(7) Uiso 0.50 1 d PDU . . C84 C 0.1508(9) 0.2791(10) 0.3038(14) 0.094(8) Uani 0.50 1 d PU . . H84A H 0.1626 0.2492 0.2854 0.113 Uiso 0.50 1 calc PR . . H84B H 0.1523 0.2600 0.3402 0.113 Uiso 0.50 1 calc PR . . C85 C 0.1893(5) 0.3281(6) 0.3289(7) 0.071(5) Uani 0.50 1 d PGU . . C86 C 0.2014(5) 0.3544(6) 0.3852(7) 0.065(5) Uani 0.50 1 d PGU . . H86 H 0.1837 0.3425 0.4049 0.078 Uiso 0.50 1 calc PR . . C87 C 0.2394(6) 0.3980(6) 0.4127(6) 0.075(6) Uani 0.50 1 d PGU . . H87 H 0.2476 0.4159 0.4512 0.090 Uiso 0.50 1 calc PR . . C88 C 0.2653(5) 0.4154(6) 0.3838(8) 0.101(7) Uani 0.50 1 d PGU . . H88 H 0.2913 0.4452 0.4026 0.122 Uiso 0.50 1 calc PR . . C89 C 0.2532(6) 0.3891(8) 0.3275(8) 0.091(6) Uani 0.50 1 d PGU . . H89 H 0.2709 0.4010 0.3078 0.109 Uiso 0.50 1 calc PR . . C810 C 0.2152(6) 0.3455(7) 0.3000(6) 0.080(6) Uani 0.50 1 d PGU . . H810 H 0.2069 0.3276 0.2615 0.096 Uiso 0.50 1 calc PR . . OW1 O 0.3513(6) 0.0000 0.3719(8) 0.120 Uiso 1 2 d S . . OW2 O 0.0140(2) 0.0844(3) 0.0606(3) 0.0470(15) Uiso 1 1 d . . . OW3 O 0.0542(4) 0.0000 -0.0386(4) 0.063(3) Uiso 1 2 d SD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sb1 0.0225(4) 0.0547(5) 0.0207(4) 0.000 0.0031(3) 0.000 Sb2 0.0233(3) 0.0404(3) 0.0248(3) -0.0070(2) 0.0051(2) -0.0034(2) Sb3 0.0277(3) 0.0408(3) 0.0285(3) -0.0062(2) 0.0081(2) -0.0083(2) Sb4 0.0261(4) 0.0380(4) 0.0235(4) 0.000 0.0066(3) 0.000 Sb5 0.0205(3) 0.0356(3) 0.0237(3) -0.0024(2) 0.0033(2) 0.0002(2) Sb6 0.0254(3) 0.0298(3) 0.0249(3) -0.0015(2) 0.0042(2) -0.0005(2) Sb7 0.0264(3) 0.0306(3) 0.0217(3) 0.0005(2) 0.0043(2) -0.0008(2) Na1 0.059(3) 0.038(2) 0.027(2) 0.000 0.020(2) 0.000 Na2 0.031(2) 0.034(2) 0.024(2) 0.000 0.0041(19) 0.000 O1 0.033(3) 0.074(4) 0.025(3) -0.008(3) 0.008(3) 0.001(3) O2 0.022(3) 0.044(3) 0.027(3) -0.001(2) 0.006(2) -0.003(2) O3 0.029(3) 0.047(3) 0.027(3) -0.007(2) 0.012(2) -0.007(2) O4 0.052(4) 0.046(3) 0.045(4) -0.014(3) 0.021(3) -0.015(3) O5 0.043(3) 0.047(3) 0.029(3) -0.005(3) 0.014(3) -0.010(3) O6 0.025(3) 0.043(3) 0.024(3) -0.005(2) 0.006(2) 0.000(2) O7 0.021(3) 0.034(3) 0.023(3) -0.001(2) 0.005(2) -0.001(2) O8 0.024(3) 0.035(3) 0.022(3) 0.001(2) 0.006(2) -0.003(2) O9 0.030(3) 0.034(3) 0.029(3) -0.004(2) 0.007(3) -0.003(2) O10 0.024(3) 0.044(3) 0.027(3) -0.010(2) 0.006(2) -0.003(2) O11 0.025(3) 0.031(3) 0.023(3) -0.004(2) 0.005(2) -0.001(2) O12 0.017(3) 0.032(4) 0.026(4) 0.000 0.002(3) 0.000 O13 0.024(3) 0.032(3) 0.023(3) 0.000(2) 0.004(2) 0.001(2) O14 0.020(4) 0.041(4) 0.020(4) 0.000 0.003(3) 0.000 O15 0.031(3) 0.037(3) 0.023(3) 0.000(2) 0.007(2) -0.003(2) O16 0.019(4) 0.043(4) 0.021(4) 0.000 0.003(3) 0.000 O17 0.027(4) 0.028(4) 