Electronic Supplementary Material for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name M.Albrecht _publ_contact_author_address ; Institut fur Organische Chemie RWTH-Aachen Professor-Pirlet-Str 1 Aachen D-52074 GERMANY ; _publ_contact_author_email MARKUS.ALBRECHT@OC.RWTH-AACHEN.DE _publ_section_title ; Dicatechol cis-dioxomolybdenum(VI): a building block for a lithium cation templated monomer-dimer equillibrium ; loop_ _publ_author_name M.Albrecht 'Miriam Baumert' 'Roland Frohlich' 'Jurgen Klankermayer' 'Michael Kogej' ; C.Schalley ; # Attachment 'fro3513.cif' data_fro3513 _database_code_depnum_ccdc_archive 'CCDC 294184' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H48 Li4 Mo2 O26' _chemical_formula_weight 1140.40 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.512(1) _cell_length_b 13.150(1) _cell_length_c 17.638(1) _cell_angle_alpha 75.17(1) _cell_angle_beta 79.09(1) _cell_angle_gamma 72.49(1) _cell_volume 2443.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used 8584 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 28.28 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 0.599 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7955 _exptl_absorpt_correction_T_max 0.9155 _exptl_absorpt_process_details 'Denzo (Otwinwoski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30986 _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_av_sigmaI/netI 0.0424 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 28.30 _reflns_number_total 11940 _reflns_number_gt 9362 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'De3nzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0581P)^2^+2.9213P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11940 _refine_ls_number_parameters 647 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1154 _refine_ls_wR_factor_gt 0.1061 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 Li1 Li 1.0737(5) 1.3016(4) -0.3043(3) 0.0285(11) Uani 1 1 d . . . Li2 Li 1.0046(5) 1.2665(4) -0.0788(3) 0.0292(11) Uani 1 1 d . . . O2 O 0.9761(2) 1.1920(2) 0.02953(14) 0.0389(5) Uani 1 1 d . . . H2 H 0.9242 1.1554 0.0429 0.058 Uiso 1 1 calc R . . C2 C 1.0799(4) 1.1363(3) 0.0690(2) 0.0442(9) Uani 1 1 d . . . H2A H 1.1376 1.1816 0.0567 0.066 Uiso 1 1 calc R . . H2B H 1.1197 1.0675 0.0518 0.066 Uiso 1 1 calc R . . H2C H 1.0546 1.1210 0.1262 0.066 Uiso 1 1 calc R . . Li3 Li 0.8188(5) 1.1565(4) -0.1569(3) 0.0282(11) Uani 1 1 d . . . O3 O 0.7125(2) 1.1239(2) -0.05957(13) 0.0371(5) Uani 1 1 d . . . H3 H 0.7387 1.1260 -0.0189 0.056 Uiso 1 1 calc R . . C3 C 0.6265(4) 1.0606(3) -0.0380(2) 0.0463(9) Uani 1 1 d . . . H3A H 0.6460 1.0059 0.0105 0.069 Uiso 1 1 calc R . . H3B H 0.6304 1.0238 -0.0806 0.069 Uiso 1 1 calc R . . H3C H 0.5437 1.1082 -0.0291 0.069 Uiso 1 1 calc R . . Mo1A Mo 1.14008(2) 1.050985(18) -0.161104(13) 0.01978(7) Uani 1 1 d . . . O1A O 1.1871(2) 0.94472(16) -0.08298(12) 0.0296(5) Uani 1 1 d . . . O2A O 0.98559(18) 1.09774(16) -0.13076(12) 0.0249(4) Uani 1 1 d . . . O11A O 1.10478(18) 1.14489(15) -0.27835(11) 0.0223(4) Uani 1 1 d . . . O12A O 1.15720(19) 0.94089(15) -0.22339(12) 0.0257(4) Uani 1 1 d . . . C11A C 1.1123(3) 1.0866(2) -0.33106(16) 0.0237(6) Uani 1 1 d . . . C12A C 1.1411(3) 0.9728(2) -0.30124(17) 0.0271(6) Uani 1 1 d . . . C13A C 1.1518(4) 0.9004(3) -0.3477(2) 0.0433(9) Uani 1 1 d . . . H13A H 1.1732 0.8240 -0.3265 0.052 Uiso 1 1 calc R . . C14A C 1.1309(4) 0.9403(3) -0.4261(2) 0.0550(11) Uani 1 1 d . . . H14A H 1.1342 0.8913 -0.4583 0.066 Uiso 1 1 calc R . . C15A C 1.1055(4) 1.0508(3) -0.4574(2) 0.0489(10) Uani 1 1 d . . . H15A H 1.0946 1.0767 -0.5118 0.059 Uiso 1 1 calc R . . C16A C 1.0951(3) 1.1261(3) -0.41123(18) 0.0316(7) Uani 1 1 d . . . C17A C 1.0681(3) 1.2439(3) -0.44659(18) 0.0339(7) Uani 1 1 d . . . O18A O 1.0486(2) 1.31615(18) -0.41139(13) 0.0359(5) Uani 1 1 d . . . O19A O 1.0680(3) 1.2640(2) -0.52475(13) 0.0508(7) Uani 1 1 d . . . C20A C 1.0441(5) 1.3775(4) -0.5653(2) 0.0639(13) Uani 1 1 d . . . H20A H 0.9618 1.4174 -0.5459 0.096 Uiso 1 1 calc R . . H20B H 1.0493 1.3827 -0.6223 0.096 Uiso 1 1 calc R . . H20C H 1.1052 1.4093 -0.5554 0.096 Uiso 1 1 calc R . . O21A O 1.15689(17) 1.18469(15) -0.13200(11) 0.0209(4) Uani 1 1 d . . . O22A O 1.31935(18) 1.05766(16) -0.20656(12) 0.0260(4) Uani 1 1 d . . . C21A C 1.2669(2) 1.2069(2) -0.14890(16) 0.0203(5) Uani 1 1 d . . . C22A C 1.3568(3) 1.1366(2) -0.19172(17) 0.0235(6) Uani 1 1 d . . . C23A C 1.4724(3) 1.1533(2) -0.21499(18) 0.0295(6) Uani 1 1 d . . . H23A H 1.5333 1.1065 -0.2443 0.035 Uiso 1 1 calc R . . C24A C 1.4992(3) 1.2390(3) -0.19530(19) 0.0321(7) Uani 1 1 d . . . H24A H 1.5784 1.2509 -0.2119 0.039 Uiso 1 1 calc R . . C25A C 1.4124(3) 1.3069(2) -0.15206(18) 0.0281(6) Uani 1 1 d . . . H25A H 1.4328 1.3644 -0.1386 0.034 Uiso 1 1 calc R . . C26A C 1.2942(3) 1.2919(2) -0.12775(16) 0.0221(6) Uani 1 1 d . . . C27A C 1.2002(3) 1.3648(2) -0.08155(16) 0.0227(6) Uani 1 1 d . . . O28A O 1.09311(19) 1.36513(16) -0.06524(12) 0.0280(5) Uani 1 1 d . . . O29A O 1.2470(2) 1.43148(18) -0.05857(13) 0.0332(5) Uani 1 1 d . . . C30A C 1.1614(3) 1.5065(3) -0.0135(2) 0.0418(8) Uani 1 1 d . . . H30A H 1.0999 1.5572 -0.0466 0.063 Uiso 1 1 calc R . . H30B H 1.2059 1.5478 0.0039 0.063 Uiso 1 1 calc R . . H30C H 1.1206 1.4655 0.0328 0.063 Uiso 1 1 calc R . . Mo1B Mo 0.78434(2) 1.424028(18) -0.195467(14) 0.02234(7) Uani 1 1 d . . . O1B O 0.6329(2) 1.46938(18) -0.16429(14) 0.0349(5) Uani 1 1 d . . . O2B O 0.84197(19) 1.33134(16) -0.11361(12) 0.0267(4) Uani 1 1 d . . . O11B O 0.97632(18) 1.41445(15) -0.24884(12) 0.0248(4) Uani 1 1 d . . . O12B O 0.81353(19) 1.56141(15) -0.18728(13) 0.0273(4) Uani 1 1 d . . . C11B C 1.0171(3) 1.4945(2) -0.24099(16) 0.0230(6) Uani 1 1 d . . . C12B C 0.9287(3) 1.5752(2) -0.20534(17) 0.0259(6) Uani 1 1 d . . . C13B C 0.9577(3) 1.6608(3) -0.1893(2) 0.0364(7) Uani 1 1 d . . . H13B H 0.8967 1.7128 -0.1643 0.044 Uiso 1 1 calc R . . C14B C 1.0766(4) 1.6708(3) -0.2099(2) 0.0452(9) Uani 1 1 d . . . H14B H 1.0980 1.7287 -0.1978 0.054 Uiso 1 1 calc R . . C15B C 1.1639(3) 1.5968(3) -0.2480(2) 0.0383(8) Uani 1 1 d . . . H15B H 1.2446 1.6056 -0.2630 0.046 Uiso 1 1 calc R . . C16B C 1.1362(3) 1.5086(2) -0.26519(17) 0.0263(6) Uani 1 1 d . . . C17B C 1.2295(3) 1.4337(2) -0.30936(17) 0.0275(6) Uani 1 1 d . . . O18B O 1.2184(2) 1.35118(17) -0.32194(13) 0.0334(5) Uani 1 1 d . . . O19B O 1.3307(2) 1.46751(19) -0.33722(14) 0.0386(5) Uani 1 1 d . . . C20B C 1.4278(3) 1.3989(3) -0.3809(2) 0.0443(9) Uani 1 1 d . . . H20D H 1.4624 1.3301 -0.3451 0.066 Uiso 1 1 calc R . . H20E H 1.4922 1.4361 -0.4043 0.066 Uiso 1 1 calc R . . H20F H 1.3948 1.3837 -0.4229 0.066 Uiso 1 1 calc R . . O21B O 0.79583(18) 1.29066(15) -0.23782(11) 0.0213(4) Uani 1 1 d . . . O22B O 0.75567(19) 1.48627(15) -0.31431(12) 0.0272(4) Uani 1 1 d . . . C21B C 0.7749(2) 1.3052(2) -0.31297(16) 0.0217(5) Uani 1 1 d . . . C22B C 0.7554(3) 1.4146(2) -0.35558(17) 0.0246(6) Uani 1 1 d . . . C23B C 0.7385(3) 1.4384(3) -0.43439(18) 0.0312(7) Uani 1 1 d . . . H23B H 0.7286 1.5110 -0.4644 0.037 Uiso 1 1 calc R . . C24B C 0.7359(3) 1.3564(3) -0.46970(18) 0.0356(7) Uani 1 1 d . . . H24B H 0.7237 1.3734 -0.5238 0.043 Uiso 1 1 calc R . . C25B C 0.7507(3) 1.2508(3) -0.42748(18) 0.0324(7) Uani 1 1 d . . . H25B H 0.7462 1.1962 -0.4523 0.039 Uiso 1 1 calc R . . C26B C 0.7723(3) 1.2226(2) -0.34786(17) 0.0254(6) Uani 1 1 d . . . C27B C 0.7907(3) 1.1090(2) -0.30277(17) 0.0261(6) Uani 1 1 d . . . O28B O 0.8038(2) 1.07793(16) -0.23318(12) 0.0301(5) Uani 1 1 d . . . O29B O 0.7893(2) 1.04060(18) -0.34667(14) 0.0407(6) Uani 1 1 d . . . C30B C 0.8084(4) 0.9265(3) -0.3065(2) 0.0505(10) Uani 1 1 d . . . H30D H 0.8885 0.9000 -0.2867 