# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address S.Bulut ; Albert-Ludwigs-Universit\"at Freiburg Institut f r Anorganische und Allgemeine Chemie and Freiburger Materialforschungszentrum (FMF) Albertstr. 21 D-79104 Freiburg GERMANY ; P.Klose ; Albert-Ludwigs-Universit\"at Freiburg Institut f r Anorganische und Allgemeine Chemie and Freiburger Materialforschungszentrum (FMF) Albertstr. 21 D-79104 Freiburg GERMANY ; I.Krossing ; Albert-Ludwigs-Universit\"at Freiburg Institut f r Anorganische und Allgemeine Chemie and Freiburger Materialforschungszentrum (FMF) Albertstr. 21 D-79104 Freiburg GERMANY ; _publ_contact_author_address ; Albert-Ludwigs-Universit\"at Freiburg Institut f r Anorganische und Allgemeine Chemie Albertstr. 21 D-79104 Freiburg GERMANY ; _publ_contact_author_email krossing@uni-freiburg.de _publ_contact_author_fax '+49 761 203-6001' _publ_contact_author_phone '+49 761 203-6122' _publ_contact_author_name 'Prof Ingo Krossing' #===END # Attachment '- Na[B(hfip)4]x(THF)2_REVISED.cif' data_p-1 _database_code_depnum_ccdc_archive 'CCDC 820689' #TrackingRef '- Na[B(hfip)4]x(THF)2_REVISED.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; sodium ditetrahydrofurane tetrakis(hexafluoroisoproxy)borate ; _chemical_name_common 'sodium ditetrahydrofurane tetrakis(hexafluoroisoproxy)borate' _chemical_formula_moiety 'Na C8 H16 O2, B O4 C12 H4 F24' _chemical_formula_sum 'C20 H20 B F24 Na O6' _chemical_properties_physical moisture-sensitive _exptl_crystal_recrystallization_method ; by sublimation during drying in vacuum (0.1 Pa) at r.t. ; _exptl_crystal_description isometric _exptl_crystal_colour colourless _diffrn_ambient_temperature 113(2) _chemical_formula_weight 846.16 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' B B 0.0013 0.0007 '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' 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' _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 9.2805(19) _cell_length_b 10.964(2) _cell_length_c 15.890(3) _cell_angle_alpha 87.32(3) _cell_angle_beta 85.69(3) _cell_angle_gamma 78.66(3) _cell_volume 1580.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.779 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 0.227 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.687 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ; Empirical Absorption Correction (T Higashi, March 2001) ; _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector' _diffrn_measurement_method '\w scans' _diffrn_reflns_number 28052 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7219 _reflns_number_gt 5263 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0418P)^2^+0.5437P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7219 _refine_ls_number_parameters 549 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0616 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1051 _refine_ls_wR_factor_gt 0.0952 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.003 _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 0.74156(8) 0.45877(6) 0.26236(4) 0.03053(17) Uani 1 1 d . . . B1 B 0.5680(2) 0.71932(18) 0.23728(12) 0.0244(4) Uani 1 1 d . . . O1 O 0.67429(13) 0.66688(11) 0.30127(7) 0.0259(3) Uani 1 1 d . . . O2 O 0.45253(13) 0.81342(11) 0.27527(7) 0.0270(3) Uani 1 1 d . . . O3 O 0.64330(13) 0.77270(11) 0.16423(7) 0.0252(3) Uani 1 1 d . . . O4 O 0.51775(13) 0.60760(11) 0.21274(7) 0.0252(3) Uani 1 1 d . . . O5 O 0.83574(16) 0.32832(13) 0.36746(8) 0.0405(3) Uani 1 1 d . . . O6 O 0.78001(17) 0.29573(12) 0.17358(9) 0.0404(3) Uani 1 1 d . . . F1 F 0.95136(15) 0.73552(15) 0.25218(8) 0.0603(4) Uani 1 1 d . . . F2 F 0.98084(17) 0.75772(17) 0.38285(9) 0.0703(5) Uani 1 1 d . . . F3 F 0.95059(15) 0.58149(15) 0.33869(11) 0.0704(5) Uani 1 1 d . . . F4 F 0.54532(16) 