0.019(4) 0.000 0.008(3) 0.000 C21 0.024(4) 0.044(4) 0.036(4) -0.012(4) 0.014(4) 0.003(3) C22 0.035(5) 0.060(5) 0.033(5) -0.011(4) 0.013(4) -0.004(4) C23 0.036(5) 0.074(6) 0.033(5) -0.013(4) 0.011(4) 0.005(4) C24 0.025(4) 0.061(5) 0.029(4) -0.021(4) -0.004(4) -0.001(3) C25 0.051(6) 0.069(6) 0.061(6) -0.035(5) 0.025(5) -0.026(5) C26 0.057(6) 0.079(7) 0.050(6) -0.031(5) 0.033(5) -0.027(5) N2 0.047(5) 0.079(6) 0.046(5) -0.027(5) 0.005(4) -0.001(4) O2A 0.069(5) 0.099(6) 0.050(5) -0.045(4) 0.017(4) -0.004(4) O2B 0.128(9) 0.104(7) 0.080(6) -0.056(6) 0.036(6) -0.074(6) C31 0.039(5) 0.068(6) 0.036(4) -0.016(4) 0.017(4) -0.012(4) C32 0.042(5) 0.168(12) 0.029(5) -0.018(7) 0.011(5) -0.034(7) C33 0.041(6) 0.229(16) 0.045(6) -0.022(9) 0.015(5) -0.030(8) C34 0.046(6) 0.240(15) 0.048(6) -0.035(9) 0.023(5) -0.052(8) C35 0.054(7) 0.36(2) 0.051(7) -0.032(12) 0.025(6) -0.069(11) C36 0.063(7) 0.299(19) 0.056(7) -0.061(11) 0.035(6) -0.082(10) C51 0.030(4) 0.066(6) 0.034(5) 0.000(4) 0.005(4) 0.005(4) C52 0.030(5) 0.210(15) 0.036(6) -0.024(8) 0.003(4) -0.006(7) C53 0.026(5) 0.215(16) 0.056(6) 0.000(9) 0.010(5) 0.021(7) C54 0.047(6) 0.49(2) 0.079(8) -0.069(14) 0.026(6) 0.020(13) C55 0.063(7) 0.56(3) 0.062(8) -0.058(16) 0.026(6) 0.019(16) C56 0.046(6) 0.37(2) 0.047(7) -0.064(12) 0.013(6) -0.023(12) N5 0.076(7) 0.74(3) 0.135(14) -0.120(18) 0.064(9) 0.000(17) O5A 0.183(16) 0.66(4) 0.209(19) -0.10(2) 0.141(15) 0.076(19) O5B 0.059(6) 0.87(5) 0.118(11) -0.049(18) 0.053(8) -0.022(16) C61 0.047(5) 0.036(4) 0.039(5) -0.001(4) 0.018(4) 0.002(4) C62 0.049(6) 0.055(6) 0.076(8) 0.024(5) -0.005(5) 0.000(5) C63 0.075(8) 0.090(7) 0.105(10) 0.070(7) 0.012(7) -0.004(6) C64 0.080(7) 0.050(5) 0.068(6) 0.024(5) 0.039(5) 0.024(5) C65 0.128(11) 0.057(6) 0.065(7) 0.026(6) 0.024(6) -0.005(6) C66 0.104(9) 0.048(6) 0.050(6) 0.011(5) 0.005(6) -0.028(5) N6 0.107(9) 0.080(6) 0.095(8) 0.051(6) 0.037(6) 0.017(6) O6A 0.191(11) 0.061(5) 0.090(7) 0.040(5) 0.044(7) 0.009(6) O6B 0.151(12) 0.118(9) 0.196(14) 0.108(10) -0.021(8) 0.007(7) C71 0.037(4) 0.033(4) 0.033(4) 0.007(3) 0.014(3) 0.009(3) C72 0.053(6) 0.062(6) 0.059(7) 0.019(5) -0.001(5) -0.017(5) C73 0.060(7) 0.087(7) 0.050(6) 0.037(6) -0.005(5) -0.011(5) C74 0.060(6) 0.054(5) 0.045(5) 0.023(4) 0.026(4) 0.011(4) C75 0.063(6) 0.065(6) 0.083(8) 0.036(6) 0.022(5) -0.003(5) C76 0.044(6) 0.057(6) 0.074(7) 0.023(5) 0.004(5) -0.004(4) N7 0.065(6) 0.083(6) 0.078(6) 0.044(5) 0.039(5) 0.020(5) O7A 0.113(8) 0.068(5) 0.163(10) 0.074(6) 0.045(7) 0.007(5) O7B 0.061(6) 0.167(9) 0.091(6) 0.089(6) 0.004(5) 0.016(5) C84 0.061(13) 0.051(12) 0.111(19) -0.015(11) 0.008(12) 0.007(8) C85 0.036(9) 0.058(11) 