0.076 Uiso 1 1 calc R . . H30E H 0.8061 0.8833 -0.3437 0.076 Uiso 1 1 calc R . . H30F H 0.7436 0.9194 -0.2622 0.076 Uiso 1 1 calc R . . Li4 Li 0.5150(6) 1.7801(5) -0.2585(4) 0.0444(14) Uani 1 1 d . . . O41 O 0.3627(3) 1.7595(2) -0.19806(19) 0.0570(8) Uani 1 1 d . . . H41 H 0.3084 1.8177 -0.1938 0.086 Uiso 1 1 calc R . . C42 C 0.3530(6) 1.6779(5) -0.1264(4) 0.104(2) Uani 1 1 d . . . H42A H 0.4315 1.6220 -0.1222 0.155 Uiso 1 1 calc R . . H42B H 0.2886 1.6439 -0.1278 0.155 Uiso 1 1 calc R . . H42C H 0.3322 1.7123 -0.0807 0.155 Uiso 1 1 calc R . . O43 O 0.6292(2) 1.7482(2) -0.18442(17) 0.0490(7) Uani 1 1 d . . . H43 H 0.6839 1.6888 -0.1791 0.073 Uiso 1 1 calc R . . C44 C 0.6034(5) 1.7862(4) -0.1145(3) 0.0750(15) Uani 1 1 d . . . H44A H 0.6706 1.8145 -0.1094 0.112 Uiso 1 1 calc R . . H44B H 0.5949 1.7262 -0.0694 0.112 Uiso 1 1 calc R . . H44C H 0.5268 1.8447 -0.1156 0.112 Uiso 1 1 calc R . . O45 O 0.5810(3) 1.6893(2) -0.33513(18) 0.0533(7) Uani 1 1 d . . . H45 H 0.6356 1.6302 -0.3259 0.080 Uiso 1 1 calc R . . C46 C 0.4994(7) 1.6792(7) -0.3807(6) 0.150(4) Uani 1 1 d . . . H46A H 0.4946 1.6034 -0.3681 0.225 Uiso 1 1 calc R . . H46B H 0.5287 1.6997 -0.4369 0.225 Uiso 1 1 calc R . . H46C H 0.4179 1.7273 -0.3689 0.225 Uiso 1 1 calc R . . O47 O 0.4687(3) 1.9347(2) -0.30600(16) 0.0507(7) Uani 1 1 d . . . H47 H 0.4187 1.9734 -0.2766 0.076 Uiso 1 1 calc R . . C48 C 0.4750(5) 1.9955(4) -0.3843(3) 0.0792(16) Uani 1 1 d . . . H48A H 0.3961 2.0114 -0.4042 0.119 Uiso 1 1 calc R . . H48B H 0.5399 1.9533 -0.4175 0.119 Uiso 1 1 calc R . . H48C H 0.4933 2.0640 -0.3856 0.119 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.031(3) 0.023(2) 0.030(3) -0.007(2) -0.001(2) -0.005(2) Li2 0.023(3) 0.035(3) 0.030(3) -0.012(2) 0.001(2) -0.007(2) O2 0.0401(14) 0.0470(14) 0.0321(12) 0.0000(10) -0.0051(10) -0.0220(11) C2 0.050(2) 0.0358(18) 0.050(2) -0.0002(16) -0.0186(18) -0.0154(16) Li3 0.031(3) 0.027(2) 0.025(2) 0.000(2) -0.007(2) -0.009(2) O3 0.0381(13) 0.0532(14) 0.0264(11) -0.0072(10) -0.0039(10) -0.0229(11) C3 0.042(2) 0.059(2) 0.042(2) -0.0024(18) -0.0070(16) -0.0256(18) Mo1A 0.02226(13) 0.01827(12) 0.01925(12) -0.00389(9) -0.00401(9) -0.00520(9) O1A 0.0329(12) 0.0264(10) 0.0267(11) 0.0023(8) -0.0108(9) -0.0063(9) O2A 0.0245(11) 0.0266(10) 0.0259(10) -0.0068(8) -0.0034(8) -0.0091(8) O11A 0.0291(11) 0.0178(9) 0.0198(9) -0.0060(7) -0.0042(8) -0.0034(8) O12A 0.0305(11) 0.0185(9) 0.0295(11) -0.0075(8) -0.0071(9) -0.0044(8) C11A 0.0239(15) 0.0289(14) 0.0210(14) -0.0124(11) -0.0003(11) -0.0065(11) C12A 0.0295(16) 0.0268(14) 0.0268(15) -0.0116(12) -0.0027(12) -0.0057(12) C13A 0.056(2) 0.0338(17) 0.044(2) -0.0218(16) -0.0059(17) -0.0070(16) C14A 0.075(3) 0.055(2) 0.046(2) -0.036(2) -0.004(2) -0.014(2) C15A 0.065(3) 0.061(2) 0.0251(17) -0.0198(17) -0.0069(17) -0.013(2) C16A 0.0334(17) 0.0390(17) 0.0224(15) -0.0112(13) -0.0012(12) -0.0067(14) C17A 0.0272(16) 0.050(2) 0.0210(15) -0.0016(14) -0.0024(12) -0.0102(14) O18A 0.0386(13) 0.0357(12) 0.0279(11) 0.0012(10) -0.0058(10) -0.0076(10) O19A 0.0630(18) 0.0640(17) 0.0183(11) 0.0045(11) -0.0073(11) -0.0162(14) C20A 0.072(3) 0.076(3) 0.031(2) 0.019(2) -0.011(2) -0.022(2) O21A 0.0195(10) 0.0223(9) 0.0239(10) -0.0090(8) -0.0012(8) -0.0073(7) O22A 0.0216(10) 0.0252(10) 0.0323(11) -0.0131(8) 0.0003(8) -0.0043(8) C21A 0.0187(13) 0.0208(12) 0.0215(13) -0.0027(10) -0.0037(10) -0.0059(10) C22A 0.0220(14) 0.0228(13) 0.0242(14) -0.0039(11) -0.0043(11) -0.0038(11) C23A 0.0209(15) 0.0316(15) 0.0338(16) -0.0109(13) 0.0002(12) -0.0025(12) C24A 0.0212(15) 0.0390(17) 0.0383(17) -0.0103(14) 0.0013(13) -0.0125(13) C25A 0.0248(15) 0.0318(15) 0.0318(16) -0.0098(13) -0.0039(12) -0.0108(12) C26A 0.0210(14) 0.0257(13) 0.0204(13) -0.0059(11) -0.0011(11) -0.0075(11) C27A 0.0265(15) 0.0233(13) 0.0206(13) -0.0051(11) -0.0032(11) -0.0093(11) O28A 0.0241(11) 0.0310(11) 0.0330(11) -0.0165(9) 0.0043(9) -0.0100(9) O29A 0.0304(12) 0.0383(12) 0.0421(13) -0.0255(10) 0.0008(10) -0.0146(10) C30A 0.045(2) 0.0441(19) 0.047(2) -0.0296(17) 0.0098(16) -0.0207(16) Mo1B 0.02037(13) 0.02005(12) 0.02688(14) -0.00832(10) -0.00210(10) -0.00349(9) O1B 0.0209(11) 0.0356(12) 0.0475(14) -0.0170(10) -0.0027(9) -0.0006(9) O2B 0.0299(11) 0.0256(10) 0.0251(10) -0.0072(8) -0.0055(8) -0.0051(8) O11B 0.0219(10) 0.0204(9) 0.0336(11) -0.0094(8) -0.0001(8) -0.0069(8) O12B 0.0249(11) 0.0198(9) 0.0381(12) -0.0132(9) -0.0008(9) -0.0031(8) C11B 0.0283(15) 0.0160(12) 0.0234(14) -0.0005(10) -0.0048(11) -0.0061(11) C12B 0.0291(16) 0.0183(13) 0.0292(15) -0.0030(11) -0.0041(12) -0.0061(11) C13B 0.0384(19) 0.0260(15) 0.047(2) -0.0131(14) -0.0005(15) -0.0098(13) C14B 0.047(2) 0.0353(18) 0.062(2) -0.0181(17) -0.0001(18) -0.0211(16) C15B 0.0376(19) 0.0358(17) 0.047(2) -0.0076(15) -0.0010(15) -0.0212(15) C16B 0.0250(15) 0.0255(14) 0.0275(15) -0.0006(12) -0.0022(12) -0.0102(11) C17B 0.0251(15) 0.0283(15) 0.0253(15) 0.0018(12) -0.0034(12) -0.0076(12) O18B 0.0264(12) 0.0311(11) 0.0412(13) -0.0118(10) 0.0037(9) -0.0066(9) O19B 0.0235(12) 0.0422(13) 0.0478(14) -0.0088(11) 0.0057(10) -0.0123(10) C20B 0.0267(18) 0.053(2) 0.050(2) -0.0121(18) 0.0042(15) -0.0099(16) O21B 0.0232(10) 0.0190(9) 0.0227(10) -0.0049(7) -0.0048(8) -0.0053(7) O22B 0.0314(12) 0.0206(9) 0.0285(11) -0.0029(8) -0.0062(9) -0.0054(8) C21B 0.0177(13) 0.0251(13) 0.0212(13) -0.0064(11) -0.0009(10) -0.0041(10) C22B 0.0176(14) 0.0258(14) 0.0284(15) -0.0058(12) -0.0014(11) -0.0038(11) C23B 0.0285(16) 0.0314(16) 0.0278(16) -0.0006(12) -0.0048(13) -0.0030(13) C24B 0.0375(19) 0.0449(19) 0.0205(15) -0.0065(13) -0.0044(13) -0.0052(15) C25B 0.0352(18) 0.0369(17) 0.0262(15) -0.0163(13) -0.0020(13) -0.0043(13) C26B 0.0239(15) 0.0283(14) 0.0234(14) -0.0098(12) 0.0007(11) -0.0046(11) C27B 0.0245(15) 0.0277(14) 0.0281(16) -0.0119(12) 0.0012(12) -0.0075(12) O28B 0.0371(13) 0.0248(10) 0.0297(11) -0.0064(9) -0.0073(9) -0.0079(9) O29B 0.0659(17) 0.0288(11) 0.0337(12) -0.0135(10) -0.0069(11) -0.0155(11) C30B 0.081(3) 0.0276(17) 0.048(2) -0.0120(16) -0.004(2) -0.0211(18) Li4 0.039(3) 0.032(3) 0.062(4) -0.017(3) -0.005(3) -0.004(2) O41 0.0393(16) 0.0326(13) 0.083(2) -0.0013(13) -0.0059(14) 0.0048(11) C42 0.078(4) 0.076(4) 0.142(6) 0.004(4) -0.004(4) -0.026(3) O43 0.0401(15) 0.0408(14) 0.0674(18) -0.0273(13) -0.0133(13) 0.0045(11) C44 0.061(3) 0.083(3) 0.093(4) -0.053(3) -0.010(3) -0.008(3) O45 0.0522(17) 0.0385(14) 0.0653(18) -0.0230(13) -0.0192(14) 0.0112(12) C46 0.101(5) 0.152(7) 0.222(9) -0.142(7) -0.094(6) 0.062(5) O47 0.0586(18) 0.0348(13) 0.0473(15) -0.0150(12) 0.0065(13) 0.0018(12) C48 0.095(4) 0.077(3) 0.051(3) -0.011(2) 0.009(3) -0.015(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 Li1 O18B 1.911(6) . ? Li1 O18A 1.917(6) . ? Li1 O11A 1.928(5) . ? Li1 O11B 1.935(5) . ? Li2 O2B 1.953(6) . ? Li2 O28A 1.955(6) . ? Li2 O21A 1.967(5) . ? Li2 Mo1A 3.341(5) . ? O2 C2 1.406(4) . ? Li3 O2A 1.938(6) . ? Li3 O21B 1.947(5) . ? Li3 O28B 1.952(6) . ? Li3 Mo1B 3.322(5) . ? O3 C3 1.417(4) . ? Mo1A O2A 1.726(2) . ? Mo1A O1A 1.7282(19) . ? Mo1A O12A 1.9753(19) . ? Mo1A O21A 2.0240(18) . ? Mo1A O22A 2.087(2) . ? Mo1A O11A 2.1622(19) . ? O11A C11A 1.324(3) . ? O12A C12A 1.360(4) . ? C11A C16A 1.406(4) . ? C11A C12A 1.412(4) . ? C12A C13A 1.373(4) . ? C13A C14A 1.387(5) . ? C14A C15A 1.377(6) . ? C15A C16A 1.401(5) . ? C16A C17A 1.475(5) . ? C17A O18A 1.208(4) . ? C17A O19A 1.336(4) . ? O19A C20A 1.448(5) . ? O21A C21A 1.347(3) . ? O22A C22A 1.335(3) . ? C21A C26A 1.398(4) . ? C21A C22A 1.408(4) . ? C22A C23A 1.383(4) . ? C23A C24A 1.391(4) . ? C24A C25A 1.379(4) . ? C25A C26A 1.404(4) . ? C26A C27A 1.483(4) . ? C27A O28A 1.211(3) . ? C27A O29A 1.331(3) . ? O29A C30A 1.448(4) . ? Mo1B O1B 1.696(2) . ? Mo1B O2B 1.728(2) . ? Mo1B O12B 1.9786(19) . ? Mo1B O21B 2.0360(18) . ? Mo1B O22B 2.096(2) . ? Mo1B O11B 2.212(2) . ? O11B C11B 1.320(3) . ? O12B C12B 1.359(4) . ? C11B C16B 1.410(4) . ? C11B C12B 1.417(4) . ? C12B C13B 1.372(4) . ? C13B C14B 1.385(5) . ? C14B C15B 1.378(5) . ? C15B C16B 1.406(4) . ? C16B C17B 1.473(4) . ? C17B O18B 1.209(4) . ? C17B O19B 1.335(4) . ? O19B C20B 1.442(4) . ? O21B C21B 1.347(3) . ? O22B C22B 1.331(4) . ? C21B C26B 1.389(4) . ? C21B C22B 1.415(4) . ? C22B C23B 1.382(4) . ? C23B C24B 1.387(5) . ? C24B C25B 1.374(5) . ? C25B C26B 1.408(4) . ? C26B C27B 1.474(4) . ? C27B O28B 1.214(4) . ? C27B O29B 1.333(4) . ? O29B C30B 1.455(4) . ? O41 C42 1.444(6) . ? O43 C44 1.395(5) . ? O45 C46 1.400(6) . ? O47 C48 1.408(5) . ? 