# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1472 data_naclo418 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H26 Cl Na O11' _chemical_formula_weight 404.77 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' 'Cl' 'Cl' 0.1484 0.1585 '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 orthorhombic _symmetry_space_group_name_H-M Pc21n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, z+1/2' '-x, y+1/2, -z' 'x+1/2, y+1/2, -z+1/2' _cell_length_a 9.1846(3) _cell_length_b 13.9712(5) _cell_length_c 14.6305(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1877.38(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.8 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 0.278 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '2o phi frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 16095 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3448 _reflns_number_gt 3309 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics RES2INS _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+0.4438P] 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 SHELXL _refine_ls_extinction_coef 0.026(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.49(5) _refine_ls_number_reflns 3448 _refine_ls_number_parameters 236 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.56617(5) 0.34802(3) 0.32140(3) 0.03342(13) Uani 1 1 d . . . Na1 Na 0.36102(9) 0.50582(7) 0.19358(6) 0.0438(2) Uani 1 1 d . . . O1 O 0.3438(2) 0.66366(13) 0.14018(13) 0.0495(4) Uani 1 1 d . . . H2 H 0.389(5) 0.682(3) 0.184(3) 0.104(15) Uiso 1 1 d . . . H1 H 0.266(5) 0.694(3) 0.133(3) 0.100(14) Uiso 1 1 d . . . O2 O 0.4333(2) 0.36542(17) 0.27446(16) 0.0788(7) Uani 1 1 d . . . O3 O 0.6773(3) 0.32749(16) 0.25861(17) 0.0930(9) Uani 1 1 d . . . O4 O 0.54783(18) 0.26764(12) 0.38128(14) 0.0552(5) Uani 1 1 d . . . O5 O 0.6019(3) 0.42989(15) 0.37275(17) 0.0819(7) Uani 1 1 d . . . O1A O 0.48541(14) 0.44373(10) 0.04525(9) 0.0376(3) Uani 1 1 d . . . O2A O 0.20692(14) 0.39015(10) 0.09505(9) 0.0379(3) Uani 1 1 d . . . O3A O 0.07955(14) 0.50481(11) 0.22717(10) 0.0373(3) Uani 1 1 d . . . O4A O 0.26133(15) 0.59066(11) 0.35635(9) 0.0407(3) Uani 1 1 d . . . O5A O 0.53131(16) 0.66853(12) 0.30117(12) 0.0455(3) Uani 1 1 d . . . O6A O 0.65991(15) 0.56209(10) 0.15866(10) 0.0409(3) Uani 1 1 d . . . C1A C 0.4277(2) 0.35308(17) 0.02168(13) 0.0421(4) Uani 1 1 d . . . H1A2 H 0.4474 0.3063 0.0710 0.050 Uiso 1 1 calc R . . H1A1 H 0.4732 0.3295 -0.0354 0.050 Uiso 1 1 calc R . . C2A C 0.2667(2) 0.36490(16) 0.00863(13) 0.0417(5) Uani 1 1 d . . . H2A2 H 0.2468 0.4158 -0.0368 0.050 Uiso 1 1 calc R . . H2A1 H 0.2231 0.3044 -0.0136 0.050 Uiso 1 1 calc R . . C3A C 0.0589(2) 0.41959(16) 0.08867(15) 0.0420(5) Uani 1 1 d . . . H3A2 H 0.0015 0.3716 0.0543 0.050 Uiso 1 1 calc R . . H3A1 H 0.0519 0.4818 0.0565 0.050 Uiso 1 1 calc R . . C4A C 0.0025(2) 0.42865(16) 0.18386(14) 0.0403(4) Uani 1 1 d . . . H4A2 H -0.1031 0.4427 0.1829 0.048 Uiso 1 1 calc R . . H4A1 H 0.0180 0.3681 0.2177 0.048 Uiso 1 1 calc R . . C5A C 0.0405(2) 0.51203(18) 0.32043(14) 0.0425(5) Uani 1 1 d . . . H5A2 H 0.0749 0.4548 0.3539 0.051 Uiso 1 1 calc R . . H5A1 H -0.0668 0.5154 0.3263 0.051 Uiso 1 1 calc R . . C6A C 0.1078(2) 0.60002(18) 0.36041(15) 0.0470(5) Uani 1 1 d . . . H6A2 H 0.0765 0.6572 0.3255 0.056 Uiso 1 1 calc R . . H6A1 H 0.0762 0.6079 0.4247 0.056 Uiso 1 1 calc R . . C7A C 0.3307(3) 0.66825(17) 0.40259(16) 0.0487(5) Uani 1 1 d . . . H7A2 H 0.3021 0.6686 0.4678 0.058 Uiso 1 1 calc R . . H7A1 H 0.3006 0.7299 0.3750 0.058 Uiso 1 1 calc R . . C8A C 0.4912(3) 0.65595(16) 0.39419(15) 0.0473(5) Uani 1 1 d . . . H8A2 H 0.5419 0.7037 0.4328 0.057 Uiso 1 1 calc R . . H8A1 H 0.5197 0.5912 0.4151 0.057 Uiso 1 1 calc R . . C9A C 0.6845(2) 0.66105(18) 0.28920(18) 0.0506(5) Uani 1 1 d . . . H9A2 H 0.7220 0.6044 0.3224 0.061 Uiso 1 1 calc R . . H9A1 H 0.7332 0.7188 0.3138 0.061 Uiso 1 1 calc R . . C10A C 0.7155(3) 0.65150(16) 0.18935(18) 0.0516(6) Uani 1 1 d . . . H10B H 0.6686 0.7045 0.1554 0.062 Uiso 1 1 calc R . . H10A H 0.8218 0.6546 0.1784 0.062 Uiso 1 1 calc R . . C11A C 0.6901(2) 0.54449(18) 0.06535(15) 0.0468(5) Uani 1 1 d . . . H11B H 0.7959 0.5507 0.0539 0.056 Uiso 1 1 calc R . . H11A H 0.6384 0.5918 0.0268 0.056 Uiso 1 1 calc R . . C12A C 0.6407(2) 0.44585(18) 0.04199(15) 0.0447(5) Uani 1 1 d . . . H12B H 0.6749 0.4283 -0.0200 0.054 Uiso 1 1 calc R . . H12A H 0.6815 0.3993 0.0862 0.054 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0368(2) 0.0309(2) 0.0326(2) 0.00115(18) -0.00144(15) 0.00443(19) Na1 0.0470(5) 0.0396(4) 0.0449(4) 0.0068(3) 0.0011(3) 0.0075(4) O1 0.0566(10) 0.0460(9) 0.0460(9) 0.0041(7) 0.0009(7) 0.0134(8) O2 0.0657(12) 0.0754(14) 0.0955(15) 0.0365(12) -0.0425(10) -0.0092(10) O3 0.1081(18) 0.0736(14) 0.0971(16) 0.0216(12) 0.0672(14) 0.0333(12) O4 0.0545(10) 0.0500(9) 0.0610(11) 0.0271(8) 0.0026(7) 0.0043(7) O5 0.1254(19) 0.0504(11) 0.0700(14) -0.0198(10) -0.0227(12) -0.0071(11) O1A 0.0290(7) 0.0422(7) 0.0414(7) -0.0010(6) 0.0014(5) 0.0041(6) O2A 0.0340(7) 0.0468(8) 0.0330(7) 0.0005(6) -0.0014(5) 0.0021(6) O3A 0.0333(7) 0.0416(7) 0.0370(7) 0.0049(6) 0.0030(5) -0.0024(6) O4A 0.0404(7) 0.0416(8) 0.0402(8) -0.0060(6) 0.0017(6) 0.0030(6) O5A 0.0393(7) 0.0437(8) 0.0533(9) 0.0015(6) -0.0068(7) 0.0005(7) O6A 0.0365(7) 0.0419(8) 0.0444(8) 0.0066(6) 0.0026(6) -0.0042(6) C1A 0.0502(11) 0.0370(9) 0.0390(9) -0.0014(10) 0.0072(8) 0.0038(10) C2A 0.0457(11) 0.0462(12) 0.0334(9) -0.0019(8) 0.0017(8) -0.0087(9) C3A 0.0339(10) 0.0478(12) 0.0444(12) 0.0020(9) -0.0085(8) -0.0027(8) C4A 0.0276(9) 0.0460(11) 0.0473(11) 0.0042(9) -0.0010(8) -0.0049(8) C5A 0.0336(9) 0.0551(12) 0.0388(11) 0.0074(9) 0.0091(7) 0.0024(9) C6A 0.0436(12) 0.0568(14) 0.0405(11) -0.0037(10) 0.0092(9) 0.0095(10) C7A 0.0588(13) 0.0450(12) 0.0422(12) -0.0109(9) -0.0043(9) 0.0035(10) C8A 0.0552(13) 0.0429(11) 0.0436(12) -0.0067(9) -0.0132(9) 0.0006(10) C9A 0.0384(11) 0.0443(12) 0.0693(15) -0.0058(11) -0.0096(10) -0.0033(10) C10A 0.0388(11) 0.0413(12) 0.0747(16) 0.0104(11) -0.0004(10) -0.0102(10) C11A 0.0280(9) 0.0687(14) 0.0438(11) 0.0158(10) 0.0007(8) -0.0028(9) C12A 0.0301(10) 0.0661(14) 0.0380(11) 0.0014(10) 0.0040(8) 0.0114(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 O3 1.4031(18) . ? Cl1 O5 1.407(2) . ? Cl1 O2 1.4213(17) . ? Cl1 O4 1.4342(16) . ? Na1 O1 2.345(2) . ? Na1 O2 2.385(2) . ? Na1 O2A 2.5871(17) . ? Na1 O1A 2.6014(16) . ? Na1 O3A 2.6316(15) . ? Na1 O4A 2.8132(16) . ? Na1 O6A 2.9008(16) . ? O1A C1A 1.415(3) . ? O1A C12A 1.427(2) . ? O2A C2A 1.423(2) . ? O2A C3A 1.423(2) . ? O3A C5A 1.414(2) . ? O3A C4A 1.426(3) . ? O4A C6A 1.417(3) . ? O4A C7A 1.428(3) . ? O5A C8A 1.421(3) . ? O5A C9A 1.422(3) . ? O6A C11A 1.415(3) . ? O6A C10A 1.422(3) . ? C1A C2A 1.500(3) . ? C3A C4A 1.491(3) . ? C5A C6A 1.495(3) . ? C7A C8A 1.490(3) . ? C9A C10A 1.494(4) . ? C11A C12A 1.491(3) . ? 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 Cl1 O5 110.25(17) . . ? O3 Cl1 O2 110.10(16) . . ? O5 Cl1 O2 108.60(15) . . ? O3 Cl1 O4 108.99(12) . . ? O5 Cl1 O4 109.73(12) . . ? O2 Cl1 O4 109.16(12) . . ? O1 Na1 O2 163.25(8) . . ? O1 Na1 O2A 111.40(7) . . ? O2 Na1 O2A 85.12(7) . . ? O1 Na1 O1A 93.74(6) . . ? O2 Na1 O1A 91.00(8) . . ? O2A Na1 O1A 64.35(5) . . ? O1 Na1 O3A 90.05(7) . . ? O2 Na1 O3A 100.16(7) . . ? O2A Na1 O3A 64.10(5) . . ? O1A Na1 O3A 125.83(6) . . ? O1 Na1 O4A 82.17(6) . . ? O2 Na1 O4A 90.98(7) . . ? O2A Na1 O4A 123.84(5) . . ? O1A Na1 O4A 171.73(6) . . ? O3A Na1 O4A 61.60(5) . . ? O1 Na1 O6A 75.54(6) . . ? O2 Na1 O6A 92.69(6) . . ? O2A Na1 O6A 126.08(5) . . ? O1A Na1 O6A 61.83(5) . . ? O3A Na1 O6A 164.58(6) . . ? O4A Na1 O6A 110.05(5) . . ? Cl1 O2 Na1 128.26(13) . . ? C1A O1A C12A 112.60(15) . . ? C1A O1A Na1 109.71(11) . . ? C12A O1A Na1 117.38(11) . . ? C2A O2A C3A 112.46(15) . . ? C2A O2A Na1 116.03(11) . . ? C3A O2A Na1 112.24(12) . . ? C5A O3A C4A 110.86(15) . . ? C5A O3A Na1 115.39(11) . . ? C4A O3A Na1 114.10(12) . . ? C6A O4A C7A 110.72(17) . . ? C6A O4A Na1 113.46(12) . . ? C7A O4A Na1 125.16(12) . . ? C8A O5A C9A 111.43(18) . . ? C11A O6A C10A 112.78(17) . . ? C11A O6A Na1 107.94(11) . . ? C10A O6A Na1 121.48(13) . . ? O1A C1A C2A 107.54(17) . . ? O2A C2A C1A 107.14(15) . . ? O2A C3A C4A 107.15(16) . . ? O3A C4A C3A 107.82(16) . . ? O3A C5A C6A 109.34(17) . . ? O4A C6A C5A 108.61(17) . . ? O4A C7A C8A 108.35(17) . . ? O5A C8A C7A 108.74(17) . . ? O5A C9A C10A 108.39(19) . . ? O6A C10A C9A 108.59(18) . . ? O6A C11A C12A 108.82(17) . . ? O1A C12A C11A 108.38(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Cl1 O2 Na1 -76.9(2) . . . . ? O5 Cl1 O2 Na1 43.9(2) . . . . ? O4 Cl1 O2 Na1 163.50(16) . . . . ? O1 Na1 O2 Cl1 -19.6(4) . . . . ? O2A Na1 O2 Cl1 151.1(2) . . . . ? O1A Na1 O2 Cl1 86.9(2) . . . . ? O3A Na1 O2 Cl1 -146.34(19) . . . . ? O4A Na1 O2 Cl1 -85.03(19) . . . . ? O6A Na1 O2 Cl1 25.1(2) . . . . ? O1 Na1 O1A C1A -139.38(12) . . . . ? O2 Na1 O1A C1A 56.70(12) . . . . ? O2A Na1 O1A C1A -27.40(11) . . . . ? O3A Na1 O1A C1A -46.60(14) . . . . ? O4A Na1 O1A C1A 160.5(4) . . . . ? O6A Na1 O1A C1A 149.22(12) . . . . ? O1 Na1 O1A C12A 90.44(15) . . . . ? O2 Na1 O1A C12A -73.48(14) . . . . ? O2A Na1 O1A C12A -157.58(14) . . . . ? O3A Na1 O1A C12A -176.78(13) . . . . ? O4A Na1 O1A C12A 30.4(4) . . . . ? O6A Na1 O1A C12A 19.04(13) . . . . ? O1 Na1 O2A C2A 76.38(14) . . . . ? O2 Na1 O2A C2A -100.75(14) . . . . ? O1A Na1 O2A C2A -7.28(12) . . . . ? O3A Na1 O2A C2A 155.47(14) . . . . ? O4A Na1 O2A C2A 171.35(12) . . . . ? O6A Na1 O2A C2A -10.97(15) . . . . ? O1 Na1 O2A C3A -54.84(14) . . . . ? O2 Na1 O2A C3A 128.03(14) . . . . ? O1A Na1 O2A C3A -138.50(14) . . . . ? O3A Na1 O2A C3A 24.25(12) . . . . ? O4A Na1 O2A C3A 40.13(15) . . . . ? O6A Na1 O2A C3A -142.19(12) . . . . ? O1 Na1 O3A C5A -105.20(15) . . . . ? O2 Na1 O3A C5A 61.45(16) . . . . ? O2A Na1 O3A C5A 140.90(15) . . . . ? O1A Na1 O3A C5A 160.14(14) . . . . ? O4A Na1 O3A C5A -24.13(14) . . . . ? O6A Na1 O3A C5A -84.5(2) . . . . ? O1 Na1 O3A C4A 124.71(13) . . . . ? O2 Na1 O3A C4A -68.65(14) . . . . ? O2A Na1 O3A C4A 10.81(12) . . . . ? O1A Na1 O3A C4A 30.05(15) . . . . ? O4A Na1 O3A C4A -154.23(13) . . . . ? O6A Na1 O3A C4A 145.4(2) . . . . ? O1 Na1 O4A C6A 84.59(15) . . . . ? O2 Na1 O4A C6A -110.76(14) . . . . ? O2A Na1 O4A C6A -25.98(16) . . . . ? O1A Na1 O4A C6A 145.4(4) . . . . ? O3A Na1 O4A C6A -9.74(13) . . . . ? O6A Na1 O4A C6A 156.02(13) . . . . ? O1 Na1 O4A C7A -56.45(16) . . . . ? O2 Na1 O4A C7A 108.21(16) . . . . ? O2A Na1 O4A C7A -167.01(15) . . . . ? O1A Na1 O4A C7A 4.4(5) . . . . ? O3A Na1 O4A C7A -150.77(17) . . . . ? O6A Na1 O4A C7A 14.98(17) . . . . ? O1 Na1 O6A C11A -85.77(14) . . . . ? O2 Na1 O6A C11A 106.31(14) . . . . ? O2A Na1 O6A C11A 20.39(15) . . . . ? O1A Na1 O6A C11A 16.62(12) . . . . ? O3A Na1 O6A C11A -107.1(2) . . . . ? O4A Na1 O6A C11A -161.66(13) . . . . ? O1 Na1 O6A C10A 46.72(16) . . . . ? O2 Na1 O6A C10A -121.20(16) . . . . ? O2A Na1 O6A C10A 152.88(14) . . . . ? O1A Na1 O6A C10A 149.11(16) . . . . ? O3A Na1 O6A C10A 25.3(3) . . . . ? O4A Na1 O6A C10A -29.17(16) . . . . ? C12A O1A C1A C2A -168.50(15) . . . . ? Na1 O1A C1A C2A 58.79(15) . . . . ? C3A O2A C2A C1A 169.76(17) . . . . ? Na1 O2A C2A C1A 38.64(19) . . . . ? O1A C1A C2A O2A -65.17(19) . . . . ? C2A O2A C3A C4A 171.05(17) . . . . ? Na1 O2A C3A C4A -55.96(18) . . . . ? C5A O3A C4A C3A -174.88(17) . . . . ? Na1 O3A C4A C3A -42.57(18) . . . . ? O2A C3A C4A O3A 65.5(2) . . . . ? C4A O3A C5A C6A -172.60(17) . . . . ? Na1 O3A C5A C6A 55.8(2) . . . . ? C7A O4A C6A C5A -173.76(18) . . . . ? Na1 O4A C6A C5A 39.6(2) . . . . ? O3A C5A C6A O4A -63.1(2) . . . . ? C6A O4A C7A C8A -178.65(17) . . . . ? Na1 O4A C7A C8A -36.7(2) . . . . ? C9A O5A C8A C7A 177.89(18) . . . . ? O4A C7A C8A O5A 67.4(2) . . . . ? C8A O5A C9A C10A 166.66(18) . . . . ? C11A O6A C10A C9A -177.28(17) . . . . ? Na1 O6A C10A C9A 52.3(2) . . . . ? O5A C9A C10A O6A -66.9(2) . . . . ? C10A O6A C11A C12A 174.56(17) . . . . ? Na1 O6A C11A C12A -48.45(17) . . . . ? C1A O1A C12A C11A 178.51(16) . . . . ? Na1 O1A C12A C11A -52.66(19) . . . . ? O6A C11A C12A O1A 68.72(19) . . . . ? 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 H2 O5A 0.80(5) 2.16(5) 2.919(3) 157(4) . O1 H1 O4 0.84(5) 2.26(5) 3.098(3) 176(4) 4_455 O1 H1 O3 0.84(5) 2.58(4) 3.126(3) 124(3) 4_455 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.217 _refine_diff_density_min -0.218 _refine_diff_density_rms 0.033 #===END data_nano318 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H26 N Na O10' _chemical_formula_weight 367.33 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' 'N' 'N' 0.0061 0.0033 '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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.0590(4) _cell_length_b 10.5053(3) _cell_length_c 14.0593(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.295(2) _cell_angle_gamma 90.00 _cell_volume 1733.35(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.70 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.142 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.8950 _exptl_absorpt_correction_T_max 0.9454 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '2o phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 14177 _diffrn_reflns_av_R_equivalents 0.0163 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3381 _reflns_number_gt 2923 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics RES2INS _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+0.4818P] 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 SHELXL _refine_ls_extinction_coef 0.018(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3381 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0837 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na1 Na 0.50326(4) 0.77328(5) 0.20195(4) 0.03170(16) Uani 1 1 d . . . O1 O 0.30895(9) 0.85955(10) 0.13895(7) 0.0414(3) Uani 1 1 d . . . O2 O 0.35010(9) 0.70554(10) 0.05200(8) 0.0421(3) Uani 1 1 d . . . O3 O 0.18516(8) 0.79905(10) 0.00995(7) 0.0382(2) Uani 1 1 d . . . O4 O 0.64557(9) 0.84275(11) 0.33442(8) 0.0372(3) Uani 1 1 d . . . H42 H 0.611(2) 0.905(3) 0.3388(18) 0.090(9) Uiso 1 1 d . . . H41 H 0.6601(17) 0.8068(19) 0.3934(16) 0.060(6) Uiso 1 1 d . . . N1 N 0.28142(9) 0.78805(10) 0.06628(7) 0.0275(2) Uani 1 1 d . . . O1A O 0.59239(8) 0.97291(9) 0.13734(7) 0.0332(2) Uani 1 1 d . . . O2A O 0.64659(8) 0.72733(10) 0.09546(7) 0.0362(2) Uani 1 1 d . . . O3A O 0.57336(7) 0.55181(8) 0.22078(6) 0.0290(2) Uani 1 1 d . . . O4A O 0.41209(8) 0.63963(8) 0.31807(6) 0.0293(2) Uani 1 1 d . . . O5A O 0.40164(8) 0.90732(9) 0.37117(7) 0.0356(2) Uani 1 1 d . . . O6A O 0.51972(8) 1.10136(10) 0.28877(7) 0.0376(2) Uani 1 1 d . . . C1A C 0.68509(12) 0.94950(15) 0.09254(10) 0.0364(3) Uani 1 1 d . . . H1A2 H 0.7446 1.0153 0.1130 0.044 Uiso 1 1 calc R . . H1A1 H 0.6583 0.9531 0.0205 0.044 Uiso 1 1 calc R . . C2A C 0.73324(11) 0.82079(15) 0.12290(10) 0.0367(3) Uani 1 1 d . . . H2A2 H 0.7967 0.8023 0.0911 0.044 Uiso 1 1 calc R . . H2A1 H 0.7636 0.8188 0.1946 0.044 Uiso 1 1 calc R . . C3A C 0.69029(13) 0.60039(15) 0.11287(11) 0.0401(3) Uani 1 1 d . . . H3A2 H 0.7554 0.5996 0.1704 0.048 Uiso 1 1 calc R . . H3A1 H 0.7175 