0.76120(16) 0.44979(8) 0.0659(4) Uani 1 1 d . . . F5 F 0.73951(19) 0.81869(19) 0.48312(10) 0.0855(6) Uani 1 1 d . . . F6 F 0.7408(2) 0.62540(17) 0.47392(9) 0.0807(5) Uani 1 1 d . . . F7 F 0.19631(15) 1.04780(12) 0.17237(9) 0.0553(4) Uani 1 1 d . . . F8 F 0.15225(13) 0.91632(12) 0.27097(8) 0.0497(3) Uani 1 1 d . . . F9 F 0.25171(14) 0.85165(12) 0.15149(8) 0.0501(3) Uani 1 1 d . . . F10 F 0.54262(14) 1.02264(11) 0.32522(8) 0.0468(3) Uani 1 1 d . . . F11 F 0.32222(16) 1.01357(13) 0.37333(9) 0.0586(4) Uani 1 1 d . . . F12 F 0.35870(16) 1.14360(11) 0.27224(10) 0.0598(4) Uani 1 1 d . . . F13 F 0.85583(12) 0.55993(10) 0.14055(7) 0.0375(3) Uani 1 1 d . . . F14 F 0.92888(12) 0.71672(11) 0.07681(8) 0.0422(3) Uani 1 1 d . . . F15 F 0.85448(14) 0.58224(11) 0.00503(7) 0.0469(3) Uani 1 1 d . . . F16 F 0.71168(14) 0.90759(10) 0.02185(7) 0.0409(3) Uani 1 1 d . . . F17 F 0.66494(17) 0.77215(11) -0.05946(7) 0.0512(3) Uani 1 1 d . . . F18 F 0.49356(15) 0.86850(12) 0.02540(9) 0.0540(3) Uani 1 1 d . . . F19 F 0.49490(13) 0.40274(11) 0.30945(8) 0.0445(3) Uani 1 1 d . . . F20 F 0.40216(15) 0.56359(12) 0.38086(7) 0.0485(3) Uani 1 1 d . . . F21 F 0.25999(13) 0.45571(12) 0.33161(8) 0.0511(3) Uani 1 1 d . . . F22 F 0.33406(16) 0.59911(14) 0.09097(8) 0.0566(4) Uani 1 1 d . . . F23 F 0.41628(16) 0.41703(12) 0.14187(9) 0.0584(4) Uani 1 1 d . . . F24 F 0.19175(15) 0.50609(15) 0.17199(9) 0.0613(4) Uani 1 1 d . . . C1 C 0.7404(2) 0.74411(19) 0.34605(12) 0.0340(4) Uani 1 1 d . . . C2 C 0.9077(3) 0.7042(2) 0.33038(14) 0.0463(5) Uani 1 1 d . . . C3 C 0.6915(3) 0.7359(3) 0.43921(14) 0.0512(6) Uani 1 1 d . . . C4 C 0.4031(2) 0.93026(17) 0.23853(12) 0.0311(4) Uani 1 1 d . . . C5 C 0.2496(2) 0.93724(18) 0.20868(13) 0.0375(5) Uani 1 1 d . . . C6 C 0.4049(2) 1.02799(18) 0.30288(14) 0.0403(5) Uani 1 1 d . . . C7 C 0.6710(2) 0.71598(16) 0.08686(11) 0.0262(4) Uani 1 1 d . . . C8 C 0.8289(2) 0.64527(18) 0.07632(11) 0.0324(4) Uani 1 1 d . . . C9 C 0.6368(2) 0.81664(18) 0.01787(12) 0.0335(4) Uani 1 1 d . . . C10 C 0.3777(2) 0.58424(17) 0.23485(11) 0.0285(4) Uani 1 1 d . . . C11 C 0.3814(2) 0.50062(18) 0.31464(13) 0.0345(4) Uani 1 1 d . . . C12 C 0.3286(2) 0.5252(2) 0.15989(14) 0.0399(5) Uani 1 1 d . . . C13 C 0.7761(3) 0.3146(2) 0.45266(14) 0.0465(5) Uani 1 1 d . . . C14 C 0.9717(3) 0.2387(2) 0.36199(16) 0.0468(6) Uani 1 1 d . . . C15 C 0.8037(3) 0.1756(2) 0.47030(16) 0.0467(5) Uani 1 1 d . . . C16 C 0.9449(3) 0.1279(2) 0.41695(17) 0.0494(6) Uani 1 1 d . . . C17 C 0.8747(3) 0.2665(2) 0.09854(15) 0.0487(6) Uani 1 1 d . . . C18 C 0.7137(3) 0.1901(2) 0.19858(17) 0.0496(6) Uani 1 1 d . . . C19 C 0.8143(3) 0.0807(2) 0.16155(15) 0.0494(6) Uani 1 1 d . . . C20 C 0.8684(3) 0.1350(2) 0.07793(15) 0.0470(6) Uani 1 1 d . . . H1A H 0.719(2) 0.831(2) 0.3263(14) 0.043(6) Uiso 1 1 d . . . H4A H 0.465(2) 0.9492(17) 0.1916(12) 0.025(5) Uiso 1 1 d . . . H7A H 0.608(2) 0.6568(18) 0.0780(11) 0.025(5) Uiso 1 1 d . . . H10A H 0.307(2) 0.6554(19) 0.2473(12) 0.027(5) Uiso 1 1 d . . . H13A H 0.831(3) 0.358(2) 0.4907(17) 0.062(8) Uiso 1 1 d . . . H13B H 0.671(3) 0.354(3) 0.4553(17) 0.065(8) Uiso 1 1 d . . . H14A H 0.999(3) 0.222(3) 0.3016(19) 0.070(8) Uiso 1 1 d . . . H14B H 1.044(3) 0.280(2) 0.3843(16) 0.057(8) Uiso 1 1 d . . . H15A H 0.722(3) 0.142(3) 0.4525(17) 0.067(8) Uiso 1 1 d . . . H15B H 0.808(3) 0.158(3) 0.5292(18) 0.066(8) Uiso 1 1 d . . . H16A H 0.929(3) 0.064(3) 0.3804(17) 0.064(8) Uiso 1 1 d . . . H16B H 1.025(3) 0.101(3) 0.4524(18) 0.067(8) Uiso 1 1 d . . . H17A H 0.843(3) 0.324(3) 0.0565(19) 0.073(9) Uiso 1 1 d . . . H17B H 0.985(4) 0.273(3) 0.116(2) 0.087(10) Uiso 1 1 d . . . H18A H 0.703(3) 0.187(2) 0.2595(16) 0.046(6) Uiso 1 1 d . . . H18B H 0.617(4) 0.186(3) 0.163(2) 0.110(12) Uiso 1 1 d . . . H19A H 0.761(3) 0.015(2) 0.1559(15) 0.052(7) Uiso 1 1 d . . . H19B H 