# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_publication_text _publ_requested_journal Chem.Commun. _publ_contact_author_name 'Guo-Yu Yang' _publ_contact_author_address ;State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China. ; _publ_contact_author_email ygy@fjirsm.ac.cn _publ_contact_author_phone ' (+86) 591-83710051' _publ_contact_author_fax ' (+86) 591-83710051' loop_ _publ_author_name _publ_author_address 'Guang-Zhen, Liu' ;State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China. ; 'Shou-Tian, Zheng' ;State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China. ; 'Guo-Yu, Yang' ;State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China. ; data_s _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'F2 Na13 Nb3 O28 P6' _chemical_formula_weight 1249.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nb' 'Nb' -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 10.6887(9) _cell_length_b 10.6887(9) _cell_length_c 6.6917(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 662.09(13) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1610 _cell_measurement_theta_min 3.0448 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.1000 _exptl_crystal_size_mid 0.0700 _exptl_crystal_size_min 0.0500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.134 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 598 _exptl_absorpt_coefficient_mu 1.989 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.7684 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Mercury70 _diffrn_measurement_method 'CCD_Profile_fitting' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5097 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.45 _reflns_number_total 1011 _reflns_number_gt 994 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0109P)^2^+15.7657P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0124(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1011 _refine_ls_number_parameters 88 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0683 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.1311 _refine_ls_wR_factor_gt 0.1308 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.000 _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 F F 0.5012(8) 0.8762(7) 0.2907(10) 0.0235(15) Uani 0.33 1 d P A 1 O O 0.5012(8) 0.8762(7) 0.2907(10) 0.0235(15) Uani 0.67 1 d P A 2 Nb Nb 0.5000 1.0000 0.5000 0.0280(4) Uani 1 2 d S . . P P 0.6283(3) 0.8107(3) 0.7431(5) 0.0176(6) Uani 1 1 d . . . O1 O 0.5746(12) 0.7397(9) 0.9399(12) 0.039(2) Uani 1 1 d . . . O2 O 0.7866(9) 0.8818(9) 0.727(2) 0.053(3) Uani 1 1 d . . . O3 O 0.5799(8) 0.9240(8) 0.7116(12) 0.0251(17) Uani 1 1 d . . . O4 O 0.5534(11) 0.6989(9) 0.5695(12) 0.033(2) Uani 1 1 d . . . Na1 Na 0.8619(5) 0.7039(5) 0.7573(11) 0.0351(12) Uani 1 1 d . . . Na2 Na 0.5000 0.5000 1.0000 0.0317(12) Uani 1 2 d S . . Na3 Na 1.0000 1.0000 0.5000 0.049(4) Uani 1 6 d S . . Na4 Na 1.0000 1.0000 1.0000 0.076(5) Uani 1 6 d S . . Na5 Na 0.3333 0.6667 0.1042(19) 0.022(2) Uani 0.67 3 d SP . . Na5' Na 0.3333 0.6667 0.392(6) 0.052(10) Uani 0.33 3 d SP . . 