0.5700 0.0556 0.048 Uiso 1 1 calc R . . C4A C 0.59857(12) 0.51460(14) 0.13056(10) 0.0365(3) Uani 1 1 d . . . H4A2 H 0.5298 0.5224 0.0767 0.044 Uiso 1 1 calc R . . H4A1 H 0.6245 0.4250 0.1341 0.044 Uiso 1 1 calc R . . C5A C 0.49360(11) 0.46882(13) 0.24900(10) 0.0334(3) Uani 1 1 d . . . H5A2 H 0.5263 0.3822 0.2608 0.040 Uiso 1 1 calc R . . H5A1 H 0.4234 0.4638 0.1963 0.040 Uiso 1 1 calc R . . C6A C 0.46616(12) 0.51929(12) 0.34015(10) 0.0325(3) Uani 1 1 d . . . H6A2 H 0.4148 0.4598 0.3638 0.039 Uiso 1 1 calc R . . H6A1 H 0.5368 0.5289 0.3919 0.039 Uiso 1 1 calc R . . C7A C 0.37296(12) 0.68751(13) 0.39902(10) 0.0337(3) Uani 1 1 d . . . H7A2 H 0.4379 0.6970 0.4562 0.040 Uiso 1 1 calc R . . H7A1 H 0.3178 0.6273 0.4166 0.040 Uiso 1 1 calc R . . C8A C 0.31716(12) 0.81392(13) 0.37256(10) 0.0339(3) Uani 1 1 d . . . H8A2 H 0.2642 0.8087 0.3074 0.041 Uiso 1 1 calc R . . H8A1 H 0.2727 0.8378 0.4209 0.041 Uiso 1 1 calc R . . C9A C 0.35171(12) 1.02928(13) 0.34627(12) 0.0390(3) Uani 1 1 d . . . H9A2 H 0.3035 1.0526 0.3919 0.047 Uiso 1 1 calc R . . H9A1 H 0.3031 1.0275 0.2792 0.047 Uiso 1 1 calc R . . C10A C 0.44561(14) 1.12527(14) 0.35257(12) 0.0433(4) Uani 1 1 d . . . H10B H 0.4110 1.2105 0.3375 0.052 Uiso 1 1 calc R . . H10A H 0.4916 1.1274 0.4206 0.052 Uiso 1 1 calc R . . C11A C 0.46787(12) 1.11882(13) 0.18733(11) 0.0364(3) Uani 1 1 d . . . H11B H 0.4342 1.2050 0.1763 0.044 Uiso 1 1 calc R . . H11A H 0.4064 1.0555 0.1659 0.044 Uiso 1 1 calc R . . C12A C 0.55754(12) 1.10240(13) 0.13016(10) 0.0364(3) Uani 1 1 d . . . H12B H 0.5265 1.1255 0.0609 0.044 Uiso 1 1 calc R . . H12A H 0.6234 1.1584 0.1568 0.044 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.0287(3) 0.0331(3) 0.0312(3) 0.0005(2) 0.0025(2) -0.0005(2) O1 0.0459(6) 0.0387(6) 0.0341(5) -0.0109(4) -0.0019(4) -0.0034(5) O2 0.0352(5) 0.0480(6) 0.0420(6) -0.0075(5) 0.0071(4) 0.0077(5) O3 0.0305(5) 0.0488(6) 0.0309(5) -0.0027(4) -0.0023(4) 0.0026(4) O4 0.0377(6) 0.0385(6) 0.0321(5) 0.0042(4) 0.0010(4) -0.0012(5) N1 0.0289(6) 0.0286(5) 0.0248(5) 0.0022(4) 0.0056(4) -0.0033(4) O1A 0.0340(5) 0.0323(5) 0.0359(5) 0.0054(4) 0.0130(4) -0.0010(4) O2A 0.0310(5) 0.0406(6) 0.0364(5) 0.0037(4) 0.0069(4) 0.0018(4) O3A 0.0299(5) 0.0302(5) 0.0279(5) -0.0056(4) 0.0089(4) -0.0029(4) O4A 0.0342(5) 0.0262(4) 0.0298(5) -0.0002(4) 0.0118(4) 0.0014(4) O5A 0.0326(5) 0.0293(5) 0.0442(6) -0.0052(4) 0.0077(4) 0.0012(4) O6A 0.0355(5) 0.0382(5) 0.0380(5) -0.0059(4) 0.0064(4) -0.0014(4) C1A 0.0323(7) 0.0496(8) 0.0289(7) 0.0022(6) 0.0103(5) -0.0098(6) C2A 0.0284(7) 0.0530(9) 0.0299(7) -0.0010(6) 0.0096(5) -0.0011(6) C3A 0.0432(8) 0.0444(8) 0.0377(8) 0.0033(6) 0.0196(6) 0.0113(7) C4A 0.0445(8) 0.0375(7) 0.0280(7) -0.0074(6) 0.0091(6) 0.0055(6) C5A 0.0306(7) 0.0249(6) 0.0457(8) -0.0042(6) 0.0107(6) -0.0036(5) C6A 0.0339(7) 0.0258(6) 0.0400(7) 0.0052(5) 0.0130(6) 0.0002(5) C7A 0.0392(7) 0.0359(7) 0.0294(7) -0.0013(5) 0.0146(6) -0.0015(6) C8A 0.0338(7) 0.0356(7) 0.0356(7) -0.0055(6) 0.0147(6) -0.0018(6) C9A 0.0376(8) 0.0309(7) 0.0498(8) -0.0064(6) 0.0129(6) 0.0036(6) C10A 0.0488(9) 0.0335(7) 0.0501(9) -0.0119(6) 0.0164(7) -0.0029(7) C11A 0.0349(7) 0.0278(7) 0.0421(8) -0.0011(6) 0.0000(6) -0.0005(6) C12A 0.0392(7) 0.0310(7) 0.0357(7) 0.0073(6) 0.0019(6) -0.0050(6) _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 Na1 O4 2.3402(11) . ? Na1 O3A 2.4688(10) . ? Na1 O1 2.4782(12) . ? Na1 O2 2.5634(11) . ? Na1 O2A 2.5792(11) . ? Na1 O4A 2.5828(10) . ? Na1 O1A 2.6130(10) . ? Na1 N1 2.9107(12) . ? O1 N1 1.2499(14) . ? O2 N1 1.2467(15) . ? O3 N1 1.2511(14) . ? O1A C12A 1.4206(17) . ? O1A C1A 1.4250(16) . ? O2A C2A 1.4210(17) . ? O2A C3A 1.4340(18) . ? O3A C5A 1.4207(16) . ? O3A C4A 1.4253(15) . ? O4A C7A 1.4205(16) . ? O4A C6A 1.4237(15) . ? O5A C8A 1.4178(17) . ? O5A C9A 1.4247(17) . ? O6A C10A 1.4267(18) . ? O6A C11A 1.4312(17) . ? C1A C2A 1.494(2) . ? C3A C4A 1.491(2) . ? C5A C6A 1.4925(19) . ? C7A C8A 1.496(2) . ? C9A C10A 1.504(2) . ? C11A C12A 1.498(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 Na1 O3A 92.19(4) . . ? O4 Na1 O1 129.08(4) . . ? O3A Na1 O1 130.94(4) . . ? O4 Na1 O2 177.31(4) . . ? O3A Na1 O2 89.47(3) . . ? O1 Na1 O2 50.54(3) . . ? O4 Na1 O2A 93.08(4) . . ? O3A Na1 O2A 68.11(3) . . ? O1 Na1 O2A 124.45(4) . . ? O2 Na1 O2A 85.58(4) . . ? O4 Na1 O4A 90.42(4) . . ? O3A Na1 O4A 66.73(3) . . ? O1 Na1 O4A 85.40(4) . . ? O2 Na1 O4A 92.18(4) . . ? O2A Na1 O4A 134.80(4) . . ? O4 Na1 O1A 75.01(4) . . ? O3A Na1 O1A 129.46(4) . . ? O1 Na1 O1A 90.74(4) . . ? O2 Na1 O1A 102.30(4) . . ? O2A Na1 O1A 64.17(3) . . ? O4A Na1 O1A 157.66(4) . . ? O4 Na1 N1 154.18(4) . . ? O3A Na1 N1 111.16(3) . . ? O1 Na1 N1 25.22(3) . . ? O2 Na1 N1 25.32(3) . . ? O2A Na1 N1 105.50(3) . . ? O4A Na1 N1 89.00(3) . . ? O1A Na1 N1 96.83(3) . . ? N1 O1 Na1 97.13(8) . . ? N1 O2 Na1 93.11(7) . . ? O2 N1 O1 119.21(11) . . ? O2 N1 O3 121.09(11) . . ? O1 N1 O3 119.70(11) . . ? O2 N1 Na1 61.57(6) . . ? O1 N1 Na1 57.65(6) . . ? O3 N1 Na1 177.32(9) . . ? C12A O1A C1A 112.53(10) . . ? C12A O1A Na1 130.90(8) . . ? C1A O1A Na1 116.25(8) . . ? C2A O2A C3A 112.19(11) . . ? C2A O2A Na1 105.20(8) . . ? C3A O2A Na1 110.12(8) . . ? C5A O3A C4A 112.14(10) . . ? C5A O3A Na1 111.79(7) . . ? C4A O3A Na1 107.51(8) . . ? C7A O4A C6A 111.08(10) . . ? C7A O4A Na1 125.59(8) . . ? C6A O4A Na1 112.35(7) . . ? C8A O5A C9A 111.18(10) . . ? C10A O6A C11A 114.25(11) . . ? O1A C1A C2A 108.82(11) . . ? O2A C2A C1A 109.54(11) . . ? O2A C3A C4A 109.45(11) . . ? O3A C4A C3A 107.50(11) . . ? O3A C5A C6A 108.65(10) . . ? O4A C6A C5A 108.01(11) . . ? O4A C7A C8A 109.16(11) . . ? O5A C8A C7A 109.52(11) . . ? O5A C9A C10A 108.58(12) . . ? O6A C10A C9A 114.65(12) . . ? O6A C11A C12A 108.42(11) . . ? O1A C12A C11A 108.08(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Na1 O1 N1 175.75(7) . . . . ? O3A Na1 O1 N1 -43.92(9) . . . . ? O2 Na1 O1 N1 -0.81(7) . . . . ? O2A Na1 O1 N1 45.88(9) . . . . ? O4A Na1 O1 N1 -97.45(8) . . . . ? O1A Na1 O1 N1 104.58(8) . . . . ? O4 Na1 O2 N1 -82.1(10) . . . . ? O3A Na1 O2 N1 149.73(8) . . . . ? O1 Na1 O2 N1 0.81(7) . . . . ? O2A Na1 O2 N1 -142.19(8) . . . . ? O4A Na1 O2 N1 83.03(8) . . . . ? O1A Na1 O2 N1 -79.85(8) . . . . ? Na1 O2 N1 O1 -1.42(12) . . . . ? Na1 O2 N1 O3 179.61(10) . . . . ? Na1 O1 N1 O2 1.48(12) . . . . ? Na1 O1 N1 O3 -179.54(10) . . . . ? O4 Na1 N1 O2 173.88(10) . . . . ? O3A Na1 N1 O2 -32.72(8) . . . . ? O1 Na1 N1 O2 -178.53(12) . . . . ? O2A Na1 N1 O2 39.37(8) . . . . ? O4A Na1 N1 O2 -97.23(8) . . . . ? O1A Na1 N1 O2 104.40(8) . . . . ? O4 Na1 N1 O1 -7.59(13) . . . . ? O3A Na1 N1 O1 145.81(8) . . . . ? O2 Na1 N1 O1 178.53(12) . . . . ? O2A Na1 N1 O1 -142.10(8) . . . . ? O4A Na1 N1 O1 81.31(8) . . . . ? O1A Na1 N1 O1 -77.07(8) . . . . ? O4 Na1 N1 O3 1.1(19) . . . . ? O3A Na1 N1 O3 154.5(19) . . . . ? O1 Na1 N1 O3 8.7(19) . . . . ? O2 Na1 N1 O3 -172.8(19) . . . . ? O2A Na1 N1 O3 -133.4(19) . . . . ? O4A Na1 N1 O3 90.0(19) . . . . ? O1A Na1 N1 O3 -68.4(19) . . . . ? O4 Na1 O1A C12A -96.14(11) . . . . ? O3A Na1 O1A C12A -176.40(10) . . . . ? O1 Na1 O1A C12A 34.35(11) . . . . ? O2 Na1 O1A C12A 83.98(11) . . . . ? O2A Na1 O1A C12A 162.83(11) . . . . ? O4A Na1 O1A C12A -45.31(15) . . . . ? N1 Na1 O1A C12A 58.89(11) . . . . ? O4 Na1 O1A C1A 90.91(9) . . . . ? O3A Na1 O1A C1A 10.65(10) . . . . ? O1 Na1 O1A C1A -138.61(8) . . . . ? O2 Na1 O1A C1A -88.98(9) . . . . ? O2A Na1 O1A C1A -10.12(8) . . . . ? O4A Na1 O1A C1A 141.74(10) . . . . ? N1 Na1 O1A C1A -114.07(8) . . . . ? O4 Na1 O2A C2A -33.40(8) . . . . ? O3A Na1 O2A C2A -124.52(8) . . . . ? O1 Na1 O2A C2A 109.97(8) . . . . ? O2 Na1 O2A C2A 144.27(8) . . . . ? O4A Na1 O2A C2A -127.05(8) . . . . ? O1A Na1 O2A C2A 38.32(8) . . . . ? N1 Na1 O2A C2A 128.48(8) . . . . ? O4 Na1 O2A C3A 87.69(9) . . . . ? O3A Na1 O2A C3A -3.43(8) . . . . ? O1 Na1 O2A C3A -128.94(9) . . . . ? O2 Na1 O2A C3A -94.64(9) . . . . ? O4A Na1 O2A C3A -5.96(11) . . . . ? O1A Na1 O2A C3A 159.40(9) . . . . ? N1 Na1 O2A C3A -110.43(9) . . . . ? O4 Na1 O3A C5A 113.81(8) . . . . ? O1 Na1 O3A C5A -36.46(10) . . . . ? O2 Na1 O3A C5A -68.30(8) . . . . ? O2A Na1 O3A C5A -153.75(8) . . . . ? O4A Na1 O3A C5A 24.30(8) . . . . ? O1A Na1 O3A C5A -173.87(8) . . . . ? N1 Na1 O3A C5A -54.94(8) . . . . ? O4 Na1 O3A C4A -122.70(8) . . . . ? O1 Na1 O3A C4A 87.03(9) . . . . ? O2 Na1 O3A C4A 55.18(8) . . . . ? O2A Na1 O3A C4A -30.27(8) . . . . ? O4A Na1 O3A C4A 147.78(8) . . . . ? O1A Na1 O3A C4A -50.39(9) . . . . ? N1 Na1 O3A C4A 68.55(8) . . . . ? O4 Na1 O4A C7A 57.70(10) . . . . ? O3A Na1 O4A C7A 149.91(10) . . . . ? O1 Na1 O4A C7A -71.49(10) . . . . ? O2 Na1 O4A C7A -121.61(10) . . . . ? O2A Na1 O4A C7A 152.46(9) . . . . ? O1A Na1 O4A C7A 9.21(15) . . . . ? N1 Na1 O4A C7A -96.48(10) . . . . ? O4 Na1 O4A C6A -82.88(8) . . . . ? O3A Na1 O4A C6A 9.33(8) . . . . ? O1 Na1 O4A C6A 147.93(8) . . . . ? O2 Na1 O4A C6A 97.81(8) . . . . ? O2A Na1 O4A C6A 11.88(10) . . . . ? O1A Na1 O4A C6A -131.37(10) . . . . ? N1 Na1 O4A C6A 122.94(8) . . . . ? C12A O1A C1A C2A 167.11(11) . . . . ? Na1 O1A C1A C2A -18.65(13) . . . . ? C3A O2A C2A C1A 173.56(11) . . . . ? Na1 O2A C2A C1A -66.72(11) . . . . ? O1A C1A C2A O2A 58.11(14) . . . . ? C2A O2A C3A C4A 152.41(11) . . . . ? Na1 O2A C3A C4A 35.60(13) . . . . ? C5A O3A C4A C3A -174.88(11) . . . . ? Na1 O3A C4A C3A 61.85(11) . . . . ? O2A C3A C4A O3A -67.20(14) . . . . ? C4A O3A C5A C6A -176.24(11) . . . . ? Na1 O3A C5A C6A -55.41(12) . . . . ? C7A O4A C6A C5A 174.00(11) . . . . ? Na1 O4A C6A C5A -39.59(12) . . . . ? O3A C5A C6A O4A 63.71(13) . . . . ? C6A O4A C7A C8A 179.85(11) . . . . ? Na1 O4A C7A C8A 38.86(14) . . . . ? C9A O5A C8A C7A -179.96(11) . . . . ? O4A C7A C8A O5A -73.84(14) . . . . ? C8A O5A C9A C10A 176.28(12) . . . . ? C11A O6A C10A C9A 69.18(16) . . . . ? O5A C9A C10A O6A 60.27(17) . . . . ? C10A O6A C11A C12A 174.87(11) . . . . ? C1A O1A C12A C11A -174.73(11) . . . . ? Na1 O1A C12A C11A 12.10(15) . . . . ? O6A C11A C12A O1A 67.45(13) . . . . ? 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 O4 H42 O6A 0.79(3) 2.36(3) 3.1061(16) 157(2) . O4 H41 O3 0.89(2) 1.95(2) 2.8275(15) 170.1(18) 4_676 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.169 _refine_diff_density_min -0.202 _refine_diff_density_rms 0.034 #===END data_nareo418 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H27 Na O11 Re' _chemical_formula_weight 556.53 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' 'Re' 'Re' -1.0185 7.2310 '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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.9787(12) _cell_length_b 14.3770(6) _cell_length_c 16.9546(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.254(2) _cell_angle_gamma 90.00 _cell_volume 1924.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used n/a _cell_measurement_theta_min n/a _cell_measurement_theta_max n/a _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.921 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1092 _exptl_absorpt_coefficient_mu 6.386 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '2o phi frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 16756 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0799 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _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 3.73 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3648 _reflns_number_gt 3351 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement Denzo-SMN _computing_data_reduction Denzo-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics RES2INS _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^)+(0.1374P)^2^+1.5020P] 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 SHELXL _refine_ls_extinction_coef 0.0047(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3648 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0716 _refine_ls_R_factor_gt 0.0688 _refine_ls_wR_factor_ref 0.1831 _refine_ls_wR_factor_gt 0.1789 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 Re1 Re 0.45431(3) 1.197062(18) 0.353333(15) 0.0222(2) Uani 1 d . . . Na1 Na 0.1908(5) 1.1784(3) 0.1405(2) 0.0384(8) Uani 1 d . . . O1 O 0.0776(13) 1.0939(5) 0.0254(4) 0.073(3) Uani 1 d . . . O2 O 0.3736(8) 1.2159(4) 0.2544(3) 0.0371(13) Uani 1 d . . . O3 O 0.2929(8) 1.1796(5) 0.4089(4) 0.0476(16) Uani 1 d . . . O4 O 0.5837(7) 1.1015(4) 0.3600(3) 0.0353(12) Uani 1 d . . . O5 O 0.5712(8) 1.2935(4) 0.3890(4) 0.0329(14) Uani 1 d . . . O1A O 0.2006(7) 1.3398(4) 0.0601(3) 0.0312(12) Uani 1 d . . . O2A O -0.0169(7) 1.3134(3) 0.1706(4) 0.0280(12) Uani 1 d . . . O3A O -0.0509(6) 1.1346(3) 0.2254(3) 0.0254(10) Uani 1 d . . . O4A O 0.2011(6) 1.0074(3) 0.2113(3) 0.0282(10) Uani 1 d . . . O5A O 0.4418(6) 1.0370(4) 0.1058(3) 0.0313(11) Uani 1 d . . . O6A O 0.4801(7) 1.2225(4) 0.0598(3) 0.0294(11) Uani 1 d . . . C1A C 0.1081(10) 1.4147(5) 0.0876(5) 0.0351(17) Uani 1 d . . . H1A2 H 0.0861 1.4630 0.0458 0.042 Uiso 1 calc R . . H1A1 H 0.1739 1.4432 0.1355 0.042 Uiso 1 calc R . . C2A C -0.0560(9) 1.3769(5) 0.1074(5) 0.0307(15) Uani 1 d . . . H2A2 H -0.1271 1.4281 0.1235 0.037 Uiso 1 calc R . . H2A1 H -0.1191 1.3453 0.0604 0.037 Uiso 1 calc R . . C3A C -0.1620(10) 1.2871(5) 0.2065(5) 0.0277(15) Uani 1 d . . . H3A2 H -0.2524 1.2627 0.1656 0.033 Uiso 1 calc R . . H3A1 H -0.2070 1.3414 0.2327 0.033 Uiso 1 calc R . . C4A C -0.1046(10) 1.2137(5) 0.2665(5) 0.0284(15) Uani 1 d . . . H4A2 H -0.0096 1.2372 0.3054 0.034 Uiso 1 calc R . . H4A1 H -0.1985 1.1960 0.2958 0.034 Uiso 1 calc R . . C5A C -0.0286(10) 1.0552(5) 0.2751(4) 0.0294(15) Uani 1 d . . . H5A2 H -0.1380 1.0361 0.2912 0.035 Uiso 1 calc R . . H5A1 H 0.0519 1.0690 0.3238 0.035 Uiso 1 calc R . . C6A C 0.0396(9) 0.9792(5) 0.2283(4) 0.0299(15) Uani 1 d . . . H6A2 H 0.0498 0.9208 0.2595 0.036 Uiso 1 calc R . . H6A1 H -0.0378 0.9682 0.1781 0.036 Uiso 1 calc R . . C7A C 0.2879(10) 0.9344(5) 0.1776(4) 0.0308(15) Uani 1 d . . . H7A2 H 0.2248 0.9158 0.1254 0.037 Uiso 1 calc R . . H7A1 H 0.2979 0.8795 0.2132 0.037 Uiso 1 calc R . . C8A C 0.4605(9) 0.9697(5) 0.1674(4) 0.0308(15) Uani 1 d . . . H8A2 H 0.5160 0.9978 0.2177 0.037 Uiso 1 calc R . . H8A1 H 0.5320 0.9177 0.1533 0.037 Uiso 1 calc R . . C9A C 0.6004(9) 1.0746(6) 0.0945(6) 0.043(2) Uani 1 d . . . H9A2 H 0.6736 1.0252 0.0773 0.052 Uiso 1 calc R . . H9A1 H 0.6578 1.1015 0.1450 0.052 Uiso 1 calc R . . C10A C 0.5689(10) 1.1504(6) 0.0303(6) 0.041(2) Uani 1 d . . . H10B H 0.6782 1.1737 0.0169 0.049 Uiso 1 calc R . . H10A H 0.5027 1.1247 -0.0187 0.049 Uiso 1 calc R . . C11A C 0.4381(11) 1.2930(5) 0.0007(5) 0.0314(17) Uani 1 d . . . H11B H 0.3616 1.2671 -0.0452 0.038 Uiso 1 calc R . . H11A H 0.5422 1.3154 -0.0187 0.038 Uiso 1 calc R . . C12A C 0.3537(10) 1.3711(6) 0.0362(5) 0.0346(16) Uani 1 d . . . H12B H 0.4293 1.3958 0.0829 0.042 Uiso 1 calc R . . H12A H 0.3298 1.4218 -0.0033 0.042 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.0135(3) 0.0266(3) 0.0266(3) -0.00252(8) 0.00333(16) 0.00141(7) Na1 0.0302(19) 0.053(2) 0.0284(17) 0.0021(14) -0.0066(14) -0.0121(15) O1 0.137(8) 0.050(5) 0.027(3) 0.001(3) -0.007(4) -0.046(5) O2 0.042(3) 0.033(3) 0.032(3) 0.001(2) -0.008(2) -0.003(3) O3 0.023(3) 0.089(5) 0.033(3) -0.004(3) 0.011(3) 0.000(3) O4 0.022(3) 0.031(3) 0.053(3) 0.001(2) 0.007(2) 0.000(2) O5 0.030(3) 0.030(3) 0.035(3) -0.008(2) -0.009(3) 0.001(2) O1A 0.027(3) 0.032(3) 0.035(3) 0.004(2) 0.005(2) -0.003(2) O2A 0.012(3) 0.034(3) 0.037(3) 0.0036(19) 0.004(2) 0.0021(18) O3A 0.025(3) 0.016(2) 0.035(3) 0.0002(19) 0.006(2) 0.0035(18) O4A 0.023(2) 0.027(3) 0.034(2) -0.0038(19) 0.001(2) 0.0006(19) O5A 0.016(2) 0.030(3) 0.047(3) 0.000(2) 0.000(2) 0.0029(19) O6A 0.024(3) 0.034(3) 0.031(3) -0.002(2) 0.006(2) 0.000(2) C1A 0.029(4) 0.036(4) 0.039(4) 0.009(3) 0.003(3) 0.004(3) C2A 0.025(4) 0.025(4) 0.041(4) 0.002(3) 0.000(3) 0.007(3) C3A 0.014(3) 0.030(4) 0.038(4) -0.005(3) 0.002(3) -0.001(3) C4A 0.022(4) 0.030(3) 0.036(4) -0.007(3) 0.010(3) -0.002(3) C5A 0.029(4) 0.021(4) 0.037(4) 0.003(3) 0.002(3) 0.002(3) C6A 0.026(4) 0.020(3) 0.041(4) 0.002(3) -0.001(3) -0.003(3) C7A 0.032(4) 0.026(4) 0.034(4) 0.004(3) 0.004(3) 0.005(3) C8A 0.020(3) 0.028(4) 0.041(4) -0.004(3) -0.005(3) 0.010(3) C9A 0.013(3) 0.037(4) 0.079(6) -0.013(4) 0.007(4) -0.003(3) C10A 0.026(4) 0.038(5) 0.064(5) -0.015(4) 0.025(4) -0.009(3) C11A 0.018(4) 0.050(5) 0.026(4) 0.004(3) 0.002(3) -0.008(3) C12A 0.024(4) 0.040(4) 0.039(4) 0.010(3) 0.002(3) -0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 O4 1.712(6) . ? Re1 O3 1.720(6) . ? Re1 O5 1.731(5) . ? Re1 O2 1.730(6) . ? Na1 O2 2.310(7) . ? Na1 O1 2.365(7) . ? Na1 O3A 2.643(6) . ? Na1 O2A 2.650(7) . ? Na1 O1A 2.698(8) . ? Na1 O4A 2.732(6) . ? Na1 O6A 2.917(7) . ? Na1 O5A 2.970(7) . ? O1A C12A 1.415(9) . ? O1A C1A 1.421(10) . ? O2A C2A 1.408(9) . ? O2A C3A 1.435(9) . ? O3A C5A 1.416(8) . ? O3A C4A 1.432(8) . ? O4A C6A 1.419(9) . ? O4A C7A 1.422(8) . ? O5A C8A 1.416(9) . ? O5A C9A 1.414(9) . ? O6A C10A 1.389(9) . ? O6A C11A 1.431(9) . ? C1A C2A 1.499(11) . ? C3A C4A 1.492(11) . ? C5A C6A 1.497(10) . ? C7A C8A 1.501(11) . ? C9A C10A 1.536(13) . ? C11A C12A 1.481(12) . ? 