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 O18B Li1 O18A 100.0(3) . . ? O18B Li1 O11A 113.8(3) . . ? O18A Li1 O11A 94.6(2) . . ? O18B Li1 O11B 94.0(2) . . ? O18A Li1 O11B 118.3(3) . . ? O11A Li1 O11B 132.7(3) . . ? O2B Li2 O28A 117.7(3) . . ? O2B Li2 O21A 130.1(3) . . ? O28A Li2 O21A 89.4(2) . . ? O2B Li2 Mo1A 107.7(2) . . ? O28A Li2 Mo1A 123.0(2) . . ? O21A Li2 Mo1A 33.71(11) . . ? O2A Li3 O21B 113.4(3) . . ? O2A Li3 O28B 106.4(3) . . ? O21B Li3 O28B 89.8(2) . . ? O2A Li3 Mo1B 102.6(2) . . ? O21B Li3 Mo1B 34.35(11) . . ? O28B Li3 Mo1B 123.9(2) . . ? O2A Mo1A O1A 102.01(10) . . ? O2A Mo1A O12A 107.04(9) . . ? O1A Mo1A O12A 88.02(9) . . ? O2A Mo1A O21A 85.49(8) . . ? O1A Mo1A O21A 104.91(9) . . ? O12A Mo1A O21A 159.99(8) . . ? O2A Mo1A O22A 158.28(9) . . ? O1A Mo1A O22A 93.00(9) . . ? O12A Mo1A O22A 88.89(8) . . ? O21A Mo1A O22A 75.46(8) . . ? O2A Mo1A O11A 87.88(9) . . ? O1A Mo1A O11A 162.62(9) . . ? O12A Mo1A O11A 75.34(7) . . ? O21A Mo1A O11A 89.94(7) . . ? O22A Mo1A O11A 81.88(8) . . ? O2A Mo1A Li2 53.15(11) . . ? O1A Mo1A Li2 104.70(12) . . ? O12A Mo1A Li2 157.89(11) . . ? O21A Mo1A Li2 32.64(10) . . ? O22A Mo1A Li2 108.04(10) . . ? O11A Mo1A Li2 92.67(10) . . ? Mo1A O2A Li3 149.04(19) . . ? C11A O11A Li1 123.0(2) . . ? C11A O11A Mo1A 115.15(17) . . ? Li1 O11A Mo1A 121.73(18) . . ? C12A O12A Mo1A 120.12(17) . . ? O11A C11A C16A 127.2(3) . . ? O11A C11A C12A 114.5(2) . . ? C16A C11A C12A 118.3(3) . . ? O12A C12A C13A 123.0(3) . . ? O12A C12A C11A 114.9(2) . . ? C13A C12A C11A 122.2(3) . . ? C12A C13A C14A 119.0(3) . . ? C15A C14A C13A 120.1(3) . . ? C14A C15A C16A 121.7(3) . . ? C15A C16A C11A 118.6(3) . . ? C15A C16A C17A 120.4(3) . . ? C11A C16A C17A 121.0(3) . . ? O18A C17A O19A 122.1(3) . . ? O18A C17A C16A 125.9(3) . . ? O19A C17A C16A 112.0(3) . . ? C17A O18A Li1 127.3(3) . . ? C17A O19A C20A 116.3(3) . . ? C21A O21A Li2 127.6(2) . . ? C21A O21A Mo1A 118.72(16) . . ? Li2 O21A Mo1A 113.66(18) . . ? C22A O22A Mo1A 116.79(17) . . ? O21A C21A C26A 125.1(2) . . ? O21A C21A C22A 114.2(2) . . ? C26A C21A C22A 120.7(3) . . ? O22A C22A C23A 125.7(3) . . ? O22A C22A C21A 114.6(2) . . ? C23A C22A C21A 119.7(3) . . ? C22A C23A C24A 119.7(3) . . ? C25A C24A C23A 120.9(3) . . ? C24A C25A C26A 120.6(3) . . ? C21A C26A C25A 118.3(3) . . ? C21A C26A C27A 120.7(2) . . ? C25A C26A C27A 121.0(3) . . ? O28A C27A O29A 122.6(3) . . ? O28A C27A C26A 125.3(3) . . ? O29A C27A C26A 112.0(2) . . ? C27A O28A Li2 131.4(2) . . ? C27A O29A C30A 116.0(2) . . ? O1B Mo1B O2B 103.61(11) . . ? O1B Mo1B O12B 90.90(10) . . ? O2B Mo1B O12B 103.54(9) . . ? O1B Mo1B O21B 104.15(9) . . ? O2B Mo1B O21B 85.51(8) . . ? O12B Mo1B O21B 160.26(8) . . ? O1B Mo1B O22B 92.02(10) . . ? O2B Mo1B O22B 157.90(9) . . ? O12B Mo1B O22B 91.56(8) . . ? O21B Mo1B O22B 75.45(8) . . ? O1B Mo1B O11B 163.88(9) . . ? O2B Mo1B O11B 87.63(9) . . ? O12B Mo1B O11B 75.06(8) . . ? O21B Mo1B O11B 88.02(7) . . ? O22B Mo1B O11B 80.69(8) . . ? O1B Mo1B Li3 101.00(12) . . ? O2B Mo1B Li3 54.09(11) . . ? O12B Mo1B Li3 156.47(11) . . ? O21B Mo1B Li3 32.65(10) . . ? O22B Mo1B Li3 108.05(10) . . ? O11B Mo1B Li3 94.95(10) . . ? Mo1B O2B Li2 135.14(19) . . ? C11B O11B Li1 123.2(2) . . ? C11B O11B Mo1B 113.69(17) . . ? Li1 O11B Mo1B 123.07(18) . . ? C12B O12B Mo1B 119.91(17) . . ? O11B C11B C16B 127.4(3) . . ? O11B C11B C12B 115.0(3) . . ? C16B C11B C12B 117.6(3) . . ? O12B C12B C13B 122.3(3) . . ? O12B C12B C11B 115.5(2) . . ? C13B C12B C11B 122.3(3) . . ? C12B C13B C14B 119.4(3) . . ? C15B C14B C13B 120.1(3) . . ? C14B C15B C16B 121.5(3) . . ? C15B C16B C11B 119.0(3) . . ? C15B C16B C17B 120.4(3) . . ? C11B C16B C17B 120.5(3) . . ? O18B C17B O19B 121.6(3) . . ? O18B C17B C16B 125.7(3) . . ? O19B C17B C16B 112.7(3) . . ? C17B O18B Li1 128.4(3) . . ? C17B O19B C20B 116.7(3) . . ? C21B O21B Li3 127.9(2) . . ? C21B O21B Mo1B 118.70(16) . . ? Li3 O21B Mo1B 113.00(18) . . ? C22B O22B Mo1B 116.57(17) . . ? O21B C21B C26B 124.7(2) . . ? O21B C21B C22B 114.0(2) . . ? C26B C21B C22B 121.3(3) . . ? O22B C22B C23B 125.8(3) . . ? O22B C22B C21B 115.2(3) . . ? C23B C22B C21B 119.0(3) . . ? C22B C23B C24B 120.0(3) . . ? C25B C24B C23B 120.9(3) . . ? C24B C25B C26B 120.8(3) . . ? C21B C26B C25B 117.9(3) . . ? C21B C26B C27B 121.1(3) . . ? C25B C26B C27B 121.0(3) . . ? O28B C27B O29B 121.8(3) . . ? O28B C27B C26B 125.7(3) . . ? O29B C27B C26B 112.5(3) . . ? C27B O28B Li3 130.6(2) . . ? C27B O29B C30B 115.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2B Li2 Mo1A O2A -33.39(17) . . . . ? O28A Li2 Mo1A O2A -175.5(3) . . . . ? O21A Li2 Mo1A O2A -171.1(2) . . . . ? O2B Li2 Mo1A O1A -127.5(2) . . . . ? O28A Li2 Mo1A O1A 90.4(3) . . . . ? O21A Li2 Mo1A O1A 94.79(19) . . . . ? O2B Li2 Mo1A O12A -4.1(4) . . . . ? O28A Li2 Mo1A O12A -146.2(2) . . . . ? O21A Li2 Mo1A O12A -141.8(2) . . . . ? O2B Li2 Mo1A O21A 137.7(3) . . . . ? O28A Li2 Mo1A O21A -4.42(16) . . . . ? O2B Li2 Mo1A O22A 134.28(19) . . . . ? O28A Li2 Mo1A O22A -7.8(3) . . . . ? O21A Li2 Mo1A O22A -3.4(2) . . . . ? O2B Li2 Mo1A O11A 52.0(2) . . . . ? O28A Li2 Mo1A O11A -90.2(3) . . . . ? O21A Li2 Mo1A O11A -85.73(18) . . . . ? O1A Mo1A O2A Li3 -142.4(4) . . . . ? O12A Mo1A O2A Li3 -50.8(4) . . . . ? O21A Mo1A O2A Li3 113.3(4) . . . . ? O22A Mo1A O2A Li3 84.8(4) . . . . ? O11A Mo1A O2A Li3 23.2(4) . . . . ? Li2 Mo1A O2A Li3 118.1(4) . . . . ? O21B Li3 O2A Mo1A -56.5(5) . . . . ? O28B Li3 O2A Mo1A 40.6(5) . . . . ? Mo1B Li3 O2A Mo1A -90.8(4) . . . . ? O18B Li1 O11A C11A -98.0(3) . . . . ? O18A Li1 O11A C11A 5.2(4) . . . . ? O11B Li1 O11A C11A 141.3(4) . . . . ? O18B Li1 O11A Mo1A 78.5(3) . . . . ? O18A Li1 O11A Mo1A -178.34(14) . . . . ? O11B Li1 O11A Mo1A -42.2(5) . . . . ? O2A Mo1A O11A C11A -108.7(2) . . . . ? O1A Mo1A O11A C11A 16.7(4) . . . . ? O12A Mo1A O11A C11A -0.46(19) . . . . ? O21A Mo1A O11A C11A 165.83(19) . . . . ? O22A Mo1A O11A C11A 90.51(19) . . . . ? Li2 Mo1A O11A C11A -161.6(2) . . . . ? O2A Mo1A O11A Li1 74.6(2) . . . . ? O1A Mo1A O11A Li1 -160.1(3) . . . . ? O12A Mo1A O11A Li1 -177.2(2) . . . . ? O21A Mo1A O11A Li1 -10.9(2) . . . . ? O22A Mo1A O11A Li1 -86.2(2) . . . . ? Li2 Mo1A O11A Li1 21.6(2) . . . . ? O2A Mo1A O12A C12A 83.4(2) . . . . ? O1A Mo1A O12A C12A -174.6(2) . . . . ? O21A Mo1A O12A C12A -43.6(4) . . . . ? O22A Mo1A O12A C12A -81.6(2) . . . . ? O11A Mo1A O12A C12A 0.3(2) . . . . ? Li2 Mo1A O12A C12A 59.2(4) . . . . ? Li1 O11A C11A C16A -2.6(5) . . . . ? Mo1A O11A C11A C16A -179.3(3) . . . . ? Li1 O11A C11A C12A 177.3(3) . . . . ? Mo1A O11A C11A C12A 0.6(3) . . . . ? Mo1A O12A C12A C13A 180.0(3) . . . . ? Mo1A O12A C12A C11A -0.1(3) . . . . ? O11A C11A C12A O12A -0.3(4) . . . . ? C16A C11A C12A O12A 179.6(3) . . . . ? O11A C11A C12A C13A 179.6(3) . . . . ? C16A C11A C12A C13A -0.5(5) . . . . ? O12A C12A C13A C14A 178.4(3) . . . . ? C11A C12A C13A C14A -1.5(6) . . . . ? C12A C13A C14A C15A 3.0(6) . . . . ? C13A C14A C15A C16A -2.5(7) . . . . ? C14A C15A C16A C11A 0.5(6) . . . . ? C14A C15A C16A C17A 179.8(4) . . . . ? O11A C11A C16A C15A -179.1(3) . . . . ? C12A C11A C16A C15A 1.0(5) . . . . ? O11A C11A C16A C17A 1.5(5) . . . . ? C12A C11A C16A C17A -178.3(3) . . . . ? C15A C16A C17A O18A 174.4(4) . . . . ? C11A C16A C17A O18A -6.3(5) . . . . ? C15A C16A C17A O19A -6.0(5) . . . . ? C11A C16A C17A O19A 173.3(3) . . . . ? O19A C17A O18A Li1 -167.9(3) . . . . ? C16A C17A O18A Li1 11.6(5) . . . . ? O18B Li1 O18A C17A 105.3(3) . . . . ? O11A Li1 O18A C17A -9.9(4) . . . . ? O11B Li1 O18A C17A -154.5(3) . . . . ? O18A C17A O19A C20A 0.5(5) . . . . ? C16A C17A O19A C20A -179.1(3) . . . . ? O2B Li2 O21A C21A 124.3(3) . . . . ? O28A Li2 O21A C21A -2.5(3) . . . . ? Mo1A Li2 O21A C21A -178.8(3) . . . . ? O2B Li2 O21A Mo1A -57.0(4) . . . . ? O28A Li2 O21A Mo1A 176.29(14) . . . . ? O2A Mo1A O21A C21A -173.97(19) . . . . ? O1A Mo1A O21A C21A 84.78(19) . . . . ? O12A Mo1A O21A C21A -44.0(3) . . . . ? O22A Mo1A O21A C21A -4.47(18) . . . . ? O11A Mo1A O21A C21A -86.09(18) . . . . ? Li2 Mo1A O21A C21A 178.9(3) . . . . ? O2A Mo1A O21A Li2 7.2(2) . . . . ? O1A Mo1A O21A Li2 -94.1(2) . . . . ? O12A Mo1A O21A Li2 137.1(3) . . . . ? O22A Mo1A O21A Li2 176.7(2) . . . . ? O11A Mo1A O21A Li2 95.03(19) . . . . ? O2A Mo1A O22A C22A 32.7(3) . . . . ? O1A Mo1A O22A C22A -101.3(2) . . . . ? O12A Mo1A O22A C22A 170.76(19) . . . . ? O21A Mo1A O22A C22A 3.34(18) . . . . ? O11A Mo1A O22A C22A 95.41(19) . . . . ? Li2 Mo1A O22A C22A 5.2(2) . . . . ? Li2 O21A C21A C26A 3.1(4) . . . . ? Mo1A O21A C21A C26A -175.6(2) . . . . ? Li2 O21A C21A C22A -176.4(3) . . . . ? Mo1A O21A C21A C22A 4.9(3) . . . . ? Mo1A O22A C22A C23A 178.5(2) . . . . ? Mo1A O22A C22A C21A -1.9(3) . . . . ? O21A C21A C22A O22A -1.8(3) . . . . ? C26A C21A C22A O22A 178.6(2) . . . . ? O21A C21A C22A C23A 177.8(2) . . . . ? C26A C21A C22A C23A -1.7(4) . . . . ? O22A C22A C23A C24A -179.9(3) . . . . ? C21A C22A C23A C24A 0.5(4) . . . . ? C22A C23A C24A C25A 0.8(5) . . . . ? C23A C24A C25A C26A -0.8(5) . . . . ? O21A C21A C26A C25A -177.9(3) . . . . ? C22A C21A C26A C25A 1.6(4) . . . . ? O21A C21A C26A C27A 1.5(4) . . . . ? C22A C21A C26A C27A -179.0(2) . . . . ? C24A C25A C26A C21A -0.4(4) . . . . ? C24A C25A C26A C27A -179.7(3) . . . . ? C21A C26A C27A O28A -7.4(4) . . . . ? C25A C26A C27A O28A 171.9(3) . . . . ? C21A C26A C27A O29A 172.1(2) . . . . ? C25A C26A C27A O29A -8.6(4) . . . . ? O29A C27A O28A Li2 -171.2(3) . . . . ? C26A C27A O28A Li2 8.3(5) . . . . ? O2B Li2 O28A C27A -139.5(3) . . . . ? O21A Li2 O28A C27A -3.3(4) . . . . ? Mo1A Li2 O28A C27A -0.8(5) . . . . ? O28A C27A O29A C30A -0.9(4) . . . . ? C26A C27A O29A C30A 179.5(3) . . . . ? O2A Li3 Mo1B O1B -147.57(19) . . . . ? O21B Li3 Mo1B O1B 99.12(19) . . . . ? O28B Li3 Mo1B O1B 92.5(3) . . . . ? O2A Li3 Mo1B O2B -48.63(17) . . . . ? O21B Li3 Mo1B O2B -161.9(2) . . . . ? O28B Li3 Mo1B O2B -168.6(3) . . . . ? O2A Li3 Mo1B O12B -28.5(4) . . . . ? O21B Li3 Mo1B O12B -141.8(2) . . . . ? O28B Li3 Mo1B O12B -148.4(2) . . . . ? O2A Li3 Mo1B O21B 113.3(3) . . . . ? O28B Li3 Mo1B O21B -6.64(17) . . . . ? O2A Li3 Mo1B O22B 116.63(18) . . . . ? O21B Li3 Mo1B O22B 3.3(2) . . . . ? O28B Li3 Mo1B O22B -3.3(3) . . . . ? O2A Li3 Mo1B O11B 34.8(2) . . . . ? O21B Li3 Mo1B O11B -78.49(18) . . . . ? O28B Li3 Mo1B O11B -85.1(3) . . . . ? O1B Mo1B O2B Li2 -159.9(3) . . . . ? O12B Mo1B O2B Li2 -65.6(3) . . . . ? O21B Mo1B O2B Li2 96.6(3) . . . . ? O22B Mo1B O2B Li2 66.3(4) . . . . ? O11B Mo1B O2B Li2 8.4(3) . . . . ? Li3 Mo1B O2B Li2 106.2(3) . . . . ? O28A Li2 O2B Mo1B 59.5(4) . . . . ? O21A Li2 O2B Mo1B -55.7(5) . . . . ? Mo1A Li2 O2B Mo1B -85.0(3) . . . . ? O18B Li1 O11B C11B 5.0(3) . . . . ? O18A Li1 O11B C11B -98.6(3) . . . . ? O11A Li1 O11B C11B 133.0(4) . . . . ? O18B Li1 O11B Mo1B -176.75(14) . . . . ? O18A Li1 O11B Mo1B 79.6(3) . . . . ? O11A Li1 O11B Mo1B -48.8(5) . . . . ? O1B Mo1B O11B C11B 37.1(4) . . . . ? O2B Mo1B O11B C11B -97.70(19) . . . . ? O12B Mo1B O11B C11B 6.99(18) . . . . ? O21B Mo1B O11B C11B 176.71(19) . . . . ? O22B Mo1B O11B C11B 101.13(19) . . . . ? Li3 Mo1B O11B C11B -151.3(2) . . . . ? O1B Mo1B O11B Li1 -141.2(4) . . . . ? O2B Mo1B O11B Li1 83.9(2) . . . . ? O12B Mo1B O11B Li1 -171.4(2) . . . . ? O21B Mo1B O11B Li1 -1.7(2) . . . . ? O22B Mo1B O11B Li1 -77.3(2) . . . . ? Li3 Mo1B O11B Li1 30.3(2) . . . . ? O1B Mo1B O12B C12B 179.2(2) . . . . ? O2B Mo1B O12B C12B 75.0(2) . . . . ? O21B Mo1B O12B C12B -40.6(4) . . . . ? O22B Mo1B O12B C12B -88.7(2) . . . . ? O11B Mo1B O12B C12B -8.8(2) . . . . ? Li3 Mo1B O12B C12B 58.3(4) . . . . ? Li1 O11B C11B C16B -4.7(4) . . . . ? Mo1B O11B C11B C16B 176.9(2) . . . . ? Li1 O11B C11B C12B 174.0(3) . . . . ? Mo1B O11B C11B C12B -4.4(3) . . . . ? Mo1B O12B C12B C13B -169.8(2) . . . . ? Mo1B O12B C12B C11B 9.5(3) . . . . ? O11B C11B C12B O12B -2.6(4) . . . . ? C16B C11B C12B O12B 176.3(2) . . . . ? O11B C11B C12B C13B 176.7(3) . . . . ? C16B C11B C12B C13B -4.4(4) . . . . ? O12B C12B C13B C14B -179.4(3) . . . . ? C11B C12B C13B C14B 1.4(5) . . . . ? C12B C13B C14B C15B 1.7(6) . . . . ? C13B C14B C15B C16B -1.5(6) . . . . ? C14B C15B C16B C11B -1.6(5) . . . . ? C14B C15B C16B C17B 177.0(3) . . . . ? O11B C11B C16B C15B -176.8(3) . . . . ? C12B C11B C16B C15B 4.4(4) . . . . ? O11B C11B C16B C17B 4.5(4) . . . . ? C12B C11B C16B C17B -174.2(3) . . . . ? C15B C16B C17B O18B 174.0(3) . . . . ? C11B C16B C17B O18B -7.3(5) . . . . ? C15B C16B C17B O19B -7.6(4) . . . . ? C11B C16B C17B O19B 171.1(3) . . . . ? O19B C17B O18B Li1 -168.0(3) . . . . ? C16B C17B O18B Li1 10.3(5) . . . . ? O18A Li1 O18B C17B 111.5(3) . . . . ? O11A Li1 O18B C17B -148.8(3) . . . . ? O11B Li1 O18B C17B -8.1(4) . . . . ? O18B C17B O19B C20B -2.0(4) . . . . ? C16B C17B O19B C20B 179.6(3) . . . . ? O2A Li3 O21B C21B 109.7(3) . . . . ? O28B Li3 O21B C21B 1.8(3) . . . . ? Mo1B Li3 O21B C21B -172.7(3) . . . . ? O2A Li3 O21B Mo1B -77.7(3) . . . . ? O28B Li3 O21B Mo1B 174.49(14) . . . . ? O1B Mo1B O21B C21B 85.1(2) . . . . ? O2B Mo1B O21B C21B -172.0(2) . . . . ? O12B Mo1B O21B C21B -53.6(3) . . . . ? O22B Mo1B O21B C21B -3.33(18) . . . . ? O11B Mo1B O21B C21B -84.23(19) . . . . ? Li3 Mo1B O21B C21B 173.4(3) . . . . ? O1B Mo1B O21B Li3 -88.3(2) . . . . ? O2B Mo1B O21B Li3 14.6(2) . . . . ? O12B Mo1B O21B Li3 133.0(3) . . . . ? O22B Mo1B O21B Li3 -176.7(2) . . . . ? O11B Mo1B O21B Li3 102.36(19) . . . . ? O1B Mo1B O22B C22B -102.3(2) . . . . ? O2B Mo1B O22B C22B 33.1(4) . . . . ? O12B Mo1B O22B C22B 166.7(2) . . . . ? O21B Mo1B O22B C22B 1.76(19) . . . . ? O11B Mo1B O22B C22B 92.1(2) . . . . ? Li3 Mo1B O22B C22B -0.1(2) . . . . ? Li3 O21B C21B C26B -3.6(4) . . . . ? Mo1B O21B C21B C26B -175.9(2) . . . . ? Li3 O21B C21B C22B 176.6(3) . . . . ? Mo1B O21B C21B C22B 4.3(3) . . . . ? Mo1B O22B C22B C23B -179.8(2) . . . . ? Mo1B O22B C22B C21B -0.1(3) . . . . ? O21B C21B C22B O22B -2.6(4) . . . . ? C26B C21B C22B O22B 177.6(3) . . . . ? O21B C21B C22B C23B 177.1(3) . . . . ? C26B C21B C22B C23B -2.6(4) . . . . ? O22B C22B C23B C24B -177.7(3) . . . . ? C21B C22B C23B C24B 2.6(4) . . . . ? C22B C23B C24B C25B -0.4(5) . . . . ? C23B C24B C25B C26B -1.9(5) . . . . ? O21B C21B C26B C25B -179.2(3) . . . . ? C22B C21B C26B C25B 0.5(4) . . . . ? O21B C21B C26B C27B 1.3(4) . . . . ? C22B C21B C26B C27B -179.0(3) . . . . ? C24B C25B C26B C21B 1.8(5) . . . . ? C24B C25B C26B C27B -178.8(3) . . . . ? C21B C26B C27B O28B 3.3(5) . . . . ? C25B C26B C27B O28B -176.2(3) . . . . ? C21B C26B C27B O29B -177.9(3) . . . . ? C25B C26B C27B O29B 2.7(4) . . . . ? O29B C27B O28B Li3 176.0(3) . . . . ? C26B C27B O28B Li3 -5.2(5) . . . . ? O2A Li3 O28B C27B -111.9(3) . . . . ? O21B Li3 O28B C27B 2.6(4) . . . . ? Mo1B Li3 O28B C27B 6.3(5) . . . . ? O28B C27B O29B C30B -1.9(5) . . . . ? C26B C27B O29B C30B 179.