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 F 0.034(4) 0.025(3) 0.017(4) 0.000(3) 0.004(3) 0.019(3) O 0.034(4) 0.025(3) 0.017(4) 0.000(3) 0.004(3) 0.019(3) Nb 0.0133(6) 0.0409(9) 0.0300(8) 0.0214(8) 0.0067(7) 0.0137(6) P 0.0189(12) 0.0133(11) 0.0217(12) 0.0038(11) 0.0038(12) 0.0087(10) O1 0.068(7) 0.028(4) 0.021(4) -0.003(3) -0.004(4) 0.023(4) O2 0.021(4) 0.025(4) 0.114(10) -0.003(6) -0.003(6) 0.013(4) O3 0.031(4) 0.026(4) 0.026(5) -0.007(3) -0.006(3) 0.020(3) O4 0.062(6) 0.026(4) 0.019(4) -0.004(3) -0.002(4) 0.028(4) Na1 0.025(2) 0.031(2) 0.051(3) 0.016(3) 0.010(3) 0.016(2) Na2 0.048(4) 0.037(3) 0.012(2) -0.001(3) 0.003(3) 0.023(3) Na3 0.065(6) 0.065(6) 0.017(6) 0.000 0.000 0.032(3) Na4 0.064(7) 0.064(7) 0.098(14) 0.000 0.000 0.032(3) Na5 0.016(3) 0.016(3) 0.033(7) 0.000 0.000 0.0081(16) Na5' 0.012(7) 0.012(7) 0.13(3) 0.000 0.000 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 F Nb 1.932(7) . ? F Na5' 2.162(15) . ? F Na2 2.356(7) 2_664 ? F Na1 2.392(8) 5_566 ? F Na5 2.403(10) . ? Nb O 1.932(7) 4_676 ? Nb F 1.932(7) 4_676 ? Nb O4 1.962(8) 2_665 ? Nb O4 1.962(8) 5_566 ? Nb O3 2.022(8) . ? Nb O3 2.022(8) 4_676 ? Nb Na5' 3.169(10) 4_676 ? Nb Na5' 3.169(10) . ? Nb Na2 3.3458(5) 2_665 ? Nb Na2 3.3458(5) 2_664 ? P O2 1.472(8) . ? P O1 1.485(9) . ? P O3 1.551(7) . ? P O4 1.569(8) . ? P Na1 3.078(6) 3_675 ? P Na1 3.224(5) . ? P Na2 3.364(3) . ? P Na1 3.416(7) 5_567 ? P Na2 3.421(3) 2_665 ? P Na1 3.422(7) 5_566 ? O1 Na2 2.306(8) . ? O1 Na1 2.387(10) 5_567 ? O1 Na5 2.541(12) 1_556 ? O2 Na1 2.416(9) . ? O2 Na3 2.494(11) . ? O2 Na1 2.505(9) 3_675 ? O2 Na4 2.695(11) . ? O3 Na2 2.410(8) 2_665 ? O3 Na1 2.602(9) 3_675 ? O4 Nb 1.962(8) 3_565 ? O4 Na5' 2.50(2) . ? O4 Na1 2.693(11) 5_566 ? Na1 O1 2.387(10) 6_657 ? Na1 O 2.392(8) 6_656 ? Na1 F 2.392(8) 6_656 ? Na1 O2 2.505(10) 2_765 ? Na1 O3 2.602(9) 2_765 ? Na1 O4 2.693(11) 6_656 ? Na1 P 3.078(6) 2_765 ? Na1 Na4 3.188(6) . ? Na1 Na3 3.239(5) . ? Na1 P 3.416(7) 6_657 ? Na2 O1 2.306(8) 4_667 ? Na2 O 2.356(7) 3_566 ? Na2 F 2.356(7) 3_566 ? Na2 O 2.356(7) 6_656 ? Na2 F 2.356(7) 6_656 ? Na2 O3 2.410(8) 6_657 ? Na2 O3 2.410(8) 3_565 ? Na2 Na5 3.163(3) 1_556 ? Na2 Na5 3.163(3) 4_666 ? Na2 Nb 3.3458(5) 3_566 ? Na2 Nb 3.3459(5) 3_565 ? Na3 O2 2.494(11) 3_675 ? Na3 O2 2.494(11) 6_656 ? Na3 O2 2.494(11) 2_765 ? Na3 O2 2.494(11) 5_566 ? Na3 O2 2.494(11) 4_776 ? Na3 Na1 3.239(5) 2_765 ? Na3 Na1 3.239(5) 5_566 ? Na3 Na1 3.239(5) 3_675 ? Na3 Na1 3.239(5) 4_776 ? Na3 Na1 