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 Re1 O3 109.8(3) . . ? O4 Re1 O5 109.3(3) . . ? O3 Re1 O5 109.5(3) . . ? O4 Re1 O2 109.1(3) . . ? O3 Re1 O2 110.5(3) . . ? O5 Re1 O2 108.7(3) . . ? O2 Na1 O1 158.5(4) . . ? O2 Na1 O3A 91.3(2) . . ? O1 Na1 O3A 96.0(3) . . ? O2 Na1 O2A 90.3(2) . . ? O1 Na1 O2A 111.1(3) . . ? O3A Na1 O2A 62.89(18) . . ? O2 Na1 O1A 99.2(2) . . ? O1 Na1 O1A 93.4(2) . . ? O3A Na1 O1A 123.8(2) . . ? O2A Na1 O1A 62.0(2) . . ? O2 Na1 O4A 82.4(2) . . ? O1 Na1 O4A 83.4(2) . . ? O3A Na1 O4A 61.60(16) . . ? O2A Na1 O4A 123.7(2) . . ? O1A Na1 O4A 174.1(3) . . ? O2 Na1 O6A 83.9(2) . . ? O1 Na1 O6A 87.6(3) . . ? O3A Na1 O6A 174.7(2) . . ? O2A Na1 O6A 119.3(2) . . ? O1A Na1 O6A 59.58(19) . . ? O4A Na1 O6A 115.2(2) . . ? O2 Na1 O5A 87.9(2) . . ? O1 Na1 O5A 71.0(3) . . ? O3A Na1 O5A 120.7(2) . . ? O2A Na1 O5A 176.0(2) . . ? O1A Na1 O5A 114.8(2) . . ? O4A Na1 O5A 59.54(17) . . ? O6A Na1 O5A 56.96(17) . . ? Re1 O2 Na1 151.2(4) . . ? C12A O1A C1A 111.3(6) . . ? C12A O1A Na1 120.5(5) . . ? C1A O1A Na1 115.6(4) . . ? C2A O2A C3A 112.9(6) . . ? C2A O2A Na1 113.9(4) . . ? C3A O2A Na1 117.0(4) . . ? C5A O3A C4A 111.8(6) . . ? C5A O3A Na1 118.5(4) . . ? C4A O3A Na1 111.6(4) . . ? C6A O4A C7A 112.3(5) . . ? C6A O4A Na1 112.0(4) . . ? C7A O4A Na1 118.2(4) . . ? C8A O5A C9A 111.1(6) . . ? C8A O5A Na1 109.0(4) . . ? C9A O5A Na1 114.1(4) . . ? C10A O6A C11A 110.9(6) . . ? C10A O6A Na1 119.0(5) . . ? C11A O6A Na1 111.2(4) . . ? O1A C1A C2A 108.1(6) . . ? O2A C2A C1A 107.4(6) . . ? O2A C3A C4A 106.8(6) . . ? O3A C4A C3A 108.3(6) . . ? O3A C5A C6A 107.2(6) . . ? O4A C6A C5A 108.0(6) . . ? O4A C7A C8A 107.8(6) . . ? O5A C8A C7A 108.3(5) . . ? O5A C9A C10A 108.0(6) . . ? O6A C10A C9A 108.3(7) . . ? O6A C11A C12A 109.0(6) . . ? O1A C12A C11A 109.7(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Re1 O2 Na1 75.2(8) . . . . ? O3 Re1 O2 Na1 -45.6(9) . . . . ? O5 Re1 O2 Na1 -165.8(7) . . . . ? O1 Na1 O2 Re1 -73.5(12) . . . . ? O3A Na1 O2 Re1 36.7(8) . . . . ? O2A Na1 O2 Re1 99.5(8) . . . . ? O1A Na1 O2 Re1 161.2(7) . . . . ? O4A Na1 O2 Re1 -24.5(8) . . . . ? O6A Na1 O2 Re1 -141.0(8) . . . . ? O5A Na1 O2 Re1 -84.0(8) . . . . ? O2 Na1 O1A C12A 63.2(6) . . . . ? O1 Na1 O1A C12A -99.4(6) . . . . ? O3A Na1 O1A C12A 161.1(5) . . . . ? O2A Na1 O1A C12A 148.5(6) . . . . ? O4A Na1 O1A C12A -43(2) . . . . ? O6A Na1 O1A C12A -14.1(5) . . . . ? O5A Na1 O1A C12A -28.8(6) . . . . ? O2 Na1 O1A C1A -75.3(5) . . . . ? O1 Na1 O1A C1A 122.2(6) . . . . ? O3A Na1 O1A C1A 22.6(6) . . . . ? O2A Na1 O1A C1A 10.1(5) . . . . ? O4A Na1 O1A C1A 179(2) . . . . ? O6A Na1 O1A C1A -152.6(5) . . . . ? O5A Na1 O1A C1A -167.2(4) . . . . ? O2 Na1 O2A C2A 125.2(5) . . . . ? O1 Na1 O2A C2A -57.6(5) . . . . ? O3A Na1 O2A C2A -143.5(5) . . . . ? O1A Na1 O2A C2A 24.8(4) . . . . ? O4A Na1 O2A C2A -153.8(4) . . . . ? O6A Na1 O2A C2A 42.0(5) . . . . ? O5A Na1 O2A C2A 63(3) . . . . ? O2 Na1 O2A C3A -100.1(5) . . . . ? O1 Na1 O2A C3A 77.2(6) . . . . ? O3A Na1 O2A C3A -8.7(5) . . . . ? O1A Na1 O2A C3A 159.6(6) . . . . ? O4A Na1 O2A C3A -19.0(6) . . . . ? O6A Na1 O2A C3A 176.7(5) . . . . ? O5A Na1 O2A C3A -163(3) . . . . ? O2 Na1 O3A C5A -67.9(5) . . . . ? O1 Na1 O3A C5A 91.9(5) . . . . ? O2A Na1 O3A C5A -157.5(5) . . . . ? O1A Na1 O3A C5A -169.9(4) . . . . ? O4A Na1 O3A C5A 12.8(4) . . . . ? O6A Na1 O3A C5A -42(3) . . . . ? O5A Na1 O3A C5A 20.5(5) . . . . ? O2 Na1 O3A C4A 64.2(5) . . . . ? O1 Na1 O3A C4A -136.1(5) . . . . ? O2A Na1 O3A C4A -25.5(4) . . . . ? O1A Na1 O3A C4A -37.9(5) . . . . ? O4A Na1 O3A C4A 144.8(5) . . . . ? O6A Na1 O3A C4A 90(2) . . . . ? O5A Na1 O3A C4A 152.5(4) . . . . ? O2 Na1 O4A C6A 117.9(5) . . . . ? O1 Na1 O4A C6A -78.4(5) . . . . ? O3A Na1 O4A C6A 22.2(4) . . . . ? O2A Na1 O4A C6A 32.6(5) . . . . ? O1A Na1 O4A C6A -135(2) . . . . ? O6A Na1 O4A C6A -162.6(4) . . . . ? O5A Na1 O4A C6A -150.1(5) . . . . ? O2 Na1 O4A C7A -109.1(5) . . . . ? O1 Na1 O4A C7A 54.7(5) . . . . ? O3A Na1 O4A C7A 155.2(5) . . . . ? O2A Na1 O4A C7A 165.7(4) . . . . ? O1A Na1 O4A C7A -2(2) . . . . ? O6A Na1 O4A C7A -29.5(5) . . . . ? O5A Na1 O4A C7A -17.1(4) . . . . ? O2 Na1 O5A C8A 62.9(4) . . . . ? O1 Na1 O5A C8A -113.1(4) . . . . ? O3A Na1 O5A C8A -27.4(5) . . . . ? O2A Na1 O5A C8A 125(3) . . . . ? O1A Na1 O5A C8A 162.1(4) . . . . ? O4A Na1 O5A C8A -19.6(4) . . . . ? O6A Na1 O5A C8A 147.0(4) . . . . ? O2 Na1 O5A C9A -61.9(6) . . . . ? O1 Na1 O5A C9A 122.2(6) . . . . ? O3A Na1 O5A C9A -152.2(5) . . . . ? O2A Na1 O5A C9A 1(3) . . . . ? O1A Na1 O5A C9A 37.3(6) . . . . ? O4A Na1 O5A C9A -144.3(6) . . . . ? O6A Na1 O5A C9A 22.3(5) . . . . ? O2 Na1 O6A C10A 105.6(6) . . . . ? O1 Na1 O6A C10A -54.6(6) . . . . ? O3A Na1 O6A C10A 79(3) . . . . ? O2A Na1 O6A C10A -167.5(5) . . . . ? O1A Na1 O6A C10A -150.0(6) . . . . ? O4A Na1 O6A C10A 26.9(6) . . . . ? O5A Na1 O6A C10A 14.2(5) . . . . ? O2 Na1 O6A C11A -123.7(5) . . . . ? O1 Na1 O6A C11A 76.1(5) . . . . ? O3A Na1 O6A C11A -150(2) . . . . ? O2A Na1 O6A C11A -36.8(6) . . . . ? O1A Na1 O6A C11A -19.2(5) . . . . ? O4A Na1 O6A C11A 157.7(4) . . . . ? O5A Na1 O6A C11A 144.9(5) . . . . ? C12A O1A C1A C2A 176.9(6) . . . . ? Na1 O1A C1A C2A -40.9(7) . . . . ? C3A O2A C2A C1A 167.6(6) . . . . ? Na1 O2A C2A C1A -55.8(7) . . . . ? O1A C1A C2A O2A 63.6(8) . . . . ? C2A O2A C3A C4A 174.8(6) . . . . ? Na1 O2A C3A C4A 39.6(7) . . . . ? C5A O3A C4A C3A -167.5(6) . . . . ? Na1 O3A C4A C3A 57.2(6) . . . . ? O2A C3A C4A O3A -63.6(8) . . . . ? C4A O3A C5A C6A -175.8(6) . . . . ? Na1 O3A C5A C6A -43.8(7) . . . . ? C7A O4A C6A C5A 171.0(5) . . . . ? Na1 O4A C6A C5A -53.1(6) . . . . ? O3A C5A C6A O4A 63.7(7) . . . . ? C6A O4A C7A C8A -176.2(5) . . . . ? Na1 O4A C7A C8A 50.9(7) . . . . ? C9A O5A C8A C7A 178.7(6) . . . . ? Na1 O5A C8A C7A 52.2(6) . . . . ? O4A C7A C8A O5A -69.9(7) . . . . ? C8A O5A C9A C10A -177.0(6) . . . . ? Na1 O5A C9A C10A -53.4(7) . . . . ? C11A O6A C10A C9A -176.5(6) . . . . ? Na1 O6A C10A C9A -45.7(7) . . . . ? O5A C9A C10A O6A 65.5(8) . . . . ? C10A O6A C11A C12A -176.3(6) . . . . ? Na1 O6A C11A C12A 48.8(7) . . . . ? C1A O1A C12A C11A -174.5(6) . . . . ? Na1 O1A C12A C11A 45.4(8) . . . . ? O6A C11A C12A O1A -62.5(8) . . . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 4.334 _refine_diff_density_min -6.044 _refine_diff_density_rms 0.393 #===END data_nan318 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H28 N3 Na O8' _chemical_formula_weight 365.36 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' 'N' 'N' 0.0061 0.0033 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5186(8) _cell_length_b 10.4064(9) _cell_length_c 11.0250(6) _cell_angle_alpha 67.8250(10) _cell_angle_beta 76.1130(10) _cell_angle_gamma 67.5510(10) _cell_volume 928.78(12) _cell_formula_units_Z 2 _cell_measurement_temperature 123(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 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.306 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 392 _exptl_absorpt_coefficient_mu 0.127 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9392 _exptl_absorpt_correction_T_max 0.9750 _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _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 5761 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min -11 _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 3.24 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3388 _reflns_number_gt 1998 _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^)+(0.0644P)^2^+0.7419P] 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 SHELXL _refine_ls_extinction_coef 0.070(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3388 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0892 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1824 _refine_ls_wR_factor_gt 0.1611 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.002 _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 Na1 Na 0.51930(19) 1.0198(2) 0.45896(15) 0.0213(5) Uani 0.50 d P . . Na2 Na 0.9764(2) 0.4750(2) 0.05150(19) 0.0316(5) Uani 0.50 d P . . O1 O 0.6344(5) 1.1128(5) 0.5251(4) 0.0427(10) Uani 0.50 d P . . O2 O 0.8721(5) 0.3903(4) -0.0332(4) 0.0286(9) Uani 0.50 d P . . O11 O 0.5718(4) 1.0890(5) 0.6133(5) 0.0412(10) Uani 0.50 d P . . O12 O 0.9222(4) 0.4065(4) -0.1028(4) 0.0278(9) Uani 0.50 d P . . O1A O 0.52128(18) 1.23850(18) 0.27191(15) 0.0256(4) Uani 1 d . . . O2A O 0.72100(18) 0.95647(17) 0.28642(15) 0.0247(4) Uani 1 d . . . O3A O 0.73714(18) 0.73833(17) 0.54126(15) 0.0246(4) Uani 1 d . . . C1A C 0.5978(3) 1.1992(3) 0.1561(2) 0.0279(6) Uani 1 d . . . H1A2 H 0.6136 1.2862 0.0838 0.033 Uiso 1 calc R . . H1A1 H 0.5352 1.1612 0.1271 0.033 Uiso 1 calc R . . C2A C 0.7489(3) 1.0834(3) 0.1887(2) 0.0277(6) Uani 1 d . . . H2A2 H 0.8078 1.0590 0.1087 0.033 Uiso 1 calc R . . H2A1 H 0.8091 1.1195 0.2225 0.033 Uiso 1 calc R . . C3A C 0.8594(3) 0.8487(3) 0.3338(3) 0.0308(6) Uani 1 d . . . H3A2 H 0.9034 0.8858 0.3812 0.037 Uiso 1 calc R . . H3A1 H 0.9347 0.8271 0.2588 0.037 Uiso 1 calc R . . C4A C 0.8264(3) 0.7118(3) 0.4249(2) 0.0306(6) Uani 1 d . . . H4B H 0.7703 0.6819 0.3810 0.037 Uiso 1 calc R . . H4A H 0.9235 0.6312 0.4474 0.037 Uiso 1 calc R . . C5A C 0.6946(3) 0.6132(3) 0.6269(2) 0.0279(6) Uani 1 d . . . H5A2 H 0.7867 0.5251 0.6434 0.034 Uiso 1 calc R . . H5A1 H 0.6249 0.5961 0.5853 0.034 Uiso 1 calc R . . C6A C 0.6166(3) 0.6399(3) 0.7535(2) 0.0291(6) Uani 1 d . . . H6A2 H 0.5927 0.5515 0.8162 0.035 Uiso 1 calc R . . H6A1 H 0.6845 0.6616 0.7932 0.035 Uiso 1 calc R . . O1B O 0.77882(19) 0.54363(19) 0.21354(16) 0.0288(5) Uani 1 d . . . O2B O 0.97869(19) 0.26146(19) 0.22864(17) 0.0305(5) Uani 1 d . . . O3B O 1.2370(2) 0.23845(19) 0.04110(17) 0.0305(5) Uani 1 d . . . C1B C 0.7522(3) 0.4163(3) 0.3114(3) 0.0334(6) Uani 1 d . . . H1B2 H 0.6913 0.3803 0.2783 0.040 Uiso 1 calc R . . H1B1 H 0.6942 0.4404 0.3918 0.040 Uiso 1 calc R . . C2B C 0.9039(3) 0.3000(3) 0.3432(3) 0.0356(6) Uani 1 d . . . H2B2 H 0.9669 0.3376 0.3721 0.043 Uiso 1 calc R . . H2B1 H 0.8882 0.2129 0.4155 0.043 Uiso 1 calc R . . C3B C 1.1168(3) 0.1400(3) 0.2536(3) 0.0328(6) Uani 1 d . . . H3B2 H 1.0932 0.0514 0.3160 0.039 Uiso 1 calc R . . H3B1 H 1.1847 0.1615 0.2933 0.039 Uiso 1 calc R . . C4B C 1.1944(3) 0.1141(3) 0.1264(3) 0.0376(7) Uani 1 d . . . H4B2 H 1.2864 0.0258 0.1426 0.045 Uiso 1 calc R . . H4B1 H 1.1244 0.0973 0.0848 0.045 Uiso 1 calc R . . C5B C 1.3255(3) 0.2126(3) -0.0755(3) 0.0376(7) Uani 1 d . . . H5B2 H 1.2686 0.1838 -0.1196 0.045 Uiso 1 calc R . . H5B1 H 1.4222 0.1313 -0.0533 0.045 Uiso 1 calc R . . C6B C 1.3598(3) 0.3480(3) -0.1659(3) 0.0365(7) Uani 1 d . . . H6B2 H 1.4040 0.3848 -0.1183 0.044 Uiso 1 calc R . . H6B1 H 1.4351 0.3260 -0.2408 0.044 Uiso 1 calc R . . N1S N 1.2303(3) -0.2441(2) 0.1468(2) 0.0331(6) Uani 1 d . . . N2S N 1.2499(2) -0.2504(2) 0.2498(2) 0.0237(4) Uani 1 d . . . N3S N 1.2698(3) -0.2571(3) 0.3539(2) 0.0383(6) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.0236(10) 0.0278(11) 0.0183(11) -0.0096(9) 0.0002(8) -0.0137(8) Na2 0.0363(12) 0.0341(12) 0.0302(11) -0.0085(9) -0.0049(9) -0.0185(10) O1 0.055(3) 0.042(2) 0.039(2) -0.0006(19) -0.021(2) -0.026(2) O2 0.040(2) 0.026(2) 0.025(2) 0.0002(17) -0.0123(17) -0.0205(18) O11 0.031(2) 0.056(3) 0.047(3) -0.031(2) -0.0058(18) -0.010(2) O12 0.026(2) 0.042(2) 0.025(2) -0.0171(19) -0.0006(16) -0.0149(17) O1A 0.0253(9) 0.0231(9) 0.0250(9) -0.0069(7) -0.0051(7) -0.0035(7) O2A 0.0231(9) 0.0219(9) 0.0253(9) -0.0058(7) -0.0037(7) -0.0045(7) O3A 0.0271(9) 0.0192(9) 0.0290(9) -0.0111(7) -0.0028(7) -0.0058(7) C1A 0.0349(14) 0.0228(13) 0.0228(13) -0.0057(10) -0.0036(10) -0.0075(11) C2A 0.0285(13) 0.0260(13) 0.0262(13) -0.0079(10) 0.0008(10) -0.0088(11) C3A 0.0206(12) 0.0346(15) 0.0314(14) -0.0124(11) -0.0036(10) -0.0005(11) C4A 0.0305(13) 0.0250(13) 0.0295(13) -0.0128(10) -0.0048(10) 0.0029(11) C5A 0.0297(13) 0.0160(12) 0.0366(14) -0.0071(10) -0.0060(10) -0.0057(10) C6A 0.0251(13) 0.0207(13) 0.0345(14) -0.0014(10) -0.0077(10) -0.0046(10) O1B 0.0266(9) 0.0290(10) 0.0298(10) -0.0113(7) -0.0077(7) -0.0034(8) O2B 0.0258(9) 0.0242(9) 0.0375(11) -0.0045(8) -0.0075(7) -0.0069(8) O3B 0.0316(10) 0.0247(9) 0.0373(10) -0.0118(8) -0.0094(8) -0.0060(8) C1B 0.0343(14) 0.0343(15) 0.0325(15) -0.0113(11) -0.0051(11) -0.0106(12) C2B 0.0394(15) 0.0313(15) 0.0379(15) -0.0094(11) -0.0115(12) -0.0106(12) C3B 0.0303(14) 0.0206(13) 0.0440(16) -0.0009(11) -0.0127(11) -0.0086(11) C4B 0.0344(15) 0.0199(13) 0.0576(18) -0.0108(12) -0.0128(13) -0.0047(11) C5B 0.0346(15) 0.0292(14) 0.0448(16) -0.0167(12) -0.0120(12) 0.0036(12) C6B 0.0292(14) 0.0366(16) 0.0361(15) -0.0108(12) -0.0098(11) 0.0001(12) N1S 0.0467(14) 0.0345(13) 0.0260(12) -0.0128(9) -0.0015(10) -0.0199(11) N2S 0.0239(9) 0.0184(8) 0.0306(11) -0.0092(7) 0.0007(7) -0.0098(7) N3S 0.0581(16) 0.0346(13) 0.0318(13) -0.0112(10) -0.0122(11) -0.0202(12) _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 Na1 Na1 0.894(3) 2_676 ? Na1 O1 2.096(4) . ? Na1 O11 2.105(4) 2_676 ? Na1 O11 2.296(4) . ? Na1 O1 2.304(4) 2_676 ? Na1 O1A 2.430(2) . ? Na1 O2A 2.443(2) . ? Na1 O3A 2.757(2) 2_676 ? Na1 O3A 2.822(2) . ? Na2 Na2 1.118(4) 2_765 ? Na2 O2 2.090(4) . ? Na2 O12 2.115(4) 2_765 ? Na2 O2 2.298(4) 2_765 ? Na2 O12 2.298(4) . ? Na2 O2B 2.336(3) . ? Na2 O1B 2.359(3) . ? Na2 O3B 2.764(3) . ? Na2 O3B 2.852(3) 2_765 ? Na2 C2B 3.100(3) . ? O1 O11 1.007(5) . ? O1 Na1 2.304(4) 2_676 ? O2 O12 0.795(4) . ? O2 Na2 2.298(4) 2_765 ? O11 Na1 2.105(4) 2_676 ? O12 Na2 2.115(4) 2_765 ? O1A C6A 1.429(3) 2_676 ? O1A C1A 1.431(3) . ? O2A C3A 1.423(3) . ? O2A C2A 1.425(3) . ? O3A C4A 1.418(3) . ? O3A C5A 1.429(3) . ? O3A Na1 2.757(2) 2_676 ? C1A C2A 1.499(3) . ? C3A C4A 1.499(4) . ? C5A C6A 1.488(3) . ? C6A O1A 1.429(3) 2_676 ? O1B C1B 1.425(3) . ? O1B C6B 1.428(3) 2_765 ? O2B C2B 1.413(3) . ? O2B C3B 1.429(3) . ? O3B C5B 1.415(3) . ? O3B C4B 1.422(3) . ? O3B Na2 2.852(3) 2_765 ? C1B C2B 1.503(4) . ? C3B C4B 1.490(4) . ? C5B C6B 1.490(4) . ? C6B O1B 1.428(3) 2_765 ? N1S N2S 1.168(3) . ? N2S N3S 1.180(3) . ? 