# Copyright The Royal Society of Chemistry, 1998 # CCDC ELECTRONIC DATA DEPOSITION FORM (CIF, VERSION DEC95) # for the structures of compunds I, IV, VII in the # paper by V.G.Kessler, A.N.Panov, N.Ya.Turova et al. # "Anodic oxidation of molybdenum and tungsten in alcohols..." # submitted to J.Chem.Soc. Dalton, ms. No. 7/04198E. #---------------------------------------------------------------- #1 Data block identification for start of deposition data_str_I #---------------------------------------------------------------- #2 Person making the deposition _publ_contact_author ? _publ_contact_author_email yan@xrpent.ineos.ac.ru #---------------------------------------------------------------- #3 Publication details loop_ _publ_author_name 'V.G.Kessler' 'A.N.Panov' 'N.Ya.Turova' 'Z.A.Starikova' 'A.I.Yanovsky' 'F.M.Dolgushin' 'A.P.Pisarevsky' 'Yu.T.Struchkov' _journal_name_full 'J.Chem.Soc.,Dalton Trans.' _journal_volume '?' _journal_page_first '?' _journal_page_last '?' _journal_year '1998' _ccdc_journal_depnumber '?' #---------------------------------------------------------------- #4 Chemical and physical data _ccdc_compound_id 'I' _ccdc_biological_activity '?' _ccdc_polymorph '?' _ccdc_chemdiag_type 'QUEST' _ccdc_chemdiag_records ; NFRAG 1 AT1 Mo 6 E :XY 504 561 AT2 Mo 6 E :XY 484 334 AT3 O 3 E :XY 612 453 AT4 O 3 E :XY 482 453 AT5 O 3 E :XY 393 467 AT6 O 3 E :XY 427 644 AT7 O 3 E :XY 561 652 AT8 O 3 E :XY 405 260 AT9 O 3 E :XY 527 231 AT10 O 1 E :XY 618 575 AT11 O 1 E :XY 575 325 AT12 O 2 1 E :XY 561 783 AT13 C 1 3 E :XY 638 794 AT14 C 1 3 E :XY 649 678 AT15 C 1 3 E :XY 345 632 AT16 C 1 3 E :XY 305 450 AT17 C 1 3 E :XY 544 447 AT18 C 1 3 E :XY 695 493 AT19 C 1 3 E :XY 598 194 AT20 C 1 3 E :XY 336 226 AT21 Li 5 E :XY 493 729 AT22 Li 2 E :XY 447 154 AT23 O 1 E :XY 459 846 AT24 O 1 E :XY 373 777 BO 1 3 1 BO 2 3 1 BO 1 4 1 BO 2 4 1 BO 1 5 1 BO 2 5 1 BO 1 6 1 BO 1 7 1 BO 2 8 1 BO 2 9 1 BO 1 10 2 BO 2 11 2 BO 12 13 1 BO 7 14 1 BO 6 15 1 BO 5 16 1 BO 4 17 1 BO 3 18 1 BO 9 19 1 BO 8 20 1 BO 12 21 1 BO 7 21 1 BO 6 21 1 BO 9 22 6 BO 8 22 6 BO 21 23 6 BO 21 24 6 END ; #---------------------------------------------------------------- #5 Other data relating to the structure determination and refinement _ccdc_temp_data_collection ? _ccdc_ls_R_squared ? _refine_ls_abs_structure_details '?' _ccdc_disorder '?' _ccdc_comments '?' #---------------------------------------------------------------- #6 Include your "standard" CIF file here _audit_creation_method SHELXL _chemical_name_systematic ; Lithium-heptamethoxy-methanol-dioxo-di-molybdenum(v) ; _chemical_name_common '?' _chemical_formula_moiety 'C8 H25 Li1 Mo2 O10' _chemical_formula_sum 'C8 H25 Li1 Mo2 O10' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_weight 480.10 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 '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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.449(2) _cell_length_b 14.256(3) _cell_length_c 14.223(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.33(3) _cell_angle_gamma 90.00 _cell_volume 1699.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 13.5 _cell_measurement_theta_max 14.5 _exptl_crystal_description ? _exptl_crystal_colour 'reddish orange' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.877 _exptl_crystal_density_method ? _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 1.515 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'CAD4 Enraf Nonius' _diffrn_measurement_method ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.0 _diffrn_reflns_number 5049 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 28.97 _reflns_number_total 4509 _reflns_number_observed 3058 