3.239(5) 6_656 ? Na4 O2 2.695(11) 4_777 ? Na4 O2 2.695(11) 5_567 ? Na4 O2 2.695(11) 6_657 ? Na4 O2 2.695(11) 2_765 ? Na4 O2 2.695(11) 3_675 ? Na4 Na1 3.188(6) 4_777 ? Na4 Na1 3.188(6) 5_567 ? Na4 Na1 3.188(6) 6_657 ? Na4 Na1 3.188(6) 2_765 ? Na4 Na1 3.188(6) 3_675 ? Na5 Na5' 1.93(4) . ? Na5 O 2.403(10) 2_665 ? Na5 F 2.403(10) 2_665 ? Na5 O 2.403(10) 3_565 ? Na5 F 2.403(10) 3_565 ? Na5 O1 2.541(12) 2_664 ? Na5 O1 2.541(12) 3_564 ? Na5 O1 2.541(12) 1_554 ? Na5 Na2 3.163(3) 3_564 ? Na5 Na2 3.163(3) 2_664 ? Na5' O 2.162(15) 2_665 ? Na5' F 2.162(15) 2_665 ? Na5' O 2.162(15) 3_565 ? Na5' F 2.162(15) 3_565 ? Na5' O4 2.50(2) 2_665 ? Na5' O4 2.50(2) 3_565 ? Na5' Nb 3.169(9) 2_665 ? 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 Nb F Na5' 101.3(9) . . ? Nb F Na2 102.1(3) . 2_664 ? Na5' F Na2 127.3(9) . 2_664 ? Nb F Na1 121.3(4) . 5_566 ? Na5' F Na1 103.3(3) . 5_566 ? Na2 F Na1 103.6(3) 2_664 5_566 ? Nb F Na5 139.2(4) . . ? Na5' F Na5 49.5(10) . . ? Na2 F Na5 83.3(3) 2_664 . ? Na1 F Na5 95.7(3) 5_566 . ? O Nb F 0.0(5) 4_676 4_676 ? O Nb F 180.000(1) 4_676 . ? F Nb F 180.000(1) 4_676 . ? O Nb O4 89.7(3) 4_676 2_665 ? F Nb O4 89.7(3) 4_676 2_665 ? F Nb O4 90.3(3) . 2_665 ? O Nb O4 90.3(3) 4_676 5_566 ? F Nb O4 90.3(3) 4_676 5_566 ? F Nb O4 89.7(3) . 5_566 ? O4 Nb O4 180.0(5) 2_665 5_566 ? O Nb O3 85.2(3) 4_676 . ? F Nb O3 85.2(3) 4_676 . ? F Nb O3 94.8(3) . . ? O4 Nb O3 91.3(4) 2_665 . ? O4 Nb O3 88.7(4) 5_566 . ? O Nb O3 94.8(3) 4_676 4_676 ? F Nb O3 94.8(3) 4_676 4_676 ? F Nb O3 85.2(3) . 4_676 ? O4 Nb O3 88.7(4) 2_665 4_676 ? O4 Nb O3 91.3(4) 5_566 4_676 ? O3 Nb O3 180.000(2) . 4_676 ? O Nb Na5' 42.0(7) 4_676 4_676 ? F Nb Na5' 42.0(7) 4_676 4_676 ? F Nb Na5' 138.0(7) . 4_676 ? O4 Nb Na5' 127.9(4) 2_665 4_676 ? O4 Nb Na5' 52.1(4) 5_566 4_676 ? O3 Nb Na5' 100.3(6) . 4_676 ? O3 Nb Na5' 79.7(6) 4_676 4_676 ? O Nb Na5' 138.0(7) 4_676 . ? F Nb Na5' 138.0(7) 4_676 . ? F Nb Na5' 42.0(7) . . ? O4 Nb Na5' 52.1(4) 2_665 . ? O4 Nb Na5' 127.9(4) 5_566 . ? O3 Nb Na5' 79.7(6) . . ? O3 Nb Na5' 100.3(6) 4_676 . ? Na5' Nb Na5' 180.000(1) 4_676 . ? O Nb Na2 43.5(2) 4_676 2_665 ? F Nb Na2 43.5(2) 4_676 2_665 ? F Nb Na2 136.5(2) . 2_665 ? O4 Nb Na2 76.3(2) 2_665 2_665 ? O4 Nb Na2 103.7(2) 5_566 2_665 ? O3 Nb Na2 45.5(2) . 2_665 ? O3 Nb Na2 134.5(2) 4_676 2_665 ? Na5' Nb Na2 76.8(7) 4_676 2_665 ? Na5' Nb Na2 103.2(7) . 2_665 ? O Nb Na2 136.5(2) 4_676 2_664 ? F Nb Na2 136.5(2) 4_676 2_664 ? F Nb Na2 43.5(2) . 2_664 ? O4 Nb Na2 103.7(2) 2_665 2_664 ? O4 Nb Na2 76.3(2) 5_566 2_664 ? O3 Nb Na2 134.5(2) . 2_664 ? O3 Nb Na2 45.5(2) 4_676 2_664 ? Na5' Nb Na2 103.2(7) 4_676 2_664 ? Na5' Nb Na2 76.8(7) . 2_664 ? Na2 Nb Na2 180.0 2_665 2_664 ? O2 P O1 112.4(7) . . ? O2 P O3 109.5(5) . . ? O1 P O3 109.0(5) . . ? O2 P O4 110.8(6) . . ? O1 P O4 110.3(5) . . ? O3 P O4 104.6(5) . . ? O2 P Na1 53.7(3) . 