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 Na1 Na1 O1 91.8(2) 2_676 . ? Na1 Na1 O11 90.6(3) 2_676 2_676 ? O1 Na1 O11 173.52(18) . 2_676 ? Na1 Na1 O11 66.5(2) 2_676 . ? O1 Na1 O11 26.01(14) . . ? O11 Na1 O11 157.09(9) 2_676 . ? Na1 Na1 O1 65.4(2) 2_676 2_676 ? O1 Na1 O1 157.19(9) . 2_676 ? O11 Na1 O1 25.91(14) 2_676 2_676 ? O11 Na1 O1 131.50(15) . 2_676 ? Na1 Na1 O1A 148.5(3) 2_676 . ? O1 Na1 O1A 78.54(13) . . ? O11 Na1 O1A 102.31(15) 2_676 . ? O11 Na1 O1A 97.83(15) . . ? O1 Na1 O1A 120.74(13) 2_676 . ? Na1 Na1 O2A 141.5(3) 2_676 . ? O1 Na1 O2A 95.92(16) . . ? O11 Na1 O2A 78.49(13) 2_676 . ? O11 Na1 O2A 119.19(14) . . ? O1 Na1 O2A 102.11(15) 2_676 . ? O1A Na1 O2A 69.87(7) . . ? Na1 Na1 O3A 84.9(2) 2_676 2_676 ? O1 Na1 O3A 88.28(15) . 2_676 ? O11 Na1 O3A 97.91(12) 2_676 2_676 ? O11 Na1 O3A 80.76(12) . 2_676 ? O1 Na1 O3A 89.61(14) 2_676 2_676 ? O1A Na1 O3A 65.00(7) . 2_676 ? O2A Na1 O3A 132.80(8) . 2_676 ? Na1 Na1 O3A 76.7(2) 2_676 . ? O1 Na1 O3A 92.26(13) . . ? O11 Na1 O3A 82.46(13) 2_676 . ? O11 Na1 O3A 91.75(13) . . ? O1 Na1 O3A 82.80(13) 2_676 . ? O1A Na1 O3A 133.05(8) . . ? O2A Na1 O3A 65.43(6) . . ? O3A Na1 O3A 161.61(6) 2_676 . ? Na2 Na2 O2 85.9(2) 2_765 . ? Na2 Na2 O12 84.7(2) 2_765 2_765 ? O2 Na2 O12 169.10(16) . 2_765 ? Na2 Na2 O2 65.1(2) 2_765 2_765 ? O2 Na2 O2 150.96(11) . 2_765 ? O12 Na2 O2 20.22(11) 2_765 2_765 ? Na2 Na2 O12 66.4(2) 2_765 . ? O2 Na2 O12 20.17(11) . . ? O12 Na2 O12 151.02(11) 2_765 . ? O2 Na2 O12 131.19(14) 2_765 . ? Na2 Na2 O2B 147.4(3) 2_765 . ? O2 Na2 O2B 82.83(13) . . ? O12 Na2 O2B 108.07(14) 2_765 . ? O2 Na2 O2B 121.58(13) 2_765 . ? O12 Na2 O2B 97.16(14) . . ? Na2 Na2 O1B 139.4(3) 2_765 . ? O2 Na2 O1B 100.75(15) . . ? O12 Na2 O1B 83.13(13) 2_765 . ? O2 Na2 O1B 101.53(15) 2_765 . ? O12 Na2 O1B 118.66(14) . . ? O2B Na2 O1B 72.93(8) . . ? Na2 Na2 O3B 83.0(2) 2_765 . ? O2 Na2 O3B 87.14(14) . . ? O12 Na2 O3B 97.00(12) 2_765 . ? O2 Na2 O3B 89.18(13) 2_765 . ? O12 Na2 O3B 80.11(12) . . ? O2B Na2 O3B 66.08(8) . . ? O1B Na2 O3B 136.89(10) . . ? Na2 Na2 O3B 74.1(2) 2_765 2_765 ? O2 Na2 O3B 91.15(13) . 2_765 ? O12 Na2 O3B 81.10(12) 2_765 2_765 ? O2 Na2 O3B 81.30(12) 2_765 2_765 ? O12 Na2 O3B 90.53(12) . 2_765 ? O2B Na2 O3B 136.34(10) . 2_765 ? O1B Na2 O3B 65.81(7) . 2_765 ? O3B Na2 O3B 157.09(8) . 2_765 ? Na2 Na2 C2B 169.9(3) 2_765 . ? O2 Na2 C2B 97.38(14) . . ? O12 Na2 C2B 92.88(14) 2_765 . ? O2 Na2 C2B 111.25(13) 2_765 . ? O12 Na2 C2B 115.65(14) . . ? O2B Na2 C2B 25.52(7) . . ? O1B Na2 C2B 49.44(7) . . ? O3B Na2 C2B 87.66(8) . . ? O3B Na2 C2B 115.20(9) 2_765 . ? O11 O1 Na1 88.2(3) . . ? O11 O1 Na1 65.9(3) . 2_676 ? Na1 O1 Na1 22.81(9) . 2_676 ? O12 O2 Na2 94.9(4) . . ? O12 O2 Na2 66.8(4) . 2_765 ? Na2 O2 Na2 29.04(11) . 2_765 ? O1 O11 Na1 88.2(3) . 2_676 ? O1 O11 Na1 65.8(3) . . ? Na1 O11 Na1 22.91(9) 2_676 . ? O2 O12 Na2 93.0(4) . 2_765 ? O2 O12 Na2 64.9(3) . . ? Na2 O12 Na2 28.98(11) 2_765 . ? C6A O1A C1A 112.15(17) 2_676 . ? C6A O1A Na1 119.76(14) 2_676 . ? C1A O1A Na1 110.21(14) . . ? C3A O2A C2A 111.21(18) . . ? C3A O2A Na1 114.41(14) . . ? C2A O2A Na1 111.77(13) . . ? C4A O3A C5A 111.00(18) . . ? C4A O3A Na1 123.55(14) . 2_676 ? C5A O3A Na1 106.52(13) . 2_676 ? C4A O3A Na1 106.08(13) . . ? C5A O3A Na1 122.13(13) . . ? Na1 O3A Na1 18.39(6) 2_676 . ? O1A C1A C2A 108.14(18) . . ? O2A C2A C1A 108.36(19) . . ? O2A C3A C4A 109.1(2) . . ? O3A C4A C3A 109.4(2) . . ? O3A C5A C6A 108.97(19) . . ? O1A C6A C5A 108.73(19) 2_676 . ? C1B O1B C6B 111.82(19) . 2_765 ? C1B O1B Na2 109.86(15) . . ? C6B O1B Na2 115.88(15) 2_765 . ? C2B O2B C3B 112.10(19) . . ? C2B O2B Na2 109.04(16) . . ? C3B O2B Na2 120.67(15) . . ? C5B O3B C4B 111.3(2) . . ? C5B O3B Na2 125.47(15) . . ? C4B O3B Na2 104.44(15) . . ? C5B O3B Na2 103.69(14) . 2_765 ? C4B O3B Na2 123.81(15) . 2_765 ? Na2 O3B Na2 22.91(8) . 2_765 ? O1B C1B C2B 108.7(2) . . ? O2B C2B C1B 108.3(2) . . ? O2B C2B Na2 45.44(12) . . ? C1B C2B Na2 77.65(14) . . ? O2B C3B C4B 108.7(2) . . ? O3B C4B C3B 109.3(2) . . ? O3B C5B C6B 109.8(2) . . ? O1B C6B C5B 108.7(2) 2_765 . ? N1S N2S N3S 179.9(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Na1 Na1 O1 O11 -12.6(4) 2_676 . . . ? O11 Na1 O1 O11 -124.7(13) 2_676 . . . ? O1 Na1 O1 O11 -12.6(4) 2_676 . . . ? O1A Na1 O1 O11 137.1(4) . . . . ? O2A Na1 O1 O11 -154.9(4) . . . . ? O3A Na1 O1 O11 72.3(4) 2_676 . . . ? O3A Na1 O1 O11 -89.4(4) . . . . ? O11 Na1 O1 Na1 -112.1(15) 2_676 . . 2_676 ? O11 Na1 O1 Na1 12.6(4) . . . 2_676 ? O1 Na1 O1 Na1 0.0 2_676 . . 2_676 ? O1A Na1 O1 Na1 149.7(3) . . . 2_676 ? O2A Na1 O1 Na1 -142.3(3) . . . 2_676 ? O3A Na1 O1 Na1 84.9(2) 2_676 . . 2_676 ? O3A Na1 O1 Na1 -76.7(2) . . . 2_676 ? Na2 Na2 O2 O12 14.4(5) 2_765 . . . ? O12 Na2 O2 O12 44.0(12) 2_765 . . . ? O2 Na2 O2 O12 14.4(5) 2_765 . . . ? O2B Na2 O2 O12 -135.0(5) . . . . ? O1B Na2 O2 O12 154.0(4) . . . . ? O3B Na2 O2 O12 -68.7(4) . . . . ? O3B Na2 O2 O12 88.4(4) 2_765 . . . ? C2B Na2 O2 O12 -156.0(4) . . . . ? O12 Na2 O2 Na2 29.6(8) 2_765 . . 2_765 ? O2 Na2 O2 Na2 0.000(1) 2_765 . . 2_765 ? O12 Na2 O2 Na2 -14.4(5) . . . 2_765 ? O2B Na2 O2 Na2 -149.4(3) . . . 2_765 ? O1B Na2 O2 Na2 139.6(3) . . . 2_765 ? O3B Na2 O2 Na2 -83.1(2) . . . 2_765 ? O3B Na2 O2 Na2 74.0(2) 2_765 . . 2_765 ? C2B Na2 O2 Na2 -170.4(3) . . . 2_765 ? Na1 O1 O11 Na1 5.32(17) . . . 2_676 ? Na1 O1 O11 Na1 -5.32(17) 2_676 . . . ? Na1 Na1 O11 O1 166.2(4) 2_676 . . . ? O11 Na1 O11 O1 166.2(4) 2_676 . . . ? O1 Na1 O11 O1 173.5(2) 2_676 . . . ? O1A Na1 O11 O1 -42.3(4) . . . . ? O2A Na1 O11 O1 28.9(4) . . . . ? O3A Na1 O11 O1 -105.3(4) 2_676 . . . ? O3A Na1 O11 O1 91.6(4) . . . . ? O1 Na1 O11 Na1 -166.2(4) . . . 2_676 ? O11 Na1 O11 Na1 0.000(2) 2_676 . . 2_676 ? O1 Na1 O11 Na1 7.3(2) 2_676 . . 2_676 ? O1A Na1 O11 Na1 151.4(3) . . . 2_676 ? O2A Na1 O11 Na1 -137.3(3) . . . 2_676 ? O3A Na1 O11 Na1 88.5(2) 2_676 . . 2_676 ? O3A Na1 O11 Na1 -74.6(2) . . . 2_676 ? Na2 O2 O12 Na2 -7.6(2) . . . 2_765 ? Na2 O2 O12 Na2 7.6(2) 2_765 . . . ? Na2 Na2 O12 O2 -164.3(5) 2_765 . . . ? O12 Na2 O12 O2 -164.3(5) 2_765 . . . ? O2 Na2 O12 O2 -170.8(3) 2_765 . . . ? O2B Na2 O12 O2 45.0(4) . . . . ? O1B Na2 O12 O2 -29.4(5) . . . . ? O3B Na2 O12 O2 109.1(4) . . . . ? O3B Na2 O12 O2 -91.9(4) 2_765 . . . ? C2B Na2 O12 O2 26.6(5) . . . . ? O2 Na2 O12 Na2 164.3(5) . . . 2_765 ? O12 Na2 O12 Na2 0.0 2_765 . . 2_765 ? O2 Na2 O12 Na2 -6.5(2) 2_765 . . 2_765 ? O2B Na2 O12 Na2 -150.7(3) . . . 2_765 ? O1B Na2 O12 Na2 134.9(3) . . . 2_765 ? O3B Na2 O12 Na2 -86.6(2) . . . 2_765 ? O3B Na2 O12 Na2 72.4(2) 2_765 . . 2_765 ? C2B Na2 O12 Na2 -169.1(3) . . . 2_765 ? Na1 Na1 O1A C6A -32.1(5) 2_676 . . 2_676 ? O1 Na1 O1A C6A -106.6(2) . . . 2_676 ? O11 Na1 O1A C6A 80.0(2) 2_676 . . 2_676 ? O11 Na1 O1A C6A -89.06(19) . . . 2_676 ? O1 Na1 O1A C6A 60.3(2) 2_676 . . 2_676 ? O2A Na1 O1A C6A 152.65(17) . . . 2_676 ? O3A Na1 O1A C6A -13.12(15) 2_676 . . 2_676 ? O3A Na1 O1A C6A 171.11(15) . . . 2_676 ? Na1 Na1 O1A C1A -164.4(5) 2_676 . . . ? O1 Na1 O1A C1A 121.1(2) . . . . ? O11 Na1 O1A C1A -52.35(19) 2_676 . . . ? O11 Na1 O1A C1A 138.63(17) . . . . ? O1 Na1 O1A C1A -72.1(2) 2_676 . . . ? O2A Na1 O1A C1A 20.34(14) . . . . ? O3A Na1 O1A C1A -145.44(15) 2_676 . . . ? O3A Na1 O1A C1A 38.80(19) . . . . ? Na1 Na1 O2A C3A -35.3(4) 2_676 . . . ? O1 Na1 O2A C3A 65.21(19) . . . . ? O11 Na1 O2A C3A -111.5(2) 2_676 . . . ? O11 Na1 O2A C3A 52.9(2) . . . . ? O1 Na1 O2A C3A -100.75(19) 2_676 . . . ? O1A Na1 O2A C3A 140.68(16) . . . . ? O3A Na1 O2A C3A 158.35(16) 2_676 . . . ? O3A Na1 O2A C3A -24.58(15) . . . . ? Na1 Na1 O2A C2A -162.8(4) 2_676 . . . ? O1 Na1 O2A C2A -62.32(19) . . . . ? O11 Na1 O2A C2A 120.99(19) 2_676 . . . ? O11 Na1 O2A C2A -74.6(2) . . . . ? O1 Na1 O2A C2A 131.72(18) 2_676 . . . ? O1A Na1 O2A C2A 13.15(14) . . . . ? O3A Na1 O2A C2A 30.82(19) 2_676 . . . ? O3A Na1 O2A C2A -152.11(15) . . . . ? Na1 Na1 O3A C4A 162.9(2) 2_676 . . . ? O1 Na1 O3A C4A -105.8(2) . . . . ? O11 Na1 O3A C4A 70.5(2) 2_676 . . . ? O11 Na1 O3A C4A -131.78(19) . . . . ? O1 Na1 O3A C4A 96.59(19) 2_676 . . . ? O1A Na1 O3A C4A -29.36(19) . . . . ? O2A Na1 O3A C4A -10.28(14) . . . . ? O3A Na1 O3A C4A 162.9(2) 2_676 . . . ? Na1 Na1 O3A C5A 34.5(3) 2_676 . . . ? O1 Na1 O3A C5A 125.8(2) . . . . ? O11 Na1 O3A C5A -58.0(2) 2_676 . . . ? O11 Na1 O3A C5A 99.8(2) . . . . ? O1 Na1 O3A C5A -31.8(2) 2_676 . . . ? O1A Na1 O3A C5A -157.79(16) . . . . ? O2A Na1 O3A C5A -138.71(17) . . . . ? O3A Na1 O3A C5A 34.5(3) 2_676 . . . ? O1 Na1 O3A Na1 91.4(3) . . . 2_676 ? O11 Na1 O3A Na1 -92.4(3) 2_676 . . 2_676 ? O11 Na1 O3A Na1 65.3(2) . . . 2_676 ? O1 Na1 O3A Na1 -66.3(2) 2_676 . . 2_676 ? O1A Na1 O3A Na1 167.8(3) . . . 2_676 ? O2A Na1 O3A Na1 -173.2(2) . . . 2_676 ? O3A Na1 O3A Na1 0.000(3) 2_676 . . 2_676 ? C6A O1A C1A C2A 173.47(19) 2_676 . . . ? Na1 O1A C1A C2A -50.4(2) . . . . ? C3A O2A C2A C1A -172.79(19) . . . . ? Na1 O2A C2A C1A -43.6(2) . . . . ? O1A C1A C2A O2A 63.7(2) . . . . ? C2A O2A C3A C4A -173.90(19) . . . . ? Na1 O2A C3A C4A 58.3(2) . . . . ? C5A O3A C4A C3A 176.1(2) . . . . ? Na1 O3A C4A C3A 47.8(2) 2_676 . . . ? Na1 O3A C4A C3A 41.4(2) . . . . ? O2A C3A C4A O3A -68.3(2) . . . . ? C4A O3A C5A C6A 173.64(19) . . . . ? Na1 O3A C5A C6A -49.4(2) 2_676 . . . ? Na1 O3A C5A C6A -60.1(2) . . . . ? O3A C5A C6A O1A 63.5(2) . . . 2_676 ? Na2 Na2 O1B C1B 162.8(4) 2_765 . . . ? O2 Na2 O1B C1B 66.55(19) . . . . ? O12 Na2 O1B C1B -123.77(18) 2_765 . . . ? O2 Na2 O1B C1B -132.19(17) 2_765 . . . ? O12 Na2 O1B C1B 76.5(2) . . . . ? O2B Na2 O1B C1B -12.43(15) . . . . ? O3B Na2 O1B C1B -30.8(2) . . . . ? O3B Na2 O1B C1B 152.93(16) 2_765 . . . ? C2B Na2 O1B C1B -23.99(14) . . . . ? Na2 Na2 O1B C6B 34.9(4) 2_765 . . 2_765 ? O2 Na2 O1B C6B -61.4(2) . . . 2_765 ? O12 Na2 O1B C6B 108.3(2) 2_765 . . 2_765 ? O2 Na2 O1B C6B 99.9(2) 2_765 . . 2_765 ? O12 Na2 O1B C6B -51.5(2) . . . 2_765 ? O2B Na2 O1B C6B -140.34(18) . . . 2_765 ? O3B Na2 O1B C6B -158.76(18) . . . 2_765 ? O3B Na2 O1B C6B 25.02(17) 2_765 . . 2_765 ? C2B Na2 O1B C6B -151.9(2) . . . 2_765 ? Na2 Na2 O2B C2B 165.1(4) 2_765 . . . ? O2 Na2 O2B C2B -124.3(2) . . . . ? O12 Na2 O2B C2B 55.9(2) 2_765 . . . ? O2 Na2 O2B C2B 72.5(2) 2_765 . . . ? O12 Na2 O2B C2B -138.55(18) . . . . ? O1B Na2 O2B C2B -20.71(15) . . . . ? O3B Na2 O2B C2B 145.63(16) . . . . ? O3B Na2 O2B C2B -40.2(2) 2_765 . . . ? Na2 Na2 O2B C3B 33.2(5) 2_765 . . . ? O2 Na2 O2B C3B 103.8(2) . . . . ? O12 Na2 O2B C3B -76.0(2) 2_765 . . . ? O2 Na2 O2B C3B -59.3(3) 2_765 . . . ? O12 Na2 O2B C3B 89.6(2) . . . . ? O1B Na2 O2B C3B -152.58(18) . . . . ? O3B Na2 O2B C3B 13.76(17) . . . . ? O3B Na2 O2B C3B -172.09(17) 2_765 . . . ? C2B Na2 O2B C3B -131.9(2) . . . . ? Na2 Na2 O3B C5B -20.1(3) 2_765 . . . ? O2 Na2 O3B C5B 66.1(2) . . . . ? O12 Na2 O3B C5B -103.8(2) 2_765 . . . ? O2 Na2 O3B C5B -85.1(2) 2_765 . . . ? O12 Na2 O3B C5B 47.1(2) . . . . ? O2B Na2 O3B C5B 149.5(2) . . . . ? O1B Na2 O3B C5B 168.84(19) . . . . ? O3B Na2 O3B C5B -20.1(3) 2_765 . . . ? C2B Na2 O3B C5B 163.63(19) . . . . ? Na2 Na2 O3B C4B -150.1(2) 2_765 . . . ? O2 Na2 O3B C4B -63.9(2) . . . . ? O12 Na2 O3B C4B 126.22(19) 2_765 . . . ? O2 Na2 O3B C4B 144.91(18) 2_765 . . . ? O12 Na2 O3B C4B -82.94(19) . . . . ? O2B Na2 O3B C4B 19.52(16) . . . . ? O1B Na2 O3B C4B 38.8(2) . . . . ? O3B Na2 O3B C4B -150.1(2) 2_765 . . . ? C2B Na2 O3B C4B 33.60(16) . . . . ? O2 Na2 O3B Na2 86.2(2) . . . 2_765 ? O12 Na2 O3B Na2 -83.7(2) 2_765 . . 2_765 ? O2 Na2 O3B Na2 -65.0(2) 2_765 . . 2_765 ? O12 Na2 O3B Na2 67.1(2) . . . 2_765 ? O2B Na2 O3B Na2 169.6(2) . . . 2_765 ? O1B Na2 O3B Na2 -171.1(3) . . . 2_765 ? O3B Na2 O3B Na2 0.000(1) 2_765 . . 2_765 ? C2B Na2 O3B Na2 -176.3(2) . . . 2_765 ? C6B O1B C1B C2B 172.4(2) 2_765 . . . ? Na2 O1B C1B C2B 42.3(2) . . . . ? C3B O2B C2B C1B -173.7(2) . . . . ? Na2 O2B C2B C1B 50.1(2) . . . . ? C3B O2B C2B Na2 136.3(2) . . . . ? O1B C1B C2B O2B -63.5(3) . . . . ? O1B C1B C2B Na2 -29.52(16) . . . . ? Na2 Na2 C2B O2B -52.5(14) 2_765 . . . ? O2 Na2 C2B O2B 55.72(19) . . . . ? O12 Na2 C2B O2B -127.99(19) 2_765 . . . ? O2 Na2 C2B O2B -119.3(2) 2_765 . . . ? O12 Na2 C2B O2B 46.8(2) . . . . ? O1B Na2 C2B O2B 153.59(19) . . . . ? O3B Na2 C2B O2B -31.09(15) . . . . ? O3B Na2 C2B O2B 150.49(16) 2_765 . . . ? Na2 Na2 C2B C1B 175.7(14) 2_765 . . . ? O2 Na2 C2B C1B -76.09(19) . . . . ? O12 Na2 C2B C1B 100.20(18) 2_765 . . . ? O2 Na2 C2B C1B 108.9(2) 2_765 . . . ? O12 Na2 C2B C1B -85.04(19) . . . . ? O2B Na2 C2B C1B -131.8(2) . . . . ? O1B Na2 C2B C1B 21.78(13) . . . . ? O3B Na2 C2B C1B -162.90(15) . . . . ? O3B Na2 C2B C1B 18.69(17) 2_765 . . . ? C2B O2B C3B C4B -175.6(2) . . . . ? Na2 O2B C3B C4B -45.1(2) . . . . ? C5B O3B C4B C3B 173.7(2) . . . . ? Na2 O3B C4B C3B -48.3(2) . . . . ? Na2 O3B C4B C3B -61.8(3) 2_765 . . . ? O2B C3B C4B O3B 63.6(3) . . . . ? C4B O3B C5B C6B 176.5(2) . . . . ? Na2 O3B C5B C6B 49.3(3) . . . . ? Na2 O3B C5B C6B 41.4(2) 2_765 . . . ? O3B C5B C6B O1B -68.7(3) . . . 