0.902(3) 0.058(3) 0.208(2) 0.083(9) Uiso 1 1 d . . . H20A H 0.803(3) 0.138(2) 0.0384(17) 0.055(8) Uiso 1 1 d . . . H20B H 0.961(4) 0.093(3) 0.0595(19) 0.074(9) Uiso 1 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 0.0351(4) 0.0261(4) 0.0282(4) 0.0011(3) 0.0021(3) -0.0026(3) B1 0.0236(10) 0.0245(9) 0.0252(9) -0.0016(7) 0.0006(7) -0.0051(8) O1 0.0263(6) 0.0268(6) 0.0254(6) -0.0024(5) -0.0020(5) -0.0063(5) O2 0.0270(6) 0.0234(6) 0.0288(6) -0.0006(5) 0.0041(5) -0.0029(5) O3 0.0274(6) 0.0245(6) 0.0235(6) -0.0025(5) 0.0026(5) -0.0061(5) O4 0.0246(6) 0.0254(6) 0.0261(6) -0.0029(5) 0.0021(5) -0.0073(5) O5 0.0445(9) 0.0391(8) 0.0311(7) 0.0074(6) 0.0028(6) 0.0048(6) O6 0.0522(9) 0.0322(7) 0.0372(7) -0.0075(6) 0.0168(6) -0.0149(6) F1 0.0485(8) 0.0946(11) 0.0466(8) -0.0046(7) 0.0010(6) -0.0367(8) F2 0.0553(9) 0.1189(14) 0.0518(8) -0.0023(8) -0.0179(7) -0.0486(9) F3 0.0359(8) 0.0665(10) 0.1028(13) 0.0097(9) -0.0084(8) 0.0032(7) F4 0.0537(9) 0.1054(12) 0.0406(7) -0.0250(8) 0.0102(6) -0.0204(8) F5 0.0751(11) 0.1246(15) 0.0655(10) -0.0588(10) -0.0084(8) -0.0266(10) F6 0.1103(14) 0.0899(12) 0.0355(8) 0.0165(8) -0.0061(8) -0.0080(10) F7 0.0471(8) 0.0395(7) 0.0738(9) 0.0204(6) -0.0093(7) 0.0017(6) F8 0.0316(7) 0.0565(8) 0.0597(8) 0.0084(6) 0.0072(6) -0.0118(6) F9 0.0460(8) 0.0492(7) 0.0550(8) -0.0051(6) -0.0143(6) -0.0045(6) F10 0.0497(8) 0.0349(6) 0.0594(8) -0.0098(6) -0.0001(6) -0.0163(5) F11 0.0672(9) 0.0542(8) 0.0559(8) -0.0256(7) 0.0292(7) -0.0226(7) F12 0.0634(9) 0.0230(6) 0.0898(11) -0.0062(6) 0.0004(8) -0.0021(6) F13 0.0349(6) 0.0348(6) 0.0368(6) 0.0077(5) 0.0069(5) 0.0021(5) F14 0.0312(6) 0.0490(7) 0.0461(7) 0.0070(5) 0.0072(5) -0.0125(5) F15 0.0542(8) 0.0470(7) 0.0336(6) -0.0098(5) 0.0143(5) 0.0000(6) F16 0.0614(8) 0.0291(6) 0.0365(6) 0.0046(5) -0.0067(5) -0.0192(5) F17 0.0930(11) 0.0399(7) 0.0248(6) -0.0001(5) -0.0094(6) -0.0208(7) F18 0.0468(8) 0.0501(8) 0.0618(8) 0.0190(6) -0.0135(6) -0.0026(6) F19 0.0396(7) 0.0367(6) 0.0523(7) 0.0112(5) 0.0061(5) -0.0015(5) F20 0.0624(8) 0.0565(8) 0.0292(6) -0.0024(5) 0.0046(5) -0.0205(6) F21 0.0375(7) 0.0551(8) 0.0629(8) 0.0122(6) 0.0082(6) -0.0222(6) F22 0.0656(9) 0.0727(9) 0.0380(7) 0.0001(7) -0.0171(6) -0.0246(7) F23 0.0610(9) 0.0498(8) 0.0675(9) -0.0310(7) -0.0086(7) -0.0100(7) F24 0.0403(8) 0.0867(11) 0.0672(9) -0.0151(8) -0.0082(6) -0.0328(7) C1 0.0390(11) 0.0322(10) 0.0337(10) -0.0031(8) -0.0083(8) -0.0115(8) C2 0.0421(13) 0.0590(14) 0.0440(12) 0.0031(10) -0.0100(10) -0.0232(11) C3 0.0531(15) 0.0678(16) 0.0357(11) -0.0165(11) -0.0035(10) -0.0154(12) C4 0.0308(10) 0.0242(9) 0.0364(10) 0.0005(8) 0.0071(8) -0.0047(7) C5 0.0326(11) 0.0314(10) 0.0454(12) 0.0058(9) 0.0023(9) -0.0021(8) C6 0.0406(12) 0.0271(10) 0.0522(12) -0.0060(9) 0.0099(10) -0.0081(8) C7 0.0314(10) 0.0242(8) 0.0234(8) -0.0013(7) 0.0005(7) -0.0067(7) C8 0.0327(10) 0.0338(10) 0.0285(9) 0.0007(8) 0.0081(8) -0.0052(8) C9 0.0427(12) 0.0311(10) 0.0287(9) -0.0017(8) -0.0028(8) -0.0118(8) C10 0.0246(9) 0.0291(9) 0.0322(9) -0.0032(7) 0.0022(7) -0.0074(8) C11 0.0285(10) 0.0346(10) 0.0398(11) -0.0019(8) 0.0067(8) -0.0080(8) C12 0.0345(11) 0.0465(12) 0.0426(11) -0.0086(9) -0.0034(9) -0.0160(9) C13 0.0505(14) 0.0531(14) 0.0294(10) 0.0029(10) 0.0022(9) 0.0029(11) C14 0.0371(13) 0.0480(13) 0.0487(14) 0.0130(11) 0.0022(10) 0.0030(10) C15 0.0458(14) 0.0531(14) 0.0420(13) 0.0100(10) -0.0011(10) -0.0151(11) C16 0.0482(14) 0.0415(13) 0.0532(14) 0.0108(11) 0.0012(11) -0.0007(11) C17 0.0656(17) 0.0464(13) 0.0346(11) -0.0085(10) 0.0157(11) -0.0172(12) C18 0.0619(16) 0.0389(12) 0.0506(14) -0.0075(10) 0.0179(12) -0.0226(11) C19 0.0656(16) 0.0383(12) 0.0476(13) -0.0085(10) 0.0075(12) -0.0207(12) C20 0.0582(16) 0.0470(13) 0.0373(12) -0.0132(10) 0.0056(11) -0.0142(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 O5 2.2589(17) . ? Na1 