3_675 ? O1 P Na1 115.5(4) . 3_675 ? O3 P Na1 57.6(3) . 3_675 ? O4 P Na1 134.0(4) . 3_675 ? O2 P Na1 44.9(3) . . ? O1 P Na1 87.9(4) . . ? O3 P Na1 154.2(3) . . ? O4 P Na1 86.7(4) . . ? Na1 P Na1 97.82(17) 3_675 . ? O2 P Na2 110.1(4) . . ? O1 P Na2 34.8(3) . . ? O3 P Na2 135.2(3) . . ? O4 P Na2 79.9(3) . . ? Na1 P Na2 144.20(19) 3_675 . ? Na1 P Na2 68.95(11) . . ? O2 P Na1 82.4(6) . 5_567 ? O1 P Na1 36.3(4) . 5_567 ? O3 P Na1 102.2(3) . 5_567 ? O4 P Na1 143.6(3) . 5_567 ? Na1 P Na1 81.6(2) 3_675 5_567 ? Na1 P Na1 79.6(2) . 5_567 ? Na2 P Na1 63.65(9) . 5_567 ? O2 P Na2 115.4(4) . 2_665 ? O1 P Na2 71.9(4) . 2_665 ? O3 P Na2 38.5(3) . 2_665 ? O4 P Na2 128.3(4) . 2_665 ? Na1 P Na2 66.50(11) 3_675 2_665 ? Na1 P Na2 143.60(18) . 2_665 ? Na2 P Na2 103.94(8) . 2_665 ? Na1 P Na2 66.14(10) 5_567 2_665 ? O2 P Na1 73.9(6) . 5_566 ? O1 P Na1 158.4(4) . 5_566 ? O3 P Na1 86.9(3) . 5_566 ? O4 P Na1 49.9(4) . 5_566 ? Na1 P Na1 85.10(19) 3_675 5_566 ? Na1 P Na1 82.92(18) . 5_566 ? Na2 P Na1 123.81(11) . 5_566 ? Na1 P Na1 156.28(16) 5_567 5_566 ? Na2 P Na1 125.37(11) 2_665 5_566 ? P O1 Na2 123.6(5) . . ? P O1 Na1 122.1(6) . 5_567 ? Na2 O1 Na1 99.2(3) . 5_567 ? P O1 Na5 127.9(6) . 1_556 ? Na2 O1 Na5 81.3(3) . 1_556 ? Na1 O1 Na5 92.3(4) 5_567 1_556 ? P O2 Na1 109.7(4) . . ? P O2 Na3 146.2(8) . . ? Na1 O2 Na3 82.5(3) . . ? P O2 Na1 98.1(4) . 3_675 ? Na1 O2 Na1 149.8(4) . 3_675 ? Na3 O2 Na1 80.8(3) . 3_675 ? P O2 Na4 132.6(8) . . ? Na1 O2 Na4 77.0(3) . . ? Na3 O2 Na4 80.2(2) . . ? Na1 O2 Na4 75.5(3) 3_675 . ? P O3 Nb 141.4(5) . . ? P O3 Na2 117.9(4) . 2_665 ? Nb O3 Na2 97.7(3) . 2_665 ? P O3 Na1 92.1(4) . 3_675 ? Nb O3 Na1 102.4(4) . 3_675 ? Na2 O3 Na1 90.9(3) 2_665 3_675 ? P O4 Nb 139.7(5) . 3_565 ? P O4 Na5' 122.9(7) . . ? Nb O4 Na5' 89.7(4) 3_565 . ? P O4 Na1 103.7(5) . 5_566 ? Nb O4 Na1 101.0(3) 3_565 5_566 ? Na5' O4 Na1 86.9(8) . 5_566 ? O1 Na1 O 79.8(3) 6_657 6_656 ? O1 Na1 F 79.8(3) 6_657 6_656 ? O Na1 F 0.0(6) 6_656 6_656 ? O1 Na1 O2 122.4(5) 6_657 . ? O Na1 O2 94.8(3) 6_656 . ? F Na1 O2 94.8(3) 6_656 . ? O1 Na1 O2 109.2(5) 6_657 2_765 ? O Na1 O2 166.9(5) 6_656 2_765 ? F Na1 O2 166.9(5) 6_656 2_765 ? O2 Na1 O2 88.3(4) . 2_765 ? O1 Na1 O3 81.3(3) 6_657 2_765 ? O Na1 O3 116.3(3) 6_656 2_765 ? F Na1 O3 116.3(3) 6_656 2_765 ? O2 Na1 O3 144.8(3) . 2_765 ? O2 Na1 O3 57.8(3) 2_765 2_765 ? O1 Na1 O4 112.6(3) 6_657 6_656 ? O Na1 O4 69.4(3) 6_656 6_656 ? F Na1 O4 69.4(3) 6_656 6_656 ? O2 Na1 O4 118.6(5) . 6_656 ? O2 Na1 O4 98.0(4) 2_765 6_656 ? O3 Na1 O4 63.4(3) 2_765 6_656 ? O1 Na1 P 92.3(3) 6_657 2_765 ? O Na1 P 146.4(3) 6_656 2_765 ? F Na1 P 146.4(3) 6_656 2_765 ? O2 Na1 P 116.5(2) . 