2_765 ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 0.410 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.049 #===END data_nai18 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H28 I3 Na O8' _chemical_formula_weight 704.03 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' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 '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 20.6803(8) _cell_length_b 11.0480(5) _cell_length_c 10.8675(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.989(2) _cell_angle_gamma 90.00 _cell_volume 2333.38(15) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.004 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 4.066 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.4968 _exptl_absorpt_correction_T_max 0.8225 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '2o phi frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10176 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.60 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2241 _reflns_number_gt 2088 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement Denzo-smn _computing_data_reduction Denzo-smn _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics RES2INS _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+3.3232P] 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 SHELXL _refine_ls_extinction_coef 0.00086(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2241 _refine_ls_number_parameters 121 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0266 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0628 _refine_ls_wR_factor_gt 0.0615 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.7500 0.7500 0.5000 0.02359(11) Uani 1 2 d S . . I2 I 0.833463(10) 0.96840(2) 0.57361(2) 0.03492(11) Uani 1 1 d . . . Na1 Na 0.5000 1.0000 0.5000 0.0369(4) Uani 1 2 d S . . O1 O 0.43791(12) 1.0860(3) 0.6199(2) 0.0351(6) Uani 1 1 d . . . H12 H 0.411(3) 1.121(6) 0.564(6) 0.11(2) Uiso 1 1 d . . . H11 H 0.435(3) 1.094(5) 0.685(5) 0.068(16) Uiso 1 1 d . . . O1A O 0.48203(12) 0.7582(2) 0.5402(2) 0.0315(5) Uani 1 1 d . . . O2A O 0.61096(11) 0.8602(2) 0.65230(19) 0.0322(5) Uani 1 1 d . . . O3A O 0.61882(10) 1.1104(2) 0.6610(2) 0.0311(5) Uani 1 1 d . . . C1A C 0.5424(2) 0.6852(4) 0.5966(4) 0.0469(9) Uani 1 1 d . . . H1A2 H 0.5628 0.6648 0.5290 0.056 Uiso 1 1 calc R . . H1A1 H 0.5300 0.6087 0.6306 0.056 Uiso 1 1 calc R . . C2A C 0.59303(19) 0.7535(4) 0.7049(4) 0.0455(10) Uani 1 1 d . . . H2A2 H 0.5727 0.7743 0.7725 0.055 Uiso 1 1 calc R . . H2A1 H 0.6345 0.7034 0.7463 0.055 Uiso 1 1 calc R . . C3A C 0.66755(16) 0.9222(4) 0.7443(3) 0.0406(9) Uani 1 1 d . . . H3A2 H 0.7095 0.8716 0.7665 0.049 Uiso 1 1 calc R . . H3A1 H 0.6576 0.9382 0.8257 0.049 Uiso 1 1 calc R . . C4A C 0.67858(16) 1.0373(4) 0.6859(3) 0.0390(9) Uani 1 1 d . . . H4A2 H 0.7191 1.0796 0.7467 0.047 Uiso 1 1 calc R . . H4A1 H 0.6872 1.0215 0.6032 0.047 Uiso 1 1 calc R . . C5A C 0.62977(18) 1.2284(4) 0.6159(3) 0.0390(8) Uani 1 1 d . . . H5A2 H 0.6465 1.2204 0.5411 0.047 Uiso 1 1 calc R . . H5A1 H 0.6651 1.2724 0.6870 0.047 Uiso 1 1 calc R . . C6A C 0.56408(19) 1.2971(3) 0.5749(3) 0.0384(8) Uani 1 1 d . . . H6A2 H 0.5440 1.2958 0.6456 0.046 Uiso 1 1 calc R . . H6A1 H 0.5724 1.3824 0.5568 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.02447(16) 0.02539(18) 0.02354(16) 0.00010(9) 0.01160(11) 0.00350(10) I2 0.03275(15) 0.03137(17) 0.04653(17) -0.00691(9) 0.02118(11) -0.00584(8) Na1 0.0362(10) 0.0496(12) 0.0336(10) -0.0122(8) 0.0231(8) -0.0079(9) O1 0.0335(12) 0.0546(16) 0.0209(11) 0.0054(11) 0.0142(9) 0.0098(11) O1A 0.0364(12) 0.0289(13) 0.0350(12) 0.0008(9) 0.0195(10) 0.0028(9) O2A 0.0283(10) 0.0448(14) 0.0234(10) 0.0058(9) 0.0087(8) 0.0096(10) O3A 0.0230(10) 0.0444(14) 0.0292(11) -0.0063(9) 0.0132(8) -0.0019(9) C1A 0.052(2) 0.0303(19) 0.070(2) 0.0173(18) 0.0349(19) 0.0145(17) C2A 0.0383(19) 0.057(3) 0.043(2) 0.0262(17) 0.0156(16) 0.0192(17) C3A 0.0287(16) 0.062(3) 0.0253(16) -0.0046(15) 0.0013(12) 0.0237(17) C4A 0.0192(14) 0.065(3) 0.0321(18) -0.0190(16) 0.0081(12) -0.0010(15) C5A 0.0385(18) 0.052(2) 0.0301(18) -0.0066(14) 0.0163(14) -0.0195(16) C6A 0.055(2) 0.0291(19) 0.0407(19) -0.0063(14) 0.0291(16) -0.0139(16) _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 I1 I2 2.9150(2) 7_666 ? I1 I2 2.9150(2) . ? Na1 O1 2.322(2) . ? Na1 O1 2.322(2) 5_676 ? Na1 O1A 2.753(2) 5_676 ? Na1 O1A 2.753(2) . ? Na1 O3A 2.765(2) . ? Na1 O3A 2.765(2) 5_676 ? Na1 O2A 2.792(2) 5_676 ? Na1 O2A 2.792(2) . ? O1A C6A 1.425(4) 5_676 ? O1A C1A 1.436(4) . ? O2A C2A 1.415(4) . ? O2A C3A 1.427(4) . ? O3A C4A 1.423(4) . ? O3A C5A 1.438(4) . ? C1A C2A 1.486(6) . ? C3A C4A 1.473(6) . ? C5A C6A 1.485(5) . ? C6A O1A 1.425(4) 5_676 ? 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 I2 I1 I2 180.0 7_666 . ? O1 Na1 O1 180.0 . 5_676 ? O1 Na1 O1A 79.79(8) . 5_676 ? O1 Na1 O1A 100.21(8) 5_676 5_676 ? O1 Na1 O1A 100.21(8) . . ? O1 Na1 O1A 79.79(8) 5_676 . ? O1A Na1 O1A 180.0 5_676 . ? O1 Na1 O3A 90.39(8) . . ? O1 Na1 O3A 89.61(8) 5_676 . ? O1A Na1 O3A 62.19(7) 5_676 . ? O1A Na1 O3A 117.81(7) . . ? O1 Na1 O3A 89.61(8) . 5_676 ? O1 Na1 O3A 90.39(8) 5_676 5_676 ? O1A Na1 O3A 117.81(7) 5_676 5_676 ? O1A Na1 O3A 62.19(7) . 5_676 ? O3A Na1 O3A 180.0 . 5_676 ? O1 Na1 O2A 66.81(8) . 5_676 ? O1 Na1 O2A 113.19(8) 5_676 5_676 ? O1A Na1 O2A 59.82(7) 5_676 5_676 ? O1A Na1 O2A 120.18(7) . 5_676 ? O3A Na1 O2A 120.25(7) . 5_676 ? O3A Na1 O2A 59.75(7) 5_676 5_676 ? O1 Na1 O2A 113.19(8) . . ? O1 Na1 O2A 66.81(8) 5_676 . ? O1A Na1 O2A 120.18(7) 5_676 . ? O1A Na1 O2A 59.82(7) . . ? O3A Na1 O2A 59.75(7) . . ? O3A Na1 O2A 120.25(7) 5_676 . ? O2A Na1 O2A 180.0 5_676 . ? C6A O1A C1A 110.9(3) 5_676 . ? C6A O1A Na1 111.25(18) 5_676 . ? C1A O1A Na1 117.9(2) . . ? C2A O2A C3A 112.5(3) . . ? C2A O2A Na1 115.15(19) . . ? C3A O2A Na1 117.5(2) . . ? C4A O3A C5A 110.6(2) . . ? C4A O3A Na1 113.32(19) . . ? C5A O3A Na1 113.19(18) . . ? O1A C1A C2A 109.1(3) . . ? O2A C2A C1A 108.3(3) . . ? O2A C3A C4A 108.8(3) . . ? O3A C4A C3A 108.7(3) . . ? O3A C5A C6A 109.3(3) . . ? O1A C6A C5A 108.3(3) 5_676 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Na1 O1A C6A 107.2(2) . . . 5_676 ? O1 Na1 O1A C6A -72.8(2) 5_676 . . 5_676 ? O1A Na1 O1A C6A 90(100) 5_676 . . 5_676 ? O3A Na1 O1A C6A -156.91(19) . . . 5_676 ? O3A Na1 O1A C6A 23.09(19) 5_676 . . 5_676 ? O2A Na1 O1A C6A 38.2(2) 5_676 . . 5_676 ? O2A Na1 O1A C6A -141.8(2) . . . 5_676 ? O1 Na1 O1A C1A -123.1(2) . . . . ? O1 Na1 O1A C1A 56.9(2) 5_676 . . . ? O1A Na1 O1A C1A -140(100) 5_676 . . . ? O3A Na1 O1A C1A -27.2(2) . . . . ? O3A Na1 O1A C1A 152.8(2) 5_676 . . . ? O2A Na1 O1A C1A 167.9(2) 5_676 . . . ? O2A Na1 O1A C1A -12.1(2) . . . . ? O1 Na1 O2A C2A 67.0(2) . . . . ? O1 Na1 O2A C2A -113.0(2) 5_676 . . . ? O1A Na1 O2A C2A 158.5(2) 5_676 . . . ? O1A Na1 O2A C2A -21.5(2) . . . . ? O3A Na1 O2A C2A 143.1(2) . . . . ? O3A Na1 O2A C2A -36.9(2) 5_676 . . . ? O2A Na1 O2A C2A 84(100) 5_676 . . . ? O1 Na1 O2A C3A -69.0(2) . . . . ? O1 Na1 O2A C3A 111.0(2) 5_676 . . . ? O1A Na1 O2A C3A 22.5(2) 5_676 . . . ? O1A Na1 O2A C3A -157.5(2) . . . . ? O3A Na1 O2A C3A 7.04(19) . . . . ? O3A Na1 O2A C3A -172.96(19) 5_676 . . . ? O2A Na1 O2A C3A -52(100) 5_676 . . . ? O1 Na1 O3A C4A 143.0(2) . . . . ? O1 Na1 O3A C4A -37.0(2) 5_676 . . . ? O1A Na1 O3A C4A -138.7(2) 5_676 . . . ? O1A Na1 O3A C4A 41.3(2) . . . . ? O3A Na1 O3A C4A 162(100) 5_676 . . . ? O2A Na1 O3A C4A -153.82(19) 5_676 . . . ? O2A Na1 O3A C4A 26.18(19) . . . . ? O1 Na1 O3A C5A -90.0(2) . . . . ? O1 Na1 O3A C5A 90.0(2) 5_676 . . . ? O1A Na1 O3A C5A -11.74(18) 5_676 . . . ? O1A Na1 O3A C5A 168.26(18) . . . . ? O3A Na1 O3A C5A -71(100) 5_676 . . . ? O2A Na1 O3A C5A -26.8(2) 5_676 . . . ? O2A Na1 O3A C5A 153.2(2) . . . . ? C6A O1A C1A C2A 172.3(3) 5_676 . . . ? Na1 O1A C1A C2A 42.4(3) . . . . ? C3A O2A C2A C1A -170.4(3) . . . . ? Na1 O2A C2A C1A 51.4(3) . . . . ? O1A C1A C2A O2A -61.1(4) . . . . ? C2A O2A C3A C4A -174.8(3) . . . . ? Na1 O2A C3A C4A -37.7(3) . . . . ? C5A O3A C4A C3A 174.3(2) . . . . ? Na1 O3A C4A C3A -57.3(3) . . . . ? O2A C3A C4A O3A 62.4(3) . . . . ? C4A O3A C5A C6A 172.9(3) . . . . ? Na1 O3A C5A C6A 44.5(3) . . . . ? O3A C5A C6A O1A -68.5(3) . . . 5_676 ? 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 H12 O2A 0.77(7) 2.25(6) 2.842(3) 135(6) 5_676 O1 H11 O3A 0.73(5) 2.31(5) 3.005(3) 157(5) 2_656 _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.951 _refine_diff_density_min -1.097 _refine_diff_density_rms 0.104 #===END data_nabph418 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H93 B2 Na2 O15' _chemical_formula_weight 1290.08 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' 'B' 'B' 0.0013 0.0007 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.4119(9) _cell_length_b 13.9456(10) _cell_length_c 22.5930(17) _cell_angle_alpha 77.532(2) _cell_angle_beta 74.082(2) _cell_angle_gamma 62.094(2) _cell_volume 3572.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1378 _exptl_absorpt_coefficient_mu 0.092 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.9729 _exptl_absorpt_correction_T_max 0.9818 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '2o phi frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 20041 _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_sigmaI/netI 0.0794 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11756 _reflns_number_gt 8253 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Xseed (Barbour, 1999)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+2.5570P] 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 SHELXL _refine_ls_extinction_coef 0.0077(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 11756 _refine_ls_number_parameters 1052 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0959 _refine_ls_R_factor_gt 0.0617 _refine_ls_wR_factor_ref 0.1540 _refine_ls_wR_factor_gt 0.1366 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.341 _refine_ls_shift/su_mean 0.005 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 Na1 Na -0.0462(3) 0.6103(3) -0.08670(16) 0.0463(8) Uani 0.50 1 d P . 1 Na11 Na 0.0116(3) 0.5822(3) -0.09624(17) 0.0478(9) Uani 0.50 1 d P . 2 O1 O 0.0032(3) 0.6342(3) -0.19705(16) 0.0356(9) Uani 0.50 1 d P A 1 O2 O -0.0325(18) 0.5399(12) 0.0182(7) 0.017(3) Uani 0.25 1 d P . 1 O11 O -0.1088(4) 0.6486(4) -0.1668(2) 0.0591(13) Uani 0.50 1 d P B 2 C25 C -0.3357(2) 0.1614(2) -0.02675(11) 0.0257(6) Uani 1 1 d . . . C26 C -0.3932(2) 0.0948(2) -0.00385(12) 0.0280(6) Uani 1 1 d . . . H26 H -0.4061 0.0631 -0.0326 0.034 Uiso 1 1 calc R . . C27 C -0.4325(2) 0.0730(2) 0.05938(12) 0.0316(6) Uani 1 1 d . . . H27 H -0.4706 0.0270 0.0727 0.038 Uiso 1 1 calc R . . C28 C -0.4159(2) 0.1182(2) 0.10239(12) 0.0351(7) Uani 1 1 d . . . H28 H -0.4422 0.1036 0.1454 0.042 Uiso 1 1 calc R . . C29 C -0.3602(2) 0.1852(2) 0.08173(12) 0.0328(6) Uani 1 1 d . . . H29 H -0.3484 0.2170 0.1108 0.039 Uiso 1 1 calc R . . C30 C -0.3215(2) 0.2062(2) 0.01887(12) 0.0297(6) Uani 1 1 d . . . H30 H -0.2840 0.2527 0.0061 0.036 Uiso 1 1 calc R . . C31 C -0.1462(2) 0.14094(19) -0.11773(11) 0.0235(5) Uani 1 1 d . . . C32 C -0.0851(2) 0.1293(2) -0.17952(12) 0.0286(6) Uani 1 1 d . . . H32 H -0.1274 0.1476 -0.2111 0.034 Uiso 1 1 calc R . . C33 C 0.0336(2) 0.0924(2) -0.19665(13) 0.0310(6) Uani 1 1 d . . . H33 H 0.0699 0.0878 -0.2391 0.037 Uiso 1 1 calc R . . C34 C 0.0992(2) 0.0623(2) -0.15233(13) 0.0318(6) Uani 1 1 d . . . H34 H 0.1804 0.0366 -0.1638 0.038 Uiso 1 1 calc R . . C35 C 0.0436(2) 0.0704(2) -0.09059(13) 0.0312(6) Uani 1 1 d . . . H35 H 0.0872 0.0493 -0.0594 0.037 Uiso 1 1 calc R . . C36 C -0.0763(2) 0.1095(2) -0.07418(12) 0.0273(6) Uani 1 1 d . . . H36 H -0.1120 0.1149 -0.0317 0.033 Uiso 1 1 calc R . . C37 C -0.3222(2) 0.1241(2) -0.14100(11) 0.0244(5) Uani 1 1 d . . . C38 C -0.2615(2) 0.0105(2) -0.14258(11) 0.0274(6) Uani 1 1 d . . . H38 H -0.1974 -0.0278 -0.1227 0.033 Uiso 1 1 calc R . . C39 C -0.2900(2) -0.0486(2) -0.17162(12) 0.0327(6) Uani 1 1 d . . . H39 H -0.2470 -0.1256 -0.1707 0.039 Uiso 1 1 calc R . . C40 C -0.3819(2) 0.0054(2) -0.20212(13) 0.0361(7) Uani 1 1 d . . . H40 H -0.4019 -0.0341 -0.2225 0.043 Uiso 1 1 calc R . . C41 C -0.4435(2) 0.1171(2) -0.20233(14) 0.0380(7) Uani 1 1 d . . . H41 H -0.5059 0.1550 -0.2234 0.046 Uiso 1 1 calc R . . C42 C -0.4148(2) 0.1746(2) -0.17180(12) 0.0322(6) Uani 1 1 d . . . H42 H -0.4598 0.2512 -0.1719 0.039 Uiso 1 1 calc R . . C43 C -0.3489(2) 0.3197(2) -0.12234(12) 0.0256(6) Uani 1 1 d . . . C44 C -0.4319(2) 0.3982(2) -0.08317(12) 0.0274(6) Uani 1 1 d . . . H44 H -0.4568 0.3742 -0.0416 0.033 Uiso 1 1 calc R . . C45 C -0.4799(2) 0.5097(2) -0.10211(13) 0.0331(6) Uani 1 1 d . . . H45 H -0.5352 0.5596 -0.0734 0.040 Uiso 1 1 calc R . . C46 C -0.4476(3) 0.5479(2) -0.16215(14) 0.0399(7) Uani 1 1 d . . . H46 H -0.4793 0.6239 -0.1752 0.048 Uiso 1 1 calc R . . C47 C -0.3682(3) 0.4735(2) -0.20315(14) 0.0467(8) Uani 1 1 d . . . H47 H -0.3459 0.4982 -0.2450 0.056 Uiso 1 1 calc R . . C48 C -0.3209(3) 0.3629(2) -0.18341(13) 0.0374(7) Uani 1 1 d . . . H48 H -0.2666 0.3138 -0.2127 0.045 Uiso 1 1 calc R . . C73 C -0.1477(2) -0.3553(2) 0.38053(12) 0.0284(6) Uani 1 1 d . . . C74 C -0.0879(2) -0.3180(2) 0.32620(12) 0.0310(6) Uani 1 1 d . . . H74 H -0.1309 -0.2631 0.2980 0.037 Uiso 1 1 calc R . . C75 C 0.0315(2) -0.3585(2) 0.31223(13) 0.0370(7) Uani 1 1 d . . . H75 H 0.0683 -0.3305 0.2754 0.044 Uiso 1 1 calc R . . C76 C 0.0968(2) -0.4396(3) 0.35205(13) 0.0414(7) Uani 1 1 d . . . H76 H 0.1784 -0.4680 0.3426 0.050 Uiso 1 1 calc R . . C77 C 0.0413(2) -0.4789(3) 0.40595(14) 0.0430(7) Uani 1 1 d . . . H77 H 0.0847 -0.5343 0.4339 0.052 Uiso 1 1 calc R . . C78 C -0.0781(2) -0.4366(2) 0.41869(12) 0.0361(7) Uani 1 1 d . . . H78 H -0.1142 -0.4649 0.4556 0.043 Uiso 1 1 calc R . . C79 C -0.3190(2) -0.3792(2) 0.35600(11) 0.0293(6) Uani 1 1 d . . . C80 C -0.4268(2) -0.3405(2) 0.34038(12) 0.0332(6) Uani 1 1 d . . . H80 H -0.4826 -0.2683 0.3480 0.040 Uiso 1 1 calc R . . C81 C -0.4551(3) -0.4037(3) 0.31425(13) 0.0381(7) Uani 1 1 d . . . H81 H -0.5287 -0.3739 0.3040 0.046 Uiso 1 1 calc R . . C82 C -0.3769(2) -0.5095(2) 0.30311(12) 0.0355(7) Uani 1 1 d . . . H82 H -0.3966 -0.5535 0.2862 0.043 Uiso 1 1 calc R . . C83 C -0.2694(3) -0.5500(2) 0.31710(13) 0.0386(7) Uani 1 1 d . . . H83 H -0.2143 -0.6223 0.3094 0.046 Uiso 1 1 calc R . . C84 C -0.2417(2) -0.4856(2) 0.34230(13) 0.0360(7) Uani 1 1 d . . . H84 H -0.1666 -0.5151 0.3507 0.043 Uiso 1 1 calc R . . C85 C -0.3338(2) -0.3398(2) 0.46925(12) 0.0274(6) Uani 1 1 d . . . C86 C -0.3956(2) -0.4022(2) 0.49239(12) 0.0293(6) Uani 1 1 d . . . H86 H -0.4154 -0.4280 0.4637 0.035 Uiso 1 1 calc R . . C87 C -0.4299(2) -0.4284(2) 0.55566(12) 0.0342(6) Uani 1 1 d . . . H87 H -0.4710 -0.4717 0.5691 0.041 Uiso 1 1 calc R . . C88 C -0.4036(2) -0.3913(2) 0.59847(13) 0.0365(7) Uani 1 1 d . . . H88 H -0.4274 -0.4078 0.6415 0.044 Uiso 1 1 calc R . . C89 C -0.3419(2) -0.3295(2) 0.57802(12) 0.0354(7) Uani 1 1 d . . . H89 H -0.3231 -0.3037 0.6071 0.042 Uiso 1 1 calc R . . C90 C -0.3077(2) -0.3055(2) 0.51493(12) 0.0332(6) Uani 1 1 d . . . H90 H -0.2646 -0.2640 0.5020 0.040 Uiso 1 1 calc R . . C91 C -0.3511(2) -0.1796(2) 0.37313(12) 0.0279(6) Uani 1 1 d . . . C92 C -0.3532(2) -0.1404(2) 0.31058(13) 0.0352(6) Uani 1 1 d . . . H92 H -0.3230 -0.1919 0.2814 0.042 Uiso 1 1 calc R . . C93 C -0.3970(3) -0.0303(3) 0.28904(15) 0.0428(7) Uani 1 1 d . . . H93 H -0.3954 -0.0085 0.2461 0.051 Uiso 1 1 calc R . . C94 C -0.4428(3) 0.0476(3) 0.32996(16) 0.0482(8) Uani 1 1 d . . . H94 H -0.4724 0.1231 0.3156 0.058 Uiso 1 1 calc R . . C95 C -0.4447(3) 0.0135(3) 0.39241(16) 0.0450(8) Uani 1 1 d . . . H95 H -0.4764 0.0660 0.4212 0.054 Uiso 1 1 calc R . . C96 C -0.4006(2) -0.0970(2) 0.41326(14) 0.0351(6) Uani 1 1 d . . . H96 H -0.4038 -0.1179 0.4564 0.042 Uiso 1 1 calc R . . B2 B -0.2891(2) 0.1870(2) -0.10125(13) 0.0252(6) Uani 1 1 d . . . B4 B -0.2895(3) -0.3117(3) 0.39496(14) 0.0282(7) Uani 1 1 d . . . O1A O 0.20382(15) 0.47301(15) -0.15743(8) 0.0345(4) Uani 1 1 d . . . O2A O 0.14337(15) 0.66104(14) -0.10442(8) 0.0337(4) Uani 1 1 d . . . O3A O -0.08809(15) 0.77996(14) -0.05420(8) 0.0300(4) Uani 1 1 d . . . O4A O -0.23918(15) 0.68422(14) -0.01393(9) 0.0333(4) Uani 1 1 d . . . O5A O -0.18238(16) 0.51438(14) -0.08238(8) 0.0334(4) Uani 1 1 d . . . O6A O 0.05139(15) 0.37835(15) -0.12825(8) 0.0338(4) Uani 1 1 d . . . C1A C 0.2886(2) 0.4965(2) -0.14589(13) 0.0346(6) Uani 1 1 d . . . H1A2 H 0.3615 0.4647 -0.1762 0.042 Uiso 1 1 calc R . . H1A1 H 0.3037 0.4650 -0.1038 0.042 Uiso 1 1 calc R . . C2A C 0.2436(2) 0.6179(2) -0.15170(13) 0.0364(7) Uani 1 1 d . . . H2A2 H 0.3033 0.6373 -0.1474 0.044 Uiso 1 1 calc R . . H2A1 H 0.2240 0.6495 -0.1929 0.044 Uiso 1 1 calc R . . C3A C 0.0898(2) 0.7772(2) -0.11133(14) 0.0367(7) Uani 1 1 d . . . H3A2 H 0.0575 0.8046 -0.1494 0.044 Uiso 1 1 calc R . . H3A1 H 0.1472 0.8050 -0.1149 0.044 Uiso 1 1 calc R . . C4A C -0.0039(2) 0.8162(2) -0.05617(13) 0.0333(6) Uani 1 1 d . . . H4A2 H 0.0280 0.7868 -0.0180 0.040 Uiso 1 1 calc R . . H4A1 H -0.0395 0.8969 -0.0590 0.040 Uiso 1 1 calc R . . C5A C -0.1792(2) 0.8130(2) -0.00105(13) 0.0349(6) Uani 1 1 d . . . H5A2 H -0.2045 0.8906 0.0033 0.042 Uiso 1 1 calc R . . H5A1 H -0.1518 0.7686 0.0368 0.042 Uiso 1 1 calc R . . C6A C -0.2773(2) 0.7974(2) -0.00922(14) 0.0353(6) Uani 1 1 d . . . H6A2 H -0.3421 0.8216 0.0265 0.042 Uiso 1 1 calc R . . H6A1 H -0.3044 0.8417 -0.0472 0.042 Uiso 1 1 calc R . . C7A C -0.3253(2) 0.6662(2) -0.02899(15) 0.0390(7) Uani 1 1 d . . . H7A2 H -0.3441 0.7080 -0.0690 0.047 Uiso 1 1 calc R . . H7A1 H -0.3964 0.6910 0.0033 0.047 Uiso 1 1 calc R . . C8A C -0.2804(2) 0.5471(2) -0.03323(14) 0.0382(7) Uani 1 1 d . . . H8A2 H -0.2588 0.5051 0.0063 0.046 Uiso 1 1 calc R . . H8A1 H -0.3408 0.5323 -0.0410 0.046 Uiso 1 1 calc R . . C9A C -0.1414(2) 0.4017(2) -0.09055(14) 0.0361(7) Uani 1 1 d . . . H9A2 H -0.2036 0.3904 -0.0989 0.043 Uiso 1 1 calc R . . H9A1 H -0.1184 0.3553 -0.0522 0.043 Uiso 1 1 calc R . . C10A C -0.0410(2) 0.3701(2) -0.14310(13) 0.0354(6) Uani 1 1 d . . . H10B H -0.0165 0.2944 -0.1510 0.042 Uiso 1 1 calc R . . H10A H -0.0627 0.4189 -0.1810 0.042 Uiso 1 1 calc R . . C11A C 0.1519(3) 0.3431(3) -0.17615(14) 0.0414(7) Uani 1 1 d . . . H11B H 0.1333 0.3856 -0.2161 0.050 Uiso 1 1 calc R . . H11A H 0.1790 0.2651 -0.1803 0.050 Uiso 1 1 calc R . . C12A C 0.2445(2) 0.3592(2) -0.16082(14) 0.0401(7) Uani 1 1 d . . . H12B H 0.2627 0.3175 -0.1207 0.048 Uiso 1 1 calc R . . H12A H 0.3153 0.3328 -0.1932 0.048 Uiso 1 1 calc R . . C2S C -0.0925(6) 0.6053(6) -0.2800(3) 0.0051(15) Uiso 0.25 1 d P A 1 C4S C -0.1620(10) 0.6620(8) -0.2377(5) 0.086(3) Uiso 0.50 1 d P B 2 Na3 Na -0.0723(7) -0.0329(8) 0.4277(7) 0.0359(14) Uani 0.50 1 d P . 