0.091(13) -0.020(9) 0.015(9) 0.008(7) C86 0.051(10) 0.053(10) 0.052(10) 0.018(7) 0.002(8) 0.029(7) C87 0.063(12) 0.066(12) 0.057(12) -0.024(9) 0.007(9) 0.027(8) C88 0.099(17) 0.064(14) 0.109(17) -0.026(12) 0.035(13) -0.021(12) C89 0.071(14) 0.096(16) 0.111(16) -0.011(13) 0.053(13) -0.001(10) C810 0.048(11) 0.088(14) 0.084(14) -0.031(11) 0.021(10) 0.016(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 Sb1 O2 1.977(6) . ? Sb1 O2 1.977(6) 6 ? Sb1 O1 1.980(6) 6 ? Sb1 O1 1.980(6) . ? Sb1 O16 2.123(7) . ? Sb1 C11 2.140(8) 6 ? Sb1 C11 2.140(8) . ? Sb2 O2 1.947(5) . ? Sb2 O3 1.951(6) . ? Sb2 O10 2.012(6) . ? Sb2 O9 2.023(5) . ? Sb2 C21 2.117(7) . ? Sb2 O7 2.125(5) . ? Sb2 Sb5 3.1514(7) . ? Sb2 Sb6 3.1546(7) . ? Sb2 Na1 3.427(3) . ? Sb3 O3 1.966(6) . ? Sb3 O5 1.979(6) . ? Sb3 O6 1.981(5) . ? Sb3 O4 2.008(6) . ? Sb3 O8 2.123(5) . ? Sb3 C31 2.140(8) . ? Sb3 Na1 3.742(3) . ? Sb4 O6 1.930(5) 6 ? Sb4 O6 1.930(5) . ? Sb4 O15 2.014(5) 6 ? Sb4 O15 2.014(5) . ? Sb4 C41 2.101(4) . ? Sb4 O17 2.144(7) . ? Sb4 Sb7 3.1511(8) 6 ? Sb4 Sb7 3.1511(8) . ? Sb4 Na1 3.362(5) . ? Sb5 O10 1.967(5) . ? Sb5 O12 1.982(4) . ? Sb5 O11 1.986(5) . ? Sb5 O16 2.069(5) . ? Sb5 O7 2.077(5) . ? Sb5 C51 2.119(4) . ? Sb5 Sb6 3.1338(8) . ? Sb5 Sb5 3.1380(10) 6 ? Sb6 O13 1.968(5) . ? Sb6 O9 1.970(5) . ? Sb6 O11 1.989(5) . ? Sb6 O8 2.061(5) . ? Sb6 O7 2.072(5) . ? Sb6 C61 2.119(8) . ? Sb6 Sb7 3.1386(8) . ? Sb7 O15 1.959(6) . ? Sb7 O13 1.984(5) . ? Sb7 O14 1.994(4) . ? Sb7 O17 2.059(4) . ? Sb7 O8 2.073(5) . ? Sb7 C71 2.118(7) . ? Sb7 Sb7 3.1266(10) 6 ? Na1 O17 2.535(8) . ? Na1 O7 2.584(6) 6 ? Na1 O7 2.584(6) . ? Na1 OW1 2.642(17) . ? Na1 O6 2.735(7) . ? Na1 O6 2.735(7) 6 ? Na1 O3 2.775(6) 6 ? Na1 O3 2.775(6) . ? Na1 O2 2.815(7) 6 ? Na1 O2 2.815(7) . ? Na1 Sb2 3.427(3) 6 ? Na2 O12 2.349(9) . ? Na2 O13 2.350(6) . ? Na2 O13 2.350(6) 6 ? Na2 OW2 2.593(7) 6 ? Na2 OW2 2.593(7) . ? Na2 OW3 2.733(10) . ? O12 Sb5 1.982(4) 6 ? O14 Sb7 1.994(4) 6 ? O16 Sb5 2.069(5) 6 ? O17 Sb7 2.059(4) 6 ? C11 C12 1.3900 . ? C11 C12A 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C14 C13A 1.3900 . ? C14 N1 1.60(3) . ? C13A C12A 1.3900 . ? N1 O1A 1.322(16) . ? C21 C22 1.363(10) . ? C21 C26 1.367(10) . ? C22 C23 1.401(10) . ? C23 C24 1.334(11) . ? C24 C25 1.325(11) . ? C24 N2 1.490(9) . ? C25 C26 1.398(10) . ? N2 O2A 1.216(10) . ? N2 O2B 1.225(10) . ? C31 C36 1.331(11) . ? C31 C32 1.350(10) . ? C32 C33 1.410(11) . ? C33 C34 1.333(12) . ? C34 C35 1.306(12) . ? C34 N3 1.491(12) . ? C35 C36 1.408(12) . ? N3 O3B 1.224(12) . ? N3 O3A 1.235(13) . ? C41 C42 1.3900 . ? C41 C42A 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C43A 1.3900 . ? C44 