O6 2.2852(16) . ? Na1 O1 2.3436(15) . ? Na1 F13 2.4607(15) . ? Na1 O4 2.5282(16) . ? Na1 F19 2.5357(16) . ? Na1 F3 2.929(2) . ? Na1 B1 3.016(2) . ? B1 O2 1.450(2) . ? B1 O3 1.467(2) . ? B1 O4 1.472(2) . ? B1 O1 1.487(2) . ? O1 C1 1.388(2) . ? O2 C4 1.390(2) . ? O3 C7 1.388(2) . ? O4 C10 1.390(2) . ? O5 C13 1.437(3) . ? O5 C14 1.438(3) . ? O6 C17 1.437(2) . ? O6 C18 1.441(3) . ? F1 C2 1.329(3) . ? F2 C2 1.337(3) . ? F3 C2 1.329(3) . ? F4 C3 1.329(3) . ? F5 C3 1.333(3) . ? F6 C3 1.318(3) . ? F7 C5 1.337(2) . ? F8 C5 1.332(2) . ? F9 C5 1.333(2) . ? F10 C6 1.342(3) . ? F11 C6 1.330(2) . ? F12 C6 1.337(2) . ? F13 C8 1.355(2) . ? F14 C8 1.327(2) . ? F15 C8 1.336(2) . ? F16 C9 1.329(2) . ? F17 C9 1.332(2) . ? F18 C9 1.338(2) . ? F19 C11 1.349(2) . ? F20 C11 1.331(2) . ? F21 C11 1.321(2) . ? F22 C12 1.335(3) . ? F23 C12 1.330(3) . ? F24 C12 1.326(2) . ? C1 C3 1.519(3) . ? C1 C2 1.533(3) . ? C4 C6 1.519(3) . ? C4 C5 1.521(3) . ? C7 C8 1.518(3) . ? C7 C9 1.524(3) . ? C10 C12 1.521(3) . ? C10 C11 1.528(3) . ? C13 C15 1.511(3) . ? C14 C16 1.512(3) . ? C15 C16 1.522(3) . ? C17 C20 1.507(3) . ? C18 C19 1.484(3) . ? C19 C20 1.522(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 O5 Na1 O6 89.87(6) . . ? O5 Na1 O1 113.49(6) . . ? O6 Na1 O1 156.56(6) . . ? O5 Na1 F13 132.81(6) . . ? O6 Na1 F13 82.27(5) . . ? O1 Na1 F13 80.25(5) . . ? O5 Na1 O4 145.98(6) . . ? O6 Na1 O4 105.50(6) . . ? O1 Na1 O4 56.10(5) . . ? F13 Na1 O4 80.09(5) . . ? O5 Na1 F19 86.70(6) . . ? O6 Na1 F19 87.75(6) . . ? O1 Na1 F19 95.22(5) . . ? F13 Na1 F19 138.84(5) . . ? O4 Na1 F19 64.33(5) . . ? O5 Na1 F3 73.95(6) . . ? O6 Na1 F3 130.82(6) . . ? O1 Na1 F3 59.19(5) . . ? F13 Na1 F3 76.67(5) . . ? O4 Na1 F3 113.72(5) . . ? F19 Na1 F3 135.39(5) . . ? O5 Na1 B1 139.67(6) . . ? O6 Na1 B1 129.12(6) . . ? O1 Na1 B1 28.88(5) . . ? F13 Na1 B1 71.13(5) . . ? O4 Na1 B1 29.13(5) . . ? F19 Na1 B1 85.26(6) . . ? F3 Na1 B1 84.59(6) . . ? O2 B1 O3 110.39(14) . . ? O2 B1 O4 114.30(15) . . ? O3 B1 O4 109.93(14) . . ? O2 B1 O1 109.50(14) . . ? O3 B1 O1 110.58(14) . . ? O4 B1 O1 101.85(14) . . ? O2 B1 Na1 143.69(12) . . ? O3 B1 Na1 105.33(11) . . ? O4 B1 Na1 56.74(8) . . ? O1 B1 Na1 49.59(8) . . ? C1 O1 B1 120.82(14) . . ? C1 O1 Na1 133.92(12) . . ? B1 O1 Na1 101.53(10) . . ? C4 O2 B1 124.18(14) . . ? C7 O3 B1 122.70(14) . . ? C10 O4 B1 123.52(13) . . ? C10 O4 Na1 119.88(11) . . ? B1 O4 Na1 94.13(10) . . ? C13 O5 C14 104.82(16) . . ? C13 O5 Na1 128.94(13) . . ? C14 O5 Na1 126.24(13) . . ? C17 O6 C18 108.75(16) . . ? C17 O6 Na1 132.83(13) . . ? C18 O6 Na1 117.95(12) . . ? C2 F3 Na1 109.48(13) . . ? C8 F13 Na1 144.24(11) . . ? C11 F19 Na1 114.53(11) . . ? O1 C1 C3 109.72(17) . . ? O1 C1 C2 107.99(16) . . ? C3 C1 C2 111.96(18) . . ? F3 C2 F1 106.4(2) . . ? F3 C2 F2 108.4(2) . . ? F1 C2 F2 107.20(18) . . ? F3 C2 C1 111.62(18) . . ? F1 C2 C1 110.91(18) . . ? F2 C2 C1 112.1(2) . . ? F6 C3 F4 109.0(2) . . ? F6 C3 F5 106.8(2) . . ? F4 C3 F5 106.48(19) . . ? F6 C3 C1 112.40(19) . . ? F4 C3 C1 110.31(19) . . ? F5 C3 C1 111.6(2) . . ? O2 C4 C6 108.56(16) . . ? O2 C4 C5 109.67(16) . . ? C6 C4 C5 111.77(16) . . ? F8 C5 F9 106.58(17) . . ? F8 C5 F7 107.33(16) . . ? F9 C5 F7 106.98(17) . . ? F8 C5 C4 112.79(17) . . ? F9 C5 C4 110.44(16) . . ? F7 C5 C4 112.37(17) . . ? F11 C6 F12 107.43(17) . . ? F11 C6 F10 107.06(19) . . ? F12 C6 F10 106.42(17) . . ? F11 C6 C4 113.07(17) . . ? F12 C6 C4 112.28(19) . . ? F10 C6 C4 110.22(16) . . ? O3 C7 C8 111.07(15) . . ? O3 C7 C9 107.93(14) . . ? C8 C7 C9 111.73(15) . . ? F14 C8 F15 107.72(15) . . ? F14 C8 F13 106.70(16) . . ? F15 C8 F13 106.50(15) . . ? F14 C8 C7 113.94(16) . . ? F15 C8 C7 111.91(16) . . ? F13 C8 C7 109.67(14) . . ? F16 C9 F17 107.07(16) . . ? F16 C9 F18 107.17(16) . . ? F17 C9 F18 107.15(16) . . ? F16 C9 C7 113.04(16) . . ? F17 C9 