1 O14 O -0.1474(12) -0.1426(13) 0.4167(8) 0.077(5) Uani 0.50 1 d P . 2 O5 O 0.0327(3) -0.0179(3) 0.48970(19) 0.0304(10) Uani 0.50 1 d P . . O1X O -0.1764(18) 0.1392(19) 0.3648(13) 0.036(3) Uani 0.50 1 d P . 2 O2C O -0.27695(16) 0.07973(17) 0.47750(9) 0.0423(5) Uani 1 1 d . . . O5C O 0.1541(17) -0.1947(19) 0.4088(14) 0.061(6) Uani 0.50 1 d P . 1 O6C O 0.064(2) -0.0406(14) 0.3221(13) 0.041(4) Uani 0.50 1 d P . 1 C1X C -0.297(2) 0.1753(17) 0.3851(12) 0.044(5) Uani 0.50 1 d P . 2 H1X1 H -0.3201 0.1277 0.3706 0.052 Uiso 0.50 1 calc PR . 2 H1X2 H -0.3367 0.2502 0.3654 0.052 Uiso 0.50 1 calc PR . 2 C5X C -0.0946(10) -0.2199(8) 0.5779(5) 0.045(2) Uani 0.50 1 d P . 2 H5X1 H -0.1013 -0.2569 0.5474 0.054 Uiso 0.50 1 calc PR . 2 H5X2 H -0.1390 -0.2345 0.6188 0.054 Uiso 0.50 1 calc PR . 2 C8C C 0.1969(19) -0.3080(18) 0.4460(8) 0.061(6) Uani 0.50 1 d P . 1 H8C1 H 0.2821 -0.3433 0.4388 0.073 Uiso 0.50 1 calc PR . 1 H8C2 H 0.1719 -0.3552 0.4328 0.073 Uiso 0.50 1 calc PR . 1 C9C C 0.215(3) -0.207(2) 0.3472(13) 0.050(5) Uani 0.50 1 d P . 1 H9C1 H 0.1902 -0.2459 0.3267 0.060 Uiso 0.50 1 calc PR . 1 H9C2 H 0.2986 -0.2485 0.3458 0.060 Uiso 0.50 1 calc PR . 1 C10C C 0.1865(17) -0.0921(16) 0.3154(10) 0.046(6) Uani 0.50 1 d P . 1 H10C H 0.2118 -0.0530 0.3354 0.055 Uiso 0.50 1 calc PR . 1 H10D H 0.2245 -0.0940 0.2711 0.055 Uiso 0.50 1 calc PR . 1 C11X C -0.0111(11) 0.0860(13) 0.2891(7) 0.032(3) Uani 0.50 1 d P . 2 H11C H 0.0177 0.0782 0.2443 0.038 Uiso 0.50 1 calc PR . 2 H11D H 0.0091 0.1394 0.2993 0.038 Uiso 0.50 1 calc PR . 2 C12C C -0.0975(14) 0.1217(16) 0.2946(9) 0.050(5) Uani 0.50 1 d P . 1 H12C H -0.1220 0.0739 0.2816 0.060 Uiso 0.50 1 calc PR . 1 H12D H -0.1254 0.1931 0.2693 0.060 Uiso 0.50 1 calc PR . 1 O3X O -0.1402(6) -0.1029(6) 0.5595(4) 0.0378(18) Uani 0.50 1 d P . 2 O4C O 0.0244(4) -0.2455(4) 0.52216(19) 0.0389(10) Uani 0.50 1 d P . 1 O5X O 0.1591(14) -0.1939(12) 0.4021(12) 0.036(4) Uani 0.50 1 d P . 2 O6X O 0.0389(19) -0.0123(13) 0.3222(13) 0.032(3) Uani 0.50 1 d P . 2 O1C O -0.1467(19) 0.137(2) 0.3616(12) 0.044(4) Uani 0.50 1 d P . 1 C2C C -0.3140(15) 0.1943(14) 0.4406(10) 0.041(3) Uani 0.50 1 d P . 1 H2C1 H -0.3989 0.2362 0.4499 0.049 Uiso 0.50 1 calc PR . 1 H2C2 H -0.2795 0.2355 0.4516 0.049 Uiso 0.50 1 calc PR . 1 C4X C -0.2638(11) -0.0509(12) 0.5703(6) 0.042(3) Uani 0.50 1 d P . 2 H4X1 H -0.2957 -0.0556 0.6153 0.050 Uiso 0.50 1 calc PR . 2 H4X2 H -0.2909 -0.0888 0.5505 0.050 Uiso 0.50 1 calc PR . 2 C6X C 0.0270(11) -0.2616(16) 0.5811(10) 0.055(4) Uani 0.50 1 d P . 2 H6X1 H 0.0320 -0.2248 0.6123 0.066 Uiso 0.50 1 calc PR . 2 H6X2 H 0.0575 -0.3406 0.5951 0.066 Uiso 0.50 1 calc PR . 2 C10X C 0.1594(18) -0.0570(17) 0.3154(8) 0.040(4) Uani 0.50 1 d P . 2 H10E H 0.1781 -0.0181 0.3394 0.048 Uiso 0.50 1 calc PR . 2 H10F H 0.1941 -0.0459 0.2713 0.048 Uiso 0.50 1 calc PR . 2 C7X C 0.1260(6) -0.3205(5) 0.4804(4) 0.0422(15) Uani 0.50 1 d P . 2 H7X1 H 0.0554 -0.3106 0.4689 0.051 Uiso 0.50 1 calc PR . 2 H7X2 H 0.1640 -0.3963 0.4993 0.051 Uiso 0.50 1 calc PR . 2 C8X C 0.2046(15) -0.2979(14) 0.4254(8) 0.036(3) Uani 0.50 1 d P . 2 H8X1 H 0.2779 -0.3157 0.4370 0.043 Uiso 0.50 1 calc PR . 2 H8X2 H 0.2221 -0.3452 0.3935 0.043 Uiso 0.50 1 calc PR . 2 C1C C -0.271(2) 0.176(2) 0.3716(12) 0.049(7) Uani 0.50 1 d P . 1 H1C1 H -0.2898 0.1207 0.3624 0.059 Uiso 0.50 1 calc PR . 1 H1C2 H -0.3050 0.2444 0.3451 0.059 Uiso 0.50 1 calc PR . 1 C12X C -0.1391(13) 0.1256(14) 0.3044(8) 0.037(3) Uani 0.50 1 d P . 2 H12E H -0.1760 0.1956 0.2794 0.044 Uiso 0.50 1 calc PR . 2 H12F H -0.1594 0.0718 0.2948 0.044 Uiso 0.50 1 calc PR . 2 C11C C 0.0317(13) 0.0708(18) 0.2851(10) 0.059(5) Uani 0.50 1 d P . 1 H11E H 0.0571 0.1155 0.3005 0.071 Uiso 0.50 1 calc PR . 1 H11F H 0.0674 0.0635 0.2407 0.071 Uiso 0.50 1 calc PR . 1 C9X C 0.210(2) -0.1751(15) 0.3368(10) 0.034(4) Uani 0.50 1 d P . 2 H9X1 H 0.1957 -0.2150 0.3112 0.041 Uiso 0.50 1 calc PR . 2 H9X2 H 0.2944 -0.2033 0.3318 0.041 Uiso 0.50 1 calc PR . 2 C3X C -0.3046(15) 0.0638(12) 0.5446(10) 0.038(4) Uani 0.50 1 d P . 2 H3X1 H -0.3892 0.1012 0.5586 0.045 Uiso 0.50 1 calc PR . 2 H3X2 H -0.2703 0.0986 0.5616 0.045 Uiso 0.50 1 calc PR . 2 C5C C -0.1511(8) -0.1807(7) 0.5944(4) 0.043(2) Uani 0.50 1 d P . 1 H5C1 H -0.1779 -0.2155 0.5723 0.052 Uiso 0.50 1 calc PR . 1 H5C2 H -0.1863 -0.1866 0.6389 0.052 Uiso 0.50 1 calc PR . 1 C7C C 0.1467(9) -0.2923(9) 0.5135(6) 0.050(3) Uani 0.50 1 d P . 1 H7C1 H 0.1752 -0.3633 0.5391 0.060 Uiso 0.50 1 calc PR . 1 H7C2 H 0.1700 -0.2434 0.5263 0.060 Uiso 0.50 1 calc PR . 1 C6C C -0.0228(12) -0.2397(14) 0.5863(8) 0.051(4) Uani 0.50 1 d P . 1 H6C1 H 0.0060 -0.2003 0.6036 0.062 Uiso 0.50 1 calc PR . 1 H6C2 H 0.0000 -0.3141 0.6083 0.062 Uiso 0.50 1 calc PR . 1 O4X O 0.0983(6) -0.2450(5) 0.5224(3) 0.0393(15) Uani 0.50 1 d P . 2 C4C C -0.3082(11) -0.0107(12) 0.5737(8) 0.049(3) Uani 0.50 1 d P . 1 H4C1 H -0.3507 -0.0056 0.6171 0.058 Uiso 0.50 1 calc PR . 1 H4C2 H -0.3341 -0.0483 0.5530 0.058 Uiso 0.50 1 calc PR . 1 C2X C -0.3373(15) 0.1757(14) 0.4513(10) 0.041(3) Uani 0.50 1 d P . 2 H2X1 H -0.3280 0.2325 0.4659 0.049 Uiso 0.50 1 calc PR . 2 H2X2 H -0.4200 0.1920 0.4622 0.049 Uiso 0.50 1 calc PR . 2 C3C C -0.3312(16) 0.1009(14) 0.5412(12) 0.044(4) Uani 0.50 1 d P . 1 H3C1 H -0.4149 0.1482 0.5455 0.053 Uiso 0.50 1 calc PR . 1 H3C2 H -0.2962 0.1358 0.5575 0.053 Uiso 0.50 1 calc PR . 1 O3C O -0.1875(7) -0.0702(7) 0.5717(4) 0.0363(17) Uani 0.50 1 d P . 1 Na13 Na -0.0386(7) -0.0581(9) 0.4288(7) 0.048(2) Uani 0.50 1 d P . 2 O4 O -0.1379(8) -0.1249(11) 0.4001(7) 0.051(3) Uani 0.50 1 d P C 1 C1S C -0.0685(7) 0.6328(6) -0.2408(4) 0.0621(19) Uiso 0.50 1 d P A 1 O21 O 0.022(9) 0.504(8) 0.002(4) 0.118(12) Uani 0.25 1 d P . 2 C5S C -0.2672(14) 0.7145(14) -0.2304(7) 0.053(4) Uiso 0.25 1 d P B 2 C3S C -0.2173(12) 0.6675(10) -0.2392(5) 0.022(2) Uiso 0.25 1 d P A 1 C6S C -0.2071(12) 0.6303(12) -0.2618(7) 0.050(3) Uiso 0.25 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.0411(18) 0.056(2) 0.0290(16) 0.0004(14) -0.0080(17) -0.0118(18) Na11 0.0394(18) 0.060(2) 0.0367(18) -0.0093(14) -0.0040(18) -0.0157(19) O1 0.031(2) 0.038(2) 0.0241(19) 0.0004(16) -0.0070(17) -0.0045(17) O2 0.015(5) 0.023(4) 0.021(4) -0.004(4) -0.006(4) -0.012(4) O11 0.079(4) 0.047(3) 0.053(3) 0.001(2) -0.021(3) -0.027(3) C25 0.0233(13) 0.0232(13) 0.0267(13) -0.0033(11) -0.0060(11) -0.0063(11) C26 0.0259(13) 0.0246(13) 0.0299(14) -0.0035(11) -0.0046(12) -0.0083(11) C27 0.0289(14) 0.0271(14) 0.0308(14) 0.0006(11) -0.0008(12) -0.0100(12) C28 0.0329(15) 0.0379(16) 0.0246(14) 0.0008(12) -0.0028(12) -0.0105(13) C29 0.0319(14) 0.0337(15) 0.0275(14) -0.0066(12) -0.0073(12) -0.0079(13) C30 0.0282(14) 0.0315(15) 0.0286(14) -0.0038(11) -0.0044(12) -0.0127(12) C31 0.0286(13) 0.0184(12) 0.0258(13) -0.0021(10) -0.0068(11) -0.0113(11) C32 0.0294(14) 0.0273(14) 0.0289(14) -0.0064(11) -0.0060(12) -0.0105(12) C33 0.0309(14) 0.0282(14) 0.0317(14) -0.0094(12) 0.0004(12) -0.0121(12) C34 0.0251(13) 0.0280(14) 0.0440(16) -0.0109(12) -0.0037(13) -0.0117(12) C35 0.0298(14) 0.0282(14) 0.0385(16) -0.0036(12) -0.0135(13) -0.0114(12) C36 0.0309(14) 0.0261(13) 0.0269(13) -0.0027(11) -0.0049(12) -0.0145(12) C37 0.0254(13) 0.0272(14) 0.0212(12) -0.0016(10) -0.0026(11) -0.0134(11) C38 0.0294(14) 0.0296(14) 0.0247(13) -0.0016(11) -0.0061(11) -0.0141(12) C39 0.0406(16) 0.0295(15) 0.0305(14) -0.0018(12) -0.0064(13) -0.0184(13) C40 0.0406(16) 0.0470(18) 0.0339(15) -0.0082(13) -0.0068(13) -0.0286(15) C41 0.0327(15) 0.0454(18) 0.0419(17) -0.0043(14) -0.0137(14) -0.0187(14) C42 0.0302(14) 0.0330(15) 0.0346(15) -0.0015(12) -0.0106(13) -0.0134(12) C43 0.0247(13) 0.0281(14) 0.0277(13) -0.0024(11) -0.0064(11) -0.0140(11) C44 0.0248(13) 0.0282(14) 0.0299(14) -0.0033(11) -0.0060(12) -0.0118(11) C45 0.0274(14) 0.0282(14) 0.0418(16) -0.0098(12) -0.0056(13) -0.0086(12) C46 0.0395(16) 0.0259(15) 0.0467(18) 0.0022(13) -0.0074(15) -0.0113(13) C47 0.0487(18) 0.0337(17) 0.0384(17) 0.0070(13) 0.0027(15) -0.0130(15) C48 0.0408(16) 0.0260(14) 0.0315(15) -0.0034(12) 0.0016(13) -0.0077(13) C73 0.0280(14) 0.0355(15) 0.0253(13) -0.0072(12) -0.0049(12) -0.0153(12) C74 0.0312(14) 0.0372(15) 0.0281(14) -0.0041(12) -0.0060(12) -0.0173(13) C75 0.0341(15) 0.0476(18) 0.0320(15) -0.0051(13) -0.0007(13) -0.0227(14) C76 0.0268(14) 0.057(2) 0.0371(16) -0.0093(15) -0.0051(14) -0.0143(14) C77 0.0310(15) 0.057(2) 0.0356(16) -0.0031(15) -0.0104(14) -0.0131(15) C78 0.0318(15) 0.0479(18) 0.0259(14) 0.0000(13) -0.0061(13) -0.0166(14) C79 0.0284(14) 0.0382(16) 0.0208(13) -0.0015(11) -0.0026(11) -0.0161(13) C80 0.0289(14) 0.0378(16) 0.0338(15) -0.0061(13) -0.0057(13) -0.0145(13) C81 0.0353(15) 0.0517(19) 0.0346(15) -0.0052(14) -0.0074(13) -0.0244(15) C82 0.0424(16) 0.0476(18) 0.0260(14) -0.0054(13) -0.0010(13) -0.0298(15) C83 0.0419(17) 0.0383(17) 0.0372(16) -0.0119(13) -0.0040(14) -0.0174(14) C84 0.0313(15) 0.0422(17) 0.0341(15) -0.0066(13) -0.0062(13) -0.0147(13) C85 0.0213(12) 0.0275(14) 0.0287(14) -0.0060(11) -0.0035(11) -0.0063(11) C86 0.0252(13) 0.0245(13) 0.0316(14) -0.0032(11) -0.0048(12) -0.0059(11) C87 0.0329(15) 0.0282(14) 0.0334(15) 0.0032(12) -0.0033(13) -0.0111(12) C88 0.0284(14) 0.0365(16) 0.0279(14) 0.0021(12) -0.0030(12) -0.0043(13) C89 0.0340(15) 0.0419(17) 0.0266(14) -0.0062(12) -0.0080(13) -0.0115(14) C90 0.0309(14) 0.0398(16) 0.0301(14) -0.0018(12) -0.0074(12) -0.0163(13) C91 0.0198(12) 0.0369(15) 0.0291(14) -0.0025(12) -0.0067(11) -0.0136(12) C92 0.0317(15) 0.0424(17) 0.0348(15) -0.0017(13) -0.0119(13) -0.0169(13) C93 0.0371(16) 0.0484(19) 0.0432(17) 0.0109(15) -0.0198(15) -0.0191(15) C94 0.0397(17) 0.0348(17) 0.064(2) 0.0057(16) -0.0197(17) -0.0109(14) C95 0.0350(16) 0.0383(17) 0.057(2) -0.0140(15) -0.0091(16) -0.0082(14) C96 0.0265(14) 0.0388(16) 0.0381(16) -0.0055(13) -0.0061(13) -0.0122(13) B2 0.0257(15) 0.0244(15) 0.0265(15) -0.0012(12) -0.0066(13) -0.0115(13) B4 0.0264(15) 0.0349(17) 0.0264(15) -0.0052(13) -0.0060(13) -0.0145(14) O1A 0.0319(10) 0.0311(10) 0.0359(10) -0.0026(8) -0.0065(9) -0.0106(9) O2A 0.0315(10) 0.0279(10) 0.0360(10) -0.0052(8) -0.0048(9) -0.0086(8) O3A 0.0288(9) 0.0289(10) 0.0342(10) -0.0070(8) -0.0075(8) -0.0120(8) O4A 0.0310(10) 0.0281(10) 0.0392(11) -0.0059(8) -0.0110(9) -0.0084(8) O5A 0.0364(10) 0.0267(10) 0.0337(10) -0.0063(8) -0.0041(9) -0.0113(8) O6A 0.0332(10) 0.0375(11) 0.0304(10) -0.0095(8) -0.0026(9) -0.0148(9) C1A 0.0285(14) 0.0395(16) 0.0316(15) -0.0054(13) -0.0054(12) -0.0108(13) C2A 0.0266(14) 0.0411(17) 0.0381(16) -0.0079(13) -0.0017(13) -0.0131(13) C3A 0.0323(15) 0.0314(15) 0.0460(17) -0.0010(13) -0.0091(14) -0.0141(13) C4A 0.0319(14) 0.0264(14) 0.0431(16) -0.0030(12) -0.0131(13) -0.0112(12) C5A 0.0335(15) 0.0287(15) 0.0372(15) -0.0089(12) -0.0062(13) -0.0074(12) C6A 0.0322(15) 0.0287(15) 0.0398(16) -0.0059(12) -0.0030(13) -0.0102(12) C7A 0.0271(14) 0.0406(17) 0.0491(18) -0.0135(14) -0.0079(14) -0.0105(13) C8A 0.0344(15) 0.0399(17) 0.0394(16) -0.0130(13) 0.0033(13) -0.0176(14) C9A 0.0374(15) 0.0306(15) 0.0460(17) -0.0096(13) -0.0081(14) -0.0172(13) C10A 0.0422(16) 0.0283(14) 0.0389(16) -0.0104(12) -0.0109(14) -0.0136(13) C11A 0.0435(17) 0.0395(17) 0.0362(16) -0.0142(13) 0.0059(14) -0.0172(14) C12A 0.0351(16) 0.0307(15) 0.0429(17) -0.0055(13) 0.0030(14) -0.0102(13) Na3 0.044(4) 0.033(3) 0.040(2) -0.004(2) -0.013(3) -0.021(3) O14 0.081(6) 0.078(7) 0.091(8) -0.036(5) 0.026(4) -0.063(5) O5 0.033(3) 0.032(3) 0.030(3) -0.0051(18) -0.010(2) -0.014(2) O1X 0.040(8) 0.031(4) 0.040(5) -0.008(3) -0.006(6) -0.018(5) O2C 0.0308(11) 0.0469(13) 0.0428(12) -0.0101(10) -0.0081(10) -0.0090(10) O5C 0.059(9) 0.066(10) 0.062(11) -0.010(6) 0.006(6) -0.039(7) O6C 0.052(11) 0.025(8) 0.033(4) -0.007(6) 0.004(6) -0.013(7) C1X 0.035(8) 0.025(5) 0.048(13) 0.009(6) -0.014(8) 0.002(5) C5X 0.065(8) 0.037(6) 0.040(6) 0.011(4) -0.020(6) -0.028(6) C8C 0.055(8) 0.029(6) 0.070(13) 0.013(7) -0.016(8) 0.000(5) C9C 0.042(6) 0.043(12) 0.058(10) -0.016(9) -0.004(7) -0.012(8) C10C 0.040(10) 0.069(15) 0.046(7) -0.028(8) 0.004(6) -0.036(12) C11X 0.037(9) 0.038(7) 0.019(5) -0.013(4) 0.012(7) -0.021(7) C12C 0.070(14) 0.049(6) 0.010(5) -0.014(4) 0.022(9) -0.022(10) O3X 0.028(4) 0.044(4) 0.043(4) 0.008(3) -0.007(3) -0.022(3) O4C 0.044(3) 0.047(3) 0.035(3) -0.001(2) -0.015(2) -0.026(2) O5X 0.028(5) 0.011(5) 0.045(7) -0.018(4) 0.012(4) 0.007(4) O6X 0.037(7) 0.019(7) 0.035(4) 0.000(6) -0.011(5) -0.008(5) O1C 0.067(12) 0.052(5) 0.024(4) -0.003(3) -0.009(7) -0.034(8) C2C 0.030(7) 0.028(7) 0.052(7) 0.005(5) -0.010(5) -0.005(4) C4X 0.035(10) 0.073(9) 0.031(4) -0.009(5) 0.001(6) -0.038(7) C6X 0.074(11) 0.046(7) 0.058(7) 0.010(6) -0.025(8) -0.036(8) C10X 0.036(8) 0.056(11) 0.018(5) -0.004(5) 0.004(5) -0.017(8) C7X 0.043(4) 0.029(3) 0.050(4) -0.004(3) -0.005(4) -0.014(3) C8X 0.037(5) 0.019(6) 0.054(9) 0.004(6) -0.016(6) -0.012(4) C1C 0.072(17) 0.044(6) 0.029(9) -0.002(5) -0.010(10) -0.025(8) C12X 0.043(8) 0.026(4) 0.026(9) -0.003(5) -0.001(7) -0.006(5) C11C 0.059(11) 0.054(7) 0.036(5) -0.011(4) 0.024(8) -0.017(9) C9X 0.034(6) 0.036(11) 0.028(7) -0.021(7) 0.007(5) -0.012(9) C3X 0.031(8) 0.052(11) 0.035(5) -0.020(8) 0.006(5) -0.022(7) C5C 0.055(6) 0.040(5) 0.043(5) 0.006(4) -0.016(4) -0.029(5) C7C 0.054(7) 0.046(6) 0.053(6) 0.013(5) -0.029(6) -0.023(5) C6C 0.080(13) 0.054(9) 0.028(5) 0.018(5) -0.028(9) -0.035(11) O4X 