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 Enraf-Nonius' _computing_cell_refinement 'CAD4 Enraf-Nonius' _computing_data_reduction 'SHELXTL PLUS 5 (gamma version)' _computing_structure_solution 'SHELXTL PLUS 5 (gamma verion)' _computing_structure_refinement 'SHELXTL PLUS 5 (gamma version)' _computing_molecular_graphics 'SHELXTL PLUS 5 (gamma version)' _computing_publication_material 'SHELXTL PLUS 5 (gamma version)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 13 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+2.4710P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4496 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0698 _refine_ls_R_factor_obs 0.0337 _refine_ls_wR_factor_all 0.1030 _refine_ls_wR_factor_obs 0.0886 _refine_ls_goodness_of_fit_all 1.238 _refine_ls_goodness_of_fit_obs 1.374 _refine_ls_restrained_S_all 1.299 _refine_ls_restrained_S_obs 1.374 _refine_ls_shift/esd_max 0.186 _refine_ls_shift/esd_mean 0.009 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo -0.39492(4) 0.20116(3) 0.55981(2) 0.02239(10) Uani 1 d . . Mo2 Mo -0.07919(4) 0.20284(3) 0.56872(2) 0.02215(10) Uani 1 d . . Li1 Li -0.7138(10) 0.2281(6) 0.6523(6) 0.036(2) Uani 1 d . . O1 O -0.2445(3) 0.3069(2) 0.5177(2) 0.0281(6) Uani 1 d . . O2 O -0.2243(3) 0.2374(2) 0.6778(2) 0.0260(6) Uani 1 d . . O3 O -0.2325(3) 0.0928(2) 0.5873(2) 0.0254(6) Uani 1 d . . O4 O -0.4469(4) 0.1698(2) 0.4453(2) 0.0345(7) Uani 1 d . . O5 O -0.5476(4) 0.2996(2) 0.5833(3) 0.0357(8) Uani 1 d . . O6 O -0.5349(3) 0.1327(2) 0.6338(2) 0.0309(7) Uani 1 d . . O7 O 0.0792(4) 0.3024(2) 0.5988(3) 0.0362(8) Uani 1 d . . O8 O -0.0598(4) 0.1691(3) 0.4575(2) 0.0356(7) Uani 1 d . . O9 O 0.0869(4) 0.1362(2) 0.6501(2) 0.0308(7) Uani 1 d . . O10 O -0.6698(5) 0.2601(4) 0.7880(3) 0.0624(13) Uani 1 d . . C1 C -0.2567(8) 0.3445(5) 0.4243(4) 0.0458(13) Uani 1 d . . C2 C -0.2241(7) 0.3242(4) 0.7276(4) 0.0398(12) Uani 1 d . . C3 C -0.2413(7) 0.0081(4) 0.5324(5) 0.0448(14) Uani 1 d . . C5 C -0.5431(10) 0.3958(5) 0.5662(8) 0.064(2) Uani 1 d . . C6 C -0.4970(7) 0.0575(4) 0.6971(4) 0.0406(12) Uani 1 d . . C7 C 0.0654(8) 0.4000(4) 0.5859(7) 0.056(2) Uani 1 d . . C9 C 0.0708(8) 0.0562(5) 0.7064(5) 0.049(2) Uani 1 d . . C10 C -0.7915(9) 0.2658(10) 0.8458(7) 0.079(3) Uani 1 d . . H1 H -0.5696(129) 0.2765(73) 0.8131(74) 0.139(41) Uiso 1 d . . H11 H -0.1649(94) 0.3749(55) 0.4096(51) 0.077(24) Uiso 1 d . . H12 H -0.3572(133) 0.3657(79) 0.3987(73) 0.143(41) Uiso 1 d . . H13 H -0.2517(116) 0.2947(66) 0.3756(74) 0.115(35) Uiso 1 d . . H21 H -0.3262(90) 0.3238(50) 0.7641(52) 0.077(23) Uiso 1 d . . H22 H -0.1308(98) 0.3227(56) 0.7890(59) 0.096(27) Uiso 1 d . . H23 H -0.2324(90) 0.3785(53) 0.6870(52) 0.082(24) Uiso 1 d . . H31 H -0.2394(103) 0.0290(66) 0.4657(67) 0.111(34) Uiso 1 d . . H32 H -0.1530(90) -0.0255(50) 0.5447(50) 0.071(22) Uiso 1 d . . H33 H -0.3310(89) -0.0224(52) 0.5293(51) 0.074(23) Uiso 1 d . . H51 H -0.5908(118) 0.4322(71) 0.6184(68) 0.124(35) Uiso 1 d . . H52 H -0.4611(85) 0.4116(47) 0.5585(46) 0.050(20) Uiso 1 d . . H53 H -0.5800(81) 0.4105(51) 0.5065(50) 0.062(23) Uiso 1 d . . H61 H -0.3839(75) 0.0555(41) 0.7241(41) 0.048(17) Uiso 1 d . . H62 H -0.5249(72) 0.0006(46) 0.6650(43) 0.052(18) Uiso 1 d . . H63 H -0.5374(88) 0.0642(53) 0.7520(52) 0.076(24) Uiso 1 d . . H71 H 0.1268(86) 0.4254(48) 0.6393(49) 0.066(22) Uiso 1 d . . H72 H 0.0980(71) 0.4122(44) 0.5236(44) 0.048(18) Uiso 1 d . . H73 H -0.0304(64) 0.4213(34) 0.5751(33) 0.023(12) Uiso 1 d . . H91 H 0.0915(84) -0.0078(52) 0.6600(51) 0.076(22) Uiso 1 d . . H92 H -0.0009(112) 0.0508(67) 0.7230(66) 0.100(36) Uiso 1 d . . H93 H 0.1515(87) 0.0593(49) 0.7585(50) 0.071(22) Uiso 1 d . . H101 H -0.7594(109) 0.2315(67) 0.8939(73) 0.098(35) Uiso 