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.566 _refine_diff_density_min -1.023 _refine_diff_density_rms 0.096 # Attachment 'fro3583.cif' data_fro3583 _database_code_depnum_ccdc_archive 'CCDC 294766' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H22 Li2 Mo N2 O10' _chemical_formula_weight 560.22 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.389(1) _cell_length_b 8.850(1) _cell_length_c 15.623(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.76(1) _cell_angle_gamma 90.00 _cell_volume 2404.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used 2617 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description column _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 0.601 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7950 _exptl_absorpt_correction_T_max 0.8892 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotataing anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w an d\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9858 _diffrn_reflns_av_R_equivalents 0.029 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.48 _diffrn_reflns_theta_max 28.28 _reflns_number_total 2895 _reflns_number_gt 2698 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.v., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0434P)^2^+2.5413P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2895 _refine_ls_number_parameters 161 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0829 _refine_ls_wR_factor_gt 0.0804 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 Mo Mo 0.5000 0.22452(2) 0.2500 0.03741(10) Uani 1 2 d S . . C1 C 0.62146(11) -0.0119(2) 0.26447(12) 0.0381(4) Uani 1 1 d . . . O1 O 0.56383(8) 0.03458(15) 0.31123(8) 0.0388(3) Uani 1 1 d . . . C2 C 0.62744(11) 0.0546(2) 0.18236(12) 0.0392(4) Uani 1 1 d . . . O2 O 0.57567(8) 0.16368(17) 0.16351(8) 0.0426(3) Uani 1 1 d . . . C3 C 0.68277(12) 0.0073(3) 0.12592(14) 0.0516(5) Uani 1 1 d . . . H3 H 0.6847 0.0496 0.0701 0.062 Uiso 1 1 calc R . . C4 C 0.73590(15) -0.1025(4) 0.15091(17) 0.0709(8) Uani 1 1 d . . . H4 H 0.7740 -0.1350 0.1119 0.085 Uiso 1 1 calc R . . C5 C 0.73362(16) -0.1636(4) 0.23102(18) 0.0744(9) Uani 1 1 d . . . H5 H 0.7710 -0.2366 0.2477 0.089 Uiso 1 1 calc R . . C6 C 0.67633(13) -0.1197(3) 0.28960(14) 0.0539(6) Uani 1 1 d . . . C7 C 0.67696(17) -0.1865(4) 0.37396(16) 0.0682(8) Uani 1 1 d . . . H7 H 0.7169 -0.2569 0.3858 0.082 Uiso 1 1 calc R . . O7 O 0.63202(11) -0.1625(2) 0.43166(10) 0.0640(5) Uani 1 1 d . . . O10 O 0.45061(10) 0.34447(18) 0.18370(10) 0.0518(4) Uani 1 1 d . . . O11 O 0.54067(9) 0.13155(17) 0.51578(9) 0.0456(3) Uani 1 1 d . . . C12 C 0.57231(13) 0.2562(2) 0.50785(14) 0.0437(4) Uani 1 1 d . . . H12 H 0.5953 0.2774 0.4543 0.052 Uiso 1 1 calc R . . N13 N 0.57688(11) 0.3615(2) 0.56685(12) 0.0492(4) Uani 1 1 d . . . C14 C 0.5454(2) 0.3396(3) 0.65173(15) 0.0742(9) Uani 1 1 d . . . H14A H 0.4953 0.3899 0.6550 0.111 Uiso 1 1 calc R . . H14B H 0.5805 0.3828 0.6947 0.111 Uiso 1 1 calc R . . H14C H 0.5390 0.2313 0.6626 0.111 Uiso 1 1 calc R . . C15 C 0.6141(2) 0.5054(4) 0.5504(2) 0.0800(9) Uani 1 1 d . . . H15A H 0.6603 0.5144 0.5867 0.120 Uiso 1 1 calc R . . H15B H 0.5786 0.5880 0.5634 0.120 Uiso 1 1 calc R . . H15C H 0.6286 0.5108 0.4901 0.120 Uiso 1 1 calc R . . Li Li 0.5429(2) -0.0253(4) 0.4269(2) 0.0464(8) Uani 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 Mo 0.04724(15) 0.02255(13) 0.04251(14) 0.000 0.00368(9) 0.000 C1 0.0403(9) 0.0336(9) 0.0406(9) 0.0004(7) 0.0144(7) 0.0019(7) O1 0.0460(7) 0.0311(7) 0.0397(6) 0.0051(5) 0.0174(5) 0.0084(5) C2 0.0392(9) 0.0386(10) 0.0399(9) 0.0006(7) 0.0115(7) -0.0074(7) O2 0.0503(7) 0.0367(7) 0.0409(7) 0.0077(6) 0.0104(5) -0.0063(6) C3 0.0485(11) 0.0635(15) 0.0432(10) -0.0004(9) 0.0179(8) -0.0102(10) C4 0.0557(13) 0.097(2) 0.0604(14) 0.0008(14) 0.0315(11) 0.0181(14) C5 0.0665(16) 0.092(2) 0.0654(15) 0.0083(15) 0.0271(13) 0.0383(16) C6 0.0556(12) 0.0583(14) 0.0483(11) 0.0046(10) 0.0175(9) 0.0207(11) C7 0.0808(18) 0.0702(17) 0.0541(13) 0.0095(12) 0.0172(12) 0.0435(15) O7 0.0873(12) 0.0584(11) 0.0470(8) 0.0090(8) 0.0210(8) 0.0316(10) O10 0.0651(9) 0.0330(8) 0.0570(8) 0.0025(6) -0.0061(7) 0.0008(7) O11 0.0624(9) 0.0340(7) 0.0408(7) -0.0015(6) 0.0184(6) 0.0020(6) C12 0.0492(11) 0.0420(11) 0.0402(10) -0.0007(8) 0.0138(8) 0.0021(8) N13 0.0644(11) 0.0358(9) 0.0476(9) -0.0032(7) 0.0101(8) 0.0048(8) C14 0.138(3) 0.0422(14) 0.0430(11) -0.0041(10) 0.0210(14) 0.0156(15) C15 0.094(2) 0.0535(17) 0.093(2) -0.0162(15) 0.0249(17) -0.0204(15) Li 0.064(2) 0.0340(17) 0.0417(16) -0.0003(13) 0.0218(15) 0.0061(15) _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 Mo O10 1.7070(16) . ? Mo O10 1.7070(16) 2_655 ? Mo O2 1.9733(14) . ? Mo O2 1.9733(14) 2_655 ? Mo O1 2.2236(13) 2_655 ? Mo O1 2.2236(13) . ? C1 O1 1.314(2) . ? C1 C6 1.402(3) . ? C1 C2 1.416(3) . ? O1 Li 1.922(3) . ? C2 O2 1.350(3) . ? C2 C3 1.379(3) . ? C3 C4 1.393(4) . ? C4 C5 1.365(4) . ? C5 C6 1.416(3) . ? C6 C7 1.444(3) . ? C7 O7 1.219(3) . ? O7 Li 1.969(4) . ? O11 C12 1.240(3) . ? O11 Li 1.958(4) 5_656 ? O11 Li 1.965(4) . ? C12 N13 1.312(3) . ? N13 C15 1.453(3) . ? N13 C14 1.455(3) . ? Li O11 1.958(4) 5_656 ? Li Li 2.782(6) 5_656 ? 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 O10 Mo O10 103.10(11) . 2_655 ? O10 Mo O2 95.10(7) . . ? O10 Mo O2 104.51(7) 2_655 . ? O10 Mo O2 104.51(7) . 2_655 ? O10 Mo O2 95.10(7) 2_655 2_655 ? O2 Mo O2 148.33(8) . 2_655 ? O10 Mo O1 87.98(7) . 2_655 ? O10 Mo O1 167.27(7) 2_655 2_655 ? O2 Mo O1 80.37(5) . 2_655 ? O2 Mo O1 75.80(5) 2_655 2_655 ? O10 Mo O1 167.27(7) . . ? O10 Mo O1 87.98(7) 2_655 . ? O2 Mo O1 75.80(5) . . ? O2 Mo O1 80.37(5) 2_655 . ? O1 Mo O1 81.78(8) 2_655 . ? O1 C1 C6 125.37(17) . . ? O1 C1 C2 116.03(17) . . ? C6 C1 C2 118.60(17) . . ? C1 O1 Li 126.25(16) . . ? C1 O1 Mo 112.19(11) . . ? Li O1 Mo 120.87(12) . . ? O2 C2 C3 123.13(18) . . ? O2 C2 C1 115.98(16) . . ? C3 C2 C1 120.9(2) . . ? C2 O2 Mo 119.64(11) . . ? C2 C3 C4 119.9(2) . . ? C5 C4 C3 120.4(2) . . ? C4 C5 C6 120.9(2) . . ? C1 C6 C5 119.2(2) . . ? C1 C6 C7 122.06(19) . . ? C5 C6 C7 118.7(2) . . ? O7 C7 C6 127.3(2) . . ? C7 O7 Li 126.19(19) . . ? C12 O11 Li 143.72(17) . 5_656 ? C12 O11 Li 123.03(16) . . ? Li O11 Li 90.35(14) 5_656 . ? O11 C12 N13 125.76(19) . . ? C12 N13 C15 121.4(2) . . ? C12 N13 C14 121.7(2) . . ? C15 N13 C14 116.9(2) . . ? O1 Li O11 135.5(2) . 5_656 ? O1 Li O11 118.39(19) . . ? O11 Li O11 89.65(14) 5_656 . ? O1 Li O7 92.71(15) . . ? O11 Li O7 105.95(18) 5_656 . ? O11 Li O7 115.6(2) . . ? O1 Li Li 146.9(3) . 5_656 ? O11 Li Li 44.92(11) 5_656 5_656 ? O11 Li Li 44.73(11) . 5_656 ? O7 Li Li 119.9(2) . 5_656 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 O1 Li 3.1(3) . . . . ? C2 C1 O1 Li -176.61(19) . . . . ? C6 C1 O1 Mo 173.66(19) . . . . ? C2 C1 O1 Mo -6.1(2) . . . . ? O10 Mo O1 C1 50.6(3) . . . . ? O10 Mo O1 C1 -100.22(14) 2_655 . . . ? O2 Mo O1 C1 5.30(13) . . . . ? O2 Mo O1 C1 164.26(14) 2_655 . . . ? O1 Mo O1 C1 87.38(13) 2_655 . . . ? O10 Mo O1 Li -138.3(3) . . . . ? O10 Mo O1 Li 70.89(17) 2_655 . . . ? O2 Mo O1 Li 176.41(17) . . . . ? O2 Mo O1 Li -24.63(16) 2_655 . . . ? O1 Mo O1 Li -101.51(16) 2_655 . . . ? O1 C1 C2 O2 3.4(3) . . . . ? C6 C1 C2 O2 -176.40(19) . . . . ? O1 C1 C2 C3 -175.89(19) . . . . ? C6 C1 C2 C3 4.3(3) . . . . ? C3 C2 O2 Mo -179.05(16) . . . . ? C1 C2 O2 Mo 1.7(2) . . . . ? O10 Mo O2 C2 -174.63(14) . . . . ? O10 Mo O2 C2 80.41(15) 2_655 . . . ? O2 Mo O2 C2 -46.05(13) 2_655 . . . ? O1 Mo O2 C2 -87.55(14) 2_655 . . . ? O1 Mo O2 C2 -3.68(13) . . . . ? O2 C2 C3 C4 177.9(2) . . . . ? C1 C2 C3 C4 -2.9(3) . . . . ? C2 C3 C4 C5 -0.1(4) . . . . ? C3 C4 C5 C6 1.5(5) . . . . ? O1 C1 C6 C5 177.4(2) . . . . ? C2 C1 C6 C5 -2.8(4) . . . . ? O1 C1 C6 C7 -3.4(4) . . . . ? C2 C1 C6 C7 176.4(2) . . . . ? C4 C5 C6 C1 0.0(5) . . . . ? C4 C5 C6 C7 -179.3(3) . . . . ? C1 C6 C7 O7 1.3(5) . . . . ? C5 C6 C7 O7 -179.5(4) . . . . ? C6 C7 O7 Li 0.7(5) . . . . ? Li O11 C12 N13 30.6(5) 5_656 . . . ? Li O11 C12 N13 -175.5(2) . . . . ? O11 C12 N13 C15 -178.8(3) . . . . ? O11 C12 N13 C14 1.5(4) . . . . ? C1 O1 Li O11 -117.2(3) . . . 