0.058(5) 0.031(3) 0.034(3) 0.009(3) -0.018(3) -0.024(3) C4C 0.033(8) 0.071(10) 0.048(5) -0.010(6) 0.004(6) -0.033(6) C2X 0.038(7) 0.027(6) 0.057(9) -0.009(6) -0.006(6) -0.013(4) C3C 0.031(7) 0.044(10) 0.051(6) -0.016(8) 0.001(6) -0.012(6) O3C 0.025(5) 0.046(5) 0.040(4) 0.001(3) -0.003(4) -0.022(4) Na13 0.060(5) 0.062(6) 0.038(2) -0.014(4) -0.003(4) -0.039(4) O4 0.018(3) 0.052(5) 0.092(8) -0.030(5) -0.008(4) -0.016(3) O21 0.14(3) 0.17(3) 0.12(2) 0.11(2) -0.098(18) -0.14(2) _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 Na1 O2 2.307(14) 2_565 ? Na1 O2 2.383(15) . ? Na1 O1 2.389(5) . ? Na1 O3A 2.394(4) . ? Na1 O4A 2.523(4) . ? Na1 O5A 2.696(4) . ? Na1 O2A 2.851(4) . ? Na11 O21 2.24(4) 2_565 ? Na11 O21 2.27(4) . ? Na11 O11 2.320(6) . ? Na11 O2A 2.433(4) . ? Na11 O1A 2.481(4) . ? Na11 O3A 2.698(4) . ? Na11 O6A 2.854(4) . ? O1 C1S 1.566(9) . ? O2 O2 1.33(3) 2_565 ? O2 Na1 2.307(14) 2_565 ? O11 C4S 1.867(12) . ? C25 C26 1.403(3) . ? C25 C30 1.410(4) . ? C25 B2 1.650(4) . ? C26 C27 1.400(4) . ? C27 C28 1.380(4) . ? C28 C29 1.387(4) . ? C29 C30 1.390(4) . ? C31 C36 1.405(3) . ? C31 C32 1.411(3) . ? C31 B2 1.669(4) . ? C32 C33 1.390(4) . ? C33 C34 1.381(4) . ? C34 C35 1.390(4) . ? C35 C36 1.400(4) . ? C37 C42 1.402(4) . ? C37 C38 1.405(4) . ? C37 B2 1.643(4) . ? C38 C39 1.387(4) . ? C39 C40 1.390(4) . ? C40 C41 1.380(4) . ? C41 C42 1.393(4) . ? C43 C44 1.399(4) . ? C43 C48 1.406(4) . ? C43 B2 1.653(4) . ? C44 C45 1.394(4) . ? C45 C46 1.376(4) . ? C46 C47 1.382(4) . ? C47 C48 1.386(4) . ? C73 C78 1.389(4) . ? C73 C74 1.413(4) . ? C73 B4 1.660(4) . ? C74 C75 1.391(4) . ? C75 C76 1.386(4) . ? C76 C77 1.391(4) . ? C77 C78 1.390(4) . ? C79 C84 1.397(4) . ? C79 C80 1.405(4) . ? C79 B4 1.648(4) . ? C80 C81 1.389(4) . ? C81 C82 1.381(4) . ? C82 C83 1.381(4) . ? C83 C84 1.385(4) . ? C85 C86 1.400(4) . ? C85 C90 1.409(4) . ? C85 B4 1.646(4) . ? C86 C87 1.400(4) . ? C87 C88 1.379(4) . ? C88 C89 1.387(4) . ? C89 C90 1.391(4) . ? C91 C92 1.404(4) . ? C91 C96 1.412(4) . ? C91 B4 1.651(4) . ? C92 C93 1.388(4) . ? C93 C94 1.382(5) . ? C94 C95 1.385(5) . ? C95 C96 1.390(4) . ? O1A C1A 1.420(3) . ? O1A C12A 1.429(3) . ? O2A C3A 1.424(3) . ? O2A C2A 1.429(3) . ? O3A C4A 1.425(3) . ? O3A C5A 1.433(3) . ? O4A C7A 1.428(3) . ? O4A C6A 1.433(3) . ? O5A C8A 1.424(3) . ? O5A C9A 1.438(3) . ? O6A C11A 1.428(3) . ? O6A C10A 1.428(3) . ? C1A C2A 1.496(4) . ? C3A C4A 1.491(4) . ? C5A C6A 1.493(4) . ? C7A C8A 1.493(4) . ? C9A C10A 1.486(4) . ? C11A C12A 1.497(4) . ? C2S C1S 1.206(10) . ? C4S C6S 1.180(18) . ? C4S C5S 1.230(19) . ? Na3 O4 2.124(18) . ? Na3 O5 2.340(14) . ? Na3 O5 2.395(15) 2_556 ? Na3 O1C 2.43(3) . ? Na3 O2C 2.511(10) . ? Na3 O6C 2.56(3) . ? Na3 O5C 2.79(2) . ? O14 Na13 2.36(2) . ? O5 Na13 2.349(16) 2_556 ? O1X C12X 1.34(3) . ? O1X C1X 1.42(3) . ? O1X Na13 2.84(3) . ? O2C C2X 1.305(19) . ? O2C C3C 1.45(3) . ? O2C C3X 1.45(2) . ? O2C C2C 1.550(17) . ? O2C Na13 2.891(9) . ? O5C C8C 1.54(3) . ? O5C C9C 1.41(4) . ? O6C C10C 1.43(3) . ? O6C C11C 1.52(3) . ? C1X C2X 1.44(3) . ? C5X O3X 1.457(13) . ? C5X C6X 1.470(14) . ? C8C C7C 1.51(2) . ? C9C C10C 1.52(2) . ? C11X O6X 1.36(3) . ? C11X C12X 1.496(13) . ? C12C C11C 1.505(15) . ? C12C O1C 1.49(3) . ? O3X C4X 1.436(11) . ? O3X Na13 2.960(18) . ? O4C C6C 1.417(18) . ? O4C C7C 1.425(11) . ? O5X C8X 1.33(3) . ? O5X C9X 1.47(4) . ? O5X Na13 2.428(15) . ? O6X C10X 1.41(3) . ? O6X Na13 2.42(3) . ? O1C C1C 1.45(3) . ? C2C C1C 1.54(3) . ? C4X C3X 1.46(2) . ? C6X O4X 1.45(2) . ? C10X C9X 1.48(2) . ? C7X O4X 1.421(10) . ? C7X C8X 1.475(18) . ? C5C O3C 1.403(12) . ? C5C C6C 1.496(14) . ? C4C O3C 1.424(11) . ? C4C C3C 1.50(2) . ? Na13 O5 2.349(16) 2_556 ? C1S C3S 1.812(14) . ? O21 O21 0.70(5) 2_565 ? O21 Na11 2.24(4) 2_565 ? 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 Na1 O2 32.9(7) 2_565 . ? O2 Na1 O1 130.0(4) 2_565 . ? O2 Na1 O1 161.0(4) . . ? O2 Na1 O3A 114.1(5) 2_565 . ? O2 Na1 O3A 85.0(5) . . ? O1 Na1 O3A 104.90(18) . . ? O2 Na1 O4A 93.2(5) 2_565 . ? O2 Na1 O4A 67.9(5) . . ? O1 Na1 O4A 130.62(17) . . ? O3A Na1 O4A 68.73(11) . . ? O2 Na1 O5A 81.5(7) 2_565 . ? O2 Na1 O5A 89.6(6) . . ? O1 Na1 O5A 95.41(16) . . ? O3A Na1 O5A 131.58(14) . . ? O4A Na1 O5A 64.74(10) . . ? O2 Na1 O2A 91.6(6) 2_565 . ? O2 Na1 O2A 91.7(6) . . ? O1 Na1 O2A 78.86(14) . . ? O3A Na1 O2A 63.34(11) . . ? O4A Na1 O2A 129.22(16) . . ? O5A Na1 O2A 165.07(15) . . ? O21 Na11 O21 17.9(12) 2_565 . ? O21 Na11 O11 124.5(10) 2_565 . ? O21 Na11 O11 141.8(14) . . ? O21 Na11 O2A 113.2(8) 2_565 . ? O21 Na11 O2A 95.5(6) . . ? O11 Na11 O2A 118.7(2) . . ? O21 Na11 O1A 112(3) 2_565 . ? O21 Na11 O1A 104(3) . . ? O11 Na11 O1A 103.74(19) . . ? O2A Na11 O1A 69.28(11) . . ? O21 Na11 O3A 94(3) 2_565 . ? O21 Na11 O3A 89(3) . . ? O11 Na11 O3A 90.56(17) . . ? O2A Na11 O3A 65.42(11) . . ? O1A Na11 O3A 133.84(16) . . ? O21 Na11 O6A 79(3) 2_565 . ? O21 Na11 O6A 88(3) . . ? O11 Na11 O6A 81.66(16) . . ? O2A Na11 O6A 131.08(14) . . ? O1A Na11 O6A 62.53(10) . . ? O3A Na11 O6A 163.48(14) . . ? C1S O1 Na1 123.8(4) . . ? O2 O2 Na1 76.7(12) 2_565 2_565 ? O2 O2 Na1 70.4(12) 2_565 . ? Na1 O2 Na1 147.1(7) 2_565 . ? C4S O11 Na11 159.9(4) . . ? C26 C25 C30 114.8(2) . . ? C26 C25 B2 123.1(2) . . ? C30 C25 B2 122.1(2) . . ? C27 C26 C25 123.0(2) . . ? C28 C27 C26 120.1(3) . . ? C27 C28 C29 118.8(2) . . ? C28 C29 C30 120.6(3) . . ? C29 C30 C25 122.7(2) . . ? C36 C31 C32 114.2(2) . . ? C36 C31 B2 125.4(2) . . ? C32 C31 B2 120.4(2) . . ? C33 C32 C31 123.5(3) . . ? C34 C33 C32 120.4(3) . . ? C33 C34 C35 118.5(2) . . ? C34 C35 C36 120.4(3) . . ? C35 C36 C31 123.0(2) . . ? C42 C37 C38 114.7(2) . . ? C42 C37 B2 124.6(2) . . ? C38 C37 B2 120.5(2) . . ? C39 C38 C37 123.4(2) . . ? C38 C39 C40 119.7(3) . . ? C41 C40 C39 119.0(3) . . ? C40 C41 C42 120.4(3) . . ? C41 C42 C37 122.8(3) . . ? C44 C43 C48 114.0(2) . . ? C44 C43 B2 124.6(2) . . ? C48 C43 B2 121.4(2) . . ? C45 C44 C43 123.3(2) . . ? C46 C45 C44 120.3(3) . . ? C45 C46 C47 118.7(3) . . ? C46 C47 C48 120.2(3) . . ? C47 C48 C43 123.5(3) . . ? C78 C73 C74 114.8(2) . . ? C78 C73 B4 122.6(2) . . ? C74 C73 B4 122.4(2) . . ? C75 C74 C73 122.7(3) . . ? C76 C75 C74 120.0(3) . . ? C75 C76 C77 119.1(3) . . ? C78 C77 C76 119.5(3) . . ? C73 C78 C77 123.8(3) . . ? C84 C79 C80 114.9(2) . . ? C84 C79 B4 121.5(2) . . ? C80 C79 B4 123.2(2) . . ? C81 C80 C79 122.6(3) . . ? C82 C81 C80 120.5(3) . . ? C83 C82 C81 118.6(3) . . ? C82 C83 C84 120.3(3) . . ? C83 C84 C79 123.1(3) . . ? C86 C85 C90 114.6(2) . . ? C86 C85 B4 123.7(2) . . ? C90 C85 B4 121.7(2) . . ? C85 C86 C87 123.2(3) . . ? C88 C87 C86 119.8(3) . . ? C87 C88 C89 119.3(3) . . ? C88 C89 C90 119.9(3) . . ? C89 C90 C85 123.2(3) . . ? C92 C91 C96 114.1(2) . . ? C92 C91 B4 121.1(2) . . ? C96 C91 B4 124.7(2) . . ? C93 C92 C91 123.6(3) . . ? C94 C93 C92 120.2(3) . . ? C93 C94 C95 118.7(3) . . ? C94 C95 C96 120.5(3) . . ? C95 C96 C91 122.9(3) . . ? C37 B2 C25 109.2(2) . . ? C37 B2 C43 109.5(2) . . ? C25 B2 C43 110.4(2) . . ? C37 B2 C31 107.8(2) . . ? C25 B2 C31 110.9(2) . . ? C43 B2 C31 109.0(2) . . ? C85 B4 C79 108.2(2) . . ? C85 B4 C91 111.8(2) . . ? C79 B4 C91 110.4(2) . . ? C85 B4 C73 108.8(2) . . ? C79 B4 C73 108.4(2) . . ? C91 B4 C73 109.2(2) . . ? C1A O1A C12A 112.0(2) . . ? C1A O1A Na11 110.37(17) . . ? C12A O1A Na11 121.69(18) . . ? C3A O2A C2A 111.7(2) . . ? C3A O2A Na11 113.29(17) . . ? C2A O2A Na11 111.80(17) . . ? C3A O2A Na1 102.49(16) . . ? C2A O2A Na1 121.79(17) . . ? Na11 O2A Na1 11.67(11) . . ? C4A O3A C5A 111.0(2) . . ? C4A O3A Na1 124.63(17) . . ? C5A O3A Na1 114.78(17) . . ? C4A O3A Na11 110.90(16) . . ? C5A O3A Na11 125.21(17) . . ? Na1 O3A Na11 13.74(9) . . ? C7A O4A C6A 111.4(2) . . ? C7A O4A Na1 114.16(18) . . ? C6A O4A Na1 110.12(17) . . ? C8A O5A C9A 110.6(2) . . ? C8A O5A Na1 111.88(17) . . ? C9A O5A Na1 124.69(17) . . ? C11A O6A C10A 111.0(2) . . ? C11A O6A Na11 108.57(17) . . ? C10A O6A Na11 118.56(16) . . ? O1A C1A C2A 107.7(2) . . ? O2A C2A C1A 109.1(2) . . ? O2A C3A C4A 108.7(2) . . ? O3A C4A C3A 108.6(2) . . ? O3A C5A C6A 108.5(2) . . ? O4A C6A C5A 108.8(2) . . ? O4A C7A C8A 108.7(2) . . ? O5A C8A C7A 109.1(2) . . ? O5A C9A C10A 109.7(2) . . ? O6A C10A C9A 109.1(2) . . ? O6A C11A C12A 109.5(2) . . ? O1A C12A C11A 108.2(2) . . ? C6S C4S C5S 65.3(13) . . ? C6S C4S O11 145.7(10) . . ? C5S C4S O11 111.8(10) . . ? O4 Na3 O5 150.1(7) . . ? O4 Na3 O5 147.8(8) . 2_556 ? O5 Na3 O5 20.32(19) . 2_556 ? O4 Na3 O1C 100.9(8) . . ? O5 Na3 O1C 109.0(8) . . ? O5 Na3 O1C 103.8(8) 2_556 . ? O4 Na3 O2C 86.0(5) . . ? O5 Na3 O2C 102.6(5) . . ? O5 Na3 O2C 82.3(4) 2_556 . ? O1C Na3 O2C 72.0(6) . . ? O4 Na3 O6C 91.1(9) . . ? O5 Na3 O6C 99.9(7) . . ? O5 Na3 O6C 117.0(8) 2_556 . ? O1C Na3 O6C 68.6(8) . . ? O2C Na3 O6C 139.1(6) . . ? O4 Na3 O5C 93.9(7) . . ? O5 Na3 O5C 69.3(6) . . ? O5 Na3 O5C 88.5(6) 2_556 . ? O1C Na3 O5C 125.5(10) . . ? O2C Na3 O5C 162.0(9) . . ? O6C Na3 O5C 58.8(8) . . ? Na3 O5 Na13 150.1(4) . 2_556 ? C12X O1X C1X 114(2) . . ? C12X O1X Na13 106.4(14) . . ? C1X O1X Na13 115.2(16) . . ? C2X O2C C3C 97.9(11) . . ? C2X O2C C3X 116.8(10) . . ? C3C O2C C3X 18.9(9) . . ? C2X O2C C2C 16.7(10) . . ? C3C O2C C2C 104.6(11) . . ? C3X O2C C2C 122.8(10) . . ? C2X O2C Na3 120.5(8) . . ? C3C O2C Na3 131.7(8) . . ? C3X O2C Na3 115.9(7) . . ? C2C O2C Na3 106.4(7) . . ? C2X O2C Na13 124.3(8) . . ? C3C O2C Na13 127.8(7) . . ? C3X O2C Na13 111.8(7) . . ? C2C O2C Na13 109.9(7) . . ? Na3 O2C Na13 4.1(6) . . ? C8C O5C C9C 108.0(17) . . ? C8C O5C Na3 125.0(16) . . ? C9C O5C Na3 117.1(19) . . ? C10C O6C C11C 107(2) . . ? C10C O6C Na3 122.5(17) . . ? C11C O6C Na3 112.2(12) . . ? O1X C1X C2X 115(2) . . ? O3X C5X C6X 108.7(12) . . ? O5C C8C C7C 107.8(16) . . ? O5C C9C C10C 106(2) . . ? O6C C10C C9C 105(2) . . ? O6X C11X C12X 109.4(16) . . ? C11C C12C O1C 108.4(18) . . ? C4X O3X C5X 112.2(9) . . ? C4X O3X Na13 111.3(8) . . ? C5X O3X Na13 110.6(6) . . ? C6C O4C C7C 108.5(9) . . ? C8X O5X C9X 113.7(16) . . ? C8X O5X Na13 127.4(18) . . ? C9X O5X Na13 111.5(14) . . ? C11X O6X C10X 116(2) . . ? C11X O6X Na13 124.3(14) . . ? C10X O6X Na13 107.5(15) . . ? C1C O1C C12C 108(2) . . ? C1C O1C Na3 107.7(17) . . ? C12C O1C Na3 112.3(16) . . ? C1C C2C O2C 106.5(15) . . ? O3X C4X C3X 110.0(12) . . ? O4X C6X C5X 113.2(16) . . ? O6X C10X C9X 112.0(19) . . ? O4X C7X C8X 106.3(8) . . ? O5X C8X C7X 111.6(16) . . ? O1C C1C C2C 104(2) . . ? O1X C12X C11X 108.6(19) . . ? C12C C11C O6C 104.9(17) . . ? O5X C9X C10X 110.3(17) . . ? O2C C3X C4X 114.1(13) . . ? O3C C5C C6C 111.6(10) . . ? O4C C7C C8C 108.2(11) . . ? O4C C6C C5C 108.0(11) . . ? C7X O4X C6X 113.1(10) . . ? O3C C4C C3C 108.2(13) . . ? O2C C2X C1X 108.4(16) . . ? O2C C3C C4C 102.9(13) . . ? C5C O3C C4C 114.7(10) . . ? O5 Na13 O14 134.9(8) 2_556 . ? O5 Na13 O6X 121.3(8) 2_556 . ? O14 Na13 O6X 101.7(9) . . ? O5 Na13 O5X 102.4(7) 2_556 . ? O14 Na13 O5X 103.5(8) . . ? O6X Na13 O5X 71.7(8) . . ? O5 Na13 O1X 97.8(7) 2_556 . ? O14 Na13 O1X 90.7(7) . . ? O6X Na13 O1X 61.5(7) . . ? O5X Na13 O1X 132.9(10) . . ? O5 Na13 O2C 75.3(4) 2_556 . ? O14 Na13 O2C 73.3(5) . . ? O6X Na13 O2C 117.1(5) . . ? O5X Na13 O2C 171.0(9) . . ? O1X Na13 O2C 56.0(5) . . ? O5 Na13 O3X 57.2(4) 2_556 . ? O14 Na13 O3X 79.3(6) . . ? O6X Na13 O3X 177.3(6) . . ? O5X Na13 O3X 110.6(8) . . ? O1X Na13 O3X 116.1(6) . . ? O2C Na13 O3X 60.7(3) . . ? C2S C1S O1 160.1(8) . . ? C2S C1S C3S 59.9(6) . . ? O1 C1S C3S 137.9(7) . . ? O21 O21 Na11 84(7) 2_565 2_565 ? O21 O21 Na11 79(7) 2_565 . ? Na11 O21 Na11 162.1(12) 2_565 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Na1 O1 C1S 103.4(9) 2_565 . . . ? O2 Na1 O1 C1S 124.6(19) . . . . ? O3A Na1 O1 C1S -115.7(4) . . . . ? O4A Na1 O1 C1S -41.2(5) . . . . ? O5A Na1 O1 C1S 19.9(4) . . . . ? O2A Na1 O1 C1S -174.0(4) . . . . ? O1 Na1 O2 O2 -31(4) . . . 2_565 ? O3A Na1 O2 O2 -153(2) . . . 2_565 ? O4A Na1 O2 O2 138(2) . . . 2_565 ? O5A Na1 O2 O2 75(2) . . . 2_565 ? O2A Na1 O2 O2 -90(2) . . . 2_565 ? O2 Na1 O2 Na1 0.000(2) 2_565 . . 2_565 ? O1 Na1 O2 Na1 -31(4) . . . 2_565 ? O3A Na1 O2 Na1 -153(2) . . . 2_565 ? O4A Na1 O2 Na1 138(2) . . . 2_565 ? O5A Na1 O2 Na1 75(2) . . . 2_565 ? O2A Na1 O2 Na1 -90(2) . . . 2_565 ? O21 Na11 O11 C4S -111(4) 2_565 . . . ? O21 Na11 O11 C4S -117(5) . . . . ? O2A Na11 O11 C4S 92.1(13) . . . . ? O1A Na11 O11 C4S 18.5(13) . . . . ? O3A Na11 O11 C4S 154.1(13) . . . . ? O6A Na11 O11 C4S -40.5(13) . . . . ? C30 C25 C26 C27 -0.8(4) . . . . ? B2 C25 C26 C27 179.9(2) . . . . ? C25 C26 C27 C28 0.4(4) . . . . ? C26 C27 C28 C29 0.1(4) . . . . ? C27 C28 C29 C30 -0.2(4) . . . . ? C28 C29 C30 C25 -0.3(4) . . . . ? C26 C25 C30 C29 0.7(4) . . . . ? B2 C25 C30 C29 -179.9(2) . . . . ? C36 C31 C32 C33 -1.5(4) . . . . ? B2 C31 C32 C33 179.4(2) . . . . ? C31 C32 C33 C34 1.5(4) . . . . ? C32 C33 C34 C35 -0.4(4) . . . . ? C33 C34 C35 C36 -0.7(4) . . . . ? C34 C35 C36 C31 0.7(4) . . . . ? C32 C31 C36 C35 0.3(4) . . . . ? B2 C31 C36 C35 179.4(2) . . . . ? C42 C37 C38 C39 -0.5(4) . . . . ? B2 C37 C38 C39 175.4(2) . . . . ? C37 C38 C39 C40 1.2(4) . . . . ? C38 C39 C40 C41 -0.6(4) . . . . ? C39 C40 C41 C42 -0.7(4) . . . . ? C40 C41 C42 C37 1.5(4) . . . . ? C38 C37 C42 C41 -0.8(4) . . . . ? B2 C37 C42 C41 -176.5(2) . . . . ? C48 C43 C44 C45 -2.2(4) . . . . ? B2 C43 C44 C45 179.3(2) . . . . ? C43 C44 C45 C46 0.9(4) . . . . ? C44 C45 C46 C47 0.9(4) . . . . ? C45 C46 C47 C48 -1.2(5) . . . . ? C46 C47 C48 C43 -0.2(5) . . . . ? C44 C43 C48 C47 1.8(4) . . . . ? B2 C43 C48 C47 -179.6(3) . . . . ? C78 C73 C74 C75 -0.8(4) . . . . ? B4 C73 C74 C75 -176.4(3) . . . . ? C73 C74 C75 C76 0.8(4) . . . . ? C74 C75 C76 C77 -0.5(4) . . . . ? C75 C76 C77 C78 0.3(5) . . . . ? C74 C73 C78 C77 0.6(4) . . . . ? B4 C73 C78 C77 176.2(3) . . . . ? C76 C77 C78 C73 -0.4(5) . . . . ? C84 C79 C80 C81 1.0(4) . . . . ? B4 C79 C80 C81 -172.0(3) . . . . ? C79 C80 C81 C82 0.7(4) . . . . ? C80 C81 C82 C83 -1.5(4) . . . . ? C81 C82 C83 C84 0.6(4) . . . . ? C82 C83 C84 C79 1.3(4) . . . . ? C80 C79 C84 C83 -2.0(4) . . . . ? B4 C79 C84 C83 171.1(3) . . . . ? C90 C85 C86 C87 0.3(4) . . . . ? B4 C85 C86 C87 178.0(3) . . . . ? C85 C86 C87 C88 0.7(4) . . . . ? C86 C87 C88 C89 -0.9(4) . . . . ? C87 C88 C89 C90 0.2(4) . . . . ? C88 C89 C90 C85 0.9(4) . . . . ? C86 C85 C90 C89 -1.1(4) . . . . ? B4 C85 C90 C89 -178.8(3) . . . . ? C96 C91 C92 C93 1.6(4) . . . . ? B4 C91 C92 C93 -175.7(2) . . . . ? C91 C92 C93 C94 -0.6(4) . . . . ? C92 C93 C94 C95 -0.5(4) . . . . ? C93 C94 C95 C96 0.5(4) . . . . ? C94 C95 C96 C91 0.7(4) . . . . ? C92 C91 C96 C95 -1.6(4) . . . . ? B4 C91 C96 C95 175.6(2) . . . . ? C42 C37 B2 C25 101.5(3) . . . . ? C38 C37 B2 C25 -74.0(3) . . . . ? C42 C37 B2 C43 -19.5(3) . . . . ? C38 C37 B2 C43 165.1(2) . . . . ? C42 C37 B2 C31 -137.9(2) . . . . ? C38 C37 B2 C31 46.6(3) . . . . ? C26 C25 B2 C37 0.4(3) . . . . ? C30 C25 B2 C37 -178.8(2) . . . . ? C26 C25 B2 C43 120.9(2) . . . . ? C30 C25 B2 C43 -58.4(3) . . . . ? C26 C25 B2 C31 -118.2(2) . . . . ? C30 C25 B2 C31 62.6(3) . . . . ? C44 C43 B2 C37 117.0(3) . . . . ? C48 C43 B2 C37 -61.5(3) . . . . ? C44 C43 B2 C25 -3.3(3) . . . . ? C48 C43 B2 C25 178.3(2) . . . . ? C44 C43 B2 C31 -125.3(2) . . . . ? C48 C43 B2 C31 56.2(3) . . . . ? C36 C31 B2 C37 -134.3(2) . . . . ? C32 C31 B2 C37 