1 d . . H102 H -0.8899(91) 0.2336(52) 0.8148(50) 0.072(22) Uiso 1 d . . H103 H -0.8091(182) 0.3344(116) 0.8366(113) 0.230(78) Uiso 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 Mo1 0.0136(2) 0.0237(2) 0.0296(2) -0.00041(15) 0.00204(12) 0.00056(13) Mo2 0.0142(2) 0.0232(2) 0.0293(2) 0.00154(15) 0.00399(12) 0.00092(14) Li1 0.027(4) 0.042(5) 0.038(4) -0.003(4) 0.003(3) -0.002(3) O1 0.0218(14) 0.027(2) 0.035(2) 0.0068(13) 0.0028(12) 0.0033(12) O2 0.0208(14) 0.0284(14) 0.029(2) -0.0038(12) 0.0041(11) -0.0012(12) O3 0.0169(13) 0.0222(14) 0.037(2) -0.0013(12) 0.0027(12) 0.0004(11) O4 0.025(2) 0.042(2) 0.034(2) -0.0036(14) -0.0053(13) -0.0018(14) O5 0.0199(14) 0.030(2) 0.059(2) 0.003(2) 0.0120(14) 0.0074(13) O6 0.0188(14) 0.033(2) 0.042(2) 0.0039(14) 0.0087(12) -0.0019(13) O7 0.0209(15) 0.029(2) 0.059(2) 0.005(2) 0.0037(14) -0.0052(13) O8 0.026(2) 0.048(2) 0.035(2) 0.002(2) 0.0111(13) 0.0046(15) O9 0.0191(14) 0.031(2) 0.042(2) 0.0089(14) 0.0033(13) 0.0023(12) O10 0.029(2) 0.110(4) 0.049(2) -0.027(3) 0.006(2) -0.002(2) C1 0.049(3) 0.046(3) 0.042(3) 0.020(3) 0.008(2) 0.006(3) C2 0.044(3) 0.036(3) 0.040(3) -0.016(2) 0.007(2) -0.001(2) C3 0.031(3) 0.028(2) 0.076(4) -0.018(3) 0.006(3) 0.000(2) C5 0.048(4) 0.033(3) 0.115(7) 0.014(4) 0.025(4) 0.013(3) C6 0.040(3) 0.039(3) 0.045(3) 0.009(2) 0.011(2) -0.002(2) C7 0.036(3) 0.033(3) 0.099(6) 0.010(3) 0.003(3) -0.006(3) C9 0.038(3) 0.046(3) 0.061(4) 0.025(3) -0.006(3) -0.001(3) C10 0.035(3) 0.132(9) 0.069(5) -0.038(6) 0.011(3) -0.012(5) _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 Mo1 O4 1.692(3) . ? Mo1 O6 1.944(3) . ? Mo1 O5 1.963(3) . ? Mo1 O3 2.070(3) . ? Mo1 O1 2.108(3) . ? Mo1 O2 2.132(3) . ? Mo1 Mo2 2.6545(7) . ? Mo1 Li1 3.169(9) . ? Mo2 O8 1.681(3) . ? Mo2 O9 1.949(3) . ? Mo2 O7 1.961(3) . ? Mo2 O3 2.072(3) . ? Mo2 O1 2.102(3) . ? Mo2 O2 2.154(3) . ? Mo2 Li1 3.184(8) 1_655 ? Li1 O10 1.972(9) . ? Li1 O6 2.075(9) . ? Li1 O5 2.080(9) . ? Li1 O7 2.103(9) 1_455 ? Li1 O9 2.130(9) 1_455 ? Li1 Mo2 3.184(8) 1_455 ? O1 C1 1.424(6) . ? O2 C2 1.426(6) . ? O3 C3 1.435(6) . ? O5 C5 1.394(7) . ? O6 C6 1.409(6) . ? O7 C7 1.405(7) . ? O7 Li1 2.103(9) 1_655 ? O9 C9 1.410(6) . ? O9 Li1 2.130(9) 1_655 ? O10 C10 1.398(9) . ? 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 Mo1 O6 106.7(2) . . ? O4 Mo1 O5 104.9(2) . . ? O6 Mo1 O5 78.94(14) . . ? O4 Mo1 O3 93.97(14) . . ? O6 Mo1 O3 87.55(13) . . ? O5 Mo1 O3 159.24(14) . . ? O4 Mo1 O1 90.44(15) . . ? O6 Mo1 O1 160.74(14) . . ? O5 Mo1 O1 88.31(13) . . ? O3 Mo1 O1 100.26(11) . . ? O4 Mo1 O2 152.66(14) . . ? O6 Mo1 O2 95.30(13) . . ? O5 Mo1 O2 94.93(14) . . ? O3 Mo1 O2 70.50(11) . . ? O1 Mo1 O2 71.26(12) . . ? O4 Mo1 Mo2 100.62(12) . . ? O6 Mo1 Mo2 130.99(9) . . ? O5 Mo1 Mo2 131.58(10) . . ? O3 Mo1 Mo2 50.19(8) . . ? O1 Mo1 Mo2 50.82(8) . . ? O2 Mo1 Mo2 52.10(8) . . ? O4 Mo1 Li1 107.6(2) . . ? O6 Mo1 Li1 39.4(2) . . ? O5 Mo1 Li1 39.7(2) . . ? O3 Mo1 Li1 126.2(2) . . ? O1 Mo1 Li1 127.4(2) . . ? O2 Mo1 Li1 99.7(2) . . ? Mo2 Mo1 Li1 151.82(15) . . ? O8 Mo2 O9 105.6(2) . . ? O8 Mo2 O7 105.5(2) . . ? O9 Mo2 O7 78.69(14) . . ? O8 Mo2 O3 92.3(2) . . ? O9 Mo2 O3 88.26(12) . . ? O7 Mo2 O3 160.13(14) . . ? O8 Mo2 O1 90.99(15) . . ? O9 Mo2 O1 161.01(14) . . ? O7 Mo2 O1 88.22(13) . . ? O3 Mo2 O1 100.36(11) . . ? O8 Mo2 O2 151.15(14) . . ? O9 Mo2 O2 96.72(13) . . ? O7 Mo2 O2 96.47(14) . . ? O3 Mo2 O2 70.02(12) . . ? O1 Mo2 O2 70.93(12) . . ? O8 Mo2 Mo1 99.80(12) . . ? O9 Mo2 Mo1 131.86(10) . . ? O7 Mo2 Mo1 132.12(10) . . ? O3 Mo2 Mo1 50.10(8) . . ? O1 Mo2 Mo1 51.01(8) . . ? O2 Mo2 Mo1 51.35(8) . . ? O8 Mo2 Li1 100.2(2) . 1_655 ? O9 Mo2 Li1 40.8(2) . 1_655 ? O7 Mo2 Li1 40.0(2) . 1_655 ? O3 Mo2 Li1 129.0(2) . 1_655 ? O1 Mo2 Li1 128.2(2) . 