2_765 ? O2 Na1 P 28.2(2) 2_765 2_765 ? O3 Na1 P 30.22(17) 2_765 2_765 ? O4 Na1 P 84.2(2) 6_656 2_765 ? O1 Na1 Na4 90.2(3) 6_657 . ? O Na1 Na4 136.3(3) 6_656 . ? F Na1 Na4 136.3(3) 6_656 . ? O2 Na1 Na4 55.4(3) . . ? O2 Na1 Na4 54.9(3) 2_765 . ? O3 Na1 Na4 103.8(2) 2_765 . ? O4 Na1 Na4 150.2(3) 6_656 . ? P Na1 Na4 75.71(13) 2_765 . ? O1 Na1 P 109.8(3) 6_657 . ? O Na1 P 70.2(2) 6_656 . ? F Na1 P 70.2(2) 6_656 . ? O2 Na1 P 25.5(2) . . ? O2 Na1 P 113.7(2) 2_765 . ? O3 Na1 P 168.4(3) 2_765 . ? O4 Na1 P 113.0(3) 6_656 . ? P Na1 P 141.97(16) 2_765 . ? Na4 Na1 P 73.71(12) . . ? O1 Na1 Na3 151.8(4) 6_657 . ? O Na1 Na3 124.9(3) 6_656 . ? F Na1 Na3 124.9(3) 6_656 . ? O2 Na1 Na3 49.8(3) . . ? O2 Na1 Na3 49.5(3) 2_765 . ? O3 Na1 Na3 96.6(2) 2_765 . ? O4 Na1 Na3 90.8(3) 6_656 . ? P Na1 Na3 74.04(12) 2_765 . ? Na4 Na1 Na3 62.74(9) . . ? P Na1 Na3 72.15(11) . . ? O1 Na1 P 21.6(2) 6_657 6_657 ? O Na1 P 87.6(2) 6_656 6_657 ? F Na1 P 87.6(2) 6_656 6_657 ? O2 Na1 P 102.0(4) . 6_657 ? O2 Na1 P 104.2(4) 2_765 6_657 ? O3 Na1 P 95.7(3) 2_765 6_657 ? O4 Na1 P 134.0(3) 6_656 6_657 ? P Na1 P 96.86(19) 2_765 6_657 ? Na4 Na1 P 71.14(15) . 6_657 ? P Na1 P 94.15(18) . 6_657 ? Na3 Na1 P 133.86(19) . 6_657 ? O1 Na2 O1 180.000(2) 4_667 . ? O1 Na2 O 88.3(3) 4_667 3_566 ? O1 Na2 O 91.7(3) . 3_566 ? O1 Na2 F 88.3(3) 4_667 3_566 ? O1 Na2 F 91.7(3) . 3_566 ? O Na2 F 0.0(3) 3_566 3_566 ? O1 Na2 O 91.7(3) 4_667 6_656 ? O1 Na2 O 88.3(3) . 6_656 ? O Na2 O 180.000(1) 3_566 6_656 ? F Na2 O 180.000(1) 3_566 6_656 ? O1 Na2 F 91.7(3) 4_667 6_656 ? O1 Na2 F 88.3(3) . 6_656 ? O Na2 F 180.000(1) 3_566 6_656 ? F Na2 F 180.000(1) 3_566 6_656 ? O Na2 F 0.0(4) 6_656 6_656 ? O1 Na2 O3 92.7(3) 4_667 6_657 ? O1 Na2 O3 87.3(3) . 6_657 ? O Na2 O3 68.3(2) 3_566 6_657 ? F Na2 O3 68.3(2) 3_566 6_657 ? O Na2 O3 111.7(2) 6_656 6_657 ? F Na2 O3 111.7(2) 6_656 6_657 ? O1 Na2 O3 87.3(3) 4_667 3_565 ? O1 Na2 O3 92.7(3) . 3_565 ? O Na2 O3 111.7(2) 3_566 3_565 ? F Na2 O3 111.7(2) 3_566 3_565 ? O Na2 O3 68.3(2) 6_656 3_565 ? F Na2 O3 68.3(2) 6_656 3_565 ? O3 Na2 O3 180.000(1) 6_657 3_565 ? O1 Na2 Na5 127.4(3) 4_667 1_556 ? O1 Na2 Na5 52.6(3) . 1_556 ? O Na2 Na5 49.0(3) 3_566 1_556 ? F Na2 Na5 49.0(3) 3_566 1_556 ? O Na2 Na5 131.0(3) 6_656 1_556 ? F Na2 Na5 131.0(3) 6_656 1_556 ? O3 Na2 Na5 96.2(3) 6_657 1_556 ? O3 Na2 Na5 83.8(3) 3_565 1_556 ? O1 Na2 Na5 52.6(3) 4_667 4_666 ? O1 Na2 Na5 127.4(3) . 4_666 ? O Na2 Na5 131.0(3) 3_566 4_666 ? F Na2 Na5 131.0(3) 3_566 4_666 ? O Na2 Na5 49.0(3) 6_656 4_666 ? F Na2 Na5 49.0(3) 6_656 4_666 ? O3 Na2 Na5 83.8(3) 6_657 4_666 ? O3 Na2 Na5 96.2(3) 3_565 4_666 ? Na5 Na2 Na5 180.0 1_556 4_666 ? O1 Na2 Nb 79.95(19) 4_667 3_566 ? O1 Na2 Nb 100.05(19) . 3_566 ? O Na2 Nb 34.37(16) 3_566 3_566 ? F Na2 Nb 34.37(16) 3_566 3_566 ? O Na2 Nb 145.63(16) 6_656 3_566 ? F Na2 Nb 145.63(16) 6_656 3_566 ? O3 Na2 Nb 36.79(18) 6_657 3_566 ? O3 Na2 Nb 143.21(18) 3_565 3_566 ? Na5 Na2 Nb 77.3(2) 1_556 3_566 ? Na5 Na2 Nb 102.7(2) 4_666 3_566 ? O1 Na2 Nb 100.05(19) 4_667 3_565 ? O1 Na2 Nb 79.95(19) . 