44.7(3) . . . . ? C36 C31 B2 C25 -14.9(3) . . . . ? C32 C31 B2 C25 164.2(2) . . . . ? C36 C31 B2 C43 106.8(3) . . . . ? C32 C31 B2 C43 -74.1(3) . . . . ? C86 C85 B4 C79 -5.7(3) . . . . ? C90 C85 B4 C79 171.8(2) . . . . ? C86 C85 B4 C91 116.1(3) . . . . ? C90 C85 B4 C91 -66.5(3) . . . . ? C86 C85 B4 C73 -123.2(3) . . . . ? C90 C85 B4 C73 54.3(3) . . . . ? C84 C79 B4 C85 -88.2(3) . . . . ? C80 C79 B4 C85 84.3(3) . . . . ? C84 C79 B4 C91 149.2(2) . . . . ? C80 C79 B4 C91 -38.3(3) . . . . ? C84 C79 B4 C73 29.6(3) . . . . ? C80 C79 B4 C73 -157.8(2) . . . . ? C92 C91 B4 C85 -161.0(2) . . . . ? C96 C91 B4 C85 21.9(3) . . . . ? C92 C91 B4 C79 -40.6(3) . . . . ? C96 C91 B4 C79 142.4(2) . . . . ? C92 C91 B4 C73 78.4(3) . . . . ? C96 C91 B4 C73 -98.6(3) . . . . ? C78 C73 B4 C85 22.6(3) . . . . ? C74 C73 B4 C85 -162.1(2) . . . . ? C78 C73 B4 C79 -94.8(3) . . . . ? C74 C73 B4 C79 80.5(3) . . . . ? C78 C73 B4 C91 144.9(3) . . . . ? C74 C73 B4 C91 -39.8(3) . . . . ? O21 Na11 O1A C1A -89.0(15) 2_565 . . . ? O21 Na11 O1A C1A -72.1(15) . . . . ? O11 Na11 O1A C1A 134.5(2) . . . . ? O2A Na11 O1A C1A 18.66(18) . . . . ? O3A Na11 O1A C1A 30.1(3) . . . . ? O6A Na11 O1A C1A -152.65(17) . . . . ? O21 Na11 O1A C12A 45.4(16) 2_565 . . . ? O21 Na11 O1A C12A 62.3(15) . . . . ? O11 Na11 O1A C12A -91.1(3) . . . . ? O2A Na11 O1A C12A 153.1(2) . . . . ? O3A Na11 O1A C12A 164.5(2) . . . . ? O6A Na11 O1A C12A -18.3(2) . . . . ? O21 Na11 O2A C3A -112(4) 2_565 . . . ? O21 Na11 O2A C3A -115(3) . . . . ? O11 Na11 O2A C3A 47.6(3) . . . . ? O1A Na11 O2A C3A 142.29(18) . . . . ? O3A Na11 O2A C3A -28.63(18) . . . . ? O6A Na11 O2A C3A 152.5(2) . . . . ? O21 Na11 O2A C2A 121(4) 2_565 . . . ? O21 Na11 O2A C2A 118(3) . . . . ? O11 Na11 O2A C2A -79.7(3) . . . . ? O1A Na11 O2A C2A 15.02(18) . . . . ? O3A Na11 O2A C2A -155.90(17) . . . . ? O6A Na11 O2A C2A 25.3(3) . . . . ? O21 Na11 O2A Na1 -89(4) 2_565 . . . ? O21 Na11 O2A Na1 -92(4) . . . . ? O11 Na11 O2A Na1 70.6(7) . . . . ? O1A Na11 O2A Na1 165.3(8) . . . . ? O3A Na11 O2A Na1 -5.6(7) . . . . ? O6A Na11 O2A Na1 175.5(9) . . . . ? O2 Na1 O2A C3A -144.4(4) 2_565 . . . ? O2 Na1 O2A C3A -111.5(4) . . . . ? O1 Na1 O2A C3A 85.06(19) . . . . ? O3A Na1 O2A C3A -28.03(17) . . . . ? O4A Na1 O2A C3A -49.0(2) . . . . ? O5A Na1 O2A C3A 153.6(6) . . . . ? O2 Na1 O2A C2A 90.0(4) 2_565 . . . ? O2 Na1 O2A C2A 122.9(4) . . . . ? O1 Na1 O2A C2A -40.6(2) . . . . ? O3A Na1 O2A C2A -153.66(19) . . . . ? O4A Na1 O2A C2A -174.7(2) . . . . ? O5A Na1 O2A C2A 28.0(7) . . . . ? O2 Na1 O2A Na11 57.2(8) 2_565 . . . ? O2 Na1 O2A Na11 90.0(8) . . . . ? O1 Na1 O2A Na11 -73.4(7) . . . . ? O3A Na1 O2A Na11 173.5(8) . . . . ? O4A Na1 O2A Na11 152.5(9) . . . . ? O5A Na1 O2A Na11 -4.8(4) . . . . ? O2 Na1 O3A C4A 75.3(6) 2_565 . . . ? O2 Na1 O3A C4A 90.8(6) . . . . ? O1 Na1 O3A C4A -72.7(2) . . . . ? O4A Na1 O3A C4A 159.0(2) . . . . ? O5A Na1 O3A C4A 175.8(2) . . . . ? O2A Na1 O3A C4A -3.7(2) . . . . ? O2 Na1 O3A C5A -67.8(6) 2_565 . . . ? O2 Na1 O3A C5A -52.2(6) . . . . ? O1 Na1 O3A C5A 144.21(19) . . . . ? O4A Na1 O3A C5A 15.94(17) . . . . ? O5A Na1 O3A C5A 32.7(3) . . . . ? O2A Na1 O3A C5A -146.72(17) . . . . ? O2 Na1 O3A Na11 74.0(8) 2_565 . . . ? O2 Na1 O3A Na11 89.5(8) . . . . ? O1 Na1 O3A Na11 -74.0(6) . . . . ? O4A Na1 O3A Na11 157.7(7) . . . . ? O5A Na1 O3A Na11 174.5(8) . . . . ? O2A Na1 O3A Na11 -5.0(6) . . . . ? O21 Na11 O3A C4A 109.2(12) 2_565 . . . ? O21 Na11 O3A C4A 92.0(14) . . . . ? O11 Na11 O3A C4A -126.2(2) . . . . ? O2A Na11 O3A C4A -4.57(18) . . . . ? O1A Na11 O3A C4A -16.4(3) . . . . ? O6A Na11 O3A C4A 172.3(5) . . . . ? O21 Na11 O3A C5A -28.5(12) 2_565 . . . ? O21 Na11 O3A C5A -45.7(14) . . . . ? O11 Na11 O3A C5A 96.1(2) . . . . ? O2A Na11 O3A C5A -142.26(19) . . . . ? O1A Na11 O3A C5A -154.1(2) . . . . ? O6A Na11 O3A C5A 34.6(6) . . . . ? O21 Na11 O3A Na1 -71.9(13) 2_565 . . . ? O21 Na11 O3A Na1 -89.1(15) . . . . ? O11 Na11 O3A Na1 52.7(6) . . . . ? O2A Na11 O3A Na1 174.3(7) . . . . ? O1A Na11 O3A Na1 162.5(8) . . . . ? O6A Na11 O3A Na1 -8.8(3) . . . . ? O2 Na1 O4A C7A -102.6(6) 2_565 . . . ? O2 Na1 O4A C7A -124.1(6) . . . . ? O1 Na1 O4A C7A 51.0(3) . . . . ? O3A Na1 O4A C7A 142.68(19) . . . . ? O5A Na1 O4A C7A -23.52(18) . . . . ? O2A Na1 O4A C7A 162.8(2) . . . . ? O2 Na1 O4A C6A 131.3(6) 2_565 . . . ? O2 Na1 O4A C6A 109.8(6) . . . . ? O1 Na1 O4A C6A -75.2(3) . . . . ? O3A Na1 O4A C6A 16.55(18) . . . . ? O5A Na1 O4A C6A -149.65(18) . . . . ? O2A Na1 O4A C6A 36.7(3) . . . . ? O2 Na1 O5A C8A 87.7(4) 2_565 . . . ? O2 Na1 O5A C8A 55.7(4) . . . . ? O1 Na1 O5A C8A -142.64(19) . . . . ? O3A Na1 O5A C8A -27.2(3) . . . . ? O4A Na1 O5A C8A -9.92(18) . . . . ? O2A Na1 O5A C8A 150.8(6) . . . . ? O2 Na1 O5A C9A -50.1(4) 2_565 . . . ? O2 Na1 O5A C9A -82.1(4) . . . . ? O1 Na1 O5A C9A 79.6(2) . . . . ? O3A Na1 O5A C9A -165.0(2) . . . . ? O4A Na1 O5A C9A -147.7(2) . . . . ? O2A Na1 O5A C9A 13.1(7) . . . . ? O21 Na11 O6A C11A -137.5(19) 2_565 . . . ? O21 Na11 O6A C11A -122(2) . . . . ? O11 Na11 O6A C11A 94.8(2) . . . . ? O2A Na11 O6A C11A -26.3(3) . . . . ? O1A Na11 O6A C11A -15.49(18) . . . . ? O3A Na11 O6A C11A 157.4(6) . . . . ? O21 Na11 O6A C10A 94.6(19) 2_565 . . . ? O21 Na11 O6A C10A 110(2) . . . . ? O11 Na11 O6A C10A -33.1(2) . . . . ? O2A Na11 O6A C10A -154.2(2) . . . . ? O1A Na11 O6A C10A -143.36(19) . . . . ? O3A Na11 O6A C10A 29.6(6) . . . . ? C12A O1A C1A C2A 172.5(2) . . . . ? Na11 O1A C1A C2A -48.5(3) . . . . ? C3A O2A C2A C1A -174.1(2) . . . . ? Na11 O2A C2A C1A -46.0(3) . . . . ? Na1 O2A C2A C1A -52.8(3) . . . . ? O1A C1A C2A O2A 64.2(3) . . . . ? C2A O2A C3A C4A -172.5(2) . . . . ? Na11 O2A C3A C4A 60.2(3) . . . . ? Na1 O2A C3A C4A 55.6(2) . . . . ? C5A O3A C4A C3A 178.6(2) . . . . ? Na1 O3A C4A C3A 34.4(3) . . . . ? Na11 O3A C4A C3A 34.7(2) . . . . ? O2A C3A C4A O3A -62.7(3) . . . . ? C4A O3A C5A C6A 166.3(2) . . . . ? Na1 O3A C5A C6A -45.7(3) . . . . ? Na11 O3A C5A C6A -56.0(3) . . . . ? C7A O4A C6A C5A -173.2(2) . . . . ? Na1 O4A C6A C5A -45.5(3) . . . . ? O3A C5A C6A O4A 61.0(3) . . . . ? C6A O4A C7A C8A 180.0(2) . . . . ? Na1 O4A C7A C8A 54.5(3) . . . . ? C9A O5A C8A C7A -176.1(2) . . . . ? Na1 O5A C8A C7A 40.1(3) . . . . ? O4A C7A C8A O5A -63.1(3) . . . . ? C8A O5A C9A C10A 178.5(2) . . . . ? Na1 O5A C9A C10A -43.3(3) . . . . ? C11A O6A C10A C9A 176.9(2) . . . . ? Na11 O6A C10A C9A -56.4(3) . . . . ? O5A C9A C10A O6A 64.0(3) . . . . ? C10A O6A C11A C12A 176.6(2) . . . . ? Na11 O6A C11A C12A 44.6(3) . . . . ? C1A O1A C12A C11A -177.2(2) . . . . ? Na11 O1A C12A C11A 49.1(3) . . . . ? O6A C11A C12A O1A -61.5(3) . . . . ? Na11 O11 C4S C6S 83(3) . . . . ? Na11 O11 C4S C5S 160.5(11) . . . . ? O4 Na3 O5 Na13 -109.8(13) . . . 2_556 ? O5 Na3 O5 Na13 -8.8(13) 2_556 . . 2_556 ? O1C Na3 O5 Na13 69.4(18) . . . 2_556 ? O2C Na3 O5 Na13 -5.6(17) . . . 2_556 ? O6C Na3 O5 Na13 140.0(12) . . . 2_556 ? O5C Na3 O5 Na13 -168.9(14) . . . 2_556 ? O4 Na3 O2C C2X -103.0(11) . . . . ? O5 Na3 O2C C2X 106.0(11) . . . . ? O5 Na3 O2C C2X 107.1(10) 2_556 . . . ? O1C Na3 O2C C2X -0.1(12) . . . . ? O6C Na3 O2C C2X -15.9(16) . . . . ? O5C Na3 O2C C2X 167(2) . . . . ? O4 Na3 O2C C3C 119.4(14) . . . . ? O5 Na3 O2C C3C -31.6(15) . . . . ? O5 Na3 O2C C3C -30.5(14) 2_556 . . . ? O1C Na3 O2C C3C -137.8(15) . . . . ? O6C Na3 O2C C3C -153.5(17) . . . . ? O5C Na3 O2C C3C 29(3) . . . . ? O4 Na3 O2C C3X 106.9(10) . . . . ? O5 Na3 O2C C3X -44.1(10) . . . . ? O5 Na3 O2C C3X -43.0(10) 2_556 . . . ? O1C Na3 O2C C3X -150.3(11) . . . . ? O6C Na3 O2C C3X -166.0(14) . . . . ? O5C Na3 O2C C3X 17(3) . . . . ? O4 Na3 O2C C2C -112.7(9) . . . . ? O5 Na3 O2C C2C 96.3(9) . . . . ? O5 Na3 O2C C2C 97.4(9) 2_556 . . . ? O1C Na3 O2C C2C -9.9(11) . . . . ? O6C Na3 O2C C2C -25.7(15) . . . . ? O5C Na3 O2C C2C 157(2) . . . . ? O4 Na3 O2C Na13 100(8) . . . . ? O5 Na3 O2C Na13 -51(8) . . . . ? O5 Na3 O2C Na13 -50(8) 2_556 . . . ? O1C Na3 O2C Na13 -157(8) . . . . ? O6C Na3 O2C Na13 -173(9) . . . . ? O5C Na3 O2C Na13 10(6) . . . . ? O4 Na3 O5C C8C -66(2) . . . . ? O5 Na3 O5C C8C 89.0(19) . . . . ? O5 Na3 O5C C8C 82.3(18) 2_556 . . . ? O1C Na3 O5C C8C -171.8(17) . . . . ? O2C Na3 O5C C8C 23(4) . . . . ? O6C Na3 O5C C8C -155(2) . . . . ? O4 Na3 O5C C9C 76.0(19) . . . . ? O5 Na3 O5C C9C -129.4(19) . . . . ? O5 Na3 O5C C9C -136.2(18) 2_556 . . . ? O1C Na3 O5C C9C -30(2) . . . . ? O2C Na3 O5C C9C 165(2) . . . . ? O6C Na3 O5C C9C -13.0(17) . . . . ? O4 Na3 O6C C10C -117.7(17) . . . . ? O5 Na3 O6C C10C 34.4(18) . . . . ? O5 Na3 O6C C10C 46.0(18) 2_556 . . . ? O1C Na3 O6C C10C 141(2) . . . . ? O2C Na3 O6C C10C 157.2(14) . . . . ? O5C Na3 O6C C10C -23.9(16) . . . . ? O4 Na3 O6C C11C 112.5(16) . . . . ? O5 Na3 O6C C11C -95.4(16) . . . . ? O5 Na3 O6C C11C -83.8(17) 2_556 . . . ? O1C Na3 O6C C11C 11.2(16) . . . . ? O2C Na3 O6C C11C 27(2) . . . . ? O5C Na3 O6C C11C -154(2) . . . . ? C12X O1X C1X C2X 171.6(19) . . . . ? Na13 O1X C1X C2X 48(3) . . . . ? C9C O5C C8C C7C 170.7(19) . . . . ? Na3 O5C C8C C7C -45(2) . . . . ? C8C O5C C9C C10C -170(2) . . . . ? Na3 O5C C9C C10C 43(2) . . . . ? C11C O6C C10C C9C -174.0(19) . . . . ? Na3 O6C C10C C9C 54(2) . . . . ? O5C C9C C10C O6C -59(3) . . . . ? C6X C5X O3X C4X -165.2(13) . . . . ? C6X C5X O3X Na13 69.9(13) . . . . ? C12X C11X O6X C10X -176.4(19) . . . . ? C12X C11X O6X Na13 -39(2) . . . . ? C11C C12C O1C C1C -174(2) . . . . ? C11C C12C O1C Na3 -55.7(19) . . . . ? O4 Na3 O1C C1C 55(2) . . . . ? O5 Na3 O1C C1C -124.9(18) . . . . ? O5 Na3 O1C C1C -104.4(18) 2_556 . . . ? O2C Na3 O1C C1C -27.4(17) . . . . ? O6C Na3 O1C C1C 142(2) . . . . ? O5C Na3 O1C C1C 157.4(17) . . . . ? O4 Na3 O1C C12C -64.4(15) . . . . ? O5 Na3 O1C C12C 116.0(14) . . . . ? O5 Na3 O1C C12C 136.5(14) 2_556 . . . ? O2C Na3 O1C C12C -146.5(15) . . . . ? O6C Na3 O1C C12C 22.5(14) . . . . ? O5C Na3 O1C C12C 38.4(19) . . . . ? C2X O2C C2C C1C -105(6) . . . . ? C3C O2C C2C C1C -173.3(17) . . . . ? C3X O2C C2C C1C -178.8(16) . . . . ? Na3 O2C C2C C1C 44.2(15) . . . . ? Na13 O2C C2C C1C 46.6(15) . . . . ? C5X O3X C4X C3X -173.6(12) . . . . ? Na13 O3X C4X C3X -49.1(14) . . . . ? O3X C5X C6X O4X -60.7(17) . . . . ? C11X O6X C10X C9X -162.8(17) . . . . ? Na13 O6X C10X C9X 53.3(19) . . . . ? C9X O5X C8X C7X -158.2(15) . . . . ? Na13 O5X C8X C7X -11(2) . . . . ? O4X C7X C8X O5X -55.0(16) . . . . ? C12C O1C C1C C2C -177.1(17) . . . . ? Na3 O1C C1C C2C 61(2) . . . . ? O2C C2C C1C O1C -73(2) . . . . ? C1X O1X C12X C11X -179.1(18) . . . . ? Na13 O1X C12X C11X -51.1(16) . . . . ? O6X C11X C12X O1X 62(2) . . . . ? O1C C12C C11C O6C 64(2) . . . . ? C10C O6C C11C C12C -179.2(18) . . . . ? Na3 O6C C11C C12C -42(2) . . . . ? C8X O5X C9X C10X -176.8(19) . . . . ? Na13 O5X C9X C10X 31(2) . . . . ? O6X C10X C9X O5X -58(3) . . . . ? C2X O2C C3X C4X 160.7(12) . . . . ? C3C O2C C3X C4X 162(7) . . . . ? C2C O2C C3X C4X 178.7(11) . . . . ? Na3 O2C C3X C4X -48.0(17) . . . . ? Na13 O2C C3X C4X -47.5(16) . . . . ? O3X C4X C3X O2C 68.0(17) . . . . ? C6C O4C C7C C8C 174.8(13) . . . . ? O5C C8C C7C O4C 62.1(18) . . . . ? C7C O4C C6C C5C 174.5(10) . . . . ? O3C C5C C6C O4C -68.5(14) . . . . ? C8X C7X O4X C6X -176.1(11) . . . . ? C5X C6X O4X C7X -77.2(16) . . . . ? C3C O2C C2X C1X 179.6(19) . . . . ? C3X O2C C2X C1X 180.0(18) . . . . ? C2C O2C C2X C1X 65(6) . . . . ? Na3 O2C C2X C1X 30.1(19) . . . . ? Na13 O2C C2X C1X 32.1(19) . . . . ? O1X C1X C2X O2C -52(2) . . . . ? C2X O2C C3C C4C 156.3(13) . . . . ? C3X O2C C3C C4C -23(5) . . . . ? C2C O2C C3C C4C 171.9(12) . . . . ? Na3 O2C C3C C4C -60(2) . . . . ? Na13 O2C C3C C4C -57.8(19) . . . . ? O3C C4C C3C O2C 67.3(17) . . . . ? C6C C5C O3C C4C 175.5(12) . . . . ? C3C C4C O3C C5C -173.3(14) . . . . ? C11X O6X Na13 O5 -72.1(19) . . . 2_556 ? C10X O6X Na13 O5 68.1(15) . . . 2_556 ? C11X O6X Na13 O14 93.8(18) . . . . ? C10X O6X Na13 O14 -126.1(14) . . . . ? C11X O6X Na13 O5X -166(2) . . . . ? C10X O6X Na13 O5X -25.6(14) . . . . ? C11X O6X Na13 O1X 9.4(16) . . . . ? C10X O6X Na13 O1X 149.5(17) . . . . ? C11X O6X Na13 O2C 17(2) . . . . ? C10X O6X Na13 O2C 156.8(13) . . . . ? C11X O6X Na13 O3X -16(18) . . . . ? C10X O6X Na13 O3X 124(16) . . . . ? C8X O5X Na13 O5 89.9(19) . . . 2_556 ? C9X O5X Na13 O5 -122.5(13) . . . 2_556 ? C8X O5X Na13 O14 -53(2) . . . . ? C9X O5X Na13 O14 94.8(14) . . . . ? C8X O5X Na13 O6X -151(2) . . . . ? C9X O5X Na13 O6X -3.3(14) . . . . ? C8X O5X Na13 O1X -156.8(18) . . . . ? C9X O5X Na13 O1X -9(2) . . . . ? C8X O5X Na13 O2C 15(6) . . . . ? C9X O5X Na13 O2C 163(5) . . . . ? C8X O5X Na13 O3X 31(2) . . . . ? C9X O5X Na13 O3X 178.2(12) . . . . ? C12X O1X Na13 O5 145.8(14) . . . 2_556 ? C1X O1X Na13 O5 -87(2) . . . 2_556 ? C12X O1X Na13 O14 -78.6(15) . . . . ? C1X O1X Na13 O14 49(2) . . . . ? C12X O1X Na13 O6X 24.3(14) . . . . ? C1X O1X Na13 O6X 151(2) . . . . ? C12X O1X Na13 O5X 31(2) . . . . ? C1X O1X Na13 O5X 158(2) . . . . ? C12X O1X Na13 O2C -147.8(17) . . . . ? C1X O1X Na13 O2C -20.7(19) . . . . ? C12X O1X Na13 O3X -157.0(13) . . . . ? C1X O1X Na13 O3X -30(2) . . . . ? C2X O2C Na13 O5 103.0(11) . . . 2_556 ? C3C O2C Na13 O5 -34.7(13) . . . 2_556 ? C3X O2C Na13 O5 -46.3(10) . . . 2_556 ? C2C O2C Na13 O5 93.5(9) . . . 2_556 ? Na3 O2C Na13 O5 127(8) . . . 2_556 ? C2X O2C Na13 O14 -109.9(11) . . . . ? C3C O2C Na13 O14 112.4(13) . . . . ? C3X O2C Na13 O14 100.8(10) . . . . ? C2C O2C Na13 O14 -119.3(10) . . . . ? Na3 O2C Na13 O14 -86(8) . . . . ? C2X O2C Na13 O6X -15.0(14) . . . . ? C3C O2C Na13 O6X -152.7(14) . . . . ? C3X O2C Na13 O6X -164.3(11) . . . . ? C2C O2C Na13 O6X -24.5(12) . . . . ? Na3 O2C Na13 O6X 9(7) . . . . ? C2X O2C Na13 O5X 180(100) . . . . ? C3C O2C Na13 O5X 42(5) . . . . ? C3X O2C Na13 O5X 30(5) . . . . ? C2C O2C Na13 O5X 170(5) . . . . ? Na3 O2C Na13 O5X -156(12) . . . . ? C2X O2C Na13 O1X -7.3(12) . . . . ? C3C O2C Na13 O1X -145.0(14) . . . . ? C3X O2C Na13 O1X -156.6(11) . . . . ? C2C O2C Na13 O1X -16.7(11) . . . . ? Na3 O2C Na13 O1X 17(8) . . . . ? C2X O2C Na13 O3X 163.3(11) . . . . ? C3C O2C Na13 O3X 25.6(13) . . . . ? C3X O2C Na13 O3X 14.0(9) . . . . ? C2C O2C Na13 O3X 153.8(9) . . . . ? Na3 O2C Na13 O3X -173(8) . . . . ? C4X O3X Na13 O5 109.1(8) . . . 2_556 ? C5X O3X Na13 O5 -125.5(7) . . . 2_556 ? C4X O3X Na13 O14 -58.7(9) . . . . ? C5X O3X Na13 O14 66.8(8) . . . . ? C4X O3X Na13 O6X 52(17) . . . . ? C5X O3X Na13 O6X 178(100) . . . . ? C4X O3X Na13 O5X -159.2(10) . . . . ? C5X O3X Na13 O5X -33.7(10) . . . . ? C4X O3X Na13 O1X 26.8(11) . . . . ? C5X O3X Na13 O1X 152.3(9) . . . . ? C4X O3X Na13 O2C 18.1(8) . . . . ? C5X O3X Na13 O2C 143.6(7) . . . . ? Na1 O1 C1S C2S -119(2) . . . . ? Na1 O1 C1S C3S 30.2(10) . . . . ? O11 Na11 O21 O21 17(26) . . . 2_565 ? O2A Na11 O21 O21 171(21) . . . 2_565 ? O1A Na11 O21 O21 -119(21) . . . 2_565 ? O3A Na11 O21 O21 106(22) . . . 2_565 ? O6A Na11 O21 O21 -58(22) . . . 2_565 ? O21 Na11 O21 Na11 0.00(7) 2_565 . . 2_565 ? O11 Na11 O21 Na11 17(26) . . . 2_565 ? O2A Na11 O21 Na11 171(22) . . . 2_565 ? O1A Na11 O21 Na11 -119(22) . . . 2_565 ? O3A Na11 O21 Na11 106(22) . . . 2_565 ? O6A Na11 O21 Na11 -58(22) . . . 2_565 ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.935 _refine_diff_density_max 0.832 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.045