N4 1.4603 . ? C43A C42A 1.3900 . ? N4 O4A 1.220(13) 6 ? N4 O4A 1.2188 . ? N4 C44 1.460(2) 6 ? C51 C56 1.324(11) . ? C51 C52 1.3552 . ? C52 C53 1.370(10) . ? C53 C54 1.318(12) . ? C54 C55 1.343(13) . ? C54 N5 1.489(13) . ? C55 C56 1.416(13) . ? N5 O5B 1.249(13) . ? N5 O5A 1.254(15) . ? C61 C62 1.370(10) . ? C61 C66 1.370(10) . ? C62 C63 1.399(11) . ? C63 C64 1.360(12) . ? C64 C65 1.316(12) . ? C64 N6 1.475(10) . ? C65 C66 1.408(11) . ? N6 O6A 1.208(11) . ? N6 O6B 1.246(12) . ? C71 C72 1.352(10) . ? C71 C76 1.362(10) . ? C72 C73 1.385(11) . ? C73 C74 1.322(11) . ? C74 C75 1.329(11) . ? C74 N7 1.484(10) . ? C75 C76 1.397(11) . ? N7 O7A 1.198(11) . ? N7 O7B 1.240(11) . ? N8 C82 1.39(3) . ? N8 C81 1.46(2) . ? N8 C84 1.47(2) . ? N8 C83 1.480(17) . ? C84 C85 1.48(3) . ? C85 C86 1.3900 . ? C85 C810 1.3900 . ? C86 C87 1.3900 . ? C87 C88 1.3900 . ? C88 C89 1.3900 . ? C89 C810 1.3900 . ? 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 Sb1 O2 84.1(3) . 6 ? O2 Sb1 O1 175.4(2) . 6 ? O2 Sb1 O1 93.1(3) 6 6 ? O2 Sb1 O1 93.1(3) . . ? O2 Sb1 O1 175.4(2) 6 . ? O1 Sb1 O1 89.4(4) 6 . ? O2 Sb1 O16 89.6(2) . . ? O2 Sb1 O16 89.6(2) 6 . ? O1 Sb1 O16 86.7(2) 6 . ? O1 Sb1 O16 86.7(2) . . ? O2 Sb1 C11 94.7(4) . 6 ? O2 Sb1 C11 90.4(4) 6 6 ? O1 Sb1 C11 89.0(4) 6 6 ? O1 Sb1 C11 93.5(4) . 6 ? O16 Sb1 C11 175.7(4) . 6 ? O2 Sb1 C11 90.4(4) . . ? O2 Sb1 C11 94.7(4) 6 . ? O1 Sb1 C11 93.5(4) 6 . ? O1 Sb1 C11 89.0(4) . . ? O16 Sb1 C11 175.7(4) . . ? C11 Sb1 C11 6.4(9) 6 . ? O2 Sb2 O3 86.5(2) . . ? O2 Sb2 O10 90.8(2) . . ? O3 Sb2 O10 165.0(2) . . ? O2 Sb2 O9 164.6(2) . . ? O3 Sb2 O9 90.5(2) . . ? O10 Sb2 O9 88.2(2) . . ? O2 Sb2 C21 98.4(3) . . ? O3 Sb2 C21 98.5(3) . . ? O10 Sb2 C21 96.5(2) . . ? O9 Sb2 C21 96.9(3) . . ? O2 Sb2 O7 87.1(2) . . ? O3 Sb2 O7 87.3(2) . . ? O10 Sb2 O7 77.8(2) . . ? O9 Sb2 O7 77.7(2) . . ? C21 Sb2 O7 172.1(2) . . ? O2 Sb2 Sb5 86.13(15) . . ? O3 Sb2 Sb5 127.93(16) . . ? O10 Sb2 Sb5 37.12(15) . . ? O9 Sb2 Sb5 83.83(15) . . ? C21 Sb2 Sb5 133.6(2) . . ? O7 Sb2 Sb5 40.84(14) . . ? O2 Sb2 Sb6 127.45(16) . . ? O3 Sb2 Sb6 85.89(16) . . ? O10 Sb2 Sb6 84.09(15) . . ? O9 Sb2 Sb6 37.22(14) . . ? C21 Sb2 Sb6 134.1(2) . . ? O7 Sb2 Sb6 40.62(14) . . ? Sb5 Sb2 Sb6 59.597(17) . . ? O2 Sb2 Na1 55.22(18) . . ? O3 Sb2 Na1 54.05(18) . . ? O10 Sb2 Na1 112.87(17) . . ? O9 Sb2 Na1 111.39(17) . . ? C21 Sb2 Na1 139.0(2) . . ? O7 Sb2 Na1 48.84(16) . . ? Sb5 Sb2 Na1 80.22(8) . . ? Sb6 Sb2 Na1 79.00(8) . . ? O3 Sb3 O5 174.7(2) . . ? O3 Sb3 O6 85.7(2) . . ? O5 Sb3 O6 93.4(2) . . ? O3 Sb3 O4 91.5(3) . . ? O5 Sb3 O4 88.9(3) . . ? O6 Sb3 O4 174.1(2) . . ? O3 Sb3 O8 89.4(2) . . ? O5 Sb3 O8 85.4(2) . . ? O6 Sb3 