1_655 ? O2 Mo2 Li1 108.6(2) . 1_655 ? Mo1 Mo2 Li1 160.0(2) . 1_655 ? O10 Li1 O6 103.1(4) . . ? O10 Li1 O5 107.1(4) . . ? O6 Li1 O5 73.4(3) . . ? O10 Li1 O7 106.4(4) . 1_455 ? O6 Li1 O7 150.5(5) . 1_455 ? O5 Li1 O7 99.4(4) . 1_455 ? O10 Li1 O9 102.0(4) . 1_455 ? O6 Li1 O9 100.5(4) . 1_455 ? O5 Li1 O9 150.9(5) . 1_455 ? O7 Li1 O9 71.7(3) 1_455 1_455 ? O10 Li1 Mo1 111.7(3) . . ? O6 Li1 Mo1 36.5(2) . . ? O5 Li1 Mo1 37.1(2) . . ? O7 Li1 Mo1 128.5(4) 1_455 . ? O9 Li1 Mo1 129.1(4) 1_455 . ? O10 Li1 Mo2 116.4(4) . 1_455 ? O6 Li1 Mo2 124.4(3) . 1_455 ? O5 Li1 Mo2 124.1(4) . 1_455 ? O7 Li1 Mo2 36.9(2) 1_455 1_455 ? O9 Li1 Mo2 36.7(2) 1_455 1_455 ? Mo1 Li1 Mo2 131.8(3) . 1_455 ? C1 O1 Mo2 123.6(3) . . ? C1 O1 Mo1 124.0(3) . . ? Mo2 O1 Mo1 78.17(10) . . ? C2 O2 Mo1 124.0(3) . . ? C2 O2 Mo2 126.3(3) . . ? Mo1 O2 Mo2 76.55(10) . . ? C3 O3 Mo1 122.5(3) . . ? C3 O3 Mo2 123.9(3) . . ? Mo1 O3 Mo2 79.71(10) . . ? C5 O5 Mo1 129.8(4) . . ? C5 O5 Li1 126.8(5) . . ? Mo1 O5 Li1 103.2(3) . . ? C6 O6 Mo1 128.5(3) . . ? C6 O6 Li1 121.8(4) . . ? Mo1 O6 Li1 104.0(3) . . ? C7 O7 Mo2 130.2(4) . . ? C7 O7 Li1 126.7(4) . 1_655 ? Mo2 O7 Li1 103.1(3) . 1_655 ? C9 O9 Mo2 128.1(3) . . ? C9 O9 Li1 128.5(4) . 1_655 ? Mo2 O9 Li1 102.5(3) . 1_655 ? C10 O10 Li1 121.9(5) . . ? _refine_diff_density_max 0.901 _refine_diff_density_min -0.914 _refine_diff_density_rms 0.122 #---------------------------------------------------------------- # CCDC ELECTRONIC DATA DEPOSITION FORM (CIF, VERSION DEC95) #---------------------------------------------------------------- #1 Data block identification for start of deposition data_str_VII #---------------------------------------------------------------- #2 Person making the deposition _publ_contact_author ? _publ_contact_author_email yan@xrpent.ineos.ac.ru #---------------------------------------------------------------- #3 Publication details loop_ _publ_author_name 'V.G.Kessler' 'A.N.Panov' 'N.Ya.Turova' 'Z.A.Starikova' 'A.I.Yanovsky' 'F.M.Dolgushin' 'A.P.Pisarevsky' 'Yu.T.Struchkov' _journal_name_full 'J.Chem.Soc.,Dalton Trans.' _journal_volume '?' _journal_page_first '?' _journal_page_last '?' _journal_year '1998' _ccdc_journal_depnumber '?' #---------------------------------------------------------------- #4 Chemical and physical data _ccdc_compound_id 'VII' _ccdc_biological_activity '?' _ccdc_polymorph '?' _ccdc_chemdiag_type 'QUEST' _exptl_crystal_density_diffrn ? #---------------------------------------------------------------- #5 Other data relating to the structure determination and refinement _ccdc_temp_data_collection ? _ccdc_ls_R_squared ? _refine_ls_abs_structure_details '?' _ccdc_disorder '?' _ccdc_comments '?' #---------------------------------------------------------------- #6 Include your "standard" CIF file here _audit_creation_method SHELXL _chemical_name_systematic ; Tetralithium-hexakis(2-methoxyethoxy)-tetrakis(2- -methoxyethanol)-tetraoxo-di-tungsten hexawolframate ; _chemical_name_common '?' _chemical_formula_moiety 'C30 H74 Li4 O24 W2 ++, O19 W6 --' _chemical_formula_sum 'C30 H74 Li4 O43 W8' _chemical_formula_weight 2621.5 _chemical_melting_point ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 '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 11.461(5) _cell_length_b 11.828(4) _cell_length_c 12.623(5) _cell_angle_alpha 89.90(3) _cell_angle_beta 110.73(3) _cell_angle_gamma 103.01(3) _cell_volume 1553.6(11) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 11 _cell_measurement_theta_max 12 _exptl_crystal_description ? _exptl_crystal_colour 'colourless' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 1202 _exptl_absorpt_coefficient_mu 14.843 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.246 _exptl_absorpt_correction_T_max 0.983 _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 'CAD4 Enraf-Nonius' _diffrn_measurement_method 'CAD4 Enraf-Nonius' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.0 _diffrn_reflns_number 8628 _diffrn_reflns_av_R_equivalents 0.0194 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 28.98 _reflns_number_total 8230 _reflns_number_observed 5988 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 Enraf-Nonius' _computing_cell_refinement 'CAD4 Enraf-Nonius' _computing_data_reduction 'SHELXTL PLUS 5 (gamma version)' _computing_structure_solution 'SHELXTL PLUS 5 (gamma version)' _computing_structure_refinement 'SHELXTL PLUS 5 (gamma version)' _computing_molecular_graphics 'SHELXTL PLUS 5 (gamma version)' _computing_publication_material 'SHELXTL PLUS 5 (gamma version)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 38 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1360P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8192 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0893 _refine_ls_R_factor_obs 0.0591 _refine_ls_wR_factor_all 0.1761 _refine_ls_wR_factor_obs 0.1594 _refine_ls_goodness_of_fit_all 0.976 _refine_ls_goodness_of_fit_obs 1.070 _refine_ls_restrained_S_all 1.007 _refine_ls_restrained_S_obs 1.070 _refine_ls_shift/esd_max -0.011 _refine_ls_shift/esd_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W1 W -0.35408(4) 0.47312(3) -0.00278(3) 0.02557(13) Uani 1 d . . W2 W 0.00859(5) 0.19201(4) -0.54309(4) 0.03486(15) Uani 1 d . . W3 W -0.11775(5) -0.06318(4) -0.69044(4) 0.0373(2) Uani 1 d . . W4 W -0.18946(5) -0.00992(4) -0.46905(5) 0.0409(2) Uani 1 d . . Li1 Li -0.1887(21) 0.3192(21) -0.1263(16) 0.042(5) Uani 1 d . . Li2 Li -0.4897(21) 0.3521(16) 0.1927(17) 0.038(4) Uani 1 d . . O1 O -0.2021(8) 0.5275(8) 0.0968(7) 0.039(2) Uani 1 d . . O2 O -0.3282(8) 0.3923(7) -0.1018(8) 0.039(2) Uani 1 d . . O3 O -0.4450(6) 0.5473(6) 0.0961(6) 0.0262(14) Uani 1 d . . O4 O -0.3605(8) 0.4585(8) 0.3132(7) 0.041(2) Uani 1 d . . O5 O -0.4046(8) 0.3348(6) 0.0729(7) 0.033(2) Uani 1 d . . O6 O -0.4895(9) 0.1787(8) 0.1991(9) 0.048(2) Uani 1 d . . O7 O -0.6472(8) 0.3820(7) 0.0770(7) 0.036(2) Uani 1 d . . O8 O -0.6221(9) 0.3281(10) 0.2855(9) 0.057(3) Uani 1 d . . O9 O -0.2888(10) 0.2628(11) -0.2895(9) 0.063(3) Uani 1 d . . O10 O -0.0606(9) 0.3995(11) -0.1952(8) 0.056(3) Uani 1 d . . H10 H -0.0051(9) 0.3363(11) -0.1820(8) 0.079(59) Uiso 1 d R . O11 O -0.1871(10) 0.1609(9) -0.0632(8) 0.053(2) Uani 1 d . . O12 O -0.0560(10) 0.3684(8) 0.0405(8) 0.047(2) Uani 1 d . . H12 H -0.0271(10) 0.4484(8) 0.0971(8) 0.032(32) Uiso 1 d R . O13 O -0.3295(11) -0.0163(11) -0.4482(12) 0.071(3) Uani 1 d . . O14 O -0.0587(10) 0.0434(9) -0.3236(8) 0.049(2) Uani 1 d . . O15 O -0.1450(9) 0.1471(7) -0.5094(8) 0.041(2) Uani 1 d . . O16 O -0.2468(8) -0.0593(7) -0.6265(8) 0.042(2) Uani 1 d . . O17 O -0.1599(9) -0.1608(7) -0.4416(8) 0.044(2) Uani 1 d . . O18 O 0.0157(11) 0.3320(8) -0.5750(9) 0.057(3) Uani 1 d . . O19 O -0.2024(12) -0.1083(9) -0.8308(8) 0.064(3) Uani 1 d . . O20 O 0.1013(9) 0.2057(7) -0.3811(7) 0.041(2) Uani 1 d . . O21 O -0.0882(9) 0.1034(7) -0.6887(7) 0.042(2) Uani 1 d . . O22 O 0.0000 0.0000 -0.5000 0.027(2) Uani 1 d S . C1 C -0.3694(10) 0.6270(9) 0.1973(8) 0.029(2) Uani 1 d . . H1B H -0.3961(10) 0.6997(9) 0.1889(8) 0.034 Uiso 1 calc R . H1C H -0.2791(10) 0.6437(9) 0.2073(8) 0.034 Uiso 1 calc R . C2 C -0.3891(12) 0.5707(9) 0.3026(8) 0.033(2) Uani 1 d . . H2A H -0.3339(12) 0.6213(9) 0.3705(8) 0.040 Uiso 1 calc R . H2B H -0.4775(12) 0.5629(9) 0.2961(8) 0.040 Uiso 1 calc R . C3 C -0.2263(14) 0.4615(15) 0.3548(13) 0.058(4) Uani 1 d . . H3A H -0.2151(14) 0.3834(15) 0.3596(13) 0.086 Uiso 1 calc R . H3B