C7 112.67(15) . . ? F18 C9 C7 109.43(16) . . ? O4 C10 C12 107.49(15) . . ? O4 C10 C11 109.66(16) . . ? C12 C10 C11 112.48(16) . . ? F21 C11 F20 108.06(15) . . ? F21 C11 F19 107.25(16) . . ? F20 C11 F19 106.04(17) . . ? F21 C11 C10 113.56(17) . . ? F20 C11 C10 109.97(16) . . ? F19 C11 C10 111.60(15) . . ? F24 C12 F23 108.03(18) . . ? F24 C12 F22 107.30(18) . . ? F23 C12 F22 106.56(18) . . ? F24 C12 C10 112.71(17) . . ? F23 C12 C10 111.83(18) . . ? F22 C12 C10 110.13(17) . . ? O5 C13 C15 104.44(18) . . ? O5 C14 C16 106.03(19) . . ? C13 C15 C16 103.62(19) . . ? C14 C16 C15 104.83(19) . . ? O6 C17 C20 106.73(19) . . ? O6 C18 C19 105.71(19) . . ? C18 C19 C20 102.0(2) . . ? C17 C20 C19 103.32(18) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.577 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.049 #===END data_p-1a _database_code_depnum_ccdc_archive 'CCDC 820690' _audit_creation_method SHELXL-97 _chemical_name_systematic 'sodium monodimethoxyethane tetrakis(hexafluoroisoproxy)borate' _chemical_name_common 'sodium monodimethoxyethane tetrakis(hexafluoroisoproxy)borate' _chemical_formula_moiety 'Na C4 H10 O2, B O4 C12 H4 F24' _chemical_formula_sum 'C16 H14 B F24 Na O6' _chemical_properties_physical moisture-sensitive _exptl_crystal_recrystallization_method ; by sublimation during drying in vacuum (0.1 Pa) at 313-318 K ; _chemical_melting_point 329 _exptl_crystal_description isometric _exptl_crystal_colour colourless _diffrn_ambient_temperature 100(2) _chemical_formula_weight 792.07 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' B B 0.0013 0.0007 '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' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.491(2) _cell_length_b 10.546(2) _cell_length_c 13.212(3) _cell_angle_alpha 77.05(3) _cell_angle_beta 80.40(3) _cell_angle_gamma 81.33(3) _cell_volume 1394.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.886 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 0.250 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.851 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ; Empirical Absorption Correction (T Higashi, March 2001) ; _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector' _diffrn_measurement_method '\w scans' _diffrn_reflns_number 26660 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 27.46 _reflns_number_total 6359 _reflns_number_gt 5219 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0273P)^2^+0.6890P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6359 _refine_ls_number_parameters 489 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0420 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0792 _refine_ls_wR_factor_gt 0.0714 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na1 Na 0.15610(6) 0.41032(6) 0.26210(5) 0.02505(14) Uani 1 1 d . . . B1 B 0.35089(15) 0.17085(15) 0.26221(12) 0.0165(3) Uani 1 1 d . . . O1 O 0.36780(9) 0.31017(9) 0.25698(8) 0.0173(2) Uani 1 1 d . . . O2 O 0.22073(9) 0.18548(10) 0.22868(7) 0.0177(2) Uani 1 1 d . . . O3 O 0.35059(9) 0.09567(10) 0.36977(8) 0.0183(2) Uani 1 1 d . . . O4 O 0.45340(9) 0.11296(9) 0.19161(8) 0.0181(2) Uani 1 1 d . . . O5 O 0.10843(11) 0.61676(11) 0.16702(9) 0.0270(2) Uani 1 1 d . . . O6 O -0.03468(10) 0.50387(11) 0.35176(9) 0.0265(2) Uani 1 1 d . . . F1 F 0.56317(10) 0.36546(10) 0.09807(7) 0.0335(2) Uani 1 1 d . . . F2 F 0.48183(11) 0.54338(9) 0.14961(8) 0.0383(3) Uani 1 1 d . . . F3 F 0.66866(10) 0.44677(12) 0.18964(9) 0.0438(3) Uani 1 1 d . . . F4 F 0.41358(10) 0.34040(10) 0.45736(7) 0.0334(2) Uani 1 1 d . . . F5 F 0.34651(10) 0.51316(10) 0.34992(8) 0.0356(2) Uani 1 1 d . . . F6 F 0.54642(11) 0.47978(11) 0.37845(9) 0.0422(3) Uani 1 1 d . . . F7 F 0.05047(12) 0.05890(13) 0.07108(9) 0.0514(3) Uani 1 1 d . . . F8 F 0.08059(12) -0.00932(11) 0.23196(9) 