O8 88.8(2) . . ? O4 Sb3 O8 86.0(2) . . ? O3 Sb3 C31 93.1(3) . . ? O5 Sb3 C31 92.2(3) . . ? O6 Sb3 C31 93.3(3) . . ? O4 Sb3 C31 92.0(3) . . ? O8 Sb3 C31 176.9(3) . . ? O3 Sb3 Na1 46.30(17) . . ? O5 Sb3 Na1 130.48(18) . . ? O6 Sb3 Na1 45.21(17) . . ? O4 Sb3 Na1 130.0(2) . . ? O8 Sb3 Na1 70.83(16) . . ? C31 Sb3 Na1 112.2(3) . . ? O6 Sb4 O6 87.2(3) 6 . ? O6 Sb4 O15 89.7(2) 6 6 ? O6 Sb4 O15 163.8(2) . 6 ? O6 Sb4 O15 163.8(2) 6 . ? O6 Sb4 O15 89.7(2) . . ? O15 Sb4 O15 88.9(3) 6 . ? O6 Sb4 C41 98.7(2) 6 . ? O6 Sb4 C41 99.5(2) . . ? O15 Sb4 C41 96.7(2) 6 . ? O15 Sb4 C41 97.5(2) . . ? O6 Sb4 O17 86.7(2) 6 . ? O6 Sb4 O17 86.7(2) . . ? O15 Sb4 O17 77.2(2) 6 . ? O15 Sb4 O17 77.2(2) . . ? C41 Sb4 O17 171.9(2) . . ? O6 Sb4 Sb7 85.19(15) 6 6 ? O6 Sb4 Sb7 126.89(16) . 6 ? O15 Sb4 Sb7 36.92(16) 6 6 ? O15 Sb4 Sb7 83.99(15) . 6 ? C41 Sb4 Sb7 133.64(14) . 6 ? O17 Sb4 Sb7 40.43(12) . 6 ? O6 Sb4 Sb7 126.89(16) 6 . ? O6 Sb4 Sb7 85.19(15) . . ? O15 Sb4 Sb7 83.99(15) 6 . ? O15 Sb4 Sb7 36.92(16) . . ? C41 Sb4 Sb7 134.39(15) . . ? O17 Sb4 Sb7 40.43(12) . . ? Sb7 Sb4 Sb7 59.48(2) 6 . ? O6 Sb4 Na1 54.43(17) 6 . ? O6 Sb4 Na1 54.43(17) . . ? O15 Sb4 Na1 111.47(17) 6 . ? O15 Sb4 Na1 111.47(17) . . ? C41 Sb4 Na1 139.17(14) . . ? O17 Sb4 Na1 48.9(2) . . ? Sb7 Sb4 Na1 79.31(8) 6 . ? Sb7 Sb4 Na1 79.31(8) . . ? O10 Sb5 O12 165.7(2) . . ? O10 Sb5 O11 97.3(2) . . ? O12 Sb5 O11 92.3(2) . . ? O10 Sb5 O16 90.0(2) . . ? O12 Sb5 O16 78.2(2) . . ? O11 Sb5 O16 163.9(3) . . ? O10 Sb5 O7 79.9(2) . . ? O12 Sb5 O7 91.6(3) . . ? O11 Sb5 O7 78.6(2) . . ? O16 Sb5 O7 88.5(2) . . ? O10 Sb5 C51 94.5(3) . . ? O12 Sb5 C51 95.2(3) . . ? O11 Sb5 C51 95.8(3) . . ? O16 Sb5 C51 98.0(3) . . ? O7 Sb5 C51 171.5(3) . . ? O10 Sb5 Sb6 85.37(17) . . ? O12 Sb5 Sb6 95.8(2) . . ? O11 Sb5 Sb6 38.00(15) . . ? O16 Sb5 Sb6 129.2(2) . . ? O7 Sb5 Sb6 40.88(14) . . ? C51 Sb5 Sb6 132.8(2) . . ? O10 Sb5 Sb5 130.55(16) . 6 ? O12 Sb5 Sb5 37.68(16) . 6 ? O11 Sb5 Sb5 129.38(14) . 6 ? O16 Sb5 Sb5 40.67(15) . 6 ? O7 Sb5 Sb5 92.73(14) . 6 ? C51 Sb5 Sb5 95.8(2) . 6 ? Sb6 Sb5 Sb5 119.729(13) . 6 ? O10 Sb5 Sb2 38.12(16) . . ? O12 Sb5 Sb2 131.6(2) . . ? O11 Sb5 Sb2 90.51(14) . . ? O16 Sb5 Sb2 86.36(17) . . ? O7 Sb5 Sb2 41.98(14) . . ? C51 Sb5 Sb2 132.6(2) . . ? Sb6 Sb5 Sb2 60.253(17) . . ? Sb5 Sb5 Sb2 115.728(13) 6 . ? O13 Sb6 O9 166.1(2) . . ? O13 Sb6 O11 93.0(2) . . ? O9 Sb6 O11 96.7(2) . . ? O13 Sb6 O8 78.2(2) . . ? O9 Sb6 O8 90.0(2) . . ? O11 Sb6 O8 164.3(2) . . ? O13 Sb6 O7 92.1(2) . . ? O9 Sb6 O7 80.1(2) . . ? O11 Sb6 O7 78.7(2) . . ? O8 Sb6 O7 88.5(2) . . ? O13 Sb6 C61 95.3(3) . . ? O9 Sb6 C61 93.8(3) . . ? O11 Sb6 C61 94.8(3) . . ? O8 Sb6 C61 98.9(3) . . ? O7 