H -0.1856(14) 0.5029(15) 0.4289(13) 0.086 Uiso 1 calc R . H3C H -0.1882(14) 0.5003(15) 0.3039(13) 0.086 Uiso 1 calc R . C4 C -0.4545(16) 0.2194(10) 0.0276(13) 0.050(3) Uani 1 d . . H4A H -0.4128(16) 0.2015(10) -0.0229(13) 0.060 Uiso 1 calc R . H4B H -0.5461(16) 0.2056(10) -0.0153(13) 0.060 Uiso 1 calc R . C5 C -0.4300(16) 0.1452(11) 0.1254(14) 0.054(4) Uani 1 d . . H5A H -0.4661(16) 0.0636(11) 0.0982(14) 0.065 Uiso 1 calc R . H5B H -0.3384(16) 0.1566(11) 0.1661(14) 0.065 Uiso 1 calc R . C6 C -0.4618(17) 0.1233(15) 0.3033(14) 0.065(4) Uani 1 d . . H6A H -0.5044(17) 0.1495(15) 0.3484(14) 0.097 Uiso 1 calc R . H6B H -0.3707(17) 0.1429(15) 0.3447(14) 0.097 Uiso 1 calc R . H6C H -0.4918(17) 0.0404(15) 0.2867(14) 0.097 Uiso 1 calc R . C7 C -0.7529(11) 0.3045(12) 0.0916(12) 0.045(3) Uani 1 d . . H7A H -0.7485(11) 0.2246(12) 0.0811(12) 0.054 Uiso 1 calc R . H7B H -0.8329(11) 0.3151(12) 0.0364(12) 0.054 Uiso 1 calc R . C8 C -0.7468(13) 0.3308(15) 0.2102(12) 0.055(4) Uani 1 d . . H8A H -0.7628(13) 0.4069(15) 0.2177(12) 0.066 Uiso 1 calc R . H8B H -0.8112(13) 0.2731(15) 0.2272(12) 0.066 Uiso 1 calc R . C9 C -0.6031(20) 0.3602(18) 0.3961(13) 0.081(6) Uani 1 d . . H9A H -0.5178(20) 0.3574(18) 0.4444(13) 0.121 Uiso 1 calc R . H9B H -0.6646(20) 0.3077(18) 0.4196(13) 0.121 Uiso 1 calc R . H9C H -0.6136(20) 0.4380(18) 0.4015(13) 0.121 Uiso 1 calc R . C10 C -0.1023(15) 0.3586(24) -0.3104(16) 0.097(8) Uani 1 d . . H10A H -0.0720(15) 0.4209(24) -0.3513(16) 0.116 Uiso 1 calc R . H10B H -0.0630(15) 0.2954(24) -0.3158(16) 0.116 Uiso 1 calc R . C11 C -0.2363(14) 0.3192(17) -0.3639(12) 0.062(4) Uani 1 d . . H11A H -0.2736(14) 0.3848(17) -0.3896(12) 0.075 Uiso 1 calc R . H11B H -0.2560(14) 0.2662(17) -0.4299(12) 0.075 Uiso 1 calc R . C12 C -0.4238(16) 0.2150(14) -0.3340(14) 0.061(4) Uani 1 d . . H12A H -0.4502(16) 0.1780(14) -0.2757(14) 0.091 Uiso 1 calc R . H12B H -0.4451(16) 0.1586(14) -0.3966(14) 0.091 Uiso 1 calc R . H12C H -0.4672(16) 0.2761(14) -0.3596(14) 0.091 Uiso 1 calc R . C13 C -0.0949(13) 0.2798(13) 0.1092(10) 0.046(3) Uani 1 d . . H13A H -0.1766(13) 0.2843(13) 0.1136(10) 0.055 Uiso 1 calc R . H13B H -0.0312(13) 0.2906(13) 0.1857(10) 0.055 Uiso 1 calc R . C14 C -0.1067(15) 0.1645(13) 0.0526(12) 0.053(3) Uani 1 d . . H14B H -0.0227(15) 0.1557(13) 0.0581(12) 0.064 Uiso 1 calc R . H14C H -0.1440(15) 0.1017(13) 0.0891(12) 0.064 Uiso 1 calc R . C15 C -0.2014(23) 0.0557(15) -0.1289(16) 0.078(6) Uani 1 d . . H15A H -0.2565(23) 0.0580(15) -0.2061(16) 0.116 Uiso 1 calc R . H15B H -0.2385(23) -0.0104(15) -0.0972(16) 0.116 Uiso 1 calc R . H15C H -0.1187(23) 0.0494(15) -0.1270(16) 0.116 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 W1 0.0164(2) 0.0352(2) 0.0302(2) 0.00863(15) 0.01281(14) 0.00911(14) W2 0.0352(3) 0.0303(2) 0.0352(2) 0.0069(2) 0.0095(2) 0.0058(2) W3 0.0406(3) 0.0366(2) 0.0265(2) 0.0033(2) 0.0074(2) 0.0012(2) W4 0.0284(3) 0.0481(3) 0.0523(3) 0.0047(2) 0.0234(2) 0.0067(2) Li1 0.035(10) 0.070(13) 0.031(9) 0.016(9) 0.011(8) 0.032(10) Li2 0.045(11) 0.033(9) 0.035(9) 0.007(7) 0.015(8) 0.008(8) O1 0.024(4) 0.052(5) 0.043(4) 0.011(4) 0.013(3) 0.013(3) O2 0.026(4) 0.052(5) 0.050(5) 0.011(4) 0.024(3) 0.015(3) O3 0.013(3) 0.041(4) 0.027(3) -0.001(3) 0.010(2) 0.008(3) O4 0.030(4) 0.054(5) 0.037(4) 0.012(4) 0.007(3) 0.015(4) O5 0.034(4) 0.033(3) 0.039(4) 0.010(3) 0.021(3) 0.009(3) O6 0.042(5) 0.051(5) 0.063(6) 0.026(4) 0.027(4) 0.024(4) O7 0.028(4) 0.041(4) 0.041(4) 0.016(3) 0.018(3) 0.005(3) O8 0.033(5) 0.093(8) 0.048(5) 0.012(5) 0.023(4) 0.008(5) O9 0.049(6) 0.090(8) 0.044(5) -0.003(5) 0.021(4) -0.001(5) O10 0.034(5) 0.097(8) 0.044(5) 0.008(5) 0.022(4) 0.018(5) O11 0.053(6) 0.059(5) 0.048(5) 0.007(4) 0.012(4) 0.024(5) O12 0.050(5) 