0.0473(3) Uani 1 1 d . . . F9 F -0.02603(10) 0.17928(13) 0.18406(11) 0.0535(3) Uani 1 1 d . . . F10 F 0.11646(12) 0.37866(10) 0.07996(8) 0.0429(3) Uani 1 1 d . . . F11 F 0.16989(12) 0.26383(11) -0.03972(8) 0.0421(3) Uani 1 1 d . . . F12 F 0.31785(11) 0.32376(11) 0.02796(8) 0.0420(3) Uani 1 1 d . . . F13 F 0.15349(10) 0.26648(9) 0.44268(7) 0.0325(2) Uani 1 1 d . . . F14 F 0.24450(12) 0.15319(10) 0.57397(8) 0.0394(3) Uani 1 1 d . . . F15 F 0.05747(11) 0.11342(12) 0.55021(9) 0.0476(3) Uani 1 1 d . . . F16 F 0.38428(10) -0.08265(10) 0.54628(8) 0.0384(3) Uani 1 1 d . . . F17 F 0.18618(11) -0.12702(10) 0.57239(8) 0.0430(3) Uani 1 1 d . . . F18 F 0.31715(14) -0.17354(10) 0.43841(9) 0.0505(3) Uani 1 1 d . . . F19 F 0.68660(10) 0.06415(10) 0.07181(7) 0.0355(2) Uani 1 1 d . . . F20 F 0.75760(10) -0.08536(10) 0.19648(8) 0.0373(2) Uani 1 1 d . . . F21 F 0.71173(9) 0.11450(10) 0.21564(8) 0.0353(2) Uani 1 1 d . . . F22 F 0.55449(12) -0.23105(10) 0.23775(10) 0.0458(3) Uani 1 1 d . . . F23 F 0.51558(12) -0.11211(11) 0.08839(8) 0.0438(3) Uani 1 1 d . . . F24 F 0.36516(10) -0.12311(10) 0.22072(9) 0.0365(2) Uani 1 1 d . . . C1 C 0.48232(14) 0.34424(14) 0.27785(12) 0.0189(3) Uani 1 1 d . . . C2 C 0.54980(15) 0.42628(16) 0.17771(13) 0.0257(3) Uani 1 1 d . . . C3 C 0.44818(16) 0.42027(16) 0.36625(13) 0.0257(3) Uani 1 1 d . . . C4 C 0.20327(15) 0.15635(15) 0.13424(11) 0.0197(3) Uani 1 1 d . . . C5 C 0.07558(17) 0.09656(18) 0.15469(14) 0.0324(4) Uani 1 1 d . . . C6 C 0.20152(17) 0.28125(16) 0.04918(12) 0.0273(3) Uani 1 1 d . . . C7 C 0.24072(15) 0.04927(15) 0.43172(11) 0.0209(3) Uani 1 1 d . . . C8 C 0.17437(16) 0.14455(16) 0.50135(12) 0.0281(4) Uani 1 1 d . . . C9 C 0.28265(18) -0.08445(16) 0.49822(13) 0.0299(4) Uani 1 1 d . . . C10 C 0.53417(14) -0.00116(14) 0.22398(12) 0.0201(3) Uani 1 1 d . . . C11 C 0.67327(15) 0.02290(16) 0.17572(13) 0.0262(3) Uani 1 1 d . . . C12 C 0.49322(17) -0.11781(16) 0.19163(13) 0.0283(3) Uani 1 1 d . . . C13 C 0.1935(2) 0.6930(2) 0.08943(17) 0.0390(4) Uani 1 1 d . . . C14 C 0.01443(17) 0.69522(16) 0.22454(14) 0.0279(3) Uani 1 1 d . . . C15 C -0.09090(16) 0.61389(16) 0.28178(14) 0.0287(4) Uani 1 1 d . . . C16 C -0.13252(19) 0.4352(2) 0.42101(18) 0.0427(5) Uani 1 1 d . . . H1A H 0.5445(15) 0.2718(16) 0.2998(12) 0.014(4) Uiso 1 1 d . . . H4A H 0.2736(16) 0.0929(16) 0.1093(12) 0.016(4) Uiso 1 1 d . . . H7A H 0.1758(17) 0.0371(17) 0.3947(13) 0.022(4) Uiso 1 1 d . . . H10A H 0.5374(15) -0.0255(15) 0.2953(13) 0.013(4) Uiso 1 1 d . . . H13A H 0.143(2) 0.753(2) 0.0370(18) 0.050(6) Uiso 1 1 d . . . H13B H 0.255(2) 0.632(2) 0.0538(18) 0.049(6) Uiso 1 1 d . . . H13C H 0.245(2) 0.735(2) 0.1202(19) 0.059(7) Uiso 1 1 d . . . H14A H -0.0229(19) 0.772(2) 0.1775(15) 0.035(5) Uiso 1 1 d . . . H14B H 0.0549(19) 0.7260(19) 0.2746(16) 0.035(5) Uiso 1 1 d . . . H15A H -0.1341(19) 0.580(2) 0.2318(16) 0.038(5) Uiso 1 1 d . . . H15B H -0.159(2) 0.669(2) 0.3249(16) 0.039(5) Uiso 1 1 d . . . H16A H -0.091(2) 0.370(2) 0.4699(17) 0.044(6) Uiso 1 1 d . . . H16B H -0.197(2) 0.494(2) 0.4591(19) 0.060(7) Uiso 1 1 d . . . H16C H -0.184(3) 0.399(3) 0.380(2) 0.066(8) Uiso 1 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 0.0227(3) 0.0209(3) 0.0272(3) -0.0023(2) -0.0013(2) 0.0049(2) B1 0.0159(7) 0.0156(7) 0.0181(8) -0.0026(6) -0.0038(6) -0.0016(6) O1 0.0158(5) 0.0146(5) 0.0219(5) -0.0036(4) -0.0035(4) -0.0018(4) O2 0.0168(5) 0.0199(5) 0.0170(5) -0.0035(4) -0.0045(4) -0.0023(4) O3 0.0177(5) 0.0181(5) 0.0181(5) -0.0007(4) -0.0040(4) -0.0019(4) O4 0.0175(5) 0.0155(5) 0.0201(5) -0.0032(4) -0.0030(4) 0.0018(4) O5 0.0260(6) 0.0205(5) 0.0288(6) -0.0009(4) 0.0035(5) 0.0005(4) O6 0.0210(6) 0.0270(6) 0.0261(6) 0.0002(5) 0.0006(4) 0.0013(4) F1 0.0363(6) 0.0387(6) 0.0255(5) -0.0088(4) 0.0062(4) -0.0124(4) F2 0.0488(6) 0.0227(5) 0.0379(6) 