3_565 ? O Na2 Nb 145.63(16) 3_566 3_565 ? F Na2 Nb 145.63(16) 3_566 3_565 ? O Na2 Nb 34.37(16) 6_656 3_565 ? F Na2 Nb 34.37(16) 6_656 3_565 ? O3 Na2 Nb 143.21(18) 6_657 3_565 ? O3 Na2 Nb 36.79(18) 3_565 3_565 ? Na5 Na2 Nb 102.7(2) 1_556 3_565 ? Na5 Na2 Nb 77.3(2) 4_666 3_565 ? Nb Na2 Nb 180.0 3_566 3_565 ? O2 Na3 O2 180.000(1) 3_675 6_656 ? O2 Na3 O2 86.8(4) 3_675 2_765 ? O2 Na3 O2 93.2(4) 6_656 2_765 ? O2 Na3 O2 86.8(4) 3_675 . ? O2 Na3 O2 93.2(4) 6_656 . ? O2 Na3 O2 86.8(4) 2_765 . ? O2 Na3 O2 93.2(4) 3_675 5_566 ? O2 Na3 O2 86.8(4) 6_656 5_566 ? O2 Na3 O2 180.000(2) 2_765 5_566 ? O2 Na3 O2 93.2(4) . 5_566 ? O2 Na3 O2 93.2(4) 3_675 4_776 ? O2 Na3 O2 86.8(4) 6_656 4_776 ? O2 Na3 O2 93.2(4) 2_765 4_776 ? O2 Na3 O2 180.000(2) . 4_776 ? O2 Na3 O2 86.8(4) 5_566 4_776 ? O2 Na3 Na1 49.8(2) 3_675 2_765 ? O2 Na3 Na1 130.2(2) 6_656 2_765 ? O2 Na3 Na1 47.7(2) 2_765 2_765 ? O2 Na3 Na1 110.4(3) . 2_765 ? O2 Na3 Na1 132.3(2) 5_566 2_765 ? O2 Na3 Na1 69.6(3) 4_776 2_765 ? O2 Na3 Na1 130.2(2) 3_675 5_566 ? O2 Na3 Na1 49.8(2) 6_656 5_566 ? O2 Na3 Na1 132.3(2) 2_765 5_566 ? O2 Na3 Na1 69.6(3) . 5_566 ? O2 Na3 Na1 47.7(2) 5_566 5_566 ? O2 Na3 Na1 110.4(3) 4_776 5_566 ? Na1 Na3 Na1 180.000(1) 2_765 5_566 ? O2 Na3 Na1 47.7(2) 3_675 3_675 ? O2 Na3 Na1 132.3(2) 6_656 3_675 ? O2 Na3 Na1 110.4(3) 2_765 3_675 ? O2 Na3 Na1 49.8(2) . 3_675 ? O2 Na3 Na1 69.6(3) 5_566 3_675 ? O2 Na3 Na1 130.2(2) 4_776 3_675 ? Na1 Na3 Na1 94.36(17) 2_765 3_675 ? Na1 Na3 Na1 85.64(17) 5_566 3_675 ? O2 Na3 Na1 110.4(3) 3_675 . ? O2 Na3 Na1 69.6(3) 6_656 . ? O2 Na3 Na1 49.8(2) 2_765 . ? O2 Na3 Na1 47.7(2) . . ? O2 Na3 Na1 130.2(2) 5_566 . ? O2 Na3 Na1 132.3(2) 4_776 . ? Na1 Na3 Na1 94.36(17) 2_765 . ? Na1 Na3 Na1 85.64(17) 5_566 . ? Na1 Na3 Na1 94.36(17) 3_675 . ? O2 Na3 Na1 69.6(3) 3_675 4_776 ? O2 Na3 Na1 110.4(3) 6_656 4_776 ? O2 Na3 Na1 130.2(2) 2_765 4_776 ? O2 Na3 Na1 132.3(2) . 4_776 ? O2 Na3 Na1 49.8(2) 5_566 4_776 ? O2 Na3 Na1 47.7(2) 4_776 4_776 ? Na1 Na3 Na1 85.64(17) 2_765 4_776 ? Na1 Na3 Na1 94.36(17) 5_566 4_776 ? Na1 Na3 Na1 85.64(17) 3_675 4_776 ? Na1 Na3 Na1 180.000(1) . 4_776 ? O2 Na3 Na1 132.3(2) 3_675 6_656 ? O2 Na3 Na1 47.7(2) 6_656 6_656 ? O2 Na3 Na1 69.6(3) 2_765 6_656 ? O2 Na3 Na1 130.2(2) . 6_656 ? O2 Na3 Na1 110.4(3) 5_566 6_656 ? O2 Na3 Na1 49.8(2) 4_776 6_656 ? Na1 Na3 Na1 85.64(17) 2_765 6_656 ? Na1 Na3 Na1 94.36(17) 5_566 6_656 ? Na1 Na3 Na1 180.000(1) 3_675 6_656 ? Na1 Na3 Na1 85.64(17) . 6_656 ? Na1 Na3 Na1 94.36(17) 4_776 6_656 ? O2 Na4 O2 180.000(2) 4_777 . ? O2 Na4 O2 79.0(4) 4_777 5_567 ? O2 Na4 O2 101.0(4) . 5_567 ? O2 Na4 O2 79.0(4) 4_777 6_657 ? O2 Na4 O2 101.0(4) . 