0.052(5) 0.046(5) 0.001(4) 0.023(4) 0.017(4) O13 0.043(6) 0.087(8) 0.096(9) -0.009(7) 0.040(6) 0.014(6) O14 0.055(6) 0.057(5) 0.043(5) 0.002(4) 0.030(4) 0.005(4) O15 0.041(5) 0.040(4) 0.051(5) -0.001(4) 0.025(4) 0.010(4) O16 0.026(4) 0.046(4) 0.047(5) 0.010(4) 0.007(3) 0.005(3) O17 0.043(5) 0.040(4) 0.049(5) 0.005(4) 0.025(4) -0.003(4) O18 0.067(7) 0.039(4) 0.055(6) 0.012(4) 0.012(5) 0.012(4) O19 0.081(8) 0.052(5) 0.033(4) -0.004(4) 0.004(5) -0.009(5) O20 0.047(5) 0.037(4) 0.029(4) 0.002(3) 0.006(3) 0.006(4) O21 0.043(5) 0.044(4) 0.033(4) 0.012(3) 0.009(3) 0.004(4) O22 0.016(4) 0.028(4) 0.032(5) 0.003(4) 0.005(4) 0.003(4) C1 0.024(5) 0.035(5) 0.030(5) -0.002(4) 0.013(4) 0.008(4) C2 0.045(6) 0.039(5) 0.021(4) 0.008(4) 0.021(4) 0.006(5) C3 0.036(7) 0.080(10) 0.057(8) 0.016(7) 0.014(6) 0.019(7) C4 0.067(9) 0.032(5) 0.069(9) 0.004(6) 0.049(8) 0.007(6) C5 0.062(9) 0.035(6) 0.074(10) 0.017(6) 0.034(8) 0.015(6) C6 0.058(10) 0.079(10) 0.065(9) 0.038(9) 0.024(8) 0.030(8) C7 0.021(5) 0.057(7) 0.054(7) 0.017(6) 0.016(5) 0.001(5) C8 0.039(7) 0.086(10) 0.051(7) 0.031(7) 0.033(6) 0.007(7) C9 0.086(13) 0.103(14) 0.043(8) 0.016(9) 0.034(8) -0.017(11) C10 0.033(8) 0.177(23) 0.070(11) -0.050(13) 0.024(7) -0.004(11) C11 0.041(8) 0.104(12) 0.042(7) 0.022(8) 0.018(6) 0.012(8) C12 0.051(9) 0.058(8) 0.066(9) -0.004(7) 0.015(7) 0.008(7) C13 0.038(6) 0.076(9) 0.033(5) 0.012(6) 0.022(5) 0.016(6) C14 0.050(8) 0.064(8) 0.050(7) 0.030(7) 0.019(6) 0.023(7) C15 0.115(17) 0.066(10) 0.063(10) 0.018(8) 0.038(11) 0.035(11) _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 W1 O2 1.720(8) . ? W1 O1 1.725(8) . ? W1 O7 1.952(8) 2_465 ? W1 O5 1.971(8) . ? W1 O3 2.140(7) 2_465 ? W1 O3 2.179(7) . ? W2 O18 1.695(9) . ? W2 O15 1.916(9) . ? W2 O17 1.925(10) 2_554 ? W2 O20 1.929(8) . ? W2 O21 1.935(8) . ? W2 O22 2.3230(9) . ? W3 O19 1.708(9) . ? W3 O21 1.922(8) . ? W3 O14 1.926(10) 2_554 ? W3 O20 1.926(8) 2_554 ? W3 O16 1.929(10) . ? W3 O22 2.3268(12) . ? W4 O13 1.701(11) . ? W4 O17 1.899(9) . ? W4 O16 1.904(9) . ? W4 O14 1.909(10) . ? W4 O15 1.929(9) . ? W4 O22 2.3167(11) . ? Li1 O9 2.00(2) . ? Li1 O10 2.02(3) . ? Li1 O11 2.04(2) . ? Li1 O2 2.09(2) . ? Li1 O12 2.10(2) . ? Li2 O4 1.91(2) . ? Li2 O7 1.98(2) . ? Li2 O6 2.05(2) . ? Li2 O5 2.10(2) . ? Li2 O8 2.19(2) . ? Li2 O3 2.64(2) . ? Li2 C2 2.73(2) . ? Li2 C7 2.75(3) . ? O3 C1 1.458(11) . ? O3 W1 2.140(7) 2_465 ? O4 C3 1.43(2) . ? O4 C2 1.432(14) . ? O5 C4 1.391(14) . ? O6 C6 1.43(2) . ? O6 C5 1.44(2) . ? O7 C7 1.414(13) . ? O7 W1 1.952(8) 2_465 ? O8 C9 1.38(2) . ? O8 C8 1.42(2) . ? O9 C11 1.38(2) . ? O9 C12 1.42(2) . ? O10 C10 1.41(2) . ? O11 C14 1.42(2) . ? O11 C15 1.44(2) . ? O12 C13 1.45(2) . ? O14 W3 1.926(10) 2_554 ? O17 W2 1.925(10) 2_554 ? O20 W3 1.926(8) 2_554 ? O22 W4 2.3167(11) 2_554 ? O22 W2 2.3230(9) 2_554 ? O22 W3 2.3268(12) 2_554 ? C1 C2 1.549(14) . ? C4 C5 1.50(2) . ? C7 C8 1.50(2) . ? C10 C11 1.41(2) . ? C13 C14 1.50(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 O2 W1 O1 103.7(4) . . ? O2 W1 O7 98.1(4) . 2_465 ? O1 W1 O7 92.5(4) . 2_465 ? O2 W1 O5 92.9(4) . . ? O1 W1 O5 97.9(4) . . ? O7 W1 O5 162.6(3) 2_465 . ? O2 W1 O3 95.5(3) . 2_465 ? O1 W1 O3 160.1(3) . 2_465 ? O7 W1 O3 79.2(3) 2_465 2_465 ? O5 W1 O3 86.4(3) . 2_465 ? O2 W1 O3 163.1(3) . . ? O1 W1 O3 92.7(3) . . ? O7 W1 O3 85.0(3) 2_465 . ? O5 W1 O3 80.7(3) . . ? O3 W1 O3 68.7(3) 2_465 . ? O18 W2 O15 104.1(5) . . ? O18 W2 O17 103.8(5) . 2_554 ? O15 W2 O17 152.1(4) . 2_554 ? O18 W2 O20 103.6(4) . . ? O15 W2 O20 86.7(4) . . ? O17 W2 O20 86.4(4) 2_554 . ? O18 W2 O21 103.4(4) . . ? O15 W2 O21 86.9(4) . . ? O17 W2 O21 87.1(4) 2_554 . ? O20 W2 O21 152.9(3) . . ? O18 W2 O22 179.5(4) . . ? O15 W2 O22 76.3(3) . . ? O17 W2 O22 75.7(3) 2_554 . ? O20 W2 O22 76.5(2) . . ? O21 W2 O22 76.4(2) . . ? O19 W3 O21 102.9(4) . . ? O19 W3 O14 103.7(5) . 