0.0034(4) -0.0010(5) -0.0067(4) F3 0.0283(5) 0.0620(8) 0.0446(6) -0.0086(5) 0.0006(5) -0.0258(5) F4 0.0425(6) 0.0374(6) 0.0223(5) -0.0088(4) -0.0031(4) -0.0080(5) F5 0.0381(6) 0.0260(5) 0.0420(6) -0.0153(4) -0.0001(4) 0.0046(4) F6 0.0392(6) 0.0503(7) 0.0493(7) -0.0281(5) -0.0028(5) -0.0205(5) F7 0.0595(8) 0.0607(8) 0.0482(7) -0.0139(6) -0.0257(6) -0.0278(6) F8 0.0604(8) 0.0424(6) 0.0445(6) 0.0045(5) -0.0154(5) -0.0336(6) F9 0.0198(5) 0.0683(8) 0.0754(9) -0.0201(7) -0.0055(5) -0.0079(5) F10 0.0608(7) 0.0258(5) 0.0370(6) -0.0027(4) -0.0135(5) 0.0131(5) F11 0.0639(7) 0.0435(6) 0.0223(5) -0.0041(4) -0.0196(5) -0.0057(5) F12 0.0490(7) 0.0463(6) 0.0295(5) 0.0065(5) -0.0052(5) -0.0235(5) F13 0.0354(5) 0.0262(5) 0.0268(5) 0.0007(4) 0.0033(4) 0.0069(4) F14 0.0613(7) 0.0341(6) 0.0232(5) -0.0078(4) -0.0107(5) 0.0010(5) F15 0.0360(6) 0.0497(7) 0.0420(6) 0.0040(5) 0.0177(5) -0.0037(5) F16 0.0404(6) 0.0347(6) 0.0351(6) 0.0082(4) -0.0164(5) 0.0010(5) F17 0.0534(7) 0.0346(6) 0.0352(6) 0.0120(5) -0.0026(5) -0.0201(5) F18 0.0879(9) 0.0200(5) 0.0414(6) -0.0048(5) -0.0077(6) -0.0029(5) F19 0.0302(5) 0.0437(6) 0.0267(5) -0.0030(4) 0.0025(4) 0.0008(4) F20 0.0274(5) 0.0387(6) 0.0402(6) -0.0097(5) -0.0053(4) 0.0162(4) F21 0.0195(5) 0.0423(6) 0.0486(6) -0.0188(5) -0.0020(4) -0.0059(4) F22 0.0577(7) 0.0169(5) 0.0642(8) -0.0072(5) -0.0247(6) 0.0074(5) F23 0.0625(7) 0.0408(6) 0.0348(6) -0.0199(5) -0.0092(5) -0.0063(5) F24 0.0375(6) 0.0272(5) 0.0492(6) -0.0093(5) -0.0110(5) -0.0098(4) C1 0.0171(7) 0.0165(7) 0.0240(7) -0.0049(6) -0.0042(6) -0.0021(5) C2 0.0231(8) 0.0269(8) 0.0281(8) -0.0055(6) -0.0012(6) -0.0093(6) C3 0.0265(8) 0.0241(8) 0.0296(8) -0.0093(6) -0.0043(6) -0.0063(6) C4 0.0205(7) 0.0204(7) 0.0201(7) -0.0055(6) -0.0070(6) -0.0013(6) C5 0.0323(9) 0.0354(9) 0.0347(9) -0.0061(7) -0.0134(7) -0.0118(7) C6 0.0354(9) 0.0265(8) 0.0211(8) -0.0037(6) -0.0093(7) -0.0024(7) C7 0.0211(7) 0.0223(7) 0.0185(7) 0.0008(6) -0.0038(6) -0.0066(6) C8 0.0286(8) 0.0293(9) 0.0199(8) 0.0031(6) 0.0024(6) -0.0016(7) C9 0.0398(10) 0.0230(8) 0.0252(8) 0.0014(6) -0.0046(7) -0.0080(7) C10 0.0218(7) 0.0178(7) 0.0204(7) -0.0051(6) -0.0053(6) 0.0031(6) C11 0.0224(8) 0.0283(8) 0.0269(8) -0.0086(7) -0.0037(6) 0.0048(6) C12 0.0335(9) 0.0204(8) 0.0313(9) -0.0070(6) -0.0083(7) 0.0026(6) C13 0.0312(10) 0.0385(11) 0.0380(10) 0.0070(9) 0.0036(8) -0.0064(8) C14 0.0300(9) 0.0180(8) 0.0344(9) -0.0056(7) -0.0041(7) 0.0014(6) C15 0.0234(8) 0.0248(8) 0.0337(9) -0.0038(7) -0.0022(7) 0.0057(6) C16 0.0252(9) 0.0430(11) 0.0448(11) 0.0102(9) 0.0085(8) -0.0005(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Na1 O5 2.2854(14) . ? Na1 O1 2.3083(13) . ? Na1 O6 2.3496(14) . ? Na1 O2 2.4824(13) . ? Na1 F13 2.5224(14) . ? Na1 F10 2.6098(14) . ? Na1 F5 2.9160(14) . ? Na1 B1 3.000(2) . ? Na1 C14 3.1168(19) . ? Na1 C15 3.121(2) . ? B1 O4 1.4567(19) . ? B1 O3 1.4636(19) . ? B1 O2 1.4807(18) . ? B1 O1 1.4913(18) . ? O1 C1 1.3905(17) . ? O2 C4 1.3963(17) . ? O3 C7 1.3834(18) . ? O4 C10 1.3900(17) . ? O5 C14 1.422(2) . ? O5 C13 1.426(2) . ? O6 C16 1.424(2) . ? O6 C15 1.430(2) . ? F1 C2 1.3283(19) . ? F2 C2 1.337(2) . ? F3 C2 1.3374(18) . ? F4 C3 1.3350(19) . ? F5 C3 1.346(2) . ? F6 C3 1.3334(18) . ? F7 C5 1.331(2) . ? F8 C5 1.335(2) . ? F9 C5 1.335(2) . ? F10 C6 1.344(2) . ? F11 C6 1.3299(19) . ? F12 C6 1.328(2) . ? F13 C8 1.3518(19) . ? F14 C8 1.329(2) . ? F15 C8 1.338(2) . ? F16 C9 1.333(2) . ? F17 C9 1.340(2) . ? F18 C9 1.332(2) . ? F19 C11 1.3342(19) . ? F20 C11 1.3408(19) . ? F21 C11 1.338(2) . ? F22 C12 1.3355(19) . ? F23 C12 1.334(2) . ? F24 C12 1.340(2) . ? C1 C3 1.526(2) . ? C1 C2 1.536(2) . ? C4 C5 1.524(2) . ? C4 C6 1.528(2) . ? C7 C8 1.527(2) . ? C7 C9 1.530(2) . ? C10 C11 1.526(2) . ? C10 C12 1.529(2) . ? C14 C15 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 O5 Na1 O1 120.94(5) . . ? O5 