6_657 ? O2 Na4 O2 79.0(4) 5_567 6_657 ? O2 Na4 O2 101.0(4) 4_777 2_765 ? O2 Na4 O2 79.0(4) . 2_765 ? O2 Na4 O2 180.000(2) 5_567 2_765 ? O2 Na4 O2 101.0(4) 6_657 2_765 ? O2 Na4 O2 101.0(4) 4_777 3_675 ? O2 Na4 O2 79.0(4) . 3_675 ? O2 Na4 O2 101.0(4) 5_567 3_675 ? O2 Na4 O2 180.0(3) 6_657 3_675 ? O2 Na4 O2 79.0(4) 2_765 3_675 ? O2 Na4 Na1 47.59(19) 4_777 4_777 ? O2 Na4 Na1 132.41(19) . 4_777 ? O2 Na4 Na1 49.5(2) 5_567 4_777 ? O2 Na4 Na1 106.6(3) 6_657 4_777 ? O2 Na4 Na1 130.5(2) 2_765 4_777 ? O2 Na4 Na1 73.4(3) 3_675 4_777 ? O2 Na4 Na1 132.41(19) 4_777 . ? O2 Na4 Na1 47.59(19) . . ? O2 Na4 Na1 130.5(2) 5_567 . ? O2 Na4 Na1 73.4(3) 6_657 . ? O2 Na4 Na1 49.5(2) 2_765 . ? O2 Na4 Na1 106.6(3) 3_675 . ? Na1 Na4 Na1 180.000(1) 4_777 . ? O2 Na4 Na1 106.6(3) 4_777 5_567 ? O2 Na4 Na1 73.4(3) . 5_567 ? O2 Na4 Na1 47.59(19) 5_567 5_567 ? O2 Na4 Na1 49.5(2) 6_657 5_567 ? O2 Na4 Na1 132.41(19) 2_765 5_567 ? O2 Na4 Na1 130.5(2) 3_675 5_567 ? Na1 Na4 Na1 96.36(15) 4_777 5_567 ? Na1 Na4 Na1 83.64(15) . 5_567 ? O2 Na4 Na1 49.5(2) 4_777 6_657 ? O2 Na4 Na1 130.5(2) . 6_657 ? O2 Na4 Na1 106.6(3) 5_567 6_657 ? O2 Na4 Na1 47.59(19) 6_657 6_657 ? O2 Na4 Na1 73.4(3) 2_765 6_657 ? O2 Na4 Na1 132.41(19) 3_675 6_657 ? Na1 Na4 Na1 96.36(15) 4_777 6_657 ? Na1 Na4 Na1 83.64(15) . 6_657 ? Na1 Na4 Na1 96.36(15) 5_567 6_657 ? O2 Na4 Na1 73.4(3) 4_777 2_765 ? O2 Na4 Na1 106.6(3) . 2_765 ? O2 Na4 Na1 132.41(19) 5_567 2_765 ? O2 Na4 Na1 130.5(2) 6_657 2_765 ? O2 Na4 Na1 47.59(19) 2_765 2_765 ? O2 Na4 Na1 49.5(2) 3_675 2_765 ? Na1 Na4 Na1 83.64(15) 4_777 2_765 ? Na1 Na4 Na1 96.36(15) . 2_765 ? Na1 Na4 Na1 180.000(1) 5_567 2_765 ? Na1 Na4 Na1 83.64(15) 6_657 2_765 ? O2 Na4 Na1 130.5(2) 4_777 3_675 ? O2 Na4 Na1 49.55(19) . 3_675 ? O2 Na4 Na1 73.4(3) 5_567 3_675 ? O2 Na4 Na1 132.41(19) 6_657 3_675 ? O2 Na4 Na1 106.6(3) 2_765 3_675 ? O2 Na4 Na1 47.59(19) 3_675 3_675 ? Na1 Na4 Na1 83.64(15) 4_777 3_675 ? Na1 Na4 Na1 96.36(15) . 3_675 ? Na1 Na4 Na1 83.64(15) 5_567 3_675 ? Na1 Na4 Na1 180.000(1) 6_657 3_675 ? Na1 Na4 Na1 96.36(15) 2_765 3_675 ? Na5' Na5 O 58.7(3) . 2_665 ? Na5' Na5 F 58.7(3) . 2_665 ? O Na5 F 0.0(2) 2_665 2_665 ? Na5' Na5 F 58.7(3) . . ? O Na5 F 95.5(4) 2_665 . ? F Na5 F 95.5(4) 2_665 . ? Na5' Na5 O 58.7(3) . 3_565 ? O Na5 O 95.5(4) 2_665 3_565 ? F Na5 O 95.5(4) 2_665 3_565 ? F Na5 O 95.5(4) . 3_565 ? Na5' Na5 F 58.7(3) . 3_565 ? O Na5 F 95.5(4) 2_665 3_565 ? F Na5 F 95.5(4) 2_665 3_565 ? F Na5 F 95.5(4) . 3_565 ? O Na5 F 0.0(4) 3_565 3_565 ? Na5' Na5 O1 115.6(3) . 2_664 ? O Na5 O1 76.6(2) 2_665 2_664 ? F Na5 O1 76.6(2) 2_665 2_664 ? F Na5 O1 85.2(2) . 2_664 ? O Na5 O1 172.1(4) 3_565 2_664 ? F Na5 O1 172.1(4) 3_565 2_664 ? Na5' Na5 O1 115.6(3) . 3_564 ? O Na5 O1 85.2(2) 2_665 3_564 ? F Na5 O1 85.2(2) 2_665 3_564 ? F Na5 O1 172.1(4) . 