Sb6 C61 170.4(3) . . ? O13 Sb6 Sb5 96.61(16) . . ? O9 Sb6 Sb5 85.13(17) . . ? O11 Sb6 Sb5 37.94(15) . . ? O8 Sb6 Sb5 129.38(14) . . ? O7 Sb6 Sb5 41.01(14) . . ? C61 Sb6 Sb5 131.6(3) . . ? O13 Sb6 Sb7 37.58(15) . . ? O9 Sb6 Sb7 130.67(16) . . ? O11 Sb6 Sb7 130.04(14) . . ? O8 Sb6 Sb7 40.76(14) . . ? O7 Sb6 Sb7 93.16(15) . . ? C61 Sb6 Sb7 96.4(2) . . ? Sb5 Sb6 Sb7 120.47(2) . . ? O13 Sb6 Sb2 131.95(14) . . ? O9 Sb6 Sb2 38.40(16) . . ? O11 Sb6 Sb2 90.37(14) . . ? O8 Sb6 Sb2 86.09(14) . . ? O7 Sb6 Sb2 41.89(14) . . ? C61 Sb6 Sb2 132.1(2) . . ? Sb5 Sb6 Sb2 60.151(17) . . ? Sb7 Sb6 Sb2 115.85(2) . . ? O15 Sb7 O13 165.7(2) . . ? O15 Sb7 O14 96.8(3) . . ? O13 Sb7 O14 93.2(3) . . ? O15 Sb7 O17 80.4(3) . . ? O13 Sb7 O17 91.6(2) . . ? O14 Sb7 O17 78.8(2) . . ? O15 Sb7 O8 90.4(2) . . ? O13 Sb7 O8 77.5(2) . . ? O14 Sb7 O8 164.2(2) . . ? O17 Sb7 O8 88.7(2) . . ? O15 Sb7 C71 94.9(3) . . ? O13 Sb7 C71 93.9(3) . . ? O14 Sb7 C71 97.5(3) . . ? O17 Sb7 C71 173.5(3) . . ? O8 Sb7 C71 95.9(3) . . ? O15 Sb7 Sb7 85.51(15) . 6 ? O13 Sb7 Sb7 96.18(14) . 6 ? O14 Sb7 Sb7 38.39(15) . 6 ? O17 Sb7 Sb7 40.61(14) . 6 ? O8 Sb7 Sb7 129.09(14) . 6 ? C71 Sb7 Sb7 135.0(2) . 6 ? O15 Sb7 Sb6 130.72(15) . . ? O13 Sb7 Sb6 37.23(14) . . ? O14 Sb7 Sb6 129.9(2) . . ? O17 Sb7 Sb6 92.88(18) . . ? O8 Sb7 Sb6 40.46(15) . . ? C71 Sb7 Sb6 93.6(2) . . ? Sb7 Sb7 Sb6 119.799(13) 6 . ? O15 Sb7 Sb4 38.12(15) . . ? O13 Sb7 Sb4 132.00(14) . . ? O14 Sb7 Sb4 90.38(17) . . ? O17 Sb7 Sb4 42.5(2) . . ? O8 Sb7 Sb4 86.65(14) . . ? C71 Sb7 Sb4 133.0(2) . . ? Sb7 Sb7 Sb4 60.258(11) 6 . ? Sb6 Sb7 Sb4 116.14(2) . . ? O17 Na1 O7 81.9(2) . 6 ? O17 Na1 O7 81.9(2) . . ? O7 Na1 O7 80.4(3) 6 . ? O17 Na1 OW1 142.5(5) . . ? O7 Na1 OW1 124.6(3) 6 . ? O7 Na1 OW1 124.6(3) . . ? O17 Na1 O6 64.1(2) . . ? O7 Na1 O6 145.2(2) 6 . ? O7 Na1 O6 101.11(17) . . ? OW1 Na1 O6 83.5(4) . . ? O17 Na1 O6 64.1(2) . 6 ? O7 Na1 O6 101.11(17) 6 6 ? O7 Na1 O6 145.2(2) . 6 ? OW1 Na1 O6 83.5(4) . 6 ? O6 Na1 O6 58.2(2) . 6 ? O17 Na1 O3 101.47(15) . 6 ? O7 Na1 O3 63.31(16) 6 6 ? O7 Na1 O3 142.4(2) . 6 ? OW1 Na1 O3 74.09(15) . 6 ? O6 Na1 O3 114.2(2) . 6 ? O6 Na1 O3 58.29(17) 6 6 ? O17 Na1 O3 101.47(15) . . ? O7 Na1 O3 142.4(2) 6 . ? O7 Na1 O3 63.31(16) . . ? OW1 Na1 O3 74.09(15) . . ? O6 Na1 O3 58.29(17) . . ? O6 Na1 O3 114.2(2) 6 . ? O3 Na1 O3 148.0(3) 6 . ? O17 Na1 O2 143.7(2) . 6 ? O7 Na1 O2 62.54(18) 6 6 ? O7 Na1 O2 98.4(2) . 6 ? OW1 Na1 O2 65.2(3) . 6 ? O6 Na1 O2 148.6(2) . 6 ? O6 Na1 O2 113.29(18) 6 6 ? O3 Na1 O2 57.08(17) 6 6 ? O3 Na1 O2 111.1(2) . 