5_656 ? Mo O1 Li O11 73.0(3) . . . 5_656 ? C1 O1 Li O11 120.1(2) . . . . ? Mo O1 Li O11 -49.7(3) . . . . ? C1 O1 Li O7 -1.0(3) . . . . ? Mo O1 Li O7 -170.81(11) . . . . ? C1 O1 Li Li 169.6(4) . . . 5_656 ? Mo O1 Li Li -0.2(6) . . . 5_656 ? C12 O11 Li O1 -21.0(3) . . . . ? Li O11 Li O1 143.9(3) 5_656 . . . ? C12 O11 Li O11 -164.9(2) . . . 5_656 ? Li O11 Li O11 0.0 5_656 . . 5_656 ? C12 O11 Li O7 87.5(3) . . . . ? Li O11 Li O7 -107.6(2) 5_656 . . . ? C12 O11 Li Li -164.9(2) . . . 5_656 ? C7 O7 Li O1 -0.8(4) . . . . ? C7 O7 Li O11 138.3(3) . . . 5_656 ? C7 O7 Li O11 -124.2(3) . . . . ? C7 O7 Li Li -174.9(3) . . . 5_656 ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.273 _refine_diff_density_min -0.719 _refine_diff_density_rms 0.056 # Attachment 'fro3585.cif' data_fro3585 _database_code_depnum_ccdc_archive 'CCDC 294767' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H74 Li4 Mo4 N6 O32' _chemical_formula_weight 1778.75 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 '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 9.366(1) _cell_length_b 12.826(1) _cell_length_c 16.219(1) _cell_angle_alpha 85.79(1) _cell_angle_beta 73.76(1) _cell_angle_gamma 75.38(1) _cell_volume 1810.0(3) _cell_formula_units_Z 1 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used 3172 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 0.767 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6562 _exptl_absorpt_correction_T_max 0.8026 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995 & 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12594 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 27.88 _reflns_number_total 8101 _reflns_number_gt 7229 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'CollecT (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0348P)^2^+2.8223P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8101 _refine_ls_number_parameters 475 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0878 _refine_ls_wR_factor_gt 0.0842 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 Mo1 Mo 0.80757(2) 1.753692(16) 0.384136(13) 0.01975(6) Uani 1 1 d . . . Mo2 Mo 0.88377(2) 1.472623(16) 0.353258(13) 0.02009(6) Uani 1 1 d . . . O1 O 0.77625(19) 1.61792(13) 0.36076(11) 0.0215(3) Uani 1 1 d . . . O11 O 0.8907(2) 1.75528(14) 0.24758(11) 0.0226(3) Uani 1 1 d . . . O12 O 0.9312(2) 1.86388(14) 0.35961(11) 0.0264(4) Uani 1 1 d . . . C11 C 0.9692(3) 1.8283(2) 0.21509(16) 0.0227(5) Uani 1 1 d . . . C12 C 0.9913(3) 1.8899(2) 0.27733(17) 0.0258(5) Uani 1 1 d . . . C13 C 1.0724(4) 1.9683(2) 0.2530(2) 0.0357(6) Uani 1 1 d . . . H13 H 1.0881 2.0088 0.2950 0.043 Uiso 1 1 calc R . . C14 C 1.1313(4) 1.9874(3) 0.1654(2) 0.0423(7) Uani 1 1 d . . . H14 H 1.1865 2.0417 0.1481 0.051 Uiso 1 1 calc R . . C15 C 1.1105(4) 1.9286(3) 0.1039(2) 0.0385(7) Uani 1 1 d . . . H15 H 1.1502 1.9435 0.0449 0.046 Uiso 1 1 calc R . . C16 C 1.0310(3) 1.8467(2) 0.12750(17) 0.0279(5) Uani 1 1 d . . . C17 C 1.0177(3) 1.7777(2) 0.06279(17) 0.0279(5) Uani 1 1 d . . . O18 O 0.9599(2) 1.70117(16) 0.07797(12) 0.0317(4) Uani 1 1 d . . . O19 O 1.0793(3) 1.8060(2) -0.01747(13) 0.0453(6) Uani 1 1 d . . . C20 C 1.0712(5) 1.7418(3) -0.0853(2) 0.0510(9) Uani 1 1 d . . . H20A H 0.9694 1.7673 -0.0966 0.061 Uiso 1 1 calc R . . H20B H 1.0831 1.6656 -0.0666 0.061 Uiso 1 1 calc R . . C21 C 1.1901(5) 1.7493(4) -0.1635(2) 0.0605(11) Uani 1 1 d . . . H21 H 1.1948 1.7092 -0.2116 0.073 Uiso 1 1 calc R . . C22 C 1.2864(9) 1.8037(7) -0.1733(4) 0.140(4) Uani 1 1 d . . . H22A H 1.2861 1.8451 -0.1271 0.167 Uiso 1 1 calc R . . H22B H 1.3604 1.8038 -0.2271 0.167 Uiso 1 1 calc R . . O31 O 1.0790(2) 1.34920(14) 0.31238(11) 0.0232(4) Uani 1 1 d . . . O32 O 0.9768(2) 1.50582(14) 0.22459(11) 0.0245(4) Uani 1 1 d . . . C31 C 1.1493(3) 1.3416(2) 0.22821(15) 0.0211(5) Uani 1 1 d . . . C32 C 1.0926(3) 1.42936(19) 0.17890(16) 0.0218(5) Uani 1 1 d . . . C33 C 1.1544(3) 1.4321(2) 0.09104(17) 0.0295(6) Uani 1 1 d . . . H33 H 1.1162 1.4913 0.0580 0.035 Uiso 1 1 calc R . . C34 C 1.2741(4) 1.3463(2) 0.05157(17) 0.0341(6) Uani 1 1 d . . . H34 H 1.3166 1.3471 -0.0089 0.041 Uiso 1 1 calc R . . C35 C 1.3312(3) 1.2609(2) 0.09907(17) 0.0311(6) Uani 1 1 d . . . H35 H 1.4133 1.2038 0.0710 0.037 Uiso 1 1 calc R . . C36 C 1.2700(3) 1.2568(2) 0.18857(16) 0.0235(5) Uani 1 1 d . . . C37 C 1.3291(3) 1.1646(2) 0.23978(16) 0.0253(5) Uani 1 1 d . . . O38 O 1.2922(2) 1.15685(16) 0.31763(12) 0.0341(5) Uani 1 1 d . . . O39 O 1.4317(2) 1.08616(15) 0.18983(12) 0.0314(4) Uani 1 1 d . . . C40 C 1.4987(4) 0.9912(2) 0.2322(2) 0.0365(7) Uani 1 1 d . . . H40A H 1.4176 0.9570 0.2670 0.044 Uiso 1 1 calc R . . H40B H 1.5528 1.0109 0.2709 0.044 Uiso 1 1 calc R . . C41 C 1.6083(4) 0.9153(2) 0.1651(2) 0.0395(7) Uani 1 1 d . . . H41 H 1.6672 0.8516 0.1846 0.047 Uiso 1 1 calc R . . C42 C 1.6315(5) 0.9275(3) 0.0826(2) 0.0566(10) Uani 1 1 d . . . H42A H 1.5755 0.9898 0.0599 0.068 Uiso 1 1 calc R . . H42B H 1.7046 0.8741 0.0448 0.068 Uiso 1 1 calc R . . O111 O 0.6316(2) 1.83309(16) 0.38515(13) 0.0320(4) Uani 1 1 d . . . O112 O 0.8091(2) 1.74504(15) 0.49047(11) 0.0275(4) Uani 1 1 d . . . O211 O 0.7468(2) 1.40940(16) 0.34922(14) 0.0344(4) Uani 1 1 d . . . O212 O 0.9149(2) 1.44415(16) 0.45150(12) 0.0319(4) Uani 1 1 d . . . O101 O 1.0558(2) 1.63014(16) 0.35885(12) 0.0274(4) Uani 1 1 d . . . C102 C 1.1595(3) 1.6561(2) 0.38186(16) 0.0264(5) Uani 1 1 d . . . H102 H 1.1403 1.7280 0.4006 0.032 Uiso 1 1 calc R . . N103 N 1.2927(2) 1.59104(19) 0.38190(14) 0.0278(5) Uani 1 1 d . . . C104 C 1.4015(3) 1.6272(3) 0.4155(2) 0.0403(7) Uani 1 1 d . . . H10A H 1.3691 1.7056 0.4230 0.060 Uiso 1 1 calc R . . H10B H 1.5037 1.6078 0.3751 0.060 Uiso 1 1 calc R . . H10C H 1.4047 1.5924 0.4711 0.060 Uiso 1 1 calc R . . C105 C 1.3256(4) 1.4765(3) 0.3655(2) 0.0437(8) Uani 1 1 d . . . H10D H 1.3011 1.4380 0.4201 0.066 Uiso 1 1 calc R . . H10E H 1.4345 1.4502 0.3360 0.066 Uiso 1 1 calc R . . H10F H 1.2634 1.4641 0.3294 0.066 Uiso 1 1 calc R . . Li1 Li 0.8648(5) 1.6416(4) 0.1882(3) 0.0278(9) Uani 1 1 d . . . Li2 Li 1.1189(5) 1.2471(4) 0.4073(3) 0.0256(9) Uani 1 1 d . . . O201 O 0.6773(3) 1.6192(2) 0.18302(16) 0.0541(7) Uani 1 1 d . . . C202 C 0.5508(7) 1.6398(7) 0.1813(3) 0.119(3) Uani 1 1 d . . . H202 H 0.5000 1.7095 0.2046 0.143 Uiso 1 1 calc R . . N203 N 0.4614(3) 1.6003(3) 0.15882(19) 0.0476(7) Uani 1 1 d . . . C204 C 0.3145(6) 1.6361(7) 0.1515(4) 0.120(3) Uani 1 1 d . . . H20C H 0.2703 1.7088 0.1755 0.180 Uiso 1 1 calc R . . H20D H 0.2524 1.5873 0.1829 0.180 Uiso 1 1 calc R . . H20E H 0.3159 1.6376 0.0907 0.180 Uiso 1 1 calc R . . C205 C 0.5297(8) 1.4850(5) 0.1285(5) 0.109(2) Uani 1 1 d . . . H20F H 0.5676 1.4838 0.0657 0.164 Uiso 1 1 calc R . . H20G H 0.4510 1.4438 0.1467 0.164 Uiso 1 1 calc R . . H20H H 0.6148 1.4526 0.1535 0.164 Uiso 1 1 calc R . . O301 O 0.9575(3) 1.17492(18) 0.44196(15) 0.0406(5) Uani 1 1 d . . . C302 C 0.8472(4) 1.1692(2) 0.41675(19) 0.0337(6) Uani 1 1 d . . . H302 H 0.8333 1.2088 0.3666 0.040 Uiso 1 1 calc R . . N303 N 0.7469(3) 1.11230(19) 0.45414(15) 0.0311(5) Uani 1 1 d . . . C304 C 0.6206(4) 1.1077(3) 