2_554 ? O21 W3 O14 86.9(4) . 2_554 ? O19 W3 O20 104.0(4) . 2_554 ? O21 W3 O20 153.1(3) . 2_554 ? O14 W3 O20 86.2(4) 2_554 2_554 ? O19 W3 O16 104.8(5) . . ? O21 W3 O16 87.2(4) . . ? O14 W3 O16 151.5(4) 2_554 . ? O20 W3 O16 86.5(4) 2_554 . ? O19 W3 O22 179.1(4) . . ? O21 W3 O22 76.6(2) . . ? O14 W3 O22 75.6(3) 2_554 . ? O20 W3 O22 76.5(2) 2_554 . ? O16 W3 O22 76.0(2) . . ? O13 W4 O17 104.2(5) . . ? O13 W4 O16 102.7(5) . . ? O17 W4 O16 86.3(4) . . ? O13 W4 O14 104.5(5) . . ? O17 W4 O14 87.4(4) . . ? O16 W4 O14 152.8(4) . . ? O13 W4 O15 103.2(5) . . ? O17 W4 O15 152.6(4) . . ? O16 W4 O15 87.4(4) . . ? O14 W4 O15 86.2(4) . . ? O13 W4 O22 179.1(5) . . ? O17 W4 O22 76.4(3) . . ? O16 W4 O22 76.6(3) . . ? O14 W4 O22 76.1(3) . . ? O15 W4 O22 76.2(3) . . ? O9 Li1 O10 80.7(9) . . ? O9 Li1 O11 97.8(11) . . ? O10 Li1 O11 122.9(11) . . ? O9 Li1 O2 96.0(9) . . ? O10 Li1 O2 124.5(12) . . ? O11 Li1 O2 112.5(12) . . ? O9 Li1 O12 169.5(12) . . ? O10 Li1 O12 92.5(10) . . ? O11 Li1 O12 79.2(8) . . ? O2 Li1 O12 94.4(9) . . ? O4 Li2 O7 127.7(11) . . ? O4 Li2 O6 117.6(11) . . ? O7 Li2 O6 113.5(10) . . ? O4 Li2 O5 105.3(11) . . ? O7 Li2 O5 93.4(9) . . ? O6 Li2 O5 80.3(8) . . ? O4 Li2 O8 91.3(9) . . ? O7 Li2 O8 78.1(9) . . ? O6 Li2 O8 89.9(9) . . ? O5 Li2 O8 163.3(11) . . ? O4 Li2 O3 75.5(7) . . ? O7 Li2 O3 67.0(6) . . ? O6 Li2 O3 148.1(11) . . ? O5 Li2 O3 68.0(6) . . ? O8 Li2 O3 120.0(9) . . ? O4 Li2 C2 29.7(5) . . ? O7 Li2 C2 98.0(8) . . ? O6 Li2 C2 146.8(10) . . ? O5 Li2 C2 109.1(9) . . ? O8 Li2 C2 86.5(8) . . ? O3 Li2 C2 54.3(4) . . ? O4 Li2 C7 136.0(11) . . ? O7 Li2 C7 29.5(5) . . ? O6 Li2 C7 92.6(8) . . ? O5 Li2 C7 111.2(9) . . ? O8 Li2 C7 55.4(6) . . ? O3 Li2 C7 95.8(7) . . ? C2 Li2 C7 111.9(8) . . ? W1 O2 Li1 141.9(7) . . ? C1 O3 W1 125.1(6) . 2_465 ? C1 O3 W1 121.5(5) . . ? W1 O3 W1 111.3(3) 2_465 . ? C1 O3 Li2 99.7(7) . . ? W1 O3 Li2 91.4(5) 2_465 . ? W1 O3 Li2 92.6(5) . . ? C3 O4 C2 114.4(10) . . ? C3 O4 Li2 125.0(11) . . ? C2 O4 Li2 108.8(9) . . ? C4 O5 W1 128.5(8) . . ? C4 O5 Li2 104.9(9) . . ? W1 O5 Li2 118.5(6) . . ? C6 O6 C5 113.8(11) . . ? C6 O6 Li2 122.5(11) . . ? C5 O6 Li2 110.7(10) . . ? C7 O7 W1 127.8(8) . 2_465 ? C7 O7 Li2 106.8(9) . . ? W1 O7 Li2 121.9(7) 2_465 . ? C9 O8 C8 111.9(13) . . ? C9 O8 Li2 131.5(11) . . ? C8 O8 Li2 109.8(9) . . ? C11 O9 C12 116.2(12) . . ? C11 O9 Li1 113.9(11) . . ? C12 O9 Li1 123.7(12) . . ? C10 O10 Li1 110.0(12) . . ? C14 O11 C15 113.1(12) . . ? C14 O11 Li1 114.9(10) . . ? C15 O11 Li1 124.4(11) . . ? C13 O12 Li1 105.6(10) . . ? W4 O14 W3 118.1(5) . 2_554 ? W2 O15 W4 117.3(4) . . ? W4 O16 W3 117.6(4) . . ? W4 O17 W2 118.0(4) . 2_554 ? W3 O20 W2 117.0(4) 2_554 . ? W3 O21 W2 117.0(4) . . ? W4 O22 W4 180.0 . 2_554 ? W4 O22 W2 89.89(3) . 2_554 ? W4 O22 W2 90.11(3) 2_554 2_554 ? W4 O22 W2 90.11(3) . . ? W4 O22 W2 89.89(3) 2_554 . ? W2 O22 W2 180.0 2_554 . ? W4 O22 W3 89.82(4) . . ? W4 O22 W3 90.18(4) 2_554 . ? W2 O22 W3 89.99(4) 2_554 . ? W2 O22 W3 90.01(4) . . ? W4 O22 W3 90.18(4) . 2_554 ? W4 O22 W3 89.82(4) 2_554 2_554 ? W2 O22 W3 90.01(4) 2_554 2_554 ? W2 O22 W3 89.99(4) . 2_554 ? W3 O22 W3 180.0 . 2_554 ? O3 C1 C2 109.3(8) . . ? O4 C2 C1 111.8(9) . . ? O4 C2 Li2 41.5(6) . . ? C1 C2 Li2 93.6(7) . . ? O5 C4 C5 107.0(12) . . ? O6 C5 C4 107.8(11) . . ? O7 C7 C8 107.6(10) . . ? O7 C7 Li2 43.7(6) . . ? C8 C7 Li2 83.8(9) . . ? O8 C8 C7 107.3(11) . . ? C11 C10 O10 114.5(14) . . ? O9 C11 C10 110.3(15) . . ? O12 C13 C14 106.8(10) . . ? O11 C14 C13 107.6(11) . . ? _refine_diff_density_max 7.705 _refine_diff_density_min -5.568 _refine_diff_density_rms 0.448 #----------------------------------------------------------------