6 ? O17 Na1 O2 143.7(2) . . ? O7 Na1 O2 98.4(2) 6 . ? O7 Na1 O2 62.54(18) . . ? OW1 Na1 O2 65.2(3) . . ? O6 Na1 O2 113.29(18) . . ? O6 Na1 O2 148.6(2) 6 . ? O3 Na1 O2 111.1(2) 6 . ? O3 Na1 O2 57.08(17) . . ? O2 Na1 O2 56.1(2) 6 . ? O17 Na1 Sb4 39.60(18) . . ? O7 Na1 Sb4 111.75(17) 6 . ? O7 Na1 Sb4 111.75(17) . . ? OW1 Na1 Sb4 102.9(4) . . ? O6 Na1 Sb4 35.04(12) . . ? O6 Na1 Sb4 35.04(12) 6 . ? O3 Na1 Sb4 91.80(16) 6 . ? O3 Na1 Sb4 91.80(16) . . ? O2 Na1 Sb4 148.25(15) 6 . ? O2 Na1 Sb4 148.25(15) . . ? O17 Na1 Sb2 110.70(11) . 6 ? O7 Na1 Sb2 38.25(11) 6 6 ? O7 Na1 Sb2 108.7(2) . 6 ? OW1 Na1 Sb2 87.0(2) . 6 ? O6 Na1 Sb2 148.79(17) . 6 ? O6 Na1 Sb2 91.22(12) 6 6 ? O3 Na1 Sb2 34.69(12) 6 6 ? O3 Na1 Sb2 145.6(2) . 6 ? O2 Na1 Sb2 34.62(12) 6 6 ? O2 Na1 Sb2 89.04(16) . 6 ? Sb4 Na1 Sb2 120.76(7) . 6 ? O12 Na2 O13 98.5(2) . . ? O12 Na2 O13 98.5(2) . 6 ? O13 Na2 O13 98.2(3) . 6 ? O12 Na2 OW2 85.7(2) . 6 ? O13 Na2 OW2 175.1(3) . 6 ? O13 Na2 OW2 83.55(18) 6 6 ? O12 Na2 OW2 85.7(2) . . ? O13 Na2 OW2 83.55(18) . . ? O13 Na2 OW2 175.1(3) 6 . ? OW2 Na2 OW2 94.3(3) 6 . ? O12 Na2 OW3 176.7(3) . . ? O13 Na2 OW3 83.7(2) . . ? O13 Na2 OW3 83.7(2) 6 . ? OW2 Na2 OW3 92.0(2) 6 . ? OW2 Na2 OW3 92.0(2) . . ? Sb2 O2 Sb1 135.7(3) . . ? Sb2 O2 Na1 90.2(2) . . ? Sb1 O2 Na1 105.1(2) . . ? Sb2 O3 Sb3 136.3(3) . . ? Sb2 O3 Na1 91.3(2) . . ? Sb3 O3 Na1 102.9(2) . . ? Sb4 O6 Sb3 137.8(3) . . ? Sb4 O6 Na1 90.5(2) . . ? Sb3 O6 Na1 103.9(2) . . ? Sb6 O7 Sb5 98.1(2) . . ? Sb6 O7 Sb2 97.5(2) . . ? Sb5 O7 Sb2 97.2(2) . . ? Sb6 O7 Na1 128.1(3) . . ? Sb5 O7 Na1 130.8(2) . . ? Sb2 O7 Na1 92.91(19) . . ? Sb6 O8 Sb7 98.8(2) . . ? Sb6 O8 Sb3 129.4(3) . . ? Sb7 O8 Sb3 128.6(3) . . ? Sb6 O9 Sb2 104.4(2) . . ? Sb5 O10 Sb2 104.8(3) . . ? Sb5 O11 Sb6 104.1(2) . . ? Sb5 O12 Sb5 104.6(3) 6 . ? Sb5 O12 Na2 122.7(2) 6 . ? Sb5 O12 Na2 122.7(2) . . ? Sb6 O13 Sb7 105.2(2) . . ? Sb6 O13 Na2 122.4(3) . . ? Sb7 O13 Na2 122.7(3) . . ? Sb7 O14 Sb7 103.2(3) 6 . ? Sb7 O15 Sb4 105.0(3) . . ? Sb5 O16 Sb5 98.7(3) 6 . ? Sb5 O16 Sb1 128.86(16) 6 . ? Sb5 O16 Sb1 128.86(16) . . ? Sb7 O17 Sb7 98.8(3) 6 . ? Sb7 O17 Sb4 97.1(2) 6 . ? Sb7 O17 Sb4 97.1(2) . . ? Sb7 O17 Na1 129.47(16) 6 . ? Sb7 O17 Na1 129.47(16) . . ? Sb4 O17 Na1 91.5(3) . . ? C12 C11 C12A 120.0 . . ? C12 C11 Sb1 123.8(9) . . ? C12A C11 Sb1 116.2(9) . . ? C13 C12 C11 120.0 . . ? C12 C13 C14 120.0 . . ? C13 C14 C13A 120.0 . . ? C13 C14 N1 124.4(11) . . ? C13A C14 N1 114.8(11) . . ? C12A C13A C14 120.0 . . ? C13A C12A C11 120.0 . . ? O1A N1 C14 103.9(15) . . ? C22 C21 C26 118.0(7) . . ? C22 C21 Sb2 121.0(6) . . ? C26 C21 Sb2 121.0(6) . . ? C21 C22 C23 121.8(8) . . ? C24 C23 C22 117.7(8) . . ? C25 C24 C23 122.8(8) . . ? C25 C24 N2 118.6(8) . . ? C23 C24 N2 118.6(8) . . ? C24 C25 C26 119.8(9) . . ? C21 C26 