0.4196(2) 0.0503(9) Uani 1 1 d . . . H30A H 0.6187 1.1575 0.3709 0.075 Uiso 1 1 calc R . . H30B H 0.5236 1.1282 0.4643 0.075 Uiso 1 1 calc R . . H30C H 0.6347 1.0342 0.4003 0.075 Uiso 1 1 calc R . . C305 C 0.7628(4) 1.0460(3) 0.5286(2) 0.0429(7) Uani 1 1 d . . . H30D H 0.7994 0.9700 0.5116 0.064 Uiso 1 1 calc R . . H30E H 0.6631 1.0568 0.5716 0.064 Uiso 1 1 calc R . . H30F H 0.8365 1.0661 0.5531 0.064 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.02005(11) 0.01802(10) 0.01927(11) -0.00313(8) -0.00480(8) -0.00091(8) Mo2 0.02077(11) 0.01878(11) 0.01776(11) -0.00098(8) -0.00283(8) -0.00190(8) O1 0.0194(8) 0.0199(8) 0.0238(8) -0.0025(7) -0.0047(7) -0.0027(6) O11 0.0257(9) 0.0222(8) 0.0215(8) 0.0000(7) -0.0075(7) -0.0077(7) O12 0.0331(10) 0.0231(9) 0.0243(9) -0.0040(7) -0.0071(8) -0.0085(7) C11 0.0228(11) 0.0204(11) 0.0260(12) 0.0011(10) -0.0089(10) -0.0047(9) C12 0.0293(13) 0.0214(12) 0.0277(13) -0.0010(10) -0.0095(10) -0.0058(10) C13 0.0441(17) 0.0310(14) 0.0383(16) -0.0028(12) -0.0135(13) -0.0169(13) C14 0.0518(19) 0.0406(17) 0.0428(17) 0.0054(14) -0.0109(15) -0.0295(15) C15 0.0449(17) 0.0417(17) 0.0326(15) 0.0076(13) -0.0076(13) -0.0222(14) C16 0.0306(13) 0.0289(13) 0.0260(13) 0.0028(11) -0.0087(11) -0.0099(11) C17 0.0293(13) 0.0310(14) 0.0226(12) 0.0028(10) -0.0065(10) -0.0069(11) O18 0.0433(12) 0.0303(10) 0.0244(9) 0.0013(8) -0.0106(8) -0.0130(9) O19 0.0640(15) 0.0558(14) 0.0223(10) 0.0010(9) -0.0054(10) -0.0330(12) C20 0.066(2) 0.065(2) 0.0268(15) -0.0060(15) -0.0081(15) -0.028(2) C21 0.066(3) 0.089(3) 0.0318(17) -0.0060(18) -0.0078(17) -0.034(2) C22 0.157(7) 0.244(10) 0.050(3) -0.029(4) 0.013(3) -0.146(7) O31 0.0259(9) 0.0212(8) 0.0167(8) -0.0021(7) -0.0026(7) 0.0021(7) O32 0.0278(9) 0.0205(8) 0.0200(8) -0.0015(7) -0.0046(7) 0.0017(7) C31 0.0240(11) 0.0224(11) 0.0165(11) -0.0023(9) -0.0043(9) -0.0056(9) C32 0.0241(12) 0.0191(11) 0.0200(11) -0.0036(9) -0.0038(9) -0.0026(9) C33 0.0385(15) 0.0268(13) 0.0199(12) 0.0011(10) -0.0067(11) -0.0038(11) C34 0.0425(16) 0.0329(14) 0.0180(12) -0.0029(11) 0.0000(11) -0.0015(12) C35 0.0353(14) 0.0289(13) 0.0210(12) -0.0059(10) 0.0005(11) -0.0003(11) C36 0.0253(12) 0.0216(11) 0.0210(12) -0.0043(9) -0.0042(9) -0.0022(9) C37 0.0260(12) 0.0236(12) 0.0242(12) -0.0054(10) -0.0056(10) -0.0022(10) O38 0.0406(11) 0.0303(10) 0.0224(9) -0.0020(8) -0.0058(8) 0.0052(8) O39 0.0361(11) 0.0237(9) 0.0259(9) -0.0050(8) -0.0064(8) 0.0069(8) C40 0.0433(17) 0.0269(14) 0.0331(15) -0.0017(12) -0.0133(13) 0.0062(12) C41 0.0360(16) 0.0289(14) 0.0516(19) -0.0095(13) -0.0189(14) 0.0063(12) C42 0.058(2) 0.048(2) 0.051(2) -0.0213(17) -0.0195(18) 0.0200(17) O111 0.0278(10) 0.0273(10) 0.0357(10) -0.0026(8) -0.0089(8) 0.0038(8) O112 0.0325(10) 0.0277(9) 0.0212(9) -0.0033(7) -0.0062(7) -0.0056(8) O211 0.0321(10) 0.0264(10) 0.0445(12) -0.0019(9) -0.0082(9) -0.0086(8) O212 0.0350(11) 0.0349(10) 0.0185(9) 0.0010(8) -0.0031(8) -0.0004(8) O101 0.0208(9) 0.0349(10) 0.0257(9) -0.0026(8) -0.0083(7) -0.0023(7) C102 0.0231(12) 0.0345(14) 0.0199(11) -0.0017(10) -0.0035(10) -0.0058(10) N103 0.0188(10) 0.0365(12) 0.0263(11) -0.0030(9) -0.0046(8) -0.0045(9) C104 0.0254(14) 0.0540(19) 0.0454(17) -0.0047(15) -0.0149(13) -0.0095(13) C105 0.0325(16) 0.0370(16) 0.058(2) -0.0088(15) -0.0134(14) 0.0010(13) Li1 0.030(2) 0.028(2) 0.031(2) -0.0003(18) -0.0158(19) -0.0066(18) Li2 0.029(2) 0.029(2) 0.0197(19) 0.0051(17) -0.0090(17) -0.0074(18) O201 0.0368(13) 0.089(2) 0.0487(14) 0.0131(13) -0.0240(11) -0.0275(13) C202 0.107(4) 0.266(9) 0.033(2) 0.037(3) -0.025(2) -0.136(6) N203 0.0366(15) 0.070(2) 0.0429(15) 0.0055(14) -0.0122(12) -0.0243(14) C204 0.049(3) 0.240(9) 0.078(4) 0.009(5) -0.024(3) -0.044(4) C205 0.095(5) 0.080(4) 0.134(6) -0.034(4) 0.006(4) -0.022(3) O301 0.0435(12) 0.0404(12) 0.0432(12) 0.0055(10) -0.0152(10) -0.0175(10) C302 0.0467(17) 0.0254(13) 0.0285(14) 0.0024(11) -0.0105(12) -0.0082(12) N303 0.0366(13) 0.0269(11) 0.0294(12) -0.0006(9) -0.0088(10) -0.0068(10) C304 0.053(2) 0.057(2) 0.050(2) -0.0009(17) -0.0217(17) -0.0230(18) C305 0.0485(19) 0.0410(17) 0.0362(16) 0.0118(14) -0.0078(14) -0.0129(15) _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 O111 1.7007(19) . ? Mo1 O112 1.7238(18) . ? Mo1 O1 1.9181(17) . ? Mo1 O12 1.9954(18) . ? Mo1 O11 2.1328(17) . ? Mo1 O101 2.4056(18) . ? Mo2 O212 1.6964(19) . ? Mo2 O211 1.700(2) . ? Mo2 O1 1.8760(17) . ? Mo2 O31 2.0744(17) . ? Mo2 O32 2.0821(18) . ? Mo2 Li1 3.334(5) . ? O11 C11 1.324(3) . ? O11 Li1 1.904(5) . ? O12 C12 1.349(3) . ? C11 C16 1.403(4) . ? C11 C12 1.416(3) . ? C12 C13 1.380(4) . ? C13 C14 1.400(4) . ? C14 C15 1.376(4) . ? C15 C16 1.407(4) . ? C16 C17 1.472(4) . ? C17 O18 1.214(3) . ? C17 O19 1.333(3) . ? O18 Li1 1.956(5) . ? O19 C20 1.451(4) . ? C20 C21 1.452(5) . ? C21 C22 1.243(7) . ? O31 C31 1.338(3) . ? O31 Li2 2.002(5) . ? O32 C32 1.344(3) . ? O32 Li1 1.938(5) . ? C31 C36 1.397(3) . ? C31 C32 1.411(4) . ? C32 C33 1.382(3) . ? C33 C34 1.399(4) . ? C34 C35 1.375(4) . ? C35 C36 1.406(4) . ? C36 C37 1.476(4) . ? C37 O38 1.216(3) . ? C37 O39 1.337(3) . ? O38 Li2 2.017(5) . ? O39 C40 1.443(3) . ? C40 C41 1.488(4) . ? C41 C42 1.300(5) . ? O112 Li2 1.974(5) 2_786 ? O101 C102 1.256(3) . ? C102 N103 1.314(3) . ? N103 C105 1.451(4) . ? N103 C104 1.462(4) . ? Li1 O201 1.875(5) . ? Li2 O301 1.900(5) . ? Li2 O112 1.974(5) 2_786 ? O201 C202 1.155(6) . ? C202 N203 1.226(5) . ? N203 C204 1.372(6) . ? N203 C205 1.514(6) . ? O301 C302 1.232(4) . ? C302 N303 1.322(4) . ? N303 C305 1.446(4) . ? N303 C304 1.458(4) . ? 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 O111 Mo1 O112 104.30(9) . . ? O111 Mo1 O1 98.89(9) . . ? O112 Mo1 O1 104.41(8) . . ? O111 Mo1 O12 100.27(9) . . ? O112 Mo1 O12 91.91(8) . . ? O1 Mo1 O12 150.83(7) . . ? O111 Mo1 O11 93.92(8) . . ? O112 Mo1 O11 159.57(8) . . ? O1 Mo1 O11 81.37(7) . . ? O12 Mo1 O11 75.57(7) . . ? O111 Mo1 O101 169.87(8) . . ? O112 Mo1 O101 85.12(8) . . ? O1 Mo1 O101 74.77(7) . . ? O12 Mo1 O101 82.89(7) . . ? O11 Mo1 O101 77.46(7) . . ? O212 Mo2 O211 105.98(11) . . ? O212 Mo2 O1 104.08(9) . . ? O211 Mo2 O1 102.06(9) . . ? O212 Mo2 O31 84.08(8) . . ? O211 Mo2 O31 100.27(9) . . ? O1 Mo2 O31 152.94(7) . . ? O212 Mo2 O32 146.68(9) . . ? O211 Mo2 O32 102.87(9) . . ? O1 Mo2 O32 85.61(7) . . ? O31 Mo2 O32 74.63(7) . . ? O212 Mo2 Li1 150.13(11) . . ? O211 Mo2 Li1 99.22(11) . . ? O1 Mo2 Li1 54.19(10) . . ? O31 Mo2 Li1 107.16(9) . . ? O32 Mo2 Li1 32.62(9) . . ? Mo2 O1 Mo1 137.71(10) . . ? C11 O11 Li1 127.5(2) . . ? C11 O11 Mo1 115.66(15) . . ? Li1 O11 Mo1 116.34(17) . . ? C12 O12 Mo1 119.15(15) . . ? O11 C11 C16 126.0(2) . . ? O11 C11 C12 114.3(2) . . ? C16 C11 C12 119.7(2) . . ? O12 C12 C13 124.1(2) . . ? O12 C12 C11 115.0(2) . . ? C13 C12 C11 120.8(3) . . ? C12 C13 C14 119.1(3) . . ? C15 C14 C13 121.0(3) . . ? C14 C15 C16 120.8(3) . . ? C11 C16 C15 118.6(3) . . ? C11 C16 C17 119.8(2) . . ? C15 C16 C17 121.5(3) . . ? O18 C17 O19 121.5(3) . . ? O18 C17 C16 125.6(2) . . ? O19 C17 C16 112.9(2) . . ? C17 O18 Li1 129.8(2) . . ? C17 O19 C20 116.4(2) . . ? O19 C20 C21 110.9(3) . . ? C22 C21 C20 125.8(4) . . ? C31 O31 Li2 129.2(2) . . ? C31 O31 Mo2 117.88(15) . . ? Li2 O31 Mo2 112.44(15) . . ? C32 O32 Li1 130.3(2) . . ? C32 O32 Mo2 117.41(15) . . ? Li1 O32 Mo2 111.99(16) . . ? O31 C31 C36 125.4(2) . . ? O31 C31 C32 114.4(2) . . ? C36 C31 C32 120.2(2) . . ? O32 C32 C33 125.0(2) . . ? O32 C32 C31 114.4(2) . . ? C33 C32 C31 120.6(2) . . ? C32 C33 C34 118.9(2) . . ? C35 C34 C33 120.9(2) . . ? C34 C35 C36 120.9(2) . . ? C31 C36 C35 118.4(2) . . ? C31 C36 C37 120.4(2) . . ? C35 C36 C37 121.2(2) . . ? O38 C37 O39 122.0(2) . . ? O38 C37 C36 126.3(2) . . ? O39 C37 C36 111.7(2) . . ? C37 O38 Li2 130.9(2) . . ? C37 O39 C40 117.1(2) . . ? O39 C40 C41 108.1(2) . . ? C42 C41 C40 126.4(3) . . ? Mo1 O112 Li2 158.65(18) . 