3_564 ? O Na5 O1 76.6(2) 3_565 3_564 ? F Na5 O1 76.6(2) 3_565 3_564 ? O1 Na5 O1 102.7(4) 2_664 3_564 ? Na5' Na5 O1 115.6(3) . 1_554 ? O Na5 O1 172.1(4) 2_665 1_554 ? F Na5 O1 172.1(4) 2_665 1_554 ? F Na5 O1 76.6(2) . 1_554 ? O Na5 O1 85.2(2) 3_565 1_554 ? F Na5 O1 85.2(2) 3_565 1_554 ? O1 Na5 O1 102.7(4) 2_664 1_554 ? O1 Na5 O1 102.7(4) 3_564 1_554 ? Na5' Na5 Na2 102.7(2) . 3_564 ? O Na5 Na2 47.72(16) 2_665 3_564 ? F Na5 Na2 47.72(16) 2_665 3_564 ? F Na5 Na2 138.2(3) . 3_564 ? O Na5 Na2 105.72(18) 3_565 3_564 ? F Na5 Na2 105.72(18) 3_565 3_564 ? O1 Na5 Na2 69.2(2) 2_664 3_564 ? O1 Na5 Na2 46.1(2) 3_564 3_564 ? O1 Na5 Na2 139.6(5) 1_554 3_564 ? Na5' Na5 Na2 102.7(2) . 2_664 ? O Na5 Na2 105.72(18) 2_665 2_664 ? F Na5 Na2 105.72(18) 2_665 2_664 ? F Na5 Na2 47.72(16) . 2_664 ? O Na5 Na2 138.2(3) 3_565 2_664 ? F Na5 Na2 138.2(3) 3_565 2_664 ? O1 Na5 Na2 46.1(2) 2_664 2_664 ? O1 Na5 Na2 139.6(5) 3_564 2_664 ? O1 Na5 Na2 69.2(2) 1_554 2_664 ? Na2 Na5 Na2 115.28(16) 3_564 2_664 ? Na5 Na5' O 71.7(10) . 2_665 ? Na5 Na5' F 71.7(10) . 2_665 ? O Na5' F 0.00(15) 2_665 2_665 ? Na5 Na5' F 71.7(10) . . ? O Na5' F 110.7(10) 2_665 . ? F Na5' F 110.7(10) 2_665 . ? Na5 Na5' O 71.7(10) . 3_565 ? O Na5' O 110.7(10) 2_665 3_565 ? F Na5' O 110.7(10) 2_665 3_565 ? F Na5' O 110.7(10) . 3_565 ? Na5 Na5' F 71.7(10) . 3_565 ? O Na5' F 110.7(10) 2_665 3_565 ? F Na5' F 110.7(10) 2_665 3_565 ? F Na5' F 110.7(10) . 3_565 ? O Na5' F 0.0(4) 3_565 3_565 ? Na5 Na5' O4 118.4(8) . 2_665 ? O Na5' O4 76.7(3) 2_665 2_665 ? F Na5' O4 76.7(3) 2_665 2_665 ? F Na5' O4 72.2(3) . 2_665 ? O Na5' O4 169.5(18) 3_565 2_665 ? F Na5' O4 169.5(18) 3_565 2_665 ? Na5 Na5' O4 118.4(8) . 3_565 ? O Na5' O4 72.2(3) 2_665 3_565 ? F Na5' O4 72.2(3) 2_665 3_565 ? F Na5' O4 169.5(18) . 3_565 ? O Na5' O4 76.7(3) 3_565 3_565 ? F Na5' O4 76.7(3) 3_565 3_565 ? O4 Na5' O4 99.3(11) 2_665 3_565 ? Na5 Na5' O4 118.4(8) . . ? O Na5' O4 169.5(18) 2_665 . ? F Na5' O4 169.5(18) 2_665 . ? F Na5' O4 76.7(3) . . ? O Na5' O4 72.2(3) 3_565 . ? F Na5' O4 72.2(3) 3_565 . ? O4 Na5' O4 99.3(11) 2_665 . ? O4 Na5' O4 99.3(11) 3_565 . ? Na5 Na5' Nb 103.2(7) . . ? O Na5' Nb 104.18(18) 2_665 . ? F Na5' Nb 104.18(18) 2_665 . ? F Na5' Nb 36.7(3) . . ? O Na5' Nb 140.5(3) 3_565 . ? F Na5' Nb 140.5(3) 3_565 . ? O4 Na5' Nb 38.2(2) 2_665 . ? O4 Na5' Nb 133.2(14) 3_565 . ? O4 Na5' Nb 77.0(5) . . ? Na5 Na5' Nb 103.2(7) . 2_665 ? O Na5' Nb 36.7(3) 2_665 2_665 ? F Na5' Nb 36.7(3) 2_665 2_665 ? F Na5' Nb 140.5(3) . 2_665 ? O Na5' Nb 104.18(18) 3_565 2_665 ? F Na5' Nb 104.18(18) 3_565 2_665 ? O4 Na5' Nb 77.0(5) 2_665 2_665 ? O4 Na5' Nb 38.2(2) 3_565 2_665 ? O4 Na5' Nb 133.2(14) . 2_665 ? Nb Na5' Nb 115.0(5) . 2_665 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.069 _refine_diff_density_min -1.635 _refine_diff_density_rms 0.197