C25 120.0(9) . . ? O2A N2 O2B 123.2(9) . . ? O2A N2 C24 117.4(9) . . ? O2B N2 C24 119.4(9) . . ? C36 C31 C32 116.8(9) . . ? C36 C31 Sb3 120.3(7) . . ? C32 C31 Sb3 122.9(7) . . ? C31 C32 C33 121.8(9) . . ? C34 C33 C32 117.7(10) . . ? C35 C34 C33 122.9(10) . . ? C35 C34 N3 117.8(10) . . ? C33 C34 N3 118.5(10) . . ? C34 C35 C36 118.0(11) . . ? C31 C36 C35 122.6(10) . . ? O3B N3 O3A 123.3(15) . . ? O3B N3 C34 119.9(13) . . ? O3A N3 C34 116.6(14) . . ? C42 C41 C42A 120.0 . . ? C42 C41 Sb4 123.9(2) . . ? C42A C41 Sb4 116.0(2) . . ? C43 C42 C41 120.0 . . ? C42 C43 C44 120.0 . . ? C43A C44 C43 120.0 . . ? C43A C44 N4 132.2 . . ? C43 C44 N4 107.6 . . ? C44 C43A C42A 120.0 . . ? C43A C42A C41 120.0 . . ? O4A N4 O4A 123.4(3) 6 . ? O4A N4 C44 109.5(8) 6 6 ? O4A N4 C44 127.0(5) . 6 ? O4A N4 C44 127.0(3) 6 . ? O4A N4 C44 109.6 . . ? C44 N4 C44 17.5(5) 6 . ? C56 C51 C52 116.4(6) . . ? C56 C51 Sb5 121.1(6) . . ? C52 C51 Sb5 122.43(15) . . ? C51 C52 C53 124.0(6) . . ? C54 C53 C52 117.2(9) . . ? C53 C54 C55 123.2(11) . . ? C53 C54 N5 117.6(11) . . ? C55 C54 N5 117.9(12) . . ? C54 C55 C56 116.8(11) . . ? C51 C56 C55 122.3(10) . . ? O5B N5 O5A 124.0(18) . . ? O5B N5 C54 115.0(13) . . ? O5A N5 C54 117.6(15) . . ? C62 C61 C66 117.3(8) . . ? C62 C61 Sb6 120.6(6) . . ? C66 C61 Sb6 121.7(6) . . ? C61 C62 C63 121.5(9) . . ? C64 C63 C62 117.9(10) . . ? C65 C64 C63 122.5(9) . . ? C65 C64 N6 119.0(9) . . ? C63 C64 N6 118.5(9) . . ? C64 C65 C66 119.2(10) . . ? C61 C66 C65 120.8(9) . . ? O6A N6 O6B 125.5(10) . . ? O6A N6 C64 120.0(10) . . ? O6B N6 C64 114.4(10) . . ? C72 C71 C76 117.2(8) . . ? C72 C71 Sb7 122.6(6) . . ? C76 C71 Sb7 120.2(6) . . ? C71 C72 C73 121.6(9) . . ? C74 C73 C72 119.6(9) . . ? C73 C74 C75 120.5(8) . . ? C73 C74 N7 120.6(8) . . ? C75 C74 N7 118.9(8) . . ? C74 C75 C76 120.1(9) . . ? C71 C76 C75 120.1(9) . . ? O7A N7 O7B 126.4(10) . . ? O7A N7 C74 118.7(9) . . ? O7B N7 C74 114.6(9) . . ? C82 N8 C81 106.5(16) . . ? C82 N8 C84 101(2) . . ? C81 N8 C84 115.9(15) . . ? C82 N8 C83 106.1(18) . . ? C81 N8 C83 111.6(15) . . ? C84 N8 C83 114.5(15) . . ? N8 C84 C85 119.6(17) . . ? C86 C85 C810 120.0 . . ? C86 C85 C84 117.7(18) . . ? C810 C85 C84 122.2(18) . . ? C87 C86 C85 120.0 . . ? C86 C87 C88 120.0 . . ? C89 C88 C87 120.0 . . ? C88 C89 C810 120.0 . . ? C89 C810 C85 120.0 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.282 _refine_diff_density_min -1.597 _refine_diff_density_rms 0.201 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.013 0.000 0.487 1591.8 232.3 2 0.500 0.000 0.500 269.5 72.8 3 0.246 0.500 0.246 1591.8 232.3 4 0.000 0.500 0.500 269.6 72.8 _platon_squeeze_details ; ;