Na1 O6 73.22(5) . . ? O1 Na1 O6 151.21(5) . . ? O5 Na1 O2 137.74(5) . . ? O1 Na1 O2 57.15(4) . . ? O6 Na1 O2 131.30(5) . . ? O5 Na1 F13 146.06(5) . . ? O1 Na1 F13 77.92(5) . . ? O6 Na1 F13 78.70(5) . . ? O2 Na1 F13 75.82(4) . . ? O5 Na1 F10 74.44(5) . . ? O1 Na1 F10 97.30(5) . . ? O6 Na1 F10 111.11(5) . . ? O2 Na1 F10 64.81(4) . . ? F13 Na1 F10 134.84(4) . . ? O5 Na1 F5 88.08(5) . . ? O1 Na1 F5 59.92(4) . . ? O6 Na1 F5 98.67(4) . . ? O2 Na1 F5 115.12(4) . . ? F13 Na1 F5 77.58(4) . . ? F10 Na1 F5 138.59(5) . . ? O5 Na1 B1 141.67(5) . . ? O1 Na1 B1 29.08(4) . . ? O6 Na1 B1 145.12(5) . . ? O2 Na1 B1 29.45(4) . . ? F13 Na1 B1 68.41(5) . . ? F10 Na1 B1 85.70(5) . . ? F5 Na1 B1 85.68(4) . . ? O5 Na1 C14 24.95(4) . . ? O1 Na1 C14 137.38(5) . . ? O6 Na1 C14 49.21(5) . . ? O2 Na1 C14 155.77(5) . . ? F13 Na1 C14 122.18(5) . . ? F10 Na1 C14 91.81(5) . . ? F5 Na1 C14 86.32(5) . . ? B1 Na1 C14 164.81(5) . . ? O5 Na1 C15 49.05(5) . . ? O1 Na1 C15 162.70(5) . . ? O6 Na1 C15 25.68(4) . . ? O2 Na1 C15 140.15(5) . . ? F13 Na1 C15 104.37(5) . . ? F10 Na1 C15 92.99(5) . . ? F5 Na1 C15 103.45(5) . . ? B1 Na1 C15 167.17(5) . . ? C14 Na1 C15 27.80(5) . . ? O4 B1 O3 110.49(12) . . ? O4 B1 O2 112.85(12) . . ? O3 B1 O2 111.09(12) . . ? O4 B1 O1 110.41(12) . . ? O3 B1 O1 110.46(12) . . ? O2 B1 O1 101.20(11) . . ? O4 B1 Na1 140.07(10) . . ? O3 B1 Na1 109.07(9) . . ? O2 B1 Na1 55.53(7) . . ? O1 B1 Na1 48.79(6) . . ? C1 O1 B1 121.30(11) . . ? C1 O1 Na1 133.69(9) . . ? B1 O1 Na1 102.13(8) . . ? C4 O2 B1 122.12(11) . . ? C4 O2 Na1 120.42(9) . . ? B1 O2 Na1 95.02(8) . . ? C7 O3 B1 123.51(11) . . ? C10 O4 B1 123.32(11) . . ? C14 O5 C13 112.42(14) . . ? C14 O5 Na1 112.35(9) . . ? C13 O5 Na1 127.75(11) . . ? C16 O6 C15 111.30(13) . . ? C16 O6 Na1 126.52(12) . . ? C15 O6 Na1 108.90(9) . . ? C3 F5 Na1 108.94(9) . . ? C6 F10 Na1 110.43(9) . . ? C8 F13 Na1 147.69(10) . . ? O1 C1 C3 108.31(12) . . ? O1 C1 C2 109.31(12) . . ? C3 C1 C2 111.54(12) . . ? F1 C2 F3 107.50(13) . . ? F1 C2 F2 107.29(13) . . ? F3 C2 F2 107.65(13) . . ? F1 C2 C1 110.58(13) . . ? F3 C2 C1 111.62(13) . . ? F2 C2 C1 111.98(13) . . ? F6 C3 F4 107.59(13) . . ? F6 C3 F5 107.14(13) . . ? F4 C3 F5 106.55(13) . . ? F6 C3 C1 113.07(13) . . ? F4 C3 C1 110.56(13) . . ? F5 C3 C1 111.62(13) . . ? O2 C4 C5 106.64(13) . . ? O2 C4 C6 109.51(12) . . ? C5 C4 C6 112.34(13) . . ? F7 C5 F8 107.21(14) . . ? F7 C5 F9 107.57(14) . . ? F8 C5 F9 107.08(16) . . ? F7 C5 C4 112.52(15) . . ? F8 C5 C4 109.90(14) . . ? F9 C5 C4 112.28(14) . . ? F12 C6 F11 107.95(14) . . ? F12 C6 F10 106.71(14) . . ? F11 C6 F10 107.31(13) . . ? F12 C6 C4 110.20(13) . . ? F11 C6 C4 112.70(14) . . ? F10 C6 C4 111.72(13) . . ? O3 C7 C8 110.86(13) . . ? O3 C7 C9 107.91(13) . . ? C8 C7 C9 110.76(13) . . ? F14 C8 F15 107.70(13) . . ? F14 C8 F13 106.75(14) . . ? F15 C8 F13 106.13(13) . . ? F14 C8 C7 113.24(14) . . ? F15 C8 C7 112.48(15) . . ? F13 C8 C7 110.14(12) . . ? F18 C9 F16 107.12(15) . . ? F18 C9 F17 107.43(14) . . ? F16 C9 F17 107.37(13) . . ? F18 C9 C7 110.41(13) . . ? F16 C9 C7 112.50(14) . . ? F17 C9 C7 111.75(15) . . ? O4 C10 C11 107.46(12) . . ? O4 C10 C12 110.98(12) . . ? C11 C10 C12 111.64(13) . . ? F19 C11 F21 107.14(14) . . ? F19 C11 F20 107.35(13) . . ? F21 C11 F20 106.89(13) . . ? F19 C11 C10 113.18(13) . . ? F21 C11 C10 110.13(13) . . ? F20 C11 C10 111.83(14) . . ? F23 C12 F22 107.56(14) . . ? F23 C12 F24 106.71(14) . . ? F22 C12 F24 107.29(14) . . ? F23 C12 C10 113.47(14) . . ? F22 C12 C10 111.48(13) . . ? F24 C12 C10 110.04(13) . . ? O5 C14 C15 108.45(13) . . ? O5 C14 Na1 42.70(7) . . ? C15 C14 Na1 76.26(9) . . ? O6 C15 C14 108.77(13) . . ? O6 C15 Na1 45.42(7) . . ? C14 C15 Na1 75.95(9) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.367 _refine_diff_density_min -0.321 _refine_diff_density_rms 0.054