2_786 ? C102 O101 Mo1 118.94(17) . . ? O101 C102 N103 124.8(3) . . ? C102 N103 C105 121.8(2) . . ? C102 N103 C104 120.4(2) . . ? C105 N103 C104 116.6(2) . . ? O201 Li1 O11 126.0(3) . . ? O201 Li1 O32 106.2(2) . . ? O11 Li1 O32 108.6(2) . . ? O201 Li1 O18 108.2(2) . . ? O11 Li1 O18 90.6(2) . . ? O32 Li1 O18 117.6(3) . . ? O201 Li1 Mo2 93.01(19) . . ? O11 Li1 Mo2 92.21(17) . . ? O32 Li1 Mo2 35.39(10) . . ? O18 Li1 Mo2 151.4(2) . . ? O301 Li2 O112 106.8(2) . 2_786 ? O301 Li2 O31 108.0(2) . . ? O112 Li2 O31 134.6(3) 2_786 . ? O301 Li2 O38 108.5(2) . . ? O112 Li2 O38 108.5(2) 2_786 . ? O31 Li2 O38 87.05(18) . . ? C202 O201 Li1 158.6(5) . . ? O201 C202 N203 140.0(9) . . ? C202 N203 C204 135.6(6) . . ? C202 N203 C205 113.2(6) . . ? C204 N203 C205 111.1(5) . . ? C302 O301 Li2 136.7(2) . . ? O301 C302 N303 125.0(3) . . ? C302 N303 C305 121.3(3) . . ? C302 N303 C304 122.0(3) . . ? C305 N303 C304 116.6(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O212 Mo2 O1 Mo1 58.94(16) . . . . ? O211 Mo2 O1 Mo1 169.06(14) . . . . ? O31 Mo2 O1 Mo1 -46.0(2) . . . . ? O32 Mo2 O1 Mo1 -88.70(14) . . . . ? Li1 Mo2 O1 Mo1 -98.20(17) . . . . ? O111 Mo1 O1 Mo2 -174.40(14) . . . . ? O112 Mo1 O1 Mo2 -67.04(15) . . . . ? O12 Mo1 O1 Mo2 55.0(2) . . . . ? O11 Mo1 O1 Mo2 92.95(14) . . . . ? O101 Mo1 O1 Mo2 13.69(13) . . . . ? O111 Mo1 O11 C11 95.47(18) . . . . ? O112 Mo1 O11 C11 -57.8(3) . . . . ? O1 Mo1 O11 C11 -166.12(17) . . . . ? O12 Mo1 O11 C11 -4.14(16) . . . . ? O101 Mo1 O11 C11 -89.91(17) . . . . ? O111 Mo1 O11 Li1 -91.77(19) . . . . ? O112 Mo1 O11 Li1 114.9(3) . . . . ? O1 Mo1 O11 Li1 6.64(18) . . . . ? O12 Mo1 O11 Li1 168.63(19) . . . . ? O101 Mo1 O11 Li1 82.85(18) . . . . ? O111 Mo1 O12 C12 -86.70(19) . . . . ? O112 Mo1 O12 C12 168.40(19) . . . . ? O1 Mo1 O12 C12 43.6(3) . . . . ? O11 Mo1 O12 C12 4.74(17) . . . . ? O101 Mo1 O12 C12 83.56(18) . . . . ? Li1 O11 C11 C16 10.2(4) . . . . ? Mo1 O11 C11 C16 -178.0(2) . . . . ? Li1 O11 C11 C12 -168.8(2) . . . . ? Mo1 O11 C11 C12 3.0(3) . . . . ? Mo1 O12 C12 C13 176.9(2) . . . . ? Mo1 O12 C12 C11 -4.8(3) . . . . ? O11 C11 C12 O12 0.9(3) . . . . ? C16 C11 C12 O12 -178.2(2) . . . . ? O11 C11 C12 C13 179.3(3) . . . . ? C16 C11 C12 C13 0.3(4) . . . . ? O12 C12 C13 C14 179.2(3) . . . . ? C11 C12 C13 C14 0.9(5) . . . . ? C12 C13 C14 C15 -0.6(5) . . . . ? C13 C14 C15 C16 -0.8(5) . . . . ? O11 C11 C16 C15 179.4(3) . . . . ? C12 C11 C16 C15 -1.6(4) . . . . ? O11 C11 C16 C17 -3.3(4) . . . . ? C12 C11 C16 C17 175.7(2) . . . . ? C14 C15 C16 C11 1.9(5) . . . . ? C14 C15 C16 C17 -175.3(3) . . . . ? C11 C16 C17 O18 -2.2(4) . . . . ? C15 C16 C17 O18 175.0(3) . . . . ? C11 C16 C17 O19 178.9(3) . . . . ? C15 C16 C17 O19 -3.8(4) . . . . ? O19 C17 O18 Li1 179.1(3) . . . . ? C16 C17 O18 Li1 0.4(5) . . . . ? O18 C17 O19 C20 1.0(4) . . . . ? C16 C17 O19 C20 179.9(3) . . . . ? C17 O19 C20 C21 -156.7(3) . . . . ? O19 C20 C21 C22 -0.7(9) . . . . ? O212 Mo2 O31 C31 -163.88(19) . . . . ? O211 Mo2 O31 C31 90.90(18) . . . . ? O1 Mo2 O31 C31 -54.3(3) . . . . ? O32 Mo2 O31 C31 -9.76(17) . . . . ? Li1 Mo2 O31 C31 -12.18(19) . . . . ? O212 Mo2 O31 Li2 22.96(17) . . . . ? O211 Mo2 O31 Li2 -82.27(18) . . . . ? O1 Mo2 O31 Li2 132.52(19) . . . . ? O32 Mo2 O31 Li2 177.07(18) . . . . ? Li1 Mo2 O31 Li2 174.65(17) . . . . ? O212 Mo2 O32 C32 61.8(2) . . . . ? O211 Mo2 O32 C32 -87.73(18) . . . . ? O1 Mo2 O32 C32 170.89(18) . . . . ? O31 Mo2 O32 C32 9.56(17) . . . . ? Li1 Mo2 O32 C32 -174.7(3) . . . . ? O212 Mo2 O32 Li1 -123.5(2) . . . . ? O211 Mo2 O32 Li1 87.00(18) . . . . ? O1 Mo2 O32 Li1 -14.38(17) . . . . ? O31 Mo2 O32 Li1 -175.71(18) . . . . ? Li2 O31 C31 C36 0.0(4) . . . . ? Mo2 O31 C31 C36 -171.8(2) . . . . ? Li2 O31 C31 C32 -179.5(2) . . . . ? Mo2 O31 C31 C32 8.6(3) . . . . ? Li1 O32 C32 C33 -2.2(4) . . . . ? Mo2 O32 C32 C33 171.4(2) . . . . ? Li1 O32 C32 C31 178.2(2) . . . . ? Mo2 O32 C32 C31 -8.2(3) . . . . ? O31 C31 C32 O32 -0.2(3) . . . . ? C36 C31 C32 O32 -179.8(2) . . . . ? O31 C31 C32 C33 -179.9(2) . . . . ? C36 C31 C32 C33 0.6(4) . . . . ? O32 C32 C33 C34 -179.5(3) . . . . ? C31 C32 C33 C34 0.1(4) . . . . ? C32 C33 C34 C35 -0.7(5) . . . . ? C33 C34 C35 C36 0.6(5) . . . . ? O31 C31 C36 C35 179.8(2) . . . . ? C32 C31 C36 C35 -0.7(4) . . . . ? O31 C31 C36 C37 0.9(4) . . . . ? C32 C31 C36 C37 -179.6(2) . . . . ? C34 C35 C36 C31 0.1(4) . . . . ? C34 C35 C36 C37 179.0(3) . . . . ? C31 C36 C37 O38 -6.9(4) . . . . ? C35 C36 C37 O38 174.2(3) . . . . ? C31 C36 C37 O39 172.8(2) . . . . ? C35 C36 C37 O39 -6.1(4) . . . . ? O39 C37 O38 Li2 -168.1(3) . . . . ? C36 C37 O38 Li2 11.5(5) . . . . ? O38 C37 O39 C40 -0.5(4) . . . . ? C36 C37 O39 C40 179.9(2) . . . . ? C37 O39 C40 C41 180.0(3) . . . . ? O39 C40 C41 C42 -5.2(5) . . . . ? O111 Mo1 O112 Li2 -127.1(5) . . . 2_786 ? O1 Mo1 O112 Li2 129.6(5) . . . 2_786 ? O12 Mo1 O112 Li2 -26.0(5) . . . 2_786 ? O11 Mo1 O112 Li2 25.3(6) . . . 2_786 ? O101 Mo1 O112 Li2 56.7(5) . . . 2_786 ? O111 Mo1 O101 C102 143.9(5) . . . . ? O112 Mo1 O101 C102 -57.50(19) . . . . ? O1 Mo1 O101 C102 -163.9(2) . . . . ? O12 Mo1 O101 C102 35.04(19) . . . . ? O11 Mo1 O101 C102 111.78(19) . . . . ? Mo1 O101 C102 N103 170.8(2) . . . . ? O101 C102 N103 C105 -8.4(4) . . . . ? O101 C102 N103 C104 -175.8(3) . . . . ? C11 O11 Li1 O201 -122.2(3) . . . . ? Mo1 O11 Li1 O201 66.0(3) . . . . ? C11 O11 Li1 O32 110.4(3) . . . . ? Mo1 O11 Li1 O32 -61.4(3) . . . . ? C11 O11 Li1 O18 -9.1(3) . . . . ? Mo1 O11 Li1 O18 179.18(12) . . . . ? C11 O11 Li1 Mo2 142.4(2) . . . . ? Mo1 O11 Li1 Mo2 -29.32(17) . . . . ? C32 O32 Li1 O201 102.1(3) . . . . ? Mo2 O32 Li1 O201 -71.7(2) . . . . ? C32 O32 Li1 O11 -119.9(3) . . . . ? Mo2 O32 Li1 O11 66.3(3) . . . . ? C32 O32 Li1 O18 -19.1(4) . . . . ? Mo2 O32 Li1 O18 167.05(18) . . . . ? C32 O32 Li1 Mo2 173.9(3) . . . . ? C17 O18 Li1 O201 132.6(3) . . . . ? C17 O18 Li1 O11 4.1(4) . . . . ? C17 O18 Li1 O32 -107.3(3) . . . . ? C17 O18 Li1 Mo2 -91.6(5) . . . . ? O212 Mo2 Li1 O201 -132.90(19) . . . . ? O211 Mo2 Li1 O201 14.53(19) . . . . ? O1 Mo2 Li1 O201 -83.74(19) . . . . ? O31 Mo2 Li1 O201 118.37(17) . . . . ? O32 Mo2 Li1 O201 114.0(3) . . . . ? O212 Mo2 Li1 O11 -6.7(3) . . . . ? O211 Mo2 Li1 O11 140.77(16) . . . . ? O1 Mo2 Li1 O11 42.50(14) . . . . ? O31 Mo2 Li1 O11 -115.39(16) . . . . ? O32 Mo2 Li1 O11 -119.7(3) . . . . ? O212 Mo2 Li1 O32 113.1(2) . . . . ? O211 Mo2 Li1 O32 -99.51(17) . . . . ? O1 Mo2 Li1 O32 162.2(2) . . . . ? O31 Mo2 Li1 O32 4.33(18) . . . . ? O212 Mo2 Li1 O18 88.6(5) . . . . ? O211 Mo2 Li1 O18 -124.0(4) . . . . ? O1 Mo2 Li1 O18 137.7(5) . . . . ? O31 Mo2 Li1 O18 -20.1(4) . . . . ? O32 Mo2 Li1 O18 -24.5(3) . . . . ? C31 O31 Li2 O301 -106.2(3) . . . . ? Mo2 O31 Li2 O301 66.0(2) . . . . ? C31 O31 Li2 O112 115.5(3) . . . 2_786 ? Mo2 O31 Li2 O112 -72.3(4) . . . 2_786 ? C31 O31 Li2 O38 2.3(3) . . . . ? Mo2 O31 Li2 O38 174.48(12) . . . . ? C37 O38 Li2 O301 99.9(3) . . . . ? C37 O38 Li2 O112 -144.5(3) . . . 2_786 ? C37 O38 Li2 O31 -8.1(3) . . . . ? O11 Li1 O201 C202 32.1(10) . . . . ? O32 Li1 O201 C202 160.4(8) . . . . ? O18 Li1 O201 C202 -72.5(9) . . . . ? Mo2 Li1 O201 C202 127.0(8) . . . . ? Li1 O201 C202 N203 158.8(7) . . . . ? O201 C202 N203 C204 -171.9(6) . . . . ? O201 C202 N203 C205 5.4(8) . . . . ? O112 Li2 O301 C302 157.7(3) 2_786 . . . ? O31 Li2 O301 C302 7.4(5) . . . . ? O38 Li2 O301 C302 -85.6(4) . . . . ? Li2 O301 C302 N303 -179.0(3) . . . . ? O301 C302 N303 C305 -2.7(5) . . . . ? O301 C302 N303 C304 -178.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 1.298 _refine_diff_density_min -1.158 _refine_diff_density_rms 0.082